data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 loop_ _publ_author_name 'Israel Goldberg' 'Goutam Kumar Patra' _publ_contact_author_name 'Prof Israel Goldberg' _publ_contact_author_address ; School of Chemistry Tel-Aviv University Ramat-Aviv Tel-Aviv 69978 ISRAEL ; _publ_contact_author_email GOLDBERG@POST.TAU.AC.IL _publ_section_title ; The synthesis and characterization of new bis-bidentate Schiff base ligands and their supramolecular complexes with silver(I), copper(I) and zinc(II) d10 metal ions ; #======END============================================================ data_Ligand-1 _database_code_CSD 204782 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H18 N4' _chemical_formula_weight 338.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7590(2) _cell_length_b 7.4030(2) _cell_length_c 17.3190(5) _cell_angle_alpha 78.2670(12) _cell_angle_beta 87.2810(13) _cell_angle_gamma 85.4210(16) _cell_volume 845.34(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2333 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 28.23 _exptl_crystal_description prisms _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 0.081 _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 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3868 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 28.23 _reflns_number_total 3868 _reflns_number_gt 2333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0893P)^2^+0.0309P] 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 3868 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1673 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.4010(2) 0.28844(18) 0.75255(8) 0.0196(3) Uani 1 1 d . . . C2 C 0.5651(2) 0.3043(2) 0.70245(10) 0.0187(4) Uani 1 1 d . . . C3 C 0.5459(3) 0.4205(2) 0.62763(10) 0.0245(4) Uani 1 1 d . . . H3 H 0.4219 0.4854 0.6131 0.029 Uiso 1 1 calc R . . C4 C 0.7051(3) 0.4401(3) 0.57594(11) 0.0272(4) Uani 1 1 d . . . H4 H 0.6909 0.5175 0.5253 0.033 Uiso 1 1 calc R . . C5 C 0.8910(3) 0.3462(2) 0.59715(11) 0.0267(4) Uani 1 1 d . . . H5 H 1.0007 0.3615 0.5606 0.032 Uiso 1 1 calc R . . C6 C 0.9147(3) 0.2339(2) 0.66945(11) 0.0235(4) Uani 1 1 d . . . H6 H 1.0408 0.1727 0.6832 0.028 Uiso 1 1 calc R . . C7 C 0.7514(2) 0.2083(2) 0.72409(10) 0.0180(4) Uani 1 1 d . . . C8 C 0.7629(2) 0.0934(2) 0.80019(10) 0.0198(4) Uani 1 1 d . . . H8 H 0.8848 0.0271 0.8168 0.024 Uiso 1 1 calc R . . C9 C 0.5998(2) 0.0780(2) 0.84951(10) 0.0192(4) Uani 1 1 d . . . H9 H 0.6058 0.0011 0.9006 0.023 Uiso 1 1 calc R . . C10 C 0.4200(2) 0.1796(2) 0.82289(10) 0.0181(4) Uani 1 1 d . . . C11 C 0.2390(2) 0.1747(2) 0.87385(10) 0.0203(4) Uani 1 1 d . . . H11 H 0.1242 0.2494 0.8543 0.024 Uiso 1 1 calc R . . N12 N 0.22946(19) 0.07517(19) 0.94258(8) 0.0207(4) Uani 1 1 d . . . C13 C 0.0431(2) 0.0929(2) 0.98767(10) 0.0214(4) Uani 1 1 d . . . H13A H -0.0526 0.1809 0.9550 0.026 Uiso 1 1 calc R . . H13B H 0.0674 0.1425 1.0351 0.026 Uiso 1 1 calc R . . N1' N 0.09206(19) 0.33336(18) 0.25981(8) 0.0183(3) Uani 1 1 d . . . C2' C -0.0650(2) 0.2533(2) 0.30293(10) 0.0176(4) Uani 1 1 d . . . C3' C -0.0524(3) 0.2025(2) 0.38554(10) 0.0232(4) Uani 1 1 d . . . H3' H 0.0627 0.2266 0.4102 0.028 Uiso 1 1 calc R . . C4' C -0.2034(3) 0.1193(2) 0.43061(11) 0.0257(4) Uani 1 1 d . . . H4' H -0.1931 0.0859 0.4863 0.031 Uiso 1 1 calc R . . C5' C -0.3755(3) 0.0827(2) 0.39455(11) 0.0269(4) Uani 1 1 d . . . H5' H -0.4794 0.0232 0.4263 0.032 Uiso 1 1 calc R . . C6' C -0.3939(2) 0.1318(2) 0.31503(11) 0.0231(4) Uani 1 1 d . . . H6' H -0.5113 0.1088 0.2917 0.028 Uiso 1 1 calc R . . C7' C -0.2387(2) 0.2171(2) 0.26684(10) 0.0177(4) Uani 1 1 d . . . C8' C -0.2468(2) 0.2695(2) 0.18389(10) 0.0189(4) Uani 1 1 d . . . H8' H -0.3604 0.2478 0.1578 0.023 Uiso 1 1 calc R . . C9' C -0.0917(2) 0.3510(2) 0.14145(10) 0.0177(4) Uani 1 1 d . . . H9' H -0.0962 0.3889 0.0857 0.021 Uiso 1 1 calc R . . C10' C 0.0779(2) 0.3783(2) 0.18254(10) 0.0172(4) Uani 1 1 d . . . C11' C 0.2546(2) 0.4566(2) 0.13900(10) 0.0183(4) Uani 1 1 d . . . H11' H 0.3591 0.4871 0.1677 0.022 Uiso 1 1 calc R . . N12' N 0.27095(19) 0.48427(18) 0.06431(8) 0.0198(4) Uani 1 1 d . . . C13' C 0.4526(2) 0.5613(2) 0.02700(10) 0.0195(4) Uani 1 1 d . . . H13C H 0.5466 0.5698 0.0680 0.023 Uiso 1 1 calc R . . H13D H 0.4210 0.6875 -0.0039 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0206(8) 0.0181(7) 0.0211(8) -0.0048(6) -0.0012(6) -0.0041(6) C2 0.0197(9) 0.0161(8) 0.0219(10) -0.0062(7) -0.0012(7) -0.0037(7) C3 0.0262(10) 0.0224(9) 0.0242(10) -0.0020(7) -0.0043(8) -0.0013(8) C4 0.0336(10) 0.0279(10) 0.0197(10) -0.0017(8) -0.0012(8) -0.0077(8) C5 0.0263(10) 0.0285(10) 0.0260(11) -0.0065(8) 0.0069(8) -0.0077(8) C6 0.0198(9) 0.0215(9) 0.0305(11) -0.0086(8) 0.0014(8) -0.0014(7) C7 0.0190(8) 0.0145(8) 0.0220(10) -0.0063(7) -0.0007(7) -0.0027(7) C8 0.0178(8) 0.0160(8) 0.0266(10) -0.0059(7) -0.0045(7) -0.0005(7) C9 0.0217(9) 0.0144(8) 0.0215(9) -0.0025(7) -0.0024(7) -0.0022(7) C10 0.0188(9) 0.0146(8) 0.0225(10) -0.0064(7) -0.0001(7) -0.0040(7) C11 0.0182(9) 0.0172(8) 0.0274(10) -0.0084(7) -0.0004(8) -0.0026(7) N12 0.0188(7) 0.0197(7) 0.0233(8) -0.0040(6) 0.0021(6) -0.0022(6) C13 0.0189(9) 0.0206(9) 0.0245(10) -0.0056(7) 0.0041(7) 0.0003(7) N1' 0.0185(7) 0.0158(7) 0.0203(8) -0.0037(6) 0.0009(6) -0.0007(6) C2' 0.0191(8) 0.0147(8) 0.0191(9) -0.0038(7) -0.0004(7) -0.0015(7) C3' 0.0246(9) 0.0217(9) 0.0240(10) -0.0055(7) -0.0021(8) -0.0030(7) C4' 0.0301(10) 0.0258(9) 0.0201(10) -0.0027(7) 0.0027(8) -0.0024(8) C5' 0.0266(10) 0.0254(9) 0.0284(11) -0.0043(8) 0.0077(8) -0.0077(8) C6' 0.0206(9) 0.0203(8) 0.0287(11) -0.0055(7) 0.0015(8) -0.0035(7) C7' 0.0193(9) 0.0128(8) 0.0214(9) -0.0052(7) 0.0001(7) 0.0004(7) C8' 0.0172(8) 0.0151(8) 0.0250(10) -0.0059(7) -0.0027(7) 0.0014(7) C9' 0.0184(8) 0.0155(8) 0.0190(9) -0.0043(7) 0.0006(7) 0.0012(7) C10' 0.0181(8) 0.0130(8) 0.0207(9) -0.0053(7) 0.0008(7) 0.0015(7) C11' 0.0162(8) 0.0145(8) 0.0245(10) -0.0051(7) -0.0016(7) 0.0003(7) N12' 0.0177(7) 0.0176(7) 0.0234(9) -0.0029(6) 0.0022(6) -0.0010(6) C13' 0.0177(8) 0.0184(8) 0.0221(10) -0.0031(7) 0.0007(7) -0.0035(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C10 1.322(2) . ? N1 C2 1.373(2) . ? C2 C3 1.407(2) . ? C2 C7 1.423(2) . ? C3 C4 1.364(2) . ? C3 H3 0.9500 . ? C4 C5 1.413(3) . ? C4 H4 0.9500 . ? C5 C6 1.364(2) . ? C5 H5 0.9500 . ? C6 C7 1.418(2) . ? C6 H6 0.9500 . ? C7 C8 1.418(2) . ? C8 C9 1.360(2) . ? C8 H8 0.9500 . ? C9 C10 1.422(2) . ? C9 H9 0.9500 . ? C10 C11 1.472(2) . ? C11 N12 1.268(2) . ? C11 H11 0.9500 . ? N12 C13 1.461(2) . ? C13 C13 1.511(3) 2_557 ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? N1' C10' 1.318(2) . ? N1' C2' 1.3718(19) . ? C2' C3' 1.408(2) . ? C2' C7' 1.424(2) . ? C3' C4' 1.364(2) . ? C3' H3' 0.9500 . ? C4' C5' 1.416(3) . ? C4' H4' 0.9500 . ? C5' C6' 1.360(2) . ? C5' H5' 0.9500 . ? C6' C7' 1.416(2) . ? C6' H6' 0.9500 . ? C7' C8' 1.412(2) . ? C8' C9' 1.361(2) . ? C8' H8' 0.9500 . ? C9' C10' 1.426(2) . ? C9' H9' 0.9500 . ? C10' C11' 1.476(2) . ? C11' N12' 1.269(2) . ? C11' H11' 0.9500 . ? N12' C13' 1.4618(19) . ? C13' C13' 1.518(3) 2_665 ? C13' H13C 0.9900 . ? C13' H13D 0.9900 . ? 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 C10 N1 C2 117.90(14) . . ? N1 C2 C3 118.13(15) . . ? N1 C2 C7 122.12(15) . . ? C3 C2 C7 119.75(15) . . ? C4 C3 C2 120.07(17) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.56(16) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 120.74(16) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 120.12(16) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 123.72(15) . . ? C8 C7 C2 117.52(15) . . ? C6 C7 C2 118.75(15) . . ? C9 C8 C7 120.09(15) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 118.45(15) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N1 C10 C9 123.91(15) . . ? N1 C10 C11 114.49(15) . . ? C9 C10 C11 121.58(15) . . ? N12 C11 C10 122.97(16) . . ? N12 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? C11 N12 C13 116.57(15) . . ? N12 C13 C13 110.28(18) . 2_557 ? N12 C13 H13A 109.6 . . ? C13 C13 H13A 109.6 2_557 . ? N12 C13 H13B 109.6 . . ? C13 C13 H13B 109.6 2_557 . ? H13A C13 H13B 108.1 . . ? C10' N1' C2' 117.78(14) . . ? N1' C2' C3' 118.76(15) . . ? N1' C2' C7' 122.21(15) . . ? C3' C2' C7' 119.02(14) . . ? C4' C3' C2' 120.76(16) . . ? C4' C3' H3' 119.6 . . ? C2' C3' H3' 119.6 . . ? C3' C4' C5' 120.10(17) . . ? C3' C4' H4' 119.9 . . ? C5' C4' H4' 119.9 . . ? C6' C5' C4' 120.73(16) . . ? C6' C5' H5' 119.6 . . ? C4' C5' H5' 119.6 . . ? C5' C6' C7' 120.28(16) . . ? C5' C6' H6' 119.9 . . ? C7' C6' H6' 119.9 . . ? C8' C7' C6' 123.24(15) . . ? C8' C7' C2' 117.67(14) . . ? C6' C7' C2' 119.09(16) . . ? C9' C8' C7' 119.90(15) . . ? C9' C8' H8' 120.0 . . ? C7' C8' H8' 120.0 . . ? C8' C9' C10' 118.48(16) . . ? C8' C9' H9' 120.8 . . ? C10' C9' H9' 120.8 . . ? N1' C10' C9' 123.94(14) . . ? N1' C10' C11' 115.36(14) . . ? C9' C10' C11' 120.68(15) . . ? N12' C11' C10' 121.89(15) . . ? N12' C11' H11' 119.1 . . ? C10' C11' H11' 119.1 . . ? C11' N12' C13' 117.54(14) . . ? N12' C13' C13' 109.77(16) . 2_665 ? N12' C13' H13C 109.7 . . ? C13' C13' H13C 109.7 2_665 . ? N12' C13' H13D 109.7 . . ? C13' C13' H13D 109.7 2_665 . ? H13C C13' H13D 108.2 . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.340 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.060 #=====END====================================================== #=====END====================================================== data_Ligand-2 _database_code_CSD 204783 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C34 H24 N6), (C H2 Cl2)' _chemical_formula_sum 'C35 H26 Cl2 N6' _chemical_formula_weight 601.52 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.73700(10) _cell_length_b 11.4350(2) _cell_length_c 14.9620(3) _cell_angle_alpha 91.4540(6) _cell_angle_beta 102.7070(7) _cell_angle_gamma 112.4550(13) _cell_volume 1490.79(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4463 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.29 _exptl_crystal_description 'parallelpiped rods' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9164 _exptl_absorpt_correction_T_max 0.9629 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6977 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6977 _reflns_number_gt 4463 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+0.4491P] 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 6977 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.47644(17) -0.10282(15) 0.38496(11) 0.0184(4) Uani 1 1 d . . . C2 C 0.3501(2) -0.10942(18) 0.41441(14) 0.0192(4) Uani 1 1 d . . . C3 C 0.2930(2) -0.2038(2) 0.47151(15) 0.0234(5) Uani 1 1 d . . . H3 H 0.3427 -0.2598 0.4889 0.028 Uiso 1 1 calc R . . C4 C 0.1663(2) -0.2147(2) 0.50188(16) 0.0305(5) Uani 1 1 d . . . H4 H 0.1288 -0.2780 0.5404 0.037 Uiso 1 1 calc R . . C5 C 0.0911(3) -0.1324(2) 0.47636(17) 0.0326(5) Uani 1 1 d . . . H5 H 0.0035 -0.1405 0.4980 0.039 Uiso 1 1 calc R . . C6 C 0.1429(2) -0.0414(2) 0.42087(16) 0.0285(5) Uani 1 1 d . . . H6 H 0.0904 0.0127 0.4036 0.034 Uiso 1 1 calc R . . C7 C 0.2743(2) -0.02657(19) 0.38872(14) 0.0216(4) Uani 1 1 d . . . C8 C 0.3335(2) 0.06511(19) 0.33070(15) 0.0231(4) Uani 1 1 d . . . H8 H 0.2861 0.1224 0.3121 0.028 Uiso 1 1 calc R . . C9 C 0.4584(2) 0.07138(19) 0.30139(14) 0.0210(4) Uani 1 1 d . . . H9 H 0.4989 0.1325 0.2621 0.025 Uiso 1 1 calc R . . C10 C 0.5275(2) -0.01493(18) 0.33046(14) 0.0182(4) Uani 1 1 d . . . C11 C 0.6604(2) -0.01192(18) 0.29832(13) 0.0179(4) Uani 1 1 d . . . H11 H 0.7051 -0.0711 0.3160 0.021 Uiso 1 1 calc R . . N12 N 0.71518(18) 0.07119(16) 0.24630(12) 0.0205(4) Uani 1 1 d . . . N13 N 0.83543(18) 0.05819(15) 0.21547(12) 0.0197(4) Uani 1 1 d . . . C14 C 0.9026(2) 0.15325(18) 0.17422(13) 0.0160(4) Uani 1 1 d . . . C15 C 0.8572(2) 0.26632(18) 0.16617(14) 0.0171(4) Uani 1 1 d . . . N16 N 0.92086(18) 0.36363(16) 0.22868(11) 0.0196(4) Uani 1 1 d . . . N17 N 1.03303(18) 0.34829(16) 0.29907(12) 0.0204(4) Uani 1 1 d . . . C18 C 1.0729(2) 0.42265(18) 0.37357(14) 0.0192(4) Uani 1 1 d . . . H18 H 1.0270 0.4817 0.3784 0.023 Uiso 1 1 calc R . . C19 C 1.1896(2) 0.41651(18) 0.45173(14) 0.0175(4) Uani 1 1 d . . . C20 C 1.2567(2) 0.32711(19) 0.44464(15) 0.0211(4) Uani 1 1 d . . . H20 H 1.2268 0.2714 0.3893 0.025 Uiso 1 1 calc R . . C21 C 1.3649(2) 0.32231(19) 0.51840(15) 0.0223(4) Uani 1 1 d . . . H21 H 1.4087 0.2614 0.5156 0.027 Uiso 1 1 calc R . . C22 C 1.4109(2) 0.40911(18) 0.59890(14) 0.0200(4) Uani 1 1 d . . . C23 C 1.5280(2) 0.4160(2) 0.67674(15) 0.0258(5) Uani 1 1 d . . . H23 H 1.5764 0.3579 0.6772 0.031 Uiso 1 1 calc R . . C24 C 1.5719(2) 0.5053(2) 0.75097(16) 0.0308(5) Uani 1 1 d . . . H24 H 1.6534 0.5113 0.8018 0.037 Uiso 1 1 calc R . . C25 C 1.4968(3) 0.5889(2) 0.75263(16) 0.0316(5) Uani 1 1 d . . . H25 H 1.5274 0.6500 0.8050 0.038 Uiso 1 1 calc R . . C26 C 1.3805(2) 0.5831(2) 0.67975(15) 0.0276(5) Uani 1 1 d . . . H26 H 1.3292 0.6385 0.6824 0.033 Uiso 1 1 calc R . . C27 C 1.3367(2) 0.49461(19) 0.60050(14) 0.0197(4) Uani 1 1 d . . . N28 N 1.22495(18) 0.49621(15) 0.52688(12) 0.0201(4) Uani 1 1 d . . . C29 C 1.0238(2) 0.15136(18) 0.13062(13) 0.0171(4) Uani 1 1 d . . . C30 C 1.0931(2) 0.24948(19) 0.08130(14) 0.0218(4) Uani 1 1 d . . . H30 H 1.0649 0.3204 0.0772 0.026 Uiso 1 1 calc R . . C31 C 1.2032(2) 0.2438(2) 0.03815(16) 0.0266(5) Uani 1 1 d . . . H31 H 1.2497 0.3106 0.0043 0.032 Uiso 1 1 calc R . . C32 C 1.2454(2) 0.1410(2) 0.04433(15) 0.0260(5) Uani 1 1 d . . . H32 H 1.3211 0.1375 0.0149 0.031 Uiso 1 1 calc R . . C33 C 1.1774(2) 0.0435(2) 0.09339(15) 0.0256(5) Uani 1 1 d . . . H33 H 1.2071 -0.0267 0.0978 0.031 Uiso 1 1 calc R . . C34 C 1.0666(2) 0.0473(2) 0.13613(15) 0.0224(4) Uani 1 1 d . . . H34 H 1.0196 -0.0205 0.1692 0.027 Uiso 1 1 calc R . . C35 C 0.7445(2) 0.26585(19) 0.08217(14) 0.0186(4) Uani 1 1 d . . . C36 C 0.7124(3) 0.3731(2) 0.06320(16) 0.0282(5) Uani 1 1 d . . . H36 H 0.7586 0.4472 0.1071 0.034 Uiso 1 1 calc R . . C37 C 0.6135(3) 0.3716(2) -0.01938(17) 0.0326(5) Uani 1 1 d . . . H37 H 0.5919 0.4448 -0.0315 0.039 Uiso 1 1 calc R . . C38 C 0.5458(2) 0.2650(2) -0.08448(15) 0.0272(5) Uani 1 1 d . . . H38 H 0.4799 0.2655 -0.1415 0.033 Uiso 1 1 calc R . . C39 C 0.5749(2) 0.1577(2) -0.06588(15) 0.0248(5) Uani 1 1 d . . . H39 H 0.5276 0.0836 -0.1098 0.030 Uiso 1 1 calc R . . C40 C 0.6731(2) 0.15810(19) 0.01683(14) 0.0207(4) Uani 1 1 d . . . H40 H 0.6920 0.0838 0.0292 0.025 Uiso 1 1 calc R . . C41 C 0.9799(3) -0.3283(2) 0.25058(17) 0.0327(5) Uani 1 1 d . . . H41A H 0.9345 -0.4215 0.2529 0.039 Uiso 1 1 calc R . . H41B H 1.0386 -0.2867 0.3138 0.039 Uiso 1 1 calc R . . Cl42 Cl 0.83176(7) -0.27523(6) 0.21337(5) 0.0466(2) Uani 1 1 d . . . Cl43 Cl 1.10603(8) -0.29476(7) 0.17761(6) 0.0545(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0175(8) 0.0183(9) 0.0181(9) 0.0017(7) 0.0052(7) 0.0055(7) C2 0.0176(9) 0.0196(10) 0.0182(11) -0.0010(8) 0.0036(8) 0.0056(8) C3 0.0211(10) 0.0237(11) 0.0238(12) 0.0037(9) 0.0076(9) 0.0061(8) C4 0.0287(11) 0.0307(13) 0.0282(13) 0.0031(10) 0.0119(10) 0.0051(10) C5 0.0263(11) 0.0308(13) 0.0408(15) -0.0027(11) 0.0183(10) 0.0065(10) C6 0.0236(11) 0.0242(11) 0.0395(14) -0.0027(10) 0.0112(10) 0.0100(9) C7 0.0207(10) 0.0191(10) 0.0221(11) -0.0050(8) 0.0038(8) 0.0062(8) C8 0.0258(10) 0.0195(10) 0.0268(12) 0.0002(9) 0.0044(9) 0.0134(9) C9 0.0236(10) 0.0182(10) 0.0226(12) 0.0039(9) 0.0057(8) 0.0097(8) C10 0.0181(9) 0.0179(10) 0.0169(11) -0.0004(8) 0.0027(8) 0.0065(8) C11 0.0189(9) 0.0168(10) 0.0179(11) 0.0024(8) 0.0035(8) 0.0076(8) N12 0.0196(8) 0.0219(9) 0.0223(10) 0.0022(7) 0.0068(7) 0.0100(7) N13 0.0186(8) 0.0210(9) 0.0220(9) 0.0033(7) 0.0079(7) 0.0091(7) C14 0.0156(9) 0.0176(10) 0.0126(10) -0.0007(8) -0.0004(7) 0.0066(7) C15 0.0155(9) 0.0173(10) 0.0193(11) 0.0025(8) 0.0053(8) 0.0068(8) N16 0.0188(8) 0.0217(9) 0.0176(9) 0.0001(7) 0.0013(7) 0.0092(7) N17 0.0189(8) 0.0209(9) 0.0187(9) -0.0002(7) -0.0005(7) 0.0080(7) C18 0.0200(9) 0.0175(10) 0.0211(11) 0.0027(8) 0.0052(8) 0.0086(8) C19 0.0175(9) 0.0151(10) 0.0183(11) 0.0027(8) 0.0047(8) 0.0046(7) C20 0.0215(10) 0.0194(10) 0.0221(11) -0.0003(8) 0.0037(8) 0.0091(8) C21 0.0219(10) 0.0205(11) 0.0270(12) 0.0025(9) 0.0067(9) 0.0107(8) C22 0.0173(9) 0.0178(10) 0.0224(11) 0.0050(8) 0.0045(8) 0.0046(8) C23 0.0239(10) 0.0230(11) 0.0281(13) 0.0064(9) 0.0021(9) 0.0091(9) C24 0.0278(11) 0.0311(12) 0.0255(13) 0.0075(10) -0.0037(9) 0.0087(10) C25 0.0385(13) 0.0272(12) 0.0216(12) -0.0031(10) -0.0013(10) 0.0100(10) C26 0.0331(12) 0.0231(11) 0.0238(12) -0.0018(9) 0.0018(9) 0.0114(9) C27 0.0191(9) 0.0193(10) 0.0182(11) 0.0025(8) 0.0032(8) 0.0058(8) N28 0.0205(8) 0.0187(9) 0.0193(9) 0.0010(7) 0.0030(7) 0.0071(7) C29 0.0150(9) 0.0180(10) 0.0151(10) 0.0002(8) 0.0011(7) 0.0047(7) C30 0.0212(10) 0.0197(10) 0.0238(12) 0.0008(9) 0.0060(8) 0.0071(8) C31 0.0243(10) 0.0232(11) 0.0285(13) 0.0019(9) 0.0092(9) 0.0040(9) C32 0.0209(10) 0.0294(12) 0.0287(13) -0.0023(10) 0.0088(9) 0.0098(9) C33 0.0253(10) 0.0263(11) 0.0294(13) 0.0019(9) 0.0071(9) 0.0148(9) C34 0.0231(10) 0.0230(11) 0.0241(12) 0.0053(9) 0.0071(8) 0.0116(8) C35 0.0178(9) 0.0219(10) 0.0178(11) 0.0025(8) 0.0044(8) 0.0096(8) C36 0.0341(12) 0.0209(11) 0.0268(13) -0.0001(9) -0.0009(9) 0.0129(9) C37 0.0343(12) 0.0286(13) 0.0361(14) 0.0094(11) 0.0009(10) 0.0178(10) C38 0.0224(10) 0.0362(13) 0.0209(12) 0.0063(10) 0.0011(8) 0.0117(9) C39 0.0220(10) 0.0301(12) 0.0187(11) -0.0029(9) 0.0012(8) 0.0091(9) C40 0.0179(9) 0.0215(11) 0.0227(11) -0.0007(9) 0.0027(8) 0.0094(8) C41 0.0388(13) 0.0233(12) 0.0312(14) 0.0010(10) -0.0014(10) 0.0129(10) Cl42 0.0432(4) 0.0485(4) 0.0581(5) 0.0242(3) 0.0153(3) 0.0265(3) Cl43 0.0501(4) 0.0526(4) 0.0691(5) 0.0120(4) 0.0245(4) 0.0238(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C10 1.327(2) . ? N1 C2 1.372(2) . ? C2 C3 1.414(3) . ? C2 C7 1.420(3) . ? C3 C4 1.370(3) . ? C3 H3 0.9500 . ? C4 C5 1.410(3) . ? C4 H4 0.9500 . ? C5 C6 1.362(3) . ? C5 H5 0.9500 . ? C6 C7 1.417(3) . ? C6 H6 0.9500 . ? C7 C8 1.410(3) . ? C8 C9 1.359(3) . ? C8 H8 0.9500 . ? C9 C10 1.420(3) . ? C9 H9 0.9500 . ? C10 C11 1.466(3) . ? C11 N12 1.275(2) . ? C11 H11 0.9500 . ? N12 N13 1.405(2) . ? N13 C14 1.288(2) . ? C14 C29 1.475(3) . ? C14 C15 1.517(2) . ? C15 N16 1.289(2) . ? C15 C35 1.474(3) . ? N16 N17 1.408(2) . ? N17 C18 1.275(3) . ? C18 C19 1.465(3) . ? C18 H18 0.9500 . ? C19 N28 1.323(3) . ? C19 C20 1.421(3) . ? C20 C21 1.366(3) . ? C20 H20 0.9500 . ? C21 C22 1.414(3) . ? C21 H21 0.9500 . ? C22 C23 1.416(3) . ? C22 C27 1.423(3) . ? C23 C24 1.364(3) . ? C23 H23 0.9500 . ? C24 C25 1.410(3) . ? C24 H24 0.9500 . ? C25 C26 1.368(3) . ? C25 H25 0.9500 . ? C26 C27 1.414(3) . ? C26 H26 0.9500 . ? C27 N28 1.373(2) . ? C29 C30 1.393(3) . ? C29 C34 1.402(3) . ? C30 C31 1.388(3) . ? C30 H30 0.9500 . ? C31 C32 1.385(3) . ? C31 H31 0.9500 . ? C32 C33 1.383(3) . ? C32 H32 0.9500 . ? C33 C34 1.383(3) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.394(3) . ? C35 C36 1.397(3) . ? C36 C37 1.385(3) . ? C36 H36 0.9500 . ? C37 C38 1.383(3) . ? C37 H37 0.9500 . ? C38 C39 1.383(3) . ? C38 H38 0.9500 . ? C39 C40 1.386(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 Cl42 1.758(2) . ? C41 Cl43 1.760(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? 