data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H31 Cu N8 O2, C2 H3 O2, 6(H2 O)' _chemical_formula_sum 'C40 H46 Cu N8 O10' _chemical_formula_structural 'Cu 2+, 2(C18 H14 N4), 2(C2 H3 O2 -), 6(H2 O)' _chemical_formula_weight 862.39 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-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.513(11) _cell_length_b 13.875(14) _cell_length_c 15.776(16) _cell_angle_alpha 70.98(2) _cell_angle_beta 83.57(2) _cell_angle_gamma 69.665(18) _cell_volume 2040(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 680 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 22.56 _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 0.603 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.897632 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details '(SADABS; bruker, 1996)' _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 'BRUKER CCD AREA-DETECTOR' _diffrn_measurement_method '\F AND \W SCANS' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8480 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.2373 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7168 _reflns_number_gt 3005 _reflns_threshold_expression I>2s\(I) _computing_data_collection 'SMART, BRUKER, 1998' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT, BRUKER 1998' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997A)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997A)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997B)' _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^)+(0.0255P)^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 7168 _refine_ls_number_parameters 580 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.2135 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.947 _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 0.39713(8) 0.30510(6) 0.43560(5) 0.0359(3) Uani 1 1 d . . . C1 C 0.2044(8) 0.5334(6) 0.0136(5) 0.068(2) Uani 1 1 d . . . H1A H 0.1243 0.5917 -0.0003 0.082 Uiso 1 1 calc R . . C2 C 0.2329(10) 0.4592(8) -0.0342(5) 0.082(3) Uani 1 1 d . . . H2A H 0.1731 0.4683 -0.0776 0.098 Uiso 1 1 calc R . . C3 C 0.3468(10) 0.3759(7) -0.0162(5) 0.071(3) Uani 1 1 d . . . H3A H 0.3655 0.3243 -0.0455 0.085 Uiso 1 1 calc R . . C4 C 0.5638(9) 0.2799(6) 0.0701(5) 0.069(2) Uani 1 1 d . . . H4A H 0.5899 0.2275 0.0410 0.083 Uiso 1 1 calc R . . C5 C 0.6460(8) 0.2728(6) 0.1338(5) 0.065(2) Uani 1 1 d . . . H5A H 0.7282 0.2165 0.1473 0.078 Uiso 1 1 calc R . . C6 C 0.6070(8) 0.3510(6) 0.1799(4) 0.053(2) Uani 1 1 d . . . H6A H 0.6638 0.3459 0.2235 0.063 Uiso 1 1 calc R . . C7 C 0.4868(7) 0.4334(5) 0.1607(4) 0.0423(17) Uani 1 1 d . . . C8 C 0.4004(8) 0.4422(6) 0.0942(4) 0.0441(18) Uani 1 1 d . . . C9 C 0.4405(9) 0.3645(6) 0.0472(5) 0.055(2) Uani 1 1 d . . . C10 C 0.4437(6) 0.5167(5) 0.2092(4) 0.0439(18) Uani 1 1 d . . . H10A H 0.4467 0.5850 0.1675 0.053 Uiso 1 1 calc R . . H10B H 0.3503 0.5266 0.2282 0.053 Uiso 1 1 calc R . . C11 C 0.6225(6) 0.5300(5) 0.2949(5) 0.0486(19) Uani 1 1 d . . . H11A H 0.6519 0.5801 0.2495 0.058 Uiso 1 1 calc R . . C12 C 0.6699(6) 0.4843(5) 0.3796(5) 0.0464(19) Uani 1 1 d . . . H12A H 0.7366 0.4966 0.4045 0.056 Uiso 1 1 calc R . . C13 C 0.5980(6) 0.4150(5) 0.4217(4) 0.0354(16) Uani 1 1 d . . . C14 C 0.6016(6) 0.3457(5) 0.5137(4) 0.0341(16) Uani 1 1 d . . . C15 C 0.6811(6) 0.3446(5) 0.5785(5) 0.0421(17) Uani 1 1 d . . . H15A H 0.7347 0.3888 0.5640 0.051 Uiso 1 1 calc R . . C16 C 0.6801(7) 0.2779(6) 0.6642(5) 0.051(2) Uani 1 1 d . . . H16A H 0.7344 0.2758 0.7079 0.061 Uiso 1 1 calc R . . C17 C 0.6001(7) 0.2146(5) 0.6857(4) 0.0486(19) Uani 1 1 d . . . H17A H 0.5970 0.1700 0.7440 0.058 Uiso 1 1 calc R . . C18 C 0.5227(6) 0.2188(5) 0.6174(4) 0.0402(17) Uani 1 1 d . . . H18A H 0.4686 0.1751 0.6311 0.048 Uiso 1 1 calc R . . C19 C 0.8957(7) -0.0155(5) 0.7111(5) 0.054(2) Uani 1 1 d . . . H19A H 0.8784 -0.0624 0.7650 0.065 Uiso 1 1 calc R . . C20 C 0.9930(7) 0.0325(6) 0.7117(5) 0.059(2) Uani 1 1 d . . . H20A H 1.0392 0.0169 0.7641 0.071 Uiso 1 1 calc R . . C21 C 1.0177(6) 0.1014(5) 0.6349(5) 0.0503(19) Uani 1 1 d . . . H21A H 1.0804 0.1352 0.6342 0.060 Uiso 1 1 calc R . . C22 C 0.9734(6) 0.1914(5) 0.4723(5) 0.0464(18) Uani 1 1 d . . . H22A H 1.0378 0.2249 0.4676 0.056 Uiso 1 1 calc R . . C23 C 0.9028(6) 0.2091(5) 0.3983(4) 0.0474(19) Uani 1 1 d . . . H23A H 0.9181 0.2554 0.3434 0.057 Uiso 1 1 calc R . . C24 C 0.8063(6) 0.1572(5) 0.4051(4) 0.0391(17) Uani 1 1 d . . . H24A H 0.7583 0.1696 0.3544 0.047 Uiso 1 1 calc R . . C25 C 0.7829(6) 0.0899(4) 0.4842(4) 0.0307(15) Uani 1 1 d . . . C26 C 0.8538(6) 0.0705(5) 0.5625(4) 0.0340(16) Uani 1 1 d . . . C27 C 0.9498(6) 0.1231(5) 0.5554(5) 0.0390(17) Uani 1 1 d . . . C28 C 0.6806(6) 0.0330(4) 0.4953(4) 0.0362(16) Uani 1 1 d . . . H28A H 0.7284 -0.0438 0.5078 0.043 Uiso 1 1 calc R . . H28B H 0.6239 0.0434 0.5466 0.043 Uiso 1 1 calc R . . C29 C 0.6038(6) 0.0187(5) 0.3560(4) 0.0382(16) Uani 1 1 d . . . H29A H 0.6695 -0.0463 0.3549 0.046 Uiso 1 1 calc R . . C30 C 0.4998(6) 0.0789(5) 0.2965(4) 0.0368(16) Uani 1 1 d . . . H30A H 0.4801 0.0640 0.2470 0.044 Uiso 1 1 calc R . . C31 C 0.4301(6) 0.1671(5) 0.3256(4) 0.0317(16) Uani 1 1 d . . . C32 C 0.3077(6) 0.2579(5) 0.2925(4) 0.0288(15) Uani 1 1 d . . . C33 C 0.2277(6) 0.2664(5) 0.2249(4) 0.0400(17) Uani 1 1 d . . . H33A H 0.2521 0.2135 0.1963 0.048 Uiso 1 1 calc R . . C34 C 0.1126(7) 0.3533(6) 0.2008(4) 0.0476(19) Uani 1 1 d . . . H34A H 0.0577 0.3601 0.1554 0.057 Uiso 1 1 calc R . . C35 C 0.0777(6) 0.4302(5) 0.2426(4) 0.0469(18) Uani 1 1 d . . . H35A H -0.0004 0.4901 0.2265 0.056 Uiso 1 1 calc R . . C36 C 0.1612(6) 0.4172(5) 0.3098(4) 0.0432(18) Uani 1 1 d . . . H36A H 0.1382 0.4700 0.3383 0.052 Uiso 1 1 calc R . . C37 C 0.1951(6) 0.3308(6) 0.5469(4) 0.0395(17) Uani 1 1 d . . . C38 C 0.0765(7) 0.3734(5) 0.6028(4) 0.064(2) Uani 1 1 d . . . H38A H 0.0486 0.3146 0.6413 0.096 Uiso 1 1 calc R . . H38B H 0.0026 0.4249 0.5642 0.096 Uiso 1 1 calc R . . H38C H 0.1025 0.4077 0.6386 0.096 Uiso 1 1 calc R . . C39 C 0.7647(9) 0.7624(6) 0.1596(4) 0.0483(19) Uani 1 1 d . . . C40 C 0.7663(8) 0.8676(6) 0.1666(5) 0.096(3) Uani 1 1 d . . . H40A H 0.8581 0.8675 0.1628 0.144 Uiso 1 1 calc R . . H40B H 0.7280 0.8760 0.2230 0.144 Uiso 1 1 calc R . . H40C H 0.7139 0.9263 0.1186 0.144 Uiso 1 1 calc R . . N1 N 0.2815(6) 0.5274(5) 0.0766(4) 0.0532(16) Uani 1 1 d . . . N2 N 0.5252(5) 0.4907(4) 0.2870(3) 0.0394(14) Uani 1 1 d . . . N3 N 0.5099(5) 0.4174(4) 0.3648(3) 0.0367(13) Uani 1 1 d . . . N4 N 0.5226(5) 0.2827(4) 0.5332(3) 0.0340(13) Uani 1 1 d . . . N5 N 0.8272(5) 0.0010(4) 0.6400(4) 0.0419(14) Uani 1 1 d . . . N6 N 0.5941(5) 0.0705(4) 0.4171(3) 0.0311(12) Uani 1 1 d . . . N7 N 0.4882(5) 0.1639(4) 0.3986(3) 0.0317(12) Uani 1 1 d . . . N8 N 0.2737(5) 0.3323(4) 0.3356(3) 0.0310(13) Uani 1 1 d . . . O1 O 0.2417(4) 0.3991(3) 0.4926(3) 0.0435(12) Uani 1 1 d . . . O1W O 0.1167(6) 0.2294(5) 0.0447(5) 0.0764(16) Uani 1 1 d D . . O2 O 0.2403(4) 0.2333(4) 0.5550(3) 0.0579(14) Uani 1 1 d . . . O2W O 0.9757(8) 0.0851(5) 0.0718(4) 0.0841(17) Uani 1 1 d D . . O3 O 0.6518(5) 0.7507(4) 0.1628(3) 0.0710(16) Uani 1 1 d . . . O3W O 0.4314(5) 0.8880(5) 0.0689(5) 0.0691(15) Uani 1 1 d D . . O4 O 0.8726(5) 0.6925(4) 0.1499(3) 0.0690(15) Uani 1 1 d . . . O4W O 0.1282(7) 0.6900(5) 0.1660(4) 0.0724(16) Uani 1 1 d D . . O5W O 0.3858(7) 0.0897(6) 0.0876(4) 0.0759(16) Uani 1 1 d D . . O6W O 0.1698(6) 0.8819(5) 0.0808(4) 0.0870(18) Uani 1 1 d D . . H2WA H 0.925(5) 0.102(4) 0.030(3) 0.08(3) Uiso 1 1 d D . . H3WA H 0.483(6) 0.853(6) 0.111(3) 0.11(4) Uiso 1 1 d D . . H1WB H 0.062(5) 0.197(5) 0.060(3) 0.05(3) Uiso 1 1 d D . . H6WB H 0.243(3) 0.887(4) 0.088(4) 0.07(3) Uiso 1 1 d D . . H1WA H 0.126(8) 0.247(7) -0.0099(11) 0.16(5) Uiso 1 1 d D . . H4WB H 0.0462(16) 0.701(7) 0.166(6) 0.16(5) Uiso 1 1 d D . . H4WA H 0.168(6) 0.647(5) 0.138(4) 0.09(4) Uiso 1 1 d D . . H6WA H 0.162(5) 0.824(3) 0.112(4) 0.06(3) Uiso 1 1 d D . . H5WA H 0.307(4) 0.126(6) 0.072(7) 0.21(7) Uiso 1 1 d D . . H5WB H 0.408(7) 0.031(3) 0.079(5) 0.11(4) Uiso 1 1 d D . . H3WB H 0.471(6) 0.885(7) 0.021(2) 0.16(5) Uiso 1 1 d D . . H2WB H 1.043(4) 0.033(3) 0.070(4) 0.05(3) Uiso 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 0.0286(5) 0.0381(5) 0.0415(5) -0.0184(4) -0.0015(4) -0.0055(4) C1 0.070(6) 0.069(6) 0.056(6) 0.000(5) -0.012(5) -0.027(5) C2 0.116(9) 0.086(8) 0.054(6) -0.008(5) -0.023(6) -0.052(7) C3 0.124(9) 0.075(7) 0.033(5) -0.012(5) 0.002(5) -0.061(6) C4 0.097(7) 0.056(6) 0.071(6) -0.033(5) 0.031(5) -0.043(6) C5 0.059(6) 0.048(5) 0.082(6) -0.023(5) 0.015(5) -0.010(4) C6 0.070(6) 0.039(5) 0.054(5) -0.015(4) 0.007(4) -0.024(5) C7 0.052(5) 0.031(5) 0.039(4) -0.005(3) 0.009(4) -0.016(4) C8 0.055(5) 0.048(5) 0.039(4) -0.012(4) 0.015(4) -0.035(5) C9 0.076(6) 0.045(5) 0.049(5) -0.018(4) 0.019(5) -0.030(5) C10 0.052(5) 0.033(4) 0.040(4) -0.007(3) 0.000(4) -0.011(4) C11 0.039(5) 0.045(5) 0.064(5) -0.013(4) 0.010(4) -0.023(4) C12 0.043(5) 0.040(5) 0.060(5) -0.013(4) -0.004(4) -0.019(4) C13 0.035(4) 0.034(4) 0.039(4) -0.014(3) 0.000(3) -0.013(3) C14 0.026(4) 0.032(4) 0.048(5) -0.022(3) 0.005(3) -0.007(3) C15 0.034(4) 0.046(5) 0.054(5) -0.025(4) -0.005(4) -0.011(4) C16 0.034(5) 0.072(6) 0.052(5) -0.039(4) -0.004(4) -0.006(4) C17 0.044(5) 0.061(5) 0.030(4) -0.015(4) -0.009(4) 0.000(4) C18 0.037(4) 0.044(5) 0.040(4) -0.014(4) 0.007(3) -0.015(4) C19 0.059(5) 0.048(5) 0.050(5) -0.010(4) 0.003(4) -0.017(4) C20 0.060(6) 0.061(6) 0.055(5) -0.023(4) -0.014(4) -0.010(5) C21 0.027(4) 0.048(5) 0.080(6) -0.031(4) -0.002(4) -0.005(4) C22 0.033(4) 0.044(5) 0.068(5) -0.021(4) 0.005(4) -0.019(4) C23 0.042(5) 0.037(5) 0.051(5) 0.002(3) -0.001(4) -0.012(4) C24 0.031(4) 0.041(4) 0.036(4) -0.005(3) 0.001(3) -0.006(4) C25 0.024(4) 0.028(4) 0.037(4) -0.010(3) -0.001(3) -0.004(3) C26 0.018(4) 0.034(4) 0.048(5) -0.019(3) -0.002(3) 0.001(3) C27 0.026(4) 0.042(5) 0.048(5) -0.023(4) -0.005(4) 0.001(4) C28 0.029(4) 0.032(4) 0.041(4) -0.005(3) -0.007(3) -0.006(3) C29 0.028(4) 0.031(4) 0.057(5) -0.026(4) -0.001(4) 0.000(3) C30 0.031(4) 0.038(4) 0.044(4) -0.020(3) 0.004(3) -0.008(4) C31 0.031(4) 0.031(4) 0.034(4) -0.010(3) -0.007(3) -0.011(4) C32 0.030(4) 0.026(4) 0.030(4) -0.008(3) 0.003(3) -0.011(3) C33 0.044(5) 0.037(4) 0.042(4) -0.018(3) 0.002(4) -0.012(4) C34 0.037(5) 0.052(5) 0.051(5) -0.016(4) -0.014(4) -0.007(4) C35 0.031(4) 0.041(5) 0.055(5) -0.008(4) -0.011(4) 0.001(4) C36 0.030(4) 0.038(5) 0.051(5) -0.014(3) -0.003(4) 0.002(4) C37 0.028(4) 0.058(6) 0.039(4) -0.019(4) -0.001(3) -0.018(4) C38 0.056(5) 0.058(5) 0.061(5) -0.020(4) 0.018(4) -0.003(4) C39 0.060(6) 0.032(5) 0.041(4) 0.002(4) -0.011(4) -0.010(5) C40 0.094(7) 0.070(6) 0.130(7) -0.044(5) -0.006(6) -0.023(6) N1 0.055(4) 0.054(4) 0.047(4) -0.005(3) 0.000(3) -0.022(4) N2 0.039(4) 0.037(4) 0.042(4) -0.015(3) 0.000(3) -0.011(3) N3 0.041(4) 0.036(3) 0.036(3) -0.016(3) 0.002(3) -0.013(3) N4 0.030(3) 0.033(3) 0.038(4) -0.010(3) 0.001(3) -0.010(3) N5 0.038(4) 0.045(4) 0.039(4) -0.009(3) -0.006(3) -0.011(3) N6 0.020(3) 0.030(3) 0.041(3) -0.014(3) -0.004(3) -0.002(3) N7 0.023(3) 0.026(3) 0.044(3) -0.016(2) 0.004(3) -0.003(3) N8 0.030(3) 0.027(3) 0.031(3) -0.010(3) -0.004(3) -0.002(3) O1 0.048(3) 0.050(3) 0.035(3) -0.017(2) 0.007(2) -0.018(3) O1W 0.080(5) 0.085(5) 0.070(5) -0.026(3) 0.001(3) -0.032(4) O2 0.039(3) 0.043(3) 0.090(4) -0.029(3) 0.000(3) -0.004(3) O2W 0.083(5) 0.081(5) 0.078(5) -0.025(4) -0.020(4) -0.008(4) O3 0.049(4) 0.060(4) 0.095(4) -0.008(3) -0.002(3) -0.021(3) O3W 0.062(4) 0.076(4) 0.069(4) -0.025(4) 0.002(4) -0.021(3) O4 0.048(4) 0.053(4) 0.095(4) -0.025(3) -0.012(3) 0.002(3) O4W 0.056(4) 0.060(4) 0.098(5) -0.029(4) -0.011(4) -0.008(3) O5W 0.083(5) 0.063(4) 0.084(4) -0.035(4) -0.003(4) -0.016(4) O6W 0.061(5) 0.067(5) 0.121(5) -0.008(4) -0.018(4) -0.022(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 N8 2.012(4) . ? Cu1 N4 2.016(5) . ? Cu1 O1 2.033(4) . ? Cu1 N7 2.101(5) . ? Cu1 N3 2.221(5) . ? C1 N1 1.316(7) . ? C1 C2 1.399(10) . ? C1 H1A 0.9300 . ? C2 C3 1.323(10) . ? C2 H2A 0.9300 . ? C3 C9 1.415(9) . ? C3 H3A 0.9300 . ? C4 C5 1.354(8) . ? C4 C9 1.401(9) . ? C4 H4A 0.9300 . ? C5 C6 1.420(8) . ? C5 H5A 0.9300 . ? C6 C7 1.361(8) . ? C6 H6A 0.9300 . ? C7 C8 1.413(8) . ? C7 C10 1.504(8) . ? C8 N1 1.369(8) . ? C8 C9 1.423(8) . ? C10 N2 1.449(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.348(7) . ? C11 N2 1.349(7) . ? C11 H11A 0.9300 . ? C12 C13 1.384(7) . ? C12 H12A 0.9300 . ? C13 N3 1.344(6) . ? C13 C14 1.452(8) . ? C14 N4 1.349(7) . ? C14 C15 1.386(7) . ? C15 C16 1.369(8) . ? C15 H15A 0.9300 . ? C16 C17 1.359(8) . ? C16 H16A 0.9300 . ? C17 C18 1.397(7) . ? C17 H17A 0.9300 . ? C18 N4 1.334(6) . ? C18 H18A 0.9300 . ? C19 N5 1.314(7) . ? C19 C20 1.403(8) . ? C19 H19A 0.9300 . ? C20 C21 1.340(8) . ? C20 H20A 0.9300 . ? C21 C27 1.407(7) . ? C21 H21A 0.9300 . ? C22 C23 1.362(7) . ? C22 C27 1.400(8) . ? C22 H22A 0.9300 . ? C23 C24 1.411(7) . ? C23 H23A 0.9300 . ? C24 C25 1.350(7) . ? C24 H24A 0.9300 . ? C25 C26 1.416(7) . ? C25 C28 1.506(7) . ? C26 N5 1.359(7) . ? C26 C27 1.413(8) . ? C28 N6 1.456(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N6 1.355(6) . ? C29 C30 1.363(7) . ? C29 H29A 0.9300 . ? C30 C31 1.384(7) . ? C30 H30A 0.9300 . ? C31 N7 1.343(6) . ? C31 C32 1.453(7) . ? C32 N8 1.342(6) . ? C32 C33 1.382(7) . ? C33 C34 1.362(8) . ? C33 H33A 0.9300 . ? C34 C35 1.358(8) . ? C34 H34A 0.9300 . ? C35 C36 1.378(7) . ? C35 H35A 0.9300 . ? C36 N8 1.334(6) . ? C36 H36A 0.9300 . ? C37 O2 1.235(7) . ? C37 O1 1.253(7) . ? C37 C38 1.505(8) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 O4 1.243(8) . ? C39 O3 1.246(7) . ? C39 C40 1.506(9) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? N2 N3 1.351(6) . ? N6 N7 1.352(6) . ? O1W H1WB 0.819(10) . ? O1W H1WA 0.820(10) . ? O2W H2WA 0.823(10) . ? O2W H2WB 0.823(10) . ? O3W H3WA 0.818(10) . ? O3W H3WB 0.820(10) . ? O4W H4WB 0.820(10) . ? O4W H4WA 0.822(10) . ? O5W H5WA 0.819(10) . ? O5W H5WB 0.821(10) . ? O6W H6WB 0.816(10) . ? O6W H6WA 0.819(10) . ? 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 N8 Cu1 N4 177.9(2) . . ? N8 Cu1 O1 90.16(19) . . ? N4 Cu1 O1 89.83(18) . . ? N8 Cu1 N7 79.1(2) . . ? N4 Cu1 N7 101.91(19) . . ? O1 Cu1 N7 150.47(17) . . ? N8 Cu1 N3 99.31(19) . . ? N4 Cu1 N3 78.6(2) . . ? O1 Cu1 N3 102.17(19) . . ? N7 Cu1 N3 106.64(19) . . ? N1 C1 C2 125.4(8) . . ? N1 C1 H1A 117.3 . . ? C2 C1 H1A 117.3 . . ? C3 C2 C1 118.5(8) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C9 120.8(8) . . ? C2 C3 H3A 119.6 . . ? C9 C3 H3A 119.6 . . ? C5 C4 C9 121.4(7) . . ? C5 C4 H4A 119.3 . . ? C9 C4 H4A 119.3 . . ? C4 C5 C6 120.1(7) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C7 C6 C5 120.3(7) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C8 120.2(7) . . ? C6 C7 C10 121.0(6) . . ? C8 C7 C10 118.8(6) . . ? N1 C8 C7 117.9(7) . . ? N1 C8 C9 122.7(7) . . ? C7 C8 C9 119.4(7) . . ? C4 C9 C3 125.0(8) . . ? C4 C9 C8 118.5(7) . . ? C3 C9 C8 116.4(8) . . ? N2 C10 C7 114.9(5) . . ? N2 C10 H10A 108.5 . . ? C7 C10 H10A 108.5 . . ? N2 C10 H10B 108.5 . . ? C7 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C12 C11 N2 108.3(6) . . ? C12 C11 H11A 125.8 . . ? N2 C11 H11A 125.8 . . ? C11 C12 C13 105.2(6) . . ? C11 C12 H12A 127.4 . . ? C13 C12 H12A 127.4 . . ? N3 C13 C12 111.1(5) . . ? N3 C13 C14 118.0(6) . . ? C12 C13 C14 130.9(6) . . ? N4 C14 C15 121.5(6) . . ? N4 C14 C13 116.6(6) . . ? C15 C14 C13 121.9(6) . . ? C16 C15 C14 119.3(6) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C17 C16 C15 120.3(6) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C18 117.7(6) . . ? C16 C17 H17A 121.1 . . ? C18 C17 H17A 121.1 . . ? N4 C18 C17 123.1(6) . . ? N4 C18 H18A 118.4 . . ? C17 C18 H18A 118.4 . . ? N5 C19 C20 124.8(7) . . ? N5 C19 H19A 117.6 . . ? C20 C19 H19A 117.6 . . ? C21 C20 C19 118.3(6) . . ? C21 C20 H20A 120.8 . . ? C19 C20 H20A 120.8 . . ? C20 C21 C27 120.7(6) . . ? C20 C21 H21A 119.7 . . ? C27 C21 H21A 119.7 . . ? C23 C22 C27 120.5(6) . . ? C23 C22 H22A 119.8 . . ? C27 C22 H22A 119.8 . . ? C22 C23 C24 119.8(6) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C25 C24 C23 120.9(6) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C24 C25 C26 120.7(6) . . ? C24 C25 C28 123.0(5) . . ? C26 C25 C28 116.3(5) . . ? N5 C26 C27 123.7(6) . . ? N5 C26 C25 118.1(6) . . ? C27 C26 C25 118.2(6) . . ? C22 C27 C21 123.8(7) . . ? C22 C27 C26 120.0(6) . . ? C21 C27 C26 116.2(6) . . ? N6 C28 C25 113.8(4) . . ? N6 C28 H28A 108.8 . . ? C25 C28 H28A 108.8 . . ? N6 C28 H28B 108.8 . . ? C25 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? N6 C29 C30 107.7(6) . . ? N6 C29 H29A 126.2 . . ? C30 C29 H29A 126.2 . . ? C29 C30 C31 104.9(5) . . ? C29 C30 H30A 127.5 . . ? C31 C30 H30A 127.5 . . ? N7 C31 C30 111.7(5) . . ? N7 C31 C32 116.7(6) . . ? C30 C31 C32 131.5(6) . . ? N8 C32 C33 121.7(5) . . ? N8 C32 C31 114.7(5) . . ? C33 C32 C31 123.6(6) . . ? C34 C33 C32 118.9(6) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C35 C34 C33 120.2(6) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C36 118.3(6) . . ? C34 C35 H35A 120.9 . . ? C36 C35 H35A 120.9 . . ? N8 C36 C35 122.8(6) . . ? N8 C36 H36A 118.6 . . ? C35 C36 H36A 118.6 . . ? O2 C37 O1 123.5(7) . . ? O2 C37 C38 120.0(7) . . ? O1 C37 C38 116.5(7) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O4 C39 O3 123.0(7) . . ? O4 C39 C40 120.1(7) . . ? O3 C39 C40 117.0(7) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C1 N1 C8 116.1(6) . . ? N3 N2 C11 110.6(5) . . ? N3 N2 C10 120.7(5) . . ? C11 N2 C10 128.7(6) . . ? C13 N3 N2 104.8(5) . . ? C13 N3 Cu1 109.6(4) . . ? N2 N3 Cu1 145.6(4) . . ? C18 N4 C14 118.1(5) . . ? C18 N4 Cu1 124.7(4) . . ? C14 N4 Cu1 116.8(4) . . ? C19 N5 C26 116.3(5) . . ? N7 N6 C29 111.1(5) . . ? N7 N6 C28 122.2(5) . . ? C29 N6 C28 126.6(5) . . ? C31 N7 N6 104.6(4) . . ? C31 N7 Cu1 112.4(4) . . ? N6 N7 Cu1 142.8(4) . . ? C36 N8 C32 118.1(5) . . ? C36 N8 Cu1 125.2(4) . . ? C32 N8 Cu1 116.7(4) . . ? C37 O1 Cu1 102.1(4) . . ? H1WB O1W H1WA 110.8(19) . . ? H2WA O2W H2WB 109.9(19) . . ? H3WA O3W H3WB 111.0(19) . . ? H4WB O4W H4WA 110.5(19) . . ? H5WA O5W H5WB 111.0(19) . . ? H6WB O6W H6WA 111.8(19) . . ? 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 N1 C1 C2 C3 -0.6(13) . . . . ? C1 C2 C3 C9 -2.6(12) . . . . ? C9 C4 C5 C6 1.0(11) . . . . ? C4 C5 C6 C7 0.1(10) . . . . ? C5 C6 C7 C8 -0.4(10) . . . . ? C5 C6 C7 C10 179.7(6) . . . . ? C6 C7 C8 N1 -179.1(6) . . . . ? C10 C7 C8 N1 0.7(8) . . . . ? C6 C7 C8 C9 -0.4(9) . . . . ? C10 C7 C8 C9 179.4(5) . . . . ? C5 C4 C9 C3 -177.8(7) . . . . ? C5 C4 C9 C8 -1.8(10) . . . . ? C2 C3 C9 C4 -179.5(8) . . . . ? C2 C3 C9 C8 4.5(11) . . . . ? N1 C8 C9 C4 -179.8(6) . . . . ? C7 C8 C9 C4 1.5(9) . . . . ? N1 C8 C9 C3 -3.6(9) . . . . ? C7 C8 C9 C3 177.8(6) . . . . ? C6 C7 C10 N2 -11.1(8) . . . . ? C8 C7 C10 N2 169.0(5) . . . . ? N2 C11 C12 C13 0.7(7) . . . . ? C11 C12 C13 N3 0.3(7) . . . . ? C11 C12 C13 C14 -178.3(6) . . . . ? N3 C13 C14 N4 4.8(8) . . . . ? C12 C13 C14 N4 -176.7(6) . . . . ? N3 C13 C14 C15 -174.7(5) . . . . ? C12 C13 C14 C15 3.8(10) . . . . ? N4 C14 C15 C16 0.3(9) . . . . ? C13 C14 C15 C16 179.8(6) . . . . ? C14 C15 C16 C17 -1.1(10) . . . . ? C15 C16 C17 C18 1.4(10) . . . . ? C16 C17 C18 N4 -0.9(9) . . . . ? N5 C19 C20 C21 0.9(11) . . . . ? C19 C20 C21 C27 -1.4(10) . . . . ? C27 C22 C23 C24 -0.8(9) . . . . ? C22 C23 C24 C25 0.0(9) . . . . ? C23 C24 C25 C26 0.6(9) . . . . ? C23 C24 C25 C28 179.6(5) . . . . ? C24 C25 C26 N5 -179.3(5) . . . . ? C28 C25 C26 N5 1.7(8) . . . . ? C24 C25 C26 C27 -0.3(8) . . . . ? C28 C25 C26 C27 -179.4(5) . . . . ? C23 C22 C27 C21 -179.5(6) . . . . ? C23 C22 C27 C26 1.1(9) . . . . ? C20 C21 C27 C22 -178.0(6) . . . . ? C20 C21 C27 C26 1.5(9) . . . . ? N5 C26 C27 C22 178.4(6) . . . . ? C25 C26 C27 C22 -0.5(8) . . . . ? N5 C26 C27 C21 -1.1(9) . . . . ? C25 C26 C27 C21 180.0(5) . . . . ? C24 C25 C28 N6 -9.5(8) . . . . ? C26 C25 C28 N6 169.6(5) . . . . ? N6 C29 C30 C31 0.0(6) . . . . ? C29 C30 C31 N7 1.1(7) . . . . ? C29 C30 C31 C32 -177.5(6) . . . . ? N7 C31 C32 N8 5.0(7) . . . . ? C30 C31 C32 N8 -176.4(6) . . . . ? N7 C31 C32 C33 -172.3(5) . . . . ? C30 C31 C32 C33 6.3(10) . . . . ? N8 C32 C33 C34 0.9(9) . . . . ? C31 C32 C33 C34 178.0(6) . . . . ? C32 C33 C34 C35 0.1(10) . . . . ? C33 C34 C35 C36 -0.3(10) . . . . ? C34 C35 C36 N8 -0.5(9) . . . . ? C2 C1 N1 C8 1.5(10) . . . . ? C7 C8 N1 C1 179.3(5) . . . . ? C9 C8 N1 C1 0.7(9) . . . . ? C12 C11 N2 N3 -1.6(7) . . . . ? C12 C11 N2 C10 179.1(5) . . . . ? C7 C10 N2 N3 -76.5(7) . . . . ? C7 C10 N2 C11 102.8(7) . . . . ? C12 C13 N3 N2 -1.2(7) . . . . ? C14 C13 N3 N2 177.6(5) . . . . ? C12 C13 N3 Cu1 -179.9(4) . . . . ? C14 C13 N3 Cu1 -1.2(6) . . . . ? C11 N2 N3 C13 1.7(6) . . . . ? C10 N2 N3 C13 -178.9(5) . . . . ? C11 N2 N3 Cu1 179.5(5) . . . . ? C10 N2 N3 Cu1 -1.0(9) . . . . ? N8 Cu1 N3 C13 178.0(4) . . . . ? N4 Cu1 N3 C13 -1.5(4) . . . . ? O1 Cu1 N3 C13 85.8(4) . . . . ? N7 Cu1 N3 C13 -100.7(4) . . . . ? N8 Cu1 N3 N2 0.2(7) . . . . ? N4 Cu1 N3 N2 -179.3(7) . . . . ? O1 Cu1 N3 N2 -92.0(7) . . . . ? N7 Cu1 N3 N2 81.5(7) . . . . ? C17 C18 N4 C14 0.2(9) . . . . ? C17 C18 N4 Cu1 -172.5(4) . . . . ? C15 C14 N4 C18 0.1(8) . . . . ? C13 C14 N4 C18 -179.3(5) . . . . ? C15 C14 N4 Cu1 173.3(4) . . . . ? C13 C14 N4 Cu1 -6.1(7) . . . . ? N8 Cu1 N4 C18 164(6) . . . . ? O1 Cu1 N4 C18 74.4(5) . . . . ? N7 Cu1 N4 C18 -78.3(5) . . . . ? N3 Cu1 N4 C18 176.9(5) . . . . ? N8 Cu1 N4 C14 -9(6) . . . . ? O1 Cu1 N4 C14 -98.3(4) . . . . ? N7 Cu1 N4 C14 109.0(4) . . . . ? N3 Cu1 N4 C14 4.2(4) . . . . ? C20 C19 N5 C26 -0.5(9) . . . . ? C27 C26 N5 C19 0.6(9) . . . . ? C25 C26 N5 C19 179.5(5) . . . . ? C30 C29 N6 N7 -1.0(6) . . . . ? C30 C29 N6 C28 177.2(5) . . . . ? C25 C28 N6 N7 -78.0(6) . . . . ? C25 C28 N6 C29 104.1(6) . . . . ? C30 C31 N7 N6 -1.6(6) . . . . ? C32 C31 N7 N6 177.2(5) . . . . ? C30 C31 N7 Cu1 173.6(4) . . . . ? C32 C31 N7 Cu1 -7.5(6) . . . . ? C29 N6 N7 C31 1.6(6) . . . . ? C28 N6 N7 C31 -176.6(4) . . . . ? C29 N6 N7 Cu1 -171.2(5) . . . . ? C28 N6 N7 Cu1 10.6(9) . . . . ? N8 Cu1 N7 C31 5.8(4) . . . . ? N4 Cu1 N7 C31 -172.3(4) . . . . ? O1 Cu1 N7 C31 76.3(5) . . . . ? N3 Cu1 N7 C31 -90.7(4) . . . . ? N8 Cu1 N7 N6 178.3(6) . . . . ? N4 Cu1 N7 N6 0.2(6) . . . . ? O1 Cu1 N7 N6 -111.3(6) . . . . ? N3 Cu1 N7 N6 81.7(6) . . . . ? C35 C36 N8 C32 1.5(9) . . . . ? C35 C36 N8 Cu1 -177.8(4) . . . . ? C33 C32 N8 C36 -1.7(8) . . . . ? C31 C32 N8 C36 -179.0(5) . . . . ? C33 C32 N8 Cu1 177.7(4) . . . . ? C31 C32 N8 Cu1 0.3(6) . . . . ? N4 Cu1 N8 C36 -66(6) . . . . ? O1 Cu1 N8 C36 23.7(5) . . . . ? N7 Cu1 N8 C36 176.0(5) . . . . ? N3 Cu1 N8 C36 -78.7(5) . . . . ? N4 Cu1 N8 C32 115(6) . . . . ? O1 Cu1 N8 C32 -155.6(4) . . . . ? N7 Cu1 N8 C32 -3.3(4) . . . . ? N3 Cu1 N8 C32 102.0(4) . . . . ? O2 C37 O1 Cu1 -1.6(6) . . . . ? C38 C37 O1 Cu1 179.4(4) . . . . ? N8 Cu1 O1 C37 93.6(3) . . . . ? N4 Cu1 O1 C37 -88.5(4) . . . . ? N7 Cu1 O1 C37 25.9(5) . . . . ? N3 Cu1 O1 C37 -166.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.319 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.071 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H39 Cu N10 O11.50' _chemical_formula_weight 860.32 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 'c/2c' 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 12.395(3) _cell_length_b 26.267(6) _cell_length_c 26.362(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.635(5) _cell_angle_gamma 90.00 _cell_volume 8574(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 642 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 22.89 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3576 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.850618 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details '(Bruker sadabs, 1996)' _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 'bruker ccd area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23762 _diffrn_reflns_av_R_equivalents 0.1090 _diffrn_reflns_av_sigmaI/netI 0.1779 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.44 _reflns_number_total 8695 _reflns_number_gt 2604 _reflns_threshold_expression I>2s\(I) _computing_data_collection 'smart, bruker, 1998' _computing_cell_refinement 'smart' _computing_data_reduction 'saint, bruker, 1998' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'shelxtl (sheldrick, 1997)' _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^)+(0.1616P)^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 8695 _refine_ls_number_parameters 528 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2879 _refine_ls_R_factor_gt 0.1122 _refine_ls_wR_factor_ref 0.3422 _refine_ls_wR_factor_gt 0.2531 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.947 _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 -0.10627(8) 0.37824(4) 0.98552(4) 0.0847(5) Uani 1 1 d . . . C1 C -0.1930(9) 0.3048(8) 0.7472(5) 0.124(5) Uani 1 1 d . . . H1A H -0.2378 0.3236 0.7250 0.148 Uiso 1 1 calc R . . C2 C -0.1981(11) 0.2536(9) 0.7429(6) 0.146(6) Uani 1 1 d . . . H2A H -0.2439 0.2386 0.7183 0.175 Uiso 1 1 calc R . . C3 C -0.1326(12) 0.2227(6) 0.7764(5) 0.131(4) Uani 1 1 d . . . H3A H -0.1342 0.1874 0.7752 0.158 Uiso 1 1 calc R . . C4 C -0.0634(8) 0.2506(5) 0.8123(4) 0.091(3) Uani 1 1 d . . . C5 C 0.0045(10) 0.2242(4) 0.8460(5) 0.101(3) Uani 1 1 d . . . H5A H 0.0042 0.1888 0.8459 0.121 Uiso 1 1 calc R . . C6 C 0.0732(8) 0.2503(4) 0.8802(4) 0.093(3) Uani 1 1 d . . . H6A H 0.1205 0.2328 0.9024 0.112 Uiso 1 1 calc R . . C7 C 0.0697(7) 0.3031(4) 0.8804(3) 0.077(2) Uani 1 1 d . . . H7A H 0.1152 0.3210 0.9031 0.093 Uiso 1 1 calc R . . C8 C 0.0001(7) 0.3294(3) 0.8477(3) 0.069(2) Uani 1 1 d . . . C9 C -0.0666(7) 0.3034(5) 0.8121(3) 0.079(3) Uani 1 1 d . . . C10 C -0.0086(7) 0.3863(4) 0.8492(4) 0.087(3) Uani 1 1 d . . . H10A H 0.0171 0.3998 0.8177 0.104 Uiso 1 1 calc R . . H10B H -0.0842 0.3953 0.8507 0.104 Uiso 1 1 calc R . . C11 C 0.1456(8) 0.4354(4) 0.8919(5) 0.093(3) Uani 1 1 d . . . H11A H 0.1866 0.4407 0.8637 0.111 Uiso 1 1 calc R . . C12 C 0.1713(9) 0.4510(4) 0.9390(6) 0.102(3) Uani 1 1 d . . . H12A H 0.2327 0.4688 0.9503 0.123 Uiso 1 1 calc R . . C13 C 0.0872(8) 0.4351(3) 0.9674(4) 0.075(2) Uani 1 1 d . . . C14 C 0.0688(8) 0.4428(3) 1.0207(4) 0.080(3) Uani 1 1 d . . . C15 C 0.1361(9) 0.4706(3) 1.0539(5) 0.098(3) Uani 1 1 d . . . H15A H 0.1994 0.4852 1.0430 0.118 Uiso 1 1 calc R . . C16 C 0.1063(15) 0.4760(5) 1.1038(6) 0.130(5) Uani 1 1 d . . . H16A H 0.1483 0.4960 1.1261 0.156 Uiso 1 1 calc R . . C17 C 0.0179(14) 0.4529(6) 1.1203(5) 0.126(5) Uani 1 1 d . . . H17A H -0.0003 0.4556 1.1540 0.152 Uiso 1 1 calc R . . C18 C -0.0465(10) 0.4244(5) 1.0852(5) 0.114(4) Uani 1 1 d . . . H18A H -0.1095 0.4092 1.0958 0.137 Uiso 1 1 calc R . . C19 C 0.2376(17) 0.3800(7) 1.1854(7) 0.150(5) Uani 1 1 d . . . H19A H 0.2143 0.3816 1.2183 0.180 Uiso 1 1 calc R . . C20 C 0.331(2) 0.4067(9) 1.1747(10) 0.196(12) Uani 1 1 d . . . H20A H 0.3686 0.4254 1.1997 0.236 Uiso 1 1 calc R . . C21 C 0.3644(14) 0.4045(6) 1.1280(10) 0.157(7) Uani 1 1 d . . . H21A H 0.4256 0.4224 1.1193 0.188 Uiso 1 1 calc R . . C22 C 0.3079(12) 0.3756(5) 1.0919(6) 0.113(4) Uani 1 1 d . . . C23 C 0.3402(8) 0.3710(5) 1.0392(8) 0.125(5) Uani 1 1 d . . . H23A H 0.4017 0.3879 1.0292 0.150 Uiso 1 1 calc R . . C24 C 0.2835(10) 0.3435(5) 1.0056(5) 0.118(4) Uani 1 1 d . . . H24A H 0.3057 0.3412 0.9725 0.141 Uiso 1 1 calc R . . C25 C 0.1902(7) 0.3176(4) 1.0194(4) 0.086(3) Uani 1 1 d . . . H25A H 0.1516 0.2976 0.9957 0.103 Uiso 1 1 calc R . . C26 C 0.1563(7) 0.3221(4) 1.0681(4) 0.079(3) Uani 1 1 d . . . C27 C 0.2158(9) 0.3506(4) 1.1046(5) 0.086(3) Uani 1 1 d . . . C28 C 0.0543(7) 0.2964(4) 1.0832(4) 0.088(3) Uani 1 1 d . . . H28A H 0.0729 0.2707 1.1086 0.105 Uiso 1 1 calc R . . H28B H 0.0090 0.3214 1.0989 0.105 Uiso 1 1 calc R . . C29 C -0.0185(9) 0.2225(4) 1.0293(5) 0.092(3) Uani 1 1 d . . . H29A H 0.0145 