# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email houhongw@zzu.edu.cn _publ_contact_author_name 'Hongwei Hou' _publ_author_name 'Hongwei Hou' data_1 _database_code_depnum_ccdc_archive 'CCDC 869678' #TrackingRef '- 1,2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H84 Cd3 I6 N36' _chemical_formula_weight 2552.35 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' Cd Cd -0.8075 1.2024 '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 tetragonal _symmetry_space_group_name_H-M I4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' _cell_length_a 17.232(2) _cell_length_b 17.232(2) _cell_length_c 16.444(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4882.7(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.9117 _cell_measurement_theta_max 1.0000 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2460 _exptl_absorpt_coefficient_mu 2.601 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.594 _exptl_absorpt_correction_T_max 0.600 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 P4' _diffrn_measurement_method '\w 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 23885 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4170 _reflns_number_gt 3820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1705P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4170 _refine_ls_number_parameters 288 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2267 _refine_ls_wR_factor_gt 0.2200 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.004 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 C11 C 0.3046(10) 0.3009(9) 0.1759(9) 0.068(4) Uani 1 1 d . . . H11A H 0.2819 0.3509 0.1605 0.102 Uiso 1 1 calc R . . H11B H 0.2675 0.2593 0.1641 0.102 Uiso 1 1 calc R . . H11C H 0.3524 0.2923 0.1448 0.102 Uiso 1 1 calc R . . I1 I 0.6080(5) 0.0103(4) 0.4269(4) 0.121(3) Uani 0.25 1 d PU . . I2 I 0.0000 0.0000 0.09422(8) 0.0471(4) Uani 1 4 d S . . I3 I 0.5000 0.5000 0.22601(16) 0.0746(6) Uani 1 4 d S . . I4 I 0.5322(8) 0.4701(5) 0.0579(4) 0.127(5) Uani 0.25 1 d P . . I5 I 0.5390(2) 0.3174(2) 0.01165(18) 0.1116(10) Uani 0.50 1 d P . . Cd1 Cd 0.5000 0.0000 0.56268(10) 0.0536(4) Uani 1 2 d S . . Cd2 Cd 0.0000 0.0000 0.27072(15) 0.0574(5) Uani 1 4 d S . . N1 N 0.4716(6) 0.1312(5) 0.5703(7) 0.051(2) Uani 1 1 d . . . N2 N 0.4571(7) 0.2516(6) 0.6275(8) 0.062(3) Uani 1 1 d . . . N3 N 0.4183(6) 0.2468(5) 0.5542(6) 0.050(2) Uani 1 1 d . . . N4 N 0.1569(6) 0.2057(5) 0.2882(8) 0.054(3) Uani 1 1 d . . . N5 N 0.1944(7) 0.1578(7) 0.2295(9) 0.072(3) Uani 1 1 d . . . N6 N 0.0929(5) 0.0969(6) 0.2799(7) 0.052(2) Uani 1 1 d . . . N7 N 0.4806(8) 0.2097(7) 0.2220(10) 0.078(4) Uani 1 1 d . . . N8 N 0.5244(15) 0.1695(7) 0.2772(8) 0.111(7) Uani 1 1 d . . . N9 N 0.4842(8) 0.0992(8) 0.1650(9) 0.073(4) Uani 1 1 d . . . C1 C 0.4245(9) 0.1744(6) 0.5251(10) 0.063(4) Uani 1 1 d . . . H1 H 0.3984 0.1562 0.4779 0.076 Uiso 1 1 calc R . . C2 C 0.4874(12) 0.1816(9) 0.6358(11) 0.080(5) Uani 1 1 d . . . H2 H 0.5172 0.1666 0.6818 0.096 Uiso 1 1 calc R . . C3 C 0.3742(8) 0.3126(6) 0.5227(8) 0.050(3) Uani 1 1 d . . . H3 H 0.3583 0.3557 0.5546 0.060 Uiso 1 1 calc R . . C4 C 0.3580(7) 0.3041(6) 0.4378(8) 0.047(3) Uani 1 1 d . . . C5 C 0.2792(6) 0.2910(6) 0.4134(9) 0.045(2) Uani 1 1 d . . . C6 C 0.2172(11) 0.2802(11) 0.4737(13) 0.081(5) Uani 1 1 d . . . H6A H 0.2373 0.2921 0.5281 0.122 Uiso 1 1 calc R . . H6B H 0.1992 0.2263 0.4723 0.122 Uiso 1 1 calc R . . H6C H 0.1739 0.3151 0.4612 0.122 Uiso 1 1 calc R . . C7 C 0.2621(6) 0.2934(6) 0.3273(8) 0.042(2) Uani 1 1 d . . . C8 C 0.1795(7) 0.2871(7) 0.2985(9) 0.055(3) Uani 1 1 d . . . H8A H 0.1446 0.3122 0.3384 0.066 Uiso 1 1 calc R . . H8B H 0.1739 0.3147 0.2460 0.066 Uiso 1 1 calc R . . C9 C 0.0907(8) 0.1707(8) 0.3078(9) 0.061(4) Uani 1 1 d . . . H9 H 0.0488 0.1936 0.3367 0.073 Uiso 1 1 calc R . . C10 C 0.1532(9) 0.0988(9) 0.2294(8) 0.065(4) Uani 1 1 d . . . H10 H 0.1643 0.0564 0.1944 0.079 Uiso 1 1 calc R . . C12 C 0.3239(8) 0.3012(6) 0.2701(8) 0.049(3) Uani 1 1 d . . . C13 C 0.4141(6) 0.3072(6) 0.3779(6) 0.037(2) Uani 1 1 d . . . C18 C 0.3970(8) 0.3022(7) 0.2959(8) 0.050(3) Uani 1 1 d . . . C14 C 0.4655(9) 0.2932(7) 0.2360(10) 0.062(3) Uani 1 1 d . . . H14A H 0.4528 0.3189 0.1838 0.074 Uiso 1 1 calc R . . H14B H 0.5124 0.3183 0.2587 0.074 Uiso 1 1 calc R . . C15 C 0.4673(8) 0.1674(10) 0.1539(10) 0.067(4) Uani 1 1 d . . . H15 H 0.4475 0.1878 0.1044 0.081 Uiso 1 1 calc R . . C16 C 0.5138(12) 0.0980(11) 0.2457(15) 0.091(6) Uani 1 1 d . . . H16 H 0.5249 0.0516 0.2746 0.110 Uiso 1 1 calc R . . C17 C 0.4968(8) 0.3238(9) 0.4109(12) 0.073(4) Uani 1 1 d . . . H17A H 0.4930 0.3464 0.4655 0.109 Uiso 1 1 calc R . . H17B H 0.5233 0.3604 0.3747 0.109 Uiso 1 1 calc R . . H17C H 0.5263 0.2753 0.4135 0.109 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 C11 0.093(10) 0.078(9) 0.032(6) 0.005(7) -0.005(7) 0.009(7) I1 0.160(5) 0.119(4) 0.084(3) 0.037(3) -0.029(3) -0.086(4) I2 0.0459(5) 0.0459(5) 0.0495(8) 0.000 0.000 0.000 I3 0.0632(7) 0.0632(7) 0.0974(15) 0.000 0.000 0.000 I4 0.209(16) 0.096(5) 0.078(3) 0.003(3) -0.058(6) -0.002(3) I5 0.117(2) 0.146(3) 0.0726(16) 0.0032(17) -0.0074(14) -0.0101(18) Cd1 0.0483(6) 0.0383(5) 0.0743(8) 0.000 0.000 -0.0011(4) Cd2 0.0432(6) 0.0432(6) 0.0860(14) 0.000 0.000 0.000 N1 0.069(6) 0.040(4) 0.046(5) -0.006(4) -0.019(5) 0.003(4) N2 0.080(8) 0.049(6) 0.058(6) -0.015(5) -0.030(6) 0.014(5) N3 0.062(5) 0.048(5) 0.040(5) -0.006(4) -0.016(5) 0.002(4) N4 0.049(5) 0.027(4) 0.087(8) -0.009(5) -0.018(5) 0.000(4) N5 0.060(6) 0.061(7) 0.094(9) -0.028(6) 0.007(6) -0.008(6) N6 0.035(4) 0.046(5) 0.076(7) -0.010(5) -0.006(5) 0.001(4) N7 0.074(7) 0.056(6) 0.103(10) -0.029(7) 0.063(8) -0.017(6) N8 0.25(2) 0.045(7) 0.036(6) -0.010(6) 0.016(10) 0.028(10) N9 0.063(7) 0.060(7) 0.095(11) -0.050(7) 0.012(6) -0.007(6) C1 0.088(9) 0.022(5) 0.080(8) -0.002(5) -0.037(8) -0.011(5) C2 0.106(13) 0.059(8) 0.076(10) 0.002(7) -0.064(10) -0.001(8) C3 0.061(7) 0.039(5) 0.050(6) 0.001(5) -0.007(6) 0.029(5) C4 0.040(6) 0.027(5) 0.072(8) -0.015(4) -0.008(5) -0.011(4) C5 0.040(5) 0.039(5) 0.056(6) -0.006(6) 0.006(6) -0.004(4) C6 0.072(10) 0.077(10) 0.095(13) 0.004(9) 0.015(9) -0.001(8) C7 0.031(5) 0.034(5) 0.061(7) -0.004(5) -0.008(5) 0.012(4) C8 0.049(6) 0.043(6) 0.073(9) -0.027(6) -0.022(6) 0.005(5) C9 0.061(7) 0.060(8) 0.061(8) -0.037(7) 0.009(6) -0.016(6) C10 0.070(8) 0.076(9) 0.051(7) -0.030(7) 0.004(6) -0.032(7) C12 0.078(8) 0.031(5) 0.037(6) -0.003(4) -0.005(6) -0.002(5) C13 0.044(5) 0.034(5) 0.034(5) 0.001(4) 0.009(4) -0.002(4) C18 0.059(7) 0.036(5) 0.054(7) -0.005(5) 0.019(6) -0.004(5) C14 0.071(8) 0.038(6) 0.076(9) -0.017(6) 0.012(7) -0.006(6) C15 0.048(7) 0.065(9) 0.089(11) -0.028(7) -0.006(6) 0.009(6) C16 0.095(13) 0.061(10) 0.118(17) -0.003(9) 0.011(11) 0.036(9) C17 0.047(7) 0.084(10) 0.088(10) -0.035(10) -0.002(8) -0.001(7) _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 C11 C12 1.585(17) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? I1 Cd1 2.913(8) . ? I2 Cd2 