###================================================= ### AUTHOR INFORMATION ###================================================= data_global _publ_contact_author_name 'Professor Daniel L. Reger' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina 29208 USA ; _publ_contact_author_phone '1 803 777 2587' _publ_contact_author_fax '1 803 777 9521' _publ_contact_author_email reger@mail.chem.sc.edu _publ_requested_journal 'Inorganic Chemistry' loop_ _publ_author_name _publ_author_address 'Reger, Daniel L.' ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; 'Horger Jacob' ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; 'Debreczeni, Agota' ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; 'Smith, Mark D.' ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; ###================================================= ### CRYSTAL DATA ###================================================= data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H56 Cu2 N4 O18, 3.333(C4 H8 O), C6 H14' _chemical_formula_sum 'C87.33 H96.67 Cu2 N4 O21.33' _chemical_formula_weight 1670.77 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 63' _symmetry_space_group_name_Hall 'P 6c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 25.6612(5) _cell_length_b 25.6612(5) _cell_length_c 21.6189(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12328.7(6) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9465 _cell_measurement_theta_min 2.425 _cell_measurement_theta_max 23.584 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5264 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7307 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS Version 2.05 (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104024 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.09 _reflns_number_total 14582 _reflns_number_gt 12400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; Disorder of three thf molecules: (1) coordinated THF (O6) (affects two atoms) (2) interstitial THF (O51/O52) two orientations (3) interstitial THF (O71) (disordered about three-fold axis; refined as a rigid pentagon with 1/3 occupancy; hydrogen atoms not calculated. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0962P)^2^+4.6784P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(11) _refine_ls_number_reflns 14582 _refine_ls_number_parameters 934 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.34552(2) 0.36262(2) 0.65655(3) 0.02912(13) Uani 1 1 d . A . Cu2 Cu 0.42614(2) 0.33052(2) 0.64147(2) 0.02592(12) Uani 1 1 d . . . C1A C 0.3111(2) 0.1202(2) 0.7783(3) 0.0413(12) Uani 1 1 d . A . C2A C 0.3480(2) 0.1103(2) 0.8240(2) 0.0396(11) Uani 1 1 d . . . C3A C 0.3820(2) 0.1535(2) 0.8671(2) 0.0408(12) Uani 1 1 d . . . C4A C 0.3845(2) 0.2094(2) 0.8688(2) 0.0391(11) Uani 1 1 d . . . C5A C 0.3499(2) 0.2223(2) 0.8222(2) 0.0368(11) Uani 1 1 d . A . C6A C 0.3478(3) 0.0564(2) 0.8229(3) 0.0514(14) Uani 1 1 d . . . H6A H 0.3241 0.0265 0.7933 0.062 Uiso 1 1 calc R . . C7A C 0.3825(3) 0.0460(3) 0.8653(3) 0.0564(15) Uani 1 1 d . . . H7A H 0.3828 0.0091 0.8638 0.068 Uiso 1 1 calc R . . C8A C 0.4154(3) 0.0869(3) 0.9081(3) 0.0559(15) Uani 1 1 d . . . H8A H 0.4374 0.0780 0.9374 0.067 Uiso 1 1 calc R . . C9A C 0.4181(3) 0.1431(3) 0.9103(3) 0.0484(13) Uani 1 1 d . . . C10A C 0.4518(3) 0.1882(3) 0.9542(3) 0.0580(16) Uani 1 1 d . . . H10A H 0.4745 0.1808 0.9841 0.070 Uiso 1 1 calc R . . C11A C 0.4531(3) 0.2415(3) 0.9555(3) 0.0526(14) Uani 1 1 d . . . H11A H 0.4768 0.2713 0.9853 0.063 Uiso 1 1 calc R . . C12A C 0.4183(2) 0.2525(3) 0.9117(2) 0.0462(13) Uani 1 1 d . . . H12A H 0.4186 0.2896 0.9121 0.055 Uiso 1 1 calc R . . C13A C 0.2799(2) 0.1904(2) 0.7360(3) 0.0374(11) Uani 1 1 d . A . H13A H 0.2654 0.1582 0.7039 0.045 Uiso 1 1 calc R . . C14A C 0.2234(2) 0.1863(3) 0.7653(3) 0.0517(14) Uani 1 1 d . . . H14A H 0.2000 0.1925 0.7333 0.078 Uiso 1 1 calc R . . H14B H 0.2353 0.2172 0.7973 0.078 Uiso 1 1 calc R . . H14C H 0.1989 0.1464 0.7839 0.078 Uiso 1 1 calc R . . C15A C 0.3201(2) 0.2493(2) 0.7028(2) 0.0315(10) Uani 1 1 d . . . N1A N 0.31504(19) 0.17712(18) 0.78091(18) 0.0369(9) Uani 1 1 d . . . O1A O 0.27979(19) 0.08392(16) 0.7396(2) 0.0540(10) Uani 1 1 d . . . O2A O 0.35176(16) 0.27091(15) 0.81979(16) 0.0412(8) Uani 1 1 d . . . O3A O 0.29981(14) 0.28387(14) 0.69509(15) 0.0340(7) Uani 1 1 d . A . O4A O 0.36951(13) 0.25608(14) 0.68427(14) 0.0317(7) Uani 1 1 d . A . C1B C 0.3370(2) 0.2004(2) 0.4237(2) 0.0413(12) Uani 1 1 d . A . C2B C 0.3329(2) 0.1407(3) 0.4176(3) 0.0476(13) Uani 1 1 d . . . C3B C 0.3124(2) 0.1004(2) 0.4678(3) 0.0468(14) Uani 1 1 d . . . C4B C 0.2935(2) 0.1141(2) 0.5227(3) 0.0453(13) Uani 1 1 d . . . C5B C 0.2925(2) 0.1710(2) 0.5292(2) 0.0387(11) Uani 1 1 d . A . C6B C 0.3498(3) 0.1259(3) 0.3636(3) 0.0589(16) Uani 1 1 d . . . H6B H 0.3637 0.1533 0.3300 0.071 Uiso 1 1 calc R . . C7B C 0.3466(3) 0.0698(4) 0.3580(4) 0.073(2) Uani 1 1 d . . . H7B H 0.3577 0.0594 0.3200 0.087 Uiso 1 1 calc R . . C8B C 0.3282(3) 0.0308(4) 0.4053(4) 0.075(2) Uani 1 1 d . . . H8B H 0.3271 -0.0066 0.4005 0.089 Uiso 1 1 calc R . . C9B C 0.3104(3) 0.0444(3) 0.4621(3) 0.0603(17) Uani 1 1 d . . . C10B C 0.2907(3) 0.0051(3) 0.5144(4) 0.073(2) Uani 1 1 d . . . H10B H 0.2888 -0.0328 0.5110 0.088 Uiso 1 1 calc R . . C11B C 0.2743(3) 0.0197(3) 0.5697(4) 0.0679(18) Uani 1 1 d . . . H11B H 0.2627 -0.0062 0.6046 0.081 Uiso 1 1 calc R . . C12B C 0.2756(3) 0.0753(3) 0.5712(3) 0.0569(16) Uani 1 1 d . . . H12B H 0.2634 0.0862 0.6082 0.068 Uiso 1 1 calc R . . C13B C 0.3156(2) 0.2684(2) 0.4845(2) 0.0343(10) Uani 1 1 d . A . H13B H 0.3427 0.2957 0.4513 0.041 Uiso 1 1 calc R . . C14B C 0.2532(2) 0.2597(2) 0.4727(3) 0.0436(12) Uani 1 1 d . . . H14D H 0.2387 0.2410 0.4321 0.065 Uiso 1 1 calc R . . H14E H 0.2552 0.2989 0.4735 0.065 Uiso 1 1 calc R . . H14F H 0.2254 0.2338 0.5048 0.065 Uiso 1 1 calc R . . C15B C 0.3435(2) 0.2981(2) 0.5468(2) 0.0304(10) Uani 1 1 d . . . N1B N 0.31591(18) 0.21097(18) 0.47898(19) 0.0363(9) Uani 1 1 d . . . O1B O 0.35822(18) 0.23850(19) 0.38432(18) 0.0550(10) Uani 1 1 d . . . O2B O 0.27201(16) 0.18311(16) 0.57368(17) 0.0439(9) Uani 1 1 d . . . O3B O 0.32037(14) 0.32456(14) 0.57447(15) 0.0350(7) Uani 1 1 d . A . O4B O 0.38866(14) 0.29492(14) 0.56316(14) 0.0310(7) Uani 1 1 d . A . C1C C 0.5859(2) 0.5246(2) 0.5152(2) 0.0369(11) Uani 1 1 d . A . C2C C 0.6187(2) 0.5025(2) 0.4776(2) 0.0385(11) Uani 1 1 d . . . C3C C 0.5869(2) 0.4508(2) 0.4405(2) 0.0380(11) Uani 1 1 d . . . C4C C 0.5232(2) 0.4193(2) 0.4387(2) 0.0354(11) Uani 1 1 d . . . C5C C 0.4895(2) 0.4400(2) 0.4767(2) 0.0330(10) Uani 1 1 d . A . C6C C 0.6808(2) 0.5317(3) 0.4799(3) 0.0483(13) Uani 1 1 d . . . H6C H 0.7023 0.5664 0.5050 0.058 Uiso 1 1 calc R . . C7C C 0.7118(3) 0.5104(3) 0.4455(3) 0.0629(18) Uani 1 1 d . . . H7C H 0.7545 0.5305 0.4478 0.075 Uiso 1 1 calc R . . C8C C 0.6820(3) 0.4605(3) 0.4081(3) 0.0561(15) Uani 1 1 d . . . H8C H 0.7042 0.4471 0.3845 0.067 Uiso 1 1 calc R . . C9C C 0.6186(2) 0.4294(2) 0.4045(3) 0.0451(13) Uani 1 1 d . . . C10C C 0.5852(3) 0.3780(3) 0.3667(3) 0.0495(14) Uani 1 1 d . . . H10C H 0.6058 0.3636 0.3418 0.059 Uiso 1 1 calc R . . C11C C 0.5246(3) 0.3493(2) 0.3655(3) 0.0456(12) Uani 1 1 d . . . H11C H 0.5031 0.3152 0.3396 0.055 Uiso 1 1 calc R . . C12C C 0.4932(2) 0.3695(2) 0.4021(2) 0.0402(11) Uani 1 1 d . . . H12C H 0.4505 0.3482 0.4015 0.048 Uiso 1 1 calc R . . C13C C 0.4890(2) 0.5040(2) 0.5612(2) 0.0367(11) Uani 1 1 d . A . H13C H 0.5191 0.5320 0.5919 0.044 Uiso 1 1 calc R . . C14C C 0.4593(3) 0.5368(2) 0.5343(3) 0.0489(13) Uani 1 1 d . . . H14I H 0.4894 0.5729 0.5126 0.073 Uiso 1 1 calc R . . H14G H 0.4413 0.5484 0.5677 0.073 Uiso 1 1 calc R . . H14H H 0.4279 0.5104 0.5051 0.073 Uiso 1 1 calc R . . C15C C 0.4484(2) 0.4461(2) 0.5959(2) 0.0321(10) Uani 1 1 d . . . N1C N 0.52380(18) 0.49013(18) 0.51430(18) 0.0368(9) Uani 1 1 d . . . O1C O 0.61163(17) 0.57061(17) 0.54629(18) 0.0507(9) Uani 1 1 d . . . O2C O 0.43560(15) 0.41613(15) 0.47653(15) 0.0363(7) Uani 1 1 d . . . O3C O 0.39877(15) 0.43870(14) 0.61552(15) 0.0353(7) Uani 1 1 d . A . O4C O 0.46808(14) 0.41073(14) 0.60375(14) 0.0322(7) Uani 1 1 d . A . C1D C 0.5655(2) 0.4319(2) 0.8321(2) 0.0374(11) Uani 1 1 d . A . C2D C 0.6289(2) 0.4550(2) 0.8122(2) 0.0384(11) Uani 1 1 d . . . C3D C 0.6534(2) 0.4962(2) 0.7630(2) 0.0361(11) Uani 1 1 d . . . C4D C 0.6179(2) 0.5153(2) 0.7310(2) 0.0364(11) Uani 1 1 d . . . C5D C 0.5549(2) 0.4919(2) 0.7486(2) 0.0321(10) Uani 1 1 d . A . C6D C 0.6640(3) 0.4364(3) 0.8421(3) 0.0499(14) Uani 1 1 d . . . H6D H 0.6476 0.4090 0.8756 0.060 Uiso 1 1 calc R . . C7D C 0.7236(3) 0.4572(3) 0.8238(3) 0.0539(15) Uani 1 1 d . . . H7D H 0.7473 0.4438 0.8447 0.065 Uiso 1 1 calc R . . C8D C 0.7477(3) 0.4973(3) 0.7753(3) 0.0574(17) Uani 1 1 d . . . H8D H 0.7881 0.5113 0.7631 0.069 Uiso 1 1 calc R . . C9D C 0.7138(2) 0.5181(2) 0.7435(3) 0.0441(13) Uani 1 1 d . . . C10D C 0.7369(2) 0.5590(3) 0.6935(3) 0.0494(14) Uani 1 1 d . . . H10D H 0.7771 0.5735 0.6801 0.059 Uiso 1 1 calc R . . C11D C 0.7022(2) 0.5781(3) 0.6644(3) 0.0525(14) Uani 1 1 d . . . H11D H 0.7188 0.6065 0.6317 0.063 Uiso 1 1 calc R . . C12D C 0.6421(2) 0.5560(2) 0.6824(2) 0.0436(12) Uani 1 1 d . . . H12D H 0.6180 0.5689 0.6613 0.052 Uiso 1 1 calc R . . C13D C 0.4677(2) 0.4238(2) 0.8100(2) 0.0330(10) Uani 1 1 d . A . H13D H 0.4573 0.3905 0.8402 0.040 Uiso 1 1 calc R . . C14D C 0.4510(2) 0.4672(3) 0.8407(2) 0.0446(12) Uani 1 1 d . . . H14K H 0.4610 0.5010 0.8127 0.067 Uiso 1 1 calc R . . H14J H 0.4736 0.4823 0.8793 0.067 Uiso 1 1 calc R . . H14L H 0.4078 0.4460 0.8496 0.067 Uiso 1 1 calc R . . C15D C 0.4343(2) 0.39449(19) 0.7505(2) 0.0294(10) Uani 1 1 d . . . N1D N 0.53201(17) 0.45164(17) 0.79805(18) 0.0328(8) Uani 1 1 d . . . O1D O 0.54323(17) 0.39725(17) 0.87426(18) 0.0498(9) Uani 1 1 d . . . O2D O 0.52192(15) 0.50551(15) 0.72124(16) 0.0387(8) Uani 1 1 d . . . O3D O 0.38752(13) 0.39652(14) 0.73652(14) 0.0319(7) Uani 1 1 d . A . O4D O 0.45605(13) 0.36780(13) 0.72112(14) 0.0301(7) Uani 1 1 d . A . C21 C 0.2112(2) 0.3299(3) 0.6853(3) 0.0511(14) Uani 1 1 d . A . H21A H 0.1890 0.3473 0.7062 0.061 Uiso 1 1 calc R . . H21B H 0.2183 0.3050 0.7154 0.061 Uiso 1 1 calc R . . C22 C 0.1769(3) 0.2932(3) 0.6297(3) 0.0648(18) Uani 1 1 d . . . H22A H 0.1330 0.2718 0.6374 0.078 Uiso 1 1 calc R . . H22B H 0.1892 0.2634 0.6188 0.078 Uiso 1 1 calc R . . C23 C 0.1941(3) 0.3399(3) 0.5791(3) 0.0568(15) Uani 1 1 d . . . H23A H 0.2011 0.3251 0.5395 0.068 Uiso 1 1 calc R . . H23B H 0.1622 0.3505 0.5732 0.068 Uiso 1 1 calc R . . C24 C 0.2512(3) 0.3931(3) 0.6025(3) 0.0548(15) Uani 1 1 d . A . H24A H 0.2840 0.4046 0.5721 0.066 Uiso 1 1 calc R . . H24B H 0.2452 0.4280 0.6089 0.066 Uiso 1 1 calc R . . O5 O 0.26673(14) 0.37624(15) 0.66020(16) 0.0412(8) Uani 1 1 d . . . C25A C 0.5164(3) 0.2996(3) 0.5721(3) 0.0601(17) Uani 0.285(12) 1 d P A 1 H25A H 0.4896 0.3010 0.5400 0.072 Uiso 0.285(12) 1 calc PR A 1 H25B H 0.5090 0.2580 0.5748 0.072 Uiso 0.285(12) 1 calc PR A 1 C26A C 0.5810(3) 0.3423(3) 0.5561(3) 0.070(2) Uani 0.285(12) 1 d PD A 1 H26A H 0.5849 0.3758 0.5300 0.084 Uiso 0.285(12) 1 calc PR A 1 H26B H 0.5990 0.3213 0.5341 0.084 Uiso 0.285(12) 1 calc PR A 1 C27A C 0.6104(7) 0.3651(11) 0.6191(6) 0.073(3) Uani 0.285(12) 1 d PD A 1 H27A H 0.6230 0.3377 0.6374 0.088 Uiso 0.285(12) 1 calc PR A 1 H27B H 0.6459 0.4060 0.6160 0.088 Uiso 0.285(12) 1 calc PR A 1 C28A C 0.5616(2) 0.3654(2) 0.6563(3) 0.0504(13) Uani 0.285(12) 1 d PD A 1 H28A H 0.5654 0.3573 0.7004 0.060 Uiso 0.285(12) 1 calc PR A 1 H28B H 0.5640 0.4050 0.6532 0.060 Uiso 0.285(12) 1 calc PR A 1 O6A O 0.50484(13) 0.31837(14) 0.63126(15) 0.0337(7) Uani 0.285(12) 1 d P A 1 C25B C 0.5164(3) 0.2996(3) 0.5721(3) 0.0601(17) Uani 0.715(12) 1 d P A 2 H25C H 0.4896 0.3010 0.5400 0.072 Uiso 0.715(12) 1 calc PR A 2 H25D H 0.5090 0.2580 0.5748 0.072 Uiso 0.715(12) 1 calc PR A 2 C26B C 0.5810(3) 0.3423(3) 0.5561(3) 0.070(2) Uani 0.715(12) 1 d PD A 2 H26C H 0.5852 0.3553 0.5124 0.084 Uiso 0.715(12) 1 calc PR A 2 H26D H 0.6062 0.3237 0.5634 0.084 Uiso 0.715(12) 1 calc PR A 2 C27B C 0.5979(4) 0.3946(4) 0.5995(4) 0.073(3) Uani 0.715(12) 1 d PD A 2 H27C H 0.6415 0.4158 0.6088 0.088 Uiso 0.715(12) 1 calc PR A 2 H27D H 0.5872 0.4235 0.5817 0.088 Uiso 0.715(12) 1 calc PR A 2 C28B C 0.5616(2) 0.3654(2) 0.6563(3) 0.0504(13) Uani 0.715(12) 1 d PD A 2 H28C H 0.5811 0.3482 0.6823 0.060 Uiso 0.715(12) 1 calc PR A 2 H28D H 0.5558 0.3944 0.6813 0.060 Uiso 0.715(12) 1 calc PR A 2 O6B O 0.50484(13) 0.31837(14) 0.63126(15) 0.0337(7) Uani 0.715(12) 1 d P A 2 C31 C 0.1052(5) 0.4271(5) 0.6316(6) 0.115(3) Uiso 1 1 d . . . H31A H 0.0675 0.4190 0.6108 0.138 Uiso 1 1 calc R . . H31B H 0.1392 0.4486 0.6025 0.138 Uiso 1 1 calc R . . C32 C 0.1157(6) 0.4652(6) 0.6928(6) 0.138(4) Uiso 1 1 d . . . H32A H 0.1590 0.4905 0.7027 0.166 Uiso 1 1 calc R . . H32B H 0.0969 0.4906 0.6904 0.166 Uiso 1 1 calc R . . C33 C 0.0835(5) 0.4136(4) 0.7385(5) 0.105(3) Uiso 1 1 d . . . H33A H 0.1101 0.4183 0.7738 0.126 Uiso 1 1 calc R . . H33B H 0.0467 0.4123 0.7546 0.126 Uiso 1 1 calc R . . C34 C 0.0681(5) 0.3592(5) 0.7040(6) 0.118(3) Uiso 1 1 d . . . H34A H 0.0761 0.3319 0.7296 0.141 Uiso 1 1 calc R . . H34B H 0.0248 0.3380 0.6933 0.141 Uiso 1 1 calc R . . O31 O 0.1014(3) 0.3738(3) 0.6518(4) 0.131(2) Uiso 1 1 d . . . C41 C 0.3123(6) 0.4933(6) 0.7556(6) 0.140(4) Uiso 1 1 d D . . H41A H 0.3173 0.4826 0.7983 0.167 Uiso 1 1 calc R . . H41B H 0.2858 0.4559 0.7326 0.167 Uiso 1 1 calc R . . C42 C 0.2867(5) 0.5340(5) 0.7560(5) 0.107(3) Uiso 1 1 d D . . H42B H 0.2423 0.5109 0.7592 0.128 Uiso 1 1 calc R . . H42A H 0.3031 0.5630 0.7907 0.128 Uiso 1 1 calc R . . C43 C 0.3047(6) 0.5626(6) 0.7003(6) 0.147(5) Uiso 1 1 d D . . H43B H 0.3167 0.6056 0.7055 0.177 Uiso 1 1 calc R . . H43A H 0.2706 0.5444 0.6708 0.177 Uiso 1 1 calc R . . C44 C 0.3571(5) 0.5579(5) 0.6744(6) 0.126(4) Uiso 1 1 d D . . H44A H 0.3458 0.5339 0.6359 0.151 Uiso 1 1 calc R . . H44B H 0.3923 0.5982 0.6662 0.151 Uiso 1 1 calc R . . O41 O 0.3695(4) 0.5268(4) 0.7255(5) 0.167(4) Uiso 1 1 d D . . C51 C 0.0589(11) 0.1806(9) 0.8495(9) 0.150 Uiso 0.595(8) 1 d PD B 3 H51A H 0.0186 0.1731 0.8618 0.180 Uiso 0.595(8) 1 calc PR B 3 H51B H 0.0871 0.1976 0.8848 0.180 Uiso 0.595(8) 1 calc PR B 3 C52 C 0.0569(11) 0.1240(9) 0.8226(10) 0.150 Uiso 0.595(8) 1 d PD B 3 H52A H 0.0967 0.1326 0.8069 0.180 Uiso 0.595(8) 1 calc PR B 3 H52B H 0.0419 0.0908 0.8531 0.180 Uiso 0.595(8) 1 calc PR B 3 C53 C 0.0166(10) 0.1119(8) 0.7756(10) 0.150 Uiso 0.595(8) 1 d PD B 3 H53A H -0.0242 0.0997 0.7912 0.180 Uiso 0.595(8) 1 calc PR B 3 H53B H 0.0146 0.0810 0.7468 0.180 Uiso 0.595(8) 1 calc PR B 3 C54 C 0.0476(10) 0.1756(9) 0.7461(9) 0.150 Uiso 0.595(8) 1 d PD B 3 H54A H 0.0747 0.1781 0.7122 0.180 Uiso 0.595(8) 1 calc PR B 3 H54B H 0.0171 0.1844 0.7290 0.180 Uiso 0.595(8) 1 calc PR B 3 O51 O 0.0815(7) 0.2179(6) 0.7941(7) 0.150 Uiso 0.595(8) 1 d PD B 3 C55 C 0.0870(12) 0.1744(12) 0.8580(12) 0.150 Uiso 0.405(8) 1 d PD B 4 H55A H 0.1060 0.1685 0.8952 0.180 Uiso 0.405(8) 1 calc PR B 4 H55B H 0.1105 0.1773 0.8205 0.180 Uiso 0.405(8) 1 calc PR B 4 C56 C 0.0198(12) 0.1272(11) 0.8520(15) 0.150 Uiso 0.405(8) 1 d PD B 4 H56A H 0.0135 0.0862 0.8457 0.180 Uiso 0.405(8) 1 calc PR B 4 H56B H -0.0034 0.1272 0.8886 0.180 Uiso 0.405(8) 1 calc PR B 4 C57 C 0.0054(13) 0.1478(12) 0.8008(15) 0.150 Uiso 0.405(8) 1 d PD B 4 H57A H -0.0385 0.1324 0.7988 0.180 Uiso 0.405(8) 1 calc PR B 4 H57B H 0.0179 0.1355 0.7628 0.180 Uiso 0.405(8) 1 calc PR B 4 C58 C 0.0402(15) 0.2168(11) 0.8078(15) 0.150 Uiso 0.405(8) 1 d PD B 4 H58A H 0.0664 0.2366 0.7716 0.180 Uiso 0.405(8) 1 calc PR B 4 H58B H 0.0127 0.2329 0.8138 0.180 Uiso 0.405(8) 1 calc PR B 4 O52 O 0.0758(10) 0.2237(9) 0.8640(10) 0.150 Uiso 0.405(8) 1 d PD B 4 C61 C 0.0957(6) 0.2261(6) 0.4314(6) 0.150 Uiso 1 1 d D . . H61A H 0.1049 0.2026 0.4022 0.225 Uiso 1 1 calc RD . . H61B H 0.1310 0.2662 0.4363 0.225 Uiso 1 1 calc R . . H61C H 0.0619 0.2299 0.4156 0.225 Uiso 1 1 calc R . . C62 C 0.0785(5) 0.1937(5) 0.4949(6) 0.150 Uiso 1 1 d D . . H62A H 0.1086 0.1821 0.5065 0.180 Uiso 1 1 calc R . . H62B H 0.0793 0.2219 0.5268 0.180 Uiso 1 1 calc R . . C63 C 0.0166(5) 0.1382(5) 0.4937(5) 0.150 Uiso 1 1 d D . . H63A H 0.0175 0.1060 0.4692 0.180 Uiso 1 1 calc R . . H63B H -0.0127 0.1476 0.4745 0.180 Uiso 1 1 calc RD . . C64 C -0.0025(5) 0.1164(5) 0.5634(5) 0.150 Uiso 1 1 d D . . H64A H 0.0294 0.1117 0.5838 0.180 Uiso 1 1 calc R . . H64B H -0.0073 0.1471 0.5865 0.180 Uiso 1 1 calc R . . C65 C -0.0611(5) 0.0571(5) 0.5643(6) 0.150 Uiso 1 1 d D . . H65A H -0.0551 0.0264 0.5430 0.180 Uiso 1 1 calc R . . H65B H -0.0917 0.0616 0.5408 0.180 Uiso 1 1 calc R . . C66 C -0.0850(6) 0.0348(6) 0.6292(6) 0.150 Uiso 1 1 d D . . H66A H -0.0864 0.0668 0.6524 0.225 Uiso 1 1 calc R . . H66B H -0.0584 0.0234 0.6504 0.225 Uiso 1 1 calc R . . H66C H -0.1256 -0.0003 0.6265 0.225 Uiso 1 1 calc R . . C71 C 0.3878(12) 0.6568(14) 0.5353(13) 0.150 Uiso 0.33 1 d PG . . C72 C 0.3257(14) 0.6134(10) 0.5404(13) 0.150 Uiso 0.33 1 d PG . . C73 C 0.2931(10) 0.6320(13) 0.5021(15) 0.150 Uiso 0.33 1 d PG . . C74 C 0.3349(13) 0.6870(12) 0.4734(11) 0.150 Uiso 0.33 1 d PG . . O71 O 0.3935(11) 0.7024(10) 0.4938(11) 0.150 Uiso 0.33 1 d PG . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0307(3) 0.0346(3) 0.0282(3) -0.0030(2) 0.0002(2) 0.0209(2) Cu2 0.0285(2) 0.0300(2) 0.0235(2) -0.0022(2) 0.0004(2) 0.0178(2) C1A 0.046(3) 0.031(3) 0.044(3) 0.007(2) 0.011(2) 0.017(2) C2A 0.045(3) 0.036(3) 0.037(3) 0.011(2) 0.010(2) 0.019(2) C3A 0.047(3) 0.040(3) 0.031(3) 0.013(2) 0.015(2) 0.019(2) C4A 0.043(3) 0.047(3) 0.032(3) 0.010(2) 0.013(2) 0.026(2) C5A 0.040(3) 0.039(3) 0.033(3) 0.002(2) 0.010(2) 0.021(2) C6A 0.063(4) 0.037(3) 0.056(4) 0.018(3) 0.014(3) 0.026(3) C7A 0.068(4) 0.040(3) 0.068(4) 0.019(3) 0.016(3) 0.032(3) C8A 0.061(4) 0.050(3) 0.057(4) 0.020(3) 0.004(3) 0.028(3) C9A 0.056(3) 0.056(3) 0.039(3) 0.019(3) 0.010(3) 0.032(3) C10A 0.066(4) 0.071(4) 0.042(3) 0.019(3) 0.001(3) 0.038(3) C11A 0.055(3) 0.061(4) 0.040(3) 0.008(3) 0.003(3) 0.028(3) C12A 0.055(3) 0.049(3) 0.035(3) 0.001(2) 0.003(2) 0.026(3) C13A 0.032(2) 0.035(3) 0.045(3) 0.003(2) -0.001(2) 0.017(2) C14A 0.043(3) 0.059(3) 0.055(4) 0.013(3) 0.010(3) 0.027(3) C15A 0.036(2) 0.039(3) 0.022(2) -0.0037(19) -0.0047(19) 0.020(2) N1A 0.042(2) 0.035(2) 0.035(2) 0.0105(18) 0.0096(18) 0.0202(19) O1A 0.062(2) 0.0316(19) 0.059(3) -0.0043(18) -0.007(2) 0.0163(18) O2A 0.052(2) 0.0414(19) 0.039(2) 0.0009(15) 0.0057(16) 0.0301(17) O3A 0.0334(17) 0.0376(17) 0.0352(18) -0.0013(14) -0.0013(14) 0.0209(15) O4A 0.0285(16) 0.0384(17) 0.0308(17) -0.0005(13) 0.0027(13) 0.0188(14) C1B 0.041(3) 0.052(3) 0.035(3) -0.015(3) -0.003(2) 0.026(3) C2B 0.039(3) 0.055(3) 0.054(3) -0.020(3) -0.013(3) 0.028(3) C3B 0.036(3) 0.043(3) 0.061(4) -0.026(3) -0.020(3) 0.020(2) C4B 0.041(3) 0.045(3) 0.050(3) -0.013(3) -0.012(2) 0.022(3) C5B 0.033(3) 0.035(3) 0.044(3) -0.010(2) -0.006(2) 0.015(2) C6B 0.057(4) 0.077(4) 0.055(4) -0.032(3) -0.013(3) 0.043(3) C7B 0.084(5) 0.088(5) 0.068(5) -0.054(4) -0.032(4) 0.059(4) C8B 0.073(4) 0.068(4) 0.095(6) -0.051(5) -0.039(4) 0.045(4) C9B 0.048(3) 0.050(3) 0.085(5) -0.026(3) -0.026(3) 0.026(3) C10B 0.061(4) 0.042(3) 0.114(7) -0.013(4) -0.031(4) 0.023(3) C11B 0.070(4) 0.046(3) 0.085(5) -0.006(3) -0.020(4) 0.026(3) C12B 0.054(4) 0.044(3) 0.072(4) -0.007(3) -0.014(3) 0.023(3) C13B 0.038(3) 0.040(3) 0.030(3) -0.008(2) -0.002(2) 0.023(2) C14B 0.045(3) 0.053(3) 0.041(3) -0.015(2) -0.013(2) 0.030(3) C15B 0.032(2) 0.030(2) 0.030(2) -0.0011(19) 0.0029(19) 0.016(2) N1B 0.037(2) 0.037(2) 0.035(2) -0.0091(18) -0.0038(17) 0.0183(18) O1B 0.063(2) 0.065(3) 0.037(2) -0.012(2) 0.0071(19) 0.032(2) O2B 0.042(2) 0.041(2) 0.041(2) -0.0025(16) 0.0031(17) 0.0159(17) O3B 0.0405(18) 0.0416(19) 0.0277(17) -0.0080(14) -0.0022(14) 0.0242(16) O4B 0.0334(17) 0.0351(17) 0.0266(16) -0.0085(13) -0.0030(13) 0.0188(14) C1C 0.036(3) 0.034(3) 0.036(3) 0.010(2) 0.001(2) 0.014(2) C2C 0.036(3) 0.042(3) 0.036(3) 0.018(2) 0.003(2) 0.018(2) C3C 0.038(3) 0.043(3) 0.039(3) 0.014(2) -0.001(2) 0.025(2) C4C 0.046(3) 0.040(3) 0.028(2) 0.008(2) -0.001(2) 0.027(2) C5C 0.041(3) 0.037(3) 0.024(2) 0.0092(19) -0.001(2) 0.022(2) C6C 0.042(3) 0.049(3) 0.047(3) 0.019(3) -0.003(2) 0.017(2) C7C 0.039(3) 0.079(5) 0.074(4) 0.031(4) 0.011(3) 0.032(3) C8C 0.051(3) 0.065(4) 0.060(4) 0.026(3) 0.016(3) 0.036(3) C9C 0.054(3) 0.050(3) 0.043(3) 0.023(2) 0.017(3) 0.035(3) C10C 0.076(4) 0.054(3) 0.039(3) 0.012(3) 0.014(3) 0.049(3) C11C 0.057(3) 0.047(3) 0.042(3) 0.000(2) 0.004(3) 0.032(3) C12C 0.052(3) 0.037(3) 0.035(3) 0.008(2) -0.002(2) 0.024(2) C13C 0.041(3) 0.035(2) 0.036(3) -0.002(2) -0.001(2) 0.020(2) C14C 0.060(3) 0.047(3) 0.051(3) 0.005(3) 0.000(3) 0.035(3) C15C 0.037(3) 0.032(2) 0.027(2) -0.0056(19) -0.0026(19) 0.018(2) N1C 0.045(2) 0.038(2) 0.026(2) 0.0036(17) -0.0013(17) 0.0196(19) O1C 0.045(2) 0.044(2) 0.051(2) 0.0001(18) -0.0008(18) 0.0130(17) O2C 0.0348(19) 0.0460(19) 0.0289(17) -0.0004(15) -0.0039(14) 0.0209(16) O3C 0.0402(18) 0.0383(18) 0.0328(17) 0.0000(14) 0.0017(14) 0.0236(15) O4C 0.0360(17) 0.0329(17) 0.0292(17) 0.0015(13) 0.0001(13) 0.0184(14) C1D 0.047(3) 0.036(3) 0.030(3) -0.003(2) -0.007(2) 0.022(2) C2D 0.041(3) 0.034(2) 0.042(3) -0.015(2) -0.014(2) 0.020(2) C3D 0.032(2) 0.039(3) 0.040(3) -0.016(2) -0.008(2) 0.020(2) C4D 0.030(2) 0.033(2) 0.041(3) -0.011(2) -0.004(2) 0.012(2) C5D 0.033(2) 0.032(2) 0.029(2) -0.0080(19) -0.001(2) 0.015(2) C6D 0.053(3) 0.045(3) 0.057(3) -0.013(3) -0.018(3) 0.029(3) C7D 0.048(3) 0.049(3) 0.076(4) -0.016(3) -0.023(3) 0.032(3) C8D 0.038(3) 0.060(4) 0.080(4) -0.041(4) -0.019(3) 0.028(3) C9D 0.036(3) 0.042(3) 0.053(3) -0.021(3) -0.007(2) 0.018(2) C10D 0.033(3) 0.050(3) 0.053(3) -0.015(3) 0.007(2) 0.012(2) C11D 0.043(3) 0.049(3) 0.051(3) -0.008(3) 0.004(3) 0.012(2) C12D 0.037(3) 0.043(3) 0.038(3) -0.008(2) -0.004(2) 0.010(2) C13D 0.032(2) 0.037(3) 0.028(2) -0.006(2) 0.0029(19) 0.017(2) C14D 0.044(3) 0.053(3) 0.040(3) -0.020(2) -0.003(2) 0.026(3) C15D 0.032(2) 0.029(2) 0.025(2) 0.0005(18) 0.0057(18) 0.014(2) N1D 0.034(2) 0.030(2) 0.033(2) -0.0040(16) -0.0011(16) 0.0152(17) O1D 0.057(2) 0.051(2) 0.041(2) 0.0040(18) -0.0054(18) 0.0270(19) O2D 0.0378(18) 0.0400(18) 0.041(2) 0.0001(15) -0.0063(15) 0.0211(16) O3D 0.0311(17) 0.0403(17) 0.0299(17) -0.0067(14) -0.0003(13) 0.0219(14) O4D 0.0333(16) 0.0343(16) 0.0259(16) -0.0032(13) 0.0020(13) 0.0193(14) C21 0.043(3) 0.074(4) 0.053(3) 0.007(3) 0.011(3) 0.042(3) C22 0.050(3) 0.058(4) 0.084(5) -0.004(3) 0.005(3) 0.025(3) C23 0.058(4) 0.082(4) 0.046(3) -0.011(3) -0.006(3) 0.047(3) C24 0.061(4) 0.073(4) 0.053(4) 0.001(3) -0.009(3) 0.051(3) O5 0.0383(17) 0.055(2) 0.043(2) -0.0035(17) -0.0011(16) 0.0324(16) C25A 0.066(4) 0.101(5) 0.035(3) -0.023(3) -0.005(3) 0.058(4) C26A 0.097(5) 0.093(5) 0.049(4) 0.023(3) 0.037(4) 0.071(5) C27A 0.049(5) 0.056(5) 0.118(8) 0.004(5) 0.030(5) 0.028(4) C28A 0.029(2) 0.060(3) 0.056(3) -0.003(3) -0.001(2) 0.018(2) O6A 0.0330(16) 0.0428(17) 0.0311(17) -0.0015(13) 0.0026(13) 0.0232(14) C25B 0.066(4) 0.101(5) 0.035(3) -0.023(3) -0.005(3) 0.058(4) C26B 0.097(5) 0.093(5) 0.049(4) 0.023(3) 0.037(4) 0.071(5) C27B 0.049(5) 0.056(5) 0.118(8) 0.004(5) 0.030(5) 0.028(4) C28B 0.029(2) 0.060(3) 0.056(3) -0.003(3) -0.001(2) 0.018(2) O6B 0.0330(16) 0.0428(17) 0.0311(17) -0.0015(13) 0.0026(13) 0.0232(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3A 1.945(3) . ? Cu1 O3C 1.949(3) . ? Cu1 O3B 1.972(3) . ? Cu1 O3D 1.992(3) . ? Cu1 O5 2.219(3) . ? Cu1 Cu2 2.6018(6) . ? Cu2 O4D 1.933(3) . ? Cu2 O4B 1.936(3) . ? Cu2 O4A 1.960(3) . ? Cu2 O4C 1.961(3) . ? Cu2 O6A 2.203(3) . ? C1A O1A 1.210(7) . ? C1A N1A 1.414(7) . ? C1A C2A 1.475(8) . ? C2A C3A 1.376(8) . ? C2A C6A 1.380(7) . ? C3A C4A 1.403(7) . ? C3A C9A 1.432(8) . ? C4A C12A 1.370(8) . ? C4A C5A 1.484(7) . ? C5A O2A 1.226(6) . ? C5A N1A 1.380(7) . ? C6A C7A 1.394(9) . ? C6A H6A 0.9500 . ? C7A C8A 1.335(9) . ? C7A H7A 0.9500 . ? C8A C9A 1.410(8) . ? C8A H8A 0.9500 . ? C9A C10A 1.409(9) . ? C10A C11A 1.354(9) . ? C10A H10A 0.9500 . ? C11A C12A 1.422(8) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A N1A 1.477(6) . ? C13A C15A 1.517(7) . ? C13A C14A 1.535(7) . ? C13A H13A 1.0000 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A O3A 1.243(6) . ? C15A O4A 1.257(5) . ? C1B O1B 1.202(7) . ? C1B N1B 1.393(6) . ? C1B C2B 1.487(8) . ? C2B C6B 1.363(8) . ? C2B C3B 1.409(9) . ? C3B C4B 1.392(8) . ? C3B C9B 1.420(8) . ? C4B C12B 1.358(9) . ? C4B C5B 1.480(7) . ? C5B O2B 1.208(6) . ? C5B N1B 1.405(7) . ? C6B C7B 1.404(9) . ? C6B H6B 0.9500 . ? C7B C8B 1.341(11) . ? C7B H7B 0.9500 . ? C8B C9B 1.413(10) . ? C8B H8B 0.9500 . ? C9B C10B 1.429(11) . ? C10B C11B 1.381(11) . ? C10B H10B 0.9500 . ? C11B C12B 1.410(9) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B N1B 1.482(6) . ? C13B C14B 1.526(7) . ? C13B C15B 1.538(6) . ? C13B H13B 1.0000 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B O4B 1.253(5) . ? C15B O3B 1.254(5) . ? C1C O1C 1.225(6) . ? C1C N1C 1.383(6) . ? C1C C2C 1.473(7) . ? C2C C6C 1.382(7) . ? C2C C3C 1.410(7) . ? C3C C4C 1.417(7) . ? C3C C9C 1.419(7) . ? C4C C12C 1.368(7) . ? C4C C5C 1.471(7) . ? C5C O2C 1.201(6) . ? C5C N1C 1.399(6) . ? C6C C7C 1.386(9) . ? C6C H6C 0.9500 . ? C7C C8C 1.377(10) . ? C7C H7C 0.9500 . ? C8C C9C 1.410(8) . ? C8C H8C 0.9500 . ? C9C C10C 1.419(9) . ? C10C C11C 1.347(8) . ? C10C H10C 0.9500 . ? C11C C12C 1.399(7) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C C14C 1.505(7) . ? C13C N1C 1.506(6) . ? C13C C15C 1.519(7) . ? C13C H13C 1.0000 . ? C14C H14I 0.9800 . ? C14C H14G 0.9800 . ? C14C H14H 0.9800 . ? C15C O4C 1.252(6) . ? C15C O3C 1.263(6) . ? C1D O1D 1.200(6) . ? C1D N1D 1.404(6) . ? C1D C2D 1.490(7) . ? C2D C6D 1.373(7) . ? C2D C3D 1.408(8) . ? C3D C4D 1.410(7) . ? C3D C9D 1.422(7) . ? C4D C12D 1.392(7) . ? C4D C5D 1.465(6) . ? C5D O2D 1.219(6) . ? C5D N1D 1.396(6) . ? C6D C7D 1.401(9) . ? C6D H6D 0.9500 . ? C7D C8D 1.380(10) . ? C7D H7D 0.9500 . ? C8D C9D 1.406(8) . ? C8D H8D 0.9500 . ? C9D C10D 1.415(9) . ? C10D C11D 1.365(8) . ? C10D H10D 0.9500 . ? C11D C12D 1.405(8) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D N1D 1.457(6) . ? C13D C15D 1.519(6) . ? C13D C14D 1.529(7) . ? C13D H13D 1.0000 . ? C14D H14K 0.9800 . ? C14D H14J 0.9800 . ? C14D H14L 0.9800 . ? C15D O4D 1.252(5) . ? C15D O3D 1.264(5) . ? C21 O5 1.430(7) . ? C21 C22 1.510(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.516(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.507(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O5 1.440(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25A O6A 1.447(6) . ? C25A C26A 1.501(10) . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? C26A C27A 1.525(13) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? C27A C28A 1.491(12) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? C28A O6A 1.455(6) . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? C31 O31 1.390(12) . ? C31 C32 1.586(17) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.523(15) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.453(14) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O31 1.350(12) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C41 O41 1.434(13) . ? C41 C42 1.484(11) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.366(11) . ? C42 H42B 0.9900 . ? C42 H42A 0.9900 . ? C43 C44 1.518(12) . ? C43 H43B 0.9900 . ? C43 H43A 0.9900 . ? C44 O41 1.488(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C51 O51 1.460(18) . ? C51 C52 1.541(18) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.370(18) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.553(18) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 O51 1.438(17) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 O52 1.436(19) . ? C55 C56 1.540(19) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.357(19) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.539(19) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 O52 1.48(2) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C61 C62 1.549(10) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.513(10) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.595(10) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.514(10) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.524(10) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C71 C72 1.4200 . ? C71 O71 1.4200 . ? C72 C73 1.4200 . ? C73 C74 1.4200 . ? C74 O71 1.4200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3A Cu1 O3C 172.88(13) . . ? O3A Cu1 O3B 89.59(14) . . ? O3C Cu1 O3B 88.77(14) . . ? O3A Cu1 O3D 89.75(13) . . ? O3C Cu1 O3D 90.13(13) . . ? O3B Cu1 O3D 165.62(12) . . ? O3A Cu1 O5 91.43(13) . . ? O3C Cu1 O5 95.52(13) . . ? O3B Cu1 O5 90.67(13) . . ? O3D Cu1 O5 103.71(12) . . ? O3A Cu1 Cu2 83.49(9) . . ? O3C Cu1 Cu2 89.41(9) . . ? O3B Cu1 Cu2 81.11(9) . . ? O3D Cu1 Cu2 84.54(8) . . ? O5 Cu1 Cu2 170.34(9) . . ? O4D Cu2 O4B 173.45(12) . . ? O4D Cu2 O4A 88.80(13) . . ? O4B Cu2 O4A 90.10(13) . . ? O4D Cu2 O4C 88.69(13) . . ? O4B Cu2 O4C 90.81(13) . . ? O4A Cu2 O4C 165.88(13) . . ? O4D Cu2 O6A 89.66(12) . . ? O4B Cu2 O6A 96.89(12) . . ? O4A Cu2 O6A 101.23(12) . . ? O4C Cu2 O6A 92.64(12) . . ? O4D Cu2 Cu1 85.03(9) . . ? O4B Cu2 Cu1 88.45(9) . . ? O4A Cu2 Cu1 85.98(9) . . ? O4C Cu2 Cu1 79.96(9) . . ? O6A Cu2 Cu1 170.97(9) . . ? O1A C1A N1A 120.0(5) . . ? O1A C1A C2A 124.5(5) . . ? N1A C1A C2A 115.5(5) . . ? C3A C2A C6A 120.1(5) . . ? C3A C2A C1A 121.2(5) . . ? C6A C2A C1A 118.8(5) . . ? C2A C3A C4A 121.9(5) . . ? C2A C3A C9A 120.0(5) . . ? C4A C3A C9A 118.1(5) . . ? C12A C4A C3A 121.9(5) . . ? C12A C4A C5A 119.2(5) . . ? C3A C4A C5A 118.9(5) . . ? O2A C5A N1A 120.4(5) . . ? O2A C5A C4A 122.2(5) . . ? N1A C5A C4A 117.4(4) . . ? C2A C6A C7A 120.0(6) . . ? C2A C6A H6A 120.0 . . ? C7A C6A H6A 120.0 . . ? C8A C7A C6A 121.1(5) . . ? C8A C7A H7A 119.4 . . ? C6A C7A H7A 119.4 . . ? C7A C8A C9A 121.1(6) . . ? C7A C8A H8A 119.4 . . ? C9A C8A H8A 119.4 . . ? C10A C9A C8A 124.0(5) . . ? C10A C9A C3A 118.4(5) . . ? C8A C9A C3A 117.6(6) . . ? C11A C10A C9A 122.6(6) . . ? C11A C10A H10A 118.7 . . ? C9A C10A H10A 118.7 . . ? C10A C11A C12A 119.0(6) . . ? C10A C11A H11A 120.5 . . ? C12A C11A H11A 120.5 . . ? C4A C12A C11A 119.9(5) . . ? C4A C12A H12A 120.0 . . ? C11A C12A H12A 120.0 . . ? N1A C13A C15A 110.5(4) . . ? N1A C13A C14A 112.2(4) . . ? C15A C13A C14A 114.4(4) . . ? N1A C13A H13A 106.4 . . ? C15A C13A H13A 106.4 . . ? C14A C13A H13A 106.4 . . ? C13A C14A H14A 109.5 . . ? C13A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C13A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? O3A C15A O4A 127.7(4) . . ? O3A C15A C13A 117.1(4) . . ? O4A C15A C13A 115.2(4) . . ? C5A N1A C1A 125.1(4) . . ? C5A N1A C13A 116.4(4) . . ? C1A N1A C13A 118.4(4) . . ? C15A O3A Cu1 123.3(3) . . ? C15A O4A Cu2 119.4(3) . . ? O1B C1B N1B 120.7(5) . . ? O1B C1B C2B 123.0(5) . . ? N1B C1B C2B 116.3(5) . . ? C6B C2B C3B 120.5(5) . . ? C6B C2B C1B 119.8(6) . . ? C3B C2B C1B 119.7(5) . . ? C4B C3B C2B 121.5(5) . . ? C4B C3B C9B 119.4(6) . . ? C2B C3B C9B 119.2(6) . . ? C12B C4B C3B 120.4(5) . . ? C12B C4B C5B 119.0(5) . . ? C3B C4B C5B 120.6(5) . . ? O2B C5B N1B 120.7(5) . . ? O2B C5B C4B 123.6(5) . . ? N1B C5B C4B 115.8(5) . . ? C2B C6B C7B 119.8(7) . . ? C2B C6B H6B 120.1 . . ? C7B C6B H6B 120.1 . . ? C8B C7B C6B 121.2(7) . . ? C8B C7B H7B 119.4 . . ? C6B C7B H7B 119.4 . . ? C7B C8B C9B 120.9(6) . . ? C7B C8B H8B 119.5 . . ? C9B C8B H8B 119.5 . . ? C8B C9B C3B 118.3(7) . . ? C8B C9B C10B 123.9(7) . . ? C3B C9B C10B 117.8(6) . . ? C11B C10B C9B 122.8(6) . . ? C11B C10B H10B 118.6 . . ? C9B C10B H10B 118.6 . . ? C10B C11B C12B 116.1(7) . . ? C10B C11B H11B 121.9 . . ? C12B C11B H11B 121.9 . . ? C4B C12B C11B 123.5(7) . . ? C4B C12B H12B 118.3 . . ? C11B C12B H12B 118.3 . . ? N1B C13B C14B 111.7(4) . . ? N1B C13B C15B 109.3(4) . . ? C14B C13B C15B 114.4(4) . . ? N1B C13B H13B 107.0 . . ? C14B C13B H13B 107.0 . . ? C15B C13B H13B 107.0 . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? O4B C15B O3B 127.2(4) . . ? O4B C15B C13B 115.5(4) . . ? O3B C15B C13B 117.2(4) . . ? C1B N1B C5B 125.9(4) . . ? C1B N1B C13B 117.3(4) . . ? C5B N1B C13B 116.8(4) . . ? C15B O3B Cu1 124.8(3) . . ? C15B O4B Cu2 118.2(3) . . ? O1C C1C N1C 121.2(5) . . ? O1C C1C C2C 122.5(4) . . ? N1C C1C C2C 116.3(4) . . ? C6C C2C C3C 119.9(5) . . ? C6C C2C C1C 119.8(5) . . ? C3C C2C C1C 120.3(4) . . ? C2C C3C C4C 120.7(5) . . ? C2C C3C C9C 120.2(5) . . ? C4C C3C C9C 119.1(5) . . ? C12C C4C C3C 119.8(5) . . ? C12C C4C C5C 120.3(5) . . ? C3C C4C C5C 119.9(5) . . ? O2C C5C N1C 120.3(4) . . ? O2C C5C C4C 123.3(5) . . ? N1C C5C C4C 116.3(4) . . ? C2C C6C C7C 120.0(6) . . ? C2C C6C H6C 120.0 . . ? C7C C6C H6C 120.0 . . ? C8C C7C C6C 121.3(6) . . ? C8C C7C H7C 119.4 . . ? C6C C7C H7C 119.4 . . ? C7C C8C C9C 120.4(6) . . ? C7C C8C H8C 119.8 . . ? C9C C8C H8C 119.8 . . ? C8C C9C C3C 118.2(6) . . ? C8C C9C C10C 123.2(5) . . ? C3C C9C C10C 118.6(5) . . ? C11C C10C C9C 121.0(5) . . ? C11C C10C H10C 119.5 . . ? C9C C10C H10C 119.5 . . ? C10C C11C C12C 120.5(5) . . ? C10C C11C H11C 119.8 . . ? C12C C11C H11C 119.8 . . ? C4C C12C C11C 121.0(5) . . ? C4C C12C H12C 119.5 . . ? C11C C12C H12C 119.5 . . ? C14C C13C N1C 113.5(4) . . ? C14C C13C C15C 116.4(4) . . ? N1C C13C C15C 107.4(4) . . ? C14C C13C H13C 106.3 . . ? N1C C13C H13C 106.3 . . ? C15C C13C H13C 106.3 . . ? C13C C14C H14I 109.5 . . ? C13C C14C H14G 109.5 . . ? H14I C14C H14G 109.5 . . ? C13C C14C H14H 109.5 . . ? H14I C14C H14H 109.5 . . ? H14G C14C H14H 109.5 . . ? O4C C15C O3C 125.9(4) . . ? O4C C15C C13C 116.6(4) . . ? O3C C15C C13C 117.4(4) . . ? C1C N1C C5C 126.2(4) . . ? C1C N1C C13C 118.0(4) . . ? C5C N1C C13C 115.7(4) . . ? C15C O3C Cu1 117.0(3) . . ? C15C O4C Cu2 127.5(3) . . ? O1D C1D N1D 121.0(5) . . ? O1D C1D C2D 122.3(5) . . ? N1D C1D C2D 116.7(4) . . ? C6D C2D C3D 119.6(5) . . ? C6D C2D C1D 120.1(5) . . ? C3D C2D C1D 120.3(4) . . ? C2D C3D C4D 120.5(4) . . ? C2D C3D C9D 120.5(5) . . ? C4D C3D C9D 118.9(5) . . ? C12D C4D C3D 120.5(4) . . ? C12D C4D C5D 119.3(5) . . ? C3D C4D C5D 120.2(5) . . ? O2D C5D N1D 119.2(4) . . ? O2D C5D C4D 122.7(4) . . ? N1D C5D C4D 118.1(4) . . ? C2D C6D C7D 121.0(6) . . ? C2D C6D H6D 119.5 . . ? C7D C6D H6D 119.5 . . ? C8D C7D C6D 119.7(5) . . ? C8D C7D H7D 120.2 . . ? C6D C7D H7D 120.2 . . ? C7D C8D C9D 121.5(5) . . ? C7D C8D H8D 119.3 . . ? C9D C8D H8D 119.3 . . ? C8D C9D C10D 123.1(5) . . ? C8D C9D C3D 117.7(6) . . ? C10D C9D C3D 119.2(5) . . ? C11D C10D C9D 120.8(5) . . ? C11D C10D H10D 119.6 . . ? C9D C10D H10D 119.6 . . ? C10D C11D C12D 120.6(6) . . ? C10D C11D H11D 119.7 . . ? C12D C11D H11D 119.7 . . ? C4D C12D C11D 119.9(5) . . ? C4D C12D H12D 120.1 . . ? C11D C12D H12D 120.1 . . ? N1D C13D C15D 108.3(4) . . ? N1D C13D C14D 112.4(4) . . ? C15D C13D C14D 115.7(4) . . ? N1D C13D H13D 106.7 . . ? C15D C13D H13D 106.7 . . ? C14D C13D H13D 106.7 . . ? C13D C14D H14K 109.5 . . ? C13D C14D H14J 109.5 . . ? H14K C14D H14J 109.5 . . ? C13D C14D H14L 109.5 . . ? H14K C14D H14L 109.5 . . ? H14J C14D H14L 109.5 . . ? O4D C15D O3D 126.4(4) . . ? O4D C15D C13D 113.9(4) . . ? O3D C15D C13D 119.6(4) . . ? C5D N1D C1D 124.1(4) . . ? C5D N1D C13D 117.0(4) . . ? C1D N1D C13D 118.5(4) . . ? C15D O3D Cu1 120.5(3) . . ? C15D O4D Cu2 123.2(3) . . ? O5 C21 C22 104.1(4) . . ? O5 C21 H21A 110.9 . . ? C22 C21 H21A 110.9 . . ? O5 C21 H21B 110.9 . . ? C22 C21 H21B 110.9 . . ? H21A C21 H21B 108.9 . . ? C21 C22 C23 103.5(5) . . ? C21 C22 H22A 111.1 . . ? C23 C22 H22A 111.1 . . ? C21 C22 H22B 111.1 . . ? C23 C22 H22B 111.1 . . ? H22A C22 H22B 109.0 . . ? C24 C23 C22 104.0(5) . . ? C24 C23 H23A 111.0 . . ? C22 C23 H23A 111.0 . . ? C24 C23 H23B 111.0 . . ? C22 C23 H23B 111.0 . . ? H23A C23 H23B 109.0 . . ? O5 C24 C23 107.9(5) . . ? O5 C24 H24A 110.1 . . ? C23 C24 H24A 110.1 . . ? O5 C24 H24B 110.1 . . ? C23 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? C21 O5 C24 105.6(4) . . ? C21 O5 Cu1 119.4(3) . . ? C24 O5 Cu1 115.3(3) . . ? O6A C25A C26A 107.3(5) . . ? O6A C25A H25A 110.3 . . ? C26A C25A H25A 110.3 . . ? O6A C25A H25B 110.3 . . ? C26A C25A H25B 110.3 . . ? H25A C25A H25B 108.5 . . ? C25A C26A C27A 103.1(8) . . ? C25A C26A H26A 111.1 . . ? C27A C26A H26A 111.1 . . ? C25A C26A H26B 111.1 . . ? C27A C26A H26B 111.1 . . ? H26A C26A H26B 109.1 . . ? C28A C27A C26A 103.2(9) . . ? C28A C27A H27A 111.1 . . ? C26A C27A H27A 111.1 . . ? C28A C27A H27B 111.1 . . ? C26A C27A H27B 111.1 . . ? H27A C27A H27B 109.1 . . ? O6A C28A C27A 106.8(8) . . ? O6A C28A H28A 110.4 . . ? C27A C28A H28A 110.4 . . ? O6A C28A H28B 110.4 . . ? C27A C28A H28B 110.4 . . ? H28A C28A H28B 108.6 . . ? C25A O6A C28A 108.5(4) . . ? C25A O6A Cu2 119.3(3) . . ? C28A O6A Cu2 117.0(3) . . ? H27C C27B H27D 109.0 . . ? O31 C31 C32 104.5(10) . . ? O31 C31 H31A 110.9 . . ? C32 C31 H31A 110.9 . . ? O31 C31 H31B 110.9 . . ? C32 C31 H31B 110.9 . . ? H31A C31 H31B 108.9 . . ? C33 C32 C31 98.9(9) . . ? C33 C32 H32A 112.0 . . ? C31 C32 H32A 112.0 . . ? C33 C32 H32B 112.0 . . ? C31 C32 H32B 112.0 . . ? H32A C32 H32B 109.7 . . ? C34 C33 C32 105.6(10) . . ? C34 C33 H33A 110.6 . . ? C32 C33 H33A 110.6 . . ? C34 C33 H33B 110.6 . . ? C32 C33 H33B 110.6 . . ? H33A C33 H33B 108.7 . . ? O31 C34 C33 109.4(10) . . ? O31 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? O31 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? C34 O31 C31 105.0(9) . . ? O41 C41 C42 105.2(9) . . ? O41 C41 H41A 110.7 . . ? C42 C41 H41A 110.7 . . ? O41 C41 H41B 110.7 . . ? C42 C41 H41B 110.7 . . ? H41A C41 H41B 108.8 . . ? C43 C42 C41 103.0(10) . . ? C43 C42 H42B 111.2 . . ? C41 C42 H42B 111.2 . . ? C43 C42 H42A 111.2 . . ? C41 C42 H42A 111.2 . . ? H42B C42 H42A 109.1 . . ? C42 C43 C44 110.8(10) . . ? C42 C43 H43B 109.5 . . ? C44 C43 H43B 109.5 . . ? C42 C43 H43A 109.5 . . ? C44 C43 H43A 109.5 . . ? H43B C43 H43A 108.1 . . ? O41 C44 C43 101.9(9) . . ? O41 C44 H44A 111.4 . . ? C43 C44 H44A 111.4 . . ? O41 C44 H44B 111.4 . . ? C43 C44 H44B 111.4 . . ? H44A C44 H44B 109.3 . . ? C41 O41 C44 103.2(9) . . ? O51 C51 C52 97.1(14) . . ? O51 C51 H51A 112.3 . . ? C52 C51 H51A 112.3 . . ? O51 C51 H51B 112.3 . . ? C52 C51 H51B 112.3 . . ? H51A C51 H51B 109.9 . . ? C53 C52 C51 99.1(16) . . ? C53 C52 H52A 111.9 . . ? C51 C52 H52A 111.9 . . ? C53 C52 H52B 111.9 . . ? C51 C52 H52B 111.9 . . ? H52A C52 H52B 109.6 . . ? C52 C53 C54 97.7(15) . . ? C52 C53 H53A 112.2 . . ? C54 C53 H53A 112.2 . . ? C52 C53 H53B 112.2 . . ? C54 C53 H53B 112.2 . . ? H53A C53 H53B 109.8 . . ? O51 C54 C53 107.2(14) . . ? O51 C54 H54A 110.3 . . ? C53 C54 H54A 110.3 . . ? O51 C54 H54B 110.3 . . ? C53 C54 H54B 110.3 . . ? H54A C54 H54B 108.5 . . ? C54 O51 C51 101.8(13) . . ? O52 C55 C56 93.5(16) . . ? O52 C55 H55A 113.0 . . ? C56 C55 H55A 113.0 . . ? O52 C55 H55B 113.0 . . ? C56 C55 H55B 113.0 . . ? H55A C55 H55B 110.4 . . ? C57 C56 C55 100.3(18) . . ? C57 C56 H56A 111.7 . . ? C55 C56 H56A 111.7 . . ? C57 C56 H56B 111.7 . . ? C55 C56 H56B 111.7 . . ? H56A C56 H56B 109.5 . . ? C56 C57 C58 104.7(18) . . ? C56 C57 H57A 110.8 . . ? C58 C57 H57A 110.8 . . ? C56 C57 H57B 110.8 . . ? C58 C57 H57B 110.8 . . ? H57A C57 H57B 108.9 . . ? O52 C58 C57 100.9(15) . . ? O52 C58 H58A 111.6 . . ? C57 C58 H58A 111.6 . . ? O52 C58 H58B 111.6 . . ? C57 C58 H58B 111.6 . . ? H58A C58 H58B 109.4 . . ? C55 O52 C58 101.7(16) . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C63 C62 C61 111.9(9) . . ? C63 C62 H62A 109.2 . . ? C61 C62 H62A 109.2 . . ? C63 C62 H62B 109.2 . . ? C61 C62 H62B 109.2 . . ? H62A C62 H62B 107.9 . . ? C62 C63 C64 107.9(8) . . ? C62 C63 H63A 110.1 . . ? C64 C63 H63A 110.1 . . ? C62 C63 H63B 110.1 . . ? C64 C63 H63B 110.1 . . ? H63A C63 H63B 108.4 . . ? C65 C64 C63 110.0(9) . . ? C65 C64 H64A 109.7 . . ? C63 C64 H64A 109.7 . . ? C65 C64 H64B 109.7 . . ? C63 C64 H64B 109.7 . . ? H64A C64 H64B 108.2 . . ? C64 C65 C66 113.7(10) . . ? C64 C65 H65A 108.8 . . ? C66 C65 H65A 108.8 . . ? C64 C65 H65B 108.8 . . ? C66 C65 H65B 108.8 . . ? H65A C65 H65B 107.7 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C72 C71 O71 108.0 . . ? C73 C72 C71 108.0 . . ? C72 C73 C74 108.0 . . ? O71 C74 C73 108.0 . . ? C74 O71 C71 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3A Cu1 Cu2 O4D -90.39(13) . . . . ? O3C Cu1 Cu2 O4D 90.16(13) . . . . ? O3B Cu1 Cu2 O4D 179.00(14) . . . . ? O3D Cu1 Cu2 O4D -0.02(13) . . . . ? O3A Cu1 Cu2 O4B 88.96(14) . . . . ? O3C Cu1 Cu2 O4B -90.49(13) . . . . ? O3B Cu1 Cu2 O4B -1.65(14) . . . . ? O3D Cu1 Cu2 O4B 179.33(14) . . . . ? O3A Cu1 Cu2 O4A -1.25(13) . . . . ? O3C Cu1 Cu2 O4A 179.30(14) . . . . ? O3B Cu1 Cu2 O4A -91.85(14) . . . . ? O3D Cu1 Cu2 O4A 89.12(13) . . . . ? O3A Cu1 Cu2 O4C -179.94(14) . . . . ? O3C Cu1 Cu2 O4C 0.61(13) . . . . ? O3B Cu1 Cu2 O4C 89.45(13) . . . . ? O3D Cu1 Cu2 O4C -89.57(13) . . . . ? O1A C1A C2A C3A -179.3(5) . . . . ? N1A C1A C2A C3A 2.0(7) . . . . ? O1A C1A C2A C6A 0.6(8) . . . . ? N1A C1A C2A C6A -178.0(5) . . . . ? C6A C2A C3A C4A 178.5(5) . . . . ? C1A C2A C3A C4A -1.6(7) . . . . ? C6A C2A C3A C9A 1.0(8) . . . . ? C1A C2A C3A C9A -179.1(5) . . . . ? C2A C3A C4A C12A -180.0(5) . . . . ? C9A C3A C4A C12A -2.4(7) . . . . ? C2A C3A C4A C5A -0.8(7) . . . . ? C9A C3A C4A C5A 176.8(4) . . . . ? C12A C4A C5A O2A 1.8(7) . . . . ? C3A C4A C5A O2A -177.4(4) . . . . ? C12A C4A C5A N1A -178.2(4) . . . . ? C3A C4A C5A N1A 2.5(7) . . . . ? C3A C2A C6A C7A -0.4(8) . . . . ? C1A C2A C6A C7A 179.6(5) . . . . ? C2A C6A C7A C8A 1.2(9) . . . . ? C6A C7A C8A C9A -2.5(9) . . . . ? C7A C8A C9A C10A 179.9(6) . . . . ? C7A C8A C9A C3A 3.0(9) . . . . ? C2A C3A C9A C10A -179.3(5) . . . . ? C4A C3A C9A C10A 3.1(7) . . . . ? C2A C3A C9A C8A -2.2(8) . . . . ? C4A C3A C9A C8A -179.8(5) . . . . ? C8A C9A C10A C11A -179.4(6) . . . . ? C3A C9A C10A C11A -2.6(9) . . . . ? C9A C10A C11A C12A 1.1(9) . . . . ? C3A C4A C12A C11A 1.0(8) . . . . ? C5A C4A C12A C11A -178.2(5) . . . . ? C10A C11A C12A C4A -0.3(8) . . . . ? N1A C13A C15A O3A -137.6(4) . . . . ? C14A C13A C15A O3A -9.8(6) . . . . ? N1A C13A C15A O4A 45.0(6) . . . . ? C14A C13A C15A O4A 172.9(4) . . . . ? O2A C5A N1A C1A 177.9(4) . . . . ? C4A C5A N1A C1A -2.1(7) . . . . ? O2A C5A N1A C13A -1.6(6) . . . . ? C4A C5A N1A C13A 178.5(4) . . . . ? O1A C1A N1A C5A -178.9(5) . . . . ? C2A C1A N1A C5A -0.1(7) . . . . ? O1A C1A N1A C13A 0.6(7) . . . . ? C2A C1A N1A C13A 179.3(4) . . . . ? C15A C13A N1A C5A 51.8(5) . . . . ? C14A C13A N1A C5A -77.2(5) . . . . ? C15A C13A N1A C1A -127.7(4) . . . . ? C14A C13A N1A C1A 103.3(5) . . . . ? O4A C15A O3A Cu1 -5.5(7) . . . . ? C13A C15A O3A Cu1 177.5(3) . . . . ? O3B Cu1 O3A C15A 84.6(4) . . . . ? O3D Cu1 O3A C15A -81.0(4) . . . . ? O5 Cu1 O3A C15A 175.3(4) . . . . ? Cu2 Cu1 O3A C15A 3.5(3) . . . . ? O3A C15A O4A Cu2 3.6(6) . . . . ? C13A C15A O4A Cu2 -179.3(3) . . . . ? O4D Cu2 O4A C15A 84.6(3) . . . . ? O4B Cu2 O4A C15A -89.0(3) . . . . ? O4C Cu2 O4A C15A 4.8(7) . . . . ? O6A Cu2 O4A C15A 174.0(3) . . . . ? Cu1 Cu2 O4A C15A -0.5(3) . . . . ? O1B C1B C2B C6B -4.6(8) . . . . ? N1B C1B C2B C6B 176.7(5) . . . . ? O1B C1B C2B C3B 174.5(5) . . . . ? N1B C1B C2B C3B -4.3(7) . . . . ? C6B C2B C3B C4B -178.4(5) . . . . ? C1B C2B C3B C4B 2.6(8) . . . . ? C6B C2B C3B C9B 1.1(8) . . . . ? C1B C2B C3B C9B -178.0(5) . . . . ? C2B C3B C4B C12B -178.0(5) . . . . ? C9B C3B C4B C12B 2.6(8) . . . . ? C2B C3B C4B C5B 2.1(8) . . . . ? C9B C3B C4B C5B -177.4(5) . . . . ? C12B C4B C5B O2B -6.2(8) . . . . ? C3B C4B C5B O2B 173.7(5) . . . . ? C12B C4B C5B N1B 175.3(5) . . . . ? C3B C4B C5B N1B -4.8(7) . . . . ? C3B C2B C6B C7B 0.1(8) . . . . ? C1B C2B C6B C7B 179.2(5) . . . . ? C2B C6B C7B C8B -1.2(10) . . . . ? C6B C7B C8B C9B 1.0(11) . . . . ? C7B C8B C9B C3B 0.2(9) . . . . ? C7B C8B C9B C10B -179.6(6) . . . . ? C4B C3B C9B C8B 178.2(5) . . . . ? C2B C3B C9B C8B -1.3(8) . . . . ? C4B C3B C9B C10B -1.9(8) . . . . ? C2B C3B C9B C10B 178.6(5) . . . . ? C8B C9B C10B C11B 179.2(6) . . . . ? C3B C9B C10B C11B -0.7(9) . . . . ? C9B C10B C11B C12B 2.5(10) . . . . ? C3B C4B C12B C11B -0.6(9) . . . . ? C5B C4B C12B C11B 179.3(5) . . . . ? C10B C11B C12B C4B -1.9(9) . . . . ? N1B C13B C15B O4B 40.2(5) . . . . ? C14B C13B C15B O4B 166.3(4) . . . . ? N1B C13B C15B O3B -142.2(4) . . . . ? C14B C13B C15B O3B -16.1(6) . . . . ? O1B C1B N1B C5B -177.4(5) . . . . ? C2B C1B N1B C5B 1.4(7) . . . . ? O1B C1B N1B C13B 5.4(7) . . . . ? C2B C1B N1B C13B -175.8(4) . . . . ? O2B C5B N1B C1B -175.6(5) . . . . ? C4B C5B N1B C1B 3.0(7) . . . . ? O2B C5B N1B C13B 1.7(6) . . . . ? C4B C5B N1B C13B -179.8(4) . . . . ? C14B C13B N1B C1B 99.9(5) . . . . ? C15B C13B N1B C1B -132.5(4) . . . . ? C14B C13B N1B C5B -77.6(5) . . . . ? C15B C13B N1B C5B 50.0(5) . . . . ? O4B C15B O3B Cu1 -5.8(7) . . . . ? C13B C15B O3B Cu1 176.9(3) . . . . ? O3A Cu1 O3B C15B -79.4(4) . . . . ? O3C Cu1 O3B C15B 93.7(4) . . . . ? O3D Cu1 O3B C15B 8.0(8) . . . . ? O5 Cu1 O3B C15B -170.8(4) . . . . ? Cu2 Cu1 O3B C15B 4.1(4) . . . . ? O3B C15B O4B Cu2 3.3(6) . . . . ? C13B C15B O4B Cu2 -179.4(3) . . . . ? O4A Cu2 O4B C15B 85.9(3) . . . . ? O4C Cu2 O4B C15B -80.0(3) . . . . ? O6A Cu2 O4B C15B -172.8(3) . . . . ? Cu1 Cu2 O4B C15B -0.1(3) . . . . ? O1C C1C C2C C6C 4.3(7) . . . . ? N1C C1C C2C C6C -174.8(4) . . . . ? O1C C1C C2C C3C -177.1(5) . . . . ? N1C C1C C2C C3C 3.8(6) . . . . ? C6C C2C C3C C4C 178.5(4) . . . . ? C1C C2C C3C C4C -0.1(7) . . . . ? C6C C2C C3C C9C -1.1(7) . . . . ? C1C C2C C3C C9C -179.7(4) . . . . ? C2C C3C C4C C12C 179.7(4) . . . . ? C9C C3C C4C C12C -0.7(7) . . . . ? C2C C3C C4C C5C -1.0(7) . . . . ? C9C C3C C4C C5C 178.6(4) . . . . ? C12C C4C C5C O2C -2.1(7) . . . . ? C3C C4C C5C O2C 178.6(4) . . . . ? C12C C4C C5C N1C 177.8(4) . . . . ? C3C C4C C5C N1C -1.5(6) . . . . ? C3C C2C C6C C7C 0.2(7) . . . . ? C1C C2C C6C C7C 178.8(5) . . . . ? C2C C6C C7C C8C 0.8(8) . . . . ? C6C C7C C8C C9C -0.9(9) . . . . ? C7C C8C C9C C3C 0.0(8) . . . . ? C7C C8C C9C C10C 179.7(5) . . . . ? C2C C3C C9C C8C 1.0(7) . . . . ? C4C C3C C9C C8C -178.6(5) . . . . ? C2C C3C C9C C10C -178.7(4) . . . . ? C4C C3C C9C C10C 1.7(7) . . . . ? C8C C9C C10C C11C 179.2(5) . . . . ? C3C C9C C10C C11C -1.1(8) . . . . ? C9C C10C C11C C12C -0.5(8) . . . . ? C3C C4C C12C C11C -1.0(7) . . . . ? C5C C4C C12C C11C 179.8(4) . . . . ? C10C C11C C12C C4C 1.6(8) . . . . ? C14C C13C C15C O4C 161.4(4) . . . . ? N1C C13C C15C O4C 32.9(5) . . . . ? C14C C13C C15C O3C -20.4(6) . . . . ? N1C C13C C15C O3C -148.9(4) . . . . ? O1C C1C N1C C5C 174.1(4) . . . . ? C2C C1C N1C C5C -6.8(7) . . . . ? O1C C1C N1C C13C -10.9(7) . . . . ? C2C C1C N1C C13C 168.2(4) . . . . ? O2C C5C N1C C1C -174.4(4) . . . . ? C4C C5C N1C C1C 5.7(6) . . . . ? O2C C5C N1C C13C 10.5(6) . . . . ? C4C C5C N1C C13C -169.4(4) . . . . ? C14C C13C N1C C1C 104.6(5) . . . . ? C15C C13C N1C C1C -125.3(4) . . . . ? C14C C13C N1C C5C -79.9(5) . . . . ? C15C C13C N1C C5C 50.3(5) . . . . ? O4C C15C O3C Cu1 -4.8(6) . . . . ? C13C C15C O3C Cu1 177.2(3) . . . . ? O3B Cu1 O3C C15C -79.5(3) . . . . ? O3D Cu1 O3C C15C 86.2(3) . . . . ? O5 Cu1 O3C C15C -170.0(3) . . . . ? Cu2 Cu1 O3C C15C 1.6(3) . . . . ? O3C C15C O4C Cu2 6.2(7) . . . . ? C13C C15C O4C Cu2 -175.8(3) . . . . ? O4D Cu2 O4C C15C -88.6(4) . . . . ? O4B Cu2 O4C C15C 84.9(4) . . . . ? O4A Cu2 O4C C15C -8.8(8) . . . . ? O6A Cu2 O4C C15C -178.2(4) . . . . ? Cu1 Cu2 O4C C15C -3.4(3) . . . . ? O1D C1D C2D C6D 0.4(7) . . . . ? N1D C1D C2D C6D -178.1(4) . . . . ? O1D C1D C2D C3D -179.1(5) . . . . ? N1D C1D C2D C3D 2.3(6) . . . . ? C6D C2D C3D C4D 179.1(4) . . . . ? C1D C2D C3D C4D -1.4(7) . . . . ? C6D C2D C3D C9D 0.9(7) . . . . ? C1D C2D C3D C9D -179.6(4) . . . . ? C2D C3D C4D C12D -179.9(5) . . . . ? C9D C3D C4D C12D -1.7(7) . . . . ? C2D C3D C4D C5D -0.4(7) . . . . ? C9D C3D C4D C5D 177.8(4) . . . . ? C12D C4D C5D O2D 1.8(7) . . . . ? C3D C4D C5D O2D -177.7(4) . . . . ? C12D C4D C5D N1D -179.2(4) . . . . ? C3D C4D C5D N1D 1.2(6) . . . . ? C3D C2D C6D C7D -0.9(8) . . . . ? C1D C2D C6D C7D 179.6(5) . . . . ? C2D C6D C7D C8D 0.4(8) . . . . ? C6D C7D C8D C9D 0.1(8) . . . . ? C7D C8D C9D C10D -179.8(5) . . . . ? C7D C8D C9D C3D -0.1(7) . . . . ? C2D C3D C9D C8D -0.4(7) . . . . ? C4D C3D C9D C8D -178.6(4) . . . . ? C2D C3D C9D C10D 179.4(5) . . . . ? C4D C3D C9D C10D 1.1(7) . . . . ? C8D C9D C10D C11D -179.6(5) . . . . ? C3D C9D C10D C11D 0.6(8) . . . . ? C9D C10D C11D C12D -1.9(8) . . . . ? C3D C4D C12D C11D 0.5(7) . . . . ? C5D C4D C12D C11D -179.0(4) . . . . ? C10D C11D C12D C4D 1.3(8) . . . . ? N1D C13D C15D O4D 41.1(5) . . . . ? C14D C13D C15D O4D 168.2(4) . . . . ? N1D C13D C15D O3D -141.8(4) . . . . ? C14D C13D C15D O3D -14.7(6) . . . . ? O2D C5D N1D C1D 178.8(4) . . . . ? C4D C5D N1D C1D -0.2(6) . . . . ? O2D C5D N1D C13D 5.9(6) . . . . ? C4D C5D N1D C13D -173.1(4) . . . . ? O1D C1D N1D C5D 179.9(4) . . . . ? C2D C1D N1D C5D -1.5(6) . . . . ? O1D C1D N1D C13D -7.3(7) . . . . ? C2D C1D N1D C13D 171.3(4) . . . . ? C15D C13D N1D C5D 53.8(5) . . . . ? C14D C13D N1D C5D -75.2(5) . . . . ? C15D C13D N1D C1D -119.5(4) . . . . ? C14D C13D N1D C1D 111.5(5) . . . . ? O4D C15D O3D Cu1 -6.8(6) . . . . ? C13D C15D O3D Cu1 176.5(3) . . . . ? O3A Cu1 O3D C15D 86.6(3) . . . . ? O3C Cu1 O3D C15D -86.3(3) . . . . ? O3B Cu1 O3D C15D -0.8(7) . . . . ? O5 Cu1 O3D C15D 178.0(3) . . . . ? Cu2 Cu1 O3D C15D 3.1(3) . . . . ? O3D C15D O4D Cu2 7.0(6) . . . . ? C13D C15D O4D Cu2 -176.2(3) . . . . ? O4A Cu2 O4D C15D -89.2(3) . . . . ? O4C Cu2 O4D C15D 76.9(3) . . . . ? O6A Cu2 O4D C15D 169.5(3) . . . . ? Cu1 Cu2 O4D C15D -3.2(3) . . . . ? O5 C21 C22 C23 -36.0(6) . . . . ? C21 C22 C23 C24 19.6(6) . . . . ? C22 C23 C24 O5 3.1(6) . . . . ? C22 C21 O5 C24 38.6(5) . . . . ? C22 C21 O5 Cu1 -93.2(4) . . . . ? C23 C24 O5 C21 -26.1(5) . . . . ? C23 C24 O5 Cu1 107.9(4) . . . . ? O3A Cu1 O5 C21 -0.8(4) . . . . ? O3C Cu1 O5 C21 177.6(4) . . . . ? O3B Cu1 O5 C21 88.8(4) . . . . ? O3D Cu1 O5 C21 -90.9(4) . . . . ? O3A Cu1 O5 C24 -128.2(4) . . . . ? O3C Cu1 O5 C24 50.2(4) . . . . ? O3B Cu1 O5 C24 -38.6(4) . . . . ? O3D Cu1 O5 C24 141.7(3) . . . . ? O6A C25A C26A C27A 25.5(11) . . . . ? C25A C26A C27A C28A -32.9(16) . . . . ? C26A C27A C28A O6A 29.0(16) . . . . ? C26A C25A O6A C28A -8.0(6) . . . . ? C26A C25A O6A Cu2 129.6(4) . . . . ? C27A C28A O6A C25A -13.6(11) . . . . ? C27A C28A O6A Cu2 -152.2(10) . . . . ? O4D Cu2 O6A C25A -169.6(4) . . . . ? O4B Cu2 O6A C25A 10.2(4) . . . . ? O4A Cu2 O6A C25A 101.7(4) . . . . ? O4C Cu2 O6A C25A -80.9(4) . . . . ? O4D Cu2 O6A C28A -35.5(3) . . . . ? O4B Cu2 O6A C28A 144.3(3) . . . . ? O4A Cu2 O6A C28A -124.2(3) . . . . ? O4C Cu2 O6A C28A 53.2(3) . . . . ? O31 C31 C32 C33 -29.0(11) . . . . ? C31 C32 C33 C34 7.4(12) . . . . ? C32 C33 C34 O31 17.3(13) . . . . ? C33 C34 O31 C31 -37.7(12) . . . . ? C32 C31 O31 C34 41.4(11) . . . . ? O41 C41 C42 C43 37.1(14) . . . . ? C41 C42 C43 C44 -19.2(14) . . . . ? C42 C43 C44 O41 -4.3(14) . . . . ? C42 C41 O41 C44 -39.8(12) . . . . ? C43 C44 O41 C41 26.8(12) . . . . ? C61 C62 C63 C64 -168.1(12) . . . . ? C62 C63 C64 C65 -173.9(12) . . . . ? C63 C64 C65 C66 -176.2(12) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.773 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.080 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C75 H51 Cu2 N5 O20, 5.0(C H2 Cl2), 0.73 (H2 O)' _chemical_formula_sum 'C80.02 H51 Cl10.03 Cu2 N5 O20.73' _chemical_formula_weight 1896.97 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.6310(10) _cell_length_b 16.2439(11) _cell_length_c 32.635(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8286.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5805 _cell_measurement_theta_min 2.197 _cell_measurement_theta_max 18.820 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3842 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Rapid decomposition when removed from mother liquor ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82477 _diffrn_reflns_av_R_equivalents 0.1427 _diffrn_reflns_av_sigmaI/netI 0.1339 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 23.30 _reflns_number_total 11942 _reflns_number_gt 6819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; 45 distance restraints used to model heavily disordered CH2Cl2 solvent. Isolated electron density peak modeled as water oxygen. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 11942 _refine_ls_number_parameters 1082 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.1205 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1912 _refine_ls_wR_factor_gt 0.1714 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.64072(7) 0.22178(8) 0.55329(3) 0.0395(3) Uani 1 1 d . . . Cu2 Cu 0.51617(7) 0.21064(8) 0.60656(3) 0.0389(3) Uani 1 1 d . . . C1A C 0.3887(7) 0.4217(6) 0.5398(3) 0.040(3) Uani 1 1 d . . . C2A C 0.3290(8) 0.4718(6) 0.5666(3) 0.051(3) Uani 1 1 d . . . C3A C 0.2447(7) 0.4459(6) 0.5692(3) 0.044(3) Uani 1 1 d . . . C4A C 0.2120(6) 0.3786(6) 0.5474(3) 0.039(2) Uani 1 1 d . . . C5A C 0.2630(6) 0.3338(7) 0.5187(3) 0.040(3) Uani 1 1 d . . . C6A C 0.3617(9) 0.5380(6) 0.5874(3) 0.056(3) Uani 1 1 d . . . H6A H 0.4206 0.5519 0.5856 0.067 Uiso 1 1 calc R . . C7A C 0.3070(10) 0.5832(7) 0.6108(4) 0.070(4) Uani 1 1 d . . . H7A H 0.3277 0.6320 0.6234 0.084 Uiso 1 1 calc R . . C8A C 0.2221(9) 0.5612(8) 0.6170(4) 0.067(4) Uani 1 1 d . . . H8A H 0.1867 0.5932 0.6344 0.081 Uiso 1 1 calc R . . C9A C 0.1876(8) 0.4886(7) 0.5965(3) 0.047(3) Uani 1 1 d . . . C10A C 0.1032(9) 0.4621(9) 0.6021(4) 0.072(4) Uani 1 1 d . . . H10A H 0.0667 0.4917 0.6201 0.087 Uiso 1 1 calc R . . C11A C 0.0726(8) 0.3953(9) 0.5822(3) 0.072(4) Uani 1 1 d . . . H11A H 0.0158 0.3765 0.5868 0.086 Uiso 1 1 calc R . . C12A C 0.1285(7) 0.3529(8) 0.5537(3) 0.064(3) Uani 1 1 d . . . H12A H 0.1075 0.3066 0.5391 0.076 Uiso 1 1 calc R . . C13A C 0.4107(6) 0.3031(6) 0.4943(3) 0.040(3) Uani 1 1 d . . . H13A H 0.3775 0.2532 0.4861 0.048 Uiso 1 1 calc R . . C14A C 0.4430(7) 0.3427(7) 0.4543(3) 0.054(3) Uani 1 1 d . . . H14A H 0.3944 0.3525 0.4359 0.080 Uiso 1 1 calc R . . H14B H 0.4838 0.3056 0.4409 0.080 Uiso 1 1 calc R . . H14C H 0.4711 0.3951 0.4605 0.080 Uiso 1 1 calc R . . C15A C 0.4806(7) 0.2726(5) 0.5247(3) 0.036(2) Uani 1 1 d . . . N1A N 0.3509(5) 0.3558(5) 0.5175(2) 0.042(2) Uani 1 1 d . . . O1A O 0.4643(5) 0.4331(4) 0.5370(2) 0.0482(19) Uani 1 1 d . . . O2A O 0.2388(4) 0.2800(4) 0.49618(19) 0.0434(17) Uani 1 1 d . . . O3A O 0.5560(4) 0.2661(4) 0.51350(17) 0.0376(17) Uani 1 1 d . . . O4A O 0.4490(4) 0.2522(4) 0.55962(18) 0.0400(17) Uani 1 1 d . . . C1B C 0.3851(7) 0.0205(6) 0.5242(3) 0.038(3) Uani 1 1 d . . . C2B C 0.2908(6) 0.0051(6) 0.5249(3) 0.035(2) Uani 1 1 d . . . C3B C 0.2605(7) -0.0658(6) 0.5433(3) 0.041(3) Uani 1 1 d . . . C4B C 0.3188(8) -0.1213(7) 0.5631(3) 0.048(3) Uani 1 1 d . . . C5B C 0.4079(7) -0.1045(6) 0.5657(3) 0.036(2) Uani 1 1 d . . . C6B C 0.2357(7) 0.0607(7) 0.5077(3) 0.044(3) Uani 1 1 d . . . H6B H 0.2572 0.1105 0.4964 0.053 Uiso 1 1 calc R . . C7B C 0.1505(8) 0.0450(7) 0.5066(3) 0.046(3) Uani 1 1 d . . . H7B H 0.1129 0.0836 0.4942 0.055 Uiso 1 1 calc R . . C8B C 0.1181(8) -0.0258(8) 0.5231(3) 0.059(3) Uani 1 1 d . . . H8B H 0.0585 -0.0365 0.5213 0.070 Uiso 1 1 calc R . . C9B C 0.1714(7) -0.0825(7) 0.5425(3) 0.052(3) Uani 1 1 d . . . C10B C 0.1424(9) -0.1594(8) 0.5607(4) 0.084(4) Uani 1 1 d . . . H10B H 0.0834 -0.1734 0.5601 0.101 Uiso 1 1 calc R . . C11B C 0.1973(9) -0.2091(8) 0.5777(4) 0.089(4) Uani 1 1 d . . . H11B H 0.1768 -0.2582 0.5901 0.106 Uiso 1 1 calc R . . C12B C 0.2860(8) -0.1927(7) 0.5785(4) 0.070(4) Uani 1 1 d . . . H12B H 0.3237 -0.2322 0.5901 0.083 Uiso 1 1 calc R . . C13B C 0.5297(7) -0.0162(7) 0.5457(3) 0.050(3) Uani 1 1 d . . . H13B H 0.5548 -0.0514 0.5677 0.061 Uiso 1 1 calc R . . C14B C 0.5734(8) -0.0409(7) 0.5052(4) 0.074(4) Uani 1 1 d . . . H14D H 0.5741 -0.1010 0.5028 0.110 Uiso 1 1 calc R . . H14E H 0.6323 -0.0200 0.5049 0.110 Uiso 1 1 calc R . . H14F H 0.5417 -0.0173 0.4821 0.110 Uiso 1 1 calc R . . C15B C 0.5457(6) 0.0730(6) 0.5577(3) 0.040(3) Uani 1 1 d . . . N1B N 0.4361(5) -0.0330(5) 0.5449(2) 0.036(2) Uani 1 1 d . . . O1B O 0.4161(5) 0.0799(4) 0.5059(2) 0.0508(19) Uani 1 1 d . . . O2B O 0.4592(5) -0.1468(4) 0.5846(2) 0.0517(19) Uani 1 1 d . . . O3B O 0.6075(4) 0.1095(4) 0.54144(19) 0.0440(18) Uani 1 1 d . . . O4B O 0.4978(4) 0.1000(4) 0.5869(2) 0.0416(17) Uani 1 1 d . . . C1C C 0.6743(7) -0.0069(8) 0.6655(4) 0.060(3) Uani 1 1 d . . . C2C C 0.6357(8) -0.0751(7) 0.6871(4) 0.057(3) Uani 1 1 d . . . C3C C 0.6317(7) -0.0728(8) 0.7308(4) 0.054(3) Uani 1 1 d . . . C4C C 0.6589(7) -0.0047(9) 0.7519(4) 0.068(4) Uani 1 1 d . . . C5C C 0.6958(10) 0.0640(10) 0.7308(4) 0.087(5) Uani 1 1 d . . . C6C C 0.6092(8) -0.1437(8) 0.6681(4) 0.069(4) Uani 1 1 d . . . H6C H 0.6134 -0.1451 0.6391 0.083 Uiso 1 1 calc R . . C7C C 0.5756(10) -0.2141(9) 0.6878(5) 0.100(5) Uani 1 1 d . . . H7C H 0.5600 -0.2620 0.6729 0.120 Uiso 1 1 calc R . . C8C C 0.5664(10) -0.2099(9) 0.7299(5) 0.094(5) Uani 1 1 d . . . H8C H 0.5408 -0.2545 0.7442 0.112 Uiso 1 1 calc R . . C9C C 0.5946(8) -0.1401(8) 0.7518(4) 0.063(3) Uani 1 1 d . . . C10C C 0.5901(9) -0.1342(9) 0.7955(5) 0.075(4) Uani 1 1 d . . . H10C H 0.5685 -0.1797 0.8106 0.090 Uiso 1 1 calc R . . C11C C 0.6149(10) -0.0682(11) 0.8154(4) 0.087(5) Uani 1 1 d . . . H11C H 0.6075 -0.0648 0.8442 0.104 Uiso 1 1 calc R . . C12C C 0.6529(10) -0.0018(9) 0.7937(4) 0.093(5) Uani 1 1 d . . . H12C H 0.6742 0.0446 0.8082 0.111 Uiso 1 1 calc R . . C13C C 0.7396(8) 0.1291(8) 0.6651(4) 0.074(4) Uani 1 1 d . . . H13C H 0.7450 0.1750 0.6853 0.089 Uiso 1 1 calc R . . C14C C 0.8294(8) 0.1102(10) 0.6505(4) 0.099(6) Uani 1 1 d . . . H14G H 0.8650 0.0946 0.6740 0.148 Uiso 1 1 calc R . . H14H H 0.8537 0.1592 0.6373 0.148 Uiso 1 1 calc R . . H14I H 0.8277 0.0648 0.6308 0.148 Uiso 1 1 calc R . . C15C C 0.6794(9) 0.1588(8) 0.6329(4) 0.062(4) Uani 1 1 d . . . N1C N 0.7016(6) 0.0585(6) 0.6877(3) 0.063(3) Uani 1 1 d . . . O1C O 0.6794(5) -0.0041(5) 0.6273(2) 0.071(2) Uani 1 1 d . . . O2C O 0.7228(9) 0.1252(8) 0.7472(3) 0.139(5) Uani 1 1 d . . . O3C O 0.7112(5) 0.1807(5) 0.5984(2) 0.059(2) Uani 1 1 d . . . O4C O 0.6024(5) 0.1666(5) 0.6429(2) 0.056(2) Uani 1 1 d . . . C1D C 0.6619(8) 0.3872(11) 0.6883(4) 0.074(5) Uani 1 1 d . . . C2D C 0.6519(10) 0.3872(12) 0.7321(4) 0.095(6) Uani 1 1 d . . . C3D C 0.6068(10) 0.4475(14) 0.7509(4) 0.097(6) Uani 1 1 d . . . C4D C 0.5689(9) 0.5176(11) 0.7283(4) 0.076(4) Uani 1 1 d . . . C5D C 0.5781(11) 0.5162(12) 0.6814(5) 0.095(6) Uani 1 1 d . . . C6D C 0.6849(10) 0.3245(15) 0.7561(4) 0.134(8) Uani 1 1 d . . . H6D H 0.7157 0.2803 0.7441 0.161 Uiso 1 1 calc R . . C7D C 0.6719(11) 0.3278(14) 0.7980(5) 0.134(8) Uani 1 1 d . . . H7D H 0.6942 0.2841 0.8141 0.160 Uiso 1 1 calc R . . C8D C 0.6320(12) 0.3854(17) 0.8165(5) 0.135(9) Uani 1 1 d . . . H8D H 0.6270 0.3833 0.8455 0.162 Uiso 1 1 calc R . . C9D C 0.5971(10) 0.4487(13) 0.7961(4) 0.093(6) Uani 1 1 d . . . C10D C 0.5511(10) 0.5210(14) 0.8116(4) 0.103(7) Uani 1 1 d . . . H10D H 0.5416 0.5241 0.8403 0.123 Uiso 1 1 calc R . . C11D C 0.5212(13) 0.5832(11) 0.7886(5) 0.114(7) Uani 1 1 d . . . H11D H 0.4961 0.6298 0.8014 0.137 Uiso 1 1 calc R . . C12D C 0.5268(11) 0.5799(9) 0.7458(4) 0.103(6) Uani 1 1 d . . . H12D H 0.5010 0.6214 0.7294 0.123 Uiso 1 1 calc R . . C13D C 0.6296(7) 0.4442(7) 0.6198(3) 0.057(3) Uani 1 1 d . . . H13D H 0.5823 0.4791 0.6087 0.068 Uiso 1 1 calc R . . C14D C 0.7099(10) 0.4844(11) 0.6057(4) 0.112(6) Uani 1 1 d . . . H14J H 0.7063 0.5438 0.6106 0.167 Uiso 1 1 calc R . . H14K H 0.7177 0.4742 0.5764 0.167 Uiso 1 1 calc R . . H14L H 0.7586 0.4616 0.6209 0.167 Uiso 1 1 calc R . . C15D C 0.6106(7) 0.3594(7) 0.6052(3) 0.049(3) Uani 1 1 d . . . N1D N 0.6199(7) 0.4481(7) 0.6650(3) 0.060(3) Uani 1 1 d . . . O1D O 0.7064(5) 0.3352(6) 0.6704(2) 0.081(3) Uani 1 1 d . . . O2D O 0.5474(8) 0.5684(7) 0.6593(3) 0.103(4) Uani 1 1 d . . . O3D O 0.6562(4) 0.3321(4) 0.57522(19) 0.0457(18) Uani 1 1 d . . . O4D O 0.5483(4) 0.3226(4) 0.62054(18) 0.0470(19) Uani 1 1 d . . . C1E C 0.2170(7) 0.2693(7) 0.6813(3) 0.053(3) Uani 1 1 d . . . C2E C 0.1892(7) 0.3110(8) 0.7194(3) 0.056(3) Uani 1 1 d . . . C3E C 0.1946(6) 0.2684(7) 0.7572(3) 0.043(3) Uani 1 1 d . . . C4E C 0.2193(7) 0.1849(7) 0.7583(3) 0.045(3) Uani 1 1 d . . . C5E C 0.2335(7) 0.1408(7) 0.7200(3) 0.041(3) Uani 1 1 d . . . C6E C 0.1628(8) 0.3921(8) 0.7185(4) 0.077(4) Uani 1 1 d . . . H6E H 0.1605 0.4209 0.6932 0.092 Uiso 1 1 calc R . . C7E C 0.1393(9) 0.4316(9) 0.7548(5) 0.082(4) Uani 1 1 d . . . H7E H 0.1198 0.4870 0.7539 0.099 Uiso 1 1 calc R . . C8E C 0.1444(8) 0.3893(9) 0.7937(5) 0.083(4) Uani 1 1 d . . . H8E H 0.1287 0.4159 0.8185 0.099 Uiso 1 1 calc R . . C9E C 0.1721(8) 0.3114(9) 0.7934(4) 0.066(4) Uani 1 1 d . . . C10E C 0.1802(9) 0.2720(11) 0.8308(4) 0.083(4) Uani 1 1 d . . . H10E H 0.1680 0.3001 0.8556 0.100 Uiso 1 1 calc R . . C11E C 0.2066(9) 0.1901(11) 0.8311(4) 0.087(5) Uani 1 1 d . . . H11E H 0.2131 0.1633 0.8568 0.105 Uiso 1 1 calc R . . C12E C 0.2237(8) 0.1459(9) 0.7958(4) 0.074(4) Uani 1 1 d . . . H12E H 0.2384 0.0892 0.7973 0.088 Uiso 1 1 calc R . . C13E C 0.2458(7) 0.1434(7) 0.6452(3) 0.052(3) Uani 1 1 d . . . H13E H 0.2623 0.0857 0.6523 0.063 Uiso 1 1 calc R . . C14E C 0.1638(7) 0.1369(8) 0.6200(3) 0.065(4) Uani 1 1 d . . . H14M H 0.1206 0.1066 0.6357 0.098 Uiso 1 1 calc R . . H14N H 0.1756 0.1077 0.5944 0.098 Uiso 1 1 calc R . . H14O H 0.1424 0.1923 0.6139 0.098 Uiso 1 1 calc R . . C15E C 0.3224(8) 0.1800(6) 0.6220(3) 0.043(3) Uani 1 1 d . . . N1E N 0.2335(5) 0.1862(5) 0.6841(3) 0.048(2) Uani 1 1 d . . . O1E O 0.2210(5) 0.3045(4) 0.6478(2) 0.063(2) Uani 1 1 d . . . O2E O 0.2452(5) 0.0672(5) 0.7190(2) 0.055(2) Uani 1 1 d . . . O3E O 0.3085(4) 0.1837(5) 0.58218(19) 0.057(2) Uani 1 1 d . . . H3E H 0.3561 0.2024 0.5737 0.085 Uiso 1 1 d R . . O4E O 0.3869(5) 0.2019(4) 0.63854(19) 0.0453(18) Uani 1 1 d . . . C1SA C 0.3114(15) 0.5458(19) 0.4353(6) 0.097(2) Uiso 0.469(8) 1 d PD A 1 Cl1A Cl 0.4064(6) 0.5623(6) 0.4070(3) 0.097(2) Uiso 0.469(8) 1 d PD A 1 Cl1B Cl 0.3185(6) 0.5868(6) 0.4831(3) 0.097(2) Uiso 0.469(8) 1 d PD A 1 C1SB C 0.2913(17) 0.581(3) 0.4455(10) 0.097(2) Uiso 0.329(7) 1 d PD B 2 Cl1C Cl 0.3940(8) 0.5886(8) 0.4255(4) 0.097(2) Uiso 0.329(7) 1 d PD B 2 Cl1D Cl 0.2819(8) 0.6381(9) 0.4905(4) 0.097(2) Uiso 0.329(7) 1 d PD B 2 C2SA C 0.395(2) 0.1551(12) 0.3239(16) 0.121(2) Uiso 0.406(9) 1 d PD C 3 Cl2A Cl 0.4171 0.0492 0.3234 0.121(2) Uiso 0.406(9) 1 d PD C 3 Cl2B Cl 0.4863(8) 0.2088(7) 0.3087(5) 0.121(2) Uiso 0.406(9) 1 d PD C 3 C2SB C 0.402(6) 0.1457(16) 0.3321(13) 0.121(2) Uiso 0.270(8) 1 d PD D 4 Cl2C Cl 0.4105(13) 0.0405(11) 0.3209(6) 0.121(2) Uiso 0.270(8) 1 d PD D 4 Cl2D Cl 0.4340(14) 0.1998(10) 0.2881(6) 0.121(2) Uiso 0.270(8) 1 d PD D 4 C2SC C 0.392(4) 0.170(4) 0.344(3) 0.121(2) Uiso 0.194(7) 1 d PD E 5 Cl2E Cl 0.4099(18) 0.0869(17) 0.3101(9) 0.121(2) Uiso 0.194(7) 1 d PD E 5 Cl2F Cl 0.4848(16) 0.2304(15) 0.3400(9) 0.121(2) Uiso 0.194(7) 1 d PD E 5 C2SD C 0.379(5) 0.176(2) 0.297(2) 0.121(2) Uiso 0.224(6) 1 d PD F 6 Cl2G Cl 0.3727(14) 0.0751(13) 0.2784(7) 0.121(2) Uiso 0.224(6) 1 d PD F 6 Cl2H Cl 0.4556(16) 0.1751(15) 0.3371(7) 0.121(2) Uiso 0.224(6) 1 d PD F 6 C3SA C 0.530(2) 0.397(5) 0.2235(10) 0.122(2) Uiso 0.210(6) 1 d PD G 7 Cl3A Cl 0.5147(15) 0.3714(15) 0.2749(6) 0.122(2) Uiso 0.210(6) 1 d PD G 7 Cl3B Cl 0.4284(17) 0.3976(15) 0.2014(7) 0.122(2) Uiso 0.210(6) 1 d PD G 7 C3SB C 0.4137(15) 0.0413(11) 0.2138(5) 0.122(2) Uiso 0.728(8) 1 d PD H 8 Cl3C Cl 0.4660(4) -0.0575(4) 0.2132(2) 0.122(2) Uiso 0.728(8) 1 d PD H 8 Cl3D Cl 0.4138(4) 0.0805(4) 0.1637(2) 0.122(2) Uiso 0.728(8) 1 d PD H 8 C4SA C 0.4767(14) 0.2986(19) 0.1949(6) 0.111(2) Uiso 0.499(8) 1 d PD I 9 Cl4A Cl 0.3750(6) 0.3228(6) 0.2119(3) 0.111(2) Uiso 0.499(8) 1 d PD I 9 Cl4B Cl 0.4828(6) 0.3251(5) 0.1425(3) 0.111(2) Uiso 0.499(8) 1 d PD I 9 C4SB C 0.369(2) 0.277(4) 0.2242(19) 0.111(2) Uiso 0.202(5) 1 d PD J 10 Cl4C Cl 0.3847(13) 0.2097(13) 0.1830(6) 0.111(2) Uiso 0.202(5) 1 d PD J 10 Cl4D Cl 0.4652(14) 0.3290(12) 0.2326(7) 0.111(2) Uiso 0.202(5) 1 d PD J 10 C4SC C 0.474(9) 0.299(3) 0.1685(15) 0.111(2) Uiso 0.122(7) 1 d PD K 11 Cl4E Cl 0.486(3) 0.397(2) 0.1908(10) 0.111(2) Uiso 0.122(7) 1 d PD K 11 Cl4F Cl 0.492(3) 0.313(2) 0.1153(11) 0.111(2) Uiso 0.122(7) 1 d PD K 11 C5SA C 1.0650(14) 0.799(2) 0.4234(7) 0.1091(18) Uiso 0.469(7) 1 d PD L 12 Cl5A Cl 1.1644(5) 0.7594(5) 0.4372(3) 0.1091(18) Uiso 0.469(7) 1 d PD L 12 Cl5B Cl 0.9968(6) 0.8185(6) 0.4640(3) 0.1091(18) Uiso 0.469(7) 1 d PD L 12 C5SB C 0.868(2) 0.686(2) 0.5464(17) 0.1091(18) Uiso 0.273(6) 1 d PD M 13 Cl5C Cl 0.8896(11) 0.5869(10) 0.5654(5) 0.1091(18) Uiso 0.273(6) 1 d PD M 13 Cl5D Cl 0.9577(10) 0.7306(9) 0.5221(5) 0.1091(18) Uiso 0.273(6) 1 d PD M 13 C5SC C 0.917(2) 0.7122(19) 0.5586(13) 0.1091(18) Uiso 0.305(6) 1 d PD N 14 Cl5E Cl 0.8536(9) 0.6274(10) 0.5544(5) 0.1091(18) Uiso 0.305(6) 1 d PD N 14 Cl5F Cl 0.9968(9) 0.6888(9) 0.5935(5) 0.1091(18) Uiso 0.305(6) 1 d PD N 14 C5SD C 1.0841(17) 0.795(3) 0.4598(9) 0.1091(18) Uiso 0.316(7) 1 d PD O 15 Cl5G Cl 1.0815(9) 0.8440(9) 0.4129(4) 0.1091(18) Uiso 0.316(7) 1 d PD O 15 Cl5H Cl 0.9811(9) 0.7994(9) 0.4812(4) 0.1091(18) Uiso 0.316(7) 1 d PD O 15 O1S O 0.3589(10) 0.1517(9) 0.4263(4) 0.112(7) Uiso 0.73(3) 1 d P P 16 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0330(6) 0.0594(8) 0.0261(6) 0.0075(6) 0.0002(5) -0.0033(7) Cu2 0.0401(7) 0.0525(7) 0.0243(6) 0.0035(6) 0.0010(5) -0.0072(7) C1A 0.046(7) 0.041(6) 0.032(6) 0.012(5) -0.002(5) 0.006(6) C2A 0.065(9) 0.029(6) 0.058(8) 0.012(5) 0.013(6) 0.011(6) C3A 0.042(7) 0.045(7) 0.046(7) 0.008(6) -0.011(5) 0.020(6) C4A 0.035(6) 0.057(7) 0.024(6) 0.007(5) 0.001(5) 0.002(5) C5A 0.028(6) 0.065(8) 0.027(6) 0.016(6) -0.006(5) 0.006(6) C6A 0.085(9) 0.043(7) 0.040(7) -0.006(6) -0.008(7) 0.002(7) C7A 0.125(13) 0.025(6) 0.060(8) -0.013(6) -0.008(9) 0.011(8) C8A 0.076(10) 0.070(9) 0.056(8) -0.003(7) 0.009(7) 0.027(8) C9A 0.056(8) 0.059(8) 0.027(6) 0.002(5) -0.009(5) 0.022(7) C10A 0.068(9) 0.117(12) 0.032(7) 0.000(8) 0.013(7) 0.031(9) C11A 0.056(8) 0.131(13) 0.028(7) -0.027(8) 0.017(6) 0.009(8) C12A 0.044(8) 0.100(10) 0.046(7) 0.005(7) -0.013(6) 0.005(7) C13A 0.033(6) 0.063(8) 0.024(5) -0.001(5) 0.002(4) 0.006(5) C14A 0.052(7) 0.081(8) 0.028(6) 0.011(6) 0.003(5) -0.009(6) C15A 0.048(7) 0.018(5) 0.041(6) -0.009(5) -0.005(5) -0.002(5) N1A 0.039(5) 0.057(6) 0.029(5) 0.004(4) -0.003(4) 0.003(5) O1A 0.035(5) 0.056(5) 0.053(5) 0.000(4) 0.001(4) -0.006(4) O2A 0.031(4) 0.061(5) 0.039(4) -0.010(4) -0.004(3) -0.004(4) O3A 0.020(4) 0.060(5) 0.033(4) 0.006(3) 0.001(3) 0.004(3) O4A 0.037(4) 0.052(4) 0.031(4) 0.007(3) 0.002(3) -0.012(3) C1B 0.054(7) 0.033(6) 0.028(6) 0.004(5) -0.009(5) 0.003(6) C2B 0.041(6) 0.042(7) 0.023(5) -0.013(5) 0.003(5) 0.000(5) C3B 0.048(7) 0.038(6) 0.037(6) -0.008(5) -0.001(5) 0.001(6) C4B 0.061(8) 0.042(7) 0.040(7) 0.002(5) -0.002(5) -0.004(6) C5B 0.046(7) 0.029(6) 0.034(6) -0.004(5) -0.002(5) 0.005(5) C6B 0.046(7) 0.066(8) 0.021(5) -0.007(5) 0.000(5) 0.009(6) C7B 0.063(8) 0.049(7) 0.025(6) 0.001(5) -0.008(5) 0.005(6) C8B 0.053(8) 0.073(9) 0.049(7) -0.012(7) -0.012(6) 0.001(7) C9B 0.043(7) 0.050(7) 0.062(8) -0.010(6) -0.004(6) -0.009(6) C10B 0.065(9) 0.072(9) 0.116(12) 0.028(9) -0.002(9) -0.031(8) C11B 0.081(10) 0.058(9) 0.126(12) 0.044(9) -0.022(9) -0.011(9) C12B 0.067(9) 0.053(9) 0.089(10) 0.008(7) -0.012(7) -0.002(7) C13B 0.049(7) 0.057(7) 0.045(7) 0.005(6) 0.013(6) 0.006(6) C14B 0.087(10) 0.068(9) 0.066(9) -0.004(7) 0.016(7) 0.017(7) C15B 0.035(6) 0.043(7) 0.041(6) 0.013(5) -0.011(5) 0.007(5) N1B 0.043(5) 0.030(5) 0.036(5) -0.002(4) 0.003(4) 0.005(4) O1B 0.071(5) 0.049(5) 0.033(4) 0.005(4) 0.005(4) -0.008(4) O2B 0.057(5) 0.044(4) 0.055(5) 0.005(4) -0.010(4) 0.013(4) O3B 0.024(4) 0.065(5) 0.043(4) 0.014(4) 0.006(3) 0.004(4) O4B 0.041(4) 0.041(4) 0.043(4) 0.005(3) 0.008(4) 0.002(3) C1C 0.044(7) 0.074(9) 0.061(9) 0.026(8) 0.000(6) 0.005(7) C2C 0.062(8) 0.048(8) 0.063(8) 0.025(7) 0.000(7) 0.004(7) C3C 0.045(7) 0.060(8) 0.057(8) 0.029(7) 0.002(6) 0.006(6) C4C 0.049(8) 0.101(11) 0.054(8) 0.043(8) -0.002(6) -0.005(8) C5C 0.108(12) 0.096(12) 0.057(10) 0.029(9) -0.037(8) -0.051(10) C6C 0.077(9) 0.073(9) 0.058(8) 0.033(8) 0.017(7) -0.002(8) C7C 0.146(14) 0.070(10) 0.084(11) 0.008(9) 0.043(10) 0.004(10) C8C 0.135(13) 0.063(10) 0.083(11) 0.025(9) 0.033(9) 0.027(10) C9C 0.078(9) 0.054(8) 0.055(9) 0.018(7) 0.012(7) 0.008(7) C10C 0.076(10) 0.063(10) 0.086(12) 0.042(9) 0.018(8) 0.026(8) C11C 0.097(12) 0.110(13) 0.054(9) 0.030(10) 0.006(8) 0.035(11) C12C 0.140(14) 0.093(11) 0.045(8) 0.036(8) 0.003(9) 0.002(10) C13C 0.073(10) 0.077(9) 0.071(9) 0.033(7) -0.033(8) -0.022(8) C14C 0.044(9) 0.148(14) 0.104(11) 0.076(10) -0.028(8) -0.012(9) C15C 0.066(9) 0.077(9) 0.043(8) 0.019(6) -0.013(7) -0.045(8) N1C 0.055(7) 0.076(7) 0.056(7) 0.034(6) -0.023(5) -0.036(6) O1C 0.072(6) 0.105(7) 0.035(5) 0.018(5) -0.004(4) 0.014(5) O2C 0.231(14) 0.147(10) 0.039(6) 0.019(6) -0.058(7) -0.081(10) O3C 0.047(5) 0.075(5) 0.054(5) 0.017(4) -0.006(4) -0.002(4) O4C 0.053(5) 0.079(6) 0.038(4) 0.017(4) -0.004(4) -0.030(5) C1D 0.034(8) 0.140(14) 0.048(9) -0.047(9) 0.013(6) -0.039(8) C2D 0.064(10) 0.181(17) 0.039(8) -0.044(10) 0.010(8) -0.036(11) C3D 0.068(10) 0.172(18) 0.052(10) -0.065(12) 0.016(8) -0.070(11) C4D 0.071(10) 0.100(12) 0.058(10) -0.038(9) 0.031(8) -0.048(9) C5D 0.113(14) 0.104(14) 0.068(12) -0.044(10) 0.034(10) -0.083(12) C6D 0.091(12) 0.28(3) 0.033(9) -0.008(12) -0.016(8) 0.048(14) C7D 0.100(13) 0.25(3) 0.047(10) -0.033(12) -0.010(9) 0.043(14) C8D 0.097(14) 0.28(3) 0.027(9) 0.005(13) -0.007(9) 0.032(17) C9D 0.061(10) 0.164(17) 0.053(10) -0.049(11) 0.029(8) -0.068(11) C10D 0.092(12) 0.175(19) 0.042(9) -0.046(11) 0.035(9) -0.092(13) C11D 0.177(19) 0.099(13) 0.067(11) -0.042(10) 0.052(12) -0.072(13) C12D 0.165(16) 0.099(11) 0.045(8) -0.044(8) 0.054(9) -0.059(11) C13D 0.048(8) 0.085(9) 0.037(7) -0.018(6) 0.012(5) -0.024(7) C14D 0.124(13) 0.178(16) 0.033(7) -0.017(9) 0.019(8) -0.071(12) C15D 0.055(7) 0.070(8) 0.023(6) 0.007(6) 0.004(6) -0.012(6) N1D 0.070(8) 0.069(7) 0.041(6) -0.021(6) 0.019(5) -0.026(6) O1D 0.050(5) 0.146(9) 0.045(5) -0.026(5) -0.002(4) -0.017(6) O2D 0.166(12) 0.074(7) 0.068(7) -0.017(6) 0.046(7) -0.038(7) O3D 0.044(4) 0.071(5) 0.022(4) 0.000(3) 0.000(3) -0.012(4) O4D 0.050(5) 0.070(5) 0.022(4) 0.004(3) 0.004(3) -0.013(4) C1E 0.071(8) 0.047(8) 0.040(7) 0.008(6) -0.015(6) -0.012(7) C2E 0.042(7) 0.071(9) 0.055(8) -0.014(6) -0.018(6) 0.005(6) C3E 0.042(6) 0.055(8) 0.031(6) -0.002(6) 0.005(5) -0.005(6) C4E 0.053(7) 0.061(8) 0.022(6) 0.014(5) 0.018(5) 0.017(6) C5E 0.048(7) 0.029(6) 0.046(7) 0.013(5) -0.016(5) 0.008(5) C6E 0.090(11) 0.067(9) 0.073(9) -0.023(7) -0.026(8) 0.034(8) C7E 0.079(10) 0.078(10) 0.090(11) -0.031(9) -0.032(9) 0.036(8) C8E 0.055(8) 0.095(12) 0.098(12) -0.052(10) 0.008(8) 0.009(9) C9E 0.062(8) 0.079(10) 0.059(9) -0.012(8) 0.007(6) 0.014(7) C10E 0.091(10) 0.102(12) 0.057(9) -0.030(10) 0.021(7) -0.013(10) C11E 0.098(11) 0.141(15) 0.023(7) -0.001(8) 0.003(7) -0.030(10) C12E 0.060(9) 0.101(11) 0.059(9) -0.002(8) 0.006(7) 0.012(8) C13E 0.066(8) 0.061(8) 0.031(6) -0.018(6) 0.022(6) -0.014(6) C14E 0.051(8) 0.106(10) 0.039(7) -0.017(7) 0.003(5) -0.033(7) C15E 0.051(7) 0.040(7) 0.039(7) 0.002(5) 0.005(6) -0.011(6) N1E 0.051(6) 0.052(6) 0.043(6) 0.001(5) 0.016(4) -0.010(5) O1E 0.083(6) 0.052(5) 0.054(5) 0.004(4) -0.008(4) -0.008(4) O2E 0.058(5) 0.060(6) 0.045(5) 0.014(4) 0.012(4) 0.009(4) O3E 0.047(4) 0.097(6) 0.027(4) -0.002(4) 0.000(3) -0.015(4) O4E 0.052(5) 0.054(5) 0.030(4) 0.004(3) 0.001(3) -0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3B 1.936(7) . ? Cu1 O3D 1.944(7) . ? Cu1 O3C 1.956(7) . ? Cu1 O3A 1.989(6) . ? Cu1 O2A 2.227(6) 4_556 ? Cu1 Cu2 2.6165(15) . ? Cu2 O4B 1.930(6) . ? Cu2 O4C 1.932(8) . ? Cu2 O4D 1.941(7) . ? Cu2 O4A 1.976(6) . ? Cu2 O4E 2.278(7) . ? C1A O1A 1.199(11) . ? C1A N1A 1.424(13) . ? C1A C2A 1.514(14) . ? C2A C6A 1.372(15) . ? C2A C3A 1.386(15) . ? C3A C4A 1.403(14) . ? C3A C9A 1.440(14) . ? C4A C12A 1.386(14) . ? C4A C5A 1.428(14) . ? C5A O2A 1.202(12) . ? C5A N1A 1.421(13) . ? C6A C7A 1.360(16) . ? C6A H6A 0.9500 . ? C7A C8A 1.389(17) . ? C7A H7A 0.9500 . ? C8A C9A 1.458(16) . ? C8A H8A 0.9500 . ? C9A C10A 1.399(16) . ? C10A C11A 1.352(17) . ? C10A H10A 0.9500 . ? C11A C12A 1.450(15) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A N1A 1.475(12) . ? C13A C14A 1.542(12) . ? C13A C15A 1.555(13) . ? C13A H13A 1.0000 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A O3A 1.239(11) . ? C15A O4A 1.286(11) . ? O2A Cu1 2.227(6) 4_456 ? C1B O1B 1.234(11) . ? C1B N1B 1.357(12) . ? C1B C2B 1.495(14) . ? C2B C6B 1.369(13) . ? C2B C3B 1.383(13) . ? C3B C9B 1.419(14) . ? C3B C4B 1.436(14) . ? C4B C12B 1.365(15) . ? C4B C5B 1.421(14) . ? C5B O2B 1.223(11) . ? C5B N1B 1.415(12) . ? C6B C7B 1.357(14) . ? C6B H6B 0.9500 . ? C7B C8B 1.367(14) . ? C7B H7B 0.9500 . ? C8B C9B 1.395(15) . ? C8B H8B 0.9500 . ? C9B C10B 1.455(15) . ? C10B C11B 1.302(16) . ? C10B H10B 0.9500 . ? C11B C12B 1.413(17) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B N1B 1.489(12) . ? C13B C15B 1.523(14) . ? C13B C14B 1.541(14) . ? C13B H13B 1.0000 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B O3B 1.250(11) . ? C15B O4B 1.288(11) . ? C1C O1C 1.250(13) . ? C1C N1C 1.355(15) . ? C1C C2C 1.446(16) . ? C2C C6C 1.339(16) . ? C2C C3C 1.427(16) . ? C3C C4C 1.371(17) . ? C3C C9C 1.416(15) . ? C4C C12C 1.367(16) . ? C4C C5C 1.433(17) . ? C5C O2C 1.206(16) . ? C5C N1C 1.410(16) . ? C6C C7C 1.413(17) . ? C6C H6C 0.9500 . ? C7C C8C 1.383(18) . ? C7C H7C 0.9500 . ? C8C C9C 1.411(18) . ? C8C H8C 0.9500 . ? C9C C10C 1.430(18) . ? C10C C11C 1.313(18) . ? C10C H10C 0.9500 . ? C11C C12C 1.420(19) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C N1C 1.488(14) . ? C13C C15C 1.491(16) . ? C13C C14C 1.514(18) . ? C13C H13C 1.0000 . ? C14C H14G 0.9800 . ? C14C H14H 0.9800 . ? C14C H14I 0.9800 . ? C15C O4C 1.253(14) . ? C15C O3C 1.280(13) . ? C1D O1D 1.241(15) . ? C1D N1D 1.412(18) . ? C1D C2D 1.437(17) . ? C2D C3D 1.35(2) . ? C2D C6D 1.38(2) . ? C3D C4D 1.48(2) . ? C3D C9D 1.484(19) . ? C4D C12D 1.336(19) . ? C4D C5D 1.54(2) . ? C5D O2D 1.21(2) . ? C5D N1D 1.39(2) . ? C6D C7D 1.38(2) . ? C6D H6D 0.9500 . ? C7D C8D 1.28(2) . ? C7D H7D 0.9500 . ? C8D C9D 1.34(2) . ? C8D H8D 0.9500 . ? C9D C10D 1.47(2) . ? C10D C11D 1.34(2) . ? C10D H10D 0.9500 . ? C11D C12D 1.400(19) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D N1D 1.482(13) . ? C13D C15D 1.487(15) . ? C13D C14D 1.489(16) . ? C13D H13D 1.0000 . ? C14D H14J 0.9800 . ? C14D H14K 0.9800 . ? C14D H14L 0.9800 . ? C15D O4D 1.247(11) . ? C15D O3D 1.289(12) . ? C1E O1E 1.235(11) . ? C1E N1E 1.377(13) . ? C1E C2E 1.481(15) . ? C2E C6E 1.381(15) . ? C2E C3E 1.417(14) . ? C3E C4E 1.410(14) . ? C3E C9E 1.417(15) . ? C4E C12E 1.378(15) . ? C4E C5E 1.459(14) . ? C5E O2E 1.209(11) . ? C5E N1E 1.386(12) . ? C6E C7E 1.396(17) . ? C6E H6E 0.9500 . ? C7E C8E 1.445(19) . ? C7E H7E 0.9500 . ? C8E C9E 1.337(17) . ? C8E H8E 0.9500 . ? C9E C10E 1.384(18) . ? C10E C11E 1.393(19) . ? C10E H10E 0.9500 . ? C11E C12E 1.385(17) . ? C11E H11E 0.9500 . ? C12E H12E 0.9500 . ? C13E N1E 1.461(12) . ? C13E C14E 1.527(15) . ? C13E C15E 1.534(14) . ? C13E H13E 1.0000 . ? C14E H14M 0.9800 . ? C14E H14N 0.9800 . ? C14E H14O 0.9800 . ? C15E O4E 1.198(11) . ? C15E O3E 1.320(12) . ? O3E H3E 0.8500 . ? C1SA Cl1B 1.699(18) . ? C1SA Cl1A 1.768(18) . ? C1SB Cl1C 1.739(19) . ? C1SB Cl1D 1.746(19) . ? C2SA Cl2B 1.75(2) . ? C2SA Cl2A 1.75(2) . ? C2SB Cl2C 1.75(2) . ? C2SB Cl2D 1.76(2) . ? C2SC Cl2F 1.76(2) . ? C2SC Cl2E 1.76(2) . ? C2SD Cl2G 1.75(2) . ? C2SD Cl2H 1.77(2) . ? C3SA Cl3B 1.74(2) . ? C3SA Cl3A 1.74(2) . ? C3SB Cl3D 1.755(16) . ? C3SB Cl3C 1.801(16) . ? C4SA Cl4A 1.729(18) . ? C4SA Cl4B 1.765(18) . ? C4SB Cl4D 1.75(2) . ? C4SB Cl4C 1.75(2) . ? C4SC Cl4E 1.76(2) . ? C4SC Cl4F 1.77(2) . ? C5SA Cl5B 1.732(18) . ? C5SA Cl5A 1.742(18) . ? C5SB Cl5C 1.75(2) . ? C5SB Cl5D 1.77(2) . ? C5SC Cl5E 1.70(2) . ? C5SC Cl5F 1.73(2) . ? C5SD Cl5G 1.73(2) . ? C5SD Cl5H 1.76(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3B Cu1 O3D 167.2(3) . . ? O3B Cu1 O3C 88.9(3) . . ? O3D Cu1 O3C 88.1(3) . . ? O3B Cu1 O3A 91.8(3) . . ? O3D Cu1 O3A 89.4(3) . . ? O3C Cu1 O3A 171.7(3) . . ? O3B Cu1 O2A 91.6(3) . 4_556 ? O3D Cu1 O2A 101.1(3) . 4_556 ? O3C Cu1 O2A 98.8(3) . 4_556 ? O3A Cu1 O2A 89.4(2) . 