0.1951 1.0462 0.111 Uiso 1 1 calc R . . C30 C -0.0861(8) 0.2199(4) 0.9877(4) 0.093(3) Uani 1 1 d . . . H30A H -0.1093 0.1906 0.9708 0.111 Uiso 1 1 calc R . . C31 C -0.1133(7) 0.2683(4) 0.9756(3) 0.072(2) Uani 1 1 d . . . C32 C -0.1853(7) 0.2875(4) 0.9361(4) 0.073(2) Uani 1 1 d . . . C33 C -0.2474(8) 0.2573(4) 0.9027(4) 0.091(3) Uani 1 1 d . . . H33A H -0.2419 0.2220 0.9041 0.109 Uiso 1 1 calc R . . C34 C -0.3159(9) 0.2798(7) 0.8679(5) 0.110(4) Uani 1 1 d . . . H34A H -0.3574 0.2599 0.8454 0.132 Uiso 1 1 calc R . . C35 C -0.3244(8) 0.3305(6) 0.8659(4) 0.106(4) Uani 1 1 d . . . H35A H -0.3716 0.3456 0.8419 0.127 Uiso 1 1 calc R . . C36 C -0.2631(7) 0.3608(4) 0.8993(4) 0.096(3) Uani 1 1 d . . . H36A H -0.2697 0.3960 0.8976 0.115 Uiso 1 1 calc R . . N1 N -0.1318(7) 0.3300(4) 0.7792(3) 0.099(3) Uani 1 1 d . . . N2 N 0.0516(6) 0.4108(3) 0.8918(3) 0.0765(19) Uani 1 1 d . . . N3 N 0.0135(6) 0.4101(3) 0.9392(3) 0.0722(19) Uani 1 1 d . . . N4 N -0.0191(7) 0.4186(3) 1.0369(3) 0.080(2) Uani 1 1 d . . . N5 N 0.1801(8) 0.3526(4) 1.1523(5) 0.116(3) Uani 1 1 d . . . N6 N -0.0078(6) 0.2724(3) 1.0419(3) 0.081(2) Uani 1 1 d . . . N7 N -0.0662(6) 0.3016(3) 1.0085(3) 0.0725(18) Uani 1 1 d . . . N8 N -0.1946(5) 0.3397(3) 0.9341(3) 0.0715(19) Uani 1 1 d . . . N9 N -0.2955(11) 0.4100(6) 1.0236(5) 0.175(6) Uani 1 1 d D . . N10 N 0.3970(14) 0.3585(6) 0.8647(7) 0.290(18) Uani 1 1 d D . . O1W O 0.5098(17) 0.1820(10) 0.7974(6) 0.363(13) Uani 1 1 d . . . O1 O -0.2478(11) 0.3718(6) 1.0436(7) 0.265(8) Uani 1 1 d D . . O2W O 0.586(2) 0.0106(8) 0.7551(10) 0.43(2) Uani 1 1 d . . . O2 O -0.2519(11) 0.4341(5) 0.9883(6) 0.221(7) Uani 1 1 d D . . O3 O -0.3854(12) 0.4259(9) 1.0403(10) 0.52(3) Uani 1 1 d D . . O3W O 0.3357(19) 0.5965(14) 0.8451(14) 0.50(2) Uani 1 1 d . . . O4W O 1.0000 0.2048(9) 0.2500 0.280(10) Uani 1 2 d S . . O4 O 0.433(2) 0.3772(7) 0.9074(6) 0.48(3) Uani 1 1 d D . . O5W O 0.7990(15) 0.4321(9) 0.7651(11) 0.457(17) Uani 1 1 d . . . O5 O 0.4020(13) 0.3817(6) 0.8210(6) 0.298(9) Uani 1 1 d D . . O6W O 0.209(4) 0.6174(19) 0.8214(12) 0.70(4) Uani 1 1 d . . . O6 O 0.3760(13) 0.3111(6) 0.8589(6) 0.301(11) 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 0.0732(8) 0.0855(8) 0.0955(9) 0.0031(7) 0.0047(6) 0.0135(6) C1 0.073(8) 0.213(17) 0.083(8) -0.016(10) -0.009(6) 0.016(10) C2 0.088(9) 0.23(2) 0.117(11) -0.059(14) 0.004(8) -0.015(12) C3 0.109(10) 0.165(13) 0.123(10) -0.055(10) 0.044(8) -0.019(10) C4 0.069(6) 0.123(10) 0.082(7) -0.016(7) 0.010(5) 0.013(7) C5 0.130(9) 0.067(6) 0.109(8) -0.012(7) 0.047(8) 0.010(7) C6 0.105(8) 0.082(8) 0.093(7) -0.005(6) 0.009(6) 0.032(6) C7 0.080(6) 0.076(7) 0.076(6) -0.002(5) 0.000(5) 0.012(5) C8 0.062(5) 0.075(6) 0.071(6) 0.008(5) 0.013(5) 0.015(5) C9 0.061(6) 0.105(9) 0.072(6) 0.002(6) 0.011(5) 0.015(6) C10 0.075(6) 0.106(8) 0.080(6) 0.031(6) 0.010(5) 0.030(5) C11 0.066(7) 0.080(7) 0.134(10) 0.019(7) 0.021(6) -0.019(5) C12 0.082(8) 0.076(7) 0.148(11) -0.003(7) -0.011(8) -0.004(6) C13 0.059(6) 0.063(6) 0.102(8) 0.009(6) -0.002(6) 0.012(5) C14 0.070(6) 0.059(6) 0.109(9) 0.014(6) -0.006(6) 0.019(5) C15 0.106(8) 0.058(6) 0.128(10) 0.001(6) -0.032(8) 0.004(6) C16 0.176(15) 0.088(9) 0.119(12) -0.021(8) -0.050(11) 0.055(10) C17 0.161(13) 0.117(11) 0.101(10) -0.014(9) 0.002(10) 0.049(10) C18 0.134(10) 0.117(9) 0.091(8) 0.002(8) 0.012(8) 0.038(8) C19 0.182(17) 0.138(13) 0.126(12) -0.012(11) -0.030(13) 0.043(12) C20 0.20(2) 0.144(16) 0.24(3) -0.052(19) -0.10(2) 0.049(16) C21 0.117(12) 0.099(10) 0.25(2) -0.014(15) -0.049(16) 0.003(8) C22 0.105(10) 0.084(8) 0.148(12) 0.017(9) 0.000(10) 0.027(8) C23 0.050(6) 0.085(8) 0.237(18) 0.055(10) -0.007(9) -0.001(6) C24 0.068(7) 0.131(11) 0.156(11) 0.056(9) 0.026(8) 0.037(7) C25 0.056(6) 0.110(8) 0.093(7) 0.022(6) 0.011(5) 0.017(5) C26 0.065(6) 0.079(6) 0.095(7) 0.037(6) 0.019(6) 0.031(5) C27 0.077(7) 0.081(7) 0.100(9) 0.015(7) -0.009(7) 0.022(6) C28 0.078(6) 0.107(7) 0.079(6) 0.032(6) 0.012(5) 0.029(6) C29 0.093(7) 0.062(7) 0.125(9) 0.022(6) 0.047(7) 0.026(6) C30 0.077(7) 0.106(9) 0.098(8) 0.014(7) 0.032(6) 0.006(6) C31 0.059(5) 0.073(6) 0.084(7) 0.017(5) 0.018(5) 0.014(5) C32 0.055(5) 0.073(7) 0.094(7) -0.002(6) 0.028(5) 0.003(5) C33 0.068(6) 0.110(8) 0.098(7) -0.013(7) 0.018(6) -0.011(6) C34 0.061(7) 0.156(12) 0.112(9) -0.029(9) 0.012(6) -0.024(8) C35 0.058(6) 0.157(12) 0.103(8) 0.000(9) 0.000(6) 0.009(8) C36 0.055(6) 0.121(9) 0.112(8) 0.012(7) 0.010(6) 0.020(6) N1 0.065(5) 0.159(8) 0.071(5) 0.004(6) -0.004(4) 0.016(5) N2 0.081(5) 0.068(5) 0.081(6) 0.011(4) 0.002(5) 0.014(4) N3 0.065(5) 0.065(5) 0.086(5) 0.012(4) 0.000(4) 0.011(4) N4 0.089(6) 0.069(5) 0.080(6) 0.005(4) -0.004(4) 0.026(4) N5 0.134(8) 0.114(7) 0.099(7) 0.004(6) -0.012(7) 0.043(6) N6 0.069(5) 0.099(7) 0.077(5) 0.024(5) 0.018(4) 0.018(5) N7 0.070(4) 0.070(5) 0.078(5) 0.006(4) 0.009(4) 0.009(4) N8 0.055(4) 0.076(5) 0.084(5) 0.011(4) 0.005(4) 0.017(4) N9 0.202(19) 0.133(13) 0.185(15) -0.041(11) -0.050(13) 0.000(13) N10 0.109(10) 0.32(3) 0.44(4) 0.28(3) 0.028(18) 0.051(15) O1W 0.38(2) 0.53(3) 0.187(11) -0.126(16) 0.136(14) -0.17(2) O1 0.186(12) 0.186(14) 0.42(3) -0.035(14) -0.058(14) -0.013(10) O2W 0.69(6) 0.31(2) 0.31(2) -0.03(2) 0.17(4) -0.05(2) O2 0.215(12) 0.169(12) 0.284(17) -0.078(11) 0.067(12) -0.060(9) O3 0.144(12) 0.50(4) 0.92(6) -0.30(4) 0.18(2) 0.049(16) O3W 0.27(2) 0.55(4) 0.66(6) 0.26(4) -0.15(3) -0.07(3) O4W 0.156(14) 0.33(3) 0.35(3) 0.000 -0.084(15) 0.000 O4 0.50(5) 0.43(3) 0.53(4) 0.27(3) 0.32(4) 0.26(3) O5W 0.30(2) 0.37(2) 0.68(4) 0.26(3) -0.17(2) 0.056(17) O5 0.271(17) 0.278(18) 0.33(2) 0.137(15) -0.100(15) -0.067(13) O6W 0.73(8) 1.00(10) 0.40(4) 0.37(5) 0.19(5) -0.14(7) O6 0.269(17) 0.271(17) 0.35(2) 0.178(16) -0.178(15) -0.066(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 N8 1.981(7) . ? Cu1 N4 1.997(8) . ? Cu1 N3 2.136(7) . ? Cu1 N7 2.154(7) . ? Cu1 O2 2.330(14) . ? Cu1 O1 2.386(17) . ? C1 N1 1.291(15) . ? C1 C2 1.350(18) . ? C1 H1A 0.9300 . ? C2 C3 1.424(19) . ? C2 H2A 0.9300 . ? C3 C4 1.446(15) . ? C3 H3A 0.9300 . ? C4 C5 1.382(14) . ? C4 C9 1.387(13) . ? C5 C6 1.392(14) . ? C5 H5A 0.9300 . ? C6 C7 1.386(12) . ? C6 H6A 0.9300 . ? C7 C8 1.378(11) . ? C7 H7A 0.9300 . ? C8 C9 1.399(12) . ? C8 C10 1.498(12) . ? C9 N1 1.354(11) . ? C10 N2 1.469(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.332(11) . ? C11 C12 1.335(13) . ? C11 H11A 0.9300 . ? C12 C13 1.375(13) . ? C12 H12A 0.9300 . ? C13 N3 1.326(10) . ? C13 C14 1.449(13) . ? C14 N4 1.347(11) . ? C14 C15 1.388(13) . ? C15 C16 1.389(16) . ? C15 H15A 0.9300 . ? C16 C17 1.344(17) . ? C16 H16A 0.9300 . ? C17 C18 1.410(17) . ? C17 H17A 0.9300 . ? C18 N4 1.342(12) . ? C18 H18A 0.9300 . ? C19 N5 1.314(19) . ? C19 C20 1.39(3) . ? C19 H19A 0.9300 . ? C20 C21 1.32(2) . ? C20 H20A 0.9300 . ? C21 C22 1.38(2) . ? C21 H21A 0.9300 . ? C22 C27 1.372(16) . ? C22 C23 1.469(18) . ? C23 C24 1.319(17) . ? C23 H23A 0.9300 . ? C24 C25 1.403(14) . ? C24 H24A 0.9300 . ? C25 C26 1.374(12) . ? C25 H25A 0.9300 . ? C26 C27 1.401(13) . ? C26 C28 1.504(12) . ? C27 N5 1.354(13) . ? C28 N6 1.448(11) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.350(13) . ? C29 N6 1.357(11) . ? C29 H29A 0.9300 . ? C30 C31 1.348(12) . ? C30 H30A 0.9300 . ? C31 N7 1.346(10) . ? C31 C32 1.433(12) . ? C32 N8 1.378(10) . ? C32 C33 1.391(12) . ? C33 C34 1.356(15) . ? C33 H33A 0.9300 . ? C34 C35 1.336(15) . ? C34 H34A 0.9300 . ? C35 C36 1.388(14) . ? C35 H35A 0.9300 . ? C36 N8 1.339(11) . ? C36 H36A 0.9300 . ? N2 N3 1.356(9) . ? N6 N7 1.352(9) . ? N9 O2 1.265(8) . ? N9 O1 1.268(8) . ? N9 O3 1.287(9) . ? N10 O6 1.279(9) . ? N10 O4 1.286(9) . ? N10 O5 1.309(9) . ? O3W O6W 1.75(5) . ? 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 N8 Cu1 N4 178.6(3) . . ? N8 Cu1 N3 100.7(3) . . ? N4 Cu1 N3 79.1(3) . . ? N8 Cu1 N7 80.1(3) . . ? N4 Cu1 N7 101.2(3) . . ? N3 Cu1 N7 111.7(2) . . ? N8 Cu1 O2 86.5(4) . . ? N4 Cu1 O2 92.3(4) . . ? N3 Cu1 O2 109.3(4) . . ? N7 Cu1 O2 138.5(4) . . ? N8 Cu1 O1 90.2(4) . . ? N4 Cu1 O1 89.6(4) . . ? N3 Cu1 O1 160.9(4) . . ? N7 Cu1 O1 85.4(4) . . ? O2 Cu1 O1 55.3(3) . . ? N1 C1 C2 126.1(14) . . ? N1 C1 H1A 116.9 . . ? C2 C1 H1A 116.9 . . ? C1 C2 C3 119.5(14) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C2 C3 C4 114.9(14) . . ? C2 C3 H3A 122.5 . . ? C4 C3 H3A 122.5 . . ? C5 C4 C9 121.3(10) . . ? C5 C4 C3 119.5(14) . . ? C9 C4 C3 119.2(12) . . ? C4 C5 C6 120.4(10) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C7 C6 C5 118.5(9) . . ? C7 C6 H6A 120.7 . . ? C5 C6 H6A 120.7 . . ? C8 C7 C6 121.2(9) . . ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C7 C8 C9 120.5(9) . . ? C7 C8 C10 121.9(9) . . ? C9 C8 C10 117.6(9) . . ? N1 C9 C4 122.3(10) . . ? N1 C9 C8 119.6(10) . . ? C4 C9 C8 118.1(9) . . ? N2 C10 C8 115.0(7) . . ? N2 C10 H10A 108.5 . . ? C8 C10 H10A 108.5 . . ? N2 C10 H10B 108.5 . . ? C8 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? N2 C11 C12 108.8(10) . . ? N2 C11 H11A 125.6 . . ? C12 C11 H11A 125.6 . . ? C11 C12 C13 105.0(10) . . ? C11 C12 H12A 127.5 . . ? C13 C12 H12A 127.5 . . ? N3 C13 C12 111.4(10) . . ? N3 C13 C14 118.6(10) . . ? C12 C13 C14 130.0(11) . . ? N4 C14 C15 121.4(10) . . ? N4 C14 C13 114.0(9) . . ? C15 C14 C13 124.5(11) . . ? C14 C15 C16 118.1(12) . . ? C14 C15 H15A 120.9 . . ? C16 C15 H15A 120.9 . . ? C17 C16 C15 121.1(14) . . ? C17 C16 H16A 119.4 . . ? C15 C16 H16A 119.4 . . ? C16 C17 C18 118.3(14) . . ? C16 C17 H17A 120.9 . . ? C18 C17 H17A 120.9 . . ? N4 C18 C17 121.5(13) . . ? N4 C18 H18A 119.2 . . ? C17 C18 H18A 119.2 . . ? N5 C19 C20 125(2) . . ? N5 C19 H19A 117.6 . . ? C20 C19 H19A 117.6 . . ? C21 C20 C19 118(2) . . ? C21 C20 H20A 121.1 . . ? C19 C20 H20A 121.1 . . ? C20 C21 C22 120(2) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C27 C22 C21 119.8(16) . . ? C27 C22 C23 117.2(14) . . ? C21 C22 C23 123.0(18) . . ? C24 C23 C22 121.2(12) . . ? C24 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? C23 C24 C25 120.8(13) . . ? C23 C24 H24A 119.6 . . ? C25 C24 H24A 119.6 . . ? C26 C25 C24 119.3(11) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? C25 C26 C27 120.9(10) . . ? C25 C26 C28 120.4(10) . . ? C27 C26 C28 118.7(10) . . ? N5 C27 C22 121.2(13) . . ? N5 C27 C26 118.4(12) . . ? C22 C27 C26 120.4(12) . . ? N6 C28 C26 114.9(8) . . ? N6 C28 H28A 108.5 . . ? C26 C28 H28A 108.5 . . ? N6 C28 H28B 108.5 . . ? C26 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? C30 C29 N6 107.3(9) . . ? C30 C29 H29A 126.4 . . ? N6 C29 H29A 126.4 . . ? C31 C30 C29 106.5(11) . . ? C31 C30 H30A 126.7 . . ? C29 C30 H30A 126.7 . . ? N7 C31 C30 111.3(9) . . ? N7 C31 C32 118.5(9) . . ? C30 C31 C32 130.2(11) . . ? N8 C32 C33 120.1(9) . . ? N8 C32 C31 115.3(9) . . ? C33 C32 C31 124.5(9) . . ? C34 C33 C32 119.3(11) . . ? C34 C33 H33A 120.4 . . ? C32 C33 H33A 120.4 . . ? C35 C34 C33 120.6(11) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C36 120.4(11) . . ? C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? N8 C36 C35 120.6(11) . . ? N8 C36 H36A 119.7 . . ? C35 C36 H36A 119.7 . . ? C1 N1 C9 118.0(11) . . ? C11 N2 N3 110.3(9) . . ? C11 N2 C10 128.8(9) . . ? N3 N2 C10 120.8(8) . . ? C13 N3 N2 104.5(8) . . ? C13 N3 Cu1 110.6(7) . . ? N2 N3 Cu1 144.4(7) . . ? C18 N4 C14 119.3(10) . . ? C18 N4 Cu1 123.4(9) . . ? C14 N4 Cu1 117.2(7) . . ? C19 N5 C27 116.6(13) . . ? N7 N6 C29 110.2(9) . . ? N7 N6 C28 119.5(8) . . ? C29 N6 C28 130.3(9) . . ? C31 N7 N6 104.7(7) . . ? C31 N7 Cu1 109.8(6) . . ? N6 N7 Cu1 145.4(7) . . ? C36 N8 C32 119.1(8) . . ? C36 N8 Cu1 124.8(7) . . ? C32 N8 Cu1 116.1(6) . . ? O2 N9 O1 119.6(13) . . ? O2 N9 O3 119.7(14) . . ? O1 N9 O3 120.6(14) . . ? O6 N10 O4 122.5(14) . . ? O6 N10 O5 111.4(13) . . ? O4 N10 O5 124.3(14) . . ? N9 O1 Cu1 91.1(9) . . ? N9 O2 Cu1 93.8(9) . . ? 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 N1 C1 C2 C3 1(2) . . . . ? C1 C2 C3 C4 -1.1(18) . . . . ? C2 C3 C4 C5 -179.1(10) . . . . ? C2 C3 C4 C9 0.9(14) . . . . ? C9 C4 C5 C6 -1.3(14) . . . . ? C3 C4 C5 C6 178.7(9) . . . . ? C4 C5 C6 C7 1.8(14) . . . . ? C5 C6 C7 C8 -0.1(13) . . . . ? C6 C7 C8 C9 -2.1(12) . . . . ? C6 C7 C8 C10 177.0(8) . . . . ? C5 C4 C9 N1 179.5(8) . . . . ? C3 C4 C9 N1 -0.6(13) . . . . ? C5 C4 C9 C8 -0.8(13) . . . . ? C3 C4 C9 C8 179.2(8) . . . . ? C7 C8 C9 N1 -177.8(7) . . . . ? C10 C8 C9 N1 3.2(11) . . . . ? C7 C8 C9 C4 2.5(12) . . . . ? C10 C8 C9 C4 -176.6(8) . . . . ? C7 C8 C10 N2 -7.4(11) . . . . ? C9 C8 C10 N2 171.6(7) . . . . ? N2 C11 C12 C13 -0.7(11) . . . . ? C11 C12 C13 N3 0.9(11) . . . . ? C11 C12 C13 C14 -177.7(9) . . . . ? N3 C13 C14 N4 6.1(10) . . . . ? C12 C13 C14 N4 -175.4(8) . . . . ? N3 C13 C14 C15 -176.2(8) . . . . ? C12 C13 C14 C15 2.2(14) . . . . ? N4 C14 C15 C16 -4.5(13) . . . . ? C13 C14 C15 C16 178.0(8) . . . . ? C14 C15 C16 C17 3.4(16) . . . . ? C15 C16 C17 C18 -2.4(18) . . . . ? C16 C17 C18 N4 2.5(17) . . . . ? N5 C19 C20 C21 0(3) . . . . ? C19 C20 C21 C22 -1(3) . . . . ? C20 C21 C22 C27 2(2) . . . . ? C20 C21 C22 C23 -179.7(16) . . . . ? C27 C22 C23 C24 -0.8(15) . . . . ? C21 C22 C23 C24 -179.2(12) . . . . ? C22 C23 C24 C25 0.1(16) . . . . ? C23 C24 C25 C26 1.6(14) . . . . ? C24 C25 C26 C27 -2.4(12) . . . . ? C24 C25 C26 C28 177.7(8) . . . . ? C21 C22 C27 N5 -1.6(16) . . . . ? C23 C22 C27 N5 180.0(9) . . . . ? C21 C22 C27 C26 178.4(10) . . . . ? C23 C22 C27 C26 0.0(14) . . . . ? C25 C26 C27 N5 -178.4(8) . . . . ? C28 C26 C27 N5 1.5(12) . . . . ? C25 C26 C27 C22 1.6(13) . . . . ? C28 C26 C27 C22 -178.5(8) . . . . ? C25 C26 C28 N6 -6.3(11) . . . . ? C27 C26 C28 N6 173.8(8) . . . . ? N6 C29 C30 C31 1.0(10) . . . . ? C29 C30 C31 N7 -0.7(10) . . . . ? C29 C30 C31 C32 -177.7(8) . . . . ? N7 C31 C32 N8 3.4(10) . . . . ? C30 C31 C32 N8 -179.8(8) . . . . ? N7 C31 C32 C33 -173.5(8) . . . . ? C30 C31 C32 C33 3.3(14) . . . . ? N8 C32 C33 C34 0.7(12) . . . . ? C31 C32 C33 C34 177.5(8) . . . . ? C32 C33 C34 C35 -0.3(15) . . . . ? C33 C34 C35 C36 -0.1(16) . . . . ? C34 C35 C36 N8 0.1(15) . . . . ? C2 C1 N1 C9 -0.6(17) . . . . ? C4 C9 N1 C1 0.4(13) . . . . ? C8 C9 N1 C1 -179.4(8) . . . . ? C12 C11 N2 N3 0.3(10) . . . . ? C12 C11 N2 C10 -179.1(8) . . . . ? C8 C10 N2 C11 102.6(10) . . . . ? C8 C10 N2 N3 -76.8(9) . . . . ? C12 C13 N3 N2 -0.7(9) . . . . ? C14 C13 N3 N2 178.0(7) . . . . ? C12 C13 N3 Cu1 173.2(6) . . . . ? C14 C13 N3 Cu1 -8.1(9) . . . . ? C11 N2 N3 C13 0.2(9) . . . . ? C10 N2 N3 C13 179.7(7) . . . . ? C11 N2 N3 Cu1 -169.9(7) . . . . ? C10 N2 N3 Cu1 9.6(12) . . . . ? N8 Cu1 N3 C13 -175.6(5) . . . . ? N4 Cu1 N3 C13 5.9(5) . . . . ? N7 Cu1 N3 C13 -92.0(6) . . . . ? O2 Cu1 N3 C13 94.4(6) . . . . ? O1 Cu1 N3 C13 60.7(14) . . . . ? N8 Cu1 N3 N2 -5.8(9) . . . . ? N4 Cu1 N3 N2 175.6(9) . . . . ? N7 Cu1 N3 N2 77.7(9) . . . . ? O2 Cu1 N3 N2 -95.8(9) . . . . ? O1 Cu1 N3 N2 -129.6(14) . . . . ? C17 C18 N4 C14 -3.6(14) . . . . ? C17 C18 N4 Cu1 179.5(8) . . . . ? C15 C14 N4 C18 4.7(12) . . . . ? C13 C14 N4 C18 -177.6(7) . . . . ? C15 C14 N4 Cu1 -178.2(6) . . . . ? C13 C14 N4 Cu1 -0.5(9) . . . . ? N8 Cu1 N4 C18 92(14) . . . . ? N3 Cu1 N4 C18 174.2(7) . . . . ? N7 Cu1 N4 C18 -75.6(7) . . . . ? O2 Cu1 N4 C18 64.9(8) . . . . ? O1 Cu1 N4 C18 9.7(8) . . . . ? N8 Cu1 N4 C14 -85(14) . . . . ? N3 Cu1 N4 C14 -2.8(5) . . . . ? N7 Cu1 N4 C14 107.4(6) . . . . ? O2 Cu1 N4 C14 -112.1(7) . . . . ? O1 Cu1 N4 C14 -167.3(7) . . . . ? C20 C19 N5 C27 0(2) . . . . ? C22 C27 N5 C19 0.4(15) . . . . ? C26 C27 N5 C19 -179.5(10) . . . . ? C30 C29 N6 N7 -0.9(9) . . . . ? C30 C29 N6 C28 179.6(8) . . . . ? C26 C28 N6 N7 -75.1(9) . . . . ? C26 C28 N6 C29 104.4(10) . . . . ? C30 C31 N7 N6 0.1(9) . . . . ? C32 C31 N7 N6 177.5(6) . . . . ? C30 C31 N7 Cu1 177.4(5) . . . . ? C32 C31 N7 Cu1 -5.2(9) . . . . ? C29 N6 N7 C31 0.5(8) . . . . ? C28 N6 N7 C31 -180.0(7) . . . . ? C29 N6 N7 Cu1 -175.0(7) . . . . ? C28 N6 N7 Cu1 4.5(13) . . . . ? N8 Cu1 N7 C31 4.2(5) . . . . ? N4 Cu1 N7 C31 -176.2(5) . . . . ? N3 Cu1 N7 C31 -93.5(6) . . . . ? O2 Cu1 N7 C31 77.3(8) . . . . ? O1 Cu1 N7 C31 95.1(6) . . . . ? N8 Cu1 N7 N6 179.6(9) . . . . ? N4 Cu1 N7 N6 -0.8(9) . . . . ? N3 Cu1 N7 N6 81.9(9) . . . . ? O2 Cu1 N7 N6 -107.3(10) . . . . ? O1 Cu1 N7 N6 -89.5(9) . . . . ? C35 C36 N8 C32 0.3(12) . . . . ? C35 C36 N8 Cu1 -177.8(7) . . . . ? C33 C32 N8 C36 -0.7(11) . . . . ? C31 C32 N8 C36 -177.8(7) . . . . ? C33 C32 N8 Cu1 177.6(6) . . . . ? C31 C32 N8 Cu1 0.6(8) . . . . ? N4 Cu1 N8 C36 8(14) . . . . ? N3 Cu1 N8 C36 -73.9(7) . . . . ? N7 Cu1 N8 C36 175.7(7) . . . . ? O2 Cu1 N8 C36 35.1(7) . . . . ? O1 Cu1 N8 C36 90.3(7) . . . . ? N4 Cu1 N8 C32 -170(14) . . . . ? N3 Cu1 N8 C32 107.9(5) . . . . ? N7 Cu1 N8 C32 -2.5(5) . . . . ? O2 Cu1 N8 C32 -143.1(6) . . . . ? O1 Cu1 N8 C32 -87.9(6) . . . . ? O2 N9 O1 Cu1 -3.7(17) . . . . ? O3 N9 O1 Cu1 179.5(17) . . . . ? N8 Cu1 O1 N9 -83.5(10) . . . . ? N4 Cu1 O1 N9 95.1(10) . . . . ? N3 Cu1 O1 N9 42(2) . . . . ? N7 Cu1 O1 N9 -163.6(11) . . . . ? O2 Cu1 O1 N9 2.1(10) . . . . ? O1 N9 O2 Cu1 3.8(18) . . . . ? O3 N9 O2 Cu1 -179.4(16) . . . . ? N8 Cu1 O2 N9 90.5(10) . . . . ? N4 Cu1 O2 N9 -90.1(11) . . . . ? N3 Cu1 O2 N9 -169.4(9) . . . . ? N7 Cu1 O2 N9 19.7(14) . . . . ? O1 Cu1 O2 N9 -2.1(10) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.565 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.085 #===END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 Cl2 Cu N8 O11' _chemical_formula_weight 889.15 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 'Pbca' 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' '-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 13.326(4) _cell_length_b 21.715(6) _cell_length_c 26.318(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7616(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1054 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 22.89 _exptl_crystal_description BLOCK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3656 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.786407 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details '(SADABS; bruker, 1996)' _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 'BRUKER CCD -AREA-DETECTOR' _diffrn_measurement_method '\F AND \W SCANS' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41548 _diffrn_reflns_av_R_equivalents 0.1662 _diffrn_reflns_av_sigmaI/netI 0.1195 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.43 _reflns_number_total 7780 _reflns_number_gt 3307 _reflns_threshold_expression I>2s\(I) _computing_data_collection 'SMART, BRUKER, 1998' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT, BRUKER 1998' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997A)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997A)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997B)' _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^)+(0.0779P)^2^+3.0530P] 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 7780 _refine_ls_number_parameters 550 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2054 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2049 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.030 _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 0.25201(6) 0.10530(3) 0.65432(3) 0.0378(2) Uani 1 1 d . . . C1 C 0.2737(7) 0.1659(4) 0.4060(3) 0.070(3) Uani 1 1 d . . . H1A H 0.3336 0.1716 0.3884 0.084 Uiso 1 1 calc R . . C2 C 0.1931(9) 0.2030(4) 0.3926(3) 0.078(3) Uani 1 1 d . . . H2A H 0.1996 0.2325 0.3672 0.094 Uiso 1 1 calc R . . C3 C 0.1042(8) 0.1954(4) 0.4173(3) 0.075(3) Uani 1 1 d . . . H3A H 0.0495 0.2202 0.4095 0.090 Uiso 1 1 calc R . . C4 C 0.0053(6) 0.1368(4) 0.4801(3) 0.062(2) Uani 1 1 d . . . H4A H -0.0523 0.1591 0.4723 0.075 Uiso 1 1 calc R . . C5 C 0.0015(6) 0.0917(4) 0.5160(3) 0.063(2) Uani 1 1 d . . . H5A H -0.0586 0.0837 0.5327 0.076 Uiso 1 1 calc R . . C6 C 0.0873(5) 0.0573(3) 0.5280(3) 0.0491(18) Uani 1 1 d . . . H6A H 0.0832 0.0266 0.5526 0.059 Uiso 1 1 calc R . . C7 C 0.1762(5) 0.0679(3) 0.5043(3) 0.0442(17) Uani 1 1 d . . . C8 C 0.1820(6) 0.1148(3) 0.4663(3) 0.0447(17) Uani 1 1 d . . . C9 C 0.0959(6) 0.1500(3) 0.4546(3) 0.055(2) Uani 1 1 d . . . C10 C 0.2707(5) 0.0326(3) 0.5168(2) 0.0484(19) Uani 1 1 d . . . H10A H 0.2887 0.0070 0.4879 0.058 Uiso 1 1 calc R . . H10B H 0.3250 0.0615 0.5225 0.058 Uiso 1 1 calc R . . C11 C 0.2549(6) -0.0685(3) 0.5627(3) 0.0535(18) Uani 1 1 d . . . H11A H 0.2579 -0.0948 0.5349 0.064 Uiso 1 1 calc R . . C12 C 0.2450(6) -0.0854(3) 0.6120(3) 0.0538(18) Uani 1 1 d . . . H12A H 0.2401 -0.1252 0.6248 0.065 Uiso 1 1 calc R . . C13 C 0.2438(5) -0.0305(3) 0.6397(2) 0.0366(14) Uani 1 1 d . . . C14 C 0.2391(4) -0.0193(3) 0.6940(2) 0.0323(14) Uani 1 1 d . . . C15 C 0.2373(5) -0.0662(3) 0.7295(3) 0.0442(17) Uani 1 1 d . . . H15A H 0.2373 -0.1070 0.7188 0.053 Uiso 1 1 calc R . . C16 C 0.2358(5) -0.0527(3) 0.7803(3) 0.0462(18) Uani 1 1 d . . . H16A H 0.2346 -0.0842 0.8042 0.055 Uiso 1 1 calc R . . C17 C 0.2360(5) 0.0083(3) 0.7958(3) 0.0453(17) Uani 1 1 d . . . H17A H 0.2349 0.0187 0.8301 0.054 Uiso 1 1 calc R . . C18 C 0.2378(4) 0.0527(3) 0.7586(2) 0.0387(15) Uani 1 1 d . . . H18A H 0.2380 0.0937 0.7688 0.046 Uiso 1 1 calc R . . C19 C -0.0114(5) -0.0355(4) 0.8325(3) 0.055(2) Uani 1 1 d . . . H19A H -0.0109 -0.0221 0.8661 0.066 Uiso 1 1 calc R . . C20 C -0.0120(5) -0.0993(4) 0.8232(4) 0.065(2) Uani 1 1 d . . . H20A H -0.0110 -0.1273 0.8500 0.078 Uiso 1 1 calc R . . C21 C -0.0141(5) -0.1192(4) 0.7748(4) 0.062(2) Uani 1 1 d . . . H21A H -0.0160 -0.1612 0.7679 0.075 Uiso 1 1 calc R . . C22 C -0.0186(6) -0.0939(4) 0.6839(4) 0.073(3) Uani 1 1 d . . . H22A H -0.0216 -0.1355 0.6756 0.087 Uiso 1 1 calc R . . C23 C -0.0196(6) -0.0515(4) 0.6461(4) 0.075(3) Uani 1 1 d . . . H23A H -0.0245 -0.0640 0.6124 0.089 Uiso 1 1 calc R . . C24 C -0.0130(5) 0.0123(4) 0.6584(3) 0.054(2) Uani 1 1 d . . . H24A H -0.0126 0.0416 0.6326 0.064 Uiso 1 1 calc R . . C25 C -0.0073(4) 0.0306(3) 0.7079(3) 0.0413(17) Uani 1 1 d . . . C26 C -0.0106(5) -0.0130(3) 0.7476(3) 0.0439(17) Uani 1 1 d . . . C27 C -0.0133(5) -0.0767(3) 0.7350(3) 0.050(2) Uani 1 1 d . . . C28 C 0.0024(5) 0.0983(3) 0.7220(3) 0.0440(17) Uani 1 1 d . . . H28A H -0.0587 0.1112 0.7390 0.053 Uiso 1 1 calc R . . H28B H 0.0572 0.1028 0.7460 0.053 Uiso 1 1 calc R . . C29 C -0.0446(5) 0.1793(4) 0.6591(3) 0.063(2) Uani 1 1 d . . . H29A H -0.1110 0.1845 0.6690 0.075 Uiso 1 1 calc R . . C30 C 0.0025(6) 0.2113(4) 0.6217(3) 0.065(2) Uani 1 1 d . . . H30A H -0.0239 0.2427 0.6017 0.078 Uiso 1 1 calc R . . C31 C 0.0983(5) 0.1869(3) 0.6198(3) 0.0436(17) Uani 1 1 d . . . C32 C 0.1848(5) 0.2014(3) 0.5882(3) 0.0402(17) Uani 1 1 d . . . C33 C 0.1854(6) 0.2456(3) 0.5504(3) 0.057(2) Uani 1 1 d . . . H33A H 0.1279 0.2685 0.5440 0.068 Uiso 1 1 calc R . . C34 C 0.2696(6) 0.2556(3) 0.5225(3) 0.056(2) Uani 1 1 d . . . H34A H 0.2712 0.2858 0.4974 0.067 Uiso 1 1 calc R . . C35 C 0.3523(6) 0.2199(3) 0.5326(3) 0.053(2) Uani 1 1 d . . . H35A H 0.4106 0.2247 0.5135 0.064 Uiso 1 1 calc R . . C36 C 0.3484(5) 0.1767(3) 0.5711(3) 0.0493(19) Uani 1 1 d . . . H36A H 0.4055 0.1536 0.5781 0.059 Uiso 1 1 calc R . . N1 N 0.2721(5) 0.1230(3) 0.4419(2) 0.0584(18) Uani 1 1 d . . . N2 N 0.2596(4) -0.0061(2) 0.5613(2) 0.0453(14) Uani 1 1 d . . . N3 N 0.2532(4) 0.0180(2) 0.60827(18) 0.0404(12) Uani 1 1 d . . . N4 N 0.2394(4) 0.0409(2) 0.70859(18) 0.0326(11) Uani 1 1 d . . . N5 N -0.0115(4) 0.0063(3) 0.7961(2) 0.0432(15) Uani 1 1 d . . . N6 N 0.0203(4) 0.1392(3) 0.6792(2) 0.0472(15) Uani 1 1 d . . . N7 N 0.1093(4) 0.1422(2) 0.6548(2) 0.0373(12) Uani 1 1 d . . . N8 N 0.2660(4) 0.1672(2) 0.59833(19) 0.0385(13) Uani 1 1 d . . . O1W O 0.4012(3) 0.1074(2) 0.66390(17) 0.0466(12) Uani 1 1 d . . . O1 O 0.610(3) 0.0633(10) 0.5789(12) 0.236(19) Uani 0.50 1 d P A 1 O1' O 0.658(2) 0.0482(8) 0.5866(7) 0.216(19) Uani 0.50 1 d PD A 2 O2W O 0.4949(6) 0.2168(3) 0.6783(3) 0.128(3) Uani 1 1 d . . . O2 O 0.6105(7) 0.1517(4) 0.5527(4) 0.157(4) Uani 1 1 d . A . O3 O 0.667(2) 0.1356(9) 0.6339(8) 0.138(10) Uani 0.70 1 d P A 1 O3' O 0.697(7) 0.143(3) 0.636(2) 0.19(3) Uani 0.30 1 d P A 2 O3W O 0.4925(6) 0.1221(5) 0.4541(3) 0.160(4) Uani 1 1 d . . . O4 O 0.7635(7) 0.1225(7) 0.5635(4) 0.206(5) Uani 1 1 d D A . O5 O 0.2463(7) 0.2796(3) 0.6905(2) 0.133(3) Uani 1 1 d . B . O6 O 0.316(2) 0.2860(16) 0.7682(13) 0.145(14) Uani 0.50 1 d P B 1 O6' O 0.274(3) 0.2856(16) 0.7762(10) 0.160(16) Uani 0.50 1 d P B 2 O7 O 0.1452(7) 0.2455(6) 0.7517(4) 0.207(5) Uani 1 1 d . B . O8 O 0.2839(5) 0.1926(2) 0.7337(3) 0.111(3) Uani 1 1 d . B . Cl1 Cl 0.6717(3) 0.11463(12) 0.58474(11) 0.0982(10) Uani 1 1 d . . . Cl2 Cl 0.24599(19) 0.25219(8) 0.73816(7) 0.0601(5) 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 0.0355(4) 0.0378(4) 0.0399(4) 0.0085(3) 0.0010(4) 0.0017(5) C1 0.081(7) 0.077(6) 0.053(5) -0.004(5) 0.008(4) -0.022(5) C2 0.120(9) 0.066(6) 0.050(6) 0.017(5) -0.005(6) -0.006(6) C3 0.109(8) 0.062(6) 0.054(6) -0.001(5) -0.026(6) 0.002(6) C4 0.064(6) 0.049(5) 0.074(6) -0.023(5) -0.018(5) 0.019(5) C5 0.056(5) 0.067(6) 0.066(6) -0.008(5) 0.003(4) 0.005(5) C6 0.049(5) 0.054(5) 0.044(4) 0.002(4) 0.003(4) -0.001(4) C7 0.054(5) 0.044(4) 0.035(4) -0.008(3) -0.004(3) -0.002(4) C8 0.055(5) 0.046(4) 0.033(4) -0.010(3) -0.002(3) -0.004(4) C9 0.073(6) 0.053(5) 0.040(5) -0.006(4) -0.017(4) 0.005(5) C10 0.055(5) 0.053(4) 0.037(4) -0.003(3) 0.007(3) 0.009(4) C11 0.065(5) 0.042(4) 0.053(5) -0.011(3) 0.002(5) 0.002(5) C12 0.064(5) 0.037(4) 0.060(5) -0.005(3) 0.001(5) 0.002(4) C13 0.032(3) 0.037(3) 0.041(4) 0.006(3) -0.005(3) 0.002(4) C14 0.022(3) 0.039(3) 0.036(3) 0.004(3) 0.001(3) -0.001(3) C15 0.037(4) 0.038(4) 0.058(5) 0.009(3) -0.002(4) 0.005(3) C16 0.038(4) 0.049(4) 0.051(5) 0.022(3) -0.001(3) -0.002(4) C17 0.034(4) 0.065(5) 0.037(4) 0.002(3) 0.000(3) -0.001(4) C18 0.032(4) 0.041(4) 0.043(4) 0.002(3) -0.004(3) 0.002(3) C19 0.040(4) 0.066(6) 0.059(5) 0.004(4) -0.003(4) 0.003(4) C20 0.039(4) 0.059(6) 0.095(7) 0.021(5) 0.002(5) 0.007(4) C21 0.044(5) 0.046(5) 0.097(7) 0.000(5) 0.002(5) -0.003(4) C22 0.057(5) 0.054(5) 0.107(8) -0.033(6) 0.015(5) -0.011(4) C23 0.066(6) 0.083(7) 0.074(7) -0.041(6) 0.011(5) -0.020(5) C24 0.047(4) 0.067(5) 0.047(5) -0.010(4) 0.015(4) -0.012(4) C25 0.024(3) 0.057(5) 0.043(4) -0.013(4) 0.011(3) -0.004(3) C26 0.025(4) 0.050(4) 0.057(5) -0.006(4) 0.005(3) -0.003(4) C27 0.036(4) 0.051(5) 0.063(6) -0.022(4) 0.007(4) -0.005(4) C28 0.038(4) 0.048(4) 0.047(4) -0.003(4) 0.010(3) 0.006(4) C29 0.038(4) 0.077(6) 0.074(6) 0.009(5) 0.005(4) 0.022(4) C30 0.053(5) 0.069(5) 0.074(6) 0.016(5) -0.005(5) 0.020(5) C31 0.051(5) 0.037(4) 0.042(4) -0.002(3) -0.006(3) 0.002(4) C32 0.050(5) 0.038(4) 0.033(4) -0.005(3) -0.003(3) 0.006(3) C33 0.076(6) 0.041(4) 0.053(5) 0.013(4) -0.022(4) -0.001(4) C34 0.085(7) 0.046(4) 0.037(4) 0.015(3) -0.005(4) -0.008(5) C35 0.068(5) 0.053(5) 0.039(5) 0.004(4) 0.007(4) -0.018(4) C36 0.050(5) 0.051(4) 0.046(5) 0.004(4) -0.004(4) 0.000(4) N1 0.074(5) 0.060(4) 0.042(4) -0.001(3) 0.004(3) -0.004(3) N2 0.050(4) 0.041(3) 0.044(3) -0.002(3) 0.008(3) 0.006(3) N3 0.044(3) 0.041(3) 0.037(3) -0.006(2) -0.001(3) 0.008(3) N4 0.028(3) 0.040(3) 0.030(3) 0.001(2) -0.005(3) 0.002(3) N5 0.033(3) 0.050(4) 0.046(4) -0.003(3) 0.001(3) 0.002(3) N6 0.043(3) 0.054(4) 0.045(4) 0.002(3) 0.002(3) 0.008(3) N7 0.033(3) 0.037(3) 0.042(3) 0.001(3) 0.000(3) 0.001(3) N8 0.036(3) 0.046(3) 0.033(3) 0.000(2) -0.001(3) -0.003(3) O1W 0.037(2) 0.048(3) 0.055(3) 0.012(2) -0.005(2) -0.003(2) O1 0.34(4) 0.043(12) 0.33(4) 0.053(15) 0.17(3) -0.035(19) O1' 0.56(6) 0.039(10) 0.052(10) -0.008(8) -0.007(17) 0.066(17) O2W 0.159(7) 0.104(5) 0.120(7) 0.006(4) 0.013(5) -0.072(5) O2 0.181(9) 0.138(7) 0.153(9) 0.026(6) -0.032(7) 0.005(7) O3 0.24(2) 0.092(12) 0.079(15) 0.011(10) 0.065(14) 0.044(13) O3' 0.29(7) 0.18(5) 0.09(4) -0.10(3) -0.04(4) -0.02(4) O3W 0.096(6) 0.273(12) 0.112(7) -0.003(7) 0.036(5) 0.012(7) O4 0.135(8) 0.346(17) 0.137(9) -0.010(9) 0.039(7) 0.062(9) O5 0.266(10) 0.065(4) 0.068(5) 0.011(3) -0.011(6) -0.003(5) O6 0.149(18) 0.066(13) 0.22(3) 0.013(17) -0.12(2) -0.053(12) O6' 