# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wei Huang' _publ_contact_author_address ; Nanjing Jiangsu China 210093 ; _publ_contact_author_email whuang@nju.edu.cn _publ_author_name 'Wei Huang' #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 694303' #TrackingRef '- 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H32 Cu2 N9, 3(Cl O4), C H4 O' _chemical_formula_sum 'C42 H36 Cl3 Cu2 N9 O13' _chemical_formula_weight 1108.23 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3980(15) _cell_length_b 13.738(2) _cell_length_c 19.206(3) _cell_angle_alpha 79.856(2) _cell_angle_beta 82.962(2) _cell_angle_gamma 72.719(2) _cell_volume 2324.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1589 _cell_measurement_theta_min 2.435 _cell_measurement_theta_max 20.401 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8450 _exptl_absorpt_correction_T_max 0.8927 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; The structure was solved by direct methods (Bruker, 2000) and successive difference Fourier syntheses. ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11802 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.1538 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8065 _reflns_number_gt 3911 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0508P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8065 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1403 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 0.834 _refine_ls_restrained_S_all 0.834 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.48295(8) 0.51699(5) 0.26985(4) 0.0323(2) Uani 1 1 d . . . Cu2 Cu 0.11134(9) 0.86550(5) 0.28721(4) 0.0361(2) Uani 1 1 d . . . C5 C 0.5843(7) 0.3863(5) 0.3959(3) 0.0356(15) Uani 1 1 d . . . C4 C 0.6460(7) 0.3549(5) 0.4618(3) 0.0484(18) Uani 1 1 d . . . H4 H 0.6577 0.2878 0.4849 0.058 Uiso 1 1 calc R . . C3 C 0.6886(8) 0.4239(6) 0.4919(4) 0.056(2) Uani 1 1 d . . . H3 H 0.7260 0.4047 0.5365 0.067 Uiso 1 1 calc R . . C2 C 0.6764(7) 0.5210(6) 0.4566(3) 0.0486(18) Uani 1 1 d . . . H2 H 0.7088 0.5677 0.4756 0.058 Uiso 1 1 calc R . . C1 C 0.6157(7) 0.5474(5) 0.3932(3) 0.0403(16) Uani 1 1 d . . . H1 H 0.6040 0.6143 0.3698 0.048 Uiso 1 1 calc R . . C6 C 0.5386(7) 0.3194(5) 0.3569(3) 0.0382(16) Uani 1 1 d . . . C7 C 0.5374(8) 0.2199(5) 0.3830(4) 0.0507(19) Uani 1 1 d . . . H7 H 0.5675 0.1908 0.4283 0.061 Uiso 1 1 calc R . . C8 C 0.4921(9) 0.1638(5) 0.3426(5) 0.065(2) Uani 1 1 d . . . H8 H 0.4897 0.0968 0.3605 0.078 Uiso 1 1 calc R . . C9 C 0.4504(8) 0.2067(6) 0.2757(5) 0.065(2) Uani 1 1 d . . . H9 H 0.4225 0.1685 0.2471 0.078 Uiso 1 1 calc R . . C10 C 0.4505(7) 0.3102(5) 0.2508(4) 0.0480(18) Uani 1 1 d . . . H10 H 0.4198 0.3408 0.2059 0.058 Uiso 1 1 calc R . . C15 C 0.6617(7) 0.5271(4) 0.1326(3) 0.0366(16) Uani 1 1 d . . . C14 C 0.7805(8) 0.5128(5) 0.0807(3) 0.0479(18) Uani 1 1 d . . . H14 H 0.7626 0.5281 0.0329 0.058 Uiso 1 1 calc R . . C13 C 0.9247(9) 0.4757(5) 0.1011(4) 0.057(2) Uani 1 1 d . . . H13 H 1.0051 0.4647 0.0672 0.069 Uiso 1 1 calc R . . C12 C 0.9486(8) 0.4549(5) 0.1719(4) 0.0516(19) Uani 1 1 d . . . H12 H 1.0449 0.4294 0.1869 0.062 Uiso 1 1 calc R . . C11 C 0.8243(8) 0.4733(5) 0.2211(3) 0.0425(17) Uani 1 1 d . . . H11A H 0.8400 0.4606 0.2691 0.051 Uiso 1 1 calc R . . C16 C 0.5049(7) 0.5615(4) 0.1165(3) 0.0349(15) Uani 1 1 d . . . C17 C 0.4553(9) 0.6027(5) 0.0504(3) 0.0490(19) Uani 1 1 d . . . H17 H 0.5243 0.6114 0.0124 0.059 Uiso 1 1 calc R . . C18 C 0.3063(9) 0.6314(5) 0.0391(4) 0.055(2) Uani 1 1 d . . . H18 H 0.2738 0.6600 -0.0058 0.066 Uiso 1 1 calc R . . C19 C 0.2059(8) 0.6168(5) 0.0956(4) 0.0509(19) Uani 1 1 d . . . H19 H 0.1045 0.6334 0.0891 0.061 Uiso 1 1 calc R . . C20 C 0.2575(8) 0.5771(5) 0.1627(4) 0.0456(17) Uani 1 1 d . . . H20 H 0.1892 0.5697 0.2012 0.055 Uiso 1 1 calc R . . C37 C -0.0703(7) 0.9192(5) 0.4110(3) 0.0361(15) Uani 1 1 d . . . C38 C -0.1674(7) 0.9113(6) 0.4711(3) 0.0501(18) Uani 1 1 d . . . H38 H -0.2216 0.9695 0.4912 0.060 Uiso 1 1 calc R . . C39 C -0.1811(9) 0.8146(7) 0.5004(4) 0.061(2) Uani 1 1 d . . . H39 H -0.2441 0.8069 0.5410 0.074 Uiso 1 1 calc R . . C40 C -0.1020(9) 0.7310(6) 0.4695(4) 0.056(2) Uani 1 1 d . . . H40 H -0.1108 0.6658 0.4887 0.067 Uiso 1 1 calc R . . C41 C -0.0091(8) 0.7436(5) 0.4096(3) 0.0465(18) Uani 1 1 d . . . H41 H 0.0449 0.6861 0.3888 0.056 Uiso 1 1 calc R . . C36 C -0.0387(6) 1.0172(5) 0.3768(3) 0.0329(15) Uani 1 1 d . . . C35 C -0.0830(8) 1.1065(5) 0.4061(4) 0.0533(19) Uani 1 1 d . . . H35 H -0.1418 1.1099 0.4487 0.064 Uiso 1 1 calc R . . C34 C -0.0396(8) 1.1907(5) 0.3720(4) 0.054(2) Uani 1 1 d . . . H34 H -0.0674 1.2515 0.3917 0.064 Uiso 1 1 calc R . . C33 C 0.0462(8) 1.1842(5) 0.3080(4) 0.0499(18) Uani 1 1 d . . . H33 H 0.0758 1.2406 0.2836 0.060 Uiso 1 1 calc R . . C32 C 0.0865(7) 1.0918(4) 0.2815(3) 0.0406(16) Uani 1 1 d . . . H32 H 0.1445 1.0872 0.2387 0.049 Uiso 1 1 calc R . . C26 C -0.0228(7) 0.8533(5) 0.1582(3) 0.0415(16) Uani 1 1 d . . . C25 C -0.1084(8) 0.8328(5) 0.1121(3) 0.0519(19) Uani 1 1 d . . . H25 H -0.0808 0.8393 0.0637 0.062 Uiso 1 1 calc R . . C24 C -0.2337(9) 0.8028(5) 0.1376(4) 0.060(2) Uani 1 1 d . . . H24 H -0.2916 0.7884 0.1070 0.072 Uiso 1 1 calc R . . C23 C -0.2723(8) 0.7944(5) 0.2095(4) 0.058(2) Uani 1 1 d . . . H23 H -0.3572 0.7747 0.2284 0.070 Uiso 1 1 calc R . . C22 C -0.1825(8) 0.8158(5) 0.2524(4) 0.0510(18) Uani 1 1 d . . . H22 H -0.2087 0.8099 0.3009 0.061 Uiso 1 1 calc R . . C27 C 0.1146(7) 0.8858(4) 0.1347(3) 0.0383(16) Uani 1 1 d . . . C28 C 0.1708(9) 0.8975(5) 0.0643(3) 0.055(2) Uani 1 1 d . . . H28 H 0.1220 0.8849 0.0290 0.066 Uiso 1 1 calc R . . C29 C 0.2984(10) 0.9279(5) 0.0473(4) 0.063(2) Uani 1 1 d . . . H29 H 0.3346 0.9380 0.0001 0.076 Uiso 1 1 calc R . . C30 C 0.3737(8) 0.9436(5) 0.0998(4) 0.0533(19) Uani 1 1 d . . . H30 H 0.4616 0.9629 0.0889 0.064 Uiso 1 1 calc R . . C31 C 0.3142(8) 0.9298(5) 0.1692(3) 0.0454(17) Uani 1 1 d . . . H31 H 0.3638 0.9402 0.2051 0.054 Uiso 1 1 calc R . . C21 C 0.3646(7) 0.6539(4) 0.2872(3) 0.0321(15) Uani 1 1 d . . . C42 C 0.8314(12) 0.1696(11) 0.1407(5) 0.201(7) Uani 1 1 d . . . H42A H 0.7840 0.2323 0.1599 0.302 Uiso 1 1 calc R . . H42B H 0.8958 0.1219 0.1743 0.302 Uiso 1 1 calc R . . H42C H 0.7566 0.1399 0.1312 0.302 Uiso 1 1 calc R . . Cl1 Cl 0.0847(2) 0.47172(14) 0.35550(10) 0.0525(5) Uani 1 1 d . . . Cl2 Cl 0.2954(3) 0.24561(16) 0.08051(11) 0.0703(6) Uani 1 1 d . . . Cl3 Cl 0.43270(19) 0.88433(11) 0.39648(8) 0.0370(4) Uani 1 1 d . . . N1 N 0.5722(5) 0.4823(4) 0.3628(2) 0.0306(12) Uani 1 1 d . . . N2 N 0.4946(5) 0.3644(4) 0.2916(3) 0.0350(12) Uani 1 1 d . . . N3 N 0.6855(6) 0.5079(3) 0.2021(2) 0.0348(13) Uani 1 1 d . . . N4 N 0.4047(6) 0.5492(3) 0.1729(2) 0.0338(12) Uani 1 1 d . . . N9 N 0.0059(6) 0.8359(4) 0.3806(2) 0.0352(12) Uani 1 1 d . . . N8 N 0.0465(5) 1.0091(3) 0.3142(2) 0.0332(12) Uani 1 1 d . . . N6 N -0.0594(6) 0.8448(4) 0.2283(3) 0.0410(13) Uani 1 1 d . . . N7 N 0.1879(6) 0.9019(3) 0.1867(2) 0.0375(13) Uani 1 1 d . . . N5 N 0.2736(7) 0.7297(4) 0.2923(3) 0.0517(16) Uani 1 1 d . . . O1 O 0.0119(9) 0.5650(4) 0.3138(3) 0.118(3) Uani 1 1 d . . . O2 O 0.1999(9) 0.4744(5) 0.3902(4) 0.141(3) Uani 1 1 d . . . O3 O -0.0211(9) 0.4221(7) 0.3849(4) 0.096(3) Uani 0.696(7) 1 d P . . O4 O 0.1445(10) 0.3965(6) 0.3101(5) 0.188(4) Uani 1 1 d . . . O5 O 0.4411(10) 0.1794(6) 0.0768(6) 0.226(6) Uani 1 1 d . . . O6 O 0.2316(14) 0.2532(7) 0.0203(3) 0.209(6) Uani 1 1 d . . . O7 O 0.2147(7) 0.2035(4) 0.1382(3) 0.093(2) Uani 1 1 d . . . O8 O 0.3022(6) 0.3442(4) 0.0898(2) 0.0644(14) Uani 1 1 d . . . O9 O 0.4736(5) 0.9439(3) 0.4400(2) 0.0569(13) Uani 1 1 d . . . O10 O 0.5463(5) 0.7888(3) 0.3953(3) 0.0654(14) Uani 1 1 d . . . O11 O 0.4149(6) 0.9396(3) 0.3264(2) 0.0608(14) Uani 1 1 d . . . O12 O 0.2934(5) 0.8664(3) 0.4258(2) 0.0580(13) Uani 1 1 d . . . O13 O 0.9317(7) 0.1947(5) 0.0658(3) 0.117(2) Uani 1 1 d . . . H13A H 1.0314 0.1642 0.0783 0.176 Uiso 1 1 d R . . O3' O 0.016(2) 0.4996(15) 0.4278(10) 0.096(3) Uani 0.304(7) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0388(5) 0.0275(4) 0.0296(4) -0.0045(3) 0.0002(3) -0.0085(4) Cu2 0.0433(5) 0.0314(4) 0.0299(5) -0.0071(3) -0.0002(4) -0.0043(4) C5 0.033(4) 0.039(4) 0.027(4) -0.004(3) 0.007(3) -0.004(3) C4 0.038(4) 0.047(4) 0.039(4) 0.006(3) 0.012(3) 0.007(4) C3 0.038(5) 0.089(6) 0.036(4) -0.017(4) -0.001(3) -0.005(4) C2 0.043(5) 0.060(5) 0.043(4) -0.022(4) 0.003(4) -0.009(4) C1 0.038(4) 0.050(4) 0.036(4) -0.016(3) 0.006(3) -0.014(3) C6 0.031(4) 0.038(4) 0.038(4) 0.002(3) 0.008(3) -0.007(3) C7 0.048(5) 0.039(4) 0.060(5) 0.003(4) 0.011(4) -0.017(4) C8 0.056(6) 0.037(4) 0.095(7) 0.001(4) 0.004(5) -0.012(4) C9 0.054(5) 0.052(5) 0.105(7) -0.044(5) 0.022(5) -0.030(4) C10 0.042(5) 0.050(4) 0.058(5) -0.021(4) 0.005(4) -0.016(4) C15 0.046(5) 0.033(4) 0.035(4) -0.004(3) 0.000(3) -0.019(3) C14 0.053(5) 0.067(5) 0.030(4) -0.007(3) 0.008(4) -0.031(4) C13 0.052(5) 0.082(6) 0.040(5) -0.011(4) 0.020(4) -0.030(5) C12 0.040(5) 0.059(5) 0.055(5) -0.012(4) 0.004(4) -0.014(4) C11 0.047(5) 0.045(4) 0.037(4) -0.003(3) -0.002(4) -0.016(4) C16 0.041(4) 0.033(4) 0.033(4) -0.007(3) -0.003(3) -0.013(3) C17 0.065(6) 0.050(4) 0.037(4) 0.003(3) -0.011(4) -0.026(4) C18 0.067(6) 0.051(5) 0.051(5) 0.005(4) -0.027(4) -0.021(4) C19 0.049(5) 0.043(4) 0.064(5) -0.011(4) -0.020(4) -0.010(4) C20 0.040(5) 0.044(4) 0.055(5) -0.009(3) -0.005(4) -0.013(4) C37 0.026(4) 0.049(4) 0.032(4) -0.012(3) -0.005(3) -0.004(3) C38 0.037(4) 0.074(5) 0.040(4) -0.022(4) 0.005(3) -0.014(4) C39 0.053(5) 0.090(6) 0.045(5) -0.003(5) 0.004(4) -0.033(5) C40 0.060(6) 0.071(6) 0.044(5) 0.010(4) -0.010(4) -0.038(5) C41 0.053(5) 0.047(4) 0.045(4) -0.002(3) -0.011(4) -0.021(4) C36 0.023(4) 0.037(4) 0.034(4) -0.009(3) -0.003(3) 0.002(3) C35 0.050(5) 0.051(5) 0.057(5) -0.028(4) -0.013(4) 0.004(4) C34 0.059(5) 0.034(4) 0.070(5) -0.024(4) -0.010(4) -0.005(4) C33 0.059(5) 0.038(4) 0.052(5) -0.011(3) -0.005(4) -0.010(4) C32 0.045(4) 0.032(4) 0.038(4) -0.002(3) -0.001(3) -0.004(3) C26 0.035(4) 0.048(4) 0.038(4) -0.012(3) -0.008(3) -0.002(3) C25 0.050(5) 0.070(5) 0.033(4) -0.018(3) -0.003(4) -0.007(4) C24 0.052(5) 0.072(5) 0.058(5) -0.031(4) -0.018(4) -0.003(4) C23 0.041(5) 0.077(6) 0.061(5) -0.016(4) -0.008(4) -0.017(4) C22 0.043(5) 0.070(5) 0.041(4) -0.009(4) -0.001(4) -0.018(4) C27 0.045(4) 0.027(3) 0.035(4) -0.007(3) -0.003(3) 0.004(3) C28 0.069(6) 0.062(5) 0.029(4) -0.011(3) 0.003(4) -0.012(4) C29 0.085(7) 0.068(5) 0.026(4) -0.004(4) 0.006(4) -0.011(5) C30 0.053(5) 0.055(5) 0.045(5) -0.003(4) 0.004(4) -0.010(4) C31 0.043(5) 0.049(4) 0.042(4) -0.008(3) 0.001(4) -0.009(4) C21 0.042(4) 0.022(3) 0.022(3) -0.003(3) -0.004(3) 0.006(3) C42 0.107(10) 0.41(2) 0.037(6) 0.039(9) -0.034(6) -0.031(12) Cl1 0.0604(13) 0.0486(11) 0.0520(12) 0.0013(9) -0.0035(10) -0.0259(10) Cl2 0.0947(18) 0.0590(13) 0.0572(13) -0.0152(10) 0.0320(12) -0.0330(13) Cl3 0.0474(11) 0.0298(8) 0.0353(9) -0.0048(7) -0.0043(8) -0.0128(8) N1 0.032(3) 0.034(3) 0.024(3) -0.005(2) 0.004(2) -0.008(2) N2 0.030(3) 0.035(3) 0.041(3) -0.011(3) 0.010(3) -0.014(3) N3 0.044(4) 0.033(3) 0.030(3) 0.000(2) -0.003(3) -0.016(3) N4 0.035(3) 0.034(3) 0.033(3) -0.010(2) 0.002(3) -0.009(3) N9 0.038(3) 0.040(3) 0.028(3) -0.006(2) -0.005(2) -0.009(3) N8 0.033(3) 0.029(3) 0.037(3) -0.009(2) -0.005(3) -0.005(2) N6 0.041(4) 0.044(3) 0.034(3) -0.010(3) -0.003(3) -0.002(3) N7 0.039(4) 0.034(3) 0.032(3) -0.005(2) 0.000(3) -0.002(3) N5 0.065(5) 0.057(4) 0.039(3) -0.002(3) -0.016(3) -0.025(4) O1 0.231(8) 0.059(4) 0.087(4) 0.017(3) -0.075(5) -0.066(5) O2 0.119(7) 0.136(6) 0.200(7) -0.061(5) -0.075(6) -0.036(5) O3 0.074(6) 0.122(7) 0.085(6) 0.053(5) -0.004(5) -0.055(5) O4 0.163(9) 0.149(7) 0.261(10) -0.125(7) -0.111(8) 0.035(6) O5 0.111(7) 0.097(6) 0.429(16) -0.081(8) 0.141(9) -0.008(5) O6 0.468(18) 0.204(9) 0.064(5) 0.011(5) -0.071(7) -0.256(11) O7 0.112(5) 0.086(4) 0.078(4) 0.010(3) 0.035(4) -0.052(4) O8 0.089(4) 0.059(3) 0.049(3) -0.013(2) 0.004(3) -0.028(3) O9 0.075(4) 0.056(3) 0.048(3) -0.018(2) -0.017(3) -0.022(3) O10 0.048(3) 0.035(3) 0.106(4) -0.022(3) 0.000(3) 0.003(2) O11 0.083(4) 0.069(3) 0.033(3) 0.008(2) -0.008(3) -0.033(3) O12 0.043(3) 0.067(3) 0.061(3) 0.009(2) 0.001(3) -0.023(3) O13 0.076(5) 0.172(6) 0.103(5) -0.040(4) -0.048(4) -0.007(5) O3' 0.074(6) 0.122(7) 0.085(6) 0.053(5) -0.004(5) -0.055(5) _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 C21 1.943(6) . ? Cu1 N1 1.987(4) . ? Cu1 N4 2.013(5) . ? Cu1 N2 2.037(5) . ? Cu1 N3 2.155(5) . ? Cu2 N9 1.978(5) . ? Cu2 N7 2.007(5) . ? Cu2 N5 2.024(6) . ? Cu2 N8 2.025(5) . ? Cu2 N6 2.184(5) . ? C5 N1 1.337(7) . ? C5 C4 1.402(8) . ? C5 C6 1.466(8) . ? C4 C3 1.367(9) . ? C4 H4 0.9300 . ? C3 C2 1.364(9) . ? C3 H3 0.9300 . ? C2 C1 1.353(8) . ? C2 H2 0.9300 . ? C1 N1 1.330(7) . ? C1 H1 0.9300 . ? C6 N2 1.353(7) . ? C6 C7 1.372(8) . ? C7 C8 1.366(9) . ? C7 H7 0.9300 . ? C8 C9 1.368(9) . ? C8 H8 0.9300 . ? C9 C10 1.418(9) . ? C9 H9 0.9300 . ? C10 N2 1.345(7) . ? C10 H10 0.9300 . ? C15 N3 1.347(7) . ? C15 C14 1.394(8) . ? C15 C16 1.462(8) . ? C14 C13 1.378(9) . ? C14 H14 0.9300 . ? C13 C12 1.372(8) . ? C13 H13 0.9300 . ? C12 C11 1.399(9) . ? C12 H12 0.9300 . ? C11 N3 1.323(7) . ? C11 H11A 0.9300 . ? C16 N4 1.368(7) . ? C16 C17 1.373(8) . ? C17 C18 1.371(9) . ? C17 H17 0.9300 . ? C18 C19 1.376(9) . ? C18 H18 0.9300 . ? C19 C20 1.393(8) . ? C19 H19 0.9300 . ? C20 N4 1.351(7) . ? C20 H20 0.9300 . ? C37 N9 1.345(7) . ? C37 C38 1.391(8) . ? C37 C36 1.486(8) . ? C38 C39 1.385(9) . ? C38 H38 0.9300 . ? C39 C40 1.360(9) . ? C39 H39 0.9300 . ? C40 C41 1.374(9) . ? C40 H40 0.9300 . ? C41 N9 1.332(7) . ? C41 H41 0.9300 . ? C36 N8 1.362(7) . ? C36 C35 1.371(8) . ? C35 C34 1.372(9) . ? C35 H35 0.9300 . ? C34 C33 1.386(9) . ? C34 H34 0.9300 . ? C33 C32 1.382(8) . ? C33 H33 0.9300 . ? C32 N8 1.331(7) . ? C32 H32 0.9300 . ? C26 N6 1.341(7) . ? C26 C25 1.381(8) . ? C26 C27 1.482(9) . ? C25 C24 1.368(9) . ? C25 H25 0.9300 . ? C24 C23 1.377(9) . ? C24 H24 0.9300 . ? C23 C22 1.371(8) . ? C23 H23 0.9300 . ? C22 N6 1.337(8) . ? C22 H22 0.9300 . ? C27 N7 1.363(7) . ? C27 C28 1.391(8) . ? C28 C29 1.368(9) . ? C28 H28 0.9300 . ? C29 C30 1.381(9) . ? C29 H29 0.9300 . ? C30 C31 1.385(8) . ? C30 H30 0.9300 . ? C31 N7 1.340(7) . ? C31 H31 0.9300 . ? C21 N5 1.145(7) . ? C42 O13 1.662(11) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? Cl1 O2 1.351(6) . ? Cl1 O3 1.380(7) . ? Cl1 O4 1.413(7) . ? Cl1 O1 1.416(5) . ? Cl1 O3' 1.52(2) . ? Cl2 O6 1.341(7) . ? Cl2 O5 1.402(8) . ? Cl2 O7 1.402(5) . ? Cl2 O8 1.418(4) . ? Cl3 O9 1.422(4) . ? Cl3 O11 1.426(4) . ? Cl3 O10 1.427(4) . ? Cl3 O12 1.434(4) . ? O13 H13A 0.9479 . ? 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 C21 Cu1 N1 93.8(2) . . ? C21 Cu1 N4 88.5(2) . . ? N1 Cu1 N4 176.6(2) . . ? C21 Cu1 N2 144.2(2) . . ? N1 Cu1 N2 80.5(2) . . ? N4 Cu1 N2 99.19(19) . . ? C21 Cu1 N3 116.4(2) . . ? N1 Cu1 N3 98.27(19) . . ? N4 Cu1 N3 78.5(2) . . ? N2 Cu1 N3 99.34(18) . . ? N9 Cu2 N7 171.4(2) . . ? N9 Cu2 N5 96.9(2) . . ? N7 Cu2 N5 88.7(2) . . ? N9 Cu2 N8 81.2(2) . . ? N7 Cu2 N8 97.87(19) . . ? N5 Cu2 N8 145.4(2) . . ? N9 Cu2 N6 93.6(2) . . ? N7 Cu2 N6 78.6(2) . . ? N5 Cu2 N6 104.84(19) . . ? N8 Cu2 N6 109.78(18) . . ? N1 C5 C4 119.4(6) . . ? N1 C5 C6 115.8(5) . . ? C4 C5 C6 124.7(6) . . ? C3 C4 C5 119.2(6) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C2 C3 C4 120.1(6) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C1 C2 C3 118.2(6) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? N1 C1 C2 123.1(6) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? N2 C6 C7 121.5(6) . . ? N2 C6 C5 114.1(5) . . ? C7 C6 C5 124.4(6) . . ? C8 C7 C6 120.0(7) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 119.6(7) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C8 C9 C10 118.9(7) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 120.5(7) . . ? N2 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? N3 C15 C14 121.2(6) . . ? N3 C15 C16 115.4(6) . . ? C14 C15 C16 123.4(6) . . ? C13 C14 C15 119.2(6) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C12 C13 C14 119.4(7) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C13 C12 C11 118.3(7) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? N3 C11 C12 122.7(6) . . ? N3 C11 H11A 118.6 . . ? C12 C11 H11A 118.6 . . ? N4 C16 C17 120.0(6) . . ? N4 C16 C15 115.3(5) . . ? C17 C16 C15 124.7(6) . . ? C18 C17 C16 121.4(7) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 118.6(6) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C18 C19 C20 119.3(7) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? N4 C20 C19 121.4(6) . . ? N4 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? N9 C37 C38 121.3(6) . . ? N9 C37 C36 115.0(5) . . ? C38 C37 C36 123.7(6) . . ? C39 C38 C37 118.3(7) . . ? C39 C38 H38 120.9 . . ? C37 C38 H38 120.9 . . ? C40 C39 C38 119.7(7) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 119.4(7) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? N9 C41 C40 121.9(7) . . ? N9 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? N8 C36 C35 122.2(6) . . ? N8 C36 C37 113.5(5) . . ? C35 C36 C37 124.2(6) . . ? C36 C35 C34 119.4(7) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C34 C33 119.2(7) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C32 C33 C34 118.2(6) . . ? C32 C33 H33 120.9 . . ? C34 C33 H33 120.9 . . ? N8 C32 C33 123.2(6) . . ? N8 C32 H32 118.4 . . ? C33 C32 H32 118.4 . . ? N6 C26 C25 121.5(6) . . ? N6 C26 C27 115.2(6) . . ? C25 C26 C27 123.3(6) . . ? C24 C25 C26 120.0(6) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C24 C23 118.7(7) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C22 C23 C24 118.4(7) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? N6 C22 C23 123.6(6) . . ? N6 C22 H22 118.2 . . ? C23 C22 H22 118.2 . . ? N7 C27 C28 120.3(6) . . ? N7 C27 C26 116.3(5) . . ? C28 C27 C26 123.4(6) . . ? C29 C28 C27 119.5(7) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 120.4(7) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C31 117.9(7) . . ? C29 C30 H30 121.0 . . ? C31 C30 H30 121.0 . . ? N7 C31 C30 122.5(6) . . ? N7 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? N5 C21 Cu1 166.8(6) . . ? O13 C42 H42A 109.5 . . ? O13 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O13 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O2 Cl1 O3 123.8(5) . . ? O2 Cl1 O4 106.2(5) . . ? O3 Cl1 O4 90.3(6) . . ? O2 Cl1 O1 116.1(4) . . ? O3 Cl1 O1 108.2(5) . . ? O4 Cl1 O1 108.0(5) . . ? O2 Cl1 O3' 74.7(8) . . ? O3 Cl1 O3' 66.4(7) . . ? O4 Cl1 O3' 149.7(8) . . ? O1 Cl1 O3' 98.0(8) . . ? O6 Cl2 O5 109.7(7) . . ? O6 Cl2 O7 110.0(5) . . ? O5 Cl2 O7 107.7(5) . . ? O6 Cl2 O8 109.6(4) . . ? O5 Cl2 O8 108.8(5) . . ? O7 Cl2 O8 111.0(3) . . ? O9 Cl3 O11 109.7(3) . . ? O9 Cl3 O10 109.0(3) . . ? O11 Cl3 O10 110.3(3) . . ? O9 Cl3 O12 108.4(3) . . ? O11 Cl3 O12 109.2(3) . . ? O10 Cl3 O12 110.2(3) . . ? C1 N1 C5 119.9(5) . . ? C1 N1 Cu1 124.7(4) . . ? C5 N1 Cu1 115.3(4) . . ? C10 N2 C6 119.4(5) . . ? C10 N2 Cu1 126.4(4) . . ? C6 N2 Cu1 113.9(4) . . ? C11 N3 C15 119.0(6) . . ? C11 N3 Cu1 127.3(4) . . ? C15 N3 Cu1 112.9(4) . . ? C20 N4 C16 119.3(5) . . ? C20 N4 Cu1 123.0(4) . . ? C16 N4 Cu1 116.5(4) . . ? C41 N9 C37 119.4(6) . . ? C41 N9 Cu2 124.9(5) . . ? C37 N9 Cu2 115.2(4) . . ? C32 N8 C36 117.7(5) . . ? C32 N8 Cu2 128.0(4) . . ? C36 N8 Cu2 114.1(4) . . ? C22 N6 C26 117.7(6) . . ? C22 N6 Cu2 129.5(4) . . ? C26 N6 Cu2 112.3(4) . . ? C31 N7 C27 119.4(5) . . ? C31 N7 Cu2 123.4(4) . . ? C27 N7 Cu2 116.8(4) . . ? C21 N5 Cu2 172.3(5) . . ? C42 O13 H13A 103.1 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.039 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.098 # Attachment '- 1-7.