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 C10 N1 C2 117.53(16) . . ? N1 C2 C3 118.23(17) . . ? N1 C2 C7 122.49(17) . . ? C3 C2 C7 119.27(17) . . ? C4 C3 C2 120.3(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.5(2) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 120.50(19) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 120.7(2) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 123.56(19) . . ? C8 C7 C2 117.58(17) . . ? C6 C7 C2 118.85(19) . . ? C9 C8 C7 119.89(18) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 118.93(18) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N1 C10 C9 123.58(17) . . ? N1 C10 C11 116.38(16) . . ? C9 C10 C11 120.03(17) . . ? N12 C11 C10 119.17(17) . . ? N12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 N12 N13 113.37(16) . . ? C14 N13 N12 111.92(15) . . ? N13 C14 C29 119.58(17) . . ? N13 C14 C15 121.90(16) . . ? C29 C14 C15 118.49(16) . . ? N16 C15 C35 120.37(17) . . ? N16 C15 C14 121.24(17) . . ? C35 C15 C14 118.30(16) . . ? C15 N16 N17 110.97(15) . . ? C18 N17 N16 114.49(15) . . ? N17 C18 C19 119.65(17) . . ? N17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? N28 C19 C20 123.64(18) . . ? N28 C19 C18 116.35(16) . . ? C20 C19 C18 120.01(18) . . ? C21 C20 C19 119.18(19) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 119.23(18) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C21 C22 C23 123.25(18) . . ? C21 C22 C27 117.88(18) . . ? C23 C22 C27 118.86(19) . . ? C24 C23 C22 120.63(19) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.3(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 120.8(2) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 120.0(2) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? N28 C27 C26 118.28(17) . . ? N28 C27 C22 122.39(18) . . ? C26 C27 C22 119.32(18) . . ? C19 N28 C27 117.60(16) . . ? C30 C29 C34 119.27(17) . . ? C30 C29 C14 121.05(17) . . ? C34 C29 C14 119.64(17) . . ? C31 C30 C29 120.16(19) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 120.2(2) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C33 C32 C31 119.95(19) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.52(19) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C33 C34 C29 119.90(19) . . ? C33 C34 H34 120.1 . . ? C29 C34 H34 120.1 . . ? C40 C35 C36 118.39(18) . . ? C40 C35 C15 119.55(17) . . ? C36 C35 C15 121.97(18) . . ? C37 C36 C35 120.2(2) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 120.8(2) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 119.5(2) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C38 C39 C40 120.0(2) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C35 121.04(18) . . ? C39 C40 H40 119.5 . . ? C35 C40 H40 119.5 . . ? Cl42 C41 Cl43 112.36(13) . . ? Cl42 C41 H41A 109.1 . . ? Cl43 C41 H41A 109.1 . . ? Cl42 C41 H41B 109.1 . . ? Cl43 C41 H41B 109.1 . . ? H41A C41 H41B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.295 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.062 #=====END=========================================================== data_Ligand-3 _database_code_CSD 204784 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H18 N4 . 2(C H Cl3)' _chemical_formula_sum 'C28 H20 Cl6 N4' _chemical_formula_weight 625.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.23400(10) _cell_length_b 9.3440(2) _cell_length_c 12.6120(3) _cell_angle_alpha 70.9570(9) _cell_angle_beta 77.6140(9) _cell_angle_gamma 84.1600(15) _cell_volume 677.89(2) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2712 _cell_measurement_theta_min 3.30 _cell_measurement_theta_max 28.17 _exptl_crystal_description rods _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 318 _exptl_absorpt_coefficient_mu 0.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7552 _exptl_absorpt_correction_T_max 0.9368 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3162 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 28.17 _reflns_number_total 3162 _reflns_number_gt 2712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+0.3897P] 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 3162 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.48844(7) -0.35172(5) 0.29672(4) 0.03013(12) Uani 1 1 d . . . Cl2 Cl 0.85229(6) -0.34823(5) 0.40607(4) 0.02757(11) Uani 1 1 d . . . Cl3 Cl 0.41822(7) -0.23591(5) 0.48915(4) 0.03290(12) Uani 1 1 d . . . N1 N 0.70500(18) 0.09804(13) 0.22539(10) 0.0144(2) Uani 1 1 d . . . C2 C 0.8573(2) 0.17248(16) 0.24992(12) 0.0138(3) Uani 1 1 d . . . C3 C 0.9814(2) 0.08953(17) 0.33323(12) 0.0171(3) Uani 1 1 d . . . H3 H 0.9569 -0.0151 0.3712 0.020 Uiso 1 1 calc R . . C5 C 1.1747(2) 0.31479(17) 0.30442(13) 0.0195(3) Uani 1 1 d . . . H5 H 1.2814 0.3623 0.3240 0.023 Uiso 1 1 calc R . . C4 C 1.1373(2) 0.15939(17) 0.35958(13) 0.0190(3) Uani 1 1 d . . . H4 H 1.2204 0.1025 0.4154 0.023 Uiso 1 1 calc R . . C6 C 1.0577(2) 0.39782(17) 0.22256(13) 0.0183(3) Uani 1 1 d . . . H6 H 1.0847 0.5024 0.1855 0.022 Uiso 1 1 calc R . . C7 C 0.8971(2) 0.32882(16) 0.19282(12) 0.0148(3) Uani 1 1 d . . . C8 C 0.7760(2) 0.40717(16) 0.10628(13) 0.0173(3) Uani 1 1 d . . . H8 H 0.7960 0.5120 0.0670 0.021 Uiso 1 1 calc R . . C9 C 0.6306(2) 0.33029(16) 0.08022(13) 0.0166(3) Uani 1 1 d . . . H9 H 0.5525 0.3799 0.0205 0.020 Uiso 1 1 calc R . . C10 C 0.5975(2) 0.17540(15) 0.14337(12) 0.0139(3) Uani 1 1 d . . . C11 C 0.4370(2) 0.09025(16) 0.11981(12) 0.0154(3) Uani 1 1 d . . . H11 H 0.4228 -0.0148 0.1600 0.018 Uiso 1 1 calc R . . N12 N 0.31665(18) 0.15512(13) 0.04622(10) 0.0151(2) Uani 1 1 d . . . C13 C 0.1596(2) 0.07097(16) 0.02697(12) 0.0134(3) Uani 1 1 d . . . C14 C 0.0947(2) -0.07487(16) 0.09507(12) 0.0162(3) Uani 1 1 d . . . H14 H 0.1579 -0.1263 0.1601 0.019 Uiso 1 1 calc R . . C15 C -0.0620(2) -0.14404(16) 0.06730(12) 0.0156(3) Uani 1 1 d . . . H15 H -0.1040 -0.2435 0.1135 0.019 Uiso 1 1 calc R . . C16 C 0.6069(2) -0.25400(17) 0.36797(13) 0.0205(3) Uani 1 1 d . . . H16 H 0.6430 -0.1502 0.3144 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0346(2) 0.0259(2) 0.0331(2) -0.00723(17) -0.01182(17) -0.01080(16) Cl2 0.0239(2) 0.0272(2) 0.0308(2) -0.00690(17) -0.00927(15) 0.00377(15) Cl3 0.0300(2) 0.0354(2) 0.0297(2) -0.01033(19) -0.00095(16) 0.00499(17) N1 0.0129(5) 0.0144(6) 0.0165(6) -0.0050(5) -0.0030(4) -0.0025(4) C2 0.0118(6) 0.0152(7) 0.0151(7) -0.0063(5) -0.0011(5) -0.0018(5) C3 0.0188(7) 0.0159(7) 0.0154(7) -0.0027(6) -0.0035(5) -0.0026(5) C5 0.0174(7) 0.0232(8) 0.0219(8) -0.0105(6) -0.0049(6) -0.0047(6) C4 0.0183(7) 0.0233(8) 0.0164(7) -0.0056(6) -0.0061(5) -0.0016(6) C6 0.0195(7) 0.0157(7) 0.0216(8) -0.0067(6) -0.0047(6) -0.0039(5) C7 0.0139(6) 0.0147(7) 0.0168(7) -0.0067(6) -0.0023(5) -0.0011(5) C8 0.0177(7) 0.0122(7) 0.0217(8) -0.0036(6) -0.0052(5) -0.0019(5) C9 0.0163(7) 0.0142(7) 0.0197(7) -0.0039(6) -0.0069(5) 0.0001(5) C10 0.0128(6) 0.0135(7) 0.0168(7) -0.0062(5) -0.0031(5) -0.0006(5) C11 0.0130(6) 0.0138(7) 0.0201(7) -0.0059(6) -0.0032(5) -0.0020(5) N12 0.0131(6) 0.0158(6) 0.0178(6) -0.0070(5) -0.0023(4) -0.0029(4) C13 0.0104(6) 0.0147(7) 0.0166(7) -0.0071(5) -0.0020(5) -0.0010(5) C14 0.0154(7) 0.0167(7) 0.0170(7) -0.0037(6) -0.0064(5) -0.0012(5) C15 0.0161(7) 0.0129(6) 0.0173(7) -0.0037(5) -0.0029(5) -0.0021(5) C16 0.0223(7) 0.0168(7) 0.0218(8) -0.0029(6) -0.0065(6) -0.0026(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 Cl1 C16 1.7731(16) . ? Cl2 C16 1.7640(15) . ? Cl3 C16 1.7620(16) . ? N1 C10 1.3240(18) . ? N1 C2 1.3717(17) . ? C2 C3 1.4137(19) . ? C2 C7 1.4230(19) . ? C3 C4 1.375(2) . ? C3 H3 0.9500 . ? C5 C6 1.373(2) . ? C5 C4 1.410(2) . ? C5 H5 0.9500 . ? C4 H4 0.9500 . ? C6 C7 1.4176(19) . ? C6 H6 0.9500 . ? C7 C8 1.420(2) . ? C8 C9 1.364(2) . ? C8 H8 0.9500 . ? C9 C10 1.4177(19) . ? C9 H9 0.9500 . ? C10 C11 1.4714(18) . ? C11 N12 1.2773(18) . ? C11 H11 0.9500 . ? N12 C13 1.4208(17) . ? C13 C15 1.3948(19) 2 ? C13 C14 1.399(2) . ? C14 C15 1.3848(19) . ? C14 H14 0.9500 . ? C15 C13 1.3948(19) 2 ? C15 H15 0.9500 . ? C16 H16 1.0000 . ? 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 C10 N1 C2 117.85(12) . . ? N1 C2 C3 118.52(12) . . ? N1 C2 C7 122.24(12) . . ? C3 C2 C7 119.23(12) . . ? C4 C3 C2 120.41(13) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C6 C5 C4 120.34(13) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C3 C4 C5 120.49(13) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C5 C6 C7 120.53(14) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C8 123.24(13) . . ? C6 C7 C2 119.00(13) . . ? C8 C7 C2 117.75(12) . . ? C9 C8 C7 119.29(13) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 119.16(13) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N1 C10 C9 123.66(13) . . ? N1 C10 C11 115.75(12) . . ? C9 C10 C11 120.59(12) . . ? N12 C11 C10 121.15(13) . . ? N12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 N12 C13 119.99(12) . . ? C15 C13 C14 118.72(12) 2 . ? C15 C13 N12 115.72(12) 2 . ? C14 C13 N12 125.55(13) . . ? C15 C14 C13 119.79(13) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C13 121.49(13) . 2 ? C14 C15 H15 119.3 . . ? C13 C15 H15 119.3 2 . ? Cl3 C16 Cl2 111.01(8) . . ? Cl3 C16 Cl1 110.28(8) . . ? Cl2 C16 Cl1 110.38(8) . . ? Cl3 C16 H16 108.4 . . ? Cl2 C16 H16 108.4 . . ? Cl1 C16 H16 108.4 . . ? 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 C10 N1 C2 C3 -176.84(13) . . . . ? C10 N1 C2 C7 1.9(2) . . . . ? N1 C2 C3 C4 179.35(13) . . . . ? C7 C2 C3 C4 0.6(2) . . . . ? C2 C3 C4 C5 0.4(2) . . . . ? C6 C5 C4 C3 -0.9(2) . . . . ? C4 C5 C6 C7 0.4(2) . . . . ? C5 C6 C7 C8 -177.81(14) . . . . ? C5 C6 C7 C2 0.6(2) . . . . ? N1 C2 C7 C6 -179.78(13) . . . . ? C3 C2 C7 C6 -1.1(2) . . . . ? N1 C2 C7 C8 -1.3(2) . . . . ? C3 C2 C7 C8 177.42(13) . . . . ? C6 C7 C8 C9 177.46(14) . . . . ? C2 C7 C8 C9 -1.0(2) . . . . ? C7 C8 C9 C10 2.5(2) . . . . ? C2 N1 C10 C9 -0.2(2) . . . . ? C2 N1 C10 C11 179.61(12) . . . . ? C8 C9 C10 N1 -2.0(2) . . . . ? C8 C9 C10 C11 178.17(13) . . . . ? N1 C10 C11 N12 176.71(13) . . . . ? C9 C10 C11 N12 -3.4(2) . . . . ? C10 C11 N12 C13 -178.60(12) . . . . ? C11 N12 C13 C15 -169.84(13) . . . 2 ? C11 N12 C13 C14 11.4(2) . . . . ? C15 C13 C14 C15 0.7(2) 2 . . . ? N12 C13 C14 C15 179.45(13) . . . . ? C13 C14 C15 C13 -0.7(2) . . . 2 ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.17 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.321 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.055 #=======END======================================================== data_Complex-1a _database_code_CSD 204785 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C22 H18 N4), (Ag Cl O4), (C2 H3 N)' _chemical_formula_sum 'C24 H21 Ag Cl N5 O4' _chemical_formula_weight 586.78 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' Ag Ag -0.8971 1.1015 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.1870(3) _cell_length_b 13.8900(2) _cell_length_c 20.1180(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.4500(7) _cell_angle_gamma 90.00 _cell_volume 4848.27(14) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4409 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 27.89 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 0.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7249 _exptl_absorpt_correction_T_max 0.9081 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5748 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.89 _reflns_number_total 5748 _reflns_number_gt 4409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+2.2330P] 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 5748 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.051 _refine_ls_shift/su_mean 0.002 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 Ag Ag 0.012555(11) 0.091912(14) -0.165001(11) 0.02116(8) Uani 1 1 d . . . N1 N 0.04138(13) 0.25839(15) -0.16550(11) 0.0181(5) Uani 1 1 d . . . C2 C -0.00165(15) 0.33639(19) -0.15957(13) 0.0185(5) Uani 1 1 d . . . C3 C -0.07640(15) 0.32198(19) -0.15365(14) 0.0212(6) Uani 1 1 d . . . H3 H -0.0950 0.2584 -0.1518 0.025 Uiso 1 1 calc R . . C4 C -0.12207(17) 0.3991(2) -0.15058(16) 0.0267(6) Uani 1 1 d . . . H4 H -0.1724 0.3887 -0.1472 0.032 Uiso 1 1 calc R . . C5 C -0.09481(18) 0.4941(2) -0.15247(17) 0.0330(7) Uani 1 1 d . . . H5 H -0.1268 0.5471 -0.1498 0.040 Uiso 1 1 calc R . . C6 C -0.02321(19) 0.5100(2) -0.15807(17) 0.0322(7) Uani 1 1 d . . . H6 H -0.0057 0.5742 -0.1598 0.039 Uiso 1 1 calc R . . C7 C 0.02559(17) 0.4318(2) -0.16141(14) 0.0251(6) Uani 1 1 d . . . C8 C 0.09990(17) 0.4446(2) -0.16832(15) 0.0278(6) Uani 1 1 d . . . H8 H 0.1200 0.5075 -0.1695 0.033 Uiso 1 1 calc R . . C9 C 0.14247(16) 0.3657(2) -0.17334(15) 0.0254(6) Uani 1 1 d . . . H9 H 0.1928 0.3729 -0.1776 0.031 Uiso 1 1 calc R . . C10 C 0.11106(15) 0.27336(19) -0.17212(14) 0.0206(6) Uani 1 1 d . . . C11 C 0.15517(16) 0.1880(2) -0.18124(14) 0.0222(6) Uani 1 1 d . . . H11 H 0.2044 0.1971 -0.1877 0.027 Uiso 1 1 calc R . . N12 N 0.13011(12) 0.10282(15) -0.18086(11) 0.0182(5) Uani 1 1 d . . . C13 C 0.17690(15) 0.0240(2) -0.19402(14) 0.0232(6) Uani 1 1 d . . . H13A H 0.2001 -0.0116 -0.1501 0.028 Uiso 1 1 calc R . . H13B H 0.2194 0.0508 -0.2097 0.028 Uiso 1 1 calc R . . C14 C -0.12988(16) -0.04515(19) -0.25110(14) 0.0231(6) Uani 1 1 d . . . H14A H -0.1636 -0.0972 -0.2434 0.028 Uiso 1 1 calc R . . H14B H -0.0889 -0.0748 -0.2675 0.028 Uiso 1 1 calc R . . N15 N -0.09503(12) 0.00609(15) -0.18565(11) 0.0183(5) Uani 1 1 d . . . C16 C -0.12557(15) -0.00208(18) -0.13710(14) 0.0215(6) Uani 1 1 d . . . H16 H -0.1692 -0.0427 -0.1438 0.026 Uiso 1 1 calc R . . C17 C -0.09531(15) 0.04965(19) -0.07033(14) 0.0212(6) Uani 1 1 d . . . C18 C -0.13675(18) 0.0484(2) -0.02127(16) 0.0319(7) Uani 1 1 d . . . H18 H -0.1836 0.0134 -0.0305 0.038 Uiso 1 1 calc R . . C19 C -0.1085(2) 0.0981(2) 0.03966(16) 0.0361(8) Uani 1 1 d . . . H19 H -0.1361 0.0986 0.0730 0.043 Uiso 1 1 calc R . . C20 C -0.03863(19) 0.1483(2) 0.05301(15) 0.0302(7) Uani 1 1 d . . . C21 C -0.0042(2) 0.1996(2) 0.11559(17) 0.0435(9) Uani 1 1 d . . . H21 H -0.0292 0.2020 0.1508 0.052 Uiso 1 1 calc R . . C22 C 0.0642(3) 0.2452(2) 0.12530(17) 0.0457(10) Uani 1 1 d . . . H22 H 0.0869 0.2787 0.1676 0.055 Uiso 1 1 calc R . . C23 C 0.1017(2) 0.2434(2) 0.07376(17) 0.0409(8) Uani 1 1 d . . . H23 H 0.1492 0.2765 0.0813 0.049 Uiso 1 1 calc R . . C24 C 0.07041(19) 0.1945(2) 0.01270(16) 0.0325(7) Uani 