2.902(3) . ? I3 I4 2.866(7) 4_565 ? I3 I4 2.866(7) 3_665 ? I3 I4 2.866(7) 2_655 ? I3 I4 2.866(7) . ? I4 I4 1.071(11) 2_655 ? I4 I4 1.071(11) 4_565 ? I4 I4 1.515(15) 3_665 ? I4 I5 2.742(10) . ? I4 I5 2.950(16) 2_655 ? I5 I4 2.950(16) 4_565 ? Cd1 N1 2.316(9) 3_655 ? Cd1 N1 2.316(9) . ? Cd1 N9 2.414(11) 8 ? Cd1 N9 2.414(11) 6_545 ? Cd1 I1 2.913(8) 3_655 ? Cd2 N6 2.319(10) 3 ? Cd2 N6 2.319(10) . ? Cd2 N6 2.319(10) 2 ? Cd2 N6 2.319(10) 4 ? N1 C1 1.329(17) . ? N1 C2 1.411(19) . ? N2 C2 1.32(2) . ? N2 N3 1.381(14) . ? N3 C1 1.340(15) . ? N3 C3 1.460(14) . ? N4 C9 1.330(18) . ? N4 N5 1.426(17) . ? N4 C8 1.466(15) . ? N5 C10 1.239(18) . ? N6 C10 1.330(18) . ? N6 C9 1.351(16) . ? N7 C15 1.36(2) . ? N7 N8 1.37(2) . ? N7 C14 1.482(17) . ? N8 C16 1.35(2) . ? N9 C15 1.22(2) . ? N9 C16 1.42(3) . ? N9 Cd1 2.414(11) 6_544 ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C4 1.432(19) . ? C3 H3 0.9500 . ? C4 C13 1.381(16) . ? C4 C5 1.434(16) . ? C5 C7 1.45(2) . ? C5 C6 1.47(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C12 1.428(19) . ? C7 C8 1.504(15) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 C18 1.329(19) . ? C13 C18 1.382(18) . ? C13 C17 1.552(17) . ? C18 C14 1.545(18) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? I4 I3 I4 21.5(2) 4_565 3_665 ? I4 I3 I4 30.6(3) 4_565 2_655 ? I4 I3 I4 21.5(2) 3_665 2_655 ? I4 I3 I4 21.54(19) 4_565 . ? I4 I3 I4 30.6(3) 3_665 . ? I4 I3 I4 21.5(2) 2_655 . ? I4 I4 I4 90.000(2) 2_655 4_565 ? I4 I4 I4 45.000(2) 2_655 3_665 ? I4 I4 I4 45.000(2) 4_565 3_665 ? I4 I4 I5 163.88(17) 2_655 . ? I4 I4 I5 90.4(14) 4_565 . ? I4 I4 I5 133.1(13) 3_665 . ? I4 I4 I3 79.23(10) 2_655 . ? I4 I4 I3 79.23(10) 4_565 . ? I4 I4 I3 74.68(14) 3_665 . ? I5 I4 I3 116.6(3) . . ? I4 I4 I5 68.4(11) 2_655 2_655 ? I4 I4 I5 153.2(9) 4_565 2_655 ? I4 I4 I5 111.7(11) 3_665 2_655 ? I5 I4 I5 106.1(3) . 2_655 ? I3 I4 I5 110.3(4) . 2_655 ? I4 I5 I4 21.3(3) . 4_565 ? N1 Cd1 N1 173.8(5) 3_655 . ? N1 Cd1 N9 85.6(4) 3_655 8 ? N1 Cd1 N9 90.1(4) . 8 ? N1 Cd1 N9 90.1(4) 3_655 6_545 ? N1 Cd1 N9 85.6(4) . 6_545 ? N9 Cd1 N9 91.6(8) 8 6_545 ? N1 Cd1 I1 96.7(3) 3_655 3_655 ? N1 Cd1 I1 88.0(3) . 3_655 ? N9 Cd1 I1 173.6(4) 8 3_655 ? N9 Cd1 I1 94.3(4) 6_545 3_655 ? N1 Cd1 I1 88.0(3) 3_655 . ? N1 Cd1 I1 96.7(3) . . ? N9 Cd1 I1 94.3(4) 8 . ? N9 Cd1 I1 173.6(4) 6_545 . ? I1 Cd1 I1 79.9(3) 3_655 . ? N6 Cd2 N6 172.5(6) 3 . ? N6 Cd2 N6 89.76(4) 3 2 ? N6 Cd2 N6 89.76(4) . 2 ? N6 Cd2 N6 89.76(4) 3 4 ? N6 Cd2 N6 89.76(4) . 4 ? N6 Cd2 N6 172.5(6) 2 4 ? N6 Cd2 I2 93.7(3) 3 . ? N6 Cd2 I2 93.7(3) . . ? N6 Cd2 I2 93.7(3) 2 . ? N6 Cd2 I2 93.7(3) 4 . ? C1 N1 C2 101.5(10) . . ? C1 N1 Cd1 130.2(8) . . ? C2 N1 Cd1 127.0(9) . . ? C2 N2 N3 103.1(10) . . ? C1 N3 N2 109.2(10) . . ? C1 N3 C3 129.7(10) . . ? N2 N3 C3 121.0(9) . . ? C9 N4 N5 106.9(9) . . ? C9 N4 C8 129.4(11) . . ? N5 N4 C8 120.8(12) . . ? C10 N5 N4 102.5(12) . . ? C10 N6 C9 102.2(11) . . ? C10 N6 Cd2 121.1(8) . . ? C9 N6 Cd2 132.8(8) . . ? C15 N7 N8 111.7(12) . . ? C15 N7 C14 128.4(16) . . ? N8 N7 C14 119.1(14) . . ? C16 N8 N7 97.7(16) . . ? C15 N9 C16 103.8(13) . . ? C15 N9 Cd1 127.0(13) . 6_544 ? C16 N9 Cd1 126.9(11) . 6_544 ? N1 C1 N3 111.8(11) . . ? N1 C1 H1 124.1 . . ? N3 C1 H1 124.1 . . ? N2 C2 N1 114.0(11) . . ? N2 C2 H2 123.0 . . ? N1 C2 H2 123.0 . . ? C4 C3 N3 111.6(10) . . ? C4 C3 H3 124.2 . . ? N3 C3 H3 124.2 . . ? C13 C4 C5 118.0(11) . . ? C13 C4 C3 123.7(11) . . ? C5 C4 C3 118.3(12) . . ? C4 C5 C7 117.5(11) . . ? C4 C5 C6 121.2(14) . . ? C7 C5 C6 121.2(12) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C5 119.7(10) . . ? C12 C7 C8 120.3(12) . . ? C5 C7 C8 120.0(11) . . ? N4 C8 C7 110.9(10) . . ? N4 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? N4 C9 N6 108.7(11) . . ? N4 C9 H9 125.7 . . ? N6 C9 H9 125.7 . . ? N5 C10 N6 117.8(13) . . ? N5 C10 H10 121.1 . . ? N6 C10 H10 121.1 . . ? C18 C12 C7 119.8(11) . . ? C18 C12 C11 120.8(13) . . ? C7 C12 C11 119.2(12) . . ? C4 C13 C18 122.9(11) . . ? C4 C13 C17 113.6(11) . . ? C18 C13 C17 123.3(11) . . ? C12 C18 C13 121.0(11) . . ? C12 C18 C14 121.2(12) . . ? C13 C18 C14 117.7(12) . . ? N7 C14 C18 109.2(10) . . ? N7 C14 H14A 109.8 . . ? C18 C14 H14A 109.8 . . ? N7 C14 H14B 109.8 . . ? C18 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? N9 C15 N7 110.6(16) . . ? N9 C15 H15 124.7 . . ? N7 C15 H15 124.7 . . ? N8 C16 N9 113.2(16) . . ? N8 C16 H16 123.4 . . ? N9 C16 H16 123.4 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I4 I3 I4 I4 92.07(4) 4_565 . . 2_655 ? I4 I3 I4 I4 46.04(2) 3_665 . . 2_655 ? I4 I3 I4 I4 -46.037(19) 3_665 . . 4_565 ? I4 I3 I4 I4 -92.07(4) 2_655 . . 4_565 ? I4 I3 I4 I4 46.037(17) 4_565 . . 3_665 ? I4 I3 I4 I4 -46.037(19) 2_655 . . 3_665 ? I4 I3 I4 I5 -84.9(15) 4_565 . . . ? I4 I3 I4 I5 -131.0(15) 3_665 . . . ? I4 I3 I4 I5 -177.0(15) 2_655 . . . ? I4 I3 I4 I5 154.0(11) 4_565 . . 2_655 ? I4 I3 I4 I5 108.0(11) 3_665 . . 2_655 ? I4 I3 I4 I5 61.9(11) 2_655 . . 2_655 ? I4 I4 I5 I4 -91(5) 2_655 . . 4_565 ? I4 I4 I5 I4 -15.6(4) 3_665 . . 4_565 ? I3 I4 I5 I4 78.1(7) . . . 4_565 ? I5 I4 I5 I4 -158.6(3) 2_655 . . 4_565 ? N1 Cd1 N1 C1 -141.3(13) 3_655 . . . ? N9 Cd1 N1 C1 173.0(14) 8 . . . ? N9 Cd1 N1 C1 -95.4(14) 6_545 . . . ? I1 Cd1 N1 C1 -0.9(13) 3_655 . . . ? I1 Cd1 N1 C1 78.7(14) . . . . ? N1 Cd1 N1 C2 23.6(14) 3_655 . . . ? N9 Cd1 N1 C2 -22.2(15) 8 . . . ? N9 Cd1 N1 C2 69.4(15) 6_545 . . . ? I1 Cd1 N1 C2 163.9(14) 3_655 . . . ? I1 Cd1 N1 C2 -116.5(14) . . . . ? C2 N2 N3 C1 2.7(17) . . . . ? C2 N2 N3 C3 178.4(14) . . . . ? C9 N4 N5 C10 -7.8(17) . . . . ? C8 N4 N5 C10 -170.1(13) . . . . ? N6 Cd2 N6 C10 140.3(11) 3 . . . ? N6 Cd2 N6 C10 -133.4(10) 2 . . . ? N6 Cd2 N6 C10 54.1(13) 4 . . . ? I2 Cd2 N6 C10 -39.7(11) . . . . ? N6 Cd2 N6 C9 -66.2(13) 3 . . . ? N6 Cd2 N6 C9 20.1(16) 2 . . . ? N6 Cd2 N6 C9 -152.5(12) 4 . . . ? I2 Cd2 N6 C9 113.8(13) . . . . ? C15 N7 N8 C16 -17.2(19) . . . . ? C14 N7 N8 C16 172.7(14) . . . . ? C2 N1 C1 N3 6.2(18) . . . . ? Cd1 N1 C1 N3 173.9(9) . . . . ? N2 N3 C1 N1 -6.0(17) . . . . ? C3 N3 C1 N1 178.8(13) . . . . ? N3 N2 C2 N1 1(2) . . . . ? C1 N1 C2 N2 -5(2) . . . . ? Cd1 N1 C2 N2 -172.8(12) . . . . ? C1 N3 C3 C4 -22(2) . . . . ? N2 N3 C3 C4 163.1(11) . . . . ? N3 C3 C4 C13 -68.4(15) . . . . ? N3 C3 C4 C5 111.2(12) . . . . ? C13 C4 C5 C7 -9.0(15) . . . . ? C3 C4 C5 C7 171.5(10) . . . . ? C13 C4 C5 C6 174.7(12) . . . . ? C3 C4 C5 C6 -4.9(17) . . . . ? C4 C5 C7 C12 5.8(15) . . . . ? C6 C5 C7 C12 -177.8(12) . . . . ? C4 C5 C7 C8 -174.6(10) . . . . ? C6 C5 C7 C8 1.7(16) . . . . ? C9 N4 C8 C7 138.5(15) . . . . ? N5 N4 C8 C7 -63.6(16) . . . . ? C12 C7 C8 N4 92.3(14) . . . . ? C5 C7 C8 N4 -87.2(14) . . . . ? N5 N4 C9 N6 13.8(17) . . . . ? C8 N4 C9 N6 174.0(13) . . . . ? C10 N6 C9 N4 -13.7(16) . . . . ? Cd2 N6 C9 N4 -170.7(10) . . . . ? N4 N5 C10 N6 -1.1(19) . . . . ? C9 N6 C10 N5 9.3(19) . . . . ? Cd2 N6 C10 N5 169.7(12) . . . . ? C5 C7 C12 C18 3.4(15) . . . . ? C8 C7 C12 C18 -176.1(10) . . . . ? C5 C7 C12 C11 178.0(11) . . . . ? C8 C7 C12 C11 -1.6(16) . . . . ? C5 C4 C13 C18 3.4(16) . . . . ? C3 C4 C13 C18 -177.1(10) . . . . ? C5 C4 C13 C17 178.4(11) . . . . ? C3 C4 C13 C17 -2.1(16) . . . . ? C7 C12 C18 C13 -9.5(16) . . . . ? C11 C12 C18 C13 176.0(11) . . . . ? C7 C12 C18 C14 167.1(10) . . . . ? C11 C12 C18 C14 -7.4(17) . . . . ? C4 C13 C18 C12 6.2(17) . . . . ? C17 C13 C18 C12 -168.3(11) . . . . ? C4 C13 C18 C14 -170.4(10) . . . . ? C17 C13 C18 C14 15.0(17) . . . . ? C15 N7 C14 C18 109.5(16) . . . . ? N8 N7 C14 C18 -82.3(17) . . . . ? C12 C18 C14 N7 -85.3(16) . . . . ? C13 C18 C14 N7 91.4(14) . . . . ? C16 N9 C15 N7 -2.5(18) . . . . ? Cd1 N9 C15 N7 -166.1(9) 6_544 . . . ? N8 N7 C15 N9 13.4(19) . . . . ? C14 N7 C15 N9 -177.6(13) . . . . ? N7 N8 C16 N9 16(2) . . . . ? C15 N9 C16 N8 -9(2) . . . . ? Cd1 N9 C16 N8 154.3(15) 6_544 . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.635 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.192 #==end=== data_2 _database_code_depnum_ccdc_archive 'CCDC 869679' #TrackingRef '- 1,2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H96 Cu4 I6 N42 O24' _chemical_formula_weight 2949.47 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.365(4) _cell_length_b 17.032(5) _cell_length_c 24.275(8) _cell_angle_alpha 89.682(7) _cell_angle_beta 89.479(5) _cell_angle_gamma 88.829(7) _cell_volume 5111(3) _cell_formula_units_Z 2 _cell_measurement_temperature 386(2) _cell_measurement_reflns_used 13087 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 27.8 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 2.723 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.803 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 383 _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 ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method 'profile data from \w-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 37859 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17680 _reflns_number_gt 14068 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17680 _refine_ls_number_parameters 1350 _refine_ls_number_restraints 834 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.002 _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 0.18520(4) 0.10014(4) 0.03180(2) 0.01467(14) Uani 1 1 d . . . Cu2 Cu -0.18520(4) 0.10285(3) 0.52895(2) 0.01297(13) Uani 1 1 d . . . Cu3 Cu 0.69166(4) 0.58220(4) 0.53299(2) 0.01321(13) Uani 1 1 d . . . Cu4 Cu 0.31268(4) 0.59962(4) 1.02537(2) 0.01353(13) Uani 1 1 d . . . N1 N 0.5688(3) 0.1519(2) -0.36075(14) 0.0129(9) Uani 1 1 d U . . N2 N 0.5433(4) 0.0758(3) -0.36813(18) 0.0294(11) Uani 1 1 d U . . N3 N 0.6885(3) 0.1065(2) -0.41913(15) 0.0165(9) Uani 1 1 d U . . N4 N 0.0471(3) 0.1549(2) -0.35540(14) 0.0108(8) Uani 1 1 d U . . N5 N 0.0610(3) 0.0752(2) -0.35474(16) 0.0208(10) Uani 1 1 d U . . N6 N -0.0752(3) 0.1112(2) -0.41083(14) 0.0135(9) Uani 1 1 d U . . N7 N 0.3128(3) 0.0759(2) -0.12311(14) 0.0132(9) Uani 1 1 d U . . N8 N 0.3918(3) 0.1238(2) -0.10426(15) 0.0169(9) Uani 1 1 d U . . N9 N 0.2702(3) 0.0984(2) -0.03751(15) 0.0150(9) Uani 1 1 d U . . N10 N 0.0806(3) 0.1038(2) 0.09440(15) 0.0157(9) Uani 1 1 d U . . N11 N -0.0474(3) 0.0649(2) 0.15391(16) 0.0200(10) Uani 1 1 d U . . N12 N -0.0429(3) 0.1450(2) 0.15226(15) 0.0139(9) Uani 1 1 d U . . N13 N -0.5612(3) 0.1426(2) 0.13774(15) 0.0158(9) Uani 1 1 d U . . N14 N -0.5210(4) 0.0705(3) 0.12288(19) 0.0338(12) Uani 1 1 d U . . N15 N -0.6786(3) 0.0973(2) 0.08038(15) 0.0197(10) Uani 1 1 d U . . N16 N -0.3277(3) 0.0687(2) 0.38054(14) 0.0124(9) Uani 1 1 d U . . N17 N -0.4093(3) 0.1166(2) 0.39935(15) 0.0184(9) Uani 1 1 d U . . N18 N -0.2823(3) 0.0966(2) 0.46478(14) 0.0129(9) Uani 1 1 d U . . N19 N 0.4716(3) 0.6414(2) 0.65521(14) 0.0129(9) Uani 1 1 d U . . N20 N 0.4406(3) 0.5655(2) 0.64783(16) 0.0214(10) Uani 1 1 d U . . N21 N 0.5883(3) 0.5924(2) 0.59669(14) 0.0131(9) Uani 1 1 d U . . N22 N -0.0117(3) 0.5712(2) 0.61711(17) 0.0228(10) Uani 1 1 d U . . N23 N -0.0499(3) 0.6447(2) 0.62851(14) 0.0136(9) Uani 1 1 d U . . N24 N -0.1755(3) 0.5921(2) 0.57932(14) 0.0121(8) Uani 1 1 d U . . N25 N 0.1647(3) 0.5820(2) 0.87563(15) 0.0140(9) Uani 1 1 d U . . N26 N 0.0927(3) 0.6368(2) 0.89609(15) 0.0167(9) Uani 1 1 d U . . N27 N 0.2161(3) 0.6018(2) 0.95987(14) 0.0130(9) Uani 1 1 d U . . N28 N 0.0643(3) 0.6423(2) 1.13591(15) 0.0140(9) Uani 1 1 d U . . N29 N 0.0394(4) 0.5665(3) 1.12646(19) 0.0324(12) Uani 1 1 d U . . N30 N 0.1872(3) 0.5994(2) 1.07780(14) 0.0119(8) Uani 1 1 d U . . N31 N -0.1844(3) 0.5681(2) 1.37694(14) 0.0134(9) Uani 1 1 d U . . N33 N -0.2205(3) 0.5838(2) 1.46416(14) 0.0142(9) Uani 1 1 d U . . N34 N -0.4595(3) 0.6481(2) 1.14476(15) 0.0141(9) Uani 1 1 d U . . N35 N -0.4408(3) 0.5690(2) 1.14158(17) 0.0211(10) Uani 1 1 d U . . N36 N -0.5786(3) 0.6058(2) 1.08642(14) 0.0142(9) Uani 1 1 d U . . N38 N -0.0052(4) 0.1675(3) -0.04935(19) 0.0327(12) Uani 1 1 d U . . N39 N -0.1954(3) -0.0894(3) 0.50775(17) 0.0231(10) Uani 1 1 d U . . N40 N 0.8744(3) 0.3016(3) 0.50909(16) 0.0197(10) Uani 1 1 d U . . N41 N 0.5429(3) 0.6798(3) 0.48349(16) 0.0237(10) Uani 1 1 d U . . N42 N 0.3030(3) 0.4085(3) 1.00360(16) 0.0213(10) Uani 1 1 d U . . N43 N -0.1101(3) 0.6211(2) 1.39479(15) 0.0146(9) Uani 1 1 d U . . N44 N 0.3637(4) 0.8040(3) 0.00916(17) 0.0265(11) Uani 1 1 d U . . O1 O 0.1834(3) 0.2350(2) 0.03325(15) 0.0345(10) Uani 1 1 d . . . H1 H 0.1284 0.2520 0.0184 0.052 Uiso 1 1 calc R . . O2 O 0.1618(3) -0.0268(2) 0.01712(15) 0.0316(9) Uani 1 1 d . . . H2 H 0.2045 -0.0526 0.0359 0.047 Uiso 1 1 calc R . . O3 O 0.0044(3) 0.2353(2) -0.03289(16) 0.0371(10) Uani 1 1 d U . . O4 O 0.0352(3) 0.1081(2) -0.02136(15) 0.0322(9) Uani 1 1 d U . . O5 O -0.0528(4) 0.1536(2) -0.09298(17) 0.0493(12) Uani 1 1 d U . . O6 O 0.8634(3) 0.3738(2) 0.51362(16) 0.0349(10) Uani 1 1 d U . . O7 O 0.8047(3) 0.2559(2) 0.52695(13) 0.0230(8) Uani 1 1 d U . . O8 O 0.9594(3) 0.2737(2) 0.48513(13) 0.0218(8) Uani 1 1 d U . . O9 O -0.1317(3) -0.0333(2) 0.51672(15) 0.0261(9) Uani 1 1 d U . . O10 O -0.2932(3) -0.0821(2) 0.51847(17) 0.0376(10) Uani 1 1 d U . . O11 O -0.1580(3) -0.1500(3) 0.4872(2) 0.0596(14) Uani 1 1 d U . . O13 O 0.5567(3) 0.6033(2) 0.48361(13) 0.0197(8) Uani 1 1 d U . . O14 O 0.4651(3) 0.7089(3) 0.45986(17) 0.0444(11) Uani 1 1 d U . . O15 O 0.6113(3) 0.7193(2) 0.50862(14) 0.0321(9) Uani 1 1 d U . . O16 O 0.3679(3) 0.4650(2) 1.00944(13) 0.0213(8) Uani 1 1 d U . . O17 O 0.2039(3) 0.4207(2) 1.00034(15) 0.0290(9) Uani 1 1 d U . . O18 O 0.3421(3) 0.3397(2) 1.00069(15) 0.0311(9) Uani 1 1 d U . . O19 O 0.3497(3) 0.8769(2) 0.01317(18) 0.0444(11) Uani 1 1 d U . . O20 O 0.2931(3) 0.7577(2) 0.02548(15) 0.0340(10) Uani 1 1 d U . . O21 O 0.4508(3) 0.7772(2) -0.01193(15) 0.0281(9) Uani 1 1 d U . . O22 O 0.6989(3) 0.8084(2) 0.61214(17) 0.0432(11) Uani 1 1 d . . . O23 O 0.6624(3) 0.4545(2) 0.51611(15) 0.0250(8) Uani 1 1 d . . . H23 H 0.7195 0.4294 0.5188 0.037 Uiso 1 1 calc R . . O24 O 0.4348(3) 0.6194(2) 0.97134(13) 0.0191(8) Uani 1 1 d . . . H24 H 0.4545 0.6649 0.9743 0.029 Uiso 1 1 calc R . . C1 C 0.6180(4) 