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 694304' #TrackingRef '- 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H40 Cl Cu3 N12 O4, 2(Cl O4)' _chemical_formula_sum 'C52 H40 Cl3 Cu3 N12 O12' _chemical_formula_weight 1321.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 23.007(6) _cell_length_b 21.202(5) _cell_length_c 23.327(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.605(3) _cell_angle_gamma 90.00 _cell_volume 10650(5) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2706 _cell_measurement_theta_min 2.558 _cell_measurement_theta_max 21.127 _exptl_crystal_description block _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5360 _exptl_absorpt_coefficient_mu 1.414 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8266 _exptl_absorpt_correction_T_max 0.8953 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; The structure was solved by direct methods (Bruker, 2000) and successive difference Fourier syntheses. ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25972 _diffrn_reflns_av_R_equivalents 0.1235 _diffrn_reflns_av_sigmaI/netI 0.1658 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9363 _reflns_number_gt 4237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0282P)^2^+1.6900P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9363 _refine_ls_number_parameters 761 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1544 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.12156(3) 0.34802(3) 0.06262(4) 0.0395(2) Uani 1 1 d . . . Cu2 Cu 0.20106(3) 0.14995(3) 0.18152(4) 0.0412(2) Uani 1 1 d . . . Cu3 Cu 0.11648(3) -0.06919(3) 0.13451(3) 0.0347(2) Uani 1 1 d . . . C1 C 0.0341(4) 0.3095(3) 0.1260(3) 0.0495(19) Uani 1 1 d . . . H1 H 0.0681 0.2907 0.1555 0.059 Uiso 1 1 calc R . . C2 C -0.0224(4) 0.3041(3) 0.1320(3) 0.054(2) Uani 1 1 d . . . H2 H -0.0266 0.2829 0.1652 0.065 Uiso 1 1 calc R . . C3 C -0.0727(4) 0.3304(3) 0.0886(4) 0.059(2) Uani 1 1 d . . . H3 H -0.1118 0.3269 0.0918 0.071 Uiso 1 1 calc R . . C4 C -0.0656(3) 0.3620(3) 0.0400(3) 0.051(2) Uani 1 1 d . . . H4 H -0.0996 0.3795 0.0094 0.062 Uiso 1 1 calc R . . C5 C -0.0064(3) 0.3670(3) 0.0380(3) 0.0372(17) Uani 1 1 d . . . C6 C 0.0083(3) 0.4040(3) -0.0089(3) 0.0362(17) Uani 1 1 d . . . C7 C -0.0367(3) 0.4354(3) -0.0561(3) 0.053(2) Uani 1 1 d . . . H7 H -0.0786 0.4325 -0.0615 0.064 Uiso 1 1 calc R . . C8 C -0.0163(4) 0.4712(3) -0.0948(4) 0.062(2) Uani 1 1 d . . . H8 H -0.0451 0.4927 -0.1272 0.074 Uiso 1 1 calc R . . C9 C 0.0448(4) 0.4754(3) -0.0865(3) 0.0513(19) Uani 1 1 d . . . H9 H 0.0583 0.5008 -0.1118 0.062 Uiso 1 1 calc R . . C10 C 0.0866(3) 0.4415(3) -0.0398(3) 0.0452(18) Uani 1 1 d . . . H10 H 0.1285 0.4434 -0.0344 0.054 Uiso 1 1 calc R . . C11 C 0.1737(5) 0.4504(3) 0.1713(3) 0.089(3) Uani 1 1 d . . . H11 H 0.1365 0.4455 0.1783 0.107 Uiso 1 1 calc R . . C12 C 0.2198(5) 0.4952(4) 0.2073(4) 0.086(3) Uani 1 1 d . . . H12 H 0.2126 0.5209 0.2364 0.104 Uiso 1 1 calc R . . C13 C 0.2744(6) 0.4977(4) 0.1963(5) 0.107(4) Uani 1 1 d . . . H13 H 0.3049 0.5256 0.2193 0.128 Uiso 1 1 calc R . . C14 C 0.2862(4) 0.4626(4) 0.1545(4) 0.080(3) Uani 1 1 d . . . H14 H 0.3241 0.4656 0.1488 0.096 Uiso 1 1 calc R . . C15 C 0.2396(4) 0.4204(3) 0.1187(4) 0.057(2) Uani 1 1 d . . . C16 C 0.2468(3) 0.3829(3) 0.0700(3) 0.048(2) Uani 1 1 d . . . C17 C 0.3031(3) 0.3765(3) 0.0592(4) 0.059(2) Uani 1 1 d . . . H17 H 0.3397 0.3937 0.0861 0.070 Uiso 1 1 calc R . . C18 C 0.3023(4) 0.3441(4) 0.0075(4) 0.071(3) Uani 1 1 d . . . H18 H 0.3387 0.3393 -0.0008 0.085 Uiso 1 1 calc R . . C19 C 0.2488(4) 0.3194(3) -0.0309(4) 0.062(2) Uani 1 1 d . . . H19 H 0.2474 0.2993 -0.0668 0.074 Uiso 1 1 calc R . . C20 C 0.1966(3) 0.3244(3) -0.0158(3) 0.0466(19) Uani 1 1 d . . . H20 H 0.1602 0.3058 -0.0417 0.056 Uiso 1 1 calc R . . C21 C 0.1731(3) 0.2254(3) 0.1349(3) 0.0397(18) Uani 1 1 d . . . C22 C 0.1870(4) 0.1859(3) 0.3021(4) 0.061(2) Uani 1 1 d . . . H22 H 0.1447 0.1812 0.2809 0.073 Uiso 1 1 calc R . . C23 C 0.2067(4) 0.2078(4) 0.3618(5) 0.073(3) Uani 1 1 d . . . H23 H 0.1784 0.2174 0.3808 0.087 Uiso 1 1 calc R . . C24 C 0.2701(5) 0.2151(4) 0.3925(4) 0.077(3) Uani 1 1 d . . . H24 H 0.2849 0.2304 0.4324 0.093 Uiso 1 1 calc R . . C25 C 0.3105(4) 0.1996(3) 0.3640(4) 0.055(2) Uani 1 1 d . . . H25 H 0.3531 0.2044 0.3838 0.066 Uiso 1 1 calc R . . C26 C 0.2869(3) 0.1769(3) 0.3052(3) 0.0398(17) Uani 1 1 d . . . C27 C 0.3273(3) 0.1562(3) 0.2719(3) 0.0384(17) Uani 1 1 d . . . C28 C 0.3911(3) 0.1534(3) 0.2973(4) 0.063(2) Uani 1 1 d . . . H28 H 0.4111 0.1672 0.3373 0.076 Uiso 1 1 calc R . . C29 C 0.4251(3) 0.1306(4) 0.2642(4) 0.087(3) Uani 1 1 d . . . H29 H 0.4682 0.1279 0.2815 0.105 Uiso 1 1 calc R . . C30 C 0.3945(4) 0.1120(4) 0.2053(4) 0.072(3) Uani 1 1 d . . . H30 H 0.4162 0.0966 0.1815 0.087 Uiso 1 1 calc R . . C31 C 0.3308(3) 0.1164(3) 0.1818(3) 0.0496(19) Uani 1 1 d . . . H31 H 0.3102 0.1030 0.1418 0.059 Uiso 1 1 calc R . . C32 C 0.1629(3) 0.0696(3) 0.1582(3) 0.0435(18) Uani 1 1 d . . . C33 C 0.2448(3) -0.0767(3) 0.1372(3) 0.0432(18) Uani 1 1 d . . . H33 H 0.2314 -0.0475 0.1056 0.052 Uiso 1 1 calc R . . C34 C 0.3061(3) -0.0950(3) 0.1572(3) 0.0489(19) Uani 1 1 d . . . H34 H 0.3336 -0.0784 0.1399 0.059 Uiso 1 1 calc R . . C35 C 0.3252(3) -0.1392(3) 0.2040(3) 0.0503(19) Uani 1 1 d . . . H35 H 0.3660 -0.1535 0.2186 0.060 Uiso 1 1 calc R . . C36 C 0.2833(3) -0.1614(3) 0.2284(3) 0.0399(17) Uani 1 1 d . . . H36 H 0.2958 -0.1912 0.2597 0.048 Uiso 1 1 calc R . . C37 C 0.2228(3) -0.1403(3) 0.2073(3) 0.0296(15) Uani 1 1 d . . . C38 C 0.1744(3) -0.1570(3) 0.2323(3) 0.0289(15) Uani 1 1 d . . . C39 C 0.1853(3) -0.1994(3) 0.2813(3) 0.0359(17) Uani 1 1 d . . . H39 H 0.2237 -0.2192 0.2987 0.043 Uiso 1 1 calc R . . C40 C 0.1386(3) -0.2108(3) 0.3027(3) 0.0399(17) Uani 1 1 d . . . H40 H 0.1446 -0.2388 0.3351 0.048 Uiso 1 1 calc R . . C41 C 0.0825(3) -0.1812(3) 0.2767(3) 0.0447(18) Uani 1 1 d . . . H41 H 0.0503 -0.1882 0.2913 0.054 Uiso 1 1 calc R . . C42 C 0.0749(3) -0.1407(3) 0.2280(3) 0.0384(17) Uani 1 1 d . . . H42 H 0.0366 -0.1211 0.2099 0.046 Uiso 1 1 calc R . . C43 C 0.1172(3) -0.1427(3) 0.0215(3) 0.0497(19) Uani 1 1 d . . . H43 H 0.1595 -0.1483 0.0420 0.060 Uiso 1 1 calc R . . C44 C 0.0908(4) -0.1684(3) -0.0357(4) 0.063(2) Uani 1 1 d . . . H44 H 0.1148 -0.1910 -0.0534 0.075 Uiso 1 1 calc R . . C45 C 0.0289(4) -0.1601(3) -0.0664(4) 0.067(2) Uani 1 1 d . . . H45 H 0.0100 -0.1770 -0.1053 0.080 Uiso 1 1 calc R . . C46 C -0.0049(3) -0.1268(3) -0.0392(3) 0.056(2) Uani 1 1 d . . . H46 H -0.0473 -0.1211 -0.0597 0.067 Uiso 1 1 calc R . . C47 C 0.0235(3) -0.1012(3) 0.0190(3) 0.0391(18) Uani 1 1 d . . . C48 C -0.0077(3) -0.0621(3) 0.0506(3) 0.0410(17) Uani 1 1 d . . . C49 C -0.0693(3) -0.0429(3) 0.0253(3) 0.049(2) Uani 1 1 d . . . H49 H -0.0941 -0.0558 -0.0138 0.058 Uiso 1 1 calc R . . C50 C -0.0923(3) -0.0047(3) 0.0592(4) 0.055(2) Uani 1 1 d . . . H50 H -0.1332 0.0090 0.0425 0.067 Uiso 1 1 calc R . . C51 C -0.0572(3) 0.0137(3) 0.1164(4) 0.0479(19) Uani 1 1 d . . . H51 H -0.0736 0.0389 0.1396 0.057 Uiso 1 1 calc R . . C52 C 0.0033(3) -0.0062(3) 0.1389(3) 0.0460(19) Uani 1 1 d . . . H52 H 0.0284 0.0073 0.1776 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.02767(8) 0.24453(7) -0.08385(8) 0.0405(4) Uani 1 1 d U . . Cl2 Cl 0.26742(9) 0.06671(9) 0.47940(9) 0.0577(5) Uani 1 1 d . . . Cl3 Cl 0.0000 0.44262(13) 0.2500 0.0670(9) Uani 1 2 d S . . Cl4 Cl 0.0000 0.14994(19) 0.2500 0.0844(10) Uani 1 2 d S . . N1 N 0.0433(2) 0.3404(2) 0.0798(2) 0.0412(14) Uani 1 1 d . . . N2 N 0.0683(2) 0.4059(2) -0.0020(2) 0.0390(14) Uani 1 1 d . . . N3 N 0.1847(3) 0.4165(2) 0.1287(3) 0.0547(18) Uani 1 1 d . . . N4 N 0.1946(2) 0.3547(2) 0.0340(3) 0.0402(14) Uani 1 1 d . . . N5 N 0.1562(2) 0.2710(2) 0.1086(2) 0.0396(14) Uani 1 1 d . . . N6 N 0.2262(3) 0.1714(2) 0.2740(3) 0.0406(14) Uani 1 1 d . . . N7 N 0.2972(2) 0.1386(2) 0.2131(2) 0.0354(13) Uani 1 1 d . . . N8 N 0.1425(2) 0.0209(2) 0.1441(2) 0.0434(15) Uani 1 1 d . . . N9 N 0.2036(2) -0.0982(2) 0.1602(2) 0.0331(13) Uani 1 1 d . . . N10 N 0.1194(2) -0.1285(2) 0.2061(2) 0.0291(12) Uani 1 1 d . . . N11 N 0.0851(2) -0.1101(2) 0.0491(2) 0.0359(13) Uani 1 1 d . . . N12 N 0.0278(2) -0.0444(2) 0.1071(2) 0.0346(13) Uani 1 1 d . . . O1 O 0.0378(2) 0.1830(2) -0.1040(2) 0.0716(15) Uani 1 1 d . . . O2 O 0.0694(2) 0.2517(2) -0.0229(2) 0.0618(14) Uani 1 1 d U . . O3 O 0.0405(2) 0.2902(2) -0.1227(2) 0.0655(15) Uani 1 1 d . . . O4 O -0.0339(2) 0.2500(2) -0.0858(3) 0.0843(18) Uani 1 1 d . . . O5 O 0.3136(2) 0.0552(2) 0.4526(2) 0.0660(15) Uani 1 1 d . . . O6 O 0.2823(2) 0.1230(2) 0.5166(2) 0.0675(15) Uani 1 1 d . . . O7 O 0.2671(3) 0.0147(2) 0.5186(3) 0.0864(18) Uani 1 1 d . . . O8 O 0.2073(2) 0.0729(2) 0.4335(3) 0.0829(17) Uani 1 1 d . . . O9 O 0.0446(4) 0.4232(5) 0.2929(5) 0.246(6) Uani 1 1 d . . . O10 O 0.0407(5) 0.4373(5) 0.2075(5) 0.084(3) Uani 0.50 1 d P . . O11 O 0.0000 0.5055(5) 0.2500 0.216(6) Uani 1 2 d S . . O12 O 0.0484(5) 0.1618(6) 0.3082(5) 0.113(6) Uani 0.602(16) 1 d P . . O13 O 0.0000 0.0896(6) 0.2500 0.337(15) Uani 1 2 d S . . O14 O 0.0354(7) 0.1964(8) 0.2424(15) 0.188(11) Uani 0.50 1 d P . . O12' O 0.0373(8) 0.1377(12) 0.2123(9) 0.129(11) Uani 0.398(16) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0460(5) 0.0236(4) 0.0433(5) 0.0030(4) 0.0086(4) 0.0089(4) Cu2 0.0387(5) 0.0202(4) 0.0546(6) 0.0036(4) 0.0038(4) -0.0029(4) Cu3 0.0341(4) 0.0227(4) 0.0428(5) 0.0011(4) 0.0079(4) -0.0014(4) C1 0.067(6) 0.036(4) 0.045(5) 0.000(4) 0.020(4) 0.016(4) C2 0.076(6) 0.039(4) 0.061(6) 0.003(4) 0.040(5) 0.011(4) C3 0.059(5) 0.035(4) 0.098(7) -0.003(4) 0.045(5) 0.005(4) C4 0.057(5) 0.032(4) 0.063(6) 0.004(4) 0.020(4) 0.013(4) C5 0.044(4) 0.024(4) 0.041(5) -0.008(3) 0.012(4) 0.010(3) C6 0.047(4) 0.017(3) 0.039(5) -0.002(3) 0.008(4) 0.014(3) C7 0.051(5) 0.039(4) 0.063(6) 0.007(4) 0.011(4) 0.008(4) C8 0.063(6) 0.047(5) 0.063(6) 0.006(4) 0.006(5) 0.029(4) C9 0.073(6) 0.035(4) 0.047(5) 0.011(4) 0.022(4) 0.018(4) C10 0.065(5) 0.026(4) 0.047(5) -0.005(3) 0.023(4) 0.009(4) C11 0.173(9) 0.028(4) 0.037(5) 0.000(4) -0.001(6) 0.045(5) C12 0.166(10) 0.034(5) 0.034(6) -0.004(4) 0.003(7) 0.036(7) C13 0.206(14) 0.039(6) 0.058(8) 0.005(5) 0.025(9) 0.007(8) C14 0.094(7) 0.041(5) 0.064(7) 0.010(5) -0.022(5) -0.022(5) C15 0.068(6) 0.027(4) 0.051(6) 0.021(4) -0.011(5) 0.002(4) C16 0.056(5) 0.019(4) 0.047(5) 0.013(3) -0.008(4) -0.006(4) C17 0.032(5) 0.051(5) 0.075(7) 0.021(5) -0.003(5) -0.021(4) C18 0.057(6) 0.058(6) 0.091(7) 0.039(5) 0.019(5) 0.013(5) C19 0.045(5) 0.038(4) 0.109(7) 0.017(4) 0.035(5) 0.005(4) C20 0.044(5) 0.029(4) 0.068(6) 0.004(4) 0.022(4) 0.002(3) C21 0.025(4) 0.038(4) 0.047(5) 0.004(4) 0.001(3) -0.005(3) C22 0.075(6) 0.041(5) 0.072(7) 0.021(4) 0.032(5) -0.002(4) C23 0.090(7) 0.070(6) 0.084(8) 0.017(5) 0.063(6) -0.005(5) C24 0.119(8) 0.065(6) 0.052(6) 0.002(4) 0.034(6) -0.002(6) C25 0.073(6) 0.044(5) 0.041(5) 0.006(4) 0.011(5) -0.009(4) C26 0.048(5) 0.024(4) 0.044(5) 0.014(3) 0.012(4) -0.008(3) C27 0.036(4) 0.027(4) 0.042(5) 0.009(3) 0.002(4) 0.002(3) C28 0.042(5) 0.059(5) 0.069(6) -0.013(4) -0.004(4) 0.001(4) C29 0.031(5) 0.118(8) 0.098(8) -0.031(6) 0.005(5) 0.023(5) C30 0.046(5) 0.091(7) 0.071(7) -0.023(5) 0.009(5) 0.016(5) C31 0.046(5) 0.037(4) 0.056(5) 0.007(4) 0.006(4) 0.000(4) C32 0.031(4) 0.027(4) 0.061(5) 0.004(4) 0.003(3) -0.004(3) C33 0.045(4) 0.042(4) 0.040(5) 0.009(3) 0.012(4) 0.003(4) C34 0.038(4) 0.047(5) 0.067(6) 0.001(4) 0.023(4) -0.006(4) C35 0.029(4) 0.053(5) 0.065(6) -0.006(4) 0.012(4) -0.001(4) C36 0.036(4) 0.035(4) 0.040(4) -0.001(3) 0.002(3) 0.000(3) C37 0.025(4) 0.023(3) 0.035(4) 0.000(3) 0.004(3) -0.003(3) C38 0.029(4) 0.019(3) 0.032(4) -0.009(3) 0.002(3) -0.006(3) C39 0.039(4) 0.024(4) 0.034(4) 0.002(3) -0.001(3) 0.003(3) C40 0.044(4) 0.022(4) 0.053(5) 0.008(3) 0.017(4) -0.001(3) C41 0.040(4) 0.044(4) 0.053(5) 0.001(4) 0.020(4) 0.000(4) C42 0.032(4) 0.038(4) 0.044(5) 0.004(3) 0.011(3) 0.008(3) C43 0.056(5) 0.037(4) 0.059(6) -0.001(4) 0.025(4) 0.000(4) C44 0.080(6) 0.048(5) 0.065(6) -0.016(4) 0.032(5) -0.006(5) C45 0.095(7) 0.046(5) 0.050(6) -0.016(4) 0.015(5) -0.023(5) C46 0.064(5) 0.044(5) 0.049(6) 0.005(4) 0.005(4) -0.016(4) C47 0.046(5) 0.021(4) 0.036(5) 0.010(3) -0.003(4) -0.012(3) C48 0.044(4) 0.021(4) 0.055(5) 0.016(3) 0.013(4) -0.007(3) C49 0.030(4) 0.035(4) 0.071(6) 0.024(4) 0.006(4) -0.006(3) C50 0.040(5) 0.037(5) 0.094(7) 0.032(4) 0.030(5) 0.014(4) C51 0.050(5) 0.028(4) 0.068(6) 0.014(4) 0.025(4) 0.004(4) C52 0.051(5) 0.019(4) 0.072(6) 0.002(4) 0.027(4) -0.004(3) Cl1 0.0416(10) 0.0319(10) 0.0427(12) 0.0018(8) 0.0083(9) -0.0031(8) Cl2 0.0617(13) 0.0459(12) 0.0729(15) -0.0177(11) 0.0330(12) -0.0148(10) Cl3 0.081(2) 0.0369(17) 0.060(2) 0.000 -0.0037(19) 0.000 Cl4 0.108(3) 0.078(3) 0.069(3) 0.000 0.035(3) 0.000 N1 0.058(4) 0.024(3) 0.037(4) 0.001(3) 0.012(3) 0.012(3) N2 0.045(4) 0.029(3) 0.039(4) 0.004(3) 0.010(3) 0.011(3) N3 0.090(5) 0.023(3) 0.034(4) -0.001(3) 0.000(4) 0.025(3) N4 0.036(3) 0.024(3) 0.048(4) 0.002(3) -0.001(3) -0.003(3) N5 0.036(3) 0.029(3) 0.043(4) 0.006(3) 0.001(3) 0.006(3) N6 0.038(4) 0.026(3) 0.061(4) 0.009(3) 0.021(3) 0.002(3) N7 0.042(3) 0.027(3) 0.034(4) 0.003(3) 0.010(3) -0.004(3) N8 0.036(3) 0.027(3) 0.054(4) 0.003(3) -0.001(3) -0.010(3) N9 0.035(3) 0.028(3) 0.037(3) 0.002(3) 0.013(3) -0.006(3) N10 0.026(3) 0.024(3) 0.032(3) -0.005(2) 0.003(3) -0.001(2) N11 0.048(4) 0.017(3) 0.044(4) 0.003(2) 0.017(3) 0.001(3) N12 0.044(3) 0.017(3) 0.042(4) 0.002(3) 0.013(3) -0.008(3) O1 0.124(4) 0.031(3) 0.069(4) -0.013(3) 0.046(3) -0.003(3) O2 0.075(3) 0.050(3) 0.039(3) -0.003(2) -0.006(3) -0.009(3) O3 0.083(4) 0.048(3) 0.067(4) 0.024(3) 0.028(3) -0.007(3) O4 0.040(3) 0.091(4) 0.122(5) 0.047(4) 0.029(3) 0.015(3) O5 0.052(3) 0.076(4) 0.081(4) -0.026(3) 0.038(3) -0.022(3) O6 0.090(4) 0.048(3) 0.070(4) -0.022(3) 0.035(3) -0.020(3) O7 0.139(5) 0.047(3) 0.098(5) -0.010(3) 0.073(4) -0.005(3) O8 0.049(3) 0.091(4) 0.098(4) -0.022(3) 0.013(3) -0.021(3) O9 0.136(7) 0.337(14) 0.271(12) 0.204(11) 0.080(7) 0.133(8) O10 0.112(9) 0.082(8) 0.083(9) 0.017(7) 0.065(8) 0.015(7) O11 0.41(2) 0.078(8) 0.180(13) 0.000 0.131(13) 0.000 O12 0.108(10) 0.172(14) 0.062(9) -0.054(8) 0.033(7) -0.033(8) O13 0.79(4) 0.067(9) 0.140(14) 0.000 0.14(2) 0.000 O14 0.091(11) 0.116(14) 0.31(3) 0.131(18) 0.014(15) -0.011(10) O12' 0.088(13) 0.20(3) 0.116(16) -0.089(17) 0.062(11) -0.012(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 N5 1.962(5) . ? Cu1 N1 1.985(5) . ? Cu1 N2 1.995(5) . ? Cu1 N4 2.021(5) . ? Cu1 N3 2.240(6) . ? Cu1 O2 2.812(4) . ? Cu2 C32 1.906(6) . ? Cu2 C21 1.913(7) . ? Cu2 N6 2.077(6) . ? Cu2 N7 2.085(5) . ? Cu3 N9 1.978(5) . ? Cu3 N12 1.983(5) . ? Cu3 N8 1.990(5) . ? Cu3 N11 2.057(5) . ? Cu3 N10 2.073(5) . ? C1 N1 1.340(8) . ? C1 C2 1.361(8) . ? C1 H1 0.9300 . ? C2 C3 1.360(9) . ? C2 H2 0.9300 . ? C3 C4 1.376(9) . ? C3 H3 0.9300 . ? C4 C5 1.383(8) . ? C4 H4 0.9300 . ? C5 N1 1.338(7) . ? C5 C6 1.479(8) . ? C6 N2 1.334(7) . ? C6 C7 1.387(8) . ? C7 C8 1.381(9) . ? C7 H7 0.9300 . ? C8 C9 1.353(8) . ? C8 H8 0.9300 . ? C9 C10 1.374(8) . ? C9 H9 0.9300 . ? C10 N2 1.335(7) . ? C10 H10 0.9300 . ? C11 N3 1.323(9) . ? C11 C12 1.452(11) . ? C11 H11 0.9300 . ? C12 C13 1.369(12) . ? C12 H12 0.9300 . ? C13 C14 1.328(12) . ? C13 H13 0.9300 . ? C14 C15 1.420(9) . ? C14 H14 0.9300 . ? C15 N3 1.364(9) . ? C15 C16 1.445(10) . ? C16 N4 1.340(7) . ? C16 C17 1.410(9) . ? C17 C18 1.383(10) . ? C17 H17 0.9300 . ? C18 C19 1.347(9) . ? C18 H18 0.9300 . ? C19 C20 1.370(8) . ? C19 H19 0.9300 . ? C20 N4 1.341(8) . ? C20 H20 0.9300 . ? C21 N5 1.139(6) . ? C22 N6 1.324(8) . ? C22 C23 1.385(10) . ? C22 H22 0.9300 . ? C23 C24 1.388(10) . ? C23 H23 0.9300 . ? C24 C25 1.359(10) . ? C24 H24 0.9300 . ? C25 C26 1.372(9) . ? C25 H25 0.9300 . ? C26 N6 1.334(7) . ? C26 C27 1.472(9) . ? C27 N7 1.354(7) . ? C27 C28 1.377(8) . ? C28 C29 1.367(9) . ? C28 H28 0.9300 . ? C29 C30 1.363(10) . ? C29 H29 0.9300 . ? C30 C31 1.375(9) . ? C30 H30 0.9300 . ? C31 N7 1.321(8) . ? C31 H31 0.9300 . ? C32 N8 1.135(6) . ? C33 N9 1.322(7) . ? C33 C34 1.376(8) . ? C33 H33 0.9300 . ? C34 C35 1.389(8) . ? C34 H34 0.9300 . ? C35 C36 1.363(8) . ? C35 H35 0.9300 . ? C36 C37 1.378(7) . ? C36 H36 0.9300 . ? C37 N9 1.363(7) . ? C37 C38 1.471(8) . ? C38 N10 1.339(6) . ? C38 C39 1.407(8) . ? C39 C40 1.358(8) . ? C39 H39 0.9300 . ? C40 C41 1.370(7) . ? C40 H40 0.9300 . ? C41 C42 1.384(8) . ? C41 H41 0.9300 . ? C42 N10 1.322(7) . ? C42 H42 0.9300 . ? C43 N11 