data_complex3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.50 H35 Cl3 Cu2 N8' _chemical_formula_weight 855.18 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7258(2) _cell_length_b 20.3270(2) _cell_length_c 25.0991(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7512.95(15) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3496 _exptl_absorpt_coefficient_mu 1.387 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6278 _exptl_absorpt_correction_T_max 0.8853 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70825 _diffrn_reflns_av_R_equivalents 0.1132 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8594 _reflns_number_gt 5275 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0470P)^2^+11.7915P] 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 8594 _refine_ls_number_parameters 487 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.051 _refine_ls_shift/su_mean 0.003 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 0.53737(3) 0.34306(2) 0.308492(18) 0.02656(14) Uani 1 1 d . . . Cu2 Cu 0.38410(3) 0.45651(2) 0.257276(19) 0.02734(14) Uani 1 1 d . . . N1 N 0.6129(2) 0.41339(16) 0.33091(13) 0.0298(8) Uani 1 1 d . . . N2 N 0.5618(2) 0.38214(15) 0.23503(13) 0.0270(8) Uani 1 1 d . . . N3 N 0.4386(2) 0.46303(16) 0.18471(13) 0.0285(8) Uani 1 1 d . . . N4 N 0.3949(2) 0.55079(15) 0.25355(13) 0.0282(8) Uani 1 1 d . . . N5 N 0.3255(2) 0.46833(15) 0.32444(13) 0.0281(8) Uani 1 1 d . . . N6 N 0.3405(2) 0.36067(16) 0.26829(13) 0.0283(8) Uani 1 1 d . . . N7 N 0.4593(2) 0.26349(16) 0.29996(13) 0.0288(8) Uani 1 1 d . . . N8 N 0.5442(2) 0.31193(17) 0.37989(13) 0.0304(8) Uani 1 1 d . . . C1 C 0.6504(3) 0.4332(2) 0.37717(16) 0.0315(10) Uani 1 1 d . . . C2 C 0.7026(3) 0.4896(2) 0.36708(18) 0.0392(11) Uani 1 1 d . . . H2 H 0.7364 0.5143 0.3930 0.047 Uiso 1 1 d R . . C3 C 0.6965(3) 0.5038(2) 0.31268(17) 0.0349(10) Uani 1 1 d . . . H3 H 0.7249 0.5396 0.2942 0.042 Uiso 1 1 d R . . C4 C 0.6407(3) 0.4553(2) 0.29080(16) 0.0282(9) Uani 1 1 d . . . C5 C 0.6107(3) 0.43663(19) 0.24012(16) 0.0285(9) Uani 1 1 d . . . H5 H 0.6248 0.4630 0.2095 0.034 Uiso 1 1 d R . . C6 C 0.5308(3) 0.36563(19) 0.18318(15) 0.0262(9) Uani 1 1 d . . . C7 C 0.5553(3) 0.3067(2) 0.15930(17) 0.0317(10) Uani 1 1 d . . . H7 H 0.5921 0.2757 0.1785 0.038 Uiso 1 1 d R . . C8 C 0.5271(3) 0.2925(2) 0.10799(17) 0.0386(11) Uani 1 1 d . . . H8A H 0.5452 0.2519 0.0915 0.046 Uiso 1 1 d R . . C9 C 0.4739(3) 0.3362(2) 0.08008(17) 0.0399(11) Uani 1 1 d . . . H9A H 0.4564 0.3267 0.0440 0.048 Uiso 1 1 d R . . C10 C 0.4444(3) 0.3939(2) 0.10432(16) 0.0363(11) Uani 1 1 d . . . H10 H 0.4052 0.4236 0.0855 0.044 Uiso 1 1 d R . . C11 C 0.4724(3) 0.4088(2) 0.15562(15) 0.0274(9) Uani 1 1 d . . . C12 C 0.4336(3) 0.5230(2) 0.16602(17) 0.0309(10) Uani 1 1 d . . . H12 H 0.4495 0.5328 0.1298 0.037 Uiso 1 1 d R . . C13 C 0.4038(3) 0.5726(2) 0.20145(16) 0.0285(9) Uani 1 1 d . . . C14 C 0.3695(3) 0.6362(2) 0.19803(17) 0.0319(10) Uani 1 1 d . . . H14 H 0.3679 0.6636 0.1669 0.038 Uiso 1 1 d R . . C15 C 0.3381(3) 0.6528(2) 0.24883(17) 0.0331(10) Uani 1 1 d . . . H15 H 0.3105 0.6936 0.2592 0.040 Uiso 1 1 d R . . C16 C 0.3544(3) 0.59887(19) 0.28184(17) 0.0295(10) Uani 1 1 d . . . C17 C 0.3382(3) 0.5886(2) 0.34152(16) 0.0322(10) Uani 1 1 d . . . C18 C 0.2988(3) 0.5209(2) 0.35269(16) 0.0297(9) Uani 1 1 d . . . C19 C 0.2379(3) 0.4998(2) 0.39230(17) 0.0390(11) Uani 1 1 d . . . H19 H 0.2088 0.5270 0.4185 0.047 Uiso 1 1 d R . . C20 C 0.2272(3) 0.4321(2) 0.38681(17) 0.0389(11) Uani 1 1 d . . . H20 H 0.1897 0.4038 0.4081 0.047 Uiso 1 1 d R . . C21 C 0.2822(3) 0.4136(2) 0.34393(16) 0.0293(9) Uani 1 1 d . . . C22 C 0.2939(3) 0.35653(19) 0.31266(15) 0.0279(9) Uani 1 1 d . . . H22 H 0.2680 0.3153 0.3236 0.033 Uiso 1 1 d R . . C23 C 0.3490(3) 0.30191(19) 0.23663(16) 0.0281(9) Uani 1 1 d . . . C24 C 0.3031(3) 0.2959(2) 0.18885(16) 0.0332(10) Uani 1 1 d . . . H24 H 0.2665 0.3316 0.1761 0.040 Uiso 1 1 d R . . C25 C 0.3098(3) 0.2387(2) 0.15965(18) 0.0374(11) Uani 1 1 d . . . H25 H 0.2784 0.2347 0.1263 0.045 Uiso 1 1 d R . . C26 C 0.3618(3) 0.1867(2) 0.17802(18) 0.0358(11) Uani 1 1 d . . . H26 H 0.3638 0.1462 0.1583 0.043 Uiso 1 1 d R . . C27 C 0.4108(3) 0.1927(2) 0.22497(17) 0.0326(10) Uani 1 1 d . . . H27 H 0.4490 0.1572 0.2366 0.039 Uiso 1 1 d R . . C28 C 0.4049(3) 0.25008(19) 0.25487(16) 0.0270(9) Uani 1 1 d . . . C29 C 0.4645(3) 0.2250(2) 0.34149(17) 0.0325(10) Uani 1 1 d . . . H29 H 0.4355 0.1827 0.3418 0.039 Uiso 1 1 d R . . C30 C 0.5148(3) 0.2481(2) 0.38587(16) 0.0314(10) Uani 1 1 d . . . C31 C 0.5462(3) 0.2248(2) 0.43472(18) 0.0449(12) Uani 1 1 d . . . H31 H 0.5357 0.1819 0.4496 0.054 Uiso 1 1 d R . . C32 C 0.5948(3) 0.2756(3) 0.45764(18) 0.0460(12) Uani 1 1 d . . . H32 H 0.6244 0.2742 0.4917 0.055 Uiso 1 1 d R . . C33 C 0.5940(3) 0.3292(2) 0.42274(17) 0.0349(10) Uani 1 1 d . . . C34 C 0.6297(3) 0.3989(2) 0.42965(17) 0.0363(11) Uani 1 1 d . . . C35 C 0.4298(3) 0.5943(2) 0.37050(18) 0.0437(12) Uani 1 1 d . . . H35A H 0.4701 0.5606 0.3578 0.066 Uiso 1 1 d R . . H35B H 0.4208 0.5891 0.4081 0.066 Uiso 1 1 d R . . H35C H 0.4560 0.6367 0.3635 0.066 Uiso 1 1 d R . . C36 C 0.2739(4) 0.6419(2) 0.3623(2) 0.0508(13) Uani 1 1 d . . . H36A H 0.2165 0.6383 0.3444 0.076 Uiso 1 1 d R . . H36B H 0.2998 0.6844 0.3554 0.076 Uiso 1 1 d R . . H36C H 0.2652 0.6365 0.3999 0.076 Uiso 1 1 d R . . C37 C 0.5548(4) 0.4402(3) 0.4574(2) 0.0530(14) Uani 1 1 d . . . H37A H 0.5014 0.4408 0.4354 0.079 Uiso 1 1 d R . . H37B H 0.5763 0.4844 0.4624 0.079 Uiso 1 1 d R . . H37C H 0.5404 0.4212 0.4913 0.079 Uiso 1 1 d R . . C38 C 0.7145(4) 0.3976(3) 0.46468(19) 0.0628(17) Uani 1 1 d . . . H38A H 0.7608 0.3717 0.4478 0.094 Uiso 1 1 d R . . H38B H 0.6998 0.3787 0.4987 0.094 Uiso 1 1 d R . . H38C H 0.7363 0.4417 0.4697 0.094 Uiso 1 1 d R . . Cl1A Cl 0.3398(2) 0.36261(12) 0.53234(7) 0.1316(10) Uani 1 1 d . . . Cl2A Cl 0.28852(11) 0.26970(8) 0.44957(7) 0.0810(5) Uani 1 1 d . . . C1A C 0.3624(3) 0.3323(3) 0.4702(2) 0.0517(13) Uani 1 1 d . . . H1AA H 0.4235 0.3158 0.4696 0.062 Uiso 1 1 d R . . H1AB H 0.3585 0.3678 0.4451 0.062 Uiso 1 1 d R . . Cl1B Cl -0.0592(4) 0.5104(4) 0.5066(3) 0.1324(19) Uani 0.50 1 d PU . . Cl2B Cl 0.1023(4) 0.4512(2) 0.51635(14) 0.0950(13) Uani 0.50 1 d PU . . C1B C 0.0409(8) 0.5430(7) 0.4737(5) 0.065(3) Uani 0.50 1 d PU . . H1BA H 0.0673 0.5839 0.4848 0.078 Uiso 0.50 1 d PR . . H1BB H 0.0444 0.5396 0.4356 0.078 Uiso 0.50 1 d PR . . 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 0.0276(3) 0.0292(3) 0.0228(2) 0.0003(2) -0.0014(2) -0.0029(2) Cu2 0.0306(3) 0.0261(2) 0.0253(3) 0.0032(2) 0.0051(2) 0.0036(2) N1 0.030(2) 0.0354(19) 0.0234(18) -0.0013(15) 0.0002(16) -0.0040(16) N2 0.0280(19) 0.0270(17) 0.0260(18) -0.0012(15) -0.0017(15) -0.0009(15) N3 0.0270(19) 0.0306(18) 0.0279(18) 0.0026(16) 0.0011(15) 0.0031(15) N4 0.0269(18) 0.0293(17) 0.0284(18) 0.0025(15) 0.0014(15) 0.0019(15) N5 0.032(2) 0.0259(17) 0.0265(18) 0.0021(15) 0.0031(15) -0.0003(15) N6 0.0281(19) 0.0292(18) 0.0277(19) -0.0001(15) 0.0026(15) 0.0005(15) N7 0.0294(19) 0.0291(17) 0.0280(18) 0.0006(15) -0.0003(16) 0.0005(16) N8 0.0281(19) 0.0365(19) 0.0267(18) 0.0015(16) 0.0002(16) -0.0007(16) C1 0.026(2) 0.042(2) 0.027(2) -0.007(2) 0.0020(18) -0.0014(19) C2 0.033(3) 0.048(3) 0.036(3) -0.014(2) 0.001(2) -0.008(2) C3 0.031(2) 0.038(2) 0.035(2) -0.004(2) 0.007(2) -0.005(2) C4 0.025(2) 0.032(2) 0.027(2) -0.0027(19) 0.0018(17) -0.0029(18) C5 0.025(2) 0.029(2) 0.031(2) 0.0016(18) 0.0031(19) 0.0033(18) C6 0.025(2) 0.032(2) 0.022(2) -0.0008(17) 0.0019(17) -0.0018(18) C7 0.031(2) 0.030(2) 0.034(2) -0.0026(19) 0.0036(19) -0.0017(19) C8 0.049(3) 0.034(2) 0.033(2) -0.009(2) 0.006(2) -0.006(2) C9 0.054(3) 0.044(3) 0.022(2) -0.004(2) 0.002(2) -0.010(2) C10 0.039(3) 0.040(2) 0.029(2) 0.007(2) -0.004(2) -0.006(2) C11 0.025(2) 0.033(2) 0.024(2) 0.0035(18) 0.0048(18) -0.0005(18) C12 0.026(2) 0.038(2) 0.028(2) 0.0067(19) -0.0026(18) -0.0025(19) C13 0.026(2) 0.030(2) 0.030(2) 0.0050(19) -0.0019(18) -0.0041(18) C14 0.029(2) 0.029(2) 0.038(3) 0.0084(19) -0.0050(19) -0.0037(18) C15 0.032(2) 0.026(2) 0.041(3) 0.000(2) -0.001(2) -0.0025(18) C16 0.024(2) 0.026(2) 0.038(2) -0.0024(19) -0.0005(19) 0.0006(18) C17 0.037(3) 0.030(2) 0.029(2) -0.0027(19) 0.002(2) 0.0023(19) C18 0.029(2) 0.031(2) 0.028(2) -0.0017(19) -0.0012(19) 0.0019(18) C19 0.047(3) 0.040(3) 0.030(2) -0.006(2) 0.011(2) 0.001(2) C20 0.042(3) 0.045(3) 0.029(2) -0.004(2) 0.010(2) -0.005(2) C21 0.031(2) 0.032(2) 0.025(2) 0.0024(19) -0.0017(18) 0.0008(18) C22 0.031(2) 0.026(2) 0.026(2) 0.0041(18) -0.0030(18) -0.0033(17) C23 0.026(2) 0.029(2) 0.029(2) -0.0044(18) 0.0050(18) -0.0017(18) C24 0.031(2) 0.038(2) 0.031(2) -0.001(2) 0.001(2) -0.007(2) C25 0.039(3) 0.041(3) 0.032(2) -0.002(2) -0.002(2) -0.011(2) C26 0.040(3) 0.031(2) 0.037(3) -0.009(2) 0.005(2) -0.010(2) C27 0.030(2) 0.030(2) 0.037(2) -0.001(2) 0.005(2) -0.0015(19) C28 0.024(2) 0.029(2) 0.028(2) -0.0004(18) 0.0050(17) -0.0051(17) C29 0.033(2) 0.027(2) 0.037(2) 0.0030(19) 0.005(2) -0.0004(19) C30 0.031(2) 0.035(2) 0.028(2) 0.0033(19) 0.0041(19) 0.0061(19) C31 0.051(3) 0.047(3) 0.036(3) 0.012(2) 0.005(2) 0.009(3) C32 0.046(3) 0.061(3) 0.030(2) 0.008(2) -0.004(2) 0.007(3) C33 0.027(2) 0.053(3) 0.025(2) -0.002(2) 0.0020(18) 0.002(2) C34 0.028(2) 0.053(3) 0.027(2) -0.004(2) -0.0006(19) -0.007(2) C35 0.055(3) 0.043(3) 0.033(3) -0.005(2) -0.006(2) -0.010(2) C36 0.065(4) 0.035(3) 0.052(3) -0.005(2) 0.019(3) 0.008(2) C37 0.060(4) 0.056(3) 0.043(3) -0.015(2) 0.020(3) -0.009(3) C38 0.053(4) 0.101(5) 0.034(3) 0.011(3) -0.014(2) -0.029(3) Cl1A 0.189(3) 0.1441(19) 0.0615(11) -0.0356(12) 0.0465(14) -0.0624(18) Cl2A 0.0695(11) 0.0762(10) 0.0973(12) -0.0167(9) 0.0181(9) -0.0349(9) C1A 0.046(3) 0.059(3) 0.050(3) -0.002(3) 0.006(2) -0.011(3) Cl1B 0.090(3) 0.172(4) 0.135(4) -0.085(3) 0.023(3) -0.027(3) Cl2B 0.151(3) 0.085(2) 0.0491(18) -0.0178(17) 0.023(2) -0.044(2) C1B 0.063(5) 0.083(5) 0.048(5) -0.022(4) -0.004(4) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.897(3) . ? Cu1 N8 1.903(3) . ? Cu1 N7 1.996(3) . ? Cu1 N2 2.040(3) . ? Cu2 N5 1.909(3) . ? Cu2 N4 1.925(3) . ? Cu2 N3 1.994(3) . ? Cu2 N6 2.069(3) . ? N1 C1 1.347(5) . ? N1 C4 1.380(5) . ? N2 C5 1.327(5) . ? N2 C6 1.419(5) . ? N3 C12 1.307(5) . ? N3 C11 1.414(5) . ? N4 C16 1.348(5) . ? N4 C13 1.387(5) . ? N5 C18 1.341(5) . ? N5 C21 1.373(5) . ? N6 C22 1.311(5) . ? N6 C23 1.440(5) . ? N7 C29 1.305(5) . ? N7 C28 1.413(5) . ? N8 C33 1.348(5) . ? N8 C30 1.376(5) . ? C1 C2 1.404(6) . ? C1 C34 1.522(6) . ? C2 C3 1.398(6) . ? C2 H2 0.9602 . ? C3 C4 1.396(6) . ? C3 H3 0.9600 . ? C4 C5 1.399(6) . ? C5 H5 0.9599 . ? C6 C7 1.387(6) . ? C6 C11 1.410(6) . ? C7 C8 1.384(6) . ? C7 H7 0.9600 . ? C8 C9 1.376(6) . ? C8 H8A 0.9599 . ? C9 C10 1.391(6) . ? C9 H9A 0.9599 . ? C10 C11 1.385(6) . ? C10 H10 0.9598 . ? C12 C13 1.414(6) . ? C12 H12 0.9598 . ? C13 C14 1.392(6) . ? C14 C15 1.397(6) . ? C14 H14 0.9601 . ? C15 C16 1.395(6) . ? C15 H15 0.9600 . ? C16 C17 1.531(6) . ? C17 C18 1.520(6) . ? C17 C36 1.529(6) . ? C17 C35 1.538(6) . ? C18 C19 1.406(6) . ? C19 C20 1.391(6) . ? C19 H19 0.9600 . ? C20 C21 1.398(6) . ? C20 H20 0.9601 . ? C21 C22 1.411(5) . ? C22 H22 0.9600 . ? C23 C24 1.382(6) . ? C23 C28 1.414(6) . ? C24 C25 1.377(6) . ? C24 H24 0.9600 . ? C25 C26 1.384(6) . ? C25 H25 0.9599 . ? C26 C27 1.387(6) . ? C26 H26 0.9600 . ? C27 C28 1.390(6) . ? C27 H27 0.9600 . ? C29 C30 1.418(6) . ? C29 H29 0.9601 . ? C30 C31 1.394(6) . ? C31 C32 1.382(7) . ? C31 H31 0.9601 . ? C32 C33 1.398(6) . ? C32 H32 0.9599 . ? C33 C34 1.521(6) . ? C34 C38 1.528(6) . ? C34 C37 1.551(6) . ? C35 H35A 0.9599 . ? C35 H35B 0.9599 . ? C35 H35C 0.9602 . ? C36 H36A 0.9599 . ? C36 H36B 0.9602 . ? C36 H36C 0.9601 . ? C37 H37A 0.9602 . ? C37 H37B 0.9601 . ? C37 H37C 0.9601 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? Cl1A C1A 1.709(5) . ? Cl2A C1A 1.752(5) . ? C1A H1AA 0.9600 . ? C1A H1AB 0.9600 . ? Cl1B Cl2B 1.160(8) 5_566 ? Cl1B C1B 1.223(13) 5_566 ? Cl1B C1B 1.815(14) . ? Cl1B Cl1B 1.824(11) 5_566 ? Cl2B Cl1B 1.160(8) 5_566 ? Cl2B C1B 2.126(14) 5_566 ? C1B Cl1B 1.223(13) 5_566 ? C1B Cl2B 2.126(14) 5_566 ? C1B H1BA 0.9599 . ? C1B H1BB 0.9600 . ? 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 N8 86.57(14) . . ? N1 Cu1 N7 168.64(14) . . ? N8 Cu1 N7 82.07(14) . . ? N1 Cu1 N2 82.59(13) . . ? N8 Cu1 N2 166.25(14) . . ? N7 Cu1 N2 108.69(13) . . ? N5 Cu2 N4 87.43(14) . . ? N5 Cu2 N3 168.46(13) . . ? N4 Cu2 N3 81.73(14) . . ? N5 Cu2 N6 81.97(13) . . ? N4 Cu2 N6 165.74(14) . . ? N3 Cu2 N6 108.01(13) . . ? C1 N1 C4 108.8(3) . . ? C1 N1 Cu1 136.2(3) . . ? C4 N1 Cu1 115.0(3) . . ? C5 N2 C6 117.4(3) . . ? C5 N2 Cu1 109.5(3) . . ? C6 N2 Cu1 132.8(3) . . ? C12 N3 C11 124.1(3) . . ? C12 N3 Cu2 111.6(3) . . ? C11 N3 Cu2 124.2(3) . . ? C16 N4 C13 107.9(3) . . ? C16 N4 Cu2 131.3(3) . . ? C13 N4 Cu2 111.8(3) . . ? C18 N5 C21 108.8(3) . . ? C18 N5 Cu2 134.4(3) . . ? C21 N5 Cu2 115.0(3) . . ? C22 N6 C23 117.4(3) . . ? C22 N6 Cu2 109.7(3) . . ? C23 N6 Cu2 132.9(3) . . ? C29 N7 C28 123.9(3) . . ? C29 N7 Cu1 111.5(3) . . ? C28 N7 Cu1 124.7(3) . . ? C33 N8 C30 109.2(4) . . ? C33 N8 Cu1 133.9(3) . . ? C30 N8 Cu1 113.6(3) . . ? N1 C1 C2 108.3(4) . . ? N1 C1 C34 121.8(4) . . ? C2 C1 C34 129.9(4) . . ? C3 C2 C1 108.0(4) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? C4 C3 C2 106.1(4) . . ? C4 C3 H3 127.0 . . ? C2 C3 H3 126.9 . . ? N1 C4 C3 108.8(4) . . ? N1 C4 C5 113.8(3) . . ? C3 C4 C5 137.3(4) . . ? N2 C5 C4 119.0(4) . . ? N2 C5 H5 120.4 . . ? C4 C5 H5 120.6 . . ? C7 C6 C11 118.9(4) . . ? C7 C6 N2 121.1(4) . . ? C11 C6 N2 119.9(3) . . ? C8 C7 C6 120.3(4) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 120.0(4) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 119.8(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.2 . . ? C10 C11 C6 120.1(4) . . ? C10 C11 N3 123.0(4) . . ? C6 C11 N3 116.5(3) . . ? N3 C12 C13 117.1(4) . . ? N3 C12 H12 121.4 . . ? C13 C12 H12 121.5 . . ? N4 C13 C14 108.7(4) . . ? N4 C13 C12 113.2(3) . . ? C14 C13 C12 137.5(4) . . ? C13 C14 C15 106.7(4) . . ? C13 C14 H14 126.7 . . ? C15 C14 H14 126.5 . . ? C16 C15 C14 107.2(4) . . ? C16 C15 H15 126.2 . . ? C14 C15 H15 126.6 . . ? N4 C16 C15 109.4(4) . . ? N4 C16 C17 119.1(4) . . ? C15 C16 C17 131.4(4) . . ? C18 C17 C36 110.1(4) . . ? C18 C17 C16 111.3(3) . . ? C36 C17 C16 109.5(4) . . ? C18 C17 C35 108.4(3) . . ? C36 