1 1 d . . . H24 H 0.0963 0.1937 -0.0219 0.039 Uiso 1 1 calc R . . C25 C 0.00010(17) 0.14535(19) 0.00114(14) 0.0243(6) Uani 1 1 d . . . N26 N -0.02921(13) 0.09586(14) -0.05964(11) 0.0187(5) Uani 1 1 d . . . Cl Cl 0.30015(4) 0.20687(5) 0.67952(4) 0.02408(15) Uani 1 1 d . . . O1 O 0.38202(12) 0.19414(16) 0.70090(11) 0.0347(5) Uani 1 1 d . . . O2 O 0.27584(14) 0.23861(16) 0.73759(12) 0.0411(6) Uani 1 1 d . . . O3 O 0.26466(14) 0.11721(18) 0.65410(16) 0.0578(8) Uani 1 1 d . . . O4 O 0.28038(16) 0.27948(19) 0.62665(14) 0.0553(7) Uani 1 1 d . . . N27 N 0.70017(18) 0.0398(2) 0.52544(17) 0.0490(8) Uani 1 1 d . . . C28 C 0.67310(19) -0.0322(3) 0.50711(17) 0.0384(8) Uani 1 1 d . . . C29 C 0.6407(2) -0.1270(3) 0.48413(19) 0.0508(9) Uani 1 1 d . . . H29A H 0.6725 -0.1767 0.5139 0.076 Uiso 1 1 calc R . . H29B H 0.6398 -0.1375 0.4357 0.076 Uiso 1 1 calc R . . H29C H 0.5881 -0.1306 0.4874 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.01931(12) 0.02072(12) 0.02582(13) -0.00140(8) 0.01037(9) -0.00479(8) N1 0.0198(11) 0.0184(11) 0.0172(11) -0.0006(9) 0.0072(9) -0.0017(9) C2 0.0229(13) 0.0182(12) 0.0143(13) -0.0018(10) 0.0053(11) -0.0035(11) C3 0.0236(14) 0.0199(13) 0.0222(14) -0.0008(11) 0.0098(12) -0.0034(11) C4 0.0273(15) 0.0269(15) 0.0302(16) -0.0020(12) 0.0153(13) 0.0014(12) C5 0.0361(17) 0.0222(15) 0.0434(19) -0.0063(13) 0.0159(15) 0.0048(13) C6 0.0402(18) 0.0171(13) 0.0414(19) -0.0044(13) 0.0154(15) -0.0044(13) C7 0.0296(16) 0.0201(13) 0.0252(15) -0.0021(11) 0.0077(13) -0.0034(12) C8 0.0294(16) 0.0216(14) 0.0334(17) -0.0022(12) 0.0108(13) -0.0114(13) C9 0.0233(14) 0.0270(14) 0.0268(16) -0.0016(12) 0.0088(12) -0.0067(12) C10 0.0185(13) 0.0249(14) 0.0189(14) 0.0005(11) 0.0065(11) -0.0030(11) C11 0.0189(13) 0.0306(15) 0.0175(14) 0.0010(11) 0.0060(11) -0.0025(12) N12 0.0122(10) 0.0250(12) 0.0176(11) 0.0009(9) 0.0047(9) 0.0006(9) C13 0.0185(13) 0.0271(14) 0.0240(15) 0.0047(12) 0.0062(11) 0.0077(12) C14 0.0249(14) 0.0175(13) 0.0262(15) -0.0017(11) 0.0064(12) -0.0048(11) N15 0.0164(11) 0.0149(10) 0.0234(12) 0.0014(9) 0.0054(9) -0.0032(9) C16 0.0172(13) 0.0188(13) 0.0280(15) 0.0076(11) 0.0060(12) -0.0010(11) C17 0.0218(13) 0.0221(13) 0.0227(14) 0.0078(11) 0.0114(11) 0.0042(11) C18 0.0289(16) 0.0414(18) 0.0319(17) 0.0152(14) 0.0190(14) 0.0121(14) C19 0.0420(19) 0.048(2) 0.0257(17) 0.0137(14) 0.0213(15) 0.0247(16) C20 0.0434(18) 0.0257(15) 0.0238(16) 0.0073(12) 0.0134(14) 0.0205(14) C21 0.072(3) 0.0352(18) 0.0221(17) 0.0048(13) 0.0120(17) 0.0337(19) C22 0.078(3) 0.0253(16) 0.0222(17) -0.0035(13) -0.0032(17) 0.0201(18) C23 0.057(2) 0.0245(15) 0.0290(18) -0.0028(13) -0.0054(16) 0.0011(15) C24 0.0413(18) 0.0274(15) 0.0251(16) -0.0012(12) 0.0041(14) 0.0014(14) C25 0.0331(15) 0.0191(14) 0.0208(15) 0.0037(11) 0.0083(12) 0.0118(12) N26 0.0228(11) 0.0173(11) 0.0173(11) 0.0021(9) 0.0082(9) 0.0042(9) Cl 0.0236(3) 0.0208(3) 0.0285(4) -0.0040(3) 0.0088(3) -0.0005(3) O1 0.0237(11) 0.0434(13) 0.0376(13) -0.0068(10) 0.0100(10) -0.0038(10) O2 0.0455(14) 0.0457(13) 0.0457(14) -0.0050(11) 0.0345(12) -0.0064(11) O3 0.0348(14) 0.0383(13) 0.091(2) -0.0310(14) 0.0052(14) -0.0119(11) O4 0.0693(18) 0.0550(16) 0.0475(16) 0.0237(13) 0.0264(14) 0.0323(14) N27 0.0397(17) 0.058(2) 0.050(2) 0.0005(16) 0.0135(15) -0.0035(16) C28 0.0341(18) 0.057(2) 0.0263(17) 0.0016(16) 0.0128(14) 0.0040(17) C29 0.062(3) 0.059(2) 0.030(2) -0.0089(17) 0.0116(18) -0.007(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 Ag N15 2.221(2) . ? Ag N12 2.259(2) . ? Ag N1 2.372(2) . ? Ag N26 2.457(2) . ? Ag Ag 3.3119(4) 2_554 ? N1 C10 1.330(3) . ? N1 C2 1.362(3) . ? C2 C3 1.414(4) . ? C2 C7 1.420(4) . ? C3 C4 1.368(4) . ? C3 H3 0.9500 . ? C4 C5 1.414(4) . ? C4 H4 0.9500 . ? C5 C6 1.358(4) . ? C5 H5 0.9500 . ? C6 C7 1.417(4) . ? C6 H6 0.9500 . ? C7 C8 1.411(4) . ? C8 C9 1.364(4) . ? C8 H8 0.9500 . ? C9 C10 1.407(4) . ? C9 H9 0.9500 . ? C10 C11 1.473(4) . ? C11 N12 1.269(3) . ? C11 H11 0.9500 . ? N12 C13 1.459(3) . ? C13 C14 1.519(4) 2_554 ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N15 1.463(3) . ? C14 C13 1.519(4) 2_554 ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? N15 C16 1.265(3) . ? C16 C17 1.477(4) . ? C16 H16 0.9500 . ? C17 N26 1.322(3) . ? C17 C18 1.410(4) . ? C18 C19 1.366(5) . ? C18 H18 0.9500 . ? C19 C20 1.403(5) . ? C19 H19 0.9500 . ? C20 C21 1.418(5) . ? C20 C25 1.424(4) . ? C21 C22 1.357(5) . ? C21 H21 0.9500 . ? C22 C23 1.402(5) . ? C22 H22 0.9500 . ? C23 C24 1.370(4) . ? C23 H23 0.9500 . ? C24 C25 1.406(4) . ? C24 H24 0.9500 . ? C25 N26 1.364(3) . ? Cl O3 1.425(2) . ? Cl O4 1.431(2) . ? Cl O1 1.432(2) . ? Cl O2 1.437(2) . ? N27 C28 1.127(5) . ? C28 C29 1.461(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N15 Ag N12 145.82(8) . . ? N15 Ag N1 134.90(8) . . ? N12 Ag N1 73.40(8) . . ? N15 Ag N26 71.97(8) . . ? N12 Ag N26 132.12(8) . . ? N1 Ag N26 96.18(7) . . ? N15 Ag Ag 88.05(6) . 2_554 ? N12 Ag Ag 72.39(6) . 2_554 ? N1 Ag Ag 87.59(5) . 2_554 ? N26 Ag Ag 155.26(5) . 2_554 ? C10 N1 C2 118.3(2) . . ? C10 N1 Ag 111.80(17) . . ? C2 N1 Ag 129.90(17) . . ? N1 C2 C3 119.1(2) . . ? N1 C2 C7 121.8(2) . . ? C3 C2 C7 119.1(2) . . ? C4 C3 C2 120.3(2) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.6(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 122.7(3) . . ? C8 C7 C2 118.2(3) . . ? C6 C7 C2 119.1(3) . . ? C9 C8 C7 119.2(3) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 119.3(3) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N1 C10 C9 123.3(2) . . ? N1 C10 C11 117.2(2) . . ? C9 C10 C11 119.5(2) . . ? N12 C11 C10 122.7(2) . . ? N12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C11 N12 C13 117.9(2) . . ? C11 N12 Ag 114.85(18) . . ? C13 N12 Ag 127.12(16) . . ? N12 C13 C14 112.0(2) . 2_554 ? N12 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 2_554 . ? N12 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 2_554 . ? H13A C13 H13B 107.9 . . ? N15 C14 C13 110.1(2) . 2_554 ? N15 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 2_554 . ? N15 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 2_554 . ? H14A C14 H14B 108.1 . . ? C16 N15 C14 118.6(2) . . ? C16 N15 Ag 118.02(18) . . ? C14 N15 Ag 123.28(16) . . ? N15 C16 C17 121.9(2) . . ? N15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? N26 C17 C18 122.9(3) . . ? N26 C17 C16 117.2(2) . . ? C18 C17 C16 119.9(3) . . ? C19 C18 C17 119.0(3) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 119.9(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 123.6(3) . . ? C19 C20 C25 117.6(3) . . ? C21 C20 C25 118.8(3) . . ? C22 C21 C20 120.2(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.9(3) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 120.6(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? N26 C25 C24 119.0(3) . . ? N26 C25 C20 121.7(3) . . ? C24 C25 C20 119.3(3) . . ? C17 N26 C25 118.8(2) . . ? C17 N26 Ag 110.49(17) . . ? C25 N26 Ag 130.22(18) . . ? O3 Cl O4 111.30(18) . . ? O3 Cl O1 108.56(14) . . ? O4 Cl O1 108.49(15) . . ? O3 Cl O2 110.07(16) . . ? O4 Cl O2 108.54(15) . . ? O1 Cl O2 109.85(14) . . ? N27 C28 C29 178.0(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.990 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.099 #======END============================================================== data_Complex-1b _database_code_CSD 204786 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C44 H36 N8), 4(Cu Cl O4), 2(C H4 O), (C4 H10 O)' _chemical_formula_sum 'C94 H90 Cl4 Cu4 N16 O19' _chemical_formula_weight 2143.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 11.9300(2) _cell_length_b 36.5370(5) _cell_length_c 21.2510(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.7140(5) _cell_angle_gamma 90.00 _cell_volume 9179.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8876 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 25.67 _exptl_crystal_description prisms _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4408 _exptl_absorpt_coefficient_mu 1.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6648 _exptl_absorpt_correction_T_max 0.8510 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '0.6 deg. Phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15583 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0970 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.67 _reflns_number_total 15583 _reflns_number_gt 8876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains two units of the dinuclear complex. It also contains two molecules of methanol and one molecule of diethyl ether solvent. The latter and some of the perchlorate anions are severely disordered. ; _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^)+(0.1240P)^2^+55.6798P] 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 15583 _refine_ls_number_parameters 1196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1570 _refine_ls_R_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.2695 _refine_ls_wR_factor_gt 0.2265 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.194 _refine_ls_shift/su_mean 0.039 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 0.60972(9) -0.66319(3) 0.98055(5) 0.0365(3) Uani 1 1 d . . . Cu2 Cu 0.78720(9) -0.59305(3) 0.92045(5) 0.0420(3) Uani 1 1 d . . . N1 N 0.6692(6) -0.70012(19) 0.9207(4) 0.0398(18) Uani 1 1 d . . . C2 C 0.7322(8) -0.7305(2) 0.9356(5) 0.043(2) Uani 1 1 d . . . C3 C 0.7833(8) -0.7360(3) 0.9988(5) 0.053(3) Uani 1 1 d . . . H3 H 0.7689 -0.7190 1.0306 0.063 Uiso 1 1 calc R . . C4 C 0.8535(9) -0.7654(3) 1.0155(6) 0.069(3) Uani 1 1 d . . . H4 H 0.8893 -0.7687 1.0578 0.083 Uiso 1 1 calc R . . C5 C 0.8704(10) -0.7914(3) 0.9647(8) 0.081(4) Uani 1 1 d . . . H5 H 0.9176 -0.8122 0.9743 0.097 Uiso 1 1 calc R . . C6 C 0.8198(10) -0.7861(3) 0.9049(7) 0.070(3) Uani 1 1 d . . . H6 H 0.8321 -0.8035 0.8734 0.084 Uiso 1 1 calc R . . C7 C 0.7503(9) -0.7563(3) 0.8871(6) 0.055(3) Uani 1 1 d . . . C8 C 0.6954(9) -0.7497(3) 0.8253(5) 0.062(3) Uani 1 1 d . . . H8 H 0.7019 -0.7670 0.7926 0.074 Uiso 1 1 calc R . . C9 C 0.6333(9) -0.7190(3) 0.8123(5) 0.059(3) Uani 1 1 d . . . H9 H 0.5967 -0.7145 0.7706 0.071 Uiso 1 1 calc R . . C10 C 0.6240(8) -0.6943(3) 0.8608(4) 0.041(2) Uani 1 1 d . . . C11 C 0.5655(7) -0.6592(3) 0.8503(4) 0.044(2) Uani 1 1 d . . . H11 H 0.5392 -0.6511 0.8084 0.053 Uiso 1 1 calc R . . N12 N 0.5505(6) -0.6398(2) 0.8978(3) 0.0415(18) Uani 1 1 d . . . C13 C 0.4933(8) -0.6039(3) 0.8886(5) 0.051(3) Uani 1 1 d . . . H13A H 0.5051 -0.5939 0.8466 0.061 Uiso 1 1 calc R . . H13B H 0.4110 -0.6074 0.8885 0.061 Uiso 1 1 calc R . . C14 C 0.5349(8) -0.5773(3) 0.9380(5) 0.051(3) Uani 1 1 d . . . H14A H 0.5357 -0.5888 0.9803 0.061 Uiso 1 1 calc R . . H14B H 0.4828 -0.5562 0.9356 0.061 Uiso 1 1 calc R . . N15 N 0.6493(6) -0.5645(2) 0.9312(4) 0.0437(19) Uani 1 1 d . . . C16 C 0.6672(9) -0.5301(2) 0.9368(4) 0.049(2) Uani 1 1 d . . . H16 H 0.6086 -0.5139 0.9452 0.059 Uiso 1 1 calc R . . C17 C 0.7780(9) -0.5162(2) 0.9301(4) 0.048(2) Uani 1 1 d . . . C18 C 0.8074(11) -0.4789(3) 0.9326(5) 0.061(3) Uani 1 1 d . . . H18 H 0.7521 -0.4611 0.9393 0.073 Uiso 1 1 calc R . . C19 C 0.9134(12) -0.4680(3) 0.9257(5) 0.071(4) Uani 1 1 d . . . H19 H 0.9321 -0.4427 0.9276 0.085 Uiso 1 1 calc R . . C20 C 0.9952(10) -0.4937(3) 0.9156(5) 0.060(3) Uani 1 1 d . . . C21 C 1.1088(13) -0.4851(4) 0.9071(6) 0.083(4) Uani 1 1 d . . . H21 H 1.1328 -0.4603 0.9099 0.099 Uiso 1 1 calc R . . C22 C 1.1822(12) -0.5108(4) 0.8955(6) 0.080(4) Uani 1 1 d . . . H22 H 1.2566 -0.5040 0.8890 0.096 Uiso 1 1 calc R . . C23 C 1.1517(9) -0.5476(3) 0.8929(5) 0.062(3) Uani 1 1 d . . . H23 H 1.2048 -0.5658 0.8847 0.075 Uiso 1 1 calc R . . C24 C 1.0427(8) -0.5574(3) 0.9025(4) 0.054(3) Uani 1 1 d . . . H24 H 1.0219 -0.5825 0.9019 0.065 Uiso 1 1 calc R . . C25 C 0.9635(9) -0.5308(3) 0.9128(4) 0.049(2) Uani 1 1 d . . . N26 N 0.8543(7) -0.5416(2) 0.9202(3) 0.0425(18) Uani 1 1 d . . . N27 N 0.5189(6) -0.69168(17) 1.0400(3) 0.0332(16) Uani 1 1 d . . . C28 C 0.4429(7) -0.7198(2) 1.0270(4) 0.035(2) Uani 1 1 d . . . C29 C 0.4071(7) -0.7297(2) 0.9630(4) 0.036(2) Uani 1 1 d . . . H29 H 0.4339 -0.7163 0.9297 0.043 Uiso 1 1 calc R . . C30 C 0.3357(7) -0.7577(2) 0.9488(4) 0.039(2) Uani 1 1 d . . . H30 H 0.3113 -0.7637 0.9056 0.047 Uiso 1 1 calc R . . C31 C 0.2962(8) -0.7785(2) 0.9977(4) 0.044(2) Uani 1 1 d . . . H31 H 0.2480 -0.7990 0.9871 0.052 Uiso 1 1 calc R . . C32 C 0.3266(7) -0.7695(2) 1.0593(4) 0.043(2) Uani 1 1 d . . . H32 H 0.2977 -0.7832 1.0916 0.051 Uiso 1 1 calc R . . C33 C 0.4024(7) -0.7394(2) 1.0766(4) 0.0335(19) Uani 1 1 d . . . C34 C 0.4380(8) -0.7295(2) 1.1391(4) 0.044(2) Uani 1 1 d . . . H34 H 0.4100 -0.7419 1.1730 0.053 Uiso 1 1 calc R . . C35 C 0.5145(7) -0.7015(2) 1.1510(4) 0.040(2) Uani 1 1 d . . . H35 H 0.5397 -0.6940 1.1934 0.048 Uiso 1 1 calc R . . C36 C 0.5549(7) -0.6839(2) 1.1001(4) 0.037(2) Uani 1 1 d . . . C37 C 0.6418(7) -0.6555(2) 1.1102(4) 0.038(2) Uani 1 1 d . . . H37 H 0.6647 -0.6461 1.1516 0.046 Uiso 1 1 calc R . . N38 N 0.6868(6) -0.64355(17) 1.0625(3) 0.0357(17) Uani 1 1 d . . . C39 C 0.7791(8) -0.6177(2) 1.0735(4) 0.044(2) Uani 1 1 d . . . H39A H 0.7982 -0.6133 1.1197 0.053 Uiso 1 1 calc R . . H39B H 0.7555 -0.5941 1.0530 0.053 Uiso 1 1 calc R . . C40 C 0.8828(7) -0.6320(2) 1.0468(4) 0.042(2) Uani 1 1 d . . . H40A H 0.9491 -0.6167 1.0626 0.051 Uiso 1 1 calc R . . H40B H 0.8987 -0.6574 1.0618 0.051 Uiso 1 1 calc R . . N41 N 0.8655(6) -0.6314(2) 0.9788(4) 0.0412(18) Uani 1 1 d . . . C42 C 0.9019(7) -0.6582(3) 0.9479(5) 0.045(2) Uani 1 1 d . . . H42 H 0.9407 -0.6781 0.9698 0.054 Uiso 1 1 calc R . . C43 C 0.8824(7) -0.6575(3) 0.8777(5) 0.043(2) Uani 1 1 d . . . C44 C 0.9259(8) -0.6850(3) 0.8417(6) 0.059(3) Uani 1 1 d . . . H44 H 0.9689 -0.7048 0.8615 0.071 Uiso 1 1 calc R . . C45 C 0.9039(9) -0.6823(3) 0.7766(5) 0.064(3) Uani 1 1 d . . . H45 H 0.9304 -0.7007 0.7505 0.076 Uiso 1 1 calc R . . C46 C 0.8418(8) -0.6522(3) 0.7487(5) 0.052(3) Uani 1 1 d . . . C47 C 0.8171(11) -0.6469(4) 0.6821(6) 0.074(3) Uani 1 1 d . . . H47 H 0.8429 -0.6643 0.6540 0.089 Uiso 1 1 calc R . . C48 C 0.7574(11) -0.6176(3) 0.6580(5) 0.073(3) Uani 1 1 d . . . H48 H 0.7426 -0.6145 0.6133 0.087 Uiso 1 1 calc R . . C49 C 0.7171(9) -0.5917(3) 0.6982(5) 0.057(3) Uani 1 1 d . . . H49 H 0.6747 -0.5714 0.6802 0.069 Uiso 1 1 calc R . . C50 C 0.7375(8) -0.5952(2) 0.7622(4) 0.045(2) Uani 1 1 d . . . H50 H 0.7087 -0.5777 0.7890 0.054 Uiso 1 1 calc R . . C51 C 0.8037(7) -0.6258(2) 0.7892(4) 0.040(2) Uani 1 1 d . . . N52 N 0.8242(6) -0.62850(18) 0.8532(3) 0.0384(17) Uani 1 1 d . . . Cu1' Cu 0.64341(10) -0.38191(3) 0.60214(5) 0.0439(3) Uani 1 1 d . . . Cu2' Cu 0.77472(10) -0.37330(3) 0.76808(5) 0.0441(3) Uani 1 1 d . . . N1' N 0.6701(7) -0.4368(2) 0.5993(3) 0.047(2) Uani 1 1 d . . . C2' C 0.5935(9) -0.4645(2) 0.5910(4) 0.044(2) Uani 1 1 d . . . C3' C 0.4781(9) -0.4565(3) 0.5938(4) 0.049(3) Uani 1 1 d . . . H3' H 0.4558 -0.4320 0.6004 0.059 Uiso 1 1 calc R . . C4' C 0.3989(11) -0.4835(3) 0.5870(5) 0.062(3) Uani 1 1 d . . . H4' H 0.3219 -0.4780 0.5896 0.075 Uiso 1 1 calc R . . C5' C 0.4324(13) -0.5206(3) 0.5757(5) 0.070(3) Uani 1 1 d . . . H5' H 0.3773 -0.5395 0.5715 0.084 Uiso 1 1 calc R . . C6' C 0.5404(13) -0.5285(3) 0.5710(5) 0.071(4) Uani 1 1 d . . . H6' H 0.5605 -0.5528 0.5615 0.085 Uiso 1 1 calc R . . C7' C 0.6254(11) -0.5013(3) 0.5801(4) 0.061(3) Uani 1 1 d . . . C8' C 0.7416(12) -0.5080(3) 0.5768(5) 0.069(4) Uani 1 1 d . . . H8' H 0.7663 -0.5320 0.5679 0.082 Uiso 1 1 calc R . . C9' C 0.8174(11) -0.4802(3) 0.5862(5) 0.065(3) Uani 1 1 d . . . H9' H 0.8955 -0.4849 0.5855 0.078 Uiso 1 1 calc R . . C10' C 0.7803(9) -0.4446(3) 0.5972(4) 0.053(3) Uani 1 1 d . . . C11' C 0.8561(10) -0.4138(3) 0.6092(4) 0.054(3) Uani 1 1 d . . . H11' H 0.9356 -0.4173 0.6129 0.064 Uiso 1 1 calc R . . N12' N 0.8161(7) -0.3818(2) 0.6148(3) 0.048(2) Uani 1 1 d . . . C13' C 0.8904(8) -0.3502(3) 0.6266(5) 0.053(3) Uani 1 1 d . . . H13C H 0.9106 -0.3411 0.5858 0.064 Uiso 1 1 calc R . . H13D H 0.9611 -0.3578 0.6533 0.064 Uiso 1 1 calc R . . C14' C 0.8359(9) -0.3201(3) 0.6592(5) 0.057(3) Uani 1 1 d . . . H14C H 0.8791 -0.2972 0.6557 0.069 Uiso 1 1 calc R . . H14D H 0.7583 -0.3162 0.6372 0.069 Uiso 1 1 calc R . . N15' N 0.8303(6) -0.3278(2) 0.7269(4) 0.046(2) Uani 1 1 d . . . C16' C 0.8605(8) -0.3024(3) 0.7670(5) 0.048(2) Uani 1 1 d . . . H16' H 0.8881 -0.2798 0.7534 0.057 Uiso 1 1 calc R . . C17' C 0.8520(8) -0.3088(2) 0.8339(5) 0.045(2) Uani 1 1 d . . . C18' C 0.8881(9) -0.2821(3) 0.8797(6) 0.060(3) Uani 1 1 d . . . H18' H 0.9186 -0.2596 0.8670 0.072 Uiso 1 1 calc R . . C19' C 0.8799(8) -0.2880(3) 0.9406(6) 0.057(3) Uani 1 1 d . . . H19' H 0.9080 -0.2705 0.9719 0.069 Uiso 1 1 calc R . . C20' C 0.8284(8) -0.3208(3) 0.9582(5) 0.046(2) Uani 1 1 d . . . C21' C 0.8123(8) -0.3284(3) 1.0213(5) 