1.332(7) . ? C43 C44 1.370(9) . ? C43 H43 0.9300 . ? C44 C45 1.361(9) . ? C44 H44 0.9300 . ? C45 C46 1.361(9) . ? C45 H45 0.9300 . ? C46 C47 1.395(9) . ? C46 H46 0.9300 . ? C47 N11 1.355(7) . ? C47 C48 1.453(9) . ? C48 N12 1.337(8) . ? C48 C49 1.390(8) . ? C49 C50 1.363(9) . ? C49 H49 0.9300 . ? C50 C51 1.351(9) . ? C50 H50 0.9300 . ? C51 C52 1.369(8) . ? C51 H51 0.9300 . ? C52 N12 1.349(7) . ? C52 H52 0.9300 . ? Cl1 O4 1.405(5) . ? Cl1 O2 1.416(4) . ? Cl1 O3 1.426(4) . ? Cl1 O1 1.434(4) . ? Cl2 O8 1.425(5) . ? Cl2 O5 1.430(5) . ? Cl2 O7 1.434(5) . ? Cl2 O6 1.443(4) . ? Cl3 O9 1.225(8) 2 ? Cl3 O9 1.225(8) . ? Cl3 O11 1.334(10) . ? Cl3 O10 1.589(11) . ? Cl3 O10 1.589(11) 2 ? Cl4 O13 1.279(12) . ? Cl4 O14 1.329(14) 2 ? Cl4 O14 1.329(14) . ? Cl4 O12 1.442(11) 2 ? Cl4 O12 1.442(11) . ? Cl4 O12' 1.451(17) . ? Cl4 O12' 1.451(17) 2 ? O13 O12' 1.75(2) 2 ? O14 O14 1.79(5) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cu1 N1 92.6(2) . . ? N5 Cu1 N2 161.5(2) . . ? N1 Cu1 N2 81.0(2) . . ? N5 Cu1 N4 90.8(2) . . ? N1 Cu1 N4 172.9(2) . . ? N2 Cu1 N4 93.9(2) . . ? N5 Cu1 N3 97.08(19) . . ? N1 Cu1 N3 109.2(2) . . ? N2 Cu1 N3 101.41(19) . . ? N4 Cu1 N3 76.6(2) . . ? N5 Cu1 O2 76.89(17) . . ? N1 Cu1 O2 83.87(17) . . ? N2 Cu1 O2 85.15(17) . . ? N4 Cu1 O2 90.77(18) . . ? N3 Cu1 O2 166.1(2) . . ? C32 Cu2 C21 123.8(3) . . ? C32 Cu2 N6 115.1(2) . . ? C21 Cu2 N6 108.8(2) . . ? C32 Cu2 N7 108.8(2) . . ? C21 Cu2 N7 113.6(2) . . ? N6 Cu2 N7 77.6(2) . . ? N9 Cu3 N12 177.1(2) . . ? N9 Cu3 N8 91.79(19) . . ? N12 Cu3 N8 90.98(19) . . ? N9 Cu3 N11 97.8(2) . . ? N12 Cu3 N11 80.1(2) . . ? N8 Cu3 N11 120.2(2) . . ? N9 Cu3 N10 79.9(2) . . ? N12 Cu3 N10 99.1(2) . . ? N8 Cu3 N10 124.64(19) . . ? N11 Cu3 N10 115.15(17) . . ? N1 C1 C2 123.3(7) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.9(7) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.7(7) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 118.0(7) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N1 C5 C4 122.8(6) . . ? N1 C5 C6 113.8(6) . . ? C4 C5 C6 123.4(6) . . ? N2 C6 C7 122.2(6) . . ? N2 C6 C5 115.0(6) . . ? C7 C6 C5 122.8(6) . . ? C8 C7 C6 117.0(7) . . ? C8 C7 H7 121.5 . . ? C6 C7 H7 121.5 . . ? C9 C8 C7 121.1(7) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 118.7(7) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 121.7(7) . . ? N2 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? N3 C11 C12 119.7(9) . . ? N3 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 116.7(9) . . ? C13 C12 H12 121.6 . . ? C11 C12 H12 121.6 . . ? C14 C13 C12 123.6(12) . . ? C14 C13 H13 118.2 . . ? C12 C13 H13 118.2 . . ? C13 C14 C15 118.6(10) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? N3 C15 C14 119.4(8) . . ? N3 C15 C16 118.0(7) . . ? C14 C15 C16 122.5(9) . . ? N4 C16 C17 121.5(7) . . ? N4 C16 C15 114.4(7) . . ? C17 C16 C15 124.1(7) . . ? C18 C17 C16 118.2(7) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C19 C18 C17 120.1(8) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 118.6(8) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? N4 C20 C19 124.0(7) . . ? N4 C20 H20 118.0 . . ? C19 C20 H20 118.0 . . ? N5 C21 Cu2 177.9(6) . . ? N6 C22 C23 122.5(8) . . ? N6 C22 H22 118.7 . . ? C23 C22 H22 118.7 . . ? C22 C23 C24 117.9(8) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C25 C24 C23 119.8(8) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 118.4(8) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? N6 C26 C25 123.2(7) . . ? N6 C26 C27 114.8(6) . . ? C25 C26 C27 122.1(7) . . ? N7 C27 C28 120.7(7) . . ? N7 C27 C26 115.2(6) . . ? C28 C27 C26 124.1(7) . . ? C29 C28 C27 120.6(7) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 118.3(7) . . ? C30 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? C29 C30 C31 118.9(8) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? N7 C31 C30 123.5(7) . . ? N7 C31 H31 118.3 . . ? C30 C31 H31 118.3 . . ? N8 C32 Cu2 177.0(6) . . ? N9 C33 C34 124.1(6) . . ? N9 C33 H33 117.9 . . ? C34 C33 H33 117.9 . . ? C33 C34 C35 117.3(6) . . ? C33 C34 H34 121.4 . . ? C35 C34 H34 121.4 . . ? C36 C35 C34 119.2(6) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 120.8(6) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? N9 C37 C36 120.0(6) . . ? N9 C37 C38 113.7(5) . . ? C36 C37 C38 126.3(6) . . ? N10 C38 C39 122.0(6) . . ? N10 C38 C37 115.9(5) . . ? C39 C38 C37 122.1(5) . . ? C40 C39 C38 118.3(6) . . ? C40 C39 H39 120.9 . . ? C38 C39 H39 120.9 . . ? C39 C40 C41 120.0(6) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C40 C41 C42 118.4(6) . . ? C40 C41 H41 120.8 . . ? C42 C41 H41 120.8 . . ? N10 C42 C41 123.2(6) . . ? N10 C42 H42 118.4 . . ? C41 C42 H42 118.4 . . ? N11 C43 C44 123.1(7) . . ? N11 C43 H43 118.4 . . ? C44 C43 H43 118.4 . . ? C45 C44 C43 118.9(7) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C46 C45 C44 119.1(8) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? C45 C46 C47 120.5(7) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? N11 C47 C46 119.8(7) . . ? N11 C47 C48 115.4(6) . . ? C46 C47 C48 124.7(7) . . ? N12 C48 C49 120.8(7) . . ? N12 C48 C47 114.9(6) . . ? C49 C48 C47 124.2(7) . . ? C50 C49 C48 118.3(7) . . ? C50 C49 H49 120.8 . . ? C48 C49 H49 120.8 . . ? C51 C50 C49 121.7(7) . . ? C51 C50 H50 119.2 . . ? C49 C50 H50 119.2 . . ? C50 C51 C52 117.6(7) . . ? C50 C51 H51 121.2 . . ? C52 C51 H51 121.2 . . ? N12 C52 C51 122.6(7) . . ? N12 C52 H52 118.7 . . ? C51 C52 H52 118.7 . . ? O4 Cl1 O2 110.0(3) . . ? O4 Cl1 O3 110.8(3) . . ? O2 Cl1 O3 110.3(3) . . ? O4 Cl1 O1 110.0(3) . . ? O2 Cl1 O1 107.2(3) . . ? O3 Cl1 O1 108.4(3) . . ? O8 Cl2 O5 111.1(3) . . ? O8 Cl2 O7 109.2(3) . . ? O5 Cl2 O7 108.6(3) . . ? O8 Cl2 O6 109.7(3) . . ? O5 Cl2 O6 110.4(3) . . ? O7 Cl2 O6 107.8(3) . . ? O9 Cl3 O9 140.8(12) 2 . ? O9 Cl3 O11 109.6(6) 2 . ? O9 Cl3 O11 109.6(6) . . ? O9 Cl3 O10 88.6(6) 2 . ? O9 Cl3 O10 88.7(6) . . ? O11 Cl3 O10 94.1(4) . . ? O9 Cl3 O10 88.7(6) 2 2 ? O9 Cl3 O10 88.6(6) . 2 ? O11 Cl3 O10 94.1(4) . 2 ? O10 Cl3 O10 171.8(8) . 2 ? O13 Cl4 O14 137.8(11) . 2 ? O13 Cl4 O14 137.8(11) . . ? O14 Cl4 O14 84(2) 2 . ? O13 Cl4 O12 100.1(6) . 2 ? O14 Cl4 O12 71.9(11) 2 2 ? O14 Cl4 O12 93.0(12) . 2 ? O13 Cl4 O12 100.1(6) . . ? O14 Cl4 O12 93.0(12) 2 . ? O14 Cl4 O12 71.9(11) . . ? O12 Cl4 O12 159.9(11) 2 . ? O13 Cl4 O12' 79.7(11) . . ? O14 Cl4 O12' 137(2) 2 . ? O14 Cl4 O12' 62.0(12) . . ? O12 Cl4 O12' 83.5(9) 2 . ? O12 Cl4 O12' 100.1(8) . . ? O13 Cl4 O12' 79.7(11) . 2 ? O14 Cl4 O12' 62.0(12) 2 2 ? O14 Cl4 O12' 137(2) . 2 ? O12 Cl4 O12' 100.1(8) 2 2 ? O12 Cl4 O12' 83.5(9) . 2 ? O12' Cl4 O12' 159(2) . 2 ? C5 N1 C1 117.2(6) . . ? C5 N1 Cu1 114.9(5) . . ? C1 N1 Cu1 127.8(5) . . ? C6 N2 C10 119.3(6) . . ? C6 N2 Cu1 114.0(4) . . ? C10 N2 Cu1 126.5(5) . . ? C11 N3 C15 122.0(8) . . ? C11 N3 Cu1 128.3(7) . . ? C15 N3 Cu1 109.7(5) . . ? C16 N4 C20 117.5(6) . . ? C16 N4 Cu1 119.3(5) . . ? C20 N4 Cu1 122.6(4) . . ? C21 N5 Cu1 176.3(5) . . ? C22 N6 C26 118.2(7) . . ? C22 N6 Cu2 125.2(5) . . ? C26 N6 Cu2 116.2(5) . . ? C31 N7 C27 118.0(6) . . ? C31 N7 Cu2 126.8(5) . . ? C27 N7 Cu2 115.2(4) . . ? C32 N8 Cu3 169.7(5) . . ? C33 N9 C37 118.5(5) . . ? C33 N9 Cu3 124.3(4) . . ? C37 N9 Cu3 117.0(4) . . ? C42 N10 C38 118.1(5) . . ? C42 N10 Cu3 128.4(4) . . ? C38 N10 Cu3 113.5(4) . . ? C43 N11 C47 118.6(6) . . ? C43 N11 Cu3 128.5(5) . . ? C47 N11 Cu3 112.9(4) . . ? C48 N12 C52 118.9(6) . . ? C48 N12 Cu3 116.4(5) . . ? C52 N12 Cu3 124.3(5) . . ? Cl1 O2 Cu1 139.4(3) . . ? Cl4 O13 O12' 54.5(8) . 2 ? Cl4 O14 O14 47.8(11) . 2 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.752 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.101 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 752337' #TrackingRef '- 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H40 Cu3 N12, 3(Cl O4)' _chemical_formula_sum 'C52 H40 Cl3 Cu3 N12 O12' _chemical_formula_weight 1321.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.658(2) _cell_length_b 13.320(3) _cell_length_c 22.255(5) _cell_angle_alpha 74.632(3) _cell_angle_beta 82.523(4) _cell_angle_gamma 86.757(4) _cell_volume 2736.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1123 _cell_measurement_theta_min 2.435 _cell_measurement_theta_max 17.177 _exptl_crystal_description block _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8747 _exptl_absorpt_correction_T_max 0.8747 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; The structure was solved by direct methods (Bruker, 2000) and successive difference Fourier syntheses. ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13854 _diffrn_reflns_av_R_equivalents 0.0995 _diffrn_reflns_av_sigmaI/netI 0.2606 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9488 _reflns_number_gt 2949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0517P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9488 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2125 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1605 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 0.735 _refine_ls_restrained_S_all 0.735 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.47663(13) 0.69882(8) 0.62558(5) 0.0637(4) Uani 1 1 d . . . Cu2 Cu 0.54586(12) 0.90449(8) 0.77475(5) 0.0599(4) Uani 1 1 d . . . Cu3 Cu 0.52558(11) 0.71554(7) 1.00333(4) 0.0485(3) Uani 1 1 d . . . C1 C 0.7706(14) 0.6356(9) 0.6433(5) 0.094(4) Uani 1 1 d . . . H1 H 0.7762 0.6998 0.6519 0.113 Uiso 1 1 calc R . . C2 C 0.8842(13) 0.5703(11) 0.6483(5) 0.097(4) Uani 1 1 d . . . H2 H 0.9652 0.5896 0.6606 0.116 Uiso 1 1 calc R . . C3 C 0.8783(15) 0.4739(11) 0.6349(5) 0.108(4) Uani 1 1 d . . . H3 H 0.9548 0.4280 0.6374 0.129 Uiso 1 1 calc R . . C4 C 0.7569(16) 0.4498(8) 0.6182(5) 0.095(4) Uani 1 1 d . . . H4 H 0.7498 0.3864 0.6089 0.115 Uiso 1 1 calc R . . C5 C 0.6432(13) 0.5186(8) 0.6148(4) 0.068(3) Uani 1 1 d . . . C6 C 0.5082(13) 0.4990(7) 0.5970(4) 0.070(3) Uani 1 1 d . . . C7 C 0.4745(14) 0.4134(8) 0.5783(5) 0.085(3) Uani 1 1 d . . . H7 H 0.5404 0.3601 0.5772 0.103 Uiso 1 1 calc R . . C8 C 0.3482(16) 0.4067(9) 0.5619(5) 0.099(4) Uani 1 1 d . . . H8 H 0.3248 0.3467 0.5521 0.118 Uiso 1 1 calc R . . C9 C 0.2532(12) 0.4866(9) 0.5595(4) 0.091(3) Uani 1 1 d . . . H9 H 0.1666 0.4841 0.5460 0.109 Uiso 1 1 calc R . . C10 C 0.2904(13) 0.5716(8) 0.5778(4) 0.081(3) Uani 1 1 d . . . H10 H 0.2261 0.6265 0.5769 0.097 Uiso 1 1 calc R . . C11 C 0.5905(14) 0.8321(8) 0.4911(5) 0.101(4) Uani 1 1 d . . . H11 H 0.6766 0.7987 0.4974 0.121 Uiso 1 1 calc R . . C12 C 0.570(2) 0.9011(11) 0.4338(8) 0.156(8) Uani 1 1 d . . . H12 H 0.6431 0.9123 0.4015 0.187 Uiso 1 1 calc R . . C13 C 0.451(2) 0.9505(12) 0.4235(9) 0.153(9) Uani 1 1 d . . . H13 H 0.4413 0.9980 0.3851 0.183 Uiso 1 1 calc R . . C14 C 0.3387(17) 0.9314(9) 0.4705(6) 0.121(5) Uani 1 1 d . . . H14 H 0.2514 0.9625 0.4638 0.145 Uiso 1 1 calc R . . C15 C 0.3612(15) 0.8644(8) 0.5278(5) 0.076(3) Uani 1 1 d . . . C16 C 0.2508(13) 0.8455(8) 0.5827(5) 0.067(3) Uani 1 1 d . . . C17 C 0.1313(16) 0.9014(10) 0.5840(7) 0.108(5) Uani 1 1 d . . . H17 H 0.1125 0.9543 0.5491 0.130 Uiso 1 1 calc R . . C18 C 0.0380(19) 0.8804(14) 0.6363(9) 0.138(7) Uani 1 1 d . . . H18 H -0.0449 0.9194 0.6374 0.166 Uiso 1 1 calc R . . C19 C 0.0643(15) 0.8038(14) 0.6865(8) 0.128(6) Uani 1 1 d . . . H19 H -0.0011 0.7884 0.7220 0.154 Uiso 1 1 calc R . . C20 C 0.1904(14) 0.7471(8) 0.6852(5) 0.086(3) Uani 1 1 d . . . H20 H 0.2104 0.6956 0.7205 0.103 Uiso 1 1 calc R . . C21 C 0.5569(10) 0.8268(7) 0.7141(4) 0.061(3) Uani 1 1 d . . . C22 C 0.2685(11) 1.0055(7) 0.7327(3) 0.053(2) Uani 1 1 d . . . H22 H 0.2390 0.9375 0.7406 0.064 Uiso 1 1 calc R . . C23 C 0.1788(10) 1.0848(10) 0.7079(4) 0.075(3) Uani 1 1 d . . . H23 H 0.0947 1.0712 0.6959 0.090 Uiso 1 1 calc R . . C24 C 0.2176(13) 1.1850(9) 0.7015(4) 0.082(3) Uani 1 1 d . . . H24 H 0.1557 1.2401 0.6882 0.099 Uiso 1 1 calc R . . C25 C 0.3454(12) 1.2043(7) 0.7144(4) 0.071(3) Uani 1 1 d . . . H25 H 0.3729 1.2721 0.7095 0.085 Uiso 1 1 calc R . . C26 C 0.4348(10) 1.1189(7) 0.7355(4) 0.052(2) Uani 1 1 d . . . C27 C 0.5783(10) 1.1328(7) 0.7486(4) 0.054(2) Uani 1 1 d . . . C28 C 0.6285(12) 1.2250(7) 0.7515(4) 0.073(3) Uani 1 1 d . . . H28 H 0.5715 1.2846 0.7448 0.087 Uiso 1 1 calc R . . C29 C 0.7636(12) 1.2298(9) 0.7642(4) 0.084(3) Uani 1 1 d . . . H29 H 0.7990 1.2928 0.7652 0.101 Uiso 1 1 calc R . . C30 C 0.8450(11) 1.1405(10) 0.7753(4) 0.086(3) Uani 1 1 d . . . H30 H 0.9364 1.1408 0.7842 0.103 Uiso 1 1 calc R . . C31 C 0.7842(11) 1.0477(8) 0.7726(4) 0.062(3) Uani 1 1 d . . . H31 H 0.8383 0.9867 0.7800 0.074 Uiso 1 1 calc R . . C32 C 0.5334(8) 0.8301(6) 0.8605(4) 0.053(2) Uani 1 1 d . . . C33 C 0.2608(10) 0.8360(6) 1.0052(4) 0.055(2) Uani 1 1 d . . . H33 H 0.2363 0.7935 0.9813 0.066 Uiso 1 1 calc R . . C34 C 0.1641(10) 0.9092(8) 1.0193(4) 0.069(3) Uani 1 1 d . . . H34 H 0.0751 0.9146 1.0068 0.083 Uiso 1 1 calc R . . C35 C 0.2036(11) 0.9728(7) 1.0520(4) 0.073(3) Uani 1 1 d . . . H35 H 0.1420 1.0242 1.0616 0.088 Uiso 1 1 calc R . . C36 C 0.3378(11) 0.9615(6) 1.0717(4) 0.062(3) Uani 1 1 d . . . H36 H 0.3642 1.0053 1.0944 0.074 Uiso 1 1 calc R . . C37 C 0.4302(10) 0.8859(6) 1.0576(4) 0.047(2) Uani 1 1 d . . . C38 C 0.5728(10) 0.8686(7) 1.0734(4) 0.049(2) Uani 1 1 d . . . C39 C 0.6280(12) 0.9232(7) 1.1081(4) 0.063(3) Uani 1 1 d . . . H39 H 0.5763 0.9754 1.1221 0.076 Uiso 1 1 calc R . . C40 C 0.7604(13) 0.8990(8) 1.1216(4) 0.076(3) Uani 1 1 d . . . H40 H 0.7996 0.9356 1.1452 0.091 Uiso 1 1 calc R . . C41 C 0.8383(10) 0.8229(8) 1.1017(4) 0.071(3) Uani 1 1 d . . . H41 H 0.9288 0.8062 1.1116 0.085 Uiso 1 1 calc R . . C42 C 0.7749(11) 0.7708(6) 1.0654(4) 0.063(3) Uani 1 1 d . . . H42 H 0.8262 0.7193 1.0505 0.075 Uiso 1 1 calc R . . C43 C 0.3516(12) 0.6029(7) 1.1250(5) 0.084(3) Uani 1 1 d . . . H43 H 0.2911 0.6605 1.1183 0.101 Uiso 1 1 calc R . . C44 C 0.3262(13) 0.5248(9) 1.1791(5) 0.106(4) Uani 1 1 d . . . H44 H 0.2508 0.5292 1.2090 0.128 Uiso 1 1 calc R . . C45 C 0.4177(16) 0.4384(9) 1.1879(5) 0.115(5) Uani 1 1 d . . . H45 H 0.4041 0.3844 1.2243 0.138 Uiso 1 1 calc R . . C46 C 0.5252(14) 0.4329(8) 1.1439(5) 0.101(4) Uani 1 1 d . . . H46 H 0.5845 0.3746 1.1496 0.121 Uiso 1 1 calc R . . C47 C 0.5482(11) 0.5148(7) 1.0895(4) 0.055(2) Uani 1 1 d . . . C48 C 0.6573(10) 0.5175(7) 1.0386(4) 0.059(3) Uani 1 1 d . . . C49 C 0.7564(12) 0.4357(7) 1.0388(6) 0.080(3) Uani 1 1 d . . . H49 H 0.7541 0.3767 1.0725 0.096 Uiso 1 1 calc R . . C50 C 0.8561(12) 0.4458(8) 0.9881(6) 0.092(4) Uani 1 1 d . . . H50 H 0.9234 0.3932 0.9873 0.110 Uiso 1 1 calc R . . C51 C 0.8583(10) 0.5333(9) 0.9379(5) 0.081(3) Uani 1 1 d . . . H51 H 0.9252 0.5396 0.9031 0.097 Uiso 1 1 calc R . . C52 C 0.7571(10) 0.6121(7) 0.9406(5) 0.070(3) Uani 1 1 d . . . H52 H 0.7564 0.6708 0.9069 0.084 Uiso 1 1 calc R . . Cl1 Cl 0.0217(5) 0.7666(3) 0.4553(2) 0.1091(12) Uani 1 1 d . . . Cl2 Cl 0.1260(8) 0.4411(4) 0.7851(3) 0.181(2) Uani 1 1 d . . . Cl3 Cl 0.0374(3) 0.8171(2) 0.87170(12) 0.0668(7) Uani 1 1 d . . . N1 N 0.6539(10) 0.6125(6) 0.6270(3) 0.067(2) Uani 1 1 d . . . N2 N 0.4128(10) 0.5789(6) 0.5967(3) 0.071(2) Uani 1 1 d . . . N3 N 0.4835(11) 0.8154(6) 0.5369(4) 0.074(3) Uani 1 1 d . . . N4 N 0.2840(8) 0.7671(6) 0.6324(4) 0.060(2) Uani 1 1 d . . . N5 N 0.5366(8) 0.7774(5) 0.6804(3) 0.069(2) Uani 1 1 d . . . N6 N 0.3932(8) 1.0194(5) 0.7460(3) 0.0524(19) Uani 1 1 d . . . N7 N 0.6552(8) 1.0428(5) 0.7601(3) 0.056(2) Uani 1 1 d . . . N8 N 0.5268(7) 0.7840(5) 0.9132(3) 0.058(2) Uani 1 1 d . . . N9 N 0.3880(7) 0.8232(5) 1.0241(3) 0.0451(18) Uani 1 1 d . . . N10 N 0.6457(8) 0.7920(5) 1.0516(3) 0.0473(18) Uani 1 1 d . . . N11 N 0.4605(9) 0.5997(5) 1.0811(3) 0.060(2) Uani 1 1 d . . . N12 N 0.6616(7) 0.6051(5) 0.9906(3) 0.0526(19) Uani 1 1 d . . . O1 O -0.0627(16) 0.7035(13) 0.4518(13) 0.368(15) Uani 1 1 d . . . O2 O 0.048(3) 0.800(3) 0.4031(9) 0.47(2) Uani 1 1 d . . . O3 O 0.1379(15) 0.7281(8) 0.4754(7) 0.292(9) Uani 1 1 d . . . O4 O -0.0278(15) 0.8449(14) 0.4754(11) 0.335(12) Uani 1 1 d . . . O5 O 0.0402(17) 0.3693(10) 0.7912(9) 0.329(12) Uani 1 1 d . . . O6 O 0.231(3) 0.4608(16) 0.7344(9) 0.451(18) Uani 1 1 d . . . O7 O 0.060(2) 0.5311(12) 0.7802(8) 0.382(13) Uani 1 1 d . . . O8 O 0.219(3) 0.4198(15) 0.8230(9) 0.53(2) Uani 1 1 d . . . O9 O -0.0626(9) 0.7918(6) 0.8381(3) 0.135(3) Uani 1 1 d . . . O10 O 0.1643(8) 0.7771(7) 0.8542(4) 0.158(4) Uani 1 1 d . . . O11 O 0.0412(8) 0.9248(6) 0.8547(4) 0.125(3) Uani 1 1 d . . . O12 O -0.0022(7) 0.7773(6) 0.9367(3) 0.106(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0968(10) 0.0458(7) 0.0499(7) -0.0143(6) -0.0093(6) -0.0024(6) Cu2 0.0855(9) 0.0464(7) 0.0483(7) -0.0110(5) -0.0148(6) 0.0044(6) Cu3 0.0639(8) 0.0360(6) 0.0451(7) -0.0074(5) -0.0138(5) 0.0051(5) C1 0.076(10) 0.095(10) 0.116(10) -0.041(8) -0.008(8) 0.016(8) C2 0.097(11) 0.101(10) 0.101(9) -0.033(8) -0.027(7) -0.007(9) C3 0.105(12) 0.107(12) 0.099(10) -0.007(8) -0.010(8) -0.002(9) C4 0.130(12) 0.043(7) 0.102(9) -0.007(6) -0.003(9) 0.013(8) C5 0.098(10) 0.054(7) 0.046(6) -0.002(5) -0.008(6) -0.009(7) C6 0.115(10) 0.026(6) 0.064(7) -0.009(5) -0.005(6) 0.001(6) C7 0.116(11) 0.052(7) 0.093(8) -0.033(6) 0.002(8) -0.004(7) C8 0.141(13) 0.054(8) 0.105(10) -0.033(7) 0.006(9) -0.027(9) C9 0.112(10) 0.092(9) 0.081(8) -0.037(7) -0.018(7) -0.020(8) C10 0.123(11) 0.064(7) 0.062(7) -0.033(6) 0.006(7) -0.018(7) C11 0.176(13) 0.079(8) 0.048(7) -0.028(7) 0.026(8) -0.030(8) C12 0.32(3) 0.071(12) 0.073(12) -0.035(10) 0.054(14) -0.073(13) C13 0.32(3) 0.066(12) 0.072(11) -0.002(10) -0.044(16) -0.022(13) C14 0.212(17) 0.084(10) 0.072(9) -0.006(8) -0.062(10) -0.021(10) C15 0.133(12) 0.043(7) 0.061(8) -0.022(6) -0.019(8) -0.014(7) C16 0.100(9) 0.053(7) 0.062(8) -0.027(6) -0.037(7) 0.001(6) C17 0.116(13) 0.096(10) 0.130(14) -0.047(10) -0.055(10) 0.029(10) C18 0.123(15) 0.158(17) 0.18(2) -0.107(15) -0.076(14) 0.046(13) C19 0.071(11) 0.188(18) 0.171(17) -0.135(14) 0.008(11) -0.015(11) C20 0.118(11) 0.083(9) 0.063(8) -0.029(6) 0.000(8) -0.028(8) C21 0.101(8) 0.047(6) 0.034(5) -0.006(5) -0.017(5) 0.000(5) C22 0.065(7) 0.051(6) 0.041(5) -0.007(4) -0.009(5) 