0.35(5) 0.081(14) 0.048(11) -0.027(10) 0.00(2) -0.06(3) O7 0.098(7) 0.331(15) 0.192(11) 0.014(11) 0.040(7) 0.038(9) O8 0.141(6) 0.045(4) 0.147(7) 0.006(4) -0.016(5) 0.025(4) Cl1 0.155(3) 0.0747(18) 0.0648(18) 0.0091(14) 0.0470(18) 0.0141(19) Cl2 0.0812(14) 0.0396(9) 0.0594(12) 0.0002(9) -0.0030(13) 0.0051(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 N8 2.002(5) . ? Cu1 O1W 2.005(4) . ? Cu1 N4 2.005(5) . ? Cu1 N7 2.064(5) . ? Cu1 N3 2.250(5) . ? C1 N1 1.327(10) . ? C1 C2 1.388(11) . ? C1 H1A 0.9300 . ? C2 C3 1.361(12) . ? C2 H2A 0.9300 . ? C3 C9 1.395(11) . ? C3 H3A 0.9300 . ? C4 C5 1.360(10) . ? C4 C9 1.412(11) . ? C4 H4A 0.9300 . ? C5 C6 1.403(9) . ? C5 H5A 0.9300 . ? C6 C7 1.359(9) . ? C6 H6A 0.9300 . ? C7 C8 1.430(9) . ? C7 C10 1.511(9) . ? C8 N1 1.374(9) . ? C8 C9 1.412(10) . ? C10 N2 1.449(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.355(8) . ? C11 C12 1.355(9) . ? C11 H11A 0.9300 . ? C12 C13 1.396(8) . ? C12 H12A 0.9300 . ? C13 N3 1.344(7) . ? C13 C14 1.453(8) . ? C14 N4 1.363(7) . ? C14 C15 1.381(8) . ? C15 C16 1.368(9) . ? C15 H15A 0.9300 . ? C16 C17 1.385(9) . ? C16 H16A 0.9300 . ? C17 C18 1.375(9) . ? C17 H17A 0.9300 . ? C18 N4 1.340(7) . ? C18 H18A 0.9300 . ? C19 N5 1.322(9) . ? C19 C20 1.408(10) . ? C19 H19A 0.9300 . ? C20 C21 1.344(11) . ? C20 H20A 0.9300 . ? C21 C27 1.396(11) . ? C21 H21A 0.9300 . ? C22 C23 1.355(12) . ? C22 C27 1.398(11) . ? C22 H22A 0.9300 . ? C23 C24 1.426(10) . ? C23 H23A 0.9300 . ? C24 C25 1.364(9) . ? C24 H24A 0.9300 . ? C25 C26 1.412(10) . ? C25 C28 1.522(9) . ? C26 N5 1.344(8) . ? C26 C27 1.423(9) . ? C28 N6 1.455(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N6 1.337(8) . ? C29 C30 1.357(10) . ? C29 H29A 0.9300 . ? C30 C31 1.384(9) . ? C30 H30A 0.9300 . ? C31 N7 1.347(8) . ? C31 C32 1.456(9) . ? C32 N8 1.340(8) . ? C32 C33 1.382(9) . ? C33 C34 1.358(10) . ? C33 H33A 0.9300 . ? C34 C35 1.374(10) . ? C34 H34A 0.9300 . ? C35 C36 1.381(9) . ? C35 H35A 0.9300 . ? C36 N8 1.329(8) . ? C36 H36A 0.9300 . ? N2 N3 1.346(7) . ? N6 N7 1.349(7) . ? O1 Cl1 1.39(2) . ? O1' Cl1 1.456(17) . ? O2 Cl1 1.423(9) . ? O3 Cl1 1.37(2) . ? O3' Cl1 1.52(5) . ? O4 Cl1 1.357(9) . ? O5 Cl2 1.389(6) . ? O6 Cl2 1.43(2) . ? O6' Cl2 1.29(2) . ? O7 Cl2 1.398(9) . ? O8 Cl2 1.394(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 N8 Cu1 O1W 89.12(19) . . ? N8 Cu1 N4 177.9(2) . . ? O1W Cu1 N4 90.56(18) . . ? N8 Cu1 N7 80.2(2) . . ? O1W Cu1 N7 154.71(19) . . ? N4 Cu1 N7 100.9(2) . . ? N8 Cu1 N3 99.7(2) . . ? O1W Cu1 N3 94.61(19) . . ? N4 Cu1 N3 78.28(19) . . ? N7 Cu1 N3 109.7(2) . . ? N1 C1 C2 125.1(8) . . ? N1 C1 H1A 117.4 . . ? C2 C1 H1A 117.4 . . ? C3 C2 C1 118.8(8) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C2 C3 C9 119.4(9) . . ? C2 C3 H3A 120.3 . . ? C9 C3 H3A 120.3 . . ? C5 C4 C9 120.5(8) . . ? C5 C4 H4A 119.7 . . ? C9 C4 H4A 119.7 . . ? C4 C5 C6 120.7(8) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C7 C6 C5 121.1(7) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C6 C7 C8 119.3(7) . . ? C6 C7 C10 122.7(7) . . ? C8 C7 C10 118.0(6) . . ? N1 C8 C9 122.6(7) . . ? N1 C8 C7 117.8(7) . . ? C9 C8 C7 119.6(7) . . ? C3 C9 C8 118.1(8) . . ? C3 C9 C4 123.0(8) . . ? C8 C9 C4 118.8(7) . . ? N2 C10 C7 112.7(5) . . ? N2 C10 H10A 109.1 . . ? C7 C10 H10A 109.1 . . ? N2 C10 H10B 109.1 . . ? C7 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? N2 C11 C12 107.6(6) . . ? N2 C11 H11A 126.2 . . ? C12 C11 H11A 126.2 . . ? C11 C12 C13 105.6(6) . . ? C11 C12 H12A 127.2 . . ? C13 C12 H12A 127.2 . . ? N3 C13 C12 110.3(5) . . ? N3 C13 C14 118.6(5) . . ? C12 C13 C14 131.1(6) . . ? N4 C14 C15 121.2(6) . . ? N4 C14 C13 115.9(5) . . ? C15 C14 C13 122.9(6) . . ? C16 C15 C14 120.2(6) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C17 119.6(6) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 117.4(6) . . ? C18 C17 H17A 121.3 . . ? C16 C17 H17A 121.3 . . ? N4 C18 C17 124.5(6) . . ? N4 C18 H18A 117.8 . . ? C17 C18 H18A 117.8 . . ? N5 C19 C20 123.3(8) . . ? N5 C19 H19A 118.3 . . ? C20 C19 H19A 118.3 . . ? C21 C20 C19 118.8(8) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? C20 C21 C27 119.9(8) . . ? C20 C21 H21A 120.1 . . ? C27 C21 H21A 120.1 . . ? C23 C22 C27 121.7(8) . . ? C23 C22 H22A 119.1 . . ? C27 C22 H22A 119.1 . . ? C22 C23 C24 119.6(8) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C25 C24 C23 120.2(8) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 120.6(7) . . ? C24 C25 C28 121.3(7) . . ? C26 C25 C28 118.0(6) . . ? N5 C26 C25 119.6(6) . . ? N5 C26 C27 121.6(7) . . ? C25 C26 C27 118.8(7) . . ? C21 C27 C22 123.1(8) . . ? C21 C27 C26 117.9(7) . . ? C22 C27 C26 118.9(8) . . ? N6 C28 C25 114.4(6) . . ? N6 C28 H28A 108.7 . . ? C25 C28 H28A 108.7 . . ? N6 C28 H28B 108.7 . . ? C25 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? N6 C29 C30 108.7(7) . . ? N6 C29 H29A 125.6 . . ? C30 C29 H29A 125.6 . . ? C29 C30 C31 104.9(7) . . ? C29 C30 H30A 127.5 . . ? C31 C30 H30A 127.5 . . ? N7 C31 C30 110.5(7) . . ? N7 C31 C32 117.5(6) . . ? C30 C31 C32 131.9(7) . . ? N8 C32 C33 121.6(7) . . ? N8 C32 C31 113.8(6) . . ? C33 C32 C31 124.5(7) . . ? C34 C33 C32 120.3(7) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C33 C34 C35 117.9(7) . . ? C33 C34 H34A 121.1 . . ? C35 C34 H34A 121.1 . . ? C34 C35 C36 119.7(7) . . ? C34 C35 H35A 120.2 . . ? C36 C35 H35A 120.2 . . ? N8 C36 C35 122.2(7) . . ? N8 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? C1 N1 C8 116.0(7) . . ? N3 N2 C11 111.1(5) . . ? N3 N2 C10 121.6(5) . . ? C11 N2 C10 127.3(6) . . ? C13 N3 N2 105.4(5) . . ? C13 N3 Cu1 109.2(4) . . ? N2 N3 Cu1 145.4(4) . . ? C18 N4 C14 117.3(5) . . ? C18 N4 Cu1 124.6(4) . . ? C14 N4 Cu1 118.0(4) . . ? C19 N5 C26 118.3(6) . . ? C29 N6 N7 110.4(6) . . ? C29 N6 C28 126.8(6) . . ? N7 N6 C28 122.8(5) . . ? C31 N7 N6 105.4(5) . . ? C31 N7 Cu1 112.0(4) . . ? N6 N7 Cu1 142.6(4) . . ? C36 N8 C32 118.2(6) . . ? C36 N8 Cu1 125.4(5) . . ? C32 N8 Cu1 116.4(4) . . ? O4 Cl1 O3 112.6(15) . . ? O4 Cl1 O1 125.9(14) . . ? O3 Cl1 O1 110.2(17) . . ? O4 Cl1 O2 101.6(7) . . ? O3 Cl1 O2 110.4(11) . . ? O1 Cl1 O2 92.9(16) . . ? O4 Cl1 O1' 104.6(11) . . ? O3 Cl1 O1' 106.9(12) . . ? O1 Cl1 O1' 30(2) . . ? O2 Cl1 O1' 120.6(12) . . ? O4 Cl1 O3' 96(3) . . ? O3 Cl1 O3' 16(4) . . ? O1 Cl1 O3' 124(3) . . ? O2 Cl1 O3' 115(3) . . ? O1' Cl1 O3' 113(3) . . ? O6' Cl2 O5 117.2(16) . . ? O6' Cl2 O8 118.8(18) . . ? O5 Cl2 O8 108.7(5) . . ? O6' Cl2 O7 98.0(18) . . ? O5 Cl2 O7 106.1(6) . . ? O8 Cl2 O7 105.9(6) . . ? O6' Cl2 O6 25(3) . . ? O5 Cl2 O6 106.1(15) . . ? O8 Cl2 O6 106.6(15) . . ? O7 Cl2 O6 122.8(16) . . ? 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 N1 C1 C2 C3 -0.6(14) . . . . ? C1 C2 C3 C9 -1.2(13) . . . . ? C9 C4 C5 C6 -0.4(12) . . . . ? C4 C5 C6 C7 0.1(11) . . . . ? C5 C6 C7 C8 -0.4(11) . . . . ? C5 C6 C7 C10 179.0(6) . . . . ? C6 C7 C8 N1 -177.8(6) . . . . ? C10 C7 C8 N1 2.8(9) . . . . ? C6 C7 C8 C9 1.1(10) . . . . ? C10 C7 C8 C9 -178.3(6) . . . . ? C2 C3 C9 C8 2.0(12) . . . . ? C2 C3 C9 C4 -176.5(8) . . . . ? N1 C8 C9 C3 -1.2(10) . . . . ? C7 C8 C9 C3 179.9(7) . . . . ? N1 C8 C9 C4 177.4(7) . . . . ? C7 C8 C9 C4 -1.5(10) . . . . ? C5 C4 C9 C3 179.7(7) . . . . ? C5 C4 C9 C8 1.1(11) . . . . ? C6 C7 C10 N2 -9.0(9) . . . . ? C8 C7 C10 N2 170.4(6) . . . . ? N2 C11 C12 C13 0.2(9) . . . . ? C11 C12 C13 N3 -0.4(9) . . . . ? C11 C12 C13 C14 -177.1(7) . . . . ? N3 C13 C14 N4 3.3(9) . . . . ? C12 C13 C14 N4 179.8(7) . . . . ? N3 C13 C14 C15 -174.8(6) . . . . ? C12 C13 C14 C15 1.7(12) . . . . ? N4 C14 C15 C16 0.1(10) . . . . ? C13 C14 C15 C16 178.1(6) . . . . ? C14 C15 C16 C17 0.0(10) . . . . ? C15 C16 C17 C18 0.0(10) . . . . ? C16 C17 C18 N4 0.0(10) . . . . ? N5 C19 C20 C21 -0.9(12) . . . . ? C19 C20 C21 C27 1.4(11) . . . . ? C27 C22 C23 C24 1.3(13) . . . . ? C22 C23 C24 C25 -1.0(12) . . . . ? C23 C24 C25 C26 -1.7(10) . . . . ? C23 C24 C25 C28 178.5(6) . . . . ? C24 C25 C26 N5 -175.7(6) . . . . ? C28 C25 C26 N5 4.1(9) . . . . ? C24 C25 C26 C27 4.1(10) . . . . ? C28 C25 C26 C27 -176.1(6) . . . . ? C20 C21 C27 C22 -177.8(7) . . . . ? C20 C21 C27 C26 -0.2(11) . . . . ? C23 C22 C27 C21 178.8(8) . . . . ? C23 C22 C27 C26 1.2(12) . . . . ? N5 C26 C27 C21 -1.7(10) . . . . ? C25 C26 C27 C21 178.5(6) . . . . ? N5 C26 C27 C22 176.0(6) . . . . ? C25 C26 C27 C22 -3.8(10) . . . . ? C24 C25 C28 N6 -8.9(9) . . . . ? C26 C25 C28 N6 171.2(5) . . . . ? N6 C29 C30 C31 1.4(10) . . . . ? C29 C30 C31 N7 -0.4(9) . . . . ? C29 C30 C31 C32 -179.6(7) . . . . ? N7 C31 C32 N8 0.3(9) . . . . ? C30 C31 C32 N8 179.4(7) . . . . ? N7 C31 C32 C33 179.5(6) . . . . ? C30 C31 C32 C33 -1.4(13) . . . . ? N8 C32 C33 C34 -0.4(11) . . . . ? C31 C32 C33 C34 -179.5(7) . . . . ? C32 C33 C34 C35 1.2(11) . . . . ? C33 C34 C35 C36 -1.8(11) . . . . ? C34 C35 C36 N8 1.7(11) . . . . ? C2 C1 N1 C8 1.4(12) . . . . ? C9 C8 N1 C1 -0.5(10) . . . . ? C7 C8 N1 C1 178.4(6) . . . . ? C12 C11 N2 N3 0.0(9) . . . . ? C12 C11 N2 C10 179.7(6) . . . . ? C7 C10 N2 N3 -71.2(8) . . . . ? C7 C10 N2 C11 109.2(8) . . . . ? C12 C13 N3 N2 0.4(8) . . . . ? C14 C13 N3 N2 177.6(6) . . . . ? C12 C13 N3 Cu1 -179.6(5) . . . . ? C14 C13 N3 Cu1 -2.4(8) . . . . ? C11 N2 N3 C13 -0.3(8) . . . . ? C10 N2 N3 C13 -179.9(6) . . . . ? C11 N2 N3 Cu1 179.7(6) . . . . ? C10 N2 N3 Cu1 0.0(11) . . . . ? N8 Cu1 N3 C13 -179.7(5) . . . . ? O1W Cu1 N3 C13 90.4(5) . . . . ? N4 Cu1 N3 C13 0.8(4) . . . . ? N7 Cu1 N3 C13 -96.7(5) . . . . ? N8 Cu1 N3 N2 0.4(8) . . . . ? O1W Cu1 N3 N2 -89.5(8) . . . . ? N4 Cu1 N3 N2 -179.1(8) . . . . ? N7 Cu1 N3 N2 83.4(8) . . . . ? C17 C18 N4 C14 0.0(9) . . . . ? C17 C18 N4 Cu1 -175.4(5) . . . . ? C15 C14 N4 C18 -0.1(9) . . . . ? C13 C14 N4 C18 -178.3(5) . . . . ? C15 C14 N4 Cu1 175.7(5) . . . . ? C13 C14 N4 Cu1 -2.5(7) . . . . ? N8 Cu1 N4 C18 163(5) . . . . ? O1W Cu1 N4 C18 81.8(5) . . . . ? N7 Cu1 N4 C18 -75.5(5) . . . . ? N3 Cu1 N4 C18 176.4(5) . . . . ? N8 Cu1 N4 C14 -13(6) . . . . ? O1W Cu1 N4 C14 -93.7(4) . . . . ? N7 Cu1 N4 C14 109.0(4) . . . . ? N3 Cu1 N4 C14 0.9(4) . . . . ? C20 C19 N5 C26 -1.0(10) . . . . ? C25 C26 N5 C19 -177.9(6) . . . . ? C27 C26 N5 C19 2.3(10) . . . . ? C30 C29 N6 N7 -2.0(9) . . . . ? C30 C29 N6 C28 176.4(7) . . . . ? C25 C28 N6 C29 108.4(8) . . . . ? C25 C28 N6 N7 -73.4(8) . . . . ? C30 C31 N7 N6 -0.8(8) . . . . ? C32 C31 N7 N6 178.5(6) . . . . ? C30 C31 N7 Cu1 -179.0(5) . . . . ? C32 C31 N7 Cu1 0.3(7) . . . . ? C29 N6 N7 C31 1.7(8) . . . . ? C28 N6 N7 C31 -176.8(6) . . . . ? C29 N6 N7 Cu1 179.0(6) . . . . ? C28 N6 N7 Cu1 0.6(11) . . . . ? N8 Cu1 N7 C31 -0.5(4) . . . . ? O1W Cu1 N7 C31 65.8(7) . . . . ? N4 Cu1 N7 C31 -178.7(4) . . . . ? N3 Cu1 N7 C31 -97.4(4) . . . . ? N8 Cu1 N7 N6 -177.8(7) . . . . ? O1W Cu1 N7 N6 -111.4(7) . . . . ? N4 Cu1 N7 N6 4.0(7) . . . . ? N3 Cu1 N7 N6 85.4(7) . . . . ? C35 C36 N8 C32 -0.8(10) . . . . ? C35 C36 N8 Cu1 179.3(5) . . . . ? C33 C32 N8 C36 0.2(10) . . . . ? C31 C32 N8 C36 179.4(6) . . . . ? C33 C32 N8 Cu1 -180.0(5) . . . . ? C31 C32 N8 Cu1 -0.8(7) . . . . ? O1W Cu1 N8 C36 23.6(6) . . . . ? N4 Cu1 N8 C36 -58(6) . . . . ? N7 Cu1 N8 C36 -179.4(6) . . . . ? N3 Cu1 N8 C36 -70.9(6) . . . . ? O1W Cu1 N8 C32 -156.2(5) . . . . ? N4 Cu1 N8 C32 123(6) . . . . ? N7 Cu1 N8 C32 0.7(4) . . . . ? N3 Cu1 N8 C32 109.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.731 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.076 #===END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H42 Cd N12 O2, 2(Cl O4), 2.5(H2 O)' _chemical_formula_sum 'C54 H47 Cd Cl2 N12 O10.50' _chemical_formula_structural 'Cd 2+, 3(C18 H14 N4), 2(Cl O4 -), 2.5(H2 O)' _chemical_formula_weight 1215.34 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' 'Cd' 'Cd' -0.8075 1.2024 '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 12.485(5) _cell_length_b 15.142(6) _cell_length_c 15.190(6) _cell_angle_alpha 83.104(7) _cell_angle_beta 75.796(7) _cell_angle_gamma 79.584(7) _cell_volume 2729.4(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1054 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 22.79 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1242 _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.784585 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details '(SADABS; bruker, 1996)' _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 'BRUKER CCD AREA-DETECTOR' _diffrn_measurement_method '\F AND \W SCANS' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15859 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.46 _reflns_number_total 11083 _reflns_number_gt 6355 _reflns_threshold_expression I>2s\(I) _computing_data_collection 'SMART, BRUKER 1998' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT, BRUKER 1998' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997A)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997A)' _computing_molecular_graphics 'SHELXTL SHELDRICK, 1997B' _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^)+(0.0744P)^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 11083 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1310 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1646 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Cd1 Cd 0.63734(3) 0.63670(3) 0.71542(3) 0.04975(15) Uani 1 1 d . . . C1 C 0.8372(5) 0.5764(4) 0.8348(4) 0.0727(17) Uani 1 1 d . . . H1A H 0.8276 0.6383 0.8389 0.087 Uiso 1 1 calc R . . C2 C 0.9161(6) 0.5230(5) 0.8737(5) 0.085(2) Uani 1 1 d . . . H2A H 0.9578 0.5476 0.9047 0.101 Uiso 1 1 calc R . . C3 C 0.9326(6) 0.4308(5) 0.8660(5) 0.0800(19) Uani 1 1 d . . . H3A H 0.9874 0.3925 0.8899 0.096 Uiso 1 1 calc R . . C4 C 0.8667(5) 0.3976(4) 0.8226(4) 0.0656(16) Uani 1 1 d . . . H4A H 0.8758 0.3360 0.8171 0.079 Uiso 1 1 calc R . . C5 C 0.7855(4) 0.4562(4) 0.7865(3) 0.0527(13) Uani 1 1 d . . . C6 C 0.7093(4) 0.4234(3) 0.7435(3) 0.0499(13) Uani 1 1 d . . . C7 C 0.6949(5) 0.3356(4) 0.7362(4) 0.0620(16) Uani 1 1 d . . . H7A H 0.7360 0.2827 0.7559 0.074 Uiso 1 1 calc R . . C8 C 0.6085(5) 0.3431(4) 0.6943(4) 0.0625(15) Uani 1 1 d . . . H8A H 0.5784 0.2960 0.6808 0.075 Uiso 1 1 calc R . . C9 C 0.4819(5) 0.4741(4) 0.6357(4) 0.0580(14) Uani 1 1 d . . . H9A H 0.4613 0.4301 0.6041 0.070 Uiso 1 1 calc R . . H9B H 0.5059 0.5223 0.5911 0.070 Uiso 1 1 calc R . . C10 C 0.3810(5) 0.5120(3) 0.7051(3) 0.0485(12) Uani 1 1 d . . . C11 C 0.3684(5) 0.4934(4) 0.7975(4) 0.0612(15) Uani 1 1 d . . . H11A H 0.4248 0.4550 0.8195 0.073 Uiso 1 1 calc R . . C12 C 0.2736(6) 0.5305(4) 0.8590(4) 0.0687(17) Uani 1 1 d . . . H12A H 0.2665 0.5160 0.9212 0.082 Uiso 1 1 calc R . . C13 C 0.1919(5) 0.5872(4) 0.8286(4) 0.0683(17) Uani 1 1 d . . . H13A H 0.1306 0.6138 0.8706 0.082 Uiso 1 1 calc R . . C14 C 0.1968(5) 0.6073(4) 0.7354(4) 0.0608(15) Uani 1 1 d . . . C15 C 0.1134(5) 0.6640(4) 0.6994(5) 0.0781(19) Uani 1 1 d . . . H15A H 0.0488 0.6904 0.7382 0.094 Uiso 1 1 calc R . . C16 C 0.1271(6) 0.6804(5) 0.6080(5) 0.0813(19) Uani 1 1 d . . . H16A H 0.0725 0.7184 0.5835 0.098 Uiso 1 1 calc R . . C17 C 0.2247(6) 0.6391(4) 0.5510(4) 0.0730(17) Uani 1 1 d . . . H17A H 0.2317 0.6499 0.4885 0.088 Uiso 1 1 calc R . . C18 C 0.2931(5) 0.5685(3) 0.6728(4) 0.0516(13) Uani 1 1 d . . . C19 C 0.5169(6) 0.6271(4) 0.9343(4) 0.0671(16) Uani 1 1 d . . . H19A H 0.5832 0.5892 0.9387 0.080 Uiso 1 1 calc R . . C20 C 0.4385(6) 0.6456(5) 1.0127(4) 0.0754(19) Uani 1 1 d . . . H20A H 0.4505 0.6198 1.0688 0.091 Uiso 1 1 calc R . . C21 C 0.3434(6) 0.7019(5) 1.0069(4) 0.0723(18) Uani 1 1 d . . . H21A H 0.2898 0.7174 1.0594 0.087 Uiso 1 1 calc R . . C22 C 0.3262(5) 0.7368(4) 0.9219(4) 0.0604(15) Uani 1 1 d . . . H22A H 0.2602 0.7748 0.9167 0.072 Uiso 1 1 calc R . . C23 C 0.4076(4) 0.7147(3) 0.8457(3) 0.0476(12) Uani 1 1 d . . . C24 C 0.3930(5) 0.7475(3) 0.7539(3) 0.0491(13) Uani 1 1 d . . . C25 C 0.3041(5) 0.8039(4) 0.7272(4) 0.0635(15) Uani 1 1 d . . . H25A H 0.2398 0.8323 0.7649 0.076 Uiso 1 1 calc R . . C26 C 0.3301(5) 0.8092(4) 0.6355(4) 0.0665(16) Uani 1 1 d . . . H26A H 0.2859 0.8421 0.5980 0.080 Uiso 1 1 calc R . . C27 C 0.4929(5) 0.7474(4) 0.5154(3) 0.0567(14) Uani 1 1 d . . . H27A H 0.4414 0.7540 0.4756 0.068 Uiso 1 1 calc R . . H27B H 0.5339 0.6866 0.5130 0.068 Uiso 1 1 calc R . . C28 C 0.5736(5) 0.8126(3) 0.4806(3) 0.0531(13) Uani 1 1 d . . . C29 C 0.5818(5) 0.8801(4) 0.5286(4) 0.0623(15) Uani 1 1 d . . . H29A H 0.5332 0.8884 0.5852 0.075 Uiso 1 1 calc R . . C30 C 0.6612(6) 0.9376(4) 0.4956(5) 0.0766(18) Uani 1 1 d . . . H30A H 0.6656 0.9830 0.5301 0.092 Uiso 1 1 calc R . . C31 C 0.7323(6) 0.9266(4) 0.4119(5) 0.080(2) Uani 1 1 d . . . H31A H 0.7852 0.9648 0.3899 0.096 Uiso 1 1 calc R . . C32 C 0.7266(6) 0.8586(4) 0.3588(4) 0.0682(17) Uani 1 1 d . . . C33 C 0.7959(6) 0.8425(5) 0.2715(5) 0.093(2) Uani 1 1 d . . . H33A H 0.8512 0.8779 0.2464 0.111 Uiso 1 1 calc R . . C34 C 0.7832(7) 0.7768(6) 0.2244(5) 0.101(2) Uani 1 1 d . . . H34A H 0.8288 0.7665 0.1670 0.121 Uiso 1 1 calc R . . C35 C 0.6996(7) 0.7247(5) 0.2640(4) 0.092(2) Uani 1 1 d . . . H35A H 0.6904 0.6801 0.2306 0.111 Uiso 1 1 calc R . . C36 C 0.6455(5) 0.8014(4) 0.3930(4) 0.0607(15) Uani 1 1 d . . . C37 C 0.7743(6) 0.5868(4) 0.5080(4) 0.0732(18) Uani 1 1 d . . . H37A H 0.7295 0.5420 0.5199 0.088 Uiso 1 1 calc R . . C38 C 0.8508(6) 0.5899(5) 0.4265(4) 0.086(2) Uani 1 1 d . . . H38A H 0.8585 0.5482 0.3842 0.103 Uiso 1 1 calc R . . C39 C 0.9162(6) 0.6568(5) 0.4094(4) 0.087(2) Uani 1 1 d . . . H39A H 0.9697 0.6606 0.3549 0.104 Uiso 1 1 calc R . . C40 C 0.9027(5) 0.7179(4) 0.4722(4) 0.0688(17) Uani 1 1 d . . . H40A H 0.9452 0.7643 0.4603 0.083 Uiso 1 1 calc R . . C41 C 0.8247(5) 0.7096(3) 0.5538(3) 0.0520(13) Uani 1 1 d . . . C42 C 0.8096(4) 0.7697(3) 0.6258(3) 0.0489(13) Uani 1 1 d . . . C43 C 0.8630(5) 0.8422(4) 0.6275(4) 0.0673(16) Uani 1 1 d . . . H43A H 0.9155 0.8662 0.5805 0.081 Uiso 1 1 calc R . . C44 C 0.8222(6) 0.8706(4) 0.7125(4) 0.0715(17) Uani 1 1 d . . . H44A H 0.8430 0.9178 0.7351 0.086 Uiso 1 1 calc R . . C45 C 0.6810(5) 0.8263(4) 0.8506(4) 0.0592(15) Uani 1 1 d . . . H45A H 0.7220 0.8519 0.8852 0.071 Uiso 1 1 calc R . . H45B H 0.6712 0.7663 0.8784 0.071 Uiso 1 1 calc R . . C46 C 0.5690(5) 0.8825(3) 0.8569(4) 0.0593(15) Uani 1 1 d . . . C47 C 0.5328(6) 0.9274(4) 0.7844(5) 0.080(2) Uani 1 1 d . . . H47A H 0.5794 0.9229 0.7266 0.096 Uiso 1 1 calc R . . C48 C 0.4270(8) 0.9806(5) 0.7944(6) 0.104(3) Uani 1 1 d . . . H48A H 0.4037 1.0110 0.7438 0.125 Uiso 1 1 calc R . . C49 C 0.3576(7) 0.9875(5) 0.8804(7) 0.099(2) Uani 1 1 d . . . H49A H 0.2874 1.0227 0.8868 0.119 Uiso 1 1 calc R . . C50 C 0.3895(6) 0.9440(4) 0.9565(6) 0.0788(19) Uani 1 1 d . . . C51 C 0.3214(7) 0.9500(5) 1.0456(7) 0.100(3) Uani 1 1 d . . . H51A H 0.2500 0.9836 1.0552 0.120 Uiso 1 1 calc R . . C52 C 0.3612(8) 0.9065(6) 1.1163(6) 0.103(3) Uani 1 1 d . . . H52A H 0.3184 0.9106 1.1756 0.124 Uiso 1 1 calc R . . C53 C 0.4671(8) 0.8554(5) 1.0994(5) 0.095(2) Uani 1 1 d . . . H53A H 0.4926 0.8257 1.1494 0.114 Uiso 1 1 calc R . . C54 C 0.4961(5) 0.8908(4) 0.9464(4) 0.0623(16) Uani 1 1 d . . . N1 N 0.7727(4) 0.5453(3) 0.7909(3) 0.0544(11) Uani 1 1 d . . . N2 N 0.6340(4) 0.4823(3) 0.7070(3) 0.0495(10) Uani 1 1 d . . . N3 N 0.5751(4) 0.4315(3) 0.6761(3) 0.0529(11) Uani 1 1 d . . . N4 N 0.3067(4) 0.5864(3) 0.5795(3) 0.0606(12) Uani 1 1 d . . . N5 N 0.5033(4) 0.6608(3) 0.8512(3) 0.0497(11) Uani 1 1 d . . . N6 N 0.4708(4) 0.7204(3) 0.6807(3) 0.0472(10) Uani 1 1 d . . . N7 N 0.4291(4) 0.7599(3) 0.6079(3) 0.0532(11) Uani 1 1 d . . . N8 N 0.6329(5) 0.7341(3) 0.3453(3) 0.0734(14) Uani 1 1 d . . . N9 N 0.7602(4) 0.6445(3) 0.5714(3) 0.0548(11) Uani 1 1 d . . . N10 N 0.7379(4) 0.7555(3) 0.7066(3) 0.0493(10) Uani 1 1 d . . . N11 N 0.7469(4) 0.8191(3) 0.7581(3) 0.0558(11) Uani 1 1 d . . . N12 N 0.5344(5) 0.8456(3) 1.0183(4) 0.0726(14) Uani 1 1 d . . . O1 O 0.8409(11) 0.0713(6) 0.6683(6) 0.251(6) Uani 1 1 d . . . O1W O 0.9034(7) 0.1794(5) 0.8103(8) 0.227(5) Uani 1 1 d . . . O2 O 0.8587(8) 0.0796(6) 0.5150(6) 0.214(4) Uani 1 1 d . . . O2W O 0.6954(5) 0.6850(4) 0.0423(3) 0.1187(19) Uani 1 1 d . . . O3 O 0.7056(7) 0.1442(7) 0.6100(7) 0.218(4) Uani 1 1 d . . . O4 O 0.8638(6) 0.2004(4) 0.5926(5) 0.158(3) Uani 1 1 d . . . O5 O 0.9292(7) 0.7197(6) 0.9507(10) 0.277(7) Uani 1 1 d . . . O6 O 0.8795(6) 0.8617(4) 0.9847(5) 0.160(3) Uani 1 1 d . . . O7 O 1.0388(9) 0.7788(8) 1.0022(8) 0.260(5) Uani 1 1 d . . . O8 O 1.0241(12) 0.8209(7) 0.8717(7) 0.297(7) Uani 1 1 d . . . Cl1 Cl 0.82083(18) 0.12174(12) 0.59507(13) 0.0883(5) Uani 1 1 d . . . Cl2 Cl 0.96506(17) 0.79756(14) 0.95046(13) 0.0894(5) Uani 1 1 d . . . O3W O 0.9837(18) 0.9738(14) 0.145(3) 0.50(3) Uani 0.50 1 d P . . 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 Cd1 0.0500(3) 0.0495(2) 0.0470(2) -0.00254(16) -0.00802(17) -0.00569(17) C1 0.069(5) 0.064(4) 0.091(5) 0.003(3) -0.033(4) -0.011(3) C2 0.076(5) 0.096(6) 0.093(5) 0.004(4) -0.039(4) -0.023(4) C3 0.059(4) 0.084(5) 0.095(5) 0.018(4) -0.030(4) -0.006(4) C4 0.052(4) 0.062(4) 0.077(4) 0.005(3) -0.014(3) -0.004(3) C5 0.045(3) 0.055(3) 0.051(3) 0.004(3) -0.004(2) -0.005(3) C6 0.044(3) 0.054(3) 0.044(3) -0.007(2) -0.001(2) 0.000(3) C7 0.081(5) 0.045(3) 0.056(3) -0.005(3) -0.019(3) 0.005(3) C8 0.078(5) 0.048(3) 0.061(4) -0.011(3) -0.015(3) -0.005(3) C9 0.052(4) 0.068(4) 0.055(3) -0.012(3) -0.015(3) -0.006(3) C10 0.054(4) 0.045(3) 0.047(3) -0.003(2) -0.012(3) -0.012(2) C11 0.062(4) 0.061(4) 0.060(4) 0.000(3) -0.016(3) -0.009(3) C12 0.075(5) 0.076(4) 0.051(3) -0.009(3) -0.001(3) -0.016(4) C13 0.055(4) 0.078(4) 0.067(4) -0.012(3) 0.002(3) -0.016(3) C14 0.052(4) 0.068(4) 0.064(4) -0.012(3) -0.008(3) -0.016(3) C15 0.052(4) 0.081(5) 0.096(5) -0.013(4) -0.012(4) 0.000(3) C16 0.061(5) 0.089(5) 0.093(5) -0.008(4) -0.026(4) 0.003(4) C17 0.074(5) 0.080(4) 0.071(4) -0.002(3) -0.032(4) -0.011(4) C18 0.050(4) 0.054(3) 0.055(3) -0.004(3) -0.014(3) -0.014(3) C19 0.075(5) 0.075(4) 0.052(4) 0.004(3) -0.018(3) -0.015(3) C20 0.089(5) 0.100(5) 0.035(3) 0.003(3) -0.008(3) -0.022(4) C21 0.078(5) 0.090(5) 0.047(4) -0.011(3) 0.006(3) -0.033(4) C22 0.050(4) 0.069(4) 0.062(4) -0.015(3) -0.001(3) -0.017(3) C23 0.045(3) 0.051(3) 0.049(3) -0.006(2) -0.009(2) -0.013(3) C24 0.051(3) 0.046(3) 0.049(3) -0.008(2) -0.007(3) -0.010(2) C25 0.053(4) 0.068(4) 0.065(4) -0.012(3) -0.010(3) 0.004(3) C26 0.058(4) 0.070(4) 0.071(4) 0.001(3) -0.023(3) -0.001(3) C27 0.070(4) 0.063(3) 0.041(3) 0.000(3) -0.020(3) -0.015(3) C28 0.064(4) 0.054(3) 0.045(3) 0.005(3) -0.023(3) -0.010(3) C29 0.072(4) 0.060(4) 0.055(3) 0.001(3) -0.017(3) -0.014(3) C30 0.090(5) 0.060(4) 0.087(5) -0.001(3) -0.034(4) -0.011(4) C31 0.087(5) 0.071(4) 0.090(5) 0.020(4) -0.031(4) -0.034(4) C32 0.072(5) 0.068(4) 0.063(4) 0.014(3) -0.020(3) -0.015(3) C33 0.084(6) 0.103(6) 0.077(5) 0.026(4) -0.002(4) -0.022(4) C34 0.112(7) 0.112(6) 0.063(4) 0.003(4) 0.008(4) -0.024(5) C35 0.114(7) 0.108(6) 0.053(4) -0.011(4) -0.005(4) -0.028(5) C36 0.074(4) 0.062(4) 0.051(3) 0.011(3) -0.025(3) -0.016(3) C37 0.074(5) 0.083(4) 0.059(4) -0.016(3) 0.000(3) -0.019(3) C38 0.092(6) 0.106(5) 0.058(4) -0.028(4) 0.007(4) -0.031(4) C39 0.076(5) 0.121(6) 0.052(4) -0.009(4) 0.008(3) -0.015(4) C40 0.065(4) 0.089(4) 0.051(3) 0.001(3) -0.006(3) -0.022(3) C41 0.053(4) 0.056(3) 0.046(3) 0.003(3) -0.012(3) -0.009(3) C42 0.052(3) 0.048(3) 0.048(3) 0.006(2) -0.019(3) -0.005(2) C43 0.078(5) 0.062(4) 0.060(4) 0.005(3) -0.007(3) -0.023(3) C44 0.083(5) 0.053(4) 0.083(5) -0.006(3) -0.018(4) -0.025(3) C45 0.072(4) 0.056(3) 0.053(3) -0.010(3) -0.018(3) -0.010(3) C46 0.067(4) 0.046(3) 0.072(4) -0.011(3) -0.027(3) -0.009(3) C47 0.097(6) 0.072(4) 0.075(4) -0.022(4) -0.034(4) 0.008(4) C48 0.122(8) 0.084(5) 0.119(7) -0.026(5) -0.071(6) 0.025(5) C49 0.079(6) 0.088(5) 0.134(8) -0.045(5) -0.031(5) 0.011(4) C50 0.079(5) 0.059(4) 0.100(6) -0.024(4) -0.013(4) -0.014(4) C51 0.082(6) 0.078(5) 0.132(7) -0.044(5) 0.012(6) -0.017(4) C52 0.109(8) 0.088(6) 0.105(7) -0.029(5) 0.014(6) -0.034(5) C53 0.128(8) 0.083(5) 0.073(5) -0.010(4) -0.002(5) -0.038(5) C54 0.067(4) 0.048(3) 0.076(4) -0.019(3) -0.013(3) -0.016(3) N1 0.053(3) 0.051(3) 0.061(3) 0.000(2) -0.019(2) -0.007(2) N2 0.046(3) 0.049(2) 0.053(3) -0.006(2) -0.012(2) -0.006(2) N3 0.053(3) 0.057(3) 0.049(3) -0.009(2) -0.010(2) -0.007(2) N4 0.067(3) 0.061(3) 0.056(3) -0.004(2) -0.023(2) -0.005(2) N5 0.055(3) 0.053(3) 0.041(2) -0.003(2) -0.008(2) -0.012(2) N6 0.053(3) 0.048(2) 0.042(2) -0.0040(19) -0.013(2) -0.008(2) N7 0.053(3) 0.060(3) 0.047(3) -0.005(2) -0.012(2) -0.008(2) N8 0.091(4) 0.081(4) 0.048(3) -0.007(3) -0.010(3) -0.021(3) N9 0.057(3) 0.059(3) 0.048(3) -0.008(2) -0.009(2) -0.009(2) N10 0.053(3) 0.050(3) 0.047(2) -0.004(2) -0.014(2) -0.010(2) N11 0.065(3) 0.048(3) 0.056(3) -0.004(2) -0.015(2) -0.013(2) N12 0.093(4) 0.063(3) 0.059(3) -0.007(3) -0.006(3) -0.021(3) O1 0.421(17) 0.158(7) 0.199(9) 0.086(7) -0.153(10) -0.067(9) O1W 0.153(8) 0.129(6) 0.412(15) -0.045(7) -0.099(9) 0.003(5) O2 0.208(9) 0.219(8) 0.194(8) -0.120(7) 0.032(7) -0.018(7) O2W 0.156(6) 0.107(4) 0.095(4) 0.012(3) -0.044(4) -0.016(4) O3 0.090(6) 0.268(10) 0.303(11) -0.127(9) -0.015(6) -0.014(6) O4 0.165(7) 0.103(4) 0.199(7) -0.009(4) -0.003(5) -0.062(4) O5 0.130(7) 0.144(7) 0.56(2) -0.170(10) -0.013(9) -0.032(5) O6 0.130(6) 0.128(5) 0.198(7) -0.059(5) -0.017(5) 0.046(4) O7 0.159(9) 0.343(14) 0.303(13) -0.046(10) -0.132(9) 0.012(9) O8 0.357(16) 0.263(11) 0.152(8) 0.021(8) 0.107(9) 0.009(11) Cl1 0.1015(16) 0.0619(10) 0.0906(13) 0.0041(10) -0.0053(11) -0.0146(10) Cl2 0.0747(13) 0.0983(14) 0.0850(13) -0.0154(10) -0.0109(10) 0.0081(11) O3W 0.158(19) 0.196(19) 1.05(9) 0.33(4) -0.08(3) -0.083(15) _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 Cd1 N5 2.335(4) . ? Cd1 N10 2.347(4) . ? Cd1 N9 2.347(4) . ? Cd1 N2 2.366(4) . ? Cd1 N6 2.373(4) . ? Cd1 N1 2.411(4) . ? C1 N1 1.338(7) . ? C1 C2 1.363(9) . ? C1 H1A 0.9300 . ? C2 C3 1.389(9) . ? C2 H2A 0.9300 . ? C3 C4 1.363(9) . ? C3 H3A 0.9300 . ? C4 C5 1.396(8) . ? C4 H4A 0.9300 . ? C5 N1 1.336(6) . ? C5 C6 1.461(7) . ? C6 N2 1.349(6) . ? C6 C7 1.394(7) . ? C7 C8 1.362(8) . ? C7 H7A 0.9300 . ? C8 N3 1.344(6) . ? C8 H8A 0.9300 . ? C9 N3 1.460(7) . ? C9 C10 1.503(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.374(7) . ? C10 C18 1.415(7) . ? C11 C12 1.390(8) . ? C11 H11A 0.9300 . ? C12 C13 1.345(8) . ? C12 H12A 0.9300 . ? C13 C14 1.400(8) . ? C13 H13A 0.9300 . ? C14 C15 1.401(9) . ? C14 C18 1.419(8) . ? C15 C16 1.354(9) . ? C15 H15A 0.9300 . ? C16 C17 1.401(9) . ? C16 H16A 0.9300 . ? C17 N4 1.308(7) . ? C17 H17A 0.9300 . ? C18 N4 1.385(6) . ? C19 N5 1.343(7) . ? C19 C20 1.365(8) . ? C19 H19A 0.9300 . ? C20 C21 1.346(9) . ? C20 H20A 0.9300 . ? C21 C22 1.387(8) . ? C21 H21A 0.9300 . ? C22 C23 1.371(7) . ? C22 H22A 0.9300 . ? C23 N5 1.334(6) . ? C23 C24 1.465(7) . ? C24 N6 1.337(6) . ? C24 C25 1.386(7) . ? C25 C26 1.346(8) . ? C25 H25A 0.9300 . ? C26 N7 1.323(7) . ? C26 H26A 0.9300 . ? C27 N7 1.451(6) . ? C27 C28 1.497(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.357(7) . ? C28 C36 1.420(8) . ? C29 C30 1.398(8) . ? C29 H29A 0.9300 . ? C30 C31 1.370(9) . ? C30 H30A 0.9300 . ? C31 C32 1.404(9) . ? C31 H31A 0.9300 . ? C32 C36 1.412(8) . ? C32 C33 1.415(9) . ? C33 C34 1.346(10) . ? C33 H33A 0.9300 . ? C34 C35 1.397(10) . ? C34 H34A 0.9300 . ? C35 N8 1.317(8) . ? C35 H35A 0.9300 . ? C36 N8 1.372(7) . ? C37 N9 1.336(7) . ? C37 C38 1.367(8) . ? C37 H37A 0.9300 . ? C38 C39 1.375(9) . ? C38 H38A 0.9300 . ? C39 C40 1.368(8) . ? C39 H39A 0.9300 . ? C40 C41 1.385(7) . ? C40 H40A 0.9300 . ? C41 N9 1.344(6) . ? C41 C42 1.461(7) . ? C42 N10 1.349(6) . ? C42 C43 1.389(7) . ? C43 C44 1.358(8) . ? C43 H43A 0.9300 . ? C44 N11 1.336(7) . ? C44 H44A 0.9300 . ? C45 N11 1.449(7) . ? C45 C46 1.488(8) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.353(8) . ? C46 C54 1.444(8) . ? C47 C48 1.401(10) . ? C47 H47A 0.9300 . ? C48 C49 1.383(11) . ? C48 H48A 0.9300 . ? C49 C50 1.370(10) . ? C49 H49A 0.9300 . ? C50 C54 1.409(9) . ? C50 C51 1.414(10) . ? C51 C52 1.345(11) . ? C51 H51A 0.9300 . ? C52 C53 1.387(11) . ? C52 H52A 0.9300 . ? C53 N12 1.318(8) . ? C53 H53A 0.9300 . ? C54 N12 1.360(8) . ? N2 N3 1.345(6) . ? N6 N7 1.364(6) . ? N10 N11 1.348(5) . ? O1 Cl1 1.322(7) . ? O2 Cl1 1.381(7) . ? O3 Cl1 1.385(8) . ? O4 Cl1 1.384(6) . ? O5 Cl2 1.333(7) . ? O6 Cl2 1.353(6) . ? O7 Cl2 1.324(9) . ? O8 Cl2 1.288(8) . ? 