0.055(3) Uani 1 1 d . . . H21' H 0.8375 -0.3114 1.0539 0.066 Uiso 1 1 calc R . . C22' C 0.7618(9) -0.3594(3) 1.0357(5) 0.064(3) Uani 1 1 d . . . H22' H 0.7515 -0.3643 1.0784 0.077 Uiso 1 1 calc R . . C23' C 0.7239(8) -0.3845(3) 0.9878(5) 0.054(3) Uani 1 1 d . . . H23' H 0.6858 -0.4061 0.9983 0.064 Uiso 1 1 calc R . . C24' C 0.7405(7) -0.3787(3) 0.9266(5) 0.044(2) Uani 1 1 d . . . H24' H 0.7163 -0.3965 0.8951 0.053 Uiso 1 1 calc R . . C25' C 0.7935(7) -0.3465(2) 0.9098(4) 0.038(2) Uani 1 1 d . . . N26' N 0.8066(6) -0.34029(19) 0.8479(4) 0.0426(18) Uani 1 1 d . . . N27' N 0.5557(6) -0.35899(19) 0.5204(3) 0.0381(17) Uani 1 1 d . . . C28' C 0.5726(9) -0.3615(2) 0.4572(4) 0.046(2) Uani 1 1 d . . . C29' C 0.6612(9) -0.3837(2) 0.4427(4) 0.049(2) Uani 1 1 d . . . H29' H 0.7081 -0.3966 0.4749 0.059 Uiso 1 1 calc R . . C30' C 0.6784(9) -0.3861(3) 0.3785(5) 0.059(3) Uani 1 1 d . . . H30' H 0.7362 -0.4016 0.3671 0.071 Uiso 1 1 calc R . . C31' C 0.6125(11) -0.3663(3) 0.3317(5) 0.063(3) Uani 1 1 d . . . H31' H 0.6265 -0.3684 0.2889 0.076 Uiso 1 1 calc R . . C32' C 0.5291(10) -0.3442(3) 0.3458(5) 0.066(3) Uani 1 1 d . . . H32' H 0.4860 -0.3304 0.3132 0.079 Uiso 1 1 calc R . . C33' C 0.5052(9) -0.3415(3) 0.4095(4) 0.052(3) Uani 1 1 d . . . C34' C 0.4203(10) -0.3188(3) 0.4270(5) 0.068(3) Uani 1 1 d . . . H34' H 0.3745 -0.3049 0.3957 0.081 Uiso 1 1 calc R . . C35' C 0.4037(8) -0.3168(3) 0.4879(5) 0.054(3) Uani 1 1 d . . . H35' H 0.3457 -0.3017 0.5002 0.065 Uiso 1 1 calc R . . C36' C 0.4749(8) -0.3379(3) 0.5347(4) 0.045(2) Uani 1 1 d . . . C37' C 0.4592(8) -0.3357(3) 0.5999(4) 0.049(2) Uani 1 1 d . . . H37' H 0.3991 -0.3216 0.6125 0.058 Uiso 1 1 calc R . . N38' N 0.5277(7) -0.3532(2) 0.6418(3) 0.048(2) Uani 1 1 d . . . C39' C 0.5118(8) -0.3482(3) 0.7085(4) 0.050(3) Uani 1 1 d . . . H39C H 0.4390 -0.3355 0.7105 0.060 Uiso 1 1 calc R . . H39D H 0.5731 -0.3325 0.7297 0.060 Uiso 1 1 calc R . . C40' C 0.5120(8) -0.3839(3) 0.7431(5) 0.055(3) Uani 1 1 d . . . H40C H 0.4877 -0.3799 0.7854 0.066 Uiso 1 1 calc R . . H40D H 0.4578 -0.4009 0.7190 0.066 Uiso 1 1 calc R . . N41' N 0.6252(7) -0.3998(2) 0.7507(3) 0.0424(19) Uani 1 1 d . . . C42' C 0.6360(8) -0.4340(3) 0.7497(4) 0.047(2) Uani 1 1 d . . . H42' H 0.5712 -0.4494 0.7452 0.056 Uiso 1 1 calc R . . C43' C 0.7504(8) -0.4500(3) 0.7556(4) 0.042(2) Uani 1 1 d . . . C44' C 0.7689(9) -0.4877(3) 0.7495(4) 0.050(3) Uani 1 1 d . . . H44' H 0.7081 -0.5047 0.7480 0.059 Uiso 1 1 calc R . . C45' C 0.8770(10) -0.4995(3) 0.7459(4) 0.054(3) Uani 1 1 d . . . H45' H 0.8911 -0.5249 0.7413 0.065 Uiso 1 1 calc R . . C46' C 0.9662(9) -0.4749(3) 0.7489(4) 0.054(3) Uani 1 1 d . . . C47' C 1.0780(10) -0.4841(3) 0.7395(6) 0.073(4) Uani 1 1 d . . . H47' H 1.0958 -0.5089 0.7318 0.087 Uiso 1 1 calc R . . C48' C 1.1601(11) -0.4584(4) 0.7414(6) 0.079(4) Uani 1 1 d . . . H48' H 1.2346 -0.4653 0.7353 0.095 Uiso 1 1 calc R . . C49' C 1.1358(9) -0.4216(3) 0.7524(5) 0.065(3) Uani 1 1 d . . . H49' H 1.1937 -0.4037 0.7532 0.078 Uiso 1 1 calc R . . C50' C 1.0303(8) -0.4115(3) 0.7619(5) 0.052(3) Uani 1 1 d . . . H50' H 1.0155 -0.3866 0.7707 0.063 Uiso 1 1 calc R . . C51' C 0.9415(9) -0.4374(3) 0.7590(4) 0.046(2) Uani 1 1 d . . . N52' N 0.8347(6) -0.4252(2) 0.7622(3) 0.0393(18) Uani 1 1 d . . . Cl55 Cl 0.7242(2) -0.21434(7) 0.71849(12) 0.0561(7) Uani 1 1 d . . . O56 O 0.8196(6) -0.22014(18) 0.6863(3) 0.0598(19) Uani 1 1 d . . . O57 O 0.7591(7) -0.2098(2) 0.7850(3) 0.079(2) Uani 1 1 d . . . O58 O 0.6505(6) -0.2463(2) 0.7091(4) 0.082(3) Uani 1 1 d . . . O59 O 0.6664(8) -0.1825(3) 0.6936(4) 0.100(3) Uani 1 1 d . . . Cl60 Cl 0.4587(2) -0.45211(7) 0.87933(11) 0.0460(6) Uani 1 1 d . . . O61 O 0.4329(7) -0.4700(2) 0.9336(4) 0.082(2) Uiso 1 1 d . . . O62 O 0.5675(13) -0.4659(5) 0.8605(7) 0.057(4) Uiso 0.50 1 d P . . O62A O 0.501(3) -0.4805(9) 0.8370(15) 0.182(11) Uiso 0.50 1 d P . . O63 O 0.5074(11) -0.4157(4) 0.8987(6) 0.055(3) Uiso 0.50 1 d P . . O63A O 0.572(2) -0.4432(8) 0.8868(13) 0.138(9) Uiso 0.50 1 d P . . O64 O 0.3700(12) -0.4369(4) 0.8365(7) 0.066(4) Uiso 0.50 1 d P . . O64A O 0.402(3) -0.4704(8) 0.8256(13) 0.156(9) Uiso 0.50 1 d P . . Cl65 Cl 1.1604(3) -0.29958(9) 0.78744(16) 0.0812(9) Uani 1 1 d . . . O66 O 1.2285(11) -0.2743(3) 0.8302(5) 0.059(4) Uiso 0.620(18) 1 d P . . O66A O 1.1535(10) -0.2617(3) 0.8175(5) 0.013(4) Uiso 0.380(18) 1 d P . . O67 O 1.0906(6) -0.2778(2) 0.7442(3) 0.066(2) Uiso 1 1 d . . . O68 O 1.0924(8) -0.3236(3) 0.8224(4) 0.093(3) Uiso 1 1 d . . . O69 O 1.2305(19) -0.3369(7) 0.7383(11) 0.114(8) Uiso 0.50 1 d P . . O69A O 1.2379(9) -0.3202(3) 0.7566(5) 0.025(2) Uiso 0.50 1 d P . . Cl70 Cl 1.1768(3) -0.40406(9) 0.55314(17) 0.0812(10) Uani 1 1 d . . . O71 O 1.1340(9) -0.4391(3) 0.5693(5) 0.112(3) Uani 1 1 d . . . O72 O 1.2384(11) -0.4063(3) 0.5032(5) 0.134(4) Uani 1 1 d . . . O73 O 1.0821(10) -0.3805(3) 0.5405(8) 0.157(6) Uani 1 1 d . . . O74 O 1.2493(12) -0.3904(4) 0.6059(7) 0.172(6) Uani 1 1 d . . . C75 C 0.9222(13) -0.0413(4) 0.9294(7) 0.103(5) Uiso 1 1 d . . . C76 C 0.9706(14) -0.0595(5) 0.8838(8) 0.116(5) Uiso 1 1 d . . . O77 O 0.8914(17) -0.0727(6) 0.8222(10) 0.110(6) Uiso 0.50 1 d P . . C78 C 0.930(3) -0.0957(10) 0.7750(17) 0.118(11) Uiso 0.50 1 d P . . C79 C 0.8638(13) -0.1122(4) 0.7358(7) 0.089(4) Uiso 1 1 d . . . C80 C 0.7633(18) -0.1168(6) 0.6944(10) 0.140(7) Uiso 1 1 d . . . O80 O 0.5248(8) -0.5333(2) 0.7764(4) 0.091(3) Uani 1 1 d . . . C81 C 0.4155(13) -0.5396(4) 0.7440(7) 0.107(5) Uani 1 1 d . . . H81A H 0.3655 -0.5478 0.7742 0.160 Uiso 1 1 calc R . . H81B H 0.4191 -0.5584 0.7115 0.160 Uiso 1 1 calc R . . H81C H 0.3858 -0.5168 0.7237 0.160 Uiso 1 1 calc R . . O82 O 0.9609(10) -0.1923(3) 0.8576(7) 0.144(4) Uani 1 1 d . . . C83 C 0.9306(12) -0.1656(4) 0.9048(7) 0.095(4) Uani 1 1 d . . . H83A H 0.9184 -0.1785 0.9437 0.142 Uiso 1 1 calc R . . H83B H 0.8612 -0.1527 0.8875 0.142 Uiso 1 1 calc R . . H83C H 0.9922 -0.1479 0.9144 0.142 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0434(6) 0.0312(6) 0.0347(6) 0.0004(4) 0.0048(5) -0.0042(5) Cu2 0.0438(7) 0.0302(6) 0.0516(7) 0.0085(5) 0.0052(5) -0.0017(5) N1 0.038(4) 0.033(4) 0.053(5) -0.006(3) 0.020(4) -0.009(3) C2 0.044(6) 0.036(5) 0.052(6) 0.001(4) 0.014(5) -0.008(4) C3 0.050(6) 0.031(5) 0.081(8) 0.005(5) 0.019(6) -0.004(4) C4 0.043(6) 0.051(7) 0.110(10) 0.023(7) 0.000(6) 0.001(5) C5 0.053(7) 0.043(7) 0.153(14) 0.002(8) 0.037(8) 0.020(5) C6 0.073(8) 0.055(7) 0.084(9) -0.006(7) 0.024(7) 0.004(6) C7 0.052(6) 0.039(6) 0.083(8) -0.006(5) 0.038(6) 0.001(5) C8 0.070(8) 0.077(8) 0.044(6) -0.019(6) 0.023(6) -0.012(6) C9 0.065(7) 0.068(7) 0.049(6) -0.013(5) 0.026(5) -0.008(6) C10 0.044(5) 0.054(6) 0.028(5) -0.002(4) 0.008(4) -0.012(5) C11 0.035(5) 0.056(6) 0.040(5) 0.011(5) 0.000(4) -0.014(5) N12 0.036(4) 0.047(5) 0.040(4) 0.001(4) 0.002(3) -0.014(4) C13 0.043(6) 0.049(6) 0.060(6) 0.026(5) 0.002(5) 0.013(5) C14 0.055(6) 0.036(5) 0.063(7) 0.015(5) 0.010(5) 0.010(5) N15 0.042(4) 0.037(4) 0.053(5) 0.017(4) 0.008(4) -0.004(4) C16 0.063(7) 0.031(5) 0.053(6) 0.009(4) 0.012(5) 0.008(5) C17 0.075(7) 0.031(5) 0.036(5) 0.008(4) 0.005(5) -0.001(5) C18 0.094(9) 0.035(6) 0.050(6) 0.000(5) -0.004(6) -0.004(6) C19 0.105(10) 0.042(7) 0.060(7) 0.007(5) -0.009(7) -0.034(7) C20 0.071(8) 0.056(7) 0.049(6) 0.009(5) -0.011(6) -0.035(6) C21 0.107(11) 0.070(9) 0.063(8) 0.002(7) -0.018(8) -0.059(9) C22 0.071(9) 0.095(11) 0.067(8) 0.015(8) -0.015(7) -0.048(8) C23 0.047(6) 0.077(8) 0.058(7) 0.011(6) -0.010(5) -0.017(6) C24 0.048(6) 0.068(7) 0.044(6) 0.009(5) -0.001(5) -0.018(6) C25 0.060(7) 0.041(6) 0.040(5) 0.008(4) -0.012(5) -0.006(5) N26 0.052(5) 0.039(4) 0.036(4) 0.007(3) 0.002(4) -0.014(4) N27 0.045(4) 0.026(4) 0.028(4) -0.003(3) 0.003(3) 0.004(3) C28 0.045(5) 0.020(4) 0.043(5) -0.001(4) 0.012(4) -0.005(4) C29 0.044(5) 0.034(5) 0.030(5) -0.004(4) 0.004(4) -0.003(4) C30 0.051(6) 0.036(5) 0.031(5) -0.003(4) 0.002(4) -0.009(4) C31 0.047(6) 0.031(5) 0.050(6) -0.002(4) -0.003(5) -0.008(4) C32 0.044(5) 0.034(5) 0.053(6) 0.011(4) 0.017(5) -0.006(4) C33 0.032(5) 0.034(5) 0.035(5) -0.002(4) 0.005(4) -0.003(4) C34 0.054(6) 0.041(5) 0.040(5) 0.000(4) 0.019(5) -0.001(5) C35 0.038(5) 0.050(6) 0.033(5) -0.008(4) 0.011(4) -0.005(4) C36 0.041(5) 0.028(5) 0.043(5) -0.004(4) 0.011(4) 0.001(4) C37 0.040(5) 0.036(5) 0.039(5) -0.008(4) 0.003(4) 0.000(4) N38 0.041(4) 0.020(3) 0.046(4) -0.002(3) 0.006(4) 0.001(3) C39 0.051(6) 0.035(5) 0.045(5) 0.004(4) -0.004(5) -0.010(4) C40 0.037(5) 0.035(5) 0.050(6) 0.009(4) -0.010(4) -0.013(4) N41 0.022(4) 0.042(5) 0.058(5) 0.012(4) -0.001(3) -0.007(3) C42 0.035(5) 0.035(5) 0.065(7) 0.018(5) 0.004(5) 0.000(4) C43 0.032(5) 0.045(6) 0.056(6) 0.005(5) 0.012(4) -0.006(4) C44 0.049(6) 0.052(6) 0.080(8) 0.012(6) 0.026(6) 0.010(5) C45 0.069(8) 0.063(7) 0.065(8) 0.007(6) 0.032(6) 0.017(6) C46 0.048(6) 0.056(6) 0.056(7) 0.004(5) 0.021(5) -0.003(5) C47 0.091(9) 0.073(8) 0.066(8) 0.005(7) 0.032(7) 0.005(7) C48 0.104(10) 0.071(8) 0.046(7) 0.004(6) 0.020(7) -0.006(7) C49 0.064(7) 0.053(6) 0.053(7) 0.003(5) 0.004(5) -0.001(5) C50 0.053(6) 0.036(5) 0.047(6) 0.006(4) 0.010(5) -0.010(4) C51 0.034(5) 0.038(5) 0.048(6) 0.009(4) 0.010(4) -0.010(4) N52 0.037(4) 0.030(4) 0.049(5) 0.011(3) 0.008(4) 0.000(3) Cu1' 0.0508(7) 0.0445(7) 0.0386(6) 0.0069(5) 0.0144(5) 0.0147(5) Cu2' 0.0515(7) 0.0334(6) 0.0481(7) 0.0094(5) 0.0088(6) 0.0011(5) N1' 0.069(6) 0.039(5) 0.035(4) 0.005(3) 0.017(4) 0.015(4) C2' 0.066(7) 0.038(5) 0.026(5) -0.001(4) 0.004(4) 0.014(5) C3' 0.077(8) 0.034(5) 0.037(5) 0.003(4) 0.005(5) -0.008(5) C4' 0.088(9) 0.063(7) 0.036(6) 0.008(5) 0.008(5) -0.003(6) C5' 0.114(11) 0.048(7) 0.042(6) 0.005(5) -0.008(7) -0.019(7) C6' 0.117(11) 0.045(7) 0.045(6) -0.006(5) -0.011(7) 0.018(7) C7' 0.100(10) 0.049(6) 0.030(5) 0.000(5) -0.004(6) 0.010(7) C8' 0.115(11) 0.058(7) 0.034(6) -0.003(5) 0.011(6) 0.038(8) C9' 0.088(9) 0.068(8) 0.039(6) 0.002(5) 0.004(6) 0.039(7) C10' 0.070(7) 0.054(6) 0.035(5) 0.008(5) 0.009(5) 0.029(6) C11' 0.068(7) 0.060(7) 0.035(5) 0.013(5) 0.019(5) 0.022(6) N12' 0.054(5) 0.057(5) 0.036(4) 0.009(4) 0.014(4) 0.015(4) C13' 0.043(6) 0.060(7) 0.059(6) 0.023(5) 0.016(5) 0.008(5) C14' 0.060(7) 0.043(6) 0.073(7) 0.028(5) 0.021(6) 0.009(5) N15' 0.046(5) 0.040(5) 0.057(5) 0.019(4) 0.022(4) 0.007(4) C16' 0.047(6) 0.034(5) 0.065(7) 0.004(5) 0.014(5) 0.009(4) C17' 0.038(5) 0.039(5) 0.059(6) 0.009(5) 0.016(5) 0.007(4) C18' 0.056(7) 0.036(6) 0.087(9) -0.004(6) 0.010(6) 0.001(5) C19' 0.044(6) 0.052(7) 0.073(8) -0.010(6) -0.005(5) 0.001(5) C20' 0.036(5) 0.048(6) 0.053(6) -0.005(5) 0.009(5) 0.012(4) C21' 0.034(5) 0.071(8) 0.057(7) -0.015(6) -0.006(5) 0.017(5) C22' 0.060(7) 0.087(9) 0.047(7) 0.004(6) 0.015(5) 0.012(7) C23' 0.055(6) 0.058(7) 0.049(6) 0.006(5) 0.010(5) -0.003(5) C24' 0.030(5) 0.045(6) 0.057(6) 0.004(5) 0.002(4) 0.005(4) C25' 0.027(5) 0.040(5) 0.045(5) 0.008(4) 0.001(4) 0.010(4) N26' 0.040(4) 0.030(4) 0.059(5) 0.007(4) 0.009(4) 0.001(3) N27' 0.049(5) 0.035(4) 0.031(4) 0.002(3) 0.007(3) 0.000(4) C28' 0.067(7) 0.028(5) 0.047(6) 0.000(4) 0.019(5) -0.016(5) C29' 0.068(7) 0.040(5) 0.043(6) 0.005(4) 0.023(5) -0.007(5) C30' 0.069(7) 0.076(8) 0.035(6) -0.007(5) 0.022(5) -0.009(6) C31' 0.089(9) 0.072(8) 0.034(6) 0.003(5) 0.022(6) -0.026(7) C32' 0.078(8) 0.079(8) 0.035(6) -0.004(5) -0.005(6) -0.011(7) C33' 0.065(7) 0.052(6) 0.036(5) 0.006(5) -0.002(5) -0.008(5) C34' 0.070(8) 0.077(8) 0.050(7) 0.012(6) -0.014(6) 0.012(7) C35' 0.050(6) 0.059(7) 0.053(7) 0.011(5) 0.005(5) 0.009(5) C36' 0.048(6) 0.047(6) 0.040(5) 0.006(4) 0.002(5) 0.009(5) C37' 0.053(6) 0.048(6) 0.046(6) 0.005(5) 0.010(5) 0.021(5) N38' 0.064(5) 0.048(5) 0.034(4) -0.002(4) 0.014(4) 0.014(4) C39' 0.051(6) 0.070(7) 0.034(5) -0.001(5) 0.019(4) 0.025(5) C40' 0.038(6) 0.091(8) 0.039(6) 0.004(5) 0.015(4) 0.004(5) N41' 0.055(5) 0.042(5) 0.031(4) 0.009(3) 0.013(4) 0.005(4) C42' 0.047(6) 0.063(7) 0.031(5) 0.005(4) 0.009(4) -0.015(5) C43' 0.054(6) 0.044(6) 0.027(5) 0.012(4) 0.004(4) -0.001(5) C44' 0.071(8) 0.036(5) 0.039(5) 0.001(4) -0.001(5) -0.013(5) C45' 0.081(8) 0.035(5) 0.041(6) 0.003(4) -0.007(5) 0.016(6) C46' 0.065(7) 0.050(6) 0.041(6) -0.003(5) -0.010(5) 0.005(6) C47' 0.060(8) 0.067(8) 0.082(9) -0.021(6) -0.024(7) 0.031(7) C48' 0.057(8) 0.100(10) 0.075(8) -0.028(7) -0.007(6) 0.028(8) C49' 0.050(7) 0.074(8) 0.068(7) -0.027(6) -0.007(6) 0.004(6) C50' 0.047(6) 0.057(6) 0.049(6) -0.006(5) -0.004(5) 0.006(5) C51' 0.054(6) 0.045(6) 0.036(5) 0.005(4) -0.001(5) 0.009(5) N52' 0.043(5) 0.042(4) 0.032(4) 0.007(3) 0.002(3) -0.008(4) Cl55 0.0547(16) 0.0676(17) 0.0446(14) -0.0117(12) 0.0014(12) 0.0117(14) O56 0.054(4) 0.055(4) 0.075(5) 0.007(4) 0.025(4) 0.001(3) O57 0.100(6) 0.099(6) 0.034(4) -0.005(4) -0.008(4) 0.011(5) O58 0.069(5) 0.114(7) 0.066(5) -0.022(5) 0.025(4) -0.039(5) O59 0.105(7) 0.120(8) 0.066(5) -0.005(5) -0.019(5) 0.063(6) Cl60 0.0492(14) 0.0499(14) 0.0382(13) 0.0007(10) 0.0029(11) -0.0017(11) Cl65 0.076(2) 0.083(2) 0.087(2) 0.0263(18) 0.0216(18) 0.0066(18) Cl70 0.091(2) 0.0635(19) 0.096(2) 0.0069(17) 0.038(2) 0.0056(18) O71 0.119(8) 0.078(7) 0.140(9) 0.045(6) 0.014(7) -0.013(6) O72 0.181(11) 0.119(9) 0.125(9) 0.033(7) 0.106(9) 0.034(8) O73 0.130(10) 0.065(7) 0.295(18) 0.035(8) 0.097(11) 0.029(6) O74 0.175(13) 0.193(14) 0.142(11) -0.066(10) -0.001(10) -0.077(11) O80 0.097(7) 0.071(6) 0.104(7) 0.002(5) 0.016(6) 0.012(5) C81 0.120(13) 0.077(10) 0.106(11) 0.001(8) -0.051(10) -0.009(9) O82 0.117(9) 0.118(10) 0.189(13) 0.011(9) -0.012(9) -0.004(8) C83 0.095(11) 0.101(11) 0.090(10) 0.018(9) 0.015(8) 0.037(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 N38 1.992(7) . ? Cu1 N12 1.998(7) . ? Cu1 N1 2.045(7) . ? Cu1 N27 2.054(7) . ? Cu2 N15 1.988(7) . ? Cu2 N41 2.015(7) . ? Cu2 N52 2.022(7) . ? Cu2 N26 2.042(7) . ? N1 C10 1.332(11) . ? N1 C2 1.353(11) . ? C2 C3 1.412(13) . ? C2 C7 1.435(13) . ? C3 C4 1.380(14) . ? C4 C5 1.471(17) . ? C5 C6 1.347(17) . ? C6 C7 1.388(15) . ? C7 C8 1.407(15) . ? C8 C9 1.352(15) . ? C9 C10 1.386(13) . ? C10 C11 1.462(13) . ? C11 N12 1.267(11) . ? N12 C13 1.478(11) . ? C13 C14 1.467(14) . ? C14 N15 1.468(12) . ? N15 C16 1.278(11) . ? C16 C17 1.440(14) . ? C17 N26 1.337(12) . ? C17 C18 1.407(13) . ? C18 C19 1.352(16) . ? C19 C20 1.391(16) . ? C20 C25 1.406(13) . ? C20 C21 1.427(17) . ? C21 C22 1.330(18) . ? C22 C23 1.393(16) . ? C23 C24 1.389(13) . ? C24 C25 1.391(14) . ? C25 N26 1.390(12) . ? N27 C36 1.323(10) . ? N27 C28 1.374(10) . ? C28 C33 1.412(11) . ? C28 C29 1.416(11) . ? C29 C30 1.341(11) . ? C30 C31 1.418(12) . ? C31 C32 1.351(12) . ? C32 C33 1.439(12) . ? C33 C34 1.388(12) . ? C34 C35 1.374(12) . ? C35 C36 1.396(12) . ? C36 C37 1.462(12) . ? C37 N38 1.286(10) . ? N38 C39 1.446(11) . ? C39 C40 1.521(13) . ? C40 N41 1.434(11) . ? N41 C42 1.286(11) . ? C42 C43 1.479(13) . ? C43 N52 1.333(11) . ? C43 C44 1.405(13) . ? C44 C45 1.377(15) . ? C45 C46 1.411(14) . ? C46 C51 1.407(13) . ? C46 C47 1.420(15) . ? C47 C48 1.348(16) . ? C48 C49 1.402(15) . ? C49 C50 1.357(13) . ? C50 C51 1.443(13) . ? C51 N52 1.353(11) . ? Cu1' N38' 2.007(7) . ? Cu1' N1' 2.034(7) . ? Cu1' N12' 2.041(8) . ? Cu1' N27' 2.080(7) . ? Cu2' N41' 2.019(8) . ? Cu2' N15' 2.031(7) . ? Cu2' N52' 2.037(8) . ? Cu2' N26' 2.075(8) . ? N1' C10' 1.352(12) . ? N1' C2' 1.359(12) . ? C2' C3' 1.416(14) . ? C2' C7' 1.425(13) . ? C3' C4' 1.361(14) . ? C4' C5' 1.441(16) . ? C5' C6' 1.337(17) . ? C6' C7' 1.414(17) . ? C7' C8' 1.418(16) . ? C8' C9' 1.357(17) . ? C9' C10' 1.404(14) . ? C10' C11' 1.445(15) . ? C11' N12' 1.273(12) . ? N12' C13' 1.457(13) . ? C13' C14' 1.495(14) . ? C14' N15' 1.477(12) . ? N15' C16' 1.277(12) . ? C16' C17' 1.457(13) . ? C17' N26' 1.324(11) . ? C17' C18' 1.404(14) . ? C18' C19' 1.330(15) . ? C19' C20' 1.418(14) . ? C20' C21' 1.408(14) . ? C20' C25' 1.413(13) . ? C21' C22' 1.336(15) . ? C22' C23' 1.401(15) . ? C23' C24' 1.357(13) . ? C24' C25' 1.406(12) . ? C25' N26' 1.364(11) . ? N27' C36' 1.300(11) . ? N27' C28' 1.388(11) . ? C28' C29' 1.399(13) . ? C28' C33' 1.410(13) . ? C29' C30' 1.408(12) . ? C30' C31' 1.386(15) . ? C31' C32' 1.345(15) . ? C32' C33' 1.423(14) . ? C33' C34' 1.398(15) . ? C34' C35' 1.337(14) . ? C35' C36' 1.442(13) . ? C36' C37' 1.426(13) . ? C37' N38' 1.293(11) . ? N38' C39' 1.466(11) . ? C39' C40' 1.496(14) . ? C40' N41' 1.459(12) . ? N41' C42' 1.259(11) . ? C42' C43' 1.474(13) . ? C43' N52' 1.347(11) . ? C43' C44' 1.405(13) . ? C44' C45' 1.371(14) . ? C45' C46' 1.390(14) . ? C46' C47' 1.416(15) . ? C46' C51' 1.421(13) . ? C47' C48' 1.354(17) . ? C48' C49' 1.401(16) . ? C49' C50' 1.354(14) . ? C50' C51' 1.417(14) . ? C51' N52' 1.360(11) . ? Cl55 O59 1.418(8) . ? Cl55 O56 1.421(7) . ? Cl55 O57 1.428(7) . ? Cl55 O58 1.460(8) . ? Cl60 O63A 1.38(3) . ? Cl60 O61 1.395(9) . ? Cl60 O64 1.413(15) . ? Cl60 O64A 1.41(3) . ? Cl60 O63 1.487(14) . ? Cl60 O62 1.496(15) . ? Cl60 O62A 1.51(3) . ? Cl65 O67 1.402(8) . ? Cl65 O69A 1.419(11) . ? Cl65 O68 1.462(9) . ? Cl65 O66 1.464(12) . ? Cl65 O66A 1.533(12) . ? Cl65 O69 1.97(2) . ? Cl70 O72 1.371(9) . ? Cl70 O74 1.411(12) . ? Cl70 O73 1.417(11) . ? Cl70 O71 1.437(9) . ? C75 C76 1.36(2) . ? C76 O77 1.59(2) . ? O77 C78 1.43(4) . ? C78 C79 1.23(4) . ? C79 C80 1.40(2) . ? O80 C81 1.410(15) . ? O82 C83 1.478(17) . ? 