Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Goutam Kumar Patra' ; School of Chemistry Sackler Faculty of Exact Sciences Tel-Aviv University Ramat-Aviv 69978 Tel-Aviv Israel ; 'Israel Goldberg' ; School of Chemistry Sackler Faculty of Exact Sciences Tel-Aviv University Ramat-Aviv 69978 Tel-Aviv Israel ; #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof Israel Goldberg' _publ_contact_author_address ; School of Chemistry Tel Aviv University Ramat Aviv Campus Tel Aviv 69978 ISRAEL ; _publ_contact_author_phone '972 3 6409965' _publ_contact_author_fax '972 3 6409293' _publ_contact_author_email goldberg@post.tau.ac.il _publ_requested_journal 'Dalton Transactions' #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Coordination polymers of transition metal ions with polydentate imine ligands. Syntheses, materials characterization, and crystal structures of polymeric complexes of copper(I), silver(I) and zinc(II) ; data_Compound-1a _database_code_CSD 171379 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 N4' _chemical_formula_weight 238.29 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 5.9900(3) _cell_length_b 7.0300(3) _cell_length_c 7.8110(4) _cell_angle_alpha 100.9010(17) _cell_angle_beta 99.0060(18) _cell_angle_gamma 106.180(2) _cell_volume 302.46(3) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1266 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 27.44 _exptl_crystal_description 'plates' _exptl_crystal_colour 'white' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 126 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type ? _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 0.71070 _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 '1.3 degree 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 1266 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.44 _reflns_number_total 1266 _reflns_number_gt 983 _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^)+(0.0807P)^2^+0.0552P] 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 1266 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1468 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0925(3) 0.0439(2) -0.0399(2) 0.0232(4) Uani 1 1 d . . . H1A H -0.2309 0.0138 0.0167 0.028 Uiso 1 1 calc R . . H1B H -0.0231 0.1941 -0.0167 0.028 Uiso 1 1 calc R . . N2 N -0.1704(2) -0.04553(19) -0.23231(17) 0.0218(4) Uani 1 1 d . . . C3 C -0.3909(3) -0.1366(2) -0.2939(2) 0.0200(4) Uani 1 1 d . . . H3 H -0.4951 -0.1430 -0.2136 0.024 Uiso 1 1 calc R . . C4 C -0.4922(3) -0.2331(2) -0.4856(2) 0.0185(4) Uani 1 1 d . . . C5 C -0.7374(3) -0.3251(2) -0.5465(2) 0.0210(4) Uani 1 1 d . . . H5 H -0.8400 -0.3252 -0.4653 0.025 Uiso 1 1 calc R . . C6 C -0.8302(3) -0.4166(2) -0.7269(2) 0.0227(4) Uani 1 1 d . . . H6 H -0.9980 -0.4782 -0.7662 0.027 Uiso 1 1 calc R . . N7 N -0.6969(2) -0.4230(2) -0.84877(18) 0.0240(4) Uani 1 1 d . . . C8 C -0.4607(3) -0.3322(2) -0.7891(2) 0.0229(4) Uani 1 1 d . . . H8 H -0.3626 -0.3345 -0.8734 0.027 Uiso 1 1 calc R . . C9 C -0.3513(3) -0.2350(2) -0.6115(2) 0.0213(4) Uani 1 1 d . . . H9 H -0.1835 -0.1710 -0.5765 0.026 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 C1 0.0249(8) 0.0246(9) 0.0177(8) 0.0027(6) 0.0024(6) 0.0072(7) N2 0.0239(7) 0.0228(7) 0.0172(7) 0.0038(5) 0.0027(5) 0.0070(6) C3 0.0227(8) 0.0189(8) 0.0189(8) 0.0051(6) 0.0048(6) 0.0068(6) C4 0.0218(8) 0.0145(8) 0.0193(8) 0.0043(6) 0.0032(6) 0.0066(6) C5 0.0213(8) 0.0196(8) 0.0216(8) 0.0059(6) 0.0058(6) 0.0047(7) C6 0.0195(7) 0.0192(8) 0.0253(8) 0.0031(6) 0.0011(6) 0.0035(6) N7 0.0255(7) 0.0209(7) 0.0226(7) 0.0018(5) 0.0026(5) 0.0064(6) C8 0.0244(8) 0.0234(8) 0.0201(8) 0.0029(6) 0.0059(6) 0.0076(7) C9 0.0191(7) 0.0202(8) 0.0229(8) 0.0029(6) 0.0028(6) 0.0063(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 C1 N2 1.4597(19) . ? C1 C1 1.520(3) 2 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N2 C3 1.264(2) . ? C3 C4 1.474(2) . ? C3 H3 0.9500 . ? C4 C5 1.392(2) . ? C4 C9 1.393(2) . ? C5 C6 1.386(2) . ? C5 H5 0.9500 . ? C6 N7 1.337(2) . ? C6 H6 0.9500 . ? N7 C8 1.343(2) . ? C8 C9 1.388(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C1 109.68(15) . 2 ? N2 C1 H1A 109.7 . . ? C1 C1 H1A 109.7 2 . ? N2 C1 H1B 109.7 . . ? C1 C1 H1B 109.7 2 . ? H1A C1 H1B 108.2 . . ? C3 N2 C1 117.14(13) . . ? N2 C3 C4 122.45(14) . . ? N2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C5 C4 C9 117.73(14) . . ? C5 C4 C3 119.86(13) . . ? C9 C4 C3 122.42(14) . . ? C6 C5 C4 119.27(14) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N7 C6 C5 123.69(14) . . ? N7 C6 H6 118.2 . . ? C5 C6 H6 118.2 . . ? C6 N7 C8 116.60(13) . . ? N7 C8 C9 123.97(14) . . ? N7 C8 H8 118.0 . . ? C9 C8 H8 118.0 . . ? C8 C9 C4 118.72(14) . . ? C8 C9 H9 120.6 . . ? C4 C9 H9 120.6 . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.321 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.057 #====END=================================================== data_Compound-1b _database_code_CSD 171380 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 N4' _chemical_formula_weight 266.34 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 '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 7.3740(5) _cell_length_b 10.9250(9) _cell_length_c 8.9120(9) _cell_angle_alpha 90.00 _cell_angle_beta 110.490(3) _cell_angle_gamma 90.00 _cell_volume 672.54(10) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1419 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'needles' _exptl_crystal_colour 'white' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 284 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type ? _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 0.71070 _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 '1.4 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 1419 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1419 _reflns_number_gt 860 _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^)+(0.0757P)^2^+0.4131P] 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 1419 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1211 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1553 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.345 _refine_ls_shift/su_mean 0.013 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4578(4) 0.0478(3) 0.9362(3) 0.0283(7) Uani 1 1 d . . . H1A H 0.3458 0.0876 0.9530 0.034 Uiso 1 1 calc R . . H1B H 0.5561 0.1114 0.9435 0.034 Uiso 1 1 calc R . . N2 N 0.3954(3) -0.0096(2) 0.7772(2) 0.0242(6) Uani 1 1 d . . . C3 C 0.3072(3) 0.0572(2) 0.6553(3) 0.0217(6) Uani 1 1 d . . . C4 C 0.2442(3) -0.0031(2) 0.4946(3) 0.0214(6) Uani 1 1 d . . . C5 C 0.1278(4) 0.0570(3) 0.3563(3) 0.0258(6) Uani 1 1 d . . . H5 H 0.0860 0.1385 0.3623 0.031 Uiso 1 1 calc R . . C6 C 0.0733(4) -0.0030(3) 0.2097(3) 0.0293(7) Uani 1 1 d . . . H6 H -0.0067 0.0398 0.1175 0.035 Uiso 1 1 calc R . . N7 N 0.1265(3) -0.1171(2) 0.1902(3) 0.0292(6) Uani 1 1 d . . . C8 C 0.2383(4) -0.1742(3) 0.3234(3) 0.0261(6) Uani 1 1 d . . . H8 H 0.2781 -0.2556 0.3135 0.031 Uiso 1 1 calc R . . C9 C 0.3001(4) -0.1219(2) 0.4757(3) 0.0236(6) Uani 1 1 d . . . H9 H 0.3797 -0.1670 0.5658 0.028 Uiso 1 1 calc R . . C10 C 0.2625(4) 0.1907(3) 0.6601(3) 0.0287(7) Uani 1 1 d . . . H10A H 0.3011 0.2177 0.7718 0.043 Uiso 1 1 calc R . . H10B H 0.1232 0.2040 0.6065 0.043 Uiso 1 1 calc R . . H10C H 0.3339 0.2377 0.6053 0.043 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 C1 0.0395(16) 0.0235(15) 0.0182(14) -0.0030(12) 0.0055(11) -0.0003(12) N2 0.0319(13) 0.0223(13) 0.0159(11) -0.0025(9) 0.0054(9) -0.0025(9) C3 0.0230(14) 0.0231(14) 0.0180(13) 0.0004(11) 0.0058(10) -0.0021(10) C4 0.0217(14) 0.0234(14) 0.0183(13) -0.0010(11) 0.0060(9) -0.0012(10) C5 0.0297(15) 0.0241(15) 0.0227(14) 0.0014(11) 0.0079(11) -0.0004(11) C6 0.0347(16) 0.0310(16) 0.0185(14) 0.0037(12) 0.0046(11) 0.0063(12) N7 0.0325(13) 0.0315(15) 0.0206(12) 0.0000(10) 0.0055(9) 0.0007(10) C8 0.0311(15) 0.0249(15) 0.0218(14) -0.0024(12) 0.0085(11) 0.0005(11) C9 0.0268(14) 0.0227(15) 0.0195(13) 0.0012(11) 0.0059(10) 0.0015(10) C10 0.0366(16) 0.0221(15) 0.0242(14) 0.0011(12) 0.0068(11) 0.0019(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.469(3) . ? C1 C1 1.508(5) 3_657 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? N2 C3 1.281(3) . ? C3 C4 1.495(3) . ? C3 C10 1.499(4) . ? C4 C9 1.390(4) . ? C4 C5 1.395(4) . ? C5 C6 1.389(4) . ? C5 H5 0.9500 . ? C6 N7 1.336(4) . ? C6 H6 0.9500 . ? N7 C8 1.339(3) . ? C8 C9 1.394(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 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 N2 C1 C1 109.8(3) . 