C17 C35 109.2(4) . . ? C16 C17 C35 108.4(4) . . ? N5 C18 C19 108.5(4) . . ? N5 C18 C17 120.8(4) . . ? C19 C18 C17 130.5(4) . . ? C20 C19 C18 107.7(4) . . ? C20 C19 H19 126.0 . . ? C18 C19 H19 126.3 . . ? C19 C20 C21 106.1(4) . . ? C19 C20 H20 127.0 . . ? C21 C20 H20 126.9 . . ? N5 C21 C20 108.9(4) . . ? N5 C21 C22 114.3(3) . . ? C20 C21 C22 136.1(4) . . ? N6 C22 C21 118.9(4) . . ? N6 C22 H22 120.4 . . ? C21 C22 H22 120.6 . . ? C24 C23 C28 120.0(4) . . ? C24 C23 N6 120.7(4) . . ? C28 C23 N6 119.3(4) . . ? C25 C24 C23 120.1(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 120.3(4) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.0(4) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 120.1 . . ? C27 C28 C23 119.1(4) . . ? C27 C28 N7 124.0(4) . . ? C23 C28 N7 116.5(3) . . ? N7 C29 C30 117.4(4) . . ? N7 C29 H29 121.2 . . ? C30 C29 H29 121.4 . . ? N8 C30 C31 108.2(4) . . ? N8 C30 C29 113.0(4) . . ? C31 C30 C29 138.8(4) . . ? C32 C31 C30 106.5(4) . . ? C32 C31 H31 126.9 . . ? C30 C31 H31 126.7 . . ? C31 C32 C33 108.5(4) . . ? C31 C32 H32 125.7 . . ? C33 C32 H32 125.8 . . ? N8 C33 C32 107.6(4) . . ? N8 C33 C34 121.4(4) . . ? C32 C33 C34 130.7(4) . . ? C1 C34 C33 113.4(3) . . ? C1 C34 C38 110.0(4) . . ? C33 C34 C38 109.4(4) . . ? C1 C34 C37 106.4(4) . . ? C33 C34 C37 108.1(4) . . ? C38 C34 C37 109.4(4) . . ? C17 C35 H35A 109.4 . . ? C17 C35 H35B 109.6 . . ? H35A C35 H35B 109.5 . . ? C17 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C17 C36 H36A 109.5 . . ? C17 C36 H36B 109.3 . . ? H36A C36 H36B 109.5 . . ? C17 C36 H36C 109.7 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.4 . . ? C34 C37 H37B 109.3 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.7 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.6 . . ? C34 C38 H38B 109.4 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.4 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Cl1A C1A Cl2A 114.2(3) . . ? Cl1A C1A H1AA 108.9 . . ? Cl2A C1A H1AA 108.9 . . ? Cl1A C1A H1AB 108.4 . . ? Cl2A C1A H1AB 108.3 . . ? H1AA C1A H1AB 107.9 . . ? Cl2B Cl1B C1B 156.9(8) 5_566 5_566 ? Cl2B Cl1B C1B 88.4(8) 5_566 . ? C1B Cl1B C1B 109.2(9) 5_566 . ? Cl2B Cl1B Cl1B 126.0(9) 5_566 5_566 ? C1B Cl1B Cl1B 70.0(8) 5_566 5_566 ? C1B Cl1B Cl1B 39.3(4) . 5_566 ? Cl1B Cl2B C1B 58.6(6) 5_566 5_566 ? Cl1B C1B Cl1B 70.8(8) 5_566 . ? Cl1B C1B Cl2B 102.7(9) 5_566 5_566 ? Cl1B C1B Cl2B 33.1(3) . 5_566 ? Cl1B C1B H1BA 124.2 5_566 . ? Cl1B C1B H1BA 120.8 . . ? Cl2B C1B H1BA 108.6 5_566 . ? Cl1B C1B H1BB 109.1 5_566 . ? Cl1B C1B H1BB 118.1 . . ? Cl2B C1B H1BB 100.1 5_566 . ? H1BA C1B H1BB 109.3 . . ? 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 Cu1 N1 C1 -2.6(4) . . . . ? N7 Cu1 N1 C1 -1.0(10) . . . . ? N2 Cu1 N1 C1 -174.1(4) . . . . ? N8 Cu1 N1 C4 175.0(3) . . . . ? N7 Cu1 N1 C4 176.6(6) . . . . ? N2 Cu1 N1 C4 3.4(3) . . . . ? N1 Cu1 N2 C5 -3.9(3) . . . . ? N8 Cu1 N2 C5 -42.2(7) . . . . ? N7 Cu1 N2 C5 177.5(3) . . . . ? N1 Cu1 N2 C6 -177.6(4) . . . . ? N8 Cu1 N2 C6 144.2(5) . . . . ? N7 Cu1 N2 C6 3.9(4) . . . . ? N5 Cu2 N3 C12 4.7(9) . . . . ? N4 Cu2 N3 C12 -15.4(3) . . . . ? N6 Cu2 N3 C12 153.9(3) . . . . ? N5 Cu2 N3 C11 -171.1(6) . . . . ? N4 Cu2 N3 C11 168.8(3) . . . . ? N6 Cu2 N3 C11 -21.9(3) . . . . ? N5 Cu2 N4 C16 -14.4(4) . . . . ? N3 Cu2 N4 C16 161.7(4) . . . . ? N6 Cu2 N4 C16 27.5(8) . . . . ? N5 Cu2 N4 C13 -156.7(3) . . . . ? N3 Cu2 N4 C13 19.4(3) . . . . ? N6 Cu2 N4 C13 -114.7(5) . . . . ? N4 Cu2 N5 C18 4.5(4) . . . . ? N3 Cu2 N5 C18 -15.4(10) . . . . ? N6 Cu2 N5 C18 -165.9(4) . . . . ? N4 Cu2 N5 C21 166.9(3) . . . . ? N3 Cu2 N5 C21 147.0(6) . . . . ? N6 Cu2 N5 C21 -3.5(3) . . . . ? N5 Cu2 N6 C22 2.2(3) . . . . ? N4 Cu2 N6 C22 -40.2(7) . . . . ? N3 Cu2 N6 C22 -171.8(3) . . . . ? N5 Cu2 N6 C23 179.5(4) . . . . ? N4 Cu2 N6 C23 137.1(5) . . . . ? N3 Cu2 N6 C23 5.4(4) . . . . ? N1 Cu1 N7 C29 -13.0(9) . . . . ? N8 Cu1 N7 C29 -11.3(3) . . . . ? N2 Cu1 N7 C29 159.9(3) . . . . ? N1 Cu1 N7 C28 166.9(6) . . . . ? N8 Cu1 N7 C28 168.6(3) . . . . ? N2 Cu1 N7 C28 -20.2(3) . . . . ? N1 Cu1 N8 C33 -9.0(4) . . . . ? N7 Cu1 N8 C33 171.3(4) . . . . ? N2 Cu1 N8 C33 28.9(8) . . . . ? N1 Cu1 N8 C30 -165.7(3) . . . . ? N7 Cu1 N8 C30 14.6(3) . . . . ? N2 Cu1 N8 C30 -127.7(5) . . . . ? C4 N1 C1 C2 0.9(5) . . . . ? Cu1 N1 C1 C2 178.5(3) . . . . ? C4 N1 C1 C34 177.2(4) . . . . ? Cu1 N1 C1 C34 -5.1(7) . . . . ? N1 C1 C2 C3 -0.5(5) . . . . ? C34 C1 C2 C3 -176.4(4) . . . . ? C1 C2 C3 C4 -0.1(5) . . . . ? C1 N1 C4 C3 -0.9(5) . . . . ? Cu1 N1 C4 C3 -179.1(3) . . . . ? C1 N1 C4 C5 175.8(4) . . . . ? Cu1 N1 C4 C5 -2.4(4) . . . . ? C2 C3 C4 N1 0.6(5) . . . . ? C2 C3 C4 C5 -175.0(5) . . . . ? C6 N2 C5 C4 178.6(3) . . . . ? Cu1 N2 C5 C4 3.8(4) . . . . ? N1 C4 C5 N2 -1.2(5) . . . . ? C3 C4 C5 N2 174.3(5) . . . . ? C5 N2 C6 C7 120.3(4) . . . . ? Cu1 N2 C6 C7 -66.4(5) . . . . ? C5 N2 C6 C11 -61.2(5) . . . . ? Cu1 N2 C6 C11 112.0(4) . . . . ? C11 C6 C7 C8 3.8(6) . . . . ? N2 C6 C7 C8 -177.7(4) . . . . ? C6 C7 C8 C9 -0.4(7) . . . . ? C7 C8 C9 C10 -3.1(7) . . . . ? C8 C9 C10 C11 3.2(7) . . . . ? C9 C10 C11 C6 0.2(6) . . . . ? C9 C10 C11 N3 -173.7(4) . . . . ? C7 C6 C11 C10 -3.7(6) . . . . ? N2 C6 C11 C10 177.8(4) . . . . ? C7 C6 C11 N3 170.6(4) . . . . ? N2 C6 C11 N3 -7.8(5) . . . . ? C12 N3 C11 C10 -49.2(6) . . . . ? Cu2 N3 C11 C10 126.1(4) . . . . ? C12 N3 C11 C6 136.7(4) . . . . ? Cu2 N3 C11 C6 -48.1(5) . . . . ? C11 N3 C12 C13 -175.9(4) . . . . ? Cu2 N3 C12 C13 8.3(5) . . . . ? C16 N4 C13 C14 1.3(5) . . . . ? Cu2 N4 C13 C14 152.4(3) . . . . ? C16 N4 C13 C12 -171.5(3) . . . . ? Cu2 N4 C13 C12 -20.4(4) . . . . ? N3 C12 C13 N4 7.7(5) . . . . ? N3 C12 C13 C14 -162.1(5) . . . . ? N4 C13 C14 C15 -0.9(5) . . . . ? C12 C13 C14 C15 169.3(5) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C13 N4 C16 C15 -1.2(5) . . . . ? Cu2 N4 C16 C15 -144.5(3) . . . . ? C13 N4 C16 C17 -178.5(4) . . . . ? Cu2 N4 C16 C17 38.2(6) . . . . ? C14 C15 C16 N4 0.6(5) . . . . ? C14 C15 C16 C17 177.5(4) . . . . ? N4 C16 C17 C18 -45.8(5) . . . . ? C15 C16 C17 C18 137.6(5) . . . . ? N4 C16 C17 C36 -167.7(4) . . . . ? C15 C16 C17 C36 15.7(6) . . . . ? N4 C16 C17 C35 73.3(5) . . . . ? C15 C16 C17 C35 -103.3(5) . . . . ? C21 N5 C18 C19 1.1(5) . . . . ? Cu2 N5 C18 C19 164.3(3) . . . . ? C21 N5 C18 C17 177.8(4) . . . . ? Cu2 N5 C18 C17 -19.1(6) . . . . ? C36 C17 C18 N5 158.3(4) . . . . ? C16 C17 C18 N5 36.7(5) . . . . ? C35 C17 C18 N5 -82.3(5) . . . . ? C36 C17 C18 C19 -25.9(6) . . . . ? C16 C17 C18 C19 -147.4(5) . . . . ? C35 C17 C18 C19 93.5(5) . . . . ? N5 C18 C19 C20 -0.8(5) . . . . ? C17 C18 C19 C20 -177.0(4) . . . . ? C18 C19 C20 C21 0.1(5) . . . . ? C18 N5 C21 C20 -1.1(5) . . . . ? Cu2 N5 C21 C20 -167.9(3) . . . . ? C18 N5 C21 C22 171.0(4) . . . . ? Cu2 N5 C21 C22 4.2(5) . . . . ? C19 C20 C21 N5 0.6(5) . . . . ? C19 C20 C21 C22 -169.0(5) . . . . ? C23 N6 C22 C21 -178.3(4) . . . . ? Cu2 N6 C22 C21 -0.6(5) . . . . ? N5 C21 C22 N6 -2.3(6) . . . . ? C20 C21 C22 N6 166.9(5) . . . . ? C22 N6 C23 C24 108.3(4) . . . . ? Cu2 N6 C23 C24 -68.8(5) . . . . ? C22 N6 C23 C28 -71.7(5) . . . . ? Cu2 N6 C23 C28 111.2(4) . . . . ? C28 C23 C24 C25 1.8(6) . . . . ? N6 C23 C24 C25 -178.2(4) . . . . ? C23 C24 C25 C26 0.5(6) . . . . ? C24 C25 C26 C27 -2.7(7) . . . . ? C25 C26 C27 C28 2.5(6) . . . . ? C26 C27 C28 C23 -0.2(6) . . . . ? C26 C27 C28 N7 -173.0(4) . . . . ? C24 C23 C28 C27 -1.9(6) . . . . ? N6 C23 C28 C27 178.1(3) . . . . ? C24 C23 C28 N7 171.3(4) . . . . ? N6 C23 C28 N7 -8.6(5) . . . . ? C29 N7 C28 C27 -55.8(6) . . . . ? Cu1 N7 C28 C27 124.3(4) . . . . ? C29 N7 C28 C23 131.3(4) . . . . ? Cu1 N7 C28 C23 -48.6(5) . . . . ? C28 N7 C29 C30 -173.9(4) . . . . ? Cu1 N7 C29 C30 6.0(5) . . . . ? C33 N8 C30 C31 0.9(5) . . . . ? Cu1 N8 C30 C31 163.3(3) . . . . ? C33 N8 C30 C29 -177.8(4) . . . . ? Cu1 N8 C30 C29 -15.4(4) . . . . ? N7 C29 C30 N8 5.8(5) . . . . ? N7 C29 C30 C31 -172.3(5) . . . . ? N8 C30 C31 C32 -0.1(5) . . . . ? C29 C30 C31 C32 178.1(5) . . . . ? C30 C31 C32 C33 -0.7(5) . . . . ? C30 N8 C33 C32 -1.4(5) . . . . ? Cu1 N8 C33 C32 -158.7(3) . . . . ? C30 N8 C33 C34 -175.1(4) . . . . ? Cu1 N8 C33 C34 27.5(6) . . . . ? C31 C32 C33 N8 1.3(5) . . . . ? C31 C32 C33 C34 174.3(4) . . . . ? N1 C1 C34 C33 21.1(6) . . . . ? C2 C1 C34 C33 -163.4(4) . . . . ? N1 C1 C34 C38 144.0(4) . . . . ? C2 C1 C34 C38 -40.5(7) . . . . ? N1 C1 C34 C37 -97.6(5) . . . . ? C2 C1 C34 C37 77.9(6) . . . . ? N8 C33 C34 C1 -31.3(6) . . . . ? C32 C33 C34 C1 156.6(5) . . . . ? N8 C33 C34 C38 -154.4(4) . . . . ? C32 C33 C34 C38 33.4(6) . . . . ? N8 C33 C34 C37 86.5(5) . . . . ? C32 C33 C34 C37 -85.7(6) . . . . ? Cl2B Cl1B C1B Cl1B -164.7(8) 5_566 . . 5_566 ? C1B Cl1B C1B Cl1B 0.000(2) 5_566 . . 5_566 ? C1B Cl1B C1B Cl2B 164.7(8) 5_566 . . 5_566 ? Cl1B Cl1B C1B Cl2B 164.7(8) 5_566 . . 5_566 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.975 _refine_diff_density_min -0.980 _refine_diff_density_rms 0.094 #===END data_complex4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H52 Cl2 Cu2 N8 O2' _chemical_formula_weight 946.94 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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.9594(1) _cell_length_b 15.0893(1) _cell_length_c 18.9670(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.5110(5) _cell_angle_gamma 90.00 _cell_volume 4416.34(6) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prisms _exptl_crystal_colour 'red orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 1.132 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19669 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10107 _reflns_number_gt 6918 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _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. A large peak was found near Cu2 and within bonding distance of the imine nitrogen atoms N6 and N7. It was assumed that this peak was due to a disorder of the Cu ion, Cu2. The site occupancy factor for this pair of atoms was refined by assigning the variable, x, to the site occupancy for Cu2 and (1-x) to the site occupancy for Cu2a. At the same time as the site occupancy factor was refined, a common isotropic displacement factor was refined for both Cu2 and Cu2a. In this way, the site occupancy for Cu2 refined to 92(2)%. In addition, a smaller peak persisted in the difference electron density map and was found to be 1.87\a from pyrrole nitrogen atom, N5. This peak could not be explained in a chemically reasonable way. Both the peak near Cu2 and the unexplained peak near N5 persisted in two data collections on two different batches of crystals. ; _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^)+(0.0493P)^2^+2.5494P] 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 10107 _refine_ls_number_parameters 568 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1222 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.007 _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 0.54938(2) 0.12857(2) 0.160590(19) 0.03517(12) Uani 1 1 d . . . Cu2 Cu 0.60230(3) -0.02637(3) 0.40848(3) 0.03290(12) Uani 0.92 1 d P . . Cu2A Cu 0.5754(6) -0.0137(5) 0.3555(7) 0.086(2) Uani 0.08 1 d PU . . Cl1 Cl 0.59514(5) 0.08717(5) 0.27883(4) 0.03706(18) Uani 1 1 d U . . Cl2 Cl 0.70766(4) 0.05880(5) 0.48414(4) 0.03247(17) Uani 1 1 d . . . N1 N 0.47283(14) 0.27841(16) 0.24028(13) 0.0304(5) Uani 1 1 d . . . H1A H 0.5082 0.2311 0.2504 0.037 Uiso 1 1 d R . . N2 N 0.45213(16) 0.20215(17) 0.08670(13) 0.0331(6) Uani 1 1 d . . . N3 N 0.57815(18) 0.10719(15) 0.06915(13) 0.0347(6) Uani 1 1 d . . . N4 N 0.74441(16) 0.05290(15) 0.20237(13) 0.0302(5) Uani 1 1 d . . . H4A H 0.7038 0.0575 0.2211 0.036 Uiso 1 1 d R . . N5 N 0.74966(15) -0.07984(15) 0.35111(13) 0.0289(5) Uani 1 1 d . . . H5B H 0.7261 -0.0341 0.3661 0.035 Uiso 1 1 d R . . N6 N 0.59357(15) -0.15230(15) 0.36915(14) 0.0315(5) Uani 1 1 d . . . N7 N 0.47785(15) -0.04606(16) 0.39215(13) 0.0300(5) Uani 1 1 d . . . N8 N 0.48977(14) 0.15410(15) 0.39829(13) 0.0280(5) Uani 1 1 d . . . H8B H 0.5347 0.1349 0.3889 0.034 Uiso 1 1 d R . . C1 C 0.46552(18) 0.33277(19) 0.29465(17) 0.0307(6) Uani 1 1 d . . . C2 C 0.40464(19) 0.3972(2) 0.25597(18) 0.0379(7) Uani 1 1 d . . . H2A H 0.3870 0.4448 0.2797 0.046 Uiso 1 1 d R . . C3 C 0.37504(19) 0.3806(2) 0.17681(18) 0.0402(8) Uani 1 1 d . . . H3A H 0.3322 0.4142 0.1358 0.048 Uiso 1 1 d R . . C4 C 0.41729(18) 0.3063(2) 0.16699(16) 0.0326(7) Uani 1 1 d . . . C5 C 0.41004(19) 0.2696(2) 0.09549(17) 0.0363(7) Uani 1 1 d . . . H5A H 0.3694 0.2972 0.0489 0.044 Uiso 1 1 d R . . C6 C 0.4356(2) 0.1726(2) 0.01026(16) 0.0383(8) Uani 1 1 d . . . C7 C 0.3565(2) 0.1862(2) -0.05357(18) 0.0496(9) Uani 1 1 d . . . H7A H 0.3095 0.2153 -0.0472 0.060 Uiso 1 1 d R . . C8 C 0.3457(3) 0.1558(3) -0.12613(19) 0.0601(11) Uani 1 1 d . . . H8A H 0.2919 0.1650 -0.1705 0.072 Uiso 1 1 d R . . C9 C 0.4115(3) 0.1124(2) -0.1360(2) 0.0594(11) Uani 1 1 d . . . H9A H 0.4036 0.0939 -0.1869 0.071 Uiso 1 1 d R . . C10 C 0.4885(3) 0.0958(2) -0.07319(17) 0.0484(9) Uani 1 1 d . . . H10A H 0.5339 0.0635 -0.0796 0.058 Uiso 1 1 d R . . C11 C 0.5015(2) 0.12527(19) 0.00091(17) 0.0380(7) Uani 1 1 d . . . C12 C 0.6493(2) 0.0883(2) 0.06349(17) 0.0379(7) Uani 1 1 d . . . H12A H 0.6484 0.0903 0.0126 0.046 Uiso 1 1 d R . . C13 C 0.7293(2) 0.06444(19) 0.12568(17) 0.0353(7) Uani 1 1 d . . . C14 C 0.8078(2) 0.0516(2) 0.1213(2) 0.0459(9) Uani 1 1 d . . . H14A H 0.8173 0.0567 0.0750 0.055 Uiso 1 1 d R . . C15 C 0.8704(2) 0.0322(2) 0.1955(2) 0.0419(8) Uani 1 1 d . . . H15A H 0.9306 0.0200 0.2094 0.050 Uiso 1 1 d R . . C16 C 0.8295(2) 0.03319(18) 0.24536(18) 0.0329(7) Uani 1 1 d . . . C17 C 0.86369(19) 0.0116(2) 0.33088(18) 0.0348(7) Uani 1 1 d . . . C18 C 0.82141(18) -0.07481(19) 0.33605(16) 0.0298(6) Uani 1 1 d . . . C19 C 0.8386(2) -0.15863(19) 0.31709(17) 0.0348(7) Uani 1 1 d . . . H19A H 0.8862 -0.1747 0.3048 0.042 Uiso 1 1 d R . . C20 C 0.7748(2) -0.2145(2) 0.31920(18) 0.0387(7) Uani 1 1 d . . . H20A H 0.7697 -0.2768 0.3080 0.046 Uiso 1 1 d R . . C21 C 0.71925(19) -0.16515(18) 0.34076(16) 0.0307(6) Uani 1 1 d . . . C22 C 0.6441(2) -0.19653(19) 0.34714(16) 0.0330(7) Uani 1 1 d . . . H22A H 0.6290 -0.2574 0.3334 0.040 Uiso 1 1 d R . . C23 C 0.51890(19) -0.19356(19) 0.37137(16) 0.0324(6) Uani 1 1 d . . . C24 C 0.5034(2) -0.2851(2) 0.36255(19) 0.0428(8) Uani 1 1 d . . . H24A H 0.5453 -0.3231 0.3562 0.051 Uiso 1 1 d R . . C25 C 0.4290(2) -0.3205(2) 0.3633(2) 0.0467(8) Uani 1 1 d . . . H25A H 0.4184 -0.3831 0.3564 0.056 Uiso 1 1 d R . . C26 C 0.3693(2) -0.2661(2) 0.3732(2) 0.0516(9) Uani 1 1 d . . . H26A H 0.3176 -0.2909 0.3741 0.062 Uiso 1 1 d R . . C27 C 0.3840(2) -0.1764(2) 0.3832(2) 0.0451(8) Uani 1 1 d . . . H27A H 0.3415 -0.1390 0.3893 0.054 Uiso 1 1 d R . . C28 C 0.45895(19) -0.1386(2) 0.38311(16) 0.0330(7) Uani 1 1 d . . . C29 C 0.42770(18) 0.0063(2) 0.40874(15) 0.0301(6) Uani 1 1 d . . . H29A H 0.3827 -0.0208 0.4195 0.036 Uiso 1 1 d R . . C30 C 0.43229(18) 0.09994(19) 0.41235(16) 0.0294(6) Uani 1 1 d . . . C31 C 0.3753(2) 0.1552(2) 0.4249(2) 0.0461(8) Uani 1 1 d . . . H31A H 0.3283 0.1363 0.4371 0.055 Uiso 1 1 d R . . C32 C 0.3972(2) 0.2427(2) 0.4178(2) 0.0482(9) Uani 1 1 d . . . H32A H 0.3682 0.2951 0.4233 0.058 Uiso 1 1 d R . . C33 C 0.46905(18) 0.2407(2) 0.40139(16) 0.0306(6) Uani 1 1 d . . . C34 C 0.51447(18) 0.31642(19) 0.38085(16) 0.0321(6) Uani 1 1 d . . . C35 C 0.9623(2) -0.0026(3) 0.3643(2) 0.0545(9) Uani 1 1 d . . . H35A H 0.9756 -0.0500 0.3372 0.082 Uiso 1 1 d R . . H35B H 0.9898 0.0508 0.3587 0.082 Uiso 1 1 d R . . H35C H 0.9832 -0.0174 0.4183 0.082 Uiso 1 1 d R . . C36 C 0.8439(2) 0.0874(2) 0.37537(19) 0.0431(8) Uani 1 1 d . . . H36A H 0.7824 0.0966 0.3546 0.065 Uiso 1 1 d R . . H36B H 0.8650 0.0724 0.4293 0.065 Uiso 1 1 d R . . H36C H 0.8716 0.1407 0.3697 0.065 Uiso 1 1 d R . . C37 C 0.61023(18) 0.2951(2) 0.40220(17) 0.0358(7) Uani 1 1 d . . . H37A H 0.6146 0.2435 0.3745 0.054 Uiso 1 1 d R . . H37B H 0.6372 0.3445 0.3890 0.054 Uiso 1 1 d R . . H37C H 0.6389 0.2842 0.4569 0.054 Uiso 1 1 d R . . C38 C 0.5093(2) 0.3997(2) 0.42530(18) 0.0418(8) Uani 1 1 d . . . H38A H 0.4496 0.4137 0.4121 0.063 Uiso 1 1 d R . . H38B H 0.5383 0.3885 0.4799 0.063 Uiso 1 1 d R . . H38C H 0.5366 0.4488 0.4120 0.063 Uiso 1 1 d R . . O1A O 0.20074(15) 0.01211(19) 0.15306(14) 0.0575(7) Uani 1 1 d . . . C2A C 0.2279(2) 0.0036(3) 0.0925(2) 0.0554(9) Uani 1 1 d . . . H2AA H 0.1861 0.0303 0.0461 0.066 Uiso 1 1 d R . . H2AB H 0.2334 -0.0579 0.0825 0.066 Uiso 1 1 d R . . C3A C 0.3129(4) 0.0469(4) 0.1172(3) 0.100(2) Uani 1 1 d . . . H3AA H 0.3067 0.1021 0.0903 0.120 Uiso 1 1 d R . . H3AB H 0.3535 0.0104 0.1072 0.120 Uiso 1 1 d R . . C4A C 0.3431(3) 0.0641(4) 0.2014(3) 0.0888(17) Uani 1 1 d . . . H4AA H 0.3465 0.1264 0.2125 0.107 Uiso 1 1 d R . . H4AB H 0.3992 0.0382 0.2296 0.107 Uiso 1 1 d R . . C5A C 0.2764(3) 0.0222(4) 0.2221(2) 0.0832(16) Uani 1 1 d . . . H5AA H 0.2965 -0.0348 0.2450 0.100 Uiso 1 1 d R . . H5AB H 0.2649 0.0582 0.2585 0.100 Uiso 1 1 d R . . O1B O 0.1693(2) 0.3087(2) 0.41627(16) 0.0864(10) Uani 1 1 d . A . C2B C 0.1254(4) 0.2758(4) 0.3410(3) 0.1040(19) Uani 1 1 d . . . H2BA H 0.1517 0.2971 0.3082 0.125 Uiso 1 1 d R A . H2BB H 0.0660 0.2944 0.3201 0.125 Uiso 1 1 d R . . C3B C 0.1309(7) 0.1693(7) 0.3483(5) 0.079(3) Uani 0.56 1 d P A 1 H3BA H 0.1771 0.1477 0.3362 0.095 Uiso 0.56 1 d PR A 1 H3BB H 0.0778 0.1418 0.3141 0.095 Uiso 0.56 1 d PR A 1 C4B C 0.1483(8) 0.1551(9) 0.4256(8) 0.074(3) Uani 0.56 1 d P A 1 H4BA H 0.1876 0.1061 0.4452 0.088 Uiso 0.56 1 d PR A 1 H4BB H 0.0959 0.1425 0.4315 0.088 Uiso 0.56 1 d PR A 1 C5B C 0.1902(3) 0.2385(3) 0.4674(3) 0.0750(13) Uani 1 1 d . . . H5BA H 0.1707 0.2514 0.5071 0.090 Uiso 1 1 d R A . H5BB H 0.2520 0.2319 0.4916 0.090 Uiso 1 1 d R . . C3BA C 0.0743(8) 0.2019(8) 0.3463(6) 0.071(3) Uani 0.44 1 d P A . H3BC H 0.0792 0.1528 0.3161 0.086 Uiso 0.44 1 d PR B 2 H3BD H 0.0143 0.2170 0.3297 0.086 Uiso 0.44 1 d PR B 2 C4BA C 0.1174(9) 0.1815(13) 0.4354(10) 0.088(6) Uani 0.44 1 d P A 2 H4BC H 0.1359 0.1208 0.4437 0.105 Uiso 0.44 1 d PR A 2 H4BD H 0.0773 0.1915 0.4583 0.105 Uiso 0.44 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0429(2) 0.0355(2) 0.02498(19) 0.00433(15) 0.01191(16) -0.00439(17) Cu2 0.0286(2) 0.0295(2) 0.0413(3) -0.0082(2) 0.0152(2) -0.00538(18) Cu2A 0.086(5) 0.059(4) 0.142(7) 0.005(5) 0.075(5) 0.000(4) Cl1 0.0395(4) 0.0471(4) 0.0289(4) 0.0117(3) 0.0185(3) 0.0139(3) Cl2 0.0304(4) 0.0429(4) 0.0244(3) -0.0066(3) 0.0118(3) -0.0110(3) N1 0.0250(12) 0.0298(13) 0.0349(13) 0.0051(11) 0.0107(10) 0.0018(10) N2 0.0342(13) 0.0338(14) 0.0276(12) 0.0055(10) 0.0092(11) -0.0079(11) N3 0.0528(17) 0.0236(12) 0.0275(12) -0.0012(10) 0.0163(12) -0.0081(12) N4 0.0395(14) 0.0238(12) 0.0374(13) -0.0013(10) 0.0261(12) -0.0027(11) N5 0.0295(13) 0.0247(12) 0.0355(13) -0.0037(10) 0.0165(11) 0.0038(10) N6 0.0331(13) 0.0276(13) 0.0352(13) -0.0026(11) 0.0156(11) -0.0023(11) N7 0.0280(12) 0.0313(13) 0.0310(12) -0.0023(10) 0.0126(10) -0.0024(10) N8 0.0238(12) 0.0328(13) 0.0307(12) 0.0003(10) 0.0147(10) 0.0038(10) C1 0.0241(14) 0.0316(15) 0.0392(16) 0.0049(13) 0.0159(13) 0.0001(12) C2 0.0305(16) 0.0380(17) 0.0472(18) 0.0101(15) 0.0180(14) 0.0100(14) C3 0.0267(16) 0.0469(19) 0.0452(18) 0.0185(15) 0.0130(14) 0.0090(14) C4 0.0224(14) 0.0382(17) 0.0350(16) 0.0108(13) 0.0098(12) -0.0005(13) C5 0.0262(15) 0.0425(18) 0.0353(16) 0.0108(14) 0.0080(13) -0.0094(14) C6 0.0482(19) 0.0333(17) 0.0262(15) 0.0043(13) 0.0082(14) -0.0177(15) C7 0.051(2) 0.046(2) 0.0382(18) 0.0071(15) 0.0047(16) -0.0181(17) C8 0.075(3) 0.049(2) 0.0290(18) 0.0068(16) -0.0056(18) -0.027(2) C9 0.093(3) 0.042(2) 0.0302(18) -0.0026(15) 0.012(2) -0.026(2) C10 0.079(3) 0.0301(17) 0.0310(17) -0.0028(14) 0.0183(17) -0.0152(17) C11 0.054(2) 0.0274(15) 0.0267(15) 0.0020(12) 0.0112(14) -0.0127(14) C12 0.062(2) 0.0269(15) 0.0328(16) -0.0033(13) 0.0275(16) -0.0083(15) C13 0.056(2) 0.0229(15) 0.0372(17) -0.0040(12) 0.0299(16) -0.0044(14) C14 0.069(2) 0.0363(18) 0.056(2) -0.0046(16) 0.050(2) -0.0034(17) C15 0.0468(19) 0.0355(17) 0.058(2) -0.0049(15) 0.0364(17) -0.0041(15) C16 0.0393(17) 0.0202(14) 0.0495(18) -0.0049(13) 0.0287(15) -0.0028(12) C17 0.0309(16) 0.0314(16) 0.0458(17) -0.0066(14) 0.0195(14) -0.0020(13) C18 0.0276(15) 0.0344(16) 0.0277(14) 0.0022(12) 0.0118(12) 0.0062(12) C19 0.0404(17) 0.0301(15) 0.0419(17) 0.0075(13) 0.0250(15) 0.0119(14) C20 0.057(2) 0.0241(15) 0.0460(18) 0.0072(13) 0.0324(16) 0.0115(14) C21 0.0411(17) 0.0246(14) 0.0289(14) 0.0057(12) 0.0170(13) 0.0038(13) C22 0.0464(18) 0.0233(14) 0.0345(15) 0.0022(12) 0.0220(14) 0.0026(13) C23 0.0375(17) 0.0304(15) 0.0303(15) -0.0029(12) 0.0152(13) -0.0063(13) C24 0.053(2) 0.0324(17) 0.0494(19) -0.0073(15) 0.0278(17) -0.0086(15) C25 0.061(2) 0.0346(18) 0.052(2) -0.0104(15) 0.0309(18) -0.0181(17) C26 0.056(2) 0.049(2) 0.062(2) -0.0122(18) 0.0365(19) -0.0263(18) C27 0.0400(18) 0.045(2) 0.060(2) -0.0088(17) 0.0300(17) -0.0078(16) C28 0.0362(16) 0.0333(16) 0.0302(15) -0.0022(13) 0.0143(13) -0.0075(13) C29 0.0293(15) 0.0383(16) 0.0262(14) 0.0039(12) 0.0149(12) -0.0015(13) C30 0.0317(15) 0.0330(16) 0.0289(14) 0.0040(12) 0.0178(12) 0.0010(13) C31 0.046(2) 0.0426(19) 0.069(2) 0.0066(17) 0.0431(19) 0.0071(16) C32 0.049(2) 0.0401(19) 0.072(2) 0.0076(17) 0.0413(19) 0.0142(16) C33 0.0293(15) 0.0349(16) 0.0275(14) 0.0013(12) 0.0117(12) 0.0064(13) C34 0.0303(15) 0.0291(15) 0.0363(16) 0.0041(13) 0.0133(13) 0.0030(12) C35 0.0347(18) 0.064(2) 0.065(2) -0.007(2) 0.0210(17) -0.0046(17) C36 0.0472(19) 0.0390(18) 0.0490(19) -0.0166(15) 0.0260(16) -0.0098(15) C37 0.0286(16) 0.0380(17) 0.0375(16) 0.0051(14) 0.0104(13) 0.0003(13) C38 0.0440(19) 0.0361(17) 0.0427(18) -0.0005(14) 0.0152(15) 0.0013(15) O1A 0.0386(13) 0.0806(19) 0.0500(14) 0.0028(13) 0.0150(11) -0.0034(13) C2A 0.052(2) 0.063(2) 0.054(2) -0.0054(19) 0.0246(18) 0.0004(19) C3A 0.115(4) 0.116(4) 0.110(4) -0.047(3) 0.087(4) -0.059(4) C4A 0.052(3) 0.138(5) 0.066(3) 0.005(3) 0.014(2) -0.035(3) C5A 0.046(2) 0.145(5) 0.048(2) 0.010(3) 0.0086(19) -0.029(3) O1B 0.122(3) 0.089(2) 0.0494(17) -0.0137(17) 0.0371(18) -0.021(2) C2B 0.149(5) 0.116(4) 0.052(3) -0.019(3) 0.046(3) -0.048(4) C3B 0.082(7) 0.089(7) 0.056(5) -0.019(5) 0.020(5) -0.043(6) C4B 0.056(7) 0.085(7) 0.077(7) -0.022(5) 0.025(6) -0.031(6) C5B 0.074(3) 0.085(3) 0.066(3) -0.014(3) 0.030(2) 0.017(3) C3BA 0.076(8) 0.077(8) 0.056(6) 0.001(5) 0.022(6) -0.034(6) C4BA 0.053(9) 0.139(17) 0.062(8) 0.046(10) 0.014(6) -0.022(9) _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 2.000(2) . ? Cu1 N3 2.013(2) . ? Cu1 Cl1 2.1395(7) . ? Cu2 Cu2A 0.935(12) . ? Cu2 N7 2.024(2) . ? Cu2 N6 2.024(2) . ? Cu2 Cl2 2.1855(8) . ? Cu2A N7 2.101(8) . ? Cu2A N6 2.114(8) . ? Cu2A Cl1 2.224(9) . ? Cu2A Cl2 2.765(11) . ? N1 C1 1.363(4) . ? N1 C4 1.382(4) . ? N1 H1A 0.9000 . ? N2 C5 1.293(4) . ? N2 C6 1.429(4) . ? N3 C12 1.287(4) . ? N3 C11 1.429(4) . ? N4 C16 1.364(4) . ? N4 C13 1.379(4) . ? N4 H4A 0.8999 . ? N5 C18 1.362(4) . ? N5 C21 1.370(4) . ? N5 H5B 0.9001 . ? N6 C22 1.285(4) . ? N6 C23 1.427(4) . ? N7 C29 1.292(4) . ? N7 C28 1.427(4) . ? N8 C33 1.360(4) . ? N8 C30 1.380(4) . ? N8 H8B 0.9000 . ? C1 C2 1.386(4) . ? C1 C34 1.516(4) . ? C2 C3 1.394(5) . ? C2 H2A 0.9601 . ? C3 C4 1.385(4) . ? C3 H3A 0.9599 . ? C4 C5 1.422(4) . ? C5 H5A 0.9603 . ? C6 C11 1.398(5) . ? C6 C7 1.401(4) . ? C7 C8 1.389(5) . ? C7 H7A 0.9599 . ? C8 C9 1.372(6) . ? C8 H8A 0.9599 . ? C9 C10 1.377(5) . ? C9 H9A 0.9600 . ? C10 C11 1.402(4) . ? C10 H10A 0.9601 . ? C12 C13 1.426(5) . ? C12 H12A 0.9600 . ? C13 C14 1.381(5) . ? C14 C15 1.397(5) . ? C14 H14A 0.9603 . ? C15 C16 1.386(4) . ? C15 H15A 0.9598 . ? C16 C17 1.514(4) . ? C17 C18 1.511(4) . ? C17 C35 1.538(4) . ? C17 C36 1.539(4) . ? C18 C19 1.379(4) . ? C19 C20 1.385(4) . ? C19 H19A 0.9599 . ? C20 C21 1.389(4) . ? C20 H20A 0.9601 . ? C21 C22 1.411(4) . ? C22 H22A 0.9599 . ? C23 C28 1.400(4) . ? C23 C24 1.402(4) . ? C24 C25 1.376(5) . ? C24 H24A 0.9599 . ? C25 C26 1.375(5) . ? C25 H25A 0.9600 . ? C26 C27 1.375(5) . ? C26 H26A 0.9598 . ? C27 C28 1.394(4) . ? C27 H27A 0.9600 . ? C29 C30 1.414(4) . ? C29 H29A 0.9600 . ? C30 C31 1.370(4) . ? C31 C32 1.394(5) . ? C31 H31A 0.9600 . ? C32 C33 1.377(4) . ? C32 H32A 0.9601 . ? C33 C34 1.517(4) . ? C34 C37 1.536(4) . ? C34 C38 1.537(4) . ? C35 H35A 0.9602 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9599 . ? C36 H36B 0.9600 . ? C36 H36C 0.9601 . ? C37 H37A 0.9600 . ? C37 H37B 0.9599 . ? C37 H37C 0.9599 . ? C38 H38A 0.9601 . ? C38 H38B 0.9599 . ? C38 H38C 0.9600 . ? O1A C2A 1.409(4) . ? O1A C5A 1.411(4) . ? C2A C3A 1.471(6) . ? C2A H2AA 0.9600 . ? C2A H2AB 0.9600 . ? C3A C4A 1.484(6) . ? C3A H3AA 0.9600 . ? C3A H3AB 0.9601 . ? C4A C5A 1.483(6) . ? C4A H4AA 0.9602 . ? C4A H4AB 0.9599 . ? C5A H5AA 0.9599 . ? C5A H5AB 0.9599 . ? O1B C5B 1.379(5) . ? O1B C2B 1.399(5) . ? C2B C3BA 1.441(11) . ? C2B C3B 1.612(11) . ? C2B H2BA 0.9600 . ? C2B H2BB 0.9600 . ? C3B C3BA 1.066(14) . ? C3B C4B 1.386(16) . ? C3B H3BA 0.9602 . ? C3B H3BB 0.9598 . ? C3B H3BC 0.8713 . ? C4B C5B 1.500(14) . ? C4B C3BA 1.664(18) . ? C4B H4BA 0.9600 . ? C4B H4BB 0.9600 . ? C4B H4BC 0.7004 . ? C5B C4BA 1.418(17) . ? C5B H5BA 0.9601 . ? C5B H5BB 0.9600 . ? C3BA C4BA 1.567(19) . ? C3BA H2BB 1.4694 . ? C3BA H3BB 1.1096 . ? C3BA H3BC 0.9601 . ? C3BA H3BD 0.9599 . ? C4BA H4BB 0.6798 . ? C4BA H4BC 0.9600 . ? C4BA H4BD 0.9600 . ? 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 N3 84.80(10) . . ? N2 Cu1 Cl1 137.03(8) . . ? N3 Cu1 Cl1 138.08(8) . . ? Cu2A Cu2 N7 81.5(5) . . ? Cu2A Cu2 N6 82.4(5) . . ? N7 Cu2 N6 83.89(10) . . ? Cu2A Cu2 Cl2 119.2(5) . . ? N7 Cu2 Cl2 134.70(7) . . ? N6 Cu2 Cl2 135.14(7) . . ? Cu2 Cu2A N7 72.3(5) . . ? Cu2 Cu2A N6 71.6(5) . . ? N7 Cu2A N6 79.9(3) . . ? Cu2 Cu2A Cl1 134.7(7) . . ? N7 Cu2A Cl1 136.7(5) . . ? N6 Cu2A Cl1 134.7(4) . . ? Cu2 Cu2A Cl2 43.7(5) . . ? N7 Cu2A Cl2 105.2(4) . . ? N6 Cu2A Cl2 105.1(4) . . ? Cl1 Cu2A Cl2 91.1(3) . . ? Cu1 Cl1 Cu2A 142.9(3) . . ? Cu2 Cl2 Cu2A 17.18(18) . . ? C1 N1 C4 109.9(2) . . ? C1 N1 H1A 125.2 . . ? C4 N1 H1A 124.9 . . ? C5 N2 C6 119.4(3) . . ? C5 N2 Cu1 133.3(2) . . ? C6 N2 Cu1 107.2(2) . . ? C12 N3 C11 119.9(3) . . ? C12 N3 Cu1 132.7(2) . . ? C11 N3 Cu1 107.2(2) . . ? C16 N4 C13 110.2(2) . . ? C16 N4 H4A 125.1 . . ? C13 N4 H4A 124.7 . . ? C18 N5 C21 109.8(2) . . ? C18 N5 H5B 125.1 . . ? C21 N5 H5B 125.1 . . ? C22 N6 C23 120.2(2) . . ? C22 N6 Cu2 130.6(2) . . ? C23 N6 Cu2 109.20(18) . . ? C22 N6 Cu2A 123.8(3) . . ? C23 N6 Cu2A 110.4(3) . . ? Cu2 N6 Cu2A 26.0(3) . . ? C29 N7 C28 119.4(2) . . ? C29 N7 Cu2 128.5(2) . . ? C28 N7 Cu2 109.28(18) . . ? C29 N7 Cu2A 128.8(3) . . ? C28 N7 Cu2A 110.9(3) . . ? Cu2 N7 Cu2A 26.1(3) . . ? C33 N8 C30 110.2(2) . . ? C33 N8 H8B 124.9 . . ? C30 N8 H8B 124.9 . . ? N1 C1 C2 107.6(3) . . ? N1 C1 C34 122.5(2) . . ? C2 C1 C34 129.8(3) . . ? C1 C2 C3 107.5(3) . . ? C1 C2 H2A 125.9 . . ? C3 C2 H2A 126.6 . . ? C4 C3 C2 108.3(3) . . ? C4 C3 H3A 125.4 . . ? C2 C3 H3A 126.2 . . ? N1 C4 C3 106.6(3) . . ? N1 C4 C5 126.5(3) . . ? C3 C4 C5 126.8(3) . . ? N2 C5 C4 126.5(3) . . ? N2 C5 H5A 116.5 . . ? C4 C5 H5A 117.0 . . ? C11 C6 C7 119.7(3) . . ? C11 C6 N2 117.2(3) . . ? C7 C6 N2 123.0(3) . . ? C8 C7 C6 119.5(4) . . ? C8 C7 H7A 120.1 . . ? C6 C7 H7A 120.4 . . ? C9 C8 C7 120.8(4) . . ? C9 C8 H8A 118.7 . . ? C7 C8 H8A 120.5 . . ? C8 C9 C10 120.2(3) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 120.2 . . ? C9 C10 C11 120.5(4) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 119.2 . . ? C6 C11 C10 119.2(3) . . ? C6 C11 N3 117.2(3) . . ? C10 C11 N3 123.6(3) . . ? N3 C12 C13 126.1(3) . . ? N3 C12 H12A 116.9 . . ? C13 C12 H12A 116.9 . . ? N4 C13 C14 106.4(3) . . ? N4 C13 C12 127.0(3) . . ? C14 C13 C12 126.6(3) . . ? C13 C14 C15 108.6(3) . . ? C13 C14 H14A 125.2 . . ? C15 C14 H14A 126.2 . . ? C16 C15 C14 107.3(3) . . ? C16 C15 H15A 126.2 . . ? C14 C15 H15A 126.5 . . ? N4 C16 C15 107.4(3) . . ? N4 C16 C17 121.8(2) . . ? C15 C16 C17 130.6(3) . . ? C18 C17 C16 105.9(2) . . ? C18 C17 C35 108.5(3) . . ? C16 C17 C35 109.8(3) . . ? C18 C17 C36 112.8(2) . . ? C16 C17 C36 110.7(3) . . ? C35 C17 C36 109.0(3) . . ? N5 C18 C19 107.9(3) . . ? N5 C18 C17 123.4(2) . . ? C19 C18 C17 128.1(3) . . ? C18 C19 C20 107.4(3) . . ? C18 C19 H19A 125.8 . . ? C20 C19 H19A 126.8 . . ? C19 C20 C21 108.4(3) . . ? C19 C20 H20A 126.1 . . ? C21 C20 H20A 125.5 . . ? N5 C21 C20 106.6(3) . . ? N5 C21 C22 127.1(3) . . ? C20 C21 C22 126.3(3) . . ? N6 C22 C21 127.0(3) . . ? N6 C22 H22A 116.5 . . ? C21 C22 H22A 116.5 . . ? C28 C23 C24 119.3(3) . . ? C28 C23 N6 117.2(3) . . ? C24 C23 N6 123.4(3) . . ? C25 C24 C23 120.6(3) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 119.4 . . ? C26 C25 C24 119.9(3) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.1 . . ? C27 C26 C25 