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 N38 Cu1 N12 133.1(3) . . ? N38 Cu1 N1 128.6(3) . . ? N12 Cu1 N1 81.2(3) . . ? N38 Cu1 N27 82.2(3) . . ? N12 Cu1 N27 127.2(3) . . ? N1 Cu1 N27 107.7(3) . . ? N15 Cu2 N41 128.1(3) . . ? N15 Cu2 N52 132.9(3) . . ? N41 Cu2 N52 82.1(3) . . ? N15 Cu2 N26 81.2(3) . . ? N41 Cu2 N26 119.5(3) . . ? N52 Cu2 N26 117.7(3) . . ? C10 N1 C2 119.8(8) . . ? C10 N1 Cu1 111.0(6) . . ? C2 N1 Cu1 128.5(6) . . ? N1 C2 C3 119.7(8) . . ? N1 C2 C7 120.2(9) . . ? C3 C2 C7 120.1(9) . . ? C4 C3 C2 121.7(10) . . ? C3 C4 C5 116.8(11) . . ? C6 C5 C4 120.7(11) . . ? C5 C6 C7 123.1(11) . . ? C6 C7 C8 125.0(11) . . ? C6 C7 C2 117.4(11) . . ? C8 C7 C2 117.5(9) . . ? C9 C8 C7 120.4(10) . . ? C8 C9 C10 119.1(11) . . ? N1 C10 C9 122.9(10) . . ? N1 C10 C11 114.2(8) . . ? C9 C10 C11 122.9(9) . . ? N12 C11 C10 119.0(8) . . ? C11 N12 C13 120.2(8) . . ? C11 N12 Cu1 113.0(7) . . ? C13 N12 Cu1 126.8(6) . . ? C14 C13 N12 112.7(8) . . ? C13 C14 N15 111.8(8) . . ? C16 N15 C14 116.9(8) . . ? C16 N15 Cu2 113.4(6) . . ? C14 N15 Cu2 129.6(6) . . ? N15 C16 C17 118.8(9) . . ? N26 C17 C18 120.5(10) . . ? N26 C17 C16 115.1(8) . . ? C18 C17 C16 124.4(10) . . ? C19 C18 C17 120.9(11) . . ? C18 C19 C20 120.2(10) . . ? C19 C20 C25 117.9(10) . . ? C19 C20 C21 124.6(11) . . ? C25 C20 C21 117.5(12) . . ? C22 C21 C20 121.8(12) . . ? C21 C22 C23 121.1(12) . . ? C24 C23 C22 119.0(12) . . ? C23 C24 C25 120.9(10) . . ? N26 C25 C24 119.1(9) . . ? N26 C25 C20 121.3(10) . . ? C24 C25 C20 119.6(10) . . ? C17 N26 C25 119.3(8) . . ? C17 N26 Cu2 111.3(6) . . ? C25 N26 Cu2 129.4(6) . . ? C36 N27 C28 118.3(7) . . ? C36 N27 Cu1 110.9(5) . . ? C28 N27 Cu1 130.1(5) . . ? N27 C28 C33 120.8(7) . . ? N27 C28 C29 119.3(7) . . ? C33 C28 C29 119.9(7) . . ? C30 C29 C28 120.7(8) . . ? C29 C30 C31 120.6(8) . . ? C32 C31 C30 120.4(8) . . ? C31 C32 C33 120.7(8) . . ? C34 C33 C28 119.4(8) . . ? C34 C33 C32 123.0(8) . . ? C28 C33 C32 117.6(8) . . ? C35 C34 C33 118.8(8) . . ? C34 C35 C36 119.3(8) . . ? N27 C36 C35 123.3(8) . . ? N27 C36 C37 115.2(7) . . ? C35 C36 C37 121.5(8) . . ? N38 C37 C36 119.3(8) . . ? C37 N38 C39 119.0(7) . . ? C37 N38 Cu1 112.0(6) . . ? C39 N38 Cu1 128.9(6) . . ? N38 C39 C40 110.8(7) . . ? N41 C40 C39 110.9(7) . . ? C42 N41 C40 119.4(8) . . ? C42 N41 Cu2 112.1(6) . . ? C40 N41 Cu2 128.5(6) . . ? N41 C42 C43 118.9(8) . . ? N52 C43 C44 124.6(9) . . ? N52 C43 C42 114.3(8) . . ? C44 C43 C42 121.1(9) . . ? C45 C44 C43 117.4(10) . . ? C44 C45 C46 119.8(10) . . ? C51 C46 C45 118.1(9) . . ? C51 C46 C47 118.3(10) . . ? C45 C46 C47 123.5(10) . . ? C48 C47 C46 121.0(11) . . ? C47 C48 C49 120.8(11) . . ? C50 C49 C48 121.2(10) . . ? C49 C50 C51 119.1(9) . . ? N52 C51 C46 122.4(8) . . ? N52 C51 C50 118.0(8) . . ? C46 C51 C50 119.6(9) . . ? C43 N52 C51 117.6(8) . . ? C43 N52 Cu2 112.6(6) . . ? C51 N52 Cu2 129.6(6) . . ? N38' Cu1' N1' 130.3(3) . . ? N38' Cu1' N12' 133.1(3) . . ? N1' Cu1' N12' 81.1(3) . . ? N38' Cu1' N27' 81.0(3) . . ? N1' Cu1' N27' 115.8(3) . . ? N12' Cu1' N27' 119.7(3) . . ? N41' Cu2' N15' 130.2(3) . . ? N41' Cu2' N52' 81.5(3) . . ? N15' Cu2' N52' 126.8(3) . . ? N41' Cu2' N26' 119.2(3) . . ? N15' Cu2' N26' 80.9(3) . . ? N52' Cu2' N26' 124.3(3) . . ? C10' N1' C2' 118.7(8) . . ? C10' N1' Cu1' 111.4(7) . . ? C2' N1' Cu1' 129.2(7) . . ? N1' C2' C3' 118.8(8) . . ? N1' C2' C7' 122.2(10) . . ? C3' C2' C7' 118.9(10) . . ? C4' C3' C2' 120.7(10) . . ? C3' C4' C5' 119.7(12) . . ? C6' C5' C4' 120.4(11) . . ? C5' C6' C7' 121.3(11) . . ? C6' C7' C8' 124.0(11) . . ? C6' C7' C2' 118.9(11) . . ? C8' C7' C2' 117.1(11) . . ? C9' C8' C7' 120.0(10) . . ? C8' C9' C10' 120.0(11) . . ? N1' C10' C9' 121.9(11) . . ? N1' C10' C11' 114.8(9) . . ? C9' C10' C11' 123.3(11) . . ? N12' C11' C10' 119.8(10) . . ? C11' N12' C13' 121.0(9) . . ? C11' N12' Cu1' 111.8(8) . . ? C13' N12' Cu1' 127.2(6) . . ? N12' C13' C14' 111.8(8) . . ? N15' C14' C13' 113.0(8) . . ? C16' N15' C14' 117.8(8) . . ? C16' N15' Cu2' 112.7(6) . . ? C14' N15' Cu2' 129.4(7) . . ? N15' C16' C17' 119.0(9) . . ? N26' C17' C18' 123.0(9) . . ? N26' C17' C16' 116.3(9) . . ? C18' C17' C16' 120.7(9) . . ? C19' C18' C17' 120.3(10) . . ? C18' C19' C20' 119.1(10) . . ? C21' C20' C25' 119.8(9) . . ? C21' C20' C19' 122.5(10) . . ? C25' C20' C19' 117.7(9) . . ? C22' C21' C20' 120.6(10) . . ? C21' C22' C23' 120.1(10) . . ? C24' C23' C22' 121.2(10) . . ? C23' C24' C25' 120.2(9) . . ? N26' C25' C24' 119.8(8) . . ? N26' C25' C20' 122.1(8) . . ? C24' C25' C20' 118.1(9) . . ? C17' N26' C25' 117.7(8) . . ? C17' N26' Cu2' 110.9(6) . . ? C25' N26' Cu2' 131.3(6) . . ? C36' N27' C28' 118.3(8) . . ? C36' N27' Cu1' 110.4(6) . . ? C28' N27' Cu1' 131.3(6) . . ? N27' C28' C29' 117.7(9) . . ? N27' C28' C33' 121.3(9) . . ? C29' C28' C33' 121.0(9) . . ? C28' C29' C30' 117.5(10) . . ? C31' C30' C29' 121.3(10) . . ? C32' C31' C30' 121.3(10) . . ? C31' C32' C33' 120.1(11) . . ? C34' C33' C28' 118.6(9) . . ? C34' C33' C32' 122.6(10) . . ? C28' C33' C32' 118.7(10) . . ? C35' C34' C33' 119.8(10) . . ? C34' C35' C36' 119.2(10) . . ? N27' C36' C37' 117.3(8) . . ? N27' C36' C35' 122.8(9) . . ? C37' C36' C35' 119.9(9) . . ? N38' C37' C36' 119.2(8) . . ? C37' N38' C39' 116.8(8) . . ? C37' N38' Cu1' 112.0(6) . . ? C39' N38' Cu1' 131.1(6) . . ? N38' C39' C40' 111.9(8) . . ? N41' C40' C39' 110.0(8) . . ? C42' N41' C40' 119.3(9) . . ? C42' N41' Cu2' 112.9(7) . . ? C40' N41' Cu2' 127.7(7) . . ? N41' C42' C43' 119.3(9) . . ? N52' C43' C44' 123.0(9) . . ? N52' C43' C42' 114.4(8) . . ? C44' C43' C42' 122.4(9) . . ? C45' C44' C43' 118.3(9) . . ? C44' C45' C46' 120.9(9) . . ? C45' C46' C47' 124.6(10) . . ? C45' C46' C51' 117.2(10) . . ? C47' C46' C51' 118.1(10) . . ? C48' C47' C46' 121.3(11) . . ? C47' C48' C49' 120.4(11) . . ? C50' C49' C48' 120.3(11) . . ? C49' C50' C51' 121.0(10) . . ? N52' C51' C50' 118.5(9) . . ? N52' C51' C46' 122.6(9) . . ? C50' C51' C46' 118.8(9) . . ? C43' N52' C51' 117.7(8) . . ? C43' N52' Cu2' 111.7(6) . . ? C51' N52' Cu2' 130.4(6) . . ? O59 Cl55 O56 108.8(5) . . ? O59 Cl55 O57 109.7(5) . . ? O56 Cl55 O57 110.3(5) . . ? O59 Cl55 O58 110.6(6) . . ? O56 Cl55 O58 108.7(4) . . ? O57 Cl55 O58 108.6(5) . . ? O63A Cl60 O61 109.7(12) . . ? O63A Cl60 O64 128.2(13) . . ? O61 Cl60 O64 119.1(7) . . ? O63A Cl60 O64A 123.9(16) . . ? O61 Cl60 O64A 108.3(12) . . ? O61 Cl60 O63 108.1(6) . . ? O64 Cl60 O63 93.4(8) . . ? O61 Cl60 O62 111.1(7) . . ? O64 Cl60 O62 124.1(8) . . ? O63 Cl60 O62 93.1(8) . . ? O67 Cl65 O69A 111.4(6) . . ? O67 Cl65 O68 110.7(5) . . ? O69A Cl65 O68 110.8(6) . . ? O67 Cl65 O66 106.3(6) . . ? O69A Cl65 O66 106.3(7) . . ? O68 Cl65 O66 111.3(6) . . ? O67 Cl65 O69 107.6(8) . . ? O68 Cl65 O69 99.0(8) . . ? O66 Cl65 O69 121.8(9) . . ? O72 Cl70 O74 107.5(9) . . ? O72 Cl70 O73 112.7(8) . . ? O74 Cl70 O73 109.0(10) . . ? O72 Cl70 O71 112.1(7) . . ? O74 Cl70 O71 108.9(8) . . ? O73 Cl70 O71 106.6(6) . . ? C75 C76 O77 118.2(16) . . ? C78 O77 C76 123(2) . . ? C79 C78 O77 122(3) . . ? C78 C79 C80 155(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 N12 C13 C14 N15 72.1(10) . . . . ? N38 C39 C40 N41 71.1(9) . . . . ? N12' C13' C14' N15' 74.2(11) . . . . ? N38' C39' C40' N41' 69.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 1.752 _refine_diff_density_min -1.171 _refine_diff_density_rms 0.121 #======END========================================================== data_Complex-2a _database_code_CSD 204787 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C34 H24 N6), (Ag Cl O4), (C H2 Cl2)' _chemical_formula_sum 'C35 H26 Ag Cl3 N6 O4' _chemical_formula_weight 808.84 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' Ag Ag -0.8971 1.1015 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.9900(3) _cell_length_b 12.7440(2) _cell_length_c 22.6650(3) _cell_angle_alpha 90.00 _cell_angle_beta 125.8021(6) _cell_angle_gamma 90.00 _cell_volume 6557.04(15) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5654 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.90 _exptl_crystal_description prisms _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8044 _exptl_absorpt_correction_T_max 0.9145 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7695 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.90 _reflns_number_total 7695 _reflns_number_gt 5654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+12.7901P] 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 7695 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.01107(11) 0.12905(19) 0.35132(13) 0.0179(5) Uani 1 1 d . . . C2 C -0.02295(13) 0.0884(2) 0.37081(16) 0.0215(7) Uani 1 1 d . . . C3 C -0.05600(15) 0.1573(3) 0.38292(18) 0.0298(8) Uani 1 1 d . . . H3 H -0.0552 0.2307 0.3762 0.036 Uiso 1 1 calc R . . C4 C -0.08914(17) 0.1184(3) 0.4043(2) 0.0376(9) Uani 1 1 d . . . H4 H -0.1117 0.1649 0.4116 0.045 Uiso 1 1 calc R . . C5 C -0.09012(17) 0.0097(3) 0.4155(2) 0.0395(9) Uani 1 1 d . . . H5 H -0.1123 -0.0162 0.4319 0.047 Uiso 1 1 calc R . . C6 C -0.05968(16) -0.0578(3) 0.4031(2) 0.0378(9) Uani 1 1 d . . . H6 H -0.0612 -0.1308 0.4102 0.045 Uiso 1 1 calc R . . C7 C -0.02551(15) -0.0210(3) 0.37948(18) 0.0285(8) Uani 1 1 d . . . C8 C 0.00553(16) -0.0871(3) 0.3640(2) 0.0360(9) Uani 1 1 d . . . H8 H 0.0029 -0.1610 0.3667 0.043 Uiso 1 1 calc R . . C9 C 0.03986(15) -0.0458(2) 0.34479(19) 0.0290(8) Uani 1 1 d . . . H9 H 0.0616 -0.0902 0.3349 0.035 Uiso 1 1 calc R . . C10 C 0.04203(13) 0.0633(2) 0.34024(16) 0.0185(6) Uani 1 1 d . . . C11 C 0.08058(13) 0.1079(2) 0.32239(15) 0.0184(6) Uani 1 1 d . . . H11 H 0.1023 0.0622 0.3131 0.022 Uiso 1 1 calc R . . N12 N 0.08546(10) 0.20706(18) 0.31912(13) 0.0167(5) Uani 1 1 d . . . N13 N 0.12468(11) 0.23130(19) 0.30138(13) 0.0175(5) Uani 1 1 d . . . C14 C 0.14299(13) 0.3268(2) 0.31377(15) 0.0168(6) Uani 1 1 d . . . C15 C 0.12576(12) 0.4075(2) 0.34704(15) 0.0157(6) Uani 1 1 d . . . N16 N 0.08164(10) 0.46976(18) 0.30796(13) 0.0170(5) Uani 1 1 d . . . N17 N 0.04759(10) 0.45011(19) 0.23283(12) 0.0160(5) Uani 1 1 d . . . C18 C 0.03233(13) 0.5320(2) 0.19373(16) 0.0188(6) Uani 1 1 d . . . H18 H 0.0460 0.5989 0.2160 0.023 Uiso 1 1 calc R . . C19 C -0.00654(13) 0.5234(2) 0.11400(16) 0.0181(6) Uani 1 1 d . . . C20 C -0.01680(15) 0.6125(2) 0.07121(17) 0.0240(7) Uani 1 1 d . . . H20 H 0.0011 0.6778 0.0935 0.029 Uiso 1 1 calc R . . C21 C -0.05298(15) 0.6035(2) -0.00311(18) 0.0267(7) Uani 1 1 d . . . H21 H -0.0608 0.6631 -0.0326 0.032 Uiso 1 1 calc R . . C22 C -0.07864(14) 0.5060(2) -0.03581(17) 0.0236(7) Uani 1 1 d . . . C23 C -0.11508(15) 0.4892(3) -0.11155(18) 0.0290(8) Uani 1 1 d . . . H23 H -0.1243 0.5463 -0.1436 0.035 Uiso 1 1 calc R . . C24 C -0.13716(15) 0.3922(3) -0.13928(18) 0.0324(8) Uani 1 1 d . . . H24 H -0.1612 0.3818 -0.1904 0.039 Uiso 1 1 calc R . . C25 C -0.12470(14) 0.3075(3) -0.09272(17) 0.0265(7) Uani 1 1 d . . . H25 H -0.1408 0.2404 -0.1129 0.032 Uiso 1 1 calc R . . C26 C -0.08964(13) 0.3197(2) -0.01858(17) 0.0223(7) Uani 1 1 d . . . H26 H -0.0814 0.2616 0.0123 0.027 Uiso 1 1 calc R . . C27 C -0.06593(13) 0.4196(2) 0.01148(16) 0.0184(6) Uani 1 1 d . . . N28 N -0.03060(11) 0.43028(19) 0.08529(13) 0.0176(5) Uani 1 1 d . . . C29 C 0.18388(13) 0.3589(2) 0.29607(15) 0.0203(6) Uani 1 1 d . . . C30 C 0.20786(13) 0.4587(3) 0.31255(16) 0.0228(7) Uani 1 1 d . . . H30 H 0.1970 0.5083 0.3340 0.027 Uiso 1 1 calc R . . C31 C 0.24817(14) 0.4868(3) 0.29759(18) 0.0293(8) Uani 1 1 d . . . H31 H 0.2647 0.5552 0.3093 0.035 Uiso 1 1 calc R . . C32 C 0.26403(14) 0.4157(3) 0.26605(18) 0.0320(8) Uani 1 1 d . . . H32 H 0.2920 0.4346 0.2569 0.038 Uiso 1 1 calc R . . C33 C 0.23897(15) 0.3163(3) 0.24769(18) 0.0311(8) Uani 1 1 d . . . H33 H 0.2486 0.2681 0.2241 0.037 Uiso 1 1 calc R . . C34 C 0.20014(15) 0.2873(3) 0.26365(17) 0.0248(7) Uani 1 1 d . . . H34 H 0.1843 0.2183 0.2526 0.030 Uiso 1 1 calc R . . C35 C 0.16199(12) 0.4204(2) 0.42656(15) 0.0159(6) Uani 1 1 d . . . C36 C 0.19039(13) 0.3335(2) 0.47195(16) 0.0201(6) Uani 1 1 d . . . H36 H 0.1868 0.2665 0.4514 0.024 Uiso 1 1 calc R . . C37 C 0.22379(14) 0.3450(3) 0.54699(17) 0.0247(7) Uani 1 1 d . . . H37 H 0.2423 0.2857 0.5776 0.030 Uiso 1 1 calc R . . C38 C 0.23008(14) 0.4428(3) 0.57708(17) 0.0273(7) Uani 1 1 d . . . H38 H 0.2538 0.4508 0.6285 0.033 Uiso 1 1 calc R . . C39 C 0.20198(14) 0.5294(3) 0.53268(17) 0.0251(7) Uani 1 1 d . . . H39 H 0.2062 0.5962 0.5539 0.030 Uiso 1 1 calc R . . C40 C 0.16774(13) 0.5192(2) 0.45758(16) 0.0208(7) Uani 1 1 d . . . H40 H 0.1483 0.5786 0.4273 0.025 Uiso 1 1 calc R . . Ag41 Ag 0.015036(10) 0.303141(17) 0.332414(13) 0.02136(8) Uani 1 1 d . . . Cl42 Cl 0.35811(4) 0.28000(6) 0.19851(4) 0.02498(18) Uani 1 1 d . . . O43 O 0.34717(12) 0.38973(18) 0.18346(15) 0.0418(7) Uani 1 1 d . . . O44 O 0.38557(15) 0.2608(2) 0.27359(15) 0.0550(8) Uani 1 1 d . . . O45 O 0.30413(14) 0.2235(2) 0.1578(2) 0.0749(11) Uani 1 1 d . . . O46 O 0.39622(17) 0.2455(2) 0.1802(2) 0.0666(10) Uani 1 1 d . . . C47 C 0.30220(17) 0.3882(3) 0.0029(2) 0.0365(9) Uani 1 1 d . . . H47A H 0.3055 0.3766 0.0483 0.044 Uiso 1 1 calc R . . H47B H 0.2610 0.3733 -0.0386 0.044 Uiso 1 1 calc R . . Cl48 Cl 0.34988(4) 0.30062(7) 0.00017(6) 0.0417(2) Uani 1 1 d . . . Cl49 Cl 0.31880(4) 0.52085(7) -0.00114(5) 0.0365(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0170(13) 0.0169(13) 0.0146(12) -0.0005(10) 0.0064(11) -0.0021(10) C2 0.0190(16) 0.0255(16) 0.0157(14) -0.0038(13) 0.0078(13) -0.0048(13) C3 0.035(2) 0.0303(18) 0.0324(18) -0.0070(15) 0.0247(17) -0.0058(15) C4 0.036(2) 0.047(2) 0.040(2) -0.0153(18) 0.0282(19) -0.0136(17) C5 0.035(2) 0.053(2) 0.036(2) -0.0046(18) 0.0235(19) -0.0195(18) C6 0.033(2) 0.035(2) 0.046(2) 0.0043(18) 0.0232(19) -0.0110(16) C7 0.0238(18) 0.0264(18) 0.0307(18) 0.0021(15) 0.0133(15) -0.0066(14) C8 0.033(2) 0.0199(17) 0.056(2) 0.0033(17) 0.0265(19) -0.0050(15) C9 0.0237(18) 0.0168(16) 0.040(2) -0.0013(15) 0.0152(16) 0.0005(13) C10 0.0178(15) 0.0138(15) 0.0160(14) 0.0003(12) 0.0054(12) -0.0006(12) C11 0.0176(16) 0.0173(16) 0.0168(14) -0.0012(12) 0.0080(13) 0.0019(12) N12 0.0152(13) 0.0183(14) 0.0159(12) 0.0001(10) 0.0088(10) -0.0006(10) N13 0.0175(13) 0.0200(13) 0.0157(12) 0.0041(10) 0.0102(11) 0.0044(10) C14 0.0158(15) 0.0199(16) 0.0114(13) 0.0064(12) 0.0061(12) 0.0059(11) C15 0.0127(14) 0.0159(14) 0.0177(14) -0.0004(12) 0.0085(12) -0.0046(11) N16 0.0149(13) 0.0182(13) 0.0150(12) -0.0002(10) 0.0072(11) -0.0029(10) N17 0.0129(12) 0.0178(13) 0.0146(12) 0.0008(10) 0.0065(10) 0.0007(9) C18 0.0191(16) 0.0150(15) 0.0230(15) -0.0009(13) 0.0126(13) -0.0003(12) C19 0.0203(16) 0.0160(15) 0.0220(15) 0.0027(12) 0.0145(14) 0.0053(12) C20 0.0354(19) 0.0137(15) 0.0268(17) 0.0016(13) 0.0204(16) 0.0029(13) C21 0.036(2) 0.0225(17) 0.0284(17) 0.0119(14) 0.0226(16) 0.0121(14) C22 0.0255(18) 0.0278(17) 0.0222(16) 0.0088(14) 0.0167(15) 0.0141(14) C23 0.0300(19) 0.037(2) 0.0228(17) 0.0129(15) 0.0171(16) 0.0186(15) C24 0.0300(19) 0.046(2) 0.0185(16) 0.0014(16) 0.0127(15) 0.0165(16) C25 0.0215(17) 0.0316(18) 0.0205(16) -0.0059(14) 0.0091(14) 0.0068(14) C26 0.0187(16) 0.0251(17) 0.0226(16) 0.0035(13) 0.0118(14) 0.0085(13) C27 0.0143(15) 0.0256(16) 0.0157(14) 0.0013(12) 0.0090(12) 0.0075(12) N28 0.0168(13) 0.0187(13) 0.0184(13) 0.0024(10) 0.0109(11) 0.0045(10) C29 0.0165(15) 0.0293(17) 0.0136(14) 0.0067(13) 0.0079(13) 0.0037(13) C30 0.0178(16) 0.0293(17) 0.0159(15) 0.0067(13) 0.0069(13) -0.0001(13) C31 0.0203(17) 0.038(2) 0.0236(17) 0.0104(15) 0.0095(15) -0.0008(14) C32 0.0178(17) 0.052(2) 0.0275(18) 0.0171(17) 0.0140(15) 0.0064(16) C33 0.0288(19) 0.042(2) 0.0274(17) 0.0100(16) 0.0190(16) 0.0126(16) C34 0.0265(18) 0.0267(18) 0.0258(17) 0.0066(14) 0.0179(15) 0.0077(13) C35 0.0114(14) 0.0220(15) 0.0149(14) 0.0000(12) 0.0081(12) -0.0020(11) C36 0.0169(15) 0.0247(16) 0.0199(15) 0.0000(13) 0.0114(13) -0.0001(12) C37 0.0190(16) 0.0350(19) 0.0187(15) 0.0077(14) 0.0103(14) 0.0050(14) C38 0.0209(17) 0.043(2) 0.0164(15) -0.0015(15) 0.0100(14) -0.0027(14) C39 0.0242(17) 0.0275(18) 0.0250(17) -0.0068(14) 0.0152(15) -0.0045(13) C40 0.0177(16) 0.0226(16) 0.0222(16) -0.0025(13) 0.0117(14) -0.0009(12) Ag41 0.02382(14) 0.01451(13) 0.02465(13) -0.00184(9) 0.01355(11) 0.00062(9) Cl42 0.0292(4) 0.0208(4) 0.0262(4) 0.0024(3) 0.0169(4) -0.0012(3) O43 0.0503(17) 0.0228(13) 0.0512(16) 0.0109(12) 0.0290(14) 0.0069(11) O44 0.085(2) 0.0479(17) 0.0318(15) 0.0110(13) 0.0337(16) 0.0004(16) O45 0.045(2) 0.0500(19) 0.088(3) -0.0176(18) 0.0159(19) -0.0238(15) O46 0.106(3) 0.0427(17) 0.111(3) 0.0071(18) 0.097(3) 0.0090(18) C47 0.037(2) 0.049(2) 0.035(2) -0.0014(17) 0.0274(18) -0.0004(17) Cl48 0.0427(6) 0.0428(5) 0.0522(6) -0.0098(5) 0.0350(5) -0.0037(4) Cl49 0.0293(5) 0.0447(5) 0.0270(4) 0.0002(4) 0.0117(4) 0.0066(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 N1 C10 1.330(4) . ? N1 C2 1.365(4) . ? N1 Ag41 2.275(2) . ? C2 C7 1.416(5) . ? C2 C3 1.414(5) . ? C3 C4 1.366(5) . ? C3 H3 0.9500 . ? C4 C5 1.411(5) . ? C4 H4 0.9500 . ? C5 C6 1.351(5) . ? C5 H5 0.9500 . ? C6 C7 1.420(5) . ? C6 H6 0.9500 . ? C7 C8 1.394(5) . ? C8 C9 1.370(5) . ? C8 H8 0.9500 . ? C9 C10 1.399(4) . ? C9 H9 0.9500 . ? C10 C11 1.470(4) . ? C11 N12 1.277(4) . ? C11 H11 0.9500 . ? N12 N13 1.407(3) . ? N12 Ag41 2.484(2) . ? N13 C14 1.286(4) . ? C14 C29 1.475(4) . ? C14 C15 1.512(4) . ? C15 N16 1.288(4) . ? C15 C35 1.472(4) . ? N16 N17 1.404(3) . ? N17 C18 1.271(4) . ? N17 Ag41 2.395(2) 2 ? C18 C19 1.470(4) . ? C18 H18 0.9500 . ? C19 N28 1.331(4) . ? C19 C20 1.409(4) . ? C20 C21 1.371(5) . ? C20 H20 0.9500 . ? C21 C22 1.409(5) . ? C21 H21 0.9500 . ? C22 C23 1.408(5) . ? C22 C27 1.429(4) . ? C23 C24 1.360(5) . ? C23 H23 0.9500 . ? C24 C25 1.404(5) . ? C24 H24 0.9500 . ? C25 C26 1.372(4) . ? C25 H25 0.9500 . ? C26 C27 1.412(4) . ? C26 H26 0.9500 . ? C27 N28 1.364(4) . ? N28 Ag41 2.312(2) 2 ? C29 C30 1.384(4) . ? C29 C34 1.404(4) . ? C30 C31 1.401(5) . ? C30 H30 0.9500 . ? C31 C32 1.378(5) . ? C31 H31 0.9500 . ? C32 C33 1.389(5) . ? C32 H32 0.9500 . ? C33 C34 1.381(5) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.400(4) . ? C35 C40 1.405(4) . ? C36 C37 1.389(4) . ? C36 H36 0.9500 . ? C37 C38 1.381(5) . ? C37 H37 0.9500 . ? C38 C39 1.387(5) . ? C38 H38 0.9500 . ? C39 C40 1.387(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? Ag41 N28 2.312(2) 2 ? Ag41 N17 2.395(2) 2 ? Ag41 Ag41 3.3145(5) 2 ? Cl42 O46 1.421(3) . ? Cl42 O44 1.420(3) . ? Cl42 O45 1.422(3) . ? Cl42 O43 1.430(2) . ? C47 Cl48 1.769(4) . ? C47 Cl49 1.769(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? 