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 N5 Cd1 N10 101.10(14) . . ? N5 Cd1 N9 168.03(14) . . ? N10 Cd1 N9 71.36(15) . . ? N5 Cd1 N2 99.32(14) . . ? N10 Cd1 N2 150.15(15) . . ? N9 Cd1 N2 91.28(14) . . ? N5 Cd1 N6 71.17(15) . . ? N10 Cd1 N6 99.06(14) . . ? N9 Cd1 N6 100.35(15) . . ? N2 Cd1 N6 108.04(14) . . ? N5 Cd1 N1 93.55(15) . . ? N10 Cd1 N1 87.16(15) . . ? N9 Cd1 N1 95.30(16) . . ? N2 Cd1 N1 70.01(15) . . ? N6 Cd1 N1 164.29(14) . . ? N1 C1 C2 124.0(6) . . ? N1 C1 H1A 118.0 . . ? C2 C1 H1A 118.0 . . ? C1 C2 C3 118.3(7) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 120.9 . . ? C4 C3 C2 118.6(6) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C3 C4 C5 119.8(6) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? N1 C5 C4 121.5(5) . . ? N1 C5 C6 116.8(5) . . ? C4 C5 C6 121.8(5) . . ? N2 C6 C7 109.6(5) . . ? N2 C6 C5 120.1(5) . . ? C7 C6 C5 130.2(5) . . ? C8 C7 C6 106.1(5) . . ? C8 C7 H7A 126.9 . . ? C6 C7 H7A 126.9 . . ? N3 C8 C7 107.1(5) . . ? N3 C8 H8A 126.4 . . ? C7 C8 H8A 126.4 . . ? N3 C9 C10 112.8(4) . . ? N3 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? N3 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C18 118.4(5) . . ? C11 C10 C9 123.9(5) . . ? C18 C10 C9 117.8(5) . . ? C10 C11 C12 121.6(6) . . ? C10 C11 H11A 119.2 . . ? C12 C11 H11A 119.2 . . ? C13 C12 C11 120.1(6) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 121.7(6) . . ? C12 C13 H13A 119.1 . . ? C14 C13 H13A 119.1 . . ? C13 C14 C15 124.5(6) . . ? C13 C14 C18 118.0(6) . . ? C15 C14 C18 117.4(6) . . ? C16 C15 C14 120.0(6) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 118.9(6) . . ? C15 C16 H16A 120.6 . . ? C17 C16 H16A 120.6 . . ? N4 C17 C16 124.7(6) . . ? N4 C17 H17A 117.7 . . ? C16 C17 H17A 117.7 . . ? N4 C18 C10 117.8(5) . . ? N4 C18 C14 122.1(5) . . ? C10 C18 C14 120.0(5) . . ? N5 C19 C20 123.4(6) . . ? N5 C19 H19A 118.3 . . ? C20 C19 H19A 118.3 . . ? C21 C20 C19 118.6(6) . . ? C21 C20 H20A 120.7 . . ? C19 C20 H20A 120.7 . . ? C20 C21 C22 119.4(6) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C23 C22 C21 119.2(6) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? N5 C23 C22 121.7(5) . . ? N5 C23 C24 116.6(4) . . ? C22 C23 C24 121.7(5) . . ? N6 C24 C25 110.0(5) . . ? N6 C24 C23 120.3(5) . . ? C25 C24 C23 129.6(5) . . ? C26 C25 C24 105.8(5) . . ? C26 C25 H25A 127.1 . . ? C24 C25 H25A 127.1 . . ? N7 C26 C25 108.5(5) . . ? N7 C26 H26A 125.8 . . ? C25 C26 H26A 125.8 . . ? N7 C27 C28 113.3(4) . . ? N7 C27 H27A 108.9 . . ? C28 C27 H27A 108.9 . . ? N7 C27 H27B 108.9 . . ? C28 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C29 C28 C36 119.1(5) . . ? C29 C28 C27 123.5(5) . . ? C36 C28 C27 117.4(5) . . ? C28 C29 C30 122.0(6) . . ? C28 C29 H29A 119.0 . . ? C30 C29 H29A 119.0 . . ? C31 C30 C29 119.4(6) . . ? C31 C30 H30A 120.3 . . ? C29 C30 H30A 120.3 . . ? C30 C31 C32 121.0(6) . . ? C30 C31 H31A 119.5 . . ? C32 C31 H31A 119.5 . . ? C31 C32 C36 118.7(6) . . ? C31 C32 C33 125.0(7) . . ? C36 C32 C33 116.3(6) . . ? C34 C33 C32 121.1(7) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? C33 C34 C35 118.1(7) . . ? C33 C34 H34A 121.0 . . ? C35 C34 H34A 121.0 . . ? N8 C35 C34 124.7(7) . . ? N8 C35 H35A 117.6 . . ? C34 C35 H35A 117.6 . . ? N8 C36 C32 122.7(6) . . ? N8 C36 C28 117.6(5) . . ? C32 C36 C28 119.7(5) . . ? N9 C37 C38 123.8(6) . . ? N9 C37 H37A 118.1 . . ? C38 C37 H37A 118.1 . . ? C37 C38 C39 117.6(6) . . ? C37 C38 H38A 121.2 . . ? C39 C38 H38A 121.2 . . ? C40 C39 C38 120.2(6) . . ? C40 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C39 C40 C41 118.9(6) . . ? C39 C40 H40A 120.6 . . ? C41 C40 H40A 120.6 . . ? N9 C41 C40 121.5(5) . . ? N9 C41 C42 116.7(5) . . ? C40 C41 C42 121.9(5) . . ? N10 C42 C43 110.3(5) . . ? N10 C42 C41 119.9(5) . . ? C43 C42 C41 129.8(5) . . ? C44 C43 C42 105.2(5) . . ? C44 C43 H43A 127.4 . . ? C42 C43 H43A 127.4 . . ? N11 C44 C43 108.2(5) . . ? N11 C44 H44A 125.9 . . ? C43 C44 H44A 125.9 . . ? N11 C45 C46 113.7(5) . . ? N11 C45 H45A 108.8 . . ? C46 C45 H45A 108.8 . . ? N11 C45 H45B 108.8 . . ? C46 C45 H45B 108.8 . . ? H45A C45 H45B 107.7 . . ? C47 C46 C54 118.5(6) . . ? C47 C46 C45 124.0(6) . . ? C54 C46 C45 117.5(5) . . ? C46 C47 C48 121.6(7) . . ? C46 C47 H47A 119.2 . . ? C48 C47 H47A 119.2 . . ? C49 C48 C47 119.3(7) . . ? C49 C48 H48A 120.4 . . ? C47 C48 H48A 120.4 . . ? C50 C49 C48 121.9(7) . . ? C50 C49 H49A 119.1 . . ? C48 C49 H49A 119.1 . . ? C49 C50 C54 118.8(7) . . ? C49 C50 C51 123.5(8) . . ? C54 C50 C51 117.7(8) . . ? C52 C51 C50 119.2(8) . . ? C52 C51 H51A 120.4 . . ? C50 C51 H51A 120.4 . . ? C51 C52 C53 118.9(8) . . ? C51 C52 H52A 120.6 . . ? C53 C52 H52A 120.6 . . ? N12 C53 C52 125.3(8) . . ? N12 C53 H53A 117.3 . . ? C52 C53 H53A 117.3 . . ? N12 C54 C50 122.6(6) . . ? N12 C54 C46 117.5(6) . . ? C50 C54 C46 119.9(6) . . ? C5 N1 C1 117.8(5) . . ? C5 N1 Cd1 116.7(4) . . ? C1 N1 Cd1 125.5(4) . . ? N3 N2 C6 105.6(4) . . ? N3 N2 Cd1 138.3(3) . . ? C6 N2 Cd1 116.1(3) . . ? C8 N3 N2 111.6(5) . . ? C8 N3 C9 128.1(5) . . ? N2 N3 C9 120.2(4) . . ? C17 N4 C18 116.8(5) . . ? C23 N5 C19 117.8(5) . . ? C23 N5 Cd1 117.3(3) . . ? C19 N5 Cd1 124.9(4) . . ? C24 N6 N7 105.1(4) . . ? C24 N6 Cd1 113.8(3) . . ? N7 N6 Cd1 140.7(3) . . ? C26 N7 N6 110.6(4) . . ? C26 N7 C27 128.4(5) . . ? N6 N7 C27 120.9(4) . . ? C35 N8 C36 117.1(6) . . ? C37 N9 C41 118.1(5) . . ? C37 N9 Cd1 124.9(4) . . ? C41 N9 Cd1 116.9(3) . . ? N11 N10 C42 105.2(4) . . ? N11 N10 Cd1 139.8(3) . . ? C42 N10 Cd1 115.1(3) . . ? C44 N11 N10 111.1(5) . . ? C44 N11 C45 127.3(5) . . ? N10 N11 C45 121.6(4) . . ? C53 N12 C54 116.4(7) . . ? O1 Cl1 O2 114.6(7) . . ? O1 Cl1 O4 106.9(6) . . ? O2 Cl1 O4 113.3(5) . . ? O1 Cl1 O3 106.1(7) . . ? O2 Cl1 O3 108.0(6) . . ? O4 Cl1 O3 107.5(5) . . ? O8 Cl2 O7 103.4(9) . . ? O8 Cl2 O5 111.7(8) . . ? O7 Cl2 O5 104.6(8) . . ? O8 Cl2 O6 114.3(6) . . ? O7 Cl2 O6 111.2(6) . . ? O5 Cl2 O6 111.0(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 N1 C1 C2 C3 1.5(11) . . . . ? C1 C2 C3 C4 -2.2(10) . . . . ? C2 C3 C4 C5 0.6(10) . . . . ? C3 C4 C5 N1 2.1(9) . . . . ? C3 C4 C5 C6 -176.9(5) . . . . ? N1 C5 C6 N2 2.8(7) . . . . ? C4 C5 C6 N2 -178.1(5) . . . . ? N1 C5 C6 C7 -173.4(5) . . . . ? C4 C5 C6 C7 5.7(9) . . . . ? N2 C6 C7 C8 -0.1(6) . . . . ? C5 C6 C7 C8 176.5(5) . . . . ? C6 C7 C8 N3 1.2(6) . . . . ? N3 C9 C10 C11 -12.4(8) . . . . ? N3 C9 C10 C18 169.0(5) . . . . ? C18 C10 C11 C12 -1.7(8) . . . . ? C9 C10 C11 C12 179.7(5) . . . . ? C10 C11 C12 C13 -1.0(9) . . . . ? C11 C12 C13 C14 3.1(10) . . . . ? C12 C13 C14 C15 178.4(6) . . . . ? C12 C13 C14 C18 -2.3(9) . . . . ? C13 C14 C15 C16 178.8(6) . . . . ? C18 C14 C15 C16 -0.4(9) . . . . ? C14 C15 C16 C17 0.6(10) . . . . ? C15 C16 C17 N4 -1.6(11) . . . . ? C11 C10 C18 N4 -179.7(5) . . . . ? C9 C10 C18 N4 -1.0(7) . . . . ? C11 C10 C18 C14 2.4(8) . . . . ? C9 C10 C18 C14 -178.9(5) . . . . ? C13 C14 C18 N4 -178.3(5) . . . . ? C15 C14 C18 N4 1.0(8) . . . . ? C13 C14 C18 C10 -0.4(8) . . . . ? C15 C14 C18 C10 178.9(5) . . . . ? N5 C19 C20 C21 -1.5(10) . . . . ? C19 C20 C21 C22 2.3(10) . . . . ? C20 C21 C22 C23 -1.4(9) . . . . ? C21 C22 C23 N5 -0.4(8) . . . . ? C21 C22 C23 C24 178.4(5) . . . . ? N5 C23 C24 N6 3.0(7) . . . . ? C22 C23 C24 N6 -175.9(5) . . . . ? N5 C23 C24 C25 -179.6(5) . . . . ? C22 C23 C24 C25 1.5(9) . . . . ? N6 C24 C25 C26 0.7(6) . . . . ? C23 C24 C25 C26 -176.9(5) . . . . ? C24 C25 C26 N7 -0.6(7) . . . . ? N7 C27 C28 C29 -3.7(8) . . . . ? N7 C27 C28 C36 175.5(5) . . . . ? C36 C28 C29 C30 -1.8(9) . . . . ? C27 C28 C29 C30 177.4(6) . . . . ? C28 C29 C30 C31 0.7(9) . . . . ? C29 C30 C31 C32 0.1(10) . . . . ? C30 C31 C32 C36 0.2(10) . . . . ? C30 C31 C32 C33 179.6(7) . . . . ? C31 C32 C33 C34 -178.6(7) . . . . ? C36 C32 C33 C34 0.7(10) . . . . ? C32 C33 C34 C35 -0.1(12) . . . . ? C33 C34 C35 N8 -1.1(13) . . . . ? C31 C32 C36 N8 179.0(6) . . . . ? C33 C32 C36 N8 -0.3(9) . . . . ? C31 C32 C36 C28 -1.4(9) . . . . ? C33 C32 C36 C28 179.3(5) . . . . ? C29 C28 C36 N8 -178.2(5) . . . . ? C27 C28 C36 N8 2.5(8) . . . . ? C29 C28 C36 C32 2.1(8) . . . . ? C27 C28 C36 C32 -177.2(5) . . . . ? N9 C37 C38 C39 -0.4(11) . . . . ? C37 C38 C39 C40 -0.7(11) . . . . ? C38 C39 C40 C41 1.7(10) . . . . ? C39 C40 C41 N9 -1.8(9) . . . . ? C39 C40 C41 C42 177.0(6) . . . . ? N9 C41 C42 N10 3.3(7) . . . . ? C40 C41 C42 N10 -175.6(5) . . . . ? N9 C41 C42 C43 -179.8(6) . . . . ? C40 C41 C42 C43 1.3(9) . . . . ? N10 C42 C43 C44 0.8(7) . . . . ? C41 C42 C43 C44 -176.4(5) . . . . ? C42 C43 C44 N11 -1.3(7) . . . . ? N11 C45 C46 C47 -3.5(8) . . . . ? N11 C45 C46 C54 177.9(4) . . . . ? C54 C46 C47 C48 -0.5(10) . . . . ? C45 C46 C47 C48 -179.0(6) . . . . ? C46 C47 C48 C49 0.0(11) . . . . ? C47 C48 C49 C50 0.3(12) . . . . ? C48 C49 C50 C54 -0.1(11) . . . . ? C48 C49 C50 C51 179.5(7) . . . . ? C49 C50 C51 C52 -178.4(8) . . . . ? C54 C50 C51 C52 1.1(10) . . . . ? C50 C51 C52 C53 -1.4(12) . . . . ? C51 C52 C53 N12 0.3(12) . . . . ? C49 C50 C54 N12 179.8(6) . . . . ? C51 C50 C54 N12 0.3(9) . . . . ? C49 C50 C54 C46 -0.4(9) . . . . ? C51 C50 C54 C46 -179.9(5) . . . . ? C47 C46 C54 N12 -179.6(5) . . . . ? C45 C46 C54 N12 -1.0(7) . . . . ? C47 C46 C54 C50 0.7(8) . . . . ? C45 C46 C54 C50 179.3(5) . . . . ? C4 C5 N1 C1 -2.9(8) . . . . ? C6 C5 N1 C1 176.2(5) . . . . ? C4 C5 N1 Cd1 175.7(4) . . . . ? C6 C5 N1 Cd1 -5.2(6) . . . . ? C2 C1 N1 C5 1.1(9) . . . . ? C2 C1 N1 Cd1 -177.4(5) . . . . ? N5 Cd1 N1 C5 102.9(4) . . . . ? N10 Cd1 N1 C5 -156.2(4) . . . . ? N9 Cd1 N1 C5 -85.2(4) . . . . ? N2 Cd1 N1 C5 4.2(3) . . . . ? N6 Cd1 N1 C5 89.9(6) . . . . ? N5 Cd1 N1 C1 -78.6(5) . . . . ? N10 Cd1 N1 C1 22.3(5) . . . . ? N9 Cd1 N1 C1 93.3(5) . . . . ? N2 Cd1 N1 C1 -177.3(5) . . . . ? N6 Cd1 N1 C1 -91.6(7) . . . . ? C7 C6 N2 N3 -1.1(5) . . . . ? C5 C6 N2 N3 -178.0(4) . . . . ? C7 C6 N2 Cd1 178.1(3) . . . . ? C5 C6 N2 Cd1 1.1(6) . . . . ? N5 Cd1 N2 N3 85.7(5) . . . . ? N10 Cd1 N2 N3 -141.7(4) . . . . ? N9 Cd1 N2 N3 -88.8(5) . . . . ? N6 Cd1 N2 N3 12.6(5) . . . . ? N1 Cd1 N2 N3 176.1(5) . . . . ? N5 Cd1 N2 C6 -93.1(4) . . . . ? N10 Cd1 N2 C6 39.6(5) . . . . ? N9 Cd1 N2 C6 92.5(4) . . . . ? N6 Cd1 N2 C6 -166.2(3) . . . . ? N1 Cd1 N2 C6 -2.7(3) . . . . ? C7 C8 N3 N2 -1.9(6) . . . . ? C7 C8 N3 C9 -176.8(5) . . . . ? C6 N2 N3 C8 1.9(5) . . . . ? Cd1 N2 N3 C8 -177.0(4) . . . . ? C6 N2 N3 C9 177.2(4) . . . . ? Cd1 N2 N3 C9 -1.7(7) . . . . ? C10 C9 N3 C8 101.8(6) . . . . ? C10 C9 N3 N2 -72.7(6) . . . . ? C16 C17 N4 C18 2.1(9) . . . . ? C10 C18 N4 C17 -179.7(5) . . . . ? C14 C18 N4 C17 -1.8(8) . . . . ? C22 C23 N5 C19 1.3(7) . . . . ? C24 C23 N5 C19 -177.6(4) . . . . ? C22 C23 N5 Cd1 -176.5(4) . . . . ? C24 C23 N5 Cd1 4.7(6) . . . . ? C20 C19 N5 C23 -0.3(8) . . . . ? C20 C19 N5 Cd1 177.2(5) . . . . ? N10 Cd1 N5 C23 89.3(4) . . . . ? N9 Cd1 N5 C23 39.5(9) . . . . ? N2 Cd1 N5 C23 -112.6(4) . . . . ? N6 Cd1 N5 C23 -6.6(3) . . . . ? N1 Cd1 N5 C23 177.1(4) . . . . ? N10 Cd1 N5 C19 -88.3(4) . . . . ? N9 Cd1 N5 C19 -138.1(7) . . . . ? N2 Cd1 N5 C19 69.9(4) . . . . ? N6 Cd1 N5 C19 175.9(4) . . . . ? N1 Cd1 N5 C19 -0.5(4) . . . . ? C25 C24 N6 N7 -0.5(6) . . . . ? C23 C24 N6 N7 177.4(4) . . . . ? C25 C24 N6 Cd1 173.4(4) . . . . ? C23 C24 N6 Cd1 -8.7(6) . . . . ? N5 Cd1 N6 C24 7.8(3) . . . . ? N10 Cd1 N6 C24 -90.9(3) . . . . ? N9 Cd1 N6 C24 -163.5(3) . . . . ? N2 Cd1 N6 C24 101.7(3) . . . . ? N1 Cd1 N6 C24 21.5(7) . . . . ? N5 Cd1 N6 N7 178.5(5) . . . . ? N10 Cd1 N6 N7 79.7(5) . . . . ? N9 Cd1 N6 N7 7.2(5) . . . . ? N2 Cd1 N6 N7 -87.6(5) . . . . ? N1 Cd1 N6 N7 -167.8(5) . . . . ? C25 C26 N7 N6 0.3(7) . . . . ? C25 C26 N7 C27 -177.9(5) . . . . ? C24 N6 N7 C26 0.1(6) . . . . ? Cd1 N6 N7 C26 -171.0(4) . . . . ? C24 N6 N7 C27 178.4(4) . . . . ? Cd1 N6 N7 C27 7.3(7) . . . . ? C28 C27 N7 C26 92.5(7) . . . . ? C28 C27 N7 N6 -85.6(6) . . . . ? C34 C35 N8 C36 1.5(11) . . . . ? C32 C36 N8 C35 -0.7(9) . . . . ? C28 C36 N8 C35 179.7(6) . . . . ? C38 C37 N9 C41 0.3(9) . . . . ? C38 C37 N9 Cd1 -176.3(5) . . . . ? C40 C41 N9 C37 0.8(8) . . . . ? C42 C41 N9 C37 -178.1(5) . . . . ? C40 C41 N9 Cd1 177.7(4) . . . . ? C42 C41 N9 Cd1 -1.2(6) . . . . ? N5 Cd1 N9 C37 -131.5(7) . . . . ? N10 Cd1 N9 C37 176.2(5) . . . . ? N2 Cd1 N9 C37 21.0(5) . . . . ? N6 Cd1 N9 C37 -87.6(5) . . . . ? N1 Cd1 N9 C37 91.1(5) . . . . ? N5 Cd1 N9 C41 51.9(9) . . . . ? N10 Cd1 N9 C41 -0.4(4) . . . . ? N2 Cd1 N9 C41 -155.6(4) . . . . ? N6 Cd1 N9 C41 95.8(4) . . . . ? N1 Cd1 N9 C41 -85.6(4) . . . . ? C43 C42 N10 N11 0.0(6) . . . . ? C41 C42 N10 N11 177.5(4) . . . . ? C43 C42 N10 Cd1 179.0(4) . . . . ? C41 C42 N10 Cd1 -3.6(6) . . . . ? N5 Cd1 N10 N11 10.1(5) . . . . ? N9 Cd1 N10 N11 -179.5(5) . . . . ? N2 Cd1 N10 N11 -122.2(5) . . . . ? N6 Cd1 N10 N11 82.5(5) . . . . ? N1 Cd1 N10 N11 -83.0(5) . . . . ? N5 Cd1 N10 C42 -168.3(3) . . . . ? N9 Cd1 N10 C42 2.1(3) . . . . ? N2 Cd1 N10 C42 59.4(5) . . . . ? N6 Cd1 N10 C42 -95.9(4) . . . . ? N1 Cd1 N10 C42 98.6(4) . . . . ? C43 C44 N11 N10 1.4(7) . . . . ? C43 C44 N11 C45 -178.9(5) . . . . ? C42 N10 N11 C44 -0.9(6) . . . . ? Cd1 N10 N11 C44 -179.4(4) . . . . ? C42 N10 N11 C45 179.4(5) . . . . ? Cd1 N10 N11 C45 0.9(8) . . . . ? C46 C45 N11 C44 93.5(7) . . . . ? C46 C45 N11 N10 -86.8(6) . . . . ? C52 C53 N12 C54 1.0(10) . . . . ? C50 C54 N12 C53 -1.3(8) . . . . ? C46 C54 N12 C53 178.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.729 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.075 #===END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H40 Cu2 N12 O2, 4(Cl O4), H2 O' _chemical_formula_sum 'C40 H42 Cl4 Cu2 N12 O19' _chemical_formula_structural '2(Cu 2+), 2(C20 H18 N4), 4(Cl O4 -), 3(H2 O)' _chemical_formula_weight 1263.74 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 Triclinic _symmetry_space_group_name_H-M 'p-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.791(4) _cell_length_b 13.923(7) _cell_length_c 19.756(9) _cell_angle_alpha 72.297(12) _cell_angle_beta 78.201(14) _cell_angle_gamma 68.683(13) _cell_volume 2619(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1052 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 22.89 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 1.100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.839177 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details '(sadabs; bruker, 1996)' _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 'bruker ccd area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14852 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.1992 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.41 _reflns_number_total 10543 _reflns_number_gt 4568 _reflns_threshold_expression I>2s\(I) _computing_data_collection 'SMART, BRUKER 1998' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT, BRUKER 1998' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997A)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997A)' _computing_molecular_graphics 'SHELXTL (SHELDRICK, 1997B)' _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^)+(0.2000P)^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 10543 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2458 _refine_ls_R_factor_gt 0.1352 _refine_ls_wR_factor_ref 0.3906 _refine_ls_wR_factor_gt 0.3250 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.52609(15) 0.57624(12) 0.26535(8) 0.0448(5) Uani 1 1 d . . . Cu2 Cu 1.07638(16) 0.09500(12) 0.26423(8) 0.0468(5) Uani 1 1 d . . . C1 C 0.6289(16) 0.7578(12) 0.2023(8) 0.071(4) Uani 1 1 d . . . H1A H 0.5958 0.7750 0.2459 0.085 Uiso 1 1 calc R . . C2 C 0.6847(18) 0.8242(14) 0.1508(10) 0.081(5) Uani 1 1 d . . . H2A H 0.6846 0.8875 0.1575 0.097 Uiso 1 1 calc R . . C3 C 0.740(2) 0.7953(17) 0.0898(11) 0.107(7) Uani 1 1 d . . . H3A H 0.7870 0.8352 0.0553 0.128 Uiso 1 1 calc R . . C4 C 0.7275(18) 0.7055(14) 0.0777(8) 0.082(5) Uani 1 1 d . . . H4A H 0.7605 0.6879 0.0342 0.098 Uiso 1 1 calc R . . C5 C 0.6662(14) 0.6446(12) 0.1309(8) 0.058(4) Uani 1 1 d . . . C6 C 0.6378(14) 0.5538(11) 0.1263(7) 0.057(4) Uani 1 1 d . . . C7 C 0.6481(17) 0.5136(16) 0.0661(8) 0.084(5) Uani 1 1 d . . . H7A H 0.6743 0.5408 0.0184 0.101 Uiso 1 1 calc R . . C8 C 0.6081(19) 0.4216(15) 0.0977(10) 0.087(6) Uani 1 1 d . . . H8A H 0.6077 0.3728 0.0744 0.105 Uiso 1 1 calc R . . C9 C 0.5181(15) 0.3372(11) 0.2143(8) 0.064(4) Uani 1 1 d . . . H9A H 0.4871 0.3047 0.1869 0.076 Uiso 1 1 calc R . . H9B H 0.4407 0.3731 0.2429 0.076 Uiso 1 1 calc R . . C10 C 0.6112(14) 0.2509(9) 0.2635(8) 0.057(4) Uani 1 1 d . . . H10A H 0.6496 0.2708 0.2929 0.068 Uiso 1 1 calc R . . C11 C 0.6420(13) 0.1526(10) 0.2684(8) 0.053(3) Uani 1 1 d . . . H11A H 0.6064 0.1359 0.2361 0.064 Uiso 1 1 calc R . . C12 C 0.7281(15) 0.0579(11) 0.3190(10) 0.074(5) Uani 1 1 d . . . H12A H 0.6740 0.0146 0.3479 0.089 Uiso 1 1 calc R . . H12B H 0.7991 0.0147 0.2913 0.089 Uiso 1 1 calc R . . C13 C 0.7350(16) 0.1062(12) 0.4307(10) 0.076(5) Uani 1 1 d . . . H13A H 0.6516 0.1037 0.4538 0.092 Uiso 1 1 calc R . . C14 C 0.8259(16) 0.1288(12) 0.4563(8) 0.067(4) Uani 1 1 d . . . H14A H 0.8182 0.1442 0.4999 0.081 Uiso 1 1 calc R . . C15 C 0.9360(13) 0.1240(9) 0.4018(6) 0.044(3) Uani 1 1 d . . . C16 C 1.0662(14) 0.1333(9) 0.3984(7) 0.047(3) Uani 1 1 d . . . C17 C 1.1066(18) 0.1514(10) 0.4571(7) 0.064(4) Uani 1 1 d . . . H17A H 1.0475 0.1617 0.4977 0.076 Uiso 1 1 calc R . . C18 C 1.230(2) 0.1530(11) 0.4521(10) 0.075(5) Uani 1 1 d . . . H18A H 1.2600 0.1579 0.4913 0.090 Uiso 1 1 calc R . . C19 C 1.3177(19) 0.1475(12) 0.3873(11) 0.079(5) Uani 1 1 d . . . H19A H 1.4025 0.1530 0.3826 0.095 Uiso 1 1 calc R . . C20 C 1.2704(13) 0.1336(11) 0.3321(8) 0.058(4) Uani 1 1 d . . . H20A H 1.3253 0.1290 0.2895 0.069 Uiso 1 1 calc R . . C21 C 1.0073(19) -0.0409(13) 0.1997(9) 0.081(5) Uani 1 1 d . . . H21A H 1.0319 -0.0934 0.2414 0.097 Uiso 1 1 calc R . . C22 C 0.962(2) -0.0650(14) 0.1472(10) 0.086(6) Uani 1 1 d . . . H22A H 0.9631 -0.1339 0.1522 0.104 Uiso 1 1 calc R . . C23 C 0.916(2) 0.0157(16) 0.0875(10) 0.099(7) Uani 1 1 d . . . H23A H 0.8825 0.0019 0.0528 0.118 Uiso 1 1 calc R . . C24 C 0.9195(19) 0.1182(16) 0.0798(9) 0.092(6) Uani 1 1 d . . . H24A H 0.8882 0.1740 0.0408 0.110 Uiso 1 1 calc R . . C25 C 0.9724(15) 0.1326(11) 0.1335(7) 0.056(4) Uani 1 1 d . . . C26 C 0.9870(15) 0.2327(11) 0.1307(6) 0.055(4) Uani 1 1 d . . . C27 C 0.9738(17) 0.3249(14) 0.0773(9) 0.083(5) Uani 1 1 d . . . H27A H 0.9463 0.3387 0.0326 0.099 Uiso 1 1 calc R . . C28 C 1.013(2) 0.4010(13) 0.1046(8) 0.093(6) Uani 1 1 d . . . H28A H 1.0136 0.4702 0.0830 0.112 Uiso 1 1 calc R . . C29 C 1.0899(13) 0.3742(9) 0.2204(7) 0.050(3) Uani 1 1 d . . . H29A H 1.1336 0.4261 0.1932 0.060 Uiso 1 1 calc R . . H29B H 1.1550 0.3147 0.2483 0.060 Uiso 1 1 calc R . . C30 C 0.9770(13) 0.4237(10) 0.2698(7) 0.050(3) Uani 1 1 d . . . H30A H 0.9237 0.3836 0.2981 0.060 Uiso 1 1 calc R . . C31 C 0.9500(12) 0.5187(10) 0.2752(8) 0.053(3) Uani 1 1 d . . . H31A H 1.0000 0.5589 0.2435 0.064 Uiso 1 1 calc R . . C32 C 0.8437(13) 0.5735(11) 0.3285(8) 0.057(4) Uani 1 1 d . . . H32A H 0.8879 0.5898 0.3596 0.068 Uiso 1 1 calc R . . H32B H 0.7857 0.6402 0.3023 0.068 Uiso 1 1 calc R . . C33 C 0.7833(16) 0.4452(13) 0.4356(8) 0.065(4) Uani 1 1 d . . . H33A H 0.8541 0.4329 0.4606 0.078 Uiso 1 1 calc R . . C34 C 0.6866(16) 0.4007(11) 0.4591(7) 0.059(4) Uani 1 1 d . . . H34A H 0.6778 0.3509 0.5020 0.070 Uiso 1 1 calc R . . C35 C 0.6029(12) 0.4448(10) 0.4058(7) 0.044(3) Uani 1 1 d . . . C36 C 0.4731(13) 0.4379(10) 0.3998(6) 0.046(3) Uani 1 1 d . . . C37 C 0.4090(14) 0.3816(10) 0.4562(7) 0.052(3) Uani 1 1 d . . . H37A H 0.4480 0.3451 0.4986 0.063 Uiso 1 1 calc R . . C38 C 0.2849(17) 0.3804(11) 0.4485(8) 0.066(4) Uani 1 1 d . . . H38A H 0.2393 0.3420 0.4853 0.080 Uiso 1 1 calc R . . C39 C 0.2317(15) 0.4362(12) 0.3864(9) 0.064(4) Uani 1 1 d . . . H39A H 0.1471 0.4385 0.3808 0.077 Uiso 1 1 calc R . . C40 C 0.3023(13) 0.4900(11) 0.3310(7) 0.054(3) Uani 1 1 d . . . H40A H 0.2637 0.5286 0.2887 0.064 Uiso 1 1 calc R . . Cl1 Cl 0.4230(7) 0.1524(5) 0.1115(3) 0.113(2) Uani 1 1 d . . . Cl2 Cl 0.2056(5) 0.6311(4) 0.1049(2) 0.0883(14) Uani 1 1 d . . . Cl3 Cl 0.5116(3) 0.8560(2) 0.38274(15) 0.0455(7) Uani 1 1 d . . . Cl4 Cl 0.0360(3) 0.7323(2) 0.38149(16) 0.0464(7) Uani 1 1 d . . . N1 N 0.6187(10) 0.6698(8) 0.1946(5) 0.048(3) Uani 1 1 d . . . N2 N 0.5900(10) 0.4950(7) 0.1847(5) 0.039(2) Uani 1 1 d . . . N3 N 0.5730(11) 0.4183(8) 0.1638(6) 0.053(3) Uani 1 1 d . . . N4 N 0.7870(11) 0.0881(9) 0.3658(7) 0.059(3) Uani 1 1 d . . . N5 N 0.9084(9) 0.1004(8) 0.3477(6) 0.045(2) Uani 1 1 d . . . N6 N 1.1455(9) 0.1265(7) 0.3384(5) 0.040(2) Uani 1 1 d . . . N7 N 1.0158(12) 0.0548(9) 0.1915(5) 0.055(3) Uani 1 1 d . . . N8 N 1.0329(10) 0.2398(7) 0.1870(5) 0.043(2) Uani 1 1 d . . . N9 N 1.0456(11) 0.3363(9) 0.1706(6) 0.056(3) Uani 1 1 d . . . N10 N 0.7627(11) 0.5091(9) 0.3719(7) 0.056(3) Uani 1 1 d . . . N11 N 0.6512(9) 0.5133(7) 0.3502(5) 0.039(2) Uani 1 1 d . . . N12 N 0.4270(9) 0.4878(7) 0.3368(5) 0.041(2) Uani 1 1 d . . . O1 O 0.553(3) 0.121(4) 0.113(2) 0.36(3) Uani 1 1 d . . . O2 O 0.408(5) 0.111(3) 0.1768(12) 0.34(2) Uani 1 1 d . . . O3 O 0.413(4) 0.117(3) 0.0624(15) 0.32(2) Uani 1 1 d . . . O4 O 0.363(3) 0.251(2) 0.109(2) 0.277(18) Uani 1 1 d . . . O5 O 0.265(2) 0.6861(16) 0.0448(8) 0.167(8) Uani 1 1 d . . . O6 O 0.078(2) 0.655(3) 0.1010(13) 0.30(2) Uani 1 1 d . . . O7 O 0.262(3) 0.530(2) 0.111(2) 0.32(2) Uani 1 1 d . . . O8 O 0.202(3) 0.646(3) 0.1666(12) 0.274(18) Uani 1 1 d . . . O9 O 0.6050(16) 0.7532(9) 0.3815(6) 0.122(6) Uani 1 1 d . . . O10 O 0.5228(12) 0.9271(8) 0.3147(5) 0.080(3) Uani 1 1 d . . . O11 O 0.5433(11) 0.8905(9) 0.4372(5) 0.082(3) Uani 1 1 d . . . O12 O 0.3788(13) 0.8545(14) 0.3985(7) 0.120(5) Uani 1 1 d . . . O13 O 0.1633(13) 0.7219(13) 0.3953(7) 0.120(5) Uani 1 1 d . . . O14 O -0.0104(11) 0.6565(8) 0.4371(5) 0.079(3) Uani 1 1 d . . . O15 O -0.0464(17) 0.8381(9) 0.3777(6) 0.119(5) Uani 1 1 d . . . O16 O 0.0504(12) 0.7112(8) 0.3141(5) 0.077(3) Uani 1 1 d . . . O1W O 0.3713(11) 0.7087(7) 0.2725(7) 0.088(4) Uani 1 1 d . . . O2W O 1.2180(11) -0.0479(8) 0.2798(7) 0.084(4) Uani 1 1 d . . . O3W O 0.683(3) 0.094(3) 0.9648(13) 0.163(17) Uani 0.50 1 d P . . O4W O 0.336(4) 0.881(4) 0.1571(14) 0.25(3) Uani 0.50 1 d P . . 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 0.0512(10) 0.0418(9) 0.0413(9) -0.0071(7) 0.0025(7) -0.0215(7) Cu2 0.0594(10) 0.0449(9) 0.0421(9) -0.0134(7) -0.0147(7) -0.0170(8) C1 0.082(11) 0.074(11) 0.071(10) -0.016(8) 0.008(9) -0.053(9) C2 0.089(13) 0.088(12) 0.082(12) -0.030(10) 0.008(10) -0.050(11) C3 0.144(19) 0.102(15) 0.088(14) -0.006(12) 0.014(13) -0.083(15) C4 0.104(14) 0.094(13) 0.047(9) -0.006(8) 0.010(9) -0.051(11) C5 0.052(8) 0.070(10) 0.058(9) -0.023(7) 0.002(7) -0.026(7) C6 0.053(8) 0.062(9) 0.047(8) -0.018(7) -0.009(7) -0.001(7) C7 0.095(13) 0.115(15) 0.052(9) -0.050(10) 0.027(9) -0.042(11) C8 0.100(14) 0.088(13) 0.097(14) -0.072(11) -0.009(11) -0.019(11) C9 0.063(9) 0.055(9) 0.078(10) -0.019(8) -0.012(8) -0.020(7) C10 0.064(9) 0.026(6) 0.089(10) -0.021(6) -0.027(8) -0.008(6) C11 0.043(7) 0.048(8) 0.074(9) -0.013(7) -0.007(7) -0.022(6) C12 0.051(9) 0.048(8) 0.142(15) -0.032(9) -0.011(9) -0.030(7) C13 0.056(10) 0.063(10) 0.086(12) -0.006(9) 0.023(9) -0.019(8) C14 0.067(10) 0.065(10) 0.055(9) -0.013(7) 0.013(8) -0.016(8) C15 0.062(8) 0.044(7) 0.025(6) -0.006(5) -0.003(6) -0.018(6) C16 0.070(9) 0.029(6) 0.045(7) 0.008(5) -0.039(7) -0.016(6) C17 0.103(13) 0.049(8) 0.047(8) -0.009(6) -0.031(8) -0.023(8) C18 0.108(14) 0.053(9) 0.085(12) -0.026(8) -0.051(11) -0.020(9) C19 0.084(12) 0.048(9) 0.110(15) -0.012(9) -0.048(12) -0.012(8) C20 0.041(8) 0.072(9) 0.073(10) -0.034(8) -0.010(7) -0.019(7) C21 0.127(15) 0.063(10) 0.081(11) -0.005(8) -0.035(11) -0.062(11) C22 0.118(15) 0.069(11) 0.105(14) -0.027(10) -0.025(12) -0.058(11) C23 0.146(18) 0.109(15) 0.094(13) -0.030(12) -0.055(13) -0.076(14) C24 0.098(14) 0.111(15) 0.077(12) -0.015(10) -0.056(11) -0.028(12) C25 0.066(9) 0.060(9) 0.044(8) -0.024(7) -0.011(7) -0.011(7) C26 0.080(10) 0.054(8) 0.031(7) -0.003(6) -0.018(7) -0.022(7) C27 0.085(12) 0.086(12) 0.065(10) 0.004(9) -0.030(9) -0.020(10) C28 0.145(17) 0.057(10) 0.036(8) 0.001(7) -0.023(10) 0.012(10) C29 0.051(8) 0.029(6) 0.071(9) -0.015(6) 0.002(7) -0.016(6) C30 0.045(7) 0.052(8) 0.060(8) -0.013(6) -0.005(6) -0.025(6) C31 0.033(7) 0.039(7) 0.093(11) -0.024(7) -0.014(7) -0.009(6) C32 0.047(8) 0.058(8) 0.075(10) -0.029(7) -0.008(7) -0.017(7) C33 0.069(10) 0.077(11) 0.047(9) -0.031(8) -0.023(8) 0.001(9) C34 0.073(10) 0.057(9) 0.047(8) -0.017(7) -0.024(7) -0.010(8) C35 0.044(7) 0.046(7) 0.050(7) -0.011(6) -0.020(6) -0.014(6) C36 0.059(8) 0.046(7) 0.039(7) -0.015(6) 0.009(6) -0.026(6) C37 0.059(9) 0.054(8) 0.045(7) -0.007(6) -0.007(6) -0.022(7) C38 0.084(11) 0.045(8) 0.071(10) -0.023(8) 0.027(9) -0.034(8) C39 0.047(8) 0.059(9) 0.090(12) -0.030(9) -0.002(8) -0.015(7) C40 0.043(8) 0.064(9) 0.052(8) -0.005(7) -0.015(6) -0.017(7) Cl1 0.139(5) 0.107(4) 0.073(3) -0.040(3) -0.045(3) 0.016(4) Cl2 0.094(3) 0.076(3) 0.056(3) -0.002(2) -0.006(2) 0.003(2) Cl3 0.0513(18) 0.0461(17) 0.0384(16) -0.0075(13) -0.0097(14) -0.0147(14) Cl4 0.0519(19) 0.0491(18) 0.0395(16) -0.0119(14) -0.0012(14) -0.0191(15) N1 0.057(7) 0.047(6) 0.044(6) -0.014(5) 0.013(5) -0.027(5) N2 0.048(6) 0.026(5) 0.044(6) -0.007(4) -0.007(5) -0.013(4) N3 0.054(7) 0.047(6) 0.061(7) -0.014(6) -0.013(6) -0.016(5) N4 0.039(6) 0.050(7) 0.077(9) 0.002(6) -0.007(6) -0.017(5) N5 0.029(5) 0.038(6) 0.061(7) -0.007(5) 0.003(5) -0.011(4) N6 0.032(5) 0.045(6) 0.054(6) -0.030(5) -0.005(5) -0.008(4) N7 0.072(8) 0.061(7) 0.045(6) -0.003(5) -0.028(6) -0.032(6) N8 0.047(6) 0.025(5) 0.052(6) -0.006(4) -0.002(5) -0.008(4) N9 0.057(7) 0.050(7) 0.069(8) -0.014(6) 0.003(6) -0.032(6) N10 0.041(6) 0.063(7) 0.076(8) -0.039(7) -0.012(6) -0.010(6) N11 0.035(5) 0.038(5) 0.052(6) -0.024(5) -0.008(5) -0.010(4) N12 0.034(5) 0.040(5) 0.047(6) 0.001(5) -0.003(4) -0.021(4) O1 0.109(19) 0.57(7) 0.36(5) -0.26(5) -0.06(3) 0.08(3) O2 0.42(6) 0.37(5) 0.092(17) 0.02(2) -0.04(2) -0.04(4) O3 0.57(6) 0.31(4) 0.19(2) -0.01(2) -0.18(3) -0.22(4) O4 0.20(2) 0.18(2) 0.48(5) -0.17(3) -0.14(3) 0.036(19) O5 0.193(18) 0.200(18) 0.077(10) 0.028(11) 0.016(11) -0.096(16) O6 0.098(15) 0.43(4) 0.22(2) 0.13(3) -0.077(16) -0.05(2) O7 0.27(3) 0.123(18) 0.42(5) 0.01(2) 0.16(3) -0.07(2) O8 0.25(3) 0.54(6) 0.112(16) -0.11(2) 0.032(17) -0.23(4) O9 0.178(14) 0.064(7) 0.047(6) -0.014(5) 0.001(7) 0.045(8) O10 0.117(9) 0.066(7) 0.048(6) 0.006(5) -0.011(6) -0.034(6) O11 0.089(8) 0.111(9) 0.059(6) -0.026(6) -0.023(6) -0.036(7) O12 0.091(9) 0.218(17) 0.106(10) -0.067(10) 0.016(8) -0.105(11) O13 0.085(9) 0.205(16) 0.098(9) -0.002(10) -0.018(7) -0.104(11) O14 0.087(8) 0.080(7) 0.063(7) 0.006(6) 0.007(6) -0.045(6) O15 0.186(14) 0.057(7) 0.062(7) -0.015(6) 0.003(8) 0.013(8) O16 0.113(9) 0.074(7) 0.048(6) -0.020(5) -0.004(6) -0.032(7) O1W 0.079(7) 0.035(5) 0.127(10) -0.013(6) 0.025(7) -0.017(5) O2W 0.073(7) 0.062(6) 0.126(10) -0.044(6) -0.048(7) 0.005(5) O3W 0.061(16) 0.29(4) 0.057(15) -0.04(2) 0.007(13) 0.02(2) O4W 0.15(3) 0.28(5) 0.055(16) 0.05(2) 0.042(18) 0.11(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 N1 1.980(10) . ? Cu1 N12 1.984(9) . ? Cu1 O1W 2.009(10) . ? Cu1 N2 2.091(10) . ? Cu1 N11 2.138(9) . ? Cu2 N7 1.985(10) . ? Cu2 N6 1.993(9) . ? Cu2 O2W 2.000(10) . ? Cu2 N8 2.085(9) . ? Cu2 N5 2.183(10) . ? C1 N1 1.324(17) . ? C1 C2 1.35(2) . ? C1 H1A 0.9300 . ? C2 C3 1.34(2) . ? C2 H2A 0.9300 . ? C3 C4 1.40(3) . ? C3 H3A 0.9300 . ? C4 C5 1.36(2) . ? C4 H4A 0.9300 . ? C5 N1 1.358(16) . ? C5 C6 1.44(2) . ? C6 N2 1.325(16) . ? C6 C7 1.430(19) . ? C7 C8 1.42(2) . ? C7 H7A 0.9300 . ? C8 N3 1.27(2) . ? C8 H8A 0.9300 . ? C9 N3 1.477(17) . ? C9 C10 1.486(18) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.263(16) . ? C10 H10A 0.9300 . ? C11 C12 1.51(2) . ? C11 H11A 0.9300 . ? C12 N4 1.452(18) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N4 1.35(2) . ? C13 C14 1.36(2) . ? C13 H13A 0.9300 . ? C14 C15 1.428(18) . ? C14 H14A 0.9300 . ? C15 N5 1.323(15) . ? C15 C16 1.443(18) . ? C16 N6 1.320(16) . ? C16 C17 1.436(17) . ? C17 C18 1.32(2) . ? C17 H17A 0.9300 . ? C18 C19 1.43(3) . ? C18 H18A 0.9300 . ? C19 C20 1.38(2) . ? C19 H19A 0.9300 . ? C20 N6 1.365(15) . ? C20 H20A 0.9300 . ? C21 N7 1.328(17) . ? C21 C22 1.40(2) . ? C21 H21A 0.9300 . ? C22 C23 1.39(2) . ? C22 H22A 0.9300 . ? C23 C24 1.40(2) . ? C23 H23A 0.9300 . ? C24 C25 1.397(18) . ? C24 H24A 0.9300 . ? C25 N7 1.342(16) . ? C25 C26 1.441(19) . ? C26 N8 1.350(15) . ? C26 C27 1.374(19) . ? C27 C28 1.53(3) . ? C27 H27A 0.9300 . ? C28 N9 1.371(17) . ? C28 H28A 0.9300 . ? C29 N9 1.471(16) . ? C29 C30 1.491(18) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.281(17) . ? C30 H30A 0.9300 . ? C31 C32 1.538(19) . ? C31 H31A 0.9300 . ? C32 N10 1.448(17) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 N10 1.309(17) . ? C33 C34 1.34(2) . ? C33 H33A 0.9300 . ? C34 C35 1.377(16) . ? C34 H34A 0.9300 . ? C35 N11 1.370(15) . ? C35 C36 1.468(17) . ? C36 N12 1.325(15) . ? C36 C37 1.372(17) . ? C37 C38 1.39(2) . ? C37 H37A 0.9300 . ? C38 C39 1.35(2) . ? C38 H38A 0.9300 . ? C39 C40 1.384(19) . ? C39 H39A 0.9300 . ? C40 N12 1.363(15) . ? C40 H40A 0.9300 . ? Cl1 O2 1.25(2) . ? Cl1 O3 1.25(3) . ? Cl1 O4 1.27(2) . ? Cl1 O1 1.31(3) . ? Cl2 O8 1.29(2) . ? Cl2 O7 1.29(3) . ? Cl2 O6 1.31(2) . ? Cl2 O5 1.378(15) . ? Cl3 O12 1.409(12) . ? Cl3 O10 1.419(10) . ? Cl3 O9 1.424(11) . ? Cl3 O11 1.446(10) . ? Cl4 O13 1.402(11) . ? Cl4 O15 1.406(11) . ? Cl4 O16 1.416(10) . ? Cl4 O14 1.423(9) . ? N2 N3 1.336(13) . ? N4 N5 1.344(14) . ? N8 N9 1.334(13) . ? N10 N11 1.334(13) . ? 