# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email liuchl@mail.ccnu.edu.cn _publ_contact_author_name 'Chang-Lin Liu' loop_ _publ_author_name 'Chang-Lin Liu' 'Xiang-Gao Meng' data_1 #TrackingRef '- 1-9.cif' _database_code_depnum_ccdc_archive 'CCDC 788582' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H23 Cu N7 O, 2(Cl O4)' _chemical_formula_sum 'C24 H23 Cl2 Cu N7 O9 ' _chemical_formula_weight 687.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.693(3) _cell_length_b 12.334(3) _cell_length_c 15.004(4) _cell_angle_alpha 80.155(5) _cell_angle_beta 67.328(4) _cell_angle_gamma 81.907(5) _cell_volume 1960.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2668 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.34 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 702 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8807 _exptl_absorpt_correction_T_max 0.9297 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 11333 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6830 _reflns_number_gt 3131 _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. In the refinement, both the perchlorate anion (Cl1/O2-O5 and Cl2/O6-O9) were found to be disordered over two sites. The command DFIX were used in the refinement to restrain some distances (eg. Cl-O=1.42(1)\%A and O-O=2.55(2)\%A). The thermal factors of some disordered oxygen atoms were restrained using commands of EADP and ISOR. The final most satisfactory occupancies for the Cl1-, Cl2-involved perchlorate anions were 0.55(1):0.45(1) and 0.52(1):0.48(1), respectively. Some residual electron densities, which should be considered as peaks from disordered methanol or water molecules, did not give a chemical meaningful result after a carefull refinement. Therefor, the contributions of the disordered solvent molecules (c.a. 107 e/unit cell) were removed from the diffraction data using the SQUEEZE routine of PLATON software and then final refinements were carried out. These electon densities account to ca. four methanol and four water molecules, i.e. the suitable formula should be 1.(CH~3~OH)~2~.(H2O)~2~. ; _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^)+(0.0758P)^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 6830 _refine_ls_number_parameters 394 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1393 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.2068 _refine_ls_wR_factor_gt 0.1835 _refine_ls_goodness_of_fit_ref 0.870 _refine_ls_restrained_S_all 0.900 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.54983(7) 0.67013(7) 0.70787(6) 0.0514(3) Uani 1 1 d . . . C1 C 0.7579(6) 0.5334(6) 0.5909(5) 0.0592(19) Uani 1 1 d . . . H1A H 0.7363 0.4598 0.6231 0.071 Uiso 1 1 calc R . . H1B H 0.8447 0.5289 0.5479 0.071 Uiso 1 1 calc R . . C2 C 0.6777(7) 0.5789(6) 0.5340(5) 0.0533(17) Uani 1 1 d . . . C3 C 0.6015(4) 0.6077(4) 0.4206(4) 0.064(2) Uani 1 1 d G . . C4 C 0.5717(5) 0.6166(4) 0.3384(3) 0.087(3) Uani 1 1 d G . . H4 H 0.6229 0.5798 0.2859 0.104 Uiso 1 1 calc R . . C5 C 0.4654(6) 0.6804(5) 0.3344(3) 0.096(3) Uani 1 1 d G . . H5 H 0.4455 0.6864 0.2794 0.115 Uiso 1 1 calc R . . C6 C 0.3890(5) 0.7353(4) 0.4128(4) 0.087(3) Uani 1 1 d G . . H6 H 0.3179 0.7781 0.4102 0.104 Uiso 1 1 calc R . . C7 C 0.4188(4) 0.7264(4) 0.4951(3) 0.072(2) Uani 1 1 d G . . H7 H 0.3677 0.7632 0.5475 0.086 Uiso 1 1 calc R . . C8 C 0.5251(4) 0.6626(4) 0.4990(3) 0.0541(17) Uani 1 1 d G . . C9 C 0.8107(6) 0.7044(6) 0.6223(5) 0.065(2) Uani 1 1 d . . . H9A H 0.8179 0.7263 0.5552 0.078 Uiso 1 1 calc R . . H9B H 0.8937 0.6859 0.6232 0.078 Uiso 1 1 calc R . . C10 C 0.7474(7) 0.7964(6) 0.6809(5) 0.0631(19) Uani 1 1 d . . . C11 C 0.7061(5) 0.9450(5) 0.7500(4) 0.083(3) Uani 1 1 d G . . C12 C 0.7034(7) 1.0408(5) 0.7882(5) 0.132(4) Uani 1 1 d G . . H12 H 0.7765 1.0742 0.7723 0.159 Uiso 1 1 calc R . . C13 C 0.5914(9) 1.0868(4) 0.8501(5) 0.141(5) Uani 1 1 d G . . H13 H 0.5896 1.1509 0.8757 0.169 Uiso 1 1 calc R . . C14 C 0.4822(7) 1.0369(6) 0.8739(4) 0.112(4) Uani 1 1 d G . . H14 H 0.4073 1.0677 0.9153 0.135 Uiso 1 1 calc R . . C15 C 0.4849(5) 0.9411(6) 0.8357(4) 0.090(3) Uani 1 1 d G . . H15 H 0.4118 0.9078 0.8516 0.109 Uiso 1 1 calc R . . C16 C 0.5969(6) 0.8952(4) 0.7738(4) 0.069(2) Uani 1 1 d G . . C17 C 0.7569(6) 0.5490(6) 0.7538(5) 0.0580(18) Uani 1 1 d . . . H17A H 0.8261 0.4932 0.7361 0.070 Uiso 1 1 calc R . . H17B H 0.7756 0.6007 0.7873 0.070 Uiso 1 1 calc R . . C18 C 0.6418(6) 0.4970(6) 0.8178(5) 0.0496(16) Uani 1 1 d . . . C19 C 0.5143(4) 0.3912(4) 0.9318(3) 0.0583(18) Uani 1 1 d G . . C20 C 0.4518(6) 0.3119(3) 1.0060(3) 0.081(2) Uani 1 1 d G . . H20 H 0.4956 0.2599 1.0361 0.097 Uiso 1 1 calc R . . C21 C 0.3238(6) 0.3103(4) 1.0351(3) 0.093(3) Uani 1 1 d G . . H21 H 0.2820 0.2572 1.0847 0.112 Uiso 1 1 calc R . . C22 C 0.2583(4) 0.3880(5) 0.9901(4) 0.084(3) Uani 1 1 d G . . H22 H 0.1727 0.3870 1.0096 0.100 Uiso 1 1 calc R . . C23 C 0.3209(4) 0.4674(4) 0.9159(3) 0.066(2) Uani 1 1 d G . . H23 H 0.2771 0.5194 0.8858 0.080 Uiso 1 1 calc R . . C24 C 0.4489(4) 0.4690(3) 0.8868(3) 0.0534(18) Uani 1 1 d G . . N1 N 0.7372(4) 0.6083(4) 0.6643(4) 0.0533(14) Uani 1 1 d . . . N2 N 0.5751(5) 0.6430(4) 0.5704(4) 0.0541(14) Uani 1 1 d . . . N3 N 0.6959(5) 0.5552(4) 0.4443(4) 0.0632(16) Uani 1 1 d . . . H3 H 0.7567 0.5141 0.4093 0.076 Uiso 1 1 calc R . . N4 N 0.6254(6) 0.8013(5) 0.7289(4) 0.0632(16) Uani 1 1 d . . . N5 N 0.7966(6) 0.8803(6) 0.6919(5) 0.080(2) Uani 1 1 d . . . H5A H 0.8741 0.8919 0.6661 0.096 Uiso 1 1 calc R . . N6 N 0.5331(5) 0.5356(4) 0.8135(4) 0.0503(13) Uani 1 1 d . . . N7 N 0.6357(5) 0.4117(5) 0.8866(4) 0.0625(16) Uani 1 1 d . . . H7A H 0.6972 0.3762 0.8998 0.075 Uiso 1 1 calc R . . O1 O 0.3790(4) 0.7357(4) 0.7488(4) 0.0838(16) Uani 1 1 d . . . H1C H 0.3621 0.8001 0.7298 0.101 Uiso 1 1 d R . . H1D H 0.3288 0.6979 0.7454 0.101 Uiso 1 1 d R . . Cl1 Cl 0.0796(13) 0.6099(11) 0.7557(11) 0.091(2) Uani 0.55 1 d PD A 1 O2 O 0.0484(15) 0.5391(15) 0.8462(11) 0.252(9) Uani 0.55 1 d PD A 1 O3 O 0.067(2) 0.5503(15) 0.6838(13) 0.167(9) Uani 0.55 1 d PD A 1 O4 O -0.0152(15) 0.7042(11) 0.7660(12) 0.139(5) Uani 0.55 1 d PD A 1 O5 O 0.2071(13) 0.6340(16) 0.7204(14) 0.188(6) Uani 0.55 1 d PD A 1 Cl1' Cl 0.0973(17) 0.6360(14) 0.7374(14) 0.091(2) Uani 0.45 1 d PD B 2 O2' O 0.197(2) 0.5625(19) 0.751(2) 0.252(9) Uani 0.45 1 d PD B 2 O3' O 0.090(3) 0.6193(19) 0.6446(15) 0.167(9) Uani 0.45 1 d PD B 2 O4' O -0.0250(16) 0.6322(17) 0.8102(13) 0.139(5) Uani 0.45 1 d PD B 2 O5' O 0.1339(15) 0.7521(13) 0.7217(15) 0.188(6) Uani 0.45 1 d PD B 2 Cl2 Cl 0.9669(16) 0.2760(14) 0.6345(12) 0.100(2) Uani 0.52 1 d PD C 1 O6 O 0.9126(18) 0.2676(19) 0.5628(14) 0.188(9) Uani 0.52 1 d PD C 1 O7 O 0.868(2) 0.2635(15) 0.7319(11) 0.159(10) Uani 0.52 1 d PD C 1 O8 O 1.001(2) 0.3882(14) 0.6149(19) 0.160(6) Uani 0.52 1 d PD C 1 O9 O 1.0729(16) 0.1987(17) 0.6274(15) 0.219(7) Uani 0.52 1 d PD C 1 Cl2' Cl 0.9598(17) 0.2596(16) 0.6535(13) 0.100(2) Uani 0.48 1 d PD D 2 O6' O 0.9691(19) 0.1893(15) 0.5821(12) 0.142(7) Uani 0.48 1 d PD D 2 O7' O 0.8273(15) 0.2984(16) 0.6979(13) 0.120(7) Uani 0.48 1 d PD D 2 O8' O 1.031(2) 0.3515(16) 0.603(2) 0.160(6) Uani 0.48 1 d PD D 2 O9' O 0.999(2) 0.1962(18) 0.7304(14) 0.219(7) Uani 0.48 1 d PD D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0388(4) 0.0642(6) 0.0482(5) -0.0113(4) -0.0113(4) -0.0034(4) C1 0.050(4) 0.072(5) 0.054(4) -0.023(4) -0.016(4) 0.008(4) C2 0.062(4) 0.061(5) 0.036(4) -0.007(3) -0.013(3) -0.016(4) C3 0.077(5) 0.066(5) 0.056(5) -0.016(4) -0.029(4) -0.007(4) C4 0.104(7) 0.101(7) 0.071(6) -0.027(5) -0.041(5) -0.018(6) C5 0.130(8) 0.101(7) 0.086(7) -0.004(6) -0.073(7) -0.018(6) C6 0.098(6) 0.092(6) 0.093(7) -0.012(5) -0.060(6) -0.006(5) C7 0.087(6) 0.077(5) 0.061(5) -0.012(4) -0.038(5) -0.002(5) C8 0.055(4) 0.057(4) 0.053(4) -0.006(4) -0.022(4) -0.007(3) C9 0.048(4) 0.087(6) 0.059(5) -0.002(4) -0.017(4) -0.020(4) C10 0.069(5) 0.064(5) 0.061(5) -0.005(4) -0.026(4) -0.017(4) C11 0.121(8) 0.056(5) 0.081(6) 0.002(5) -0.047(6) -0.026(5) C12 0.206(13) 0.083(8) 0.134(10) 0.002(7) -0.080(10) -0.068(8) C13 0.235(16) 0.083(8) 0.123(11) -0.011(7) -0.082(11) -0.024(10) C14 0.163(10) 0.088(7) 0.098(8) -0.036(6) -0.067(8) 0.032(7) C15 0.131(8) 0.062(6) 0.097(7) -0.017(5) -0.066(7) 0.007(5) C16 0.095(6) 0.058(5) 0.063(5) 0.006(4) -0.044(5) -0.010(5) C17 0.055(4) 0.064(5) 0.062(5) -0.014(4) -0.031(4) 0.004(4) C18 0.052(4) 0.062(5) 0.036(4) -0.014(3) -0.016(3) -0.003(3) C19 0.084(5) 0.058(5) 0.038(4) -0.010(4) -0.028(4) 0.000(4) C20 0.127(8) 0.058(5) 0.051(5) -0.009(4) -0.026(5) -0.003(5) C21 0.125(8) 0.088(7) 0.052(5) -0.002(5) -0.009(6) -0.041(6) C22 0.084(6) 0.108(7) 0.055(5) 0.000(5) -0.012(5) -0.049(5) C23 0.065(5) 0.088(6) 0.047(4) -0.008(4) -0.020(4) -0.012(4) C24 0.063(4) 0.066(5) 0.036(4) -0.019(4) -0.016(3) -0.016(4) N1 0.039(3) 0.062(4) 0.058(4) -0.015(3) -0.016(3) -0.001(3) N2 0.051(3) 0.067(4) 0.046(3) -0.016(3) -0.017(3) -0.005(3) N3 0.072(4) 0.060(4) 0.059(4) -0.016(3) -0.022(3) -0.001(3) N4 0.069(4) 0.066(4) 0.063(4) -0.013(3) -0.031(3) -0.007(3) N5 0.080(5) 0.079(5) 0.080(5) 0.002(4) -0.023(4) -0.040(4) N6 0.045(3) 0.055(3) 0.053(3) -0.011(3) -0.018(3) -0.004(3) N7 0.064(4) 0.072(4) 0.051(4) -0.011(3) -0.024(3) 0.010(3) O1 0.055(3) 0.097(4) 0.097(4) -0.028(3) -0.024(3) 0.009(3) Cl1 0.050(4) 0.121(6) 0.105(5) -0.027(4) -0.025(4) -0.012(4) O2 0.165(14) 0.30(2) 0.198(17) 0.077(16) -0.037(12) 0.052(15) O3 0.143(11) 0.19(2) 0.199(17) -0.091(16) -0.085(13) 0.016(15) O4 0.129(7) 0.163(16) 0.122(13) 0.000(9) -0.054(9) -0.006(11) O5 0.108(11) 0.221(17) 0.238(15) 0.004(15) -0.065(11) -0.060(10) Cl1' 0.050(4) 0.121(6) 0.105(5) -0.027(4) -0.025(4) -0.012(4) O2' 0.165(14) 0.30(2) 0.198(17) 0.077(16) -0.037(12) 0.052(15) O3' 0.143(11) 0.19(2) 0.199(17) -0.091(16) -0.085(13) 0.016(15) O4' 0.129(7) 0.163(16) 0.122(13) 0.000(9) -0.054(9) -0.006(11) O5' 0.108(11) 0.221(17) 0.238(15) 0.004(15) -0.065(11) -0.060(10) Cl2 0.105(2) 0.084(4) 0.081(6) -0.005(4) -0.005(4) -0.008(3) O6 0.151(17) 0.24(2) 0.22(2) -0.11(2) -0.108(16) 0.035(16) O7 0.24(3) 0.100(15) 0.099(13) -0.005(11) -0.015(16) -0.027(14) O8 0.098(11) 0.116(13) 0.204(11) -0.050(11) 0.022(9) 0.000(11) O9 0.185(17) 0.236(14) 0.173(16) 0.000(15) -0.046(14) 0.087(13) Cl2' 0.105(2) 0.084(4) 0.081(6) -0.005(4) -0.005(4) -0.008(3) O6' 0.144(18) 0.134(16) 0.133(15) -0.052(13) -0.025(13) 0.005(13) O7' 0.109(12) 0.114(14) 0.102(14) 0.043(10) -0.028(11) -0.001(9) O8' 0.098(11) 0.116(13) 0.204(11) -0.050(11) 0.022(9) 0.000(11) O9' 0.185(17) 0.236(14) 0.173(16) 0.000(15) -0.046(14) 0.087(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.947(4) . ? Cu1 N2 2.048(5) . ? Cu1 N6 2.063(5) . ? Cu1 N4 2.071(6) . ? Cu1 N1 2.098(5) . ? C1 N1 1.485(7) . ? C1 C2 1.492(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.319(7) . ? C2 N3 1.356(7) . ? C3 N3 1.337(7) . ? C3 C4 1.3900 . ? C3 C8 1.3900 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C8 N2 1.379(6) . ? C9 N1 1.468(8) . ? C9 C10 1.488(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N5 1.315(8) . ? C10 N4 1.325(8) . ? C11 N5 1.343(8) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 N4 1.375(7) . ? C17 C18 1.477(9) . ? C17 N1 1.499(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.315(7) . ? C18 N7 1.331(8) . ? C19 N7 1.356(7) . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9300 . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 N6 1.393(6) . ? N3 H3 0.8600 . ? N5 H5A 0.8600 . ? N7 H7A 0.8600 . ? O1 H1C 0.8201 . ? O1 H1D 0.8199 . ? Cl1 O2 1.430(15) . ? Cl1 O5 1.433(13) . ? Cl1 O3 1.467(14) . ? Cl1 O4 1.473(14) . ? Cl1' O4' 1.428(15) . ? Cl1' O2' 1.431(16) . ? Cl1' O3' 1.477(16) . ? Cl1' O5' 1.506(16) . ? Cl2 O9 1.434(15) . ? Cl2 O8 1.446(15) . ? Cl2 O6 1.468(15) . ? Cl2 O7 1.470(14) . ? Cl2' O8' 1.427(15) . ? Cl2' O6' 1.454(16) . ? Cl2' O9' 1.466(16) . ? Cl2' O7' 1.475(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 99.5(2) . . ? O1 Cu1 N6 100.8(2) . . ? N2 Cu1 N6 118.3(2) . . ? O1 Cu1 N4 96.2(2) . . ? N2 Cu1 N4 120.6(2) . . ? N6 Cu1 N4 114.1(2) . . ? O1 Cu1 N1 176.6(2) . . ? N2 Cu1 N1 81.9(2) . . ? N6 Cu1 N1 81.0(2) . . ? N4 Cu1 N1 80.5(2) . . ? N1 C1 C2 107.9(5) . . ? N1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N2 C2 N3 112.7(6) . . ? N2 C2 C1 121.9(5) . . ? N3 C2 C1 125.3(6) . . ? N3 C3 C4 133.3(4) . . ? N3 C3 C8 106.6(4) . . ? C4 C3 C8 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 120.0 . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? N2 C8 C7 130.8(4) . . ? N2 C8 C3 109.2(4) . . ? C7 C8 C3 120.0 . . ? N1 C9 C10 108.6(6) . . ? N1 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? N1 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N5 C10 N4 111.7(7) . . ? N5 C10 C9 128.4(7) . . ? N4 C10 C9 120.0(6) . . ? N5 C11 C12 134.4(5) . . ? N5 C11 C16 105.6(5) . . ? C12 C11 C16 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? N4 C16 C15 131.6(5) . . ? N4 C16 C11 108.4(5) . . ? C15 C16 C11 120.0 . . ? C18 C17 N1 108.1(5) . . ? C18 C17 H17A 110.1 . . ? N1 C17 H17A 110.1 . . ? C18 C17 H17B 110.1 . . ? N1 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? N6 C18 N7 113.7(6) . . ? N6 C18 C17 121.5(6) . . ? N7 C18 C17 124.7(6) . . ? N7 C19 C20 133.6(4) . . ? N7 C19 C24 106.4(4) . . ? C20 C19 C24 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 N6 131.5(4) . . ? C19 C24 N6 108.5(4) . . ? C9 N1 C1 111.9(5) . . ? C9 N1 C17 112.0(5) . . ? C1 N1 C17 112.4(5) . . ? C9 N1 Cu1 106.3(4) . . ? C1 N1 Cu1 106.8(4) . . ? C17 N1 Cu1 106.9(4) . . ? C2 N2 C8 104.4(5) . . ? C2 N2 Cu1 110.5(4) . . ? C8 N2 Cu1 145.0(4) . . ? C3 N3 C2 107.0(5) . . ? C3 N3 H3 126.5 . . ? C2 N3 H3 126.5 . . ? C10 N4 C16 105.4(6) . . ? C10 N4 Cu1 110.9(5) . . ? C16 N4 Cu1 143.8(5) . . ? C10 N5 C11 109.0(6) . . ? C10 N5 H5A 125.5 . . ? C11 N5 H5A 125.5 . . ? C18 N6 C24 104.4(5) . . ? C18 N6 Cu1 111.3(4) . . ? C24 N6 Cu1 144.3(4) . . ? C18 N7 C19 107.0(5) . . ? C18 N7 H7A 126.5 . . ? C19 N7 H7A 126.5 . . ? Cu1 O1 H1C 121.4 . . ? Cu1 O1 H1D 114.8 . . ? H1C O1 H1D 108.1 . . ? O2 Cl1 O5 110.5(12) . . ? O2 Cl1 O3 108.0(12) . . ? O5 Cl1 O3 106.9(12) . . ? O2 Cl1 O4 108.8(11) . . ? O5 Cl1 O4 117.5(12) . . ? O3 Cl1 O4 104.6(11) . . ? O4' Cl1' O2' 120.2(15) . . ? O4' Cl1' O3' 107.8(13) . . ? O2' Cl1' O3' 107.5(14) . . ? O4' Cl1' O5' 107.5(13) . . ? O2' Cl1' O5' 107.6(13) . . ? O3' Cl1' O5' 105.3(13) . . ? O9 Cl2 O8 110.8(13) . . ? O9 Cl2 O6 112.8(13) . . ? O8 Cl2 O6 105.2(13) . . ? O9 Cl2 O7 112.3(13) . . ? O8 Cl2 O7 107.3(12) . . ? O6 Cl2 O7 108.1(13) . . ? O8' Cl2' O6' 107.8(14) . . ? O8' Cl2' O9' 113.7(15) . . ? O6' Cl2' O9' 110.5(14) . . ? O8' Cl2' O7' 109.6(13) . . ? O6' Cl2' O7' 106.8(13) . . ? O9' Cl2' O7' 108.3(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -25.2(8) . . . . ? N1 C1 C2 N3 159.1(6) . . . . ? N3 C3 C4 C5 -178.8(6) . . . . ? C8 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C8 0.0 . . . . ? C6 C7 C8 N2 178.5(5) . . . . ? C6 C7 C8 C3 0.0 . . . . ? N3 C3 C8 N2 0.3(4) . . . . ? C4 C3 C8 N2 -178.8(4) . . . . ? N3 C3 C8 C7 179.1(4) . . . . ? C4 C3 C8 C7 0.0 . . . . ? N1 C9 C10 N5 154.4(7) . . . . ? N1 C9 C10 N4 -26.9(9) . . . . ? N5 C11 C12 C13 -178.1(7) . . . . ? C16 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 N4 178.1(6) . . . . ? C14 C15 C16 C11 0.0 . . . . ? N5 C11 C16 N4 0.0(5) . . . . ? C12 C11 C16 N4 -178.5(5) . . . . ? N5 C11 C16 C15 178.6(5) . . . . ? C12 C11 C16 C15 0.0 . . . . ? N1 C17 C18 N6 -24.9(8) . . . . ? N1 C17 C18 N7 157.9(6) . . . . ? N7 C19 C20 C21 -177.8(5) . . . . ? C24 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C19 0.0 . . . . ? C22 C23 C24 N6 177.4(5) . . . . ? N7 C19 C24 C23 178.4(4) . . . . ? C20 C19 C24 C23 0.0 . . . . ? N7 C19 C24 N6 0.4(4) . . . . ? C20 C19 C24 N6 -177.9(4) . . . . ? C10 C9 N1 C1 154.6(5) . . . . ? C10 C9 N1 C17 -78.1(6) . . . . ? C10 C9 N1 Cu1 38.4(6) . . . . ? C2 C1 N1 C9 -81.9(6) . . . . ? C2 C1 N1 C17 151.0(5) . . . . ? C2 C1 N1 Cu1 34.0(6) . . . . ? C18 C17 N1 C9 150.6(5) . . . . ? C18 C17 N1 C1 -82.4(6) . . . . ? C18 C17 N1 Cu1 34.4(6) . . . . ? N2 Cu1 N1 C9 91.8(4) . . . . ? N6 Cu1 N1 C9 -147.7(4) . . . . ? N4 Cu1 N1 C9 -31.3(4) . . . . ? N2 Cu1 N1 C1 -27.8(4) . . . . ? N6 Cu1 N1 C1 92.7(4) . . . . ? N4 Cu1 N1 C1 -150.9(5) . . . . ? N2 Cu1 N1 C17 -148.3(4) . . . . ? N6 Cu1 N1 C17 -27.9(4) . . . . ? N4 Cu1 N1 C17 88.6(4) . . . . ? N3 C2 N2 C8 -0.7(7) . . . . ? C1 C2 N2 C8 -176.9(6) . . . . ? N3 C2 N2 Cu1 177.6(4) . . . . ? C1 C2 N2 Cu1 1.4(7) . . . . ? C7 C8 N2 C2 -178.4(4) . . . . ? C3 C8 N2 C2 0.2(5) . . . . ? C7 C8 N2 Cu1 4.3(9) . . . . ? C3 C8 N2 Cu1 -177.1(5) . . . . ? O1 Cu1 N2 C2 -167.9(4) . . . . ? N6 Cu1 N2 C2 -60.0(5) . . . . ? N4 Cu1 N2 C2 89.0(5) . . . . ? N1 Cu1 N2 C2 15.2(4) . . . . ? O1 Cu1 N2 C8 9.3(7) . . . . ? N6 Cu1 N2 C8 117.2(7) . . . . ? N4 Cu1 N2 C8 -93.8(7) . . . . ? N1 Cu1 N2 C8 -167.6(7) . . . . ? C4 C3 N3 C2 178.2(4) . . . . ? C8 C3 N3 C2 -0.7(6) . . . . ? N2 C2 N3 C3 0.9(7) . . . . ? C1 C2 N3 C3 177.0(6) . . . . ? N5 C10 N4 C16 -0.4(8) . . . . ? C9 C10 N4 C16 -179.4(6) . . . . ? N5 C10 N4 Cu1 178.8(5) . . . . ? C9 C10 N4 Cu1 -0.2(8) . . . . ? C15 C16 N4 C10 -178.1(5) . . . . ? C11 C16 N4 C10 0.2(6) . . . . ? C15 C16 N4 Cu1 3.2(10) . . . . ? C11 C16 N4 Cu1 -178.5(6) . . . . ? O1 Cu1 N4 C10 -161.7(5) . . . . ? N2 Cu1 N4 C10 -56.7(6) . . . . ? N6 Cu1 N4 C10 93.5(5) . . . . ? N1 Cu1 N4 C10 17.9(5) . . . . ? O1 Cu1 N4 C16 17.0(7) . . . . ? N2 Cu1 N4 C16 122.0(7) . . . . ? N6 Cu1 N4 C16 -87.8(7) . . . . ? N1 Cu1 N4 C16 -163.4(8) . . . . ? N4 C10 N5 C11 0.4(8) . . . . ? C9 C10 N5 C11 179.3(7) . . . . ? C12 C11 N5 C10 178.0(5) . . . . ? C16 C11 N5 C10 -0.3(7) . . . . ? N7 C18 N6 C24 0.2(7) . . . . ? C17 C18 N6 C24 -177.3(5) . . . . ? N7 C18 N6 Cu1 178.4(4) . . . . ? C17 C18 N6 Cu1 1.0(7) . . . . ? C23 C24 N6 C18 -178.0(4) . . . . ? C19 C24 N6 C18 -0.4(5) . . . . ? C23 C24 N6 Cu1 4.8(8) . . . . ? C19 C24 N6 Cu1 -177.6(5) . . . . ? O1 Cu1 N6 C18 -161.5(4) . . . . ? N2 Cu1 N6 C18 91.4(4) . . . . ? N4 Cu1 N6 C18 -59.6(5) . . . . ? N1 Cu1 N6 C18 15.7(4) . . . . ? O1 Cu1 N6 C24 15.6(6) . . . . ? N2 Cu1 N6 C24 -91.5(6) . . . . ? N4 Cu1 N6 C24 117.5(6) . . . . ? N1 Cu1 N6 C24 -167.2(6) . . . . ? N6 C18 N7 C19 0.1(7) . . . . ? C17 C18 N7 C19 177.4(5) . . . . ? C20 C19 N7 C18 177.7(4) . . . . ? C24 C19 N7 C18 -0.3(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C17 H17A O8 0.97 2.52 3.42(2) 153.1 . C12 H12 O7 0.93 2.59 3.38(2) 143.3 1_565 C9 H9A O9 0.97 2.60 3.51(2) 156.0 2_766 C1 H1B O8 0.97 2.55 3.38(2) 143.3 2_766 N3 H3 O3 0.86 2.13 2.97(2) 164.9 2_666 O1 H1D O5 0.82 1.90 2.710(15) 168.7 . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.550 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.085 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.009 0.000 0.010 626 107 ' ' _platon_squeeze_details ; Owing to the serious crystal deterioration, although the crystals selected were sealed in capillaries with mother liquid, the non-coordinated solvent molecules could not be modeled by discrete atoms. Then the contribution of the solvent to the diffraction pattern was subtracted using the SQUEEZE procedure in PLATON. The result indicated that the solvent-accessible void in the unit cell has a volume of 626\%A^3^. (consisting of about 32% of the crystal volume). The residual electron density count amounted to 107 e per unit cell, i.e. every Cu(NTB)(ClO~4~)~2~ molecule being distributed with 53.5 electrons, corresponding to nearly two methanol and two water molecules (as the crystals were grown in the mixture of methanol and water solvent.). The formula of the title complex should be Cu(NTB)(ClO~4~)~2~(CH~3~OH)~2~(H~2~O)~2~. ; # start Validation Reply Form _vrf_PLAT420_1 ; PROBLEM: D-H Without Acceptor O1 - H1C ... ? RESPONSE: These potential hydrogen-bond acceptors were treated using the SQUEEZE routine from PLATON due to their disorders. ; _vrf_PLAT606_1 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: These residual electron densities are too diffuse to allow accurate refinement for unit methanol or water solvent molecules. Then, these solvent molecules were treated using the SQUEEZE routine from PLATON. ; # end Validation Reply Form data_2 #TrackingRef '- 1-9.cif' _database_code_depnum_ccdc_archive 'CCDC 788586' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H46 Cu2 N15 O2, 3(Cl O4), 4(H2 O)' _chemical_formula_sum 'C54 H54 Cl3 Cu2 N15 O18' _chemical_formula_weight 1434.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9417(6) _cell_length_b 15.2306(7) _cell_length_c 16.0023(7) _cell_angle_alpha 71.288(1) _cell_angle_beta 63.771(2) _cell_angle_gamma 82.833(1) _cell_volume 3093.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7549 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.17 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8404 _exptl_absorpt_correction_T_max 0.9822 _exptl_absorpt_process_details 'SADABS, Sheldrick,1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 33501 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.50 _reflns_number_total 12601 _reflns_number_gt 9078 _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. In the refinement, two perchlorate anion (Cl2/O7-O10, Cl3/O11-O14) were found to be disordered at two sites. Then the command DFIX was used to restrain some distances (eg. Cl-O=1.38(1)\%A and O-O=2.25(2)\%A). For O12', EADP was used to restrain its thermal factor to be same as that of O12. Because the electron densities of solvent molecules are too diffused to allow the accurate refinement of one unit molecule, the occupancies for water O17-O20 molecules were refined freeely and their final occupancies are ca. 0.67, 0.33, 0.40 and 0.60 respectively. All the C- and N-bounded hydrogen atoms were postitioned geometrically. Hydrogen atoms attached to water oxygen atoms were positioned best matching their hydrogen-bond environment with O-H=0.82\%A and U~iso~(H)=1.2U~eq~(O). ; _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^)+(0.1207P)^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 12601 _refine_ls_number_parameters 935 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1717 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.03361(3) 1.08405(3) 0.21005(3) 0.03555(14) Uani 1 1 d . . . Cu2 Cu 0.68585(3) 0.62505(3) 0.59198(3) 0.03821(14) Uani 1 1 d . . . C1 C 0.5760(4) 0.5547(3) 0.8094(3) 0.0649(12) Uani 1 1 d . . . H1A H 0.5053 0.5414 0.8351 0.078 Uiso 1 1 calc R . . H1B H 0.5968 0.5268 0.8615 0.078 Uiso 1 1 calc R . . C2 C 0.5938(3) 0.6556(3) 0.7746(3) 0.0533(10) Uani 1 1 d . . . C3 C 0.5896(3) 0.8019(4) 0.7707(4) 0.0649(12) Uani 1 1 d . . . C4 C 0.5802(4) 0.8879(4) 0.7892(5) 0.0841(16) Uani 1 1 d . . . H4 H 0.5627 0.8920 0.8512 0.101 Uiso 1 1 calc R . . C5 C 0.5985(4) 0.9646(4) 0.7104(6) 0.0916(19) Uani 1 1 d . . . H5 H 0.5936 1.0227 0.7194 0.110 Uiso 1 1 calc R . . C6 C 0.6236(4) 0.9598(3) 0.6190(5) 0.0844(18) Uani 1 1 d . . . H6 H 0.6315 1.0144 0.5686 0.101 Uiso 1 1 calc R . . C7 C 0.6373(3) 0.8771(3) 0.6000(4) 0.0671(13) Uani 1 1 d . . . H7 H 0.6563 0.8745 0.5371 0.081 Uiso 1 1 calc R . . C8 C 0.6221(3) 0.7966(3) 0.6770(3) 0.0549(10) Uani 1 1 d . . . C9 C 0.7242(3) 0.4667(3) 0.7323(3) 0.0506(10) Uani 1 1 d . . . H9A H 0.7077 0.4036 0.7749 0.061 Uiso 1 1 calc R . . H9B H 0.7539 0.4987 0.7577 0.061 Uiso 1 1 calc R . . C10 C 0.7952(3) 0.4670(2) 0.6311(3) 0.0430(9) Uani 1 1 d . . . C11 C 0.8677(3) 0.5142(2) 0.4737(3) 0.0390(8) Uani 1 1 d . . . C12 C 0.8993(3) 0.5597(2) 0.3737(3) 0.0451(9) Uani 1 1 d . . . H12 H 0.8681 0.6128 0.3516 0.054 Uiso 1 1 calc R . . C13 C 0.9786(3) 0.5227(3) 0.3092(3) 0.0525(10) Uani 1 1 d . . . H13 H 1.0011 0.5520 0.2426 0.063 Uiso 1 1 calc R . . C14 C 1.0256(3) 0.4432(3) 0.3410(3) 0.0545(10) Uani 1 1 d . . . H14 H 1.0783 0.4202 0.2953 0.065 Uiso 1 1 calc R . . C15 C 0.9956(3) 0.3980(3) 0.4386(3) 0.0498(10) Uani 1 1 d . . . H15 H 1.0274 0.3449 0.4598 0.060 Uiso 1 1 calc R . . C16 C 0.9162(3) 0.4341(2) 0.5045(3) 0.0429(9) Uani 1 1 d . . . C17 C 0.5709(3) 0.4500(3) 0.7217(3) 0.0597(11) Uani 1 1 d . . . H17A H 0.5232 0.4174 0.7868 0.072 Uiso 1 1 calc R . . H17B H 0.6127 0.4046 0.6916 0.072 Uiso 1 1 calc R . . C18 C 0.5172(3) 0.5042(3) 0.6627(3) 0.0517(10) Uani 1 1 d . . . C19 C 0.4089(3) 0.5438(3) 0.6005(4) 0.0642(12) Uani 1 1 d . . . C20 C 0.3294(4) 0.5535(5) 0.5752(6) 0.095(2) Uani 1 1 d . . . H20 H 0.2778 0.5096 0.6070 0.114 Uiso 1 1 calc R . . C21 C 0.3307(5) 0.6300(5) 0.5023(7) 0.110(3) Uani 1 1 d . . . H21 H 0.2790 0.6380 0.4833 0.132 Uiso 1 1 calc R . . C22 C 0.4052(5) 0.6961(4) 0.4555(5) 0.0935(19) Uani 1 1 d . . . H22 H 0.4010 0.7480 0.4072 0.112 Uiso 1 1 calc R . . C23 C 0.4878(4) 0.6889(4) 0.4772(4) 0.0745(14) Uani 1 1 d . . . H23 H 0.5393 0.7330 0.4440 0.089 Uiso 1 1 calc R . . C24 C 0.4861(3) 0.6104(3) 0.5526(3) 0.0540(10) Uani 1 1 d . . . C25 C 1.0918(3) 1.2089(2) 0.2834(3) 0.0421(8) Uani 1 1 d . . . H25A H 1.0256 1.2320 0.3146 0.051 Uiso 1 1 calc R . . H25B H 1.1404 1.2503 0.2768 0.051 Uiso 1 1 calc R . . C26 C 1.1010(3) 1.1127(2) 0.3434(2) 0.0373(8) Uani 1 1 d . . . C27 C 1.1321(3) 0.9956(2) 0.4489(2) 0.0372(7) Uani 1 1 d . . . C28 C 1.1580(3) 0.9364(3) 0.5195(3) 0.0450(9) Uani 1 1 d . . . H28 H 1.1703 0.9579 0.5618 0.054 Uiso 1 1 calc R . . C29 C 1.1651(3) 0.8438(3) 0.5252(3) 0.0492(9) Uani 1 1 d . . . H29 H 1.1834 0.8018 0.5716 0.059 Uiso 1 1 calc R . . C30 C 1.1451(3) 0.8121(3) 0.4622(3) 0.0479(9) Uani 1 1 d . . . H30 H 1.1509 0.7493 0.4674 0.057 Uiso 1 1 calc R . . C31 C 1.1174(3) 0.8708(2) 0.3931(3) 0.0449(9) Uani 1 1 d . . . H31 H 1.1039 0.8489 0.3519 0.054 Uiso 1 1 calc R . . C32 C 1.1103(3) 0.9636(2) 0.3869(2) 0.0365(7) Uani 1 1 d . . . C33 C 1.2182(3) 1.1948(3) 0.1254(3) 0.0466(9) Uani 1 1 d . . . H33A H 1.2529 1.1739 0.1670 0.056 Uiso 1 1 calc R . . H33B H 1.2466 1.2545 0.0792 0.056 Uiso 1 1 calc R . . C34 C 1.2310(3) 1.1265(2) 0.0718(3) 0.0418(8) Uani 1 1 d . . . C35 C 1.2988(3) 1.0408(3) -0.0272(3) 0.0490(9) Uani 1 1 d . . . C36 C 1.3594(3) 0.9981(4) -0.0954(3) 0.0680(13) Uani 1 1 d . . . H36 H 1.4247 1.0190 -0.1373 0.082 Uiso 1 1 calc R . . C37 C 1.3209(4) 0.9233(4) -0.1001(4) 0.0719(14) Uani 1 1 d . . . H37 H 1.3598 0.8938 -0.1468 0.086 Uiso 1 1 calc R . . C38 C 1.2235(4) 0.8916(3) -0.0350(3) 0.0620(12) Uani 1 1 d . . . H38 H 1.1994 0.8400 -0.0383 0.074 Uiso 1 1 calc R . . C39 C 1.1623(3) 0.9339(3) 0.0335(3) 0.0466(9) Uani 1 1 d . . . H39 H 1.0974 0.9124 0.0763 0.056 Uiso 1 1 calc R . . C40 C 1.2012(3) 1.0101(2) 0.0364(3) 0.0405(8) Uani 1 1 d . . . C41 C 1.0649(3) 1.2826(2) 0.1369(3) 0.0485(9) Uani 1 1 d . . . H41A H 1.0939 1.2901 0.0675 0.058 Uiso 1 1 calc R . . H41B H 1.0763 1.3395 0.1460 0.058 Uiso 1 1 calc R . . C42 C 0.9558(3) 1.2612(2) 0.1820(3) 0.0425(8) Uani 1 1 d . . . C43 C 0.7937(3) 1.2741(3) 0.2289(3) 0.0554(10) Uani 1 1 d . . . C44 C 0.6966(4) 1.3017(4) 0.2509(4) 0.0762(15) Uani 1 1 d . . . H44 H 0.6809 1.3640 0.2341 0.091 Uiso 1 1 calc R . . C45 C 0.6258(4) 1.2349(4) 0.2975(4) 0.0807(16) Uani 1 1 d . . . H45 H 0.5596 1.2518 0.3135 0.097 Uiso 1 1 calc R . . C46 C 0.6473(3) 1.1419(4) 0.3227(4) 0.0677(13) Uani 1 1 d . . . H46 H 0.5954 1.0982 0.3546 0.081 Uiso 1 1 calc R . . C47 C 0.7441(3) 1.1121(3) 0.3016(3) 0.0514(10) Uani 1 1 d . . . H47 H 0.7585 1.0494 0.3188 0.062 Uiso 1 1 calc R . . C48 C 0.8189(3) 1.1805(3) 0.2531(3) 0.0440(8) Uani 1 1 d . . . C49 C 0.8447(3) 0.8469(2) 0.3507(2) 0.0348(7) Uani 1 1 d . . . C50 C 0.9173(3) 0.9118(2) 0.3225(2) 0.0345(7) Uani 1 1 d . . . H50 H 0.9453 0.9088 0.3650 0.041 Uiso 1 1 calc R . . C51 C 0.8055(3) 0.8510(2) 0.2855(3) 0.0431(8) Uani 1 1 d . . . H51 H 0.7568 0.8081 0.3019 0.052 Uiso 1 1 calc R . . C52 C 0.8387(3) 0.9186(3) 0.1966(3) 0.0506(10) Uani 1 1 d . . . H52 H 0.8133 0.9216 0.1521 0.061 Uiso 1 1 calc R . . C53 C 0.9101(3) 0.9817(2) 0.1748(3) 0.0438(9) Uani 1 1 d . . . H53 H 0.9321 1.0279 0.1151 0.053 Uiso 1 1 calc R . . C54 C 0.8101(3) 0.7757(2) 0.4497(2) 0.0343(7) Uani 1 1 d . . . Cl1 Cl 0.96248(11) 0.74142(8) 0.08263(9) 0.0719(3) Uani 1 1 d . . . N1 N 0.6334(2) 0.5148(2) 0.7271(2) 0.0482(8) Uani 1 1 d . . . N2 N 0.6266(2) 0.7034(2) 0.6820(2) 0.0478(8) Uani 1 1 d . . . N3 N 0.5712(3) 0.7119(3) 0.8319(3) 0.0676(10) Uani 1 1 d . . . H3 H 0.5496 0.6948 0.8943 0.081 Uiso 1 1 calc R . . N4 N 0.7915(2) 0.53287(19) 0.5549(2) 0.0392(7) Uani 1 1 d . . . N5 N 0.8669(2) 0.4068(2) 0.6052(2) 0.0461(8) Uani 1 1 d . . . H5A H 0.8802 0.3592 0.6443 0.055 Uiso 1 1 calc R . . N6 N 0.5534(2) 0.5827(2) 0.5941(2) 0.0491(8) Uani 1 1 d . . . N7 N 0.4301(3) 0.4785(3) 0.6704(3) 0.0682(11) Uani 1 1 d . . . H7A H 0.3944 0.4300 0.7117 0.082 Uiso 1 1 calc R . . N8 N 1.1098(2) 1.20415(18) 0.1859(2) 0.0380(7) Uani 1 1 d . . . N9 N 1.0888(2) 1.03964(19) 0.3220(2) 0.0371(6) Uani 1 1 d . . . N10 N 1.1261(2) 1.09125(18) 0.4184(2) 0.0366(6) Uani 1 1 d . . . H10 H 1.1364 1.1296 0.4429 0.044 Uiso 1 1 calc R . . N11 N 1.1605(2) 1.06630(19) 0.0982(2) 0.0373(6) Uani 1 1 d . . . N12 N 1.3151(2) 1.1152(2) -0.0035(2) 0.0510(8) Uani 1 1 d . . . H12A H 1.3691 1.1482 -0.0318 0.061 Uiso 1 1 calc R . . N13 N 0.9222(2) 1.1749(2) 0.2226(2) 0.0398(7) Uani 1 1 d . . . N14 N 0.8837(3) 1.3227(2) 0.1841(3) 0.0557(9) Uani 1 1 d . . . H14A H 0.8915 1.3820 0.1616 0.067 Uiso 1 1 calc R . . N15 N 0.9494(2) 0.97864(18) 0.2372(2) 0.0368(6) Uani 1 1 d . . . O1 O 0.74122(19) 0.72156(15) 0.46892(17) 0.0432(6) Uani 1 1 d . . . O2 O 0.84901(19) 0.77441(16) 0.50440(17) 0.0408(6) Uani 1 1 d . . . O3 O 0.9862(4) 0.7490(3) 0.1551(3) 0.1116(15) Uani 1 1 d . . . O4 O 0.8646(5) 0.7172(6) 0.1206(6) 0.223(4) Uani 1 1 d . . . O5 O 0.9768(5) 0.8260(3) 0.0127(4) 0.141(2) Uani 1 1 d . . . O6 O 1.0172(6) 0.6752(4) 0.0404(5) 0.174(3) Uani 1 1 d . . . Cl2 Cl 0.5964(3) 0.1680(3) 0.8451(3) 0.0654(10) Uani 0.62 1 d PD A 1 O7 O 0.5388(9) 0.1868(7) 0.7884(7) 0.155(4) Uani 0.62 1 d PD A 1 O8 O 0.6681(6) 0.2344(6) 0.8024(9) 0.130(4) Uani 0.62 1 d PD A 1 O9 O 0.5251(6) 0.1725(8) 0.9365(5) 0.124(3) Uani 0.62 1 d PD A 1 O10 O 0.6331(8) 0.0799(5) 0.8495(9) 0.130(4) Uani 0.62 1 d PD A 1 Cl2' Cl 0.5910(8) 0.1835(8) 0.8467(8) 0.151(5) Uani 0.38 1 d PD B 2 O7' O 0.6590(11) 0.2083(12) 0.8715(12) 0.137(6) Uani 0.38 1 d PD B 2 O9' O 0.5004(8) 0.2227(9) 0.8833(12) 0.123(5) Uani 0.38 1 d PD B 2 O8' O 0.6308(14) 0.2114(14) 0.7457(8) 0.166(7) Uani 0.38 1 d PD B 2 O10' O 0.5790(13) 0.0870(8) 0.8829(16) 0.154(9) Uani 0.38 1 d PD B 2 Cl3 Cl 0.2679(8) 0.4731(8) 0.0276(9) 0.204(6) Uani 0.53 1 d PD C 1 O11 O 0.2565(16) 0.4088(15) 0.1167(10) 0.100(6) Uani 0.53 1 d PD C 1 O12 O 0.3527(12) 0.5274(12) -0.0127(14) 0.191(6) Uani 0.53 1 d PD C 1 O13 O 0.1790(11) 0.5155(12) 0.0395(13) 0.197(8) Uani 0.53 1 d PD C 1 O14 O 0.2881(16) 0.4217(11) -0.0367(9) 0.170(6) Uani 0.53 1 d PD C 1 Cl3' Cl 0.2776(5) 0.4724(4) 0.0254(3) 0.097(3) Uani 0.47 1 d PD D 2 O11' O 0.2273(17) 0.4227(16) 0.1240(9) 0.109(7) Uani 0.47 1 d PD D 2 O12' O 0.2923(15) 0.5614(9) 0.0225(16) 0.191(6) Uani 0.47 1 d PD D 2 O13' O 0.3683(12) 0.4274(14) -0.0116(13) 0.205(8) Uani 0.47 1 d PD D 2 O14' O 0.2167(18) 0.4729(17) -0.0188(16) 0.202(9) Uani 0.47 1 d PD D 2 O15 O 0.8804(3) 0.2589(2) 0.7553(3) 0.0821(11) Uani 1 1 d . . . H15A H 0.8295 0.2278 0.7942 0.123 Uiso 1 1 d R . . H15B H 0.9254 0.2360 0.7711 0.123 Uiso 1 1 d R . . O16 O 0.4293(5) 0.6643(5) 0.0267(4) 0.169(2) Uani 1 1 d . . . H16A H 0.4284 0.7113 0.0414 0.254 Uiso 1 1 d R . . H16B H 0.3779 0.6445 0.0318 0.254 Uiso 1 1 d R . . O17 O 0.6530(6) 0.7027(5) 0.2214(6) 0.135(3) Uani 0.67 1 d P E 1 H17C H 0.6096 0.7375 0.2121 0.203 Uiso 0.67 1 d PR E 1 H17D H 0.7126 0.7147 0.1870 0.203 Uiso 0.67 1 d PR E 1 O18 O 0.6969(17) 0.6543(14) 0.1456(16) 0.167(7) Uani 0.33 1 d P F 2 H18A H 0.7175 0.6197 0.1112 0.250 Uiso 0.33 1 d PR F 2 H18B H 0.7500 0.6733 0.1374 0.250 Uiso 0.33 1 d PR F 2 O19 O 0.1488(11) 0.4933(8) 0.8576(10) 0.115(4) Uani 0.40 1 d P G 2 H19A H 0.1760 0.4847 0.8942 0.173 Uiso 0.40 1 d PR G 2 H19B H 0.1074 0.4510 0.8823 0.173 Uiso 0.40 1 d PR G 2 O20 O 0.0624(11) 0.4967(6) 0.9180(9) 0.175(5) Uani 0.60 1 d P H 1 H20A H 0.0363 0.4473 0.9295 0.262 Uiso 0.60 1 d PR H 1 H20B H 0.1082 0.4860 0.9348 0.262 Uiso 0.60 1 d PR H 1 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 0.0317(3) 0.0341(2) 0.0373(2) -0.00722(17) -0.01216(19) -0.00695(17) Cu2 0.0353(3) 0.0346(2) 0.0406(3) -0.00175(17) -0.0170(2) -0.00773(18) C1 0.063(3) 0.066(3) 0.044(2) -0.001(2) -0.013(2) -0.007(2) C2 0.034(2) 0.069(3) 0.054(2) -0.023(2) -0.0140(19) 0.0049(19) C3 0.042(3) 0.073(3) 0.088(3) -0.039(3) -0.027(2) 0.010(2) C4 0.056(3) 0.096(4) 0.110(5) -0.060(4) -0.029(3) 0.021(3) C5 0.052(3) 0.077(4) 0.145(6) -0.061(4) -0.025(4) 0.010(3) C6 0.042(3) 0.058(3) 0.106(4) -0.023(3) 0.008(3) 0.004(2) C7 0.040(2) 0.049(2) 0.089(3) -0.018(2) -0.009(2) 0.0025(19) C8 0.031(2) 0.060(2) 0.070(3) -0.026(2) -0.015(2) 0.0025(18) C9 0.052(3) 0.050(2) 0.044(2) -0.0001(17) -0.0238(19) -0.0074(18) C10 0.041(2) 0.0383(18) 0.051(2) -0.0024(16) -0.0265(18) -0.0094(16) C11 0.0327(19) 0.0352(16) 0.051(2) -0.0080(15) -0.0207(17) -0.0057(14) C12 0.045(2) 0.0409(18) 0.049(2) -0.0049(16) -0.0243(19) -0.0024(16) C13 0.054(3) 0.050(2) 0.050(2) -0.0110(18) -0.020(2) -0.0066(19) C14 0.045(2) 0.051(2) 0.069(3) -0.027(2) -0.019(2) -0.0001(18) C15 0.041(2) 0.0370(18) 0.080(3) -0.0196(19) -0.032(2) 0.0022(16) C16 0.042(2) 0.0362(17) 0.059(2) -0.0074(16) -0.0318(19) -0.0064(16) C17 0.051(3) 0.049(2) 0.066(3) 0.0030(19) -0.021(2) -0.0220(19) C18 0.037(2) 0.049(2) 0.065(3) -0.0108(19) -0.020(2) -0.0115(17) C19 0.046(3) 0.067(3) 0.102(4) -0.041(3) -0.041(3) 0.004(2) C20 0.070(4) 0.090(4) 0.172(6) -0.059(4) -0.083(4) 0.018(3) C21 0.104(5) 0.109(5) 0.199(8) -0.090(6) -0.118(6) 0.043(4) C22 0.115(5) 0.088(4) 0.128(5) -0.047(4) -0.095(5) 0.039(4) C23 0.085(4) 0.076(3) 0.084(3) -0.026(3) -0.057(3) 0.014(3) C24 0.052(3) 0.061(2) 0.066(3) -0.030(2) -0.034(2) 0.010(2) C25 0.051(2) 0.0334(17) 0.049(2) -0.0127(15) -0.0270(18) -0.0008(15) C26 0.0354(19) 0.0402(17) 0.0391(18) -0.0143(14) -0.0161(16) -0.0014(15) C27 0.0294(18) 0.0443(18) 0.0396(18) -0.0150(15) -0.0144(15) 0.0011(14) C28 0.049(2) 0.050(2) 0.0397(19) -0.0138(16) -0.0217(18) -0.0005(17) C29 0.046(2) 0.049(2) 0.048(2) -0.0081(17) -0.0221(19) 0.0041(17) C30 0.046(2) 0.0369(18) 0.062(2) -0.0118(17) -0.026(2) 0.0013(16) C31 0.043(2) 0.0416(19) 0.056(2) -0.0192(17) -0.0232(19) 0.0011(16) C32 0.0313(19) 0.0403(17) 0.0394(18) -0.0137(14) -0.0148(15) -0.0007(14) C33 0.037(2) 0.049(2) 0.052(2) -0.0137(17) -0.0155(18) -0.0084(16) C34 0.032(2) 0.0452(19) 0.0418(19) -0.0061(15) -0.0136(17) -0.0040(15) C35 0.037(2) 0.061(2) 0.049(2) -0.0205(18) -0.0156(18) 0.0005(18) C36 0.038(2) 0.101(4) 0.064(3) -0.040(3) -0.010(2) 0.002(2) C37 0.052(3) 0.097(4) 0.079(3) -0.056(3) -0.022(3) 0.016(3) C38 0.066(3) 0.066(3) 0.073(3) -0.040(2) -0.036(3) 0.015(2) C39 0.046(2) 0.049(2) 0.047(2) -0.0154(17) -0.0230(19) 0.0030(17) C40 0.036(2) 0.0476(19) 0.0385(19) -0.0114(15) -0.0186(17) 0.0056(16) C41 0.053(2) 0.0399(19) 0.052(2) -0.0045(16) -0.026(2) -0.0081(17) C42 0.047(2) 0.0394(18) 0.044(2) -0.0102(15) -0.0237(18) -0.0012(16) C43 0.054(3) 0.059(2) 0.067(3) -0.027(2) -0.034(2) 0.013(2) C44 0.062(3) 0.078(3) 0.113(4) -0.049(3) -0.053(3) 0.032(3) C45 0.040(3) 0.111(4) 0.113(4) -0.064(4) -0.036(3) 0.021(3) C46 0.036(2) 0.101(4) 0.076(3) -0.042(3) -0.021(2) 0.000(2) C47 0.040(2) 0.068(3) 0.048(2) -0.0224(19) -0.0167(19) -0.0037(19) C48 0.038(2) 0.056(2) 0.043(2) -0.0182(17) -0.0193(17) 0.0030(17) C49 0.0356(19) 0.0304(15) 0.0358(17) -0.0059(13) -0.0144(15) -0.0046(14) C50 0.0332(19) 0.0340(16) 0.0361(17) -0.0088(13) -0.0150(15) -0.0021(14) C51 0.048(2) 0.0405(18) 0.044(2) -0.0068(15) -0.0229(18) -0.0128(16) C52 0.061(3) 0.054(2) 0.044(2) -0.0077(17) -0.030(2) -0.0129(19) C53 0.048(2) 0.0421(19) 0.0362(19) -0.0032(15) -0.0176(17) -0.0074(16) C54 0.0350(19) 0.0290(15) 0.0407(18) -0.0097(13) -0.0184(16) 0.0014(14) Cl1 0.0928(10) 0.0592(6) 0.0698(7) -0.0127(5) -0.0419(7) -0.0086(6) N1 0.0440(19) 0.0489(17) 0.0436(17) -0.0017(14) -0.0166(15) -0.0122(14) N2 0.0387(18) 0.0507(18) 0.0500(19) -0.0142(15) -0.0152(15) -0.0020(14) N3 0.058(2) 0.091(3) 0.056(2) -0.034(2) -0.0214(19) 0.016(2) N4 0.0382(17) 0.0378(14) 0.0412(16) 0.0004(12) -0.0234(14) -0.0055(12) N5 0.047(2) 0.0348(15) 0.057(2) 0.0013(14) -0.0317(17) -0.0066(14) N6 0.0375(18) 0.0536(18) 0.060(2) -0.0104(15) -0.0266(16) -0.0077(14) N7 0.045(2) 0.060(2) 0.099(3) -0.015(2) -0.031(2) -0.0172(17) N8 0.0365(17) 0.0349(14) 0.0400(16) -0.0084(12) -0.0144(14) -0.0051(12) N9 0.0376(17) 0.0365(14) 0.0403(15) -0.0113(12) -0.0190(14) -0.0012(12) N10 0.0392(17) 0.0368(14) 0.0405(15) -0.0148(12) -0.0199(14) -0.0014(12) N11 0.0329(16) 0.0405(15) 0.0342(15) -0.0081(12) -0.0117(13) -0.0035(12) N12 0.0279(17) 0.070(2) 0.0488(18) -0.0184(16) -0.0084(15) -0.0079(15) N13 0.0353(17) 0.0418(15) 0.0421(16) -0.0099(13) -0.0176(14) -0.0012(13) N14 0.064(2) 0.0396(17) 0.076(2) -0.0166(16) -0.044(2) 0.0098(16) N15 0.0367(16) 0.0338(14) 0.0357(15) -0.0067(11) -0.0128(13) -0.0051(12) O1 0.0469(15) 0.0372(12) 0.0421(13) 0.0015(10) -0.0215(12) -0.0133(11) O2 0.0455(15) 0.0376(12) 0.0433(13) -0.0078(10) -0.0251(12) -0.0006(11) O3 0.166(5) 0.105(3) 0.102(3) -0.032(3) -0.095(3) 0.024(3) O4 0.108(5) 0.285(9) 0.258(8) -0.121(8) -0.007(5) -0.105(6) O5 0.224(6) 0.095(3) 0.108(3) 0.023(3) -0.105(4) -0.020(3) O6 0.265(8) 0.154(5) 0.166(5) -0.109(5) -0.130(5) 0.101(5) Cl2 0.068(2) 0.0628(16) 0.065(2) -0.0176(16) -0.0269(18) -0.0101(14) O7 0.148(9) 0.168(9) 0.157(10) -0.003(8) -0.101(9) -0.009(8) O8 0.085(6) 0.104(6) 0.167(11) -0.037(7) -0.015(7) -0.040(5) O9 0.107(7) 0.169(10) 0.105(6) -0.046(7) -0.044(6) -0.021(7) O10 0.157(12) 0.106(7) 0.140(9) -0.040(6) -0.078(9) 0.024(6) Cl2' 0.157(12) 0.127(8) 0.156(11) 0.029(6) -0.097(10) -0.026(7) O7' 0.127(13) 0.173(17) 0.148(15) -0.051(13) -0.077(13) -0.038(10) O9' 0.084(10) 0.094(9) 0.154(15) -0.037(10) -0.017(9) -0.004(7) O8' 0.19(2) 0.180(18) 0.120(14) -0.028(13) -0.078(15) 0.047(16) O10' 0.15(2) 0.135(17) 0.17(2) -0.020(15) -0.075(18) -0.024(13) Cl3 0.186(11) 0.229(13) 0.248(13) -0.035(11) -0.144(12) -0.065(10) O11 0.095(10) 0.110(10) 0.096(11) -0.022(8) -0.042(7) -0.016(7) O12 0.175(16) 0.149(12) 0.206(15) -0.039(8) -0.041(13) -0.044(11) O13 0.193(18) 0.169(14) 0.202(18) -0.052(12) -0.076(14) 0.055(13) O14 0.204(19) 0.179(14) 0.111(9) -0.047(9) -0.051(11) 0.006(13) Cl3' 0.087(4) 0.102(4) 0.073(3) 0.043(3) -0.041(3) -0.068(3) O11' 0.108(15) 0.106(12) 0.094(11) -0.017(9) -0.028(8) -0.028(10) O12' 0.175(16) 0.149(12) 0.206(15) -0.039(8) -0.041(13) -0.044(11) O13' 0.19(2) 0.23(2) 0.156(14) -0.013(13) -0.059(14) -0.002(16) O14' 0.21(3) 0.23(3) 0.20(2) -0.051(17) -0.12(2) -0.013(18) O15 0.097(3) 0.070(2) 0.080(2) 0.0089(17) -0.057(2) -0.0071(19) O16 0.201(7) 0.159(5) 0.124(4) -0.046(4) -0.040(4) -0.018(5) O17 0.121(6) 0.105(5) 0.134(6) -0.007(5) -0.028(5) -0.023(5) O18 0.174(19) 0.154(17) 0.163(17) -0.022(14) -0.075(15) -0.020(14) O19 0.133(11) 0.071(6) 0.146(11) -0.008(7) -0.079(9) -0.006(7) O20 0.212(13) 0.079(6) 0.191(11) -0.028(7) -0.057(10) -0.005(8) _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 N15 1.981(3) . ? Cu1 N13 2.009(3) . ? Cu1 N11 2.013(3) . ? Cu1 N8 2.114(3) . ? Cu1 N9 2.175(3) . ? Cu2 O1 1.931(2) . ? Cu2 N4 1.992(3) . ? Cu2 N2 1.998(3) . ? Cu2 N6 2.140(3) . ? Cu2 N1 2.147(3) . ? C1 C2 1.471(6) . ? C1 N1 1.492(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.312(5) . ? C2 N3 1.360(5) . ? C3 N3 1.381(6) . ? C3 C8 1.383(6) . ? C3 C4 1.410(7) . ? C4 C5 1.364(9) . ? C4 H4 0.9300 . ? C5 C6 1.365(9) . ? C5 H5 0.9300 . ? C6 C7 1.360(7) . ? C6 H6 0.9300 . ? C7 C8 1.389(6) . ? C7 H7 0.9300 . ? C8 N2 1.390(5) . ? C9 N1 1.483(5) . ? C9 C10 1.492(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.324(4) . ? C10 N5 1.329(5) . ? C11 N4 1.384(5) . ? C11 C12 1.401(5) . ? C11 C16 1.402(5) . ? C12 C13 1.383(6) . ? C12 H12 0.9300 . ? C13 C14 1.388(6) . ? C13 H13 0.9300 . ? C14 C15 1.372(6) . ? C14 H14 0.9300 . ? C15 C16 1.388(6) . ? C15 H15 0.9300 . ? C16 N5 1.383(5) . ? C17 N1 1.487(5) . ? C17 C18 1.490(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.312(5) . ? C18 N7 1.348(5) . ? C19 N7 1.363(6) . ? C19 C20 1.393(7) . ? C19 C24 1.400(6) . ? C20 C21 1.354(10) . ? C20 H20 0.9300 . ? C21 C22 1.368(10) . ? C21 H21 0.9300 . ? C22 C23 1.406(7) . ? C22 H22 0.9300 . ? C23 C24 1.393(6) . ? C23 H23 0.9300 . ? C24 N6 1.391(5) . ? C25 N8 1.486(4) . ? C25 C26 1.501(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N9 1.319(4) . ? C26 N10 1.343(4) . ? C27 C28 1.374(5) . ? C27 N10 1.385(4) . ? C27 C32 1.401(5) . ? C28 C29 1.378(5) . ? C28 H28 0.9300 . ? C29 C30 1.397(6) . ? C29 H29 0.9300 . ? C30 C31 1.368(5) . ? C30 H30 0.9300 . ? C31 C32 1.379(5) . ? C31 H31 0.9300 . ? C32 N9 1.398(4) . ? C33 N8 1.492(5) . ? C33 C34 1.494(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N11 1.314(4) . ? C34 N12 1.343(5) . ? C35 C36 1.367(6) . ? C35 N12 1.383(5) . ? C35 C40 1.391(5) . ? C36 C37 1.375(7) . ? C36 H36 0.9300 . ? C37 C38 1.396(7) . ? C37 H37 0.9300 . ? C38 C39 1.369(6) . ? C38 H38 0.9300 . ? C39 C40 1.383(5) . ? C39 H39 0.9300 . ? C40 N11 1.402(4) . ? C41 N8 1.469(5) . ? C41 C42 1.493(5) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N13 1.316(4) . ? C42 N14 1.332(5) . ? C43 C44 1.377(6) . ? C43 N14 1.388(6) . ? C43 C48 1.401(6) . ? C44 C45 1.340(8) . ? C44 H44 0.9300 . ? C45 C46 1.380(8) . ? C45 H45 0.9300 . ? C46 C47 1.384(6) . ? C46 H46 0.9300 . ? C47 C48 1.394(6) . ? C47 H47 0.9300 . ? C48 N13 1.398(5) . ? C49 C50 1.382(4) . ? C49 C51 1.386(5) . ? C49 C54 1.506(4) . ? C50 N15 1.334(4) . ? C50 H50 0.9300 . ? C51 C52 1.377(5) . ? C51 H51 0.9300 . ? C52 C53 1.376(5) . ? C52 H52 0.9300 . ? C53 N15 1.351(4) . ? C53 H53 0.9300 . ? C54 O2 1.240(4) . ? C54 O1 1.267(4) . ? Cl1 O4 1.360(6) . ? Cl1 O6 1.374(5) . ? Cl1 O5 1.374(4) . ? Cl1 O3 1.394(4) . ? N3 H3 0.8600 . ? N5 H5A 0.8600 . ? N7 H7A 0.8600 . ? N10 H10 0.8600 . ? N12 H12A 0.8600 . ? N14 H14A 0.8600 . ? Cl2 O8 1.349(6) . ? Cl2 O10 1.376(7) . ? Cl2 O9 1.396(6) . ? Cl2 O7 1.451(8) . ? Cl2' O9' 1.361(8) . ? Cl2' O7' 1.371(9) . ? Cl2' O8' 1.386(9) . ? Cl2' O10' 1.398(8) . ? Cl3 O13 1.363(9) . ? Cl3 O12 1.380(8) . ? Cl3 O14 1.396(9) . ? Cl3 O11 1.398(9) . ? Cl3' O14' 1.376(9) . ? Cl3' O12' 1.384(8) . ? Cl3' O11' 1.397(8) . ? Cl3' O13' 1.406(9) . ? O15 H15A 0.8199 . ? O15 H15B 0.8201 . ? O16 H16A 0.8201 . ? O16 H16B 0.8200 . ? O17 H17C 0.8200 . ? O17 H17D 0.8200 . ? O18 H18A 0.8200 . ? O18 H18B 0.8201 . ? O19 H19A 0.8200 . ? O19 H19B 0.8199 . ? O20 H20A 0.8200 . ? O20 H20B 0.8201 . ? 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 N15 Cu1 N13 93.81(12) . . ? N15 Cu1 N11 101.94(11) . . ? N13 Cu1 N11 134.50(11) . . ? N15 Cu1 N8 174.10(12) . . ? N13 Cu1 N8 80.42(12) . . ? N11 Cu1 N8 83.13(11) . . ? N15 Cu1 N9 104.60(11) . . ? N13 Cu1 N9 119.59(11) . . ? N11 Cu1 N9 97.41(11) . . ? N8 Cu1 N9 77.50(11) . . ? O1 Cu2 N4 96.41(11) . . ? O1 Cu2 N2 99.41(12) . . ? N4 Cu2 N2 142.88(12) . . ? O1 Cu2 N6 102.92(11) . . ? N4 Cu2 N6 108.76(12) . . ? N2 Cu2 N6 100.11(13) . . ? O1 Cu2 N1 176.49(12) . . ? N4 Cu2 N1 80.52(12) . . ? N2 Cu2 N1 82.24(13) . . ? N6 Cu2 N1 79.76(12) . . ? C2 C1 N1 109.5(3) . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1B 109.8 . . ? N1 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? N2 C2 N3 111.4(4) . . ? N2 C2 C1 122.6(4) . . ? N3 C2 C1 125.8(4) . . ? N3 C3 C8 106.6(4) . . ? N3 C3 C4 132.0(5) . . ? C8 C3 C4 121.5(5) . . ? C5 C4 C3 115.9(6) . . ? C5 C4 H4 122.1 . . ? C3 C4 H4 122.1 . . ? C4 C5 C6 122.8(5) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C7 C6 C5 121.5(6) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 118.2(5) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? C3 C8 C7 119.9(4) . . ? C3 C8 N2 108.0(4) . . ? C7 C8 N2 131.9(4) . . ? N1 C9 C10 107.1(3) . . ? N1 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? N1 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? N4 C10 N5 112.6(3) . . ? N4 C10 C9 120.3(3) . . ? N5 C10 C9 127.1(3) . . ? N4 C11 C12 131.4(3) . . ? N4 C11 C16 108.8(3) . . ? C12 C11 C16 119.8(4) . . ? C13 C12 C11 117.5(4) . . ? C13 C12 H12 121.3 . . ? C11 C12 H12 121.3 . . ? C12 C13 C14 122.0(4) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C15 C14 C13 121.2(4) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 117.7(4) . . ? C14 C15 H15 121.2 . . ? C16 C15 H15 121.2 . . ? N5 C16 C15 133.1(3) . . ? N5 C16 C11 105.0(3) . . ? C15 C16 C11 121.9(4) . . ? N1 C17 C18 108.9(3) . . ? N1 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? N1 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? N6 C18 N7 112.7(4) . . ? N6 C18 C17 121.9(3) . . ? N7 C18 C17 125.3(4) . . ? N7 C19 C20 132.5(5) . . ? N7 C19 C24 106.3(4) . . ? C20 C19 C24 121.2(5) . . ? C21 C20 C19 116.9(6) . . ? C21 C20 H20 121.6 . . ? C19 C20 H20 121.6 . . ? C20 C21 C22 122.5(5) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C21 C22 C23 122.9(6) . . ? C21 C22 H22 118.6 . . ? C23 C22 H22 118.6 . . ? C24 C23 C22 114.5(5) . . ? C24 C23 H23 122.7 . . ? C22 C23 H23 122.7 . . ? N6 C24 C23 129.9(4) . . ? N6 C24 C19 108.1(4) . . ? C23 C24 C19 122.0(4) . . ? N8 C25 C26 107.6(3) . . ? N8 C25 H25A 110.2 . . ? C26 C25 H25A 110.2 . . ? N8 C25 H25B 110.2 . . ? C26 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? N9 C26 N10 113.6(3) . . ? N9 C26 C25 120.7(3) . . ? N10 C26 C25 125.7(3) . . ? C28 C27 N10 132.2(3) . . ? C28 C27 C32 121.9(3) . . ? N10 C27 C32 105.8(3) . . ? C27 C28 C29 117.2(3) . . ? C27 C28 H28 121.4 . . ? C29 C28 H28 121.4 . . ? C28 C29 C30 120.8(4) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 122.0(3) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 117.6(3) . . ? C30 C31 H31 121.2 . . ? C32 C31 H31 121.2 . . ? C31 C32 N9 130.7(3) . . ? C31 C32 C27 120.5(3) . . ? N9 C32 C27 108.7(3) . . ? N8 C33 C34 109.4(3) . . ? N8 C33 H33A 109.8 . . ? C34 C33 H33A 109.8 . . ? N8 C33 H33B 109.8 . . ? C34 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? N11 C34 N12 112.3(3) . . ? N11 C34 C33 122.4(3) . . ? N12 C34 C33 125.2(3) . . ? C36 C35 N12 131.9(4) . . ? C36 C35 C40 121.7(4) . . ? N12 C35 C40 106.4(3) . . ? C35 C36 C37 118.0(4) . . ? C35 C36 H36 121.0 . . ? C37 C36 H36 121.0 . . ? C36 C37 C38 120.2(4) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C39 C38 C37 122.2(4) . . ? C39 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? C38 C39 C40 117.1(4) . . ? C38 C39 H39 121.5 . . ? C40 C39 H39 121.5 . . ? C39 C40 C35 120.8(4) . . ? C39 C40 N11 131.5(3) . . ? C35 C40 N11 107.7(3) . . ? N8 C41 C42 106.8(3) . . ? N8 C41 H41A 110.4 . . ? C42 C41 H41A 110.4 . . ? N8 C41 H41B 110.4 . . ? C42 C41 H41B 110.4 . . ? H41A C41 H41B 108.6 . . ? N13 C42 N14 113.1(3) . . ? N13 C42 C41 120.7(3) . . ? N14 C42 C41 126.2(3) . . ? C44 C43 N14 132.8(4) . . ? C44 C43 C48 122.3(4) . . ? N14 C43 C48 104.9(4) . . ? C45 C44 C43 117.1(5) . . ? C45 C44 H44 121.4 . . ? C43 C44 H44 121.4 . . ? C44 C45 C46 122.5(5) . . ? C44 C45 H45 118.8 . . ? C46 C45 H45 118.8 . . ? C45 C46 C47 121.7(5) . . ? C45 C46 H46 119.2 . . ? C47 C46 H46 119.2 . . ? C46 C47 C48 116.7(4) . . ? C46 C47 H47 121.6 . . ? C48 C47 H47 121.6 . . ? C47 C48 N13 131.5(4) . . ? C47 C48 C43 119.7(4) . . ? N13 C48 C43 108.8(3) . . ? C50 C49 C51 117.7(3) . . ? C50 C49 C54 119.8(3) . . ? C51 C49 C54 122.5(3) . . ? N15 C50 C49 123.1(3) . . ? N15 C50 H50 118.4 . . ? C49 C50 H50 118.4 . . ? C52 C51 C49 120.0(3) . . ? C52 C51 H51 120.0 . . ? C49 C51 H51 120.0 . . ? C53 C52 C51 118.7(3) . . ? C53 C52 H52 120.7 . . ? C51 C52 H52 120.7 . . ? N15 C53 C52 122.2(3) . . ? N15 C53 H53 118.9 . . ? C52 C53 H53 118.9 . . ? O2 C54 O1 126.0(3) . . ? O2 C54 C49 119.6(3) . . ? O1 C54 C49 114.4(3) . . ? O4 Cl1 O6 107.1(5) . . ? O4 Cl1 O5 107.1(5) . . ? O6 Cl1 O5 110.1(4) . . ? O4 Cl1 O3 110.5(4) . . ? O6 Cl1 O3 112.4(3) . . ? O5 Cl1 O3 109.5(3) . . ? C9 N1 C17 109.3(3) . . ? C9 N1 C1 112.7(3) . . ? C17 N1 C1 111.8(3) . . ? C9 N1 Cu2 105.5(2) . . ? C17 N1 Cu2 108.1(2) . . ? C1 N1 Cu2 109.3(2) . . ? C2 N2 C8 106.9(3) . . ? C2 N2 Cu2 113.5(3) . . ? C8 N2 Cu2 138.7(3) . . ? C2 N3 C3 106.9(4) . . ? C2 N3 H3 126.5 . . ? C3 N3 H3 126.5 . . ? C10 N4 C11 105.6(3) . . ? C10 N4 Cu2 113.3(3) . . ? C11 N4 Cu2 141.1(2) . . ? C10 N5 C16 107.9(3) . . ? C10 N5 H5A 126.0 . . ? C16 N5 H5A 126.0 . . ? C18 N6 C24 105.7(3) . . ? C18 N6 Cu2 111.1(3) . . ? C24 N6 Cu2 143.1(3) . . ? C18 N7 C19 107.2(4) . . ? C18 N7 H7A 126.4 . . ? C19 N7 H7A 126.4 . . ? C41 N8 C25 111.3(3) . . ? C41 N8 C33 113.0(3) . . ? C25 N8 C33 111.1(3) . . ? C41 N8 Cu1 106.0(2) . . ? C25 N8 Cu1 106.81(19) . . ? C33 N8 Cu1 108.4(2) . . ? C26 N9 C32 105.0(3) . . ? C26 N9 Cu1 109.3(2) . . ? C32 N9 Cu1 145.5(2) . . ? C26 N10 C27 106.8(3) . . ? C26 N10 H10 126.6 . . ? C27 N10 H10 126.6 . . ? C34 N11 C40 106.4(3) . . ? C34 N11 Cu1 112.5(2) . . ? C40 N11 Cu1 141.2(2) . . ? C34 N12 C35 107.2(3) . . ? C34 N12 H12A 126.4 . . ? C35 N12 H12A 126.4 . . ? C42 N13 C48 105.3(3) . . ? C42 N13 Cu1 111.9(2) . . ? C48 N13 Cu1 142.5(2) . . ? C42 N14 C43 107.9(3) . . ? C42 N14 H14A 126.1 . . ? C43 N14 H14A 126.1 . . ? C50 N15 C53 118.3(3) . . ? C50 N15 Cu1 121.7(2) . . ? C53 N15 Cu1 119.2(2) . . ? C54 O1 Cu2 121.2(2) . . ? O8 Cl2 O10 113.6(6) . . ? O8 Cl2 O9 112.5(6) . . ? O10 Cl2 O9 111.3(6) . . ? O8 Cl2 O7 108.1(6) . . ? O10 Cl2 O7 107.7(6) . . ? O9 Cl2 O7 102.9(6) . . ? O9' Cl2' O7' 113.1(8) . . ? O9' Cl2' O8' 109.7(8) . . ? O7' Cl2' O8' 107.1(8) . . ? O9' Cl2' O10' 109.0(8) . . ? O7' Cl2' O10' 107.9(8) . . ? O8' Cl2' O10' 110.0(8) . . ? O13 Cl3 O12 118.8(12) . . ? O13 Cl3 O14 107.8(11) . . ? O12 Cl3 O14 104.1(11) . . ? O13 Cl3 O11 108.4(11) . . ? O12 Cl3 O11 111.0(11) . . ? O14 Cl3 O11 106.0(11) . . ? O14' Cl3' O12' 110.5(11) . . ? O14' Cl3' O11' 107.4(11) . . ? O12' Cl3' O11' 106.4(11) . . ? O14' Cl3' O13' 113.5(11) . . ? O12' Cl3' O13' 112.0(10) . . ? O11' Cl3' O13' 106.6(10) . . ? H15A O15 H15B 107.7 . . ? H16A O16 H16B 120.3 . . ? H17C O17 H17D 122.2 . . ? H17D O18 H18A 151.5 . . ? H17D O18 H18B 51.6 . . ? H18A O18 H18B 100.0 . . ? H19A O19 H19B 106.0 . . ? H19A O19 H20B 56.7 . . ? H19B O19 H20B 71.6 . . ? H19B O20 H20A 63.6 . . ? H19B O20 H20B 74.6 . . ? H20A O20 H20B 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 20.4(6) . . . . ? N1 C1 C2 N3 -165.6(4) . . . . ? N3 C3 C4 C5 -175.3(5) . . . . ? C8 C3 C4 C5 4.3(7) . . . . ? C3 C4 C5 C6 0.5(8) . . . . ? C4 C5 C6 C7 -3.7(9) . . . . ? C5 C6 C7 C8 1.9(8) . . . . ? N3 C3 C8 C7 173.6(4) . . . . ? C4 C3 C8 C7 -6.1(7) . . . . ? N3 C3 C8 N2 -2.1(5) . . . . ? C4 C3 C8 N2 178.1(4) . . . . ? C6 C7 C8 C3 2.9(7) . . . . ? C6 C7 C8 N2 177.5(4) . . . . ? N1 C9 C10 N4 26.6(4) . . . . ? N1 C9 C10 N5 -154.1(3) . . . . ? N4 C11 C12 C13 -179.2(3) . . . . ? C16 C11 C12 C13 -0.2(5) . . . . ? C11 C12 C13 C14 0.4(6) . . . . ? C12 C13 C14 C15 -0.5(6) . . . . ? C13 C14 C15 C16 0.4(6) . . . . ? C14 C15 C16 N5 179.2(4) . . . . ? C14 C15 C16 C11 -0.2(5) . . . . ? N4 C11 C16 N5 -0.2(4) . . . . ? C12 C11 C16 N5 -179.4(3) . . . . ? N4 C11 C16 C15 179.4(3) . . . . ? C12 C11 C16 C15 0.2(5) . . . . ? N1 C17 C18 N6 27.9(6) . . . . ? N1 C17 C18 N7 -154.2(4) . . . . ? N7 C19 C20 C21 177.9(6) . . . . ? C24 C19 C20 C21 0.2(8) . . . . ? C19 C20 C21 C22 -0.8(10) . . . . ? C20 C21 C22 C23 1.8(10) . . . . ? C21 C22 C23 C24 -2.0(8) . . . . ? C22 C23 C24 N6 -178.4(5) . . . . ? C22 C23 C24 C19 1.4(7) . . . . ? N7 C19 C24 N6 1.0(5) . . . . ? C20 C19 C24 N6 179.2(5) . . . . ? N7 C19 C24 C23 -178.8(4) . . . . ? C20 C19 C24 C23 -0.6(7) . . . . ? N8 C25 C26 N9 -22.6(5) . . . . ? N8 C25 C26 N10 154.1(3) . . . . ? N10 C27 C28 C29 -174.2(4) . . . . ? C32 C27 C28 C29 2.1(6) . . . . ? C27 C28 C29 C30 -0.9(6) . . . . ? C28 C29 C30 C31 -0.4(6) . . . . ? C29 C30 C31 C32 0.5(6) . . . . ? C30 C31 C32 N9 176.6(4) . . . . ? C30 C31 C32 C27 0.8(5) . . . . ? C28 C27 C32 C31 -2.1(6) . . . . ? N10 C27 C32 C31 175.1(3) . . . . ? C28 C27 C32 N9 -178.8(3) . . . . ? N10 C27 C32 N9 -1.6(4) . . . . ? N8 C33 C34 N11 -18.5(5) . . . . ? N8 C33 C34 N12 165.5(3) . . . . ? N12 C35 C36 C37 179.0(5) . . . . ? C40 C35 C36 C37 0.4(7) . . . . ? C35 C36 C37 C38 -1.6(8) . . . . ? C36 C37 C38 C39 1.6(8) . . . . ? C37 C38 C39 C40 -0.4(6) . . . . ? C38 C39 C40 C35 -0.8(5) . . . . ? C38 C39 C40 N11 -177.7(4) . . . . ? C36 C35 C40 C39 0.8(6) . . . . ? N12 C35 C40 C39 -178.1(3) . . . . ? C36 C35 C40 N11 178.4(4) . . . . ? N12 C35 C40 N11 -0.5(4) . . . . ? N8 C41 C42 N13 -25.7(5) . . . . ? N8 C41 C42 N14 156.3(4) . . . . ? N14 C43 C44 C45 -178.5(5) . . . . ? C48 C43 C44 C45 0.3(7) . . . . ? C43 C44 C45 C46 -0.4(8) . . . . ? C44 C45 C46 C47 0.4(9) . . . . ? C45 C46 C47 C48 -0.3(7) . . . . ? C46 C47 C48 N13 178.9(4) . . . . ? C46 C47 C48 C43 0.2(6) . . . . ? C44 C43 C48 C47 -0.2(6) . . . . ? N14 C43 C48 C47 178.9(3) . . . . ? C44 C43 C48 N13 -179.2(4) . . . . ? N14 C43 C48 N13 -0.1(4) . . . . ? C51 C49 C50 N15 1.5(5) . . . . ? C54 C49 C50 N15 -177.9(3) . . . . ? C50 C49 C51 C52 -0.5(6) . . . . ? C54 C49 C51 C52 178.9(3) . . . . ? C49 C51 C52 C53 -0.6(6) . . . . ? C51 C52 C53 N15 0.8(6) . . . . ? C50 C49 C54 O2 -1.7(5) . . . . ? C51 C49 C54 O2 178.8(3) . . . . ? C50 C49 C54 O1 178.0(3) . . . . ? C51 C49 C54 O1 -1.5(5) . . . . ? C10 C9 N1 C17 79.3(4) . . . . ? C10 C9 N1 C1 -155.8(3) . . . . ? C10 C9 N1 Cu2 -36.7(3) . . . . ? C18 C17 N1 C9 -148.1(3) . . . . ? C18 C17 N1 C1 86.5(4) . . . . ? C18 C17 N1 Cu2 -33.8(4) . . . . ? C2 C1 N1 C9 103.6(4) . . . . ? C2 C1 N1 C17 -132.9(4) . . . . ? C2 C1 N1 Cu2 -13.3(4) . . . . ? N4 Cu2 N1 C9 30.7(2) . . . . ? N2 Cu2 N1 C9 -116.3(3) . . . . ? N6 Cu2 N1 C9 141.9(3) . . . . ? N4 Cu2 N1 C17 -86.1(3) . . . . ? N2 Cu2 N1 C17 126.9(3) . . . . ? N6 Cu2 N1 C17 25.1(3) . . . . ? N4 Cu2 N1 C1 152.0(3) . . . . ? N2 Cu2 N1 C1 5.0(3) . . . . ? N6 Cu2 N1 C1 -96.8(3) . . . . ? N3 C2 N2 C8 -2.4(5) . . . . ? C1 C2 N2 C8 172.3(4) . . . . ? N3 C2 N2 Cu2 168.8(3) . . . . ? C1 C2 N2 Cu2 -16.5(5) . . . . ? C3 C8 N2 C2 2.8(5) . . . . ? C7 C8 N2 C2 -172.3(5) . . . . ? C3 C8 N2 Cu2 -165.0(3) . . . . ? C7 C8 N2 Cu2 20.0(7) . . . . ? O1 Cu2 N2 C2 -171.5(3) . . . . ? N4 Cu2 N2 C2 -57.5(4) . . . . ? N6 Cu2 N2 C2 83.5(3) . . . . ? N1 Cu2 N2 C2 5.4(3) . . . . ? O1 Cu2 N2 C8 -4.2(4) . . . . ? N4 Cu2 N2 C8 109.7(4) . . . . ? N6 Cu2 N2 C8 -109.3(4) . . . . ? N1 Cu2 N2 C8 172.6(4) . . . . ? N2 C2 N3 C3 1.1(5) . . . . ? C1 C2 N3 C3 -173.4(4) . . . . ? C8 C3 N3 C2 0.7(5) . . . . ? C4 C3 N3 C2 -179.6(5) . . . . ? N5 C10 N4 C11 -0.8(4) . . . . ? C9 C10 N4 C11 178.6(3) . . . . ? N5 C10 N4 Cu2 -179.2(2) . . . . ? C9 C10 N4 Cu2 0.2(4) . . . . ? C12 C11 N4 C10 179.7(4) . . . . ? C16 C11 N4 C10 0.6(4) . . . . ? C12 C11 N4 Cu2 -2.7(6) . . . . ? C16 C11 N4 Cu2 178.2(3) . . . . ? O1 Cu2 N4 C10 160.6(2) . . . . ? N2 Cu2 N4 C10 45.7(3) . . . . ? N6 Cu2 N4 C10 -93.4(2) . . . . ? N1 Cu2 N4 C10 -17.7(2) . . . . ? O1 Cu2 N4 C11 -16.8(4) . . . . ? N2 Cu2 N4 C11 -131.7(3) . . . . ? N6 Cu2 N4 C11 89.2(4) . . . . ? N1 Cu2 N4 C11 164.9(4) . . . . ? N4 C10 N5 C16 0.7(4) . . . . ? C9 C10 N5 C16 -178.6(3) . . . . ? C15 C16 N5 C10 -179.8(4) . . . . ? C11 C16 N5 C10 -0.3(4) . . . . ? N7 C18 N6 C24 -0.8(5) . . . . ? C17 C18 N6 C24 177.3(4) . . . . ? N7 C18 N6 Cu2 175.9(3) . . . . ? C17 C18 N6 Cu2 -6.0(5) . . . . ? C23 C24 N6 C18 179.6(5) . . . . ? C19 C24 N6 C18 -0.1(5) . . . . ? C23 C24 N6 Cu2 4.8(8) . . . . ? C19 C24 N6 Cu2 -175.0(4) . . . . ? O1 Cu2 N6 C18 166.5(3) . . . . ? N4 Cu2 N6 C18 65.0(3) . . . . ? N2 Cu2 N6 C18 -91.3(3) . . . . ? N1 Cu2 N6 C18 -11.2(3) . . . . ? O1 Cu2 N6 C24 -18.9(5) . . . . ? N4 Cu2 N6 C24 -120.4(5) . . . . ? N2 Cu2 N6 C24 83.3(5) . . . . ? N1 Cu2 N6 C24 163.4(5) . . . . ? N6 C18 N7 C19 1.4(5) . . . . ? C17 C18 N7 C19 -176.6(4) . . . . ? C20 C19 N7 C18 -179.4(6) . . . . ? C24 C19 N7 C18 -1.4(5) . . . . ? C42 C41 N8 C25 -78.0(3) . . . . ? C42 C41 N8 C33 156.3(3) . . . . ? C42 C41 N8 Cu1 37.8(3) . . . . ? C26 C25 N8 C41 157.4(3) . . . . ? C26 C25 N8 C33 -75.8(3) . . . . ? C26 C25 N8 Cu1 42.2(3) . . . . ? C34 C33 N8 C41 -95.4(3) . . . . ? C34 C33 N8 C25 138.8(3) . . . . ? C34 C33 N8 Cu1 21.7(3) . . . . ? N13 Cu1 N8 C41 -32.4(2) . . . . ? N11 Cu1 N8 C41 105.0(2) . . . . ? N9 Cu1 N8 C41 -155.8(2) . . . . ? N13 Cu1 N8 C25 86.3(2) . . . . ? N11 Cu1 N8 C25 -136.3(2) . . . . ? N9 Cu1 N8 C25 -37.1(2) . . . . ? N13 Cu1 N8 C33 -153.9(2) . . . . ? N11 Cu1 N8 C33 -16.5(2) . . . . ? N9 Cu1 N8 C33 82.7(2) . . . . ? N10 C26 N9 C32 -1.7(4) . . . . ? C25 C26 N9 C32 175.4(3) . . . . ? N10 C26 N9 Cu1 174.1(2) . . . . ? C25 C26 N9 Cu1 -8.8(4) . . . . ? C31 C32 N9 C26 -174.2(4) . . . . ? C27 C32 N9 C26 2.0(4) . . . . ? C31 C32 N9 Cu1 12.8(7) . . . . ? C27 C32 N9 Cu1 -171.0(3) . . . . ? N15 Cu1 N9 C26 -148.6(2) . . . . ? N13 Cu1 N9 C26 -45.5(3) . . . . ? N11 Cu1 N9 C26 106.9(2) . . . . ? N8 Cu1 N9 C26 25.7(2) . . . . ? N15 Cu1 N9 C32 24.2(4) . . . . ? N13 Cu1 N9 C32 127.3(4) . . . . ? N11 Cu1 N9 C32 -80.2(4) . . . . ? N8 Cu1 N9 C32 -161.4(4) . . . . ? N9 C26 N10 C27 0.7(4) . . . . ? C25 C26 N10 C27 -176.2(3) . . . . ? C28 C27 N10 C26 177.4(4) . . . . ? C32 C27 N10 C26 0.6(4) . . . . ? N12 C34 N11 C40 0.7(4) . . . . ? C33 C34 N11 C40 -175.8(3) . . . . ? N12 C34 N11 Cu1 -179.2(2) . . . . ? C33 C34 N11 Cu1 4.3(4) . . . . ? C39 C40 N11 C34 177.2(4) . . . . ? C35 C40 N11 C34 -0.1(4) . . . . ? C39 C40 N11 Cu1 -3.0(6) . . . . ? C35 C40 N11 Cu1 179.8(3) . . . . ? N15 Cu1 N11 C34 -175.8(2) . . . . ? N13 Cu1 N11 C34 76.6(3) . . . . ? N8 Cu1 N11 C34 7.3(2) . . . . ? N9 Cu1 N11 C34 -69.1(3) . . . . ? N15 Cu1 N11 C40 4.4(4) . . . . ? N13 Cu1 N11 C40 -103.2(4) . . . . ? N8 Cu1 N11 C40 -172.5(4) . . . . ? N9 Cu1 N11 C40 111.1(4) . . . . ? N11 C34 N12 C35 -1.0(4) . . . . ? C33 C34 N12 C35 175.3(4) . . . . ? C36 C35 N12 C34 -177.8(5) . . . . ? C40 C35 N12 C34 0.9(4) . . . . ? N14 C42 N13 C48 0.6(4) . . . . ? C41 C42 N13 C48 -177.7(3) . . . . ? N14 C42 N13 Cu1 176.1(3) . . . . ? C41 C42 N13 Cu1 -2.2(4) . . . . ? C47 C48 N13 C42 -179.1(4) . . . . ? C43 C48 N13 C42 -0.3(4) . . . . ? C47 C48 N13 Cu1 7.8(7) . . . . ? C43 C48 N13 Cu1 -173.4(3) . . . . ? N15 Cu1 N13 C42 -161.7(2) . . . . ? N11 Cu1 N13 C42 -50.9(3) . . . . ? N8 Cu1 N13 C42 19.5(2) . . . . ? N9 Cu1 N13 C42 89.1(3) . . . . ? N15 Cu1 N13 C48 11.1(4) . . . . ? N11 Cu1 N13 C48 122.0(4) . . . . ? N8 Cu1 N13 C48 -167.7(4) . . . . ? N9 Cu1 N13 C48 -98.0(4) . . . . ? N13 C42 N14 C43 -0.7(5) . . . . ? C41 C42 N14 C43 177.5(4) . . . . ? C44 C43 N14 C42 179.5(5) . . . . ? C48 C43 N14 C42 0.5(4) . . . . ? C49 C50 N15 C53 -1.4(5) . . . . ? C49 C50 N15 Cu1 168.0(3) . . . . ? C52 C53 N15 C50 0.2(6) . . . . ? C52 C53 N15 Cu1 -169.5(3) . . . . ? N13 Cu1 N15 C50 -105.8(3) . . . . ? N11 Cu1 N15 C50 117.1(3) . . . . ? N9 Cu1 N15 C50 16.1(3) . . . . ? N13 Cu1 N15 C53 63.4(3) . . . . ? N11 Cu1 N15 C53 -73.6(3) . . . . ? N9 Cu1 N15 C53 -174.7(3) . . . . ? O2 C54 O1 Cu2 -0.3(5) . . . . ? C49 C54 O1 Cu2 -180.0(2) . . . . ? N4 Cu2 O1 C54 -82.6(3) . . . . ? N2 Cu2 O1 C54 63.7(3) . . . . ? N6 Cu2 O1 C54 166.4(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O16 0.86 2.04 2.799(7) 147.3 1_556 N5 H5A O15 0.86 1.94 2.780(4) 166.3 . N7 H7A O17 0.86 2.01 2.836(8) 161.4 2_666 N10 H10 O2 0.86 1.98 2.840(4) 174.6 2_776 N12 H12A O9 0.86 2.21 3.002(9) 153.3 1_664 N14 H14A O20 0.86 1.88 2.720(10) 163.8 2_676 O15 H15A O8 0.82 2.35 2.961(9) 132.3 . O15 H15B O3 0.82 2.19 2.898(5) 143.9 2_766 O16 H16A O9 0.82 2.16 2.951(12) 162.3 2_666 O16 H16B O12 0.82 2.25 2.850(16) 130.7 . O17 H17D O4 0.82 2.04 2.844(10) 167.4 . O20 H20A O6 0.82 1.95 2.769(13) 175.4 2_666 C1 H1A O12 0.97 2.46 3.255(16) 138.9 1_556 C9 H9A O8 0.97 2.57 3.441(8) 149.6 . C15 H15 O2 0.93 2.54 3.454(5) 166.2 2_766 C33 H33B O14 0.97 2.58 3.538(16) 169.3 1_665 C53 H53 O5 0.93 2.52 3.400(6) 157.2 2_775 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.814 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.091 # start Validation Reply Form _vrf_PLAT420_2 ; PROBLEM: D-H Without Acceptor >O17 - >H17C ... ? RESPONSE: This is due to the disorder of these water molecules. ; # end Validation Reply Form data_3 #TrackingRef '- 1-9.cif' _database_code_depnum_ccdc_archive 'CCDC 788587' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H50 Cu2 N16, 4(Cl O4), H2 O' _chemical_formula_sum 'C58 H52 Cl4 Cu2 N16 O17' _chemical_formula_weight 1514.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8253(10) _cell_length_b 16.9498(11) _cell_length_c 17.9303(13) _cell_angle_alpha 68.450(2) _cell_angle_beta 84.851(3) _cell_angle_gamma 69.359(2) _cell_volume 3653.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 3654 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 18.11 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8371 _exptl_absorpt_correction_T_max 0.9242 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(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 35001 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12662 _reflns_number_gt 7068 _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. In the refinement, all the four perchlorate anion (Cl1/O1-O4, Cl2/O5-O8, Cl3/O9-O12 and Cl4/O13-O16)) were found to be disordered over two sites. The commands DFIX, EADP and ISOR were used in the refinement to restrain some distances (eg. Cl-O=1.38(1)\%A and O-O=2.25(2)\%A) and thermal factors. The final most satisfactory occupancies for the Cl1-, Cl2-, Cl3- and Cl4-involved perchlorate anions were 0.63(1):0.37(1), 0.56(1):0.44(1), 0.56(1):0.44(1) and 0.59(1):0.41(1), respectively. All the C- and N-bounded hydrogen atoms were postitioned geometrically. For the residual electron densities, only water O17 molecule can be assigned unambiguously. For the other residual electron densities, which should be considered as peaks from disordered water molecules, did not give a chemical meaningful result after a carefull refinement. Therefor, the contributions of the disordered solvent molecules (c.a. 113 e/unit cell) were removed from the diffraction data using the SQUEEZE routine of PLATON software and then final refinements were carried out. These electon densities account to ca. eleven water molecules, i.e. the suitable moiety formula should be Cu~2~C~58~H~50~N~16~.(Cl O~4~)~4~.(H~2~O)~6.5~ . ; _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^)+(0.1355P)^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 12662 _refine_ls_number_parameters 1046 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.1235 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2335 _refine_ls_wR_factor_gt 0.2135 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.69339(5) 0.21458(5) 0.69308(4) 0.0496(2) Uani 1 1 d . . . Cu2 Cu 1.24656(5) 0.31276(5) 0.22583(4) 0.0505(2) Uani 1 1 d . . . N1 N 0.5787(3) 0.2359(3) 0.7766(3) 0.0497(11) Uani 1 1 d . . . N2 N 0.7828(4) 0.1909(3) 0.7841(3) 0.0524(12) Uani 1 1 d . . . N3 N 0.7920(5) 0.2154(4) 0.8955(3) 0.0713(15) Uani 1 1 d . . . H3A H 0.7727 0.2323 0.9358 0.086 Uiso 1 1 calc R . . N4 N 0.6417(3) 0.0989(3) 0.7105(3) 0.0509(11) Uani 1 1 d . . . N5 N 0.5186(4) 0.0467(3) 0.7734(3) 0.0643(14) Uani 1 1 d . . . H5A H 0.4739 0.0361 0.8088 0.077 Uiso 1 1 calc R . . N6 N 0.5800(4) 0.3096(3) 0.6134(3) 0.0513(11) Uani 1 1 d . . . N7 N 0.4144(4) 0.3947(4) 0.5939(3) 0.0673(14) Uani 1 1 d . . . H7 H 0.3513 0.4187 0.6046 0.081 Uiso 1 1 calc R . . N8 N 1.3735(4) 0.3320(4) 0.1585(4) 0.0698(15) Uani 1 1 d . . . N9 N 1.3425(4) 0.2922(4) 0.3145(3) 0.0679(14) Uani 1 1 d . . . N10 N 1.5027(5) 0.2456(4) 0.3573(5) 0.099(2) Uani 1 1 d . . . H10A H 1.5688 0.2317 0.3560 0.118 Uiso 1 1 calc R . . N11 N 1.2633(3) 0.2238(3) 0.1664(3) 0.0520(12) Uani 1 1 d . . . N12 N 1.3378(4) 0.1804(4) 0.0681(3) 0.0721(15) Uani 1 1 d . . . H12A H 1.3791 0.1758 0.0299 0.086 Uiso 1 1 calc R . . N13 N 1.1720(4) 0.4367(3) 0.1356(3) 0.0551(12) Uani 1 1 d . . . N14 N 1.1943(6) 0.5626(4) 0.0569(3) 0.0806(17) Uani 1 1 d . . . H14A H 1.2253 0.6002 0.0317 0.097 Uiso 1 1 calc R . . N15 N 0.8055(4) 0.2131(3) 0.6157(3) 0.0574(13) Uani 1 1 d . . . N16 N 1.1355(3) 0.2897(3) 0.2983(3) 0.0497(11) Uani 1 1 d . . . C1 C 0.8856(5) 0.1579(4) 0.8110(4) 0.0600(16) Uani 1 1 d . . . C2 C 0.9757(6) 0.1133(5) 0.7794(5) 0.084(2) Uani 1 1 d . . . H2 H 0.9734 0.1024 0.7325 0.101 Uiso 1 1 calc R . . C3 C 1.0670(7) 0.0868(6) 0.8208(6) 0.109(3) Uani 1 1 d . . . H3 H 1.1282 0.0583 0.8007 0.131 Uiso 1 1 calc R . . C4 C 1.0717(9) 0.1007(8) 0.8909(7) 0.135(4) Uani 1 1 d . . . H4 H 1.1353 0.0799 0.9178 0.162 Uiso 1 1 calc R . . C5 C 0.9835(9) 0.1450(7) 0.9222(6) 0.118(3) Uani 1 1 d . . . H5 H 0.9858 0.1552 0.9694 0.142 Uiso 1 1 calc R . . C6 C 0.8917(7) 0.1733(5) 0.8793(4) 0.079(2) Uani 1 1 d . . . C7 C 0.7313(5) 0.2251(4) 0.8375(3) 0.0593(16) Uani 1 1 d . . . C8 C 0.6167(5) 0.2714(5) 0.8270(4) 0.0655(17) Uani 1 1 d . . . H8A H 0.5853 0.2591 0.8787 0.079 Uiso 1 1 calc R . . H8B H 0.5998 0.3363 0.8012 0.079 Uiso 1 1 calc R . . C9 C 0.5734(5) 0.1457(4) 0.8243(3) 0.0575(15) Uani 1 1 d . . . H9A H 0.5094 0.1520 0.8524 0.069 Uiso 1 1 calc R . . H9B H 0.6307 0.1121 0.8638 0.069 Uiso 1 1 calc R . . C10 C 0.5782(4) 0.0967(4) 0.7698(3) 0.0511(14) Uani 1 1 d . . . C11 C 0.5420(5) 0.0163(4) 0.7117(4) 0.0620(17) Uani 1 1 d . . . C12 C 0.4987(7) -0.0310(5) 0.6843(5) 0.087(2) Uani 1 1 d . . . H12 H 0.4455 -0.0508 0.7101 0.104 Uiso 1 1 calc R . . C13 C 0.5408(8) -0.0467(5) 0.6150(6) 0.098(3) Uani 1 1 d . . . H13 H 0.5144 -0.0782 0.5942 0.118 Uiso 1 1 calc R . . C14 C 0.6193(7) -0.0179(5) 0.5764(5) 0.081(2) Uani 1 1 d . . . H14 H 0.6439 -0.0306 0.5306 0.097 Uiso 1 1 calc R . . C15 C 0.6630(6) 0.0293(5) 0.6031(4) 0.0732(19) Uani 1 1 d . . . H15 H 0.7159 0.0486 0.5763 0.088 Uiso 1 1 calc R . . C16 C 0.6230(5) 0.0470(4) 0.6739(4) 0.0600(16) Uani 1 1 d . . . C17 C 0.4781(5) 0.2977(5) 0.7349(4) 0.0673(17) Uani 1 1 d . . . H17A H 0.4498 0.3466 0.7553 0.081 Uiso 1 1 calc R . . H17B H 0.4299 0.2654 0.7448 0.081 Uiso 1 1 calc R . . C18 C 0.4918(5) 0.3354(4) 0.6470(4) 0.0548(15) Uani 1 1 d . . . C19 C 0.4553(6) 0.4103(4) 0.5177(4) 0.0667(18) Uani 1 1 d . . . C20 C 0.4075(7) 0.4627(5) 0.4416(5) 0.083(2) Uani 1 1 d . . . H20 H 0.3376 0.4976 0.4339 0.100 Uiso 1 1 calc R . . C21 C 0.4735(9) 0.4586(6) 0.3773(5) 0.094(3) Uani 1 1 d . . . H21 H 0.4461 0.4926 0.3251 0.113 Uiso 1 1 calc R . . C22 C 0.5776(8) 0.4058(6) 0.3890(4) 0.090(3) Uani 1 1 d . . . H22 H 0.6178 0.4050 0.3447 0.108 Uiso 1 1 calc R . . C23 C 0.6235(6) 0.3534(5) 0.4663(4) 0.0694(18) Uani 1 1 d . . . H23 H 0.6933 0.3181 0.4742 0.083 Uiso 1 1 calc R . . C24 C 0.5601(5) 0.3565(4) 0.5309(4) 0.0596(16) Uani 1 1 d . . . C25 C 0.8505(5) 0.1485(4) 0.5859(4) 0.0678(18) Uani 1 1 d . . . H25 H 0.8363 0.0949 0.6071 0.081 Uiso 1 1 calc R . . C26 C 0.9180(5) 0.1585(4) 0.5240(4) 0.0659(17) Uani 1 1 d . . . H26 H 0.9476 0.1129 0.5033 0.079 Uiso 1 1 calc R . . C27 C 0.9408(4) 0.2371(4) 0.4936(3) 0.0573(15) Uani 1 1 d . . . C28 C 0.8983(4) 0.3008(4) 0.5292(3) 0.0568(15) Uani 1 1 d . . . H28 H 0.9138 0.3538 0.5113 0.068 Uiso 1 1 calc R . . C29 C 0.8340(5) 0.2856(5) 0.5902(3) 0.0609(16) Uani 1 1 d . . . H29 H 0.8087 0.3276 0.6154 0.073 Uiso 1 1 calc R . . C30 C 1.0082(4) 0.2532(4) 0.4234(3) 0.0555(15) Uani 1 1 d . . . C31 C 0.9911(4) 0.3400(4) 0.3696(3) 0.0600(16) Uani 1 1 d . . . H31 H 0.9361 0.3881 0.3753 0.072 Uiso 1 1 calc R . . C32 C 1.0553(4) 0.3544(4) 0.3084(3) 0.0603(16) Uani 1 1 d . . . H32 H 1.0419 0.4130 0.2718 0.072 Uiso 1 1 calc R . . C33 C 1.1515(4) 0.2066(4) 0.3496(3) 0.0527(14) Uani 1 1 d . . . H33 H 1.2074 0.1598 0.3426 0.063 Uiso 1 1 calc R . . C34 C 1.0901(4) 0.1861(4) 0.4123(3) 0.0545(15) Uani 1 1 d . . . H34 H 1.1044 0.1267 0.4472 0.065 Uiso 1 1 calc R . . C35 C 1.4671(5) 0.2813(5) 0.2118(6) 0.093(3) Uani 1 1 d . . . H35A H 1.5166 0.3125 0.1951 0.112 Uiso 1 1 calc R . . H35B H 1.4988 0.2216 0.2088 0.112 Uiso 1 1 calc R . . C36 C 1.4381(6) 0.2731(4) 0.2964(6) 0.080(2) Uani 1 1 d . . . C37 C 1.4450(4) 0.2430(3) 0.4232(4) 0.096(3) Uani 1 1 d G . . C38 C 1.4686(5) 0.2166(3) 0.5044(4) 0.109(3) Uani 1 1 d G . . H38 H 1.5372 0.1949 0.5228 0.131 Uiso 1 1 calc R . . C39 C 1.3898(7) 0.2227(4) 0.5581(3) 0.114(3) Uani 1 1 d G . . H39 H 1.4056 0.2051 0.6124 0.137 Uiso 1 1 calc R . . C40 C 1.2872(6) 0.2552(4) 0.5306(3) 0.110(3) Uani 1 1 d G . . H40 H 1.2345 0.2593 0.5665 0.133 Uiso 1 1 calc R . . C41 C 1.2635(4) 0.2816(4) 0.4493(3) 0.099(3) Uani 1 1 d G . . H41 H 1.1949 0.3033 0.4309 0.119 Uiso 1 1 calc R . . C42 C 1.3424(5) 0.2755(3) 0.3956(3) 0.082(2) Uani 1 1 d G . . C43 C 1.3789(5) 0.3032(5) 0.0908(4) 0.080(2) Uani 1 1 d . . . H43A H 1.4506 0.2786 0.0786 0.096 Uiso 1 1 calc R . . H43B H 1.3435 0.3546 0.0439 0.096 Uiso 1 1 calc R . . C44 C 1.3291(4) 0.2328(4) 0.1109(4) 0.0579(16) Uani 1 1 d . . . C45 C 1.2702(5) 0.1366(4) 0.0956(4) 0.0598(16) Uani 1 1 d . . . C46 C 1.2424(7) 0.0769(5) 0.0708(4) 0.089(2) Uani 1 1 d . . . H46 H 1.2769 0.0565 0.0309 0.106 Uiso 1 1 calc R . . C47 C 1.1625(7) 0.0507(5) 0.1085(5) 0.089(2) Uani 1 1 d . . . H47 H 1.1399 0.0140 0.0918 0.106 Uiso 1 1 calc R . . C48 C 1.1129(6) 0.0781(5) 0.1726(5) 0.087(2) Uani 1 1 d . . . H48 H 1.0598 0.0579 0.1978 0.104 Uiso 1 1 calc R . . C49 C 1.1422(5) 0.1331(5) 0.1970(4) 0.0666(17) Uani 1 1 d . . . H49 H 1.1102 0.1506 0.2391 0.080 Uiso 1 1 calc R . . C50 C 1.2222(4) 0.1632(4) 0.1575(3) 0.0510(14) Uani 1 1 d . . . C51 C 1.3500(5) 0.4316(4) 0.1319(5) 0.0742(19) Uani 1 1 d . . . H51A H 1.3665 0.4466 0.1753 0.089 Uiso 1 1 calc R . . H51B H 1.3912 0.4510 0.0868 0.089 Uiso 1 1 calc R . . C52 C 1.2396(5) 0.4771(4) 0.1085(4) 0.0619(16) Uani 1 1 d . . . C53 C 1.0891(6) 0.5789(5) 0.0519(4) 0.0708(18) Uani 1 1 d . . . C54 C 1.0075(9) 0.6536(5) 0.0092(5) 0.095(3) Uani 1 1 d . . . H54 H 1.0162 0.7069 -0.0251 0.114 Uiso 1 1 calc R . . C55 C 0.9135(10) 0.6435(9) 0.0211(7) 0.128(4) Uani 1 1 d . . . H55 H 0.8560 0.6939 -0.0039 0.154 Uiso 1 1 calc R . . C56 C 0.8962(7) 0.5627(7) 0.0683(5) 0.101(3) Uani 1 1 d . . . H56 H 0.8304 0.5588 0.0721 0.121 Uiso 1 1 calc R . . C57 C 0.9808(6) 0.4903(5) 0.1082(4) 0.078(2) Uani 1 1 d . . . H57 H 0.9730 0.4358 0.1401 0.093 Uiso 1 1 calc R . . C58 C 1.0783(5) 0.4982(4) 0.1010(4) 0.0590(16) Uani 1 1 d . . . Cl1 Cl 0.1548(9) 0.5685(11) 0.2928(8) 0.124(7) Uani 0.63 1 d PD A 1 O1 O 0.2455(13) 0.587(2) 0.2746(15) 0.172(11) Uani 0.63 1 d PD A 1 O2 O 0.0704(13) 0.6466(11) 0.2631(14) 0.238(8) Uani 0.63 1 d PD A 1 O3 O 0.1530(19) 0.5018(16) 0.2692(15) 0.215(10) Uani 0.63 1 d PD A 1 O4 O 0.1487(15) 0.5386(15) 0.3775(9) 0.182(8) Uani 0.63 1 d PD A 1 Cl1' Cl 0.1559(16) 0.5670(17) 0.2824(13) 0.124(12) Uani 0.37 1 d PD B 2 O1' O 0.0949(14) 0.5986(15) 0.2145(10) 0.119(6) Uani 0.37 1 d PD B 2 O2' O 0.091(3) 0.579(3) 0.3445(13) 0.182(15) Uani 0.37 1 d PD B 2 O3' O 0.214(3) 0.4769(19) 0.302(2) 0.215(17) Uani 0.37 1 d PD B 2 O4' O 0.221(3) 0.615(3) 0.273(2) 0.172(19) Uani 0.37 1 d PD B 2 Cl2 Cl 0.2068(18) 0.8864(14) 0.6306(13) 0.143(6) Uani 0.56 1 d PD C 1 O5 O 0.263(3) 0.892(3) 0.686(2) 0.279(19) Uani 0.56 1 d PD C 1 O6 O 0.1345(17) 0.8467(16) 0.6683(14) 0.208(9) Uani 0.56 1 d PD C 1 O7 O 0.157(3) 0.9672(14) 0.572(2) 0.194(14) Uani 0.56 1 d PD C 1 O8 O 0.275(2) 0.8282(18) 0.5943(14) 0.188(10) Uani 0.56 1 d PD C 1 Cl2' Cl 0.208(2) 0.9093(18) 0.6304(14) 0.143(7) Uani 0.44 1 d PD D 2 O5' O 0.180(4) 0.955(2) 0.5499(14) 0.194(19) Uani 0.44 1 d PD D 2 O6' O 0.122(2) 0.9189(19) 0.6747(18) 0.200(11) Uani 0.44 1 d PD D 2 O7' O 0.278(3) 0.938(3) 0.653(3) 0.28(3) Uani 0.44 1 d PD D 2 O8' O 0.258(3) 0.8167(19) 0.644(2) 0.188(14) Uani 0.44 1 d PD D 2 Cl3 Cl 0.3775(8) 0.9222(6) 0.9295(7) 0.066(3) Uani 0.56 1 d PD E 1 O9 O 0.4531(12) 0.8798(10) 0.9906(8) 0.135(7) Uani 0.56 1 d PD E 1 O10 O 0.2839(11) 0.9157(13) 0.9577(13) 0.154(10) Uani 0.56 1 d PD E 1 O11 O 0.3666(10) 1.0127(7) 0.8952(8) 0.126(5) Uani 0.56 1 d PD E 1 O12 O 0.4085(15) 0.8843(13) 0.8706(10) 0.154(8) Uani 0.56 1 d PD E 1 Cl3' Cl 0.3815(10) 0.9154(9) 0.9434(8) 0.084(5) Uani 0.44 1 d PD F 2 O9' O 0.3690(18) 0.9171(16) 0.8669(9) 0.154(11) Uani 0.44 1 d PD F 2 O10' O 0.2888(10) 0.9316(12) 0.9800(12) 0.076(5) Uani 0.44 1 d PD F 2 O11' O 0.4263(12) 0.9777(10) 0.9386(10) 0.105(5) Uani 0.44 1 d PD F 2 O12' O 0.4475(11) 0.8302(8) 0.9892(9) 0.086(5) Uani 0.44 1 d PD F 2 Cl4 Cl 0.5756(9) 0.5302(7) 0.1137(6) 0.102(3) Uani 0.59 1 d PD G 1 O13 O 0.5270(10) 0.5072(10) 0.1841(5) 0.120(4) Uani 0.59 1 d PD G 1 O14 O 0.5036(10) 0.5726(11) 0.0503(6) 0.136(6) Uani 0.59 1 d PD G 1 O15 O 0.6501(15) 0.4570(11) 0.1048(12) 0.233(13) Uani 0.59 1 d PD G 1 O16 O 0.6195(12) 0.5925(11) 0.1143(9) 0.171(6) Uani 0.59 1 d PD G 1 Cl4' Cl 0.5969(14) 0.5079(11) 0.1310(9) 0.102(4) Uani 0.41 1 d PD H 2 O13' O 0.5876(17) 0.4266(12) 0.1786(12) 0.156(7) Uani 0.41 1 d PD H 2 O14' O 0.4995(19) 0.5707(15) 0.1029(18) 0.26(2) Uani 0.41 1 d PD H 2 O15' O 0.659(3) 0.500(2) 0.0685(16) 0.233(18) Uani 0.41 1 d PD H 2 O16' O 0.6397(18) 0.5380(15) 0.1775(14) 0.171(9) Uani 0.41 1 d PD H 2 O17 O 0.2978(5) 0.6906(4) 0.9950(3) 0.119(2) Uani 1 1 d . . . H17C H 0.3612 0.6699 0.9969 0.142 Uiso 1 1 d R . . H17D H 0.2785 0.7243 0.9486 0.142 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0540(4) 0.0576(5) 0.0361(4) -0.0149(3) 0.0128(3) -0.0228(4) Cu2 0.0447(4) 0.0523(5) 0.0517(4) -0.0159(4) 0.0113(3) -0.0188(3) N1 0.056(3) 0.057(3) 0.040(2) -0.017(2) 0.009(2) -0.025(2) N2 0.063(3) 0.050(3) 0.047(3) -0.017(2) 0.008(2) -0.025(2) N3 0.101(5) 0.081(4) 0.050(3) -0.028(3) 0.006(3) -0.048(4) N4 0.055(3) 0.052(3) 0.044(3) -0.015(2) -0.004(2) -0.018(2) N5 0.067(3) 0.063(3) 0.058(3) -0.007(3) 0.002(3) -0.031(3) N6 0.064(3) 0.048(3) 0.044(3) -0.014(2) 0.006(2) -0.025(2) N7 0.054(3) 0.057(3) 0.087(4) -0.029(3) -0.004(3) -0.009(3) N8 0.059(3) 0.059(4) 0.097(4) -0.028(3) 0.032(3) -0.033(3) N9 0.058(3) 0.062(4) 0.079(4) -0.018(3) -0.018(3) -0.018(3) N10 0.072(4) 0.058(4) 0.164(7) -0.034(5) -0.044(5) -0.014(3) N11 0.056(3) 0.042(3) 0.052(3) -0.015(2) 0.016(2) -0.016(2) N12 0.078(4) 0.056(3) 0.072(4) -0.028(3) 0.029(3) -0.011(3) N13 0.063(3) 0.043(3) 0.056(3) -0.016(2) 0.006(3) -0.017(3) N14 0.120(5) 0.048(4) 0.068(4) -0.015(3) 0.027(4) -0.035(4) N15 0.063(3) 0.064(3) 0.049(3) -0.023(3) 0.016(2) -0.027(3) N16 0.050(3) 0.054(3) 0.046(3) -0.021(3) 0.008(2) -0.017(2) C1 0.071(4) 0.059(4) 0.054(4) -0.017(3) -0.004(3) -0.029(3) C2 0.080(5) 0.078(5) 0.092(5) -0.027(4) -0.003(4) -0.026(4) C3 0.078(6) 0.105(7) 0.140(8) -0.049(6) -0.028(6) -0.015(5) C4 0.103(8) 0.160(10) 0.141(9) -0.057(8) -0.042(7) -0.032(7) C5 0.113(8) 0.124(8) 0.115(7) -0.048(7) -0.048(7) -0.020(6) C6 0.092(6) 0.083(5) 0.070(5) -0.023(4) -0.004(4) -0.042(5) C7 0.087(5) 0.060(4) 0.042(3) -0.018(3) 0.012(3) -0.040(4) C8 0.076(5) 0.068(4) 0.061(4) -0.035(4) 0.026(3) -0.029(4) C9 0.061(4) 0.071(4) 0.045(3) -0.016(3) 0.014(3) -0.035(3) C10 0.059(4) 0.045(3) 0.048(3) -0.010(3) 0.006(3) -0.023(3) C11 0.065(4) 0.045(4) 0.058(4) 0.002(3) -0.018(3) -0.015(3) C12 0.121(7) 0.062(5) 0.082(5) -0.013(4) -0.033(5) -0.042(5) C13 0.129(8) 0.041(4) 0.119(7) -0.019(5) -0.062(6) -0.018(5) C14 0.104(6) 0.053(5) 0.076(5) -0.030(4) -0.028(5) 0.001(4) C15 0.085(5) 0.063(4) 0.057(4) -0.025(4) -0.005(3) -0.002(4) C16 0.075(4) 0.034(3) 0.052(4) -0.007(3) -0.015(3) -0.001(3) C17 0.064(4) 0.076(5) 0.057(4) -0.026(4) 0.012(3) -0.020(4) C18 0.058(4) 0.043(4) 0.058(4) -0.016(3) -0.001(3) -0.012(3) C19 0.096(5) 0.047(4) 0.058(4) -0.005(3) -0.004(4) -0.039(4) C20 0.103(6) 0.052(4) 0.080(5) -0.006(4) -0.033(5) -0.020(4) C21 0.141(8) 0.068(5) 0.063(5) 0.000(4) -0.033(6) -0.040(6) C22 0.162(9) 0.085(6) 0.039(4) -0.009(4) 0.000(5) -0.074(6) C23 0.090(5) 0.070(5) 0.054(4) -0.016(3) 0.002(3) -0.041(4) C24 0.079(5) 0.053(4) 0.049(4) -0.012(3) -0.007(3) -0.030(4) C25 0.089(5) 0.057(4) 0.073(4) -0.034(4) 0.037(4) -0.039(4) C26 0.077(4) 0.062(4) 0.070(4) -0.034(3) 0.030(3) -0.033(4) C27 0.051(3) 0.069(4) 0.054(3) -0.023(3) 0.016(3) -0.025(3) C28 0.066(4) 0.061(4) 0.058(4) -0.032(3) 0.025(3) -0.034(3) C29 0.072(4) 0.078(5) 0.053(4) -0.037(3) 0.023(3) -0.041(4) C30 0.058(4) 0.066(4) 0.044(3) -0.021(3) 0.016(3) -0.025(3) C31 0.052(3) 0.060(4) 0.049(3) -0.016(3) 0.015(3) -0.003(3) C32 0.052(4) 0.057(4) 0.051(3) -0.006(3) 0.004(3) -0.009(3) C33 0.054(3) 0.047(4) 0.052(3) -0.024(3) 0.008(3) -0.007(3) C34 0.062(4) 0.046(4) 0.054(3) -0.020(3) 0.016(3) -0.019(3) C35 0.041(4) 0.064(5) 0.166(9) -0.035(5) 0.016(5) -0.018(4) C36 0.060(5) 0.048(4) 0.130(7) -0.024(4) -0.019(5) -0.018(4) C37 0.126(8) 0.036(4) 0.118(7) -0.013(5) -0.069(6) -0.018(5) C38 0.135(8) 0.060(5) 0.132(8) -0.024(6) -0.062(7) -0.027(5) C39 0.166(10) 0.081(6) 0.101(7) -0.020(5) -0.041(7) -0.050(7) C40 0.149(9) 0.095(7) 0.096(7) -0.031(5) -0.019(6) -0.050(6) C41 0.149(8) 0.105(7) 0.056(5) -0.024(5) -0.026(5) -0.054(6) C42 0.114(7) 0.050(4) 0.081(6) -0.015(4) -0.040(5) -0.026(4) C43 0.077(5) 0.070(5) 0.088(5) -0.028(4) 0.047(4) -0.029(4) C44 0.051(3) 0.047(4) 0.067(4) -0.023(3) 0.028(3) -0.010(3) C45 0.073(4) 0.043(4) 0.050(3) -0.017(3) 0.001(3) -0.004(3) C46 0.139(7) 0.056(5) 0.063(5) -0.023(4) -0.005(5) -0.021(5) C47 0.123(7) 0.066(5) 0.070(5) -0.012(4) -0.030(5) -0.030(5) C48 0.102(6) 0.077(5) 0.088(5) -0.021(5) -0.005(5) -0.044(5) C49 0.086(5) 0.070(4) 0.058(4) -0.026(3) 0.013(3) -0.044(4) C50 0.057(3) 0.043(3) 0.047(3) -0.009(3) -0.006(3) -0.016(3) C51 0.062(4) 0.061(4) 0.096(5) -0.017(4) 0.022(4) -0.034(4) C52 0.062(4) 0.052(4) 0.058(4) -0.005(3) 0.015(3) -0.022(3) C53 0.094(6) 0.051(5) 0.055(4) -0.015(3) 0.003(4) -0.014(4) C54 0.142(8) 0.044(5) 0.068(5) -0.009(4) -0.006(5) -0.007(5) C55 0.133(10) 0.117(10) 0.108(8) -0.038(7) -0.026(7) -0.006(8) C56 0.084(6) 0.116(8) 0.082(6) -0.028(6) -0.019(5) -0.011(6) C57 0.088(5) 0.078(5) 0.055(4) -0.021(4) -0.004(4) -0.017(4) C58 0.065(4) 0.047(4) 0.051(4) -0.014(3) 0.002(3) -0.008(3) Cl1 0.175(16) 0.089(10) 0.120(8) -0.039(7) -0.024(8) -0.050(10) O1 0.158(17) 0.168(18) 0.19(2) -0.032(14) 0.005(15) -0.089(15) O2 0.209(19) 0.21(2) 0.25(3) -0.06(2) -0.010(18) -0.050(17) O3 0.26(3) 0.19(2) 0.24(2) -0.11(2) -0.02(2) -0.094(19) O4 0.20(2) 0.20(2) 0.141(13) -0.060(14) -0.005(13) -0.063(16) Cl1' 0.17(3) 0.089(17) 0.120(14) -0.039(12) -0.024(13) -0.050(17) O1' 0.125(14) 0.128(17) 0.105(13) -0.060(12) -0.048(11) -0.013(12) O2' 0.17(3) 0.20(4) 0.16(3) -0.08(3) 0.06(3) -0.04(3) O3' 0.26(4) 0.19(4) 0.24(4) -0.11(3) -0.02(3) -0.09(3) O4' 0.16(3) 0.17(3) 0.19(4) -0.03(3) 0.00(3) -0.09(2) Cl2 0.164(13) 0.163(12) 0.103(8) -0.054(8) -0.007(8) -0.049(9) O5 0.29(4) 0.29(5) 0.28(4) -0.11(4) -0.02(3) -0.12(3) O6 0.173(19) 0.22(2) 0.22(2) -0.06(2) 0.045(15) -0.087(19) O7 0.21(3) 0.18(3) 0.18(2) -0.07(2) 0.00(2) -0.049(19) O8 0.181(18) 0.18(2) 0.19(2) -0.069(18) 0.018(18) -0.046(15) Cl2' 0.164(16) 0.163(17) 0.103(11) -0.054(12) -0.007(9) -0.049(12) O5' 0.21(3) 0.18(3) 0.18(3) -0.07(3) 0.00(3) -0.05(3) O6' 0.17(2) 0.20(3) 0.21(2) -0.07(2) 0.072(19) -0.05(2) O7' 0.29(5) 0.29(6) 0.28(5) -0.11(4) -0.02(4) -0.12(4) O8' 0.18(3) 0.18(3) 0.19(4) -0.07(3) 0.02(3) -0.05(2) Cl3 0.073(5) 0.062(5) 0.056(4) -0.024(3) 0.025(3) -0.017(4) O9 0.138(13) 0.154(18) 0.095(11) -0.054(13) 0.003(9) -0.019(14) O10 0.132(14) 0.148(17) 0.17(2) -0.054(13) 0.050(12) -0.052(11) O11 0.122(12) 0.107(10) 0.125(12) -0.019(9) 0.047(8) -0.043(9) O12 0.169(17) 0.164(17) 0.136(15) -0.080(12) 0.004(11) -0.037(14) Cl3' 0.080(8) 0.098(9) 0.064(7) -0.021(5) 0.016(5) -0.031(7) O9' 0.17(2) 0.16(2) 0.14(2) -0.080(17) 0.004(16) -0.037(19) O10' 0.068(9) 0.075(9) 0.083(9) -0.042(8) 0.038(7) -0.020(7) O11' 0.115(14) 0.106(14) 0.119(14) -0.051(12) 0.033(10) -0.061(12) O12' 0.074(8) 0.068(9) 0.076(9) -0.003(7) 0.019(7) -0.007(7) Cl4 0.108(6) 0.106(6) 0.084(5) -0.030(4) 0.031(4) -0.037(5) O13 0.134(10) 0.142(11) 0.068(6) -0.029(7) 0.038(7) -0.047(8) O14 0.114(10) 0.168(13) 0.101(9) -0.009(9) -0.005(7) -0.060(9) O15 0.24(3) 0.21(3) 0.22(3) -0.10(3) 0.05(2) -0.032(19) O16 0.173(14) 0.185(17) 0.173(16) -0.060(13) -0.004(13) -0.083(14) Cl4' 0.108(8) 0.106(8) 0.084(7) -0.030(6) 0.031(6) -0.037(7) O13' 0.163(18) 0.144(18) 0.160(18) -0.029(16) 0.024(15) -0.082(15) O14' 0.25(4) 0.26(5) 0.28(6) -0.10(5) 0.00(4) -0.09(4) O15' 0.24(4) 0.21(3) 0.22(3) -0.10(3) 0.05(3) -0.03(3) O16' 0.17(2) 0.19(2) 0.17(2) -0.060(19) -0.004(18) -0.083(19) O17 0.148(5) 0.137(5) 0.110(4) -0.070(4) 0.059(4) -0.081(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.970(5) . ? Cu1 N15 1.985(4) . ? Cu1 N6 2.006(5) . ? Cu1 N1 2.110(4) . ? Cu1 N4 2.225(5) . ? Cu2 N16 1.972(4) . ? Cu2 N9 2.014(5) . ? Cu2 N11 2.086(5) . ? Cu2 N13 2.090(5) . ? Cu2 N8 2.092(5) . ? N1 C8 1.472(7) . ? N1 C17 1.474(7) . ? N1 C9 1.477(7) . ? N2 C7 1.325(7) . ? N2 C1 1.389(7) . ? N3 C7 1.323(7) . ? N3 C6 1.371(9) . ? N3 H3A 0.8600 . ? N4 C10 1.315(7) . ? N4 C16 1.373(7) . ? N5 C11 1.355(8) . ? N5 C10 1.359(7) . ? N5 H5A 0.8600 . ? N6 C18 1.314(7) . ? N6 C24 1.397(7) . ? N7 C18 1.335(7) . ? N7 C19 1.400(8) . ? N7 H7 0.8600 . ? N8 C43 1.453(9) . ? N8 C35 1.470(9) . ? N8 C51 1.494(8) . ? N9 C36 1.286(9) . ? N9 C42 1.377(7) . ? N10 C36 1.309(9) . ? N10 C37 1.360(9) . ? N10 H10A 0.8600 . ? N11 C44 1.290(6) . ? N11 C50 1.396(7) . ? N12 C44 1.341(8) . ? N12 C45 1.343(8) . ? N12 H12A 0.8600 . ? N13 C52 1.305(7) . ? N13 C58 1.367(7) . ? N14 C52 1.351(7) . ? N14 C53 1.386(9) . ? N14 H14A 0.8600 . ? N15 C25 1.328(7) . ? N15 C29 1.331(7) . ? N16 C32 1.310(7) . ? N16 C33 1.321(7) . ? C1 C6 1.357(9) . ? C1 C2 1.403(10) . ? C2 C3 1.368(10) . ? C2 H2 0.9300 . ? C3 C4 1.372(13) . ? C3 H3 0.9300 . ? C4 C5 1.380(13) . ? C4 H4 0.9300 . ? C5 C6 1.381(11) . ? C5 H5 0.9300 . ? C7 C8 1.493(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.481(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.387(9) . ? C11 C16 1.414(9) . ? C12 C13 1.399(12) . ? C12 H12 0.9300 . ? C13 C14 1.374(11) . ? C13 H13 0.9300 . ? C14 C15 1.382(10) . ? C14 H14 0.9300 . ? C15 C16 1.429(9) . ? C15 H15 0.9300 . ? C17 C18 1.490(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C19 C20 1.394(9) . ? C19 C24 1.400(9) . ? C20 C21 1.411(11) . ? C20 H20 0.9300 . ? C21 C22 1.388(11) . ? C21 H21 0.9300 . ? C22 C23 1.403(9) . ? C22 H22 0.9300 . ? C23 C24 1.393(9) . ? C23 H23 0.9300 . ? C25 C26 1.385(8) . ? C25 H25 0.9300 . ? C26 C27 1.379(8) . ? C26 H26 0.9300 . ? C27 C28 1.383(8) . ? C27 C30 1.496(7) . ? C28 C29 1.355(7) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C34 1.354(8) . ? C30 C31 1.380(8) . ? C31 C32 1.354(8) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.362(7) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.503(11) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 C40 1.3900 . ? C39 H39 0.9300 . ? C40 C41 1.3900 . ? C40 H40 0.9300 . ? C41 C42 1.3900 . ? C41 H41 0.9300 . ? C43 C44 1.499(9) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C45 C50 1.379(8) . ? C45 C46 1.416(10) . ? C46 C47 1.365(11) . ? C46 H46 0.9300 . ? C47 C48 1.426(11) . ? C47 H47 0.9300 . ? C48 C49 1.350(9) . ? C48 H48 0.9300 . ? C49 C50 1.406(8) . ? C49 H49 0.9300 . ? C51 C52 1.466(9) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C53 C54 1.378(11) . ? C53 C58 1.380(9) . ? C54 C55 1.358(13) . ? C54 H54 0.9300 . ? C55 C56 1.412(14) . ? C55 H55 0.9300 . ? C56 C57 1.371(10) . ? C56 H56 0.9300 . ? C57 C58 1.391(9) . ? C57 H57 0.9300 . ? Cl1 O3 1.352(8) . ? Cl1 O2 1.379(9) . ? Cl1 O1 1.383(8) . ? Cl1 O4 1.418(9) . ? Cl1' O1' 1.366(9) . ? Cl1' O3' 1.375(9) . ? Cl1' O4' 1.383(9) . ? Cl1' O2' 1.398(9) . ? Cl2 O5 1.358(9) . ? Cl2 O7 1.367(9) . ? Cl2 O6 1.389(9) . ? Cl2 O8 1.413(9) . ? Cl2' O7' 1.362(9) . ? Cl2' O6' 1.367(9) . ? Cl2' O5' 1.379(9) . ? Cl2' O8' 1.408(9) . ? Cl3 O10 1.372(8) . ? Cl3 O9 1.381(8) . ? Cl3 O11 1.384(8) . ? Cl3 O12 1.392(8) . ? Cl3' O10' 1.372(8) . ? Cl3' O11' 1.375(9) . ? Cl3' O9' 1.386(9) . ? Cl3' O12' 1.388(9) . ? Cl4 O15 1.358(8) . ? Cl4 O13 1.367(8) . ? Cl4 O14 1.378(9) . ? Cl4 O16 1.395(8) . ? Cl4' O15' 1.365(9) . ? Cl4' O13' 1.374(9) . ? Cl4' O16' 1.385(9) . ? Cl4' O14' 1.385(9) . ? O17 H17C 0.8201 . ? O17 H17D 0.8198 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N15 94.49(19) . . ? N2 Cu1 N6 144.14(19) . . ? N15 Cu1 N6 95.83(19) . . ? N2 Cu1 N1 81.05(18) . . ? N15 Cu1 N1 169.97(19) . . ? N6 Cu1 N1 82.96(18) . . ? N2 Cu1 N4 111.83(17) . . ? N15 Cu1 N4 108.87(19) . . ? N6 Cu1 N4 97.03(17) . . ? N1 Cu1 N4 81.15(17) . . ? N16 Cu2 N9 94.1(2) . . ? N16 Cu2 N11 100.66(18) . . ? N9 Cu2 N11 125.4(2) . . ? N16 Cu2 N13 104.02(19) . . ? N9 Cu2 N13 125.9(2) . . ? N11 Cu2 N13 100.86(18) . . ? N16 Cu2 N8 174.6(2) . . ? N9 Cu2 N8 80.6(2) . . ? N11 Cu2 N8 81.53(19) . . ? N13 Cu2 N8 80.2(2) . . ? C8 N1 C17 112.8(5) . . ? C8 N1 C9 110.7(4) . . ? C17 N1 C9 110.7(5) . . ? C8 N1 Cu1 106.1(3) . . ? C17 N1 Cu1 110.7(3) . . ? C9 N1 Cu1 105.5(3) . . ? C7 N2 C1 104.0(5) . . ? C7 N2 Cu1 112.8(4) . . ? C1 N2 Cu1 142.8(4) . . ? C7 N3 C6 107.0(6) . . ? C7 N3 H3A 126.5 . . ? C6 N3 H3A 126.5 . . ? C10 N4 C16 105.1(5) . . ? C10 N4 Cu1 105.5(4) . . ? C16 N4 Cu1 145.2(4) . . ? C11 N5 C10 108.0(5) . . ? C11 N5 H5A 126.0 . . ? C10 N5 H5A 126.0 . . ? C18 N6 C24 106.0(5) . . ? C18 N6 Cu1 112.8(4) . . ? C24 N6 Cu1 141.1(4) . . ? C18 N7 C19 107.0(5) . . ? C18 N7 H7 126.5 . . ? C19 N7 H7 126.5 . . ? C43 N8 C35 112.4(6) . . ? C43 N8 C51 111.7(6) . . ? C35 N8 C51 111.3(5) . . ? C43 N8 Cu2 109.5(4) . . ? C35 N8 Cu2 108.2(4) . . ? C51 N8 Cu2 103.3(4) . . ? C36 N9 C42 105.7(6) . . ? C36 N9 Cu2 113.7(6) . . ? C42 N9 Cu2 139.2(4) . . ? C36 N10 C37 106.7(7) . . ? C36 N10 H10A 126.7 . . ? C37 N10 H10A 126.7 . . ? C44 N11 C50 105.1(5) . . ? C44 N11 Cu2 110.8(4) . . ? C50 N11 Cu2 143.6(4) . . ? C44 N12 C45 107.7(5) . . ? C44 N12 H12A 126.2 . . ? C45 N12 H12A 126.2 . . ? C52 N13 C58 106.4(5) . . ? C52 N13 Cu2 107.8(4) . . ? C58 N13 Cu2 144.9(4) . . ? C52 N14 C53 107.8(5) . . ? C52 N14 H14A 126.1 . . ? C53 N14 H14A 126.1 . . ? C25 N15 C29 118.5(5) . . ? C25 N15 Cu1 125.8(4) . . ? C29 N15 Cu1 115.7(4) . . ? C32 N16 C33 117.5(5) . . ? C32 N16 Cu2 123.1(4) . . ? C33 N16 Cu2 118.2(4) . . ? C6 C1 N2 109.7(6) . . ? C6 C1 C2 120.1(7) . . ? N2 C1 C2 130.2(6) . . ? C3 C2 C1 116.7(8) . . ? C3 C2 H2 121.6 . . ? C1 C2 H2 121.6 . . ? C2 C3 C4 122.4(9) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C3 C4 C5 121.1(9) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 116.2(9) . . ? C4 C5 H5 121.9 . . ? C6 C5 H5 121.9 . . ? C1 C6 N3 106.2(6) . . ? C1 C6 C5 123.3(8) . . ? N3 C6 C5 130.4(8) . . ? N3 C7 N2 113.0(6) . . ? N3 C7 C8 126.7(6) . . ? N2 C7 C8 120.2(5) . . ? N1 C8 C7 106.9(5) . . ? N1 C8 H8A 110.3 . . ? C7 C8 H8A 110.3 . . ? N1 C8 H8B 110.3 . . ? C7 C8 H8B 110.3 . . ? H8A C8 H8B 108.6 . . ? N1 C9 C10 109.0(4) . . ? N1 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? N1 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N4 C10 N5 112.4(5) . . ? N4 C10 C9 122.3(5) . . ? N5 C10 C9 125.3(5) . . ? N5 C11 C12 131.5(7) . . ? N5 C11 C16 104.7(5) . . ? C12 C11 C16 123.8(7) . . ? C11 C12 C13 115.0(8) . . ? C11 C12 H12 122.5 . . ? C13 C12 H12 122.5 . . ? C14 C13 C12 123.1(7) . . ? C14 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? C13 C14 C15 122.3(7) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C14 C15 C16 116.9(7) . . ? C14 C15 H15 121.5 . . ? C16 C15 H15 121.5 . . ? N4 C16 C11 109.7(5) . . ? N4 C16 C15 131.1(6) . . ? C11 C16 C15 118.9(6) . . ? N1 C17 C18 109.8(5) . . ? N1 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? N1 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N6 C18 N7 113.2(5) . . ? N6 C18 C17 123.3(5) . . ? N7 C18 C17 123.4(6) . . ? C20 C19 C24 123.7(7) . . ? C20 C19 N7 130.8(7) . . ? C24 C19 N7 105.5(5) . . ? C19 C20 C21 114.8(7) . . ? C19 C20 H20 122.6 . . ? C21 C20 H20 122.6 . . ? C22 C21 C20 122.5(7) . . ? C22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C21 C22 C23 121.4(8) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C24 C23 C22 117.2(7) . . ? C24 C23 H23 121.4 . . ? C22 C23 H23 121.4 . . ? C23 C24 N6 131.3(6) . . ? C23 C24 C19 120.4(6) . . ? N6 C24 C19 108.3(6) . . ? N15 C25 C26 121.8(5) . . ? N15 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C27 C26 C25 119.2(5) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 117.8(5) . . ? C26 C27 C30 120.9(5) . . ? C28 C27 C30 121.2(5) . . ? C29 C28 C27 119.5(5) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? N15 C29 C28 122.8(5) . . ? N15 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? C34 C30 C31 117.5(5) . . ? C34 C30 C27 122.6(6) . . ? C31 C30 C27 119.8(5) . . ? C32 C31 C30 119.4(5) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? N16 C32 C31 123.2(6) . . ? N16 C32 H32 118.4 . . ? C31 C32 H32 118.4 . . ? N16 C33 C34 123.1(5) . . ? N16 C33 H33 118.4 . . ? C34 C33 H33 118.4 . . ? C30 C34 C33 119.4(6) . . ? C30 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? N8 C35 C36 109.1(6) . . ? N8 C35 H35A 109.9 . . ? C36 C35 H35A 109.9 . . ? N8 C35 H35B 109.9 . . ? C36 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? N9 C36 N10 114.1(9) . . ? N9 C36 C35 120.0(7) . . ? N10 C36 C35 125.9(8) . . ? N10 C37 C38 133.9(5) . . ? N10 C37 C42 106.1(5) . . ? C38 C37 C42 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? N9 C42 C41 132.6(5) . . ? N9 C42 C37 107.3(5) . . ? C41 C42 C37 120.0 . . ? N8 C43 C44 109.5(5) . . ? N8 C43 H43A 109.8 . . ? C44 C43 H43A 109.8 . . ? N8 C43 H43B 109.8 . . ? C44 C43 H43B 109.8 . . ? H43A C43 H43B 108.2 . . ? N11 C44 N12 112.7(5) . . ? N11 