120.3(3) . . ? C27 C26 H26A 119.7 . . ? C25 C26 H26A 119.9 . . ? C26 C27 C28 121.1(3) . . ? C26 C27 H27A 119.5 . . ? C28 C27 H27A 119.4 . . ? C27 C28 C23 118.7(3) . . ? C27 C28 N7 124.1(3) . . ? C23 C28 N7 117.2(3) . . ? N7 C29 C30 126.5(3) . . ? N7 C29 H29A 116.9 . . ? C30 C29 H29A 116.6 . . ? C31 C30 N8 106.2(3) . . ? C31 C30 C29 125.9(3) . . ? N8 C30 C29 127.7(3) . . ? C30 C31 C32 108.8(3) . . ? C30 C31 H31A 125.2 . . ? C32 C31 H31A 125.9 . . ? C33 C32 C31 107.3(3) . . ? C33 C32 H32A 125.7 . . ? C31 C32 H32A 126.9 . . ? N8 C33 C32 107.4(3) . . ? N8 C33 C34 123.0(2) . . ? C32 C33 C34 129.2(3) . . ? C1 C34 C33 106.9(2) . . ? C1 C34 C37 111.4(2) . . ? C33 C34 C37 111.6(2) . . ? C1 C34 C38 109.2(2) . . ? C33 C34 C38 109.0(2) . . ? C37 C34 C38 108.7(2) . . ? C17 C35 H35A 109.8 . . ? C17 C35 H35B 109.4 . . ? H35A C35 H35B 109.5 . . ? C17 C35 H35C 109.2 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C17 C36 H36A 109.2 . . ? C17 C36 H36B 109.8 . . ? H36A C36 H36B 109.5 . . ? C17 C36 H36C 109.4 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.8 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.1 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.3 . . ? C34 C38 H38B 109.1 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 110.1 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C2A O1A C5A 106.7(3) . . ? O1A C2A C3A 108.0(3) . . ? O1A C2A H2AA 110.0 . . ? C3A C2A H2AA 111.1 . . ? O1A C2A H2AB 109.9 . . ? C3A C2A H2AB 109.2 . . ? H2AA C2A H2AB 108.6 . . ? C2A C3A C4A 106.0(3) . . ? C2A C3A H3AA 109.8 . . ? C4A C3A H3AA 109.5 . . ? C2A C3A H3AB 111.8 . . ? C4A C3A H3AB 111.0 . . ? H3AA C3A H3AB 108.8 . . ? C5A C4A C3A 104.4(4) . . ? C5A C4A H4AA 110.1 . . ? C3A C4A H4AA 111.7 . . ? C5A C4A H4AB 111.5 . . ? C3A C4A H4AB 110.3 . . ? H4AA C4A H4AB 108.7 . . ? O1A C5A C4A 107.5(3) . . ? O1A C5A H5AA 109.9 . . ? C4A C5A H5AA 109.6 . . ? O1A C5A H5AB 110.5 . . ? C4A C5A H5AB 110.7 . . ? H5AA C5A H5AB 108.7 . . ? C5B O1B C2B 108.5(4) . . ? O1B C2B C3BA 106.5(5) . . ? O1B C2B C3B 106.2(5) . . ? C3BA C2B C3B 40.4(5) . . ? O1B C2B H2BA 110.4 . . ? C3BA C2B H2BA 139.5 . . ? C3B C2B H2BA 111.4 . . ? O1B C2B H2BB 109.9 . . ? C3BA C2B H2BB 72.3 . . ? C3B C2B H2BB 110.0 . . ? H2BA C2B H2BB 109.0 . . ? C3BA C3B C4B 84.4(10) . . ? C3BA C3B C2B 61.2(9) . . ? C4B C3B C2B 103.0(8) . . ? C3BA C3B H3BA 163.9 . . ? C4B C3B H3BA 111.3 . . ? C2B C3B H3BA 109.9 . . ? C3BA C3B H3BB 66.2 . . ? C4B C3B H3BB 112.2 . . ? C2B C3B H3BB 111.6 . . ? H3BA C3B H3BB 108.8 . . ? C3BA C3B H3BC 58.4 . . ? C4B C3B H3BC 114.1 . . ? C2B C3B H3BC 102.6 . . ? H3BA C3B H3BC 114.9 . . ? H3BB C3B H3BC 9.2 . . ? C3B C4B C5B 106.0(10) . . ? C3B C4B C3BA 39.6(6) . . ? C5B C4B C3BA 97.8(9) . . ? C3B C4B H4BA 109.8 . . ? C5B C4B H4BA 109.9 . . ? C3BA C4B H4BA 145.0 . . ? C3B C4B H4BB 110.6 . . ? C5B C4B H4BB 111.3 . . ? C3BA C4B H4BB 78.5 . . ? H4BA C4B H4BB 109.2 . . ? C3B C4B H4BC 131.1 . . ? C5B C4B H4BC 122.2 . . ? C3BA C4B H4BC 119.3 . . ? H4BA C4B H4BC 62.8 . . ? H4BB C4B H4BC 46.7 . . ? O1B C5B C4BA 104.0(7) . . ? O1B C5B C4B 110.3(6) . . ? C4BA C5B C4B 29.3(7) . . ? O1B C5B H5BA 109.0 . . ? C4BA C5B H5BA 86.4 . . ? C4B C5B H5BA 110.1 . . ? O1B C5B H5BB 109.1 . . ? C4BA C5B H5BB 136.5 . . ? C4B C5B H5BB 110.4 . . ? H5BA C5B H5BB 108.0 . . ? C3B C3BA C2B 78.5(9) . . ? C3B C3BA C4BA 82.0(11) . . ? C2B C3BA C4BA 101.7(9) . . ? C3B C3BA C4B 56.0(8) . . ? C2B C3BA C4B 98.1(8) . . ? C4BA C3BA C4B 26.3(7) . . ? C3B C3BA H2BB 114.2 . . ? C2B C3BA H2BB 38.5 . . ? C4BA C3BA H2BB 119.2 . . ? C4B C3BA H2BB 129.8 . . ? C3B C3BA H3BB 52.3 . . ? C2B C3BA H3BB 115.0 . . ? C4BA C3BA H3BB 109.0 . . ? C4B C3BA H3BB 87.6 . . ? H2BB C3BA H3BB 127.6 . . ? C3B C3BA H3BC 50.6 . . ? C2B C3BA H3BC 110.5 . . ? C4BA C3BA H3BC 112.0 . . ? C4B C3BA H3BC 89.5 . . ? H2BB C3BA H3BC 123.4 . . ? H3BB C3BA H3BC 4.6 . . ? C3B C3BA H3BD 159.8 . . ? C2B C3BA H3BD 112.4 . . ? C4BA C3BA H3BD 110.9 . . ? C4B C3BA H3BD 134.2 . . ? H2BB C3BA H3BD 74.0 . . ? H3BB C3BA H3BD 107.7 . . ? H3BC C3BA H3BD 109.2 . . ? C5B C4BA C3BA 106.0(10) . . ? C5B C4BA H4BB 154.6 . . ? C3BA C4BA H4BB 93.7 . . ? C5B C4BA H4BC 109.9 . . ? C3BA C4BA H4BC 109.9 . . ? H4BB C4BA H4BC 46.8 . . ? C5B C4BA H4BD 111.4 . . ? C3BA C4BA H4BD 110.9 . . ? H4BB C4BA H4BD 74.8 . . ? H4BC C4BA H4BD 108.7 . . ? 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 N6 Cu2 Cu2A N7 84.92(13) . . . . ? Cl2 Cu2 Cu2A N7 -137.0(2) . . . . ? N7 Cu2 Cu2A N6 -84.92(13) . . . . ? Cl2 Cu2 Cu2A N6 138.1(2) . . . . ? N7 Cu2 Cu2A Cl1 139.5(8) . . . . ? N6 Cu2 Cu2A Cl1 -135.6(8) . . . . ? Cl2 Cu2 Cu2A Cl1 2.5(10) . . . . ? N7 Cu2 Cu2A Cl2 137.0(2) . . . . ? N6 Cu2 Cu2A Cl2 -138.1(2) . . . . ? N2 Cu1 Cl1 Cu2A 83.1(4) . . . . ? N3 Cu1 Cl1 Cu2A -92.3(4) . . . . ? Cu2 Cu2A Cl1 Cu1 177.2(6) . . . . ? N7 Cu2A Cl1 Cu1 -67.4(8) . . . . ? N6 Cu2A Cl1 Cu1 66.3(8) . . . . ? Cl2 Cu2A Cl1 Cu1 178.88(12) . . . . ? N7 Cu2 Cl2 Cu2A -108.4(6) . . . . ? N6 Cu2 Cl2 Cu2A 110.2(6) . . . . ? N7 Cu2A Cl2 Cu2 42.3(4) . . . . ? N6 Cu2A Cl2 Cu2 -41.0(4) . . . . ? Cl1 Cu2A Cl2 Cu2 -178.2(7) . . . . ? N3 Cu1 N2 C5 -152.5(3) . . . . ? Cl1 Cu1 N2 C5 30.6(3) . . . . ? N3 Cu1 N2 C6 22.07(18) . . . . ? Cl1 Cu1 N2 C6 -154.84(14) . . . . ? N2 Cu1 N3 C12 153.5(3) . . . . ? Cl1 Cu1 N3 C12 -29.6(3) . . . . ? N2 Cu1 N3 C11 -20.79(18) . . . . ? Cl1 Cu1 N3 C11 156.05(14) . . . . ? Cu2A Cu2 N6 C22 85.2(5) . . . . ? N7 Cu2 N6 C22 167.4(3) . . . . ? Cl2 Cu2 N6 C22 -39.0(3) . . . . ? Cu2A Cu2 N6 C23 -97.5(5) . . . . ? N7 Cu2 N6 C23 -15.20(18) . . . . ? Cl2 Cu2 N6 C23 138.36(15) . . . . ? N7 Cu2 N6 Cu2A 82.3(5) . . . . ? Cl2 Cu2 N6 Cu2A -124.2(5) . . . . ? Cu2 Cu2A N6 C22 -114.4(5) . . . . ? N7 Cu2A N6 C22 171.0(3) . . . . ? Cl1 Cu2A N6 C22 21.3(9) . . . . ? Cl2 Cu2A N6 C22 -85.8(4) . . . . ? Cu2 Cu2A N6 C23 92.1(5) . . . . ? N7 Cu2A N6 C23 17.5(4) . . . . ? Cl1 Cu2A N6 C23 -132.3(6) . . . . ? Cl2 Cu2A N6 C23 120.6(3) . . . . ? N7 Cu2A N6 Cu2 -74.6(4) . . . . ? Cl1 Cu2A N6 Cu2 135.6(10) . . . . ? Cl2 Cu2A N6 Cu2 28.5(3) . . . . ? Cu2A Cu2 N7 C29 -101.3(6) . . . . ? N6 Cu2 N7 C29 175.6(3) . . . . ? Cl2 Cu2 N7 C29 21.8(3) . . . . ? Cu2A Cu2 N7 C28 98.2(5) . . . . ? N6 Cu2 N7 C28 15.10(18) . . . . ? Cl2 Cu2 N7 C28 -138.68(15) . . . . ? N6 Cu2 N7 Cu2A -83.1(5) . . . . ? Cl2 Cu2 N7 Cu2A 123.1(5) . . . . ? Cu2 Cu2A N7 C29 100.1(5) . . . . ? N6 Cu2A N7 C29 173.9(3) . . . . ? Cl1 Cu2A N7 C29 -37.6(10) . . . . ? Cl2 Cu2A N7 C29 70.9(5) . . . . ? Cu2 Cu2A N7 C28 -91.5(5) . . . . ? N6 Cu2A N7 C28 -17.7(4) . . . . ? Cl1 Cu2A N7 C28 130.9(6) . . . . ? Cl2 Cu2A N7 C28 -120.7(3) . . . . ? N6 Cu2A N7 Cu2 73.8(5) . . . . ? Cl1 Cu2A N7 Cu2 -137.7(11) . . . . ? Cl2 Cu2A N7 Cu2 -29.2(3) . . . . ? C4 N1 C1 C2 -0.3(3) . . . . ? C4 N1 C1 C34 176.5(2) . . . . ? N1 C1 C2 C3 0.1(3) . . . . ? C34 C1 C2 C3 -176.4(3) . . . . ? C1 C2 C3 C4 0.2(3) . . . . ? C1 N1 C4 C3 0.5(3) . . . . ? C1 N1 C4 C5 176.1(3) . . . . ? C2 C3 C4 N1 -0.4(3) . . . . ? C2 C3 C4 C5 -176.0(3) . . . . ? C6 N2 C5 C4 178.6(3) . . . . ? Cu1 N2 C5 C4 -7.3(5) . . . . ? N1 C4 C5 N2 2.4(5) . . . . ? C3 C4 C5 N2 177.2(3) . . . . ? C5 N2 C6 C11 155.8(3) . . . . ? Cu1 N2 C6 C11 -19.7(3) . . . . ? C5 N2 C6 C7 -26.6(4) . . . . ? Cu1 N2 C6 C7 157.9(2) . . . . ? C11 C6 C7 C8 -2.8(5) . . . . ? N2 C6 C7 C8 179.7(3) . . . . ? C6 C7 C8 C9 0.2(5) . . . . ? C7 C8 C9 C10 2.1(5) . . . . ? C8 C9 C10 C11 -1.8(5) . . . . ? C7 C6 C11 C10 3.0(4) . . . . ? N2 C6 C11 C10 -179.3(3) . . . . ? C7 C6 C11 N3 -175.0(3) . . . . ? N2 C6 C11 N3 2.7(4) . . . . ? C9 C10 C11 C6 -0.7(5) . . . . ? C9 C10 C11 N3 177.1(3) . . . . ? C12 N3 C11 C6 -159.5(3) . . . . ? Cu1 N3 C11 C6 15.7(3) . . . . ? C12 N3 C11 C10 22.5(4) . . . . ? Cu1 N3 C11 C10 -162.2(2) . . . . ? C11 N3 C12 C13 -176.6(3) . . . . ? Cu1 N3 C12 C13 9.7(5) . . . . ? C16 N4 C13 C14 -0.1(3) . . . . ? C16 N4 C13 C12 -178.0(3) . . . . ? N3 C12 C13 N4 3.5(5) . . . . ? N3 C12 C13 C14 -173.9(3) . . . . ? N4 C13 C14 C15 0.0(3) . . . . ? C12 C13 C14 C15 177.9(3) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C13 N4 C16 C15 0.1(3) . . . . ? C13 N4 C16 C17 -176.2(2) . . . . ? C14 C15 C16 N4 -0.1(3) . . . . ? C14 C15 C16 C17 175.8(3) . . . . ? N4 C16 C17 C18 66.1(3) . . . . ? C15 C16 C17 C18 -109.3(3) . . . . ? N4 C16 C17 C35 -176.9(3) . . . . ? C15 C16 C17 C35 7.6(4) . . . . ? N4 C16 C17 C36 -56.5(4) . . . . ? C15 C16 C17 C36 128.0(3) . . . . ? C21 N5 C18 C19 -1.1(3) . . . . ? C21 N5 C18 C17 171.0(3) . . . . ? C16 C17 C18 N5 -97.7(3) . . . . ? C35 C17 C18 N5 144.5(3) . . . . ? C36 C17 C18 N5 23.6(4) . . . . ? C16 C17 C18 C19 72.8(4) . . . . ? C35 C17 C18 C19 -45.0(4) . . . . ? C36 C17 C18 C19 -165.9(3) . . . . ? N5 C18 C19 C20 1.3(3) . . . . ? C17 C18 C19 C20 -170.4(3) . . . . ? C18 C19 C20 C21 -1.0(4) . . . . ? C18 N5 C21 C20 0.5(3) . . . . ? C18 N5 C21 C22 -176.8(3) . . . . ? C19 C20 C21 N5 0.3(3) . . . . ? C19 C20 C21 C22 177.7(3) . . . . ? C23 N6 C22 C21 179.0(3) . . . . ? Cu2 N6 C22 C21 -3.8(5) . . . . ? Cu2A N6 C22 C21 27.9(6) . . . . ? N5 C21 C22 N6 -5.3(5) . . . . ? C20 C21 C22 N6 177.8(3) . . . . ? C22 N6 C23 C28 -169.5(3) . . . . ? Cu2 N6 C23 C28 12.8(3) . . . . ? Cu2A N6 C23 C28 -14.8(5) . . . . ? C22 N6 C23 C24 10.6(4) . . . . ? Cu2 N6 C23 C24 -167.1(2) . . . . ? Cu2A N6 C23 C24 165.2(4) . . . . ? C28 C23 C24 C25 1.8(5) . . . . ? N6 C23 C24 C25 -178.3(3) . . . . ? C23 C24 C25 C26 -0.5(5) . . . . ? C24 C25 C26 C27 -0.6(6) . . . . ? C25 C26 C27 C28 0.3(6) . . . . ? C26 C27 C28 C23 1.0(5) . . . . ? C26 C27 C28 N7 179.2(3) . . . . ? C24 C23 C28 C27 -2.0(4) . . . . ? N6 C23 C28 C27 178.1(3) . . . . ? C24 C23 C28 N7 179.7(3) . . . . ? N6 C23 C28 N7 -0.2(4) . . . . ? C29 N7 C28 C27 6.8(4) . . . . ? Cu2 N7 C28 C27 169.3(3) . . . . ? Cu2A N7 C28 C27 -162.9(4) . . . . ? C29 N7 C28 C23 -175.0(3) . . . . ? Cu2 N7 C28 C23 -12.5(3) . . . . ? Cu2A N7 C28 C23 15.3(5) . . . . ? C28 N7 C29 C30 -173.5(3) . . . . ? Cu2 N7 C29 C30 27.7(4) . . . . ? Cu2A N7 C29 C30 -5.9(6) . . . . ? C33 N8 C30 C31 -0.4(3) . . . . ? C33 N8 C30 C29 175.0(3) . . . . ? N7 C29 C30 C31 175.3(3) . . . . ? N7 C29 C30 N8 0.8(5) . . . . ? N8 C30 C31 C32 0.6(4) . . . . ? C29 C30 C31 C32 -174.9(3) . . . . ? C30 C31 C32 C33 -0.5(4) . . . . ? C30 N8 C33 C32 0.1(3) . . . . ? C30 N8 C33 C34 -173.9(2) . . . . ? C31 C32 C33 N8 0.3(4) . . . . ? C31 C32 C33 C34 173.8(3) . . . . ? N1 C1 C34 C33 -75.7(3) . . . . ? C2 C1 C34 C33 100.4(3) . . . . ? N1 C1 C34 C37 46.5(4) . . . . ? C2 C1 C34 C37 -137.4(3) . . . . ? N1 C1 C34 C38 166.6(3) . . . . ? C2 C1 C34 C38 -17.3(4) . . . . ? N8 C33 C34 C1 89.1(3) . . . . ? C32 C33 C34 C1 -83.5(4) . . . . ? N8 C33 C34 C37 -33.0(4) . . . . ? C32 C33 C34 C37 154.5(3) . . . . ? N8 C33 C34 C38 -153.1(3) . . . . ? C32 C33 C34 C38 34.3(4) . . . . ? C5A O1A C2A C3A -24.9(5) . . . . ? O1A C2A C3A C4A 11.9(6) . . . . ? C2A C3A C4A C5A 4.9(6) . . . . ? C2A O1A C5A C4A 28.2(5) . . . . ? C3A C4A C5A O1A -20.1(6) . . . . ? C5B O1B C2B C3BA 34.7(9) . . . . ? C5B O1B C2B C3B -7.4(7) . . . . ? O1B C2B C3B C3BA 96.6(9) . . . . ? O1B C2B C3B C4B 20.6(10) . . . . ? C3BA C2B C3B C4B -76.1(10) . . . . ? C3BA C3B C4B C5B -82.8(11) . . . . ? C2B C3B C4B C5B -24.1(10) . . . . ? C2B C3B C4B C3BA 58.7(9) . . . . ? C2B O1B C5B C4BA -37.6(9) . . . . ? C2B O1B C5B C4B -7.6(7) . . . . ? C3B C4B C5B O1B 21.8(10) . . . . ? C3BA C4B C5B O1B -17.8(8) . . . . ? C3B C4B C5B C4BA 104(2) . . . . ? C3BA C4B C5B C4BA 65(2) . . . . ? C4B C3B C3BA C2B 108.1(7) . . . . ? C4B C3B C3BA C4BA 4.4(12) . . . . ? C2B C3B C3BA C4BA -103.7(9) . . . . ? C2B C3B C3BA C4B -108.1(7) . . . . ? O1B C2B C3BA C3B -95.8(9) . . . . ? O1B C2B C3BA C4BA -16.5(12) . . . . ? C3B C2B C3BA C4BA 79.2(11) . . . . ? O1B C2B C3BA C4B -43.0(10) . . . . ? C3B C2B C3BA C4B 52.7(8) . . . . ? C5B C4B C3BA C3B 105.7(10) . . . . ? C3B C4B C3BA C2B -70.1(9) . . . . ? C5B C4B C3BA C2B 35.6(9) . . . . ? C3B C4B C3BA C4BA -170(3) . . . . ? C5B C4B C3BA C4BA -64(2) . . . . ? O1B C5B C4BA C3BA 25.2(13) . . . . ? C4B C5B C4BA C3BA -81(2) . . . . ? C3B C3BA C4BA C5B 71.1(13) . . . . ? C2B C3BA C4BA C5B -5.3(15) . . . . ? C4B C3BA C4BA C5B 79.4(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A Cl1 0.90 2.54 3.439(3) 174 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.084 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.073 #===END data_complex5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H74 Cl2 Cu2 N8 O3' _chemical_formula_weight 1129.23 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 24.2390(6) _cell_length_b 15.9732(4) _cell_length_c 14.2036(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.937(1) _cell_angle_gamma 90.00 _cell_volume 5432.