# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'RSC Advances' _journal_coden_cambridge 1500 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email dli@stu.edu.cn _publ_contact_author_name 'Dan Li' _publ_author_name 'Dan Li' data_HL _database_code_depnum_ccdc_archive 'CCDC 838375' #TrackingRef '- complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H15 N3' _chemical_formula_sum 'C12 H15 N3' _chemical_formula_weight 201.27 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 17.241(3) _cell_length_b 34.415(5) _cell_length_c 8.1449(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4832.8(13) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 860 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 24.42 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9865 _exptl_absorpt_correction_T_max 0.9919 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7325 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2203 _reflns_number_gt 1096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -2(5) _refine_ls_number_reflns 2203 _refine_ls_number_parameters 142 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1248 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.2047 _refine_ls_wR_factor_gt 0.1631 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 4.799 _refine_ls_shift/su_mean 0.068 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 N1 N 0.3674(3) -0.07009(9) 0.9365(5) 0.0978(12) Uani 1 1 d . . . N2 N 0.35524(18) 0.07316(8) 0.8001(4) 0.0825(10) Uani 1 1 d . . . N3 N 0.3211(2) 0.10816(8) 0.8083(5) 0.0897(11) Uani 1 1 d . . . H1N H 0.3399 0.1286 0.7623 0.108 Uiso 1 1 calc R . . C1 C 0.3917(3) -0.00737(12) 0.8237(6) 0.1007(15) Uani 1 1 d . . . H1 H 0.4236 0.0080 0.7585 0.121 Uiso 1 1 calc R . . C2 C 0.4077(3) -0.04603(12) 0.8442(6) 0.1073(16) Uani 1 1 d . . . H2 H 0.4503 -0.0561 0.7887 0.129 Uiso 1 1 calc R . . C3 C 0.3054(3) -0.05466(12) 1.0031(7) 0.1119(17) Uani 1 1 d . . . H3 H 0.2731 -0.0711 1.0628 0.134 Uiso 1 1 calc R . . C4 C 0.2841(3) -0.01640(12) 0.9923(7) 0.1004(14) Uani 1 1 d . . . H4 H 0.2402 -0.0075 1.0469 0.120 Uiso 1 1 calc R . . C5 C 0.3277(2) 0.00866(9) 0.9008(5) 0.0759(10) Uani 1 1 d . . . C6 C 0.3091(2) 0.05011(9) 0.8845(5) 0.0758(11) Uani 1 1 d . . . C7 C 0.2459(2) 0.07087(11) 0.9478(5) 0.0921(13) Uani 1 1 d . . . H7 H 0.2059 0.0611 1.0126 0.110 Uiso 1 1 calc R . . C8 C 0.2548(3) 0.10841(10) 0.8951(6) 0.0893(12) Uani 1 1 d . . . C9 C 0.2072(3) 0.14434(12) 0.9172(7) 0.1167(18) Uani 1 1 d . . . H9A H 0.2216 0.1624 0.8309 0.140 Uiso 1 1 calc R . . H9B H 0.1534 0.1373 0.8989 0.140 Uiso 1 1 calc R . . C10 C 0.2110(6) 0.1645(3) 1.0668(13) 0.240(7) Uani 1 1 d . . . H10 H 0.257(7) 0.178(4) 1.03(2) 0.288 Uiso 1 1 calc . . . C11 C 0.1646(8) 0.2020(3) 1.0645(14) 0.275(6) Uani 1 1 d . . . H11A H 0.1925 0.2218 1.1227 0.412 Uiso 1 1 calc R . . H11B H 0.1153 0.1978 1.1164 0.412 Uiso 1 1 calc R . . H11C H 0.1566 0.2101 0.9530 0.412 Uiso 1 1 calc R . . C12 C 0.2437(8) 0.1568(4) 1.2068(16) 0.293(7) Uani 1 1 d . . . H12A H 0.2051 0.1482 1.2835 0.440 Uiso 1 1 calc R . . H12B H 0.2684 0.1798 1.2482 0.440 Uiso 1 1 calc R . . H12C H 0.2817 0.1368 1.1921 0.440 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.134(3) 0.0534(18) 0.106(3) 0.0079(18) -0.005(2) 0.005(2) N2 0.103(2) 0.0469(16) 0.098(2) 0.0101(15) 0.0029(19) -0.0056(16) N3 0.118(3) 0.0483(18) 0.103(3) 0.0054(16) -0.012(2) -0.0011(17) C1 0.116(3) 0.068(2) 0.118(4) 0.028(3) 0.026(3) 0.007(2) C2 0.125(4) 0.062(3) 0.135(4) 0.009(3) 0.025(3) 0.017(2) C3 0.129(4) 0.062(3) 0.145(5) 0.022(3) 0.037(3) -0.008(2) C4 0.116(3) 0.061(2) 0.125(4) 0.019(2) 0.030(3) 0.002(2) C5 0.090(3) 0.0508(19) 0.087(3) 0.0077(19) 0.002(2) -0.0015(18) C6 0.093(3) 0.0516(19) 0.083(3) 0.007(2) -0.0087(19) -0.002(2) C7 0.093(3) 0.064(2) 0.119(4) 0.004(2) 0.004(2) 0.003(2) C8 0.106(3) 0.057(2) 0.104(3) -0.004(2) -0.006(3) 0.009(2) C9 0.134(4) 0.072(3) 0.144(5) -0.009(3) -0.019(4) 0.024(2) C10 0.353(16) 0.225(10) 0.142(7) -0.077(8) -0.102(9) 0.198(11) C11 0.419(14) 0.188(8) 0.217(10) -0.095(7) -0.097(10) 0.187(10) C12 0.375(15) 0.314(13) 0.191(9) -0.095(10) -0.051(11) 0.219(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 N1 C3 1.311(6) . ? N1 C2 1.316(5) . ? N2 C6 1.317(5) . ? N2 N3 1.342(4) . ? N3 C8 1.344(5) . ? C1 C2 1.369(6) . ? C1 C5 1.384(6) . ? C3 C4 1.370(6) . ? C4 C5 1.365(6) . ? C5 C6 1.468(4) . ? C6 C7 1.401(6) . ? C7 C8 1.370(5) . ? C8 C9 1.495(6) . ? C9 C10 1.403(10) . ? C10 C12 1.298(13) . ? C10 C11 1.520(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 N1 C2 114.3(3) . . ? C6 N2 N3 104.4(3) . . ? N2 N3 C8 113.9(3) . . ? C2 C1 C5 119.5(4) . . ? N1 C2 C1 125.1(4) . . ? N1 C3 C4 125.5(4) . . ? C5 C4 C3 119.7(4) . . ? C4 C5 C1 115.8(3) . . ? C4 C5 C6 122.8(4) . . ? C1 C5 C6 121.4(3) . . ? N2 C6 C7 110.8(3) . . ? N2 C6 C5 120.0(4) . . ? C7 C6 C5 129.2(4) . . ? C8 C7 C6 106.1(4) . . ? N3 C8 C7 104.8(3) . . ? N3 C8 C9 122.4(4) . . ? C7 C8 C9 132.8(5) . . ? C10 C9 C8 119.2(5) . . ? C12 C10 C9 133.0(7) . . ? C12 C10 C11 114.3(7) . . ? C9 C10 C11 112.6(7) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.257 _refine_diff_density_min -0.120 _refine_diff_density_rms 0.031 data_1 _database_code_depnum_ccdc_archive 'CCDC 838376' #TrackingRef '- complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H86 Cu9 I3 N18 O' _chemical_formula_sum 'C72 H86 Cu9 I3 N18 O' _chemical_formula_weight 2172.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6702(2) _cell_length_b 17.3216(3) _cell_length_c 17.4721(2) _cell_angle_alpha 84.6490(10) _cell_angle_beta 79.6620(10) _cell_angle_gamma 77.6360(10) _cell_volume 3969.18(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2410 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 24 _exptl_crystal_description block _exptl_crystal_colour ywllow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 3.581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5344 _exptl_absorpt_correction_T_max 0.7159 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51231 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 27.50 _reflns_number_total 18116 _reflns_number_gt 12382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+1.0086P] 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 18116 _refine_ls_number_parameters 938 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.003 _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 C1 C 0.8052(4) 0.5780(4) 0.4899(3) 0.0271(13) Uani 1 1 d . . . H1 H 0.7789 0.6120 0.5316 0.033 Uiso 1 1 calc R . . C2 C 0.7453(4) 0.5313(4) 0.4681(3) 0.0274(13) Uani 1 1 d . . . H2 H 0.6776 0.5351 0.4949 0.033 Uiso 1 1 calc R . . C3 C 0.8751(4) 0.4754(4) 0.3761(3) 0.0299(13) Uani 1 1 d . . . H3 H 0.9009 0.4385 0.3368 0.036 Uiso 1 1 calc R . . C4 C 0.9387(4) 0.5197(4) 0.3938(3) 0.0277(13) Uani 1 1 d . . . H4 H 1.0068 0.5126 0.3672 0.033 Uiso 1 1 calc R . . C5 C 0.9051(4) 0.5749(4) 0.4501(3) 0.0247(12) Uani 1 1 d . . . C6 C 0.9676(4) 0.6288(4) 0.4643(3) 0.0250(12) Uani 1 1 d . . . C7 C 1.0714(4) 0.6241(4) 0.4428(3) 0.0257(12) Uani 1 1 d . . . H7 H 1.1190 0.5831 0.4158 0.031 Uiso 1 1 calc R . . C8 C 1.0910(4) 0.6920(4) 0.4690(3) 0.0307(14) Uani 1 1 d . . . C9 C 1.1865(5) 0.7236(5) 0.4616(4) 0.0421(17) Uani 1 1 d . . . H9A H 1.2444 0.6786 0.4649 0.051 Uiso 1 1 calc R . . H9B H 1.1808 0.7568 0.5060 0.051 Uiso 1 1 calc R . . C10 C 1.2086(5) 0.7731(5) 0.3847(4) 