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 N1 Cu1 N12 177.6(4) . . ? N1 Cu1 O1W 87.2(4) . . ? N12 Cu1 O1W 90.4(4) . . ? N1 Cu1 N2 80.5(4) . . ? N12 Cu1 N2 101.2(4) . . ? O1W Cu1 N2 129.9(5) . . ? N1 Cu1 N11 101.2(4) . . ? N12 Cu1 N11 79.7(4) . . ? O1W Cu1 N11 115.2(5) . . ? N2 Cu1 N11 114.8(4) . . ? N7 Cu2 N6 176.5(4) . . ? N7 Cu2 O2W 87.6(4) . . ? N6 Cu2 O2W 88.9(4) . . ? N7 Cu2 N8 80.2(4) . . ? N6 Cu2 N8 102.6(4) . . ? O2W Cu2 N8 138.7(5) . . ? N7 Cu2 N5 101.7(5) . . ? N6 Cu2 N5 79.5(4) . . ? O2W Cu2 N5 112.2(5) . . ? N8 Cu2 N5 108.9(4) . . ? N1 C1 C2 124.2(15) . . ? N1 C1 H1A 117.9 . . ? C2 C1 H1A 117.9 . . ? C3 C2 C1 117.5(17) . . ? C3 C2 H2A 121.2 . . ? C1 C2 H2A 121.2 . . ? C2 C3 C4 120.5(17) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 118.5(16) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? N1 C5 C4 120.8(14) . . ? N1 C5 C6 113.2(12) . . ? C4 C5 C6 126.0(14) . . ? N2 C6 C7 110.0(13) . . ? N2 C6 C5 119.4(12) . . ? C7 C6 C5 130.6(14) . . ? C8 C7 C6 102.5(14) . . ? C8 C7 H7A 128.7 . . ? C6 C7 H7A 128.7 . . ? N3 C8 C7 107.3(13) . . ? N3 C8 H8A 126.4 . . ? C7 C8 H8A 126.4 . . ? N3 C9 C10 116.1(12) . . ? N3 C9 H9A 108.3 . . ? C10 C9 H9A 108.3 . . ? N3 C9 H9B 108.3 . . ? C10 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C11 C10 C9 124.9(13) . . ? C11 C10 H10A 117.6 . . ? C9 C10 H10A 117.6 . . ? C10 C11 C12 129.7(13) . . ? C10 C11 H11A 115.1 . . ? C12 C11 H11A 115.1 . . ? N4 C12 C11 113.0(11) . . ? N4 C12 H12A 109.0 . . ? C11 C12 H12A 109.0 . . ? N4 C12 H12B 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? N4 C13 C14 107.9(13) . . ? N4 C13 H13A 126.1 . . ? C14 C13 H13A 126.1 . . ? C13 C14 C15 105.1(14) . . ? C13 C14 H14A 127.5 . . ? C15 C14 H14A 127.5 . . ? N5 C15 C14 109.2(12) . . ? N5 C15 C16 118.5(11) . . ? C14 C15 C16 132.2(12) . . ? N6 C16 C17 121.4(13) . . ? N6 C16 C15 116.9(10) . . ? C17 C16 C15 121.6(14) . . ? C18 C17 C16 118.4(16) . . ? C18 C17 H17A 120.8 . . ? C16 C17 H17A 120.8 . . ? C17 C18 C19 121.4(14) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C20 C19 C18 116.8(16) . . ? C20 C19 H19A 121.6 . . ? C18 C19 H19A 121.6 . . ? N6 C20 C19 121.9(15) . . ? N6 C20 H20A 119.0 . . ? C19 C20 H20A 119.0 . . ? N7 C21 C22 121.8(14) . . ? N7 C21 H21A 119.1 . . ? C22 C21 H21A 119.1 . . ? C23 C22 C21 118.9(14) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C22 C23 C24 119.5(13) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C25 C24 C23 117.1(15) . . ? C25 C24 H24A 121.5 . . ? C23 C24 H24A 121.5 . . ? N7 C25 C24 123.3(14) . . ? N7 C25 C26 114.1(11) . . ? C24 C25 C26 122.6(13) . . ? N8 C26 C27 109.8(13) . . ? N8 C26 C25 117.9(11) . . ? C27 C26 C25 132.0(13) . . ? C26 C27 C28 107.5(13) . . ? C26 C27 H27A 126.2 . . ? C28 C27 H27A 126.2 . . ? N9 C28 C27 98.8(13) . . ? N9 C28 H28A 130.6 . . ? C27 C28 H28A 130.6 . . ? N9 C29 C30 112.5(10) . . ? N9 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? N9 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C31 C30 C29 123.0(12) . . ? C31 C30 H30A 118.5 . . ? C29 C30 H30A 118.5 . . ? C30 C31 C32 126.9(13) . . ? C30 C31 H31A 116.5 . . ? C32 C31 H31A 116.5 . . ? N10 C32 C31 113.2(10) . . ? N10 C32 H32A 108.9 . . ? C31 C32 H32A 108.9 . . ? N10 C32 H32B 108.9 . . ? C31 C32 H32B 108.9 . . ? H32A C32 H32B 107.8 . . ? N10 C33 C34 109.4(13) . . ? N10 C33 H33A 125.3 . . ? C34 C33 H33A 125.3 . . ? C33 C34 C35 104.7(13) . . ? C33 C34 H34A 127.7 . . ? C35 C34 H34A 127.7 . . ? N11 C35 C34 110.3(11) . . ? N11 C35 C36 116.5(10) . . ? C34 C35 C36 133.0(13) . . ? N12 C36 C37 124.3(12) . . ? N12 C36 C35 114.9(10) . . ? C37 C36 C35 120.8(11) . . ? C36 C37 C38 118.4(12) . . ? C36 C37 H37A 120.8 . . ? C38 C37 H37A 120.8 . . ? C39 C38 C37 118.5(14) . . ? C39 C38 H38A 120.7 . . ? C37 C38 H38A 120.7 . . ? C38 C39 C40 120.4(14) . . ? C38 C39 H39A 119.8 . . ? C40 C39 H39A 119.8 . . ? N12 C40 C39 121.6(12) . . ? N12 C40 H40A 119.2 . . ? C39 C40 H40A 119.2 . . ? O2 Cl1 O3 126(3) . . ? O2 Cl1 O4 102(2) . . ? O3 Cl1 O4 118(2) . . ? O2 Cl1 O1 91(2) . . ? O3 Cl1 O1 102(3) . . ? O4 Cl1 O1 115(3) . . ? O8 Cl2 O7 107(2) . . ? O8 Cl2 O6 100.5(19) . . ? O7 Cl2 O6 108(2) . . ? O8 Cl2 O5 120.2(17) . . ? O7 Cl2 O5 109.0(16) . . ? O6 Cl2 O5 111.4(13) . . ? O12 Cl3 O10 108.2(8) . . ? O12 Cl3 O9 112.0(10) . . ? O10 Cl3 O9 109.1(7) . . ? O12 Cl3 O11 109.3(7) . . ? O10 Cl3 O11 110.7(7) . . ? O9 Cl3 O11 107.6(8) . . ? O13 Cl4 O15 108.3(10) . . ? O13 Cl4 O16 107.4(8) . . ? O15 Cl4 O16 108.9(7) . . ? O13 Cl4 O14 107.2(7) . . ? O15 Cl4 O14 113.4(8) . . ? O16 Cl4 O14 111.5(7) . . ? C1 N1 C5 118.2(12) . . ? C1 N1 Cu1 125.7(9) . . ? C5 N1 Cu1 115.9(8) . . ? C6 N2 N3 105.6(10) . . ? C6 N2 Cu1 109.6(8) . . ? N3 N2 Cu1 142.2(8) . . ? C8 N3 N2 114.5(12) . . ? C8 N3 C9 123.8(13) . . ? N2 N3 C9 121.7(11) . . ? N5 N4 C13 110.7(12) . . ? N5 N4 C12 121.5(12) . . ? C13 N4 C12 127.8(13) . . ? C15 N5 N4 107.2(11) . . ? C15 N5 Cu2 108.8(8) . . ? N4 N5 Cu2 144.1(9) . . ? C16 N6 C20 119.8(10) . . ? C16 N6 Cu2 116.0(7) . . ? C20 N6 Cu2 124.0(9) . . ? C21 N7 C25 119.2(11) . . ? C21 N7 Cu2 123.9(9) . . ? C25 N7 Cu2 116.7(9) . . ? N9 N8 C26 107.1(10) . . ? N9 N8 Cu2 141.5(8) . . ? C26 N8 Cu2 111.0(8) . . ? N8 N9 C28 116.7(13) . . ? N8 N9 C29 122.7(11) . . ? C28 N9 C29 120.6(12) . . ? C33 N10 N11 112.1(13) . . ? C33 N10 C32 126.6(13) . . ? N11 N10 C32 121.2(11) . . ? N10 N11 C35 103.5(9) . . ? N10 N11 Cu1 146.2(9) . . ? C35 N11 Cu1 110.3(7) . . ? C36 N12 C40 116.6(10) . . ? C36 N12 Cu1 118.0(8) . . ? C40 N12 Cu1 124.2(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 N1 C1 C2 C3 -4(3) . . . . ? C1 C2 C3 C4 6(3) . . . . ? C2 C3 C4 C5 -4(3) . . . . ? C3 C4 C5 N1 0(3) . . . . ? C3 C4 C5 C6 176.0(17) . . . . ? N1 C5 C6 N2 -10.4(18) . . . . ? C4 C5 C6 N2 173.0(14) . . . . ? N1 C5 C6 C7 167.3(15) . . . . ? C4 C5 C6 C7 -9(3) . . . . ? N2 C6 C7 C8 -3.2(18) . . . . ? C5 C6 C7 C8 178.8(15) . . . . ? C6 C7 C8 N3 3.9(19) . . . . ? N3 C9 C10 C11 -122.6(16) . . . . ? C9 C10 C11 C12 -175.9(15) . . . . ? C10 C11 C12 N4 -3(2) . . . . ? N4 C13 C14 C15 0.5(16) . . . . ? C13 C14 C15 N5 0.4(16) . . . . ? C13 C14 C15 C16 -175.3(13) . . . . ? N5 C15 C16 N6 5.7(16) . . . . ? C14 C15 C16 N6 -179.0(13) . . . . ? N5 C15 C16 C17 -175.6(11) . . . . ? C14 C15 C16 C17 0(2) . . . . ? N6 C16 C17 C18 -5.2(19) . . . . ? C15 C16 C17 C18 176.2(12) . . . . ? C16 C17 C18 C19 6(2) . . . . ? C17 C18 C19 C20 -4(2) . . . . ? C18 C19 C20 N6 1(2) . . . . ? N7 C21 C22 C23 -5(3) . . . . ? C21 C22 C23 C24 2(3) . . . . ? C22 C23 C24 C25 1(3) . . . . ? C23 C24 C25 N7 -2(3) . . . . ? C23 C24 C25 C26 177.4(17) . . . . ? N7 C25 C26 N8 -4(2) . . . . ? C24 C25 C26 N8 176.7(15) . . . . ? N7 C25 C26 C27 169.1(17) . . . . ? C24 C25 C26 C27 -10(3) . . . . ? N8 C26 C27 C28 -1.9(19) . . . . ? C25 C26 C27 C28 -175.7(17) . . . . ? C26 C27 C28 N9 1.4(18) . . . . ? N9 C29 C30 C31 -123.6(13) . . . . ? C29 C30 C31 C32 -174.7(12) . . . . ? C30 C31 C32 N10 -5(2) . . . . ? N10 C33 C34 C35 -1.9(16) . . . . ? C33 C34 C35 N11 1.4(15) . . . . ? C33 C34 C35 C36 -173.9(14) . . . . ? N11 C35 C36 N12 9.0(16) . . . . ? C34 C35 C36 N12 -175.9(13) . . . . ? N11 C35 C36 C37 -172.2(11) . . . . ? C34 C35 C36 C37 3(2) . . . . ? N12 C36 C37 C38 -3(2) . . . . ? C35 C36 C37 C38 178.1(12) . . . . ? C36 C37 C38 C39 -1(2) . . . . ? C37 C38 C39 C40 2(2) . . . . ? C38 C39 C40 N12 1(2) . . . . ? C2 C1 N1 C5 0(2) . . . . ? C2 C1 N1 Cu1 -175.1(13) . . . . ? C4 C5 N1 C1 3(2) . . . . ? C6 C5 N1 C1 -174.1(13) . . . . ? C4 C5 N1 Cu1 177.8(12) . . . . ? C6 C5 N1 Cu1 1.0(15) . . . . ? N12 Cu1 N1 C1 45(11) . . . . ? O1W Cu1 N1 C1 48.2(13) . . . . ? N2 Cu1 N1 C1 179.4(13) . . . . ? N11 Cu1 N1 C1 -67.0(12) . . . . ? N12 Cu1 N1 C5 -130(10) . . . . ? O1W Cu1 N1 C5 -126.6(10) . . . . ? N2 Cu1 N1 C5 4.6(9) . . . . ? N11 Cu1 N1 C5 118.3(10) . . . . ? C7 C6 N2 N3 1.4(15) . . . . ? C5 C6 N2 N3 179.6(12) . . . . ? C7 C6 N2 Cu1 -164.5(10) . . . . ? C5 C6 N2 Cu1 13.7(14) . . . . ? N1 Cu1 N2 C6 -9.7(8) . . . . ? N12 Cu1 N2 C6 168.6(8) . . . . ? O1W Cu1 N2 C6 68.5(9) . . . . ? N11 Cu1 N2 C6 -107.7(8) . . . . ? N1 Cu1 N2 N3 -167.2(13) . . . . ? N12 Cu1 N2 N3 11.1(13) . . . . ? O1W Cu1 N2 N3 -89.0(13) . . . . ? N11 Cu1 N2 N3 94.8(12) . . . . ? C7 C8 N3 N2 -3.5(19) . . . . ? C7 C8 N3 C9 176.6(13) . . . . ? C6 N2 N3 C8 1.4(15) . . . . ? Cu1 N2 N3 C8 159.4(12) . . . . ? C6 N2 N3 C9 -178.8(11) . . . . ? Cu1 N2 N3 C9 -20.7(18) . . . . ? C10 C9 N3 C8 103.6(17) . . . . ? C10 C9 N3 N2 -76.3(16) . . . . ? C14 C13 N4 N5 -1.2(16) . . . . ? C14 C13 N4 C12 177.9(12) . . . . ? C11 C12 N4 N5 -91.6(15) . . . . ? C11 C12 N4 C13 89.3(18) . . . . ? C14 C15 N5 N4 -1.1(14) . . . . ? C16 C15 N5 N4 175.3(10) . . . . ? C14 C15 N5 Cu2 179.4(8) . . . . ? C16 C15 N5 Cu2 -4.3(13) . . . . ? C13 N4 N5 C15 1.5(14) . . . . ? C12 N4 N5 C15 -177.8(11) . . . . ? C13 N4 N5 Cu2 -179.3(11) . . . . ? C12 N4 N5 Cu2 1(2) . . . . ? N7 Cu2 N5 C15 178.4(8) . . . . ? N6 Cu2 N5 C15 1.7(8) . . . . ? O2W Cu2 N5 C15 86.2(8) . . . . ? N8 Cu2 N5 C15 -98.1(8) . . . . ? N7 Cu2 N5 N4 -0.9(14) . . . . ? N6 Cu2 N5 N4 -177.5(14) . . . . ? O2W Cu2 N5 N4 -93.1(13) . . . . ? N8 Cu2 N5 N4 82.6(14) . . . . ? C17 C16 N6 C20 2.0(17) . . . . ? C15 C16 N6 C20 -179.3(11) . . . . ? C17 C16 N6 Cu2 177.5(9) . . . . ? C15 C16 N6 Cu2 -3.9(13) . . . . ? C19 C20 N6 C16 0.2(19) . . . . ? C19 C20 N6 Cu2 -174.9(10) . . . . ? N7 Cu2 N6 C16 -109(7) . . . . ? O2W Cu2 N6 C16 -111.6(9) . . . . ? N8 Cu2 N6 C16 108.4(9) . . . . ? N5 Cu2 N6 C16 1.2(8) . . . . ? N7 Cu2 N6 C20 66(8) . . . . ? O2W Cu2 N6 C20 63.6(11) . . . . ? N8 Cu2 N6 C20 -76.3(10) . . . . ? N5 Cu2 N6 C20 176.5(11) . . . . ? C22 C21 N7 C25 4(3) . . . . ? C22 C21 N7 Cu2 179.1(14) . . . . ? C24 C25 N7 C21 -1(2) . . . . ? C26 C25 N7 C21 -179.9(15) . . . . ? C24 C25 N7 Cu2 -176.2(13) . . . . ? C26 C25 N7 Cu2 4.8(17) . . . . ? N6 Cu2 N7 C21 39(8) . . . . ? O2W Cu2 N7 C21 41.5(14) . . . . ? N8 Cu2 N7 C21 -178.1(14) . . . . ? N5 Cu2 N7 C21 -70.7(14) . . . . ? N6 Cu2 N7 C25 -146(7) . . . . ? O2W Cu2 N7 C25 -143.5(11) . . . . ? N8 Cu2 N7 C25 -3.1(10) . . . . ? N5 Cu2 N7 C25 104.3(11) . . . . ? C27 C26 N8 N9 1.6(17) . . . . ? C25 C26 N8 N9 176.4(12) . . . . ? C27 C26 N8 Cu2 -173.1(11) . . . . ? C25 C26 N8 Cu2 1.7(16) . . . . ? N7 Cu2 N8 N9 -171.2(14) . . . . ? N6 Cu2 N8 N9 6.7(14) . . . . ? O2W Cu2 N8 N9 -96.3(14) . . . . ? N5 Cu2 N8 N9 89.7(13) . . . . ? N7 Cu2 N8 C26 0.7(9) . . . . ? N6 Cu2 N8 C26 178.5(9) . . . . ? O2W Cu2 N8 C26 75.6(11) . . . . ? N5 Cu2 N8 C26 -98.4(9) . . . . ? C26 N8 N9 C28 -0.6(17) . . . . ? Cu2 N8 N9 C28 171.4(12) . . . . ? C26 N8 N9 C29 178.2(12) . . . . ? Cu2 N8 N9 C29 -10(2) . . . . ? C27 C28 N9 N8 -0.5(18) . . . . ? C27 C28 N9 C29 -179.3(12) . . . . ? C30 C29 N9 N8 -86.6(14) . . . . ? C30 C29 N9 C28 92.2(16) . . . . ? C34 C33 N10 N11 1.8(16) . . . . ? C34 C33 N10 C32 179.1(12) . . . . ? C31 C32 N10 C33 94.4(15) . . . . ? C31 C32 N10 N11 -88.5(14) . . . . ? C33 N10 N11 C35 -0.8(13) . . . . ? C32 N10 N11 C35 -178.3(11) . . . . ? C33 N10 N11 Cu1 -177.1(11) . . . . ? C32 N10 N11 Cu1 5(2) . . . . ? C34 C35 N11 N10 -0.4(13) . . . . ? C36 C35 N11 N10 175.8(10) . . . . ? C34 C35 N11 Cu1 177.4(8) . . . . ? C36 C35 N11 Cu1 -6.4(13) . . . . ? N1 Cu1 N11 N10 -3.8(14) . . . . ? N12 Cu1 N11 N10 178.4(14) . . . . ? O1W Cu1 N11 N10 -96.0(13) . . . . ? N2 Cu1 N11 N10 80.8(13) . . . . ? N1 Cu1 N11 C35 -180.0(8) . . . . ? N12 Cu1 N11 C35 2.3(8) . . . . ? O1W Cu1 N11 C35 87.8(8) . . . . ? N2 Cu1 N11 C35 -95.4(8) . . . . ? C37 C36 N12 C40 6.0(18) . . . . ? C35 C36 N12 C40 -175.2(11) . . . . ? C37 C36 N12 Cu1 174.3(10) . . . . ? C35 C36 N12 Cu1 -6.9(14) . . . . ? C39 C40 N12 C36 -4.6(19) . . . . ? C39 C40 N12 Cu1 -172.1(10) . . . . ? N1 Cu1 N12 C36 -110(10) . . . . ? O1W Cu1 N12 C36 -112.9(10) . . . . ? N2 Cu1 N12 C36 116.2(9) . . . . ? N11 Cu1 N12 C36 2.7(9) . . . . ? N1 Cu1 N12 C40 58(10) . . . . ? O1W Cu1 N12 C40 54.5(11) . . . . ? N2 Cu1 N12 C40 -76.5(11) . . . . ? N11 Cu1 N12 C40 170.0(11) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 3.171 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.171 #===END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H40 Co2 N14 O8, 2(N O3)' _chemical_formula_sum 'C40 H40 Co2 N16 O14' _chemical_formula_structural '2(Co 2+), 2(C20 H18 N6), 4(N O3), 2(H2 O)' _chemical_formula_weight 1086.74 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pbcn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.170(7) _cell_length_b 13.240(5) _cell_length_c 19.064(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4586(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1050 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 22.98 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.866349 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details '(SADABS; bruker, 1996)' _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 'bruker ccd area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25135 _diffrn_reflns_av_R_equivalents 0.0926 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.41 _reflns_number_total 4691 _reflns_number_gt 2497 _reflns_threshold_expression I>2s\(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _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^)+(0.0304P)^2^+2.7643P] 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 4691 _refine_ls_number_parameters 363 _refine_ls_number_restraints 182 _refine_ls_R_factor_all 0.1259 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.027 _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 Co1 Co 0.0000 0.95739(4) 0.2500 0.03312(17) Uani 1 2 d S . . Co2 Co 0.0000 0.36312(4) 0.2500 0.03907(19) Uani 1 2 d S . . C1 C -0.0555(2) 1.0166(3) 0.4005(2) 0.0478(10) Uani 1 1 d . . . H1 H -0.0156 1.0607 0.4013 0.057 Uiso 1 1 calc R . . C2 C -0.0999(2) 1.0111(3) 0.4586(2) 0.0581(11) Uani 1 1 d . . . H2 H -0.0900 1.0502 0.4980 0.070 Uiso 1 1 calc R . . C3 C -0.1588(2) 0.9475(4) 0.4575(2) 0.0669(13) Uani 1 1 d . . . H3 H -0.1890 0.9414 0.4966 0.080 Uiso 1 1 calc R . . C4 C -0.1733(2) 0.8926(3) 0.3979(2) 0.0564(11) Uani 1 1 d . . . H4 H -0.2140 0.8500 0.3959 0.068 Uiso 1 1 calc R . . C5 C -0.12661(19) 0.9014(3) 0.34124(19) 0.0389(9) Uani 1 1 d . . . C6 C -0.13704(19) 0.8450(3) 0.27633(19) 0.0395(9) Uani 1 1 d . . . C7 C -0.19507(19) 0.7885(3) 0.2508(2) 0.0540(10) Uani 1 1 d . . . H7 H -0.2398 0.7758 0.2729 0.065 Uiso 1 1 calc R . . C8 C -0.1732(2) 0.7556(3) 0.1869(2) 0.0550(12) Uani 1 1 d . . . H8 H -0.2005 0.7152 0.1566 0.066 Uiso 1 1 calc R . . C9 C -0.0571(2) 0.7716(3) 0.1153(2) 0.0515(11) Uani 1 1 d . . . H9A H -0.0279 0.8314 0.1059 0.062 Uiso 1 1 calc R . . H9B H -0.0869 0.7580 0.0742 0.062 Uiso 1 1 calc R . . C10 C -0.0060(2) 0.6829(3) 0.1280(2) 0.0517(10) Uani 1 1 d . . . H10 H 0.0230 0.6835 0.1681 0.062 Uiso 1 1 calc R . . C11 C -0.0007(2) 0.6082(3) 0.0871(2) 0.0574(10) Uani 1 1 d . . . H11 H -0.0330 0.6081 0.0492 0.069 Uiso 1 1 calc R . . C12 C 0.0497(2) 0.5208(3) 0.0910(2) 0.0552(11) Uani 1 1 d . . . H12A H 0.0204 0.4596 0.0910 0.066 Uiso 1 1 calc R . . H12B H 0.0795 0.5201 0.0487 0.066 Uiso 1 1 calc R . . C13 C 0.1666(2) 0.5564(3) 0.1559(3) 0.0648(13) Uani 1 1 d . . . H13 H 0.1908 0.5929 0.1211 0.078 Uiso 1 1 calc R . . C14 C 0.1939(2) 0.5334(3) 0.2198(3) 0.0637(13) Uani 1 1 d . . . H14 H 0.2399 0.5502 0.2378 0.076 Uiso 1 1 calc R . . C15 C 0.13844(19) 0.4793(3) 0.2531(2) 0.0462(9) Uani 1 1 d . . . C16 C 0.1372(2) 0.4286(3) 0.3210(2) 0.0480(10) Uani 1 1 d . . . C17 C 0.1934(2) 0.4396(4) 0.3694(2) 0.0660(13) Uani 1 1 d . . . H17 H 0.2321 0.4839 0.3610 0.079 Uiso 1 1 calc R . . C18 C 0.1908(3) 0.3840(4) 0.4300(3) 0.0786(16) Uani 1 1 d . . . H18 H 0.2281 0.3898 0.4631 0.094 Uiso 1 1 calc R . . C19 C 0.1329(3) 0.3197(4) 0.4416(2) 0.0694(14) Uani 1 1 d . . . H19 H 0.1311 0.2802 0.4819 0.083 Uiso 1 1 calc R . . C20 C 0.0771(2) 0.3147(3) 0.3922(2) 0.0567(11) Uani 1 1 d . . . H20 H 0.0371 0.2726 0.4005 0.068 Uiso 1 1 calc R . . N1 N -0.06688(14) 0.9612(2) 0.34271(14) 0.0374(7) Uani 1 1 d . . . N2 N -0.08183(15) 0.8472(2) 0.22941(14) 0.0368(7) Uani 1 1 d . . . N3 N -0.10524(16) 0.7913(2) 0.17479(15) 0.0416(8) Uani 1 1 d . . . N4 N 0.09879(17) 0.5178(2) 0.15120(17) 0.0473(8) Uani 1 1 d . . . N5 N 0.08016(16) 0.4692(2) 0.21077(16) 0.0422(8) Uani 1 1 d . . . N6 N 0.07919(17) 0.3686(2) 0.33286(16) 0.0456(8) Uani 1 1 d . . . N7 N 0.12281(17) 1.0731(3) 0.32588(18) 0.0445(8) Uani 1 1 d . . . O1 O 0.06723(14) 1.07815(18) 0.28565(14) 0.0532(7) Uani 1 1 d . . . O2 O 0.17247(16) 1.1331(2) 0.3170(2) 0.0891(11) Uani 1 1 d . . . O3 O 0.12404(16) 1.0099(2) 0.37287(15) 0.0694(9) Uani 1 1 d . . . N8 N 0.1627(7) 0.2638(7) 0.0495(7) 0.059(5) Uani 0.47(3) 1 d PDU A 1 O4 O 0.0961(5) 0.2745(13) 0.0591(7) 0.062(3) Uani 0.47(3) 1 d PDU A 1 O5 O 0.1917(7) 0.3076(16) -0.0014(5) 0.088(4) Uani 0.47(3) 1 d PDU A 1 O6 O 0.1996(8) 0.2108(9) 0.0893(11) 0.092(5) Uani 0.47(3) 1 d PDU A 1 N8' N 0.1617(7) 0.2660(6) 0.0611(7) 0.072(5) Uani 0.53(3) 1 d PDU A 2 O4' O 0.1022(8) 0.3079(14) 0.0545(9) 0.111(6) Uani 0.53(3) 1 d PDU A 2 O5' O 0.2006(6) 0.2494(15) 0.0085(7) 0.096(4) Uani 0.53(3) 1 d PDU A 2 O6' O 0.1806(7) 0.2415(13) 0.1197(7) 0.097(4) Uani 0.53(3) 1 d PDU A 2 O1W O 0.05835(14) 0.24798(18) 0.20105(13) 0.0583(8) Uani 1 1 d . . . H1WA H 0.0874 0.2603 0.1671 0.087 Uiso 1 1 d R . . H1WB H 0.0745 0.1995 0.2259 0.087 Uiso 1 1 d 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 Co1 0.0313(3) 0.0350(4) 0.0330(4) 0.000 0.0001(3) 0.000 Co2 0.0402(4) 0.0371(4) 0.0399(4) 0.000 0.0000(4) 0.000 C1 0.044(2) 0.055(3) 0.045(3) -0.010(2) -0.001(2) 0.000(2) C2 0.060(3) 0.072(3) 0.043(3) -0.009(2) 0.003(2) 0.007(3) C3 0.061(3) 0.093(4) 0.047(3) 0.005(3) 0.021(2) 0.002(3) C4 0.041(2) 0.074(3) 0.054(3) -0.001(2) 0.013(2) -0.007(2) C5 0.031(2) 0.047(2) 0.039(2) 0.0028(18) 0.0035(18) 0.0041(18) C6 0.033(2) 0.041(2) 0.044(2) 0.0057(18) -0.0013(17) -0.0012(19) C7 0.038(2) 0.056(2) 0.067(3) -0.006(3) 0.005(2) -0.0120(18) C8 0.041(3) 0.048(3) 0.075(3) -0.011(2) -0.013(2) -0.012(2) C9 0.063(3) 0.051(3) 0.040(3) -0.010(2) -0.002(2) -0.006(2) C10 0.053(2) 0.059(3) 0.043(2) -0.0126(18) -0.001(2) 0.004(3) C11 0.071(3) 0.052(2) 0.049(2) -0.002(2) -0.001(3) -0.007(3) C12 0.068(3) 0.048(3) 0.050(3) 0.006(2) 0.006(2) 0.000(2) C13 0.051(3) 0.062(3) 0.081(4) 0.008(3) 0.021(3) -0.012(2) C14 0.042(3) 0.071(3) 0.078(3) 0.001(3) 0.006(2) -0.011(2) C15 0.041(2) 0.044(2) 0.054(2) -0.007(2) 0.005(2) 0.0013(17) C16 0.033(2) 0.058(3) 0.053(3) -0.012(2) -0.0018(19) 0.006(2) C17 0.045(3) 0.090(4) 0.063(3) -0.004(3) -0.004(2) -0.003(2) C18 0.052(3) 0.118(5) 0.066(4) -0.014(3) -0.020(3) 0.018(3) C19 0.076(3) 0.084(4) 0.048(3) 0.007(2) -0.006(3) 0.026(3) C20 0.056(3) 0.066(3) 0.047(3) 0.001(2) -0.001(2) 0.009(2) N1 0.0336(17) 0.0433(18) 0.0354(18) -0.0014(15) 0.0008(13) 0.0003(15) N2 0.0384(17) 0.0368(17) 0.0352(18) -0.0035(14) -0.0038(13) -0.0015(15) N3 0.0434(19) 0.0399(18) 0.041(2) -0.0065(15) -0.0067(15) 0.0001(15) N4 0.051(2) 0.0404(19) 0.050(2) 0.0041(16) 0.0095(17) -0.0009(16) N5 0.0427(19) 0.0392(19) 0.045(2) 0.0017(15) 0.0034(16) -0.0003(15) N6 0.0427(19) 0.051(2) 0.043(2) 0.0002(16) -0.0028(15) 0.0044(16) N7 0.0354(19) 0.048(2) 0.050(2) -0.0086(17) 0.0055(17) -0.0002(17) O1 0.0530(17) 0.0425(16) 0.0642(19) 0.0039(13) -0.0251(15) -0.0071(13) O2 0.0425(18) 0.076(2) 0.149(3) 0.005(2) 0.004(2) -0.0174(18) O3 0.074(2) 0.083(2) 0.0507(19) 0.0134(17) -0.0134(16) 0.0059(18) N8 0.062(8) 0.073(8) 0.043(6) -0.016(6) -0.003(6) -0.011(6) O4 0.058(5) 0.069(7) 0.059(5) 0.010(4) 0.017(4) 0.019(4) O5 0.080(6) 0.116(9) 0.067(5) 0.002(5) -0.001(4) -0.038(6) O6 0.087(7) 0.088(6) 0.101(8) 0.007(6) -0.034(6) -0.007(5) N8' 0.060(8) 0.089(8) 0.066(7) -0.006(6) -0.004(6) -0.019(6) O4' 0.120(8) 0.101(9) 0.113(8) 0.016(6) 0.027(6) 0.038(6) O5' 0.075(5) 0.121(9) 0.093(7) -0.034(6) 0.035(5) -0.003(5) O6' 0.076(6) 0.151(8) 0.063(6) 0.003(5) -0.013(5) -0.030(5) O1W 0.078(2) 0.0458(17) 0.0511(18) 0.0091(13) 0.0151(15) 0.0142(15) _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 Co1 N2 2.120(3) . ? Co1 N2 2.120(3) 3 ? Co1 O1 2.124(3) . ? Co1 O1 2.124(3) 3 ? Co1 N1 2.145(3) 3 ? Co1 N1 2.145(3) . ? Co2 O1W 2.078(2) 3 ? Co2 O1W 2.078(2) . ? Co2 N6 2.138(3) 3 ? Co2 N6 2.138(3) . ? Co2 N5 2.157(3) 3 ? Co2 N5 2.157(3) . ? C1 N1 1.340(4) . ? C1 C2 1.373(5) . ? C1 H1 0.9300 . ? C2 C3 1.362(6) . ? C2 H2 0.9300 . ? C3 C4 1.374(6) . ? C3 H3 0.9300 . ? C4 C5 1.378(5) . ? C4 H4 0.9300 . ? C5 N1 1.344(4) . ? C5 C6 1.458(5) . ? C6 N2 1.344(4) . ? C6 C7 1.381(5) . ? C7 C8 1.354(5) . ? C7 H7 0.9300 . ? C8 N3 1.342(4) . ? C8 H8 0.9300 . ? C9 N3 1.455(4) . ? C9 C10 1.516(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.264(5) . ? C10 H10 0.9300 . ? C11 C12 1.477(5) . ? C11 H11 0.9300 . ? C12 N4 1.455(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N4 1.337(5) . ? C13 C14 1.351(6) . ? C13 H13 0.9300 . ? C14 C15 1.389(5) . ? C14 H14 0.9300 . ? C15 N5 1.338(4) . ? C15 C16 1.458(5) . ? C16 N6 1.340(5) . ? C16 C17 1.383(5) . ? C17 C18 1.372(6) . ? C17 H17 0.9300 . ? C18 C19 1.370(6) . ? C18 H18 0.9300 . ? C19 C20 1.385(5) . ? C19 H19 0.9300 . ? C20 N6 1.338(5) . ? C20 H20 0.9300 . ? N2 N3 1.346(4) . ? N4 N5 1.348(4) . ? N7 O2 1.214(4) . ? N7 O3 1.225(4) . ? N7 O1 1.270(4) . ? N8 O4 1.231(10) . ? N8 O6 1.231(10) . ? N8 O5 1.248(10) . ? N8' O6' 1.214(10) . ? N8' O4' 1.220(10) . ? N8' O5' 1.246(10) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8499 . ? 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 N2 Co1 N2 93.00(15) . 3 ? N2 Co1 O1 168.77(11) . . ? N2 Co1 O1 93.19(10) 3 . ? N2 Co1 O1 93.19(10) . 3 ? N2 Co1 O1 168.77(11) 3 3 ? O1 Co1 O1 82.32(14) . 3 ? N2 Co1 N1 105.12(11) . 3 ? N2 Co1 N1 76.79(11) 3 3 ? O1 Co1 N1 85.42(10) . 3 ? O1 Co1 N1 92.55(11) 3 3 ? N2 Co1 N1 76.79(11) . . ? N2 Co1 N1 105.12(11) 3 . ? O1 Co1 N1 92.55(11) . . ? O1 Co1 N1 85.42(10) 3 . ? N1 Co1 N1 177.31(16) 3 . ? O1W Co2 O1W 85.63(14) 3 . ? O1W Co2 N6 90.77(11) 3 3 ? O1W Co2 N6 92.09(12) . 3 ? O1W Co2 N6 92.09(12) 3 . ? O1W Co2 N6 90.77(11) . . ? N6 Co2 N6 176.10(17) 3 . ? O1W Co2 N5 88.71(11) 3 3 ? O1W Co2 N5 167.89(11) . 3 ? N6 Co2 N5 77.27(12) 3 3 ? N6 Co2 N5 100.14(12) . 3 ? O1W Co2 N5 167.89(11) 3 . ? O1W Co2 N5 88.71(11) . . ? N6 Co2 N5 100.14(12) 3 . ? N6 Co2 N5 77.27(12) . . ? N5 Co2 N5 98.75(16) 3 . ? N1 C1 C2 122.9(4) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 118.8(4) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.0(4) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.1(4) . . ? N1 C5 C6 115.1(3) . . ? C4 C5 C6 122.8(4) . . ? N2 C6 C7 110.3(3) . . ? N2 C6 C5 117.2(3) . . ? C7 C6 C5 132.5(4) . . ? C8 C7 C6 105.5(3) . . ? C8 C7 H7 127.2 . . ? C6 C7 H7 127.2 . . ? N3 C8 C7 108.1(3) . . ? N3 C8 H8 125.9 . . ? C7 C8 H8 125.9 . . ? N3 C9 C10 112.5(3) . . ? N3 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N3 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C9 123.7(4) . . ? C11 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? C10 C11 C12 129.0(4) . . ? C10 C11 H11 115.5 . . ? C12 C11 H11 115.5 . . ? N4 C12 C11 116.2(3) . . ? N4 C12 H12A 108.2 . . ? C11 C12 H12A 108.2 . . ? N4 C12 H12B 108.2 . . ? C11 C12 H12B 108.2 . . ? H12A C12 H12B 107.4 . . ? N4 C13 C14 108.2(4) . . ? N4 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? C13 C14 C15 105.2(4) . . ? C13 C14 H14 127.4 . . ? C15 C14 H14 127.4 . . ? N5 C15 C14 110.5(4) . . ? N5 C15 C16 118.5(3) . . ? C14 C15 C16 130.8(4) . . ? N6 C16 C17 122.0(4) . . ? N6 C16 C15 115.8(3) . . ? C17 C16 C15 122.2(4) . . ? C18 C17 C16 118.7(4) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C19 C18 C17 119.7(4) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 118.8(4) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? N6 C20 C19 121.9(4) . . ? N6 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C1 N1 C5 117.7(3) . . ? C1 N1 Co1 127.1(2) . . ? C5 N1 Co1 115.2(2) . . ? C6 N2 N3 105.5(3) . . ? C6 N2 Co1 114.5(2) . . ? N3 N2 Co1 138.0(2) . . ? C8 N3 N2 110.6(3) . . ? C8 N3 C9 128.6(3) . . ? N2 N3 C9 120.7(3) . . ? C13 N4 N5 111.0(3) . . ? C13 N4 C12 127.3(4) . . ? N5 N4 C12 121.6(3) . . ? C15 N5 N4 105.2(3) . . ? C15 N5 Co2 113.0(2) . . ? N4 N5 Co2 140.5(2) . . ? C20 N6 C16 118.8(3) . . ? C20 N6 Co2 126.0(3) . . ? C16 N6 Co2 115.2(3) . . ? O2 N7 O3 122.3(4) . . ? O2 N7 O1 118.2(4) . . ? O3 N7 O1 119.5(3) . . ? N7 O1 Co1 127.6(2) . . ? O4 N8 O6 120.7(11) . . ? O4 N8 O5 118.5(11) . . ? O6 N8 O5 120.8(11) . . ? O6' N8' O4' 117.9(12) . . ? O6' N8' O5' 122.1(11) . . ? O4' N8' O5' 120.0(12) . . ? Co2 O1W H1WA 121.2 . . ? Co2 O1W H1WB 118.7 . . ? H1WA O1W H1WB 110.7 . . ? 