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour brown _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 0.934 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11259 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.1288 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.43 _reflns_number_total 6112 _reflns_number_gt 2982 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _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^)+(0.0200P)^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 6112 _refine_ls_number_parameters 272 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1366 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1220 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.415 _refine_ls_restrained_S_all 1.417 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 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 -0.047440(18) 0.35526(3) 0.65364(4) 0.03446(17) Uani 1 1 d . . . Cl2 Cl 0.0000 0.24480(8) 0.7500 0.0263(3) Uani 1 2 d S . . Cl1 Cl 0.0000 0.45884(8) 0.7500 0.0310(3) Uani 1 2 d S . . N1 N 0.04199(11) 0.26057(18) 0.5386(2) 0.0273(8) Uani 1 1 d . . . H1N H 0.0217 0.2575 0.5865 0.033 Uiso 1 1 d R . . N2 N -0.04675(11) 0.38476(17) 0.5109(2) 0.0226(7) Uani 1 1 d . . . N3 N -0.13209(11) 0.36806(17) 0.6102(2) 0.0239(7) Uani 1 1 d . . . N4 N -0.13492(11) 0.24503(18) 0.7609(2) 0.0271(8) Uani 1 1 d . . . H4N H -0.1011 0.2694 0.7672 0.032 Uiso 1 1 d R . . C1 C 0.08708(15) 0.2119(2) 0.5304(3) 0.0329(10) Uani 1 1 d . . . C2 C 0.10758(16) 0.2366(3) 0.4490(3) 0.0442(12) Uani 1 1 d D . . C3 C 0.07381(15) 0.3027(3) 0.4065(3) 0.0375(11) Uani 1 1 d . . . C4 C 0.03187(14) 0.3165(2) 0.4631(3) 0.0263(9) Uani 1 1 d . . . C5 C -0.01270(13) 0.3737(2) 0.4495(3) 0.0267(9) Uani 1 1 d . . . H5 H -0.0179 0.4067 0.3924 0.032 Uiso 1 1 d R . . C6 C -0.09256(13) 0.4424(2) 0.4883(3) 0.0245(9) Uani 1 1 d . . . C7 C -0.09467(15) 0.5057(2) 0.4209(3) 0.0311(10) Uani 1 1 d . . . H7 H -0.0643 0.5128 0.3857 0.037 Uiso 1 1 d R . . C8 C -0.14102(15) 0.5581(2) 0.4049(3) 0.0377(11) Uani 1 1 d . . . H8 H -0.1430 0.6005 0.3566 0.045 Uiso 1 1 d R . . C9 C -0.18423(15) 0.5490(3) 0.4566(3) 0.0396(11) Uani 1 1 d . . . H9 H -0.2153 0.5871 0.4468 0.047 Uiso 1 1 d R . . C10 C -0.18237(14) 0.4858(2) 0.5238(3) 0.0315(10) Uani 1 1 d . . . H10 H -0.2127 0.4787 0.5592 0.038 Uiso 1 1 d R . . C11 C -0.13664(13) 0.4316(2) 0.5401(3) 0.0231(9) Uani 1 1 d . . . C12 C -0.17687(14) 0.3274(2) 0.6238(3) 0.0253(9) Uani 1 1 d . . . H12 H -0.2109 0.3412 0.5825 0.030 Uiso 1 1 d R . . C13 C -0.17968(14) 0.2659(2) 0.6934(3) 0.0265(9) Uani 1 1 d . . . C14 C -0.22358(14) 0.2132(2) 0.7079(3) 0.0337(10) Uani 1 1 d . . . C15 C -0.20387(15) 0.1610(2) 0.7848(3) 0.0335(10) Uani 1 1 d . . . C16 C -0.14893(15) 0.1812(2) 0.8165(3) 0.0296(10) Uani 1 1 d . . . C17 C -0.10750(15) 0.1468(2) 0.8962(3) 0.0327(10) Uani 1 1 d . . . H17A H -0.0716 0.1197 0.8797 0.039 Uiso 1 1 d R . . H17B H -0.1229 0.0947 0.9404 0.039 Uiso 1 1 d R . . C18 C 0.1589(2) 0.2019(4) 0.4141(4) 0.106(3) Uani 1 1 d D . . H18C H 0.1495 0.1917 0.3469 0.127 Uiso 0.50 1 d PR . . H18D H 0.1658 0.1482 0.4441 0.127 Uiso 0.50 1 d PR . . H18A H 0.1774 0.1678 0.4652 0.127 Uiso 0.50 1 d PR . . H18B H 0.1832 0.2484 0.4080 0.127 Uiso 0.50 1 d PR . . C19 C 0.1583(4) 0.1585(5) 0.3408(7) 0.059(3) Uani 0.50 1 d PD . . H19A H 0.1953 0.1420 0.3324 0.089 Uiso 0.50 1 d PR . . H19B H 0.1359 0.1095 0.3454 0.089 Uiso 0.50 1 d PR . . H19C H 0.1418 0.1915 0.2872 0.089 Uiso 0.50 1 d PR . . C19A C 0.2050(3) 0.2342(7) 0.4308(9) 0.088(4) Uani 0.50 1 d PD . . H19D H 0.2326 0.2019 0.4051 0.132 Uiso 0.50 1 d PR . . H19E H 0.2004 0.2873 0.3988 0.132 Uiso 0.50 1 d PR . . H19F H 0.2170 0.2431 0.4977 0.132 Uiso 0.50 1 d PR . . C20 C 0.08227(17) 0.3509(3) 0.3187(3) 0.0626(15) Uani 1 1 d . . . H20A H 0.0536 0.3925 0.3051 0.094 Uiso 1 1 d R . . H20B H 0.1182 0.3776 0.3286 0.094 Uiso 1 1 d R . . H20C H 0.0802 0.3128 0.2659 0.094 Uiso 1 1 d R . . C21 C -0.28177(15) 0.2120(3) 0.6503(3) 0.0516(13) Uani 1 1 d . . . H21A H -0.3039 0.1687 0.6727 0.077 Uiso 1 1 d R . . H21B H -0.2989 0.2654 0.6571 0.077 Uiso 1 1 d R . . H21C H -0.2793 0.2024 0.5843 0.077 Uiso 1 1 d R . . C22 C -0.23488(16) 0.0893(3) 0.8213(3) 0.0490(13) Uani 1 1 d . . . H22A H -0.2742 0.1012 0.8112 0.059 Uiso 1 1 d R . . H22B H -0.2228 0.0825 0.8886 0.059 Uiso 1 1 d R . . C23 C -0.2244(2) 0.0064(3) 0.7699(4) 0.0834(19) Uani 1 1 d . . . H23A H -0.2443 -0.0391 0.7934 0.125 Uiso 1 1 d R . . H23B H -0.2369 0.0133 0.7029 0.125 Uiso 1 1 d R . . H23C H -0.1852 -0.0055 0.7808 0.125 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 Cu1 0.0301(3) 0.0474(3) 0.0257(3) 0.0059(3) 0.0040(2) -0.0003(2) Cl2 0.0286(7) 0.0305(8) 0.0207(8) 0.000 0.0064(6) 0.000 Cl1 0.0418(8) 0.0263(8) 0.0261(9) 0.000 0.0096(7) 0.000 N1 0.0295(17) 0.0352(19) 0.020(2) -0.0006(16) 0.0119(15) 0.0038(15) N2 0.0201(15) 0.0265(17) 0.0203(19) -0.0018(15) -0.0002(14) -0.0010(13) N3 0.0264(16) 0.0266(18) 0.0200(18) -0.0050(15) 0.0078(14) 0.0016(14) N4 0.0266(17) 0.0302(18) 0.025(2) -0.0044(16) 0.0054(15) -0.0080(14) C1 0.033(2) 0.039(2) 0.026(3) -0.006(2) 0.0034(19) 0.008(2) C2 0.047(3) 0.067(3) 0.023(3) 0.013(2) 0.020(2) 0.027(2) C3 0.037(2) 0.053(3) 0.026(3) 0.007(2) 0.015(2) 0.013(2) C4 0.027(2) 0.034(2) 0.018(2) 0.0021(19) 0.0033(17) 0.0017(18) C5 0.025(2) 0.036(2) 0.020(2) 0.0000(19) 0.0059(17) 0.0022(18) C6 0.025(2) 0.027(2) 0.022(2) -0.0036(19) 0.0047(18) -0.0027(17) C7 0.037(2) 0.031(2) 0.027(3) 0.004(2) 0.0113(19) 0.002(2) C8 0.042(2) 0.039(3) 0.032(3) 0.011(2) 0.004(2) 0.010(2) C9 0.038(2) 0.038(3) 0.042(3) -0.001(2) 0.004(2) 0.015(2) C10 0.028(2) 0.038(2) 0.032(3) -0.004(2) 0.0139(19) 0.0074(19) C11 0.024(2) 0.026(2) 0.019(2) -0.0031(19) 0.0057(17) 0.0000(17) C12 0.025(2) 0.030(2) 0.022(2) -0.0075(19) 0.0091(17) -0.0017(17) C13 0.028(2) 0.031(2) 0.022(2) -0.0067(19) 0.0088(18) -0.0065(18) C14 0.030(2) 0.042(3) 0.030(3) -0.009(2) 0.009(2) -0.0117(19) C15 0.036(2) 0.037(3) 0.030(3) -0.007(2) 0.0130(19) -0.012(2) C16 0.042(2) 0.027(2) 0.022(2) -0.0040(19) 0.0122(19) -0.0128(19) C17 0.040(2) 0.032(2) 0.026(2) 0.002(2) 0.0039(18) -0.006(2) C18 0.107(5) 0.154(7) 0.074(5) 0.086(5) 0.070(4) 0.109(5) C19 0.070(6) 0.056(7) 0.061(7) -0.020(6) 0.037(6) 0.028(5) C19A 0.045(6) 0.099(9) 0.122(12) -0.017(8) 0.018(7) 0.029(7) C20 0.067(3) 0.087(4) 0.042(3) 0.041(3) 0.034(2) 0.045(3) C21 0.037(2) 0.072(3) 0.046(3) -0.003(3) 0.007(2) -0.019(2) C22 0.050(3) 0.054(3) 0.043(3) 0.002(3) 0.009(2) -0.032(2) C23 0.136(5) 0.063(4) 0.058(4) -0.008(3) 0.037(4) -0.065(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 N3 2.059(3) . ? Cu1 N2 2.084(3) . ? Cu1 Cl1 2.3332(10) . ? Cu1 Cl2 2.4124(10) . ? Cl2 Cu1 2.4124(10) 2_556 ? Cl1 Cu1 2.3332(10) 2_556 ? N1 C1 1.361(4) . ? N1 C4 1.387(4) . ? N1 H1N 0.9000 . ? N2 C5 1.302(4) . ? N2 C6 1.439(4) . ? N3 C12 1.305(4) . ? N3 C11 1.413(4) . ? N4 C16 1.364(4) . ? N4 C13 1.373(4) . ? N4 H4N 0.9000 . ? C1 C2 1.384(5) . ? C1 C17 1.501(5) 2_556 ? C2 C3 1.413(5) . ? C2 C18 1.515(6) . ? C3 C4 1.409(5) . ? C3 C20 1.506(5) . ? C4 C5 1.405(5) . ? C5 H5 0.9600 . ? C6 C7 1.388(5) . ? C6 C11 1.399(5) . ? C7 C8 1.391(5) . ? C7 H7 0.9600 . ? C8 C9 1.378(5) . ? C8 H8 0.9601 . ? C9 C10 1.385(5) . ? C9 H9 0.9600 . ? C10 C11 1.398(5) . ? C10 H10 0.9600 . ? C12 C13 1.403(5) . ? C12 H12 0.9600 . ? C13 C14 1.397(5) . ? C14 C15 1.398(5) . ? C14 C21 1.517(5) . ? C15 C16 1.376(5) . ? C15 C22 1.506(5) . ? C16 C17 1.497(5) . ? C17 C1 1.501(5) 2_556 ? C17 H17A 1.0304 . ? C17 H17B 1.1394 . ? C18 C19A 1.220(7) . ? C18 C19 1.250(7) . ? C18 H18C 0.9601 . ? C18 H18D 0.9600 . ? C18 H18A 0.9599 . ? C18 H18B 0.9600 . ? C19 C19A 1.983(14) . ? C19 H18C 0.5831 . ? C19 H18D 1.4594 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C19A H18A 1.3830 . ? C19A H18B 0.6185 . ? C19A H19D 0.9600 . ? C19A H19E 0.9600 . ? C19A H19F 0.9601 . ? C20 H20A 0.9599 . ? C20 H20B 0.9600 . ? C20 H20C 0.9599 . ? C21 H21A 0.9601 . ? C21 H21B 0.9601 . ? C21 H21C 0.9599 . ? C22 C23 1.551(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C23 H23A 0.9602 . ? C23 H23B 0.9599 . ? C23 H23C 0.9599 . ? 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 N3 Cu1 N2 81.03(11) . . ? N3 Cu1 Cl1 118.88(8) . . ? N2 Cu1 Cl1 109.43(8) . . ? N3 Cu1 Cl2 127.42(9) . . ? N2 Cu1 Cl2 129.95(8) . . ? Cl1 Cu1 Cl2 92.16(3) . . ? Cu1 Cl2 Cu1 85.99(5) 2_556 . ? Cu1 Cl1 Cu1 89.68(5) . 2_556 ? C1 N1 C4 110.5(3) . . ? C1 N1 H1N 125.0 . . ? C4 N1 H1N 124.5 . . ? C5 N2 C6 119.0(3) . . ? C5 N2 Cu1 136.2(2) . . ? C6 N2 Cu1 103.8(2) . . ? C12 N3 C11 119.1(3) . . ? C12 N3 Cu1 136.0(3) . . ? C11 N3 Cu1 104.3(2) . . ? C16 N4 C13 110.2(3) . . ? C16 N4 H4N 124.8 . . ? C13 N4 H4N 125.0 . . ? N1 C1 C2 107.8(3) . . ? N1 C1 C17 121.3(3) . 2_556 ? C2 C1 C17 130.9(3) . 2_556 ? C1 C2 C3 108.1(3) . . ? C1 C2 C18 126.1(4) . . ? C3 C2 C18 125.7(4) . . ? C4 C3 C2 107.1(3) . . ? C4 C3 C20 126.6(3) . . ? C2 C3 C20 126.3(3) . . ? N1 C4 C5 124.4(3) . . ? N1 C4 C3 106.5(3) . . ? C5 C4 C3 129.1(4) . . ? N2 C5 C4 123.4(3) . . ? N2 C5 H5 118.6 . . ? C4 C5 H5 118.1 . . ? C7 C6 C11 120.2(3) . . ? C7 C6 N2 124.3(3) . . ? C11 C6 N2 115.5(3) . . ? C6 C7 C8 119.6(4) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 120.6 . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.9(3) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 120.4(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 119.5 . . ? C10 C11 C6 119.1(4) . . ? C10 C11 N3 122.4(3) . . ? C6 C11 N3 118.4(3) . . ? N3 C12 C13 125.8(3) . . ? N3 C12 H12 116.8 . . ? C13 C12 H12 117.4 . . ? N4 C13 C14 106.7(3) . . ? N4 C13 C12 122.9(3) . . ? C14 C13 C12 130.4(4) . . ? C13 C14 C15 107.4(3) . . ? C13 C14 C21 126.4(4) . . ? C15 C14 C21 126.2(4) . . ? C16 C15 C14 108.1(3) . . ? C16 C15 C22 125.1(4) . . ? C14 C15 C22 126.5(3) . . ? N4 C16 C15 107.6(3) . . ? N4 C16 C17 120.9(3) . . ? C15 C16 C17 131.5(3) . . ? C16 C17 C1 112.4(3) . 2_556 ? C16 C17 H17A 118.2 . . ? C1 C17 H17A 104.5 2_556 . ? C16 C17 H17B 116.5 . . ? C1 C17 H17B 103.0 2_556 . ? H17A C17 H17B 100.3 . . ? C19A C18 C19 106.8(8) . . ? C19A C18 C2 123.8(7) . . ? C19 C18 C2 124.9(6) . . ? C19A C18 H18C 109.5 . . ? C19 C18 H18C 26.7 . . ? C2 C18 H18C 107.9 . . ? C19A C18 H18D 101.6 . . ? C19 C18 H18D 81.5 . . ? C2 C18 H18D 106.0 . . ? H18C C18 H18D 106.7 . . ? C19A C18 H18A 77.7 . . ? C19 C18 H18A 105.0 . . ? C2 C18 H18A 105.7 . . ? H18C C18 H18A 131.7 . . ? H18D C18 H18A 29.6 . . ? C19A C18 H18B 30.1 . . ? C19 C18 H18B 106.4 . . ? C2 C18 H18B 107.0 . . ? H18C C18 H18B 95.5 . . ? H18D C18 H18B 131.7 . . ? H18A C18 H18B 106.6 . . ? C18 C19 C19A 36.1(4) . . ? C18 C19 H18C 47.8 . . ? C19A C19 H18C 62.2 . . ? C18 C19 H18D 40.6 . . ? C19A C19 H18D 56.7 . . ? H18C C19 H18D 86.7 . . ? C18 C19 H19A 111.4 . . ? C19A C19 H19A 78.2 . . ? H18C C19 H19A 129.6 . . ? H18D C19 H19A 97.0 . . ? C18 C19 H19B 109.2 . . ? C19A C19 H19B 136.5 . . ? H18C C19 H19B 120.5 . . ? H18D C19 H19B 79.8 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 107.8 . . ? C19A C19 H19C 107.5 . . ? H18C C19 H19C 60.2 . . ? H18D C19 H19C 146.1 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C19A C19 37.1(4) . . ? C18 C19A H18A 42.7 . . ? C19 C19A H18A 60.0 . . ? C18 C19A H18B 51.0 . . ? C19 C19A H18B 62.0 . . ? H18A C19A H18B 92.5 . . ? C18 C19A H19D 111.6 . . ? C19 C19A H19D 77.8 . . ? H18A C19A H19D 97.1 . . ? H18B C19A H19D 126.0 . . ? C18 C19A H19E 104.2 . . ? C19 C19A H19E 102.8 . . ? H18A C19A H19E 144.8 . . ? H18B C19A H19E 53.2 . . ? H19D C19A H19E 109.5 . . ? C18 C19A H19F 112.4 . . ? C19 C19A H19F 141.5 . . ? H18A C19A H19F 81.5 . . ? H18B C19A H19F 124.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C3 C20 H20A 109.4 . . ? C3 C20 H20B 110.1 . . ? H20A C20 H20B 109.5 . . ? C3 C20 H20C 109.0 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C21 H21A 110.6 . . ? C14 C21 H21B 108.3 . . ? H21A C21 H21B 109.5 . . ? C14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C22 C23 111.1(4) . . ? C15 C22 H22A 109.6 . . ? C23 C22 H22A 109.2 . . ? C15 C22 H22B 109.7 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 108.2 . . ? C22 C23 H23A 110.8 . . ? C22 C23 H23B 108.7 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 108.9 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 Cl2 Cu1 -129.60(10) . . . 2_556 ? N2 Cu1 Cl2 Cu1 117.77(10) . . . 2_556 ? Cl1 Cu1 Cl2 Cu1 0.0 . . . 2_556 ? N3 Cu1 Cl1 Cu1 135.67(10) . . . 2_556 ? N2 Cu1 Cl1 Cu1 -134.00(8) . . . 2_556 ? Cl2 Cu1 Cl1 Cu1 0.0 . . . 2_556 ? N3 Cu1 N2 C5 -157.4(3) . . . . ? Cl1 Cu1 N2 C5 85.0(3) . . . . ? Cl2 Cu1 N2 C5 -25.4(4) . . . . ? N3 Cu1 N2 C6 34.41(19) . . . . ? Cl1 Cu1 N2 C6 -83.16(19) . . . . ? Cl2 Cu1 N2 C6 166.50(16) . . . . ? N2 Cu1 N3 C12 137.0(4) . . . . ? Cl1 Cu1 N3 C12 -115.7(3) . . . . ? Cl2 Cu1 N3 C12 2.8(4) . . . . ? N2 Cu1 N3 C11 -33.6(2) . . . . ? Cl1 Cu1 N3 C11 73.7(2) . . . . ? Cl2 Cu1 N3 C11 -167.86(17) . . . . ? C4 N1 C1 C2 0.8(4) . . . . ? C4 N1 C1 C17 179.1(3) . . . 2_556 ? N1 C1 C2 C3 0.1(5) . . . . ? C17 C1 C2 C3 -178.0(4) 2_556 . . . ? N1 C1 C2 C18 177.4(4) . . . . ? C17 C1 C2 C18 -0.7(7) 2_556 . . . ? C1 C2 C3 C4 -0.9(5) . . . . ? C18 C2 C3 C4 -178.2(4) . . . . ? C1 C2 C3 C20 177.4(4) . . . . ? C18 C2 C3 C20 0.1(7) . . . . ? C1 N1 C4 C5 178.1(3) . . . . ? C1 N1 C4 C3 -1.3(4) . . . . ? C2 C3 C4 N1 1.4(4) . . . . ? C20 C3 C4 N1 -177.0(4) . . . . ? C2 C3 C4 C5 -178.0(4) . . . . ? C20 C3 C4 C5 3.6(7) . . . . ? C6 N2 C5 C4 -177.4(3) . . . . ? Cu1 N2 C5 C4 15.8(5) . . . . ? N1 C4 C5 N2 5.7(6) . . . . ? C3 C4 C5 N2 -175.0(4) . . . . ? C5 N2 C6 C7 -20.5(5) . . . . ? Cu1 N2 C6 C7 150.2(3) . . . . ? C5 N2 C6 C11 160.0(3) . . . . ? Cu1 N2 C6 C11 -29.3(3) . . . . ? C11 C6 C7 C8 -0.4(5) . . . . ? N2 C6 C7 C8 -179.8(3) . . . . ? C6 C7 C8 C9 1.5(6) . . . . ? C7 C8 C9 C10 -1.6(6) . . . . ? C8 C9 C10 C11 0.6(6) . . . . ? C9 C10 C11 C6 0.5(5) . . . . ? C9 C10 C11 N3 177.8(3) . . . . ? C7 C6 C11 C10 -0.6(5) . . . . ? N2 C6 C11 C10 178.9(3) . . . . ? C7 C6 C11 N3 -178.0(3) . . . . ? N2 C6 C11 N3 1.5(5) . . . . ? C12 N3 C11 C10 37.7(5) . . . . ? Cu1 N3 C11 C10 -149.7(3) . . . . ? C12 N3 C11 C6 -144.9(3) . . . . ? Cu1 N3 C11 C6 27.6(4) . . . . ? C11 N3 C12 C13 -176.7(3) . . . . ? Cu1 N3 C12 C13 13.7(6) . . . . ? C16 N4 C13 C14 0.4(4) . . . . ? C16 N4 C13 C12 -177.5(3) . . . . ? N3 C12 C13 N4 4.6(6) . . . . ? N3 C12 C13 C14 -172.7(4) . . . . ? N4 C13 C14 C15 -0.1(4) . . . . ? C12 C13 C14 C15 177.5(4) . . . . ? N4 C13 C14 C21 -179.5(4) . . . . ? C12 C13 C14 C21 -1.8(7) . . . . ? C13 C14 C15 C16 -0.2(4) . . . . ? C21 C14 C15 C16 179.2(4) . . . . ? C13 C14 C15 C22 -174.7(4) . . . . ? C21 C14 C15 C22 4.7(7) . . . . ? C13 N4 C16 C15 -0.5(4) . . . . ? C13 N4 C16 C17 -179.6(3) . . . . ? C14 C15 C16 N4 0.4(4) . . . . ? C22 C15 C16 N4 175.0(4) . . . . ? C14 C15 C16 C17 179.4(4) . . . . ? C22 C15 C16 C17 -6.0(7) . . . . ? N4 C16 C17 C1 60.0(5) . . . 2_556 ? C15 C16 C17 C1 -118.9(5) . . . 