0.000(6) C23 0.058(7) 0.108(10) 0.061(7) -0.029(7) -0.005(5) 0.000(7) C24 0.089(10) 0.079(9) 0.071(7) -0.008(6) -0.011(7) 0.014(7) C25 0.082(8) 0.053(7) 0.066(7) 0.004(5) -0.008(6) -0.008(6) C26 0.059(7) 0.046(6) 0.046(6) -0.006(5) -0.003(5) 0.008(5) C27 0.060(7) 0.051(6) 0.044(5) -0.002(5) -0.005(5) -0.006(6) C28 0.087(9) 0.054(7) 0.078(7) -0.018(5) -0.011(6) 0.001(6) C29 0.078(9) 0.075(9) 0.087(8) -0.002(6) -0.005(7) -0.015(7) C30 0.083(9) 0.102(10) 0.077(8) -0.035(7) -0.002(6) -0.010(8) C31 0.055(7) 0.068(7) 0.067(6) -0.022(5) -0.016(5) 0.007(6) C32 0.062(7) 0.046(6) 0.051(6) -0.018(5) 0.001(5) 0.005(5) C33 0.058(7) 0.038(5) 0.067(6) -0.011(5) -0.004(5) -0.004(5) C34 0.065(7) 0.075(8) 0.064(7) -0.020(6) 0.000(5) 0.002(6) C35 0.090(9) 0.063(7) 0.056(7) -0.005(5) -0.014(6) 0.038(6) C36 0.098(9) 0.041(6) 0.048(6) -0.013(5) -0.006(6) -0.003(6) C37 0.063(7) 0.036(5) 0.040(5) -0.005(4) -0.003(5) -0.002(5) C38 0.068(7) 0.041(6) 0.034(5) -0.002(4) -0.004(5) -0.005(5) C39 0.093(9) 0.049(6) 0.053(6) -0.014(5) -0.021(6) -0.006(6) C40 0.113(10) 0.059(7) 0.050(6) 0.005(5) -0.021(7) -0.026(7) C41 0.058(7) 0.083(8) 0.065(7) -0.003(6) -0.018(6) -0.001(6) C42 0.093(9) 0.042(6) 0.060(6) -0.014(5) -0.032(6) -0.002(6) C43 0.136(10) 0.055(7) 0.051(7) 0.002(6) -0.001(7) -0.021(7) C44 0.182(13) 0.062(8) 0.061(8) -0.002(6) 0.016(7) -0.021(8) C45 0.238(16) 0.048(8) 0.048(8) 0.004(6) -0.003(9) -0.020(9) C46 0.203(14) 0.052(7) 0.046(7) -0.004(6) -0.034(8) 0.002(8) C47 0.092(8) 0.032(5) 0.043(6) -0.003(5) -0.031(6) -0.012(5) C48 0.077(8) 0.039(6) 0.063(7) -0.008(5) -0.036(6) 0.010(5) C49 0.093(9) 0.033(6) 0.113(10) -0.003(6) -0.039(7) -0.007(6) C50 0.085(10) 0.045(7) 0.148(12) -0.015(8) -0.048(9) 0.006(6) C51 0.055(7) 0.085(9) 0.111(9) -0.044(8) -0.004(6) 0.008(6) C52 0.069(7) 0.057(7) 0.085(8) -0.026(6) -0.004(6) 0.009(6) Cl1 0.143(4) 0.078(2) 0.123(3) -0.032(2) -0.069(3) 0.008(2) Cl2 0.321(8) 0.073(3) 0.152(4) -0.006(3) -0.082(5) -0.011(4) Cl3 0.073(2) 0.0613(18) 0.0634(18) -0.0126(14) -0.0108(15) 0.0057(14) N1 0.081(7) 0.048(5) 0.071(6) -0.019(4) -0.006(5) 0.001(5) N2 0.106(8) 0.055(6) 0.054(5) -0.012(4) -0.015(5) -0.026(6) N3 0.125(8) 0.049(5) 0.054(6) -0.028(4) 0.009(6) -0.018(5) N4 0.078(6) 0.056(5) 0.055(5) -0.027(4) -0.013(5) -0.007(4) N5 0.108(7) 0.049(5) 0.047(5) -0.001(4) -0.033(5) 0.011(5) N6 0.063(6) 0.048(5) 0.046(5) -0.009(4) -0.010(4) -0.002(4) N7 0.057(6) 0.056(5) 0.053(5) -0.008(4) -0.010(4) -0.009(4) N8 0.087(6) 0.032(4) 0.047(5) -0.002(4) -0.002(4) 0.007(4) N9 0.046(5) 0.042(4) 0.039(4) 0.002(3) -0.005(4) 0.007(4) N10 0.060(5) 0.034(4) 0.046(4) 0.001(3) -0.021(4) -0.003(4) N11 0.100(7) 0.035(5) 0.041(5) 0.002(4) -0.020(5) -0.013(4) N12 0.071(6) 0.032(4) 0.054(5) -0.006(4) -0.019(4) 0.005(4) O1 0.212(15) 0.206(16) 0.76(5) -0.24(2) -0.07(2) -0.057(12) O2 0.42(3) 0.67(5) 0.199(17) 0.10(2) -0.12(2) 0.13(3) O3 0.365(18) 0.139(9) 0.46(2) -0.121(11) -0.350(17) 0.126(11) O4 0.255(16) 0.262(17) 0.63(4) -0.31(2) -0.185(19) 0.105(14) O5 0.35(2) 0.094(10) 0.59(3) -0.043(14) -0.31(2) 0.049(11) O6 0.66(4) 0.29(2) 0.31(2) -0.083(18) 0.27(3) 0.03(2) O7 0.64(3) 0.125(12) 0.34(2) -0.076(13) 0.16(2) -0.118(17) O8 0.78(4) 0.36(2) 0.44(3) 0.22(2) -0.53(3) -0.35(3) O9 0.170(8) 0.145(8) 0.097(6) -0.027(5) -0.032(6) -0.059(6) O10 0.116(7) 0.160(8) 0.143(7) 0.020(6) 0.024(6) 0.084(6) O11 0.148(7) 0.066(5) 0.144(7) -0.014(5) 0.015(5) 0.001(5) O12 0.116(6) 0.145(7) 0.045(4) -0.001(4) -0.002(4) -0.027(5) _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 N5 1.961(8) . ? Cu1 N1 2.007(8) . ? Cu1 N2 2.025(8) . ? Cu1 N4 2.030(7) . ? Cu1 N3 2.159(8) . ? Cu2 C32 1.896(9) . ? Cu2 C21 1.896(9) . ? Cu2 N6 2.097(7) . ? Cu2 N7 2.105(7) . ? Cu3 N8 1.969(7) . ? Cu3 N12 1.969(7) . ? Cu3 N9 2.003(6) . ? Cu3 N11 2.045(7) . ? Cu3 N10 2.139(7) . ? C1 N1 1.305(12) . ? C1 C2 1.359(13) . ? C1 H1 0.9300 . ? C2 C3 1.400(15) . ? C2 H2 0.9300 . ? C3 C4 1.354(14) . ? C3 H3 0.9300 . ? C4 C5 1.387(13) . ? C4 H4 0.9300 . ? C5 N1 1.360(11) . ? C5 C6 1.467(13) . ? C6 N2 1.367(11) . ? C6 C7 1.381(13) . ? C7 C8 1.332(13) . ? C7 H7 0.9300 . ? C8 C9 1.360(13) . ? C8 H8 0.9300 . ? C9 C10 1.381(12) . ? C9 H9 0.9300 . ? C10 N2 1.322(11) . ? C10 H10 0.9300 . ? C11 N3 1.337(11) . ? C11 C12 1.392(16) . ? C11 H11 0.9300 . ? C12 C13 1.31(2) . ? C12 H12 0.9300 . ? C13 C14 1.39(2) . ? C13 H13 0.9300 . ? C14 C15 1.383(13) . ? C14 H14 0.9300 . ? C15 N3 1.329(11) . ? C15 C16 1.492(13) . ? C16 C17 1.339(14) . ? C16 N4 1.363(10) . ? C17 C18 1.352(17) . ? C17 H17 0.9300 . ? C18 C19 1.339(17) . ? C18 H18 0.9300 . ? C19 C20 1.397(15) . ? C19 H19 0.9300 . ? C20 N4 1.361(11) . ? C20 H20 0.9300 . ? C21 N5 1.162(9) . ? C22 N6 1.312(9) . ? C22 C23 1.372(11) . ? C22 H22 0.9300 . ? C23 C24 1.371(12) . ? C23 H23 0.9300 . ? C24 C25 1.357(12) . ? C24 H24 0.9300 . ? C25 C26 1.404(11) . ? C25 H25 0.9300 . ? C26 N6 1.358(10) . ? C26 C27 1.484(11) . ? C27 N7 1.357(10) . ? C27 C28 1.364(11) . ? C28 C29 1.379(11) . ? C28 H28 0.9300 . ? C29 C30 1.373(12) . ? C29 H29 0.9300 . ? C30 C31 1.416(12) . ? C30 H30 0.9300 . ? C31 N7 1.319(9) . ? C31 H31 0.9300 . ? C32 N8 1.166(8) . ? C33 N9 1.338(9) . ? C33 C34 1.380(11) . ? C33 H33 0.9300 . ? C34 C35 1.353(12) . ? C34 H34 0.9300 . ? C35 C36 1.410(11) . ? C35 H35 0.9300 . ? C36 C37 1.380(10) . ? C36 H36 0.9300 . ? C37 N9 1.367(10) . ? C37 C38 1.456(11) . ? C38 C39 1.363(11) . ? C38 N10 1.365(9) . ? C39 C40 1.353(12) . ? C39 H39 0.9300 . ? C40 C41 1.361(12) . ? C40 H40 0.9300 . ? C41 C42 1.408(12) . ? C41 H41 0.9300 . ? C42 N10 1.322(9) . ? C42 H42 0.9300 . ? C43 N11 1.346(11) . ? C43 C44 1.372(11) . ? C43 H43 0.9300 . ? C44 C45 1.398(14) . ? C44 H44 0.9300 . ? C45 C46 1.344(14) . ? C45 H45 0.9300 . ? C46 C47 1.401(11) . ? C46 H46 0.9300 . ? C47 N11 1.361(10) . ? C47 C48 1.438(11) . ? C48 N12 1.356(9) . ? C48 C49 1.408(12) . ? C49 C50 1.369(12) . ? C49 H49 0.9300 . ? C50 C51 1.382(12) . ? C50 H50 0.9300 . ? C51 C52 1.402(11) . ? C51 H51 0.9300 . ? C52 N12 1.334(9) . ? C52 H52 0.9300 . ? Cl1 O2 1.128(17) . ? Cl1 O1 1.227(13) . ? Cl1 O4 1.286(12) . ? Cl1 O3 1.291(10) . ? Cl2 O5 1.269(14) . ? Cl2 O8 1.280(12) . ? Cl2 O7 1.310(18) . ? Cl2 O6 1.395(16) . ? Cl3 O10 1.360(7) . ? Cl3 O11 1.385(7) . ? Cl3 O9 1.401(7) . ? Cl3 O12 1.412(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cu1 N1 92.9(3) . . ? N5 Cu1 N2 160.4(3) . . ? N1 Cu1 N2 80.3(4) . . ? N5 Cu1 N4 89.6(3) . . ? N1 Cu1 N4 171.6(3) . . ? N2 Cu1 N4 94.8(3) . . ? N5 Cu1 N3 101.9(3) . . ? N1 Cu1 N3 109.0(4) . . ? N2 Cu1 N3 97.7(3) . . ? N4 Cu1 N3 78.2(4) . . ? C32 Cu2 C21 117.9(3) . . ? C32 Cu2 N6 118.6(3) . . ? C21 Cu2 N6 103.2(3) . . ? C32 Cu2 N7 110.0(3) . . ? C21 Cu2 N7 122.9(3) . . ? N6 Cu2 N7 77.7(3) . . ? N8 Cu3 N12 94.7(3) . . ? N8 Cu3 N9 90.1(3) . . ? N12 Cu3 N9 175.2(3) . . ? N8 Cu3 N11 150.7(3) . . ? N12 Cu3 N11 80.7(3) . . ? N9 Cu3 N11 95.3(3) . . ? N8 Cu3 N10 114.3(3) . . ? N12 Cu3 N10 98.9(3) . . ? N9 Cu3 N10 78.6(3) . . ? N11 Cu3 N10 94.9(2) . . ? N1 C1 C2 123.1(12) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 119.3(12) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 117.6(13) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C3 C4 C5 120.8(13) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? N1 C5 C4 119.9(11) . . ? N1 C5 C6 115.6(10) . . ? C4 C5 C6 124.5(12) . . ? N2 C6 C7 119.8(11) . . ? N2 C6 C5 113.4(10) . . ? C7 C6 C5 126.7(11) . . ? C8 C7 C6 120.5(12) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 120.7(12) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C10 117.4(12) . . ? C8 C9 H9 121.3 . . ? C10 C9 H9 121.3 . . ? N2 C10 C9 123.3(11) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N3 C11 C12 118.2(14) . . ? N3 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? C13 C12 C11 123(2) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 C13 C14 119.2(19) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C15 C14 C13 117.7(15) . . ? C15 C14 H14 121.1 . . ? C13 C14 H14 121.1 . . ? N3 C15 C14 121.6(12) . . ? N3 C15 C16 116.6(10) . . ? C14 C15 C16 121.7(14) . . ? C17 C16 N4 122.8(11) . . ? C17 C16 C15 123.5(12) . . ? N4 C16 C15 113.7(10) . . ? C16 C17 C18 119.6(15) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 120.3(19) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 119.7(17) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N4 C20 C19 120.2(12) . . ? N4 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? N5 C21 Cu2 167.0(9) . . ? N6 C22 C23 124.2(9) . . ? N6 C22 H22 117.9 . . ? C23 C22 H22 117.9 . . ? C24 C23 C22 117.7(10) . . ? C24 C23 H23 121.1 . . ? C22 C23 H23 121.1 . . ? C25 C24 C23 120.6(10) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 118.0(10) . . ? C24 C25 H25 121.0 . . ? C26 C25 H25 121.0 . . ? N6 C26 C25 121.6(9) . . ? N6 C26 C27 116.7(8) . . ? C25 C26 C27 121.7(9) . . ? N7 C27 C28 122.3(9) . . ? N7 C27 C26 113.1(9) . . ? C28 C27 C26 124.5(10) . . ? C27 C28 C29 120.1(10) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 119.0(11) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C31 117.3(11) . . ? C29 C30 H30 121.4 . . ? C31 C30 H30 121.4 . . ? N7 C31 C30 123.9(9) . . ? N7 C31 H31 118.1 . . ? C30 C31 H31 118.1 . . ? N8 C32 Cu2 179.5(8) . . ? N9 C33 C34 123.1(9) . . ? N9 C33 H33 118.4 . . ? C34 C33 H33 118.4 . . ? C35 C34 C33 117.5(10) . . ? C35 C34 H34 121.3 . . ? C33 C34 H34 121.3 . . ? C34 C35 C36 120.2(9) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C37 C36 C35 120.3(9) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? N9 C37 C36 118.2(9) . . ? N9 C37 C38 116.1(8) . . ? C36 C37 C38 125.6(9) . . ? C39 C38 N10 122.9(9) . . ? C39 C38 C37 122.6(9) . . ? N10 C38 C37 114.5(8) . . ? C40 C39 C38 117.9(10) . . ? C40 C39 H39 121.1 . . ? C38 C39 H39 121.1 . . ? C39 C40 C41 122.2(10) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C40 C41 C42 116.7(10) . . ? C40 C41 H41 121.7 . . ? C42 C41 H41 121.7 . . ? N10 C42 C41 122.8(9) . . ? N10 C42 H42 118.6 . . ? C41 C42 H42 118.6 . . ? N11 C43 C44 122.8(11) . . ? N11 C43 H43 118.6 . . ? C44 C43 H43 118.6 . . ? C43 C44 C45 117.7(11) . . ? C43 C44 H44 121.2 . . ? C45 C44 H44 121.2 . . ? C46 C45 C44 120.3(10) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 120.3(11) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? N11 C47 C46 119.7(10) . . ? N11 C47 C48 114.7(8) . . ? C46 C47 C48 125.6(10) . . ? N12 C48 C49 121.6(10) . . ? N12 C48 C47 116.0(8) . . ? C49 C48 C47 122.4(9) . . ? C50 C49 C48 117.9(10) . . ? C50 C49 H49 121.0 . . ? C48 C49 H49 121.0 . . ? C49 C50 C51 120.9(11) . . ? C49 C50 H50 119.6 . . ? C51 C50 H50 119.6 . . ? C50 C51 C52 118.4(10) . . ? C50 C51 H51 120.8 . . ? C52 C51 H51 120.8 . . ? N12 C52 C51 121.6(9) . . ? N12 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? O2 Cl1 O1 96.2(16) . . ? O2 Cl1 O4 104.1(15) . . ? O1 Cl1 O4 116.9(11) . . ? O2 Cl1 O3 105.6(14) . . ? O1 Cl1 O3 116.1(10) . . ? O4 Cl1 O3 114.6(9) . . ? O5 Cl2 O8 115.2(10) . . ? O5 Cl2 O7 110.7(13) . . ? O8 Cl2 O7 116.1(15) . . ? O5 Cl2 O6 119.6(14) . . ? O8 Cl2 O6 89.9(16) . . ? O7 Cl2 O6 103.7(10) . . ? O10 Cl3 O11 109.6(5) . . ? O10 Cl3 O9 109.5(6) . . ? O11 Cl3 O9 105.6(5) . . ? O10 Cl3 O12 110.5(5) . . ? O11 Cl3 O12 111.8(5) . . ? O9 Cl3 O12 109.7(4) . . ? C1 N1 C5 119.4(10) . . ? C1 N1 Cu1 125.5(8) . . ? C5 N1 Cu1 114.9(8) . . ? C10 N2 C6 118.2(10) . . ? C10 N2 Cu1 126.5(8) . . ? C6 N2 Cu1 115.3(8) . . ? C15 N3 C11 120.5(10) . . ? C15 N3 Cu1 112.8(7) . . ? C11 N3 Cu1 126.2(9) . . ? C20 N4 C16 117.3(9) . . ? C20 N4 Cu1 124.6(8) . . ? C16 N4 Cu1 117.8(8) . . ? C21 N5 Cu1 172.5(9) . . ? C22 N6 C26 117.6(8) . . ? C22 N6 Cu2 127.1(6) . . ? C26 N6 Cu2 115.0(6) . . ? C31 N7 C27 117.3(8) . . ? C31 N7 Cu2 125.0(7) . . ? C27 N7 Cu2 116.4(6) . . ? C32 N8 Cu3 175.0(7) . . ? C33 N9 C37 120.5(7) . . ? C33 N9 Cu3 122.2(6) . . ? C37 N9 Cu3 117.2(6) . . ? C42 N10 C38 117.6(8) . . ? C42 N10 Cu3 128.7(6) . . ? C38 N10 Cu3 113.6(6) . . ? C43 N11 C47 119.3(8) . . ? C43 N11 Cu3 127.6(7) . . ? C47 N11 Cu3 112.9(6) . . ? C52 N12 C48 119.5(8) . . ? C52 N12 Cu3 125.4(6) . . ? C48 N12 Cu3 115.0(6) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.553 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.089 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 752338' #TrackingRef '- 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H16 Cu N5, Cl O4' _chemical_formula_sum 'C21 H16 Cl Cu N5 O4' _chemical_formula_weight 501.38 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.304(3) _cell_length_b 11.451(2) _cell_length_c 14.804(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.524(3) _cell_angle_gamma 90.00 _cell_volume 2112.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2259 _cell_measurement_theta_min 2.307 _cell_measurement_theta_max 21.266 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 1.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8500 _exptl_absorpt_correction_T_max 0.8894 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; The structure was solved by direct methods (Bruker, 2000) and successive difference Fourier syntheses. ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10390 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3721 _reflns_number_gt 2247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1212P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3721 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1935 _refine_ls_wR_factor_gt 0.1747 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.76471(5) 0.47359(6) 0.00883(4) 0.0575(3) Uani 1 1 d . . . C1 C 0.9098(5) 0.5498(5) 0.2151(4) 0.0758(17) Uani 1 1 d . . . H1 H 0.8524 0.5952 0.2166 0.091 Uiso 1 1 calc R . . C2 C 1.0021(6) 0.5463(6) 0.2952(5) 0.090(2) Uani 1 1 d . . . H2 H 1.0058 0.5864 0.3509 0.108 Uiso 1 1 calc R . . C3 C 1.0869(6) 0.4843(7) 0.2924(5) 0.091(2) Uani 1 1 d . . . H3 H 1.1503 0.4841 0.3456 0.109 Uiso 1 1 calc R . . C4 C 1.0807(5) 0.4222(6) 0.2127(5) 0.0804(18) Uani 1 1 d . . . H4 H 1.1389 0.3784 0.2110 0.097 Uiso 1 1 calc R . . C5 C 0.9852(4) 0.4252(5) 0.1329(4) 0.0600(13) Uani 1 1 d . . . C6 C 0.9676(4) 0.3603(4) 0.0439(4) 0.0594(13) Uani 1 1 d . . . C7 C 1.0458(5) 0.2931(5) 0.0290(5) 0.0764(17) Uani 1 1 d . . . H7 H 1.1143 0.2890 0.0754 0.092 Uiso 1 1 calc R . . C8 C 1.0204(6) 0.2318(6) -0.0565(6) 0.092(2) Uani 1 1 d . . . H8 H 1.0709 0.1831 -0.0674 0.110 Uiso 1 1 calc R . . C9 C 0.9220(6) 0.2430(5) -0.1241(5) 0.0848(19) Uani 1 1 d . . . H9 H 0.9048 0.2040 -0.1827 0.102 Uiso 1 1 calc R . . C10 C 0.8471(5) 0.3126(5) -0.1056(4) 0.0748(16) Uani 1 1 d . . . H10 H 0.7792 0.3200 -0.1525 0.090 Uiso 1 1 calc R . . C11 C 0.6956(4) 0.2301(5) 0.0640(4) 0.0701(15) Uani 1 1 d . . . H11 H 0.7402 0.1976 0.0344 0.084 Uiso 1 1 calc R . . C12 C 0.6419(5) 0.1572(5) 0.1050(5) 0.0799(17) Uani 1 1 d . . . H12 H 0.6506 0.0767 0.1035 0.096 Uiso 1 1 calc R . . C13 C 0.5752(5) 0.2042(6) 0.1484(4) 0.0788(17) Uani 1 1 d . . . H13 H 0.5376 0.1560 0.1759 0.095 Uiso 1 1 calc R . . C14 C 0.5650(4) 0.3225(5) 0.1505(4) 0.0665(14) Uani 1 1 d . . . H14 H 0.5206 0.3562 0.1797 0.080 Uiso 1 1 calc R . . C15 C 0.6219(4) 0.3916(4) 0.1083(3) 0.0507(12) Uani 1 1 d . . . C16 C 0.6152(4) 0.5218(4) 0.1055(3) 0.0490(11) Uani 1 1 d . . . C17 C 0.5547(4) 0.5865(5) 0.1459(4) 0.0643(14) Uani 1 1 d . . . H17 H 0.5151 0.5489 0.1780 0.077 Uiso 1 1 calc R . . C18 C 0.5523(5) 0.7064(5) 0.1392(4) 0.0741(16) Uani 1 1 d . . . H18 H 0.5121 0.7506 0.1669 0.089 Uiso 1 1 calc R . . C19 C 0.6115(5) 0.7592(5) 0.0902(4) 0.0763(16) Uani 1 1 d . . . H19 H 0.6118 0.8400 0.0843 0.092 Uiso 1 1 calc R . . C20 C 0.6701(5) 0.6909(5) 0.0502(4) 0.0710(15) Uani 1 1 d . . . H20 H 0.7088 0.7266 0.0163 0.085 Uiso 1 1 calc R . . C21 C 0.7035(5) 0.5337(5) -0.1232(5) 0.0659(15) Uani 1 1 d . . . Cl1 Cl 0.73708(15) 0.52430(14) 0.40320(11) 0.0783(5) Uani 1 1 d . . . N1 N 0.9005(3) 0.4895(4) 0.1351(3) 0.0577(11) Uani 1 1 d . . . N2 N 0.8690(3) 0.3692(4) -0.0233(3) 0.0587(11) Uani 1 1 d . . . N3 N 0.6860(3) 0.3457(3) 0.0651(3) 0.0536(10) Uani 1 1 d . . . N4 N 0.6728(3) 0.5746(4) 0.0587(3) 0.0577(10) Uani 1 1 d . . . N5 N 0.6626(4) 0.5588(5) -0.2054(5) 0.0852(15) Uani 1 1 d . . . O1 O 0.6932(9) 0.4390(6) 0.3498(5) 0.261(6) Uani 1 1 d . . . O2 O 0.7548(6) 0.6213(7) 0.3561(5) 0.207(4) Uani 1 1 d . . . O3 O 0.8255(9) 0.4846(7) 0.4774(6) 0.227(5) Uani 1 1 d . . . O4 O 0.6867(16) 0.5624(12) 0.4520(14) 0.389(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0591(5) 0.0597(5) 0.0600(5) 0.0018(3) 0.0287(3) 0.0067(3) C1 0.080(4) 0.085(4) 0.064(4) -0.004(3) 0.027(3) -0.012(3) C2 0.099(5) 0.110(6) 0.061(4) 0.000(3) 0.028(4) -0.032(4) C3 0.075(5) 0.124(6) 0.065(4) 0.012(4) 0.015(3) -0.030(4) C4 0.059(4) 0.103(5) 0.081(4) 0.025(4) 0.028(3) -0.012(3) C5 0.047(3) 0.069(3) 0.068(4) 0.016(3) 0.025(3) -0.005(3) C6 0.059(3) 0.054(3) 0.076(4) 0.012(3) 0.037(3) 0.001(2) C7 0.060(3) 0.077(4) 0.101(5) -0.001(4) 0.039(3) 0.004(3) C8 0.078(5) 0.075(4) 0.141(7) 0.003(4) 0.062(5) 0.012(3) C9 0.111(5) 0.059(4) 0.109(5) -0.017(3) 0.068(5) -0.003(4) C10 0.078(4) 0.070(4) 0.081(4) -0.005(3) 0.034(3) 0.005(3) C11 0.070(4) 0.059(3) 0.092(4) 0.002(3) 0.042(3) 0.010(3) C12 0.090(4) 0.050(3) 0.104(5) 0.013(3) 0.041(4) 0.009(3) C13 0.079(4) 0.074(4) 0.091(5) 0.026(3) 0.040(3) 0.002(3) C14 0.068(3) 0.074(4) 0.067(3) 0.009(3) 0.035(3) 0.006(3) C15 0.046(3) 0.055(3) 0.049(3) 0.003(2) 0.015(2) 0.003(2) C16 0.044(3) 0.058(3) 0.041(3) -0.002(2) 0.011(2) -0.001(2) C17 0.062(3) 0.080(4) 0.055(3) -0.011(3) 0.025(3) -0.002(3) C18 0.090(4) 0.065(4) 0.077(4) -0.020(3) 0.042(3) 0.006(3) C19 0.094(4) 0.057(3) 0.082(4) -0.011(3) 0.035(4) 0.005(3) C20 0.076(4) 0.060(3) 0.089(4) -0.002(3) 0.044(3) -0.005(3) C21 0.059(3) 0.068(4) 0.081(4) 0.012(3) 0.038(3) 0.010(3) Cl1 0.0979(12) 0.0789(11) 0.0598(9) -0.0045(8) 0.0296(8) 0.0032(9) N1 0.059(3) 0.065(3) 0.052(3) 0.000(2) 0.023(2) -0.007(2) N2 0.060(3) 0.061(3) 0.062(3) 0.003(2) 0.030(2) 0.004(2) N3 0.052(2) 0.052(2) 0.062(3) 0.005(2) 0.026(2) 0.0040(19) N4 0.061(3) 0.053(2) 0.065(3) 0.001(2) 0.030(2) 0.005(2) N5 0.078(3) 0.085(4) 0.104(4) 0.008(3) 0.046(3) 0.007(3) O1 0.384(13) 0.141(6) 