0.0509(3) -0.4033(2) 0.0309(14) Uani 1 1 d U . . H1A H 0.6219 -0.0005 -0.4161 0.037 Uiso 1 1 calc R . . C2 C 0.6552(4) 0.1693(3) -0.39093(18) 0.0155(11) Uani 1 1 d U . . H2A H 0.6876 0.2181 -0.3922 0.019 Uiso 1 1 calc R . . C3 C 0.5105(4) 0.2051(3) -0.32251(18) 0.0151(11) Uani 1 1 d U . . H3A H 0.4927 0.2537 -0.3418 0.018 Uiso 1 1 calc R . . H3B H 0.5580 0.2177 -0.2924 0.018 Uiso 1 1 calc R . . C4 C 0.4062(4) 0.1711(3) -0.29863(18) 0.0144(10) Uani 1 1 d U . . C5 C 0.3079(4) 0.1907(3) -0.32357(17) 0.0124(10) Uani 1 1 d U . . C6 C 0.3059(4) 0.2294(3) -0.37997(18) 0.0169(11) Uani 1 1 d U . . H6A H 0.3080 0.2854 -0.3759 0.025 Uiso 1 1 calc R . . H6B H 0.2409 0.2157 -0.3986 0.025 Uiso 1 1 calc R . . H6C H 0.3676 0.2117 -0.4011 0.025 Uiso 1 1 calc R . . C7 C 0.2112(4) 0.1722(3) -0.29572(17) 0.0132(10) Uani 1 1 d U . . C8 C 0.2133(4) 0.1277(3) -0.24721(17) 0.0120(10) Uani 1 1 d U . . C9 C 0.1092(4) 0.1047(3) -0.21811(18) 0.0158(11) Uani 1 1 d U . . H9A H 0.1093 0.0489 -0.2124 0.024 Uiso 1 1 calc R . . H9B H 0.0484 0.1200 -0.2403 0.024 Uiso 1 1 calc R . . H9C H 0.1040 0.1307 -0.1832 0.024 Uiso 1 1 calc R . . C10 C 0.3132(4) 0.1009(3) -0.22556(17) 0.0131(10) Uani 1 1 d U . . C11 C 0.4109(4) 0.1259(3) -0.24952(17) 0.0109(10) Uani 1 1 d U . . C12 C 0.5198(4) 0.1052(3) -0.22524(18) 0.0184(11) Uani 1 1 d U . . H12A H 0.5670 0.0848 -0.2536 0.028 Uiso 1 1 calc R . . H12B H 0.5112 0.0662 -0.1969 0.028 Uiso 1 1 calc R . . H12C H 0.5505 0.1514 -0.2098 0.028 Uiso 1 1 calc R . . C13 C 0.1048(4) 0.2071(3) -0.31694(18) 0.0142(10) Uani 1 1 d U . . H13A H 0.0578 0.2186 -0.2857 0.017 Uiso 1 1 calc R . . H13B H 0.1193 0.2563 -0.3356 0.017 Uiso 1 1 calc R . . C14 C 0.3160(4) 0.0416(3) -0.17878(17) 0.0142(10) Uani 1 1 d U . . H14A H 0.2549 0.0072 -0.1825 0.017 Uiso 1 1 calc R . . H14B H 0.3814 0.0095 -0.1824 0.017 Uiso 1 1 calc R . . C15 C 0.2423(4) 0.0606(3) -0.08335(18) 0.0172(11) Uani 1 1 d U . . H15A H 0.1826 0.0287 -0.0867 0.021 Uiso 1 1 calc R . . C16 C 0.3627(4) 0.1355(3) -0.05206(18) 0.0165(11) Uani 1 1 d U . . H16 H 0.4016 0.1661 -0.0279 0.020 Uiso 1 1 calc R . . C17 C -0.0334(4) 0.1752(3) -0.38865(18) 0.0167(11) Uani 1 1 d U . . H17A H -0.0571 0.2264 -0.3955 0.020 Uiso 1 1 calc R . . C18 C -0.0143(4) 0.0520(3) -0.38874(19) 0.0202(12) Uani 1 1 d U . . H18A H -0.0247 -0.0005 -0.3969 0.024 Uiso 1 1 calc R . . C19 C 0.0346(4) 0.1669(3) 0.11747(18) 0.0160(11) Uani 1 1 d U . . H19A H 0.0537 0.2185 0.1103 0.019 Uiso 1 1 calc R . . C20 C 0.0282(4) 0.0433(3) 0.11859(19) 0.0204(12) Uani 1 1 d U . . H20A H 0.0446 -0.0091 0.1108 0.024 Uiso 1 1 calc R . . C21 C -0.1032(4) 0.1952(3) 0.19221(18) 0.0141(10) Uani 1 1 d U . . H21A H -0.1168 0.2463 0.1755 0.017 Uiso 1 1 calc R . . H21B H -0.0583 0.2029 0.2242 0.017 Uiso 1 1 calc R . . C22 C -0.2101(4) 0.1618(3) 0.21101(18) 0.0136(10) Uani 1 1 d U . . C23 C -0.3032(4) 0.1807(3) 0.18035(18) 0.0147(10) Uani 1 1 d U . . C24 C -0.2941(4) 0.2196(3) 0.12425(18) 0.0204(12) Uani 1 1 d U . . H24A H -0.3551 0.2060 0.1023 0.031 Uiso 1 1 calc R . . H24B H -0.2286 0.2019 0.1063 0.031 Uiso 1 1 calc R . . H24C H -0.2929 0.2756 0.1286 0.031 Uiso 1 1 calc R . . C25 C -0.4049(4) 0.1616(3) 0.20241(18) 0.0146(11) Uani 1 1 d U . . C26 C -0.5071(4) 0.1949(3) 0.1768(2) 0.0234(12) Uani 1 1 d U . . H26A H -0.5579 0.2083 0.2061 0.028 Uiso 1 1 calc R . . H26B H -0.4896 0.2432 0.1577 0.028 Uiso 1 1 calc R . . C27 C -0.4139(4) 0.1170(3) 0.25107(18) 0.0143(10) Uani 1 1 d U . . C28 C -0.5252(4) 0.0983(3) 0.2736(2) 0.0223(12) Uani 1 1 d U . . H28A H -0.5578 0.1449 0.2891 0.034 Uiso 1 1 calc R . . H28B H -0.5188 0.0585 0.3015 0.034 Uiso 1 1 calc R . . H28C H -0.5695 0.0798 0.2443 0.034 Uiso 1 1 calc R . . C29 C -0.3185(4) 0.0914(3) 0.27802(17) 0.0131(10) Uani 1 1 d U . . C30 C -0.2173(4) 0.1175(3) 0.25965(18) 0.0127(10) Uani 1 1 d U . . C31 C -0.1159(4) 0.0956(3) 0.29213(19) 0.0171(11) Uani 1 1 d U . . H31A H -0.0535 0.0993 0.2685 0.026 Uiso 1 1 calc R . . H31B H -0.1214 0.0428 0.3058 0.026 Uiso 1 1 calc R . . H31C H -0.1091 0.1309 0.3225 0.026 Uiso 1 1 calc R . . C32 C -0.6532(4) 0.1578(3) 0.11260(19) 0.0215(12) Uani 1 1 d U . . H32 H -0.6945 0.2037 0.1166 0.026 Uiso 1 1 calc R . . C34 C -0.2533(4) 0.0567(3) 0.41940(18) 0.0158(11) Uani 1 1 d U . . H34 H -0.1911 0.0255 0.4156 0.019 Uiso 1 1 calc R . . C35 C -0.3789(4) 0.1316(3) 0.45062(19) 0.0171(11) Uani 1 1 d U . . H35 H -0.4195 0.1631 0.4746 0.021 Uiso 1 1 calc R . . C36 C 0.5586(4) 0.6565(3) 0.62464(18) 0.0175(11) Uani 1 1 d U . . H36 H 0.5933 0.7044 0.6230 0.021 Uiso 1 1 calc R . . C37 C 0.5142(4) 0.5386(3) 0.61222(19) 0.0195(11) Uani 1 1 d U . . H37 H 0.5151 0.4874 0.5990 0.023 Uiso 1 1 calc R . . C38 C 0.4131(4) 0.6939(3) 0.69474(18) 0.0152(11) Uani 1 1 d U . . H38A H 0.4082 0.7464 0.6791 0.018 Uiso 1 1 calc R . . H38B H 0.4544 0.6967 0.7284 0.018 Uiso 1 1 calc R . . C39 C 0.3003(4) 0.6667(3) 0.70862(18) 0.0125(10) Uani 1 1 d U . . C40 C 0.2147(4) 0.6872(3) 0.67371(18) 0.0143(10) Uani 1 1 d U . . C41 C 0.2370(4) 0.7228(3) 0.61735(18) 0.0215(12) Uani 1 1 d U . . H41A H 0.1923 0.6985 0.5905 0.032 Uiso 1 1 calc R . . H41B H 0.3118 0.7142 0.6077 0.032 Uiso 1 1 calc R . . H41C H 0.2211 0.7782 0.6183 0.032 Uiso 1 1 calc R . . C42 C 0.1074(4) 0.6729(3) 0.69099(17) 0.0129(10) Uani 1 1 d U . . C43 C 0.0865(4) 0.6332(3) 0.74099(18) 0.0131(10) Uani 1 1 d U . . C44 C -0.0293(4) 0.6207(3) 0.75998(19) 0.0177(11) Uani 1 1 d U . . H44A H -0.0691 0.6697 0.7584 0.027 Uiso 1 1 calc R . . H44B H -0.0295 0.6013 0.7972 0.027 Uiso 1 1 calc R . . H44C H -0.0626 0.5833 0.7364 0.027 Uiso 1 1 calc R . . C45 C 0.0142(4) 0.7049(3) 0.65653(19) 0.0171(11) Uani 1 1 d U . . H45A H -0.0339 0.7355 0.6802 0.021 Uiso 1 1 calc R . . H45B H 0.0431 0.7402 0.6288 0.021 Uiso 1 1 calc R . . C46 C 0.1750(4) 0.6046(3) 0.77258(17) 0.0111(10) Uani 1 1 d U . . C47 C 0.2811(4) 0.6233(3) 0.75727(17) 0.0115(10) Uani 1 1 d U . . C48 C 0.3765(4) 0.5943(3) 0.79169(19) 0.0188(11) Uani 1 1 d U . . H48A H 0.3897 0.6313 0.8204 0.028 Uiso 1 1 calc R . . H48B H 0.4397 0.5892 0.7686 0.028 Uiso 1 1 calc R . . H48C H 0.3603 0.5442 0.8077 0.028 Uiso 1 1 calc R . . C49 C 0.1537(4) 0.5480(3) 0.82024(17) 0.0149(11) Uani 1 1 d U . . H49A H 0.0810 0.5284 0.8168 0.018 Uiso 1 1 calc R . . H49B H 0.2035 0.5035 0.8170 0.018 Uiso 1 1 calc R . . C50 C 0.2362(4) 0.5613(3) 0.91378(17) 0.0139(10) Uani 1 1 d U . . H50 H 0.2918 0.5242 0.9091 0.017 Uiso 1 1 calc R . . C51 C 0.1277(4) 0.6467(3) 0.94735(18) 0.0164(11) Uani 1 1 d U . . H51 H 0.0946 0.6811 0.9722 0.020 Uiso 1 1 calc R . . C52 C -0.1463(4) 0.6564(3) 0.60569(19) 0.0187(11) Uani 1 1 d U . . H52 H -0.1873 0.7027 0.6079 0.022 Uiso 1 1 calc R . . C53 C -0.0893(4) 0.5412(3) 0.5875(2) 0.0227(12) Uani 1 1 d U . . H53 H -0.0860 0.4906 0.5734 0.027 Uiso 1 1 calc R . . C54 C 0.1511(4) 0.6604(3) 1.10716(18) 0.0167(11) Uani 1 1 d U . . H54 H 0.1830 0.7094 1.1074 0.020 Uiso 1 1 calc R . . C56 C 0.0022(4) 0.6954(3) 1.1727(2) 0.0201(11) Uani 1 1 d U . . H56A H -0.0183 0.7421 1.1519 0.024 Uiso 1 1 