3_657 ? N2 C1 H1A 109.7 . . ? C1 C1 H1A 109.7 3_657 . ? N2 C1 H1B 109.7 . . ? C1 C1 H1B 109.7 3_657 . ? H1A C1 H1B 108.2 . . ? C3 N2 C1 118.0(2) . . ? N2 C3 C4 117.2(2) . . ? N2 C3 C10 125.5(2) . . ? C4 C3 C10 117.3(2) . . ? C9 C4 C5 116.7(2) . . ? C9 C4 C3 121.4(2) . . ? C5 C4 C3 121.9(2) . . ? C6 C5 C4 119.7(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? N7 C6 C5 124.1(3) . . ? N7 C6 H6 117.9 . . ? C5 C6 H6 117.9 . . ? C6 N7 C8 115.9(2) . . ? N7 C8 C9 124.2(3) . . ? N7 C8 H8 117.9 . . ? C9 C8 H8 117.9 . . ? C4 C9 C8 119.4(2) . . ? C4 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C3 C10 H10A 109.5 . . ? C3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C1 N2 C3 175.0(3) 3_657 . . . ? C1 N2 C3 C4 -179.7(2) . . . . ? C1 N2 C3 C10 0.5(4) . . . . ? N2 C3 C4 C9 -8.1(4) . . . . ? C10 C3 C4 C9 171.8(2) . . . . ? N2 C3 C4 C5 172.4(3) . . . . ? C10 C3 C4 C5 -7.8(4) . . . . ? C9 C4 C5 C6 0.3(4) . . . . ? C3 C4 C5 C6 179.9(2) . . . . ? C4 C5 C6 N7 -0.4(4) . . . . ? C5 C6 N7 C8 0.4(4) . . . . ? C6 N7 C8 C9 -0.2(4) . . . . ? C5 C4 C9 C8 -0.2(4) . . . . ? C3 C4 C9 C8 -179.8(2) . . . . ? N7 C8 C9 C4 0.2(4) . . . . ? N2 C1 C1 N2 180.0 . . 3_657 3_657 ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.260 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.064 #======END=========================================================== data_Compound-2a _database_code_CSD 171381 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 N6' _chemical_formula_weight 416.48 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 9.5290(5) _cell_length_b 11.2180(7) _cell_length_c 11.4780(6) _cell_angle_alpha 76.320(4) _cell_angle_beta 85.512(4) _cell_angle_gamma 67.003(3) _cell_volume 1097.27(11) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2536 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.55 _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type ? _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 0.71070 _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 '0.8 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 4562 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1131 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.55 _reflns_number_total 4562 _reflns_number_gt 2536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.6797P] 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 4562 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1521 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.1935 _refine_ls_wR_factor_gt 0.1535 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 -0.1523(3) 1.1362(3) 0.1149(2) 0.0213(6) Uani 1 1 d . . . N2 N -0.1041(3) 1.1929(3) 0.1939(2) 0.0229(6) Uani 1 1 d . . . N3 N -0.0649(3) 0.9014(3) 0.3670(2) 0.0226(6) Uani 1 1 d . . . N4 N 0.0469(3) 0.8403(3) 0.2877(2) 0.0214(6) Uani 1 1 d . . . C5 C -0.1858(4) 1.0380(3) 0.1738(3) 0.0208(7) Uani 1 1 d . . . C6 C -0.1791(3) 0.9996(3) 0.3089(3) 0.0206(7) Uani 1 1 d . . . C7 C -0.2390(3) 0.9645(3) 0.1078(3) 0.0216(7) Uani 1 1 d . . . C8 C -0.2068(4) 0.9681(3) -0.0135(3) 0.0258(8) Uani 1 1 d . . . H8 H -0.1488 1.0170 -0.0546 0.031 Uiso 1 1 calc R . . C9 C -0.2602(4) 0.8996(4) -0.0738(3) 0.0339(9) Uani 1 1 d . . . H9 H -0.2378 0.9011 -0.1561 0.041 Uiso 1 1 calc R . . C10 C -0.3459(4) 0.8292(4) -0.0140(4) 0.0366(9) Uani 1 1 d . . . H10 H -0.3832 0.7837 -0.0559 0.044 Uiso 1 1 calc R . . C11 C -0.3771(4) 0.8249(4) 0.1057(4) 0.0366(9) Uani 1 1 d . . . H11 H -0.4359 0.7766 0.1463 0.044 Uiso 1 1 calc R . . C12 C -0.3227(4) 0.8914(3) 0.1671(3) 0.0275(8) Uani 1 1 d . . . H12 H -0.3428 0.8869 0.2501 0.033 Uiso 1 1 calc R . . C13 C -0.3063(4) 1.0756(3) 0.3770(3) 0.0237(7) Uani 1 1 d . . . C14 C -0.4363(4) 1.1768(4) 0.3169(3) 0.0336(9) Uani 1 1 d . . . H14 H -0.4412 1.1980 0.2318 0.040 Uiso 1 1 calc R . . C15 C -0.5576(4) 1.2460(4) 0.3810(4) 0.0391(10) Uani 1 1 d . . . H15 H -0.6453 1.3144 0.3396 0.047 Uiso 1 1 calc R . . C16 C -0.5520(4) 1.2167(4) 0.5035(3) 0.0371(9) Uani 1 1 d . . . H16 H -0.6361 1.2638 0.5471 0.045 Uiso 1 1 calc R . . C17 C -0.4239(4) 1.1187(4) 0.5636(3) 0.0400(10) Uani 1 1 d . . . H17 H -0.4195 1.0993 0.6487 0.048 Uiso 1 1 calc R . . C18 C -0.3022(4) 1.0485(4) 0.5015(3) 0.0323(9) Uani 1 1 d . . . H18 H -0.2148 0.9809 0.5441 0.039 Uiso 1 1 calc R . . C19 C -0.1035(4) 1.3074(3) 0.1428(3) 0.0223(7) Uani 1 1 d . . . H19 H -0.1338 1.3447 0.0610 0.027 Uiso 1 1 calc R . . C20 C -0.0557(3) 1.3801(3) 0.2114(3) 0.0216(7) Uani 1 1 d . . . C21 C -0.0074(4) 1.3272(3) 0.3306(3) 0.0241(7) Uani 1 1 d . . . H21 H -0.0025 1.2411 0.3702 0.029 Uiso 1 1 calc R . . C22 C 0.0331(4) 1.4028(4) 0.3899(3) 0.0306(8) Uani 1 1 d . . . H22 H 0.0655 1.3659 0.4714 0.037 Uiso 1 1 calc R . . N23 N 0.0300(3) 1.5243(3) 0.3408(3) 0.0331(7) Uani 1 1 d . . . C24 C -0.0180(4) 1.5745(4) 0.2261(3) 0.0298(8) Uani 1 1 d . . . H24 H -0.0225 1.6612 0.1890 0.036 Uiso 1 1 calc R . . C25 C -0.0611(4) 1.5062(3) 0.1592(3) 0.0261(8) Uani 1 1 d . . . H25 H -0.0941 