2_556 ? C1 C2 C18 C19A -95.8(10) . . . . ? C3 C2 C18 C19A 81.0(10) . . . . ? C1 C2 C18 C19 111.3(8) . . . . ? C3 C2 C18 C19 -71.9(9) . . . . ? C2 C18 C19 C19A 156.6(12) . . . . ? C2 C18 C19A C19 -157.0(11) . . . . ? C16 C15 C22 C23 -84.5(5) . . . . ? C14 C15 C22 C23 89.1(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4N Cl2 0.90 2.53 3.298(2) 144 . N1 H1N Cl2 0.90 2.47 3.326(2) 159 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.480 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.095 #===END data_complex3' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34.50 H39 Cl3 Cu1.50 N6 O4.50' _chemical_formula_weight 811.38 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8840(2) _cell_length_b 13.3000(2) _cell_length_c 23.9560(4) _cell_angle_alpha 89.0440(6) _cell_angle_beta 76.4860(6) _cell_angle_gamma 68.3240(6) _cell_volume 3698.11(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _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 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1674 _exptl_absorpt_coefficient_mu 1.135 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22885 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.1296 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 16275 _reflns_number_gt 9119 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0200P)^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 16275 _refine_ls_number_parameters 932 _refine_ls_number_restraints 613 _refine_ls_R_factor_all 0.1679 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.1932 _refine_ls_wR_factor_gt 0.1706 _refine_ls_goodness_of_fit_ref 1.906 _refine_ls_restrained_S_all 1.946 _refine_ls_shift/su_max 0.717 _refine_ls_shift/su_mean 0.016 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 0.72366(6) 0.67179(6) 0.65529(4) 0.0246(2) Uani 1 1 d U . . Cu2 Cu 0.81334(7) 0.51128(6) 0.79259(4) 0.0263(2) Uani 1 1 d U . . N1 N 0.7067(4) 0.6363(4) 0.5822(2) 0.0261(13) Uani 1 1 d U . . N2 N 0.8902(4) 0.6145(4) 0.6149(2) 0.0245(13) Uani 1 1 d U . . N3 N 0.9215(4) 0.4971(4) 0.7126(2) 0.0246(13) Uani 1 1 d U . . N4 N 0.8224(4) 0.3725(4) 0.7677(2) 0.0277(14) Uani 1 1 d U . . N5 N 0.7242(4) 0.4914(4) 0.8637(2) 0.0282(14) Uani 1 1 d U . . N6 N 0.7731(4) 0.6561(4) 0.8307(2) 0.0270(13) Uani 1 1 d U . . N7 N 0.7022(4) 0.7451(4) 0.7325(2) 0.0273(14) Uani 1 1 d U . . N8 N 0.5641(4) 0.7045(4) 0.6827(2) 0.0233(13) Uani 1 1 d U . . C1 C 0.6191(5) 0.6405(5) 0.5593(3) 0.0238(15) Uani 1 1 d U . . C2 C 0.6626(6) 0.6163(5) 0.4993(3) 0.0365(19) Uani 1 1 d U . . H2A H 0.6187 0.6138 0.4724 0.044 Uiso 1 1 d R . . C3 C 0.7809(6) 0.5948(5) 0.4858(3) 0.0317(17) Uani 1 1 d U . . H3A H 0.8341 0.5751 0.4486 0.038 Uiso 1 1 d R . . C4 C 0.8071(5) 0.6089(5) 0.5384(3) 0.0255(16) Uani 1 1 d U . . C5 C 0.9055(5) 0.5987(5) 0.5593(3) 0.0266(16) Uani 1 1 d U . . H5A H 0.9805 0.5798 0.5337 0.032 Uiso 1 1 d R . . C6 C 0.9826(5) 0.6080(5) 0.6390(3) 0.0223(15) Uani 1 1 d U . . C7 C 1.0574(6) 0.6600(6) 0.6151(3) 0.0338(18) Uani 1 1 d U . . H7A H 1.0517 0.6948 0.5800 0.041 Uiso 1 1 d R . . C8 C 1.1422(6) 0.6592(6) 0.6432(3) 0.0366(19) Uani 1 1 d U . . H8A H 1.1950 0.6936 0.6271 0.044 Uiso 1 1 d R . . C9 C 1.1497(6) 0.6096(6) 0.6935(3) 0.0377(19) Uani 1 1 d U . . H9A H 1.2067 0.6110 0.7128 0.045 Uiso 1 1 d R . . C10 C 1.0745(5) 0.5602(5) 0.7175(3) 0.0304(17) Uani 1 1 d U . . H10A H 1.0797 0.5259 0.7529 0.036 Uiso 1 1 d R . . C11 C 0.9926(5) 0.5553(5) 0.6887(3) 0.0244(16) Uani 1 1 d U . . C12 C 0.9345(5) 0.4077(5) 0.6839(3) 0.0266(16) Uani 1 1 d U . . H12A H 0.9795 0.3901 0.6448 0.032 Uiso 1 1 d R . . C13 C 0.8799(5) 0.3399(5) 0.7108(3) 0.0270(16) Uani 1 1 d U . . C14 C 0.8781(6) 0.2381(5) 0.6989(3) 0.0386(19) Uani 1 1 d U . . H14A H 0.9132 0.1948 0.6629 0.046 Uiso 1 1 d R . . C15 C 0.8180(6) 0.2120(5) 0.7493(3) 0.0362(19) Uani 1 1 d U . . H15A H 0.8011 0.1475 0.7546 0.043 Uiso 1 1 d R . . C16 C 0.7835(6) 0.2959(5) 0.7914(3) 0.0307(17) Uani 1 1 d U . . C17 C 0.7247(6) 0.3026(5) 0.8546(3) 0.0322(18) Uani 1 1 d U . . C18 C 0.6937(5) 0.4125(5) 0.8876(3) 0.0303(17) Uani 1 1 d U . . C19 C 0.6363(6) 0.4441(6) 0.9453(3) 0.0373(19) Uani 1 1 d U . . H19A H 0.6063 0.4007 0.9717 0.045 Uiso 1 1 d R . . C20 C 0.6330(6) 0.5476(6) 0.9565(3) 0.042(2) Uani 1 1 d U . . H20A H 0.5973 0.5918 0.9923 0.050 Uiso 1 1 d R . . C21 C 0.6903(6) 0.5760(5) 0.9058(3) 0.0292(17) Uani 1 1 d U . . C22 C 0.7192(6) 0.6627(5) 0.8850(3) 0.0339(18) Uani 1 1 d U . . H22A H 0.6981 0.7270 0.9095 0.041 Uiso 1 1 d R . . C23 C 0.8090(6) 0.7387(5) 0.8065(3) 0.0279(17) Uani 1 1 d U . . C24 C 0.8801(6) 0.7756(5) 0.8290(3) 0.0344(18) Uani 1 1 d U . . H24A H 0.8980 0.7516 0.8649 0.041 Uiso 1 1 d R . . C25 C 0.9250(6) 0.8473(6) 0.7990(4) 0.042(2) Uani 1 1 d U . . H25A H 0.9745 0.8721 0.8144 0.051 Uiso 1 1 d R . . C26 C 0.8996(6) 0.8818(5) 0.7480(3) 0.0371(19) Uani 1 1 d U . . H26A H 0.9314 0.9311 0.7281 0.044 Uiso 1 1 d R . . C27 C 0.8269(6) 0.8461(5) 0.7248(3) 0.0316(17) Uani 1 1 d U . . H27A H 0.8104 0.8684 0.6885 0.038 Uiso 1 1 d R . . C28 C 0.7801(5) 0.7760(5) 0.7556(3) 0.0264(16) Uani 1 1 d U . . C29 C 0.5965(5) 0.7685(5) 0.7633(3) 0.0230(15) Uani 1 1 d U . . H29A H 0.5746 0.7992 0.8023 0.028 Uiso 1 1 d R . . C30 C 0.5163(6) 0.7481(5) 0.7379(3) 0.0305(17) Uani 1 1 d U . . C31 C 0.3978(5) 0.7766(5) 0.7502(3) 0.0270(16) Uani 1 1 d U . . H31A H 0.3435 0.8091 0.7861 0.032 Uiso 1 1 d R . . C32 C 0.3743(6) 0.7490(5) 0.7004(3) 0.0330(18) Uani 1 1 d U . . H32A H 0.2993 0.7586 0.6957 0.040 Uiso 1 1 d R . . C33 C 0.4791(5) 0.7042(5) 0.6582(3) 0.0260(16) Uani 1 1 d U . . C34 C 0.4980(5) 0.6618(5) 0.5960(3) 0.0290(17) Uani 1 1 d U . . C35 C 0.8108(6) 0.2165(6) 0.8818(4) 0.049(2) Uani 1 1 d U . . H35A H 0.8327 0.1465 0.8624 0.073 Uiso 1 1 d R . . H35B H 0.8779 0.2341 0.8781 0.073 Uiso 1 1 d R . . H35C H 0.7765 0.2152 0.9218 0.073 Uiso 1 1 d R . . C36 C 0.6177(6) 0.2744(6) 0.8621(4) 0.046(2) Uani 1 1 d U . . H36A H 0.5616 0.3270 0.8455 0.070 Uiso 1 1 d R . . H36B H 0.6394 0.2038 0.8434 0.070 Uiso 1 1 d R . . H36C H 0.5853 0.2739 0.9025 0.070 Uiso 1 1 d R . . C37 C 0.4116(6) 0.7464(6) 0.5686(3) 0.041(2) Uani 1 1 d U . . H37A H 0.4250 0.8129 0.5677 0.062 Uiso 1 1 d R . . H37B H 0.4218 0.7194 0.5300 0.062 Uiso 1 1 d R . . H37C H 0.3344 0.7597 0.5902 0.062 Uiso 1 1 d R . . C38 C 0.4795(6) 0.5541(5) 0.5976(3) 0.0382(19) Uani 1 1 d U . . H38A H 0.4898 0.5256 0.5593 0.057 Uiso 1 1 d R . . H38B H 0.5349 0.5036 0.6154 0.057 Uiso 1 1 d R . . H38C H 0.4031 0.5655 0.6197 0.057 Uiso 1 1 d R . . Cu1' Cu 0.31051(7) 0.32270(6) 0.75506(4) 0.0291(2) Uani 1 1 d U . . Cu2' Cu 0.32207(6) 0.02062(6) 0.79828(3) 0.0240(2) Uani 1 1 d U . . N1' N 0.1877(4) 0.3987(4) 0.8188(3) 0.0290(14) Uani 1 1 d U . . N2' N 0.1956(4) 0.2609(4) 0.7425(2) 0.0256(13) Uani 1 1 d U . . N3' N 0.1894(4) 0.0524(4) 0.7621(2) 0.0252(13) Uani 1 1 d U . . N4' N 0.2227(4) -0.0219(4) 0.8590(2) 0.0247(13) Uani 1 1 d U . . N5' N 0.4189(4) -0.0021(4) 0.8497(2) 0.0253(13) Uani 1 1 d U . . N6' N 0.4517(4) 0.0523(4) 0.7435(2) 0.0237(13) Uani 1 1 d U . . N7' N 0.4618(5) 0.2494(4) 0.6988(3) 0.0315(14) Uani 1 1 d U . . N8' N 0.3850(5) 0.4143(4) 0.7709(3) 0.0343(15) Uani 1 1 d U . . C1' C 0.1647(6) 0.4828(5) 0.8567(3) 0.0323(18) Uani 1 1 d U . . C2' C 0.0528(6) 0.5085(5) 0.8910(3) 0.0379(19) Uani 1 1 d U . . H2'A H 0.0143 0.5653 0.9214 0.045 Uiso 1 1 d R . . C3' C 0.0086(6) 0.4399(5) 0.8730(3) 0.0327(18) Uani 1 1 d U . . H3'A H -0.0660 0.4376 0.8892 0.039 Uiso 1 1 d R . . C4' C 0.0924(6) 0.3727(5) 0.8281(3) 0.0305(17) Uani 1 1 d U . . C5' C 0.1019(5) 0.2956(5) 0.7848(3) 0.0265(16) Uani 1 1 d U . . H5'A H 0.0408 0.2700 0.7863 0.032 Uiso 1 1 d R . . C6' C 0.2015(5) 0.1911(5) 0.6968(3) 0.0273(16) Uani 1 1 d U . . C7' C 0.2170(6) 0.2225(6) 0.6405(3) 0.0348(18) Uani 1 1 d U . . H7'A H 0.2268 0.2899 0.6329 0.042 Uiso 1 1 d R . . C8' C 0.2205(6) 0.1572(6) 0.5957(4) 0.046(2) Uani 1 1 d U . . H8'A H 0.2354 0.1784 0.5571 0.055 Uiso 1 1 d R . . C9' C 0.1999(6) 0.0627(6) 0.6057(3) 0.044(2) Uani 1 1 d U . . H9'A H 0.1962 0.0204 0.5747 0.052 Uiso 1 1 d R . . C10' C 0.1860(5) 0.0293(6) 0.6614(3) 0.0326(18) Uani 1 1 d U . . H10B H 0.1758 -0.0382 0.6686 0.039 Uiso 1 1 d R . . C11' C 0.1878(5) 0.0908(5) 0.7068(3) 0.0286(17) Uani 1 1 d U . . C12' C 0.1048(6) 0.0295(5) 0.7938(3) 0.0272(16) Uani 1 1 d U . . H12B H 0.0369 0.0387 0.7809 0.033 Uiso 1 1 d R . . C13' C 0.1190(5) -0.0098(5) 0.8487(3) 0.0254(16) Uani 1 1 d U . . C14' C 0.0539(6) -0.0380(5) 0.8979(3) 0.0300(17) Uani 1 1 d U . . H14B H -0.0224 -0.0377 0.9033 0.036 Uiso 1 1 d R . . C15' C 0.1200(6) -0.0641(5) 0.9369(3) 0.0323(18) Uani 1 1 d U . . H15B H 0.0993 -0.0861 0.9749 0.039 Uiso 1 1 d R . . C16' C 0.2259(5) -0.0547(5) 0.9110(3) 0.0238(16) Uani 1 1 d U . . C17' C 0.3338(5) -0.0830(5) 0.9354(3) 0.0250(16) Uani 1 1 d U . . C18' C 0.4213(5) -0.0408(5) 0.9019(3) 0.0252(16) Uani 1 1 d U . . C19' C 0.5236(6) -0.0447(5) 0.9152(3) 0.0312(17) Uani 1 1 d U . . H19B H 0.5479 -0.0700 0.9496 0.037 Uiso 1 1 d R . . C20' C 0.5827(6) -0.0055(5) 0.8692(3) 0.0317(18) Uani 1 1 d U . . H20B H 0.6550 0.0024 0.8658 0.038 Uiso 1 1 d R . . C21' C 0.5167(5) 0.0209(5) 0.8288(3) 0.0249(16) Uani 1 1 d U . . C22' C 0.5298(6) 0.0480(5) 0.7712(3) 0.0266(16) Uani 1 1 d U . . H22B H 0.5944 0.0664 0.7528 0.032 Uiso 1 1 d R . . C23' C 0.4794(5) 0.0649(5) 0.6830(3) 0.0290(17) Uani 1 1 d U . . C24' C 0.4959(6) -0.0220(6) 0.6453(3) 0.0353(18) Uani 1 1 d U . . H24B H 0.4868 -0.0860 0.6609 0.042 Uiso 1 1 d R . . C25' C 0.5270(6) -0.0190(6) 0.5874(3) 0.044(2) Uani 1 1 d U . . H25B H 0.5370 -0.0789 0.5622 0.053 Uiso 1 1 d R . . C26' C 0.5410(6) 0.0735(6) 0.5653(3) 0.044(2) Uani 1 1 d U . . H26B H 0.5669 0.0741 0.5244 0.053 Uiso 1 1 d R . . C27' C 0.5204(6) 0.1622(6) 0.6005(3) 0.0390(19) Uani 1 1 d U . . H27B H 0.5265 0.2269 0.5843 0.047 Uiso 1 1 d R . . C28' C 0.4896(6) 0.1587(5) 0.6594(3) 0.0304(17) Uani 1 1 d U . . C29' C 0.5285(6) 0.3025(5) 0.6958(3) 0.0340(18) Uani 1 1 d U . . H29B H 0.6013 0.2797 0.6680 0.041 Uiso 1 1 d R . . C30' C 0.4900(6) 0.3941(5) 0.7352(3) 0.0351(18) Uani 1 1 d U . . C31' C 0.5358(6) 0.4665(6) 0.7541(4) 0.041(2) Uani 1 1 d U . . H31B H 0.6097 0.4699 0.7375 0.049 Uiso 1 1 d R . . C32' C 0.4548(6) 0.5288(6) 0.7990(4) 0.042(2) Uani 1 1 d U . . H32B H 0.4599 0.5870 0.8199 0.051 Uiso 1 1 d R . . C33' C 0.3612(6) 0.4964(5) 0.8111(3) 0.0351(18) Uani 1 1 d U . . C34' C 0.2501(6) 0.5372(5) 0.8589(3) 0.0356(18) Uani 1 1 d U . . C35' C 0.3891(6) -0.2085(5) 0.9318(3) 0.0338(18) Uani 1 1 d U . . H35D H 0.4572 -0.2303 0.9462 0.051 Uiso 1 1 d R . . H35E H 0.3349 -0.2355 0.9549 0.051 Uiso 1 1 d R . . H35F H 0.4092 -0.2375 0.8926 0.051 Uiso 1 1 d R . . C36' C 0.2976(6) -0.0421(6) 0.9990(3) 0.0382(19) Uani 1 1 d U . . H36D H 0.2632 0.0357 1.0027 0.057 Uiso 1 1 d R . . H36E H 0.2430 -0.0711 1.0197 0.057 Uiso 1 1 d R . . H36F H 0.3643 -0.0656 1.0145 0.057 Uiso 1 1 d R . . C37' C 0.2827(7) 0.5181(6) 0.9165(4) 0.053(2) Uani 1 1 d U . . H37D H 0.3202 0.4416 0.9190 0.080 Uiso 1 1 d R . . H37E H 0.3340 0.5538 0.9193 0.080 Uiso 1 1 d R . . H37F H 0.2145 0.5465 0.9473 0.080 Uiso 1 1 d R . . C38' C 0.1885(6) 0.6604(5) 0.8560(4) 0.043(2) Uani 1 1 d U . . H38D H 0.1185 0.6880 0.8859 0.064 Uiso 1 1 d R . . H38E H 0.2385 0.6964 0.8607 0.064 Uiso 1 1 d R . . H38F H 0.1709 0.6733 0.8191 0.064 Uiso 1 1 d R . . Cl1A Cl 0.8195(3) -0.1256(3) 0.56048(18) 0.1346(14) Uani 1 1 d U . . Cl2A Cl 0.9496(6) -0.0158(4) 0.5937(3) 0.218(3) Uani 1 1 d U . . C1A C 0.8441(13) -0.0074(11) 0.5604(8) 0.146(5) Uani 1 1 d U . . Cl1B Cl 0.95003(16) 0.28764(17) 0.54909(9) 0.0494(5) Uani 1 1 d U . . Cl2B Cl 0.7349(2) 0.2837(2) 0.53507(14) 0.0904(10) Uani 1 1 d U . . C1B C 0.7985(7) 0.3566(6) 0.5672(4) 0.049(2) Uiso 1 1 d . . . Cl1C Cl 0.3161(4) 0.2296(3) 0.9624(2) 0.0756(8) Uiso 0.608(4) 1 d PD A 1 Cl2C Cl 0.0792(4) 0.2402(3) 0.9988(2) 0.0756(8) Uiso 0.608(4) 1 d PD A 1 Cl1D Cl 0.2443(6) 0.2694(5) 0.9892(3) 0.0756(8) Uiso 0.392(4) 1 d PD A 2 Cl2D Cl 0.0400(5) 0.2370(5) 0.9774(3) 0.0756(8) Uiso 0.392(4) 1 d PD A 2 C1C C 0.1852(5) 0.2383(7) 0.9358(4) 0.071(3) Uiso 1 1 d D A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0230(4) 0.0329(5) 0.0218(5) -0.0018(4) -0.0053(4) -0.0148(4) Cu2 0.0308(5) 0.0276(5) 0.0237(5) 0.0021(4) -0.0050(4) -0.0156(4) N1 0.021(3) 0.040(3) 0.021(3) -0.001(3) -0.008(2) -0.014(2) N2 0.030(3) 0.030(3) 0.018(3) -0.002(3) -0.004(2) -0.017(2) N3 0.024(3) 0.031(3) 0.028(3) 0.003(3) -0.012(2) -0.017(2) N4 0.023(3) 0.029(3) 0.032(4) 0.006(3) -0.008(3) -0.010(2) N5 0.031(3) 0.030(3) 0.026(3) 0.003(3) 0.000(3) -0.018(3) N6 0.033(3) 0.027(3) 0.021(3) -0.002(3) -0.003(3) -0.014(3) N7 0.032(3) 0.026(3) 0.025(3) 0.002(3) -0.006(3) -0.013(3) N8 0.020(3) 0.030(3) 0.023(3) -0.001(3) -0.012(2) -0.009(2) C1 0.028(3) 0.026(3) 0.024(4) 0.004(3) -0.016(3) -0.013(3) C2 0.042(4) 0.040(4) 0.031(4) 0.000(3) -0.017(3) -0.014(3) C3 0.033(4) 0.037(4) 0.024(4) -0.004(3) -0.004(3) -0.014(3) C4 0.028(3) 0.030(4) 0.020(4) -0.004(3) -0.002(3) -0.014(3) C5 0.023(3) 0.032(4) 0.028(4) 0.003(3) -0.007(3) -0.013(3) C6 0.011(3) 0.034(4) 0.027(4) 0.002(3) -0.010(3) -0.011(3) C7 0.036(4) 0.048(4) 0.025(4) 0.007(3) -0.011(3) -0.023(3) C8 0.030(4) 0.044(4) 0.046(5) 0.012(4) -0.009(3) -0.025(3) C9 0.038(4) 0.046(4) 0.041(5) 0.006(4) -0.016(3) -0.025(3) C10 0.028(4) 0.032(4) 0.035(4) 0.006(3) -0.013(3) -0.012(3) C11 0.015(3) 0.029(3) 0.027(4) 0.003(3) -0.002(3) -0.007(3) C12 0.028(3) 0.031(4) 0.021(4) -0.002(3) -0.004(3) -0.012(3) C13 0.032(4) 0.023(3) 0.028(4) 0.000(3) -0.007(3) -0.012(3) C14 0.044(4) 0.031(4) 0.037(5) 0.002(3) -0.009(4) -0.010(3) C15 0.044(4) 0.029(4) 0.040(5) 0.001(3) -0.011(4) -0.017(3) C16 0.029(4) 0.027(4) 0.038(4) 0.004(3) -0.008(3) -0.013(3) C17 0.029(4) 0.027(4) 0.043(5) 0.015(3) -0.010(3) -0.013(3) C18 0.027(4) 0.034(4) 0.027(4) 0.005(3) -0.003(3) -0.010(3) C19 0.039(4) 0.045(4) 0.029(4) 0.012(4) -0.005(3) -0.020(3) C20 0.050(4) 0.040(4) 0.028(4) 0.005(4) -0.005(4) -0.012(4) C21 0.034(4) 0.035(4) 0.020(4) -0.002(3) -0.010(3) -0.012(3) C22 0.039(4) 0.032(4) 0.029(4) -0.005(3) -0.008(3) -0.011(3) C23 0.035(4) 0.026(3) 0.023(4) -0.003(3) -0.003(3) -0.015(3) C24 0.045(4) 0.035(4) 0.031(4) -0.006(3) -0.011(3) -0.021(3) C25 0.041(4) 0.041(4) 0.050(5) -0.001(4) -0.011(4) -0.020(3) C26 0.044(4) 0.033(4) 0.043(5) 0.000(3) -0.009(4) -0.026(3) C27 0.036(4) 0.029(4) 0.032(4) 0.000(3) -0.009(3) -0.014(3) C28 0.031(4) 0.024(3) 0.029(4) -0.003(3) -0.010(3) -0.014(3) C29 0.030(4) 0.022(3) 0.017(4) 0.000(3) -0.005(3) -0.011(3) C30 0.031(4) 0.022(3) 0.032(4) 0.001(3) 0.002(3) -0.007(3) C31 0.024(3) 0.027(3) 0.030(4) -0.005(3) 0.000(3) -0.013(3) C32 0.021(3) 0.030(4) 0.042(5) 0.002(3) -0.003(3) -0.006(3) C33 0.021(3) 0.024(3) 0.035(4) 0.004(3) -0.009(3) -0.009(3) C34 0.026(3) 0.034(4) 0.032(4) 0.000(3) -0.011(3) -0.014(3) C35 0.052(5) 0.043(4) 0.047(5) 0.013(4) -0.012(4) -0.013(4) C36 0.040(4) 0.043(4) 0.059(5) 0.005(4) 0.000(4) -0.027(4) C37 0.031(4) 0.050(4) 0.043(5) 0.008(4) -0.010(3) -0.015(3) C38 0.042(4) 0.049(4) 0.034(4) -0.005(3) -0.004(3) -0.032(4) Cu1' 0.0317(5) 0.0324(5) 0.0322(5) 0.0066(4) -0.0138(4) -0.0189(4) Cu2' 0.0263(4) 0.0299(5) 0.0216(5) 0.0036(4) -0.0085(4) -0.0156(4) N1' 0.024(3) 0.030(3) 0.040(4) 0.012(3) -0.017(3) -0.012(2) N2' 0.032(3) 0.026(3) 0.026(3) 0.005(3) -0.014(3) -0.015(2) N3' 0.029(3) 0.029(3) 0.023(3) 0.003(3) -0.009(3) -0.014(2) N4' 0.024(3) 0.024(3) 0.026(3) 0.001(3) -0.001(2) -0.012(2) N5' 0.028(3) 0.021(3) 0.026(3) 0.003(3) -0.002(3) -0.011(2) N6' 0.029(3) 0.033(3) 0.020(3) 0.002(2) -0.017(3) -0.018(2) N7' 0.032(3) 0.036(3) 0.038(4) 0.016(3) -0.012(3) -0.024(3) N8' 