4_556 ? O3B Cu1 Cu2 82.40(19) . . ? O3D Cu1 Cu2 84.9(2) . . ? O3C Cu1 Cu2 84.0(2) . . ? O3A Cu1 Cu2 87.91(18) . . ? O2A Cu1 Cu2 173.34(18) 4_556 . ? O4B Cu2 O4C 87.9(3) . . ? O4B Cu2 O4D 171.5(3) . . ? O4C Cu2 O4D 91.3(3) . . ? O4B Cu2 O4A 88.9(3) . . ? O4C Cu2 O4A 166.6(3) . . ? O4D Cu2 O4A 90.0(3) . . ? O4B Cu2 O4E 87.9(3) . . ? O4C Cu2 O4E 108.3(3) . . ? O4D Cu2 O4E 100.4(3) . . ? O4A Cu2 O4E 84.6(2) . . ? O4B Cu2 Cu1 87.3(2) . . ? O4C Cu2 Cu1 85.1(2) . . ? O4D Cu2 Cu1 84.2(2) . . ? O4A Cu2 Cu1 81.76(18) . . ? O4E Cu2 Cu1 165.59(17) . . ? O1A C1A N1A 119.1(9) . . ? O1A C1A C2A 124.6(10) . . ? N1A C1A C2A 116.4(10) . . ? C6A C2A C3A 124.0(11) . . ? C6A C2A C1A 118.6(11) . . ? C3A C2A C1A 117.3(10) . . ? C2A C3A C4A 123.4(10) . . ? C2A C3A C9A 118.9(11) . . ? C4A C3A C9A 117.7(11) . . ? C12A C4A C3A 120.1(10) . . ? C12A C4A C5A 118.0(10) . . ? C3A C4A C5A 121.9(10) . . ? O2A C5A N1A 118.0(9) . . ? O2A C5A C4A 126.6(10) . . ? N1A C5A C4A 115.4(10) . . ? C7A C6A C2A 117.9(13) . . ? C7A C6A H6A 121.1 . . ? C2A C6A H6A 121.1 . . ? C6A C7A C8A 122.9(12) . . ? C6A C7A H7A 118.6 . . ? C8A C7A H7A 118.6 . . ? C7A C8A C9A 119.7(11) . . ? C7A C8A H8A 120.1 . . ? C9A C8A H8A 120.1 . . ? C10A C9A C3A 121.1(11) . . ? C10A C9A C8A 122.6(11) . . ? C3A C9A C8A 116.3(11) . . ? C11A C10A C9A 121.3(12) . . ? C11A C10A H10A 119.4 . . ? C9A C10A H10A 119.4 . . ? C10A C11A C12A 118.4(12) . . ? C10A C11A H11A 120.8 . . ? C12A C11A H11A 120.8 . . ? C4A C12A C11A 121.4(12) . . ? C4A C12A H12A 119.3 . . ? C11A C12A H12A 119.3 . . ? N1A C13A C14A 113.5(8) . . ? N1A C13A C15A 107.7(7) . . ? C14A C13A C15A 116.3(8) . . ? N1A C13A H13A 106.2 . . ? C14A C13A H13A 106.2 . . ? C15A C13A H13A 106.2 . . ? C13A C14A H14A 109.5 . . ? C13A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C13A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? O3A C15A O4A 127.2(9) . . ? O3A C15A C13A 120.5(8) . . ? O4A C15A C13A 112.2(8) . . ? C5A N1A C1A 125.2(9) . . ? C5A N1A C13A 118.8(9) . . ? C1A N1A C13A 115.8(8) . . ? C5A O2A Cu1 132.0(6) . 4_456 ? C15A O3A Cu1 118.2(6) . . ? C15A O4A Cu2 124.8(6) . . ? O1B C1B N1B 120.7(10) . . ? O1B C1B C2B 121.6(9) . . ? N1B C1B C2B 117.7(9) . . ? C6B C2B C3B 120.8(10) . . ? C6B C2B C1B 120.3(10) . . ? C3B C2B C1B 118.9(9) . . ? C2B C3B C9B 119.3(10) . . ? C2B C3B C4B 120.0(10) . . ? C9B C3B C4B 120.7(10) . . ? C12B C4B C5B 120.6(11) . . ? C12B C4B C3B 117.5(11) . . ? C5B C4B C3B 121.9(10) . . ? O2B C5B N1B 119.9(9) . . ? O2B C5B C4B 124.3(10) . . ? N1B C5B C4B 115.7(9) . . ? C7B C6B C2B 120.3(11) . . ? C7B C6B H6B 119.8 . . ? C2B C6B H6B 119.8 . . ? C6B C7B C8B 120.7(11) . . ? C6B C7B H7B 119.6 . . ? C8B C7B H7B 119.6 . . ? C7B C8B C9B 120.9(11) . . ? C7B C8B H8B 119.5 . . ? C9B C8B H8B 119.5 . . ? C8B C9B C3B 117.9(10) . . ? C8B C9B C10B 124.5(11) . . ? C3B C9B C10B 117.6(11) . . ? C11B C10B C9B 120.1(12) . . ? C11B C10B H10B 120.0 . . ? C9B C10B H10B 120.0 . . ? C10B C11B C12B 122.5(12) . . ? C10B C11B H11B 118.7 . . ? C12B C11B H11B 118.7 . . ? C4B C12B C11B 121.5(12) . . ? C4B C12B H12B 119.3 . . ? C11B C12B H12B 119.3 . . ? N1B C13B C15B 109.9(8) . . ? N1B C13B C14B 112.0(9) . . ? C15B C13B C14B 113.3(9) . . ? N1B C13B H13B 107.1 . . ? C15B C13B H13B 107.1 . . ? C14B C13B H13B 107.1 . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? O3B C15B O4B 126.9(10) . . ? O3B C15B C13B 117.9(10) . . ? O4B C15B C13B 114.8(9) . . ? C1B N1B C5B 125.5(9) . . ? C1B N1B C13B 117.9(8) . . ? C5B N1B C13B 116.6(8) . . ? C15B O3B Cu1 124.6(7) . . ? C15B O4B Cu2 118.5(6) . . ? O1C C1C N1C 119.0(11) . . ? O1C C1C C2C 122.7(13) . . ? N1C C1C C2C 118.1(11) . . ? C6C C2C C3C 118.0(11) . . ? C6C C2C C1C 122.8(12) . . ? C3C C2C C1C 119.0(12) . . ? C4C C3C C9C 120.4(12) . . ? C4C C3C C2C 120.7(11) . . ? C9C C3C C2C 118.8(12) . . ? C12C C4C C3C 120.5(12) . . ? C12C C4C C5C 118.7(15) . . ? C3C C4C C5C 120.7(12) . . ? O2C C5C N1C 118.2(12) . . ? O2C C5C C4C 124.6(14) . . ? N1C C5C C4C 117.2(13) . . ? C2C C6C C7C 125.3(13) . . ? C2C C6C H6C 117.4 . . ? C7C C6C H6C 117.4 . . ? C8C C7C C6C 116.7(15) . . ? C8C C7C H7C 121.6 . . ? C6C C7C H7C 121.6 . . ? C7C C8C C9C 120.8(14) . . ? C7C C8C H8C 119.6 . . ? C9C C8C H8C 119.6 . . ? C8C C9C C3C 120.1(12) . . ? C8C C9C C10C 123.0(12) . . ? C3C C9C C10C 116.9(13) . . ? C11C C10C C9C 122.2(13) . . ? C11C C10C H10C 118.9 . . ? C9C C10C H10C 118.9 . . ? C10C C11C C12C 119.9(13) . . ? C10C C11C H11C 120.1 . . ? C12C C11C H11C 120.1 . . ? C4C C12C C11C 120.0(15) . . ? C4C C12C H12C 120.0 . . ? C11C C12C H12C 120.0 . . ? N1C C13C C15C 110.4(10) . . ? N1C C13C C14C 111.7(11) . . ? C15C C13C C14C 115.5(12) . . ? N1C C13C H13C 106.2 . . ? C15C C13C H13C 106.2 . . ? C14C C13C H13C 106.2 . . ? C13C C14C H14G 109.5 . . ? C13C C14C H14H 109.5 . . ? H14G C14C H14H 109.5 . . ? C13C C14C H14I 109.5 . . ? H14G C14C H14I 109.5 . . ? H14H C14C H14I 109.5 . . ? O4C C15C O3C 125.0(11) . . ? O4C C15C C13C 117.1(11) . . ? O3C C15C C13C 117.6(12) . . ? C1C N1C C5C 124.2(10) . . ? C1C N1C C13C 117.6(10) . . ? C5C N1C C13C 118.2(11) . . ? C15C O3C Cu1 122.5(8) . . ? C15C O4C Cu2 123.2(7) . . ? O1D C1D N1D 118.9(12) . . ? O1D C1D C2D 122.0(18) . . ? N1D C1D C2D 119.1(15) . . ? C3D C2D C6D 118.1(15) . . ? C3D C2D C1D 120.4(18) . . ? C6D C2D C1D 121.4(17) . . ? C2D C3D C4D 122.7(14) . . ? C2D C3D C9D 121(2) . . ? C4D C3D C9D 116.5(17) . . ? C12D C4D C3D 124.5(15) . . ? C12D C4D C5D 118.9(18) . . ? C3D C4D C5D 116.6(15) . . ? O2D C5D N1D 120.9(14) . . ? O2D C5D C4D 123.0(18) . . ? N1D C5D C4D 116.1(17) . . ? C7D C6D C2D 118.4(18) . . ? C7D C6D H6D 120.8 . . ? C2D C6D H6D 120.8 . . ? C8D C7D C6D 125(2) . . ? C8D C7D H7D 117.7 . . ? C6D C7D H7D 117.7 . . ? C7D C8D C9D 121.7(17) . . ? C7D C8D H8D 119.1 . . ? C9D C8D H8D 119.1 . . ? C8D C9D C10D 130.0(16) . . ? C8D C9D C3D 116.3(18) . . ? C10D C9D C3D 113.7(19) . . ? C11D C10D C9D 125.6(15) . . ? C11D C10D H10D 117.2 . . ? C9D C10D H10D 117.2 . . ? C10D C11D C12D 120.4(17) . . ? C10D C11D H11D 119.8 . . ? C12D C11D H11D 119.8 . . ? C4D C12D C11D 119.2(18) . . ? C4D C12D H12D 120.4 . . ? C11D C12D H12D 120.4 . . ? N1D C13D C15D 109.9(9) . . ? N1D C13D C14D 112.0(9) . . ? C15D C13D C14D 118.4(11) . . ? N1D C13D H13D 105.1 . . ? C15D C13D H13D 105.1 . . ? C14D C13D H13D 105.1 . . ? C13D C14D H14J 109.5 . . ? C13D C14D H14K 109.5 . . ? H14J C14D H14K 109.5 . . ? C13D C14D H14L 109.5 . . ? H14J C14D H14L 109.5 . . ? H14K C14D H14L 109.5 . . ? O4D C15D O3D 124.8(10) . . ? O4D C15D C13D 118.0(10) . . ? O3D C15D C13D 116.9(9) . . ? C5D N1D C1D 124.6(12) . . ? C5D N1D C13D 117.7(12) . . ? C1D N1D C13D 117.3(10) . . ? C15D O3D Cu1 121.9(7) . . ? C15D O4D Cu2 123.8(7) . . ? O1E C1E N1E 120.1(10) . . ? O1E C1E C2E 123.2(11) . . ? N1E C1E C2E 116.6(10) . . ? C6E C2E C3E 120.2(11) . . ? C6E C2E C1E 120.3(11) . . ? C3E C2E C1E 119.4(10) . . ? C4E C3E C9E 121.4(10) . . ? C4E C3E C2E 120.6(10) . . ? C9E C3E C2E 118.0(11) . . ? C12E C4E C3E 118.6(10) . . ? C12E C4E C5E 121.8(11) . . ? C3E C4E C5E 119.5(9) . . ? O2E C5E N1E 120.2(10) . . ? O2E C5E C4E 122.1(9) . . ? N1E C5E C4E 117.7(9) . . ? C2E C6E C7E 119.9(13) . . ? C2E C6E H6E 120.0 . . ? C7E C6E H6E 120.0 . . ? C6E C7E C8E 120.7(12) . . ? C6E C7E H7E 119.6 . . ? C8E C7E H7E 119.6 . . ? C9E C8E C7E 117.6(13) . . ? C9E C8E H8E 121.2 . . ? C7E C8E H8E 121.2 . . ? C8E C9E C10E 117.6(14) . . ? C8E C9E C3E 123.5(13) . . ? C10E C9E C3E 118.9(12) . . ? C9E C10E C11E 118.4(12) . . ? C9E C10E H10E 120.8 . . ? C11E C10E H10E 120.8 . . ? C12E C11E C10E 123.1(13) . . ? C12E C11E H11E 118.5 . . ? C10E C11E H11E 118.5 . . ? C4E C12E C11E 119.4(13) . . ? C4E C12E H12E 120.3 . . ? C11E C12E H12E 120.3 . . ? N1E C13E C14E 112.9(9) . . ? N1E C13E C15E 110.2(9) . . ? C14E C13E C15E 114.7(9) . . ? N1E C13E H13E 106.1 . . ? C14E C13E H13E 106.1 . . ? C15E C13E H13E 106.1 . . ? C13E C14E H14M 109.5 . . ? C13E C14E H14N 109.5 . . ? H14M C14E H14N 109.5 . . ? C13E C14E H14O 109.5 . . ? H14M C14E H14O 109.5 . . ? H14N C14E H14O 109.5 . . ? O4E C15E O3E 124.6(9) . . ? O4E C15E C13E 123.5(10) . . ? O3E C15E C13E 112.0(10) . . ? C1E N1E C5E 125.3(9) . . ? C1E N1E C13E 115.8(9) . . ? C5E N1E C13E 118.8(9) . . ? C15E O3E H3E 101.2 . . ? C15E O4E Cu2 124.0(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3B Cu1 Cu2 O4B -1.0(3) . . . . ? O3D Cu1 Cu2 O4B -179.3(3) . . . . ? O3C Cu1 Cu2 O4B -90.7(3) . . . . ? O3A Cu1 Cu2 O4B 91.1(3) . . . . ? O3B Cu1 Cu2 O4C 87.1(3) . . . . ? O3D Cu1 Cu2 O4C -91.2(3) . . . . ? O3C Cu1 Cu2 O4C -2.6(3) . . . . ? O3A Cu1 Cu2 O4C 179.2(3) . . . . ? O3B Cu1 Cu2 O4D 178.9(3) . . . . ? O3D Cu1 Cu2 O4D 0.6(3) . . . . ? O3C Cu1 Cu2 O4D 89.2(3) . . . . ? O3A Cu1 Cu2 O4D -89.0(3) . . . . ? O3B Cu1 Cu2 O4A -90.3(3) . . . . ? O3D Cu1 Cu2 O4A 91.4(3) . . . . ? O3C Cu1 Cu2 O4A -180.0(3) . . . . ? O3A Cu1 Cu2 O4A 1.8(3) . . . . ? O3B Cu1 Cu2 O4E -71.8(8) . . . . ? O3D Cu1 Cu2 O4E 109.9(8) . . . . ? O3C Cu1 Cu2 O4E -161.5(8) . . . . ? O3A Cu1 Cu2 O4E 20.3(8) . . . . ? O1A C1A C2A C6A 4.1(15) . . . . ? N1A C1A C2A C6A -177.4(9) . . . . ? O1A C1A C2A C3A -174.2(10) . . . . ? N1A C1A C2A C3A 4.4(13) . . . . ? C6A C2A C3A C4A 179.3(10) . . . . ? C1A C2A C3A C4A -2.5(15) . . . . ? C6A C2A C3A C9A -2.4(16) . . . . ? C1A C2A C3A C9A 175.8(8) . . . . ? C2A C3A C4A C12A 175.6(10) . . . . ? C9A C3A C4A C12A -2.7(14) . . . . ? C2A C3A C4A C5A -3.4(15) . . . . ? C9A C3A C4A C5A 178.2(9) . . . . ? C12A C4A C5A O2A 7.6(15) . . . . ? C3A C4A C5A O2A -173.3(9) . . . . ? C12A C4A C5A N1A -172.0(9) . . . . ? C3A C4A C5A N1A 7.1(13) . . . . ? C3A C2A C6A C7A -3.0(16) . . . . ? C1A C2A C6A C7A 178.9(9) . . . . ? C2A C6A C7A C8A 5.5(17) . . . . ? C6A C7A C8A C9A -2.7(18) . . . . ? C2A C3A C9A C10A -176.4(10) . . . . ? C4A C3A C9A C10A 2.0(15) . . . . ? C2A C3A C9A C8A 5.0(14) . . . . ? C4A C3A C9A C8A -176.6(9) . . . . ? C7A C8A C9A C10A 178.8(11) . . . . ? C7A C8A C9A C3A -2.7(15) . . . . ? C3A C9A C10A C11A 0.5(17) . . . . ? C8A C9A C10A C11A 179.0(11) . . . . ? C9A C10A C11A C12A -2.2(18) . . . . ? C3A C4A C12A C11A 1.1(15) . . . . ? C5A C4A C12A C11A -179.8(10) . . . . ? C10A C11A C12A C4A 1.4(17) . . . . ? N1A C13A C15A O3A -142.3(9) . . . . ? C14A C13A C15A O3A -13.6(13) . . . . ? N1A C13A C15A O4A 41.4(10) . . . . ? C14A C13A C15A O4A 170.1(8) . . . . ? O2A C5A N1A C1A 175.3(8) . . . . ? C4A C5A N1A C1A -5.1(13) . . . . ? O2A C5A N1A C13A -10.4(13) . . . . ? C4A C5A N1A C13A 169.2(8) . . . . ? O1A C1A N1A C5A 178.1(9) . . . . ? C2A C1A N1A C5A -0.5(13) . . . . ? O1A C1A N1A C13A 3.7(12) . . . . ? C2A C1A N1A C13A -174.9(8) . . . . ? C14A C13A N1A C5A 108.3(9) . . . . ? C15A C13A N1A C5A -121.3(9) . . . . ? C14A C13A N1A C1A -76.8(10) . . . . ? C15A C13A N1A C1A 53.5(10) . . . . ? N1A C5A O2A Cu1 -120.7(8) . . . 4_456 ? C4A C5A O2A Cu1 59.8(13) . . . 4_456 ? O4A C15A O3A Cu1 -1.6(13) . . . . ? C13A C15A O3A Cu1 -177.3(6) . . . . ? O3B Cu1 O3A C15A 81.5(7) . . . . ? O3D Cu1 O3A C15A -85.8(7) . . . . ? O2A Cu1 O3A C15A 173.1(7) 4_556 . . . ? Cu2 Cu1 O3A C15A -0.8(7) . . . . ? O3A C15A O4A Cu2 4.1(13) . . . . ? C13A C15A O4A Cu2 -179.9(6) . . . . ? O4B Cu2 O4A C15A -90.9(7) . . . . ? O4C Cu2 O4A C15A -14.6(17) . . . . ? O4D Cu2 O4A C15A 80.7(7) . . . . ? O4E Cu2 O4A C15A -178.9(7) . . . . ? Cu1 Cu2 O4A C15A -3.4(6) . . . . ? O1B C1B C2B C6B -5.0(14) . . . . ? N1B C1B C2B C6B 174.4(8) . . . . ? O1B C1B C2B C3B 175.1(9) . . . . ? N1B C1B C2B C3B -5.5(13) . . . . ? C6B C2B C3B C9B 2.9(14) . . . . ? C1B C2B C3B C9B -177.3(9) . . . . ? C6B C2B C3B C4B -176.8(9) . . . . ? C1B C2B C3B C4B 3.1(13) . . . . ? C2B C3B C4B C12B -176.1(10) . . . . ? C9B C3B C4B C12B 4.3(15) . . . . ? C2B C3B C4B C5B 2.0(15) . . . . ? C9B C3B C4B C5B -177.6(9) . . . . ? C12B C4B C5B O2B -7.2(16) . . . . ? C3B C4B C5B O2B 174.8(9) . . . . ? C12B C4B C5B N1B 173.5(10) . . . . ? C3B C4B C5B N1B -4.5(14) . . . . ? C3B C2B C6B C7B -3.3(14) . . . . ? C1B C2B C6B C7B 176.9(9) . . . . ? C2B C6B C7B C8B 0.9(15) . . . . ? C6B C7B C8B C9B 1.9(15) . . . . ? C7B C8B C9B C3B -2.2(15) . . . . ? C7B C8B C9B C10B -179.7(11) . . . . ? C2B C3B C9B C8B -0.1(14) . . . . ? C4B C3B C9B C8B 179.5(10) . . . . ? C2B C3B C9B C10B 177.5(10) . . . . ? C4B C3B C9B C10B -2.9(15) . . . . ? C8B C9B C10B C11B 179.1(13) . . . . ? C3B C9B C10B C11B 1.6(19) . . . . ? C9B C10B C11B C12B -2(2) . . . . ? C5B C4B C12B C11B 177.5(12) . . . . ? C3B C4B C12B C11B -4.4(18) . . . . ? C10B C11B C12B C4B 3(2) . . . . ? N1B C13B C15B O3B -144.8(8) . . . . ? C14B C13B C15B O3B -18.7(13) . . . . ? N1B C13B C15B O4B 41.6(11) . . . . ? C14B C13B C15B O4B 167.7(9) . . . . ? O1B C1B N1B C5B -177.7(8) . . . . ? C2B C1B N1B C5B 2.9(13) . . . . ? O1B C1B N1B C13B 1.7(13) . . . . ? C2B C1B N1B C13B -177.7(8) . . . . ? O2B C5B N1B C1B -177.4(9) . . . . ? C4B C5B N1B C1B 1.9(13) . . . . ? O2B C5B N1B C13B 3.2(13) . . . . ? C4B C5B N1B C13B -177.4(8) . . . . ? C15B C13B N1B C1B 49.1(11) . . . . ? C14B C13B N1B C1B -77.8(11) . . . . ? C15B C13B N1B C5B -131.4(8) . . . . ? C14B C13B N1B C5B 101.7(10) . . . . ? O4B C15B O3B Cu1 -5.8(13) . . . . ? C13B C15B O3B Cu1 -178.5(6) . . . . ? O3D Cu1 O3B C15B 11.3(16) . . . . ? O3C Cu1 O3B C15B 87.6(7) . . . . ? O3A Cu1 O3B C15B -84.1(7) . . . . ? O2A Cu1 O3B C15B -173.6(7) 4_556 . . . ? Cu2 Cu1 O3B C15B 3.5(7) . . . . ? O3B C15B O4B Cu2 4.1(12) . . . . ? C13B C15B O4B Cu2 177.0(6) . . . . ? O4C Cu2 O4B C15B -86.1(7) . . . . ? O4A Cu2 O4B C15B 80.9(6) . . . . ? O4E Cu2 O4B C15B 165.5(6) . . . . ? Cu1 Cu2 O4B C15B -0.9(6) . . . . ? O1C C1C C2C C6C 6.1(19) . . . . ? N1C C1C C2C C6C -177.8(12) . . . . ? O1C C1C C2C C3C -179.2(11) . . . . ? N1C C1C C2C C3C -3.1(16) . . . . ? C6C C2C C3C C4C 179.2(12) . . . . ? C1C C2C C3C C4C 4.3(17) . . . . ? C6C C2C C3C C9C -4.4(17) . . . . ? C1C C2C C3C C9C -179.3(10) . . . . ? C9C C3C C4C C12C 1.9(19) . . . . ? C2C C3C C4C C12C 178.3(12) . . . . ? C9C C3C C4C C5C -179.5(12) . . . . ? C2C C3C C4C C5C -3.1(19) . . . . ? C12C C4C C5C O2C 0(2) . . . . ? C3C C4C C5C O2C -178.4(16) . . . . ? C12C C4C C5C N1C 179.5(13) . . . . ? C3C C4C C5C N1C 1(2) . . . . ? C3C C2C C6C C7C 1(2) . . . . ? C1C C2C C6C C7C 176.2(12) . . . . ? C2C C6C C7C C8C 3(2) . . . . ? C6C C7C C8C C9C -4(2) . . . . ? C7C C8C C9C C3C 1(2) . . . . ? C7C C8C C9C C10C -177.1(13) . . . . ? C4C C3C C9C C8C 179.7(12) . . . . ? C2C C3C C9C C8C 3.3(18) . . . . ? C4C C3C C9C C10C -2.1(17) . . . . ? C2C C3C C9C C10C -178.5(11) . . . . ? C8C C9C C10C C11C -178.5(14) . . . . ? C3C C9C C10C C11C 3(2) . . . . ? C9C C10C C11C C12C -4(2) . . . . ? C3C C4C C12C C11C -3(2) . . . . ? C5C C4C C12C C11C 178.6(14) . . . . ? C10C C11C C12C C4C 4(2) . . . . ? N1C C13C C15C O4C 44.7(17) . . . . ? C14C C13C C15C O4C 172.6(12) . . . . ? N1C C13C C15C O3C -140.9(12) . . . . ? C14C C13C C15C O3C -13.0(18) . . . . ? O1C C1C N1C C5C 177.1(12) . . . . ? C2C C1C N1C C5C 0.9(18) . . . . ? O1C C1C N1C C13C -2.5(16) . . . . ? C2C C1C N1C C13C -178.7(10) . . . . ? O2C C5C N1C C1C 179.5(14) . . . . ? C4C C5C N1C C1C 0(2) . . . . ? O2C C5C N1C C13C -1(2) . . . . ? C4C C5C N1C C13C 179.9(12) . . . . ? C15C C13C N1C C1C 54.4(16) . . . . ? C14C C13C N1C C1C -75.5(13) . . . . ? C15C C13C N1C C5C -125.2(13) . . . . ? C14C C13C N1C C5C 104.9(15) . . . . ? O4C C15C O3C Cu1 -5.7(18) . . . . ? C13C C15C O3C Cu1 -179.6(8) . . . . ? O3B Cu1 O3C C15C -77.7(9) . . . . ? O3D Cu1 O3C C15C 89.9(9) . . . . ? O2A Cu1 O3C C15C -169.1(9) 4_556 . . . ? Cu2 Cu1 O3C C15C 4.8(9) . . . . ? O3C C15C O4C Cu2 2.1(18) . . . . ? C13C C15C O4C Cu2 176.1(8) . . . . ? O4B Cu2 O4C C15C 88.7(10) . . . . ? O4D Cu2 O4C C15C -82.8(10) . . . . ? O4A Cu2 O4C C15C 12.3(19) . . . . ? O4E Cu2 O4C C15C 175.8(9) . . . . ? Cu1 Cu2 O4C C15C 1.2(9) . . . . ? O1D C1D C2D C3D 176.2(12) . . . . ? N1D C1D C2D C3D -3.7(19) . . . . ? O1D C1D C2D C6D -6(2) . . . . ? N1D C1D C2D C6D 173.8(14) . . . . ? C6D C2D C3D C4D 179.8(14) . . . . ? C1D C2D C3D C4D -3(2) . . . . ? C6D C2D C3D C9D 3(2) . . . . ? C1D C2D C3D C9D -179.1(11) . . . . ? C2D C3D C4D C12D -177.4(13) . . . . ? C9D C3D C4D C12D -1(2) . . . . ? C2D C3D C4D C5D 3.9(19) . . . . ? C9D C3D C4D C5D -179.5(10) . . . . ? C12D C4D C5D O2D -1(2) . . . . ? C3D C4D C5D O2D 177.4(14) . . . . ? C12D C4D C5D N1D -177.7(12) . . . . ? C3D C4D C5D N1D 1.1(17) . . . . ? C3D C2D C6D C7D -2(2) . . . . ? C1D C2D C6D C7D -179.1(15) . . . . ? C2D C6D C7D C8D -1(3) . . . . ? C6D C7D C8D C9D 1(3) . . . . ? C7D C8D C9D C10D -178.4(16) . . . . ? C7D C8D C9D C3D 1(3) . . . . ? C2D C3D C9D C8D -3(2) . . . . ? C4D C3D C9D C8D -179.5(14) . . . . ? C2D C3D C9D C10D 176.3(12) . . . . ? C4D C3D C9D C10D -0.4(16) . . . . ? C8D C9D C10D C11D 177.2(18) . . . . ? C3D C9D C10D C11D -2(2) . . . . ? C9D C10D C11D C12D 5(3) . . . . ? C3D C4D C12D C11D 4(2) . . . . ? C5D C4D C12D C11D -177.4(13) . . . . ? C10D C11D C12D C4D -6(2) . . . . ? N1D C13D C15D O4D 41.9(14) . . . . ? C14D C13D C15D O4D 172.2(11) . . . . ? N1D C13D C15D O3D -143.2(10) . . . . ? C14D C13D C15D O3D -12.8(16) . . . . ? O2D C5D N1D C1D 176.0(13) . . . . ? C4D C5D N1D C1D -7.7(17) . . . . ? O2D C5D N1D C13D 3.2(19) . . . . ? C4D C5D N1D C13D 179.6(10) . . . . ? O1D C1D N1D C5D -170.6(11) . . . . ? C2D C1D N1D C5D 9.3(17) . . . . ? O1D C1D N1D C13D 2.1(15) . . . . ? C2D C1D N1D C13D -178.0(10) . . . . ? C15D C13D N1D C5D -136.9(11) . . . . ? C14D C13D N1D C5D 89.5(15) . . . . ? C15D C13D N1D C1D 49.9(13) . . . . ? C14D C13D N1D C1D -83.8(14) . . . . ? O4D C15D O3D Cu1 -6.7(14) . . . . ? C13D C15D O3D Cu1 178.8(7) . . . . ? O3B Cu1 O3D C15D -5.2(17) . . . . ? O3C Cu1 O3D C15D -81.6(7) . . . . ? O3A Cu1 O3D C15D 90.5(7) . . . . ? O2A Cu1 O3D C15D 179.8(7) 4_556 . . . ? Cu2 Cu1 O3D C15D 2.5(7) . . . . ? O3D C15D O4D Cu2 7.6(14) . . . . ? C13D C15D O4D Cu2 -177.9(7) . . . . ? O4C Cu2 O4D C15D 80.8(8) . . . . ? O4A Cu2 O4D C15D -85.8(8) . . . . ? O4E Cu2 O4D C15D -170.3(7) . . . . ? Cu1 Cu2 O4D C15D -4.1(7) . . . . ? O1E C1E C2E C6E 2.7(17) . . . . ? N1E C1E C2E C6E -173.2(11) . . . . ? O1E C1E C2E C3E -173.7(10) . . . . ? N1E C1E C2E C3E 10.4(15) . . . . ? C6E C2E C3E C4E 178.3(11) . . . . ? C1E C2E C3E C4E -5.3(16) . . . . ? C6E C2E C3E C9E 0.1(16) . . . . ? C1E C2E C3E C9E 176.5(10) . . . . ? C9E C3E C4E C12E -2.0(16) . . . . ? C2E C3E C4E C12E 180.0(10) . . . . ? C9E C3E C4E C5E 173.8(10) . . . . ? C2E C3E C4E C5E -4.3(15) . . . . ? C12E C4E C5E O2E 4.1(17) . . . . ? C3E C4E C5E O2E -171.4(10) . . . . ? C12E C4E C5E N1E -175.7(10) . . . . ? C3E C4E C5E N1E 8.8(15) . . . . ? C3E C2E C6E C7E -1.6(19) . . . . ? C1E C2E C6E C7E -177.9(12) . . . . ? C2E C6E C7E C8E 2(2) . . . . ? C6E C7E C8E C9E 0(2) . . . . ? C7E C8E C9E C10E 177.5(13) . . . . ? C7E C8E C9E C3E -1(2) . . . . ? C4E C3E C9E C8E -176.7(12) . . . . ? C2E C3E C9E C8E 1.4(18) . . . . ? C4E C3E C9E C10E 4.5(17) . . . . ? C2E C3E C9E C10E -177.4(11) . . . . ? C8E C9E C10E C11E 178.2(13) . . . . ? C3E C9E C10E C11E -2.9(19) . . . . ? C9E C10E C11E C12E -1(2) . . . . ? C3E C4E C12E C11E -2.0(18) . . . . ? C5E C4E C12E C11E -177.6(11) . . . . ? C10E C11E C12E C4E 4(2) . . . . ? N1E C13E C15E O4E 38.6(15) . . . . ? C14E C13E C15E O4E 167.4(10) . . . . ? N1E C13E C15E O3E -141.8(10) . . . . ? C14E C13E C15E O3E -13.0(13) . . . . ? O1E C1E N1E C5E 177.9(10) . . . . ? C2E C1E N1E C5E -6.0(16) . . . . ? O1E C1E N1E C13E -6.6(16) . . . . ? C2E C1E N1E C13E 169.5(9) . . . . ? O2E C5E N1E C1E 176.8(10) . . . . ? C4E C5E N1E C1E -3.4(16) . . . . ? O2E C5E N1E C13E 1.4(15) . . . . ? C4E C5E N1E C13E -178.8(9) . . . . ? C14E C13E N1E C1E -69.2(12) . . . . ? C15E C13E N1E C1E 60.5(13) . . . . ? C14E C13E N1E C5E 106.6(12) . . . . ? C15E C13E N1E C5E -123.7(10) . . . . ? O3E C15E O4E Cu2 -23.4(15) . . . . ? C13E C15E O4E Cu2 156.1(8) . . . . ? O4B Cu2 O4E C15E -50.1(8) . . . . ? O4C Cu2 O4E C15E -137.2(8) . . . . ? O4D Cu2 O4E C15E 128.0(8) . . . . ? O4A Cu2 O4E C15E 39.0(8) . . . . ? Cu1 Cu2 O4E C15E 20.6(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3E H3E O4A 0.85 1.72 2.569(9) 172 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.886 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.093 _vrf_PLAT431_2 ; PROBLEM: Short Inter HL..A Contact Cl3C .. Cl3A .. 1.26 Ang. RESPONSE: These atoms are part of disordered groups whose occupancies sum to less than one, i.e. Cl3C present in a given asymmetric unit, Cl3A is absent, etc. ; _vrf_PLAT432_2 ; PROBLEM: Short Inter X...Y Contact Cl3C .. C3SA .. 2.20 Ang. RESPONSE: These atoms are part of disordered groups whose occupancies sum to less than one, i.e. Cl3C present in a given asymmetric unit, C3SA is absent, etc. ; #===END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H53 Cu2 N5 O17, 2.5(C4 H8 O), 0.5(C6 H14)' _chemical_formula_sum 'C82 H80 Cu2 N5 O19.50' _chemical_formula_weight 1574.59 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 17.7756(12) _cell_length_b 18.5085(13) _cell_length_c 22.7270(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7477.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8251 _cell_measurement_theta_min 2.200 _cell_measurement_theta_max 23.692 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3284 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 108015 _diffrn_reflns_av_R_equivalents 0.0798 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.12 _reflns_number_total 13308 _reflns_number_gt 10992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1218P)^2^+5.4941P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.056(16) _refine_ls_number_reflns 13308 _refine_ls_number_parameters 908 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1890 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.20071(4) 0.70829(3) 0.67571(3) 0.03841(19) Uani 1 1 d . . . Cu2 Cu 0.21876(4) 0.84909(3) 0.67941(3) 0.03352(18) Uani 1 1 d . A . C1A C 0.3185(4) 0.8424(4) 0.9199(3) 0.0435(15) Uani 1 1 d . . . C2A C 0.2919(4) 0.8986(3) 0.9595(3) 0.0471(16) Uani 1 1 d . . . C3A C 0.2138(4) 0.9137(3) 0.9645(3) 0.0447(15) Uani 1 1 d . . . C4A C 0.1618(4) 0.8771(3) 0.9310(3) 0.0404(15) Uani 1 1 d . . . C5A C 0.1867(4) 0.8209(3) 0.8891(3) 0.0373(14) Uani 1 1 d . . . C6A C 0.3432(5) 0.9374(4) 0.9926(3) 0.0537(18) Uani 1 1 d . . . H6A H 0.3951 0.9256 0.9900 0.064 Uiso 1 1 calc R . . C7A C 0.3212(6) 0.9929(4) 1.0294(3) 0.062(2) Uani 1 1 d . . . H7A H 0.3579 1.0194 1.0508 0.075 Uiso 1 1 calc R . . C8A C 0.2448(6) 1.0104(4) 1.0352(3) 0.070(3) Uani 1 1 d . . . H8A H 0.2297 1.0484 1.0607 0.083 Uiso 1 1 calc R . . C9A C 0.1906(5) 0.9714(3) 1.0033(3) 0.0523(19) Uani 1 1 d . . . C10A C 0.1125(5) 0.9855(4) 1.0068(3) 0.061(2) Uani 1 1 d . . . H10A H 0.0946 1.0221 1.0326 0.073 Uiso 1 1 calc R . . C11A C 0.0635(5) 0.9479(4) 0.9744(4) 0.068(2) Uani 1 1 d . . . H11A H 0.0114 0.9587 0.9778 0.082 Uiso 1 1 calc R . . C12A C 0.0862(4) 0.8931(4) 0.9355(3) 0.0536(18) Uani 1 1 d . . . H12A H 0.0501 0.8675 0.9127 0.064 Uiso 1 1 calc R . . C13A C 0.2885(4) 0.7518(3) 0.8430(3) 0.0418(14) Uani 1 1 d . . . H13A H 0.3440 0.7585 0.8383 0.050 Uiso 1 1 calc R . . C14A C 0.2783(4) 0.6769(3) 0.8698(3) 0.0489(16) Uani 1 1 d . . . H14A H 0.3050 0.6745 0.9075 0.073 Uiso 1 1 calc R . . H14B H 0.2988 0.6405 0.8429 0.073 Uiso 1 1 calc R . . H14C H 0.2247 0.6677 0.8762 0.073 Uiso 1 1 calc R . . C15A C 0.2548(3) 0.7618(3) 0.7814(3) 0.0422(15) Uani 1 1 d . . . C1B C 0.4905(4) 0.8879(4) 0.6212(3) 0.0474(16) Uani 1 1 d . . . C2B C 0.5103(4) 0.9520(4) 0.6563(3) 0.0502(17) Uani 1 1 d . . . C3B C 0.5052(4) 0.9508(4) 0.7179(3) 0.0553(18) Uani 1 1 d . . . C4B C 0.4827(4) 0.8873(4) 0.7470(4) 0.0560(19) Uani 1 1 d . . . C5B C 0.4612(4) 0.8213(3) 0.7128(3) 0.0440(15) Uani 1 1 d . . . C6B C 0.5291(4) 1.0163(4) 0.6276(4) 0.063(2) Uani 1 1 d . . . H6B H 0.5304 1.0182 0.5859 0.076 Uiso 1 1 calc R . . C7B C 0.5460(4) 1.0778(4) 0.6607(4) 0.070(2) Uani 1 1 d . . . H7B H 0.5601 1.1210 0.6411 0.084 Uiso 1 1 calc R . . C8B C 0.5427(5) 1.0770(5) 0.7199(4) 0.077(3) Uani 1 1 d . . . H8B H 0.5555 1.1195 0.7411 0.093 Uiso 1 1 calc R . . C9B C 0.5206(5) 1.0140(4) 0.7518(4) 0.069(2) Uani 1 1 d . . . C10B C 0.5162(6) 1.0095(5) 0.8132(4) 0.091(3) Uani 1 1 d . . . H10B H 0.5299 1.0503 0.8362 0.109 Uiso 1 1 calc R . . C11B C 0.4929(6) 0.9482(5) 0.8409(4) 0.092(3) Uani 1 1 d . . . H11B H 0.4875 0.9469 0.8824 0.110 Uiso 1 1 calc R . . C12B C 0.4768(5) 0.8856(5) 0.8061(4) 0.075(3) Uani 1 1 d . . . H12B H 0.4616 0.8422 0.8250 0.090 Uiso 1 1 calc R . . C13B C 0.4243(4) 0.7709(3) 0.6194(3) 0.0419(14) Uani 1 1 d . . . H13B H 0.4219 0.7873 0.5775 0.050 Uiso 1 1 calc R . . C14B C 0.4617(4) 0.6961(4) 0.6192(4) 0.063(2) Uani 1 1 d . . . H14D H 0.5121 0.6998 0.6021 0.094 Uiso 1 1 calc R . . H14F H 0.4313 0.6626 0.5958 0.094 Uiso 1 1 calc R . . H14E H 0.4656 0.6781 0.6597 0.094 Uiso 1 1 calc R . . C15B C 0.3430(3) 0.7712(3) 0.6428(3) 0.0382(13) Uani 1 1 d . . . C1C C 0.1740(5) 0.8793(3) 0.4345(3) 0.0468(17) Uani 1 1 d . . . C2C C 0.2298(4) 0.9183(3) 0.3957(3) 0.0414(15) Uani 1 1 d . . . C3C C 0.3054(4) 0.9005(3) 0.3996(3) 0.0443(15) Uani 1 1 d . . . C4C C 0.3322(4) 0.8446(3) 0.4381(3) 0.0424(15) Uani 1 1 d . . . C5C C 0.2777(4) 0.8067(3) 0.4744(3) 0.0438(15) Uani 1 1 d . . . C6C C 0.2043(4) 0.9722(3) 0.3611(3) 0.0470(16) Uani 1 1 d . . . H6C H 0.1521 0.9829 0.3589 0.056 Uiso 1 1 calc R . . C7C C 0.2580(5) 1.0131(3) 0.3276(3) 0.0561(19) Uani 1 1 d . . . H7C H 0.2411 1.0516 0.3033 0.067 Uiso 1 1 calc R . . C8C C 0.3329(5) 0.9977(4) 0.3301(3) 0.0560(19) Uani 1 1 d . . . H8C H 0.3673 1.0265 0.3082 0.067 Uiso 1 1 calc R . . C9C C 0.3609(5) 0.9395(4) 0.3646(3) 0.0502(18) Uani 1 1 d . . . C10C C 0.4354(4) 0.9210(4) 0.3673(3) 0.0546(18) Uani 1 1 d . . . H10C H 0.4710 0.9463 0.3439 0.066 Uiso 1 1 calc R . . C11C C 0.4595(5) 0.8660(4) 0.4039(3) 0.0556(18) Uani 1 1 d . . . H11C H 0.5114 0.8537 0.4055 0.067 Uiso 1 1 calc R . . C12C C 0.4072(4) 0.8284(4) 0.4386(3) 0.0491(16) Uani 1 1 d . . . H12C H 0.4246 0.7905 0.4633 0.059 Uiso 1 1 calc R . . C13C C 0.1463(4) 0.7835(4) 0.5061(3) 0.0469(15) Uani 1 1 d . . . H13C H 0.0978 0.8108 0.5043 0.056 Uiso 1 1 calc R . . C14C C 0.1314(5) 0.7109(4) 0.4793(3) 0.062(2) Uani 1 1 d . . . H14G H 0.1240 0.7163 0.4368 0.092 Uiso 1 1 calc R . . H14I H 0.0861 0.6899 0.4969 0.092 Uiso 1 1 calc R . . H14H H 0.1744 0.6790 0.4866 0.092 Uiso 1 1 calc R . . C15C C 0.1695(3) 0.7817(3) 0.5707(2) 0.0357(13) Uani 1 1 d . . . C1D C -0.0418(3) 0.9377(3) 0.7216(3) 0.0391(14) Uani 1 1 d . . . C2D C -0.0540(3) 1.0021(3) 0.6835(3) 0.0394(13) Uani 1 1 d . . . C3D C -0.0512(3) 0.9953(3) 0.6218(3) 0.0401(14) Uani 1 1 d . . . C4D C -0.0372(4) 0.9271(4) 0.5949(3) 0.0453(15) Uani 1 1 d . . . C5D C -0.0214(4) 0.8646(3) 0.6313(3) 0.0420(15) Uani 1 1 d . . . C6D C -0.0692(4) 1.0689(4) 0.7083(3) 0.0457(15) Uani 1 1 d . . . H6D H -0.0723 1.0732 0.7499 0.055 Uiso 1 1 calc R . . C7D C -0.0800(4) 1.1287(3) 0.6741(3) 0.0540(17) Uani 1 1 d . . . H7D H -0.0906 1.1741 0.6918 0.065 Uiso 1 1 calc R . . C8D C -0.0756(4) 1.1230(4) 0.6141(3) 0.0524(17) Uani 1 1 d . . . H8D H -0.0821 1.1653 0.5909 0.063 Uiso 1 1 calc R . . C9D C -0.0618(4) 1.0566(4) 0.5852(3) 0.0479(16) Uani 1 1 d . . . C10D C -0.0603(5) 1.0467(4) 0.5243(3) 0.061(2) Uani 1 1 d . . . H10D H -0.0688 1.0871 0.4994 0.073 Uiso 1 1 calc RD . . C11D C -0.0473(6) 0.9820(4) 0.4996(3) 0.074(3) Uani 1 1 d . . . H11D H -0.0469 0.9773 0.4580 0.089 Uiso 1 1 calc R . . C12D C -0.0345(5) 0.9218(4) 0.5349(3) 0.061(2) Uani 1 1 d . . . H12D H -0.0237 0.8765 0.5171 0.073 Uiso 1 1 calc R . . C13D C -0.0029(4) 0.8104(3) 0.7299(3) 0.0417(15) Uani 1 1 d . . . H13D H -0.0004 0.8273 0.7717 0.050 Uiso 1 1 calc R . . C14D C -0.0583(4) 0.7463(4) 0.7285(3) 0.0555(18) Uani 1 1 d . . . H14J H -0.0998 0.7555 0.7560 0.083 Uiso 1 1 calc R . . H14L H -0.0320 0.7020 0.7401 0.083 Uiso 1 1 calc R . . H14K H -0.0784 0.7407 0.6887 0.083 Uiso 1 1 calc R . . C15D C 0.0768(4) 0.7946(3) 0.7111(2) 0.0412(15) Uani 1 1 d . . . C61 C 0.2972(5) 1.0009(4) 0.6857(3) 0.064(2) Uani 1 1 d . . . H61 H 0.3424 0.9736 0.6861 0.077 Uiso 1 1 calc R . . C62 C 0.2997(7) 1.0728(5) 0.6891(6) 0.110(4) Uani 1 1 d . . . H62 H 0.3465 1.0970 0.6932 0.131 Uiso 1 1 calc R . . C63 C 0.2379(8) 1.1092(6) 0.6869(7) 0.129(5) Uani 1 1 d . . . H63 H 0.2418 1.1603 0.6884 0.155 Uiso 1 1 calc R . . C64 C 0.1688(8) 1.0810(5) 0.6827(6) 0.106(4) Uani 1 1 d . . . H64 H 0.1247 1.1100 0.6810 0.127 Uiso 1 1 calc R . . C65 C 0.1668(5) 1.0095(3) 0.6812(3) 0.0557(17) Uani 1 1 d . . . H65 H 0.1190 0.9867 0.6796 0.067 Uiso 1 1 calc R . . N1A N 0.2639(3) 0.8085(3) 0.8837(2) 0.0407(13) Uani 1 1 d . . . N1B N 0.4676(3) 0.8267(3) 0.6521(2) 0.0431(13) Uani 1 1 d . . . N1C N 0.2021(3) 0.8258(2) 0.4707(2) 0.0396(12) Uani 1 1 d . . . N1D N -0.0298(3) 0.8734(3) 0.6939(2) 0.0379(11) Uani 1 1 d . . . N5 N 0.2286(3) 0.9666(2) 0.6817(2) 0.0350(10) Uani 1 1 d . . . O1A O 0.3850(3) 0.8245(3) 0.91470(19) 0.0562(13) Uani 1 1 d . . . O2A O 0.1436(2) 0.7857(2) 0.85818(18) 0.0424(10) Uani 1 1 d . . . O3A O 0.2382(3) 0.7046(2) 0.75541(16) 0.0400(10) Uani 1 1 d . . . O4A O 0.2508(2) 0.8254(2) 0.76204(18) 0.0403(10) Uani 1 1 d . A . O1B O 0.4899(3) 0.8877(3) 0.5673(2) 0.0560(12) Uani 1 1 d . . . O2B O 0.4403(3) 0.7676(3) 0.7371(2) 0.0518(12) Uani 1 1 d . . . O3B O 0.3079(2) 0.7136(2) 0.64617(18) 0.0451(10) Uani 1 1 d . . . O4B O 0.3205(2) 0.8338(2) 0.65444(19) 0.0413(10) Uani 1 1 d . A . O1C O 0.1062(3) 0.8914(2) 0.4317(2) 0.0508(11) Uani 1 1 d . . . O2C O 0.2975(3) 0.7587(2) 0.50941(18) 0.0482(11) Uani 1 1 d . . . O3C O 0.1642(2) 0.7218(2) 0.59597(17) 0.0421(10) Uani 1 1 d . . . O4C O 0.1886(2) 0.8403(2) 0.59464(16) 0.0386(9) Uani 1 1 d . A . O1D O -0.0422(3) 0.9422(2) 0.77600(18) 0.0524(12) Uani 1 1 d . . . O2D O -0.0028(3) 0.8066(2) 0.61215(19) 0.0497(12) Uani 1 1 d . . . O3D O 0.0980(2) 0.7305(2) 0.70694(17) 0.0405(10) Uani 1 1 d . . . O4D O 0.1164(2) 0.8504(2) 0.70296(17) 0.0370(9) Uani 1 1 d . A . C66A C 0.2537(9) 0.5521(11) 0.6919(7) 0.091(2) Uiso 0.50 1 d PD A 1 H66A H 0.2377 0.5119 0.7177 0.109 Uiso 0.50 1 calc PR A 1 H66B H 0.2877 0.5844 0.7142 0.109 Uiso 0.50 1 calc PR A 1 C67A C 0.2910(11) 0.5245(11) 0.6382(7) 0.091(2) Uiso 0.50 1 d PD A 1 H67A H 0.3388 0.5507 0.6316 0.109 Uiso 0.50 1 calc PR A 1 H67B H 0.3026 0.4725 0.6428 0.109 Uiso 0.50 1 calc PR A 1 C68A C 0.2405(9) 0.5352(12) 0.5879(8) 0.091(2) Uiso 0.50 1 d PD A 1 H68A H 0.2356 0.4906 0.5642 0.109 Uiso 0.50 1 calc PR A 1 H68B H 0.2581 0.5751 0.5623 0.109 Uiso 0.50 1 calc PR A 1 C69A C 0.1689(10) 0.5538(18) 0.6176(9) 0.091(2) Uiso 0.50 1 d PD A 1 H69A H 0.1376 0.5852 0.5922 0.109 Uiso 0.50 1 calc PR A 1 H69B H 0.1401 0.5096 0.6272 0.109 Uiso 0.50 1 calc PR A 1 O17A O 0.1903(3) 0.5909(2) 0.6699(2) 0.0520(11) Uiso 0.50 1 d PD A 1 C66B C 0.2347(12) 0.5470(10) 0.7072(7) 0.091(2) Uiso 0.50 1 d PD A 2 H66C H 0.2034 0.5280 0.7398 0.109 Uiso 0.50 1 calc PR A 2 H66D H 0.2759 0.5761 0.7245 0.109 Uiso 0.50 1 calc PR A 2 C67B C 0.2665(12) 0.4866(10) 0.6735(8) 0.091(2) Uiso 0.50 1 d PD A 2 H67C H 0.2443 0.4401 0.6864 0.109 Uiso 0.50 1 calc PR A 2 H67D H 0.3217 0.4843 0.6785 0.109 Uiso 0.50 1 calc PR A 2 C68B C 0.2465(12) 0.5022(11) 0.6114(8) 0.091(2) Uiso 0.50 1 d PD A 2 H68C H 0.2901 0.5228 0.5901 0.109 Uiso 0.50 1 calc PR A 2 H68D H 0.2301 0.4576 0.5910 0.109 Uiso 0.50 1 calc PR A 2 C69B C 0.1845(12) 0.5549(16) 0.6146(8) 0.091(2) Uiso 0.50 1 d PD A 2 H69C H 0.1884 0.5902 0.5820 0.109 Uiso 0.50 1 calc PR A 2 H69D H 0.1354 0.5299 0.6115 0.109 Uiso 0.50 1 calc PR A 2 O17B O 0.1903(3) 0.5909(2) 0.6699(2) 0.0520(11) Uiso 0.50 1 d PD A 2 O71 O 0.1139(8) 0.3632(6) 0.5583(6) 0.186(3) Uiso 1 1 d D B 3 C71 C 0.1292(11) 0.3388(9) 0.6165(7) 0.186(3) Uiso 1 1 d D B 3 H71A H 0.1035 0.3696 0.6460 0.223 Uiso 1 1 calc R B 3 H71B H 0.1840 0.3392 0.6246 0.223 Uiso 1 1 calc R B 3 C72 C 0.0990(12) 0.2636(8) 0.6177(7) 0.186(3) Uiso 1 1 d D B 3 H72A H 0.1357 0.2306 0.6365 0.223 Uiso 1 1 calc R B 3 H72B H 0.0516 0.2619 0.6406 0.223 Uiso 1 1 calc R B 3 C73 C 0.0851(12) 0.2413(8) 0.5562(7) 0.186(3) Uiso 1 1 d D B 3 H73A H 0.1149 0.1979 0.5461 0.223 Uiso 1 1 calc R B 3 H73B H 0.0311 0.2309 0.5497 0.223 Uiso 1 1 calc R B 3 C74 C 0.1090(12) 0.3026(9) 0.5219(7) 0.186(3) Uiso 1 1 d D B 3 H74A H 0.1586 0.2926 0.5039 0.223 Uiso 1 1 calc R B 3 H74B H 0.0724 0.3118 0.4899 0.223 Uiso 1 1 calc R B 3 O81 O 0.3947(11) 0.2335(11) 0.6153(8) 0.144(3) Uiso 0.50 1 d PD C 5 C81 C 0.4434(13) 0.2453(18) 0.5672(11) 0.144(3) Uiso 0.50 1 d PD C 5 H81A H 0.4704 0.2002 0.5573 0.173 Uiso 0.50 1 calc PR C 5 H81B H 0.4809 0.2828 0.5772 0.173 Uiso 0.50 1 calc PR C 5 C82 C 0.3987(14) 0.2683(8) 0.5184(9) 0.144(3) Uiso 0.50 1 d PD C 5 H82A H 0.3924 0.2283 0.4900 0.173 Uiso 0.50 1 calc PR C 5 H82B H 0.4233 0.3093 0.4981 0.173 Uiso 0.50 1 calc PR C 5 C83 C 0.3249(14) 0.2907(18) 0.5419(11) 0.144(3) Uiso 0.50 1 d PD C 5 H83A H 0.2836 0.2728 0.5166 0.173 Uiso 0.50 1 calc PR C 5 H83B H 0.3215 0.3440 0.5444 0.173 Uiso 0.50 1 calc PR C 5 C84 C 0.3209(13) 0.2576(17) 0.6014(11) 0.144(3) Uiso 0.50 1 d PD C 5 H84A H 0.3036 0.2937 0.6306 0.173 Uiso 0.50 1 calc PR C 5 H84B H 0.2852 0.2165 0.6014 0.173 Uiso 0.50 1 calc PR C 5 O82 O 0.3530(11) 0.3239(9) 0.5676(9) 0.144(3) Uiso 0.50 1 d PD D 6 C85 C 0.3453(18) 0.2538(12) 0.5413(11) 0.144(3) Uiso 0.50 1 d PD D 6 H85A H 0.3634 0.2539 0.5001 0.173 Uiso 0.50 1 calc PR D 6 H85B H 0.2923 0.2374 0.5421 0.173 Uiso 0.50 1 calc PR D 6 C86 C 0.3933(18) 0.2072(11) 0.5789(13) 0.144(3) Uiso 0.50 1 d PD D 6 H86A H 0.4342 0.1859 0.5550 0.173 Uiso 0.50 1 calc PR D 6 H86B H 0.3628 0.1673 0.5954 0.173 Uiso 0.50 1 calc PR D 6 C87 C 0.4257(17) 0.2509(14) 0.6273(11) 0.144(3) Uiso 0.50 1 d PD D 6 H87A H 0.4281 0.2238 0.6648 0.173 Uiso 0.50 1 calc PR D 6 H87B H 0.4761 0.2701 0.6173 0.173 Uiso 0.50 1 calc PR D 6 C88 C 0.3679(16) 0.3079(14) 0.6284(9) 0.144(3) Uiso 0.50 1 d PD D 6 H88A H 0.3218 0.2907 0.6484 0.173 Uiso 0.50 1 calc PR D 6 H88B H 0.3867 0.3513 0.6492 0.173 Uiso 0.50 1 calc PR D 6 O91 O 0.2659(13) 0.2569(10) 0.8073(10) 0.164(5) Uiso 0.50 1 d PD E 7 C91 C 0.2780(19) 0.2887(15) 0.7523(10) 0.164(5) Uiso 0.50 1 d PD E 7 H91A H 0.2303 0.3064 0.7350 0.197 Uiso 0.50 1 calc PR E 7 H91B H 0.3018 0.2543 0.7246 0.197 Uiso 0.50 1 calc PR E 7 C92 C 0.3290(18) 0.3490(16) 0.7663(13) 0.164(5) Uiso 0.50 1 d PD E 7 H92A H 0.3275 0.3867 0.7354 0.197 Uiso 0.50 1 calc PR E 7 H92B H 0.3815 0.3320 0.7712 0.197 Uiso 0.50 1 calc PR E 7 C93 C 0.2977(19) 0.3760(13) 0.8224(13) 0.164(5) Uiso 0.50 1 d PD E 7 H93A H 0.2757 0.4247 0.8178 0.197 Uiso 0.50 1 calc PR E 7 H93B H 0.3366 0.3773 0.8537 0.197 Uiso 0.50 1 calc PR E 7 C94 C 0.2389(16) 0.3212(15) 0.8355(15) 0.164(5) Uiso 0.50 1 d PD E 7 H94A H 0.2336 0.3138 0.8784 0.197 Uiso 0.50 1 calc PR E 7 H94B H 0.1897 0.3361 0.8191 0.197 Uiso 0.50 1 calc PR E 7 C95 C 0.344(2) 0.2479(13) 0.7954(16) 0.172(6) Uiso 0.50 1 d PD F 8 H95A H 0.3550 0.2182 0.8300 0.258 Uiso 0.50 1 calc PR F 8 H95B H 0.3784 0.2347 0.7634 0.258 Uiso 0.50 1 calc PR F 8 H95C H 0.2920 0.2397 0.7828 0.258 Uiso 0.50 1 calc PR F 8 C96 C 0.3548(14) 0.3283(15) 0.8109(16) 0.172(6) Uiso 0.50 1 d PD F 8 H96A H 0.3998 0.3475 0.7905 0.206 Uiso 0.50 1 calc PR F 8 H96B H 0.3624 0.3337 0.8538 0.206 Uiso 0.50 1 calc PR F 8 C97 C 0.2843(19) 0.3707(15) 0.7915(11) 0.172(6) Uiso 0.50 1 d PD F 8 H97A H 0.3001 0.4135 0.7686 0.206 Uiso 0.50 1 calc PR F 8 H97B H 0.2533 0.3397 0.7655 0.206 Uiso 0.50 1 calc PR F 8 C98 C 0.2371(15) 0.3951(14) 0.8435(13) 0.172(6) Uiso 0.50 1 d PD F 8 H98A H 0.1832 0.3882 0.8341 0.206 Uiso 0.50 1 calc PR F 8 H98B H 0.2490 0.3645 0.8781 0.206 Uiso 0.50 1 calc PR F 8 C99 C 0.251(2) 0.4737(12) 0.8592(12) 0.172(6) Uiso 0.50 1 d PD F 8 H99A H 0.2039 0.5019 0.8532 0.206 Uiso 0.50 1 calc PR F 8 H99B H 0.2902 0.4941 0.8334 0.206 Uiso 0.50 1 calc PR F 8 C100 C 0.275(2) 0.4787(16) 0.9245(12) 0.172(6) Uiso 0.50 1 d PD F 8 H101 H 0.2365 0.4577 0.9497 0.258 Uiso 0.50 1 calc PR F 8 H102 H 0.2831 0.5295 0.9352 0.258 Uiso 0.50 1 calc PR F 8 H103 H 0.3226 0.4521 0.9299 0.258 Uiso 0.50 1 calc PR F 8 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0565(5) 0.0280(3) 0.0307(4) -0.0035(3) 0.0095(3) -0.0025(3) Cu2 0.0426(4) 0.0274(3) 0.0305(3) -0.0028(3) 0.0067(3) -0.0008(3) C1A 0.050(4) 0.048(4) 0.032(3) 0.013(3) -0.002(3) -0.005(3) C2A 0.067(5) 0.044(3) 0.030(3) 0.011(3) -0.003(3) -0.008(3) C3A 0.069(5) 0.034(3) 0.031(3) 0.006(2) 0.011(3) -0.001(3) C4A 0.054(4) 0.031(3) 0.036(3) -0.003(2) 0.017(3) -0.008(3) C5A 0.044(4) 0.035(3) 0.032(3) 0.005(2) 0.010(3) -0.001(3) C6A 0.072(5) 0.050(4) 0.038(4) 0.005(3) -0.016(3) -0.014(4) C7A 0.090(7) 0.066(5) 0.030(4) 0.006(3) -0.007(4) -0.024(4) C8A 0.137(9) 0.038(4) 0.033(4) 0.000(3) 0.013(4) -0.018(4) C9A 0.092(6) 0.036(3) 0.029(3) -0.001(3) 0.009(3) -0.003(3) C10A 0.090(6) 0.040(4) 0.052(4) -0.001(3) 0.032(4) 0.003(4) C11A 0.069(5) 0.059(5) 0.077(6) -0.003(4) 0.028(5) 0.015(4) C12A 0.070(5) 0.042(4) 0.049(4) -0.007(3) 0.016(4) 0.000(3) C13A 0.045(4) 0.045(3) 0.035(3) -0.005(2) 0.004(3) 0.016(3) C14A 0.059(4) 0.049(3) 0.039(3) -0.004(3) -0.006(3) 0.013(3) C15A 0.039(4) 0.042(4) 0.046(4) 0.007(3) 0.011(3) 0.011(3) C1B 0.035(4) 0.059(4) 0.048(4) 0.015(3) 0.011(3) 0.009(3) C2B 0.038(4) 0.054(4) 0.059(4) 0.010(3) 0.005(3) 0.003(3) C3B 0.057(5) 0.050(4) 0.058(5) -0.003(3) 0.004(4) 0.001(3) C4B 0.053(5) 0.048(4) 0.066(5) -0.005(3) 0.007(4) -0.004(3) C5B 0.051(4) 0.042(4) 0.039(4) 0.001(3) 0.010(3) 0.008(3) C6B 0.048(5) 0.057(5) 0.084(6) 0.016(4) -0.004(4) -0.008(4) C7B 0.055(5) 0.061(5) 0.094(7) 0.003(4) -0.004(4) -0.023(4) C8B 0.083(6) 0.061(5) 0.087(7) -0.012(4) -0.010(5) -0.011(4) C9B 0.070(6) 0.059(5) 0.079(6) -0.005(4) -0.003(5) -0.024(4) C10B 0.109(8) 0.088(6) 0.077(7) -0.033(5) 0.011(6) -0.037(6) C11B 0.121(9) 0.094(7) 0.061(6) -0.013(5) 0.002(5) -0.043(6) C12B 0.092(7) 0.076(5) 0.056(5) -0.016(4) 0.028(4) -0.021(5) C13B 0.044(4) 0.043(3) 0.039(3) -0.007(3) 0.005(3) 0.001(3) C14B 0.055(5) 0.065(5) 0.068(5) -0.009(4) 0.018(4) 0.019(4) C15B 0.038(3) 0.040(3) 0.037(3) -0.009(3) 0.002(3) 0.003(3) C1C 0.072(5) 0.042(3) 0.026(3) -0.008(3) -0.010(3) -0.006(3) C2C 0.062(4) 0.034(3) 0.028(3) -0.002(2) -0.011(3) -0.014(3) C3C 0.063(4) 0.040(3) 0.030(3) -0.005(3) 0.009(3) -0.012(3) C4C 0.058(4) 0.040(3) 0.030(3) 0.000(3) 0.007(3) -0.004(3) C5C 0.064(4) 0.033(3) 0.035(3) -0.007(3) 0.009(3) 0.000(3) C6C 0.066(5) 0.043(3) 0.032(3) -0.004(3) -0.016(3) -0.003(3) C7C 0.096(6) 0.039(3) 0.034(4) 0.003(3) 0.002(4) -0.016(3) C8C 0.100(6) 0.047(3) 0.021(3) 0.001(3) 0.009(3) -0.019(4) C9C 0.083(6) 0.049(4) 0.019(3) -0.006(3) 0.005(3) -0.018(4) C10C 0.060(5) 0.060(4) 0.045(4) -0.003(3) 0.022(3) -0.010(4) C11C 0.062(5) 0.058(4) 0.046(4) -0.008(3) 0.016(3) 0.000(3) C12C 0.060(5) 0.047(4) 0.040(4) -0.001(3) 0.009(3) 0.003(3) C13C 0.045(4) 0.052(4) 0.044(4) 0.003(3) 0.006(3) -0.010(3) C14C 0.094(6) 0.063(4) 0.027(3) 0.000(3) -0.001(3) -0.033(4) C15C 0.043(3) 0.033(3) 0.032(3) 0.002(2) 0.008(2) -0.004(3) C1D 0.033(3) 0.049(4) 0.035(3) -0.007(3) 0.001(3) 0.002(3) C2D 0.038(3) 0.044(3) 0.036(3) -0.006(3) 0.002(3) 0.002(2) C3D 0.033(3) 0.047(3) 0.040(3) -0.003(3) 0.003(3) 0.004(3) C4D 0.048(4) 0.056(4) 0.032(3) -0.003(3) 0.007(3) 0.000(3) C5D 0.042(4) 0.050(4) 0.034(3) -0.013(3) -0.002(3) -0.001(3) C6D 0.046(4) 0.055(4) 0.036(3) -0.008(3) 0.005(3) 0.002(3) C7D 0.063(4) 0.044(3) 0.056(4) -0.010(3) 0.003(4) 0.016(3) C8D 0.070(5) 0.047(4) 0.040(4) 0.004(3) -0.006(3) 0.014(3) C9D 0.057(4) 0.058(4) 0.029(3) 0.005(3) 0.006(3) 0.007(3) C10D 0.081(6) 0.069(5) 0.033(4) 0.008(3) 0.004(4) 0.023(4) C11D 0.120(8) 0.069(5) 0.034(4) -0.003(4) -0.015(4) 0.023(5) C12D 0.081(6) 0.067(5) 0.034(4) -0.007(3) -0.005(4) 0.016(4) C13D 0.052(4) 0.044(3) 0.028(3) 0.002(2) 0.006(3) -0.006(3) C14D 0.049(4) 0.058(4) 0.059(5) 0.008(3) 0.008(3) -0.011(3) C15D 0.066(4) 0.035(3) 0.022(3) 0.000(2) 0.008(3) -0.009(3) C61 0.088(6) 0.045(3) 0.059(5) 0.005(3) 0.028(4) -0.011(4) C62 0.092(8) 0.054(5) 0.182(13) -0.022(6) 0.029(8) -0.024(5) C63 0.119(10) 0.060(6) 0.210(16) -0.004(8) 0.075(10) -0.014(6) C64 0.141(10) 0.050(5) 0.127(9) -0.008(6) 0.001(9) 0.027(6) C65 0.081(5) 0.046(3) 0.040(4) -0.001(3) 0.003(4) 0.018(3) N1A 0.049(3) 0.042(3) 0.031(3) -0.006(2) 0.000(2) -0.004(2) N1B 0.043(3) 0.045(3) 0.041(3) 0.002(2) 0.008(2) 0.003(2) N1C 0.055(3) 0.039(3) 0.026(2) -0.0048(19) -0.003(2) -0.009(2) N1D 0.046(3) 0.042(3) 0.026(3) -0.0026(19) 0.001(2) 0.002(2) N5 0.054(3) 0.023(2) 0.028(2) -0.0047(19) 0.015(2) -0.002(2) O1A 0.052(3) 0.081(3) 0.036(2) -0.001(2) -0.012(2) 0.004(3) O2A 0.047(3) 0.037(2) 0.043(2) -0.0068(19) 0.0002(19) -0.006(2) O3A 0.069(3) 0.030(2) 0.0211(18) -0.0038(16) 0.0082(18) 0.0060(19) O4A 0.049(3) 0.037(2) 0.035(2) -0.0077(17) 0.0058(18) -0.0016(18) O1B 0.057(3) 0.060(3) 0.051(3) 0.006(2) 0.017(2) 0.011(2) O2B 0.063(3) 0.048(3) 0.044(3) 0.008(2) 0.000(2) 0.002(2) O3B 0.054(3) 0.041(2) 0.040(2) -0.0048(18) 0.0149(19) 0.005(2) O4B 0.033(2) 0.033(2) 0.057(3) -0.0026(18) 0.0093(19) 0.0029(17) O1C 0.046(3) 0.050(3) 0.057(3) -0.001(2) -0.014(2) -0.008(2) O2C 0.065(3) 0.048(2) 0.031(2) 0.0046(19) 0.007(2) -0.002(2) O3C 0.055(3) 0.038(2) 0.034(2) -0.0033(18) 0.0071(19) -0.0099(19) O4C 0.050(2) 0.038(2) 0.028(2) -0.0024(17) 0.0022(17) -0.0104(19) O1D 0.079(4) 0.052(3) 0.026(2) -0.0057(19) 0.007(2) 0.006(2) O2D 0.070(3) 0.042(2) 0.038(2) -0.0109(19) -0.003(2) 0.005(2) O3D 0.048(3) 0.038(2) 0.035(2) 0.0039(17) 0.0118(18) 0.0037(18) O4D 0.041(2) 0.035(2) 0.034(2) 0.0004(17) 0.0067(17) 0.0015(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3A 1.931(4) . ? Cu1 O3C 1.941(4) . ? Cu1 O3D 2.002(4) . ? Cu1 O3B 2.023(4) . ? Cu1 O17A 2.185(4) . ? Cu1 Cu2 2.6270(8) . ? Cu2 O4D 1.896(4) . ? Cu2 O4B 1.917(4) . ? Cu2 O4C 2.006(4) . ? Cu2 O4A 2.011(4) . ? Cu2 N5 2.183(4) . ? C1A O1A 1.233(8) . ? C1A N1A 1.419(8) . ? C1A C2A 1.454(9) . ? C2A C6A 1.384(9) . ? C2A C3A 1.422(10) . ? C3A C4A 1.376(9) . ? C3A C9A 1.445(9) . ? C4A C12A 1.381(10) . ? C4A C5A 1.478(8) . ? C5A O2A 1.227(7) . ? C5A N1A 1.398(8) . ? C6A C7A 1.381(11) . ? C6A H6A 0.9500 . ? C7A C8A 1.403(13) . ? C7A H7A 0.9500 . ? C8A C9A 1.404(12) . ? C8A H8A 0.9500 . ? C9A C10A 1.415(12) . ? C10A C11A 1.335(12) . ? C10A H10A 0.9500 . ? C11A C12A 1.406(10) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A N1A 1.465(7) . ? C13A C14A 1.525(9) . ? C13A C15A 1.533(9) . ? C13A H13A 1.0000 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C15A O3A 1.249(7) . ? C15A O4A 1.258(7) . ? C1B O1B 1.225(8) . ? C1B N1B 1.394(8) . ? C1B C2B 1.473(10) . ? C2B C6B 1.397(10) . ? C2B C3B 1.402(10) . ? C3B C4B 1.407(10) . ? C3B C9B 1.429(11) . ? C4B C12B 1.348(11) . ? C4B C5B 1.498(10) . ? C5B O2B 1.196(8) . ? C5B N1B 1.388(8) . ? C6B C7B 1.397(11) . ? C6B H6B 0.9500 . ? C7B C8B 1.347(13) . ? C7B H7B 0.9500 . ? C8B C9B 1.427(12) . ? C8B H8B 0.9500 . ? C9B C10B 1.399(13) . ? C10B C11B 1.362(13) . ? C10B H10B 0.9500 . ? C11B C12B 1.430(12) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B N1B 1.486(8) . ? C13B C14B 1.537(9) . ? C13B C15B 1.539(9) . ? C13B H13B 1.0000 . ? C14B H14D 0.9800 . ? C14B H14F 0.9800 . ? C14B H14E 0.9800 . ? C15B O3B 1.238(7) . ? C15B O4B 1.253(7) . ? C1C O1C 1.229(9) . ? C1C N1C 1.380(8) . ? C1C C2C 1.510(10) . ? C2C C6C 1.349(9) . ? C2C C3C 1.388(10) . ? C3C C4C 1.434(9) . ? C3C C9C 1.459(9) . ? C4C C12C 1.368(10) . ? C4C C5C 1.453(9) . ? C5C O2C 1.243(7) . ? C5C N1C 1.393(9) . ? C6C C7C 1.437(10) . ? C6C H6C 0.9500 . ? C7C C8C 1.363(11) . ? C7C H7C 0.9500 . ? C8C C9C 1.423(10) . ? C8C H8C 0.9500 . ? C9C C10C 1.369(11) . ? C10C C11C 1.382(10) . ? C10C H10C 0.9500 . ? C11C C12C 1.404(10) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C N1C 1.498(8) . ? C13C C14C 1.499(9) . ? C13C C15C 1.524(9) . ? C13C H13C 1.0000 . ? C14C H14G 0.9800 . ? C14C H14I 0.9800 . ? C14C H14H 0.9800 . ? C15C O3C 1.252(7) . ? C15C O4C 1.261(7) . ? C1D O1D 1.239(7) . ? C1D N1D 1.363(8) . ? C1D C2D 1.489(9) . ? C2D C6D 1.385(9) . ? C2D C3D 1.409(9) . ? C3D C9D 1.419(9) . ? C3D C4D 1.424(9) . ? C4D C12D 1.369(9) . ? C4D C5D 1.450(9) . ? C5D O2D 1.204(7) . ? C5D N1D 1.439(8) . ? C6D C7D 1.367(9) . ? C6D H6D 0.9500 . ? C7D C8D 1.370(10) . ? C7D H7D 0.9500 . ? C8D C9D 1.415(9) . ? C8D H8D 0.9500 . ? C9D C10D 1.397(9) . ? C10D C11D 1.341(10) . ? C10D H10D 0.9500 . ? C11D C12D 1.392(10) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D N1D 1.504(8) . ? C13D C15D 1.510(9) . ? C13D C14D 1.542(9) . ? C13D H13D 1.0000 . ? C14D H14J 0.9800 . ? C14D H14L 0.9800 . ? C14D H14K 0.9800 . ? C15D O3D 1.247(7) . ? C15D O4D 1.263(7) . ? C61 C62 1.333(11) . ? C61 N5 1.378(9) . ? C61 H61 0.9500 . ? C62 C63 1.288(16) . ? C62 H62 0.9500 . ? C63 C64 1.339(16) . ? C63 H63 0.9500 . ? C64 C65 1.325(11) . ? C64 H64 0.9500 . ? C65 N5 1.355(8) . ? C65 H65 0.9500 . ? C66A O17A 1.426(9) . ? C66A C67A 1.479(10) . ? C66A H66A 0.9900 . ? C66A H66B 0.9900 . ? C67A C68A 1.467(10) . ? C67A H67A 0.9900 . ? C67A H67B 0.9900 . ? C68A C69A 1.481(10) . ? C68A H68A 0.9900 . ? C68A H68B 0.9900 . ? C69A O17A 1.425(10) . ? C69A H69A 0.9900 . ? C69A H69B 0.9900 . ? C66B C67B 1.467(10) . ? C66B H66C 0.9900 . ? C66B H66D 0.9900 . ? C67B C68B 1.484(10) . ? C67B H67C 0.9900 . ? C67B H67D 0.9900 . ? C68B C69B 1.475(10) . ? C68B H68C 0.9900 . ? C68B H68D 0.9900 . ? C69B H69C 0.9900 . ? C69B H69D 0.9900 . ? O71 C74 1.395(12) . ? O71 C71 1.425(12) . ? C71 C72 1.493(13) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.478(13) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.441(13) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? O81 C81 1.411(14) . ? O81 C84 1.422(14) . ? C81 C82 1.429(14) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.476(15) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.486(14) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? O82 C85 1.435(14) . ? O82 C88 1.438(13) . ? C85 C86 1.482(14) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C87 1.483(14) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.472(14) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? O91 C91 1.398(14) . ? O91 C94 1.434(14) . ? C91 C92 1.472(14) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 C93 1.479(14) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C94 1.485(15) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.541(15) . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 C97 1.542(15) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 C98 1.520(14) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C99 1.518(15) . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 C100 1.552(15) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C100 H101 0.9800 . ? C100 H101 0.9800 . ? C100 H101 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3A Cu1 O3C 174.63(17) . . ? O3A Cu1 O3D 89.40(17) . . ? O3C Cu1 O3D 90.00(18) . . ? O3A Cu1 O3B 89.30(18) . . ? O3C Cu1 O3B 89.93(18) . . ? O3D Cu1 O3B 165.26(17) . . ? O3A Cu1 O17A 92.87(16) . . ? O3C Cu1 O17A 92.51(17) . . ? O3D Cu1 O17A 98.55(17) . . ? O3B Cu1 O17A 96.17(17) . . ? O3A Cu1 Cu2 87.89(11) . . ? O3C Cu1 Cu2 86.73(12) . . ? O3D Cu1 Cu2 84.03(12) . . ? O3B Cu1 Cu2 81.25(12) . . ? O17A Cu1 Cu2 177.31(13) . . ? O4D Cu2 O4B 172.16(17) . . ? O4D Cu2 O4C 90.88(17) . . ? O4B Cu2 O4C 87.50(18) . . ? O4D Cu2 O4A 90.62(17) . . ? O4B Cu2 O4A 88.67(18) . . ? O4C Cu2 O4A 162.72(16) . . ? O4D Cu2 N5 93.31(17) . . ? O4B Cu2 N5 94.50(17) . . ? O4C Cu2 N5 97.16(17) . . ? O4A Cu2 N5 99.94(17) . . ? O4D Cu2 Cu1 84.51(12) . . ? O4B Cu2 Cu1 87.67(12) . . ? O4C Cu2 Cu1 81.75(11) . . ? O4A Cu2 Cu1 81.26(11) . . ? N5 Cu2 Cu1 177.54(14) . . ? O1A C1A N1A 118.7(6) . . ? O1A C1A C2A 124.3(6) . . ? N1A C1A C2A 116.9(6) . . ? C6A C2A C3A 119.9(7) . . ? C6A C2A C1A 119.6(7) . . ? C3A C2A C1A 120.6(6) . . ? C4A C3A C2A 121.0(6) . . ? C4A C3A C9A 120.7(7) . . ? C2A C3A C9A 118.2(6) . . ? C3A C4A C12A 120.5(6) . . ? C3A C4A C5A 120.2(6) . . ? C12A C4A C5A 119.3(6) . . ? O2A C5A N1A 118.4(5) . . ? O2A C5A C4A 123.8(6) . . ? N1A C5A C4A 117.8(6) . . ? C7A C6A C2A 121.9(8) . . ? C7A C6A H6A 119.0 . . ? C2A C6A H6A 119.0 . . ? C6A C7A C8A 120.2(7) . . ? C6A C7A H7A 119.9 . . ? C8A C7A H7A 119.9 . . ? C7A C8A C9A 119.8(7) . . ? C7A C8A H8A 120.1 . . ? C9A C8A H8A 120.1 . . ? C8A C9A C10A 123.3(7) . . ? C8A C9A C3A 119.9(8) . . ? C10A C9A C3A 116.8(7) . . ? C11A C10A C9A 120.9(7) . . ? C11A C10A H10A 119.6 . . ? C9A C10A H10A 119.6 . . ? C10A C11A C12A 122.5(8) . . ? C10A C11A H11A 118.8 . . ? C12A C11A H11A 118.8 . . ? C4A C12A C11A 118.7(7) . . ? C4A C12A H12A 120.7 . . ? C11A C12A H12A 120.7 . . ? N1A C13A C14A 111.2(5) . . ? N1A C13A C15A 112.0(5) . . ? C14A C13A C15A 115.3(5) . . ? N1A C13A H13A 105.8 . . ? C14A C13A H13A 105.8 . . ? C15A C13A H13A 105.8 . . ? C13A C14A H14A 109.5 . . ? C13A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C13A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? O3A C15A O4A 127.9(6) . . ? O3A C15A C13A 115.0(5) . . ? O4A C15A C13A 117.0(6) . . ? O1B C1B N1B 120.0(7) . . ? O1B C1B C2B 123.1(6) . . ? N1B C1B C2B 116.9(6) . . ? C6B C2B C3B 119.7(7) . . ? C6B C2B C1B 119.4(7) . . ? C3B C2B C1B 120.8(6) . . ? C2B C3B C4B 120.1(7) . . ? C2B C3B C9B 120.9(7) . . ? C4B C3B C9B 119.0(8) . . ? C12B C4B C3B 120.6(7) . . ? C12B C4B C5B 118.6(7) . . ? C3B C4B C5B 120.7(7) . . ? O2B C5B N1B 123.0(6) . . ? O2B C5B C4B 121.2(6) . . ? N1B C5B C4B 115.8(6) . . ? C2B C6B C7B 119.6(8) . . ? C2B C6B H6B 120.2 . . ? C7B C6B H6B 120.2 . . ? C8B C7B C6B 121.3(8) . . ? C8B C7B H7B 119.4 . . ? C6B C7B H7B 119.4 . . ? C7B C8B C9B 121.9(8) . . ? C7B C8B H8B 119.1 . . ? C9B C8B H8B 119.1 . . ? C10B C9B C8B 124.8(8) . . ? C10B C9B C3B 118.6(8) . . ? C8B C9B C3B 116.6(8) . . ? C11B C10B C9B 121.8(8) . . ? C11B C10B H10B 119.1 . . ? C9B C10B H10B 119.1 . . ? C10B C11B C12B 118.7(9) . . ? C10B C11B H11B 120.7 . . ? C12B C11B H11B 120.7 . . ? C4B C12B C11B 121.1(8) . . ? C4B C12B H12B 119.4 . . ? C11B C12B H12B 119.4 . . ? N1B C13B C14B 113.8(6) . . ? N1B C13B C15B 108.2(5) . . ? C14B C13B C15B 114.2(6) . . ? N1B C13B H13B 106.7 . . ? C14B C13B H13B 106.7 . . ? C15B C13B H13B 106.7 . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? C13B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? H14F C14B H14E 109.5 . . ? O3B C15B O4B 128.6(6) . . ? O3B C15B C13B 119.4(5) . . ? O4B C15B C13B 112.0(5) . . ? O1C C1C N1C 121.1(6) . . ? O1C C1C C2C 121.8(6) . . ? N1C C1C C2C 117.0(6) . . ? C6C C2C C3C 122.6(6) . . ? C6C C2C C1C 118.3(7) . . ? C3C C2C C1C 119.0(6) . . ? C2C C3C C4C 122.1(6) . . ? C2C C3C C9C 120.2(6) . . ? C4C C3C C9C 117.7(6) . . ? C12C C4C C3C 119.1(6) . . ? C12C C4C C5C 122.6(6) . . ? C3C C4C C5C 118.3(6) . . ? O2C C5C N1C 119.5(6) . . ? O2C C5C C4C 121.4(7) . . ? N1C C5C C4C 119.1(6) . . ? C2C C6C C7C 118.4(7) . . ? C2C C6C H6C 120.8 . . ? C7C C6C H6C 120.8 . . ? C8C C7C C6C 121.1(7) . . ? C8C C7C H7C 119.5 . . ? C6C C7C H7C 119.5 . . ? C7C C8C C9C 121.6(7) . . ? C7C C8C H8C 119.2 . . ? C9C C8C H8C 119.2 . . ? C10C C9C C8C 123.5(7) . . ? C10C C9C C3C 120.4(7) . . ? C8C C9C C3C 116.1(7) . . ? C9C C10C C11C 120.7(7) . . ? C9C C10C H10C 119.7 . . ? C11C C10C H10C 119.7 . . ? C10C C11C C12C 119.9(7) . . ? C10C C11C H11C 120.1 . . ? C12C C11C H11C 120.1 . . ? C4C C12C C11C 122.1(7) . . ? C4C C12C H12C 118.9 . . ? C11C C12C H12C 118.9 . . ? N1C C13C C14C 111.5(5) . . ? N1C C13C C15C 110.4(5) . . ? C14C C13C C15C 114.8(5) . . ? N1C C13C H13C 106.5 . . ? C14C C13C H13C 106.5 . . ? C15C C13C H13C 106.5 . . ? C13C C14C H14G 109.5 . . ? C13C C14C H14I 109.5 . . ? H14G C14C H14I 109.5 . . ? C13C C14C H14H 109.5 . . ? H14G C14C H14H 109.5 . . ? H14I C14C H14H 109.5 . . ? O3C C15C O4C 125.7(5) . . ? O3C C15C C13C 116.2(5) . . ? O4C C15C C13C 118.0(5) . . ? O1D C1D N1D 121.4(6) . . ? O1D C1D C2D 121.7(5) . . ? N1D C1D C2D 116.9(5) . . ? C6D C2D C3D 119.5(6) . . ? C6D C2D C1D 120.4(6) . . ? C3D C2D C1D 120.1(5) . . ? C2D C3D C9D 120.4(5) . . ? C2D C3D C4D 120.8(6) . . ? C9D C3D C4D 118.7(6) . . ? C12D C4D C3D 119.9(6) . . ? C12D C4D C5D 120.2(6) . . ? C3D C4D C5D 119.8(6) . . ? O2D C5D N1D 119.1(6) . . ? O2D C5D C4D 123.9(6) . . ? N1D C5D C4D 116.9(5) . . ? C7D C6D C2D 121.2(6) . . ? C7D C6D H6D 119.4 . . ? C2D C6D H6D 119.4 . . ? C6D C7D C8D 119.8(6) . . ? C6D C7D H7D 120.1 . . ? C8D C7D H7D 120.1 . . ? C7D C8D C9D 122.6(6) . . ? C7D C8D H8D 118.7 . . ? C9D C8D H8D 118.7 . . ? C10D C9D C8D 125.2(6) . . ? C10D C9D C3D 118.2(6) . . ? C8D C9D C3D 116.5(6) . . ? C11D C10D C9D 122.3(7) . . ? C11D C10D H10D 118.8 . . ? C9D C10D H10D 118.8 . . ? C10D C11D C12D 120.1(7) . . ? C10D C11D H11D 119.9 . . ? C12D C11D H11D 119.9 . . ? C4D C12D C11D 120.7(7) . . ? C4D C12D H12D 119.7 . . ? C11D C12D H12D 119.7 . . ? N1D C13D C15D 107.1(5) . . ? N1D C13D C14D 112.5(5) . . ? C15D C13D C14D 116.4(5) . . ? N1D C13D H13D 106.8 . . ? C15D C13D H13D 106.8 . . ? C14D C13D H13D 106.8 . . ? C13D C14D H14J 109.5 . . ? C13D C14D H14L 109.5 . . ? H14J C14D H14L 109.5 . . ? C13D C14D H14K 109.5 . . ? H14J C14D H14K 109.5 . . ? H14L C14D H14K 109.5 . . ? O3D C15D O4D 126.7(6) . . ? O3D C15D C13D 119.3(5) . . ? O4D C15D C13D 114.0(5) . . ? C62 C61 N5 119.5(9) . . ? C62 C61 H61 120.2 . . ? N5 C61 H61 120.2 . . ? C63 C62 C61 119.4(10) . . ? C63 C62 H62 120.3 . . ? C61 C62 H62 120.3 . . ? C62 C63 C64 125.5(10) . . ? C62 C63 H63 117.2 . . ? C64 C63 H63 117.2 . . ? C65 C64 C63 114.5(10) . . ? C65 C64 H64 122.7 . . ? C63 C64 H64 122.7 . . ? C64 C65 N5 124.3(9) . . ? C64 C65 H65 117.8 . . ? N5 C65 H65 117.8 . . ? C5A N1A C1A 123.2(5) . . ? C5A N1A C13A 117.8(5) . . ? C1A N1A C13A 118.6(5) . . ? C5B N1B C1B 125.7(6) . . ? C5B N1B C13B 113.8(5) . . ? C1B N1B C13B 117.7(6) . . ? C1C N1C C5C 124.5(6) . . ? C1C N1C C13C 117.2(6) . . ? C5C N1C C13C 118.3(5) . . ? C1D N1D C5D 124.9(5) . . ? C1D N1D C13D 118.3(5) . . ? C5D N1D C13D 114.7(5) . . ? C65 N5 C61 116.6(5) . . ? C65 N5 Cu2 121.2(4) . . ? C61 N5 Cu2 122.1(4) . . ? C15A O3A Cu1 119.7(4) . . ? C15A O4A Cu2 123.2(4) . . ? C15B O3B Cu1 122.4(4) . . ? C15B O4B Cu2 120.0(4) . . ? C15C O3C Cu1 121.2(4) . . ? C15C O4C Cu2 123.8(4) . . ? C15D O3D Cu1 119.8(4) . . ? C15D O4D Cu2 124.4(4) . . ? O17A C66A C67A 103.9(12) . . ? O17A C66A H66A 111.0 . . ? C67A C66A H66A 111.0 . . ? O17A C66A H66B 111.0 . . ? C67A C66A H66B 111.0 . . ? H66A C66A H66B 109.0 . . ? C68A C67A C66A 108.8(15) . . ? C68A C67A H67A 109.9 . . ? C66A C67A H67A 109.9 . . ? C68A C67A H67B 109.9 . . ? C66A C67A H67B 109.9 . . ? H67A C67A H67B 108.3 . . ? C67A C68A C69A 101.6(17) . . ? C67A C68A H68A 111.4 . . ? C69A C68A H68A 111.4 . . ? C67A C68A H68B 111.4 . . ? C69A C68A H68B 111.4 . . ? H68A C68A H68B 109.3 . . ? O17A C69A C68A 105.3(13) . . ? O17A C69A H69A 110.7 . . ? C68A C69A H69A 110.7 . . ? O17A C69A H69B 110.7 . . ? C68A C69A H69B 110.7 . . ? H69A C69A H69B 108.8 . . ? C69A O17A C66A 105.1(14) . . ? C69A O17A Cu1 123.5(15) . . ? C66A O17A Cu1 114.4(10) . . ? C67B C66B H66C 109.7 . . ? C67B C66B H66D 109.7 . . ? H66C C66B H66D 108.2 . . ? C66B C67B C68B 104.9(15) . . ? C66B C67B H67C 110.8 . . ? C68B C67B H67C 110.8 . . ? C66B C67B H67D 110.8 . . ? C68B C67B H67D 110.8 . . ? H67C C67B H67D 108.8 . . ? C69B C68B C67B 105.1(18) . . ? C69B C68B H68C 110.7 . . ? C67B C68B H68C 110.7 . . ? C69B C68B H68D 110.7 . . ? C67B C68B H68D 110.7 . . ? H68C C68B H68D 108.8 . . ? C68B C69B H69C 110.2 . . ? C68B C69B H69D 110.2 . . ? H69C C69B H69D 108.5 . . ? C74 O71 C71 107.9(12) . . ? O71 C71 C72 104.1(12) . . ? O71 C71 H71A 110.9 . . ? C72 C71 H71A 110.9 . . ? O71 C71 H71B 110.9 . . ? C72 C71 H71B 110.9 . . ? H71A C71 H71B 109.0 . . ? C73 C72 C71 107.6(12) . . ? C73 C72 H72A 110.2 . . ? C71 C72 H72A 110.2 . . ? C73 C72 H72B 110.2 . . ? C71 C72 H72B 110.2 . . ? H72A C72 H72B 108.5 . . ? C74 C73 C72 104.1(12) . . ? C74 C73 H73A 110.9 . . ? C72 C73 H73A 110.9 . . ? C74 C73 H73B 110.9 . . ? C72 C73 H73B 110.9 . . ? H73A C73 H73B 109.0 . . ? O71 C74 C73 109.3(13) . . ? O71 C74 H74A 109.8 . . ? C73 C74 H74A 109.8 . . ? O71 C74 H74B 109.8 . . ? C73 C74 H74B 109.8 . . ? H74A C74 H74B 108.3 . . ? C81 O81 C84 110.2(14) . . ? O81 C81 C82 107.9(15) . . ? O81 C81 H81A 110.1 . . ? C82 C81 H81A 110.1 . . ? O81 C81 H81B 110.1 . . ? C82 C81 H81B 110.1 . . ? H81A C81 H81B 108.4 . . ? C81 C82 C83 107.3(15) . . ? C81 C82 H82A 110.3 . . ? C83 C82 H82A 110.3 . . ? C81 C82 H82B 110.3 . . ? C83 C82 H82B 110.3 . . ? H82A C82 H82B 108.5 . . ? C82 C83 C84 104.8(14) . . ? C82 C83 H83A 110.8 . . ? C84 C83 H83A 110.8 . . ? C82 C83 H83B 110.8 . . ? C84 C83 H83B 110.8 . . ? H83A C83 H83B 108.9 . . ? O81 C84 C83 106.7(15) . . ? O81 C84 H84A 110.4 . . ? C83 C84 H84A 110.4 . . ? O81 C84 H84B 110.4 . . ? C83 C84 H84B 110.4 . . ? H84A C84 H84B 108.6 . . ? C85 O82 C88 103.4(12) . . ? O82 C85 C86 103.4(13) . . ? O82 C85 H85A 111.1 . . ? C86 C85 H85A 111.1 . . ? O82 C85 H85B 111.1 . . ? C86 C85 H85B 111.1 . . ? H85A C85 H85B 109.0 . . ? C85 C86 C87 109.5(14) . . ? C85 C86 H86A 109.8 . . ? C87 C86 H86A 109.8 . . ? C85 C86 H86B 109.8 . . ? C87 C86 H86B 109.8 . . ? H86A C86 H86B 108.2 . . ? C88 C87 C86 97.7(17) . . ? C88 C87 H87A 112.2 . . ? C86 C87 H87A 112.2 . . ? C88 C87 H87B 112.2 . . ? C86 C87 H87B 112.2 . . ? H87A C87 H87B 109.8 . . ? O82 C88 C87 105.0(14) . . ? O82 C88 H88A 110.7 . . ? C87 C88 H88A 110.7 . . ? O82 C88 H88B 110.7 . . ? C87 C88 H88B 110.7 . . ? H88A C88 H88B 108.8 . . ? C91 O91 C94 96(2) . . ? O91 C91 C92 102.7(13) . . ? O91 C91 H91A 111.2 . . ? C92 C91 H91A 111.2 . . ? O91 C91 H91B 111.2 . . ? C92 C91 H91B 111.2 . . ? H91A C91 H91B 109.1 . . ? C91 C92 C93 102.2(13) . . ? C91 C92 H92A 111.3 . . ? C93 C92 H92A 111.3 . . ? C91 C92 H92B 111.3 . . ? C93 C92 H92B 111.3 . . ? H92A C92 H92B 109.2 . . ? C92 C93 C94 101.9(15) . . ? C92 C93 H93A 111.4 . . ? C94 C93 H93A 111.4 . . ? C92 C93 H93B 111.4 . . ? C94 C93 H93B 111.4 . . ? H93A C93 H93B 109.3 . . ? O91 C94 C93 104.0(14) . . ? O91 C94 H94A 111.0 . . ? C93 C94 H94A 111.0 . . ? O91 C94 H94B 111.0 . . ? C93 C94 H94B 111.0 . . ? H94A C94 H94B 109.0 . . ? C96 C95 H95A 109.5 . . ? C96 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C96 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C95 C96 C97 109.0(14) . . ? C95 C96 H96A 109.9 . . ? C97 C96 H96A 109.9 . . ? C95 C96 H96B 109.9 . . ? C97 C96 H96B 109.9 . . ? H96A C96 H96B 108.3 . . ? C98 C97 C96 112.2(15) . . ? C98 C97 H97A 109.2 . . ? C96 C97 H97A 109.2 . . ? C98 C97 H97B 109.2 . . ? C96 C97 H97B 109.2 . . ? H97A C97 H97B 107.9 . . ? C99 C98 C97 112.3(14) . . ? C99 C98 H98A 109.1 . . ? C97 C98 H98A 109.1 . . ? C99 C98 H98B 109.1 . . ? C97 C98 H98B 109.1 . . ? H98A C98 H98B 107.9 . . ? C98 C99 C100 109.0(14) . . ? C98 C99 H99A 109.9 . . ? C100 C99 H99A 109.9 . . ? C98 C99 H99B 109.9 . . ? C100 C99 H99B 109.9 . . ? H99A C99 H99B 108.3 . . ? C99 C100 H101 109.5 . . ? C99 C100 H102 109.5 . . ? H101 C100 H102 109.5 . . ? C99 C100 H103 109.5 . . ? H101 C100 H103 109.5 . . ? H102 C100 H103 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3A Cu1 Cu2 O4D -93.65(18) . . . . ? O3C Cu1 Cu2 O4D 86.31(18) . . . . ? O3D Cu1 Cu2 O4D -4.03(17) . . . . ? O3B Cu1 Cu2 O4D 176.74(18) . . . . ? O3A Cu1 Cu2 O4B 86.85(19) . . . . ? O3C Cu1 Cu2 O4B -93.20(19) . . . . ? O3D Cu1 Cu2 O4B 176.46(18) . . . . ? O3B Cu1 Cu2 O4B -2.77(18) . . . . ? O3A Cu1 Cu2 O4C 174.66(18) . . . . ? O3C Cu1 Cu2 O4C -5.39(17) . . . . ? O3D Cu1 Cu2 O4C -95.73(17) . . . . ? O3B Cu1 Cu2 O4C 85.04(17) . . . . ? O3A Cu1 Cu2 O4A -2.17(18) . . . . ? O3C Cu1 Cu2 O4A 177.78(18) . . . . ? O3D Cu1 Cu2 O4A 87.45(17) . . . . ? O3B Cu1 Cu2 O4A -91.78(18) . . . . ? O1A C1A C2A C6A 2.5(9) . . . . ? N1A C1A C2A C6A -175.1(5) . . . . ? O1A C1A C2A C3A -177.5(6) . . . . ? N1A C1A C2A C3A 5.0(8) . . . . ? C6A C2A C3A C4A 178.3(6) . . . . ? C1A C2A C3A C4A -1.8(9) . . . . ? C6A C2A C3A C9A 1.8(8) . . . . ? C1A C2A C3A C9A -178.3(5) . . . . ? C2A C3A C4A C12A -178.9(6) . . . . ? C9A C3A C4A C12A -2.5(9) . . . . ? C2A C3A C4A C5A 0.2(9) . . . . ? C9A C3A C4A C5A 176.6(5) . . . . ? C3A C4A C5A O2A 179.3(6) . . . . ? C12A C4A C5A O2A -1.6(9) . . . . ? C3A C4A C5A N1A -2.0(8) . . . . ? C12A C4A C5A N1A 177.1(6) . . . . ? C3A C2A C6A C7A -2.3(9) . . . . ? C1A C2A C6A C7A 177.8(6) . . . . ? C2A C6A C7A C8A 1.5(11) . . . . ? C6A C7A C8A C9A -0.3(11) . . . . ? C7A C8A C9A C10A 179.8(7) . . . . ? C7A C8A C9A C3A -0.2(10) . . . . ? C4A C3A C9A C8A -177.1(6) . . . . ? C2A C3A C9A C8A -0.6(9) . . . . ? C4A C3A C9A C10A 2.9(9) . . . . ? C2A C3A C9A C10A 179.4(6) . . . . ? C8A C9A C10A C11A 178.4(7) . . . . ? C3A C9A C10A C11A -1.6(10) . . . . ? C9A C10A C11A C12A 0.0(12) . . . . ? C3A C4A C12A C11A 0.7(10) . . . . ? C5A C4A C12A C11A -178.4(6) . . . . ? C10A C11A C12A C4A 0.6(12) . . . . ? N1A C13A C15A O3A -143.7(6) . . . . ? C14A C13A C15A O3A -15.2(8) . . . . ? N1A C13A C15A O4A 39.8(8) . . . . ? C14A C13A C15A O4A 168.4(6) . . . . ? O1B C1B C2B C6B 0.2(10) . . . . ? N1B C1B C2B C6B -176.0(6) . . . . ? O1B C1B C2B C3B 175.6(7) . . . . ? N1B C1B C2B C3B -0.6(10) . . . . ? C6B C2B C3B C4B 176.9(7) . . . . ? C1B C2B C3B C4B 1.6(11) . . . . ? C6B C2B C3B C9B -1.5(12) . . . . ? C1B C2B C3B C9B -176.8(7) . . . . ? C2B C3B C4B C12B -179.3(8) . . . . ? C9B C3B C4B C12B -0.8(12) . . . . ? C2B C3B C4B C5B -2.4(11) . . . . ? C9B C3B C4B C5B 176.0(7) . . . . ? C12B C4B C5B O2B -1.2(11) . . . . ? C3B C4B C5B O2B -178.2(7) . . . . ? C12B C4B C5B N1B 179.1(7) . . . . ? C3B C4B C5B N1B 2.2(10) . . . . ? C3B C2B C6B C7B 3.0(11) . . . . ? C1B C2B C6B C7B 178.4(7) . . . . ? C2B C6B C7B C8B -1.7(13) . . . . ? C6B C7B C8B C9B -1.1(15) . . . . ? C7B C8B C9B C10B 179.8(10) . . . . ? C7B C8B C9B C3B 2.6(14) . . . . ? C2B C3B C9B C10B -178.7(9) . . . . ? C4B C3B C9B C10B 2.9(13) . . . . ? C2B C3B C9B C8B -1.2(12) . . . . ? C4B C3B C9B C8B -179.6(8) . . . . ? C8B C9B C10B C11B 178.4(10) . . . . ? C3B C9B C10B C11B -4.4(16) . . . . ? C9B C10B C11B C12B 3.7(17) . . . . ? C3B C4B C12B C11B 0.1(14) . . . . ? C5B C4B C12B C11B -176.9(9) . . . . ? C10B C11B C12B C4B -1.4(16) . . . . ? N1B C13B C15B O3B -144.7(6) . . . . ? C14B C13B C15B O3B -16.9(8) . . . . ? N1B C13B C15B O4B 37.5(7) . . . . ? C14B C13B C15B O4B 165.3(6) . . . . ? O1C C1C C2C C6C 6.1(9) . . . . ? N1C C1C C2C C6C -178.2(5) . . . . ? O1C C1C C2C C3C -177.9(6) . . . . ? N1C C1C C2C C3C -2.1(8) . . . . ? C6C C2C C3C C4C 177.9(6) . . . . ? C1C C2C C3C C4C 2.0(9) . . . . ? C6C C2C C3C C9C -1.4(9) . . . . ? C1C C2C C3C C9C -177.3(5) . . . . ? C2C C3C C4C C12C 178.2(6) . . . . ? C9C C3C C4C C12C -2.6(9) . . . . ? C2C C3C C4C C5C -1.0(9) . . . . ? C9C C3C C4C C5C 178.3(5) . . . . ? C12C C4C C5C O2C 2.2(9) . . . . ? C3C C4C C5C O2C -178.7(5) . . . . ? C12C C4C C5C N1C -179.0(6) . . . . ? C3C C4C C5C N1C 0.1(8) . . . . ? C3C C2C C6C C7C -0.7(9) . . . . ? C1C C2C C6C C7C 175.2(5) . . . . ? C2C C6C C7C C8C 0.6(10) . . . . ? C6C C7C C8C C9C 1.6(10) . . . . ? C7C C8C C9C C10C 178.4(7) . . . . ? C7C C8C C9C C3C -3.5(9) . . . . ? C2C C3C C9C C10C -178.5(6) . . . . ? C4C C3C C9C C10C 2.2(9) . . . . ? C2C C3C C9C C8C 3.4(8) . . . . ? C4C C3C C9C C8C -175.9(5) . . . . ? C8C C9C C10C C11C 176.9(6) . . . . ? C3C C9C C10C C11C -1.0(10) . . . . ? C9C C10C C11C C12C 0.1(11) . . . . ? C3C C4C C12C C11C 1.8(10) . . . . ? C5C C4C C12C C11C -179.1(6) . . . . ? C10C C11C C12C C4C -0.5(11) . . . . ? N1C C13C C15C O3C -136.0(6) . . . . ? C14C C13C C15C O3C -8.9(8) . . . . ? N1C C13C C15C O4C 47.5(8) . . . . ? C14C C13C C15C O4C 174.5(6) . . . . ? O1D C1D C2D C6D -2.7(9) . . . . ? N1D C1D C2D C6D 177.7(6) . . . . ? O1D C1D C2D C3D 178.3(6) . . . . ? N1D C1D C2D C3D -1.3(8) . . . . ? C6D C2D C3D C9D 1.8(9) . . . . ? C1D C2D C3D C9D -179.3(6) . . . . ? C6D C2D C3D C4D -178.7(6) . . . . ? C1D C2D C3D C4D 0.3(9) . . . . ? C2D C3D C4D C12D -179.7(7) . . . . ? C9D C3D C4D C12D -0.2(10) . . . . ? C2D C3D C4D C5D -3.5(10) . . . . ? C9D C3D C4D C5D 176.1(6) . . . . ? C12D C4D C5D O2D 2.8(11) . . . . ? C3D C4D C5D O2D -173.4(6) . . . . ? C12D C4D C5D N1D -176.4(7) . . . . ? C3D C4D C5D N1D 7.3(9) . . . . ? C3D C2D C6D C7D -1.5(10) . . . . ? C1D C2D C6D C7D 179.6(6) . . . . ? C2D C6D C7D C8D -0.1(11) . . . . ? C6D C7D C8D C9D 1.5(12) . . . . ? C7D C8D C9D C10D 176.7(8) . . . . ? C7D C8D C9D C3D -1.1(11) . . . . ? C2D C3D C9D C10D -178.5(7) . . . . ? C4D C3D C9D C10D 1.9(10) . . . . ? C2D C3D C9D C8D -0.5(10) . . . . ? C4D C3D C9D C8D 179.9(6) . . . . ? C8D C9D C10D C11D -179.5(9) . . . . ? C3D C9D C10D C11D -1.7(13) . . . . ? C9D C10D C11D C12D -0.2(15) . . . . ? C3D C4D C12D C11D -1.8(12) . . . . ? C5D C4D C12D C11D -178.1(8) . . . . ? C10D C11D C12D C4D 2.1(15) . . . . ? N1D C13D C15D O3D -141.0(5) . . . . ? C14D C13D C15D O3D -14.2(8) . . . . ? N1D C13D C15D O4D 41.3(6) . . . . ? C14D C13D C15D O4D 168.1(5) . . . . ? N5 C61 C62 C63 -1.9(19) . . . . ? C61 C62 C63 C64 2(3) . . . . ? C62 C63 C64 C65 0(2) . . . . ? C63 C64 C65 N5 -2.1(17) . . . . ? O2A C5A N1A C1A -175.6(5) . . . . ? C4A C5A N1A C1A 5.6(8) . . . . ? O2A C5A N1A C13A -2.3(8) . . . . ? C4A C5A N1A C13A 178.9(5) . . . . ? O1A C1A N1A C5A 175.2(5) . . . . ? C2A C1A N1A C5A -7.1(8) . . . . ? O1A C1A N1A C13A 2.0(8) . . . . ? C2A C1A N1A C13A 179.7(5) . . . . ? C14A C13A N1A C5A -78.1(7) . . . . ? C15A C13A N1A C5A 52.6(7) . . . . ? C14A C13A N1A C1A 95.5(7) . . . . ? C15A C13A N1A C1A -133.8(6) . . . . ? O2B C5B N1B C1B 179.1(6) . . . . ? C4B C5B N1B C1B -1.3(10) . . . . ? O2B C5B N1B C13B 18.6(10) . . . . ? C4B C5B N1B C13B -161.7(6) . . . . ? O1B C1B N1B C5B -175.8(6) . . . . ? C2B C1B N1B C5B 0.5(9) . . . . ? O1B C1B N1B C13B -16.0(9) . . . . ? C2B C1B N1B C13B 160.3(6) . . . . ? C14B C13B N1B C5B -76.9(7) . . . . ? C15B C13B N1B C5B 51.2(7) . . . . ? C14B C13B N1B C1B 121.0(6) . . . . ? C15B C13B N1B C1B -111.0(6) . . . . ? O1C C1C N1C C5C 177.1(5) . . . . ? C2C C1C N1C C5C 1.3(8) . . . . ? O1C C1C N1C C13C -0.1(8) . . . . ? C2C C1C N1C C13C -175.9(5) . . . . ? O2C C5C N1C C1C 178.5(5) . . . . ? C4C C5C N1C C1C -0.4(8) . . . . ? O2C C5C N1C C13C -4.4(8) . . . . ? C4C C5C N1C C13C 176.8(5) . . . . ? C14C C13C N1C C1C 101.9(7) . . . . ? C15C C13C N1C C1C -129.2(6) . . . . ? C14C C13C N1C C5C -75.5(7) . . . . ? C15C C13C N1C C5C 53.4(7) . . . . ? O1D C1D N1D C5D -173.8(6) . . . . ? C2D C1D N1D C5D 5.7(9) . . . . ? O1D C1D N1D C13D -11.0(9) . . . . ? C2D C1D N1D C13D 168.5(5) . . . . ? O2D C5D N1D C1D 171.9(6) . . . . ? C4D C5D N1D C1D -8.8(9) . . . . ? O2D C5D N1D C13D 8.5(9) . . . . ? C4D C5D N1D C13D -172.2(5) . . . . ? C15D C13D N1D C1D -111.5(6) . . . . ? C14D C13D N1D C1D 119.4(6) . . . . ? C15D C13D N1D C5D 53.0(6) . . . . ? C14D C13D N1D C5D -76.1(7) . . . . ? C64 C65 N5 C61 1.8(12) . . . . ? C64 C65 N5 Cu2 179.7(8) . . . . ? C62 C61 N5 C65 0.3(11) . . . . ? C62 C61 N5 Cu2 -177.5(8) . . . . ? O4D Cu2 N5 C65 -17.9(5) . . . . ? O4B Cu2 N5 C65 161.4(5) . . . . ? O4C Cu2 N5 C65 73.4(5) . . . . ? O4A Cu2 N5 C65 -109.1(5) . . . . ? O4D Cu2 N5 C61 159.8(5) . . . . ? O4B Cu2 N5 C61 -20.8(5) . . . . ? O4C Cu2 N5 C61 -108.9(5) . . . . ? O4A Cu2 N5 C61 68.6(5) . . . . ? O4A C15A O3A Cu1 -0.4(9) . . . . ? C13A C15A O3A Cu1 -176.4(4) . . . . ? O3D Cu1 O3A C15A -82.0(5) . . . . ? O3B Cu1 O3A C15A 83.4(5) . . . . ? O17A Cu1 O3A C15A 179.5(4) . . . . ? Cu2 Cu1 O3A C15A 2.1(4) . . . . ? O3A C15A O4A Cu2 -2.6(9) . . . . ? C13A C15A O4A Cu2 173.3(4) . . . . ? O4D Cu2 O4A C15A 87.4(5) . . . . ? O4B Cu2 O4A C15A -84.8(5) . . . . ? O4C Cu2 O4A C15A -7.6(9) . . . . ? N5 Cu2 O4A C15A -179.2(5) . . . . ? Cu1 Cu2 O4A C15A 3.0(4) . . . . ? O4B C15B O3B Cu1 -2.1(9) . . . . ? C13B C15B O3B Cu1 -179.5(4) . . . . ? O3A Cu1 O3B C15B -84.7(5) . . . . ? O3C Cu1 O3B C15B 90.0(5) . . . . ? O3D Cu1 O3B C15B 0.3(10) . . . . ? O17A Cu1 O3B C15B -177.5(5) . . . . ? Cu2 Cu1 O3B C15B 3.3(4) . . . . ? O3B C15B O4B Cu2 -1.6(9) . . . . ? C13B C15B O4B Cu2 175.9(4) . . . . ? O4C Cu2 O4B C15B -78.7(5) . . . . ? O4A Cu2 O4B C15B 84.5(5) . . . . ? N5 Cu2 O4B C15B -175.7(5) . . . . ? Cu1 Cu2 O4B C15B 3.2(4) . . . . ? O4C C15C O3C Cu1 -9.8(8) . . . . ? C13C C15C O3C Cu1 174.0(4) . . . . ? O3D Cu1 O3C C15C 93.3(4) . . . . ? O3B Cu1 O3C C15C -72.0(5) . . . . ? O17A Cu1 O3C C15C -168.1(4) . . . . ? Cu2 Cu1 O3C C15C 9.3(4) . . . . ? O3C C15C O4C Cu2 2.5(8) . . . . ? C13C C15C O4C Cu2 178.7(4) . . . . ? O4D Cu2 O4C C15C -80.8(5) . . . . ? O4B Cu2 O4C C15C 91.6(5) . . . . ? O4A Cu2 O4C C15C 14.2(9) . . . . ? N5 Cu2 O4C C15C -174.2(5) . . . . ? Cu1 Cu2 O4C C15C 3.6(4) . . . . ? O4D C15D O3D Cu1 -7.7(8) . . . . ? C13D C15D O3D Cu1 175.0(4) . . . . ? O3A Cu1 O3D C15D 94.8(4) . . . . ? O3C Cu1 O3D C15D -79.9(4) . . . . ? O3B Cu1 O3D C15D 9.8(9) . . . . ? O17A Cu1 O3D C15D -172.4(4) . . . . ? Cu2 Cu1 O3D C15D 6.8(4) . . . . ? O3D C15D O4D Cu2 2.3(8) . . . . ? C13D C15D O4D Cu2 179.8(4) . . . . ? O4C Cu2 O4D C15D 84.2(4) . . . . ? O4A Cu2 O4D C15D -78.6(4) . . . . ? N5 Cu2 O4D C15D -178.6(4) . . . . ? Cu1 Cu2 O4D C15D 2.6(4) . . . . ? O17A C66A C67A C68A -11(2) . . . . ? C66A C67A C68A C69A -12(3) . . . . ? C67A C68A C69A O17A 32(3) . . . . ? C68A C69A O17A C66A -41(3) . . . . ? C68A C69A O17A Cu1 93(2) . . . . ? C67A C66A O17A C69A 32(2) . . . . ? C67A C66A O17A Cu1 -106.8(15) . . . . ? O3A Cu1 O17A C69A -175.3(9) . . . . ? O3C Cu1 O17A C69A 4.5(10) . . . . ? O3D Cu1 O17A C69A 94.8(10) . . . . ? O3B Cu1 O17A C69A -85.7(10) . . . . ? O3A Cu1 O17A C66A -45.4(8) . . . . ? O3C Cu1 O17A C66A 134.4(8) . . . . ? O3D Cu1 O17A C66A -135.2(8) . . . . ? O3B Cu1 O17A C66A 44.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.178 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.094 #===END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H64 Cu2 N4 O18, 2(C4 H8 O)' _chemical_formula_sum 'C96 H80 Cu2 N4 O20' _chemical_formula_weight 1736.72 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.0013(8) _cell_length_b 23.3563(12) _cell_length_c 23.8248(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.6580(10) _cell_angle_gamma 90.00 _cell_volume 8347.