1.5457 0.0782 0.031 Uiso 1 1 calc R . . C26 C 0.1679(4) 0.7541(3) 0.3429(3) 0.0232(7) Uani 1 1 d . . . H26 H 0.1749 0.7403 0.4275 0.028 Uiso 1 1 calc R . . C27 C 0.2956(4) 0.6762(3) 0.2790(3) 0.0218(7) Uani 1 1 d . . . C28 C 0.2909(4) 0.6836(3) 0.1568(3) 0.0217(7) Uani 1 1 d . . . H28 H 0.2025 0.7427 0.1102 0.026 Uiso 1 1 calc R . . C29 C 0.4164(4) 0.6040(3) 0.1038(3) 0.0249(7) Uani 1 1 d . . . H29 H 0.4104 0.6106 0.0201 0.030 Uiso 1 1 calc R . . N30 N 0.5455(3) 0.5187(3) 0.1615(3) 0.0318(7) Uani 1 1 d . . . C31 C 0.5508(4) 0.5138(4) 0.2789(3) 0.0387(10) Uani 1 1 d . . . H31 H 0.6417 0.4549 0.3227 0.046 Uiso 1 1 calc R . . C32 C 0.4314(4) 0.5896(4) 0.3397(3) 0.0352(9) Uani 1 1 d . . . H32 H 0.4417 0.5827 0.4230 0.042 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 0.0247(14) 0.0205(14) 0.0196(14) -0.0081(11) -0.0015(11) -0.0070(12) N2 0.0288(15) 0.0230(15) 0.0200(14) -0.0090(11) 0.0003(12) -0.0109(12) N3 0.0239(14) 0.0203(14) 0.0226(14) -0.0090(11) 0.0046(11) -0.0058(12) N4 0.0207(14) 0.0196(14) 0.0204(14) -0.0068(11) 0.0019(11) -0.0028(11) C5 0.0199(16) 0.0186(16) 0.0218(17) -0.0073(13) 0.0021(13) -0.0040(13) C6 0.0179(16) 0.0185(17) 0.0253(17) -0.0044(13) -0.0006(13) -0.0073(13) C7 0.0177(16) 0.0194(17) 0.0235(17) -0.0046(13) -0.0040(13) -0.0021(13) C8 0.0248(17) 0.0223(18) 0.0264(18) -0.0091(14) -0.0023(14) -0.0024(14) C9 0.031(2) 0.034(2) 0.034(2) -0.0161(16) -0.0084(16) -0.0025(17) C10 0.028(2) 0.029(2) 0.054(3) -0.0199(18) -0.0123(18) -0.0023(17) C11 0.030(2) 0.030(2) 0.054(3) -0.0104(18) -0.0071(18) -0.0142(17) C12 0.0261(18) 0.0273(19) 0.0292(19) -0.0090(14) -0.0005(15) -0.0087(15) C13 0.0220(17) 0.0214(17) 0.0284(18) -0.0075(14) 0.0052(14) -0.0087(14) C14 0.033(2) 0.035(2) 0.0256(19) -0.0080(15) 0.0021(16) -0.0059(17) C15 0.027(2) 0.035(2) 0.041(2) -0.0122(17) 0.0041(17) 0.0053(17) C16 0.032(2) 0.040(2) 0.042(2) -0.0214(18) 0.0168(17) -0.0121(18) C17 0.037(2) 0.045(2) 0.030(2) -0.0171(17) 0.0061(17) -0.0040(19) C18 0.030(2) 0.035(2) 0.0263(19) -0.0094(15) 0.0022(15) -0.0054(16) C19 0.0270(17) 0.0213(17) 0.0186(16) -0.0047(13) 0.0005(13) -0.0092(14) C20 0.0177(16) 0.0199(17) 0.0275(18) -0.0089(13) 0.0014(13) -0.0056(13) C21 0.0253(18) 0.0228(18) 0.0236(18) -0.0063(13) 0.0004(14) -0.0080(14) C22 0.031(2) 0.037(2) 0.0230(18) -0.0071(15) -0.0031(15) -0.0111(17) N23 0.0334(17) 0.0378(19) 0.0346(17) -0.0145(14) 0.0047(14) -0.0176(15) C24 0.034(2) 0.0253(19) 0.034(2) -0.0099(15) 0.0038(16) -0.0150(16) C25 0.0284(18) 0.0283(19) 0.0229(18) -0.0076(14) 0.0017(14) -0.0112(15) C26 0.0259(18) 0.0221(18) 0.0180(16) -0.0048(13) -0.0025(13) -0.0047(14) C27 0.0197(16) 0.0217(17) 0.0189(16) -0.0028(13) -0.0004(13) -0.0035(13) C28 0.0225(17) 0.0184(17) 0.0229(17) -0.0036(13) -0.0026(13) -0.0065(14) C29 0.0259(18) 0.0272(19) 0.0214(17) -0.0075(13) -0.0015(14) -0.0086(15) N30 0.0303(17) 0.0309(17) 0.0291(17) -0.0085(13) 0.0005(13) -0.0055(14) C31 0.0254(19) 0.037(2) 0.032(2) -0.0032(16) -0.0043(16) 0.0088(17) C32 0.029(2) 0.038(2) 0.0221(18) -0.0013(15) -0.0050(15) 0.0026(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C5 1.290(4) . ? N1 N2 1.416(4) . ? N2 C19 1.281(4) . ? N3 C6 1.293(4) . ? N3 N4 1.417(3) . ? N4 C26 1.273(4) . ? C5 C7 1.480(5) . ? C5 C6 1.508(4) . ? C6 C13 1.472(4) . ? C7 C12 1.391(5) . ? C7 C8 1.396(5) . ? C8 C9 1.393(5) . ? C8 H8 0.9500 . ? C9 C10 1.386(6) . ? C9 H9 0.9500 . ? C10 C11 1.377(5) . ? C10 H10 0.9500 . ? C11 C12 1.390(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.389(5) . ? C13 C14 1.401(5) . ? C14 C15 1.384(5) . ? C14 H14 0.9500 . ? C15 C16 1.366(5) . ? C15 H15 0.9500 . ? C16 C17 1.378(5) . ? C16 H16 0.9500 . ? C17 C18 1.376(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.464(5) . ? C19 H19 0.9500 . ? C20 C25 1.382(5) . ? C20 C21 1.393(4) . ? C21 C22 1.379(5) . ? C21 H21 0.9500 . ? C22 N23 1.335(5) . ? C22 H22 0.9500 . ? N23 C24 1.342(4) . ? C24 C25 1.386(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.455(4) . ? C26 H26 0.9500 . ? C27 C28 1.389(4) . ? C27 C32 1.393(4) . ? C28 C29 1.380(4) . ? C28 H28 0.9500 . ? C29 N30 1.333(4) . ? C29 H29 0.9500 . ? N30 C31 1.339(5) . ? C31 C32 1.381(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? 