C44 C43 122.5(5) . . ? N12 C44 C43 124.3(5) . . ? N12 C45 C50 106.1(5) . . ? N12 C45 C46 132.4(6) . . ? C50 C45 C46 121.4(7) . . ? C47 C46 C45 116.8(7) . . ? C47 C46 H46 121.6 . . ? C45 C46 H46 121.6 . . ? C46 C47 C48 121.8(7) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C49 C48 C47 120.7(7) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C48 C49 C50 118.6(6) . . ? C48 C49 H49 120.7 . . ? C50 C49 H49 120.7 . . ? C45 C50 N11 108.3(5) . . ? C45 C50 C49 120.7(6) . . ? N11 C50 C49 130.9(5) . . ? C52 C51 N8 108.2(5) . . ? C52 C51 H51A 110.0 . . ? N8 C51 H51A 110.0 . . ? C52 C51 H51B 110.0 . . ? N8 C51 H51B 110.0 . . ? H51A C51 H51B 108.4 . . ? N13 C52 N14 111.4(6) . . ? N13 C52 C51 122.2(6) . . ? N14 C52 C51 126.5(6) . . ? C54 C53 C58 123.3(8) . . ? C54 C53 N14 132.5(8) . . ? C58 C53 N14 104.2(6) . . ? C55 C54 C53 115.0(9) . . ? C55 C54 H54 122.5 . . ? C53 C54 H54 122.5 . . ? C54 C55 C56 125.1(10) . . ? C54 C55 H55 117.4 . . ? C56 C55 H55 117.4 . . ? C57 C56 C55 117.0(9) . . ? C57 C56 H56 121.5 . . ? C55 C56 H56 121.5 . . ? C56 C57 C58 120.2(8) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? N13 C58 C53 110.2(6) . . ? N13 C58 C57 130.5(6) . . ? C53 C58 C57 119.3(7) . . ? O3 Cl1 O2 113.0(9) . . ? O3 Cl1 O1 112.4(9) . . ? O2 Cl1 O1 110.3(8) . . ? O3 Cl1 O4 107.7(8) . . ? O2 Cl1 O4 105.7(8) . . ? O1 Cl1 O4 107.3(8) . . ? O1' Cl1' O3' 110.8(9) . . ? O1' Cl1' O4' 111.1(9) . . ? O3' Cl1' O4' 109.3(9) . . ? O1' Cl1' O2' 107.5(9) . . ? O3' Cl1' O2' 109.9(9) . . ? O4' Cl1' O2' 108.2(9) . . ? O5 Cl2 O7 114.7(9) . . ? O5 Cl2 O6 110.2(9) . . ? O7 Cl2 O6 109.1(8) . . ? O5 Cl2 O8 107.5(8) . . ? O7 Cl2 O8 108.2(8) . . ? O6 Cl2 O8 106.7(9) . . ? O7' Cl2' O6' 112.2(9) . . ? O7' Cl2' O5' 111.0(9) . . ? O6' Cl2' O5' 109.6(9) . . ? O7' Cl2' O8' 107.2(8) . . ? O6' Cl2' O8' 108.0(9) . . ? O5' Cl2' O8' 108.6(9) . . ? O10 Cl3 O9 111.4(8) . . ? O10 Cl3 O11 108.6(7) . . ? O9 Cl3 O11 109.0(8) . . ? O10 Cl3 O12 110.7(8) . . ? O9 Cl3 O12 109.1(7) . . ? O11 Cl3 O12 107.9(8) . . ? O10' Cl3' O11' 111.3(8) . . ? O10' Cl3' O9' 111.1(9) . . ? O11' Cl3' O9' 109.1(8) . . ? O10' Cl3' O12' 108.1(8) . . ? O11' Cl3' O12' 108.4(8) . . ? O9' Cl3' O12' 108.7(8) . . ? O15 Cl4 O13 111.6(9) . . ? O15 Cl4 O14 110.4(8) . . ? O13 Cl4 O14 109.5(7) . . ? O15 Cl4 O16 109.9(8) . . ? O13 Cl4 O16 107.8(8) . . ? O14 Cl4 O16 107.5(8) . . ? O15' Cl4' O13' 111.3(9) . . ? O15' Cl4' O16' 109.2(9) . . ? O13' Cl4' O16' 108.6(9) . . ? O15' Cl4' O14' 110.4(9) . . ? O13' Cl4' O14' 109.2(9) . . ? O16' Cl4' O14' 108.0(9) . . ? H17C O17 H17D 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 N1 C8 31.3(4) . . . . ? N15 Cu1 N1 C8 -32.9(13) . . . . ? N6 Cu1 N1 C8 -116.5(4) . . . . ? N4 Cu1 N1 C8 145.2(4) . . . . ? N2 Cu1 N1 C17 154.0(4) . . . . ? N15 Cu1 N1 C17 89.9(11) . . . . ? N6 Cu1 N1 C17 6.2(4) . . . . ? N4 Cu1 N1 C17 -92.1(4) . . . . ? N2 Cu1 N1 C9 -86.2(3) . . . . ? N15 Cu1 N1 C9 -150.3(10) . . . . ? N6 Cu1 N1 C9 126.0(4) . . . . ? N4 Cu1 N1 C9 27.8(3) . . . . ? N15 Cu1 N2 C7 151.7(4) . . . . ? N6 Cu1 N2 C7 45.2(5) . . . . ? N1 Cu1 N2 C7 -19.3(4) . . . . ? N4 Cu1 N2 C7 -96.0(4) . . . . ? N15 Cu1 N2 C1 -19.2(7) . . . . ? N6 Cu1 N2 C1 -125.6(6) . . . . ? N1 Cu1 N2 C1 169.9(7) . . . . ? N4 Cu1 N2 C1 93.2(6) . . . . ? N2 Cu1 N4 C10 68.7(4) . . . . ? N15 Cu1 N4 C10 171.8(4) . . . . ? N6 Cu1 N4 C10 -89.6(4) . . . . ? N1 Cu1 N4 C10 -7.9(4) . . . . ? N2 Cu1 N4 C16 -140.1(6) . . . . ? N15 Cu1 N4 C16 -37.0(7) . . . . ? N6 Cu1 N4 C16 61.6(7) . . . . ? N1 Cu1 N4 C16 143.3(7) . . . . ? N2 Cu1 N6 C18 -67.6(5) . . . . ? N15 Cu1 N6 C18 -173.6(4) . . . . ? N1 Cu1 N6 C18 -3.6(4) . . . . ? N4 Cu1 N6 C18 76.6(4) . . . . ? N2 Cu1 N6 C24 117.2(6) . . . . ? N15 Cu1 N6 C24 11.2(6) . . . . ? N1 Cu1 N6 C24 -178.9(6) . . . . ? N4 Cu1 N6 C24 -98.7(6) . . . . ? N9 Cu2 N8 C43 148.6(5) . . . . ? N11 Cu2 N8 C43 20.4(4) . . . . ? N13 Cu2 N8 C43 -82.3(5) . . . . ? N9 Cu2 N8 C35 25.8(4) . . . . ? N11 Cu2 N8 C35 -102.4(4) . . . . ? N13 Cu2 N8 C35 154.9(5) . . . . ? N9 Cu2 N8 C51 -92.3(5) . . . . ? N11 Cu2 N8 C51 139.5(5) . . . . ? N13 Cu2 N8 C51 36.9(4) . . . . ? N16 Cu2 N9 C36 159.1(5) . . . . ? N11 Cu2 N9 C36 52.9(5) . . . . ? N13 Cu2 N9 C36 -90.2(5) . . . . ? N8 Cu2 N9 C36 -19.6(5) . . . . ? N16 Cu2 N9 C42 -4.9(6) . . . . ? N11 Cu2 N9 C42 -111.1(6) . . . . ? N13 Cu2 N9 C42 105.7(6) . . . . ? N8 Cu2 N9 C42 176.4(6) . . . . ? N16 Cu2 N11 C44 175.6(4) . . . . ? N9 Cu2 N11 C44 -81.5(4) . . . . ? N13 Cu2 N11 C44 68.9(4) . . . . ? N8 Cu2 N11 C44 -9.4(4) . . . . ? N16 Cu2 N11 C50 5.3(6) . . . . ? N9 Cu2 N11 C50 108.3(6) . . . . ? N13 Cu2 N11 C50 -101.4(6) . . . . ? N8 Cu2 N11 C50 -179.6(6) . . . . ? N16 Cu2 N13 C52 150.5(4) . . . . ? N9 Cu2 N13 C52 44.6(5) . . . . ? N11 Cu2 N13 C52 -105.5(4) . . . . ? N8 Cu2 N13 C52 -26.2(4) . . . . ? N16 Cu2 N13 C58 -15.7(7) . . . . ? N9 Cu2 N13 C58 -121.6(7) . . . . ? N11 Cu2 N13 C58 88.3(7) . . . . ? N8 Cu2 N13 C58 167.6(7) . . . . ? N2 Cu1 N15 C25 108.0(5) . . . . ? N6 Cu1 N15 C25 -106.4(5) . . . . ? N1 Cu1 N15 C25 171.1(9) . . . . ? N4 Cu1 N15 C25 -6.9(6) . . . . ? N2 Cu1 N15 C29 -74.5(5) . . . . ? N6 Cu1 N15 C29 71.1(5) . . . . ? N1 Cu1 N15 C29 -11.4(13) . . . . ? N4 Cu1 N15 C29 170.6(4) . . . . ? N9 Cu2 N16 C32 98.7(5) . . . . ? N11 Cu2 N16 C32 -134.1(5) . . . . ? N13 Cu2 N16 C32 -30.0(5) . . . . ? N9 Cu2 N16 C33 -68.6(4) . . . . ? N11 Cu2 N16 C33 58.6(4) . . . . ? N13 Cu2 N16 C33 162.7(4) . . . . ? C7 N2 C1 C6 0.1(7) . . . . ? Cu1 N2 C1 C6 171.4(5) . . . . ? C7 N2 C1 C2 179.2(7) . . . . ? Cu1 N2 C1 C2 -9.5(11) . . . . ? C6 C1 C2 C3 0.4(11) . . . . ? N2 C1 C2 C3 -178.6(7) . . . . ? C1 C2 C3 C4 1.4(13) . . . . ? C2 C3 C4 C5 -1.9(17) . . . . ? C3 C4 C5 C6 0.5(17) . . . . ? N2 C1 C6 N3 0.6(7) . . . . ? C2 C1 C6 N3 -178.6(6) . . . . ? N2 C1 C6 C5 177.4(7) . . . . ? C2 C1 C6 C5 -1.8(11) . . . . ? C7 N3 C6 C1 -1.1(7) . . . . ? C7 N3 C6 C5 -177.5(8) . . . . ? C4 C5 C6 C1 1.3(14) . . . . ? C4 C5 C6 N3 177.3(9) . . . . ? C6 N3 C7 N2 1.2(7) . . . . ? C6 N3 C7 C8 -176.7(6) . . . . ? C1 N2 C7 N3 -0.8(6) . . . . ? Cu1 N2 C7 N3 -175.1(4) . . . . ? C1 N2 C7 C8 177.2(5) . . . . ? Cu1 N2 C7 C8 2.9(7) . . . . ? C17 N1 C8 C7 -157.2(5) . . . . ? C9 N1 C8 C7 78.1(5) . . . . ? Cu1 N1 C8 C7 -35.9(5) . . . . ? N3 C7 C8 N1 -158.3(6) . . . . ? N2 C7 C8 N1 24.0(7) . . . . ? C8 N1 C9 C10 -156.6(5) . . . . ? C17 N1 C9 C10 77.4(6) . . . . ? Cu1 N1 C9 C10 -42.3(5) . . . . ? C16 N4 C10 N5 -0.4(6) . . . . ? Cu1 N4 C10 N5 163.1(4) . . . . ? C16 N4 C10 C9 -179.4(5) . . . . ? Cu1 N4 C10 C9 -15.9(6) . . . . ? C11 N5 C10 N4 -1.8(7) . . . . ? C11 N5 C10 C9 177.1(6) . . . . ? N1 C9 C10 N4 41.7(7) . . . . ? N1 C9 C10 N5 -137.1(5) . . . . ? C10 N5 C11 C12 -174.2(7) . . . . ? C10 N5 C11 C16 3.2(6) . . . . ? N5 C11 C12 C13 176.8(6) . . . . ? C16 C11 C12 C13 -0.2(10) . . . . ? C11 C12 C13 C14 0.0(11) . . . . ? C12 C13 C14 C15 -0.1(12) . . . . ? C13 C14 C15 C16 0.2(10) . . . . ? C10 N4 C16 C11 2.5(6) . . . . ? Cu1 N4 C16 C11 -148.8(5) . . . . ? C10 N4 C16 C15 175.2(6) . . . . ? Cu1 N4 C16 C15 23.9(11) . . . . ? N5 C11 C16 N4 -3.5(6) . . . . ? C12 C11 C16 N4 174.1(6) . . . . ? N5 C11 C16 C15 -177.3(5) . . . . ? C12 C11 C16 C15 0.3(9) . . . . ? C14 C15 C16 N4 -172.5(6) . . . . ? C14 C15 C16 C11 -0.4(8) . . . . ? C8 N1 C17 C18 111.3(5) . . . . ? C9 N1 C17 C18 -124.0(5) . . . . ? Cu1 N1 C17 C18 -7.4(6) . . . . ? C24 N6 C18 N7 0.6(6) . . . . ? Cu1 N6 C18 N7 -176.3(4) . . . . ? C24 N6 C18 C17 177.0(6) . . . . ? Cu1 N6 C18 C17 0.1(7) . . . . ? C19 N7 C18 N6 -0.3(7) . . . . ? C19 N7 C18 C17 -176.8(6) . . . . ? N1 C17 C18 N6 5.2(8) . . . . ? N1 C17 C18 N7 -178.8(5) . . . . ? C18 N7 C19 C20 176.6(7) . . . . ? C18 N7 C19 C24 -0.1(6) . . . . ? C24 C19 C20 C21 -0.7(10) . . . . ? N7 C19 C20 C21 -176.8(6) . . . . ? C19 C20 C21 C22 0.6(11) . . . . ? C20 C21 C22 C23 -0.4(12) . . . . ? C21 C22 C23 C24 0.2(10) . . . . ? C22 C23 C24 N6 176.0(6) . . . . ? C22 C23 C24 C19 -0.2(9) . . . . ? C18 N6 C24 C23 -177.2(6) . . . . ? Cu1 N6 C24 C23 -1.7(11) . . . . ? C18 N6 C24 C19 -0.7(6) . . . . ? Cu1 N6 C24 C19 174.8(4) . . . . ? C20 C19 C24 C23 0.5(10) . . . . ? N7 C19 C24 C23 177.5(5) . . . . ? C20 C19 C24 N6 -176.5(6) . . . . ? N7 C19 C24 N6 0.4(6) . . . . ? C29 N15 C25 C26 -6.4(10) . . . . ? Cu1 N15 C25 C26 171.0(5) . . . . ? N15 C25 C26 C27 1.3(10) . . . . ? C25 C26 C27 C28 2.9(10) . . . . ? C25 C26 C27 C30 -176.2(6) . . . . ? C26 C27 C28 C29 -2.0(9) . . . . ? C30 C27 C28 C29 177.0(6) . . . . ? C25 N15 C29 C28 7.4(9) . . . . ? Cu1 N15 C29 C28 -170.3(5) . . . . ? C27 C28 C29 N15 -3.2(10) . . . . ? C26 C27 C30 C34 -36.2(9) . . . . ? C28 C27 C30 C34 144.7(6) . . . . ? C26 C27 C30 C31 147.6(6) . . . . ? C28 C27 C30 C31 -31.5(9) . . . . ? C34 C30 C31 C32 0.6(9) . . . . ? C27 C30 C31 C32 177.0(6) . . . . ? C33 N16 C32 C31 1.9(9) . . . . ? Cu2 N16 C32 C31 -165.4(5) . . . . ? C30 C31 C32 N16 -1.7(10) . . . . ? C32 N16 C33 C34 -1.2(8) . . . . ? Cu2 N16 C33 C34 166.8(5) . . . . ? C31 C30 C34 C33 0.1(9) . . . . ? C27 C30 C34 C33 -176.2(5) . . . . ? N16 C33 C34 C30 0.2(9) . . . . ? C43 N8 C35 C36 -148.3(5) . . . . ? C51 N8 C35 C36 85.5(6) . . . . ? Cu2 N8 C35 C36 -27.3(6) . . . . ? C42 N9 C36 N10 -0.3(8) . . . . ? Cu2 N9 C36 N10 -169.6(5) . . . . ? C42 N9 C36 C35 178.3(6) . . . . ? Cu2 N9 C36 C35 9.0(8) . . . . ? C37 N10 C36 N9 2.2(8) . . . . ? C37 N10 C36 C35 -176.3(6) . . . . ? N8 C35 C36 N9 13.4(9) . . . . ? N8 C35 C36 N10 -168.2(6) . . . . ? C36 N10 C37 C38 177.2(4) . . . . ? C36 N10 C37 C42 -3.1(6) . . . . ? N10 C37 C38 C39 179.7(7) . . . . ? C42 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C40 0.0 . . . . ? C38 C39 C40 C41 0.0 . . . . ? C39 C40 C41 C42 0.0 . . . . ? C36 N9 C42 C41 -178.5(4) . . . . ? Cu2 N9 C42 C41 -13.6(9) . . . . ? C36 N9 C42 C37 -1.7(5) . . . . ? Cu2 N9 C42 C37 163.2(5) . . . . ? C40 C41 C42 N9 176.5(6) . . . . ? C40 C41 C42 C37 0.0 . . . . ? N10 C37 C42 N9 2.9(5) . . . . ? C38 C37 C42 N9 -177.3(4) . . . . ? N10 C37 C42 C41 -179.8(5) . . . . ? C38 C37 C42 C41 0.0 . . . . ? C35 N8 C43 C44 93.8(6) . . . . ? C51 N8 C43 C44 -140.3(5) . . . . ? Cu2 N8 C43 C44 -26.5(6) . . . . ? C50 N11 C44 N12 -2.4(7) . . . . ? Cu2 N11 C44 N12 -176.4(4) . . . . ? C50 N11 C44 C43 170.1(6) . . . . ? Cu2 N11 C44 C43 -3.9(7) . . . . ? C45 N12 C44 N11 2.3(7) . . . . ? C45 N12 C44 C43 -170.0(6) . . . . ? N8 C43 C44 N11 21.3(9) . . . . ? N8 C43 C44 N12 -167.0(6) . . . . ? C44 N12 C45 C50 -1.2(7) . . . . ? C44 N12 C45 C46 176.4(7) . . . . ? N12 C45 C46 C47 -174.1(7) . . . . ? C50 C45 C46 C47 3.2(10) . . . . ? C45 C46 C47 C48 -3.2(11) . . . . ? C46 C47 C48 C49 1.5(12) . . . . ? C47 C48 C49 C50 0.5(11) . . . . ? N12 C45 C50 N11 -0.2(6) . . . . ? C46 C45 C50 N11 -178.1(6) . . . . ? N12 C45 C50 C49 176.6(5) . . . . ? C46 C45 C50 C49 -1.3(9) . . . . ? C44 N11 C50 C45 1.6(6) . . . . ? Cu2 N11 C50 C45 172.1(5) . . . . ? C44 N11 C50 C49 -174.8(6) . . . . ? Cu2 N11 C50 C49 -4.2(11) . . . . ? C48 C49 C50 C45 -0.5(9) . . . . ? C48 C49 C50 N11 175.4(6) . . . . ? C43 N8 C51 C52 76.3(6) . . . . ? C35 N8 C51 C52 -157.2(6) . . . . ? Cu2 N8 C51 C52 -41.3(6) . . . . ? C58 N13 C52 N14 -0.5(7) . . . . ? Cu2 N13 C52 N14 -172.3(4) . . . . ? C58 N13 C52 C51 -179.4(6) . . . . ? Cu2 N13 C52 C51 8.8(7) . . . . ? C53 N14 C52 N13 1.4(7) . . . . ? C53 N14 C52 C51 -179.7(7) . . . . ? N8 C51 C52 N13 23.3(9) . . . . ? N8 C51 C52 N14 -155.5(6) . . . . ? C52 N14 C53 C54 179.8(7) . . . . ? C52 N14 C53 C58 -1.6(7) . . . . ? C58 C53 C54 C55 2.4(11) . . . . ? N14 C53 C54 C55 -179.3(8) . . . . ? C53 C54 C55 C56 -4.3(14) . . . . ? C54 C55 C56 C57 3.4(14) . . . . ? C55 C56 C57 C58 -0.2(11) . . . . ? C52 N13 C58 C53 -0.6(7) . . . . ? Cu2 N13 C58 C53 165.7(5) . . . . ? C52 N13 C58 C57 179.1(7) . . . . ? Cu2 N13 C58 C57 -14.6(12) . . . . ? C54 C53 C58 N13 -179.9(6) . . . . ? N14 C53 C58 N13 1.4(7) . . . . ? C54 C53 C58 C57 0.4(10) . . . . ? N14 C53 C58 C57 -178.3(6) . . . . ? C56 C57 C58 N13 178.9(6) . . . . ? C56 C57 C58 C53 -1.5(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O17 0.86 2.07 2.898(8) 162.4 2_667 N5 H5A O11 0.86 2.08 2.936(13) 178.6 1_545 N10 H10A O8 0.86 2.15 2.95(3) 155.6 2_766 N12 H12A O9 0.86 2.23 2.944(17) 140.8 2_766 N14 H14A O17 0.86 2.00 2.849(8) 168.1 1_654 O17 H17C O14 0.82 2.10 2.850(15) 152.1 1_556 C29 H29 O4 0.93 2.58 3.33(2) 137.2 2_666 C32 H32 O3 0.93 2.49 3.08(2) 121.5 1_655 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.756 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.091 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.500 584 113 ' ' _platon_squeeze_details ; For the residual electron densities, only water O17 molecule can be assigned unambiguously. For the other residual electron densities, which should be considered as peaks from disordered water molecules, did not give a chemical meaningful result after a carefull refinement. Therefor, the contributions of the disordered solvent molecules (c.a. 113 e/unit cell) were removed from the diffraction data using the SQUEEZE routine of PLATON software and then final refinements were carried out. These electon densities account to ca. eleven water molecules, i.e. the suitable moiety formula should be Cu~2~C~58~H~50~N~16~.(Cl O~4~)~4~.(H~2~O)~6.5~ . ; # start Validation Reply Form _vrf_PLAT420_3 ; PROBLEM: D-H Without Acceptor O17 - H17D ... ? RESPONSE: The hydrogen acceptor may come largely from the water molecules. However, the densities of these solvent molecules are too diffuse to allow accurate refinement for unit water molecule. Then, these disordered water molecules were treated using the SQUEEZE routine from PLATON. ; data_4 #TrackingRef '- 1-9.cif' _database_code_depnum_ccdc_archive 'CCDC 788588' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cu2 C52 H44 N14 O4, 2(Cl O4), 8(H2 O)' _chemical_formula_sum 'C52 H60 Cl2 Cu2 N14 O20' _chemical_formula_weight 1399.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8077(6) _cell_length_b 11.9857(6) _cell_length_c 13.8019(7) _cell_angle_alpha 112.315(2) _cell_angle_beta 98.880(1) _cell_angle_gamma 100.592(1) _cell_volume 1575.62(14) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2853 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 23.12 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 722 _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8740 _exptl_absorpt_correction_T_max 0.9512 _exptl_absorpt_process_details 'SADABS,(Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo k\a' _diffrn_radiation_source 'fine focus sealed Siemens Mo tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex CCD area-detector' _diffrn_measurement_method '0.3\% wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25694 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6445 _reflns_number_gt 5468 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART,(Version 5.628)2001' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+,(Version 6.45)2001 ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material PLATON _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. The Cl1/O3-O6 perchlorate ion and water O10 are both are both of 0.56(1):0.44(1) for the major and minor components, respectively. Command 'DFIX' was used to restrain the some bond lengths. ; _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^)+(0.0640P)^2^+2.3095P] 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 6445 _refine_ls_number_parameters 483 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1441 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.93545(4) 0.70068(3) 0.65088(3) 0.03319(13) Uani 1 1 d . . . C1 C 1.2310(3) 0.8377(3) 0.7789(3) 0.0467(8) Uani 1 1 d . . . H1A H 1.2996 0.8908 0.7658 0.056 Uiso 1 1 calc R . . H1B H 1.2701 0.8159 0.8350 0.056 Uiso 1 1 calc R . . C2 C 1.1359(3) 0.9089(3) 0.8174(3) 0.0356(7) Uani 1 1 d . . . C3 C 0.9579(3) 0.9635(3) 0.8352(2) 0.0337(7) Uani 1 1 d . . . C4 C 0.8309(4) 0.9718(3) 0.8256(3) 0.0432(8) Uani 1 1 d . . . H4 H 0.7627 0.9081 0.7725 0.052 Uiso 1 1 calc R . . C5 C 0.8100(4) 1.0790(4) 0.8987(3) 0.0517(9) Uani 1 1 d . . . H5 H 0.7256 1.0869 0.8954 0.062 Uiso 1 1 calc R . . C6 C 0.9117(4) 1.1751(3) 0.9767(3) 0.0515(10) Uani 1 1 d . . . H6 H 0.8932 1.2459 1.0236 0.062 Uiso 1 1 calc R . . C7 C 1.0379(4) 1.1698(3) 0.9873(3) 0.0495(9) Uani 1 1 d . . . H7 H 1.1055 1.2346 1.0401 0.059 Uiso 1 1 calc R . . C8 C 1.0593(3) 1.0613(3) 0.9141(3) 0.0371(7) Uani 1 1 d . . . C9 C 1.1860(3) 0.6102(3) 0.6932(3) 0.0404(7) Uani 1 1 d . . . H9A H 1.2696 0.6278 0.7413 0.048 Uiso 1 1 calc R . . H9B H 1.1822 0.5446 0.6238 0.048 Uiso 1 1 calc R . . C10 C 1.0795(3) 0.5676(3) 0.7388(3) 0.0372(7) Uani 1 1 d . . . C11 C 0.8930(3) 0.5328(3) 0.7768(3) 0.0387(7) Uani 1 1 d . . . C12 C 0.7686(4) 0.5302(4) 0.7917(3) 0.0501(9) Uani 1 1 d . . . H12 H 0.7189 0.5752 0.7686 0.060 Uiso 1 1 calc R . . C13 C 0.7217(5) 0.4575(4) 0.8425(4) 0.0661(12) Uani 1 1 d . . . H13 H 0.6387 0.4535 0.8538 0.079 Uiso 1 1 calc R . . C14 C 0.7959(5) 0.3905(5) 0.8770(5) 0.0778(15) Uani 1 1 d . . . H14 H 0.7609 0.3425 0.9105 0.093 Uiso 1 1 calc R . . C15 C 0.9186(5) 0.3928(5) 0.8633(4) 0.0691(13) Uani 1 1 d . . . H15 H 0.9679 0.3479 0.8870 0.083 Uiso 1 1 calc R . . C16 C 0.9663(4) 0.4654(4) 0.8122(3) 0.0479(9) Uani 1 1 d . . . C17 C 1.2006(3) 0.7302(4) 0.5814(3) 0.0450(8) Uani 1 1 d . . . H17A H 1.2063 0.6490 0.5326 0.054 Uiso 1 1 calc R . . H17B H 1.2839 0.7899 0.5999 0.054 Uiso 1 1 calc R . . C18 C 1.0977(3) 0.7689(3) 0.5262(3) 0.0387(7) Uani 1 1 d . . . C19 C 0.9138(4) 0.8029(3) 0.4735(3) 0.0422(8) Uani 1 1 d . . . C20 C 0.7894(4) 0.8174(4) 0.4602(3) 0.0565(10) Uani 1 1 d . . . H20 H 0.7344 0.7994 0.5010 0.068 Uiso 1 1 calc R . . C21 C 0.7501(5) 0.8601(5) 0.3834(4) 0.0714(13) Uani 1 1 d . . . H21 H 0.6669 0.8711 0.3723 0.086 Uiso 1 1 calc R . . C22 C 0.8326(6) 0.8869(5) 0.3224(4) 0.0790(15) Uani 1 1 d . . . H22 H 0.8025 0.9140 0.2706 0.095 Uiso 1 1 calc R . . C23 C 0.9570(5) 0.8744(4) 0.3363(4) 0.0690(13) Uani 1 1 d . . . H23 H 1.0120 0.8934 0.2959 0.083 Uiso 1 1 calc R . . C24 C 0.9970(4) 0.8320(4) 0.4136(3) 0.0495(9) Uani 1 1 d . . . C25 C 0.6849(3) 0.5894(3) 0.5626(3) 0.0414(8) Uani 1 1 d . . . C26 C 0.5608(4) 0.4891(4) 0.4867(4) 0.0724(15) Uani 1 1 d . . . H26 H 0.5629 0.4189 0.4277 0.087 Uiso 1 1 calc R . . Cl1 Cl 0.50491(10) 0.76079(12) 0.00945(10) 0.0677(3) Uani 1 1 d D . . N1 N 1.1717(3) 0.7234(2) 0.6797(2) 0.0345(6) Uani 1 1 d . . . N2 N 1.0103(2) 0.8690(2) 0.7763(2) 0.0332(6) Uani 1 1 d . . . N3 N 1.1713(3) 1.0232(3) 0.9001(2) 0.0392(6) Uani 1 1 d D . . H3A H 1.246(2) 1.068(3) 0.935(3) 0.047 Uiso 1 1 d D . . N4 N 0.9683(3) 0.5972(2) 0.7310(2) 0.0349(6) Uani 1 1 d . . . N5 N 1.0847(3) 0.4903(3) 0.7880(3) 0.0466(7) Uani 1 1 d D . . H5A H 1.151(3) 0.468(4) 0.807(3) 0.056 Uiso 1 1 d D . . N6 N 0.9805(3) 0.7629(3) 0.5435(2) 0.0388(6) Uani 1 1 d . . . N7 N 1.1118(3) 0.8094(3) 0.4487(3) 0.0483(7) Uani 1 1 d D . . H7A H 1.183(3) 0.820(4) 0.432(3) 0.058 Uiso 1 1 d D . . O1 O 0.7884(2) 0.5655(2) 0.54461(19) 0.0435(6) Uani 1 1 d . . . O2 O 0.6785(2) 0.6852(3) 0.6355(2) 0.0584(7) Uani 1 1 d . . . O3 O 0.3725(3) 0.7325(4) -0.0373(3) 0.0883(11) Uani 1 1 d D A . O4 O 0.5189(10) 0.6521(12) 0.0220(11) 0.131(4) Uani 0.56 1 d P A 1 O5 O 0.5890(10) 0.7868(11) -0.0485(8) 0.096(3) Uani 0.56 1 d P A 1 O6 O 0.5397(13) 0.8650(17) 0.1147(10) 0.157(7) Uani 0.56 1 d P A 1 O4' O 0.5508(14) 0.6591(13) -0.0402(19) 0.266(16) Uani 0.44 1 d PD A 2 O5' O 0.5639(10) 0.8541(12) -0.0244(12) 0.114(6) Uani 0.44 1 d PD A 2 O6' O 0.5345(15) 0.805(2) 0.1146(8) 0.192(14) Uani 0.44 1 d PD A 2 O7 O 0.5032(3) 0.7989(4) 0.7332(3) 0.0800(10) Uani 1 1 d D . . H7C H 0.554(5) 0.762(6) 0.702(4) 0.120 Uiso 1 1 d D . . H7D H 0.525(6) 0.806(6) 0.798(2) 0.120 Uiso 1 1 d D . . O8 O 0.3111(6) 0.4272(5) 0.8423(5) 0.139(2) Uani 1 1 d D . . H8A H 0.365(8) 0.484(7) 0.895(5) 0.209 Uiso 1 1 d D . . H8B H 0.272(9) 0.378(8) 0.863(8) 0.209 Uiso 1 1 d D . . O9 O 0.3514(6) 0.8335(6) 0.3891(6) 0.145(2) Uani 1 1 d D . . H9C H 0.382(11) 0.892(7) 0.450(4) 0.218 Uiso 1 1 d D . . H9D H 0.314(11) 0.860(10) 0.349(7) 0.218 Uiso 1 1 d D . . O10 O 0.4917(9) 0.9914(13) 0.3122(13) 0.134(4) Uani 0.56 1 d PD B 1 H10A H 0.431(11) 0.933(10) 0.302(17) 0.201 Uiso 0.56 1 d PD C 1 H10B H 0.472(17) 1.058(8) 0.334(18) 0.201 Uiso 0.56 1 d PD D 1 O10' O 0.4766(12) 1.0743(15) 0.4046(11) 0.122(4) Uani 0.44 1 d PD E 2 H10D H 0.484(19) 1.146(7) 0.448(16) 0.183 Uiso 0.44 1 d PD F 2 H10C H 0.405(10) 1.028(14) 0.393(17) 0.183 Uiso 0.44 1 d PD G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0286(2) 0.0333(2) 0.0313(2) 0.01252(16) 0.00191(15) 0.00037(15) C1 0.0309(17) 0.048(2) 0.048(2) 0.0114(17) 0.0035(15) 0.0050(15) C2 0.0351(16) 0.0370(17) 0.0328(16) 0.0163(14) 0.0055(13) 0.0038(13) C3 0.0384(17) 0.0326(16) 0.0310(15) 0.0147(13) 0.0095(13) 0.0078(13) C4 0.044(2) 0.0385(18) 0.0443(19) 0.0148(15) 0.0115(15) 0.0108(15) C5 0.059(2) 0.050(2) 0.056(2) 0.0245(19) 0.0234(19) 0.0241(19) C6 0.081(3) 0.0349(18) 0.043(2) 0.0143(16) 0.0201(19) 0.0261(19) C7 0.070(3) 0.0326(18) 0.0373(19) 0.0113(15) 0.0080(17) 0.0066(17) C8 0.0453(19) 0.0329(16) 0.0323(16) 0.0170(13) 0.0065(14) 0.0036(14) C9 0.0339(17) 0.0430(18) 0.0469(19) 0.0197(16) 0.0120(14) 0.0131(14) C10 0.0368(17) 0.0364(17) 0.0377(17) 0.0157(14) 0.0081(14) 0.0088(13) C11 0.0423(18) 0.0301(16) 0.0369(17) 0.0105(13) 0.0091(14) 0.0027(13) C12 0.044(2) 0.046(2) 0.060(2) 0.0216(18) 0.0175(18) 0.0082(16) C13 0.058(3) 0.067(3) 0.081(3) 0.037(3) 0.035(2) 0.008(2) C14 0.083(4) 0.081(3) 0.101(4) 0.065(3) 0.042(3) 0.021(3) C15 0.075(3) 0.070(3) 0.092(4) 0.059(3) 0.031(3) 0.023(2) C16 0.051(2) 0.045(2) 0.053(2) 0.0251(17) 0.0154(17) 0.0108(16) C17 0.0400(19) 0.057(2) 0.047(2) 0.0277(18) 0.0187(16) 0.0132(16) C18 0.0394(18) 0.0374(17) 0.0365(17) 0.0151(14) 0.0100(14) 0.0039(14) C19 0.0449(19) 0.0430(19) 0.0377(18) 0.0197(15) 0.0040(15) 0.0085(15) C20 0.052(2) 0.062(3) 0.055(2) 0.031(2) 0.0037(18) 0.0114(19) C21 0.068(3) 0.074(3) 0.076(3) 0.044(3) -0.004(2) 0.021(2) C22 0.095(4) 0.074(3) 0.074(3) 0.051(3) -0.003(3) 0.013(3) C23 0.084(3) 0.070(3) 0.061(3) 0.045(2) 0.011(2) 0.007(2) C24 0.058(2) 0.046(2) 0.042(2) 0.0219(17) 0.0061(17) 0.0046(17) C25 0.0334(18) 0.0394(18) 0.0383(18) 0.0082(15) 0.0034(14) 0.0017(14) C26 0.0264(18) 0.064(3) 0.073(3) -0.019(2) 0.0050(18) -0.0003(17) Cl1 0.0415(5) 0.0788(8) 0.0813(8) 0.0399(6) 0.0053(5) 0.0070(5) N1 0.0306(13) 0.0388(14) 0.0340(14) 0.0151(12) 0.0091(11) 0.0084(11) N2 0.0318(13) 0.0315(13) 0.0324(13) 0.0111(11) 0.0069(11) 0.0050(11) N3 0.0369(15) 0.0338(14) 0.0346(15) 0.0094(12) 0.0016(12) -0.0018(12) N4 0.0316(14) 0.0373(14) 0.0367(14) 0.0182(12) 0.0064(11) 0.0071(11) N5 0.0457(18) 0.0486(18) 0.0538(18) 0.0288(15) 0.0113(14) 0.0169(14) N6 0.0356(15) 0.0448(16) 0.0355(14) 0.0197(13) 0.0055(11) 0.0062(12) N7 0.0474(18) 0.0557(19) 0.0460(17) 0.0283(15) 0.0153(14) 0.0052(15) O1 0.0291(12) 0.0426(13) 0.0419(13) 0.0058(11) 0.0038(10) 0.0007(10) O2 0.0345(13) 0.0492(15) 0.0624(17) -0.0031(13) 0.0093(12) 0.0042(11) O3 0.0480(18) 0.114(3) 0.097(3) 0.047(2) 0.0053(18) 0.0130(19) O4 0.101(7) 0.142(10) 0.192(12) 0.116(10) 0.008(7) 0.051(6) O5 0.073(5) 0.119(8) 0.076(5) 0.033(6) 0.023(4) -0.009(6) O6 0.104(8) 0.155(11) 0.106(9) -0.030(7) 0.030(6) -0.028(7) O4' 0.24(2) 0.22(2) 0.44(4) 0.15(3) 0.20(3) 0.19(2) O5' 0.078(8) 0.110(10) 0.128(12) 0.072(10) -0.033(7) -0.038(7) O6' 0.167(16) 0.27(3) 0.074(10) 0.086(16) -0.053(9) -0.047(16) O7 0.0536(19) 0.101(3) 0.075(2) 0.023(2) 0.0169(17) 0.0283(18) O8 0.103(4) 0.089(3) 0.188(5) 0.036(3) -0.029(4) 0.042(3) O9 0.102(4) 0.170(5) 0.171(5) 0.075(5) 0.068(4) 0.017(4) O10 0.084(6) 0.178(10) 0.184(11) 0.125(10) 0.028(7) 0.034(6) O10' 0.089(8) 0.168(13) 0.101(9) 0.068(9) 0.014(7) -0.002(8) _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 O1 1.957(2) . ? Cu1 N6 1.979(3) . ? Cu1 N4 1.993(3) . ? Cu1 N2 2.009(3) . ? Cu1 N1 2.470(3) . ? C1 N1 1.464(4) . ? C1 C2 1.488(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.308(4) . ? C2 N3 1.345(4) . ? C3 C4 1.384(5) . ? C3 N2 1.394(4) . ? C3 C8 1.396(4) . ? C4 C5 1.383(5) . ? C4 H4 0.9300 . ? C5 C6 1.386(6) . ? C5 H5 0.9300 . ? C6 C7 1.364(6) . ? C6 H6 0.9300 . ? C7 C8 1.397(5) . ? C7 H7 0.9300 . ? C8 N3 1.385(5) . ? C9 N1 1.469(4) . ? C9 C10 1.494(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.314(4) . ? C10 N5 1.344(4) . ? C11 C12 1.387(5) . ? C11 C16 1.392(5) . ? C11 N4 1.399(4) . ? C12 C13 1.386(6) . ? C12 H12 0.9300 . ? C13 C14 1.386(7) . ? C13 H13 0.9300 . ? C14 C15 1.365(7) . ? C14 H14 0.9300 . ? C15 C16 1.391(5) . ? C15 H15 0.9300 . ? C16 N5 1.380(5) . ? C17 N1 1.467(4) . ? C17 C18 1.493(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.318(4) . ? C18 N7 1.351(4) . ? C19 C20 1.381(6) . ? C19 C24 1.395(5) . ? C19 N6 1.396(4) . ? C20 C21 1.385(6) . ? C20 H20 0.9300 . ? C21 C22 1.393(7) . ? C21 H21 0.9300 . ? C22 C23 1.372(7) . ? C22 H22 0.9300 . ? C23 C24 1.391(5) . ? C23 H23 0.9300 . ? C24 N7 1.373(5) . ? C25 O2 1.229(4) . ? C25 O1 1.243(4) . ? C25 C26 1.536(5) . ? C26 C26 1.459(8) 2_666 ? C26 H26 0.9300 . ? Cl1 O6' 1.304(10) . ? Cl1 O5 1.368(9) . ? Cl1 O4' 1.377(10) . ? Cl1 O3 1.396(3) . ? Cl1 O4 1.408(10) . ? Cl1 O6 1.447(13) . ? Cl1 O5' 1.451(9) . ? N3 H3A 0.836(19) . ? N5 H5A 0.85(4) . ? N7 H7A 0.84(4) . ? O7 H7C 0.84(6) . ? O7 H7D 0.851(19) . ? O8 H8A 0.82(8) . ? O8 H8B 0.83(10) . ? O9 H9C 0.83(6) . ? O9 H9D 0.83(11) . ? O10 H10A 0.82(2) . ? O10 H10B 0.82(2) . ? O10' H10B 0.9(2) . ? O10' H10D 0.82(2) . ? O10' H10C 0.81(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N6 92.90(11) . . ? O1 Cu1 N4 91.33(11) . . ? N6 Cu1 N4 147.89(12) . . ? O1 Cu1 N2 151.84(11) . . ? N6 Cu1 N2 93.75(11) . . ? N4 Cu1 N2 97.36(11) . . ? O1 Cu1 N1 130.96(9) . . ? N6 Cu1 N1 77.26(10) . . ? N4 Cu1 N1 76.01(10) . . ? N2 Cu1 N1 77.20(10) . . ? N1 C1 C2 112.7(3) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? N2 C2 N3 112.4(3) . . ? N2 C2 C1 124.8(3) . . ? N3 C2 C1 122.8(3) . . ? C4 C3 N2 130.9(3) . . ? C4 C3 C8 120.7(3) . . ? N2 C3 C8 108.4(3) . . ? C5 C4 C3 117.0(3) . . ? C5 C4 H4 121.5 . . ? C3 C4 H4 121.5 . . ? C4 C5 C6 121.7(4) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 122.6(3) . . ? C7 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? C6 C7 C8 115.9(3) . . ? C6 C7 H7 122.0 . . ? C8 C7 H7 122.0 . . ? N3 C8 C3 105.5(3) . . ? N3 C8 C7 132.3(3) . . ? C3 C8 C7 122.2(3) . . ? N1 C9 C10 109.6(3) . . ? N1 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? N1 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? N4 C10 N5 112.6(3) . . ? N4 C10 C9 123.6(3) . . ? N5 C10 C9 123.7(3) . . ? C12 C11 C16 120.8(3) . . ? C12 C11 N4 131.2(3) . . ? C16 C11 N4 107.9(3) . . ? C13 C12 C11 117.0(4) . . ? C13 C12 H12 121.5 . . ? C11 C12 H12 121.5 . . ? C14 C13 C12 121.5(4) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C15 C14 C13 122.2(4) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 C15 C16 116.8(4) . . ? C14 C15 H15 121.6 . . ? C16 C15 H15 121.6 . . ? N5 C16 C15 131.8(4) . . ? N5 C16 C11 106.4(3) . . ? C15 C16 C11 121.8(4) . . ? N1 C17 C18 110.9(3) . . ? N1 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? N6 C18 N7 111.7(3) . . ? N6 C18 C17 124.5(3) . . ? N7 C18 C17 123.7(3) . . ? C20 C19 C24 121.5(3) . . ? C20 C19 N6 130.4(3) . . ? C24 C19 N6 108.1(3) . . ? C19 C20 C21 117.0(4) . . ? C19 C20 H20 121.5 . . ? C21 C20 H20 121.5 . . ? C20 C21 C22 121.3(5) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C21 122.0(4) . . ? C23 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C22 C23 C24 116.9(4) . . ? C22 C23 H23 121.6 . . ? C24 C23 H23 121.6 . . ? N7 C24 C23 132.6(4) . . ? N7 C24 C19 106.1(3) . . ? C23 C24 C19 121.3(4) . . ? O2 C25 O1 124.0(3) . . ? O2 C25 C26 120.6(3) . . ? O1 C25 C26 115.4(3) . . ? C26 C26 C25 115.8(4) 2_666 . ? C26 C26 H26 122.1 2_666 . ? C25 C26 H26 122.1 . . ? C1 N1 C17 114.8(3) . . ? C1 N1 C9 112.6(3) . . ? C17 N1 C9 115.3(3) . . ? C1 N1 Cu1 105.27(19) . . ? C17 N1 Cu1 103.89(19) . . ? C9 N1 Cu1 103.23(18) . . ? C2 N2 C3 106.2(3) . . ? C2 N2 Cu1 119.3(2) . . ? C3 N2 Cu1 134.4(2) . . ? C2 N3 C8 107.5(3) . . ? C2 N3 H3A 128(3) . . ? C8 N3 H3A 124(3) . . ? C10 N4 C11 106.0(3) . . ? C10 N4 Cu1 119.1(2) . . ? C11 N4 Cu1 134.6(2) . . ? C10 N5 C16 107.0(3) . . ? C10 N5 H5A 126(3) . . ? C16 N5 H5A 126(3) . . ? C18 N6 C19 106.3(3) . . ? C18 N6 Cu1 118.9(2) . . ? C19 N6 Cu1 134.8(2) . . ? C18 N7 C24 107.8(3) . . ? C18 N7 H7A 121(3) . . ? C24 N7 H7A 131(3) . . ? C25 O1 Cu1 109.7(2) . . ? H7C O7 H7D 105(3) . . ? H8A O8 H8B 108(9) . . ? H9C O9 H9D 108(9) . . ? H10A O10 H10B 111(4) . . ? H10B O10' H10D 120(10) . . ? H10B O10' H10C 95(10) . . ? H10D O10' H10C 112(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 7.6(5) . . . . ? N1 C1 C2 N3 -172.7(3) . . . . ? N2 C3 C4 C5 179.1(3) . . . . ? C8 C3 C4 C5 -1.4(5) . . . . ? C3 C4 C5 C6 1.2(5) . . . . ? C4 C5 C6 C7 -0.7(6) . . . . ? C5 C6 C7 C8 0.3(5) . . . . ? C4 C3 C8 N3 -179.2(3) . . . . ? N2 C3 C8 N3 0.4(3) . . . . ? C4 C3 C8 C7 1.1(5) . . . . ? N2 C3 C8 C7 -179.3(3) . . . . ? C6 C7 C8 N3 179.9(3) . . . . ? C6 C7 C8 C3 -0.5(5) . . . . ? N1 C9 C10 N4 22.5(5) . . . . ? N1 C9 C10 N5 -160.7(3) . . . . ? C16 C11 C12 C13 -0.3(6) . . . . ? N4 C11 C12 C13 -178.8(4) . . . . ? C11 C12 C13 C14 0.0(7) . . . . ? C12 C13 C14 C15 0.3(9) . . . . ? C13 C14 C15 C16 -0.4(8) . . . . ? C14 C15 C16 N5 178.4(5) . . . . ? C14 C15 C16 C11 0.1(7) . . . . ? C12 C11 C16 N5 -178.5(3) . . . . ? N4 C11 C16 N5 0.3(4) . . . . ? C12 C11 C16 C15 0.2(6) . . . . ? N4 C11 C16 C15 179.0(4) . . . . ? N1 C17 C18 N6 -18.2(5) . . . . ? N1 C17 C18 N7 164.8(3) . . . . ? C24 C19 C20 C21 1.1(6) . . . . ? N6 C19 C20 C21 179.7(4) . . . . ? C19 C20 C21 C22 0.1(7) . . . . ? C20 C21 C22 C23 -1.1(8) . . . . ? C21 C22 C23 C24 0.8(8) . . . . ? C22 C23 C24 N7 -179.7(5) . . . . ? C22 C23 C24 C19 0.4(7) . . . . ? C20 C19 C24 N7 178.7(4) . . . . ? N6 C19 C24 N7 -0.1(4) . . . . ? C20 C19 C24 C23 -1.4(6) . . . . ? N6 C19 C24 C23 179.8(4) . . . . ? O2 C25 C26 C26 -5.0(9) . . . 2_666 ? O1 C25 C26 C26 174.6(6) . . . 2_666 ? C2 C1 N1 C17 105.0(3) . . . . ? C2 C1 N1 C9 -120.4(3) . . . . ? C2 C1 N1 Cu1 -8.7(3) . . . . ? C18 C17 N1 C1 -93.1(3) . . . . ? C18 C17 N1 C9 133.4(3) . . . . ? C18 C17 N1 Cu1 21.3(3) . . . . ? C10 C9 N1 C1 84.7(3) . . . . ? C10 C9 N1 C17 -140.9(3) . . . . ? C10 C9 N1 Cu1 -28.4(3) . . . . ? O1 Cu1 N1 C1 -173.7(2) . . . . ? N6 Cu1 N1 C1 103.7(2) . . . . ? N4 Cu1 N1 C1 -94.3(2) . . . . ? N2 Cu1 N1 C1 6.8(2) . . . . ? O1 Cu1 N1 C17 65.3(2) . . . . ? N6 Cu1 N1 C17 -17.4(2) . . . . ? N4 Cu1 N1 C17 144.7(2) . . . . ? N2 Cu1 N1 C17 -114.3(2) . . . . ? O1 Cu1 N1 C9 -55.3(2) . . . . ? N6 Cu1 N1 C9 -138.0(2) . . . . ? N4 Cu1 N1 C9 24.0(2) . . . . ? N2 Cu1 N1 C9 125.1(2) . . . . ? N3 C2 N2 C3 0.4(4) . . . . ? C1 C2 N2 C3 -179.8(3) . . . . ? N3 C2 N2 Cu1 179.5(2) . . . . ? C1 C2 N2 Cu1 -0.8(4) . . . . ? C4 C3 N2 C2 179.1(3) . . . . ? C8 C3 N2 C2 -0.5(3) . . . . ? C4 C3 N2 Cu1 0.2(5) . . . . ? C8 C3 N2 Cu1 -179.4(2) . . . . ? O1 Cu1 N2 C2 177.2(2) . . . . ? N6 Cu1 N2 C2 -79.5(2) . . . . ? N4 Cu1 N2 C2 70.3(2) . . . . ? N1 Cu1 N2 C2 -3.5(2) . . . . ? O1 Cu1 N2 C3 -4.0(4) . . . . ? N6 Cu1 N2 C3 99.3(3) . . . . ? N4 Cu1 N2 C3 -110.9(3) . . . . ? N1 Cu1 N2 C3 175.3(3) . . . . ? N2 C2 N3 C8 -0.2(4) . . . . ? C1 C2 N3 C8 -179.9(3) . . . . ? C3 C8 N3 C2 -0.1(3) . . . . ? C7 C8 N3 C2 179.5(3) . . . . ? N5 C10 N4 C11 -1.0(4) . . . . ? C9 C10 N4 C11 176.0(3) . . . . ? N5 C10 N4 Cu1 -175.4(2) . . . . ? C9 C10 N4 Cu1 1.6(4) . . . . ? C12 C11 N4 C10 179.1(4) . . . . ? C16 C11 N4 C10 0.4(4) . . . . ? C12 C11 N4 Cu1 -7.8(6) . . . . ? C16 C11 N4 Cu1 173.5(3) . . . . ? O1 Cu1 N4 C10 117.7(3) . . . . ? N6 Cu1 N4 C10 20.1(4) . . . . ? N2 Cu1 N4 C10 -89.2(3) . . . . ? N1 Cu1 N4 C10 -14.4(2) . . . . ? O1 Cu1 N4 C11 -54.8(3) . . . . ? N6 Cu1 N4 C11 -152.4(3) . . . . ? N2 Cu1 N4 C11 98.3(3) . . . . ? N1 Cu1 N4 C11 173.1(3) . . . . ? N4 C10 N5 C16 1.2(4) . . . . ? C9 C10 N5 C16 -175.8(3) . . . . ? C15 C16 N5 C10 -179.4(5) . . . . ? C11 C16 N5 C10 -0.9(4) . . . . ? N7 C18 N6 C19 -0.5(4) . . . . ? C17 C18 N6 C19 -177.8(3) . . . . ? N7 C18 N6 Cu1 178.1(2) . . . . ? C17 C18 N6 Cu1 0.8(5) . . . . ? C20 C19 N6 C18 -178.3(4) . . . . ? C24 C19 N6 C18 0.4(4) . . . . ? C20 C19 N6 Cu1 3.4(6) . . . . ? C24 C19 N6 Cu1 -177.9(3) . . . . ? O1 Cu1 N6 C18 -122.0(3) . . . . ? N4 Cu1 N6 C18 -24.8(4) . . . . ? N2 Cu1 N6 C18 85.4(3) . . . . ? N1 Cu1 N6 C18 9.4(2) . . . . ? O1 Cu1 N6 C19 56.1(3) . . . . ? N4 Cu1 N6 C19 153.3(3) . . . . ? N2 Cu1 N6 C19 -96.5(3) . . . . ? N1 Cu1 N6 C19 -172.5(3) . . . . ? N6 C18 N7 C24 0.4(4) . . . . ? C17 C18 N7 C24 177.7(3) . . . . ? C23 C24 N7 C18 180.0(4) . . . . ? C19 C24 N7 C18 -0.1(4) . . . . ? O2 C25 O1 Cu1 1.1(5) . . . . ? C26 C25 O1 Cu1 -178.5(3) . . . . ? N6 Cu1 O1 C25 -107.9(3) . . . . ? N4 Cu1 O1 C25 103.9(3) . . . . ? N2 Cu1 O1 C25 -4.4(4) . . . . ? N1 Cu1 O1 C25 176.5(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O5 0.836(19) 2.14(2) 2.957(11) 165(4) 2_776 N3 H3A O6 0.836(19) 2.59(3) 3.234(14) 135(3) 2_776 N5 H5A O8 0.85(4) 1.92(2) 2.769(6) 173(4) 1_655 N7 H7A O9 0.84(4) 1.99(2) 2.833(7) 177(4) 1_655 O7 H7C O2 0.84(6) 1.92(6) 2.759(4) 177(7) . C9 H9B O1 0.97 2.30 3.244(4) 163.9 2_766 C17 H17A O1 0.97 2.40 3.336(5) 163.3 2_766 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.485 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.079 # start Validation Reply Form _vrf_PLAT417_4 ; PROBLEM: Short Inter D-H..H-D H9D .. H10A .. 1.75 Ang. RESPONSE: This is due to the disorder of solvent water molecules. ; # END data_5 #TrackingRef '- 1-9.cif' _database_code_depnum_ccdc_archive 'CCDC 788589' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cu2 C52 H46 N14 O4, 2 (Cl O4), 8 (H2 O)' _chemical_formula_sum 'C52 H62 Cl2 Cu2 N14 O20' _chemical_formula_weight 1401.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7934(11) _cell_length_b 11.9882(13) _cell_length_c 13.8076(14) _cell_angle_alpha 112.292(1) _cell_angle_beta 99.127(2) _cell_angle_gamma 100.434(2) _cell_volume 1574.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6309 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.03 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8883 _exptl_absorpt_correction_T_max 0.9204 _exptl_absorpt_process_details 'SADABS, Sheldrick, 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo k\a' _diffrn_radiation_source 'fine focus sealed Siemens Mo tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex CCD area-detector' _diffrn_measurement_method '0.3\% wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17215 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6448 _reflns_number_gt 5133 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART,(Version 5.628)2001' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+,(Version 6.45)2001 ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material PLATON _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. The Cl1/O3-O6 perchlorate ion was found to be disordered over two sites and their occupancies are of the 0.62(1):0.38(1) for the major and minor components, respectively. The O10 water was disordered over two sites with the final occupancies of 0.57(1):0.43(1), respectively. The C26 atom was also disordered over two sites with their occupancies of 0.65(1):0.35(1). Command 'DFIX' was used in the refinement to restrain the Cl-O and O...O distances of 1.38(1) \%A and 2.42(2)\%A for the anion, respectively, and the O-H and H...H distances of 0.82(1) \%A and 1.35(2) \%A for the water molecule. 'SADI' command was used to restrain the C26-C26 (1 - x, 1 - y, 1 - z) distance. ; _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^)+(0.0752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6448 _refine_ls_number_parameters 493 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.93553(3) 0.70130(2) 0.65074(2) 0.03481(12) Uani 1 1 d . . . C1 C 1.2325(3) 0.8379(2) 0.7792(2) 0.0479(7) Uani 1 1 d . . . H1A H 1.3007 0.8910 0.7661 0.057 Uiso 1 1 calc R . . H1B H 1.2723 0.8161 0.8353 0.057 Uiso 1 1 calc R . . C2 C 1.1368(2) 0.9090(2) 0.81814(19) 0.0358(5) Uani 1 1 d . . . C3 C 0.9582(2) 0.9637(2) 0.83524(19) 0.0343(5) Uani 1 1 d . . . C4 C 0.8310(3) 0.9716(2) 0.8258(2) 0.0440(6) Uani 1 1 d . . . H4 H 0.7628 0.9075 0.7729 0.053 Uiso 1 1 calc R . . C5 C 0.8093(3) 1.0791(3) 0.8982(2) 0.0525(7) Uani 1 1 d . . . H5A H 0.7248 1.0872 0.8943 0.063 Uiso 1 1 calc R . . C6 C 0.9120(3) 1.1751(2) 0.9767(2) 0.0530(7) Uani 1 1 d . . . H6 H 0.8938 1.2460 1.0239 0.064 Uiso 1 1 calc R . . C7 C 1.0378(3) 1.1693(2) 0.9871(2) 0.0506(7) Uani 1 1 d . . . H7 H 1.1056 1.2340 1.0399 0.061 Uiso 1 1 calc R . . C8 C 1.0600(3) 1.0612(2) 0.91428(19) 0.0382(6) Uani 1 1 d . . . C9 C 1.2013(3) 0.7299(3) 0.5826(2) 0.0472(6) Uani 1 1 d . . . H9A H 1.2067 0.6486 0.5341 0.057 Uiso 1 1 calc R . . H9B H 1.2849 0.7892 0.6011 0.057 Uiso 1 1 calc R . . C10 C 1.0980(3) 0.7691(2) 0.5263(2) 0.0405(6) Uani 1 1 d . . . C11 C 0.9141(3) 0.8034(2) 0.4732(2) 0.0430(6) Uani 1 1 d . . . C12 C 0.7893(3) 0.8179(3) 0.4594(3) 0.0578(8) Uani 1 1 d . . . H12 H 0.7340 0.8000 0.4999 0.069 Uiso 1 1 calc R . . C13 C 0.7508(4) 0.8605(3) 0.3822(3) 0.0748(10) Uani 1 1 d . . . H13 H 0.6676 0.8718 0.3706 0.090 Uiso 1 1 calc R . . C14 C 0.8337(4) 0.8869(3) 0.3216(3) 0.0766(11) Uani 1 1 d . . . H14 H 0.8039 0.9143 0.2699 0.092 Uiso 1 1 calc R . . C15 C 0.9560(4) 0.8741(3) 0.3358(3) 0.0686(9) Uani 1 1 d . . . H15 H 1.0109 0.8930 0.2954 0.082 Uiso 1 1 calc R . . C16 C 0.9970(3) 0.8314(3) 0.4129(2) 0.0505(7) Uani 1 1 d . . . C17 C 1.1864(2) 0.6104(2) 0.6937(2) 0.0416(6) Uani 1 1 d . . . H17A H 1.2701 0.6276 0.7421 0.050 Uiso 1 1 calc R . . H17B H 1.1826 0.5449 0.6243 0.050 Uiso 1 1 calc R . . C18 C 1.0795(2) 0.5681(2) 0.7390(2) 0.0383(6) Uani 1 1 d . . . C19 C 0.8931(3) 0.5332(2) 0.7762(2) 0.0404(6) Uani 1 1 d . . . C20 C 0.7687(3) 0.5310(3) 0.7910(2) 0.0519(7) Uani 1 1 d . . . H20 H 0.7193 0.5766 0.7682 0.062 Uiso 1 1 calc R . . C21 C 0.7213(3) 0.4580(3) 0.8410(3) 0.0683(9) Uani 1 1 d . . . H21 H 0.6378 0.4537 0.8515 0.082 Uiso 1 1 calc R . . C22 C 0.7956(4) 0.3913(3) 0.8758(3) 0.0785(11) Uani 1 1 d . . . H22 H 0.7603 0.3436 0.9093 0.094 Uiso 1 1 calc R . . C23 C 0.9178(4) 0.3928(3) 0.8631(3) 0.0709(10) Uani 1 1 d . . . H23 H 0.9667 0.3477 0.8871 0.085 Uiso 1 1 calc R . . C24 C 0.9665(3) 0.4657(3) 0.8121(2) 0.0490(7) Uani 1 1 d . . . C25 C 0.6828(2) 0.5907(2) 0.5615(2) 0.0452(6) Uani 1 1 d D . . C26 C 0.5628(8) 0.4817(10) 0.4900(6) 0.053(3) Uani 0.65(3) 1 d PD . 1 H26A H 0.5624 0.4582 0.4145 0.064 Uiso 0.65(3) 1 calc PR . 1 H26B H 0.5670 0.4099 0.5057 0.064 Uiso 0.65(3) 1 calc PR . 1 C26' C 0.5555(14) 0.512(2) 0.4771(13) 0.058(5) Uani 0.35(3) 1 d PD . 2 H26C H 0.5344 0.5543 0.4316 0.070 Uiso 0.35(3) 1 calc PR . 2 H26D H 0.5680 0.4326 0.4315 0.070 Uiso 0.35(3) 1 calc PR . 2 Cl1 Cl 0.50455(8) 0.76119(9) 1.01035(8) 0.0708(2) Uani 1 1 d D . . N1 N 1.17277(19) 0.72398(18) 0.68031(16) 0.0365(5) Uani 1 1 d . . . N2 N 1.01091(19) 0.86918(17) 0.77657(15) 0.0340(4) Uani 1 1 d . . . N3 N 1.1715(2) 1.02319(18) 0.90089(17) 0.0414(5) Uani 1 1 d . . . H3 H 1.2494 1.0650 0.9386 0.050 Uiso 1 1 calc R . . N4 N 0.9814(2) 0.76358(18) 0.54382(16) 0.0386(5) Uani 1 1 d . . . N5 N 1.1124(2) 0.8092(2) 0.44895(18) 0.0494(6) Uani 1 1 d . . . H5 H 1.1814 0.8191 0.4261 0.059 Uiso 1 1 calc R . . N6 N 0.96823(19) 0.59741(18) 0.73094(16) 0.0368(5) Uani 1 1 d . . . N7 N 1.0842(2) 0.4904(2) 0.78799(19) 0.0468(5) Uani 1 1 d . . . H7A H 1.1490 0.4616 0.8017 0.056 Uiso 1 1 calc R . . O1 O 0.78872(16) 0.56622(16) 0.54383(14) 0.0439(4) Uani 1 1 d . . . O2 O 0.67825(18) 0.68707(18) 0.63387(18) 0.0628(6) Uani 1 1 d . . . O3 O 0.5890(8) 0.7934(15) 0.9522(5) 0.106(4) Uani 0.62(2) 1 d PD A 1 O4 O 0.5342(10) 0.8630(12) 1.1155(7) 0.140(5) Uani 0.62(2) 1 d PD A 1 O5 O 0.3743(7) 0.737(2) 0.9581(17) 0.087(5) Uani 0.62(2) 1 d PD A 1 O6 O 0.5231(11) 0.6535(8) 1.0221(12) 0.149(5) Uani 0.62(2) 1 d PD A 1 O3' O 0.5559(15) 0.8622(18) 0.9820(19) 0.115(6) Uani 0.38(2) 1 d PD A 2 O4' O 0.543(2) 0.794(3) 1.1182(9) 0.181(10) Uani 0.38(2) 1 d PD A 2 O6' O 0.544(2) 0.6557(19) 0.946(3) 0.229(13) Uani 0.38(2) 1 d PD A 2 O5' O 0.3684(10) 0.721(3) 0.968(2) 0.082(6) Uani 0.38(2) 1 d PD A 2 O7 O 0.3500(4) 0.8340(5) 0.3877(4) 0.1423(14) Uani 1 1 d D . . H7B H 0.386(8) 0.896(5) 0.445(4) 0.213 Uiso 1 1 d D . . H7C H 0.328(8) 0.859(8) 0.341(5) 0.213 Uiso 1 1 d D . . O8 O 0.5046(3) 0.7999(3) 0.7339(2) 0.0897(8) Uani 1 1 d D . . H8B H 0.565(4) 0.771(5) 0.712(4) 0.135 Uiso 1 1 d D . . H8A H 0.524(5) 0.824(5) 0.8021(11) 0.135 Uiso 1 1 d D . . O9 O 0.3113(4) 0.4280(4) 0.8435(4) 0.1437(16) Uani 1 1 d D . . H9C H 0.269(7) 0.392(7) 0.874(6) 0.216 Uiso 1 1 d D . . H9D H 0.373(5) 0.484(5) 0.890(5) 0.216 Uiso 1 1 d D . . O10 O 0.4759(9) 0.0769(14) 0.4037(10) 0.160(6) Uani 0.573(14) 1 d PD B 1 H10A H 0.48(3) 0.023(19) 0.346(11) 0.240 Uiso 0.573(14) 1 d PD B 1 H10B H 0.456(16) 0.136(11) 0.396(16) 0.240 Uiso 0.573(14) 1 d PD B 1 O10' O 0.4892(10) -0.0140(12) 0.3078(12) 0.112(5) Uani 0.427(14) 1 d PD B 2 H10C H 0.470(16) 0.037(12) 0.287(14) 0.168 Uiso 0.427(14) 1 d PD B 2 H10D H 0.451(15) -0.085(6) 0.263(11) 0.168 Uiso 0.427(14) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.03128(19) 0.03340(17) 0.03323(19) 0.01220(13) 0.00372(12) 0.00105(12) C1 0.0311(14) 0.0457(14) 0.0550(17) 0.0140(13) 0.0036(12) 0.0046(11) C2 0.0348(13) 0.0348(12) 0.0344(13) 0.0145(10) 0.0072(10) 0.0027(10) C3 0.0443(14) 0.0303(11) 0.0311(12) 0.0157(10) 0.0127(10) 0.0071(10) C4 0.0458(16) 0.0398(13) 0.0441(15) 0.0152(12) 0.0110(12) 0.0114(11) C5 0.0578(19) 0.0500(16) 0.0583(18) 0.0232(14) 0.0238(15) 0.0248(14) C6 0.079(2) 0.0392(14) 0.0453(16) 0.0150(12) 0.0243(15) 0.0243(14) C7 0.072(2) 0.0334(13) 0.0381(15) 0.0105(11) 0.0123(14) 0.0071(13) C8 0.0502(15) 0.0324(12) 0.0310(13) 0.0151(10) 0.0097(11) 0.0048(11) C9 0.0371(15) 0.0604(16) 0.0536(17) 0.0305(14) 0.0201(12) 0.0129(13) C10 0.0434(15) 0.0382(13) 0.0374(14) 0.0152(11) 0.0115(11) 0.0051(11) C11 0.0479(16) 0.0393(13) 0.0373(14) 0.0177(11) 0.0022(11) 0.0042(11) C12 0.0521(18) 0.0640(18) 0.0598(19) 0.0334(16) 0.0045(14) 0.0133(14) C13 0.069(2) 0.077(2) 0.082(3) 0.045(2) -0.0041(19) 0.0217(18) C14 0.093(3) 0.075(2) 0.071(2) 0.050(2) 0.002(2) 0.017(2) C15 0.084(3) 0.069(2) 0.062(2) 0.0437(18) 0.0139(18) 0.0093(18) C16 0.0575(18) 0.0475(15) 0.0438(16) 0.0231(13) 0.0060(13) 0.0043(13) C17 0.0396(14) 0.0456(14) 0.0430(14) 0.0196(12) 0.0127(11) 0.0150(11) C18 0.0411(14) 0.0358(12) 0.0346(13) 0.0125(10) 0.0086(11) 0.0081(10) C19 0.0433(15) 0.0339(12) 0.0408(14) 0.0148(11) 0.0116(11) 0.0036(11) C20 0.0480(17) 0.0489(15) 0.0604(18) 0.0233(14) 0.0205(14) 0.0100(13) C21 0.063(2) 0.067(2) 0.082(2) 0.0364(19) 0.0356(18) 0.0060(17) C22 0.086(3) 0.081(2) 0.103(3) 0.067(2) 0.044(2) 0.021(2) C23 0.080(3) 0.070(2) 0.089(3) 0.056(2) 0.033(2) 0.0204(18) C24 0.0545(18) 0.0450(14) 0.0526(17) 0.0259(13) 0.0169(14) 0.0101(13) C25 0.0315(14) 0.0441(14) 0.0440(15) 0.0081(12) 0.0045(11) 0.0001(11) C26 0.023(3) 0.040(4) 0.068(4) -0.002(3) 0.002(2) 0.004(3) C26' 0.046(8) 0.045(8) 0.064(8) 0.005(6) 0.010(5) 0.011(5) Cl1 0.0443(5) 0.0790(6) 0.0874(6) 0.0413(5) 0.0055(4) 0.0079(4) N1 0.0326(11) 0.0402(11) 0.0373(11) 0.0170(9) 0.0100(9) 0.0085(9) N2 0.0363(11) 0.0310(9) 0.0311(10) 0.0112(8) 0.0076(8) 0.0055(8) N3 0.0393(12) 0.0346(10) 0.0380(12) 0.0114(9) 0.0019(9) -0.0034(9) N4 0.0360(12) 0.0432(11) 0.0368(12) 0.0190(9) 0.0083(9) 0.0065(9) N5 0.0516(14) 0.0533(13) 0.0475(14) 0.0265(11) 0.0187(11) 0.0062(11) N6 0.0348(11) 0.0359(10) 0.0391(12) 0.0159(9) 0.0102(9) 0.0064(9) N7 0.0474(14) 0.0466(12) 0.0551(14) 0.0285(11) 0.0135(11) 0.0164(10) O1 0.0261(9) 0.0454(10) 0.0437(10) 0.0058(8) 0.0053(7) 0.0020(7) O2 0.0352(11) 0.0488(11) 0.0698(14) -0.0077(10) 0.0129(10) 0.0032(8) O3 0.066(4) 0.148(9) 0.073(4) 0.035(5) 0.020(3) -0.018(5) O4 0.102(6) 0.158(9) 0.083(6) -0.007(4) 0.008(4) 0.000(5) O5 0.042(4) 0.117(8) 0.109(9) 0.062(6) 0.003(5) 0.018(5) O6 0.148(7) 0.151(8) 0.183(11) 0.102(8) 0.005(7) 0.078(5) O3' 0.072(7) 0.109(10) 0.144(13) 0.071(10) -0.018(7) -0.024(6) O4' 0.193(15) 0.24(3) 0.081(10) 0.084(14) -0.042(9) 0.027(16) O6' 0.203(17) 0.23(2) 0.26(3) 0.062(19) 0.100(18) 0.131(17) O5' 0.062(9) 0.101(11) 0.073(8) 0.038(9) 0.018(6) -0.009(7) O7 0.101(3) 0.181(5) 0.156(4) 0.078(3) 0.066(3) 0.020(3) O8 0.0606(16) 0.107(2) 0.0889(19) 0.0223(18) 0.0229(15) 0.0313(15) O9 0.103(3) 0.100(3) 0.191(4) 0.040(3) -0.026(3) 0.046(2) O10 0.096(5) 0.244(14) 0.143(10) 0.118(11) 0.002(5) -0.007(7) O10' 0.086(6) 0.152(9) 0.126(12) 0.085(8) 0.029(6) 0.035(6) _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 O1 1.9564(17) . ? Cu1 N4 1.979(2) . ? Cu1 N6 1.996(2) . ? Cu1 N2 2.0091(19) . ? Cu1 N1 2.476(2) . ? C1 N1 1.461(3) . ? C1 C2 1.493(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.309(3) . ? C2 N3 1.346(3) . ? C3 C4 1.382(4) . ? C3 N2 1.395(3) . ? C3 C8 1.397(3) . ? C4 C5 1.386(4) . ? C4 H4 0.9300 . ? C5 C6 1.392(4) . ? C5 H5A 0.9300 . ? C6 C7 1.360(4) . ? C6 H6 0.9300 . ? C7 C8 1.396(4) . ? C7 H7 0.9300 . ? C8 N3 1.377(3) . ? C9 N1 1.455(3) . ? C9 C10 1.503(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.313(3) . ? C10 N5 1.346(3) . ? C11 C12 1.382(4) . ? C11 C16 1.395(4) . ? C11 N4 1.400(3) . ? C12 C13 1.386(4) . ? C12 H12 0.9300 . ? C13 C14 1.390(5) . ? C13 H13 0.9300 . ? C14 C15 1.349(5) . ? C14 H14 0.9300 . ? C15 C16 1.392(4) . ? C15 H15 0.9300 . ? C16 N5 1.376(4) . ? C17 N1 1.471(3) . ? C17 C18 1.497(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.311(3) . ? C18 N7 1.346(3) . ? C19 C20 1.386(4) . ? C19 C24 1.392(4) . ? C19 N6 1.393(3) . ? C20 C21 1.384(4) . ? C20 H20 0.9300 . ? C21 C22 1.383(5) . ? C21 H21 0.9300 . ? C22 C23 1.356(5) . ? C22 H22 0.9300 . ? C23 C24 1.398(4) . ? C23 H23 0.9300 . ? C24 N7 1.373(4) . ? C25 O2 1.223(3) . ? C25 O1 1.268(3) . ? C25 C26' 1.524(8) . ? C25 C26 1.537(5) . ? C26 C26 1.53(2) 2_666 ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26' C26' 1.47(5) 2_666 ? C26' H26C 0.9700 . ? C26' H26D 0.9700 . ? Cl1 O4' 1.357(9) . ? Cl1 O5 1.398(6) . ? Cl1 O3 1.402(5) . ? Cl1 O6 1.405(6) . ? Cl1 O5' 1.411(9) . ? Cl1 O6' 1.425(9) . ? Cl1 O4 1.437(7) . ? Cl1 O3' 1.454(8) . ? N3 H3 0.8600 . ? N5 H5 0.8600 . ? N7 H7A 0.8600 . ? O7 H7B 0.83(6) . ? O7 H7C 0.83(8) . ? O8 H8B 0.84(5) . ? O8 H8A 0.851(10) . ? O9 H9C 0.84(8) . ? O9 H9D 0.83(6) . ? O10 H10A 0.821(11) . ? O10 H10B 0.818(11) . ? O10' H10A 0.59(5) . ? O10' H10C 0.819(11) . ? O10' H10D 0.822(11) . ? 