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8701 _cell_measurement_theta_min 2.210 _cell_measurement_theta_max 20.673 _exptl_crystal_description 'irregular, cleaved' _exptl_crystal_colour green-blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3608 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8292 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS Version 2.05 (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43700 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 22.59 _reflns_number_total 22082 _reflns_number_gt 17430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1387P)^2^+0.6425P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(13) _refine_ls_number_reflns 22082 _refine_ls_number_parameters 1969 _refine_ls_number_restraints 442 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.2014 _refine_ls_wR_factor_gt 0.1838 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.88092(6) 0.03894(4) 0.48205(4) 0.0393(2) Uani 1 1 d . . . Cu2 Cu 0.82097(6) 0.14248(4) 0.46214(4) 0.0384(2) Uani 1 1 d . C . Cu3 Cu 0.61105(7) 0.46678(5) 0.01316(4) 0.0582(3) Uani 1 1 d D . . Cu4 Cu 0.68114(6) 0.36569(5) 0.03169(4) 0.0485(3) Uani 1 1 d D A . C1A C 1.1322(5) 0.2630(3) 0.5180(4) 0.053(2) Uani 1 1 d D . . C2A C 1.1636(5) 0.3053(3) 0.4777(3) 0.050(2) Uani 1 1 d D . . C3A C 1.1620(5) 0.2939(3) 0.4197(3) 0.0469(19) Uani 1 1 d D . . C4A C 1.1375(5) 0.2391(3) 0.3996(3) 0.0461(19) Uani 1 1 d D . . C5A C 1.1121(5) 0.1939(3) 0.4393(3) 0.0449(19) Uani 1 1 d D . . C6A C 1.1945(5) 0.3576(4) 0.4974(4) 0.065(2) Uani 1 1 d D . . H6A H 1.1953 0.3654 0.5366 0.079 Uiso 1 1 calc R . . C7A C 1.2247(6) 0.3989(4) 0.4595(4) 0.069(3) Uani 1 1 d D . . H7A H 1.2482 0.4339 0.4734 0.083 Uiso 1 1 calc R . . C8A C 1.2210(6) 0.3896(3) 0.4020(5) 0.070(3) Uani 1 1 d D . . H8A H 1.2386 0.4188 0.3767 0.084 Uiso 1 1 calc R . . C9A C 1.1907(5) 0.3363(3) 0.3816(4) 0.061(2) Uani 1 1 d D . . C10A C 1.1896(6) 0.3224(4) 0.3230(4) 0.065(2) Uani 1 1 d D . . H10A H 1.2073 0.3504 0.2964 0.078 Uiso 1 1 calc R . . C11A C 1.1638(6) 0.2700(4) 0.3050(4) 0.061(2) Uani 1 1 d D . . H11A H 1.1639 0.2616 0.2660 0.073 Uiso 1 1 calc R . . C12A C 1.1370(6) 0.2278(4) 0.3431(4) 0.058(2) Uani 1 1 d D . . H12A H 1.1183 0.1914 0.3297 0.070 Uiso 1 1 calc R . . C13A C 1.0704(5) 0.1655(3) 0.5351(3) 0.0462(19) Uani 1 1 d . . . H13A H 1.0490 0.1883 0.5678 0.055 Uiso 1 1 calc R . . C20A C 0.9872(5) 0.1377(4) 0.5105(3) 0.0444(18) Uani 1 1 d . . . N1A N 1.1079(4) 0.2084(3) 0.4957(3) 0.0471(16) Uani 1 1 d . . . O1A O 1.1241(4) 0.2724(3) 0.5677(3) 0.0706(17) Uani 1 1 d . . . O2A O 1.0926(4) 0.1448(2) 0.4244(2) 0.0564(13) Uani 1 1 d . . . O3A O 0.9799(3) 0.0855(2) 0.5141(2) 0.0467(12) Uani 1 1 d . . . O4A O 0.9332(3) 0.1740(2) 0.4883(2) 0.0470(13) Uani 1 1 d . C . C14A C 1.1374(5) 0.1233(3) 0.5598(4) 0.050(2) Uani 1 1 d . . . C15A C 1.2111(6) 0.1039(4) 0.5310(5) 0.072(3) Uani 1 1 d . . . H15A H 1.2256 0.1195 0.4954 0.086 Uiso 1 1 calc R . . C16A C 1.2634(7) 0.0613(5) 0.5549(5) 0.081(3) Uani 1 1 d . . . H16A H 1.3137 0.0475 0.5353 0.097 Uiso 1 1 calc R C . C17A C 1.2443(8) 0.0392(5) 0.6051(6) 0.092(4) Uani 1 1 d . . . H17A H 1.2819 0.0107 0.6211 0.111 Uiso 1 1 calc R . . C18A C 1.1708(10) 0.0574(6) 0.6338(6) 0.114(5) Uani 1 1 d . . . H18A H 1.1556 0.0410 0.6688 0.137 Uiso 1 1 calc R C . C19A C 1.1201(8) 0.1000(5) 0.6103(5) 0.094(4) Uani 1 1 d . . . H19A H 1.0703 0.1137 0.6305 0.113 Uiso 1 1 calc R . . C1B C 0.9233(5) 0.1597(3) 0.2476(3) 0.0452(18) Uani 1 1 d . . . C2B C 0.8644(6) 0.1973(3) 0.2123(3) 0.050(2) Uani 1 1 d . . . C3B C 0.7744(6) 0.1836(3) 0.2058(3) 0.053(2) Uani 1 1 d . . . C4B C 0.7358(5) 0.1359(3) 0.2340(3) 0.052(2) Uani 1 1 d . . . C5B C 0.7908(5) 0.1024(3) 0.2724(3) 0.0440(18) Uani 1 1 d . . . C6B C 0.8992(6) 0.2448(3) 0.1882(3) 0.057(2) Uani 1 1 d . . . H6B H 0.9608 0.2534 0.1923 0.068 Uiso 1 1 calc R . . C7B C 0.8432(8) 0.2810(4) 0.1573(4) 0.066(2) Uani 1 1 d . . . H7B H 0.8665 0.3151 0.1414 0.080 Uiso 1 1 calc R . . C8B C 0.7591(8) 0.2684(4) 0.1502(3) 0.067(3) Uani 1 1 d . . . H8B H 0.7227 0.2938 0.1288 0.081 Uiso 1 1 calc R . . C9B C 0.7201(7) 0.2190(4) 0.1725(4) 0.061(2) Uani 1 1 d . . . C10B C 0.6279(7) 0.2045(5) 0.1648(4) 0.082(3) Uani 1 1 d . . . H10B H 0.5908 0.2277 0.1416 0.098 Uiso 1 1 calc R . . C11B C 0.5939(7) 0.1583(4) 0.1903(5) 0.077(3) Uani 1 1 d . . . H11B H 0.5332 0.1483 0.1840 0.092 Uiso 1 1 calc R . . C12B C 0.6469(6) 0.1245(4) 0.2262(4) 0.067(3) Uani 1 1 d . . . H12B H 0.6207 0.0932 0.2454 0.080 Uiso 1 1 calc R . . C13B C 0.9371(5) 0.0779(3) 0.3140(3) 0.0476(19) Uani 1 1 d . . . H13B H 0.9994 0.0930 0.3118 0.057 Uiso 1 1 calc R . . C14B C 0.9400(7) 0.0156(4) 0.2922(4) 0.064(3) Uani 1 1 d . . . C15B C 0.8905(7) -0.0263(4) 0.3123(4) 0.071(3) Uani 1 1 d . . . H15B H 0.8520 -0.0187 0.3428 0.085 Uiso 1 1 calc R . . C16B C 0.8936(9) -0.0824(5) 0.2895(5) 0.100(4) Uani 1 1 d . . . H16B H 0.8575 -0.1125 0.3035 0.120 Uiso 1 1 calc R . . C17B C 0.9540(14) -0.0909(6) 0.2444(5) 0.138(7) Uani 1 1 d . . . H17B H 0.9546 -0.1266 0.2252 0.166 Uiso 1 1 calc R . . C18B C 1.0111(12) -0.0485(6) 0.2284(6) 0.123(5) Uani 1 1 d . . . H18B H 1.0569 -0.0560 0.2022 0.148 Uiso 1 1 calc R . . C19B C 1.0009(8) 0.0049(5) 0.2507(4) 0.092(4) Uani 1 1 d . . . H19B H 1.0367 0.0354 0.2372 0.110 Uiso 1 1 calc R . . C20B C 0.9071(5) 0.0869(3) 0.3745(3) 0.0402(17) Uani 1 1 d . . . N1B N 0.8810(4) 0.1146(3) 0.2759(2) 0.0428(15) Uani 1 1 d . . . O1B O 1.0030(4) 0.1673(2) 0.2522(2) 0.0575(14) Uani 1 1 d . . . O2B O 0.7595(4) 0.0647(2) 0.3032(2) 0.0539(14) Uani 1 1 d . . . O3B O 0.9282(3) 0.0464(2) 0.4075(2) 0.0472(12) Uani 1 1 d . . . O4B O 0.8695(3) 0.1324(2) 0.3865(2) 0.0426(12) Uani 1 1 d . C . C1C C 0.5125(6) 0.1066(4) 0.3887(5) 0.063(2) Uani 1 1 d . . . C2C C 0.4592(5) 0.1539(4) 0.4113(5) 0.066(3) Uani 1 1 d . . . C3C C 0.4492(6) 0.1592(4) 0.4697(6) 0.069(3) Uani 1 1 d . . . C4C C 0.4859(6) 0.1208(4) 0.5067(4) 0.061(2) Uani 1 1 d . . . C5C C 0.5463(5) 0.0732(3) 0.4862(4) 0.048(2) Uani 1 1 d . . . C6C C 0.4248(6) 0.1934(5) 0.3757(7) 0.100(4) Uani 1 1 d . . . H6C H 0.4292 0.1885 0.3362 0.121 Uiso 1 1 calc R . . C7C C 0.3810(7) 0.2432(6) 0.3988(9) 0.117(6) Uani 1 1 d . . . H7C H 0.3604 0.2728 0.3745 0.141 Uiso 1 1 calc R . . C8C C 0.3694(9) 0.2478(7) 0.4549(11) 0.141(8) Uani 1 1 d . . . H8C H 0.3389 0.2804 0.4690 0.169 Uiso 1 1 calc R . . C9C C 0.4007(6) 0.2061(5) 0.4933(7) 0.085(4) Uani 1 1 d . . . C10C C 0.3874(8) 0.2119(6) 0.5488(9) 0.108(5) Uani 1 1 d . . . H10C H 0.3536 0.2431 0.5627 0.129 Uiso 1 1 calc R . . C11C C 0.4233(9) 0.1722(7) 0.5851(7) 0.110(5) Uani 1 1 d . . . H11C H 0.4138 0.1756 0.6244 0.132 Uiso 1 1 calc R . . C12C C 0.4752(6) 0.1258(5) 0.5638(6) 0.085(3) Uani 1 1 d . . . H12C H 0.5018 0.0988 0.5887 0.102 Uiso 1 1 calc R . . C13C C 0.6203(5) 0.0299(3) 0.4062(3) 0.0453(18) Uani 1 1 d . . . H13C H 0.6256 0.0380 0.3651 0.054 Uiso 1 1 calc R . . C14C C 0.5956(5) -0.0330(3) 0.4107(3) 0.0418(17) Uani 1 1 d . . . C15C C 0.5094(6) -0.0515(4) 0.4265(4) 0.069(3) Uani 1 1 d . . . H15C H 0.4667 -0.0239 0.4380 0.083 Uiso 1 1 calc R . . C16C C 0.4864(7) -0.1075(4) 0.4257(5) 0.084(3) Uani 1 1 d . . . H16C H 0.4291 -0.1189 0.4381 0.101 Uiso 1 1 calc R . . C17C C 0.5455(7) -0.1483(4) 0.4068(4) 0.068(3) Uani 1 1 d . . . H17C H 0.5282 -0.1874 0.4046 0.081 Uiso 1 1 calc R . . C18C C 0.6288(6) -0.1321(3) 0.3913(4) 0.060(2) Uani 1 1 d . . . H18C H 0.6706 -0.1600 0.3794 0.072 Uiso 1 1 calc R . . C19C C 0.6530(6) -0.0744(4) 0.3928(4) 0.063(2) Uani 1 1 d . . . H19C H 0.7109 -0.0636 0.3810 0.076 Uiso 1 1 calc R . . C20C C 0.7086(5) 0.0488(3) 0.4328(3) 0.0377(17) Uani 1 1 d . . . N1C N 0.5514(4) 0.0698(3) 0.4272(3) 0.0483(16) Uani 1 1 d . . . O1C O 0.5232(4) 0.0997(3) 0.3383(3) 0.0778(19) Uani 1 1 d . . . O2C O 0.5872(4) 0.0426(3) 0.5160(2) 0.0572(14) Uani 1 1 d . . . O3C O 0.7654(3) 0.0129(2) 0.4465(2) 0.0423(12) Uani 1 1 d . . . O4C O 0.7158(3) 0.1025(2) 0.4365(2) 0.0428(12) Uani 1 1 d . C . C1D C 0.6677(7) 0.1744(4) 0.6654(4) 0.061(2) Uani 1 1 d D . . C2D C 0.6688(8) 0.2344(4) 0.6783(4) 0.077(3) Uani 1 1 d D . . C3D C 0.7490(9) 0.2654(4) 0.6736(4) 0.086(4) Uani 1 1 d D . . C4D C 0.8290(8) 0.2409(4) 0.6566(3) 0.071(3) Uani 1 1 d D . . C5D C 0.8302(7) 0.1788(4) 0.6457(4) 0.065(3) Uani 1 1 d D . . C6D C 0.5924(9) 0.2619(5) 0.6947(4) 0.104(4) Uani 1 1 d D . . H6D H 0.5383 0.2411 0.6983 0.124 Uiso 1 1 calc R . . C7D C 0.5947(12) 0.3220(7) 0.7064(6) 0.125(7) Uani 1 1 d D . . H7D H 0.5411 0.3405 0.7171 0.150 Uiso 1 1 calc R . . C8D C 0.6664(14) 0.3524(6) 0.7029(6) 0.132(8) Uani 1 1 d D . . H8D H 0.6654 0.3918 0.7128 0.159 Uiso 1 1 calc R . . C9D C 0.7417(12) 0.3286(4) 0.6856(4) 0.102(5) Uani 1 1 d D . . C10D C 0.8202(14) 0.3557(6) 0.6810(6) 0.144(8) Uani 1 1 d D . . H10D H 0.8216 0.3949 0.6918 0.172 Uiso 1 1 calc R . . C11D C 0.8989(13) 0.3325(6) 0.6624(6) 0.142(8) Uani 1 1 d D . . H11D H 0.9498 0.3560 0.6572 0.171 Uiso 1 1 calc R . . C12D C 0.9032(9) 0.2717(4) 0.6508(4) 0.099(4) Uani 1 1 d D . . H12D H 0.9572 0.2543 0.6394 0.119 Uiso 1 1 calc R . . C13D C 0.7449(6) 0.0906(3) 0.6277(3) 0.056(2) Uani 1 1 d D . . H13D H 0.6802 0.0826 0.6209 0.068 Uiso 1 1 calc R . . C14D C 0.7760(5) 0.0454(2) 0.6689(2) 0.069(3) Uani 1 1 d GD . . C15D C 0.8650(5) 0.0337(3) 0.6809(3) 0.099(4) Uani 1 1 d GD . . H15D H 0.9106 0.0535 0.6615 0.119 Uiso 1 1 calc R . . C16D C 0.8874(6) -0.0069(3) 0.7212(3) 0.133(6) Uani 1 1 d GD . . H16D H 0.9483 -0.0149 0.7294 0.159 Uiso 1 1 calc R . . C17D C 0.8207(8) -0.0359(3) 0.7496(3) 0.151(8) Uani 1 1 d GD . . H17D H 0.8360 -0.0637 0.7772 0.181 Uiso 1 1 calc R . . C18D C 0.7316(7) -0.0242(3) 0.7376(3) 0.150(6) Uani 1 1 d GDU . . H18D H 0.6861 -0.0440 0.7570 0.180 Uiso 1 1 calc R . . C19D C 0.7093(5) 0.0164(3) 0.6973(3) 0.085(3) Uani 1 1 d GD . . H19D H 0.6484 0.0244 0.6891 0.102 Uiso 1 1 calc R . . C20D C 0.7888(5) 0.0879(3) 0.5686(3) 0.0452(18) Uani 1 1 d D . . N1D N 0.7490(4) 0.1499(3) 0.6486(3) 0.0533(17) Uani 1 1 d D . . O1D O 0.6016(5) 0.1441(3) 0.6678(3) 0.0751(17) Uani 1 1 d D . . O2D O 0.8983(4) 0.1529(3) 0.6344(3) 0.0711(17) Uani 1 1 d D . . O3D O 0.8236(3) 0.0415(2) 0.5542(2) 0.0466(12) Uani 1 1 d D . . O4D O 0.7810(3) 0.1322(2) 0.5398(2) 0.0477(13) Uani 1 1 d D C . C1E C 0.5757(9) 0.2640(5) -0.1573(5) 0.082(3) Uani 1 1 d . A . C2E C 0.6405(12) 0.2221(4) -0.1726(4) 0.093(4) Uani 1 1 d . . . C3E C 0.7312(11) 0.2380(5) -0.1798(4) 0.088(4) Uani 1 1 d . . . C4E C 0.7584(8) 0.2941(4) -0.1712(3) 0.064(3) Uani 1 1 d . . . C5E C 0.6915(9) 0.3362(4) -0.1539(4) 0.069(3) Uani 1 1 d . A . C6E C 0.6087(12) 0.1645(5) -0.1793(5) 0.114(5) Uani 1 1 d . . . H6E H 0.5485 0.1532 -0.1738 0.136 Uiso 1 1 calc R . . C7E C 0.6795(16) 0.1253(7) -0.1956(7) 0.143(8) Uani 1 1 d . . . H7E H 0.6636 0.0862 -0.2000 0.172 Uiso 1 1 calc R . . C8E C 0.7607(14) 0.1382(8) -0.2046(6) 0.127(7) Uani 1 1 d . . . H8E H 0.8015 0.1099 -0.2170 0.153 Uiso 1 1 calc R . . C9E C 0.7892(12) 0.1954(6) -0.1957(4) 0.100(5) Uani 1 1 d . . . C10E C 0.8769(13) 0.2107(7) -0.2035(6) 0.130(7) Uani 1 1 d . . . H10E H 0.9183 0.1822 -0.2145 0.156 Uiso 1 1 calc R . . C11E C 0.9058(10) 0.2650(7) -0.1959(5) 0.104(4) Uani 1 1 d . . . H11E H 0.9663 0.2752 -0.2017 0.124 Uiso 1 1 calc R . . C12E C 0.8415(9) 0.3063(5) -0.1789(4) 0.087(3) Uani 1 1 d . . . H12E H 0.8606 0.3447 -0.1730 0.104 Uiso 1 1 calc R . . C13E C 0.5456(6) 0.3621(4) -0.1250(4) 0.069(2) Uiso 0.50 1 d PD A 5 H13E H 0.4873 0.3429 -0.1178 0.083 Uiso 0.50 1 calc PR A 5 C14E C 0.5307(10) 0.4080(5) -0.1708(5) 0.065(5) Uiso 0.50 1 d PGD A 5 C15E C 0.5808(9) 0.4564(6) -0.1828(6) 0.093(7) Uiso 0.50 1 d PG A 5 H15E H 0.6331 0.4647 -0.1614 0.111 Uiso 0.50 1 calc PR A 5 C16E C 0.5544(11) 0.4928(5) -0.2261(7) 0.153(12) Uiso 0.50 1 d PG A 5 H16E H 0.5887 0.5259 -0.2342 0.184 Uiso 0.50 1 calc PR A 5 C17E C 0.4779(12) 0.4808(6) -0.2573(6) 0.098(7) Uiso 0.50 1 d PG A 5 H17E H 0.4599 0.5056 -0.2869 0.118 Uiso 0.50 1 calc PR A 5 C18E C 0.4278(10) 0.4323(7) -0.2454(6) 0.114(8) Uiso 0.50 1 d PG A 5 H18E H 0.3755 0.4240 -0.2667 0.136 Uiso 0.50 1 calc PR A 5 C19E C 0.4542(10) 0.3959(5) -0.2021(6) 0.087(6) Uiso 0.50 1 d PG A 5 H19E H 0.4200 0.3628 -0.1939 0.104 Uiso 0.50 1 calc PR A 5 C13K C 0.5456(6) 0.3621(4) -0.1250(4) 0.069(2) Uiso 0.50 1 d PD A 6 H13K H 0.4969 0.3367 -0.1112 0.083 Uiso 0.50 1 calc PR A 6 C14K C 0.4932(6) 0.4012(4) -0.1638(4) 0.037(3) Uiso 0.50 1 d PGD A 6 C15K C 0.5403(6) 0.4491(4) -0.1816(4) 0.051(4) Uiso 0.50 1 d PG A 6 H15K H 0.5963 0.4581 -0.1648 0.062 Uiso 0.50 1 calc PR A 6 C16K C 0.5053(7) 0.4837(4) -0.2238(4) 0.071(5) Uiso 0.50 1 d PG A 6 H16K H 0.5374 0.5164 -0.2360 0.085 Uiso 0.50 1 calc PR A 6 C17K C 0.4233(7) 0.4706(4) -0.2483(4) 0.058(4) Uiso 0.50 1 d PG A 6 H17K H 0.3994 0.4943 -0.2772 0.070 Uiso 0.50 1 calc PR A 6 C18K C 0.3763(6) 0.4227(5) -0.2306(4) 0.090(6) Uiso 0.50 1 d PG A 6 H18K H 0.3202 0.4137 -0.2474 0.108 Uiso 0.50 1 calc PR A 6 C19K C 0.4112(6) 0.3881(4) -0.1884(4) 0.077(6) Uiso 0.50 1 d PG A 6 H19K H 0.3791 0.3554 -0.1762 0.093 Uiso 0.50 1 calc PR A 6 C20E C 0.5800(6) 0.3868(4) -0.0701(3) 0.058(2) Uani 1 1 d . . . N1E N 0.6056(6) 0.3204(3) -0.1473(3) 0.064(2) Uani 1 1 d . . . O1E O 0.4954(7) 0.2533(4) -0.1518(4) 0.116(3) Uani 1 1 d . . . O2E O 0.7159(5) 0.3859(3) -0.1439(3) 0.0748(18) Uani 1 1 d . . . O3E O 0.5675(4) 0.4379(3) -0.0585(2) 0.0590(15) Uani 1 1 d . A . O4E O 0.6214(4) 0.3507(2) -0.0401(2) 0.0570(14) Uani 1 1 d . A . C1F C 0.9903(7) 0.3951(4) -0.0568(5) 0.070(3) Uani 1 1 d D . . C2F C 1.0497(6) 0.3555(4) -0.0257(4) 0.071(3) Uani 1 1 d D . . C3F C 1.0583(6) 0.3565(4) 0.0329(4) 0.065(3) Uani 1 1 d D . . C4F C 1.0108(5) 0.3963(4) 0.0644(4) 0.058(2) Uani 1 1 d D . . C5F C 0.9505(6) 0.4375(4) 0.0361(4) 0.063(2) Uani 1 1 d D . . C6F C 1.0986(7) 0.3180(5) -0.0582(5) 0.097(4) Uani 1 1 d D . . H6F H 1.0945 0.3190 -0.0980 0.117 Uiso 1 1 calc R . . C7F C 1.1555(10) 0.2777(6) -0.0301(8) 0.135(5) Uani 1 1 d DU . . H7F H 1.1892 0.2514 -0.0516 0.162 Uiso 1 1 calc R . . C8F C 1.1625(8) 0.2763(5) 0.0285(7) 0.117(5) Uani 1 1 d D . . H8F H 1.1998 0.2487 0.0463 0.141 Uiso 1 1 calc R . . C9F C 1.1142(6) 0.3156(4) 0.0609(6) 0.094(4) Uani 1 1 d D . . C10F C 1.1211(8) 0.3175(5) 0.1198(6) 0.104(4) Uani 1 1 d D . . H10F H 1.1605 0.2920 0.1388 0.125 Uiso 1 1 calc R . . C11F C 1.0724(8) 0.3551(5) 0.1497(5) 0.088(3) Uani 1 1 d D . . H11F H 1.0755 0.3545 0.1895 0.106 Uiso 1 1 calc R . . C12F C 1.0168(6) 0.3954(4) 0.1219(4) 0.076(3) Uani 1 1 d D . . H12F H 0.9833 0.4220 0.1433 0.091 Uiso 1 1 calc R . . C13F C 0.8713(5) 0.4674(4) -0.0509(4) 0.058(2) Uani 1 1 d . . . H13F H 0.8660 0.4509 -0.0895 0.070 Uiso 1 1 calc R . . C14F C 0.8903(6) 0.5308(3) -0.0592(3) 0.081(3) Uani 1 1 d G . . C15F C 0.8922(7) 0.5698(4) -0.0151(3) 0.126(5) Uani 1 1 d GU . . H15F H 0.8793 0.5574 0.0219 0.152 Uiso 1 1 calc R . . C16F C 0.9129(8) 0.6268(3) -0.0252(4) 0.151(6) Uani 1 1 d GU . . H16F H 0.9142 0.6535 0.0049 0.181 Uiso 1 1 calc R . . C17F C 0.9318(8) 0.6449(3) -0.0794(5) 0.138(5) Uani 1 1 d GU . . H17F H 0.9459 0.6839 -0.0862 0.166 Uiso 1 1 calc R . . C18F C 0.9299(8) 0.6060(4) -0.1234(4) 0.155(6) Uani 1 1 d GU . . H18F H 0.9428 0.6183 -0.1605 0.185 Uiso 1 1 calc R . . C19F C 0.9092(8) 0.5489(4) -0.1134(3) 0.162(8) Uani 1 1 d G . . H19F H 0.9079 0.5223 -0.1435 0.195 Uiso 1 1 calc R . . C20F C 0.7844(6) 0.4539(4) -0.0230(3) 0.056(2) Uani 1 1 d . . . N1F N 0.9449(5) 0.4346(3) -0.0228(3) 0.0570(18) Uani 1 1 d . . . O1F O 0.9761(5) 0.3939(3) -0.1078(3) 0.087(2) Uani 1 1 d . . . O2F O 0.9045(4) 0.4723(3) 0.0613(3) 0.0693(17) Uani 1 1 d . . . O3F O 0.7223(4) 0.4896(3) -0.0207(3) 0.0678(17) Uani 1 1 d . . . O4F O 0.7796(4) 0.4021(2) -0.0066(2) 0.0573(14) Uani 1 1 d . A . C1G C 0.8298(5) 0.4177(3) 0.2404(3) 0.0405(17) Uani 1 1 d . B . C2G C 0.8394(5) 0.3680(4) 0.2785(3) 0.0464(19) Uani 1 1 d . . . C3G C 0.7714(5) 0.3298(3) 0.2876(3) 0.0438(18) Uani 1 1 d . . . C4G C 0.6875(6) 0.3374(4) 0.2617(3) 0.060(2) Uani 1 1 d . . . C5G C 0.6727(5) 0.3861(4) 0.2235(3) 0.051(2) Uani 1 1 d . B . C6G C 0.9220(5) 0.3597(4) 0.3042(3) 0.050(2) Uani 1 1 d . . . H6G H 0.9690 0.3861 0.2980 0.060 Uiso 1 1 calc R . . C7G C 0.9362(6) 0.3115(4) 0.3398(4) 0.059(2) Uani 1 1 d . . . H7G H 0.9925 0.3062 0.3578 0.071 Uiso 1 1 calc R . . C8G C 0.8706(6) 0.2739(4) 0.3479(4) 0.059(2) Uani 1 1 d . . . H8G H 0.8818 0.2417 0.3714 0.071 Uiso 1 1 calc R . . C9G C 0.7847(6) 0.2801(3) 0.3229(3) 0.051(2) Uani 1 1 d . . . C10G C 0.7148(8) 0.2425(4) 0.3299(4) 0.073(3) Uani 1 1 d . . . H10G H 0.7243 0.2094 0.3524 0.088 Uiso 1 1 calc R . . C11G C 0.6346(8) 0.2505(5) 0.3066(5) 0.086(3) Uani 1 1 d . . . H11G H 0.5881 0.2237 0.3128 0.103 Uiso 1 1 calc R . . C12G C 0.6185(6) 0.3006(5) 0.2715(4) 0.073(3) Uani 1 1 d . . . H12G H 0.5611 0.3076 0.2556 0.087 Uiso 1 1 calc R . . C13G C 0.7346(5) 0.4697(4) 0.1735(3) 0.055(2) Uiso 0.50 1 d PD B 3 H13G H 0.7979 0.4799 0.1654 0.066 Uiso 1 1 calc R B 3 C14G C 0.6972(8) 0.5278(3) 0.1962(4) 0.045(4) Uiso 0.50 1 d PGD B 3 C15G C 0.6487(9) 0.5261(4) 0.2455(4) 0.061(4) Uiso 0.50 1 d PG B 3 H15G H 0.6448 0.4914 0.2662 0.074 Uiso 0.50 1 calc PR B 3 C16G C 0.6059(9) 0.5750(5) 0.2646(4) 0.091(8) Uiso 0.50 1 d PG B 3 H16G H 0.5727 0.5738 0.2983 0.109 Uiso 0.50 1 calc PR B 3 C17G C 0.6116(9) 0.6257(4) 0.2343(5) 0.068(5) Uiso 0.50 1 d PG B 3 H17G H 0.5823 0.6592 0.2473 0.082 Uiso 0.50 1 calc PR B 3 C18G C 0.6601(8) 0.6275(3) 0.1849(5) 0.088(6) Uiso 0.50 1 d PG B 3 H18G H 0.6640 0.6621 0.1642 0.106 Uiso 0.50 1 calc PR B 3 C19G C 0.7029(8) 0.5785(4) 0.1659(4) 0.060(4) Uiso 0.50 1 d PG B 3 H19G H 0.7360 0.5797 0.1322 0.072 Uiso 0.50 1 calc PR B 3 C13J C 0.7346(5) 0.4697(4) 0.1735(3) 0.055(2) Uiso 0.50 1 d P B 4 C14J C 0.6655(6) 0.5104(5) 0.2029(4) 0.050(4) Uiso 0.50 1 d PGD B 4 C15J C 0.5760(6) 0.5074(4) 0.1873(5) 0.089(7) Uiso 0.50 1 d PG B 4 H15J H 0.5571 0.4810 0.1593 0.107 Uiso 0.50 1 calc PR B 4 C16J C 0.5143(6) 0.5431(5) 0.2126(6) 0.110(8) Uiso 0.50 1 d PG B 4 H16J H 0.4531 0.5411 0.2020 0.132 Uiso 0.50 1 calc PR B 4 C17J C 0.5419(7) 0.5818(6) 0.2536(6) 0.106(8) Uiso 0.50 1 d PG B 4 H17J H 0.4997 0.6062 0.2710 0.128 Uiso 0.50 1 calc PR B 4 C18J C 0.6314(7) 0.5848(5) 0.2692(5) 0.067(6) Uiso 0.50 1 d PG B 4 H18J H 0.6503 0.6112 0.2972 0.081 Uiso 0.50 1 calc PR B 4 C19J C 0.6932(6) 0.5491(5) 0.2439(5) 0.076(5) Uiso 0.50 1 d PG B 4 H19J H 0.7543 0.5511 0.2545 0.091 Uiso 0.50 1 calc PR B 4 C20G C 0.7014(5) 0.4483(4) 0.1159(3) 0.051(2) Uani 1 1 d . . . N1G N 0.7456(4) 0.4227(3) 0.2136(3) 0.0501(17) Uani 1 1 d . . . O1G O 0.8872(4) 0.4504(2) 0.2309(2) 0.0578(14) Uani 1 1 d . . . O2G O 0.6030(4) 0.3951(3) 0.1993(3) 0.079(2) Uani 1 1 d . . . O3G O 0.6612(4) 0.4843(2) 0.0871(2) 0.0664(17) Uani 1 1 d . B . O4G O 0.7227(3) 0.3985(2) 0.1027(2) 0.0460(12) Uani 1 1 d . A . C1H C 0.3853(7) 0.2931(7) 0.1661(6) 0.083(6) Uiso 0.50 1 d PD A 1 C2H C 0.3596(7) 0.2350(7) 0.1715(8) 0.135(11) Uiso 0.50 1 d PD A 1 C3H C 0.3535(6) 0.1998(7) 0.1241(8) 0.096(7) Uiso 0.50 1 d PD A 1 C4H C 0.3725(9) 0.2197(7) 0.0707(8) 0.144(12) Uiso 0.50 1 d PD A 1 C5H C 0.3994(9) 0.2803(6) 0.0630(6) 0.093(7) Uiso 0.50 1 d PD A 1 C6H C 0.3404(12) 0.2135(11) 0.2245(9) 0.171(16) Uiso 0.50 1 d PD A 1 H6H H 0.3444 0.2381 0.2562 0.205 Uiso 0.50 1 calc PR A 1 C7H C 0.3143(13) 0.1543(12) 0.2324(11) 0.22(2) Uiso 0.50 1 d PD A 1 H7H H 0.3017 0.1401 0.2688 0.265 Uiso 0.50 1 calc PR A 1 C8H C 0.3087(12) 0.1218(11) 0.1895(11) 0.172(14) Uiso 0.50 1 d PD A 1 H8H H 0.2913 0.0831 0.1949 0.206 Uiso 0.50 1 calc PR A 1 C9H C 0.3254(10) 0.1386(7) 0.1390(9) 0.124(9) Uiso 0.50 1 d PD A 1 C10H C 0.3188(11) 0.1061(9) 0.0926(9) 0.114(8) Uiso 0.50 1 d PD A 1 H10H H 0.3011 0.0673 0.0964 0.137 Uiso 0.50 1 calc PR A 1 C11H C 0.3365(11) 0.1267(8) 0.0402(9) 0.112(8) Uiso 0.50 1 d PD A 1 H11H H 0.3293 0.1014 0.0093 0.135 Uiso 0.50 1 calc PR A 1 C12H C 0.3652(9) 0.1845(7) 0.0287(8) 0.085(4) Uiso 0.50 1 d PD A 1 H12H H 0.3784 0.1964 -0.0084 0.102 Uiso 0.50 1 calc PR A 1 C13H C 0.4327(9) 0.3724(5) 0.1071(7) 0.085(4) Uiso 0.50 1 d PD A 1 H13H H 0.4510 0.3834 0.1462 0.102 Uiso 0.50 1 calc PR A 1 C14H C 0.3567(10) 0.4122(6) 0.0921(6) 0.064(5) Uiso 0.50 1 d PD A 1 C15H C 0.3113(9) 0.4154(5) 0.0391(5) 0.106(8) Uiso 0.50 1 d PD A 1 H15H H 0.3322 0.3943 0.0078 0.127 Uiso 0.50 1 calc PR A 1 C16H C 0.2362(9) 0.4500(5) 0.0342(5) 0.105(9) Uiso 0.50 1 d PRD A 1 H16H H 0.2008 0.4489 0.0009 0.126 Uiso 0.50 1 calc PR A 1 C17H C 0.2128(9) 0.4861(5) 0.0780(5) 0.111(16) Uiso 0.50 1 d PRD A 1 H17H H 0.1615 0.5097 0.0746 0.133 Uiso 0.50 1 calc PR A 1 C18H C 0.2646(9) 0.4876(5) 0.1267(5) 0.170(14) Uiso 0.50 1 d PRD A 1 H18H H 0.2486 0.5123 0.1567 0.204 Uiso 0.50 1 calc PR A 1 C19H C 0.3397(9) 0.4531(5) 0.1317(5) 0.140(11) Uiso 0.50 1 d PRD A 1 H19H H 0.3794 0.4579 0.1627 0.168 Uiso 0.50 1 calc PR A 1 C20H C 0.5151(8) 0.3847(6) 0.0708(7) 0.056(5) Uiso 0.50 1 d PD A 1 N1H N 0.4048(7) 0.3133(5) 0.1112(5) 0.065(4) Uiso 0.50 1 d PD A 1 O1H O 0.3903(9) 0.3261(7) 0.2060(6) 0.107(5) Uiso 0.50 1 d PD A 1 O2H O 0.4158(8) 0.3013(6) 0.0178(5) 0.085(4) Uiso 0.50 1 d PD A 1 O3H O 0.5176(8) 0.4346(6) 0.0522(6) 0.067(5) Uiso 0.50 1 d PD A 1 O4H O 0.5744(7) 0.3481(7) 0.0714(7) 0.064(6) Uiso 0.50 1 d PD A 1 C1I C 0.3342(8) 0.3701(6) -0.0164(7) 0.109(8) Uiso 0.50 1 d PD A 2 C2I C 0.2748(8) 0.4120(5) -0.0387(7) 0.086(6) Uiso 0.50 1 d PD A 2 C3I C 0.2327(7) 0.4523(5) -0.0045(6) 0.081(6) Uiso 0.50 1 d PD A 2 C4I C 0.2450(8) 0.4530(6) 0.0533(7) 0.069(5) Uiso 0.50 1 d PD A 2 C5I C 0.3076(9) 0.4107(6) 0.0769(6) 0.073(5) Uiso 0.50 1 d PD A 2 C6I C 0.2569(12) 0.4146(8) -0.0960(8) 0.125(9) Uiso 0.50 1 d PD A 2 H6I H 0.2848 0.3880 -0.1203 0.150 Uiso 0.50 1 calc PR A 2 C7I C 0.1968(11) 0.4568(8) -0.1197(8) 0.097(7) Uiso 0.50 1 d PD A 2 H7I H 0.1866 0.4576 -0.1591 0.116 Uiso 0.50 1 calc PR A 2 C8I C 0.1575(11) 0.4929(8) -0.0886(8) 0.102(7) Uiso 0.50 1 d PD A 2 H8I H 0.1174 0.5195 -0.1052 0.122 Uiso 0.50 1 calc PR A 2 C9I C 0.1707(10) 0.4943(7) -0.0345(7) 0.093(7) Uiso 0.50 1 d PD A 2 C10I C 0.1337(11) 0.5315(8) 0.0019(8) 0.111(8) Uiso 0.50 1 d PD A 2 H10I H 0.0942 0.5596 -0.0130 0.133 Uiso 0.50 1 calc PR A 2 C11I C 0.1490(10) 0.5315(7) 0.0585(8) 0.119(9) Uiso 0.50 1 d PD A 2 H11I H 0.1190 0.5589 0.0808 0.142 Uiso 0.50 1 calc PR A 2 C12I C 0.2088(10) 0.4917(7) 0.0858(9) 0.089(12) Uiso 0.50 1 d PD A 2 H12I H 0.2212 0.4934 0.1250 0.107 Uiso 0.50 1 calc PR A 2 C13I C 0.4172(10) 0.3323(7) 0.0650(8) 0.111(8) Uiso 0.50 1 d PD A 2 H13I H 0.4248 0.3052 0.0329 0.133 Uiso 0.50 1 calc PR A 2 C14I C 0.3967(16) 0.2913(8) 0.1130(7) 0.100(9) Uiso 0.50 1 d PD A 2 C15I C 0.3633(10) 0.2355(6) 0.1046(6) 0.152(13) Uiso 0.50 1 d PD A 2 H15I H 0.3565 0.2208 0.0676 0.183 Uiso 0.50 1 calc PR A 2 C16I C 0.3402(10) 0.2022(6) 0.1505(6) 0.104(8) Uiso 0.50 1 d PRD A 2 H16I H 0.3165 0.1648 0.1449 0.125 Uiso 0.50 1 calc PR A 2 C17I C 0.3517(10) 0.2234(6) 0.2046(6) 0.148(13) Uiso 0.50 1 d PRD A 2 H17I H 0.3359 0.2006 0.2359 0.178 Uiso 0.50 1 calc PR A 2 C18I C 0.3863(10) 0.2780(6) 0.2128(6) 0.125(9) Uiso 0.50 1 d PRD A 2 H18I H 0.3941 0.2925 0.2497 0.150 Uiso 0.50 1 calc PR A 2 C19I C 0.4093(10) 0.3114(6) 0.1669(6) 0.137(12) Uiso 0.50 1 d PRD A 2 H19I H 0.4341 0.3484 0.1727 0.164 Uiso 0.50 1 calc PR A 2 C20I C 0.5080(8) 0.3647(8) 0.0652(9) 0.071(6) Uiso 0.50 1 d PD A 2 N1I N 0.3469(8) 0.3700(6) 0.0434(6) 0.100(6) Uiso 0.50 1 d PD A 2 O1I O 0.3746(11) 0.3337(7) -0.0433(8) 0.143(7) Uiso 0.50 1 d PD A 2 O2I O 0.3246(10) 0.4106(6) 0.1278(6) 0.132(6) Uiso 0.50 1 d PD A 2 O3I O 0.5152(8) 0.4160(6) 0.0464(6) 0.067(5) Uiso 0.50 1 d PD A 2 O4I O 0.5754(7) 0.3328(7) 0.0670(6) 0.053(5) Uiso 0.50 1 d PD A 2 C21 C 0.9987(7) -0.0472(4) 0.5509(4) 0.074(3) Uani 1 1 d . C 3 H21A H 0.9635 -0.0711 0.5769 0.089 Uiso 1 1 calc R C 3 H21B H 1.0100 -0.0097 0.5688 0.089 Uiso 1 1 calc R C 3 C22 C 1.0845(7) -0.0760(5) 0.5378(6) 0.093(4) Uani 1 1 d . C 3 H22A H 1.1016 -0.1034 0.5677 0.111 Uiso 1 1 calc R C 3 H22B H 1.1330 -0.0476 0.5333 0.111 Uiso 1 1 calc R C 3 C23 C 1.0657(8) -0.1063(5) 0.4839(5) 0.100(4) Uani 1 1 d . C 3 H23A H 1.0445 -0.1457 0.4910 0.120 Uiso 1 1 calc R C 3 H23B H 1.1200 -0.1082 0.4608 0.120 Uiso 1 1 calc R C 3 C24 C 0.9950(7) -0.0718(4) 0.4550(4) 0.076(3) Uani 1 1 d . C 3 H24A H 1.0217 -0.0456 0.4272 0.091 Uiso 1 1 calc R C 3 H24B H 0.9520 -0.0972 0.4354 0.091 Uiso 1 1 calc R C 3 O5 O 0.9515(4) -0.0399(2) 0.4986(2) 0.0533(14) Uani 1 1 d . C 3 C25 C 0.6587(5) 0.2272(3) 0.4721(4) 0.055(2) Uani 1 1 d . C 3 H25A H 0.6264 0.2425 0.4389 0.066 Uiso 1 1 calc R C 3 H25B H 0.6372 0.1879 0.4795 0.066 Uiso 1 1 calc R C 3 C26 C 0.6438(7) 0.2635(5) 0.5206(5) 0.087(3) Uani 1 1 d . C 3 H26A H 0.6478 0.2413 0.5559 0.105 Uiso 1 1 calc R C 3 H26B H 0.5849 0.2825 0.5183 0.105 Uiso 1 1 calc R C 3 C27 C 0.7194(6) 0.3067(4) 0.5164(5) 0.080(3) Uani 1 1 d . C 3 H27A H 0.7030 0.3385 0.4909 0.096 Uiso 1 1 calc R C 3 H27B H 0.7349 0.3226 0.5538 0.096 Uiso 1 1 calc R C 3 C28 C 0.7951(6) 0.2727(3) 0.4934(4) 0.056(2) Uani 1 1 d . C 3 H28A H 0.8322 0.2967 0.4686 0.067 Uiso 1 1 calc R C 3 H28B H 0.8331 0.2575 0.5242 0.067 Uiso 1 1 calc R C 3 O6 O 0.7541(3) 0.2270(2) 0.4624(2) 0.0432(12) Uani 1 1 d . C 3 C29 C 0.4667(13) 0.5499(7) -0.0402(7) 0.151(6) Uani 1 1 d U A 3 H29A H 0.4972 0.5552 -0.0765 0.181 Uiso 1 1 calc R A 3 H29B H 0.4283 0.5156 -0.0428 0.181 Uiso 1 1 calc R A 3 C30 C 0.4158(14) 0.5987(10) -0.0270(8) 0.185(10) Uani 1 1 d . A 3 H30A H 0.3536 0.5937 -0.0404 0.222 Uiso 1 1 calc R A 3 H30B H 0.4410 0.6330 -0.0453 0.222 Uiso 1 1 calc R A 3 C31 C 0.4182(15) 0.6053(10) 0.0336(7) 0.206(12) Uani 1 1 d . A 3 H31A H 0.3578 0.6005 0.0492 0.247 Uiso 1 1 calc R A 3 H31B H 0.4407 0.6438 0.0440 0.247 Uiso 1 1 calc R A 3 C32 C 0.4796(12) 0.5599(8) 0.0555(7) 0.153(6) Uani 1 1 d U A 3 H32A H 0.5185 0.5749 0.0859 0.184 Uiso 1 1 calc R A 3 H32B H 0.4457 0.5267 0.0698 0.184 Uiso 1 1 calc R A 3 O7 O 0.5322(5) 0.5440(3) 0.0059(3) 0.086(2) Uani 1 1 d U A 3 C33 C 0.7069(7) 0.2315(4) 0.0022(5) 0.076(3) Uani 1 1 d . A 3 H33A H 0.6625 0.2407 -0.0275 0.091 Uiso 1 1 calc R A 3 H33B H 0.6761 0.2126 0.0338 0.091 Uiso 1 1 calc R A 3 C34 C 0.7780(8) 0.1944(5) -0.0198(7) 0.106(4) Uani 1 1 d . A 3 H34A H 0.7807 0.1584 0.0021 0.127 Uiso 1 1 calc R A 3 H34B H 0.7647 0.1845 -0.0595 0.127 Uiso 1 1 calc R A 3 C35 C 0.8596(9) 0.2225(6) -0.0162(8) 0.139(6) Uani 1 1 d . A 3 H35A H 0.8887 0.2228 -0.0532 0.167 Uiso 1 1 calc R A 3 H35B H 0.8994 0.2028 0.0110 0.167 Uiso 1 1 calc R A 3 C36 C 0.8422(7) 0.2823(5) 0.0027(5) 0.080(3) Uani 1 1 d . A 3 H36A H 0.8836 0.2929 0.0337 0.096 Uiso 1 1 calc R A 3 H36B H 0.8503 0.3095 -0.0286 0.096 Uiso 1 1 calc R A 3 O8 O 0.7531(4) 0.2834(2) 0.0214(2) 0.0559(14) Uani 1 1 d . A 3 O41 O 0.6761(8) 0.7425(6) 0.3114(5) 0.169(3) Uiso 1 1 d D D 3 C41 C 0.6791(9) 0.7759(9) 0.2596(7) 0.169(3) Uiso 1 1 d D D 3 H41A H 0.6650 0.8165 0.2676 0.203 Uiso 1 1 calc R D 3 H41B H 0.6343 0.7612 0.2324 0.203 Uiso 1 1 calc R D 3 C42 C 0.7688(11) 0.7716(9) 0.2356(6) 0.169(3) Uiso 1 1 d D D 3 H42A H 0.7883 0.8089 0.2202 0.203 Uiso 1 1 calc R D 3 H42B H 0.7704 0.7425 0.2054 0.203 Uiso 1 1 calc R D 3 C43 C 0.8275(9) 0.7537(9) 0.2857(8) 0.169(3) Uiso 1 1 d D D 3 H43A H 0.8786 0.7301 0.2736 0.203 Uiso 1 1 calc R D 3 H43B H 0.8501 0.7875 0.3065 0.203 Uiso 1 1 calc R D 3 C44 C 0.7651(11) 0.7200(8) 0.3200(7) 0.169(3) Uiso 1 1 d D D 3 H44A H 0.7671 0.6792 0.3087 0.203 Uiso 1 1 calc R D 3 H44B H 0.7822 0.7227 0.3601 0.203 Uiso 1 1 calc R D 3 O51 O 0.6014(13) 0.4359(9) 0.3465(9) 0.166(4) Uiso 0.588(14) 1 d PD E 7 C51 C 0.5073(16) 0.4227(16) 0.3236(11) 0.166(4) Uiso 0.588(14) 1 d PD E 7 H51A H 0.4736 0.4588 0.3184 0.199 Uiso 0.588(14) 1 calc PR E 7 H51B H 0.5114 0.4035 0.2867 0.199 Uiso 0.588(14) 1 calc PR E 7 C52 C 0.4601(14) 0.3850(15) 0.3638(13) 0.166(4) Uiso 0.588(14) 1 d PD E 7 H52A H 0.4396 0.3497 0.3446 0.199 Uiso 0.588(14) 1 calc PR E 7 H52B H 0.4074 0.4049 0.3790 0.199 Uiso 0.588(14) 1 calc PR E 7 C53 C 0.5247(18) 0.3701(14) 0.4109(11) 0.166(4) Uiso 0.588(14) 1 d PD E 7 H53A H 0.5310 0.3280 0.4140 0.199 Uiso 0.588(14) 1 calc PR E 7 H53B H 0.5023 0.3849 0.4470 0.199 Uiso 0.588(14) 1 calc PR E 7 C54 C 0.6139(15) 0.3969(14) 0.3979(12) 0.166(4) Uiso 0.588(14) 1 d PD E 7 H54A H 0.6583 0.3668 0.3899 0.199 Uiso 0.588(14) 1 calc PR E 7 H54B H 0.6355 0.4196 0.4304 0.199 Uiso 0.588(14) 1 calc PR E 7 O52 O 0.512(2) 0.4625(12) 0.3442(12) 0.166(4) Uiso 0.412(14) 1 d PD E 8 C55 C 0.5843(16) 0.4224(11) 0.3635(15) 0.166(4) Uiso 0.412(14) 1 d PD E 8 H55A H 0.6447 0.4390 0.3600 0.199 Uiso 0.412(14) 1 calc PR E 8 H55B H 0.5814 0.3847 0.3444 0.199 Uiso 0.412(14) 1 calc PR E 8 C56 C 0.553(2) 0.420(2) 0.4235(12) 0.166(4) Uiso 0.412(14) 1 d PD E 8 H56A H 0.5839 0.3890 0.4447 0.199 Uiso 0.412(14) 1 calc PR E 8 H56B H 0.5630 0.4568 0.4430 0.199 Uiso 0.412(14) 1 calc PR E 8 C57 C 0.459(2) 0.4077(19) 0.4163(14) 0.166(4) Uiso 0.412(14) 1 d PD E 8 H57A H 0.4238 0.4310 0.4426 0.199 Uiso 0.412(14) 1 calc PR E 8 H57B H 0.4472 0.3668 0.4237 0.199 Uiso 0.412(14) 1 calc PR E 8 C58 C 0.4355(18) 0.4220(19) 0.3584(15) 0.166(4) Uiso 0.412(14) 1 d PD E 8 H58A H 0.3770 0.4415 0.3558 0.199 Uiso 0.412(14) 1 calc PR E 8 H58B H 0.4349 0.3878 0.3339 0.199 Uiso 0.412(14) 1 calc PR E 8 O61 O 0.0180(10) 0.0667(6) 0.8371(7) 0.206(4) Uiso 1 1 d D . . C61 C 0.0611(16) 0.0960(9) 0.7921(7) 0.206(4) Uiso 1 1 d D . . H61A H 0.0194 0.1004 0.7599 0.247 Uiso 1 1 calc R . . H61B H 0.1134 0.0737 0.7795 0.247 Uiso 1 1 calc R . . C62 C 0.0895(13) 0.1521(8) 0.8125(8) 0.206(4) Uiso 1 1 d D . . H62A H 0.0520 0.1828 0.7960 0.247 Uiso 1 1 calc R . . H62B H 0.1526 0.1594 0.8031 0.247 Uiso 1 1 calc R . . C63 C 0.0781(15) 0.1490(9) 0.8732(8) 0.206(4) Uiso 1 1 d D . . H63A H 0.1326 0.1336 0.8916 0.247 Uiso 1 1 calc R . . H63B H 0.0659 0.1875 0.8888 0.247 Uiso 1 1 calc R . . C64 C 0.0043(13) 0.1117(9) 0.8820(7) 0.206(4) Uiso 1 1 d D . . H64A H -0.0531 0.1320 0.8766 0.247 Uiso 1 1 calc R . . H64B H 0.0063 0.0947 0.9201 0.247 Uiso 1 1 calc R . . O71 O 0.3196(14) 0.0477(10) 0.3989(9) 0.156(4) Uiso 0.541(11) 1 d PD F 9 C71 C 0.2632(19) -0.0060(10) 0.3971(13) 0.156(4) Uiso 0.541(11) 1 d PD F 9 H71A H 0.2908 -0.0360 0.3736 0.188 Uiso 0.541(11) 1 calc PR F 9 H71B H 0.2534 -0.0214 0.4353 0.188 Uiso 0.541(11) 1 calc PR F 9 C72 C 0.1775(15) 0.0157(15) 0.3710(14) 0.156(4) Uiso 0.541(11) 1 d PD F 9 H72A H 0.1421 0.0380 0.3982 0.188 Uiso 0.541(11) 1 calc PR F 9 H72B H 0.1408 -0.0160 0.3558 0.188 Uiso 0.541(11) 1 calc PR F 9 C73 C 0.215(2) 0.0541(13) 0.3239(11) 0.156(4) Uiso 0.541(11) 1 d PD F 9 H73A H 0.2400 0.0311 0.2930 0.188 Uiso 0.541(11) 1 calc PR F 9 H73B H 0.1682 0.0801 0.3085 0.188 Uiso 0.541(11) 1 calc PR F 9 C74 C 0.2843(19) 0.0858(10) 0.3552(12) 0.156(4) Uiso 0.541(11) 1 d PD F 9 H74A H 0.3326 0.0975 0.3296 0.188 Uiso 0.541(11) 1 calc PR F 9 H74B H 0.2588 0.1207 0.3723 0.188 Uiso 0.541(11) 1 calc PR F 9 O72 O 0.3258(13) 0.0150(12) 0.3470(10) 0.156(4) Uiso 0.459(11) 1 d PD F 10 C75 C 0.2456(18) 0.0108(12) 0.3103(9) 0.156(4) Uiso 0.459(11) 1 d PD F 10 H75A H 0.2477 0.0402 0.2804 0.188 Uiso 0.459(11) 1 calc PR F 10 H75B H 0.2428 -0.0274 0.2924 0.188 Uiso 0.459(11) 1 calc PR F 10 C76 C 0.1669(15) 0.020(2) 0.3458(14) 0.156(4) Uiso 0.459(11) 1 d PD F 10 H76A H 0.1195 -0.0080 0.3360 0.188 Uiso 0.459(11) 1 calc PR F 10 H76B H 0.1430 0.0590 0.3404 0.188 Uiso 0.459(11) 1 calc PR F 10 C77 C 0.198(2) 0.011(2) 0.4052(11) 0.156(4) Uiso 0.459(11) 1 d PD F 10 H77A H 0.1935 -0.0292 0.4164 0.188 Uiso 0.459(11) 1 calc PR F 10 H77B H 0.1618 0.0349 0.4313 0.188 Uiso 0.459(11) 1 calc PR F 10 C78 C 0.294(2) 0.032(2) 0.4044(11) 0.156(4) Uiso 0.459(11) 1 d PD F 10 H78A H 0.2984 0.0735 0.4100 0.188 Uiso 0.459(11) 1 calc PR F 10 H78B H 0.3301 0.0122 0.4340 0.188 Uiso 0.459(11) 1 calc PR F 10 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0437(5) 0.0305(5) 0.0433(5) -0.0005(4) -0.0087(4) 0.0063(4) Cu2 0.0390(5) 0.0285(5) 0.0477(5) -0.0010(4) -0.0068(4) 0.0027(4) Cu3 0.0717(7) 0.0613(7) 0.0413(6) -0.0091(5) -0.0190(5) 0.0258(6) Cu4 0.0562(6) 0.0508(6) 0.0382(5) -0.0028(4) -0.0120(4) 0.0085(5) C1A 0.036(4) 0.047(5) 0.077(7) -0.013(5) -0.017(4) 0.010(4) C2A 0.040(4) 0.030(4) 0.080(6) -0.010(4) -0.008(4) 0.006(3) C3A 0.038(4) 0.038(4) 0.064(5) 0.002(4) -0.005(4) 0.001(3) C4A 0.036(4) 0.041(4) 0.062(5) -0.012(4) -0.015(4) 0.001(3) C5A 0.033(4) 0.035(5) 0.066(6) 0.002(4) -0.007(4) 0.003(3) C6A 0.053(5) 0.066(6) 0.077(6) -0.019(5) -0.001(4) 0.014(5) C7A 0.068(6) 0.042(5) 0.096(8) -0.005(5) -0.008(5) -0.008(4) C8A 0.071(6) 0.035(5) 0.105(8) 0.004(5) 0.002(5) -0.001(4) C9A 0.037(4) 0.051(5) 0.095(7) 0.001(5) -0.007(4) -0.001(4) C10A 0.068(6) 0.052(6) 0.076(7) 0.007(5) 0.000(5) 0.001(5) C11A 0.068(6) 0.057(6) 0.058(5) -0.006(4) -0.009(4) -0.005(4) C12A 0.057(5) 0.051(5) 0.066(6) 0.001(4) -0.005(4) 0.004(4) C13A 0.044(4) 0.045(4) 0.049(5) -0.009(4) -0.011(4) -0.004(4) C20A 0.039(4) 0.045(5) 0.049(5) -0.009(4) -0.011(3) 0.002(4) N1A 0.040(3) 0.049(4) 0.052(4) -0.013(3) -0.012(3) 0.003(3) O1A 0.097(5) 0.056(4) 0.059(4) -0.018(3) -0.011(3) -0.003(3) O2A 0.059(3) 0.047(3) 0.063(3) -0.006(3) -0.006(3) -0.007(3) O3A 0.054(3) 0.038(3) 0.047(3) 0.004(2) -0.016(2) 0.004(2) O4A 0.044(3) 0.033(3) 0.063(3) 0.001(2) -0.005(3) -0.003(2) C14A 0.045(5) 0.048(5) 0.057(5) -0.002(4) -0.020(4) -0.003(4) C15A 0.050(5) 0.053(6) 0.112(8) 0.007(5) -0.021(5) -0.004(5) C16A 0.059(6) 0.072(7) 0.111(9) 0.006(7) -0.027(6) 0.003(5) C17A 0.090(8) 0.075(7) 0.110(9) 0.022(7) -0.053(7) -0.013(7) C18A 0.131(11) 0.128(12) 0.082(8) 0.007(8) -0.037(8) 0.045(9) C19A 0.100(8) 0.114(9) 0.068(7) 0.009(7) -0.022(6) 0.034(7) C1B 0.045(5) 0.043(5) 0.048(5) -0.006(4) 0.000(4) 0.007(4) C2B 0.065(5) 0.044(5) 0.040(4) 0.000(4) 0.006(4) 0.003(4) C3B 0.065(6) 0.042(5) 0.051(5) -0.005(4) -0.004(4) -0.003(4) C4B 0.057(5) 0.041(5) 0.056(5) 0.012(4) -0.019(4) -0.007(4) C5B 0.050(5) 0.035(4) 0.046(5) 0.000(4) -0.001(4) 0.000(4) C6B 0.074(6) 0.042(5) 0.054(5) -0.004(4) 0.003(4) -0.007(4) C7B 0.102(8) 0.052(6) 0.045(5) 0.010(4) -0.006(5) -0.007(5) C8B 0.116(9) 0.049(5) 0.036(5) 0.009(4) 0.000(5) 0.019(6) C9B 0.084(7) 0.046(5) 0.053(5) 0.008(4) -0.022(5) 0.011(5) C10B 0.086(7) 0.085(8) 0.074(7) 0.001(6) -0.036(6) 0.016(6) C11B 0.062(6) 0.059(6) 0.108(8) 0.002(6) -0.031(6) 0.001(5) C12B 0.061(6) 0.060(6) 0.079(7) 0.007(5) -0.029(5) -0.008(5) C13B 0.052(5) 0.049(5) 0.041(4) 0.003(4) -0.009(4) 0.015(4) C14B 0.092(7) 0.056(6) 0.043(5) 0.003(4) -0.016(5) 0.028(5) C15B 0.090(7) 0.038(5) 0.085(7) -0.011(5) -0.010(6) 0.018(5) C16B 0.150(11) 0.062(7) 0.087(8) -0.022(6) -0.031(8) 0.018(7) C17B 0.28(2) 0.064(8) 0.066(8) -0.034(7) -0.051(11) 0.084(12) C18B 0.201(16) 0.076(9) 0.094(9) -0.015(8) 0.021(9) 0.063(10) C19B 0.131(10) 0.091(8) 0.054(6) 0.002(5) 0.024(6) 0.042(7) C20B 0.040(4) 0.041(5) 0.040(4) 0.001(4) -0.009(3) -0.005(4) N1B 0.044(4) 0.045(4) 0.040(4) 0.002(3) -0.009(3) 0.002(3) O1B 0.057(4) 0.063(4) 0.053(3) 0.003(3) 0.001(3) -0.004(3) O2B 0.052(3) 0.046(3) 0.063(4) 0.003(3) 0.003(3) -0.005(3) O3B 0.048(3) 0.043(3) 0.051(3) 0.003(3) -0.005(2) 0.009(2) O4B 0.050(3) 0.032(3) 0.046(3) 0.002(2) -0.006(2) 0.004(2) C1C 0.046(5) 0.059(6) 0.084(8) 0.005(5) 0.004(5) 0.002(4) C2C 0.039(5) 0.043(5) 0.116(9) 0.012(6) 0.003(5) -0.004(4) C3C 0.039(5) 0.032(5) 0.136(10) -0.023(6) 0.006(6) -0.001(4) C4C 0.054(5) 0.045(5) 0.085(7) -0.028(5) 0.012(5) -0.005(4) C5C 0.048(5) 0.039(5) 0.057(6) -0.019(4) 0.006(4) -0.009(4) C6C 0.043(5) 0.082(8) 0.175(13) 0.034(8) -0.013(7) 0.009(6) C7C 0.047(7) 0.065(8) 0.239(19) 0.036(10) -0.001(9) 0.030(6) C8C 0.057(8) 0.074(10) 0.29(3) -0.053(15) -0.009(13) -0.016(7) C9C 0.042(5) 0.054(7) 0.159(13) -0.032(8) -0.012(6) 0.003(5) C10C 0.051(7) 0.087(10) 0.185(16) -0.080(11) 0.001(8) -0.012(6) C11C 0.075(8) 0.128(12) 0.128(12) -0.071(10) 0.016(8) -0.012(8) C12C 0.055(6) 0.071(7) 0.130(10) -0.042(7) 0.000(6) -0.006(5) C13C 0.049(4) 0.036(4) 0.051(5) 0.002(4) 0.001(4) 0.003(4) C14C 0.043(4) 0.036(4) 0.046(4) -0.001(3) -0.006(3) -0.003(3) C15C 0.066(6) 0.045(5) 0.096(7) -0.003(5) -0.004(5) 0.004(4) C16C 0.079(7) 0.050(6) 0.124(9) -0.001(6) 0.020(6) -0.021(5) C17C 0.087(7) 0.039(5) 0.077(6) 0.009(4) -0.011(5) -0.014(5) C18C 0.058(5) 0.037(5) 0.086(6) -0.009(4) -0.011(5) -0.006(4) C19C 0.071(6) 0.046(5) 0.071(6) -0.002(4) -0.012(5) -0.002(5) C20C 0.047(4) 0.029(4) 0.037(4) -0.007(3) -0.002(3) 0.004(4) N1C 0.044(4) 0.031(3) 0.070(5) 0.006(3) 0.003(3) 0.006(3) O1C 0.057(4) 0.087(5) 0.090(5) 0.034(4) -0.002(3) 0.028(3) O2C 0.067(4) 0.051(3) 0.053(3) -0.007(3) 0.004(3) -0.001(3) O3C 0.049(3) 0.029(3) 0.049(3) -0.003(2) -0.009(2) -0.002(2) O4C 0.045(3) 0.032(3) 0.051(3) -0.005(2) -0.008(2) -0.002(2) C1D 0.083(7) 0.054(6) 0.044(5) -0.011(4) -0.001(5) 0.006(5) C2D 0.112(9) 0.068(7) 0.049(5) 0.008(5) -0.013(6) 0.045(7) C3D 0.173(13) 0.060(7) 0.025(5) -0.005(4) -0.010(6) 0.034(8) C4D 0.125(9) 0.059(6) 0.029(4) -0.002(4) -0.012(5) -0.019(7) C5D 0.084(7) 0.073(7) 0.038(5) -0.006(5) -0.018(5) -0.008(6) C6D 0.160(12) 0.097(9) 0.054(6) 0.013(6) -0.004(7) 0.076(9) C7D 0.199(18) 0.108(13) 0.067(8) -0.001(9) -0.004(10) 0.100(12) C8D 0.27(3) 0.076(11) 0.055(7) -0.010(7) -0.011(12) 0.084(14) C9D 0.227(17) 0.038(6) 0.041(6) 0.001(5) -0.028(8) -0.022(9) C10D 0.31(3) 0.068(10) 0.054(8) -0.015(7) -0.030(12) -0.025(14) C11D 0.27(2) 0.095(12) 0.063(9) 0.012(8) -0.024(11) -0.089(14) C12D 0.177(13) 0.067(7) 0.053(6) 0.001(5) -0.024(7) -0.044(8) C13D 0.077(6) 0.034(4) 0.059(5) -0.008(4) 0.000(4) 0.005(4) C14D 0.127(9) 0.037(5) 0.043(5) -0.012(4) -0.011(5) 0.019(6) C15D 0.164(12) 0.047(6) 0.084(8) -0.017(6) -0.046(8) 0.027(7) C16D 0.238(19) 0.066(8) 0.092(10) -0.027(7) -0.066(11) 0.063(10) C17D 0.31(3) 0.058(8) 0.084(10) -0.013(7) -0.045(13) 0.051(12) C18D 0.223(14) 0.090(9) 0.138(11) 0.021(9) 0.042(11) 0.002(10) C19D 0.150(10) 0.030(5) 0.075(7) 0.009(5) 0.022(7) 0.004(6) C20D 0.047(4) 0.038(5) 0.051(5) 0.003(4) -0.009(4) -0.001(4) N1D 0.070(5) 0.036(4) 0.054(4) -0.001(3) -0.003(3) 0.004(4) O1D 0.079(4) 0.085(5) 0.061(4) -0.014(4) 0.011(3) 0.013(4) O2D 0.068(4) 0.080(5) 0.065(4) -0.013(3) -0.017(3) -0.003(4) O3D 0.060(3) 0.033(3) 0.047(3) -0.007(2) -0.010(2) 0.009(3) O4D 0.046(3) 0.040(3) 0.057(3) 0.002(3) 0.000(2) 0.002(2) C1E 0.102(9) 0.067(7) 0.075(7) -0.018(6) -0.039(6) 0.006(7) C2E 0.180(14) 0.054(7) 0.043(6) -0.014(5) -0.043(7) 0.027(8) C3E 0.153(12) 0.075(8) 0.035(5) -0.006(5) -0.031(6) 0.047(8) C4E 0.102(8) 0.059(6) 0.031(4) -0.002(4) -0.001(5) 0.029(6) C5E 0.122(10) 0.041(6) 0.043(5) 0.002(4) 0.000(5) 0.020(6) C6E 0.182(14) 0.064(8) 0.094(9) -0.019(7) -0.050(9) 0.004(8) C7E 0.25(2) 0.070(9) 0.106(12) -0.039(8) -0.037(15) 0.073(15) C8E 0.202(18) 0.101(13) 0.079(9) -0.031(8) -0.012(11) 0.088(14) C9E 0.179(14) 0.073(9) 0.049(6) -0.005(6) -0.008(8) 0.065(10) C10E 0.220(19) 0.093(11) 0.078(9) -0.012(8) -0.003(11) 0.105(14) C11E 0.127(10) 0.129(12) 0.056(6) 0.006(7) 0.008(6) 0.051(9) C12E 0.128(10) 0.080(8) 0.052(6) 0.006(5) 0.016(6) 0.041(8) C20E 0.072(6) 0.068(6) 0.034(4) 0.000(4) -0.019(4) 0.010(5) N1E 0.085(6) 0.051(5) 0.055(4) -0.010(4) -0.023(4) 0.022(4) O1E 0.137(8) 0.086(6) 0.123(7) -0.017(5) -0.063(6) -0.005(6) O2E 0.116(5) 0.048(4) 0.061(4) 0.007(3) 0.008(4) 0.012(4) O3E 0.076(4) 0.059(4) 0.041(3) -0.009(3) -0.019(3) 0.020(3) O4E 0.067(4) 0.055(3) 0.048(3) -0.009(3) -0.022(3) 0.009(3) C1F 0.089(7) 0.045(5) 0.077(7) 0.010(5) 0.030(6) -0.005(5) C2F 0.057(5) 0.058(6) 0.098(8) 0.002(6) 0.018(5) 0.001(5) C3F 0.046(5) 0.056(6) 0.093(8) 0.012(5) -0.006(5) -0.007(5) C4F 0.042(4) 0.057(5) 0.076(6) -0.001(5) -0.006(4) -0.012(4) C5F 0.063(6) 0.062(6) 0.064(6) 0.004(5) -0.008(5) -0.015(5) C6F 0.086(8) 0.076(8) 0.130(10) -0.019(7) 0.024(7) 0.015(7) C7F 0.104(9) 0.107(10) 0.195(13) 0.004(10) 0.041(10) 0.022(8) C8F 0.075(8) 0.077(8) 0.200(17) 0.017(10) -0.029(10) 0.024(7) C9F 0.049(6) 0.059(7) 0.175(14) 0.023(8) -0.016(7) -0.008(5) C10F 0.081(8) 0.087(9) 0.142(13) 0.027(9) -0.055(9) -0.028(7) C11F 0.085(8) 0.080(8) 0.098(8) 0.009(7) -0.020(7) -0.029(7) C12F 0.062(6) 0.070(7) 0.094(8) 0.011(6) -0.026(5) -0.024(5) C13F 0.056(5) 0.061(5) 0.057(5) -0.006(4) -0.008(4) 0.004(4) C14F 0.101(8) 0.059(6) 0.083(7) 0.010(6) -0.010(6) -0.002(6) C15F 0.183(12) 0.067(7) 0.128(10) -0.010(7) -0.026(9) -0.023(8) C16F 0.187(13) 0.090(9) 0.175(13) -0.016(9) -0.029(11) -0.017(9) C17F 0.157(11) 0.097(9) 0.161(12) 0.050(9) 0.035(10) -0.013(9) C18F 0.226(14) 0.116(11) 0.123(10) 0.022(9) 0.068(10) -0.009(10) C19F 0.31(2) 0.063(8) 0.113(11) 0.030(8) 0.073(13) 0.015(11) C20F 0.082(6) 0.046(5) 0.039(4) -0.003(4) -0.016(4) -0.001(5) N1F 0.068(5) 0.046(4) 0.057(5) -0.008(3) 0.005(4) 0.000(4) O1F 0.117(6) 0.075(5) 0.068(5) 0.003(4) 0.028(4) 0.004(4) O2F 0.074(4) 0.065(4) 0.069(4) -0.019(3) -0.008(3) -0.001(3) O3F 0.085(4) 0.047(3) 0.071(4) -0.014(3) -0.024(3) 0.025(3) O4F 0.067(3) 0.048(4) 0.057(3) -0.009(3) -0.016(3) 0.011(3) C1G 0.032(4) 0.044(4) 0.046(4) 0.000(4) -0.013(3) 0.004(4) C2G 0.052(5) 0.050(5) 0.037(4) 0.003(4) -0.009(3) 0.006(4) C3G 0.043(4) 0.051(5) 0.038(4) -0.006(4) 0.003(3) -0.013(4) C4G 0.062(6) 0.076(6) 0.041(5) -0.008(4) 0.007(4) -0.012(5) C5G 0.042(5) 0.069(6) 0.042(4) -0.008(4) -0.010(4) -0.001(4) C6G 0.053(5) 0.057(5) 0.040(4) 0.002(4) -0.004(4) -0.002(4) C7G 0.055(5) 0.056(5) 0.067(6) 0.005(4) -0.028(4) 0.010(5) C8G 0.077(6) 0.048(5) 0.053(5) 0.003(4) -0.012(4) 0.011(5) C9G 0.065(6) 0.044(5) 0.045(5) -0.002(4) 0.009(4) -0.005(4) C10G 0.109(9) 0.065(6) 0.046(5) 0.002(5) -0.001(5) -0.022(6) C11G 0.092(8) 0.094(8) 0.072(7) -0.006(6) 0.011(6) -0.049(7) C12G 0.054(5) 0.102(8) 0.063(6) 0.007(6) -0.013(4) -0.021(5) C20G 0.052(5) 0.056(5) 0.044(5) -0.003(4) -0.001(4) 0.011(4) N1G 0.060(4) 0.051(4) 0.039(4) 0.000(3) -0.009(3) 0.007(3) O1G 0.058(3) 0.057(3) 0.059(4) 0.015(3) -0.020(3) -0.007(3) O2G 0.043(3) 0.129(6) 0.065(4) 0.005(4) -0.019(3) -0.005(4) O3G 0.095(4) 0.056(3) 0.048(3) -0.008(3) -0.029(3) 0.033(3) O4G 0.051(3) 0.051(3) 0.036(3) 0.002(2) -0.009(2) 0.009(3) C21 0.080(7) 0.070(6) 0.071(6) 0.011(5) -0.020(5) 0.029(5) C22 0.062(6) 0.095(8) 0.120(10) 0.019(7) -0.034(6) 0.023(6) C23 0.115(9) 0.099(9) 0.086(8) -0.002(7) -0.034(7) 0.055(7) C24 0.099(7) 0.068(6) 0.060(6) 0.001(5) 0.006(5) 0.052(6) O5 0.055(3) 0.057(3) 0.048(3) 0.006(3) -0.009(3) 0.019(3) C25 0.042(5) 0.031(4) 0.092(6) 0.003(4) -0.012(4) 0.007(3) C26 0.067(6) 0.087(8) 0.109(9) -0.044(7) 0.009(6) -0.008(6) C27 0.073(6) 0.050(6) 0.116(9) -0.051(6) -0.001(6) -0.002(5) C28 0.059(5) 0.034(4) 0.076(6) -0.012(4) -0.004(4) -0.003(4) O6 0.041(3) 0.026(3) 0.063(3) -0.005(2) -0.004(2) -0.001(2) C29 0.181(12) 0.127(11) 0.142(11) -0.006(9) -0.051(10) 0.056(10) C30 0.187(18) 0.21(2) 0.154(17) -0.005(14) -0.018(13) 0.153(17) C31 0.25(2) 0.27(3) 0.097(12) 0.038(14) -0.007(12) 0.19(2) C32 0.164(12) 0.158(12) 0.138(11) -0.016(10) 0.029(10) 0.076(10) O7 0.100(5) 0.094(5) 0.062(4) -0.005(4) -0.019(4) 0.065(4) C33 0.067(6) 0.054(6) 0.106(8) -0.016(6) -0.024(6) -0.011(5) C34 0.107(10) 0.046(6) 0.163(13) -0.023(7) 0.003(9) -0.001(7) C35 0.098(10) 0.087(10) 0.23(2) -0.033(11) 0.034(11) 0.016(8) C36 0.062(6) 0.075(7) 0.105(8) 0.016(6) 0.013(6) 0.022(5) O8 0.059(4) 0.049(3) 0.059(3) -0.003(3) -0.006(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O3B 1.927(5) . ? Cu1 O3D 1.932(5) . ? Cu1 O3A 1.985(5) . ? Cu1 O3C 2.014(5) . ? Cu1 O5 2.158(5) . ? Cu1 Cu2 2.6213(11) . ? Cu2 O4C 1.926(5) . ? Cu2 O4A 1.935(5) . ? Cu2 O4B 1.966(5) . ? Cu2 O4D 1.966(5) . ? Cu2 O6 2.214(5) . ? Cu3 O3H 1.852(10) . ? Cu3 O3F 1.937(7) . ? Cu3 O3E 1.942(5) . ? Cu3 O3G 1.951(5) . ? Cu3 O3I 2.032(11) . ? Cu3 O7 2.163(6) . ? Cu3 Cu4 2.6201(13) . ? Cu4 O4H 1.914(10) . ? Cu4 O4F 1.941(6) . ? Cu4 O4E 1.953(5) . ? Cu4 O4G 1.953(5) . ? Cu4 O4I 1.961(10) . ? Cu4 O8 2.219(6) . ? C1A O1A 1.214(10) . ? C1A N1A 1.426(10) . ? C1A C2A 1.459(11) . ? C2A C6A 1.386(11) . ? C2A C3A 1.409(10) . ? C3A C4A 1.412(10) . ? C3A C9A 1.415(11) . ? C4A C12A 1.373(10) . ? C4A C5A 1.470(10) . ? C5A O2A 1.236(9) . ? C5A N1A 1.387(10) . ? C6A C7A 1.401(12) . ? C6A H6A 0.9500 . ? C7A C8A 1.386(13) . ? C7A H7A 0.9500 . ? C8A C9A 1.410(12) . ? C8A H8A 0.9500 . ? C9A C10A 1.433(12) . ? C10A C11A 1.353(11) . ? C10A H10A 0.9500 . ? C11A C12A 1.400(11) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A N1A 1.490(10) . ? C13A C20A 1.518(10) . ? C13A C14A 1.520(11) . ? C13A H13A 1.0000 . ? C20A O3A 1.227(9) . ? C20A O4A 1.283(9) . ? C14A C19A 1.349(14) . ? C14A C15A 1.384(13) . ? C15A C16A 1.385(14) . ? C15A H15A 0.9500 . ? C16A C17A 1.336(16) . ? C16A H16A 0.9500 . ? C17A C18A 1.370(18) . ? C17A H17A 0.9500 . ? C18A C19A 1.367(16) . ? C18A H18A 0.9500 . ? C19A H19A 0.9500 . ? C1B O1B 1.212(9) . ? C1B N1B 1.408(10) . ? C1B C2B 1.496(11) . ? C2B C6B 1.357(11) . ? C2B C3B 1.395(12) . ? C3B C9B 1.400(12) . ? C3B C4B 1.426(11) . ? C4B C12B 1.370(12) . ? C4B C5B 1.454(11) . ? C5B O2B 1.241(9) . ? C5B N1B 1.384(10) . ? C6B C7B 1.396(13) . ? C6B H6B 0.9500 . ? C7B C8B 1.304(14) . ? C7B H7B 0.9500 . ? C8B C9B 1.402(14) . ? C8B H8B 0.9500 . ? C9B C10B 1.433(14) . ? C10B C11B 1.342(15) . ? C10B H10B 0.9500 . ? C11B C12B 1.405(13) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B N1B 1.499(9) . ? C13B C20B 1.531(11) . ? C13B C14B 1.545(12) . ? C13B H13B 1.0000 . ? C14B C15B 1.322(14) . ? C14B C19B 1.377(14) . ? C15B C16B 1.419(14) . ? C15B H15B 0.9500 . ? C16B C17B 1.43(2) . ? C16B H16B 0.9500 . ? C17B C18B 1.37(2) . ? C17B H17B 0.9500 . ? C18B C19B 1.365(17) . ? C18B H18B 0.9500 . ? C19B H19B 0.9500 . ? C20B O4B 1.238(9) . ? C20B O3B 1.267(9) . ? C1C O1C 1.224(11) . ? C1C N1C 1.382(12) . ? C1C C2C 1.469(14) . ? C2C C6C 1.352(15) . ? C2C C3C 1.404(15) . ? C3C C4C 1.368(15) . ? C3C C9C 1.435(14) . ? C4C C12C 1.378(15) . ? C4C C5C 1.519(12) . ? C5C O2C 1.174(10) . ? C5C N1C 1.412(11) . ? C6C C7C 1.45(2) . ? C6C H6C 0.9500 . ? C7C C8C 1.35(2) . ? C7C H7C 0.9500 . ? C8C C9C 1.41(2) . ? C8C H8C 0.9500 . ? C9C C10C 1.348(19) . ? C10C C11C 1.37(2) . ? C10C H10C 0.9500 . ? C11C C12C 1.431(17) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C N1C 1.482(10) . ? C13C C14C 1.519(10) . ? C13C C20C 1.527(10) . ? C13C H13C 1.0000 . ? C14C C19C 1.366(11) . ? C14C C15C 1.420(12) . ? C15C C16C 1.353(12) . ? C15C H15C 0.9500 . ? C16C C17C 1.381(14) . ? C16C H16C 0.9500 . ? C17C C18C 1.361(12) . ? C17C H17C 0.9500 . ? C18C C19C 1.395(12) . ? C18C H18C 0.9500 . ? C19C H19C 0.9500 . ? C20C O3C 1.235(8) . ? C20C O4C 1.264(8) . ? C1D O1D 1.219(10) . ? C1D N1D 1.410(10) . ? C1D C2D 1.433(13) . ? C2D C6D 1.375(14) . ? C2D C3D 1.411(15) . ? C3D C4D 1.394(14) . ? C3D C9D 1.506(13) . ? C4D C12D 1.334(14) . ? C4D C5D 1.475(13) . ? C5D O2D 1.219(10) . ? C5D N1D 1.394(11) . ? C6D C7D 1.433(18) . ? C6D H6D 0.9500 . ? C7D C8D 1.292(18) . ? C7D H7D 0.9500 . ? C8D C9D 1.328(17) . ? C8D H8D 0.9500 . ? C9D C10D 1.344(18) . ? C10D C11D 1.378(19) . ? C10D H10D 0.9500 . ? C11D C12D 1.447(16) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D N1D 1.474(9) . ? C13D C14D 1.510(8) . ? C13D C20D 1.562(10) . ? C13D H13D 1.0000 . ? C14D C15D 1.3900 . ? C14D C19D 1.3900 . ? C15D C16D 1.3900 . ? C15D H15D 0.9500 . ? C16D C17D 1.3900 . ? C16D H16D 0.9500 . ? C17D C18D 1.3900 . ? C17D H17D 0.9500 . ? C18D C19D 1.3900 . ? C18D H18D 0.9500 . ? C19D H19D 0.9500 . ? C20D O4D 1.248(8) . ? C20D O3D 1.252(8) . ? C1E O1E 1.239(14) . ? C1E N1E 1.410(14) . ? C1E C2E 1.431(17) . ? C2E C3E 1.422(18) . ? C2E C6E 1.436(17) . ? C3E C9E 1.377(17) . ? C3E C4E 1.389(16) . ? C4E C12E 1.294(15) . ? C4E C5E 1.466(14) . ? C5E O2E 1.240(12) . ? C5E N1E 1.351(13) . ? C6E C7E 1.46(2) . ? C6E H6E 0.9500 . ? C7E C8E 1.27(2) . ? C7E H7E 0.9500 . ? C8E C9E 1.42(2) . ? C8E H8E 0.9500 . ? C9E C10E 1.38(2) . ? C10E C11E 1.35(2) . ? C10E H10E 0.9500 . ? C11E C12E 1.426(16) . ? C11E H11E 0.9500 . ? C12E H12E 0.9500 . ? C13E N1E 1.433(12) . ? C13E C20E 1.515(12) . ? C13E C14E 1.543(12) . ? C13E H13E 1.0000 . ? C14E C15E 1.3900 . ? C14E C19E 1.3900 . ? C15E C16E 1.3900 . ? C15E H15E 0.9500 . ? C16E C17E 1.3900 . ? C16E H16E 0.9500 . ? C17E C18E 1.3900 . ? C17E H17E 0.9500 . ? C18E C19E 1.3900 . ? C18E H18E 0.9500 . ? C19E H19E 0.9500 . ? C14K C15K 1.3900 . ? C14K C19K 1.3900 . ? C15K C16K 1.3900 . ? C15K H15K 0.9500 . ? C16K C17K 1.3900 . ? C16K H16K 0.9500 . ? C17K C18K 1.3900 . ? C17K H17K 0.9500 . ? C18K C19K 1.3900 . ? C18K H18K 0.9500 . ? C19K H19K 0.9500 . ? C20E O3E 1.241(10) . ? C20E O4E 1.264(10) . ? C1F O1F 1.233(12) . ? C1F N1F 1.409(12) . ? C1F C2F 1.478(12) . ? C2F C6F 1.385(12) . ? C2F C3F 1.401(12) . ? C3F C4F 1.394(11) . ? C3F C9F 1.432(12) . ? C4F C12F 1.372(12) . ? C4F C5F 1.479(11) . ? C5F O2F 1.227(11) . ? C5F N1F 1.406(11) . ? C6F C7F 1.433(15) . ? C6F H6F 0.9500 . ? C7F C8F 1.397(16) . ? C7F H7F 0.9500 . ? C8F C9F 1.407(15) . ? C8F H8F 0.9500 . ? C9F C10F 1.406(14) . ? C10F C11F 1.351(14) . ? C10F H10F 0.9500 . ? C11F C12F 1.417(13) . ? C11F H11F 0.9500 . ? C12F H12F 0.9500 . ? C13F N1F 1.495(11) . ? C13F C20F 1.502(13) . ? C13F C14F 1.522(11) . ? C13F H13F 1.0000 . ? C14F C15F 1.3900 . ? C14F C19F 1.3900 . ? C15F C16F 1.3900 . ? C15F H15F 0.9500 . ? C16F C17F 1.3900 . ? C16F H16F 0.9500 . ? C17F C18F 1.3900 . ? C17F H17F 0.9500 . ? C18F C19F 1.3900 . ? C18F H18F 0.9500 . ? C19F H19F 0.9500 . ? C20F O3F 1.252(10) . ? C20F O4F 1.275(10) . ? C1G O1G 1.175(8) . ? C1G N1G 1.414(9) . ? C1G C2G 1.479(11) . ? C2G C3G 1.375(11) . ? C2G C6G 1.390(11) . ? C3G C4G 1.406(12) . ? C3G C9G 1.446(11) . ? C4G C12G 1.367(13) . ? C4G C5G 1.473(12) . ? C5G O2G 1.206(9) . ? C5G N1G 1.410(11) . ? C6G C7G 1.423(12) . ? C6G H6G 0.9500 . ? C7G C8G 1.336(12) . ? C7G H7G 0.9500 . ? C8G C9G 1.422(12) . ? C8G H8G 0.9500 . ? C9G C10G 1.380(13) . ? C10G C11G 1.333(15) . ? C10G H10G 0.9500 . ? C11G C12G 1.458(16) . ? C11G H11G 0.9500 . ? C12G H12G 0.9500 . ? C13G N1G 1.465(10) . ? C13G C20G 1.537(11) . ? C13G C14G 1.567(10) . ? C13G H13G 1.0000 . ? C14G C15G 1.3900 . ? C14G C19G 1.3900 . ? C15G C16G 1.3900 . ? C15G H15G 0.9500 . ? C16G C17G 1.3900 . ? C16G H16G 0.9500 . ? C17G C18G 1.3900 . ? C17G H17G 0.9500 . ? C18G C19G 1.3900 . ? C18G H18G 0.9500 . ? C19G H19G 0.9500 . ? C14J C15J 1.3900 . ? C14J C19J 1.3900 . ? C15J C16J 1.3900 . ? C15J H15J 0.9500 . ? C16J C17J 1.3900 . ? C16J H16J 0.9500 . ? C17J C18J 1.3900 . ? C17J H17J 0.9500 . ? C18J C19J 1.3900 . ? C18J H18J 0.9500 . ? C19J H19J 0.9500 . ? C20G O3G 1.236(9) . ? C20G O4G 1.249(9) . ? C1H O1H 1.225(15) . ? C1H C2H 1.415(17) . ? C1H N1H 1.425(14) . ? C2H C6H 1.392(18) . ? C2H C3H 1.399(18) . ? C3H C4H 1.387(18) . ? C3H C9H 1.535(17) . ? C4H C12H 1.298(17) . ? C4H C5H 1.485(16) . ? C5H O2H 1.210(14) . ? C5H N1H 1.385(14) . ? C6H C7H 1.45(2) . ? C6H H6H 0.9500 . ? C7H C8H 1.28(2) . ? C7H H7H 0.9500 . ? C8H C9H 1.29(2) . ? C8H H8H 0.9500 . ? C9H C10H 1.34(2) . ? C10H C11H 1.37(2) . ? C10H H10H 0.9500 . ? C11H C12H 1.443(18) . ? C11H H11H 0.9500 . ? C12H H12H 0.9500 . ? C13H N1H 1.444(14) . ? C13H C14H 1.511(12) . ? C13H C20H 1.545(14) . ? C13H H13H 1.0000 . ? C14H C19H 1.369(11) . ? C14H C15H 1.429(11) . ? C15H C16H 1.3900 . ? C15H H15H 0.9500 . ? C16H C17H 1.3900 . ? C16H H16H 0.9500 . ? C17H C18H 1.3900 . ? C17H H17H 0.9500 . ? C18H C19H 1.3900 . ? C18H H18H 0.9500 . ? C19H H19H 0.9500 . ? C20H O4H 1.233(12) . ? C20H O3H 1.247(14) . ? C1I O1I 1.228(15) . ? C1I C2I 1.423(16) . ? C1I N1I 1.435(15) . ? C2I C6I 1.392(17) . ? C2I C3I 1.400(17) . ? C3I C4I 1.388(17) . ? C3I C9I 1.523(16) . ? C4I C12I 1.313(18) . ? C4I C5I 1.470(16) . ? C5I O2I 1.236(15) . ? C5I N1I 1.378(14) . ? C6I C7I 1.44(2) . ? C6I H6I 0.9500 . ? C7I C8I 1.27(2) . ? C7I H7I 0.9500 . ? C8I C9I 1.302(19) . ? C8I H8I 0.9500 . ? C9I C10I 1.35(2) . ? C10I C11I 1.37(2) . ? C10I H10I 0.9500 . ? C11I C12I 1.441(18) . ? C11I H11I 0.9500 . ? C12I H12I 0.9500 . ? C13I N1I 1.463(14) . ? C13I C14I 1.524(10) . ? C13I C20I 1.559(15) . ? C13I H13I 1.0000 . ? C14I C19I 1.378(12) . ? C14I C15I 1.409(12) . ? C15I C16I 1.3900 . ? C15I H15I 0.9500 . ? C16I C17I 1.3900 . ? C16I H16I 0.9500 . ? C17I C18I 1.3900 . ? C17I H17I 0.9500 . ? C18I C19I 1.3900 . ? C18I H18I 0.9500 . ? C19I H19I 0.9500 . ? C20I O4I 1.256(13) . ? C20I O3I 1.284(13) . ? C21 O5 1.436(10) . ? C21 C22 1.488(14) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.489(16) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.494(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O5 1.441(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.451(13) . ? C25 O6 1.453(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.523(14) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.494(12) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O6 1.435(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.41(2) . ? C29 O7 1.472(16) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.45(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.50(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O7 1.476(16) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O8 1.466(11) . ? C33 C34 1.476(15) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.391(11) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.490(17) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 O8 1.414(11) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O41 C44 1.447(14) . ? O41 C41 1.461(14) . ? C41 C42 1.472(15) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.534(15) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.475(15) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? O51 C54 1.536(17) . ? O51 C51 1.540(17) . ? C51 C52 1.488(18) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.513(18) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.513(18) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? O52 C55 1.499(15) . ? O52 C58 1.530(15) . ? C55 C56 1.509(15) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.447(15) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.459(15) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? O61 C61 1.431(15) . ? O61 C64 1.517(15) . ? C61 C62 1.459(16) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.460(16) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.427(16) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? O71 C74 1.465(18) . ? O71 C71 1.514(18) . ? C71 C72 1.509(19) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.546(18) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.479(18) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? O72 C75 1.482(18) . ? O72 C78 1.503(19) . ? C75 C76 1.475(19) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 C77 1.496(19) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.527(19) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3B Cu1 O3D 171.6(2) . . ? O3B Cu1 O3A 91.3(2) . . ? O3D Cu1 O3A 88.8(2) . . ? O3B Cu1 O3C 87.9(2) . . ? O3D Cu1 O3C 89.7(2) . . ? O3A Cu1 O3C 164.3(2) . . ? O3B Cu1 O5 93.5(2) . . ? O3D Cu1 O5 94.9(2) . . ? O3A Cu1 O5 91.9(2) . . ? O3C Cu1 O5 103.7(2) . . ? O3B Cu1 Cu2 83.04(15) . . ? O3D Cu1 Cu2 88.71(15) . . ? O3A Cu1 Cu2 79.51(14) . . ? O3C Cu1 Cu2 84.87(14) . . ? O5 Cu1 Cu2 170.65(16) . . ? O4C Cu2 O4A 173.4(2) . . ? O4C Cu2 O4B 87.8(2) . . ? O4A Cu2 O4B 90.6(2) . . ? O4C Cu2 O4D 89.0(2) . . ? O4A Cu2 O4D 91.0(2) . . ? O4B Cu2 O4D 165.5(2) . . ? O4C Cu2 O6 93.61(19) . . ? O4A Cu2 O6 93.03(19) . . ? O4B Cu2 O6 106.4(2) . . ? O4D Cu2 O6 87.9(2) . . ? O4C Cu2 Cu1 83.61(14) . . ? O4A Cu2 Cu1 89.85(15) . . ? O4B Cu2 Cu1 85.73(14) . . ? O4D Cu2 Cu1 79.91(14) . . ? O6 Cu2 Cu1 167.53(14) . . ? O3H Cu3 O3F 169.2(5) . . ? O3H Cu3 O3E 93.0(6) . . ? O3F Cu3 O3E 90.7(3) . . ? O3H Cu3 O3G 85.3(6) . . ? O3F Cu3 O3G 89.6(3) . . ? O3E Cu3 O3G 171.5(2) . . ? O3H Cu3 O3I 12.4(7) . . ? O3F Cu3 O3I 160.1(5) . . ? O3E Cu3 O3I 84.7(5) . . ? O3G Cu3 O3I 92.2(5) . . ? O3H Cu3 O7 87.9(5) . . ? O3F Cu3 O7 102.1(3) . . ? O3E Cu3 O7 92.3(2) . . ? O3G Cu3 O7 95.9(2) . . ? O3I Cu3 O7 97.4(5) . . ? O3H Cu3 Cu4 81.6(4) . . ? O3F Cu3 Cu4 88.42(17) . . ? O3E Cu3 Cu4 88.03(17) . . ? O3G Cu3 Cu4 83.49(16) . . ? O3I Cu3 Cu4 72.1(4) . . ? O7 Cu3 Cu4 169.5(2) . . ? O4H Cu4 O4F 166.4(5) . . ? O4H Cu4 O4E 90.9(5) . . ? O4F Cu4 O4E 90.6(2) . . ? O4H Cu4 O4G 85.2(5) . . ? O4F Cu4 O4G 89.9(2) . . ? O4E Cu4 O4G 165.4(2) . . ? O4H Cu4 O4I 10.9(7) . . ? O4F Cu4 O4I 175.5(4) . . ? O4E Cu4 O4I 86.6(5) . . ? O4G Cu4 O4I 91.9(5) . . ? O4H Cu4 O8 106.2(5) . . ? O4F Cu4 O8 87.4(2) . . ? O4E Cu4 O8 88.1(2) . . ? O4G Cu4 O8 106.5(2) . . ? O4I Cu4 O8 96.0(5) . . ? O4H Cu4 Cu3 86.6(4) . . ? O4F Cu4 Cu3 80.31(16) . . ? O4E Cu4 Cu3 80.50(16) . . ? O4G Cu4 Cu3 85.19(15) . . ? O4I Cu4 Cu3 95.7(4) . . ? O8 Cu4 Cu3 163.05(15) . . ? O1A C1A N1A 119.8(8) . . ? O1A C1A C2A 123.8(7) . . ? N1A C1A C2A 116.4(7) . . ? C6A C2A C3A 120.1(8) . . ? C6A C2A C1A 118.9(8) . . ? C3A C2A C1A 120.9(7) . . ? C2A C3A C4A 120.4(7) . . ? C2A C3A C9A 119.7(7) . . ? C4A C3A C9A 119.8(7) . . ? C12A C4A C3A 120.3(7) . . ? C12A C4A C5A 119.6(7) . . ? C3A C4A C5A 120.0(7) . . ? O2A C5A N1A 119.4(7) . . ? O2A C5A C4A 123.0(7) . . ? N1A C5A C4A 117.5(7) . . ? C2A C6A C7A 119.8(8) . . ? C2A C6A H6A 120.1 . . ? C7A C6A H6A 120.1 . . ? C8A C7A C6A 121.4(8) . . ? C8A C7A H7A 119.3 . . ? C6A C7A H7A 119.3 . . ? C7A C8A C9A 119.2(8) . . ? C7A C8A H8A 120.4 . . ? C9A C8A H8A 120.4 . . ? C8A C9A C3A 119.7(8) . . ? C8A C9A C10A 122.4(8) . . ? C3A C9A C10A 117.8(7) . . ? C11A C10A C9A 120.8(8) . . ? C11A C10A H10A 119.6 . . ? C9A C10A H10A 119.6 . . ? C10A C11A C12A 121.0(8) . . ? C10A C11A H11A 119.5 . . ? C12A C11A H11A 119.5 . . ? C4A C12A C11A 120.1(8) . . ? C4A C12A H12A 119.9 . . ? C11A C12A H12A 119.9 . . ? N1A C13A C20A 111.1(6) . . ? N1A C13A C14A 115.3(6) . . ? C20A C13A C14A 114.2(6) . . ? N1A C13A H13A 105.0 . . ? C20A C13A H13A 105.0 . . ? C14A C13A H13A 105.0 . . ? O3A C20A O4A 129.0(7) . . ? O3A C20A C13A 118.2(7) . . ? O4A C20A C13A 112.8(7) . . ? C5A N1A C1A 124.4(7) . . ? C5A N1A C13A 117.9(6) . . ? C1A N1A C13A 117.6(6) . . ? C20A O3A Cu1 125.8(5) . . ? C20A O4A Cu2 115.1(5) . . ? C19A C14A C15A 118.2(9) . . ? C19A C14A C13A 118.3(8) . . ? C15A C14A C13A 123.3(8) . . ? C14A C15A C16A 118.9(11) . . ? C14A C15A H15A 120.5 . . ? C16A C15A H15A 120.5 . . ? C17A C16A C15A 121.2(11) . . ? C17A C16A H16A 119.4 . . ? C15A C16A H16A 119.4 . . ? C16A C17A C18A 120.5(11) . . ? C16A C17A H17A 119.7 . . ? C18A C17A H17A 119.7 . . ? C19A C18A C17A 117.9(13) . . ? C19A C18A H18A 121.0 . . ? C17A C18A H18A 121.0 . . ? C14A C19A C18A 123.2(12) . . ? C14A C19A H19A 118.4 . . ? C18A C19A H19A 118.4 . . ? O1B C1B N1B 121.0(7) . . ? O1B C1B C2B 122.8(7) . . ? N1B C1B C2B 116.2(7) . . ? C6B C2B C3B 121.1(8) . . ? C6B C2B C1B 119.3(8) . . ? C3B C2B C1B 119.6(7) . . ? C2B C3B C9B 118.9(8) . . ? C2B C3B C4B 121.6(7) . . ? C9B C3B C4B 119.4(8) . . ? C12B C4B C3B 119.2(7) . . ? C12B C4B C5B 121.6(7) . . ? C3B C4B C5B 119.1(7) . . ? O2B C5B N1B 119.0(7) . . ? O2B C5B C4B 122.6(7) . . ? N1B C5B C4B 118.4(7) . . ? C2B C6B C7B 119.1(9) . . ? C2B C6B H6B 120.4 . . ? C7B C6B H6B 120.4 . . ? C8B C7B C6B 120.5(9) . . ? C8B C7B H7B 119.8 . . ? C6B C7B H7B 119.8 . . ? C7B C8B C9B 122.9(9) . . ? C7B C8B H8B 118.5 . . ? C9B C8B H8B 118.5 . . ? C3B C9B C8B 117.3(9) . . ? C3B C9B C10B 119.1(9) . . ? C8B C9B C10B 123.5(9) . . ? C11B C10B C9B 120.2(9) . . ? C11B C10B H10B 119.9 . . ? C9B C10B H10B 119.9 . . ? C10B C11B C12B 120.9(9) . . ? C10B C11B H11B 119.6 . . ? C12B C11B H11B 119.6 . . ? C4B C12B C11B 121.0(9) . . ? C4B C12B H12B 119.5 . . ? C11B C12B H12B 119.5 . . ? N1B C13B C20B 108.8(6) . . ? N1B C13B C14B 110.6(6) . . ? C20B C13B C14B 117.1(7) . . ? N1B C13B H13B 106.6 . . ? C20B C13B H13B 106.6 . . ? C14B C13B H13B 106.6 . . ? C15B C14B C19B 120.4(10) . . ? C15B C14B C13B 123.9(8) . . ? C19B C14B C13B 115.7(10) . . ? C14B C15B C16B 121.6(11) . . ? C14B C15B H15B 119.2 . . ? C16B C15B H15B 119.2 . . ? C15B C16B C17B 116.1(13) . . ? C15B C16B H16B 121.9 . . ? C17B C16B H16B 121.9 . . ? C18B C17B C16B 120.9(11) . . ? C18B C17B H17B 119.6 . . ? C16B C17B H17B 119.6 . . ? C19B C18B C17B 118.8(13) . . ? C19B C18B H18B 120.6 . . ? C17B C18B H18B 120.6 . . ? C18B C19B C14B 121.6(13) . . ? C18B C19B H19B 119.2 . . ? C14B C19B H19B 119.2 . . ? O4B C20B O3B 127.5(7) . . ? O4B C20B C13B 118.3(6) . . ? O3B C20B C13B 114.2(6) . . ? C5B N1B C1B 124.8(6) . . ? C5B N1B C13B 117.4(6) . . ? C1B N1B C13B 117.7(6) . . ? C20B O3B Cu1 123.2(5) . . ? C20B O4B Cu2 119.2(5) . . ? O1C C1C N1C 120.6(8) . . ? O1C C1C C2C 122.5(9) . . ? N1C C1C C2C 116.9(10) . . ? C6C C2C C3C 121.2(10) . . ? C6C C2C C1C 119.2(11) . . ? C3C C2C C1C 119.6(9) . . ? C4C C3C C2C 122.3(8) . . ? C4C C3C C9C 116.7(12) . . ? C2C C3C C9C 121.0(12) . . ? C3C C4C C12C 122.1(9) . . ? C3C C4C C5C 120.7(9) . . ? C12C C4C C5C 117.0(10) . . ? O2C C5C N1C 122.3(7) . . ? O2C C5C C4C 124.1(8) . . ? N1C C5C C4C 113.6(8) . . ? C2C C6C C7C 118.8(15) . . ? C2C C6C H6C 120.6 . . ? C7C C6C H6C 120.6 . . ? C8C C7C C6C 120.2(14) . . ? C8C C7C H7C 119.9 . . ? C6C C7C H7C 119.9 . . ? C7C C8C C9C 122.6(15) . . ? C7C C8C H8C 118.7 . . ? C9C C8C H8C 118.7 . . ? C10C C9C C8C 121.0(14) . . ? C10C C9C C3C 122.9(14) . . ? C8C C9C C3C 116.1(15) . . ? C9C C10C C11C 119.4(12) . . ? C9C C10C H10C 120.3 . . ? C11C C10C H10C 120.3 . . ? C10C C11C C12C 119.9(14) . . ? C10C C11C H11C 120.0 . . ? C12C C11C H11C 120.0 . . ? C4C C12C C11C 118.9(13) . . ? C4C C12C H12C 120.5 . . ? C11C C12C H12C 120.5 . . ? N1C C13C C14C 114.3(6) . . ? N1C C13C C20C 106.4(6) . . ? C14C C13C C20C 117.4(6) . . ? N1C C13C H13C 106.0 . . ? C14C C13C H13C 106.0 . . ? C20C C13C H13C 106.0 . . ? C19C C14C C15C 116.5(7) . . ? C19C C14C C13C 120.5(7) . . ? C15C C14C C13C 122.5(7) . . ? C16C C15C C14C 121.6(9) . . ? C16C C15C H15C 119.2 . . ? C14C C15C H15C 119.2 . . ? C15C C16C C17C 120.5(9) . . ? C15C C16C H16C 119.8 . . ? C17C C16C H16C 119.8 . . ? C18C C17C C16C 119.5(8) . . ? C18C C17C H17C 120.3 . . ? C16C C17C H17C 120.3 . . ? C17C C18C C19C 120.0(9) . . ? C17C C18C H18C 120.0 . . ? C19C C18C H18C 120.0 . . ? C14C C19C C18C 121.8(9) . . ? C14C C19C H19C 119.1 . . ? C18C C19C H19C 119.1 . . ? O3C C20C O4C 126.7(6) . . ? O3C C20C C13C 120.4(6) . . ? O4C C20C C13C 112.9(6) . . ? C1C N1C C5C 126.8(7) . . ? C1C N1C C13C 117.2(7) . . ? C5C N1C C13C 114.7(7) . . ? C20C O3C Cu1 119.6(4) . . ? C20C O4C Cu2 124.9(5) . . ? O1D C1D N1D 119.0(7) . . ? O1D C1D C2D 124.4(9) . . ? N1D C1D C2D 116.7(9) . . ? C6D C2D C3D 119.8(10) . . ? C6D C2D C1D 120.6(11) . . ? C3D C2D C1D 119.6(9) . . ? C4D C3D C2D 123.3(9) . . ? C4D C3D C9D 121.5(12) . . ? C2D C3D C9D 115.1(11) . . ? C12D C4D C3D 122.0(10) . . ? C12D C4D C5D 120.0(11) . . ? C3D C4D C5D 117.9(9) . . ? O2D C5D N1D 120.4(8) . . ? O2D C5D C4D 122.6(9) . . ? N1D C5D C4D 117.0(9) . . ? C2D C6D C7D 119.6(14) . . ? C2D C6D H6D 120.2 . . ? C7D C6D H6D 120.2 . . ? C8D C7D C6D 123.0(15) . . ? C8D C7D H7D 118.5 . . ? C6D C7D H7D 118.5 . . ? C7D C8D C9D 120.1(15) . . ? C7D C8D H8D 119.9 . . ? C9D C8D H8D 119.9 . . ? C8D C9D C10D 125.2(13) . . ? C8D C9D C3D 122.2(14) . . ? C10D C9D C3D 112.4(13) . . ? C9D C10D C11D 126.5(13) . . ? C9D C10D H10D 116.8 . . ? C11D C10D H10D 116.8 . . ? C10D C11D C12D 119.2(13) . . ? C10D C11D H11D 120.4 . . ? C12D C11D H11D 120.4 . . ? C4D C12D C11D 118.0(13) . . ? C4D C12D H12D 121.0 . . ? C11D C12D H12D 121.0 . . ? N1D C13D C14D 115.2(6) . . ? N1D C13D C20D 109.0(6) . . ? C14D C13D C20D 115.2(6) . . ? N1D C13D H13D 105.5 . . ? C14D C13D H13D 105.5 . . ? C20D C13D H13D 105.5 . . ? C15D C14D C19D 120.0 . . ? C15D C14D C13D 124.0(6) . . ? C19D C14D C13D 116.0(6) . . ? C16D C15D C14D 120.0 . . ? C16D C15D H15D 120.0 . . ? C14D C15D H15D 120.0 . . ? C15D C16D C17D 120.0 . . ? C15D C16D H16D 120.0 . . ? C17D C16D H16D 120.0 . . ? C18D C17D C16D 120.0 . . ? C18D C17D H17D 120.0 . . ? C16D C17D H17D 120.0 . . ? C17D C18D C19D 120.0 . . ? C17D C18D H18D 120.0 . . ? C19D C18D H18D 120.0 . . ? C18D C19D C14D 120.0 . . ? C18D C19D H19D 120.0 . . ? C14D C19D H19D 120.0 . . ? O4D C20D O3D 127.1(7) . . ? O4D C20D C13D 115.1(6) . . ? O3D C20D C13D 117.7(6) . . ? C5D N1D C1D 125.3(7) . . ? C5D N1D C13D 118.1(7) . . ? C1D N1D C13D 116.4(7) . . ? C20D O3D Cu1 117.5(5) . . ? C20D O4D Cu2 126.3(5) . . ? O1E C1E N1E 118.7(10) . . ? O1E C1E C2E 123.5(12) . . ? N1E C1E C2E 117.8(12) . . ? C3E C2E C1E 120.4(11) . . ? C3E C2E C6E 123.3(13) . . ? C1E C2E C6E 116.3(15) . . ? C9E C3E C4E 122.5(15) . . ? C9E C3E C2E 116.9(14) . . ? C4E C3E C2E 120.6(10) . . ? C12E C4E C3E 118.0(11) . . ? C12E C4E C5E 123.8(11) . . ? C3E C4E C5E 118.2(12) . . ? O2E C5E N1E 120.9(9) . . ? O2E C5E C4E 118.6(11) . . ? N1E C5E C4E 120.5(9) . . ? C2E C6E C7E 112.0(15) . . ? C2E C6E H6E 124.0 . . ? C7E C6E H6E 124.0 . . ? C8E C7E C6E 126.7(17) . . ? C8E C7E H7E 116.7 . . ? C6E C7E H7E 116.7 . . ? C7E C8E C9E 119.0(15) . . ? C7E C8E H8E 120.5 . . ? C9E C8E H8E 120.5 . . ? C3E C9E C10E 117.2(15) . . ? C3E C9E C8E 122.1(17) . . ? C10E C9E C8E 120.8(14) . . ? C11E C10E C9E 122.1(13) . . ? C11E C10E H10E 118.9 . . ? C9E C10E H10E 118.9 . . ? C10E C11E C12E 117.0(14) . . ? C10E C11E H11E 121.5 . . ? C12E C11E H11E 121.5 . . ? C4E C12E C11E 123.2(13) . . ? C4E C12E H12E 118.4 . . ? C11E C12E H12E 118.4 . . ? N1E C13E C20E 111.7(8) . . ? N1E C13E C14E 107.1(9) . . ? C20E C13E C14E 113.1(9) . . ? N1E C13E H13E 108.2 . . ? C20E C13E H13E 108.2 . . ? C14E C13E H13E 108.2 . . ? C15E C14E C19E 120.0 . . ? C15E C14E C13E 129.5(10) . . ? C19E C14E C13E 110.5(10) . . ? C16E C15E C14E 120.0 . . ? C16E C15E H15E 120.0 . . ? C14E C15E H15E 120.0 . . ? C15E C16E C17E 120.0 . . ? C15E C16E H16E 120.0 . . ? C17E C16E H16E 120.0 . . ? C18E C17E C16E 120.0 . . ? C18E C17E H17E 120.0 . . ? C16E C17E H17E 120.0 . . ? C17E C18E C19E 120.0 . . ? C17E C18E H18E 120.0 . . ? C19E C18E H18E 120.0 . . ? C18E C19E C14E 120.0 . . ? C18E C19E H19E 120.0 . . ? C14E C19E H19E 120.0 . . ? C15K C14K C19K 120.0 . . ? C16K C15K C14K 120.0 . . ? C16K C15K H15K 120.0 . . ? C14K C15K H15K 120.0 . . ? C15K C16K C17K 120.0 . . ? C15K C16K H16K 120.0 . . ? C17K C16K H16K 120.0 . . ? C16K C17K C18K 120.0 . . ? C16K C17K H17K 120.0 . . ? C18K C17K H17K 120.0 . . ? C19K C18K C17K 120.0 . . ? C19K C18K H18K 120.0 . . ? C17K C18K H18K 120.0 . . ? C18K C19K C14K 120.0 . . ? C18K C19K H19K 120.0 . . ? C14K C19K H19K 120.0 . . ? O3E C20E O4E 126.2(7) . . ? O3E C20E C13E 120.5(8) . . ? O4E C20E C13E 113.3(8) . . ? C5E N1E C1E 122.5(9) . . ? C5E N1E C13E 117.5(8) . . ? C1E N1E C13E 119.8(9) . . ? C20E O3E Cu3 118.7(5) . . ? C20E O4E Cu4 126.4(5) . . ? O1F C1F N1F 120.1(9) . . ? O1F C1F C2F 125.3(9) . . ? N1F C1F C2F 114.5(9) . . ? C6F C2F C3F 121.7(9) . . ? C6F C2F C1F 115.8(10) . . ? C3F C2F C1F 122.5(8) . . ? C4F C3F C2F 120.4(8) . . ? C4F C3F C9F 119.6(9) . . ? C2F C3F C9F 119.9(9) . . ? C12F C4F C3F 120.0(8) . . ? C12F C4F C5F 119.8(8) . . ? C3F C4F C5F 120.1(8) . . ? O2F C5F N1F 119.5(8) . . ? O2F C5F C4F 123.5(8) . . ? N1F C5F C4F 116.9(8) . . ? C2F C6F C7F 118.0(12) . . ? C2F C6F H6F 121.0 . . ? C7F C6F H6F 121.0 . . ? C8F C7F C6F 121.3(12) . . ? C8F C7F H7F 119.3 . . ? C6F C7F H7F 119.3 . . ? C7F C8F C9F 120.0(11) . . ? C7F C8F H8F 120.0 . . ? C9F C8F H8F 120.0 . . ? C10F C9F C8F 122.4(11) . . ? C10F C9F C3F 118.6(10) . . ? C8F C9F C3F 118.9(11) . . ? C11F C10F C9F 120.9(11) . . ? C11F C10F H10F 119.6 . . ? C9F C10F H10F 119.6 . . ? C10F C11F C12F 120.3(11) . . ? C10F C11F H11F 119.9 . . ? C12F C11F H11F 119.9 . . ? C4F C12F C11F 120.5(10) . . ? C4F C12F H12F 119.8 . . ? C11F C12F H12F 119.8 . . ? N1F C13F C20F 109.6(7) . . ? N1F C13F C14F 114.7(7) . . ? C20F C13F C14F 115.2(7) . . ? N1F C13F H13F 105.4 . . ? C20F C13F H13F 105.4 . . ? C14F C13F H13F 105.4 . . ? C15F C14F C19F 120.0 . . ? C15F C14F C13F 122.7(6) . . ? C19F C14F C13F 117.2(6) . . ? C16F C15F C14F 120.0 . . ? C16F C15F H15F 120.0 . . ? C14F C15F H15F 120.0 . . ? C17F C16F C15F 120.0 . . ? C17F C16F H16F 120.0 . . ? C15F C16F H16F 120.0 . . ? C16F C17F C18F 120.0 . . ? C16F C17F H17F 120.0 . . ? C18F C17F H17F 120.0 . . ? C19F C18F C17F 120.0 . . ? C19F C18F H18F 120.0 . . ? C17F C18F H18F 120.0 . . ? C18F C19F C14F 120.0 . . ? C18F C19F H19F 120.0 . . ? C14F C19F H19F 120.0 . . ? O3F C20F O4F 125.0(9) . . ? O3F C20F C13F 122.0(8) . . ? O4F C20F C13F 112.7(8) . . ? C5F N1F C1F 125.5(8) . . ? C5F N1F C13F 117.2(7) . . ? C1F N1F C13F 115.9(7) . . ? C20F O3F Cu3 118.7(6) . . ? C20F O4F Cu4 127.4(6) . . ? O1G C1G N1G 120.8(7) . . ? O1G C1G C2G 124.2(6) . . ? N1G C1G C2G 115.0(7) . . ? C3G C2G C6G 119.9(7) . . ? C3G C2G C1G 122.6(7) . . ? C6G C2G C1G 117.4(7) . . ? C2G C3G C4G 120.7(8) . . ? C2G C3G C9G 121.0(7) . . ? C4G C3G C9G 118.3(7) . . ? C12G C4G C3G 121.4(9) . . ? C12G C4G C5G 118.7(8) . . ? C3G C4G C5G 119.8(8) . . ? O2G C5G N1G 119.0(8) . . ? O2G C5G C4G 123.7(8) . . ? N1G C5G C4G 117.3(7) . . ? C2G C6G C7G 120.0(8) . . ? C2G C6G H6G 120.0 . . ? C7G C6G H6G 120.0 . . ? C8G C7G C6G 120.1(8) . . ? C8G C7G H7G 119.9 . . ? C6G C7G H7G 119.9 . . ? C7G C8G C9G 122.5(8) . . ? C7G C8G H8G 118.8 . . ? C9G C8G H8G 118.8 . . ? C10G C9G C8G 124.8(9) . . ? C10G C9G C3G 118.8(8) . . ? C8G C9G C3G 116.4(7) . . ? C11G C10G C9G 122.9(10) . . ? C11G C10G H10G 118.5 . . ? C9G C10G H10G 118.5 . . ? C10G C11G C12G 119.6(9) . . ? C10G C11G H11G 120.2 . . ? C12G C11G H11G 120.2 . . ? C4G C12G C11G 118.8(9) . . ? C4G C12G H12G 120.6 . . ? C11G C12G H12G 120.6 . . ? N1G C13G C20G 111.9(7) . . ? N1G C13G C14G 117.5(7) . . ? C20G C13G C14G 118.5(7) . . ? N1G C13G H13G 101.8 . . ? C20G C13G H13G 101.8 . . ? C14G C13G H13G 101.8 . . ? C15G C14G C19G 120.0 . . ? C15G C14G C13G 117.4(7) . . ? C19G C14G C13G 122.3(7) . . ? C14G C15G C16G 120.0 . . ? C14G C15G H15G 120.0 . . ? C16G C15G H15G 120.0 . . ? C15G C16G C17G 120.0 . . ? C15G C16G H16G 120.0 . . ? C17G C16G H16G 120.0 . . ? C18G C17G C16G 120.0 . . ? C18G C17G H17G 120.0 . . ? C16G C17G H17G 120.0 . . ? C19G C18G C17G 120.0 . . ? C19G C18G H18G 120.0 . . ? C17G C18G H18G 120.0 . . ? C18G C19G C14G 120.0 . . ? C18G C19G H19G 120.0 . . ? C14G C19G H19G 120.0 . . ? C15J C14J C19J 120.0 . . ? C14J C15J C16J 120.0 . . ? C14J C15J H15J 120.0 . . ? C16J C15J H15J 120.0 . . ? C15J C16J C17J 120.0 . . ? C15J C16J H16J 120.0 . . ? C17J C16J H16J 120.0 . . ? C18J C17J C16J 120.0 . . ? C18J C17J H17J 120.0 . . ? C16J C17J H17J 120.0 . . ? C17J C18J C19J 120.0 . . ? C17J C18J H18J 120.0 . . ? C19J C18J H18J 120.0 . . ? C18J C19J C14J 120.0 . . ? C18J C19J H19J 120.0 . . ? C14J C19J H19J 120.0 . . ? O3G C20G O4G 128.2(7) . . ? O3G C20G C13G 115.2(7) . . ? O4G C20G C13G 116.5(7) . . ? C5G N1G C1G 124.4(7) . . ? C5G N1G C13G 118.8(6) . . ? C1G N1G C13G 116.8(7) . . ? C20G O3G Cu3 122.6(5) . . ? C20G O4G Cu4 120.2(5) . . ? O1H C1H C2H 123.1(14) . . ? O1H C1H N1H 119.5(14) . . ? C2H C1H N1H 117.4(13) . . ? C6H C2H C3H 120.5(16) . . ? C6H C2H C1H 119.3(16) . . ? C3H C2H C1H 120.3(14) . . ? C4H C3H C2H 122.2(13) . . ? C4H C3H C9H 125.7(14) . . ? C2H C3H C9H 112.1(13) . . ? C12H C4H C3H 118.6(14) . . ? C12H C4H C5H 121.9(15) . . ? C3H C4H C5H 119.4(14) . . ? O2H C5H N1H 120.2(13) . . ? O2H C5H C4H 123.6(14) . . ? N1H C5H C4H 116.2(13) . . ? C2H C6H C7H 122(2) . . ? C2H C6H H6H 119.2 . . ? C7H C6H H6H 119.2 . . ? C8H C7H C6H 119(2) . . ? C8H C7H H7H 120.7 . . ? C6H C7H H7H 120.7 . . ? C7H C8H C9H 124(2) . . ? C7H C8H H8H 118.2 . . ? C9H C8H H8H 118.2 . . ? C8H C9H C10H 125.5(18) . . ? C8H C9H C3H 123.7(18) . . ? C10H C9H C3H 110.7(16) . . ? C9H C10H C11H 122.7(18) . . ? C9H C10H H10H 118.7 . . ? C11H C10H H10H 118.7 . . ? C10H C11H C12H 124.3(17) . . ? C10H C11H H11H 117.9 . . ? C12H C11H H11H 117.9 . . ? C4H C12H C11H 117.9(16) . . ? C4H C12H H12H 121.0 . . ? C11H C12H H12H 121.0 . . ? N1H C13H C14H 112.7(11) . . ? N1H C13H C20H 116.7(10) . . ? C14H C13H C20H 111.0(11) . . ? N1H C13H H13H 105.1 . . ? C14H C13H H13H 105.1 . . ? C20H C13H H13H 105.1 . . ? C19H C14H C15H 118.7(8) . . ? C19H C14H C13H 114.3(9) . . ? C15H C14H C13H 126.3(10) . . ? C16H C15H C14H 118.9(5) . . ? C16H C15H H15H 120.6 . . ? C14H C15H H15H 120.6 . . ? C17H C16H C15H 120.0 . . ? C17H C16H H16H 120.0 . . ? C15H C16H H16H 120.0 . . ? C18H C17H C16H 120.0 . . ? C18H C17H H17H 120.0 . . ? C16H C17H H17H 120.0 . . ? C17H C18H C19H 120.0 . . ? C17H C18H H18H 120.0 . . ? C19H C18H H18H 120.0 . . ? C14H C19H C18H 120.3(5) . . ? C14H C19H H19H 119.9 . . ? C18H C19H H19H 119.9 . . ? O4H C20H O3H 128.8(13) . . ? O4H C20H C13H 116.5(11) . . ? O3H C20H C13H 113.6(10) . . ? C5H N1H C1H 124.5(12) . . ? C5H N1H C13H 119.4(11) . . ? C1H N1H C13H 116.1(11) . . ? C20H O3H Cu3 125.7(10) . . ? C20H O4H Cu4 116.9(11) . . ? O1I C1I C2I 126.2(16) . . ? O1I C1I N1I 117.2(15) . . ? C2I C1I N1I 116.6(13) . . ? C6I C2I C3I 117.3(14) . . ? C6I C2I C1I 120.7(15) . . ? C3I C2I C1I 122.0(13) . . ? C4I C3I C2I 121.9(12) . . ? C4I C3I C9I 122.2(13) . . ? C2I C3I C9I 115.9(13) . . ? C12I C4I C3I 122.8(13) . . ? C12I C4I C5I 120.3(14) . . ? C3I C4I C5I 116.7(13) . . ? O2I C5I N1I 118.8(13) . . ? O2I C5I C4I 120.1(13) . . ? N1I C5I C4I 121.2(13) . . ? C2I C6I C7I 121.7(18) . . ? C2I C6I H6I 119.1 . . ? C7I C6I H6I 119.1 . . ? C8I C7I C6I 121.0(18) . . ? C8I C7I H7I 119.5 . . ? C6I C7I H7I 119.5 . . ? C7I C8I C9I 121.9(18) . . ? C7I C8I H8I 119.1 . . ? C9I C8I H8I 119.1 . . ? C8I C9I C10I 126.3(16) . . ? C8I C9I C3I 122.2(16) . . ? C10I C9I C3I 111.5(15) . . ? C9I C10I C11I 124.6(17) . . ? C9I C10I H10I 117.7 . . ? C11I C10I H10I 117.7 . . ? C10I C11I C12I 122.9(16) . . ? C10I C11I H11I 118.6 . . ? C12I C11I H11I 118.6 . . ? C4I C12I C11I 115.9(16) . . ? C4I C12I H12I 122.0 . . ? C11I C12I H12I 122.0 . . ? N1I C13I C14I 119.4(13) . . ? N1I C13I C20I 109.5(10) . . ? C14I C13I C20I 119.2(13) . . ? N1I C13I H13I 101.6 . . ? C14I C13I H13I 101.6 . . ? C20I C13I H13I 101.6 . . ? C19I C14I C15I 119.5(9) . . ? C19I C14I C13I 117.2(11) . . ? C15I C14I C13I 123.3(11) . . ? C16I C15I C14I 119.9(5) . . ? C16I C15I H15I 120.1 . . ? C14I C15I H15I 120.1 . . ? C17I C16I C15I 120.0 . . ? C17I C16I H16I 120.0 . . ? C15I C16I H16I 120.0 . . ? C16I C17I C18I 120.0 . . ? C16I C17I H17I 120.0 . . ? C18I C17I H17I 120.0 . . ? C19I C18I C17I 120.0 . . ? C19I C18I H18I 120.0 . . ? C17I C18I H18I 120.0 . . ? C14I C19I C18I 120.6(5) . . ? C14I C19I H19I 119.7 . . ? C18I C19I H19I 119.7 . . ? O4I C20I O3I 119.7(13) . . ? O4I C20I C13I 114.5(13) . . ? O3I C20I C13I 122.0(11) . . ? C5I N1I C1I 121.4(12) . . ? C5I N1I C13I 121.6(13) . . ? C1I N1I C13I 115.9(12) . . ? C20I O3I Cu3 138.0(11) . . ? C20I O4I Cu4 114.1(10) . . ? O5 C21 C22 106.9(8) . . ? O5 C21 H21A 110.3 . . ? C22 C21 H21A 110.3 . . ? O5 C21 H21B 110.3 . . ? C22 C21 H21B 110.3 . . ? H21A C21 H21B 108.6 . . ? C21 C22 C23 103.9(8) . . ? C21 C22 H22A 111.0 . . ? C23 C22 H22A 111.0 . . ? C21 C22 H22B 111.0 . . ? C23 C22 H22B 111.0 . . ? H22A C22 H22B 109.0 . . ? C22 C23 C24 105.5(9) . . ? C22 C23 H23A 110.6 . . ? C24 C23 H23A 110.6 . . ? C22 C23 H23B 110.6 . . ? C24 C23 H23B 110.6 . . ? H23A C23 H23B 108.8 . . ? O5 C24 C23 105.7(8) . . ? O5 C24 H24A 110.6 . . ? C23 C24 H24A 110.6 . . ? O5 C24 H24B 110.6 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.7 . . ? C21 O5 C24 109.9(6) . . ? C21 O5 Cu1 119.8(5) . . ? C24 O5 Cu1 122.3(5) . . ? C26 C25 O6 106.9(7) . . ? C26 C25 H25A 110.3 . . ? O6 C25 H25A 110.3 . . ? C26 C25 H25B 110.3 . . ? O6 C25 H25B 110.3 . . ? H25A C25 H25B 108.6 . . ? C25 C26 C27 102.3(8) . . ? C25 C26 H26A 111.3 . . ? C27 C26 H26A 111.3 . . ? C25 C26 H26B 111.3 . . ? C27 C26 H26B 111.3 . . ? H26A C26 H26B 109.2 . . ? C28 C27 C26 104.0(7) . . ? C28 C27 H27A 111.0 . . ? C26 C27 H27A 111.0 . . ? C28 C27 H27B 111.0 . . ? C26 C27 H27B 111.0 . . ? H27A C27 H27B 109.0 . . ? O6 C28 C27 105.1(7) . . ? O6 C28 H28A 110.7 . . ? C27 C28 H28A 110.7 . . ? O6 C28 H28B 110.7 . . ? C27 C28 H28B 110.7 . . ? H28A C28 H28B 108.8 . . ? C28 O6 C25 109.4(6) . . ? C28 O6 Cu2 118.3(4) . . ? C25 O6 Cu2 116.8(4) . . ? C30 C29 O7 105.5(14) . . ? C30 C29 H29A 110.6 . . ? O7 C29 H29A 110.6 . . ? C30 C29 H29B 110.6 . . ? O7 C29 H29B 110.6 . . ? H29A C29 H29B 108.8 . . ? C29 C30 C31 107.6(15) . . ? C29 C30 H30A 110.2 . . ? C31 C30 H30A 110.2 . . ? C29 C30 H30B 110.2 . . ? C31 C30 H30B 110.2 . . ? H30A C30 H30B 108.5 . . ? C30 C31 C32 106.2(15) . . ? C30 C31 H31A 110.5 . . ? C32 C31 H31A 110.5 . . ? C30 C31 H31B 110.5 . . ? C32 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? O7 C32 C31 103.4(14) . . ? O7 C32 H32A 111.1 . . ? C31 C32 H32A 111.1 . . ? O7 C32 H32B 111.1 . . ? C31 C32 H32B 111.1 . . ? H32A C32 H32B 109.0 . . ? C29 O7 C32 102.5(11) . . ? C29 O7 Cu3 119.9(8) . . ? C32 O7 Cu3 116.2(8) . . ? O8 C33 C34 104.8(8) . . ? O8 C33 H33A 110.8 . . ? C34 C33 H33A 110.8 . . ? O8 C33 H33B 110.8 . . ? C34 C33 H33B 110.8 . . ? H33A C33 H33B 108.9 . . ? C35 C34 C33 109.8(9) . . ? C35 C34 H34A 109.7 . . ? C33 C34 H34A 109.7 . . ? C35 C34 H34B 109.7 . . ? C33 C34 H34B 109.7 . . ? H34A C34 H34B 108.2 . . ? C34 C35 C36 107.8(10) . . ? C34 C35 H35A 110.2 . . ? C36 C35 H35A 110.2 . . ? C34 C35 H35B 110.2 . . ? C36 C35 H35B 110.2 . . ? H35A C35 H35B 108.5 . . ? O8 C36 C35 106.4(9) . . ? O8 C36 H36A 110.5 . . ? C35 C36 H36A 110.5 . . ? O8 C36 H36B 110.5 . . ? C35 C36 H36B 110.5 . . ? H36A C36 H36B 108.6 . . ? C36 O8 C33 109.4(7) . . ? C36 O8 Cu4 120.9(5) . . ? C33 O8 Cu4 121.5(5) . . ? C44 O41 C41 106.0(8) . . ? O41 C41 C42 109.3(8) . . ? O41 C41 H41A 109.8 . . ? C42 C41 H41A 109.8 . . ? O41 C41 H41B 109.8 . . ? C42 C41 H41B 109.8 . . ? H41A C41 H41B 108.3 . . ? C41 C42 C43 103.5(8) . . ? C41 C42 H42A 111.1 . . ? C43 C42 H42A 111.1 . . ? C41 C42 H42B 111.1 . . ? C43 C42 H42B 111.1 . . ? H42A C42 H42B 109.0 . . ? C44 C43 C42 102.4(9) . . ? C44 C43 H43A 111.3 . . ? C42 C43 H43A 111.3 . . ? C44 C43 H43B 111.3 . . ? C42 C43 H43B 111.3 . . ? H43A C43 H43B 109.2 . . ? O41 C44 C43 108.6(9) . . ? O41 C44 H44A 110.0 . . ? C43 C44 H44A 110.0 . . ? O41 C44 H44B 110.0 . . ? C43 C44 H44B 110.0 . . ? H44A C44 H44B 108.4 . . ? C54 O51 C51 105.5(8) . . ? C52 C51 O51 109.3(9) . . ? C52 C51 H51A 109.8 . . ? O51 C51 H51A 109.8 . . ? C52 C51 H51B 109.8 . . ? O51 C51 H51B 109.8 . . ? H51A C51 H51B 108.3 . . ? C51 C52 C53 108.0(8) . . ? C51 C52 H52A 110.1 . . ? C53 C52 H52A 110.1 . . ? C51 C52 H52B 110.1 . . ? C53 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? C52 C53 C54 108.3(8) . . ? C52 C53 H53A 110.0 . . ? C54 C53 H53A 110.0 . . ? C52 C53 H53B 110.0 . . ? C54 C53 H53B 110.0 . . ? H53A C53 H53B 108.4 . . ? C53 C54 O51 107.9(9) . . ? C53 C54 H54A 110.1 . . ? O51 C54 H54A 110.1 . . ? C53 C54 H54B 110.1 . . ? O51 C54 H54B 110.1 . . ? H54A C54 H54B 108.4 . . ? C55 O52 C58 95.1(13) . . ? O52 C55 C56 94.9(13) . . ? O52 C55 H55A 112.8 . . ? C56 C55 H55A 112.8 . . ? O52 C55 H55B 112.8 . . ? C56 C55 H55B 112.8 . . ? H55A C55 H55B 110.2 . . ? C57 C56 C55 101.9(11) . . ? C57 C56 H56A 111.4 . . ? C55 C56 H56A 111.4 . . ? C57 C56 H56B 111.4 . . ? C55 C56 H56B 111.4 . . ? H56A C56 H56B 109.2 . . ? C56 C57 C58 107.1(8) . . ? C56 C57 H57A 110.3 . . ? C58 C57 H57A 110.3 . . ? C56 C57 H57B 110.3 . . ? C58 C57 H57B 110.3 . . ? H57A C57 H57B 108.6 . . ? C57 C58 O52 100.1(11) . . ? C57 C58 H58A 111.8 . . ? O52 C58 H58A 111.8 . . ? C57 C58 H58B 111.8 . . ? O52 C58 H58B 111.8 . . ? H58A C58 H58B 109.5 . . ? C61 O61 C64 105.3(9) . . ? O61 C61 C62 108.1(8) . . ? O61 C61 H61A 110.1 . . ? C62 C61 H61A 110.1 . . ? O61 C61 H61B 110.1 . . ? C62 C61 H61B 110.1 . . ? H61A C61 H61B 108.4 . . ? C61 C62 C63 104.4(9) . . ? C61 C62 H62A 110.9 . . ? C63 C62 H62A 110.9 . . ? C61 C62 H62B 110.9 . . ? C63 C62 H62B 110.9 . . ? H62A C62 H62B 108.9 . . ? C64 C63 C62 106.0(10) . . ? C64 C63 H63A 110.5 . . ? C62 C63 H63A 110.5 . . ? C64 C63 H63B 110.5 . . ? C62 C63 H63B 110.5 . . ? H63A C63 H63B 108.7 . . ? C63 C64 O61 101.9(9) . . ? C63 C64 H64A 111.4 . . ? O61 C64 H64A 111.4 . . ? C63 C64 H64B 111.4 . . ? O61 C64 H64B 111.4 . . ? H64A C64 H64B 109.3 . . ? C74 O71 C71 106.7(9) . . ? C72 C71 O71 101.9(12) . . ? C72 C71 H71A 111.4 . . ? O71 C71 H71A 111.4 . . ? C72 C71 H71B 111.4 . . ? O71 C71 H71B 111.4 . . ? H71A C71 H71B 109.3 . . ? C71 C72 C73 100.6(14) . . ? C71 C72 H72A 111.7 . . ? C73 C72 H72A 111.7 . . ? C71 C72 H72B 111.7 . . ? C73 C72 H72B 111.7 . . ? H72A C72 H72B 109.4 . . ? C74 C73 C72 100.5(12) . . ? C74 C73 H73A 111.7 . . ? C72 C73 H73A 111.7 . . ? C74 C73 H73B 111.7 . . ? C72 C73 H73B 111.7 . . ? H73A C73 H73B 109.4 . . ? O71 C74 C73 107.6(10) . . ? O71 C74 H74A 110.2 . . ? C73 C74 H74A 110.2 . . ? O71 C74 H74B 110.2 . . ? C73 C74 H74B 110.2 . . ? H74A C74 H74B 108.5 . . ? C75 O72 C78 107.0(10) . . ? C76 C75 O72 107.6(9) . . ? C76 C75 H75A 110.2 . . ? O72 C75 H75A 110.2 . . ? C76 C75 H75B 110.2 . . ? O72 C75 H75B 110.2 . . ? H75A C75 H75B 108.5 . . ? C75 C76 C77 106.5(12) . . ? C75 C76 H76A 110.4 . . ? C77 C76 H76A 110.4 . . ? C75 C76 H76B 110.4 . . ? C77 C76 H76B 110.4 . . ? H76A C76 H76B 108.6 . . ? C76 C77 C78 103.3(13) . . ? C76 C77 H77A 111.1 . . ? C78 C77 H77A 111.1 . . ? H77A C77 H77B 109.1 . . ? O72 C78 C77 103.9(12) . . ? O72 C78 H78A 111.0 . . ? C77 C78 H78A 111.0 . . ? O72 C78 H78B 111.0 . . ? C77 C78 H78B 111.0 . . ? H78A C78 H78B 109.