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 C5 N1 N2 110.7(3) . . ? C19 N2 N1 112.2(3) . . ? C6 N3 N4 111.2(2) . . ? C26 N4 N3 112.1(3) . . ? N1 C5 C7 119.4(3) . . ? N1 C5 C6 121.6(3) . . ? C7 C5 C6 118.9(3) . . ? N3 C6 C13 118.8(3) . . ? N3 C6 C5 121.9(3) . . ? C13 C6 C5 119.2(3) . . ? C12 C7 C8 119.5(3) . . ? C12 C7 C5 119.6(3) . . ? C8 C7 C5 120.9(3) . . ? C9 C8 C7 119.6(4) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 120.2(4) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.0(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 120.4(3) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C18 C13 C14 118.2(3) . . ? C18 C13 C6 121.5(3) . . ? C14 C13 C6 120.3(3) . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 120.5(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 119.7(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 120.7(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C13 120.5(3) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? N2 C19 C20 119.5(3) . . ? N2 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C25 C20 C21 117.9(3) . . ? C25 C20 C19 120.2(3) . . ? C21 C20 C19 121.8(3) . . ? C22 C21 C20 118.4(3) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? N23 C22 C21 124.5(3) . . ? N23 C22 H22 117.7 . . ? C21 C22 H22 117.7 . . ? C22 N23 C24 116.4(3) . . ? N23 C24 C25 123.3(3) . . ? N23 C24 H24 118.4 . . ? C25 C24 H24 118.4 . . ? C20 C25 C24 119.4(3) . . ? C20 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? N4 C26 C27 121.3(3) . . ? N4 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C32 116.6(3) . . ? C28 C27 C26 123.0(3) . . ? C32 C27 C26 120.4(3) . . ? C29 C28 C27 119.2(3) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? N30 C29 C28 124.7(3) . . ? N30 C29 H29 117.7 . . ? C28 C29 H29 117.7 . . ? C29 N30 C31 116.0(3) . . ? N30 C31 C32 123.5(3) . . ? N30 C31 H31 118.2 . . ? C32 C31 H31 118.2 . . ? C31 C32 C27 120.0(3) . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 N2 C19 -165.1(3) . . . . ? C6 N3 N4 C26 172.1(3) . . . . ? N2 N1 C5 C7 180.0(3) . . . . ? N2 N1 C5 C6 2.8(4) . . . . ? N4 N3 C6 C13 -179.7(3) . . . . ? N4 N3 C6 C5 0.6(4) . . . . ? N1 C5 C6 N3 -100.3(4) . . . . ? C7 C5 C6 N3 82.5(4) . . . . ? N1 C5 C6 C13 80.0(4) . . . . ? C7 C5 C6 C13 -97.2(4) . . . . ? N1 C5 C7 C12 -158.3(3) . . . . ? C6 C5 C7 C12 19.0(4) . . . . ? N1 C5 C7 C8 21.4(5) . . . . ? C6 C5 C7 C8 -161.3(3) . . . . ? C12 C7 C8 C9 0.7(5) . . . . ? C5 C7 C8 C9 -179.1(3) . . . . ? C7 C8 C9 C10 0.5(5) . . . . ? C8 C9 C10 C11 -0.9(5) . . . . ? C9 C10 C11 C12 0.0(5) . . . . ? C10 C11 C12 C7 1.2(5) . . . . ? C8 C7 C12 C11 -1.5(5) . . . . ? C5 C7 C12 C11 178.2(3) . . . . ? N3 C6 C13 C18 3.5(5) . . . . ? C5 C6 C13 C18 -176.8(3) . . . . ? N3 C6 C13 C14 -175.7(3) . . . . ? C5 C6 C13 C14 4.0(5) . . . . ? C18 C13 C14 C15 -0.8(6) . . . . ? C6 C13 C14 C15 178.4(4) . . . . ? C13 C14 C15 C16 0.1(6) . . . . ? C14 C15 C16 C17 0.8(6) . . . . ? C15 C16 C17 C18 -1.0(7) . . . . ? C16 C17 C18 C13 0.2(6) . . . . ? C14 C13 C18 C17 0.7(6) . . . . ? C6 C13 C18 C17 -178.5(4) . . . . ? N1 N2 C19 C20 -179.6(3) . . . . ? N2 C19 C20 C25 -177.0(3) . . . . ? N2 C19 C20 C21 1.4(5) . . . . ? C25 C20 C21 C22 -0.4(5) . . . . ? C19 C20 C21 C22 -178.8(3) . . . . ? C20 C21 C22 N23 -0.2(5) . . . . ? C21 C22 N23 C24 0.7(5) . . . . ? C22 N23 C24 C25 -0.7(5) . . . . ? C21 C20 C25 C24 0.4(5) . . . . ? C19 C20 C25 C24 178.9(3) . . . . ? N23 C24 C25 C20 0.1(5) . . . . ? N3 N4 C26 C27 178.0(3) . . . . ? N4 C26 C27 C28 -4.5(5) . . . . ? N4 C26 C27 C32 175.1(4) . . . . ? C32 C27 C28 C29 1.7(5) . . . . ? C26 C27 C28 C29 -178.7(3) . . . . ? C27 C28 C29 N30 -0.3(5) . . . . ? C28 C29 N30 C31 -1.1(5) . . . . ? C29 N30 C31 C32 0.9(6) . . . . ? N30 C31 C32 C27 0.6(7) . . . . ? C28 C27 C32 C31 -1.9(6) . . . . ? C26 C27 C32 C31 178.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.328 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.067 #=====END============================================================== data_Compound-3 _database_code_CSD 171382 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H17 Cl Cu N5 O4' _chemical_formula_weight 442.34 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 9.89400(10) _cell_length_b 21.3850(4) _cell_length_c 9.2910(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.2350(7) _cell_angle_gamma 90.00 _cell_volume 1819.64(6) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3408 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.88 _exptl_crystal_description 'chunks' _exptl_crystal_colour 'yellow-red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6822 _exptl_absorpt_correction_T_max 0.7698 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71070 _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 4294 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.88 _reflns_number_total 4294 _reflns_number_gt 3408 _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^)+(0.0352P)^2^+1.1780P] 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 4294 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.033 _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 Cu1 Cu 0.05125(3) 0.109198(11) -0.11688(3) 0.01748(9) Uani 1 1 d . . . N2 N 0.13014(19) 0.02631(8) -0.16467(19) 0.0159(4) Uani 1 1 d . . . C3 C 0.2810(2) 0.02288(10) -0.0480(2) 0.0183(4) Uani 1 1 d . . . H3A H 0.3431 0.0542 -0.0722 0.022 Uiso 1 1 calc R . . H3B H 0.3223 -0.0191 -0.0499 0.022 Uiso 1 1 calc R . . C4 C 0.2783(2) 0.03574(9) 0.1118(2) 0.0184(4) Uani 1 1 d . . . H4A H 0.2220 0.0027 0.1389 0.022 Uiso 1 1 calc R . . H4B H 0.3791 0.0355 0.1909 0.022 Uiso 1 1 calc R . . N5 N 0.21036(19) 0.09706(8) 0.11084(19) 0.0154(4) Uani 1 1 d . . . C6 C 0.2728(2) 0.13255(10) 0.2268(2) 0.0166(4) Uani 1 1 d . . . H6 H 0.3610 0.1182 0.3049 0.020 Uiso 1 1 calc R . . C7 C 0.2177(2) 0.19472(10) 0.2488(2) 0.0166(4) Uani 1 1 d . . . C8 C 0.0753(2) 0.21503(10) 0.1682(3) 0.0215(5) Uani 1 1 d . . . H8 H 0.0084 0.1894 0.0900 0.026 Uiso 1 1 calc R . . C9 C 0.0316(2) 0.27271(10) 0.2025(3) 0.0207(5) Uani 1 1 d . . . H9 H -0.0661 0.2858 0.1466 0.025 Uiso 1 1 calc R . . N10 N 0.12192(19) 0.31112(8) 0.3122(2) 0.0169(4) Uani 1 1 d . . . C11 C 0.2597(2) 0.29145(10) 0.3886(2) 0.0184(4) Uani 1 1 d . . . H11 H 0.3251 0.3182 0.4651 0.022 Uiso 1 1 calc R . . C12 C 0.3112(2) 0.23430(10) 0.3617(2) 0.0179(4) Uani 1 1 d . . . H12 H 0.4092 0.2222 0.4196 0.021 Uiso 1 1 calc R . . C13 C 0.0850(2) -0.02144(10) -0.2528(2) 0.0175(4) Uani 1 1 d . . . H13 H 0.1518 -0.0549 -0.2391 0.021 Uiso 1 1 calc R . . C14 C -0.0620(2) -0.02869(10) -0.3734(2) 0.0177(4) Uani 1 1 d . . . C15 C -0.1688(2) 0.01769(10) -0.4172(2) 0.0206(5) Uani 1 1 d . . . H15 H -0.1484 0.0581 -0.3714 0.025 Uiso 1 1 calc R . . C16 C -0.3051(3) 0.00404(11) -0.5285(3) 0.0239(5) Uani 1 1 d . . . H16 H -0.3775 0.0358 -0.5556 0.029 Uiso 1 1 calc R . . N17 N -0.3409(2) -0.05152(9) -0.6004(2) 0.0258(4) Uani 1 1 d . . . C18 C -0.2360(3) -0.09489(11) -0.5612(3) 0.0233(5) Uani 1 1 d . . . H18 H -0.2580 -0.1341 -0.6129 0.028 Uiso 1 1 calc R . . C19 C -0.0970(2) -0.08622(11) -0.4498(3) 0.0209(5) Uani 1 1 d . . . H19 H -0.0267 -0.1188 -0.4257 0.025 Uiso 1 1 calc R . . N20 N -0.1491(2) 0.12258(8) -0.1357(2) 0.0217(4) Uani 1 1 d . . . C21 C -0.2655(2) 0.13505(10) -0.1495(3) 0.0212(5) Uani 1 1 d . . . C22 C -0.4136(3) 0.14959(12) -0.1653(3) 0.0318(6) Uani 1 1 d . . . H22A H -0.4787 0.1153 -0.2195 0.048 Uiso 1 1 calc R . . H22B H -0.4454 0.1883 -0.2252 0.048 Uiso 1 1 calc R . . H22C H -0.4169 0.1550 -0.0620 0.048 Uiso 1 1 calc R . . Cl23 Cl 0.65356(6) 0.16625(3) 0.27325(7) 0.02951(15) Uani 1 1 d . . . O24 O 0.6016(2) 0.10744(8) 0.1963(2) 0.0389(5) Uani 1 1 d . . . O25 O 0.5551(2) 0.21429(9) 0.1886(2) 0.0444(5) Uani 1 1 d . . . O26 O 0.6559(2) 0.16342(10) 0.4288(2) 0.0490(5) Uani 1 1 d . . . O27 O 0.7965(2) 0.17764(11) 0.2761(3) 0.0623(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01755(15) 0.01250(14) 0.02219(15) 0.00092(10) 0.00732(11) 0.00052(10) N2 0.0180(9) 0.0155(9) 0.0154(8) 0.0004(7) 0.0076(7) 0.0010(7) C3 0.0169(11) 0.0165(10) 0.0202(10) -0.0013(8) 0.0058(8) 0.0024(8) C4 0.0224(11) 0.0123(10) 0.0192(10) 0.0002(8) 0.0064(9) 0.0026(8) N5 0.0201(9) 0.0119(8) 0.0159(8) 0.0020(7) 0.0087(7) 0.0016(7) C6 0.0189(11) 0.0156(10) 0.0162(10) 0.0006(8) 0.0077(8) 0.0008(8) C7 0.0200(11) 0.0149(10) 0.0166(10) 0.0005(8) 0.0090(8) -0.0005(8) C8 0.0199(12) 0.0211(11) 0.0218(11) -0.0077(9) 0.0061(9) -0.0033(9) C9 0.0183(11) 0.0186(11) 0.0231(11) -0.0042(9) 0.0056(9) -0.0011(9) N10 0.0194(9) 0.0132(8) 0.0198(9) -0.0007(7) 0.0092(7) -0.0011(7) C11 0.0176(11) 0.0172(10) 0.0201(10) -0.0041(9) 0.0070(9) -0.0018(8) C12 0.0165(11) 0.0191(10) 0.0181(10) -0.0014(9) 0.0064(8) 0.0007(8) C13 0.0224(11) 0.0161(10) 0.0164(10) 0.0003(8) 0.0102(9) 0.0019(8) C14 0.0216(11) 0.0198(11) 0.0152(10) -0.0006(8) 0.0111(9) -0.0028(8) C15 0.0236(12) 0.0205(11) 0.0191(10) -0.0018(9) 0.0097(9) -0.0020(9) C16 0.0231(12) 0.0279(12) 0.0200(11) 0.0005(10) 0.0073(9) 0.0024(9) N17 0.0254(11) 0.0294(11) 0.0231(10) -0.0030(8) 0.0099(8) -0.0049(9) C18 0.0296(13) 0.0229(11) 0.0202(11) -0.0055(9) 0.0128(9) -0.0080(10) C19 0.0239(12) 0.0202(11) 0.0223(11) -0.0011(9) 0.0130(9) -0.0018(9) N20 0.0231(11) 0.0172(9) 0.0241(10) -0.0040(8) 0.0081(8) -0.0033(8) C21 0.0211(12) 0.0145(10) 0.0247(11) -0.0025(9) 