0.117(5) -0.038(5) -0.091(7) 0.003(7) O2 0.235(8) 0.216(8) 0.115(5) 0.050(5) -0.007(5) -0.103(7) O3 0.238(10) 0.184(7) 0.150(7) 0.026(5) -0.068(7) -0.048(6) O4 0.57(3) 0.247(13) 0.59(2) 0.120(15) 0.50(2) 0.171(16) _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 C21 1.959(7) . ? Cu1 N4 2.003(4) . ? Cu1 N2 2.011(4) . ? Cu1 N1 2.103(4) . ? Cu1 N3 2.132(4) . ? C1 N1 1.339(7) . ? C1 C2 1.376(8) . ? C1 H1 0.9300 . ? C2 C3 1.346(10) . ? C2 H2 0.9300 . ? C3 C4 1.356(10) . ? C3 H3 0.9300 . ? C4 C5 1.399(7) . ? C4 H4 0.9300 . ? C5 N1 1.355(7) . ? C5 C6 1.460(7) . ? C6 N2 1.344(6) . ? C6 C7 1.372(7) . ? C7 C8 1.383(9) . ? C7 H7 0.9300 . ? C8 C9 1.346(9) . ? C8 H8 0.9300 . ? C9 C10 1.376(8) . ? C9 H9 0.9300 . ? C10 N2 1.319(7) . ? C10 H10 0.9300 . ? C11 N3 1.331(6) . ? C11 C12 1.371(7) . ? C11 H11 0.9300 . ? C12 C13 1.375(8) . ? C12 H12 0.9300 . ? C13 C14 1.362(8) . ? C13 H13 0.9300 . ? C14 C15 1.386(7) . ? C14 H14 0.9300 . ? C15 N3 1.339(6) . ? C15 C16 1.494(7) . ? C16 N4 1.344(6) . ? C16 C17 1.376(7) . ? C17 C18 1.375(8) . ? C17 H17 0.9300 . ? C18 C19 1.384(8) . ? C18 H18 0.9300 . ? C19 C20 1.376(7) . ? C19 H19 0.9300 . ? C20 N4 1.337(7) . ? C20 H20 0.9300 . ? C21 N5 1.182(7) . ? Cl1 O4 1.225(10) . ? Cl1 O1 1.263(6) . ? Cl1 O2 1.375(7) . ? Cl1 O3 1.376(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 C21 Cu1 N4 94.0(2) . . ? C21 Cu1 N2 93.0(2) . . ? N4 Cu1 N2 172.60(17) . . ? C21 Cu1 N1 141.6(2) . . ? N4 Cu1 N1 93.87(17) . . ? N2 Cu1 N1 79.21(17) . . ? C21 Cu1 N3 122.8(2) . . ? N4 Cu1 N3 78.80(17) . . ? N2 Cu1 N3 99.11(16) . . ? N1 Cu1 N3 95.66(15) . . ? N1 C1 C2 121.7(6) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 119.6(7) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 120.5(6) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C5 118.8(7) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 120.7(6) . . ? N1 C5 C6 115.3(4) . . ? C4 C5 C6 124.1(6) . . ? N2 C6 C7 121.5(5) . . ? N2 C6 C5 115.8(5) . . ? C7 C6 C5 122.7(5) . . ? C6 C7 C8 118.4(6) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C9 C8 C7 119.6(6) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.4(6) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N2 C10 C9 121.8(6) . . ? N2 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? N3 C11 C12 122.2(5) . . ? N3 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C11 C12 C13 119.4(5) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 119.1(6) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 118.8(5) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N3 C15 C14 122.1(5) . . ? N3 C15 C16 114.8(4) . . ? C14 C15 C16 123.1(5) . . ? N4 C16 C17 120.5(5) . . ? N4 C16 C15 115.1(4) . . ? C17 C16 C15 124.4(5) . . ? C18 C17 C16 120.6(6) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 118.1(5) . . ? C17 C18 H18 121.0 . . ? C19 C18 H18 121.0 . . ? C20 C19 C18 119.4(5) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? N4 C20 C19 121.7(5) . . ? N4 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? N5 C21 Cu1 173.3(5) . . ? O4 Cl1 O1 114.6(12) . . ? O4 Cl1 O2 103.7(7) . . ? O1 Cl1 O2 115.6(6) . . ? O4 Cl1 O3 98.0(11) . . ? O1 Cl1 O3 108.8(5) . . ? O2 Cl1 O3 114.9(5) . . ? C1 N1 C5 118.7(5) . . ? C1 N1 Cu1 128.0(4) . . ? C5 N1 Cu1 113.2(3) . . ? C10 N2 C6 119.2(5) . . ? C10 N2 Cu1 124.3(4) . . ? C6 N2 Cu1 116.5(4) . . ? C11 N3 C15 118.4(4) . . ? C11 N3 Cu1 128.0(4) . . ? C15 N3 Cu1 113.5(3) . . ? C20 N4 C16 119.7(5) . . ? C20 N4 Cu1 122.7(4) . . ? C16 N4 Cu1 117.5(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.928 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.091 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 752339' #TrackingRef '- 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H40 Cu3 N12, 2(C2 H6 O), 3(Cl O4)' _chemical_formula_sum 'C66 H52 Cl3 Cu3 N12 O14' _chemical_formula_weight 1534.17 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 13.0200(12) _cell_length_b 23.760(2) _cell_length_c 21.3761(19) _cell_angle_alpha 90.00 _cell_angle_beta 96.296(2) _cell_angle_gamma 90.00 _cell_volume 6572.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2549 _cell_measurement_theta_min 2.327 _cell_measurement_theta_max 17.816 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3128 _exptl_absorpt_coefficient_mu 1.160 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8545 _exptl_absorpt_correction_T_max 0.8928 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; The structure was solved by direct methods (Bruker, 2000) and successive difference Fourier syntheses. ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 32911 _diffrn_reflns_av_R_equivalents 0.0985 _diffrn_reflns_av_sigmaI/netI 0.1639 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11566 _reflns_number_gt 3928 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0106P)^2^+1.9800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11566 _refine_ls_number_parameters 884 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1728 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.885 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.87661(6) 0.99791(3) 0.85886(3) 0.0638(2) Uani 1 1 d . . . Cu2 Cu 0.84106(7) 0.78991(3) 0.83534(3) 0.0715(3) Uani 1 1 d . . . Cu3 Cu 0.89346(6) 0.67645(3) 1.03057(3) 0.0684(3) Uani 1 1 d . . . C1 C 0.6531(6) 0.9929(3) 0.8777(3) 0.076(2) Uani 1 1 d . . . H1A H 0.6728 0.9672 0.9096 0.091 Uiso 1 1 calc R . . C2 C 0.5495(6) 1.0082(3) 0.8674(4) 0.094(2) Uani 1 1 d . . . H2A H 0.5017 0.9942 0.8927 0.113 Uiso 1 1 calc R . . C3 C 0.5200(7) 1.0445(3) 0.8191(5) 0.103(3) Uani 1 1 d . . . H3A H 0.4514 1.0557 0.8113 0.124 Uiso 1 1 calc R . . C4 C 0.5922(7) 1.0647(3) 0.7817(4) 0.080(2) Uani 1 1 d . . . C5 C 0.5691(8) 1.1018(4) 0.7294(5) 0.117(4) Uani 1 1 d . . . H5A H 0.5009 1.1125 0.7179 0.141 Uiso 1 1 calc R . . C6 C 0.6424(10) 1.1214(4) 0.6969(5) 0.122(4) Uani 1 1 d . . . H6A H 0.6243 1.1459 0.6636 0.146 Uiso 1 1 calc R . . C7 C 0.7487(9) 1.1060(3) 0.7115(4) 0.095(3) Uani 1 1 d . . . C8 C 0.8279(11) 1.1256(4) 0.6799(5) 0.126(5) Uani 1 1 d U . . H8A H 0.8137 1.1496 0.6457 0.151 Uiso 1 1 calc R . . C9 C 0.9249(10) 1.1101(4) 0.6981(4) 0.129(4) Uani 1 1 d U . . H9A H 0.9788 1.1242 0.6775 0.155 Uiso 1 1 calc R . . C10 C 0.9457(7) 1.0721(3) 0.7491(4) 0.091(2) Uani 1 1 d . . . H10A H 1.0134 1.0607 0.7608 0.110 Uiso 1 1 calc R . . C11 C 0.7718(7) 1.0696(3) 0.7625(3) 0.066(2) Uani 1 1 d . . . C12 C 0.6952(6) 1.0481(3) 0.7968(3) 0.0636(19) Uani 1 1 d . . . C13 C 0.8331(5) 1.0766(2) 0.9696(3) 0.0597(18) Uani 1 1 d . . . H13A H 0.7633 1.0677 0.9617 0.072 Uiso 1 1 calc R . . C14 C 0.8641(5) 1.1162(3) 1.0159(3) 0.0653(19) Uani 1 1 d . . . H14A H 0.8151 1.1333 1.0382 0.078 Uiso 1 1 calc R . . C15 C 0.9650(6) 1.1300(3) 1.0287(3) 0.0680(19) Uani 1 1 d . . . H15A H 0.9860 1.1564 1.0596 0.082 Uiso 1 1 calc R . . C16 C 1.0371(5) 1.1036(3) 0.9945(3) 0.0561(17) Uani 1 1 d . . . C17 C 1.1455(6) 1.1138(3) 1.0039(3) 0.075(2) Uani 1 1 d . . . H17A H 1.1707 1.1403 1.0336 0.091 Uiso 1 1 calc R . . C18 C 1.2121(5) 1.0864(3) 0.9715(3) 0.073(2) Uani 1 1 d . . . H18A H 1.2822 1.0948 0.9784 0.087 Uiso 1 1 calc R . . C19 C 1.1767(6) 1.0445(3) 0.9265(3) 0.0591(18) Uani 1 1 d . . . C20 C 1.2405(5) 1.0133(3) 0.8924(3) 0.080(2) Uani 1 1 d . . . H20A H 1.3116 1.0188 0.8986 0.096 Uiso 1 1 calc R . . C21 C 1.2005(7) 0.9751(3) 0.8503(3) 0.092(2) Uani 1 1 d . . . H21A H 1.2437 0.9541 0.8274 0.111 Uiso 1 1 calc R . . C22 C 1.0923(6) 0.9671(3) 0.8410(3) 0.079(2) Uani 1 1 d . . . H22A H 1.0648 0.9404 0.8121 0.095 Uiso 1 1 calc R . . C23 C 1.0708(5) 1.0351(3) 0.9157(3) 0.0534(17) Uani 1 1 d . . . C24 C 1.0016(5) 1.0640(2) 0.9498(3) 0.0500(16) Uani 1 1 d . . . C25 C 0.8583(5) 0.8697(3) 0.8357(2) 0.0550(17) Uani 1 1 d . . . C26 C 0.6038(7) 0.7810(3) 0.8445(3) 0.090(2) Uani 1 1 d . . . H26A H 0.6161 0.7970 0.8843 0.107 Uiso 1 1 calc R . . C27 C 0.5031(7) 0.7666(3) 0.8228(5) 0.117(3) Uani 1 1 d . . . H27A H 0.4499 0.7722 0.8479 0.141 Uiso 1 1 calc R . . C28 C 0.4834(7) 0.7442(3) 0.7640(5) 0.109(3) Uani 1 1 d . . . H28A H 0.4162 0.7345 0.7485 0.131 Uiso 1 1 calc R . . C29 C 0.5627(8) 0.7359(3) 0.7279(4) 0.083(2) Uani 1 1 d . . . C30 C 0.5477(8) 0.7123(3) 0.6668(5) 0.106(3) Uani 1 1 d . . . H30A H 0.4810 0.7038 0.6491 0.127 Uiso 1 1 calc R . . C31 C 0.6281(9) 0.7017(3) 0.6336(4) 0.106(3) Uani 1 1 d . . . H31A H 0.6166 0.6851 0.5941 0.127 Uiso 1 1 calc R . . C32 C 0.7289(9) 0.7158(3) 0.6587(4) 0.091(3) Uani 1 1 d . . . C33 C 0.8158(10) 0.7057(4) 0.6271(4) 0.116(4) Uani 1 1 d . . . H33A H 0.8077 0.6891 0.5875 0.139 Uiso 1 1 calc R . . C34 C 0.9116(9) 0.7198(4) 0.6537(4) 0.122(3) Uani 1 1 d . . . H34A H 0.9693 0.7128 0.6327 0.146 Uiso 1 1 calc R . . C35 C 0.9223(7) 0.7456(3) 0.7140(4) 0.096(3) Uani 1 1 d . . . H35A H 0.9882 0.7559 0.7315 0.115 Uiso 1 1 calc R . . C36 C 0.7485(7) 0.7404(3) 0.7188(3) 0.069(2) Uani 1 1 d . . . C37 C 0.6627(7) 0.7501(3) 0.7535(4) 0.068(2) Uani 1 1 d . . . C38 C 0.8844(5) 0.7460(2) 0.9081(3) 0.067(2) Uani 1 1 d . . . C39 C 0.7008(7) 0.7422(3) 1.0401(3) 0.087(2) Uani 1 1 d . . . H39A H 0.7440 0.7707 1.0573 0.105 Uiso 1 1 calc R . . C40 C 0.5945(8) 0.7517(4) 1.0297(4) 0.110(3) Uani 1 1 d . . . H40A H 0.5670 0.7863 1.0396 0.132 Uiso 1 1 calc R . . C41 C 0.5308(7) 0.7093(5) 1.0047(4) 0.110(3) Uani 1 1 d . . . H41A H 0.4599 0.7154 0.9972 0.132 Uiso 1 1 calc R . . C42 C 0.5718(8) 0.6578(4) 0.9906(3) 0.089(2) Uani 1 1 d . . . C43 C 0.5105(7) 0.6123(5) 0.9660(4) 0.119(3) Uani 1 1 d . . . H43A H 0.4391 0.6163 0.9606 0.143 Uiso 1 1 calc R . . C44 C 0.5529(9) 0.5624(4) 0.9500(4) 0.115(3) Uani 1 1 d . . . H44A H 0.5102 0.5332 0.9341 0.138 Uiso 1 1 calc R . . C45 C 0.6631(9) 0.5548(4) 0.9574(4) 0.100(3) Uani 1 1 d . . . C46 C 0.7149(9) 0.5082(4) 0.9368(4) 0.119(3) Uani 1 1 d . . . H46A H 0.6777 0.4775 0.9194 0.143 Uiso 1 1 calc R . . C47 C 0.8189(9) 0.5076(4) 0.9422(4) 0.136(4) Uani 1 1 d . . . H47A H 0.8536 0.4767 0.9280 0.163 Uiso 1 1 calc R . . C48 C 0.8738(6) 0.5529(4) 0.9688(3) 0.106(3) Uani 1 1 d . . . H48A H 0.9456 0.5512 0.9725 0.127 Uiso 1 1 calc R . . C49 C 0.7265(8) 0.5989(4) 0.9828(3) 0.075(2) Uani 1 1 d . . . C50 C 0.6779(7) 0.6509(4) 1.0005(3) 0.081(2) Uani 1 1 d . . . C51 C 0.8303(6) 0.6441(3) 1.1594(4) 0.090(2) Uani 1 1 d . . . H51A H 0.7627 0.6535 1.1444 0.108 Uiso 1 1 calc R . . C52 C 0.8508(7) 0.6223(3) 1.2208(4) 0.109(3) Uani 1 1 d . . . H52A H 0.7974 0.6172 1.2459 0.131 Uiso 1 1 calc R . . C53 C 0.9495(8) 0.6088(3) 1.2429(4) 0.102(3) Uani 1 1 d . . . H53A H 0.9638 0.5949 1.2836 0.122 Uiso 1 1 calc R . . C54 C 1.0290(7) 0.6155(3) 1.2055(4) 0.080(2) Uani 1 1 d . . . C55 C 1.1339(8) 0.6045(3) 1.2242(4) 0.092(3) Uani 1 1 d . . . H55A H 1.1525 0.5899 1.2642 0.110 Uiso 1 1 calc R . . C56 C 1.2078(7) 0.6140(3) 1.1872(4) 0.091(3) Uani 1 1 d . . . H56A H 1.2763 0.6068 1.2021 0.110 Uiso 1 1 calc R . . C57 C 1.1828(7) 0.6351(3) 1.1249(4) 0.075(2) Uani 1 1 d . . . C58 C 1.2543(7) 0.6476(3) 1.0828(4) 0.100(3) Uani 1 1 d . . . H58A H 1.3246 0.6431 1.0952 0.120 Uiso 1 1 calc R . . C59 C 1.2220(7) 0.6662(3) 1.0241(4) 0.109(3) Uani 1 1 d . . . H59A H 1.2698 0.6729 0.9956 0.131 Uiso 1 1 calc R . . C60 C 1.1167(7) 0.6754(3) 1.0063(3) 0.095(2) Uani 1 1 d . . . H60A H 1.0955 0.6883 0.9658 0.115 Uiso 1 1 calc R . . C61 C 1.0800(6) 0.6463(2) 1.1042(3) 0.0651(19) Uani 1 1 d . . . C62 C 1.0030(6) 0.6371(2) 1.1449(3) 0.0612(18) Uani 1 1 d . . . C63 C 0.2078(17) 0.7566(5) 0.8773(9) 0.382(17) Uani 1 1 d D . . H63A H 0.2608 0.7756 0.9049 0.458 Uiso 1 1 calc R . . H63B H 0.1482 0.7541 0.9007 0.458 Uiso 1 1 calc R . . C64 C 0.1790(10) 0.7956(5) 0.8295(5) 0.223(6) Uani 1 1 d D . . H64A H 0.2059 0.8320 0.8420 0.335 Uiso 1 1 calc R . . H64B H 0.1050 0.7975 0.8222 0.335 Uiso 1 1 calc R . . H64C H 0.2062 0.7841 0.7916 0.335 Uiso 1 1 calc R . . C65 C 0.1789(14) 0.5227(7) 0.8588(10) 0.401(19) Uani 1 1 d D . . H65A H 0.2129 0.4864 0.8582 0.481 Uiso 1 1 calc R . . H65B H 0.1565 0.5317 0.8152 0.481 Uiso 1 1 calc R . . C66 C 0.0878(12) 0.5126(8) 0.8861(8) 0.287(10) Uani 1 1 d D . . H66A H 0.0971 0.4803 0.9133 0.430 Uiso 1 1 calc R . . H66B H 0.0323 0.5056 0.8537 0.430 Uiso 1 1 calc R . . H66C H 0.0716 0.5448 0.9102 0.430 Uiso 1 1 calc R . . Cl1 Cl 0.43797(19) 0.88451(11) 0.96045(12) 0.0986(7) Uani 1 1 d . . . Cl2 Cl 0.2278(3) 0.65859(14) 0.69477(15) 0.1367(10) Uani 1 1 d . . . Cl3 Cl 0.0457(2) 0.91330(14) 0.66271(13) 0.1124(8) Uani 1 1 d . . . N1 N 0.7245(4) 1.0125(2) 0.8452(2) 0.0598(14) Uani 1 1 d . . . N2 N 0.8716(6) 1.0525(2) 0.7801(2) 0.0720(17) Uani 1 1 d . . . N3 N 0.8997(4) 1.05101(18) 0.93641(19) 0.0513(13) Uani 1 1 d . . . N4 N 1.0299(4) 0.9969(2) 0.8725(2) 0.0621(14) Uani 1 1 d . . . N5 N 0.8631(4) 0.9181(2) 0.8407(2) 0.0655(16) Uani 1 1 d . . . N6 N 0.6842(5) 0.7732(2) 0.8119(3) 0.0714(16) Uani 1 1 d . . . N7 N 0.8436(5) 0.7555(2) 0.7465(2) 0.0698(16) Uani 1 1 d . . . N8 N 0.9012(4) 0.7214(2) 0.9542(2) 0.0687(17) Uani 1 1 d . . . N9 N 0.7415(4) 0.6931(3) 1.0258(2) 0.0688(16) Uani 1 1 d . . . N10 N 0.8312(5) 0.5980(2) 0.9891(2) 0.0742(17) Uani 1 1 d . . . N11 N 0.9040(5) 0.6516(2) 1.1223(2) 0.0683(16) Uani 1 1 d . . . N12 N 1.0466(4) 0.6663(2) 1.0452(3) 0.0699(15) Uani 1 1 d . . . O1 O 0.5432(4) 0.8800(2) 0.9576(3) 0.154(2) Uani 1 1 d . . . O2 O 0.3914(5) 0.8880(3) 0.8989(3) 0.180(3) Uani 1 1 d . . . O3 O 0.4073(5) 0.9347(3) 0.9852(3) 0.187(3) Uani 1 1 d . . . O4 O 0.3978(5) 0.8396(3) 0.9881(3) 0.196(3) Uani 1 1 d . . . O5 O 0.1998(11) 0.6406(6) 0.7457(4) 0.413(10) Uani 1 1 d . . . O6 O 0.2360(7) 0.7145(3) 0.6936(4) 0.264(5) Uani 1 1 d . . . O7 O 0.1611(6) 0.6387(3) 0.6453(4) 0.205(3) Uani 1 1 d . . . O8 O 0.3197(7) 0.6378(5) 0.6963(7) 0.370(9) Uani 1 1 d . . . O9 O 0.1050(6) 0.9048(5) 0.7106(3) 0.333(7) Uani 1 1 d . . . O10 O 0.0213(9) 0.8640(5) 0.6407(5) 0.334(7) Uani 1 1 d . . . O11 O -0.0289(8) 0.9465(4) 0.6775(4) 0.299(6) Uani 1 1 d . . . O12 O 0.0853(9) 0.9307(4) 0.6122(4) 0.301(6) Uani 1 1 d . . . O13 O 0.2389(14) 0.7077(5) 0.8744(5) 0.453(11) Uani 1 1 d D . . H13B H 0.1941 0.6877 0.8526 0.679 Uiso 1 1 d R . . O14 O 0.2485(14) 0.5564(9) 0.8749(10) 0.661(18) Uani 1 1 d D . . H14B H 0.2378 0.5909 0.8518 0.992 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 0.0587(6) 0.0620(5) 0.0696(5) -0.0035(4) 0.0026(4) -0.0005(5) Cu2 0.0839(7) 0.0696(6) 0.0591(5) -0.0038(4) -0.0014(4) -0.0078(5) Cu3 0.0672(7) 0.0738(6) 0.0634(5) 0.0052(4) 0.0043(4) 0.0033(5) C1 0.062(6) 0.082(5) 0.080(5) 0.013(4) -0.008(4) -0.003(5) C2 0.058(6) 0.104(7) 0.120(7) -0.008(5) 0.009(5) -0.003(5) C3 0.067(7) 0.095(7) 0.142(9) -0.008(6) -0.016(6) 0.028(6) C4 0.080(8) 0.068(6) 0.088(7) -0.012(5) -0.011(5) 0.014(5) C5 0.133(11) 0.077(7) 0.128(9) 0.013(6) -0.050(7) 0.024(6) C6 0.191(15) 0.054(6) 0.107(9) 0.010(5) -0.043(8) 0.006(7) C7 0.167(11) 0.052(5) 0.063(6) 0.004(4) -0.002(6) -0.002(6) C8 0.230(15) 0.073(7) 0.077(7) 0.012(5) 0.026(9) -0.027(9) C9 0.233(14) 0.080(7) 0.087(8) -0.010(6) 0.067(8) -0.035(9) C10 0.119(8) 0.079(6) 0.081(6) -0.003(4) 0.035(5) -0.014(5) C11 0.094(7) 0.040(4) 0.061(5) -0.006(4) -0.001(5) 0.000(5) C12 0.069(6) 0.047(4) 0.071(5) -0.009(4) -0.010(5) 0.005(4) C13 0.058(5) 0.068(5) 0.053(4) 0.007(4) 0.003(4) 0.003(4) C14 0.070(6) 0.080(5) 0.048(4) -0.001(4) 0.013(4) 0.010(4) C15 0.070(6) 0.075(5) 0.057(5) -0.015(3) 0.001(4) -0.001(5) C16 0.045(5) 0.070(5) 0.052(4) 0.003(4) 0.000(4) -0.004(4) C17 0.081(7) 0.090(6) 0.055(5) 0.005(4) 0.007(4) -0.019(5) C18 0.035(5) 0.114(6) 0.068(5) 0.005(4) 0.003(4) -0.006(4) C19 0.056(6) 0.062(5) 0.060(5) 0.004(4) 0.007(4) 0.000(4) C20 0.053(5) 0.094(6) 0.094(6) 0.004(5) 0.009(5) 0.004(5) C21 0.075(7) 0.101(6) 0.108(7) -0.010(5) 0.040(5) 0.020(5) C22 0.080(7) 0.083(5) 0.078(5) -0.014(4) 0.022(5) 0.008(5) C23 0.049(5) 0.067(5) 0.045(4) 0.008(3) 0.006(4) 0.000(4) C24 0.048(5) 0.051(4) 0.050(4) 0.003(3) 0.006(4) 0.002(4) C25 0.051(5) 0.063(4) 0.049(4) 0.002(4) -0.003(3) 0.000(4) C26 0.094(8) 0.105(6) 0.073(6) 0.003(4) 0.021(5) 0.004(6) C27 0.058(7) 0.131(8) 0.168(10) -0.003(7) 0.031(6) -0.003(6) C28 0.085(8) 0.105(7) 0.133(9) -0.013(6) -0.013(7) -0.016(6) C29 0.089(8) 0.066(5) 0.091(7) 0.001(5) 0.000(6) -0.013(5) C30 0.118(10) 0.072(6) 0.113(9) -0.012(6) -0.053(6) -0.003(6) C31 0.152(11) 0.075(6) 0.082(7) -0.024(5) -0.026(7) 0.000(7) C32 0.155(10) 0.059(5) 0.056(6) -0.013(4) -0.009(6) -0.004(6) C33 0.164(12) 0.109(7) 0.081(7) -0.020(5) 0.041(8) 0.007(8) C34 0.161(11) 0.116(8) 0.100(8) -0.005(6) 0.061(7) 0.016(7) C35 0.107(8) 0.117(7) 0.067(6) -0.006(5) 0.022(5) 0.001(6) C36 0.100(8) 0.054(5) 0.050(5) 0.006(4) 0.005(5) -0.005(5) C37 0.077(7) 0.055(4) 0.068(6) 0.001(4) -0.007(5) -0.011(4) C38 0.090(6) 0.047(4) 0.061(5) -0.008(4) -0.002(4) -0.005(4) C39 0.092(8) 0.090(6) 0.085(6) 0.013(4) 0.027(5) 0.018(5) C40 0.097(9) 0.137(9) 0.104(7) 0.028(6) 0.048(6) 0.054(7) C41 0.076(8) 0.162(10) 0.095(7) 0.023(7) 0.024(5) 0.013(8) C42 0.076(8) 0.118(8) 0.075(6) 0.010(5) 0.014(5) 0.005(7) C43 0.084(8) 0.192(11) 0.080(7) 0.002(7) 0.007(5) -0.029(9) C44 0.106(10) 0.141(10) 0.097(7) -0.009(6) 0.007(6) -0.047(8) C45 0.096(9) 0.105(8) 0.093(6) 0.014(6) -0.013(6) -0.025(8) C46 0.139(10) 0.072(7) 0.138(8) -0.021(5) -0.026(7) -0.005(7) C47 0.124(10) 0.099(8) 0.173(9) -0.025(6) -0.037(8) 0.031(8) C48 0.105(8) 0.077(6) 0.128(7) -0.027(5) -0.018(5) 0.013(6) C49 0.087(7) 0.080(6) 0.057(5) 0.001(4) 0.005(5) -0.004(6) C50 0.063(7) 0.117(8) 0.063(5) 0.022(5) 0.006(4) -0.013(6) C51 0.075(7) 0.105(6) 0.089(6) 0.012(5) 0.002(5) -0.015(5) C52 0.114(9) 0.142(7) 0.073(6) 0.032(5) 0.022(5) -0.012(6) C53 0.102(8) 0.129(7) 0.072(6) 0.030(5) 0.000(6) 0.000(6) C54 0.081(7) 0.088(5) 0.068(6) 0.004(4) -0.011(5) -0.008(5) C55 0.099(9) 0.091(6) 0.079(6) 0.012(5) -0.021(6) -0.017(6) C56 0.082(8) 0.078(5) 0.104(8) -0.009(5) -0.035(5) 0.008(5) C57 0.060(6) 0.078(5) 0.084(6) -0.004(4) -0.006(5) 0.000(5) C58 0.079(7) 0.103(6) 0.115(8) -0.006(6) -0.005(6) 0.005(5) C59 0.064(7) 0.146(8) 0.122(8) 0.013(6) 0.031(5) 0.015(6) C60 0.069(7) 0.132(7) 0.088(6) 0.005(5) 0.022(5) 0.011(6) C61 0.067(6) 0.059(4) 0.067(5) -0.003(4) -0.002(5) -0.005(4) C62 0.060(6) 