0.040(3) 0.036(3) 0.040(4) 0.006(3) -0.019(3) -0.025(3) C1' 0.045(4) 0.020(3) 0.038(4) 0.002(3) -0.020(4) -0.012(3) C2' 0.037(4) 0.030(4) 0.045(5) -0.006(3) -0.012(4) -0.010(3) C3' 0.027(4) 0.035(4) 0.037(4) 0.005(3) -0.011(3) -0.011(3) C4' 0.033(4) 0.027(4) 0.037(4) 0.008(3) -0.014(3) -0.014(3) C5' 0.023(3) 0.030(4) 0.033(4) 0.009(3) -0.014(3) -0.014(3) C6' 0.026(3) 0.035(4) 0.026(4) 0.005(3) -0.015(3) -0.012(3) C7' 0.034(4) 0.044(4) 0.033(4) 0.012(4) -0.017(3) -0.017(3) C8' 0.048(4) 0.054(5) 0.036(5) 0.008(4) -0.009(4) -0.020(4) C9' 0.050(4) 0.051(5) 0.034(5) 0.000(4) -0.013(4) -0.021(4) C10' 0.030(4) 0.038(4) 0.037(4) 0.007(3) -0.019(3) -0.016(3) C11' 0.021(3) 0.039(4) 0.032(4) 0.008(3) -0.014(3) -0.013(3) C12' 0.027(4) 0.027(3) 0.027(4) 0.003(3) -0.009(3) -0.008(3) C13' 0.022(3) 0.031(4) 0.028(4) -0.003(3) -0.004(3) -0.016(3) C14' 0.025(3) 0.035(4) 0.032(4) 0.002(3) -0.006(3) -0.013(3) C15' 0.038(4) 0.029(4) 0.028(4) 0.005(3) -0.001(3) -0.016(3) C16' 0.031(4) 0.019(3) 0.020(4) 0.001(3) -0.001(3) -0.011(3) C17' 0.026(3) 0.032(4) 0.021(4) 0.004(3) -0.011(3) -0.012(3) C18' 0.029(4) 0.021(3) 0.026(4) -0.001(3) -0.006(3) -0.011(3) C19' 0.045(4) 0.027(4) 0.031(4) 0.003(3) -0.018(3) -0.019(3) C20' 0.032(4) 0.033(4) 0.036(4) -0.002(3) -0.013(3) -0.017(3) C21' 0.027(3) 0.024(3) 0.027(4) 0.004(3) -0.009(3) -0.012(3) C22' 0.032(4) 0.020(3) 0.029(4) -0.001(3) -0.001(3) -0.015(3) C23' 0.026(3) 0.035(4) 0.025(4) 0.001(3) 0.000(3) -0.014(3) C24' 0.042(4) 0.042(4) 0.027(4) 0.004(3) -0.006(3) -0.024(3) C25' 0.049(4) 0.061(5) 0.036(5) 0.000(4) -0.013(4) -0.033(4) C26' 0.053(5) 0.067(5) 0.024(4) 0.010(4) -0.011(4) -0.034(4) C27' 0.038(4) 0.052(4) 0.032(4) 0.012(4) -0.007(3) -0.024(4) C28' 0.030(4) 0.035(4) 0.032(4) 0.003(3) -0.007(3) -0.018(3) C29' 0.034(4) 0.039(4) 0.036(4) 0.016(3) -0.013(3) -0.019(3) C30' 0.037(4) 0.036(4) 0.044(5) 0.005(3) -0.012(3) -0.026(3) C31' 0.034(4) 0.040(4) 0.066(5) 0.025(4) -0.032(4) -0.022(3) C32' 0.048(4) 0.031(4) 0.056(5) 0.002(4) -0.018(4) -0.021(4) C33' 0.040(4) 0.028(4) 0.048(5) 0.006(3) -0.026(4) -0.015(3) C34' 0.044(4) 0.030(4) 0.040(4) 0.003(3) -0.022(4) -0.014(3) C35' 0.041(4) 0.033(4) 0.034(4) 0.003(3) -0.018(3) -0.015(3) C36' 0.053(4) 0.043(4) 0.026(4) 0.000(3) -0.009(3) -0.028(4) C37' 0.072(5) 0.060(5) 0.051(5) 0.002(4) -0.032(4) -0.042(4) C38' 0.047(4) 0.033(4) 0.052(5) 0.002(4) -0.018(4) -0.014(3) Cl1A 0.121(3) 0.153(3) 0.119(3) -0.010(2) -0.040(2) -0.032(2) Cl2A 0.320(6) 0.190(4) 0.226(6) 0.030(4) -0.109(5) -0.163(4) C1A 0.161(9) 0.130(8) 0.202(11) 0.001(7) -0.107(8) -0.078(7) Cl1B 0.0459(11) 0.0639(13) 0.0413(13) 0.0040(10) -0.0106(10) -0.0239(10) Cl2B 0.0682(16) 0.0992(19) 0.120(3) -0.0326(18) -0.0274(16) -0.0456(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 Cu1 N8 1.888(5) . ? Cu1 N1 1.904(5) . ? Cu1 N2 1.992(5) . ? Cu1 N7 2.018(5) . ? Cu2 N5 1.893(5) . ? Cu2 N4 1.902(5) . ? Cu2 N6 1.978(5) . ? Cu2 N3 2.053(5) . ? N1 C1 1.348(8) . ? N1 C4 1.391(8) . ? N2 C5 1.308(8) . ? N2 C6 1.415(8) . ? N3 C12 1.320(8) . ? N3 C11 1.425(8) . ? N4 C16 1.355(8) . ? N4 C13 1.381(8) . ? N5 C18 1.329(8) . ? N5 C21 1.393(8) . ? N6 C22 1.311(8) . ? N6 C23 1.408(8) . ? N7 C29 1.311(8) . ? N7 C28 1.433(8) . ? N8 C33 1.361(8) . ? N8 C30 1.358(8) . ? C1 C2 1.410(9) . ? C1 C34 1.525(9) . ? C2 C3 1.399(9) . ? C2 H2A 0.9600 . ? C3 C4 1.413(9) . ? C3 H3A 0.9600 . ? C4 C5 1.429(9) . ? C5 H5A 0.9600 . ? C6 C11 1.380(9) . ? C6 C7 1.397(9) . ? C7 C8 1.407(10) . ? C7 H7A 0.9599 . ? C8 C9 1.370(10) . ? C8 H8A 0.9601 . ? C9 C10 1.378(9) . ? C9 H9A 0.9600 . ? C10 C11 1.410(9) . ? C10 H10A 0.9599 . ? C12 C13 1.402(9) . ? C12 H12A 0.9600 . ? C13 C14 1.398(9) . ? C14 C15 1.389(10) . ? C14 H14A 0.9598 . ? C15 C16 1.386(9) . ? C15 H15A 0.9601 . ? C16 C17 1.513(10) . ? C17 C36 1.529(9) . ? C17 C35 1.530(10) . ? C17 C18 1.543(9) . ? C18 C19 1.395(10) . ? C19 C20 1.391(10) . ? C19 H19A 0.9601 . ? C20 C21 1.392(10) . ? C20 H20A 0.9601 . ? C21 C22 1.389(9) . ? C22 H22A 0.9601 . ? C23 C24 1.394(9) . ? C23 C28 1.390(10) . ? C24 C25 1.397(10) . ? C24 H24A 0.9600 . ? C25 C26 1.366(11) . ? C25 H25A 0.9600 . ? C26 C27 1.413(9) . ? C26 H26A 0.9600 . ? C27 C28 1.399(9) . ? C27 H27A 0.9600 . ? C29 C30 1.420(9) . ? C29 H29A 0.9600 . ? C30 C31 1.389(9) . ? C31 C32 1.383(10) . ? C31 H31A 0.9600 . ? C32 C33 1.411(9) . ? C32 H32A 0.9600 . ? C33 C34 1.533(10) . ? C34 C37 1.526(10) . ? C34 C38 1.535(9) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9599 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9601 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9602 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? Cu1' N8' 1.897(5) . ? Cu1' N1' 1.897(5) . ? Cu1' N7' 1.995(5) . ? Cu1' N2' 2.018(5) . ? Cu2' N5' 1.894(6) . ? Cu2' N4' 1.926(5) . ? Cu2' N3' 1.999(5) . ? Cu2' N6' 2.041(5) . ? N1' C1' 1.351(8) . ? N1' C4' 1.364(8) . ? N2' C5' 1.315(8) . ? N2' C6' 1.418(8) . ? N3' C12' 1.307(8) . ? N3' C11' 1.413(9) . ? N4' C16' 1.318(8) . ? N4' C13' 1.366(8) . ? N5' C18' 1.348(9) . ? N5' C21' 1.384(8) . ? N6' C22' 1.313(8) . ? N6' C23' 1.432(8) . ? N7' C29' 1.288(8) . ? N7' C28' 1.427(8) . ? N8' C30' 1.353(8) . ? N8' C33' 1.366(9) . ? C1' C2' 1.401(9) . ? C1' C34' 1.534(9) . ? C2' C3' 1.362(9) . ? C2' H2'A 0.9600 . ? C3' C4' 1.378(9) . ? C3' H3'A 0.9600 . ? C4' C5' 1.423(9) . ? C5' H5'A 0.9601 . ? C6' C7' 1.395(10) . ? C6' C11' 1.419(9) . ? C7' C8' 1.374(10) . ? C7' H7'A 0.9600 . ? C8' C9' 1.384(10) . ? C8' H8'A 0.9600 . ? C9' C10' 1.393(10) . ? C9' H9'A 0.9599 . ? C10' C11' 1.382(9) . ? C10' H10B 0.9600 . ? C12' C13' 1.433(10) . ? C12' H12B 0.9600 . ? C13' C14' 1.410(9) . ? C14' C15' 1.366(10) . ? C14' H14B 0.9600 . ? C15' C16' 1.410(9) . ? C15' H15B 0.9599 . ? C16' C17' 1.550(9) . ? C17' C18' 1.504(9) . ? C17' C36' 1.530(9) . ? C17' C35' 1.548(8) . ? C18' C19' 1.408(9) . ? C19' C20' 1.397(9) . ? C19' H19B 0.9601 . ? C20' C21' 1.391(9) . ? C20' H20B 0.9600 . ? C21' C22' 1.408(9) . ? C22' H22B 0.9600 . ? C23' C24' 1.400(9) . ? C23' C28' 1.399(9) . ? C24' C25' 1.354(10) . ? C24' H24B 0.9599 . ? C25' C26' 1.387(10) . ? C25' H25B 0.9601 . ? C26' C27' 1.368(10) . ? C26' H26B 0.9599 . ? C27' C28' 1.379(10) . ? C27' H27B 0.9601 . ? C29' C30' 1.412(10) . ? C29' H29B 0.9601 . ? C30' C31' 1.428(9) . ? C31' C32' 1.341(10) . ? C31' H31B 0.9600 . ? C32' C33' 1.393(9) . ? C32' H32B 0.9598 . ? C33' C34' 1.529(10) . ? C34' C37' 1.523(11) . ? C34' C38' 1.543(9) . ? C35' H35D 0.9600 . ? C35' H35E 0.9601 . ? C35' H35F 0.9599 . ? C36' H36D 0.9599 . ? C36' H36E 0.9601 . ? C36' H36F 0.9599 . ? C37' H37D 0.9601 . ? C37' H37E 0.9600 . ? C37' H37F 0.9600 . ? C38' H38D 0.9599 . ? C38' H38E 0.9600 . ? C38' H38F 0.9599 . ? Cl1A C1A 1.714(14) . ? Cl2A C1A 1.701(14) . ? Cl1B C1B 1.770(8) . ? Cl2B C1B 1.765(8) . ? Cl1D C1C 1.759(9) . ? Cl2D C1C 1.909(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 N8 Cu1 N1 86.7(2) . . ? N8 Cu1 N2 167.8(2) . . ? N1 Cu1 N2 82.8(2) . . ? N8 Cu1 N7 82.2(2) . . ? N1 Cu1 N7 164.2(2) . . ? N2 Cu1 N7 109.3(2) . . ? N5 Cu2 N4 85.7(2) . . ? N5 Cu2 N6 82.7(2) . . ? N4 Cu2 N6 167.4(2) . . ? N5 Cu2 N3 167.6(2) . . ? N4 Cu2 N3 82.6(2) . . ? N6 Cu2 N3 109.3(2) . . ? C1 N1 C4 109.2(5) . . ? C1 N1 Cu1 136.6(4) . . ? C4 N1 Cu1 113.8(4) . . ? C5 N2 C6 121.2(5) . . ? C5 N2 Cu1 111.6(4) . . ? C6 N2 Cu1 126.4(4) . . ? C12 N3 C11 118.3(5) . . ? C12 N3 Cu2 109.3(4) . . ? C11 N3 Cu2 131.7(4) . . ? C16 N4 C13 109.5(5) . . ? C16 N4 Cu2 136.2(5) . . ? C13 N4 Cu2 114.3(4) . . ? C18 N5 C21 108.3(6) . . ? C18 N5 Cu2 137.2(5) . . ? C21 N5 Cu2 114.0(4) . . ? C22 N6 C23 122.3(6) . . ? C22 N6 Cu2 111.3(4) . . ? C23 N6 Cu2 125.9(4) . . ? C29 N7 C28 119.2(5) . . ? C29 N7 Cu1 110.1(4) . . ? C28 N7 Cu1 130.6(4) . . ? C33 N8 C30 108.9(5) . . ? C33 N8 Cu1 134.5(5) . . ? C30 N8 Cu1 116.3(5) . . ? N1 C1 C2 108.1(6) . . ? N1 C1 C34 122.7(6) . . ? C2 C1 C34 129.2(6) . . ? C3 C2 C1 108.6(7) . . ? C3 C2 H2A 125.8 . . ? C1 C2 H2A 125.6 . . ? C2 C3 C4 105.8(6) . . ? C2 C3 H3A 127.9 . . ? C4 C3 H3A 126.3 . . ? N1 C4 C3 108.4(5) . . ? N1 C4 C5 112.8(6) . . ? C3 C4 C5 138.7(6) . . ? N2 C5 C4 117.6(6) . . ? N2 C5 H5A 121.0 . . ? C4 C5 H5A 121.4 . . ? C11 C6 C7 120.7(6) . . ? C11 C6 N2 118.4(6) . . ? C7 C6 N2 120.7(6) . . ? C6 C7 C8 118.9(7) . . ? C6 C7 H7A 120.5 . . ? C8 C7 H7A 120.5 . . ? C9 C8 C7 120.2(7) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 120.8(7) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C9 C10 C11 119.9(7) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 119.5 . . ? C6 C11 C10 119.3(6) . . ? C6 C11 N3 122.2(6) . . ? C10 C11 N3 118.5(6) . . ? N3 C12 C13 119.0(6) . . ? N3 C12 H12A 120.6 . . ? C13 C12 H12A 120.4 . . ? N4 C13 C12 114.2(6) . . ? N4 C13 C14 107.7(6) . . ? C12 C13 C14 137.5(6) . . ? C15 C14 C13 106.5(6) . . ? C15 C14 H14A 127.3 . . ? C13 C14 H14A 126.2 . . ? C16 C15 C14 108.9(6) . . ? C16 C15 H15A 124.8 . . ? C14 C15 H15A 126.3 . . ? N4 C16 C15 107.5(6) . . ? N4 C16 C17 122.9(6) . . ? C15 C16 C17 129.3(6) . . ? C16 C17 C36 110.6(6) . . ? C16 C17 C35 106.3(5) . . ? C36 C17 C35 108.0(6) . . ? C16 C17 C18 114.5(5) . . ? C36 C17 C18 110.2(5) . . ? C35 C17 C18 107.0(6) . . ? N5 C18 C19 109.6(6) . . ? N5 C18 C17 122.6(6) . . ? C19 C18 C17 127.7(6) . . ? C20 C19 C18 107.2(6) . . ? C20 C19 H19A 127.6 . . ? C18 C19 H19A 125.2 . . ? C21 C20 C19 106.9(6) . . ? C21 C20 H20A 126.3 . . ? C19 C20 H20A 126.8 . . ? C22 C21 C20 139.2(7) . . ? C22 C21 N5 112.8(6) . . ? C20 C21 N5 108.0(6) . . ? N6 C22 C21 118.6(6) . . ? N6 C22 H22A 120.6 . . ? C21 C22 H22A 120.8 . . ? C24 C23 C28 120.0(6) . . ? C24 C23 N6 122.1(7) . . ? C28 C23 N6 117.6(6) . . ? C23 C24 C25 119.5(7) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.5 . . ? C26 C25 C24 120.8(7) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.4 . . ? C25 C26 C27 120.6(7) . . ? C25 C26 H26A 119.4 . . ? C27 C26 H26A 120.1 . . ? C28 C27 C26 118.6(7) . . ? C28 C27 H27A 120.4 . . ? C26 C27 H27A 121.0 . . ? C27 C28 C23 120.5(6) . . ? C27 C28 N7 117.6(6) . . ? C23 C28 N7 121.9(6) . . ? N7 C29 C30 118.9(6) . . ? N7 C29 H29A 119.9 . . ? C30 C29 H29A 121.2 . . ? N8 C30 C31 109.6(7) . . ? N8 C30 C29 112.2(6) . . ? C31 C30 C29 137.1(6) . . ? C32 C31 C30 106.1(6) . . ? C32 C31 H31A 127.3 . . ? C30 C31 H31A 126.6 . . ? C31 C32 C33 108.4(6) . . ? C31 C32 H32A 125.6 . . ? C33 C32 H32A 126.0 . . ? N8 C33 C32 107.0(6) . . ? N8 C33 C34 124.9(5) . . ? C32 C33 C34 128.1(6) . . ? C37 C34 C33 108.3(5) . . ? C37 C34 C1 108.4(6) . . ? C33 C34 C1 113.2(5) . . ? C37 C34 C38 111.0(6) . . ? C33 C34 C38 108.2(6) . . ? C1 C34 C38 107.8(5) . . ? C17 C35 H35A 109.7 . . ? C17 C35 H35B 108.9 . . ? H35A C35 H35B 109.5 . . ? C17 C35 H35C 109.8 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C17 C36 H36A 110.2 . . ? C17 C36 H36B 109.1 . . ? H36A C36 H36B 109.5 . . ? C17 C36 H36C 109.1 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.7 . . ? C34 C37 H37B 108.6 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 110.1 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 110.5 . . ? C34 C38 H38B 108.3 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.6 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N8' Cu1' N1' 87.2(2) . . ? N8' Cu1' N7' 81.8(2) . . ? N1' Cu1' N7' 166.8(2) . . ? N8' Cu1' N2' 165.4(2) . . ? N1' Cu1' N2' 82.0(2) . . ? N7' Cu1' N2' 110.1(2) . . ? N5' Cu2' N4' 85.5(2) . . ? N5' Cu2' N3' 165.8(2) . . ? N4' Cu2' N3' 81.9(2) . . ? N5' Cu2' N6' 83.1(2) . . ? N4' Cu2' N6' 168.3(2) . . ? N3' Cu2' N6' 109.7(2) . . ? C1' N1' C4' 107.9(5) . . ? C1' N1' Cu1' 135.4(5) . . ? C4' N1' Cu1' 116.4(5) . . ? C5' N2' C6' 118.8(5) . . ? C5' N2' Cu1' 110.7(4) . . ? C6' N2' Cu1' 130.5(4) . . ? C12' N3' C11' 122.6(6) . . ? C12' N3' Cu2' 113.1(5) . . ? C11' N3' Cu2' 124.2(4) . . ? C16' N4' C13' 109.5(5) . . ? C16' N4' Cu2' 135.9(5) . . ? C13' N4' Cu2' 114.4(5) . . ? C18' N5' C21' 108.8(6) . . ? C18' N5' Cu2' 136.5(5) . . ? C21' N5' Cu2' 114.6(5) . . ? C22' N6' C23' 116.6(6) . . ? C22' N6' Cu2' 108.8(4) . . ? C23' N6' Cu2' 134.2(4) . . ? C29' N7' C28' 121.9(6) . . ? C29' N7' Cu1' 112.0(5) . . ? C28' N7' Cu1' 125.4(4) . . ? C30' N8' C33' 109.2(6) . . ? C30' N8' Cu1' 114.6(5) . . ? C33' N8' Cu1' 136.1(5) . . ? N1' C1' C2' 107.9(6) . . ? N1' C1' C34' 123.7(6) . . ? C2' C1' C34' 128.5(6) . . ? C3' C2' C1' 108.0(6) . . ? C3' C2' H2'A 126.5 . . ? C1' C2' H2'A 125.5 . . ? C2' C3' C4' 106.9(6) . . ? C2' C3' H3'A 126.5 . . ? C4' C3' H3'A 126.6 . . ? N1' C4' C3' 109.3(6) . . ? N1' C4' C5' 112.1(6) . . ? C3' C4' C5' 137.9(7) . . ? N2' C5' C4' 118.6(6) . . ? N2' C5' H5'A 120.8 . . ? C4' C5' H5'A 120.6 . . ? C7' C6' C11' 118.5(7) . . ? C7' C6' N2' 119.9(6) . . ? C11' C6' N2' 121.6(6) . . ? C8' C7' C6' 120.9(7) . . ? C8' C7' H7'A 119.5 . . ? C6' C7' H7'A 119.6 . . ? C7' C8' C9' 120.9(8) . . ? C7' C8' H8'A 119.7 . . ? C9' C8' H8'A 119.4 . . ? C8' C9' C10' 118.8(7) . . ? C8' C9' H9'A 120.6 . . ? C10' C9' H9'A 120.5 . . ? C11' C10' C9' 121.3(7) . . ? C11' C10' H10B 119.1 . . ? C9' C10' H10B 119.7 . . ? C10' C11' N3' 122.5(6) . . ? C10' C11' C6' 119.4(7) . . ? N3' C11' C6' 117.8(6) . . ? N3' C12' C13' 116.4(6) . . ? N3' C12' H12B 121.7 . . ? C13' C12' H12B 122.0 . . ? N4' C13' C14' 107.8(6) . . ? N4' C13' C12' 114.1(6) . . ? C14' C13' C12' 138.0(6) . . ? C15' C14' C13' 106.5(6) . . ? C15' C14' H14B 126.5 . . ? C13' C14' H14B 127.0 . . ? C14' C15' C16' 107.6(7) . . ? C14' C15' H15B 126.5 . . ? C16' C15' H15B 125.8 . . ? N4' C16' C15' 108.6(6) . . ? N4' C16' C17' 123.2(6) . . ? C15' C16' C17' 128.2(6) . . ? C18' C17' C36' 110.8(6) . . ? C18' C17' C16' 113.3(6) . . ? C36' C17' C16' 109.9(5) . . ? C18' C17' C35' 108.7(5) . . ? C36' C17' C35' 107.8(6) . . ? C16' C17' C35' 106.1(5) . . ? N5' C18' C19' 108.4(6) . . ? N5' C18' C17' 123.6(6) . . ? C19' C18' C17' 127.6(6) . . ? C20' C19' C18' 107.3(6) . . ? C20' C19' H19B 126.5 . . ? C18' C19' H19B 126.2 . . ? C21' C20' C19' 107.0(6) . . ? C21' C20' H20B 126.1 . . ? C19' C20' H20B 127.0 . . ? N5' C21' C20' 108.5(6) . . ? N5' C21' C22' 113.0(6) . . ? C20' C21' C22' 137.6(7) . . ? N6' C22' C21' 120.2(6) . . ? N6' C22' H22B 120.1 . . ? C21' C22' H22B 119.7 . . ? C24' C23' C28' 118.1(7) . . ? C24' C23' N6' 117.7(6) . . ? C28' C23' N6' 124.1(6) . . ? C25' C24' C23' 121.7(7) . . ? C25' C24' H24B 119.2 . . ? C23' C24' H24B 119.0 . . ? C24' C25' C26' 118.8(7) . . ? C24' C25' H25B 120.7 . . ? C26' C25' H25B 120.5 . . ? C27' C26' C25' 