0.0408(17) Uani 1 1 d . . . H10 H 1.1428 0.8064 0.3735 0.049 Uiso 1 1 calc R . . C11 C 1.2512(5) 0.7166(5) 0.3179(4) 0.0449(18) Uani 1 1 d . . . H11A H 1.2637 0.7477 0.2686 0.067 Uiso 1 1 calc R . . H11B H 1.2019 0.6840 0.3144 0.067 Uiso 1 1 calc R . . H11C H 1.3149 0.6823 0.3283 0.067 Uiso 1 1 calc R . . C12 C 1.2810(6) 0.8281(5) 0.3878(5) 0.059(2) Uani 1 1 d . . . H12A H 1.2537 0.8630 0.4310 0.089 Uiso 1 1 calc R . . H12B H 1.2885 0.8602 0.3386 0.089 Uiso 1 1 calc R . . H12C H 1.3474 0.7966 0.3957 0.089 Uiso 1 1 calc R . . C13 C 0.6394(4) 0.7400(4) 0.4144(3) 0.0279(13) Uani 1 1 d . . . H13 H 0.6934 0.7678 0.4081 0.033 Uiso 1 1 calc R . . C14 C 0.6334(4) 0.6934(4) 0.3568(3) 0.0273(13) Uani 1 1 d . . . H14 H 0.6834 0.6906 0.3112 0.033 Uiso 1 1 calc R . . C15 C 0.4895(4) 0.6603(4) 0.4256(3) 0.0299(14) Uani 1 1 d . . . H15 H 0.4355 0.6328 0.4299 0.036 Uiso 1 1 calc R . . C16 C 0.4896(4) 0.7065(4) 0.4854(3) 0.0296(13) Uani 1 1 d . . . H16 H 0.4364 0.7108 0.5290 0.035 Uiso 1 1 calc R . . C17 C 0.5676(4) 0.7468(3) 0.4817(3) 0.0264(13) Uani 1 1 d . . . C18 C 0.5716(5) 0.7942(4) 0.5467(3) 0.0290(13) Uani 1 1 d . . . C19 C 0.4941(5) 0.8365(4) 0.5970(4) 0.0354(15) Uani 1 1 d . . . H19 H 0.4232 0.8417 0.5981 0.043 Uiso 1 1 calc R . . C20 C 0.5409(5) 0.8697(4) 0.6456(3) 0.0339(15) Uani 1 1 d . . . C21 C 0.4958(5) 0.9297(4) 0.7059(4) 0.0440(18) Uani 1 1 d . . . H21A H 0.5188 0.9096 0.7560 0.053 Uiso 1 1 calc R . . H21B H 0.4208 0.9372 0.7143 0.053 Uiso 1 1 calc R . . C22 C 0.5286(6) 1.0148(6) 0.6793(5) 0.067(3) Uani 1 1 d . . . H22 H 0.6035 1.0081 0.6774 0.080 Uiso 1 1 calc R . . C23 C 0.4729(8) 1.0719(6) 0.7432(6) 0.083(3) Uani 1 1 d . . . H23A H 0.4904 1.1240 0.7298 0.124 Uiso 1 1 calc R . . H23B H 0.4934 1.0511 0.7933 0.124 Uiso 1 1 calc R . . H23C H 0.3994 1.0769 0.7472 0.124 Uiso 1 1 calc R . . C24 C 0.5035(7) 1.0444(5) 0.6017(5) 0.062(2) Uani 1 1 d . . . H24A H 0.5253 1.0948 0.5870 0.092 Uiso 1 1 calc R . . H24B H 0.4300 1.0523 0.6034 0.092 Uiso 1 1 calc R . . H24C H 0.5384 1.0057 0.5632 0.092 Uiso 1 1 calc R . . C25 C 0.7123(5) 0.9643(4) 0.8201(4) 0.0414(16) Uani 1 1 d . . . H25 H 0.7142 0.9139 0.8018 0.050 Uiso 1 1 calc R . . C26 C 0.6430(6) 0.9914(5) 0.8837(4) 0.052(2) Uani 1 1 d . . . H26 H 0.5983 0.9581 0.9084 0.062 Uiso 1 1 calc R . . C27 C 0.6998(7) 1.1045(5) 0.8761(5) 0.059(2) Uani 1 1 d . . . H27 H 0.6967 1.1543 0.8959 0.071 Uiso 1 1 calc R . . C28 C 0.7708(6) 1.0836(5) 0.8125(5) 0.0511(19) Uani 1 1 d . . . H28 H 0.8140 1.1185 0.7888 0.061 Uiso 1 1 calc R . . C29 C 0.7792(5) 1.0105(4) 0.7828(4) 0.0398(17) Uani 1 1 d . . . C30 C 0.8590(5) 0.9856(4) 0.7163(4) 0.0408(16) Uani 1 1 d . . . C31 C 0.9452(6) 1.0121(5) 0.6884(5) 0.054(2) Uani 1 1 d . . . H31 H 0.9646 1.0559 0.7061 0.065 Uiso 1 1 calc R . . C32 C 1.0001(6) 0.9649(5) 0.6301(5) 0.054(2) Uani 1 1 d . . . C33 C 1.1007(6) 0.9625(5) 0.5783(5) 0.059(2) Uani 1 1 d . . . H33A H 1.0901 0.9652 0.5235 0.070 Uiso 1 1 calc R . . H33B H 1.1453 0.9108 0.5884 0.070 Uiso 1 1 calc R . . C34 C 1.1566(6) 1.0282(6) 0.5876(5) 0.063(2) Uani 1 1 d . . . H34 H 1.1108 1.0815 0.5853 0.075 Uiso 1 1 calc R . . C35 C 1.1957(7) 1.0106(7) 0.6682(5) 0.088(4) Uani 1 1 d . . . H35A H 1.2299 1.0526 0.6767 0.132 Uiso 1 1 calc R . . H35B H 1.2436 0.9596 0.6678 0.132 Uiso 1 1 calc R . . H35C H 1.1380 1.0087 0.7101 0.132 Uiso 1 1 calc R . . C36 C 1.2475(6) 1.0227(6) 0.5236(5) 0.070(3) Uani 1 1 d . . . H36A H 1.2246 1.0338 0.4729 0.105 Uiso 1 1 calc R . . H36B H 1.2896 0.9694 0.5257 0.105 Uiso 1 1 calc R . . H36C H 1.2874 1.0615 0.5306 0.105 Uiso 1 1 calc R . . C37 C 0.4746(4) 0.4134(4) 0.0827(3) 0.0242(12) Uani 1 1 d . . . H37 H 0.4476 0.4498 0.0440 0.029 Uiso 1 1 calc R . . C38 C 0.5550(4) 0.4262(4) 0.1143(3) 0.0249(12) Uani 1 1 d . A . H38 H 0.5817 0.4722 0.0966 0.030 Uiso 1 1 calc R . . C39 C 0.5575(4) 0.3134(4) 0.1932(3) 0.0307(14) Uani 1 1 d . A . H39 H 0.5859 0.2784 0.2323 0.037 Uiso 1 1 calc R . . C40 C 0.4780(4) 0.2959(4) 0.1649(3) 0.0293(13) Uani 1 1 d . . . H40 H 0.4532 0.2494 0.1839 0.035 Uiso 1 1 calc R . . C41 C 0.4333(4) 0.3468(3) 0.1078(3) 0.0230(12) Uani 1 1 d . . . C42 C 0.3501(4) 0.3273(3) 0.0762(3) 0.0228(12) Uani 1 1 d . . . C43 C 0.3316(4) 0.2512(4) 0.0753(3) 0.0275(13) Uani 1 1 d . . . H43 H 0.3687 0.2030 0.0951 0.033 Uiso 1 1 calc R . . C44 C 0.2474(4) 0.2617(4) 0.0394(3) 0.0283(13) Uani 1 1 d . . . C45 C 0.2006(5) 0.1993(4) 0.0159(4) 0.0330(14) Uani 1 1 d . . . H45A H 0.1379 0.2246 -0.0048 0.040 Uiso 1 1 calc R . . H45B H 0.1816 0.1649 0.0623 0.040 Uiso 1 1 calc R . . C46 C 0.2729(6) 0.1484(5) -0.0462(5) 0.060(2) Uani 1 1 d . . . H46 H 0.3367 0.1252 -0.0248 0.072 Uiso 1 1 calc R . . C47 C 0.3007(7) 0.2000(6) -0.1198(5) 0.074(3) Uani 1 1 d . . . H47A H 0.3482 0.1670 -0.1585 0.111 Uiso 1 1 calc R . . H47B H 0.3327 0.2414 -0.1065 0.111 Uiso 1 1 calc R . . H47C H 0.2392 0.2244 -0.1413 0.111 Uiso 1 1 calc R . . C48 C 0.2274(8) 0.0804(6) -0.0629(7) 0.091(4) Uani 1 1 d . . . H48A H 0.2140 0.0477 -0.0149 0.136 Uiso 1 1 calc R . . H48B H 0.2752 0.0480 -0.1020 0.136 Uiso 1 1 calc R . . H48C H 0.1638 0.1015 -0.0828 0.136 Uiso 1 1 calc R . . C49 C 0.3226(4) 0.5812(4) 0.1479(3) 0.0250(12) Uani 1 1 d . . . H49 H 0.2692 0.5531 0.1519 0.030 Uiso 1 1 calc R . . C50 C 0.3850(4) 0.5671(4) 0.2029(3) 0.0273(13) Uani 1 1 d . . . H50 H 0.3731 0.5292 0.2446 0.033 Uiso 1 1 calc R . . C51 C 0.4761(4) 0.6573(4) 0.1420(3) 0.0289(14) Uani 1 1 d . . . H51 H 0.5304 0.6843 0.1396 0.035 Uiso 1 1 calc R . . C52 C 0.4159(4) 0.6754(4) 0.0843(3) 0.0272(13) Uani 1 1 d . . . H52 H 0.4283 0.7141 0.0436 0.033 Uiso 1 1 calc R . . C53 C 0.3367(4) 0.6356(3) 0.0871(3) 0.0214(12) Uani 1 1 d . . . C54 C 0.2674(4) 0.6547(3) 0.0285(3) 0.0206(11) Uani 1 1 d . . . C55 C 0.2341(4) 0.7267(3) -0.0077(3) 0.0234(12) Uani 1 1 d . . . H55 H 0.2549 0.7750 -0.0039 0.028 Uiso 1 1 calc R . . C56 C 0.1637(4) 0.7146(3) -0.0513(3) 0.0238(12) Uani 1 1 d . . . C57 C 0.0977(5) 0.7729(4) -0.0995(4) 0.0309(14) Uani 1 1 d . . . H57A H 0.0257 0.7712 -0.0789 0.037 Uiso 1 1 calc R . . H57B H 0.1123 0.7560 -0.1536 0.037 Uiso 1 1 calc R . . C58 C 0.1112(5) 0.8579(4) -0.1010(4) 0.0429(17) Uani 1 1 d . . . H58 H 0.1070 0.8738 -0.0467 0.052 Uiso 1 1 calc R . . C59 C 0.0322(7) 0.9131(5) -0.1408(6) 0.075(3) Uani 1 1 d . . . H59A H -0.0356 0.9097 -0.1126 0.113 Uiso 1 1 calc R . . H59B H 0.0386 0.8982 -0.1945 0.113 Uiso 1 1 calc R . . H59C H 0.0423 0.9675 -0.1412 0.113 Uiso 1 1 calc R . . C60 C 0.2165(7) 0.8676(5) -0.1515(5) 0.067(3) Uani 1 1 d . . . H60A H 0.2718 0.8332 -0.1285 0.101 Uiso 1 1 calc R . . H60B H 0.2236 0.9228 -0.1526 0.101 Uiso 1 1 calc R . . H60C H 0.2193 0.8528 -0.2048 0.101 Uiso 1 1 calc R . . C61 C -0.0557(4) 0.6716(4) -0.2117(4) 0.0309(14) Uani 1 1 d . . . H61 H 0.0037 0.6675 -0.1892 0.037 Uiso 1 1 calc R . . C62 C -0.0979(5) 0.7425(4) -0.2467(4) 0.0336(14) Uani 1 1 d . . . H62 H -0.0661 0.7863 -0.2475 0.040 Uiso 1 1 calc R . . C63 C -0.2244(4) 0.6900(4) -0.2773(3) 0.0291(13) Uani 1 1 d . . . H63 H -0.2836 0.6961 -0.3005 0.035 Uiso 1 1 calc R . . C64 C -0.1880(4) 0.6171(4) -0.2434(3) 0.0270(13) Uani 1 1 d . . . H64 H -0.2221 0.5748 -0.2432 0.032 Uiso 1 1 calc R . . C65 C -0.1003(4) 0.6055(3) -0.2092(3) 0.0228(12) Uani 1 1 d . . . C66 C -0.0596(4) 0.5294(4) -0.1749(3) 0.0225(12) Uani 1 1 d . . . C67 C -0.0727(4) 0.4564(4) -0.1943(3) 0.0243(12) Uani 1 1 d . . . H67 H -0.1099 0.4468 -0.2322 0.029 Uiso 1 1 