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 C10 N1 C2 118.5(3) . . ? C10 N1 Ag41 118.0(2) . . ? C2 N1 Ag41 123.5(2) . . ? N1 C2 C7 121.4(3) . . ? N1 C2 C3 119.1(3) . . ? C7 C2 C3 119.5(3) . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.6(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 120.4(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 121.0(3) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C2 118.0(3) . . ? C8 C7 C6 123.5(3) . . ? C2 C7 C6 118.5(3) . . ? C9 C8 C7 120.3(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 118.3(3) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N1 C10 C9 123.4(3) . . ? N1 C10 C11 118.2(3) . . ? C9 C10 C11 118.4(3) . . ? N12 C11 C10 121.3(3) . . ? N12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 N12 N13 111.2(2) . . ? C11 N12 Ag41 111.2(2) . . ? N13 N12 Ag41 137.20(17) . . ? C14 N13 N12 115.1(2) . . ? N13 C14 C29 118.5(3) . . ? N13 C14 C15 123.4(3) . . ? C29 C14 C15 118.1(3) . . ? N16 C15 C35 118.1(3) . . ? N16 C15 C14 122.2(3) . . ? C35 C15 C14 119.6(2) . . ? C15 N16 N17 114.9(2) . . ? C18 N17 N16 114.3(2) . . ? C18 N17 Ag41 112.7(2) . 2 ? N16 N17 Ag41 128.36(17) . 2 ? N17 C18 C19 120.1(3) . . ? N17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? N28 C19 C20 122.7(3) . . ? N28 C19 C18 117.8(3) . . ? C20 C19 C18 119.5(3) . . ? C21 C20 C19 119.0(3) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 123.9(3) . . ? C21 C22 C27 117.3(3) . . ? C23 C22 C27 118.9(3) . . ? C24 C23 C22 120.7(3) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.4(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 121.2(3) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 119.4(3) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? N28 C27 C26 118.7(3) . . ? N28 C27 C22 121.8(3) . . ? C26 C27 C22 119.5(3) . . ? C19 N28 C27 119.0(3) . . ? C19 N28 Ag41 115.32(19) . 2 ? C27 N28 Ag41 125.4(2) . 2 ? C30 C29 C34 119.0(3) . . ? C30 C29 C14 120.9(3) . . ? C34 C29 C14 120.2(3) . . ? C29 C30 C31 120.1(3) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 120.5(3) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 119.7(3) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C34 C33 C32 120.2(3) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C29 120.6(3) . . ? C33 C34 H34 119.7 . . ? C29 C34 H34 119.7 . . ? C36 C35 C40 119.5(3) . . ? C36 C35 C15 120.0(3) . . ? C40 C35 C15 120.5(3) . . ? C37 C36 C35 120.1(3) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 120.0(3) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.3(3) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 120.5(3) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C35 119.5(3) . . ? C39 C40 H40 120.2 . . ? C35 C40 H40 120.2 . . ? N1 Ag41 N28 122.59(8) . 2 ? N1 Ag41 N17 141.31(8) . 2 ? N28 Ag41 N17 71.00(8) 2 2 ? N1 Ag41 N12 70.83(8) . . ? N28 Ag41 N12 130.92(8) 2 . ? N17 Ag41 N12 131.05(8) 2 . ? N1 Ag41 Ag41 101.78(6) . 2 ? N28 Ag41 Ag41 135.50(6) 2 2 ? N17 Ag41 Ag41 72.09(6) 2 2 ? N12 Ag41 Ag41 63.87(5) . 2 ? O46 Cl42 O44 108.9(2) . . ? O46 Cl42 O45 110.4(2) . . ? O44 Cl42 O45 108.4(2) . . ? O46 Cl42 O43 109.00(17) . . ? O44 Cl42 O43 110.17(17) . . ? O45 Cl42 O43 110.04(19) . . ? Cl48 C47 Cl49 112.0(2) . . ? Cl48 C47 H47A 109.2 . . ? Cl49 C47 H47A 109.2 . . ? Cl48 C47 H47B 109.2 . . ? Cl49 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.598 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.099 #=====END============================================================== data_Complex-2b _database_code_CSD 204788 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C34 H24 N6), 2(Cu Cl O4), (C H2 Cl2), (C6 H14)' _chemical_formula_sum 'C75 H64 Cl4 Cu2 N12 O8' _chemical_formula_weight 1530.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 12.8350(2) _cell_length_b 41.4820(7) _cell_length_c 13.3050(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.6280(9) _cell_angle_gamma 90.00 _cell_volume 6629.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6679 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 25.44 _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8113 _exptl_absorpt_correction_T_max 0.9334 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '0.7 Phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11469 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1125 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.44 _reflns_number_total 11469 _reflns_number_gt 6679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains two units of the di-nuclear complex, and severely disordered molecules of dichloromethane and n-hexane solvent. ; _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^)+(0.0753P)^2^+41.3385P] 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 11469 _refine_ls_number_parameters 928 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1475 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.2153 _refine_ls_wR_factor_gt 0.1779 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.197 _refine_ls_shift/su_mean 0.025 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.7703(5) 0.16602(13) 0.6590(4) 0.0269(13) Uani 1 1 d . . . C2 C 0.8752(6) 0.17556(16) 0.7214(5) 0.0316(17) Uani 1 1 d . . . C3 C 0.9654(6) 0.15751(18) 0.7184(6) 0.0399(19) Uani 1 1 d . . . H3 H 0.9536 0.1391 0.6731 0.048 Uiso 1 1 calc R . . C4 C 1.0721(7) 0.1664(2) 0.7813(7) 0.050(2) Uani 1 1 d . . . H4 H 1.1338 0.1540 0.7799 0.060 Uiso 1 1 calc R . . C5 C 1.0897(7) 0.1940(2) 0.8480(6) 0.052(2) Uani 1 1 d . . . H5 H 1.1635 0.1998 0.8910 0.062 Uiso 1 1 calc R . . C6 C 1.0043(7) 0.2119(2) 0.8516(6) 0.046(2) Uani 1 1 d . . . H6 H 1.0178 0.2303 0.8970 0.055 Uiso 1 1 calc R . . C7 C 0.8924(6) 0.20333(16) 0.7866(5) 0.0325(17) Uani 1 1 d . . . C8 C 0.7999(6) 0.22169(16) 0.7853(5) 0.0366(18) Uani 1 1 d . . . H8 H 0.8101 0.2409 0.8267 0.044 Uiso 1 1 calc R . . C9 C 0.6954(6) 0.21187(16) 0.7242(5) 0.0315(17) Uani 1 1 d . . . H9 H 0.6318 0.2237 0.7235 0.038 Uiso 1 1 calc R . . C10 C 0.6845(6) 0.18376(16) 0.6623(5) 0.0267(15) Uani 1 1 d . . . C11 C 0.5728(6) 0.17172(15) 0.5963(5) 0.0270(16) Uani 1 1 d . . . H11 H 0.5079 0.1836 0.5914 0.032 Uiso 1 1 calc R . . N12 N 0.5648(5) 0.14483(13) 0.5456(4) 0.0287(13) Uani 1 1 d . . . N13 N 0.4515(5) 0.13863(13) 0.4859(4) 0.0304(14) Uani 1 1 d . . . C14 C 0.4263(6) 0.11122(16) 0.4396(5) 0.0365(18) Uani 1 1 d . . . C15 C 0.5049(7) 0.08315(17) 0.4466(6) 0.047(2) Uani 1 1 d . . . N16 N 0.5485(6) 0.07568(14) 0.3757(5) 0.0482(19) Uani 1 1 d . . . N17 N 0.5233(5) 0.09541(14) 0.2843(5) 0.0426(17) Uani 1 1 d . . . C18 C 0.5564(7) 0.08151(18) 0.2144(6) 0.049(2) Uani 1 1 d . . . H18 H 0.5942 0.0614 0.2306 0.058 Uiso 1 1 calc R . . C19 C 0.5360(7) 0.09657(18) 0.1107(6) 0.047(2) Uani 1 1 d . . . C20 C 0.5621(7) 0.0801(2) 0.0312(6) 0.059(3) Uani 1 1 d . . . H20 H 0.5980 0.0597 0.0459 0.071 Uiso 1 1 calc R . . C21 C 0.5348(8) 0.0939(2) -0.0690(7) 0.066(3) Uani 1 1 d . . . H21 H 0.5509 0.0829 -0.1244 0.079 Uiso 1 1 calc R . . C22 C 0.4829(7) 0.1244(2) -0.0889(6) 0.052(2) Uani 1 1 d . . . C23 C 0.4501(8) 0.1398(2) -0.1895(6) 0.058(2) Uani 1 1 d . . . H23 H 0.4617 0.1293 -0.2482 0.069 Uiso 1 1 calc R . . C24 C 0.4025(7) 0.1692(2) -0.2039(6) 0.049(2) Uani 1 1 d . . . H24 H 0.3818 0.1794 -0.2720 0.059 Uiso 1 1 calc R . . C25 C 0.3832(6) 0.18494(19) -0.1175(6) 0.043(2) Uani 1 1 d . . . H25 H 0.3500 0.2057 -0.1284 0.052 Uiso 1 1 calc R . . C26 C 0.4115(6) 0.17074(18) -0.0192(6) 0.0384(18) Uani 1 1 d . . . H26 H 0.3985 0.1816 0.0382 0.046 Uiso 1 1 calc R . . C27 C 0.4602(7) 0.13991(18) -0.0031(6) 0.042(2) Uani 1 1 d . . . N28 N 0.4879(5) 0.12577(14) 0.0964(5) 0.0437(17) Uani 1 1 d . . . C29 C 0.3072(7) 0.10509(17) 0.3805(6) 0.045(2) Uani 1 1 d . . . C30 C 0.2269(7) 0.1264(2) 0.3896(7) 0.058(2) Uani 1 1 d . . . H30 H 0.2491 0.1449 0.4341 0.070 Uiso 1 1 calc R . . C31 C 0.1145(7) 0.1206(2) 0.3340(8) 0.074(3) Uani 1 1 d . . . H31 H 0.0603 0.1353 0.3400 0.089 Uiso 1 1 calc R . . C32 C 0.0822(9) 0.0943(3) 0.2716(9) 0.090(4) Uani 1 1 d . . . H32 H 0.0052 0.0907 0.2337 0.108 Uiso 1 1 calc R . . C33 C 0.1591(9) 0.0725(2) 0.2617(8) 0.082(4) Uani 1 1 d . . . H33 H 0.1347 0.0537 0.2187 0.098 Uiso 1 1 calc R . . C34 C 0.2714(8) 0.07780(19) 0.3143(7) 0.062(3) Uani 1 1 d . . . H34 H 0.3244 0.0631 0.3058 0.074 Uiso 1 1 calc R . . C35 C 0.5245(7) 0.06075(17) 0.5381(6) 0.048(2) Uani 1 1 d . . . C36 C 0.5929(7) 0.03416(18) 0.5478(7) 0.064(3) Uani 1 1 d . . . H36 H 0.6298 0.0309 0.4979 0.077 Uiso 1 1 calc R . . C37 C 0.6071(11) 0.0124(3) 0.6302(11) 0.095(5) Uani 1 1 d . . . H37 H 0.6567 -0.0051 0.6377 0.114 Uiso 1 1 calc R . . C38 C 0.5539(11) 0.0152(2) 0.6998(9) 0.092(5) Uani 1 1 d . . . H38 H 0.5641 -0.0005 0.7546 0.110 Uiso 1 1 calc R . . C39 C 0.4826(10) 0.0414(2) 0.6905(7) 0.079(3) Uani 1 1 d . . . H39 H 0.4438 0.0436 0.7391 0.095 Uiso 1 1 calc R . . C40 C 0.4681(9) 0.0648(2) 0.6092(7) 0.063(3) Uani 1 1 d . . . H40 H 0.4207 0.0828 0.6033 0.076 Uiso 1 1 calc R . . Cu41 Cu 0.71836(7) 0.128305(19) 0.55644(6) 0.0301(2) Uani 1 1 d . . . Cl42 Cl 0.36059(15) 0.24224(4) 0.58970(13) 0.0330(4) Uani 1 1 d . . . O43 O 0.4226(5) 0.24423(13) 0.7025(4) 0.0532(15) Uani 1 1 d . . . O44 O 0.4343(5) 0.24586(13) 0.5316(4) 0.0520(15) Uani 1 1 d . . . O45 O 0.3080(4) 0.21110(12) 0.5647(4) 0.0480(14) Uani 1 1 d . . . O46 O 0.2785(4) 0.26730(13) 0.5586(4) 0.0526(15) Uani 1 1 d . . . N47 N 0.3218(5) 0.16451(13) 0.2157(4) 0.0325(14) Uani 1 1 d . . . C48 C 0.2156(6) 0.15704(17) 0.1515(6) 0.041(2) Uani 1 1 d . . . C49 C 0.1993(8) 0.13036(19) 0.0808(6) 0.060(3) Uani 1 1 d . . . H49 H 0.2607 0.1180 0.0784 0.072 Uiso 1 1 calc R . . C50 C 0.0900(9) 0.1227(2) 0.0145(7) 0.075(3) Uani 1 1 d . . . H50 H 0.0771 0.1047 -0.0329 0.090 Uiso 1 1 calc R . . C51 C 0.0018(8) 0.1408(2) 0.0177(8) 0.073(3) Uani 1 1 d . . . H51 H -0.0712 0.1353 -0.0288 0.087 Uiso 1 1 calc R . . C52 C 0.0146(8) 0.16605(19) 0.0836(7) 0.063(3) Uani 1 1 d . . . H52 H -0.0486 0.1780 0.0835 0.076 Uiso 1 1 calc R . . C53 C 0.1239(7) 0.17514(18) 0.1547(6) 0.045(2) Uani 1 1 d . . . C54 C 0.1434(6) 0.20082(17) 0.2289(6) 0.0388(19) Uani 1 1 d . . . H54 H 0.0829 0.2127 0.2356 0.047 Uiso 1 1 calc R . . C55 C 0.2491(6) 0.20824(16) 0.2899(5) 0.0312(17) Uani 1 1 d . . . H55 H 0.2640 0.2258 0.3389 0.037 Uiso 1 1 calc R . . C56 C 0.3375(6) 0.18964(15) 0.2801(5) 0.0275(16) Uani 1 1 d . . . C57 C 0.4512(6) 0.19835(15) 0.3425(5) 0.0281(16) Uani 1 1 d . . . H57 H 0.4669 0.2161 0.3908 0.034 Uiso 1 1 calc R . . N58 N 0.5313(5) 0.18137(12) 0.3308(4) 0.0278(13) Uani 1 1 d . . . N59 N 0.6355(5) 0.19379(12) 0.3979(4) 0.0269(13) Uani 1 1 d . . . C60 C 0.7236(6) 0.18215(16) 0.3862(5) 0.0295(16) Uani 1 1 d . . . C61 C 0.7250(6) 0.15736(16) 0.3037(5) 0.0303(16) Uani 1 1 d . . . N62 N 0.7497(5) 0.12759(13) 0.3236(4) 0.0334(14) Uani 1 1 d . . . N63 N 0.7645(5) 0.11676(13) 0.4277(4) 0.0338(14) Uani 1 1 d . . . C64 C 0.8099(6) 0.08851(17) 0.4423(6) 0.0370(18) Uani 1 1 d . . . H64 H 0.8295 0.0787 0.3870 0.044 Uiso 1 1 calc R . . C65 C 0.8308(6) 0.07185(16) 0.5439(6) 0.0348(18) Uani 1 1 d . . . C66 C 0.8868(7) 0.04153(18) 0.5643(6) 0.047(2) Uani 1 1 d . . . H66 H 0.9092 0.0314 0.5111 0.056 Uiso 1 1 calc R . . C67 C 0.9075(7) 0.02744(19) 0.6624(6) 0.048(2) Uani 1 1 d . . . H67 H 0.9442 0.0072 0.6776 0.058 Uiso 1 1 calc R . . C68 C 0.8750(6) 0.04260(16) 0.7408(6) 0.0349(17) Uani 1 1 d . . . C69 C 0.8945(6) 0.02948(18) 0.8427(6) 0.0396(19) Uani 1 1 d . . . H69 H 0.9329 0.0096 0.8617 0.048 Uiso 1 1 calc R . . C70 C 0.8589(6) 0.04498(18) 0.9143(6) 0.0404(19) Uani 1 1 d . . . H70 H 0.8737 0.0360 0.9836 0.049 Uiso 1 1 calc R . . C71 C 0.8010(6) 0.07396(17) 0.8877(6) 0.0370(18) Uani 1 1 d . . . H71 H 0.7771 0.0847 0.9389 0.044 Uiso 1 1 calc R . . C72 C 0.7785(6) 0.08701(17) 0.7884(5) 0.0323(17) Uani 1 1 d . . . H72 H 0.7367 0.1064 0.7697 0.039 Uiso 1 1 calc R . . C73 C 0.8165(5) 0.07210(15) 0.7138(5) 0.0273(16) Uani 1 1 d . . . N74 N 0.7948(5) 0.08634(12) 0.6150(4) 0.0282(13) Uani 1 1 d . . . C75 C 0.8308(6) 0.19642(15) 0.4488(5) 0.0294(16) Uani 1 1 d . . . C76 C 0.9316(6) 0.18516(19) 0.4425(6) 0.044(2) Uani 1 1 d . . . H76 H 0.9300 0.1675 0.3967 0.053 Uiso 1 1 calc R . . C77 C 1.0336(7) 0.1990(2) 0.5009(6) 0.048(2) Uani 1 1 d . . . H77 H 1.1009 0.1907 0.4970 0.057 Uiso 1 1 calc R . . C78 C 1.0341(7) 0.22511(19) 0.5644(6) 0.043(2) Uani 1 1 d . . . H78 H 1.1028 0.2351 0.6042 0.052 Uiso 1 1 calc R . . C79 C 0.9365(6) 0.23707(17) 0.5715(6) 0.0360(18) Uani 1 1 d . . . H79 H 0.9389 0.2553 0.6154 0.043 Uiso 1 1 calc R . . C80 C 0.8373(6) 0.22308(15) 0.5164(5) 0.0291(16) Uani 1 1 d . . . H80 H 0.7712 0.2314 0.5235 0.035 Uiso 1 1 calc R . . C81 C 0.7112(6) 0.16957(16) 0.1946(5) 0.0326(17) Uani 1 1 d . . . C82 C 0.7411(7) 0.15046(18) 0.1233(6) 0.045(2) Uani 1 1 d . . . H82 H 0.7721 0.1297 0.1449 0.054 Uiso 1 1 calc R . . C83 C 0.7261(8) 0.1615(2) 0.0210(6) 0.051(2) Uani 1 1 d . . . H83 H 0.7447 0.1481 -0.0281 0.061 Uiso 1 1 calc R . . C84 C 0.6841(7) 0.1918(2) -0.0091(6) 0.048(2) Uani 1 1 d . . . H84 H 0.6761 0.1996 -0.0786 0.057 Uiso 1 1 calc R . . C85 C 0.6531(6) 0.21141(18) 0.0602(6) 0.0387(19) Uani 1 1 d . . . H85 H 0.6223 0.2322 0.0380 0.046 Uiso 1 1 calc R . . C86 C 0.6677(6) 0.20012(16) 0.1622(5) 0.0310(16) Uani 1 1 d . . . H86 H 0.6479 0.2134 0.2108 0.037 Uiso 1 1 calc R . . Cu87 Cu 0.46697(8) 0.14203(2) 0.23186(7) 0.0380(3) Uani 1 1 d . . . Cl88 Cl 0.83922(19) 0.03316(6) 0.21496(15) 0.0550(6) Uani 1 1 d . . . O89 O 0.9171(5) 0.03637(15) 0.3228(4) 0.0593(17) Uani 1 1 d . . . O90 O 0.8196(5) 0.06413(16) 0.1642(5) 0.078(2) Uani 1 1 d . . . O91 O 0.7376(5) 0.02016(15) 0.2163(5) 0.0722(19) Uani 1 1 d . . . O92 O 0.8666(10) 0.0052(3) 0.1592(9) 0.044(3) Uani 0.50 1 d P . . O92A O 0.9017(10) 0.0182(3) 0.1573(10) 0.036(3) Uiso 0.50 1 d P . . C93 C 0.645(2) -0.0146(6) -0.0079(19) 0.091(7) Uiso 0.50 1 d P . . Cl94 Cl 0.6947(8) -0.0450(2) -0.0742(11) 0.059(2) Uani 0.50 1 d P . . Cl95 Cl 0.5088(5) -0.00563(11) -0.0677(5) 0.0748(15) Uani 0.50 1 d P . . C96 C 0.8460(16) -0.0583(6) 0.4753(12) 0.063(6) Uani 0.50 1 d P . . Cl97 Cl 0.8119(4) -0.03259(11) 0.3901(4) 0.0630(13) Uani 0.50 1 d P . . Cl98 Cl 0.8805(6) -0.09801(17) 0.4112(4) 0.0750(17) Uani 0.50 1 d P . . C99 C 0.7503(7) -0.0840(2) 0.1937(10) 0.057(3) Uani 1 1 d . . . C100 C 0.7721(12) -0.0788(4) 0.1244(11) 0.060(4) Uani 1 1 d . . . C101 C 0.743(3) -0.0429(8) 0.073(2) 0.264(13) Uiso 1 1 d . . . C102 C 0.7276(18) -0.0414(5) -0.0592(17) 0.060(7) Uiso 1 1 d . . . C103 C 0.825(2) -0.0983(6) 0.381(2) 0.069(8) Uiso 0.50 1 d P . . C104 C 0.807(2) -0.0825(7) 0.133(2) 0.043(8) Uiso 0.50 1 d P . . C105 C 0.841(3) -0.0624(8) 0.296(3) 0.142(11) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.030(3) 