0.0052(9) -0.0047(9) C22 0.0166(12) 0.0341(14) 0.0427(15) 0.0001(12) 0.0088(11) 0.0014(10) Cl23 0.0207(3) 0.0240(3) 0.0400(3) -0.0019(2) 0.0071(2) 0.0055(2) O24 0.0491(12) 0.0260(9) 0.0474(11) -0.0092(8) 0.0250(9) -0.0031(8) O25 0.0390(11) 0.0333(10) 0.0473(11) -0.0026(9) 0.0010(9) 0.0168(9) O26 0.0546(13) 0.0527(13) 0.0320(10) -0.0073(9) 0.0077(9) 0.0091(10) O27 0.0264(11) 0.0519(14) 0.109(2) 0.0137(13) 0.0260(12) -0.0014(10) _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 N20 1.945(2) . ? Cu1 N10 2.0434(17) 4_565 ? Cu1 N2 2.0519(17) . ? Cu1 N5 2.1217(17) . ? N2 C13 1.279(3) . ? N2 C3 1.478(3) . ? C3 C4 1.520(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N5 1.472(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N5 C6 1.271(3) . ? C6 C7 1.480(3) . ? C6 H6 0.9500 . ? C7 C12 1.392(3) . ? C7 C8 1.392(3) . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 N10 1.350(3) . ? C9 H9 0.9500 . ? N10 C11 1.344(3) . ? N10 Cu1 2.0435(17) 4_566 ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.470(3) . ? C13 H13 0.9500 . ? C14 C15 1.393(3) . ? C14 C19 1.397(3) . ? C15 C16 1.385(3) . ? C15 H15 0.9500 . ? C16 N17 1.343(3) . ? C16 H16 0.9500 . ? N17 C18 1.336(3) . ? C18 C19 1.385(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? N20 C21 1.141(3) . ? C21 C22 1.450(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? Cl23 O27 1.426(2) . ? Cl23 O25 1.4292(18) . ? Cl23 O26 1.438(2) . ? Cl23 O24 1.4418(18) . ? 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 N20 Cu1 N10 108.06(7) . 4_565 ? N20 Cu1 N2 124.48(7) . . ? N10 Cu1 N2 116.48(7) 4_565 . ? N20 Cu1 N5 117.00(7) . . ? N10 Cu1 N5 102.02(7) 4_565 . ? N2 Cu1 N5 84.87(6) . . ? C13 N2 C3 116.17(17) . . ? C13 N2 Cu1 139.36(15) . . ? C3 N2 Cu1 104.21(12) . . ? N2 C3 C4 108.72(17) . . ? N2 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? N2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? N5 C4 C3 109.38(16) . . ? N5 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? N5 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? C6 N5 C4 116.91(18) . . ? C6 N5 Cu1 135.37(15) . . ? C4 N5 Cu1 106.25(12) . . ? N5 C6 C7 124.55(19) . . ? N5 C6 H6 117.7 . . ? C7 C6 H6 117.7 . . ? C12 C7 C8 117.64(19) . . ? C12 C7 C6 118.42(19) . . ? C8 C7 C6 123.86(19) . . ? C9 C8 C7 119.7(2) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? N10 C9 C8 122.8(2) . . ? N10 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? C11 N10 C9 117.24(18) . . ? C11 N10 Cu1 119.53(14) . 4_566 ? C9 N10 Cu1 122.77(14) . 4_566 ? N10 C11 C12 123.38(19) . . ? N10 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C7 119.3(2) . . ? C11 C12 H12 120.4 . . ? C7 C12 H12 120.4 . . ? N2 C13 C14 125.3(2) . . ? N2 C13 H13 117.4 . . ? C14 C13 H13 117.4 . . ? C15 C14 C19 117.6(2) . . ? C15 C14 C13 124.73(19) . . ? C19 C14 C13 117.7(2) . . ? C16 C15 C14 119.0(2) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? N17 C16 C15 123.8(2) . . ? N17 C16 H16 118.1 . . ? C15 C16 H16 118.1 . . ? C18 N17 C16 116.5(2) . . ? N17 C18 C19 124.1(2) . . ? N17 C18 H18 118.0 . . ? C19 C18 H18 118.0 . . ? C18 C19 C14 118.9(2) . . ? C18 C19 H19 120.6 . . ? C14 C19 H19 120.6 . . ? C21 N20 Cu1 174.77(18) . . ? N20 C21 C22 178.7(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O27 Cl23 O25 110.61(13) . . ? O27 Cl23 O26 110.49(15) . . ? O25 Cl23 O26 109.39(12) . . ? O27 Cl23 O24 108.88(13) . . ? O25 Cl23 O24 108.26(12) . . ? O26 Cl23 O24 109.17(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N20 Cu1 N2 C13 29.6(2) . . . . ? N10 Cu1 N2 C13 -110.1(2) 4_565 . . . ? N5 Cu1 N2 C13 149.0(2) . . . . ? N20 Cu1 N2 C3 -144.02(12) . . . . ? N10 Cu1 N2 C3 76.30(14) 4_565 . . . ? N5 Cu1 N2 C3 -24.59(12) . . . . ? C13 N2 C3 C4 -125.77(19) . . . . ? Cu1 N2 C3 C4 49.59(17) . . . . ? N2 C3 C4 N5 -56.9(2) . . . . ? C3 C4 N5 C6 -135.82(19) . . . . ? C3 C4 N5 Cu1 32.49(19) . . . . ? N20 Cu1 N5 C6 -73.0(2) . . . . ? N10 Cu1 N5 C6 44.7(2) 4_565 . . . ? N2 Cu1 N5 C6 160.7(2) . . . . ? N20 Cu1 N5 C4 121.91(13) . . . . ? N10 Cu1 N5 C4 -120.43(13) 4_565 . . . ? N2 Cu1 N5 C4 -4.41(13) . . . . ? C4 N5 C6 C7 -177.71(19) . . . . ? Cu1 N5 C6 C7 18.4(3) . . . . ? N5 C6 C7 C12 -166.2(2) . . . . ? N5 C6 C7 C8 17.0(3) . . . . ? C12 C7 C8 C9 -0.2(3) . . . . ? C6 C7 C8 C9 176.6(2) . . . . ? C7 C8 C9 N10 0.1(3) . . . . ? C8 C9 N10 C11 0.4(3) . . . . ? C8 C9 N10 Cu1 -171.72(16) . . . 