calc R . . C68 C -0.0198(4) 0.4006(3) -0.1463(3) 0.0242(12) Uani 1 1 d . . . C69 C -0.0081(5) 0.3123(4) -0.1421(4) 0.0309(14) Uani 1 1 d . . . H69A H 0.0528 0.2881 -0.1186 0.037 Uiso 1 1 calc R . . H69B H -0.0677 0.2976 -0.1072 0.037 Uiso 1 1 calc R . . C70 C 0.0016(6) 0.2783(4) -0.2194(4) 0.0471(18) Uani 1 1 d . . . H70 H -0.0576 0.3060 -0.2445 0.057 Uiso 1 1 calc R . . C71 C 0.0965(6) 0.2873(5) -0.2739(4) 0.0502(19) Uani 1 1 d . . . H71A H 0.1002 0.3435 -0.2814 0.075 Uiso 1 1 calc R . . H71B H 0.0961 0.2667 -0.3242 0.075 Uiso 1 1 calc R . . H71C H 0.1556 0.2578 -0.2519 0.075 Uiso 1 1 calc R . . C72 C -0.0029(9) 0.1885(5) -0.2069(6) 0.086(3) Uani 1 1 d . . . H72A H 0.0038 0.1662 -0.2575 0.129 Uiso 1 1 calc R . . H72B H -0.0679 0.1826 -0.1752 0.129 Uiso 1 1 calc R . . H72C H 0.0528 0.1605 -0.1800 0.129 Uiso 1 1 calc R . . Cu1 Cu 0.68444(6) 0.43171(5) 0.36709(5) 0.0376(2) Uani 1 1 d . . . Cu2 Cu 0.70003(6) 0.40437(5) 0.22335(5) 0.0395(2) Uani 1 1 d . A . Cu3 Cu 0.55713(5) 0.57524(5) 0.28204(4) 0.03232(19) Uani 1 1 d . . . Cu4 Cu 0.79404(5) 0.74924(4) 0.53321(4) 0.02698(17) Uani 1 1 d . . . Cu5 Cu 0.75680(6) 0.86320(5) 0.66685(4) 0.03178(18) Uani 1 1 d . . . Cu6 Cu 0.97308(6) 0.82440(5) 0.56155(5) 0.0374(2) Uani 1 1 d . . . Cu7 Cu 0.24852(5) 0.48985(4) 0.02501(4) 0.02193(15) Uani 1 1 d . . . Cu8 Cu 0.11594(5) 0.39289(4) -0.03566(4) 0.02472(16) Uani 1 1 d . . . Cu9 Cu 0.07604(5) 0.57898(4) -0.07963(4) 0.02307(16) Uani 1 1 d . . . I1 I 0.73656(3) 0.54196(3) 0.19268(2) 0.02936(10) Uani 1 1 d . A . I2 I 0.49595(3) 0.45496(3) 0.37023(2) 0.03200(11) Uani 1 1 d . A . I3 I 0.7802(3) 0.29341(19) 0.3166(4) 0.0312(5) Uani 0.85(3) 1 d P A 1 I3' I 0.793(2) 0.2959(12) 0.297(2) 0.040(3) Uani 0.15(3) 1 d PU A 2 N1 N 0.7787(4) 0.4810(3) 0.4109(3) 0.0289(11) Uani 1 1 d . A . N2 N 0.9261(3) 0.6960(3) 0.5016(3) 0.0263(11) Uani 1 1 d . . . N3 N 1.0030(4) 0.7350(3) 0.5042(3) 0.0321(12) Uani 1 1 d . . . N4 N 0.5604(3) 0.6515(3) 0.3616(3) 0.0268(11) Uani 1 1 d . A . N5 N 0.6612(4) 0.8001(3) 0.5657(3) 0.0261(11) Uani 1 1 d . . . N6 N 0.6414(4) 0.8473(3) 0.6273(3) 0.0292(11) Uani 1 1 d . . . N7 N 0.6342(6) 1.0613(4) 0.9132(4) 0.0600(19) Uani 1 1 d . . . N8 N 0.8557(4) 0.9237(3) 0.6748(3) 0.0349(12) Uani 1 1 d . . . N9 N 0.9444(4) 0.9097(3) 0.6229(3) 0.0417(14) Uani 1 1 d . . . N10 N 0.5969(3) 0.3773(3) 0.1685(3) 0.0265(11) Uani 1 1 d . . . N11 N 0.2806(3) 0.3802(3) 0.0431(2) 0.0218(10) Uani 1 1 d . . . N12 N 0.2165(3) 0.3387(3) 0.0207(3) 0.0248(10) Uani 1 1 d . . . N13 N 0.4616(3) 0.6039(3) 0.2010(3) 0.0262(11) Uani 1 1 d . A . N14 N 0.2217(3) 0.5992(3) 0.0076(2) 0.0211(10) Uani 1 1 d . . . N15 N 0.1572(3) 0.6375(3) -0.0420(3) 0.0213(10) Uani 1 1 d . . . N16 N -0.1813(4) 0.7531(3) -0.2795(3) 0.0313(12) Uani 1 1 d . . . N17 N -0.0010(3) 0.5175(3) -0.1177(3) 0.0214(10) Uani 1 1 d . . . N18 N 0.0218(3) 0.4377(3) -0.1007(3) 0.0222(10) Uani 1 1 d . . . O1W O 0.5483(5) 0.1161(5) 0.0624(4) 0.097(2) Uani 1 1 d . . . H1W1 H 0.5780 0.1187 0.0161 0.145 Uiso 1 1 d R . . H1W2 H 0.5866 0.1112 0.0959 0.145 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 C1 0.028(3) 0.023(3) 0.029(3) 0.000(2) -0.007(2) 0.000(3) C2 0.021(3) 0.025(3) 0.035(3) 0.002(3) -0.005(2) -0.002(2) C3 0.032(3) 0.026(4) 0.029(3) -0.006(3) -0.005(2) 0.001(3) C4 0.023(3) 0.030(4) 0.028(3) -0.002(3) -0.002(2) -0.002(3) C5 0.026(3) 0.024(3) 0.025(3) 0.001(2) -0.008(2) -0.003(2) C6 0.024(3) 0.026(3) 0.024(3) 0.000(2) -0.008(2) -0.002(2) C7 0.028(3) 0.022(3) 0.027(3) 0.002(2) -0.008(2) -0.004(2) C8 0.030(3) 0.040(4) 0.023(3) 0.000(3) -0.006(2) -0.009(3) C9 0.032(3) 0.060(5) 0.039(4) -0.014(3) -0.007(3) -0.015(3) C10 0.039(4) 0.055(5) 0.035(4) -0.010(3) 0.003(3) -0.028(3) C11 0.038(4) 0.054(5) 0.045(4) -0.016(4) -0.002(3) -0.013(3) C12 0.050(5) 0.058(6) 0.071(6) -0.002(4) -0.013(4) -0.011(4) C13 0.033(3) 0.025(3) 0.026(3) 0.002(2) -0.008(2) -0.006(3) C14 0.030(3) 0.027(3) 0.023(3) 0.000(2) -0.008(2) -0.002(3) C15 0.028(3) 0.036(4) 0.028(3) -0.002(3) -0.008(2) -0.008(3) C16 0.027(3) 0.031(4) 0.028(3) -0.002(3) -0.003(2) 0.000(3) C17 0.034(3) 0.019(3) 0.025(3) 0.004(2) -0.015(2) 0.004(3) C18 0.038(3) 0.023(3) 0.025(3) -0.005(2) -0.010(2) 0.002(3) C19 0.030(3) 0.037(4) 0.036(3) -0.004(3) -0.010(3) 0.006(3) C20 0.037(3) 0.034(4) 0.030(3) -0.007(3) -0.011(3) 0.002(3) C21 0.045(4) 0.049(5) 0.037(4) -0.017(3) -0.014(3) 0.005(3) C22 0.055(5) 0.069(7) 0.076(6) -0.045(5) -0.017(4) 0.011(4) C23 0.086(7) 0.069(7) 0.089(7) -0.034(6) -0.019(6) 0.010(6) C24 0.070(6) 0.046(5) 0.067(5) -0.016(4) -0.024(4) 0.007(4) C25 0.050(4) 0.037(4) 0.040(4) -0.006(3) -0.011(3) -0.010(3) C26 0.058(5) 0.048(5) 0.047(4) -0.008(4) -0.010(4) 0.000(4) C27 0.087(6) 0.043(5) 0.047(5) -0.013(4) -0.013(4) -0.004(5) C28 0.061(5) 0.037(5) 0.057(5) -0.012(4) -0.019(4) -0.001(4) C29 0.045(4) 0.036(4) 0.039(4) -0.014(3) -0.020(3) 0.007(3) C30 0.050(4) 0.039(4) 0.038(4) -0.003(3) -0.009(3) -0.019(3) C31 0.065(5) 0.046(5) 0.061(5) -0.018(4) -0.012(4) -0.025(4) C32 0.062(5) 0.048(5) 0.063(5) -0.016(4) -0.009(4) -0.028(4) C33 0.056(5) 0.060(6) 0.068(5) -0.027(4) -0.015(4) -0.015(4) C34 0.057(5) 0.083(7) 0.056(5) -0.001(5) -0.015(4) -0.028(5) C35 0.068(6) 0.149(11) 0.064(6) -0.011(6) -0.022(5) -0.046(7) C36 0.059(5) 0.095(8) 0.062(5) 0.021(5) -0.019(4) -0.032(5) C37 0.020(3) 0.027(3) 0.025(3) -0.003(2) -0.004(2) -0.001(2) C38 0.022(3) 0.026(3) 0.027(3) -0.009(2) -0.003(2) -0.004(2) C39 0.035(3) 0.028(4) 0.030(3) -0.001(3) -0.016(3) 0.000(3) C40 0.033(3) 0.025(3) 0.032(3) -0.002(3) -0.014(3) -0.004(3) C41 0.023(3) 0.022(3) 0.023(3) -0.001(2) -0.007(2) 0.000(2) C42 0.022(3) 0.019(3) 0.026(3) 0.000(2) -0.006(2) 0.000(2) C43 0.031(3) 0.017(3) 0.036(3) 0.005(3) -0.013(2) -0.005(2) C44 0.027(3) 0.021(3) 0.037(3) 0.000(3) -0.009(2) -0.003(2) C45 0.031(3) 0.025(3) 0.047(4) 0.006(3) -0.016(3) -0.010(3) C46 0.056(5) 0.044(5) 0.093(7) -0.023(5) -0.034(5) -0.011(4) C47 0.078(6) 0.079(7) 0.067(6) -0.023(5) -0.005(5) -0.018(5) C48 0.102(8) 0.050(6) 0.138(10) -0.037(6) -0.047(7) -0.018(6) C49 0.021(3) 0.029(3) 0.024(3) -0.004(2) -0.001(2) -0.004(2) C50 0.023(3) 0.037(4) 0.021(3) -0.003(3) -0.003(2) -0.005(3) C51 0.026(3) 0.036(4) 0.028(3) -0.011(3) -0.005(2) -0.008(3) C52 0.024(3) 0.029(3) 0.029(3) -0.006(3) -0.003(2) -0.007(3) C53 0.020(3) 0.017(3) 0.026(3) -0.007(2) -0.002(2) 0.000(2) C54 0.021(3) 0.021(3) 0.021(3) 0.000(2) -0.005(2) -0.007(2) C55 0.027(3) 0.019(3) 0.026(3) -0.006(2) -0.004(2) -0.006(2) C56 0.024(3) 0.022(3) 0.026(3) 0.003(2) -0.002(2) -0.008(2) C57 0.034(3) 0.023(3) 0.038(3) 0.002(3) -0.011(3) -0.009(3) C58 0.055(4) 0.019(4) 0.057(4) 0.002(3) -0.021(4) -0.005(3) C59 0.064(6) 0.038(5) 0.124(8) 0.026(5) -0.038(6) -0.004(4) C60 0.092(7) 0.048(5) 0.079(6) 0.013(5) -0.042(5) -0.032(5) C61 0.031(3) 0.027(4) 0.040(3) 0.003(3) -0.017(3) -0.008(3) C62 0.038(3) 0.025(4) 0.043(4) 0.001(3) -0.021(3) -0.008(3) C63 0.025(3) 0.036(4) 0.029(3) 0.007(3) -0.013(2) -0.009(3) C64 0.022(3) 0.031(4) 0.032(3) 0.006(3) -0.009(2) -0.012(3) C65 0.020(3) 0.026(3) 0.022(3) 0.001(2) -0.003(2) -0.004(2) C66 0.017(2) 0.031(3) 0.021(3) -0.001(2) -0.005(2) -0.006(2) C67 0.022(3) 0.031(4) 0.022(3) -0.003(2) -0.004(2) -0.011(3) C68 0.019(3) 0.024(3) 0.031(3) -0.001(2) -0.002(2) -0.008(2) C69 0.031(3) 0.025(3) 0.037(3) -0.002(3) -0.007(3) -0.007(3) C70 0.053(4) 0.035(4) 0.059(5) -0.011(4) -0.023(4) -0.009(3) C71 0.073(5) 0.036(4) 