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3B Cu1 Cu2 O4C 92.7(2) . . . . ? O3D Cu1 Cu2 O4C -85.6(2) . . . . ? O3A Cu1 Cu2 O4C -174.6(2) . . . . ? O3C Cu1 Cu2 O4C 4.2(2) . . . . ? O3B Cu1 Cu2 O4A -86.2(2) . . . . ? O3D Cu1 Cu2 O4A 95.5(2) . . . . ? O3A Cu1 Cu2 O4A 6.5(2) . . . . ? O3C Cu1 Cu2 O4A -174.7(2) . . . . ? O3B Cu1 Cu2 O4B 4.5(2) . . . . ? O3D Cu1 Cu2 O4B -173.9(2) . . . . ? O3A Cu1 Cu2 O4B 97.1(2) . . . . ? O3C Cu1 Cu2 O4B -84.1(2) . . . . ? O3B Cu1 Cu2 O4D -177.2(2) . . . . ? O3D Cu1 Cu2 O4D 4.5(2) . . . . ? O3A Cu1 Cu2 O4D -84.5(2) . . . . ? O3C Cu1 Cu2 O4D 94.3(2) . . . . ? O3B Cu1 Cu2 O6 170.4(6) . . . . ? O3D Cu1 Cu2 O6 -7.9(6) . . . . ? O3A Cu1 Cu2 O6 -97.0(6) . . . . ? O3C Cu1 Cu2 O6 81.9(6) . . . . ? O3H Cu3 Cu4 O4H -1.5(7) . . . . ? O3F Cu3 Cu4 O4H 174.5(6) . . . . ? O3E Cu3 Cu4 O4H -94.8(6) . . . . ? O3G Cu3 Cu4 O4H 84.7(6) . . . . ? O3I Cu3 Cu4 O4H -9.7(7) . . . . ? O7 Cu3 Cu4 O4H -2.6(11) . . . . ? O3H Cu3 Cu4 O4F -177.7(6) . . . . ? O3F Cu3 Cu4 O4F -1.7(2) . . . . ? O3E Cu3 Cu4 O4F 89.0(2) . . . . ? O3G Cu3 Cu4 O4F -91.5(3) . . . . ? O3I Cu3 Cu4 O4F 174.1(5) . . . . ? O3H Cu3 Cu4 O4E 90.0(6) . . . . ? O3F Cu3 Cu4 O4E -94.0(3) . . . . ? O3E Cu3 Cu4 O4E -3.2(2) . . . . ? O3G Cu3 Cu4 O4E 176.2(3) . . . . ? O3I Cu3 Cu4 O4E 81.8(5) . . . . ? O7 Cu3 Cu4 O4E 88.9(10) . . . . ? O3H Cu3 Cu4 O4G -87.0(6) . . . . ? O3F Cu3 Cu4 O4G 89.0(2) . . . . ? O3E Cu3 Cu4 O4G 179.7(2) . . . . ? O3G Cu3 Cu4 O4G -0.8(2) . . . . ? O3I Cu3 Cu4 O4G -95.2(5) . . . . ? O7 Cu3 Cu4 O4G -88.1(10) . . . . ? O3H Cu3 Cu4 O4I 4.5(7) . . . . ? O3F Cu3 Cu4 O4I -179.6(5) . . . . ? O3E Cu3 Cu4 O4I -88.8(5) . . . . ? O3G Cu3 Cu4 O4I 90.7(5) . . . . ? O3I Cu3 Cu4 O4I -3.7(7) . . . . ? O7 Cu3 Cu4 O4I 3.4(11) . . . . ? O3H Cu3 Cu4 O8 138.3(7) . . . . ? O3F Cu3 Cu4 O8 -45.8(5) . . . . ? O3E Cu3 Cu4 O8 45.0(5) . . . . ? O3G Cu3 Cu4 O8 -135.5(5) . . . . ? O3I Cu3 Cu4 O8 130.1(7) . . . . ? O7 Cu3 Cu4 O8 137.2(11) . . . . ? O1A C1A C2A C6A 6.7(12) . . . . ? N1A C1A C2A C6A -175.1(7) . . . . ? O1A C1A C2A C3A -172.8(7) . . . . ? N1A C1A C2A C3A 5.4(10) . . . . ? C6A C2A C3A C4A 174.8(7) . . . . ? C1A C2A C3A C4A -5.8(11) . . . . ? C6A C2A C3A C9A -1.1(11) . . . . ? C1A C2A C3A C9A 178.3(7) . . . . ? C2A C3A C4A C12A -179.3(7) . . . . ? C9A C3A C4A C12A -3.4(11) . . . . ? C2A C3A C4A C5A 1.0(10) . . . . ? C9A C3A C4A C5A 176.9(7) . . . . ? C12A C4A C5A O2A 2.4(11) . . . . ? C3A C4A C5A O2A -177.8(7) . . . . ? C12A C4A C5A N1A -175.8(7) . . . . ? C3A C4A C5A N1A 4.0(10) . . . . ? C3A C2A C6A C7A -0.3(12) . . . . ? C1A C2A C6A C7A -179.8(7) . . . . ? C2A C6A C7A C8A 2.7(13) . . . . ? C6A C7A C8A C9A -3.5(14) . . . . ? C7A C8A C9A C3A 2.0(13) . . . . ? C7A C8A C9A C10A -176.4(9) . . . . ? C2A C3A C9A C8A 0.3(11) . . . . ? C4A C3A C9A C8A -175.6(7) . . . . ? C2A C3A C9A C10A 178.8(7) . . . . ? C4A C3A C9A C10A 2.9(11) . . . . ? C8A C9A C10A C11A 177.1(8) . . . . ? C3A C9A C10A C11A -1.4(12) . . . . ? C9A C10A C11A C12A 0.3(14) . . . . ? C3A C4A C12A C11A 2.3(12) . . . . ? C5A C4A C12A C11A -177.9(7) . . . . ? C10A C11A C12A C4A -0.8(13) . . . . ? N1A C13A C20A O3A 134.7(7) . . . . ? C14A C13A C20A O3A 2.3(10) . . . . ? N1A C13A C20A O4A -45.4(8) . . . . ? C14A C13A C20A O4A -177.8(7) . . . . ? O2A C5A N1A C1A 177.4(6) . . . . ? C4A C5A N1A C1A -4.3(10) . . . . ? O2A C5A N1A C13A -6.5(9) . . . . ? C4A C5A N1A C13A 171.8(6) . . . . ? O1A C1A N1A C5A 178.0(7) . . . . ? C2A C1A N1A C5A -0.3(10) . . . . ? O1A C1A N1A C13A 1.9(10) . . . . ? C2A C1A N1A C13A -176.4(6) . . . . ? C20A C13A N1A C5A -43.3(8) . . . . ? C14A C13A N1A C5A 88.6(8) . . . . ? C20A C13A N1A C1A 133.0(6) . . . . ? C14A C13A N1A C1A -95.1(8) . . . . ? O4A C20A O3A Cu1 3.3(12) . . . . ? C13A C20A O3A Cu1 -176.8(5) . . . . ? O3B Cu1 O3A C20A 75.6(6) . . . . ? O3D Cu1 O3A C20A -96.0(6) . . . . ? O3C Cu1 O3A C20A -11.4(12) . . . . ? O5 Cu1 O3A C20A 169.1(6) . . . . ? Cu2 Cu1 O3A C20A -7.1(6) . . . . ? O3A C20A O4A Cu2 5.2(10) . . . . ? C13A C20A O4A Cu2 -174.7(5) . . . . ? O4B Cu2 O4A C20A -93.5(5) . . . . ? O4D Cu2 O4A C20A 72.1(5) . . . . ? O6 Cu2 O4A C20A 160.1(5) . . . . ? Cu1 Cu2 O4A C20A -7.8(5) . . . . ? N1A C13A C14A C19A 153.2(9) . . . . ? C20A C13A C14A C19A -76.5(10) . . . . ? N1A C13A C14A C15A -32.8(10) . . . . ? C20A C13A C14A C15A 97.6(9) . . . . ? C19A C14A C15A C16A 0.4(13) . . . . ? C13A C14A C15A C16A -173.7(8) . . . . ? C14A C15A C16A C17A -0.5(15) . . . . ? C15A C16A C17A C18A 1.5(17) . . . . ? C16A C17A C18A C19A -2.3(19) . . . . ? C15A C14A C19A C18A -1.2(17) . . . . ? C13A C14A C19A C18A 173.1(11) . . . . ? C17A C18A C19A C14A 2(2) . . . . ? O1B C1B C2B C6B -6.0(11) . . . . ? N1B C1B C2B C6B 173.6(7) . . . . ? O1B C1B C2B C3B 175.5(7) . . . . ? N1B C1B C2B C3B -4.9(10) . . . . ? C6B C2B C3B C9B 1.7(12) . . . . ? C1B C2B C3B C9B -179.8(7) . . . . ? C6B C2B C3B C4B -175.6(8) . . . . ? C1B C2B C3B C4B 2.8(12) . . . . ? C2B C3B C4B C12B 179.9(8) . . . . ? C9B C3B C4B C12B 2.5(13) . . . . ? C2B C3B C4B C5B 2.9(12) . . . . ? C9B C3B C4B C5B -174.5(8) . . . . ? C12B C4B C5B O2B -5.5(13) . . . . ? C3B C4B C5B O2B 171.4(7) . . . . ? C12B C4B C5B N1B 176.7(8) . . . . ? C3B C4B C5B N1B -6.4(11) . . . . ? C3B C2B C6B C7B 1.2(12) . . . . ? C1B C2B C6B C7B -177.3(7) . . . . ? C2B C6B C7B C8B -2.2(13) . . . . ? C6B C7B C8B C9B 0.2(14) . . . . ? C2B C3B C9B C8B -3.6(12) . . . . ? C4B C3B C9B C8B 173.9(8) . . . . ? C2B C3B C9B C10B 178.8(8) . . . . ? C4B C3B C9B C10B -3.7(13) . . . . ? C7B C8B C9B C3B 2.7(13) . . . . ? C7B C8B C9B C10B -179.8(10) . . . . ? C3B C9B C10B C11B 1.5(15) . . . . ? C8B C9B C10B C11B -176.0(10) . . . . ? C9B C10B C11B C12B 2.1(17) . . . . ? C3B C4B C12B C11B 1.1(14) . . . . ? C5B C4B C12B C11B 178.0(9) . . . . ? C10B C11B C12B C4B -3.4(16) . . . . ? N1B C13B C14B C15B -99.8(9) . . . . ? C20B C13B C14B C15B 25.5(12) . . . . ? N1B C13B C14B C19B 82.5(10) . . . . ? C20B C13B C14B C19B -152.1(8) . . . . ? C19B C14B C15B C16B -4.6(15) . . . . ? C13B C14B C15B C16B 177.9(9) . . . . ? C14B C15B C16B C17B 1.0(16) . . . . ? C15B C16B C17B C18B 6.0(19) . . . . ? C16B C17B C18B C19B -9(2) . . . . ? C17B C18B C19B C14B 6(2) . . . . ? C15B C14B C19B C18B 1.3(17) . . . . ? C13B C14B C19B C18B 179.0(11) . . . . ? N1B C13B C20B O4B -24.5(9) . . . . ? C14B C13B C20B O4B -150.8(7) . . . . ? N1B C13B C20B O3B 158.6(6) . . . . ? C14B C13B C20B O3B 32.3(10) . . . . ? O2B C5B N1B C1B -173.5(7) . . . . ? C4B C5B N1B C1B 4.3(11) . . . . ? O2B C5B N1B C13B 4.7(10) . . . . ? C4B C5B N1B C13B -177.4(6) . . . . ? O1B C1B N1B C5B -179.1(7) . . . . ? C2B C1B N1B C5B 1.3(10) . . . . ? O1B C1B N1B C13B 2.7(10) . . . . ? C2B C1B N1B C13B -177.0(6) . . . . ? C20B C13B N1B C5B -64.5(8) . . . . ? C14B C13B N1B C5B 65.4(9) . . . . ? C20B C13B N1B C1B 113.9(7) . . . . ? C14B C13B N1B C1B -116.2(8) . . . . ? O4B C20B O3B Cu1 15.3(10) . . . . ? C13B C20B O3B Cu1 -168.2(5) . . . . ? O3A Cu1 O3B C20B -89.9(5) . . . . ? O3C Cu1 O3B C20B 74.5(5) . . . . ? O5 Cu1 O3B C20B 178.1(5) . . . . ? Cu2 Cu1 O3B C20B -10.6(5) . . . . ? O3B C20B O4B Cu2 -8.8(10) . . . . ? C13B C20B O4B Cu2 174.8(5) . . . . ? O4C Cu2 O4B C20B -83.6(5) . . . . ? O4A Cu2 O4B C20B 89.9(5) . . . . ? O4D Cu2 O4B C20B -6.4(11) . . . . ? O6 Cu2 O4B C20B -176.7(5) . . . . ? Cu1 Cu2 O4B C20B 0.1(5) . . . . ? O1C C1C C2C C6C -4.1(14) . . . . ? N1C C1C C2C C6C 175.5(8) . . . . ? O1C C1C C2C C3C 179.6(9) . . . . ? N1C C1C C2C C3C -0.8(12) . . . . ? C6C C2C C3C C4C -177.8(9) . . . . ? C1C C2C C3C C4C -1.6(13) . . . . ? C6C C2C C3C C9C 1.2(13) . . . . ? C1C C2C C3C C9C 177.4(8) . . . . ? C2C C3C C4C C12C -179.3(8) . . . . ? C9C C3C C4C C12C 1.6(13) . . . . ? C2C C3C C4C C5C 5.4(13) . . . . ? C9C C3C C4C C5C -173.7(7) . . . . ? C3C C4C C5C O2C 171.8(8) . . . . ? C12C C4C C5C O2C -3.8(12) . . . . ? C3C C4C C5C N1C -6.5(11) . . . . ? C12C C4C C5C N1C 178.0(7) . . . . ? C3C C2C C6C C7C 3.2(14) . . . . ? C1C C2C C6C C7C -173.1(9) . . . . ? C2C C6C C7C C8C -4.7(18) . . . . ? C6C C7C C8C C9C 2(2) . . . . ? C7C C8C C9C C10C -179.6(13) . . . . ? C7C C8C C9C C3C 2.4(18) . . . . ? C4C C3C C9C C10C -2.9(14) . . . . ? C2C C3C C9C C10C 178.1(9) . . . . ? C4C C3C C9C C8C 175.1(9) . . . . ? C2C C3C C9C C8C -3.9(13) . . . . ? C8C C9C C10C C11C -176.2(11) . . . . ? C3C C9C C10C C11C 1.7(16) . . . . ? C9C C10C C11C C12C 0.8(18) . . . . ? C3C C4C C12C C11C 0.7(14) . . . . ? C5C C4C C12C C11C 176.1(8) . . . . ? C10C C11C C12C C4C -2.0(16) . . . . ? N1C C13C C14C C19C 179.9(7) . . . . ? C20C C13C C14C C19C -54.4(10) . . . . ? N1C C13C C14C C15C 8.2(11) . . . . ? C20C C13C C14C C15C 133.9(8) . . . . ? C19C C14C C15C C16C 2.2(14) . . . . ? C13C C14C C15C C16C 174.2(9) . . . . ? C14C C15C C16C C17C -3.0(17) . . . . ? C15C C16C C17C C18C 2.8(16) . . . . ? C16C C17C C18C C19C -2.1(14) . . . . ? C15C C14C C19C C18C -1.4(13) . . . . ? C13C C14C C19C C18C -173.6(8) . . . . ? C17C C18C C19C C14C 1.4(14) . . . . ? N1C C13C C20C O3C 144.7(6) . . . . ? C14C C13C C20C O3C 15.2(10) . . . . ? N1C C13C C20C O4C -37.9(8) . . . . ? C14C C13C C20C O4C -167.3(6) . . . . ? O1C C1C N1C C5C 178.7(8) . . . . ? C2C C1C N1C C5C -0.9(12) . . . . ? O1C C1C N1C C13C 12.4(12) . . . . ? C2C C1C N1C C13C -167.2(7) . . . . ? O2C C5C N1C C1C -173.9(8) . . . . ? C4C C5C N1C C1C 4.3(11) . . . . ? O2C C5C N1C C13C -7.4(10) . . . . ? C4C C5C N1C C13C 170.9(6) . . . . ? C14C C13C N1C C1C -116.4(8) . . . . ? C20C C13C N1C C1C 112.4(7) . . . . ? C14C C13C N1C C5C 75.7(8) . . . . ? C20C C13C N1C C5C -55.5(8) . . . . ? O4C C20C O3C Cu1 3.3(9) . . . . ? C13C C20C O3C Cu1 -179.6(5) . . . . ? O3B Cu1 O3C C20C -88.3(5) . . . . ? O3D Cu1 O3C C20C 83.6(5) . . . . ? O3A Cu1 O3C C20C -0.8(11) . . . . ? O5 Cu1 O3C C20C 178.6(5) . . . . ? Cu2 Cu1 O3C C20C -5.1(5) . . . . ? O3C C20C O4C Cu2 2.5(10) . . . . ? C13C C20C O4C Cu2 -174.8(4) . . . . ? O4B Cu2 O4C C20C 81.0(5) . . . . ? O4D Cu2 O4C C20C -84.9(5) . . . . ? O6 Cu2 O4C C20C -172.7(5) . . . . ? Cu1 Cu2 O4C C20C -4.9(5) . . . . ? O1D C1D C2D C6D 0.2(15) . . . . ? N1D C1D C2D C6D 179.7(8) . . . . ? O1D C1D C2D C3D -179.4(9) . . . . ? N1D C1D C2D C3D 0.1(13) . . . . ? C6D C2D C3D C4D -179.2(9) . . . . ? C1D C2D C3D C4D 0.3(14) . . . . ? C6D C2D C3D C9D -2.2(13) . . . . ? C1D C2D C3D C9D 177.4(8) . . . . ? C2D C3D C4D C12D 177.8(9) . . . . ? C9D C3D C4D C12D 0.9(14) . . . . ? C2D C3D C4D C5D -3.0(13) . . . . ? C9D C3D C4D C5D -179.9(8) . . . . ? C12D C4D C5D O2D 4.4(14) . . . . ? C3D C4D C5D O2D -174.8(8) . . . . ? C12D C4D C5D N1D -175.6(8) . . . . ? C3D C4D C5D N1D 5.2(12) . . . . ? C3D C2D C6D C7D 0.7(15) . . . . ? C1D C2D C6D C7D -178.9(10) . . . . ? C2D C6D C7D C8D -1(2) . . . . ? C6D C7D C8D C9D 3(3) . . . . ? C7D C8D C9D C10D -179.1(15) . . . . ? C7D C8D C9D C3D -5(2) . . . . ? C4D C3D C9D C8D -178.6(11) . . . . ? C2D C3D C9D C8D 4.3(15) . . . . ? C4D C3D C9D C10D -3.5(14) . . . . ? C2D C3D C9D C10D 179.4(10) . . . . ? C8D C9D C10D C11D -178.9(15) . . . . ? C3D C9D C10D C11D 6(2) . . . . ? C9D C10D C11D C12D -6(2) . . . . ? C3D C4D C12D C11D -0.4(15) . . . . ? C5D C4D C12D C11D -179.6(9) . . . . ? C10D C11D C12D C4D 2.6(19) . . . . ? N1D C13D C14D C15D -77.7(8) . . . . ? C20D C13D C14D C15D 50.6(8) . . . . ? N1D C13D C14D C19D 99.6(7) . . . . ? C20D C13D C14D C19D -132.1(6) . . . . ? C19D C14D C15D C16D 0.0 . . . . ? C13D C14D C15D C16D 177.2(6) . . . . ? C14D C15D C16D C17D 0.0 . . . . ? C15D C16D C17D C18D 0.0 . . . . ? C16D C17D C18D C19D 0.0 . . . . ? C17D C18D C19D C14D 0.0 . . . . ? C15D C14D C19D C18D 0.0 . . . . ? C13D C14D C19D C18D -177.4(6) . . . . ? N1D C13D C20D O4D -31.5(9) . . . . ? C14D C13D C20D O4D -162.9(6) . . . . ? N1D C13D C20D O3D 151.9(6) . . . . ? C14D C13D C20D O3D 20.6(10) . . . . ? O2D C5D N1D C1D 174.8(8) . . . . ? C4D C5D N1D C1D -5.2(12) . . . . ? O2D C5D N1D C13D -11.3(12) . . . . ? C4D C5D N1D C13D 168.7(7) . . . . ? O1D C1D N1D C5D -178.0(8) . . . . ? C2D C1D N1D C5D 2.6(12) . . . . ? O1D C1D N1D C13D 8.0(11) . . . . ? C2D C1D N1D C13D -171.5(7) . . . . ? C14D C13D N1D C5D 83.3(9) . . . . ? C20D C13D N1D C5D -48.1(9) . . . . ? C14D C13D N1D C1D -102.2(8) . . . . ? C20D C13D N1D C1D 126.4(7) . . . . ? O4D C20D O3D Cu1 5.7(10) . . . . ? C13D C20D O3D Cu1 -178.3(5) . . . . ? O3A Cu1 O3D C20D 73.1(5) . . . . ? O3C Cu1 O3D C20D -91.3(5) . . . . ? O5 Cu1 O3D C20D 165.0(5) . . . . ? Cu2 Cu1 O3D C20D -6.4(5) . . . . ? O3D C20D O4D Cu2 0.3(11) . . . . ? C13D C20D O4D Cu2 -175.9(5) . . . . ? O4C Cu2 O4D C20D 79.6(6) . . . . ? O4A Cu2 O4D C20D -93.7(6) . . . . ? O4B Cu2 O4D C20D 2.6(12) . . . . ? O6 Cu2 O4D C20D 173.3(6) . . . . ? Cu1 Cu2 O4D C20D -4.1(5) . . . . ? O1E C1E C2E C3E 178.0(10) . . . . ? N1E C1E C2E C3E -2.8(14) . . . . ? O1E C1E C2E C6E -2.5(16) . . . . ? N1E C1E C2E C6E 176.7(9) . . . . ? C1E C2E C3E C9E -178.6(9) . . . . ? C6E C2E C3E C9E 1.9(15) . . . . ? C1E C2E C3E C4E 1.2(15) . . . . ? C6E C2E C3E C4E -178.2(9) . . . . ? C9E C3E C4E C12E 0.5(14) . . . . ? C2E C3E C4E C12E -179.3(9) . . . . ? C9E C3E C4E C5E -179.6(9) . . . . ? C2E C3E C4E C5E 0.6(13) . . . . ? C12E C4E C5E O2E -3.0(14) . . . . ? C3E C4E C5E O2E 177.2(8) . . . . ? C12E C4E C5E N1E 179.1(9) . . . . ? C3E C4E C5E N1E -0.7(12) . . . . ? C3E C2E C6E C7E -1.3(16) . . . . ? C1E C2E C6E C7E 179.2(11) . . . . ? C2E C6E C7E C8E -1(2) . . . . ? C6E C7E C8E C9E 3(3) . . . . ? C4E C3E C9E C10E -0.6(16) . . . . ? C2E C3E C9E C10E 179.2(11) . . . . ? C4E C3E C9E C8E -179.8(11) . . . . ? C2E C3E C9E C8E 0.0(16) . . . . ? C7E C8E C9E C3E -3(2) . . . . ? C7E C8E C9E C10E 178.3(16) . . . . ? C3E C9E C10E C11E 0.1(19) . . . . ? C8E C9E C10E C11E 179.3(12) . . . . ? C9E C10E C11E C12E 0.5(19) . . . . ? C3E C4E C12E C11E 0.2(15) . . . . ? C5E C4E C12E C11E -179.7(9) . . . . ? C10E C11E C12E C4E -0.7(17) . . . . ? N1E C13E C14E C15E -85.8(13) . . . . ? C20E C13E C14E C15E 37.8(15) . . . . ? N1E C13E C14E C19E 95.0(10) . . . . ? C20E C13E C14E C19E -141.4(9) . . . . ? C19E C14E C15E C16E 0.0 . . . . ? C13E C14E C15E C16E -179.1(14) . . . . ? C14E C15E C16E C17E 0.0 . . . . ? C15E C16E C17E C18E 0.0 . . . . ? C16E C17E C18E C19E 0.0 . . . . ? C17E C18E C19E C14E 0.0 . . . . ? C15E C14E C19E C18E 0.0 . . . . ? C13E C14E C19E C18E 179.3(12) . . . . ? C19K C14K C15K C16K 0.0 . . . . ? C14K C15K C16K C17K 0.0 . . . . ? C15K C16K C17K C18K 0.0 . . . . ? C16K C17K C18K C19K 0.0 . . . . ? C17K C18K C19K C14K 0.0 . . . . ? C15K C14K C19K C18K 0.0 . . . . ? N1E C13E C20E O3E 143.8(9) . . . . ? C14E C13E C20E O3E 22.8(13) . . . . ? N1E C13E C20E O4E -35.3(11) . . . . ? C14E C13E C20E O4E -156.3(9) . . . . ? O2E C5E N1E C1E -178.8(8) . . . . ? C4E C5E N1E C1E -0.9(13) . . . . ? O2E C5E N1E C13E -4.0(13) . . . . ? C4E C5E N1E C13E 173.8(8) . . . . ? O1E C1E N1E C5E -178.1(9) . . . . ? C2E C1E N1E C5E 2.7(14) . . . . ? O1E C1E N1E C13E 7.3(14) . . . . ? C2E C1E N1E C13E -172.0(9) . . . . ? C20E C13E N1E C5E -53.5(11) . . . . ? C14E C13E N1E C5E 70.9(11) . . . . ? C20E C13E N1E C1E 121.4(9) . . . . ? C14E C13E N1E C1E -114.2(10) . . . . ? O4E C20E O3E Cu3 -2.2(12) . . . . ? C13E C20E O3E Cu3 178.8(6) . . . . ? O3H Cu3 O3E C20E -77.7(8) . . . . ? O3F Cu3 O3E C20E 92.2(7) . . . . ? O3I Cu3 O3E C20E -68.4(8) . . . . ? O7 Cu3 O3E C20E -165.6(7) . . . . ? Cu4 Cu3 O3E C20E 3.8(6) . . . . ? O3E C20E O4E Cu4 -2.3(13) . . . . ? C13E C20E O4E Cu4 176.7(6) . . . . ? O4H Cu4 O4E C20E 90.3(8) . . . . ? O4F Cu4 O4E C20E -76.2(7) . . . . ? O4G Cu4 O4E C20E 15.8(14) . . . . ? O4I Cu4 O4E C20E 100.3(8) . . . . ? O8 Cu4 O4E C20E -163.5(7) . . . . ? Cu3 Cu4 O4E C20E 3.9(6) . . . . ? O1F C1F C2F C6F 6.2(14) . . . . ? N1F C1F C2F C6F -176.9(9) . . . . ? O1F C1F C2F C3F -175.5(9) . . . . ? N1F C1F C2F C3F 1.4(12) . . . . ? C6F C2F C3F C4F 177.4(9) . . . . ? C1F C2F C3F C4F -0.7(13) . . . . ? C6F C2F C3F C9F -4.3(14) . . . . ? C1F C2F C3F C9F 177.6(8) . . . . ? C2F C3F C4F C12F 177.2(8) . . . . ? C9F C3F C4F C12F -1.1(12) . . . . ? C2F C3F C4F C5F 0.3(12) . . . . ? C9F C3F C4F C5F -178.0(8) . . . . ? C12F C4F C5F O2F 0.5(13) . . . . ? C3F C4F C5F O2F 177.4(8) . . . . ? C12F C4F C5F N1F -177.6(8) . . . . ? C3F C4F C5F N1F -0.6(11) . . . . ? C3F C2F C6F C7F 3.3(16) . . . . ? C1F C2F C6F C7F -178.5(11) . . . . ? C2F C6F C7F C8F -1(2) . . . . ? C6F C7F C8F C9F -1(2) . . . . ? C7F C8F C9F C10F -177.6(13) . . . . ? C7F C8F C9F C3F 0.2(18) . . . . ? C4F C3F C9F C10F -1.3(13) . . . . ? C2F C3F C9F C10F -179.6(9) . . . . ? C4F C3F C9F C8F -179.2(9) . . . . ? C2F C3F C9F C8F 2.5(14) . . . . ? C8F C9F C10F C11F -178.7(11) . . . . ? C3F C9F C10F C11F 3.5(16) . . . . ? C9F C10F C11F C12F -3.3(16) . . . . ? C3F C4F C12F C11F 1.4(13) . . . . ? C5F C4F C12F C11F 178.3(8) . . . . ? C10F C11F C12F C4F 0.8(14) . . . . ? N1F C13F C14F C15F -71.9(10) . . . . ? C20F C13F C14F C15F 56.8(10) . . . . ? N1F C13F C14F C19F 106.0(8) . . . . ? C20F C13F C14F C19F -125.3(8) . . . . ? C19F C14F C15F C16F 0.0 . . . . ? C13F C14F C15F C16F 177.8(9) . . . . ? C14F C15F C16F C17F 0.0 . . . . ? C15F C16F C17F C18F 0.0 . . . . ? C16F C17F C18F C19F 0.0 . . . . ? C17F C18F C19F C14F 0.0 . . . . ? C15F C14F C19F C18F 0.0 . . . . ? C13F C14F C19F C18F -177.9(8) . . . . ? N1F C13F C20F O3F 149.6(7) . . . . ? C14F C13F C20F O3F 18.4(11) . . . . ? N1F C13F C20F O4F -35.3(9) . . . . ? C14F C13F C20F O4F -166.5(7) . . . . ? O2F C5F N1F C1F -176.7(8) . . . . ? C4F C5F N1F C1F 1.5(12) . . . . ? O2F C5F N1F C13F -10.3(12) . . . . ? C4F C5F N1F C13F 167.8(7) . . . . ? O1F C1F N1F C5F 175.3(9) . . . . ? C2F C1F N1F C5F -1.8(12) . . . . ? O1F C1F N1F C13F 8.8(12) . . . . ? C2F C1F N1F C13F -168.3(7) . . . . ? C20F C13F N1F C5F -49.7(10) . . . . ? C14F C13F N1F C5F 81.7(9) . . . . ? C20F C13F N1F C1F 118.0(8) . . . . ? C14F C13F N1F C1F -110.6(8) . . . . ? O4F C20F O3F Cu3 2.7(10) . . . . ? C13F C20F O3F Cu3 177.2(6) . . . . ? O3E Cu3 O3F C20F -87.8(6) . . . . ? O3G Cu3 O3F C20F 83.7(6) . . . . ? O3I Cu3 O3F C20F -11.5(16) . . . . ? O7 Cu3 O3F C20F 179.7(5) . . . . ? Cu4 Cu3 O3F C20F 0.2(5) . . . . ? O3F C20F O4F Cu4 -5.5(11) . . . . ? C13F C20F O4F Cu4 179.6(5) . . . . ? O4H Cu4 O4F C20F -12(2) . . . . ? O4E Cu4 O4F C20F 84.3(6) . . . . ? O4G Cu4 O4F C20F -81.1(6) . . . . ? O8 Cu4 O4F C20F 172.4(6) . . . . ? Cu3 Cu4 O4F C20F 4.1(6) . . . . ? O1G C1G C2G C3G -178.6(8) . . . . ? N1G C1G C2G C3G -0.5(11) . . . . ? O1G C1G C2G C6G -0.6(12) . . . . ? N1G C1G C2G C6G 177.5(7) . . . . ? C6G C2G C3G C4G -179.7(7) . . . . ? C1G C2G C3G C4G -1.7(11) . . . . ? C6G C2G C3G C9G -1.3(11) . . . . ? C1G C2G C3G C9G 176.7(7) . . . . ? C2G C3G C4G C12G -178.4(8) . . . . ? C9G C3G C4G C12G 3.2(12) . . . . ? C2G C3G C4G C5G 1.3(11) . . . . ? C9G C3G C4G C5G -177.2(7) . . . . ? C12G C4G C5G O2G -1.1(13) . . . . ? C3G C4G C5G O2G 179.2(8) . . . . ? C12G C4G C5G N1G -179.0(8) . . . . ? C3G C4G C5G N1G 1.3(11) . . . . ? C3G C2G C6G C7G 0.2(12) . . . . ? C1G C2G C6G C7G -177.9(7) . . . . ? C2G C6G C7G C8G 0.9(13) . . . . ? C6G C7G C8G C9G -1.0(14) . . . . ? C7G C8G C9G C10G 180.0(9) . . . . ? C7G C8G C9G C3G -0.1(12) . . . . ? C2G C3G C9G C10G -178.8(8) . . . . ? C4G C3G C9G C10G -0.4(11) . . . . ? C2G C3G C9G C8G 1.2(11) . . . . ? C4G C3G C9G C8G 179.6(7) . . . . ? C8G C9G C10G C11G 178.5(10) . . . . ? C3G C9G C10G C11G -1.4(14) . . . . ? C9G C10G C11G C12G 0.6(16) . . . . ? C3G C4G C12G C11G -4.1(14) . . . . ? C5G C4G C12G C11G 176.3(8) . . . . ? C10G C11G C12G C4G 2.2(16) . . . . ? N1G C13G C14G C15G -22.1(11) . . . . ? C20G C13G C14G C15G 117.4(8) . . . . ? N1G C13G C14G C19G 165.0(7) . . . . ? C20G C13G C14G C19G -55.6(11) . . . . ? C19G C14G C15G C16G 0.0 . . . . ? C13G C14G C15G C16G -173.2(10) . . . . ? C14G C15G C16G C17G 0.0 . . . . ? C15G C16G C17G C18G 0.0 . . . . ? C16G C17G C18G C19G 0.0 . . . . ? C17G C18G C19G C14G 0.0 . . . . ? C15G C14G C19G C18G 0.0 . . . . ? C13G C14G C19G C18G 172.8(10) . . . . ? C19J C14J C15J C16J 0.0 . . . . ? C14J C15J C16J C17J 0.0 . . . . ? C15J C16J C17J C18J 0.0 . . . . ? C16J C17J C18J C19J 0.0 . . . . ? C17J C18J C19J C14J 0.0 . . . . ? C15J C14J C19J C18J 0.0 . . . . ? N1G C13G C20G O3G 155.4(7) . . . . ? C14G C13G C20G O3G 13.8(11) . . . . ? N1G C13G C20G O4G -28.7(10) . . . . ? C14G C13G C20G O4G -170.2(7) . . . . ? O2G C5G N1G C1G 178.2(7) . . . . ? C4G C5G N1G C1G -3.8(11) . . . . ? O2G C5G N1G C13G -1.2(11) . . . . ? C4G C5G N1G C13G 176.7(7) . . . . ? O1G C1G N1G C5G -178.5(7) . . . . ? C2G C1G N1G C5G 3.4(10) . . . . ? O1G C1G N1G C13G 1.0(11) . . . . ? C2G C1G N1G C13G -177.2(6) . . . . ? C20G C13G N1G C5G -54.6(9) . . . . ? C14G C13G N1G C5G 87.4(9) . . . . ? C20G C13G N1G C1G 125.9(7) . . . . ? C14G C13G N1G C1G -92.2(9) . . . . ? O4G C20G O3G Cu3 5.8(12) . . . . ? C13G C20G O3G Cu3 -178.8(5) . . . . ? O3H Cu3 O3G C20G 80.2(8) . . . . ? O3F Cu3 O3G C20G -90.3(7) . . . . ? O3I Cu3 O3G C20G 69.8(8) . . . . ? O7 Cu3 O3G C20G 167.5(7) . . . . ? Cu4 Cu3 O3G C20G -1.9(6) . . . . ? O3G C20G O4G Cu4 -6.8(11) . . . . ? C13G C20G O4G Cu4 177.9(5) . . . . ? O4H Cu4 O4G C20G -83.3(7) . . . . ? O4F Cu4 O4G C20G 83.9(6) . . . . ? O4E Cu4 O4G C20G -8.1(12) . . . . ? O4I Cu4 O4G C20G -92.0(7) . . . . ? O8 Cu4 O4G C20G 171.2(5) . . . . ? Cu3 Cu4 O4G C20G 3.6(5) . . . . ? O1H C1H C2H C6H -1.1(8) . . . . ? N1H C1H C2H C6H 179.8(7) . . . . ? O1H C1H C2H C3H 178.7(6) . . . . ? N1H C1H C2H C3H -0.5(4) . . . . ? C6H C2H C3H C4H -179.7(7) . . . . ? C1H C2H C3H C4H 0.5(5) . . . . ? C6H C2H C3H C9H -0.6(7) . . . . ? C1H C2H C3H C9H 179.6(4) . . . . ? C2H C3H C4H C12H -179.9(7) . . . . ? C9H C3H C4H C12H 1.2(13) . . . . ? C2H C3H C4H C5H -0.7(11) . . . . ? C9H C3H C4H C5H -179.7(8) . . . . ? C12H C4H C5H O2H 0.3(17) . . . . ? C3H C4H C5H O2H -178.8(9) . . . . ? C12H C4H C5H N1H -180.0(10) . . . . ? C3H C4H C5H N1H 0.9(14) . . . . ? C3H C2H C6H C7H 0.6(12) . . . . ? C1H C2H C6H C7H -179.6(7) . . . . ? C2H C6H C7H C8H -0.4(16) . . . . ? C6H C7H C8H C9H 0.4(18) . . . . ? C7H C8H C9H C10H -178.7(11) . . . . ? C7H C8H C9H C3H -0.5(18) . . . . ? C4H C3H C9H C8H 179.6(10) . . . . ? C2H C3H C9H C8H 0.6(12) . . . . ? C4H C3H C9H C10H -1.9(12) . . . . ? C2H C3H C9H C10H 179.0(7) . . . . ? C8H C9H C10H C11H 179.2(11) . . . . ? C3H C9H C10H C11H 0.8(14) . . . . ? C9H C10H C11H C12H 1.0(17) . . . . ? C3H C4H C12H C11H 0.7(15) . . . . ? C5H C4H C12H C11H -178.4(9) . . . . ? C10H C11H C12H C4H -1.9(16) . . . . ? N1H C13H C14H C19H 118.8(15) . . . . ? C20H C13H C14H C19H -108.2(16) . . . . ? N1H C13H C14H C15H -70.0(19) . . . . ? C19H C14H C15H C16H -16(2) . . . . ? C13H C14H C15H C16H 172.8(11) . . . . ? C14H C15H C16H C17H 8.1(10) . . . . ? C15H C16H C17H C18H 0.0 . . . . ? C16H C17H C18H C19H 0.0 . . . . ? C15H C14H C19H C18H 17(2) . . . . ? C13H C14H C19H C18H -171.5(8) . . . . ? C17H C18H C19H C14H -8.6(10) . . . . ? C14H C13H C20H O4H -166.1(15) . . . . ? N1H C13H C20H O3H 155.6(15) . . . . ? C14H C13H C20H O3H 25(2) . . . . ? O2H C5H N1H C1H 178.8(9) . . . . ? C4H C5H N1H C1H -0.9(14) . . . . ? O2H C5H N1H C13H -1.8(16) . . . . ? C4H C5H N1H C13H 178.4(11) . . . . ? O1H C1H N1H C5H -178.5(9) . . . . ? C2H C1H N1H C5H 0.7(11) . . . . ? O1H C1H N1H C13H 2.1(11) . . . . ? C2H C1H N1H C13H -178.7(8) . . . . ? C14H C13H N1H C5H 84.3(13) . . . . ? C20H C13H N1H C5H -45.8(17) . . . . ? C14H C13H N1H C1H -96.3(13) . . . . ? C20H C13H N1H C1H 133.6(12) . . . . ? C13H C20H O3H Cu3 173.6(12) . . . . ? O3E Cu3 O3H C20H 86.2(16) . . . . ? O3G Cu3 O3H C20H -85.5(16) . . . . ? O7 Cu3 O3H C20H 178.4(17) . . . . ? Cu4 Cu3 O3H C20H -1.4(16) . . . . ? O3H C20H O4H Cu4 -8(3) . . . . ? C13H C20H O4H Cu4 -174.8(11) . . . . ? O4E Cu4 O4H C20H -75.9(15) . . . . ? O4G Cu4 O4H C20H 90.0(15) . . . . ? O8 Cu4 O4H C20H -164.2(14) . . . . ? Cu3 Cu4 O4H C20H 4.5(15) . . . . ? O1I C1I C2I C6I 0.4(8) . . . . ? N1I C1I C2I C6I -178.6(7) . . . . ? O1I C1I C2I C3I -179.1(6) . . . . ? N1I C1I C2I C3I 1.9(5) . . . . ? C6I C2I C3I C4I 179.1(7) . . . . ? C1I C2I C3I C4I -1.4(5) . . . . ? C6I C2I C3I C9I 0.7(7) . . . . ? C1I C2I C3I C9I -179.8(4) . . . . ? C2I C3I C4I C12I 177.4(8) . . . . ? C9I C3I C4I C12I -4.4(13) . . . . ? C2I C3I C4I C5I 2.6(10) . . . . ? C9I C3I C4I C5I -179.2(7) . . . . ? C12I C4I C5I O2I 1.9(16) . . . . ? C3I C4I C5I O2I 176.9(9) . . . . ? C12I C4I C5I N1I -179.5(10) . . . . ? C3I C4I C5I N1I -4.6(14) . . . . ? C3I C2I C6I C7I -0.5(11) . . . . ? C1I C2I C6I C7I -180.0(7) . . . . ? C2I C6I C7I C8I -0.6(16) . . . . ? C6I C7I C8I C9I 1.4(17) . . . . ? C7I C8I C9I C10I 178.6(11) . . . . ? C7I C8I C9I C3I -1.1(16) . . . . ? C4I C3I C9I C8I -178.4(9) . . . . ? C2I C3I C9I C8I 0.0(11) . . . . ? C4I C3I C9I C10I 1.9(11) . . . . ? C2I C3I C9I C10I -179.8(6) . . . . ? C8I C9I C10I C11I 179.8(11) . . . . ? C3I C9I C10I C11I -0.5(15) . . . . ? C9I C10I C11I C12I 1.2(17) . . . . ? C3I C4I C12I C11I 4.7(14) . . . . ? C5I C4I C12I C11I 179.4(9) . . . . ? C10I C11I C12I C4I -3.3(16) . . . . ? C13I C14I C15I C16I -175.4(13) . . . . ? C14I C15I C16I C17I -1.2(13) . . . . ? C15I C16I C17I C18I 0.0 . . . . ? C16I C17I C18I C19I 0.0 . . . . ? C13I C14I C19I C18I 175.5(11) . . . . ? C17I C18I C19I C14I 1.3(14) . . . . ? N1I C13I C20I O4I -160.3(17) . . . . ? C14I C13I C20I O3I -145.1(19) . . . . ? O2I C5I N1I C1I -176.1(9) . . . . ? C4I C5I N1I C1I 5.3(14) . . . . ? O2I C5I N1I C13I -8.9(17) . . . . ? C4I C5I N1I C13I 172.5(11) . . . . ? O1I C1I N1I C5I 177.0(9) . . . . ? C2I C1I N1I C5I -3.9(10) . . . . ? O1I C1I N1I C13I 9.1(12) . . . . ? C2I C1I N1I C13I -171.8(9) . . . . ? C14I C13I N1I C5I 62.0(19) . . . . ? C20I C13I N1I C5I -80.5(17) . . . . ? C14I C13I N1I C1I -130.1(14) . . . . ? C20I C13I N1I C1I 87.4(16) . . . . ? C13I C20I O3I Cu3 -154.4(15) . . . . ? C13I C20I O4I Cu4 151.7(13) . . . . ? O4E Cu4 O4I C20I -73.4(15) . . . . ? O4G Cu4 O4I C20I 92.1(15) . . . . ? O8 Cu4 O4I C20I -161.1(15) . . . . ? Cu3 Cu4 O4I C20I 6.7(16) . . . . ? O5 C21 C22 C23 -24.3(12) . . . . ? C21 C22 C23 C24 28.5(14) . . . . ? C22 C23 C24 O5 -22.5(13) . . . . ? C22 C21 O5 C24 10.7(11) . . . . ? C22 C21 O5 Cu1 -138.9(7) . . . . ? C23 C24 O5 C21 7.4(12) . . . . ? C23 C24 O5 Cu1 156.1(7) . . . . ? O3B Cu1 O5 C21 133.5(6) . . . . ? O3D Cu1 O5 C21 -46.9(6) . . . . ? O3A Cu1 O5 C21 42.1(6) . . . . ? O3C Cu1 O5 C21 -137.8(6) . . . . ? O3B Cu1 O5 C24 -12.2(7) . . . . ? O3D Cu1 O5 C24 167.4(7) . . . . ? O3A Cu1 O5 C24 -103.7(7) . . . . ? O3C Cu1 O5 C24 76.5(7) . . . . ? O6 C25 C26 C27 30.4(11) . . . . ? C25 C26 C27 C28 -34.9(12) . . . . ? C26 C27 C28 O6 26.4(11) . . . . ? C27 C28 O6 C25 -7.9(9) . . . . ? C27 C28 O6 Cu2 -145.0(6) . . . . ? C26 C25 O6 C28 -14.8(10) . . . . ? C26 C25 O6 Cu2 123.0(7) . . . . ? O4C Cu2 O6 C28 162.8(5) . . . . ? O4A Cu2 O6 C28 -16.9(6) . . . . ? O4B Cu2 O6 C28 -108.5(5) . . . . ? O4D Cu2 O6 C28 73.9(6) . . . . ? Cu1 Cu2 O6 C28 86.2(8) . . . . ? O4C Cu2 O6 C25 28.8(5) . . . . ? O4A Cu2 O6 C25 -150.9(5) . . . . ? O4B Cu2 O6 C25 117.5(5) . . . . ? O4D Cu2 O6 C25 -60.1(5) . . . . ? Cu1 Cu2 O6 C25 -47.8(9) . . . . ? C30 C29 O7 C32 38.5(19) . . . . ? C30 C29 O7 Cu3 168.9(13) . . . . ? C31 C32 O7 C29 -34.8(19) . . . . ? C31 C32 O7 Cu3 -167.4(13) . . . . ? O3H Cu3 O7 C29 -85.3(12) . . . . ? O3F Cu3 O7 C29 98.8(11) . . . . ? O3E Cu3 O7 C29 7.6(11) . . . . ? O3G Cu3 O7 C29 -170.3(11) . . . . ? O3I Cu3 O7 C29 -77.4(12) . . . . ? Cu4 Cu3 O7 C29 -84.2(14) . . . . ? O3H Cu3 O7 C32 38.8(12) . . . . ? O3F Cu3 O7 C32 -137.1(11) . . . . ? O3E Cu3 O7 C32 131.6(11) . . . . ? O3G Cu3 O7 C32 -46.3(11) . . . . ? O3I Cu3 O7 C32 46.7(12) . . . . ? Cu4 Cu3 O7 C32 39.9(17) . . . . ? O8 C33 C34 C35 -2.1(16) . . . . ? C33 C34 C35 C36 -6.3(19) . . . . ? C34 C35 C36 O8 12.6(18) . . . . ? C35 C36 O8 C33 -14.0(13) . . . . ? C35 C36 O8 Cu4 -162.9(9) . . . . ? C34 C33 O8 C36 10.2(12) . . . . ? C34 C33 O8 Cu4 158.8(8) . . . . ? O4H Cu4 O8 C36 -168.5(8) . . . . ? O4F Cu4 O8 C36 10.4(7) . . . . ? O4E Cu4 O8 C36 101.1(7) . . . . ? O4G Cu4 O8 C36 -78.7(7) . . . . ? O4I Cu4 O8 C36 -172.5(8) . . . . ? Cu3 Cu4 O8 C36 53.7(9) . . . . ? O4H Cu4 O8 C33 46.4(9) . . . . ? O4F Cu4 O8 C33 -134.7(7) . . . . ? O4E Cu4 O8 C33 -44.0(7) . . . . ? O4G Cu4 O8 C33 136.2(7) . . . . ? O4I Cu4 O8 C33 42.4(8) . . . . ? Cu3 Cu4 O8 C33 -91.4(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.59 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.869 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.089 _vrf_THETM01_4 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Weakly diffracting crystal due to extensive ligand and solvent disorder. No observable diffraction at high angle, therefore no data included above 2-theta ca 45 degrees. ; _vrf_PLAT023_4 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.59 Deg. RESPONSE: Weakly diffracting crystal due to extensive ligand and solvent disorder. No observable diffraction at high angle, therefore no data included above 2-theta ca 45 degrees. ; _vrf_PLAT220_4 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.95 Ratio RESPONSE: Some carbon atoms of napthalimide rings and coordinated THF groups display large displacement parameters as a result of positional disorder. This was modeled in three ligands, but could not be modeled in all cases and this is reflected in the Ueq values. ; #===END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C134 H97 Cu4 N17 O41, C4 H10 O, 2(C H4 O), 3(C H2 Cl2)' _chemical_formula_sum 'C143 H121 Cl6 Cu4 N17 O44' _chemical_formula_weight 3248.43 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.3235(5) _cell_length_b 21.9549(8) _cell_length_c 50.9472(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17140.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8473 _cell_measurement_theta_min 2.277 _cell_measurement_theta_max 23.950 _exptl_crystal_description bar _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6672 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8534 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS Version 2.05 (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 218466 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 25.07 _reflns_number_total 30385 _reflns_number_gt 26850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.043 0.569 0.117 829 200 ' ' 2 -0.052 0.069 0.383 829 200 ' ' 3 -0.001 0.431 0.617 829 200 ' ' 4 -0.060 0.842 0.680 166 51 ' ' 5 0.060 0.342 0.820 166 52 ' ' 6 0.002 0.931 0.883 829 200 ' ' 7 0.440 0.658 0.320 166 51 ' ' 8 0.560 0.158 0.180 166 51 ' ' Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+2.0459P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.044(6) _refine_ls_number_reflns 30385 _refine_ls_number_parameters 1932 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.95180(2) 0.430566(19) 0.304273(7) 0.02413(9) Uani 1 1 d . . . Cu2 Cu 0.92221(2) 0.410011(18) 0.356134(7) 0.02310(9) Uani 1 1 d . . . Cu3 Cu 0.54704(2) 0.541179(18) 0.462315(7) 0.02245(9) Uani 1 1 d . . . Cu4 Cu 0.56691(2) 0.516345(17) 0.411332(7) 0.02102(9) Uani 1 1 d . . . C1A C 0.6749(2) 0.42593(18) 0.27532(7) 0.0310(8) Uani 1 1 d . . . C2A C 0.6621(2) 0.43125(19) 0.24628(7) 0.0365(9) Uani 1 1 d . . . C3A C 0.6406(2) 0.48664(19) 0.23501(7) 0.0360(9) Uani 1 1 d . . . C4A C 0.6308(2) 0.53862(19) 0.25032(7) 0.0363(9) Uani 1 1 d . . . C5A C 0.6483(2) 0.53669(18) 0.27916(7) 0.0309(8) Uani 1 1 d . . . C6A C 0.6727(3) 0.3798(2) 0.23118(8) 0.0499(11) Uani 1 1 d . . . H6A H 0.6880 0.3421 0.2391 0.060 Uiso 1 1 calc R . . C7A C 0.6605(3) 0.3835(3) 0.20371(9) 0.0600(13) Uani 1 1 d . . . H7A H 0.6665 0.3481 0.1932 0.072 Uiso 1 1 calc R . . C8A C 0.6403(3) 0.4375(3) 0.19243(9) 0.0663(15) Uani 1 1 d . . . H8A H 0.6340 0.4393 0.1739 0.080 Uiso 1 1 calc R . . C9A C 0.6283(3) 0.4911(2) 0.20723(8) 0.0476(11) Uani 1 1 d . . . C10A C 0.6036(3) 0.5474(3) 0.19658(9) 0.0604(14) Uani 1 1 d . . . H10A H 0.5947 0.5508 0.1782 0.072 Uiso 1 1 calc R . . C11A C 0.5921(3) 0.5970(3) 0.21189(9) 0.0544(12) Uani 1 1 d . . . H11A H 0.5752 0.6346 0.2042 0.065 Uiso 1 1 calc R . . C12A C 0.6051(3) 0.5929(2) 0.23911(8) 0.0475(11) Uani 1 1 d . . . H12A H 0.5962 0.6277 0.2499 0.057 Uiso 1 1 calc R . . C13A C 0.6891(2) 0.47650(17) 0.31792(6) 0.0276(8) Uani 1 1 d . . . H13A H 0.6815 0.5185 0.3252 0.033 Uiso 1 1 calc R . . C14A C 0.6281(2) 0.43446(18) 0.33371(7) 0.0320(8) Uani 1 1 d . . . H14A H 0.5677 0.4397 0.3272 0.038 Uiso 1 1 calc R . . H14B H 0.6452 0.3916 0.3305 0.038 Uiso 1 1 calc R . . C15A C 0.6290(2) 0.44620(16) 0.36313(7) 0.0274(8) Uani 1 1 d . . . C16A C 0.7850(2) 0.45989(15) 0.32151(6) 0.0217(7) Uani 1 1 d . . . N1A N 0.66648(18) 0.47957(14) 0.28991(5) 0.0279(6) Uani 1 1 d . . . N2A N 0.65597(19) 0.40124(14) 0.37772(6) 0.0335(7) Uani 1 1 d . . . H2A1 H 0.6553 0.4047 0.3949 0.040 Uiso 1 1 calc R . . H2A2 H 0.6748 0.3674 0.3704 0.040 Uiso 1 1 calc R . . O1A O 0.69383(16) 0.37856(12) 0.28579(5) 0.0351(6) Uani 1 1 d . . . O2A O 0.6473(2) 0.58165(13) 0.29252(6) 0.0497(7) Uani 1 1 d . . . O3A O 0.60132(15) 0.49544(11) 0.37159(4) 0.0291(5) Uani 1 1 d . . . O4A O 0.83459(14) 0.46395(11) 0.30181(4) 0.0266(5) Uani 1 1 d . . . O5A O 0.80598(14) 0.44417(11) 0.34419(4) 0.0283(5) Uani 1 1 d . . . C1B C 0.9827(2) 0.21602(17) 0.30711(7) 0.0320(8) Uani 1 1 d . . . C2B C 1.0401(2) 0.18392(18) 0.28843(7) 0.0355(9) Uani 1 1 d . . . C3B C 1.0016(2) 0.15058(17) 0.26777(8) 0.0357(9) Uani 1 1 d . . . C4B C 0.9116(2) 0.14939(18) 0.26412(8) 0.0375(9) Uani 1 1 d . . . C5B C 0.8534(2) 0.18343(17) 0.28169(7) 0.0350(9) Uani 1 1 d . . . C6B C 1.1281(3) 0.1867(2) 0.29133(9) 0.0475(11) Uani 1 1 d . . . H6B H 1.1530 0.2095 0.3053 0.057 Uiso 1 1 calc R . . C7B C 1.1830(3) 0.1551(2) 0.27326(10) 0.0583(13) Uani 1 1 d . . . H7B H 1.2446 0.1574 0.2751 0.070 Uiso 1 1 calc R . . C8B C 1.1483(3) 0.1223(2) 0.25362(9) 0.0520(11) Uani 1 1 d . . . H8B H 1.1860 0.1011 0.2420 0.062 Uiso 1 1 calc R . . C9B C 1.0562(3) 0.11837(18) 0.24982(8) 0.0418(9) Uani 1 1 d . . . C10B C 1.0180(3) 0.08594(19) 0.22916(8) 0.0465(11) Uani 1 1 d . . . H10B H 1.0540 0.0644 0.2171 0.056 Uiso 1 1 calc R . . C11B C 0.9296(3) 0.08495(18) 0.22611(8) 0.0458(10) Uani 1 1 d . . . H11B H 0.9046 0.0626 0.2120 0.055 Uiso 1 1 calc R . . C12B C 0.8753(3) 0.11655(19) 0.24352(8) 0.0423(10) Uani 1 1 d . . . H12B H 0.8138 0.1155 0.2413 0.051 Uiso 1 1 calc R . . C13B C 0.8378(2) 0.25250(16) 0.31943(7) 0.0283(8) Uani 1 1 d . . . H13B H 0.7812 0.2592 0.3101 0.034 Uiso 1 1 calc R . . C14B C 0.8174(2) 0.21764(17) 0.34478(7) 0.0334(8) Uani 1 1 d . . . H14C H 0.7982 0.1758 0.3403 0.040 Uiso 1 1 calc R . . H14D H 0.8710 0.2145 0.3555 0.040 Uiso 1 1 calc R . . C15B C 0.7466(2) 0.24920(17) 0.36056(7) 0.0294(8) Uani 1 1 d . . . C16B C 0.8779(2) 0.31466(16) 0.32425(7) 0.0264(8) Uani 1 1 d . . . N1B N 0.89416(17) 0.21661(13) 0.30176(6) 0.0276(6) Uani 1 1 d . . . N2B N 0.7532(2) 0.24587(17) 0.38619(6) 0.0467(9) Uani 1 1 d . . . H2B1 H 0.7136 0.2632 0.3962 0.056 Uiso 1 1 calc R . . H2B2 H 0.7972 0.2263 0.3934 0.056 Uiso 1 1 calc R . . O1B O 1.01071(16) 0.24219(13) 0.32657(5) 0.0392(6) Uani 1 1 d . . . O2B O 0.77459(17) 0.18405(15) 0.27945(6) 0.0529(8) Uani 1 1 d . . . O3B O 0.68620(16) 0.27612(13) 0.34960(5) 0.0390(6) Uani 1 1 d . . . O4B O 0.90171(14) 0.34485(11) 0.30478(4) 0.0265(5) Uani 1 1 d . . . O5B O 0.87930(15) 0.33130(11) 0.34790(5) 0.0295(5) Uani 1 1 d . . . C1C C 1.2463(2) 0.45109(18) 0.30930(7) 0.0320(8) Uani 1 1 d . . . C2C C 1.2998(2) 0.47199(18) 0.28653(7) 0.0353(9) Uani 1 1 d . . . C3C C 1.3428(2) 0.42835(19) 0.27064(7) 0.0358(9) Uani 1 1 d . . . C4C C 1.3357(2) 0.36628(18) 0.27587(7) 0.0316(8) Uani 1 1 d . . . C5C C 1.2817(2) 0.34407(18) 0.29794(7) 0.0293(8) Uani 1 1 d . . . C6C C 1.3080(3) 0.5329(2) 0.28128(9) 0.0482(11) Uani 1 1 d . . . H6C H 1.2793 0.5619 0.2921 0.058 Uiso 1 1 calc R . . C7C C 1.3584(3) 0.5527(2) 0.26008(10) 0.0596(13) Uani 1 1 d . . . H7C H 1.3635 0.5950 0.2565 0.072 Uiso 1 1 calc R . . C8C C 1.3999(3) 0.5116(3) 0.24464(10) 0.0615(13) Uani 1 1 d . . . H8C H 1.4339 0.5260 0.2303 0.074 Uiso 1 1 calc R . . C9C C 1.3945(3) 0.4484(2) 0.24902(8) 0.0474(11) Uani 1 1 d . . . C10C C 1.4355(3) 0.4049(2) 0.23340(8) 0.0526(11) Uani 1 1 d . . . H10C H 1.4686 0.4176 0.2186 0.063 Uiso 1 1 calc R . . C11C C 1.4291(3) 0.3449(2) 0.23892(8) 0.0525(12) Uani 1 1 d . . . H11C H 1.4584 0.3161 0.2282 0.063 Uiso 1 1 calc R . . C12C C 1.3788(2) 0.3243(2) 0.26068(8) 0.0417(10) Uani 1 1 d . . . H12C H 1.3752 0.2820 0.2646 0.050 Uiso 1 1 calc R . . C13C C 1.1891(2) 0.36884(17) 0.33595(7) 0.0280(8) Uani 1 1 d . . . H13C H 1.1926 0.3234 0.3363 0.034 Uiso 1 1 calc R . . C14C C 1.2224(2) 0.39177(19) 0.36286(7) 0.0354(9) Uani 1 1 d . . . H14E H 1.2070 0.4353 0.3649 0.042 Uiso 1 1 calc R . . H14F H 1.1926 0.3688 0.3770 0.042 Uiso 1 1 calc R . . C15C C 1.3189(2) 0.38451(18) 0.36583(7) 0.0340(9) Uani 1 1 d . . . C16C C 1.0927(2) 0.38550(15) 0.33214(7) 0.0262(8) Uani 1 1 d . . . N1C N 1.24230(17) 0.38939(13) 0.31390(6) 0.0273(6) Uani 1 1 d . . . N2C N 1.3603(2) 0.43111(15) 0.37691(6) 0.0396(8) Uani 1 1 d . . . H2C1 H 1.4171 0.4294 0.3794 0.048 Uiso 1 1 calc R . . H2C2 H 1.3310 0.4637 0.3817 0.048 Uiso 1 1 calc R . . O1C O 1.20527(16) 0.48639(12) 0.32291(5) 0.0360(6) Uani 1 1 d . . . O2C O 1.27017(16) 0.29081(12) 0.30231(5) 0.0376(6) Uani 1 1 d . . . O3C O 1.35587(17) 0.33788(13) 0.35869(6) 0.0474(7) Uani 1 1 d . . . O4C O 1.06765(14) 0.39809(10) 0.30931(4) 0.0280(5) Uani 1 1 d . . . O5C O 1.04689(15) 0.38410(11) 0.35255(4) 0.0291(5) Uani 1 1 d . . . C1D C 0.8913(3) 0.63825(19) 0.33156(9) 0.0446(10) Uani 1 1 d . . . C2D C 0.8590(3) 0.6858(2) 0.31390(10) 0.0560(13) Uani 1 1 d . . . C3D C 0.9175(3) 0.72198(19) 0.29947(11) 0.0604(13) Uani 1 1 d . . . C4D C 1.0083(3) 0.71808(19) 0.30404(10) 0.0563(12) Uani 1 1 d . . . C5D C 1.0418(3) 0.67518(18) 0.32440(9) 0.0479(10) Uani 1 1 d . . . C6D C 0.7696(4) 0.6913(2) 0.31018(13) 0.0753(17) Uani 1 1 d . . . H6D H 0.7297 0.6669 0.3198 0.090 Uiso 1 1 calc R . . C7D C 0.7398(5) 0.7346(3) 0.29144(16) 0.100(2) Uani 1 1 d . . . H7D H 0.6789 0.7402 0.2890 0.120 Uiso 1 1 calc R . . C8D C 0.7968(5) 0.7682(3) 0.27702(16) 0.104(3) Uani 1 1 d . . . H8D H 0.7746 0.7960 0.2644 0.124 Uiso 1 1 calc R . . C9D C 0.8865(4) 0.7629(2) 0.28017(13) 0.0800(18) Uani 1 1 d . . . C10D C 0.9484(6) 0.7948(3) 0.26432(14) 0.100(2) Uani 1 1 d . . . H10D H 0.9283 0.8200 0.2504 0.119 Uiso 1 1 calc R . . C11D C 1.0338(5) 0.7897(2) 0.26863(13) 0.088(2) Uani 1 1 d . . . H11D H 1.0738 0.8116 0.2580 0.106 Uiso 1 1 calc R . . C12D C 1.0652(4) 0.7517(2) 0.28916(10) 0.0706(15) Uani 1 1 d . . . H12D H 1.1261 0.7495 0.2926 0.085 Uiso 1 1 calc R . . C13D C 1.0143(2) 0.58955(17) 0.35387(7) 0.0363(9) Uani 1 1 d . . . H13D H 1.0795 0.5905 0.3531 0.044 Uiso 1 1 calc R . . C14D C 0.9881(3) 0.60203(18) 0.38244(8) 0.0397(9) Uani 1 1 d . . . H14G H 0.9236 0.6029 0.3837 0.048 Uiso 1 1 calc R . . H14H H 1.0092 0.5681 0.3936 0.048 Uiso 1 1 calc R . . C15D C 1.0239(3) 0.6613(2) 0.39303(9) 0.0418(10) Uani 1 1 d . . . C16D C 0.9856(2) 0.52570(15) 0.34473(7) 0.0249(7) Uani 1 1 d . . . N1D N 0.9824(2) 0.63581(14) 0.33551(6) 0.0380(8) Uani 1 1 d . . . N2D N 1.0875(2) 0.65645(19) 0.41041(7) 0.0554(10) Uani 1 1 d . . . H2D1 H 1.1111 0.6894 0.4172 0.067 Uiso 1 1 calc R . . H2D2 H 1.1063 0.6202 0.4152 0.067 Uiso 1 1 calc R . . O1D O 0.84510(18) 0.60194(14) 0.34238(6) 0.0503(8) Uani 1 1 d . . . O2D O 1.1182(2) 0.67301(14) 0.33025(7) 0.0589(9) Uani 1 1 d . . . O3D O 0.9949(2) 0.71016(14) 0.38559(7) 0.0583(8) Uani 1 1 d . . . O4D O 0.99010(15) 0.51213(11) 0.32131(5) 0.0292(5) Uani 1 1 d . . . O5D O 0.96236(15) 0.49126(10) 0.36344(4) 0.0275(5) Uani 1 1 d . . . C1E C 0.7189(2) 0.37737(17) 0.48802(7) 0.0291(8) Uani 1 1 d . . . C2E C 0.7201(3) 0.34537(18) 0.51348(7) 0.0368(9) Uani 1 1 d . . . C3E C 0.7878(3) 0.35737(17) 0.53182(7) 0.0336(9) Uani 1 1 d . . . C4E C 0.8535(3) 0.40027(18) 0.52599(7) 0.0371(9) Uani 1 1 d . . . C5E C 0.8540(2) 0.43268(18) 0.50058(7) 0.0319(8) Uani 1 1 d . . . C6E C 0.6565(3) 0.3038(2) 0.51953(8) 0.0455(10) Uani 1 1 d . . . H6E H 0.6112 0.2960 0.5072 0.055 Uiso 1 1 calc R . . C7E C 0.6571(3) 0.2728(2) 0.54336(10) 0.0595(13) Uani 1 1 d . . . H7E H 0.6124 0.2442 0.5473 0.071 Uiso 1 1 calc R . . C8E C 0.7225(4) 0.2837(2) 0.56097(9) 0.0646(14) Uani 1 1 d . . . H8E H 0.7229 0.2619 0.5771 0.078 Uiso 1 1 calc R . . C9E C 0.7891(3) 0.3261(2) 0.55608(8) 0.0484(11) Uani 1 1 d . . . C10E C 0.8571(4) 0.3390(2) 0.57370(9) 0.0593(14) Uani 1 1 d . . . H10E H 0.8589 0.3186 0.5901 0.071 Uiso 1 1 calc R . . C11E C 0.9205(3) 0.3803(2) 0.56774(8) 0.0556(12) Uani 1 1 d . . . H11E H 0.9660 0.3878 0.5800 0.067 Uiso 1 1 calc R . . C12E C 0.9196(3) 0.4116(2) 0.54403(8) 0.0500(11) Uani 1 1 d . . . H12E H 0.9639 0.4405 0.5402 0.060 Uiso 1 1 calc R . . C13E C 0.7856(2) 0.44950(16) 0.45753(6) 0.0249(7) Uani 1 1 d . . . H13E H 0.8291 0.4834 0.4582 0.030 Uiso 1 1 calc R . . C14E C 0.8164(2) 0.40433(16) 0.43624(6) 0.0249(7) Uani 1 1 d . . . H14I H 0.8621 0.3782 0.4441 0.030 Uiso 1 1 calc R . . H14J H 0.7665 0.3775 0.4319 0.030 Uiso 1 1 calc R . . C15E C 0.8518(2) 0.42966(16) 0.41089(7) 0.0261(7) Uani 1 1 d . . . C16E C 0.6963(2) 0.47784(15) 0.45202(6) 0.0234(7) Uani 1 1 d . . . N1E N 0.78577(17) 0.41938(13) 0.48349(5) 0.0267(6) Uani 1 1 d . . . N2E N 0.8430(2) 0.48693(15) 0.40526(6) 0.0414(8) Uani 1 1 d . . . H2E1 H 0.8644 0.5014 0.3905 0.050 Uiso 1 1 calc R . . H2E2 H 0.8156 0.5113 0.4162 0.050 Uiso 1 1 calc R . . O1E O 0.66454(15) 0.36820(12) 0.47117(5) 0.0318(6) Uani 1 1 d . . . O2E O 0.90954(17) 0.47002(13) 0.49460(5) 0.0409(6) Uani 1 1 d . . . O3E O 0.88990(16) 0.39308(11) 0.39614(4) 0.0298(5) Uani 1 1 d . . . O4E O 0.65715(14) 0.50139(10) 0.47090(4) 0.0255(5) Uani 1 1 d . . . O5E O 0.67227(13) 0.47754(10) 0.42834(4) 0.0238(5) Uani 1 1 d . . . C1F C 0.3221(2) 0.38035(16) 0.45953(7) 0.0284(8) Uani 1 1 d . . . C2F C 0.2506(2) 0.37061(18) 0.47898(7) 0.0352(9) Uani 1 1 d . . . C3F C 0.2633(3) 0.33015(17) 0.50010(7) 0.0350(9) Uani 1 1 d . . . C4F C 0.3419(2) 0.29935(16) 0.50371(7) 0.0316(8) Uani 1 1 d . . . C5F C 0.4136(2) 0.30628(16) 0.48440(7) 0.0302(8) Uani 1 1 d . . . C6F C 0.1732(3) 0.4000(2) 0.47564(9) 0.0526(12) Uani 1 1 d . . . H6F H 0.1664 0.4280 0.4616 0.063 Uiso 1 1 calc R . . C7F C 0.1039(3) 0.3893(3) 0.49271(10) 0.0631(14) Uani 1 1 d . . . H7F H 0.0500 0.4099 0.4902 0.076 Uiso 1 1 calc R . . C8F C 0.1131(3) 0.3491(3) 0.51303(10) 0.0636(14) Uani 1 1 d . . . H8F H 0.0644 0.3408 0.5240 0.076 Uiso 1 1 calc R . . C9F C 0.1927(3) 0.31988(19) 0.51800(8) 0.0460(11) Uani 1 1 d . . . C10F C 0.2063(4) 0.2805(2) 0.53923(9) 0.0556(13) Uani 1 1 d . . . H10F H 0.1598 0.2725 0.5511 0.067 Uiso 1 1 calc R . . C11F C 0.2854(4) 0.25349(19) 0.54314(8) 0.0517(12) Uani 1 1 d . . . H11F H 0.2944 0.2286 0.5581 0.062 Uiso 1 1 calc R . . C12F C 0.3528(3) 0.26225(18) 0.52527(7) 0.0450(10) Uani 1 1 d . . . H12F H 0.4072 0.2424 0.5280 0.054 Uiso 1 1 calc R . . C13F C 0.4705(2) 0.35657(15) 0.44531(6) 0.0248(7) Uani 1 1 d . . . H13F H 0.5243 0.3397 0.4537 0.030 Uiso 1 1 calc R . . C14F C 0.4528(2) 0.31692(15) 0.42126(7) 0.0283(7) Uani 1 1 d . . . H14K H 0.4262 0.2782 0.4272 0.034 Uiso 1 1 calc R . . H14L H 0.4098 0.3379 0.4100 0.034 Uiso 1 1 calc R . . C15F C 0.5329(2) 0.30247(15) 0.40502(6) 0.0250(7) Uani 1 1 d . . . C16F C 0.48990(19) 0.42318(16) 0.43957(6) 0.0243(7) Uani 1 1 d . . . N1F N 0.40083(17) 0.34961(12) 0.46452(5) 0.0244(6) Uani 1 1 d . . . N2F N 0.51918(19) 0.29283(15) 0.37946(6) 0.0357(7) Uani 1 1 d . . . H2F1 H 0.5627 0.2816 0.3693 0.043 Uiso 1 1 calc R . . H2F2 H 0.4666 0.2977 0.3728 0.043 Uiso 1 1 calc R . . O1F O 0.31550(15) 0.41134(12) 0.44045(5) 0.0351(6) Uani 1 1 d . . . O2F O 0.47940(17) 0.27589(13) 0.48522(5) 0.0425(7) Uani 1 1 d . . . O3F O 0.60526(15) 0.29639(12) 0.41546(5) 0.0331(6) Uani 1 1 d . . . O4F O 0.49051(14) 0.45867(10) 0.45894(4) 0.0251(5) Uani 1 1 d . . . O5F O 0.50995(13) 0.43694(10) 0.41620(4) 0.0232(5) Uani 1 1 d . . . C1G C 0.4282(2) 0.72529(16) 0.42806(7) 0.0293(8) Uani 1 1 d . . . C2G C 0.4327(2) 0.78791(16) 0.43885(7) 0.0306(8) Uani 1 1 d . . . C3G C 0.3607(2) 0.81138(16) 0.45373(7) 0.0314(8) Uani 1 1 d . . . C4G C 0.2861(2) 0.77560(17) 0.45769(7) 0.0314(8) Uani 1 1 d . . . C5G C 0.2807(2) 0.71312(17) 0.44725(7) 0.0304(8) Uani 1 1 d . . . C6G C 0.5051(3) 0.82292(17) 0.43500(8) 0.0369(9) Uani 1 1 d . . . H6G H 0.5526 0.8074 0.4251 0.044 Uiso 1 1 calc R . . C7G C 0.5099(3) 0.88193(19) 0.44565(8) 0.0435(10) Uani 1 1 d . . . H7G H 0.5604 0.9061 0.4428 0.052 Uiso 1 1 calc R . . C8G C 0.4419(3) 0.90472(18) 0.46010(8) 0.0469(10) Uani 1 1 d . . . H8G H 0.4462 0.9445 0.4673 0.056 Uiso 1 1 calc R . . C9G C 0.3661(3) 0.87029(18) 0.46438(7) 0.0372(9) Uani 1 1 d . . . C10G C 0.2933(3) 0.89246(19) 0.47925(8) 0.0438(10) Uani 1 1 d . . . H10G H 0.2953 0.9321 0.4867 0.053 Uiso 1 1 calc R . . C11G C 0.2216(3) 0.8573(2) 0.48269(8) 0.0469(11) Uani 1 1 d . . . H11G H 0.1736 0.8728 0.4924 0.056 Uiso 1 1 calc R . . C12G C 0.2171(3) 0.79823(19) 0.47208(7) 0.0400(9) Uani 1 1 d . . . H12G H 0.1665 0.7740 0.4748 0.048 Uiso 1 1 calc R . . C13G C 0.3441(2) 0.63117(15) 0.42038(7) 0.0270(8) Uani 1 1 d . . . H13G H 0.2921 0.6110 0.4284 0.032 Uiso 1 1 calc R . . C14G C 0.3235(2) 0.63969(16) 0.39149(7) 0.0305(8) Uani 1 1 d . . . H14M H 0.3776 0.6512 0.3821 0.037 Uiso 1 1 calc R . . H14N H 0.2813 0.6735 0.3895 0.037 Uiso 1 1 calc R . . C15G C 0.2859(2) 0.58260(19) 0.37907(8) 0.0373(9) Uani 1 1 d . . . C16G C 0.4234(2) 0.58946(15) 0.42598(6) 0.0245(7) Uani 1 1 d . . . N1G N 0.35320(17) 0.69120(13) 0.43331(5) 0.0254(6) Uani 1 1 d . . . N2G N 0.2854(3) 0.58239(19) 0.35354(8) 0.0688(12) Uani 1 1 d . . . H2G1 H 0.2632 0.5512 0.3450 0.083 Uiso 1 1 calc R . . H2G2 H 0.3071 0.6135 0.3448 0.083 Uiso 1 1 calc R . . O1G O 0.48664(15) 0.70314(11) 0.41488(5) 0.0323(6) Uani 1 1 d . . . O2G O 0.21694(16) 0.68063(13) 0.45028(5) 0.0413(7) Uani 1 1 d . . . O3G O 0.25653(18) 0.54069(13) 0.39172(6) 0.0479(7) Uani 1 1 d . . . O4G O 0.44502(14) 0.58566(10) 0.44973(4) 0.0262(5) Uani 1 1 d . . . O5G O 0.45422(14) 0.56064(10) 0.40720(4) 0.0263(5) Uani 1 1 d . . . C1H C 0.8236(2) 0.64067(17) 0.44603(7) 0.0313(8) Uani 1 1 d . . . C2H C 0.9042(2) 0.64626(17) 0.46169(7) 0.0315(8) Uani 1 1 d . . . C3H C 0.9201(2) 0.70072(17) 0.47606(7) 0.0334(8) Uani 1 1 d . . . C4H C 0.8577(3) 0.74733(18) 0.47623(7) 0.0368(9) Uani 1 1 d . . . C5H C 0.7757(2) 0.74240(17) 0.46146(8) 0.0361(9) Uani 1 1 d . . . C6H C 0.9648(2) 0.60036(18) 0.46177(8) 0.0387(9) Uani 1 1 d . . . H6H H 0.9539 0.5642 0.4521 0.046 Uiso 1 1 calc R . . C7H C 1.0421(3) 0.6063(2) 0.47591(8) 0.0479(11) Uani 1 1 d . . . H7H H 1.0835 0.5741 0.4757 0.057 Uiso 1 1 calc R . . C8H C 1.0592(3) 0.6577(2) 0.49001(8) 0.0458(10) Uani 1 1 d . . . H8H H 1.1121 0.6608 0.4996 0.055 Uiso 1 1 calc R . . C9H C 0.9986(2) 0.7066(2) 0.49048(8) 0.0430(10) Uani 1 1 d . . . C10H C 1.0126(3) 0.7605(2) 0.50482(8) 0.0516(12) Uani 1 1 d . . . H10H H 1.0648 0.7652 0.5147 0.062 Uiso 1 1 calc R . . C11H C 0.9516(3) 0.8063(2) 0.50473(8) 0.0511(12) Uani 1 1 d . . . H11H H 0.9622 0.8425 0.5144 0.061 Uiso 1 1 calc R . . C12H C 0.8744(3) 0.80015(19) 0.49057(8) 0.0468(11) Uani 1 1 d . . . H12H H 0.8328 0.8322 0.4907 0.056 Uiso 1 1 calc R . . C13H C 0.6916(2) 0.68530(17) 0.42763(8) 0.0344(9) Uani 1 1 d . . . H13H H 0.6507 0.7190 0.4324 0.041 Uiso 1 1 calc R . . C14H C 0.7191(3) 0.69601(18) 0.39890(8) 0.0393(9) Uani 1 1 d . . . H14O H 0.7675 0.6681 0.3942 0.047 Uiso 1 1 calc R . . H14P H 0.6694 0.6874 0.3871 0.047 Uiso 1 1 calc R . . C15H C 0.7483(3) 0.76137(19) 0.39548(9) 0.0426(10) Uani 1 1 d . . . C16H C 0.6416(2) 0.62573(16) 0.43154(7) 0.0286(8) Uani 1 1 d . . . N1H N 0.76612(18) 0.68946(13) 0.44575(6) 0.0299(7) Uani 1 1 d . . . N2H N 0.8305(2) 0.77179(17) 0.39152(8) 0.0555(10) Uani 1 1 d . . . H2H1 H 0.8491 0.8094 0.3893 0.067 Uiso 1 1 calc R . . H2H2 H 0.8677 0.7413 0.3910 0.067 Uiso 1 1 calc R . . O1H O 0.80692(16) 0.59541(12) 0.43324(5) 0.0369(6) Uani 1 1 d . . . O2H O 0.71797(19) 0.78042(13) 0.46161(6) 0.0516(8) Uani 1 1 d . . . O3H O 0.6921(2) 0.80224(15) 0.39644(7) 0.0628(9) Uani 1 1 d . . . O4H O 0.61741(15) 0.61430(11) 0.45457(5) 0.0288(5) Uani 1 1 d . . . O5H O 0.62569(14) 0.59482(11) 0.41131(5) 0.0298(5) Uani 1 1 d . . . C21 C 0.9030(3) 0.4441(2) 0.24698(8) 0.0494(11) Uani 1 1 d . . . H21 H 0.8466 0.4385 0.2543 0.059 Uiso 1 1 calc R . . C22 C 0.9093(4) 0.4554(3) 0.22075(9) 0.0822(18) Uani 1 1 d . . . H22 H 0.8584 0.4568 0.2101 0.099 Uiso 1 1 calc R . . C23 C 0.9901(5) 0.4647(3) 0.21001(10) 0.088(2) Uani 1 1 d . . . H23 H 0.9960 0.4742 0.1919 0.105 Uiso 1 1 calc R . . C24 C 1.0627(4) 0.4601(2) 0.22582(10) 0.0708(15) Uani 1 1 d . . . H24 H 1.1197 0.4654 0.2188 0.085 Uiso 1 1 calc R . . C25 C 1.0501(3) 0.4475(2) 0.25225(8) 0.0494(11) Uani 1 1 d . . . H25 H 1.0999 0.4436 0.2632 0.059 Uiso 1 1 calc R . . N3 N 0.97149(19) 0.44049(14) 0.26285(6) 0.0334(7) Uani 1 1 d . . . C26 C 0.5423(4) 0.4978(3) 0.52014(9) 0.0818(18) Uani 1 1 d . . . H26A H 0.5247 0.4585 0.5127 0.123 Uiso 1 1 calc R . . H26B H 0.5165 0.5026 0.5376 0.123 Uiso 1 1 calc R . . H26C H 0.6061 0.4993 0.5215 0.123 Uiso 1 1 calc R . . O6 O 0.51288(17) 0.54578(13) 0.50346(5) 0.0396(6) Uani 1 1 d . . . H6M H 0.4603 0.5490 0.5073 0.059 Uiso 1 1 d R . . C27 C 0.2808(4) 0.5417(3) 0.48900(15) 0.097(2) Uani 1 1 d . . . H27A H 0.2263 0.5230 0.4951 0.146 Uiso 1 1 calc R . . H27B H 0.3074 0.5159 0.4755 0.146 Uiso 1 1 calc R . . H27C H 0.2683 0.5820 0.4816 0.146 Uiso 1 1 calc R . . O7 O 0.3402(2) 0.5479(2) 0.51086(9) 0.0945(14) Uani 1 1 d . . . H7M H 0.3545 0.5125 0.5161 0.142 Uiso 1 1 d R . . C28 C 0.0851(3) 0.4635(3) 0.41887(10) 0.0715(15) Uani 1 1 d . . . H28A H 0.1247 0.4291 0.4216 0.107 Uiso 1 1 calc R . . H28B H 0.0716 0.4672 0.4001 0.107 Uiso 1 1 calc R . . H28C H 0.0310 0.4567 0.4287 0.107 Uiso 1 1 calc R . . O8 O 0.1250(2) 0.51723(18) 0.42766(7) 0.0673(10) Uani 1 1 d . . . H8M H 0.1648 0.5347 0.4192 0.101 Uiso 1 1 d R . . C1S C 0.5909(3) 0.2491(2) 0.29492(8) 0.0462(10) Uani 1 1 d . . . H1S1 H 0.6258 0.2194 0.3051 0.055 Uiso 1 1 calc R . . H1S2 H 0.6275 0.2856 0.2919 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.56251(9) 0.21702(7) 0.26451(2) 0.0711(4) Uani 1 1 d . . . Cl2 Cl 0.49866(8) 0.26975(8) 0.31309(2) 0.0735(4) Uani 1 1 d . . . C2S C 0.6328(5) 0.6988(3) 0.63179(12) 0.092(2) Uani 1 1 d . . . H2S1 H 0.5698 0.6940 0.6281 0.110 Uiso 1 1 calc R . . H2S2 H 0.6417 0.7395 0.6397 0.110 Uiso 1 1 calc R . . Cl3 Cl 0.66600(13) 0.64213(10) 0.65432(4) 0.1076(6) Uani 1 1 d . . . Cl4 Cl 0.69184(11) 0.69412(7) 0.60221(3) 0.0841(4) Uani 1 1 d . . . C3S C 1.0164(5) 0.6806(5) 0.63519(13) 0.128(3) Uani 1 1 d . . . H3S1 H 1.0397 0.7204 0.6293 0.154 Uiso 1 1 calc R . . H3S2 H 1.0349 0.6495 0.6223 0.154 Uiso 1 1 calc R . . Cl5 Cl 0.90366(11) 0.68420(9) 0.63546(3) 0.0956(5) Uani 1 1 d . . . Cl6 Cl 1.06099(16) 0.66294(12) 0.66557(3) 0.1308(8) Uani 1 1 d . . . C29 C 0.4714(7) 0.6332(5) 0.56904(14) 0.162(5) Uani 1 1 d D . . H29D H 0.4116 0.6460 0.5651 0.243 Uiso 1 1 calc R . . H29E H 0.4970 0.6136 0.5536 0.243 Uiso 1 1 calc R . . H29F H 0.5064 0.6689 0.5738 0.243 Uiso 1 1 calc R . . C30 C 0.4704(6) 0.5881(3) 0.59202(16) 0.131(3) Uani 1 1 d D . . H30C H 0.4332 0.5526 0.5877 0.158 Uiso 1 1 calc R . . H30D H 0.5303 0.5733 0.5956 0.158 Uiso 1 1 calc R . . C31 C 0.4300(6) 0.5842(4) 0.63762(17) 0.137(3) Uani 1 1 d D . . H31C H 0.4882 0.5689 0.6429 0.164 Uiso 1 1 calc R . . H31D H 0.3910 0.5489 0.6348 0.164 Uiso 1 1 calc R . . C32 C 0.3915(7) 0.6273(5) 0.65972(17) 0.158(4) Uani 1 1 d D . . H32D H 0.4343 0.6589 0.6641 0.237 Uiso 1 1 calc R . . H32E H 0.3784 0.6032 0.6754 0.237 Uiso 1 1 calc R . . H32F H 0.3378 0.6466 0.6533 0.237 Uiso 1 1 calc R . . O10 O 0.4368(3) 0.61893(17) 0.61426(8) 0.0892(12) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01950(18) 0.0333(2) 0.01960(19) -0.00006(17) 0.00129(16) 0.00182(17) Cu2 0.02074(19) 0.0288(2) 0.0197(2) -0.00313(17) 0.00179(16) 0.00013(16) Cu3 0.02001(19) 0.0270(2) 0.02030(19) -0.00259(16) 0.00132(16) 0.00079(16) Cu4 0.01848(19) 0.0245(2) 0.02006(19) -0.00060(16) 0.00163(15) -0.00091(16) C1A 0.0238(17) 0.043(2) 0.0267(19) -0.0021(18) -0.0033(14) -0.0016(16) C2A 0.0308(19) 0.058(3) 0.0206(18) -0.0123(18) 0.0039(15) -0.0054(18) C3A 0.0281(18) 0.055(3) 0.0248(18) 0.0073(18) -0.0053(15) -0.0087(18) C4A 0.0235(18) 0.051(2) 0.034(2) 0.0124(19) 0.0029(15) -0.0053(17) C5A 0.0216(17) 0.042(2) 0.0288(19) 0.0031(18) 0.0003(14) -0.0005(16) C6A 0.049(3) 0.065(3) 0.035(2) -0.007(2) -0.0012(19) 0.002(2) C7A 0.072(3) 0.079(4) 0.030(2) -0.015(2) 0.003(2) -0.018(3) C8A 0.064(3) 0.108(5) 0.027(2) -0.004(3) 0.000(2) -0.015(3) C9A 0.041(2) 0.076(3) 0.027(2) 0.001(2) -0.0024(17) -0.017(2) C10A 0.053(3) 0.094(4) 0.034(2) 0.024(3) -0.009(2) -0.015(3) C11A 0.046(3) 0.075(3) 0.043(3) 0.025(3) -0.009(2) -0.007(2) C12A 0.038(2) 0.063(3) 0.042(2) 0.015(2) 0.0009(18) -0.008(2) C13A 0.0239(17) 0.035(2) 0.0234(17) -0.0029(15) -0.0016(14) 0.0032(15) C14A 0.0254(17) 0.046(2) 0.0248(18) -0.0058(16) 0.0006(14) -0.0007(16) C15A 0.0208(16) 0.035(2) 0.0265(19) -0.0013(16) 0.0044(14) -0.0051(15) C16A 0.0277(16) 0.0211(16) 0.0163(16) -0.0051(13) 0.0002(13) 0.0035(14) N1A 0.0277(15) 0.0374(17) 0.0186(14) -0.0041(13) -0.0012(11) 0.0052(13) N2A 0.0371(17) 0.0389(18) 0.0245(15) -0.0019(14) 0.0067(13) 0.0058(15) O1A 0.0362(14) 0.0385(16) 0.0305(14) -0.0080(12) -0.0001(11) 0.0012(12) O2A 0.069(2) 0.0347(16) 0.0451(17) 0.0004(14) -0.0026(15) 0.0011(15) O3A 0.0359(13) 0.0305(14) 0.0210(12) -0.0002(10) 0.0045(10) 0.0031(11) O4A 0.0239(11) 0.0350(13) 0.0210(12) -0.0017(10) 0.0010(10) 0.0035(10) O5A 0.0206(11) 0.0403(15) 0.0239(13) -0.0014(11) -0.0001(9) 0.0041(10) C1B 0.0314(18) 0.033(2) 0.032(2) -0.0111(17) 0.0024(16) -0.0003(15) C2B 0.0306(19) 0.039(2) 0.036(2) -0.0102(17) 0.0059(16) 0.0055(17) C3B 0.035(2) 0.032(2) 0.040(2) -0.0068(17) 0.0083(17) 0.0009(17) C4B 0.038(2) 0.035(2) 0.040(2) -0.0133(17) 0.0103(17) -0.0004(17) C5B 0.034(2) 0.035(2) 0.036(2) -0.0135(17) 0.0026(17) -0.0008(17) C6B 0.036(2) 0.055(3) 0.051(3) -0.020(2) 0.0036(19) 0.008(2) C7B 0.031(2) 0.076(3) 0.068(3) -0.019(3) 0.011(2) 0.012(2) C8B 0.041(2) 0.057(3) 0.058(3) -0.020(2) 0.014(2) 0.011(2) C9B 0.047(2) 0.040(2) 0.038(2) -0.0091(18) 0.0143(19) 0.0008(19) C10B 0.059(3) 0.041(2) 0.039(2) -0.0137(19) 0.018(2) -0.001(2) C11B 0.055(3) 0.041(2) 0.042(2) -0.0181(19) 0.007(2) -0.006(2) C12B 0.044(2) 0.049(2) 0.034(2) -0.0110(19) 0.0037(18) -0.0013(19) C13B 0.0253(17) 0.0323(19) 0.0273(18) -0.0096(15) 0.0035(14) 0.0020(15) C14B 0.0310(18) 0.031(2) 0.038(2) -0.0077(17) 0.0058(16) 0.0036(16) C15B 0.0232(17) 0.034(2) 0.031(2) -0.0047(16) 0.0030(15) -0.0044(15) C16B 0.0185(16) 0.034(2) 0.0263(19) -0.0023(16) 0.0017(14) 0.0070(14) N1B 0.0228(14) 0.0294(16) 0.0305(16) -0.0109(13) 0.0043(12) 0.0013(12) N2B 0.0364(18) 0.071(3) 0.0330(19) -0.0044(17) 0.0031(15) 0.0248(18) O1B 0.0303(13) 0.0494(17) 0.0378(15) -0.0131(13) -0.0054(12) 0.0084(12) O2B 0.0259(14) 0.077(2) 0.0556(19) -0.0390(17) -0.0016(13) -0.0024(14) O3B 0.0292(13) 0.0566(17) 0.0312(14) -0.0037(13) 0.0038(11) 0.0096(13) O4B 0.0258(12) 0.0305(13) 0.0233(12) -0.0041(11) 0.0016(10) 0.0010(10) O5B 0.0279(12) 0.0340(14) 0.0265(13) -0.0055(11) 0.0022(10) -0.0023(11) C1C 0.0216(17) 0.041(2) 0.033(2) -0.0061(18) -0.0099(15) -0.0056(16) C2C 0.0288(18) 0.040(2) 0.037(2) 0.0019(18) -0.0080(16) -0.0077(16) C3C 0.0225(17) 0.053(2) 0.032(2) -0.0004(18) -0.0009(15) -0.0023(17) C4C 0.0211(17) 0.050(2) 0.0241(18) -0.0040(17) 0.0004(14) -0.0025(16) C5C 0.0195(16) 0.044(2) 0.0243(18) -0.0105(16) -0.0036(14) 0.0045(16) C6C 0.040(2) 0.051(3) 0.053(3) 0.002(2) -0.002(2) -0.009(2) C7C 0.056(3) 0.054(3) 0.069(3) 0.013(3) -0.002(3) -0.014(2) C8C 0.056(3) 0.080(4) 0.049(3) 0.013(3) 0.010(2) -0.018(3) C9C 0.032(2) 0.069(3) 0.042(2) 0.003(2) 0.0013(18) -0.009(2) C10C 0.042(2) 0.076(3) 0.040(2) 0.000(2) 0.009(2) -0.008(2) C11C 0.042(2) 0.085(4) 0.031(2) -0.014(2) 0.0083(19) 0.005(2) C12C 0.0285(19) 0.057(3) 0.040(2) -0.009(2) 0.0033(17) 0.0018(18) C13C 0.0269(18) 0.032(2) 0.0248(18) -0.0022(15) 0.0017(14) 0.0020(15) C14C 0.0293(19) 0.046(2) 0.031(2) -0.0028(17) 0.0002(16) 0.0040(17) C15C 0.0312(19) 0.038(2) 0.033(2) -0.0003(17) -0.0065(16) 0.0074(18) C16C 0.0240(17) 0.0241(18) 0.030(2) -0.0065(15) 0.0006(15) 0.0007(14) N1C 0.0188(14) 0.0367(17) 0.0265(16) -0.0023(13) -0.0002(11) 0.0008(12) N2C 0.0341(17) 0.0441(19) 0.0407(18) -0.0054(16) -0.0064(14) 0.0044(16) O1C 0.0354(14) 0.0338(14) 0.0388(15) -0.0113(12) -0.0017(12) 0.0029(12) O2C 0.0330(14) 0.0380(16) 0.0417(15) -0.0048(13) 0.0085(12) 0.0012(12) O3C 0.0339(14) 0.0540(18) 0.0543(18) -0.0218(15) -0.0166(13) 0.0178(14) O4C 0.0189(11) 0.0377(14) 0.0273(13) -0.0025(10) -0.0023(10) 0.0057(10) O5C 0.0216(11) 0.0390(13) 0.0268(13) -0.0012(10) 0.0031(10) 0.0040(11) C1D 0.038(2) 0.033(2) 0.062(3) -0.009(2) -0.010(2) 0.0021(19) C2D 0.061(3) 0.035(2) 0.071(3) -0.001(2) -0.026(3) 0.011(2) C3D 0.072(3) 0.028(2) 0.081(3) 0.006(2) -0.024(3) -0.001(2) C4D 0.078(3) 0.023(2) 0.068(3) 0.004(2) -0.012(3) -0.011(2) C5D 0.050(3) 0.033(2) 0.061(3) 0.002(2) -0.003(2) -0.007(2) C6D 0.066(3) 0.049(3) 0.111(5) 0.002(3) -0.032(3) 0.017(3) C7D 0.090(5) 0.067(4) 0.144(7) 0.003(4) -0.054(5) 0.023(4) C8D 0.108(5) 0.058(4) 0.145(7) 0.025(4) -0.062(5) 0.018(4) C9D 0.097(4) 0.031(3) 0.112(5) 0.013(3) -0.036(4) 0.000(3) C10D 0.137(6) 0.048(3) 0.114(5) 0.033(3) -0.045(5) -0.008(4) C11D 0.133(6) 0.036(3) 0.096(5) 0.020(3) -0.026(4) -0.021(3) C12D 0.097(4) 0.042(3) 0.073(3) 0.012(2) -0.011(3) -0.021(3) C13D 0.0315(18) 0.036(2) 0.041(2) 0.0050(18) -0.0015(16) -0.0007(16) C14D 0.042(2) 0.038(2) 0.039(2) -0.0054(18) -0.0029(18) -0.0080(18) C15D 0.032(2) 0.040(2) 0.053(3) -0.013(2) 0.0045(19) -0.0029(18) C16D 0.0198(15) 0.0273(19) 0.0275(19) -0.0018(15) -0.0038(14) 0.0001(13) N1D 0.0401(18) 0.0302(17) 0.0437(19) 0.0068(15) -0.0099(15) -0.0021(14) N2D 0.043(2) 0.065(2) 0.058(2) -0.019(2) -0.0100(19) -0.0073(19) O1D 0.0341(15) 0.0440(18) 0.073(2) -0.0017(16) -0.0045(15) -0.0014(14) O2D 0.0469(19) 0.053(2) 0.076(2) 0.0196(17) -0.0051(16) -0.0168(15) O3D 0.0512(18) 0.0368(18) 0.087(2) -0.0120(17) -0.0002(17) -0.0027(15) O4D 0.0291(12) 0.0297(13) 0.0288(14) -0.0002(11) -0.0017(10) -0.0040(11) O5D 0.0317(12) 0.0271(12) 0.0236(12) -0.0010(10) 0.0027(10) -0.0021(11) C1E 0.0281(18) 0.035(2) 0.0239(18) -0.0027(15) 0.0064(15) 0.0114(16) C2E 0.041(2) 0.044(2) 0.0248(19) 0.0009(17) 0.0016(16) 0.0167(19) C3E 0.047(2) 0.035(2) 0.0192(18) -0.0047(15) -0.0021(16) 0.0139(18) C4E 0.044(2) 0.040(2) 0.0272(19) -0.0089(17) -0.0095(17) 0.0197(19) C5E 0.0273(18) 0.041(2) 0.0277(19) -0.0123(17) -0.0042(15) 0.0099(18) C6E 0.046(2) 0.049(3) 0.041(2) 0.007(2) 0.0046(19) 0.006(2) C7E 0.073(3) 0.054(3) 0.051(3) 0.019(2) 0.008(3) 0.000(3) C8E 0.090(4) 0.069(3) 0.035(2) 0.018(2) 0.004(3) 0.023(3) C9E 0.068(3) 0.050(3) 0.028(2) 0.0000(19) 0.002(2) 0.020(2) C10E 0.088(4) 0.058(3) 0.032(2) 0.001(2) -0.021(2) 0.035(3) C11E 0.071(3) 0.059(3) 0.036(2) -0.005(2) -0.027(2) 0.008(3) C12E 0.054(3) 0.057(3) 0.039(2) -0.009(2) -0.021(2) 0.017(2) C13E 0.0201(15) 0.038(2) 0.0170(16) -0.0015(14) 0.0013(13) 0.0009(14) C14E 0.0260(16) 0.0322(19) 0.0166(16) -0.0029(14) 0.0003(13) 0.0069(15) C15E 0.0240(16) 0.0310(19) 0.0232(17) -0.0046(16) -0.0014(14) 0.0014(15) C16E 0.0211(16) 0.0243(17) 0.0247(18) -0.0019(14) -0.0006(14) -0.0032(14) N1E 0.0252(14) 0.0377(17) 0.0171(14) -0.0018(12) -0.0015(11) 0.0056(13) N2E 0.056(2) 0.0348(19) 0.0332(18) -0.0025(15) 0.0209(15) 0.0039(16) O1E 0.0273(13) 0.0420(15) 0.0259(13) 0.0027(11) -0.0016(11) 0.0019(11) O2E 0.0341(14) 0.0496(17) 0.0390(15) -0.0024(13) -0.0146(12) -0.0002(13) O3E 0.0371(13) 0.0307(13) 0.0216(12) -0.0053(10) 0.0073(10) 0.0019(11) O4E 0.0211(11) 0.0328(13) 0.0226(12) -0.0024(10) 0.0005(9) 0.0067(10) O5E 0.0203(11) 0.0316(13) 0.0195(12) 0.0022(10) -0.0024(9) 0.0020(10) C1F 0.0238(17) 0.0328(19) 0.029(2) 0.0028(17) 0.0046(15) -0.0009(15) C2F 0.0279(19) 0.047(2) 0.031(2) 0.0037(18) 0.0050(15) -0.0026(17) C3F 0.044(2) 0.031(2) 0.030(2) 0.0014(16) 0.0095(17) -0.0118(17) C4F 0.045(2) 0.0255(19) 0.0237(18) 0.0003(15) 0.0047(16) -0.0043(17) C5F 0.038(2) 0.0269(19) 0.0254(18) 0.0003(15) -0.0027(15) -0.0022(16) C6F 0.032(2) 0.076(3) 0.049(3) 0.008(2) 0.0073(19) 0.008(2) C7F 0.031(2) 0.096(4) 0.063(3) 0.000(3) 0.016(2) 0.004(2) C8F 0.043(3) 0.087(4) 0.060(3) -0.002(3) 0.027(2) -0.016(3) C9F 0.058(3) 0.043(2) 0.037(2) 0.0010(19) 0.023(2) -0.015(2) C10F 0.084(3) 0.045(3) 0.037(2) 0.001(2) 0.034(2) -0.016(3) C11F 0.092(4) 0.035(2) 0.028(2) 0.0087(18) 0.016(2) -0.012(2) C12F 0.077(3) 0.030(2) 0.029(2) 0.0067(17) 0.003(2) -0.006(2) C13F 0.0201(16) 0.0307(19) 0.0234(17) 0.0038(14) 0.0052(13) 0.0022(14) C14F 0.0258(17) 0.0242(17) 0.0350(19) -0.0027(15) 0.0003(15) -0.0019(15) C15F 0.0275(18) 0.0208(17) 0.0266(18) -0.0009(14) 0.0002(14) 0.0006(14) C16F 0.0153(14) 0.037(2) 0.0201(17) 0.0021(15) 0.0006(13) -0.0005(14) N1F 0.0241(14) 0.0235(14) 0.0257(15) 0.0048(12) 0.0002(12) 0.0002(11) N2F 0.0237(15) 0.056(2) 0.0270(16) -0.0085(15) -0.0001(12) 0.0077(14) O1F 0.0256(12) 0.0494(16) 0.0303(14) 0.0137(13) 0.0023(10) 0.0055(12) O2F 0.0417(15) 0.0443(16) 0.0415(16) 0.0131(13) -0.0005(12) 0.0112(13) O3F 0.0265(13) 0.0412(15) 0.0315(14) -0.0002(11) 0.0010(11) 0.0136(11) O4F 0.0247(11) 0.0297(12) 0.0209(12) -0.0016(10) 0.0046(9) -0.0045(10) O5F 0.0213(11) 0.0271(12) 0.0211(12) -0.0001(10) 0.0014(9) -0.0030(9) C1G 0.0275(18) 0.0342(19) 0.0260(18) 0.0030(15) -0.0040(15) 0.0010(16) C2G 0.0300(19) 0.032(2) 0.0295(18) -0.0021(15) -0.0041(15) 0.0015(16) C3G 0.0366(19) 0.031(2) 0.0267(19) -0.0016(15) -0.0066(15) 0.0067(16) C4G 0.0287(18) 0.0324(19) 0.033(2) -0.0071(16) -0.0024(15) 0.0070(15) C5G 0.0246(18) 0.040(2) 0.0261(19) -0.0005(16) -0.0001(14) 0.0067(16) C6G 0.038(2) 0.036(2) 0.037(2) -0.0018(17) -0.0029(17) -0.0006(17) C7G 0.046(2) 0.037(2) 0.048(2) -0.0056(19) 0.000(2) -0.0102(19) C8G 0.056(3) 0.029(2) 0.056(3) -0.0112(19) -0.011(2) -0.001(2) C9G 0.044(2) 0.037(2) 0.030(2) -0.0065(17) -0.0029(17) 0.0054(17) C10G 0.054(3) 0.039(2) 0.038(2) -0.0118(18) -0.0056(19) 0.015(2) C11G 0.045(2) 0.052(3) 0.044(2) -0.008(2) 0.005(2) 0.017(2) C12G 0.037(2) 0.048(2) 0.035(2) -0.0055(19) 0.0003(17) 0.0064(18) C13G 0.0219(17) 0.0274(19) 0.0318(19) -0.0031(15) 0.0005(14) -0.0016(14) C14G 0.0273(18) 0.032(2) 0.032(2) -0.0046(16) -0.0060(15) 0.0063(15) C15G 0.033(2) 0.039(2) 0.040(2) -0.0112(19) -0.0105(17) 0.0092(18) C16G 0.0221(16) 0.0247(17) 0.0269(18) 0.0000(14) 0.0031(14) -0.0054(14) N1G 0.0232(14) 0.0266(15) 0.0265(15) -0.0032(12) 0.0018(12) 0.0021(12) N2G 0.111(4) 0.050(2) 0.045(2) -0.012(2) -0.017(2) -0.014(2) O1G 0.0268(12) 0.0325(14) 0.0378(14) -0.0043(11) 0.0086(11) 0.0006(11) O2G 0.0264(13) 0.0478(17) 0.0497(16) -0.0153(13) 0.0074(12) -0.0056(12) O3G 0.0455(16) 0.0388(16) 0.0595(19) -0.0088(15) -0.0022(14) -0.0087(14) O4G 0.0274(12) 0.0281(12) 0.0232(12) -0.0047(10) -0.0008(10) 0.0052(10) O5G 0.0208(11) 0.0318(13) 0.0262(12) -0.0018(10) 0.0018(10) 0.0042(10) C1H 0.0246(17) 0.032(2) 0.037(2) -0.0067(17) 0.0057(15) -0.0014(15) C2H 0.0216(17) 0.041(2) 0.0322(19) -0.0042(17) 0.0063(15) -0.0093(15) C3H 0.0305(18) 0.042(2) 0.0279(18) -0.0056(16) 0.0096(15) -0.0095(17) C4H 0.040(2) 0.036(2) 0.035(2) -0.0047(17) 0.0060(17) -0.0123(18) C5H 0.037(2) 0.033(2) 0.039(2) -0.0101(18) 0.0144(17) -0.0096(17) C6H 0.0320(19) 0.043(2) 0.041(2) -0.0052(18) 0.0013(17) 0.0001(17) C7H 0.0275(19) 0.069(3) 0.047(2) 0.001(2) -0.0039(18) -0.002(2) C8H 0.028(2) 0.073(3) 0.036(2) -0.003(2) -0.0044(17) -0.010(2) C9H 0.031(2) 0.062(3) 0.036(2) -0.012(2) 0.0053(17) -0.021(2) C10H 0.049(2) 0.070(3) 0.036(2) -0.014(2) 0.0088(19) -0.032(2) C11H 0.063(3) 0.054(3) 0.036(2) -0.016(2) 0.010(2) -0.032(3) C12H 0.058(3) 0.040(2) 0.042(2) -0.0102(19) 0.015(2) -0.013(2) C13H 0.0230(17) 0.030(2) 0.051(2) -0.0049(18) 0.0007(16) -0.0043(15) C14H 0.035(2) 0.036(2) 0.047(2) 0.0080(18) -0.0062(18) -0.0090(17) C15H 0.035(2) 0.039(2) 0.054(3) 0.007(2) 0.0005(19) -0.0029(19) C16H 0.0232(17) 0.0268(19) 0.036(2) 0.0007(16) 0.0012(15) 0.0033(14) N1H 0.0246(14) 0.0258(16) 0.0391(18) -0.0055(13) 0.0051(13) -0.0062(12) N2H 0.042(2) 0.041(2) 0.083(3) 0.005(2) 0.0116(19) -0.0117(17) O1H 0.0323(13) 0.0309(14) 0.0475(16) -0.0162(13) -0.0076(12) 0.0024(11) O2H 0.0448(16) 0.0352(15) 0.075(2) -0.0196(15) 0.0040(16) 0.0062(14) O3H 0.0482(18) 0.0445(18) 0.096(3) 0.0153(18) 0.0124(17) 0.0006(16) O4H 0.0262(12) 0.0292(13) 0.0311(14) -0.0024(11) -0.0005(10) -0.0024(10) O5H 0.0263(12) 0.0310(13) 0.0321(13) 0.0023(12) -0.0006(10) -0.0059(10) C21 0.045(2) 0.069(3) 0.034(2) 0.001(2) -0.0016(19) 0.016(2) C22 0.100(4) 0.118(5) 0.028(2) 0.006(3) -0.004(3) 0.023(4) C23 0.124(6) 0.106(5) 0.033(3) 0.012(3) 0.022(3) 0.016(4) C24 0.080(4) 0.079(4) 0.054(3) 0.002(3) 0.041(3) -0.006(3) C25 0.050(2) 0.055(3) 0.043(2) 0.002(2) 0.014(2) 0.000(2) N3 0.0361(17) 0.0373(18) 0.0269(16) -0.0008(13) 0.0090(13) 0.0012(14) C26 0.084(4) 0.128(5) 0.034(3) 0.013(3) 0.012(3) 0.028(4) O6 0.0388(14) 0.0554(17) 0.0245(13) -0.0024(12) 0.0081(11) 0.0070(13) C27 0.072(4) 0.093(5) 0.127(6) 0.003(4) 0.007(4) -0.020(4) O7 0.047(2) 0.115(3) 0.122(4) 0.025(3) 0.017(2) 0.010(2) C28 0.055(3) 0.108(5) 0.052(3) 0.002(3) -0.019(2) 0.015(3) O8 0.0489(18) 0.095(3) 0.058(2) -0.021(2) -0.0004(15) 0.0080(19) C1S 0.039(2) 0.059(3) 0.040(2) -0.014(2) -0.0005(18) -0.005(2) Cl1 0.0621(8) 0.0920(9) 0.0592(7) -0.0301(7) -0.0097(6) 0.0185(7) Cl2 0.0433(6) 0.1381(13) 0.0391(6) -0.0143(7) -0.0027(5) 0.0157(7) C2S 0.110(5) 0.097(5) 0.069(4) 0.007(3) 0.007(4) 0.041(4) Cl3 0.1097(13) 0.1303(15) 0.0829(11) 0.0389(11) 0.0043(10) 0.0463(12) Cl4 0.0967(11) 0.0761(9) 0.0794(10) 0.0111(8) 0.0234(8) 0.0196(8) C3S 0.096(5) 0.229(10) 0.059(4) 0.030(5) -0.002(4) -0.024(6) Cl5 0.0915(11) 0.1198(14) 0.0755(10) 0.0127(9) 0.0140(9) -0.0069(10) Cl6 0.1300(17) 0.195(2) 0.0671(10) 0.0130(12) -0.0154(11) 0.0139(17) C29 0.242(12) 0.184(9) 0.059(4) -0.032(5) -0.017(6) 0.092(9) C30 0.150(7) 0.099(6) 0.145(8) -0.062(6) -0.036(6) 0.052(5) C31 0.134(7) 0.108(6) 0.168(8) 0.087(6) -0.029(6) 0.016(6) C32 0.187(10) 0.192(10) 0.095(6) 0.059(7) 0.013(6) 0.075(8) O10 0.097(3) 0.065(2) 0.106(3) -0.002(2) -0.025(3) 0.027(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O4C 1.930(2) . ? Cu1 O4A 1.944(2) . ? Cu1 O4B 2.033(2) . ? Cu1 O4D 2.075(2) . ? Cu1 N3 2.143(3) . ? Cu1 Cu2 2.7185(5) . ? Cu2 O5B 1.896(2) . ? Cu2 O5D 1.923(2) . ? Cu2 O5C 2.002(2) . ? Cu2 O5A 2.026(2) . ? Cu2 O3E 2.130(2) . ? Cu3 O4E 1.950(2) . ? Cu3 O4G 1.952(2) . ? Cu3 O4H 1.974(2) . ? Cu3 O4F 2.015(2) . ? Cu3 O6 2.163(2) . ? Cu3 Cu4 2.6714(5) . ? Cu4 O5H 1.944(2) . ? Cu4 O5F 1.965(2) . ? Cu4 O5G 1.993(2) . ? Cu4 O5E 2.021(2) . ? Cu4 O3A 2.142(2) . ? C1A O1A 1.204(4) . ? C1A N1A 1.399(5) . ? C1A C2A 1.497(5) . ? C2A C6A 1.377(6) . ? C2A C3A 1.385(6) . ? C3A C4A 1.390(6) . ? C3A C9A 1.431(5) . ? C4A C12A 1.379(6) . ? C4A C5A 1.494(5) . ? C5A O2A 1.199(5) . ? C5A N1A 1.396(5) . ? C6A C7A 1.414(6) . ? C6A H6A 0.9500 . ? C7A C8A 1.352(7) . ? C7A H7A 0.9500 . ? C8A C9A 1.409(7) . ? C8A H8A 0.9500 . ? C9A C10A 1.404(7) . ? C10A C11A 1.350(7) . ? C10A H10A 0.9500 . ? C11A C12A 1.404(6) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A N1A 1.470(4) . ? C13A C16A 1.525(5) . ? C13A C14A 1.541(5) . ? C13A H13A 1.0000 . ? C14A C15A 1.521(5) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A O3A 1.239(4) . ? C15A N2A 1.303(4) . ? C16A O5A 1.248(4) . ? C16A O4A 1.262(4) . ? N2A H2A1 0.8800 . ? N2A H2A2 0.8800 . ? C1B O1B 1.223(4) . ? C1B N1B 1.384(4) . ? C1B C2B 1.475(5) . ? C2B C6B 1.358(6) . ? C2B C3B 1.411(5) . ? C3B C4B 1.392(5) . ? C3B C9B 1.427(5) . ? C4B C12B 1.389(5) . ? C4B C5B 1.468(5) . ? C5B O2B 1.213(4) . ? C5B N1B 1.403(5) . ? C6B C7B 1.426(6) . ? C6B H6B 0.9500 . ? C7B C8B 1.343(6) . ? C7B H7B 0.9500 . ? C8B C9B 1.427(6) . ? C8B H8B 0.9500 . ? C9B C10B 1.399(6) . ? C10B C11B 1.363(6) . ? C10B H10B 0.9500 . ? C11B C12B 1.400(6) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B N1B 1.475(4) . ? C13B C16B 1.516(5) . ? C13B C14B 1.533(5) . ? C13B H13B 1.0000 . ? C14B C15B 1.517(5) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B O3B 1.233(4) . ? C15B N2B 1.312(5) . ? C16B O4B 1.247(4) . ? C16B O5B 1.259(4) . ? N2B H2B1 0.8800 . ? N2B H2B2 0.8800 . ? C1C O1C 1.215(4) . ? C1C N1C 1.376(5) . ? C1C C2C 1.492(5) . ? C2C C6C 1.370(6) . ? C2C C3C 1.417(6) . ? C3C C4C 1.393(6) . ? C3C C9C 1.427(6) . ? C4C C12C 1.374(5) . ? C4C C5C 1.479(5) . ? C5C O2C 1.203(5) . ? C5C N1C 1.419(4) . ? C6C C7C 1.396(6) . ? C6C H6C 0.9500 . ? C7C C8C 1.355(7) . ? C7C H7C 0.9500 . ? C8C C9C 1.408(7) . ? C8C H8C 0.9500 . ? C9C C10C 1.393(6) . ? C10C C11C 1.351(7) . ? C10C H10C 0.9500 . ? C11C C12C 1.424(6) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C N1C 1.460(4) . ? C13C C16C 1.533(5) . ? C13C C14C 1.547(5) . ? C13C H13C 1.0000 . ? C14C C15C 1.495(5) . ? C14C H14E 0.9900 . ? C14C H14F 0.9900 . ? C15C O3C 1.225(4) . ? C15C N2C 1.330(5) . ? C16C O5C 1.255(4) . ? C16C O4C 1.256(4) . ? N2C H2C1 0.8800 . ? N2C H2C2 0.8800 . ? C1D O1D 1.200(5) . ? C1D N1D 1.412(5) . ? C1D C2D 1.465(6) . ? C2D C6D 1.388(7) . ? C2D C3D 1.405(7) . ? C3D C4D 1.412(7) . ? C3D C9D 1.415(7) . ? C4D C12D 1.371(7) . ? C4D C5D 1.492(6) . ? C5D O2D 1.208(5) . ? C5D N1D 1.377(5) . ? C6D C7D 1.423(8) . ? C6D H6D 0.9500 . ? C7D C8D 1.358(10) . ? C7D H7D 0.9500 . ? C8D C9D 1.389(9) . ? C8D H8D 0.9500 . ? C9D C10D 1.429(10) . ? C10D C11D 1.330(9) . ? C10D H10D 0.9500 . ? C11D C12D 1.423(8) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D N1D 1.464(5) . ? C13D C14D 1.535(5) . ? C13D C16D 1.541(5) . ? C13D H13D 1.0000 . ? C14D C15D 1.512(5) . ? C14D H14G 0.9900 . ? C14D H14H 0.9900 . ? C15D O3D 1.221(5) . ? C15D N2D 1.321(5) . ? C16D O4D 1.232(4) . ? C16D O5D 1.268(4) . ? N2D H2D1 0.8800 . ? N2D H2D2 0.8800 . ? C1E O1E 1.213(4) . ? C1E N1E 1.398(5) . ? C1E C2E 1.476(5) . ? C2E C6E 1.372(6) . ? C2E C3E 1.420(5) . ? C3E C4E 1.410(6) . ? C3E C9E 1.415(5) . ? C4E C12E 1.390(5) . ? C4E C5E 1.477(5) . ? C5E O2E 1.220(5) . ? C5E N1E 1.392(4) . ? C6E C7E 1.392(6) . ? C6E H6E 0.9500 . ? C7E C8E 1.367(7) . ? C7E H7E 0.9500 . ? C8E C9E 1.403(7) . ? C8E H8E 0.9500 . ? C9E C10E 1.404(7) . ? C10E C11E 1.363(7) . ? C10E H10E 0.9500 . ? C11E C12E 1.390(6) . ? C11E H11E 0.9500 . ? C12E H12E 0.9500 . ? C13E N1E 1.479(4) . ? C13E C16E 1.529(4) . ? C13E C14E 1.544(4) . ? C13E H13E 1.0000 . ? C14E C15E 1.507(5) . ? C14E H14I 0.9900 . ? C14E H14J 0.9900 . ? C15E O3E 1.245(4) . ? C15E N2E 1.297(5) . ? C16E O4E 1.246(4) . ? C16E O5E 1.261(4) . ? N2E H2E1 0.8800 . ? N2E H2E2 0.8800 . ? C1F O1F 1.191(4) . ? C1F N1F 1.405(4) . ? C1F C2F 1.493(5) . ? C2F C6F 1.361(6) . ? C2F C3F 1.409(5) . ? C3F C4F 1.393(5) . ? C3F C9F 1.432(5) . ? C4F C12F 1.378(5) . ? C4F C5F 1.483(5) . ? C5F O2F 1.209(4) . ? C5F N1F 1.403(4) . ? C6F C7F 1.392(6) . ? C6F H6F 0.9500 . ? C7F C8F 1.368(7) . ? C7F H7F 0.9500 . ? C8F C9F 1.402(7) . ? C8F H8F 0.9500 . ? C9F C10F 1.401(6) . ? C10F C11F 1.364(7) . ? C10F H10F 0.9500 . ? C11F C12F 1.391(6) . ? C11F H11F 0.9500 . ? C12F H12F 0.9500 . ? C13F N1F 1.457(4) . ? C13F C16F 1.521(5) . ? C13F C14F 1.527(5) . ? C13F H13F 1.0000 . ? C14F C15F 1.514(5) . ? C14F H14K 0.9900 . ? C14F H14L 0.9900 . ? C15F O3F 1.237(4) . ? C15F N2F 1.336(4) . ? C16F O4F 1.257(4) . ? C16F O5F 1.266(4) . ? N2F H2F1 0.8800 . ? N2F H2F2 0.8800 . ? C1G O1G 1.220(4) . ? C1G N1G 1.397(4) . ? C1G C2G 1.482(5) . ? C2G C6G 1.364(5) . ? C2G C3G 1.434(5) . ? C3G C4G 1.402(5) . ? C3G C9G 1.405(5) . ? C4G C12G 1.380(5) . ? C4G C5G 1.474(5) . ? C5G O2G 1.219(4) . ? C5G N1G 1.404(4) . ? C6G C7G 1.407(6) . ? C6G H6G 0.9500 . ? C7G C8G 1.370(6) . ? C7G H7G 0.9500 . ? C8G C9G 1.403(6) . ? C8G H8G 0.9500 . ? C9G C10G 1.434(6) . ? C10G C11G 1.354(6) . ? C10G H10G 0.9500 . ? C11G C12G 1.407(6) . ? C11G H11G 0.9500 . ? C12G H12G 0.9500 . ? C13G N1G 1.480(4) . ? C13G C14G 1.517(5) . ? C13G C16G 1.549(5) . ? C13G H13G 1.0000 . ? C14G C15G 1.518(5) . ? C14G H14M 0.9900 . ? C14G H14N 0.9900 . ? C15G O3G 1.210(5) . ? C15G N2G 1.301(5) . ? C16G O5G 1.241(4) . ? C16G O4G 1.257(4) . ? N2G H2G1 0.8800 . ? N2G H2G2 0.8800 . ? C1H O1H 1.215(4) . ? C1H N1H 1.387(5) . ? C1H C2H 1.476(5) . ? C2H C6H 1.370(5) . ? C2H C3H 1.423(5) . ? C3H C4H 1.400(6) . ? C3H C9H 1.415(5) . ? C4H C12H 1.394(6) . ? C4H C5H 1.469(5) . ? C5H O2H 1.216(5) . ? C5H N1H 1.419(5) . ? C6H C7H 1.392(5) . ? C6H H6H 0.9500 . ? C7H C8H 1.364(6) . ? C7H H7H 0.9500 . ? C8H C9H 1.420(6) . ? C8H H8H 0.9500 . ? C9H C10H 1.406(6) . ? C10H C11H 1.373(7) . ? C10H H10H 0.9500 . ? C11H C12H 1.392(6) . ? C11H H11H 0.9500 . ? C12H H12H 0.9500 . ? C13H N1H 1.471(5) . ? C13H C16H 1.529(5) . ? C13H C14H 1.541(6) . ? C13H H13H 1.0000 . ? C14H C15H 1.513(6) . ? C14H H14O 0.9900 . ? C14H H14P 0.9900 . ? C15H O3H 1.244(5) . ? C15H N2H 1.296(5) . ? C16H O4H 1.256(4) . ? C16H O5H 1.258(4) . ? N2H H2H1 0.8800 . ? N2H H2H2 0.8800 . ? C21 N3 1.327(5) . ? C21 C22 1.362(6) . ? C21 H21 0.9500 . ? C22 C23 1.369(9) . ? C22 H22 0.9500 . ? C23 C24 1.377(8) . ? C23 H23 0.9500 . ? C24 C25 1.388(6) . ? C24 H24 0.9500 . ? C25 N3 1.329(5) . ? C25 H25 0.9500 . ? C26 O6 1.427(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O6 H6M 0.8316 . ? C27 O7 1.445(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O7 H7M 0.8493 . ? C28 O8 1.402(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O8 H8M 0.8401 . ? C1S Cl2 1.749(4) . ? C1S Cl1 1.757(4) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S Cl4 1.761(6) . ? C2S Cl3 1.767(6) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S Cl5 1.729(7) . ? C3S Cl6 1.736(7) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C29 C30 1.534(10) . ? C29 H29D 0.9800 . ? C29 H29E 0.9800 . ? C29 H29F 0.9800 . ? C30 O10 1.417(7) . ? C30 H30C 0.9900 . ? C30 H30D 0.9900 . ? C31 O10 1.417(7) . ? C31 C32 1.585(10) . ? C31 H31C 0.9900 . ? C31 H31D 0.9900 . ? C32 H32D 0.9800 . ? C32 H32E 0.9800 . ? C32 H32F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4C Cu1 O4A 176.06(9) . . ? O4C Cu1 O4B 90.20(9) . . ? O4A Cu1 O4B 90.06(9) . . ? O4C Cu1 O4D 90.18(9) . . ? O4A Cu1 O4D 87.87(9) . . ? O4B Cu1 O4D 154.24(9) . . ? O4C Cu1 N3 92.23(10) . . ? O4A Cu1 N3 91.61(10) . . ? O4B Cu1 N3 99.20(10) . . ? O4D Cu1 N3 106.52(11) . . ? O4C Cu1 Cu2 87.87(7) . . ? O4A Cu1 Cu2 88.36(7) . . ? O4B Cu1 Cu2 76.75(6) . . ? O4D Cu1 Cu2 77.52(7) . . ? N3 Cu1 Cu2 175.96(8) . . ? O5B Cu2 O5D 177.61(10) . . ? O5B Cu2 O5C 92.97(10) . . ? O5D Cu2 O5C 88.62(10) . . ? O5B Cu2 O5A 88.06(10) . . ? O5D Cu2 O5A 89.77(10) . . ? O5C Cu2 O5A 156.47(9) . . ? O5B Cu2 O3E 88.40(10) . . ? O5D Cu2 O3E 92.92(9) . . ? O5C Cu2 O3E 105.04(9) . . ? O5A Cu2 O3E 98.49(9) . . ? O5B Cu2 Cu1 89.66(7) . . ? O5D Cu2 Cu1 88.90(7) . . ? O5C Cu2 Cu1 78.43(7) . . ? O5A Cu2 Cu1 78.07(6) . . ? O3E Cu2 Cu1 176.11(7) . . ? O4E Cu3 O4G 172.36(10) . . ? O4E Cu3 O4H 86.35(10) . . ? O4G Cu3 O4H 87.99(10) . . ? O4E Cu3 O4F 89.33(9) . . ? O4G Cu3 O4F 94.45(9) . . ? O4H Cu3 O4F 161.60(9) . . ? O4E Cu3 O6 90.74(10) . . ? O4G Cu3 O6 95.81(9) . . ? O4H Cu3 O6 106.73(10) . . ? O4F Cu3 O6 91.19(10) . . ? O4E Cu3 Cu4 91.61(6) . . ? O4G Cu3 Cu4 82.76(6) . . ? O4H Cu3 Cu4 84.80(7) . . ? O4F Cu3 Cu4 77.44(6) . . ? O6 Cu3 Cu4 168.36(8) . . ? O5H Cu4 O5F 172.71(10) . . ? O5H Cu4 O5G 88.22(10) . . ? O5F Cu4 O5G 93.52(9) . . ? O5H Cu4 O5E 90.21(9) . . ? O5F Cu4 O5E 85.79(9) . . ? O5G Cu4 O5E 160.61(9) . . ? O5H Cu4 O3A 94.32(10) . . ? O5F Cu4 O3A 92.21(9) . . ? O5G Cu4 O3A 102.59(9) . . ? O5E Cu4 O3A 96.80(9) . . ? O5H Cu4 Cu3 82.68(7) . . ? O5F Cu4 Cu3 90.44(6) . . ? O5G Cu4 Cu3 84.51(6) . . ? O5E Cu4 Cu3 76.12(6) . . ? O3A Cu4 Cu3 172.24(7) . . ? O1A C1A N1A 120.9(3) . . ? O1A C1A C2A 122.5(4) . . ? N1A C1A C2A 116.6(3) . . ? C6A C2A C3A 121.1(4) . . ? C6A C2A C1A 118.2(4) . . ? C3A C2A C1A 120.6(3) . . ? C2A C3A C4A 120.9(3) . . ? C2A C3A C9A 120.1(4) . . ? C4A C3A C9A 119.0(4) . . ? C12A C4A C3A 120.5(4) . . ? C12A C4A C5A 118.9(4) . . ? C3A C4A C5A 120.6(3) . . ? O2A C5A N1A 121.3(3) . . ? O2A C5A C4A 122.2(4) . . ? N1A C5A C4A 116.5(3) . . ? C2A C6A C7A 119.3(5) . . ? C2A C6A H6A 120.3 . . ? C7A C6A H6A 120.3 . . ? C8A C7A C6A 120.1(5) . . ? C8A C7A H7A 119.9 . . ? C6A C7A H7A 119.9 . . ? C7A C8A C9A 122.2(4) . . ? C7A C8A H8A 118.9 . . ? C9A C8A H8A 118.9 . . ? C10A C9A C8A 124.3(4) . . ? C10A C9A C3A 118.5(4) . . ? C8A C9A C3A 117.1(4) . . ? C11A C10A C9A 121.5(4) . . ? C11A C10A H10A 119.3 . . ? C9A C10A H10A 119.3 . . ? C10A C11A C12A 120.0(5) . . ? C10A C11A H11A 120.0 . . ? C12A C11A H11A 120.0 . . ? C4A C12A C11A 120.3(5) . . ? C4A C12A H12A 119.8 . . ? C11A C12A H12A 119.8 . . ? N1A C13A C16A 110.8(3) . . ? N1A C13A C14A 113.0(3) . . ? C16A C13A C14A 112.3(3) . . ? N1A C13A H13A 106.8 . . ? C16A C13A H13A 106.8 . . ? C14A C13A H13A 106.8 . . ? C15A C14A C13A 114.0(3) . . ? C15A C14A H14A 108.7 . . ? C13A C14A H14A 108.7 . . ? C15A C14A H14B 108.7 . . ? C13A C14A H14B 108.7 . . ? H14A C14A H14B 107.6 . . ? O3A C15A N2A 124.8(3) . . ? O3A C15A C14A 119.2(3) . . ? N2A C15A C14A 115.9(3) . . ? O5A C16A O4A 126.9(3) . . ? O5A C16A C13A 115.2(3) . . ? O4A C16A C13A 117.9(3) . . ? C5A N1A C1A 124.5(3) . . ? C5A N1A C13A 118.0(3) . . ? C1A N1A C13A 117.1(3) . . ? C15A N2A H2A1 120.0 . . ? C15A N2A H2A2 120.0 . . ? H2A1 N2A H2A2 120.0 . . ? C15A O3A Cu4 126.9(2) . . ? C16A O4A Cu1 118.6(2) . . ? C16A O5A Cu2 127.4(2) . . ? O1B C1B N1B 119.9(3) . . ? O1B C1B C2B 122.6(3) . . ? N1B C1B C2B 117.5(3) . . ? C6B C2B C3B 121.3(3) . . ? C6B C2B C1B 120.0(4) . . ? C3B C2B C1B 118.7(3) . . ? C4B C3B C2B 121.6(3) . . ? C4B C3B C9B 119.1(4) . . ? C2B C3B C9B 119.3(3) . . ? C12B C4B C3B 120.5(4) . . ? C12B C4B C5B 118.8(4) . . ? C3B C4B C5B 120.7(4) . . ? O2B C5B N1B 120.4(3) . . ? O2B C5B C4B 123.6(3) . . ? N1B C5B C4B 116.0(3) . . ? C2B C6B C7B 119.6(4) . . ? C2B C6B H6B 120.2 . . ? C7B C6B H6B 120.2 . . ? C8B C7B C6B 120.5(4) . . ? C8B C7B H7B 119.8 . . ? C6B C7B H7B 119.8 . . ? C7B C8B C9B 121.7(4) . . ? C7B C8B H8B 119.2 . . ? C9B C8B H8B 119.2 . . ? C10B C9B C8B 123.1(4) . . ? C10B C9B C3B 119.3(4) . . ? C8B C9B C3B 117.6(4) . . ? C11B C10B C9B 120.6(4) . . ? C11B C10B H10B 119.7 . . ? C9B C10B H10B 119.7 . . ? C10B C11B C12B 120.7(4) . . ? C10B C11B H11B 119.7 . . ? C12B C11B H11B 119.7 . . ? C4B C12B C11B 119.8(4) . . ? C4B C12B H12B 120.1 . . ? C11B C12B H12B 120.1 . . ? N1B C13B C16B 110.1(3) . . ? N1B C13B C14B 111.5(3) . . ? C16B C13B C14B 113.3(3) . . ? N1B C13B H13B 107.2 . . ? C16B C13B H13B 107.2 . . ? C14B C13B H13B 107.2 . . ? C15B C14B C13B 111.4(3) . . ? C15B C14B H14C 109.4 . . ? C13B C14B H14C 109.4 . . ? C15B C14B H14D 109.4 . . ? C13B C14B H14D 109.4 . . ? H14C C14B H14D 108.0 . . ? O3B C15B N2B 122.4(3) . . ? O3B C15B C14B 121.1(3) . . ? N2B C15B C14B 116.6(3) . . ? O4B C16B O5B 127.0(3) . . ? O4B C16B C13B 117.9(3) . . ? O5B C16B C13B 115.0(3) . . ? C1B N1B C5B 125.1(3) . . ? C1B N1B C13B 117.3(3) . . ? C5B N1B C13B 117.5(3) . . ? C15B N2B H2B1 120.0 . . ? C15B N2B H2B2 120.0 . . ? H2B1 N2B H2B2 120.0 . . ? C16B O4B Cu1 127.8(2) . . ? C16B O5B Cu2 118.8(2) . . ? O1C C1C N1C 120.5(3) . . ? O1C C1C C2C 122.1(4) . . ? N1C C1C C2C 117.3(3) . . ? C6C C2C C3C 120.4(4) . . ? C6C C2C C1C 120.2(4) . . ? C3C C2C C1C 119.4(3) . . ? C4C C3C C2C 121.1(3) . . ? C4C C3C C9C 119.5(4) . . ? C2C C3C C9C 119.4(4) . . ? C12C C4C C3C 120.8(3) . . ? C12C C4C C5C 118.4(4) . . ? C3C C4C C5C 120.8(3) . . ? O2C C5C N1C 120.8(3) . . ? O2C C5C C4C 122.9(3) . . ? N1C C5C C4C 116.3(3) . . ? C2C C6C C7C 120.4(4) . . ? C2C C6C H6C 119.8 . . ? C7C C6C H6C 119.8 . . ? C8C C7C C6C 120.1(5) . . ? C8C C7C H7C 119.9 . . ? C6C C7C H7C 119.9 . . ? C7C C8C C9C 122.4(4) . . ? C7C C8C H8C 118.8 . . ? C9C C8C H8C 118.8 . . ? C10C C9C C8C 124.0(4) . . ? C10C C9C C3C 118.7(4) . . ? C8C C9C C3C 117.3(4) . . ? C11C C10C C9C 121.1(4) . . ? C11C C10C H10C 119.4 . . ? C9C C10C H10C 119.4 . . ? C10C C11C C12C 120.8(4) . . ? C10C C11C H11C 119.6 . . ? C12C C11C H11C 119.6 . . ? C4C C12C C11C 119.0(4) . . ? C4C C12C H12C 120.5 . . ? C11C C12C H12C 120.5 . . ? N1C C13C C16C 111.5(3) . . ? N1C C13C C14C 113.4(3) . . ? C16C C13C C14C 110.6(3) . . ? N1C C13C H13C 107.0 . . ? C16C C13C H13C 107.0 . . ? C14C C13C H13C 107.0 . . ? C15C C14C C13C 112.4(3) . . ? C15C C14C H14E 109.1 . . ? C13C C14C H14E 109.1 . . ? C15C C14C H14F 109.1 . . ? C13C C14C H14F 109.1 . . ? H14E C14C H14F 107.9 . . ? O3C C15C N2C 123.2(3) . . ? O3C C15C C14C 121.1(4) . . ? N2C C15C C14C 115.7(3) . . ? O5C C16C O4C 127.0(3) . . ? O5C C16C C13C 115.3(3) . . ? O4C C16C C13C 117.7(3) . . ? C1C N1C C5C 125.0(3) . . ? C1C N1C C13C 117.4(3) . . ? C5C N1C C13C 117.5(3) . . ? C15C N2C H2C1 120.0 . . ? C15C N2C H2C2 120.0 . . ? H2C1 N2C H2C2 120.0 . . ? C16C O4C Cu1 119.1(2) . . ? C16C O5C Cu2 127.1(2) . . ? O1D C1D N1D 119.5(4) . . ? O1D C1D C2D 123.8(4) . . ? N1D C1D C2D 116.6(4) . . ? C6D C2D C3D 120.6(5) . . ? C6D C2D C1D 118.6(5) . . ? C3D C2D C1D 120.6(4) . . ? C2D C3D C4D 120.5(4) . . ? C2D C3D C9D 120.5(5) . . ? C4D C3D C9D 119.0(5) . . ? C12D C4D C3D 120.2(5) . . ? C12D C4D C5D 120.3(5) . . ? C3D C4D C5D 119.5(4) . . ? O2D C5D N1D 120.9(4) . . ? O2D C5D C4D 122.0(4) . . ? N1D C5D C4D 117.0(4) . . ? C2D C6D C7D 117.8(6) . . ? C2D C6D H6D 121.1 . . ? C7D C6D H6D 121.1 . . ? C8D C7D C6D 121.3(6) . . ? C8D C7D H7D 119.4 . . ? C6D C7D H7D 119.4 . . ? C7D C8D C9D 121.9(6) . . ? C7D C8D H8D 119.0 . . ? C9D C8D H8D 119.0 . . ? C8D C9D C3D 117.8(6) . . ? C8D C9D C10D 123.5(6) . . ? C3D C9D C10D 118.7(6) . . ? C11D C10D C9D 121.3(6) . . ? C11D C10D H10D 119.4 . . ? C9D C10D H10D 119.4 . . ? C10D C11D C12D 120.2(6) . . ? C10D C11D H11D 119.9 . . ? C12D C11D H11D 119.9 . . ? C4D C12D C11D 120.4(6) . . ? C4D C12D H12D 119.8 . . ? C11D C12D H12D 119.8 . . ? N1D C13D C14D 113.2(3) . . ? N1D C13D C16D 110.1(3) . . ? C14D C13D C16D 112.0(3) . . ? N1D C13D H13D 107.1 . . ? C14D C13D H13D 107.1 . . ? C16D C13D H13D 107.1 . . ? C15D C14D C13D 113.4(3) . . ? C15D C14D H14G 108.9 . . ? C13D C14D H14G 108.9 . . ? C15D C14D H14H 108.9 . . ? C13D C14D H14H 108.9 . . ? H14G C14D H14H 107.7 . . ? O3D C15D N2D 123.2(4) . . ? O3D C15D C14D 120.8(4) . . ? N2D C15D C14D 115.9(4) . . ? O4D C16D O5D 126.9(3) . . ? O4D C16D C13D 119.8(3) . . ? O5D C16D C13D 113.3(3) . . ? C5D N1D C1D 124.8(4) . . ? C5D N1D C13D 118.5(3) . . ? C1D N1D C13D 116.5(3) . . ? C15D N2D H2D1 120.0 . . ? C15D N2D H2D2 120.0 . . ? H2D1 N2D H2D2 120.0 . . ? C16D O4D Cu1 126.7(2) . . ? C16D O5D Cu2 119.8(2) . . ? O1E C1E N1E 119.7(3) . . ? O1E C1E C2E 123.5(3) . . ? N1E C1E C2E 116.7(3) . . ? C6E C2E C3E 119.7(4) . . ? C6E C2E C1E 120.3(4) . . ? C3E C2E C1E 120.0(4) . . ? C4E C3E C9E 119.9(4) . . ? C4E C3E C2E 120.4(3) . . ? C9E C3E C2E 119.7(4) . . ? C12E C4E C3E 120.0(4) . . ? C12E C4E C5E 119.3(4) . . ? C3E C4E C5E 120.7(3) . . ? O2E C5E N1E 120.6(3) . . ? O2E C5E C4E 123.1(3) . . ? N1E C5E C4E 116.3(3) . . ? C2E C6E C7E 121.1(4) . . ? C2E C6E H6E 119.4 . . ? C7E C6E H6E 119.4 . . ? C8E C7E C6E 119.4(5) . . ? C8E C7E H7E 120.3 . . ? C6E C7E H7E 120.3 . . ? C7E C8E C9E 122.3(4) . . ? C7E C8E H8E 118.8 . . ? C9E C8E H8E 118.8 . . ? C8E C9E C10E 124.1(4) . . ? C8E C9E C3E 117.8(4) . . ? C10E C9E C3E 118.1(5) . . ? C11E C10E C9E 121.4(4) . . ? C11E C10E H10E 119.3 . . ? C9E C10E H10E 119.3 . . ? C10E C11E C12E 121.0(4) . . ? C10E C11E H11E 119.5 . . ? C12E C11E H11E 119.5 . . ? C4E C12E C11E 119.6(5) . . ? C4E C12E H12E 120.2 . . ? C11E C12E H12E 120.2 . . ? N1E C13E C16E 110.3(2) . . ? N1E C13E C14E 109.9(3) . . ? C16E C13E C14E 113.9(3) . . ? N1E C13E H13E 107.5 . . ? C16E C13E H13E 107.5 . . ? C14E C13E H13E 107.5 . . ? C15E C14E C13E 118.4(3) . . ? C15E C14E H14I 107.7 . . ? C13E C14E H14I 107.7 . . ? C15E C14E H14J 107.7 . . ? C13E C14E H14J 107.7 . . ? H14I C14E H14J 107.1 . . ? O3E C15E N2E 122.8(3) . . ? O3E C15E C14E 116.6(3) . . ? N2E C15E C14E 120.6(3) . . ? O4E C16E O5E 126.9(3) . . ? O4E C16E C13E 117.2(3) . . ? O5E C16E C13E 115.8(3) . . ? C5E N1E C1E 125.9(3) . . ? C5E N1E C13E 117.8(3) . . ? C1E N1E C13E 116.2(3) . . ? C15E N2E H2E1 120.0 . . ? C15E N2E H2E2 120.0 . . ? H2E1 N2E H2E2 120.0 . . ? C15E O3E Cu2 125.0(2) . . ? C16E O4E Cu3 115.4(2) . . ? C16E O5E Cu4 129.9(2) . . ? O1F C1F N1F 119.7(3) . . ? O1F C1F C2F 124.1(3) . . ? N1F C1F C2F 116.2(3) . . ? C6F C2F C3F 121.0(4) . . ? C6F C2F C1F 119.3(4) . . ? C3F C2F C1F 119.7(3) . . ? C4F C3F C2F 121.8(3) . . ? C4F C3F C9F 119.5(4) . . ? C2F C3F C9F 118.8(4) . . ? C12F C4F C3F 119.9(4) . . ? C12F C4F C5F 119.9(4) . . ? C3F C4F C5F 120.2(3) . . ? O2F C5F N1F 121.0(3) . . ? O2F C5F C4F 122.6(3) . . ? N1F C5F C4F 116.4(3) . . ? C2F C6F C7F 120.4(4) . . ? C2F C6F H6F 119.8 . . ? C7F C6F H6F 119.8 . . ? C8F C7F C6F 120.2(5) . . ? C8F C7F H7F 119.9 . . ? C6F C7F H7F 119.9 . . ? C7F C8F C9F 121.4(4) . . ? C7F C8F H8F 119.3 . . ? C9F C8F H8F 119.3 . . ? C10F C9F C8F 123.4(4) . . ? C10F C9F C3F 118.5(4) . . ? C8F C9F C3F 118.1(4) . . ? C11F C10F C9F 120.9(4) . . ? C11F C10F H10F 119.6 . . ? C9F C10F H10F 119.6 . . ? C10F C11F C12F 120.3(4) . . ? C10F C11F H11F 119.8 . . ? C12F C11F H11F 119.8 . . ? C4F C12F C11F 120.9(4) . . ? C4F C12F H12F 119.6 . . ? C11F C12F H12F 119.6 . . ? N1F C13F C16F 111.9(3) . . ? N1F C13F C14F 110.4(3) . . ? C16F C13F C14F 115.4(3) . . ? N1F C13F H13F 106.1 . . ? C16F C13F H13F 106.1 . . ? C14F C13F H13F 106.1 . . ? C15F C14F C13F 114.5(3) . . ? C15F C14F H14K 108.6 . . ? C13F C14F H14K 108.6 . . ? C15F C14F H14L 108.6 . . ? C13F C14F H14L 108.6 . . ? H14K C14F H14L 107.6 . . ? O3F C15F N2F 122.9(3) . . ? O3F C15F C14F 121.0(3) . . ? N2F C15F C14F 116.0(3) . . ? O4F C16F O5F 126.0(3) . . ? O4F C16F C13F 116.5(3) . . ? O5F C16F C13F 117.2(3) . . ? C5F N1F C1F 125.2(3) . . ? C5F N1F C13F 117.0(3) . . ? C1F N1F C13F 117.2(3) . . ? C15F N2F H2F1 120.0 . . ? C15F N2F H2F2 120.0 . . ? H2F1 N2F H2F2 120.0 . . ? C16F O4F Cu3 128.8(2) . . ? C16F O5F Cu4 116.0(2) . . ? O1G C1G N1G 119.7(3) . . ? O1G C1G C2G 122.6(3) . . ? N1G C1G C2G 117.7(3) . . ? C6G C2G C3G 119.9(3) . . ? C6G C2G C1G 120.5(3) . . ? C3G C2G C1G 119.6(3) . . ? C4G C3G C9G 120.5(3) . . ? C4G C3G C2G 120.1(3) . . ? C9G C3G C2G 119.3(3) . . ? C12G C4G C3G 120.0(3) . . ? C12G C4G C5G 118.9(3) . . ? C3G C4G C5G 121.1(3) . . ? O2G C5G N1G 119.8(3) . . ? O2G C5G C4G 123.0(3) . . ? N1G C5G C4G 117.2(3) . . ? C2G C6G C7G 120.4(4) . . ? C2G C6G H6G 119.8 . . ? C7G C6G H6G 119.8 . . ? C8G C7G C6G 120.3(4) . . ? C8G C7G H7G 119.8 . . ? C6G C7G H7G 119.8 . . ? C7G C8G C9G 121.1(4) . . ? C7G C8G H8G 119.5 . . ? C9G C8G H8G 119.5 . . ? C8G C9G C3G 119.0(4) . . ? C8G C9G C10G 122.9(4) . . ? C3G C9G C10G 118.1(4) . . ? C11G C10G C9G 120.4(4) . . ? C11G C10G H10G 119.8 . . ? C9G C10G H10G 119.8 . . ? C10G C11G C12G 121.1(4) . . ? C10G C11G H11G 119.5 . . ? C12G C11G H11G 119.5 . . ? C4G C12G C11G 119.9(4) . . ? C4G C12G H12G 120.1 . . ? C11G C12G H12G 120.1 . . ? N1G C13G C14G 110.0(3) . . ? N1G C13G C16G 111.7(3) . . ? C14G C13G C16G 114.5(3) . . ? N1G C13G H13G 106.7 . . ? C14G C13G H13G 106.7 . . ? C16G C13G H13G 106.7 . . ? C13G C14G C15G 112.4(3) . . ? C13G C14G H14M 109.1 . . ? C15G C14G H14M 109.1 . . ? C13G C14G H14N 109.1 . . ? C15G C14G H14N 109.1 . . ? H14M C14G H14N 107.9 . . ? O3G C15G N2G 121.8(4) . . ? O3G C15G C14G 123.2(4) . . ? N2G C15G C14G 115.0(4) . . ? O5G C16G O4G 127.5(3) . . ? O5G C16G C13G 117.2(3) . . ? O4G C16G C13G 115.1(3) . . ? C1G N1G C5G 124.4(3) . . ? C1G N1G C13G 118.0(3) . . ? C5G N1G C13G 117.1(3) . . ? C15G N2G H2G1 120.0 . . ? C15G N2G H2G2 120.0 . . ? H2G1 N2G H2G2 120.0 . . ? C16G O4G Cu3 124.1(2) . . ? C16G O5G Cu4 119.8(2) . . ? O1H C1H N1H 119.5(3) . . ? O1H C1H C2H 122.3(3) . . ? N1H C1H C2H 118.2(3) . . ? C6H C2H C3H 120.1(3) . . ? C6H C2H C1H 120.5(3) . . ? C3H C2H C1H 119.4(3) . . ? C4H C3H C9H 120.7(3) . . ? C4H C3H C2H 120.1(3) . . ? C9H C3H C2H 119.3(4) . . ? C12H C4H C3H 119.0(4) . . ? C12H C4H C5H 119.1(4) . . ? C3H C4H C5H 121.8(3) . . ? O2H C5H N1H 119.4(4) . . ? O2H C5H C4H 124.6(3) . . ? N1H C5H C4H 116.0(3) . . ? C2H C6H C7H 120.6(4) . . ? C2H C6H H6H 119.7 . . ? C7H C6H H6H 119.7 . . ? C8H C7H C6H 120.9(4) . . ? C8H C7H H7H 119.6 . . ? C6H C7H H7H 119.6 . . ? C7H C8H C9H 120.6(4) . . ? C7H C8H H8H 119.7 . . ? C9H C8H H8H 119.7 . . ? C10H C9H C3H 118.5(4) . . ? C10H C9H C8H 123.0(4) . . ? C3H C9H C8H 118.6(4) . . ? C11H C10H C9H 120.7(4) . . ? C11H C10H H10H 119.7 . . ? C9H C10H H10H 119.7 . . ? C10H C11H C12H 120.6(4) . . ? C10H C11H H11H 119.7 . . ? C12H C11H H11H 119.7 . . ? C11H C12H C4H 120.5(4) . . ? C11H C12H H12H 119.7 . . ? C4H C12H H12H 119.7 . . ? N1H C13H C16H 111.1(3) . . ? N1H C13H C14H 112.0(3) . . ? C16H C13H C14H 113.0(3) . . ? N1H C13H H13H 106.8 . . ? C16H C13H H13H 106.8 . . ? C14H C13H H13H 106.8 . . ? C15H C14H C13H 109.6(3) . . ? C15H C14H H14O 109.8 . . ? C13H C14H H14O 109.8 . . ? C15H C14H H14P 109.8 . . ? C13H C14H H14P 109.8 . . ? H14O C14H H14P 108.2 . . ? O3H C15H N2H 123.4(4) . . ? O3H C15H C14H 118.4(4) . . ? N2H C15H C14H 118.2(4) . . ? O4H C16H O5H 126.9(3) . . ? O4H C16H C13H 116.2(3) . . ? O5H C16H C13H 116.9(3) . . ? C1H N1H C5H 124.1(3) . . ? C1H N1H C13H 116.8(3) . . ? C5H N1H C13H 119.0(3) . . ? C15H N2H H2H1 120.0 . . ? C15H N2H H2H2 120.0 . . ? H2H1 N2H H2H2 120.0 . . ? C16H O4H Cu3 120.7(2) . . ? C16H O5H Cu4 124.6(2) . . ? N3 C21 C22 123.6(5) . . ? N3 C21 H21 118.2 . . ? C22 C21 H21 118.2 . . ? C21 C22 C23 118.9(5) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C22 C23 C24 119.1(5) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C25 118.0(5) . . ? C23 C24 H24 121.0 . . ? C25 C24 H24 121.0 . . ? N3 C25 C24 122.9(5) . . ? N3 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? C21 N3 C25 117.5(3) . . ? C21 N3 Cu1 119.7(3) . . ? C25 N3 Cu1 122.6(3) . . ? O6 C26 H26A 109.5 . . ? O6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C26 O6 Cu3 117.8(3) . . ? C26 O6 H6M 103.2 . . ? Cu3 O6 H6M 117.7 . . ? O7 C27 H27A 109.5 . . ? O7 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O7 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C27 O7 H7M 108.5 . . ? O8 C28 H28A 109.5 . . ? O8 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O8 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C28 O8 H8M 122.5 . . ? Cl2 C1S Cl1 111.7(2) . . ? Cl2 C1S H1S1 109.3 . . ? Cl1 C1S H1S1 109.3 . . ? Cl2 C1S H1S2 109.3 . . ? Cl1 C1S H1S2 109.3 . . ? H1S1 C1S H1S2 107.9 . . ? Cl4 C2S Cl3 111.5(3) . . ? Cl4 C2S H2S1 109.3 . . ? Cl3 C2S H2S1 109.3 . . ? Cl4 C2S H2S2 109.3 . . ? Cl3 C2S H2S2 109.3 . . ? H2S1 C2S H2S2 108.0 . . ? Cl5 C3S Cl6 113.4(4) . . ? Cl5 C3S H3S1 108.9 . . ? Cl6 C3S H3S1 108.9 . . ? Cl5 C3S H3S2 108.9 . . ? Cl6 C3S H3S2 108.9 . . ? H3S1 C3S H3S2 107.7 . . ? C30 C29 H29D 109.5 . . ? C30 C29 H29E 109.5 . . ? H29D C29 H29E 109.5 . . ? C30 C29 H29F 109.5 . . ? H29D C29 H29F 109.5 . . ? H29E C29 H29F 109.5 . . ? O10 C30 C29 107.7(6) . . ? O10 C30 H30C 110.2 . . ? C29 C30 H30C 110.2 . . ? O10 C30 H30D 110.2 . . ? C29 C30 H30D 110.2 . . ? H30C C30 H30D 108.5 . . ? O10 C31 C32 107.6(6) . . ? O10 C31 H31C 110.2 . . ? C32 C31 H31C 110.2 . . ? O10 C31 H31D 110.2 . . ? C32 C31 H31D 110.2 . . ? H31C C31 H31D 108.5 . . ? C31 C32 H32D 109.5 . . ? C31 C32 H32E 109.5 . . ? H32D C32 H32E 109.5 . . ? C31 C32 H32F 109.5 . . ? H32D C32 H32F 109.5 . . ? H32E C32 H32F 109.5 . . ? C31 O10 C30 116.