data_cu #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Feng,Shouhua Department of Chemistry Jilin University Changchun, 130023 P. R. China ; _publ_contact_author_phone '86-431-5671974' _publ_contact_author_fax '86-431-5671974' _publ_contact_author_email 'shfeng@mail.jlu.edu.cn' _publ_requested_journal ? _publ_requested_coeditor_name ? #========================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Novel Coordination Polymers with Mixed Ligands and Orientated Enantiomers ; loop_ _publ_author_name _publ_author_address 'Shi, Zhan' ; Department of Chemistry Jilin University Changchun, 130023 P. R. China ; 'Feng, Shouhua' ; Department of Chemistry Jilin University Changchun, 130023 P. R. China ; 'Sun, Yan' ; Department of Chemistry Jilin University Changchun, 130023 P. R. China ; 'Hua, Jia' ; Department of Chemistry Jilin University Changchun, 130023 P. R. China ; #============================================================ data_CyDTA _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H58 Cu2 N6 O20' _chemical_formula_weight 997.94 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1593(8) _cell_length_b 11.5796(9) _cell_length_c 19.8628(15) _cell_angle_alpha 90.487(2) _cell_angle_beta 98.530(2) _cell_angle_gamma 101.598(2) _cell_volume 2484.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.550 _exptl_crystal_size_min 0.550 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12263 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 23.38 _reflns_number_total 7127 _reflns_number_gt 5626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _computing_publication_material 'SHELXTL' _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^)+(0.1322P)^2^+0.5966P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7127 _refine_ls_number_parameters 679 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1920 _refine_ls_wR_factor_gt 0.1780 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 0.12571(5) 0.33248(5) 0.25937(3) 0.0310(2) Uani 1 1 d . . . Cu2 Cu 0.14623(5) 0.82715(5) 0.30117(3) 0.0366(2) Uani 1 1 d . . . O1 O 0.1145(3) 1.1976(3) 0.33060(18) 0.0431(8) Uani 1 1 d . . . O2 O 0.0584(4) 1.0214(3) 0.27692(18) 0.0489(9) Uani 1 1 d . . . O3 O 0.0011(3) 0.7128(3) 0.31850(18) 0.0423(8) Uani 1 1 d . . . O4 O -0.1723(4) 0.6869(4) 0.3641(3) 0.0752(14) Uani 1 1 d . . . O5 O 0.2986(3) 0.9362(3) 0.28610(17) 0.0424(8) Uani 1 1 d . . . O6 O 0.4950(4) 0.9427(4) 0.2757(2) 0.0600(11) Uani 1 1 d . . . O7 O 0.1796(3) 0.4492(3) 0.33742(16) 0.0348(7) Uani 1 1 d . . . O8 O 0.1946(3) 0.5984(3) 0.26687(17) 0.0399(8) Uani 1 1 d . . . N1 N 0.0846(4) 0.2930(3) 0.1583(2) 0.0373(9) Uani 1 1 d . . . N2 N -0.0885(4) 0.1959(3) -0.1981(2) 0.0370(9) Uani 1 1 d . . . N3 N 0.3064(3) 0.3306(4) 0.2534(2) 0.0359(9) Uani 1 1 d . . . N4 N 0.9438(3) 0.3343(3) 0.2603(2) 0.0333(9) Uani 1 1 d . . . N5 N 0.2879(3) 0.7636(3) 0.37483(19) 0.0319(9) Uani 1 1 d . . . N6 N 0.1113(3) 0.9070(3) 0.39624(19) 0.0318(9) Uani 1 1 d . . . C1 C 0.0910(7) 0.3815(5) 0.1159(3) 0.0588(16) Uani 1 1 d . . . H1 H 0.1156 0.4583 0.1342 0.071 Uiso 1 1 calc . . . C2 C 0.0633(7) 0.3650(5) 0.0470(3) 0.0642(18) Uani 1 1 d . . . H2 H 0.0727 0.4294 0.0192 0.077 Uiso 1 1 calc . . . C3 C 0.0208(5) 0.2513(4) 0.0182(2) 0.0445(13) Uani 1 1 d . . . C4 C 0.0139(6) 0.1609(5) 0.0620(3) 0.0544(15) Uani 1 1 d . . . C5 C 0.0478(6) 0.1834(5) 0.1308(3) 0.0513(14) Uani 1 1 d . . . H5 H 0.0451 0.1202 0.1595 0.062 Uiso 1 1 calc . . . C6 C -0.0029(6) 0.2872(5) -0.1706(3) 0.0517(15) Uani 1 1 d . . . C7 C 0.0358(6) 0.3079(5) -0.1023(3) 0.0573(16) Uani 1 1 d . . . H7 H 0.0971 0.3733 -0.0864 0.069 Uiso 1 1 calc . . . C8 C -0.0163(5) 0.2314(5) -0.0572(3) 0.0436(12) Uani 1 1 d . . . C9 C -0.1053(6) 0.1357(5) -0.0849(3) 0.0546(15) Uani 1 1 d . . . H9 H -0.1428 0.0812 -0.0564 0.065 Uiso 1 1 calc . . . C10 C -0.1386(6) 0.1203(5) -0.1536(3) 0.0517(14) Uani 1 1 d . . . C11 C 0.3870(5) 0.4276(5) 0.2448(3) 0.0520(14) Uani 1 1 d . . . C12 C 0.5108(6) 0.4309(6) 0.2449(4) 0.0560(17) Uani 1 1 d . . . C13 C 0.5579(4) 0.3310(4) 0.2540(2) 0.0355(11) Uani 1 1 d . . . C14 C 0.4716(5) 0.2282(5) 0.2612(3) 0.0411(12) Uani 1 1 d . . . C15 C 0.3500(4) 0.2317(4) 0.2601(3) 0.0408(12) Uani 1 1 d . . . H15 H 0.2947 0.1614 0.2642 0.080 Uiso 1 1 calc . . . C16 C 0.9033(5) 0.4316(5) 0.2719(3) 0.0425(13) Uani 1 1 d . . . C17 C 0.7805(5) 0.4343(5) 0.2701(3) 0.0465(13) Uani 1 1 d . . . C18 C 0.6906(4) 0.3314(4) 0.2557(3) 0.0373(11) Uani 1 1 d . . . C19 C 0.7332(5) 0.2294(5) 0.2451(3) 0.0439(13) Uani 1 1 d . . . C20 C 0.8591(4) 0.2353(4) 0.2481(3) 0.0437(13) Uani 1 1 d . . . H20 H 0.8858 0.1656 0.2411 0.080 Uiso 1 1 calc . . . C21 C 0.1808(5) 0.8552(4) 0.4551(2) 0.0342(11) Uani 1 1 d . . . C22 C 0.3048(5) 0.8415(4) 0.4377(2) 0.0362(11) Uani 1 1 d . . . C23 C 0.3841(5) 0.7989(5) 0.4992(3) 0.0504(14) Uani 1 1 d . . . H23A H 0.3460 0.7189 0.5086 0.080 Uiso 1 1 calc . . . H23B H 0.4656 0.7979 0.4880 0.080 Uiso 1 1 calc . . . C24 C 0.3973(6) 0.8786(6) 0.5629(3) 