0.033(4) -0.004(3) -0.003(3) 0.003(4) C72 0.132(9) 0.041(6) 0.103(8) -0.020(5) -0.026(7) -0.042(6) Cu1 0.0321(4) 0.0410(5) 0.0440(5) -0.0081(4) -0.0093(3) -0.0120(4) Cu2 0.0412(5) 0.0355(5) 0.0489(5) -0.0032(4) -0.0273(4) -0.0064(4) Cu3 0.0258(4) 0.0507(5) 0.0250(4) -0.0078(3) -0.0063(3) -0.0135(4) Cu4 0.0295(4) 0.0245(4) 0.0274(4) -0.0041(3) -0.0073(3) -0.0031(3) Cu5 0.0404(4) 0.0259(4) 0.0310(4) -0.0071(3) -0.0143(3) -0.0015(3) Cu6 0.0416(5) 0.0369(5) 0.0387(4) -0.0096(4) -0.0070(3) -0.0153(4) Cu7 0.0214(3) 0.0186(4) 0.0263(3) 0.0003(3) -0.0074(3) -0.0027(3) Cu8 0.0224(3) 0.0215(4) 0.0314(4) 0.0031(3) -0.0109(3) -0.0037(3) Cu9 0.0227(3) 0.0215(4) 0.0276(4) 0.0007(3) -0.0114(3) -0.0048(3) I1 0.02232(18) 0.0359(2) 0.0301(2) -0.00549(17) -0.00114(14) -0.00755(16) I2 0.0280(2) 0.0380(3) 0.0287(2) -0.00009(17) -0.00453(15) -0.00461(18) I3 0.0299(6) 0.0324(4) 0.0325(11) -0.0048(6) -0.0123(6) -0.0017(4) I3' 0.045(5) 0.035(3) 0.038(7) -0.007(4) -0.018(5) 0.007(3) N1 0.028(3) 0.025(3) 0.035(3) -0.001(2) -0.010(2) -0.006(2) N2 0.028(2) 0.024(3) 0.029(3) -0.002(2) -0.008(2) -0.007(2) N3 0.031(3) 0.037(3) 0.031(3) -0.004(2) -0.008(2) -0.010(2) N4 0.022(2) 0.030(3) 0.030(3) -0.004(2) -0.010(2) -0.003(2) N5 0.035(3) 0.018(3) 0.027(2) -0.009(2) -0.011(2) -0.001(2) N6 0.036(3) 0.023(3) 0.028(3) -0.006(2) -0.013(2) 0.002(2) N7 0.078(5) 0.050(5) 0.048(4) -0.021(3) -0.005(3) -0.002(4) N8 0.053(3) 0.024(3) 0.031(3) -0.005(2) -0.016(2) -0.005(3) N9 0.051(3) 0.033(3) 0.048(3) -0.013(3) -0.013(3) -0.016(3) N10 0.023(2) 0.026(3) 0.031(3) -0.004(2) -0.007(2) -0.003(2) N11 0.022(2) 0.023(3) 0.022(2) -0.001(2) -0.0038(18) -0.007(2) N12 0.024(2) 0.018(3) 0.033(3) 0.000(2) -0.0052(19) -0.004(2) N13 0.023(2) 0.033(3) 0.025(2) -0.009(2) -0.0058(19) -0.006(2) N14 0.018(2) 0.023(3) 0.022(2) 0.000(2) -0.0049(17) -0.0050(19) N15 0.022(2) 0.017(3) 0.025(2) -0.0028(19) -0.0078(18) -0.0003(19) N16 0.037(3) 0.030(3) 0.029(3) 0.002(2) -0.014(2) -0.003(2) N17 0.022(2) 0.018(3) 0.027(2) 0.0005(19) -0.0099(18) -0.0039(19) N18 0.018(2) 0.023(3) 0.026(2) -0.002(2) -0.0029(18) -0.006(2) O1W 0.077(5) 0.137(7) 0.070(4) -0.045(4) -0.002(3) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.387(8) . ? C1 C5 1.409(8) . ? C2 N1 1.339(7) . ? C3 N1 1.335(7) . ? C3 C4 1.368(8) . ? C4 C5 1.385(8) . ? C5 C6 1.458(8) . ? C6 N2 1.351(7) . ? C6 C7 1.387(8) . ? C7 C8 1.396(8) . ? C8 N3 1.349(8) . ? C8 C9 1.500(8) . ? C9 C10 1.544(10) . ? C10 C12 1.524(10) . ? C10 C11 1.544(9) . ? C13 C14 1.372(8) . ? C13 C17 1.386(8) . ? C14 N4 1.340(7) . ? C15 N4 1.339(7) . ? C15 C16 1.375(8) . ? C16 C17 1.384(8) . ? C17 C18 1.477(8) . ? C18 N5 1.352(7) . ? C18 C19 1.373(8) . ? C19 C20 1.382(8) . ? C20 N6 1.333(8) . ? C20 C21 1.506(9) . ? C21 C22 1.633(12) . ? C22 C24 1.477(12) . ? C22 C23 1.545(11) . ? C25 C26 1.373(10) . ? C25 C29 1.380(10) . ? C26 N7 1.334(10) . ? C27 N7 1.331(11) . ? C27 C28 1.358(11) . ? C28 C29 1.387(10) . ? C29 C30 1.471(9) . ? C30 C31 1.350(10) . ? C30 N8 1.361(8) . ? C31 C32 1.374(11) . ? C32 N9 1.371(9) . ? C32 C33 1.499(11) . ? C33 C34 1.535(11) . ? C34 C36 1.508(11) . ? C34 C35 1.575(11) . ? C37 C38 1.381(7) . ? C37 C41 1.392(8) . ? C38 N10 1.334(7) . ? C39 N10 1.336(8) . ? C39 C40 1.370(8) . ? C40 C41 1.403(8) . ? C41 C42 1.462(7) . ? C42 N11 1.343(7) . ? C42 C43 1.396(8) . ? C43 C44 1.379(8) . ? C44 N12 1.338(7) . ? C44 C45 1.490(8) . ? C45 C46 1.532(10) . ? C46 C48 1.518(11) . ? C46 C47 1.533(13) . ? C49 C53 1.368(8) . ? C49 C50 1.370(7) . ? C50 N13 1.330(7) . ? C51 N13 1.336(8) . ? C51 C52 1.386(8) . ? C52 C53 1.393(8) . ? C53 C54 1.484(7) . ? C54 N14 1.363(7) . ? C54 C55 1.370(8) . ? C55 C56 1.390(7) . ? C56 N15 1.350(7) . ? C56 C57 1.505(8) . ? C57 C58 1.519(9) . ? C58 C59 1.506(10) . ? C58 C60 1.581(11) . ? C61 C62 1.378(8) . ? C61 C65 1.401(8) . ? C62 N16 1.338(7) . ? C63 N16 1.341(8) . ? C63 C64 1.374(8) . ? C64 C65 1.403(7) . ? C65 C66 1.437(8) . ? C66 N17 1.363(6) . ? C66 C67 1.396(8) . ? C67 C68 1.387(8) . ? C68 N18 1.336(7) . ? C68 C69 1.501(8) . ? C69 C70 1.497(9) . ? C70 C71 1.493(10) . ? C70 C72 1.562(11) . ? Cu1 N1 1.981(5) . ? Cu1 I2 2.5127(8) . ? Cu1 Cu2 2.5619(11) . ? Cu1 I3 2.620(4) . ? Cu1 I3' 2.76(3) . ? Cu2 N10 1.996(5) . ? Cu2 I3' 2.44(2) . ? Cu2 I1 2.5282(10) . ? Cu2 I3 2.590(4) . ? Cu3 N4 2.017(5) . ? Cu3 N13 2.053(5) . ? Cu3 I1 2.6409(8) . ? Cu3 I2 2.6645(9) . ? Cu4 N5 1.853(5) . ? Cu4 N2 1.854(5) . ? Cu5 N8 1.910(5) . ? Cu5 N6 1.911(5) . ? Cu5 N16 2.120(5) 1_656 ? Cu6 N9 1.838(5) . ? Cu6 N3 1.854(5) . ? Cu7 N14 1.857(5) . ? Cu7 N11 1.865(5) . ? Cu8 N18 1.866(4) . ? Cu8 N12 1.871(5) . ? Cu8 Cu9 2.9867(10) 2_565 ? Cu9 N17 1.885(4) . ? Cu9 N15 1.887(4) . ? Cu9 Cu8 2.9867(10) 2_565 ? N2 N3 1.375(7) . ? N5 N6 1.366(6) . ? N8 N9 1.368(8) . ? N11 N12 1.373(6) . ? N14 N15 1.374(6) . ? N16 Cu5 2.120(5) 1_454 ? N17 N18 1.366(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 C2 C1 C5 119.9(5) . . ? N1 C2 C1 122.8(5) . . ? N1 C3 C4 123.6(5) . . ? C3 C4 C5 120.8(5) . . ? C4 C5 C1 115.7(5) . . ? C4 C5 C6 121.8(5) . . ? C1 C5 C6 122.4(5) . . ? N2 C6 C7 109.5(5) . . ? N2 C6 C5 121.2(5) . . ? C7 C6 C5 129.3(5) . . ? C6 C7 C8 105.5(5) . . ? N3 C8 C7 108.8(5) . . ? N3 C8 C9 119.0(6) . . ? C7 C8 C9 132.2(6) . . ? C8 C9 C10 113.2(5) . . ? C12 C10 C9 113.5(6) . . ? C12 C10 C11 110.3(6) . . ? C9 C10 C11 108.9(6) . . ? C14 C13 C17 120.7(6) . . ? N4 C14 C13 123.3(5) . . ? N4 C15 C16 124.5(6) . . ? C15 C16 C17 119.5(5) . . ? C16 C17 C13 116.3(5) . . ? C16 C17 C18 120.5(5) . . ? C13 C17 C18 123.2(5) . . ? N5 C18 C19 108.9(5) . . ? N5 C18 C17 121.2(5) . . ? C19 C18 C17 129.9(6) . . ? C18 C19 C20 105.4(6) . . ? N6 C20 C19 109.9(5) . . ? N6 C20 C21 120.0(5) . . ? C19 C20 C21 129.8(6) . . ? C20 C21 C22 111.6(6) . . ? C24 C22 C23 112.0(8) . . ? C24 C22 C21 111.5(7) . . ? C23 C22 C21 106.5(8) . . ? C26 C25 C29 119.6(7) . . ? N7 C26 C25 124.4(8) . . ? N7 C27 C28 125.9(8) . . ? C27 C28 C29 118.8(8) . . ? C25 C29 C28 116.7(7) . . ? C25 C29 C30 123.9(6) . . ? C28 C29 C30 119.4(7) . . ? C31 C30 N8 109.0(6) . . ? C31 C30 C29 130.2(7) . . ? N8 C30 C29 120.8(6) . . ? C30 C31 C32 108.4(7) . . ? N9 C32 C31 106.7(7) . . ? N9 C32 C33 118.9(6) . . ? C31 C32 C33 134.4(7) . . ? C32 C33 C34 115.9(7) . . ? C36 C34 C33 107.9(7) . . ? C36 C34 C35 108.3(7) . . ? C33 C34 C35 107.4(8) . . ? C38 C37 C41 119.7(5) . . ? N10 C38 C37 123.3(6) . . ? N10 C39 C40 123.1(6) . . ? C39 C40 C41 120.0(6) . . ? C37 C41 C40 116.4(5) . . ? C37 C41 C42 123.5(5) . . ? C40 C41 C42 120.1(5) . . ? N11 C42 C43 110.0(5) . . ? N11 C42 C41 124.8(5) . . ? C43 C42 C41 125.2(5) . . ? C44 C43 C42 104.6(5) . . ? N12 C44 C43 109.6(5) . . ? N12 C44 C45 122.5(5) . . ? C43 C44 C45 127.6(6) . . ? C44 C45 C46 112.0(5) . . ? C48 C46 C45 110.7(7) . . ? C48 C46 C47 112.4(8) . . ? C45 C46 C47 110.2(7) . . ? C53 C49 C50 120.3(5) . . ? N13 C50 C49 123.3(6) . . ? N13 C51 C52 123.2(5) . . ? C51 C52 C53 118.8(6) . . ? C49 C53 C52 117.4(5) . . ? C49 C53 C54 121.5(5) . . ? C52 C53 C54 121.1(5) . . ? N14 C54 C55 110.1(5) . . ? N14 C54 C53 121.4(5) . . ? C55 C54 C53 128.3(5) . . ? C54 C55 C56 105.8(5) . . ? N15 C56 C55 108.5(5) . . ? N15 C56 C57 121.4(5) . . ? C55 C56 C57 130.0(5) . . ? C56 C57 C58 114.7(5) . . ? C59 C58 C57 110.7(6) . . ? C59 C58 C60 105.1(7) . . ? C57 C58 C60 110.5(6) . . ? C62 C61 C65 120.1(5) . . ? N16 C62 C61 123.6(6) . . ? N16 C63 C64 123.9(5) . . ? C63 C64 C65 119.8(5) . . ? C61 C65 