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4C Cu1 Cu2 O5B -90.66(10) . . . . ? O4A Cu1 Cu2 O5B 90.51(10) . . . . ? O4B Cu1 Cu2 O5B 0.05(10) . . . . ? O4D Cu1 Cu2 O5B 178.69(10) . . . . ? O4C Cu1 Cu2 O5D 91.26(10) . . . . ? O4A Cu1 Cu2 O5D -87.58(10) . . . . ? O4B Cu1 Cu2 O5D -178.03(9) . . . . ? O4D Cu1 Cu2 O5D 0.61(10) . . . . ? O4C Cu1 Cu2 O5C 2.45(10) . . . . ? O4A Cu1 Cu2 O5C -176.39(10) . . . . ? O4B Cu1 Cu2 O5C 93.16(9) . . . . ? O4D Cu1 Cu2 O5C -88.21(10) . . . . ? O4C Cu1 Cu2 O5A -178.74(10) . . . . ? O4A Cu1 Cu2 O5A 2.42(10) . . . . ? O4B Cu1 Cu2 O5A -88.03(9) . . . . ? O4D Cu1 Cu2 O5A 90.61(10) . . . . ? O4E Cu3 Cu4 O5H -89.99(10) . . . . ? O4G Cu3 Cu4 O5H 84.83(10) . . . . ? O4H Cu3 Cu4 O5H -3.80(10) . . . . ? O4F Cu3 Cu4 O5H -178.95(10) . . . . ? O6 Cu3 Cu4 O5H 168.5(4) . . . . ? O4E Cu3 Cu4 O5F 87.61(9) . . . . ? O4G Cu3 Cu4 O5F -97.57(9) . . . . ? O4H Cu3 Cu4 O5F 173.80(9) . . . . ? O4F Cu3 Cu4 O5F -1.35(9) . . . . ? O6 Cu3 Cu4 O5F -13.9(4) . . . . ? O4E Cu3 Cu4 O5G -178.89(9) . . . . ? O4G Cu3 Cu4 O5G -4.07(9) . . . . ? O4H Cu3 Cu4 O5G -92.70(9) . . . . ? O4F Cu3 Cu4 O5G 92.15(9) . . . . ? O6 Cu3 Cu4 O5G 79.6(4) . . . . ? O4E Cu3 Cu4 O5E 2.05(10) . . . . ? O4G Cu3 Cu4 O5E 176.87(10) . . . . ? O4H Cu3 Cu4 O5E 88.24(9) . . . . ? O4F Cu3 Cu4 O5E -86.91(9) . . . . ? O6 Cu3 Cu4 O5E -99.5(4) . . . . ? O1A C1A C2A C6A 0.0(5) . . . . ? N1A C1A C2A C6A 177.9(3) . . . . ? O1A C1A C2A C3A -179.8(3) . . . . ? N1A C1A C2A C3A -1.9(5) . . . . ? C6A C2A C3A C4A -179.4(4) . . . . ? C1A C2A C3A C4A 0.5(5) . . . . ? C6A C2A C3A C9A 0.4(6) . . . . ? C1A C2A C3A C9A -179.8(3) . . . . ? C2A C3A C4A C12A -176.8(4) . . . . ? C9A C3A C4A C12A 3.5(5) . . . . ? C2A C3A C4A C5A 3.4(5) . . . . ? C9A C3A C4A C5A -176.3(3) . . . . ? C12A C4A C5A O2A -5.9(5) . . . . ? C3A C4A C5A O2A 173.9(4) . . . . ? C12A C4A C5A N1A 174.5(3) . . . . ? C3A C4A C5A N1A -5.7(5) . . . . ? C3A C2A C6A C7A -0.6(6) . . . . ? C1A C2A C6A C7A 179.6(4) . . . . ? C2A C6A C7A C8A 1.2(7) . . . . ? C6A C7A C8A C9A -1.7(8) . . . . ? C7A C8A C9A C10A -177.0(5) . . . . ? C7A C8A C9A C3A 1.5(7) . . . . ? C2A C3A C9A C10A 177.8(4) . . . . ? C4A C3A C9A C10A -2.4(6) . . . . ? C2A C3A C9A C8A -0.8(6) . . . . ? C4A C3A C9A C8A 178.9(4) . . . . ? C8A C9A C10A C11A 179.2(4) . . . . ? C3A C9A C10A C11A 0.7(6) . . . . ? C9A C10A C11A C12A 0.1(7) . . . . ? C3A C4A C12A C11A -2.8(6) . . . . ? C5A C4A C12A C11A 177.1(3) . . . . ? C10A C11A C12A C4A 0.9(6) . . . . ? N1A C13A C14A C15A -160.4(3) . . . . ? C16A C13A C14A C15A 73.4(4) . . . . ? C13A C14A C15A O3A 65.4(4) . . . . ? C13A C14A C15A N2A -117.7(3) . . . . ? N1A C13A C16A O5A -166.1(3) . . . . ? C14A C13A C16A O5A -38.7(4) . . . . ? N1A C13A C16A O4A 14.7(4) . . . . ? C14A C13A C16A O4A 142.1(3) . . . . ? O2A C5A N1A C1A -175.3(3) . . . . ? C4A C5A N1A C1A 4.4(5) . . . . ? O2A C5A N1A C13A -3.2(5) . . . . ? C4A C5A N1A C13A 176.4(3) . . . . ? O1A C1A N1A C5A 177.3(3) . . . . ? C2A C1A N1A C5A -0.7(5) . . . . ? O1A C1A N1A C13A 5.1(5) . . . . ? C2A C1A N1A C13A -172.9(3) . . . . ? C16A C13A N1A C5A -110.4(3) . . . . ? C14A C13A N1A C5A 122.6(3) . . . . ? C16A C13A N1A C1A 62.2(4) . . . . ? C14A C13A N1A C1A -64.7(4) . . . . ? N2A C15A O3A Cu4 -12.2(5) . . . . ? C14A C15A O3A Cu4 164.5(2) . . . . ? O5H Cu4 O3A C15A 135.5(3) . . . . ? O5F Cu4 O3A C15A -41.2(3) . . . . ? O5G Cu4 O3A C15A -135.3(3) . . . . ? O5E Cu4 O3A C15A 44.8(3) . . . . ? O5A C16A O4A Cu1 10.9(4) . . . . ? C13A C16A O4A Cu1 -170.0(2) . . . . ? O4B Cu1 O4A C16A 69.8(2) . . . . ? O4D Cu1 O4A C16A -84.5(2) . . . . ? N3 Cu1 O4A C16A 169.0(2) . . . . ? Cu2 Cu1 O4A C16A -7.0(2) . . . . ? O4A C16A O5A Cu2 -8.2(5) . . . . ? C13A C16A O5A Cu2 172.7(2) . . . . ? O5B Cu2 O5A C16A -88.4(3) . . . . ? O5D Cu2 O5A C16A 90.6(3) . . . . ? O5C Cu2 O5A C16A 4.5(4) . . . . ? O3E Cu2 O5A C16A -176.5(3) . . . . ? Cu1 Cu2 O5A C16A 1.6(3) . . . . ? O1B C1B C2B C6B -5.2(6) . . . . ? N1B C1B C2B C6B 173.8(4) . . . . ? O1B C1B C2B C3B 174.6(4) . . . . ? N1B C1B C2B C3B -6.3(5) . . . . ? C6B C2B C3B C4B -177.6(4) . . . . ? C1B C2B C3B C4B 2.6(6) . . . . ? C6B C2B C3B C9B 1.0(6) . . . . ? C1B C2B C3B C9B -178.9(4) . . . . ? C2B C3B C4B C12B 179.6(4) . . . . ? C9B C3B C4B C12B 1.0(6) . . . . ? C2B C3B C4B C5B 0.4(6) . . . . ? C9B C3B C4B C5B -178.2(4) . . . . ? C12B C4B C5B O2B 0.8(7) . . . . ? C3B C4B C5B O2B 180.0(4) . . . . ? C12B C4B C5B N1B -178.8(4) . . . . ? C3B C4B C5B N1B 0.4(6) . . . . ? C3B C2B C6B C7B -0.3(7) . . . . ? C1B C2B C6B C7B 179.6(4) . . . . ? C2B C6B C7B C8B -0.7(8) . . . . ? C6B C7B C8B C9B 0.9(8) . . . . ? C7B C8B C9B C10B 178.2(5) . . . . ? C7B C8B C9B C3B -0.2(7) . . . . ? C4B C3B C9B C10B -0.6(6) . . . . ? C2B C3B C9B C10B -179.2(4) . . . . ? C4B C3B C9B C8B 177.9(4) . . . . ? C2B C3B C9B C8B -0.7(6) . . . . ? C8B C9B C10B C11B -178.4(4) . . . . ? C3B C9B C10B C11B 0.0(6) . . . . ? C9B C10B C11B C12B 0.3(7) . . . . ? C3B C4B C12B C11B -0.7(7) . . . . ? C5B C4B C12B C11B 178.4(4) . . . . ? C10B C11B C12B C4B 0.1(7) . . . . ? N1B C13B C14B C15B -169.4(3) . . . . ? C16B C13B C14B C15B 65.7(4) . . . . ? C13B C14B C15B O3B 34.8(5) . . . . ? C13B C14B C15B N2B -145.6(3) . . . . ? N1B C13B C16B O4B 50.0(4) . . . . ? C14B C13B C16B O4B 175.7(3) . . . . ? N1B C13B C16B O5B -133.3(3) . . . . ? C14B C13B C16B O5B -7.7(4) . . . . ? O1B C1B N1B C5B -173.3(4) . . . . ? C2B C1B N1B C5B 7.7(6) . . . . ? O1B C1B N1B C13B 3.4(5) . . . . ? C2B C1B N1B C13B -175.7(3) . . . . ? O2B C5B N1B C1B 175.7(4) . . . . ? C4B C5B N1B C1B -4.7(6) . . . . ? O2B C5B N1B C13B -1.0(6) . . . . ? C4B C5B N1B C13B 178.6(3) . . . . ? C16B C13B N1B C1B 46.3(4) . . . . ? C14B C13B N1B C1B -80.4(4) . . . . ? C16B C13B N1B C5B -136.8(3) . . . . ? C14B C13B N1B C5B 96.6(4) . . . . ? O5B C16B O4B Cu1 0.6(5) . . . . ? C13B C16B O4B Cu1 176.7(2) . . . . ? O4C Cu1 O4B C16B 87.5(3) . . . . ? O4A Cu1 O4B C16B -88.6(3) . . . . ? O4D Cu1 O4B C16B -3.4(4) . . . . ? N3 Cu1 O4B C16B 179.8(3) . . . . ? Cu2 Cu1 O4B C16B -0.3(2) . . . . ? O4B C16B O5B Cu2 -0.4(4) . . . . ? C13B C16B O5B Cu2 -176.7(2) . . . . ? O5C Cu2 O5B C16B -78.2(2) . . . . ? O5A Cu2 O5B C16B 78.2(2) . . . . ? O3E Cu2 O5B C16B 176.8(2) . . . . ? Cu1 Cu2 O5B C16B 0.1(2) . . . . ? O1C C1C C2C C6C 3.8(5) . . . . ? N1C C1C C2C C6C -178.5(3) . . . . ? O1C C1C C2C C3C -177.0(3) . . . . ? N1C C1C C2C C3C 0.7(5) . . . . ? C6C C2C C3C C4C 179.4(4) . . . . ? C1C C2C C3C C4C 0.2(5) . . . . ? C6C C2C C3C C9C -0.2(5) . . . . ? C1C C2C C3C C9C -179.5(3) . . . . ? C2C C3C C4C C12C -178.8(3) . . . . ? C9C C3C C4C C12C 0.9(5) . . . . ? C2C C3C C4C C5C 1.1(5) . . . . ? C9C C3C C4C C5C -179.2(3) . . . . ? C12C C4C C5C O2C -4.0(5) . . . . ? C3C C4C C5C O2C 176.1(3) . . . . ? C12C C4C C5C N1C 176.7(3) . . . . ? C3C C4C C5C N1C -3.2(5) . . . . ? C3C C2C C6C C7C 0.4(6) . . . . ? C1C C2C C6C C7C 179.7(4) . . . . ? C2C C6C C7C C8C -0.4(7) . . . . ? C6C C7C C8C C9C 0.1(8) . . . . ? C7C C8C C9C C10C 179.3(5) . . . . ? C7C C8C C9C C3C 0.1(7) . . . . ? C4C C3C C9C C10C 1.0(6) . . . . ? C2C C3C C9C C10C -179.3(4) . . . . ? C4C C3C C9C C8C -179.7(4) . . . . ? C2C C3C C9C C8C 0.0(6) . . . . ? C8C C9C C10C C11C 178.8(4) . . . . ? C3C C9C C10C C11C -2.0(6) . . . . ? C9C C10C C11C C12C 1.0(7) . . . . ? C3C C4C C12C C11C -1.8(6) . . . . ? C5C C4C C12C C11C 178.2(3) . . . . ? C10C C11C C12C C4C 0.9(6) . . . . ? N1C C13C C14C C15C -45.6(4) . . . . ? C16C C13C C14C C15C -171.8(3) . . . . ? C13C C14C C15C O3C -43.0(5) . . . . ? C13C C14C C15C N2C 138.0(4) . . . . ? N1C C13C C16C O5C -162.3(3) . . . . ? C14C C13C C16C O5C -35.1(4) . . . . ? N1C C13C C16C O4C 18.7(4) . . . . ? C14C C13C C16C O4C 145.9(3) . . . . ? O1C C1C N1C C5C 174.5(3) . . . . ? C2C C1C N1C C5C -3.2(5) . . . . ? O1C C1C N1C C13C -1.5(5) . . . . ? C2C C1C N1C C13C -179.2(3) . . . . ? O2C C5C N1C C1C -174.9(3) . . . . ? C4C C5C N1C C1C 4.4(5) . . . . ? O2C C5C N1C C13C 1.1(5) . . . . ? C4C C5C N1C C13C -179.6(3) . . . . ? C16C C13C N1C C1C 62.4(4) . . . . ? C14C C13C N1C C1C -63.2(4) . . . . ? C16C C13C N1C C5C -113.9(3) . . . . ? C14C C13C N1C C5C 120.4(3) . . . . ? O5C C16C O4C Cu1 10.0(5) . . . . ? C13C C16C O4C Cu1 -171.1(2) . . . . ? O4B Cu1 O4C C16C -83.3(2) . . . . ? O4D Cu1 O4C C16C 70.9(2) . . . . ? N3 Cu1 O4C C16C 177.5(3) . . . . ? Cu2 Cu1 O4C C16C -6.6(2) . . . . ? O4C C16C O5C Cu2 -7.1(5) . . . . ? C13C C16C O5C Cu2 174.0(2) . . . . ? O5B Cu2 O5C C16C 90.1(3) . . . . ? O5D Cu2 O5C C16C -88.1(3) . . . . ? O5A Cu2 O5C C16C -1.8(4) . . . . ? O3E Cu2 O5C C16C 179.3(3) . . . . ? Cu1 Cu2 O5C C16C 1.1(3) . . . . ? O1D C1D C2D C6D 2.8(7) . . . . ? N1D C1D C2D C6D -177.7(4) . . . . ? O1D C1D C2D C3D -172.2(5) . . . . ? N1D C1D C2D C3D 7.2(7) . . . . ? C6D C2D C3D C4D 177.4(5) . . . . ? C1D C2D C3D C4D -7.6(7) . . . . ? C6D C2D C3D C9D -2.4(8) . . . . ? C1D C2D C3D C9D 172.5(5) . . . . ? C2D C3D C4D C12D 177.4(5) . . . . ? C9D C3D C4D C12D -2.8(8) . . . . ? C2D C3D C4D C5D 0.0(7) . . . . ? C9D C3D C4D C5D 179.8(5) . . . . ? C12D C4D C5D O2D 7.5(7) . . . . ? C3D C4D C5D O2D -175.1(5) . . . . ? C12D C4D C5D N1D -169.6(4) . . . . ? C3D C4D C5D N1D 7.8(7) . . . . ? C3D C2D C6D C7D -0.2(8) . . . . ? C1D C2D C6D C7D -175.3(5) . . . . ? C2D C6D C7D C8D 2.2(10) . . . . ? C6D C7D C8D C9D -1.4(12) . . . . ? C7D C8D C9D C3D -1.3(11) . . . . ? C7D C8D C9D C10D 176.2(7) . . . . ? C2D C3D C9D C8D 3.2(9) . . . . ? C4D C3D C9D C8D -176.7(6) . . . . ? C2D C3D C9D C10D -174.4(5) . . . . ? C4D C3D C9D C10D 5.7(8) . . . . ? C8D C9D C10D C11D 177.8(7) . . . . ? C3D C9D C10D C11D -4.7(10) . . . . ? C9D C10D C11D C12D 0.6(10) . . . . ? C3D C4D C12D C11D -1.4(8) . . . . ? C5D C4D C12D C11D 176.0(5) . . . . ? C10D C11D C12D C4D 2.5(9) . . . . ? N1D C13D C14D C15D -61.3(4) . . . . ? C16D C13D C14D C15D 173.6(3) . . . . ? C13D C14D C15D O3D 71.8(5) . . . . ? C13D C14D C15D N2D -107.9(4) . . . . ? N1D C13D C16D O4D 42.4(4) . . . . ? C14D C13D C16D O4D 169.3(3) . . . . ? N1D C13D C16D O5D -140.4(3) . . . . ? C14D C13D C16D O5D -13.5(4) . . . . ? O2D C5D N1D C1D 174.4(4) . . . . ? C4D C5D N1D C1D -8.4(6) . . . . ? O2D C5D N1D C13D -2.4(6) . . . . ? C4D C5D N1D C13D 174.8(4) . . . . ? O1D C1D N1D C5D -179.4(4) . . . . ? C2D C1D N1D C5D 1.1(6) . . . . ? O1D C1D N1D C13D -2.5(6) . . . . ? C2D C1D N1D C13D 178.0(4) . . . . ? C14D C13D N1D C5D 109.0(4) . . . . ? C16D C13D N1D C5D -124.8(4) . . . . ? C14D C13D N1D C1D -68.1(4) . . . . ? C16D C13D N1D C1D 58.1(4) . . . . ? O5D C16D O4D Cu1 5.3(5) . . . . ? C13D C16D O4D Cu1 -177.9(2) . . . . ? O4C Cu1 O4D C16D -90.8(3) . . . . ? O4A Cu1 O4D C16D 85.8(3) . . . . ? O4B Cu1 O4D C16D 0.1(4) . . . . ? N3 Cu1 O4D C16D 176.9(3) . . . . ? Cu2 Cu1 O4D C16D -3.0(2) . . . . ? O4D C16D O5D Cu2 -4.1(4) . . . . ? C13D C16D O5D Cu2 178.9(2) . . . . ? O5C Cu2 O5D C16D 79.7(2) . . . . ? O5A Cu2 O5D C16D -76.8(2) . . . . ? O3E Cu2 O5D C16D -175.3(2) . . . . ? Cu1 Cu2 O5D C16D 1.3(2) . . . . ? O1E C1E C2E C6E -1.7(6) . . . . ? N1E C1E C2E C6E 179.5(3) . . . . ? O1E C1E C2E C3E 177.9(3) . . . . ? N1E C1E C2E C3E -0.8(5) . . . . ? C6E C2E C3E C4E -179.6(4) . . . . ? C1E C2E C3E C4E 0.7(5) . . . . ? C6E C2E C3E C9E 0.3(5) . . . . ? C1E C2E C3E C9E -179.3(3) . . . . ? C9E C3E C4E C12E 0.2(5) . . . . ? C2E C3E C4E C12E -179.8(4) . . . . ? C9E C3E C4E C5E 179.0(3) . . . . ? C2E C3E C4E C5E -1.0(5) . . . . ? C12E C4E C5E O2E -1.0(5) . . . . ? C3E C4E C5E O2E -179.8(3) . . . . ? C12E C4E C5E N1E -179.7(3) . . . . ? C3E C4E C5E N1E 1.5(5) . . . . ? C3E C2E C6E C7E -0.2(6) . . . . ? C1E C2E C6E C7E 179.4(4) . . . . ? C2E C6E C7E C8E -0.4(7) . . . . ? C6E C7E C8E C9E 0.9(8) . . . . ? C7E C8E C9E C10E 179.5(5) . . . . ? C7E C8E C9E C3E -0.8(7) . . . . ? C4E C3E C9E C8E -179.9(4) . . . . ? C2E C3E C9E C8E 0.2(6) . . . . ? C4E C3E C9E C10E -0.1(6) . . . . ? C2E C3E C9E C10E 179.9(4) . . . . ? C8E C9E C10E C11E 179.4(5) . . . . ? C3E C9E C10E C11E -0.3(6) . . . . ? C9E C10E C11E C12E 0.6(7) . . . . ? C3E C4E C12E C11E 0.1(6) . . . . ? C5E C4E C12E C11E -178.7(4) . . . . ? C10E C11E C12E C4E -0.5(7) . . . . ? N1E C13E C14E C15E -158.3(3) . . . . ? C16E C13E C14E C15E 77.2(4) . . . . ? C13E C14E C15E O3E 167.8(3) . . . . ? C13E C14E C15E N2E -11.6(5) . . . . ? N1E C13E C16E O4E 37.3(4) . . . . ? C14E C13E C16E O4E 161.5(3) . . . . ? N1E C13E C16E O5E -146.3(3) . . . . ? C14E C13E C16E O5E -22.1(4) . . . . ? O2E C5E N1E C1E 179.6(3) . . . . ? C4E C5E N1E C1E -1.7(5) . . . . ? O2E C5E N1E C13E 3.1(5) . . . . ? C4E C5E N1E C13E -178.1(3) . . . . ? O1E C1E N1E C5E -177.4(3) . . . . ? C2E C1E N1E C5E 1.4(5) . . . . ? O1E C1E N1E C13E -0.9(4) . . . . ? C2E C1E N1E C13E 177.9(3) . . . . ? C16E C13E N1E C5E -130.6(3) . . . . ? C14E C13E N1E C5E 102.9(3) . . . . ? C16E C13E N1E C1E 52.6(4) . . . . ? C14E C13E N1E C1E -73.9(3) . . . . ? N2E C15E O3E Cu2 -14.5(5) . . . . ? C14E C15E O3E Cu2 166.1(2) . . . . ? O5B Cu2 O3E C15E -134.6(3) . . . . ? O5D Cu2 O3E C15E 43.4(3) . . . . ? O5C Cu2 O3E C15E 132.7(3) . . . . ? O5A Cu2 O3E C15E -46.8(3) . . . . ? O5E C16E O4E Cu3 0.4(4) . . . . ? C13E C16E O4E Cu3 176.4(2) . . . . ? O4H Cu3 O4E C16E -86.7(2) . . . . ? O4F Cu3 O4E C16E 75.4(2) . . . . ? O6 Cu3 O4E C16E 166.6(2) . . . . ? Cu4 Cu3 O4E C16E -2.0(2) . . . . ? O4E C16E O5E Cu4 2.6(5) . . . . ? C13E C16E O5E Cu4 -173.4(2) . . . . ? O5H Cu4 O5E C16E 79.4(3) . . . . ? O5F Cu4 O5E C16E -94.5(3) . . . . ? O5G Cu4 O5E C16E -5.9(5) . . . . ? O3A Cu4 O5E C16E 173.7(3) . . . . ? Cu3 Cu4 O5E C16E -3.0(3) . . . . ? O1F C1F C2F C6F -2.3(6) . . . . ? N1F C1F C2F C6F 178.6(4) . . . . ? O1F C1F C2F C3F 176.2(4) . . . . ? N1F C1F C2F C3F -2.9(5) . . . . ? C6F C2F C3F C4F 179.6(4) . . . . ? C1F C2F C3F C4F 1.1(6) . . . . ? C6F C2F C3F C9F 0.6(6) . . . . ? C1F C2F C3F C9F -177.8(4) . . . . ? C2F C3F C4F C12F 177.2(4) . . . . ? C9F C3F C4F C12F -3.9(6) . . . . ? C2F C3F C4F C5F -3.0(5) . . . . ? C9F C3F C4F C5F 176.0(3) . . . . ? C12F C4F C5F O2F 7.6(6) . . . . ? C3F C4F C5F O2F -172.3(4) . . . . ? C12F C4F C5F N1F -173.6(3) . . . . ? C3F C4F C5F N1F 6.6(5) . . . . ? C3F C2F C6F C7F -1.8(7) . . . . ? C1F C2F C6F C7F 176.6(4) . . . . ? C2F C6F C7F C8F 0.1(8) . . . . ? C6F C7F C8F C9F 2.9(8) . . . . ? C7F C8F C9F C10F 177.1(5) . . . . ? C7F C8F C9F C3F -4.0(7) . . . . ? C4F C3F C9F C10F 2.2(6) . . . . ? C2F C3F C9F C10F -178.8(4) . . . . ? C4F C3F C9F C8F -176.7(4) . . . . ? C2F C3F C9F C8F 2.3(6) . . . . ? C8F C9F C10F C11F -179.8(5) . . . . ? C3F C9F C10F C11F 1.4(7) . . . . ? C9F C10F C11F C12F -3.3(7) . . . . ? C3F C4F C12F C11F 2.0(6) . . . . ? C5F C4F C12F C11F -177.8(4) . . . . ? C10F C11F C12F C4F 1.6(6) . . . . ? N1F C13F C14F C15F -158.8(3) . . . . ? C16F C13F C14F C15F 73.1(4) . . . . ? C13F C14F C15F O3F 32.9(4) . . . . ? C13F C14F C15F N2F -151.5(3) . . . . ? N1F C13F C16F O4F 41.3(4) . . . . ? C14F C13F C16F O4F 168.7(3) . . . . ? N1F C13F C16F O5F -143.6(3) . . . . ? C14F C13F C16F O5F -16.2(4) . . . . ? O2F C5F N1F C1F 169.9(3) . . . . ? C4F C5F N1F C1F -9.0(5) . . . . ? O2F C5F N1F C13F -0.7(5) . . . . ? C4F C5F N1F C13F -179.6(3) . . . . ? O1F C1F N1F C5F -171.9(3) . . . . ? C2F C1F N1F C5F 7.2(5) . . . . ? O1F C1F N1F C13F -1.4(5) . . . . ? C2F C1F N1F C13F 177.8(3) . . . . ? C16F C13F N1F C5F -135.9(3) . . . . ? C14F C13F N1F C5F 94.1(3) . . . . ? C16F C13F N1F C1F 52.7(4) . . . . ? C14F C13F N1F C1F -77.3(4) . . . . ? O5F C16F O4F Cu3 -15.3(5) . . . . ? C13F C16F O4F Cu3 159.3(2) . . . . ? O4E Cu3 O4F C16F -83.5(3) . . . . ? O4G Cu3 O4F C16F 89.8(3) . . . . ? O4H Cu3 O4F C16F -7.2(5) . . . . ? O6 Cu3 O4F C16F -174.2(3) . . . . ? Cu4 Cu3 O4F C16F 8.3(2) . . . . ? O4F C16F O5F Cu4 11.8(4) . . . . ? C13F C16F O5F Cu4 -162.8(2) . . . . ? O5G Cu4 O5F C16F -88.6(2) . . . . ? O5E Cu4 O5F C16F 71.9(2) . . . . ? O3A Cu4 O5F C16F 168.6(2) . . . . ? Cu3 Cu4 O5F C16F -4.1(2) . . . . ? O1G C1G C2G C6G -2.1(5) . . . . ? N1G C1G C2G C6G 178.3(3) . . . . ? O1G C1G C2G C3G 178.7(3) . . . . ? N1G C1G C2G C3G -0.9(5) . . . . ? C6G C2G C3G C4G 179.9(3) . . . . ? C1G C2G C3G C4G -0.9(5) . . . . ? C6G C2G C3G C9G -0.5(5) . . . . ? C1G C2G C3G C9G 178.7(3) . . . . ? C9G C3G C4G C12G 0.2(5) . . . . ? C2G C3G C4G C12G 179.8(3) . . . . ? C9G C3G C4G C5G -178.3(3) . . . . ? C2G C3G C4G C5G 1.3(5) . . . . ? C12G C4G C5G O2G 1.5(5) . . . . ? C3G C4G C5G O2G -180.0(3) . . . . ? C12G C4G C5G N1G -178.4(3) . . . . ? C3G C4G C5G N1G 0.2(5) . . . . ? C3G C2G C6G C7G 0.3(6) . . . . ? C1G C2G C6G C7G -178.9(4) . . . . ? C2G C6G C7G C8G 0.3(6) . . . . ? C6G C7G C8G C9G -0.7(6) . . . . ? C7G C8G C9G C3G 0.4(6) . . . . ? C7G C8G C9G C10G -179.7(4) . . . . ? C4G C3G C9G C8G 179.7(4) . . . . ? C2G C3G C9G C8G 0.1(5) . . . . ? C4G C3G C9G C10G -0.2(5) . . . . ? C2G C3G C9G C10G -179.8(3) . . . . ? C8G C9G C10G C11G 179.8(4) . . . . ? C3G C9G C10G C11G -0.3(6) . . . . ? C9G C10G C11G C12G 0.6(6) . . . . ? C3G C4G C12G C11G 0.1(6) . . . . ? C5G C4G C12G C11G 178.7(4) . . . . ? C10G C11G C12G C4G -0.6(6) . . . . ? N1G C13G C14G C15G -162.0(3) . . . . ? C16G C13G C14G C15G 71.2(4) . . . . ? C13G C14G C15G O3G 16.4(5) . . . . ? C13G C14G C15G N2G -165.2(4) . . . . ? N1G C13G C16G O5G -135.8(3) . . . . ? C14G C13G C16G O5G -9.9(4) . . . . ? N1G C13G C16G O4G 49.1(4) . . . . ? C14G C13G C16G O4G 175.0(3) . . . . ? O1G C1G N1G C5G -177.1(3) . . . . ? C2G C1G N1G C5G 2.5(5) . . . . ? O1G C1G N1G C13G -5.9(5) . . . . ? C2G C1G N1G C13G 173.8(3) . . . . ? O2G C5G N1G C1G 177.9(3) . . . . ? C4G C5G N1G C1G -2.2(5) . . . . ? O2G C5G N1G C13G 6.6(5) . . . . ? C4G C5G N1G C13G -173.5(3) . . . . ? C14G C13G N1G C1G -73.0(4) . . . . ? C16G C13G N1G C1G 55.3(4) . . . . ? C14G C13G N1G C5G 98.9(3) . . . . ? C16G C13G N1G C5G -132.8(3) . . . . ? O5G C16G O4G Cu3 9.9(5) . . . . ? C13G C16G O4G Cu3 -175.6(2) . . . . ? O4H Cu3 O4G C16G 84.3(3) . . . . ? O4F Cu3 O4G C16G -77.5(3) . . . . ? O6 Cu3 O4G C16G -169.1(2) . . . . ? Cu4 Cu3 O4G C16G -0.7(2) . . . . ? O4G C16G O5G Cu4 -15.2(4) . . . . ? C13G C16G O5G Cu4 170.4(2) . . . . ? O5H Cu4 O5G C16G -72.6(2) . . . . ? O5F Cu4 O5G C16G 100.3(2) . . . . ? O5E Cu4 O5G C16G 13.0(4) . . . . ? O3A Cu4 O5G C16G -166.6(2) . . . . ? Cu3 Cu4 O5G C16G 10.2(2) . . . . ? O1H C1H C2H C6H 1.6(6) . . . . ? N1H C1H C2H C6H -177.4(3) . . . . ? O1H C1H C2H C3H 179.5(3) . . . . ? N1H C1H C2H C3H 0.5(5) . . . . ? C6H C2H C3H C4H -179.2(3) . . . . ? C1H C2H C3H C4H 2.9(5) . . . . ? C6H C2H C3H C9H -0.4(5) . . . . ? C1H C2H C3H C9H -178.3(3) . . . . ? C9H C3H C4H C12H 0.8(5) . . . . ? C2H C3H C4H C12H 179.7(3) . . . . ? C9H C3H C4H C5H -180.0(3) . . . . ? C2H C3H C4H C5H -1.1(5) . . . . ? C12H C4H C5H O2H -3.4(6) . . . . ? C3H C4H C5H O2H 177.3(4) . . . . ? C12H C4H C5H N1H 175.3(3) . . . . ? C3H C4H C5H N1H -3.9(5) . . . . ? C3H C2H C6H C7H 0.2(6) . . . . ? C1H C2H C6H C7H 178.1(4) . . . . ? C2H C6H C7H C8H 0.2(6) . . . . ? C6H C7H C8H C9H -0.4(6) . . . . ? C4H C3H C9H C10H -0.4(6) . . . . ? C2H C3H C9H C10H -179.2(3) . . . . ? C4H C3H C9H C8H 179.0(3) . . . . ? C2H C3H C9H C8H 0.2(5) . . . . ? C7H C8H C9H C10H 179.6(4) . . . . ? C7H C8H C9H C3H 0.2(6) . . . . ? C3H C9H C10H C11H -0.2(6) . . . . ? C8H C9H C10H C11H -179.6(4) . . . . ? C9H C10H C11H C12H 0.4(6) . . . . ? C10H C11H C12H C4H 0.0(6) . . . . ? C3H C4H C12H C11H -0.6(6) . . . . ? C5H C4H C12H C11H -179.9(4) . . . . ? N1H C13H C14H C15H -67.0(4) . . . . ? C16H C13H C14H C15H 166.5(3) . . . . ? C13H C14H C15H O3H -70.6(5) . . . . ? C13H C14H C15H N2H 109.9(4) . . . . ? N1H C13H C16H O4H 53.0(4) . . . . ? C14H C13H C16H O4H 179.9(3) . . . . ? N1H C13H C16H O5H -130.1(3) . . . . ? C14H C13H C16H O5H -3.2(4) . . . . ? O1H C1H N1H C5H 174.9(3) . . . . ? C2H C1H N1H C5H -6.1(5) . . . . ? O1H C1H N1H C13H -5.8(5) . . . . ? C2H C1H N1H C13H 173.2(3) . . . . ? O2H C5H N1H C1H -173.5(4) . . . . ? C4H C5H N1H C1H 7.7(5) . . . . ? O2H C5H N1H C13H 7.2(5) . . . . ? C4H C5H N1H C13H -171.6(3) . . . . ? C16H C13H N1H C1H 52.5(4) . . . . ? C14H C13H N1H C1H -74.9(4) . . . . ? C16H C13H N1H C5H -128.2(3) . . . . ? C14H C13H N1H C5H 104.4(4) . . . . ? O5H C16H O4H Cu3 0.3(5) . . . . ? C13H C16H O4H Cu3 176.8(2) . . . . ? O4E Cu3 O4H C16H 95.1(2) . . . . ? O4G Cu3 O4H C16H -79.8(2) . . . . ? O4F Cu3 O4H C16H 18.3(5) . . . . ? O6 Cu3 O4H C16H -175.2(2) . . . . ? Cu4 Cu3 O4H C16H 3.1(2) . . . . ? O4H C16H O5H Cu4 -5.7(5) . . . . ? C13H C16H O5H Cu4 177.7(2) . . . . ? O5G Cu4 O5H C16H 90.6(3) . . . . ? O5E Cu4 O5H C16H -70.0(3) . . . . ? O3A Cu4 O5H C16H -166.9(3) . . . . ? Cu3 Cu4 O5H C16H 5.9(2) . . . . ? N3 C21 C22 C23 -1.2(9) . . . . ? C21 C22 C23 C24 2.4(10) . . . . ? C22 C23 C24 C25 -1.4(9) . . . . ? C23 C24 C25 N3 -0.9(8) . . . . ? C22 C21 N3 C25 -1.1(7) . . . . ? C22 C21 N3 Cu1 174.4(4) . . . . ? C24 C25 N3 C21 2.1(6) . . . . ? C24 C25 N3 Cu1 -173.2(4) . . . . ? O4C Cu1 N3 C21 159.1(3) . . . . ? O4A Cu1 N3 C21 -21.8(3) . . . . ? O4B Cu1 N3 C21 68.5(3) . . . . ? O4D Cu1 N3 C21 -110.1(3) . . . . ? O4C Cu1 N3 C25 -25.7(3) . . . . ? O4A Cu1 N3 C25 153.4(3) . . . . ? O4B Cu1 N3 C25 -116.3(3) . . . . ? O4D Cu1 N3 C25 65.1(3) . . . . ? O4E Cu3 O6 C26 -32.7(4) . . . . ? O4G Cu3 O6 C26 151.2(4) . . . . ? O4H Cu3 O6 C26 -119.1(4) . . . . ? O4F Cu3 O6 C26 56.6(4) . . . . ? Cu4 Cu3 O6 C26 68.9(5) . . . . ? C32 C31 O10 C30 179.9(7) . . . . ? C29 C30 O10 C31 179.5(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2A H2A1 O5E 0.88 2.35 3.085(4) 141 . N2A H2A1 O5F 0.88 2.58 3.076(4) 117 . N2A H2A2 O3B 0.88 2.27 3.133(4) 165 . N2B H2B1 O3F 0.88 2.06 2.932(4) 170 . N2E H2E1 O5D 0.88 2.05 2.810(4) 144 . N2E H2E2 O1H 0.88 2.04 2.830(4) 148 . N2E H2E2 O5E 0.88 2.40 2.876(4) 114 . N2F H2F1 O3B 0.88 2.15 3.000(4) 164 . N2H H2H2 O3D 0.88 2.08 2.875(5) 149 . O6 H6M O7 0.83 1.85 2.673(4) 170 . N2C H2C1 O5F 0.88 2.36 3.047(4) 135 1_655 N2C H2C2 O3G 0.88 2.10 2.981(4) 177 1_655 N2D H2D1 O2G 0.88 2.35 2.888(4) 120 1_655 N2D H2D2 O8 0.88 2.37 3.232(6) 168 1_655 N2F H2F2 O3C 0.88 2.04 2.891(4) 161 1_455 N2G H2G1 O1C 0.88 2.02 2.895(5) 174 1_455 N2H H2H1 O10 0.88 2.08 2.915(5) 159 4_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.531 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.060 _vrf_PLAT602_5 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The voids contain heavily disordered solvent species, which could not be modeled and therefore were accounted for with the Squeeze program. ; #===END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C138 H103 Cu4 N17 O43, 3(C5 H10 O3) ' _chemical_formula_sum 'C153 H133 Cu4 N17 O52' _chemical_formula_weight 3295.92 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.1091(8) _cell_length_b 21.4458(12) _cell_length_c 52.381(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16972.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4043 _cell_measurement_theta_min 2.266 _cell_measurement_theta_max 15.533 _exptl_crystal_description 'rectangular bar' _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6808 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 167453 _diffrn_reflns_av_R_equivalents 0.2058 _diffrn_reflns_av_sigmaI/netI 0.2214 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 0.78 _diffrn_reflns_theta_max 22.59 _reflns_number_total 22429 _reflns_number_gt 9535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_number_reflns 22429 _refine_ls_number_parameters 850 _refine_ls_number_restraints 1351 _refine_ls_R_factor_all 0.1534 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2220 _refine_ls_wR_factor_gt 0.1940 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.854 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.96193(9) 0.41574(7) 0.30634(3) 0.0413(4) Uani 1 1 d D . . Cu2 Cu 0.92841(10) 0.40402(7) 0.35698(3) 0.0415(4) Uani 1 1 d . A . Cu3 Cu 0.55116(9) 0.54425(7) 0.45920(3) 0.0369(4) Uani 1 1 d . A . Cu4 Cu 0.57194(9) 0.51860(7) 0.41089(3) 0.0349(4) Uani 1 1 d D . . C1G C 0.4290(7) 0.7299(5) 0.4290(2) 0.048(4) Uiso 1 1 d D . . C2G C 0.4366(7) 0.7924(5) 0.4412(2) 0.055(4) Uiso 1 1 d D . . C3G C 0.3645(7) 0.8119(5) 0.4557(2) 0.049(4) Uiso 1 1 d D . . C4G C 0.2878(7) 0.7799(5) 0.4578(2) 0.053(4) Uiso 1 1 d D . . C5G C 0.2791(8) 0.7187(5) 0.4452(2) 0.061(4) Uiso 1 1 d D . . C6G C 0.5119(8) 0.8269(5) 0.4384(2) 0.055(4) Uiso 1 1 d D . . H6G H 0.5592 0.8129 0.4279 0.065 Uiso 1 1 calc R . . C7G C 0.5169(9) 0.8858(6) 0.4520(3) 0.071(5) Uiso 1 1 d D . . H7G H 0.5688 0.9107 0.4511 0.085 Uiso 1 1 calc R . . C8G C 0.4488(9) 0.9041(7) 0.4656(3) 0.093(5) Uiso 1 1 d D . . H8G H 0.4542 0.9437 0.4736 0.111 Uiso 1 1 calc R . . C9G C 0.3715(8) 0.8734(6) 0.4696(3) 0.066(4) Uiso 1 1 d D . . C10G C 0.2972(8) 0.8884(6) 0.4828(3) 0.077(5) Uiso 1 1 d D . . H10G H 0.2986 0.9277 0.4911 0.093 Uiso 1 1 calc R . . C11G C 0.2239(8) 0.8568(6) 0.4857(2) 0.057(4) Uiso 1 1 d D . . H11G H 0.1771 0.8724 0.4960 0.068 Uiso 1 1 calc R . . C12G C 0.2164(8) 0.7989(6) 0.4730(2) 0.066(4) Uiso 1 1 d D . . H12G H 0.1649 0.7739 0.4747 0.079 Uiso 1 1 calc R . . C13G C 0.3482(8) 0.6340(5) 0.4188(2) 0.041(3) Uiso 1 1 d D . . H13G H 0.2939 0.6129 0.4255 0.049 Uiso 1 1 calc R . . N1G N 0.3530(6) 0.6964(4) 0.43244(18) 0.045(3) Uiso 1 1 d D . . O1G O 0.4901(5) 0.7097(4) 0.41568(16) 0.054(2) Uiso 1 1 d D . . O2G O 0.2133(6) 0.6868(4) 0.44469(18) 0.072(3) Uiso 1 1 d D . . C14G C 0.3286(10) 0.6488(7) 0.3908(3) 0.066(4) Uiso 1 1 d . . . H14O H 0.2845 0.6829 0.3899 0.079 Uiso 1 1 calc R . . H14P H 0.3835 0.6634 0.3824 0.079 Uiso 1 1 calc R . . C15G C 0.2939(9) 0.5930(7) 0.3769(3) 0.061(4) Uiso 1 1 d . . . C16G C 0.4223(8) 0.5918(6) 0.4247(2) 0.043(3) Uiso 1 1 d . . . N2G N 0.3098(8) 0.5900(6) 0.3522(2) 0.092(4) Uiso 1 1 d . . . H2G1 H 0.2934 0.5570 0.3435 0.110 Uiso 1 1 calc R . . H2G2 H 0.3369 0.6210 0.3445 0.110 Uiso 1 1 calc R . . O3G O 0.2551(7) 0.5485(5) 0.38798(19) 0.079(3) Uiso 1 1 d . . . O4G O 0.4460(5) 0.5876(3) 0.44762(13) 0.040(2) Uiso 1 1 d . A . O5G O 0.4554(5) 0.5630(3) 0.40650(14) 0.038(2) Uiso 1 1 d . . . C1A C 0.6867(10) 0.3881(6) 0.2844(3) 0.0993(14) Uiso 1 1 d D A . C2A C 0.6777(7) 0.3626(6) 0.2578(2) 0.0993(14) Uiso 1 1 d D . . C3A C 0.6605(7) 0.4056(6) 0.2387(2) 0.0993(14) Uiso 1 1 d D . . C4A C 0.6493(11) 0.4670(6) 0.2426(2) 0.0993(14) Uiso 1 1 d D . . C5A C 0.6578(11) 0.4927(6) 0.2692(2) 0.0993(14) Uiso 1 1 d D A . C6A C 0.6851(11) 0.2986(7) 0.2553(3) 0.0993(14) Uiso 1 1 d D . . H6A H 0.6982 0.2722 0.2694 0.119 Uiso 1 1 calc R . . C7A C 0.6714(11) 0.2739(7) 0.2294(3) 0.0993(14) Uiso 1 1 d D . . H7A H 0.6665 0.2305 0.2261 0.119 Uiso 1 1 calc R . . C8A C 0.6664(11) 0.3150(7) 0.2114(3) 0.0993(14) Uiso 1 1 d D . . H8A H 0.6711 0.2980 0.1947 0.119 Uiso 1 1 calc R . . C9A C 0.6560(11) 0.3765(6) 0.2118(3) 0.0993(14) Uiso 1 1 d D . . C10A C 0.6355(10) 0.4217(7) 0.1968(3) 0.0993(14) Uiso 1 1 d D . . H10A H 0.6247 0.4080 0.1799 0.119 Uiso 1 1 calc R . . C11A C 0.6260(11) 0.4814(7) 0.1992(3) 0.0993(14) Uiso 1 1 d D . . H11A H 0.6133 0.5061 0.1846 0.119 Uiso 1 1 calc R . . C12A C 0.6344(10) 0.5095(7) 0.2230(3) 0.0993(14) Uiso 1 1 d D . . H12A H 0.6304 0.5532 0.2256 0.119 Uiso 1 1 calc R . . C16A C 0.7898(8) 0.4500(6) 0.3197(2) 0.043(3) Uiso 1 1 d D . . N1A N 0.6761(9) 0.4509(6) 0.2894(2) 0.0993(14) Uiso 1 1 d D . . O1A O 0.7032(7) 0.3512(5) 0.3016(2) 0.0993(14) Uiso 1 1 d D . . O2A O 0.6495(7) 0.5480(5) 0.2750(2) 0.0993(14) Uiso 1 1 d D . . O4A O 0.8456(5) 0.4498(4) 0.30175(16) 0.051(2) Uiso 1 1 d . A . O5A O 0.8126(5) 0.4389(4) 0.34326(14) 0.040(2) Uiso 1 1 d . A . C13A C 0.7000(7) 0.4697(6) 0.3150(2) 0.0417(17) Uiso 0.50 1 d PD A 3 H13A H 0.6953 0.5160 0.3167 0.050 Uiso 0.50 1 calc PR A 3 C14A C 0.6356(14) 0.4374(11) 0.3337(3) 0.0417(17) Uiso 0.50 1 d PD A 3 H14A H 0.5751 0.4493 0.3283 0.050 Uiso 0.50 1 calc PR A 3 H14B H 0.6411 0.3920 0.3307 0.050 Uiso 0.50 1 calc PR A 3 C15A C 0.6396(14) 0.4468(8) 0.3625(3) 0.0417(17) Uiso 0.50 1 d PD A 3 N2A N 0.6689(11) 0.3997(8) 0.3780(3) 0.0417(17) Uiso 0.50 1 d PD A 3 H2A1 H 0.6632 0.4029 0.3947 0.050 Uiso 0.50 1 calc PR A 3 H2A2 H 0.6935 0.3663 0.3713 0.050 Uiso 0.50 1 calc PR A 3 O3A O 0.6048(10) 0.4939(8) 0.3728(2) 0.0417(17) Uiso 0.50 1 d PD A 3 C13Z C 0.7000(7) 0.4697(6) 0.3150(2) 0.0417(17) Uiso 0.50 1 d PD A 4 H13Z H 0.7092 0.5154 0.3124 0.050 Uiso 0.50 1 calc PR A 4 C14Z C 0.6302(13) 0.4708(11) 0.3345(3) 0.0417(17) Uiso 0.50 1 d PD A 4 H14Z H 0.6183 0.4267 0.3389 0.050 Uiso 0.50 1 calc PR A 4 H14Y H 0.5764 0.4865 0.3259 0.050 Uiso 0.50 1 calc PR A 4 C15Z C 0.6363(12) 0.5051(9) 0.3594(3) 0.0417(17) Uiso 0.50 1 d PD A 4 N2Z N 0.7007(11) 0.5473(8) 0.3608(3) 0.0417(17) Uiso 0.50 1 d PD A 4 H2Z1 H 0.7008 0.5749 0.3732 0.050 Uiso 0.50 1 calc PR A 4 H2Z2 H 0.7431 0.5476 0.3493 0.050 Uiso 0.50 1 calc PR A 4 O3Z O 0.5701(10) 0.4928(8) 0.37196(18) 0.0417(17) Uiso 0.50 1 d PD A 4 C1B C 0.9871(8) 0.1950(7) 0.3126(3) 0.0788(12) Uiso 1 1 d D . . C2B C 1.0464(8) 0.1589(7) 0.2945(2) 0.0788(12) Uiso 1 1 d D . . C3B C 1.0051(8) 0.1276(7) 0.2751(3) 0.0788(12) Uiso 1 1 d D . . C4B C 0.9190(8) 0.1306(7) 0.2698(2) 0.0788(12) Uiso 1 1 d D . . C5B C 0.8560(8) 0.1654(7) 0.2878(2) 0.0788(12) Uiso 1 1 d D . . C6B C 1.1343(8) 0.1581(7) 0.2988(3) 0.0788(12) Uiso 1 1 d D . . H6B H 1.1597 0.1811 0.3124 0.095 Uiso 1 1 calc R . . C7B C 1.1902(9) 0.1198(7) 0.2814(3) 0.0788(12) Uiso 1 1 d D . . H7B H 1.2523 0.1155 0.2837 0.095 Uiso 1 1 calc R . . C8B C 1.1484(8) 0.0930(7) 0.2631(3) 0.0788(12) Uiso 1 1 d D . . H8B H 1.1856 0.0701 0.2519 0.095 Uiso 1 1 calc R . . C9B C 1.0643(8) 0.0911(7) 0.2568(2) 0.0788(12) Uiso 1 1 d D . . C10B C 1.0189(9) 0.0653(7) 0.2378(3) 0.0788(12) Uiso 1 1 d D . . H10B H 1.0532 0.0403 0.2265 0.095 Uiso 1 1 calc R . . C11B C 0.9374(9) 0.0687(6) 0.2322(2) 0.0788(12) Uiso 1 1 d D . . H11B H 0.9143 0.0497 0.2172 0.095 Uiso 1 1 calc R . . C12B C 0.8820(9) 0.1021(7) 0.2494(2) 0.0788(12) Uiso 1 1 d D . . H12B H 0.8199 0.1044 0.2466 0.095 Uiso 1 1 calc R . . C13B C 0.8446(10) 0.2387(7) 0.3244(3) 0.0788(12) Uiso 1 1 d D B . H13B H 0.7853 0.2445 0.3162 0.095 Uiso 1 1 calc R . . N1B N 0.8982(7) 0.1968(6) 0.3077(2) 0.0788(12) Uiso 1 1 d D . . O1B O 1.0196(6) 0.2215(5) 0.33077(19) 0.0788(12) Uiso 1 1 d D . . O2B O 0.7787(6) 0.1738(5) 0.28386(18) 0.0788(12) Uiso 1 1 d D . . C14B C 0.8315(9) 0.2040(6) 0.3490(2) 0.057(4) Uiso 1 1 d . . . H14C H 0.8865 0.2062 0.3592 0.068 Uiso 1 1 calc R . . H14D H 0.8194 0.1596 0.3453 0.068 Uiso 1 1 calc R . . C15B C 0.7511(10) 0.2327(7) 0.3651(3) 0.066(4) Uiso 1 1 d . . . C16B C 0.8860(8) 0.3014(6) 0.3275(2) 0.043(3) Uiso 1 1 d . . . N2B N 0.7611(8) 0.2321(6) 0.3889(2) 0.076(4) Uiso 1 1 d . . . H2B1 H 0.7234 0.2520 0.3988 0.091 Uiso 1 1 calc R . . H2B2 H 0.8059 0.2117 0.3957 0.091 Uiso 1 1 calc R . . O3B O 0.6895(7) 0.2604(5) 0.3544(2) 0.092(4) Uiso 1 1 d . . . O4B O 0.9136(5) 0.3286(3) 0.30763(14) 0.040(2) Uiso 1 1 d . B . O5B O 0.8851(5) 0.3221(4) 0.34994(15) 0.039(2) Uiso 1 1 d . A . C1C C 1.2567(11) 0.4452(6) 0.3125(3) 0.0982(16) Uiso 1 1 d D . . C2C C 1.3061(11) 0.4680(6) 0.2888(3) 0.0982(16) Uiso 1 1 d D . . C3C C 1.3471(11) 0.4213(6) 0.2747(3) 0.0982(16) Uiso 1 1 d D . . C4C C 1.3433(11) 0.3600(6) 0.2800(3) 0.0982(16) Uiso 1 1 d D . . C5C C 1.2876(11) 0.3362(6) 0.3015(3) 0.0982(16) Uiso 1 1 d D . . C6C C 1.3110(10) 0.5301(7) 0.2846(3) 0.0982(16) Uiso 1 1 d D . . H6C H 1.2838 0.5588 0.2960 0.118 Uiso 1 1 calc R . . C7C C 1.3605(11) 0.5523(7) 0.2615(3) 0.0982(16) Uiso 1 1 d D . . H7C H 1.3646 0.5949 0.2566 0.118 Uiso 1 1 calc R . . C8C C 1.3973(11) 0.5063(7) 0.2490(3) 0.0982(16) Uiso 1 1 d D . . H8C H 1.4322 0.5206 0.2351 0.118 Uiso 1 1 calc R . . C9C C 1.3981(11) 0.4446(7) 0.2509(3) 0.0982(16) Uiso 1 1 d D . . C10C C 1.4274(11) 0.3952(7) 0.2383(3) 0.0982(16) Uiso 1 1 d D . . H10C H 1.4574 0.4047 0.2228 0.118 Uiso 1 1 calc R . . C11C C 1.4223(11) 0.3372(7) 0.2432(3) 0.0982(16) Uiso 1 1 d D . . H11C H 1.4479 0.3088 0.2315 0.118 Uiso 1 1 calc R . . C12C C 1.3801(10) 0.3121(7) 0.2656(3) 0.0982(16) Uiso 1 1 d D . . H12C H 1.3777 0.2691 0.2699 0.118 Uiso 1 1 calc R . . C13C C 1.2021(11) 0.3618(8) 0.3406(3) 0.0982(16) Uiso 1 1 d D B . H13C H 1.2075 0.3154 0.3418 0.118 Uiso 1 1 calc R . . N1C N 1.2526(9) 0.3833(5) 0.3181(2) 0.0982(16) Uiso 1 1 d D . . O1C O 1.2154(7) 0.4823(5) 0.32542(19) 0.085(3) Uiso 1 1 d D . . O2C O 1.2766(7) 0.2835(5) 0.3072(2) 0.103(4) Uiso 1 1 d D . . C14C C 1.2327(8) 0.3905(7) 0.3663(3) 0.062(4) Uiso 1 1 d . . . H14E H 1.2151 0.4349 0.3671 0.074 Uiso 1 1 calc R . . H14F H 1.2045 0.3682 0.3807 0.074 Uiso 1 1 calc R . . C15C C 1.3346(9) 0.3847(7) 0.3682(3) 0.060(4) Uiso 1 1 d . . . C16C C 1.1050(8) 0.3782(6) 0.3358(2) 0.046(4) Uiso 1 1 d . . . N2C N 1.3756(8) 0.4346(6) 0.3756(2) 0.071(4) Uiso 1 1 d . . . H2C1 H 1.4336 0.4344 0.3772 0.085 Uiso 1 1 calc R . . H2C2 H 1.3455 0.4688 0.3789 0.085 Uiso 1 1 calc R . . O3C O 1.3693(7) 0.3364(5) 0.3632(2) 0.086(3) Uiso 1 1 d . . . O4C O 1.0779(5) 0.3856(4) 0.31395(15) 0.049(2) Uiso 1 1 d . B . O5C O 1.0560(5) 0.3773(4) 0.35570(15) 0.047(2) Uiso 1 1 d . A . C1D C 0.9055(7) 0.6295(6) 0.3228(2) 0.064(4) Uiso 1 1 d D . . C2D C 0.8775(7) 0.6708(5) 0.3016(2) 0.048(4) Uiso 1 1 d D . . C3D C 0.9394(7) 0.7048(6) 0.2884(2) 0.064(4) Uiso 1 1 d D . . C4D C 1.0255(8) 0.7051(6) 0.2951(2) 0.068(4) Uiso 1 1 d D . . C5D C 1.0567(9) 0.6666(7) 0.3169(3) 0.108(6) Uiso 1 1 d D . . C6D C 0.7894(8) 0.6690(7) 0.2953(3) 0.080(5) Uiso 1 1 d D . . H6D H 0.7488 0.6424 0.3038 0.097 Uiso 1 1 calc R . . C7D C 0.7620(10) 0.7108(8) 0.2747(3) 0.112(7) Uiso 1 1 d D . . H7D H 0.7011 0.7177 0.2713 0.135 Uiso 1 1 calc R . . C8D C 0.8228(9) 0.7383(8) 0.2612(3) 0.095(6) Uiso 1 1 d D . . H8D H 0.8029 0.7577 0.2459 0.114 Uiso 1 1 calc R . . C9D C 0.9106(8) 0.7431(6) 0.2660(2) 0.070(5) Uiso 1 1 d D . . C10D C 0.9786(8) 0.7706(6) 0.2532(3) 0.067(4) Uiso 1 1 d D . . H10D H 0.9633 0.7930 0.2381 0.080 Uiso 1 1 calc R . . C11D C 1.0618(10) 0.7696(7) 0.2592(3) 0.100(6) Uiso 1 1 d D . . H11D H 1.1044 0.7894 0.2486 0.120 Uiso 1 1 calc R . . C12D C 1.0883(9) 0.7382(7) 0.2819(3) 0.086(5) Uiso 1 1 d D . . H12D H 1.1478 0.7402 0.2877 0.104 Uiso 1 1 calc R . . C13D C 1.0238(9) 0.5848(6) 0.3482(2) 0.068(4) Uiso 1 1 d D B . H13D H 1.0900 0.5852 0.3486 0.082 Uiso 1 1 calc R . . N1D N 0.9945(6) 0.6289(5) 0.3291(2) 0.057(3) Uiso 1 1 d D . . O1D O 0.8559(6) 0.5940(4) 0.33409(17) 0.067(3) Uiso 1 1 d D . . O2D O 1.1328(8) 0.6670(6) 0.3250(2) 0.127(5) Uiso 1 1 d D . . C14D C 0.9870(11) 0.6057(8) 0.3759(3) 0.095(6) Uiso 1 1 d . . . H14G H 0.9216 0.6066 0.3753 0.114 Uiso 1 1 calc R . . H14H H 1.0048 0.5740 0.3886 0.114 Uiso 1 1 calc R . . C15D C 1.0194(14) 0.6672(10) 0.3844(4) 0.107(7) Uiso 1 1 d . . . C16D C 0.9935(8) 0.5196(6) 0.3427(2) 0.045(4) Uiso 1 1 d . . . N2D N 1.0916(10) 0.6635(7) 0.4009(3) 0.116(5) Uiso 1 1 d . . . H2D1 H 1.1125 0.6976 0.4081 0.139 Uiso 1 1 calc R . . H2D2 H 1.1164 0.6272 0.4041 0.139 Uiso 1 1 calc R . . O3D O 0.9847(10) 0.7140(7) 0.3796(3) 0.141(5) Uiso 1 1 d . . . O4D O 0.9974(5) 0.5028(4) 0.32006(15) 0.043(2) Uiso 1 1 d . B . O5D O 0.9719(5) 0.4869(4) 0.36132(15) 0.051(2) Uiso 1 1 d . A . C1E C 0.7299(7) 0.3828(5) 0.48725(19) 0.045(4) Uiso 1 1 d D . . C2E C 0.7377(8) 0.3513(6) 0.5128(2) 0.058(4) Uiso 1 1 d D . . C3E C 0.8080(8) 0.3676(6) 0.5286(2) 0.063(4) Uiso 1 1 d D . . C4E C 0.8720(8) 0.4072(7) 0.5217(2) 0.073(5) Uiso 1 1 d D . . C5E C 0.8677(8) 0.4382(6) 0.4968(2) 0.053(4) Uiso 1 1 d D . . C6E C 0.6760(9) 0.3094(6) 0.5199(2) 0.070(5) Uiso 1 1 d D . . H6E H 0.6296 0.2987 0.5085 0.084 Uiso 1 1 calc R . . C7E C 0.6800(10) 0.2798(8) 0.5456(3) 0.102(6) Uiso 1 1 d D . . H7E H 0.6357 0.2521 0.5516 0.122 Uiso 1 1 calc R . . C8E C 0.7482(10) 0.2948(8) 0.5588(3) 0.100(6) Uiso 1 1 d D . . H8E H 0.7533 0.2729 0.5746 0.120 Uiso 1 1 calc R . . C9E C 0.8130(10) 0.3354(7) 0.5545(3) 0.087(5) Uiso 1 1 d D . . C10E C 0.8853(10) 0.3520(8) 0.5681(3) 0.112(7) Uiso 1 1 d D . . H10E H 0.8904 0.3341 0.5846 0.135 Uiso 1 1 calc R . . C11E C 0.9485(11) 0.3893(7) 0.5614(3) 0.100(6) Uiso 1 1 d D . . H11E H 0.9978 0.3960 0.5723 0.121 Uiso 1 1 calc R . . C12E C 0.9427(9) 0.4197(7) 0.5375(3) 0.090(5) Uiso 1 1 d D . . H12E H 0.9871 0.4485 0.5324 0.108 Uiso 1 1 calc R . . C13E C 0.7908(8) 0.4489(6) 0.45451(19) 0.043(3) Uiso 1 1 d D A . H13E H 0.8369 0.4822 0.4537 0.051 Uiso 1 1 calc R . . N1E N 0.7968(6) 0.4215(4) 0.48006(16) 0.042(3) Uiso 1 1 d D . . O1E O 0.6705(5) 0.3693(4) 0.47200(15) 0.048(2) Uiso 1 1 d D . . O2E O 0.9227(6) 0.4740(4) 0.48841(17) 0.079(3) Uiso 1 1 d D . . C14E C 0.8181(10) 0.3990(7) 0.4350(3) 0.072(5) Uiso 1 1 d . . . H14I H 0.7647 0.3751 0.4301 0.087 Uiso 1 1 calc R . . H14J H 0.8592 0.3696 0.4435 0.087 Uiso 1 1 calc R . . C15E C 0.8629(13) 0.4234(10) 0.4104(4) 0.106(6) Uiso 1 1 d . B . C16E C 0.7040(8) 0.4802(6) 0.4499(2) 0.036(3) Uiso 1 1 d . . . N2E N 0.8620(10) 0.4849(8) 0.4066(3) 0.133(6) Uiso 1 1 d . . . H2E1 H 0.8852 0.5007 0.3925 0.159 Uiso 1 1 calc R . . H2E2 H 0.8383 0.5098 0.4181 0.159 Uiso 1 1 calc R . . O3E O 0.8922(6) 0.3940(4) 0.39605(18) 0.062(3) Uiso 1 1 d . . . O4E O 0.6643(5) 0.5045(4) 0.46775(14) 0.043(2) Uiso 1 1 d . A . O5E O 0.6821(5) 0.4808(4) 0.42622(14) 0.040(2) Uiso 1 1 d . A . C1F C 0.3245(8) 0.3771(7) 0.4564(3) 0.0796(12) Uiso 1 1 d D . . C2F C 0.2445(8) 0.3643(7) 0.4729(2) 0.0796(12) Uiso 1 1 d D . . C3F C 0.2580(8) 0.3346(7) 0.4957(2) 0.0796(12) Uiso 1 1 d D . . C4F C 0.3339(8) 0.3083(7) 0.5028(2) 0.0796(12) Uiso 1 1 d D . . C5F C 0.4127(8) 0.3128(7) 0.4855(2) 0.0796(12) Uiso 1 1 d D . . C6F C 0.1667(8) 0.3888(7) 0.4640(3) 0.0796(12) Uiso 1 1 d D . . H6F H 0.1623 0.4124 0.4487 0.096 Uiso 1 1 calc R . . C7F C 0.0894(9) 0.3744(7) 0.4808(3) 0.0796(12) Uiso 1 1 d D . . H7F H 0.0312 0.3875 0.4765 0.096 Uiso 1 1 calc R . . C8F C 0.1050(9) 0.3436(7) 0.5015(3) 0.0796(12) Uiso 1 1 d D . . H8F H 0.0525 0.3322 0.5103 0.096 Uiso 1 1 calc R . . C9F C 0.1773(8) 0.3243(7) 0.5131(3) 0.0796(12) Uiso 1 1 d D . . C10F C 0.1957(9) 0.2885(7) 0.5332(3) 0.0796(12) Uiso 1 1 d D . . H10F H 0.1464 0.2766 0.5434 0.096 Uiso 1 1 calc R . . C11F C 0.2707(9) 0.2680(7) 0.5407(3) 0.0796(12) Uiso 1 1 d D . . H11F H 0.2758 0.2486 0.5569 0.096 Uiso 1 1 calc R . . C12F C 0.3470(9) 0.2742(7) 0.5248(2) 0.0796(12) Uiso 1 1 d D . . H12F H 0.4025 0.2562 0.5291 0.096 Uiso 1 1 calc R . . C13F C 0.4760(9) 0.3550(7) 0.4453(3) 0.0796(12) Uiso 1 1 d D A . H13F H 0.5295 0.3382 0.4542 0.096 Uiso 1 1 calc R . . N1F N 0.4019(7) 0.3484(5) 0.4632(2) 0.0796(12) Uiso 1 1 d D . . O1F O 0.3212(6) 0.4078(5) 0.43682(19) 0.0796(12) Uiso 1 1 d D . . O2F O 0.4823(6) 0.2854(5) 0.48831(18) 0.0796(12) Uiso 1 1 d D . . C14F C 0.4613(8) 0.3143(6) 0.4219(2) 0.044(3) Uiso 1 1 d . . . H14K H 0.4343 0.2744 0.4273 0.053 Uiso 1 1 calc R . . H14L H 0.4190 0.3354 0.4103 0.053 Uiso 1 1 calc R . . C15F C 0.5463(10) 0.3009(6) 0.4074(3) 0.058(4) Uiso 1 1 d . . . C16F C 0.4935(7) 0.4236(6) 0.4405(2) 0.035(3) Uiso 1 1 d . . . N2F N 0.5395(9) 0.2943(5) 0.3821(2) 0.088(4) Uiso 1 1 d . . . H2F1 H 0.5866 0.2853 0.3730 0.105 Uiso 1 1 calc R . . H2F2 H 0.4878 0.2990 0.3746 0.105 Uiso 1 1 calc R . . O3F O 0.6193(6) 0.2943(4) 0.41780(16) 0.053(2) Uiso 1 1 d . . . O4F O 0.4959(5) 0.4605(4) 0.45781(15) 0.039(2) Uiso 1 1 d . A . O5F O 0.5194(5) 0.4379(3) 0.41746(14) 0.041(2) Uiso 1 1 d . A . C1H C 0.8300(7) 0.6477(5) 0.4434(2) 0.052(4) Uiso 1 1 d D . . C2H C 0.9126(7) 0.6501(5) 0.4590(2) 0.048(3) Uiso 1 1 d D . . C3H C 0.9245(7) 0.7030(5) 0.4743(2) 0.049(4) Uiso 1 1 d D . . C4H C 0.8635(7) 0.7491(5) 0.4763(2) 0.044(3) Uiso 1 1 d D . . C5H C 0.7792(7) 0.7458(5) 0.4619(2) 0.042(3) Uiso 1 1 d D . . C6H C 0.9755(7) 0.6054(6) 0.4559(2) 0.062(4) Uiso 1 1 d D . . H6H H 0.9666 0.5719 0.4443 0.074 Uiso 1 1 calc R . . C7H C 1.0575(9) 0.6099(6) 0.4710(3) 0.081(5) Uiso 1 1 d D . . H7H H 1.1021 0.5787 0.4700 0.097 Uiso 1 1 calc R . . C8H C 1.0664(9) 0.6591(6) 0.4859(3) 0.075(5) Uiso 1 1 d D . . H8H H 1.1197 0.6613 0.4954 0.090 Uiso 1 1 calc R . . C9H C 1.0094(8) 0.7065(6) 0.4893(3) 0.072(5) Uiso 1 1 d D . . C10H C 1.0148(9) 0.7578(6) 0.5047(3) 0.074(5) Uiso 1 1 d D . . H10H H 1.0661 0.7614 0.5151 0.089 Uiso 1 1 calc R . . C11H C 0.9569(8) 0.8018(6) 0.5064(2) 0.066(4) Uiso 1 1 d D . . H11H H 0.9685 0.8366 0.5171 0.079 Uiso 1 1 calc R . . C12H C 0.8766(8) 0.7991(5) 0.4927(2) 0.051(4) Uiso 1 1 d D . . H12H H 0.8328 0.8305 0.4947 0.061 Uiso 1 1 calc R . . C13H C 0.6944(8) 0.6935(6) 0.4265(2) 0.052(4) Uiso 1 1 d D A . H13H H 0.6527 0.7274 0.4318 0.062 Uiso 1 1 calc R . . N1H N 0.7712(6) 0.6963(4) 0.44447(17) 0.043(3) Uiso 1 1 d D . . O1H O 0.8153(5) 0.6032(4) 0.42897(15) 0.051(2) Uiso 1 1 d D . . O2H O 0.7182(6) 0.7830(4) 0.46331(17) 0.066(3) Uiso 1 1 d D . . C14H C 0.7231(10) 0.7083(7) 0.3985(3) 0.065(4) Uiso 1 1 d . . . H14M H 0.7745 0.6821 0.3938 0.078 Uiso 1 1 calc R . . H14N H 0.6740 0.6986 0.3867 0.078 Uiso 1 1 calc R . . C15H C 0.7468(13) 0.7740(10) 0.3963(3) 0.100(6) Uiso 1 1 d . . . C16H C 0.6431(8) 0.6304(6) 0.4295(2) 0.043(3) Uiso 1 1 d . . . N2H N 0.8320(10) 0.7881(7) 0.3903(3) 0.104(5) Uiso 1 1 d . . . H2H1 H 0.8495 0.8272 0.3900 0.124 Uiso 1 1 calc R . . H2H2 H 0.8697 0.7581 0.3867 0.124 Uiso 1 1 calc R . . O3H O 0.6943(8) 0.8193(6) 0.4014(2) 0.101(4) Uiso 1 1 d . . . O4H O 0.6216(5) 0.6195(4) 0.45234(15) 0.040(2) Uiso 1 1 d . A . O5H O 0.6294(4) 0.6009(3) 0.40981(14) 0.0330(19) Uiso 1 1 d . A . N3I N 0.9749(11) 0.4176(11) 0.26561(19) 0.056(2) Uiso 0.50 1 d PGD B 1 C21I C 0.9028(9) 0.4229(11) 0.2493(3) 0.056(2) Uiso 0.50 1 d PG B 1 H21I H 0.8445 0.4238 0.2560 0.067 Uiso 0.50 1 calc PR B 1 C22I C 0.9161(10) 0.4269(10) 0.2231(3) 0.056(2) Uiso 0.50 1 d PG B 1 H22I H 0.8668 0.4305 0.2119 0.067 Uiso 0.50 1 calc PR B 1 C23I C 1.0014(12) 0.4255(9) 0.21319(19) 0.056(2) Uiso 0.50 1 d PG B 1 H23I H 1.0105 0.4283 0.1953 0.067 Uiso 0.50 1 calc PR B 1 C24I C 1.0736(9) 0.4203(10) 0.2295(3) 0.056(2) Uiso 0.50 1 d PG B 1 H24I H 1.1319 0.4194 0.2228 0.067 Uiso 0.50 1 calc PR B 1 C25I C 1.0603(9) 0.4163(11) 0.2557(3) 0.056(2) Uiso 0.50 1 d PG B 1 H25I H 1.1096 0.4127 0.2669 0.067 Uiso 0.50 1 calc PR B 1 N3J N 1.0046(11) 0.4177(11) 0.2671(2) 0.056(2) Uiso 0.50 1 d PGD B 2 C21J C 0.9400(8) 0.4250(11) 0.2485(3) 0.056(2) Uiso 0.50 1 d PG B 2 H21J H 0.8791 0.4242 0.2531 0.067 Uiso 0.50 1 calc PR B 2 C22J C 0.9643(10) 0.4335(10) 0.2231(3) 0.056(2) Uiso 0.50 1 d PG B 2 H22J H 0.9202 0.4385 0.2104 0.067 Uiso 0.50 1 calc PR B 2 C23J C 1.0533(12) 0.4347(9) 0.2164(2) 0.056(2) Uiso 0.50 1 d PG B 2 H23J H 1.0700 0.4405 0.1991 0.067 Uiso 0.50 1 calc PR B 2 C24J C 1.1180(8) 0.4274(10) 0.2351(3) 0.056(2) Uiso 0.50 1 d PG B 2 H24J H 1.1788 0.4282 0.2305 0.067 Uiso 0.50 1 calc PR B 2 C25J C 1.0936(10) 0.4189(11) 0.2604(3) 0.056(2) Uiso 0.50 1 d PG B 2 H25J H 1.1378 0.4139 0.2732 0.067 Uiso 0.50 1 calc PR B 2 O36 O 0.5122(6) 0.5484(5) 0.50055(17) 0.069(3) Uiso 1 1 d D . . O37 O 0.4011(8) 0.4844(6) 0.5144(3) 0.148(5) Uiso 1 1 d D . . O38 O 0.6373(8) 0.4761(6) 0.5217(2) 0.126(5) Uiso 1 1 d D A . C31 C 0.4898(12) 0.5004(9) 0.5124(4) 0.120(7) Uiso 1 1 d D A . C32 C 0.3246(11) 0.5271(9) 0.5014(4) 0.132(8) Uiso 1 1 d D A . H32A H 0.3416 0.5717 0.5016 0.158 Uiso 1 1 calc R . . H32B H 0.3136 0.5141 0.4835 0.158 Uiso 1 1 calc R . . C33 C 0.2489(12) 0.5167(10) 0.5168(4) 0.154(9) Uiso 1 1 d D . . H33A H 0.2043 0.4938 0.5069 0.231 Uiso 1 1 calc R A . H33B H 0.2243 0.5568 0.5223 0.231 Uiso 1 1 calc R . . H33C H 0.2656 0.4922 0.5318 0.231 Uiso 1 1 calc R . . C34 C 0.5499(10) 0.4517(7) 0.5213(3) 0.095(5) Uiso 1 1 d D . . H34 H 0.5481 0.4166 0.5087 0.114 Uiso 1 1 calc R A . C35 C 0.5233(11) 0.4268(8) 0.5469(3) 0.118(7) Uiso 1 1 d D A . H35A H 0.5556 0.3880 0.5503 0.176 Uiso 1 1 calc R . . H35B H 0.4595 0.4184 0.5470 0.176 Uiso 1 1 calc R . . H35C H 0.5374 0.4575 0.5601 0.176 Uiso 1 1 calc R . . O46 O 0.6823(10) 0.7066(8) 0.6073(3) 0.166(6) Uiso 1 1 d D . . O47 O 0.5571(10) 0.6491(7) 0.6028(3) 0.165(6) Uiso 1 1 d D . . O48 O 0.6761(10) 0.6975(8) 0.6584(3) 0.182(7) Uiso 1 1 d D . . C41 C 0.6186(15) 0.6795(13) 0.6182(4) 0.207(13) Uiso 1 1 d D . . C42 C 0.5504(16) 0.6654(10) 0.5725(3) 0.166(9) Uiso 1 1 d D . . H42A H 0.5289 0.7085 0.5697 0.199 Uiso 1 1 calc R . . H42B H 0.6082 0.6601 0.5639 0.199 Uiso 1 1 calc R . . C43 C 0.4884(15) 0.6210(11) 0.5641(4) 0.176(10) Uiso 1 1 d D . . H43A H 0.5065 0.5795 0.5698 0.264 Uiso 1 1 calc R . . H43B H 0.4855 0.6218 0.5454 0.264 Uiso 1 1 calc R . . H43C H 0.4300 0.6310 0.5711 0.264 Uiso 1 1 calc R . . C44 C 0.6141(12) 0.6603(9) 0.6454(3) 0.140(8) Uiso 1 1 d D . . H44 H 0.6307 0.6154 0.6470 0.168 Uiso 1 1 calc R . . C45 C 0.5224(12) 0.6700(11) 0.6553(4) 0.183(11) Uiso 1 1 d D . . H45A H 0.5154 0.6478 0.6715 0.274 Uiso 1 1 calc R . . H45B H 0.4796 0.6538 0.6428 0.274 Uiso 1 1 calc R . . H45C H 0.5120 0.7146 0.6579 0.274 Uiso 1 1 calc R . . O56 O 0.7690(13) 0.5810(9) 0.6327(3) 0.230(3) Uiso 1 1 d D . . O57 O 0.8194(13) 0.5889(8) 0.5927(3) 0.230(3) Uiso 1 1 d D . . O58 O 0.8407(12) 0.6963(9) 0.6434(4) 0.230(3) Uiso 1 1 d D . . C51 C 0.8286(17) 0.6032(12) 0.6186(4) 0.230(3) Uiso 1 1 d D . . C52 C 0.7350(15) 0.5507(12) 0.5805(5) 0.230(3) Uiso 1 1 d D . . H52A H 0.6797 0.5574 0.5903 0.276 Uiso 1 1 calc R . . H52B H 0.7253 0.5606 0.5623 0.276 Uiso 1 1 calc R . . C53 C 0.7707(18) 0.4903(10) 0.5842(5) 0.230(3) Uiso 1 1 d D . . H53A H 0.8349 0.4933 0.5865 0.345 Uiso 1 1 calc R . . H53B H 0.7577 0.4644 0.5692 0.345 Uiso 1 1 calc R . . H53C H 0.7441 0.4713 0.5994 0.345 Uiso 1 1 calc R . . C54 C 0.8773(15) 0.6616(10) 0.6230(5) 0.230(3) Uiso 1 1 d D . . H54 H 0.8700 0.6874 0.6072 0.276 Uiso 1 1 calc R . . C55 C 0.9749(14) 0.6485(12) 0.6257(5) 0.230(3) Uiso 1 1 d D . . H55A H 1.0031 0.6826 0.6351 0.345 Uiso 1 1 calc R . . H55B H 1.0018 0.6450 0.6087 0.345 Uiso 1 1 calc R . . H55C H 0.9833 0.6093 0.6350 0.345 Uiso 1 1 calc R . . O66 O 0.5212(12) 0.7884(9) 0.3140(4) 0.230(3) Uiso 1 1 d D . . O67 O 0.6426(12) 0.7645(8) 0.3371(4) 0.230(3) Uiso 1 1 d D . . O68 O 0.4205(12) 0.7029(9) 0.3362(4) 0.230(3) Uiso 1 1 d D . . C61 C 0.5591(16) 0.7507(11) 0.3285(5) 0.230(3) Uiso 1 1 d D . . C62 C 0.7151(15) 0.8159(12) 0.3274(6) 0.230(3) Uiso 1 1 d D . . H62A H 0.7745 0.8082 0.3347 0.276 Uiso 1 1 calc R . . H62B H 0.7189 0.8177 0.3086 0.276 Uiso 1 1 calc R . . C63 C 0.6751(19) 0.8699(10) 0.3378(6) 0.230(3) Uiso 1 1 d D . . H63A H 0.6106 0.8650 0.3376 0.345 Uiso 1 1 calc R . . H63B H 0.6916 0.9063 0.3276 0.345 Uiso 1 1 calc R . . H63C H 0.6954 0.8757 0.3554 0.345 Uiso 1 1 calc R . . C64 C 0.5128(15) 0.6994(10) 0.3412(5) 0.230(3) Uiso 1 1 d D . . H64 H 0.5226 0.7028 0.3601 0.276 Uiso 1 1 calc R . . C65 C 0.5509(16) 0.6387(10) 0.3320(5) 0.230(3) Uiso 1 1 d D . . H65A H 0.5190 0.6040 0.3399 0.345 Uiso 1 1 calc R . . H65B H 0.6137 0.6365 0.3366 0.345 Uiso 1 1 calc R . . H65C H 0.5449 0.6362 0.3134 0.345 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0346(9) 0.0552(11) 0.0341(9) -0.0045(8) -0.0005(7) 0.0051(9) Cu2 0.0373(9) 0.0562(10) 0.0311(8) -0.0052(8) -0.0019(7) 0.0108(9) Cu3 0.0304(9) 0.0500(10) 0.0303(8) -0.0011(8) 0.0015(7) 0.0012(8) Cu4 0.0272(8) 0.0482(9) 0.0294(8) 0.0016(7) -0.0005(7) -0.0011(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O4C 1.910(8) . ? Cu1 O4A 1.918(8) . ? Cu1 O4B 2.008(8) . ? Cu1 O4D 2.071(8) . ? Cu1 N3I 2.143(10) . ? Cu1 N3J 2.152(10) . ? Cu1 Cu2 2.712(2) . ? Cu2 O5D 1.908(9) . ? Cu2 O5B 1.910(8) . ? Cu2 O5C 2.013(8) . ? Cu2 O5A 2.034(8) . ? Cu2 O3E 2.129(10) . ? Cu3 O4G 1.939(7) . ? Cu3 O4E 1.962(8) . ? Cu3 O4H 1.967(8) . ? Cu3 O4F 1.982(8) . ? Cu3 O36 2.246(9) . ? Cu3 Cu4 2.6088(19) . ? Cu4 O5F 1.935(8) . ? Cu4 O5H 1.967(7) . ? Cu4 O5G 2.016(8) . ? Cu4 O5E 2.018(8) . ? Cu4 O3Z 2.113(9) . ? Cu4 O3A 2.125(9) . ? C1G O1G 1.235(10) . ? C1G N1G 1.366(10) . ? C1G C2G 1.490(11) . ? C2G C6G 1.366(11) . ? C2G C3G 1.390(11) . ? C3G C4G 1.351(11) . ? C3G C9G 1.513(12) . ? C4G C12G 1.400(12) . ? C4G C5G 1.477(11) . ? C5G O2G 1.207(10) . ? C5G N1G 1.387(11) . ? C6G C7G 1.453(12) . ? C6G H6G 0.9500 . ? C7G C8G 1.312(12) . ? C7G H7G 0.9500 . ? C8G C9G 1.356(12) . ? C8G H8G 0.9500 . ? C9G C10G 1.356(12) . ? C10G C11G 1.307(12) . ? C10G H10G 0.9500 . ? C11G C12G 1.412(12) . ? C11G H11G 0.9500 . ? C12G H12G 0.9500 . ? C13G C16G 1.472(15) . ? C13G N1G 1.520(10) . ? C13G C14G 1.530(16) . ? C13G H13G 1.0000 . ? C14G C15G 1.494(18) . ? C14G H14O 0.9900 . ? C14G H14P 0.9900 . ? C15G O3G 1.262(15) . ? C15G N2G 1.318(16) . ? C16G O5G 1.242(12) . ? C16G O4G 1.254(12) . ? N2G H2G1 0.8800 . ? N2G H2G2 0.8800 . ? C1A O1A 1.222(11) . ? C1A N1A 1.380(12) . ? C1A C2A 1.505(12) . ? C2A C3A 1.383(12) . ? C2A C6A 1.385(12) . ? C3A C4A 1.343(12) . ? C3A C9A 1.542(13) . ? C4A C12A 1.389(12) . ? C4A C5A 1.505(12) . ? C5A O2A 1.231(12) . ? C5A N1A 1.415(12) . ? C6A C7A 1.471(13) . ? C6A H6A 0.9500 . ? C7A C8A 1.292(13) . ? C7A H7A 0.9500 . ? C8A C9A 1.329(12) . ? C8A H8A 0.9500 . ? C9A C10A 1.286(12) . ? C10A C11A 1.293(12) . ? C10A H10A 0.9500 . ? C11A C12A 1.391(13) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C16A O4A 1.264(13) . ? C16A O5A 1.303(12) . ? C16A C13A 1.442(15) . ? N1A C13A 1.445(15) . ? C13A C14A 1.546(13) . ? C13A H13A 1.0000 . ? C14A C15A 1.523(13) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A O3A 1.259(9) . ? C15A N2A 1.370(9) . ? N2A H2A1 0.8800 . ? N2A H2A2 0.8800 . ? C14Z C15Z 1.500(13) . ? C14Z H14Z 0.9900 . ? C14Z H14Y 0.9900 . ? C15Z O3Z 1.226(9) . ? C15Z N2Z 1.330(9) . ? N2Z H2Z1 0.8800 . ? N2Z H2Z2 0.8800 . ? C1B O1B 1.212(11) . ? C1B N1B 1.368(11) . ? C1B C2B 1.517(12) . ? C2B C6B 1.348(12) . ? C2B C3B 1.367(11) . ? C3B C4B 1.331(12) . ? C3B C9B 1.529(12) . ? C4B C12B 1.351(12) . ? C4B C5B 1.533(12) . ? C5B O2B 1.199(11) . ? C5B N1B 1.396(11) . ? C6B C7B 1.489(12) . ? C6B H6B 0.9500 . ? C7B C8B 1.284(12) . ? C7B H7B 0.9500 . ? C8B C9B 1.313(12) . ? C8B H8B 0.9500 . ? C9B C10B 1.329(12) . ? C10B C11B 1.267(12) . ? C10B H10B 0.9500 . ? C11B C12B 1.425(12) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B N1B 1.492(12) . ? C13B C16B 1.492(18) . ? C13B C14B 1.503(18) . ? C13B H13B 1.0000 . ? C14B C15B 1.604(18) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B O3B 1.238(15) . ? C15B N2B 1.253(16) . ? C16B O5B 1.256(13) . ? C16B O4B 1.265(13) . ? N2B H2B1 0.8800 . ? N2B H2B2 0.8800 . ? C1C O1C 1.217(11) . ? C1C N1C 1.361(12) . ? C1C C2C 1.529(12) . ? C2C C6C 1.350(12) . ? C2C C3C 1.389(12) . ? C3C C4C 1.343(12) . ? C3C C9C 1.548(13) . ? C4C C12C 1.391(13) . ? C4C C5C 1.496(12) . ? C5C O2C 1.182(11) . ? C5C N1C 1.435(12) . ? C6C C7C 1.500(13) . ? C6C H6C 0.9500 . ? C7C C8C 1.309(13) . ? C7C H7C 0.9500 . ? C8C C9C 1.325(12) . ? C8C H8C 0.9500 . ? C9C C10C 1.327(12) . ? C10C C11C 1.274(12) . ? C10C H10C 0.9500 . ? C11C C12C 1.437(13) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C N1C 1.478(12) . ? C13C C16C 1.530(19) . ? C13C C14C 1.549(19) . ? C13C H13C 1.0000 . ? C14C C15C 1.548(18) . ? C14C H14E 0.9900 . ? C14C H14F 0.9900 . ? C15C O3C 1.189(15) . ? C15C N2C 1.296(16) . ? C16C O4C 1.225(13) . ? C16C O5C 1.279(13) . ? N2C H2C1 0.8800 . ? N2C H2C2 0.8800 . ? C1D O1D 1.221(10) . ? C1D N1D 1.383(11) . ? C1D C2D 1.483(11) . ? C2D C3D 1.372(11) . ? C2D C6D 1.372(12) . ? C3D C4D 1.347(11) . ? C3D C9D 1.497(12) . ? C4D C12D 1.374(12) . ? C4D C5D 1.488(12) . ? C5D O2D 1.226(12) . ? C5D N1D 1.393(12) . ? C6D C7D 1.462(13) . ? C6D H6D 0.9500 . ? C7D C8D 1.301(13) . ? C7D H7D 0.9500 . ? C8D C9D 1.355(12) . ? C8D H8D 0.9500 . ? C9D C10D 1.362(12) . ? C10D C11D 1.296(12) . ? C10D H10D 0.9500 . ? C11D C12D 1.424(13) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D N1D 1.446(11) . ? C13D C16D 1.500(17) . ? C13D C14D 1.619(19) . ? C13D H13D 1.0000 . ? C14D C15D 1.48(2) . ? C14D H14G 0.9900 . ? C14D H14H 0.9900 . ? C15D O3D 1.16(2) . ? C15D N2D 1.40(2) . ? C16D O4D 1.241(13) . ? C16D O5D 1.244(13) . ? N2D H2D1 0.8800 . ? N2D H2D2 0.8800 . ? C1E O1E 1.235(10) . ? C1E N1E 1.361(10) . ? C1E C2E 1.505(11) . ? C2E C6E 1.347(12) . ? C2E C3E 1.390(11) . ? C3E C4E 1.337(11) . ? C3E C9E 1.527(12) . ? C4E C12E 1.377(12) . ? C4E C5E 1.466(11) . ? C5E O2E 1.213(10) . ? C5E N1E 1.430(10) . ? C6E C7E 1.486(13) . ? C6E H6E 0.9500 . ? C7E C8E 1.285(13) . ? C7E H7E 0.9500 . ? C8E C9E 1.329(12) . ? C8E H8E 0.9500 . ? C9E C10E 1.350(13) . ? C10E C11E 1.293(13) . ? C10E H10E 0.9500 . ? C11E C12E 1.414(12) . ? C11E H11E 0.9500 . ? C12E H12E 0.9500 . ? C13E N1E 1.464(10) . ? C13E C16E 1.493(15) . ? C13E C14E 1.533(17) . ? C13E H13E 1.0000 . ? C14E C15E 1.55(2) . ? C14E H14I 0.9900 . ? C14E H14J 0.9900 . ? C15E O3E 1.07(2) . ? C15E N2E 1.33(2) . ? C16E O4E 1.226(12) . ? C16E O5E 1.286(12) . ? N2E H2E1 0.8800 . ? N2E H2E2 0.8800 . ? C1F O1F 1.220(11) . ? C1F N1F 1.367(11) . ? C1F C2F 1.512(12) . ? C2F C3F 1.367(12) . ? C2F C6F 1.370(12) . ? C3F C4F 1.332(12) . ? C3F C9F 1.539(12) . ? C4F C12F 1.379(12) . ? C4F C5F 1.499(12) . ? C5F O2F 1.214(11) . ? C5F N1F 1.408(11) . ? C6F C7F 1.495(12) . ? C6F H6F 0.9500 . ? C7F C8F 1.291(12) . ? C7F H7F 0.9500 . ? C8F C9F 1.317(12) . ? C8F H8F 0.9500 . ? C9F C10F 1.334(12) . ? C10F C11F 1.276(12) . ? C10F H10F 0.9500 . ? C11F C12F 1.428(12) . ? C11F H11F 0.9500 . ? C12F H12F 0.9500 . ? C13F N1F 1.465(11) . ? C13F C16F 1.516(18) . ? C13F C14F 1.523(17) . ? C13F H13F 1.0000 . ? C14F C15F 1.519(17) . ? C14F H14K 0.9900 . ? C14F H14L 0.9900 . ? C15F O3F 1.238(14) . ? C15F N2F 1.335(15) . ? C16F O4F 1.205(12) . ? C16F O5F 1.304(12) . ? N2F H2F1 0.8800 . ? N2F H2F2 0.8800 . ? C1H O1H 1.237(10) . ? C1H N1H 1.370(10) . ? C1H C2H 1.492(11) . ? C2H C6H 1.360(11) . ? C2H C3H 1.400(11) . ? C3H C4H 1.356(11) . ? C3H C9H 1.507(12) . ? C4H C12H 1.388(11) . ? C4H C5H 1.485(11) . ? C5H O2H 1.221(10) . ? C5H N1H 1.405(10) . ? C6H C7H 1.473(12) . ? C6H H6H 0.9500 . ? C7H C8H 1.321(12) . ? C7H H7H 0.9500 . ? C8H C9H 1.343(12) . ? C8H H8H 0.9500 . ? C9H C10H 1.366(12) . ? C10H C11H 1.290(12) . ? C10H H10H 0.9500 . ? C11H C12H 1.411(12) . ? C11H H11H 0.9500 . ? C12H H12H 0.9500 . ? C13H N1H 1.495(11) . ? C13H C14H 1.559(17) . ? C13H C16H 1.568(17) . ? C13H H13H 1.0000 . ? C14H C15H 1.46(2) . ? C14H H14M 0.9900 . ? C14H H14N 0.9900 . ? C15H O3H 1.28(2) . ? C15H N2H 1.36(2) . ? C16H O5H 1.229(13) . ? C16H O4H 1.261(13) . ? N2H H2H1 0.8800 . ? N2H H2H2 0.8800 . ? N3I C21I 1.3900 . ? N3I C25I 1.3900 . ? C21I C22I 1.3900 . ? C21I H21I 0.9500 . ? C22I C23I 1.3900 . ? C22I H22I 0.9500 . ? C23I C24I 1.3900 . ? C23I H23I 0.9500 . ? C24I C25I 1.3900 . ? C24I H24I 0.9500 . ? C25I H25I 0.9500 . ? N3J C21J 1.3900 . ? N3J C25J 1.3900 . ? C21J C22J 1.3900 . ? C21J H21J 0.9500 . ? C22J C23J 1.3900 . ? C22J H22J 0.9500 . ? C23J C24J 1.3900 . ? C23J H23J 0.9500 . ? C24J C25J 1.3900 . ? C24J H24J 0.9500 . ? C25J H25J 0.9500 . ? O36 C31 1.249(16) . ? O37 C31 1.387(16) . ? O37 C32 1.624(15) . ? O38 C34 1.420(14) . ? C31 C34 1.459(17) . ? C32 C33 1.419(16) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.498(15) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O46 C41 1.261(17) . ? O47 C41 1.389(17) . ? O47 C42 1.631(15) . ? O48 C44 1.406(15) . ? C41 C44 1.486(18) . ? C42 C43 1.407(16) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.493(16) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? O56 C51 1.258(18) . ? O57 C51 1.399(17) . ? O57 C52 1.644(16) . ? O58 C54 1.417(16) . ? C51 C54 1.470(18) . ? C52 C53 1.418(17) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.509(17) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? O66 C61 1.247(17) . ? O67 C61 1.372(17) . ? O67 C62 1.633(16) . ? O68 C64 1.421(16) . ? C61 C64 1.466(18) . ? C62 C63 1.415(17) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.503(17) . ? C64 H64 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4C Cu1 O4A 174.7(3) . . ? O4C Cu1 O4B 90.6(3) . . ? O4A Cu1 O4B 91.4(3) . . ? O4C Cu1 O4D 89.8(3) . . ? O4A Cu1 O4D 86.4(3) . . ? O4B Cu1 O4D 157.2(3) . . ? O4C Cu1 N3I 97.5(5) . . ? O4A Cu1 N3I 87.2(6) . . ? O4B Cu1 N3I 94.8(7) . . ? O4D Cu1 N3I 107.7(7) . . ? O4C Cu1 N3J 86.0(5) . . ? O4A Cu1 N3J 98.5(5) . . ? O4B Cu1 N3J 99.2(7) . . ? O4D Cu1 N3J 103.6(7) . . ? N3I Cu1 N3J 12.2(7) . . ? O4C Cu1 Cu2 86.3(2) . . ? O4A Cu1 Cu2 89.3(3) . . ? O4B Cu1 Cu2 79.2(2) . . ? O4D Cu1 Cu2 78.0(2) . . ? N3I Cu1 Cu2 173.0(5) . . ? N3J Cu1 Cu2 172.2(5) . . ? O5D Cu2 O5B 175.7(3) . . ? O5D Cu2 O5C 86.5(3) . . ? O5B Cu2 O5C 93.4(3) . . ? O5D Cu2 O5A 89.8(3) . . ? O5B Cu2 O5A 88.6(3) . . ? O5C Cu2 O5A 156.5(3) . . ? O5D Cu2 O3E 93.9(4) . . ? O5B Cu2 O3E 90.3(3) . . ? O5C Cu2 O3E 104.4(3) . . ? O5A Cu2 O3E 99.0(3) . . ? O5D Cu2 Cu1 88.1(3) . . ? O5B Cu2 Cu1 87.7(2) . . ? O5C Cu2 Cu1 79.3(2) . . ? O5A Cu2 Cu1 77.3(2) . . ? O3E Cu2 Cu1 175.8(3) . . ? O4G Cu3 O4E 173.8(3) . . ? O4G Cu3 O4H 89.6(3) . . ? O4E Cu3 O4H 85.8(3) . . ? O4G Cu3 O4F 94.5(3) . . ? O4E Cu3 O4F 89.0(3) . . ? O4H Cu3 O4F 164.8(3) . . ? O4G Cu3 O36 93.9(3) . . ? O4E Cu3 O36 91.4(3) . . ? O4H Cu3 O36 106.6(3) . . ? O4F Cu3 O36 87.8(3) . . ? O4G Cu3 Cu4 84.1(2) . . ? O4E Cu3 Cu4 91.4(2) . . ? O4H Cu3 Cu4 86.0(2) . . ? O4F Cu3 Cu4 79.9(2) . . ? O36 Cu3 Cu4 167.3(3) . . ? O5F Cu4 O5H 171.2(3) . . ? O5F Cu4 O5G 94.8(3) . . ? O5H Cu4 O5G 87.6(3) . . ? O5F Cu4 O5E 84.8(3) . . ? O5H Cu4 O5E 90.4(3) . . ? O5G Cu4 O5E 162.9(3) . . ? O5F Cu4 O3Z 86.1(5) . . ? O5H Cu4 O3Z 102.3(5) . . ? O5G Cu4 O3Z 90.1(5) . . ? O5E Cu4 O3Z 106.8(5) . . ? O5F Cu4 O3A 92.3(5) . . ? O5H Cu4 O3A 95.3(5) . . ? O5G Cu4 O3A 102.4(5) . . ? O5E Cu4 O3A 94.7(5) . . ? O3Z Cu4 O3A 14.3(6) . . ? O5F Cu4 Cu3 88.1(2) . . ? O5H Cu4 Cu3 83.8(2) . . ? O5G Cu4 Cu3 84.6(2) . . ? O5E Cu4 Cu3 78.3(2) . . ? O3Z Cu4 Cu3 171.8(4) . . ? O3A Cu4 Cu3 172.9(4) . . ? O1G C1G N1G 121.2(9) . . ? O1G C1G C2G 120.0(9) . . ? N1G C1G C2G 118.7(9) . . ? C6G C2G C3G 123.4(10) . . ? C6G C2G C1G 120.3(9) . . ? C3G C2G C1G 116.3(9) . . ? C4G C3G C2G 124.5(9) . . ? C4G C3G C9G 117.5(9) . . ? C2G C3G C9G 118.0(9) . . ? C3G C4G C12G 124.1(10) . . ? C3G C4G C5G 119.3(9) . . ? C12G C4G C5G 116.4(10) . . ? O2G C5G N1G 117.1(10) . . ? O2G C5G C4G 126.0(10) . . ? N1G C5G C4G 116.8(9) . . ? C2G C6G C7G 117.3(10) . . ? C2G C6G H6G 121.3 . . ? C7G C6G H6G 121.3 . . ? C8G C7G C6G 119.2(12) . . ? C8G C7G H7G 120.4 . . ? C6G C7G H7G 120.4 . . ? C7G C8G C9G 127.9(13) . . ? C7G C8G H8G 116.1 . . ? C9G C8G H8G 116.1 . . ? C10G C9G C8G 132.6(12) . . ? C10G C9G C3G 113.2(10) . . ? C8G C9G C3G 114.1(10) . . ? C11G C10G C9G 129.6(13) . . ? C11G C10G H10G 115.2 . . ? C9G C10G H10G 115.2 . . ? C10G C11G C12G 118.0(12) . . ? C10G C11G H11G 121.0 . . ? C12G C11G H11G 121.0 . . ? C4G C12G C11G 117.4(11) . . ? C4G C12G H12G 121.3 . . ? C11G C12G H12G 121.3 . . ? C16G C13G N1G 114.0(9) . . ? C16G C13G C14G 118.5(10) . . ? N1G C13G C14G 106.1(9) . . ? C16G C13G H13G 105.8 . . ? N1G C13G H13G 105.8 . . ? C14G C13G H13G 105.8 . . ? C1G N1G C5G 124.0(9) . . ? C1G N1G C13G 116.2(8) . . ? C5G N1G C13G 119.5(9) . . ? C15G C14G C13G 111.5(11) . . ? C15G C14G H14O 109.3 . . ? C13G C14G H14O 109.3 . . ? C15G C14G H14P 109.3 . . ? C13G C14G H14P 109.3 . . ? H14O C14G H14P 108.0 . . ? O3G C15G N2G 119.9(14) . . ? O3G C15G C14G 123.1(13) . . ? N2G C15G C14G 116.9(14) . . ? O5G C16G O4G 125.8(11) . . ? O5G C16G C13G 116.7(10) . . ? O4G C16G C13G 117.6(11) . . ? C15G N2G H2G1 120.0 . . ? C15G N2G H2G2 120.0 . . ? H2G1 N2G H2G2 120.0 . . ? C16G O4G Cu3 124.6(8) . . ? C16G O5G Cu4 119.9(7) . . ? O1A C1A N1A 121.0(12) . . ? O1A C1A C2A 117.7(12) . . ? N1A C1A C2A 121.2(11) . . ? C3A C2A C6A 127.4(12) . . ? C3A C2A C1A 116.4(11) . . ? C6A C2A C1A 116.1(11) . . ? C4A C3A C2A 124.7(12) . . ? C4A C3A C9A 121.8(11) . . ? C2A C3A C9A 113.5(11) . . ? C3A C4A C12A 123.6(12) . . ? C3A C4A C5A 119.1(11) . . ? C12A C4A C5A 117.2(11) . . ? O2A C5A N1A 116.4(12) . . ? O2A C5A C4A 125.0(12) . . ? N1A C5A C4A 118.6(11) . . ? C2A C6A C7A 115.6(12) . . ? C2A C6A H6A 122.2 . . ? C7A C6A H6A 122.2 . . ? C8A C7A C6A 115.9(14) . . ? C8A C7A H7A 122.0 . . ? C6A C7A H7A 122.0 . . ? C7A C8A C9A 132.1(15) . . ? C7A C8A H8A 114.0 . . ? C9A C8A H8A 114.0 . . ? C10A C9A C8A 140.0(15) . . ? C10A C9A C3A 105.3(12) . . ? C8A C9A C3A 114.3(12) . . ? C9A C10A C11A 135.5(15) . . ? C9A C10A H10A 112.2 . . ? C11A C10A H10A 112.2 . . ? C10A C11A C12A 120.3(14) . . ? C10A C11A H11A 119.9 . . ? C12A C11A H11A 119.9 . . ? C4A C12A C11A 113.1(12) . . ? C4A C12A H12A 123.5 . . ? C11A C12A H12A 123.5 . . ? O4A C16A O5A 121.8(11) . . ? O4A C16A C13A 120.1(11) . . ? O5A C16A C13A 117.7(11) . . ? C1A N1A C5A 119.9(11) . . ? C1A N1A C13A 114.8(11) . . ? C5A N1A C13A 124.4(11) . . ? C16A O4A Cu1 121.3(8) . . ? C16A O5A Cu2 129.0(8) . . ? C16A C13A N1A 108.2(10) . . ? C16A C13A C14A 110.6(13) . . ? N1A C13A C14A 107.8(11) . . ? C16A C13A H13A 110.1 . . ? N1A C13A H13A 110.1 . . ? C14A C13A H13A 110.1 . . ? C15A C14A C13A 123.0(15) . . ? C15A C14A H14A 106.6 . . ? C13A C14A H14A 106.6 . . ? C15A C14A H14B 106.6 . . ? C13A C14A H14B 106.6 . . ? H14A C14A H14B 106.6 . . ? O3A C15A N2A 118.2(15) . . ? O3A C15A C14A 120.8(15) . . ? N2A C15A C14A 120.2(16) . . ? C15A N2A H2A1 120.0 . . ? C15A N2A H2A2 120.0 . . ? H2A1 N2A H2A2 120.0 . . ? C15A O3A Cu4 134.3(12) . . ? C15Z C14Z H14Z 106.2 . . ? C15Z C14Z H14Y 106.2 . . ? H14Z C14Z H14Y 106.4 . . ? O3Z C15Z N2Z 135.5(16) . . ? O3Z C15Z C14Z 108.2(12) . . ? N2Z C15Z C14Z 115.2(15) . . ? C15Z N2Z H2Z1 120.0 . . ? C15Z N2Z H2Z2 120.0 . . ? H2Z1 N2Z H2Z2 120.0 . . ? C15Z O3Z Cu4 116.8(11) . . ? O1B C1B N1B 122.1(11) . . ? O1B C1B C2B 119.4(11) . . ? N1B C1B C2B 118.4(10) . . ? C6B C2B C3B 124.6(11) . . ? C6B C2B C1B 118.9(11) . . ? C3B C2B C1B 116.5(10) . . ? C4B C3B C2B 125.2(11) . . ? C4B C3B C9B 117.7(10) . . ? C2B C3B C9B 116.8(10) . . ? C3B C4B C12B 123.2(11) . . ? C3B C4B C5B 120.1(11) . . ? C12B C4B C5B 116.6(11) . . ? O2B C5B N1B 120.0(11) . . ? O2B C5B C4B 124.9(11) . . ? N1B C5B C4B 114.2(10) . . ? C2B C6B C7B 117.7(11) . . ? C2B C6B H6B 121.2 . . ? C7B C6B H6B 121.2 . . ? C8B C7B C6B 115.0(12) . . ? C8B C7B H7B 122.5 . . ? C6B C7B H7B 122.5 . . ? C7B C8B C9B 132.8(14) . . ? C7B C8B H8B 113.6 . . ? C9B C8B H8B 113.6 . . ? C8B C9B C10B 134.5(13) . . ? C8B C9B C3B 113.0(11) . . ? C10B C9B C3B 112.4(11) . . ? C11B C10B C9B 130.5(14) . . ? C11B C10B H10B 114.8 . . ? C9B C10B H10B 114.8 . . ? C10B C11B C12B 117.1(13) . . ? C10B C11B H11B 121.5 . . ? C12B C11B H11B 121.5 . . ? C4B C12B C11B 118.9(12) . . ? C4B C12B H12B 120.5 . . ? C11B C12B H12B 120.5 . . ? N1B C13B C16B 112.3(12) . . ? N1B C13B C14B 106.0(12) . . ? C16B C13B C14B 113.9(12) . . ? N1B C13B H13B 108.1 . . ? C16B C13B H13B 108.1 . . ? C14B C13B H13B 108.1 . . ? C1B N1B C5B 125.1(10) . . ? C1B N1B C13B 116.2(10) . . ? C5B N1B C13B 118.6(10) . . ? C13B C14B C15B 111.2(11) . . ? C13B C14B H14C 109.4 . . ? C15B C14B H14C 109.4 . . ? C13B C14B H14D 109.4 . . ? C15B C14B H14D 109.4 . . ? H14C C14B H14D 108.0 . . ? O3B C15B N2B 123.1(15) . . ? O3B C15B C14B 120.9(14) . . ? N2B C15B C14B 115.3(14) . . ? O5B C16B O4B 127.6(12) . . ? O5B C16B C13B 114.8(11) . . ? O4B C16B C13B 117.5(12) . . ? C15B N2B H2B1 120.0 . . ? C15B N2B H2B2 120.0 . . ? H2B1 N2B H2B2 120.0 . . ? C16B O4B Cu1 125.2(8) . . ? C16B O5B Cu2 120.2(8) . . ? O1C C1C N1C 119.6(12) . . ? O1C C1C C2C 119.6(12) . . ? N1C C1C C2C 120.6(11) . . ? C6C C2C C3C 126.9(12) . . ? C6C C2C C1C 118.2(11) . . ? C3C C2C C1C 114.7(11) . . ? C4C C3C C2C 125.3(12) . . ? C4C C3C C9C 120.1(11) . . ? C2C C3C C9C 114.6(10) . . ? C3C C4C C12C 126.6(12) . . ? C3C C4C C5C 120.8(12) . . ? C12C C4C C5C 112.3(11) . . ? O2C C5C N1C 117.9(12) . . ? O2C C5C C4C 126.6(13) . . ? N1C C5C C4C 115.1(11) . . ? C2C C6C C7C 118.1(12) . . ? C2C C6C H6C 120.9 . . ? C7C C6C H6C 120.9 . . ? C8C C7C C6C 112.0(13) . . ? C8C C7C H7C 124.0 . . ? C6C C7C H7C 124.0 . . ? C7C C8C C9C 136.0(15) . . ? C7C C8C H8C 112.0 . . ? C9C C8C H8C 112.0 . . ? C8C C9C C10C 139.7(14) . . ? C8C C9C C3C 112.2(12) . . ? C10C C9C C3C 108.1(11) . . ? C11C C10C C9C 131.1(15) . . ? C11C C10C H10C 114.4 . . ? C9C C10C H10C 114.4 . . ? C10C C11C C12C 124.1(14) . . ? C10C C11C H11C 117.9 . . ? C12C C11C H11C 117.9 . . ? C4C C12C C11C 109.9(12) . . ? C4C C12C H12C 125.1 . . ? C11C C12C H12C 125.1 . . ? N1C C13C C16C 106.9(13) . . ? N1C C13C C14C 114.4(13) . . ? C16C C13C C14C 109.7(12) . . ? N1C C13C H13C 108.5 . . ? C16C C13C H13C 108.5 . . ? C14C C13C H13C 108.5 . . ? C1C N1C C5C 122.6(11) . . ? C1C N1C C13C 120.1(12) . . ? C5C N1C C13C 117.0(11) . . ? C15C C14C C13C 108.8(12) . . ? C15C C14C H14E 109.9 . . ? C13C C14C H14E 109.9 . . ? C15C C14C H14F 109.9 . . ? C13C C14C H14F 109.9 . . ? H14E C14C H14F 108.3 . . ? O3C C15C N2C 125.0(15) . . ? O3C C15C C14C 119.5(14) . . ? N2C C15C C14C 115.4(14) . . ? O4C C16C O5C 124.8(12) . . ? O4C C16C C13C 120.3(12) . . ? O5C C16C C13C 114.6(11) . . ? C15C N2C H2C1 120.0 . . ? C15C N2C H2C2 120.0 . . ? H2C1 N2C H2C2 120.0 . . ? C16C O4C Cu1 123.0(8) . . ? C16C O5C Cu2 125.2(8) . . ? O1D C1D N1D 118.5(10) . . ? O1D C1D C2D 124.0(10) . . ? N1D C1D C2D 117.3(10) . . ? C3D C2D C6D 123.6(10) . . ? C3D C2D C1D 120.1(9) . . ? C6D C2D C1D 116.2(10) . . ? C4D C3D C2D 122.0(10) . . ? C4D C3D C9D 118.7(10) . . ? C2D C3D C9D 119.3(9) . . ? C3D C4D C12D 122.6(11) . . ? C3D C4D C5D 120.2(11) . . ? C12D C4D C5D 117.1(10) . . ? O2D C5D N1D 118.6(12) . . ? O2D C5D C4D 124.0(12) . . ? N1D C5D C4D 117.3(11) . . ? C2D C6D C7D 115.9(12) . . ? C2D C6D H6D 122.1 . . ? C7D C6D H6D 122.1 . . ? C8D C7D C6D 118.6(14) . . ? C8D C7D H7D 120.7 . . ? C6D C7D H7D 120.7 . . ? C7D C8D C9D 128.7(14) . . ? C7D C8D H8D 115.7 . . ? C9D C8D H8D 115.7 . . ? C8D C9D C10D 132.8(12) . . ? C8D C9D C3D 112.9(11) . . ? C10D C9D C3D 114.0(10) . . ? C11D C10D C9D 127.2(13) . . ? C11D C10D H10D 116.4 . . ? C9D C10D H10D 116.4 . . ? C10D C11D C12D 118.9(13) . . ? C10D C11D H11D 120.6 . . ? C12D C11D H11D 120.6 . . ? C4D C12D C11D 118.1(12) . . ? C4D C12D H12D 120.9 . . ? C11D C12D H12D 120.9 . . ? N1D C13D C16D 112.6(11) . . ? N1D C13D C14D 109.6(11) . . ? C16D C13D C14D 108.9(11) . . ? N1D C13D H13D 108.6 . . ? C16D C13D H13D 108.6 . . ? C14D C13D H13D 108.6 . . ? C1D N1D C5D 122.9(10) . . ? C1D N1D C13D 117.8(10) . . ? C5D N1D C13D 119.2(10) . . ? C15D C14D C13D 113.8(14) . . ? C15D C14D H14G 108.8 . . ? C13D C14D H14G 108.8 . . ? C15D C14D H14H 108.8 . . ? C13D C14D H14H 108.8 . . ? H14G C14D H14H 107.7 . . ? O3D C15D N2D 122(2) . . ? O3D C15D C14D 124(2) . . ? N2D C15D C14D 113.3(19) . . ? O4D C16D O5D 126.7(12) . . ? O4D C16D C13D 116.0(12) . . ? O5D C16D C13D 117.2(12) . . ? C15D N2D H2D1 120.0 . . ? C15D N2D H2D2 120.0 . . ? H2D1 N2D H2D2 120.0 . . ? C16D O4D Cu1 125.5(8) . . ? C16D O5D Cu2 121.4(8) . . ? O1E C1E N1E 120.2(9) . . ? O1E C1E C2E 121.8(9) . . ? N1E C1E C2E 117.5(9) . . ? C6E C2E C3E 122.1(10) . . ? C6E C2E C1E 119.5(10) . . ? C3E C2E C1E 118.4(9) . . ? C4E C3E C2E 123.5(10) . . ? C4E C3E C9E 119.4(10) . . ? C2E C3E C9E 117.0(10) . . ? C3E C4E C12E 121.6(11) . . ? C3E C4E C5E 119.7(10) . . ? C12E C4E C5E 118.7(11) . . ? O2E C5E N1E 116.7(10) . . ? O2E C5E C4E 125.4(10) . . ? N1E C5E C4E 117.7(9) . . ? C2E C6E C7E 120.4(12) . . ? C2E C6E H6E 119.8 . . ? C7E C6E H6E 119.8 . . ? C8E C7E C6E 114.6(13) . . ? C8E C7E H7E 122.7 . . ? C6E C7E H7E 122.7 . . ? C7E C8E C9E 131.5(15) . . ? C7E C8E H8E 114.2 . . ? C9E C8E H8E 114.2 . . ? C8E C9E C10E 132.9(13) . . ? C8E C9E C3E 114.2(11) . . ? C10E C9E C3E 112.8(12) . . ? C11E C10E C9E 128.2(15) . . ? C11E C10E H10E 115.9 . . ? C9E C10E H10E 115.9 . . ? C10E C11E C12E 118.7(14) . . ? C10E C11E H11E 120.7 . . ? C12E C11E H11E 120.7 . . ? C4E C12E C11E 119.2(12) . . ? C4E C12E H12E 120.4 . . ? C11E C12E H12E 120.4 . . ? N1E C13E C16E 112.4(9) . . ? N1E C13E C14E 108.1(10) . . ? C16E C13E C14E 116.3(10) . . ? N1E C13E H13E 106.4 . . ? C16E C13E H13E 106.4 . . ? C14E C13E H13E 106.4 . . ? C1E N1E C5E 122.7(8) . . ? C1E N1E C13E 116.8(8) . . ? C5E N1E C13E 120.4(8) . . ? C13E C14E C15E 115.9(14) . . ? C13E C14E H14I 108.3 . . ? C15E C14E H14I 108.3 . . ? C13E C14E H14J 108.3 . . ? C15E C14E H14J 108.3 . . ? H14I C14E H14J 107.4 . . ? O3E C15E N2E 119(2) . . ? O3E C15E C14E 124(2) . . ? N2E C15E C14E 117.0(19) . . ? O4E C16E O5E 127.2(11) . . ? O4E C16E C13E 120.0(10) . . ? O5E C16E C13E 112.7(10) . . ? C15E N2E H2E1 120.0 . . ? C15E N2E H2E2 120.0 . . ? H2E1 N2E H2E2 120.0 . . ? C15E O3E Cu2 135.8(14) . . ? C16E O4E Cu3 115.9(7) . . ? C16E O5E Cu4 127.0(7) . . ? O1F C1F N1F 119.7(11) . . ? O1F C1F C2F 123.1(11) . . ? N1F C1F C2F 117.0(10) . . ? C3F C2F C6F 127.1(11) . . ? C3F C2F C1F 117.7(10) . . ? C6F C2F C1F 114.9(10) . . ? C4F C3F C2F 124.8(11) . . ? C4F C3F C9F 117.1(10) . . ? C2F C3F C9F 117.8(10) . . ? C3F C4F C12F 125.6(11) . . ? C3F C4F C5F 119.2(11) . . ? C12F C4F C5F 115.2(11) . . ? O2F C5F N1F 117.7(11) . . ? O2F C5F C4F 125.7(11) . . ? N1F C5F C4F 116.4(10) . . ? C2F C6F C7F 113.0(11) . . ? C2F C6F H6F 123.5 . . ? C7F C6F H6F 123.5 . . ? C8F C7F C6F 117.2(12) . . ? C8F C7F H7F 121.4 . . ? C6F C7F H7F 121.4 . . ? C7F C8F C9F 134.4(14) . . ? C7F C8F H8F 112.8 . . ? C9F C8F H8F 112.8 . . ? C8F C9F C10F 136.0(13) . . ? C8F C9F C3F 109.8(11) . . ? C10F C9F C3F 112.7(11) . . ? C11F C10F C9F 128.6(14) . . ? C11F C10F H10F 115.7 . . ? C9F C10F H10F 115.7 . . ? C10F C11F C12F 120.5(13) . . ? C10F C11F H11F 119.8 . . ? C12F C11F H11F 119.8 . . ? C4F C12F C11F 114.9(12) . . ? C4F C12F H12F 122.6 . . ? C11F C12F H12F 122.6 . . ? N1F C13F C16F 109.5(12) . . ? N1F C13F C14F 110.4(12) . . ? C16F C13F C14F 116.5(11) . . ? N1F C13F H13F 106.6 . . ? C16F C13F H13F 106.6 . . ? C14F C13F H13F 106.6 . . ? C1F N1F C5F 124.0(10) . . ? C1F N1F C13F 116.4(10) . . ? C5F N1F C13F 119.6(10) . . ? C15F C14F C13F 112.8(10) . . ? C15F C14F H14K 109.0 . . ? C13F C14F H14K 109.0 . . ? C15F C14F H14L 109.0 . . ? C13F C14F H14L 109.0 . . ? H14K C14F H14L 107.8 . . ? O3F C15F N2F 119.5(13) . . ? O3F C15F C14F 123.8(12) . . ? N2F C15F C14F 116.7(13) . . ? O4F C16F O5F 122.2(11) . . ? O4F C16F C13F 121.2(11) . . ? O5F C16F C13F 115.8(11) . . ? C15F N2F H2F1 120.0 . . ? C15F N2F H2F2 120.0 . . ? H2F1 N2F H2F2 120.0 . . ? C16F O4F Cu3 129.5(8) . . ? C16F O5F Cu4 119.9(7) . . ? O1H C1H N1H 119.7(9) . . ? O1H C1H C2H 120.7(9) . . ? N1H C1H C2H 119.6(9) . . ? C6H C2H C3H 123.3(9) . . ? C6H C2H C1H 119.7(9) . . ? C3H C2H C1H 116.6(9) . . ? C4H C3H C2H 123.3(9) . . ? C4H C3H C9H 120.0(9) . . ? C2H C3H C9H 116.7(9) . . ? C3H C4H C12H 121.1(9) . . ? C3H C4H C5H 120.5(9) . . ? C12H C4H C5H 118.4(9) . . ? O2H C5H N1H 118.0(9) . . ? O2H C5H C4H 125.8(9) . . ? N1H C5H C4H 116.2(9) . . ? C2H C6H C7H 118.6(11) . . ? C2H C6H H6H 120.7 . . ? C7H C6H H6H 120.7 . . ? C8H C7H C6H 117.0(12) . . ? C8H C7H H7H 121.5 . . ? C6H C7H H7H 121.5 . . ? C7H C8H C9H 128.2(13) . . ? C7H C8H H8H 115.9 . . ? C9H C8H H8H 115.9 . . ? C8H C9H C10H 130.5(12) . . ? C8H C9H C3H 116.0(10) . . ? C10H C9H C3H 113.5(10) . . ? C11H C10H C9H 126.2(13) . . ? C11H C10H H10H 116.9 . . ? C9H C10H H10H 116.9 . . ? C10H C11H C12H 121.1(12) . . ? C10H C11H H11H 119.4 . . ? C12H C11H H11H 119.4 . . ? C4H C12H C11H 118.0(10) . . ? C4H C12H H12H 121.0 . . ? C11H C12H H12H 121.0 . . ? N1H C13H C14H 111.6(10) . . ? N1H C13H C16H 110.7(10) . . ? C14H C13H C16H 114.1(10) . . ? N1H C13H H13H 106.6 . . ? C14H C13H H13H 106.6 . . ? C16H C13H H13H 106.6 . . ? C1H N1H C5H 123.1(9) . . ? C1H N1H C13H 116.6(9) . . ? C5H N1H C13H 120.3(9) . . ? C15H C14H C13H 109.9(13) . . ? C15H C14H H14M 109.7 . . ? C13H C14H H14M 109.7 . . ? C15H C14H H14N 109.7 . . ? C13H C14H H14N 109.7 . . ? H14M C14H H14N 108.2 . . ? O3H C15H N2H 117.8(18) . . ? O3H C15H C14H 124.3(18) . . ? N2H C15H C14H 117.7(18) . . ? O5H C16H O4H 131.1(12) . . ? O5H C16H C13H 116.3(11) . . ? O4H C16H C13H 112.5(11) . . ? C15H N2H H2H1 120.0 . . ? C15H N2H H2H2 120.0 . . ? H2H1 N2H H2H2 120.0 . . ? C16H O4H Cu3 117.7(8) . . ? C16H O5H Cu4 120.9(8) . . ? C21I N3I C25I 120.0 . . ? C21I N3I Cu1 122.9(9) . . ? C25I N3I Cu1 117.1(9) . . ? C22I C21I N3I 120.0 . . ? C22I C21I H21I 120.0 . . ? N3I C21I H21I 120.0 . . ? C21I C22I C23I 120.0 . . ? C21I C22I H22I 120.0 . . ? C23I C22I H22I 120.0 . . ? C22I C23I C24I 120.0 . . ? C22I C23I H23I 120.0 . . ? C24I C23I H23I 120.0 . . ? C25I C24I C23I 120.0 . . ? C25I C24I H24I 120.0 . . ? C23I C24I H24I 120.0 . . ? C24I C25I N3I 120.0 . . ? C24I C25I H25I 120.0 . . ? N3I C25I H25I 120.0 . . ? C21J N3J C25J 120.0 . . ? C21J N3J Cu1 117.5(9) . . ? C25J N3J Cu1 122.1(9) . . ? C22J C21J N3J 120.0 . . ? C22J C21J H21J 120.0 . . ? N3J C21J H21J 120.0 . . ? C21J C22J C23J 120.0 . . ? C21J C22J H22J 120.0 . . ? C23J C22J H22J 120.0 . . ? C24J C23J C22J 120.0 . . ? C24J C23J H23J 120.0 . . ? C22J C23J H23J 120.0 . . ? C23J C24J C25J 120.0 . . ? C23J C24J H24J 120.0 . . ? C25J C24J H24J 120.0 . . ? C24J C25J N3J 120.0 . . ? C24J C25J H25J 120.0 . . ? N3J C25J H25J 120.0 . . ? C31 O36 Cu3 121.1(12) . . ? C31 O37 C32 121.1(13) . . ? O36 C31 O37 120.2(15) . . ? O36 C31 C34 125.5(15) . . ? O37 C31 C34 113.5(15) . . ? C33 C32 O37 104.3(13) . . ? C33 C32 H32A 110.9 . . ? O37 C32 H32A 110.9 . . ? C33 C32 H32B 110.9 . . ? O37 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O38 C34 C31 108.7(13) . . ? O38 C34 C35 111.5(13) . . ? C31 C34 C35 112.0(13) . . ? O38 C34 H34 108.2 . . ? C31 C34 H34 108.2 . . ? C35 C34 H34 108.