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 N1 C1 C2 C3 -0.7(6) . . . . ? C1 C2 C3 C4 -1.6(7) . . . . ? C2 C3 C4 C5 1.6(7) . . . . ? C3 C4 C5 N1 0.8(6) . . . . ? C3 C4 C5 C6 179.1(4) . . . . ? N1 C5 C6 N2 9.0(5) . . . . ? C4 C5 C6 N2 -169.4(4) . . . . ? N1 C5 C6 C7 -169.4(4) . . . . ? C4 C5 C6 C7 12.2(6) . . . . ? N2 C6 C7 C8 0.5(4) . . . . ? C5 C6 C7 C8 179.0(4) . . . . ? C6 C7 C8 N3 -0.3(5) . . . . ? N3 C9 C10 C11 126.3(4) . . . . ? C9 C10 C11 C12 175.8(4) . . . . ? C10 C11 C12 N4 2.2(6) . . . . ? N4 C13 C14 C15 -0.2(5) . . . . ? C13 C14 C15 N5 0.5(5) . . . . ? C13 C14 C15 C16 175.4(4) . . . . ? N5 C15 C16 N6 5.3(5) . . . . ? C14 C15 C16 N6 -169.2(4) . . . . ? N5 C15 C16 C17 -176.4(4) . . . . ? C14 C15 C16 C17 9.1(7) . . . . ? N6 C16 C17 C18 2.8(6) . . . . ? C15 C16 C17 C18 -175.4(4) . . . . ? C16 C17 C18 C19 -0.5(7) . . . . ? C17 C18 C19 C20 -1.7(7) . . . . ? C18 C19 C20 N6 1.8(7) . . . . ? C2 C1 N1 C5 3.0(5) . . . . ? C2 C1 N1 Co1 -177.4(3) . . . . ? C4 C5 N1 C1 -3.1(5) . . . . ? C6 C5 N1 C1 178.5(3) . . . . ? C4 C5 N1 Co1 177.3(3) . . . . ? C6 C5 N1 Co1 -1.1(4) . . . . ? N2 Co1 N1 C1 176.5(3) . . . . ? N2 Co1 N1 C1 86.9(3) 3 . . . ? O1 Co1 N1 C1 -7.1(3) . . . . ? O1 Co1 N1 C1 -89.2(3) 3 . . . ? N1 Co1 N1 C1 -48.1(3) 3 . . . ? N2 Co1 N1 C5 -4.0(2) . . . . ? N2 Co1 N1 C5 -93.5(2) 3 . . . ? O1 Co1 N1 C5 172.5(2) . . . . ? O1 Co1 N1 C5 90.4(2) 3 . . . ? N1 Co1 N1 C5 131.5(2) 3 . . . ? C7 C6 N2 N3 -0.5(4) . . . . ? C5 C6 N2 N3 -179.2(3) . . . . ? C7 C6 N2 Co1 166.4(2) . . . . ? C5 C6 N2 Co1 -12.4(4) . . . . ? N2 Co1 N2 C6 113.6(3) 3 . . . ? O1 Co1 N2 C6 -9.8(7) . . . . ? O1 Co1 N2 C6 -75.8(2) 3 . . . ? N1 Co1 N2 C6 -169.3(2) 3 . . . ? N1 Co1 N2 C6 8.8(2) . . . . ? N2 Co1 N2 N3 -85.5(3) 3 . . . ? O1 Co1 N2 N3 151.1(4) . . . . ? O1 Co1 N2 N3 85.1(3) 3 . . . ? N1 Co1 N2 N3 -8.4(3) 3 . . . ? N1 Co1 N2 N3 169.7(3) . . . . ? C7 C8 N3 N2 0.0(4) . . . . ? C7 C8 N3 C9 176.0(4) . . . . ? C6 N2 N3 C8 0.3(4) . . . . ? Co1 N2 N3 C8 -161.7(3) . . . . ? C6 N2 N3 C9 -176.1(3) . . . . ? Co1 N2 N3 C9 21.9(5) . . . . ? C10 C9 N3 C8 -91.9(5) . . . . ? C10 C9 N3 N2 83.8(4) . . . . ? C14 C13 N4 N5 -0.1(5) . . . . ? C14 C13 N4 C12 -177.6(4) . . . . ? C11 C12 N4 C13 -90.6(5) . . . . ? C11 C12 N4 N5 92.1(4) . . . . ? C14 C15 N5 N4 -0.5(4) . . . . ? C16 C15 N5 N4 -176.1(3) . . . . ? C14 C15 N5 Co2 169.2(3) . . . . ? C16 C15 N5 Co2 -6.4(4) . . . . ? C13 N4 N5 C15 0.4(4) . . . . ? C12 N4 N5 C15 178.1(3) . . . . ? C13 N4 N5 Co2 -164.6(3) . . . . ? C12 N4 N5 Co2 13.1(5) . . . . ? O1W Co2 N5 C15 -24.8(6) 3 . . . ? O1W Co2 N5 C15 -86.8(2) . . . . ? N6 Co2 N5 C15 -178.7(2) 3 . . . ? N6 Co2 N5 C15 4.3(2) . . . . ? N5 Co2 N5 C15 102.8(3) 3 . . . ? O1W Co2 N5 N4 139.4(5) 3 . . . ? O1W Co2 N5 N4 77.4(4) . . . . ? N6 Co2 N5 N4 -14.5(4) 3 . . . ? N6 Co2 N5 N4 168.4(4) . . . . ? N5 Co2 N5 N4 -93.1(4) 3 . . . ? C19 C20 N6 C16 0.4(6) . . . . ? C19 C20 N6 Co2 176.9(3) . . . . ? C17 C16 N6 C20 -2.7(6) . . . . ? C15 C16 N6 C20 175.6(3) . . . . ? C17 C16 N6 Co2 -179.6(3) . . . . ? C15 C16 N6 Co2 -1.2(4) . . . . ? O1W Co2 N6 C20 -4.0(3) 3 . . . ? O1W Co2 N6 C20 -89.6(3) . . . . ? N6 Co2 N6 C20 133.2(3) 3 . . . ? N5 Co2 N6 C20 85.1(3) 3 . . . ? N5 Co2 N6 C20 -178.1(3) . . . . ? O1W Co2 N6 C16 172.6(3) 3 . . . ? O1W Co2 N6 C16 87.0(3) . . . . ? N6 Co2 N6 C16 -50.2(3) 3 . . . ? N5 Co2 N6 C16 -98.3(3) 3 . . . ? N5 Co2 N6 C16 -1.5(3) . . . . ? O2 N7 O1 Co1 147.3(3) . . . . ? O3 N7 O1 Co1 -34.3(5) . . . . ? N2 Co1 O1 N7 102.8(6) . . . . ? N2 Co1 O1 N7 -20.6(3) 3 . . . ? O1 Co1 O1 N7 169.7(4) 3 . . . ? N1 Co1 O1 N7 -97.1(3) 3 . . . ? N1 Co1 O1 N7 84.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.341 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.058 #===END data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Cl Cu N8 O4, Cl O4' _chemical_formula_sum 'C26 H20 Cl2 Cu N8 O8' _chemical_formula_structural 'Cu 2+, C26 H20 N8, 2(Cl O4 -)' _chemical_formula_weight 706.94 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' '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 triclinic _symmetry_space_group_name_H-M 'p-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1298(6) _cell_length_b 12.3163(6) _cell_length_c 12.9485(7) _cell_angle_alpha 111.533(2) _cell_angle_beta 106.068(2) _cell_angle_gamma 99.921(2) _cell_volume 1374.57(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 850 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 21.98 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.782009 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details '(SADABS; Bruker, 1996)' _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 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7176 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.07 _reflns_number_total 4813 _reflns_number_gt 3331 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _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^)+(0.1569P)^2^+4.2860P] 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 4813 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2528 _refine_ls_wR_factor_gt 0.1984 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 -0.47284(9) -0.44227(8) -0.21300(8) 0.0406(3) Uani 1 1 d . . . C1 C -0.1814(8) 0.0091(7) 0.3460(6) 0.0414(17) Uani 1 1 d . . . C2 C -0.1630(9) 0.0609(8) 0.4686(7) 0.050(2) Uani 1 1 d . . . H2A H -0.2324 0.0317 0.4943 0.060 Uiso 1 1 calc R . . C3 C -0.0403(9) 0.1550(8) 0.5478(7) 0.054(2) Uani 1 1 d . . . H3A H -0.0264 0.1888 0.6286 0.065 Uiso 1 1 calc R . . C4 C 0.0640(9) 0.2018(8) 0.5124(7) 0.056(2) Uani 1 1 d . . . H4A H 0.1454 0.2666 0.5693 0.067 Uiso 1 1 calc R . . C5 C 0.0490(9) 0.1535(7) 0.3935(8) 0.051(2) Uani 1 1 d . . . H5A H 0.1192 0.1843 0.3694 0.062 Uiso 1 1 calc R . . C6 C -0.0785(8) 0.0547(6) 0.3090(6) 0.0383(16) Uani 1 1 d . . . C7 C -0.2117(8) -0.0834(6) 0.1148(6) 0.0372(16) Uani 1 1 d . . . C8 C -0.3177(8) -0.1307(6) 0.1530(6) 0.0369(16) Uani 1 1 d . . . C9 C -0.4485(9) -0.2420(7) 0.0703(7) 0.0447(18) Uani 1 1 d . . . H9A H -0.4160 -0.3135 0.0437 0.054 Uiso 1 1 calc R . . H9B H -0.5073 -0.2544 0.1152 0.054 Uiso 1 1 calc R . . C10 C -0.2231(9) -0.1321(7) -0.0140(6) 0.0405(17) Uani 1 1 d . . . H10A H -0.3229 -0.1538 -0.0656 0.049 Uiso 1 1 calc R . . H10B H -0.1663 -0.0680 -0.0248 0.049 Uiso 1 1 calc R . . C11 C -0.6345(10) -0.1718(8) -0.0430(8) 0.056(2) Uani 1 1 d . . . H11A H -0.6465 -0.1129 0.0205 0.068 Uiso 1 1 calc R . . C12 C -0.7116(10) -0.2106(8) -0.1616(8) 0.055(2) Uani 1 1 d . . . H12A H -0.7845 -0.1825 -0.1941 0.067 Uiso 1 1 calc R . . C13 C -0.6608(8) -0.2986(7) -0.2229(6) 0.0366(16) Uani 1 1 d . . . C14 C -0.7007(7) -0.3839(6) -0.3489(6) 0.0357(16) Uani 1 1 d . . . C15 C -0.8027(9) -0.3795(9) -0.4419(8) 0.056(2) Uani 1 1 d . . . H15A H -0.8490 -0.3196 -0.4276 0.067 Uiso 1 1 calc R . . C16 C -0.8344(10) -0.4659(9) -0.5564(8) 0.057(2) Uani 1 1 d . . . H16A H -0.9056 -0.4671 -0.6204 0.069 Uiso 1 1 calc R . . C17 C -0.7602(9) -0.5509(8) -0.5760(7) 0.051(2) Uani 1 1 d . . . H17A H -0.7797 -0.6088 -0.6531 0.061 Uiso 1 1 calc R . . C18 C -0.6579(8) -0.5483(7) -0.4804(6) 0.0416(17) Uani 1 1 d . . . H18A H -0.6082 -0.6057 -0.4935 0.050 Uiso 1 1 calc R . . C21 C -0.0348(8) -0.2391(8) -0.0198(7) 0.0468(19) Uani 1 1 d . . . H21A H 0.0461 -0.1705 0.0278 0.056 Uiso 1 1 calc R . . C22 C -0.0341(9) -0.3580(7) -0.0719(7) 0.0459(19) Uani 1 1 d . . . H22A H 0.0459 -0.3859 -0.0686 0.055 Uiso 1 1 calc R . . C23 C -0.1792(7) -0.4280(6) -0.1310(6) 0.0341(15) Uani 1 1 d . . . C24 C -0.2533(7) -0.5580(6) -0.2029(6) 0.0335(15) Uani 1 1 d . . . C25 C -0.1880(8) -0.6487(7) -0.2122(7) 0.0401(17) Uani 1 1 d . . . H25A H -0.0889 -0.6290 -0.1733 0.048 Uiso 1 1 calc R . . C26 C -0.2730(9) -0.7699(7) -0.2806(7) 0.0453(19) Uani 1 1 d . . . H26A H -0.2310 -0.8324 -0.2879 0.054 Uiso 1 1 calc R . . C27 C -0.4191(9) -0.7981(7) -0.3378(7) 0.050(2) Uani 1 1 d . . . H27A H -0.4770 -0.8791 -0.3844 0.060 Uiso 1 1 calc R . . C28 C -0.4775(9) -0.7036(7) -0.3243(7) 0.0454(18) Uani 1 1 d . . . H28A H -0.5766 -0.7225 -0.3619 0.054 Uiso 1 1 calc R . . N1 N -0.5381(6) -0.2340(5) -0.0344(5) 0.0389(14) Uani 1 1 d . . . N2 N -0.5565(6) -0.3147(5) -0.1462(5) 0.0357(13) Uani 1 1 d . . . N3 N -0.6261(6) -0.4646(5) -0.3665(5) 0.0353(13) Uani 1 1 d . . . N4 N -0.1727(6) -0.2394(5) -0.0496(5) 0.0354(13) Uani 1 1 d . . . N5 N -0.2630(6) -0.3546(5) -0.1159(5) 0.0321(13) Uani 1 1 d . . . N6 N -0.3980(6) -0.5849(5) -0.2591(5) 0.0358(13) Uani 1 1 d . . . N7 N -0.0943(7) 0.0083(5) 0.1907(6) 0.0412(14) Uani 1 1 d . . . N8 N -0.3036(7) -0.0865(5) 0.2656(5) 0.0390(14) Uani 1 1 d . . . O1 O -0.8585(6) -0.5359(6) -0.2390(6) 0.0634(17) Uani 1 1 d . . . O2 O -0.7253(7) -0.4621(6) -0.0363(5) 0.0674(18) Uani 1 1 d . . . O3 O -0.6393(6) -0.5746(5) -0.1790(6) 0.0570(16) Uani 1 1 d . . . O4 O -0.8381(6) -0.6720(5) -0.1538(5) 0.0517(14) Uani 1 1 d . . . O5 O -0.2812(16) -0.0018(8) -0.1909(8) 0.154(5) Uani 1 1 d . . . O6 O -0.3535(9) -0.2123(6) -0.2975(6) 0.076(2) Uani 1 1 d . . . O7 O -0.5068(16) -0.1019(14) -0.289(2) 0.280(13) Uani 1 1 d . . . O8 O -0.3554(14) -0.0800(9) -0.3867(8) 0.133(4) Uani 1 1 d . . . Cl1 Cl -0.76600(18) -0.56091(16) -0.15138(15) 0.0371(4) Uani 1 1 d . . . Cl2 Cl -0.3791(3) -0.1015(2) -0.2945(2) 0.0561(6) 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 0.0336(5) 0.0418(6) 0.0345(5) 0.0064(4) 0.0051(4) 0.0196(4) C1 0.039(4) 0.045(4) 0.034(4) 0.012(3) 0.007(3) 0.020(3) C2 0.048(5) 0.059(5) 0.031(4) 0.009(4) 0.011(4) 0.017(4) C3 0.043(5) 0.055(5) 0.037(4) 0.001(4) 0.007(4) 0.006(4) C4 0.037(5) 0.055(5) 0.041(5) -0.001(4) -0.002(4) 0.009(4) C5 0.040(4) 0.040(4) 0.056(5) 0.007(4) 0.014(4) 0.004(4) C6 0.039(4) 0.037(4) 0.040(4) 0.014(3) 0.018(3) 0.013(3) C7 0.050(4) 0.028(3) 0.034(4) 0.011(3) 0.013(3) 0.021(3) C8 0.044(4) 0.031(4) 0.032(4) 0.008(3) 0.014(3) 0.015(3) C9 0.052(5) 0.036(4) 0.036(4) 0.013(3) 0.009(4) 0.008(3) C10 0.047(4) 0.039(4) 0.034(4) 0.016(3) 0.015(3) 0.012(3) C11 0.064(6) 0.052(5) 0.049(5) 0.011(4) 0.020(4) 0.035(4) C12 0.058(5) 0.057(5) 0.055(5) 0.021(4) 0.015(4) 0.040(4) C13 0.033(4) 0.043(4) 0.042(4) 0.025(3) 0.013(3) 0.019(3) C14 0.031(4) 0.036(4) 0.038(4) 0.017(3) 0.009(3) 0.008(3) C15 0.047(5) 0.069(6) 0.053(5) 0.033(5) 0.008(4) 0.025(4) C16 0.057(5) 0.071(6) 0.041(5) 0.025(4) 0.012(4) 0.021(5) C17 0.051(5) 0.056(5) 0.034(4) 0.018(4) 0.007(4) 0.007(4) C18 0.041(4) 0.042(4) 0.037(4) 0.016(3) 0.011(3) 0.011(3) C21 0.032(4) 0.050(5) 0.044(4) 0.009(4) 0.011(3) 0.009(3) C22 0.037(4) 0.053(5) 0.048(5) 0.018(4) 0.020(4) 0.017(4) C23 0.031(4) 0.045(4) 0.029(3) 0.015(3) 0.013(3) 0.018(3) C24 0.029(4) 0.046(4) 0.033(4) 0.020(3) 0.016(3) 0.016(3) C25 0.042(4) 0.049(4) 0.042(4) 0.025(4) 0.019(3) 0.025(4) C26 0.049(5) 0.044(4) 0.058(5) 0.024(4) 0.030(4) 0.028(4) C27 0.054(5) 0.036(4) 0.049(5) 0.005(4) 0.025(4) 0.010(4) C28 0.038(4) 0.051(5) 0.039(4) 0.012(4) 0.013(3) 0.015(4) N1 0.035(3) 0.038(3) 0.035(3) 0.007(3) 0.010(3) 0.015(3) N2 0.030(3) 0.034(3) 0.037(3) 0.012(3) 0.007(3) 0.013(3) N3 0.037(3) 0.038(3) 0.024(3) 0.010(3) 0.007(2) 0.009(3) N4 0.038(3) 0.033(3) 0.033(3) 0.010(3) 0.017(3) 0.010(3) N5 0.032(3) 0.033(3) 0.029(3) 0.011(2) 0.008(2) 0.012(3) N6 0.030(3) 0.038(3) 0.033(3) 0.010(3) 0.008(3) 0.015(3) N7 0.042(4) 0.032(3) 0.045(4) 0.014(3) 0.014(3) 0.012(3) N8 0.041(4) 0.035(3) 0.034(3) 0.010(3) 0.012(3) 0.012(3) O1 0.048(4) 0.077(4) 0.076(4) 0.049(4) 0.012(3) 0.026(3) O2 0.073(4) 0.059(4) 0.046(4) 0.001(3) 0.027(3) 0.004(3) O3 0.052(4) 0.064(4) 0.091(5) 0.050(3) 0.047(3) 0.033(3) O4 0.046(3) 0.055(3) 0.054(3) 0.027(3) 0.018(3) 0.010(3) O5 0.256(15) 0.062(5) 0.074(6) 0.015(5) -0.003(7) 0.021(7) O6 0.113(6) 0.050(4) 0.076(5) 0.028(3) 0.044(4) 0.038(4) O7 0.195(14) 0.185(13) 0.68(4) 0.27(2) 0.31(2) 0.151(12) O8 0.250(13) 0.102(7) 0.072(6) 0.057(5) 0.060(7) 0.068(8) Cl1 0.0349(9) 0.0418(10) 0.0348(9) 0.0151(7) 0.0136(7) 0.0146(7) Cl2 0.0692(15) 0.0524(12) 0.0576(13) 0.0270(10) 0.0306(11) 0.0260(11) _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 N2 1.949(6) . ? Cu1 N6 1.989(6) . ? Cu1 N5 1.999(6) . ? Cu1 N3 2.045(6) . ? Cu1 O3 2.384(5) . ? C1 N8 1.374(9) . ? C1 C6 1.380(11) . ? C1 C2 1.419(10) . ? C2 C3 1.365(11) . ? C2 H2A 0.9300 . ? C3 C4 1.382(13) . ? C3 H3A 0.9300 . ? C4 C5 1.384(12) . ? C4 H4A 0.9300 . ? C5 C6 1.430(10) . ? C5 H5A 0.9300 . ? C6 N7 1.374(9) . ? C7 N7 1.316(9) . ? C7 C8 1.424(11) . ? C7 C10 1.514(10) . ? C8 N8 1.311(9) . ? C8 C9 1.514(10) . ? C9 N1 1.456(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.461(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N1 1.347(10) . ? C11 C12 1.365(12) . ? C11 H11A 0.9300 . ? C12 C13 1.363(10) . ? C12 H12A 0.9300 . ? C13 N2 1.333(9) . ? C13 C14 1.470(10) . ? C14 N3 1.342(9) . ? C14 C15 1.377(10) . ? C15 C16 1.376(12) . ? C15 H15A 0.9300 . ? C16 C17 1.380(12) . ? C16 H16A 0.9300 . ? C17 C18 1.363(11) . ? C17 H17A 0.9300 . ? C18 N3 1.359(9) . ? C18 H18A 0.9300 . ? C21 N4 1.342(10) . ? C21 C22 1.371(11) . ? C21 H21A 0.9300 . ? C22 C23 1.395(10) . ? C22 H22A 0.9300 . ? C23 N5 1.343(8) . ? C23 C24 1.448(10) . ? C24 N6 1.362(9) . ? C24 C25 1.379(10) . ? C25 C26 1.385(11) . ? C25 H25A 0.9300 . ? C26 C27 1.374(12) . ? C26 H26A 0.9300 . ? C27 C28 1.371(11) . ? C27 H27A 0.9300 . ? C28 N6 1.346(10) . ? C28 H28A 0.9300 . ? N1 N2 1.360(8) . ? N4 N5 1.346(8) . ? O1 Cl1 1.424(6) . ? O2 Cl1 1.424(6) . ? O3 Cl1 1.445(5) . ? O4 Cl1 1.420(6) . ? O5 Cl2 1.388(9) . ? O6 Cl2 1.422(6) . ? O7 Cl2 1.316(11) . ? O8 Cl2 1.385(9) . ? 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 N2 Cu1 N6 168.5(3) . . ? N2 Cu1 N5 100.6(2) . . ? N6 Cu1 N5 81.3(2) . . ? N2 Cu1 N3 80.1(2) . . ? N6 Cu1 N3 106.0(2) . . ? N5 Cu1 N3 139.0(2) . . ? N2 Cu1 O3 87.1(2) . . ? N6 Cu1 O3 83.0(2) . . ? N5 Cu1 O3 128.6(2) . . ? N3 Cu1 O3 92.4(2) . . ? N8 C1 C6 121.0(7) . . ? N8 C1 C2 118.6(7) . . ? C6 C1 C2 120.3(7) . . ? C3 C2 C1 118.0(8) . . ? C3 C2 H2A 121.0 . . ? C1 C2 H2A 121.0 . . ? C2 C3 C4 122.4(8) . . ? C2 C3 H3A 118.8 . . ? C4 C3 H3A 118.8 . . ? C3 C4 C5 120.9(8) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C4 C5 C6 117.6(8) . . ? C4 C5 H5A 121.2 . . ? C6 C5 H5A 121.2 . . ? N7 C6 C1 121.8(7) . . ? N7 C6 C5 117.5(7) . . ? C1 C6 C5 120.6(7) . . ? N7 C7 C8 121.7(6) . . ? N7 C7 C10 114.3(7) . . ? C8 C7 C10 123.9(7) . . ? N8 C8 C7 122.1(7) . . ? N8 C8 C9 114.2(6) . . ? C7 C8 C9 123.4(6) . . ? N1 C9 C8 114.6(6) . . ? N1 C9 H9A 108.6 . . ? C8 C9 H9A 108.6 . . ? N1 C9 H9B 108.6 . . ? C8 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? N4 C10 C7 112.3(6) . . ? N4 C10 H10A 109.1 . . ? C7 C10 H10A 109.1 . . ? N4 C10 H10B 109.1 . . ? C7 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? N1 C11 C12 107.9(7) . . ? N1 C11 H11A 126.1 . . ? C12 C11 H11A 126.1 . . ? C13 C12 C11 106.5(7) . . ? C13 C12 H12A 126.8 . . ? C11 C12 H12A 126.8 . . ? N2 C13 C12 109.7(7) . . ? N2 C13 C14 114.4(6) . . ? C12 C13 C14 135.6(7) . . ? N3 C14 C15 122.5(7) . . ? N3 C14 C13 114.2(6) . . ? C15 C14 C13 123.2(7) . . ? C16 C15 C14 118.3(8) . . ? C16 C15 H15A 120.8 . . ? C14 C15 H15A 120.8 . . ? C15 C16 C17 119.9(8) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 C16 118.8(8) . . ? C18 C17 H17A 120.6 . . ? C16 C17 H17A 120.6 . . ? N3 C18 C17 122.2(7) . . ? N3 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? N4 C21 C22 107.9(7) . . ? N4 C21 H21A 126.0 . . ? C22 C21 H21A 126.0 . . ? C21 C22 C23 105.2(7) . . ? C21 C22 H22A 127.4 . . ? C23 C22 H22A 127.4 . . ? N5 C23 C22 109.9(6) . . ? N5 C23 C24 116.4(6) . . ? C22 C23 C24 133.8(6) . . ? N6 C24 C25 121.7(7) . . ? N6 C24 C23 113.7(6) . . ? C25 C24 C23 124.6(6) . . ? C24 C25 C26 118.6(7) . . ? C24 C25 H25A 120.7 . . ? C26 C25 H25A 120.7 . . ? C27 C26 C25 120.3(7) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C28 C27 C26 118.3(7) . . ? C28 C27 H27A 120.8 . . ? C26 C27 H27A 120.9 . . ? N6 C28 C27 123.0(7) . . ? N6 C28 H28A 118.5 . . ? C27 C28 H28A 118.5 . . ? C11 N1 N2 108.8(6) . . ? C11 N1 C9 129.2(7) . . ? N2 N1 C9 120.5(6) . . ? C13 N2 N1 107.0(6) . . ? C13 N2 Cu1 117.3(5) . . ? N1 N2 Cu1 135.6(4) . . ? C14 N3 C18 118.1(6) . . ? C14 N3 Cu1 113.8(4) . . ? C18 N3 Cu1 128.0(5) . . ? C21 N4 N5 110.8(6) . . ? C21 N4 C10 126.3(6) . . ? N5 N4 C10 122.9(6) . . ? C23 N5 N4 106.2(5) . . ? C23 N5 Cu1 113.5(4) . . ? N4 N5 Cu1 139.6(4) . . ? C28 N6 C24 118.2(6) . . ? C28 N6 Cu1 126.4(5) . . ? C24 N6 Cu1 114.6(5) . . ? C7 N7 C6 116.4(6) . . ? C8 N8 C1 116.8(6) . . ? Cl1 O3 Cu1 130.7(3) . . ? O4 Cl1 O1 109.9(4) . . ? O4 Cl1 O2 110.1(4) . . ? O1 Cl1 O2 109.4(4) . . ? O4 Cl1 O3 108.7(3) . . ? O1 Cl1 O3 108.8(4) . . ? O2 Cl1 O3 110.0(4) . . ? O7 Cl2 O8 115.6(11) . . ? O7 Cl2 O5 105.4(12) . . ? O8 Cl2 O5 104.7(7) . . ? O7 Cl2 O6 109.2(6) . . ? O8 Cl2 O6 111.3(5) . . ? O5 Cl2 O6 110.4(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 N8 C1 C2 C3 179.2(7) . . . . ? C6 C1 C2 C3 -0.9(12) . . . . ? C1 C2 C3 C4 1.0(13) . . . . ? C2 C3 C4 C5 -0.8(14) . . . . ? C3 C4 C5 C6 0.5(13) . . . . ? N8 C1 C6 N7 1.2(11) . . . . ? C2 C1 C6 N7 -178.7(7) . . . . ? N8 C1 C6 C5 -179.4(7) . . . . ? C2 C1 C6 C5 0.7(11) . . . . ? C4 C5 C6 N7 178.9(7) . . . . ? C4 C5 C6 C1 -0.5(12) . . . . ? N7 C7 C8 N8 -0.7(11) . . . . ? C10 C7 C8 N8 179.5(6) . . . . ? N7 C7 C8 C9 -175.1(7) . . . . ? C10 C7 C8 C9 5.1(11) . . . . ? N8 C8 C9 N1 129.6(7) . . . . ? C7 C8 C9 N1 -55.6(10) . . . . ? N7 C7 C10 N4 96.6(7) . . . . ? C8 C7 C10 N4 -83.7(9) . . . . ? N1 C11 C12 C13 1.1(10) . . . . ? C11 C12 C13 N2 0.2(10) . . . . ? C11 C12 C13 C14 174.2(9) . . . . ? N2 C13 C14 N3 0.3(9) . . . . ? C12 C13 C14 N3 -173.5(9) . . . . ? N2 C13 C14 C15 -177.9(7) . . . . ? C12 C13 C14 C15 8.4(14) . . . . ? N3 C14 C15 C16 3.7(13) . . . . ? C13 C14 C15 C16 -178.4(8) . . . . ? C14 C15 C16 C17 -2.6(14) . . . . ? C15 C16 C17 C18 1.0(13) . . . . ? C16 C17 C18 N3 -0.3(12) . . . . ? N4 C21 C22 C23 -1.6(9) . . . . ? C21 C22 C23 N5 0.5(8) . . . . ? C21 C22 C23 C24 179.8(7) . . . . ? N5 C23 C24 N6 9.0(9) . . . . ? C22 C23 C24 N6 -170.2(8) . . . . ? N5 C23 C24 C25 -168.8(6) . . . . ? C22 C23 C24 C25 12.0(12) . . . . ? N6 C24 C25 C26 -0.1(10) . . . . ? C23 C24 C25 C26 177.5(7) . . . . ? C24 C25 C26 C27 0.1(11) . . . . ? C25 C26 C27 C28 -0.5(12) . . . . ? C26 C27 C28 N6 0.9(12) . . . . ? C12 C11 N1 N2 -2.0(10) . . . . ? C12 C11 N1 C9 -168.4(8) . . . . ? C8 C9 N1 C11 -77.3(10) . . . . ? C8 C9 N1 N2 117.7(7) . . . . ? C12 C13 N2 N1 -1.4(9) . . . . ? C14 C13 N2 N1 -176.8(6) . . . . ? C12 C13 N2 Cu1 177.1(6) . . . . ? C14 C13 N2 Cu1 1.7(8) . . . . ? C11 N1 N2 C13 2.1(8) . . . . ? C9 N1 N2 C13 169.9(6) . . . . ? C11 N1 N2 Cu1 -176.0(6) . . . . ? C9 N1 N2 Cu1 -8.2(10) . . . . ? N6 Cu1 N2 C13 -125.3(11) . . . . ? N5 Cu1 N2 C13 136.1(5) . . . . ? N3 Cu1 N2 C13 -2.2(5) . . . . ? O3 Cu1 N2 C13 -95.2(5) . . . . ? N6 Cu1 N2 N1 52.6(15) . . . . ? N5 Cu1 N2 N1 -45.9(7) . . . . ? N3 Cu1 N2 N1 175.8(7) . . . . ? O3 Cu1 N2 N1 82.8(7) . . . . ? C15 C14 N3 C18 -3.0(11) . . . . ? C13 C14 N3 C18 178.9(6) . . . . ? C15 C14 N3 Cu1 176.1(6) . . . . ? C13 C14 N3 Cu1 -2.0(8) . . . . ? C17 C18 N3 C14 1.2(11) . . . . ? C17 C18 N3 Cu1 -177.7(6) . . . . ? N2 Cu1 N3 C14 2.3(5) . . . . ? N6 Cu1 N3 C14 172.3(5) . . . . ? N5 Cu1 N3 C14 -92.6(6) . . . . ? O3 Cu1 N3 C14 88.9(5) . . . . ? N2 Cu1 N3 C18 -178.7(6) . . . . ? N6 Cu1 N3 C18 -8.8(7) . . . . ? N5 Cu1 N3 C18 86.4(7) . . . . ? O3 Cu1 N3 C18 -92.1(6) . . . . ? C22 C21 N4 N5 2.2(9) . . . . ? C22 C21 N4 C10 -179.5(6) . . . . ? C7 C10 N4 C21 -75.7(9) . . . . ? C7 C10 N4 N5 102.3(7) . . . . ? C22 C23 N5 N4 0.8(8) . . . . ? C24 C23 N5 N4 -178.6(5) . . . . ? C22 C23 N5 Cu1 172.9(5) . . . . ? C24 C23 N5 Cu1 -6.5(7) . . . . ? C21 N4 N5 C23 -1.9(8) . . . . ? C10 N4 N5 C23 179.8(6) . . . . ? C21 N4 N5 Cu1 -170.6(6) . . . . ? C10 N4 N5 Cu1 11.0(10) . . . . ? N2 Cu1 N5 C23 170.6(5) . . . . ? N6 Cu1 N5 C23 2.1(5) . . . . ? N3 Cu1 N5 C23 -102.3(5) . . . . ? O3 Cu1 N5 C23 75.8(5) . . . . ? N2 Cu1 N5 N4 -21.2(7) . . . . ? N6 Cu1 N5 N4 170.3(7) . . . . ? N3 Cu1 N5 N4 65.9(8) . . . . ? O3 Cu1 N5 N4 -116.0(6) . . . . ? C27 C28 N6 C24 -0.9(11) . . . . ? C27 C28 N6 Cu1 -170.0(6) . . . . ? C25 C24 N6 C28 0.5(10) . . . . ? C23 C24 N6 C28 -177.3(6) . . . . ? C25 C24 N6 Cu1 170.9(5) . . . . ? C23 C24 N6 Cu1 -7.0(7) . . . . ? N2 Cu1 N6 C28 71.8(14) . . . . ? N5 Cu1 N6 C28 172.3(6) . . . . ? N3 Cu1 N6 C28 -49.1(7) . . . . ? O3 Cu1 N6 C28 41.4(6) . . . . ? N2 Cu1 N6 C24 -97.6(12) . . . . ? N5 Cu1 N6 C24 2.9(5) . . . . ? N3 Cu1 N6 C24 141.5(5) . . . . ? O3 Cu1 N6 C24 -128.0(5) . . . . ? C8 C7 N7 C6 0.9(10) . . . . ? C10 C7 N7 C6 -179.3(6) . . . . ? C1 C6 N7 C7 -1.2(10) . . . . ? C5 C6 N7 C7 179.4(7) . . . . ? C7 C8 N8 C1 0.6(10) . . . . ? C9 C8 N8 C1 175.5(6) . . . . ? C6 C1 N8 C8 -0.9(10) . . . . ? C2 C1 N8 C8 179.0(7) . . . . ? N2 Cu1 O3 Cl1 13.9(5) . . . . ? N6 Cu1 O3 Cl1 -171.9(5) . . . . ? N5 Cu1 O3 Cl1 115.1(5) . . . . ? N3 Cu1 O3 Cl1 -66.1(5) . . . . ? Cu1 O3 Cl1 O4 173.0(4) . . . . ? Cu1 O3 Cl1 O1 53.5(6) . . . . ? Cu1 O3 Cl1 O2 -66.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.554 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.099 #===END data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 N19 Ni2 O4, 2(B F4), O4 S, 4(H2 O), 4(C H4 O)' _chemical_formula_sum 'C56 H72 B2 F8 N16 Ni2 O16 S' _chemical_formula_structural '2(Ni 2+), 2(C26 H20 N8), 2(B F4 -), O4 S 2-, 8(H2 O), 4(C H4 O)' _chemical_formula_weight 1540.33 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 '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 13.818(8) _cell_length_b 16.645(8) _cell_length_c 20.937(11) _cell_angle_alpha 109.508(10) _cell_angle_beta 107.144(9) _cell_angle_gamma 90.923(9) _cell_volume 4302(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1054 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 22.98 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.717342 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS; Bruker, 1996' _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 'bruker ccd area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24715 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.1689 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.51 _reflns_number_total 17324 _reflns_number_gt 6460 _reflns_threshold_expression I>2s\(I) _computing_data_collection 'BRUKER SMART, 1998' _computing_cell_refinement 'SMART' _computing_data_reduction 'BRUKER SAINT, 1998' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'shelxtl (sheldrick, 1997b)' _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^)+(0.1839P)^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 17324 _refine_ls_number_parameters 946 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2487 _refine_ls_R_factor_gt 0.1125 _refine_ls_wR_factor_ref 0.3636 _refine_ls_wR_factor_gt 0.2745 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.981 _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 Ni1 Ni 0.11923(9) 0.78731(7) 0.77522(6) 0.0532(4) Uani 1 1 d . . . Ni2 Ni 0.27117(8) 0.35911(7) 0.68041(5) 0.0508(3) Uani 1 1 d . . . B1 B 0.3164(12) 0.2543(14) 0.0659(9) 0.112(6) Uani 1 1 d . . . B2 B 0.154(4) 0.7618(15) 0.177(2) 0.206(18) Uani 1 1 d . . . C1 C -0.0075(8) 0.9412(6) 0.7943(5) 0.070(3) Uani 1 1 d . . . H1A H -0.0635 0.9014 0.7626 0.084 Uiso 1 1 calc R . . C2 C -0.0226(10) 1.0258(7) 0.8234(6) 0.085(3) Uani 1 1 d . . . H2A H -0.0874 1.0426 0.8115 0.101 Uiso 1 1 calc R . . C3 C 0.0588(10) 1.0838(7) 0.8694(6) 0.090(3) Uani 1 1 d . . . H3A H 0.0500 1.1409 0.8901 0.108 Uiso 1 1 calc R . . C4 C 0.1561(9) 1.0581(6) 0.8861(5) 0.077(3) Uani 1 1 d . . . H4A H 0.2122 1.0979 0.9176 0.092 Uiso 1 1 calc R . . C5 C 0.1681(8) 0.9742(6) 0.8557(5) 0.062(2) Uani 1 1 d . . . C6 C 0.2670(8) 0.9400(6) 0.8677(5) 0.064(2) Uani 1 1 d . . . C7 C 0.3652(8) 0.9793(6) 0.9078(6) 0.083(3) Uani 1 1 d . . . H7A H 0.3851 1.0367 0.9371 0.099 Uiso 1 1 calc R . . C8 C 0.4254(8) 0.9183(7) 0.8959(6) 0.083(3) Uani 1 1 d . . . H8A H 0.4960 0.9254 0.9162 0.100 Uiso 1 1 calc R . . C9 C 0.3980(8) 0.7594(6) 0.8222(5) 0.066(2) Uani 1 1 d . . . H9A H 0.4656 0.7665 0.8185 0.079 Uiso 1 1 calc R . . H9B H 0.3516 0.7282 0.7746 0.079 Uiso 1 1 calc R . . C10 C 0.3997(6) 0.7065(5) 0.8690(4) 0.053(2) Uani 1 1 d . . . C11 C 0.3939(7) 0.6983(7) 0.9741(5) 0.067(3) Uani 1 1 d . . . C12 C 0.3848(9) 0.7369(8) 1.0433(6) 0.095(4) Uani 1 1 d . . . H12A H 0.3779 0.7950 1.0605 0.114 Uiso 1 1 calc R . . C13 C 0.3864(10) 0.6877(11) 1.0843(6) 0.105(4) Uani 1 1 d . . . H13A H 0.3840 0.7136 1.1305 0.126 Uiso 1 1 calc R . . C14 C 0.3914(10) 0.6022(10) 1.0593(6) 0.105(4) Uani 1 1 d . . . H14A H 0.3872 0.5691 1.0867 0.125 Uiso 1 1 calc R . . C15 C 0.4029(9) 0.5644(8) 0.9928(5) 0.084(3) Uani 1 1 d . . . H15A H 0.4103 0.5063 0.9771 0.101 Uiso 1 1 calc R . . C16 C 0.4038(7) 0.6104(6) 0.9492(5) 0.061(2) Uani 1 1 d . . . C17 C 0.4155(6) 0.6181(5) 0.8449(4) 0.052(2) Uani 1 1 d . . . C18 C 0.4296(7) 0.5774(5) 0.7735(4) 0.058(2) Uani 1 1 d . . . H18A H 0.3634 0.5651 0.7369 0.070 Uiso 1 1 calc R . . H18B H 0.4715 0.6184 0.7659 0.070 Uiso 1 1 calc R . . C19 C 0.5784(7) 0.4933(6) 0.7861(5) 0.063(2) Uani 1 1 d . . . H19A H 0.6298 0.5395 0.8108 0.075 Uiso 1 1 calc R . . C20 C 0.5913(8) 0.4092(6) 0.7655(5) 0.065(2) Uani 1 1 d . . . H20A H 0.6527 0.3861 0.7734 0.078 Uiso 1 1 calc R . . C21 C 0.4929(7) 0.3643(6) 0.7296(4) 0.055(2) Uani 1 1 d . . . C22 C 0.4561(7) 0.2724(5) 0.6943(4) 0.059(2) Uani 1 1 d . . . C23 C 0.5203(9) 0.2097(7) 0.6922(6) 0.083(3) Uani 1 1 d . . . H23A H 0.5906 0.2241 0.7129 0.099 Uiso 1 1 calc R . . C24 C 0.4764(11) 0.1235(7) 0.6579(7) 0.104(4) Uani 1 1 d . . . H24A H 0.5168 0.0795 0.6587 0.125 Uiso 1 1 calc R . . C25 C 0.3729(10) 0.1051(7) 0.6230(6) 0.094(4) Uani 1 1 d . . . H25A H 0.3433 0.0486 0.5969 0.113 Uiso 1 1 calc R . . C26 C 0.3131(8) 0.1716(6) 0.6272(5) 0.076(3) Uani 1 1 d . . . H26A H 0.2428 0.1583 0.6054 0.091 Uiso 1 1 calc R . . C27 C 0.3292(8) 0.3546(6) 0.8343(5) 0.069(3) Uani 1 1 d . . . H27A H 0.3906 0.3864 0.8427 0.083 Uiso 1 1 calc R . . C28 C 0.3167(9) 0.3300(7) 0.8877(5) 0.080(3) Uani 1 1 d . . . H28A H 0.3691 0.3422 0.9307 0.096 Uiso 1 1 calc R . . C29 C 0.2229(11) 0.2861(7) 0.8755(6) 0.096(4) Uani 1 1 d . . . H29A H 0.2110 0.2701 0.9114 0.115 Uiso 1 1 calc R . . C30 C 0.1469(9) 0.2660(7) 0.8101(5) 0.084(3) Uani 1 1 d . . . H30A H 0.0837 0.2374 0.8022 0.101 Uiso 1 1 calc R . . C31 C 0.1652(8) 0.2886(6) 0.7573(5) 0.066(2) Uani 1 1 d . . . C32 C 0.0933(7) 0.2673(6) 0.6872(5) 0.062(2) Uani 1 1 d . . . C33 C -0.0047(9) 0.2288(8) 0.6597(6) 0.101(4) Uani 1 1 d . . . H33A H -0.0421 0.2082 0.6827 0.121 Uiso 1 1 calc R . . C34 C -0.0373(9) 0.2270(8) 0.5887(7) 0.099(4) Uani 1 1 d . . . H34A H -0.1010 0.2041 0.5547 0.119 Uiso 1 1 calc R . . C35 C 0.0448(7) 0.2802(6) 0.5167(5) 0.070(3) Uani 1 1 d . . . H35A H 0.0830 0.3361 0.5308 0.085 Uiso 1 1 calc R . . H35B H -0.0244 0.2818 0.4885 0.085 Uiso 1 1 calc R . . C36 C 0.0926(7) 0.2129(6) 0.4704(4) 0.063(2) Uani 1 1 d . . . C37 C 0.1560(8) 0.0836(6) 0.4408(6) 0.075(3) Uani 1 1 d . . . C38 C 0.1767(10) 0.0042(8) 0.4535(7) 0.106(4) Uani 1 1 d . . . H38A H 0.1606 -0.0068 0.4902 0.127 Uiso 1 1 calc R . . C39 C 0.2203(11) -0.0543(8) 0.4107(10) 0.123(5) Uani 1 1 d . . . H39A H 0.2321 -0.1065 0.4168 0.147 Uiso 1 1 calc R . . C40 C 0.2473(12) -0.0347(10) 0.3571(10) 0.128(6) Uani 1 1 d . . . H40A H 0.2790 -0.0739 0.3292 0.154 Uiso 1 1 calc R . . C41 C 0.2290(11) 0.0372(10) 0.3453(7) 0.121(5) Uani 1 1 d . . . H41A H 0.2475 0.0476 0.3093 0.145 Uiso 1 1 calc R . . C42 C 0.1811(8) 0.0995(8) 0.3872(6) 0.085(3) Uani 1 1 d . . . C43 C 0.1158(7) 0.2278(6) 0.4137(5) 0.066(2) Uani 1 1 d . . . C44 C -0.0932(9) 0.6922(7) 0.6018(5) 0.079(3) Uani 1 1 d . . . H44A H -0.1369 0.6439 0.5622 0.095 Uiso 1 1 calc R . . H44B H -0.0231 0.6840 0.6039 0.095 Uiso 1 1 calc R . . C45 C -0.1885(11) 0.6587(10) 0.6755(8) 0.130(5) Uani 1 1 d . . . H45A H -0.2485 0.6301 0.6392 0.156 Uiso 1 1 calc R . . C46 C -0.1696(11) 0.6746(12) 0.7468(9) 0.147(7) Uani 1 1 d . . . H46A H -0.2138 0.6608 0.7686 0.176 Uiso 1 1 calc R . . C47 C -0.0717(9) 0.7153(7) 0.7790(6) 0.077(3) Uani 1 1 d . . . C48 C -0.0056(9) 0.7411(6) 0.8520(6) 0.073(3) Uani 1 1 d . . . C49 C -0.0401(10) 0.7305(8) 0.9048(7) 0.099(4) Uani 1 1 d . . . H49A H -0.1074 0.7088 0.8949 0.119 Uiso 1 1 calc R . . C50 C 0.0292(13) 0.7532(9) 0.9727(7) 0.108(4) Uani 1 1 d . . . H50A H 0.0094 0.7450 1.0091 0.129 Uiso 1 1 calc R . . C51 C 0.1285(11) 0.7884(9) 0.9867(6) 0.098(4) Uani 1 1 d . . . H51A H 0.1750 0.8055 1.0326 0.118 Uiso 1 1 calc R . . C52 C 0.1566(9) 0.7975(6) 0.9318(5) 0.074(3) Uani 1 1 d . . . H52A H 0.2228 0.8213 0.9410 0.089 Uiso 1 1 calc R . . C53 C 0.1150(18) 1.0122(14) 0.6668(13) 0.194(9) Uani 1 1 d . . . C54 C 0.382(3) 0.1362(17) 0.810(2) 0.32(2) Uani 1 1 d . . . C55 C 0.1425(19) 0.5431(15) 0.8754(13) 0.197(9) Uani 1 1 d . . . C56 C 0.139(3) 0.505(3) 0.096(3) 0.35(3) Uani 1 1 d . . . N1 N 0.0857(6) 0.9138(4) 0.8100(4) 0.0583(18) Uani 1 1 d . . . N2 N 0.2678(5) 0.8554(4) 0.8316(3) 0.0512(17) Uani 1 1 d . . . N3 N 0.3665(6) 0.8437(5) 0.8493(4) 0.0609(19) Uani 1 1 d . . . N4 N 0.3912(6) 0.7460(5) 0.9321(4) 0.067(2) Uani 1 1 d . . . N5 N 0.4156(6) 0.5707(5) 0.8836(4) 0.0612(19) Uani 1 1 d . . . N6 N 0.4770(6) 0.4978(4) 0.7643(4) 