0.027(3) 0.024(3) 0.002(2) 0.009(2) 0.004(3) C2 0.036(4) 0.024(4) 0.032(4) 0.000(3) 0.008(3) 0.000(3) C3 0.036(4) 0.037(4) 0.037(4) -0.007(3) 0.001(3) 0.002(4) C4 0.037(5) 0.046(5) 0.062(5) -0.002(4) 0.010(4) 0.007(4) C5 0.039(5) 0.050(5) 0.047(5) -0.007(4) -0.008(4) -0.001(4) C6 0.043(5) 0.045(5) 0.042(5) -0.005(4) 0.004(4) 0.000(4) C7 0.031(4) 0.027(4) 0.033(4) 0.002(3) 0.004(3) 0.002(3) C8 0.056(5) 0.024(4) 0.028(4) -0.006(3) 0.013(4) -0.005(4) C9 0.038(4) 0.028(4) 0.027(4) 0.000(3) 0.010(3) 0.010(3) C10 0.030(4) 0.029(4) 0.022(3) 0.004(3) 0.010(3) -0.001(3) C11 0.040(4) 0.020(4) 0.022(3) 0.006(3) 0.012(3) 0.007(3) N12 0.035(3) 0.025(3) 0.020(3) 0.005(2) 0.002(2) 0.006(3) N13 0.039(3) 0.026(3) 0.025(3) 0.002(2) 0.009(3) 0.002(3) C14 0.050(5) 0.022(4) 0.027(4) 0.007(3) -0.001(3) 0.005(3) C15 0.064(6) 0.019(4) 0.036(4) 0.002(3) -0.009(4) -0.005(4) N16 0.068(5) 0.019(3) 0.035(4) -0.002(3) -0.009(3) 0.006(3) N17 0.051(4) 0.025(3) 0.032(3) 0.000(3) -0.010(3) 0.011(3) C18 0.055(5) 0.031(4) 0.036(4) -0.015(4) -0.014(4) 0.020(4) C19 0.055(5) 0.035(4) 0.031(4) -0.017(3) -0.010(4) 0.010(4) C20 0.062(6) 0.046(5) 0.043(5) -0.016(4) -0.014(4) 0.032(4) C21 0.078(7) 0.058(6) 0.044(5) -0.019(4) 0.002(5) 0.026(5) C22 0.057(5) 0.055(5) 0.028(4) -0.006(4) -0.005(4) 0.025(4) C23 0.066(6) 0.071(6) 0.028(4) -0.009(4) 0.006(4) 0.018(5) C24 0.054(5) 0.059(6) 0.029(4) 0.006(4) 0.007(4) 0.008(4) C25 0.046(5) 0.042(5) 0.034(4) 0.007(4) 0.004(4) 0.009(4) C26 0.037(4) 0.041(4) 0.033(4) -0.002(3) 0.007(3) 0.006(4) C27 0.055(5) 0.035(4) 0.028(4) -0.005(3) 0.005(4) 0.020(4) N28 0.050(4) 0.034(4) 0.032(3) -0.007(3) -0.004(3) 0.013(3) C29 0.048(5) 0.028(4) 0.040(4) 0.011(3) -0.007(4) 0.000(4) C30 0.050(5) 0.044(5) 0.062(6) 0.012(4) -0.003(4) -0.004(4) C31 0.039(5) 0.065(7) 0.091(8) 0.024(6) -0.012(5) -0.001(5) C32 0.050(6) 0.067(7) 0.103(9) 0.036(6) -0.034(6) -0.015(6) C33 0.076(7) 0.051(6) 0.073(7) 0.010(5) -0.030(6) -0.018(6) C34 0.061(6) 0.030(5) 0.071(6) 0.012(4) -0.005(5) -0.003(4) C35 0.057(5) 0.026(4) 0.035(4) 0.003(3) -0.015(4) -0.007(4) C36 0.064(6) 0.023(4) 0.066(6) 0.006(4) -0.027(5) 0.001(4) C37 0.096(10) 0.035(6) 0.098(9) 0.026(7) -0.036(7) -0.014(6) C38 0.109(10) 0.036(6) 0.070(8) 0.032(6) -0.044(7) -0.027(6) C39 0.105(8) 0.056(6) 0.044(5) 0.014(5) -0.014(5) -0.037(6) C40 0.088(7) 0.030(5) 0.046(5) 0.009(4) -0.008(5) -0.011(5) Cu41 0.0402(5) 0.0225(4) 0.0258(4) -0.0008(3) 0.0092(4) 0.0082(4) Cl42 0.0354(10) 0.0297(9) 0.0296(9) -0.0032(7) 0.0062(8) 0.0011(8) O43 0.067(4) 0.044(3) 0.033(3) -0.010(2) -0.001(3) 0.007(3) O44 0.067(4) 0.044(3) 0.060(4) -0.008(3) 0.042(3) -0.001(3) O45 0.052(3) 0.033(3) 0.042(3) 0.001(2) -0.004(3) -0.014(3) O46 0.044(3) 0.043(3) 0.064(4) 0.013(3) 0.011(3) 0.015(3) N47 0.043(4) 0.024(3) 0.023(3) 0.000(2) 0.002(3) 0.000(3) C48 0.044(5) 0.032(4) 0.030(4) 0.003(3) -0.008(3) 0.001(4) C49 0.074(6) 0.033(4) 0.042(5) -0.002(4) -0.018(4) 0.000(4) C50 0.097(8) 0.035(5) 0.049(5) -0.002(4) -0.028(5) -0.013(5) C51 0.062(6) 0.035(5) 0.073(6) 0.005(5) -0.035(5) -0.008(5) C52 0.058(6) 0.031(5) 0.065(6) 0.009(4) -0.021(5) -0.003(4) C53 0.046(5) 0.034(4) 0.040(4) 0.009(4) -0.003(4) -0.001(4) C54 0.036(4) 0.032(4) 0.037(4) 0.010(3) -0.002(3) 0.005(3) C55 0.036(4) 0.026(4) 0.028(4) 0.008(3) 0.006(3) 0.003(3) C56 0.038(4) 0.018(3) 0.019(3) 0.003(3) 0.001(3) 0.000(3) C57 0.039(4) 0.020(3) 0.019(3) 0.001(3) 0.002(3) 0.003(3) N58 0.036(3) 0.016(3) 0.023(3) 0.000(2) 0.000(2) 0.003(3) N59 0.035(3) 0.022(3) 0.020(3) 0.001(2) 0.005(3) -0.001(3) C60 0.042(4) 0.022(4) 0.024(4) 0.005(3) 0.013(3) 0.004(3) C61 0.035(4) 0.028(4) 0.029(4) -0.003(3) 0.013(3) -0.004(3) N62 0.052(4) 0.025(3) 0.027(3) 0.004(3) 0.018(3) 0.014(3) N63 0.043(4) 0.024(3) 0.031(3) 0.002(3) 0.009(3) 0.003(3) C64 0.056(5) 0.029(4) 0.031(4) 0.002(3) 0.021(4) 0.011(4) C65 0.050(5) 0.024(4) 0.035(4) 0.004(3) 0.021(4) 0.014(3) C66 0.070(6) 0.035(4) 0.043(5) 0.013(4) 0.030(4) 0.022(4) C67 0.065(6) 0.034(4) 0.054(5) 0.015(4) 0.031(5) 0.020(4) C68 0.044(5) 0.029(4) 0.036(4) 0.003(3) 0.019(4) 0.007(3) C69 0.044(5) 0.036(4) 0.036(4) 0.013(3) 0.011(4) 0.010(4) C70 0.042(5) 0.043(5) 0.031(4) 0.008(4) 0.008(4) 0.006(4) C71 0.050(5) 0.032(4) 0.032(4) -0.005(3) 0.018(4) -0.001(4) C72 0.036(4) 0.029(4) 0.028(4) -0.002(3) 0.007(3) 0.008(3) C73 0.030(4) 0.023(4) 0.027(4) 0.000(3) 0.006(3) 0.000(3) N74 0.034(3) 0.024(3) 0.025(3) 0.000(2) 0.009(3) 0.008(3) C75 0.034(4) 0.022(4) 0.030(4) 0.003(3) 0.009(3) -0.002(3) C76 0.043(5) 0.039(5) 0.049(5) -0.006(4) 0.016(4) 0.006(4) C77 0.037(5) 0.054(5) 0.055(5) -0.003(4) 0.021(4) 0.003(4) C78 0.042(5) 0.043(5) 0.043(5) -0.007(4) 0.014(4) -0.010(4) C79 0.051(5) 0.028(4) 0.033(4) -0.004(3) 0.020(4) -0.008(4) C80 0.037(4) 0.021(4) 0.032(4) 0.002(3) 0.015(3) -0.002(3) C81 0.048(5) 0.023(4) 0.029(4) -0.005(3) 0.016(3) -0.001(3) C82 0.072(6) 0.031(4) 0.041(5) 0.007(4) 0.031(4) 0.005(4) C83 0.075(6) 0.046(5) 0.039(5) -0.003(4) 0.028(4) 0.001(5) C84 0.063(6) 0.055(5) 0.031(4) 0.007(4) 0.023(4) -0.008(4) C85 0.043(5) 0.035(4) 0.034(4) 0.007(3) 0.009(4) -0.002(4) C86 0.036(4) 0.028(4) 0.028(4) 0.004(3) 0.010(3) 0.000(3) Cu87 0.0521(6) 0.0230(5) 0.0285(5) -0.0034(4) 0.0012(4) 0.0095(4) Cl88 0.0576(14) 0.0719(15) 0.0302(10) -0.0055(10) 0.0088(10) 0.0349(12) O89 0.064(4) 0.076(4) 0.025(3) -0.012(3) 0.001(3) 0.028(3) O90 0.065(4) 0.083(5) 0.073(4) 0.030(4) 0.008(3) 0.039(4) O91 0.052(4) 0.060(4) 0.095(5) -0.002(4) 0.015(4) 0.008(3) O92 0.048(8) 0.042(7) 0.041(7) -0.017(6) 0.016(6) -0.003(6) Cl94 0.056(5) 0.046(4) 0.066(4) -0.008(3) 0.013(5) -0.002(3) Cl95 0.083(4) 0.040(3) 0.111(4) -0.011(3) 0.048(3) -0.005(2) C96 0.058(12) 0.108(16) 0.010(7) -0.011(9) -0.004(7) 0.012(11) Cl97 0.063(3) 0.061(3) 0.062(3) 0.020(2) 0.020(2) -0.004(2) Cl98 0.072(4) 0.106(5) 0.043(3) -0.013(3) 0.016(3) 0.003(4) C99 0.033(5) 0.026(4) 0.114(9) -0.009(5) 0.030(6) -0.007(4) C100 0.039(7) 0.078(9) 0.050(7) -0.018(6) -0.001(6) 0.033(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C10 1.339(8) . ? N1 C2 1.368(8) . ? N1 Cu41 2.028(5) . ? C2 C3 1.390(10) . ? C2 C7 1.413(9) . ? C3 C4 1.380(10) . ? C4 C5 1.415(11) . ? C5 C6 1.340(11) . ? C6 C7 1.437(10) . ? C7 C8 1.405(10) . ? C8 C9 1.362(10) . ? C9 C10 1.405(9) . ? C10 C11 1.479(9) . ? C11 N12 1.289(8) . ? N12 N13 1.414(8) . ? N12 Cu41 2.043(6) . ? N13 C14 1.279(8) . ? C14 C29 1.473(10) . ? C14 C15 1.522(11) . ? C15 N16 1.292(11) . ? C15 C35 1.482(10) . ? N16 N17 1.406(8) . ? N17 C18 1.287(9) . ? N17 Cu87 2.096(6) . ? C18 C19 1.452(11) . ? C19 N28 1.342(9) . ? C19 C20 1.395(11) . ? C20 C21 1.377(12) . ? C21 C22 1.411(11) . ? C22 C23 1.406(11) . ? C22 C27 1.428(10) . ? C23 C24 1.348(11) . ? C24 C25 1.417(11) . ? C25 C26 1.362(10) . ? C26 C27 1.406(10) . ? C27 N28 1.375(9) . ? N28 Cu87 2.029(6) . ? C29 C30 1.394(12) . ? C29 C34 1.409(11) . ? C30 C31 1.391(12) . ? C31 C32 1.346(14) . ? C32 C33 1.380(15) . ? C33 C34 1.380(13) . ? C35 C40 1.388(13) . ? C35 C36 1.387(11) . ? C36 C37 1.381(14) . ? C37 C38 1.335(17) . ? C38 C39 1.399(16) . ? C39 C40 1.414(11) . ? Cu41 N74 2.015(5) . ? Cu41 N63 2.056(6) . ? Cl42 O44 1.425(5) . ? Cl42 O46 1.434(5) . ? Cl42 O43 1.432(5) . ? Cl42 O45 1.441(5) . ? N47 C56 1.319(8) . ? N47 C48 1.365(9) . ? N47 Cu87 2.026(6) . ? C48 C53 1.410(11) . ? C48 C49 1.419(10) . ? C49 C50 1.406(12) . ? C50 C51 1.374(14) . ? C51 C52 1.338(12) . ? C52 C53 1.438(11) . ? C53 C54 1.413(10) . ? C54 C55 1.348(9) . ? C55 C56 1.416(10) . ? C56 C57 1.448(9) . ? C57 N58 1.299(8) . ? N58 N59 1.418(7) . ? N58 Cu87 2.076(5) . ? N59 C60 1.288(8) . ? C60 C75 1.460(9) . ? C60 C61 1.509(9) . ? C61 N62 1.279(8) . ? C61 C81 1.488(9) . ? N62 N63 1.404(7) . ? N63 C64 1.293(8) . ? C64 C65 1.456(9) . ? C65 N74 1.334(8) . ? C65 C66 1.427(10) . ? C66 C67 1.369(10) . ? C67 C68 1.401(10) . ? C68 C69 1.399(9) . ? C68 C73 1.414(9) . ? C69 C70 1.355(10) . ? C70 C71 1.392(10) . ? C71 C72 1.362(9) . ? C72 C73 1.395(9) . ? C73 N74 1.377(8) . ? C75 C76 1.406(10) . ? C75 C80 1.409(9) . ? C76 C77 1.389(11) . ? C77 C78 1.371(11) . ? C78 C79 1.381(10) . ? C79 C80 1.355(10) . ? C81 C86 1.391(9) . ? C81 C82 1.391(10) . ? C82 C83 1.382(10) . ? C83 C84 1.373(11) . ? C84 C85 1.388(10) . ? C85 C86 1.385(9) . ? Cl88 O91 1.417(7) . ? Cl88 O92A 1.432(13) . ? Cl88 O90 1.432(6) . ? Cl88 O89 1.437(5) . ? Cl88 O92 1.485(11) . ? O92 O92A 0.709(13) . ? C93 Cl95 1.69(2) . ? C93 Cl94 1.78(3) . ? C93 C101 1.78(4) . ? C93 C102 1.82(3) . ? Cl94 C101 1.84(3) . ? Cl95 Cl95 1.950(11) 3_655 ? C96 Cl97 1.50(2) . ? C96 Cl98 1.98(2) . ? Cl97 C105 1.89(3) . ? Cl98 C103 0.69(2) . ? Cl98 C105 2.06(3) . ? C99 C100 1.076(16) . ? C99 C104 1.26(3) . ? C99 C105 1.71(3) . ? C100 C101 1.62(3) . ? C101 C102 1.71(3) . ? C101 C104 1.88(4) . ? C103 C105 1.93(4) . ? 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 C10 N1 C2 117.8(6) . . ? C10 N1 Cu41 111.5(4) . . ? C2 N1 Cu41 130.7(5) . . ? N1 C2 C3 118.5(6) . . ? N1 C2 C7 121.1(6) . . ? C3 C2 C7 120.4(6) . . ? C4 C3 C2 119.8(7) . . ? C3 C4 C5 120.1(7) . . ? C6 C5 C4 121.3(7) . . ? C5 C6 C7 119.8(7) . . ? C8 C7 C2 119.1(6) . . ? C8 C7 C6 122.3(7) . . ? C2 C7 C6 118.6(7) . . ? C9 C8 C7 119.7(6) . . ? C8 C9 C10 118.2(7) . . ? N1 C10 C9 124.2(6) . . ? N1 C10 C11 115.5(6) . . ? C9 C10 C11 120.3(6) . . ? N12 C11 C10 119.0(6) . . ? C11 N12 N13 109.1(5) . . ? C11 N12 Cu41 110.9(5) . . ? N13 N12 Cu41 139.0(4) . . ? C14 N13 N12 117.9(6) . . ? N13 C14 C29 116.7(7) . . ? N13 C14 C15 126.9(7) . . ? C29 C14 C15 116.2(6) . . ? N16 C15 C35 117.2(7) . . ? N16 C15 C14 126.0(7) . . ? C35 C15 C14 116.5(8) . . ? C15 N16 N17 117.7(6) . . ? C18 N17 N16 109.3(6) . . ? C18 N17 Cu87 109.6(5) . . ? N16 N17 Cu87 140.5(5) . . ? N17 C18 C19 119.9(7) . . ? N28 C19 C20 123.7(7) . . ? N28 C19 C18 116.3(7) . . ? C20 C19 C18 119.9(7) . . ? C21 C20 C19 118.9(7) . . ? C20 C21 C22 119.8(8) . . ? C23 C22 C21 123.3(8) . . ? C23 C22 C27 118.7(7) . . ? C21 C22 C27 118.0(7) . . ? C24 C23 C22 120.9(8) . . ? C23 C24 C25 120.2(7) . . ? C26 C25 C24 121.0(7) . . ? C25 C26 C27 119.6(7) . . ? N28 C27 C26 119.0(6) . . ? N28 C27 C22 121.4(6) . . ? C26 C27 C22 119.5(7) . . ? C19 N28 C27 118.1(6) . . ? C19 N28 Cu87 111.9(5) . . ? C27 N28 Cu87 130.0(5) . . ? C30 C29 C34 118.4(8) . . ? C30 C29 C14 120.2(7) . . ? C34 C29 C14 121.4(8) . . ? C31 C30 C29 120.3(9) . . ? C32 C31 C30 120.3(10) . . ? C31 C32 C33 121.1(9) . . ? C34 C33 C32 120.1(9) . . ? C33 C34 C29 119.9(9) . . ? C40 C35 C36 119.8(8) . . ? C40 C35 C15 120.4(8) . . ? C36 C35 C15 119.6(9) . . ? C37 C36 C35 119.6(11) . . ? C38 C37 C36 122.6(12) . . ? C37 C38 C39 118.8(10) . . ? C38 C39 C40 120.4(12) . . ? C35 C40 C39 118.6(10) . . ? N74 Cu41 N1 114.0(2) . . ? N74 Cu41 N12 130.0(2) . . ? N1 Cu41 N12 82.5(2) . . ? N74 Cu41 N63 82.9(2) . . ? N1 Cu41 N63 128.1(2) . . ? N12 Cu41 N63 125.0(2) . . ? O44 Cl42 O46 109.1(3) . . ? O44 Cl42 O43 109.4(4) . . ? O46 Cl42 O43 110.0(3) . . ? O44 Cl42 O45 108.4(3) . . ? O46 Cl42 O45 110.2(3) . . ? O43 Cl42 O45 109.6(3) . . ? C56 N47 C48 118.4(6) . . ? C56 N47 Cu87 111.8(5) . . ? C48 N47 Cu87 129.8(5) . . ? N47 C48 C53 121.3(7) . . ? N47 C48 C49 118.3(7) . . ? C53 C48 C49 120.4(7) . . ? C50 C49 C48 118.4(9) . . ? C51 C50 C49 120.5(8) . . ? C52 C51 C50 122.5(8) . . ? C51 C52 C53 120.2(9) . . ? C54 C53 C48 118.6(7) . . ? C54 C53 C52 123.3(8) . . ? C48 C53 C52 118.1(7) . . ? C55 C54 C53 119.1(7) . . ? C54 C55 C56 119.3(7) . . ? N47 C56 C55 123.2(6) . . ? N47 C56 C57 117.5(6) . . ? C55 C56 C57 119.3(6) . . ? N58 C57 C56 118.4(6) . . ? C57 N58 N59 109.8(5) . . ? C57 N58 Cu87 110.3(4) . . ? N59 N58 Cu87 139.5(4) . . ? C60 N59 N58 117.5(5) . . ? N59 C60 C75 118.0(6) . . ? N59 C60 C61 125.4(6) . . ? C75 C60 C61 116.2(6) . . ? N62 C61 C81 117.8(6) . . ? N62 C61 C60 125.0(6) . . ? C81 C61 C60 116.7(6) . . ? C61 N62 N63 116.7(5) . . ? C64 N63 N62 109.6(6) . . ? C64 N63 Cu41 109.4(5) . . ? N62 N63 Cu41 140.2(4) . . ? N63 C64 C65 119.7(6) . . ? N74 C65 C66 122.7(6) . . ? N74 C65 C64 116.6(6) . . ? C66 C65 C64 120.7(6) . . ? C67 C66 C65 118.3(7) . . ? C66 C67 C68 120.7(7) . . ? C69 C68 C67 123.2(7) . . ? C69 C68 C73 118.7(7) . . ? C67 C68 C73 118.0(6) . . ? C70 C69 C68 120.5(7) . . ? C69 C70 C71 120.8(7) . . ? C72 C71 C70 120.1(7) . . ? C71 C72 C73 120.4(6) . . ? N74 C73 C72 119.0(6) . . ? N74 C73 C68 121.6(6) . . ? C72 C73 C68 119.3(6) . . ? C65 N74 C73 118.7(5) . . ? C65 N74 Cu41 111.0(4) . . ? C73 N74 Cu41 130.3(4) . . ? C76 C75 C80 116.7(6) . . ? C76 C75 C60 122.3(6) . . ? C80 C75 C60 121.0(6) . . ? C77 C76 C75 122.3(7) . . ? C78 C77 C76 118.1(8) . . ? C77 C78 C79 121.2(7) . . ? C80 C79 C78 120.7(7) . . ? C79 C80 C75 121.0(7) . . ? C86 C81 C82 119.0(6) . . ? C86 C81 C61 120.6(6) . . ? C82 C81 C61 120.4(6) . . ? C83 C82 C81 120.5(7) . . ? C84 C83 C82 119.6(7) . . ? C83 C84 C85 121.2(7) . . ? C86 C85 C84 118.8(7) . . ? C85 C86 C81 120.9(7) . . ? N47 Cu87 N28 117.6(2) . . ? N47 Cu87 N58 81.4(2) . . ? N28 Cu87 N58 132.6(3) . . ? N47 Cu87 N17 131.0(3) . . ? N28 Cu87 N17 81.4(2) . . ? N58 Cu87 N17 120.1(2) . . ? O91 Cl88 O92A 122.3(6) . . ? O91 Cl88 O90 109.7(4) . . ? O92A Cl88 O90 100.0(6) . . ? O91 Cl88 O89 110.0(4) . . ? O92A Cl88 O89 104.6(5) . . ? O90 Cl88 O89 109.4(4) . . ? O91 Cl88 O92 95.2(6) . . ? O92A Cl88 O92 28.1(5) . . ? O90 Cl88 O92 119.9(6) . . ? O89 Cl88 O92 111.6(5) . . ? O92A O92 Cl88 71.8(15) . . ? O92 O92A Cl88 80.1(16) . . ? Cl95 C93 Cl94 114.5(14) . . ? Cl95 C93 C101 145.4(18) . . ? Cl94 C93 C101 62.4(13) . . ? Cl95 C93 C102 126.8(15) . . ? Cl94 C93 C102 13.5(7) . . ? C101 C93 C102 56.6(13) . . ? C93 Cl94 C101 58.8(12) . . ? C93 Cl95 Cl95 93.2(9) . 3_655 ? Cl97 C96 Cl98 108.4(9) . . ? C96 Cl97 C105 87.7(13) . . ? C103 Cl98 C96 85(3) . . ? C103 Cl98 C105 70(3) . . ? C96 Cl98 C105 71.8(11) . . ? C100 C99 C104 20.2(14) . . ? C100 C99 C105 105.6(15) . . ? C104 C99 C105 95.5(17) . . ? C99 C100 C101 116.8(15) . . ? C100 C101 C102 113(2) . . ? C100 C101 C93 150(2) . . ? C102 C101 C93 63.0(15) . . ? C100 C101 Cl94 110.2(17) . . ? C102 C101 Cl94 13.0(9) . . ? C93 C101 Cl94 58.7(13) . . ? C100 C101 C104 12.1(11) . . ? C102 C101 C104 110(2) . . ? C93 C101 C104 160(2) . . ? Cl94 C101 C104 110.1(18) . . ? C101 C102 C93 60.4(15) . . ? Cl98 C103 C105 91(3) . . ? C99 C104 C101 92.8(18) . . ? C99 C105 Cl97 129(2) . . ? C99 C105 C103 82.9(17) . . ? Cl97 C105 C103 91.7(16) . . ? C99 C105 Cl98 97.9(16) . . ? Cl97 C105 Cl98 91.9(14) . . ? C103 C105 Cl98 19.5(8) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.44 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.728 _refine_diff_density_min -0.792 _refine_diff_density_rms 0.100 data_Complex-2c _database_code_CSD 204789 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C34 H24 N6), (Zn Cl2 O8), 2.50(C2 H3 N), (C4 H10 O), (H2 O)' _chemical_formula_sum 'C43 H43.50 Cl2 N8.50 O10 Zn' _chemical_formula_weight 975.63 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' Zn Zn 0.2839 1.4301 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 18.8160(3) _cell_length_b 12.6210(2) _cell_length_c 20.3570(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.6890(7) _cell_angle_gamma 90.00 _cell_volume 4605.75(14) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7343 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 27.89 _exptl_crystal_description prisms _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2020 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8412 _exptl_absorpt_correction_T_max 0.9001 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10472 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.89 _reflns_number_total 10472 _reflns_number_gt 7343 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution SHELXS-86 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains three molecules of acetonitrile. One coordinated MeCN, N52-C53-C54, the methyl end of which is severely disordered, with full occupancy (the second possible site of methyl C54 is characterized by the following insert C54B C 0.0426(8) 0.1336(20) 0.0484(19) 0.25(2) Uani 0.50 1 d P . .); another uncoordinated and disordered MeCN with full occupancy, N56-C57-C58; and a third MeCN, N59-C60-C61, with half occupancy. ; _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^)+(0.0999P)^2^+8.7056P] 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 10472 _refine_ls_number_parameters 671 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.2020 _refine_ls_wR_factor_gt 0.1787 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.209 _refine_ls_shift/su_mean 0.059 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.20166(17) -0.0871(2) -0.05315(16) 0.0310(7) Uani 1 1 d . . . C2 C 0.1772(2) -0.1897(3) -0.0655(2) 0.0360(9) Uani 1 1 d . . . C3 C 0.2142(3) -0.2706(3) -0.0204(3) 0.0494(11) Uani 1 1 d . . . H3 H 0.2557 -0.2545 0.0185 0.059 Uiso 1 1 