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 O47 C42 120.3(14) . . ? O46 C41 O47 117.8(18) . . ? O46 C41 C44 126.6(18) . . ? O47 C41 C44 113.2(17) . . ? C43 C42 O47 101.7(14) . . ? C43 C42 H42A 111.4 . . ? O47 C42 H42A 111.4 . . ? C43 C42 H42B 111.4 . . ? O47 C42 H42B 111.4 . . ? H42A C42 H42B 109.3 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O48 C44 C41 106.2(15) . . ? O48 C44 C45 111.8(16) . . ? C41 C44 C45 109.6(16) . . ? O48 C44 H44 109.7 . . ? C41 C44 H44 109.7 . . ? C45 C44 H44 109.7 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C51 O57 C52 124.3(17) . . ? O56 C51 O57 114.6(18) . . ? O56 C51 C54 126(2) . . ? O57 C51 C54 112.8(19) . . ? C53 C52 O57 96.2(12) . . ? C53 C52 H52A 112.5 . . ? O57 C52 H52A 112.5 . . ? C53 C52 H52B 112.5 . . ? O57 C52 H52B 112.5 . . ? H52A C52 H52B 110.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O58 C54 C51 111.8(18) . . ? O58 C54 C55 114.1(18) . . ? C51 C54 C55 110.2(18) . . ? O58 C54 H54 106.8 . . ? C51 C54 H54 106.8 . . ? C55 C54 H54 106.8 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C61 O67 C62 131.3(18) . . ? O66 C61 O67 118.8(19) . . ? O66 C61 C64 123(2) . . ? O67 C61 C64 116.9(19) . . ? C63 C62 O67 98.4(15) . . ? C63 C62 H62A 112.1 . . ? O67 C62 H62A 112.1 . . ? C63 C62 H62B 112.1 . . ? O67 C62 H62B 112.1 . . ? H62A C62 H62B 109.7 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O68 C64 C61 110.2(17) . . ? O68 C64 C65 111.3(18) . . ? C61 C64 C65 108.7(18) . . ? O68 C64 H64 108.9 . . ? C61 C64 H64 108.9 . . ? C65 C64 H64 108.9 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4C Cu1 Cu2 O5D 88.4(3) . . . . ? O4A Cu1 Cu2 O5D -88.6(3) . . . . ? O4B Cu1 Cu2 O5D 179.8(3) . . . . ? O4D Cu1 Cu2 O5D -2.1(3) . . . . ? O4C Cu1 Cu2 O5B -92.3(3) . . . . ? O4A Cu1 Cu2 O5B 90.7(3) . . . . ? O4B Cu1 Cu2 O5B -0.9(3) . . . . ? O4D Cu1 Cu2 O5B 177.2(3) . . . . ? O4C Cu1 Cu2 O5C 1.6(3) . . . . ? O4A Cu1 Cu2 O5C -175.4(3) . . . . ? O4B Cu1 Cu2 O5C 92.9(3) . . . . ? O4D Cu1 Cu2 O5C -88.9(3) . . . . ? O4C Cu1 Cu2 O5A 178.6(3) . . . . ? O4A Cu1 Cu2 O5A 1.6(3) . . . . ? O4B Cu1 Cu2 O5A -90.0(3) . . . . ? O4D Cu1 Cu2 O5A 88.1(3) . . . . ? O4G Cu3 Cu4 O5F -98.4(3) . . . . ? O4E Cu3 Cu4 O5F 85.9(3) . . . . ? O4H Cu3 Cu4 O5F 171.6(3) . . . . ? O4F Cu3 Cu4 O5F -2.8(3) . . . . ? O36 Cu3 Cu4 O5F -17.1(12) . . . . ? O4G Cu3 Cu4 O5H 84.9(3) . . . . ? O4E Cu3 Cu4 O5H -90.8(3) . . . . ? O4H Cu3 Cu4 O5H -5.1(3) . . . . ? O4F Cu3 Cu4 O5H -179.5(3) . . . . ? O36 Cu3 Cu4 O5H 166.1(12) . . . . ? O4G Cu3 Cu4 O5G -3.3(3) . . . . ? O4E Cu3 Cu4 O5G -179.0(3) . . . . ? O4H Cu3 Cu4 O5G -93.3(3) . . . . ? O4F Cu3 Cu4 O5G 92.3(3) . . . . ? O36 Cu3 Cu4 O5G 77.9(12) . . . . ? O4G Cu3 Cu4 O5E 176.6(3) . . . . ? O4E Cu3 Cu4 O5E 0.9(3) . . . . ? O4H Cu3 Cu4 O5E 86.6(3) . . . . ? O4F Cu3 Cu4 O5E -87.8(3) . . . . ? O36 Cu3 Cu4 O5E -102.1(12) . . . . ? O1G C1G C2G C6G -1.7(19) . . . . ? N1G C1G C2G C6G 179.4(12) . . . . ? O1G C1G C2G C3G 179.4(12) . . . . ? N1G C1G C2G C3G 0.5(17) . . . . ? C6G C2G C3G C4G 176.9(13) . . . . ? C1G C2G C3G C4G -4(2) . . . . ? C6G C2G C3G C9G -2(2) . . . . ? C1G C2G C3G C9G 176.6(11) . . . . ? C2G C3G C4G C12G 178.1(13) . . . . ? C9G C3G C4G C12G -3(2) . . . . ? C2G C3G C4G C5G 3(2) . . . . ? C9G C3G C4G C5G -178.0(12) . . . . ? C3G C4G C5G O2G -176.5(14) . . . . ? C12G C4G C5G O2G 8(2) . . . . ? C3G C4G C5G N1G 2.4(19) . . . . ? C12G C4G C5G N1G -173.2(12) . . . . ? C3G C2G C6G C7G 2(2) . . . . ? C1G C2G C6G C7G -176.6(11) . . . . ? C2G C6G C7G C8G -2(2) . . . . ? C6G C7G C8G C9G 2(3) . . . . ? C7G C8G C9G C10G -178.6(16) . . . . ? C7G C8G C9G C3G -2(2) . . . . ? C4G C3G C9G C10G -0.2(19) . . . . ? C2G C3G C9G C10G 179.0(13) . . . . ? C4G C3G C9G C8G -177.1(13) . . . . ? C2G C3G C9G C8G 2.1(19) . . . . ? C8G C9G C10G C11G 178.9(17) . . . . ? C3G C9G C10G C11G 3(2) . . . . ? C9G C10G C11G C12G -2(3) . . . . ? C3G C4G C12G C11G 3(2) . . . . ? C5G C4G C12G C11G 178.9(12) . . . . ? C10G C11G C12G C4G -1(2) . . . . ? O1G C1G N1G C5G -174.0(12) . . . . ? C2G C1G N1G C5G 4.9(18) . . . . ? O1G C1G N1G C13G -0.7(17) . . . . ? C2G C1G N1G C13G 178.2(10) . . . . ? O2G C5G N1G C1G 172.8(12) . . . . ? C4G C5G N1G C1G -6.3(19) . . . . ? O2G C5G N1G C13G -0.4(18) . . . . ? C4G C5G N1G C13G -179.4(11) . . . . ? C16G C13G N1G C1G 55.3(14) . . . . ? C14G C13G N1G C1G -76.9(13) . . . . ? C16G C13G N1G C5G -131.0(12) . . . . ? C14G C13G N1G C5G 96.8(13) . . . . ? C16G C13G C14G C15G 68.6(15) . . . . ? N1G C13G C14G C15G -161.8(11) . . . . ? C13G C14G C15G O3G 25(2) . . . . ? C13G C14G C15G N2G -151.6(13) . . . . ? N1G C13G C16G O5G -137.0(11) . . . . ? C14G C13G C16G O5G -11.2(16) . . . . ? N1G C13G C16G O4G 43.4(15) . . . . ? C14G C13G C16G O4G 169.3(11) . . . . ? O5G C16G O4G Cu3 9.3(18) . . . . ? C13G C16G O4G Cu3 -171.2(7) . . . . ? O4H Cu3 O4G C16G 84.9(9) . . . . ? O4F Cu3 O4G C16G -80.5(9) . . . . ? O36 Cu3 O4G C16G -168.6(9) . . . . ? Cu4 Cu3 O4G C16G -1.2(9) . . . . ? O4G C16G O5G Cu4 -13.4(17) . . . . ? C13G C16G O5G Cu4 167.1(7) . . . . ? O5F Cu4 O5G C16G 96.6(9) . . . . ? O5H Cu4 O5G C16G -75.0(9) . . . . ? O5E Cu4 O5G C16G 8.7(16) . . . . ? O3Z Cu4 O5G C16G -177.3(10) . . . . ? O3A Cu4 O5G C16G -169.9(9) . . . . ? Cu3 Cu4 O5G C16G 9.0(8) . . . . ? O1A C1A C2A C3A -178.9(13) . . . . ? N1A C1A C2A C3A 1.5(13) . . . . ? O1A C1A C2A C6A 2.8(15) . . . . ? N1A C1A C2A C6A -176.8(15) . . . . ? C6A C2A C3A C4A 176.2(15) . . . . ? C1A C2A C3A C4A -1.8(13) . . . . ? C6A C2A C3A C9A -4.3(15) . . . . ? C1A C2A C3A C9A 177.6(10) . . . . ? C2A C3A C4A C12A 178.3(12) . . . . ? C9A C3A C4A C5A -177.9(13) . . . . ? C3A C4A C5A O2A 179.5(16) . . . . ? C12A C4A C5A N1A -177.8(15) . . . . ? C1A C2A C6A C7A 176.8(11) . . . . ? C2A C3A C9A C10A 176.9(12) . . . . ? C4A C3A C9A C8A -178.5(15) . . . . ? C2A C3A C9A C8A 2.0(18) . . . . ? C5A C4A C12A C11A -179.0(15) . . . . ? O1A C1A N1A C5A 179.4(15) . . . . ? C2A C1A N1A C13A -170.9(9) . . . . ? O2A C5A N1A C1A -179.7(15) . . . . ? C4A C5A N1A C13A 169.5(13) . . . . ? O5A C16A O4A Cu1 13.8(16) . . . . ? C13A C16A O4A Cu1 -173.4(9) . . . . ? O4B Cu1 O4A C16A 71.0(9) . . . . ? O4D Cu1 O4A C16A -86.2(9) . . . . ? N3I Cu1 O4A C16A 165.8(11) . . . . ? N3J Cu1 O4A C16A 170.5(11) . . . . ? Cu2 Cu1 O4A C16A -8.2(9) . . . . ? O4A C16A O5A Cu2 -12.4(17) . . . . ? C13A C16A O5A Cu2 174.5(8) . . . . ? O5D Cu2 O5A C16A 92.7(10) . . . . ? O5B Cu2 O5A C16A -83.4(10) . . . . ? O5C Cu2 O5A C16A 11.9(14) . . . . ? O3E Cu2 O5A C16A -173.4(10) . . . . ? Cu1 Cu2 O5A C16A 4.6(9) . . . . ? O4A C16A C13A N1A 34.1(16) . . . . ? O5A C16A C13A N1A -152.7(11) . . . . ? O4A C16A C13A C14A 151.9(13) . . . . ? O5A C16A C13A C14A -34.9(17) . . . . ? C1A N1A C13A C16A 55.1(16) . . . . ? C5A N1A C13A C16A -114.2(16) . . . . ? C1A N1A C13A C14A -64.5(18) . . . . ? C5A N1A C13A C14A 126.1(17) . . . . ? N1A C13A C14A C15A -179.2(17) . . . . ? C13A C14A C15A N2A -108(2) . . . . ? C14A C15A O3A Cu4 166.1(13) . . . . ? C14Z C15Z O3Z Cu4 167.3(15) . . . . ? O5F Cu4 O3Z C15Z -137.2(18) . . . . ? O5H Cu4 O3Z C15Z 40.3(18) . . . . ? O5G Cu4 O3Z C15Z 127.9(18) . . . . ? O5E Cu4 O3Z C15Z -53.9(18) . . . . ? N1B C1B C2B C6B 178.4(15) . . . . ? O1B C1B C2B C3B 176.9(15) . . . . ? C6B C2B C3B C4B -176.2(17) . . . . ? C1B C2B C3B C9B -179.9(13) . . . . ? C2B C3B C4B C12B 175.4(16) . . . . ? C9B C3B C4B C5B 178.8(13) . . . . ? C3B C4B C5B O2B 175.4(17) . . . . ? C12B C4B C5B N1B -176.7(14) . . . . ? C1B C2B C6B C7B 177.0(13) . . . . ? C7B C8B C9B C10B 178.1(19) . . . . ? C4B C3B C9B C8B 177.3(16) . . . . ? C2B C3B C9B C10B -176.2(15) . . . . ? C8B C9B C10B C11B -175.4(19) . . . . ? C9B C10B C11B C12B -4(3) . . . . ? C3B C4B C12B C11B -2(3) . . . . ? C5B C4B C12B C11B -179.5(13) . . . . ? C10B C11B C12B C4B 3(2) . . . . ? O1B C1B N1B C5B -177.4(15) . . . . ? C2B C1B N1B C5B 3(2) . . . . ? O1B C1B N1B C13B 6(2) . . . . ? C2B C1B N1B C13B -173.2(13) . . . . ? O2B C5B N1B C1B -174.3(15) . . . . ? C4B C5B N1B C1B -4(2) . . . . ? O2B C5B N1B C13B 2(2) . . . . ? C4B C5B N1B C13B 172.3(13) . . . . ? C16B C13B N1B C1B 46.2(19) . . . . ? C14B C13B N1B C1B -78.8(16) . . . . ? C16B C13B N1B C5B -130.4(14) . . . . ? C14B C13B N1B C5B 104.6(15) . . . . ? N1B C13B C14B C15B -161.9(11) . . . . ? C16B C13B C14B C15B 74.1(15) . . . . ? C13B C14B C15B O3B 27(2) . . . . ? C13B C14B C15B N2B -144.6(14) . . . . ? N1B C13B C16B O5B -136.2(12) . . . . ? C14B C13B C16B O5B -15.7(17) . . . . ? N1B C13B C16B O4B 47.1(17) . . . . ? C14B C13B C16B O4B 167.6(11) . . . . ? O5B C16B O4B Cu1 -1.8(18) . . . . ? C13B C16B O4B Cu1 174.4(8) . . . . ? O4C Cu1 O4B C16B 87.7(9) . . . . ? O4A Cu1 O4B C16B -87.4(9) . . . . ? O4D Cu1 O4B C16B -3.2(14) . . . . ? N3I Cu1 O4B C16B -174.7(10) . . . . ? N3J Cu1 O4B C16B 173.8(10) . . . . ? Cu2 Cu1 O4B C16B 1.6(9) . . . . ? O4B C16B O5B Cu2 0.4(17) . . . . ? C13B C16B O5B Cu2 -175.9(8) . . . . ? O5C Cu2 O5B C16B -78.5(9) . . . . ? O5A Cu2 O5B C16B 78.0(9) . . . . ? O3E Cu2 O5B C16B 177.0(9) . . . . ? Cu1 Cu2 O5B C16B 0.7(8) . . . . ? N1C C1C C2C C6C -177.5(17) . . . . ? O1C C1C C2C C3C -176.8(17) . . . . ? C6C C2C C3C C4C 177.5(19) . . . . ? C1C C2C C3C C9C -179.2(14) . . . . ? C2C C3C C4C C12C 176.7(18) . . . . ? C9C C3C C4C C5C -174.4(15) . . . . ? C3C C4C C5C O2C 176.9(19) . . . . ? C12C C4C C5C N1C 175.9(15) . . . . ? C1C C2C C6C C7C 179.2(14) . . . . ? C7C C8C C9C C10C 173(2) . . . . ? C4C C3C C9C C8C -178.2(18) . . . . ? C2C C3C C9C C10C -174.9(16) . . . . ? C8C C9C C10C C11C 180(2) . . . . ? C5C C4C C12C C11C 171.9(15) . . . . ? C10C C11C C12C C4C 3(3) . . . . ? O1C C1C N1C C5C 169.8(16) . . . . ? C2C C1C N1C C13C -178.0(15) . . . . ? O2C C5C N1C C1C -175.7(17) . . . . ? C4C C5C N1C C13C -176.1(15) . . . . ? C16C C13C N1C C5C -109.5(16) . . . . ? C14C C13C N1C C5C 128.8(16) . . . . ? N1C C13C C14C C15C -48.6(18) . . . . ? C16C C13C C14C C15C -168.8(12) . . . . ? C13C C14C C15C O3C -47.0(18) . . . . ? C13C C14C C15C N2C 133.8(14) . . . . ? N1C C13C C16C O4C 23.3(19) . . . . ? C14C C13C C16C O4C 147.9(12) . . . . ? N1C C13C C16C O5C -163.2(11) . . . . ? C14C C13C C16C O5C -38.6(17) . . . . ? O5C C16C O4C Cu1 14.9(18) . . . . ? C13C C16C O4C Cu1 -172.3(10) . . . . ? O4B Cu1 O4C C16C -87.6(10) . . . . ? O4D Cu1 O4C C16C 69.6(10) . . . . ? N3I Cu1 O4C C16C 177.4(11) . . . . ? N3J Cu1 O4C C16C 173.3(12) . . . . ? Cu2 Cu1 O4C C16C -8.4(9) . . . . ? O4C C16C O5C Cu2 -12.8(18) . . . . ? C13C C16C O5C Cu2 174.0(9) . . . . ? O5D Cu2 O5C C16C -84.2(10) . . . . ? O5B Cu2 O5C C16C 91.5(9) . . . . ? O5A Cu2 O5C C16C -2.8(14) . . . . ? O3E Cu2 O5C C16C -177.3(9) . . . . ? Cu1 Cu2 O5C C16C 4.5(9) . . . . ? O1D C1D C2D C3D -173.7(14) . . . . ? N1D C1D C2D C6D 178.0(13) . . . . ? C6D C2D C3D C4D -179.6(14) . . . . ? C1D C2D C3D C9D 176.2(12) . . . . ? C2D C3D C4D C12D 179.0(14) . . . . ? C9D C3D C4D C5D -178.7(14) . . . . ? C3D C4D C5D O2D -175.8(17) . . . . ? C12D C4D C5D N1D -174.8(14) . . . . ? C1D C2D C6D C7D 178.8(14) . . . . ? C7D C8D C9D C10D 179.9(19) . . . . ? C4D C3D C9D C8D 179.6(15) . . . . ? C2D C3D C9D C10D -174.8(13) . . . . ? C8D C9D C10D C11D -176.6(19) . . . . ? C5D C4D C12D C11D 172.7(15) . . . . ? O1D C1D N1D C5D 178.4(14) . . . . ? C2D C1D N1D C13D -174.6(11) . . . . ? O2D C5D N1D C1D 174.0(16) . . . . ? C4D C5D N1D C13D 172.2(13) . . . . ? C16D C13D N1D C1D 51.1(17) . . . . ? C14D C13D N1D C1D -70.3(16) . . . . ? C16D C13D N1D C5D -125.9(14) . . . . ? C14D C13D N1D C5D 112.7(15) . . . . ? N1D C13D C14D C15D -61.5(18) . . . . ? C16D C13D C14D C15D 174.9(15) . . . . ? C13D C14D C15D O3D 88(2) . . . . ? C13D C14D C15D N2D -97.7(18) . . . . ? N1D C13D C16D O4D 41.1(16) . . . . ? C14D C13D C16D O4D 162.8(11) . . . . ? N1D C13D C16D O5D -142.8(11) . . . . ? C14D C13D C16D O5D -21.1(16) . . . . ? O5D C16D O4D Cu1 3.7(18) . . . . ? C13D C16D O4D Cu1 179.3(8) . . . . ? O4C Cu1 O4D C16D -86.1(9) . . . . ? O4A Cu1 O4D C16D 90.2(9) . . . . ? O4B Cu1 O4D C16D 5.0(14) . . . . ? N3I Cu1 O4D C16D 176.1(10) . . . . ? N3J Cu1 O4D C16D -172.0(10) . . . . ? Cu2 Cu1 O4D C16D 0.2(9) . . . . ? O4D C16D O5D Cu2 -6.5(18) . . . . ? C13D C16D O5D Cu2 177.9(8) . . . . ? O5C Cu2 O5D C16D 84.3(9) . . . . ? O5A Cu2 O5D C16D -72.5(9) . . . . ? O3E Cu2 O5D C16D -171.5(9) . . . . ? Cu1 Cu2 O5D C16D 4.8(9) . . . . ? N1E C1E C2E C6E -175.5(12) . . . . ? O1E C1E C2E C3E 177.9(12) . . . . ? N1E C1E C2E C3E 5.8(19) . . . . ? C6E C2E C3E C4E 177.4(14) . . . . ? C1E C2E C3E C9E 179.1(12) . . . . ? C2E C3E C4E C12E -176.9(15) . . . . ? C9E C3E C4E C5E 180.0(13) . . . . ? C3E C4E C5E O2E -178.6(14) . . . . ? C12E C4E C5E N1E 176.1(13) . . . . ? C1E C2E C6E C7E -177.2(13) . . . . ? C4E C3E C9E C8E -176.8(16) . . . . ? C2E C3E C9E C10E 177.3(15) . . . . ? C8E C9E C10E C11E 175(2) . . . . ? C5E C4E C12E C11E -178.9(14) . . . . ? O1E C1E N1E C5E -179.3(11) . . . . ? C2E C1E N1E C5E -7.1(17) . . . . ? O1E C1E N1E C13E 4.3(17) . . . . ? C2E C1E N1E C13E 176.5(11) . . . . ? O2E C5E N1E C1E -178.6(12) . . . . ? C4E C5E N1E C1E 6.2(18) . . . . ? O2E C5E N1E C13E -2.3(18) . . . . ? C4E C5E N1E C13E -177.5(11) . . . . ? C16E C13E N1E C1E 52.1(14) . . . . ? C14E C13E N1E C1E -77.7(13) . . . . ? C16E C13E N1E C5E -124.4(11) . . . . ? C14E C13E N1E C5E 105.8(12) . . . . ? N1E C13E C14E C15E -149.2(12) . . . . ? C16E C13E C14E C15E 83.2(16) . . . . ? C13E C14E C15E O3E 172.6(17) . . . . ? N1E C13E C16E O4E 31.1(16) . . . . ? C14E C13E C16E O4E 156.6(11) . . . . ? N1E C13E C16E O5E -152.5(10) . . . . ? C14E C13E C16E O5E -27.0(15) . . . . ? C14E C15E O3E Cu2 160.7(11) . . . . ? O5D Cu2 O3E C15E 39.6(19) . . . . ? O5B Cu2 O3E C15E -139.4(19) . . . . ? O5C Cu2 O3E C15E 127.0(19) . . . . ? O5A Cu2 O3E C15E -50.8(19) . . . . ? O5E C16E O4E Cu3 4.0(16) . . . . ? C13E C16E O4E Cu3 179.8(8) . . . . ? O4H Cu3 O4E C16E -88.5(9) . . . . ? O4F Cu3 O4E C16E 77.2(8) . . . . ? O36 Cu3 O4E C16E 165.0(9) . . . . ? Cu4 Cu3 O4E C16E -2.6(8) . . . . ? O4E C16E O5E Cu4 -3.2(18) . . . . ? C13E C16E O5E Cu4 -179.3(7) . . . . ? O5F Cu4 O5E C16E -88.5(9) . . . . ? O5H Cu4 O5E C16E 84.2(9) . . . . ? O5G Cu4 O5E C16E 0.9(17) . . . . ? O3Z Cu4 O5E C16E -172.8(10) . . . . ? O3A Cu4 O5E C16E 179.6(10) . . . . ? Cu3 Cu4 O5E C16E 0.6(9) . . . . ? O1F C1F C2F C3F -173.6(16) . . . . ? N1F C1F C2F C6F -173.6(14) . . . . ? C6F C2F C3F C4F 175.7(17) . . . . ? C1F C2F C3F C9F 177.2(14) . . . . ? C2F C3F C4F C12F -175.0(17) . . . . ? C9F C3F C4F C5F 175.3(14) . . . . ? C3F C4F C5F O2F -171.4(16) . . . . ? C12F C4F C5F N1F -178.7(14) . . . . ? C1F C2F C6F C7F 179.4(13) . . . . ? C7F C8F C9F C10F -173.6(19) . . . . ? C4F C3F C9F C8F -169.3(16) . . . . ? C2F C3F C9F C10F 172.5(16) . . . . ? C5F C4F C12F C11F -177.6(14) . . . . ? O1F C1F N1F C5F 179.0(15) . . . . ? C2F C1F N1F C13F 172.8(13) . . . . ? O2F C5F N1F C1F 173.9(15) . . . . ? C4F C5F N1F C13F 179.9(13) . . . . ? C16F C13F N1F C1F 55.5(17) . . . . ? C14F C13F N1F C1F -74.1(17) . . . . ? C16F C13F N1F C5F -125.9(14) . . . . ? C14F C13F N1F C5F 104.5(15) . . . . ? N1F C13F C14F C15F -159.8(11) . . . . ? C16F C13F C14F C15F 74.5(15) . . . . ? C13F C14F C15F O3F 34.2(18) . . . . ? C13F C14F C15F N2F -147.9(12) . . . . ? N1F C13F C16F O4F 45.4(17) . . . . ? C14F C13F C16F O4F 171.5(11) . . . . ? N1F C13F C16F O5F -145.1(10) . . . . ? C14F C13F C16F O5F -19.0(16) . . . . ? O5F C16F O4F Cu3 -9.6(17) . . . . ? C13F C16F O4F Cu3 159.3(9) . . . . ? O4G Cu3 O4F C16F 90.4(10) . . . . ? O4E Cu3 O4F C16F -84.3(10) . . . . ? O4H Cu3 O4F C16F -14.6(18) . . . . ? O36 Cu3 O4F C16F -175.8(10) . . . . ? Cu4 Cu3 O4F C16F 7.3(9) . . . . ? O4F C16F O5F Cu4 4.8(15) . . . . ? C13F C16F O5F Cu4 -164.6(8) . . . . ? O5G Cu4 O5F C16F -84.2(8) . . . . ? O5E Cu4 O5F C16F 78.7(8) . . . . ? O3Z Cu4 O5F C16F -174.0(9) . . . . ? O3A Cu4 O5F C16F 173.1(9) . . . . ? Cu3 Cu4 O5F C16F 0.2(8) . . . . ? O1H C1H C2H C6H 4.9(19) . . . . ? N1H C1H C2H C6H -173.0(12) . . . . ? O1H C1H C2H C3H 178.6(12) . . . . ? N1H C1H C2H C3H 0.7(18) . . . . ? C6H C2H C3H C4H 176.7(13) . . . . ? C1H C2H C3H C4H 3.2(19) . . . . ? C6H C2H C3H C9H -4.4(19) . . . . ? C1H C2H C3H C9H -177.8(11) . . . . ? C2H C3H C4H C12H 176.9(12) . . . . ? C9H C3H C4H C5H -179.4(12) . . . . ? C3H C4H C5H O2H 176.1(12) . . . . ? C3H C4H C5H N1H -6.0(18) . . . . ? C12H C4H C5H N1H 176.5(11) . . . . ? C1H C2H C6H C7H 178.2(12) . . . . ? C7H C8H C9H C10H 178.9(16) . . . . ? C4H C3H C9H C8H -179.4(13) . . . . ? C2H C3H C9H C8H 1.6(19) . . . . ? C2H C3H C9H C10H -177.1(13) . . . . ? C8H C9H C10H C11H 179.0(16) . . . . ? C3H C4H C12H C11H 2.5(19) . . . . ? C5H C4H C12H C11H 180.0(11) . . . . ? O1H C1H N1H C5H 174.4(11) . . . . ? C2H C1H N1H C5H -7.6(18) . . . . ? O1H C1H N1H C13H -3.7(17) . . . . ? C2H C1H N1H C13H 174.2(11) . . . . ? O2H C5H N1H C1H -171.8(11) . . . . ? C4H C5H N1H C1H 10.1(17) . . . . ? O2H C5H N1H C13H 6.3(17) . . . . ? C4H C5H N1H C13H -171.8(11) . . . . ? C14H C13H N1H C1H -74.0(14) . . . . ? C16H C13H N1H C1H 54.2(14) . . . . ? C14H C13H N1H C5H 107.8(12) . . . . ? C16H C13H N1H C5H -123.9(11) . . . . ? N1H C13H C14H C15H -69.7(16) . . . . ? C16H C13H C14H C15H 163.8(13) . . . . ? C13H C14H C15H N2H 116.2(16) . . . . ? N1H C13H C16H O5H -128.6(11) . . . . ? C14H C13H C16H O5H -1.7(16) . . . . ? N1H C13H C16H O4H 52.4(14) . . . . ? C14H C13H C16H O4H 179.3(11) . . . . ? O5H C16H O4H Cu3 -2.0(18) . . . . ? C13H C16H O4H Cu3 176.8(7) . . . . ? O4G Cu3 O4H C16H -78.8(8) . . . . ? O4E Cu3 O4H C16H 97.0(9) . . . . ? O4F Cu3 O4H C16H 26.9(17) . . . . ? O36 Cu3 O4H C16H -172.7(8) . . . . ? Cu4 Cu3 O4H C16H 5.3(8) . . . . ? O4H C16H O5H Cu4 -4.8(18) . . . . ? C13H C16H O5H Cu4 176.4(7) . . . . ? O5G Cu4 O5H C16H 91.3(9) . . . . ? O5E Cu4 O5H C16H -71.7(9) . . . . ? O3Z Cu4 O5H C16H -179.1(9) . . . . ? O3A Cu4 O5H C16H -166.4(9) . . . . ? Cu3 Cu4 O5H C16H 6.5(8) . . . . ? O4C Cu1 N3I C21I 165.0(11) . . . . ? O4A Cu1 N3I C21I -17.5(11) . . . . ? O4B Cu1 N3I C21I 73.7(11) . . . . ? O4D Cu1 N3I C21I -102.8(11) . . . . ? O4C Cu1 N3I C25I -18.0(11) . . . . ? O4A Cu1 N3I C25I 159.5(11) . . . . ? O4B Cu1 N3I C25I -109.3(10) . . . . ? O4D Cu1 N3I C25I 74.2(11) . . . . ? Cu2 Cu1 N3I C25I -141(4) . . . . ? C25I N3I C21I C22I 0.0 . . . . ? Cu1 N3I C21I C22I 176.9(16) . . . . ? N3I C21I C22I C23I 0.0 . . . . ? C21I C22I C23I C24I 0.0 . . . . ? C22I C23I C24I C25I 0.0 . . . . ? C23I C24I C25I N3I 0.0 . . . . ? C21I N3I C25I C24I 0.0 . . . . ? Cu1 N3I C25I C24I -177.1(15) . . . . ? O4C Cu1 N3J C21J 166.7(11) . . . . ? O4A Cu1 N3J C21J -16.1(11) . . . . ? O4B Cu1 N3J C21J 76.7(10) . . . . ? O4D Cu1 N3J C21J -104.5(10) . . . . ? O4C Cu1 N3J C25J -20.5(11) . . . . ? O4A Cu1 N3J C25J 156.6(11) . . . . ? O4B Cu1 N3J C25J -110.5(11) . . . . ? O4D Cu1 N3J C25J 68.3(12) . . . . ? C25J N3J C21J C22J 0.0 . . . . ? Cu1 N3J C21J C22J 172.9(15) . . . . ? N3J C21J C22J C23J 0.0 . . . . ? C21J C22J C23J C24J 0.0 . . . . ? C22J C23J C24J C25J 0.0 . . . . ? C23J C24J C25J N3J 0.0 . . . . ? C21J N3J C25J C24J 0.0 . . . . ? Cu1 N3J C25J C24J -172.6(16) . . . . ? O4G Cu3 O36 C31 110.1(12) . . . . ? O4E Cu3 O36 C31 -73.1(12) . . . . ? O4H Cu3 O36 C31 -159.1(12) . . . . ? O4F Cu3 O36 C31 15.8(12) . . . . ? Cu3 O36 C31 O37 -94.3(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2G H2G2 O68 0.88 2.20 3.06(2) 163.4 . N2A H2A1 O5E 0.88 2.37 3.07(2) 137.4 . N2A H2A1 O5F 0.88 2.59 3.17(2) 124.1 . N2A H2A2 O3B 0.88 2.44 3.25(2) 153.3 . N2Z H2Z1 O5H 0.88 2.27 3.01(2) 142.1 . N2Z H2Z2 O1D 0.88 2.13 2.909(19) 147.5 . N2B H2B1 O3F 0.88 2.07 2.944(15) 170.7 . N2E H2E1 O5D 0.88 2.12 2.893(18) 146.8 . N2E H2E2 O1H 0.88 2.11 2.883(19) 145.7 . N2F H2F1 O3B 0.88 1.91 2.789(17) 176.0 . N2H H2H2 O3D 0.88 2.01 2.86(2) 160.4 . N2G H2G1 O1C 0.88 2.20 3.057(17) 163.9 1_455 N2F H2F2 O3C 0.88 2.05 2.900(17) 161.7 1_455 N2C H2C1 O3Z 0.88 2.43 3.198(19) 146.1 1_655 N2C H2C2 O3G 0.88 2.24 3.114(16) 173.3 1_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.59 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.720 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.103 _vrf_THETM01_6 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: No observable diffraction at high angle due to small available crystal size, extensive disorder and large cell. ; _vrf_PLAT023_6 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.59 Deg. RESPONSE: No observable diffraction at high angle due to small available crystal size, extensive disorder and large cell. ; _vrf_PLAT201_6 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 187 RESPONSE: Due to the weak data, only the copper atoms refined anisotropically; the light atoms were refined isotropically to avoid a low data-to-parameter ratio ; _vrf_PLAT602_6 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The voids contain heavily disordered solvent species, which could not be modeled and therefore were accounted for with the Squeeze program. ; #===END data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C136.32 H100.48 Cu4 N17 O42.16' _chemical_formula_sum 'C136.32 H100.48 Cu4 N17 O42.16' _chemical_formula_weight 2905.38 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.250(2) _cell_length_b 21.548(3) _cell_length_c 52.359(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17206(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7850 _cell_measurement_theta_min 2.258 _cell_measurement_theta_max 19.190 _exptl_crystal_description 'rectangular bar' _exptl_crystal_colour blue _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5963 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7968 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS Version 2.05 (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 232763 _diffrn_reflns_av_R_equivalents 0.1064 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 24.25 _reflns_number_total 27766 _reflns_number_gt 21452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.089(13) _refine_ls_number_reflns 27766 _refine_ls_number_parameters 787 _refine_ls_number_restraints 995 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2215 _refine_ls_wR_factor_gt 0.2106 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.96252(5) 0.42472(4) 0.305010(14) 0.0380(2) Uani 1 1 d D . . Cu2 Cu 0.92865(4) 0.41589(4) 0.355898(13) 0.03246(18) Uani 1 1 d . A . Cu3 Cu 0.54662(5) 0.54480(4) 0.458103(14) 0.03675(19) Uani 1 1 d . . . Cu4 Cu 0.56345(5) 0.52070(3) 0.409359(14) 0.03413(19) Uani 1 1 d . A . C1G C 0.4215(4) 0.7309(3) 0.42969(14) 0.0537(19) Uiso 1 1 d D . . C2G C 0.4225(4) 0.7928(3) 0.44079(13) 0.0502(18) Uiso 1 1 d D . . C3G C 0.3517(5) 0.8127(3) 0.45601(15) 0.061(2) Uiso 1 1 d D . . C4G C 0.2764(5) 0.7745(3) 0.45892(16) 0.064(2) Uiso 1 1 d D . . C5G C 0.2703(5) 0.7151(3) 0.44534(15) 0.061(2) Uiso 1 1 d D . . C6G C 0.4962(6) 0.8302(4) 0.43795(18) 0.074(3) Uiso 1 1 d D . . H6G H 0.5425 0.8193 0.4267 0.088 Uiso 1 1 calc R . . C7G C 0.4987(6) 0.8856(4) 0.45277(19) 0.085(3) Uiso 1 1 d D . . H7G H 0.5506 0.9099 0.4525 0.102 Uiso 1 1 calc R . . C8G C 0.4310(6) 0.9049(4) 0.46700(18) 0.084(3) Uiso 1 1 d D . . H8G H 0.4355 0.9438 0.4754 0.100 Uiso 1 1 calc R . . C9G C 0.3545(6) 0.8705(4) 0.47001(18) 0.080(3) Uiso 1 1 d D . . C10G C 0.2819(6) 0.8861(5) 0.48525(19) 0.085(3) Uiso 1 1 d D . . H10G H 0.2838 0.9233 0.4949 0.102 Uiso 1 1 calc R . . C11G C 0.2117(6) 0.8512(4) 0.48667(18) 0.076(3) Uiso 1 1 d D . . H11G H 0.1631 0.8652 0.4964 0.091 Uiso 1 1 calc R . . C12G C 0.2064(6) 0.7932(4) 0.47398(17) 0.071(2) Uiso 1 1 d D . . H12G H 0.1560 0.7677 0.4758 0.085 Uiso 1 1 calc R . . C13G C 0.3394(5) 0.6362(3) 0.41868(13) 0.0479(17) Uiso 1 1 d D B . H13G H 0.2858 0.6146 0.4252 0.057 Uiso 1 1 calc R . . N1G N 0.3462(3) 0.6948(3) 0.43245(11) 0.0464(14) Uiso 1 1 d D . . O1G O 0.4798(3) 0.7114(2) 0.41619(10) 0.0550(13) Uiso 1 1 d D . . O2G O 0.2054(4) 0.6834(3) 0.44525(13) 0.088(2) Uiso 1 1 d D . . C14G C 0.3247(6) 0.6490(4) 0.39147(17) 0.073(2) Uiso 1 1 d . . . H14O H 0.3810 0.6624 0.3839 0.087 Uiso 1 1 calc R . . H14P H 0.2834 0.6843 0.3901 0.087 Uiso 1 1 calc R . . C15G C 0.2883(5) 0.5949(4) 0.37543(16) 0.061(2) Uiso 1 1 d . . . C16G C 0.4173(4) 0.5932(3) 0.42395(12) 0.0374(15) Uiso 1 1 d . . . N2G N 0.2894(6) 0.5972(5) 0.35075(19) 0.107(3) Uiso 1 1 d . . . H2G1 H 0.2697 0.5656 0.3418 0.128 Uiso 1 1 calc R . . H2G2 H 0.3097 0.6303 0.3429 0.128 Uiso 1 1 calc R . . O3G O 0.2611(5) 0.5505(3) 0.38728(13) 0.0876(19) Uiso 1 1 d . . . O4G O 0.4414(3) 0.5893(2) 0.44716(8) 0.0461(11) Uiso 1 1 d . B . O5G O 0.4493(3) 0.5636(2) 0.40569(8) 0.0454(11) Uiso 1 1 d . A . C1A C 0.6882(6) 0.3992(5) 0.2812(2) 0.0816(7) Uiso 1 1 d D . . C2A C 0.6763(5) 0.3772(4) 0.25339(17) 0.0816(7) Uiso 1 1 d D . . C3A C 0.6561(5) 0.4195(4) 0.23584(19) 0.0816(7) Uiso 1 1 d D . . C4A C 0.6441(7) 0.4803(4) 0.24012(18) 0.0816(7) Uiso 1 1 d D . . C5A C 0.6552(7) 0.5035(5) 0.2663(2) 0.0816(7) Uiso 1 1 d D . . C6A C 0.6855(7) 0.3137(4) 0.24850(19) 0.0816(7) Uiso 1 1 d D . . H6A H 0.6977 0.2856 0.2620 0.098 Uiso 1 1 calc R . . C7A C 0.6763(7) 0.2917(5) 0.22291(18) 0.0816(7) Uiso 1 1 d D . . H7A H 0.6824 0.2491 0.2187 0.098 Uiso 1 1 calc R . . C8A C 0.6589(7) 0.3339(5) 0.2057(2) 0.0816(7) Uiso 1 1 d D . . H8A H 0.6550 0.3195 0.1886 0.098 Uiso 1 1 calc R . . C9A C 0.6458(7) 0.3947(5) 0.2091(2) 0.0816(7) Uiso 1 1 d D . . C10A C 0.6271(6) 0.4377(5) 0.1923(2) 0.0816(7) Uiso 1 1 d D . . H10A H 0.6240 0.4244 0.1750 0.098 Uiso 1 1 calc R . . C11A C 0.6121(6) 0.4965(5) 0.19632(19) 0.0816(7) Uiso 1 1 d D . . H11A H 0.5940 0.5219 0.1824 0.098 Uiso 1 1 calc R . . C12A C 0.6221(6) 0.5238(5) 0.22092(17) 0.0816(7) Uiso 1 1 d D . . H12A H 0.6147 0.5668 0.2241 0.098 Uiso 1 1 calc R . . N1A N 0.6809(5) 0.4626(3) 0.28594(15) 0.0816(7) Uiso 1 1 d D A . O1A O 0.7046(4) 0.3633(3) 0.29778(12) 0.0816(7) Uiso 1 1 d D . . O2A O 0.6484(4) 0.5590(3) 0.27286(12) 0.0816(7) Uiso 1 1 d D . . O4A O 0.8472(3) 0.4572(2) 0.29939(9) 0.0448(11) Uiso 1 1 d . A . O5A O 0.8132(3) 0.4476(2) 0.34085(8) 0.0412(11) Uiso 1 1 d . . . C16A C 0.7948(4) 0.4606(3) 0.31786(13) 0.0424(16) Uiso 1 1 d . A . C13A C 0.7047(5) 0.4840(3) 0.31156(14) 0.0534(19) Uiso 1 1 d D . . H13A H 0.7082 0.5303 0.3109 0.064 Uiso 1 1 calc R A . C14A C 0.6350(6) 0.4676(4) 0.33146(16) 0.065(2) Uiso 1 1 d D A . H14A H 0.5767 0.4711 0.3233 0.079 Uiso 1 1 calc R . . H14B H 0.6431 0.4236 0.3364 0.079 Uiso 1 1 calc R . . C15A C 0.6345(5) 0.5059(4) 0.35524(16) 0.0558(19) Uiso 1 1 d . . . N2A N 0.6959(5) 0.5469(4) 0.36011(15) 0.075(2) Uiso 1 1 d . A . H2A1 H 0.6945 0.5683 0.3744 0.090 Uiso 1 1 calc R . . H2A2 H 0.7385 0.5530 0.3490 0.090 Uiso 1 1 calc R . . O3A O 0.5771(3) 0.4973(2) 0.36989(10) 0.0563(13) Uiso 1 1 d . A . C1B C 0.9904(4) 0.2049(3) 0.31298(13) 0.0483(18) Uiso 1 1 d D . . C2B C 1.0470(5) 0.1681(4) 0.29594(15) 0.069(2) Uiso 1 1 d D . . C3B C 1.0065(5) 0.1351(4) 0.27626(15) 0.068(2) Uiso 1 1 d D . . C4B C 0.9181(5) 0.1389(4) 0.27089(14) 0.060(2) Uiso 1 1 d D . . C5B C 0.8616(5) 0.1772(4) 0.28737(14) 0.059(2) Uiso 1 1 d D . . C6B C 1.1356(6) 0.1667(5) 0.3000(2) 0.088(3) Uiso 1 1 d D . . H6B H 1.1610 0.1885 0.3140 0.105 Uiso 1 1 calc R . . C7B C 1.1892(8) 0.1316(6) 0.2829(2) 0.113(4) Uiso 1 1 d D . . H7B H 1.2511 0.1312 0.2850 0.136 Uiso 1 1 calc R . . C8B C 1.1525(7) 0.0993(6) 0.2638(2) 0.104(4) Uiso 1 1 d D . . H8B H 1.1892 0.0741 0.2534 0.125 Uiso 1 1 calc R . . C9B C 1.0627(6) 0.1009(5) 0.25847(17) 0.084(3) Uiso 1 1 d D . . C10B C 1.0208(6) 0.0728(5) 0.23729(18) 0.087(3) Uiso 1 1 d D . . H10B H 1.0563 0.0518 0.2251 0.104 Uiso 1 1 calc R . . C11B C 0.9366(6) 0.0742(5) 0.23354(18) 0.084(3) Uiso 1 1 d D . . H11B H 0.9125 0.0534 0.2192 0.101 Uiso 1 1 calc R . . C12B C 0.8793(6) 0.1069(4) 0.25083(16) 0.072(2) Uiso 1 1 d D . . H12B H 0.8174 0.1064 0.2486 0.087 Uiso 1 1 calc R . . C13B C 0.8473(4) 0.2477(3) 0.32423(12) 0.0348(14) Uiso 1 1 d D A . H13B H 0.7893 0.2532 0.3156 0.042 Uiso 1 1 calc R . . N1B N 0.9023(3) 0.2096(2) 0.30722(10) 0.0429(13) Uiso 1 1 d D . . O1B O 1.0203(4) 0.2347(2) 0.33087(10) 0.0599(14) Uiso 1 1 d D . . O2B O 0.7849(4) 0.1831(3) 0.28409(11) 0.0708(16) Uiso 1 1 d D . . C14B C 0.8309(5) 0.2145(3) 0.34877(13) 0.0439(16) Uiso 1 1 d . . . H14C H 0.8851 0.2154 0.3592 0.053 Uiso 1 1 calc R . . H14D H 0.8170 0.1705 0.3450 0.053 Uiso 1 1 calc R . . C15B C 0.7563(4) 0.2425(3) 0.36415(12) 0.0376(15) Uiso 1 1 d . . . C16B C 0.8867(4) 0.3107(3) 0.32735(12) 0.0332(14) Uiso 1 1 d . . . N2B N 0.7611(5) 0.2377(3) 0.38924(13) 0.0605(17) Uiso 1 1 d . . . H2B1 H 0.7195 0.2536 0.3989 0.073 Uiso 1 1 calc R . . H2B2 H 0.8059 0.2185 0.3963 0.073 Uiso 1 1 calc R . . O3B O 0.6959(4) 0.2685(3) 0.35326(10) 0.0614(14) Uiso 1 1 d . . . O4B O 0.9132(3) 0.3381(2) 0.30734(8) 0.0394(10) Uiso 1 1 d . A . O5B O 0.8871(3) 0.33364(19) 0.34961(8) 0.0327(9) Uiso 1 1 d . A . C1C C 1.2492(6) 0.4564(4) 0.31297(17) 0.0809(7) Uiso 1 1 d D . . C2C C 1.2985(6) 0.4774(4) 0.29047(17) 0.0809(7) Uiso 1 1 d D . . C3C C 1.3409(6) 0.4354(4) 0.27493(17) 0.0809(7) Uiso 1 1 d D . . C4C C 1.3389(6) 0.3727(4) 0.27981(17) 0.0809(7) Uiso 1 1 d D . . C5C C 1.2852(6) 0.3486(4) 0.30129(17) 0.0809(7) Uiso 1 1 d D . . C6C C 1.3026(6) 0.5412(4) 0.28646(18) 0.0809(7) Uiso 1 1 d D . . H6C H 1.2755 0.5689 0.2982 0.097 Uiso 1 1 calc R . . C7C C 1.3476(6) 0.5648(4) 0.26459(17) 0.0809(7) Uiso 1 1 d D . . H7C H 1.3496 0.6077 0.2605 0.097 Uiso 1 1 calc R . . C8C C 1.3853(6) 0.5230(4) 0.25087(18) 0.0809(7) Uiso 1 1 d D . . H8C H 1.4145 0.5392 0.2363 0.097 Uiso 1 1 calc R . . C9C C 1.3915(6) 0.4602(4) 0.25316(17) 0.0809(7) Uiso 1 1 d D . . C10C C 1.4291(6) 0.4135(4) 0.23845(18) 0.0809(7) Uiso 1 1 d D . . H10C H 1.4604 0.4267 0.2237 0.097 Uiso 1 1 calc R . . C11C C 1.4267(7) 0.3558(4) 0.24224(17) 0.0809(7) Uiso 1 1 d D . . H11C H 1.4557 0.3288 0.2307 0.097 Uiso 1 1 calc R . . C12C C 1.3802(6) 0.3297(4) 0.26411(17) 0.0809(7) Uiso 1 1 d D . . H12C H 1.3782 0.2864 0.2674 0.097 Uiso 1 1 calc R . . C13C C 1.1967(6) 0.3705(5) 0.34000(17) 0.0809(7) Uiso 1 1 d D A . H13C H 1.2020 0.3243 0.3404 0.097 Uiso 1 1 calc R . . N1C N 1.2501(5) 0.3932(3) 0.31840(14) 0.0809(7) Uiso 1 1 d D . . O1C O 1.2079(4) 0.4917(3) 0.32595(11) 0.0665(15) Uiso 1 1 d D . . O2C O 1.2768(4) 0.2943(3) 0.30586(12) 0.0743(16) Uiso 1 1 d D . . C14C C 1.2302(4) 0.3956(3) 0.36579(13) 0.0440(17) Uiso 1 1 d . . . H14E H 1.2138 0.4399 0.3675 0.053 Uiso 1 1 calc R . . H14F H 1.2025 0.3723 0.3799 0.053 Uiso 1 1 calc R . . C15C C 1.3285(5) 0.3892(4) 0.36747(15) 0.0534(19) Uiso 1 1 d . . . C16C C 1.1017(4) 0.3860(3) 0.33595(12) 0.0348(14) Uiso 1 1 d . . . N2C N 1.3742(5) 0.4397(3) 0.37390(12) 0.0597(17) Uiso 1 1 d . . . H2C1 H 1.4318 0.4383 0.3744 0.072 Uiso 1 1 calc R . . H2C2 H 1.3466 0.4745 0.3776 0.072 Uiso 1 1 calc R . . O3C O 1.3647(3) 0.3394(2) 0.36208(10) 0.0546(13) Uiso 1 1 d . . . O4C O 1.0774(3) 0.3929(2) 0.31318(9) 0.0451(11) Uiso 1 1 d . A . O5C O 1.0534(3) 0.3887(2) 0.35519(9) 0.0466(11) Uiso 1 1 d . A . C1D C 0.9037(4) 0.6379(4) 0.31963(14) 0.057(2) Uiso 1 1 d D . . C2D C 0.8732(5) 0.6784(4) 0.29958(15) 0.068(2) Uiso 1 1 d D . . C3D C 0.9334(5) 0.7133(4) 0.28498(16) 0.074(2) Uiso 1 1 d D . . C4D C 1.0208(5) 0.7119(4) 0.29104(16) 0.074(3) Uiso 1 1 d D . . C5D C 1.0554(5) 0.6722(4) 0.31102(16) 0.076(3) Uiso 1 1 d D . . C6D C 0.7832(6) 0.6803(5) 0.2950(2) 0.099(3) Uiso 1 1 d D . . H6D H 0.7434 0.6570 0.3052 0.119 Uiso 1 1 calc R . . C7D C 0.7527(8) 0.7184(6) 0.2745(2) 0.125 Uiso 1 1 d D . . H7D H 0.6917 0.7211 0.2709 0.150 Uiso 1 1 calc R . . C8D C 0.8106(7) 0.7507(6) 0.2601(3) 0.128(5) Uiso 1 1 d D . . H8D H 0.7886 0.7763 0.2468 0.154 Uiso 1 1 calc R . . C9D C 0.8999(6) 0.7482(5) 0.26381(18) 0.086(3) Uiso 1 1 d D . . C10D C 0.9650(7) 0.7793(5) 0.2487(2) 0.105(4) Uiso 1 1 d D . . H10D H 0.9464 0.8031 0.2344 0.126 Uiso 1 1 calc R . . C11D C 1.0498(7) 0.7762(5) 0.25382(18) 0.088(3) Uiso 1 1 d D . . H11D H 1.0907 0.7946 0.2424 0.106 Uiso 1 1 calc R . . C12D C 1.0811(6) 0.7454(4) 0.27644(18) 0.088(3) Uiso 1 1 d D . . H12D H 1.1410 0.7478 0.2813 0.105 Uiso 1 1 calc R . . C13D C 1.0198(6) 0.5976(4) 0.34613(14) 0.065(2) Uiso 1 1 d D A . H13D H 1.0853 0.5983 0.3463 0.078 Uiso 1 1 calc R . . N1D N 0.9910(4) 0.6377(3) 0.32537(12) 0.0550(16) Uiso 1 1 d D . . O1D O 0.8553(4) 0.6047(3) 0.33240(10) 0.0623(14) Uiso 1 1 d D . . O2D O 1.1305(5) 0.6675(3) 0.31714(14) 0.093(2) Uiso 1 1 d D . . C14D C 0.9871(7) 0.6200(5) 0.37337(17) 0.088(3) Uiso 1 1 d D . . H14G H 0.9222 0.6199 0.3738 0.106 Uiso 1 1 calc R . . H14H H 1.0082 0.5907 0.3866 0.106 Uiso 1 1 calc R . . C15D C 1.0199(10) 0.6838(7) 0.3793(3) 0.146(6) Uiso 1 1 d D . . N2D N 1.0844(9) 0.6801(7) 0.3971(3) 0.154(5) Uiso 1 1 d D . . H2D1 H 1.1081 0.7142 0.4032 0.185 Uiso 1 1 calc R . . H2D2 H 1.1027 0.6436 0.4024 0.185 Uiso 1 1 calc R . . O3D O 0.9885(8) 0.7303(6) 0.3703(2) 0.154(4) Uiso 1 1 d D . . C16D C 0.9914(5) 0.5306(3) 0.34076(14) 0.0482(18) Uiso 1 1 d . . . O4D O 0.9975(3) 0.5102(2) 0.31799(9) 0.0485(12) Uiso 1 1 d . A . O5D O 0.9676(3) 0.4993(2) 0.35995(9) 0.0488(12) Uiso 1 1 d . A . C1E C 0.7302(4) 0.3887(3) 0.48453(11) 0.0345(14) Uiso 1 1 d D . . C2E C 0.7423(4) 0.3631(3) 0.50997(11) 0.0393(15) Uiso 1 1 d D . . C3E C 0.8192(4) 0.3775(3) 0.52370(11) 0.0396(15) Uiso 1 1 d D . . C4E C 0.8829(4) 0.4158(3) 0.51340(13) 0.0537(18) Uiso 1 1 d D . . C5E C 0.8712(4) 0.4424(3) 0.48834(12) 0.0443(17) Uiso 1 1 d D . . C6E C 0.6796(5) 0.3248(3) 0.52040(14) 0.057(2) Uiso 1 1 d D . . H6E H 0.6276 0.3152 0.5112 0.069 Uiso 1 1 calc R . . C7E C 0.6940(5) 0.2998(4) 0.54521(15) 0.065(2) Uiso 1 1 d D . . H7E H 0.6508 0.2737 0.5526 0.078 Uiso 1 1 calc R . . C8E C 0.7673(5) 0.3125(4) 0.55832(17) 0.070(2) Uiso 1 1 d D . . H8E H 0.7749 0.2946 0.5748 0.084 Uiso 1 1 calc R . . C9E C 0.8319(5) 0.3506(3) 0.54866(13) 0.0558(19) Uiso 1 1 d D . . C10E C 0.9107(5) 0.3672(4) 0.56131(17) 0.072(2) Uiso 1 1 d D . . H10E H 0.9205 0.3516 0.5780 0.087 Uiso 1 1 calc R . . C11E C 0.9708(7) 0.4033(5) 0.55110(18) 0.087(3) Uiso 1 1 d D . . H11E H 1.0233 0.4115 0.5603 0.104 Uiso 1 1 calc R . . C12E C 0.9589(5) 0.4302(4) 0.52666(15) 0.067(2) Uiso 1 1 d D . . H12E H 1.0016 0.4573 0.5196 0.081 Uiso 1 1 calc R . . C13E C 0.7856(5) 0.4506(3) 0.44930(12) 0.0493(18) Uiso 1 1 d D B . H13E H 0.8335 0.4811 0.4458 0.059 Uiso 1 1 calc R . . N1E N 0.7947(3) 0.4279(2) 0.47533(9) 0.0395(13) Uiso 1 1 d D . . O1E O 0.6688(3) 0.3747(2) 0.47097(8) 0.0392(10) Uiso 1 1 d D . . O2E O 0.9264(4) 0.4758(3) 0.47787(12) 0.0769(17) Uiso 1 1 d D . . C14E C 0.7949(6) 0.3910(4) 0.42891(16) 0.063(2) Uiso 1 1 d . . . H14I H 0.8450 0.3655 0.4348 0.076 Uiso 1 1 calc R . . H14J H 0.7417 0.3652 0.4310 0.076 Uiso 1 1 calc R . . C15E C 0.8068(6) 0.4006(4) 0.40192(17) 0.068(2) Uiso 1 1 d . A . C16E C 0.6971(4) 0.4821(3) 0.44448(13) 0.0404(15) Uiso 1 1 d . . . N2E N 0.7425(5) 0.3845(3) 0.38612(15) 0.074(2) Uiso 1 1 d . . . H2E1 H 0.7512 0.3854 0.3695 0.089 Uiso 1 1 calc R . . H2E2 H 0.6913 0.3730 0.3923 0.089 Uiso 1 1 calc R . . O3E O 0.8820(3) 0.4175(3) 0.39393(10) 0.0588(13) Uiso 1 1 d . . . O4E O 0.6609(3) 0.5056(2) 0.46383(8) 0.0407(11) Uiso 1 1 d . B . O5E O 0.6752(3) 0.4856(2) 0.42171(8) 0.0404(10) Uiso 1 1 d . A . C1F C 0.3205(4) 0.3715(3) 0.45403(11) 0.0374(15) Uiso 1 1 d D . . C2F C 0.2449(5) 0.3556(4) 0.46993(14) 0.062(2) Uiso 1 1 d D . . C3F C 0.2559(4) 0.3238(3) 0.49309(13) 0.0515(18) Uiso 1 1 d D . . C4F C 0.3404(4) 0.3054(3) 0.50136(13) 0.0509(18) Uiso 1 1 d D . . C5F C 0.4161(4) 0.3142(3) 0.48399(12) 0.0439(16) Uiso 1 1 d D . . C6F C 0.1608(5) 0.3729(4) 0.46162(18) 0.078(3) Uiso 1 1 d D . . H6F H 0.1535 0.3943 0.4459 0.093 Uiso 1 1 calc R . . C7F C 0.0869(6) 0.3583(5) 0.47692(18) 0.090(3) Uiso 1 1 d D . . H7F H 0.0296 0.3696 0.4716 0.108 Uiso 1 1 calc R . . C8F C 0.0990(6) 0.3282(4) 0.49906(17) 0.079(3) Uiso 1 1 d D . . H8F H 0.0485 0.3187 0.5090 0.095 Uiso 1 1 calc R . . C9F C 0.1805(5) 0.3098(4) 0.50859(14) 0.060(2) Uiso 1 1 d D . . C10F C 0.1982(6) 0.2781(5) 0.53149(17) 0.081(3) Uiso 1 1 d D . . H10F H 0.1500 0.2682 0.5423 0.097 Uiso 1 1 calc R . . C11F C 0.2767(6) 0.2612(4) 0.53894(18) 0.079(3) Uiso 1 1 d D . . H11F H 0.2834 0.2412 0.5550 0.095 Uiso 1 1 calc R . . C12F C 0.3529(6) 0.2723(4) 0.52352(16) 0.075(3) Uiso 1 1 d D . . H12F H 0.4092 0.2575 0.5284 0.090 Uiso 1 1 calc R . . C13F C 0.4750(4) 0.3575(3) 0.44439(11) 0.0319(14) Uiso 1 1 d D B . H13F H 0.5287 0.3417 0.4532 0.038 Uiso 1 1 calc R . . N1F N 0.4011(3) 0.3479(2) 0.46174(9) 0.0382(12) Uiso 1 1 d D . . O1F O 0.3151(3) 0.4013(2) 0.43460(9) 0.0476(12) Uiso 1 1 d D . . O2F O 0.4884(4) 0.2935(3) 0.48796(11) 0.0695(16) Uiso 1 1 d D . . C14F C 0.4622(4) 0.3177(3) 0.42020(12) 0.0378(15) Uiso 1 1 d . . . H14K H 0.4375 0.2770 0.4252 0.045 Uiso 1 1 calc R . . H14L H 0.4192 0.3384 0.4089 0.045 Uiso 1 1 calc R . . C15F C 0.5445(4) 0.3071(3) 0.40567(12) 0.0363(14) Uiso 1 1 d . . . C16F C 0.4909(4) 0.4251(3) 0.43832(12) 0.0333(14) Uiso 1 1 d . . . N2F N 0.5412(4) 0.3082(3) 0.38030(11) 0.0507(15) Uiso 1 1 d . . . H2F1 H 0.5893 0.3025 0.3713 0.061 Uiso 1 1 calc R . . H2F2 H 0.4909 0.3147 0.3725 0.061 Uiso 1 1 calc R . . O3F O 0.6175(3) 0.2978(2) 0.41654(9) 0.0454(11) Uiso 1 1 d . . . O4F O 0.4886(3) 0.46199(19) 0.45677(8) 0.0341(9) Uiso 1 1 d . B . O5F O 0.5128(3) 0.43869(18) 0.41590(8) 0.0343(10) Uiso 1 1 d . A . C1H C 0.8178(4) 0.6532(3) 0.44243(14) 0.0510(18) Uiso 1 1 d D . . C2H C 0.8965(5) 0.6581(3) 0.45754(15) 0.058(2) Uiso 1 1 d D . . C3H C 0.9060(5) 0.7099(3) 0.47355(15) 0.060(2) Uiso 1 1 d D . . C4H C 0.8402(5) 0.7547(4) 0.47543(16) 0.070(2) Uiso 1 1 d D . . C5H C 0.7611(5) 0.7504(3) 0.45965(15) 0.058(2) Uiso 1 1 d D . . C6H C 0.9616(6) 0.6131(4) 0.45591(18) 0.078(3) Uiso 1 1 d D . . H6H H 0.9544 0.5791 0.4446 0.093 Uiso 1 1 calc R . . C7H C 1.0375(7) 0.6174(5) 0.47069(19) 0.093(3) Uiso 1 1 d D . . H7H H 1.0819 0.5866 0.4696 0.112 Uiso 1 1 calc R . . C8H C 1.0463(7) 0.6665(5) 0.4865(2) 0.097(3) Uiso 1 1 d D . . H8H H 1.0977 0.6690 0.4967 0.116 Uiso 1 1 calc R . . C9H C 0.9849(6) 0.7130(4) 0.48866(19) 0.086(3) Uiso 1 1 d D . . C10H C 0.9902(7) 0.7661(5) 0.5042(2) 0.094(3) Uiso 1 1 d D . . H10H H 1.0415 0.7708 0.5144 0.113 Uiso 1 1 calc R . . C11H C 0.9310(6) 0.8094(4) 0.50587(18) 0.078(3) Uiso 1 1 d D . . H11H H 0.9407 0.8440 0.5168 0.094 Uiso 1 1 calc R . . C12H C 0.8507(6) 0.8056(4) 0.49134(18) 0.085(3) Uiso 1 1 d D . . H12H H 0.8069 0.8368 0.4926 0.102 Uiso 1 1 calc R . . C13H C 0.6813(5) 0.6948(3) 0.42531(13) 0.0492(18) Uiso 1 1 d D B . H13H H 0.6389 0.7280 0.4304 0.059 Uiso 1 1 calc R . . N1H N 0.7566(4) 0.7010(3) 0.44233(11) 0.0476(14) Uiso 1 1 d D . . O1H O 0.8041(4) 0.6087(3) 0.42799(10) 0.0630(14) Uiso 1 1 d D . . O2H O 0.6991(4) 0.7852(3) 0.46055(13) 0.0833(18) Uiso 1 1 d D . . C14H C 0.7090(7) 0.7099(4) 0.39765(17) 0.075(3) Uiso 1 1 d D . . H14M H 0.7577 0.6819 0.3928 0.089 Uiso 1 1 calc R . . H14N H 0.6591 0.7010 0.3862 0.089 Uiso 1 1 calc R . . C15H C 0.7374(9) 0.7750(6) 0.3935(2) 0.105(4) Uiso 1 1 d D . . O3H O 0.6885(7) 0.8184(5) 0.40059(19) 0.130(3) Uiso 1 1 d . . . N2H N 0.8185(9) 0.7862(6) 0.3853(2) 0.142(4) Uiso 1 1 d . . . H2H1 H 0.8385 0.8245 0.3849 0.171 Uiso 1 1 calc R . . H2H2 H 0.8523 0.7554 0.3804 0.171 Uiso 1 1 calc R . . C16H C 0.6332(5) 0.6340(3) 0.42813(14) 0.0493(18) Uiso 1 1 d . . . O4H O 0.6125(3) 0.6210(2) 0.45020(8) 0.0421(11) Uiso 1 1 d . B . O5H O 0.6188(3) 0.6025(2) 0.40841(8) 0.0418(11) Uiso 1 1 d . A . N3I N 0.9844(8) 0.4256(8) 0.26387(14) 0.0655(12) Uiso 0.50 1 d PGD A 1 C21I C 0.9126(6) 0.4250(7) 0.24753(19) 0.0655(12) Uiso 0.50 1 d PG A 1 H21I H 0.8548 0.4264 0.2543 0.079 Uiso 0.50 1 calc PR A 1 C22I C 0.9252(6) 0.4224(6) 0.22126(18) 0.0655(12) Uiso 0.50 1 d PG A 1 H22I H 0.8761 0.4221 0.2101 0.079 Uiso 0.50 1 calc PR A 1 C23I C 1.0097(7) 0.4205(5) 0.21133(14) 0.0655(12) Uiso 0.50 1 d PG A 1 H23I H 1.0183 0.4187 0.1934 0.079 Uiso 0.50 1 calc PR A 1 C24I C 1.0815(5) 0.4210(6) 0.22767(19) 0.0655(12) Uiso 0.50 1 d PG A 1 H24I H 1.1393 0.4197 0.2209 0.079 Uiso 0.50 1 calc PR A 1 C25I C 1.0689(6) 0.4236(7) 0.25394(18) 0.0655(12) Uiso 0.50 1 d PG A 1 H25I H 1.1180 0.4240 0.2651 0.079 Uiso 0.50 1 calc PR A 1 N3J N 0.9989(8) 0.4270(8) 0.26530(15) 0.0655(12) Uiso 0.50 1 d PGD A 2 C21J C 0.9372(6) 0.4376(7) 0.2462(2) 0.0655(12) Uiso 0.50 1 d PG A 2 H21J H 0.8766 0.4389 0.2504 0.079 Uiso 0.50 1 calc PR A 2 C22J C 0.9643(6) 0.4463(5) 0.22115(17) 0.0655(12) Uiso 0.50 1 d PG A 2 H22J H 0.9221 0.4536 0.2081 0.079 Uiso 0.50 1 calc PR A 2 C23J C 1.0530(7) 0.4443(5) 0.21510(15) 0.0655(12) Uiso 0.50 1 d PG A 2 H23J H 1.0715 0.4503 0.1979 0.079 Uiso 0.50 1 calc PR A 2 C24J C 1.1147(5) 0.4337(6) 0.2342(2) 0.0655(12) Uiso 0.50 1 d PG A 2 H24J H 1.1753 0.4324 0.2300 0.079 Uiso 0.50 1 calc PR A 2 C25J C 1.0876(7) 0.4250(7) 0.25925(17) 0.0655(12) Uiso 0.50 1 d PG A 2 H25J H 1.1298 0.4178 0.2723 0.079 Uiso 0.50 1 calc PR A 2 O36 O 0.6336(7) 0.5255(5) 0.5581(2) 0.0825(13) Uiso 0.580(8) 1 d PD B 1 O37 O 0.5196(7) 0.5883(5) 0.54653(19) 0.0825(13) Uiso 0.580(8) 1 d PD B 1 O38 O 0.5222(4) 0.5509(3) 0.49949(12) 0.0825(13) Uiso 0.580(8) 1 d PD B 1 C31 C 0.5779(8) 0.5414(6) 0.5422(2) 0.0825(13) Uiso 0.580(8) 1 d PD B 1 C32 C 0.5214(12) 0.6126(7) 0.5737(2) 0.0825(13) Uiso 0.580(8) 1 d PD B 1 H32A H 0.4852 0.5861 0.5850 0.099 Uiso 0.580(8) 1 calc PR B 1 H32B H 0.5821 0.6134 0.5803 0.099 Uiso 0.580(8) 1 calc PR B 1 C33 C 0.4851(11) 0.6757(7) 0.5722(3) 0.0825(13) Uiso 0.580(8) 1 d PD B 1 H33A H 0.4764 0.6870 0.5542 0.124 Uiso 0.580(8) 1 calc PR B 1 H33B H 0.5260 0.7050 0.5801 0.124 Uiso 0.580(8) 1 calc PR B 1 H33C H 0.4288 0.6771 0.5812 0.124 Uiso 0.580(8) 1 calc PR B 1 C34 C 0.5628(7) 0.5112(4) 0.51718(17) 0.0825(13) Uiso 0.580(8) 1 d PD B 1 H34 H 0.6224 0.5024 0.5101 0.099 Uiso 0.580(8) 1 calc PR B 1 C35 C 0.5185(11) 0.4501(6) 0.5193(3) 0.0825(13) Uiso 0.580(8) 1 d PD B 1 H35A H 0.4548 0.4561 0.5189 0.124 Uiso 0.580(8) 1 calc PR B 1 H35B H 0.5354 0.4302 0.5354 0.124 Uiso 0.580(8) 1 calc PR B 1 H35C H 0.5362 0.4237 0.5049 0.124 Uiso 0.580(8) 1 calc PR B 1 O39 O 0.5222(4) 0.5509(3) 0.49949(12) 0.0825(13) Uiso 0.420(8) 1 d P B 2 C36 C 0.5628(7) 0.5112(4) 0.51718(17) 0.0825(13) Uiso 0.420(8) 1 d P B 2 H36A H 0.5194 0.4823 0.5241 0.124 Uiso 0.420(8) 1 calc PR B 2 H36B H 0.5879 0.5359 0.5311 0.124 Uiso 0.420(8) 1 calc PR B 2 H36C H 0.6096 0.4879 0.5087 0.124 Uiso 0.420(8) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0311(4) 0.0562(5) 0.0265(4) 0.0041(4) 0.0007(3) 0.0015(4) Cu2 0.0277(3) 0.0447(4) 0.0250(4) 0.0005(3) 0.0004(3) 0.0018(3) Cu3 0.0324(4) 0.0421(4) 0.0358(4) -0.0043(3) 0.0027(3) 0.0008(3) Cu4 0.0298(4) 0.0396(4) 0.0329(4) -0.0015(3) 0.0027(3) -0.0002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O4A 1.915(5) . ? Cu1 O4C 1.929(5) . ? Cu1 O4B 2.017(4) . ? Cu1 O4D 2.035(5) . ? Cu1 N3J 2.152(7) . ? Cu1 N3I 2.180(7) . ? Cu1 Cu2 2.7207(10) . ? Cu2 O5D 1.905(5) . ? Cu2 O5B 1.911(4) . ? Cu2 O5C 1.991(5) . ? Cu2 O5A 2.046(4) . ? Cu2 O3E 2.115(5) . ? Cu3 O4G 1.955(5) . ? Cu3 O4E 1.959(4) . ? Cu3 O4H 1.969(5) . ? Cu3 O4F 1.993(4) . ? Cu3 O38 2.203(7) . ? Cu3 Cu4 2.6171(11) . ? Cu4 O5H 1.954(4) . ? Cu4 O5F 1.959(4) . ? Cu4 O5E 1.974(4) . ? Cu4 O5G 1.980(5) . ? Cu4 O3A 2.137(5) . ? C1G O1G 1.211(7) . ? C1G N1G 1.395(8) . ? C1G C2G 1.455(8) . ? C2G C6G 1.390(9) . ? C2G C3G 1.408(8) . ? C3G C4G 1.421(9) . ? C3G C9G 1.447(9) . ? C4G C12G 1.386(9) . ? C4G C5G 1.467(9) . ? C5G O2G 1.204(8) . ? C5G N1G 1.409(8) . ? C6G C7G 1.425(10) . ? C6G H6G 0.9500 . ? C7G C8G 1.339(10) . ? C7G H7G 0.9500 . ? C8G C9G 1.391(10) . ? C8G H8G 0.9500 . ? C9G C10G 1.405(10) . ? C10G C11G 1.309(10) . ? C10G H10G 0.9500 . ? C11G C12G 1.418(10) . ? C11G H11G 0.9500 . ? C12G H12G 0.9500 . ? C13G N1G 1.458(8) . ? C13G C14G 1.468(11) . ? C13G C16G 1.531(9) . ? C13G H13G 1.0000 . ? C14G C15G 1.541(12) . ? C14G H14O 0.9900 . ? C14G H14P 0.9900 . ? C15G O3G 1.213(10) . ? C15G N2G 1.293(12) . ? C16G O5G 1.249(7) . ? C16G O4G 1.273(7) . ? N2G H2G1 0.8800 . ? N2G H2G2 0.8800 . ? C1A O1A 1.188(11) . ? C1A N1A 1.392(12) . ? C1A C2A 1.543(13) . ? C2A C3A 1.330(10) . ? C2A C6A 1.399(11) . ? C3A C4A 1.342(10) . ? C3A C9A 1.506(14) . ? C4A C12A 1.415(11) . ? C4A C5A 1.471(13) . ? C5A O2A 1.248(11) . ? C5A N1A 1.407(12) . ? C6A C7A 1.428(11) . ? C6A H6A 0.9500 . ? C7A C8A 1.306(13) . ? C7A H7A 0.9500 . ? C8A C9A 1.338(13) . ? C8A H8A 0.9500 . ? C9A C10A 1.310(13) . ? C10A C11A 1.306(13) . ? C10A H10A 0.9500 . ? C11A C12A 1.424(11) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? N1A C13A 1.464(11) . ? O4A C16A 1.257(8) . ? O5A C16A 1.267(8) . ? C16A C13A 1.501(10) . ? C13A C14A 1.529(9) . ? C13A H13A 1.0000 . ? C14A C15A 1.494(11) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A O3A 1.178(9) . ? C15A N2A 1.313(10) . ? N2A H2A1 0.8800 . ? N2A H2A2 0.8800 . ? C1B O1B 1.223(7) . ? C1B N1B 1.380(7) . ? C1B C2B 1.473(9) . ? C2B C6B 1.369(10) . ? C2B C3B 1.396(9) . ? C3B C4B 1.380(9) . ? C3B C9B 1.465(10) . ? C4B C12B 1.390(9) . ? C4B C5B 1.471(9) . ? C5B O2B 1.190(8) . ? C5B N1B 1.397(8) . ? C6B C7B 1.432(11) . ? C6B H6B 0.9500 . ? C7B C8B 1.339(11) . ? C7B H7B 0.9500 . ? C8B C9B 1.398(11) . ? C8B H8B 0.9500 . ? C9B C10B 1.416(10) . ? C10B C11B 1.299(10) . ? C10B H10B 0.9500 . ? C11B C12B 1.443(10) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B N1B 1.473(7) . ? C13B C14B 1.492(9) . ? C13B C16B 1.494(9) . ? C13B H13B 1.0000 . ? C14B C15B 1.518(9) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B O3B 1.221(8) . ? C15B N2B 1.320(9) . ? C16B O5B 1.266(7) . ? C16B O4B 1.268(7) . ? N2B H2B1 0.8800 . ? N2B H2B2 0.8800 . ? C1C O1C 1.198(8) . ? C1C N1C 1.392(9) . ? C1C C2C 1.470(10) . ? C2C C3C 1.379(9) . ? C2C C6C 1.391(10) . ? C3C C4C 1.374(10) . ? C3C C9C 1.478(10) . ? C4C C12C 1.389(10) . ? C4C C5C 1.486(10) . ? C5C O2C 1.200(8) . ? C5C N1C 1.419(9) . ? C6C C7C 1.429(10) . ? C6C H6C 0.9500 . ? C7C C8C 1.287(10) . ? C7C H7C 0.9500 . ? C8C C9C 1.361(10) . ? C8C H8C 0.9500 . ? C9C C10C 1.391(10) . ? C10C C11C 1.260(10) . ? C10C H10C 0.9500 . ? C11C C12C 1.460(10) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C N1C 1.476(9) . ? C13C C16C 1.502(12) . ? C13C C14C 1.542(12) . ? C13C H13C 1.0000 . ? C14C C15C 1.507(10) . ? C14C H14E 0.9900 . ? C14C H14F 0.9900 . ? C15C O3C 1.240(9) . ? C15C N2C 1.336(10) . ? C16C O5C 1.250(7) . ? C16C O4C 1.257(7) . ? N2C H2C1 0.8800 . ? N2C H2C2 0.8800 . ? C1D O1D 1.226(8) . ? C1D N1D 1.364(8) . ? C1D C2D 1.442(9) . ? C2D C6D 1.395(10) . ? C2D C3D 1.411(9) . ? C3D C4D 1.371(9) . ? C3D C9D 1.434(10) . ? C4D C12D 1.396(10) . ? C4D C5D 1.451(9) . ? C5D O2D 1.194(9) . ? C5D N1D 1.442(9) . ? C6D C7D 1.431(11) . ? C6D H6D 0.9500 . ? C7D C8D 1.351(12) . ? C7D H7D 0.9500 . ? C8D C9D 1.376(11) . ? C8D H8D 0.9500 . ? C9D C10D 1.435(11) . ? C10D C11D 1.323(11) . ? C10D H10D 0.9500 . ? C11D C12D 1.439(10) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D N1D 1.457(8) . ? C13D C16D 1.533(11) . ? C13D C14D 1.586(9) . ? C13D H13D 1.0000 . ? C14D C15D 1.497(14) . ? C14D H14G 0.9900 . ? C14D H14H 0.9900 . ? C15D O3D 1.207(13) . ? C15D N2D 1.356(14) . ? N2D H2D1 0.8800 . ? N2D H2D2 0.8800 . ? C16D O5D 1.263(8) . ? C16D O4D 1.274(8) . ? C1E O1E 1.213(6) . ? C1E N1E 1.384(7) . ? C1E C2E 1.453(8) . ? C2E C6E 1.377(8) . ? C2E C3E 1.409(8) . ? C3E C4E 1.384(8) . ? C3E C9E 1.443(8) . ? C4E C12E 1.386(9) . ? C4E C5E 1.444(8) . ? C5E O2E 1.235(7) . ? C5E N1E 1.387(7) . ? C6E C7E 1.423(9) . ? C6E H6E 0.9500 . ? C7E C8E 1.339(9) . ? C7E H7E 0.9500 . ? C8E C9E 1.379(9) . ? C8E H8E 0.9500 . ? C9E C10E 1.418(9) . ? C10E C11E 1.316(10) . ? C10E H10E 0.9500 . ? C11E C12E 1.417(10) . ? C11E H11E 0.9500 . ? C12E H12E 0.9500 . ? C13E N1E 1.455(8) . ? C13E C16E 1.531(10) . ? C13E C14E 1.677(11) . ? C13E H13E 1.0000 . ? C14E C15E 1.440(12) . ? C14E H14I 0.9900 . ? C14E H14J 0.9900 . ? C15E O3E 1.275(10) . ? C15E N2E 1.328(11) . ? C16E O5E 1.240(8) . ? C16E O4E 1.260(8) . ? N2E H2E1 0.8800 . ? N2E H2E2 0.8800 . ? C1F O1F 1.206(7) . ? C1F N1F 1.391(7) . ? C1F C2F 1.463(8) . ? C2F C3F 1.402(9) . ? C2F C6F 1.406(9) . ? C3F C4F 1.416(8) . ? C3F C9F 1.440(9) . ? C4F C12F 1.376(9) . ? C4F C5F 1.482(8) . ? C5F O2F 1.207(7) . ? C5F N1F 1.392(7) . ? C6F C7F 1.418(10) . ? C6F H6F 0.9500 . ? C7F C8F 1.341(10) . ? C7F H7F 0.9500 . ? C8F C9F 1.397(10) . ? C8F H8F 0.9500 . ? C9F C10F 1.406(10) . ? C10F C11F 1.311(10) . ? C10F H10F 0.9500 . ? C11F C12F 1.435(10) . ? C11F H11F 0.9500 . ? C12F H12F 0.9500 . ? C13F N1F 1.462(7) . ? C13F C16F 1.511(9) . ? C13F C14F 1.543(9) . ? C13F H13F 1.0000 . ? C14F C15F 1.485(9) . ? C14F H14K 0.9900 . ? C14F H14L 0.9900 . ? C15F O3F 1.265(8) . ? C15F N2F 1.330(8) . ? C16F O4F 1.252(7) . ? C16F O5F 1.255(7) . ? N2F H2F1 0.8800 . ? N2F H2F2 0.8800 . ? C1H O1H 1.239(7) . ? C1H N1H 1.389(8) . ? C1H C2H 1.441(9) . ? C2H C6H 1.390(9) . ? C2H C3H 1.405(9) . ? C3H C4H 1.395(9) . ? C3H C9H 1.441(10) . ? C4H C12H 1.388(10) . ? C4H C5H 1.464(9) . ? C5H O2H 1.208(8) . ? C5H N1H 1.400(8) . ? C6H C7H 1.395(10) . ? C6H H6H 0.9500 . ? C7H C8H 1.349(10) . ? C7H H7H 0.9500 . ? C8H C9H 1.377(10) . ? C8H H8H 0.9500 . ? C9H C10H 1.408(10) . ? C10H C11H 1.301(10) . ? C10H H10H 0.9500 . ? C11H C12H 1.443(10) . ? C11H H11H 0.9500 . ? C12H H12H 0.9500 . ? C13H N1H 1.460(8) . ? C13H C16H 1.509(10) . ? C13H C14H 1.543(10) . ? C13H H13H 1.0000 . ? C14H C15H 1.483(12) . ? C14H H14M 0.9900 . ? C14H H14N 0.9900 . ? C15H O3H 1.254(14) . ? C15H N2H 1.330(16) . ? N2H H2H1 0.8800 . ? N2H H2H2 0.8800 . ? C16H O4H 1.230(8) . ? C16H O5H 1.256(8) . ? N3I C21I 1.3900 . ? N3I C25I 1.3900 . ? C21I C22I 1.3900 . ? C21I H21I 0.9500 . ? C22I C23I 1.3900 . ? C22I H22I 0.9500 . ? C23I C24I 1.3900 . ? C23I H23I 0.9500 . ? C24I C25I 1.3900 . ? C24I H24I 0.9500 . ? C25I H25I 0.9500 . ? N3J C21J 1.3900 . ? N3J C25J 1.3900 . ? C21J C22J 1.3900 . ? C21J H21J 0.9500 . ? C22J C23J 1.3900 . ? C22J H22J 0.9500 . ? C23J C24J 1.3900 . ? C23J H23J 0.9500 . ? C24J C25J 1.3900 . ? C24J H24J 0.9500 . ? C25J H25J 0.9500 . ? O36 C31 1.234(10) . ? O37 C31 1.366(10) . ? O37 C32 1.515(11) . ? O38 C34 1.404(8) . ? C31 C34 1.482(10) . ? C32 C33 1.470(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.484(11) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4A Cu1 O4C 176.0(2) . . ? O4A Cu1 O4B 90.31(19) . . ? O4C Cu1 O4B 89.79(18) . . ? O4A Cu1 O4D 87.74(19) . . ? O4C Cu1 O4D 90.57(19) . . ? O4B Cu1 O4D 156.32(18) . . ? O4A Cu1 N3J 94.6(4) . . ? O4C Cu1 N3J 89.3(4) . . ? O4B Cu1 N3J 100.1(4) . . ? O4D Cu1 N3J 103.6(4) . . ? O4A Cu1 N3I 89.2(4) . . ? O4C Cu1 N3I 94.8(4) . . ? O4B Cu1 N3I 97.2(4) . . ? O4D Cu1 N3I 106.4(4) . . ? N3J Cu1 N3I 6.2(5) . . ? O4A Cu1 Cu2 90.10(14) . . ? O4C Cu1 Cu2 86.01(14) . . ? O4B Cu1 Cu2 78.76(12) . . ? O4D Cu1 Cu2 77.65(14) . . ? N3J Cu1 Cu2 175.2(4) . . ? N3I Cu1 Cu2 175.9(4) . . ? O5D Cu2 O5B 176.22(19) . . ? O5D Cu2 O5C 88.9(2) . . ? O5B Cu2 O5C 92.32(18) . . ? O5D Cu2 O5A 89.82(19) . . ? O5B Cu2 O5A 87.57(17) . . ? O5C Cu2 O5A 155.96(18) . . ? O5D Cu2 O3E 89.1(2) . . ? O5B Cu2 O3E 93.79(19) . . ? O5C Cu2 O3E 110.1(2) . . ? O5A Cu2 O3E 93.88(19) . . ? O5D Cu2 Cu1 89.07(14) . . ? O5B Cu2 Cu1 87.65(12) . . ? O5C Cu2 Cu1 79.69(13) . . ? O5A Cu2 Cu1 76.29(12) . . ? O3E Cu2 Cu1 170.00(15) . . ? O4G Cu3 O4E 170.45(19) . . ? O4G Cu3 O4H 87.00(19) . . ? O4E Cu3 O4H 86.49(19) . . ? O4G Cu3 O4F 93.70(18) . . ? O4E Cu3 O4F 90.78(17) . . ? O4H Cu3 O4F 164.99(18) . . ? O4G Cu3 O38 96.9(2) . . ? O4E Cu3 O38 91.4(2) . . ? O4H Cu3 O38 104.1(2) . . ? O4F Cu3 O38 90.7(2) . . ? O4G Cu3 Cu4 83.80(13) . . ? O4E Cu3 Cu4 88.65(13) . . ? O4H Cu3 Cu4 84.86(13) . . ? O4F Cu3 Cu4 80.32(12) . . ? O38 Cu3 Cu4 171.03(18) . . ? O5H Cu4 O5F 171.17(18) . . ? O5H Cu4 O5E 88.92(19) . . ? O5F Cu4 O5E 86.41(17) . . ? O5H Cu4 O5G 87.53(18) . . ? O5F Cu4 O5G 95.21(18) . . ? O5E Cu4 O5G 165.89(19) . . ? O5H Cu4 O3A 98.4(2) . . ? O5F Cu4 O3A 89.70(18) . . ? O5E Cu4 O3A 98.17(19) . . ? O5G Cu4 O3A 95.85(19) . . ? O5H Cu4 Cu3 83.59(13) . . ? O5F Cu4 Cu3 88.28(12) . . ? O5E Cu4 Cu3 80.86(13) . . ? O5G Cu4 Cu3 85.18(13) . . ? O3A Cu4 Cu3 177.80(15) . . ? O1G C1G N1G 118.1(6) . . ? O1G C1G C2G 123.0(6) . . ? N1G C1G C2G 118.6(6) . . ? C6G C2G C3G 120.3(6) . . ? C6G C2G C1G 119.7(6) . . ? C3G C2G C1G 119.8(6) . . ? C2G C3G C4G 120.3(6) . . ? C2G C3G C9G 121.7(6) . . ? C4G C3G C9G 117.9(6) . . ? C12G C4G C3G 121.0(7) . . ? C12G C4G C5G 118.7(7) . . ? C3G C4G C5G 120.2(6) . . ? O2G C5G N1G 119.8(7) . . ? O2G C5G C4G 123.3(7) . . ? N1G C5G C4G 116.9(6) . . ? C2G C6G C7G 116.7(8) . . ? C2G C6G H6G 121.7 . . ? C7G C6G H6G 121.7 . . ? C8G C7G C6G 122.9(9) . . ? C8G C7G H7G 118.6 . . ? C6G C7G H7G 118.6 . . ? C7G C8G C9G 122.9(9) . . ? C7G C8G H8G 118.5 . . ? C9G C8G H8G 118.5 . . ? C8G C9G C10G 126.8(8) . . ? C8G C9G C3G 115.2(7) . . ? C10G C9G C3G 118.0(7) . . ? C11G C10G C9G 122.7(9) . . ? C11G C10G H10G 118.7 . . ? C9G C10G H10G 118.7 . . ? C10G C11G C12G 121.7(9) . . ? C10G C11G H11G 119.1 . . ? C12G C11G H11G 119.1 . . ? C4G C12G C11G 118.6(8) . . ? C4G C12G H12G 120.7 . . ? C11G C12G H12G 120.7 . . ? N1G C13G C14G 109.1(6) . . ? N1G C13G C16G 112.3(5) . . ? C14G C13G C16G 114.0(6) . . ? N1G C13G H13G 107.0 . . ? C14G C13G H13G 107.0 . . ? C16G C13G H13G 107.0 . . ? C1G N1G C5G 123.5(6) . . ? C1G N1G C13G 119.3(5) . . ? C5G N1G C13G 116.6(5) . . ? C13G C14G C15G 116.2(7) . . ? C13G C14G H14O 108.2 . . ? C15G C14G H14O 108.2 . . ? C13G C14G H14P 108.2 . . ? C15G C14G H14P 108.2 . . ? H14O C14G H14P 107.4 . . ? O3G C15G N2G 123.0(9) . . ? O3G C15G C14G 116.2(8) . . ? N2G C15G C14G 120.7(9) . . ? O5G C16G O4G 125.7(6) . . ? O5G C16G C13G 118.3(6) . . ? O4G C16G C13G 115.9(6) . . ? C15G N2G H2G1 120.0 . . ? C15G N2G H2G2 120.0 . . ? H2G1 N2G H2G2 120.0 . . ? C16G O4G Cu3 123.4(4) . . ? C16G O5G Cu4 120.5(4) . . ? O1A C1A N1A 121.7(9) . . ? O1A C1A C2A 120.9(9) . . ? N1A C1A C2A 117.4(9) . . ? C3A C2A C6A 124.5(9) . . ? C3A C2A C1A 118.0(9) . . ? C6A C2A C1A 117.5(8) . . ? C2A C3A C4A 125.8(10) . . ? C2A C3A C9A 115.1(8) . . ? C4A C3A C9A 119.1(8) . . ? C3A C4A C12A 124.1(9) . . ? C3A C4A C5A 118.2(9) . . ? C12A C4A C5A 117.7(9) . . ? O2A C5A N1A 115.1(9) . . ? O2A C5A C4A 124.8(9) . . ? N1A C5A C4A 120.0(9) . . ? C2A C6A C7A 119.1(9) . . ? C2A C6A H6A 120.4 . . ? C7A C6A H6A 120.4 . . ? C8A C7A C6A 115.9(10) . . ? C8A C7A H7A 122.1 . . ? C6A C7A H7A 122.1 . . ? C7A C8A C9A 128.3(11) . . ? C7A C8A H8A 115.9 . . ? C9A C8A H8A 115.9 . . ? C10A C9A C8A 129.5(11) . . ? C10A C9A C3A 113.4(9) . . ? C8A C9A C3A 117.1(9) . . ? C11A C10A C9A 128.1(11) . . ? C11A C10A H10A 116.0 . . ? C9A C10A H10A 116.0 . . ? C10A C11A C12A 121.9(10) . . ? C10A C11A H11A 119.1 . . ? C12A C11A H11A 119.1 . . ? C4A C12A C11A 113.3(9) . . ? C4A C12A H12A 123.4 . . ? C11A C12A H12A 123.4 . . ? C1A N1A C5A 120.5(9) . . ? C1A N1A C13A 116.8(7) . . ? C5A N1A C13A 122.6(7) . . ? C16A O4A Cu1 119.1(4) . . ? C16A O5A Cu2 129.0(4) . . ? O4A C16A O5A 125.3(6) . . ? O4A C16A C13A 115.7(6) . . ? O5A C16A C13A 119.0(6) . . ? N1A C13A C16A 108.8(6) . . ? N1A C13A C14A 112.3(7) . . ? C16A C13A C14A 114.1(6) . . ? N1A C13A H13A 107.1 . . ? C16A C13A H13A 107.1 . . ? C14A C13A H13A 107.1 . . ? C15A C14A C13A 116.4(7) . . ? C15A C14A H14A 108.2 . . ? C13A C14A H14A 108.2 . . ? C15A C14A H14B 108.2 . . ? C13A C14A H14B 108.2 . . ? H14A C14A H14B 107.3 . . ? O3A C15A N2A 120.6(8) . . ? O3A C15A C14A 117.4(7) . . ? N2A C15A C14A 122.0(8) . . ? C15A N2A H2A1 120.0 . . ? C15A N2A H2A2 120.0 . . ? H2A1 N2A H2A2 120.0 . . ? C15A O3A Cu4 131.7(5) . . ? O1B C1B N1B 119.5(6) . . ? O1B C1B C2B 121.8(6) . . ? N1B C1B C2B 118.5(6) . . ? C6B C2B C3B 122.7(7) . . ? C6B C2B C1B 119.7(7) . . ? C3B C2B C1B 117.5(6) . . ? C4B C3B C2B 123.5(7) . . ? C4B C3B C9B 118.2(7) . . ? C2B C3B C9B 117.8(7) . . ? C3B C4B C12B 122.7(7) . . ? C3B C4B C5B 119.0(7) . . ? C12B C4B C5B 118.2(7) . . ? O2B C5B N1B 119.4(7) . . ? O2B C5B C4B 123.4(7) . . ? N1B C5B C4B 117.1(6) . . ? C2B C6B C7B 118.5(9) . . ? C2B C6B H6B 120.7 . . ? C7B C6B H6B 120.7 . . ? C8B C7B C6B 120.3(11) . . ? C8B C7B H7B 119.9 . . ? C6B C7B H7B 119.9 . . ? C7B C8B C9B 123.0(10) . . ? C7B C8B H8B 118.5 . . ? C9B C8B H8B 118.5 . . ? C8B C9B C10B 126.0(9) . . ? C8B C9B C3B 117.3(8) . . ? C10B C9B C3B 116.7(8) . . ? C11B C10B C9B 123.7(9) . . ? C11B C10B H10B 118.1 . . ? C9B C10B H10B 118.1 . . ? C10B C11B C12B 121.0(9) . . ? C10B C11B H11B 119.5 . . ? C12B C11B H11B 119.5 . . ? C4B C12B C11B 117.3(8) . . ? C4B C12B H12B 121.3 . . ? C11B C12B H12B 121.3 . . ? N1B C13B C14B 110.4(5) . . ? N1B C13B C16B 110.1(5) . . ? C14B C13B C16B 114.1(5) . . ? N1B C13B H13B 107.3 . . ? C14B C13B H13B 107.3 . . ? C16B C13B H13B 107.3 . . ? C1B N1B C5B 124.0(5) . . ? C1B N1B C13B 117.5(5) . . ? C5B N1B C13B 118.4(5) . . ? C13B C14B C15B 113.1(5) . . ? C13B C14B H14C 109.0 . . ? C15B C14B H14C 109.0 . . ? C13B C14B H14D 109.0 . . ? C15B C14B H14D 109.0 . . ? H14C C14B H14D 107.8 . . ? O3B C15B N2B 122.9(7) . . ? O3B C15B C14B 120.0(6) . . ? N2B C15B C14B 117.1(6) . . ? O5B C16B O4B 125.3(6) . . ? O5B C16B C13B 117.3(5) . . ? O4B C16B C13B 117.4(5) . . ? C15B N2B H2B1 120.0 . . ? C15B N2B H2B2 120.0 . . ? H2B1 N2B H2B2 120.0 . . ? C16B O4B Cu1 126.8(4) . . ? C16B O5B Cu2 121.5(4) . . ? O1C C1C N1C 120.6(8) . . ? O1C C1C C2C 121.9(8) . . ? N1C C1C C2C 117.4(7) . . ? C3C C2C C6C 122.7(8) . . ? C3C C2C C1C 120.7(7) . . ? C6C C2C C1C 116.6(7) . . ? C4C C3C C2C 121.8(8) . . ? C4C C3C C9C 120.7(7) . . ? C2C C3C C9C 117.5(7) . . ? C3C C4C C12C 122.4(8) . . ? C3C C4C C5C 119.8(7) . . ? C12C C4C C5C 117.7(7) . . ? O2C C5C N1C 119.6(8) . . ? O2C C5C C4C 123.4(8) . . ? N1C C5C C4C 116.7(7) . . ? C2C C6C C7C 119.6(8) . . ? C2C C6C H6C 120.2 . . ? C7C C6C H6C 120.2 . . ? C8C C7C C6C 114.4(9) . . ? C8C C7C H7C 122.8 . . ? C6C C7C H7C 122.8 . . ? C7C C8C C9C 132.6(9) . . ? C7C C8C H8C 113.7 . . ? C9C C8C H8C 113.7 . . ? C8C C9C C10C 134.4(9) . . ? C8C C9C C3C 113.1(8) . . ? C10C C9C C3C 112.3(7) . . ? C11C C10C C9C 128.0(9) . . ? C11C C10C H10C 116.0 . . ? C9C C10C H10C 116.0 . . ? C10C C11C C12C 121.2(9) . . ? C10C C11C H11C 119.4 . . ? C12C C11C H11C 119.4 . . ? C4C C12C C11C 115.3(8) . . ? C4C C12C H12C 122.3 . . ? C11C C12C H12C 122.3 . . ? N1C C13C C16C 110.5(7) . . ? N1C C13C C14C 111.9(8) . . ? C16C C13C C14C 111.4(7) . . ? N1C C13C H13C 107.6 . . ? C16C C13C H13C 107.6 . . ? C14C C13C H13C 107.6 . . ? C1C N1C C5C 122.6(7) . . ? C1C N1C C13C 118.4(7) . . ? C5C N1C C13C 117.8(7) . . ? C15C C14C C13C 110.4(6) . . ? C15C C14C H14E 109.6 . . ? C13C C14C H14E 109.6 . . ? C15C C14C H14F 109.6 . . ? C13C C14C H14F 109.6 . . ? H14E C14C H14F 108.1 . . ? O3C C15C N2C 122.0(7) . . ? O3C C15C C14C 120.6(7) . . ? N2C C15C C14C 117.3(7) . . ? O5C C16C O4C 125.8(6) . . ? O5C C16C C13C 117.7(6) . . ? O4C C16C C13C 116.4(6) . . ? C15C N2C H2C1 120.0 . . ? C15C N2C H2C2 120.0 . . ? H2C1 N2C H2C2 120.0 . . ? C16C O4C Cu1 121.3(4) . . ? C16C O5C Cu2 126.3(4) . . ? O1D C1D N1D 117.7(6) . . ? O1D C1D C2D 123.8(7) . . ? N1D C1D C2D 118.4(6) . . ? C6D C2D C3D 122.1(8) . . ? C6D C2D C1D 117.4(7) . . ? C3D C2D C1D 120.5(7) . . ? C4D C3D C2D 119.7(7) . . ? C4D C3D C9D 122.4(7) . . ? C2D C3D C9D 117.9(7) . . ? C3D C4D C12D 120.2(8) . . ? C3D C4D C5D 122.2(7) . . ? C12D C4D C5D 117.4(7) . . ? O2D C5D N1D 118.1(7) . . ? O2D C5D C4D 126.3(8) . . ? N1D C5D C4D 115.6(7) . . ? C2D C6D C7D 117.8(10) . . ? C2D C6D H6D 121.1 . . ? C7D C6D H6D 121.1 . . ? C8D C7D C6D 120.0(11) . . ? C8D C7D H7D 120.0 . . ? C6D C7D H7D 120.0 . . ? C7D C8D C9D 123.4(12) . . ? C7D C8D H8D 118.3 . . ? C9D C8D H8D 118.3 . . ? C8D C9D C3D 118.7(9) . . ? C8D C9D C10D 126.1(9) . . ? C3D C9D C10D 115.2(8) . . ? C11D C10D C9D 122.7(10) . . ? C11D C10D H10D 118.7 . . ? C9D C10D H10D 118.7 . . ? C10D C11D C12D 121.0(9) . . ? C10D C11D H11D 119.5 . . ? C12D C11D H11D 119.5 . . ? C4D C12D C11D 118.1(9) . . ? C4D C12D H12D 121.0 . . ? C11D C12D H12D 121.0 . . ? N1D C13D C16D 109.7(6) . . ? N1D C13D C14D 113.3(7) . . ? C16D C13D C14D 111.2(7) . . ? N1D C13D H13D 107.4 . . ? C16D C13D H13D 107.4 . . ? C14D C13D H13D 107.4 . . ? C1D N1D C5D 123.3(6) . . ? C1D N1D C13D 117.4(6) . . ? C5D N1D C13D 119.2(6) . . ? C15D C14D C13D 111.2(9) . . ? C15D C14D H14G 109.4 . . ? C13D C14D H14G 109.4 . . ? C15D C14D H14H 109.4 . . ? C13D C14D H14H 109.4 . . ? H14G C14D H14H 108.0 . . ? O3D C15D N2D 127.2(15) . . ? O3D C15D C14D 123.3(14) . . ? N2D C15D C14D 109.4(13) . . ? C15D N2D H2D1 120.0 . . ? C15D N2D H2D2 120.0 . . ? H2D1 N2D H2D2 120.0 . . ? O5D C16D O4D 125.6(7) . . ? O5D C16D C13D 116.0(6) . . ? O4D C16D C13D 118.4(6) . . ? C16D O4D Cu1 127.2(5) . . ? C16D O5D Cu2 120.3(5) . . ? O1E C1E N1E 119.8(5) . . ? O1E C1E C2E 122.7(5) . . ? N1E C1E C2E 117.4(5) . . ? C6E C2E C3E 120.5(6) . . ? C6E C2E C1E 120.2(6) . . ? C3E C2E C1E 119.3(5) . . ? C4E C3E C2E 121.1(5) . . ? C4E C3E C9E 119.8(5) . . ? C2E C3E C9E 119.1(5) . . ? C3E C4E C12E 121.7(6) . . ? C3E C4E C5E 120.3(6) . . ? C12E C4E C5E 118.0(6) . . ? O2E C5E N1E 119.1(6) . . ? O2E C5E C4E 123.4(6) . . ? N1E C5E C4E 117.4(5) . . ? C2E C6E C7E 118.8(7) . . ? C2E C6E H6E 120.6 . . ? C7E C6E H6E 120.6 . . ? C8E C7E C6E 121.3(8) . . ? C8E C7E H7E 119.3 . . ? C6E C7E H7E 119.3 . . ? C7E C8E C9E 122.0(8) . . ? C7E C8E H8E 119.0 . . ? C9E C8E H8E 119.0 . . ? C8E C9E C10E 125.8(7) . . ? C8E C9E C3E 118.3(6) . . ? C10E C9E C3E 115.8(6) . . ? C11E C10E C9E 123.4(8) . . ? C11E C10E H10E 118.3 . . ? C9E C10E H10E 118.3 . . ? C10E C11E C12E 121.2(9) . . ? C10E C11E H11E 119.4 . . ? C12E C11E H11E 119.4 . . ? C4E C12E C11E 117.9(8) . . ? C4E C12E H12E 121.0 . . ? C11E C12E H12E 121.0 . . ? N1E C13E C16E 112.8(6) . . ? N1E C13E C14E 109.3(6) . . ? C16E C13E C14E 108.0(6) . . ? N1E C13E H13E 108.9 . . ? C16E C13E H13E 108.9 . . ? C14E C13E H13E 108.9 . . ? C1E N1E C5E 124.4(5) . . ? C1E N1E C13E 117.6(5) . . ? C5E N1E C13E 117.7(5) . . ? C15E C14E C13E 121.7(7) . . ? C15E C14E H14I 106.9 . . ? C13E C14E H14I 106.9 . . ? C15E C14E H14J 106.9 . . ? C13E C14E H14J 106.9 . . ? H14I C14E H14J 106.7 . . ? O3E C15E N2E 122.3(8) . . ? O3E C15E C14E 118.4(8) . . ? N2E C15E C14E 118.8(8) . . ? O5E C16E O4E 129.1(6) . . ? O5E C16E C13E 115.0(6) . . ? O4E C16E C13E 115.6(6) . . ? C15E N2E H2E1 120.0 . . ? C15E N2E H2E2 120.0 . . ? H2E1 N2E H2E2 120.0 . . ? C15E O3E Cu2 127.4(5) . . ? C16E O4E Cu3 116.1(4) . . ? C16E O5E Cu4 124.8(4) . . ? O1F C1F N1F 120.0(5) . . ? O1F C1F C2F 123.5(6) . . ? N1F C1F C2F 116.4(5) . . ? C3F C2F C6F 120.4(7) . . ? C3F C2F C1F 120.9(6) . . ? C6F C2F C1F 118.7(6) . . ? C2F C3F C4F 120.6(6) . . ? C2F C3F C9F 119.6(6) . . ? C4F C3F C9F 119.7(6) . . ? C12F C4F C3F 122.0(6) . . ? C12F C4F C5F 118.4(6) . . ? C3F C4F C5F 119.1(6) . . ? O2F C5F N1F 119.1(6) . . ? O2F C5F C4F 124.0(6) . . ? N1F C5F C4F 116.9(5) . . ? C2F C6F C7F 119.4(8) . . ? C2F C6F H6F 120.3 . . ? C7F C6F H6F 120.3 . . ? C8F C7F C6F 119.2(9) . . ? C8F C7F H7F 120.4 . . ? C6F C7F H7F 120.4 . . ? C7F C8F C9F 124.6(9) . . ? C7F C8F H8F 117.7 . . ? C9F C8F H8F 117.7 . . ? C8F C9F C10F 127.8(7) . . ? C8F C9F C3F 116.7(7) . . ? C10F C9F C3F 115.4(7) . . ? C11F C10F C9F 124.3(9) . . ? C11F C10F H10F 117.8 . . ? C9F C10F H10F 117.8 . . ? C10F C11F C12F 121.8(9) . . ? C10F C11F H11F 119.1 . . ? C12F C11F H11F 119.1 . . ? C4F C12F C11F 116.6(8) . . ? C4F C12F H12F 121.7 . . ? C11F C12F H12F 121.7 . . ? N1F C13F C16F 113.0(5) . . ? N1F C13F C14F 109.5(5) . . ? C16F C13F C14F 112.6(5) . . ? N1F C13F H13F 107.1 . . ? C16F C13F H13F 107.1 . . ? C14F C13F H13F 107.1 . . ? C1F N1F C5F 125.4(5) . . ? C1F N1F C13F 116.7(5) . . ? C5F N1F C13F 117.9(5) . . ? C15F C14F C13F 113.5(5) . . ? C15F C14F H14K 108.9 . . ? C13F C14F H14K 108.9 . . ? C15F C14F H14L 108.9 . . ? C13F C14F H14L 108.9 . . ? H14K C14F H14L 107.7 . . ? O3F C15F N2F 119.1(6) . . ? O3F C15F C14F 122.4(5) . . ? N2F C15F C14F 118.5(6) . . ? O4F C16F O5F 125.6(6) . . ? O4F C16F C13F 116.4(5) . . ? O5F C16F C13F 117.7(5) . . ? C15F N2F H2F1 120.0 . . ? C15F N2F H2F2 120.0 . . ? H2F1 N2F H2F2 120.0 . . ? C16F O4F Cu3 125.7(4) . . ? C16F O5F Cu4 118.6(4) . . ? O1H C1H N1H 117.3(6) . . ? O1H C1H C2H 122.1(6) . . ? N1H C1H C2H 120.5(6) . . ? C6H C2H C3H 121.1(7) . . ? C6H C2H C1H 120.7(7) . . ? C3H C2H C1H 118.1(6) . . ? C4H C3H C2H 121.2(6) . . ? C4H C3H C9H 122.1(7) . . ? C2H C3H C9H 116.7(6) . . ? C12H C4H C3H 120.4(7) . . ? C12H C4H C5H 118.9(7) . . ? C3H C4H C5H 120.6(7) . . ? O2H C5H N1H 117.3(7) . . ? O2H C5H C4H 125.7(7) . . ? N1H C5H C4H 117.0(6) . . ? C2H C6H C7H 120.8(8) . . ? C2H C6H H6H 119.6 . . ? C7H C6H H6H 119.6 . . ? C8H C7H C6H 118.4(10) . . ? C8H C7H H7H 120.8 . . ? C6H C7H H7H 120.8 . . ? C7H C8H C9H 123.5(10) . . ? C7H C8H H8H 118.2 . . ? C9H C8H H8H 118.2 . . ? C8H C9H C10H 126.9(9) . . ? C8H C9H C3H 119.4(8) . . ? C10H C9H C3H 113.8(8) . . ? C11H C10H C9H 125.5(10) . . ? C11H C10H H10H 117.2 . . ? C9H C10H H10H 117.2 . . ? C10H C11H C12H 120.9(9) . . ? C10H C11H H11H 119.6 . . ? C12H C11H H11H 119.6 . . ? C4H C12H C11H 117.3(8) . . ? C4H C12H H12H 121.3 . . ? C11H C12H H12H 121.3 . . ? N1H C13H C16H 113.7(6) . . ? N1H C13H C14H 109.7(6) . . ? C16H C13H C14H 114.1(6) . . ? N1H C13H H13H 106.2 . . ? C16H C13H H13H 106.2 . . ? C14H C13H H13H 106.2 . . ? C1H N1H C5H 121.9(6) . . ? C1H N1H C13H 117.6(5) . . ? C5H N1H C13H 120.2(6) . . ? C15H C14H C13H 114.7(8) . . ? C15H C14H H14M 108.6 . . ? C13H C14H H14M 108.6 . . ? C15H C14H H14N 108.6 . . ? C13H C14H H14N 108.6 . . ? H14M C14H H14N 107.6 . . ? O3H C15H N2H 120.9(12) . . ? O3H C15H C14H 119.1(11) . . ? N2H C15H C14H 119.4(12) . . ? C15H N2H H2H1 120.0 . . ? C15H N2H H2H2 120.0 . . ? H2H1 N2H H2H2 120.0 . . ? O4H C16H O5H 127.2(7) . . ? O4H C16H C13H 114.5(6) . . ? O5H C16H C13H 118.3(6) . . ? C16H O4H Cu3 121.2(5) . . ? C16H O5H Cu4 122.9(5) . . ? C21I N3I C25I 120.0 . . ? C21I N3I Cu1 119.2(6) . . ? C25I N3I Cu1 120.7(6) . . ? N3I C21I C22I 120.0 . . ? N3I C21I H21I 120.0 . . ? C22I C21I H21I 120.0 . . ? C23I C22I C21I 120.0 . . ? C23I C22I H22I 120.0 . . ? C21I C22I H22I 120.0 . . ? C22I C23I C24I 120.0 . . ? C22I C23I H23I 120.0 . . ? C24I C23I H23I 120.0 . . ? C23I C24I C25I 120.0 . . ? C23I C24I H24I 120.0 . . ? C25I C24I H24I 120.0 . . ? C24I C25I N3I 120.0 . . ? C24I C25I H25I 120.0 . . ? N3I C25I H25I 120.0 . . ? C21J N3J C25J 120.0 . . ? C21J N3J Cu1 121.5(6) . . ? C25J N3J Cu1 118.1(6) . . ? C22J C21J N3J 120.0 . . ? C22J C21J H21J 120.0 . . ? N3J C21J H21J 120.0 . . ? C23J C22J C21J 120.0 . . ? C23J C22J H22J 120.0 . . ? C21J C22J H22J 120.0 . . ? C22J C23J C24J 120.0 . . ? C22J C23J H23J 120.0 . . ? C24J C23J H23J 120.0 . . ? C25J C24J C23J 120.0 . . ? C25J C24J H24J 120.0 . . ? C23J C24J H24J 120.0 . . ? C24J C25J N3J 120.0 . . ? C24J C25J H25J 120.0 . . ? N3J C25J H25J 120.0 . . ? C31 O37 C32 113.5(10) . . ? C34 O38 Cu3 122.6(6) . . ? O36 C31 O37 122.9(11) . . ? O36 C31 C34 125.4(11) . . ? O37 C31 C34 111.7(10) . . ? C33 C32 O37 105.2(12) . . ? C33 C32 H32A 110.7 . . ? O37 C32 H32A 110.7 . . ? C33 C32 H32B 110.7 . . ? O37 C32 H32B 110.7 . . ? H32A C32 H32B 108.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O38 C34 C31 112.7(8) . . ? O38 C34 C35 112.8(10) . . ? C31 C34 C35 113.2(10) . . ? O38 C34 H34 105.8 . . ? C31 C34 H34 105.8 . . ? C35 C34 H34 105.