C64 116.0(5) . . ? C61 C65 C66 123.2(5) . . ? C64 C65 C66 120.8(5) . . ? N17 C66 C67 109.1(5) . . ? N17 C66 C65 124.8(5) . . ? C67 C66 C65 126.2(5) . . ? C68 C67 C66 105.3(5) . . ? N18 C68 C67 109.1(5) . . ? N18 C68 C69 122.5(5) . . ? C67 C68 C69 128.4(5) . . ? C70 C69 C68 114.0(5) . . ? C71 C70 C69 113.8(6) . . ? C71 C70 C72 109.1(7) . . ? C69 C70 C72 109.4(7) . . ? N1 Cu1 I2 136.38(15) . . ? N1 Cu1 Cu2 125.25(15) . . ? I2 Cu1 Cu2 85.83(3) . . ? N1 Cu1 I3 109.37(16) . . ? I2 Cu1 I3 113.03(6) . . ? Cu2 Cu1 I3 59.95(13) . . ? N1 Cu1 I3' 108.6(5) . . ? I2 Cu1 I3' 114.8(5) . . ? Cu2 Cu1 I3' 54.3(7) . . ? I3 Cu1 I3' 7.0(8) . . ? N10 Cu2 I3' 116.3(5) . . ? N10 Cu2 I1 116.08(15) . . ? I3' Cu2 I1 127.0(6) . . ? N10 Cu2 Cu1 128.80(14) . . ? I3' Cu2 Cu1 67.0(8) . . ? I1 Cu2 Cu1 86.48(3) . . ? N10 Cu2 I3 115.65(16) . . ? I3' Cu2 I3 7.4(10) . . ? I1 Cu2 I3 128.27(7) . . ? Cu1 Cu2 I3 61.14(12) . . ? N4 Cu3 N13 121.84(19) . . ? N4 Cu3 I1 109.77(13) . . ? N13 Cu3 I1 101.82(13) . . ? N4 Cu3 I2 102.69(15) . . ? N13 Cu3 I2 105.18(14) . . ? I1 Cu3 I2 116.26(3) . . ? N5 Cu4 N2 178.6(2) . . ? N8 Cu5 N6 152.1(2) . . ? N8 Cu5 N16 101.0(2) . 1_656 ? N6 Cu5 N16 106.3(2) . 1_656 ? N9 Cu6 N3 177.1(3) . . ? N14 Cu7 N11 177.75(19) . . ? N18 Cu8 N12 173.0(2) . . ? N18 Cu8 Cu9 79.06(13) . 2_565 ? N12 Cu8 Cu9 105.68(14) . 2_565 ? N17 Cu9 N15 178.0(2) . . ? N17 Cu9 Cu8 78.77(14) . 2_565 ? N15 Cu9 Cu8 102.66(13) . 2_565 ? Cu2 I1 Cu3 79.79(3) . . ? Cu1 I2 Cu3 74.37(3) . . ? Cu2 I3 Cu1 58.91(7) . . ? Cu2 I3' Cu1 58.6(4) . . ? C3 N1 C2 117.1(5) . . ? C3 N1 Cu1 120.6(4) . . ? C2 N1 Cu1 121.5(4) . . ? C6 N2 N3 107.7(5) . . ? C6 N2 Cu4 134.1(4) . . ? N3 N2 Cu4 117.4(4) . . ? C8 N3 N2 108.6(5) . . ? C8 N3 Cu6 132.7(4) . . ? N2 N3 Cu6 118.3(4) . . ? C15 N4 C14 115.7(5) . . ? C15 N4 Cu3 120.4(4) . . ? C14 N4 Cu3 123.9(4) . . ? C18 N5 N6 108.1(5) . . ? C18 N5 Cu4 132.9(4) . . ? N6 N5 Cu4 118.5(4) . . ? C20 N6 N5 107.7(5) . . ? C20 N6 Cu5 136.1(4) . . ? N5 N6 Cu5 116.2(4) . . ? C27 N7 C26 114.5(7) . . ? C30 N8 N9 107.1(5) . . ? C30 N8 Cu5 135.9(5) . . ? N9 N8 Cu5 116.8(4) . . ? N8 N9 C32 108.8(5) . . ? N8 N9 Cu6 120.0(4) . . ? C32 N9 Cu6 131.2(5) . . ? C38 N10 C39 117.5(5) . . ? C38 N10 Cu2 122.3(4) . . ? C39 N10 Cu2 119.6(4) . . ? C42 N11 N12 107.0(5) . . ? C42 N11 Cu7 137.2(4) . . ? N12 N11 Cu7 115.8(3) . . ? C44 N12 N11 108.8(4) . . ? C44 N12 Cu8 132.2(4) . . ? N11 N12 Cu8 118.7(4) . . ? C50 N13 C51 117.1(5) . . ? C50 N13 Cu3 121.1(4) . . ? C51 N13 Cu3 121.7(4) . . ? C54 N14 N15 106.5(4) . . ? C54 N14 Cu7 130.4(4) . . ? N15 N14 Cu7 122.5(3) . . ? C56 N15 N14 109.0(4) . . ? C56 N15 Cu9 132.7(4) . . ? N14 N15 Cu9 118.2(4) . . ? C62 N16 C63 116.7(5) . . ? C62 N16 Cu5 122.2(4) . 1_454 ? C63 N16 Cu5 121.1(4) . 1_454 ? C66 N17 N18 107.1(4) . . ? C66 N17 Cu9 134.3(4) . . ? N18 N17 Cu9 116.5(3) . . ? C68 N18 N17 109.5(4) . . ? C68 N18 Cu8 127.9(4) . . ? N17 N18 Cu8 121.8(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.641 _refine_diff_density_min -1.155 _refine_diff_density_rms 0.267 data_2 _database_code_depnum_ccdc_archive 'CCDC 838377' #TrackingRef '- complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H84 Cu9 I3 N18' _chemical_formula_sum 'C72 H84 Cu9 I3 N18' _chemical_formula_weight 2154.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.6484(3) _cell_length_b 14.7423(5) _cell_length_c 21.7997(4) _cell_angle_alpha 90.488(2) _cell_angle_beta 100.351(2) _cell_angle_gamma 117.859(3) _cell_volume 4071.10(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2120 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25 _exptl_crystal_description column _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2124 _exptl_absorpt_coefficient_mu 3.490 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6226 _exptl_absorpt_correction_T_max 0.7216 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35810 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14325 _reflns_number_gt 11113 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+13.4496P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14325 _refine_ls_number_parameters 931 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 0.38110(6) 0.60832(6) 0.67417(4) 0.0387(2) Uani 1 1 d . . . Cu2 Cu 0.42038(6) 0.64243(7) 0.79514(4) 0.0371(2) Uani 1 1 d . . . Cu3 Cu 0.51647(5) 0.52527(6) 0.75022(3) 0.02870(18) Uani 1 1 d . . . Cu4 Cu 0.74533(5) 0.64057(5) 0.48002(3) 0.02310(16) Uani 1 1 d . . . Cu5 Cu 0.87819(6) 0.57717(6) 0.40080(3) 0.02954(18) Uani 1 1 d . . . Cu6 Cu 0.88723(5) 0.79270(6) 0.39654(3) 0.02725(17) Uani 1 1 d . . . Cu7 Cu 0.35703(5) 0.25898(6) 1.01508(3) 0.02237(16) Uani 1 1 d . . . Cu8 Cu 0.18696(5) 0.11358(6) 1.09167(3) 0.02433(16) Uani 1 1 d . . . Cu9 Cu 0.40428(5) 0.11283(6) 1.10811(3) 0.02897(18) Uani 1 1 d . . . I1 I 0.61703(3) 0.71656(3) 0.803363(17) 0.03094(11) Uani 1 1 d . . . I2 I 0.31478(3) 0.41939(3) 0.689919(16) 0.02698(10) Uani 1 1 d . . . I3 I 0.31747(4) 0.71753(4) 0.725372(19) 0.03891(12) Uani 1 1 d . . . N1 N 0.4637(4) 0.6655(4) 0.6075(2) 0.0268(11) Uani 1 1 d . . . N2 N 0.7268(3) 0.7549(4) 0.4631(2) 0.0226(10) Uani 1 1 d . . . N3 N 0.7898(3) 0.8204(4) 0.4259(2) 0.0239(11) Uani 1 1 d . . . N4 N 0.5962(3) 0.5073(4) 0.6867(2) 0.0251(11) Uani 1 1 d . . . N5 N 0.7658(3) 0.5276(4) 0.4982(2) 0.0224(10) Uani 1 1 d . . . N6 N 0.8119(3) 0.4943(4) 0.4602(2) 0.0254(11) Uani 1 1 d . . . N7 N 1.1802(5) 1.1621(5) 0.3568(3) 0.0555(17) Uani 1 1 d . . . N8 N 0.9932(3) 0.7752(4) 0.3711(2) 0.0267(11) Uani 1 1 d . . . N9 N 0.9812(4) 0.6782(4) 0.3636(2) 0.0290(12) Uani 1 1 d . . . N10 N 0.3544(4) 0.5517(4) 0.8589(2) 0.0273(11) Uani 1 1 d . . . N11 N 0.2389(3) 0.2760(4) 1.0139(2) 0.0222(11) Uani 1 1 d . . . N12 N 0.1645(3) 0.2107(4) 1.0461(2) 0.0243(11) Uani 1 1 d . . . N13 N 0.5305(3) 0.4403(4) 0.8227(2) 0.0259(11) Uani 1 1 d . . . N14 N 0.4771(3) 0.2447(4) 1.0168(2) 0.0238(11) Uani 1 1 d . . . N15 N 0.5069(3) 0.1988(4) 1.0648(2) 0.0249(11) Uani 1 1 d . . . N16 N -0.1910(4) -0.1651(5) 1.1490(3) 0.0421(14) Uani 1 1 d . . . N17 N 0.1967(3) 0.0024(4) 1.1266(2) 0.0253(11) Uani 1 1 d . . . N18 N 0.2915(4) 0.0023(4) 1.1333(2) 0.0299(12) Uani 1 1 d . . . C1 C 0.5507(4) 0.6442(5) 0.5306(2) 0.0228(13) Uani 1 1 d . . . H1 H 0.5651 0.5990 0.5076 0.027 Uiso 1 1 calc R . . C2 C 0.4877(4) 0.6068(4) 0.5734(2) 0.0217(12) Uani 1 1 d . . . H2 H 0.4595 0.5357 0.5792 0.026 Uiso 1 1 calc R . . C3 C 0.5034(5) 0.7646(5) 0.5970(3) 0.0385(16) Uani 1 1 d . . . H3 H 0.4862 0.8074 0.6200 0.046 Uiso 1 1 calc R . . C4 C 0.5667(5) 0.8080(5) 0.5555(3) 0.0359(15) Uani 1 1 d . . . H4 H 0.5926 0.8792 0.5503 0.043 Uiso 1 1 calc R . . C5 C 0.5938(4) 0.7475(5) 0.5204(2) 0.0246(13) Uani 1 1 d . . . C6 C 0.6664(4) 0.7948(4) 0.4778(2) 0.0235(13) Uani 1 1 d . . . C7 C 0.6895(5) 0.8839(5) 0.4493(3) 0.0299(14) Uani 1 1 d . . . H7 H 0.6578 0.9270 0.4513 0.036 Uiso 1 1 calc R . . C8 C 0.7676(4) 0.8981(5) 0.4174(3) 0.0257(13) Uani 1 1 d . . . C9 C 0.8243(5) 0.9828(5) 0.3788(3) 0.0318(14) Uani 1 1 d . . . H9A H 0.8995 1.0217 0.4000 0.038 Uiso 1 1 calc R . . H9B H 0.7946 1.0311 0.3776 0.038 Uiso 1 1 calc R . . C10 C 0.8181(5) 0.9469(5) 0.3110(3) 0.0336(15) Uani 1 1 d . . . H10 H 0.8527 0.9022 0.3122 0.040 Uiso 1 1 calc R . . C11 C 0.7044(5) 0.8846(6) 0.2765(3) 0.0466(18) Uani 1 1 d . . . H11A H 0.6697 0.8211 0.2962 0.070 Uiso 1 1 calc R . . H11B H 0.7024 0.8672 0.2326 0.070 Uiso 1 1 calc R . . H11C H 0.6676 