calc R . . C4 C 0.1895(3) -0.3735(4) -0.0334(4) 0.0684(17) Uani 1 1 d . . . H4 H 0.2145 -0.4284 -0.0031 0.082 Uiso 1 1 calc R . . C5 C 0.1285(4) -0.3987(4) -0.0902(4) 0.0748(19) Uani 1 1 d . . . H5 H 0.1121 -0.4702 -0.0977 0.090 Uiso 1 1 calc R . . C6 C 0.0927(3) -0.3236(4) -0.1342(3) 0.0649(15) Uani 1 1 d . . . H6 H 0.0515 -0.3420 -0.1728 0.078 Uiso 1 1 calc R . . C7 C 0.1162(3) -0.2161(4) -0.1235(3) 0.0471(11) Uani 1 1 d . . . C8 C 0.0826(3) -0.1346(4) -0.1693(3) 0.0554(13) Uani 1 1 d . . . H8 H 0.0415 -0.1499 -0.2088 0.066 Uiso 1 1 calc R . . C9 C 0.1088(3) -0.0340(4) -0.1573(2) 0.0479(11) Uani 1 1 d . . . H9 H 0.0865 0.0212 -0.1885 0.057 Uiso 1 1 calc R . . C10 C 0.1685(2) -0.0122(3) -0.0991(2) 0.0328(8) Uani 1 1 d . . . C11 C 0.1997(2) 0.0947(3) -0.08630(19) 0.0330(8) Uani 1 1 d . . . H11 H 0.1867 0.1471 -0.1214 0.040 Uiso 1 1 calc R . . N12 N 0.24480(17) 0.1160(2) -0.02714(15) 0.0279(6) Uani 1 1 d . . . N13 N 0.28030(16) 0.2150(2) -0.02083(16) 0.0290(6) Uani 1 1 d . . . C14 C 0.28570(19) 0.2700(3) 0.03310(18) 0.0277(7) Uani 1 1 d . . . C15 C 0.2570(2) 0.2421(3) 0.09277(19) 0.0300(8) Uani 1 1 d . . . N16 N 0.28310(18) 0.1645(2) 0.13387(16) 0.0328(7) Uani 1 1 d . . . N17 N 0.32636(18) 0.0934(2) 0.11191(15) 0.0316(7) Uani 1 1 d . . . C18 C 0.3973(2) 0.0920(3) 0.13337(19) 0.0330(8) Uani 1 1 d . . . H18 H 0.4248 0.1398 0.1679 0.040 Uiso 1 1 calc R . . C19 C 0.4347(2) 0.0127(3) 0.10208(19) 0.0313(8) Uani 1 1 d . . . C20 C 0.5122(2) -0.0002(3) 0.1268(2) 0.0366(9) Uani 1 1 d . . . H20 H 0.5413 0.0418 0.1640 0.044 Uiso 1 1 calc R . . C21 C 0.5455(2) -0.0740(3) 0.0968(2) 0.0398(9) Uani 1 1 d . . . H21 H 0.5977 -0.0859 0.1143 0.048 Uiso 1 1 calc R . . C22 C 0.5020(2) -0.1324(3) 0.0401(2) 0.0337(8) Uani 1 1 d . . . C23 C 0.5326(2) -0.2084(3) 0.0045(2) 0.0390(9) Uani 1 1 d . . . H23 H 0.5844 -0.2243 0.0211 0.047 Uiso 1 1 calc R . . C24 C 0.4892(2) -0.2584(3) -0.0525(2) 0.0413(10) Uani 1 1 d . . . H24 H 0.5106 -0.3089 -0.0755 0.050 Uiso 1 1 calc R . . C25 C 0.4119(2) -0.2356(3) -0.0778(2) 0.0376(9) Uani 1 1 d . . . H25 H 0.3820 -0.2692 -0.1186 0.045 Uiso 1 1 calc R . . C26 C 0.3798(2) -0.1653(3) -0.0439(2) 0.0322(8) Uani 1 1 d . . . H26 H 0.3278 -0.1516 -0.0608 0.039 Uiso 1 1 calc R . . C27 C 0.4239(2) -0.1130(3) 0.01612(19) 0.0295(8) Uani 1 1 d . . . N28 N 0.39113(17) -0.0419(2) 0.04879(16) 0.0287(6) Uani 1 1 d . . . C29 C 0.3266(2) 0.3713(3) 0.0392(2) 0.0322(8) Uani 1 1 d . . . C30 C 0.3310(2) 0.4228(3) -0.0202(2) 0.0403(9) Uani 1 1 d . . . H30 H 0.3061 0.3944 -0.0645 0.048 Uiso 1 1 calc R . . C31 C 0.3723(3) 0.5160(3) -0.0141(3) 0.0509(11) Uani 1 1 d . . . H31 H 0.3757 0.5509 -0.0543 0.061 Uiso 1 1 calc R . . C32 C 0.4080(3) 0.5578(4) 0.0498(3) 0.0539(12) Uani 1 1 d . . . H32 H 0.4354 0.6218 0.0534 0.065 Uiso 1 1 calc R . . C33 C 0.4042(3) 0.5074(4) 0.1082(3) 0.0525(12) Uani 1 1 d . . . H33 H 0.4299 0.5359 0.1522 0.063 Uiso 1 1 calc R . . C34 C 0.3629(2) 0.4149(3) 0.1034(2) 0.0427(10) Uani 1 1 d . . . H34 H 0.3594 0.3813 0.1440 0.051 Uiso 1 1 calc R . . C35 C 0.1994(2) 0.3117(3) 0.1065(2) 0.0373(9) Uani 1 1 d . . . C36 C 0.1578(2) 0.3781(3) 0.0541(2) 0.0419(10) Uani 1 1 d . . . H36 H 0.1674 0.3803 0.0110 0.050 Uiso 1 1 calc R . . C37 C 0.1018(3) 0.4412(4) 0.0655(3) 0.0566(13) Uani 1 1 d . . . H37 H 0.0734 0.4870 0.0302 0.068 Uiso 1 1 calc R . . C38 C 0.0877(3) 0.4372(4) 0.1280(4) 0.0691(17) Uani 1 1 d . . . H38 H 0.0499 0.4806 0.1359 0.083 Uiso 1 1 calc R . . C39 C 0.1283(4) 0.3702(5) 0.1788(3) 0.0730(17) Uani 1 1 d . . . H39 H 0.1176 0.3669 0.2215 0.088 Uiso 1 1 calc R . . C40 C 0.1846(3) 0.3073(4) 0.1689(3) 0.0574(13) Uani 1 1 d . . . H40 H 0.2127 0.2618 0.2046 0.069 Uiso 1 1 calc R . . Zn41 Zn 0.27412(2) -0.02379(3) 0.03850(2) 0.02962(14) Uani 1 1 d . . . Cl42 Cl 0.54031(8) 0.29564(10) 0.26530(6) 0.0560(3) Uani 1 1 d . . . O43 O 0.57487(19) 0.2752(3) 0.33674(15) 0.0525(8) Uani 1 1 d . . . O44 O 0.5580(3) 0.2134(4) 0.2259(2) 0.0904(15) Uani 1 1 d . . . O45 O 0.4605(2) 0.2971(5) 0.2511(2) 0.1058(18) Uani 1 1 d . . . O46 O 0.5608(5) 0.3969(4) 0.2497(3) 0.144(3) Uani 1 1 d . . . Cl47 Cl 0.07431(16) 0.2056(3) 0.35250(19) 0.0635(7) Uani 0.50 1 d P A 1 O48 O 0.0557(3) 0.2674(3) 0.2973(2) 0.0824(13) Uani 1 1 d . A 1 O49 O 0.0222(4) 0.1242(6) 0.3432(5) 0.0615(19) Uani 0.50 1 d P A 1 O50 O 0.1505(3) 0.1626(5) 0.3747(4) 0.0552(18) Uani 0.50 1 d P A 1 O51 O 0.0674(6) 0.2800(9) 0.4105(5) 0.097(3) Uani 0.50 1 d P A 1 Cl4A Cl 0.08706(15) 0.1650(2) 0.32384(13) 0.0453(6) Uani 0.50 1 d P B 2 O48A O 0.0177(7) 0.2436(9) 0.3646(6) 0.045(3) Uani 0.25 1 d P B 2 O49A O 0.0446(5) 0.0752(7) 0.2987(6) 0.089(3) Uani 0.50 1 d P B 2 O50A O 0.1587(7) 0.1679(11) 0.3178(8) 0.055(3) Uani 0.25 1 d P B 2 O51A O 0.0953(9) 0.1690(8) 0.4001(4) 0.127(5) Uani 0.50 1 d P B 2 N52 N 0.1595(3) 0.0140(4) 0.0603(3) 0.0681(13) Uani 1 1 d . . . C53 C 0.1062(6) 0.0622(10) 0.0642(8) 0.195(7) Uani 1 1 d . . . C54 C 0.0427(9) 0.1246(19) 0.0697(19) 0.27(2) Uani 0.50 1 d P . . H54A H 0.0552 0.1571 0.1155 0.402 Uiso 0.50 1 calc PR . . H54B H -0.0007 0.0783 0.0628 0.402 Uiso 0.50 1 calc PR . . H54C H 0.0313 0.1802 0.0344 0.402 Uiso 0.50 1 calc PR . . O55 O 0.28112(19) -0.1370(3) 0.11246(17) 0.0584(9) Uani 1 1 d . . . N56 N 0.2804(6) 0.5115(10) 0.3162(5) 0.071(3) Uani 0.50 1 d P . . N56A N 0.2573(8) 0.620(2) 0.3120(7) 0.147(8) Uani 0.50 1 d P . . C57 C 0.2745(4) 0.5696(8) 0.2651(4) 0.095(2) Uani 1 1 d . . . C58A C 0.2978(14) 0.565(3) 0.2093(11) 0.155(13) Uani 0.50 1 d P . . C58B C 0.2536(11) 0.6110(17) 0.1941(10) 0.103(7) Uani 0.50 1 d P . . N59 N 0.3063(6) 0.2802(11) 0.3181(5) 0.086(3) Uani 0.50 1 d P . . C60 C 0.3472(7) 0.2064(12) 0.3202(5) 0.067(3) Uani 0.50 1 d P . . C61 C 0.3998(9) 0.1245(11) 0.3235(7) 0.087(4) Uani 0.50 1 d P . . H61A H 0.4409 0.1519 0.3083 0.130 Uiso 0.50 1 calc PR . . H61B H 0.3754 0.0660 0.2933 0.130 Uiso 0.50 1 calc PR . . H61C H 0.4193 0.0988 0.3710 0.130 Uiso 0.50 1 calc PR . . C62 C 0.1051(13) 0.7431(12) 0.0956(12) 0.146(10) Uani 0.50 1 d P D 1 H62A H 0.1377 0.6831 0.0945 0.219 Uiso 0.50 1 calc PR D 1 H62B H 0.1113 0.7984 0.0640 0.219 Uiso 0.50 1 calc PR D 1 H62C H 0.0530 0.7192 0.0814 0.219 Uiso 0.50 1 calc PR D 1 C63 C 0.1268(10) 0.7906(15) 0.1735(12) 0.056(6) Uani 0.25 1 d P D 1 H63A H 0.0857 0.8367 0.1774 0.067 Uiso 0.25 1 calc PR D 1 H63B H 0.1316 0.7312 0.2063 0.067 Uiso 0.25 1 calc PR D 1 O64 O 0.1926(6) 0.8483(7) 0.1921(4) 0.089(3) Uani 0.50 1 d P D 1 C65 C 0.2107(13) 0.9032(17) 0.2574(9) 0.127(7) Uani 0.50 1 d P . . H65A H 0.1658 0.9432 0.2585 0.152 Uiso 0.50 1 calc PR D 1 H65B H 0.2201 0.8489 0.2941 0.152 Uiso 0.50 1 calc PR D 1 C66 C 0.2642(13) 0.9657(14) 0.2729(7) 0.110(6) Uani 0.50 1 d P D . H66A H 0.3104 0.9267 0.2771 0.165 Uiso 0.50 1 calc PR . . H66B H 0.2675 0.9999 0.3169 0.165 Uiso 0.50 1 calc PR . . H66C H 0.2569 1.0197 0.2369 0.165 Uiso 0.50 1 calc 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 N1 0.0341(16) 0.0233(15) 0.0370(17) 0.0006(12) 0.0128(14) 0.0001(12) C2 0.038(2) 0.0257(18) 0.053(2) -0.0068(17) 0.0258(19) -0.0051(15) C3 0.057(3) 0.025(2) 0.079(3) 0.007(2) 0.040(3) 0.0017(18) C4 0.080(4) 0.025(2) 0.122(5) 0.002(3) 0.063(4) -0.003(2) C5 0.088(4) 0.032(3) 0.124(5) -0.029(3) 0.061(4) -0.028(3) C6 0.070(3) 0.051(3) 0.087(4) -0.031(3) 0.042(3) -0.030(3) C7 0.051(3) 0.039(2) 0.058(3) -0.016(2) 0.027(2) -0.0197(19) C8 0.052(3) 0.065(3) 0.047(3) -0.017(2) 0.011(2) -0.023(2) C9 0.048(3) 0.050(3) 0.039(2) -0.0026(19) 0.003(2) -0.007(2) C10 0.035(2) 0.0258(18) 0.0348(19) 0.0015(15) 0.0063(16) -0.0025(14) C11 0.040(2) 0.0266(18) 0.0279(18) 0.0041(14) 0.0032(16) -0.0002(15) N12 0.0337(16) 0.0185(13) 0.0318(15) 0.0039(11) 0.0102(13) -0.0006(11) N13 0.0320(16) 0.0196(14) 0.0341(16) 0.0038(12) 0.0080(13) 0.0000(11) C14 0.0284(18) 0.0195(16) 0.0344(19) 0.0043(14) 0.0082(15) 0.0041(13) C15 0.0359(19) 0.0215(16) 0.0323(18) -0.0028(14) 0.0099(16) -0.0026(14) N16 0.0427(18) 0.0234(15) 0.0324(16) -0.0019(12) 0.0115(14) 0.0006(13) N17 0.0425(19) 0.0223(14) 0.0293(15) 0.0026(12) 0.0096(14) 0.0030(12) C18 0.041(2) 0.0235(17) 0.0313(18) 0.0021(14) 0.0063(17) -0.0059(15) C19 0.037(2) 0.0210(16) 0.0347(19) 0.0056(14) 0.0083(16) -0.0042(14) C20 0.035(2) 0.033(2) 0.039(2) 0.0060(16) 0.0064(17) -0.0058(15) C21 0.031(2) 0.037(2) 0.050(2) 0.0125(18) 0.0107(18) -0.0046(16) C22 0.035(2) 0.0216(17) 0.046(2) 0.0115(15) 0.0156(17) 0.0000(14) C23 0.035(2) 0.0298(19) 0.058(3) 0.0100(18) 0.024(2) 0.0024(15) C24 0.049(2) 0.0261(19) 0.059(3) 0.0028(18) 0.032(2) 0.0000(17) C25 0.046(2) 0.0241(18) 0.049(2) 0.0005(16) 0.0227(19) -0.0066(16) C26 0.0333(19) 0.0240(17) 0.043(2) 0.0020(15) 0.0172(17) -0.0016(14) C27 0.0319(18) 0.0196(16) 0.040(2) 0.0073(14) 0.0158(16) -0.0010(13) N28 0.0318(16) 0.0196(14) 0.0344(16) 0.0053(12) 0.0096(13) -0.0019(11) C29 0.0342(19) 0.0176(16) 0.045(2) 0.0026(15) 0.0133(17) 0.0023(14) C30 0.050(2) 0.0268(19) 0.045(2) 0.0045(17) 0.0164(19) -0.0041(17) C31 0.061(3) 0.032(2) 0.060(3) 0.009(2) 0.020(2) -0.012(2) C32 0.060(3) 0.029(2) 0.071(3) 0.001(2) 0.018(3) -0.015(2) C33 0.057(3) 0.034(2) 0.058(3) -0.001(2) 0.004(2) -0.015(2) C34 0.050(2) 0.029(2) 0.047(2) 0.0006(17) 0.012(2) -0.0046(17) C35 0.041(2) 0.0233(18) 0.051(2) -0.0031(16) 0.0190(19) -0.0016(15) C36 0.037(2) 0.0289(19) 0.061(3) -0.0011(18) 0.018(2) 0.0016(16) C37 0.045(3) 0.036(2) 0.095(4) 0.006(2) 0.031(3) 0.0098(19) C38 0.064(3) 0.040(3) 0.122(5) -0.008(3) 0.057(4) 0.004(2) C39 0.095(4) 0.059(3) 0.090(4) -0.001(3) 0.065(4) 0.013(3) C40 0.081(4) 0.045(3) 0.061(3) 0.006(2) 0.042(3) 0.012(2) Zn41 0.0343(3) 0.0216(2) 0.0301(2) 0.00259(16) 0.00565(18) 0.00206(16) Cl42 0.0809(9) 0.0492(6) 0.0362(5) -0.0139(5) 0.0155(6) -0.0112(6) O43 0.071(2) 0.0463(18) 0.0358(16) -0.0079(13) 0.0094(15) 0.0007(15) O44 0.091(3) 0.114(4) 0.073(3) -0.064(3) 0.034(2) -0.022(3) O45 0.063(3) 0.140(5) 0.088(3) -0.046(3) -0.016(2) 0.024(3) O46 0.254(8) 0.089(4) 0.079(3) 0.010(3) 0.034(4) -0.072(5) Cl47 0.0543(17) 0.0553(18) 0.072(2) 0.0112(16) 0.0057(15) -0.0184(14) O48 0.104(3) 0.055(2) 0.068(2) 0.0226(19) -0.004(2) -0.015(2) O49 0.054(4) 0.040(4) 0.089(6) 0.014(4) 0.020(4) -0.017(3) O50 0.029(3) 0.053(4) 0.071(5) -0.010(4) -0.004(3) -0.008(3) O51 0.111(8) 0.098(7) 0.086(6) -0.015(6) 0.035(6) -0.031(6) Cl4A 0.0536(14) 0.0350(12) 0.0394(12) -0.0027(9) 0.0024(11) -0.0049(10) O48A 0.033(6) 0.032(6) 0.049(7) 0.003(5) -0.017(6) -0.011(5) O49A 0.077(6) 0.050(5) 0.111(7) 0.016(5) -0.016(5) -0.025(4) O50A 0.039(7) 0.056(8) 0.082(10) -0.017(7) 0.035(7) -0.016(6) O51A 0.236(16) 0.083(7) 0.038(4) 0.035(5) 0.006(7) 0.047(8) N52 0.060(3) 0.086(3) 0.070(3) -0.023(3) 0.038(2) -0.025(2) C53 0.114(7) 0.201(11) 0.319(17) -0.188(12) 0.142(10) -0.099(8) C54 0.079(11) 0.24(2) 0.55(5) -0.30(3) 0.19(2) -0.098(14) O55 0.066(2) 0.056(2) 0.0480(18) 0.0153(15) 0.0096(16) -0.0267(17) N56 0.057(6) 0.100(8) 0.053(6) 0.006(6) 0.010(5) 0.008(5) N56A 0.097(10) 0.27(3) 0.080(9) -0.057(13) 0.040(8) -0.047(13) C57 0.063(4) 0.154(8) 0.071(4) -0.014(5) 0.025(3) -0.017(4) C58A 0.138(19) 0.27(3) 0.079(13) -0.104(18) 0.061(13) -0.09(2) C58B 0.114(15) 0.121(14) 0.074(10) 0.030(10) 0.026(10) -0.038(12) N59 0.059(6) 0.136(11) 0.056(6) -0.017(6) 0.009(5) -0.002(7) C60 0.059(7) 0.099(9) 0.044(6) -0.009(6) 0.016(5) -0.009(6) C61 0.116(11) 0.077(9) 0.084(9) 0.005(7) 0.056(8) 0.015(8) C62 0.21(2) 0.069(9) 0.25(2) -0.057(12) 0.20(2) -0.087(12) C63 0.050(11) 0.047(10) 0.100(16) -0.003(10) 0.065(12) -0.014(8) O64 0.145(8) 0.083(6) 0.080(5) -0.020(4) 0.095(6) -0.054(5) C65 0.19(2) 0.138(16) 0.105(13) -0.016(12) 0.119(15) -0.021(15) C66 0.175(19) 0.104(13) 0.054(8) -0.002(8) 0.040(10) 0.000(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C10 1.342(5) . ? N1 C2 1.372(5) . ? N1 Zn41 2.105(3) . ? C2 C3 1.408(6) . ? C2 C7 1.415(6) . ? C3 C4 1.377(6) . ? C4 C5 1.397(9) . ? C5 C6 1.337(9) . ? C6 C7 1.422(6) . ? C7 C8 1.404(7) . ? C8 C9 1.357(7) . ? C9 C10 1.390(6) . ? C10 C11 1.463(5) . ? C11 N12 1.273(5) . ? N12 N13 1.404(4) . ? N12 Zn41 2.181(3) . ? N13 C14 1.276(5) . ? C14 C29 1.478(5) . ? C14 C15 1.513(5) . ? C15 N16 1.285(5) . ? C15 C35 1.486(5) . ? N16 N17 1.374(4) . ? N17 C18 1.272(5) . ? N17 Zn41 2.120(3) . ? C18 C19 1.476(5) . ? C19 N28 1.335(5) . ? C19 C20 1.400(6) . ? C20 C21 1.365(6) . ? C21 C22 1.405(6) . ? C22 C23 1.424(6) . ? C22 C27 1.423(5) . ? C23 C24 1.356(6) . ? C24 C25 1.418(6) . ? C25 C26 1.371(5) . ? C26 C27 1.414(5) . ? C27 N28 1.369(5) . ? N28 Zn41 2.159(3) . ? C29 C34 1.390(6) . ? C29 C30 1.397(6) . ? C30 C31 1.394(6) . ? C31 C32 1.374(7) . ? C32 C33 1.369(7) . ? C33 C34 1.389(6) . ? C35 C40 1.382(6) . ? C35 C36 1.395(6) . ? C36 C37 1.396(6) . ? C37 C38 1.376(8) . ? C38 C39 1.375(9) . ? C39 C40 1.387(7) . ? Zn41 O55 2.051(3) . ? Zn41 N52 2.378(5) . ? Cl42 O46 1.399(5) . ? Cl42 O44 1.412(4) . ? Cl42 O43 1.425(3) . ? Cl42 O45 1.440(5) . ? Cl47 O48 1.324(5) . ? Cl47 O49 1.393(7) . ? Cl47 O50 1.469(7) . ? Cl47 O51 1.545(11) . ? Cl4A O49A 1.391(8) . ? Cl4A O50A 1.391(12) . ? Cl4A O51A 1.513(9) . ? Cl4A O48A 2.010(14) . ? O48A O51A 1.704(17) . ? N52 C53 1.198(11) . ? C53 C54 1.462(18) . ? N56 C57 1.249(13) . ? N56 N56A 1.44(2) . ? N56A C57 1.271(17) . ? C57 C58A 1.336(19) . ? C57 C58B 1.474(18) . ? C58A C58B 0.98(3) . ? N59 C60 1.200(17) . ? C60 C61 1.419(18) . ? C62 C63 1.63(3) . ? C63 O64 1.386(19) . ? O64 C65 1.445(19) . ? C65 C66 1.24(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 C10 N1 C2 118.6(3) . . ? C10 N1 Zn41 112.9(2) . . ? C2 N1 Zn41 127.7(3) . . ? N1 C2 C3 119.6(4) . . ? N1 C2 C7 121.2(4) . . ? C3 C2 C7 119.2(4) . . ? C4 C3 C2 119.2(5) . . ? C3 C4 C5 121.2(6) . . ? C6 C5 C4 120.8(5) . . ? C5 C6 C7 120.3(5) . . ? C8 C7 C2 118.0(4) . . ? C8 C7 C6 122.7(5) . . ? C2 C7 C6 119.3(5) . . ? C9 C8 C7 120.0(4) . . ? C8 C9 C10 119.7(4) . . ? N1 C10 C9 122.6(4) . . ? N1 C10 C11 116.7(3) . . ? C9 C10 C11 120.7(4) . . ? N12 C11 C10 118.6(3) . . ? C11 N12 N13 115.9(3) . . ? C11 N12 Zn41 112.3(2) . . ? N13 N12 Zn41 129.7(2) . . ? C14 N13 N12 118.3(3) . . ? N13 C14 C29 116.5(3) . . ? N13 C14 C15 127.6(3) . . ? C29 C14 C15 115.9(3) . . ? N16 C15 C35 119.0(3) . . ? N16 C15 C14 122.7(3) . . ? C35 C15 C14 118.2(3) . . ? C15 N16 N17 115.7(3) . . ? C18 N17 N16 124.1(3) . . ? C18 N17 Zn41 116.5(3) . . ? N16 N17 Zn41 119.4(2) . . ? N17 C18 C19 116.7(3) . . ? N28 C19 C20 123.2(4) . . ? N28 C19 C18 116.4(3) . . ? C20 C19 C18 120.4(3) . . ? C21 C20 C19 119.2(4) . . ? C20 C21 C22 119.6(4) . . ? C21 C22 C23 123.1(4) . . ? C21 C22 C27 118.3(4) . . ? C23 C22 C27 118.5(4) . . ? C24 C23 C22 121.1(4) . . ? C23 C24 C25 120.1(4) . . ? C26 C25 C24 120.6(4) . . ? C25 C26 C27 120.3(4) . . ? N28 C27 C26 119.6(3) . . ? N28 C27 C22 121.1(3) . . ? C26 C27 C22 119.2(3) . . ? C19 N28 C27 118.5(3) . . ? C19 N28 Zn41 112.4(2) . . ? C27 N28 Zn41 128.2(2) . . ? C34 C29 C30 119.2(4) . . ? C34 C29 C14 121.1(3) . . ? C30 C29 C14 119.7(3) . . ? C31 C30 C29 119.5(4) . . ? C32 C31 C30 120.5(4) . . ? C33 C32 C31 120.2(4) . . ? C32 C33 C34 120.3(4) . . ? C29 C34 C33 120.2(4) . . ? C40 C35 C36 120.3(4) . . ? C40 C35 C15 120.7(4) . . ? C36 C35 C15 118.9(4) . . ? C35 C36 C37 119.5(5) . . ? C38 C37 C36 120.0(5) . . ? C39 C38 C37 120.0(5) . . ? C40 C39 C38 121.1(5) . . ? C39 C40 C35 119.2(5) . . ? O55 Zn41 N1 105.44(12) . . ? O55 Zn41 N17 93.22(12) . . ? N1 Zn41 N17 157.83(12) . . ? O55 Zn41 N28 91.08(13) . . ? N1 Zn41 N28 114.36(12) . . ? N17 Zn41 N28 76.39(12) . . ? O55 Zn41 N12 164.05(14) . . ? N1 Zn41 N12 77.81(11) . . ? N17 Zn41 N12 81.03(11) . . ? N28 Zn41 N12 101.87(11) . . ? O55 Zn41 N52 82.10(17) . . ? N1 Zn41 N52 82.04(14) . . ? N17 Zn41 N52 88.93(14) . . ? N28 Zn41 N52 163.49(14) . . ? N12 Zn41 N52 82.93(16) . . ? O46 Cl42 O44 114.4(4) . . ? O46 Cl42 O43 109.0(3) . . ? O44 Cl42 O43 109.5(3) . . ? O46 Cl42 O45 106.6(4) . . ? O44 Cl42 O45 107.9(3) . . ? O43 Cl42 O45 109.3(3) . . ? O48 Cl47 O49 109.0(4) . . ? O48 Cl47 O50 117.4(5) . . ? O49 Cl47 O50 110.5(5) . . ? O48 Cl47 O51 103.2(5) . . ? O49 Cl47 O51 109.5(6) . . ? O50 Cl47 O51 106.9(6) . . ? O49A Cl4A O50A 116.9(8) . . ? O49A Cl4A O51A 105.8(7) . . ? O50A Cl4A O51A 106.8(9) . . ? O49A Cl4A O48A 100.4(6) . . ? O50A Cl4A O48A 142.4(6) . . ? O51A Cl4A O48A 55.7(6) . . ? O51A O48A Cl4A 47.2(5) . . ? Cl4A O51A O48A 77.1(6) . . ? C53 N52 Zn41 160.2(8) . . ? N52 C53 C54 177.9(10) . . ? C57 N56 N56A 56.0(8) . . ? C57 N56A N56 54.5(11) . . ? N56 C57 N56A 69.5(11) . . ? N56 C57 C58A 135.6(19) . . ? N56A C57 C58A 152(2) . . ? N56 C57 C58B 162.6(12) . . ? N56A C57 C58B 120.3(17) . . ? C58A C57 C58B 40.5(14) . . ? C58B C58A C57 77.3(19) . . ? C58A C58B C57 62.2(16) . . ? N59 C60 C61 176.0(14) . . ? O64 C63 C62 113.5(12) . . ? C63 O64 C65 116.4(12) . . ? C66 C65 O64 119.0(13) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.021 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.092