0.0631(17) Uani 1 1 d . . . H24A H 0.4481 0.8502 0.6005 0.080 Uiso 1 1 calc . . . H24B H 0.4373 0.9584 0.5543 0.080 Uiso 1 1 calc . . . C25 C 0.2695(7) 0.8781(6) 0.5811(3) 0.0615(17) Uani 1 1 d . . . C26 C 0.1931(7) 0.9247(5) 0.5230(3) 0.0495(14) Uani 1 1 d . . . C27 C 0.1444(5) 1.0361(4) 0.3955(3) 0.0360(11) Uani 1 1 d . . . C28 C 0.1005(4) 1.0872(4) 0.3281(3) 0.0353(11) Uani 1 1 d . . . C29 C -0.0246(5) 0.8653(4) 0.3936(3) 0.0383(11) Uani 1 1 d . . . C30 C -0.0681(5) 0.7457(4) 0.3569(3) 0.0453(13) Uani 1 1 d . . . C31 C 0.3977(5) 0.7924(5) 0.3412(3) 0.0398(12) Uani 1 1 d . . . C32 C 0.3971(5) 0.8972(4) 0.2980(3) 0.0409(12) Uani 1 1 d . . . C33 C 0.2554(5) 0.6371(4) 0.3878(3) 0.0367(11) Uani 1 1 d . . . C34 C 0.2056(4) 0.5587(4) 0.3242(2) 0.0328(10) Uani 1 1 d . . . O1W O 0.3527(6) 0.3084(7) 0.4287(3) 0.117(2) Uani 1 1 d . . . O2W O 0.8372(5) 0.9382(6) 0.1898(3) 0.1077(19) Uani 1 1 d . . . O3W O 0.8358(7) 0.4778(6) 0.4475(4) 0.125(2) Uani 1 1 d . . . O4W O 0.6638(7) 0.7440(8) 0.4409(4) 0.138(3) Uani 1 1 d . . . O5W O 0.0285(7) 0.3413(7) 0.4490(3) 0.124(2) Uani 1 1 d . . . O6W O 0.5671(9) 0.4787(8) 0.4230(5) 0.176(4) Uani 1 1 d . . . O7W O 0.4657(10) 0.0072(10) 0.1380(4) 0.179(4) Uani 1 1 d . . . O8W O 0.6682(7) 0.8082(10) 0.2690(6) 0.201(5) Uani 1 1 d . . . O9W O 0.3081(16) 0.6586(14) 0.1431(10) 0.158(7) Uani 0.50 1 d P . . O10W O 0.7659(16) 0.9475(14) 0.0513(8) 0.152(7) Uani 0.50 1 d P . . O11W O 0.3365(19) 0.1786(19) 0.0743(10) 0.184(8) Uani 0.50 1 d P . . O12W O 0.380(2) 0.423(3) 0.0539(14) 0.264(15) Uani 0.50 1 d P . . O13W O 0.546(3) 1.173(2) -0.0611(12) 0.243(13) Uani 0.50 1 d P . . O14W O 0.597(3) 0.674(2) 0.1453(14) 0.294(18) Uani 0.50 1 d P . . O15W O 0.677(2) 1.138(2) 0.0650(14) 0.227(10) Uiso 0.50 1 d P . . O16W O 0.654(3) 0.517(2) 0.0773(14) 0.234(11) Uiso 0.50 1 d P . . H4 H -0.001(6) 0.080(6) 0.041(3) 0.066(18) Uiso 1 1 d . . . H6 H 0.024(4) 0.331(4) -0.196(3) 0.029(14) Uiso 1 1 d . . . H10 H -0.208(7) 0.048(7) -0.177(4) 0.10(2) Uiso 1 1 d . . . H11 H 0.344(5) 0.491(5) 0.234(3) 0.041(14) Uiso 1 1 d . . . H12 H 0.559(6) 0.483(6) 0.241(3) 0.06(2) Uiso 1 1 d . . . H14 H 0.487(4) 0.170(4) 0.265(2) 0.021(13) Uiso 1 1 d . . . H16 H 0.963(5) 0.493(4) 0.286(2) 0.032(12) Uiso 1 1 d . . . H17 H 0.750(5) 0.510(5) 0.273(3) 0.054(15) Uiso 1 1 d . . . H19 H 0.678(5) 0.150(5) 0.234(3) 0.056(16) Uiso 1 1 d . . . H21 H 0.139(4) 0.776(4) 0.458(2) 0.018(10) Uiso 1 1 d . . . H22 H 0.344(4) 0.920(4) 0.428(2) 0.033(12) Uiso 1 1 d . . . H25A H 0.257(7) 0.935(6) 0.614(4) 0.08(2) Uiso 1 1 d . . . H25B H 0.221(5) 0.799(6) 0.587(3) 0.055(16) Uiso 1 1 d . . . H26A H 0.121(6) 0.917(5) 0.534(3) 0.048(17) Uiso 1 1 d . . . H26B H 0.246(5) 1.002(5) 0.529(3) 0.050(15) Uiso 1 1 d . . . H27A H 0.120(6) 1.062(6) 0.433(4) 0.08(2) Uiso 1 1 d . . . H27B H 0.238(4) 1.062(4) 0.401(2) 0.021(10) Uiso 1 1 d . . . H29A H -0.049(4) 0.855(4) 0.444(2) 0.031(12) Uiso 1 1 d . . . H29B H -0.070(6) 0.924(5) 0.357(3) 0.065(18) Uiso 1 1 d . . . H31A H 0.464(5) 0.805(4) 0.365(2) 0.025(13) Uiso 1 1 d . . . H31B H 0.393(4) 0.732(4) 0.313(2) 0.022(11) Uiso 1 1 d . . . H33A H 0.197(5) 0.626(4) 0.420(3) 0.031(12) Uiso 1 1 d . . . H33B H 0.309(5) 0.612(5) 0.410(3) 0.038(15) Uiso 1 1 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 0.0207(3) 0.0424(4) 0.0304(3) 0.0020(2) 0.0030(2) 0.0085(2) Cu2 0.0382(4) 0.0398(4) 0.0282(4) 0.0050(2) 0.0038(2) 0.0003(3) O1 0.047(2) 0.0307(18) 0.054(2) 0.0128(15) 0.0104(16) 0.0119(15) O2 0.064(2) 0.046(2) 0.039(2) 0.0066(17) 0.0053(18) 0.0170(18) O3 0.043(2) 0.0389(18) 0.043(2) -0.0038(15) 0.0123(16) -0.0004(15) O4 0.066(3) 0.061(3) 0.093(4) -0.018(2) 0.043(3) -0.023(2) O5 0.036(2) 0.0441(19) 0.042(2) 0.0110(16) -0.0009(15) 0.0024(16) O6 0.046(2) 0.060(2) 0.073(3) 0.018(2) 0.019(2) 0.0003(19) O7 0.0341(18) 0.0289(17) 0.0405(19) 0.0019(14) 0.0038(14) 0.0057(13) O8 0.045(2) 0.0420(18) 0.0330(19) 0.0046(15) 0.0010(15) 0.0129(15) N1 0.038(2) 0.045(2) 0.030(2) 0.0005(18) 0.0028(17) 0.0126(18) N2 0.042(2) 0.037(2) 0.032(2) 0.0088(17) 0.0049(18) 0.0097(19) N3 0.023(2) 0.049(2) 0.037(2) 0.0041(18) 0.0067(16) 0.0086(18) N4 0.023(2) 0.040(2) 0.037(2) 0.0026(17) 0.0053(16) 0.0061(17) N5 0.034(2) 0.0303(19) 0.032(2) 0.0012(16) 0.0055(16) 0.0089(16) N6 0.034(2) 0.0273(19) 0.034(2) 0.0049(16) 0.0066(16) 0.0069(16) C1 0.093(5) 0.040(3) 0.040(3) 0.000(2) -0.002(3) 0.011(3) C2 0.102(5) 0.051(3) 0.037(3) 0.007(3) -0.004(3) 0.019(3) C3 0.048(3) 0.053(3) 0.033(3) 0.004(2) 0.001(2) 0.016(3) C4 0.082(4) 0.041(3) 0.036(3) 0.000(2) 0.003(3) 0.007(3) C5 0.071(4) 0.045(3) 0.036(3) 0.008(2) 0.003(3) 0.012(3) C6 0.065(4) 0.046(3) 0.037(3) 0.011(3) 0.004(3) -0.006(3) C7 0.071(4) 0.053(3) 0.036(3) 0.006(3) -0.005(3) -0.006(3) C8 0.054(3) 0.045(3) 0.031(3) 0.002(2) 0.002(2) 0.012(2) C9 0.066(4) 0.053(3) 0.036(3) 0.011(3) 0.002(3) -0.004(3) C10 0.066(4) 0.048(3) 0.035(3) 0.007(2) 0.003(3) -0.001(3) C11 0.037(3) 0.052(3) 0.076(4) 0.016(3) 0.018(3) 0.022(3) C12 0.036(3) 0.046(3) 0.089(5) 