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 O1 Cu1 N4 92.94(8) . . ? O1 Cu1 N6 91.28(8) . . ? N4 Cu1 N6 147.77(9) . . ? O1 Cu1 N2 152.15(8) . . ? N4 Cu1 N2 93.76(8) . . ? N6 Cu1 N2 97.24(8) . . ? O1 Cu1 N1 130.82(7) . . ? N4 Cu1 N1 77.00(8) . . ? N6 Cu1 N1 76.14(8) . . ? N2 Cu1 N1 77.02(7) . . ? N1 C1 C2 112.6(2) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? N2 C2 N3 112.1(2) . . ? N2 C2 C1 124.7(2) . . ? N3 C2 C1 123.1(2) . . ? C4 C3 N2 131.0(2) . . ? C4 C3 C8 120.8(2) . . ? N2 C3 C8 108.1(2) . . ? C3 C4 C5 117.3(3) . . ? C3 C4 H4 121.4 . . ? C5 C4 H4 121.4 . . ? C4 C5 C6 121.1(3) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C7 C6 C5 122.5(2) . . ? C7 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? C6 C7 C8 116.6(3) . . ? C6 C7 H7 121.7 . . ? C8 C7 H7 121.7 . . ? N3 C8 C7 132.6(2) . . ? N3 C8 C3 105.7(2) . . ? C7 C8 C3 121.7(3) . . ? N1 C9 C10 111.1(2) . . ? N1 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N1 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N4 C10 N5 112.1(2) . . ? N4 C10 C9 124.0(2) . . ? N5 C10 C9 123.9(2) . . ? C12 C11 C16 121.5(2) . . ? C12 C11 N4 130.4(3) . . ? C16 C11 N4 108.1(2) . . ? C11 C12 C13 116.6(3) . . ? C11 C12 H12 121.7 . . ? C13 C12 H12 121.7 . . ? C12 C13 C14 121.6(3) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C15 C14 C13 122.0(3) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 C16 117.6(3) . . ? C14 C15 H15 121.2 . . ? C16 C15 H15 121.2 . . ? N5 C16 C15 133.3(3) . . ? N5 C16 C11 105.8(2) . . ? C15 C16 C11 120.9(3) . . ? N1 C17 C18 109.71(19) . . ? N1 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? N1 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N6 C18 N7 112.3(2) . . ? N6 C18 C17 124.0(2) . . ? N7 C18 C17 123.7(2) . . ? C20 C19 C24 120.8(3) . . ? C20 C19 N6 131.1(2) . . ? C24 C19 N6 108.1(2) . . ? C21 C20 C19 117.1(3) . . ? C21 C20 H20 121.4 . . ? C19 C20 H20 121.4 . . ? C22 C21 C20 121.3(3) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C23 C22 C21 122.7(3) . . ? C23 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? C22 C23 C24 116.6(3) . . ? C22 C23 H23 121.7 . . ? C24 C23 H23 121.7 . . ? N7 C24 C19 106.1(2) . . ? N7 C24 C23 132.3(3) . . ? C19 C24 C23 121.6(3) . . ? O2 C25 O1 123.0(2) . . ? O2 C25 C26' 116.4(7) . . ? O1 C25 C26' 119.3(7) . . ? O2 C25 C26 123.9(5) . . ? O1 C25 C26 112.8(5) . . ? C26 C26 C25 110.8(8) 2_666 . ? C26 C26 H26A 109.5 2_666 . ? C25 C26 H26A 109.5 . . ? C26 C26 H26B 109.5 2_666 . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C26' C26' C25 114.2(15) 2_666 . ? C26' C26' H26C 108.7 2_666 . ? C25 C26' H26C 108.7 . . ? C26' C26' H26D 108.7 2_666 . ? C25 C26' H26D 108.7 . . ? H26C C26' H26D 107.6 . . ? O4' Cl1 O5 121.8(14) . . ? O4' Cl1 O3 122.4(11) . . ? O5 Cl1 O3 111.6(10) . . ? O5 Cl1 O6 108.6(11) . . ? O3 Cl1 O6 109.6(6) . . ? O4' Cl1 O5' 114.1(18) . . ? O3 Cl1 O5' 121.7(15) . . ? O6 Cl1 O5' 98.5(16) . . ? O4' Cl1 O6' 113.6(13) . . ? O5 Cl1 O6' 104.2(15) . . ? O5' Cl1 O6' 101.7(17) . . ? O5 Cl1 O4 109.4(10) . . ? O3 Cl1 O4 108.4(5) . . ? O6 Cl1 O4 109.2(6) . . ? O5' Cl1 O4 108.6(14) . . ? O6' Cl1 O4 144.3(12) . . ? O4' Cl1 O3' 111.9(11) . . ? O5 Cl1 O3' 96.7(11) . . ? O6 Cl1 O3' 146.3(8) . . ? O5' Cl1 O3' 108.2(16) . . ? O6' Cl1 O3' 106.5(11) . . ? C9 N1 C1 115.0(2) . . ? C9 N1 C17 115.0(2) . . ? C1 N1 C17 112.8(2) . . ? C9 N1 Cu1 103.89(14) . . ? C1 N1 Cu1 105.48(14) . . ? C17 N1 Cu1 102.92(14) . . ? C2 N2 C3 106.31(19) . . ? C2 N2 Cu1 119.53(16) . . ? C3 N2 Cu1 134.14(16) . . ? C2 N3 C8 107.7(2) . . ? C2 N3 H3 126.1 . . ? C8 N3 H3 126.1 . . ? C10 N4 C11 106.2(2) . . ? C10 N4 Cu1 119.30(17) . . ? C11 N4 Cu1 134.50(18) . . ? C10 N5 C16 107.8(2) . . ? C10 N5 H5 126.1 . . ? C16 N5 H5 126.1 . . ? C18 N6 C19 106.1(2) . . ? C18 N6 Cu1 118.81(17) . . ? C19 N6 Cu1 134.75(17) . . ? C18 N7 C24 107.4(2) . . ? C18 N7 H7A 126.3 . . ? C24 N7 H7A 126.3 . . ? C25 O1 Cu1 109.62(15) . . ? H7B O7 H7C 109(9) . . ? H8B O8 H8A 106(5) . . ? H9C O9 H9D 108(8) . . ? H10A O10 H10B 111(10) . . ? H10C O10' H10D 111(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 7.0(4) . . . . ? N1 C1 C2 N3 -172.7(2) . . . . ? N2 C3 C4 C5 179.3(2) . . . . ? C8 C3 C4 C5 -0.6(4) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C4 C5 C6 C7 -0.2(4) . . . . ? C5 C6 C7 C8 0.1(4) . . . . ? C6 C7 C8 N3 -179.8(3) . . . . ? C6 C7 C8 C3 -0.3(4) . . . . ? C4 C3 C8 N3 -179.8(2) . . . . ? N2 C3 C8 N3 0.3(3) . . . . ? C4 C3 C8 C7 0.6(4) . . . . ? N2 C3 C8 C7 -179.3(2) . . . . ? N1 C9 C10 N4 -18.2(4) . . . . ? N1 C9 C10 N5 164.6(2) . . . . ? C16 C11 C12 C13 0.6(4) . . . . ? N4 C11 C12 C13 179.5(3) . . . . ? C11 C12 C13 C14 0.2(5) . . . . ? C12 C13 C14 C15 -0.9(6) . . . . ? C13 C14 C15 C16 0.8(5) . . . . ? C14 C15 C16 N5 -179.1(3) . . . . ? C14 C15 C16 C11 -0.1(5) . . . . ? C12 C11 C16 N5 178.6(3) . . . . ? N4 C11 C16 N5 -0.5(3) . . . . ? C12 C11 C16 C15 -0.6(4) . . . . ? N4 C11 C16 C15 -179.8(3) . . . . ? N1 C17 C18 N6 22.7(3) . . . . ? N1 C17 C18 N7 -160.7(2) . . . . ? C24 C19 C20 C21 -0.9(4) . . . . ? N6 C19 C20 C21 -178.9(3) . . . . ? C19 C20 C21 C22 0.7(5) . . . . ? C20 C21 C22 C23 -0.2(6) . . . . ? C21 C22 C23 C24 -0.2(6) . . . . ? C20 C19 C24 N7 -178.4(2) . . . . ? N6 C19 C24 N7 0.0(3) . . . . ? C20 C19 C24 C23 0.6(4) . . . . ? N6 C19 C24 C23 179.0(3) . . . . ? C22 C23 C24 N7 178.6(3) . . . . ? C22 C23 C24 C19 0.0(5) . . . . ? O2 C25 C26 C26 8.7(18) . . . 2_666 ? O1 C25 C26 C26 -176.9(12) . . . 2_666 ? C26' C25 C26 C26 -62(3) . . . 2_666 ? O2 C25 C26' C26' -49(4) . . . 2_666 ? O1 C25 C26' C26' 143(2) . . . 2_666 ? C26 C25 C26' C26' 70(5) . . . 2_666 ? C10 C9 N1 C1 -93.2(3) . . . . ? C10 C9 N1 C17 133.3(2) . . . . ? C10 C9 N1 Cu1 21.6(2) . . . . ? C2 C1 N1 C9 105.6(3) . . . . ? C2 C1 N1 C17 -119.8(2) . . . . ? C2 C1 N1 Cu1 -8.2(3) . . . . ? C18 C17 N1 C9 -140.6(2) . . . . ? C18 C17 N1 C1 84.8(3) . . . . ? C18 C17 N1 Cu1 -28.4(2) . . . . ? O1 Cu1 N1 C9 64.81(18) . . . . ? N4 Cu1 N1 C9 -17.73(15) . . . . ? N6 Cu1 N1 C9 144.29(17) . . . . ? N2 Cu1 N1 C9 -114.76(16) . . . . ? O1 Cu1 N1 C1 -173.85(16) . . . . ? N4 Cu1 N1 C1 103.61(17) . . . . ? N6 Cu1 N1 C1 -94.38(17) . . . . ? N2 Cu1 N1 C1 6.58(16) . . . . ? O1 Cu1 N1 C17 -55.45(18) . . . . ? N4 Cu1 N1 C17 -138.00(16) . . . . ? N6 Cu1 N1 C17 24.02(14) . . . . ? N2 Cu1 N1 C17 124.97(16) . . . . ? N3 C2 N2 C3 0.4(3) . . . . ? C1 C2 N2 C3 -179.3(2) . . . . ? N3 C2 N2 Cu1 179.41(15) . . . . ? C1 C2 N2 Cu1 -0.3(3) . . . . ? C4 C3 N2 C2 179.7(2) . . . . ? C8 C3 N2 C2 -0.4(3) . . . . ? C4 C3 N2 Cu1 0.9(4) . . . . ? C8 C3 N2 Cu1 -179.22(17) . . . . ? O1 Cu1 N2 C2 177.13(17) . . . . ? N4 Cu1 N2 C2 -79.30(18) . . . . ? N6 Cu1 N2 C2 70.35(19) . . . . ? N1 Cu1 N2 C2 -3.57(17) . . . . ? O1 Cu1 N2 C3 -4.2(3) . . . . ? N4 Cu1 N2 C3 99.4(2) . . . . ? N6 Cu1 N2 C3 -111.0(2) . . . . ? N1 Cu1 N2 C3 175.1(2) . . . . ? N2 C2 N3 C8 -0.2(3) . . . . ? C1 C2 N3 C8 179.5(2) . . . . ? C7 C8 N3 C2 179.5(3) . . . . ? C3 C8 N3 C2 -0.1(3) . . . . ? N5 C10 N4 C11 -0.3(3) . . . . ? C9 C10 N4 C11 -177.7(2) . . . . ? N5 C10 N4 Cu1 177.84(16) . . . . ? C9 C10 N4 Cu1 0.4(3) . . . . ? C12 C11 N4 C10 -178.6(3) . . . . ? C16 C11 N4 C10 0.5(3) . . . . ? C12 C11 N4 Cu1 3.8(4) . . . . ? C16 C11 N4 Cu1 -177.19(18) . . . . ? O1 Cu1 N4 C10 -121.52(18) . . . . ? N6 Cu1 N4 C10 -24.4(3) . . . . ? N2 Cu1 N4 C10 85.52(19) . . . . ? N1 Cu1 N4 C10 9.77(18) . . . . ? O1 Cu1 N4 C11 55.9(2) . . . . ? N6 Cu1 N4 C11 153.0(2) . . . . ? N2 Cu1 N4 C11 -97.0(2) . . . . ? N1 Cu1 N4 C11 -172.8(2) . . . . ? N4 C10 N5 C16 -0.1(3) . . . . ? C9 C10 N5 C16 177.4(2) . . . . ? C15 C16 N5 C10 179.5(3) . . . . ? C11 C16 N5 C10 0.4(3) . . . . ? N7 C18 N6 C19 -1.0(3) . . . . ? C17 C18 N6 C19 176.0(2) . . . . ? N7 C18 N6 Cu1 -175.40(16) . . . . ? C17 C18 N6 Cu1 1.6(3) . . . . ? C20 C19 N6 C18 178.8(3) . . . . ? C24 C19 N6 C18 0.6(3) . . . . ? C20 C19 N6 Cu1 -8.1(4) . . . . ? C24 C19 N6 Cu1 173.65(19) . . . . ? O1 Cu1 N6 C18 117.51(18) . . . . ? N4 Cu1 N6 C18 19.9(3) . . . . ? N2 Cu1 N6 C18 -89.06(18) . . . . ? N1 Cu1 N6 C18 -14.40(17) . . . . ? O1 Cu1 N6 C19 -54.9(2) . . . . ? N4 Cu1 N6 C19 -152.5(2) . . . . ? N2 Cu1 N6 C19 98.5(2) . . . . ? N1 Cu1 N6 C19 173.2(2) . . . . ? N6 C18 N7 C24 1.1(3) . . . . ? C17 C18 N7 C24 -175.9(2) . . . . ? C19 C24 N7 C18 -0.6(3) . . . . ? C23 C24 N7 C18 -179.5(3) . . . . ? O2 C25 O1 Cu1 1.7(4) . . . . ? C26' C25 O1 Cu1 168.7(14) . . . . ? C26 C25 O1 Cu1 -172.7(6) . . . . ? N4 Cu1 O1 C25 -107.93(19) . . . . ? N6 Cu1 O1 C25 104.03(19) . . . . ? N2 Cu1 O1 C25 -4.2(3) . . . . ? N1 Cu1 O1 C25 176.74(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O3 0.86 2.09 2.920(8) 163.3 2_777 N5 H5 O7 0.86 1.97 2.825(5) 172.3 1_655 N7 H7A O9 0.86 1.92 2.767(4) 169.7 1_655 O7 H7B O10 0.83(6) 2.52(9) 2.891(13) 108(7) 1_565 O7 H7B O10 0.83(6) 2.24(7) 2.862(11) 133(8) 2_666 O8 H8A O3 0.851(10) 2.26(3) 3.041(10) 152(5) . O8 H8B O2 0.84(5) 1.93(5) 2.752(3) 168(5) . O9 H9D O6 0.83(6) 2.269(19) 3.088(11) 172(8) . O10 H10B O8 0.818(11) 2.27(16) 2.826(10) 126(17) 2_666 C1 H1B O5 0.97 2.44 3.41(2) 172.8 1_655 C4 H4 O2 0.93 2.49 3.331(3) 149.8 . C9 H9A O1 0.97 2.40 3.341(3) 163.8 2_766 C17 H17B O1 0.97 2.30 3.244(3) 164.2 2_766 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.475 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.075 # start Validation Reply Form _vrf_PLAT417_5 ; PROBLEM: Short Inter D-H..H-D H7A .. H9C .. 2.00 Ang. RESPONSE: This is largely due to the disorder of water O10 molecule. ; # END data_6 #TrackingRef '- 1-9.cif' _database_code_depnum_ccdc_archive 'CCDC 788590' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H48 Cu2 N14 O4, 2(Cl O4), 2(H2 O)' _chemical_formula_sum 'C53 H52 Cl2 Cu2 N14 O14' _chemical_formula_weight 1307.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n n a' _symmetry_space_group_name_HALL '-P 2a 2bc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 16.6780(9) _cell_length_b 17.1571(10) _cell_length_c 19.0110(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5439.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3754 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 18.91 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 0.962 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo k\a' _diffrn_radiation_source 'fine focus sealed Siemens Mo tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex CCD area-detector' _diffrn_measurement_method '0.3\% wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 103378 _diffrn_reflns_av_R_equivalents 0.1050 _diffrn_reflns_av_sigmaI/netI 0.0385 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5045 _reflns_number_gt 3407 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART,(Version 5.628)2001' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+,(Version 6.45)2001 ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material PLATON _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. Both the perchlorate Cl1 and Cl2 atoms lie on two-fold axis and their occupancies were assigned to be occupancies. ; _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^)+(0.1038P)^2^+6.6303P] 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 5045 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1957 _refine_ls_wR_factor_gt 0.1738 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.41394(3) 0.24641(3) 0.05738(3) 0.0474(2) Uani 1 1 d . . . N1 N 0.3223(2) 0.2607(2) -0.0209(2) 0.0470(9) Uani 1 1 d . . . N2 N 0.4504(2) 0.1642(2) -0.01310(19) 0.0440(9) Uani 1 1 d . . . N3 N 0.4239(2) 0.0971(2) -0.1094(2) 0.0517(10) Uani 1 1 d . . . H3 H 0.3983 0.0810 -0.1459 0.062 Uiso 1 1 calc R . . N4 N 0.3112(2) 0.2109(2) 0.1130(2) 0.0459(9) Uani 1 1 d . . . N5 N 0.1791(2) 0.2105(2) 0.1206(2) 0.0524(10) Uani 1 1 d . . . H5A H 0.1299 0.2192 0.1093 0.063 Uiso 1 1 calc R . . N6 N 0.4147(2) 0.3651(2) 0.0456(2) 0.0493(10) Uani 1 1 d . . . N7 N 0.3745(2) 0.4656(2) -0.0188(2) 0.0533(10) Uani 1 1 d . . . H7A H 0.3522 0.4910 -0.0526 0.064 Uiso 1 1 calc R . . O1 O 0.4881(2) 0.2244(2) 0.1316(2) 0.0677(10) Uani 1 1 d . . . O2 O 0.5925(3) 0.2913(3) 0.0974(4) 0.1004(18) Uani 1 1 d . . . C1 C 0.3184(3) 0.1893(3) -0.0646(3) 0.0518(12) Uani 1 1 d . . . H1A H 0.3041 0.2027 -0.1125 0.062 Uiso 1 1 calc R . . H1B H 0.2780 0.1541 -0.0462 0.062 Uiso 1 1 calc R . . C2 C 0.3986(3) 0.1509(3) -0.0633(2) 0.0462(11) Uani 1 1 d . . . C3 C 0.5153(3) 0.1146(3) -0.0266(2) 0.0451(10) Uani 1 1 d . . . C4 C 0.5853(3) 0.1009(3) 0.0107(3) 0.0529(12) Uani 1 1 d . . . H4 H 0.5967 0.1277 0.0520 0.063 Uiso 1 1 calc R . . C5 C 0.6375(3) 0.0459(3) -0.0162(3) 0.0621(14) Uani 1 1 d . . . H5 H 0.6847 0.0353 0.0079 0.075 Uiso 1 1 calc R . . C6 C 0.6217(4) 0.0065(3) -0.0775(3) 0.0682(15) Uani 1 1 d . . . H6 H 0.6589 -0.0293 -0.0942 0.082 Uiso 1 1 calc R . . C7 C 0.5521(4) 0.0186(3) -0.1147(3) 0.0653(14) Uani 1 1 d . . . H7 H 0.5415 -0.0083 -0.1561 0.078 Uiso 1 1 calc R . . C8 C 0.4983(3) 0.0726(2) -0.0876(2) 0.0483(11) Uani 1 1 d . . . C9 C 0.2436(3) 0.2762(3) 0.0146(3) 0.0529(12) Uani 1 1 d . . . H9A H 0.1996 0.2595 -0.0150 0.064 Uiso 1 1 calc R . . H9B H 0.2376 0.3315 0.0241 0.064 Uiso 1 1 calc R . . C10 C 0.2443(3) 0.2304(3) 0.0827(3) 0.0473(11) Uani 1 1 d . . . C11 C 0.2892(3) 0.1748(3) 0.1758(2) 0.0454(11) Uani 1 1 d . . . C12 C 0.3358(3) 0.1421(3) 0.2280(3) 0.0580(13) Uani 1 1 d . . . H12 H 0.3915 0.1428 0.2257 0.070 Uiso 1 1 calc R . . C13 C 0.2962(3) 0.1084(3) 0.2835(3) 0.0653(14) Uani 1 1 d . . . H13 H 0.3261 0.0850 0.3190 0.078 Uiso 1 1 calc R . . C14 C 0.2129(3) 0.1080(3) 0.2887(3) 0.0670(15) Uani 1 1 d . . . H14 H 0.1886 0.0853 0.3277 0.080 Uiso 1 1 calc R . . C15 C 0.1661(3) 0.1407(3) 0.2370(3) 0.0631(15) Uani 1 1 d . . . H15 H 0.1104 0.1405 0.2398 0.076 Uiso 1 1 calc R . . C16 C 0.2057(3) 0.1737(3) 0.1807(3) 0.0489(11) Uani 1 1 d . . . C17 C 0.3462(3) 0.3294(3) -0.0629(3) 0.0532(12) Uani 1 1 d . . . H17A H 0.3004 0.3504 -0.0880 0.064 Uiso 1 1 calc R . . H17B H 0.3872 0.3153 -0.0967 0.064 Uiso 1 1 calc R . . C18 C 0.3778(3) 0.3878(3) -0.0117(3) 0.0487(11) Uani 1 1 d . . . C19 C 0.4386(3) 0.4344(3) 0.0793(3) 0.0506(12) Uani 1 1 d . . . C20 C 0.4801(3) 0.4455(3) 0.1417(3) 0.0589(13) Uani 1 1 d . . . H20 H 0.4976 0.4038 0.1690 0.071 Uiso 1 1 calc R . . C21 C 0.4942(3) 0.5225(4) 0.1610(3) 0.0694(16) Uani 1 1 d . . . H21 H 0.5213 0.5328 0.2027 0.083 Uiso 1 1 calc R . . C22 C 0.4690(3) 0.5838(4) 0.1201(4) 0.0728(17) Uani 1 1 d . . . H22 H 0.4800 0.6343 0.1351 0.087 Uiso 1 1 calc R . . C23 C 0.4282(3) 0.5736(3) 0.0580(3) 0.0665(16) Uani 1 1 d . . . H23 H 0.4115 0.6156 0.0308 0.080 Uiso 1 1 calc R . . C24 C 0.4133(3) 0.4968(3) 0.0381(3) 0.0522(12) Uani 1 1 d . . . C25 C 0.5585(4) 0.2461(5) 0.1379(4) 0.082(2) Uani 1 1 d . . . C26 C 0.6042(5) 0.2094(7) 0.2006(5) 0.140(4) Uani 1 1 d . . . H26A H 0.5641 0.1821 0.2281 0.168 Uiso 1 1 calc R . . H26B H 0.6384 0.1695 0.1803 0.168 Uiso 1 1 calc R . . C27 C 0.6528(7) 0.2500 0.2500 0.111(4) Uani 1 2 d S . . H27A H 0.6870 0.2868 0.2254 0.133 Uiso 0.50 1 calc PR . . H27B H 0.6870 0.2132 0.2746 0.133 Uiso 0.50 1 calc PR . . Cl1 Cl 0.7500 0.0000 0.19874(11) 0.0704(6) Uani 1 2 d S . . Cl2 Cl 0.94476(14) 0.2500 0.2500 0.0652(5) Uani 1 2 d S . . O3 O 0.8211(5) 0.0010(5) 0.2346(4) 0.173(3) Uani 1 1 d . . . O4 O 0.7507(4) 0.0627(5) 0.1539(5) 0.184(3) Uani 1 1 d . . . O5 O 0.9945(3) 0.2396(2) 0.1888(2) 0.0835(13) Uani 1 1 d . . . O6 O 0.9009(4) 0.1807(5) 0.2594(3) 0.140(3) Uani 1 1 d . . . O7 O 0.6847(2) 0.4262(2) 0.1157(2) 0.0738(11) Uani 1 1 d . . . H7C H 0.6503 0.3946 0.1054 0.111 Uiso 1 1 d R . . H7B H 0.6903 0.4306 0.1581 0.111 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0381(3) 0.0519(4) 0.0524(4) -0.0076(3) -0.0048(2) 0.0023(2) N1 0.042(2) 0.048(2) 0.051(2) -0.0039(18) -0.0034(17) 0.0009(17) N2 0.043(2) 0.042(2) 0.047(2) -0.0037(17) 0.0025(17) 0.0030(17) N3 0.059(3) 0.047(2) 0.049(2) -0.0072(18) -0.0052(19) -0.0015(19) N4 0.038(2) 0.053(2) 0.047(2) -0.0082(18) 0.0027(17) 0.0041(17) N5 0.031(2) 0.061(2) 0.066(3) -0.006(2) -0.0029(18) 0.0049(18) N6 0.048(2) 0.047(2) 0.054(2) -0.0075(18) 0.0035(18) -0.0009(18) N7 0.051(2) 0.050(2) 0.059(2) -0.004(2) 0.007(2) 0.0084(19) O1 0.054(2) 0.090(3) 0.059(2) -0.014(2) -0.0163(18) 0.008(2) O2 0.055(3) 0.085(3) 0.161(5) -0.050(3) 0.000(3) -0.004(2) C1 0.051(3) 0.047(3) 0.058(3) -0.009(2) -0.009(2) 0.000(2) C2 0.048(3) 0.041(2) 0.049(3) -0.002(2) 0.001(2) 0.000(2) C3 0.046(3) 0.042(2) 0.048(2) 0.001(2) 0.007(2) 0.001(2) C4 0.048(3) 0.050(3) 0.060(3) -0.001(2) 0.000(2) 0.001(2) C5 0.053(3) 0.054(3) 0.079(4) -0.001(3) 0.001(3) 0.010(2) C6 0.064(4) 0.057(3) 0.084(4) -0.008(3) 0.014(3) 0.010(3) C7 0.075(4) 0.057(3) 0.064(3) -0.013(3) 0.010(3) 0.000(3) C8 0.060(3) 0.034(2) 0.051(3) -0.001(2) 0.006(2) -0.002(2) C9 0.044(3) 0.055(3) 0.060(3) -0.003(2) -0.001(2) 0.007(2) C10 0.038(2) 0.049(3) 0.055(3) -0.009(2) -0.002(2) 0.005(2) C11 0.041(2) 0.044(2) 0.051(3) -0.014(2) -0.001(2) -0.002(2) C12 0.039(3) 0.073(4) 0.062(3) -0.002(3) -0.003(2) -0.001(2) C13 0.057(3) 0.080(4) 0.059(3) 0.005(3) -0.003(3) 0.005(3) C14 0.061(3) 0.081(4) 0.059(3) 0.008(3) 0.008(3) 0.005(3) C15 0.047(3) 0.072(4) 0.071(4) -0.004(3) 0.008(3) -0.007(3) C16 0.039(2) 0.051(3) 0.057(3) -0.011(2) 0.003(2) 0.000(2) C17 0.050(3) 0.059(3) 0.050(3) 0.002(2) -0.001(2) 0.003(2) C18 0.041(3) 0.050(3) 0.054(3) -0.006(2) 0.006(2) 0.002(2) C19 0.041(2) 0.053(3) 0.058(3) -0.016(2) 0.014(2) -0.002(2) C20 0.048(3) 0.069(3) 0.060(3) -0.014(3) 0.011(2) -0.006(2) C21 0.056(3) 0.080(4) 0.072(4) -0.036(3) 0.016(3) -0.005(3) C22 0.058(3) 0.064(4) 0.097(5) -0.035(4) 0.024(3) -0.008(3) C23 0.052(3) 0.052(3) 0.095(5) -0.015(3) 0.025(3) 0.005(2) C24 0.044(3) 0.050(3) 0.063(3) -0.009(2) 0.020(2) 0.004(2) C25 0.048(3) 0.106(5) 0.091(5) -0.063(4) -0.016(3) 0.014(4) C26 0.075(5) 0.247(12) 0.097(6) -0.067(7) -0.041(4) 0.043(6) C27 0.074(7) 0.166(12) 0.093(8) 0.003(7) 0.000 0.000 Cl1 0.0770(13) 0.0720(13) 0.0620(11) 0.000 0.000 -0.0241(10) Cl2 0.0834(13) 0.0618(12) 0.0505(10) 0.0083(8) 0.000 0.000 O3 0.157(6) 0.212(8) 0.151(6) 0.000(5) -0.078(5) -0.047(6) O4 0.152(6) 0.182(6) 0.216(7) 0.117(6) 0.057(6) 0.004(5) O5 0.111(4) 0.070(3) 0.069(3) -0.001(2) 0.019(3) -0.001(2) O6 0.157(6) 0.176(6) 0.087(4) 0.011(4) 0.005(3) -0.099(5) O7 0.059(2) 0.070(2) 0.092(3) -0.002(2) -0.009(2) -0.0014(18) _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 O1 1.913(4) . ? Cu1 N2 2.039(4) . ? Cu1 N6 2.049(4) . ? Cu1 N4 2.103(4) . ? Cu1 N1 2.147(4) . ? N1 C17 1.477(6) . ? N1 C1 1.482(6) . ? N1 C9 1.500(6) . ? N2 C2 1.307(6) . ? N2 C3 1.401(6) . ? N3 C2 1.340(6) . ? N3 C8 1.374(6) . ? N3 H3 0.8600 . ? N4 C10 1.300(6) . ? N4 C11 1.394(6) . ? N5 C10 1.349(6) . ? N5 C16 1.380(6) . ? N5 H5A 0.8600 . ? N6 C18 1.309(6) . ? N6 C19 1.408(6) . ? N7 C18 1.343(6) . ? N7 C24 1.370(6) . ? N7 H7A 0.8600 . ? O1 C25 1.237(7) . ? O2 C25 1.231(9) . ? C1 C2 1.491(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C4 1.385(6) . ? C3 C8 1.395(6) . ? C4 C5 1.382(7) . ? C4 H4 0.9300 . ? C5 C6 1.372(8) . ? C5 H5 0.9300 . ? C6 C7 1.375(8) . ? C6 H6 0.9300 . ? C7 C8 1.389(7) . ? C7 H7 0.9300 . ? C9 C10 1.514(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.380(7) . ? C11 C16 1.396(6) . ? C12 C13 1.373(8) . ? C12 H12 0.9300 . ? C13 C14 1.392(7) . ? C13 H13 0.9300 . ? C14 C15 1.376(8) . ? C14 H14 0.9300 . ? C15 C16 1.379(7) . ? C15 H15 0.9300 . ? C17 C18 1.493(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C19 C20 1.387(7) . ? C19 C24 1.392(7) . ? C20 C21 1.392(8) . ? C20 H20 0.9300 . ? C21 C22 1.374(9) . ? C21 H21 0.9300 . ? C22 C23 1.374(9) . ? C22 H22 0.9300 . ? C23 C24 1.393(7) . ? C23 H23 0.9300 . ? C25 C26 1.549(12) . ? C26 C27 1.424(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C26 1.424(10) 4 ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? Cl1 O3 1.369(7) 2_655 ? Cl1 O3 1.369(7) . ? Cl1 O4 1.373(6) . ? Cl1 O4 1.373(6) 2_655 ? Cl2 O6 1.407(6) 4 ? Cl2 O6 1.407(6) . ? Cl2 O5 1.440(4) . ? Cl2 O5 1.440(4) 4 ? O7 H7C 0.8137 . ? O7 H7B 0.8143 . ? 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 O1 Cu1 N2 98.92(15) . . ? O1 Cu1 N6 105.82(17) . . ? N2 Cu1 N6 127.88(15) . . ? O1 Cu1 N4 95.69(16) . . ? N2 Cu1 N4 111.88(15) . . ? N6 Cu1 N4 110.38(15) . . ? O1 Cu1 N1 173.46(16) . . ? N2 Cu1 N1 80.56(14) . . ? N6 Cu1 N1 79.32(15) . . ? N4 Cu1 N1 78.57(15) . . ? C17 N1 C1 111.6(4) . . ? C17 N1 C9 109.7(4) . . ? C1 N1 C9 111.2(4) . . ? C17 N1 Cu1 105.9(3) . . ? C1 N1 Cu1 109.0(3) . . ? C9 N1 Cu1 109.3(3) . . ? C2 N2 C3 105.8(4) . . ? C2 N2 Cu1 113.8(3) . . ? C3 N2 Cu1 140.5(3) . . ? C2 N3 C8 107.3(4) . . ? C2 N3 H3 126.3 . . ? C8 N3 H3 126.3 . . ? C10 N4 C11 105.5(4) . . ? C10 N4 Cu1 113.7(3) . . ? C11 N4 Cu1 140.7(3) . . ? C10 N5 C16 107.4(4) . . ? C10 N5 H5A 126.3 . . ? C16 N5 H5A 126.3 . . ? C18 N6 C19 105.1(4) . . ? C18 N6 Cu1 112.5(3) . . ? C19 N6 Cu1 142.3(3) . . ? C18 N7 C24 106.8(4) . . ? C18 N7 H7A 126.6 . . ? C24 N7 H7A 126.6 . . ? C25 O1 Cu1 128.7(5) . . ? N1 C1 C2 108.5(4) . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N2 C2 N3 112.9(4) . . ? N2 C2 C1 121.9(4) . . ? N3 C2 C1 125.2(4) . . ? C4 C3 C8 120.6(4) . . ? C4 C3 N2 131.4(4) . . ? C8 C3 N2 107.9(4) . . ? C5 C4 C3 117.2(5) . . ? C5 C4 H4 121.4 . . ? C3 C4 H4 121.4 . . ? C6 C5 C4 122.0(5) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 121.6(5) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C6 C7 C8 117.1(5) . . ? C6 C7 H7 121.4 . . ? C8 C7 H7 121.4 . . ? N3 C8 C7 132.5(5) . . ? N3 C8 C3 106.1(4) . . ? C7 C8 C3 121.4(5) . . ? N1 C9 C10 106.6(4) . . ? N1 C9 H9A 110.4 . . ? C10 C9 H9A 110.4 . . ? N1 C9 H9B 110.4 . . ? C10 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? N4 C10 N5 113.0(4) . . ? N4 C10 C9 121.3(4) . . ? N5 C10 C9 125.6(4) . . ? C12 C11 N4 130.4(4) . . ? C12 C11 C16 120.5(5) . . ? N4 C11 C16 109.1(4) . . ? C13 C12 C11 117.0(5) . . ? C13 C12 H12 121.5 . . ? C11 C12 H12 121.5 . . ? C12 C13 C14 122.5(5) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 120.9(5) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 116.7(5) . . ? C14 C15 H15 121.6 . . ? C16 C15 H15 121.6 . . ? C15 C16 N5 132.6(4) . . ? C15 C16 C11 122.4(5) . . ? N5 C16 C11 105.0(4) . . ? N1 C17 C18 106.2(4) . . ? N1 C17 H17A 110.5 . . ? C18 C17 H17A 110.5 . . ? N1 C17 H17B 110.5 . . ? C18 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? N6 C18 N7 113.5(4) . . ? N6 C18 C17 120.6(4) . . ? N7 C18 C17 125.9(4) . . ? C20 C19 C24 121.8(5) . . ? C20 C19 N6 130.3(5) . . ? C24 C19 N6 107.9(4) . . ? C19 C20 C21 116.1(6) . . ? C19 C20 H20 122.0 . . ? C21 C20 H20 122.0 . . ? C22 C21 C20 121.8(6) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 122.6(5) . . ? C21 C22 H22 118.7 . . ? C23 C22 H22 118.7 . . ? C22 C23 C24 116.3(6) . . ? C22 C23 H23 121.8 . . ? C24 C23 H23 121.8 . . ? N7 C24 C19 106.7(4) . . ? N7 C24 C23 132.0(5) . . ? C19 C24 C23 121.4(5) . . ? O2 C25 O1 124.4(7) . . ? O2 C25 C26 120.7(7) . . ? O1 C25 C26 114.8(8) . . ? C27 C26 C25 126.1(9) . . ? C27 C26 H26A 105.8 . . ? C25 C26 H26A 105.8 . . ? C27 C26 H26B 105.8 . . ? C25 C26 H26B 105.8 . . ? H26A C26 H26B 106.2 . . ? C26 C27 C26 110.6(10) . 4 ? C26 C27 H27A 109.5 . . ? C26 C27 H27A 109.5 4 . ? C26 C27 H27B 109.5 . . ? C26 C27 H27B 109.5 4 . ? H27A C27 H27B 108.1 . . ? O3 Cl1 O3 120.2(7) 2_655 . ? O3 Cl1 O4 109.1(5) 2_655 . ? O3 Cl1 O4 107.0(5) . . ? O3 Cl1 O4 107.0(5) 2_655 2_655 ? O3 Cl1 O4 109.1(5) . 2_655 ? O4 Cl1 O4 103.3(9) . 2_655 ? O6 Cl2 O6 117.3(7) 4 . ? O6 Cl2 O5 107.6(3) 4 . ? O6 Cl2 O5 107.3(3) . . ? O6 Cl2 O5 107.3(3) 4 4 ? O6 Cl2 O5 107.6(3) . 4 ? O5 Cl2 O5 109.7(4) . 4 ? H7C O7 H7B 112.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O3 0.86 2.53 3.365(9) 165.0 6 N3 H3 O4 0.86 2.49 3.067(8) 125.6 6 N5 H5A O5 0.86 2.74 3.378(8) 132.0 1_455 N7 H7A O7 0.86 1.96 2.796(6) 163.7 5_665 O7 H7C O2 0.81 2.02 2.801(6) 159.6 . O7 H7B O3 0.81 2.38 3.123(9) 152.4 3_655 C9 H9A O2 0.97 2.44 3.309(7) 149.6 6 C17 H17A O7 0.97 2.38 3.319(6) 161.4 6 C22 H22 O5 0.93 2.43 3.355(7) 173.0 2_665 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.961 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.095 data_7a #TrackingRef '- 1-9.cif' _database_code_depnum_ccdc_archive 'CCDC 788591' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H50 Cu2 N14 O4, 2(Cl O4), 5(H2 O)' _chemical_formula_sum 'C54 H60 Cl2 Cu2 N14 O17' _chemical_formula_weight 1375.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.3801(12) _cell_length_b 15.1830(9) _cell_length_c 10.2220(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.282(1) _cell_angle_gamma 90.00 _cell_volume 3154.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3714 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 19.67 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8790 _exptl_absorpt_correction_T_max 0.9361 _exptl_absorpt_process_details 'SADABS, Sheldrick,1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 21408 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.1293 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5476 _reflns_number_gt 2500 _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. In the refinement, the ClO~4~^-^ anion was found to be disordered over two sites with the final occupancies of 0.57(1):0.43(1) for the major and minor components, respectively. Command 'DFIX' was used during the refinement to restrain the Cl-O bond lengths and O...O distances of 1.38(1) and 2.25(1) \%A, respectively. Because the electron densities of solvent molecules are too diffused to allow the accurate refinement of one unit molecule, the occupancies of water O8-O10 atoms were refined freely and their final outcome are of ca. 0.70(1), 0.60(1) and 0.20(1), respectively. All the C- and N-bounded hydrogen atoms were postitioned geometrically. Hydrogen atoms attached to water oxygen atoms were positioned best matching their hydrogen-bond enviroment with O-H=0.82\%A and U~iso~(H)=1.2U~eq~(O). ; _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^)+(0.0981P)^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 5476 _refine_ls_number_parameters 443 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1205 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.2012 _refine_ls_wR_factor_gt 0.1889 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.866 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.71381(3) 0.51623(5) 0.14806(7) 0.0585(3) Uani 1 1 d . . . C1 C 0.8543(3) 0.5566(4) 0.1508(7) 0.0711(19) Uani 1 1 d . . . H1A H 0.8951 0.5555 0.1077 0.085 Uiso 1 1 calc R . . H1B H 0.8547 0.6075 0.2081 0.085 Uiso 1 1 calc R . . C2 C 0.8470(3) 0.4742(4) 0.2277(6) 0.0575(15) Uani 1 1 d . . . C3 C 0.8004(3) 0.3700(4) 0.3333(6) 0.0557(16) Uani 1 1 d . . . C4 C 0.7579(3) 0.3138(4) 0.3891(7) 0.0673(18) Uani 1 1 d . . . H4 H 0.7128 0.3174 0.3686 0.081 Uiso 1 1 calc R . . C5 C 0.7840(4) 0.2522(5) 0.4764(8) 0.082(2) Uani 1 1 d . . . H5 H 0.7561 0.2136 0.5158 0.098 Uiso 1 1 calc R . . C6 C 0.8518(4) 0.2465(5) 0.5070(8) 0.096(3) Uani 1 1 d . . . H6 H 0.8677 0.2060 0.5698 0.115 Uiso 1 1 calc R . . C7 C 0.8954(4) 0.2986(6) 0.4480(8) 0.095(2) Uani 1 1 d . . . H7 H 0.9407 0.2921 0.4638 0.114 Uiso 1 1 calc R . . C8 C 0.8676(3) 0.3621(4) 0.3622(7) 0.0702(18) Uani 1 1 d . . . C9 C 0.8069(3) 0.5010(5) -0.0601(7) 0.075(2) Uani 1 1 d . . . H9A H 0.8245 0.5341 -0.1307 0.090 Uiso 1 1 calc R . . H9B H 0.8384 0.4557 -0.0323 0.090 Uiso 1 1 calc R . . C10 C 0.7444(3) 0.4601(4) -0.1074(7) 0.0604(16) Uani 1 1 d . . . C11 C 0.6467(3) 0.4039(4) -0.1018(6) 0.0577(16) Uani 1 1 d . . . C12 C 0.5848(3) 0.3782(5) -0.0692(7) 0.0729(19) Uani 1 1 d . . . H12 H 0.5681 0.3951 0.0093 0.088 Uiso 1 1 calc R . . C13 C 0.5493(4) 0.3265(5) -0.1592(8) 0.087(2) Uani 1 1 d . . . H13 H 0.5077 0.3074 -0.1401 0.105 Uiso 1 1 calc R . . C14 C 0.5724(4) 0.3023(6) -0.2746(8) 0.097(3) Uani 1 1 d . . . H14 H 0.5464 0.2671 -0.3319 0.116 Uiso 1 1 calc R . . C15 C 0.6345(4) 0.3288(5) -0.3103(7) 0.083(2) Uani 1 1 d . . . H15 H 0.6506 0.3121 -0.3893 0.099 Uiso 1 1 calc R . . C16 C 0.6694(3) 0.3801(4) -0.2221(6) 0.0591(16) Uani 1 1 d . . . C17 C 0.7839(3) 0.6530(4) 0.0090(7) 0.0687(18) Uani 1 1 d . . . H17A H 0.8252 0.6847 0.0089 0.082 Uiso 1 1 calc R . . H17B H 0.7631 0.6536 -0.0795 0.082 Uiso 1 1 calc R . . C18 C 0.7412(3) 0.6960(4) 0.0976(6) 0.0605(17) Uani 1 1 d . . . C19 C 0.6690(3) 0.7122(4) 0.2409(7) 0.0607(17) Uani 1 1 d . . . C20 C 0.6264(3) 0.7033(4) 0.3369(7) 0.0696(18) Uani 1 1 d . . . H20 H 0.6177 0.6484 0.3719 0.083 Uiso 1 1 calc R . . C21 C 0.5965(4) 0.7780(5) 0.3806(8) 0.084(2) Uani 1 1 d . . . H21 H 0.5678 0.7740 0.4469 0.101 Uiso 1 1 calc R . . C22 C 0.6093(4) 0.8598(6) 0.3249(10) 0.096(3) Uani 1 1 d . . . H22 H 0.5866 0.9088 0.3521 0.115 Uiso 1 1 calc R . . C23 C 0.6515(4) 0.8705(5) 0.2371(9) 0.089(2) Uani 1 1 d . . . H23 H 0.6604 0.9262 0.2049 0.107 Uiso 1 1 calc R . . C24 C 0.6833(3) 0.7950(4) 0.1919(7) 0.0653(18) Uani 1 1 d . . . C25 C 0.6254(3) 0.4782(4) 0.3390(8) 0.0630(17) Uani 1 1 d . . . C26 C 0.5561(3) 0.4567(5) 0.3683(8) 0.087(2) Uani 1 1 d . . . H26A H 0.5530 0.3942 0.3867 0.104 Uiso 1 1 calc R . . H26B H 0.5268 0.4694 0.2914 0.104 Uiso 1 1 calc R . . C27 C 0.5336(3) 0.5087(5) 0.4848(7) 0.084(2) Uani 1 1 d . . . H27A H 0.5628 0.4951 0.5615 0.101 Uiso 1 1 calc R . . H27B H 0.5380 0.5711 0.4668 0.101 Uiso 1 1 calc R . . N1 N 0.7966(2) 0.5606(3) 0.0513(5) 0.0606(14) Uani 1 1 d . . . N2 N 0.7889(2) 0.4414(3) 0.2467(5) 0.0551(13) Uani 1 1 d . . . N3 N 0.8958(3) 0.4286(4) 0.2918(5) 0.0752(16) Uani 1 1 d . . . H3 H 0.9373 0.4388 0.2897 0.090 Uiso 1 1 calc R . . N4 N 0.6947(2) 0.4555(3) -0.0309(5) 0.0551(13) Uani 1 1 d . . . N5 N 0.7315(3) 0.4173(3) -0.2211(5) 0.0678(14) Uani 1 1 d . . . H5A H 0.7576 0.4135 -0.2833 0.081 Uiso 1 1 calc R . . N6 N 0.7059(2) 0.6503(3) 0.1772(5) 0.0586(13) Uani 1 1 d . . . N7 N 0.7293(3) 0.7824(4) 0.1059(6) 0.0698(16) Uani 1 1 d . . . H7A H 0.7480 0.8231 0.0634 0.084 Uiso 1 1 calc R . . O1 O 0.63372(19) 0.4785(3) 0.2156(5) 0.0695(12) Uani 1 1 d . . . O2 O 0.6679(2) 0.4948(3) 0.4260(5) 0.0791(14) Uani 1 1 d . . . Cl1 Cl 0.9326(5) 0.8017(7) 0.2577(8) 0.116(2) Uani 0.57 1 d PD A 1 O3 O 0.8748(9) 0.7702(14) 0.304(2) 0.202(9) Uani 0.57 1 d PD A 1 O4 O 0.9863(9) 0.7672(12) 0.327(2) 0.254(7) Uani 0.57 1 d PD A 1 O5 O 0.9352(9) 0.8885(7) 0.2457(18) 0.254(7) Uani 0.57 1 d PD A 1 O6 O 0.9324(9) 0.7619(10) 0.1311(11) 0.197(6) Uani 0.57 1 d PD A 1 Cl1' Cl 0.9311(7) 0.7871(9) 0.3034(12) 0.116(2) Uani 0.43 1 d PD B 2 O3' O 0.9223(12) 0.7032(9) 0.3607(19) 0.236(9) Uani 0.43 1 d PD B 2 O4' O 0.9846(11) 0.7821(16) 0.233(2) 0.236(9) Uani 0.43 1 d PD B 2 O5' O 0.9385(8) 0.8460(11) 0.4031(16) 0.168(7) Uani 0.43 1 d PD B 2 O6' O 0.8736(9) 0.8038(14) 0.2263(17) 0.126(7) Uani 0.43 1 d PD B 2 O7 O 0.7841(3) 0.9235(4) 0.9868(7) 0.138(2) Uani 1 1 d . . . H7C H 0.7539 0.9431 0.9326 0.165 Uiso 1 1 d R . . H7D H 0.8070 0.9583 1.0368 0.165 Uiso 1 1 d R . . O8 O 0.8461(4) 0.4497(7) 0.6506(9) 0.139(3) Uani 0.70 1 d P . . H8A H 0.8861 0.4652 0.6633 0.167 Uiso 0.70 1 d PR . . H8B H 0.8471 0.3964 0.6253 0.167 Uiso 0.70 1 d PR . . O9 O 0.0291(5) 0.9303(8) 0.5246(13) 0.153(4) Uani 0.60 1 d P . . H9C H 0.0144 0.9746 0.4871 0.183 Uiso 0.60 1 d PR . . H9D H 0.0332 0.9226 0.6042 0.183 Uiso 0.60 1 d PR . . O10 O 0.0135(9) 0.5383(15) 0.324(2) 0.083(7) Uani 0.20 1 d P . . H10A H 0.0234 0.5720 0.2620 0.100 Uiso 0.20 1 d PR . . H10B H -0.0064 0.5552 0.3895 0.100 Uiso 0.20 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0542(5) 0.0544(5) 0.0681(6) -0.0030(4) 0.0121(4) -0.0107(3) C1 0.059(4) 0.076(5) 0.077(5) 0.002(4) 0.001(4) -0.017(3) C2 0.050(4) 0.062(4) 0.060(4) 0.006(3) -0.004(3) 0.001(3) C3 0.048(4) 0.056(4) 0.064(4) -0.007(3) 0.008(3) 0.001(3) C4 0.072(4) 0.047(4) 0.084(5) 0.005(4) 0.014(4) 0.002(3) C5 0.088(6) 0.059(5) 0.099(6) 0.009(4) 0.018(5) -0.003(4) C6 0.102(7) 0.079(5) 0.106(7) 0.036(5) -0.003(5) 0.009(5) C7 0.079(5) 0.093(6) 0.109(7) 0.016(5) -0.010(5) 0.006(5) C8 0.073(5) 0.059(4) 0.077(5) 0.014(4) -0.002(4) 0.002(4) C9 0.067(4) 0.088(5) 0.072(5) -0.007(4) 0.021(4) -0.017(4) C10 0.052(4) 0.061(4) 0.070(5) 0.000(4) 0.015(3) -0.005(3) C11 0.052(4) 0.054(4) 0.066(4) 0.001(3) -0.001(3) -0.007(3) C12 0.069(5) 0.078(5) 0.071(5) -0.008(4) 0.006(4) -0.018(4) C13 0.075(5) 0.107(6) 0.081(6) -0.011(5) 0.008(4) -0.029(4) C14 0.087(6) 0.123(7) 0.077(6) -0.024(5) -0.013(5) -0.027(5) C15 0.087(6) 0.098(6) 0.063(5) -0.015(4) 0.007(4) -0.013(4) C16 0.060(4) 0.061(4) 0.057(4) -0.008(3) 0.009(3) -0.004(3) C17 0.063(4) 0.073(5) 0.070(5) 0.015(4) 0.002(4) -0.018(3) C18 0.057(4) 0.060(5) 0.061(4) 0.011(3) -0.013(3) -0.011(3) C19 0.070(4) 0.044(4) 0.065(4) -0.004(3) -0.019(4) 0.000(3) C20 0.076(5) 0.051(4) 0.082(5) -0.010(4) 0.008(4) -0.003(3) C21 0.081(5) 0.073(5) 0.099(6) -0.029(5) -0.003(4) 0.003(4) C22 0.084(6) 0.062(6) 0.138(8) -0.027(5) -0.013(6) 0.011(4) C23 0.087(6) 0.044(4) 0.130(8) 0.003(5) -0.032(5) 0.005(4) C24 0.060(4) 0.055(5) 0.077(5) 0.011(4) -0.021(4) -0.010(3) C25 0.060(4) 0.041(3) 0.090(6) -0.012(4) 0.022(4) -0.002(3) C26 0.071(5) 0.082(5) 0.112(6) -0.025(4) 0.041(4) -0.019(4) C27 0.078(5) 0.082(5) 0.097(6) -0.010(4) 0.041(4) -0.009(4) N1 0.053(3) 0.067(4) 0.063(3) 0.003(3) 0.005(3) -0.013(2) N2 0.053(3) 0.047(3) 0.065(3) -0.003(3) 0.009(3) -0.003(2) N3 0.054(3) 0.092(4) 0.080(4) -0.002(3) 0.003(3) -0.012(3) N4 0.055(3) 0.055(3) 0.056(3) -0.001(2) 0.005(3) -0.004(2) N5 0.076(4) 0.071(4) 0.058(4) -0.013(3) 0.016(3) -0.003(3) N6 0.063(3) 0.049(3) 0.063(3) 0.002(3) 0.002(3) -0.009(2) N7 0.075(4) 0.049(4) 0.081(4) 0.019(3) -0.021(3) -0.013(3) O1 0.063(3) 0.072(3) 0.076(3) -0.019(3) 0.021(2) -0.017(2) O2 0.063(3) 0.087(4) 0.088(4) -0.007(3) 0.011(3) 0.004(3) Cl1 0.099(2) 0.131(4) 0.121(6) -0.010(4) 0.028(5) 0.004(3) O3 0.164(19) 0.23(3) 0.21(2) -0.006(19) 0.032(16) 0.003(15) O4 0.246(16) 0.243(17) 0.267(18) 0.023(15) -0.019(14) 0.026(13) O5 0.246(16) 0.243(17) 0.267(18) 0.023(15) -0.019(14) 0.026(13) O6 0.213(17) 0.196(15) 0.186(16) -0.036(13) 0.041(14) -0.022(13) Cl1' 0.099(2) 0.131(4) 0.121(6) -0.010(4) 0.028(5) 0.004(3) O3' 0.22(2) 0.25(2) 0.24(2) -0.008(18) 0.022(17) 0.016(18) O4' 0.22(2) 0.25(2) 0.24(2) -0.008(18) 0.022(17) 0.016(18) O5' 0.164(16) 0.184(18) 0.155(16) -0.054(15) 0.017(13) -0.011(13) O6' 0.078(12) 0.175(19) 0.125(16) 0.020(13) -0.004(10) -0.002(10) O7 0.096(4) 0.124(5) 0.189(6) 0.085(5) -0.014(4) -0.011(3) O8 0.129(7) 0.174(9) 0.119(7) -0.042(6) 0.042(6) -0.005(6) O9 0.109(8) 0.155(10) 0.196(12) -0.037(9) 0.028(8) -0.027(7) O10 0.040(12) 0.091(16) 0.114(19) -0.038(14) -0.027(12) -0.009(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.907(4) . ? Cu1 N4 2.059(5) . ? Cu1 N6 2.065(5) . ? Cu1 N2 2.102(5) . ? Cu1 N1 2.129(5) . ? C1 C2 1.490(8) . ? C1 N1 1.496(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.312(7) . ? C2 N3 1.342(7) . ? C3 C4 1.369(8) . ? C3 C8 1.385(8) . ? C3 N2 1.409(7) . ? C4 C5 1.372(9) . ? C4 H4 0.9300 . ? C5 C6 1.395(10) . ? C5 H5 0.9300 . ? C6 C7 1.363(10) . ? C6 H6 0.9300 . ? C7 C8 1.396(10) . ? C7 H7 0.9300 . ? C8 N3 1.389(8) . ? C9 C10 1.466(9) . ? C9 N1 1.482(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.326(7) . ? C10 N5 1.341(7) . ? C11 C12 1.385(8) . ? C11 C16 1.393(8) . ? C11 N4 1.412(7) . ? C12 C13 1.373(9) . ? C12 H12 0.9300 . ? C13 C14 1.353(10) . ? C13 H13 0.9300 . ? C14 C15 1.401(10) . ? C14 H14 0.9300 . ? C15 C16 1.353(9) . ? C15 H15 0.9300 . ? C16 N5 1.385(7) . ? C17 C18 1.457(9) . ? C17 N1 1.484(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.323(7) . ? C18 N7 1.337(8) . ? C19 C20 1.366(9) . ? C19 C24 1.392(8) . ? C19 N6 1.394(8) . ? C20 C21 1.376(9) . ? C20 H20 0.9300 . ? C21 C22 1.399(11) . ? C21 H21 0.9300 . ? C22 C23 1.298(10) . ? C22 H22 0.9300 . ? C23 C24 1.413(10) . ? C23 H23 0.9300 . ? C24 N7 1.346(8) . ? C25 O2 1.221(8) . ? C25 O1 1.285(8) . ? C25 C26 1.502(9) . ? C26 C27 1.528(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C27 1.452(12) 3_666 ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? N3 H3 0.8600 . ? N5 H5A 0.8600 . ? N7 H7A 0.8600 . ? Cl1 O5 1.326(8) . ? Cl1 O4 1.366(8) . ? Cl1 O3 1.388(8) . ? Cl1 O6 1.428(8) . ? Cl1' O4' 1.354(9) . ? Cl1' O5' 1.356(9) . ? Cl1' O6' 1.387(9) . ? Cl1' O3' 1.418(9) . ? O7 H7C 0.8499 . ? O7 H7D 0.8500 . ? O8 H8A 0.8498 . ? O8 H8B 0.8501 . ? O9 H9C 0.8200 . ? O9 H9D 0.8200 . ? O10 H10A 0.8501 . ? O10 H10B 0.8500 . ? 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 O1 Cu1 N4 94.43(19) . . ? O1 Cu1 N6 99.52(19) . . ? N4 Cu1 N6 123.89(19) . . ? O1 Cu1 N2 106.0(2) . . ? N4 Cu1 N2 105.46(18) . . ? N6 Cu1 N2 121.71(18) . . ? O1 Cu1 N1 173.3(2) . . ? N4 Cu1 N1 80.36(19) . . ? N6 Cu1 N1 80.1(2) . . ? N2 Cu1 N1 79.62(19) . . ? C2 C1 N1 106.8(5) . . ? C2 C1 H1A 110.4 . . ? N1 C1 H1A 110.4 . . ? C2 C1 H1B 110.4 . . ? N1 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? N2 C2 N3 112.1(6) . . ? N2 C2 C1 121.5(5) . . ? N3 C2 C1 126.2(6) . . ? C4 C3 C8 120.2(6) . . ? C4 C3 N2 131.4(6) . . ? C8 C3 N2 108.4(5) . . ? C3 C4 C5 118.0(7) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? C4 C5 C6 121.1(7) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 122.1(7) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C6 C7 C8 115.6(7) . . ? C6 C7 H7 122.2 . . ? C8 C7 H7 122.2 . . ? C3 C8 N3 105.6(6) . . ? C3 C8 C7 122.8(7) . . ? N3 C8 C7 131.6(7) . . ? C10 C9 N1 110.1(5) . . ? C10 C9 H9A 109.6 . . ? N1 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? N1 C9 H9B 109.6 . . ? H9A C9 H9B 108.2 . . ? N4 C10 N5 112.2(5) . . ? N4 C10 C9 120.7(6) . . ? N5 C10 C9 126.9(6) . . ? C12 C11 C16 120.6(6) . . ? C12 C11 N4 129.9(6) . . ? C16 C11 N4 109.5(5) . . ? C13 C12 C11 116.3(6) . . ? C13 C12 H12 121.9 . . ? C11 C12 H12 121.9 . . ? C14 C13 C12 122.6(7) . . ? C14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? C13 C14 C15 121.9(7) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C16 C15 C14 115.6(7) . . ? C16 C15 H15 122.2 . . ? C14 C15 H15 122.2 . . ? C15 C16 N5 132.4(6) . . ? C15 C16 C11 123.0(6) . . ? N5 C16 C11 104.6(5) . . ? C18 C17 N1 110.0(5) . . ? C18 C17 H17A 109.7 . . ? N1 C17 H17A 109.7 . . ? C18 C17 H17B 109.7 . . ? N1 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N6 C18 N7 111.5(6) . . ? N6 C18 C17 121.6(6) . . ? N7 C18 C17 126.8(6) . . ? C20 C19 C24 120.6(7) . . ? C20 C19 N6 131.6(6) . . ? C24 C19 N6 107.8(6) . . ? C19 C20 C21 118.2(7) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? C20 C21 C22 119.9(8) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 123.1(8) . . ? C23 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? C22 C23 C24 117.9(8) . . ? C22 C23 H23 121.1 . . ? C24 C23 H23 121.1 . . ? N7 C24 C19 106.4(6) . . ? N7 C24 C23 133.5(7) . . ? C19 C24 C23 120.2(8) . . ? O2 C25 O1 125.1(6) . . ? O2 C25 C26 121.8(7) . . ? O1 C25 C26 113.1(7) . . ? C25 C26 C27 112.6(6) . . ? C25 C26 H26A 109.1 . . ? C27 C26 H26A 109.1 . . ? C25 C26 H26B 109.1 . . ? C27 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C27 C27 C26 114.5(8) 3_666 . ? C27 C27 H27A 108.6 3_666 . ? C26 C27 H27A 108.6 . . ? C27 C27 H27B 108.6 3_666 . ? C26 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? C9 N1 C17 112.6(5) . . ? C9 N1 C1 110.4(5) . . ? C17 N1 C1 110.4(5) . . ? C9 N1 Cu1 109.0(4) . . ? C17 N1 Cu1 107.9(4) . . ? C1 N1 Cu1 106.3(4) . . ? C2 N2 C3 106.0(5) . . ? C2 N2 Cu1 110.9(4) . . ? C3 N2 Cu1 143.0(4) . . ? C2 N3 C8 107.9(5) . . ? C2 N3 H3 126.1 . . ? C8 N3 H3 126.1 . . ? C10 N4 C11 104.9(5) . . ? C10 N4 Cu1 113.5(4) . . ? C11 N4 Cu1 141.5(4) . . ? C10 N5 C16 108.9(5) . . ? C10 N5 H5A 125.6 . . ? C16 N5 H5A 125.6 . . ? C18 N6 C19 105.7(5) . . ? C18 N6 Cu1 112.1(4) . . ? C19 N6 Cu1 141.5(4) . . ? C18 N7 C24 108.6(6) . . ? C18 N7 H7A 125.7 . . ? C24 N7 H7A 125.7 . . ? C25 O1 Cu1 122.4(4) . . ? O5 Cl1 O4 113.2(8) . . ? O5 Cl1 O3 114.5(8) . . ? O4 Cl1 O3 110.9(8) . . ? O5 Cl1 O6 109.5(8) . . ? O4 Cl1 O6 105.0(8) . . ? O3 Cl1 O6 102.8(7) . . ? O4' Cl1' O5' 112.9(9) . . ? O4' Cl1' O6' 112.8(9) . . ? O5' Cl1' O6' 110.4(8) . . ? O4' Cl1' O3' 107.5(8) . . ? O5' Cl1' O3' 107.0(8) . . ? O6' Cl1' O3' 105.8(8) . . ? H7C O7 H7D 120.8 . . ? H8A O8 H8B 105.4 . . ? H9C O9 H9D 125.9 . . ? H10A O10 H10B 124.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -30.1(8) . . . . ? N1 C1 C2 N3 154.6(6) . . . . ? C8 C3 C4 C5 1.8(10) . . . . ? N2 C3 C4 C5 -176.7(6) . . . . ? C3 C4 C5 C6 -0.3(11) . . . . ? C4 C5 C6 C7 -3.1(13) . . . . ? C5 C6 C7 C8 4.5(12) . . . . ? C4 C3 C8 N3 -179.2(5) . . . . ? N2 C3 C8 N3 -0.4(7) . . . . ? C4 C3 C8 C7 -0.2(10) . . . . ? N2 C3 C8 C7 178.6(6) . . . . ? C6 C7 C8 C3 -2.9(11) . . . . ? C6 C7 C8 N3 175.8(7) . . . . ? N1 C9 C10 N4 -21.0(9) . . . . ? N1 C9 C10 N5 165.4(6) . . . . ? C16 C11 C12 C13 2.2(10) . . . . ? N4 C11 C12 C13 -179.4(6) . . . . ? C11 C12 C13 C14 -0.9(12) . . . . ? C12 C13 C14 C15 -0.1(13) . . . . ? C13 C14 C15 C16 -0.2(12) . . . . ? C14 C15 C16 N5 178.9(7) . . . . ? C14 C15 C16 C11 1.6(11) . . . . ? C12 C11 C16 C15 -2.7(10) . . . . ? N4 C11 C16 C15 178.6(6) . . . . ? C12 C11 C16 N5 179.3(6) . . . . ? N4 C11 C16 N5 0.6(7) . . . . ? N1 C17 C18 N6 -17.4(8) . . . . ? N1 C17 C18 N7 166.3(5) . . . . ? C24 C19 C20 C21 2.0(9) . . . . ? N6 C19 C20 C21 -179.6(6) . . . . ? C19 C20 C21 C22 1.1(10) . . . . ? C20 C21 C22 C23 -3.8(12) . . . . ? C21 C22 C23 C24 3.0(12) . . . . ? C20 C19 C24 N7 176.3(6) . . . . ? N6 C19 C24 N7 -2.5(7) . . . . ? C20 C19 C24 C23 -2.8(9) . . . . ? N6 C19 C24 C23 178.4(6) . . . . ? C22 C23 C24 N7 -178.5(7) . . . . ? C22 C23 C24 C19 0.3(10) . . . . ? O2 C25 C26 C27 35.5(9) . . . . ? O1 C25 C26 C27 -143.5(6) . . . . ? C25 C26 C27 C27 178.9(8) . . . 