calc R . . H56B H 0.0493 0.7116 1.2021 0.024 Uiso 1 1 calc R . . C57 C -0.0989(4) 0.6619(3) 1.19840(18) 0.0123(10) Uani 1 1 d U . . C59 C -0.2952(4) 0.6638(3) 1.20421(17) 0.0132(10) Uani 1 1 d U . . C60 C -0.2904(4) 0.6199(3) 1.25274(17) 0.0112(10) Uani 1 1 d U . . C61 C -0.3926(4) 0.5976(3) 1.28344(19) 0.0189(11) Uani 1 1 d U . . H61A H -0.4007 0.6294 1.3158 0.028 Uiso 1 1 calc R . . H61B H -0.3878 0.5432 1.2940 0.028 Uiso 1 1 calc R . . H61C H -0.4539 0.6060 1.2600 0.028 Uiso 1 1 calc R . . C62 C -0.2050(4) 0.7197(3) 1.11809(18) 0.0195(11) Uani 1 1 d U . . H62A H -0.2024 0.7757 1.1219 0.029 Uiso 1 1 calc R . . H62B H -0.2715 0.7060 1.1007 0.029 Uiso 1 1 calc R . . H62C H -0.1450 0.7016 1.0959 0.029 Uiso 1 1 calc R . . C63 C -0.1886(4) 0.5947(3) 1.27373(17) 0.0114(10) Uani 1 1 d U . . C64 C -0.0921(4) 0.6193(3) 1.24766(18) 0.0127(10) Uani 1 1 d U . . C65 C 0.0180(4) 0.6007(3) 1.2713(2) 0.0189(11) Uani 1 1 d U . . H65A H 0.0647 0.5799 1.2429 0.028 Uiso 1 1 calc R . . H65B H 0.0112 0.5625 1.3003 0.028 Uiso 1 1 calc R . . H65C H 0.0482 0.6477 1.2857 0.028 Uiso 1 1 calc R . . C66 C -0.1818(4) 0.5351(3) 1.32042(17) 0.0153(11) Uani 1 1 d U . . H66A H -0.2415 0.4994 1.3170 0.018 Uiso 1 1 calc R . . H66B H -0.1153 0.5044 1.3159 0.018 Uiso 1 1 calc R . . C67 C -0.4021(4) 0.6986(3) 1.18432(18) 0.0152(11) Uani 1 1 d U . . H67A H -0.4489 0.7081 1.2160 0.018 Uiso 1 1 calc R . . H67B H -0.3888 0.7489 1.1669 0.018 Uiso 1 1 calc R . . C68 C -0.5409(4) 0.6690(3) 1.11188(19) 0.0200(11) Uani 1 1 d U . . H68 H -0.5676 0.7200 1.1073 0.024 Uiso 1 1 calc R . . C69 C -0.5145(4) 0.5465(3) 1.10631(19) 0.0206(12) Uani 1 1 d U . . H69 H -0.5220 0.4944 1.0959 0.025 Uiso 1 1 calc R . . C70 C -0.2484(4) 0.5463(3) 1.41814(18) 0.0162(11) Uani 1 1 d U . . H70 H -0.3039 0.5105 1.4155 0.019 Uiso 1 1 calc R . . C71 C -0.1355(4) 0.6288(3) 1.44745(18) 0.0147(10) Uani 1 1 d U . . H71 H -0.0990 0.6617 1.4711 0.018 Uiso 1 1 calc R . . C72 C -0.1991(4) 0.6810(3) 1.17503(18) 0.0136(10) Uani 1 1 d U . . O25 O -0.0633(3) 0.1164(2) 0.47305(13) 0.0174(7) Uani 1 1 d . . . H25 H -0.0372 0.1600 0.4766 0.026 Uiso 1 1 calc R . . C75 C -0.3277(4) 0.0333(3) 0.32524(17) 0.0144(10) Uani 1 1 d U . . H75A H -0.3940 0.0046 0.3211 0.017 Uiso 1 1 calc R . . H75B H -0.2679 -0.0042 0.3227 0.017 Uiso 1 1 calc R . . C76 C 0.1150(4) 0.5438(3) 1.0911(2) 0.0294(14) Uani 1 1 d U . . H76 H 0.1184 0.4934 1.0765 0.035 Uiso 1 1 calc R . . C77 C -0.5943(4) 0.0461(3) 0.0877(2) 0.0308(14) Uani 1 1 d U . . H77 H -0.5885 -0.0019 0.0697 0.037 Uiso 1 1 calc R . . I1 I 0.19594(3) 0.82274(2) 0.260314(15) 0.03206(10) Uani 1 1 d . . . I6 I 0.29643(3) 0.61421(2) 0.333621(15) 0.03227(10) Uani 1 1 d . . . I3 I 0.18895(3) 1.16733(2) 0.247789(15) 0.03151(10) Uani 1 1 d . . . I4 I 0.30773(3) 0.37916(2) 0.157733(16) 0.03348(10) Uani 1 1 d . . . I5 I 0.30710(3) 0.49688(2) 0.245866(15) 0.02764(9) Uani 1 1 d . . . I2 I 0.18958(3) 0.99280(2) 0.254327(14) 0.02788(10) 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 0.0124(3) 0.0238(4) 0.0079(3) -0.0026(2) 0.0032(2) -0.0031(3) Cu2 0.0107(3) 0.0207(4) 0.0075(3) -0.0027(2) 0.0022(2) 0.0002(3) Cu3 0.0101(3) 0.0216(4) 0.0079(3) -0.0020(2) 0.0028(2) -0.0012(3) Cu4 0.0102(3) 0.0233(4) 0.0070(3) -0.0020(2) 0.0013(2) 0.0007(3) N1 0.012(2) 0.016(2) 0.0109(19) -0.0008(16) 0.0032(15) 0.0001(18) N2 0.033(3) 0.019(3) 0.035(3) -0.010(2) 0.024(2) -0.008(2) N3 0.014(2) 0.021(2) 0.014(2) -0.0008(18) -0.0013(16) 0.0025(19) N4 0.011(2) 0.011(2) 0.0107(18) 0.0002(16) 0.0015(15) 0.0013(17) N5 0.023(2) 0.015(2) 0.026(2) -0.0031(19) -0.0077(18) 0.0003(19) N6 0.014(2) 0.018(2) 0.0084(18) -0.0036(17) 0.0016(15) -0.0013(18) N7 0.015(2) 0.016(2) 0.0085(19) -0.0018(16) 0.0030(15) -0.0004(18) N8 0.015(2) 0.023(3) 0.012(2) -0.0020(17) 0.0009(16) -0.0048(19) N9 0.015(2) 0.020(2) 0.0110(19) -0.0022(17) -0.0008(16) -0.0041(18) N10 0.016(2) 0.018(2) 0.013(2) -0.0047(17) 0.0018(16) 0.0014(19) N11 0.026(2) 0.012(2) 0.022(2) 0.0002(18) 0.0115(18) -0.0039(19) N12 0.018(2) 0.012(2) 0.0126(19) -0.0030(16) 0.0069(16) -0.0010(18) N13 0.017(2) 0.015(2) 0.016(2) -0.0019(17) -0.0004(16) -0.0014(18) N14 0.038(3) 0.020(3) 0.043(3) -0.011(2) -0.017(2) 0.011(2) N15 0.025(2) 0.022(3) 0.013(2) 0.0004(18) 0.0013(17) -0.004(2) N16 0.013(2) 0.017(2) 0.0073(18) -0.0003(16) 0.0031(15) -0.0013(18) N17 0.019(2) 0.022(3) 0.015(2) -0.0026(18) 0.0037(17) 0.0055(19) N18 0.014(2) 0.016(2) 0.0083(18) -0.0013(16) 0.0025(15) 0.0001(18) N19 0.012(2) 0.016(2) 0.0111(19) -0.0005(17) 0.0054(15) -0.0040(18) N20 0.022(2) 0.018(3) 0.025(2) -0.0047(19) 0.0126(18) -0.004(2) N21 0.012(2) 0.016(2) 0.0113(19) 0.0004(17) 0.0016(15) -0.0012(18) N22 0.027(2) 0.016(2) 0.026(2) -0.0013(19) -0.0073(19) 0.005(2) N23 0.014(2) 0.018(2) 0.0092(18) -0.0001(17) -0.0002(15) -0.0001(18) N24 0.010(2) 0.016(2) 0.0097(18) 0.0006(16) 0.0012(15) -0.0001(18) N25 0.017(2) 0.014(2) 0.0106(19) -0.0009(17) 0.0037(16) -0.0035(18) N26 0.020(2) 0.016(2) 0.014(2) 0.0005(17) 0.0031(16) 0.0048(19) N27 0.013(2) 0.018(2) 0.0080(19) -0.0017(16) 0.0041(15) 0.0008(18) N28 0.015(2) 0.014(2) 0.0126(19) 0.0008(17) 0.0033(16) -0.0012(18) N29 0.031(3) 0.023(3) 0.043(3) -0.011(2) 0.026(2) -0.009(2) N30 0.012(2) 0.019(2) 0.0052(18) 0.0002(16) 0.0016(15) -0.0008(18) N31 0.015(2) 0.017(2) 0.0084(19) 0.0001(16) 0.0013(15) 0.0004(18) N33 0.013(2) 0.019(2) 0.0106(19) -0.0008(17) -0.0004(15) -0.0028(18) N34 0.014(2) 0.018(2) 0.0101(19) 0.0005(17) -0.0015(15) 0.0017(18) N35 0.027(2) 0.010(2) 0.026(2) -0.0018(18) -0.0082(19) 0.0002(19) N36 0.013(2) 0.020(2) 0.0095(19) -0.0021(17) 0.0014(15) 0.0008(18) N38 0.036(3) 0.033(3) 0.029(3) -0.003(2) 0.022(2) -0.012(3) N39 0.018(2) 0.023(3) 0.028(2) -0.006(2) 0.0076(19) 0.004(2) N40 0.026(3) 0.019(3) 0.014(2) 0.0009(18) -0.0069(18) 0.001(2) N41 0.022(2) 0.034(3) 0.016(2) 0.007(2) 0.0053(18) -0.001(2) N42 0.021(2) 0.030(3) 0.013(2) -0.0024(19) 0.0045(17) 0.005(2) N43 0.013(2) 0.019(2) 0.0111(19) -0.0006(17) 0.0002(15) -0.0008(18) N44 0.029(3) 0.033(3) 0.018(2) -0.001(2) -0.0027(19) -0.001(2) O1 0.039(2) 0.040(3) 0.025(2) 0.0057(18) 0.0041(17) 0.010(2) O2 0.034(2) 0.029(2) 0.032(2) -0.0019(18) 0.0077(17) -0.0082(19) O3 0.035(2) 0.029(3) 0.047(3) -0.013(2) 0.0082(19) -0.002(2) O4 0.041(2) 0.033(2) 0.023(2) 0.0054(18) 0.0010(17) -0.010(2) O5 0.078(3) 0.037(3) 0.034(2) -0.002(2) -0.008(2) -0.009(2) O6 0.040(2) 0.017(2) 0.047(3) -0.0058(19) 0.0036(19) 0.0039(19) O7 0.0211(19) 0.025(2) 0.0232(19) 0.0023(16) 0.0068(15) -0.0029(17) O8 0.0206(19) 0.022(2) 0.0228(18) -0.0016(16) 0.0038(15) -0.0017(16) O9 0.024(2) 0.017(2) 0.037(2) -0.0003(17) -0.0089(16) -0.0022(17) O10 0.024(2) 0.029(2) 0.059(3) -0.004(2) 0.0143(19) 0.0056(19) O11 0.030(3) 0.048(3) 0.101(4) -0.044(3) 0.002(2) 0.001(2) O13 0.0186(19) 0.021(2) 0.0198(18) -0.0038(15) 0.0023(14) -0.0009(16) O14 0.029(2) 0.059(3) 0.044(3) 0.016(2) -0.004(2) 0.016(2) O15 0.044(2) 0.029(2) 0.024(2) 0.0012(17) 0.0002(18) -0.009(2) O16 0.0202(19) 0.022(2) 0.0219(18) -0.0008(16) -0.0004(14) -0.0054(17) O17 