0.016(3) 0.021(3) 0.006(3) C13 0.026(2) 0.046(3) 0.037(3) 0.002(2) 0.0039(19) 0.013(2) C14 0.031(3) 0.038(3) 0.058(3) 0.004(2) 0.007(2) 0.015(2) C15 0.027(3) 0.046(3) 0.050(3) 0.001(2) 0.011(2) 0.005(2) C16 0.023(3) 0.039(3) 0.063(4) 0.001(3) 0.002(2) 0.004(2) C17 0.034(3) 0.039(3) 0.067(4) 0.002(2) 0.003(2) 0.010(2) C18 0.027(3) 0.044(3) 0.040(3) 0.004(2) 0.005(2) 0.007(2) C19 0.027(3) 0.037(3) 0.067(4) -0.003(2) 0.007(2) 0.006(2) C20 0.027(3) 0.042(3) 0.064(4) 0.001(2) 0.004(2) 0.014(2) C21 0.042(3) 0.029(2) 0.031(3) 0.0026(19) 0.003(2) 0.007(2) C22 0.043(3) 0.029(2) 0.033(3) 0.003(2) -0.003(2) 0.007(2) C23 0.052(3) 0.054(3) 0.044(3) 0.004(3) -0.012(3) 0.020(3) C24 0.076(4) 0.066(4) 0.041(3) 0.001(3) -0.010(3) 0.015(3) C25 0.099(5) 0.058(4) 0.028(3) 0.005(3) 0.005(3) 0.022(4) C26 0.063(4) 0.051(3) 0.037(3) 0.000(2) 0.011(3) 0.016(3) C27 0.044(3) 0.028(2) 0.037(3) 0.003(2) 0.005(2) 0.009(2) C28 0.027(2) 0.040(3) 0.043(3) 0.009(2) 0.010(2) 0.013(2) C29 0.036(3) 0.032(2) 0.049(3) 0.004(2) 0.013(2) 0.007(2) C30 0.049(3) 0.041(3) 0.043(3) 0.007(2) 0.012(2) 0.000(2) C31 0.032(3) 0.041(3) 0.043(3) -0.001(2) 0.000(2) 0.003(2) C32 0.043(3) 0.039(3) 0.036(3) 0.000(2) 0.005(2) -0.002(2) C33 0.041(3) 0.035(3) 0.033(3) 0.006(2) -0.001(2) 0.012(2) C34 0.023(2) 0.036(3) 0.040(3) 0.001(2) 0.0051(19) 0.0091(19) O1W 0.083(4) 0.191(7) 0.080(4) 0.032(4) -0.002(3) 0.041(4) O2W 0.077(4) 0.121(5) 0.117(5) 0.002(4) 0.000(3) 0.013(3) O3W 0.141(6) 0.112(5) 0.117(5) 0.020(4) 0.039(4) 0.001(4) O4W 0.105(5) 0.229(8) 0.110(5) 0.052(5) 0.032(4) 0.093(5) O5W 0.121(5) 0.170(6) 0.079(4) 0.017(4) 0.046(4) 0.008(5) O6W 0.160(8) 0.140(6) 0.192(9) 0.050(6) -0.027(6) -0.017(6) O7W 0.204(10) 0.225(10) 0.108(6) 0.021(6) 0.046(6) 0.026(8) O8W 0.104(6) 0.297(12) 0.257(11) 0.178(10) 0.096(6) 0.118(7) O9W 0.163(14) 0.153(13) 0.206(18) 0.104(12) 0.100(13) 0.088(11) O10W 0.140(13) 0.150(13) 0.133(13) 0.044(10) -0.022(10) -0.023(10) O11W 0.171(18) 0.22(2) 0.158(16) 0.036(15) -0.019(13) 0.067(15) O12W 0.128(17) 0.41(4) 0.25(3) 0.10(3) 0.047(17) 0.02(2) O13W 0.37(4) 0.20(2) 0.150(19) 0.002(16) -0.03(2) 0.08(2) O14W 0.44(5) 0.18(2) 0.22(3) 0.10(2) 0.02(3) -0.03(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 O7 1.988(3) . ? Cu1 N1 2.019(4) . ? Cu1 N4 2.037(4) 1_455 ? Cu1 N3 2.041(4) . ? Cu1 O1 2.114(3) 1_545 ? Cu2 O3 1.951(3) . ? Cu2 O5 1.967(3) . ? Cu2 N2 2.052(4) 2_565 ? Cu2 N6 2.215(4) . ? Cu2 N5 2.232(4) . ? O1 C28 1.256(6) . ? O1 Cu1 2.114(3) 1_565 ? O2 C28 1.240(6) . ? O3 C30 1.269(6) . ? O4 C30 1.252(7) . ? O5 C32 1.261(6) . ? O6 C32 1.258(7) . ? O7 C34 1.281(5) . ? O8 C34 1.231(6) . ? N1 C1 1.330(7) . ? N1 C5 1.337(7) . ? N2 C6 1.326(7) . ? N2 C10 1.350(7) . ? N2 Cu2 2.052(4) 2_565 ? N3 C11 1.320(7) . ? N3 C15 1.332(6) . ? N4 C20 1.326(6) . ? N4 C16 1.326(6) . ? N4 Cu1 2.037(4) 1_655 ? N5 C31 1.463(7) . ? N5 C33 1.471(6) . ? N5 C22 1.501(6) . ? N6 C27 1.467(6) . ? N6 C29 1.488(6) . ? N6 C21 1.503(6) . ? C1 C2 1.360(8) . ? C1 H1 0.9300 . ? C2 C3 1.393(8) . ? C2 H2 0.9300 . ? C3 C4 1.364(8) . ? C3 C8 1.498(7) . ? C4 C5 1.371(8) . ? C4 H4 1.00(6) . ? C5 H5 0.9300 . ? C6 C7 1.364(8) . ? C6 H6 0.78(5) . ? C7 C8 1.374(8) . ? C7 H7 0.9300 . ? C8 C9 1.379(8) . ? C9 C10 1.361(8) . ? C9 H9 0.9300 . ? C10 H10 1.07(8) . ? C11 C12 1.374(8) . ? C11 H11 0.96(5) . ? C12 C13 1.367(8) . ? C12 H12 0.74(7) . ? C13 C14 1.396(7) . ? C13 C18 1.475(7) . ? C14 C15 1.362(7) . ? C14 H14 0.73(5) . ? C15 H15 0.9300 . ? C16 C17 1.372(7) . ? C16 H16 0.88(5) . ? C17 C18 1.392(7) . ? C17 H17 1.01(6) . ? C18 C19 1.385(7) . ? C19 C20 1.385(7) . ? C19 H19 1.00(6) . ? C20 H20 0.9300 . ? C21 C22 1.513(7) . ? C21 C26 1.538(7) . ? C21 H21 0.95(4) . ? C22 C23 1.543(7) . ? C22 H22 0.96(5) . ? C23 C24 1.531(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.521(10) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.502(9) . ? C25 H25A 0.97(7) . ? C25 H25B 0.99(6) . ? C26 H26A 0.85(6) . ? C26 H26B 0.96(6) . ? C27 C28 1.522(7) . ? C27 H27A 0.90(7) . ? C27 H27B 1.02(5) . ? C29 C30 1.514(7) . ? C29 H29A 1.08(5) . ? C29 H29B 1.13(6) . ? C31 C32 1.493(7) . ? C31 H31A 0.81(5) . ? C31 H31B 0.88(5) . ? C33 C34 1.516(7) . ? C33 H33A 0.97(5) . ? C33 H33B 0.79(6) . ? 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 O7 Cu1 N1 151.05(15) . . ? O7 Cu1 N4 92.14(14) . 1_455 ? N1 Cu1 N4 88.65(16) . 1_455 ? O7 Cu1 N3 89.97(14) . . ? N1 Cu1 N3 88.61(16) . . ? N4 Cu1 N3 177.19(15) 1_455 . ? O7 Cu1 O1 88.13(13) . 1_545 ? N1 Cu1 O1 120.82(15) . 1_545 ? N4 Cu1 O1 89.51(14) 1_455 1_545 ? N3 Cu1 O1 92.42(15) . 1_545 ? O3 Cu2 O5 176.67(15) . . ? O3 Cu2 N2 90.67(15) . 2_565 ? O5 Cu2 N2 90.80(15) . 2_565 ? O3 Cu2 N6 80.04(14) . . ? O5 Cu2 N6 100.44(14) . . ? N2 Cu2 N6 144.09(15) 2_565 . ? O3 Cu2 N5 98.09(15) . . ? O5 Cu2 N5 78.77(14) . . ? N2 Cu2 N5 134.64(15) 2_565 . ? N6 Cu2 N5 81.21(14) . . ? C28 O1 Cu1 136.1(3) . 1_565 ? C30 O3 Cu2 117.9(3) . . ? C32 O5 Cu2 116.1(3) . . ? C34 O7 Cu1 117.9(3) . . ? C1 N1 C5 117.4(4) . . ? C1 N1 Cu1 118.2(3) . . ? C5 N1 Cu1 124.4(3) . . ? C6 N2 C10 115.7(5) . . ? C6 N2 Cu2 122.6(4) . 