3_666 ? C10 C9 N1 C17 -92.9(6) . . . . ? C10 C9 N1 C1 143.2(5) . . . . ? C10 C9 N1 Cu1 26.8(6) . . . . ? C18 C17 N1 C9 149.2(5) . . . . ? C18 C17 N1 C1 -86.9(6) . . . . ? C18 C17 N1 Cu1 28.9(6) . . . . ? C2 C1 N1 C9 -78.3(6) . . . . ? C2 C1 N1 C17 156.6(5) . . . . ? C2 C1 N1 Cu1 39.8(6) . . . . ? N4 Cu1 N1 C9 -20.4(4) . . . . ? N6 Cu1 N1 C9 -147.5(4) . . . . ? N2 Cu1 N1 C9 87.4(4) . . . . ? N4 Cu1 N1 C17 102.2(4) . . . . ? N6 Cu1 N1 C17 -25.0(4) . . . . ? N2 Cu1 N1 C17 -150.0(4) . . . . ? N4 Cu1 N1 C1 -139.4(4) . . . . ? N6 Cu1 N1 C1 93.4(4) . . . . ? N2 Cu1 N1 C1 -31.6(4) . . . . ? N3 C2 N2 C3 1.8(7) . . . . ? C1 C2 N2 C3 -174.1(6) . . . . ? N3 C2 N2 Cu1 178.8(4) . . . . ? C1 C2 N2 Cu1 2.9(7) . . . . ? C4 C3 N2 C2 177.8(7) . . . . ? C8 C3 N2 C2 -0.8(7) . . . . ? C4 C3 N2 Cu1 2.5(11) . . . . ? C8 C3 N2 Cu1 -176.1(5) . . . . ? O1 Cu1 N2 C2 -167.0(4) . . . . ? N4 Cu1 N2 C2 93.6(4) . . . . ? N6 Cu1 N2 C2 -54.7(5) . . . . ? N1 Cu1 N2 C2 16.7(4) . . . . ? O1 Cu1 N2 C3 8.2(7) . . . . ? N4 Cu1 N2 C3 -91.2(6) . . . . ? N6 Cu1 N2 C3 120.5(6) . . . . ? N1 Cu1 N2 C3 -168.1(6) . . . . ? N2 C2 N3 C8 -2.1(7) . . . . ? C1 C2 N3 C8 173.6(6) . . . . ? C3 C8 N3 C2 1.5(7) . . . . ? C7 C8 N3 C2 -177.4(8) . . . . ? N5 C10 N4 C11 1.1(7) . . . . ? C9 C10 N4 C11 -173.3(6) . . . . ? N5 C10 N4 Cu1 177.7(4) . . . . ? C9 C10 N4 Cu1 3.2(7) . . . . ? C12 C11 N4 C10 -179.6(7) . . . . ? C16 C11 N4 C10 -1.0(7) . . . . ? C12 C11 N4 Cu1 5.4(11) . . . . ? C16 C11 N4 Cu1 -176.0(5) . . . . ? O1 Cu1 N4 C10 -174.3(4) . . . . ? N6 Cu1 N4 C10 81.1(5) . . . . ? N2 Cu1 N4 C10 -66.3(4) . . . . ? N1 Cu1 N4 C10 10.0(4) . . . . ? O1 Cu1 N4 C11 0.4(6) . . . . ? N6 Cu1 N4 C11 -104.2(6) . . . . ? N2 Cu1 N4 C11 108.4(6) . . . . ? N1 Cu1 N4 C11 -175.3(6) . . . . ? N4 C10 N5 C16 -0.8(7) . . . . ? C9 C10 N5 C16 173.3(6) . . . . ? C15 C16 N5 C10 -177.7(7) . . . . ? C11 C16 N5 C10 0.1(7) . . . . ? N7 C18 N6 C19 -0.1(6) . . . . ? C17 C18 N6 C19 -176.9(5) . . . . ? N7 C18 N6 Cu1 172.3(4) . . . . ? C17 C18 N6 Cu1 -4.5(7) . . . . ? C20 C19 N6 C18 -176.9(7) . . . . ? C24 C19 N6 C18 1.6(6) . . . . ? C20 C19 N6 Cu1 14.4(11) . . . . ? C24 C19 N6 Cu1 -167.1(5) . . . . ? O1 Cu1 N6 C18 -156.5(4) . . . . ? N4 Cu1 N6 C18 -54.5(5) . . . . ? N2 Cu1 N6 C18 87.9(4) . . . . ? N1 Cu1 N6 C18 16.7(4) . . . . ? O1 Cu1 N6 C19 11.8(7) . . . . ? N4 Cu1 N6 C19 113.7(6) . . . . ? N2 Cu1 N6 C19 -103.9(6) . . . . ? N1 Cu1 N6 C19 -175.1(6) . . . . ? N6 C18 N7 C24 -1.5(7) . . . . ? C17 C18 N7 C24 175.1(6) . . . . ? C19 C24 N7 C18 2.4(7) . . . . ? C23 C24 N7 C18 -178.7(7) . . . . ? O2 C25 O1 Cu1 -6.1(9) . . . . ? C26 C25 O1 Cu1 172.9(4) . . . . ? N4 Cu1 O1 C25 161.6(5) . . . . ? N6 Cu1 O1 C25 -72.9(5) . . . . ? N2 Cu1 O1 C25 54.2(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5A O8 0.86 2.05 2.805(10) 146.5 1_554 N7 H7A O7 0.86 1.89 2.742(8) 172.0 1_554 O7 H7C O2 0.85 1.99 2.704(8) 141.4 4_576 O7 H7D O8 0.85 1.95 2.791(13) 170.2 4_576 O9 H9C O9 0.82 1.69 2.46(2) 154.7 3_576 C17 H17A O3 0.97 2.49 3.122(18) 123.0 4_575 N3 H3 O10 0.86 2.18 2.918(19) 144.2 1_655 O8 H8A O5 0.85 2.55 3.165(18) 129.8 4_576 O8 H8A O10 0.85 2.04 2.86(2) 161.6 3_666 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.726 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.105 _vrf_PLAT420_7a ; PROBLEM: -H Without Acceptor >O8 - >H8A ... ? RESPONSE: This is due to the disorder of some water molecules. ; # END data_7b #TrackingRef '- 1-9.cif' _database_code_depnum_ccdc_archive 'CCDC 788592' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H92 Cu4 N28 O4, 6(Cl O4), 4(H2 O)' _chemical_formula_sum 'C102 H100 Cl6 Cu4 N28 O32' _chemical_formula_weight 2697.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1837(13) _cell_length_b 14.2473(16) _cell_length_c 19.720(2) _cell_angle_alpha 71.091(2) _cell_angle_beta 84.728(3) _cell_angle_gamma 71.533(2) _cell_volume 2819.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5444 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 22.55 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1382 _exptl_absorpt_coefficient_mu 0.979 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8261 _exptl_absorpt_correction_T_max 0.9619 _exptl_absorpt_process_details 'SADABS, (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 30234 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.50 _reflns_number_total 11484 _reflns_number_gt 7148 _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. In the refinement, the perchlorate O3, O4 and O6 atoms were found to be disordered over two sites with the final satisfactory occupancies of 0.53(1):0.47(1) for the major and minor components, respectively. Command 'DFIX' was used to restrain the Cl-O bond lengths and O...O distances of 1.38(1)\%A and 2.25(2) \%A, respectively. These sites of water O16 and O17 atoms are only partially occupied with the final occupancies of ca. 0.52(1) and 0.48(1), respectively. All the C- and N-bounded hydrogen atoms were postitioned geometrically. Hydrogen atoms attached to water oxygen atoms were positioned best matching their hydrogen-bond enviroment with O-H=0.82\%A and U~iso~(H)=1.2U~eq~(O). ; _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^)+(0.0990P)^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 11484 _refine_ls_number_parameters 812 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1761 _refine_ls_wR_factor_gt 0.1590 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.24959(4) 0.23468(4) 0.30478(3) 0.03815(16) Uani 1 1 d . . . Cu2 Cu 0.15388(4) -0.01763(4) 0.23881(3) 0.04087(16) Uani 1 1 d . . . C1 C 0.1357(4) 0.3096(4) 0.1545(3) 0.0547(12) Uani 1 1 d . . . H1A H 0.1244 0.2481 0.1481 0.066 Uiso 1 1 calc R . . H1B H 0.1212 0.3642 0.1086 0.066 Uiso 1 1 calc R . . C2 C 0.0437(4) 0.3445(3) 0.2086(3) 0.0484(11) Uani 1 1 d . . . C3 C -0.1312(4) 0.4124(3) 0.2597(3) 0.0545(13) Uani 1 1 d . . . C4 C -0.2509(5) 0.4624(4) 0.2787(4) 0.0759(18) Uani 1 1 d . . . H4 H -0.3140 0.5025 0.2444 0.091 Uiso 1 1 calc R . . C5 C -0.2727(5) 0.4511(5) 0.3490(4) 0.084(2) Uani 1 1 d . . . H5 H -0.3522 0.4849 0.3628 0.100 Uiso 1 1 calc R . . C6 C -0.1803(5) 0.3905(4) 0.4015(3) 0.0709(15) Uani 1 1 d . . . H6 H -0.2000 0.3830 0.4494 0.085 Uiso 1 1 calc R . . C7 C -0.0590(4) 0.3412(4) 0.3834(3) 0.0549(12) Uani 1 1 d . . . H7 H 0.0035 0.3014 0.4181 0.066 Uiso 1 1 calc R . . C8 C -0.0358(4) 0.3538(3) 0.3123(3) 0.0460(11) Uani 1 1 d . . . C9 C 0.3117(5) 0.3764(4) 0.1584(3) 0.0613(14) Uani 1 1 d . . . H9A H 0.2566 0.4320 0.1213 0.074 Uiso 1 1 calc R . . H9B H 0.3953 0.3578 0.1386 0.074 Uiso 1 1 calc R . . C10 C 0.3170(4) 0.4141(3) 0.2200(3) 0.0468(11) Uani 1 1 d . . . C11 C 0.3484(4) 0.5110(4) 0.2804(3) 0.0593(14) Uani 1 1 d . . . C12 C 0.3727(5) 0.5844(4) 0.3046(5) 0.085(2) Uani 1 1 d . . . H12 H 0.3911 0.6425 0.2730 0.102 Uiso 1 1 calc R . . C13 C 0.3686(5) 0.5675(5) 0.3774(5) 0.088(2) Uani 1 1 d . . . H13 H 0.3839 0.6152 0.3957 0.106 Uiso 1 1 calc R . . C14 C 0.3422(5) 0.4813(5) 0.4234(4) 0.0797(18) Uani 1 1 d . . . H14 H 0.3401 0.4721 0.4723 0.096 Uiso 1 1 calc R . . C15 C 0.3185(4) 0.4076(4) 0.3998(3) 0.0609(13) Uani 1 1 d . . . H15 H 0.3012 0.3492 0.4317 0.073 Uiso 1 1 calc R . . C16 C 0.3216(4) 0.4241(3) 0.3277(3) 0.0462(11) Uani 1 1 d . . . C17 C 0.3549(4) 0.1931(4) 0.1665(3) 0.0563(12) Uani 1 1 d . . . H17A H 0.4010 0.2141 0.1230 0.068 Uiso 1 1 calc R . . H17B H 0.3099 0.1484 0.1602 0.068 Uiso 1 1 calc R . . C18 C 0.4446(4) 0.1355(3) 0.2289(2) 0.0429(10) Uani 1 1 d . . . C19 C 0.6087(4) 0.0242(3) 0.2955(2) 0.0451(10) Uani 1 1 d . . . C20 C 0.7200(4) -0.0501(4) 0.3246(3) 0.0563(13) Uani 1 1 d . . . H20 H 0.7776 -0.0855 0.2973 0.068 Uiso 1 1 calc R . . C21 C 0.7414(4) -0.0692(4) 0.3962(3) 0.0629(14) Uani 1 1 d . . . H21 H 0.8158 -0.1186 0.4175 0.076 Uiso 1 1 calc R . . C22 C 0.6558(4) -0.0173(4) 0.4381(3) 0.0587(13) Uani 1 1 d . . . H22 H 0.6738 -0.0329 0.4863 0.070 Uiso 1 1 calc R . . C23 C 0.5442(4) 0.0573(4) 0.4085(2) 0.0496(11) Uani 1 1 d . . . H23 H 0.4872 0.0931 0.4359 0.060 Uiso 1 1 calc R . . C24 C 0.5207(3) 0.0765(3) 0.3372(2) 0.0400(10) Uani 1 1 d . . . C25 C 0.0882(4) 0.0793(4) 0.0817(2) 0.0548(12) Uani 1 1 d . . . H25A H 0.0523 0.0729 0.0411 0.066 Uiso 1 1 calc R . . H25B H 0.1385 0.1264 0.0638 0.066 Uiso 1 1 calc R . . C26 C -0.0143(4) 0.1206(3) 0.1281(2) 0.0435(10) Uani 1 1 d . . . C27 C -0.1894(4) 0.2147(3) 0.1648(3) 0.0461(11) Uani 1 1 d . . . C28 C -0.3072(4) 0.2828(4) 0.1722(3) 0.0596(14) Uani 1 1 d . . . H28 H -0.3588 0.3266 0.1328 0.071 Uiso 1 1 calc R . . C29 C -0.3423(4) 0.2814(4) 0.2408(3) 0.0630(14) Uani 1 1 d . . . H29 H -0.4201 0.3259 0.2480 0.076 Uiso 1 1 calc R . . C30 C -0.2662(4) 0.2160(4) 0.3000(3) 0.0583(13) Uani 1 1 d . . . H30 H -0.2935 0.2185 0.3456 0.070 Uiso 1 1 calc R . . C31 C -0.1507(4) 0.1475(3) 0.2924(3) 0.0463(11) Uani 1 1 d . . . H31 H -0.1003 0.1029 0.3321 0.056 Uiso 1 1 calc R . . C32 C -0.1126(4) 0.1474(3) 0.2238(2) 0.0408(10) Uani 1 1 d . . . C33 C 0.1186(5) -0.1079(4) 0.1249(3) 0.0588(13) Uani 1 1 d . . . H33A H 0.1794 -0.1529 0.1016 0.071 Uiso 1 1 calc R . . H33B H 0.0414 -0.0775 0.0965 0.071 Uiso 1 1 calc R . . C34 C 0.0925(4) -0.1721(3) 0.1971(2) 0.0446(10) Uani 1 1 d . . . C35 C 0.0371(4) -0.2979(3) 0.2778(3) 0.0474(11) Uani 1 1 d . . . C36 C 0.0011(4) -0.3845(4) 0.3174(3) 0.0607(14) Uani 1 1 d . . . H36 H -0.0156 -0.4280 0.2955 0.073 Uiso 1 1 calc R . . C37 C -0.0087(5) -0.4033(4) 0.3903(3) 0.0638(14) Uani 1 1 d . . . H37 H -0.0328 -0.4606 0.4184 0.077 Uiso 1 1 calc R . . C38 C 0.0163(4) -0.3388(4) 0.4224(3) 0.0571(13) Uani 1 1 d . . . H38 H 0.0084 -0.3538 0.4718 0.068 Uiso 1 1 calc R . . C39 C 0.0525(4) -0.2534(3) 0.3841(3) 0.0500(11) Uani 1 1 d . . . H39 H 0.0694 -0.2109 0.4067 0.060 Uiso 1 1 calc R . . C40 C 0.0630(4) -0.2321(3) 0.3099(2) 0.0414(10) Uani 1 1 d . . . C41 C 0.3040(5) -0.0453(4) 0.1068(3) 0.0662(14) Uani 1 1 d . . . H41A H 0.3247 -0.0872 0.0747 0.079 Uiso 1 1 calc R . . H41B H 0.3224 0.0196 0.0828 0.079 Uiso 1 1 calc R . . C42 C 0.3796(4) -0.1019(4) 0.1741(3) 0.0549(12) Uani 1 1 d . . . C43 C 0.5352(4) -0.1965(4) 0.2516(4) 0.0711(17) Uani 1 1 d . . . C44 C 0.6464(5) -0.2634(5) 0.2894(5) 0.102(3) Uani 1 1 d . . . H44 H 0.7156 -0.2954 0.2661 0.123 Uiso 1 1 calc R . . C45 C 0.6498(6) -0.2798(5) 0.3601(5) 0.110(3) Uani 1 1 d . . . H45 H 0.7236 -0.3220 0.3858 0.132 Uiso 1 1 calc R . . C46 C 0.5456(5) -0.2352(4) 0.3963(4) 0.089(2) Uani 1 1 d . . . H46 H 0.5506 -0.2490 0.4455 0.107 Uiso 1 1 calc R . . C47 C 0.4343(5) -0.1702(4) 0.3594(3) 0.0700(16) Uani 1 1 d . . . H47 H 0.3645 -0.1404 0.3834 0.084 Uiso 1 1 calc R . . C48 C 0.4302(4) -0.1515(3) 0.2872(3) 0.0534(12) Uani 1 1 d . . . C49 C 0.1701(3) 0.0624(3) 0.3643(2) 0.0333(9) Uani 1 1 d . . . C50 C 0.1151(4) -0.0114(3) 0.4215(2) 0.0450(10) Uani 1 1 d . . . H50A H 0.1837 -0.0689 0.4488 0.054 Uiso 1 1 calc R . . H50B H 0.0683 -0.0399 0.3985 0.054 Uiso 1 1 calc R . . C51 C 0.0290(4) 0.0373(3) 0.4726(2) 0.0412(10) Uani 1 1 d . . . H51A H 0.0765 0.0629 0.4974 0.049 Uiso 1 1 calc R . . H51B H -0.0380 0.0965 0.4454 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.43439(14) 0.64898(14) 0.03956(9) 0.0794(4) Uani 1 1 d D . . Cl2 Cl -0.00515(15) 0.64793(10) 0.06382(8) 0.0725(4) Uani 1 1 d . . . Cl3 Cl 0.76373(14) 0.97601(12) 0.09547(9) 0.0770(4) Uani 1 1 d . . . N1 N 0.2650(3) 0.2856(3) 0.1805(2) 0.0476(9) Uani 1 1 d . . . N2 N 0.0729(3) 0.3138(3) 0.27778(19) 0.0428(8) Uani 1 1 d . . . N3 N -0.0772(4) 0.4046(3) 0.1950(2) 0.0567(11) Uani 1 1 d . . . H3 H -0.1140 0.4329 0.1537 0.068 Uiso 1 1 calc R . . N4 N 0.3022(3) 0.3654(3) 0.2872(2) 0.0439(9) Uani 1 1 d . . . N5 N 0.3445(4) 0.5029(3) 0.2125(3) 0.0653(12) Uani 1 1 d . . . H5A H 0.3573 0.5464 0.1727 0.078 Uiso 1 1 calc R . . N6 N 0.4180(3) 0.1456(3) 0.29281(18) 0.0400(8) Uani 1 1 d . . . N7 N 0.5568(3) 0.0646(3) 0.2275(2) 0.0496(9) Uani 1 1 d . . . H7A H 0.5904 0.0474 0.1905 0.060 Uiso 1 1 calc R . . N8 N 0.1675(3) -0.0238(3) 0.12546(19) 0.0474(9) Uani 1 1 d . . . N9 N -0.0033(3) 0.0896(2) 0.19831(18) 0.0391(8) Uani 1 1 d . . . N10 N -0.1239(3) 0.1945(3) 0.1057(2) 0.0518(10) Uani 1 1 d . . . H10 H -0.1492 0.2244 0.0618 0.062 Uiso 1 1 calc R . . N11 N 0.0980(3) -0.1532(3) 0.25694(19) 0.0414(8) Uani 1 1 d . . . N12 N 0.0582(4) -0.2572(3) 0.2063(2) 0.0538(10) Uani 1 1 d . . . H12A H 0.0507 -0.2820 0.1732 0.065 Uiso 1 1 calc R . . N13 N 0.3331(3) -0.0913(3) 0.2367(2) 0.0505(10) Uani 1 1 d . . . N14 N 0.4986(4) -0.1635(4) 0.1806(3) 0.0770(15) Uani 1 1 d . . . H14A H 0.5449 -0.1798 0.1464 0.092 Uiso 1 1 calc R . . O1 O 0.2025(2) 0.1267(2) 0.38421(14) 0.0391(6) Uani 1 1 d . . . O2 O 0.1813(2) 0.0598(2) 0.30147(15) 0.0401(7) Uani 1 1 d . . . O3 O 0.4977(9) 0.5398(9) 0.0806(6) 0.109(4) Uani 0.53 1 d P A 1 O4 O 0.3326(10) 0.6394(12) 0.0031(7) 0.134(4) Uani 0.53 1 d P A 1 O5 O 0.5152(13) 0.6850(12) -0.0078(8) 0.108(5) Uani 0.53 1 d P A 1 O6 O 0.3962(6) 0.6933(4) 0.0933(3) 0.1316(19) Uani 1 1 d . A . O3' O 0.4193(14) 0.5544(7) 0.0551(8) 0.125(5) Uani 0.47 1 d PD A 2 O4' O 0.3566(11) 0.7232(11) -0.0153(7) 0.185(8) Uani 0.47 1 d PD A 2 O5' O 0.5588(8) 0.6468(13) 0.0187(11) 0.127(7) Uani 0.47 1 d PD A 2 O7 O 0.0657(5) 0.5537(4) 0.0522(3) 0.1308(19) Uani 1 1 d . . . O8 O -0.1083(5) 0.6939(3) 0.0134(2) 0.1024(14) Uani 1 1 d . . . O9 O 0.0643(4) 0.7199(3) 0.0528(2) 0.0900(13) Uani 1 1 d . . . O10 O -0.0520(6) 0.6289(4) 0.1336(2) 0.1199(19) Uani 1 1 d . . . O11 O 0.6319(4) 1.0235(4) 0.0918(2) 0.1057(15) Uani 1 1 d . . . O12 O 0.7937(7) 0.8776(5) 0.0887(4) 0.170(3) Uani 1 1 d . . . O13 O 0.8114(4) 0.9722(4) 0.1622(2) 0.1033(15) Uani 1 1 d . . . O14 O 0.8207(4) 1.0346(4) 0.0379(2) 0.0990(14) Uani 1 1 d . . . O15 O 0.7875(4) 0.4849(4) 0.0689(2) 0.1094(16) Uani 1 1 d . . . H15A H 0.7106 0.4996 0.0724 0.164 Uiso 1 1 d R . . H15B H 0.8296 0.4734 0.0346 0.164 Uiso 1 1 d R . . O16 O 0.6152(9) 0.8211(9) 0.0407(7) 0.139(4) Uani 0.52 1 d P B 1 H16A H 0.5873 0.7835 0.0270 0.167 Uiso 0.52 1 d PR B 1 H16B H 0.6877 0.8117 0.0523 0.167 Uiso 0.52 1 d PR B 1 O17 O 0.6672(8) 0.7071(8) 0.1203(6) 0.107(3) Uani 0.48 1 d P C 2 H17C H 0.6353 0.6903 0.0920 0.128 Uiso 0.48 1 d PR C 2 H17D H 0.7442 0.6859 0.1246 0.128 Uiso 0.48 1 d PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0311(3) 0.0368(3) 0.0438(3) -0.0088(2) 0.0021(2) -0.0110(2) Cu2 0.0352(3) 0.0387(3) 0.0489(3) -0.0204(2) -0.0022(2) -0.0039(2) C1 0.051(3) 0.062(3) 0.052(3) -0.011(2) -0.011(2) -0.023(2) C2 0.044(2) 0.037(2) 0.065(3) -0.010(2) -0.011(2) -0.0166(19) C3 0.044(3) 0.036(2) 0.081(4) -0.015(2) -0.014(3) -0.009(2) C4 0.040(3) 0.054(3) 0.130(6) -0.034(4) -0.020(3) 0.001(2) C5 0.039(3) 0.082(4) 0.141(6) -0.067(4) 0.002(3) 0.000(3) C6 0.053(3) 0.074(4) 0.085(4) -0.040(3) 0.007(3) -0.006(3) C7 0.042(3) 0.053(3) 0.072(4) -0.026(3) -0.003(2) -0.010(2) C8 0.035(2) 0.035(2) 0.067(3) -0.014(2) -0.006(2) -0.0080(18) C9 0.067(3) 0.066(3) 0.046(3) 0.005(2) -0.008(2) -0.035(3) C10 0.036(2) 0.041(2) 0.058(3) -0.005(2) -0.006(2) -0.0144(18) C11 0.037(2) 0.040(3) 0.098(4) -0.020(3) -0.006(3) -0.007(2) C12 0.053(3) 0.045(3) 0.168(7) -0.044(4) -0.007(4) -0.016(2) C13 0.057(3) 0.080(5) 0.154(7) -0.077(5) -0.008(4) -0.011(3) C14 0.073(4) 0.087(4) 0.102(5) -0.060(4) 0.000(3) -0.022(3) C15 0.047(3) 0.065(3) 0.077(4) -0.035(3) 0.001(2) -0.013(2) C16 0.030(2) 0.039(2) 0.071(3) -0.021(2) -0.005(2) -0.0075(17) C17 0.055(3) 0.065(3) 0.044(3) -0.017(2) 0.004(2) -0.011(2) C18 0.045(2) 0.045(2) 0.039(3) -0.014(2) 0.0098(19) -0.016(2) C19 0.045(2) 0.043(2) 0.048(3) -0.017(2) 0.011(2) -0.0152(19) C20 0.041(2) 0.052(3) 0.072(4) -0.023(3) 0.009(2) -0.006(2) C21 0.040(3) 0.056(3) 0.080(4) -0.015(3) 0.000(3) -0.003(2) C22 0.046(3) 0.067(3) 0.050(3) -0.007(3) -0.002(2) -0.011(2) C23 0.041(2) 0.059(3) 0.043(3) -0.014(2) 0.006(2) -0.010(2) C24 0.031(2) 0.041(2) 0.044(3) -0.0078(19) 0.0063(18) -0.0123(17) C25 0.063(3) 0.055(3) 0.044(3) -0.018(2) 0.004(2) -0.012(2) C26 0.052(3) 0.039(2) 0.041(3) -0.015(2) -0.005(2) -0.0115(19) C27 0.040(2) 0.040(2) 0.059(3) -0.015(2) -0.008(2) -0.0103(19) C28 0.036(2) 0.050(3) 0.087(4) -0.018(3) -0.013(3) -0.006(2) C29 0.034(2) 0.056(3) 0.104(5) -0.038(3) 0.008(3) -0.009(2) C30 0.041(3) 0.064(3) 0.079(4) -0.037(3) 0.017(2) -0.019(2) C31 0.037(2) 0.051(3) 0.054(3) -0.025(2) 0.006(2) -0.0103(19) C32 0.033(2) 0.041(2) 0.053(3) -0.020(2) -0.0034(19) -0.0112(17) C33 0.077(3) 0.055(3) 0.052(3) -0.027(2) -0.001(3) -0.019(3) C34 0.045(2) 0.038(2) 0.051(3) -0.019(2) -0.001(2) -0.0080(19) C35 0.042(2) 0.040(2) 0.059(3) -0.017(2) -0.005(2) -0.0072(19) C36 0.056(3) 0.040(3) 0.088(4) -0.018(3) -0.014(3) -0.015(2) C37 0.058(3) 0.041(3) 0.085(4) -0.004(3) -0.003(3) -0.020(2) C38 0.055(3) 0.046(3) 0.062(3) -0.009(2) -0.001(2) -0.011(2) C39 0.050(3) 0.039(2) 0.058(3) -0.015(2) -0.005(2) -0.007(2) C40 0.031(2) 0.035(2) 0.056(3) -0.018(2) -0.0043(19) -0.0014(17) C41 0.060(3) 0.082(4) 0.066(4) -0.040(3) 0.022(3) -0.023(3) C42 0.042(3) 0.058(3) 0.075(4) -0.039(3) 0.016(2) -0.015(2) C43 0.039(3) 0.059(3) 0.130(6) -0.058(4) 0.000(3) -0.006(2) C44 0.033(3) 0.075(4) 0.215(9) -0.084(6) -0.017(4) 0.007(3) C45 0.060(4) 0.079(4) 0.188(9) -0.050(5) -0.059(5) 0.008(3) C46 0.066(4) 0.061(4) 0.128(6) -0.014(4) -0.038(4) -0.008(3) C47 0.048(3) 0.055(3) 0.099(5) -0.018(3) -0.017(3) -0.006(2) C48 0.034(2) 0.045(3) 0.084(4) -0.028(3) -0.006(2) -0.0053(19) C49 0.0266(18) 0.033(2) 0.039(3) -0.0089(18) -0.0023(16) -0.0079(15) C50 0.051(2) 0.042(2) 0.045(3) -0.015(2) 0.010(2) -0.019(2) C51 0.046(2) 0.041(2) 0.039(3) -0.0124(19) 0.0074(19) -0.0187(19) Cl1 0.0683(9) 0.0922(11) 0.0670(10) -0.0204(9) -0.0047(8) -0.0128(8) Cl2 0.1030(11) 0.0509(7) 0.0628(9) -0.0187(6) -0.0087(8) -0.0188(7) Cl3 0.0796(10) 0.0857(10) 0.0766(11) -0.0489(9) 0.0271(8) -0.0231(8) N1 0.048(2) 0.047(2) 0.047(2) -0.0099(18) -0.0034(17) -0.0169(17) N2 0.0385(19) 0.0415(19) 0.050(2) -0.0148(17) -0.0028(16) -0.0135(15) N3 0.048(2) 0.048(2) 0.071(3) -0.008(2) -0.021(2) -0.0153(18) N4 0.0366(18) 0.0372(19) 0.056(3) -0.0119(18) -0.0016(16) -0.0112(15) N5 0.061(3) 0.042(2) 0.083(3) 0.003(2) -0.008(2) -0.0223(19) N6 0.0370(18) 0.0426(19) 0.038(2) -0.0089(16) 0.0055(15) -0.0133(15) N7 0.051(2) 0.052(2) 0.049(2) -0.0221(19) 0.0136(18) -0.0159(18) N8 0.054(2) 0.045(2) 0.043(2) -0.0196(17) 0.0065(17) -0.0108(17) N9 0.0400(18) 0.0408(19) 0.038(2) -0.0181(16) -0.0004(15) -0.0074(15) N10 0.055(2) 0.046(2) 0.048(2) -0.0123(18) -0.0157(19) -0.0038(18) N11 0.0436(19) 0.0354(18) 0.043(2) -0.0121(16) -0.0026(16) -0.0089(15) N12 0.060(2) 0.046(2) 0.062(3) -0.025(2) -0.008(2) -0.0152(19) N13 0.0350(19) 0.044(2) 0.071(3) -0.024(2) 0.0010(18) -0.0037(16) N14 0.038(2) 0.088(3) 0.130(5) -0.077(3) 0.019(3) -0.013(2) O1 0.0413(15) 0.0425(16) 0.0368(16) -0.0121(13) 0.0044(12) -0.0186(13) O2 0.0430(15) 0.0473(17) 0.0348(17) -0.0172(13) 0.0039(12) -0.0168(13) O3 0.072(6) 0.113(8) 0.092(8) 0.016(6) -0.002(5) -0.008(5) O4 0.099(8) 0.163(12) 0.147(11) -0.060(10) -0.029(7) -0.028(8) O5 0.136(11) 0.091(9) 0.088(9) -0.002(6) 0.041(9) -0.059(9) O6 0.145(5) 0.133(5) 0.128(5) -0.072(4) 0.022(4) -0.031(4) O3' 0.165(15) 0.093(10) 0.129(13) -0.040(9) 0.039(11) -0.060(11) O4' 0.154(13) 0.210(17) 0.136(11) 0.078(11) -0.098(10) -0.091(12) O5' 0.096(10) 0.117(15) 0.15(2) -0.040(12) 0.012(9) -0.018(8) O7 0.143(4) 0.078(3) 0.163(5) -0.063(3) -0.008(4) 0.007(3) O8 0.128(4) 0.082(3) 0.093(3) -0.013(2) -0.039(3) -0.030(3) O9 0.118(3) 0.092(3) 0.078(3) -0.028(2) 0.002(2) -0.056(3) O10 0.220(6) 0.102(4) 0.064(3) -0.021(3) 0.013(3) -0.092(4) O11 0.088(3) 0.150(4) 0.089(3) -0.048(3) 0.013(3) -0.042(3) O12 0.212(7) 0.122(5) 0.224(7) -0.117(5) 0.075(6) -0.072(5) O13 0.108(3) 0.138(4) 0.062(3) -0.044(3) 0.013(2) -0.024(3) O14 0.109(3) 0.148(4) 0.055(3) -0.037(3) 0.029(2) -0.062(3) O15 0.087(3) 0.141(4) 0.091(3) -0.008(3) -0.026(2) -0.043(3) O16 0.119(8) 0.176(11) 0.182(11) -0.112(10) 0.047(8) -0.080(8) O17 0.075(6) 0.131(9) 0.142(9) -0.091(8) 0.023(6) -0.027(6) _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 N6 1.953(3) . ? Cu1 N2 1.963(3) . ? Cu1 O1 1.975(3) . ? Cu1 N4 2.043(3) . ? Cu1 N1 2.327(4) . ? Cu2 N13 1.950(3) . ? Cu2 N9 1.957(3) . ? Cu2 O2 2.001(3) . ? Cu2 N11 2.128(3) . ? Cu2 N8 2.255(4) . ? C1 N1 1.477(5) . ? C1 C2 1.505(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.327(6) . ? C2 N3 1.348(5) . ? C3 N3 1.382(7) . ? C3 C4 1.385(7) . ? C3 C8 1.410(6) . ? C4 C5 1.351(9) . ? C4 H4 0.9300 . ? C5 C6 1.391(8) . ? C5 H5 0.9300 . ? C6 C7 1.390(7) . ? C6 H6 0.9300 . ? C7 C8 1.366(7) . ? C7 H7 0.9300 . ? C8 N2 1.387(6) . ? C9 N1 1.469(6) . ? C9 C10 1.491(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.303(5) . ? C10 N5 1.354(6) . ? C11 C12 1.386(7) . ? C11 N5 1.387(7) . ? C11 C16 1.388(6) . ? C12 C13 1.376(9) . ? C12 H12 0.9300 . ? C13 C14 1.369(9) . ? C13 H13 0.9300 . ? C14 C15 1.381(7) . ? C14 H14 0.9300 . ? C15 C16 1.363(7) . ? C15 H15 0.9300 . ? C16 N4 1.401(5) . ? C17 N1 1.473(6) . ? C17 C18 1.497(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.312(5) . ? C18 N7 1.343(5) . ? C19 N7 1.378(6) . ? C19 C20 1.379(6) . ? C19 C24 1.410(6) . ? C20 C21 1.377(7) . ? C20 H20 0.9300 . ? C21 C22 1.396(7) . ? C21 H21 0.9300 . ? C22 C23 1.385(6) . ? C22 H22 0.9300 . ? C23 C24 1.376(6) . ? C23 H23 0.9300 . ? C24 N6 1.401(5) . ? C25 N8 1.478(5) . ? C25 C26 1.492(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N9 1.314(5) . ? C26 N10 1.337(5) . ? C27 N10 1.381(6) . ? C27 C28 1.394(6) . ? C27 C32 1.396(6) . ? C28 C29 1.369(7) . ? C28 H28 0.9300 . ? C29 C30 1.391(7) . ? C29 H29 0.9300 . ? C30 C31 1.380(6) . ? C30 H30 0.9300 . ? C31 C32 1.382(6) . ? C31 H31 0.9300 . ? C32 N9 1.393(5) . ? C33 N8 1.469(6) . ? C33 C34 1.483(7) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N11 1.304(5) . ? C34 N12 1.337(5) . ? C35 N12 1.369(6) . ? C35 C36 1.388(6) . ? C35 C40 1.397(6) . ? C36 C37 1.376(7) . ? C36 H36 0.9300 . ? C37 C38 1.376(7) . ? C37 H37 0.9300 . ? C38 C39 1.369(6) . ? C38 H38 0.9300 . ? C39 C40 1.396(6) . ? C39 H39 0.9300 . ? C40 N11 1.396(5) . ? C41 C42 1.486(7) . ? C41 N8 1.494(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N13 1.330(6) . ? C42 N14 1.333(6) . ? C43 N14 1.379(7) . ? C43 C48 1.395(7) . ? C43 C44 1.404(8) . ? C44 C45 1.339(10) . ? C44 H44 0.9300 . ? C45 C46 1.393(10) . ? C45 H45 0.9300 . ? C46 C47 1.391(7) . ? C46 H46 0.9300 . ? C47 C48 1.365(8) . ? C47 H47 0.9300 . ? C48 N13 1.400(6) . ? C49 O2 1.246(5) . ? C49 O1 1.262(4) . ? C49 C50 1.506(5) . ? C50 C51 1.510(6) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C51 1.509(8) 2_556 ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? Cl1 O5 1.335(11) . ? Cl1 O3' 1.344(7) . ? Cl1 O6 1.373(5) . ? Cl1 O4' 1.376(7) . ? Cl1 O5' 1.407(8) . ? Cl1 O4 1.464(10) . ? Cl1 O3 1.472(10) . ? Cl2 O10 1.398(5) . ? Cl2 O7 1.405(4) . ? Cl2 O9 1.426(4) . ? Cl2 O8 1.434(4) . ? Cl3 O12 1.382(5) . ? Cl3 O14 1.408(4) . ? Cl3 O11 1.411(5) . ? Cl3 O13 1.444(4) . ? N3 H3 0.8600 . ? N5 H5A 0.8600 . ? N7 H7A 0.8600 . ? N10 H10 0.8600 . ? N12 H12A 0.8600 . ? N14 H14A 0.8600 . ? O15 H15A 0.8200 . ? O15 H15B 0.8199 . ? O16 H16A 0.8200 . ? O16 H16B 0.8199 . ? O17 H17C 0.8200 . ? O17 H17D 0.8200 . ? 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 N6 Cu1 N2 155.11(15) . . ? N6 Cu1 O1 95.34(12) . . ? N2 Cu1 O1 92.55(13) . . ? N6 Cu1 N4 95.36(14) . . ? N2 Cu1 N4 93.56(13) . . ? O1 Cu1 N4 140.17(14) . . ? N6 Cu1 N1 78.96(13) . . ? N2 Cu1 N1 79.83(14) . . ? O1 Cu1 N1 139.96(12) . . ? N4 Cu1 N1 79.80(14) . . ? N13 Cu2 N9 153.99(16) . . ? N13 Cu2 O2 93.03(14) . . ? N9 Cu2 O2 92.95(12) . . ? N13 Cu2 N11 93.96(14) . . ? N9 Cu2 N11 99.69(13) . . ? O2 Cu2 N11 134.66(13) . . ? N13 Cu2 N8 80.37(15) . . ? N9 Cu2 N8 79.95(13) . . ? O2 Cu2 N8 143.95(13) . . ? N11 Cu2 N8 81.34(14) . . ? N1 C1 C2 108.7(4) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N2 C2 N3 111.9(4) . . ? N2 C2 C1 122.3(4) . . ? N3 C2 C1 125.7(4) . . ? N3 C3 C4 133.3(5) . . ? N3 C3 C8 106.1(4) . . ? C4 C3 C8 120.5(6) . . ? C5 C4 C3 117.6(5) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? C4 C5 C6 122.2(5) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C7 C6 C5 121.1(6) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C8 C7 C6 117.0(5) . . ? C8 C7 H7 121.5 . . ? C6 C7 H7 121.5 . . ? C7 C8 N2 130.7(4) . . ? C7 C8 C3 121.5(4) . . ? N2 C8 C3 107.7(5) . . ? N1 C9 C10 111.4(4) . . ? N1 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N1 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? N4 C10 N5 111.4(4) . . ? N4 C10 C9 125.6(4) . . ? N5 C10 C9 123.0(4) . . ? C12 C11 N5 132.7(6) . . ? C12 C11 C16 121.4(6) . . ? N5 C11 C16 105.9(4) . . ? C13 C12 C11 117.1(6) . . ? C13 C12 H12 121.5 . . ? C11 C12 H12 121.5 . . ? C14 C13 C12 120.9(6) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 122.5(6) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? C16 C15 C14 117.0(6) . . ? C16 C15 H15 121.5 . . ? C14 C15 H15 121.5 . . ? C15 C16 C11 121.2(5) . . ? C15 C16 N4 131.1(4) . . ? C11 C16 N4 107.7(5) . . ? N1 C17 C18 108.7(4) . . ? N1 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? N1 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? N6 C18 N7 112.3(4) . . ? N6 C18 C17 122.7(4) . . ? N7 C18 C17 124.9(4) . . ? N7 C19 C20 133.1(4) . . ? N7 C19 C24 105.3(4) . . ? C20 C19 C24 121.6(4) . . ? C21 C20 C19 116.6(4) . . ? C21 C20 H20 121.7 . . ? C19 C20 H20 121.7 . . ? C20 C21 C22 122.5(4) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C23 C22 C21 120.7(5) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 117.5(4) . . ? C24 C23 H23 121.2 . . ? C22 C23 H23 121.2 . . ? C23 C24 N6 131.0(4) . . ? C23 C24 C19 121.1(4) . . ? N6 C24 C19 107.9(4) . . ? N8 C25 C26 108.0(4) . . ? N8 C25 H25A 110.1 . . ? C26 C25 H25A 110.1 . . ? N8 C25 H25B 110.1 . . ? C26 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? N9 C26 N10 111.4(4) . . ? N9 C26 C25 122.3(4) . . ? N10 C26 C25 126.3(4) . . ? N10 C27 C28 132.4(4) . . ? N10 C27 C32 105.4(4) . . ? C28 C27 C32 122.2(5) . . ? C29 C28 C27 116.0(5) . . ? C29 C28 H28 122.0 . . ? C27 C28 H28 122.0 . . ? C28 C29 C30 122.5(4) . . ? C28 C29 H29 118.7 . . ? C30 C29 H29 118.7 . . ? C31 C30 C29 121.1(5) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C30 C31 C32 117.6(4) . . ? C30 C31 H31 121.2 . . ? C32 C31 H31 121.2 . . ? C31 C32 N9 131.7(4) . . ? C31 C32 C27 120.4(4) . . ? N9 C32 C27 107.9(4) . . ? N8 C33 C34 114.1(4) . . ? N8 C33 H33A 108.7 . . ? C34 C33 H33A 108.7 . . ? N8 C33 H33B 108.7 . . ? C34 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? N11 C34 N12 112.9(4) . . ? N11 C34 C33 125.6(4) . . ? N12 C34 C33 121.5(4) . . ? N12 C35 C36 133.0(5) . . ? N12 C35 C40 104.8(4) . . ? C36 C35 C40 122.2(5) . . ? C37 C36 C35 117.1(5) . . ? C37 C36 H36 121.5 . . ? C35 C36 H36 121.5 . . ? C36 C37 C38 121.2(5) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C39 C38 C37 122.3(5) . . ? C39 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? C38 C39 C40 117.8(5) . . ? C38 C39 H39 121.1 . . ? C40 C39 H39 121.1 . . ? N11 C40 C39 131.6(4) . . ? N11 C40 C35 109.0(4) . . ? C39 C40 C35 119.4(4) . . ? C42 C41 N8 108.4(4) . . ? C42 C41 H41A 110.0 . . ? N8 C41 H41A 110.0 . . ? C42 C41 H41B 110.0 . . ? N8 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? N13 C42 N14 111.7(5) . . ? N13 C42 C41 121.2(4) . . ? N14 C42 C41 127.0(5) . . ? N14 C43 C48 105.6(4) . . ? N14 C43 C44 133.5(6) . . ? C48 C43 C44 120.8(7) . . ? C45 C44 C43 117.9(6) . . ? C45 C44 H44 121.0 . . ? C43 C44 H44 121.0 . . ? C44 C45 C46 121.8(6) . . ? C44 C45 H45 119.1 . . ? C46 C45 H45 119.1 . . ? C47 C46 C45 120.7(7) . . ? C47 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C48 C47 C46 118.2(6) . . ? C48 C47 H47 120.9 . . ? C46 C47 H47 120.9 . . ? C47 C48 C43 120.6(5) . . ? C47 C48 N13 131.2(4) . . ? C43 C48 N13 108.3(5) . . ? O2 C49 O1 122.8(4) . . ? O2 C49 C50 121.4(4) . . ? O1 C49 C50 115.8(4) . . ? C49 C50 C51 114.4(3) . . ? C49 C50 H50A 108.7 . . ? C51 C50 H50A 108.7 . . ? C49 C50 H50B 108.7 . . ? C51 C50 H50B 108.7 . . ? H50A C50 H50B 107.6 . . ? C51 C51 C50 113.2(4) 2_556 . ? C51 C51 H51A 108.9 2_556 . ? C50 C51 H51A 108.9 . . ? C51 C51 H51B 108.9 2_556 . ? C50 C51 H51B 108.9 . . ? H51A C51 H51B 107.8 . . ? O5 Cl1 O3' 125.6(11) . . ? O5 Cl1 O6 117.0(9) . . ? O3' Cl1 O6 113.5(7) . . ? O5 Cl1 O4' 77.0(8) . . ? O3' Cl1 O4' 113.1(7) . . ? O6 Cl1 O4' 99.9(9) . . ? O3' Cl1 O5' 111.4(8) . . ? O6 Cl1 O5' 111.6(11) . . ? O4' Cl1 O5' 106.8(7) . . ? O5 Cl1 O4 110.7(9) . . ? O6 Cl1 O4 115.0(6) . . ? O5' Cl1 O4 131.2(11) . . ? O5 Cl1 O3 108.8(8) . . ? O6 Cl1 O3 101.6(6) . . ? O4' Cl1 O3 151.7(9) . . ? O4 Cl1 O3 102.1(8) . . ? O10 Cl2 O7 110.3(3) . . ? O10 Cl2 O9 108.6(3) . . ? O7 Cl2 O9 113.5(3) . . ? O10 Cl2 O8 109.5(3) . . ? O7 Cl2 O8 106.5(3) . . ? O9 Cl2 O8 108.4(3) . . ? O12 Cl3 O14 106.8(4) . . ? O12 Cl3 O11 110.7(4) . . ? O14 Cl3 O11 109.5(3) . . ? O12 Cl3 O13 111.3(4) . . ? O14 Cl3 O13 109.3(3) . . ? O11 Cl3 O13 109.2(3) . . ? C9 N1 C17 113.1(4) . . ? C9 N1 C1 113.3(4) . . ? C17 N1 C1 113.6(4) . . ? C9 N1 Cu1 107.6(3) . . ? C17 N1 Cu1 103.5(3) . . ? C1 N1 Cu1 104.6(3) . . ? C2 N2 C8 106.8(4) . . ? C2 N2 Cu1 116.5(3) . . ? C8 N2 Cu1 136.6(3) . . ? C2 N3 C3 107.5(4) . . ? C2 N3 H3 126.3 . . ? C3 N3 H3 126.3 . . ? C10 N4 C16 107.3(4) . . ? C10 N4 Cu1 114.9(3) . . ? C16 N4 Cu1 137.6(3) . . ? C10 N5 C11 107.7(4) . . ? C10 N5 H5A 126.2 . . ? C11 N5 H5A 126.2 . . ? C18 N6 C24 106.3(3) . . ? C18 N6 Cu1 116.4(3) . . ? C24 N6 Cu1 136.9(3) . . ? C18 N7 C19 108.2(4) . . ? C18 N7 H7A 125.9 . . ? C19 N7 H7A 125.9 . . ? C33 N8 C25 111.9(4) . . ? C33 N8 C41 112.2(4) . . ? C25 N8 C41 113.2(4) . . ? C33 N8 Cu2 107.3(3) . . ? C25 N8 Cu2 105.5(3) . . ? C41 N8 Cu2 106.2(3) . . ? C26 N9 C32 106.9(3) . . ? C26 N9 Cu2 115.9(3) . . ? C32 N9 Cu2 137.2(3) . . ? C26 N10 C27 108.4(4) . . ? C26 N10 H10 125.8 . . ? C27 N10 H10 125.8 . . ? C34 N11 C40 105.2(4) . . ? C34 N11 Cu2 111.1(3) . . ? C40 N11 Cu2 143.7(3) . . ? C34 N12 C35 108.1(4) . . ? C34 N12 H12A 125.9 . . ? C35 N12 H12A 125.9 . . ? C42 N13 C48 105.9(4) . . ? C42 N13 Cu2 117.0(3) . . ? C48 N13 Cu2 136.5(3) . . ? C42 N14 C43 108.5(4) . . ? C42 N14 H14A 125.7 . . ? C43 N14 H14A 125.7 . . ? C49 O1 Cu1 114.0(3) . . ? C49 O2 Cu2 142.3(3) . . ? H15A O15 H15B 126.7 . . ? H16A O16 H16B 128.9 . . ? H17C O17 H17D 117.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -27.3(6) . . . . ? N1 C1 C2 N3 156.3(4) . . . . ? N3 C3 C4 C5 178.2(5) . . . . ? C8 C3 C4 C5 -1.3(8) . . . . ? C3 C4 C5 C6 -0.9(9) . . . . ? C4 C5 C6 C7 2.0(9) . . . . ? C5 C6 C7 C8 -0.9(8) . . . . ? C6 C7 C8 N2 -178.7(4) . . . . ? C6 C7 C8 C3 -1.3(7) . . . . ? N3 C3 C8 C7 -177.1(4) . . . . ? C4 C3 C8 C7 2.5(7) . . . . ? N3 C3 C8 N2 0.8(5) . . . . ? C4 C3 C8 N2 -179.6(4) . . . . ? N1 C9 C10 N4 10.2(6) . . . . ? N1 C9 C10 N5 -173.1(4) . . . . ? N5 C11 C12 C13 -180.0(5) . . . . ? C16 C11 C12 C13 -0.3(7) . . . . ? C11 C12 C13 C14 0.4(8) . . . . ? C12 C13 C14 C15 0.0(9) . . . . ? C13 C14 C15 C16 -0.4(8) . . . . ? C14 C15 C16 C11 0.4(7) . . . . ? C14 C15 C16 N4 -180.0(4) . . . . ? C12 C11 C16 C15 -0.1(7) . . . . ? N5 C11 C16 C15 179.6(4) . . . . ? C12 C11 C16 N4 -179.7(4) . . . . ? N5 C11 C16 N4 0.0(4) . . . . ? N1 C17 C18 N6 21.8(6) . . . . ? N1 C17 C18 N7 -161.7(4) . . . . ? N7 C19 C20 C21 178.7(5) . . . . ? C24 C19 C20 C21 -1.0(7) . . . . ? C19 C20 C21 C22 0.3(8) . . . . ? C20 C21 C22 C23 -0.4(8) . . . . ? C21 C22 C23 C24 1.1(7) . . . . ? C22 C23 C24 N6 179.7(4) . . . . ? C22 C23 C24 C19 -1.7(7) . . . . ? N7 C19 C24 C23 -178.0(4) . . . . ? C20 C19 C24 C23 1.7(7) . . . . ? N7 C19 C24 N6 0.8(4) . . . . ? C20 C19 C24 N6 -179.4(4) . . . . ? N8 C25 C26 N9 23.7(6) . . . . ? N8 C25 C26 N10 -159.4(4) . . . . ? N10 C27 C28 C29 179.8(4) . . . . ? C32 C27 C28 C29 1.2(7) . . . . ? C27 C28 C29 C30 -0.2(7) . . . . ? C28 C29 C30 C31 -0.9(7) . . . . ? C29 C30 C31 C32 1.0(7) . . . . ? C30 C31 C32 N9 179.3(4) . . . . ? C30 C31 C32 C27 -0.1(6) . . . . ? N10 C27 C32 C31 180.0(4) . . . . ? C28 C27 C32 C31 -1.1(6) . . . . ? N10 C27 C32 N9 0.4(4) . . . . ? C28 C27 C32 N9 179.4(4) . . . . ? N8 C33 C34 N11 6.9(7) . . . . ? N8 C33 C34 N12 -174.0(4) . . . . ? N12 C35 C36 C37 178.7(4) . . . . ? C40 C35 C36 C37 0.3(7) . . . . ? C35 C36 C37 C38 -0.1(7) . . . . ? C36 C37 C38 C39 -0.2(7) . . . . ? C37 C38 C39 C40 0.3(7) . . . . ? C38 C39 C40 N11 -179.4(4) . . . . ? C38 C39 C40 C35 -0.2(6) . . . . ? N12 C35 C40 N11 0.5(4) . . . . ? C36 C35 C40 N11 179.2(4) . . . . ? N12 C35 C40 C39 -178.9(4) . . . . ? C36 C35 C40 C39 -0.2(6) . . . . ? N8 C41 C42 N13 -26.4(6) . . . . ? N8 C41 C42 N14 156.7(5) . . . . ? N14 C43 C44 C45 -179.2(6) . . . . ? C48 C43 C44 C45 -2.2(9) . . . . ? C43 C44 C45 C46 2.1(11) . . . . ? C44 C45 C46 C47 -1.0(10) . . . . ? C45 C46 C47 C48 -0.1(8) . . . . ? C46 C47 C48 C43 0.0(8) . . . . ? C46 C47 C48 N13 179.5(5) . . . . ? N14 C43 C48 C47 178.9(5) . . . . ? C44 C43 C48 C47 1.1(8) . . . . ? N14 C43 C48 N13 -0.7(5) . . . . ? C44 C43 C48 N13 -178.5(5) . . . . ? O2 C49 C50 C51 -140.2(4) . . . . ? O1 C49 C50 C51 39.2(5) . . . . ? C49 C50 C51 C51 177.6(4) . . . 2_556 ? C10 C9 N1 C17 -121.3(4) . . . . ? C10 C9 N1 C1 107.5(4) . . . . ? C10 C9 N1 Cu1 -7.6(4) . . . . ? C18 C17 N1 C9 86.1(4) . . . . ? C18 C17 N1 C1 -142.9(4) . . . . ? C18 C17 N1 Cu1 -30.0(4) . . . . ? C2 C1 N1 C9 -88.4(5) . . . . ? C2 C1 N1 C17 140.7(4) . . . . ? C2 C1 N1 Cu1 28.4(4) . . . . ? N6 Cu1 N1 C9 -93.6(3) . . . . ? N2 Cu1 N1 C9 99.5(3) . . . . ? O1 Cu1 N1 C9 -178.7(3) . . . . ? N4 Cu1 N1 C9 4.0(3) . . . . ? N6 Cu1 N1 C17 26.4(3) . . . . ? N2 Cu1 N1 C17 -140.5(3) . . . . ? O1 Cu1 N1 C17 -58.7(3) . . . . ? N4 Cu1 N1 C17 124.0(3) . . . . ? N6 Cu1 N1 C1 145.7(3) . . . . ? N2 Cu1 N1 C1 -21.2(3) . . . . ? O1 Cu1 N1 C1 60.6(3) . . . . ? N4 Cu1 N1 C1 -116.7(3) . . . . ? N3 C2 N2 C8 1.4(5) . . . . ? C1 C2 N2 C8 -175.4(4) . . . . ? N3 C2 N2 Cu1 -175.4(3) . . . . ? C1 C2 N2 Cu1 7.8(5) . . . . ? C7 C8 N2 C2 176.3(5) . . . . ? C3 C8 N2 C2 -1.4(4) . . . . ? C7 C8 N2 Cu1 -7.8(7) . . . . ? C3 C8 N2 Cu1 174.5(3) . . . . ? N6 Cu1 N2 C2 -23.9(5) . . . . ? O1 Cu1 N2 C2 -132.4(3) . . . . ? N4 Cu1 N2 C2 87.0(3) . . . . ? N1 Cu1 N2 C2 8.0(3) . . . . ? N6 Cu1 N2 C8 160.6(4) . . . . ? O1 Cu1 N2 C8 52.1(4) . . . . ? N4 Cu1 N2 C8 -88.5(4) . . . . ? N1 Cu1 N2 C8 -167.5(4) . . . . ? N2 C2 N3 C3 -0.9(5) . . . . ? C1 C2 N3 C3 175.8(4) . . . . ? C4 C3 N3 C2 -179.5(5) . . . . ? C8 C3 N3 C2 0.0(5) . . . . ? N5 C10 N4 C16 -0.5(5) . . . . ? C9 C10 N4 C16 176.6(4) . . . . ? N5 C10 N4 Cu1 176.4(3) . . . . ? C9 C10 N4 Cu1 -6.6(5) . . . . ? C15 C16 N4 C10 -179.3(4) . . . . ? C11 C16 N4 C10 0.3(4) . . . . ? C15 C16 N4 Cu1 4.9(7) . . . . ? C11 C16 N4 Cu1 -175.5(3) . . . . ? N6 Cu1 N4 C10 78.7(3) . . . . ? N2 Cu1 N4 C10 -78.0(3) . . . . ? O1 Cu1 N4 C10 -176.3(2) . . . . ? N1 Cu1 N4 C10 0.9(3) . . . . ? N6 Cu1 N4 C16 -105.8(4) . . . . ? N2 Cu1 N4 C16 97.5(4) . . . . ? O1 Cu1 N4 C16 -0.8(5) . . . . ? N1 Cu1 N4 C16 176.5(4) . . . . ? N4 C10 N5 C11 0.4(5) . . . . ? C9 C10 N5 C11 -176.7(4) . . . . ? C12 C11 N5 C10 179.4(5) . . . . ? C16 C11 N5 C10 -0.2(5) . . . . ? N7 C18 N6 C24 0.3(5) . . . . ? C17 C18 N6 C24 177.1(4) . . . . ? N7 C18 N6 Cu1 -173.4(3) . . . . ? C17 C18 N6 Cu1 3.4(5) . . . . ? C23 C24 N6 C18 178.0(5) . . . . ? C19 C24 N6 C18 -0.7(4) . . . . ? C23 C24 N6 Cu1 -10.2(7) . . . . ? C19 C24 N6 Cu1 171.1(3) . . . . ? N2 Cu1 N6 C18 15.3(5) . . . . ? O1 Cu1 N6 C18 123.2(3) . . . . ? N4 Cu1 N6 C18 -95.3(3) . . . . ? N1 Cu1 N6 C18 -16.8(3) . . . . ? N2 Cu1 N6 C24 -155.9(4) . . . . ? O1 Cu1 N6 C24 -48.0(4) . . . . ? N4 Cu1 N6 C24 93.6(4) . . . . ? N1 Cu1 N6 C24 172.1(4) . . . . ? N6 C18 N7 C19 0.2(5) . . . . ? C17 C18 N7 C19 -176.5(4) . . . . ? C20 C19 N7 C18 179.6(5) . . . . ? C24 C19 N7 C18 -0.7(5) . . . . ? C34 C33 N8 C25 -123.2(4) . . . . ? C34 C33 N8 C41 108.2(5) . . . . ? C34 C33 N8 Cu2 -8.0(5) . . . . ? C26 C25 N8 C33 87.2(4) . . . . ? C26 C25 N8 C41 -144.8(4) . . . . ? C26 C25 N8 Cu2 -29.1(4) . . . . ? C42 C41 N8 C33 -90.4(5) . . . . ? C42 C41 N8 C25 141.8(4) . . . . ? C42 C41 N8 Cu2 26.5(4) . . . . ? N13 Cu2 N8 C33 101.6(3) . . . . ? N9 Cu2 N8 C33 -95.5(3) . . . . ? O2 Cu2 N8 C33 -176.6(3) . . . . ? N11 Cu2 N8 C33 6.0(3) . . . . ? N13 Cu2 N8 C25 -139.0(3) . . . . ? N9 Cu2 N8 C25 23.9(3) . . . . ? O2 Cu2 N8 C25 -57.2(4) . . . . ? N11 Cu2 N8 C25 125.4(3) . . . . ? N13 Cu2 N8 C41 -18.6(3) . . . . ? N9 Cu2 N8 C41 144.3(3) . . . . ? O2 Cu2 N8 C41 63.2(4) . . . . ? N11 Cu2 N8 C41 -114.2(3) . . . . ? N10 C26 N9 C32 -0.3(5) . . . . ? C25 C26 N9 C32 177.1(4) . . . . ? N10 C26 N9 Cu2 -179.3(3) . . . . ? C25 C26 N9 Cu2 -1.9(5) . . . . ? C31 C32 N9 C26 -179.6(4) . . . . ? C27 C32 N9 C26 -0.1(4) . . . . ? C31 C32 N9 Cu2 -0.9(7) . . . . ? C27 C32 N9 Cu2 178.6(3) . . . . ? N13 Cu2 N9 C26 28.7(5) . . . . ? O2 Cu2 N9 C26 131.8(3) . . . . ? N11 Cu2 N9 C26 -91.9(3) . . . . ? N8 Cu2 N9 C26 -12.6(3) . . . . ? N13 Cu2 N9 C32 -149.9(4) . . . . ? O2 Cu2 N9 C32 -46.8(4) . . . . ? N11 Cu2 N9 C32 89.5(4) . . . . ? N8 Cu2 N9 C32 168.8(4) . . . . ? N9 C26 N10 C27 0.6(5) . . . . ? C25 C26 N10 C27 -176.6(4) . . . . ? C28 C27 N10 C26 -179.4(5) . . . . ? C32 C27 N10 C26 -0.6(5) . . . . ? N12 C34 N11 C40 -0.7(5) . . . . ? C33 C34 N11 C40 178.5(4) . . . . ? N12 C34 N11 Cu2 179.7(3) . . . . ? C33 C34 N11 Cu2 -1.1(5) . . . . ? C39 C40 N11 C34 179.4(4) . . . . ? C35 C40 N11 C34 0.1(4) . . . . ? C39 C40 N11 Cu2 -1.2(7) . . . . ? C35 C40 N11 Cu2 179.5(3) . . . . ? N13 Cu2 N11 C34 -82.5(3) . . . . ? N9 Cu2 N11 C34 75.3(3) . . . . ? O2 Cu2 N11 C34 179.3(2) . . . . ? N8 Cu2 N11 C34 -2.9(3) . . . . ? N13 Cu2 N11 C40 98.1(4) . . . . ? N9 Cu2 N11 C40 -104.1(4) . . . . ? O2 Cu2 N11 C40 -0.1(5) . . . . ? N8 Cu2 N11 C40 177.7(4) . . . . ? N11 C34 N12 C35 1.0(5) . . . . ? C33 C34 N12 C35 -178.2(4) . . . . ? C36 C35 N12 C34 -179.4(5) . . . . ? C40 C35 N12 C34 -0.9(4) . . . . ? N14 C42 N13 C48 -0.4(5) . . . . ? C41 C42 N13 C48 -177.7(4) . . . . ? N14 C42 N13 Cu2 -172.7(3) . . . . ? C41 C42 N13 Cu2 10.0(6) . . . . ? C47 C48 N13 C42 -178.9(5) . . . . ? C43 C48 N13 C42 0.6(5) . . . . ? C47 C48 N13 Cu2 -8.8(8) . . . . ? C43 C48 N13 Cu2 170.7(3) . . . . ? N9 Cu2 N13 C42 -35.7(5) . . . . ? O2 Cu2 N13 C42 -138.7(3) . . . . ? N11 Cu2 N13 C42 86.1(3) . . . . ? N8 Cu2 N13 C42 5.6(3) . . . . ? N9 Cu2 N13 C48 155.1(4) . . . . ? O2 Cu2 N13 C48 52.0(4) . . . . ? N11 Cu2 N13 C48 -83.2(4) . . . . ? N8 Cu2 N13 C48 -163.7(5) . . . . ? N13 C42 N14 C43 0.0(6) . . . . ? C41 C42 N14 C43 177.1(5) . . . . ? C48 C43 N14 C42 0.4(6) . . . . ? C44 C43 N14 C42 177.8(6) . . . . ? O2 C49 O1 Cu1 8.2(4) . . . . ? C50 C49 O1 Cu1 -171.3(2) . . . . ? N6 Cu1 O1 C49 -78.8(3) . . . . ? N2 Cu1 O1 C49 77.6(3) . . . . ? N4 Cu1 O1 C49 176.2(2) . . . . ? N1 Cu1 O1 C49 0.4(3) . . . . ? O1 C49 O2 Cu2 178.5(3) . . . . ? C50 C49 O2 Cu2 -2.1(6) . . . . ? N13 Cu2 O2 C49 -104.4(4) . . . . ? N9 Cu2 O2 C49 100.9(4) . . . . ? N11 Cu2 O2 C49 -5.8(5) . . . . ? N8 Cu2 O2 C49 177.8(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C28 H28 O4 0.93 2.57 3.279(15) 133 2_565 C25 H25B O8 0.97 2.45 3.235(7) 138 2_565 C25 H25A O14 0.97 2.56 3.199(6) 123 2_665 C20 H20 O13 0.93 2.55 3.217(7) 129 1_545 C17 H17A O5 0.97 2.54 3.487(13) 165 2_665 C9 H9A O7 0.97 2.47 3.401(7) 162 . C1 H1B O7 0.97 2.46 3.287(7) 143 . O16 H16B O12 0.82 2.03 2.719(12) 142 . O16 H16A O5 0.82 2.13 2.95(2) 180 . O17 H17C O5' 0.82 2.09 2.91(3) 178 . O17 H17D O10 0.82 2.17 2.986(11) 179 1_655 O16 H16B O8 0.82 2.59 3.148(11) 127 1_655 O15 H15B O7 0.82 2.05 2.874(8) 179 2_665 O15 H15A O3 0.82 2.27 3.089(11) 179 . N14 H14A O16 0.86 2.16 2.986(12) 162 1_545 N12 H12A O10 0.86 2.30 3.052(6) 147 1_545 N12 H12A O9 0.86 2.36 3.140(6) 152 1_545 N10 H10 O9 0.86 2.36 3.059(6) 139 2_565 N10 H10 O4 0.86 2.44 3.127(13) 137 2_565 N7 H7A O13 0.86 2.45 3.090(6) 131 1_545 N7 H7A O11 0.86 2.07 2.915(6) 167 1_545 N5 H5A O6 0.86 2.31 3.135(7) 160 . N5 H5A O3 0.86 2.30 2.974(12) 136 . N3 H3 O15 0.86 1.89 2.745(5) 172 1_455 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.963 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.105 _vrf_PLAT420_7b ; PROBLEM: D-H Without Acceptor >O16 - >H16A ... ? RESPONSE: According to the hydrogen bonding environment, O16-H16A...O5( O16...O5 = 2.949\%A ) should be considered. ; # END data_8a #TrackingRef '- 1-9.cif' _database_code_depnum_ccdc_archive 'CCDC 788593' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H46 Cu2 N14 O4, 2(Cl O4)' _chemical_formula_sum 'C56 H46 Cl2 Cu2 N14 O12' _chemical_formula_weight 1305.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.243(2) _cell_length_b 13.6868(15) _cell_length_c 20.161(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.859(3) _cell_angle_gamma 90.00 _cell_volume 6169.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 3714 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 20.12 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8292 _exptl_absorpt_correction_T_max 0.9202 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(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 22203 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5362 _reflns_number_gt 3945 _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. In the refinement, the Cl1/O3-O6 perchlorate anion was symmetrically disordered about a two-fold axis and the Cl1'/O3'-O5' perchlorate anion was symmetrically disordered by an inversion center. Then, 'PART -1' instruction was used for these atoms and the occupancies of all atoms in this group were set to 0.5. Also in the refinement command 'DFIX' was used to restrain the Cl-O and O...O distances of 1.42(1) and 2.45(2)\%A, respectively. 