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4A Cu1 Cu2 O5D -87.6(2) . . . . ? O4C Cu1 Cu2 O5D 91.5(2) . . . . ? O4B Cu1 Cu2 O5D -177.92(19) . . . . ? O4D Cu1 Cu2 O5D 0.0(2) . . . . ? O4A Cu1 Cu2 O5B 90.49(18) . . . . ? O4C Cu1 Cu2 O5B -90.38(18) . . . . ? O4B Cu1 Cu2 O5B 0.19(17) . . . . ? O4D Cu1 Cu2 O5B 178.16(18) . . . . ? O4A Cu1 Cu2 O5C -176.7(2) . . . . ? O4C Cu1 Cu2 O5C 2.41(19) . . . . ? O4B Cu1 Cu2 O5C 92.98(18) . . . . ? O4D Cu1 Cu2 O5C -89.05(19) . . . . ? O4A Cu1 Cu2 O5A 2.42(19) . . . . ? O4C Cu1 Cu2 O5A -178.46(19) . . . . ? O4B Cu1 Cu2 O5A -87.88(18) . . . . ? O4D Cu1 Cu2 O5A 90.08(19) . . . . ? O4G Cu3 Cu4 O5H 83.77(19) . . . . ? O4E Cu3 Cu4 O5H -90.37(18) . . . . ? O4H Cu3 Cu4 O5H -3.77(18) . . . . ? O4F Cu3 Cu4 O5H 178.61(18) . . . . ? O4G Cu3 Cu4 O5F -99.66(18) . . . . ? O4E Cu3 Cu4 O5F 86.21(17) . . . . ? O4H Cu3 Cu4 O5F 172.81(18) . . . . ? O4F Cu3 Cu4 O5F -4.82(17) . . . . ? O4G Cu3 Cu4 O5E 173.70(19) . . . . ? O4E Cu3 Cu4 O5E -0.44(18) . . . . ? O4H Cu3 Cu4 O5E 86.16(18) . . . . ? O4F Cu3 Cu4 O5E -91.46(17) . . . . ? O4G Cu3 Cu4 O5G -4.28(19) . . . . ? O4E Cu3 Cu4 O5G -178.41(18) . . . . ? O4H Cu3 Cu4 O5G -91.82(18) . . . . ? O4F Cu3 Cu4 O5G 90.56(17) . . . . ? O1G C1G C2G C6G -5.9(12) . . . . ? N1G C1G C2G C6G -178.9(7) . . . . ? O1G C1G C2G C3G 179.1(7) . . . . ? N1G C1G C2G C3G 6.1(11) . . . . ? C6G C2G C3G C4G 180.0(8) . . . . ? C1G C2G C3G C4G -5.0(12) . . . . ? C6G C2G C3G C9G -2.8(13) . . . . ? C1G C2G C3G C9G 172.2(8) . . . . ? C2G C3G C4G C12G 179.5(8) . . . . ? C9G C3G C4G C12G 2.2(13) . . . . ? C2G C3G C4G C5G -2.2(13) . . . . ? C9G C3G C4G C5G -179.5(8) . . . . ? C12G C4G C5G O2G 4.9(14) . . . . ? C3G C4G C5G O2G -173.4(9) . . . . ? C12G C4G C5G N1G -173.5(8) . . . . ? C3G C4G C5G N1G 8.2(12) . . . . ? C3G C2G C6G C7G 5.2(12) . . . . ? C1G C2G C6G C7G -169.8(8) . . . . ? C2G C6G C7G C8G -6.2(15) . . . . ? C6G C7G C8G C9G 4.6(17) . . . . ? C7G C8G C9G C10G 177.5(10) . . . . ? C7G C8G C9G C3G -1.7(15) . . . . ? C2G C3G C9G C8G 0.9(13) . . . . ? C4G C3G C9G C8G 178.1(9) . . . . ? C2G C3G C9G C10G -178.4(9) . . . . ? C4G C3G C9G C10G -1.2(13) . . . . ? C8G C9G C10G C11G 179.0(10) . . . . ? C3G C9G C10G C11G -1.8(16) . . . . ? C9G C10G C11G C12G 3.8(16) . . . . ? C3G C4G C12G C11G -0.5(14) . . . . ? C5G C4G C12G C11G -178.7(8) . . . . ? C10G C11G C12G C4G -2.6(15) . . . . ? O1G C1G N1G C5G -173.0(7) . . . . ? C2G C1G N1G C5G 0.3(11) . . . . ? O1G C1G N1G C13G -1.4(10) . . . . ? C2G C1G N1G C13G 172.0(6) . . . . ? O2G C5G N1G C1G 174.2(8) . . . . ? C4G C5G N1G C1G -7.3(11) . . . . ? O2G C5G N1G C13G 2.4(11) . . . . ? C4G C5G N1G C13G -179.1(7) . . . . ? C14G C13G N1G C1G -73.0(8) . . . . ? C16G C13G N1G C1G 54.4(8) . . . . ? C14G C13G N1G C5G 99.1(8) . . . . ? C16G C13G N1G C5G -133.4(7) . . . . ? N1G C13G C14G C15G -162.0(7) . . . . ? C16G C13G C14G C15G 71.5(9) . . . . ? C13G C14G C15G O3G 12.2(12) . . . . ? C13G C14G C15G N2G -166.3(9) . . . . ? N1G C13G C16G O5G -139.0(6) . . . . ? C14G C13G C16G O5G -14.2(9) . . . . ? N1G C13G C16G O4G 43.8(8) . . . . ? C14G C13G C16G O4G 168.6(6) . . . . ? O5G C16G O4G Cu3 9.9(9) . . . . ? C13G C16G O4G Cu3 -173.1(4) . . . . ? O4H Cu3 O4G C16G 84.5(5) . . . . ? O4F Cu3 O4G C16G -80.5(5) . . . . ? O38 Cu3 O4G C16G -171.7(5) . . . . ? Cu4 Cu3 O4G C16G -0.7(5) . . . . ? O4G C16G O5G Cu4 -15.4(9) . . . . ? C13G C16G O5G Cu4 167.6(4) . . . . ? O5H Cu4 O5G C16G -73.0(5) . . . . ? O5F Cu4 O5G C16G 98.6(5) . . . . ? O5E Cu4 O5G C16G 2.6(11) . . . . ? O3A Cu4 O5G C16G -171.2(5) . . . . ? Cu3 Cu4 O5G C16G 10.8(5) . . . . ? O1A C1A C2A C3A 178.5(8) . . . . ? N1A C1A C2A C3A -2.8(8) . . . . ? O1A C1A C2A C6A 0.0(10) . . . . ? N1A C1A C2A C6A 178.7(9) . . . . ? C6A C2A C3A C4A 177.6(10) . . . . ? C1A C2A C3A C4A -0.7(9) . . . . ? C6A C2A C3A C9A -1.9(10) . . . . ? C1A C2A C3A C9A 179.8(7) . . . . ? C2A C3A C4A C12A -179.6(8) . . . . ? C9A C3A C4A C12A -0.1(15) . . . . ? C2A C3A C4A C5A 1.1(13) . . . . ? C9A C3A C4A C5A -179.4(8) . . . . ? C3A C4A C5A O2A 178.0(10) . . . . ? C12A C4A C5A O2A -1.4(16) . . . . ? C3A C4A C5A N1A 2.1(14) . . . . ? C12A C4A C5A N1A -177.2(9) . . . . ? C3A C2A C6A C7A 2.6(13) . . . . ? C1A C2A C6A C7A -179.0(8) . . . . ? C2A C6A C7A C8A -0.5(14) . . . . ? C6A C7A C8A C9A -2.3(17) . . . . ? C7A C8A C9A C10A -178.9(11) . . . . ? C7A C8A C9A C3A 3.0(17) . . . . ? C2A C3A C9A C10A -179.2(8) . . . . ? C4A C3A C9A C10A 1.3(13) . . . . ? C2A C3A C9A C8A -0.8(12) . . . . ? C4A C3A C9A C8A 179.7(10) . . . . ? C8A C9A C10A C11A 177.7(11) . . . . ? C3A C9A C10A C11A -4.1(16) . . . . ? C9A C10A C11A C12A 5.6(18) . . . . ? C3A C4A C12A C11A 1.1(15) . . . . ? C5A C4A C12A C11A -179.5(9) . . . . ? C10A C11A C12A C4A -3.6(14) . . . . ? O1A C1A N1A C5A -175.4(9) . . . . ? C2A C1A N1A C5A 5.9(12) . . . . ? O1A C1A N1A C13A 7.3(13) . . . . ? C2A C1A N1A C13A -171.4(6) . . . . ? O2A C5A N1A C1A 178.1(9) . . . . ? C4A C5A N1A C1A -5.7(14) . . . . ? O2A C5A N1A C13A -4.8(14) . . . . ? C4A C5A N1A C13A 171.5(8) . . . . ? O4B Cu1 O4A C16A 74.5(5) . . . . ? O4D Cu1 O4A C16A -81.9(5) . . . . ? N3J Cu1 O4A C16A 174.7(6) . . . . ? N3I Cu1 O4A C16A 171.7(6) . . . . ? Cu2 Cu1 O4A C16A -4.3(5) . . . . ? O5D Cu2 O5A C16A 87.6(6) . . . . ? O5B Cu2 O5A C16A -89.6(6) . . . . ? O5C Cu2 O5A C16A 0.7(8) . . . . ? O3E Cu2 O5A C16A 176.7(6) . . . . ? Cu1 Cu2 O5A C16A -1.4(5) . . . . ? Cu1 O4A C16A O5A 4.6(9) . . . . ? Cu1 O4A C16A C13A -177.5(4) . . . . ? Cu2 O5A C16A O4A -1.4(10) . . . . ? Cu2 O5A C16A C13A -179.3(4) . . . . ? C1A N1A C13A C16A 52.8(9) . . . . ? C5A N1A C13A C16A -124.4(8) . . . . ? C1A N1A C13A C14A -74.5(9) . . . . ? C5A N1A C13A C14A 108.3(9) . . . . ? O4A C16A C13A N1A 34.3(8) . . . . ? O5A C16A C13A N1A -147.6(6) . . . . ? O4A C16A C13A C14A 160.6(6) . . . . ? O5A C16A C13A C14A -21.4(10) . . . . ? N1A C13A C14A C15A -157.9(7) . . . . ? C16A C13A C14A C15A 77.7(9) . . . . ? C13A C14A C15A O3A 174.1(7) . . . . ? C13A C14A C15A N2A -7.1(12) . . . . ? N2A C15A O3A Cu4 -16.8(12) . . . . ? C14A C15A O3A Cu4 162.0(5) . . . . ? O5H Cu4 O3A C15A 38.8(7) . . . . ? O5F Cu4 O3A C15A -137.7(7) . . . . ? O5E Cu4 O3A C15A -51.3(7) . . . . ? O5G Cu4 O3A C15A 127.1(7) . . . . ? O1B C1B C2B C6B 0.1(13) . . . . ? N1B C1B C2B C6B 174.9(8) . . . . ? O1B C1B C2B C3B 179.2(8) . . . . ? N1B C1B C2B C3B -6.0(11) . . . . ? C6B C2B C3B C4B -176.0(10) . . . . ? C1B C2B C3B C4B 5.0(14) . . . . ? C6B C2B C3B C9B -3.9(14) . . . . ? C1B C2B C3B C9B 177.0(8) . . . . ? C2B C3B C4B C12B 178.4(9) . . . . ? C9B C3B C4B C12B 6.4(14) . . . . ? C2B C3B C4B C5B -3.2(14) . . . . ? C9B C3B C4B C5B -175.2(8) . . . . ? C3B C4B C5B O2B 179.9(9) . . . . ? C12B C4B C5B O2B -1.7(13) . . . . ? C3B C4B C5B N1B 2.3(12) . . . . ? C12B C4B C5B N1B -179.3(7) . . . . ? C3B C2B C6B C7B 2.2(16) . . . . ? C1B C2B C6B C7B -178.7(9) . . . . ? C2B C6B C7B C8B -2.3(18) . . . . ? C6B C7B C8B C9B 4(2) . . . . ? C7B C8B C9B C10B 173.7(12) . . . . ? C7B C8B C9B C3B -5.9(18) . . . . ? C4B C3B C9B C8B 178.0(10) . . . . ? C2B C3B C9B C8B 5.5(14) . . . . ? C4B C3B C9B C10B -1.6(14) . . . . ? C2B C3B C9B C10B -174.1(9) . . . . ? C8B C9B C10B C11B 178.0(12) . . . . ? C3B C9B C10B C11B -2.4(16) . . . . ? C9B C10B C11B C12B 1.8(18) . . . . ? C3B C4B C12B C11B -7.1(14) . . . . ? C5B C4B C12B C11B 174.5(8) . . . . ? C10B C11B C12B C4B 2.9(15) . . . . ? O1B C1B N1B C5B -179.4(7) . . . . ? C2B C1B N1B C5B 5.7(11) . . . . ? O1B C1B N1B C13B -3.8(10) . . . . ? C2B C1B N1B C13B -178.7(6) . . . . ? O2B C5B N1B C1B 178.6(7) . . . . ? C4B C5B N1B C1B -3.8(11) . . . . ? O2B C5B N1B C13B 3.0(11) . . . . ? C4B C5B N1B C13B -179.3(6) . . . . ? C14B C13B N1B C1B -74.6(7) . . . . ? C16B C13B N1B C1B 52.4(8) . . . . ? C14B C13B N1B C5B 101.2(7) . . . . ? C16B C13B N1B C5B -131.8(6) . . . . ? N1B C13B C14B C15B -164.7(5) . . . . ? C16B C13B C14B C15B 70.6(7) . . . . ? C13B C14B C15B O3B 29.7(9) . . . . ? C13B C14B C15B N2B -149.7(6) . . . . ? N1B C13B C16B O5B -137.3(5) . . . . ? C14B C13B C16B O5B -12.5(8) . . . . ? N1B C13B C16B O4B 46.0(7) . . . . ? C14B C13B C16B O4B 170.8(5) . . . . ? O5B C16B O4B Cu1 -0.2(9) . . . . ? C13B C16B O4B Cu1 176.2(4) . . . . ? O4A Cu1 O4B C16B -90.1(5) . . . . ? O4C Cu1 O4B C16B 85.9(5) . . . . ? O4D Cu1 O4B C16B -5.0(8) . . . . ? N3J Cu1 O4B C16B 175.2(6) . . . . ? N3I Cu1 O4B C16B -179.3(6) . . . . ? Cu2 Cu1 O4B C16B -0.1(5) . . . . ? O4B C16B O5B Cu2 0.5(8) . . . . ? C13B C16B O5B Cu2 -176.0(4) . . . . ? O5C Cu2 O5B C16B -80.0(4) . . . . ? O5A Cu2 O5B C16B 76.0(4) . . . . ? O3E Cu2 O5B C16B 169.7(4) . . . . ? Cu1 Cu2 O5B C16B -0.4(4) . . . . ? O1C C1C C2C C3C -175.8(10) . . . . ? N1C C1C C2C C3C 2.5(15) . . . . ? O1C C1C C2C C6C 6.5(15) . . . . ? N1C C1C C2C C6C -175.2(9) . . . . ? C6C C2C C3C C4C 177.4(10) . . . . ? C1C C2C C3C C4C -0.2(16) . . . . ? C6C C2C C3C C9C -0.5(16) . . . . ? C1C C2C C3C C9C -178.1(9) . . . . ? C2C C3C C4C C12C 179.0(10) . . . . ? C9C C3C C4C C12C -3.2(17) . . . . ? C2C C3C C4C C5C 4.2(16) . . . . ? C9C C3C C4C C5C -178.0(9) . . . . ? C3C C4C C5C O2C 176.1(10) . . . . ? C12C C4C C5C O2C 1.0(16) . . . . ? C3C C4C C5C N1C -10.4(15) . . . . ? C12C C4C C5C N1C 174.6(9) . . . . ? C3C C2C C6C C7C 3.9(16) . . . . ? C1C C2C C6C C7C -178.5(9) . . . . ? C2C C6C C7C C8C -3.4(15) . . . . ? C6C C7C C8C C9C -0.7(18) . . . . ? C7C C8C C9C C10C 177.7(12) . . . . ? C7C C8C C9C C3C 3.9(18) . . . . ? C4C C3C C9C C8C 179.1(10) . . . . ? C2C C3C C9C C8C -3.0(14) . . . . ? C4C C3C C9C C10C 3.8(15) . . . . ? C2C C3C C9C C10C -178.2(9) . . . . ? C8C C9C C10C C11C -176.4(12) . . . . ? C3C C9C C10C C11C -2.6(16) . . . . ? C9C C10C C11C C12C 0.3(18) . . . . ? C3C C4C C12C C11C 0.7(15) . . . . ? C5C C4C C12C C11C 175.7(9) . . . . ? C10C C11C C12C C4C 0.7(15) . . . . ? O1C C1C N1C C5C 168.9(9) . . . . ? C2C C1C N1C C5C -9.4(15) . . . . ? O1C C1C N1C C13C 1.9(15) . . . . ? C2C C1C N1C C13C -176.4(9) . . . . ? O2C C5C N1C C1C -173.0(9) . . . . ? C4C C5C N1C C1C 13.2(14) . . . . ? O2C C5C N1C C13C -5.9(14) . . . . ? C4C C5C N1C C13C -179.7(9) . . . . ? C16C C13C N1C C1C 59.2(11) . . . . ? C14C C13C N1C C1C -65.5(11) . . . . ? C16C C13C N1C C5C -108.5(9) . . . . ? C14C C13C N1C C5C 126.8(9) . . . . ? N1C C13C C14C C15C -46.2(10) . . . . ? C16C C13C C14C C15C -170.4(7) . . . . ? C13C C14C C15C O3C -48.7(10) . . . . ? C13C C14C C15C N2C 128.6(8) . . . . ? N1C C13C C16C O5C -157.2(7) . . . . ? C14C C13C C16C O5C -32.2(10) . . . . ? N1C C13C C16C O4C 25.4(10) . . . . ? C14C C13C C16C O4C 150.3(6) . . . . ? O5C C16C O4C Cu1 12.1(9) . . . . ? C13C C16C O4C Cu1 -170.7(5) . . . . ? O4B Cu1 O4C C16C -86.4(5) . . . . ? O4D Cu1 O4C C16C 70.0(5) . . . . ? N3J Cu1 O4C C16C 173.5(6) . . . . ? N3I Cu1 O4C C16C 176.5(6) . . . . ? Cu2 Cu1 O4C C16C -7.6(5) . . . . ? O4C C16C O5C Cu2 -9.1(9) . . . . ? C13C C16C O5C Cu2 173.8(5) . . . . ? O5D Cu2 O5C C16C -87.2(5) . . . . ? O5B Cu2 O5C C16C 89.3(5) . . . . ? O5A Cu2 O5C C16C 0.0(8) . . . . ? O3E Cu2 O5C C16C -175.8(5) . . . . ? Cu1 Cu2 O5C C16C 2.1(5) . . . . ? O1D C1D C2D C6D 1.2(14) . . . . ? N1D C1D C2D C6D -176.6(9) . . . . ? O1D C1D C2D C3D -177.3(8) . . . . ? N1D C1D C2D C3D 4.9(12) . . . . ? C6D C2D C3D C4D 177.0(10) . . . . ? C1D C2D C3D C4D -4.5(14) . . . . ? C6D C2D C3D C9D -4.1(15) . . . . ? C1D C2D C3D C9D 174.3(9) . . . . ? C2D C3D C4D C12D 178.9(9) . . . . ? C9D C3D C4D C12D 0.1(16) . . . . ? C2D C3D C4D C5D 4.4(15) . . . . ? C9D C3D C4D C5D -174.4(9) . . . . ? C3D C4D C5D O2D 178.6(10) . . . . ? C12D C4D C5D O2D 4.0(16) . . . . ? C3D C4D C5D N1D -4.5(14) . . . . ? C12D C4D C5D N1D -179.1(8) . . . . ? C3D C2D C6D C7D 0.9(17) . . . . ? C1D C2D C6D C7D -177.5(10) . . . . ? C2D C6D C7D C8D 1(2) . . . . ? C6D C7D C8D C9D 1(2) . . . . ? C7D C8D C9D C3D -5(2) . . . . ? C7D C8D C9D C10D 177.4(13) . . . . ? C4D C3D C9D C8D -175.4(11) . . . . ? C2D C3D C9D C8D 5.7(16) . . . . ? C4D C3D C9D C10D 2.9(15) . . . . ? C2D C3D C9D C10D -175.9(9) . . . . ? C8D C9D C10D C11D 178.0(13) . . . . ? C3D C9D C10D C11D -0.1(17) . . . . ? C9D C10D C11D C12D -5.4(18) . . . . ? C3D C4D C12D C11D -5.5(15) . . . . ? C5D C4D C12D C11D 169.2(9) . . . . ? C10D C11D C12D C4D 8.3(16) . . . . ? O1D C1D N1D C5D 176.7(7) . . . . ? C2D C1D N1D C5D -5.4(12) . . . . ? O1D C1D N1D C13D 0.6(11) . . . . ? C2D C1D N1D C13D 178.5(7) . . . . ? O2D C5D N1D C1D -177.8(9) . . . . ? C4D C5D N1D C1D 5.1(12) . . . . ? O2D C5D N1D C13D -1.7(12) . . . . ? C4D C5D N1D C13D -178.8(7) . . . . ? C16D C13D N1D C1D 55.9(9) . . . . ? C14D C13D N1D C1D -69.1(10) . . . . ? C16D C13D N1D C5D -120.5(8) . . . . ? C14D C13D N1D C5D 114.6(9) . . . . ? N1D C13D C14D C15D -59.6(12) . . . . ? C16D C13D C14D C15D 176.2(9) . . . . ? C13D C14D C15D O3D 77.1(15) . . . . ? C13D C14D C15D N2D -106.5(11) . . . . ? N1D C13D C16D O5D -143.1(6) . . . . ? C14D C13D C16D O5D -16.9(10) . . . . ? N1D C13D C16D O4D 40.3(9) . . . . ? C14D C13D C16D O4D 166.5(7) . . . . ? O5D C16D O4D Cu1 5.2(10) . . . . ? C13D C16D O4D Cu1 -178.5(5) . . . . ? O4A Cu1 O4D C16D 88.1(6) . . . . ? O4C Cu1 O4D C16D -88.3(6) . . . . ? O4B Cu1 O4D C16D 2.5(8) . . . . ? N3J Cu1 O4D C16D -177.7(6) . . . . ? N3I Cu1 O4D C16D 176.6(6) . . . . ? Cu2 Cu1 O4D C16D -2.5(5) . . . . ? O4D C16D O5D Cu2 -4.8(10) . . . . ? C13D C16D O5D Cu2 178.8(5) . . . . ? O5C Cu2 O5D C16D 81.9(5) . . . . ? O5A Cu2 O5D C16D -74.1(5) . . . . ? O3E Cu2 O5D C16D -168.0(5) . . . . ? Cu1 Cu2 O5D C16D 2.2(5) . . . . ? O1E C1E C2E C6E -4.8(8) . . . . ? N1E C1E C2E C6E 178.7(6) . . . . ? O1E C1E C2E C3E 174.6(5) . . . . ? N1E C1E C2E C3E -1.9(6) . . . . ? C6E C2E C3E C4E 179.8(7) . . . . ? C1E C2E C3E C4E 0.3(7) . . . . ? C6E C2E C3E C9E 1.1(8) . . . . ? C1E C2E C3E C9E -178.3(6) . . . . ? C2E C3E C4E C12E -179.9(6) . . . . ? C9E C3E C4E C12E -1.2(11) . . . . ? C2E C3E C4E C5E 0.8(10) . . . . ? C9E C3E C4E C5E 179.4(7) . . . . ? C3E C4E C5E O2E -178.3(7) . . . . ? C12E C4E C5E O2E 2.3(11) . . . . ? C3E C4E C5E N1E -0.2(10) . . . . ? C12E C4E C5E N1E -179.6(7) . . . . ? C3E C2E C6E C7E -0.3(10) . . . . ? C1E C2E C6E C7E 179.2(6) . . . . ? C2E C6E C7E C8E -0.7(12) . . . . ? C6E C7E C8E C9E 0.7(14) . . . . ? C7E C8E C9E C10E 178.9(9) . . . . ? C7E C8E C9E C3E 0.2(13) . . . . ? C4E C3E C9E C8E -179.8(7) . . . . ? C2E C3E C9E C8E -1.1(10) . . . . ? C4E C3E C9E C10E 1.4(10) . . . . ? C2E C3E C9E C10E -179.9(6) . . . . ? C8E C9E C10E C11E 179.2(9) . . . . ? C3E C9E C10E C11E -2.1(13) . . . . ? C9E C10E C11E C12E 2.4(15) . . . . ? C3E C4E C12E C11E 1.5(12) . . . . ? C5E C4E C12E C11E -179.1(8) . . . . ? C10E C11E C12E C4E -2.1(14) . . . . ? O1E C1E N1E C5E -174.1(6) . . . . ? C2E C1E N1E C5E 2.5(8) . . . . ? O1E C1E N1E C13E -0.3(8) . . . . ? C2E C1E N1E C13E 176.3(5) . . . . ? O2E C5E N1E C1E 176.7(6) . . . . ? C4E C5E N1E C1E -1.5(9) . . . . ? O2E C5E N1E C13E 2.9(10) . . . . ? C4E C5E N1E C13E -175.3(6) . . . . ? C16E C13E N1E C1E 54.1(8) . . . . ? C14E C13E N1E C1E -66.1(7) . . . . ? C16E C13E N1E C5E -131.6(6) . . . . ? C14E C13E N1E C5E 108.2(7) . . . . ? N1E C13E C14E C15E -167.0(7) . . . . ? C16E C13E C14E C15E 69.9(9) . . . . ? C13E C14E C15E O3E 75.7(11) . . . . ? C13E C14E C15E N2E -112.1(9) . . . . ? N1E C13E C16E O5E -159.5(6) . . . . ? C14E C13E C16E O5E -38.6(8) . . . . ? N1E C13E C16E O4E 26.5(9) . . . . ? C14E C13E C16E O4E 147.4(6) . . . . ? N2E C15E O3E Cu2 -6.9(12) . . . . ? C14E C15E O3E Cu2 165.0(6) . . . . ? O5D Cu2 O3E C15E 131.3(7) . . . . ? O5B Cu2 O3E C15E -46.3(7) . . . . ? O5C Cu2 O3E C15E -140.2(7) . . . . ? O5A Cu2 O3E C15E 41.5(7) . . . . ? O5E C16E O4E Cu3 8.1(9) . . . . ? C13E C16E O4E Cu3 -179.0(4) . . . . ? O4H Cu3 O4E C16E -88.0(5) . . . . ? O4F Cu3 O4E C16E 77.2(5) . . . . ? O38 Cu3 O4E C16E 168.0(5) . . . . ? Cu4 Cu3 O4E C16E -3.1(4) . . . . ? O4E C16E O5E Cu4 -9.3(10) . . . . ? C13E C16E O5E Cu4 177.7(4) . . . . ? O5H Cu4 O5E C16E 88.1(5) . . . . ? O5F Cu4 O5E C16E -84.4(5) . . . . ? O5G Cu4 O5E C16E 12.7(11) . . . . ? O3A Cu4 O5E C16E -173.5(5) . . . . ? Cu3 Cu4 O5E C16E 4.5(5) . . . . ? O1F C1F C2F C3F -176.3(7) . . . . ? N1F C1F C2F C3F 6.6(11) . . . . ? O1F C1F C2F C6F 3.4(12) . . . . ? N1F C1F C2F C6F -173.7(7) . . . . ? C6F C2F C3F C4F 179.1(8) . . . . ? C1F C2F C3F C4F -1.3(12) . . . . ? C6F C2F C3F C9F -0.8(13) . . . . ? C1F C2F C3F C9F 178.8(7) . . . . ? C2F C3F C4F C12F -177.6(8) . . . . ? C9F C3F C4F C12F 2.3(12) . . . . ? C2F C3F C4F C5F -6.4(11) . . . . ? C9F C3F C4F C5F 173.5(7) . . . . ? C12F C4F C5F O2F 0.7(12) . . . . ? C3F C4F C5F O2F -170.9(7) . . . . ? C12F C4F C5F N1F 179.9(7) . . . . ? C3F C4F C5F N1F 8.4(10) . . . . ? C3F C2F C6F C7F 0.2(14) . . . . ? C1F C2F C6F C7F -179.5(9) . . . . ? C2F C6F C7F C8F 0.1(15) . . . . ? C6F C7F C8F C9F 0.2(16) . . . . ? C7F C8F C9F C10F -179.8(10) . . . . ? C7F C8F C9F C3F -0.9(15) . . . . ? C2F C3F C9F C8F 1.1(12) . . . . ? C4F C3F C9F C8F -178.8(8) . . . . ? C2F C3F C9F C10F -179.8(8) . . . . ? C4F C3F C9F C10F 0.3(11) . . . . ? C8F C9F C10F C11F 178.6(10) . . . . ? C3F C9F C10F C11F -0.4(14) . . . . ? C9F C10F C11F C12F -2.1(17) . . . . ? C3F C4F C12F C11F -4.6(13) . . . . ? C5F C4F C12F C11F -175.9(8) . . . . ? C10F C11F C12F C4F 4.6(15) . . . . ? O1F C1F N1F C5F 178.4(6) . . . . ? C2F C1F N1F C5F -4.4(10) . . . . ? O1F C1F N1F C13F -4.1(9) . . . . ? C2F C1F N1F C13F 173.1(6) . . . . ? O2F C5F N1F C1F 176.4(7) . . . . ? C4F C5F N1F C1F -2.9(10) . . . . ? O2F C5F N1F C13F -1.1(9) . . . . ? C4F C5F N1F C13F 179.6(6) . . . . ? C16F C13F N1F C1F 57.0(7) . . . . ? C14F C13F N1F C1F -69.4(7) . . . . ? C16F C13F N1F C5F -125.3(6) . . . . ? C14F C13F N1F C5F 108.3(6) . . . . ? N1F C13F C14F C15F -160.5(5) . . . . ? C16F C13F C14F C15F 72.9(7) . . . . ? C13F C14F C15F O3F 38.5(8) . . . . ? C13F C14F C15F N2F -140.9(6) . . . . ? N1F C13F C16F O4F 44.8(7) . . . . ? C14F C13F C16F O4F 169.5(5) . . . . ? N1F C13F C16F O5F -141.5(5) . . . . ? C14F C13F C16F O5F -16.8(8) . . . . ? O5F C16F O4F Cu3 -16.6(8) . . . . ? C13F C16F O4F Cu3 156.6(4) . . . . ? O4G Cu3 O4F C16F 95.0(5) . . . . ? O4E Cu3 O4F C16F -76.6(5) . . . . ? O4H Cu3 O4F C16F 2.7(10) . . . . ? O38 Cu3 O4F C16F -168.1(5) . . . . ? Cu4 Cu3 O4F C16F 11.9(4) . . . . ? O4F C16F O5F Cu4 9.0(8) . . . . ? C13F C16F O5F Cu4 -164.1(4) . . . . ? O5E Cu4 O5F C16F 81.1(4) . . . . ? O5G Cu4 O5F C16F -84.9(4) . . . . ? O3A Cu4 O5F C16F 179.3(4) . . . . ? Cu3 Cu4 O5F C16F 0.1(4) . . . . ? O1H C1H C2H C6H 1.7(13) . . . . ? N1H C1H C2H C6H -174.0(8) . . . . ? O1H C1H C2H C3H -179.5(7) . . . . ? N1H C1H C2H C3H 4.9(11) . . . . ? C6H C2H C3H C4H -179.2(8) . . . . ? C1H C2H C3H C4H 1.9(12) . . . . ? C6H C2H C3H C9H -2.0(13) . . . . ? C1H C2H C3H C9H 179.2(8) . . . . ? C2H C3H C4H C12H -180.0(9) . . . . ? C9H C3H C4H C12H 2.9(14) . . . . ? C2H C3H C4H C5H -3.3(13) . . . . ? C9H C3H C4H C5H 179.6(8) . . . . ? C12H C4H C5H O2H -6.4(14) . . . . ? C3H C4H C5H O2H 176.9(8) . . . . ? C12H C4H C5H N1H 174.8(8) . . . . ? C3H C4H C5H N1H -1.9(12) . . . . ? C3H C2H C6H C7H 1.8(14) . . . . ? C1H C2H C6H C7H -179.4(9) . . . . ? C2H C6H C7H C8H -0.4(16) . . . . ? C6H C7H C8H C9H -0.8(18) . . . . ? C7H C8H C9H C10H -178.4(11) . . . . ? C7H C8H C9H C3H 0.5(17) . . . . ? C4H C3H C9H C8H 178.1(10) . . . . ? C2H C3H C9H C8H 0.9(14) . . . . ? C4H C3H C9H C10H -2.9(14) . . . . ? C2H C3H C9H C10H 179.9(9) . . . . ? C8H C9H C10H C11H -180.0(11) . . . . ? C3H C9H C10H C11H 1.1(17) . . . . ? C9H C10H C11H C12H 0.7(18) . . . . ? C3H C4H C12H C11H -1.0(14) . . . . ? C5H C4H C12H C11H -177.7(8) . . . . ? C10H C11H C12H C4H -0.8(15) . . . . ? O1H C1H N1H C5H 173.6(7) . . . . ? C2H C1H N1H C5H -10.5(11) . . . . ? O1H C1H N1H C13H 0.2(10) . . . . ? C2H C1H N1H C13H 176.0(7) . . . . ? O2H C5H N1H C1H -170.1(7) . . . . ? C4H C5H N1H C1H 8.8(11) . . . . ? O2H C5H N1H C13H 3.2(11) . . . . ? C4H C5H N1H C13H -177.9(7) . . . . ? C16H C13H N1H C1H 51.6(8) . . . . ? C14H C13H N1H C1H -77.5(8) . . . . ? C16H C13H N1H C5H -121.9(7) . . . . ? C14H C13H N1H C5H 108.9(8) . . . . ? N1H C13H C14H C15H -64.6(11) . . . . ? C16H C13H C14H C15H 166.5(9) . . . . ? C13H C14H C15H O3H -52.0(15) . . . . ? C13H C14H C15H N2H 119.3(12) . . . . ? N1H C13H C16H O4H 51.7(9) . . . . ? C14H C13H C16H O4H 178.5(7) . . . . ? N1H C13H C16H O5H -128.2(7) . . . . ? C14H C13H C16H O5H -1.3(10) . . . . ? O5H C16H O4H Cu3 -1.7(10) . . . . ? C13H C16H O4H Cu3 178.5(4) . . . . ? O4G Cu3 O4H C16H -80.0(5) . . . . ? O4E Cu3 O4H C16H 93.0(5) . . . . ? O4F Cu3 O4H C16H 13.2(10) . . . . ? O38 Cu3 O4H C16H -176.4(5) . . . . ? Cu4 Cu3 O4H C16H 4.1(5) . . . . ? O4H C16H O5H Cu4 -3.5(10) . . . . ? C13H C16H O5H Cu4 176.3(4) . . . . ? O5E Cu4 O5H C16H -76.0(5) . . . . ? O5G Cu4 O5H C16H 90.3(5) . . . . ? O3A Cu4 O5H C16H -174.1(5) . . . . ? Cu3 Cu4 O5H C16H 4.9(5) . . . . ? O4A Cu1 N3I C21I -22.3(7) . . . . ? O4C Cu1 N3I C21I 158.3(7) . . . . ? O4B Cu1 N3I C21I 67.9(7) . . . . ? O4D Cu1 N3I C21I -109.7(7) . . . . ? N3J Cu1 N3I C21I -173(8) . . . . ? O4A Cu1 N3I C25I 160.9(7) . . . . ? O4C Cu1 N3I C25I -18.5(7) . . . . ? O4B Cu1 N3I C25I -108.9(7) . . . . ? O4D Cu1 N3I C25I 73.5(7) . . . . ? Cu1 N3I C21I C22I -176.8(10) . . . . ? N3I C21I C22I C23I 0.0 . . . . ? C21I C22I C23I C24I 0.0 . . . . ? C22I C23I C24I C25I 0.0 . . . . ? C23I C24I C25I N3I 0.0 . . . . ? C21I N3I C25I C24I 0.0 . . . . ? Cu1 N3I C25I C24I 176.8(10) . . . . ? O4A Cu1 N3J C21J -11.3(7) . . . . ? O4C Cu1 N3J C21J 169.5(7) . . . . ? O4B Cu1 N3J C21J 79.8(7) . . . . ? O4D Cu1 N3J C21J -100.1(7) . . . . ? O4A Cu1 N3J C25J 161.0(6) . . . . ? O4C Cu1 N3J C25J -18.2(6) . . . . ? O4B Cu1 N3J C25J -107.8(6) . . . . ? O4D Cu1 N3J C25J 72.2(7) . . . . ? N3I Cu1 N3J C25J -170(8) . . . . ? C25J N3J C21J C22J 0.0 . . . . ? Cu1 N3J C21J C22J 172.2(10) . . . . ? N3J C21J C22J C23J 0.0 . . . . ? C21J C22J C23J C24J 0.0 . . . . ? C22J C23J C24J C25J 0.0 . . . . ? C23J C24J C25J N3J 0.0 . . . . ? C21J N3J C25J C24J 0.0 . . . . ? Cu1 N3J C25J C24J -172.4(10) . . . . ? O4G Cu3 O38 C34 160.6(6) . . . . ? O4E Cu3 O38 C34 -24.1(7) . . . . ? O4H Cu3 O38 C34 -110.8(7) . . . . ? O4F Cu3 O38 C34 66.7(7) . . . . ? C32 O37 C31 O36 -8.2(18) . . . . ? C32 O37 C31 C34 169.3(11) . . . . ? C31 O37 C32 C33 157.4(13) . . . . ? Cu3 O38 C34 C31 148.5(7) . . . . ? Cu3 O38 C34 C35 -81.7(11) . . . . ? O36 C31 C34 O38 -156.8(12) . . . . ? O37 C31 C34 O38 25.8(13) . . . . ? O36 C31 C34 C35 73.7(17) . . . . ? O37 C31 C34 C35 -103.8(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2A H2A1 O5H 0.88 2.25 3.035(9) 149.2 . N2A H2A2 O1D 0.88 2.27 3.092(9) 154.6 . N2B H2B1 O3F 0.88 2.05 2.919(8) 171.5 . N2E H2E1 O5A 0.88 2.22 2.937(9) 138.0 . N2E H2E2 O3F 0.88 2.35 3.109(9) 144.9 . N2F H2F1 O3B 0.88 2.02 2.881(8) 166.6 . N2H H2H2 O3D 0.88 2.21 2.965(18) 143.5 . N2G H2G1 O1C 0.88 2.03 2.898(12) 169.8 1_455 N2F H2F2 O3C 0.88 2.07 2.933(8) 166.7 1_455 N2C H2C2 O3G 0.88 2.15 3.026(10) 171.0 1_655 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.859 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.104 _vrf_PLAT201_7 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 192 RESPONSE: Only the copper atoms refined anisotropically due to extensive disorder and moderate crystallinity. ; _vrf_PLAT602_7 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The voids are not empty but filled with disordered guest species which could not be modeled. They were accounted for with the Squeeze program. ; #===END data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C138 H103 Cu4 N17 O43' _chemical_formula_sum 'C138 H103 Cu4 N17 O43' _chemical_formula_weight 2941.53 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.1728(15) _cell_length_b 21.670(2) _cell_length_c 52.697(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17327(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1470 _cell_measurement_theta_min 2.149 _cell_measurement_theta_max 19.740 _exptl_crystal_description 'rectanglur bar' _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6040 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75115 _diffrn_reflns_av_R_equivalents 0.2005 _diffrn_reflns_av_sigmaI/netI 0.2089 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 18.00 _reflns_number_total 11917 _reflns_number_gt 6196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_number_reflns 11917 _refine_ls_number_parameters 742 _refine_ls_number_restraints 1041 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.1814 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.865 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.96585(14) 0.42331(11) 0.30566(4) 0.0486(7) Uani 1 1 d D . . Cu2 Cu 0.93582(15) 0.41252(11) 0.35582(4) 0.0546(8) Uani 1 1 d . B . Cu3 Cu 0.55385(14) 0.54477(10) 0.45881(4) 0.0420(7) Uani 1 1 d . A . Cu4 Cu 0.57589(14) 0.52072(10) 0.41078(4) 0.0392(7) Uani 1 1 d D . . C1G C 0.4273(10) 0.7295(6) 0.4291(3) 0.065(6) Uiso 1 1 d D . . C2G C 0.4254(9) 0.7926(6) 0.4403(3) 0.057(6) Uiso 1 1 d D . . C3G C 0.3584(9) 0.8105(7) 0.4550(3) 0.072(3) Uiso 1 1 d D . . C4G C 0.2862(9) 0.7767(6) 0.4568(3) 0.062(6) Uiso 1 1 d D . . C5G C 0.2741(10) 0.7178(7) 0.4446(3) 0.073(7) Uiso 1 1 d D . . C6G C 0.5034(10) 0.8232(7) 0.4373(3) 0.072(3) Uiso 1 1 d D . . H6G H 0.5502 0.8070 0.4274 0.087 Uiso 1 1 calc R . . C7G C 0.5104(10) 0.8830(7) 0.4504(3) 0.072(3) Uiso 1 1 d D . . H7G H 0.5617 0.9081 0.4494 0.087 Uiso 1 1 calc R . . C8G C 0.4387(10) 0.8996(7) 0.4639(3) 0.072(3) Uiso 1 1 d D . . H8G H 0.4417 0.9400 0.4708 0.087 Uiso 1 1 calc R . . C9G C 0.3643(10) 0.8696(7) 0.4692(3) 0.072(3) Uiso 1 1 d D . . C10G C 0.2915(11) 0.8807(7) 0.4825(3) 0.072(3) Uiso 1 1 d D . . H10G H 0.2933 0.9169 0.4926 0.087 Uiso 1 1 calc R . . C11G C 0.2194(11) 0.8501(7) 0.4837(3) 0.080(7) Uiso 1 1 d D . . H11G H 0.1717 0.8649 0.4937 0.096 Uiso 1 1 calc R . . C12G C 0.2110(10) 0.7937(7) 0.4700(3) 0.076(7) Uiso 1 1 d D . . H12G H 0.1585 0.7699 0.4699 0.091 Uiso 1 1 calc R . . C13G C 0.3503(10) 0.6328(6) 0.4197(3) 0.037(5) Uiso 1 1 d D . . H13G H 0.2971 0.6113 0.4265 0.044 Uiso 1 1 calc R . . N1G N 0.3532(8) 0.6938(6) 0.4316(2) 0.049(5) Uiso 1 1 d D . . O1G O 0.4865(7) 0.7099(5) 0.4154(2) 0.056(4) Uiso 1 1 d D . . O2G O 0.2147(8) 0.6800(6) 0.4447(2) 0.073(4) Uiso 1 1 d D . . C14G C 0.3293(15) 0.6484(10) 0.3893(4) 0.098(8) Uiso 1 1 d . . . H14O H 0.2859 0.6824 0.3882 0.117 Uiso 1 1 calc R . . H14P H 0.3842 0.6622 0.3808 0.117 Uiso 1 1 calc R . . C15G C 0.2933(14) 0.5920(11) 0.3756(4) 0.080(7) Uiso 1 1 d . . . C16G C 0.4256(13) 0.5904(9) 0.4231(4) 0.057(6) Uiso 1 1 d . . . N2G N 0.3126(11) 0.5872(9) 0.3519(4) 0.114(7) Uiso 1 1 d . . . H2G1 H 0.3030 0.5522 0.3438 0.137 Uiso 1 1 calc R . . H2G2 H 0.3353 0.6189 0.3437 0.137 Uiso 1 1 calc R . . O3G O 0.2613(10) 0.5463(7) 0.3866(3) 0.096(5) Uiso 1 1 d . . . O4G O 0.4480(7) 0.5855(5) 0.4466(2) 0.042(3) Uiso 1 1 d . A . O5G O 0.4578(7) 0.5620(5) 0.4061(2) 0.043(3) Uiso 1 1 d . . . C1A C 0.6875(11) 0.3896(10) 0.2832(4) 0.135(3) Uiso 1 1 d D A . C2A C 0.6747(8) 0.3721(9) 0.2558(3) 0.135(3) Uiso 1 1 d D . . C3A C 0.6563(8) 0.4153(7) 0.2390(3) 0.135(3) Uiso 1 1 d D . . C4A C 0.6475(16) 0.4738(8) 0.2460(4) 0.135(3) Uiso 1 1 d D . . C5A C 0.6625(17) 0.4972(11) 0.2712(4) 0.135(3) Uiso 1 1 d D A . C6A C 0.6866(15) 0.3094(9) 0.2525(4) 0.135(3) Uiso 1 1 d D . . H6A H 0.7037 0.2830 0.2660 0.162 Uiso 1 1 calc R . . C7A C 0.6710(15) 0.2860(9) 0.2265(4) 0.135(3) Uiso 1 1 d D . . H7A H 0.6691 0.2437 0.2219 0.162 Uiso 1 1 calc R . . C8A C 0.6596(15) 0.3336(10) 0.2101(4) 0.135(3) Uiso 1 1 d D . . H8A H 0.6608 0.3206 0.1929 0.162 Uiso 1 1 calc R . . C9A C 0.6472(16) 0.3942(10) 0.2123(4) 0.135(3) Uiso 1 1 d D . . C10A C 0.6311(15) 0.4434(10) 0.1985(4) 0.135(3) Uiso 1 1 d D . . H10A H 0.6294 0.4352 0.1808 0.162 Uiso 1 1 calc R . . C11A C 0.6173(15) 0.4999(10) 0.2040(4) 0.135(3) Uiso 1 1 d D . . H11A H 0.5988 0.5276 0.1911 0.162 Uiso 1 1 calc R . . C12A C 0.6293(15) 0.5224(9) 0.2296(4) 0.135(3) Uiso 1 1 d D . . H12A H 0.6254 0.5645 0.2345 0.162 Uiso 1 1 calc R . . N1A N 0.6787(13) 0.4560(6) 0.2892(4) 0.135(3) Uiso 1 1 d D . . O1A O 0.7036(11) 0.3570(7) 0.3001(3) 0.135(3) Uiso 1 1 d D . . O2A O 0.6516(11) 0.5546(7) 0.2782(3) 0.135(3) Uiso 1 1 d D . . O4A O 0.8490(8) 0.4572(5) 0.3022(2) 0.063(4) Uiso 1 1 d . A . O5A O 0.8218(8) 0.4493(6) 0.3440(3) 0.073(4) Uiso 1 1 d . . . C16A C 0.7973(15) 0.4584(10) 0.3215(4) 0.083(8) Uiso 1 1 d . A . C13A C 0.7057(11) 0.4768(6) 0.3153(3) 0.051(3) Uiso 0.50 1 d PD A 3 H13A H 0.6975 0.5224 0.3173 0.061 Uiso 0.50 1 calc PR A 3 C14A C 0.646(2) 0.4409(15) 0.3338(4) 0.051(3) Uiso 0.50 1 d PD A 3 H14A H 0.5844 0.4483 0.3283 0.061 Uiso 0.50 1 calc PR A 3 H14B H 0.6579 0.3965 0.3311 0.061 Uiso 0.50 1 calc PR A 3 C15A C 0.649(2) 0.4516(11) 0.3621(4) 0.051(3) Uiso 0.50 1 d PD A 3 N2A N 0.6771(16) 0.4065(11) 0.3776(5) 0.051(3) Uiso 0.50 1 d PD A 3 H2A1 H 0.6734 0.4112 0.3942 0.061 Uiso 0.50 1 calc PR A 3 H2A2 H 0.6995 0.3725 0.3712 0.061 Uiso 0.50 1 calc PR A 3 O3A O 0.6180(15) 0.4978(12) 0.3733(3) 0.051(3) Uiso 0.50 1 d PD A 3 C13Z C 0.7057(11) 0.4768(6) 0.3153(3) 0.051(3) Uiso 0.50 1 d PD A 4 H13Z H 0.7098 0.5227 0.3135 0.061 Uiso 0.50 1 calc PR A 4 C14Z C 0.642(2) 0.4685(14) 0.3377(5) 0.051(3) Uiso 0.50 1 d PD A 4 H14Y H 0.5813 0.4692 0.3306 0.061 Uiso 0.50 1 calc PR A 4 H14Z H 0.6514 0.4264 0.3445 0.061 Uiso 0.50 1 calc PR A 4 C15Z C 0.6425(18) 0.5117(13) 0.3599(5) 0.051(3) Uiso 0.50 1 d PD A 4 N2Z N 0.7102(15) 0.5522(11) 0.3599(5) 0.051(3) Uiso 0.50 1 d PD A 4 H2Z1 H 0.7176 0.5775 0.3728 0.061 Uiso 0.50 1 calc PR A 4 H2Z2 H 0.7469 0.5533 0.3469 0.061 Uiso 0.50 1 calc PR A 4 O3Z O 0.5777(14) 0.4925(11) 0.3720(3) 0.051(3) Uiso 0.50 1 d PD A 4 C1B C 0.9918(10) 0.2020(9) 0.3125(3) 0.0789(17) Uiso 1 1 d D . . C2B C 1.0464(10) 0.1671(8) 0.2937(3) 0.0789(17) Uiso 1 1 d D . . C3B C 1.0085(10) 0.1348(9) 0.2753(3) 0.0789(17) Uiso 1 1 d D . . C4B C 0.9222(10) 0.1366(9) 0.2714(3) 0.0789(17) Uiso 1 1 d D . . C5B C 0.8603(10) 0.1680(8) 0.2884(3) 0.0789(17) Uiso 1 1 d D . . C6B C 1.1326(10) 0.1683(8) 0.2982(3) 0.0789(17) Uiso 1 1 d D . . H6B H 1.1565 0.1908 0.3121 0.095 Uiso 1 1 calc R . . C7B C 1.1885(11) 0.1335(8) 0.2809(3) 0.0789(17) Uiso 1 1 d D . . H7B H 1.2509 0.1321 0.2825 0.095 Uiso 1 1 calc R . . C8B C 1.1456(11) 0.1039(9) 0.2627(3) 0.0789(17) Uiso 1 1 d D . . H8B H 1.1829 0.0813 0.2516 0.095 Uiso 1 1 calc R . . C9B C 1.0621(10) 0.0997(8) 0.2571(3) 0.0789(17) Uiso 1 1 d D . . C10B C 1.0143(11) 0.0720(9) 0.2391(3) 0.0789(17) Uiso 1 1 d D . . H10B H 1.0473 0.0457 0.2283 0.095 Uiso 1 1 calc R . . C11B C 0.9319(11) 0.0743(8) 0.2339(3) 0.0789(17) Uiso 1 1 d D . . H11B H 0.9079 0.0558 0.2191 0.095 Uiso 1 1 calc R . . C12B C 0.8781(11) 0.1068(8) 0.2520(3) 0.0789(17) Uiso 1 1 d D . . H12B H 0.8156 0.1078 0.2507 0.095 Uiso 1 1 calc R . . C13B C 0.8507(12) 0.2490(9) 0.3239(4) 0.0789(17) Uiso 1 1 d D B . H13B H 0.7931 0.2567 0.3153 0.095 Uiso 1 1 calc R . . N1B N 0.9030(9) 0.2085(7) 0.3072(3) 0.0789(17) Uiso 1 1 d D . . O1B O 1.0246(8) 0.2330(6) 0.3298(2) 0.0789(17) Uiso 1 1 d D . . O2B O 0.7827(8) 0.1818(6) 0.2853(2) 0.0789(17) Uiso 1 1 d D . . C14B C 0.8307(12) 0.2137(9) 0.3488(3) 0.061(6) Uiso 1 1 d . . . H14C H 0.8130 0.1710 0.3446 0.073 Uiso 1 1 calc R . . H14D H 0.8852 0.2115 0.3591 0.073 Uiso 1 1 calc R . . C15B C 0.7577(17) 0.2436(11) 0.3648(5) 0.104(9) Uiso 1 1 d . . . C16B C 0.8894(11) 0.3053(9) 0.3280(4) 0.045(6) Uiso 1 1 d . . . N2B N 0.7730(11) 0.2413(7) 0.3885(3) 0.084(6) Uiso 1 1 d . . . H2B1 H 0.7397 0.2623 0.3991 0.100 Uiso 1 1 calc R . . H2B2 H 0.8168 0.2188 0.3943 0.100 Uiso 1 1 calc R . . O3B O 0.6987(10) 0.2733(7) 0.3543(3) 0.096(5) Uiso 1 1 d . . . O4B O 0.9146(7) 0.3374(5) 0.3076(2) 0.044(3) Uiso 1 1 d . B . O5B O 0.8917(7) 0.3336(5) 0.3491(2) 0.040(3) Uiso 1 1 d . B . C1C C 1.2606(15) 0.4481(8) 0.3099(4) 0.114(3) Uiso 1 1 d D . . C2C C 1.3078(15) 0.4663(8) 0.2859(3) 0.114(3) Uiso 1 1 d D . . C3C C 1.3459(15) 0.4230(8) 0.2716(4) 0.114(3) Uiso 1 1 d D . . C4C C 1.3419(15) 0.3641(8) 0.2770(4) 0.114(3) Uiso 1 1 d D . . C5C C 1.2907(15) 0.3383(8) 0.2979(4) 0.114(3) Uiso 1 1 d D . . C6C C 1.3132(14) 0.5275(8) 0.2823(4) 0.114(3) Uiso 1 1 d D . . H6C H 1.2921 0.5559 0.2946 0.137 Uiso 1 1 calc R . . C7C C 1.3546(14) 0.5486(8) 0.2579(4) 0.114(3) Uiso 1 1 d D . . H7C H 1.3505 0.5895 0.2515 0.137 Uiso 1 1 calc R . . C8C C 1.3989(14) 0.5017(8) 0.2459(4) 0.114(3) Uiso 1 1 d D . . H8C H 1.4431 0.5156 0.2345 0.137 Uiso 1 1 calc R . . C9C C 1.3919(15) 0.4408(8) 0.2472(4) 0.114(3) Uiso 1 1 d D . . C10C C 1.4247(15) 0.3926(9) 0.2338(4) 0.114(3) Uiso 1 1 d D . . H10C H 1.4539 0.4019 0.2184 0.137 Uiso 1 1 calc R . . C11C C 1.4200(15) 0.3355(9) 0.2401(4) 0.114(3) Uiso 1 1 d D . . H11C H 1.4413 0.3051 0.2287 0.137 Uiso 1 1 calc R . . C12C C 1.3836(14) 0.3163(8) 0.2639(4) 0.114(3) Uiso 1 1 d D . . H12C H 1.3873 0.2752 0.2701 0.137 Uiso 1 1 calc R . . C13C C 1.2059(15) 0.3649(10) 0.3376(4) 0.114(3) Uiso 1 1 d D B . H13C H 1.2113 0.3190 0.3387 0.137 Uiso 1 1 calc R . . N1C N 1.2578(12) 0.3863(7) 0.3155(3) 0.114(3) Uiso 1 1 d D . . O1C O 1.2219(8) 0.4856(6) 0.3236(2) 0.075(4) Uiso 1 1 d D . . O2C O 1.2821(10) 0.2872(6) 0.3060(3) 0.114(6) Uiso 1 1 d D . . C14C C 1.2376(15) 0.3946(11) 0.3645(4) 0.114(9) Uiso 1 1 d . . . H14E H 1.2232 0.4392 0.3649 0.137 Uiso 1 1 calc R . . H14F H 1.2057 0.3743 0.3787 0.137 Uiso 1 1 calc R . . C15C C 1.3384(15) 0.3857(12) 0.3681(4) 0.078(8) Uiso 1 1 d . . . C16C C 1.1085(12) 0.3812(8) 0.3349(4) 0.043(6) Uiso 1 1 d . . . N2C N 1.3811(10) 0.4341(7) 0.3753(3) 0.068(5) Uiso 1 1 d . . . H2C1 H 1.4389 0.4329 0.3768 0.081 Uiso 1 1 calc R . . H2C2 H 1.3525 0.4684 0.3788 0.081 Uiso 1 1 calc R . . O3C O 1.3677(11) 0.3370(8) 0.3628(3) 0.119(6) Uiso 1 1 d . . . O4C O 1.0810(8) 0.3921(5) 0.3122(2) 0.057(4) Uiso 1 1 d . B . O5C O 1.0595(8) 0.3844(5) 0.3543(2) 0.054(3) Uiso 1 1 d . B . C1D C 0.9170(10) 0.6369(8) 0.3224(3) 0.079(7) Uiso 1 1 d D . . C2D C 0.8855(10) 0.6775(8) 0.3009(3) 0.065(6) Uiso 1 1 d D . . C3D C 0.9421(10) 0.7105(8) 0.2873(3) 0.066(6) Uiso 1 1 d D . . C4D C 1.0274(10) 0.7093(9) 0.2920(3) 0.084(7) Uiso 1 1 d D . . C5D C 1.0665(11) 0.6721(11) 0.3119(4) 0.139(10) Uiso 1 1 d D . . C6D C 0.7980(11) 0.6763(10) 0.2959(4) 0.127(10) Uiso 1 1 d D . . H6D H 0.7591 0.6504 0.3052 0.153 Uiso 1 1 calc R . . C7D C 0.7657(12) 0.7168(10) 0.2755(4) 0.125 Uiso 1 1 d D . . H7D H 0.7047 0.7223 0.2721 0.150 Uiso 1 1 calc R . . C8D C 0.8290(12) 0.7453(10) 0.2619(4) 0.112(9) Uiso 1 1 d D . . H8D H 0.8090 0.7654 0.2469 0.134 Uiso 1 1 calc R . . C9D C 0.9140(11) 0.7496(9) 0.2661(3) 0.077(7) Uiso 1 1 d D . . C10D C 0.9808(12) 0.7756(9) 0.2528(4) 0.096(8) Uiso 1 1 d D . . H10D H 0.9639 0.7966 0.2378 0.115 Uiso 1 1 calc R . . C11D C 1.0648(12) 0.7759(9) 0.2577(3) 0.098(8) Uiso 1 1 d D . . H11D H 1.1054 0.7964 0.2468 0.117 Uiso 1 1 calc R . . C12D C 1.0937(12) 0.7442(10) 0.2799(4) 0.131(10) Uiso 1 1 d D . . H12D H 1.1525 0.7464 0.2860 0.157 Uiso 1 1 calc R . . C13D C 1.0385(12) 0.5890(8) 0.3449(3) 0.071(6) Uiso 1 1 d D B . H13D H 1.1041 0.5866 0.3435 0.085 Uiso 1 1 calc R . . N1D N 1.0062(8) 0.6335(7) 0.3263(3) 0.067(5) Uiso 1 1 d D . . O1D O 0.8672(8) 0.6036(6) 0.3349(3) 0.089(5) Uiso 1 1 d D . . O2D O 1.1427(10) 0.6643(8) 0.3171(3) 0.125 Uiso 1 1 d D . . C14D C 1.0142(15) 0.6119(8) 0.3715(3) 0.125 Uiso 1 1 d D . . H14G H 0.9495 0.6068 0.3727 0.150 Uiso 1 1 calc R . . H14H H 1.0397 0.5810 0.3832 0.150 Uiso 1 1 calc R . . C15D C 1.0324(11) 0.6716(9) 0.3833(3) 0.125 Uiso 1 1 d D . . N2D N 1.1034(11) 0.6691(8) 0.3985(3) 0.125 Uiso 1 1 d D . . H2D1 H 1.1207 0.7023 0.4067 0.150 Uiso 1 1 calc R . . H2D2 H 1.1326 0.6343 0.4002 0.150 Uiso 1 1 calc R . . O3D O 0.9944(10) 0.7198(7) 0.3814(3) 0.125 Uiso 1 1 d D . . C16D C 1.0030(12) 0.5278(10) 0.3439(4) 0.064(7) Uiso 1 1 d . . . O4D O 1.0033(7) 0.5073(5) 0.3194(2) 0.052(4) Uiso 1 1 d . B . O5D O 0.9794(8) 0.4942(6) 0.3595(2) 0.058(4) Uiso 1 1 d . B . C1E C 0.7429(9) 0.3851(6) 0.4856(3) 0.074(7) Uiso 1 1 d D . . C2E C 0.7529(8) 0.3547(5) 0.5106(2) 0.039(5) Uiso 1 1 d D . . C3E C 0.8199(9) 0.3671(6) 0.5262(3) 0.067(3) Uiso 1 1 d D . . C4E C 0.8802(10) 0.4070(8) 0.5190(3) 0.067(3) Uiso 1 1 d D . . C5E C 0.8774(10) 0.4447(8) 0.4961(3) 0.067(3) Uiso 1 1 d D . . C6E C 0.6919(11) 0.3125(8) 0.5164(3) 0.080(7) Uiso 1 1 d D . . H6E H 0.6467 0.3019 0.5047 0.096 Uiso 1 1 calc R . . C7E C 0.6969(13) 0.2831(9) 0.5415(4) 0.125 Uiso 1 1 d D . . H7E H 0.6518 0.2562 0.5473 0.150 Uiso 1 1 calc R . . C8E C 0.7682(12) 0.2957(8) 0.5559(3) 0.086(8) Uiso 1 1 d D . . H8E H 0.7766 0.2712 0.5706 0.103 Uiso 1 1 calc R . . C9E C 0.8269(10) 0.3386(7) 0.5514(3) 0.052(6) Uiso 1 1 d D . . C10E C 0.9017(10) 0.3528(8) 0.5642(3) 0.067(3) Uiso 1 1 d D . . H10E H 0.9130 0.3298 0.5792 0.080 Uiso 1 1 calc R . . C11E C 0.9590(11) 0.3940(7) 0.5582(3) 0.067(3) Uiso 1 1 d D . . H11E H 1.0061 0.4036 0.5694 0.080 Uiso 1 1 calc R . . C12E C 0.9507(10) 0.4251(7) 0.5346(3) 0.067(3) Uiso 1 1 d D . . H12E H 0.9908 0.4565 0.5296 0.080 Uiso 1 1 calc R . . C13E C 0.7982(11) 0.4537(8) 0.4524(3) 0.054(6) Uiso 1 1 d D A . H13E H 0.8427 0.4877 0.4516 0.065 Uiso 1 1 calc R . . N1E N 0.8069(8) 0.4271(6) 0.4782(2) 0.042(4) Uiso 1 1 d D . . O1E O 0.6835(8) 0.3738(5) 0.4699(2) 0.065(4) Uiso 1 1 d D . . O2E O 0.9300(8) 0.4815(6) 0.4868(2) 0.086(4) Uiso 1 1 d D . . C14E C 0.8268(14) 0.4094(10) 0.4341(4) 0.095(8) Uiso 1 1 d . . . H14I H 0.7759 0.3824 0.4303 0.114 Uiso 1 1 calc R . . H14J H 0.8718 0.3832 0.4424 0.114 Uiso 1 1 calc R . . C15E C 0.8674(16) 0.4315(12) 0.4072(5) 0.099(9) Uiso 1 1 d . B . C16E C 0.7123(11) 0.4839(8) 0.4478(3) 0.035(5) Uiso 1 1 d . . . N2E N 0.8648(12) 0.4974(9) 0.4037(3) 0.112(7) Uiso 1 1 d . . . H2E1 H 0.8900 0.5141 0.3903 0.135 Uiso 1 1 calc R . . H2E2 H 0.8380 0.5209 0.4149 0.135 Uiso 1 1 calc R . . O3E O 0.8999(8) 0.4048(6) 0.3935(2) 0.057(4) Uiso 1 1 d . . . O4E O 0.6701(7) 0.5072(5) 0.4673(2) 0.048(4) Uiso 1 1 d . A . O5E O 0.6856(7) 0.4852(5) 0.4252(2) 0.041(3) Uiso 1 1 d . A . C1F C 0.3329(10) 0.3743(8) 0.4591(3) 0.0709(16) Uiso 1 1 d D . . C2F C 0.2617(10) 0.3616(9) 0.4778(3) 0.0709(16) Uiso 1 1 d D . . C3F C 0.2745(10) 0.3286(8) 0.4987(3) 0.0709(16) Uiso 1 1 d D . . C4F C 0.3517(10) 0.3037(9) 0.5032(3) 0.0709(16) Uiso 1 1 d D . . C5F C 0.4283(10) 0.3100(8) 0.4864(3) 0.0709(16) Uiso 1 1 d D . . C6F C 0.1815(10) 0.3819(8) 0.4708(3) 0.0709(16) Uiso 1 1 d D . . H6F H 0.1717 0.4025 0.4551 0.085 Uiso 1 1 calc R . . C7F C 0.1097(10) 0.3698(8) 0.4890(3) 0.0709(16) Uiso 1 1 d D . . H7F H 0.0516 0.3835 0.4853 0.085 Uiso 1 1 calc R . . C8F C 0.1264(10) 0.3393(8) 0.5110(3) 0.0709(16) Uiso 1 1 d D . . H8F H 0.0795 0.3359 0.5228 0.085 Uiso 1 1 calc R . . C9F C 0.2017(10) 0.3140(9) 0.5171(3) 0.0709(16) Uiso 1 1 d D . . C10F C 0.2253(11) 0.2800(8) 0.5368(3) 0.0709(16) Uiso 1 1 d D . . H10F H 0.1806 0.2726 0.5491 0.085 Uiso 1 1 calc R . . C11F C 0.3008(11) 0.2557(8) 0.5415(3) 0.0709(16) Uiso 1 1 d D . . H11F H 0.3088 0.2286 0.5555 0.085 Uiso 1 1 calc R . . C12F C 0.3722(11) 0.2708(8) 0.5250(3) 0.0709(16) Uiso 1 1 d D . . H12F H 0.4310 0.2589 0.5287 0.085 Uiso 1 1 calc R . . C13F C 0.4824(11) 0.3584(9) 0.4451(3) 0.0709(16) Uiso 1 1 d D A . H13F H 0.5370 0.3419 0.4532 0.085 Uiso 1 1 calc R . . N1F N 0.4130(9) 0.3475(6) 0.4639(3) 0.0709(16) Uiso 1 1 d D . . O1F O 0.3259(8) 0.4067(6) 0.4397(2) 0.0709(16) Uiso 1 1 d D . . O2F O 0.4990(8) 0.2863(6) 0.4867(2) 0.0709(16) Uiso 1 1 d D . . C14F C 0.4644(11) 0.3137(8) 0.4227(3) 0.047(6) Uiso 1 1 d . . . H14K H 0.4450 0.2732 0.4293 0.056 Uiso 1 1 calc R . . H14L H 0.4170 0.3305 0.4118 0.056 Uiso 1 1 calc R . . C15F C 0.5481(13) 0.3062(8) 0.4074(4) 0.053(6) Uiso 1 1 d . . . C16F C 0.5028(10) 0.4224(8) 0.4397(3) 0.034(5) Uiso 1 1 d . . . N2F N 0.5411(10) 0.2971(6) 0.3824(3) 0.069(5) Uiso 1 1 d . . . H2F1 H 0.5875 0.2857 0.3735 0.083 Uiso 1 1 calc R . . H2F2 H 0.4901 0.3025 0.3748 0.083 Uiso 1 1 calc R . . O3F O 0.6227(9) 0.2977(5) 0.4169(2) 0.065(4) Uiso 1 1 d . . . O4F O 0.5014(6) 0.4629(5) 0.45825(19) 0.038(3) Uiso 1 1 d . A . O5F O 0.5264(7) 0.4400(5) 0.41730(19) 0.039(3) Uiso 1 1 d . A . C1H C 0.8293(9) 0.6522(7) 0.4435(3) 0.056(6) Uiso 1 1 d D . . C2H C 0.9097(9) 0.6576(7) 0.4600(3) 0.049(6) Uiso 1 1 d D . . C3H C 0.9206(9) 0.7062(6) 0.4754(3) 0.038(5) Uiso 1 1 d D . . C4H C 0.8579(9) 0.7489(7) 0.4778(3) 0.048(6) Uiso 1 1 d D . . C5H C 0.7789(10) 0.7506(7) 0.4626(3) 0.047(6) Uiso 1 1 d D . . C6H C 0.9713(10) 0.6135(7) 0.4566(3) 0.071(7) Uiso 1 1 d D . . H6H H 0.9636 0.5814 0.4446 0.085 Uiso 1 1 calc R . . C7H C 1.0516(11) 0.6172(8) 0.4726(3) 0.088(7) Uiso 1 1 d D . . H7H H 1.0949 0.5856 0.4727 0.105 Uiso 1 1 calc R . . C8H C 1.0594(11) 0.6686(8) 0.4871(3) 0.083(7) Uiso 1 1 d D . . H8H H 1.1133 0.6727 0.4962 0.100 Uiso 1 1 calc R . . C9H C 1.0024(11) 0.7134(8) 0.4903(4) 0.089(8) Uiso 1 1 d D . . C10H C 1.0053(12) 0.7646(8) 0.5047(4) 0.094(8) Uiso 1 1 d D . . H10H H 1.0556 0.7686 0.5153 0.112 Uiso 1 1 calc R . . C11H C 0.9492(12) 0.8091(8) 0.5060(3) 0.088(7) Uiso 1 1 d D . . H11H H 0.9609 0.8450 0.5157 0.105 Uiso 1 1 calc R . . C12H C 0.8693(11) 0.8026(7) 0.4923(3) 0.066(7) Uiso 1 1 d D . . H12H H 0.8250 0.8336 0.4929 0.079 Uiso 1 1 calc R . . C13H C 0.6928(10) 0.6977(8) 0.4266(3) 0.064(7) Uiso 1 1 d D A . H13H H 0.6507 0.7307 0.4320 0.077 Uiso 1 1 calc R . . N1H N 0.7683(8) 0.6993(6) 0.4445(2) 0.054(5) Uiso 1 1 d D . . O1H O 0.8136(7) 0.6061(5) 0.4304(2) 0.048(4) Uiso 1 1 d D . . O2H O 0.7148(8) 0.7833(6) 0.4631(2) 0.087(5) Uiso 1 1 d D . . C14H C 0.7204(14) 0.7115(9) 0.3979(3) 0.079(7) Uiso 1 1 d D . . H14M H 0.7716 0.6857 0.3931 0.094 Uiso 1 1 calc R . . H14N H 0.6709 0.7018 0.3864 0.094 Uiso 1 1 calc R . . C15H C 0.7438(16) 0.7783(13) 0.3960(2) 0.150 Uiso 1 1 d D . . O3H O 0.6933(13) 0.8227(9) 0.4003(3) 0.150 Uiso 1 1 d D . . N2H N 0.8306(14) 0.7847(10) 0.3887(4) 0.150 Uiso 1 1 d D . . H2H1 H 0.8535 0.8217 0.3868 0.180 Uiso 1 1 calc R . . H2H2 H 0.8630 0.7517 0.3859 0.180 Uiso 1 1 calc R . . C16H C 0.6424(11) 0.6320(8) 0.4297(4) 0.038(5) Uiso 1 1 d . . . O4H O 0.6215(7) 0.6220(5) 0.4523(2) 0.047(4) Uiso 1 1 d . A . O5H O 0.6300(6) 0.6013(4) 0.4105(2) 0.030(3) Uiso 1 1 d . A . N3I N 0.9788(18) 0.4253(16) 0.2645(2) 0.057(3) Uiso 0.50 1 d PGD B 1 C21I C 0.9063(14) 0.4365(16) 0.2491(4) 0.057(3) Uiso 0.50 1 d PG B 1 H21I H 0.8501 0.4438 0.2564 0.068 Uiso 0.50 1 calc PR B 1 C22I C 0.9160(14) 0.4371(14) 0.2228(4) 0.057(3) Uiso 0.50 1 d PG B 1 H22I H 0.8664 0.4447 0.2123 0.068 Uiso 0.50 1 calc PR B 1 C23I C 0.9982(17) 0.4264(12) 0.2121(2) 0.057(3) Uiso 0.50 1 d PG B 1 H23I H 1.0049 0.4268 0.1941 0.068 Uiso 0.50 1 calc PR B 1 C24I C 1.0707(13) 0.4153(11) 0.2275(4) 0.057(3) Uiso 0.50 1 d PG B 1 H24I H 1.1269 0.4080 0.2202 0.068 Uiso 0.50 1 calc PR B 1 C25I C 1.0610(15) 0.4147(13) 0.2538(4) 0.057(3) Uiso 0.50 1 d PG B 1 H25I H 1.1106 0.4071 0.2643 0.068 Uiso 0.50 1 calc PR B 1 N3J N 1.0012(18) 0.4209(15) 0.2660(2) 0.057(3) Uiso 0.50 1 d PGD B 2 C21J C 0.9350(13) 0.4276(16) 0.2480(4) 0.057(3) Uiso 0.50 1 d PG B 2 H21J H 0.8749 0.4243 0.2529 0.068 Uiso 0.50 1 calc PR B 2 C22J C 0.9567(14) 0.4390(14) 0.2228(4) 0.057(3) Uiso 0.50 1 d PG B 2 H22J H 0.9115 0.4436 0.2105 0.068 Uiso 0.50 1 calc PR B 2 C23J C 1.0446(16) 0.4438(11) 0.2156(3) 0.057(3) Uiso 0.50 1 d PG B 2 H23J H 1.0595 0.4516 0.1984 0.068 Uiso 0.50 1 calc PR B 2 C24J C 1.1108(12) 0.4371(11) 0.2337(4) 0.057(3) Uiso 0.50 1 d PG B 2 H24J H 1.1709 0.4403 0.2288 0.068 Uiso 0.50 1 calc PR B 2 C25J C 1.0891(16) 0.4256(13) 0.2588(4) 0.057(3) Uiso 0.50 1 d PG B 2 H25J H 1.1343 0.4210 0.2712 0.068 Uiso 0.50 1 calc PR B 2 O36 O 0.5139(11) 0.5533(8) 0.4996(3) 0.119(3) Uiso 1 1 d . . . O37 O 0.4090(11) 0.4825(7) 0.5150(3) 0.119(3) Uiso 1 1 d D . . O38 O 0.6379(11) 0.4762(7) 0.5215(3) 0.119(3) Uiso 1 1 d . A . C31 C 0.5023(14) 0.5071(13) 0.5120(5) 0.119(3) Uiso 1 1 d D A . C32 C 0.3409(13) 0.5236(11) 0.5009(4) 0.119(3) Uiso 1 1 d D A . H32A H 0.3272 0.5055 0.4841 0.143 Uiso 1 1 calc R . . H32B H 0.3654 0.5655 0.4982 0.143 Uiso 1 1 calc R . . C33 C 0.2549(14) 0.5272(11) 0.5175(4) 0.119(3) Uiso 1 1 d D . . H33A H 0.2067 0.5059 0.5087 0.179 Uiso 1 1 calc R A . H33B H 0.2388 0.5705 0.5201 0.179 Uiso 1 1 calc R . . H33C H 0.2655 0.5074 0.5339 0.179 Uiso 1 1 calc R . . C34 C 0.5535(17) 0.4505(11) 0.5217(5) 0.119(3) Uiso 1 1 d . . . H34 H 0.5515 0.4183 0.5081 0.143 Uiso 1 1 calc R A . C35 C 0.5316(15) 0.4204(10) 0.5459(4) 0.119(3) Uiso 1 1 d . A . H35A H 0.5666 0.3826 0.5478 0.179 Uiso 1 1 calc R . . H35B H 0.4688 0.4099 0.5461 0.179 Uiso 1 1 calc R . . H35C H 0.5447 0.4485 0.5600 0.179 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0303(15) 0.076(2) 0.0394(16) -0.0023(14) -0.0027(12) 0.0116(14) Cu2 0.0461(17) 0.082(2) 0.0357(16) -0.0105(14) -0.0046(13) 0.0247(17) Cu3 0.0324(15) 0.0558(17) 0.0377(15) -0.0042(12) 0.0097(13) -0.0018(14) Cu4 0.0311(15) 0.0506(16) 0.0359(15) -0.0021(12) 0.0069(13) -0.0011(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O4C 1.905(12) . ? Cu1 O4A 1.928(12) . ? Cu1 O4B 2.020(11) . ? Cu1 O4D 2.039(12) . ? Cu1 N3J 2.158(12) . ? Cu1 N3I 2.177(12) . ? Cu1 Cu2 2.692(3) . ? Cu2 O5B 1.870(11) . ? Cu2 O5D 1.899(13) . ? Cu2 O5C 1.975(12) . ? Cu2 O5A 2.003(13) . ? Cu2 O3E 2.064(13) . ? Cu3 O4G 1.943(11) . ? Cu3 O4F 1.946(10) . ? Cu3 O4H 1.993(11) . ? Cu3 O4E 1.993(11) . ? Cu3 O36 2.242(16) . ? Cu3 Cu4 2.606(3) . ? Cu4 O5H 1.929(10) . ? Cu4 O5F 1.934(10) . ? Cu4 O5E 1.984(11) . ? Cu4 O5G 2.018(11) . ? Cu4 O3Z 2.133(13) . ? Cu4 O3A 2.136(13) . ? C1G O1G 1.229(12) . ? C1G N1G 1.372(12) . ? C1G C2G 1.490(12) . ? C2G C3G 1.334(10) . ? C2G C6G 1.367(11) . ? C3G C4G 1.322(10) . ? C3G C9G 1.484(13) . ? C4G C12G 1.385(11) . ? C4G C5G 1.441(12) . ? C5G O2G 1.217(12) . ? C5G N1G 1.479(13) . ? C6G C7G 1.471(12) . ? C6G H6G 0.9500 . ? C7G C8G 1.348(13) . ? C7G H7G 0.9500 . ? C8G C9G 1.332(13) . ? C8G H8G 0.9500 . ? C9G C10G 1.331(13) . ? C10G C11G 1.282(13) . ? C10G H10G 0.9500 . ? C11G C12G 1.425(12) . ? C11G H11G 0.9500 . ? C12G H12G 0.9500 . ? C13G N1G 1.462(12) . ? C13G C16G 1.48(2) . ? C13G C14G 1.67(2) . ? C13G H13G 1.0000 . ? C14G C15G 1.52(3) . ? C14G H14O 0.9900 . ? C14G H14P 0.9900 . ? C15G O3G 1.25(2) . ? C15G N2G 1.29(2) . ? C16G O5G 1.190(18) . ? C16G O4G 1.290(17) . ? N2G H2G1 0.8800 . ? N2G H2G2 0.8800 . ? C1A O1A 1.16(2) . ? C1A N1A 1.48(2) . ? C1A C2A 1.506(16) . ? C2A C3A 1.316(12) . ? C2A C6A 1.383(13) . ? C3A C4A 1.327(12) . ? C3A C9A 1.486(16) . ? C4A C12A 1.390(13) . ? C4A C5A 1.439(16) . ? C5A O2A 1.31(2) . ? C5A N1A 1.33(2) . ? C6A C7A 1.480(13) . ? C6A H6A 0.9500 . ? C7A C8A 1.356(16) . ? C7A H7A 0.9500 . ? C8A C9A 1.332(16) . ? C8A H8A 0.9500 . ? C9A C10A 1.312(16) . ? C10A C11A 1.276(16) . ? C10A H10A 0.9500 . ? C11A C12A 1.446(13) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? N1A C13A 1.50(2) . ? O4A C16A 1.29(2) . ? O5A C16A 1.26(2) . ? C16A C13A 1.48(2) . ? C13A C14A 1.542(14) . ? C13A H13A 1.0000 . ? C14A C15A 1.506(14) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A O3A 1.251(10) . ? C15A N2A 1.347(10) . ? N2A H2A1 0.8800 . ? N2A H2A2 0.8800 . ? C14Z C15Z 1.499(14) . ? C14Z H14Y 0.9900 . ? C14Z H14Z 0.9900 . ? C15Z O3Z 1.245(10) . ? C15Z N2Z 1.351(10) . ? N2Z H2Z1 0.8800 . ? N2Z H2Z2 0.8800 . ? C1B O1B 1.235(13) . ? C1B N1B 1.383(13) . ? C1B C2B 1.499(14) . ? C2B C3B 1.327(13) . ? C2B C6B 1.331(13) . ? C3B C4B 1.326(13) . ? C3B C9B 1.470(14) . ? C4B C12B 1.378(13) . ? C4B C5B 1.467(14) . ? C5B O2B 1.226(13) . ? C5B N1B 1.474(13) . ? C6B C7B 1.459(14) . ? C6B H6B 0.9500 . ? C7B C8B 1.323(14) . ? C7B H7B 0.9500 . ? C8B C9B 1.304(14) . ? C8B H8B 0.9500 . ? C9B C10B 1.334(13) . ? C10B C11B 1.281(14) . ? C10B H10B 0.9500 . ? C11B C12B 1.442(14) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B C16B 1.37(2) . ? C13B N1B 1.474(13) . ? C13B C14B 1.55(2) . ? C13B H13B 1.0000 . ? C14B C15B 1.54(3) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B O3B 1.23(2) . ? C15B N2B 1.27(3) . ? C16B O5B 1.272(18) . ? C16B O4B 1.334(18) . ? N2B H2B1 0.8800 . ? N2B H2B2 0.8800 . ? C1C O1C 1.235(13) . ? C1C N1C 1.372(13) . ? C1C C2C 1.508(14) . ? C2C C3C 1.336(13) . ? C2C C6C 1.341(14) . ? C3C C4C 1.311(13) . ? C3C C9C 1.512(14) . ? C4C C12C 1.397(14) . ? C4C C5C 1.458(14) . ? C5C O2C 1.193(13) . ? C5C N1C 1.482(14) . ? C6C C7C 1.505(14) . ? C6C H6C 0.9500 . ? C7C C8C 1.373(15) . ? C7C H7C 0.9500 . ? C8C C9C 1.326(14) . ? C8C H8C 0.9500 . ? C9C C10C 1.355(14) . ? C10C C11C 1.282(14) . ? C10C H10C 0.9500 . ? C11C C12C 1.430(14) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C N1C 1.477(14) . ? C13C C16C 1.53(2) . ? C13C C14C 1.63(3) . ? C13C H13C 1.0000 . ? C14C C15C 1.55(3) . ? C14C H14E 0.9900 . ? C14C H14F 0.9900 . ? C15C O3C 1.18(2) . ? C15C N2C 1.29(2) . ? C16C O5C 1.266(17) . ? C16C O4C 1.290(17) . ? N2C H2C1 0.8800 . ? N2C H2C2 0.8800 . ? C1D O1D 1.236(13) . ? C1D N1D 1.371(13) . ? C1D C2D 1.511(13) . ? C2D C3D 1.329(13) . ? C2D C6D 1.354(14) . ? C3D C4D 1.317(13) . ? C3D C9D 1.466(13) . ? C4D C12D 1.410(14) . ? C4D C5D 1.448(14) . ? C5D O2D 1.201(14) . ? C5D N1D 1.456(14) . ? C6D C7D 1.473(15) . ? C6D H6D 0.9500 . ? C7D C8D 1.349(15) . ? C7D H7D 0.9500 . ? C8D C9D 1.312(14) . ? C8D H8D 0.9500 . ? C9D C10D 1.354(14) . ? C10D C11D 1.299(14) . ? C10D H10D 0.9500 . ? C11D C12D 1.427(14) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D C16D 1.43(2) . ? C13D N1D 1.457(13) . ? C13D C14D 1.533(11) . ? C13D H13D 1.0000 . ? C14D C15D 1.462(15) . ? C14D H14G 0.9900 . ? C14D H14H 0.9900 . ? C15D O3D 1.198(15) . ? C15D N2D 1.343(15) . ? N2D H2D1 0.8800 . ? N2D H2D2 0.8800 . ? C16D O5D 1.16(2) . ? C16D O4D 1.368(19) . ? C1E O1E 1.247(13) . ? C1E N1E 1.386(13) . ? C1E C2E 1.482(13) . ? C2E C3E 1.335(13) . ? C2E C6E 1.337(13) . ? C3E C4E 1.315(13) . ? C3E C9E 1.465(13) . ? C4E C12E 1.405(13) . ? C4E C5E 1.459(13) . ? C5E O2E 1.231(13) . ? C5E N1E 1.477(13) . ? C6E C7E 1.468(14) . ? C6E H6E 0.9500 . ? C7E C8E 1.347(15) . ? C7E H7E 0.9500 . ? C8E C9E 1.309(14) . ? C8E H8E 0.9500 . ? C9E C10E 1.357(13) . ? C10E C11E 1.287(13) . ? C10E H10E 0.9500 . ? C11E C12E 1.419(13) . ? C11E H11E 0.9500 . ? C12E H12E 0.9500 . ? C13E C14E 1.43(2) . ? C13E C16E 1.48(2) . ? C13E N1E 1.484(12) . ? C13E H13E 1.0000 . ? C14E C15E 1.62(3) . ? C14E H14I 0.9900 . ? C14E H14J 0.9900 . ? C15E O3E 1.05(2) . ? C15E N2E 1.44(3) . ? C16E O5E 1.259(16) . ? C16E O4E 1.312(17) . ? N2E H2E1 0.8800 . ? N2E H2E2 0.8800 . ? C1F O1F 1.245(13) . ? C1F N1F 1.369(13) . ? C1F C2F 1.486(13) . ? C2F C3F 1.331(13) . ? C2F C6F 1.345(13) . ? C3F C4F 1.310(13) . ? C3F C9F 1.501(14) . ? C4F C12F 1.387(13) . ? C4F C5F 1.468(14) . ? C5F O2F 1.190(13) . ? C5F N1F 1.456(13) . ? C6F C7F 1.474(14) . ? C6F H6F 0.9500 . ? C7F C8F 1.358(14) . ? C7F H7F 0.9500 . ? C8F C9F 1.308(14) . ? C8F H8F 0.9500 . ? C9F C10F 1.324(13) . ? C10F C11F 1.284(14) . ? C10F H10F 0.9500 . ? C11F C12F 1.430(14) . ? C11F H11F 0.9500 . ? C12F H12F 0.9500 . ? C13F C16F 1.45(2) . ? C13F N1F 1.464(13) . ? C13F C14F 1.55(2) . ? C13F H13F 1.0000 . ? C14F C15F 1.51(2) . ? C14F H14K 0.9900 . ? C14F H14L 0.9900 . ? C15F O3F 1.252(19) . ? C15F N2F 1.338(18) . ? C16F O5F 1.292(16) . ? C16F O4F 1.314(17) . ? N2F H2F1 0.8800 . ? N2F H2F2 0.8800 . ? C1H O1H 1.237(12) . ? C1H N1H 1.380(12) . ? C1H C2H 1.501(13) . ? C2H C3H 1.340(12) . ? C2H C6H 1.349(13) . ? C3H C4H 1.334(12) . ? C3H C9H 1.477(14) . ? C4H C12H 1.400(13) . ? C4H C5H 1.442(13) . ? C5H O2H 1.204(12) . ? C5H N1H 1.472(12) . ? C6H C7H 1.484(14) . ? C6H H6H 0.9500 . ? C7H C8H 1.356(14) . ? C7H H7H 0.9500 . ? C8H C9H 1.311(14) . ? C8H H8H 0.9500 . ? C9H C10H 1.344(14) . ? C10H C11H 1.287(14) . ? C10H H10H 0.9500 . ? C11H C12H 1.418(14) . ? C11H H11H 0.9500 . ? C12H H12H 0.9500 . ? C13H N1H 1.484(13) . ? C13H C14H 1.599(15) . ? C13H C16H 1.62(2) . ? C13H H13H 1.0000 . ? C14H C15H 1.49(3) . ? C14H H14M 0.9900 . ? C14H H14N 0.9900 . ? C15H O3H 1.251(17) . ? C15H N2H 1.379(17) . ? N2H H2H1 0.8800 . ? N2H H2H2 0.8800 . ? C16H O5H 1.227(17) . ? C16H O4H 1.251(17) . ? N3I C21I 1.3900 . ? N3I C25I 1.3900 . ? C21I C22I 1.3900 . ? C21I H21I 0.9500 . ? C22I C23I 1.3900 . ? C22I H22I 0.9500 . ? C23I C24I 1.3900 . ? C23I H23I 0.9500 . ? C24I C25I 1.3900 . ? C24I H24I 0.9500 . ? C25I H25I 0.9500 . ? N3J C21J 1.3900 . ? N3J C25J 1.3900 . ? C21J C22J 1.3900 . ? C21J H21J 0.9500 . ? C22J C23J 1.3900 . ? C22J H22J 0.9500 . ? C23J C24J 1.3900 . ? C23J H23J 0.9500 . ? C24J C25J 1.3900 . ? C24J H24J 0.9500 . ? C25J H25J 0.9500 . ? O36 C31 1.21(3) . ? O37 C31 1.521(16) . ? O37 C32 1.555(15) . ? O38 C34 1.40(3) . ? C31 C34 1.54(3) . ? C32 C33 1.574(16) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.47(2) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4C Cu1 O4A 174.8(5) . . ? O4C Cu1 O4B 91.0(5) . . ? O4A Cu1 O4B 90.1(5) . . ? O4C Cu1 O4D 89.8(5) . . ? O4A Cu1 O4D 87.1(5) . . ? O4B Cu1 O4D 155.8(4) . . ? O4C Cu1 N3J 86.5(8) . . ? O4A Cu1 N3J 98.4(8) . . ? O4B Cu1 N3J 97.0(9) . . ? O4D Cu1 N3J 107.2(9) . . ? O4C Cu1 N3I 96.0(8) . . ? O4A Cu1 N3I 88.9(8) . . ? O4B Cu1 N3I 96.0(10) . . ? O4D Cu1 N3I 108.0(10) . . ? N3J Cu1 N3I 9.6(13) . . ? O4C Cu1 Cu2 86.9(4) . . ? O4A Cu1 Cu2 88.3(4) . . ? O4B Cu1 Cu2 78.7(3) . . ? O4D Cu1 Cu2 77.1(3) . . ? N3J Cu1 Cu2 172.1(8) . . ? N3I Cu1 Cu2 174.0(8) . . ? O5B Cu2 O5D 174.8(5) . . ? O5B Cu2 O5C 92.9(5) . . ? O5D Cu2 O5C 87.7(5) . . ? O5B Cu2 O5A 89.8(5) . . ? O5D Cu2 O5A 87.8(5) . . ? O5C Cu2 O5A 158.6(5) . . ? O5B Cu2 O3E 90.8(5) . . ? O5D Cu2 O3E 94.0(5) . . ? O5C Cu2 O3E 105.3(5) . . ? O5A Cu2 O3E 95.9(5) . . ? O5B Cu2 Cu1 87.3(3) . . ? O5D Cu2 Cu1 87.7(4) . . ? O5C Cu2 Cu1 80.0(3) . . ? O5A Cu2 Cu1 78.9(4) . . ? O3E Cu2 Cu1 174.4(4) . . ? O4G Cu3 O4F 94.1(4) . . ? O4G Cu3 O4H 89.3(4) . . ? O4F Cu3 O4H 166.9(5) . . ? O4G Cu3 O4E 172.5(5) . . ? O4F Cu3 O4E 89.6(4) . . ? O4H Cu3 O4E 85.7(4) . . ? O4G Cu3 O36 93.2(5) . . ? O4F Cu3 O36 88.8(5) . . ? O4H Cu3 O36 103.6(5) . . ? O4E Cu3 O36 93.3(5) . . ? O4G Cu3 Cu4 82.8(3) . . ? O4F Cu3 Cu4 81.7(3) . . ? O4H Cu3 Cu4 86.2(3) . . ? O4E Cu3 Cu4 91.3(3) . . ? O36 Cu3 Cu4 169.4(4) . . ? O5H Cu4 O5F 170.1(4) . . ? O5H Cu4 O5E 89.9(4) . . ? O5F Cu4 O5E 84.7(4) . . ? O5H Cu4 O5G 88.6(4) . . ? O5F Cu4 O5G 94.4(4) . . ? O5E Cu4 O5G 164.5(4) . . ? O5H Cu4 O3Z 104.3(7) . . ? O5F Cu4 O3Z 85.2(7) . . ? O5E Cu4 O3Z 104.1(7) . . ? O5G Cu4 O3Z 91.2(7) . . ? O5H Cu4 O3A 94.3(8) . . ? O5F Cu4 O3A 94.1(7) . . ? O5E Cu4 O3A 90.7(7) . . ? O5G Cu4 O3A 104.8(7) . . ? O3Z Cu4 O3A 16.9(9) . . ? O5H Cu4 Cu3 83.2(3) . . ? O5F Cu4 Cu3 87.6(3) . . ? O5E Cu4 Cu3 79.3(3) . . ? O5G Cu4 Cu3 85.2(3) . . ? O3Z Cu4 Cu3 171.7(6) . . ? O3A Cu4 Cu3 169.7(7) . . ? O1G C1G N1G 117.4(12) . . ? O1G C1G C2G 124.4(12) . . ? N1G C1G C2G 117.7(11) . . ? C3G C2G C6G 125.9(12) . . ? C3G C2G C1G 120.8(12) . . ? C6G C2G C1G 112.4(11) . . ? C4G C3G C2G 120.8(13) . . ? C4G C3G C9G 119.4(11) . . ? C2G C3G C9G 119.8(11) . . ? C3G C4G C12G 124.8(12) . . ? C3G C4G C5G 124.4(12) . . ? C12G C4G C5G 110.7(11) . . ? O2G C5G C4G 133.6(13) . . ? O2G C5G N1G 111.4(12) . . ? C4G C5G N1G 114.6(11) . . ? C2G C6G C7G 115.8(12) . . ? C2G C6G H6G 122.1 . . ? C7G C6G H6G 122.1 . . ? C8G C7G C6G 115.1(13) . . ? C8G C7G H7G 122.5 . . ? C6G C7G H7G 122.5 . . ? C9G C8G C7G 131.6(14) . . ? C9G C8G H8G 114.2 . . ? C7G C8G H8G 114.2 . . ? C10G C9G C8G 136.5(15) . . ? C10G C9G C3G 111.8(12) . . ? C8G C9G C3G 111.5(12) . . ? C11G C10G C9G 129.9(15) . . ? C11G C10G H10G 115.0 . . ? C9G C10G H10G 115.0 . . ? C10G C11G C12G 119.5(14) . . ? C10G C11G H11G 120.2 . . ? C12G C11G H11G 120.2 . . ? C4G C12G C11G 114.2(12) . . ? C4G C12G H12G 122.9 . . ? C11G C12G H12G 122.9 . . ? N1G C13G C16G 119.1(14) . . ? N1G C13G C14G 103.6(13) . . ? C16G C13G C14G 112.9(14) . . ? N1G C13G H13G 106.8 . . ? C16G C13G H13G 106.8 . . ? C14G C13G H13G 106.8 . . ? C1G N1G C13G 119.6(11) . . ? C1G N1G C5G 120.7(11) . . ? C13G N1G C5G 119.5(11) . . ? C15G C14G C13G 111.1(17) . . ? C15G C14G H14O 109.4 . . ? C13G C14G H14O 109.4 . . ? C15G C14G H14P 109.4 . . ? C13G C14G H14P 109.4 . . ? H14O C14G H14P 108.0 . . ? O3G C15G N2G 118(2) . . ? O3G C15G C14G 124(2) . . ? N2G C15G C14G 116(2) . . ? O5G C16G O4G 124.9(18) . . ? O5G C16G C13G 123.2(17) . . ? O4G C16G C13G 111.8(16) . . ? C15G N2G H2G1 120.0 . . ? C15G N2G H2G2 120.0 . . ? H2G1 N2G H2G2 120.0 . . ? C16G O4G Cu3 125.0(11) . . ? C16G O5G Cu4 120.1(12) . . ? O1A C1A N1A 116.5(18) . . ? O1A C1A C2A 127.5(19) . . ? N1A C1A C2A 116.0(18) . . ? C3A C2A C6A 129.8(16) . . ? C3A C2A C1A 119.6(17) . . ? C6A C2A C1A 110.6(14) . . ? C2A C3A C4A 120.9(18) . . ? C2A C3A C9A 116.0(14) . . ? C4A C3A C9A 123.1(15) . . ? C3A C4A C12A 124.9(16) . . ? C3A C4A C5A 125.2(18) . . ? C12A C4A C5A 109.7(15) . . ? O2A C5A N1A 117.3(18) . . ? O2A C5A C4A 125.2(18) . . ? N1A C5A C4A 117(2) . . ? C2A C6A C7A 115.6(16) . . ? C2A C6A H6A 122.2 . . ? C7A C6A H6A 122.2 . . ? C8A C7A C6A 110.5(17) . . ? C8A C7A H7A 124.7 . . ? C6A C7A H7A 124.7 . . ? C9A C8A C7A 135(2) . . ? C9A C8A H8A 112.3 . . ? C7A C8A H8A 112.3 . . ? C10A C9A C8A 141(2) . . ? C10A C9A C3A 107.1(16) . . ? C8A C9A C3A 111.9(17) . . ? C11A C10A C9A 133(2) . . ? C11A C10A H10A 113.5 . . ? C9A C10A H10A 113.5 . . ? C10A C11A C12A 121.1(18) . . ? C10A C11A H11A 119.5 . . ? C12A C11A H11A 119.5 . . ? C4A C12A C11A 110.4(16) . . ? C4A C12A H12A 124.8 . . ? C11A C12A H12A 124.8 . . ? C5A N1A C1A 121(2) . . ? C5A N1A C13A 120.2(14) . . ? C1A N1A C13A 117.7(12) . . ? C16A O4A Cu1 119.5(14) . . ? C16A O5A Cu2 127.6(14) . . ? O5A C16A O4A 124(2) . . ? O5A C16A C13A 122(2) . . ? O4A C16A C13A 113.7(19) . . ? C16A C13A N1A 112.1(15) . . ? C16A C13A C14A 106.1(19) . . ? N1A C13A C14A 105.4(15) . . ? C16A C13A H13A 111.0 . . ? N1A C13A H13A 111.0 . . ? C14A C13A H13A 111.0 . . ? C15A C14A C13A 122(2) . . ? C15A C14A H14A 106.8 . . ? C13A C14A H14A 106.8 . . ? C15A C14A H14B 106.8 . . ? C13A C14A H14B 106.8 . . ? H14A C14A H14B 106.6 . . ? O3A C15A N2A 114(2) . . ? O3A C15A C14A 125(2) . . ? N2A C15A C14A 120(2) . . ? C15A N2A H2A1 120.0 . . ? C15A N2A H2A2 120.0 . . ? H2A1 N2A H2A2 120.0 . . ? C15A O3A Cu4 137.1(18) . . ? C15Z C14Z H14Y 107.0 . . ? C15Z C14Z H14Z 107.0 . . ? H14Y C14Z H14Z 106.7 . . ? O3Z C15Z N2Z 145(2) . . ? O3Z C15Z C14Z 100.6(16) . . ? N2Z C15Z C14Z 114(2) . . ? C15Z N2Z H2Z1 120.0 . . ? C15Z N2Z H2Z2 120.0 . . ? H2Z1 N2Z H2Z2 120.0 . . ? C15Z O3Z Cu4 113.8(15) . . ? O1B C1B N1B 119.1(14) . . ? O1B C1B C2B 122.7(14) . . ? N1B C1B C2B 117.1(13) . . ? C3B C2B C6B 124.7(14) . . ? C3B C2B C1B 120.8(13) . . ? C6B C2B C1B 114.4(13) . . ? C4B C3B C2B 121.7(14) . . ? C4B C3B C9B 117.4(13) . . ? C2B C3B C9B 120.6(13) . . ? C3B C4B C12B 125.5(14) . . ? C3B C4B C5B 123.4(13) . . ? C12B C4B C5B 111.0(13) . . ? O2B C5B C4B 130.2(15) . . ? O2B C5B N1B 111.6(13) . . ? C4B C5B N1B 114.0(12) . . ? C2B C6B C7B 116.6(14) . . ? C2B C6B H6B 121.7 . . ? C7B C6B H6B 121.7 . . ? C8B C7B C6B 114.7(15) . . ? C8B C7B H7B 122.6 . . ? C6B C7B H7B 122.6 . . ? C9B C8B C7B 132.5(16) . . ? C9B C8B H8B 113.7 . . ? C7B C8B H8B 113.7 . . ? C8B C9B C10B 136.1(16) . . ? C8B C9B C3B 110.7(13) . . ? C10B C9B C3B 113.2(14) . . ? C11B C10B C9B 131.7(16) . . ? C11B C10B H10B 114.1 . . ? C9B C10B H10B 114.1 . . ? C10B C11B C12B 115.4(15) . . ? C10B C11B H11B 122.3 . . ? C12B C11B H11B 122.3 . . ? C4B C12B C11B 116.3(14) . . ? C4B C12B H12B 121.8 . . ? C11B C12B H12B 121.8 . . ? C16B C13B N1B 113.0(16) . . ? C16B C13B C14B 113.1(16) . . ? N1B C13B C14B 108.6(16) . . ? C16B C13B H13B 107.3 . . ? N1B C13B H13B 107.3 . . ? C14B C13B H13B 107.3 . . ? C1B N1B C5B 120.2(12) . . ? C1B N1B C13B 117.7(13) . . ? C5B N1B C13B 121.3(13) . . ? C15B C14B C13B 113.5(17) . . ? C15B C14B H14C 108.9 . . ? C13B C14B H14C 108.9 . . ? C15B C14B H14D 108.9 . . ? C13B C14B H14D 108.9 . . ? H14C C14B H14D 107.7 . . ? O3B C15B N2B 127(3) . . ? O3B C15B C14B 120(2) . . ? N2B C15B C14B 113(2) . . ? O5B C16B O4B 116.4(17) . . ? O5B C16B C13B 125.2(18) . . ? O4B C16B C13B 117.6(18) . . ? C15B N2B H2B1 120.0 . . ? C15B N2B H2B2 120.0 . . ? H2B1 N2B H2B2 120.0 . . ? C16B O4B Cu1 129.2(11) . . ? C16B O5B Cu2 128.1(12) . . ? O1C C1C N1C 120.1(14) . . ? O1C C1C C2C 123.0(14) . . ? N1C C1C C2C 116.8(13) . . ? C3C C2C C6C 126.1(15) . . ? C3C C2C C1C 119.8(14) . . ? C6C C2C C1C 113.8(14) . . ? C4C C3C C2C 122.7(15) . . ? C4C C3C C9C 117.2(14) . . ? C2C C3C C9C 120.0(14) . . ? C3C C4C C12C 126.3(15) . . ? C3C C4C C5C 124.3(15) . . ? C12C C4C C5C 109.4(14) . . ? O2C C5C C4C 133.1(16) . . ? O2C C5C N1C 113.1(14) . . ? C4C C5C N1C 112.5(13) . . ? C2C C6C C7C 116.5(15) . . ? C2C C6C H6C 121.8 . . ? C7C C6C H6C 121.8 . . ? C8C C7C C6C 111.9(15) . . ? C8C C7C H7C 124.0 . . ? C6C C7C H7C 124.0 . . ? C9C C8C C7C 132.3(18) . . ? C9C C8C H8C 113.8 . . ? C7C C8C H8C 113.8 . . ? C8C C9C C10C 135.4(17) . . ? C8C C9C C3C 109.6(14) . . ? C10C C9C C3C 114.4(14) . . ? C11C C10C C9C 126.1(17) . . ? C11C C10C H10C 116.9 . . ? C9C C10C H10C 116.9 . . ? C10C C11C C12C 121.9(16) . . ? C10C C11C H11C 119.0 . . ? C12C C11C H11C 119.0 . . ? C4C C12C C11C 113.2(15) . . ? C4C C12C H12C 123.4 . . ? C11C C12C H12C 123.4 . . ? N1C C13C C16C 111.9(18) . . ? N1C C13C C14C 113.8(18) . . ? C16C C13C C14C 105.8(16) . . ? N1C C13C H13C 108.4 . . ? C16C C13C H13C 108.4 . . ? C14C C13C H13C 108.4 . . ? C1C N1C C13C 119.5(14) . . ? C1C N1C C5C 122.7(14) . . ? C13C N1C C5C 116.8(14) . . ? C15C C14C C13C 110.3(19) . . ? C15C C14C H14E 109.6 . . ? C13C C14C H14E 109.6 . . ? C15C C14C H14F 109.6 . . ? C13C C14C H14F 109.6 . . ? H14E C14C H14F 108.1 . . ? O3C C15C N2C 128(2) . . ? O3C C15C C14C 117(2) . . ? N2C C15C C14C 115(2) . . ? O5C C16C O4C 123.3(17) . . ? O5C C16C C13C 120.6(16) . . ? O4C C16C C13C 116.1(16) . . ? C15C N2C H2C1 120.0 . . ? C15C N2C H2C2 120.0 . . ? H2C1 N2C H2C2 120.0 . . ? C16C O4C Cu1 122.0(11) . . ? C16C O5C Cu2 127.4(11) . . ? O1D C1D N1D 119.4(14) . . ? O1D C1D C2D 123.1(14) . . ? N1D C1D C2D 117.2(13) . . ? C3D C2D C6D 122.6(14) . . ? C3D C2D C1D 120.9(13) . . ? C6D C2D C1D 116.5(13) . . ? C4D C3D C2D 121.6(14) . . ? C4D C3D C9D 116.1(13) . . ? C2D C3D C9D 122.3(13) . . ? C3D C4D C12D 127.3(14) . . ? C3D C4D C5D 123.2(14) . . ? C12D C4D C5D 109.5(13) . . ? O2D C5D C4D 129.8(16) . . ? O2D C5D N1D 113.7(15) . . ? C4D C5D N1D 116.2(13) . . ? C2D C6D C7D 117.3(15) . . ? C2D C6D H6D 121.3 . . ? C7D C6D H6D 121.3 . . ? C8D C7D C6D 115.0(16) . . ? C8D C7D H7D 122.5 . . ? C6D C7D H7D 122.5 . . ? C9D C8D C7D 130.0(17) . . ? C9D C8D H8D 115.0 . . ? C7D C8D H8D 115.0 . . ? C8D C9D C10D 132.7(16) . . ? C8D C9D C3D 112.0(14) . . ? C10D C9D C3D 114.6(14) . . ? C11D C10D C9D 129.4(17) . . ? C11D C10D H10D 115.3 . . ? C9D C10D H10D 115.3 . . ? C10D C11D C12D 117.4(16) . . ? C10D C11D H11D 121.3 . . ? C12D C11D H11D 121.3 . . ? C4D C12D C11D 114.2(15) . . ? C4D C12D H12D 122.9 . . ? C11D C12D H12D 122.9 . . ? C16D C13D N1D 117.5(16) . . ? C16D C13D C14D 104.0(15) . . ? N1D C13D C14D 108.6(16) . . ? C16D C13D H13D 108.8 . . ? N1D C13D H13D 108.8 . . ? C14D C13D H13D 108.8 . . ? C1D N1D C5D 120.6(12) . . ? C1D N1D C13D 118.0(13) . . ? C5D N1D C13D 121.4(13) . . ? C15D C14D C13D 128.9(15) . . ? C15D C14D H14G 105.1 . . ? C13D C14D H14G 105.1 . . ? C15D C14D H14H 105.1 . . ? C13D C14D H14H 105.1 . . ? H14G C14D H14H 105.9 . . ? O3D C15D N2D 118.0(17) . . ? O3D C15D C14D 130.3(19) . . ? N2D C15D C14D 111.6(19) . . ? C15D N2D H2D1 120.0 . . ? C15D N2D H2D2 120.0 . . ? H2D1 N2D H2D2 120.0 . . ? O5D C16D O4D 118(2) . . ? O5D C16D C13D 133(2) . . ? O4D C16D C13D 109.5(18) . . ? C16D O4D Cu1 128.6(12) . . ? C16D O5D Cu2 128.6(15) . . ? O1E C1E N1E 116.7(13) . . ? O1E C1E C2E 125.1(13) . . ? N1E C1E C2E 118.1(12) . . ? C3E C2E C6E 121.5(13) . . ? C3E C2E C1E 122.5(12) . . ? C6E C2E C1E 116.0(12) . . ? C4E C3E C2E 118.9(13) . . ? C4E C3E C9E 119.2(12) . . ? C2E C3E C9E 121.9(12) . . ? C3E C4E C12E 123.0(13) . . ? C3E C4E C5E 126.0(13) . . ? C12E C4E C5E 110.5(12) . . ? O2E C5E C4E 132.5(14) . . ? O2E C5E N1E 112.4(12) . . ? C4E C5E N1E 114.0(12) . . ? C2E C6E C7E 117.9(14) . . ? C2E C6E H6E 121.1 . . ? C7E C6E H6E 121.1 . . ? C8E C7E C6E 117.3(16) . . ? C8E C7E H7E 121.4 . . ? C6E C7E H7E 121.4 . . ? C9E C8E C7E 126.1(16) . . ? C9E C8E H8E 117.0 . . ? C7E C8E H8E 117.0 . . ? C8E C9E C10E 129.8(15) . . ? C8E C9E C3E 114.4(13) . . ? C10E C9E C3E 114.6(13) . . ? C11E C10E C9E 126.8(15) . . ? C11E C10E H10E 116.6 . . ? C9E C10E H10E 116.6 . . ? C10E C11E C12E 119.1(14) . . ? C10E C11E H11E 120.5 . . ? C12E C11E H11E 120.5 . . ? C4E C12E C11E 116.5(13) . . ? C4E C12E H12E 121.7 . . ? C11E C12E H12E 121.7 . . ? C14E C13E C16E 117.0(16) . . ? C14E C13E N1E 109.4(15) . . ? C16E C13E N1E 113.6(13) . . ? C14E C13E H13E 105.2 . . ? C16E C13E H13E 105.2 . . ? N1E C13E H13E 105.2 . . ? C1E N1E C5E 119.8(11) . . ? C1E N1E C13E 116.8(11) . . ? C5E N1E C13E 123.4(11) . . ? C13E C14E C15E 120.6(19) . . ? C13E C14E H14I 107.2 . . ? C15E C14E H14I 107.2 . . ? C13E C14E H14J 107.2 . . ? C15E C14E H14J 107.2 . . ? H14I C14E H14J 106.8 . . ? O3E C15E N2E 118(3) . . ? O3E C15E C14E 128(3) . . ? N2E C15E C14E 113(2) . . ? O5E C16E O4E 125.1(15) . . ? O5E C16E C13E 116.7(15) . . ? O4E C16E C13E 118.2(15) . . ? C15E N2E H2E1 120.0 . . ? C15E N2E H2E2 120.0 . . ? H2E1 N2E H2E2 120.0 . . ? C15E O3E Cu2 138.0(19) . . ? C16E O4E Cu3 114.5(10) . . ? C16E O5E Cu4 129.9(11) . . ? O1F C1F N1F 117.7(13) . . ? O1F C1F C2F 125.8(13) . . ? N1F C1F C2F 116.5(12) . . ? C3F C2F C6F 122.3(13) . . ? C3F C2F C1F 122.8(13) . . ? C6F C2F C1F 114.7(13) . . ? C4F C3F C2F 120.0(13) . . ? C4F C3F C9F 117.1(12) . . ? C2F C3F C9F 122.7(13) . . ? C3F C4F C12F 124.1(13) . . ? C3F C4F C5F 124.1(13) . . ? C12F C4F C5F 111.7(13) . . ? O2F C5F N1F 113.4(13) . . ? O2F C5F C4F 131.6(14) . . ? N1F C5F C4F 114.7(12) . . ? C2F C6F C7F 115.6(13) . . ? C2F C6F H6F 122.2 . . ? C7F C6F H6F 122.2 . . ? C8F C7F C6F 120.2(14) . . ? C8F C7F H7F 119.9 . . ? C6F C7F H7F 119.9 . . ? C9F C8F C7F 125.2(15) . . ? C9F C8F H8F 117.4 . . ? C7F C8F H8F 117.4 . . ? C8F C9F C10F 131.5(15) . . ? C8F C9F C3F 113.3(13) . . ? C10F C9F C3F 115.1(13) . . ? C11F C10F C9F 128.4(16) . . ? C11F C10F H10F 115.8 . . ? C9F C10F H10F 115.8 . . ? C10F C11F C12F 117.6(15) . . ? C10F C11F H11F 121.2 . . ? C12F C11F H11F 121.2 . . ? C4F C12F C11F 116.9(14) . . ? C4F C12F H12F 121.5 . . ? C11F C12F H12F 121.5 . . ? C16F C13F N1F 116.0(15) . . ? C16F C13F C14F 119.1(15) . . ? N1F C13F C14F 106.8(15) . . ? C16F C13F H13F 104.4 . . ? N1F C13F H13F 104.4 . . ? C14F C13F H13F 104.4 . . ? C1F N1F C5F 121.8(12) . . ? C1F N1F C13F 116.5(12) . . ? C5F N1F C13F 121.7(12) . . ? C15F C14F C13F 108.9(14) . . ? C15F C14F H14K 109.9 . . ? C13F C14F H14K 109.9 . . ? C15F C14F H14L 109.9 . . ? C13F C14F H14L 109.9 . . ? H14K C14F H14L 108.3 . . ? O3F C15F N2F 116.4(17) . . ? O3F C15F C14F 124.2(17) . . ? N2F C15F C14F 118.3(17) . . ? O5F C16F O4F 119.1(15) . . ? O5F C16F C13F 121.4(15) . . ? O4F C16F C13F 119.4(15) . . ? C15F N2F H2F1 120.0 . . ? C15F N2F H2F2 120.0 . . ? H2F1 N2F H2F2 120.0 . . ? C16F O4F Cu3 127.9(10) . . ? C16F O5F Cu4 122.6(11) . . ? O1H C1H N1H 119.4(12) . . ? O1H C1H C2H 122.8(12) . . ? N1H C1H C2H 117.6(12) . . ? C3H C2H C6H 123.3(13) . . ? C3H C2H C1H 120.9(12) . . ? C6H C2H C1H 115.6(12) . . ? C4H C3H C2H 121.0(12) . . ? C4H C3H C9H 118.4(12) . . ? C2H C3H C9H 120.7(12) . . ? C3H C4H C12H 122.7(13) . . ? C3H C4H C5H 123.8(12) . . ? C12H C4H C5H 112.6(12) . . ? O2H C5H C4H 132.5(14) . . ? O2H C5H N1H 111.6(12) . . ? C4H C5H N1H 115.6(11) . . ? C2H C6H C7H 117.2(13) . . ? C2H C6H H6H 121.4 . . ? C7H C6H H6H 121.4 . . ? C8H C7H C6H 115.9(14) . . ? C8H C7H H7H 122.1 . . ? C6H C7H H7H 122.1 . . ? C9H C8H C7H 128.5(16) . . ? C9H C8H H8H 115.8 . . ? C7H C8H H8H 115.8 . . ? C8H C9H C10H 131.5(16) . . ? C8H C9H C3H 114.1(14) . . ? C10H C9H C3H 114.4(14) . . ? C11H C10H C9H 128.8(17) . . ? C11H C10H H10H 115.6 . . ? C9H C10H H10H 115.6 . . ? C10H C11H C12H 117.6(15) . . ? C10H C11H H11H 121.2 . . ? C12H C11H H11H 121.2 . . ? C4H C12H C11H 117.7(14) . . ? C4H C12H H12H 121.2 . . ? C11H C12H H12H 121.2 . . ? N1H C13H C14H 113.3(14) . . ? N1H C13H C16H 108.8(13) . . ? C14H C13H C16H 112.5(14) . . ? N1H C13H H13H 107.3 . . ? C14H C13H H13H 107.3 . . ? C16H C13H H13H 107.3 . . ? C1H N1H C5H 120.7(11) . . ? C1H N1H C13H 118.3(12) . . ? C5H N1H C13H 121.0(11) . . ? C15H C14H C13H 108.0(14) . . ? C15H C14H H14M 110.1 . . ? C13H C14H H14M 110.1 . . ? C15H C14H H14N 110.1 . . ? C13H C14H H14N 110.1 . . ? H14M C14H H14N 108.4 . . ? O3H C15H N2H 124(3) . . ? O3H C15H C14H 126(2) . . ? N2H C15H C14H 110(2) . . ? C15H N2H H2H1 120.0 . . ? C15H N2H H2H2 120.0 . . ? H2H1 N2H H2H2 120.0 . . ? O5H C16H O4H 130.8(17) . . ? O5H C16H C13H 117.8(16) . . ? O4H C16H C13H 111.5(15) . . ? C16H O4H Cu3 116.1(11) . . ? C16H O5H Cu4 123.3(11) . . ? C21I N3I C25I 120.0 . . ? C21I N3I Cu1 121.0(14) . . ? C25I N3I Cu1 119.0(14) . . ? N3I C21I C22I 120.0 . . ? N3I C21I H21I 120.0 . . ? C22I C21I H21I 120.0 . . ? C21I C22I C23I 120.0 . . ? C21I C22I H22I 120.0 . . ? C23I C22I H22I 120.0 . . ? C24I C23I C22I 120.0 . . ? C24I C23I H23I 120.0 . . ? C22I C23I H23I 120.0 . . ? C25I C24I C23I 120.0 . . ? C25I C24I H24I 120.0 . . ? C23I C24I H24I 120.0 . . ? C24I C25I N3I 120.0 . . ? C24I C25I H25I 120.0 . . ? N3I C25I H25I 120.0 . . ? C21J N3J C25J 120.0 . . ? C21J N3J Cu1 118.7(14) . . ? C25J N3J Cu1 120.0(14) . . ? N3J C21J C22J 120.0 . . ? N3J C21J H21J 120.0 . . ? C22J C21J H21J 120.0 . . ? C23J C22J C21J 120.0 . . ? C23J C22J H22J 120.0 . . ? C21J C22J H22J 120.0 . . ? C24J C23J C22J 120.0 . . ? C24J C23J H23J 120.0 . . ? C22J C23J H23J 120.0 . . ? C23J C24J C25J 120.0 . . ? C23J C24J H24J 120.0 . . ? C25J C24J H24J 120.0 . . ? C24J C25J N3J 120.0 . . ? C24J C25J H25J 120.0 . . ? N3J C25J H25J 120.0 . . ? C31 O36 Cu3 119.2(18) . . ? C31 O37 C32 111.5(17) . . ? O36 C31 O37 119(2) . . ? O36 C31 C34 140(2) . . ? O37 C31 C34 99.0(19) . . ? O37 C32 C33 108.2(17) . . ? O37 C32 H32A 110.1 . . ? C33 C32 H32A 110.1 . . ? O37 C32 H32B 110.1 . . ? C33 C32 H32B 110.1 . . ? H32A C32 H32B 108.4 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O38 C34 C35 113(2) . . ? O38 C34 C31 98.3(19) . . ? C35 C34 C31 122(2) . . ? O38 C34 H34 107.6 . . ? C35 C34 H34 107.6 . . ? C31 C34 H34 107.6 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4C Cu1 Cu2 O5B -92.0(5) . . . . ? O4A Cu1 Cu2 O5B 90.0(5) . . . . ? O4B Cu1 Cu2 O5B -0.4(4) . . . . ? O4D Cu1 Cu2 O5B 177.5(5) . . . . ? O4C Cu1 Cu2 O5D 89.5(5) . . . . ? O4A Cu1 Cu2 O5D -88.5(5) . . . . ? O4B Cu1 Cu2 O5D -178.9(5) . . . . ? O4D Cu1 Cu2 O5D -1.1(5) . . . . ? O4C Cu1 Cu2 O5C 1.4(5) . . . . ? O4A Cu1 Cu2 O5C -176.6(5) . . . . ? O4B Cu1 Cu2 O5C 93.0(4) . . . . ? O4D Cu1 Cu2 O5C -89.1(5) . . . . ? O4C Cu1 Cu2 O5A 177.7(5) . . . . ? O4A Cu1 Cu2 O5A -0.3(5) . . . . ? O4B Cu1 Cu2 O5A -90.7(5) . . . . ? O4D Cu1 Cu2 O5A 87.2(5) . . . . ? O4G Cu3 Cu4 O5H 85.5(4) . . . . ? O4F Cu3 Cu4 O5H -179.3(4) . . . . ? O4H Cu3 Cu4 O5H -4.2(4) . . . . ? O4E Cu3 Cu4 O5H -89.9(4) . . . . ? O4G Cu3 Cu4 O5F -98.3(4) . . . . ? O4F Cu3 Cu4 O5F -3.1(4) . . . . ? O4H Cu3 Cu4 O5F 171.9(4) . . . . ? O4E Cu3 Cu4 O5F 86.3(4) . . . . ? O4G Cu3 Cu4 O5E 176.7(5) . . . . ? O4F Cu3 Cu4 O5E -88.1(4) . . . . ? O4H Cu3 Cu4 O5E 86.9(4) . . . . ? O4E Cu3 Cu4 O5E 1.3(5) . . . . ? O36 Cu3 Cu4 O5E -114(2) . . . . ? O4G Cu3 Cu4 O5G -3.7(4) . . . . ? O4F Cu3 Cu4 O5G 91.6(4) . . . . ? O4H Cu3 Cu4 O5G -93.4(4) . . . . ? O4E Cu3 Cu4 O5G -179.0(4) . . . . ? O1G C1G C2G C3G 179.8(19) . . . . ? N1G C1G C2G C3G 8(3) . . . . ? O1G C1G C2G C6G -10(3) . . . . ? N1G C1G C2G C6G 178.4(16) . . . . ? C6G C2G C3G C4G -179.0(19) . . . . ? C1G C2G C3G C9G 170.6(17) . . . . ? C9G C3G C4G C5G -177.9(19) . . . . ? C12G C4G C5G N1G -175.9(16) . . . . ? C1G C2G C6G C7G -173.3(15) . . . . ? C4G C3G C9G C8G -175.8(19) . . . . ? C5G C4G C12G C11G 176.8(17) . . . . ? C2G C1G N1G C13G 176.7(15) . . . . ? O1G C1G N1G C5G -171.2(16) . . . . ? C14G C13G N1G C1G -78.7(18) . . . . ? C16G C13G N1G C5G -136.4(17) . . . . ? C14G C13G N1G C5G 97.2(17) . . . . ? O2G C5G N1G C1G 179.0(16) . . . . ? C4G C5G N1G C13G 176.8(15) . . . . ? N1G C13G C14G C15G -160.6(16) . . . . ? C13G C14G C15G N2G -148.5(19) . . . . ? N1G C13G C16G O5G -134.3(18) . . . . ? C14G C13G C16G O4G 171.4(14) . . . . ? C13G C16G O4G Cu3 -170.1(10) . . . . ? O4F Cu3 O4G C16G -83.8(13) . . . . ? O4H Cu3 O4G C16G 83.5(13) . . . . ? O36 Cu3 O4G C16G -172.9(14) . . . . ? Cu4 Cu3 O4G C16G -2.8(13) . . . . ? C13G C16G O5G Cu4 166.1(12) . . . . ? O5H Cu4 O5G C16G -71.4(13) . . . . ? O5F Cu4 O5G C16G 99.1(14) . . . . ? O3Z Cu4 O5G C16G -175.7(15) . . . . ? O3A Cu4 O5G C16G -165.5(15) . . . . ? Cu3 Cu4 O5G C16G 11.9(13) . . . . ? O1A C1A C2A C3A 179.7(19) . . . . ? N1A C1A C2A C3A -0.4(13) . . . . ? N1A C1A C2A C6A 178.5(18) . . . . ? C1A C2A C3A C4A -1.0(15) . . . . ? C1A C2A C3A C9A 178.3(14) . . . . ? C2A C3A C4A C12A 179.1(19) . . . . ? C1A C2A C6A C7A 176.8(16) . . . . ? C2A C3A C9A C10A -178.6(16) . . . . ? O2A C5A N1A C1A 176.9(19) . . . . ? C4A C5A N1A C13A 172.7(19) . . . . ? C2A C1A N1A C13A -170.0(13) . . . . ? O4B Cu1 O4A C16A 72.8(15) . . . . ? O4D Cu1 O4A C16A -83.1(15) . . . . ? N3J Cu1 O4A C16A 169.9(17) . . . . ? N3I Cu1 O4A C16A 168.8(17) . . . . ? Cu2 Cu1 O4A C16A -5.9(14) . . . . ? O5B Cu2 O5A C16A -80.0(17) . . . . ? O5D Cu2 O5A C16A 95.5(18) . . . . ? O3E Cu2 O5A C16A -170.7(17) . . . . ? Cu1 Cu2 O5A C16A 7.4(17) . . . . ? Cu2 O5A C16A C13A 170.1(12) . . . . ? Cu1 O4A C16A C13A -171.3(11) . . . . ? O5A C16A C13A N1A -152.1(17) . . . . ? O4A C16A C13A C14A 147.0(19) . . . . ? N1B C1B C2B C6B 172.7(19) . . . . ? C1B C2B C3B C9B -179.0(18) . . . . ? C9B C3B C4B C5B 178.0(19) . . . . ? C12B C4B C5B N1B -171.2(17) . . . . ? C1B C2B C6B C7B 178.2(18) . . . . ? C5B C4B C12B C11B 179.7(17) . . . . ? O1B C1B N1B C5B -174.2(18) . . . . ? C2B C1B N1B C13B -172.8(17) . . . . ? O2B C5B N1B C1B -177.1(18) . . . . ? C4B C5B N1B C13B 173.1(17) . . . . ? C16B C13B N1B C5B -141.9(18) . . . . ? N1B C13B C14B C15B -165.1(16) . . . . ? N1B C13B C16B O5B -139.2(17) . . . . ? C14B C13B C16B O4B 175.7(14) . . . . ? C13B C16B O4B Cu1 175.6(12) . . . . ? O4C Cu1 O4B C16B 84.1(13) . . . . ? O4A Cu1 O4B C16B -90.8(13) . . . . ? N3J Cu1 O4B C16B 170.7(15) . . . . ? N3I Cu1 O4B C16B -179.7(14) . . . . ? Cu2 Cu1 O4B C16B -2.6(12) . . . . ? C13B C16B O5B Cu2 -175.3(13) . . . . ? O5C Cu2 O5B C16B -76.1(14) . . . . ? O5A Cu2 O5B C16B 82.6(14) . . . . ? O3E Cu2 O5B C16B 178.5(14) . . . . ? Cu1 Cu2 O5B C16B 3.7(13) . . . . ? N1C C13C C14C C15C -52(3) . . . . ? C16C C13C C14C C15C -175.0(18) . . . . ? C13C C14C C15C O3C -44(3) . . . . ? C13C C14C C15C N2C 133(2) . . . . ? N1C C13C C16C O5C -158.0(16) . . . . ? C14C C13C C16C O4C 145.5(16) . . . . ? C13C C16C O4C Cu1 -171.8(12) . . . . ? O4B Cu1 O4C C16C -83.3(13) . . . . ? O4D Cu1 O4C C16C 72.5(13) . . . . ? N3J Cu1 O4C C16C 179.8(15) . . . . ? N3I Cu1 O4C C16C -179.4(15) . . . . ? Cu2 Cu1 O4C C16C -4.6(12) . . . . ? C13C C16C O5C Cu2 173.4(13) . . . . ? O5B Cu2 O5C C16C 88.3(14) . . . . ? O5D Cu2 O5C C16C -86.6(14) . . . . ? O3E Cu2 O5C C16C 179.9(13) . . . . ? Cu1 Cu2 O5C C16C 1.5(13) . . . . ? C1D C2D C3D C9D 179.0(18) . . . . ? C2D C1D N1D C13D -172.7(16) . . . . ? C4D C5D N1D C13D 173.1(18) . . . . ? C14D C13D C16D O4D 166.9(15) . . . . ? C13D C16D O4D Cu1 177.5(10) . . . . ? O4C Cu1 O4D C16D -86.3(14) . . . . ? O4A Cu1 O4D C16D 89.5(14) . . . . ? N3J Cu1 O4D C16D -172.6(15) . . . . ? N3I Cu1 O4D C16D 177.4(15) . . . . ? Cu2 Cu1 O4D C16D 0.6(13) . . . . ? C13D C16D O5D Cu2 -178.3(15) . . . . ? O5C Cu2 O5D C16D 82.4(17) . . . . ? O5A Cu2 O5D C16D -76.6(17) . . . . ? O3E Cu2 O5D C16D -172.4(17) . . . . ? Cu1 Cu2 O5D C16D 2.3(17) . . . . ? O1E C1E C2E C3E 177.5(13) . . . . ? N1E C1E C2E C3E 1.3(10) . . . . ? O1E C1E C2E C6E -0.9(15) . . . . ? N1E C1E C2E C6E -177.1(14) . . . . ? C6E C2E C3E C4E 177.0(16) . . . . ? C1E C2E C3E C4E -1.2(12) . . . . ? C6E C2E C3E C9E -4.5(15) . . . . ? C1E C2E C3E C9E 177.3(11) . . . . ? C2E C3E C4E C12E 177.0(14) . . . . ? C9E C3E C4E C5E -172.3(16) . . . . ? C3E C4E C5E O2E -176.9(19) . . . . ? C12E C4E C5E N1E 177.9(14) . . . . ? C1E C2E C6E C7E -177.4(14) . . . . ? C4E C3E C9E C8E -174.4(16) . . . . ? C2E C3E C9E C10E 175.7(12) . . . . ? C5E C4E C12E C11E 177.3(15) . . . . ? O1E C1E N1E C5E 177.6(13) . . . . ? C2E C1E N1E C5E -5.9(17) . . . . ? C2E C1E N1E C13E 176.0(10) . . . . ? O2E C5E N1E C1E 179.0(14) . . . . ? C4E C5E N1E C13E -172.3(15) . . . . ? C14E C13E N1E C1E -77.1(18) . . . . ? C16E C13E N1E C1E 55.7(19) . . . . ? C14E C13E N1E C5E 104.8(19) . . . . ? C16E C13E N1E C5E -122.3(17) . . . . ? N1E C13E C14E C15E -151.8(17) . . . . ? N1E C13E C16E O5E -152.4(14) . . . . ? C14E C13E C16E O4E 156.8(16) . . . . ? C14E C15E O3E Cu2 164.3(15) . . . . ? C13E C16E O4E Cu3 -178.5(11) . . . . ? O4F Cu3 O4E C16E 79.8(11) . . . . ? O4H Cu3 O4E C16E -88.0(11) . . . . ? O36 Cu3 O4E C16E 168.6(11) . . . . ? Cu4 Cu3 O4E C16E -1.9(11) . . . . ? C13E C16E O5E Cu4 -179.8(10) . . . . ? O5H Cu4 O5E C16E 82.0(14) . . . . ? O5F Cu4 O5E C16E -89.7(14) . . . . ? O3Z Cu4 O5E C16E -173.4(15) . . . . ? O3A Cu4 O5E C16E 176.2(15) . . . . ? Cu3 Cu4 O5E C16E -1.2(13) . . . . ? N1F C1F C2F C6F -171.7(18) . . . . ? C1F C2F C3F C9F -177.9(19) . . . . ? C2F C3F C4F C12F 177(2) . . . . ? C9F C3F C4F C5F 176.1(19) . . . . ? C3F C4F C5F O2F -173(2) . . . . ? C12F C4F C5F N1F -176.2(16) . . . . ? C1F C2F C6F C7F -179.9(17) . . . . ? C5F C4F C12F C11F -173.2(17) . . . . ? O1F C1F N1F C5F 178.6(18) . . . . ? C2F C1F N1F C13F 178.0(17) . . . . ? O2F C5F N1F C1F 174.6(18) . . . . ? C4F C5F N1F C13F -179.8(17) . . . . ? C16F C13F N1F C5F -124.1(18) . . . . ? C14F C13F N1F C5F 100.4(19) . . . . ? N1F C13F C14F C15F -160.3(13) . . . . ? C13F C14F C15F N2F -147.6(15) . . . . ? N1F C13F C16F O5F -146.1(15) . . . . ? C14F C13F C16F O4F 167.0(14) . . . . ? C13F C16F O4F Cu3 162.7(11) . . . . ? O4G Cu3 O4F C16F 91.9(12) . . . . ? O4E Cu3 O4F C16F -81.6(12) . . . . ? O36 Cu3 O4F C16F -174.9(13) . . . . ? Cu4 Cu3 O4F C16F 9.8(12) . . . . ? O4F C16F O5F Cu4 9.0(19) . . . . ? C13F C16F O5F Cu4 -167.7(12) . . . . ? O5E Cu4 O5F C16F 77.5(11) . . . . ? O5G Cu4 O5F C16F -86.9(12) . . . . ? O3Z Cu4 O5F C16F -177.8(13) . . . . ? O3A Cu4 O5F C16F 167.9(13) . . . . ? Cu3 Cu4 O5F C16F -1.9(11) . . . . ? O1H C1H C2H C3H -174.6(17) . . . . ? N1H C1H C2H C6H -174.0(16) . . . . ? C6H C2H C3H C4H 179.3(17) . . . . ? C1H C2H C3H C9H -176.1(17) . . . . ? C2H C3H C4H C12H -175.1(17) . . . . ? C9H C3H C4H C5H 173.8(17) . . . . ? C3H C4H C5H O2H 175.8(19) . . . . ? C12H C4H C5H N1H 172.5(15) . . . . ? C1H C2H C6H C7H -179.8(16) . . . . ? C4H C3H C9H C8H 178.7(18) . . . . ? C2H C3H C9H C10H 178.9(18) . . . . ? C5H C4H C12H C11H -173.6(17) . . . . ? O1H C1H N1H C5H 171.3(15) . . . . ? C2H C1H N1H C13H 174.2(15) . . . . ? O2H C5H N1H C1H -171.5(16) . . . . ? C4H C5H N1H C13H -176.1(15) . . . . ? C14H C13H N1H C5H 107.6(18) . . . . ? C16H C13H N1H C5H -126.5(16) . . . . ? C16H C13H C14H C15H 165.2(15) . . . . ? C13H C14H C15H O3H -61.3(15) . . . . ? C13H C14H C15H N2H 118.6(14) . . . . ? N1H C13H C16H O5H -127.2(15) . . . . ? N1H C13H C16H O4H 53.6(18) . . . . ? C14H C13H C16H O4H 179.9(15) . . . . ? C13H C16H O4H Cu3 177.2(9) . . . . ? O4G Cu3 O4H C16H -78.5(12) . . . . ? O4E Cu3 O4H C16H 95.9(12) . . . . ? O36 Cu3 O4H C16H -171.7(12) . . . . ? Cu4 Cu3 O4H C16H 4.4(11) . . . . ? C13H C16H O5H Cu4 177.2(9) . . . . ? O5E Cu4 O5H C16H -73.9(13) . . . . ? O5G Cu4 O5H C16H 90.7(13) . . . . ? O3Z Cu4 O5H C16H -178.4(13) . . . . ? O3A Cu4 O5H C16H -164.6(14) . . . . ? Cu3 Cu4 O5H C16H 5.4(12) . . . . ? O4C Cu1 N3I C21I 170.2(13) . . . . ? O4A Cu1 N3I C21I -11.4(14) . . . . ? O4B Cu1 N3I C21I 78.6(14) . . . . ? O4D Cu1 N3I C21I -98.0(14) . . . . ? O4C Cu1 N3I C25I -9.2(15) . . . . ? O4A Cu1 N3I C25I 169.2(15) . . . . ? O4B Cu1 N3I C25I -100.8(14) . . . . ? O4D Cu1 N3I C25I 82.5(15) . . . . ? O4C Cu1 N3J C21J 166.8(14) . . . . ? O4A Cu1 N3J C21J -14.8(14) . . . . ? O4B Cu1 N3J C21J 76.3(13) . . . . ? O4D Cu1 N3J C21J -104.4(13) . . . . ? O4C Cu1 N3J C25J -26.5(15) . . . . ? O4A Cu1 N3J C25J 151.8(14) . . . . ? O4B Cu1 N3J C25J -117.0(15) . . . . ? O4D Cu1 N3J C25J 62.3(16) . . . . ? O4G Cu3 O36 C31 117.8(19) . . . . ? O4F Cu3 O36 C31 23.8(19) . . . . ? O4H Cu3 O36 C31 -152.1(18) . . . . ? O4E Cu3 O36 C31 -65.7(19) . . . . ? C32 O37 C31 C34 -166.6(17) . . . . ? O37 C31 C34 O38 -173.5(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2A H2A1 O5E 0.88 2.30 3.03(3) 141.2 . N2A H2A1 O5F 0.88 2.62 3.18(3) 122.9 . N2A H2A2 O3B 0.88 2.33 3.16(3) 156.9 . N2Z H2Z1 O5H 0.88 2.45 3.12(3) 133.5 . N2Z H2Z2 O1D 0.88 2.22 2.94(3) 139.0 . N2B H2B1 O3F 0.88 2.15 2.99(2) 159.3 . N2E H2E1 O5D 0.88 2.16 2.91(2) 142.5 . N2E H2E2 O1H 0.88 2.05 2.85(2) 150.8 . N2F H2F1 O3B 0.88 1.99 2.86(2) 171.2 . N2H H2H2 O3D 0.88 2.12 2.88(3) 143.9 . N2G H2G1 O1C 0.88 2.18 2.99(2) 154.2 1_455 N2F H2F2 O3C 0.88 2.10 2.95(2) 164.3 1_455 N2C H2C1 O3Z 0.88 2.48 3.24(3) 145.1 1_655 N2C H2C2 O3G 0.88 2.22 3.09(2) 171.1 1_655 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 18.