2_565 ? C10 N2 Cu2 121.7(3) . 2_565 ? C11 N3 C15 116.4(4) . . ? C11 N3 Cu1 122.0(3) . . ? C15 N3 Cu1 121.6(3) . . ? C20 N4 C16 116.7(4) . . ? C20 N4 Cu1 120.1(3) . 1_655 ? C16 N4 Cu1 123.2(3) . 1_655 ? C31 N5 C33 112.2(4) . . ? C31 N5 C22 109.8(4) . . ? C33 N5 C22 113.3(4) . . ? C31 N5 Cu2 101.9(3) . . ? C33 N5 Cu2 113.9(3) . . ? C22 N5 Cu2 105.0(3) . . ? C27 N6 C29 111.2(4) . . ? C27 N6 C21 113.9(4) . . ? C29 N6 C21 110.5(4) . . ? C27 N6 Cu2 110.3(3) . . ? C29 N6 Cu2 102.6(3) . . ? C21 N6 Cu2 107.7(3) . . ? N1 C1 C2 123.0(5) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 119.8(5) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 116.8(5) . . ? C4 C3 C8 122.5(5) . . ? C2 C3 C8 120.7(5) . . ? C3 C4 C5 120.4(5) . . ? C3 C4 H4 116(4) . . ? C5 C4 H4 123(4) . . ? N1 C5 C4 122.5(5) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? N2 C6 C7 124.6(6) . . ? N2 C6 H6 115(4) . . ? C7 C6 H6 120(4) . . ? C6 C7 C8 119.6(5) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C9 116.6(5) . . ? C7 C8 C3 121.8(5) . . ? C9 C8 C3 121.6(5) . . ? C10 C9 C8 120.5(5) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? N2 C10 C9 123.0(5) . . ? N2 C10 H10 115(4) . . ? C9 C10 H10 123(4) . . ? N3 C11 C12 123.5(5) . . ? N3 C11 H11 110(3) . . ? C12 C11 H11 127(3) . . ? C13 C12 C11 120.9(6) . . ? C13 C12 H12 112(5) . . ? C11 C12 H12 127(5) . . ? C12 C13 C14 115.3(5) . . ? C12 C13 C18 122.4(5) . . ? C14 C13 C18 122.3(4) . . ? C15 C14 C13 120.5(5) . . ? C15 C14 H14 116(4) . . ? C13 C14 H14 124(4) . . ? N3 C15 C14 123.4(5) . . ? N3 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? N4 C16 C17 123.5(5) . . ? N4 C16 H16 114(3) . . ? C17 C16 H16 122(3) . . ? C16 C17 C18 120.2(5) . . ? C16 C17 H17 123(3) . . ? C18 C17 H17 117(3) . . ? C19 C18 C17 116.2(5) . . ? C19 C18 C13 122.2(4) . . ? C17 C18 C13 121.6(5) . . ? C18 C19 C20 119.4(5) . . ? C18 C19 H19 124(3) . . ? C20 C19 H19 117(3) . . ? N4 C20 C19 123.9(4) . . ? N4 C20 H20 118.1 . . ? C19 C20 H20 118.1 . . ? N6 C21 C22 109.4(4) . . ? N6 C21 C26 113.2(4) . . ? C22 C21 C26 112.5(4) . . ? N6 C21 H21 107(2) . . ? C22 C21 H21 103(2) . . ? C26 C21 H21 111(3) . . ? N5 C22 C21 110.7(4) . . ? N5 C22 C23 112.9(4) . . ? C21 C22 C23 111.1(4) . . ? N5 C22 H22 109(3) . . ? C21 C22 H22 104(3) . . ? C23 C22 H22 109(3) . . ? C24 C23 C22 111.7(5) . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C25 C24 C23 109.2(5) . . ? C25 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? C25 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? C26 C25 C24 109.1(5) . . ? C26 C25 H25A 93(4) . . ? C24 C25 H25A 121(4) . . ? C26 C25 H25B 104(3) . . ? C24 C25 H25B 114(3) . . ? H25A C25 H25B 112(6) . . ? C25 C26 C21 113.4(5) . . ? C25 C26 H26A 106(4) . . ? C21 C26 H26A 108(4) . . ? C25 C26 H26B 92(3) . . ? C21 C26 H26B 118(3) . . ? H26A C26 H26B 118(5) . . ? N6 C27 C28 114.2(4) . . ? N6 C27 H27A 105(4) . . ? C28 C27 H27A 117(5) . . ? N6 C27 H27B 109(2) . . ? C28 C27 H27B 103(2) . . ? H27A C27 H27B 107(5) . . ? O2 C28 O1 126.0(5) . . ? O2 C28 C27 120.3(4) . . ? O1 C28 C27 113.7(4) . . ? N6 C29 C30 110.9(4) . . ? N6 C29 H29A 111(2) . . ? C30 C29 H29A 107(2) . . ? N6 C29 H29B 106(3) . . ? C30 C29 H29B 102(3) . . ? H29A C29 H29B 120(4) . . ? O4 C30 O3 123.7(5) . . ? O4 C30 C29 118.2(5) . . ? O3 C30 C29 118.1(4) . . ? N5 C31 C32 112.5(4) . . ? N5 C31 H31A 117(3) . . ? C32 C31 H31A 106(3) . . ? N5 C31 H31B 106(3) . . ? C32 C31 H31B 106(3) . . ? H31A C31 H31B 109(4) . . ? O6 C32 O5 123.4(5) . . ? O6 C32 C31 118.4(5) . . ? O5 C32 C31 118.3(5) . . ? N5 C33 C34 114.2(4) . . ? N5 C33 H33A 108(3) . . ? C34 C33 H33A 111(3) . . ? N5 C33 H33B 114(4) . . ? C34 C33 H33B 110(4) . . ? H33A C33 H33B 99(5) . . ? O8 C34 O7 125.2(4) . . ? O8 C34 C33 122.3(4) . . ? O7 C34 C33 112.5(4) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 23.38 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.872 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.114 #==============================================END data_EDTA _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H48 Cu3 N9 O13' _chemical_formula_weight 1113.54 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 40.889(7) _cell_length_b 19.545(4) _cell_length_c 16.642(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.717(6) _cell_angle_gamma 90.00 _cell_volume 13299(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour blue _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4576 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5842 _exptl_absorpt_correction_T_max 0.6896 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12345 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.1515 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 12.83 _diffrn_reflns_theta_max 23.26 _reflns_number_total 7055 _reflns_number_gt 4111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _computing_publication_material 