'ISOR' was used to restrain some abnormal thermal factors of these oxygen atoms. ; _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^)+(0.1486P)^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 5362 _refine_ls_number_parameters 433 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.2110 _refine_ls_wR_factor_gt 0.1942 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.136 _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 0.65316(2) 0.57972(4) 0.58480(3) 0.0414(3) Uani 1 1 d . . . C1 C 0.6059(2) 0.7073(4) 0.6791(3) 0.0522(13) Uani 1 1 d . . . H1A H 0.6021 0.7751 0.6914 0.063 Uiso 1 1 calc R . . H1B H 0.5745 0.6700 0.6907 0.063 Uiso 1 1 calc R . . C2 C 0.6655(2) 0.6688(4) 0.7177(2) 0.0470(12) Uani 1 1 d . . . C3 C 0.7465(2) 0.5822(3) 0.7427(2) 0.0425(11) Uani 1 1 d . . . C4 C 0.7938(2) 0.5209(4) 0.7423(3) 0.0483(12) Uani 1 1 d . . . H4 H 0.7950 0.4863 0.7030 0.058 Uiso 1 1 calc R . . C5 C 0.8387(2) 0.5133(4) 0.8023(3) 0.0568(14) Uani 1 1 d . . . H5 H 0.8716 0.4745 0.8029 0.068 Uiso 1 1 calc R . . C6 C 0.8367(3) 0.5614(4) 0.8623(3) 0.0648(16) Uani 1 1 d . . . H6 H 0.8675 0.5518 0.9023 0.078 Uiso 1 1 calc R . . C7 C 0.7910(3) 0.6220(4) 0.8637(3) 0.0621(15) Uani 1 1 d . . . H7 H 0.7904 0.6556 0.9036 0.075 Uiso 1 1 calc R . . C8 C 0.7442(2) 0.6324(4) 0.8026(2) 0.0499(12) Uani 1 1 d . . . C9 C 0.6198(3) 0.7891(4) 0.5772(3) 0.0576(13) Uani 1 1 d . . . H9A H 0.6509 0.8206 0.6129 0.069 Uiso 1 1 calc R . . H9B H 0.5865 0.8342 0.5622 0.069 Uiso 1 1 calc R . . C10 C 0.6432(2) 0.7612(4) 0.5180(3) 0.0477(12) Uani 1 1 d . . . C11 C 0.6689(2) 0.7660(4) 0.4216(3) 0.0472(12) Uani 1 1 d . . . C12 C 0.6761(3) 0.7871(4) 0.3569(3) 0.0637(15) Uani 1 1 d . . . H12 H 0.6644 0.8466 0.3350 0.076 Uiso 1 1 calc R . . C13 C 0.7014(3) 0.7150(5) 0.3273(3) 0.0690(16) Uani 1 1 d . . . H13 H 0.7064 0.7252 0.2835 0.083 Uiso 1 1 calc R . . C14 C 0.7201(3) 0.6265(5) 0.3607(3) 0.0643(15) Uani 1 1 d . . . H14 H 0.7382 0.5802 0.3393 0.077 Uiso 1 1 calc R . . C15 C 0.7125(2) 0.6063(4) 0.4241(3) 0.0530(13) Uani 1 1 d . . . H15 H 0.7253 0.5474 0.4462 0.064 Uiso 1 1 calc R . . C16 C 0.6849(2) 0.6768(3) 0.4542(2) 0.0439(11) Uani 1 1 d . . . C17 C 0.5375(2) 0.6711(4) 0.5658(3) 0.0540(13) Uani 1 1 d . . . H17A H 0.5088 0.7103 0.5810 0.065 Uiso 1 1 calc R . . H17B H 0.5308 0.6802 0.5165 0.065 Uiso 1 1 calc R . . C18 C 0.5316(2) 0.5669(4) 0.5819(2) 0.0482(12) Uani 1 1 d . . . C19 C 0.4991(2) 0.4268(4) 0.6112(3) 0.0566(14) Uani 1 1 d . . . C20 C 0.4681(3) 0.3512(5) 0.6281(4) 0.0793(19) Uani 1 1 d . . . H20 H 0.4281 0.3573 0.6272 0.095 Uiso 1 1 calc R . . C21 C 0.4988(4) 0.2651(6) 0.6464(4) 0.089(2) Uani 1 1 d . . . H21 H 0.4787 0.2118 0.6581 0.107 Uiso 1 1 calc R . . C22 C 0.5570(3) 0.2549(5) 0.6482(4) 0.084(2) Uani 1 1 d . . . H22 H 0.5757 0.1953 0.6617 0.101 Uiso 1 1 calc R . . C23 C 0.5894(3) 0.3301(4) 0.6305(3) 0.0687(16) Uani 1 1 d . . . H23 H 0.6292 0.3227 0.6307 0.082 Uiso 1 1 calc R . . C24 C 0.5588(2) 0.4180(4) 0.6124(3) 0.0516(13) Uani 1 1 d . . . C25 C 0.6782(2) 0.4157(3) 0.5166(2) 0.0426(11) Uani 1 1 d . . . C26 C 0.71576(18) 0.3302(3) 0.5091(2) 0.0350(10) Uani 1 1 d . . . C27 C 0.69054(19) 0.2550(3) 0.4638(2) 0.0388(10) Uani 1 1 d . . . H27 H 0.6504 0.2583 0.4393 0.047 Uiso 1 1 calc R . . C28 C 0.7758(2) 0.3239(3) 0.5450(2) 0.0413(11) Uani 1 1 d . . . H28 H 0.7934 0.3735 0.5752 0.050 Uiso 1 1 calc R . . N1 N 0.60001(19) 0.6993(3) 0.6037(2) 0.0475(10) Uani 1 1 d . . . N2 N 0.69596(18) 0.6075(3) 0.68985(19) 0.0432(9) Uani 1 1 d . . . N3 N 0.6935(2) 0.6868(3) 0.7848(2) 0.0524(11) Uani 1 1 d . . . H3 H 0.6813 0.7259 0.8115 0.063 Uiso 1 1 calc R . . N4 N 0.66831(18) 0.6766(3) 0.5155(2) 0.0446(9) Uani 1 1 d . . . N5 N 0.6429(2) 0.8191(3) 0.4639(2) 0.0533(11) Uani 1 1 d . . . H5A H 0.6292 0.8777 0.4571 0.064 Uiso 1 1 calc R . . N6 N 0.57817(18) 0.5086(3) 0.5938(2) 0.0492(10) Uani 1 1 d . . . N7 N 0.48325(18) 0.5221(4) 0.5911(2) 0.0570(12) Uani 1 1 d . . . H7A H 0.4485 0.5478 0.5855 0.068 Uiso 1 1 calc R . . O1 O 0.69994(14) 0.4713(2) 0.56885(17) 0.0483(8) Uani 1 1 d . . . O2 O 0.62989(16) 0.4293(3) 0.4739(2) 0.0641(11) Uani 1 1 d . . . Cl1 Cl 0.45091(12) 0.8212(3) 0.68767(15) 0.0721(9) Uani 0.50 1 d PD A -1 O3 O 0.3906(2) 0.8466(4) 0.6850(3) 0.0344(13) Uani 0.50 1 d PDU A -1 O4 O 0.4454(7) 0.7119(6) 0.6780(8) 0.154(5) Uani 0.50 1 d PDU A -1 O5 O 0.4904(8) 0.8320(11) 0.7570(7) 0.185(8) Uani 0.50 1 d PDU A -1 O6 O 0.4744(6) 0.8546(9) 0.6331(6) 0.135(4) Uani 0.50 1 d PDU A -1 Cl1' Cl 0.53719(14) 0.9610(2) 0.94339(17) 0.0727(8) Uani 0.50 1 d PD B -1 O3' O 0.4822(5) 0.9567(14) 0.8905(7) 0.179(6) Uani 0.50 1 d PDU B -1 O4' O 0.5899(4) 0.9953(7) 0.9362(6) 0.113(4) Uani 0.50 1 d PDU B -1 O5' O 0.5305(7) 1.0212(12) 1.0012(8) 0.195(7) Uani 0.50 1 d PDU B -1 O6' O 0.5500(8) 0.8602(8) 0.9682(10) 0.211(8) Uani 0.50 1 d PDU B -1 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 0.0481(4) 0.0382(4) 0.0403(4) -0.0030(2) 0.0160(3) 0.0148(2) C1 0.065(3) 0.049(3) 0.047(3) -0.011(2) 0.021(2) 0.014(2) C2 0.057(3) 0.045(3) 0.043(3) -0.004(2) 0.020(2) 0.003(2) C3 0.048(3) 0.039(3) 0.041(2) 0.0026(19) 0.013(2) -0.004(2) C4 0.054(3) 0.045(3) 0.047(3) 0.006(2) 0.015(2) 0.002(2) C5 0.057(3) 0.049(3) 0.063(3) 0.017(3) 0.014(3) 0.005(2) C6 0.061(4) 0.075(4) 0.053(3) 0.012(3) 0.005(3) -0.008(3) C7 0.071(4) 0.068(4) 0.045(3) -0.006(3) 0.012(3) -0.012(3) C8 0.054(3) 0.054(3) 0.042(3) -0.001(2) 0.014(2) -0.010(2) C9 0.072(4) 0.046(3) 0.060(3) 0.000(2) 0.029(3) 0.015(3) C10 0.050(3) 0.042(3) 0.051(3) -0.002(2) 0.014(2) 0.007(2) C11 0.043(3) 0.045(3) 0.055(3) 0.003(2) 0.016(2) 0.001(2) C12 0.068(4) 0.058(3) 0.070(4) 0.015(3) 0.028(3) 0.001(3) C13 0.078(4) 0.075(4) 0.062(4) 0.000(3) 0.032(3) -0.012(3) C14 0.069(4) 0.073(4) 0.062(3) -0.005(3) 0.037(3) -0.004(3) C15 0.055(3) 0.049(3) 0.062(3) 0.000(2) 0.027(3) 0.004(2) C16 0.040(2) 0.046(3) 0.046(3) 0.000(2) 0.014(2) 0.002(2) C17 0.050(3) 0.058(3) 0.051(3) -0.001(2) 0.010(2) 0.022(2) C18 0.038(3) 0.062(3) 0.043(3) -0.006(2) 0.009(2) 0.013(2) C19 0.038(3) 0.068(4) 0.059(3) -0.005(3) 0.007(2) -0.004(3) C20 0.055(4) 0.082(5) 0.096(5) -0.009(4) 0.013(3) -0.007(3) C21 0.080(5) 0.078(5) 0.112(6) -0.003(4) 0.030(4) -0.023(4) C22 0.081(5) 0.055(4) 0.124(6) 0.004(4) 0.039(4) -0.001(3) C23 0.061(4) 0.052(3) 0.094(4) 0.006(3) 0.021(3) 0.008(3) C24 0.041(3) 0.054(3) 0.059(3) -0.011(2) 0.012(2) 0.006(2) C25 0.041(3) 0.042(3) 0.045(3) 0.004(2) 0.015(2) 0.015(2) C26 0.032(2) 0.037(2) 0.037(2) 0.0027(18) 0.0108(18) 0.0088(18) C27 0.027(2) 0.047(3) 0.040(2) -0.005(2) 0.0060(18) 0.0075(19) C28 0.038(2) 0.044(3) 0.040(2) -0.009(2) 0.0081(19) 0.005(2) N1 0.057(2) 0.042(2) 0.046(2) -0.0040(17) 0.0176(18) 0.0163(19) N2 0.056(2) 0.040(2) 0.038(2) -0.0001(17) 0.0186(18) 0.0096(18) N3 0.066(3) 0.053(3) 0.041(2) -0.0134(19) 0.0199(19) 0.005(2) N4 0.052(2) 0.039(2) 0.048(2) -0.0001(17) 0.0220(18) 0.0117(18) N5 0.062(3) 0.037(2) 0.065(3) 0.004(2) 0.025(2) 0.0070(19) N6 0.047(2) 0.046(2) 0.054(2) -0.0018(19) 0.0139(19) 0.0094(19) N7 0.035(2) 0.069(3) 0.063(3) -0.005(2) 0.009(2) 0.011(2) O1 0.0506(19) 0.0438(19) 0.0513(19) -0.0093(15) 0.0153(15) 0.0153(15) O2 0.047(2) 0.071(3) 0.065(2) -0.0078(18) 0.0002(18) 0.0328(18) Cl1 0.0534(16) 0.115(3) 0.0502(15) -0.0005(15) 0.0172(12) 0.0011(16) O3 0.020(3) 0.054(3) 0.028(3) 0.008(2) 0.003(2) -0.002(2) O4 0.167(9) 0.128(8) 0.172(9) 0.007(7) 0.052(8) 0.011(8) O5 0.164(11) 0.227(10) 0.152(9) 0.014(10) 0.024(8) -0.027(10) O6 0.156(8) 0.124(8) 0.153(8) 0.014(7) 0.088(7) 0.048(7) Cl1' 0.0653(18) 0.0637(18) 0.081(2) -0.0147(15) 0.0063(15) -0.0125(15) O3' 0.135(9) 0.212(10) 0.171(10) -0.007(9) 0.014(8) -0.045(9) O4' 0.072(5) 0.082(6) 0.168(8) 0.008(5) 0.002(5) -0.064(5) O5' 0.200(11) 0.172(10) 0.203(11) -0.040(9) 0.039(9) -0.041(9) O6' 0.211(11) 0.183(11) 0.243(12) 0.006(9) 0.069(9) -0.015(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.918(3) . ? Cu1 N4 2.025(4) . ? Cu1 N6 2.047(4) . ? Cu1 N2 2.114(4) . ? Cu1 N1 2.147(4) . ? C1 C2 1.488(7) . ? C1 N1 1.491(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.318(6) . ? C2 N3 1.355(6) . ? C3 C4 1.385(7) . ? C3 N2 1.396(6) . ? C3 C8 1.403(7) . ? C4 C5 1.367(7) . ? C4 H4 0.9300 . ? C5 C6 1.389(8) . ? C5 H5 0.9300 . ? C6 C7 1.355(9) . ? C6 H6 0.9300 . ? C7 C8 1.410(7) . ? C7 H7 0.9300 . ? C8 N3 1.356(7) . ? C9 N1 1.464(7) . ? C9 C10 1.491(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.305(6) . ? C10 N5 1.346(6) . ? C11 N5 1.380(6) . ? C11 C16 1.389(7) . ? C11 C12 1.390(7) . ? C12 C13 1.366(9) . ? C12 H12 0.9300 . ? C13 C14 1.397(9) . ? C13 H13 0.9300 . ? C14 C15 1.365(7) . ? C14 H14 0.9300 . ? C15 C16 1.387(7) . ? C15 H15 0.9300 . ? C16 N4 1.392(6) . ? C17 C18 1.476(7) . ? C17 N1 1.496(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.313(6) . ? C18 N7 1.338(7) . ? C19 C20 1.356(9) . ? C19 N7 1.385(7) . ? C19 C24 1.386(8) . ? C20 C21 1.375(10) . ? C20 H20 0.9300 . ? C21 C22 1.350(10) . ? C21 H21 0.9300 . ? C22 C23 1.379(9) . ? C22 H22 0.9300 . ? C23 C24 1.395(7) . ? C23 H23 0.9300 . ? C24 N6 1.405(7) . ? C25 O2 1.229(6) . ? C25 O1 1.285(6) . ? C25 C26 1.492(6) . ? C26 C28 1.389(6) . ? C26 C27 1.394(6) . ? C27 C28 1.372(6) 7_656 ? C27 H27 0.9300 . ? C28 C27 1.372(6) 7_656 ? C28 H28 0.9300 . ? N3 H3 0.8600 . ? N5 H5A 0.8600 . ? N7 H7A 0.8600 . ? Cl1 O3 1.431(5) . ? Cl1 O6 1.432(8) . ? Cl1 O5 1.456(9) . ? Cl1 O4 1.509(8) . ? Cl1' O4' 1.357(7) . ? Cl1' O3' 1.425(8) . ? Cl1' O5' 1.470(9) . ? Cl1' O6' 1.470(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 O1 Cu1 N4 100.23(15) . . ? O1 Cu1 N6 100.48(15) . . ? N4 Cu1 N6 133.23(16) . . ? O1 Cu1 N2 100.01(14) . . ? N4 Cu1 N2 116.78(16) . . ? N6 Cu1 N2 100.13(16) . . ? O1 Cu1 N1 178.92(16) . . ? N4 Cu1 N1 80.82(15) . . ? N6 Cu1 N1 78.56(16) . . ? N2 Cu1 N1 79.69(15) . . ? C2 C1 N1 108.6(4) . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1B 110.0 . . ? N1 C1 H1B 110.0 . . ? H1A C1 H1B 108.3 . . ? N2 C2 N3 112.0(4) . . ? N2 C2 C1 122.3(4) . . ? N3 C2 C1 125.6(4) . . ? C4 C3 N2 130.5(4) . . ? C4 C3 C8 121.2(4) . . ? N2 C3 C8 108.3(4) . . ? C5 C4 C3 117.2(5) . . ? C5 C4 H4 121.4 . . ? C3 C4 H4 121.4 . . ? C4 C5 C6 122.4(5) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C7 C6 C5 121.4(5) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 117.7(5) . . ? C6 C7 H7 121.1 . . ? C8 C7 H7 121.1 . . ? N3 C8 C3 106.0(4) . . ? N3 C8 C7 133.8(5) . . ? C3 C8 C7 120.1(5) . . ? N1 C9 C10 107.3(4) . . ? N1 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? N1 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? N4 C10 N5 113.3(4) . . ? N4 C10 C9 121.5(4) . . ? N5 C10 C9 125.2(4) . . ? N5 C11 C16 106.0(4) . . ? N5 C11 C12 131.1(5) . . ? C16 C11 C12 122.8(5) . . ? C13 C12 C11 115.9(5) . . ? C13 C12 H12 122.1 . . ? C11 C12 H12 122.1 . . ? C12 C13 C14 122.0(6) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C15 C14 C13 121.6(6) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C16 117.6(5) . . ? C14 C15 H15 121.2 . . ? C16 C15 H15 121.2 . . ? C15 C16 C11 119.9(5) . . ? C15 C16 N4 131.4(5) . . ? C11 C16 N4 108.7(4) . . ? C18 C17 N1 105.8(4) . . ? C18 C17 H17A 110.6 . . ? N1 C17 H17A 110.6 . . ? C18 C17 H17B 110.6 . . ? N1 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? N6 C18 N7 112.2(5) . . ? N6 C18 C17 120.4(5) . . ? N7 C18 C17 127.2(4) . . ? C20 C19 N7 132.5(5) . . ? C20 C19 C24 121.8(6) . . ? N7 C19 C24 105.7(5) . . ? C19 C20 C21 116.7(6) . . ? C19 C20 H20 121.6 . . ? C21 C20 H20 121.6 . . ? C22 C21 C20 122.5(7) . . ? C22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C21 C22 C23 122.0(7) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C22 C23 C24 115.8(6) . . ? C22 C23 H23 122.1 . . ? C24 C23 H23 122.1 . . ? C19 C24 C23 121.1(5) . . ? C19 C24 N6 108.2(4) . . ? C23 C24 N6 130.7(5) . . ? O2 C25 O1 124.3(4) . . ? O2 C25 C26 119.7(4) . . ? O1 C25 C26 116.0(4) . . ? C28 C26 C27 118.6(4) . . ? C28 C26 C25 121.9(4) . . ? C27 C26 C25 119.5(4) . . ? C28 C27 C26 120.8(4) 7_656 . ? C28 C27 H27 119.6 7_656 . ? C26 C27 H27 119.6 . . ? C27 C28 C26 120.6(4) 7_656 . ? C27 C28 H28 119.7 7_656 . ? C26 C28 H28 119.7 . . ? C9 N1 C1 111.0(4) . . ? C9 N1 C17 112.8(4) . . ? C1 N1 C17 110.2(4) . . ? C9 N1 Cu1 108.8(3) . . ? C1 N1 Cu1 109.9(3) . . ? C17 N1 Cu1 103.8(3) . . ? C2 N2 C3 105.7(4) . . ? C2 N2 Cu1 112.4(3) . . ? C3 N2 Cu1 142.0(3) . . ? C2 N3 C8 108.0(4) . . ? C2 N3 H3 126.0 . . ? C8 N3 H3 126.0 . . ? C10 N4 C16 105.5(4) . . ? C10 N4 Cu1 113.0(3) . . ? C16 N4 Cu1 139.1(3) . . ? C10 N5 C11 106.6(4) . . ? C10 N5 H5A 126.7 . . ? C11 N5 H5A 126.7 . . ? C18 N6 C24 106.1(4) . . ? C18 N6 Cu1 111.9(3) . . ? C24 N6 Cu1 141.9(3) . . ? C18 N7 C19 107.8(4) . . ? C18 N7 H7A 126.1 . . ? C19 N7 H7A 126.1 . . ? C25 O1 Cu1 118.8(3) . . ? O3 Cl1 O6 118.0(6) . . ? O3 Cl1 O5 111.4(9) . . ? O6 Cl1 O5 115.7(10) . . ? O3 Cl1 O4 100.8(6) . . ? O6 Cl1 O4 104.8(7) . . ? O5 Cl1 O4 103.5(8) . . ? O4' Cl1' O3' 125.9(8) . . ? O4' Cl1' O5' 100.7(7) . . ? O3' Cl1' O5' 110.4(9) . . ? O4' Cl1' O6' 104.8(8) . . ? O3' Cl1' O6' 105.8(9) . . ? O5' Cl1' O6' 108.2(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -22.3(7) . . . . ? N1 C1 C2 N3 161.5(5) . . . . ? N2 C3 C4 C5 177.4(5) . . . . ? C8 C3 C4 C5 -1.5(7) . . . . ? C3 C4 C5 C6 2.4(8) . . . . ? C4 C5 C6 C7 -2.7(9) . . . . ? C5 C6 C7 C8 1.9(9) . . . . ? C4 C3 C8 N3 178.6(4) . . . . ? N2 C3 C8 N3 -0.6(5) . . . . ? C4 C3 C8 C7 0.8(7) . . . . ? N2 C3 C8 C7 -178.3(5) . . . . ? C6 C7 C8 N3 -178.0(6) . . . . ? C6 C7 C8 C3 -1.0(8) . . . . ? N1 C9 C10 N4 -30.7(7) . . . . ? N1 C9 C10 N5 151.5(5) . . . . ? N5 C11 C12 C13 -176.5(5) . . . . ? C16 C11 C12 C13 -1.6(8) . . . . ? C11 C12 C13 C14 -1.3(9) . . . . ? C12 C13 C14 C15 1.9(10) . . . . ? C13 C14 C15 C16 0.5(9) . . . . ? C14 C15 C16 C11 -3.3(8) . . . . ? C14 C15 C16 N4 176.6(5) . . . . ? N5 C11 C16 C15 -180.0(4) . . . . ? C12 C11 C16 C15 4.0(8) . . . . ? N5 C11 C16 N4 0.1(5) . . . . ? C12 C11 C16 N4 -175.9(5) . . . . ? N1 C17 C18 N6 -31.1(6) . . . . ? N1 C17 C18 N7 143.9(5) . . . . ? N7 C19 C20 C21 -179.6(6) . . . . ? C24 C19 C20 C21 0.0(10) . . . . ? C19 C20 C21 C22 0.2(11) . . . . ? C20 C21 C22 C23 -1.1(13) . . . . ? C21 C22 C23 C24 1.5(11) . . . . ? C20 C19 C24 C23 0.5(9) . . . . ? N7 C19 C24 C23 -179.7(5) . . . . ? C20 C19 C24 N6 -179.0(5) . . . . ? N7 C19 C24 N6 0.8(6) . . . . ? C22 C23 C24 C19 -1.3(9) . . . . ? C22 C23 C24 N6 178.1(6) . . . . ? O2 C25 C26 C28 164.2(5) . . . . ? O1 C25 C26 C28 -15.5(7) . . . . ? O2 C25 C26 C27 -14.5(7) . . . . ? O1 C25 C26 C27 165.8(4) . . . . ? C28 C26 C27 C28 0.3(7) . . . 7_656 ? C25 C26 C27 C28 179.0(4) . . . 7_656 ? C27 C26 C28 C27 -0.3(7) . . . 7_656 ? C25 C26 C28 C27 -179.0(4) . . . 7_656 ? C10 C9 N1 C1 150.5(4) . . . . ? C10 C9 N1 C17 -85.2(5) . . . . ? C10 C9 N1 Cu1 29.4(5) . . . . ? C2 C1 N1 C9 -92.2(5) . . . . ? C2 C1 N1 C17 142.0(4) . . . . ? C2 C1 N1 Cu1 28.3(5) . . . . ? C18 C17 N1 C9 161.9(4) . . . . ? C18 C17 N1 C1 -73.4(5) . . . . ? C18 C17 N1 Cu1 44.3(4) . . . . ? N4 Cu1 N1 C9 -19.4(3) . . . . ? N6 Cu1 N1 C9 -157.2(4) . . . . ? N2 Cu1 N1 C9 100.1(4) . . . . ? N4 Cu1 N1 C1 -141.2(4) . . . . ? N6 Cu1 N1 C1 81.0(3) . . . . ? N2 Cu1 N1 C1 -21.7(3) . . . . ? N4 Cu1 N1 C17 100.9(3) . . . . ? N6 Cu1 N1 C17 -36.8(3) . . . . ? N2 Cu1 N1 C17 -139.5(3) . . . . ? N3 C2 N2 C3 1.3(6) . . . . ? C1 C2 N2 C3 -175.3(5) . . . . ? N3 C2 N2 Cu1 -179.5(3) . . . . ? C1 C2 N2 Cu1 3.8(6) . . . . ? C4 C3 N2 C2 -179.5(5) . . . . ? C8 C3 N2 C2 -0.5(5) . . . . ? C4 C3 N2 Cu1 1.8(9) . . . . ? C8 C3 N2 Cu1 -179.2(4) . . . . ? O1 Cu1 N2 C2 -168.6(3) . . . . ? N4 Cu1 N2 C2 84.4(4) . . . . ? N6 Cu1 N2 C2 -66.0(4) . . . . ? N1 Cu1 N2 C2 10.3(3) . . . . ? O1 Cu1 N2 C3 10.1(5) . . . . ? N4 Cu1 N2 C3 -96.8(5) . . . . ? N6 Cu1 N2 C3 112.7(5) . . . . ? N1 Cu1 N2 C3 -171.0(5) . . . . ? N2 C2 N3 C8 -1.7(6) . . . . ? C1 C2 N3 C8 174.8(5) . . . . ? C3 C8 N3 C2 1.3(5) . . . . ? C7 C8 N3 C2 178.6(6) . . . . ? N5 C10 N4 C16 -1.5(6) . . . . ? C9 C10 N4 C16 -179.5(5) . . . . ? N5 C10 N4 Cu1 -167.6(3) . . . . ? C9 C10 N4 Cu1 14.4(6) . . . . ? C15 C16 N4 C10 -179.1(5) . . . . ? C11 C16 N4 C10 0.8(5) . . . . ? C15 C16 N4 Cu1 -18.7(9) . . . . ? C11 C16 N4 Cu1 161.1(4) . . . . ? O1 Cu1 N4 C10 -176.8(3) . . . . ? N6 Cu1 N4 C10 68.2(4) . . . . ? N2 Cu1 N4 C10 -70.0(4) . . . . ? N1 Cu1 N4 C10 3.5(3) . . . . ? O1 Cu1 N4 C16 23.8(5) . . . . ? N6 Cu1 N4 C16 -91.2(5) . . . . ? N2 Cu1 N4 C16 130.6(5) . . . . ? N1 Cu1 N4 C16 -155.9(5) . . . . ? N4 C10 N5 C11 1.6(6) . . . . ? C9 C10 N5 C11 179.5(5) . . . . ? C16 C11 N5 C10 -1.0(5) . . . . ? C12 C11 N5 C10 174.6(6) . . . . ? N7 C18 N6 C24 -0.1(6) . . . . ? C17 C18 N6 C24 175.6(4) . . . . ? N7 C18 N6 Cu1 -176.9(3) . . . . ? C17 C18 N6 Cu1 -1.1(6) . . . . ? C19 C24 N6 C18 -0.4(6) . . . . ? C23 C24 N6 C18 -179.9(6) . . . . ? C19 C24 N6 Cu1 174.7(4) . . . . ? C23 C24 N6 Cu1 -4.8(10) . . . . ? O1 Cu1 N6 C18 -158.5(3) . . . . ? N4 Cu1 N6 C18 -43.6(4) . . . . ? N2 Cu1 N6 C18 99.2(3) . . . . ? N1 Cu1 N6 C18 22.0(3) . . . . ? O1 Cu1 N6 C24 26.6(6) . . . . ? N4 Cu1 N6 C24 141.6(5) . . . . ? N2 Cu1 N6 C24 -75.7(5) . . . . ? N1 Cu1 N6 C24 -152.9(6) . . . . ? N6 C18 N7 C19 0.6(6) . . . . ? C17 C18 N7 C19 -174.7(5) . . . . ? C20 C19 N7 C18 178.9(7) . . . . ? C24 C19 N7 C18 -0.8(6) . . . . ? O2 C25 O1 Cu1 3.0(7) . . . . ? C26 C25 O1 Cu1 -177.3(3) . . . . ? N4 Cu1 O1 C25 -79.3(4) . . . . ? N6 Cu1 O1 C25 58.5(4) . . . . ? N2 Cu1 O1 C25 160.9(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O3 0.86 2.37 3.103(7) 144.1 2_656 N5 H5A O4' 0.86 1.96 2.812(9) 173.9 6_575 N7 H7A O2 0.86 1.91 2.682(5) 148.2 5_666 C9 H9B O5' 0.97 2.50 3.414(14) 157.0 6_575 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.227 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.109 # start Validation Reply Form _vrf_PLAT221_8a ; PROBLEM: Large Solvent/Anion O Ueq(max)/Ueq(min) ... 5.3 Ratio RESPONSE: This is due to the disorder of the two perchlorate anions. ; # end Validation Reply Form data_8b #TrackingRef '- 1-9.cif' _database_code_depnum_ccdc_archive 'CCDC 788594' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H88 Cu4 N28 O4, 6(Cl O4)' _chemical_formula_sum 'C104 H88 Cl6 Cu4 N28 O28' _chemical_formula_weight 2644.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.543(8) _cell_length_b 14.6474(10) _cell_length_c 19.1303(12) _cell_angle_alpha 72.599(1) _cell_angle_beta 85.227(2) _cell_angle_gamma 74.410(1) _cell_volume 2715(2) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4916 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 21.57 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1350 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7019 _exptl_absorpt_correction_T_max 0.8387 _exptl_absorpt_process_details 'SADABS, Sheldrick,1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 26502 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9525 _reflns_number_gt 5876 _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. In the refinement, all the three perchlorate anions were found to be disordered over two sites and command 'SADI' was used to restrain the Cl-O and O...O distances to be equal to each other. The final occupancies are of 0.73(1):0.27(1), 0.74(1):0.26(1) and 0.51(1):0.49(1) for the Cl1/O3-O6, Cl2/O7-O10 and Cl3/O11-O14 anions, respectively. ; _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^)+(0.0782P)^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 9525 _refine_ls_number_parameters 892 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1439 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.68760(5) 0.75920(4) 0.76938(3) 0.0405(2) Uani 1 1 d . . . Cu2 Cu 0.58856(5) 0.48499(4) 0.75227(3) 0.04052(19) Uani 1 1 d . . . C1 C 0.7756(5) 0.8978(4) 0.6357(3) 0.0490(13) Uani 1 1 d . . . H1A H 0.8653 0.8679 0.6236 0.059 Uiso 1 1 calc R . . H1B H 0.7389 0.9532 0.5940 0.059 Uiso 1 1 calc R . . C2 C 0.7763(4) 0.9342(3) 0.7003(3) 0.0404(12) Uani 1 1 d . . . C3 C 0.7770(4) 0.9415(3) 0.8109(3) 0.0402(12) Uani 1 1 d . . . C4 C 0.7725(5) 0.9252(4) 0.8860(3) 0.0527(14) Uani 1 1 d . . . H4 H 0.7569 0.8669 0.9170 0.063 Uiso 1 1 calc R . . C5 C 0.7915(5) 0.9965(4) 0.9139(3) 0.0607(15) Uani 1 1 d . . . H5 H 0.7893 0.9860 0.9643 0.073 Uiso 1 1 calc R . . C6 C 0.8140(5) 1.0845(4) 0.8677(4) 0.0598(16) Uani 1 1 d . . . H6 H 0.8253 1.1321 0.8880 0.072 Uiso 1 1 calc R . . C7 C 0.8200(5) 1.1024(4) 0.7931(4) 0.0531(15) Uani 1 1 d . . . H7 H 0.8354 1.1609 0.7622 0.064 Uiso 1 1 calc R . . C8 C 0.8019(4) 1.0292(3) 0.7661(3) 0.0420(12) Uani 1 1 d . . . C9 C 0.5573(5) 0.8693(4) 0.6243(3) 0.0521(14) Uani 1 1 d . . . H9A H 0.5524 0.9303 0.5852 0.063 Uiso 1 1 calc R . . H9B H 0.5272 0.8243 0.6053 0.063 Uiso 1 1 calc R . . C10 C 0.4728(5) 0.8900(4) 0.6869(3) 0.0413(12) Uani 1 1 d . . . C11 C 0.4018(4) 0.8759(3) 0.7985(3) 0.0369(11) Uani 1 1 d . . . C12 C 0.3837(5) 0.8483(4) 0.8736(3) 0.0482(13) Uani 1 1 d . . . H12 H 0.4473 0.7998 0.9046 0.058 Uiso 1 1 calc R . . C13 C 0.2676(6) 0.8957(5) 0.9006(4) 0.0686(18) Uani 1 1 d . . . H13 H 0.2522 0.8794 0.9509 0.082 Uiso 1 1 calc R . . C14 C 0.1729(6) 0.9679(5) 0.8531(5) 0.079(2) Uani 1 1 d . . . H14 H 0.0954 0.9981 0.8732 0.095 Uiso 1 1 calc R . . C15 C 0.1879(5) 0.9961(4) 0.7796(4) 0.0660(17) Uani 1 1 d . . . H15 H 0.1237 1.0448 0.7491 0.079 Uiso 1 1 calc R . . C16 C 0.3058(5) 0.9477(4) 0.7518(3) 0.0477(13) Uani 1 1 d . . . C17 C 0.7666(6) 0.7395(4) 0.6210(4) 0.0721(19) Uani 1 1 d . . . H17A H 0.7050 0.7047 0.6134 0.087 Uiso 1 1 calc R . . H17B H 0.8089 0.7636 0.5747 0.087 Uiso 1 1 calc R . . C18 C 0.8643(6) 0.6741(4) 0.6756(4) 0.0674(19) Uani 1 1 d . . . C19 C 0.9503(3) 0.6003(3) 0.7800(3) 0.074(2) Uani 1 1 d G . . C20 C 0.9836(4) 0.5652(3) 0.8538(3) 0.088(2) Uani 1 1 d G . . H20 H 0.9301 0.5923 0.8875 0.106 Uiso 1 1 calc R . . C21 C 1.0968(5) 0.4897(4) 0.8771(3) 0.106(3) Uani 1 1 d G . . H21 H 1.1191 0.4662 0.9265 0.127 Uiso 1 1 calc R . . C22 C 1.1768(4) 0.4492(3) 0.8266(4) 0.099(3) Uani 1 1 d G . . H22 H 1.2525 0.3986 0.8422 0.118 Uiso 1 1 calc R . . C23 C 1.1435(4) 0.4843(3) 0.7528(4) 0.102(3) Uani 1 1 d G . . H23 H 1.1970 0.4572 0.7191 0.122 Uiso 1 1 calc R . . C24 C 1.0302(4) 0.5598(3) 0.7295(3) 0.077(2) Uani 1 1 d G . . C25 C 0.5600(5) 0.5585(3) 0.5882(3) 0.0461(13) Uani 1 1 d . . . H25A H 0.5280 0.5462 0.5466 0.055 Uiso 1 1 calc R . . H25B H 0.6213 0.5993 0.5704 0.055 Uiso 1 1 calc R . . C26 C 0.4471(5) 0.6102(3) 0.6269(3) 0.0419(12) Uani 1 1 d . . . C27 C 0.3304(4) 0.6579(3) 0.7143(3) 0.0385(12) Uani 1 1 d . . . C28 C 0.2745(5) 0.6724(4) 0.7799(3) 0.0496(14) Uani 1 1 d . . . H28 H 0.3075 0.6291 0.8247 0.059 Uiso 1 1 calc R . . C29 C 0.1686(5) 0.7530(4) 0.7765(3) 0.0548(15) Uani 1 1 d . . . H29 H 0.1313 0.7652 0.8197 0.066 Uiso 1 1 calc R . . C30 C 0.1170(5) 0.8158(4) 0.7100(4) 0.0594(16) Uani 1 1 d . . . H30 H 0.0449 0.8690 0.7099 0.071 Uiso 1 1 calc R . . C31 C 0.1672(5) 0.8033(4) 0.6446(4) 0.0589(15) Uani 1 1 d . . . H31 H 0.1317 0.8462 0.6002 0.071 Uiso 1 1 calc R . . C32 C 0.2748(5) 0.7224(4) 0.6483(3) 0.0456(13) Uani 1 1 d . . . C33 C 0.5659(6) 0.3846(4) 0.6388(3) 0.0549(14) Uani 1 1 d . . . H33A H 0.4858 0.4142 0.6101 0.066 Uiso 1 1 calc R . . H33B H 0.6258 0.3409 0.6143 0.066 Uiso 1 1 calc R . . C34 C 0.5338(4) 0.3253(3) 0.7117(3) 0.0395(12) Uani 1 1 d . . . C35 C 0.4986(4) 0.2710(3) 0.8285(3) 0.0338(11) Uani 1 1 d . . . C36 C 0.4904(5) 0.2527(3) 0.9039(3) 0.0421(12) Uani 1 1 d . . . H36 H 0.5074 0.2964 0.9263 0.051 Uiso 1 1 calc R . . C37 C 0.4564(5) 0.1679(4) 0.9446(3) 0.0515(14) Uani 1 1 d . . . H37 H 0.4484 0.1547 0.9952 0.062 Uiso 1 1 calc R . . C38 C 0.4336(5) 0.1013(4) 0.9107(3) 0.0530(14) Uani 1 1 d . . . H38 H 0.4092 0.0452 0.9395 0.064 Uiso 1 1 calc R . . C39 C 0.4460(5) 0.1162(4) 0.8370(3) 0.0483(13) Uani 1 1 d . . . H39 H 0.4333 0.0705 0.8152 0.058 Uiso 1 1 calc R . . C40 C 0.4780(4) 0.2018(3) 0.7962(3) 0.0382(12) Uani 1 1 d . . . C41 C 0.7714(5) 0.4373(4) 0.6328(3) 0.0507(14) Uani 1 1 d . . . H41A H 0.7977 0.3918 0.6032 0.061 Uiso 1 1 calc R . . H41B H 0.8009 0.4962 0.6084 0.061 Uiso 1 1 calc R . . C42 C 0.8322(5) 0.3907(4) 0.7057(3) 0.0448(13) Uani 1 1 d . . . C43 C 0.8569(5) 0.3526(4) 0.8237(3) 0.0439(12) Uani 1 1 d . . . C44 C 0.8419(6) 0.3397(4) 0.8979(3) 0.0590(15) Uani 1 1 d . . . H44 H 0.7652 0.3718 0.9174 0.071 Uiso 1 1 calc R . . C45 C 0.9467(6) 0.2765(5) 0.9422(4) 0.0712(18) Uani 1 1 d . . . H45 H 0.9405 0.2665 0.9925 0.085 Uiso 1 1 calc R . . C46 C 1.0598(6) 0.2282(5) 0.9129(4) 0.0729(19) Uani 1 1 d . . . H46 H 1.1276 0.1861 0.9442 0.088 Uiso 1 1 calc R . . C47 C 1.0750(6) 0.2401(4) 0.8404(4) 0.0651(17) Uani 1 1 d . . . H47 H 1.1515 0.2073 0.8211 0.078 Uiso 1 1 calc R . . C48 C 0.9722(5) 0.3030(4) 0.7961(3) 0.0479(13) Uani 1 1 d . . . C49 C 0.5547(4) 0.5471(3) 0.9340(2) 0.0308(10) Uani 1 1 d . . . C50 C 0.4721(4) 0.4869(3) 0.9351(3) 0.0389(12) Uani 1 1 d . . . H50 H 0.4525 0.4778 0.8915 0.047 Uiso 1 1 calc R . . C51 C 0.5816(4) 0.5600(3) 0.9994(3) 0.0392(12) Uani 1 1 d . . . H51 H 0.6361 0.6004 0.9996 0.047 Uiso 1 1 calc R . . C52 C 0.6092(4) 0.6010(3) 0.8635(3) 0.0319(10) Uani 1 1 d . . . N1 N 0.6966(4) 0.8238(3) 0.6507(2) 0.0459(11) Uani 1 1 d . . . N2 N 0.7620(3) 0.8835(3) 0.7680(2) 0.0375(9) Uani 1 1 d . . . N3 N 0.8010(4) 1.0216(3) 0.6957(3) 0.0476(11) Uani 1 1 d . . . H3 H 0.8139 1.0649 0.6560 0.057 Uiso 1 1 calc R . . N4 N 0.5058(3) 0.8404(3) 0.7553(2) 0.0371(9) Uani 1 1 d . . . N5 N 0.3539(4) 0.9541(3) 0.6819(2) 0.0506(11) Uani 1 1 d . . . H5A H 0.3146 0.9924 0.6420 0.061 Uiso 1 1 calc R . . N6 N 0.8485(4) 0.6715(3) 0.7456(3) 0.0585(13) Uani 1 1 d . . . N7 N 0.9740(5) 0.6076(4) 0.6650(4) 0.0871(19) Uani 1 1 d . . . H7A H 1.0025 0.5979 0.6237 0.104 Uiso 1 1 calc R . . N8 N 0.6263(4) 0.4638(3) 0.6406(2) 0.0389(10) Uani 1 1 d . . . N9 N 0.4380(4) 0.5876(3) 0.6994(2) 0.0424(10) Uani 1 1 d . . . N10 N 0.3515(4) 0.6888(3) 0.5944(2) 0.0512(11) Uani 1 1 d . . . H10 H 0.3397 0.7142 0.5480 0.061 Uiso 1 1 calc R . . N11 N 0.5309(3) 0.3501(3) 0.7733(2) 0.0334(9) Uani 1 1 d . . . N12 N 0.5038(4) 0.2378(3) 0.7225(2) 0.0423(10) Uani 1 1 d . . . H12A H 0.5013 0.2097 0.6893 0.051 Uiso 1 1 calc R . . N13 N 0.7720(4) 0.4071(3) 0.7658(2) 0.0421(10) Uani 1 1 d . . . N14 N 0.9528(4) 0.3289(3) 0.7209(3) 0.0537(12) Uani 1 1 d . . . H14A H 1.0082 0.3088 0.6897 0.064 Uiso 1 1 calc R . . O1 O 0.6537(3) 0.6715(2) 0.86647(16) 0.0368(7) Uani 1 1 d . . . O2 O 0.6062(3) 0.5775(2) 0.80639(18) 0.0437(8) Uani 1 1 d . . . Cl1 Cl 0.5029(3) 0.8503(3) 0.4419(3) 0.0493(8) Uani 0.73 1 d PD A 1 O3 O 0.5087(7) 0.7485(4) 0.4592(4) 0.076(2) Uani 0.73 1 d PD A 1 O4 O 0.4748(11) 0.8951(9) 0.3654(5) 0.062(3) Uani 0.73 1 d PD A 1 O5 O 0.6196(5) 0.8688(5) 0.4587(3) 0.0878(19) Uani 0.73 1 d PD A 1 O6 O 0.3964(8) 0.8962(8) 0.4827(6) 0.065(4) Uani 0.73 1 d PD A 1 Cl1' Cl 0.4561(12) 0.8377(9) 0.4462(8) 0.068(3) Uani 0.27 1 d PD B 2 O3' O 0.5713(18) 0.7731(14) 0.4906(11) 0.099(7) Uani 0.27 1 d PD B 2 O4' O 0.370(2) 0.7782(14) 0.4393(11) 0.134(8) Uani 0.27 1 d PD B 2 O5' O 0.502(3) 0.886(2) 0.3737(14) 0.074(11) Uani 0.27 1 d PD B 2 O6' O 0.387(2) 0.912(2) 0.482(2) 0.104(17) Uani 0.27 1 d PD B 2 Cl2 Cl 0.8167(2) 0.5972(2) 0.43105(13) 0.0602(7) Uani 0.74 1 d PD C 1 O7 O 0.9461(4) 0.5430(4) 0.4181(3) 0.0688(16) Uani 0.74 1 d PD C 1 O9 O 0.8142(5) 0.6281(4) 0.4954(3) 0.0598(16) Uani 0.74 1 d PD C 1 O8 O 0.7800(6) 0.6837(4) 0.3681(3) 0.114(3) Uani 0.74 1 d PD C 1 O10 O 0.7274(6) 0.5372(6) 0.4403(4) 0.101(3) Uani 0.74 1 d PD C 1 Cl2' Cl 0.7957(6) 0.5023(6) 0.4393(4) 0.071(2) Uani 0.26 1 d PD D 2 O8' O 0.7146(13) 0.4445(12) 0.4817(8) 0.089(5) Uani 0.26 1 d PD D 2 O9' O 0.7482(15) 0.5445(13) 0.3673(7) 0.118(8) Uani 0.26 1 d PD D 2 O7' O 0.9253(13) 0.4426(12) 0.4384(9) 0.126(8) Uani 0.26 1 d PD D 2 O10' O 0.7979(19) 0.5778(12) 0.4705(10) 0.100(9) Uani 0.26 1 d PD D 2 Cl3 Cl 0.0618(5) 0.8029(3) 0.4474(2) 0.0747(14) Uani 0.51 1 d PD E 1 O11 O -0.0248(16) 0.8790(12) 0.4676(11) 0.34(3) Uani 0.51 1 d PD E 1 O12 O 0.0172(17) 0.7961(12) 0.3841(6) 0.125(7) Uani 0.51 1 d PD E 1 O13 O 0.0665(14) 0.7169(10) 0.5020(7) 0.156(6) Uani 0.51 1 d PD E 1 O14 O 0.1832(10) 0.8189(9) 0.4373(6) 0.133(5) Uani 0.51 1 d PD E 1 Cl3' Cl -0.0039(7) 0.8610(6) 0.4392(4) 0.119(2) Uani 0.49 1 d PD E -1 O11' O 0.0625(19) 0.8125(12) 0.3896(9) 0.179(11) Uani 0.49 1 d PD E -1 O12' O 0.0566(15) 0.9302(10) 0.4435(8) 0.152(6) Uani 0.49 1 d PD E -1 O13' O -0.0043(12) 0.7924(11) 0.5064(6) 0.104(4) Uani 0.49 1 d PD E -1 O14' O -0.1318(14) 0.9048(12) 0.4161(10) 0.246(11) Uani 0.49 1 d PD E -1 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 0.0354(3) 0.0308(3) 0.0491(4) -0.0035(3) 0.0107(3) -0.0104(2) Cu2 0.0402(3) 0.0392(4) 0.0458(4) -0.0203(3) 0.0012(3) -0.0076(3) C1 0.055(3) 0.050(3) 0.041(3) -0.007(3) 0.015(2) -0.024(3) C2 0.039(3) 0.038(3) 0.044(3) -0.009(2) 0.005(2) -0.015(2) C3 0.028(2) 0.042(3) 0.052(4) -0.014(3) 0.006(2) -0.012(2) C4 0.054(3) 0.056(3) 0.055(4) -0.014(3) 0.008(3) -0.028(3) C5 0.058(3) 0.071(4) 0.063(4) -0.032(3) 0.009(3) -0.022(3) C6 0.048(3) 0.062(4) 0.083(5) -0.042(4) -0.002(3) -0.014(3) C7 0.044(3) 0.034(3) 0.085(5) -0.018(3) -0.003(3) -0.014(2) C8 0.031(2) 0.033(3) 0.060(4) -0.012(3) 0.001(2) -0.007(2) C9 0.069(4) 0.055(3) 0.040(3) -0.016(3) 0.000(3) -0.027(3) C10 0.046(3) 0.037(3) 0.044(3) -0.010(2) -0.004(2) -0.016(2) C11 0.033(2) 0.035(3) 0.049(3) -0.019(2) 0.003(2) -0.012(2) C12 0.042(3) 0.056(3) 0.049(4) -0.019(3) 0.005(2) -0.013(2) C13 0.057(4) 0.090(5) 0.074(5) -0.050(4) 0.023(3) -0.023(4) C14 0.048(4) 0.088(5) 0.116(7) -0.065(5) 0.018(4) -0.008(4) C15 0.039(3) 0.058(4) 0.103(6) -0.038(4) -0.009(3) 0.002(3) C16 0.042(3) 0.041(3) 0.065(4) -0.017(3) -0.006(3) -0.015(2) C17 0.081(4) 0.060(4) 0.088(5) -0.041(4) 0.040(4) -0.029(4) C18 0.059(4) 0.052(4) 0.098(6) -0.035(4) 0.041(4) -0.022(3) C19 0.047(3) 0.044(4) 0.122(6) -0.008(4) 0.011(4) -0.021(3) C20 0.037(3) 0.059(4) 0.147(7) 0.001(4) -0.002(4) -0.011(3) C21 0.074(5) 0.078(5) 0.151(8) 0.003(5) -0.012(5) -0.034(4) C22 0.055(4) 0.061(4) 0.181(9) -0.032(6) -0.007(5) -0.017(3) C23 0.082(5) 0.083(6) 0.148(8) -0.043(6) 0.012(5) -0.026(4) C24 0.042(4) 0.044(4) 0.153(8) -0.041(4) 0.028(4) -0.014(3) C25 0.055(3) 0.042(3) 0.039(3) -0.012(2) 0.010(2) -0.010(2) C26 0.046(3) 0.037(3) 0.042(3) -0.011(2) 0.002(2) -0.011(2) C27 0.031(2) 0.039(3) 0.051(3) -0.020(3) 0.007(2) -0.012(2) C28 0.044(3) 0.052(3) 0.058(4) -0.023(3) 0.006(3) -0.015(3) C29 0.041(3) 0.066(4) 0.072(4) -0.041(4) 0.015(3) -0.018(3) C30 0.036(3) 0.059(4) 0.091(5) -0.038(4) 0.002(3) -0.007(3) C31 0.048(3) 0.047(3) 0.076(5) -0.016(3) -0.002(3) -0.004(3) C32 0.039(3) 0.037(3) 0.059(4) -0.013(3) 0.002(3) -0.008(2) C33 0.076(4) 0.059(4) 0.038(3) -0.018(3) 0.001(3) -0.027(3) C34 0.040(3) 0.038(3) 0.042(3) -0.011(2) -0.005(2) -0.012(2) C35 0.030(2) 0.034(3) 0.038(3) -0.013(2) 0.002(2) -0.007(2) C36 0.050(3) 0.037(3) 0.040(3) -0.013(2) 0.002(2) -0.010(2) C37 0.054(3) 0.051(3) 0.045(3) -0.007(3) 0.008(3) -0.016(3) C38 0.054(3) 0.043(3) 0.057(4) -0.002(3) 0.002(3) -0.019(3) C39 0.052(3) 0.040(3) 0.057(4) -0.012(3) -0.007(3) -0.019(2) C40 0.029(2) 0.038(3) 0.049(3) -0.013(2) -0.004(2) -0.009(2) C41 0.046(3) 0.056(3) 0.047(4) -0.019(3) 0.014(3) -0.008(3) C42 0.042(3) 0.040(3) 0.050(4) -0.012(3) 0.007(3) -0.010(2) C43 0.044(3) 0.040(3) 0.050(4) -0.012(3) -0.003(3) -0.014(2) C44 0.057(3) 0.059(4) 0.065(4) -0.025(3) -0.006(3) -0.011(3) C45 0.077(4) 0.070(4) 0.066(4) -0.016(4) -0.020(4) -0.017(4) C46 0.057(4) 0.067(4) 0.085(6) -0.010(4) -0.027(4) -0.005(3) C47 0.048(3) 0.054(4) 0.086(5) -0.013(3) -0.008(3) -0.007(3) C48 0.040(3) 0.044(3) 0.059(4) -0.013(3) 0.002(3) -0.012(2) C49 0.036(2) 0.024(2) 0.031(3) -0.005(2) 0.000(2) -0.0077(19) C50 0.054(3) 0.041(3) 0.029(3) -0.013(2) 0.004(2) -0.022(2) C51 0.048(3) 0.040(3) 0.038(3) -0.013(2) 0.002(2) -0.023(2) C52 0.031(2) 0.031(3) 0.031(3) -0.007(2) 0.003(2) -0.007(2) N1 0.060(3) 0.041(2) 0.042(3) -0.018(2) 0.019(2) -0.020(2) N2 0.040(2) 0.034(2) 0.040(3) -0.008(2) 0.0033(18) -0.0161(18) N3 0.050(2) 0.031(2) 0.058(3) -0.002(2) 0.005(2) -0.0187(19) N4 0.041(2) 0.034(2) 0.036(3) -0.0073(19) 0.0020(18) -0.0138(18) N5 0.046(3) 0.051(3) 0.050(3) -0.004(2) -0.016(2) -0.011(2) N6 0.041(2) 0.030(2) 0.093(4) -0.007(2) 0.012(3) -0.005(2) N7 0.064(4) 0.065(4) 0.144(6) -0.053(4) 0.039(4) -0.023(3) N8 0.044(2) 0.033(2) 0.037(2) -0.0094(19) 0.0046(18) -0.0079(18) N9 0.044(2) 0.040(2) 0.046(3) -0.018(2) 0.002(2) -0.0095(19) N10 0.056(3) 0.048(3) 0.040(3) -0.009(2) 0.000(2) -0.004(2) N11 0.042(2) 0.030(2) 0.031(2) -0.0142(18) 0.0033(17) -0.0085(17) N12 0.053(2) 0.043(2) 0.039(3) -0.018(2) -0.002(2) -0.018(2) N13 0.042(2) 0.041(2) 0.043(3) -0.013(2) -0.004(2) -0.0082(19) N14 0.041(2) 0.043(3) 0.069(4) -0.015(2) 0.017(2) -0.005(2) O1 0.0457(18) 0.0305(17) 0.0381(19) -0.0085(14) 0.0022(14) -0.0183(15) O2 0.060(2) 0.044(2) 0.035(2) -0.0166(17) 0.0097(16) -0.0229(16) Cl1 0.0567(19) 0.0574(19) 0.0375(17) -0.0164(14) -0.0009(15) -0.0177(14) O3 0.101(6) 0.027(3) 0.076(5) -0.002(3) 0.023(4) 0.000(3) O4 0.101(7) 0.053(6) 0.037(6) -0.011(4) -0.013(5) -0.028(5) O5 0.075(4) 0.135(6) 0.069(4) -0.038(4) -0.010(3) -0.040(4) O6 0.090(9) 0.050(5) 0.055(8) -0.027(5) 0.007(6) -0.005(5) Cl1' 0.108(10) 0.052(5) 0.046(5) -0.013(3) -0.004(7) -0.025(6) O3' 0.120(18) 0.082(15) 0.088(16) -0.037(13) 0.003(13) 0.002(14) O4' 0.14(2) 0.131(19) 0.13(2) -0.041(16) 0.005(16) -0.037(17) O5' 0.092(18) 0.064(19) 0.06(2) -0.011(15) 0.008(14) -0.019(14) O6' 0.11(3) 0.10(3) 0.11(3) -0.03(2) 0.00(2) -0.02(2) Cl2 0.0422(11) 0.0797(17) 0.0498(16) -0.0180(13) 0.0058(11) -0.0032(11) O7 0.043(3) 0.092(4) 0.057(4) -0.022(3) 0.011(2) 0.004(3) O9 0.056(3) 0.079(4) 0.044(4) -0.023(3) 0.013(3) -0.014(3) O8 0.099(5) 0.133(6) 0.063(4) -0.030(4) -0.011(4) 0.054(4) O10 0.073(6) 0.152(8) 0.096(7) -0.049(6) 0.001(5) -0.043(6) Cl2' 0.056(4) 0.090(5) 0.057(5) -0.024(4) 0.000(4) 0.003(4) O8' 0.080(12) 0.120(16) 0.063(12) -0.027(11) 0.012(9) -0.024(11) O9' 0.117(16) 0.16(2) 0.059(14) -0.026(13) 0.015(12) -0.016(14) O7' 0.090(15) 0.17(2) 0.110(18) -0.066(18) 0.009(12) 0.004(16) O10' 0.099(19) 0.10(2) 0.10(2) -0.025(19) 0.010(17) -0.025(15) Cl3 0.111(4) 0.085(3) 0.054(3) -0.039(3) 0.030(3) -0.058(3) O11 0.35(6) 0.33(5) 0.34(7) -0.13(5) 0.01(4) -0.07(5) O12 0.157(14) 0.156(15) 0.080(11) -0.066(11) -0.005(9) -0.034(12) O13 0.179(15) 0.151(14) 0.133(13) -0.005(12) -0.002(11) -0.071(12) O14 0.118(9) 0.150(11) 0.117(10) 0.024(8) -0.003(7) -0.079(9) Cl3' 0.107(5) 0.157(7) 0.086(4) -0.003(5) 0.020(4) -0.064(5) O11' 0.19(3) 0.17(2) 0.17(3) -0.05(2) 0.026(17) -0.053(17) O12' 0.155(14) 0.164(15) 0.152(14) -0.045(11) 0.021(11) -0.073(13) O13' 0.109(10) 0.122(11) 0.073(8) -0.014(8) 0.030(7) -0.043(9) O14' 0.25(3) 0.24(2) 0.24(3) -0.07(2) -0.03(2) -0.05(2) _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 N6 1.945(4) . ? Cu1 N4 1.957(4) . ? Cu1 O1 1.984(3) . ? Cu1 N2 2.160(4) . ? Cu1 N1 2.187(4) . ? Cu2 N13 1.957(4) . ? Cu2 N9 1.970(4) . ? Cu2 O2 1.987(3) . ? Cu2 N11 2.136(4) . ? Cu2 N8 2.238(4) . ? C1 C2 1.485(7) . ? C1 N1 1.487(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.306(6) . ? C2 N3 1.349(6) . ? C3 C4 1.382(7) . ? C3 N2 1.390(6) . ? C3 C8 1.393(6) . ? C4 C5 1.371(7) . ? C4 H4 0.9300 . ? C5 C6 1.396(8) . ? C5 H5 0.9300 . ? C6 C7 1.372(8) . ? C6 H6 0.9300 . ? C7 C8 1.382(7) . ? C7 H7 0.9300 . ? C8 N3 1.386(6) . ? C9 C10 1.489(7) . ? C9 N1 1.502(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.315(6) . ? C10 N5 1.340(6) . ? C11 C12 1.382(7) . ? C11 C16 1.395(7) . ? C11 N4 1.399(6) . ? C12 C13 1.378(7) . ? C12 H12 0.9300 . ? C13 C14 1.396(9) . ? C13 H13 0.9300 . ? C14 C15 1.351(9) . ? C14 H14 0.9300 . ? C15 C16 1.404(8) . ? C15 H15 0.9300 . ? C16 N5 1.376(7) . ? C17 C18 1.456(9) . ? C17 N1 1.501(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.325(8) . ? C18 N7 1.342(7) . ? C19 N6 1.334(5) . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9300 . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 N7 1.321(7) . ? C25 N8 1.476(6) . ? C25 C26 1.498(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N9 1.326(6) . ? C26 N10 1.334(6) . ? C27 N9 1.387(6) . ? C27 C28 1.392(7) . ? C27 C32 1.393(7) . ? C28 C29 1.379(7) . ? C28 H28 0.9300 . ? C29 C30 1.381(8) . ? C29 H29 0.9300 . ? C30 C31 1.361(8) . ? C30 H30 0.9300 . ? C31 C32 1.392(7) . ? C31 H31 0.9300 . ? C32 N10 1.382(6) . ? C33 C34 1.473(7) . ? C33 N8 1.476(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N11 1.327(6) . ? C34 N12 1.354(6) . ? C35 C36 1.385(7) . ? C35 C40 1.405(6) . ? C35 N11 1.412(5) . ? C36 C37 1.376(7) . ? C36 H36 0.9300 . ? C37 C38 1.399(7) . ? C37 H37 0.9300 . ? C38 C39 1.361(7) . ? C38 H38 0.9300 . ? C39 C40 1.376(6) . ? C39 H39 0.9300 . ? C40 N12 1.382(6) . ? C41 C42 1.471(7) . ? C41 N8 1.480(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N13 1.322(6) . ? C42 N14 1.344(6) . ? C43 C44 1.375(7) . ? C43 N13 1.385(6) . ? C43 C48 1.390(7) . ? C44 C45 1.390(8) . ? C44 H44 0.9300 . ? C45 C46 1.381(9) . ? C45 H45 0.9300 . ? C46 C47 1.347(9) . ? C46 H46 0.9300 . ? C47 C48 1.375(7) . ? C47 H47 0.9300 . ? C48 N14 1.391(7) . ? C49 C51 1.383(6) . ? C49 C50 1.391(6) . ? C49 C52 1.500(6) . ? C50 C51 1.393(6) 2_667 ? C50 H50 0.9300 . ? C51 C50 1.393(6) 2_667 ? C51 H51 0.9300 . ? C52 O2 1.246(5) . ? C52 O1 1.260(5) . ? N3 H3 0.8600 . ? N5 H5A 0.8600 . ? N7 H7A 0.8600 . ? N10 H10 0.8600 . ? N12 H12A 0.8600 . ? N14 H14A 0.8600 . ? Cl1 O5 1.410(6) . ? Cl1 O3 1.413(6) . ? Cl1 O4 1.433(7) . ? Cl1 O6 1.444(7) . ? Cl1' O4' 1.455(16) . ? Cl1' O6' 1.458(17) . ? Cl1' O5' 1.465(17) . ? Cl1' O3' 1.471(17) . ? Cl2 O10 1.419(6) . ? Cl2 O7 1.425(4) . ? Cl2 O9 1.430(5) . ? Cl2 O8 1.451(5) . ? Cl2' O9' 1.403(12) . ? Cl2' O8' 1.404(12) . ? Cl2' O10' 1.412(12) . ? Cl2' O7' 1.413(12) . ? Cl3 Cl3' 0.921(8) . ? Cl3 O11' 1.073(18) . ? Cl3 O13' 1.267(12) . ? Cl3 O14 1.351(8) . ? Cl3 O13 1.366(9) . ? Cl3 O11 1.369(11) . ? Cl3 O12 1.374(10) . ? Cl3 O12' 1.829(14) . ? O11 Cl3' 0.67(2) . ? O11 O13' 1.234(17) . ? O11 O12' 1.26(2) . ? O11 O14' 1.46(3) . ? O12 O11' 0.62(3) . ? O12 Cl3' 1.582(18) . ? O13 O13' 1.178(16) . ? O13 Cl3' 2.058(13) . ? O14 O11' 1.66(2) . ? O14 Cl3' 1.903(12) . ? Cl3' O12' 1.360(12) . ? Cl3' O14' 1.375(12) . ? Cl3' O13' 1.376(11) . ? Cl3' O11' 1.385(12) . ? 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 N6 Cu1 N4 155.9(2) . . ? N6 Cu1 O1 97.86(17) . . ? N4 Cu1 O1 94.72(14) . . ? N6 Cu1 N2 99.71(16) . . ? N4 Cu1 N2 92.56(15) . . ? O1 Cu1 N2 117.37(14) . . ? N6 Cu1 N1 79.19(19) . . ? N4 Cu1 N1 82.29(16) . . ? O1 Cu1 N1 161.23(14) . . ? N2 Cu1 N1 81.34(15) . . ? N13 Cu2 N9 155.77(17) . . ? N13 Cu2 O2 95.12(15) . . ? N9 Cu2 O2 88.66(15) . . ? N13 Cu2 N11 88.60(15) . . ? N9 Cu2 N11 104.25(15) . . ? O2 Cu2 N11 138.70(14) . . ? N13 Cu2 N8 81.40(16) . . ? N9 Cu2 N8 80.32(15) . . ? O2 Cu2 N8 139.66(13) . . ? N11 Cu2 N8 81.60(14) . . ? C2 C1 N1 111.0(4) . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? N1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 N3 112.1(5) . . ? N2 C2 C1 124.4(4) . . ? N3 C2 C1 123.4(4) . . ? C4 C3 N2 131.4(4) . . ? C4 C3 C8 119.1(5) . . ? N2 C3 C8 109.6(5) . . ? C5 C4 C3 118.8(5) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.0(6) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 121.5(5) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 116.6(5) . . ? C6 C7 H7 121.7 . . ? C8 C7 H7 121.7 . . ? C7 C8 N3 132.6(5) . . ? C7 C8 C3 123.0(5) . . ? N3 C8 C3 104.4(4) . . ? C10 C9 N1 108.5(4) . . ? C10 C9 H9A 110.0 . . ? N1 C9 H9A 110.0 . . ? C10 C9 H9B 110.0 . . ? N1 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N4 C10 N5 112.1(4) . . ? N4 C10 C9 121.9(4) . . ? N5 C10 C9 125.8(5) . . ? C12 C11 C16 121.5(5) . . ? C12 C11 N4 130.7(4) . . ? C16 C11 N4 107.8(4) . . ? C13 C12 C11 117.3(5) . . ? C13 C12 H12 121.3 . . ? C11 C12 H12 121.3 . . ? C12 C13 C14 120.5(6) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 123.4(6) . . ? C15 C14 H14 118.3 . . ? C13 C14 H14 118.3 . . ? C14 C15 C16 116.3(6) . . ? C14 C15 H15 121.9 . . ? C16 C15 H15 121.9 . . ? N5 C16 C11 106.0(4) . . ? N5 C16 C15 133.0(5) . . ? C11 C16 C15 121.0(6) . . ? C18 C17 N1 106.2(5) . . ? C18 C17 H17A 110.5 . . ? N1 C17 H17A 110.5 . . ? C18 C17 H17B 110.5 . . ? N1 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? N6 C18 N7 111.5(7) . . ? N6 C18 C17 121.2(5) . . ? N7 C18 C17 127.2(7) . . ? N6 C19 C20 130.3(4) . . ? N6 C19 C24 109.7(4) . . ? C20 C19 C24 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? N7 C24 C23 134.0(4) . . ? N7 C24 C19 106.0(4) . . ? C23 C24 C19 120.0 . . ? N8 C25 C26 108.2(4) . . ? N8 C25 H25A 110.1 . . ? C26 C25 H25A 110.1 . . ? N8 C25 H25B 110.1 . . ? C26 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? N9 C26 N10 111.9(4) . . ? N9 C26 C25 122.7(4) . . ? N10 C26 C25 125.2(5) . . ? N9 C27 C28 132.0(5) . . ? N9 C27 C32 108.9(4) . . ? C28 C27 C32 119.2(4) . . ? C29 C28 C27 118.1(5) . . ? C29 C28 H28 121.0 . . ? C27 C28 H28 121.0 . . ? C28 C29 C30 121.0(5) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C31 C30 C29 122.8(5) . . ? C31 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? C30 C31 C32 116.0(5) . . ? C30 C31 H31 122.0 . . ? C32 C31 H31 122.0 . . ? N10 C32 C31 131.8(5) . . ? N10 C32 C27 105.2(4) . . ? C31 C32 C27 123.0(5) . . ? C34 C33 N8 113.9(4) . . ? C34 C33 H33A 108.8 . . ? N8 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? N8 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? N11 C34 N12 112.8(4) . . ? N11 C34 C33 125.0(4) . . ? N12 C34 C33 122.3(5) . . ? C36 C35 C40 119.9(4) . . ? C36 C35 N11 131.0(4) . . ? C40 C35 N11 109.1(4) . . ? C37 C36 C35 118.0(5) . . ? C37 C36 H36 121.0 . . ? C35 C36 H36 121.0 . . ? C36 C37 C38 120.8(5) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C39 C38 C37 122.0(5) . . ? C39 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? C38 C39 C40 117.2(5) . . ? C38 C39 H39 121.4 . . ? C40 C39 H39 121.4 . . ? C39 C40 N12 132.6(5) . . ? C39 C40 C35 122.0(5) . . ? N12 C40 C35 105.3(4) . . ? C42 C41 N8 109.6(4) . . ? C42 C41 H41A 109.7 . . ? N8 C41 H41A 109.7 . . ? C42 C41 H41B 109.7 . . ? N8 C41 H41B 109.7 . . ? H41A C41 H41B 108.2 . . ? N13 C42 N14 111.0(5) . . ? N13 C42 C41 122.4(4) . . ? N14 C42 C41 126.6(5) . . ? C44 C43 N13 131.4(5) . . ? C44 C43 C48 120.3(5) . . ? N13 C43 C48 108.3(5) . . ? C43 C44 C45 116.9(6) . . ? C43 C44 H44 121.6 . . ? C45 C44 H44 121.6 . . ? C46 C45 C44 121.3(6) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C47 C46 C45 122.2(6) . . ? C47 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C46 C47 C48 116.9(6) . . ? C46 C47 H47 121.6 . . ? C48 C47 H47 121.6 . . ? C47 C48 C43 122.5(6) . . ? C47 C48 N14 132.0(5) . . ? C43 C48 N14 105.5(4) . . ? C51 C49 C50 118.6(4) . . ? C51 C49 C52 120.0(4) . . ? C50 C49 C52 121.4(4) . . ? C49 C50 C51 120.8(4) . 2_667 ? C49 C50 H50 119.6 . . ? C51 C50 H50 119.6 2_667 . ? C49 C51 C50 120.6(4) . 2_667 ? C49 C51 H51 119.7 . . ? C50 C51 H51 119.7 2_667 . ? O2 C52 O1 123.7(4) . . ? O2 C52 C49 120.7(4) . . ? O1 C52 C49 115.5(4) . . ? C1 N1 C17 109.9(4) . . ? C1 N1 C9 112.5(4) . . ? C17 N1 C9 113.2(5) . . ? C1 N1 Cu1 108.3(3) . . ? C17 N1 Cu1 105.6(3) . . ? C9 N1 Cu1 107.0(3) . . ? C2 N2 C3 105.9(4) . . ? C2 N2 Cu1 109.5(3) . . ? C3 N2 Cu1 143.0(3) . . ? C2 N3 C8 108.1(4) . . ? C2 N3 H3 125.9 . . ? C8 N3 H3 125.9 . . ? C10 N4 C11 106.2(4) . . ? C10 N4 Cu1 115.1(3) . . ? C11 N4 Cu1 137.6(3) . . ? C10 N5 C16 107.8(4) . . ? C10 N5 H5A 126.1 . . ? C16 N5 H5A 126.1 . . ? C18 N6 C19 105.2(5) . . ? C18 N6 Cu1 115.7(4) . . ? C19 N6 Cu1 139.0(4) . . ? C24 N7 C18 107.7(6) . . ? C24 N7 H7A 126.2 . . ? C18 N7 H7A 126.2 . . ? C33 N8 C25 110.4(4) . . ? C33 N8 C41 113.5(4) . . ? C25 N8 C41 113.8(4) . . ? C33 N8 Cu2 107.0(3) . . ? C25 N8 Cu2 106.5(3) . . ? C41 N8 Cu2 105.1(3) . . ? C26 N9 C27 105.9(4) . . ? C26 N9 Cu2 114.8(3) . . ? C27 N9 Cu2 138.2(4) . . ? C26 N10 C32 108.2(4) . . ? C26 N10 H10 125.9 . . ? C32 N10 H10 125.9 . . ? C34 N11 C35 104.8(4) . . ? C34 N11 Cu2 110.3(3) . . ? C35 N11 Cu2 144.7(3) . . ? C34 N12 C40 107.9(4) . . ? C34 N12 H12A 126.0 . . ? C40 N12 H12A 126.0 . . ? C42 N13 C43 107.2(4) . . ? C42 N13 Cu2 114.8(3) . . ? C43 N13 Cu2 137.5(4) . . ? C42 N14 C48 108.0(4) . . ? C42 N14 H14A 126.0 . . ? C48 N14 H14A 126.0 . . ? C52 O1 Cu1 114.3(3) . . ? C52 O2 Cu2 152.9(3) . . ? O5 Cl1 O3 113.4(4) . . ? O5 Cl1 O4 109.6(4) . . ? O3 Cl1 O4 108.7(4) . . ? O5 Cl1 O6 108.0(4) . . ? O3 Cl1 O6 108.8(4) . . ? O4 Cl1 O6 108.1(4) . . ? O4' Cl1' O6' 110.4(6) . . ? O4' Cl1' O5' 109.9(6) . . ? O6' Cl1' O5' 109.8(6) . . ? O4' Cl1' O3' 109.3(6) . . ? O6' Cl1' O3' 109.1(6) . . ? O5' Cl1' O3' 108.4(6) . . ? O10 Cl2 O7 109.9(4) . . ? O10 Cl2 O9 109.0(3) . . ? O7 Cl2 O9 110.5(3) . . ? O10 Cl2 O8 110.5(4) . . ? O7 Cl2 O8 107.6(3) . . ? O9 Cl2 O8 109.4(3) . . ? O9' Cl2' O8' 110.1(6) . . ? O9' Cl2' O10' 109.7(6) . . ? O8' Cl2' O10' 109.3(6) . . ? O9' Cl2' O7' 109.3(6) . . ? O8' Cl2' O7' 109.6(6) . . ? O10' Cl2' O7' 108.7(6) . . ? Cl3' Cl3 O11' 87.7(10) . . ? O14 Cl3 O13 109.2(6) . . ? O14 Cl3 O11 110.2(6) . . ? O13 Cl3 O11 108.6(6) . . ? O14 Cl3 O12 110.6(6) . . ? O13 Cl3 O12 109.4(6) . . ? O11 Cl3 O12 108.7(6) . . ? Cl3' Cl3 O12' 45.9(6) . . ? O11' Cl3 O12' 97.9(9) . . ? O13' Cl3 O12' 91.3(7) . . ? O12' Cl3' O14' 110.5(6) . . ? O12' Cl3' O13' 110.5(6) . . ? O14' Cl3' O13' 108.8(6) . . ? O11 Cl3' O11' 167.8(19) . . ? O12' Cl3' O11' 109.6(6) . . ? O14' Cl3' O11' 108.7(6) . . ? O13' Cl3' O11' 108.7(6) . . ? O12' Cl3' O12 130.8(10) . . ? O12' Cl3' O13 118.7(8) . . ? O14' Cl3' O13 125.6(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 27.2(7) . . . . ? N1 C1 C2 N3 -157.5(4) . . . . ? N2 C3 C4 C5 179.8(5) . . . . ? C8 C3 C4 C5 0.6(7) . . . . ? C3 C4 C5 C6 0.5(8) . . . . ? C4 C5 C6 C7 -1.0(8) . . . . ? C5 C6 C7 C8 0.3(8) . . . . ? C6 C7 C8 N3 179.9(5) . . . . ? C6 C7 C8 C3 0.8(7) . . . . ? C4 C3 C8 C7 -1.3(7) . . . . ? N2 C3 C8 C7 179.3(4) . . . . ? C4 C3 C8 N3 179.4(4) . . . . ? N2 C3 C8 N3 0.1(5) . . . . ? N1 C9 C10 N4 -24.8(6) . . . . ? N1 C9 C10 N5 159.7(4) . . . . ? C16 C11 C12 C13 -0.8(7) . . . . ? N4 C11 C12 C13 -178.2(5) . . . . ? C11 C12 C13 C14 0.4(8) . . . . ? C12 C13 C14 C15 -0.3(10) . . . . ? C13 C14 C15 C16 0.6(9) . . . . ? C12 C11 C16 N5 -178.1(4) . . . . ? N4 C11 C16 N5 -0.1(5) . . . . ? C12 C11 C16 C15 1.1(7) . . . . ? N4 C11 C16 C15 179.1(4) . . . . ? C14 C15 C16 N5 178.0(6) . . . . ? C14 C15 C16 C11 -1.0(8) . . . . ? N1 C17 C18 N6 25.6(7) . . . . ? N1 C17 C18 N7 -158.0(5) . . . . ? N6 C19 C20 C21 -179.5(4) . . . . ? C24 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 N7 179.9(5) . . . . ? C22 C23 C24 C19 0.0 . . . . ? N6 C19 C24 N7 -0.3(4) . . . . ? C20 C19 C24 N7 -179.9(4) . . . . ? N6 C19 C24 C23 179.6(3) . . . . ? C20 C19 C24 C23 0.0 . . . . ? N8 C25 C26 N9 18.5(6) . . . . ? N8 C25 C26 N10 -167.8(4) . . . . ? N9 C27 C28 C29 177.5(5) . . . . ? C32 C27 C28 C29 -2.4(7) . . . . ? C27 C28 C29 C30 1.9(7) . . . . ? C28 C29 C30 C31 -0.8(8) . . . . ? C29 C30 C31 C32 0.2(8) . . . . ? C30 C31 C32 N10 -178.2(5) . . . . ? C30 C31 C32 C27 -0.8(8) . . . . ? N9 C27 C32 N10 0.0(5) . . . . ? C28 C27 C32 N10 180.0(4) . . . . ? N9 C27 C32 C31 -178.0(4) . . . . ? C28 C27 C32 C31 2.0(7) . . . . ? N8 C33 C34 N11 14.0(7) . . . . ? N8 C33 C34 N12 -166.0(4) . . . . ? C40 C35 C36 C37 -2.7(7) . . . . ? N11 C35 C36 C37 -179.8(4) . . . . ? C35 C36 C37 C38 1.3(7) . . . . ? C36 C37 C38 C39 1.1(8) . . . . ? C37 C38 C39 C40 -2.1(8) . . . . ? C38 C39 C40 N12 176.6(5) . . . . ? C38 C39 C40 C35 0.6(7) . . . . ? C36 C35 C40 C39 1.8(7) . . . . ? N11 C35 C40 C39 179.5(4) . . . . ? C36 C35 C40 N12 -175.1(4) . . . . ? N11 C35 C40 N12 2.5(5) . . . . ? N8 C41 C42 N13 -24.7(7) . . . . ? N8 C41 C42 N14 156.3(4) . . . . ? N13 C43 C44 C45 178.0(5) . . . . ? C48 C43 C44 C45 0.5(8) . . . . ? C43 C44 C45 C46 -0.7(9) . . . . ? C44 C45 C46 C47 0.4(10) . . . . ? C45 C46 C47 C48 0.0(9) . . . . ? C46 C47 C48 C43 -0.2(8) . . . . ? C46 C47 C48 N14 -177.0(6) . . . . ? C44 C43 C48 C47 -0.1(8) . . . . ? N13 C43 C48 C47 -178.1(5) . . . . ? C44 C43 C48 N14 177.5(5) . . . . ? N13 C43 C48 N14 -0.5(5) . . . . ? C51 C49 C50 C51 -0.4(7) . . . 2_667 ? C52 C49 C50 C51 -177.7(4) . . . 2_667 ? C50 C49 C51 C50 0.4(7) . . . 2_667 ? C52 C49 C51 C50 177.7(4) . . . 