0.0559(18) Uani 1 1 d . . . N7 N 0.4237(5) 0.4199(4) 0.7300(3) 0.0487(16) Uani 1 1 d . . . N8 N 0.3526(6) 0.2540(4) 0.6613(3) 0.0549(18) Uani 1 1 d . . . N9 N 0.2567(6) 0.3352(4) 0.7697(3) 0.0547(17) Uani 1 1 d . . . N10 N 0.1244(6) 0.2888(4) 0.6387(4) 0.0566(18) Uani 1 1 d . . . N11 N 0.0420(6) 0.2651(5) 0.5797(4) 0.069(2) Uani 1 1 d . . . N12 N 0.1103(6) 0.1408(5) 0.4843(4) 0.075(2) Uani 1 1 d . . . N13 N 0.1599(7) 0.1731(6) 0.3724(5) 0.086(3) Uani 1 1 d . . . N14 N -0.1069(7) 0.6908(6) 0.6667(4) 0.079(2) Uani 1 1 d . . . N15 N -0.0332(6) 0.7261(4) 0.7312(4) 0.063(2) Uani 1 1 d . . . N16 N 0.0905(7) 0.7727(5) 0.8642(4) 0.063(2) Uani 1 1 d . . . O1 O 0.1291(5) 0.7980(4) 0.6809(3) 0.0681(17) Uani 1 1 d . . . O1W O 0.0916(19) 0.522(2) 0.2298(17) 0.401(16) Uani 1 1 d . . . O2 O 0.1689(5) 0.6667(3) 0.7491(3) 0.0685(17) Uani 1 1 d . . . O2W O 0.0310(9) 0.4920(8) 0.6059(7) 0.178(5) Uani 1 1 d . . . O3 O 0.2015(5) 0.4704(4) 0.7030(3) 0.0718(18) Uani 1 1 d . . . O3W O 0.7165(19) 0.193(4) 0.487(4) 1.04(8) Uani 1 1 d . . . O4 O 0.2715(5) 0.3749(4) 0.5858(3) 0.0700(17) Uani 1 1 d . . . O4W O 0.4053(16) 0.3103(13) 0.5211(13) 0.301(11) Uani 1 1 d . . . O5 O 0.2043(15) 0.7048(13) 0.5649(13) 0.147(8) Uani 0.50 1 d P A 1 O6 O 0.3329(9) 0.6276(9) 0.5493(9) 0.161(6) Uani 0.80 1 d P A 1 O7 O 0.2573(15) 0.6190(18) 0.6449(7) 0.133(8) Uani 0.50 1 d P A 1 O8 O 0.202(3) 0.5097(12) 0.5128(14) 0.276(16) Uani 0.60 1 d P A 1 O5' O 0.275(2) 0.7003(18) 0.6361(15) 0.174(9) Uani 0.50 1 d PU A 2 O6' O 0.1133(16) 0.6121(13) 0.5701(11) 0.032(5) Uani 0.20 1 d PU A 2 O7' O 0.2851(17) 0.5390(14) 0.5946(18) 0.174(11) Uani 0.50 1 d P A 2 O8' O 0.1675(19) 0.596(2) 0.4780(10) 0.141(10) Uani 0.40 1 d P A 2 O9 O 0.1777(10) 0.9542(7) 0.6826(7) 0.169(5) Uani 1 1 d . . . O10 O 0.3759(16) 0.0463(18) 0.7704(13) 0.287(10) Uani 1 1 d . . . O11 O 0.0966(10) 0.5403(7) 0.7987(7) 0.155(4) Uani 1 1 d . . . O12 O 0.161(5) 0.427(6) 0.032(4) 1.00(12) Uani 1 1 d . . . F1 F 0.3621(8) 0.3136(11) 0.0451(7) 0.242(7) Uani 1 1 d . . . F2 F 0.2184(5) 0.2360(5) 0.0249(4) 0.124(3) Uani 1 1 d . . . F3 F 0.3385(9) 0.2919(6) 0.1335(5) 0.178(4) Uani 1 1 d . . . F4 F 0.3628(9) 0.1812(8) 0.0475(8) 0.248(8) Uani 1 1 d . . . F5 F 0.127(2) 0.6999(14) 0.1211(8) 0.389(16) Uani 1 1 d . . . F6 F 0.2206(13) 0.7294(13) 0.2235(13) 0.347(14) Uani 1 1 d . . . F7 F 0.0957(10) 0.7927(10) 0.2059(13) 0.271(8) Uani 1 1 d . . . F8 F 0.2176(16) 0.8211(10) 0.1752(9) 0.287(9) Uani 1 1 d . . . S1 S 0.2320(4) 0.6038(3) 0.5606(2) 0.1273(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 Ni1 0.0637(8) 0.0507(7) 0.0473(7) 0.0183(5) 0.0193(6) 0.0125(5) Ni2 0.0546(7) 0.0538(7) 0.0425(6) 0.0180(5) 0.0121(5) 0.0097(5) B1 0.052(9) 0.175(18) 0.082(11) 0.021(11) 0.011(8) -0.016(10) B2 0.36(5) 0.092(15) 0.24(3) 0.005(17) 0.25(4) -0.01(2) C1 0.074(7) 0.076(7) 0.060(6) 0.030(5) 0.015(5) 0.018(5) C2 0.095(9) 0.076(7) 0.078(7) 0.022(6) 0.024(7) 0.042(7) C3 0.110(10) 0.063(7) 0.089(8) 0.013(6) 0.035(8) 0.030(7) C4 0.088(8) 0.059(6) 0.072(7) 0.014(5) 0.017(6) 0.014(5) C5 0.079(7) 0.052(5) 0.052(5) 0.016(4) 0.018(5) 0.017(5) C6 0.074(7) 0.057(6) 0.053(5) 0.016(4) 0.014(5) 0.002(5) C7 0.078(8) 0.050(6) 0.092(8) 0.014(5) 0.000(6) 0.011(5) C8 0.060(7) 0.078(7) 0.091(8) 0.025(6) -0.002(6) -0.003(6) C9 0.065(6) 0.076(6) 0.060(6) 0.025(5) 0.023(5) 0.015(5) C10 0.046(5) 0.062(5) 0.046(5) 0.017(4) 0.009(4) 0.006(4) C11 0.053(6) 0.098(8) 0.043(5) 0.020(5) 0.009(4) 0.025(5) C12 0.105(10) 0.125(10) 0.070(7) 0.038(7) 0.043(7) 0.050(8) C13 0.108(10) 0.165(13) 0.044(6) 0.034(8) 0.031(6) 0.037(9) C14 0.110(11) 0.147(13) 0.066(8) 0.050(8) 0.027(7) 0.025(9) C15 0.088(8) 0.101(8) 0.058(6) 0.031(6) 0.014(6) 0.005(6) C16 0.051(6) 0.088(7) 0.051(5) 0.034(5) 0.015(4) 0.004(5) C17 0.044(5) 0.063(5) 0.039(4) 0.017(4) 0.002(4) 0.002(4) C18 0.065(6) 0.048(5) 0.055(5) 0.015(4) 0.015(5) -0.003(4) C19 0.047(6) 0.071(6) 0.061(6) 0.017(5) 0.013(5) -0.009(4) C20 0.060(6) 0.071(6) 0.060(6) 0.017(5) 0.020(5) 0.013(5) C21 0.053(6) 0.067(6) 0.047(5) 0.021(4) 0.016(4) 0.009(4) C22 0.060(6) 0.058(5) 0.052(5) 0.020(4) 0.008(4) 0.019(4) C23 0.072(7) 0.082(8) 0.086(8) 0.025(6) 0.019(6) 0.025(6) C24 0.098(10) 0.065(8) 0.127(11) 0.017(7) 0.024(8) 0.024(7) C25 0.088(9) 0.060(7) 0.107(9) 0.015(6) 0.010(7) 0.010(6) C26 0.072(7) 0.063(7) 0.082(7) 0.027(5) 0.008(6) 0.008(5) C27 0.074(7) 0.074(6) 0.054(6) 0.024(5) 0.012(5) -0.004(5) C28 0.089(8) 0.091(8) 0.050(6) 0.034(5) 0.001(5) -0.015(6) C29 0.135(12) 0.093(8) 0.070(7) 0.042(6) 0.034(8) -0.011(8) C30 0.087(8) 0.105(8) 0.061(7) 0.037(6) 0.015(6) -0.019(6) C31 0.075(7) 0.060(6) 0.066(6) 0.022(5) 0.028(5) -0.001(5) C32 0.055(6) 0.075(6) 0.052(5) 0.021(5) 0.012(5) 0.003(5) C33 0.068(8) 0.155(12) 0.070(8) 0.040(7) 0.011(6) -0.028(7) C34 0.053(7) 0.134(11) 0.093(9) 0.032(7) 0.009(6) -0.020(7) C35 0.058(6) 0.084(7) 0.048(5) 0.020(5) -0.010(5) 0.008(5) C36 0.053(6) 0.080(7) 0.036(5) 0.012(4) -0.003(4) 0.006(5) C37 0.068(7) 0.060(6) 0.070(7) 0.011(5) -0.004(6) 0.008(5) C38 0.097(10) 0.078(8) 0.110(10) 0.026(7) -0.005(8) 0.007(7) C39 0.096(11) 0.065(8) 0.150(15) 0.008(9) -0.010(10) 0.012(7) C40 0.117(13) 0.096(12) 0.122(13) 0.003(9) 0.006(10) 0.035(9) C41 0.109(11) 0.125(12) 0.089(10) 0.008(8) 0.009(8) 0.043(9) C42 0.071(8) 0.089(8) 0.058(7) 0.001(6) -0.002(6) 0.022(6) C43 0.065(6) 0.070(6) 0.041(5) 0.013(4) -0.006(4) -0.001(5) C44 0.087(8) 0.086(7) 0.056(6) 0.024(5) 0.014(6) 0.002(6) C45 0.079(10) 0.197(16) 0.117(12) 0.076(11) 0.013(8) -0.034(9) C46 0.088(11) 0.25(2) 0.124(13) 0.110(13) 0.021(9) -0.033(11) C47 0.070(8) 0.101(8) 0.084(8) 0.056(6) 0.032(6) 0.015(6) C48 0.077(8) 0.086(7) 0.070(7) 0.029(5) 0.044(6) 0.018(6) C49 0.088(9) 0.148(11) 0.089(9) 0.059(8) 0.049(8) 0.025(8) C50 0.138(13) 0.140(11) 0.085(9) 0.060(8) 0.070(9) 0.046(10) C51 0.103(11) 0.149(11) 0.065(7) 0.054(7) 0.038(7) 0.037(9) C52 0.083(8) 0.089(7) 0.062(6) 0.032(5) 0.032(6) 0.030(6) C53 0.21(2) 0.160(18) 0.24(2) 0.118(17) 0.044(18) 0.007(16) C54 0.28(4) 0.129(19) 0.42(5) -0.03(2) 0.05(3) 0.02(2) C55 0.21(2) 0.22(2) 0.164(19) 0.066(16) 0.065(17) 0.042(17) C56 0.28(4) 0.33(4) 0.60(8) 0.33(5) 0.16(5) -0.01(3) N1 0.066(5) 0.059(5) 0.050(4) 0.017(3) 0.020(4) 0.022(4) N2 0.063(5) 0.046(4) 0.042(4) 0.013(3) 0.016(3) 0.013(3) N3 0.050(5) 0.065(5) 0.065(5) 0.023(4) 0.014(4) 0.017(4) N4 0.072(6) 0.076(5) 0.056(5) 0.029(4) 0.018(4) 0.026(4) N5 0.060(5) 0.070(5) 0.057(5) 0.031(4) 0.014(4) 0.005(4) N6 0.064(5) 0.057(5) 0.047(4) 0.020(3) 0.017(4) -0.001(4) N7 0.056(5) 0.043(4) 0.046(4) 0.011(3) 0.020(3) 0.004(3) N8 0.063(5) 0.052(4) 0.042(4) 0.015(3) 0.007(4) 0.013(3) N9 0.057(5) 0.064(5) 0.036(4) 0.016(3) 0.009(3) 0.010(4) N10 0.054(5) 0.065(5) 0.047(4) 0.018(3) 0.014(4) 0.014(3) N11 0.052(5) 0.102(6) 0.047(5) 0.028(4) 0.005(4) 0.007(4) N12 0.076(6) 0.068(5) 0.059(5) 0.019(4) -0.005(4) 0.002(4) N13 0.088(7) 0.091(7) 0.063(6) 0.015(5) 0.016(5) 0.013(5) N14 0.064(6) 0.098(6) 0.065(6) 0.036(5) 0.001(5) -0.010(5) N15 0.075(6) 0.059(5) 0.057(5) 0.024(4) 0.018(4) 0.012(4) N16 0.073(6) 0.073(5) 0.058(5) 0.030(4) 0.032(4) 0.030(4) O1 0.086(5) 0.069(4) 0.052(4) 0.022(3) 0.025(3) 0.010(3) O1W 0.23(2) 0.59(5) 0.44(4) 0.29(3) 0.07(2) -0.04(2) O2 0.081(5) 0.047(3) 0.080(4) 0.020(3) 0.030(4) 0.020(3) O2W 0.151(11) 0.179(11) 0.186(11) 0.100(9) -0.011(8) 0.032(8) O3 0.082(5) 0.053(4) 0.079(4) 0.024(3) 0.023(4) 0.018(3) O3W 0.23(3) 1.58(14) 1.77(16) 1.60(15) -0.18(5) -0.21(5) O4 0.082(5) 0.080(4) 0.046(3) 0.026(3) 0.013(3) 0.003(3) O4W 0.27(2) 0.32(2) 0.45(3) 0.19(2) 0.23(2) 0.075(18) O5 0.127(16) 0.145(16) 0.23(2) 0.132(17) 0.074(17) 0.096(14) O6 0.102(9) 0.205(13) 0.250(16) 0.117(12) 0.120(11) 0.022(8) O7 0.145(17) 0.24(2) 0.032(8) 0.067(11) 0.029(9) 0.021(16) O8 0.38(4) 0.076(12) 0.19(2) -0.092(14) -0.01(2) -0.037(17) O5' 0.173(10) 0.173(10) 0.171(10) 0.047(6) 0.062(6) 0.026(5) O6' 0.025(6) 0.033(6) 0.041(6) 0.012(4) 0.015(5) 0.018(4) O7' 0.16(2) 0.113(16) 0.30(3) 0.17(2) 0.03(2) 0.030(14) O8' 0.14(2) 0.24(3) 0.057(12) 0.098(17) 0.004(12) 0.048(19) O9 0.191(12) 0.118(9) 0.235(13) 0.099(9) 0.083(10) 0.012(8) O10 0.27(2) 0.38(3) 0.33(2) 0.24(2) 0.12(2) 0.05(2) O11 0.167(11) 0.162(10) 0.172(11) 0.063(8) 0.101(9) 0.045(8) O12 0.45(8) 1.16(18) 0.87(14) -0.36(13) 0.28(8) -0.31(10) F1 0.114(8) 0.41(2) 0.252(13) 0.212(14) 0.018(8) -0.033(10) F2 0.063(5) 0.162(7) 0.102(5) 0.007(4) 0.009(4) -0.008(4) F3 0.221(12) 0.175(9) 0.081(6) 0.012(5) 0.008(6) -0.037(7) F4 0.119(9) 0.172(10) 0.318(16) -0.038(10) 0.016(9) 0.041(7) F5 0.61(4) 0.29(2) 0.150(12) 0.020(13) 0.020(18) -0.19(2) F6 0.225(17) 0.34(2) 0.48(3) 0.28(2) -0.047(17) 0.076(15) F7 0.160(11) 0.234(14) 0.48(3) 0.124(16) 0.194(15) 0.062(10) F8 0.43(3) 0.207(13) 0.324(19) 0.081(13) 0.27(2) 0.029(14) S1 0.161(4) 0.156(4) 0.109(3) 0.075(3) 0.073(3) 0.056(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 Ni1 O2 2.081(5) . ? Ni1 O1 2.083(6) . ? Ni1 N1 2.094(7) . ? Ni1 N16 2.103(7) . ? Ni1 N15 2.117(8) . ? Ni1 N2 2.120(7) . ? Ni2 O3 2.079(6) . ? Ni2 O4 2.084(6) . ? Ni2 N8 2.085(7) . ? Ni2 N9 2.099(7) . ? Ni2 N10 2.108(8) . ? Ni2 N7 2.117(7) . ? B1 F3 1.279(17) . ? B1 F2 1.338(15) . ? B1 F4 1.38(2) . ? B1 F1 1.41(2) . ? B2 F7 1.18(2) . ? B2 F5 1.22(3) . ? B2 F8 1.32(3) . ? B2 F6 1.39(5) . ? C1 N1 1.359(11) . ? C1 C2 1.382(13) . ? C1 H1A 0.9300 . ? C2 C3 1.353(15) . ? C2 H2A 0.9300 . ? C3 C4 1.398(15) . ? C3 H3A 0.9300 . ? C4 C5 1.364(12) . ? C4 H4A 0.9300 . ? C5 N1 1.378(12) . ? C5 C6 1.473(13) . ? C6 N2 1.360(10) . ? C6 C7 1.381(13) . ? C7 C8 1.329(13) . ? C7 H7A 0.9300 . ? C8 N3 1.358(12) . ? C8 H8A 0.9300 . ? C9 N3 1.455(11) . ? C9 C10 1.513(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.306(10) . ? C10 C17 1.431(11) . ? C11 N4 1.361(11) . ? C11 C16 1.404(13) . ? C11 C12 1.418(13) . ? C12 C13 1.367(16) . ? C12 H12A 0.9300 . ? C13 C14 1.354(17) . ? C13 H13A 0.9300 . ? C14 C15 1.381(15) . ? C14 H14A 0.9300 . ? C15 C16 1.376(13) . ? C15 H15A 0.9300 . ? C16 N5 1.372(11) . ? C17 N5 1.307(10) . ? C17 C18 1.494(11) . ? C18 N6 1.466(10) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N6 1.351(11) . ? C19 C20 1.352(12) . ? C19 H19A 0.9300 . ? C20 C21 1.401(12) . ? C20 H20A 0.9300 . ? C21 N7 1.342(10) . ? C21 C22 1.464(12) . ? C22 N8 1.370(11) . ? C22 C23 1.378(12) . ? C23 C24 1.402(15) . ? C23 H23A 0.9300 . ? C24 C25 1.377(16) . ? C24 H24A 0.9300 . ? C25 C26 1.387(14) . ? C25 H25A 0.9300 . ? C26 N8 1.335(11) . ? C26 H26A 0.9300 . ? C27 N9 1.356(11) . ? C27 C28 1.365(12) . ? C27 H27A 0.9300 . ? C28 C29 1.389(15) . ? C28 H28A 0.9300 . ? C29 C30 1.388(15) . ? C29 H29A 0.9300 . ? C30 C31 1.365(12) . ? C30 H30A 0.9300 . ? C31 N9 1.382(11) . ? C31 C32 1.432(13) . ? C32 N10 1.357(11) . ? C32 C33 1.357(13) . ? C33 C34 1.411(15) . ? C33 H33A 0.9300 . ? C34 N11 1.348(13) . ? C34 H34A 0.9300 . ? C35 N11 1.435(11) . ? C35 C36 1.519(12) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N12 1.336(11) . ? C36 C43 1.412(13) . ? C37 C42 1.369(15) . ? C37 N12 1.383(13) . ? C37 C38 1.451(15) . ? C38 C39 1.367(18) . ? C38 H38A 0.9300 . ? C39 C40 1.41(2) . ? C39 H39A 0.9300 . ? C40 C41 1.313(19) . ? C40 H40A 0.9300 . ? C41 C42 1.428(15) . ? C41 H41A 0.9300 . ? C42 N13 1.376(14) . ? C43 N13 1.322(12) . ? C43 C44 1.489(13) 2_566 ? C44 N14 1.435(12) . ? C44 C43 1.489(13) 2_566 ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 N14 1.326(14) . ? C45 C46 1.367(18) . ? C45 H45A 0.9300 . ? C46 C47 1.368(17) . ? C46 H46A 0.9300 . ? C47 N15 1.321(11) . ? C47 C48 1.442(14) . ? C48 N16 1.340(12) . ? C48 C49 1.385(13) . ? C49 C50 1.380(17) . ? C49 H49A 0.9300 . ? C50 C51 1.391(18) . ? C50 H50A 0.9300 . ? C51 C52 1.368(14) . ? C51 H51A 0.9300 . ? C52 N16 1.357(12) . ? C52 H52A 0.9300 . ? C53 O9 1.37(2) . ? C54 O10 1.44(3) . ? C55 O11 1.53(2) . ? C56 O12 1.64(6) . ? N2 N3 1.339(9) . ? N6 N7 1.332(9) . ? N10 N11 1.344(9) . ? N14 N15 1.358(10) . ? O5 S1 1.709(16) . ? O6 S1 1.547(10) . ? O7 S1 1.622(12) . ? O8 S1 1.521(14) . ? O5' S1 1.77(3) . ? O6' S1 1.71(2) . ? O7' S1 1.560(14) . ? O8' S1 1.655(16) . ? 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 O2 Ni1 O1 90.7(2) . . ? O2 Ni1 N1 173.5(3) . . ? O1 Ni1 N1 91.1(2) . . ? O2 Ni1 N16 90.6(3) . . ? O1 Ni1 N16 173.2(3) . . ? N1 Ni1 N16 88.3(3) . . ? O2 Ni1 N15 88.8(3) . . ? O1 Ni1 N15 95.8(3) . . ? N1 Ni1 N15 97.2(3) . . ? N16 Ni1 N15 77.5(3) . . ? O2 Ni1 N2 94.8(3) . . ? O1 Ni1 N2 90.4(3) . . ? N1 Ni1 N2 79.0(3) . . ? N16 Ni1 N2 96.1(3) . . ? N15 Ni1 N2 172.8(3) . . ? O3 Ni2 O4 87.8(2) . . ? O3 Ni2 N8 175.3(3) . . ? O4 Ni2 N8 91.7(3) . . ? O3 Ni2 N9 92.6(3) . . ? O4 Ni2 N9 174.2(3) . . ? N8 Ni2 N9 88.4(3) . . ? O3 Ni2 N10 87.7(3) . . ? O4 Ni2 N10 96.0(3) . . ? N8 Ni2 N10 97.0(3) . . ? N9 Ni2 N10 78.2(3) . . ? O3 Ni2 N7 96.7(3) . . ? O4 Ni2 N7 89.8(2) . . ? N8 Ni2 N7 78.6(3) . . ? N9 Ni2 N7 96.0(3) . . ? N10 Ni2 N7 172.9(2) . . ? F3 B1 F2 119.4(14) . . ? F3 B1 F4 113.0(17) . . ? F2 B1 F4 107.9(14) . . ? F3 B1 F1 103.4(15) . . ? F2 B1 F1 106.4(15) . . ? F4 B1 F1 105.5(14) . . ? F7 B2 F5 121(4) . . ? F7 B2 F8 112(2) . . ? F5 B2 F8 113(2) . . ? F7 B2 F6 105(3) . . ? F5 B2 F6 103(3) . . ? F8 B2 F6 101(4) . . ? N1 C1 C2 122.7(10) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C3 C2 C1 118.7(10) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 120.1(10) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 119.5(10) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.3 . . ? C4 C5 N1 121.2(9) . . ? C4 C5 C6 124.4(9) . . ? N1 C5 C6 114.5(7) . . ? N2 C6 C7 110.3(8) . . ? N2 C6 C5 117.8(8) . . ? C7 C6 C5 131.8(9) . . ? C8 C7 C6 105.8(9) . . ? C8 C7 H7A 127.1 . . ? C6 C7 H7A 127.1 . . ? C7 C8 N3 108.6(10) . . ? C7 C8 H8A 125.7 . . ? N3 C8 H8A 125.7 . . ? N3 C9 C10 113.2(7) . . ? N3 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N3 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? N4 C10 C17 122.5(8) . . ? N4 C10 C9 117.4(8) . . ? C17 C10 C9 120.0(7) . . ? N4 C11 C16 120.6(8) . . ? N4 C11 C12 120.2(10) . . ? C16 C11 C12 119.2(10) . . ? C13 C12 C11 119.3(11) . . ? C13 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? C14 C13 C12 121.6(11) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C15 119.5(12) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C16 C15 C14 121.8(12) . . ? C16 C15 H15A 119.1 . . ? C14 C15 H15A 119.1 . . ? C15 C16 N5 120.1(9) . . ? C15 C16 C11 118.4(9) . . ? N5 C16 C11 121.5(8) . . ? N5 C17 C10 121.3(8) . . ? N5 C17 C18 118.5(8) . . ? C10 C17 C18 120.2(7) . . ? N6 C18 C17 114.8(7) . . ? N6 C18 H18A 108.6 . . ? C17 C18 H18A 108.6 . . ? N6 C18 H18B 108.6 . . ? C17 C18 H18B 108.6 . . ? H18A C18 H18B 107.5 . . ? N6 C19 C20 107.5(8) . . ? N6 C19 H19A 126.3 . . ? C20 C19 H19A 126.3 . . ? C19 C20 C21 105.5(8) . . ? C19 C20 H20A 127.2 . . ? C21 C20 H20A 127.2 . . ? N7 C21 C20 109.8(8) . . ? N7 C21 C22 118.1(8) . . ? C20 C21 C22 132.1(8) . . ? N8 C22 C23 122.8(9) . . ? N8 C22 C21 114.2(7) . . ? C23 C22 C21 122.9(9) . . ? C22 C23 C24 118.0(11) . . ? C22 C23 H23A 121.0 . . ? C24 C23 H23A 121.0 . . ? C25 C24 C23 119.1(10) . . ? C25 C24 H24A 120.5 . . ? C23 C24 H24A 120.5 . . ? C24 C25 C26 119.4(10) . . ? C24 C25 H25A 120.3 . . ? C26 C25 H25A 120.3 . . ? N8 C26 C25 122.5(10) . . ? N8 C26 H26A 118.8 . . ? C25 C26 H26A 118.8 . . ? N9 C27 C28 123.3(10) . . ? N9 C27 H27A 118.3 . . ? C28 C27 H27A 118.3 . . ? C27 C28 C29 117.7(10) . . ? C27 C28 H28A 121.2 . . ? C29 C28 H28A 121.2 . . ? C28 C29 C30 120.2(9) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C31 C30 C29 119.7(10) . . ? C31 C30 H30A 120.2 . . ? C29 C30 H30A 120.1 . . ? C30 C31 N9 120.7(9) . . ? C30 C31 C32 123.7(10) . . ? N9 C31 C32 115.7(8) . . ? N10 C32 C33 112.2(9) . . ? N10 C32 C31 117.3(9) . . ? C33 C32 C31 130.5(9) . . ? C32 C33 C34 104.7(9) . . ? C32 C33 H33A 127.7 . . ? C34 C33 H33A 127.7 . . ? N11 C34 C33 106.5(10) . . ? N11 C34 H34A 126.8 . . ? C33 C34 H34A 126.8 . . ? N11 C35 C36 113.6(8) . . ? N11 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? N11 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N12 C36 C43 122.1(9) . . ? N12 C36 C35 118.8(8) . . ? C43 C36 C35 119.2(9) . . ? C42 C37 N12 122.6(9) . . ? C42 C37 C38 120.1(11) . . ? N12 C37 C38 117.4(11) . . ? C39 C38 C37 118.9(14) . . ? C39 C38 H38A 120.6 . . ? C37 C38 H38A 120.6 . . ? C38 C39 C40 119.4(14) . . ? C38 C39 H39A 120.3 . . ? C40 C39 H39A 120.3 . . ? C41 C40 C39 122.0(16) . . ? C41 C40 H40A 119.0 . . ? C39 C40 H40A 119.0 . . ? C40 C41 C42 120.9(16) . . ? C40 C41 H41A 119.5 . . ? C42 C41 H41A 119.5 . . ? C37 C42 N13 121.5(10) . . ? C37 C42 C41 118.7(12) . . ? N13 C42 C41 119.8(13) . . ? N13 C43 C36 122.5(9) . . ? N13 C43 C44 116.4(9) . 2_566 ? C36 C43 C44 121.1(9) . 2_566 ? N14 C44 C43 115.2(9) . 2_566 ? N14 C44 H44A 108.5 . . ? C43 C44 H44A 108.5 2_566 . ? N14 C44 H44B 108.5 . . ? C43 C44 H44B 108.5 2_566 . ? H44A C44 H44B 107.5 . . ? N14 C45 C46 108.5(12) . . ? N14 C45 H45A 125.7 . . ? C46 C45 H45A 125.7 . . ? C45 C46 C47 105.1(12) . . ? C45 C46 H46A 127.5 . . ? C47 C46 H46A 127.5 . . ? N15 C47 C46 110.5(11) . . ? N15 C47 C48 117.9(10) . . ? C46 C47 C48 131.4(10) . . ? N16 C48 C49 123.0(11) . . ? N16 C48 C47 115.8(8) . . ? C49 C48 C47 121.2(11) . . ? C50 C49 C48 117.6(12) . . ? C50 C49 H49A 121.2 . . ? C48 C49 H49A 121.2 . . ? C49 C50 C51 120.0(10) . . ? C49 C50 H50A 120.0 . . ? C51 C50 H50A 120.0 . . ? C52 C51 C50 118.9(12) . . ? C52 C51 H51A 120.6 . . ? C50 C51 H51A 120.6 . . ? N16 C52 C51 121.8(11) . . ? N16 C52 H52A 119.1 . . ? C51 C52 H52A 119.1 . . ? C1 N1 C5 117.8(8) . . ? C1 N1 Ni1 127.1(7) . . ? C5 N1 Ni1 115.1(6) . . ? N3 N2 C6 104.8(7) . . ? N3 N2 Ni1 142.0(5) . . ? C6 N2 Ni1 113.0(6) . . ? N2 N3 C8 110.4(7) . . ? N2 N3 C9 121.1(7) . . ? C8 N3 C9 128.4(8) . . ? C10 N4 C11 117.1(8) . . ? C17 N5 C16 116.9(8) . . ? N7 N6 C19 111.4(7) . . ? N7 N6 C18 123.1(7) . . ? C19 N6 C18 125.4(8) . . ? N6 N7 C21 105.8(7) . . ? N6 N7 Ni2 141.0(5) . . ? C21 N7 Ni2 113.2(6) . . ? C26 N8 C22 117.9(7) . . ? C26 N8 Ni2 126.4(7) . . ? C22 N8 Ni2 115.2(5) . . ? C27 N9 C31 118.3(8) . . ? C27 N9 Ni2 127.0(6) . . ? C31 N9 Ni2 114.4(6) . . ? N11 N10 C32 104.7(7) . . ? N11 N10 Ni2 140.5(6) . . ? C32 N10 Ni2 114.2(6) . . ? N10 N11 C34 111.9(8) . . ? N10 N11 C35 120.9(8) . . ? C34 N11 C35 127.1(9) . . ? C36 N12 C37 115.2(9) . . ? C43 N13 C42 116.1(9) . . ? C45 N14 N15 109.3(10) . . ? C45 N14 C44 128.3(10) . . ? N15 N14 C44 122.4(9) . . ? C47 N15 N14 106.4(9) . . ? C47 N15 Ni1 113.8(7) . . ? N14 N15 Ni1 139.8(6) . . ? C48 N16 C52 118.5(8) . . ? C48 N16 Ni1 114.7(6) . . ? C52 N16 Ni1 126.6(7) . . ? O8 S1 O7' 65.0(15) . . ? O8 S1 O6 102.9(15) . . ? O7' S1 O6 89.5(11) . . ? O8 S1 O7 113.2(16) . . ? O7' S1 O7 57.5(12) . . ? O6 S1 O7 107.4(10) . . ? O8 S1 O8' 70.0(15) . . ? O7' S1 O8' 133.7(16) . . ? O6 S1 O8' 90.2(11) . . ? O7 S1 O8' 160.2(12) . . ? O8 S1 O5 142.4(16) . . ? O7' S1 O5 152.3(15) . . ? O6 S1 O5 87.1(9) . . ? O7 S1 O5 97.5(13) . . ? O8' S1 O5 73.8(13) . . ? O8 S1 O6' 92.1(16) . . ? O7' S1 O6' 109.7(12) . . ? O6 S1 O6' 159.6(9) . . ? O7 S1 O6' 78.5(10) . . ? O8' S1 O6' 81.8(12) . . ? O5 S1 O6' 72.6(10) . . ? O8 S1 O5' 163.3(17) . . ? O7' S1 O5' 99.6(16) . . ? O6 S1 O5' 82.7(11) . . ? O7 S1 O5' 50.3(11) . . ? O8' S1 O5' 126.2(15) . . ? O5 S1 O5' 52.6(12) . . ? O6' S1 O5' 86.9(12) . . ? 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 N1 C1 C2 C3 0.0(15) . . . . ? C1 C2 C3 C4 0.9(17) . . . . ? C2 C3 C4 C5 -0.3(17) . . . . ? C3 C4 C5 N1 -1.3(14) . . . . ? C3 C4 C5 C6 178.4(9) . . . . ? C4 C5 C6 N2 -177.5(8) . . . . ? N1 C5 C6 N2 2.3(12) . . . . ? C4 C5 C6 C7 -1.2(17) . . . . ? N1 C5 C6 C7 178.6(10) . . . . ? N2 C6 C7 C8 -0.1(12) . . . . ? C5 C6 C7 C8 -176.6(10) . . . . ? C6 C7 C8 N3 0.7(13) . . . . ? N3 C9 C10 N4 -11.6(12) . . . . ? N3 C9 C10 C17 171.5(8) . . . . ? N4 C11 C12 C13 179.2(10) . . . . ? C16 C11 C12 C13 0.3(16) . . . . ? C11 C12 C13 C14 -3(2) . . . . ? C12 C13 C14 C15 5(2) . . . . ? C13 C14 C15 C16 -3.7(19) . . . . ? C14 C15 C16 N5 179.8(10) . . . . ? C14 C15 C16 C11 0.8(16) . . . . ? N4 C11 C16 C15 -178.0(9) . . . . ? C12 C11 C16 C15 0.9(14) . . . . ? N4 C11 C16 N5 3.0(14) . . . . ? C12 C11 C16 N5 -178.1(9) . . . . ? N4 C10 C17 N5 4.5(13) . . . . ? C9 C10 C17 N5 -178.8(8) . . . . ? N4 C10 C17 C18 -177.1(8) . . . . ? C9 C10 C17 C18 -0.4(12) . . . . ? N5 C17 C18 N6 -20.4(11) . . . . ? C10 C17 C18 N6 161.2(7) . . . . ? N6 C19 C20 C21 0.8(9) . . . . ? C19 C20 C21 N7 -1.0(10) . . . . ? C19 C20 C21 C22 179.1(9) . . . . ? N7 C21 C22 N8 3.7(11) . . . . ? C20 C21 C22 N8 -176.4(8) . . . . ? N7 C21 C22 C23 -178.4(8) . . . . ? C20 C21 C22 C23 1.5(15) . . . . ? N8 C22 C23 C24 -3.4(15) . . . . ? C21 C22 C23 C24 178.9(9) . . . . ? C22 C23 C24 C25 5.1(18) . . . . ? C23 C24 C25 C26 -5.0(19) . . . . ? C24 C25 C26 N8 3.1(18) . . . . ? N9 C27 C28 C29 -3.0(16) . . . . ? C27 C28 C29 C30 2.2(17) . . . . ? C28 C29 C30 C31 0.9(18) . . . . ? C29 C30 C31 N9 -3.4(16) . . . . ? C29 C30 C31 C32 177.1(10) . . . . ? C30 C31 C32 N10 -175.6(9) . . . . ? N9 C31 C32 N10 4.9(12) . . . . ? C30 C31 C32 C33 5.3(18) . . . . ? N9 C31 C32 C33 -174.2(11) . . . . ? N10 C32 C33 C34 -0.6(13) . . . . ? C31 C32 C33 C34 178.6(10) . . . . ? C32 C33 C34 N11 -0.8(14) . . . . ? N11 C35 C36 N12 11.4(12) . . . . ? N11 C35 C36 C43 -169.3(8) . . . . ? C42 C37 C38 C39 -0.8(17) . . . . ? N12 C37 C38 C39 179.0(10) . . . . ? C37 C38 C39 C40 2(2) . . . . ? C38 C39 C40 C41 -2(2) . . . . ? C39 C40 C41 C42 0(2) . . . . ? N12 C37 C42 N13 -1.6(16) . . . . ? C38 C37 C42 N13 178.1(10) . . . . ? N12 C37 C42 C41 179.4(10) . . . . ? C38 C37 C42 C41 -0.8(16) . . . . ? C40 C41 C42 C37 1.0(19) . . . . ? C40 C41 C42 N13 -178.0(13) . . . . ? N12 C36 C43 N13 -2.6(14) . . . . ? C35 C36 C43 N13 178.2(9) . . . . ? N12 C36 C43 C44 178.6(9) . . . 2_566 ? C35 C36 C43 C44 -0.6(13) . . . 2_566 ? N14 C45 C46 C47 -1.8(19) . . . . ? C45 C46 C47 N15 1.7(17) . . . . ? C45 C46 C47 C48 -173.5(12) . . . . ? N15 C47 C48 N16 -1.2(14) . . . . ? C46 C47 C48 N16 173.7(14) . . . . ? N15 C47 C48 C49 -178.9(10) . . . . ? C46 C47 C48 C49 -4(2) . . . . ? N16 C48 C49 C50 -0.5(17) . . . . ? C47 C48 C49 C50 177.1(10) . . . . ? C48 C49 C50 C51 2.3(18) . . . . ? C49 C50 C51 C52 -1.9(19) . . . . ? C50 C51 C52 N16 -0.4(16) . . . . ? C2 C1 N1 C5 -1.5(13) . . . . ? C2 C1 N1 Ni1 176.1(7) . . . . ? C4 C5 N1 C1 2.2(13) . . . . ? C6 C5 N1 C1 -177.6(7) . . . . ? C4 C5 N1 Ni1 -175.7(7) . . . . ? C6 C5 N1 Ni1 4.5(9) . . . . ? O2 Ni1 N1 C1 -168(2) . . . . ? O1 Ni1 N1 C1 85.5(7) . . . . ? N16 Ni1 N1 C1 -87.7(7) . . . . ? N15 Ni1 N1 C1 -10.5(7) . . . . ? N2 Ni1 N1 C1 175.7(7) . . . . ? O2 Ni1 N1 C5 9(3) . . . . ? O1 Ni1 N1 C5 -96.8(6) . . . . ? N16 Ni1 N1 C5 90.0(6) . . . . ? N15 Ni1 N1 C5 167.2(6) . . . . ? N2 Ni1 N1 C5 -6.5(6) . . . . ? C7 C6 N2 N3 -0.6(10) . . . . ? C5 C6 N2 N3 176.5(7) . . . . ? C7 C6 N2 Ni1 175.2(7) . . . . ? C5 C6 N2 Ni1 -7.7(9) . . . . ? O2 Ni1 N2 N3 2.8(8) . . . . ? O1 Ni1 N2 N3 -88.0(8) . . . . ? N1 Ni1 N2 N3 -179.0(9) . . . . ? N16 Ni1 N2 N3 93.9(8) . . . . ? N15 Ni1 N2 N3 122.4(19) . . . . ? O2 Ni1 N2 C6 -170.6(5) . . . . ? O1 Ni1 N2 C6 98.6(6) . . . . ? N1 Ni1 N2 C6 7.6(5) . . . . ? N16 Ni1 N2 C6 -79.5(6) . . . . ? N15 Ni1 N2 C6 -51(2) . . . . ? C6 N2 N3 C8 1.0(9) . . . . ? Ni1 N2 N3 C8 -172.7(7) . . . . ? C6 N2 N3 C9 178.2(7) . . . . ? Ni1 N2 N3 C9 4.5(13) . . . . ? C7 C8 N3 N2 -1.1(12) . . . . ? C7 C8 N3 C9 -178.0(9) . . . . ? C10 C9 N3 N2 -88.2(10) . . . . ? C10 C9 N3 C8 88.5(12) . . . . ? C17 C10 N4 C11 -2.6(13) . . . . ? C9 C10 N4 C11 -179.4(8) . . . . ? C16 C11 N4 C10 -1.0(13) . . . . ? C12 C11 N4 C10 -179.9(9) . . . . ? C10 C17 N5 C16 -2.3(12) . . . . ? C18 C17 N5 C16 179.2(8) . . . . ? C15 C16 N5 C17 179.9(9) . . . . ? C11 C16 N5 C17 -1.1(13) . . . . ? C20 C19 N6 N7 -0.3(9) . . . . ? C20 C19 N6 C18 -177.7(7) . . . . ? C17 C18 N6 N7 99.7(9) . . . . ? C17 C18 N6 C19 -83.2(10) . . . . ? C19 N6 N7 C21 -0.3(8) . . . . ? C18 N6 N7 C21 177.1(7) . . . . ? C19 N6 N7 Ni2 177.8(6) . . . . ? C18 N6 N7 Ni2 -4.7(12) . . . . ? C20 C21 N7 N6 0.8(9) . . . . ? C22 C21 N7 N6 -179.3(6) . . . . ? C20 C21 N7 Ni2 -177.9(5) . . . . ? C22 C21 N7 Ni2 2.0(9) . . . . ? O3 Ni2 N7 N6 -2.1(8) . . . . ? O4 Ni2 N7 N6 85.6(8) . . . . ? N8 Ni2 N7 N6 177.4(8) . . . . ? N9 Ni2 N7 N6 -95.4(8) . . . . ? N10 Ni2 N7 N6 -130.1(19) . . . . ? O3 Ni2 N7 C21 175.9(5) . . . . ? O4 Ni2 N7 C21 -96.4(5) . . . . ? N8 Ni2 N7 C21 -4.6(5) . . . . ? N9 Ni2 N7 C21 82.6(5) . . . . ? N10 Ni2 N7 C21 48(2) . . . . ? C25 C26 N8 C22 -1.2(14) . . . . ? C25 C26 N8 Ni2 -173.4(8) . . . . ? C23 C22 N8 C26 1.4(13) . . . . ? C21 C22 N8 C26 179.4(7) . . . . ? C23 C22 N8 Ni2 174.5(7) . . . . ? C21 C22 N8 Ni2 -7.6(9) . . . . ? O3 Ni2 N8 C26 -175(3) . . . . ? O4 Ni2 N8 C26 -91.5(7) . . . . ? N9 Ni2 N8 C26 82.7(7) . . . . ? N10 Ni2 N8 C26 4.7(8) . . . . ? N7 Ni2 N8 C26 179.1(8) . . . . ? O3 Ni2 N8 C22 12(3) . . . . ? O4 Ni2 N8 C22 96.1(6) . . . . ? N9 Ni2 N8 C22 -89.7(6) . . . . ? N10 Ni2 N8 C22 -167.6(6) . . . . ? N7 Ni2 N8 C22 6.7(6) . . . . ? C28 C27 N9 C31 0.5(14) . . . . ? C28 C27 N9 Ni2 -173.9(8) . . . . ? C30 C31 N9 C27 2.7(13) . . . . ? C32 C31 N9 C27 -177.8(8) . . . . ? C30 C31 N9 Ni2 177.9(8) . . . . ? C32 C31 N9 Ni2 -2.6(10) . . . . ? O3 Ni2 N9 C27 -98.1(7) . . . . ? O4 Ni2 N9 C27 169(2) . . . . ? N8 Ni2 N9 C27 77.3(7) . . . . ? N10 Ni2 N9 C27 174.8(7) . . . . ? N7 Ni2 N9 C27 -1.1(7) . . . . ? O3 Ni2 N9 C31 87.3(6) . . . . ? O4 Ni2 N9 C31 -6(3) . . . . ? N8 Ni2 N9 C31 -97.4(6) . . . . ? N10 Ni2 N9 C31 0.1(6) . . . . ? N7 Ni2 N9 C31 -175.7(6) . . . . ? C33 C32 N10 N11 1.7(11) . . . . ? C31 C32 N10 N11 -177.5(8) . . . . ? C33 C32 N10 Ni2 174.6(8) . . . . ? C31 C32 N10 Ni2 -4.7(10) . . . . ? O3 Ni2 N10 N11 78.4(9) . . . . ? O4 Ni2 N10 N11 -9.1(9) . . . . ? N8 Ni2 N10 N11 -101.6(9) . . . . ? N9 Ni2 N10 N11 171.5(9) . . . . ? N7 Ni2 N10 N11 -153.2(17) . . . . ? O3 Ni2 N10 C32 -90.7(6) . . . . ? O4 Ni2 N10 C32 -178.2(6) . . . . ? N8 Ni2 N10 C32 89.3(6) . . . . ? N9 Ni2 N10 C32 2.4(6) . . . . ? N7 Ni2 N10 C32 38(2) . . . . ? C32 N10 N11 C34 -2.3(11) . . . . ? Ni2 N10 N11 C34 -172.0(8) . . . . ? C32 N10 N11 C35 178.1(8) . . . . ? Ni2 N10 N11 C35 8.4(13) . . . . ? C33 C34 N11 N10 2.0(13) . . . . ? C33 C34 N11 C35 -178.4(9) . . . . ? C36 C35 N11 N10 81.9(10) . . . . ? C36 C35 N11 C34 -97.6(12) . . . . ? C43 C36 N12 C37 2.1(13) . . . . ? C35 C36 N12 C37 -178.7(8) . . . . ? C42 C37 N12 C36 -0.1(14) . . . . ? C38 C37 N12 C36 -179.9(9) . . . . ? C36 C43 N13 C42 0.8(14) . . . . ? C44 C43 N13 C42 179.6(9) 2_566 . . . ? C37 C42 N13 C43 1.2(15) . . . . ? C41 C42 N13 C43 -179.8(10) . . . . ? C46 C45 N14 N15 1.4(17) . . . . ? C46 C45 N14 C44 -177.4(12) . . . . ? C43 C44 N14 C45 94.4(15) 2_566 . . . ? C43 C44 N14 N15 -84.2(12) 2_566 . . . ? C46 C47 N15 N14 -0.8(13) . . . . ? C48 C47 N15 N14 175.1(8) . . . . ? C46 C47 N15 Ni1 -179.3(10) . . . . ? C48 C47 N15 Ni1 -3.4(11) . . . . ? C45 N14 N15 C47 -0.3(12) . . . . ? C44 N14 N15 C47 178.5(9) . . . . ? C45 N14 N15 Ni1 177.4(9) . . . . ? C44 N14 N15 Ni1 -3.7(14) . . . . ? O2 Ni1 N15 C47 95.4(7) . . . . ? O1 Ni1 N15 C47 -174.0(6) . . . . ? N1 Ni1 N15 C47 -82.1(7) . . . . ? N16 Ni1 N15 C47 4.6(6) . . . . ? N2 Ni1 N15 C47 -25(2) . . . . ? O2 Ni1 N15 N14 -82.2(9) . . . . ? O1 Ni1 N15 N14 8.3(9) . . . . ? N1 Ni1 N15 N14 100.2(9) . . . . ? N16 Ni1 N15 N14 -173.1(9) . . . . ? N2 Ni1 N15 N14 157.8(17) . . . . ? C49 C48 N16 C52 -1.8(14) . . . . ? C47 C48 N16 C52 -179.5(8) . . . . ? C49 C48 N16 Ni1 -177.1(8) . . . . ? C47 C48 N16 Ni1 5.2(11) . . . . ? C51 C52 N16 C48 2.2(14) . . . . ? C51 C52 N16 Ni1 176.9(8) . . . . ? O2 Ni1 N16 C48 -93.9(6) . . . . ? O1 Ni1 N16 C48 7(2) . . . . ? N1 Ni1 N16 C48 92.5(6) . . . . ? N15 Ni1 N16 C48 -5.2(6) . . . . ? N2 Ni1 N16 C48 171.2(6) . . . . ? O2 Ni1 N16 C52 91.2(7) . . . . ? O1 Ni1 N16 C52 -167.8(18) . . . . ? N1 Ni1 N16 C52 -82.4(7) . . . . ? N15 Ni1 N16 C52 179.9(7) . . . . ? N2 Ni1 N16 C52 -3.