0.062(5) 0.059(5) 0.001(4) -0.002(4) -0.004(4) C63 0.60(4) 0.136(15) 0.48(3) -0.005(17) 0.37(3) -0.09(2) C64 0.285(16) 0.207(14) 0.193(12) -0.070(10) 0.097(11) -0.087(13) C65 0.60(5) 0.24(2) 0.31(3) -0.101(19) -0.19(3) 0.29(3) C66 0.43(3) 0.302(18) 0.127(11) 0.011(10) 0.003(13) 0.243(18) Cl1 0.0738(18) 0.125(2) 0.0999(18) 0.0107(16) 0.0223(13) 0.0165(16) Cl2 0.127(3) 0.137(3) 0.143(3) -0.027(2) 0.0020(19) -0.046(2) Cl3 0.101(2) 0.150(2) 0.0828(19) -0.0233(17) -0.0060(15) 0.0071(18) N1 0.059(4) 0.061(4) 0.059(4) -0.002(3) 0.002(3) -0.008(3) N2 0.095(6) 0.068(4) 0.057(4) -0.014(3) 0.029(4) -0.027(4) N3 0.053(4) 0.056(3) 0.046(3) 0.004(2) 0.009(3) 0.009(3) N4 0.057(4) 0.063(4) 0.068(4) -0.010(3) 0.016(3) 0.004(3) N5 0.068(4) 0.064(3) 0.063(4) -0.006(3) -0.002(3) 0.003(3) N6 0.084(5) 0.074(4) 0.058(4) -0.005(3) 0.015(4) -0.006(3) N7 0.079(5) 0.066(4) 0.067(4) -0.001(3) 0.017(4) -0.002(4) N8 0.069(4) 0.068(4) 0.068(4) 0.005(3) 0.005(3) 0.004(3) N9 0.058(5) 0.083(5) 0.066(4) 0.010(3) 0.010(3) 0.009(4) N10 0.068(5) 0.067(4) 0.085(4) -0.007(3) -0.002(3) 0.007(4) N11 0.066(5) 0.079(4) 0.058(4) 0.011(3) 0.002(3) -0.006(4) N12 0.053(4) 0.087(4) 0.070(4) -0.004(3) 0.010(3) 0.008(3) O1 0.057(4) 0.179(6) 0.229(6) 0.027(4) 0.032(4) 0.015(4) O2 0.163(7) 0.224(7) 0.148(6) 0.009(5) -0.007(5) 0.016(5) O3 0.193(7) 0.186(6) 0.195(6) -0.087(5) 0.071(5) 0.016(5) O4 0.119(6) 0.214(7) 0.265(8) 0.149(6) 0.065(5) 0.022(5) O5 0.50(2) 0.56(2) 0.175(9) 0.184(11) 0.030(10) -0.183(16) O6 0.294(12) 0.160(7) 0.308(11) -0.033(7) -0.103(8) -0.052(8) O7 0.163(8) 0.203(7) 0.249(8) -0.060(6) 0.021(6) -0.042(6) O8 0.087(8) 0.301(13) 0.70(3) -0.188(13) -0.045(10) 0.020(8) O9 0.198(9) 0.679(19) 0.107(6) -0.116(8) -0.048(6) 0.175(10) O10 0.419(16) 0.302(12) 0.296(12) -0.110(10) 0.110(10) -0.175(11) O11 0.311(12) 0.348(12) 0.245(9) -0.017(7) 0.068(8) 0.222(10) O12 0.548(19) 0.216(9) 0.158(8) 0.019(6) 0.122(9) 0.008(10) O13 0.85(3) 0.327(15) 0.213(10) -0.015(11) 0.212(13) -0.17(2) O14 0.67(4) 0.67(4) 0.60(3) 0.01(2) -0.16(2) -0.22(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 N5 1.939(5) . ? Cu1 N4 1.985(5) . ? Cu1 N1 2.000(5) . ? Cu1 N3 2.079(4) . ? Cu1 N2 2.121(5) . ? Cu2 C38 1.906(6) . ? Cu2 C25 1.908(6) . ? Cu2 N7 2.071(5) . ? Cu2 N6 2.087(6) . ? Cu3 N8 1.962(5) . ? Cu3 N12 1.999(5) . ? Cu3 N9 2.009(5) . ? Cu3 N11 2.038(5) . ? Cu3 N10 2.182(5) . ? C1 N1 1.307(7) . ? C1 C2 1.391(8) . ? C1 H1A 0.9300 . ? C2 C3 1.369(8) . ? C2 H2A 0.9300 . ? C3 C4 1.384(9) . ? C3 H3A 0.9300 . ? C4 C12 1.401(9) . ? C4 C5 1.430(10) . ? C5 C6 1.325(11) . ? C5 H5A 0.9300 . ? C6 C7 1.433(12) . ? C6 H6A 0.9300 . ? C7 C8 1.374(12) . ? C7 C11 1.398(9) . ? C8 C9 1.333(12) . ? C8 H8A 0.9300 . ? C9 C10 1.418(10) . ? C9 H9A 0.9300 . ? C10 N2 1.314(8) . ? C10 H10A 0.9300 . ? C11 N2 1.374(8) . ? C11 C12 1.397(8) . ? C12 N1 1.357(7) . ? C13 N3 1.326(6) . ? C13 C14 1.394(7) . ? C13 H13A 0.9300 . ? C14 C15 1.352(7) . ? C14 H14A 0.9300 . ? C15 C16 1.400(7) . ? C15 H15A 0.9300 . ? C16 C24 1.384(7) . ? C16 C17 1.423(8) . ? C17 C18 1.336(8) . ? C17 H17A 0.9300 . ? C18 C19 1.427(7) . ? C18 H18A 0.9300 . ? C19 C20 1.378(8) . ? C19 C23 1.392(8) . ? C20 C21 1.343(8) . ? C20 H20A 0.9300 . ? C21 C22 1.414(8) . ? C21 H21A 0.9300 . ? C22 N4 1.317(7) . ? C22 H22A 0.9300 . ? C23 N4 1.361(6) . ? C23 C24 1.400(7) . ? C24 N3 1.361(7) . ? C25 N5 1.158(5) . ? C26 N6 1.332(8) . ? C26 C27 1.385(9) . ? C26 H26A 0.9300 . ? C27 C28 1.363(9) . ? C27 H27A 0.9300 . ? C28 C29 1.371(9) . ? C28 H28A 0.9300 . ? C29 C37 1.397(9) . ? C29 C30 1.415(9) . ? C30 C31 1.350(10) . ? C30 H30A 0.9300 . ? C31 C32 1.404(11) . ? C31 H31A 0.9300 . ? C32 C33 1.401(11) . ? C32 C36 1.408(8) . ? C33 C34 1.354(10) . ? C33 H33A 0.9300 . ? C34 C35 1.421(9) . ? C34 H34A 0.9300 . ? C35 N7 1.321(8) . ? C35 H35A 0.9300 . ? C36 N7 1.361(8) . ? C36 C37 1.426(9) . ? C37 N6 1.364(7) . ? C38 N8 1.147(6) . ? C39 N9 1.331(7) . ? C39 C40 1.397(9) . ? C39 H39A 0.9300 . ? C40 C41 1.375(9) . ? C40 H40A 0.9300 . ? C41 C42 1.383(10) . ? C41 H41A 0.9300 . ? C42 C50 1.384(9) . ? C42 C43 1.410(10) . ? C43 C44 1.367(10) . ? C43 H43A 0.9300 . ? C44 C45 1.437(11) . ? C44 H44A 0.9300 . ? C45 C46 1.393(10) . ? C45 C49 1.406(9) . ? C46 C47 1.346(10) . ? C46 H46A 0.9300 . ? C47 C48 1.381(9) . ? C47 H47A 0.9300 . ? C48 N10 1.302(7) . ? C48 H48A 0.9300 . ? C49 N10 1.355(8) . ? C49 C50 1.457(9) . ? C50 N9 1.372(8) . ? C51 N11 1.322(7) . ? C51 C52 1.410(8) . ? C51 H51A 0.9300 . ? C52 C53 1.359(9) . ? C52 H52A 0.9300 . ? C53 C54 1.385(9) . ? C53 H53A 0.9300 . ? C54 C62 1.401(8) . ? C54 C55 1.404(9) . ? C55 C56 1.330(9) . ? C55 H55A 0.9300 . ? C56 C57 1.428(9) . ? C56 H56A 0.9300 . ? C57 C61 1.389(8) . ? C57 C58 1.395(9) . ? C58 C59 1.353(8) . ? C58 H58A 0.9300 . ? C59 C60 1.400(9) . ? C59 H59A 0.9300 . ? C60 N12 1.318(7) . ? C60 H60A 0.9300 . ? C61 N12 1.372(7) . ? C61 C62 1.416(8) . ? C62 N11 1.371(7) . ? C63 O13 1.235(14) . ? C63 C64 1.399(15) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 O14 1.229(16) . ? C65 C66 1.400(17) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? Cl1 O4 1.352(5) . ? Cl1 O1 1.382(5) . ? Cl1 O3 1.382(6) . ? Cl1 O2 1.389(6) . ? Cl2 O5 1.259(8) . ? Cl2 O8 1.292(8) . ? Cl2 O6 1.334(7) . ? Cl2 O7 1.377(7) . ? Cl3 O9 1.229(6) . ? Cl3 O10 1.288(9) . ? Cl3 O12 1.313(8) . ? Cl3 O11 1.317(7) . ? O13 H13B 0.8500 . ? O14 H14B 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 N5 Cu1 N4 94.8(2) . . ? N5 Cu1 N1 94.3(2) . . ? N4 Cu1 N1 170.7(2) . . ? N5 Cu1 N3 139.04(18) . . ? N4 Cu1 N3 80.5(2) . . ? N1 Cu1 N3 93.8(2) . . ? N5 Cu1 N2 116.41(19) . . ? N4 Cu1 N2 93.8(2) . . ? N1 Cu1 N2 80.4(2) . . ? N3 Cu1 N2 104.53(17) . . ? C38 Cu2 C25 121.1(2) . . ? C38 Cu2 N7 119.9(2) . . ? C25 Cu2 N7 112.4(2) . . ? C38 Cu2 N6 106.7(2) . . ? C25 Cu2 N6 107.5(2) . . ? N7 Cu2 N6 79.5(2) . . ? N8 Cu3 N12 93.1(2) . . ? N8 Cu3 N9 89.5(2) . . ? N12 Cu3 N9 172.6(2) . . ? N8 Cu3 N11 162.5(2) . . ? N12 Cu3 N11 81.6(2) . . ? N9 Cu3 N11 93.9(2) . . ? N8 Cu3 N10 100.24(19) . . ? N12 Cu3 N10 106.3(2) . . ? N9 Cu3 N10 80.1(3) . . ? N11 Cu3 N10 97.24(19) . . ? N1 C1 C2 123.9(7) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C3 C2 C1 118.0(8) . . ? C3 C2 H2A 121.0 . . ? C1 C2 H2A 121.0 . . ? C2 C3 C4 120.2(9) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C3 C4 C12 117.6(8) . . ? C3 C4 C5 124.5(10) . . ? C12 C4 C5 117.9(9) . . ? C6 C5 C4 121.6(11) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C5 C6 C7 122.1(11) . . ? C5 C6 H6A 119.0 . . ? C7 C6 H6A 119.0 . . ? C8 C7 C11 119.0(11) . . ? C8 C7 C6 124.4(10) . . ? C11 C7 C6 116.6(10) . . ? C9 C8 C7 120.1(12) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 119.7(12) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? N2 C10 C9 121.7(9) . . ? N2 C10 H10A 119.2 . . ? C9 C10 H10A 119.2 . . ? N2 C11 C12 117.2(7) . . ? N2 C11 C7 120.8(9) . . ? C12 C11 C7 122.0(9) . . ? N1 C12 C11 118.0(7) . . ? N1 C12 C4 122.2(8) . . ? C11 C12 C4 119.7(8) . . ? N3 C13 C14 122.3(6) . . ? N3 C13 H13A 118.8 . . ? C14 C13 H13A 118.8 . . ? C15 C14 C13 120.4(6) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 118.7(6) . . ? C14 C15 H15A 120.7 . . ? C16 C15 H15A 120.7 . . ? C24 C16 C15 118.1(7) . . ? C24 C16 C17 117.7(7) . . ? C15 C16 C17 124.2(7) . . ? C18 C17 C16 122.3(7) . . ? C18 C17 H17A 118.9 . . ? C16 C17 H17A 118.9 . . ? C17 C18 C19 120.6(7) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C20 C19 C23 118.0(7) . . ? C20 C19 C18 124.3(7) . . ? C23 C19 C18 117.7(7) . . ? C21 C20 C19 120.4(7) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 119.5(7) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? N4 C22 C21 121.1(7) . . ? N4 C22 H22A 119.4 . . ? C21 C22 H22A 119.4 . . ? N4 C23 C19 121.8(6) . . ? N4 C23 C24 117.0(7) . . ? C19 C23 C24 121.2(7) . . ? N3 C24 C16 122.9(6) . . ? N3 C24 C23 116.6(6) . . ? C16 C24 C23 120.5(7) . . ? N5 C25 Cu2 173.4(6) . . ? N6 C26 C27 124.1(8) . . ? N6 C26 H26A 118.0 . . ? C27 C26 H26A 118.0 . . ? C28 C27 C26 118.7(9) . . ? C28 C27 H27A 120.6 . . ? C26 C27 H27A 120.6 . . ? C27 C28 C29 119.9(9) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C28 C29 C37 118.2(9) . . ? C28 C29 C30 122.7(10) . . ? C37 C29 C30 119.1(9) . . ? C31 C30 C29 121.4(10) . . ? C31 C30 H30A 119.3 . . ? C29 C30 H30A 119.3 . . ? C30 C31 C32 120.1(10) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C33 C32 C31 123.1(9) . . ? C33 C32 C36 115.9(10) . . ? C31 C32 C36 121.0(10) . . ? C34 C33 C32 120.7(10) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C33 C34 C35 118.8(10) . . ? C33 C34 H34A 120.6 . . ? C35 C34 H34A 120.6 . . ? N7 C35 C34 123.3(8) . . ? N7 C35 H35A 118.3 . . ? C34 C35 H35A 118.3 . . ? N7 C36 C32 124.8(8) . . ? N7 C36 C37 117.3(7) . . ? C32 C36 C37 117.9(9) . . ? N6 C37 C29 123.0(8) . . ? N6 C37 C36 116.6(7) . . ? C29 C37 C36 120.4(8) . . ? N8 C38 Cu2 172.8(7) . . ? N9 C39 C40 121.2(8) . . ? N9 C39 H39A 119.4 . . ? C40 C39 H39A 119.4 . . ? C41 C40 C39 119.2(9) . . ? C41 C40 H40A 120.4 . . ? C39 C40 H40A 120.4 . . ? C40 C41 C42 120.2(10) . . ? C40 C41 H41A 119.9 . . ? C42 C41 H41A 119.9 . . ? C41 C42 C50 118.3(10) . . ? C41 C42 C43 122.9(11) . . ? C50 C42 C43 118.8(10) . . ? C44 C43 C42 122.0(10) . . ? C44 C43 H43A 119.0 . . ? C42 C43 H43A 119.0 . . ? C43 C44 C45 120.5(10) . . ? C43 C44 H44A 119.8 . . ? C45 C44 H44A 119.8 . . ? C46 C45 C49 115.5(10) . . ? C46 C45 C44 125.3(10) . . ? C49 C45 C44 119.0(10) . . ? C47 C46 C45 119.9(10) . . ? C47 C46 H46A 120.0 . . ? C45 C46 H46A 120.0 . . ? C46 C47 C48 119.8(10) . . ? C46 C47 H47A 120.1 . . ? C48 C47 H47A 120.1 . . ? N10 C48 C47 123.9(9) . . ? N10 C48 H48A 118.0 . . ? C47 C48 H48A 118.0 . . ? N10 C49 C45 124.6(9) . . ? N10 C49 C50 116.7(8) . . ? C45 C49 C50 118.6(10) . . ? N9 C50 C42 121.6(9) . . ? N9 C50 C49 117.4(8) . . ? C42 C50 C49 121.0(9) . . ? N11 C51 C52 122.2(7) . . ? N11 C51 H51A 118.9 . . ? C52 C51 H51A 118.9 . . ? C53 C52 C51 119.1(8) . . ? C53 C52 H52A 120.5 . . ? C51 C52 H52A 120.5 . . ? C52 C53 C54 120.7(8) . . ? C52 C53 H53A 119.7 . . ? C54 C53 H53A 119.7 . . ? C53 C54 C62 117.1(8) . . ? C53 C54 C55 125.4(9) . . ? C62 C54 C55 117.4(8) . . ? C56 C55 C54 122.9(9) . . ? C56 C55 H55A 118.5 . . ? C54 C55 H55A 118.5 . . ? C55 C56 C57 120.6(9) . . ? C55 C56 H56A 119.7 . . ? C57 C56 H56A 119.7 . . ? C61 C57 C58 116.2(8) . . ? C61 C57 C56 118.5(8) . . ? C58 C57 C56 125.2(9) . . ? C59 C58 C57 120.3(9) . . ? C59 C58 H58A 119.8 . . ? C57 C58 H58A 119.8 . . ? C58 C59 C60 119.9(8) . . ? C58 C59 H59A 120.0 . . ? C60 C59 H59A 120.0 . . ? N12 C60 C59 121.9(7) . . ? N12 C60 H60A 119.1 . . ? C59 C60 H60A 119.1 . . ? N12 C61 C57 123.8(7) . . ? N12 C61 C62 116.4(7) . . ? C57 C61 C62 119.8(8) . . ? N11 C62 C54 122.8(7) . . ? N11 C62 C61 116.5(7) . . ? C54 C62 C61 120.7(8) . . ? O13 C63 C64 131(2) . . ? O13 C63 H63A 104.6 . . ? C64 C63 H63A 104.6 . . ? O13 C63 H63B 104.6 . . ? C64 C63 H63B 104.6 . . ? H63A C63 H63B 105.7 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O14 C65 C66 129(2) . . ? O14 C65 H65A 105.1 . . ? C66 C65 H65A 105.1 . . ? O14 C65 H65B 105.1 . . ? C66 C65 H65B 105.1 . . ? H65A C65 H65B 105.9 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O4 Cl1 O1 113.0(4) . . ? O4 Cl1 O3 111.8(4) . . ? O1 Cl1 O3 114.4(4) . . ? O4 Cl1 O2 108.2(5) . . ? O1 Cl1 O2 107.1(4) . . ? O3 Cl1 O2 101.3(4) . . ? O5 Cl2 O8 101.7(8) . . ? O5 Cl2 O6 112.7(8) . . ? O8 Cl2 O6 107.8(7) . . ? O5 Cl2 O7 109.3(7) . . ? O8 Cl2 O7 113.1(7) . . ? O6 Cl2 O7 111.9(5) . . ? O9 Cl3 O10 105.2(8) . . ? O9 Cl3 O12 118.0(8) . . ? O10 Cl3 O12 95.1(6) . . ? O9 Cl3 O11 108.0(5) . . ? O10 Cl3 O11 118.3(8) . . ? O12 Cl3 O11 112.1(6) . . ? C1 N1 C12 118.1(7) . . ? C1 N1 Cu1 127.6(5) . . ? C12 N1 Cu1 114.3(5) . . ? C10 N2 C11 118.8(7) . . ? C10 N2 Cu1 131.1(6) . . ? C11 N2 Cu1 110.1(5) . . ? C13 N3 C24 117.6(5) . . ? C13 N3 Cu1 131.2(5) . . ? C24 N3 Cu1 111.0(4) . . ? C22 N4 C23 119.2(6) . . ? C22 N4 Cu1 126.8(5) . . ? C23 N4 Cu1 113.8(4) . . ? C25 N5 Cu1 173.6(5) . . ? C26 N6 C37 116.1(7) . . ? C26 N6 Cu2 130.7(6) . . ? C37 N6 Cu2 113.2(5) . . ? C35 N7 C36 116.5(7) . . ? C35 N7 Cu2 130.1(6) . . ? C36 N7 Cu2 113.4(5) . . ? C38 N8 Cu3 166.0(6) . . ? C39 N9 C50 119.5(7) . . ? C39 N9 Cu3 125.1(6) . . ? C50 N9 Cu3 115.1(6) . . ? C48 N10 C49 116.2(7) . . ? C48 N10 Cu3 133.2(6) . . ? C49 N10 Cu3 110.6(5) . . ? C51 N11 C62 118.1(6) . . ? C51 N11 Cu3 129.8(6) . . ? C62 N11 Cu3 111.9(5) . . ? C60 N12 C61 117.7(7) . . ? C60 N12 Cu3 129.0(6) . . ? C61 N12 Cu3 113.3(5) . . ? C63 O13 H13B 110.1 . . ? C65 O14 H14B 110.6 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.587 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.073 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 752340' #TrackingRef '- 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C75 H48 Cu4 N15, 3(Cl O4), 2(H2 O)' _chemical_formula_sum 'C75 H52 Cl3 Cu4 N15 O14' _chemical_formula_weight 1747.87 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' 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.761(10) _cell_length_b 13.021(11) _cell_length_c 13.671(12) _cell_angle_alpha 96.256(13) _cell_angle_beta 99.056(13) _cell_angle_gamma 114.199(9) _cell_volume 2008(3) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1505 _cell_measurement_theta_min 2.541 _cell_measurement_theta_max 19.237 _exptl_crystal_description block _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 886 _exptl_absorpt_coefficient_mu 1.215 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8881 _exptl_absorpt_correction_T_max 0.8881 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; The structure was solved by direct methods (Bruker, 2000) and successive difference Fourier syntheses. ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9482 _diffrn_reflns_av_R_equivalents 0.1080 _diffrn_reflns_av_sigmaI/netI 0.1803 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6784 _reflns_number_gt 2669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0536P)^2^+1.9680P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6784 _refine_ls_number_parameters 531 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1919 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.1921 _refine_ls_wR_factor_gt 0.1689 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.21662(9) 0.18071(8) 0.48099(7) 0.0556(4) Uani 1 1 d . . . Cu2 Cu 0.17701(10) 0.16313(9) 0.11378(8) 0.0677(4) Uani 1 1 d . . . C1 C 0.1859(9) -0.0549(9) 0.4129(8) 0.087(3) Uani 1 1 d . . . H1 H 0.2033 -0.0339 0.3525 0.105 Uiso 1 1 calc R . . C2 C 0.1703(9) -0.1647(10) 0.4296(10) 0.098(4) Uani 1 1 d . . . H2 H 0.1789 -0.2145 0.3808 0.117 Uiso 1 1 calc R . . C3 C 0.1431(9) -0.1978(9) 0.5158(10) 0.092(3) Uani 1 1 d . . . H3 H 0.1300 -0.2715 0.5250 0.111 Uiso 1 1 calc R . . C4 C 0.1341(7) -0.1212(9) 0.5932(8) 0.070(3) Uani 1 1 d . . . C5 C 0.1071(8) -0.1444(9) 0.6897(9) 0.087(3) Uani 1 1 d . . . H5 H 0.0969 -0.2143 0.7073 0.104 Uiso 1 1 calc R . . C6 C 0.0967(9) -0.0657(11) 0.7533(9) 0.094(3) Uani 1 1 d . . . H6 H 0.0838 -0.0806 0.8165 0.113 Uiso 1 1 calc R . . C7 C 0.1047(7) 0.0400(8) 0.7288(7) 0.066(3) Uani 1 1 d . . . C8 C 0.0887(8) 0.1177(9) 0.7904(7) 0.072(3) Uani 1 1 d . . . H8 H 0.0697 0.1035 0.8521 0.086 Uiso 1 1 calc R . . C9 C 0.1012(8) 0.2179(9) 0.7601(6) 0.073(3) Uani 1 1 d . . . H9 H 0.0882 0.2718 0.8004 0.088 Uiso 1 1 calc R . . C10 C 0.1326(7) 0.2391(8) 0.6714(7) 0.067(3) Uani 1 1 d . . . H10 H 0.1424 0.3088 0.6534 0.081 Uiso 1 1 calc R . . C11 C 0.1361(7) 0.0641(8) 0.6370(7) 0.054(2) Uani 1 1 d . . . C12 C 0.1479(7) -0.0170(7) 0.5686(7) 0.061(2) Uani 1 1 d . . . C13 C 0.1922(9) 0.3966(9) 0.4757(7) 0.072(3) Uani 1 1 d . . . H13 H 0.1191 0.3511 0.4328 0.087 Uiso 1 1 calc R . . C14 C 0.2239(10) 0.5139(9) 0.5059(8) 0.079(3) Uani 1 1 d . . . H14 H 0.1723 0.5449 0.4846 0.095 Uiso 1 1 calc R . . C15 C 0.3308(11) 0.5807(8) 0.5665(8) 0.077(3) Uani 1 1 d . . . H15 H 0.3533 0.6587 0.5869 0.093 Uiso 1 1 calc R . . C16 C 0.4071(9) 0.5347(8) 0.5985(6) 0.061(2) Uani 1 1 d . . . C17 C 0.5219(11) 0.5958(9) 0.6593(7) 0.084(3) Uani 1 1 d . . . H17 H 0.5493 0.6741 0.6827 0.101 Uiso 1 1 calc R . . C18 C 0.5939(10) 0.5462(10) 0.6853(7) 0.088(4) Uani 1 1 d . . . H18 H 0.6694 0.5910 0.7247 0.105 Uiso 1 1 calc R . . C19 C 0.5567(9) 0.4276(10) 0.6538(7) 0.066(3) Uani 1 1 d . . . C20 C 0.6239(10) 0.3726(13) 0.6767(8) 0.092(4) Uani 1 1 d . . . H20 H 0.7002 0.4138 0.7155 0.110 Uiso 1 1 calc R . . C21 C 0.5821(10) 0.2588(13) 0.6444(9) 0.098(4) Uani 1 1 d . . . H21 H 0.6284 0.2210 0.6612 0.118 Uiso 1 1 calc R . . C22 C 0.4671(10) 0.1981(9) 0.5846(7) 0.078(3) Uani 1 1 d . . . H22 H 0.4382 0.1197 0.5609 0.093 Uiso 1 1 calc R . . C23 C 0.4431(8) 0.3635(8) 0.5943(6) 0.052(2) Uani 1 1 d . . . C24 C 0.3684(8) 0.4142(8) 0.5661(6) 0.053(2) Uani 1 1 d . . . C25 C 0.1981(7) 0.1678(7) 0.2542(7) 0.059(2) Uani 1 1 d . . . C26 C 0.3584(11) 0.1315(11) 0.0076(10) 0.113(4) Uani 1 1 d . . . H26 H 0.3454 0.0665 0.0355 0.136 Uiso 1 1 calc R . . C27 C 0.4373(12) 0.1632(17) -0.0632(13) 0.149(6) Uani 1 1 d . . . H27 H 0.4787 0.1207 -0.0763 0.179 Uiso 1 1 calc R . . C28 C 0.4500(16) 0.2490(19) -0.1072(13) 0.157(8) Uani 1 1 d . . . H28 H 0.4945 0.2633 -0.1562 0.189 Uiso 1 1 calc R . . C29 C 0.3995(11) 0.3178(16) -0.0831(10) 0.115(5) Uani 1 1 d . . . C30 C 0.4139(13) 0.4149(15) -0.1258(10) 0.129(6) Uani 1 1 d . . . H30 H 0.4619 0.4345 -0.1718 0.155 Uiso 1 1 calc R . . C31 C 0.3616(13) 0.4772(14) -0.1021(11) 0.121(5) Uani 1 1 d . . . H31 H 0.3721 0.5410 -0.1313 0.145 Uiso 1 1 calc R . . C32 C 0.2909(11) 0.4500(10) -0.0344(8) 0.085(3) Uani 1 1 d . . . C33 C 0.2307(13) 0.5134(11) -0.0050(11) 0.117(4) Uani 1 1 d . . . H33 H 0.2407 0.5803 -0.0288 0.140 Uiso 1 1 calc R . . C34 C 0.1575(13) 0.4753(14) 0.0589(10) 0.118(4) Uani 1 1 d . . . H34 H 0.1171 0.5170 0.0773 0.142 Uiso 1 1 calc R . . C35 C 0.1410(11) 0.3792(10) 0.0967(8) 0.083(3) Uani 1 1 d . . . H35 H 0.0916 0.3573 0.1414 0.100 Uiso 1 1 calc R . . C36 C 0.2681(9) 0.3529(8) 0.0100(6) 0.066(3) Uani 1 1 d . . . C37 C 0.3248(8) 0.2851(9) -0.0160(7) 0.066(3) Uani 1 1 d . . . C38 C 0.0414(7) 0.0381(7) 