'SHELXTL' _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^)+(0.0541P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7055 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _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 0.112637(18) 0.21081(4) 0.85764(5) 0.0328(3) Uani 1 1 d . . . Cu2 Cu 0.135020(19) -0.22512(4) 0.87981(5) 0.0318(3) Uani 1 1 d . . . Cu3 Cu 0.129228(19) 0.03405(4) 0.59742(4) 0.0305(3) Uani 1 1 d . . . O1 O 0.13329(12) 0.1103(3) 0.5185(3) 0.0403(11) Uani 1 1 d . . . O2 O 0.16154(11) 0.2056(2) 0.4970(3) 0.0407(11) Uani 1 1 d . . . O3 O 0.14911(13) -0.0451(3) 0.5160(3) 0.0505(13) Uani 1 1 d . . . O4 O 0.1900(3) -0.0434(7) 0.4312(8) 0.156(7) Uani 1 1 d . . . O5 O 0.13287(11) -0.1377(2) 0.8183(3) 0.0353(11) Uani 1 1 d . . . O6 O 0.11406(17) -0.2112(3) 0.7295(3) 0.0605(15) Uani 1 1 d . . . O7 O 0.11744(12) 0.1095(2) 0.7006(3) 0.0384(11) Uani 1 1 d . . . O8 O 0.11220(11) 0.1112(2) 0.8343(3) 0.0349(11) Uani 1 1 d . . . O9 O 0.13624(12) 0.1803(3) 0.9808(3) 0.0445(12) Uani 1 1 d . . . O10 O 0.08824(14) 0.2340(3) 0.7213(3) 0.0537(13) Uani 1 1 d . . . O11 O 0.2215(2) 0.2789(6) 0.5210(7) 0.112(3) Uani 1 1 d . . . O12 O 0.2367(6) 0.0240(11) 0.3616(11) 0.178(6) Uani 1 1 d . . . O13 O 0.1064(4) 0.3545(6) 0.6403(6) 0.127(4) Uani 1 1 d . . . N1 N 0.18077(14) -0.2395(3) 0.8340(3) 0.0384(14) Uani 1 1 d . . . N2 N 0.34130(14) -0.2777(3) 0.6888(3) 0.0347(13) Uani 1 1 d . . . N3 N 0.12789(13) -0.3284(3) 0.8914(4) 0.0336(14) Uani 1 1 d . . . N4 N 0.11229(15) -0.6870(3) 0.8822(4) 0.0402(15) Uani 1 1 d . . . N5 N 0.08998(14) -0.2098(3) 0.9271(3) 0.0335(13) Uani 1 1 d . . . N6 N 0.08244(14) 0.0176(3) 0.5660(3) 0.0344(13) Uani 1 1 d . . . N7 N 0.06714(18) 0.2008(3) 0.9042(4) 0.0426(18) Uani 1 1 d . . . N8 N 0.17743(14) 0.0556(3) 0.6133(3) 0.0327(13) Uani 1 1 d . . . N9 N 0.13374(13) -0.0291(3) 0.7026(3) 0.0316(13) Uani 1 1 d . . . C1 C 0.1909(2) -0.2978(4) 0.8015(6) 0.053(2) Uani 1 1 d . . . H1 H 0.1764 -0.3344 0.7984 0.080 Uiso 1 1 calc . . . C2 C 0.2219(2) -0.3062(4) 0.7723(6) 0.055(2) Uani 1 1 d . . . H2 H 0.2280 -0.3479 0.7502 0.080 Uiso 1 1 calc . . . C3 C 0.24399(17) -0.2532(4) 0.7757(4) 0.0374(16) Uani 1 1 d . . . C4 C 0.23366(17) -0.1922(4) 0.8098(5) 0.0422(17) Uani 1 1 d . . . H4 H 0.2477 -0.1549 0.8139 0.080 Uiso 1 1 calc . . . C5 C 0.20170(18) -0.1882(4) 0.8375(5) 0.0409(17) Uani 1 1 d . . . H5 H 0.1947 -0.1471 0.8597 0.080 Uiso 1 1 calc . . . C6 C 0.31749(19) -0.3179(4) 0.6640(4) 0.0406(18) Uani 1 1 d . . . H6 H 0.3223 -0.3524 0.6274 0.080 Uiso 1 1 calc . . . C7 C 0.28576(18) -0.3116(4) 0.6895(4) 0.0415(17) Uani 1 1 d . . . H7 H 0.2696 -0.3413 0.6705 0.080 Uiso 1 1 calc . . . C8 C 0.27800(17) -0.2599(4) 0.7444(4) 0.0362(16) Uani 1 1 d . . . C9 C 0.30360(19) -0.2187(4) 0.7717(4) 0.0425(18) Uani 1 1 d . . . H9 H 0.2999 -0.1848 0.8098 0.080 Uiso 1 1 calc . . . C10 C 0.33417(17) -0.2286(4) 0.7419(4) 0.0407(17) Uani 1 1 d . . . H10 H 0.3509 -0.1997 0.7593 0.080 Uiso 1 1 calc . . . C11 C 0.1114(2) -0.3597(4) 0.8344(5) 0.050(2) Uani 1 1 d . . . H11 H 0.1024 -0.3333 0.7933 0.080 Uiso 1 1 calc . . . C12 C 0.1066(2) -0.4295(4) 0.8317(5) 0.058(2) Uani 1 1 d . . . H12 H 0.0947 -0.4494 0.7899 0.080 Uiso 1 1 calc . . . C13 C 0.11999(17) -0.4697(4) 0.8927(4) 0.0403(17) Uani 1 1 d . . . C14 C 0.1373(2) -0.4361(4) 0.9535(5) 0.052(2) Uani 1 1 d . . . H14 H 0.1464 -0.4611 0.9958 0.080 Uiso 1 1 calc . . . C15 C 0.1411(2) -0.3669(4) 0.9515(5) 0.0458(18) Uani 1 1 d . . . H15 H 0.1530 -0.3454 0.9923 0.080 Uiso 1 1 calc . . . C16 C 0.0880(2) -0.6475(4) 0.8504(5) 0.049(2) Uani 1 1 d . . . H16 H 0.0698 -0.6678 0.8263 0.080 Uiso 1 1 calc . . . C17 C 0.0904(2) -0.5763(4) 0.8542(6) 0.051(2) Uani 1 1 d . . . H17 H 0.0739 -0.5499 0.8312 0.080 Uiso 1 1 calc . . . C18 C 0.11636(19) -0.5444(3) 0.8908(4) 0.0380(17) Uani 1 1 d . . . C19 C 0.1407(2) -0.5874(4) 0.9258(5) 0.051(2) Uani 1 1 d . . . H19 H 0.1587 -0.5685 0.9523 0.080 Uiso 1 1 calc . . . C20 C 0.1375(2) -0.6563(4) 0.9200(5) 0.0445(19) Uani 1 1 d . . . H20 H 0.1536 -0.6838 0.9435 0.080 Uiso 1 1 calc . . . C21 C 0.08425(18) -0.2372(4) 0.9978(5) 0.0457(18) Uani 1 1 d . . . H21 H 0.1010 -0.2602 1.0247 0.080 Uiso 1 1 calc . . . C22 C 0.0530(2) -0.2324(5) 1.0341(5) 0.054(2) Uani 1 1 d . . . H22 H 0.0495 -0.2525 1.0839 0.080 Uiso 1 1 calc . . . C23 C 0.02850(18) -0.1987(4) 0.9960(4) 0.0380(17) Uani 1 1 d . . . C24 C 0.0350(2) -0.1689(4) 0.9206(5) 0.053(2) Uani 1 1 d . . . H24 H 0.0189 -0.1454 0.8920 0.080 Uiso 1 1 calc . . . C25 C 0.0663(2) -0.1758(4) 0.8906(5) 0.049(2) Uani 1 1 d . . . H25 H 0.0708 -0.1552 0.8416 0.080 Uiso 1 1 calc . . . C26 C 0.0751(2) -0.0076(5) 0.4946(5) 0.056(2) Uani 1 1 d . . . H26 H 0.0921 -0.0218 0.4620 0.080 Uiso 1 1 calc . . . C27 C 0.0435(2) -0.0141(5) 0.4657(5) 0.057(2) Uani 1 1 d . . . H27 H 0.0397 -0.0306 0.4139 0.080 Uiso 1 1 calc . . . C28 C 0.0174(2) 0.0037(4) 0.5135(5) 0.0387(16) Uani 1 1 d . . . C29 C 0.0256(2) 0.0273(5) 0.5888(5) 0.051(2) Uani 1 1 d . . . H29 H 0.0092 0.0389 0.6246 0.080 