2_667 ? C51 C49 C52 O2 167.1(4) . . . . ? C50 C49 C52 O2 -15.7(6) . . . . ? C51 C49 C52 O1 -14.6(6) . . . . ? C50 C49 C52 O1 162.6(4) . . . . ? C2 C1 N1 C17 -137.9(5) . . . . ? C2 C1 N1 C9 95.0(5) . . . . ? C2 C1 N1 Cu1 -23.0(5) . . . . ? C18 C17 N1 C1 81.8(5) . . . . ? C18 C17 N1 C9 -151.5(4) . . . . ? C18 C17 N1 Cu1 -34.8(5) . . . . ? C10 C9 N1 C1 -96.3(5) . . . . ? C10 C9 N1 C17 138.4(4) . . . . ? C10 C9 N1 Cu1 22.5(4) . . . . ? N6 Cu1 N1 C1 -88.4(3) . . . . ? N4 Cu1 N1 C1 107.1(3) . . . . ? O1 Cu1 N1 C1 -170.9(4) . . . . ? N2 Cu1 N1 C1 13.3(3) . . . . ? N6 Cu1 N1 C17 29.3(3) . . . . ? N4 Cu1 N1 C17 -135.2(4) . . . . ? O1 Cu1 N1 C17 -53.3(6) . . . . ? N2 Cu1 N1 C17 131.0(4) . . . . ? N6 Cu1 N1 C9 150.1(3) . . . . ? N4 Cu1 N1 C9 -14.4(3) . . . . ? O1 Cu1 N1 C9 67.6(5) . . . . ? N2 Cu1 N1 C9 -108.2(3) . . . . ? N3 C2 N2 C3 0.5(5) . . . . ? C1 C2 N2 C3 176.3(4) . . . . ? N3 C2 N2 Cu1 169.5(3) . . . . ? C1 C2 N2 Cu1 -14.7(5) . . . . ? C4 C3 N2 C2 -179.6(5) . . . . ? C8 C3 N2 C2 -0.4(5) . . . . ? C4 C3 N2 Cu1 17.9(8) . . . . ? C8 C3 N2 Cu1 -162.9(4) . . . . ? N6 Cu1 N2 C2 77.1(3) . . . . ? N4 Cu1 N2 C2 -82.1(3) . . . . ? O1 Cu1 N2 C2 -178.8(3) . . . . ? N1 Cu1 N2 C2 -0.3(3) . . . . ? N6 Cu1 N2 C3 -120.8(5) . . . . ? N4 Cu1 N2 C3 80.0(5) . . . . ? O1 Cu1 N2 C3 -16.6(5) . . . . ? N1 Cu1 N2 C3 161.8(5) . . . . ? N2 C2 N3 C8 -0.5(5) . . . . ? C1 C2 N3 C8 -176.3(4) . . . . ? C7 C8 N3 C2 -178.9(5) . . . . ? C3 C8 N3 C2 0.3(5) . . . . ? N5 C10 N4 C11 -1.2(5) . . . . ? C9 C10 N4 C11 -177.2(4) . . . . ? N5 C10 N4 Cu1 -171.5(3) . . . . ? C9 C10 N4 Cu1 12.5(6) . . . . ? C12 C11 N4 C10 178.5(5) . . . . ? C16 C11 N4 C10 0.8(5) . . . . ? C12 C11 N4 Cu1 -14.6(8) . . . . ? C16 C11 N4 Cu1 167.7(3) . . . . ? N6 Cu1 N4 C10 -38.0(6) . . . . ? O1 Cu1 N4 C10 -159.4(3) . . . . ? N2 Cu1 N4 C10 82.9(3) . . . . ? N1 Cu1 N4 C10 2.0(3) . . . . ? N6 Cu1 N4 C11 155.9(4) . . . . ? O1 Cu1 N4 C11 34.5(4) . . . . ? N2 Cu1 N4 C11 -83.2(4) . . . . ? N1 Cu1 N4 C11 -164.1(4) . . . . ? N4 C10 N5 C16 1.1(5) . . . . ? C9 C10 N5 C16 176.9(5) . . . . ? C11 C16 N5 C10 -0.6(5) . . . . ? C15 C16 N5 C10 -179.6(5) . . . . ? N7 C18 N6 C19 -0.9(6) . . . . ? C17 C18 N6 C19 176.1(5) . . . . ? N7 C18 N6 Cu1 -176.6(3) . . . . ? C17 C18 N6 Cu1 0.3(7) . . . . ? C20 C19 N6 C18 -179.7(4) . . . . ? C24 C19 N6 C18 0.7(4) . . . . ? C20 C19 N6 Cu1 -5.5(7) . . . . ? C24 C19 N6 Cu1 174.9(4) . . . . ? N4 Cu1 N6 C18 23.2(6) . . . . ? O1 Cu1 N6 C18 144.0(4) . . . . ? N2 Cu1 N6 C18 -96.4(4) . . . . ? N1 Cu1 N6 C18 -17.2(4) . . . . ? N4 Cu1 N6 C19 -150.6(4) . . . . ? O1 Cu1 N6 C19 -29.8(5) . . . . ? N2 Cu1 N6 C19 89.9(5) . . . . ? N1 Cu1 N6 C19 169.0(5) . . . . ? C23 C24 N7 C18 179.9(3) . . . . ? C19 C24 N7 C18 -0.2(5) . . . . ? N6 C18 N7 C24 0.7(6) . . . . ? C17 C18 N7 C24 -176.0(5) . . . . ? C34 C33 N8 C25 -131.6(4) . . . . ? C34 C33 N8 C41 99.3(5) . . . . ? C34 C33 N8 Cu2 -16.0(5) . . . . ? C26 C25 N8 C33 89.0(5) . . . . ? C26 C25 N8 C41 -142.1(4) . . . . ? C26 C25 N8 Cu2 -26.8(4) . . . . ? C42 C41 N8 C33 -90.3(5) . . . . ? C42 C41 N8 C25 142.4(4) . . . . ? C42 C41 N8 Cu2 26.2(5) . . . . ? N13 Cu2 N8 C33 101.6(3) . . . . ? N9 Cu2 N8 C33 -94.4(3) . . . . ? O2 Cu2 N8 C33 -170.6(3) . . . . ? N11 Cu2 N8 C33 11.7(3) . . . . ? N13 Cu2 N8 C25 -140.3(3) . . . . ? N9 Cu2 N8 C25 23.7(3) . . . . ? O2 Cu2 N8 C25 -52.6(4) . . . . ? N11 Cu2 N8 C25 129.8(3) . . . . ? N13 Cu2 N8 C41 -19.3(3) . . . . ? N9 Cu2 N8 C41 144.7(3) . . . . ? O2 Cu2 N8 C41 68.5(3) . . . . ? N11 Cu2 N8 C41 -109.1(3) . . . . ? N10 C26 N9 C27 -1.3(5) . . . . ? C25 C26 N9 C27 173.2(4) . . . . ? N10 C26 N9 Cu2 -171.6(3) . . . . ? C25 C26 N9 Cu2 2.9(6) . . . . ? C28 C27 N9 C26 -179.2(5) . . . . ? C32 C27 N9 C26 0.8(5) . . . . ? C28 C27 N9 Cu2 -12.4(8) . . . . ? C32 C27 N9 Cu2 167.6(4) . . . . ? N13 Cu2 N9 C26 26.7(6) . . . . ? O2 Cu2 N9 C26 126.2(3) . . . . ? N11 Cu2 N9 C26 -93.5(3) . . . . ? N8 Cu2 N9 C26 -14.8(3) . . . . ? N13 Cu2 N9 C27 -139.3(5) . . . . ? O2 Cu2 N9 C27 -39.7(5) . . . . ? N11 Cu2 N9 C27 100.6(5) . . . . ? N8 Cu2 N9 C27 179.2(5) . . . . ? N9 C26 N10 C32 1.3(6) . . . . ? C25 C26 N10 C32 -173.0(5) . . . . ? C31 C32 N10 C26 177.0(5) . . . . ? C27 C32 N10 C26 -0.7(5) . . . . ? N12 C34 N11 C35 1.1(5) . . . . ? C33 C34 N11 C35 -178.9(4) . . . . ? N12 C34 N11 Cu2 177.2(3) . . . . ? C33 C34 N11 Cu2 -2.8(6) . . . . ? C36 C35 N11 C34 175.0(5) . . . . ? C40 C35 N11 C34 -2.3(5) . . . . ? C36 C35 N11 Cu2 1.4(8) . . . . ? C40 C35 N11 Cu2 -175.9(4) . . . . ? N13 Cu2 N11 C34 -86.8(3) . . . . ? N9 Cu2 N11 C34 72.4(3) . . . . ? O2 Cu2 N11 C34 177.0(3) . . . . ? N8 Cu2 N11 C34 -5.3(3) . . . . ? N13 Cu2 N11 C35 86.6(5) . . . . ? N9 Cu2 N11 C35 -114.2(5) . . . . ? O2 Cu2 N11 C35 -9.6(6) . . . . ? N8 Cu2 N11 C35 168.1(5) . . . . ? N11 C34 N12 C40 0.5(5) . . . . ? C33 C34 N12 C40 -179.5(4) . . . . ? C39 C40 N12 C34 -178.3(5) . . . . ? C35 C40 N12 C34 -1.8(5) . . . . ? N14 C42 N13 C43 -0.5(5) . . . . ? C41 C42 N13 C43 -179.6(4) . . . . ? N14 C42 N13 Cu2 -173.9(3) . . . . ? C41 C42 N13 Cu2 7.0(6) . . . . ? C44 C43 N13 C42 -177.0(5) . . . . ? C48 C43 N13 C42 0.7(5) . . . . ? C44 C43 N13 Cu2 -6.0(9) . . . . ? C48 C43 N13 Cu2 171.7(4) . . . . ? N9 Cu2 N13 C42 -33.8(6) . . . . ? O2 Cu2 N13 C42 -131.9(3) . . . . ? N11 Cu2 N13 C42 89.3(3) . . . . ? N8 Cu2 N13 C42 7.6(3) . . . . ? N9 Cu2 N13 C43 155.7(4) . . . . ? O2 Cu2 N13 C43 57.5(5) . . . . ? N11 Cu2 N13 C43 -81.3(5) . . . . ? N8 Cu2 N13 C43 -163.0(5) . . . . ? N13 C42 N14 C48 0.2(6) . . . . ? C41 C42 N14 C48 179.2(5) . . . . ? C47 C48 N14 C42 177.4(5) . . . . ? C43 C48 N14 C42 0.2(5) . . . . ? O2 C52 O1 Cu1 11.2(5) . . . . ? C49 C52 O1 Cu1 -167.0(3) . . . . ? N6 Cu1 O1 C52 -75.4(3) . . . . ? N4 Cu1 O1 C52 84.0(3) . . . . ? N2 Cu1 O1 C52 179.3(3) . . . . ? N1 Cu1 O1 C52 4.1(6) . . . . ? O1 C52 O2 Cu2 164.2(4) . . . . ? C49 C52 O2 Cu2 -17.6(9) . . . . ? N13 Cu2 O2 C52 -82.6(7) . . . . ? N9 Cu2 O2 C52 121.4(7) . . . . ? N11 Cu2 O2 C52 11.1(8) . . . . ? N8 Cu2 O2 C52 -165.3(6) . . . . ? O11' Cl3 O11 Cl3' 6(2) . . . . ? O13' Cl3 O11 Cl3' -139(3) . . . . ? O14 Cl3 O11 Cl3' 100(2) . . . . ? O13 Cl3 O11 Cl3' -141(2) . . . . ? O12 Cl3 O11 Cl3' -22(2) . . . . ? O12' Cl3 O11 Cl3' 82(2) . . . . ? Cl3' Cl3 O11 O13' 139(3) . . . . ? O11' Cl3 O11 O13' 144.3(14) . . . . ? O14 Cl3 O11 O13' -121.4(11) . . . . ? O13 Cl3 O11 O13' -1.8(12) . . . . ? O12 Cl3 O11 O13' 117.2(12) . . . . ? O12' Cl3 O11 O13' -139.3(17) . . . . ? Cl3' Cl3 O11 O12' -82(2) . . . . ? O11' Cl3 O11 O12' -76.4(16) . . . . ? O13' Cl3 O11 O12' 139.3(17) . . . . ? O14 Cl3 O11 O12' 17.9(14) . . . . ? O13 Cl3 O11 O12' 137.5(12) . . . . ? O12 Cl3 O11 O12' -103.4(13) . . . . ? Cl3' Cl3 O11 O14' 29.6(16) . . . . ? O11' Cl3 O11 O14' 35.1(16) . . . . ? O13' Cl3 O11 O14' -109.2(14) . . . . ? O14 Cl3 O11 O14' 129.4(11) . . . . ? O13 Cl3 O11 O14' -111.0(12) . . . . ? O12 Cl3 O11 O14' 8.0(14) . . . . ? O12' Cl3 O11 O14' 111.5(17) . . . . ? Cl3' Cl3 O12 O11' 96(3) . . . . ? O13' Cl3 O12 O11' 165(3) . . . . ? O14 Cl3 O12 O11' -16(3) . . . . ? O13 Cl3 O12 O11' -137(3) . . . . ? O11 Cl3 O12 O11' 105(3) . . . . ? O12' Cl3 O12 O11' 58(3) . . . . ? O11' Cl3 O12 Cl3' -96(3) . . . . ? O13' Cl3 O12 Cl3' 69.8(10) . . . . ? O14 Cl3 O12 Cl3' -112.0(9) . . . . ? O13 Cl3 O12 Cl3' 127.7(9) . . . . ? O11 Cl3 O12 Cl3' 9.2(10) . . . . ? O12' Cl3 O12 Cl3' -37.3(7) . . . . ? Cl3' Cl3 O13 O13' -18.3(13) . . . . ? O11' Cl3 O13 O13' -138.4(16) . . . . ? O14 Cl3 O13 O13' 122.1(11) . . . . ? O11 Cl3 O13 O13' 1.9(13) . . . . ? O12 Cl3 O13 O13' -116.7(12) . . . . ? O12' Cl3 O13 O13' 43.4(14) . . . . ? O11' Cl3 O13 Cl3' -120.1(18) . . . . ? O13' Cl3 O13 Cl3' 18.3(13) . . . . ? O14 Cl3 O13 Cl3' 140.4(14) . . . . ? O11 Cl3 O13 Cl3' 20.2(14) . . . . ? O12 Cl3 O13 Cl3' -98.4(14) . . . . ? O12' Cl3 O13 Cl3' 61.7(12) . . . . ? Cl3' Cl3 O14 O11' -85.8(10) . . . . ? O13' Cl3 O14 O11' -174.9(14) . . . . ? O13 Cl3 O14 O11' 127.5(13) . . . . ? O11 Cl3 O14 O11' -113.2(14) . . . . ? O12 Cl3 O14 O11' 7.0(14) . . . . ? O12' Cl3 O14 O11' -100.1(9) . . . . ? O11' Cl3 O14 Cl3' 85.8(10) . . . . ? O13' Cl3 O14 Cl3' -89.1(13) . . . . ? O13 Cl3 O14 Cl3' -146.7(12) . . . . ? O11 Cl3 O14 Cl3' -27.5(12) . . . . ? O12 Cl3 O14 Cl3' 92.8(12) . . . . ? O12' Cl3 O14 Cl3' -14.3(8) . . . . ? O13' O11 Cl3' Cl3 -34(2) . . . . ? O12' O11 Cl3' Cl3 95.4(16) . . . . ? O14' O11 Cl3' Cl3 -148.9(14) . . . . ? O13' O11 Cl3' O12' -129.4(15) . . . . ? Cl3 O11 Cl3' O12' -95.4(16) . . . . ? O14' O11 Cl3' O12' 115.7(10) . . . . ? O13' O11 Cl3' O14' 114.9(11) . . . . ? O12' O11 Cl3' O14' -115.7(10) . . . . ? Cl3 O11 Cl3' O14' 148.9(14) . . . . ? O12' O11 Cl3' O13' 129.4(15) . . . . ? Cl3 O11 Cl3' O13' 34(2) . . . . ? O14' O11 Cl3' O13' -114.9(11) . . . . ? O13' O11 Cl3' O11' -53(9) . . . . ? O12' O11 Cl3' O11' 76(9) . . . . ? Cl3 O11 Cl3' O11' -19(8) . . . . ? O14' O11 Cl3' O11' -168(9) . . . . ? O13' O11 Cl3' O12 44(6) . . . . ? O12' O11 Cl3' O12 173(5) . . . . ? Cl3 O11 Cl3' O12 78(5) . . . . ? O14' O11 Cl3' O12 -71(5) . . . . ? O13' O11 Cl3' O14 -78.6(13) . . . . ? O12' O11 Cl3' O14 50.8(14) . . . . ? Cl3 O11 Cl3' O14 -44.6(11) . . . . ? O14' O11 Cl3' O14 166.5(9) . . . . ? O13' O11 Cl3' O13 -10.4(13) . . . . ? O12' O11 Cl3' O13 119.0(9) . . . . ? Cl3 O11 Cl3' O13 23.7(12) . . . . ? O14' O11 Cl3' O13 -125.3(8) . . . . ? O11' Cl3 Cl3' O11 -175(2) . . . . ? O13' Cl3 Cl3' O11 34(2) . . . . ? O14 Cl3 Cl3' O11 -90(2) . . . . ? O13 Cl3 Cl3' O11 49(3) . . . . ? O12 Cl3 Cl3' O11 160(2) . . . . ? O12' Cl3 Cl3' O11 -72(2) . . . . ? O11' Cl3 Cl3' O12' -103.3(10) . . . . ? O13' Cl3 Cl3' O12' 105.7(7) . . . . ? O14 Cl3 Cl3' O12' -18.7(11) . . . . ? O13 Cl3 Cl3' O12' 120.7(11) . . . . ? O11 Cl3 Cl3' O12' 72(2) . . . . ? O12 Cl3 Cl3' O12' -128.8(10) . . . . ? O11' Cl3 Cl3' O14' 65.3(16) . . . . ? O13' Cl3 Cl3' O14' -85.6(15) . . . . ? O14 Cl3 Cl3' O14' 149.9(14) . . . . ? O13 Cl3 Cl3' O14' -70.6(19) . . . . ? O11 Cl3 Cl3' O14' -120(3) . . . . ? O12 Cl3 Cl3' O14' 39.8(15) . . . . ? O12' Cl3 Cl3' O14' 168.7(17) . . . . ? O11' Cl3 Cl3' O13' 151.0(12) . . . . ? O14 Cl3 Cl3' O13' -124.4(10) . . . . ? O13 Cl3 Cl3' O13' 15.0(10) . . . . ? O11 Cl3 Cl3' O13' -34(2) . . . . ? O12 Cl3 Cl3' O13' 125.5(9) . . . . ? O12' Cl3 Cl3' O13' -105.7(7) . . . . ? O13' Cl3 Cl3' O11' -151.0(12) . . . . ? O14 Cl3 Cl3' O11' 84.6(13) . . . . ? O13 Cl3 Cl3' O11' -136.0(16) . . . . ? O11 Cl3 Cl3' O11' 175(2) . . . . ? O12 Cl3 Cl3' O11' -25.5(14) . . . . ? O12' Cl3 Cl3' O11' 103.3(10) . . . . ? O11' Cl3 Cl3' O12 25.5(14) . . . . ? O13' Cl3 Cl3' O12 -125.5(9) . . . . ? O14 Cl3 Cl3' O12 110.1(7) . . . . ? O13 Cl3 Cl3' O12 -110.5(10) . . . . ? O11 Cl3 Cl3' O12 -160(2) . . . . ? O12' Cl3 Cl3' O12 128.8(10) . . . . ? O11' Cl3 Cl3' O14 -84.6(13) . . . . ? O13' Cl3 Cl3' O14 124.4(10) . . . . ? O13 Cl3 Cl3' O14 139.4(13) . . . . ? O11 Cl3 Cl3' O14 90(2) . . . . ? O12 Cl3 Cl3' O14 -110.1(7) . . . . ? O12' Cl3 Cl3' O14 18.7(11) . . . . ? O11' Cl3 Cl3' O13 136.0(16) . . . . ? O13' Cl3 Cl3' O13 -15.0(10) . . . . ? O14 Cl3 Cl3' O13 -139.4(13) . . . . ? O11 Cl3 Cl3' O13 -49(3) . . . . ? O12 Cl3 Cl3' O13 110.5(10) . . . . ? O12' Cl3 Cl3' O13 -120.7(11) . . . . ? O11' O12 Cl3' O11 -147(6) . . . . ? Cl3 O12 Cl3' O11 -88(6) . . . . ? O11' O12 Cl3' Cl3 -59(3) . . . . ? O11' O12 Cl3' O12' 24(3) . . . . ? Cl3 O12 Cl3' O12' 83.9(11) . . . . ? O11' O12 Cl3' O14' 143(3) . . . . ? Cl3 O12 Cl3' O14' -157.8(8) . . . . ? O11' O12 Cl3' O13' -108(3) . . . . ? Cl3 O12 Cl3' O13' -48.3(7) . . . . ? Cl3 O12 Cl3' O11' 59(3) . . . . ? O11' O12 Cl3' O14 -21(3) . . . . ? Cl3 O12 Cl3' O14 38.8(5) . . . . ? O11' O12 Cl3' O13 -90(3) . . . . ? Cl3 O12 Cl3' O13 -30.9(5) . . . . ? Cl3 O14 Cl3' O11 109(2) . . . . ? O11' O14 Cl3' O11 173.8(19) . . . . ? O11' O14 Cl3' Cl3 64.9(12) . . . . ? Cl3 O14 Cl3' O12' 160.2(12) . . . . ? O11' O14 Cl3' O12' -134.9(8) . . . . ? Cl3 O14 Cl3' O14' -116(3) . . . . ? O11' O14 Cl3' O14' -51(3) . . . . ? Cl3 O14 Cl3' O13' 47.5(10) . . . . ? O11' O14 Cl3' O13' 112.4(7) . . . . ? Cl3 O14 Cl3' O11' -64.9(12) . . . . ? Cl3 O14 Cl3' O12 -55.7(9) . . . . ? O11' O14 Cl3' O12 9.2(12) . . . . ? Cl3 O14 Cl3' O13 21.8(8) . . . . ? O11' O14 Cl3' O13 86.7(10) . . . . ? O13' O13 Cl3' O11 17(2) . . . . ? Cl3 O13 Cl3' O11 -138(2) . . . . ? O13' O13 Cl3' Cl3 155.0(17) . . . . ? O13' O13 Cl3' O12' 83.7(12) . . . . ? Cl3 O13 Cl3' O12' -71.3(13) . . . . ? O13' O13 Cl3' O14' -68.2(15) . . . . ? Cl3 O13 Cl3' O14' 136.8(15) . . . . ? Cl3 O13 Cl3' O13' -155.0(17) . . . . ? O13' O13 Cl3' O11' -171.3(13) . . . . ? Cl3 O13 Cl3' O11' 33.7(13) . . . . ? O13' O13 Cl3' O12 -147.8(14) . . . . ? Cl3 O13 Cl3' O12 57.2(12) . . . . ? O13' O13 Cl3' O14 127.6(13) . . . . ? Cl3 O13 Cl3' O14 -27.4(10) . . . . ? Cl3' O12 O11' Cl3 41.6(11) . . . . ? Cl3 O12 O11' Cl3' -41.6(11) . . . . ? Cl3 O12 O11' O14 31(6) . . . . ? Cl3' O12 O11' O14 73(7) . . . . ? Cl3' Cl3 O11' O12 -83(3) . . . . ? O13' Cl3 O11' O12 -23(5) . . . . ? O14 Cl3 O11' O12 165(3) . . . . ? O13 Cl3 O11' O12 54(4) . . . . ? O11 Cl3 O11' O12 -85(3) . . . . ? O12' Cl3 O11' O12 -128(3) . . . . ? O13' Cl3 O11' Cl3' 59.8(18) . . . . ? O14 Cl3 O11' Cl3' -112.7(8) . . . . ? O13 Cl3 O11' Cl3' 136.4(14) . . . . ? O11 Cl3 O11' Cl3' -2.4(10) . . . . ? O12 Cl3 O11' Cl3' 83(3) . . . . ? O12' Cl3 O11' Cl3' -44.9(6) . . . . ? Cl3' Cl3 O11' O14 112.7(8) . . . . ? O13' Cl3 O11' O14 172(2) . . . . ? O13 Cl3 O11' O14 -111.0(11) . . . . ? O11 Cl3 O11' O14 110.3(8) . . . . ? O12 Cl3 O11' O14 -165(3) . . . . ? O12' Cl3 O11' O14 67.8(7) . . . . ? O11 Cl3' O11' O12 128(9) . . . . ? Cl3 Cl3' O11' O12 106(3) . . . . ? O12' Cl3' O11' O12 -161(3) . . . . ? O14' Cl3' O11' O12 -40(3) . . . . ? O13' Cl3' O11' O12 79(3) . . . . ? O14 Cl3' O11' O12 156(3) . . . . ? O13 Cl3' O11' O12 84(2) . . . . ? O11 Cl3' O11' Cl3 22(9) . . . . ? O12' Cl3' O11' Cl3 93.6(11) . . . . ? O14' Cl3' O11' Cl3 -145.5(11) . . . . ? O13' Cl3' O11' Cl3 -27.3(11) . . . . ? O12 Cl3' O11' Cl3 -106(3) . . . . ? O14 Cl3' O11' Cl3 50.2(9) . . . . ? O13 Cl3' O11' Cl3 -22.3(8) . . . . ? O11 Cl3' O11' O14 -28(9) . . . . ? Cl3 Cl3' O11' O14 -50.2(9) . . . . ? O12' Cl3' O11' O14 43.5(9) . . . . ? O14' Cl3' O11' O14 164.3(8) . . . . ? O13' Cl3' O11' O14 -77.4(8) . . . . ? O12 Cl3' O11' O14 -156(3) . . . . ? O13 Cl3' O11' O14 -72.4(7) . . . . ? Cl3 O14 O11' O12 -38(7) . . . . ? Cl3' O14 O11' O12 -77(7) . . . . ? Cl3' O14 O11' Cl3 -39.0(6) . . . . ? Cl3 O14 O11' Cl3' 39.0(6) . . . . ? O13' O11 O12' Cl3' 81.4(17) . . . . ? Cl3 O11 O12' Cl3' 36.3(10) . . . . ? O14' O11 O12' Cl3' -65.2(19) . . . . ? Cl3' O11 O12' Cl3 -36.3(10) . . . . ? O13' O11 O12' Cl3 45.1(14) . . . . ? O14' O11 O12' Cl3 -101.5(16) . . . . ? Cl3 Cl3' O12' O11 -114(2) . . . . ? O14' Cl3' O12' O11 72.8(19) . . . . ? O13' Cl3' O12' O11 -47.6(18) . . . . ? O11' Cl3' O12' O11 -167(2) . . . . ? O12 Cl3' O12' O11 -177(2) . . . . ? O14 Cl3' O12' O11 -127.6(19) . . . . ? O13 Cl3' O12' O11 -83.1(17) . . . . ? O11 Cl3' O12' Cl3 114(2) . . . . ? O14' Cl3' O12' Cl3 -172.9(11) . . . . ? O13' Cl3' O12' Cl3 66.7(8) . . . . ? O11' Cl3' O12' Cl3 -53.1(10) . . . . ? O12 Cl3' O12' Cl3 -62.9(12) . . . . ? O14 Cl3' O12' Cl3 -13.3(8) . . . . ? O13 Cl3' O12' Cl3 31.2(7) . . . . ? Cl3' Cl3 O12' O11 36.6(16) . . . . ? O11' Cl3 O12' O11 115.6(18) . . . . ? O13' Cl3 O12' O11 -32.6(14) . . . . ? O14 Cl3 O12' O11 -161.9(14) . . . . ? O13 Cl3 O12' O11 -65.8(15) . . . . ? O12 Cl3 O12' O11 93.8(12) . . . . ? O11' Cl3 O12' Cl3' 79.0(11) . . . . ? O13' Cl3 O12' Cl3' -69.2(9) . . . . ? O14 Cl3 O12' Cl3' 161.4(11) . . . . ? O13 Cl3 O12' Cl3' -102.5(14) . . . . ? O11 Cl3 O12' Cl3' -36.6(16) . . . . ? O12 Cl3 O12' Cl3' 57.2(12) . . . . ? Cl3 O13 O13' O11 -2.8(19) . . . . ? Cl3' O13 O13' O11 -12.9(17) . . . . ? Cl3' O13 O13' Cl3 -10.1(7) . . . . ? Cl3 O13 O13' Cl3' 10.1(7) . . . . ? Cl3' O11 O13' O13 26(3) . . . . ? O12' O11 O13' O13 -54(3) . . . . ? Cl3 O11 O13' O13 2.8(19) . . . . ? O14' O11 O13' O13 93(2) . . . . ? Cl3' O11 O13' Cl3 23.1(16) . . . . ? O12' O11 O13' Cl3 -56.6(19) . . . . ? O14' O11 O13' Cl3 89.8(14) . . . . ? O12' O11 O13' Cl3' -80(2) . . . . ? Cl3 O11 O13' Cl3' -23.1(16) . . . . ? O14' O11 O13' Cl3' 67(2) . . . . ? Cl3' Cl3 O13' O13 165.1(10) . . . . ? O11' Cl3 O13' O13 102(2) . . . . ? O14 Cl3 O13' O13 -87.1(11) . . . . ? O11 Cl3 O13' O13 -177.8(15) . . . . ? O12 Cl3 O13' O13 90.7(10) . . . . ? O12' Cl3 O13' O13 -151.2(10) . . . . ? Cl3' Cl3 O13' O11 -17.1(14) . . . . ? O11' Cl3 O13' O11 -80(3) . . . . ? O14 Cl3 O13' O11 90.7(10) . . . . ? O13 Cl3 O13' O11 177.8(15) . . . . ? O12 Cl3 O13' O11 -91.4(11) . . . . ? O12' Cl3 O13' O11 26.7(12) . . . . ? O11' Cl3 O13' Cl3' -62.8(19) . . . . ? O14 Cl3 O13' Cl3' 107.8(11) . . . . ? O13 Cl3 O13' Cl3' -165.1(10) . . . . ? O11 Cl3 O13' Cl3' 17.1(14) . . . . ? O12 Cl3 O13' Cl3' -74.3(12) . . . . ? O12' Cl3 O13' Cl3' 43.8(6) . . . . ? O11 Cl3' O13' O13 -161(2) . . . . ? Cl3 Cl3' O13' O13 -14.5(10) . . . . ? O12' Cl3' O13' O13 -111.5(12) . . . . ? O14' Cl3' O13' O13 127.1(13) . . . . ? O11' Cl3' O13' O13 8.9(14) . . . . ? O12 Cl3' O13' O13 31.8(13) . . . . ? O14 Cl3' O13' O13 -47.3(11) . . . . ? Cl3 Cl3' O13' O11 146(2) . . . . ? O12' Cl3' O13' O11 49(2) . . . . ? O14' Cl3' O13' O11 -72(2) . . . . ? O11' Cl3' O13' O11 170(2) . . . . ? O12 Cl3' O13' O11 -167(2) . . . . ? O14 Cl3' O13' O11 113.6(19) . . . . ? O13 Cl3' O13' O11 161(2) . . . . ? O11 Cl3' O13' Cl3 -146(2) . . . . ? O12' Cl3' O13' Cl3 -97.0(10) . . . . ? O14' Cl3' O13' Cl3 141.6(11) . . . . ? O11' Cl3' O13' Cl3 23.4(10) . . . . ? O12 Cl3' O13' Cl3 46.3(9) . . . . ? O14 Cl3' O13' Cl3 -32.8(7) . . . . ? O13 Cl3' O13' Cl3 14.5(10) . . . . ? Cl3 Cl3' O14' O11 129(3) . . . . ? O12' Cl3' O14' O11 -62.3(17) . . . . ? O13' Cl3' O14' O11 59.1(17) . . . . ? O11' Cl3' O14' O11 177.3(19) . . . . ? O12 Cl3' O14' O11 163(2) . . . . ? O14 Cl3' O14' O11 -138(3) . . . . ? O13 Cl3' O14' O11 91.5(17) . . . . ? O13' O11 O14' Cl3' -78.1(15) . . . . ? O12' O11 O14' Cl3' 74.2(18) . . . . ? Cl3 O11 O14' Cl3' -18.2(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O14 0.86 2.07 2.923(10) 171.5 2_676 N5 H5A O5 0.86 2.55 3.183(8) 130.9 2_676 C1 H1B O6 0.97 2.40 3.344(13) 163.2 2_676 N7 H7A O7 0.86 2.35 2.998(8) 132.6 2_766 N14 H14A O8 0.86 2.42 3.159(7) 144.0 2_766 N12 H12A O4 0.86 2.05 2.885(12) 162.3 2_666 N14 H14A O12 0.86 2.45 3.046(13) 126.8 2_666 C33 H33A O10 0.97 2.36 3.317(9) 168.1 2_666 N10 H10 O3 0.86 2.40 2.986(7) 125.4 . C25 H25B O9 0.97 2.45 3.312(7) 148.4 . C41 H41B O9 0.97 2.45 3.319(8) 148.4 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.231 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.096 _vrf_PLAT430_8b ; PROBLEM: Short Inter D...A Contact O13 .. O7' .. 2.25 Ang. RESPONSE: This is due to the disorder of these perchlorate anions. ; # END data_9a _database_code_depnum_ccdc_archive 'CCDC 788595' #TrackingRef '- crystallographic CIF data 1-9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C106 H88 Cu4 N28 O8, 3(C10 H4 O8), 8(H2 O)' _chemical_formula_sum 'C136 H116 Cu4 N28 O40' _chemical_formula_weight 3036.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7676(9) _cell_length_b 14.0064(12) _cell_length_c 22.4703(19) _cell_angle_alpha 85.789(2) _cell_angle_beta 82.405(1) _cell_angle_gamma 72.247(2) _cell_volume 3197.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 2309 _cell_measurement_theta_min 1.26 _cell_measurement_theta_max 18.16 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1564 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo k\a' _diffrn_radiation_source 'fine focus sealed Siemens Mo tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex CCD area-detector' _diffrn_measurement_method '0.3\% wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30789 _diffrn_reflns_av_R_equivalents 0.1258 _diffrn_reflns_av_sigmaI/netI 0.2268 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11188 _reflns_number_gt 4021 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART,(Version 5.628)2001' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+,(Version 6.45)2001 ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material PLATON _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^)+(0.0822P)^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 11188 _refine_ls_number_parameters 1017 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1940 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.1888 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 0.80 _refine_ls_restrained_S_all 0.80 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.13259(9) -0.13136(6) 0.77020(4) 0.0651(3) Uani 1 1 d . . . Cu2 Cu 0.21289(16) 0.14038(11) 0.7965(2) 0.0398(8) Uani 0.717(10) 1 d P . . Cu2' Cu 0.2022(3) 0.1444(2) 0.8337(6) 0.039(2) Uani 0.283(10) 1 d P . . N1 N 0.1727(5) -0.1945(4) 0.6815(2) 0.0490(15) Uani 1 1 d . . . N2 N -0.0071(6) -0.0333(4) 0.7310(3) 0.0629(17) Uani 1 1 d . B . N3 N -0.0967(7) 0.0223(5) 0.6474(3) 0.0764(19) Uani 1 1 d . . . H3 H -0.1067 0.0287 0.6098 0.092 Uiso 1 1 calc R . . N4 N 0.3151(5) -0.2110(4) 0.7756(2) 0.0438(14) Uani 1 1 d . B . N5 N 0.4923(6) -0.3253(4) 0.7357(3) 0.0595(16) Uani 1 1 d . . . H5A H 0.5464 -0.3639 0.7096 0.071 Uiso 1 1 calc R . . N6 N 0.0614(5) -0.2578(4) 0.7933(2) 0.0583(17) Uani 1 1 d . B . N7 N 0.0409(5) -0.3957(4) 0.7566(3) 0.0602(16) Uani 1 1 d . . . H7A H 0.0415 -0.4383 0.7308 0.072 Uiso 1 1 calc R . . N8 N 0.1893(5) 0.1982(4) 0.7082(2) 0.0558(16) Uani 1 1 d . . . N9 N 0.0253(5) 0.2256(4) 0.8138(3) 0.0510(15) Uani 1 1 d . B . N10 N -0.1484(5) 0.3207(4) 0.7733(2) 0.0519(15) Uani 1 1 d . . . H10 H -0.1972 0.3520 0.7464 0.062 Uiso 1 1 calc R . . N11 N 0.3679(5) 0.0483(4) 0.7542(4) 0.069(2) Uani 1 1 d . B . N12 N 0.4749(7) -0.0188(5) 0.6696(4) 0.099(3) Uani 1 1 d . . . H12A H 0.4961 -0.0306 0.6320 0.119 Uiso 1 1 calc R . . N13 N 0.2745(5) 0.2667(4) 0.8073(2) 0.0453(14) Uani 1 1 d . B . N14 N 0.3006(5) 0.4029(4) 0.7574(2) 0.0440(14) Uani 1 1 d . . . H14A H 0.3052 0.4456 0.7283 0.053 Uiso 1 1 calc R . . C1 C 0.1213(7) -0.1096(5) 0.6383(3) 0.060(2) Uani 1 1 d . . . H1A H 0.1872 -0.0762 0.6247 0.072 Uiso 1 1 calc R B . H1B H 0.0968 -0.1339 0.6035 0.072 Uiso 1 1 calc R . . C2 C 0.0051(8) -0.0400(5) 0.6714(4) 0.064(2) Uani 1 1 d . B . C3 C -0.1848(9) 0.0757(6) 0.6932(5) 0.085(3) Uani 1 1 d . . . C4 C -0.3064(9) 0.1495(7) 0.6924(6) 0.103(3) Uani 1 1 d . . . H4 H -0.3437 0.1737 0.6572 0.124 Uiso 1 1 calc R . . C5 C -0.3658(10) 0.1830(9) 0.7479(8) 0.129(5) Uani 1 1 d . . . H5 H -0.4471 0.2319 0.7500 0.155 Uiso 1 1 calc R . . C6 C -0.3115(11) 0.1480(7) 0.8018(6) 0.118(5) Uani 1 1 d . . . H6 H -0.3561 0.1738 0.8383 0.142 Uiso 1 1 calc R . . C7 C -0.1922(8) 0.0756(6) 0.8003(4) 0.085(3) Uani 1 1 d . . . H7 H -0.1563 0.0507 0.8358 0.102 Uiso 1 1 calc R . . C8 C -0.1266(8) 0.0402(5) 0.7465(4) 0.073(2) Uani 1 1 d . . . C9 C 0.3167(6) -0.2428(5) 0.6692(3) 0.057(2) Uani 1 1 d . . . H9A H 0.3339 -0.3063 0.6502 0.069 Uiso 1 1 calc R B . H9B H 0.3561 -0.2000 0.6422 0.069 Uiso 1 1 calc R . . C10 C 0.3736(7) -0.2594(5) 0.7261(3) 0.0513(19) Uani 1 1 d . B . C11 C 0.5099(8) -0.3190(6) 0.7944(3) 0.058(2) Uani 1 1 d . . . C12 C 0.6131(9) -0.3717(7) 0.8241(5) 0.088(3) Uani 1 1 d . . . H12 H 0.6873 -0.4173 0.8053 0.106 Uiso 1 1 calc R . . C13 C 0.5992(10) -0.3524(8) 0.8838(5) 0.101(3) Uani 1 1 d . . . H13 H 0.6667 -0.3870 0.9063 0.121 Uiso 1 1 calc R . . C14 C 0.4892(10) -0.2836(8) 0.9127(4) 0.092(3) Uani 1 1 d . . . H14 H 0.4848 -0.2733 0.9534 0.110 Uiso 1 1 calc R . . C15 C 0.3875(9) -0.2312(6) 0.8811(3) 0.072(2) Uani 1 1 d . . . H15 H 0.3138 -0.1848 0.8997 0.086 Uiso 1 1 calc R . . C16 C 0.3982(7) -0.2498(5) 0.8194(3) 0.0532(19) Uani 1 1 d . . . C17 C 0.0988(7) -0.2676(5) 0.6834(3) 0.058(2) Uani 1 1 d . . . H17A H 0.1487 -0.3228 0.6581 0.070 Uiso 1 1 calc R B . H17B H 0.0166 -0.2356 0.6669 0.070 Uiso 1 1 calc R . . C18 C 0.0699(6) -0.3085(5) 0.7453(3) 0.0489(19) Uani 1 1 d . B . C19 C 0.0096(6) -0.4026(6) 0.8189(4) 0.062(2) Uani 1 1 d . . . C20 C -0.0243(7) -0.4756(6) 0.8550(4) 0.076(2) Uani 1 1 d . . . H20 H -0.0309 -0.5339 0.8401 0.091 Uiso 1 1 calc R . . C21 C -0.0487(8) -0.4554(8) 0.9171(4) 0.087(3) Uani 1 1 d . . . H21 H -0.0749 -0.5014 0.9438 0.105 Uiso 1 1 calc R . . C22 C -0.0354(8) -0.3722(7) 0.9390(4) 0.079(3) Uani 1 1 d . . . H22 H -0.0510 -0.3631 0.9802 0.094 Uiso 1 1 calc R . . C23 C 0.0003(7) -0.3016(6) 0.9017(3) 0.070(2) Uani 1 1 d . . . H23 H 0.0074 -0.2439 0.9171 0.084 Uiso 1 1 calc R . . C24 C 0.0256(6) -0.3167(6) 0.8414(3) 0.057(2) Uani 1 1 d . . . C25 C 0.0488(6) 0.2383(6) 0.7021(3) 0.068(2) Uani 1 1 d . . . H25A H 0.0195 0.1894 0.6839 0.081 Uiso 1 1 calc R B . H25B H 0.0324 0.2986 0.6765 0.081 Uiso 1 1 calc R . . C26 C -0.0240(7) 0.2615(5) 0.7631(3) 0.0471(17) Uani 1 1 d . B . C27 C -0.1846(7) 0.3229(5) 0.8346(3) 0.0484(18) Uani 1 1 d . . . C28 C -0.3013(8) 0.3722(6) 0.8700(3) 0.074(2) Uani 1 1 d . . . H28 H -0.3747 0.4131 0.8533 0.089 Uiso 1 1 calc R . . C29 C -0.2999(10) 0.3560(7) 0.9307(4) 0.092(3) Uani 1 1 d . . . H29 H -0.3761 0.3844 0.9559 0.111 Uiso 1 1 calc R . . C30 C -0.1893(12) 0.2988(8) 0.9560(4) 0.096(3) Uani 1 1 d . . . H30 H -0.1933 0.2911 0.9976 0.115 Uiso 1 1 calc R . . C31 C -0.0748(9) 0.2537(6) 0.9220(3) 0.076(2) Uani 1 1 d . . . H31 H -0.0001 0.2172 0.9395 0.091 Uiso 1 1 calc R . . C32 C -0.0740(7) 0.2643(5) 0.8606(3) 0.0470(17) Uani 1 1 d . . . C33 C 0.2540(8) 0.1151(6) 0.6668(4) 0.082(3) Uani 1 1 d . . . H33A H 0.1930 0.0796 0.6599 0.099 Uiso 1 1 calc R B . H33B H 0.2861 0.1407 0.6285 0.099 Uiso 1 1 calc R . . C34 C 0.3560(12) 0.0529(7) 0.6947(4) 0.093(3) Uani 1 1 d . B . C35 C 0.5466(7) -0.0637(5) 0.7129(3) 0.074(2) Uani 1 1 d G . . C36 C 0.6660(7) -0.1385(5) 0.7136(4) 0.118(4) Uani 1 1 d G . . H36 H 0.7099 -0.1684 0.6781 0.142 Uiso 1 1 calc R . . C37 C 0.7199(5) -0.1684(4) 0.7673(5) 0.128(5) Uani 1 1 d G . . H37 H 0.7998 -0.2184 0.7677 0.154 Uiso 1 1 calc R . . C38 C 0.6543(8) -0.1236(6) 0.8204(3) 0.135(4) Uani 1 1 d G . . H38 H 0.6904 -0.1436 0.8563 0.162 Uiso 1 1 calc R . . C39 C 0.5349(8) -0.0488(6) 0.8197(3) 0.102(3) Uani 1 1 d G B . H39 H 0.4910 -0.0188 0.8552 0.123 Uiso 1 1 calc R . . C40 C 0.4810(5) -0.0189(4) 0.7660(4) 0.089(3) Uani 1 1 d G . . C41 C 0.2600(6) 0.2738(5) 0.6970(3) 0.0540(19) Uani 1 1 d . . . H41A H 0.2116 0.3283 0.6721 0.065 Uiso 1 1 calc R B . H41B H 0.3454 0.2437 0.6751 0.065 Uiso 1 1 calc R . . C42 C 0.2780(6) 0.3148(5) 0.7533(3) 0.0423(17) Uani 1 1 d . B . C43 C 0.3152(6) 0.4130(5) 0.8165(3) 0.0414(17) Uani 1 1 d . . . C44 C 0.3336(6) 0.4919(5) 0.8445(3) 0.0536(19) Uani 1 1 d . . . H44 H 0.3428 0.5492 0.8230 0.064 Uiso 1 1 calc R . . C45 C 0.3376(7) 0.4809(6) 0.9057(4) 0.072(2) Uani 1 1 d . . . H45 H 0.3515 0.5314 0.9262 0.086 Uiso 1 1 calc R . . C46 C 0.3213(7) 0.3960(7) 0.9374(3) 0.067(2) Uani 1 1 d . . . H46 H 0.3234 0.3914 0.9788 0.080 Uiso 1 1 calc R . . C47 C 0.3020(6) 0.3180(6) 0.9094(3) 0.062(2) Uani 1 1 d . . . H47 H 0.2927 0.2608 0.9308 0.075 Uiso 1 1 calc R . . C48 C 0.2972(6) 0.3290(5) 0.8474(3) 0.0435(17) Uani 1 1 d . . . C49 C 0.1153(16) -0.0179(11) 0.9494(6) 0.032(4) Uani 0.50 1 d P . . C50 C 0.0043(17) -0.0328(11) 0.9637(7) 0.034(4) Uani 0.50 1 d P . . H50 H -0.0337 -0.0497 0.9328 0.041 Uiso 0.50 1 calc PR . . C51 C 0.1745(13) 0.0065(10) 0.9963(6) 0.032(4) Uani 0.50 1 d PD . . C52 C 0.301(2) 0.0102(11) 0.9931(8) 0.038(6) Uani 0.50 1 d PD A 1 C53 C 0.1652(16) -0.0022(11) 0.8841(7) 0.035(4) Uani 0.50 1 d PD B 1 O1 O 0.1379(16) -0.0526(11) 0.8483(6) 0.048(4) Uani 0.50 1 d PD B 1 O2 O 0.2203(9) 0.0608(7) 0.8724(4) 0.033(2) Uani 0.50 1 d PD B 1 O3 O 0.3332(9) 0.0821(7) 1.0216(4) 0.070(3) Uani 0.50 1 d PD A 1 H3C H 0.4227 0.0747 1.0169 0.084 Uiso 0.50 1 d PR A 1 O4 O 0.4097(9) -0.0549(8) 0.9644(4) 0.054(3) Uani 0.50 1 d PD A 1 C49' C 0.0120(16) -0.0001(12) 0.9321(7) 0.035(4) Uani 0.50 1 d P . . C50' C -0.1034(13) -0.0184(8) 0.9461(5) 0.032(3) Uani 0.50 1 d P . . H50' H -0.1388 -0.0402 0.9160 0.038 Uiso 0.50 1 calc PR . . C51' C 0.0680(13) 0.0266(10) 0.9786(7) 0.032(3) Uani 0.50 1 d PD . . C52' C 0.1961(17) 0.0474(12) 0.9715(7) 0.063(6) Uani 0.50 1 d PD C 2 C53' C 0.0786(18) -0.0184(15) 0.8685(10) 0.036(6) Uani 0.50 1 d P B 2 O1' O 0.0576(13) -0.0849(10) 0.8446(5) 0.065(3) Uani 0.50 1 d P B 2 O2' O 0.1511(14) 0.0291(12) 0.8451(8) 0.096(5) Uani 0.50 1 d P B 2 O3' O 0.3056(15) -0.0279(15) 0.9828(9) 0.127(8) Uani 0.50 1 d PD C 2 H3' H 0.3663 -0.0046 0.9842 0.191 Uiso 0.50 1 calc PR C 2 O4' O 0.2169(13) 0.1191(11) 0.9438(10) 0.180(8) Uani 0.50 1 d PD C 2 C54 C 0.7354(6) 0.4018(5) 0.5254(3) 0.0403(16) Uani 1 1 d . . . C55 C 0.7041(6) 0.4381(5) 0.4690(3) 0.0472(18) Uani 1 1 d . . . H55 H 0.7345 0.3930 0.4382 0.057 Uiso 1 1 calc R . . C56 C 0.6324(6) 0.5344(5) 0.4532(3) 0.0422(17) Uani 1 1 d . . . C57 C 0.5885(6) 0.6056(5) 0.5006(3) 0.0468(18) Uani 1 1 d . . . C58 C 0.6222(6) 0.5693(5) 0.5576(3) 0.0447(17) Uani 1 1 d . . . H58 H 0.5962 0.6147 0.5883 0.054 Uiso 1 1 calc R . . C59 C 0.6913(6) 0.4709(5) 0.5723(3) 0.0414(17) Uani 1 1 d . . . C60 C 0.8138(7) 0.2939(6) 0.5285(4) 0.056(2) Uani 1 1 d . . . C61 C 0.6103(7) 0.5533(6) 0.3879(3) 0.0533(19) Uani 1 1 d . . . C62 C 0.5116(7) 0.7165(6) 0.4976(4) 0.057(2) Uani 1 1 d . . . C63 C 0.7109(6) 0.4530(6) 0.6383(3) 0.0512(19) Uani 1 1 d . . . C64 C 0.0756(8) 0.3966(8) 0.4882(4) 0.074(3) Uani 1 1 d . . . C65 C 0.0257(7) 0.4598(7) 0.4405(4) 0.065(2) Uani 1 1 d . . . C66 C 0.0502(9) 0.4379(9) 0.5439(5) 0.100(4) Uani 1 1 d . . . H66 H 0.0855 0.3955 0.5753 0.120 Uiso 1 1 calc R . . C67 C 0.1532(10) 0.2926(9) 0.4894(5) 0.090(3) Uani 1 1 d . . . C68 C 0.0375(9) 0.4395(8) 0.3772(7) 0.103(4) Uani 1 1 d . . . O5 O 0.8500(5) 0.2495(3) 0.5778(2) 0.0705(15) Uani 1 1 d . . . H5B H 0.8008 0.3079 0.6158 0.085 Uiso 1 1 d R . . O6 O 0.8401(6) 0.2459(4) 0.4826(2) 0.0897(18) Uani 1 1 d . . . O7 O 0.6709(5) 0.4878(4) 0.35201(19) 0.0698(15) Uani 1 1 d . . . O8 O 0.5315(4) 0.6361(4) 0.37050(18) 0.0585(13) Uani 1 1 d . . . H8B H 0.4995 0.6906 0.4090 0.070 Uiso 1 1 d R . . O9 O 0.4676(5) 0.7555(4) 0.4478(2) 0.0743(15) Uani 1 1 d . . . O10 O 0.4917(5) 0.7645(4) 0.5426(2) 0.0844(17) Uani 1 1 d . . . O11 O 0.6619(5) 0.5206(4) 0.6732(2) 0.0799(17) Uani 1 1 d . . . O12 O 0.7781(5) 0.3661(4) 0.65650(19) 0.0663(14) Uani 1 1 d . . . O13 O 0.1890(7) 0.2436(5) 0.4394(4) 0.130(3) Uani 1 1 d . . . H13B H 0.1663 0.2809 0.3916 0.156 Uiso 1 1 d R . . O14 O 0.1930(6) 0.2438(5) 0.5379(3) 0.128(2) Uani 1 1 d . . . O15 O 0.1076(7) 0.3513(6) 0.3596(3) 0.120(2) Uani 1 1 d . . . O16 O -0.0213(6) 0.5061(5) 0.3385(3) 0.105(2) Uani 1 1 d . . . O17 O 0.1561(12) 0.9505(5) 0.4642(4) 0.259(6) Uani 1 1 d . . . H17C H 0.1413 0.9759 0.5050 0.311 Uiso 1 1 d R . . H17D H 0.1471 0.8943 0.4651 0.311 Uiso 1 1 d R . . O18 O 0.8970(12) 0.9166(8) 0.4449(5) 0.298(7) Uani 1 1 d . . . H18A H 0.8808 0.8638 0.4549 0.357 Uiso 1 1 d R . . H18B H 0.9759 0.9030 0.4337 0.357 Uiso 1 1 d R . . O19 O 0.5448(18) 0.9406(8) 0.5534(4) 0.338(9) Uani 1 1 d . . . H19A H 0.5611 0.8795 0.5570 0.406 Uiso 1 1 d R . . H19B H 0.6061 0.9707 0.5283 0.406 Uiso 1 1 d R . . O20 O 0.332(3) 1.003(2) 0.5472(9) 0.74(3) Uani 1 1 d . . . H20A H 0.3755 0.9439 0.5476 0.891 Uiso 1 1 d R . . H20B H 0.3011 1.0161 0.5150 0.891 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0867(7) 0.0437(6) 0.0401(5) -0.0009(4) 0.0193(5) 0.0058(5) Cu2 0.0507(8) 0.0364(8) 0.028(2) 0.0038(7) -0.0009(8) -0.0095(6) Cu2' 0.0341(19) 0.045(2) 0.039(6) -0.007(2) 0.0055(18) -0.0151(14) N1 0.063(4) 0.035(3) 0.038(3) 0.001(3) 0.009(3) -0.005(3) N2 0.076(4) 0.037(4) 0.056(4) 0.007(3) 0.025(3) -0.004(3) N3 0.096(5) 0.055(4) 0.071(5) 0.014(4) -0.011(4) -0.015(4) N4 0.056(4) 0.041(3) 0.034(3) -0.011(3) 0.005(3) -0.016(3) N5 0.054(4) 0.056(4) 0.061(4) -0.017(3) 0.014(3) -0.010(3) N6 0.060(4) 0.052(4) 0.043(4) 0.018(3) 0.005(3) 0.003(3) N7 0.055(4) 0.054(4) 0.065(4) 0.008(3) -0.007(3) -0.007(3) N8 0.050(4) 0.049(4) 0.071(4) -0.027(3) 0.001(3) -0.015(3) N9 0.044(4) 0.047(4) 0.065(4) 0.010(3) -0.012(3) -0.018(3) N10 0.039(4) 0.071(4) 0.043(3) 0.004(3) -0.009(3) -0.012(3) N11 0.038(4) 0.028(4) 0.138(7) 0.029(4) -0.019(4) -0.006(3) N12 0.081(5) 0.059(5) 0.140(7) -0.017(5) 0.019(5) -0.005(4) N13 0.038(3) 0.039(3) 0.056(4) -0.003(3) -0.012(3) -0.006(3) N14 0.044(3) 0.041(4) 0.047(4) 0.007(3) 0.001(3) -0.019(3) C1 0.085(6) 0.052(5) 0.037(4) -0.001(4) -0.002(4) -0.015(4) C2 0.074(6) 0.039(5) 0.069(6) 0.011(4) -0.005(5) -0.010(4) C3 0.073(7) 0.046(6) 0.134(9) 0.002(6) 0.011(6) -0.026(5) C4 0.061(7) 0.065(7) 0.176(11) 0.006(7) 0.002(7) -0.016(5) C5 0.048(7) 0.080(9) 0.255(18) -0.020(10) 0.027(9) -0.026(6) C6 0.093(9) 0.048(7) 0.205(14) -0.046(8) 0.065(9) -0.033(6) C7 0.083(6) 0.054(5) 0.100(7) -0.014(5) 0.043(5) -0.012(5) C8 0.081(6) 0.031(5) 0.092(7) 0.001(5) 0.022(6) -0.009(4) C9 0.055(5) 0.076(5) 0.033(4) -0.011(4) 0.011(4) -0.012(4) C10 0.060(5) 0.042(4) 0.051(5) -0.010(4) 0.011(4) -0.018(4) C11 0.063(6) 0.071(6) 0.044(5) -0.013(4) -0.002(4) -0.025(5) C12 0.071(7) 0.107(8) 0.088(7) 0.001(6) -0.007(6) -0.031(6) C13 0.075(7) 0.120(9) 0.111(9) 0.020(7) -0.023(7) -0.034(6) C14 0.096(8) 0.130(9) 0.055(6) 0.018(6) -0.030(6) -0.040(7) C15 0.094(7) 0.077(6) 0.054(5) -0.022(5) 0.012(5) -0.043(5) C16 0.061(5) 0.049(5) 0.056(5) -0.008(4) 0.005(4) -0.030(4) C17 0.069(5) 0.051(5) 0.050(4) -0.001(4) 0.003(4) -0.013(4) C18 0.035(4) 0.039(5) 0.060(5) 0.016(4) 0.009(4) -0.001(3) C19 0.036(4) 0.061(6) 0.072(6) 0.037(5) -0.004(4) 0.001(4) C20 0.061(5) 0.075(6) 0.092(7) 0.040(5) -0.024(5) -0.025(4) C21 0.057(6) 0.123(9) 0.083(7) 0.060(6) -0.024(5) -0.036(6) C22 0.073(6) 0.109(8) 0.057(5) 0.034(6) -0.015(4) -0.038(6) C23 0.070(5) 0.082(6) 0.045(5) 0.018(4) 0.002(4) -0.014(4) C24 0.040(4) 0.057(5) 0.055(5) 0.029(4) 0.007(4) 0.000(4) C25 0.037(5) 0.106(7) 0.063(5) -0.024(4) 0.002(4) -0.024(4) C26 0.041(5) 0.053(5) 0.051(5) -0.004(4) -0.009(4) -0.017(4) C27 0.048(5) 0.054(5) 0.042(4) -0.001(4) -0.006(4) -0.014(4) C28 0.071(6) 0.071(6) 0.068(6) -0.003(4) 0.005(5) -0.010(5) C29 0.097(8) 0.122(8) 0.050(6) -0.017(5) 0.018(5) -0.028(6) C30 0.149(10) 0.126(9) 0.033(5) 0.001(5) -0.009(6) -0.073(8) C31 0.096(7) 0.097(7) 0.045(5) 0.018(5) -0.013(5) -0.048(6) C32 0.054(5) 0.047(4) 0.046(4) -0.002(4) -0.012(4) -0.021(4) C33 0.095(7) 0.061(6) 0.090(7) -0.002(5) -0.019(6) -0.019(5) C34 0.161(11) 0.070(7) 0.063(6) 0.017(5) -0.038(7) -0.051(7) C35 0.062(6) 0.067(6) 0.096(7) 0.023(6) -0.025(6) -0.023(5) C36 0.087(8) 0.088(8) 0.168(11) 0.023(7) 0.002(7) -0.023(7) C37 0.058(6) 0.127(9) 0.190(12) 0.077(10) -0.031(8) -0.023(6) C38 0.117(11) 0.094(9) 0.184(13) 0.038(8) 0.007(9) -0.037(8) C39 0.062(7) 0.083(7) 0.166(11) 0.037(7) -0.017(7) -0.036(6) C40 0.112(9) 0.060(6) 0.112(8) 0.022(6) -0.012(8) -0.058(6) C41 0.054(5) 0.064(5) 0.052(4) -0.018(4) -0.011(4) -0.025(4) C42 0.030(4) 0.043(5) 0.050(4) 0.006(4) -0.007(3) -0.007(3) C43 0.034(4) 0.045(5) 0.040(4) -0.007(4) 0.000(3) -0.006(3) C44 0.051(5) 0.059(5) 0.055(5) -0.009(4) 0.000(4) -0.023(4) C45 0.074(6) 0.090(7) 0.061(6) -0.021(5) -0.011(4) -0.032(5) C46 0.063(5) 0.099(7) 0.040(4) -0.002(5) -0.010(4) -0.024(5) C47 0.055(5) 0.076(6) 0.057(5) 0.012(4) -0.010(4) -0.023(4) C48 0.027(4) 0.056(5) 0.044(4) -0.003(4) 0.002(3) -0.009(3) C49 0.046(11) 0.034(9) 0.023(8) -0.009(6) -0.007(9) -0.019(8) C50 0.033(12) 0.037(10) 0.030(10) -0.010(7) -0.014(9) -0.001(8) C51 0.050(13) 0.011(8) 0.028(9) 0.004(6) 0.007(8) -0.006(7) C52 0.047(15) 0.035(10) 0.029(9) 0.012(8) -0.018(9) -0.002(9) C53 0.035(11) 0.045(11) 0.021(9) -0.013(8) -0.001(7) -0.004(9) O1 0.051(9) 0.055(10) 0.035(7) -0.019(7) -0.002(7) -0.010(9) O2 0.056(7) 0.023(6) 0.016(5) 0.000(4) -0.004(4) -0.006(5) O3 0.061(7) 0.081(7) 0.077(7) -0.032(6) 0.009(5) -0.036(6) O4 0.034(6) 0.076(7) 0.051(6) -0.021(5) 0.006(5) -0.013(6) C49' 0.019(10) 0.048(10) 0.034(10) 0.011(8) -0.009(8) -0.004(7) C50' 0.050(9) 0.013(6) 0.028(7) -0.005(5) -0.003(7) -0.003(6) C51' 0.038(10) 0.027(9) 0.044(11) 0.000(7) -0.026(9) -0.023(8) C52' 0.050(13) 0.064(15) 0.067(12) 0.021(10) 0.011(10) -0.019(11) C53' 0.028(10) 0.029(10) 0.042(11) 0.016(8) 0.010(11) -0.006(10) O1' 0.056(9) 0.084(10) 0.048(7) -0.022(6) -0.002(6) -0.006(7) O2' 0.083(11) 0.086(12) 0.104(13) 0.028(11) 0.025(9) -0.024(9) O3' 0.096(18) 0.155(19) 0.122(17) 0.070(14) -0.043(14) -0.029(16) O4' 0.089(11) 0.116(13) 0.35(3) 0.034(16) -0.013(13) -0.071(10) C54 0.036(4) 0.050(5) 0.038(4) 0.000(3) 0.000(3) -0.019(3) C55 0.039(4) 0.044(4) 0.055(5) 0.001(4) 0.010(3) -0.015(3) C56 0.037(4) 0.055(5) 0.037(4) 0.001(3) 0.007(3) -0.023(4) C57 0.043(4) 0.057(5) 0.044(4) 0.007(4) 0.002(3) -0.026(4) C58 0.043(4) 0.058(5) 0.034(4) -0.011(3) 0.002(3) -0.018(4) C59 0.030(4) 0.057(5) 0.037(4) 0.008(3) 0.000(3) -0.018(3) C60 0.059(5) 0.052(5) 0.055(5) -0.007(4) -0.002(4) -0.016(4) C61 0.044(5) 0.060(5) 0.054(5) 0.017(4) 0.001(4) -0.021(4) C62 0.053(5) 0.053(5) 0.054(5) 0.004(4) 0.013(4) -0.008(4) C63 0.039(4) 0.069(6) 0.044(5) -0.006(4) -0.003(4) -0.013(4) C64 0.059(6) 0.101(8) 0.072(6) 0.005(6) -0.007(5) -0.040(6) C65 0.039(5) 0.055(6) 0.099(7) 0.037(6) -0.026(5) -0.013(4) C66 0.054(6) 0.133(10) 0.134(10) 0.072(8) -0.045(6) -0.064(7) C67 0.086(7) 0.093(9) 0.098(8) 0.044(7) -0.028(7) -0.042(7) C68 0.060(7) 0.079(8) 0.183(13) 0.018(9) -0.038(8) -0.035(6) O5 0.086(4) 0.057(3) 0.059(3) -0.004(3) -0.020(3) -0.002(3) O6 0.131(5) 0.056(4) 0.063(4) -0.011(3) -0.009(3) 0.002(3) O7 0.094(4) 0.066(4) 0.037(3) -0.002(3) 0.004(3) -0.012(3) O8 0.055(3) 0.075(4) 0.045(3) 0.008(3) -0.004(2) -0.020(3) O9 0.082(4) 0.057(3) 0.068(4) 0.008(3) -0.009(3) 0.002(3) O10 0.120(5) 0.054(4) 0.063(4) -0.011(3) 0.006(3) -0.007(3) O11 0.094(4) 0.090(4) 0.041(3) -0.020(3) -0.011(3) -0.001(3) O12 0.077(4) 0.070(4) 0.045(3) -0.001(3) -0.026(3) -0.005(3) O13 0.123(6) 0.129(6) 0.129(6) 0.016(5) -0.042(5) -0.014(5) O14 0.122(6) 0.109(5) 0.137(6) 0.028(5) -0.021(5) -0.018(4) O15 0.104(5) 0.113(6) 0.140(6) 0.022(5) -0.042(4) -0.023(5) O16 0.104(5) 0.086(5) 0.125(5) 0.031(4) -0.053(4) -0.020(4) O17 0.487(18) 0.053(5) 0.202(9) 0.012(5) -0.111(10) -0.002(7) O18 0.286(14) 0.234(12) 0.369(17) 0.117(11) -0.014(12) -0.110(11) O19 0.65(3) 0.201(11) 0.172(10) -0.037(8) 0.120(14) -0.198(15) O20 0.96(6) 1.11(7) 0.46(3) -0.46(4) 0.46(4) -0.88(6) _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 O1' 1.832(11) . ? Cu1 N4 1.956(5) . ? Cu1 N2 1.959(6) . ? Cu1 N6 2.141(6) . ? Cu1 O1 2.156(15) . ? Cu1 N1 2.178(5) . ? Cu2 N11 1.950(7) . ? Cu2 O2 1.965(9) . ? Cu2 N9 2.011(6) . ? Cu2 O2' 2.064(15) . ? Cu2 N8 2.104(7) . ? Cu2 N13 2.110(6) . ? Cu2' O2' 1.850(17) . ? Cu2' N9 1.988(7) . ? Cu2' N13 2.106(7) . ? N1 C17 1.471(8) . ? N1 C9 1.488(7) . ? N1 C1 1.495(7) . ? N2 C2 1.337(8) . ? N2 C8 1.401(8) . ? N3 C2 1.326(8) . ? N3 C3 1.393(9) . ? N3 H3 0.8600 . ? N4 C10 1.326(7) . ? N4 C16 1.387(8) . ? N5 C10 1.362(8) . ? N5 C11 1.370(8) . ? N5 H5A 0.8600 . ? N6 C18 1.314(8) . ? N6 C24 1.396(7) . ? N7 C18 1.348(8) . ? N7 C19 1.401(8) . ? N7 H7A 0.8600 . ? N8 C25 1.466(8) . ? N8 C41 1.472(8) . ? N8 C33 1.483(8) . ? N9 C26 1.322(7) . ? N9 C32 1.406(7) . ? N10 C26 1.343(7) . ? N10 C27 1.381(7) . ? N10 H10 0.8600 . ? N11 C40 1.337(7) . ? N11 C34 1.354(9) . ? N12 C35 1.324(9) . ? N12 C34 1.440(11) . ? N12 H12A 0.8600 . ? N13 C42 1.345(7) . ? N13 C48 1.391(8) . ? N14 C42 1.340(7) . ? N14 C43 1.381(7) . ? N14 H14A 0.8600 . ? C1 C2 1.478(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C4 1.400(11) . ? C3 C8 1.413(11) . ? C4 C5 1.370(13) . ? C4 H4 0.9300 . ? C5 C6 1.405(14) . ? C5 H5 0.9300 . ? C6 C7 1.371(12) . ? C6 H6 0.9300 . ? C7 C8 1.361(9) . ? C7 H7 0.9300 . ? C9 C10 1.463(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 C12 1.359(10) . ? C11 C16 1.376(9) . ? C12 C13 1.367(11) . ? C12 H12 0.9300 . ? C13 C14 1.395(11) . ? C13 H13 0.9300 . ? C14 C15 1.371(10) . ? C14 H14 0.9300 . ? C15 C16 1.414(9) . ? C15 H15 0.9300 . ? C17 C18 1.495(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C19 C20 1.365(9) . ? C19 C24 1.403(10) . ? C20 C21 1.417(10) . ? C20 H20 0.9300 . ? C21 C22 1.351(11) . ? C21 H21 0.9300 . ? C22 C23 1.362(10) . ? C22 H22 0.9300 . ? C23 C24 1.365(9) . ? C23 H23 0.9300 . ? C25 C26 1.492(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C27 C32 1.396(8) . ? C27 C28 1.405(8) . ? C28 C29 1.368(10) . ? C28 H28 0.9300 . ? C29 C30 1.383(11) . ? C29 H29 0.9300 . ? C30 C31 1.361(11) . ? C30 H30 0.9300 . ? C31 C32 1.376(9) . ? C31 H31 0.9300 . ? C33 C34 1.370(11) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C36 H36 0.9300 . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 C40 1.3900 . ? C39 H39 0.9300 . ? C41 C42 1.486(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C43 C48 1.373(8) . ? C43 C44 1.387(8) . ? C44 C45 1.378(9) . ? C44 H44 0.9300 . ? C45 C46 1.386(10) . ? C45 H45 0.9300 . ? C46 C47 1.381(9) . ? C46 H46 0.9300 . ? C47 C48 1.396(8) . ? C47 H47 0.9300 . ? C49 C50 1.27(2) . ? C49 C51 1.41(2) . ? C49 C53 1.52(2) . ? C50 C51' 1.414(19) 2_557 ? C50 H50 0.9300 . ? C51 C52 1.37(2) . ? C51 C50' 1.408(16) 2_557 ? C52 O4 1.36(2) . ? C52 O3 1.381(10) . ? C53 O2 1.202(15) . ? C53 O1 1.227(15) . ? O3 H3C 0.9301 . ? C49' C50' 1.34(2) . ? C49' C51' 1.40(2) . ? C49' C53' 1.51(3) . ? C50' C51 1.408(16) 2_557 ? C50' H50' 0.9300 . ? C51' C50 1.414(19) 2_557 ? C51' C52' 1.48(2) . ? C52' O4' 1.205(19) . ? C52' O3' 1.360(10) . ? C53' O1' 1.20(3) . ? C53' O2' 1.22(2) . ? O3' H3' 0.8200 . ? C54 C55 1.375(8) . ? C54 C59 1.419(8) . ? C54 C60 1.491(9) . ? C55 C56 1.381(8) . ? C55 H55 0.9300 . ? C56 C57 1.444(8) . ? C56 C61 1.509(9) . ? C57 C58 1.395(8) . ? C57 C62 1.523(9) . ? C58 C59 1.392(8) . ? C58 H58 0.9300 . ? C59 C63 1.517(8) . ? C60 O6 1.226(7) . ? C60 O5 1.276(8) . ? C61 O7 1.234(7) . ? C61 O8 1.280(7) . ? C62 O10 1.214(8) . ? C62 O9 1.291(8) . ? C63 O11 1.219(7) . ? C63 O12 1.280(7) . ? C64 C66 1.375(12) . ? C64 C65 1.395(11) . ? C64 C67 1.442(12) . ? C65 C68 1.451(13) . ? C65 C66 1.459(12) 2_566 ? C66 C65 1.460(12) 2_566 ? C66 H66 0.9300 . ? C67 O14 1.293(10) . ? C67 O13 1.310(11) . ? C68 O15 1.295(10) . ? C68 O16 1.302(11) . ? O5 H5B 1.1823 . ? O8 H8B 1.1434 . ? O9 H8B 1.2454 . ? O12 H5B 1.2210 . ? O13 H13B 1.1828 . ? O15 H13B 1.2347 . ? O17 H17C 0.9833 . ? O17 H17D 0.8201 . ? O18 H18A 0.8200 . ? O18 H18B 0.8200 . ? O19 H19A 0.8199 . ? O19 H19B 0.9834 . ? O20 H20A 0.8200 . ? O20 H20B 0.8200 . ? 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 O1' Cu1 N4 108.8(4) . . ? O1' Cu1 N2 91.8(4) . . ? N4 Cu1 N2 153.5(2) . . ? O1' Cu1 N6 87.1(4) . . ? N4 Cu1 N6 92.8(2) . . ? N2 Cu1 N6 105.1(2) . . ? O1' Cu1 O1 30.8(5) . . ? N4 Cu1 O1 89.2(4) . . ? N2 Cu1 O1 101.6(4) . . ? N6 Cu1 O1 112.1(5) . . ? O1' Cu1 N1 164.9(4) . . ? N4 Cu1 N1 82.4(2) . . ? N2 Cu1 N1 80.8(2) . . ? N6 Cu1 N1 82.2(2) . . ? O1 Cu1 N1 163.8(5) . . ? N11 Cu2 O2 95.5(3) . . ? N11 Cu2 N9 158.9(4) . . ? O2 Cu2 N9 96.5(3) . . ? N11 Cu2 O2' 94.9(5) . . ? O2 Cu2 O2' 35.2(6) . . ? N9 Cu2 O2' 85.2(4) . . ? N11 Cu2 N8 80.8(3) . . ? O2 Cu2 N8 166.2(4) . . ? N9 Cu2 N8 83.4(2) . . ? O2' Cu2 N8 131.4(6) . . ? N11 Cu2 N13 103.2(2) . . ? O2 Cu2 N13 108.8(4) . . ? N9 Cu2 N13 89.2(2) . . ? O2' Cu2 N13 141.8(6) . . ? N8 Cu2 N13 85.0(2) . . ? O2' Cu2' N9 91.8(5) . . ? O2' Cu2' N13 170.9(8) . . ? N9 Cu2' N13 89.9(3) . . ? C17 N1 C9 111.9(5) . . ? C17 N1 C1 110.2(5) . . ? C9 N1 C1 113.2(5) . . ? C17 N1 Cu1 106.6(3) . . ? C9 N1 Cu1 108.0(4) . . ? C1 N1 Cu1 106.6(4) . . ? C2 N2 C8 106.3(6) . . ? C2 N2 Cu1 114.2(5) . . ? C8 N2 Cu1 139.3(6) . . ? C2 N3 C3 108.6(7) . . ? C2 N3 H3 125.7 . . ? C3 N3 H3 125.7 . . ? C10 N4 C16 105.9(6) . . ? C10 N4 Cu1 113.8(5) . . ? C16 N4 Cu1 138.7(4) . . ? C10 N5 C11 107.7(6) . . ? C10 N5 H5A 126.2 . . ? C11 N5 H5A 126.2 . . ? C18 N6 C24 105.1(6) . . ? C18 N6 Cu1 110.3(4) . . ? C24 N6 Cu1 143.8(6) . . ? C18 N7 C19 105.9(6) . . ? C18 N7 H7A 127.1 . . ? C19 N7 H7A 127.1 . . ? C25 N8 C41 113.6(6) . . ? C25 N8 C33 110.9(6) . . ? C41 N8 C33 108.1(5) . . ? C25 N8 Cu2 109.1(4) . . ? C41 N8 Cu2 107.1(4) . . ? C33 N8 Cu2 107.8(5) . . ? C26 N9 C32 106.5(5) . . ? C26 N9 Cu2' 134.0(6) . . ? C32 N9 Cu2' 119.3(6) . . ? C26 N9 Cu2 110.2(5) . . ? C32 N9 Cu2 143.2(5) . . ? C26 N10 C27 108.3(5) . . ? C26 N10 H10 125.8 . . ? C27 N10 H10 125.8 . . ? C40 N11 C34 110.6(8) . . ? C40 N11 Cu2 139.5(7) . . ? C34 N11 Cu2 109.9(6) . . ? C35 N12 C34 109.9(7) . . ? C35 N12 H12A 125.1 . . ? C34 N12 H12A 125.1 . . ? C42 N13 C48 105.6(5) . . ? C42 N13 Cu2' 128.8(6) . . ? C48 N13 Cu2' 123.9(5) . . ? C42 N13 Cu2 107.0(5) . . ? C48 N13 Cu2 146.7(5) . . ? C42 N14 C43 107.9(5) . . ? C42 N14 H14A 126.0 . . ? C43 N14 H14A 126.0 . . ? C2 C1 N1 106.1(5) . . ? C2 C1 H1A 110.5 . . ? N1 C1 H1A 110.5 . . ? C2 C1 H1B 110.5 . . ? N1 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? N3 C2 N2 112.0(7) . . ? N3 C2 C1 126.0(7) . . ? N2 C2 C1 121.9(7) . . ? N3 C3 C4 131.8(11) . . ? N3 C3 C8 105.2(8) . . ? C4 C3 C8 123.0(10) . . ? C5 C4 C3 114.4(11) . . ? C5 C4 H4 122.8 . . ? C3 C4 H4 122.8 . . ? C4 C5 C6 124.0(12) . . ? C4 C5 H5 118.0 . . ? C6 C5 H5 118.0 . . ? C7 C6 C5 119.4(11) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C8 C7 C6 119.6(10) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 N2 132.5(9) . . ? C7 C8 C3 119.5(8) . . ? N2 C8 C3 107.8(7) . . ? C10 C9 N1 108.8(5) . . ? C10 C9 H9A 109.9 . . ? N1 C9 H9A 109.9 . . ? C10 C9 H9B 109.9 . . ? N1 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N4 C10 N5 110.9(6) . . ? N4 C10 C9 123.7(7) . . ? N5 C10 C9 125.4(6) . . ? C12 C11 N5 128.4(8) . . ? C12 C11 C16 125.5(8) . . ? N5 C11 C16 106.1(7) . . ? C11 C12 C13 114.8(9) . . ? C11 C12 H12 122.6 . . ? C13 C12 H12 122.6 . . ? C12 C13 C14 123.4(9) . . ? C12 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C15 C14 C13 120.1(8) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 118.0(8) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? C11 C16 N4 109.3(6) . . ? C11 C16 C15 118.2(8) . . ? N4 C16 C15 132.5(7) . . ? N1 C17 C18 113.5(6) . . ? N1 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? N1 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N6 C18 N7 114.3(6) . . ? N6 C18 C17 121.8(6) . . ? N7 C18 C17 123.7(7) . . ? C20 C19 N7 131.2(9) . . ? C20 C19 C24 123.0(8) . . ? N7 C19 C24 105.8(6) . . ? C19 C20 C21 114.5(8) . . ? C19 C20 H20 122.7 . . ? C21 C20 H20 122.7 . . ? C22 C21 C20 122.8(8) . . ? C22 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? C21 C22 C23 121.1(8) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C24 119.0(8) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 N6 131.5(8) . . ? C23 C24 C19 119.5(7) . . ? N6 C24 C19 108.9(7) . . ? N8 C25 C26 108.3(6) . . ? N8 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? N8 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? N9 C26 N10 111.5(6) . . ? N9 C26 C25 124.2(6) . . ? N10 C26 C25 124.2(6) . . ? N10 C27 C32 105.9(6) . . ? N10 C27 C28 132.6(7) . . ? C32 C27 C28 121.5(6) . . ? C29 C28 C27 115.5(7) . . ? C29 C28 H28 122.2 . . ? C27 C28 H28 122.2 . . ? C28 C29 C30 122.5(8) . . ? C28 C29 H29 118.7 . . ? C30 C29 H29 118.7 . . ? C31 C30 C29 122.0(8) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 117.2(8) . . ? C30 C31 H31 121.4 . . ? C32 C31 H31 121.4 . . ? C31 C32 C27 121.1(7) . . ? C31 C32 N9 131.1(7) . . ? C27 C32 N9 107.8(6) . . ? C34 C33 N8 105.7(7) . . ? C34 C33 H33A 110.6 . . ? N8 C33 H33A 110.6 . . ? C34 C33 H33B 110.6 . . ? N8 C33 H33B 110.6 . . ? H33A C33 H33B 108.7 . . ? N11 C34 C33 126.2(10) . . ? N11 C34 N12 103.9(9) . . ? C33 C34 N12 129.8(9) . . ? N12 C35 C36 133.4(7) . . ? N12 C35 C40 106.6(7) . . ? C36 C35 C40 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C39 C38 C37 120.0 . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 120.0 . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? N11 C40 C39 131.1(7) . . ? N11 C40 C35 108.8(7) . . ? C39 C40 C35 120.0 . . ? N8 C41 C42 112.7(5) . . ? N8 C41 H41A 109.1 . . ? C42 C41 H41A 109.1 . . ? N8 C41 H41B 109.1 . . ? C42 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? N14 C42 N13 111.1(6) . . ? N14 C42 C41 125.3(6) . . ? N13 C42 C41 123.6(6) . . ? C48 C43 N14 106.3(6) . . ? C48 C43 C44 122.9(7) . . ? N14 C43 C44 130.6(6) . . ? C45 C44 C43 116.5(7) . . ? C45 C44 H44 121.8 . . ? C43 C44 H44 121.8 . . ? C44 C45 C46 121.2(7) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C47 C46 C45 122.0(7) . . ? C47 C46 H46 119.0 . . ? C45 C46 H46 119.0 . . ? C46 C47 C48 117.0(7) . . ? C46 C47 H47 121.5 . . ? C48 C47 H47 121.5 . . ? C43 C48 N13 109.0(6) . . ? C43 C48 C47 120.3(7) . . ? N13 C48 C47 130.6(7) . . ? C50 C49 C51 116.7(15) . . ? C50 C49 C53 121.0(16) . . ? C51 C49 C53 120.7(13) . . ? C49 C50 C51' 127.4(17) . 2_557 ? C49 C50 C50 86.5(15) . 2_557 ? C49 C50 C51 156.3(14) . 2_557 ? C50 C50 C51 72.6(10) 2_557 2_557 ? C49 C50 H50 116.3 . . ? C51' C50 H50 116.3 2_557 . ? C50 C50 H50 152.7 2_557 . ? C51 C50 H50 81.7 2_557 . ? C52 C51 C50' 115.3(12) . 2_557 ? C52 C51 C49 126.4(13) . . ? C50' C51 C49 118.0(13) 2_557 . ? C52 C51 C50 152.0(11) . 2_557 ? C49 C51 C50 81.1(10) . 2_557 ? O4 C52 C51 126.3(11) . . ? O4 C52 O3 111.4(14) . . ? C51 C52 O3 122.3(16) . . ? O2 C53 O1 126.8(18) . . ? O2 C53 C49 117.8(12) . . ? O1 C53 C49 115.2(16) . . ? C53 O1 Cu1 164.6(17) . . ? C53 O2 Cu2 123.5(11) . . ? C52 O3 H3C 113.4 . . ? C50' C49' C51' 117.4(15) . . ? C50' C49' C53' 118.0(16) . . ? C51' C49' C53' 124.4(17) . . ? C49' C50' C51 123.8(14) . 2_557 ? C49' C50' C51' 85.3(11) . 2_557 ? C49' C50' H50' 118.1 . . ? C51 C50' H50' 118.1 2_557 . ? C51' C50' H50' 150.0 2_557 . ? C49' C51' C50 116.5(15) . 2_557 ? C49' C51' C52' 124.7(15) . . ? C50 C51' C52' 118.8(15) 2_557 . ? C49' C51' C50' 152.7(12) . 2_557 ? C52' C51' C51' 154.0(15) . 2_557 ? C50' C51' C51' 77.7(10) 2_557 2_557 ? O4' C52' O3' 115(2) . . ? O4' C52' C51' 124.1(13) . . ? O3' C52' C51' 119.1(17) . . ? O1' C53' O2' 124(2) . . ? O1' C53' C49' 114.6(16) . . ? O2' C53' C49' 122(2) . . ? C53' O1' Cu1 125.3(14) . . ? C53' O2' Cu2' 152.3(19) . . ? C53' O2' Cu2 160.1(15) . . ? C52' O3' H3' 109.5 . . ? C55 C54 C59 116.6(6) . . ? C55 C54 C60 114.8(6) . . ? C59 C54 C60 128.6(6) . . ? C54 C55 C56 127.1(6) . . ? C54 C55 H55 116.4 . . ? C56 C55 H55 116.4 . . ? C55 C56 C57 116.7(6) . . ? C55 C56 C61 115.9(6) . . ? C57 C56 C61 127.4(6) . . ? C58 C57 C56 116.3(6) . . ? C58 C57 C62 114.2(6) . . ? C56 C57 C62 129.5(6) . . ? C59 C58 C57 125.5(6) . . ? C59 C58 H58 117.2 . . ? C57 C58 H58 117.2 . . ? C58 C59 C54 117.7(6) . . ? C58 C59 C63 113.7(6) . . ? C54 C59 C63 128.5(6) . . ? O6 C60 O5 119.3(7) . . ? O6 C60 C54 118.7(7) . . ? O5 C60 C54 122.0(7) . . ? O7 C61 O8 121.3(7) . . ? O7 C61 C56 118.4(7) . . ? O8 C61 C56 120.3(7) . . ? O10 C62 O9 122.5(7) . . ? O10 C62 C57 118.6(7) . . ? O9 C62 C57 118.9(7) . . ? O11 C63 O12 121.0(6) . . ? O11 C63 C59 119.9(7) . . ? O12 C63 C59 119.1(6) . . ? C66 C64 C65 116.9(9) . . ? C66 C64 C67 112.7(10) . . ? C65 C64 C67 130.5(10) . . ? C64 C65 C68 129.9(10) . . ? C64 C65 C66 115.5(9) . 2_566 ? C68 C65 C66 114.6(9) . 2_566 ? C64 C66 C65 127.7(9) . 2_566 ? C64 C66 H66 116.2 . . ? C65 C66 H66 116.2 2_566 . ? O14 C67 O13 116.8(11) . . ? O14 C67 C64 123.2(11) . . ? O13 C67 C64 120.0(9) . . ? O15 C68 O16 119.6(12) . . ? O15 C68 C65 118.1(11) . . ? O16 C68 C65 122.2(10) . . ? C60 O5 H5B 106.2 . . ? C61 O8 H8B 109.7 . . ? C62 O9 H8B 110.0 . . ? C63 O12 H5B 108.9 . . ? C67 O13 H13B 123.7 . . ? C68 O15 H13B 126.3 . . ? H17C O17 H17D 110.5 . . ? H18A O18 H18B 107.7 . . ? H19A O19 H19B 120.4 . . ? H20A O20 H20B 107.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O17 0.86 1.79 2.641(11) 170.4 2_566 N5 H5A O11 0.86 1.88 2.707(7) 161.1 1_545 N7 H7A O16 0.86 1.95 2.793(8) 166.3 2_556 N10 H10 O12 0.86 2.06 2.814(7) 146.2 1_455 N12 H12A O19 0.86 1.81 2.673(12) 178.2 1_545 N14 H14A O7 0.86 1.99 2.831(6) 164.8 2_666 O3 H3C O4 0.93 1.84 2.735(13) 160.3 2_657 O8 H8B O9 1.14 1.25 2.386(7) 175.0 . O13 H13B O15 1.18 1.23 2.340(10) 150.9 . O17 H17C O18 0.98 1.86 2.751(15) 149.4 2_676 O17 H17C O20 0.98 2.51 3.09(3) 118.1 . O17 H17D O5 0.82 2.29 3.043(9) 153.7 2_666 O17 H17D O6 0.82 2.19 2.909(9) 146.4 2_666 O18 H18A O14 0.82 1.89 2.691(13) 163.4 2_666 O18 H18B N3 0.82 2.46 3.055(13) 130.9 2_666 O18 H18B O5 0.82 2.38 3.005(13) 133.9 2_766 O18 H18B O17 0.82 2.43 3.059(17) 134.8 1_655 O19 H19A O10 0.82 2.03 2.730(13) 142.6 . O19 H19B O20 0.98 1.80 2.662(19) 145.1 2_676 O20 H20A O10 0.82 2.44 3.26(3) 174.5 . O20 H20A O19 0.82 1.83 2.21(3) 106.8 . O20 H20B O17 0.82 2.47 3.09(3) 134.1 . C1 H1A O20 0.97 2.59 3.505(16) 156.3 1_545 C1 H1B O6 0.97 2.47 3.343(9) 148.9 2_656 C9 H9A O7 0.97 2.56 3.459(9) 153.6 2_656 C9 H9B O10 0.97 2.50 3.212(8) 130.1 1_545 C15 H15 O1 0.93 2.55 3.190(17) 126.8 . C17 H17A O7 0.97 2.53 3.387(8) 147.6 2_656 C33 H33B O14 0.97 2.54 3.331(11) 138.3 . C39 H39 O4 0.93 2.56 3.356(11) 143.7 . C41 H41B O8 0.97 2.53 3.079(8) 116.0 2_666 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.128 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.084 # start Validation Reply Form _vrf_PLAT215_9a ; PROBLEM: Disordered C51' has ADP max/min Ratio ..... 5.30 RESPONSE: This comes from the disorders of some related atoms. ; _vrf_PLAT220_9a ; PROBLEM: Large Non-Solvent O Ueq(max)/Ueq(min) ... 5.42 Ratio RESPONSE: This comes from the disorders of some related atoms. ; _vrf_PLAT417_9a ; PROBLEM: Short Inter D-H..H-D H19B .. H20B .. 1.34 Ang. RESPONSE: This is due to the disorder of some water molecules or unsuitably assigned sites of their hydrogen atoms . ; # END data_9 #TrackingRef '- 1-9.cif' _database_code_depnum_ccdc_archive 'CCDC 788596' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C106 H88 Cu4 N28 O8, 6(Cl O4), 2(H2 O)' _chemical_formula_sum 'C106 H92 Cl6 Cu4 N28 O34' _chemical_formula_weight 2768.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1980(9) _cell_length_b 17.0069(18) _cell_length_c 18.553(2) _cell_angle_alpha 74.333(2) _cell_angle_beta 74.272(3) _cell_angle_gamma 77.117(2) _cell_volume 2943.0(5) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 3255 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 20.36 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1414 _exptl_absorpt_coefficient_mu 0.942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7653 _exptl_absorpt_correction_T_max 0.9814 _exptl_absorpt_process_details 'SADABS, (Sheldrick,1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 20739 _diffrn_reflns_av_R_equivalents 0.0998 _diffrn_reflns_av_sigmaI/netI 0.1430 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10085 _reflns_number_gt 4534 _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. In the refinement, the three perchlorate anions were slightly disordered and command 'SADI' was used to restrain the Cl-O and O...O distances to be equal to each other. Both the Cl3/O13-O16 and Cl4/O17-O20 anions were disordered by inversion centers and the atomic occupancies of these atoms were assigend to be 0.5. Command 'ISOR' was also used to restrain some abnormal thermal factors. Due to the very large thermal factors, the occupancies of water O21 and O22 atoms were refined freely and their final outcome are of ca. 0.60(1) and 0.40(1), respectively. ; _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^)+(0.1162P)^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 10085 _refine_ls_number_parameters 832 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.1592 _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.2389 _refine_ls_wR_factor_gt 0.2148 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.918 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.03496(10) -0.11898(6) 0.25624(5) 0.0381(3) Uani 1 1 d . . . Cu2 Cu 0.11162(10) 0.29678(6) 0.29862(5) 0.0413(3) Uani 1 1 d . . . C1 C 0.0176(9) -0.2132(5) 0.1332(4) 0.048(2) Uani 1 1 d . . . H1A H 0.1158 -0.2367 0.1214 0.058 Uiso 1 1 calc R . . H1B H -0.0231 -0.2171 0.0924 0.058 Uiso 1 1 calc R . . C2 C -0.0523(9) -0.2621(5) 0.2088(4) 0.043(2) Uani 1 1 d . . . C3 C -0.1371(8) -0.3022(5) 0.3302(5) 0.039(2) Uani 1 1 d . . . C4 C -0.1867(8) -0.3075(5) 0.4076(4) 0.041(2) Uani 1 1 d . . . H4 H -0.1755 -0.2679 0.4315 0.049 Uiso 1 1 calc R . . C5 C -0.2540(9) -0.3735(6) 0.4491(5) 0.051(2) Uani 1 1 d . . . H5 H -0.2883 -0.3788 0.5023 0.061 Uiso 1 1 calc R . . C6 C -0.2727(10) -0.4318(6) 0.4149(6) 0.063(3) Uani 1 1 d . . . H6 H -0.3196 -0.4756 0.4448 0.076 Uiso 1 1 calc R . . C7 C -0.2216(10) -0.4259(6) 0.3352(6) 0.060(3) Uani 1 1 d . . . H7 H -0.2341 -0.4653 0.3115 0.072 Uiso 1 1 calc R . . C8 C -0.1542(9) -0.3621(5) 0.2937(5) 0.044(2) Uani 1 1 d . . . C9 C -0.1108(10) -0.0740(6) 0.1012(5) 0.062(3) Uani 1 1 d . . . H9A H -0.1390 -0.1043 0.0713 0.075 Uiso 1 1 calc R . . H9B H -0.0813 -0.0231 0.0667 0.075 Uiso 1 1 calc R . . C10 C -0.2352(9) -0.0523(5) 0.1685(4) 0.043(2) Uani 1 1 d . . . C11 C -0.3475(9) -0.0395(5) 0.2825(5) 0.041(2) Uani 1 1 d . . . C12 C -0.3912(10) -0.0419(5) 0.3609(5) 0.049(2) Uani 1 1 d . . . H12 H -0.3307 -0.0624 0.3945 0.059 Uiso 1 1 calc R . . C13 C -0.5271(12) -0.0124(6) 0.3858(6) 0.064(3) Uani 1 1 d . . . H13 H -0.5604 -0.0104 0.4379 0.077 Uiso 1 1 calc R . . C14 C -0.6191(12) 0.0149(7) 0.3369(9) 0.085(4) Uani 1 1 d . . . H14 H -0.7130 0.0322 0.3572 0.102 Uiso 1 1 calc R . . C15 C -0.5760(11) 0.0167(6) 0.2626(8) 0.071(3) Uani 1 1 d . . . H15 H -0.6378 0.0356 0.2298 0.085 Uiso 1 1 calc R . . C16 C -0.4381(9) -0.0098(5) 0.2345(6) 0.052(2) Uani 1 1 d . . . C17 C 0.1346(10) -0.0930(6) 0.0999(5) 0.062(3) Uani 1 1 d . . . H17A H 0.1799 -0.1117 0.0523 0.075 Uiso 1 1 calc R . . H17B H 0.1182 -0.0323 0.0880 0.075 Uiso 1 1 calc R . . C18 C 0.2209(10) -0.1256(6) 0.1566(6) 0.058(3) Uani 1 1 d . . . C19 C 0.2718(7) -0.1680(4) 0.2686(5) 0.062(3) Uani 1 1 d G . . C20 C 0.2713(8) -0.1905(5) 0.3464(5) 0.088(4) Uani 1 1 d G . . H20 H 0.1875 -0.1852 0.3830 0.106 Uiso 1 1 calc R . . C21 C 0.3947(11) -0.2207(5) 0.3702(5) 0.108(5) Uani 1 1 d G . . H21 H 0.3944 -0.2359 0.4228 0.130 Uiso 1 1 calc R . . C22 C 0.5187(8) -0.2284(5) 0.3160(7) 0.108(5) Uani 1 1 d G . . H22 H 0.6021 -0.2489 0.3321 0.130 Uiso 1 1 calc R . . C23 C 0.5192(7) -0.2060(5) 0.2382(6) 0.106(4) Uani 1 1 d G . . H23 H 0.6030 -0.2112 0.2016 0.128 Uiso 1 1 calc R . . C24 C 0.3958(9) -0.1757(5) 0.2144(4) 0.081(3) Uani 1 1 d G . . C25 C 0.0688(11) 0.3010(6) 0.1430(6) 0.070(3) Uani 1 1 d . . . H25A H 0.0785 0.2417 0.1456 0.083 Uiso 1 1 calc R . . H25B H 0.0669 0.3311 0.0901 0.083 Uiso 1 1 calc R . . C26 C -0.0628(11) 0.3288(6) 0.1971(6) 0.058(3) Uani 1 1 d . . . C27 C -0.1989(6) 0.3539(4) 0.3031(4) 0.063(3) Uani 1 1 d G . . C28 C -0.2621(7) 0.3629(4) 0.3775(4) 0.065(3) Uani 1 1 d G . . H28 H -0.2098 0.3488 0.4152 0.078 Uiso 1 1 calc R . . C29 C -0.4025(8) 0.3929(4) 0.3963(4) 0.077(3) Uani 1 1 d G . . H29 H -0.4452 0.3990 0.4466 0.092 Uiso 1 1 calc R . . C30 C -0.4798(6) 0.4138(4) 0.3406(6) 0.097(4) Uani 1 1 d G . . H30 H -0.5747 0.4341 0.3533 0.116 Uiso 1 1 calc R . . C31 C -0.4166(8) 0.4048(4) 0.2662(5) 0.082(4) Uani 1 1 d G . . H31 H -0.4689 0.4190 0.2285 0.098 Uiso 1 1 calc R . . C32 C -0.2762(9) 0.3749(4) 0.2475(4) 0.069(3) Uani 1 1 d G . . C33 C 0.2141(11) 0.4013(6) 0.1370(5) 0.063(3) Uani 1 1 d . . . H33A H 0.1479 0.4324 0.1056 0.076 Uiso 1 1 calc R . . H33B H 0.3069 0.4007 0.1035 0.076 Uiso 1 1 calc R . . C34 C 0.2043(10) 0.4438(5) 0.1974(5) 0.047(2) Uani 1 1 d . . . C35 C 0.1596(8) 0.4741(5) 0.3099(5) 0.044(2) Uani 1 1 d . . . C36 C 0.1216(9) 0.4751(5) 0.3860(5) 0.049(2) Uani 1 1 d . . . H36 H 0.0820 0.4316 0.4225 0.058 Uiso 1 1 calc R . . C37 C 0.1424(11) 0.5408(6) 0.4077(6) 0.069(3) Uani 1 1 d . . . H37 H 0.1178 0.5432 0.4598 0.082 Uiso 1 1 calc R . . C38 C 0.2012(11) 0.6052(6) 0.3514(7) 0.070(3) Uani 1 1 d . . . H38 H 0.2144 0.6506 0.3670 0.084 Uiso 1 1 calc R . . C39 C 0.2387(11) 0.6046(6) 0.2773(7) 0.068(3) Uani 1 1 d . . . H39 H 0.2798 0.6479 0.2414 0.081 Uiso 1 1 calc R . . C40 C 0.2168(9) 0.5399(5) 0.2536(5) 0.045(2) Uani 1 1 d . . . C41 C 0.3099(10) 0.2534(6) 0.1556(5) 0.056(3) Uani 1 1 d . . . H41A H 0.3741 0.2714 0.1068 0.067 Uiso 1 1 calc R . . H41B H 0.2823 0.2022 0.1545 0.067 Uiso 1 1 calc R . . C42 C 0.3796(9) 0.2384(5) 0.2221(5) 0.044(2) Uani 1 1 d . . . C43 C 0.3958(8) 0.2212(5) 0.3410(4) 0.0376(19) Uani 1 1 d . . . C44 C 0.3756(10) 0.2160(5) 0.4182(5) 0.048(2) Uani 1 1 d . . . H44 H 0.2872 0.2311 0.4477 0.057 Uiso 1 1 calc R . . C45 C 0.4873(11) 0.1883(5) 0.4515(5) 0.056(3) Uani 1 1 d . . . H45 H 0.4753 0.1844 0.5044 0.068 Uiso 1 1 calc R . . C46 C 0.6202(10) 0.1657(6) 0.4071(5) 0.053(2) Uani 1 1 d . . . H46 H 0.6951 0.1473 0.4311 0.063 Uiso 1 1 calc R . . C47 C 0.6424(9) 0.1698(5) 0.3322(6) 0.055(2) Uani 1 1 d . . . H47 H 0.7319 0.1552 0.3036 0.066 Uiso 1 1 calc R . . C48 C 0.5315(9) 0.1959(5) 0.2971(5) 0.043(2) Uani 1 1 d . . . C49 C -0.0109(7) -0.0079(4) 0.4267(4) 0.0295(17) Uani 1 1 d . . . C50 C 0.0173(7) 0.0677(4) 0.4346(4) 0.0288(17) Uani 1 1 d . . . C51 C 0.0265(7) 0.0707(4) 0.5079(4) 0.0302(18) Uani 1 1 d . . . H51 H 0.0450 0.1204 0.5130 0.036 Uiso 1 1 calc R . . C52 C -0.0240(8) -0.0271(5) 0.3560(4) 0.0370(19) Uani 1 1 d . . . C53 C 0.0433(7) 0.1446(5) 0.3716(4) 0.0310(18) Uani 1 1 d . . . N1 N 0.0030(7) -0.1252(4) 0.1352(4) 0.0427(17) Uani 1 1 d . . . N2 N -0.0721(6) -0.2415(4) 0.2741(3) 0.0369(16) Uani 1 1 d . . . N3 N -0.0995(7) -0.3333(4) 0.2176(4) 0.0486(19) Uani 1 1 d . . . H3 H -0.0955 -0.3569 0.1807 0.058 Uiso 1 1 calc R . . N4 N -0.2169(7) -0.0657(4) 0.2400(3) 0.0397(17) Uani 1 1 d . . . N5 N -0.3596(8) -0.0204(4) 0.1622(4) 0.055(2) Uani 1 1 d . . . H5A H -0.3897 -0.0077 0.1203 0.066 Uiso 1 1 calc R . . N6 N 0.1646(7) -0.1375(4) 0.2312(5) 0.052(2) Uani 1 1 d . . . N7 N 0.3612(9) -0.1478(5) 0.1446(6) 0.084(3) Uani 1 1 d . . . H7A H 0.4187 -0.1447 0.1000 0.101 Uiso 1 1 calc R . . N8 N 0.1875(8) 0.3179(4) 0.1662(4) 0.0490(19) Uani 1 1 d . . . N9 N -0.0665(8) 0.3279(4) 0.2689(4) 0.0482(18) Uani 1 1 d . . . N10 N -0.1875(10) 0.3579(5) 0.1817(5) 0.075(3) Uani 1 1 d . . . H10 H -0.2085 0.3649 0.1377 0.090 Uiso 1 1 calc R . . N11 N 0.1527(6) 0.4143(4) 0.2693(4) 0.0384(16) Uani 1 1 d . . . N12 N 0.2441(8) 0.5184(4) 0.1854(4) 0.0517(19) Uani 1 1 d . . . H12A H 0.2811 0.5474 0.1411 0.062 Uiso 1 1 calc R . . N13 N 0.3050(7) 0.2477(4) 0.2909(3) 0.0387(16) Uani 1 1 d . . . N14 N 0.5121(8) 0.2090(4) 0.2237(4) 0.0475(18) Uani 1 1 d . . . H14A H 0.5769 0.1995 0.1841 0.057 Uiso 1 1 calc R . . O1 O -0.0528(6) -0.0949(3) 0.3597(3) 0.0406(14) Uani 1 1 d . . . O2 O 0.0052(7) 0.0213(4) 0.2882(3) 0.0653(19) Uani 1 1 d . . . H2 H 0.0343 0.0617 0.2916 0.098 Uiso 1 1 calc R . . O3 O 0.0657(7) 0.1425(3) 0.3026(3) 0.0566(17) Uani 1 1 d . . . O4 O 0.0472(5) 0.2091(3) 0.3916(3) 0.0380(13) Uani 1 1 d . . . Cl1 Cl 0.8537(3) 0.1741(2) 0.08786(14) 0.0787(9) Uani 1 1 d . . . O5 O 0.7144(9) 0.1734(7) 0.0840(6) 0.134(4) Uani 1 1 d . . . O6 O 0.8617(9) 0.1613(6) 0.1658(4) 0.107(3) Uani 1 1 d . . . O7 O 0.8880(10) 0.2528(6) 0.0481(4) 0.110(3) Uani 1 1 d . . . O8 O 0.9465(10) 0.1163(6) 0.0519(5) 0.125(3) Uani 1 1 d . . . Cl2 Cl 0.3385(4) 0.0996(3) 0.0313(2) 0.1166(13) Uani 1 1 d . . . O9 O 0.2661(13) 0.0838(7) 0.1060(7) 0.161(4) Uani 1 1 d U . . O10 O 0.3422(11) 0.0256(6) 0.0035(5) 0.131(3) Uani 1 1 d U . . O11 O 0.3138(18) 0.1646(11) -0.0242(11) 0.241(7) Uani 1 1 d U . . O12 O 0.4636(13) 0.1136(8) 0.0379(7) 0.174(5) Uani 1 1 d U . . Cl3 Cl 0.9037(9) 0.5586(5) 0.0776(4) 0.147(3) Uani 0.50 1 d PD A -1 O13 O 0.9998(19) 0.5195(10) 0.0221(9) 0.175(10) Uani 0.50 1 d PDU A -1 O14 O 0.9173(17) 0.6412(8) 0.0623(8) 0.113(6) Uani 0.50 1 d PDU A -1 O15 O 0.9263(16) 0.5182(8) 0.1511(7) 0.106(5) Uani 0.50 1 d PDU A -1 O16 O 0.7688(16) 0.5521(12) 0.0754(11) 0.232(14) Uani 0.50 1 d PDU A -1 Cl4 Cl 0.5966(11) 0.4588(6) 0.0472(5) 0.173(4) Uani 0.50 1 d PD B -1 O17 O 0.7465(17) 0.4437(11) 0.0200(10) 0.152(8) Uani 0.50 1 d PDU B -1 O18 O 0.534(2) 0.4806(14) -0.0188(11) 0.202(12) Uani 0.50 1 d PDU B -1 O19 O 0.556(2) 0.5246(12) 0.0877(13) 0.268(16) Uani 0.50 1 d PDU B -1 O20 O 0.5547(18) 0.3826(11) 0.0974(10) 0.143(7) Uani 0.50 1 d PDU B -1 O22 O 0.3222(16) 0.6726(10) 0.0628(9) 0.135(6) Uani 0.60 1 d P . . H22A H 0.3902 0.6389 0.0501 0.162 Uiso 0.60 1 d PR . . H22B H 0.2713 0.6792 0.0334 0.162 Uiso 0.60 1 d PR . . O21 O 0.588(2) 0.6754(15) 0.0590(14) 0.131(8) Uani 0.40 1 d P . . H21B H 0.6621 0.6549 0.0355 0.158 Uiso 0.40 1 d PR . . H21A H 0.5420 0.6377 0.0726 0.158 Uiso 0.40 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0338(6) 0.0517(7) 0.0358(5) -0.0150(5) -0.0153(4) -0.0057(5) Cu2 0.0399(7) 0.0384(6) 0.0409(6) 0.0030(5) -0.0083(5) -0.0125(5) C1 0.040(5) 0.071(6) 0.040(5) -0.030(5) 0.004(4) -0.019(5) C2 0.043(6) 0.049(6) 0.040(5) -0.010(4) -0.011(4) -0.014(5) C3 0.038(5) 0.035(5) 0.050(5) -0.016(4) -0.024(4) 0.008(4) C4 0.042(5) 0.051(6) 0.032(4) -0.018(4) -0.011(4) 0.003(5) C5 0.047(6) 0.060(6) 0.039(5) -0.010(5) -0.002(4) -0.006(5) C6 0.059(7) 0.064(7) 0.064(7) 0.002(5) -0.015(5) -0.022(6) C7 0.060(7) 0.052(6) 0.075(7) -0.015(5) -0.023(5) -0.015(5) C8 0.043(6) 0.053(6) 0.042(5) -0.014(4) -0.014(4) -0.014(5) C9 0.062(7) 0.079(7) 0.046(5) -0.008(5) -0.026(5) -0.004(6) C10 0.033(5) 0.058(6) 0.044(5) -0.012(4) -0.015(4) -0.009(5) C11 0.044(6) 0.029(5) 0.049(5) -0.014(4) -0.005(5) -0.005(4) C12 0.048(6) 0.048(6) 0.056(6) -0.018(5) -0.001(5) -0.020(5) C13 0.062(8) 0.044(6) 0.079(7) -0.015(5) 0.004(6) -0.018(6) C14 0.047(8) 0.060(7) 0.136(12) -0.032(8) 0.011(8) -0.010(6) C15 0.044(7) 0.053(7) 0.131(11) -0.035(7) -0.035(7) -0.003(5) C16 0.034(6) 0.039(5) 0.080(7) -0.015(5) -0.012(5) 0.000(4) C17 0.064(7) 0.075(7) 0.049(5) -0.019(5) 0.010(5) -0.034(6) C18 0.031(6) 0.066(7) 0.080(8) -0.019(6) -0.005(5) -0.018(5) C19 0.059(7) 0.044(6) 0.097(8) -0.025(6) -0.018(7) -0.024(5) C20 0.088(9) 0.076(8) 0.138(11) -0.030(8) -0.075(8) -0.020(7) C21 0.101(11) 0.091(10) 0.160(13) -0.023(9) -0.070(11) -0.027(9) C22 0.101(13) 0.091(10) 0.160(14) -0.023(10) -0.070(11) -0.027(9) C23 0.071(10) 0.083(9) 0.172(15) -0.034(10) -0.023(10) -0.025(8) C24 0.062(9) 0.072(8) 0.124(11) -0.019(8) -0.044(8) -0.017(7) C25 0.100(9) 0.049(6) 0.071(7) 0.000(5) -0.053(7) -0.011(6) C26 0.055(7) 0.050(6) 0.070(7) -0.008(5) -0.022(6) -0.007(5) C27 0.058(7) 0.032(5) 0.097(8) 0.006(5) -0.034(7) -0.010(5) C28 0.050(7) 0.050(6) 0.094(8) -0.003(6) -0.024(6) -0.012(5) C29 0.035(7) 0.052(6) 0.127(10) -0.007(6) -0.002(6) -0.012(5) C30 0.043(7) 0.067(8) 0.180(14) -0.025(9) -0.029(9) -0.005(6) C31 0.066(9) 0.061(7) 0.132(11) -0.003(7) -0.054(8) -0.021(7) C32 0.057(8) 0.046(6) 0.106(9) -0.011(6) -0.023(7) -0.011(6) C33 0.105(9) 0.052(6) 0.031(5) 0.005(4) -0.010(5) -0.032(6) C34 0.065(7) 0.036(5) 0.039(5) 0.005(4) -0.011(5) -0.021(5) C35 0.031(5) 0.042(5) 0.062(6) -0.014(5) -0.017(4) -0.002(4) C36 0.046(6) 0.040(5) 0.059(6) -0.008(5) -0.016(5) -0.004(4) C37 0.076(8) 0.063(7) 0.078(7) -0.041(6) -0.022(6) 0.004(6) C38 0.078(8) 0.044(6) 0.102(9) -0.036(6) -0.026(7) -0.010(6) C39 0.077(8) 0.043(6) 0.086(8) -0.008(6) -0.030(6) -0.008(5) C40 0.037(5) 0.037(5) 0.065(6) -0.009(5) -0.019(5) -0.007(4) C41 0.056(7) 0.077(7) 0.035(5) -0.011(5) 0.000(4) -0.027(6) C42 0.042(6) 0.051(6) 0.040(5) -0.003(4) -0.007(4) -0.020(5) C43 0.026(5) 0.044(5) 0.041(5) -0.006(4) 0.005(4) -0.020(4) C44 0.056(6) 0.036(5) 0.049(5) -0.019(4) 0.000(5) -0.008(5) C45 0.069(7) 0.050(6) 0.059(6) -0.012(5) -0.030(6) -0.011(5) C46 0.041(6) 0.061(6) 0.063(6) -0.021(5) -0.015(5) -0.010(5) C47 0.036(6) 0.054(6) 0.079(7) -0.021(5) -0.015(5) -0.004(5) C48 0.048(6) 0.036(5) 0.045(5) -0.005(4) -0.004(4) -0.019(4) C49 0.027(5) 0.033(4) 0.031(4) -0.006(4) -0.012(3) -0.006(4) C50 0.021(4) 0.031(4) 0.034(4) -0.006(3) -0.005(3) -0.006(3) C51 0.031(5) 0.031(4) 0.030(4) -0.006(3) -0.005(3) -0.012(4) C52 0.039(5) 0.044(5) 0.031(4) 0.002(4) -0.016(4) -0.015(4) C53 0.025(5) 0.037(5) 0.028(4) 0.002(4) -0.005(3) -0.012(4) N1 0.033(4) 0.060(5) 0.037(4) -0.014(3) -0.002(3) -0.014(4) N2 0.031(4) 0.048(4) 0.032(4) -0.004(3) -0.007(3) -0.013(3) N3 0.057(5) 0.060(5) 0.042(4) -0.025(4) -0.004(4) -0.029(4) N4 0.035(4) 0.055(4) 0.032(3) -0.009(3) -0.013(3) -0.006(4) N5 0.053(5) 0.059(5) 0.059(5) 0.000(4) -0.038(4) -0.003(4) N6 0.040(5) 0.057(5) 0.071(5) -0.014(4) -0.038(4) -0.001(4) N7 0.049(6) 0.073(6) 0.121(8) -0.028(6) 0.015(6) -0.027(5) N8 0.066(6) 0.046(5) 0.042(4) 0.001(3) -0.024(4) -0.023(4) N9 0.044(5) 0.042(4) 0.055(5) 0.000(4) -0.017(4) -0.006(4) N10 0.088(7) 0.055(5) 0.097(7) -0.001(5) -0.061(6) -0.012(5) N11 0.032(4) 0.031(4) 0.053(4) -0.004(3) -0.016(3) -0.007(3) N12 0.071(6) 0.042(4) 0.033(4) 0.006(3) -0.006(4) -0.016(4) N13 0.041(4) 0.043(4) 0.029(3) -0.004(3) 0.000(3) -0.015(3) N14 0.044(5) 0.052(5) 0.040(4) -0.015(3) 0.010(3) -0.012(4) O1 0.049(4) 0.044(3) 0.035(3) -0.007(3) -0.018(3) -0.012(3) O2 0.106(6) 0.055(4) 0.047(4) 0.001(3) -0.032(4) -0.035(4) O3 0.090(5) 0.052(4) 0.033(3) -0.004(3) -0.007(3) -0.036(4) O4 0.038(3) 0.031(3) 0.043(3) -0.006(3) -0.006(3) -0.009(3) Cl1 0.089(2) 0.095(2) 0.0527(15) -0.0333(16) 0.0079(15) -0.0241(19) O5 0.061(6) 0.226(12) 0.147(8) -0.114(8) 0.013(5) -0.041(7) O6 0.126(7) 0.135(7) 0.052(4) -0.023(5) -0.006(4) -0.017(6) O7 0.151(9) 0.110(7) 0.080(5) -0.015(5) -0.010(5) -0.072(6) O8 0.149(9) 0.136(8) 0.079(5) -0.054(6) -0.013(6) 0.024(7) Cl2 0.139(4) 0.160(4) 0.080(2) -0.027(2) -0.035(2) -0.069(3) O9 0.206(9) 0.177(8) 0.116(7) -0.041(6) -0.028(6) -0.061(7) O10 0.158(7) 0.162(7) 0.114(6) -0.052(5) -0.060(5) -0.044(6) O11 0.261(11) 0.225(10) 0.235(10) 0.019(8) -0.105(9) -0.063(8) O12 0.149(8) 0.224(9) 0.199(8) -0.076(7) -0.071(7) -0.056(7) Cl3 0.180(10) 0.119(7) 0.114(6) 0.005(5) -0.043(6) 0.005(6) O13 0.182(12) 0.171(13) 0.155(13) -0.048(9) -0.024(9) 0.006(9) O14 0.151(10) 0.093(9) 0.122(9) -0.061(7) -0.010(7) -0.056(8) O15 0.132(10) 0.131(10) 0.080(8) -0.050(7) -0.045(7) -0.013(8) O16 0.222(16) 0.244(17) 0.231(16) -0.043(10) -0.064(10) -0.035(10) Cl4 0.194(11) 0.179(10) 0.134(8) -0.045(7) 0.002(7) -0.043(9) O17 0.128(11) 0.172(12) 0.141(11) -0.004(8) -0.045(9) -0.015(9) O18 0.193(15) 0.209(16) 0.194(15) -0.020(9) -0.068(10) -0.011(10) O19 0.273(19) 0.263(18) 0.261(18) -0.059(10) -0.051(10) -0.043(10) O20 0.153(11) 0.140(11) 0.121(10) -0.001(8) -0.019(8) -0.039(9) O22 0.119(13) 0.130(13) 0.141(14) -0.006(11) -0.054(11) 0.013(11) O21 0.14(2) 0.14(2) 0.15(2) -0.056(17) -0.034(17) -0.047(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 N6 1.933(7) . ? Cu1 N4 1.939(6) . ? Cu1 O1 2.021(5) . ? Cu1 N2 2.123(6) . ? Cu1 N1 2.201(6) . ? Cu2 N13 1.945(7) . ? Cu2 N9 1.959(7) . ? Cu2 O4 2.015(5) . ? Cu2 N11 2.032(6) . ? Cu2 N8 2.320(7) . ? C1 N1 1.481(10) . ? C1 C2 1.503(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 N2 1.302(9) . ? C2 N3 1.353(10) . ? C3 C4 1.372(10) . ? C3 N2 1.392(10) . ? C3 C8 1.430(10) . ? C4 C5 1.383(11) . ? C4 H4 0.9400 . ? C5 C6 1.384(12) . ? C5 H5 0.9400 . ? C6 C7 1.411(13) . ? C6 H6 0.9400 . ? C7 C8 1.357(12) . ? C7 H7 0.9400 . ? C8 N3 1.365(10) . ? C9 N1 1.467(10) . ? C9 C10 1.577(12) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 N5 1.287(10) . ? C10 N4 1.341(9) . ? C11 C16 1.377(12) . ? C11 C12 1.394(11) . ? C11 N4 1.396(10) . ? C12 C13 1.361(12) . ? C12 H12 0.9400 . ? C13 C14 1.401(15) . ? C13 H13 0.9400 . ? C14 C15 1.323(15) . ? C14 H14 0.9400 . ? C15 C16 1.378(13) . ? C15 H15 0.9400 . ? C16 N5 1.399(11) . ? C17 C18 1.468(13) . ? C17 N1 1.480(10) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N6 1.325(12) . ? C18 N7 1.368(11) . ? C19 N6 1.382(8) . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9400 . ? C21 C22 1.3900 . ? C21 H21 0.9400 . ? C22 C23 1.3900 . ? C22 H22 0.9400 . ? C23 C24 1.3900 . ? C23 H23 0.9400 . ? C24 N7 1.368(12) . ? C25 N8 1.496(11) . ? C25 C26 1.509(14) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 N9 1.320(11) . ? C26 N10 1.335(12) . ? C27 N9 1.357(9) . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28 0.9400 . ? C29 C30 1.3900 . ? C29 H29 0.9400 . ? C30 C31 1.3900 . ? C30 H30 0.9400 . ? C31 C32 1.3900 . ? C31 H31 0.9400 . ? C32 N10 1.365(11) . ? C33 N8 1.433(10) . ? C33 C34 1.461(11) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 N11 1.297(10) . ? C34 N12 1.361(10) . ? C35 C36 1.362(11) . ? C35 C40 1.420(12) . ? C35 N11 1.443(10) . ? C36 C37 1.361(12) . ? C36 H36 0.9400 . ? C37 C38 1.410(14) . ? C37 H37 0.9400 . ? C38 C39 1.326(14) . ? C38 H38 0.9400 . ? C39 C40 1.369(12) . ? C39 H39 0.9400 . ? C40 N12 1.352(10) . ? C41 N8 1.475(11) . ? C41 C42 1.523(11) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N13 1.327(10) . ? C42 N14 1.337(10) . ? C43 C44 1.372(11) . ? C43 N13 1.407(10) . ? C43 C48 1.441(11) . ? C44 C45 1.374(12) . ? C44 H44 0.9400 . ? C45 C46 1.413(12) . ? C45 H45 0.9400 . ? C46 C47 1.330(12) . ? C46 H46 0.9400 . ? C47 C48 1.385(12) . ? C47 H47 0.9400 . ? C48 N14 1.381(10) . ? C49 C51 1.383(9) 2_556 ? C49 C50 1.432(9) . ? C49 C52 1.480(9) . ? C50 C51 1.402(9) . ? C50 C53 1.520(10) . ? C51 C49 1.383(9) 2_556 ? C51 H51 0.9400 . ? C52 O1 1.232(9) . ? C52 O2 1.302(9) . ? C53 O3 1.248(8) . ? C53 O4 1.261(8) . ? N3 H3 0.8700 . ? N5 H5A 0.8700 . ? N7 H7A 0.8700 . ? N10 H10 0.8700 . ? N12 H12A 0.8700 . ? N14 H14A 0.8700 . ? O2 H2 0.8300 . ? Cl1 O8 1.379(8) . ? Cl1 O7 1.413(8) . ? Cl1 O6 1.425(7) . ? Cl1 O5 1.444(8) . ? Cl2 O11 1.322(16) . ? Cl2 O9 1.369(11) . ? Cl2 O12 1.392(11) . ? Cl2 O10 1.472(9) . ? Cl3 O14 1.388(10) . ? Cl3 O15 1.405(11) . ? Cl3 O13 1.412(11) . ? Cl3 O16 1.417(11) . ? Cl4 O19 1.437(15) . ? Cl4 O20 1.453(14) . ? Cl4 O18 1.458(15) . ? Cl4 O17 1.461(14) . ? O22 H22A 0.8200 . ? O22 H22B 0.8199 . ? O21 H21B 0.8200 . ? O21 H21A 0.8200 . ? 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 N6 Cu1 N4 155.1(3) . . ? N6 Cu1 O1 94.8(3) . . ? N4 Cu1 O1 98.7(2) . . ? N6 Cu1 N2 100.2(3) . . ? N4 Cu1 N2 95.4(3) . . ? O1 Cu1 N2 108.4(2) . . ? N6 Cu1 N1 80.4(3) . . ? N4 Cu1 N1 82.7(2) . . ? O1 Cu1 N1 169.6(2) . . ? N2 Cu1 N1 81.7(2) . . ? N13 Cu2 N9 156.5(3) . . ? N13 Cu2 O4 93.2(2) . . ? N9 Cu2 O4 94.4(3) . . ? N13 Cu2 N11 93.2(3) . . ? N9 Cu2 N11 94.8(3) . . ? O4 Cu2 N11 141.0(2) . . ? N13 Cu2 N8 79.9(3) . . ? N9 Cu2 N8 80.2(3) . . ? O4 Cu2 N8 141.1(2) . . ? N11 Cu2 N8 77.9(3) . . ? N1 C1 C2 111.1(6) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 N3 112.0(7) . . ? N2 C2 C1 123.6(7) . . ? N3 C2 C1 124.4(7) . . ? C4 C3 N2 130.0(7) . . ? C4 C3 C8 121.6(8) . . ? N2 C3 C8 108.3(7) . . ? C3 C4 C5 117.2(8) . . ? C3 C4 H4 121.4 . . ? C5 C4 H4 121.4 . . ? C4 C5 C6 122.2(8) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C7 120.3(9) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 118.4(9) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C7 C8 N3 135.4(8) . . ? C7 C8 C3 120.3(8) . . ? N3 C8 C3 104.2(7) . . ? N1 C9 C10 108.1(6) . . ? N1 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? N1 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N5 C10 N4 113.5(7) . . ? N5 C10 C9 125.9(7) . . ? N4 C10 C9 120.6(7) . . ? C16 C11 C12 121.2(9) . . ? C16 C11 N4 109.3(7) . . ? C12 C11 N4 129.5(8) . . ? C13 C12 C11 115.7(9) . . ? C13 C12 H12 122.2 . . ? C11 C12 H12 122.2 . . ? C12 C13 C14 122.5(10) . . ? C12 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C15 C14 C13 121.0(11) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 118.3(11) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C11 C16 C15 121.2(10) . . ? C11 C16 N5 104.8(7) . . ? C15 C16 N5 133.8(10) . . ? C18 C17 N1 106.3(7) . . ? C18 C17 H17A 110.5 . . ? N1 C17 H17A 110.5 . . ? C18 C17 H17B 110.5 . . ? N1 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? N6 C18 N7 110.2(9) . . ? N6 C18 C17 120.8(8) . . ? N7 C18 C17 129.0(10) . . ? N6 C19 C20 130.8(7) . . ? N6 C19 C24 109.2(7) . . ? C20 C19 C24 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? N7 C24 C23 134.5(7) . . ? N7 C24 C19 105.5(7) . . ? C23 C24 C19 120.0 . . ? N8 C25 C26 108.3(8) . . ? N8 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? N8 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? N9 C26 N10 110.5(9) . . ? N9 C26 C25 121.9(9) . . ? N10 C26 C25 127.6(9) . . ? N9 C27 C28 132.7(6) . . ? N9 C27 C32 107.3(6) . . ? C28 C27 C32 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? N10 C32 C31 133.5(6) . . ? N10 C32 C27 106.5(6) . . ? C31 C32 C27 120.0 . . ? N8 C33 C34 113.1(7) . . ? N8 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? N8 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? N11 C34 N12 112.5(7) . . ? N11 C34 C33 122.7(7) . . ? N12 C34 C33 124.8(7) . . ? C36 C35 C40 121.8(8) . . ? C36 C35 N11 131.6(8) . . ? C40 C35 N11 106.5(7) . . ? C37 C36 C35 118.2(9) . . ? C37 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? C36 C37 C38 119.4(9) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 122.7(9) . . ? C39 C38 H38 118.7 . . ? C37 C38 H38 118.7 . . ? C38 C39 C40 119.2(10) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? N12 C40 C39 135.0(9) . . ? N12 C40 C35 106.3(7) . . ? C39 C40 C35 118.6(9) . . ? N8 C41 C42 108.3(7) . . ? N8 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? N8 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? N13 C42 N14 111.4(7) . . ? N13 C42 C41 120.3(8) . . ? N14 C42 C41 128.1(8) . . ? C44 C43 N13 132.1(8) . . ? C44 C43 C48 119.9(8) . . ? N13 C43 C48 108.0(6) . . ? C43 C44 C45 118.7(8) . . ? C43 C44 H44 120.7 . . ? C45 C44 H44 120.7 . . ? C44 C45 C46 120.5(8) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C47 C46 C45 122.0(9) . . ? C47 C46 H46 119.0 . . ? C45 C46 H46 119.0 . . ? C46 C47 C48 118.9(9) . . ? C46 C47 H47 120.6 . . ? C48 C47 H47 120.6 . . ? N14 C48 C47 136.3(8) . . ? N14 C48 C43 103.6(7) . . ? C47 C48 C43 120.0(8) . . ? C51 C49 C50 116.6(6) 2_556 . ? C51 C49 C52 116.0(6) 2_556 . ? C50 C49 C52 127.4(7) . . ? C51 C50 C49 116.9(6) . . ? C51 C50 C53 116.0(6) . . ? C49 C50 C53 127.1(6) . . ? C49 C51 C50 126.5(7) 2_556 . ? C49 C51 H51 116.7 2_556 . ? C50 C51 H51 116.7 . . ? O1 C52 O2 117.5(7) . . ? O1 C52 C49 119.1(7) . . ? O2 C52 C49 123.1(7) . . ? O3 C53 O4 121.6(7) . . ? O3 C53 C50 120.8(7) . . ? O4 C53 C50 117.6(6) . . ? C9 N1 C17 112.2(7) . . ? C9 N1 C1 111.7(7) . . ? C17 N1 C1 111.6(7) . . ? C9 N1 Cu1 110.1(5) . . ? C17 N1 Cu1 103.3(5) . . ? C1 N1 Cu1 107.5(5) . . ? C2 N2 C3 106.5(6) . . ? C2 N2 Cu1 110.8(5) . . ? C3 N2 Cu1 141.0(5) . . ? C2 N3 C8 109.0(6) . . ? C2 N3 H3 125.5 . . ? C8 N3 H3 125.5 . . ? C10 N4 C11 104.0(6) . . ? C10 N4 Cu1 116.5(5) . . ? C11 N4 Cu1 139.3(5) . . ? C10 N5 C16 108.3(7) . . ? C10 N5 H5A 125.8 . . ? C16 N5 H5A 125.8 . . ? C18 N6 C19 106.7(8) . . ? C18 N6 Cu1 114.3(6) . . ? C19 N6 Cu1 138.6(7) . . ? C18 N7 C24 108.4(8) . . ? C18 N7 H7A 125.8 . . ? C24 N7 H7A 125.8 . . ? C33 N8 C41 115.0(8) . . ? C33 N8 C25 114.2(7) . . ? C41 N8 C25 112.1(7) . . ? C33 N8 Cu2 108.1(5) . . ? C41 N8 Cu2 103.6(5) . . ? C25 N8 Cu2 102.2(6) . . ? C26 N9 C27 108.0(7) . . ? C26 N9 Cu2 115.9(6) . . ? C27 N9 Cu2 136.0(6) . . ? C26 N10 C32 107.7(8) . . ? C26 N10 H10 126.2 . . ? C32 N10 H10 126.2 . . ? C34 N11 C35 105.9(7) . . ? C34 N11 Cu2 117.3(5) . . ? C35 N11 Cu2 136.0(6) . . ? C40 N12 C34 108.8(7) . . ? C40 N12 H12A 125.6 . . ? C34 N12 H12A 125.6 . . ? C42 N13 C43 106.5(7) . . ? C42 N13 Cu2 117.4(6) . . ? C43 N13 Cu2 136.0(5) . . ? C42 N14 C48 110.4(7) . . ? C42 N14 H14A 124.8 . . ? C48 N14 H14A 124.8 . . ? C52 O1 Cu1 114.1(5) . . ? C52 O2 H2 109.5 . . ? C53 O4 Cu2 110.3(4) . . ? O8 Cl1 O7 107.5(6) . . ? O8 Cl1 O6 111.6(5) . . ? O7 Cl1 O6 108.4(5) . . ? O8 Cl1 O5 111.1(6) . . ? O7 Cl1 O5 108.0(7) . . ? O6 Cl1 O5 110.1(5) . . ? O11 Cl2 O9 127.6(11) . . ? O11 Cl2 O12 98.6(9) . . ? O9 Cl2 O12 102.7(8) . . ? O11 Cl2 O10 107.0(9) . . ? O9 Cl2 O10 104.9(7) . . ? O12 Cl2 O10 116.8(8) . . ? O14 Cl3 O15 110.0(6) . . ? O14 Cl3 O13 110.0(6) . . ? O15 Cl3 O13 109.5(6) . . ? O14 Cl3 O16 110.0(6) . . ? O15 Cl3 O16 108.6(6) . . ? O13 Cl3 O16 108.7(6) . . ? O19 Cl4 O20 110.7(6) . . ? O19 Cl4 O18 110.2(6) . . ? O20 Cl4 O18 109.1(6) . . ? O19 Cl4 O17 110.3(6) . . ? O20 Cl4 O17 107.9(6) . . ? O18 Cl4 O17 108.5(6) . . ? H22A O22 H22B 107.7 . . ? H21B O21 H21A 103.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -26.0(11) . . . . ? N1 C1 C2 N3 155.5(7) . . . . ? N2 C3 C4 C5 176.5(8) . . . . ? C8 C3 C4 C5 0.1(12) . . . . ? C3 C4 C5 C6 -0.6(13) . . . . ? C4 C5 C6 C7 0.5(14) . . . . ? C5 C6 C7 C8 0.1(14) . . . . ? C6 C7 C8 N3 -175.1(10) . . . . ? C6 C7 C8 C3 -0.6(13) . . . . ? C4 C3 C8 C7 0.5(12) . . . . ? N2 C3 C8 C7 -176.6(8) . . . . ? C4 C3 C8 N3 176.5(7) . . . . ? N2 C3 C8 N3 -0.6(9) . . . . ? N1 C9 C10 N5 -167.7(8) . . . . ? N1 C9 C10 N4 13.1(11) . . . . ? C16 C11 C12 C13 -0.6(12) . . . . ? N4 C11 C12 C13 -179.1(8) . . . . ? C11 C12 C13 C14 2.9(13) . . . . ? C12 C13 C14 C15 -3.1(16) . . . . ? C13 C14 C15 C16 0.6(16) . . . . ? C12 C11 C16 C15 -1.7(13) . . . . ? N4 C11 C16 C15 177.1(8) . . . . ? C12 C11 C16 N5 -177.5(7) . . . . ? N4 C11 C16 N5 1.4(9) . . . . ? C14 C15 C16 C11 1.7(15) . . . . ? C14 C15 C16 N5 176.0(10) . . . . ? N1 C17 C18 N6 -33.2(12) . . . . ? N1 C17 C18 N7 146.7(9) . . . . ? N6 C19 C20 C21 179.5(7) . . . . ? C24 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 N7 178.9(9) . . . . ? C22 C23 C24 C19 0.0 . . . . ? N6 C19 C24 N7 1.3(6) . . . . ? C20 C19 C24 N7 -179.2(7) . . . . ? N6 C19 C24 C23 -179.6(6) . . . . ? C20 C19 C24 C23 0.0 . . . . ? N8 C25 C26 N9 -29.7(12) . . . . ? N8 C25 C26 N10 149.1(9) . . . . ? N9 C27 C28 C29 178.9(7) . . . . ? C32 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 N10 178.4(8) . . . . ? C30 C31 C32 C27 0.0 . . . . ? N9 C27 C32 N10 2.0(6) . . . . ? C28 C27 C32 N10 -178.8(6) . . . . ? N9 C27 C32 C31 -179.2(6) . . . . ? C28 C27 C32 C31 0.0 . . . . ? N8 C33 C34 N11 -11.7(14) . . . . ? N8 C33 C34 N12 169.9(8) . . . . ? C40 C35 C36 C37 -1.4(13) . . . . ? N11 C35 C36 C37 179.3(8) . . . . ? C35 C36 C37 C38 0.4(14) . . . . ? C36 C37 C38 C39 -0.5(16) . . . . ? C37 C38 C39 C40 1.7(16) . . . . ? C38 C39 C40 N12 -177.9(10) . . . . ? C38 C39 C40 C35 -2.5(14) . . . . ? C36 C35 C40 N12 179.1(8) . . . . ? N11 C35 C40 N12 -1.4(9) . . . . ? C36 C35 C40 C39 2.5(13) . . . . ? N11 C35 C40 C39 -178.0(7) . . . . ? N8 C41 C42 N13 31.3(11) . . . . ? N8 C41 C42 N14 -154.8(8) . . . . ? N13 C43 C44 C45 -178.9(8) . . . . ? C48 C43 C44 C45 1.5(12) . . . . ? C43 C44 C45 C46 0.0(13) . . . . ? C44 C45 C46 C47 -0.3(14) . . . . ? C45 C46 C47 C48 -1.0(14) . . . . ? C46 C47 C48 N14 179.1(9) . . . . ? C46 C47 C48 C43 2.5(13) . . . . ? C44 C43 C48 N14 179.6(7) . . . . ? N13 C43 C48 N14 -0.1(8) . . . . ? C44 C43 C48 C47 -2.8(12) . . . . ? N13 C43 C48 C47 177.5(7) . . . . ? C51 C49 C50 C51 0.0(11) 2_556 . . . ? C52 C49 C50 C51 -179.3(7) . . . . ? C51 C49 C50 C53 177.8(7) 2_556 . . . ? C52 C49 C50 C53 -1.5(12) . . . . ? C49 C50 C51 C49 0.0(12) . . . 2_556 ? C53 C50 C51 C49 -178.0(7) . . . 2_556 ? C51 C49 C52 O1 2.8(11) 2_556 . . . ? C50 C49 C52 O1 -177.9(7) . . . . ? C51 C49 C52 O2 -171.0(7) 2_556 . . . ? C50 C49 C52 O2 8.3(12) . . . . ? C51 C50 C53 O3 165.1(7) . . . . ? C49 C50 C53 O3 -12.6(11) . . . . ? C51 C50 C53 O4 -12.0(10) . . . . ? C49 C50 C53 O4 170.3(7) . . . . ? C10 C9 N1 C17 -128.9(7) . . . . ? C10 C9 N1 C1 104.9(8) . . . . ? C10 C9 N1 Cu1 -14.5(8) . . . . ? C18 C17 N1 C9 157.1(7) . . . . ? C18 C17 N1 C1 -76.6(8) . . . . ? C18 C17 N1 Cu1 38.6(8) . . . . ? C2 C1 N1 C9 -97.7(8) . . . . ? C2 C1 N1 C17 135.7(7) . . . . ? C2 C1 N1 Cu1 23.1(8) . . . . ? N6 Cu1 N1 C9 -150.4(6) . . . . ? N4 Cu1 N1 C9 11.1(6) . . . . ? O1 Cu1 N1 C9 -87.1(14) . . . . ? N2 Cu1 N1 C9 107.7(6) . . . . ? N6 Cu1 N1 C17 -30.4(6) . . . . ? N4 Cu1 N1 C17 131.1(6) . . . . ? O1 Cu1 N1 C17 32.9(16) . . . . ? N2 Cu1 N1 C17 -132.3(6) . . . . ? N6 Cu1 N1 C1 87.6(5) . . . . ? N4 Cu1 N1 C1 -110.8(5) . . . . ? O1 Cu1 N1 C1 151.0(12) . . . . ? N2 Cu1 N1 C1 -14.2(5) . . . . ? N3 C2 N2 C3 -0.3(9) . . . . ? C1 C2 N2 C3 -179.0(7) . . . . ? N3 C2 N2 Cu1 -168.5(5) . . . . ? C1 C2 N2 Cu1 12.8(10) . . . . ? C4 C3 N2 C2 -176.2(8) . . . . ? C8 C3 N2 C2 0.5(9) . . . . ? C4 C3 N2 Cu1 -13.9(14) . . . . ? C8 C3 N2 Cu1 162.9(6) . . . . ? N6 Cu1 N2 C2 -77.0(6) . . . . ? N4 Cu1 N2 C2 83.4(6) . . . . ? O1 Cu1 N2 C2 -175.5(5) . . . . ? N1 Cu1 N2 C2 1.7(5) . . . . ? N6 Cu1 N2 C3 121.1(8) . . . . ? N4 Cu1 N2 C3 -78.4(8) . . . . ? O1 Cu1 N2 C3 22.6(8) . . . . ? N1 Cu1 N2 C3 -160.2(8) . . . . ? N2 C2 N3 C8 0.0(10) . . . . ? C1 C2 N3 C8 178.6(8) . . . . ? C7 C8 N3 C2 175.5(10) . . . . ? C3 C8 N3 C2 0.4(9) . . . . ? N5 C10 N4 C11 0.9(9) . . . . ? C9 C10 N4 C11 -179.9(8) . . . . ? N5 C10 N4 Cu1 176.9(6) . . . . ? C9 C10 N4 Cu1 -3.9(10) . . . . ? C16 C11 N4 C10 -1.4(9) . . . . ? C12 C11 N4 C10 177.3(8) . . . . ? C16 C11 N4 Cu1 -175.9(6) . . . . ? C12 C11 N4 Cu1 2.8(14) . . . . ? N6 Cu1 N4 C10 43.8(10) . . . . ? O1 Cu1 N4 C10 165.6(6) . . . . ? N2 Cu1 N4 C10 -84.8(6) . . . . ? N1 Cu1 N4 C10 -4.0(6) . . . . ? N6 Cu1 N4 C11 -142.2(8) . . . . ? O1 Cu1 N4 C11 -20.4(8) . . . . ? N2 Cu1 N4 C11 89.2(8) . . . . ? N1 Cu1 N4 C11 170.1(8) . . . . ? N4 C10 N5 C16 0.0(10) . . . . ? C9 C10 N5 C16 -179.2(8) . . . . ? C11 C16 N5 C10 -0.8(10) . . . . ? C15 C16 N5 C10 -175.8(10) . . . . ? N7 C18 N6 C19 0.2(10) . . . . ? C17 C18 N6 C19 -179.9(8) . . . . ? N7 C18 N6 Cu1 -174.1(6) . . . . ? C17 C18 N6 Cu1 5.8(11) . . . . ? C20 C19 N6 C18 179.6(6) . . . . ? C24 C19 N6 C18 -0.9(8) . . . . ? C20 C19 N6 Cu1 -8.3(11) . . . . ? C24 C19 N6 Cu1 171.2(6) . . . . ? N4 Cu1 N6 C18 -33.5(11) . . . . ? O1 Cu1 N6 C18 -156.1(7) . . . . ? N2 Cu1 N6 C18 94.2(7) . . . . ? N1 Cu1 N6 C18 14.6(7) . . . . ? N4 Cu1 N6 C19 154.8(7) . . . . ? O1 Cu1 N6 C19 32.2(8) . . . . ? N2 Cu1 N6 C19 -77.5(8) . . . . ? N1 Cu1 N6 C19 -157.1(8) . . . . ? N6 C18 N7 C24 0.6(11) . . . . ? C17 C18 N7 C24 -179.3(9) . . . . ? C23 C24 N7 C18 179.9(6) . . . . ? C19 C24 N7 C18 -1.1(8) . . . . ? C34 C33 N8 C41 -107.6(9) . . . . ? C34 C33 N8 C25 120.6(9) . . . . ? C34 C33 N8 Cu2 7.6(10) . . . . ? C42 C41 N8 C33 85.2(8) . . . . ? C42 C41 N8 C25 -142.0(7) . . . . ? C42 C41 N8 Cu2 -32.5(7) . . . . ? C26 C25 N8 C33 -82.9(9) . . . . ? C26 C25 N8 C41 143.9(7) . . . . ? C26 C25 N8 Cu2 33.6(8) . . . . ? N13 Cu2 N8 C33 -98.4(6) . . . . ? N9 Cu2 N8 C33 94.2(6) . . . . ? O4 Cu2 N8 C33 179.1(5) . . . . ? N11 Cu2 N8 C33 -2.8(6) . . . . ? N13 Cu2 N8 C41 24.1(5) . . . . ? N9 Cu2 N8 C41 -143.3(5) . . . . ? O4 Cu2 N8 C41 -58.4(7) . . . . ? N11 Cu2 N8 C41 119.6(5) . . . . ? N13 Cu2 N8 C25 140.8(6) . . . . ? N9 Cu2 N8 C25 -26.6(5) . . . . ? O4 Cu2 N8 C25 58.3(7) . . . . ? N11 Cu2 N8 C25 -123.7(6) . . . . ? N10 C26 N9 C27 2.7(10) . . . . ? C25 C26 N9 C27 -178.2(8) . . . . ? N10 C26 N9 Cu2 -174.4(6) . . . . ? C25 C26 N9 Cu2 4.6(11) . . . . ? C28 C27 N9 C26 178.1(6) . . . . ? C32 C27 N9 C26 -2.9(7) . . . . ? C28 C27 N9 Cu2 -5.6(11) . . . . ? C32 C27 N9 Cu2 173.4(5) . . . . ? N13 Cu2 N9 C26 -19.7(11) . . . . ? O4 Cu2 N9 C26 -128.1(6) . . . . ? N11 Cu2 N9 C26 89.8(7) . . . . ? N8 Cu2 N9 C26 13.0(6) . . . . ? N13 Cu2 N9 C27 164.2(6) . . . . ? O4 Cu2 N9 C27 55.8(8) . . . . ? N11 Cu2 N9 C27 -86.3(8) . . . . ? N8 Cu2 N9 C27 -163.1(8) . . . . ? N9 C26 N10 C32 -1.5(10) . . . . ? C25 C26 N10 C32 179.6(9) . . . . ? C31 C32 N10 C26 -179.0(6) . . . . ? C27 C32 N10 C26 -0.4(8) . . . . ? N12 C34 N11 C35 -0.6(10) . . . . ? C33 C34 N11 C35 -179.2(8) . . . . ? N12 C34 N11 Cu2 -172.2(5) . . . . ? C33 C34 N11 Cu2 9.2(12) . . . . ? C36 C35 N11 C34 -179.3(9) . . . . ? C40 C35 N11 C34 1.3(9) . . . . ? C36 C35 N11 Cu2 -10.2(13) . . . . ? C40 C35 N11 Cu2 170.4(6) . . . . ? N13 Cu2 N11 C34 75.9(6) . . . . ? N9 Cu2 N11 C34 -82.0(6) . . . . ? O4 Cu2 N11 C34 175.0(5) . . . . ? N8 Cu2 N11 C34 -3.1(6) . . . . ? N13 Cu2 N11 C35 -92.3(7) . . . . ? N9 Cu2 N11 C35 109.8(7) . . . . ? O4 Cu2 N11 C35 6.7(9) . . . . ? N8 Cu2 N11 C35 -171.3(8) . . . . ? C39 C40 N12 C34 176.9(10) . . . . ? C35 C40 N12 C34 1.1(9) . . . . ? N11 C34 N12 C40 -0.3(10) . . . . ? C33 C34 N12 C40 178.3(9) . . . . ? N14 C42 N13 C43 -0.9(9) . . . . ? C41 C42 N13 C43 173.9(7) . . . . ? N14 C42 N13 Cu2 176.1(5) . . . . ? C41 C42 N13 Cu2 -9.1(10) . . . . ? C44 C43 N13 C42 -179.0(8) . . . . ? C48 C43 N13 C42 0.6(9) . . . . ? C44 C43 N13 Cu2 4.8(14) . . . . ? C48 C43 N13 Cu2 -175.5(5) . . . . ? N9 Cu2 N13 C42 23.9(10) . . . . ? O4 Cu2 N13 C42 132.5(6) . . . . ? N11 Cu2 N13 C42 -86.0(6) . . . . ? N8 Cu2 N13 C42 -8.9(6) . . . . ? N9 Cu2 N13 C43 -160.3(7) . . . . ? O4 Cu2 N13 C43 -51.6(7) . . . . ? N11 Cu2 N13 C43 89.9(7) . . . . ? N8 Cu2 N13 C43 167.0(8) . . . . ? N13 C42 N14 C48 0.9(10) . . . . ? C41 C42 N14 C48 -173.4(8) . . . . ? C47 C48 N14 C42 -177.4(9) . . . . ? C43 C48 N14 C42 -0.5(9) . . . . ? O2 C52 O1 Cu1 4.0(9) . . . . ? C49 C52 O1 Cu1 -170.1(5) . . . . ? N6 Cu1 O1 C52 72.9(6) . . . . ? N4 Cu1 O1 C52 -86.0(6) . . . . ? N2 Cu1 O1 C52 175.3(5) . . . . ? N1 Cu1 O1 C52 10.8(16) . . . . ? O3 C53 O4 Cu2 -5.8(9) . . . . ? C50 C53 O4 Cu2 171.3(5) . . . . ? N13 Cu2 O4 C53 -80.2(5) . . . . ? N9 Cu2 O4 C53 77.6(5) . . . . ? N11 Cu2 O4 C53 -179.3(5) . . . . ? N8 Cu2 O4 C53 -2.3(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O3 0.83 1.55 2.377(8) 171.4 . N3 H3 O14 0.87 2.17 2.983(14) 154.4 1_445 N3 H3 O15 0.87 2.29 3.031(14) 143.8 1_445 N5 H5A O10 0.87 2.30 3.056(11) 144.7 2 N7 H7A O12 0.87 2.48 3.333(17) 166.6 2_655 N10 H10 O17 0.87 2.34 3.144(19) 153.9 1_455 N12 H12A O22 0.87 2.28 3.069(17) 150.0 . N14 H14A O5 0.87 2.09 2.956(10) 173.2 . O22 H22A O18 0.82 2.18 2.90(3) 146.3 2_665 O22 H22B O7 0.82 2.41 3.194(17) 160.0 2_665 C1 H1A O22 0.98 2.49 3.407(18) 155.3 1_545 C9 H9B O8 0.98 2.38 3.256(14) 148.0 1_455 C15 H15 O9 0.94 2.60 3.502(17) 161.4 1_455 C33 H33A O13 0.98 2.43 3.41(2) 174.2 1_455 C33 H33A O15 0.98 2.47 3.147(19) 125.7 1_455 C33 H33B O20 0.98 2.45 3.31(2) 146.0 . C41 H41B O9 0.98 2.47 3.405(14) 159.6 . C47 H47 O6 0.94 2.53 3.303(12) 140.1 . C51 H51 O1 0.94 2.30 2.690(8) 103.9 2_556 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.085 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.128 _vrf_PLAT430_9 ; PROBLEM: Short Inter D...A Contact O16 .. O19 .. 2.26 Ang. RESPONSE: This is due to the disorder of these perchlorate anions. ; _vrf_PLAT420_9 ; PROBLEM: D-H Without Acceptor >O22 - >H22A ... ? RESPONSE: According to the hydrogen bonding invironment, O22-H22A...O19 (O22...O19=3.087\%A) weak interactions should be considered. ; # END