0.0256(5) 0.074(3) Uani 0.50 1 d P . . Cl1 Cl 0.9695(4) 0.4974(3) 0.2793(3) 0.1016(10) Uani 1 1 d . . . Cl2 Cl 0.4981(9) 0.9438(7) 0.6870(9) 0.131(3) Uani 0.50 1 d PD . . N1 N 0.1764(6) 0.0182(6) 0.4805(5) 0.0590(19) Uani 1 1 d . . . N2 N 0.1501(6) 0.1645(6) 0.6086(5) 0.0550(18) Uani 1 1 d . . . N3 N 0.2606(6) 0.3475(5) 0.5051(5) 0.0503(17) Uani 1 1 d . . . N4 N 0.3997(7) 0.2493(7) 0.5615(5) 0.0586(19) Uani 1 1 d . . . N5 N 0.3067(7) 0.1976(8) 0.0303(6) 0.079(2) Uani 1 1 d . . . N6 N 0.1931(7) 0.3188(7) 0.0712(5) 0.064(2) Uani 1 1 d . . . N7 N 0.2014(6) 0.1667(6) 0.3372(6) 0.066(2) Uani 1 1 d . . . N8 N 0.0414(7) 0.0381(7) 0.0256(5) 0.074(3) Uani 0.50 1 d P . . O1 O 1.0697(18) 0.5713(12) 0.2646(14) 0.346(12) Uani 1 1 d . . . O2 O 0.981(2) 0.4104(13) 0.256(2) 0.372(14) Uani 1 1 d . . . O3 O 0.9791(12) 0.517(2) 0.3782(12) 0.347(12) Uani 1 1 d . . . O4 O 0.930(4) 0.436(5) 0.176(3) 0.196(8) Uani 0.310(14) 1 d P . . O4' O 0.8729(16) 0.5184(16) 0.2553(11) 0.196(8) Uani 0.690(14) 1 d P . . O5 O 0.429(3) 0.955(4) 0.711(3) 0.30(2) Uani 0.50 1 d P A . O6 O 0.535(4) 0.935(5) 0.646(5) 0.53(6) Uani 0.50 1 d P A . O7 O 0.554(7) 1.013(7) 0.760(6) 0.25(3) Uani 0.165(14) 1 d P A 1 O7' O 0.411(4) 0.881(4) 0.616(4) 0.25(3) Uani 0.335(14) 1 d P A 2 O8 O 0.460(4) 0.850(3) 0.750(2) 0.94(12) Uani 0.50 1 d PD A . O9 O 0.819(2) 0.1919(11) 0.9328(18) 0.466(17) Uani 1 1 d . . . H9A H 0.8046 0.1550 0.8733 0.698 Uiso 1 1 d R . . H9B H 0.7538 0.1776 0.9499 0.698 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 0.0556(8) 0.0467(7) 0.0476(6) 0.0065(5) 0.0094(5) 0.0073(5) Cu2 0.0629(8) 0.0620(8) 0.0516(7) 0.0065(5) 0.0133(6) 0.0024(6) C1 0.090(8) 0.065(7) 0.082(8) -0.003(6) 0.010(6) 0.016(6) C2 0.091(9) 0.069(8) 0.118(10) -0.003(7) 0.028(8) 0.025(7) C3 0.070(8) 0.060(7) 0.128(10) 0.018(7) 0.012(7) 0.014(6) C4 0.037(6) 0.068(7) 0.091(8) 0.007(6) -0.008(5) 0.021(5) C5 0.070(7) 0.069(7) 0.115(10) 0.066(7) 0.034(7) 0.007(6) C6 0.072(8) 0.106(10) 0.094(9) 0.032(8) 0.020(6) 0.024(7) C7 0.052(6) 0.059(6) 0.076(7) 0.041(6) 0.011(5) 0.007(5) C8 0.075(7) 0.068(7) 0.054(6) 0.012(5) 0.030(5) 0.007(5) C9 0.062(7) 0.096(8) 0.051(6) 0.006(5) 0.027(5) 0.019(6) C10 0.064(7) 0.065(6) 0.064(6) 0.006(5) 0.023(5) 0.018(5) C11 0.029(5) 0.056(6) 0.064(6) 0.019(5) 0.006(4) 0.006(4) C12 0.043(6) 0.043(5) 0.079(7) 0.029(5) 0.010(5) -0.002(4) C13 0.056(7) 0.070(7) 0.080(7) 0.032(6) 0.016(5) 0.013(6) C14 0.086(9) 0.071(8) 0.098(8) 0.031(6) 0.035(7) 0.043(7) C15 0.079(9) 0.049(6) 0.093(8) 0.009(6) 0.027(7) 0.015(6) C16 0.059(7) 0.056(6) 0.053(6) 0.011(5) 0.021(5) 0.006(6) C17 0.079(9) 0.059(7) 0.069(7) 0.008(5) 0.017(7) -0.013(6) C18 0.053(8) 0.094(10) 0.058(7) 0.008(6) 0.003(5) -0.019(6) C19 0.036(6) 0.087(8) 0.060(6) 0.017(6) 0.017(5) 0.009(6) C20 0.045(7) 0.126(11) 0.079(8) 0.011(8) 0.015(6) 0.016(8) C21 0.054(8) 0.144(12) 0.108(9) 0.039(9) 0.015(7) 0.052(8) C22 0.072(8) 0.080(7) 0.076(7) 0.013(6) 0.025(6) 0.025(7) C23 0.050(6) 0.052(6) 0.038(5) 0.004(4) 0.008(4) 0.008(5) C24 0.051(6) 0.063(6) 0.039(5) 0.018(4) 0.012(5) 0.016(5) C25 0.054(6) 0.048(5) 0.054(5) 0.008(4) 0.019(5) -0.001(4) C26 0.084(9) 0.105(10) 0.157(12) 0.043(9) 0.043(9) 0.036(8) C27 0.088(11) 0.204(19) 0.170(16) 0.007(13) 0.062(11) 0.072(12) C28 0.145(16) 0.20(2) 0.116(13) 0.066(13) 0.082(11) 0.043(15) C29 0.064(9) 0.166(15) 0.076(9) 0.004(9) 0.022(7) 0.015(9) C30 0.092(12) 0.164(16) 0.088(10) 0.073(11) 0.044(8) -0.007(10) C31 0.102(13) 0.145(14) 0.087(10) 0.046(9) 0.027(9) 0.018(10) C32 0.090(9) 0.068(8) 0.058(7) 0.008(6) -0.003(6) 0.005(7) C33 0.121(12) 0.095(10) 0.110(11) 0.041(9) 0.008(9) 0.024(9) C34 0.122(12) 0.126(13) 0.100(10) -0.019(9) 0.013(9) 0.061(10) C35 0.098(9) 0.070(8) 0.069(7) 0.013(6) 0.013(6) 0.027(7) C36 0.060(7) 0.057(6) 0.040(5) 0.002(5) -0.005(5) -0.006(5) C37 0.055(7) 0.069(7) 0.056(6) 0.016(5) 0.013(5) 0.008(5) C38 0.079(8) 0.081(7) 0.029(5) 0.017(4) 0.010(4) 0.002(5) Cl1 0.128(3) 0.088(2) 0.093(2) 0.0189(19) 0.023(2) 0.052(2) Cl2 0.103(7) 0.096(5) 0.200(11) -0.012(6) 0.032(8) 0.060(5) N1 0.054(5) 0.050(4) 0.060(5) 0.001(4) 0.004(4) 0.016(4) N2 0.051(5) 0.055(5) 0.048(4) 0.022(4) 0.002(4) 0.013(4) N3 0.044(5) 0.046(4) 0.049(4) 0.008(3) 0.006(4) 0.010(4) N4 0.058(5) 0.079(6) 0.047(4) 0.014(4) 0.013(4) 0.037(5) N5 0.059(6) 0.074(6) 0.086(6) -0.002(5) 0.011(5) 0.019(5) N6 0.050(5) 0.071(6) 0.050(5) 0.006(4) 0.003(4) 0.010(4) N7 0.056(5) 0.063(5) 0.054(5) 0.000(4) 0.006(4) 0.005(4) N8 0.079(8) 0.081(7) 0.029(5) 0.017(4) 0.010(4) 0.002(5) O1 0.41(2) 0.167(13) 0.37(2) -0.009(13) 0.27(2) -0.021(15) O2 0.50(4) 0.130(12) 0.63(4) 0.156(17) 0.28(3) 0.201(18) O3 0.203(15) 0.70(4) 0.169(12) 0.075(17) 0.103(11) 0.21(2) O4 0.189(15) 0.30(2) 0.156(13) 0.023(12) -0.016(10) 0.186(16) O4' 0.189(15) 0.30(2) 0.156(13) 0.023(12) -0.016(10) 0.186(16) O5 0.13(2) 0.56(7) 0.20(3) -0.06(4) 0.04(2) 0.16(3) O6 0.22(5) 0.64(10) 0.63(9) -0.35(8) 0.14(5) 0.18(5) O7 0.15(3) 0.26(4) 0.24(4) -0.17(3) -0.11(3) 0.08(3) O7' 0.15(3) 0.26(4) 0.24(4) -0.17(3) -0.11(3) 0.08(3) O8 1.4(2) 0.45(7) 0.74(11) -0.44(7) -0.92(13) 0.69(11) O9 0.44(3) 0.087(10) 0.70(4) 0.015(15) -0.15(3) 0.068(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N7 1.925(8) . ? Cu1 N1 1.962(7) . ? Cu1 N3 1.982(7) . ? Cu1 N2 2.051(7) . ? Cu1 N4 2.175(8) . ? Cu2 C25 1.887(9) . ? Cu2 C38 1.925(7) . ? Cu2 N5 2.083(8) . ? Cu2 N6 2.108(8) . ? C1 N1 1.308(10) . ? C1 C2 1.410(14) . ? C1 H1 0.9300 . ? C2 C3 1.347(13) . ? C2 H2 0.9300 . ? C3 C4 1.424(13) . ? C3 H3 0.9300 . ? C4 C12 1.381(12) . ? C4 C5 1.446(13) . ? C5 C6 1.334(13) . ? C5 H5 0.9300 . ? C6 C7 1.418(13) . ? C6 H6 0.9300 . ? C7 C8 1.346(12) . ? C7 C11 1.405(11) . ? C8 C9 1.367(12) . ? C8 H8 0.9300 . ? C9 C10 1.358(11) . ? C9 H9 0.9300 . ? C10 N2 1.337(10) . ? C10 H10 0.9300 . ? C11 N2 1.354(10) . ? C11 C12 1.404(11) . ? C12 N1 1.384(10) . ? C13 N3 1.317(10) . ? C13 C14 1.404(12) . ? C13 H13 0.9300 . ? C14 C15 1.348(13) . ? C14 H14 0.9300 . ? C15 C16 1.378(12) . ? C15 H15 0.9300 . ? C16 C17 1.409(13) . ? C16 C24 1.430(11) . ? C17 C18 1.351(13) . ? C17 H17 0.9300 . ? C18 C19 1.408(13) . ? C18 H18 0.9300 . ? C19 C20 1.347(13) . ? C19 C23 1.396(12) . ? C20 C21 1.346(14) . ? C20 H20 0.9300 . ? C21 C22 1.406(13) . ? C21 H21 0.9300 . ? C22 N4 1.309(11) . ? C22 H22 0.9300 . ? C23 N4 1.350(10) . ? C23 C24 1.396(11) . ? C24 N3 1.358(10) . ? C25 N7 1.130(9) . ? C26 N5 1.321(13) . ? C26 C27 1.473(18) . ? C26 H26 0.9300 . ? C27 C28 1.29(2) . ? C27 H27 0.9300 . ? C28 C29 1.34(2) . ? C28 H28 0.9300 . ? C29 C37 1.400(14) . ? C29 C30 1.406(19) . ? C30 C31 1.288(18) . ? C30 H30 0.9300 . ? C31 C32 1.367(16) . ? C31 H31 0.9300 . ? C32 C36 1.405(13) . ? C32 C33 1.407(16) . ? C33 C34 1.360(16) . ? C33 H33 0.9300 . ? C34 C35 1.355(16) . ? C34 H34 0.9300 . ? C35 N6 1.274(12) . ? C35 H35 0.9300 . ? C36 N6 1.341(11) . ? C36 C37 1.402(13) . ? C37 N5 1.319(11) . ? C38 N8 1.160(13) 2 ? C38 C38 1.160(13) 2 ? Cl1 O2 1.215(13) . ? Cl1 O1 1.310(14) . ? Cl1 O3 1.325(14) . ? Cl1 O4' 1.367(14) . ? Cl1 O4 1.44(4) . ? Cl2 O6 0.81(3) . ? Cl2 O5 1.05(2) . ? Cl2 O7 1.17(6) . ? Cl2 O7' 1.26(3) . ? Cl2 O8 1.53(2) . ? O9 H9A 0.8485 . ? O9 H9B 0.8560 . ? 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 N7 Cu1 N1 94.9(3) . . ? N7 Cu1 N3 94.2(3) . . ? N1 Cu1 N3 170.9(3) . . ? N7 Cu1 N2 153.2(3) . . ? N1 Cu1 N2 81.0(3) . . ? N3 Cu1 N2 91.0(3) . . ? N7 Cu1 N4 111.9(3) . . ? N1 Cu1 N4 97.2(3) . . ? N3 Cu1 N4 79.1(3) . . ? N2 Cu1 N4 94.9(2) . . ? C25 Cu2 C38 118.5(3) . . ? C25 Cu2 N5 126.7(4) . . ? C38 Cu2 N5 103.5(3) . . ? C25 Cu2 N6 114.1(3) . . ? C38 Cu2 N6 109.2(3) . . ? N5 Cu2 N6 77.3(4) . . ? N1 C1 C2 121.5(10) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 120.4(11) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 120.7(11) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C12 C4 C3 114.4(10) . . ? C12 C4 C5 118.8(10) . . ? C3 C4 C5 126.7(11) . . ? C6 C5 C4 120.1(10) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 122.7(11) . . ? C5 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C8 C7 C11 120.0(9) . . ? C8 C7 C6 123.2(10) . . ? C11 C7 C6 116.7(10) . . ? C7 C8 C9 118.3(9) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? C10 C9 C8 120.3(9) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? N2 C10 C9 123.1(9) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N2 C11 C12 117.3(8) . . ? N2 C11 C7 121.1(9) . . ? C12 C11 C7 121.5(9) . . ? C4 C12 N1 125.3(9) . . ? C4 C12 C11 119.9(9) . . ? N1 C12 C11 114.8(8) . . ? N3 C13 C14 123.4(9) . . ? N3 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C15 C14 C13 118.6(10) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 120.7(10) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C17 126.0(10) . . ? C15 C16 C24 117.7(9) . . ? C17 C16 C24 116.2(10) . . ? C18 C17 C16 123.2(11) . . ? C18 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C17 C18 C19 121.1(10) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C23 118.1(11) . . ? C20 C19 C18 124.2(12) . . ? C23 C19 C18 117.7(11) . . ? C21 C20 C19 121.0(11) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 118.7(11) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? N4 C22 C21 121.6(10) . . ? N4 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? N4 C23 C24 116.6(8) . . ? N4 C23 C19 121.7(10) . . ? C24 C23 C19 121.7(10) . . ? N3 C24 C23 118.6(8) . . ? N3 C24 C16 121.2(9) . . ? C23 C24 C16 120.2(9) . . ? N7 C25 Cu2 174.6(7) . . ? N5 C26 C27 118.4(12) . . ? N5 C26 H26 120.8 . . ? C27 C26 H26 120.8 . . ? C28 C27 C26 121.1(16) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 120.6(18) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C28 C29 C37 116.6(17) . . ? C28 C29 C30 123.1(16) . . ? C37 C29 C30 120.2(15) . . ? C31 C30 C29 121.1(15) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 120.4(16) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C36 122.9(14) . . ? C31 C32 C33 123.8(14) . . ? C36 C32 C33 113.3(12) . . ? C34 C33 C32 119.0(13) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C35 C34 C33 122.8(13) . . ? C35 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? N6 C35 C34 120.2(12) . . ? N6 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? N6 C36 C37 118.5(9) . . ? N6 C36 C32 124.8(11) . . ? C37 C36 C32 116.7(11) . . ? N5 C37 C29 125.5(13) . . ? N5 C37 C36 115.7(9) . . ? C29 C37 C36 118.8(13) . . ? N8 C38 C38 0.0(14) 2 2 ? N8 C38 Cu2 178.3(10) 2 . ? C38 C38 Cu2 178.3(10) 2 . ? O2 Cl1 O1 98.2(12) . . ? O2 Cl1 O3 108.4(15) . . ? O1 Cl1 O3 105.3(11) . . ? O2 Cl1 O4' 129.6(16) . . ? O1 Cl1 O4' 117.8(13) . . ? O3 Cl1 O4' 95.5(9) . . ? O2 Cl1 O4 59.0(14) . . ? O1 Cl1 O4 94(2) . . ? O3 Cl1 O4 159(2) . . ? O4' Cl1 O4 83.2(14) . . ? O6 Cl2 O5 155(6) . . ? O6 Cl2 O7 116(6) . . ? O5 Cl2 O7 83(4) . . ? O6 Cl2 O7' 82(4) . . ? O5 Cl2 O7' 77(3) . . ? O7 Cl2 O7' 160(5) . . ? O6 Cl2 O8 115(5) . . ? O5 Cl2 O8 79(3) . . ? O7 Cl2 O8 90(5) . . ? O7' Cl2 O8 90(3) . . ? C1 N1 C12 117.6(8) . . ? C1 N1 Cu1 127.8(7) . . ? C12 N1 Cu1 114.2(6) . . ? C10 N2 C11 117.2(8) . . ? C10 N2 Cu1 131.3(6) . . ? C11 N2 Cu1 110.9(6) . . ? C13 N3 C24 118.3(8) . . ? C13 N3 Cu1 126.4(6) . . ? C24 N3 Cu1 115.0(6) . . ? C22 N4 C23 118.9(9) . . ? C22 N4 Cu1 131.0(7) . . ? C23 N4 Cu1 110.0(6) . . ? C37 N5 C26 117.4(10) . . ? C37 N5 Cu2 115.4(7) . . ? C26 N5 Cu2 126.4(8) . . ? C35 N6 C36 119.9(10) . . ? C35 N6 Cu2 127.7(8) . . ? C36 N6 Cu2 112.5(7) . . ? C25 N7 Cu1 174.4(7) . . ? H9A O9 H9B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.753 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.101 #===END #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 773341' #TrackingRef '- 1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H40 Cu3 N12, 3(B F4)' _chemical_formula_sum 'C52 H40 B3 Cu3 F12 N12' _chemical_formula_weight 1284.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 23.108(5) _cell_length_b 21.442(5) _cell_length_c 23.436(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.934(3) _cell_angle_gamma 90.00 _cell_volume 10846(4) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 5496 _cell_measurement_theta_min 2.552 _cell_measurement_theta_max 23.024 _exptl_crystal_description block _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5168 _exptl_absorpt_coefficient_mu 1.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8638 _exptl_absorpt_correction_T_max 0.8846 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; The structure was solved by direct methods (Bruker, 2000) and successive difference Fourier syntheses. ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27348 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9545 _reflns_number_gt 5744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BRUKER 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (BRUKER 2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0645P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9545 _refine_ls_number_parameters 763 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.894 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.11803(2) 0.15456(2) 0.06150(2) 0.05342(15) Uani 1 1 d . . . Cu2 Cu 0.20014(2) 0.35151(2) 0.17827(2) 0.05879(17) Uani 1 1 d . . . Cu3 Cu 0.11913(2) 0.57014(2) 0.13715(2) 0.05119(15) Uani 1 1 d . . . B1 B 0.2280(4) 0.9376(5) 0.0122(4) 0.117(3) Uani 1 1 d . . . B2 B 0.5283(3) 0.2438(3) 0.4125(3) 0.0738(15) Uani 1 1 d . . . B3 B 0.5000 0.5593(5) 0.2500 0.110(4) Uani 1 2 d S . . B4 B 0.0000 0.3502(18) 0.2500 0.213(10) Uani 1 2 d S . . C1 C 0.0839(2) 0.0618(2) -0.0408(2) 0.0740(13) Uani 1 1 d . . . H1 H 0.1259 0.0605 -0.0349 0.089 Uiso 1 1 calc R . . C2 C 0.0429(3) 0.0278(2) -0.0878(2) 0.0920(16) Uani 1 1 d . . . H2 H 0.0567 0.0039 -0.1135 0.110 Uiso 1 1 calc R . . C3 C -0.0180(3) 0.0301(3) -0.0957(3) 0.1016(19) Uani 1 1 d . . . H3 H -0.0463 0.0080 -0.1277 0.122 Uiso 1 1 calc R . . C4 C -0.0388(2) 0.0642(2) -0.0573(2) 0.0874(15) Uani 1 1 d . . . H4 H -0.0807 0.0655 -0.0628 0.105 Uiso 1 1 calc R . . C5 C 0.0048(2) 0.09708(18) -0.0100(2) 0.0618(11) Uani 1 1 d . . . C6 C -0.0099(2) 0.13270(18) 0.0361(2) 0.0614(11) Uani 1 1 d . . . C7 C -0.0688(2) 0.1363(2) 0.0397(3) 0.0816(15) Uani 1 1 d . . . H7 H -0.1025 0.1174 0.0101 0.098 Uiso 1 1 calc R . . C8 C -0.0765(3) 0.1678(3) 0.0870(3) 0.0962(18) Uani 1 1 d . . . H8 H -0.1155 0.1709 0.0898 0.115 Uiso 1 1 calc R . . C9 C -0.0260(3) 0.1948(2) 0.1307(3) 0.0903(16) Uani 1 1 d . . . H9 H -0.0300 0.2152 0.1641 0.108 Uiso 1 1 calc R . . C10 C 0.0306(2) 0.1911(2) 0.1237(2) 0.0762(13) Uani 1 1 d . . . H10 H 0.0644 0.2108 0.1524 0.091 Uiso 1 1 calc R . . C11 C 0.1659(3) 0.0532(2) 0.1706(2) 0.107(2) Uani 1 1 d . . . H11 H 0.1289 0.0603 0.1769 0.128 Uiso 1 1 calc R . . C12 C 0.2075(4) 0.0079(3) 0.2061(3) 0.136(3) Uani 1 1 d . . . H12 H 0.1984 -0.0159 0.2349 0.163 Uiso 1 1 calc R . . C13 C 0.2617(4) 0.0008(3) 0.1959(4) 0.149(3) Uani 1 1 d U . . H13 H 0.2905 -0.0281 0.2193 0.179 Uiso 1 1 calc R . . C14 C 0.2757(3) 0.0344(3) 0.1527(3) 0.133(3) Uani 1 1 d U . . H14 H 0.3129 0.0285 0.1466 0.160 Uiso 1 1 calc R . . C15 C 0.2328(3) 0.0772(2) 0.1186(2) 0.0848(16) Uani 1 1 d . . . C16 C 0.2416(2) 0.1141(2) 0.0697(2) 0.0724(13) Uani 1 1 d . . . C17 C 0.2974(2) 0.1165(3) 0.0584(3) 0.101(2) Uani 1 1 d . . . H17 H 0.3326 0.0960 0.0838 0.121 Uiso 1 1 calc R . . C18 C 0.2988(3) 0.1495(3) 0.0095(4) 0.111(2) Uani 1 1 d . . . H18 H 0.3355 0.1515 0.0017 0.133 Uiso 1 1 calc R . . C19 C 0.2481(3) 0.1794(2) -0.0283(3) 0.0916(16) Uani 1 1 d . . . H19 H 0.2487 0.2002 -0.0629 0.110 Uiso 1 1 calc R . . C20 C 0.1956(2) 0.1779(2) -0.0135(2) 0.0712(12) Uani 1 1 d . . . H20 H 0.1609 0.1996 -0.0383 0.085 Uiso 1 1 calc R . . C21 C 0.17040(17) 0.27727(18) 0.13216(18) 0.0507(10) Uani 1 1 d . . . C22 C 0.1856(3) 0.3184(2) 0.3012(3) 0.0955(16) Uani 1 1 d . . . H22 H 0.1432 0.3226 0.2800 0.115 Uiso 1 1 calc R . . C23 C 0.2056(4) 0.2992(3) 0.3605(4) 0.132(3) Uani 1 1 d . . . H23 H 0.1775 0.2917 0.3799 0.158 Uiso 1 1 calc R . . C24 C 0.2683(5) 0.2911(4) 0.3913(3) 0.142(3) Uani 1 1 d . . . H24 H 0.2825 0.2774 0.4316 0.170 Uiso 1 1 calc R . . C25 C 0.3092(3) 0.3029(3) 0.3636(3) 0.1060(19) Uani 1 1 d . . . H25 H 0.3515 0.2967 0.3838 0.127 Uiso 1 1 calc R . . C26 C 0.2860(2) 0.3247(2) 0.3036(2) 0.0691(12) Uani 1 1 d . . . C27 C 0.3262(2) 0.34341(19) 0.2704(2) 0.0647(12) Uani 1 1 d . . . C28 C 0.3907(3) 0.3438(3) 0.2978(3) 0.1032(18) Uani 1 1 d . . . H28 H 0.4101 0.3298 0.3377 0.124 Uiso 1 1 calc R . . C29 C 0.4241(3) 0.3649(4) 0.2650(4) 0.146(3) Uani 1 1 d . . . H29 H 0.4671 0.3659 0.2825 0.175 Uiso 1 1 calc R . . C30 C 0.3959(3) 0.3848(4) 0.2067(3) 0.132(2) Uani 1 1 d . . . H30 H 0.4190 0.3999 0.1843 0.158 Uiso 1 1 calc R . . C31 C 0.3320(2) 0.3823(2) 0.1813(2) 0.0839(14) Uani 1 1 d . . . H31 H 0.3125 0.3954 0.1411 0.101 Uiso 1 1 calc R . . C32 C 0.16451(17) 0.43213(19) 0.15525(19) 0.0585(11) Uani 1 1 d . . . C33 C 0.0085(2) 0.5059(2) 0.1445(2) 0.0753(13) Uani 1 1 d . . . H33 H 0.0342 0.4934 0.1833 0.090 Uiso 1 1 calc R . . C34 C -0.0525(3) 0.4849(2) 0.1212(3) 0.0948(18) Uani 1 1 d . . . H34 H -0.0677 0.4595 0.1447 0.114 Uiso 1 1 calc R . . C35 C -0.0894(3) 0.5016(3) 0.0646(3) 0.098(2) Uani 1 1 d . . . H35 H -0.1301 0.4873 0.0486 0.118 Uiso 1 1 calc R . . C36 C -0.0669(2) 0.5395(2) 0.0307(3) 0.0843(16) Uani 1 1 d . . . H36 H -0.0921 0.5510 -0.0086 0.101 Uiso 1 1 calc R . . C37 C -0.00593(18) 0.56108(18) 0.0552(2) 0.0595(11) Uani 1 1 d . . . C38 C 0.0230(2) 0.60016(19) 0.02188(19) 0.0612(11) Uani 1 1 d . . . C39 C -0.0091(2) 0.6247(2) -0.0362(2) 0.0854(15) Uani 1 1 d . . . H39 H -0.0516 0.6185 -0.0551 0.103 Uiso 1 1 calc R . . C40 C 0.0230(4) 0.6577(3) -0.0642(3) 0.109(2) Uani 1 1 d . . . H40 H 0.0027 0.6738 -0.1031 0.131 Uiso 1 1 calc R . . C41 C 0.0845(3) 0.6676(3) -0.0359(3) 0.1068(19) Uani 1 1 d . . . H41 H 0.1065 0.6902 -0.0552 0.128 Uiso 1 1 calc R . . C42 C 0.1144(2) 0.6437(2) 0.0221(2) 0.0806(14) Uani 1 1 d . . . H42 H 0.1565 0.6513 0.0418 0.097 Uiso 1 1 calc R . . C43 C 0.2470(2) 0.5798(2) 0.1386(2) 0.0689(12) Uani 1 1 d . . . H43 H 0.2343 0.5509 0.1070 0.083 Uiso 1 1 calc R . . C44 C 0.3078(2) 