Uiso 1 1 calc . . . C30 C 0.0571(2) 0.0336(5) 0.6111(5) 0.056(2) Uani 1 1 d . . . H30 H 0.0615 0.0507 0.6623 0.080 Uiso 1 1 calc . . . C31 C 0.0404(2) 0.1978(5) 0.8574(5) 0.052(2) Uani 1 1 d . . . H31 H 0.0430 0.1971 0.8020 0.080 Uiso 1 1 calc . . . C32 C 0.0093(2) 0.1956(5) 0.8881(5) 0.057(2) Uani 1 1 d . . . H32 H -0.0086 0.1935 0.8531 0.080 Uiso 1 1 calc . . . C33 C 0.0043(2) 0.1966(4) 0.9691(5) 0.042(2) Uani 1 1 d . . . C34 C 0.0325(2) 0.1989(6) 1.0176(5) 0.064(3) Uani 1 1 d . . . H34 H 0.0309 0.1984 1.0733 0.080 Uiso 1 1 calc . . . C35 C 0.0623(2) 0.2018(6) 0.9826(5) 0.063(2) Uani 1 1 d . . . H35 H 0.0806 0.2047 1.0162 0.080 Uiso 1 1 calc . . . C36 C 0.17018(18) -0.0359(4) 0.7109(4) 0.0388(16) Uani 1 1 d . . . H36A H 0.1758 -0.0510 0.7648 0.080 Uiso 1 1 calc . . . H36B H 0.1780 -0.0700 0.6733 0.080 Uiso 1 1 calc . . . C37 C 0.18641(17) 0.0313(4) 0.6946(4) 0.0401(16) Uani 1 1 d . . . H37A H 0.1797 0.0647 0.7342 0.080 Uiso 1 1 calc . . . H37B H 0.2100 0.0261 0.6989 0.080 Uiso 1 1 calc . . . C38 C 0.17978(18) 0.1301(4) 0.6023(4) 0.0379(17) Uani 1 1 d . . . H38A H 0.2021 0.1428 0.5896 0.080 Uiso 1 1 calc . . . H38B H 0.1736 0.1535 0.6512 0.080 Uiso 1 1 calc . . . C39 C 0.15681(17) 0.1503(3) 0.5337(4) 0.0322(16) Uani 1 1 d . . . C40 C 0.19690(18) 0.0203(4) 0.5482(5) 0.0435(18) Uani 1 1 d . . . H40A H 0.2068 0.0550 0.5146 0.080 Uiso 1 1 calc . . . H40B H 0.2145 -0.0055 0.5735 0.080 Uiso 1 1 calc . . . C41 C 0.1772(2) -0.0272(5) 0.4956(6) 0.060(2) Uani 1 1 d . . . C42 C 0.11897(17) -0.0964(3) 0.6865(4) 0.0357(16) Uani 1 1 d . . . H42A H 0.1280 -0.1133 0.6367 0.080 Uiso 1 1 calc . . . H42B H 0.0958 -0.0893 0.6770 0.080 Uiso 1 1 calc . . . C43 C 0.12247(16) -0.1531(4) 0.7485(4) 0.0330(16) Uani 1 1 d . . . C44 C 0.1195(2) 0.0041(4) 0.7749(4) 0.0432(18) Uani 1 1 d . . . H44A H 0.1330 -0.0069 0.8214 0.080 Uiso 1 1 calc . . . H44B H 0.0979 -0.0150 0.7839 0.080 Uiso 1 1 calc . . . C45 C 0.11654(16) 0.0816(3) 0.7683(4) 0.0316(15) Uani 1 1 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 0.0294(5) 0.0247(4) 0.0446(5) -0.0022(3) 0.0146(3) -0.0016(3) Cu2 0.0301(5) 0.0246(4) 0.0410(5) 0.0009(3) 0.0127(3) 0.0006(3) Cu3 0.0292(5) 0.0277(4) 0.0346(4) 0.0017(3) 0.0035(3) -0.0028(3) O1 0.039(3) 0.040(3) 0.042(3) 0.007(2) -0.006(2) -0.006(2) O2 0.038(3) 0.038(3) 0.046(3) 0.012(2) 0.004(2) -0.004(2) O3 0.040(3) 0.045(3) 0.066(3) -0.019(2) 0.014(2) -0.011(2) O4 0.113(7) 0.182(11) 0.174(10) -0.138(10) 0.096(7) -0.091(8) O5 0.031(3) 0.028(2) 0.047(3) 0.002(2) 0.009(2) 0.0010(19) O6 0.098(4) 0.025(3) 0.059(3) -0.002(2) 0.005(3) -0.018(3) O7 0.044(3) 0.030(2) 0.041(3) -0.002(2) 0.003(2) 0.004(2) O8 0.043(3) 0.022(2) 0.040(3) -0.0037(19) 0.013(2) 0.0001(19) O9 0.046(3) 0.044(3) 0.044(3) 0.003(2) 0.003(2) 0.009(2) O10 0.064(3) 0.046(3) 0.052(3) 0.001(2) 0.014(3) 0.005(2) O11 0.088(6) 0.124(8) 0.125(7) -0.001(6) -0.002(5) -0.030(5) O12 0.212(15) 0.180(15) 0.144(10) 0.007(10) 0.035(10) -0.046(13) O13 0.200(11) 0.092(6) 0.090(6) 0.012(5) 0.005(6) -0.016(7) N1 0.035(3) 0.035(3) 0.046(3) -0.002(2) 0.015(3) -0.001(3) N2 0.029(3) 0.034(3) 0.041(3) -0.002(3) 0.008(3) -0.002(3) N3 0.025(3) 0.032(3) 0.044(3) 0.003(3) 0.007(3) 0.000(2) N4 0.036(4) 0.032(3) 0.053(3) -0.002(3) 0.012(3) 0.001(3) N5 0.033(3) 0.028(3) 0.040(3) 0.002(2) 0.008(3) -0.001(3) N6 0.027(3) 0.038(3) 0.038(3) 0.001(2) -0.001(3) -0.001(2) N7 0.046(5) 0.033(3) 0.049(4) -0.009(3) 0.022(4) -0.005(3) N8 0.036(3) 0.026(3) 0.036(3) -0.002(2) 0.005(2) 0.000(2) N9 0.035(4) 0.019(3) 0.041(3) -0.003(2) 0.008(2) -0.005(2) C1 0.038(4) 0.039(4) 0.084(5) -0.012(4) 0.024(4) -0.007(3) C2 0.042(5) 0.044(4) 0.080(5) -0.018(4) 0.026(4) -0.001(4) C3 0.028(4) 0.038(4) 0.046(4) -0.001(3) 0.004(3) 0.001(3) C4 0.030(4) 0.037(4) 0.060(4) -0.005(3) 0.013(3) -0.002(3) C5 0.035(4) 0.034(4) 0.054(4) -0.003(3) 0.011(3) 0.007(3) C6 0.040(5) 0.042(4) 0.040(4) -0.005(3) 0.010(3) 0.002(4) C7 0.033(4) 0.046(4) 0.046(4) -0.010(3) 0.010(3) 0.001(3) C8 0.025(4) 0.038(4) 0.046(4) 0.001(3) 0.011(3) 0.003(3) C9 0.040(4) 0.039(4) 0.049(4) -0.009(3) 0.014(3) -0.001(3) C10 0.027(4) 0.041(4) 0.054(4) -0.007(3) 0.011(3) 0.003(3) C11 0.066(5) 0.028(4) 0.055(5) 0.003(3) -0.001(4) -0.009(4) C12 0.081(6) 0.030(4) 0.062(5) -0.001(4) 0.000(4) -0.002(4) C13 0.045(4) 0.030(4) 0.047(4) 0.004(3) 0.006(3) 0.004(3) C14 0.079(6) 0.032(4) 0.046(4) -0.003(3) -0.017(4) -0.003(4) C15 0.059(5) 0.027(4) 0.052(4) -0.002(3) -0.003(4) -0.010(3) C16 0.049(5) 0.030(4) 0.068(5) -0.005(3) 0.010(4) 0.002(4) C17 0.052(5) 0.029(4) 0.073(5) 0.000(4) -0.002(4) 0.007(4) C18 0.051(5) 0.024(3) 0.039(3) -0.002(3) 0.004(3) -0.005(3) C19 0.048(5) 0.037(4) 0.069(5) -0.008(4) -0.015(4) -0.003(4) C20 0.045(5) 0.028(4) 0.060(5) 0.000(3) -0.009(4) -0.004(3) C21 0.031(4) 0.061(5) 0.046(4) 0.011(4) 0.006(3) 0.005(3) C22 0.048(5) 0.070(5) 0.045(4) 0.018(4) 0.019(4) 0.005(4) C23 0.032(4) 0.039(4) 0.043(4) 0.001(3) 0.010(3) 0.004(3) C24 0.037(5) 0.059(5) 0.062(5) 0.022(4) 0.013(4) 0.014(4) C25 0.041(5) 