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.51 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.936 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.109 #===END data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H102 Cu6 N18 O18, 10(Cl O4-),2(OH-), 2(CH3CN),9(H2 O)' _chemical_formula_sum 'C76 H128 Cl10 Cu6 N20 O69' _chemical_formula_structural '6(Cu 2+), 2(C36 H33 N9), 10(Cl O4 -),2(OH-),2(CH3CN), 27(H2 O)' _chemical_formula_sum 'C76 H128 Cl10 Cu6 N20 O69' _chemical_formula_weight 3165.76 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 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 32.067(12) _cell_length_b 25.610(9) _cell_length_c 17.498(7) _cell_angle_alpha 90.00 _cell_angle_beta 115.187(6) _cell_angle_gamma 90.00 _cell_volume 13003(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1050 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 22.98 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6500 _exptl_absorpt_coefficient_mu 1.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.877998 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'sadabs; bruker, 1996' _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 'bruker ccd area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24255 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.1298 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.42 _reflns_number_total 12705 _reflns_number_gt 5130 _reflns_threshold_expression I>2si\(I) _computing_data_collection 'SMART, BRUKER 1998' _computing_cell_refinement 'SMART' _computing_data_reduction SAINT, BRUKER 1998' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997A)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997A)' _computing_molecular_graphics 'SHELXTL, SHELDRICK, 1997B' _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^)+(0.1354P)^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 12705 _refine_ls_number_parameters 844 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2143 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.2788 _refine_ls_wR_factor_gt 0.2107 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.009 _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 0.11722(4) 0.65464(5) 0.40850(8) 0.0794(5) Uani 1 1 d . . . Cu2 Cu 0.14353(4) 0.60344(4) 0.98521(7) 0.0554(3) Uani 1 1 d . . . Cu3 Cu 0.08114(4) 1.03704(4) 0.65649(7) 0.0579(4) Uani 1 1 d . . . C1 C 0.1215(3) 0.7586(3) 0.7958(5) 0.050(2) Uani 1 1 d . . . C2 C 0.1184(3) 0.8138(3) 0.7972(6) 0.052(2) Uani 1 1 d . . . C3 C 0.1078(3) 0.8413(3) 0.7233(6) 0.050(2) Uani 1 1 d . . . C4 C 0.1053(3) 0.8172(3) 0.6503(6) 0.050(2) Uani 1 1 d . . . C5 C 0.1092(3) 0.7624(3) 0.6490(5) 0.055(2) Uani 1 1 d . . . C6 C 0.1199(4) 0.6738(3) 0.7184(7) 0.077(3) Uani 1 1 d . . . H6A H 0.1156 0.6630 0.6630 0.115 Uiso 1 1 calc R . . H6B H 0.0966 0.6582 0.7317 0.115 Uiso 1 1 calc R . . H6C H 0.1498 0.6629 0.7590 0.115 Uiso 1 1 calc R . . C7 C 0.1277(4) 0.8417(4) 0.8794(6) 0.075(3) Uani 1 1 d . . . H7A H 0.1241 0.8787 0.8695 0.112 Uiso 1 1 calc R . . H7B H 0.1586 0.8344 0.9199 0.112 Uiso 1 1 calc R . . H7C H 0.1063 0.8297 0.9007 0.112 Uiso 1 1 calc R . . C8 C 0.0987(4) 0.8486(4) 0.5743(6) 0.080(3) Uani 1 1 d . . . H8A H 0.0986 0.8258 0.5307 0.119 Uiso 1 1 calc R . . H8B H 0.1234 0.8733 0.5887 0.119 Uiso 1 1 calc R . . H8C H 0.0699 0.8669 0.5545 0.119 Uiso 1 1 calc R . . C9 C 0.1049(3) 0.7351(4) 0.5697(6) 0.061(2) Uani 1 1 d . . . H9A H 0.0882 0.7026 0.5634 0.074 Uiso 1 1 calc R . . H9B H 0.0875 0.7569 0.5211 0.074 Uiso 1 1 calc R . . C10 C 0.1287(3) 0.7260(3) 0.8729(6) 0.063(2) Uani 1 1 d . . . H10A H 0.1271 0.7485 0.9162 0.075 Uiso 1 1 calc R . . H10B H 0.1041 0.7005 0.8577 0.075 Uiso 1 1 calc R . . C11 C 0.0967(3) 0.8993(3) 0.7193(6) 0.063(3) Uani 1 1 d . . . H11A H 0.0711 0.9071 0.6655 0.075 Uiso 1 1 calc R . . H11B H 0.0874 0.9079 0.7637 0.075 Uiso 1 1 calc R . . C12 C 0.1914(3) 0.7426(4) 0.6251(6) 0.064(3) Uani 1 1 d . . . H12A H 0.1966 0.7648 0.6704 0.076 Uiso 1 1 calc R . . C13 C 0.2239(3) 0.7244(4) 0.6029(6) 0.067(3) Uani 1 1 d . . . H13A H 0.2554 0.7311 0.6287 0.080 Uiso 1 1 calc R . . C14 C 0.2001(3) 0.6936(3) 0.5331(6) 0.055(2) Uani 1 1 d . . . C15 C 0.2145(3) 0.6625(4) 0.4780(6) 0.062(2) Uani 1 1 d . . . C16 C 0.2595(4) 0.6567(4) 0.4893(8) 0.081(3) Uani 1 1 d . . . H16A H 0.2832 0.6731 0.5343 0.097 Uiso 1 1 calc R . . C17 C 0.2693(5) 0.6266(5) 0.4335(10) 0.097(4) Uani 1 1 d . . . H17A H 0.2994 0.6218 0.4398 0.117 Uiso 1 1 calc R . . C18 C 0.2317(6) 0.6037(5) 0.3670(9) 0.101(4) Uani 1 1 d . . . H18A H 0.2366 0.5837 0.3272 0.121 Uiso 1 1 calc R . . C19 C 0.1887(5) 0.6102(4) 0.3597(8) 0.089(3) Uani 1 1 d . . . H19A H 0.1646 0.5931 0.3164 0.107 Uiso 1 1 calc R . . C20 C 0.2112(3) 0.7143(3) 0.9054(5) 0.056(2) Uani 1 1 d . . . H20A H 0.2164 0.7464 0.8861 0.068 Uiso 1 1 calc R . . C21 C 0.2433(3) 0.6751(3) 0.9376(6) 0.057(2) Uani 1 1 d . . . H21A H 0.2738 0.6749 0.9447 0.068 Uiso 1 1 calc R . . C22 C 0.2190(3) 0.6353(3) 0.9573(5) 0.0432(19) Uani 1 1 d . . . C23 C 0.2309(3) 0.5819(3) 0.9897(5) 0.050(2) Uani 1 1 d . . . C24 C 0.2722(3) 0.5564(4) 1.0022(6) 0.067(3) Uani 1 1 d . . . H24A H 0.2953 0.5736 0.9931 0.080 Uiso 1 1 calc R . . C25 C 0.2773(4) 0.5046(4) 1.0284(7) 0.078(3) Uani 1 1 d . . . H25A H 0.3037 0.4861 1.0359 0.094 Uiso 1 1 calc R . . C26 C 0.2438(4) 0.4816(4) 1.0428(7) 0.081(3) Uani 1 1 d . . . H26A H 0.2474 0.4472 1.0614 0.097 Uiso 1 1 calc R . . C27 C 0.2030(3) 0.5088(4) 1.0301(6) 0.068(3) Uani 1 1 d . . . H27A H 0.1799 0.4923 1.0399 0.081 Uiso 1 1 calc R . . C28 C 0.1812(3) 0.9181(4) 0.7605(6) 0.065(3) Uani 1 1 d . . . H28A H 0.1934 0.8852 0.7793 0.078 Uiso 1 1 calc R . . C29 C 0.2049(3) 0.9620(4) 0.7597(6) 0.067(3) Uani 1 1 d . . . H29A H 0.2365 0.9647 0.7769 0.080 Uiso 1 1 calc R . . C30 C 0.1731(3) 1.0015(3) 0.7288(5) 0.054(2) Uani 1 1 d . . . C31 C 0.1760(4) 1.0566(4) 0.7125(6) 0.063(3) Uani 1 1 d . . . C32 C 0.2179(4) 1.0806(5) 0.7330(7) 0.094(4) Uani 1 1 d . . . H32A H 0.2458 1.0631 0.7592 0.113 Uiso 1 1 calc R . . C33 C 0.2151(6) 1.1350(6) 0.7107(9) 0.110(5) Uani 1 1 d . . . H33A H 0.2421 1.1538 0.7236 0.132 Uiso 1 1 calc R . . C34 C 0.1761(6) 1.1582(5) 0.6734(10) 0.099(4) Uani 1 1 d . . . H34A H 0.1752 1.1932 0.6584 0.119 Uiso 1 1 calc R . . C35 C 0.1356(4) 1.1316(4) 0.6553(7) 0.082(3) Uani 1 1 d . . . H35A H 0.1076 1.1491 0.6295 0.099 Uiso 1 1 calc R . . C36 C 0.1163(3) 0.7330(3) 0.7207(5) 0.053(2) Uani 1 1 d . . . C37 C 0.0298(9) 0.5562(12) 0.026(3) 0.36(3) Uani 1 1 d . . . H37A H 0.0572 0.5675 0.0212 0.546 Uiso 1 1 calc R . . H37B H 0.0183 0.5250 -0.0068 0.546 Uiso 1 1 calc R . . H37C H 0.0368 0.5493 0.0839 0.546 Uiso 1 1 calc R . . C38 C 0.0014(6) 0.5893(10) 0.000(2) 0.247(16) Uani 1 1 d . . . N1 N 0.1365(2) 0.9319(2) 0.7288(5) 0.0568(19) Uani 1 1 d . . . N2 N 0.1312(2) 0.9835(2) 0.7110(4) 0.0522(18) Uani 1 1 d . . . N3 N 0.1360(3) 1.0808(3) 0.6744(5) 0.062(2) Uani 1 1 d . . . N4 N 0.1721(2) 0.6996(3) 0.9060(4) 0.0494(17) Uani 1 1 d . . . N5 N 0.1761(2) 0.6504(2) 0.9381(4) 0.0475(17) Uani 1 1 d . . . N6 N 0.1979(2) 0.5586(3) 1.0038(4) 0.0494(17) Uani 1 1 d . . . N7 N 0.1507(2) 0.7241(3) 0.5724(4) 0.0521(18) Uani 1 1 d . . . N8 N 0.1551(2) 0.6932(3) 0.5143(4) 0.0530(18) Uani 1 1 d . . . N9 N 0.1793(3) 0.6406(3) 0.4128(5) 0.071(2) Uani 1 1 d . . . N10 N -0.0290(12) 0.6043(17) -0.0187(19) 0.41(2) Uani 1 1 d . . . O1 O 0.1157(5) 0.4694(6) 0.2039(13) 0.256(9) Uani 1 1 d . . . O3 O 0.1813(5) 0.4482(6) 0.2966(8) 0.213(6) Uani 1 1 d . . . O2 O 0.1764(4) 0.5157(4) 0.2093(6) 0.147(4) Uani 1 1 d . . . O4 O 0.1650(5) 0.4330(5) 0.1612(9) 0.185(5) Uani 1 1 d . . . O5 O 0.2023(3) 0.7059(3) 0.2275(5) 0.100(2) Uani 1 1 d . . . O8 O 0.2619(2) 0.6901(3) 0.1924(5) 0.102(3) Uani 1 1 d . . . O7 O 0.1930(3) 0.7226(2) 0.0909(4) 0.088(2) Uani 1 1 d . . . O6 O 0.1975(3) 0.6368(2) 0.1399(5) 0.092(2) Uani 1 1 d . . . O10 O 0.1553(4) 0.7644(5) 0.3434(8) 0.182(5) Uani 1 1 d . A . O9 O 0.0922(7) 0.7528(12) 0.3453(15) 0.42(2) Uani 1 1 d . A . O12' O 0.1177(9) 0.8116(10) 0.4065(11) 0.143(9) Uani 0.50 1 d P A 1 O12 O 0.1384(8) 0.8401(8) 0.3529(17) 0.174(11) Uani 0.50 1 d P A 2 O11 O 0.0866(4) 0.8067(5) 0.2533(7) 0.171(5) Uani 1 1 d . A . O13 O 0.0030(4) 0.2317(6) 0.4953(10) 0.208(6) Uani 1 1 d . . . O14 O 0.0167(5) 0.2296(4) 0.3787(8) 0.187(5) Uani 1 1 d . . . O15 O 0.0230(4) 0.1535(4) 0.4495(7) 0.155(4) Uani 1 1 d . . . O16 O 0.0769(3) 0.2234(5) 0.5075(7) 0.159(4) Uani 1 1 d . . . O19 O 0.1406(5) 0.0120(16) 0.5337(12) 0.41(2) Uani 1 1 d . B 1 O20' O 0.114(2) 0.0452(13) 0.470(5) 0.41(5) Uani 0.50 1 d P B 1 O17 O 0.0651(3) 0.0066(4) 0.5025(5) 0.126(3) Uani 1 1 d . B 2 O18 O 0.1131(11) -0.0442(6) 0.4723(18) 0.39(2) Uani 1 1 d . B 2 O20 O 0.0883(10) 0.0176(7) 0.3898(11) 0.124(8) Uani 0.50 1 d P B 2 O1W O 0.0559(2) 0.6696(4) 0.4043(6) 0.120(3) Uani 1 1 d . . . O2W O 0.1128(3) 0.5766(3) 0.4692(8) 0.160(4) Uani 1 1 d . . . O3W O 0.0868(3) 0.6300(4) 0.2905(6) 0.161(4) Uani 1 1 d . . . O4W O 0.0974(2) 0.6549(3) 0.9844(5) 0.086(2) Uani 1 1 d . . . O5W O 0.1219(2) 0.5549(3) 1.0484(5) 0.088(2) Uani 1 1 d . . . O6W O 0.0948(3) 0.5710(4) 0.8566(6) 0.136(3) Uani 1 1 d . . . O7W O 0.0351(2) 1.0902(2) 0.5882(4) 0.082(2) Uani 1 1 d . . . O8W O 0.0786(3) 1.0707(3) 0.7736(5) 0.114(3) Uani 1 1 d . . . O9W O 0.0277(2) 0.9906(2) 0.6358(4) 0.0721(18) Uani 1 1 d . . . O10W O 0.4961(5) 0.7558(7) 0.8328(14) 0.314(11) Uani 1 1 d . . . O11W O 0.1031(4) 0.3122(6) 0.6584(11) 0.229(8) Uani 1 1 d . . . O13W O 0.0000 0.5316(6) 0.2500 0.135(5) Uani 1 2 d SU C 1 O14W O 0.0144(16) 0.5236(17) 0.317(3) 0.31(2) Uani 0.50 1 d PU D 2 O15W O 0.0150(3) 0.8602(4) 0.3460(6) 0.136(3) Uani 1 1 d . . . O16W O 0.0108(7) 0.3370(13) 0.347(3) 0.41(4) Uani 0.50 1 d P . . O17W O 0.0000 0.9548(5) 0.7500 0.201(9) Uani 1 2 d S . . O18W O 0.0000 0.8545(5) 0.7500 0.123(4) Uani 1 2 d S . . Cl1 Cl 0.15838(13) 0.46947(15) 0.2217(3) 0.1079(12) Uani 1 1 d . . . Cl2 Cl 0.21338(8) 0.68837(8) 0.16245(15) 0.0585(6) Uani 1 1 d . . . Cl3 Cl 0.11662(11) 0.79001(15) 0.3329(2) 0.0943(9) Uani 1 1 d . . . Cl4 Cl 0.03043(13) 0.21026(17) 0.4601(2) 0.1129(12) Uani 1 1 d . . . Cl5 Cl 0.09827(11) 0.00002(14) 0.47107(19) 0.0874(9) 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 0.0718(8) 0.0745(9) 0.0710(9) -0.0196(7) 0.0104(7) 0.0039(7) Cu2 0.0534(6) 0.0500(6) 0.0662(7) 0.0081(5) 0.0285(5) -0.0008(5) Cu3 0.0719(8) 0.0438(6) 0.0709(8) 0.0108(5) 0.0427(6) 0.0076(5) C1 0.053(5) 0.044(5) 0.055(6) 0.002(4) 0.024(4) -0.001(4) C2 0.054(5) 0.039(5) 0.066(6) 0.004(4) 0.028(5) 0.006(4) C3 0.048(5) 0.034(5) 0.065(6) 0.005(4) 0.021(4) 0.004(4) C4 0.049(5) 0.039(5) 0.059(6) 0.010(4) 0.023(4) 0.004(4) C5 0.056(5) 0.061(6) 0.047(5) -0.007(5) 0.019(4) 0.000(4) C6 0.113(8) 0.035(5) 0.085(8) 0.000(5) 0.045(6) 0.002(5) C7 0.094(8) 0.061(6) 0.074(7) -0.018(5) 0.041(6) 0.001(5) C8 0.090(8) 0.079(7) 0.070(7) 0.016(6) 0.034(6) 0.005(6) C9 0.057(6) 0.070(6) 0.051(6) -0.003(5) 0.016(5) -0.002(5) C10 0.078(7) 0.054(5) 0.068(6) 0.021(5) 0.043(5) 0.011(5) C11 0.062(6) 0.038(5) 0.089(7) -0.002(5) 0.033(5) 0.001(4) C12 0.058(6) 0.066(6) 0.060(6) -0.012(5) 0.020(5) -0.010(5) C13 0.052(6) 0.063(6) 0.079(7) -0.002(5) 0.020(5) -0.006(5) C14 0.056(6) 0.050(5) 0.057(6) 0.001(5) 0.020(5) -0.005(4) C15 0.066(7) 0.059(6) 0.063(6) 0.008(5) 0.029(6) 0.000(5) C16 0.092(9) 0.064(7) 0.101(9) 0.003(6) 0.055(7) -0.006(6) C17 0.123(11) 0.087(9) 0.126(12) 0.003(8) 0.096(10) -0.005(8) C18 0.149(13) 0.089(9) 0.089(9) 0.000(7) 0.074(10) 0.015(9) C19 0.109(10) 0.083(8) 0.094(9) -0.020(7) 0.061(8) 0.007(7) C20 0.062(6) 0.051(5) 0.056(6) 0.012(4) 0.026(5) -0.008(5) C21 0.054(5) 0.062(6) 0.059(6) 0.003(5) 0.028(5) -0.006(5) C22 0.052(5) 0.041(5) 0.036(5) -0.003(4) 0.019(4) -0.001(4) C23 0.057(5) 0.049(5) 0.037(5) -0.013(4) 0.015(4) -0.004(4) C24 0.056(6) 0.073(7) 0.072(7) -0.011(5) 0.028(5) 0.007(5) C25 0.079(7) 0.063(7) 0.089(8) -0.002(6) 0.033(6) 0.021(6) C26 0.102(9) 0.049(6) 0.094(8) -0.005(6) 0.043(7) 0.009(6) C27 0.080(7) 0.047(6) 0.077(7) -0.008(5) 0.036(6) -0.004(5) C28 0.052(6) 0.049(5) 0.094(8) -0.006(5) 0.032(5) 0.001(5) C29 0.041(5) 0.076(7) 0.076(7) -0.018(6) 0.018(5) -0.008(5) C30 0.057(6) 0.045(5) 0.054(5) -0.007(4) 0.020(4) -0.006(4) C31 0.071(7) 0.065(6) 0.057(6) -0.005(5) 0.031(5) -0.019(6) C32 0.113(10) 0.096(9) 0.093(9) -0.031(7) 0.063(8) -0.035(8) C33 0.142(13) 0.099(11) 0.092(10) -0.021(8) 0.055(10) -0.059(10) C34 0.155(13) 0.055(7) 0.120(12) 0.000(7) 0.090(11) -0.027(9) C35 0.119(10) 0.060(7) 0.089(8) 0.007(6) 0.066(7) -0.006(7) C36 0.061(5) 0.038(5) 0.051(6) 0.002(4) 0.016(4) -0.003(4) C37 0.19(3) 0.32(4) 0.68(8) 0.18(4) 0.28(4) 0.03(3) C38 0.055(9) 0.21(2) 0.47(4) -0.03(2) 0.105(17) 0.056(12) N1 0.056(5) 0.037(4) 0.078(5) 0.003(4) 0.029(4) 0.001(3) N2 0.062(5) 0.033(4) 0.065(5) 0.001(3) 0.030(4) -0.002(3) N3 0.090(6) 0.041(4) 0.066(5) 0.007(4) 0.045(5) -0.001(4) N4 0.054(4) 0.044(4) 0.049(4) 0.009(3) 0.021(3) 0.003(3) N5 0.046(4) 0.049(4) 0.049(4) -0.003(3) 0.021(3) 0.002(3) N6 0.053(4) 0.043(4) 0.059(5) -0.006(3) 0.030(4) -0.008(3) N7 0.041(4) 0.052(4) 0.054(4) -0.005(4) 0.012(4) -0.001(3) N8 0.054(5) 0.047(4) 0.051(4) -0.006(3) 0.016(4) 0.000(3) N9 0.075(6) 0.068(5) 0.066(6) -0.005(4) 0.026(5) 0.000(4) N10 0.33(3) 0.67(7) 0.28(3) 0.18(4) 0.18(3) 0.28(4) O1 0.146(11) 0.260(17) 0.39(3) 0.089(16) 0.137(14) -0.020(11) O3 0.212(13) 0.284(16) 0.119(9) 0.109(11) 0.046(9) 0.020(11) O2 0.195(10) 0.124(7) 0.106(7) 0.014(6) 0.048(7) -0.083(7) O4 0.247(14) 0.152(10) 0.179(12) -0.008(9) 0.114(11) 0.000(10) O5 0.140(7) 0.094(5) 0.083(5) -0.016(4) 0.063(5) 0.007(5) O8 0.069(5) 0.096(5) 0.129(7) 0.021(5) 0.029(5) 0.008(4) O7 0.112(6) 0.063(4) 0.071(5) 0.001(4) 0.022(4) 0.019(4) O6 0.132(6) 0.050(4) 0.096(6) -0.008(4) 0.051(5) -0.022(4) O10 0.118(8) 0.243(13) 0.170(11) -0.016(9) 0.047(7) 0.080(9) O9 0.27(2) 0.54(4) 0.28(2) 0.28(3) -0.045(17) -0.17(2) O12' 0.24(3) 0.154(18) 0.078(13) -0.016(13) 0.104(16) 0.054(18) O12 0.151(19) 0.116(17) 0.15(2) 0.006(14) -0.039(16) -0.006(14) O11 0.168(10) 0.204(11) 0.128(9) 0.079(8) 0.050(8) 0.034(9) O13 0.125(9) 0.281(16) 0.245(15) -0.096(13) 0.106(10) -0.005(10) O14 0.231(13) 0.156(9) 0.127(10) 0.067(8) 0.030(8) 0.009(9) O15 0.201(11) 0.133(9) 0.133(9) 0.044(7) 0.073(8) -0.016(8) O16 0.098(7) 0.221(12) 0.136(9) 0.030(8) 0.028(6) 0.006(7) O19 0.132(12) 0.92(6) 0.184(15) -0.26(3) 0.089(11) -0.10(2) O20' 0.47(8) 0.10(2) 0.87(14) 0.25(5) 0.49(10) 0.13(3) O17 0.085(5) 0.202(10) 0.107(7) -0.015(7) 0.056(5) 0.008(6) O18 0.80(5) 0.130(10) 0.57(4) 0.155(17) 0.61(4) 0.17(2) O20 0.27(3) 0.071(13) 0.086(12) 0.036(9) 0.128(15) 0.033(15) O1W 0.068(5) 0.145(7) 0.111(7) -0.047(6) 0.005(5) 0.006(5) O2W 0.125(7) 0.093(6) 0.242(13) 0.053(7) 0.058(8) 0.013(6) O3W 0.127(8) 0.198(10) 0.109(8) -0.080(7) 0.005(6) 0.000(7) O4W 0.080(5) 0.083(5) 0.117(6) 0.025(4) 0.064(4) 0.025(4) O5W 0.085(5) 0.078(5) 0.119(6) 0.033(4) 0.060(5) -0.005(4) O6W 0.116(7) 0.186(9) 0.103(7) -0.040(6) 0.042(5) -0.066(7) O7W 0.102(5) 0.065(4) 0.099(5) 0.040(4) 0.063(4) 0.036(4) O8W 0.194(9) 0.091(6) 0.090(6) -0.001(5) 0.092(6) 0.007(6) O9W 0.066(4) 0.055(4) 0.097(5) 0.016(4) 0.037(4) 0.002(3) O10W 0.176(13) 0.296(19) 0.37(3) -0.043(17) 0.016(15) -0.114(14) O11W 0.134(9) 0.260(15) 0.307(19) 0.149(14) 0.109(11) 0.051(10) O13W 0.084(7) 0.144(8) 0.148(9) 0.000 0.021(6) 0.000 O14W 0.32(2) 0.29(2) 0.30(2) -0.009(10) 0.134(13) 0.005(10) O15W 0.111(7) 0.200(10) 0.107(7) 0.012(7) 0.058(6) 0.052(6) O16W 0.057(13) 0.27(3) 0.73(9) 0.31(5) 0.00(3) -0.012(16) O17W 0.35(2) 0.098(9) 0.32(2) 0.000 0.30(2) 0.000 O18W 0.101(9) 0.113(9) 0.146(12) 0.000 0.046(8) 0.000 Cl1 0.101(2) 0.108(3) 0.114(3) 0.045(2) 0.045(2) -0.006(2) Cl2 0.0696(15) 0.0468(13) 0.0586(14) -0.0053(11) 0.0268(12) 0.0002(11) Cl3 0.085(2) 0.104(2) 0.090(2) 0.0119(19) 0.0335(18) 0.011(2) Cl4 0.093(2) 0.136(3) 0.104(3) 0.038(2) 0.037(2) 0.005(2) Cl5 0.083(2) 0.109(3) 0.0722(19) -0.0215(18) 0.0348(16) -0.0054(17) _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 O1W 1.973(8) . ? Cu1 O3W 1.975(9) . ? Cu1 N9 1.991(9) . ? Cu1 N8 1.991(7) . ? Cu1 O2W 2.295(9) . ? Cu2 O5W 1.976(6) . ? Cu2 O4W 1.978(6) . ? Cu2 N5 1.988(7) . ? Cu2 N6 1.995(7) . ? Cu2 O6W 2.281(8) . ? Cu3 O9W 1.989(6) . ? Cu3 O7W 1.989(6) . ? Cu3 N3 1.993(8) . ? Cu3 N2 2.016(7) . ? Cu3 O8W 2.257(7) . ? C1 C36 1.414(12) . ? C1 C2 1.418(11) . ? C1 C10 1.518(11) . ? C2 C3 1.380(12) . ? C2 C7 1.518(12) . ? C3 C4 1.389(12) . ? C3 C11 1.523(11) . ? C4 C5 1.410(11) . ? C4 C8 1.490(12) . ? C5 C36 1.396(12) . ? C5 C9 1.508(12) . ? C6 C36 1.522(11) . ? C9 N7 1.477(11) . ? C10 N4 1.432(10) . ? C11 N1 1.472(10) . ? C12 N7 1.324(10) . ? C12 C13 1.341(12) . ? C13 C14 1.381(12) . ? C14 N8 1.334(10) . ? C14 C15 1.469(13) . ? C15 N9 1.340(11) . ? C15 C16 1.378(14) . ? C16 C17 1.381(15) . ? C17 C18 1.399(17) . ? C18 C19 1.342(16) . ? C19 N9 1.341(13) . ? C20 N4 1.312(10) . ? C20 C21 1.375(11) . ? C21 C22 1.411(11) . ? C22 N5 1.327(10) . ? C22 C23 1.469(11) . ? C23 N6 1.325(10) . ? C23 C24 1.410(11) . ? C24 C25 1.390(14) . ? C25 C26 1.340(14) . ? C26 C27 1.412(13) . ? C27 N6 1.342(11) . ? C28 N1 1.344(10) . ? C28 C29 1.360(12) . ? C29 C30 1.373(12) . ? C30 N2 1.328(10) . ? C30 C31 1.451(13) . ? C31 N3 1.323(11) . ? C31 C32 1.379(14) . ? C32 C33 1.438(18) . ? C33 C34 1.283(17) . ? C34 C35 1.380(16) . ? C35 N3 1.343(12) . ? C37 C38 1.18(3) . ? C38 N10 0.97(2) . ? N1 N2 1.352(8) . ? N4 N5 1.363(8) . ? N7 N8 1.342(9) . ? O1 Cl1 1.268(13) . ? O3 Cl1 1.317(11) . ? O2 Cl1 1.376(8) . ? O4 Cl1 1.494(13) . ? O5 Cl2 1.403(7) . ? O8 Cl2 1.416(7) . ? O7 Cl2 1.437(7) . ? O6 Cl2 1.410(6) . ? O10 Cl3 1.344(10) . ? O9 Cl3 1.308(18) . ? O12' Cl3 1.389(15) . ? O12 Cl3 1.43(2) . ? O11 Cl3 1.382(10) . ? O13 Cl4 1.384(12) . ? O14 Cl4 1.391(11) . ? O15 Cl4 1.473(11) . ? O16 Cl4 1.403(10) . ? O19 Cl5 1.368(15) . ? O19 O20' 1.38(5) . ? O20' Cl5 1.27(4) . ? O17 Cl5 1.400(8) . ? O18 Cl5 1.225(13) . ? O20 Cl5 1.393(16) . ? 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 O1W Cu1 O3W 89.0(4) . . ? O1W Cu1 N9 179.2(4) . . ? O3W Cu1 N9 91.3(4) . . ? O1W Cu1 N8 98.2(3) . . ? O3W Cu1 N8 164.8(4) . . ? N9 Cu1 N8 81.3(3) . . ? O1W Cu1 O2W 86.0(4) . . ? O3W Cu1 O2W 96.0(5) . . ? N9 Cu1 O2W 94.7(3) . . ? N8 Cu1 O2W 97.8(4) . . ? O5W Cu2 O4W 89.1(3) . . ? O5W Cu2 N5 170.0(3) . . ? O4W Cu2 N5 96.8(3) . . ? O5W Cu2 N6 92.1(3) . . ? O4W Cu2 N6 169.8(3) . . ? N5 Cu2 N6 80.7(3) . . ? O5W Cu2 O6W 93.8(3) . . ? O4W Cu2 O6W 92.2(4) . . ? N5 Cu2 O6W 94.1(3) . . ? N6 Cu2 O6W 97.8(3) . . ? O9W Cu3 O7W 86.5(3) . . ? O9W Cu3 N3 177.0(3) . . ? O7W Cu3 N3 95.1(3) . . ? O9W Cu3 N2 97.5(3) . . ? O7W Cu3 N2 170.9(3) . . ? N3 Cu3 N2 80.6(3) . . ? O9W Cu3 O8W 91.9(3) . . ? O7W Cu3 O8W 88.8(3) . . ? N3 Cu3 O8W 90.7(3) . . ? N2 Cu3 O8W 99.2(3) . . ? C36 C1 C2 119.7(8) . . ? C36 C1 C10 119.0(7) . . ? C2 C1 C10 121.3(8) . . ? C3 C2 C1 118.9(8) . . ? C3 C2 C7 121.3(7) . . ? C1 C2 C7 119.8(8) . . ? C2 C3 C4 122.0(7) . . ? C2 C3 C11 120.0(8) . . ? C4 C3 C11 117.9(8) . . ? C3 C4 C5 119.0(8) . . ? C3 C4 C8 120.9(8) . . ? C5 C4 C8 120.1(8) . . ? C36 C5 C4 120.2(8) . . ? C36 C5 C9 119.5(8) . . ? C4 C5 C9 120.2(8) . . ? N7 C9 C5 111.1(7) . . ? N4 C10 C1 111.9(7) . . ? N1 C11 C3 112.0(7) . . ? N7 C12 C13 109.2(9) . . ? C12 C13 C14 104.5(8) . . ? N8 C14 C13 110.8(8) . . ? N8 C14 C15 116.3(8) . . ? C13 C14 C15 132.9(9) . . ? N9 C15 C16 122.0(10) . . ? N9 C15 C14 113.5(9) . . ? C16 C15 C14 124.6(10) . . ? C15 C16 C17 119.9(12) . . ? C16 C17 C18 116.5(12) . . ? C19 C18 C17 121.0(12) . . ? N9 C19 C18 122.1(12) . . ? N4 C20 C21 109.8(8) . . ? C20 C21 C22 103.4(8) . . ? N5 C22 C21 110.4(7) . . ? N5 C22 C23 116.0(7) . . ? C21 C22 C23 133.5(8) . . ? N6 C23 C24 122.5(8) . . ? N6 C23 C22 113.3(7) . . ? C24 C23 C22 124.2(8) . . ? C25 C24 C23 117.5(9) . . ? C26 C25 C24 119.4(10) . . ? C25 C26 C27 121.0(10) . . ? N6 C27 C26 119.6(9) . . ? N1 C28 C29 106.4(8) . . ? C28 C29 C30 106.8(8) . . ? N2 C30 C29 110.1(8) . . ? N2 C30 C31 115.8(8) . . ? C29 C30 C31 134.1(9) . . ? N3 C31 C32 123.6(10) . . ? N3 C31 C30 115.1(8) . . ? C32 C31 C30 121.3(11) . . ? C31 C32 C33 114.8(13) . . ? C34 C33 C32 121.4(13) . . ? C33 C34 C35 120.5(12) . . ? N3 C35 C34 120.9(11) . . ? C5 C36 C1 119.7(7) . . ? C5 C36 C6 119.9(8) . . ? C1 C36 C6 120.4(8) . . ? N10 C38 C37 156(4) . . ? C28 N1 N2 111.0(7) . . ? C28 N1 C11 128.2(7) . . ? N2 N1 C11 120.6(6) . . ? C30 N2 N1 105.7(7) . . ? C30 N2 Cu3 113.4(5) . . ? N1 N2 Cu3 140.4(6) . . ? C31 N3 C35 118.9(9) . . ? C31 N3 Cu3 114.8(6) . . ? C35 N3 Cu3 126.2(8) . . ? C20 N4 N5 110.2(7) . . ? C20 N4 C10 129.0(7) . . ? N5 N4 C10 120.6(7) . . ? C22 N5 N4 106.1(6) . . ? C22 N5 Cu2 113.0(5) . . ? N4 N5 Cu2 139.2(5) . . ? C23 N6 C27 119.9(8) . . ? C23 N6 Cu2 115.0(6) . . ? C27 N6 Cu2 125.1(6) . . ? C12 N7 N8 110.5(8) . . ? C12 N7 C9 128.7(8) . . ? N8 N7 C9 120.8(6) . . ? C14 N8 N7 105.0(7) . . ? C14 N8 Cu1 113.6(6) . . ? N7 N8 Cu1 141.0(6) . . ? C15 N9 C19 118.4(10) . . ? C15 N9 Cu1 115.1(7) . . ? C19 N9 Cu1 126.5(8) . . ? Cl5 O19 O20' 55(2) . . ? Cl5 O20' O19 62.2(16) . . ? O1 Cl1 O3 109.3(11) . . ? O1 Cl1 O2 116.5(9) . . ? O3 Cl1 O2 114.8(8) . . ? O1 Cl1 O4 106.8(11) . . ? O3 Cl1 O4 105.0(9) . . ? O2 Cl1 O4 103.3(8) . . ? O5 Cl2 O6 110.0(5) . . ? O5 Cl2 O8 108.0(5) . . ? O6 Cl2 O8 110.0(5) . . ? O5 Cl2 O7 109.4(5) . . ? O6 Cl2 O7 110.5(4) . . ? O8 Cl2 O7 108.9(5) . . ? O9 Cl3 O10 101.8(15) . . ? O9 Cl3 O11 100.5(9) . . ? O10 Cl3 O11 119.7(8) . . ? O9 Cl3 O12' 85.2(17) . . ? O10 Cl3 O12' 114.2(11) . . ? O11 Cl3 O12' 122.9(10) . . ? O9 Cl3 O12 151(2) . . ? O10 Cl3 O12 94.4(12) . . ? O11 Cl3 O12 91.6(10) . . ? O12' Cl3 O12 66.4(14) . . ? O13 Cl4 O14 109.2(9) . . ? O13 Cl4 O16 111.0(8) . . ? O14 Cl4 O16 108.3(8) . . ? O13 Cl4 O15 110.4(8) . . ? O14 Cl4 O15 104.9(7) . . ? O16 Cl4 O15 112.7(7) . . ? O18 Cl5 O20' 134(2) . . ? O18 Cl5 O19 87(2) . . ? O20' Cl5 O19 63(3) . . ? O18 Cl5 O20 103.6(13) . . ? O20' Cl5 O20 67(3) . . ? O19 Cl5 O20 117.7(17) . . ? O18 Cl5 O17 117.4(10) . . ? O20' Cl5 O17 106(2) . . ? O19 Cl5 O17 108.5(8) . . ? O20 Cl5 O17 118.6(12) . . ? 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 C36 C1 C2 C3 3.5(12) . . . . ? C10 C1 C2 C3 -174.2(8) . . . . ? C36 C1 C2 C7 -175.2(8) . . . . ? C10 C1 C2 C7 7.1(13) . . . . ? C1 C2 C3 C4 -7.6(13) . . . . ? C7 C2 C3 C4 171.1(8) . . . . ? C1 C2 C3 C11 170.3(7) . . . . ? C7 C2 C3 C11 -11.0(13) . . . . ? C2 C3 C4 C5 6.5(13) . . . . ? C11 C3 C4 C5 -171.4(7) . . . . ? C2 C3 C4 C8 -173.5(8) . . . . ? C11 C3 C4 C8 8.6(12) . . . . ? C3 C4 C5 C36 -1.4(12) . . . . ? C8 C4 C5 C36 178.6(8) . . . . ? C3 C4 C5 C9 177.8(8) . . . . ? C8 C4 C5 C9 -2.2(12) . . . . ? C36 C5 C9 N7 -83.6(10) . . . . ? C4 C5 C9 N7 97.3(9) . . . . ? C36 C1 C10 N4 67.2(10) . . . . ? C2 C1 C10 N4 -115.0(9) . . . . ? C2 C3 C11 N1 99.9(10) . . . . ? C4 C3 C11 N1 -82.1(10) . . . . ? N7 C12 C13 C14 -0.1(11) . . . . ? C12 C13 C14 N8 0.0(10) . . . . ? C12 C13 C14 C15 179.8(9) . . . . ? N8 C14 C15 N9 4.0(12) . . . . ? C13 C14 C15 N9 -175.9(9) . . . . ? N8 C14 C15 C16 -177.7(9) . . . . ? C13 C14 C15 C16 2.4(16) . . . . ? N9 C15 C16 C17 -1.7(15) . . . . ? C14 C15 C16 C17 -179.8(9) . . . . ? C15 C16 C17 C18 0.6(16) . . . . ? C16 C17 C18 C19 -1.4(18) . . . . ? C17 C18 C19 N9 3.2(19) . . . . ? N4 C20 C21 C22 0.1(10) . . . . ? C20 C21 C22 N5 -0.1(9) . . . . ? C20 C21 C22 C23 176.5(8) . . . . ? N5 C22 C23 N6 -7.1(10) . . . . ? C21 C22 C23 N6 176.4(8) . . . . ? N5 C22 C23 C24 170.6(7) . . . . ? C21 C22 C23 C24 -5.9(14) . . . . ? N6 C23 C24 C25 1.4(13) . . . . ? C22 C23 C24 C25 -176.2(8) . . . . ? C23 C24 C25 C26 -1.7(14) . . . . ? C24 C25 C26 C27 1.3(16) . . . . ? C25 C26 C27 N6 -0.5(15) . . . . ? N1 C28 C29 C30 1.4(11) . . . . ? C28 C29 C30 N2 0.1(11) . . . . ? C28 C29 C30 C31 180.0(10) . . . . ? N2 C30 C31 N3 -6.2(12) . . . . ? C29 C30 C31 N3 174.0(10) . . . . ? N2 C30 C31 C32 176.2(9) . . . . ? C29 C30 C31 C32 -3.7(17) . . . . ? N3 C31 C32 C33 0.8(15) . . . . ? C30 C31 C32 C33 178.2(10) . . . . ? C31 C32 C33 C34 -1.1(19) . . . . ? C32 C33 C34 C35 2(2) . . . . ? C33 C34 C35 N3 -2(2) . . . . ? C4 C5 C36 C1 -2.5(13) . . . . ? C9 C5 C36 C1 178.4(8) . . . . ? C4 C5 C36 C6 179.3(8) . . . . ? C9 C5 C36 C6 0.1(12) . . . . ? C2 C1 C36 C5 1.4(13) . . . . ? C10 C1 C36 C5 179.2(8) . . . . ? C2 C1 C36 C6 179.6(8) . . . . ? C10 C1 C36 C6 -2.6(13) . . . . ? C29 C28 N1 N2 -2.5(11) . . . . ? C29 C28 N1 C11 -177.3(9) . . . . ? C3 C11 N1 C28 -18.4(13) . . . . ? C3 C11 N1 N2 167.3(8) . . . . ? C29 C30 N2 N1 -1.6(10) . . . . ? C31 C30 N2 N1 178.5(7) . . . . ? C29 C30 N2 Cu3 -175.5(6) . . . . ? C31 C30 N2 Cu3 4.6(10) . . . . ? C28 N1 N2 C30 2.6(10) . . . . ? C11 N1 N2 C30 177.8(8) . . . . ? C28 N1 N2 Cu3 173.7(7) . . . . ? C11 N1 N2 Cu3 -11.1(13) . . . . ? O9W Cu3 N2 C30 175.9(6) . . . . ? O7W Cu3 N2 C30 61(2) . . . . ? N3 Cu3 N2 C30 -1.7(6) . . . . ? O8W Cu3 N2 C30 -91.0(6) . . . . ? O9W Cu3 N2 N1 5.2(9) . . . . ? O7W Cu3 N2 N1 -110.1(19) . . . . ? N3 Cu3 N2 N1 -172.5(9) . . . . ? O8W Cu3 N2 N1 98.3(9) . . . . ? C32 C31 N3 C35 -0.9(14) . . . . ? C30 C31 N3 C35 -178.5(8) . . . . ? C32 C31 N3 Cu3 -177.8(8) . . . . ? C30 C31 N3 Cu3 4.6(10) . . . . ? C34 C35 N3 C31 1.3(15) . . . . ? C34 C35 N3 Cu3 177.8(8) . . . . ? O9W Cu3 N3 C31 -52(6) . . . . ? O7W Cu3 N3 C31 -173.6(7) . . . . ? N2 Cu3 N3 C31 -1.7(7) . . . . ? O8W Cu3 N3 C31 97.5(7) . . . . ? O9W Cu3 N3 C35 132(5) . . . . ? O7W Cu3 N3 C35 9.7(8) . . . . ? N2 Cu3 N3 C35 -178.4(8) . . . . ? O8W Cu3 N3 C35 -79.2(8) . . . . ? C21 C20 N4 N5 -0.1(10) . . . . ? C21 C20 N4 C10 -174.9(8) . . . . ? C1 C10 N4 C20 31.4(12) . . . . ? C1 C10 N4 N5 -142.9(7) . . . . ? C21 C22 N5 N4 0.1(8) . . . . ? C23 C22 N5 N4 -177.2(6) . . . . ? C21 C22 N5 Cu2 -168.0(5) . . . . ? C23 C22 N5 Cu2 14.7(8) . . . . ? C20 N4 N5 C22 0.0(8) . . . . ? C10 N4 N5 C22 175.3(7) . . . . ? C20 N4 N5 Cu2 163.1(7) . . . . ? C10 N4 N5 Cu2 -21.5(12) . . . . ? O5W Cu2 N5 C22 32(2) . . . . ? O4W Cu2 N5 C22 157.0(5) . . . . ? N6 Cu2 N5 C22 -13.0(5) . . . . ? O6W Cu2 N5 C22 -110.2(6) . . . . ? O5W Cu2 N5 N4 -130.5(16) . . . . ? O4W Cu2 N5 N4 -5.3(8) . . . . ? N6 Cu2 N5 N4 -175.4(8) . . . . ? O6W Cu2 N5 N4 87.4(8) . . . . ? C24 C23 N6 C27 -0.6(12) . . . . ? C22 C23 N6 C27 177.2(7) . . . . ? C24 C23 N6 Cu2 178.1(6) . . . . ? C22 C23 N6 Cu2 -4.1(8) . . . . ? C26 C27 N6 C23 0.1(13) . . . . ? C26 C27 N6 Cu2 -178.5(7) . . . . ? O5W Cu2 N6 C23 -163.7(6) . . . . ? O4W Cu2 N6 C23 -67.1(18) . . . . ? N5 Cu2 N6 C23 9.3(5) . . . . ? O6W Cu2 N6 C23 102.2(6) . . . . ? O5W Cu2 N6 C27 15.0(7) . . . . ? O4W Cu2 N6 C27 111.6(16) . . . . ? N5 Cu2 N6 C27 -172.1(7) . . . . ? O6W Cu2 N6 C27 -79.1(7) . . . . ? C13 C12 N7 N8 0.1(10) . . . . ? C13 C12 N7 C9 -177.1(8) . . . . ? C5 C9 N7 C12 -13.1(13) . . . . ? C5 C9 N7 N8 170.0(7) . . . . ? C13 C14 N8 N7 0.1(9) . . . . ? C15 C14 N8 N7 -179.8(7) . . . . ? C13 C14 N8 Cu1 175.0(6) . . . . ? C15 C14 N8 Cu1 -4.9(10) . . . . ? C12 N7 N8 C14 -0.2(9) . . . . ? C9 N7 N8 C14 177.3(7) . . . . ? C12 N7 N8 Cu1 -172.6(7) . . . . ? C9 N7 N8 Cu1 4.8(13) . . . . ? O1W Cu1 N8 C14 -176.0(6) . . . . ? O3W Cu1 N8 C14 -58.3(16) . . . . ? N9 Cu1 N8 C14 3.4(6) . . . . ? O2W Cu1 N8 C14 97.0(6) . . . . ? O1W Cu1 N8 N7 -3.9(9) . . . . ? O3W Cu1 N8 N7 113.7(16) . . . . ? N9 Cu1 N8 N7 175.4(9) . . . . ? O2W Cu1 N8 N7 -90.9(9) . . . . ? C16 C15 N9 C19 3.3(14) . . . . ? C14 C15 N9 C19 -178.3(9) . . . . ? C16 C15 N9 Cu1 -179.4(7) . . . . ? C14 C15 N9 Cu1 -1.0(10) . . . . ? C18 C19 N9 C15 -4.1(16) . . . . ? C18 C19 N9 Cu1 178.9(9) . . . . ? O1W Cu1 N9 C15 53(26) . . . . ? O3W Cu1 N9 C15 165.5(8) . . . . ? N8 Cu1 N9 C15 -1.2(7) . . . . ? O2W Cu1 N9 C15 -98.3(7) . . . . ? O1W Cu1 N9 C19 -130(25) . . . . ? O3W Cu1 N9 C19 -17.4(9) . . . . ? N8 Cu1 N9 C19 175.9(9) . . . . ? O2W Cu1 N9 C19 78.7(9) . . . . ? O19 O20' Cl5 O18 -55(5) . . . . ? O19 O20' Cl5 O20 -142(3) . . . . ? O19 O20' Cl5 O17 103.0(14) . . . . ? O20' O19 Cl5 O18 143(3) . . . . ? O20' O19 Cl5 O20 40(3) . . . . ? O20' O19 Cl5 O17 -99(3) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.241 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.120 #===END