0.6007(2) 0.1599(2) 0.0766(13) Uani 1 1 d . . . H44 H 0.3360 0.5851 0.1434 0.092 Uiso 1 1 calc R . . C45 C 0.3258(2) 0.6438(2) 0.2048(2) 0.0764(14) Uani 1 1 d . . . H45 H 0.3662 0.6589 0.2186 0.092 Uiso 1 1 calc R . . C46 C 0.28443(18) 0.66517(19) 0.2298(2) 0.0624(11) Uani 1 1 d . . . H46 H 0.2965 0.6949 0.2607 0.075 Uiso 1 1 calc R . . C47 C 0.22434(16) 0.64230(16) 0.20866(17) 0.0468(9) Uani 1 1 d . . . C48 C 0.17692(17) 0.65816(16) 0.23459(18) 0.0484(9) Uani 1 1 d . . . C49 C 0.18695(19) 0.69848(18) 0.28294(19) 0.0600(11) Uani 1 1 d . . . H49 H 0.2249 0.7186 0.3001 0.072 Uiso 1 1 calc R . . C50 C 0.1406(2) 0.7088(2) 0.3058(2) 0.0719(13) Uani 1 1 d . . . H50 H 0.1471 0.7352 0.3390 0.086 Uiso 1 1 calc R . . C51 C 0.0843(2) 0.6796(2) 0.2787(2) 0.0776(14) Uani 1 1 d . . . H51 H 0.0519 0.6862 0.2927 0.093 Uiso 1 1 calc R . . C52 C 0.07743(19) 0.6403(2) 0.2305(2) 0.0681(12) Uani 1 1 d . . . H52 H 0.0394 0.6206 0.2122 0.082 Uiso 1 1 calc R . . F1 F 0.19020(15) 0.94515(19) 0.04297(17) 0.1397(14) Uani 1 1 d . . . F2 F 0.2877(2) 0.9371(3) 0.0566(3) 0.206(3) Uani 1 1 d . . . F3 F 0.22168(16) 0.88017(17) -0.01545(16) 0.1270(12) Uani 1 1 d . . . F4 F 0.2256(4) 0.9823(2) -0.0259(3) 0.245(3) Uani 1 1 d . . . F5 F 0.5362(2) 0.18585(17) 0.3976(2) 0.1725(18) Uani 1 1 d . . . F6 F 0.56523(19) 0.2519(2) 0.47081(17) 0.1672(16) Uani 1 1 d . . . F7 F 0.54134(18) 0.28490(17) 0.37661(18) 0.1481(14) Uani 1 1 d . . . F8 F 0.47039(18) 0.2495(2) 0.4122(2) 0.193(2) Uani 1 1 d . . . F9 F 0.5000 0.4994(5) 0.2500 0.313(6) Uani 1 2 d S . . F10 F 0.4534(5) 0.5583(5) 0.1971(4) 0.152(4) Uani 0.50 1 d P . . F11 F 0.5350(4) 0.5616(4) 0.2109(4) 0.148(3) Uani 0.50 1 d P . . F12 F 0.5313(5) 0.6078(6) 0.2634(7) 0.238(7) Uani 0.50 1 d P . . F13 F 0.0428(4) 0.3325(4) 0.3048(3) 0.182(3) Uani 0.67 1 d P . . F14 F 0.0351(4) 0.3940(5) 0.2425(6) 0.252(5) Uani 0.67 1 d P . . F15 F 0.0318(4) 0.3120(7) 0.2260(6) 0.293(7) Uani 0.67 1 d P . . N1 N 0.06520(16) 0.09661(15) -0.00329(15) 0.0593(9) Uani 1 1 d . . . N2 N 0.03933(15) 0.16070(14) 0.07802(16) 0.0592(9) Uani 1 1 d . . . N3 N 0.1787(2) 0.08652(15) 0.12772(16) 0.0739(11) Uani 1 1 d . . . N4 N 0.19198(14) 0.14685(14) 0.03488(16) 0.0571(9) Uani 1 1 d . . . N5 N 0.15200(14) 0.23187(15) 0.10597(15) 0.0562(8) Uani 1 1 d . . . N6 N 0.22488(18) 0.33132(15) 0.27221(18) 0.0670(10) Uani 1 1 d . . . N7 N 0.29729(15) 0.36164(15) 0.21233(17) 0.0591(9) Uani 1 1 d . . . N8 N 0.14595(15) 0.48186(16) 0.14385(17) 0.0665(10) Uani 1 1 d . . . N9 N 0.03057(14) 0.54394(14) 0.11172(17) 0.0560(8) Uani 1 1 d . . . N10 N 0.08414(16) 0.61021(14) 0.05056(15) 0.0575(9) Uani 1 1 d . . . N11 N 0.20635(13) 0.60070(14) 0.16278(15) 0.0528(8) Uani 1 1 d . . . N12 N 0.12202(13) 0.62879(14) 0.20827(15) 0.0527(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0518(3) 0.0497(3) 0.0520(3) -0.0040(2) 0.0102(2) -0.0110(2) Cu2 0.0506(3) 0.0454(3) 0.0695(4) -0.0073(2) 0.0082(3) 0.0024(2) Cu3 0.0420(3) 0.0497(3) 0.0564(3) -0.0017(2) 0.0109(2) 0.0002(2) B1 0.110(6) 0.145(8) 0.119(7) -0.050(6) 0.070(6) -0.056(5) B2 0.068(4) 0.078(4) 0.070(4) 0.003(3) 0.018(3) -0.014(3) B3 0.144(11) 0.063(6) 0.100(10) 0.000 0.014(10) 0.000 B4 0.27(3) 0.33(3) 0.111(15) 0.000 0.15(2) 0.000 C1 0.087(3) 0.061(3) 0.073(3) -0.014(3) 0.027(3) -0.022(2) C2 0.125(5) 0.077(3) 0.069(4) -0.026(3) 0.028(3) -0.035(3) C3 0.121(5) 0.086(4) 0.074(4) -0.024(3) 0.006(4) -0.045(4) C4 0.077(4) 0.082(3) 0.082(4) -0.009(3) 0.003(3) -0.030(3) C5 0.064(3) 0.053(2) 0.058(3) 0.007(2) 0.008(2) -0.017(2) C6 0.059(3) 0.052(2) 0.067(3) 0.011(2) 0.014(2) -0.008(2) C7 0.060(3) 0.076(3) 0.106(5) 0.011(3) 0.027(3) -0.014(2) C8 0.087(4) 0.090(4) 0.133(6) 0.013(4) 0.064(4) -0.007(3) C9 0.114(5) 0.075(3) 0.107(5) 0.005(3) 0.070(4) -0.010(3) C10 0.081(4) 0.080(3) 0.074(4) -0.002(3) 0.036(3) -0.014(3) C11 0.162(6) 0.069(3) 0.063(4) -0.005(3) 0.008(4) -0.046(4) C12 0.245(9) 0.056(4) 0.053(4) 0.007(3) -0.012(5) -0.029(5) C13 0.210(6) 0.080(4) 0.086(5) -0.007(3) -0.034(5) 0.040(5) C14 0.187(5) 0.077(4) 0.077(4) -0.010(3) -0.024(4) 0.050(4) C15 0.099(4) 0.054(3) 0.069(4) -0.016(3) -0.010(3) 0.011(3) C16 0.073(3) 0.058(3) 0.068(3) -0.019(2) 0.003(3) 0.008(2) C17 0.063(4) 0.095(4) 0.130(6) -0.033(4) 0.015(4) 0.026(3) C18 0.079(5) 0.113(5) 0.152(7) -0.040(5) 0.054(5) -0.008(4) C19 0.089(4) 0.081(4) 0.122(5) -0.016(3) 0.058(4) -0.016(3) C20 0.070(3) 0.061(3) 0.087(4) -0.001(3) 0.033(3) -0.006(2) C21 0.043(2) 0.047(2) 0.055(3) 0.004(2) 0.0090(19) 0.0041(18) C22 0.110(5) 0.094(4) 0.098(5) -0.009(4) 0.057(4) 0.002(3) C23 0.183(8) 0.134(6) 0.123(7) -0.009(5) 0.109(6) 0.000(6) C24 0.194(9) 0.158(7) 0.080(5) -0.003(5) 0.058(6) 0.012(7) C25 0.128(5) 0.117(5) 0.062(4) 0.000(3) 0.020(4) 0.012(4) C26 0.075(3) 0.062(3) 0.060(3) -0.012(2) 0.011(3) 0.002(2) C27 0.053(3) 0.061(3) 0.067(3) -0.015(2) 0.006(2) -0.002(2) C28 0.068(4) 0.133(5) 0.086(4) -0.010(4) -0.001(3) -0.003(3) C29 0.053(4) 0.238(9) 0.127(7) -0.002(6) 0.007(4) -0.031(4) C30 0.078(5) 0.201(7) 0.118(6) -0.006(5) 0.037(4) -0.036(5) C31 0.066(3) 0.097(4) 0.085(4) -0.006(3) 0.023(3) -0.016(3) C32 0.046(2) 0.053(3) 0.064(3) -0.013(2) 0.004(2) -0.0036(19) C33 0.067(3) 0.068(3) 0.095(4) -0.001(3) 0.033(3) -0.005(2) C34 0.076(4) 0.074(3) 0.155(6) -0.016(4) 0.067(4) -0.014(3) C35 0.058(4) 0.087(4) 0.150(6) -0.047(4) 0.038(4) -0.007(3) C36 0.050(3) 0.080(3) 0.106(4) -0.035(3) 0.007(3) 0.009(3) C37 0.044(2) 0.053(2) 0.073(3) -0.018(2) 0.010(2) 0.0074(19) C38 0.067(3) 0.055(2) 0.051(3) -0.010(2) 0.008(2) 0.019(2) C39 0.088(4) 0.080(3) 0.066(4) -0.001(3) 0.000(3) 0.026(3) C40 0.147(6) 0.098(4) 0.066(4) 0.018(3) 0.017(4) 0.034(4) C41 0.138(6) 0.097(4) 0.091(5) 0.031(4) 0.049(4) 0.009(4) C42 0.088(4) 0.074(3) 0.079(4) 0.019(3) 0.030(3) 0.000(3) C43 0.058(3) 0.078(3) 0.075(3) -0.008(2) 0.028(2) 0.004(2) C44 0.052(3) 0.099(4) 0.086(4) -0.006(3) 0.033(3) 0.006(3) C45 0.046(3) 0.096(4) 0.084(4) 0.002(3) 0.019(3) -0.012(2) C46 0.049(3) 0.069(3) 0.062(3) 0.001(2) 0.011(2) -0.005(2) C47 0.043(2) 0.043(2) 0.050(2) 0.0057(18) 0.0103(18) -0.0004(17) C48 0.045(2) 0.042(2) 0.051(2) 0.0028(18) 0.0085(19) -0.0014(17) C49 0.059(3) 0.051(2) 0.061(3) -0.004(2) 0.010(2) -0.012(2) C50 0.070(3) 0.075(3) 0.066(3) -0.020(2) 0.019(3) -0.005(2) C51 0.062(3) 0.094(3) 0.082(4) -0.029(3) 0.033(3) -0.008(3) C52 0.046(3) 0.080(3) 0.075(3) -0.025(3) 0.018(2) -0.007(2) F1 0.098(2) 0.201(4) 0.135(3) -0.073(3) 0.059(2) -0.048(2) F2 0.106(3) 0.242(5) 0.278(7) -0.110(5) 0.081(4) -0.071(3) F3 0.150(3) 0.126(3) 0.117(3) -0.040(2) 0.061(2) -0.040(2) F4 0.487(11) 0.120(4) 0.237(6) 0.003(4) 0.263(7) 0.023(5) F5 0.295(6) 0.094(3) 0.176(4) -0.027(3) 0.142(4) -0.030(3) F6 0.167(4) 0.212(4) 0.095(3) -0.027(3) 0.013(3) -0.058(3) F7 0.171(4) 0.134(3) 0.151(4) 0.053(3) 0.072(3) -0.013(2) F8 0.101(3) 0.246(5) 0.244(5) 0.105(4) 0.075(3) 0.044(3) F9 0.468(17) 0.199(9) 0.263(12) 0.000 0.122(12) 0.000 F10 0.141(8) 0.167(8) 0.092(6) -0.051(5) -0.025(5) 0.028(6) F11 0.190(9) 0.158(8) 0.131(7) -0.032(6) 0.099(7) -0.034(6) F12 0.195(13) 0.279(14) 0.243(17) -0.138(15) 0.082(15) -0.130(11) F13 0.197(9) 0.249(8) 0.116(6) 0.046(6) 0.074(5) 0.021(6) F14 0.227(10) 0.255(11) 0.259(12) 0.133(10) 0.070(9) -0.008(7) F15 0.159(8) 0.411(17) 0.302(13) -0.217(13) 0.075(8) -0.087(9) N1 0.066(2) 0.053(2) 0.054(2) -0.0048(17) 0.0160(18) -0.0181(17) N2 0.062(2) 0.058(2) 0.056(2) 0.0014(17) 0.0185(18) -0.0120(17) N3 0.107(3) 0.046(2) 0.046(2) 0.0011(17) 0.001(2) -0.019(2) N4 0.048(2) 0.0489(19) 0.066(2) -0.0049(17) 0.0096(17) -0.0019(15) N5 0.052(2) 0.051(2) 0.058(2) -0.0003(17) 0.0094(17) -0.0035(16) N6 0.076(3) 0.057(2) 0.073(3) -0.0079(18) 0.033(2) 0.0056(18) N7 0.049(2) 0.059(2) 0.062(2) -0.0085(18) 0.0116(19) -0.0031(16) N8 0.053(2) 0.050(2) 0.080(3) -0.0053(19) 0.0038(18) 0.0053(17) N9 0.046(2) 0.0479(19) 0.071(3) -0.0043(18) 0.0174(18) 0.0013(15) N10 0.059(2) 0.051(2) 0.059(2) 0.0014(17) 0.0164(19) 0.0054(16) N11 0.0429(19) 0.0561(19) 0.058(2) 0.0012(17) 0.0172(16) 0.0018(15) N12 0.0374(18) 0.0564(19) 0.060(2) -0.0059(16) 0.0116(16) 0.0017(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 N5 1.966(3) . ? Cu1 N2 1.994(3) . ? Cu1 N1 2.004(3) . ? Cu1 N4 2.025(3) . ? Cu1 N3 2.224(4) . ? Cu2 C32 1.908(4) . ? Cu2 C21 1.909(4) . ? Cu2 N7 2.108(3) . ? Cu2 N6 2.112(4) . ? Cu3 N8 1.980(3) . ? Cu3 N9 1.997(3) . ? Cu3 N11 1.997(3) . ? Cu3 N12 2.070(3) . ? Cu3 N10 2.083(3) . ? B1 F4 1.298(10) . ? B1 F1 1.326(7) . ? B1 F3 1.374(8) . ? B1 F2 1.399(10) . ? B2 F5 1.322(6) . ? B2 F7 1.325(6) . ? B2 F6 1.339(6) . ? B2 F8 1.340(6) . ? B3 F12 1.240(12) . ? B3 F12 1.240(12) 2_655 ? B3 F9 1.286(13) . ? B3 F10 1.321(8) 2_655 ? B3 F10 1.321(8) . ? B3 F11 1.423(8) . ? B3 F11 1.423(8) 2_655 ? B4 F14 1.29(3) . ? B4 F14 1.29(3) 2 ? B4 F15 1.35(2) . ? B4 F15 1.35(2) 2 ? B4 F13 1.365(12) . ? B4 F13 1.365(12) 2 ? C1 N1 1.337(5) . ? C1 C2 1.377(6) . ? C1 H1 0.9300 . ? C2 C3 1.353(7) . ? C2 H2 0.9300 . ? C3 C4 1.373(7) . ? C3 H3 0.9300 . ? C4 C5 1.394(6) . ? C4 H4 0.9300 . ? C5 N1 1.347(5) . ? C5 C6 1.458(6) . ? C6 N2 1.350(5) . ? C6 C7 1.397(6) . ? C7 C8 1.363(7) . ? C7 H7 0.9300 . ? C8 C9 1.375(7) . ? C8 H8 0.9300 . ? C9 C10 1.377(6) . ? C9 H9 0.9300 . ? C10 N2 1.329(5) . ? C10 H10 0.9300 . ? C11 N3 1.349(6) . ? C11 C12 1.409(8) . ? C11 H11 0.9300 . ? C12 C13 1.366(10) . ? C12 H12 0.9300 . ? C13 C14 1.373(10) . ? C13 H13 0.9300 . ? C14 C15 1.376(7) . ? C14 H14 0.9300 . ? C15 N3 1.357(6) . ? C15 C16 1.464(7) . ? C16 N4 1.344(5) . ? C16 C17 1.408(7) . ? C17 C18 1.356(8) . ? C17 H17 0.9300 . ? C18 C19 1.352(8) . ? C18 H18 0.9300 . ? C19 C20 1.375(6) . ? C19 H19 0.9300 . ? C20 N4 1.344(5) . ? C20 H20 0.9300 . ? C21 N5 1.148(4) . ? C22 N6 1.343(6) . ? C22 C23 1.363(8) . ? C22 H22 0.9300 . ? C23 C24 1.379(9) . ? C23 H23 0.9300 . ? C24 C25 1.349(9) . ? C24 H24 0.9300 . ? C25 C26 1.393(7) . ? C25 H25 0.9300 . ? C26 N6 1.348(5) . ? C26 C27 1.464(6) . ? C27 N7 1.342(5) . ? C27 C28 1.397(6) . ? C28 C29 1.351(8) . ? C28 H28 0.9300 . ? C29 C30 1.355(9) . ? C29 H29 0.9300 . ? C30 C31 1.381(7) . ? C30 H30 0.9300 . ? C31 N7 1.337(5) . ? C31 H31 0.9300 . ? C32 N8 1.145(4) . ? C33 N9 1.340(5) . ? C33 C34 1.391(6) . ? C33 H33 0.9300 . ? C34 C35 1.344(8) . ? C34 H34 0.9300 . ? C35 C36 1.363(8) . ? C35 H35 0.9300 . ? C36 C37 1.397(6) . ? C36 H36 0.9300 . ? C37 N9 1.343(5) . ? C37 C38 1.459(6) . ? C38 N10 1.348(5) . ? C38 C39 1.399(6) . ? C39 C40 1.354(8) . ? C39 H39 0.9300 . ? C40 C41 1.352(8) . ? C40 H40 0.9300 . ? C41 C42 1.384(7) . ? C41 H41 0.9300 . ? C42 N10 1.334(5) . ? C42 H42 0.9300 . ? C43 N11 1.336(5) . ? C43 C44 1.387(6) . ? C43 H43 0.9300 . ? C44 C45 1.348(6) . ? C44 H44 0.9300 . ? C45 C46 1.366(6) . ? C45 H45 0.9300 . ? C46 C47 1.386(5) . ? C46 H46 0.9300 . ? C47 N11 1.344(5) . ? C47 C48 1.470(5) . ? C48 N12 1.352(4) . ? C48 C49 1.377(5) . ? C49 C50 1.376(5) . ? C49 H49 0.9300 . ? C50 C51 1.377(6) . ? C50 H50 0.9300 . ? C51 C52 1.372(6) . ? C51 H51 0.9300 . ? C52 N12 1.333(5) . ? C52 H52 0.9300 . ? F10 F12 1.370(16) 2_655 ? F12 F12 1.36(2) 2_655 ? F12 F10 1.370(16) 2_655 ? F13 F15 1.671(12) 2 ? F14 F14 1.78(2) 2 ? F15 F13 1.671(12) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cu1 N2 93.48(13) . . ? N5 Cu1 N1 160.78(13) . . ? N2 Cu1 N1 80.62(14) . . ? N5 Cu1 N4 90.63(13) . . ? N2 Cu1 N4 173.63(14) . . ? N1 Cu1 N4 93.94(14) . . ? N5 Cu1 N3 98.65(12) . . ? N2 Cu1 N3 107.39(16) . . ? N1 Cu1 N3 100.57(13) . . ? N4 Cu1 N3 76.74(16) . . ? C32 Cu2 C21 124.32(16) . . ? C32 Cu2 N7 107.90(14) . . ? C21 Cu2 N7 114.81(14) . . ? C32 Cu2 N6 114.15(15) . . ? C21 Cu2 N6 109.14(15) . . ? N7 Cu2 N6 76.79(15) . . ? N8 Cu3 N9 90.75(13) . . ? N8 Cu3 N11 92.07(13) . . ? N9 Cu3 N11 177.16(13) . . ? N8 Cu3 N12 126.70(14) . . ? N9 Cu3 N12 98.40(13) . . ? N11 Cu3 N12 79.61(13) . . ? N8 Cu3 N10 118.23(14) . . ? N9 Cu3 N10 79.95(14) . . ? N11 Cu3 N10 99.00(13) . . ? N12 Cu3 N10 115.06(12) . . ? F4 B1 F1 114.1(9) . . ? F4 B1 F3 111.4(7) . . ? F1 B1 F3 112.8(6) . . ? F4 B1 F2 107.9(7) . . ? F1 B1 F2 105.2(7) . . ? F3 B1 F2 104.8(8) . . ? F5 B2 F7 111.8(5) . . ? F5 B2 F6 107.0(5) . . ? F7 B2 F6 110.8(5) . . ? F5 B2 F8 108.4(5) . . ? F7 B2 F8 113.0(5) . . ? F6 B2 F8 105.4(5) . . ? F12 B3 F12 66.3(15) . 2_655 ? F12 B3 F9 146.8(7) . . ? F12 B3 F9 146.8(7) 2_655 . ? F12 B3 F10 64.6(7) . 2_655 ? F12 B3 F10 117.3(13) 2_655 2_655 ? F9 B3 F10 89.0(7) . 2_655 ? F12 B3 F10 117.3(13) . . ? F12 B3 F10 64.6(7) 2_655 . ? F9 B3 F10 89.0(7) . . ? F10 B3 F10 178.0(14) 2_655 . ? F12 B3 F11 73.7(7) . . ? F12 B3 F11 102.9(9) 2_655 . ? F9 B3 F11 92.0(6) . . ? F10 B3 F11 98.4(6) 2_655 . ? F10 B3 F11 81.7(6) . . ? F12 B3 F11 102.9(9) . 2_655 ? F12 B3 F11 73.7(7) 2_655 2_655 ? F9 B3 F11 92.0(6) . 2_655 ? F10 B3 F11 81.7(6) 2_655 2_655 ? F10 B3 F11 98.4(6) . 2_655 ? F11 B3 F11 176.1(12) . 2_655 ? F14 B4 F14 87(3) . 2 ? F14 B4 F15 85.6(7) . . ? F14 B4 F15 163(2) 2 . ? F14 B4 F15 163(2) . 2 ? F14 B4 F15 85.6(7) 2 2 ? F15 B4 F15 105(3) . 2 ? F14 B4 F13 93.0(10) . . ? F14 B4 F13 110.6(11) 2 . ? F15 B4 F13 84.6(16) . . ? F15 B4 F13 76.0(11) 2 . ? F14 B4 F13 110.6(11) . 2 ? F14 B4 F13 93.0(10) 2 2 ? F15 B4 F13 76.0(11) . 2 ? F15 B4 F13 84.6(16) 2 2 ? F13 B4 F13 148(3) . 2 ? N1 C1 C2 122.0(5) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 118.3(5) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 121.4(5) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C3 C4 C5 117.8(5) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? N1 C5 C4 120.9(5) . . ? N1 C5 C6 115.0(4) . . ? C4 C5 C6 124.1(5) . . ? N2 C6 C7 121.1(4) . . ? N2 C6 C5 114.5(4) . . ? C7 C6 C5 124.3(4) . . ? C8 C7 C6 119.4(5) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 119.5(5) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C8 C9 C10 118.5(5) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 123.2(5) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N3 C11 C12 121.3(7) . . ? N3 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 116.7(7) . . ? C13 C12 H12 121.6 . . ? C11 C12 H12 121.6 . . ? C12 C13 C14 122.8(8) . . ? C12 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C13 C14 C15 117.9(8) . . ? C13 C14 H14 121.1 . . ? C15 C14 H14 121.1 . . ? N3 C15 C14 121.3(6) . . ? N3 C15 C16 115.9(4) . . ? C14 C15 C16 122.7(7) . . ? N4 C16 C17 120.3(5) . . ? N4 C16 C15 115.6(5) . . ? C17 C16 C15 124.1(5) . . ? C18 C17 C16 118.7(5) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C19 C18 C17 121.5(6) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C18 C19 C20 117.4(6) . . ? C18 C19 H19 121.3 . . ? C20 C19 H19 121.3 . . ? N4 C20 C19 123.4(5) . . ? N4 C20 H20 118.3 . . ? C19 C20 H20 118.3 . . ? N5 C21 Cu2 177.8(4) . . ? N6 C22 C23 122.2(6) . . ? N6 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C22 C23 C24 118.8(7) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C25 C24 C23 120.7(7) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 117.7(6) . . ? C24 C25 H25 121.2 . . ? C26 C25 H25 121.2 . . ? N6 C26 C25 122.5(5) . . ? N6 C26 C27 114.8(4) . . ? C25 C26 C27 122.7(5) . . ? N7 C27 C28 121.8(5) . . ? N7 C27 C26 116.1(4) . . ? C28 C27 C26 122.1(5) . . ? C29 C28 C27 118.3(6) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C28 C29 C30 120.9(6) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C31 118.6(6) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? N7 C31 C30 122.3(5) . . ? N7 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? N8 C32 Cu2 176.2(4) . . ? N9 C33 C34 120.8(5) . . ? N9 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C35 C34 C33 119.9(6) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 119.6(6) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C37 119.8(5) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? N9 C37 C36 120.0(5) . . ? N9 C37 C38 116.0(4) . . ? C36 C37 C38 123.9(5) . . ? N10 C38 C39 121.4(5) . . ? N10 C38 C37 115.1(4) . . ? C39 C38 C37 123.4(5) . . ? C40 C39 C38 118.4(5) . . ? C40 C39 H39 120.8 . . ? C38 C39 H39 120.8 . . ? C41 C40 C39 120.4(6) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C42 119.5(6) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? N10 C42 C41 121.5(5) . . ? N10 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? N11 C43 C44 121.0(4) . . ? N11 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C45 C44 C43 119.4(4) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C44 C45 C46 119.8(4) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C45 C46 C47 119.5(4) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? N11 C47 C46 120.3(4) . . ? N11 C47 C48 114.9(3) . . ? C46 C47 C48 124.8(4) . . ? N12 C48 C49 121.5(4) . . ? N12 C48 C47 114.8(3) . . ? C49 C48 C47 123.6(3) . . ? C50 C49 C48 119.7(4) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C49 C50 C51 119.0(4) . . ? C49 C50 H50 120.5 . . ? C51 C50 H50 120.5 . . ? C52 C51 C50 118.2(4) . . ? C52 C51 H51 120.9 . . ? C50 C51 H51 120.9 . . ? N12 C52 C51 123.8(4) . . ? N12 C52 H52 118.1 . . ? C51 C52 H52 118.1 . . ? B3 F10 F12 54.9(6) . 2_655 ? B3 F12 F12 56.8(7) . 2_655 ? B3 F12 F10 60.6(7) . 2_655 ? F12 F12 F10 106.7(11) 2_655 2_655 ? B4 F13 F15 51.6(9) . 2 ? B4 F14 F14 46.6(15) . 2 ? B4 F15 F13 52.4(5) . 2 ? C1 N1 C5 119.5(4) . . ? C1 N1 Cu1 126.3(3) . . ? C5 N1 Cu1 114.2(3) . . ? C10 N2 C6 118.4(4) . . ? C10 N2 Cu1 126.8(3) . . ? C6 N2 Cu1 114.7(3) . . ? C11 N3 C15 119.9(5) . . ? C11 N3 Cu1 128.0(4) . . ? C15 N3 Cu1 111.9(3) . . ? C16 N4 C20 118.4(4) . . ? C16 N4 Cu1 119.1(3) . . ? C20 N4 Cu1 122.3(3) . . ? C21 N5 Cu1 178.2(3) . . ? C22 N6 C26 117.9(5) . . ? C22 N6 Cu2 126.1(4) . . ? C26 N6 Cu2 115.6(3) . . ? C31 N7 C27 118.1(4) . . ? C31 N7 Cu2 126.4(3) . . ? C27 N7 Cu2 115.5(3) . . ? C32 N8 Cu3 171.6(4) . . ? C33 N9 C37 119.9(4) . . ? C33 N9 Cu3 124.0(3) . . ? C37 N9 Cu3 115.7(3) . . ? C42 N10 C38 118.7(4) . . ? C42 N10 Cu3 128.2(3) . . ? C38 N10 Cu3 113.1(3) . . ? C43 N11 C47 119.9(3) . . ? C43 N11 Cu3 123.4(3) . . ? C47 N11 Cu3 116.7(2) . . ? C52 N12 C48 117.8(3) . . ? C52 N12 Cu3 128.3(3) . . ? C48 N12 Cu3 113.9(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.464 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.063