0.018(2) 0.033(2) 0.037(2) -0.0049(18) 0.0024(16) 0.0018(18) O18 0.027(2) 0.025(2) 0.041(2) -0.0119(18) -0.0010(17) 0.0067(19) O19 0.050(3) 0.022(3) 0.061(3) -0.006(2) 0.004(2) 0.001(2) O20 0.036(2) 0.031(2) 0.034(2) -0.0005(19) 0.0109(18) -0.009(2) O21 0.021(2) 0.030(2) 0.034(2) -0.0023(18) -0.0032(16) -0.0035(18) O22 0.044(3) 0.034(3) 0.051(3) -0.003(2) 0.003(2) -0.003(2) O23 0.024(2) 0.023(2) 0.028(2) 0.0011(17) 0.0080(16) 0.0019(17) O24 0.0165(18) 0.026(2) 0.0150(17) -0.0018(15) 0.0019(14) -0.0053(16) C1 0.034(3) 0.022(3) 0.037(3) -0.010(3) 0.023(3) -0.012(3) C2 0.014(2) 0.016(3) 0.016(2) -0.001(2) 0.0028(19) -0.005(2) C3 0.011(2) 0.018(3) 0.016(2) -0.003(2) 0.0072(19) -0.003(2) C4 0.015(2) 0.015(3) 0.013(2) -0.009(2) 0.0039(19) 0.000(2) C5 0.018(3) 0.010(3) 0.009(2) -0.0011(19) 0.0015(18) -0.002(2) C6 0.021(3) 0.018(3) 0.012(2) 0.004(2) 0.0073(19) -0.004(2) C7 0.016(3) 0.014(3) 0.010(2) -0.0048(19) 0.0013(18) 0.000(2) C8 0.014(2) 0.011(3) 0.010(2) -0.0052(19) 0.0033(18) 0.002(2) C9 0.015(3) 0.016(3) 0.017(2) 0.002(2) 0.0083(19) -0.003(2) C10 0.019(3) 0.015(3) 0.005(2) -0.0071(19) 0.0045(18) 0.002(2) C11 0.016(2) 0.008(3) 0.009(2) -0.0020(18) 0.0026(18) 0.002(2) C12 0.017(3) 0.026(3) 0.012(2) -0.001(2) 0.0031(19) 0.003(2) C13 0.017(3) 0.013(3) 0.012(2) -0.001(2) -0.0004(19) -0.001(2) C14 0.021(3) 0.016(3) 0.006(2) -0.0030(19) 0.0030(18) 0.001(2) C15 0.014(3) 0.026(3) 0.011(2) 0.001(2) 0.0026(19) -0.004(2) C16 0.020(3) 0.019(3) 0.011(2) -0.002(2) 0.0001(19) -0.003(2) C17 0.016(3) 0.019(3) 0.015(2) 0.004(2) -0.0012(19) 0.003(2) C18 0.028(3) 0.017(3) 0.016(2) -0.004(2) -0.001(2) 0.001(2) C19 0.018(3) 0.017(3) 0.013(2) 0.002(2) 0.0050(19) -0.005(2) C20 0.023(3) 0.017(3) 0.020(3) -0.002(2) 0.010(2) 0.000(2) C21 0.017(3) 0.012(3) 0.013(2) -0.003(2) 0.0051(19) 0.001(2) C22 0.014(2) 0.014(3) 0.013(2) -0.005(2) 0.0040(18) 0.002(2) C23 0.025(3) 0.009(3) 0.010(2) -0.0033(19) 0.0005(19) 0.002(2) C24 0.026(3) 0.020(3) 0.015(2) 0.004(2) -0.003(2) 0.005(2) C25 0.012(2) 0.014(3) 0.018(2) -0.007(2) -0.0037(19) 0.004(2) C26 0.023(3) 0.022(3) 0.025(3) -0.004(2) -0.011(2) 0.004(2) C27 0.013(2) 0.016(3) 0.013(2) -0.008(2) 0.0011(18) -0.001(2) C28 0.011(3) 0.033(3) 0.023(3) -0.003(2) 0.006(2) 0.001(2) C29 0.015(2) 0.014(3) 0.010(2) -0.0047(19) 0.0040(18) -0.003(2) C30 0.015(2) 0.010(3) 0.013(2) -0.0064(19) -0.0008(18) -0.001(2) C31 0.015(3) 0.021(3) 0.016(2) 0.003(2) 0.0015(19) 0.002(2) C32 0.020(3) 0.023(3) 0.022(3) -0.008(2) 0.000(2) 0.002(2) C34 0.016(3) 0.021(3) 0.011(2) 0.003(2) 0.0016(19) -0.002(2) C35 0.014(3) 0.020(3) 0.017(2) -0.005(2) 0.0034(19) 0.002(2) C36 0.018(3) 0.021(3) 0.013(2) -0.001(2) 0.0042(19) -0.006(2) C37 0.022(3) 0.014(3) 0.023(3) -0.002(2) 0.007(2) 0.002(2) C38 0.018(3) 0.012(3) 0.015(2) -0.004(2) 0.0071(19) 0.000(2) C39 0.013(2) 0.012(3) 0.013(2) -0.0054(19) 0.0050(18) -0.001(2) C40 0.021(3) 0.011(3) 0.010(2) -0.0025(19) 0.0035(19) -0.002(2) C41 0.026(3) 0.025(3) 0.014(2) 0.005(2) 0.003(2) -0.003(2) C42 0.014(2) 0.014(3) 0.011(2) -0.0067(19) -0.0014(18) 0.001(2) C43 0.015(2) 0.012(3) 0.012(2) -0.0050(19) 0.0026(18) -0.004(2) C44 0.013(3) 0.022(3) 0.018(2) 0.000(2) -0.0003(19) 0.003(2) C45 0.019(3) 0.015(3) 0.017(2) -0.003(2) -0.001(2) -0.001(2) C46 0.015(2) 0.009(3) 0.009(2) -0.0070(18) 0.0022(18) -0.002(2) C47 0.016(2) 0.012(3) 0.006(2) -0.0047(18) 0.0012(18) 0.001(2) C48 0.016(3) 0.024(3) 0.017(2) -0.001(2) 0.0022(19) 0.001(2) C49 0.019(3) 0.017(3) 0.009(2) 0.000(2) 0.0020(19) -0.003(2) C50 0.011(2) 0.018(3) 0.013(2) 0.000(2) 0.0003(18) -0.001(2) C51 0.014(3) 0.022(3) 0.013(2) -0.002(2) 0.0053(19) 0.004(2) C52 0.015(3) 0.021(3) 0.019(3) 0.001(2) 0.000(2) 0.002(2) C53 0.023(3) 0.020(3) 0.025(3) -0.003(2) -0.003(2) 0.004(2) C54 0.017(3) 0.018(3) 0.016(2) -0.003(2) 0.005(2) -0.007(2) C56 0.017(3) 0.022(3) 0.022(3) -0.005(2) 0.012(2) 0.001(2) C57 0.011(2) 0.013(3) 0.013(2) -0.0040(19) 0.0037(18) -0.001(2) C59 0.012(2) 0.018(3) 0.010(2) -0.003(2) 0.0011(18) -0.001(2) C60 0.013(2) 0.010(3) 0.010(2) -0.0036(19) 0.0023(18) -0.001(2) C61 0.016(3) 0.023(3) 0.018(2) 0.001(2) 0.006(2) 0.000(2) C62 0.029(3) 0.019(3) 0.011(2) 0.003(2) 0.004(2) 0.000(2) C63 0.013(2) 0.015(3) 0.007(2) -0.0038(19) 0.0019(17) 0.000(2) C64 0.010(2) 0.013(3) 0.014(2) -0.005(2) 0.0016(18) 0.001(2) C65 0.012(3) 0.020(3) 0.025(3) -0.005(2) -0.002(2) 0.003(2) C66 0.022(3) 0.016(3) 0.008(2) -0.0027(19) 0.0011(19) 0.004(2) C67 0.017(3) 0.015(3) 0.014(2) -0.006(2) -0.0019(19) 0.001(2) C68 0.021(3) 0.020(3) 0.019(3) -0.002(2) -0.006(2) 0.005(2) C69 0.027(3) 0.015(3) 0.020(3) -0.003(2) -0.002(2) 0.001(2) C70 0.009(2) 0.023(3) 0.016(2) 0.000(2) 0.0034(19) 0.000(2) C71 0.013(2) 0.017(3) 0.013(2) -0.001(2) 0.0007(18) 0.001(2) C72 0.024(3) 0.007(3) 0.010(2) -0.0029(19) 0.0045(19) -0.001(2) O25 0.0168(18) 0.019(2) 0.0167(17) -0.0044(15) 0.0054(14) -0.0057(15) C75 0.017(3) 0.015(3) 0.011(2) -0.003(2) 0.0064(18) -0.004(2) C76 0.032(3) 0.024(3) 0.032(3) -0.013(3) 0.021(2) -0.005(3) C77 0.034(3) 0.020(3) 0.039(3) -0.007(3) -0.017(3) 0.009(3) I1 0.01934(19) 0.0381(2) 0.0390(2) 0.00198(18) -0.00341(15) -0.00574(17) I6 0.0262(2) 0.0299(2) 0.0409(2) -0.00662(17) -0.00368(16) -0.00073(17) I3 0.02053(19) 0.0376(2) 0.0362(2) -0.00245(17) 0.00165(15) 0.00615(17) I4 0.0318(2) 0.0302(2) 0.0383(2) -0.00560(17) 0.00459(16) 0.00267(18) I5 0.01597(18) 0.0291(2) 0.0378(2) -0.00294(17) 0.00158(15) 0.00058(16) I2 0.01539(18) 0.0388(2) 0.02932(19) 0.00145(17) 0.00127(14) 0.00053(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 N9 1.976(4) . ? Cu1 N10 1.987(4) . ? Cu1 N15 2.065(4) 1_655 ? Cu1 O2 2.218(4) . ? Cu1 O4 2.270(4) . ? Cu1 O1 2.298(4) . ? Cu2 N18 1.980(4) . ? Cu2 N3 1.998(4) 1_456 ? Cu2 N6 2.013(4) 1_556 ? Cu2 O25 2.035(3) . ? Cu2 O9 2.418(4) . ? Cu3 N33 1.985(4) 1_654 ? Cu3 N21 2.004(4) . ? Cu3 N24 2.009(4) 1_655 ? Cu3 O13 2.088(3) . ? Cu3 O23 2.253(4) . ? Cu4 N27 1.997(4) . ? Cu4 N30 1.998(4) . ? Cu4 N36 2.015(4) 1_655 ? Cu4 O24 2.023(3) . ? Cu4 O16 2.411(4) . ? N1 C2 1.328(6) . ? N1 N2 1.353(6) . ? N1 C3 1.475(6) . ? N2 C1 1.317(6) . ? N3 C2 1.330(6) . ? N3 C1 1.353(6) . ? N3 Cu2 1.998(4) 1_654 ? N4 C17 1.326(6) . ? N4 N5 1.365(5) . ? N4 C13 1.489(5) . ? N5 C18 1.318(6) . ? N6 C17 1.334(6) . ? N6 C18 1.358(6) . ? N6 Cu2 2.013(4) 1_554 ? N7 C15 1.323(6) . ? N7 N8 1.369(5) . ? N7 C14 1.475(5) . ? N8 C16 1.329(6) . ? N9 C15 1.339(6) . ? N9 C16 1.362(6) . ? N10 C19 1.329(6) . ? N10 C20 1.358(6) . ? N11 C20 1.312(6) . ? N11 N12 1.368(5) . ? N12 C19 1.329(6) . ? N12 C21 1.483(5) . ? N13 C32 1.316(6) . ? N13 N14 1.364(6) . ? N13 C26 1.479(6) . ? N14 C77 1.326(6) . ? N15 C32 1.341(6) . ? N15 C77 1.358(6) . ? N15 Cu1 2.065(4) 1_455 ? N16 C34 1.335(6) . ? N16 N17 1.362(5) . ? N16 C75 1.475(5) . ? N17 C35 1.331(6) . ? N18 C34 1.340(6) . ? N18 C35 1.370(6) . ? N19 C36 1.329(6) . ? N19 N20 1.370(5) . ? N19 C38 1.488(6) . ? N20 C37 1.326(6) . ? N21 C36 1.333(6) . ? N21 C37 1.357(6) . ? N22 C53 1.317(6) . ? N22 N23 1.359(5) . ? N23 C52 