0.9253 0.2783 0.070 Uiso 1 1 calc R . . C12 C 0.8783(5) 1.0411(6) 0.2775(3) 0.0441(18) Uani 1 1 d . . . H12A H 0.8756 1.0183 0.2346 0.066 Uiso 1 1 calc R . . H12B H 0.9520 1.0789 0.3001 0.066 Uiso 1 1 calc R . . H12C H 0.8459 1.0862 0.2765 0.066 Uiso 1 1 calc R . . C13 C 0.7227(4) 0.5732(5) 0.6207(2) 0.0244(13) Uani 1 1 d . . . H13 H 0.7790 0.6315 0.6090 0.029 Uiso 1 1 calc R . . C14 C 0.6757(4) 0.5861(5) 0.6676(2) 0.0231(13) Uani 1 1 d . . . H14 H 0.7010 0.6538 0.6870 0.028 Uiso 1 1 calc R . . C15 C 0.5649(4) 0.4121(5) 0.6592(3) 0.0262(13) Uani 1 1 d . . . H15 H 0.5103 0.3547 0.6729 0.031 Uiso 1 1 calc R . . C16 C 0.6077(4) 0.3939(5) 0.6126(2) 0.0251(13) Uani 1 1 d . . . H16 H 0.5827 0.3253 0.5949 0.030 Uiso 1 1 calc R . . C17 C 0.6885(4) 0.4766(5) 0.5911(2) 0.0219(13) Uani 1 1 d . . . C18 C 0.7345(4) 0.4594(5) 0.5409(2) 0.0225(13) Uani 1 1 d . . . C19 C 0.7598(5) 0.3816(5) 0.5299(3) 0.0316(14) Uani 1 1 d . . . H19 H 0.7458 0.3230 0.5522 0.038 Uiso 1 1 calc R . . C20 C 0.8098(4) 0.4078(5) 0.4796(3) 0.0263(13) Uani 1 1 d . . . C21 C 0.8666(5) 0.3618(5) 0.4508(3) 0.0380(16) Uani 1 1 d . . . H21A H 0.9414 0.4151 0.4557 0.046 Uiso 1 1 calc R . . H21B H 0.8360 0.3449 0.4052 0.046 Uiso 1 1 calc R . . C22 C 0.8637(5) 0.2659(5) 0.4771(3) 0.0356(16) Uani 1 1 d . . . H22 H 0.8834 0.2798 0.5238 0.043 Uiso 1 1 calc R . . C23 C 0.7532(6) 0.1736(6) 0.4595(4) 0.055(2) Uani 1 1 d . . . H23A H 0.7345 0.1544 0.4141 0.083 Uiso 1 1 calc R . . H23B H 0.7023 0.1918 0.4720 0.083 Uiso 1 1 calc R . . H23C H 0.7518 0.1152 0.4813 0.083 Uiso 1 1 calc R . . C24 C 0.9445(5) 0.2431(6) 0.4554(3) 0.0473(19) Uani 1 1 d . . . H24A H 0.9459 0.1844 0.4754 0.071 Uiso 1 1 calc R . . H24B H 1.0144 0.3037 0.4669 0.071 Uiso 1 1 calc R . . H24C H 0.9253 0.2264 0.4097 0.071 Uiso 1 1 calc R . . C25 C 1.1002(5) 1.0024(5) 0.4002(3) 0.0442(18) Uani 1 1 d . . . H25 H 1.0656 0.9670 0.4321 0.053 Uiso 1 1 calc R . . C26 C 1.1313(5) 1.1077(6) 0.3982(3) 0.051(2) Uani 1 1 d . . . H26 H 1.1155 1.1411 0.4289 0.062 Uiso 1 1 calc R . . C27 C 1.2028(6) 1.1113(6) 0.3144(4) 0.057(2) Uani 1 1 d . . . H27 H 1.2418 1.1504 0.2849 0.068 Uiso 1 1 calc R . . C28 C 1.1740(5) 1.0098(6) 0.3109(3) 0.0506(19) Uani 1 1 d . . . H28 H 1.1895 0.9782 0.2790 0.061 Uiso 1 1 calc R . . C29 C 1.1194(5) 0.9512(6) 0.3568(3) 0.0388(17) Uani 1 1 d . . . C30 C 1.0848(4) 0.8414(5) 0.3551(3) 0.0311(15) Uani 1 1 d . . . C31 C 1.1314(5) 0.7854(5) 0.3369(3) 0.0337(16) Uani 1 1 d . . . H31 H 1.1958 0.8117 0.3227 0.040 Uiso 1 1 calc R . . C32 C 1.0651(5) 0.6835(5) 0.3436(3) 0.0320(15) Uani 1 1 d . . . C33 C 1.0744(5) 0.5865(6) 0.3343(3) 0.0434(17) Uani 1 1 d . . . H33A H 1.1459 0.6067 0.3270 0.052 Uiso 1 1 calc R . . H33B H 1.0682 0.5532 0.3737 0.052 Uiso 1 1 calc R . . C34 C 0.9962(5) 0.5088(6) 0.2822(3) 0.0437(17) Uani 1 1 d . . . H34 H 0.9237 0.4946 0.2856 0.052 Uiso 1 1 calc R . . C35 C 1.0024(7) 0.4082(6) 0.2842(4) 0.059(2) Uani 1 1 d . . . H35A H 1.0691 0.4193 0.2740 0.088 Uiso 1 1 calc R . . H35B H 0.9433 0.3550 0.2535 0.088 Uiso 1 1 calc R . . H35C H 0.9986 0.3857 0.3262 0.088 Uiso 1 1 calc R . . C36 C 1.0191(6) 0.5526(6) 0.2193(3) 0.053(2) Uani 1 1 d . . . H36A H 1.0078 0.6130 0.2159 0.080 Uiso 1 1 calc R . . H36B H 0.9717 0.4998 0.1845 0.080 Uiso 1 1 calc R . . H36C H 1.0925 0.5729 0.2176 0.080 Uiso 1 1 calc R . . C37 C 0.3633(4) 0.4562(5) 0.9458(2) 0.0252(13) Uani 1 1 d . . . H37 H 0.4059 0.4412 0.9778 0.030 Uiso 1 1 calc R . . C38 C 0.4088(4) 0.5257(5) 0.9051(2) 0.0259(13) Uani 1 1 d . . . H38 H 0.4833 0.5575 0.9098 0.031 Uiso 1 1 calc R . . C39 C 0.2500(4) 0.5065(5) 0.8544(3) 0.0304(14) Uani 1 1 d . . . H39 H 0.2096 0.5246 0.8228 0.037 Uiso 1 1 calc R . . C40 C 0.1980(4) 0.4357(5) 0.8929(3) 0.0299(14) Uani 1 1 d . . . H40 H 0.1235 0.4058 0.8872 0.036 Uiso 1 1 calc R . . C41 C 0.2539(4) 0.4075(5) 0.9401(2) 0.0234(13) Uani 1 1 d . . . C42 C 0.1986(4) 0.3312(5) 0.9814(2) 0.0223(13) Uani 1 1 d . . . C43 C 0.0993(4) 0.3030(5) 0.9929(3) 0.0266(13) Uani 1 1 d . . . H43 H 0.0537 0.3303 0.9765 0.032 Uiso 1 1 calc R . . C44 C 0.0800(4) 0.2276(5) 1.0330(3) 0.0272(14) Uani 1 1 d . . . C45 C -0.0157(5) 0.1687(5) 1.0606(3) 0.0374(16) Uani 1 1 d . . . H45A H -0.0211 0.1008 1.0695 0.045 Uiso 1 1 calc R . . H45B H -0.0792 0.1558 1.0288 0.045 Uiso 1 1 calc R . . C46 C -0.0164(6) 0.2219(6) 1.1203(3) 0.049(2) Uani 1 1 d . . . H46 H -0.0847 0.1764 1.1329 0.059 Uiso 1 1 calc R . . C47 C -0.0139(8) 0.3241(7) 1.1097(4) 0.073(3) Uani 1 1 d . . . H47A H -0.0269 0.3504 1.1469 0.109 Uiso 1 1 calc R . . H47B H -0.0687 0.3147 1.0732 0.109 Uiso 1 1 calc R . . H47C H 0.0555 0.3736 1.1022 0.109 Uiso 1 1 calc R . . C48 C 0.0717(6) 0.2317(7) 1.1737(3) 0.057(2) Uani 1 1 d . . . H48A H 0.0699 0.1646 1.1767 0.085 Uiso 1 1 calc R . . H48B H 0.0617 0.2543 1.2132 0.085 Uiso 1 1 calc R . . H48C H 0.1400 0.2824 1.1655 0.085 Uiso 1 1 calc R . . C49 C 0.4537(4) 0.3059(5) 0.8877(2) 0.0240(13) Uani 1 1 d . . . H49 H 0.3925 0.2470 0.8946 0.029 Uiso 1 1 calc R . . C50 C 0.4477(4) 0.3571(5) 0.8357(3) 0.0272(14) Uani 1 1 d . . . H50 H 0.3813 0.3321 0.8077 0.033 Uiso 1 1 calc R . . C51 C 0.6236(4) 0.4731(5) 0.8626(3) 0.0309(15) Uani 1 1 d . . . H51 H 0.6836 0.5317 0.8543 0.037 Uiso 1 1 calc R . . C52 C 0.6357(4) 0.4249(5) 0.9155(3) 0.0281(14) Uani 1 1 d . . . H52 H 0.7034 0.4498 0.9420 0.034 Uiso 1 1 calc R . . C53 C 0.5491(4) 0.3403(5) 0.9297(2) 0.0231(13) Uani 1 1 d . . . C54 C 0.5580(4) 0.2890(5) 0.9858(3) 0.0240(13) Uani 1 1 d . . . C55 C 0.6399(4) 0.2716(5) 1.0154(2) 0.0252(13) Uani 1 1 d . . . H55 H 0.7069 0.2951 1.0047 0.030 Uiso 1 1 calc R . . C56 C 0.6044(4) 0.2134(5) 1.0634(3) 0.0257(13) Uani 1 1 d . . . C57 C 0.6528(5) 0.1627(5) 1.1072(3) 0.0313(15) Uani 1 1 d . . . H57A H 0.6282 0.1585 1.1471 0.038 Uiso 1 1 calc R . . H57B H 0.7304 0.2067 1.1167 0.038 Uiso 1 1 calc R . . C58 C 0.6271(5) 0.0554(5) 1.0822(3) 0.0346(15) Uani 1 1 d . . . H58 H 0.5486 0.0144 1.0686 0.042 Uiso 1 1 calc R . . C59 C 0.6740(5) 0.0566(6) 1.0254(3) 0.0436(18) Uani 1 1 d . . . H59A H 0.6444 0.0846 0.9915 0.065 Uiso 1 1 calc R . . H59B H 0.6569 -0.0139 1.0114 0.065 Uiso 1 1 calc R . . H59C H 0.7508 0.0999 1.0366 0.065 Uiso 1 1 calc R . . C60 C 0.6619(6) 0.0020(6) 1.1338(3) 0.0495(19) Uani 1 1 d . . . H60A H 0.6391 -0.0693 1.1178 0.074 Uiso 1 1 calc R . . H60B H 0.6299 0.0019 1.1697 0.074 Uiso 1 1 calc R . . H60C H 0.7390 0.0390 1.1471 0.074 Uiso 1 1 calc R . . C61 C -0.0393(5) -0.0817(5) 1.1024(3) 0.0308(14) Uani 1 1 d . . . H61 H -0.0092 -0.0423 1.0703 0.037 Uiso 1 1 calc R . . C62 C -0.1417(5) -0.1076(5) 1.1072(3) 0.0360(16) Uani 1 1 d . . . H62 H -0.1790 -0.0821 1.0785 0.043 Uiso 1 1 calc R . . C63 C -0.1356(5) -0.1987(6) 1.1891(3) 0.0434(18) Uani 1 1 d . . . H63 H -0.1697 -0.2416 1.2189 0.052 Uiso 1 1 calc R . . C64 C -0.0318(5) -0.1751(5) 1.1900(3) 0.0355(16) Uani 1 1 d . . . H64 H 0.0043 -0.1997 1.2202 0.043 Uiso 1 1 calc R . . C65 C 0.0178(4) -0.1143(5) 1.1450(3) 0.0293(14) Uani 1 1 d . . . C66 C 0.1283(4) -0.0885(5) 1.1445(2) 0.0252(13) Uani 1 1 d . . . C67 C 0.1775(5) -0.1473(5) 1.1609(3) 0.0400(16) Uani 1 1 d . . . H67 H 0.1477 -0.2139 1.1750 0.048 Uiso 1 1 calc R . . C68 C 0.2802(5) -0.0882(6) 1.1522(3) 0.0397(16) Uani 1 1 d . . . C69 C 0.3702(6) -0.1122(7) 1.1600(4) 0.061(2) Uani 1 1 d . . . H69A H 0.4316 -0.0527 1.1489 0.074 Uiso 1 1 calc R . . H69B H 0.3499 -0.1723 1.1297 0.074 Uiso 1 1 calc R . . C70 C 0.4041(10) -0.1357(9) 