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.488 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.089 _vrf_THETM01_8 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: No diffraction observed at high angle due to extensive disorder. ; _vrf_PLAT023_8 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 18.00 Deg. RESPONSE: No diffraction observed at high angle due to extensive disorder. ; _vrf_PLAT201_8 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 187 RESPONSE: Many atoms refined isotropically due to prevent physically unreasonable displacement parameters. This is because of the moderate crystallinity of the available crystals. ; _vrf_PLAT602_8 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: Voids of volume 5877.7 cubic angstroms are present which are filled with disordered species. The disorder could not be successfully modeled. The Squeeze program was used to account for the diffusely scattering species in these regions. ; #===END data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C138 H103 Cu4 N17 O43, C5 H10 O3' _chemical_formula_sum 'C143 H113 Cu4 N17 O46' _chemical_formula_weight 3059.66 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.2568(11) _cell_length_b 21.8967(16) _cell_length_c 52.720(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17612(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9135 _cell_measurement_theta_min 2.244 _cell_measurement_theta_max 23.946 _exptl_crystal_description 'rectangular bar' _exptl_crystal_colour blue _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6296 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8546 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS Version 2.05 (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 236144 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 24.14 _reflns_number_total 28085 _reflns_number_gt 24342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1287P)^2^+33.1344P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.059(13) _refine_ls_number_reflns 28085 _refine_ls_number_parameters 853 _refine_ls_number_restraints 1116 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.2128 _refine_ls_wR_factor_gt 0.2061 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.97257(5) 0.43063(4) 0.304966(13) 0.03382(19) Uani 1 1 d D . . Cu2 Cu 0.94913(5) 0.42152(3) 0.355051(12) 0.03082(18) Uani 1 1 d . B . Cu3 Cu 0.55974(5) 0.54403(3) 0.459513(13) 0.03080(17) Uani 1 1 d . . . Cu4 Cu 0.58235(4) 0.52063(3) 0.411138(13) 0.02702(17) Uani 1 1 d . A . C1G C 0.4253(4) 0.7221(3) 0.42741(13) 0.0456(17) Uiso 1 1 d D . . C2G C 0.4219(5) 0.7837(3) 0.43917(14) 0.0530(19) Uiso 1 1 d D . . C3G C 0.3517(5) 0.8021(3) 0.45369(15) 0.059(2) Uiso 1 1 d D . . C4G C 0.2782(5) 0.7642(3) 0.45659(16) 0.064(2) Uiso 1 1 d D . . C5G C 0.2767(5) 0.7041(4) 0.44488(17) 0.071(2) Uiso 1 1 d D . . C6G C 0.4909(5) 0.8217(4) 0.43594(17) 0.068(2) Uiso 1 1 d D . . H6G H 0.5372 0.8098 0.4250 0.082 Uiso 1 1 calc R . . C7G C 0.4958(7) 0.8801(4) 0.44879(19) 0.085(3) Uiso 1 1 d D . . H7G H 0.5456 0.9059 0.4472 0.102 Uiso 1 1 calc R . . C8G C 0.4258(6) 0.8963(5) 0.4632(2) 0.099(3) Uiso 1 1 d D . . H8G H 0.4276 0.9341 0.4720 0.119 Uiso 1 1 calc R . . C9G C 0.3523(5) 0.8602(4) 0.46566(17) 0.071(2) Uiso 1 1 d D . . C10G C 0.2799(6) 0.8760(5) 0.4811(2) 0.085(3) Uiso 1 1 d D . . H10G H 0.2813 0.9136 0.4901 0.102 Uiso 1 1 calc R . . C11G C 0.2129(7) 0.8415(4) 0.4835(2) 0.086(3) Uiso 1 1 d D . . H11G H 0.1651 0.8549 0.4936 0.103 Uiso 1 1 calc R . . C12G C 0.2079(6) 0.7837(4) 0.47132(19) 0.086(3) Uiso 1 1 d D . . H12G H 0.1574 0.7587 0.4732 0.103 Uiso 1 1 calc R . . C13G C 0.3509(5) 0.6251(3) 0.41819(14) 0.0516(19) Uiso 1 1 d D . . H13G H 0.2986 0.6023 0.4246 0.062 Uiso 1 1 calc R . . N1G N 0.3523(4) 0.6852(3) 0.43147(12) 0.0530(16) Uiso 1 1 d D . . O1G O 0.4868(3) 0.7037(2) 0.41517(9) 0.0427(11) Uiso 1 1 d D . . O2G O 0.2150(5) 0.6668(3) 0.44595(14) 0.090(2) Uiso 1 1 d D . . C14G C 0.3365(7) 0.6356(4) 0.38991(18) 0.071(2) Uiso 1 1 d . . . H14O H 0.2950 0.6699 0.3876 0.086 Uiso 1 1 calc R . . H14P H 0.3929 0.6476 0.3821 0.086 Uiso 1 1 calc R . . C15G C 0.3018(6) 0.5812(5) 0.37656(18) 0.069(2) Uiso 1 1 d . . . C16G C 0.4320(4) 0.5866(3) 0.42463(12) 0.0370(14) Uiso 1 1 d . . . N2G N 0.3072(7) 0.5846(5) 0.3518(2) 0.110(3) Uiso 1 1 d . . . H2G1 H 0.2879 0.5543 0.3424 0.132 Uiso 1 1 calc R . . H2G2 H 0.3301 0.6171 0.3446 0.132 Uiso 1 1 calc R . . O3G O 0.2712(5) 0.5379(3) 0.38700(14) 0.0823(19) Uiso 1 1 d . . . O4G O 0.4512(3) 0.5830(2) 0.44727(8) 0.0400(10) Uiso 1 1 d . . . O5G O 0.4662(3) 0.55772(19) 0.40604(8) 0.0367(10) Uiso 1 1 d . . . C1A C 0.6851(10) 0.4468(5) 0.27962(19) 0.044(3) Uiso 0.517(10) 1 d PD A 1 C2A C 0.6685(16) 0.4610(7) 0.2521(2) 0.089(6) Uiso 0.517(10) 1 d PD A 1 C3A C 0.6370(18) 0.5157(7) 0.2440(3) 0.090(7) Uiso 0.517(10) 1 d PD A 1 C4A C 0.6301(11) 0.5640(6) 0.2610(2) 0.067(5) Uiso 0.517(10) 1 d PD A 1 C5A C 0.6578(12) 0.5568(6) 0.2867(2) 0.052(4) Uiso 0.517(10) 1 d PD A 1 C6A C 0.6667(12) 0.4131(7) 0.2360(2) 0.067(5) Uiso 0.517(10) 1 d PD A 1 H6A H 0.6763 0.3729 0.2423 0.080 Uiso 0.517(10) 1 calc PR A 1 C7A C 0.650(2) 0.4228(9) 0.2091(3) 0.124(10) Uiso 0.517(10) 1 d PD A 1 H7A H 0.6596 0.3911 0.1970 0.148 Uiso 0.517(10) 1 calc PR A 1 C8A C 0.6208(18) 0.4784(8) 0.2017(3) 0.108(8) Uiso 0.517(10) 1 d PD A 1 H8A H 0.6070 0.4849 0.1843 0.129 Uiso 0.517(10) 1 calc PR A 1 C9A C 0.6104(18) 0.5259(8) 0.2186(3) 0.109(8) Uiso 0.517(10) 1 d PD A 1 C10A C 0.573(3) 0.5840(10) 0.2130(4) 0.120(3) Uiso 0.517(10) 1 d PD A 1 H10A H 0.5534 0.5913 0.1961 0.144 Uiso 0.517(10) 1 calc PR A 1 C11A C 0.5628(17) 0.6265(9) 0.2291(3) 0.109(8) Uiso 0.517(10) 1 d PD A 1 H11A H 0.5356 0.6636 0.2241 0.131 Uiso 0.517(10) 1 calc PR A 1 C12A C 0.5919(15) 0.6196(7) 0.2545(3) 0.095(7) Uiso 0.517(10) 1 d PD A 1 H12A H 0.5856 0.6516 0.2666 0.114 Uiso 0.517(10) 1 calc PR A 1 C13A C 0.7139(5) 0.4854(4) 0.32045(13) 0.0521(18) Uiso 0.517(10) 1 d PD A 1 H13A H 0.7116 0.5259 0.3292 0.063 Uiso 0.517(10) 1 calc PR A 1 N1A N 0.6851(10) 0.4989(5) 0.29456(17) 0.060(4) Uiso 0.517(10) 1 d PD A 1 O1A O 0.7071(7) 0.3969(4) 0.28601(18) 0.041(3) Uiso 0.517(10) 1 d PD A 1 O2A O 0.6555(11) 0.5973(6) 0.3039(3) 0.098(5) Uiso 0.517(10) 1 d PD A 1 C1Z C 0.697(3) 0.4153(8) 0.2834(3) 0.120(3) Uiso 0.483(10) 1 d PD A 2 C2Z C 0.675(2) 0.4127(8) 0.2555(3) 0.120(3) Uiso 0.483(10) 1 d PD A 2 C3Z C 0.654(2) 0.4639(8) 0.2416(3) 0.120(3) Uiso 0.483(10) 1 d PD A 2 C4Z C 0.646(2) 0.5209(8) 0.2530(3) 0.120(3) Uiso 0.483(10) 1 d PD A 2 C5Z C 0.661(2) 0.5254(8) 0.2799(3) 0.120(3) Uiso 0.483(10) 1 d PD A 2 C6Z C 0.680(2) 0.3580(8) 0.2438(3) 0.120(3) Uiso 0.483(10) 1 d PD A 2 H6Z H 0.6931 0.3225 0.2534 0.144 Uiso 0.483(10) 1 calc PR A 2 C7Z C 0.664(2) 0.3527(9) 0.2162(4) 0.120(3) Uiso 0.483(10) 1 d PD A 2 H7Z H 0.6767 0.3165 0.2071 0.144 Uiso 0.483(10) 1 calc PR A 2 C8Z C 0.630(2) 0.4027(9) 0.2050(4) 0.120(3) Uiso 0.483(10) 1 d PD A 2 H8Z H 0.6002 0.3979 0.1893 0.144 Uiso 0.483(10) 1 calc PR A 2 C9Z C 0.636(2) 0.4605(8) 0.2152(3) 0.120(3) Uiso 0.483(10) 1 d PD A 2 C10Z C 0.602(2) 0.5134(9) 0.2032(4) 0.120(3) Uiso 0.483(10) 1 d PD A 2 H10Z H 0.5897 0.5115 0.1855 0.144 Uiso 0.483(10) 1 calc PR A 2 C11Z C 0.586(3) 0.5630(11) 0.2148(4) 0.120(3) Uiso 0.483(10) 1 d PD A 2 H11Z H 0.5581 0.5957 0.2060 0.144 Uiso 0.483(10) 1 calc PR A 2 C12Z C 0.6079(19) 0.5706(9) 0.2408(4) 0.120(3) Uiso 0.483(10) 1 d PD A 2 H12Z H 0.5971 0.6080 0.2494 0.144 Uiso 0.483(10) 1 calc PR A 2 C13Z C 0.7139(5) 0.4854(4) 0.32045(13) 0.0521(18) Uiso 0.483(10) 1 d PD A 2 H13Z H 0.7057 0.5295 0.3247 0.063 Uiso 0.483(10) 1 calc PR A 2 N1Z N 0.6832(10) 0.4721(6) 0.29378(18) 0.060(4) Uiso 0.483(10) 1 d PD A 2 O1Z O 0.7157(9) 0.3697(6) 0.2955(3) 0.075(4) Uiso 0.483(10) 1 d PD A 2 O2Z O 0.6521(18) 0.5742(8) 0.2922(4) 0.126(8) Uiso 0.483(10) 1 d PD A 2 C14A C 0.6532(6) 0.4450(4) 0.33646(15) 0.061(2) Uiso 1 1 d D . . H14A H 0.5924 0.4510 0.3304 0.073 Uiso 1 1 calc R A 1 H14B H 0.6688 0.4018 0.3332 0.073 Uiso 1 1 calc R A 1 C15A C 0.6548(4) 0.4553(3) 0.36425(13) 0.0432(16) Uiso 1 1 d D A . N2A N 0.6826(4) 0.4101(3) 0.37865(12) 0.0512(15) Uiso 1 1 d D . . H2A1 H 0.6801 0.4133 0.3953 0.061 Uiso 1 1 calc R A . H2A2 H 0.7037 0.3767 0.3717 0.061 Uiso 1 1 calc R . . O3A O 0.6244(3) 0.5035(2) 0.37285(9) 0.0490(12) Uiso 1 1 d D . . O4A O 0.8550(3) 0.4662(2) 0.30238(9) 0.0458(11) Uiso 1 1 d . A . O5A O 0.8329(3) 0.4565(2) 0.34465(8) 0.0364(10) Uiso 1 1 d . . . C16A C 0.8083(5) 0.4677(3) 0.32200(13) 0.0425(16) Uiso 1 1 d . A . C1B C 1.0025(4) 0.2149(3) 0.31171(13) 0.0481(18) Uiso 1 1 d D . . C2B C 1.0526(5) 0.1764(4) 0.29377(14) 0.0566(19) Uiso 1 1 d D . . C3B C 1.0116(4) 0.1420(4) 0.27516(14) 0.0539(19) Uiso 1 1 d D . . C4B C 0.9218(4) 0.1421(3) 0.27312(14) 0.0539(19) Uiso 1 1 d D . . C5B C 0.8666(4) 0.1826(3) 0.28908(13) 0.0464(17) Uiso 1 1 d D . . C6B C 1.1424(6) 0.1765(5) 0.29631(18) 0.076(3) Uiso 1 1 d D . . H6B H 1.1704 0.1987 0.3095 0.091 Uiso 1 1 calc R . . C7B C 1.1927(7) 0.1413(5) 0.27801(19) 0.084(3) Uiso 1 1 d D . . H7B H 1.2548 0.1405 0.2790 0.101 Uiso 1 1 calc R . . C8B C 1.1511(6) 0.1098(5) 0.2597(2) 0.089(3) Uiso 1 1 d D . . H8B H 1.1857 0.0876 0.2479 0.107 Uiso 1 1 calc R . . C9B C 1.0616(5) 0.1078(4) 0.25702(16) 0.069(2) Uiso 1 1 d D . . C10B C 1.0152(5) 0.0766(4) 0.23794(16) 0.066(2) Uiso 1 1 d D . . H10B H 1.0477 0.0551 0.2254 0.079 Uiso 1 1 calc R . . C11B C 0.9332(6) 0.0756(4) 0.23659(17) 0.072(2) Uiso 1 1 d D . . H11B H 0.9057 0.0522 0.2237 0.086 Uiso 1 1 calc R . . C12B C 0.8803(5) 0.1094(4) 0.25419(15) 0.062(2) Uiso 1 1 d D . . H12B H 0.8183 0.1093 0.2529 0.075 Uiso 1 1 calc R . . C13B C 0.8596(4) 0.2563(3) 0.32471(12) 0.0354(14) Uiso 1 1 d D B . H13B H 0.8005 0.2616 0.3168 0.043 Uiso 1 1 calc R . . N1B N 0.9113(3) 0.2177(2) 0.30738(10) 0.0409(13) Uiso 1 1 d D . . O1B O 1.0340(4) 0.2449(2) 0.32865(10) 0.0564(13) Uiso 1 1 d D . . O2B O 0.7876(4) 0.1842(3) 0.28797(13) 0.0755(17) Uiso 1 1 d D . . C14B C 0.8451(5) 0.2263(3) 0.35008(13) 0.0420(16) Uiso 1 1 d . . . H14C H 0.8277 0.1832 0.3474 0.050 Uiso 1 1 calc R . . H14D H 0.9007 0.2265 0.3598 0.050 Uiso 1 1 calc R . . C15B C 0.7762(5) 0.2580(3) 0.36503(13) 0.0415(16) Uiso 1 1 d . . . C16B C 0.9000(4) 0.3195(3) 0.32656(11) 0.0313(13) Uiso 1 1 d . . . N2B N 0.7855(5) 0.2614(3) 0.39021(12) 0.0544(16) Uiso 1 1 d . . . H2B1 H 0.7458 0.2804 0.3994 0.065 Uiso 1 1 calc R . . H2B2 H 0.8313 0.2447 0.3976 0.065 Uiso 1 1 calc R . . O3B O 0.7109(4) 0.2819(2) 0.35456(10) 0.0561(13) Uiso 1 1 d . . . O4B O 0.9213(3) 0.34569(19) 0.30643(8) 0.0364(10) Uiso 1 1 d . B . O5B O 0.9043(3) 0.3412(2) 0.34865(8) 0.0369(10) Uiso 1 1 d . B . C1C C 1.2625(7) 0.4521(4) 0.30836(19) 0.0898(8) Uiso 1 1 d D . . C2C C 1.3057(7) 0.4685(4) 0.28410(18) 0.0898(8) Uiso 1 1 d D . . C3C C 1.3445(7) 0.4249(4) 0.26854(18) 0.0898(8) Uiso 1 1 d D . . C4C C 1.3432(7) 0.3646(4) 0.27439(19) 0.0898(8) Uiso 1 1 d D . . C5C C 1.2960(7) 0.3419(4) 0.29740(19) 0.0898(8) Uiso 1 1 d D . . C6C C 1.3092(7) 0.5296(5) 0.27788(19) 0.0898(8) Uiso 1 1 d D . . H6C H 1.2842 0.5591 0.2890 0.108 Uiso 1 1 calc R . . C7C C 1.3507(7) 0.5492(5) 0.25465(19) 0.0898(8) Uiso 1 1 d D . . H7C H 1.3549 0.5911 0.2501 0.108 Uiso 1 1 calc R . . C8C C 1.3830(7) 0.5046(4) 0.2397(2) 0.0898(8) Uiso 1 1 d D . . H8C H 1.4051 0.5166 0.2237 0.108 Uiso 1 1 calc R . . C9C C 1.3872(7) 0.4439(4) 0.24538(19) 0.0898(8) Uiso 1 1 d D . . C10C C 1.4227(8) 0.3962(4) 0.2313(2) 0.0898(8) Uiso 1 1 d D . . H10C H 1.4515 0.4073 0.2160 0.108 Uiso 1 1 calc R . . C11C C 1.4213(8) 0.3413(5) 0.23638(19) 0.0898(8) Uiso 1 1 d D . . H11C H 1.4486 0.3131 0.2252 0.108 Uiso 1 1 calc R . . C12C C 1.3792(7) 0.3194(5) 0.25880(19) 0.0898(8) Uiso 1 1 d D . . H12C H 1.3758 0.2772 0.2628 0.108 Uiso 1 1 calc R . . C13C C 1.2117(7) 0.3704(5) 0.33632(19) 0.0898(8) Uiso 1 1 d D B . H13C H 1.2144 0.3248 0.3371 0.108 Uiso 1 1 calc R . . N1C N 1.2618(6) 0.3892(4) 0.31313(16) 0.0898(8) Uiso 1 1 d D . . O1C O 1.2255(4) 0.4869(3) 0.32175(11) 0.0639(15) Uiso 1 1 d D . . O2C O 1.2851(5) 0.2896(3) 0.30342(13) 0.0786(18) Uiso 1 1 d D . . C14C C 1.2482(5) 0.3939(4) 0.36101(16) 0.056(2) Uiso 1 1 d . . . H14E H 1.2349 0.4381 0.3623 0.067 Uiso 1 1 calc R . . H14F H 1.2178 0.3731 0.3752 0.067 Uiso 1 1 calc R . . C15C C 1.3448(5) 0.3851(4) 0.36412(15) 0.0513(19) Uiso 1 1 d . . . C16C C 1.1154(5) 0.3875(3) 0.33310(13) 0.0405(15) Uiso 1 1 d . . . N2C N 1.3878(5) 0.4311(3) 0.37539(13) 0.0643(18) Uiso 1 1 d . . . H2C1 H 1.4436 0.4270 0.3793 0.077 Uiso 1 1 calc R . . H2C2 H 1.3603 0.4654 0.3789 0.077 Uiso 1 1 calc R . . O3C O 1.3806(4) 0.3356(3) 0.35870(12) 0.0734(17) Uiso 1 1 d . . . O4C O 1.0879(3) 0.3964(2) 0.31064(8) 0.0400(10) Uiso 1 1 d . B . O5C O 1.0724(3) 0.3909(2) 0.35335(9) 0.0444(11) Uiso 1 1 d . B . C1D C 0.9315(4) 0.6411(3) 0.32158(14) 0.0527(19) Uiso 1 1 d D . . C2D C 0.8976(5) 0.6844(4) 0.30195(17) 0.073(3) Uiso 1 1 d D . . C3D C 0.9543(5) 0.7182(4) 0.28711(16) 0.067(2) Uiso 1 1 d D . . C4D C 1.0422(5) 0.7117(4) 0.28932(16) 0.066(2) Uiso 1 1 d D . . C5D C 1.0835(5) 0.6709(4) 0.30872(15) 0.063(2) Uiso 1 1 d D . . C6D C 0.8085(6) 0.6882(5) 0.2995(2) 0.090(3) Uiso 1 1 d D . . H6D H 0.7713 0.6653 0.3103 0.108 Uiso 1 1 calc R . . C7D C 0.7718(9) 0.7275(7) 0.2803(3) 0.125 Uiso 1 1 d D . . H7D H 0.7102 0.7309 0.2780 0.150 Uiso 1 1 calc R . . C8D C 0.8288(7) 0.7592(6) 0.2656(2) 0.111(4) Uiso 1 1 d D . . H8D H 0.8050 0.7858 0.2532 0.133 Uiso 1 1 calc R . . C9D C 0.9181(6) 0.7555(5) 0.26745(18) 0.082(3) Uiso 1 1 d D . . C10D C 0.9777(6) 0.7838(5) 0.2512(2) 0.085(3) Uiso 1 1 d D . . H10D H 0.9554 0.8058 0.2371 0.102 Uiso 1 1 calc R . . C11D C 1.0591(6) 0.7819(5) 0.25428(19) 0.082(3) Uiso 1 1 d D . . H11D H 1.0959 0.8053 0.2435 0.098 Uiso 1 1 calc R . . C12D C 1.0986(7) 0.7446(5) 0.27395(19) 0.088(3) Uiso 1 1 d D . . H12D H 1.1603 0.7428 0.2762 0.106 Uiso 1 1 calc R . . C13D C 1.0574(5) 0.5949(3) 0.34354(12) 0.0467(17) Uiso 1 1 d D B . H13D H 1.1221 0.5923 0.3408 0.056 Uiso 1 1 calc R . . N1D N 1.0217(4) 0.6391(3) 0.32438(12) 0.0562(16) Uiso 1 1 d D . . O1D O 0.8861(3) 0.6099(2) 0.33488(10) 0.0515(13) Uiso 1 1 d D . . O2D O 1.1600(4) 0.6604(3) 0.31089(13) 0.0765(18) Uiso 1 1 d D . . C14D C 1.0426(6) 0.6229(4) 0.36947(13) 0.061(2) Uiso 1 1 d D . . H14G H 0.9788 0.6292 0.3716 0.073 Uiso 1 1 calc R . . H14H H 1.0608 0.5924 0.3823 0.073 Uiso 1 1 calc R . . C15D C 1.0865(5) 0.6809(4) 0.37568(16) 0.061(2) Uiso 1 1 d D . . C16D C 1.0201(4) 0.5313(3) 0.33985(13) 0.0404(15) Uiso 1 1 d D . . N2D N 1.0355(8) 0.7229(5) 0.3858(2) 0.123(4) Uiso 1 1 d D . . H2D1 H 1.0545 0.7607 0.3874 0.148 Uiso 1 1 calc R . . H2D2 H 0.9826 0.7131 0.3911 0.148 Uiso 1 1 calc R . . O3D O 1.1615(5) 0.6944(3) 0.36823(14) 0.089(2) Uiso 1 1 d D . . O4D O 1.0168(3) 0.5125(2) 0.31720(8) 0.0411(10) Uiso 1 1 d . B . O5D O 0.9965(3) 0.5033(2) 0.35921(9) 0.0407(11) Uiso 1 1 d . B . C1E C 0.7531(3) 0.3898(2) 0.48418(10) 0.0292(13) Uiso 1 1 d D . . C2E C 0.7624(4) 0.3584(2) 0.50886(11) 0.0368(15) Uiso 1 1 d D . . C3E C 0.8332(4) 0.3735(3) 0.52526(11) 0.0370(15) Uiso 1 1 d D . . C4E C 0.8942(4) 0.4187(3) 0.51929(11) 0.0369(14) Uiso 1 1 d D . . C5E C 0.8886(4) 0.4501(3) 0.49447(10) 0.0320(13) Uiso 1 1 d D . . C6E C 0.7016(5) 0.3149(3) 0.51498(13) 0.0498(18) Uiso 1 1 d D . . H6E H 0.6544 0.3057 0.5038 0.060 Uiso 1 1 calc R . . C7E C 0.7111(5) 0.2838(4) 0.53860(15) 0.059(2) Uiso 1 1 d D . . H7E H 0.6703 0.2527 0.5430 0.071 Uiso 1 1 calc R . . C8E C 0.7768(5) 0.2974(4) 0.55495(16) 0.062(2) Uiso 1 1 d D . . H8E H 0.7802 0.2765 0.5707 0.075 Uiso 1 1 calc R . . C9E C 0.8404(4) 0.3421(3) 0.54897(12) 0.0465(17) Uiso 1 1 d D . . C10E C 0.9111(5) 0.3587(4) 0.56523(15) 0.057(2) Uiso 1 1 d D . . H10E H 0.9174 0.3385 0.5811 0.068 Uiso 1 1 calc R . . C11E C 0.9676(6) 0.4010(4) 0.55897(15) 0.063(2) Uiso 1 1 d D . . H11E H 1.0130 0.4115 0.5705 0.076 Uiso 1 1 calc R . . C12E C 0.9623(5) 0.4314(3) 0.53553(13) 0.0511(18) Uiso 1 1 d D . . H12E H 1.0056 0.4606 0.5309 0.061 Uiso 1 1 calc R . . C13E C 0.8103(4) 0.4651(3) 0.45399(10) 0.0311(13) Uiso 1 1 d D . . H13E H 0.8498 0.5015 0.4548 0.037 Uiso 1 1 calc R . . N1E N 0.8160(3) 0.4348(2) 0.47875(8) 0.0268(10) Uiso 1 1 d D . . O1E O 0.6975(3) 0.3781(2) 0.46905(8) 0.0366(10) Uiso 1 1 d D . . O2E O 0.9427(3) 0.4863(2) 0.48687(9) 0.0510(12) Uiso 1 1 d D . . C14E C 0.8466(4) 0.4234(3) 0.43343(12) 0.0365(14) Uiso 1 1 d . . . H14I H 0.8961 0.4007 0.4410 0.044 Uiso 1 1 calc R . . H14J H 0.8004 0.3930 0.4296 0.044 Uiso 1 1 calc R . . C15E C 0.8778(4) 0.4478(3) 0.40872(12) 0.0339(14) Uiso 1 1 d . B . C16E C 0.7184(4) 0.4891(3) 0.44896(11) 0.0269(12) Uiso 1 1 d . A . N2E N 0.8701(4) 0.5071(3) 0.40291(11) 0.0446(14) Uiso 1 1 d . . . H2E1 H 0.8881 0.5205 0.3881 0.054 Uiso 1 1 calc R . . H2E2 H 0.8471 0.5326 0.4139 0.054 Uiso 1 1 calc R . . O3E O 0.9100(3) 0.41173(19) 0.39338(8) 0.0343(9) Uiso 1 1 d . . . O4E O 0.6765(3) 0.50942(19) 0.46749(8) 0.0344(10) Uiso 1 1 d . . . O5E O 0.6934(3) 0.48745(18) 0.42605(7) 0.0289(9) Uiso 1 1 d . . . C1F C 0.3463(4) 0.3780(3) 0.46057(12) 0.0407(15) Uiso 1 1 d D . . C2F C 0.2759(4) 0.3635(3) 0.47915(13) 0.0479(17) Uiso 1 1 d D . . C3F C 0.2918(4) 0.3258(3) 0.49992(12) 0.0459(17) Uiso 1 1 d D . . C4F C 0.3727(4) 0.2986(3) 0.50314(12) 0.0388(15) Uiso 1 1 d D . . C5F C 0.4441(4) 0.3089(3) 0.48506(11) 0.0370(14) Uiso 1 1 d D . . C6F C 0.1935(5) 0.3884(4) 0.47504(17) 0.071(2) Uiso 1 1 d D . . H6F H 0.1832 0.4151 0.4611 0.085 Uiso 1 1 calc R . . C7F C 0.1243(6) 0.3731(5) 0.49225(17) 0.076(3) Uiso 1 1 d D . . H7F H 0.0669 0.3886 0.4895 0.092 Uiso 1 1 calc R . . C8F C 0.1407(5) 0.3370(4) 0.51220(16) 0.067(2) Uiso 1 1 d D . . H8F H 0.0935 0.3274 0.5233 0.080 Uiso 1 1 calc R . . C9F C 0.2234(5) 0.3125(4) 0.51769(14) 0.057(2) Uiso 1 1 d D . . C10F C 0.2433(6) 0.2735(4) 0.53801(17) 0.070(2) Uiso 1 1 d D . . H10F H 0.1983 0.2638 0.5498 0.084 Uiso 1 1 calc R . . C11F C 0.3203(5) 0.2502(4) 0.54142(17) 0.067(2) Uiso 1 1 d D . . H11F H 0.3311 0.2259 0.5560 0.080 Uiso 1 1 calc R . . C12F C 0.3886(5) 0.2603(4) 0.52390(14) 0.0544(19) Uiso 1 1 d D . . H12F H 0.4441 0.2415 0.5261 0.065 Uiso 1 1 calc R . . C13F C 0.4951(4) 0.3577(3) 0.44536(11) 0.0304(13) Uiso 1 1 d D . . H13F H 0.5507 0.3414 0.4528 0.037 Uiso 1 1 calc R . . N1F N 0.4274(3) 0.3494(2) 0.46476(9) 0.0315(11) Uiso 1 1 d D . . O1F O 0.3374(3) 0.4109(2) 0.44234(9) 0.0474(12) Uiso 1 1 d D . . O2F O 0.5144(3) 0.2828(2) 0.48579(10) 0.0522(13) Uiso 1 1 d D . . C14F C 0.4760(4) 0.3190(3) 0.42212(11) 0.0305(13) Uiso 1 1 d . . . H14K H 0.4316 0.3400 0.4115 0.037 Uiso 1 1 calc R . . H14L H 0.4512 0.2794 0.4275 0.037 Uiso 1 1 calc R . . C15F C 0.5580(4) 0.3077(3) 0.40634(11) 0.0328(13) Uiso 1 1 d . . . C16F C 0.5112(4) 0.4256(3) 0.44012(11) 0.0294(12) Uiso 1 1 d . A . N2F N 0.5440(4) 0.3000(3) 0.38136(11) 0.0505(15) Uiso 1 1 d . . . H2F1 H 0.5880 0.2908 0.3713 0.061 Uiso 1 1 calc R . . H2F2 H 0.4908 0.3041 0.3751 0.061 Uiso 1 1 calc R . . O3F O 0.6295(3) 0.3028(2) 0.41635(9) 0.0406(11) Uiso 1 1 d . . . O4F O 0.5112(3) 0.46079(19) 0.45887(8) 0.0340(9) Uiso 1 1 d . . . O5F O 0.5320(3) 0.43968(17) 0.41758(7) 0.0283(9) Uiso 1 1 d . . . C1H C 0.8243(4) 0.6551(3) 0.44515(11) 0.0332(14) Uiso 1 1 d D . . C2H C 0.9042(4) 0.6622(3) 0.46167(13) 0.0459(16) Uiso 1 1 d D . . C3H C 0.9129(5) 0.7138(3) 0.47678(14) 0.0542(19) Uiso 1 1 d D . . C4H C 0.8493(5) 0.7591(3) 0.47736(14) 0.0525(19) Uiso 1 1 d D . . C5H C 0.7685(4) 0.7538(3) 0.46212(13) 0.0469(17) Uiso 1 1 d D . . C6H C 0.9675(4) 0.6181(3) 0.46110(14) 0.0525(18) Uiso 1 1 d D . . H6H H 0.9603 0.5839 0.4503 0.063 Uiso 1 1 calc R . . C7H C 1.0441(6) 0.6225(4) 0.47638(17) 0.071(2) Uiso 1 1 d D . . H7H H 1.0886 0.5922 0.4763 0.085 Uiso 1 1 calc R . . C8H C 1.0485(6) 0.6727(4) 0.49099(17) 0.071(2) Uiso 1 1 d D . . H8H H 1.0982 0.6759 0.5018 0.085 Uiso 1 1 calc R . . C9H C 0.9896(6) 0.7198(4) 0.49208(18) 0.074(3) Uiso 1 1 d D . . C10H C 0.9972(7) 0.7727(4) 0.5071(2) 0.086(3) Uiso 1 1 d D . . H10H H 1.0482 0.7780 0.5172 0.103 Uiso 1 1 calc R . . C11H C 0.9375(6) 0.8139(4) 0.50757(18) 0.073(2) Uiso 1 1 d D . . H11H H 0.9456 0.8487 0.5181 0.088 Uiso 1 1 calc R . . C12H C 0.8592(6) 0.8093(4) 0.49277(17) 0.074(3) Uiso 1 1 d D . . H12H H 0.8152 0.8400 0.4936 0.088 Uiso 1 1 calc R . . C13H C 0.6851(4) 0.6960(3) 0.42886(11) 0.0353(14) Uiso 1 1 d D . . H13H H 0.6410 0.7251 0.4360 0.042 Uiso 1 1 calc R . . N1H N 0.7641(3) 0.7028(2) 0.44536(10) 0.0367(12) Uiso 1 1 d D . . O1H O 0.8118(3) 0.6106(2) 0.43271(9) 0.0416(11) Uiso 1 1 d D . . O2H O 0.7090(4) 0.7906(3) 0.46154(12) 0.0691(16) Uiso 1 1 d D . . C14H C 0.7016(5) 0.7179(4) 0.40225(14) 0.0543(19) Uiso 1 1 d D . . H14M H 0.6478 0.7108 0.3921 0.065 Uiso 1 1 calc R . . H14N H 0.7117 0.7626 0.4028 0.065 Uiso 1 1 calc R . . C15H C 0.7747(5) 0.6897(4) 0.38916(16) 0.062(2) Uiso 1 1 d D . . N2H N 0.7586(5) 0.6423(3) 0.37438(14) 0.071(2) Uiso 1 1 d D . . H2H1 H 0.8011 0.6261 0.3653 0.085 Uiso 1 1 calc R . . H2H2 H 0.7054 0.6269 0.3736 0.085 Uiso 1 1 calc R . . O3H O 0.8504(5) 0.7123(4) 0.39050(16) 0.101(2) Uiso 1 1 d D . . C16H C 0.6443(4) 0.6351(3) 0.43114(12) 0.0343(14) Uiso 1 1 d . A . O4H O 0.6192(3) 0.6213(2) 0.45413(8) 0.0363(10) Uiso 1 1 d . . . O5H O 0.6315(3) 0.60405(19) 0.41175(8) 0.0354(10) Uiso 1 1 d . . . N3I N 0.9867(6) 0.4321(5) 0.26401(11) 0.0523(10) Uiso 0.50 1 d PGD B 1 C21I C 0.9102(5) 0.4335(5) 0.24969(17) 0.0523(10) Uiso 0.50 1 d PG B 1 H21I H 0.8548 0.4338 0.2579 0.063 Uiso 0.50 1 calc PR B 1 C22I C 0.9149(5) 0.4347(5) 0.22336(16) 0.0523(10) Uiso 0.50 1 d PG B 1 H22I H 0.8626 0.4357 0.2136 0.063 Uiso 0.50 1 calc PR B 1 C23I C 0.9960(6) 0.4344(5) 0.21136(11) 0.0523(10) Uiso 0.50 1 d PG B 1 H23I H 0.9991 0.4351 0.1934 0.063 Uiso 0.50 1 calc PR B 1 C24I C 1.0724(5) 0.4329(5) 0.22568(16) 0.0523(10) Uiso 0.50 1 d PG B 1 H24I H 1.1279 0.4327 0.2175 0.063 Uiso 0.50 1 calc PR B 1 C25I C 1.0678(5) 0.4318(5) 0.25200(15) 0.0523(10) Uiso 0.50 1 d PG B 1 H25I H 1.1201 0.4308 0.2618 0.063 Uiso 0.50 1 calc PR B 1 N3J N 0.9992(4) 0.4301(3) 0.26522(8) 0.0523(10) Uiso 0.50 1 d PGD B 2 C21J C 0.9330(4) 0.4392(3) 0.24749(8) 0.0523(10) Uiso 0.50 1 d PG B 2 H21J H 0.8734 0.4398 0.2528 0.063 Uiso 0.50 1 calc PR B 2 C22J C 0.9539(5) 0.4473(4) 0.22206(8) 0.0523(10) Uiso 0.50 1 d PG B 2 H22J H 0.9087 0.4534 0.2099 0.063 Uiso 0.50 1 calc PR B 2 C23J C 1.0410(5) 0.4463(4) 0.21434(9) 0.0523(10) Uiso 0.50 1 d PG B 2 H23J H 1.0553 0.4519 0.1970 0.063 Uiso 0.50 1 calc PR B 2 C24J C 1.1072(4) 0.4373(4) 0.23207(9) 0.0523(10) Uiso 0.50 1 d PG B 2 H24J H 1.1667 0.4367 0.2268 0.063 Uiso 0.50 1 calc PR B 2 C25J C 1.0863(4) 0.4292(4) 0.25751(9) 0.0523(10) Uiso 0.50 1 d PG B 2 H25J H 1.1315 0.4230 0.2696 0.063 Uiso 0.50 1 calc PR B 2 O36 O 0.5277(3) 0.54746(19) 0.50047(7) 0.0568(13) Uiso 1 1 d R . . O37 O 0.4153(3) 0.4854(3) 0.51464(8) 0.189(5) Uiso 1 1 d RD . . O38 O 0.6494(3) 0.4805(3) 0.52110(6) 0.134(3) Uiso 1 1 d R . . C31 C 0.5049(3) 0.5036(2) 0.51181(7) 0.155(7) Uiso 1 1 d RD . . C32 C 0.3423(3) 0.5202(4) 0.50003(8) 0.198(9) Uiso 1 1 d RD . . H32A H 0.3439 0.5072 0.4820 0.237 Uiso 1 1 calc R . . H32B H 0.3559 0.5644 0.5005 0.237 Uiso 1 1 calc R . . C33 C 0.2399(3) 0.5100(5) 0.51105(9) 0.234(12) Uiso 1 1 d RD . . H33A H 0.2341 0.4684 0.5178 0.352 Uiso 1 1 calc R . . H33B H 0.1979 0.5159 0.4972 0.352 Uiso 1 1 calc R . . H33C H 0.2281 0.5395 0.5246 0.352 Uiso 1 1 calc R . . C34 C 0.5595(4) 0.4642(2) 0.52003(7) 0.107(4) Uiso 1 1 d RD . . H34 H 0.5576 0.4311 0.5070 0.128 Uiso 1 1 calc R . . C35 C 0.5324(5) 0.4299(3) 0.54607(8) 0.188(8) Uiso 1 1 d RD . . H35A H 0.5369 0.4585 0.5603 0.281 Uiso 1 1 calc R . . H35B H 0.5720 0.3953 0.5490 0.281 Uiso 1 1 calc R . . H35C H 0.4721 0.4149 0.5447 0.281 Uiso 1 1 calc R . . O46 O 0.1918(6) 0.3257(4) 0.41522(17) 0.107(3) Uiso 1 1 d . . . O47 O 0.0763(6) 0.3902(4) 0.41754(15) 0.099(2) Uiso 1 1 d . . . O48 O -0.0409(4) 0.3013(3) 0.41344(13) 0.0762(17) Uiso 1 1 d . . . C41 C 0.1117(7) 0.3341(5) 0.4152(2) 0.078(3) Uiso 1 1 d . . . C42 C 0.1340(4) 0.4455(3) 0.41448(12) 0.079(3) Uiso 1 1 d . . . H42A H 0.1928 0.4373 0.4216 0.094 Uiso 1 1 calc R . . H42B H 0.1408 0.4555 0.3963 0.094 Uiso 1 1 calc R . . C43 C 0.0940(4) 0.4957(3) 0.42756(12) 0.091(3) Uiso 1 1 d R . . H43A H 0.0372 0.5050 0.4198 0.137 Uiso 1 1 calc R . . H43B H 0.1321 0.5316 0.4264 0.137 Uiso 1 1 calc R . . H43C H 0.0853 0.4849 0.4454 0.137 Uiso 1 1 calc R . . C44 C 0.0484(4) 0.2858(3) 0.41343(12) 0.096(3) Uiso 1 1 d R . . H44 H 0.0577 0.2595 0.4287 0.115 Uiso 1 1 calc R . . C45 C 0.0642(4) 0.2453(3) 0.39089(12) 0.157(6) Uiso 1 1 d R . . H45A H 0.0452 0.2036 0.3949 0.235 Uiso 1 1 calc R . . H45B H 0.1268 0.2452 0.3868 0.235 Uiso 1 1 calc R . . H45C H 0.0308 0.2606 0.3763 0.235 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0312(4) 0.0458(5) 0.0245(4) 0.0013(3) 0.0035(3) 0.0061(3) Cu2 0.0352(4) 0.0352(4) 0.0220(3) -0.0010(3) 0.0025(3) 0.0070(3) Cu3 0.0283(4) 0.0340(4) 0.0301(4) -0.0062(3) 0.0050(3) 0.0002(3) Cu4 0.0254(3) 0.0299(4) 0.0258(4) -0.0015(3) 0.0024(3) -0.0003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O4C 1.937(5) . ? Cu1 O4A 1.961(5) . ? Cu1 O4B 2.019(4) . ? Cu1 O4D 2.021(5) . ? Cu1 N3J 2.134(4) . ? Cu1 N3I 2.170(6) . ? Cu1 Cu2 2.6720(10) . ? Cu2 O5B 1.916(4) . ? Cu2 O5D 1.943(5) . ? Cu2 O5C 1.998(5) . ? Cu2 O5A 2.007(4) . ? Cu2 O3E 2.118(4) . ? Cu3 O4H 1.941(4) . ? Cu3 O4F 1.967(4) . ? Cu3 O4G 1.971(5) . ? Cu3 O4E 1.981(4) . ? Cu3 O36 2.215(3) . ? Cu3 Cu4 2.6241(10) . ? Cu4 O5F 1.961(4) . ? Cu4 O5G 1.968(4) . ? Cu4 O5H 1.975(4) . ? Cu4 O5E 2.004(4) . ? Cu4 O3A 2.151(5) . ? C1G O1G 1.207(7) . ? C1G N1G 1.392(7) . ? C1G C2G 1.485(8) . ? C2G C6G 1.353(9) . ? C2G C3G 1.377(9) . ? C3G C4G 1.403(9) . ? C3G C9G 1.420(9) . ? C4G C12G 1.391(9) . ? C4G C5G 1.455(9) . ? C5G O2G 1.246(9) . ? C5G N1G 1.416(8) . ? C6G C7G 1.450(10) . ? C6G H6G 0.9500 . ? C7G C8G 1.359(10) . ? C7G H7G 0.9500 . ? C8G C9G 1.379(10) . ? C8G H8G 0.9500 . ? C9G C10G 1.416(10) . ? C10G C11G 1.276(10) . ? C10G H10G 0.9500 . ? C11G C12G 1.422(10) . ? C11G H11G 0.9500 . ? C12G H12G 0.9500 . ? C13G N1G 1.490(7) . ? C13G C14G 1.524(12) . ? C13G C16G 1.536(10) . ? C13G H13G 1.0000 . ? C14G C15G 1.482(13) . ? C14G H14O 0.9900 . ? C14G H14P 0.9900 . ? C15G O3G 1.192(11) . ? C15G N2G 1.309(13) . ? C16G O4G 1.232(8) . ? C16G O5G 1.278(8) . ? N2G H2G1 0.8800 . ? N2G H2G2 0.8800 . ? C1A O1A 1.191(11) . ? C1A N1A 1.387(11) . ? C1A C2A 1.505(12) . ? C2A C6A 1.349(13) . ? C2A C3A 1.360(13) . ? C3A C4A 1.392(13) . ? C3A C9A 1.413(13) . ? C4A C12A 1.393(13) . ? C4A C5A 1.426(12) . ? C5A O2A 1.272(13) . ? C5A N1A 1.398(12) . ? C6A C7A 1.461(14) . ? C6A H6A 0.9500 . ? C7A C8A 1.354(15) . ? C7A H7A 0.9500 . ? C8A C9A 1.379(14) . ? C8A H8A 0.9500 . ? C9A C10A 1.429(14) . ? C10A C11A 1.270(14) . ? C10A H10A 0.9500 . ? C11A C12A 1.420(14) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A N1A 1.464(10) . ? C13A C16A 1.493(10) . ? C13A C14A 1.534(9) . ? C13A H13A 1.0000 . ? C1Z O1Z 1.221(12) . ? C1Z N1Z 1.372(12) . ? C1Z C2Z 1.509(12) . ? C2Z C6Z 1.348(13) . ? C2Z C3Z 1.377(13) . ? C3Z C4Z 1.392(13) . ? C3Z C9Z 1.417(13) . ? C4Z C12Z 1.395(14) . ? C4Z C5Z 1.434(13) . ? C5Z O2Z 1.257(14) . ? C5Z N1Z 1.423(12) . ? C6Z C7Z 1.476(14) . ? C6Z H6Z 0.9500 . ? C7Z C8Z 1.350(15) . ? C7Z H7Z 0.9500 . ? C8Z C9Z 1.379(14) . ? C8Z H8Z 0.9500 . ? C9Z C10Z 1.425(14) . ? C10Z C11Z 1.272(15) . ? C10Z H10Z 0.9500 . ? C11Z C12Z 1.421(14) . ? C11Z H11Z 0.9500 . ? C12Z H12Z 0.9500 . ? C14A C15A 1.483(11) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A O3A 1.238(8) . ? C15A N2A 1.317(8) . ? N2A H2A1 0.8800 . ? N2A H2A2 0.8800 . ? O4A C16A 1.257(8) . ? O5A C16A 1.276(8) . ? C1B O1B 1.207(7) . ? C1B N1B 1.412(8) . ? C1B C2B 1.479(9) . ? C2B C6B 1.377(10) . ? C2B C3B 1.385(9) . ? C3B C4B 1.375(9) . ? C3B C9B 1.435(9) . ? C4B C12B 1.381(9) . ? C4B C5B 1.484(8) . ? C5B O2B 1.207(8) . ? C5B N1B 1.410(8) . ? C6B C7B 1.454(11) . ? C6B H6B 0.9500 . ? C7B C8B 1.345(11) . ? C7B H7B 0.9500 . ? C8B C9B 1.372(10) . ? C8B H8B 0.9500 . ? C9B C10B 1.408(10) . ? C10B C11B 1.253(10) . ? C10B H10B 0.9500 . ? C11B C12B 1.435(10) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B N1B 1.475(7) . ? C13B C14B 1.507(9) . ? C13B C16B 1.517(9) . ? C13B H13B 1.0000 . ? C14B C15B 1.487(10) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B O3B 1.253(9) . ? C15B N2B 1.337(10) . ? C16B O4B 1.250(7) . ? C16B O5B 1.260(7) . ? N2B H2B1 0.8800 . ? N2B H2B2 0.8800 . ? C1C O1C 1.182(9) . ? C1C N1C 1.401(10) . ? C1C C2C 1.483(10) . ? C2C C6C 1.379(11) . ? C2C C3C 1.391(10) . ? C3C C4C 1.356(10) . ? C3C C9C 1.445(10) . ? C4C C12C 1.399(11) . ? C4C C5C 1.496(10) . ? C5C O2C 1.200(9) . ? C5C N1C 1.426(10) . ? C6C C7C 1.443(11) . ? C6C H6C 0.9500 . ? C7C C8C 1.348(11) . ? C7C H7C 0.9500 . ? C8C C9C 1.363(11) . ? C8C H8C 0.9500 . ? C9C C10C 1.389(11) . ? C10C C11C 1.232(11) . ? C10C H10C 0.9500 . ? C11C C12C 1.428(11) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C N1C 1.499(10) . ? C13C C14C 1.507(14) . ? C13C C16C 1.526(13) . ? C13C H13C 1.0000 . ? C14C C15C 1.495(11) . ? C14C H14E 0.9900 . ? C14C H14F 0.9900 . ? C15C O3C 1.248(10) . ? C15C N2C 1.341(11) . ? C16C O5C 1.256(8) . ? C16C O4C 1.271(8) . ? N2C H2C1 0.8800 . ? N2C H2C2 0.8800 . ? C1D O1D 1.200(7) . ? C1D N1D 1.384(8) . ? C1D C2D 1.496(9) . ? C2D C6D 1.368(10) . ? C2D C3D 1.381(9) . ? C3D C4D 1.355(9) . ? C3D C9D 1.430(10) . ? C4D C12D 1.383(10) . ? C4D C5D 1.497(9) . ? C5D O2D 1.195(8) . ? C5D N1D 1.433(9) . ? C6D C7D 1.441(12) . ? C6D H6D 0.9500 . ? C7D C8D 1.355(12) . ? C7D H7D 0.9500 . ? C8D C9D 1.369(11) . ? C8D H8D 0.9500 . ? C9D C10D 1.395(10) . ? C10D C11D 1.254(11) . ? C10D H10D 0.9500 . ? C11D C12D 1.450(11) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D N1D 1.501(8) . ? C13D C14D 1.515(8) . ? C13D C16D 1.516(10) . ? C13D H13D 1.0000 . ? C14D C15D 1.472(10) . ? C14D H14G 0.9900 . ? C14D H14H 0.9900 . ? C15D O3D 1.246(9) . ? C15D N2D 1.318(11) . ? C16D O5D 1.244(8) . ? C16D O4D 1.265(8) . ? N2D H2D1 0.8800 . ? N2D H2D2 0.8800 . ? C1E O1E 1.192(6) . ? C1E N1E 1.405(7) . ? C1E C2E 1.478(7) . ? C2E C6E 1.369(8) . ? C2E C3E 1.422(8) . ? C3E C4E 1.395(8) . ? C3E C9E 1.430(8) . ? C4E C12E 1.375(8) . ? C4E C5E 1.480(7) . ? C5E O2E 1.212(7) . ? C5E N1E 1.423(7) . ? C6E C7E 1.427(9) . ? C6E H6E 0.9500 . ? C7E C8E 1.356(10) . ? C7E H7E 0.9500 . ? C8E C9E 1.414(9) . ? C8E H8E 0.9500 . ? C9E C10E 1.425(9) . ? C10E C11E 1.307(9) . ? C10E H10E 0.9500 . ? C11E C12E 1.406(9) . ? C11E H11E 0.9500 . ? C12E H12E 0.9500 . ? C13E N1E 1.467(7) . ? C13E C16E 1.519(8) . ? C13E C14E 1.521(9) . ? C13E H13E 1.0000 . ? C14E C15E 1.486(9) . ? C14E H14I 0.9900 . ? C14E H14J 0.9900 . ? C15E O3E 1.233(7) . ? C15E N2E 1.337(9) . ? C16E O4E 1.250(7) . ? C16E O5E 1.267(7) . ? N2E H2E1 0.8800 . ? N2E H2E2 0.8800 . ? C1F O1F 1.209(7) . ? C1F N1F 1.404(7) . ? C1F C2F 1.488(8) . ? C2F C6F 1.388(9) . ? C2F C3F 1.392(8) . ? C3F C4F 1.382(8) . ? C3F C9F 1.433(9) . ? C4F C12F 1.400(9) . ? C4F C5F 1.464(8) . ? C5F O2F 1.215(7) . ? C5F N1F 1.414(7) . ? C6F C7F 1.431(10) . ? C6F H6F 0.9500 . ? C7F C8F 1.340(10) . ? C7F H7F 0.9500 . ? C8F C9F 1.401(9) . ? C8F H8F 0.9500 . ? C9F C10F 1.402(9) . ? C10F C11F 1.293(10) . ? C10F H10F 0.9500 . ? C11F C12F 1.409(10) . ? C11F H11F 0.9500 . ? C12F H12F 0.9500 . ? C13F N1F 1.464(7) . ? C13F C14F 1.517(8) . ? C13F C16F 1.534(9) . ? C13F H13F 1.0000 . ? C14F C15F 1.523(8) . ? C14F H14K 0.9900 . ? C14F H14L 0.9900 . ? C15F O3F 1.217(8) . ? C15F N2F 1.345(9) . ? C16F O4F 1.253(7) . ? C16F O5F 1.268(7) . ? N2F H2F1 0.8800 . ? N2F H2F2 0.8800 . ? C1H O1H 1.190(7) . ? C1H N1H 1.390(7) . ? C1H C2H 1.505(8) . ? C2H C6H 1.365(8) . ? C2H C3H 1.389(8) . ? C3H C4H 1.387(9) . ? C3H C9H 1.428(9) . ? C4H C12H 1.375(10) . ? C4H C5H 1.477(8) . ? C5H O2H 1.215(8) . ? C5H N1H 1.426(8) . ? C6H C7H 1.421(10) . ? C6H H6H 0.9500 . ? C7H C8H 1.345(10) . ? C7H H7H 0.9500 . ? C8H C9H 1.369(10) . ? C8H H8H 0.9500 . ? C9H C10H 1.408(10) . ? C10H C11H 1.282(10) . ? C10H H10H 0.9500 . ? C11H C12H 1.431(10) . ? C11H H11H 0.9500 . ? C12H H12H 0.9500 . ? C13H C16H 1.476(9) . ? C13H N1H 1.493(7) . ? C13H C14H 1.504(9) . ? C13H H13H 1.0000 . ? C14H C15H 1.450(9) . ? C14H H14M 0.9900 . ? C14H H14N 0.9900 . ? C15H O3H 1.258(10) . ? C15H N2H 1.321(10) . ? N2H H2H1 0.8800 . ? N2H H2H2 0.8800 . ? C16H O5H 1.244(8) . ? C16H O4H 1.307(8) . ? N3I C21I 1.3900 . ? N3I C25I 1.3900 . ? C21I C22I 1.3900 . ? C21I H21I 0.9500 . ? C22I C23I 1.3900 . ? C22I H22I 0.9500 . ? C23I C24I 1.3900 . ? C23I H23I 0.9500 . ? C24I C25I 1.3900 . ? C24I H24I 0.9500 . ? C25I H25I 0.9500 . ? N3J C21J 1.3900 . ? N3J C25J 1.3900 . ? C21J C22J 1.3900 . ? C21J H21J 0.9500 . ? C22J C23J 1.3900 . ? C22J H22J 0.9500 . ? C23J C24J 1.3900 . ? C23J H23J 0.9500 . ? C24J C25J 1.3900 . ? C24J H24J 0.9500 . ? C25J H25J 0.9500 . ? O36 C31 1.1832 . ? O37 C31 1.4303 . ? O37 C32 1.5539 . ? O38 C34 1.4183 . ? C31 C34 1.2754 . ? C32 C33 1.6816 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.6195 . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O46 C41 1.237(13) . ? O47 C41 1.347(13) . ? O47 C42 1.506(10) . ? O48 C44 1.404(9) . ? C41 C44 1.435(12) . ? C42 C43 1.4344 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.5017 . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4C Cu1 O4A 175.1(2) . . ? O4C Cu1 O4B 89.39(18) . . ? O4A Cu1 O4B 90.82(19) . . ? O4C Cu1 O4D 89.47(19) . . ? O4A Cu1 O4D 88.58(19) . . ? O4B Cu1 O4D 159.09(18) . . ? O4C Cu1 N3J 88.7(2) . . ? O4A Cu1 N3J 96.2(2) . . ? O4B Cu1 N3J 96.1(2) . . ? O4D Cu1 N3J 104.7(2) . . ? O4C Cu1 N3I 94.0(3) . . ? O4A Cu1 N3I 90.9(3) . . ? O4B Cu1 N3I 95.2(3) . . ? O4D Cu1 N3I 105.7(3) . . ? N3J Cu1 N3I 5.4(3) . . ? O4C Cu1 Cu2 86.57(13) . . ? O4A Cu1 Cu2 88.62(14) . . ? O4B Cu1 Cu2 80.89(12) . . ? O4D Cu1 Cu2 78.20(13) . . ? N3J Cu1 Cu2 174.39(18) . . ? N3I Cu1 Cu2 176.0(3) . . ? O5B Cu2 O5D 176.26(19) . . ? O5B Cu2 O5C 91.11(19) . . ? O5D Cu2 O5C 87.99(19) . . ? O5B Cu2 O5A 89.24(19) . . ? O5D Cu2 O5A 90.43(19) . . ? O5C Cu2 O5A 161.21(18) . . ? O5B Cu2 O3E 88.55(17) . . ? O5D Cu2 O3E 95.19(18) . . ? O5C Cu2 O3E 105.91(18) . . ? O5A Cu2 O3E 92.88(17) . . ? O5B Cu2 Cu1 86.68(13) . . ? O5D Cu2 Cu1 89.59(14) . . ? O5C Cu2 Cu1 81.65(14) . . ? O5A Cu2 Cu1 79.61(12) . . ? O3E Cu2 Cu1 171.15(12) . . ? O4H Cu3 O4F 168.79(18) . . ? O4H Cu3 O4G 88.13(19) . . ? O4F Cu3 O4G 94.57(18) . . ? O4H Cu3 O4E 86.78(18) . . ? O4F Cu3 O4E 89.29(17) . . ? O4G Cu3 O4E 172.02(18) . . ? O4H Cu3 O36 102.48(17) . . ? O4F Cu3 O36 88.01(17) . . ? O4G Cu3 O36 96.86(17) . . ? O4E Cu3 O36 90.24(17) . . ? O4H Cu3 Cu4 88.08(13) . . ? O4F Cu3 Cu4 81.48(12) . . ? O4G Cu3 Cu4 82.92(13) . . ? O4E Cu3 Cu4 90.77(12) . . ? O36 Cu3 Cu4 169.43(12) . . ? O5F Cu4 O5G 92.52(17) . . ? O5F Cu4 O5H 169.04(17) . . ? O5G Cu4 O5H 87.82(17) . . ? O5F Cu4 O5E 86.32(16) . . ? O5G Cu4 O5E 164.69(17) . . ? O5H Cu4 O5E 90.47(17) . . ? O5F Cu4 O3A 96.98(17) . . ? O5G Cu4 O3A 102.26(18) . . ? O5H Cu4 O3A 93.64(19) . . ? O5E Cu4 O3A 93.02(18) . . ? O5F Cu4 Cu3 87.52(11) . . ? O5G Cu4 Cu3 86.19(12) . . ? O5H Cu4 Cu3 81.58(13) . . ? O5E Cu4 Cu3 78.51(11) . . ? O3A Cu4 Cu3 170.18(14) . . ? O1G C1G N1G 120.7(5) . . ? O1G C1G C2G 123.5(6) . . ? N1G C1G C2G 115.7(5) . . ? C6G C2G C3G 119.7(6) . . ? C6G C2G C1G 118.6(6) . . ? C3G C2G C1G 121.7(6) . . ? C2G C3G C4G 120.6(6) . . ? C2G C3G C9G 120.3(6) . . ? C4G C3G C9G 119.1(6) . . ? C12G C4G C3G 119.8(7) . . ? C12G C4G C5G 120.1(7) . . ? C3G C4G C5G 120.1(7) . . ? O2G C5G N1G 116.6(7) . . ? O2G C5G C4G 125.8(7) . . ? N1G C5G C4G 117.6(6) . . ? C2G C6G C7G 121.7(8) . . ? C2G C6G H6G 119.1 . . ? C7G C6G H6G 119.1 . . ? C8G C7G C6G 116.8(9) . . ? C8G C7G H7G 121.6 . . ? C6G C7G H7G 121.6 . . ? C7G C8G C9G 122.8(9) . . ? C7G C8G H8G 118.6 . . ? C9G C8G H8G 118.6 . . ? C8G C9G C10G 123.2(8) . . ? C8G C9G C3G 118.5(7) . . ? C10G C9G C3G 118.1(7) . . ? C11G C10G C9G 122.3(9) . . ? C11G C10G H10G 118.9 . . ? C9G C10G H10G 118.9 . . ? C10G C11G C12G 121.9(9) . . ? C10G C11G H11G 119.1 . . ? C12G C11G H11G 119.1 . . ? C4G C12G C11G 118.8(8) . . ? C4G C12G H12G 120.6 . . ? C11G C12G H12G 120.6 . . ? N1G C13G C14G 109.2(6) . . ? N1G C13G C16G 111.6(6) . . ? C14G C13G C16G 114.5(6) . . ? N1G C13G H13G 107.0 . . ? C14G C13G H13G 107.0 . . ? C16G C13G H13G 107.0 . . ? C1G N1G C5G 124.0(6) . . ? C1G N1G C13G 116.9(5) . . ? C5G N1G C13G 118.7(6) . . ? C15G C14G C13G 113.3(8) . . ? C15G C14G H14O 108.9 . . ? C13G C14G H14O 108.9 . . ? C15G C14G H14P 108.9 . . ? C13G C14G H14P 108.9 . . ? H14O C14G H14P 107.7 . . ? O3G C15G N2G 122.0(10) . . ? O3G C15G C14G 124.1(9) . . ? N2G C15G C14G 113.9(10) . . ? O4G C16G O5G 127.9(6) . . ? O4G C16G C13G 116.2(6) . . ? O5G C16G C13G 115.6(5) . . ? C15G N2G H2G1 120.0 . . ? C15G N2G H2G2 120.0 . . ? H2G1 N2G H2G2 120.0 . . ? C16G O4G Cu3 123.0(4) . . ? C16G O5G Cu4 117.9(4) . . ? O1A C1A N1A 126.4(10) . . ? O1A C1A C2A 120.6(10) . . ? N1A C1A C2A 112.2(9) . . ? C6A C2A C3A 118.7(11) . . ? C6A C2A C1A 116.6(11) . . ? C3A C2A C1A 123.1(11) . . ? C2A C3A C4A 119.5(11) . . ? C2A C3A C9A 122.7(11) . . ? C4A C3A C9A 117.9(11) . . ? C3A C4A C12A 122.6(11) . . ? C3A C4A C5A 120.4(11) . . ? C12A C4A C5A 116.9(11) . . ? O2A C5A N1A 115.3(10) . . ? O2A C5A C4A 126.5(11) . . ? N1A C5A C4A 118.1(10) . . ? C2A C6A C7A 120.1(12) . . ? C2A C6A H6A 119.9 . . ? C7A C6A H6A 119.9 . . ? C8A C7A C6A 117.8(15) . . ? C8A C7A H7A 121.1 . . ? C6A C7A H7A 121.1 . . ? C7A C8A C9A 122.1(14) . . ? C7A C8A H8A 119.0 . . ? C9A C8A H8A 119.0 . . ? C8A C9A C3A 117.3(12) . . ? C8A C9A C10A 125.6(13) . . ? C3A C9A C10A 117.1(12) . . ? C11A C10A C9A 124.0(15) . . ? C11A C10A H10A 118.0 . . ? C9A C10A H10A 118.0 . . ? C10A C11A C12A 121.2(16) . . ? C10A C11A H11A 119.4 . . ? C12A C11A H11A 119.4 . . ? C4A C12A C11A 117.0(13) . . ? C4A C12A H12A 121.5 . . ? C11A C12A H12A 121.5 . . ? N1A C13A C16A 113.1(8) . . ? N1A C13A C14A 116.7(8) . . ? C16A C13A C14A 113.7(6) . . ? N1A C13A H13A 103.8 . . ? C16A C13A H13A 103.8 . . ? C14A C13A H13A 103.8 . . ? C1A N1A C5A 125.2(9) . . ? C1A N1A C13A 111.3(8) . . ? C5A N1A C13A 123.4(9) . . ? O1Z C1Z N1Z 124.6(12) . . ? O1Z C1Z C2Z 122.1(12) . . ? N1Z C1Z C2Z 113.0(11) . . ? C6Z C2Z C3Z 119.4(12) . . ? C6Z C2Z C1Z 117.9(12) . . ? C3Z C2Z C1Z 122.6(12) . . ? C2Z C3Z C4Z 121.3(12) . . ? C2Z C3Z C9Z 121.6(12) . . ? C4Z C3Z C9Z 117.1(11) . . ? C3Z C4Z C12Z 122.3(13) . . ? C3Z C4Z C5Z 118.4(12) . . ? C12Z C4Z C5Z 117.8(13) . . ? O2Z C5Z N1Z 117.1(13) . . ? O2Z C5Z C4Z 123.5(14) . . ? N1Z C5Z C4Z 119.3(12) . . ? C2Z C6Z C7Z 120.8(14) . . ? C2Z C6Z H6Z 119.6 . . ? C7Z C6Z H6Z 119.6 . . ? C8Z C7Z C6Z 115.6(15) . . ? C8Z C7Z H7Z 122.2 . . ? C6Z C7Z H7Z 122.2 . . ? C7Z C8Z C9Z 123.0(16) . . ? C7Z C8Z H8Z 118.5 . . ? C9Z C8Z H8Z 118.5 . . ? C8Z C9Z C3Z 116.5(13) . . ? C8Z C9Z C10Z 123.0(14) . . ? C3Z C9Z C10Z 117.8(13) . . ? C11Z C10Z C9Z 123.4(16) . . ? C11Z C10Z H10Z 118.3 . . ? C9Z C10Z H10Z 118.3 . . ? C10Z C11Z C12Z 121.3(16) . . ? C10Z C11Z H11Z 119.4 . . ? C12Z C11Z H11Z 119.4 . . ? C4Z C12Z C11Z 117.1(14) . . ? C4Z C12Z H12Z 121.5 . . ? C11Z C12Z H12Z 121.5 . . ? C1Z N1Z C5Z 125.0(10) . . ? C15A C14A C13A 116.5(7) . . ? C15A C14A H14A 108.2 . . ? C13A C14A H14A 108.2 . . ? C15A C14A H14B 108.2 . . ? C13A C14A H14B 108.2 . . ? H14A C14A H14B 107.3 . . ? O3A C15A N2A 123.3(7) . . ? O3A C15A C14A 119.0(7) . . ? N2A C15A C14A 117.4(7) . . ? C15A N2A H2A1 120.0 . . ? C15A N2A H2A2 120.0 . . ? H2A1 N2A H2A2 120.0 . . ? C15A O3A Cu4 127.1(5) . . ? C16A O4A Cu1 118.2(4) . . ? C16A O5A Cu2 126.2(4) . . ? O4A C16A O5A 126.7(6) . . ? O4A C16A C13A 120.6(6) . . ? O5A C16A C13A 112.7(6) . . ? O1B C1B N1B 119.2(6) . . ? O1B C1B C2B 125.3(6) . . ? N1B C1B C2B 115.4(6) . . ? C6B C2B C3B 121.2(7) . . ? C6B C2B C1B 116.8(7) . . ? C3B C2B C1B 122.0(6) . . ? C4B C3B C2B 120.3(6) . . ? C4B C3B C9B 118.6(6) . . ? C2B C3B C9B 121.1(6) . . ? C3B C4B C12B 120.8(7) . . ? C3B C4B C5B 121.4(6) . . ? C12B C4B C5B 117.4(6) . . ? O2B C5B N1B 120.0(6) . . ? O2B C5B C4B 123.8(7) . . ? N1B C5B C4B 116.1(6) . . ? C2B C6B C7B 117.4(8) . . ? C2B C6B H6B 121.3 . . ? C7B C6B H6B 121.3 . . ? C8B C7B C6B 119.9(9) . . ? C8B C7B H7B 120.0 . . ? C6B C7B H7B 120.0 . . ? C7B C8B C9B 124.0(10) . . ? C7B C8B H8B 118.0 . . ? C9B C8B H8B 118.0 . . ? C8B C9B C10B 126.1(8) . . ? C8B C9B C3B 116.4(8) . . ? C10B C9B C3B 117.5(7) . . ? C11B C10B C9B 123.5(9) . . ? C11B C10B H10B 118.3 . . ? C9B C10B H10B 118.3 . . ? C10B C11B C12B 121.1(9) . . ? C10B C11B H11B 119.5 . . ? C12B C11B H11B 119.5 . . ? C4B C12B C11B 118.5(7) . . ? C4B C12B H12B 120.8 . . ? C11B C12B H12B 120.8 . . ? N1B C13B C14B 112.2(5) . . ? N1B C13B C16B 110.2(5) . . ? C14B C13B C16B 113.6(5) . . ? N1B C13B H13B 106.8 . . ? C14B C13B H13B 106.8 . . ? C16B C13B H13B 106.8 . . ? C5B N1B C1B 124.4(5) . . ? C5B N1B C13B 118.6(5) . . ? C1B N1B C13B 116.9(5) . . ? C15B C14B C13B 111.7(6) . . ? C15B C14B H14C 109.3 . . ? C13B C14B H14C 109.3 . . ? C15B C14B H14D 109.3 . . ? C13B C14B H14D 109.3 . . ? H14C C14B H14D 107.9 . . ? O3B C15B N2B 119.9(7) . . ? O3B C15B C14B 121.6(6) . . ? N2B C15B C14B 118.5(6) . . ? O4B C16B O5B 126.7(6) . . ? O4B C16B C13B 118.0(5) . . ? O5B C16B C13B 115.2(5) . . ? C15B N2B H2B1 120.0 . . ? C15B N2B H2B2 120.0 . . ? H2B1 N2B H2B2 120.0 . . ? C16B O4B Cu1 123.8(4) . . ? C16B O5B Cu2 121.9(4) . . ? O1C C1C N1C 121.6(8) . . ? O1C C1C C2C 124.9(8) . . ? N1C C1C C2C 113.3(8) . . ? C6C C2C C3C 120.6(8) . . ? C6C C2C C1C 117.2(8) . . ? C3C C2C C1C 122.2(8) . . ? C4C C3C C2C 121.8(8) . . ? C4C C3C C9C 118.6(8) . . ? C2C C3C C9C 119.6(8) . . ? C3C C4C C12C 123.3(9) . . ? C3C C4C C5C 121.0(8) . . ? C12C C4C C5C 115.5(8) . . ? O2C C5C N1C 119.3(8) . . ? O2C C5C C4C 126.8(9) . . ? N1C C5C C4C 114.0(8) . . ? C2C C6C C7C 120.5(9) . . ? C2C C6C H6C 119.8 . . ? C7C C6C H6C 119.8 . . ? C8C C7C C6C 116.1(10) . . ? C8C C7C H7C 122.0 . . ? C6C C7C H7C 122.0 . . ? C7C C8C C9C 126.7(10) . . ? C7C C8C H8C 116.7 . . ? C9C C8C H8C 116.7 . . ? C8C C9C C10C 129.4(9) . . ? C8C C9C C3C 116.3(9) . . ? C10C C9C C3C 114.2(8) . . ? C11C C10C C9C 127.7(11) . . ? C11C C10C H10C 116.2 . . ? C9C C10C H10C 116.2 . . ? C10C C11C C12C 120.9(10) . . ? C10C C11C H11C 119.5 . . ? C12C C11C H11C 119.5 . . ? C4C C12C C11C 115.2(9) . . ? C4C C12C H12C 122.4 . . ? C11C C12C H12C 122.4 . . ? N1C C13C C14C 115.0(9) . . ? N1C C13C C16C 109.4(8) . . ? C14C C13C C16C 111.5(8) . . ? N1C C13C H13C 106.8 . . ? C14C C13C H13C 106.8 . . ? C16C C13C H13C 106.8 . . ? C1C N1C C5C 127.4(8) . . ? C1C N1C C13C 114.9(8) . . ? C5C N1C C13C 117.4(8) . . ? C15C C14C C13C 114.5(8) . . ? C15C C14C H14E 108.6 . . ? C13C C14C H14E 108.6 . . ? C15C C14C H14F 108.6 . . ? C13C C14C H14F 108.6 . . ? H14E C14C H14F 107.6 . . ? O3C C15C N2C 122.7(8) . . ? O3C C15C C14C 121.2(8) . . ? N2C C15C C14C 115.8(7) . . ? O5C C16C O4C 127.6(6) . . ? O5C C16C C13C 115.0(7) . . ? O4C C16C C13C 117.3(7) . . ? C15C N2C H2C1 120.0 . . ? C15C N2C H2C2 120.0 . . ? H2C1 N2C H2C2 120.0 . . ? C16C O4C Cu1 120.2(4) . . ? C16C O5C Cu2 123.3(4) . . ? O1D C1D N1D 119.6(6) . . ? O1D C1D C2D 124.5(7) . . ? N1D C1D C2D 116.0(6) . . ? C6D C2D C3D 122.3(8) . . ? C6D C2D C1D 116.7(8) . . ? C3D C2D C1D 121.0(7) . . ? C4D C3D C2D 121.0(7) . . ? C4D C3D C9D 120.3(7) . . ? C2D C3D C9D 118.4(7) . . ? C3D C4D C12D 120.7(8) . . ? C3D C4D C5D 122.5(7) . . ? C12D C4D C5D 116.7(7) . . ? O2D C5D N1D 119.7(7) . . ? O2D C5D C4D 126.2(7) . . ? N1D C5D C4D 114.0(6) . . ? C2D C6D C7D 119.4(10) . . ? C2D C6D H6D 120.3 . . ? C7D C6D H6D 120.3 . . ? C8D C7D C6D 117.2(11) . . ? C8D C7D H7D 121.4 . . ? C6D C7D H7D 121.4 . . ? C7D C8D C9D 124.7(11) . . ? C7D C8D H8D 117.7 . . ? C9D C8D H8D 117.7 . . ? C8D C9D C10D 125.4(9) . . ? C8D C9D C3D 117.9(9) . . ? C10D C9D C3D 116.7(8) . . ? C11D C10D C9D 123.4(10) . . ? C11D C10D H10D 118.3 . . ? C9D C10D H10D 118.3 . . ? C10D C11D C12D 121.5(10) . . ? C10D C11D H11D 119.2 . . ? C12D C11D H11D 119.2 . . ? C4D C12D C11D 117.0(9) . . ? C4D C12D H12D 121.5 . . ? C11D C12D H12D 121.5 . . ? N1D C13D C14D 107.0(6) . . ? N1D C13D C16D 111.7(6) . . ? C14D C13D C16D 115.6(6) . . ? N1D C13D H13D 107.4 . . ? C14D C13D H13D 107.4 . . ? C16D C13D H13D 107.4 . . ? C1D N1D C5D 125.2(6) . . ? C1D N1D C13D 116.9(6) . . ? C5D N1D C13D 117.5(6) . . ? C15D C14D C13D 118.8(7) . . ? C15D C14D H14G 107.6 . . ? C13D C14D H14G 107.6 . . ? C15D C14D H14H 107.6 . . ? C13D C14D H14H 107.6 . . ? H14G C14D H14H 107.0 . . ? O3D C15D N2D 120.3(9) . . ? O3D C15D C14D 123.5(8) . . ? N2D C15D C14D 115.1(9) . . ? O5D C16D O4D 127.0(6) . . ? O5D C16D C13D 117.2(6) . . ? O4D C16D C13D 115.8(6) . . ? C15D N2D H2D1 120.0 . . ? C15D N2D H2D2 120.0 . . ? H2D1 N2D H2D2 120.0 . . ? C16D O4D Cu1 127.2(4) . . ? C16D O5D Cu2 118.0(4) . . ? O1E C1E N1E 120.1(5) . . ? O1E C1E C2E 123.9(5) . . ? N1E C1E C2E 116.1(5) . . ? C6E C2E C3E 122.2(6) . . ? C6E C2E C1E 117.8(5) . . ? C3E C2E C1E 120.1(5) . . ? C4E C3E C2E 122.2(5) . . ? C4E C3E C9E 119.1(5) . . ? C2E C3E C9E 118.6(5) . . ? C12E C4E C3E 120.5(6) . . ? C12E C4E C5E 120.0(5) . . ? C3E C4E C5E 119.4(5) . . ? O2E C5E N1E 119.4(5) . . ? O2E C5E C4E 123.8(5) . . ? N1E C5E C4E 116.8(5) . . ? C2E C6E C7E 118.0(7) . . ? C2E C6E H6E 121.0 . . ? C7E C6E H6E 121.0 . . ? C8E C7E C6E 121.6(7) . . ? C8E C7E H7E 119.2 . . ? C6E C7E H7E 119.2 . . ? C7E C8E C9E 121.2(7) . . ? C7E C8E H8E 119.4 . . ? C9E C8E H8E 119.4 . . ? C8E C9E C10E 124.2(6) . . ? C8E C9E C3E 118.3(6) . . ? C10E C9E C3E 117.5(6) . . ? C11E C10E C9E 121.8(7) . . ? C11E C10E H10E 119.1 . . ? C9E C10E H10E 119.1 . . ? C10E C11E C12E 121.3(8) . . ? C10E C11E H11E 119.3 . . ? C12E C11E H11E 119.3 . . ? C4E C12E C11E 119.6(7) . . ? C4E C12E H12E 120.2 . . ? C11E C12E H12E 120.2 . . ? N1E C13E C16E 111.5(5) . . ? N1E C13E C14E 109.9(5) . . ? C16E C13E C14E 114.7(5) . . ? N1E C13E H13E 106.7 . . ? C16E C13E H13E 106.7 . . ? C14E C13E H13E 106.7 . . ? C1E N1E C5E 125.3(4) . . ? C1E N1E C13E 117.2(4) . . ? C5E N1E C13E 117.3(4) . . ? C15E C14E C13E 121.7(6) . . ? C15E C14E H14I 106.9 . . ? C13E C14E H14I 106.9 . . ? C15E C14E H14J 106.9 . . ? C13E C14E H14J 106.9 . . ? H14I C14E H14J 106.7 . . ? O3E C15E N2E 120.4(6) . . ? O3E C15E C14E 118.2(6) . . ? N2E C15E C14E 121.4(6) . . ? O4E C16E O5E 126.9(5) . . ? O4E C16E C13E 117.3(5) . . ? O5E C16E C13E 115.8(5) . . ? C15E N2E H2E1 120.0 . . ? C15E N2E H2E2 120.0 . . ? H2E1 N2E H2E2 120.0 . . ? C15E O3E Cu2 132.3(4) . . ? C16E O4E Cu3 115.5(4) . . ? C16E O5E Cu4 128.2(4) . . ? O1F C1F N1F 119.3(5) . . ? O1F C1F C2F 124.7(6) . . ? N1F C1F C2F 116.0(5) . . ? C6F C2F C3F 120.9(6) . . ? C6F C2F C1F 117.8(6) . . ? C3F C2F C1F 121.2(6) . . ? C4F C3F C2F 120.6(6) . . ? C4F C3F C9F 118.9(6) . . ? C2F C3F C9F 120.5(6) . . ? C3F C4F C12F 120.6(6) . . ? C3F C4F C5F 121.2(5) . . ? C12F C4F C5F 118.2(6) . . ? O2F C5F N1F 118.5(5) . . ? O2F C5F C4F 124.3(5) . . ? N1F C5F C4F 117.1(5) . . ? C2F C6F C7F 118.4(8) . . ? C2F C6F H6F 120.8 . . ? C7F C6F H6F 120.8 . . ? C8F C7F C6F 119.9(9) . . ? C8F C7F H7F 120.0 . . ? C6F C7F H7F 120.0 . . ? C7F C8F C9F 123.8(8) . . ? C7F C8F H8F 118.1 . . ? C9F C8F H8F 118.1 . . ? C8F C9F C10F 125.9(7) . . ? C8F C9F C3F 116.3(6) . . ? C10F C9F C3F 117.7(7) . . ? C11F C10F C9F 122.9(8) . . ? C11F C10F H10F 118.5 . . ? C9F C10F H10F 118.5 . . ? C10F C11F C12F 121.2(8) . . ? C10F C11F H11F 119.4 . . ? C12F C11F H11F 119.4 . . ? C4F C12F C11F 118.6(7) . . ? C4F C12F H12F 120.7 . . ? C11F C12F H12F 120.7 . . ? N1F C13F C14F 111.1(5) . . ? N1F C13F C16F 111.0(5) . . ? C14F C13F C16F 115.2(5) . . ? N1F C13F H13F 106.3 . . ? C14F C13F H13F 106.3 . . ? C16F C13F H13F 106.3 . . ? C1F N1F C5F 123.8(5) . . ? C1F N1F C13F 117.2(5) . . ? C5F N1F C13F 118.6(5) . . ? C13F C14F C15F 112.0(5) . . ? C13F C14F H14K 109.2 . . ? C15F C14F H14K 109.2 . . ? C13F C14F H14L 109.2 . . ? C15F C14F H14L 109.2 . . ? H14K C14F H14L 107.9 . . ? O3F C15F N2F 123.8(6) . . ? O3F C15F C14F 120.9(5) . . ? N2F C15F C14F 115.1(6) . . ? O4F C16F O5F 126.2(6) . . ? O4F C16F C13F 117.0(5) . . ? O5F C16F C13F 116.4(5) . . ? C15F N2F H2F1 120.0 . . ? C15F N2F H2F2 120.0 . . ? H2F1 N2F H2F2 120.0 . . ? C16F O4F Cu3 125.7(4) . . ? C16F O5F Cu4 118.7(4) . . ? O1H C1H N1H 120.9(5) . . ? O1H C1H C2H 122.1(5) . . ? N1H C1H C2H 117.0(5) . . ? C6H C2H C3H 121.3(6) . . ? C6H C2H C1H 119.2(6) . . ? C3H C2H C1H 119.5(6) . . ? C4H C3H C2H 121.8(6) . . ? C4H C3H C9H 119.6(6) . . ? C2H C3H C9H 118.5(6) . . ? C12H C4H C3H 120.6(7) . . ? C12H C4H C5H 118.4(6) . . ? C3H C4H C5H 121.1(6) . . ? O2H C5H N1H 118.0(6) . . ? O2H C5H C4H 125.9(6) . . ? N1H C5H C4H 115.9(5) . . ? C2H C6H C7H 121.5(7) . . ? C2H C6H H6H 119.3 . . ? C7H C6H H6H 119.3 . . ? C8H C7H C6H 114.9(8) . . ? C8H C7H H7H 122.6 . . ? C6H C7H H7H 122.6 . . ? C7H C8H C9H 127.4(9) . . ? C7H C8H H8H 116.3 . . ? C9H C8H H8H 116.3 . . ? C8H C9H C10H 126.1(8) . . ? C8H C9H C3H 116.4(7) . . ? C10H C9H C3H 117.5(8) . . ? C11H C10H C9H 122.1(9) . . ? C11H C10H H10H 119.0 . . ? C9H C10H H10H 119.0 . . ? C10H C11H C12H 122.2(9) . . ? C10H C11H H11H 118.9 . . ? C12H C11H H11H 118.9 . . ? C4H C12H C11H 118.0(8) . . ? C4H C12H H12H 121.0 . . ? C11H C12H H12H 121.0 . . ? C16H C13H N1H 112.5(5) . . ? C16H C13H C14H 115.7(6) . . ? N1H C13H C14H 112.2(5) . . ? C16H C13H H13H 105.1 . . ? N1H C13H H13H 105.1 . . ? C14H C13H H13H 105.1 . . ? C1H N1H C5H 124.2(5) . . ? C1H N1H C13H 117.0(5) . . ? C5H N1H C13H 118.4(5) . . ? C15H C14H C13H 115.9(6) . . ? C15H C14H H14M 108.3 . . ? C13H C14H H14M 108.3 . . ? C15H C14H H14N 108.3 . . ? C13H C14H H14N 108.3 . . ? H14M C14H H14N 107.4 . . ? O3H C15H N2H 120.8(8) . . ? O3H C15H C14H 120.8(8) . . ? N2H C15H C14H 118.2(8) . . ? C15H N2H H2H1 120.0 . . ? C15H N2H H2H2 120.0 . . ? H2H1 N2H H2H2 120.0 . . ? O5H C16H O4H 126.1(6) . . ? O5H C16H C13H 119.6(6) . . ? O4H C16H C13H 114.1(5) . . ? C16H O4H Cu3 118.4(4) . . ? C16H O5H Cu4 125.4(4) . . ? C21I N3I C25I 120.0 . . ? C21I N3I Cu1 117.2(5) . . ? C25I N3I Cu1 122.8(5) . . ? C22I C21I N3I 120.0 . . ? C22I C21I H21I 120.0 . . ? N3I C21I H21I 120.0 . . ? C21I C22I C23I 120.0 . . ? C21I C22I H22I 120.0 . . ? C23I C22I H22I 120.0 . . ? C22I C23I C24I 120.0 . . ? C22I C23I H23I 120.0 . . ? C24I C23I H23I 120.0 . . ? C25I C24I C23I 120.0 . . ? C25I C24I H24I 120.0 . . ? C23I C24I H24I 120.0 . . ? C24I C25I N3I 120.0 . . ? C24I C25I H25I 120.0 . . ? N3I C25I H25I 120.0 . . ? C21J N3J C25J 120.0 . . ? C21J N3J Cu1 121.42(15) . . ? C25J N3J Cu1 117.96(16) . . ? N3J C21J C22J 120.0 . . ? N3J C21J H21J 120.0 . . ? C22J C21J H21J 120.0 . . ? C21J C22J C23J 120.0 . . ? C21J C22J H22J 120.0 . . ? C23J C22J H22J 120.0 . . ? C24J C23J C22J 120.0 . . ? C24J C23J H23J 120.0 . . ? C22J C23J H23J 120.0 . . ? C23J C24J C25J 120.0 . . ? C23J C24J H24J 120.0 . . ? C25J C24J H24J 120.0 . . ? C24J C25J N3J 120.0 . . ? C24J C25J H25J 120.0 . . ? N3J C25J H25J 120.0 . . ? C31 O36 Cu3 121.99(12) . . ? C31 O37 C32 119.8 . . ? O36 C31 C34 121.8 . . ? O36 C31 O37 124.1 . . ? C34 C31 O37 113.6 . . ? O37 C32 C33 115.4 . . ? O37 C32 H32A 108.4 . . ? C33 C32 H32A 108.4 . . ? O37 C32 H32B 108.4 . . ? C33 C32 H32B 108.4 . . ? H32A C32 H32B 107.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 O38 118.4 . . ? C31 C34 C35 115.8 . . ? O38 C34 C35 109.2 . . ? C31 C34 H34 103.8 . . ? O38 C34 H34 103.8 . . ? C35 C34 H34 103.8 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 O47 C42 119.3(8) . . ? O46 C41 O47 122.1(10) . . ? O46 C41 C44 123.7(10) . . ? O47 C41 C44 114.1(9) . . ? C43 C42 O47 108.5(4) . . ? C43 C42 H42A 110.0 . . ? O47 C42 H42A 110.0 . . ? C43 C42 H42B 110.0 . . ? O47 C42 H42B 110.0 . . ? H42A C42 H42B 108.4 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O48 C44 C41 118.3(7) . . ? O48 C44 C45 107.4(4) . . ? C41 C44 C45 112.2(5) . . ? O48 C44 H44 106.0 . . ? C41 C44 H44 106.0 . . ? C45 C44 H44 106.0 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4C Cu1 Cu2 O5B -89.56(19) . . . . ? O4A Cu1 Cu2 O5B 91.43(19) . . . . ? O4B Cu1 Cu2 O5B 0.38(18) . . . . ? O4D Cu1 Cu2 O5B -179.73(19) . . . . ? O4C Cu1 Cu2 O5D 90.09(19) . . . . ? O4A Cu1 Cu2 O5D -88.92(19) . . . . ? O4B Cu1 Cu2 O5D -179.98(18) . . . . ? O4D Cu1 Cu2 O5D -0.09(19) . . . . ? O4C Cu1 Cu2 O5C 2.06(19) . . . . ? O4A Cu1 Cu2 O5C -177.0(2) . . . . ? O4B Cu1 Cu2 O5C 91.99(18) . . . . ? O4D Cu1 Cu2 O5C -88.12(19) . . . . ? O4C Cu1 Cu2 O5A -179.39(19) . . . . ? O4A Cu1 Cu2 O5A 1.59(19) . . . . ? O4B Cu1 Cu2 O5A -89.46(18) . . . . ? O4D Cu1 Cu2 O5A 90.43(19) . . . . ? O4H Cu3 Cu4 O5F 175.06(17) . . . . ? O4F Cu3 Cu4 O5F -0.86(17) . . . . ? O4G Cu3 Cu4 O5F -96.59(17) . . . . ? O4E Cu3 Cu4 O5F 88.31(17) . . . . ? O36 Cu3 Cu4 O5F -7.1(7) . . . . ? O4H Cu3 Cu4 O5G -92.25(18) . . . . ? O4F Cu3 Cu4 O5G 91.83(17) . . . . ? O4G Cu3 Cu4 O5G -3.90(18) . . . . ? O4E Cu3 Cu4 O5G -179.00(18) . . . . ? O36 Cu3 Cu4 O5G 85.6(7) . . . . ? O4H Cu3 Cu4 O5H -3.89(18) . . . . ? O4F Cu3 Cu4 O5H -179.81(18) . . . . ? O4G Cu3 Cu4 O5H 84.46(18) . . . . ? O4E Cu3 Cu4 O5H -90.64(17) . . . . ? O36 Cu3 Cu4 O5H 173.9(7) . . . . ? O4H Cu3 Cu4 O5E 88.31(17) . . . . ? O4F Cu3 Cu4 O5E -87.60(17) . . . . ? O4G Cu3 Cu4 O5E 176.66(18) . . . . ? O4E Cu3 Cu4 O5E 1.56(17) . . . . ? O36 Cu3 Cu4 O5E -93.9(7) . . . . ? O1G C1G C2G C6G 0.4(12) . . . . ? N1G C1G C2G C6G 179.9(7) . . . . ? O1G C1G C2G C3G -177.8(8) . . . . ? N1G C1G C2G C3G 1.7(11) . . . . ? C6G C2G C3G C4G 177.9(8) . . . . ? C1G C2G C3G C4G -3.9(13) . . . . ? C6G C2G C3G C9G -1.3(13) . . . . ? C1G C2G C3G C9G 177.0(8) . . . . ? C2G C3G C4G C12G -179.9(9) . . . . ? C9G C3G C4G C12G -0.8(14) . . . . ? C2G C3G C4G C5G 2.0(14) . . . . ? C9G C3G C4G C5G -178.9(9) . . . . ? C12G C4G C5G O2G 2.6(16) . . . . ? C3G C4G C5G O2G -179.3(10) . . . . ? C12G C4G C5G N1G -176.0(9) . . . . ? C3G C4G C5G N1G 2.1(13) . . . . ? C3G C2G C6G C7G 4.2(14) . . . . ? C1G C2G C6G C7G -174.1(8) . . . . ? C2G C6G C7G C8G -3.2(15) . . . . ? C6G C7G C8G C9G -0.8(18) . . . . ? C7G C8G C9G C10G 178.5(11) . . . . ? C7G C8G C9G C3G 3.6(17) . . . . ? C2G C3G C9G C8G -2.6(14) . . . . ? C4G C3G C9G C8G 178.3(9) . . . . ? C2G C3G C9G C10G -177.7(9) . . . . ? C4G C3G C9G C10G 3.1(14) . . . . ? C8G C9G C10G C11G -178.9(11) . . . . ? C3G C9G C10G C11G -4.0(17) . . . . ? C9G C10G C11G C12G 2.3(19) . . . . ? C3G C4G C12G C11G -0.9(15) . . . . ? C5G C4G C12G C11G 177.2(10) . . . . ? C10G C11G C12G C4G 0.2(17) . . . . ? O1G C1G N1G C5G -177.9(7) . . . . ? C2G C1G N1G C5G 2.6(11) . . . . ? O1G C1G N1G C13G -5.3(10) . . . . ? C2G C1G N1G C13G 175.2(6) . . . . ? O2G C5G N1G C1G 176.8(8) . . . . ? C4G C5G N1G C1G -4.5(13) . . . . ? O2G C5G N1G C13G 4.4(12) . . . . ? C4G C5G N1G C13G -176.9(8) . . . . ? C14G C13G N1G C1G -71.2(9) . . . . ? C16G C13G N1G C1G 56.4(8) . . . . ? C14G C13G N1G C5G 101.8(9) . . . . ? C16G C13G N1G C5G -130.6(7) . . . . ? N1G C13G C14G C15G -158.7(7) . . . . ? C16G C13G C14G C15G 75.3(10) . . . . ? C13G C14G C15G O3G 14.4(14) . . . . ? C13G C14G C15G N2G -165.7(9) . . . . ? N1G C13G C16G O4G 47.3(8) . . . . ? C14G C13G C16G O4G 172.1(6) . . . . ? N1G C13G C16G O5G -138.9(6) . . . . ? C14G C13G C16G O5G -14.2(9) . . . . ? O5G C16G O4G Cu3 14.3(10) . . . . ? C13G C16G O4G Cu3 -172.9(4) . . . . ? O4H Cu3 O4G C16G 85.3(5) . . . . ? O4F Cu3 O4G C16G -83.8(5) . . . . ? O36 Cu3 O4G C16G -172.3(5) . . . . ? Cu4 Cu3 O4G C16G -3.0(5) . . . . ? O4G C16G O5G Cu4 -18.8(9) . . . . ? C13G C16G O5G Cu4 168.3(4) . . . . ? O5F Cu4 O5G C16G 98.7(4) . . . . ? O5H Cu4 O5G C16G -70.3(4) . . . . ? O5E Cu4 O5G C16G 13.5(9) . . . . ? O3A Cu4 O5G C16G -163.5(4) . . . . ? Cu3 Cu4 O5G C16G 11.4(4) . . . . ? O1A C1A C2A C6A 10(3) . . . . ? N1A C1A C2A C6A -179.7(18) . . . . ? O1A C1A C2A C3A 175(2) . . . . ? N1A C1A C2A C3A -15(3) . . . . ? C6A C2A C3A C4A 174(2) . . . . ? C1A C2A C3A C4A 9(4) . . . . ? C6A C2A C3A C9A -6(4) . . . . ? C1A C2A C3A C9A -171(3) . . . . ? C2A C3A C4A C12A -175(2) . . . . ? C9A C3A C4A C12A 5(4) . . . . ? C2A C3A C4A C5A 2(4) . . . . ? C9A C3A C4A C5A -179(2) . . . . ? C3A C4A C5A O2A 179(2) . . . . ? C12A C4A C5A O2A -4(3) . . . . ? C3A C4A C5A N1A -5(3) . . . . ? C12A C4A C5A N1A 171.4(18) . . . . ? C3A C2A C6A C7A 14(4) . . . . ? C1A C2A C6A C7A 179(2) . . . . ? C2A C6A C7A C8A -12(4) . . . . ? C6A C7A C8A C9A 3(5) . . . . ? C7A C8A C9A C3A 4(4) . . . . ? C7A C8A C9A C10A -174(3) . . . . ? C2A C3A C9A C8A -3(4) . . . . ? C4A C3A C9A C8A 178(2) . . . . ? C2A C3A C9A C10A 176(3) . . . . ? C4A C3A C9A C10A -4(4) . . . . ? C8A C9A C10A C11A 179(4) . . . . ? C3A C9A C10A C11A 1(5) . . . . ? C9A C10A C11A C12A 2(6) . . . . ? C3A C4A C12A C11A -3(3) . . . . ? C5A C4A C12A C11A -179(2) . . . . ? C10A C11A C12A C4A -1(4) . . . . ? O1A C1A N1A C5A -179.1(16) . . . . ? C2A C1A N1A C5A 11(2) . . . . ? O1A C1A N1A C13A -2(2) . . . . ? C2A C1A N1A C13A -171.7(15) . . . . ? O2A C5A N1A C1A 173.8(16) . . . . ? C4A C5A N1A C13A -179.1(15) . . . . ? C16A C13A N1A C1A 67.8(14) . . . . ? C14A C13A N1A C1A -66.9(14) . . . . ? C16A C13A N1A C5A -114.9(15) . . . . ? C14A C13A N1A C5A 110.4(16) . . . . ? N1A C13A C14A C15A -150.4(8) . . . . ? C16A C13A C14A C15A 75.2(9) . . . . ? C13A C14A C15A O3A 69.0(10) . . . . ? C13A C14A C15A N2A -116.2(8) . . . . ? N2A C15A O3A Cu4 -14.2(10) . . . . ? C14A C15A O3A Cu4 160.3(5) . . . . ? O5F Cu4 O3A C15A -36.9(6) . . . . ? O5G Cu4 O3A C15A -131.0(6) . . . . ? O5H Cu4 O3A C15A 140.5(6) . . . . ? O5E Cu4 O3A C15A 49.8(6) . . . . ? O4B Cu1 O4A C16A 74.6(5) . . . . ? O4D Cu1 O4A C16A -84.5(5) . . . . ? N3J Cu1 O4A C16A 170.8(5) . . . . ? N3I Cu1 O4A C16A 169.8(6) . . . . ? Cu2 Cu1 O4A C16A -6.2(5) . . . . ? O5B Cu2 O5A C16A -84.0(5) . . . . ? O5D Cu2 O5A C16A 92.3(5) . . . . ? O5C Cu2 O5A C16A 7.3(9) . . . . ? O3E Cu2 O5A C16A -172.5(5) . . . . ? Cu1 Cu2 O5A C16A 2.8(5) . . . . ? Cu1 O4A C16A O5A 10.8(10) . . . . ? Cu1 O4A C16A C13A -170.7(5) . . . . ? Cu2 O5A C16A O4A -9.3(10) . . . . ? Cu2 O5A C16A C13A 172.0(4) . . . . ? N1A C13A C16A O4A 0.8(11) . . . . ? C14A C13A C16A O4A 136.9(7) . . . . ? N1A C13A C16A O5A 179.6(7) . . . . ? C14A C13A C16A O5A -44.4(9) . . . . ? O1B C1B C2B C6B -2.1(13) . . . . ? N1B C1B C2B C6B 175.2(8) . . . . ? O1B C1B C2B C3B 178.3(8) . . . . ? N1B C1B C2B C3B -4.4(11) . . . . ? C6B C2B C3B C4B 179.3(9) . . . . ? C1B C2B C3B C4B -1.1(13) . . . . ? C6B C2B C3B C9B -3.3(13) . . . . ? C1B C2B C3B C9B 176.3(8) . . . . ? C2B C3B C4B C12B 178.2(8) . . . . ? C9B C3B C4B C12B 0.7(13) . . . . ? C2B C3B C4B C5B 5.3(13) . . . . ? C9B C3B C4B C5B -172.1(7) . . . . ? C3B C4B C5B O2B -180.0(8) . . . . ? C12B C4B C5B O2B 7.0(12) . . . . ? C3B C4B C5B N1B -3.9(11) . . . . ? C12B C4B C5B N1B -176.9(7) . . . . ? C3B C2B C6B C7B 2.6(14) . . . . ? C1B C2B C6B C7B -177.0(8) . . . . ? C2B C6B C7B C8B -0.7(16) . . . . ? C6B C7B C8B C9B -0.7(18) . . . . ? C7B C8B C9B C10B 178.7(11) . . . . ? C7B C8B C9B C3B 0.2(17) . . . . ? C4B C3B C9B C8B 179.3(9) . . . . ? C2B C3B C9B C8B 1.8(14) . . . . ? C4B C3B C9B C10B 0.6(13) . . . . ? C2B C3B C9B C10B -176.9(8) . . . . ? C8B C9B C10B C11B 179.0(11) . . . . ? C3B C9B C10B C11B -2.5(15) . . . . ? C9B C10B C11B C12B 2.9(16) . . . . ? C3B C4B C12B C11B -0.4(13) . . . . ? C5B C4B C12B C11B 172.7(8) . . . . ? C10B C11B C12B C4B -1.4(14) . . . . ? O2B C5B N1B C1B 174.2(7) . . . . ? C4B C5B N1B C1B -2.1(10) . . . . ? O2B C5B N1B C13B -0.6(10) . . . . ? C4B C5B N1B C13B -176.9(6) . . . . ? O1B C1B N1B C5B -176.6(7) . . . . ? C2B C1B N1B C5B 5.9(10) . . . . ? O1B C1B N1B C13B -1.8(10) . . . . ? C2B C1B N1B C13B -179.2(6) . . . . ? C14B C13B N1B C5B 98.4(7) . . . . ? C16B C13B N1B C5B -134.0(6) . . . . ? C14B C13B N1B C1B -76.8(7) . . . . ? C16B C13B N1B C1B 50.8(8) . . . . ? N1B C13B C14B C15B -166.3(5) . . . . ? C16B C13B C14B C15B 67.8(7) . . . . ? C13B C14B C15B O3B 34.8(9) . . . . ? C13B C14B C15B N2B -144.5(7) . . . . ? N1B C13B C16B O4B 47.1(7) . . . . ? C14B C13B C16B O4B 174.0(6) . . . . ? N1B C13B C16B O5B -136.3(6) . . . . ? C14B C13B C16B O5B -9.4(8) . . . . ? O5B C16B O4B Cu1 2.0(9) . . . . ? C13B C16B O4B Cu1 178.1(4) . . . . ? O4C Cu1 O4B C16B 85.4(5) . . . . ? O4A Cu1 O4B C16B -89.7(5) . . . . ? O4D Cu1 O4B C16B -1.5(8) . . . . ? N3J Cu1 O4B C16B 174.0(5) . . . . ? N3I Cu1 O4B C16B 179.3(5) . . . . ? Cu2 Cu1 O4B C16B -1.2(4) . . . . ? O4B C16B O5B Cu2 -1.4(9) . . . . ? C13B C16B O5B Cu2 -177.7(4) . . . . ? O5C Cu2 O5B C16B -81.3(5) . . . . ? O5A Cu2 O5B C16B 79.9(5) . . . . ? O3E Cu2 O5B C16B 172.8(5) . . . . ? Cu1 Cu2 O5B C16B 0.3(4) . . . . ? O1C C1C C2C C6C 5.8(19) . . . . ? N1C C1C C2C C6C 179.9(11) . . . . ? O1C C1C C2C C3C -176.8(12) . . . . ? N1C C1C C2C C3C -2.6(17) . . . . ? C6C C2C C3C C4C 179.0(12) . . . . ? C1C C2C C3C C4C 1.6(19) . . . . ? C6C C2C C3C C9C -1.4(18) . . . . ? C1C C2C C3C C9C -178.7(11) . . . . ? C2C C3C C4C C12C 177.9(12) . . . . ? C9C C3C C4C C12C -1.7(19) . . . . ? C2C C3C C4C C5C 2.9(19) . . . . ? C9C C3C C4C C5C -176.8(11) . . . . ? C3C C4C C5C O2C 174.2(12) . . . . ? C12C C4C C5C O2C -1.1(19) . . . . ? C3C C4C C5C N1C -5.8(17) . . . . ? C12C C4C C5C N1C 178.8(10) . . . . ? C3C C2C C6C C7C 2.2(19) . . . . ? C1C C2C C6C C7C 179.6(10) . . . . ? C2C C6C C7C C8C 1.3(17) . . . . ? C6C C7C C8C C9C -6.1(19) . . . . ? C7C C8C C9C C10C -177.1(12) . . . . ? C7C C8C C9C C3C 6.8(19) . . . . ? C4C C3C C9C C8C 176.9(12) . . . . ? C2C C3C C9C C8C -2.8(17) . . . . ? C4C C3C C9C C10C 0.3(17) . . . . ? C2C C3C C9C C10C -179.4(11) . . . . ? C8C C9C C10C C11C -175.8(14) . . . . ? C3C C9C C10C C11C 0(2) . . . . ? C9C C10C C11C C12C 1(2) . . . . ? C3C C4C C12C C11C 2.5(18) . . . . ? C5C C4C C12C C11C 177.8(10) . . . . ? C10C C11C C12C C4C -1.8(18) . . . . ? O1C C1C N1C C5C 173.4(11) . . . . ? C2C C1C N1C C5C -0.9(17) . . . . ? O1C C1C N1C C13C -0.5(17) . . . . ? C2C C1C N1C C13C -174.8(9) . . . . ? O2C C5C N1C C1C -175.2(11) . . . . ? C4C C5C N1C C1C 4.9(17) . . . . ? O2C C5C N1C C13C -1.4(16) . . . . ? C4C C5C N1C C13C 178.7(10) . . . . ? C14C C13C N1C C1C -63.8(13) . . . . ? C16C C13C N1C C1C 62.5(12) . . . . ? C14C C13C N1C C5C 121.6(11) . . . . ? C16C C13C N1C C5C -112.0(10) . . . . ? N1C C13C C14C C15C -48.0(12) . . . . ? C16C C13C C14C C15C -173.2(7) . . . . ? C13C C14C C15C O3C -45.2(12) . . . . ? C13C C14C C15C N2C 141.4(8) . . . . ? N1C C13C C16C O5C -160.0(7) . . . . ? C14C C13C C16C O5C -31.8(11) . . . . ? N1C C13C C16C O4C 20.4(11) . . . . ? C14C C13C C16C O4C 148.7(7) . . . . ? O5C C16C O4C Cu1 10.3(10) . . . . ? C13C C16C O4C Cu1 -170.3(6) . . . . ? O4B Cu1 O4C C16C -87.2(5) . . . . ? O4D Cu1 O4C C16C 71.9(5) . . . . ? N3J Cu1 O4C C16C 176.7(5) . . . . ? N3I Cu1 O4C C16C 177.6(6) . . . . ? Cu2 Cu1 O4C C16C -6.3(5) . . . . ? O4C C16C O5C Cu2 -7.7(10) . . . . ? C13C C16C O5C Cu2 172.8(6) . . . . ? O5B Cu2 O5C C16C 88.1(5) . . . . ? O5D Cu2 O5C C16C -88.2(5) . . . . ? O5A Cu2 O5C C16C -2.8(9) . . . . ? O3E Cu2 O5C C16C 177.0(5) . . . . ? Cu1 Cu2 O5C C16C 1.7(5) . . . . ? O1D C1D C2D C6D 0.6(14) . . . . ? N1D C1D C2D C6D -178.1(9) . . . . ? O1D C1D C2D C3D -179.1(9) . . . . ? N1D C1D C2D C3D 2.3(13) . . . . ? C6D C2D C3D C4D -177.5(10) . . . . ? C1D C2D C3D C4D 2.1(15) . . . . ? C6D C2D C3D C9D -4.0(16) . . . . ? C1D C2D C3D C9D 175.6(9) . . . . ? C2D C3D C4D C12D 178.4(10) . . . . ? C9D C3D C4D C12D 5.0(15) . . . . ? C2D C3D C4D C5D -3.6(15) . . . . ? C9D C3D C4D C5D -177.0(9) . . . . ? C3D C4D C5D O2D 175.7(10) . . . . ? C12D C4D C5D O2D -6.1(15) . . . . ? C3D C4D C5D N1D 0.6(13) . . . . ? C12D C4D C5D N1D 178.8(8) . . . . ? C3D C2D C6D C7D 1.8(18) . . . . ? C1D C2D C6D C7D -177.8(10) . . . . ? C2D C6D C7D C8D 0(2) . . . . ? C6D C7D C8D C9D 1(2) . . . . ? C7D C8D C9D C10D 174.4(14) . . . . ? C7D C8D C9D C3D -4(2) . . . . ? C4D C3D C9D C8D 178.2(11) . . . . ? C2D C3D C9D C8D 4.7(16) . . . . ? C4D C3D C9D C10D 0.1(15) . . . . ? C2D C3D C9D C10D -173.5(10) . . . . ? C8D C9D C10D C11D 176.3(13) . . . . ? C3D C9D C10D C11D -5.7(17) . . . . ? C9D C10D C11D C12D 5.9(19) . . . . ? C3D C4D C12D C11D -4.8(15) . . . . ? C5D C4D C12D C11D 177.0(9) . . . . ? C10D C11D C12D C4D -0.6(17) . . . . ? O1D C1D N1D C5D 175.7(7) . . . . ? C2D C1D N1D C5D -5.5(12) . . . . ? O1D C1D N1D C13D 2.7(11) . . . . ? C2D C1D N1D C13D -178.6(7) . . . . ? O2D C5D N1D C1D -171.3(8) . . . . ? C4D C5D N1D C1D 4.2(12) . . . . ? O2D C5D N1D C13D 1.8(12) . . . . ? C4D C5D N1D C13D 177.2(7) . . . . ? C14D C13D N1D C1D -76.7(8) . . . . ? C16D C13D N1D C1D 50.7(9) . . . . ? C14D C13D N1D C5D 109.7(8) . . . . ? C16D C13D N1D C5D -122.9(7) . . . . ? N1D C13D C14D C15D -62.9(9) . . . . ? C16D C13D C14D C15D 172.1(6) . . . . ? C13D C14D C15D O3D -35.9(11) . . . . ? C13D C14D C15D N2D 132.1(9) . . . . ? N1D C13D C16D O5D -136.1(6) . . . . ? C14D C13D C16D O5D -13.5(9) . . . . ? N1D C13D C16D O4D 44.1(8) . . . . ? C14D C13D C16D O4D 166.7(6) . . . . ? O5D C16D O4D Cu1 -0.3(10) . . . . ? C13D C16D O4D Cu1 179.5(4) . . . . ? O4C Cu1 O4D C16D -86.4(5) . . . . ? O4A Cu1 O4D C16D 89.1(6) . . . . ? O4B Cu1 O4D C16D 0.5(9) . . . . ? N3J Cu1 O4D C16D -174.9(5) . . . . ? N3I Cu1 O4D C16D 179.6(6) . . . . ? Cu2 Cu1 O4D C16D 0.2(5) . . . . ? O4D C16D O5D Cu2 0.1(9) . . . . ? C13D C16D O5D Cu2 -179.6(4) . . . . ? O5C Cu2 O5D C16D 81.7(5) . . . . ? O5A Cu2 O5D C16D -79.6(5) . . . . ? O3E Cu2 O5D C16D -172.5(5) . . . . ? Cu1 Cu2 O5D C16D 0.0(5) . . . . ? O1E C1E C2E C6E -2.5(7) . . . . ? N1E C1E C2E C6E 179.1(6) . . . . ? O1E C1E C2E C3E 177.0(5) . . . . ? N1E C1E C2E C3E -1.4(6) . . . . ? C6E C2E C3E C4E -178.6(6) . . . . ? C1E C2E C3E C4E 1.9(6) . . . . ? C6E C2E C3E C9E -0.3(8) . . . . ? C1E C2E C3E C9E -179.8(5) . . . . ? C2E C3E C4E C12E -179.3(5) . . . . ? C9E C3E C4E C12E 2.5(9) . . . . ? C2E C3E C4E C5E -3.4(8) . . . . ? C9E C3E C4E C5E 178.3(6) . . . . ? C12E C4E C5E O2E 2.0(10) . . . . ? C3E C4E C5E O2E -173.8(6) . . . . ? C12E C4E C5E N1E -179.7(6) . . . . ? C3E C4E C5E N1E 4.5(8) . . . . ? C3E C2E C6E C7E -0.5(9) . . . . ? C1E C2E C6E C7E 179.0(6) . . . . ? C2E C6E C7E C8E 1.6(12) . . . . ? C6E C7E C8E C9E -1.7(13) . . . . ? C7E C8E C9E C10E 180.0(8) . . . . ? C7E C8E C9E C3E 0.8(12) . . . . ? C4E C3E C9E C8E 178.6(7) . . . . ? C2E C3E C9E C8E 0.2(9) . . . . ? C4E C3E C9E C10E -0.7(10) . . . . ? C2E C3E C9E C10E -179.0(6) . . . . ? C8E C9E C10E C11E -179.0(8) . . . . ? C3E C9E C10E C11E 0.2(12) . . . . ? C9E C10E C11E C12E -1.4(13) . . . . ? C3E C4E C12E C11E -3.7(11) . . . . ? C5E C4E C12E C11E -179.5(7) . . . . ? C10E C11E C12E C4E 3.2(12) . . . . ? O1E C1E N1E C5E -175.7(5) . . . . ? C2E C1E N1E C5E 2.8(7) . . . . ? O1E C1E N1E C13E -0.7(8) . . . . ? C2E C1E N1E C13E 177.8(4) . . . . ? O2E C5E N1E C1E 174.0(6) . . . . ? C4E C5E N1E C1E -4.4(8) . . . . ? O2E C5E N1E C13E -0.9(8) . . . . ? C4E C5E N1E C13E -179.3(5) . . . . ? C16E C13E N1E C1E 51.0(6) . . . . ? C14E C13E N1E C1E -77.3(6) . . . . ? C16E C13E N1E C5E -133.6(5) . . . . ? C14E C13E N1E C5E 98.0(6) . . . . ? N1E C13E C14E C15E -158.5(5) . . . . ? C16E C13E C14E C15E 74.9(7) . . . . ? C13E C14E C15E O3E 176.8(6) . . . . ? C13E C14E C15E N2E -4.3(9) . . . . ? N1E C13E C16E O4E 35.7(7) . . . . ? C14E C13E C16E O4E 161.4(5) . . . . ? N1E C13E C16E O5E -145.9(5) . . . . ? C14E C13E C16E O5E -20.2(7) . . . . ? N2E C15E O3E Cu2 -7.1(9) . . . . ? C14E C15E O3E Cu2 171.7(4) . . . . ? O5B Cu2 O3E C15E -141.5(5) . . . . ? O5D Cu2 O3E C15E 38.3(6) . . . . ? O5C Cu2 O3E C15E 127.7(5) . . . . ? O5A Cu2 O3E C15E -52.4(5) . . . . ? O5E C16E O4E Cu3 -1.3(8) . . . . ? C13E C16E O4E Cu3 176.9(4) . . . . ? O4H Cu3 O4E C16E -88.8(4) . . . . ? O4F Cu3 O4E C16E 80.7(4) . . . . ? O36 Cu3 O4E C16E 168.7(4) . . . . ? Cu4 Cu3 O4E C16E -0.8(4) . . . . ? O4E C16E O5E Cu4 3.8(9) . . . . ? C13E C16E O5E Cu4 -174.5(4) . . . . ? O5F Cu4 O5E C16E -91.3(5) . . . . ? O5G Cu4 O5E C16E -5.2(9) . . . . ? O5H Cu4 O5E C16E 78.2(5) . . . . ? O3A Cu4 O5E C16E 171.9(5) . . . . ? Cu3 Cu4 O5E C16E -3.1(4) . . . . ? O1F C1F C2F C6F 1.4(12) . . . . ? N1F C1F C2F C6F -177.0(7) . . . . ? O1F C1F C2F C3F -179.0(7) . . . . ? N1F C1F C2F C3F 2.6(10) . . . . ? C6F C2F C3F C4F 176.6(8) . . . . ? C1F C2F C3F C4F -3.0(11) . . . . ? C6F C2F C3F C9F -0.6(12) . . . . ? C1F C2F C3F C9F 179.8(7) . . . . ? C2F C3F C4F C12F -179.5(7) . . . . ? C9F C3F C4F C12F -2.2(11) . . . . ? C2F C3F C4F C5F 0.6(11) . . . . ? C9F C3F C4F C5F 177.8(7) . . . . ? C3F C4F C5F O2F -174.3(7) . . . . ? C12F C4F C5F O2F 5.7(11) . . . . ? C3F C4F C5F N1F 2.2(10) . . . . ? C12F C4F C5F N1F -177.8(6) . . . . ? C3F C2F C6F C7F -1.8(13) . . . . ? C1F C2F C6F C7F 177.8(8) . . . . ? C2F C6F C7F C8F 2.0(14) . . . . ? C6F C7F C8F C9F 0.3(15) . . . . ? C7F C8F C9F C10F -178.7(10) . . . . ? C7F C8F C9F C3F -2.7(14) . . . . ? C4F C3F C9F C8F -174.4(8) . . . . ? C2F C3F C9F C8F 2.8(12) . . . . ? C4F C3F C9F C10F 1.9(12) . . . . ? C2F C3F C9F C10F 179.1(8) . . . . ? C8F C9F C10F C11F 176.9(10) . . . . ? C3F C9F C10F C11F 0.9(14) . . . . ? C9F C10F C11F C12F -3.4(15) . . . . ? C3F C4F C12F C11F -0.1(11) . . . . ? C5F C4F C12F C11F 179.9(7) . . . . ? C10F C11F C12F C4F 2.9(13) . . . . ? O1F C1F N1F C5F -178.2(6) . . . . ? C2F C1F N1F C5F 0.3(9) . . . . ? O1F C1F N1F C13F -4.8(9) . . . . ? C2F C1F N1F C13F 173.7(6) . . . . ? O2F C5F N1F C1F 174.1(6) . . . . ? C4F C5F N1F C1F -2.6(9) . . . . ? O2F C5F N1F C13F 0.8(9) . . . . ? C4F C5F N1F C13F -175.9(5) . . . . ? C14F C13F N1F C1F -75.1(7) . . . . ? C16F C13F N1F C1F 54.5(7) . . . . ? C14F C13F N1F C5F 98.6(6) . . . . ? C16F C13F N1F C5F -131.8(5) . . . . ? N1F C13F C14F C15F -158.7(5) . . . . ? C16F C13F C14F C15F 74.0(6) . . . . ? C13F C14F C15F O3F 33.2(8) . . . . ? C13F C14F C15F N2F -150.8(6) . . . . ? N1F C13F C16F O4F 40.0(7) . . . . ? C14F C13F C16F O4F 167.3(5) . . . . ? N1F C13F C16F O5F -147.1(5) . . . . ? C14F C13F C16F O5F -19.7(8) . . . . ? O5F C16F O4F Cu3 -9.4(9) . . . . ? C13F C16F O4F Cu3 162.8(4) . . . . ? O4H Cu3 O4F C16F -16.4(12) . . . . ? O4G Cu3 O4F C16F 87.2(5) . . . . ? O4E Cu3 O4F C16F -85.8(5) . . . . ? O36 Cu3 O4F C16F -176.1(5) . . . . ? Cu4 Cu3 O4F C16F 5.1(4) . . . . ? O4F C16F O5F Cu4 7.7(8) . . . . ? C13F C16F O5F Cu4 -164.6(4) . . . . ? O5G Cu4 O5F C16F -88.8(4) . . . . ? O5H Cu4 O5F C16F 2.8(11) . . . . ? O5E Cu4 O5F C16F 75.9(4) . . . . ? O3A Cu4 O5F C16F 168.5(4) . . . . ? Cu3 Cu4 O5F C16F -2.7(4) . . . . ? O1H C1H C2H C6H 4.6(10) . . . . ? N1H C1H C2H C6H -176.5(6) . . . . ? O1H C1H C2H C3H -176.6(7) . . . . ? N1H C1H C2H C3H 2.2(10) . . . . ? C6H C2H C3H C4H 179.4(8) . . . . ? C1H C2H C3H C4H 0.7(12) . . . . ? C6H C2H C3H C9H -0.6(12) . . . . ? C1H C2H C3H C9H -179.3(7) . . . . ? C2H C3H C4H C12H 179.1(8) . . . . ? C9H C3H C4H C12H -0.8(13) . . . . ? C2H C3H C4H C5H 1.0(12) . . . . ? C9H C3H C4H C5H -178.9(8) . . . . ? C12H C4H C5H O2H 1.2(13) . . . . ? C3H C4H C5H O2H 179.3(8) . . . . ? C12H C4H C5H N1H 176.3(7) . . . . ? C3H C4H C5H N1H -5.5(11) . . . . ? C3H C2H C6H C7H 1.5(12) . . . . ? C1H C2H C6H C7H -179.8(7) . . . . ? C2H C6H C7H C8H -0.3(13) . . . . ? C6H C7H C8H C9H -1.9(15) . . . . ? C7H C8H C9H C10H -178.2(10) . . . . ? C7H C8H C9H C3H 2.8(16) . . . . ? C4H C3H C9H C8H 178.6(8) . . . . ? C2H C3H C9H C8H -1.4(13) . . . . ? C4H C3H C9H C10H -0.5(14) . . . . ? C2H C3H C9H C10H 179.5(9) . . . . ? C8H C9H C10H C11H -177.9(11) . . . . ? C3H C9H C10H C11H 1.1(16) . . . . ? C9H C10H C11H C12H -0.3(17) . . . . ? C3H C4H C12H C11H 1.6(14) . . . . ? C5H C4H C12H C11H 179.7(8) . . . . ? C10H C11H C12H C4H -1.1(15) . . . . ? O1H C1H N1H C5H 171.5(6) . . . . ? C2H C1H N1H C5H -7.3(9) . . . . ? O1H C1H N1H C13H -1.5(9) . . . . ? C2H C1H N1H C13H 179.6(5) . . . . ? O2H C5H N1H C1H -175.5(7) . . . . ? C4H C5H N1H C1H 8.9(10) . . . . ? O2H C5H N1H C13H -2.6(10) . . . . ? C4H C5H N1H C13H -178.2(6) . . . . ? C16H C13H N1H C1H 46.0(7) . . . . ? C14H C13H N1H C1H -86.6(7) . . . . ? C16H C13H N1H C5H -127.5(6) . . . . ? C14H C13H N1H C5H 100.0(7) . . . . ? C16H C13H C14H C15H -74.9(9) . . . . ? N1H C13H C14H C15H 56.0(9) . . . . ? C13H C14H C15H O3H -90.2(10) . . . . ? C13H C14H C15H N2H 94.5(9) . . . . ? N1H C13H C16H O5H -125.9(6) . . . . ? C14H C13H C16H O5H 4.9(9) . . . . ? N1H C13H C16H O4H 58.8(7) . . . . ? C14H C13H C16H O4H -170.4(6) . . . . ? O5H C16H O4H Cu3 2.3(9) . . . . ? C13H C16H O4H Cu3 177.3(4) . . . . ? O4F Cu3 O4H C16H 23.5(12) . . . . ? O4G Cu3 O4H C16H -80.7(4) . . . . ? O4E Cu3 O4H C16H 93.2(4) . . . . ? O36 Cu3 O4H C16H -177.3(4) . . . . ? Cu4 Cu3 O4H C16H 2.3(4) . . . . ? O4H C16H O5H Cu4 -8.0(9) . . . . ? C13H C16H O5H Cu4 177.3(4) . . . . ? O5F Cu4 O5H C16H 1.5(12) . . . . ? O5G Cu4 O5H C16H 93.5(5) . . . . ? O5E Cu4 O5H C16H -71.2(5) . . . . ? O3A Cu4 O5H C16H -164.3(5) . . . . ? Cu3 Cu4 O5H C16H 7.1(5) . . . . ? O4C Cu1 N3I C21I 158.2(5) . . . . ? O4A Cu1 N3I C21I -22.4(5) . . . . ? O4B Cu1 N3I C21I 68.5(5) . . . . ? O4D Cu1 N3I C21I -111.2(5) . . . . ? N3J Cu1 N3I C21I 169(5) . . . . ? O4C Cu1 N3I C25I -21.9(6) . . . . ? O4A Cu1 N3I C25I 157.4(6) . . . . ? O4B Cu1 N3I C25I -111.7(5) . . . . ? O4D Cu1 N3I C25I 68.7(6) . . . . ? C25I N3I C21I C22I 0.0 . . . . ? Cu1 N3I C21I C22I 179.9(7) . . . . ? N3I C21I C22I C23I 0.0 . . . . ? C21I C22I C23I C24I 0.0 . . . . ? C22I C23I C24I C25I 0.0 . . . . ? C23I C24I C25I N3I 0.0 . . . . ? C21I N3I C25I C24I 0.0 . . . . ? Cu1 N3I C25I C24I -179.8(7) . . . . ? O4C Cu1 N3J C21J 167.0(3) . . . . ? O4A Cu1 N3J C21J -13.8(3) . . . . ? O4B Cu1 N3J C21J 77.7(3) . . . . ? O4D Cu1 N3J C21J -103.9(3) . . . . ? O4C Cu1 N3J C25J -22.01(19) . . . . ? O4A Cu1 N3J C25J 157.25(19) . . . . ? O4B Cu1 N3J C25J -111.26(18) . . . . ? O4D Cu1 N3J C25J 67.1(2) . . . . ? C25J N3J C21J C22J 0.0 . . . . ? Cu1 N3J C21J C22J 170.8(2) . . . . ? N3J C21J C22J C23J 0.0 . . . . ? C21J C22J C23J C24J 0.0 . . . . ? C22J C23J C24J C25J 0.0 . . . . ? C23J C24J C25J N3J 0.0 . . . . ? C21J N3J C25J C24J 0.0 . . . . ? Cu1 N3J C25J C24J -171.1(2) . . . . ? O4H Cu3 O36 C31 -166.3(2) . . . . ? O4F Cu3 O36 C31 9.8(2) . . . . ? O4G Cu3 O36 C31 104.1(2) . . . . ? O4E Cu3 O36 C31 -79.5(2) . . . . ? Cu4 Cu3 O36 C31 16.0(8) . . . . ? Cu3 O36 C31 C34 80.82(13) . . . . ? Cu3 O36 C31 O37 -90.47(13) . . . . ? C32 O37 C31 O36 6.5 . . . . ? C32 O37 C31 C34 -165.4 . . . . ? C31 O37 C32 C33 -162.3 . . . . ? O36 C31 C34 O38 15.6 . . . . ? O37 C31 C34 O38 -172.3 . . . . ? O36 C31 C34 C35 148.3 . . . . ? O37 C31 C34 C35 -39.6 . . . . ? C42 O47 C41 O46 13.5(15) . . . . ? C42 O47 C41 C44 -168.2(8) . . . . ? C41 O47 C42 C43 -156.5(7) . . . . ? O46 C41 C44 O48 -179.7(9) . . . . ? O47 C41 C44 O48 2.1(12) . . . . ? O46 C41 C44 C45 -53.7(12) . . . . ? O47 C41 C44 C45 128.0(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2G H2G1 O1C 0.88 2.06 2.939(13) 172.0 1_455 N2F H2F2 O3C 0.88 2.01 2.873(9) 165.0 1_455 N2A H2A1 O5E 0.88 2.30 3.023(8) 138.9 . N2A H2A2 O3B 0.88 2.27 3.112(9) 161.0 . N2B H2B1 O3F 0.88 2.05 2.895(8) 161.9 . N2B H2B2 O48 0.88 2.46 3.046(10) 124.8 1_655 N2C H2C2 O3G 0.88 2.13 3.001(10) 168.9 1_655 N2D H2D2 O3H 0.88 2.02 2.845(15) 156.2 . N2E H2E1 O5D 0.88 2.28 3.005(7) 139.9 . N2E H2E2 O1H 0.88 2.05 2.898(8) 162.8 . N2F H2F1 O3B 0.88 2.08 2.939(9) 164.8 . N2H H2H1 O1D 0.88 2.09 2.937(9) 160.2 . N2H H2H2 O5H 0.88 2.36 2.889(9) 118.8 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.14 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.858 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.106 _vrf_PLAT201_9 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 192 RESPONSE: Only the copper atoms refined anisotropically due to extensive disorder and moderate crystallinity. ; _vrf_PLAT602_9 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: The voids are not empty but filled with disordered guest species which could not be modeled. They were accoumted for with the Squeeze program. ; #===END