1.330(6) . ? N23 C45 1.480(6) . ? N24 C52 1.329(6) . ? N24 C53 1.376(6) . ? N24 Cu3 2.009(4) 1_455 ? N25 C50 1.327(6) . ? N25 N26 1.369(5) . ? N25 C49 1.475(5) . ? N26 C51 1.334(6) . ? N27 C50 1.336(6) . ? N27 C51 1.357(6) . ? N28 C54 1.316(6) . ? N28 N29 1.355(6) . ? N28 C56 1.475(6) . ? N29 C76 1.317(6) . ? N30 C54 1.330(6) . ? N30 C76 1.352(6) . ? N31 C70 1.326(6) . ? N31 N43 1.375(5) . ? N31 C66 1.486(5) . ? N33 C70 1.341(6) . ? N33 C71 1.371(6) . ? N33 Cu3 1.985(4) 1_456 ? N34 C68 1.331(6) . ? N34 N35 1.366(5) . ? N34 C67 1.487(6) . ? N35 C69 1.320(6) . ? N36 C68 1.339(6) . ? N36 C69 1.359(6) . ? N36 Cu4 2.015(4) 1_455 ? N38 O3 1.233(6) . ? N38 O5 1.243(6) . ? N38 O4 1.309(6) . ? N39 O11 1.229(5) . ? N39 O10 1.239(5) . ? N39 O9 1.271(5) . ? N40 O6 1.239(5) . ? N40 O7 1.247(5) . ? N40 O8 1.281(5) . ? N41 O14 1.220(5) . ? N41 O15 1.256(5) . ? N41 O13 1.311(5) . ? N42 O17 1.242(5) . ? N42 O18 1.259(5) . ? N42 O16 1.276(5) . ? N43 C71 1.320(6) . ? N44 O20 1.249(5) . ? N44 O19 1.254(6) . ? N44 O21 1.265(5) . ? O1 H1 0.8200 . ? O2 H2 0.8200 . ? O23 H23 0.8200 . ? O24 H24 0.8200 . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.532(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.397(6) . ? C4 C11 1.416(6) . ? C5 C7 1.408(6) . ? C5 C6 1.516(6) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.397(6) . ? C7 C13 1.525(6) . ? C8 C10 1.413(6) . ? C8 C9 1.520(6) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.408(6) . ? C10 C14 1.516(6) . ? C11 C12 1.509(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9300 . ? C16 H16 0.9300 . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.515(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C30 1.400(6) . ? C22 C23 1.408(6) . ? C23 C25 1.406(7) . ? C23 C24 1.515(6) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C27 1.406(6) . ? C25 C26 1.511(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C29 1.414(6) . ? C27 C28 1.515(6) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.405(6) . ? C29 C75 1.514(6) . ? C30 C31 1.526(6) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32 0.9300 . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.513(6) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.400(6) . ? C39 C47 1.411(6) . ? C40 C42 1.413(6) . ? C40 C41 1.519(6) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.410(6) . ? C42 C45 1.521(6) . ? C43 C46 1.419(6) . ? C43 C44 1.519(6) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.403(6) . ? C46 C49 1.526(6) . ? C47 C48 1.524(6) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C56 C57 1.511(6) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C64 1.398(6) . ? C57 C72 1.400(6) . ? C59 C60 1.393(6) . ? C59 C72 1.412(6) . ? C59 C67 1.519(6) . ? C60 C63 1.420(6) . ? C60 C61 1.514(6) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 C72 1.529(6) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 C64 1.415(6) . ? C63 C66 1.520(6) . ? C64 C65 1.510(6) . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68 0.9300 . ? C69 H69 0.9300 . ? C70 H70 0.9300 . ? C71 H71 0.9300 . ? O25 H25 0.8200 . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C76 H76 0.9300 . ? C77 H77 0.9300 . ? I1 I2 2.8988(10) . ? I6 I5 2.9292(8) . ? I3 I2 2.9757(11) . ? I4 I5 2.9401(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N9 Cu1 N10 171.49(15) . . ? N9 Cu1 N15 93.21(15) . 1_655 ? N10 Cu1 N15 95.26(16) . 1_655 ? N9 Cu1 O2 85.60(15) . . ? N10 Cu1 O2 93.46(15) . . ? N15 Cu1 O2 101.33(15) 1_655 . ? N9 Cu1 O4 86.97(14) . . ? N10 Cu1 O4 84.53(14) . . ? N15 Cu1 O4 177.91(16) 1_655 . ? O2 Cu1 O4 80.76(14) . . ? N9 Cu1 O1 91.56(15) . . ? N10 Cu1 O1 87.68(15) . . ? N15 Cu1 O1 90.13(15) 1_655 . ? O2 Cu1 O1 168.31(14) . . ? O4 Cu1 O1 87.78(14) . . ? N18 Cu2 N3 91.26(15) . 1_456 ? N18 Cu2 N6 174.65(15) . 1_556 ? N3 Cu2 N6 93.96(15) 1_456 1_556 ? N18 Cu2 O25 86.26(14) . . ? N3 Cu2 O25 171.19(15) 1_456 . ? N6 Cu2 O25 88.41(14) 1_556 . ? N18 Cu2 O9 90.18(14) . . ? N3 Cu2 O9 107.84(15) 1_456 . ? N6 Cu2 O9 89.33(14) 1_556 . ? O25 Cu2 O9 80.64(13) . . ? N33 Cu3 N21 171.34(15) 1_654 . ? N33 Cu3 N24 91.48(15) 1_654 1_655 ? N21 Cu3 N24 94.51(15) . 1_655 ? N33 Cu3 O13 87.00(14) 1_654 . ? N21 Cu3 O13 85.62(14) . . ? N24 Cu3 O13 165.23(15) 1_655 . ? N33 Cu3 O23 87.34(15) 1_654 . ? N21 Cu3 O23 96.52(14) . . ? N24 Cu3 O23 109.61(14) 1_655 . ? O13 Cu3 O23 85.00(13) . . ? N27 Cu4 N30 92.35(15) . . ? N27 Cu4 N36 173.33(16) . 1_655 ? N30 Cu4 N36 92.96(15) . 1_655 ? N27 Cu4 O24 86.06(14) . . ? N30 Cu4 O24 170.39(15) . . ? N36 Cu4 O24 88.03(14) 1_655 . ? N27 Cu4 O16 92.55(14) . . ? N30 Cu4 O16 107.84(14) . . ? N36 Cu4 O16 89.66(14) 1_655 . ? O24 Cu4 O16 81.72(13) . . ? C2 N1 N2 110.0(4) . . ? C2 N1 C3 126.1(4) . . ? N2 N1 C3 123.8(4) . . ? C1 N2 N1 102.9(4) . . ? C2 N3 C1 103.2(4) . . ? C2 N3 Cu2 125.2(3) . 1_654 ? C1 N3 Cu2 131.6(3) . 1_654 ? C17 N4 N5 110.0(4) . . ? C17 N4 C13 126.9(4) . . ? N5 N4 C13 122.4(3) . . ? C18 N5 N4 102.6(4) . . ? C17 N6 C18 103.0(4) . . ? C17 N6 Cu2 129.3(3) . 1_554 ? C18 N6 Cu2 127.1(3) . 1_554 ? C15 N7 N8 110.5(4) . . ? C15 N7 C14 126.7(4) . . ? N8 N7 C14 122.6(4) . . ? C16 N8 N7 102.9(4) . . ? C15 N9 C16 104.0(4) . . ? C15 N9 Cu1 125.0(3) . . ? C16 N9 Cu1 131.0(3) . . ? C19 N10 C20 103.4(4) . . ? C19 N10 Cu1 127.9(3) . . ? C20 N10 Cu1 128.2(3) . . ? C20 N11 N12 102.8(4) . . ? C19 N12 N11 109.9(4) . . ? C19 N12 C21 127.2(4) . . ? N11 N12 C21 122.0(4) . . ? C32 N13 N14 110.5(4) . . ? C32 N13 C26 125.9(4) . . ? N14 N13 C26 123.6(4) . . ? C77 N14 N13 102.5(4) . . ? C32 N15 C77 103.1(4) . . ? C32 N15 Cu1 121.8(3) . 1_455 ? C77 N15 Cu1 135.1(3) . 1_455 ? C34 N16 N17 110.8(4) . . ? C34 N16 C75 126.4(4) . . ? N17 N16 C75 122.8(4) . . ? C35 N17 N16 102.6(4) . . ? C34 N18 C35 103.4(4) . . ? C34 N18 Cu2 121.5(3) . . ? C35 N18 Cu2 134.7(3) . . ? C36 N19 N20 110.5(4) . . ? C36 N19 C38 128.5(4) . . ? N20 N19 C38 121.0(3) . . ? C37 N20 N19 102.2(4) . . ? C36 N21 C37 103.8(4) . . ? C36 N21 Cu3 128.9(3) . . ? C37 N21 Cu3 125.8(3) . . ? C53 N22 N23 103.3(4) . . ? C52 N23 N22 110.1(4) . . ? C52 N23 C45 125.9(4) . . ? N22 N23 C45 123.6(4) . . ? C52 N24 C53 103.1(4) . . ? C52 N24 Cu3 125.7(3) . 1_455 ? C53 N24 Cu3 130.9(3) . 1_455 ? C50 N25 N26 110.4(4) . . ? C50 N25 C49 127.2(4) . . ? N26 N25 C49 122.2(4) . . ? C51 N26 N25 102.4(4) . . ? C50 N27 C51 103.8(4) . . ? C50 N27 Cu4 123.9(3) . . ? C51 N27 Cu4 131.9(3) . . ? C54 N28 N29 109.5(4) . . ? C54 N28 C56 126.0(4) . . ? N29 N28 C56 124.4(4) . . ? C76 N29 N28 102.7(4) . . ? C54 N30 C76 102.1(4) . . ? C54 N30 Cu4 125.8(3) . . ? C76 N30 Cu4 132.0(3) . . ? C70 N31 N43 110.6(4) . . ? C70 N31 C66 126.4(4) . . ? N43 N31 C66 122.6(4) . . ? C70 N33 C71 103.5(4) . . ? C70 N33 Cu3 123.3(3) . 1_456 ? C71 N33 Cu3 132.3(3) . 1_456 ? C68 N34 N35 109.8(4) . . ? C68 N34 C67 127.4(4) . . ? N35 N34 C67 122.5(4) . . ? C69 N35 N34 102.8(4) . . ? C68 N36 C69 102.9(4) . . ? C68 N36 Cu4 129.3(3) . 1_455 ? C69 N36 Cu4 127.2(3) . 