0.056(5) 0.051(4) 0.016(4) 0.019(4) 0.002(4) C26 0.037(7) 0.078(6) 0.052(5) -0.010(4) 0.008(4) -0.004(4) C27 0.031(6) 0.093(7) 0.046(4) -0.021(4) -0.008(4) -0.007(4) C28 0.028(3) 0.039(4) 0.049(4) 0.005(3) 0.001(3) -0.001(3) C29 0.023(6) 0.085(6) 0.046(4) -0.007(4) 0.002(4) 0.000(4) C30 0.044(7) 0.077(6) 0.046(4) -0.012(4) 0.003(4) -0.001(4) C31 0.042(6) 0.069(6) 0.046(4) -0.012(4) 0.006(5) -0.011(4) C32 0.038(5) 0.086(6) 0.049(4) -0.007(4) 0.019(4) -0.008(4) C33 0.036(5) 0.037(4) 0.054(5) -0.008(3) 0.012(5) -0.003(3) C34 0.043(6) 0.105(7) 0.044(4) -0.001(4) 0.016(5) -0.004(5) C35 0.038(5) 0.101(7) 0.050(5) -0.003(5) 0.010(4) -0.001(4) C36 0.035(4) 0.035(4) 0.047(4) 0.006(3) 0.002(3) 0.003(3) C37 0.038(4) 0.039(4) 0.042(4) 0.006(3) -0.005(3) -0.001(3) C38 0.042(4) 0.032(4) 0.040(4) -0.002(3) 0.004(3) -0.009(3) C39 0.033(4) 0.035(4) 0.029(3) -0.001(3) 0.008(3) -0.001(3) C40 0.034(4) 0.044(4) 0.053(4) -0.005(3) 0.013(3) 0.003(3) C41 0.052(5) 0.052(5) 0.075(6) -0.032(4) 0.022(5) -0.012(4) C42 0.046(4) 0.024(3) 0.038(3) -0.003(3) 0.005(3) -0.001(3) C43 0.033(4) 0.031(4) 0.035(4) 0.000(3) 0.006(3) -0.004(3) C44 0.069(5) 0.025(3) 0.036(4) 0.000(3) 0.014(4) 0.001(3) C45 0.031(4) 0.028(3) 0.036(4) 0.004(3) 0.010(3) -0.001(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 O8 1.985(4) . ? Cu1 N7 2.034(6) . ? Cu1 N4 2.039(6) 1_565 ? Cu1 N2 2.057(5) 4_556 ? Cu1 O9 2.333(5) . ? Cu2 O5 1.993(4) . ? Cu2 N5 2.034(5) . ? Cu2 N1 2.048(5) . ? Cu2 N3 2.048(6) . ? Cu2 O2 2.252(5) 6_556 ? Cu3 O1 1.995(5) . ? Cu3 N6 2.003(6) . ? Cu3 N8 2.030(6) . ? Cu3 N9 2.147(5) . ? Cu3 O3 2.218(5) . ? Cu3 O7 2.319(4) . ? O1 C39 1.263(9) . ? O2 C39 1.258(9) . ? O2 Cu2 2.252(5) 6 ? O3 C41 1.251(11) . ? O4 C41 1.241(13) . ? O5 C43 1.269(9) . ? O6 C43 1.226(9) . ? O7 C45 1.252(9) . ? O8 C45 1.257(8) . ? N1 C5 1.320(10) . ? N1 C1 1.329(11) . ? N2 C6 1.315(10) . ? N2 C10 1.339(10) . ? N2 Cu1 2.057(5) 4_546 ? N3 C11 1.309(11) . ? N3 C15 1.357(11) . ? N4 C20 1.342(11) . ? N4 C16 1.359(11) . ? N4 Cu1 2.039(6) 1_545 ? N5 C21 1.315(10) . ? N5 C25 1.317(11) . ? N6 C26 1.318(12) . ? N6 C30 1.325(11) . ? N7 C35 1.322(12) . ? N7 C31 1.334(13) . ? N8 C38 1.471(9) . ? N8 C37 1.476(10) . ? N8 C40 1.518(9) . ? N9 C42 1.472(9) . ? N9 C44 1.492(9) . ? N9 C36 1.500(10) . ? C1 C2 1.374(12) . ? C1 H1 0.9300 . ? C2 C3 1.373(12) . ? C2 H2 0.9300 . ? C3 C4 1.390(11) . ? C3 C8 1.496(10) . ? C4 C5 1.393(11) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.376(11) . ? C6 H6 0.9300 . ? C7 C8 1.402(11) . ? C7 H7 0.9300 . ? C8 C9 1.393(11) . ? C9 C10 1.364(11) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.380(12) . ? C11 H11 0.9300 . ? C12 C13 1.390(13) . ? C12 H12 0.9300 . ? C13 C14 1.392(13) . ? C13 C18 1.467(11) . ? C14 C15 1.363(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.395(12) . ? C16 H16 0.9300 . ? C17 C18 1.368(13) . ? C17 H17 0.9300 . ? C18 C19 1.423(12) . ? C19 C20 1.357(12) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.423(12) . ? C21 H21 0.9300 . ? C22 C23 1.351(13) . ? C22 H22 0.9300 . ? C23 C24 1.413(12) . ? C23 C33 1.470(11) 5_557 ? C24 C25 1.384(12) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.379(15) . ? C26 H26 0.9300 . ? C27 C28 1.385(13) . ? C27 H27 0.9300 . ? C28 C29 1.373(13) . ? C28 C28 1.493(18) 5_556 ? C29 C30 1.342(14) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.380(13) . ? C31 H31 0.9300 . ? C32 C33 1.366(12) . ? C32 H32 0.9300 . ? C33 C34 1.400(15) . ? C33 C23 1.470(11) 5_557 ? C34 C35 1.358(13) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.497(11) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.520(12) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C40 C41 1.503(13) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C42 C43 1.519(10) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C44 C45 1.523(10) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? 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 O8 Cu1 N7 88.5(2) . . ? O8 Cu1 N4 179.0(2) . 1_565 ? N7 Cu1 N4 90.5(2) . 1_565 ? O8 Cu1 N2 92.3(2) . 4_556 ? N7 Cu1 N2 179.2(2) . 4_556 ? N4 Cu1 N2 88.7(2) 1_565 4_556 ? O8 Cu1 O9 85.62(19) . . ? N7 Cu1 O9 90.6(3) . . ? N4 Cu1 O9 94.5(2) 1_565 . ? N2 Cu1 O9 89.3(2) 4_556 . ? O5 Cu2 N5 92.2(2) . . ? O5 Cu2 N1 87.8(2) . . ? N5 Cu2 N1 178.9(3) . . ? O5 Cu2 N3 152.6(2) . . ? N5 Cu2 N3 88.7(2) . . ? N1 Cu2 N3 91.8(2) . . ? O5 Cu2 O2 108.5(2) . 6_556 ? N5 Cu2 O2 93.9(2) . 6_556 ? N1 Cu2 O2 85.0(2) . 6_556 ? N3 Cu2 O2 98.8(2) . 6_556 ? O1 Cu3 N6 92.0(2) . . ? O1 Cu3 N8 80.9(2) . . ? N6 Cu3 N8 172.0(2) . . ? O1 Cu3 N9 163.5(2) . . ? N6 Cu3 N9 101.1(2) . . ? N8 Cu3 N9 86.5(2) . . ? O1 Cu3 O3 94.9(2) . . ? N6 Cu3 O3 94.9(2) . . ? N8 Cu3 O3 82.0(2) . . ? N9 Cu3 O3 93.9(2) . . ? O1 Cu3 O7 91.85(19) . . ? N6 Cu3 O7 95.1(2) . . ? N8 Cu3 O7 88.96(19) . . ? N9 Cu3 O7 77.21(18) . . ? O3 Cu3 O7 167.8(2) . . ? C39 O1 Cu3 113.5(4) . . ? C39 O2 Cu2 119.4(4) . 