1.2250(5) 0.097(4) Uani 1 1 d . . . H70 H 0.4752 -0.1252 1.2209 0.117 Uiso 1 1 calc R . . C71 C 0.4400(8) -0.0464(9) 1.2728(5) 0.094(3) Uani 1 1 d . . . H71A H 0.3789 -0.0397 1.2795 0.140 Uiso 1 1 calc R . . H71B H 0.4895 0.0170 1.2579 0.140 Uiso 1 1 calc R . . H71C H 0.4752 -0.0577 1.3123 0.140 Uiso 1 1 calc R . . C72 C 0.3671(18) -0.2270(12) 1.2393(6) 0.237(12) Uani 1 1 d . . . H72A H 0.4234 -0.2463 1.2474 0.356 Uiso 1 1 calc R . . H72B H 0.3111 -0.2738 1.2046 0.356 Uiso 1 1 calc R . . H72C H 0.3380 -0.2319 1.2770 0.356 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0558(5) 0.0288(5) 0.0365(4) 0.0122(4) 0.0276(4) 0.0179(4) Cu2 0.0351(4) 0.0432(5) 0.0325(4) 0.0197(4) 0.0139(3) 0.0155(4) Cu3 0.0324(4) 0.0264(4) 0.0161(4) 0.0043(3) 0.0075(3) 0.0040(3) Cu4 0.0266(4) 0.0193(4) 0.0232(4) 0.0065(3) 0.0075(3) 0.0100(3) Cu5 0.0339(4) 0.0262(5) 0.0276(4) 0.0054(3) 0.0134(3) 0.0111(3) Cu6 0.0299(4) 0.0263(4) 0.0257(4) 0.0089(3) 0.0117(3) 0.0114(3) Cu7 0.0201(3) 0.0254(4) 0.0225(4) 0.0084(3) 0.0080(3) 0.0104(3) Cu8 0.0275(4) 0.0241(4) 0.0227(4) 0.0079(3) 0.0115(3) 0.0111(3) Cu9 0.0309(4) 0.0352(5) 0.0264(4) 0.0157(3) 0.0140(3) 0.0173(4) I1 0.0294(2) 0.0263(2) 0.0248(2) -0.00176(17) 0.00804(16) 0.00242(17) I2 0.0274(2) 0.0234(2) 0.02078(19) 0.00426(16) 0.00208(15) 0.00544(17) I3 0.0566(3) 0.0424(3) 0.0260(2) 0.00598(19) 0.00946(19) 0.0300(2) N1 0.033(3) 0.023(3) 0.025(3) 0.009(2) 0.010(2) 0.013(2) N2 0.028(2) 0.020(3) 0.019(2) 0.004(2) 0.007(2) 0.010(2) N3 0.032(3) 0.019(3) 0.020(2) 0.007(2) 0.010(2) 0.010(2) N4 0.025(2) 0.027(3) 0.019(2) 0.008(2) 0.0050(19) 0.009(2) N5 0.027(2) 0.021(3) 0.019(2) 0.004(2) 0.0055(19) 0.010(2) N6 0.026(2) 0.026(3) 0.022(3) 0.000(2) 0.005(2) 0.011(2) N7 0.068(4) 0.035(4) 0.043(4) -0.002(3) 0.012(3) 0.009(3) N8 0.028(3) 0.029(3) 0.021(3) 0.009(2) 0.007(2) 0.011(2) N9 0.026(3) 0.036(3) 0.023(3) 0.004(2) 0.007(2) 0.013(2) N10 0.031(3) 0.026(3) 0.024(3) 0.008(2) 0.010(2) 0.011(2) N11 0.019(2) 0.027(3) 0.018(2) 0.008(2) 0.0092(19) 0.006(2) N12 0.027(3) 0.021(3) 0.024(3) 0.007(2) 0.011(2) 0.010(2) N13 0.027(3) 0.026(3) 0.019(2) 0.004(2) 0.007(2) 0.007(2) N14 0.024(2) 0.029(3) 0.020(2) 0.009(2) 0.0070(19) 0.014(2) N15 0.028(3) 0.032(3) 0.019(2) 0.008(2) 0.006(2) 0.017(2) N16 0.032(3) 0.039(4) 0.035(3) -0.002(3) 0.006(2) 0.000(3) N17 0.029(3) 0.025(3) 0.022(2) 0.007(2) 0.011(2) 0.010(2) N18 0.033(3) 0.031(3) 0.030(3) 0.016(2) 0.016(2) 0.016(2) C1 0.025(3) 0.022(3) 0.016(3) 0.001(2) 0.001(2) 0.009(3) C2 0.027(3) 0.015(3) 0.018(3) 0.001(2) 0.001(2) 0.007(3) C3 0.061(4) 0.028(4) 0.037(4) 0.007(3) 0.029(3) 0.024(4) C4 0.054(4) 0.027(4) 0.036(4) 0.013(3) 0.021(3) 0.022(3) C5 0.029(3) 0.025(4) 0.020(3) 0.006(3) 0.003(2) 0.013(3) C6 0.028(3) 0.016(3) 0.021(3) 0.001(2) 0.007(2) 0.006(3) C7 0.043(4) 0.021(4) 0.029(3) 0.008(3) 0.013(3) 0.016(3) C8 0.033(3) 0.015(3) 0.024(3) 0.004(3) 0.006(2) 0.006(3) C9 0.040(3) 0.022(4) 0.031(3) 0.010(3) 0.015(3) 0.011(3) C10 0.046(4) 0.023(4) 0.026(3) 0.010(3) 0.012(3) 0.010(3) C11 0.055(4) 0.034(5) 0.037(4) 0.011(3) 0.009(3) 0.011(4) C12 0.053(4) 0.039(5) 0.030(4) 0.011(3) 0.013(3) 0.011(4) C13 0.025(3) 0.022(4) 0.020(3) 0.005(3) 0.003(2) 0.007(3) C14 0.024(3) 0.023(3) 0.015(3) 0.002(2) 0.001(2) 0.007(3) C15 0.032(3) 0.020(4) 0.021(3) 0.011(3) 0.006(2) 0.007(3) C16 0.033(3) 0.016(3) 0.023(3) 0.006(2) 0.002(2) 0.010(3) C17 0.024(3) 0.027(4) 0.015(3) 0.006(3) 0.000(2) 0.013(3) C18 0.026(3) 0.021(3) 0.016(3) 0.003(2) 0.001(2) 0.009(3) C19 0.043(4) 0.027(4) 0.031(3) 0.011(3) 0.009(3) 0.020(3) C20 0.033(3) 0.020(3) 0.025(3) 0.003(3) 0.007(3) 0.012(3) C21 0.050(4) 0.038(4) 0.040(4) 0.010(3) 0.014(3) 0.031(4) C22 0.047(4) 0.043(4) 0.025(3) -0.007(3) -0.003(3) 0.032(4) C23 0.064(5) 0.040(5) 0.068(5) 0.002(4) 0.027(4) 0.025(4) C24 0.056(4) 0.047(5) 0.047(4) -0.010(4) -0.003(3) 0.036(4) C25 0.044(4) 0.030(4) 0.033(4) 0.001(3) 0.007(3) -0.003(3) C26 0.041(4) 0.040(5) 0.047(4) -0.010(4) 0.005(3) 0.000(4) C27 0.053(5) 0.041(5) 0.052(5) 0.022(4) 0.015(4) 0.001(4) C28 0.048(4) 0.043(5) 0.045(4) -0.001(4) 0.006(3) 0.009(4) C29 0.030(3) 0.036(4) 0.037(4) 0.009(3) 0.013(3) 0.002(3) C30 0.022(3) 0.038(4) 0.025(3) 0.014(3) 0.003(2) 0.007(3) C31 0.027(3) 0.050(5) 0.021(3) 0.013(3) 0.011(3) 0.014(3) C32 0.031(3) 0.043(4) 0.020(3) 0.001(3) 0.005(3) 0.016(3) C33 0.040(4) 0.039(5) 0.052(4) 0.006(4) 0.018(3) 0.017(3) C34 0.048(4) 0.040(5) 0.042(4) 0.010(3) 0.003(3) 0.022(4) C35 0.079(6) 0.052(6) 0.048(5) 0.011(4) 0.019(4) 0.031(5) C36 0.059(5) 0.052(5) 0.050(5) 0.008(4) 0.008(4) 0.028(4) C37 0.028(3) 0.027(4) 0.021(3) 0.007(3) 0.004(2) 0.014(3) C38 0.023(3) 0.025(4) 0.020(3) -0.003(3) 0.002(2) 0.004(3) C39 0.029(3) 0.035(4) 0.025(3) 0.014(3) 0.004(3) 0.014(3) C40 0.024(3) 0.033(4) 0.028(3) 0.011(3) 0.006(2) 0.009(3) C41 0.026(3) 0.022(3) 0.020(3) 0.003(3) 0.006(2) 0.009(3) C42 0.026(3) 0.022(3) 0.017(3) 0.000(2) 0.005(2) 0.009(3) C43 0.026(3) 0.027(4) 0.031(3) 0.008(3) 0.011(3) 0.015(3) C44 0.025(3) 0.030(4) 0.028(3) 0.008(3) 0.012(2) 0.012(3) C45 0.033(3) 0.038(4) 0.049(4) 0.016(3) 0.026(3) 0.017(3) C46 0.061(5) 0.064(6) 0.047(4) 0.025(4) 0.031(4) 0.042(4) C47 0.119(8) 0.074(7) 0.065(6) 0.020(5) 0.051(5) 0.068(6) C48 0.061(5) 0.076(7) 0.040(4) 0.006(4) 0.027(4) 0.033(5) C49 0.023(3) 0.023(3) 0.023(3) 0.008(3) 0.008(2) 0.007(3) C50 0.026(3) 0.025(4) 0.022(3) 0.001(3) 0.003(2) 0.006(3) C51 0.027(3) 0.034(4) 0.027(3) 0.008(3) 0.012(3) 0.008(3) C52 0.024(3) 0.037(4) 0.023(3) 0.006(3) 0.005(2) 0.013(3) C53 0.019(3) 0.027(4) 0.025(3) 0.005(3) 0.010(2) 0.011(3) C54 0.022(3) 0.022(3) 0.024(3) 0.001(3) 0.010(2) 0.006(3) C55 0.022(3) 0.038(4) 0.020(3) 0.003(3) 0.007(2) 0.017(3) C56 0.027(3) 0.034(4) 0.022(3) 0.002(3) 0.005(2) 0.019(3) C57 0.037(3) 0.046(4) 0.021(3) 0.005(3) 0.007(3) 0.027(3) C58 0.028(3) 0.039(4) 0.042(4) 0.012(3) 0.005(3) 0.021(3) C59 0.047(4) 0.056(5) 0.038(4) -0.005(4) 0.001(3) 0.036(4) C60 0.050(4) 0.052(5) 0.059(5) 0.018(4) 0.013(4) 0.033(4) C61 0.034(3) 0.026(4) 0.023(3) 0.001(3) 0.002(3) 0.008(3) C62 0.034(3) 0.027(4) 0.031(4) -0.002(3) 0.001(3) 0.003(3) C63 0.044(4) 0.037(5) 0.027(4) -0.002(3) 0.014(3) -0.001(3) C64 0.035(4) 0.030(4) 0.024(3) 0.005(3) 0.009(3) 0.001(3) C65 0.032(3) 0.016(3) 0.023(3) -0.006(3) 0.005(3) -0.001(3) C66 0.034(3) 0.019(3) 0.019(3) 0.006(2) 0.009(2) 0.008(3) C67 0.052(4) 0.025(4) 0.038(4) 0.013(3) 0.010(3) 0.014(3) C68 0.049(4) 0.035(4) 0.036(4) 0.016(3) 0.013(3) 0.020(4) C69 0.068(5) 0.058(6) 0.079(6) 0.037(5) 0.022(4) 0.044(5) C70 0.148(10) 0.087(9) 0.075(7) 0.012(7) -0.016(7) 0.085(8) C71 0.082(7) 0.106(10) 0.079(7) 0.005(7) -0.015(5) 0.044(7) C72 0.47(3) 0.085(12) 0.082(9) 0.036(9) -0.024(14) 0.101(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.996(5) . ? Cu1 I2 2.5350(9) . ? Cu1 I3 2.5402(9) . ? Cu1 Cu2 2.5885(11) . ? Cu1 Cu3 3.0500(11) . ? Cu2 N10 1.991(5) . ? Cu2 I1 2.5286(8) . ? Cu2 I3 2.5643(9) . ? Cu2 Cu3 2.9433(11) . ? Cu3 N4 2.054(4) . ? Cu3 N13 2.065(5) . ? Cu3 I1 2.6294(9) . ? Cu3 I2 2.6745(8) . ? Cu4 N2 1.858(5) . ? Cu4 N5 1.859(5) . ? Cu5 N6 1.867(5) . ? Cu5 N9 1.874(5) . ? Cu6 N8 1.862(5) . ? Cu6 N3 1.866(4) . ? Cu7 N11 1.857(4) . ? Cu7 N14 1.861(4) . ? Cu8 N17 1.868(5) . ? Cu8 N12 1.868(5) . ? Cu9 N15 1.873(5) . ? Cu9 N18 1.874(5) . ? N1 C3 1.336(8) . ? N1 C2 1.338(7) . ? N2 C6 1.347(7) . ? N2 N3 1.377(6) . ? N3 C8 1.335(7) . ? N4 C14 1.340(7) . ? N4 C15 1.350(7) . ? N5 C18 1.351(7) . ? N5 