1_455 ? O3 N38 O5 121.1(5) . . ? O3 N38 O4 120.7(5) . . ? O5 N38 O4 118.2(5) . . ? O11 N39 O10 121.1(5) . . ? O11 N39 O9 118.5(4) . . ? O10 N39 O9 120.4(4) . . ? O6 N40 O7 121.6(4) . . ? O6 N40 O8 118.9(4) . . ? O7 N40 O8 119.5(4) . . ? O14 N41 O15 123.5(5) . . ? O14 N41 O13 119.3(5) . . ? O15 N41 O13 117.3(4) . . ? O17 N42 O18 120.7(4) . . ? O17 N42 O16 121.1(4) . . ? O18 N42 O16 118.2(4) . . ? C71 N43 N31 102.6(4) . . ? O20 N44 O19 121.1(5) . . ? O20 N44 O21 119.7(5) . . ? O19 N44 O21 119.2(5) . . ? Cu1 O1 H1 109.5 . . ? Cu1 O2 H2 109.5 . . ? N38 O4 Cu1 130.0(3) . . ? N39 O9 Cu2 125.6(3) . . ? N41 O13 Cu3 104.9(3) . . ? N42 O16 Cu4 124.5(3) . . ? Cu3 O23 H23 109.5 . . ? Cu4 O24 H24 109.5 . . ? N2 C1 N3 114.1(5) . . ? N2 C1 H1A 122.9 . . ? N3 C1 H1A 122.9 . . ? N1 C2 N3 109.7(4) . . ? N1 C2 H2A 125.1 . . ? N3 C2 H2A 125.1 . . ? N1 C3 C4 113.8(4) . . ? N1 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N1 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C11 121.7(4) . . ? C5 C4 C3 118.8(4) . . ? C11 C4 C3 119.3(4) . . ? C4 C5 C7 118.5(4) . . ? C4 C5 C6 120.5(4) . . ? C7 C5 C6 121.0(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C5 120.7(4) . . ? C8 C7 C13 120.4(4) . . ? C5 C7 C13 118.7(4) . . ? C7 C8 C10 119.9(4) . . ? C7 C8 C9 121.1(4) . . ? C10 C8 C9 119.0(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C8 120.0(4) . . ? C11 C10 C14 119.6(4) . . ? C8 C10 C14 120.3(4) . . ? C10 C11 C4 118.5(4) . . ? C10 C11 C12 122.4(4) . . ? C4 C11 C12 119.1(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C7 114.0(4) . . ? N4 C13 H13A 108.8 . . ? C7 C13 H13A 108.8 . . ? N4 C13 H13B 108.8 . . ? C7 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? N7 C14 C10 114.9(4) . . ? N7 C14 H14A 108.5 . . ? C10 C14 H14A 108.5 . . ? N7 C14 H14B 108.5 . . ? C10 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? N7 C15 N9 109.4(4) . . ? N7 C15 H15A 125.3 . . ? N9 C15 H15A 125.3 . . ? N8 C16 N9 113.2(4) . . ? N8 C16 H16 123.4 . . ? N9 C16 H16 123.4 . . ? N4 C17 N6 110.0(4) . . ? N4 C17 H17A 125.0 . . ? N6 C17 H17A 125.0 . . ? N5 C18 N6 114.4(4) . . ? N5 C18 H18A 122.8 . . ? N6 C18 H18A 122.8 . . ? N10 C19 N12 109.7(4) . . ? N10 C19 H19A 125.2 . . ? N12 C19 H19A 125.2 . . ? N11 C20 N10 114.2(4) . . ? N11 C20 H20A 122.9 . . ? N10 C20 H20A 122.9 . . ? N12 C21 C22 113.9(4) . . ? N12 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N12 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C30 C22 C23 120.8(4) . . ? C30 C22 C21 120.8(4) . . ? C23 C22 C21 118.3(4) . . ? C25 C23 C22 118.7(4) . . ? C25 C23 C24 120.6(4) . . ? C22 C23 C24 120.8(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 C27 121.1(4) . . ? C23 C25 C26 120.2(4) . . ? C27 C25 C26 118.5(4) . . ? N13 C26 C25 115.4(4) . . ? N13 C26 H26A 108.4 . . ? C25 C26 H26A 108.4 . . ? N13 C26 H26B 108.4 . . ? C25 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? C25 C27 C29 119.0(4) . . ? C25 C27 C28 119.2(4) . . ? C29 C27 C28 121.8(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C27 120.0(4) . . ? C30 C29 C75 121.2(4) . . ? C27 C29 C75 118.7(4) . . ? C22 C30 C29 119.7(4) . . ? C22 C30 C31 120.6(4) . . ? C29 C30 C31 119.6(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N13 C32 N15 109.9(4) . . ? N13 C32 H32 125.1 . . ? N15 C32 H32 125.1 . . ? N16 C34 N18 109.4(4) . . ? N16 C34 H34 125.3 . . ? N18 C34 H34 125.3 . . ? N17 C35 N18 113.8(4) . . ? N17 C35 H35 123.1 . . ? N18 C35 H35 123.1 . . ? N19 C36 N21 109.4(4) . . ? N19 C36 H36 125.3 . . ? N21 C36 H36 125.3 . . ? N20 C37 N21 114.1(4) . . ? N20 C37 H37 122.9 . . ? N21 C37 H37 122.9 . . ? N19 C38 C39 113.1(4) . . ? N19 C38 H38A 109.0 . . ? C39 C38 H38A 109.0 . . ? N19 C38 H38B 109.0 . . ? C39 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? C40 C39 C47 120.3(4) . . ? C40 C39 C38 119.4(4) . . ? C47 C39 C38 120.2(4) . . ? C39 C40 C42 119.3(4) . . ? C39 C40 C41 120.3(4) . . ? C42 C40 C41 120.4(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C40 120.7(4) . . ? C43 C42 C45 120.2(4) . . ? C40 C42 C45 119.0(4) . . ? C42 C43 C46 119.0(4) . . ? C42 C43 C44 120.1(4) . . ? C46 C43 C44 120.9(4) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N23 C45 C42 115.1(4) . . ? N23 C45 H45A 108.5 . . ? C42 C45 H45A 108.5 . . ? N23 C45 H45B 108.5 . . ? C42 C45 H45B 108.5 . . ? H45A C45 H45B 107.5 . . ? C47 C46 C43 120.1(4) . . ? C47 C46 C49 120.6(4) . . ? C43 C46 C49 119.1(4) . . ? C46 C47 C39 119.9(4) . . ? C46 C47 C48 120.4(4) . . ? C39 C47 C48 119.6(4) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N25 C49 C46 115.0(4) . . ? N25 C49 H49A 108.5 . . ? C46 C49 H49A 108.5 . . ? N25 C49 H49B 108.5 . . ? C46 C49 H49B 108.5 . . ? H49A C49 H49B 107.5 . . ? N25 C50 N27 109.7(4) . . ? N25 C50 H50 125.2 . . ? N27 C50 H50 125.2 . . ? N26 C51 N27 113.7(4) . . ? N26 C51 H51 123.1 . . ? N27 C51 H51 123.1 . . ? N24 C52 N23 110.0(4) . . ? N24 C52 H52 125.0 . . ? N23 C52 H52 125.0 . . ? N22 C53 N24 113.5(4) . . ? N22 C53 H53 123.2 . . ? N24 C53 H53 123.2 . . ? N28 C54 N30 111.0(4) . . ? N28 C54 H54 124.5 . . ? N30 C54 H54 124.5 . . ? N28 C56 C57 115.9(4) . . ? N28 C56 H56A 108.3 . . ? C57 C56 H56A 108.3 . . ? N28 C56 H56B 108.3 . . ? C57 C56 H56B 108.3 . . ? H56A C56 H56B 107.4 . . ? C64 C57 C72 121.0(4) . . ? C64 C57 C56 119.9(4) . . ? C72 C57 C56 118.8(4) . . ? C60 C59 C72 120.0(4) . . ? C60 C59 C67 120.6(4) . . ? C72 C59 C67 119.2(4) . . ? C59 C60 C63 119.8(4) . . ? C59 C60 C61 121.0(4) . . ? C63 C60 C61 119.1(4) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C72 C62 H62A 109.5 . . ? C72 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C72 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C60 119.9(4) . . ? C64 C63 C66 119.2(4) . . ? C60 C63 C66 120.7(4) . . ? C57 C64 C63 119.0(4) . . ? C57 C64 C65 118.9(4) . . ? C63 C64 C65 122.0(4) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N31 C66 C63 115.7(4) . . ? N31 C66 H66A 108.4 . . ? C63 C66 H66A 108.4 . . ? N31 C66 H66B 108.4 . . ? C63 C66 H66B 108.4 . . ? H66A C66 H66B 107.4 . . ? N34 C67 C59 114.1(4) . . ? N34 C67 H67A 108.7 . . ? C59 C67 H67A 108.7 . . ? N34 C67 H67B 108.7 . . ? C59 C67 H67B 108.7 . . ? H67A C67 H67B 107.6 . . ? N34 C68 N36 110.0(4) . . ? N34 C68 H68 125.0 . . ? N36 C68 H68 125.0 . . ? N35 C69 N36 114.5(4) . . ? N35 C69 H69 122.8 . . ? N36 C69 H69 122.8 . . ? N31 C70 N33 109.4(4) . . ? N31 C70 H70 125.3 . . ? N33 C70 H70 125.3 . . ? N43 C71 N33 113.9(4) . . ? N43 C71 H71 123.1 . . ? N33 C71 H71 123.1 . . ? C57 C72 C59 119.6(4) . . ? C57 C72 C62 120.4(4) . . ? C59 C72 C62 120.0(4) . . ? Cu2 O25 H25 109.5 . . ? N16 C75 C29 114.8(4) . . ? N16 C75 H75A 108.6 . . ? C29 C75 H75A 108.6 . . ? N16 C75 H75B 108.6 . . ? C29 C75 H75B 108.6 . . ? H75A C75 H75B 107.5 . . ? N29 C76 N30 114.7(5) . . ? N29 C76 H76 122.7 . . ? N30 C76 H76 122.7 . . ? N14 C77 N15 114.0(5) . . ? N14 C77 H77 123.0 . . ? N15 C77 H77 123.0 . . ? I6 I5 I4 177.570(16) . . ? I1 I2 I3 178.582(16) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 3.210 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.132