6 ? C41 O3 Cu3 108.4(5) . . ? C43 O5 Cu2 106.2(4) . . ? C45 O7 Cu3 113.4(4) . . ? C45 O8 Cu1 128.5(4) . . ? C5 N1 C1 117.6(6) . . ? C5 N1 Cu2 118.3(4) . . ? C1 N1 Cu2 124.1(5) . . ? C6 N2 C10 118.0(5) . . ? C6 N2 Cu1 119.6(4) . 4_546 ? C10 N2 Cu1 122.3(5) . 4_546 ? C11 N3 C15 118.1(6) . . ? C11 N3 Cu2 117.7(5) . . ? C15 N3 Cu2 124.1(5) . . ? C20 N4 C16 118.8(6) . . ? C20 N4 Cu1 121.6(5) . 1_545 ? C16 N4 Cu1 119.1(5) . 1_545 ? C21 N5 C25 118.7(6) . . ? C21 N5 Cu2 117.3(5) . . ? C25 N5 Cu2 124.0(4) . . ? C26 N6 C30 115.4(7) . . ? C26 N6 Cu3 120.1(5) . . ? C30 N6 Cu3 124.5(6) . . ? C35 N7 C31 116.5(6) . . ? C35 N7 Cu1 121.6(6) . . ? C31 N7 Cu1 121.8(5) . . ? C38 N8 C37 114.7(5) . . ? C38 N8 C40 109.0(5) . . ? C37 N8 C40 112.4(5) . . ? C38 N8 Cu3 104.7(4) . . ? C37 N8 Cu3 106.4(4) . . ? C40 N8 Cu3 109.2(4) . . ? C42 N9 C44 111.8(5) . . ? C42 N9 C36 110.0(5) . . ? C44 N9 C36 111.2(5) . . ? C42 N9 Cu3 109.6(4) . . ? C44 N9 Cu3 112.2(4) . . ? C36 N9 Cu3 101.6(4) . . ? N1 C1 C2 122.7(7) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 120.3(7) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 117.5(6) . . ? C2 C3 C8 122.2(6) . . ? C4 C3 C8 120.3(6) . . ? C3 C4 C5 118.3(7) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 123.6(6) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N2 C6 C7 123.2(6) . . ? N2 C6 H6 118.4 . . ? C7 C6 H6 118.4 . . ? C6 C7 C8 119.2(7) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C9 C8 C7 117.0(6) . . ? C9 C8 C3 122.3(6) . . ? C7 C8 C3 120.5(7) . . ? C10 C9 C8 119.2(6) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? N2 C10 C9 123.3(7) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N3 C11 C12 123.9(8) . . ? N3 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? C11 C12 C13 118.7(8) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C12 C13 C14 117.2(7) . . ? C12 C13 C18 120.5(7) . . ? C14 C13 C18 122.3(7) . . ? C15 C14 C13 120.4(8) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? N3 C15 C14 121.7(7) . . ? N3 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? N4 C16 C17 119.9(8) . . ? N4 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 121.9(8) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C17 C18 C19 116.6(6) . . ? C17 C18 C13 122.8(7) . . ? C19 C18 C13 120.6(7) . . ? C20 C19 C18 119.4(7) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? N4 C20 C19 123.3(7) . . ? N4 C20 H20 118.3 . . ? C19 C20 H20 118.3 . . ? N5 C21 C22 121.6(7) . . ? N5 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C23 C22 C21 119.8(7) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 118.1(6) . . ? C22 C23 C33 120.3(7) . 5_557 ? C24 C23 C33 121.6(7) . 5_557 ? C25 C24 C23 117.8(8) . . ? C25 C24 H24 121.1 . . ? C23 C24 H24 121.1 . . ? N5 C25 C24 124.0(7) . . ? N5 C25 H25 118.0 . . ? C24 C25 H25 118.0 . . ? N6 C26 C27 123.4(7) . . ? N6 C26 H26 118.3 . . ? C27 C26 H26 118.3 . . ? C26 C27 C28 120.2(8) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 115.4(9) . . ? C29 C28 C28 121.8(8) . 5_556 ? C27 C28 C28 122.8(9) . 5_556 ? C30 C29 C28 120.3(7) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? N6 C30 C29 125.3(7) . . ? N6 C30 H30 117.4 . . ? C29 C30 H30 117.4 . . ? N7 C31 C32 122.6(7) . . ? N7 C31 H31 118.7 . . ? C32 C31 H31 118.7 . . ? C33 C32 C31 120.8(9) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 116.1(7) . . ? C32 C33 C23 122.5(8) . 5_557 ? C34 C33 C23 121.4(7) . 5_557 ? C35 C34 C33 119.4(8) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? N7 C35 C34 124.7(9) . . ? N7 C35 H35 117.7 . . ? C34 C35 H35 117.7 . . ? C37 C36 N9 110.3(6) . . ? C37 C36 H36A 109.6 . . ? N9 C36 H36A 109.6 . . ? C37 C36 H36B 109.6 . . ? N9 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? N8 C37 C36 110.0(6) . . ? N8 C37 H37A 109.7 . . ? C36 C37 H37A 109.7 . . ? N8 C37 H37B 109.7 . . ? C36 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? N8 C38 C39 108.1(6) . . ? N8 C38 H38A 110.1 . . ? C39 C38 H38A 110.1 . . ? N8 C38 H38B 110.1 . . ? C39 C38 H38B 110.1 . . ? H38A C38 H38B 108.4 . . ? O2 C39 O1 123.7(6) . . ? O2 C39 C38 119.4(6) . . ? O1 C39 C38 116.9(6) . . ? C41 C40 N8 114.5(6) . . ? C41 C40 H40A 108.6 . . ? N8 C40 H40A 108.6 . . ? C41 C40 H40B 108.6 . . ? N8 C40 H40B 108.6 . . ? H40A C40 H40B 107.6 . . ? O4 C41 O3 124.2(8) . . ? O4 C41 C40 115.6(7) . . ? O3 C41 C40 120.1(7) . . ? N9 C42 C43 119.6(6) . . ? N9 C42 H42A 107.4 . . ? C43 C42 H42A 107.4 . . ? N9 C42 H42B 107.4 . . ? C43 C42 H42B 107.4 . . ? H42A C42 H42B 106.9 . . ? O6 C43 O5 123.0(6) . . ? O6 C43 C42 118.5(6) . . ? O5 C43 C42 118.4(6) . . ? N9 C44 C45 113.9(5) . . ? N9 C44 H44A 108.8 . . ? C45 C44 H44A 108.8 . . ? N9 C44 H44B 108.8 . . ? C45 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? O7 C45 O8 126.2(6) . . ? O7 C45 C44 119.8(6) . . ? O8 C45 C44 114.0(6) . . ? _diffrn_measured_fraction_theta_max 0.738 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.738 _refine_diff_density_max 0.624 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.057 #==============================================END