N6 1.374(6) . ? N6 C20 1.335(8) . ? N7 C26 1.296(9) . ? N7 C27 1.361(10) . ? N8 C30 1.351(7) . ? N8 N9 1.361(7) . ? N9 C32 1.345(7) . ? N10 C39 1.336(7) . ? N10 C38 1.340(7) . ? N11 C42 1.349(7) . ? N11 N12 1.383(6) . ? N12 C44 1.355(7) . ? N13 C50 1.339(7) . ? N13 C51 1.342(7) . ? N14 C54 1.364(7) . ? N14 N15 1.365(6) . ? N15 C56 1.348(7) . ? N16 C62 1.323(8) . ? N16 C63 1.339(9) . ? N17 C66 1.358(7) . ? N17 N18 1.370(6) . ? N18 C68 1.343(8) . ? C1 C2 1.367(7) . ? C1 C5 1.387(8) . ? C3 C4 1.359(8) . ? C4 C5 1.403(8) . ? C5 C6 1.467(8) . ? C6 C7 1.379(8) . ? C7 C8 1.380(8) . ? C8 C9 1.502(8) . ? C9 C10 1.537(8) . ? C10 C11 1.514(9) . ? C10 C12 1.530(9) . ? C13 C17 1.376(8) . ? C13 C14 1.389(7) . ? C15 C16 1.371(8) . ? C16 C17 1.402(8) . ? C17 C18 1.463(7) . ? C18 C19 1.390(8) . ? C19 C20 1.386(8) . ? C20 C21 1.502(8) . ? C21 C22 1.516(9) . ? C22 C24 1.520(8) . ? C22 C23 1.526(10) . ? C25 C29 1.350(9) . ? C25 C26 1.402(10) . ? C27 C28 1.349(11) . ? C28 C29 1.429(10) . ? C29 C30 1.450(9) . ? C30 C31 1.387(9) . ? C31 C32 1.382(9) . ? C32 C33 1.515(9) . ? C33 C34 1.482(9) . ? C34 C35 1.528(10) . ? C34 C36 1.545(10) . ? C37 C38 1.369(8) . ? C37 C41 1.396(7) . ? C39 C40 1.369(8) . ? C40 C41 1.388(8) . ? C41 C42 1.469(8) . ? C42 C43 1.386(7) . ? C43 C44 1.375(8) . ? C44 C45 1.502(8) . ? C45 C46 1.519(9) . ? C46 C47 1.511(11) . ? C46 C48 1.523(10) . ? C49 C50 1.380(8) . ? C49 C53 1.385(7) . ? C51 C52 1.386(8) . ? C52 C53 1.390(8) . ? C53 C54 1.461(8) . ? C54 C55 1.391(8) . ? C55 C56 1.376(8) . ? C56 C57 1.495(8) . ? C57 C58 1.515(9) . ? C58 C59 1.516(9) . ? C58 C60 1.526(9) . ? C61 C65 1.378(8) . ? C61 C62 1.389(8) . ? C63 C64 1.388(9) . ? C64 C65 1.398(8) . ? C65 C66 1.482(8) . ? C66 C67 1.376(9) . ? C67 C68 1.393(9) . ? C68 C69 1.500(9) . ? C69 C70 1.514(12) . ? C70 C72 1.261(17) . ? C70 C71 1.493(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 I2 118.68(15) . . ? N1 Cu1 I3 118.39(15) . . ? I2 Cu1 I3 121.91(3) . . ? N1 Cu1 Cu2 135.07(14) . . ? I2 Cu1 Cu2 86.43(3) . . ? I3 Cu1 Cu2 59.99(3) . . ? N1 Cu1 Cu3 99.43(14) . . ? I2 Cu1 Cu3 56.32(2) . . ? I3 Cu1 Cu3 122.17(3) . . ? Cu2 Cu1 Cu3 62.30(3) . . ? N10 Cu2 I1 118.48(14) . . ? N10 Cu2 I3 119.33(14) . . ? I1 Cu2 I3 120.36(3) . . ? N10 Cu2 Cu1 130.73(15) . . ? I1 Cu2 Cu1 92.63(3) . . ? I3 Cu2 Cu1 59.07(3) . . ? N10 Cu2 Cu3 98.05(14) . . ? I1 Cu2 Cu3 56.83(2) . . ? I3 Cu2 Cu3 125.51(3) . . ? Cu1 Cu2 Cu3 66.56(3) . . ? N4 Cu3 N13 106.42(18) . . ? N4 Cu3 I1 109.80(14) . . ? N13 Cu3 I1 103.80(14) . . ? N4 Cu3 I2 102.75(13) . . ? N13 Cu3 I2 104.82(13) . . ? I1 Cu3 I2 127.68(3) . . ? N4 Cu3 Cu2 147.70(14) . . ? N13 Cu3 Cu2 104.72(13) . . ? I1 Cu3 Cu2 53.61(2) . . ? I2 Cu3 Cu2 77.13(3) . . ? N4 Cu3 Cu1 102.86(13) . . ? N13 Cu3 Cu1 146.43(13) . . ? I1 Cu3 Cu1 80.95(3) . . ? I2 Cu3 Cu1 52.07(2) . . ? Cu2 Cu3 Cu1 51.14(2) . . ? N2 Cu4 N5 178.9(2) . . ? N6 Cu5 N9 161.4(2) . . ? N8 Cu6 N3 175.3(2) . . ? N11 Cu7 N14 178.9(2) . . ? N17 Cu8 N12 171.4(2) . . ? N15 Cu9 N18 165.1(2) . . ? Cu2 I1 Cu3 69.56(3) . . ? Cu1 I2 Cu3 71.61(3) . . ? Cu1 I3 Cu2 60.94(3) . . ? C3 N1 C2 116.4(5) . . ? C3 N1 Cu1 122.5(4) . . ? C2 N1 Cu1 121.0(4) . . ? C6 N2 N3 107.0(5) . . ? C6 N2 Cu4 137.3(4) . . ? N3 N2 Cu4 115.7(3) . . ? C8 N3 N2 109.1(4) . . ? C8 N3 Cu6 130.7(4) . . ? N2 N3 Cu6 120.2(4) . . ? C14 N4 C15 116.7(5) . . ? C14 N4 Cu3 123.7(4) . . ? C15 N4 Cu3 119.5(4) . . ? C18 N5 N6 107.5(5) . . ? C18 N5 Cu4 132.2(4) . . ? N6 N5 Cu4 120.0(3) . . ? C20 N6 N5 108.7(4) . . ? C20 N6 Cu5 131.2(4) . . ? N5 N6 Cu5 119.6(4) . . ? C26 N7 C27 115.9(7) . . ? C30 N8 N9 108.2(5) . . ? C30 N8 Cu6 132.9(5) . . ? N9 N8 Cu6 118.9(4) . . ? C32 N9 N8 108.7(5) . . ? C32 N9 Cu5 133.0(5) . . ? N8 N9 Cu5 116.0(3) . . ? C39 N10 C38 116.3(5) . . ? C39 N10 Cu2 120.4(4) . . ? C38 N10 Cu2 123.1(4) . . ? C42 N11 N12 107.6(4) . . ? C42 N11 Cu7 134.3(4) . . ? N12 N11 Cu7 117.5(4) . . ? C44 N12 N11 107.8(5) . . ? C44 N12 Cu8 131.6(4) . . ? N11 N12 Cu8 120.3(3) . . ? C50 N13 C51 117.0(5) . . ? C50 N13 Cu3 122.7(4) . . ? C51 N13 Cu3 120.0(4) . . ? C54 N14 N15 107.9(4) . . ? C54 N14 Cu7 132.2(4) . . ? N15 N14 Cu7 118.6(3) . . ? C56 N15 N14 108.5(4) . . ? C56 N15 Cu9 132.4(4) . . ? N14 N15 Cu9 118.0(3) . . ? C62 N16 C63 115.9(6) . . ? C66 N17 N18 106.6(5) . . ? C66 N17 Cu8 135.6(4) . . ? N18 N17 Cu8 117.5(4) . . ? C68 N18 N17 109.1(5) . . ? C68 N18 Cu9 131.5(4) . . ? N17 N18 Cu9 119.1(4) . . ? C2 C1 C5 120.7(5) . . ? N1 C2 C1 123.2(6) . . ? N1 C3 C4 124.2(6) . . ? C3 C4 C5 119.8(6) . . ? C1 C5 C4 115.8(5) . . ? C1 C5 C6 124.0(5) . . ? C4 C5 C6 120.2(6) . . ? N2 C6 C7 109.1(5) . . ? N2 C6 C5 121.7(5) . . ? C7 C6 C5 129.1(5) . . ? C6 C7 C8 106.4(5) . . ? N3 C8 C7 108.4(5) . . ? N3 C8 C9 121.6(5) . . ? C7 C8 C9 130.1(6) . . ? C8 C9 C10 115.2(5) . . ? C11 C10 C12 111.0(5) . . ? C11 C10 C9 110.9(5) . . ? C12 C10 C9 109.3(5) . . ? C17 C13 C14 120.6(5) . . ? N4 C14 C13 122.8(6) . . ? N4 C15 C16 123.5(5) . . ? C15 C16 C17 119.9(6) . . ? C13 C17 C16 116.4(5) . . ? C13 C17 C18 122.6(5) . . ? C16 C17 C18 121.0(5) . . ? N5 C18 C19 109.1(5) . . ? N5 C18 C17 121.1(5) . . ? C19 C18 C17 129.6(5) . . ? C18 C19 C20 105.4(6) . . ? N6 C20 C19 109.3(5) . . ? N6 C20 C21 119.5(5) . . ? C19 C20 C21 130.9(6) . . ? C20 C21 C22 116.1(5) . . ? C21 C22 C24 110.3(6) . . ? C21 C22 C23 111.5(6) . . ? C24 C22 C23 111.3(6) . . ? C29 C25 C26 120.3(7) . . ? N7 C26 C25 123.8(7) . . ? C28 C27 N7 125.1(7) . . ? C27 C28 C29 117.9(7) . . ? C25 C29 C28 116.9(7) . . ? C25 C29 C30 122.5(6) . . ? C28 C29 C30 120.6(6) . . ? N8 C30 C31 108.4(6) . . ? N8 C30 C29 121.7(6) . . ? C31 C30 C29 129.8(5) . . ? C32 C31 C30 106.1(5) . . ? N9 C32 C31 108.5(6) . . ? N9 C32 C33 119.7(6) . . ? C31 C32 C33 131.7(5) . . ? C34 C33 C32 116.2(6) . . ? C33 C34 C35 111.1(6) . . ? C33 C34 C36 108.8(6) . . ? C35 C34 C36 109.3(6) . . ? C38 C37 C41 119.8(5) . . ? N10 C38 C37 123.8(5) . . ? N10 C39 C40 123.7(5) . . ? C39 C40 C41 120.2(5) . . ? C40 C41 C37 116.2(5) . . ? C40 C41 C42 120.5(5) . . ? C37 C41 C42 123.3(5) . . ? N11 C42 C43 109.3(5) . . ? N11 C42 C41 123.6(5) . . ? C43 C42 C41 127.1(5) . . ? C44 C43 C42 106.1(5) . . ? N12 C44 C43 109.2(5) . . ? N12 C44 C45 121.6(5) . . ? C43 C44 C45 129.2(5) . . ? C44 C45 C46 114.9(6) . . ? C47 C46 C45 111.7(6) . . ? C47 C46 C48 112.6(7) . . ? C45 C46 C48 111.1(5) . . ? C50 C49 C53 119.9(5) . . ? N13 C50 C49 123.4(5) . . ? N13 C51 C52 122.7(5) . . ? C51 C52 C53 120.1(5) . . ? C49 C53 C52 116.8(5) . . ? C49 C53 C54 121.4(5) . . ? C52 C53 C54 121.9(5) . . ? N14 C54 C55 108.3(5) . . ? N14 C54 C53 121.6(5) . . ? C55 C54 C53 130.1(5) . . ? C56 C55 C54 106.2(5) . . ? N15 C56 C55 109.1(5) . . ? N15 C56 C57 120.0(5) . . ? C55 C56 C57 130.8(5) . . ? C56 C57 C58 114.3(5) . . ? C59 C58 C57 112.1(6) . . ? C59 C58 C60 111.3(5) . . ? C57 C58 C60 110.7(5) . . ? C65 C61 C62 118.9(6) . . ? N16 C62 C61 124.5(6) . . ? N16 C63 C64 124.6(6) . . ? C63 C64 C65 118.0(6) . . ? C61 C65 C64 118.0(6) . . ? C61 C65 C66 122.7(5) . . ? C64 C65 C66 119.2(6) . . ? N17 C66 C67 110.2(5) . . ? N17 C66 C65 121.8(5) . . ? C67 C66 C65 128.0(6) . . ? C66 C67 C68 105.1(6) . . ? N18 C68 C67 108.9(6) . . ? N18 C68 C69 120.7(6) . . ? C67 C68 C69 130.4(7) . . ? C68 C69 C70 115.1(7) . . ? C72 C70 C71 121.7(12) . . ? C72 C70 C69 121.3(12) . . ? C71 C70 C69 111.3(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.091 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.124