121.4(7) . . ? C27' C26' H26B 119.8 . . ? C25' C26' H26B 118.7 . . ? C28' C27' C26' 119.6(7) . . ? C28' C27' H27B 120.1 . . ? C26' C27' H27B 120.2 . . ? C27' C28' C23' 120.2(6) . . ? C27' C28' N7' 122.9(6) . . ? C23' C28' N7' 116.9(6) . . ? N7' C29' C30' 117.2(6) . . ? N7' C29' H29B 120.7 . . ? C30' C29' H29B 122.0 . . ? N8' C30' C29' 113.8(6) . . ? N8' C30' C31' 107.6(6) . . ? C29' C30' C31' 138.0(7) . . ? C32' C31' C30' 106.4(7) . . ? C32' C31' H31B 127.1 . . ? C30' C31' H31B 126.5 . . ? C31' C32' C33' 109.8(7) . . ? C31' C32' H32B 125.7 . . ? C33' C32' H32B 124.6 . . ? N8' C33' C32' 106.9(6) . . ? N8' C33' C34' 122.5(6) . . ? C32' C33' C34' 130.6(6) . . ? C37' C34' C33' 108.0(6) . . ? C37' C34' C1' 108.4(6) . . ? C33' C34' C1' 115.0(6) . . ? C37' C34' C38' 108.4(6) . . ? C33' C34' C38' 108.8(6) . . ? C1' C34' C38' 108.1(6) . . ? C17' C35' H35D 109.3 . . ? C17' C35' H35E 108.9 . . ? H35D C35' H35E 109.5 . . ? C17' C35' H35F 110.2 . . ? H35D C35' H35F 109.5 . . ? H35E C35' H35F 109.5 . . ? C17' C36' H36D 109.8 . . ? C17' C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C17' C36' H36F 109.2 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C34' C37' H37D 109.2 . . ? C34' C37' H37E 109.7 . . ? H37D C37' H37E 109.5 . . ? C34' C37' H37F 109.6 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? C34' C38' H38D 110.4 . . ? C34' C38' H38E 109.2 . . ? H38D C38' H38E 109.5 . . ? C34' C38' H38F 108.9 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? Cl2A C1A Cl1A 112.3(9) . . ? Cl2B C1B Cl1B 109.6(4) . . ? Cl1D C1C Cl2D 104.2(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 Cu1 N1 C1 4.4(7) . . . . ? N2 Cu1 N1 C1 178.2(7) . . . . ? N7 Cu1 N1 C1 -40.9(12) . . . . ? N8 Cu1 N1 C4 176.1(5) . . . . ? N2 Cu1 N1 C4 -10.0(4) . . . . ? N7 Cu1 N1 C4 130.9(8) . . . . ? N8 Cu1 N2 C5 41.0(13) . . . . ? N1 Cu1 N2 C5 10.3(4) . . . . ? N7 Cu1 N2 C5 -159.2(4) . . . . ? N8 Cu1 N2 C6 -149.5(10) . . . . ? N1 Cu1 N2 C6 179.8(5) . . . . ? N7 Cu1 N2 C6 10.3(6) . . . . ? N5 Cu2 N3 C12 24.1(13) . . . . ? N4 Cu2 N3 C12 5.0(4) . . . . ? N6 Cu2 N3 C12 -170.7(4) . . . . ? N5 Cu2 N3 C11 -145.6(10) . . . . ? N4 Cu2 N3 C11 -164.8(6) . . . . ? N6 Cu2 N3 C11 19.6(6) . . . . ? N5 Cu2 N4 C16 -1.0(7) . . . . ? N6 Cu2 N4 C16 -24.4(15) . . . . ? N3 Cu2 N4 C16 175.0(7) . . . . ? N5 Cu2 N4 C13 176.9(5) . . . . ? N6 Cu2 N4 C13 153.5(10) . . . . ? N3 Cu2 N4 C13 -7.2(5) . . . . ? N4 Cu2 N5 C18 7.1(7) . . . . ? N6 Cu2 N5 C18 -177.9(7) . . . . ? N3 Cu2 N5 C18 -12.0(16) . . . . ? N4 Cu2 N5 C21 178.0(5) . . . . ? N6 Cu2 N5 C21 -7.0(5) . . . . ? N3 Cu2 N5 C21 158.9(9) . . . . ? N5 Cu2 N6 C22 6.8(5) . . . . ? N4 Cu2 N6 C22 30.3(14) . . . . ? N3 Cu2 N6 C22 -170.1(5) . . . . ? N5 Cu2 N6 C23 179.0(6) . . . . ? N4 Cu2 N6 C23 -157.5(10) . . . . ? N3 Cu2 N6 C23 2.2(6) . . . . ? N8 Cu1 N7 C29 5.4(4) . . . . ? N1 Cu1 N7 C29 51.1(10) . . . . ? N2 Cu1 N7 C29 -170.4(4) . . . . ? N8 Cu1 N7 C28 -172.2(6) . . . . ? N1 Cu1 N7 C28 -126.5(8) . . . . ? N2 Cu1 N7 C28 12.0(6) . . . . ? N1 Cu1 N8 C33 -1.7(6) . . . . ? N2 Cu1 N8 C33 -32.2(15) . . . . ? N7 Cu1 N8 C33 167.0(6) . . . . ? N1 Cu1 N8 C30 -174.3(5) . . . . ? N2 Cu1 N8 C30 155.3(10) . . . . ? N7 Cu1 N8 C30 -5.5(5) . . . . ? C4 N1 C1 C2 -0.5(7) . . . . ? Cu1 N1 C1 C2 171.5(5) . . . . ? C4 N1 C1 C34 176.3(6) . . . . ? Cu1 N1 C1 C34 -11.7(10) . . . . ? N1 C1 C2 C3 1.1(8) . . . . ? C34 C1 C2 C3 -175.4(6) . . . . ? C1 C2 C3 C4 -1.3(8) . . . . ? C1 N1 C4 C3 -0.4(7) . . . . ? Cu1 N1 C4 C3 -174.4(4) . . . . ? C1 N1 C4 C5 -177.8(5) . . . . ? Cu1 N1 C4 C5 8.2(7) . . . . ? C2 C3 C4 N1 1.1(7) . . . . ? C2 C3 C4 C5 177.5(8) . . . . ? C6 N2 C5 C4 -178.8(6) . . . . ? Cu1 N2 C5 C4 -8.7(7) . . . . ? N1 C4 C5 N2 0.7(8) . . . . ? C3 C4 C5 N2 -175.6(7) . . . . ? C5 N2 C6 C11 -137.6(6) . . . . ? Cu1 N2 C6 C11 53.9(7) . . . . ? C5 N2 C6 C7 46.6(8) . . . . ? Cu1 N2 C6 C7 -121.9(6) . . . . ? C11 C6 C7 C8 -1.0(10) . . . . ? N2 C6 C7 C8 174.7(6) . . . . ? C6 C7 C8 C9 -1.0(10) . . . . ? C7 C8 C9 C10 -0.3(11) . . . . ? C8 C9 C10 C11 3.4(10) . . . . ? C7 C6 C11 C10 4.1(9) . . . . ? N2 C6 C11 C10 -171.7(5) . . . . ? C7 C6 C11 N3 -176.9(5) . . . . ? N2 C6 C11 N3 7.3(9) . . . . ? C9 C10 C11 C6 -5.3(9) . . . . ? C9 C10 C11 N3 175.7(6) . . . . ? C12 N3 C11 C6 67.6(8) . . . . ? Cu2 N3 C11 C6 -123.4(6) . . . . ? C12 N3 C11 C10 -113.4(7) . . . . ? Cu2 N3 C11 C10 55.6(8) . . . . ? C11 N3 C12 C13 169.4(6) . . . . ? Cu2 N3 C12 C13 -1.9(8) . . . . ? C16 N4 C13 C12 -173.4(6) . . . . ? Cu2 N4 C13 C12 8.2(8) . . . . ? C16 N4 C13 C14 -0.8(8) . . . . ? Cu2 N4 C13 C14 -179.2(5) . . . . ? N3 C12 C13 N4 -3.9(9) . . . . ? N3 C12 C13 C14 -173.4(8) . . . . ? N4 C13 C14 C15 0.5(8) . . . . ? C12 C13 C14 C15 170.5(8) . . . . ? C13 C14 C15 C16 0.0(9) . . . . ? C13 N4 C16 C15 0.8(8) . . . . ? Cu2 N4 C16 C15 178.7(5) . . . . ? C13 N4 C16 C17 175.2(6) . . . . ? Cu2 N4 C16 C17 -6.9(11) . . . . ? C14 C15 C16 N4 -0.5(8) . . . . ? C14 C15 C16 C17 -174.4(7) . . . . ? N4 C16 C17 C36 135.2(7) . . . . ? C15 C16 C17 C36 -51.7(10) . . . . ? N4 C16 C17 C35 -107.8(7) . . . . ? C15 C16 C17 C35 65.3(10) . . . . ? N4 C16 C17 C18 10.1(10) . . . . ? C15 C16 C17 C18 -176.9(7) . . . . ? C21 N5 C18 C19 1.7(8) . . . . ? Cu2 N5 C18 C19 172.9(6) . . . . ? C21 N5 C18 C17 -175.9(6) . . . . ? Cu2 N5 C18 C17 -4.7(11) . . . . ? C16 C17 C18 N5 -5.1(10) . . . . ? C36 C17 C18 N5 -130.5(7) . . . . ? C35 C17 C18 N5 112.3(7) . . . . ? C16 C17 C18 C19 177.8(7) . . . . ? C36 C17 C18 C19 52.4(10) . . . . ? C35 C17 C18 C19 -64.7(9) . . . . ? N5 C18 C19 C20 -0.3(9) . . . . ? C17 C18 C19 C20 177.0(7) . . . . ? C18 C19 C20 C21 -1.1(9) . . . . ? C19 C20 C21 C22 179.3(9) . . . . ? C19 C20 C21 N5 2.1(8) . . . . ? C18 N5 C21 C22 179.6(6) . . . . ? Cu2 N5 C21 C22 6.1(8) . . . . ? C18 N5 C21 C20 -2.3(8) . . . . ? Cu2 N5 C21 C20 -175.8(5) . . . . ? C23 N6 C22 C21 -177.9(6) . . . . ? Cu2 N6 C22 C21 -5.3(8) . . . . ? C20 C21 C22 N6 -177.4(8) . . . . ? N5 C21 C22 N6 -0.3(9) . . . . ? C22 N6 C23 C24 55.9(9) . . . . ? Cu2 N6 C23 C24 -115.6(6) . . . . ? C22 N6 C23 C28 -130.1(7) . . . . ? Cu2 N6 C23 C28 58.4(8) . . . . ? C28 C23 C24 C25 -2.2(10) . . . . ? N6 C23 C24 C25 171.7(6) . . . . ? C23 C24 C25 C26 0.2(10) . . . . ? C24 C25 C26 C27 0.4(11) . . . . ? C25 C26 C27 C28 0.9(10) . . . . ? C26 C27 C28 C23 -2.9(9) . . . . ? C26 C27 C28 N7 177.1(5) . . . . ? C24 C23 C28 C27 3.5(9) . . . . ? N6 C23 C28 C27 -170.6(5) . . . . ? C24 C23 C28 N7 -176.4(6) . . . . ? N6 C23 C28 N7 9.5(9) . . . . ? C29 N7 C28 C27 -120.1(7) . . . . ? Cu1 N7 C28 C27 57.3(8) . . . . ? C29 N7 C28 C23 59.8(8) . . . . ? Cu1 N7 C28 C23 -122.7(6) . . . . ? C28 N7 C29 C30 173.3(6) . . . . ? Cu1 N7 C29 C30 -4.6(7) . . . . ? C33 N8 C30 C31 0.3(8) . . . . ? Cu1 N8 C30 C31 174.7(4) . . . . ? C33 N8 C30 C29 -169.9(5) . . . . ? Cu1 N8 C30 C29 4.5(7) . . . . ? N7 C29 C30 N8 0.4(9) . . . . ? N7 C29 C30 C31 -166.0(8) . . . . ? N8 C30 C31 C32 -0.1(8) . . . . ? C29 C30 C31 C32 166.6(8) . . . . ? C30 C31 C32 C33 -0.2(8) . . . . ? C30 N8 C33 C32 -0.5(7) . . . . ? Cu1 N8 C33 C32 -173.4(5) . . . . ? C30 N8 C33 C34 179.7(6) . . . . ? Cu1 N8 C33 C34 6.8(10) . . . . ? C31 C32 C33 N8 0.4(7) . . . . ? C31 C32 C33 C34 -179.8(6) . . . . ? N8 C33 C34 C37 -132.1(6) . . . . ? C32 C33 C34 C37 48.1(9) . . . . ? N8 C33 C34 C1 -11.9(9) . . . . ? C32 C33 C34 C1 168.4(6) . . . . ? N8 C33 C34 C38 107.5(7) . . . . ? C32 C33 C34 C38 -72.3(8) . . . . ? N1 C1 C34 C37 133.9(6) . . . . ? C2 C1 C34 C37 -50.0(9) . . . . ? N1 C1 C34 C33 13.8(9) . . . . ? C2 C1 C34 C33 -170.2(6) . . . . ? N1 C1 C34 C38 -105.8(7) . . . . ? C2 C1 C34 C38 70.2(9) . . . . ? N8' Cu1' N1' C1' 1.8(7) . . . . ? N7' Cu1' N1' C1' 34.8(14) . . . . ? N2' Cu1' N1' C1' -168.4(7) . . . . ? N8' Cu1' N1' C4' 174.6(5) . . . . ? N7' Cu1' N1' C4' -152.4(9) . . . . ? N2' Cu1' N1' C4' 4.4(5) . . . . ? N8' Cu1' N2' C5' -47.0(12) . . . . ? N1' Cu1' N2' C5' -4.7(5) . . . . ? N7' Cu1' N2' C5' 169.8(4) . . . . ? N8' Cu1' N2' C6' 131.9(9) . . . . ? N1' Cu1' N2' C6' 174.2(6) . . . . ? N7' Cu1' N2' C6' -11.3(6) . . . . ? N5' Cu2' N3' C12' -29.0(11) . . . . ? N4' Cu2' N3' C12' -1.0(4) . . . . ? N6' Cu2' N3' C12' 177.2(4) . . . . ? N5' Cu2' N3' C11' 153.9(8) . . . . ? N4' Cu2' N3' C11' -178.0(5) . . . . ? N6' Cu2' N3' C11' 0.2(5) . . . . ? N5' Cu2' N4' C16' -1.9(6) . . . . ? N3' Cu2' N4' C16' -175.3(6) . . . . ? N6' Cu2' N4' C16' 13.1(14) . . . . ? N5' Cu2' N4' C13' 172.9(4) . . . . ? N3' Cu2' N4' C13' -0.4(4) . . . . ? N6' Cu2' N4' C13' -172.1(8) . . . . ? N4' Cu2' N5' C18' 5.8(6) . . . . ? N3' Cu2' N5' C18' 33.7(12) . . . . ? N6' Cu2' N5' C18' -171.1(6) . . . . ? N4' Cu2' N5' C21' -178.1(4) . . . . ? N3' Cu2' N5' C21' -150.2(8) . . . . ? N6' Cu2' N5' C21' 4.9(4) . . . . ? N5' Cu2' N6' C22' -3.8(4) . . . . ? N4' Cu2' N6' C22' -18.9(12) . . . . ? N3' Cu2' N6' C22' 169.9(4) . . . . ? N5' Cu2' N6' C23' 167.8(6) . . . . ? N4' Cu2' N6' C23' 152.8(9) . . . . ? N3' Cu2' N6' C23' -18.4(6) . . . . ? N8' Cu1' N7' C29' -6.7(5) . . . . ? N1' Cu1' N7' C29' -40.0(12) . . . . ? N2' Cu1' N7' C29' 164.5(5) . . . . ? N8' Cu1' N7' C28' -177.4(6) . . . . ? N1' Cu1' N7' C28' 149.2(9) . . . . ? N2' Cu1' N7' C28' -6.2(6) . . . . ? N1' Cu1' N8' C30' 179.1(5) . . . . ? N7' Cu1' N8' C30' 6.3(5) . . . . ? N2' Cu1' N8' C30' -139.0(9) . . . . ? N1' Cu1' N8' C33' 1.2(7) . . . . ? N7' Cu1' N8' C33' -171.6(8) . . . . ? N2' Cu1' N8' C33' 43.1(14) . . . . ? C4' N1' C1' C2' 1.0(8) . . . . ? Cu1' N1' C1' C2' 174.2(5) . . . . ? C4' N1' C1' C34' -178.6(6) . . . . ? Cu1' N1' C1' C34' -5.3(11) . . . . ? N1' C1' C2' C3' -0.7(9) . . . . ? C34' C1' C2' C3' 178.9(7) . . . . ? C1' C2' C3' C4' 0.1(9) . . . . ? C1' N1' C4' C3' -1.0(8) . . . . ? Cu1' N1' C4' C3' -175.7(5) . . . . ? C1' N1' C4' C5' 171.4(6) . . . . ? Cu1' N1' C4' C5' -3.3(8) . . . . ? C2' C3' C4' N1' 0.6(8) . . . . ? C2' C3' C4' C5' -168.9(9) . . . . ? C6' N2' C5' C4' -174.7(6) . . . . ? Cu1' N2' C5' C4' 4.3(8) . . . . ? N1' C4' C5' N2' -1.0(9) . . . . ? C3' C4' C5' N2' 168.3(8) . . . . ? C5' N2' C6' C7' 120.2(7) . . . . ? Cu1' N2' C6' C7' -58.7(8) . . . . ? C5' N2' C6' C11' -57.5(8) . . . . ? Cu1' N2' C6' C11' 123.6(6) . . . . ? C11' C6' C7' C8' -0.8(10) . . . . ? N2' C6' C7' C8' -178.6(6) . . . . ? C6' C7' C8' C9' 5.0(11) . . . . ? C7' C8' C9' C10' -5.9(11) . . . . ? C8' C9' C10' C11' 2.6(11) . . . . ? C9' C10' C11' N3' -171.4(6) . . . . ? C9' C10' C11' C6' 1.4(10) . . . . ? C12' N3' C11' C10' -63.6(9) . . . . ? Cu2' N3' C11' C10' 113.2(6) . . . . ? C12' N3' C11' C6' 123.5(7) . . . . ? Cu2' N3' C11' C6' -59.7(7) . . . . ? C7' C6' C11' C10' -2.3(9) . . . . ? N2' C6' C11' C10' 175.4(6) . . . . ? C7' C6' C11' N3' 170.8(6) . . . . ? N2' C6' C11' N3' -11.4(9) . . . . ? C11' N3' C12' C13' 179.3(6) . . . . ? Cu2' N3' C12' C13' 2.1(7) . . . . ? C16' N4' C13' C14' -0.5(7) . . . . ? Cu2' N4' C13' C14' -176.7(4) . . . . ? C16' N4' C13' C12' 177.9(5) . . . . ? Cu2' N4' C13' C12' 1.7(7) . . . . ? N3' C12' C13' N4' -2.5(8) . . . . ? N3' C12' C13' C14' 175.1(7) . . . . ? N4' C13' C14' C15' 1.3(7) . . . . ? C12' C13' C14' C15' -176.4(7) . . . . ? C13' C14' C15' C16' -1.6(7) . . . . ? C13' N4' C16' C15' -0.6(7) . . . . ? Cu2' N4' C16' C15' 174.5(4) . . . . ? C13' N4' C16' C17' 176.3(5) . . . . ? Cu2' N4' C16' C17' -8.7(9) . . . . ? C14' C15' C16' N4' 1.4(7) . . . . ? C14' C15' C16' C17' -175.3(6) . . . . ? N4' C16' C17' C18' 16.1(8) . . . . ? C15' C16' C17' C18' -167.6(6) . . . . ? N4' C16' C17' C36' 140.7(6) . . . . ? C15' C16' C17' C36' -43.1(9) . . . . ? N4' C16' C17' C35' -103.1(7) . . . . ? C15' C16' C17' C35' 73.2(8) . . . . ? C21' N5' C18' C19' -0.9(7) . . . . ? Cu2' N5' C18' C19' 175.3(4) . . . . ? C21' N5' C18' C17' -174.7(5) . . . . ? Cu2' N5' C18' C17' 1.5(10) . . . . ? C36' C17' C18' N5' -137.0(6) . . . . ? C16' C17' C18' N5' -12.9(8) . . . . ? C35' C17' C18' N5' 104.8(7) . . . . ? C36' C17' C18' C19' 50.4(8) . . . . ? C16' C17' C18' C19' 174.5(6) . . . . ? C35' C17' C18' C19' -67.8(8) . . . . ? N5' C18' C19' C20' 0.8(7) . . . . ? C17' C18' C19' C20' 174.3(6) . . . . ? C18' C19' C20' C21' -0.3(7) . . . . ? C18' N5' C21' C20' 0.7(7) . . . . ? Cu2' N5' C21' C20' -176.4(4) . . . . ? C18' N5' C21' C22' 172.0(5) . . . . ? Cu2' N5' C21' C22' -5.1(6) . . . . ? C19' C20' C21' N5' -0.2(7) . . . . ? C19' C20' C21' C22' -168.3(7) . . . . ? C23' N6' C22' C21' -171.2(5) . . . . ? Cu2' N6' C22' C21' 2.1(7) . . . . ? N5' C21' C22' N6' 1.8(8) . . . . ? C20' C21' C22' N6' 169.5(7) . . . . ? C22' N6' C23' C24' 112.8(7) . . . . ? Cu2' N6' C23' C24' -58.4(8) . . . . ? C22' N6' C23' C28' -68.0(8) . . . . ? Cu2' N6' C23' C28' 120.9(6) . . . . ? C28' C23' C24' C25' 3.5(11) . . . . ? N6' C23' C24' C25' -177.1(7) . . . . ? C23' C24' C25' C26' -1.1(12) . . . . ? C24' C25' C26' C27' -2.1(12) . . . . ? C25' C26' C27' C28' 2.7(12) . . . . ? C26' C27' C28' C23' -0.1(11) . . . . ? C26' C27' C28' N7' -177.1(7) . . . . ? C24' C23' C28' C27' -2.9(10) . . . . ? N6' C23' C28' C27' 177.8(7) . . . . ? C24' C23' C28' N7' 174.3(6) . . . . ? N6' C23' C28' N7' -5.0(10) . . . . ? C29' N7' C28' C27' -51.0(10) . . . . ? Cu1' N7' C28' C27' 118.9(7) . . . . ? C29' N7' C28' C23' 131.9(7) . . . . ? Cu1' N7' C28' C23' -58.3(8) . . . . ? C28' N7' C29' C30' 177.0(7) . . . . ? Cu1' N7' C29' C30' 5.9(8) . . . . ? C33' N8' C30' C29' 173.4(6) . . . . ? Cu1' N8' C30' C29' -5.1(9) . . . . ? C33' N8' C30' C31' 0.6(9) . . . . ? Cu1' N8' C30' C31' -177.9(5) . . . . ? N7' C29' C30' N8' -0.8(10) . . . . ? N7' C29' C30' C31' 168.9(9) . . . . ? N8' C30' C31' C32' -1.8(9) . . . . ? C29' C30' C31' C32' -172.0(9) . . . . ? C30' C31' C32' C33' 2.3(9) . . . . ? C30' N8' C33' C32' 0.8(9) . . . . ? Cu1' N8' C33' C32' 178.8(6) . . . . ? C30' N8' C33' C34' -178.4(6) . . . . ? Cu1' N8' C33' C34' -0.4(12) . . . . ? C31' C32' C33' N8' -2.0(9) . . . . ? C31' C32' C33' C34' 177.1(7) . . . . ? N8' C33' C34' C37' 118.3(7) . . . . ? C32' C33' C34' C37' -60.7(10) . . . . ? N8' C33' C34' C1' -2.9(10) . . . . ? C32' C33' C34' C1' 178.1(7) . . . . ? N8' C33' C34' C38' -124.3(7) . . . . ? C32' C33' C34' C38' 56.7(10) . . . . ? N1' C1' C34' C37' -115.5(8) . . . . ? C2' C1' C34' C37' 65.0(9) . . . . ? N1' C1' C34' C33' 5.5(10) . . . . ? C2' C1' C34' C33' -174.0(7) . . . . ? N1' C1' C34' C38' 127.2(7) . . . . ? C2' C1' C34' C38' -52.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.739 _refine_diff_density_min -1.798 _refine_diff_density_rms 0.203 #===END