4_566 ? C9 N10 C11 C12 -0.9(3) . . . . ? Cu1 N10 C11 C12 171.53(16) 4_566 . . . ? N10 C11 C12 C7 0.8(3) . . . . ? C8 C7 C12 C11 -0.2(3) . . . . ? C6 C7 C12 C11 -177.17(19) . . . . ? C3 N2 C13 C14 178.31(19) . . . . ? Cu1 N2 C13 C14 5.2(3) . . . . ? N2 C13 C14 C15 5.5(3) . . . . ? N2 C13 C14 C19 -174.49(19) . . . . ? C19 C14 C15 C16 2.6(3) . . . . ? C13 C14 C15 C16 -177.5(2) . . . . ? C14 C15 C16 N17 -1.4(3) . . . . ? C15 C16 N17 C18 -0.9(3) . . . . ? C16 N17 C18 C19 1.9(3) . . . . ? N17 C18 C19 C14 -0.6(3) . . . . ? C15 C14 C19 C18 -1.7(3) . . . . ? C13 C14 C19 C18 178.35(19) . . . . ? N10 Cu1 N20 C21 -6(2) 4_565 . . . ? N2 Cu1 N20 C21 -149(2) . . . . ? N5 Cu1 N20 C21 108(2) . . . . ? Cu1 N20 C21 C22 -165(10) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.413 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.077 #=======END========================================================= data_Compound-4 _database_code_CSD 171383 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 Ag Cl N4 O6' _chemical_formula_weight 509.70 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 'orthorhombic' _symmetry_space_group_name_H-M 'Pnn2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.5400(5) _cell_length_b 11.5400(7) _cell_length_c 14.9430(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1989.98(16) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1844 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.86 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8419 _exptl_absorpt_correction_T_max 0.8905 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71070 _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 2438 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.86 _reflns_number_total 2438 _reflns_number_gt 1844 _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^)+(0.0469P)^2^+3.6623P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(8) _refine_ls_number_reflns 2438 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.191 _refine_ls_shift/su_mean 0.006 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 0.9272(5) -0.3104(6) -0.0738(5) 0.0282(15) Uani 1 1 d . . . C2 C 0.8763(7) -0.2826(8) 0.0047(5) 0.0275(18) Uani 1 1 d . . . H2 H 0.8653 -0.3415 0.0484 0.033 Uiso 1 1 calc R . . C3 C 0.8397(7) -0.1709(7) 0.0236(6) 0.0240(17) Uani 1 1 d . . . H3 H 0.8057 -0.1542 0.0801 0.029 Uiso 1 1 calc R . . C4 C 0.8522(6) -0.0845(7) -0.0383(5) 0.0203(15) Uani 1 1 d . . . C5 C 0.8982(6) -0.1139(7) -0.1219(6) 0.0245(17) Uani 1 1 d . . . H5 H 0.9044 -0.0577 -0.1681 0.029 Uiso 1 1 calc R . . C6 C 0.9347(6) -0.2274(7) -0.1358(5) 0.0278(17) Uani 1 1 d . . . H6 H 0.9667 -0.2469 -0.1924 0.033 Uiso 1 1 calc R . . C7 C 0.8168(6) 0.0377(7) -0.0148(5) 0.0216(15) Uani 1 1 d . . . C8 C 0.7529(7) 0.1066(7) -0.0837(6) 0.0337(19) Uani 1 1 d . . . H8A H 0.6736 0.1210 -0.0631 0.051 Uiso 1 1 calc R . . H8B H 0.7508 0.0633 -0.1401 0.051 Uiso 1 1 calc R . . H8C H 0.7925 0.1808 -0.0931 0.051 Uiso 1 1 calc R . . N9 N 0.8446(5) 0.0707(5) 0.0634(4) 0.0199(13) Uani 1 1 d . . . C10 C 0.8126(6) 0.1856(7) 0.0967(6) 0.0221(17) Uani 1 1 d . . . H10A H 0.7340 0.2056 0.0751 0.027 Uiso 1 1 calc R . . H10B H 0.8674 0.2439 0.0728 0.027 Uiso 1 1 calc R . . C11 C 0.8144(6) 0.1895(7) 0.1978(6) 0.0218(16) Uani 1 1 d . . . H11A H 0.7959 0.2688 0.2187 0.026 Uiso 1 1 calc R . . H11B H 0.7552 0.1359 0.2221 0.026 Uiso 1 1 calc R . . N12 N 0.9295(5) 0.1556(5) 0.2300(4) 0.0193(12) Uani 1 1 d . . . C13 C 0.9624(6) 0.1824(7) 0.3085(5) 0.0205(15) Uani 1 1 d . . . C14 C 0.8941(6) 0.2481(8) 0.3768(6) 0.0334(19) Uani 1 1 d . . . H14A H 0.8903 0.3299 0.3597 0.050 Uiso 1 1 calc R . . H14B H 0.9316 0.2410 0.4354 0.050 Uiso 1 1 calc R . . H14C H 0.8154 0.2163 0.3801 0.050 Uiso 1 1 calc R . . C15 C 1.0844(6) 0.1482(6) 0.3328(5) 0.0194(14) Uani 1 1 d . . . C16 C 1.1714(6) 0.1611(7) 0.2700(6) 0.0226(16) Uani 1 1 d . . . H16 H 1.1550 0.1962 0.2138 0.027 Uiso 1 1 calc R . . C17 C 1.2824(6) 0.1229(7) 0.2890(5) 0.0241(17) Uani 1 1 d . . . H17 H 1.3410 0.1325 0.2450 0.029 Uiso 1 1 calc R . . N18 N 1.3104(5) 0.0727(6) 0.3672(5) 0.0261(14) Uani 1 1 d . . . C19 C 1.2278(7) 0.0644(7) 0.4289(6) 0.0290(18) Uani 1 1 d . . . H19 H 1.2471 0.0317 0.4853 0.035 Uiso 1 1 calc R . . C20 C 1.1136(7) 0.1017(7) 0.4147(6) 0.0250(17) Uani 1 1 d . . . H20 H 1.0572 0.0949 0.4607 0.030 Uiso 1 1 calc R . . Ag21 Ag 1.0000 0.0000 0.1460 0.01797(16) Uani 1 2 d S . . Ag22 Ag 1.5000 0.0000 0.39600(8) 0.0314(2) Uani 1 2 d S . . Cl23 Cl 1.0000 0.5000 0.1769(2) 0.0331(6) Uani 1 2 d S . . O24 O 0.9131(7) 0.4504(7) 0.1197(7) 0.071(3) Uani 1 1 d . . . O25 O 1.0513(9) 0.4134(9) 0.2293(7) 0.086(3) Uani 1 1 d . . . Cl26 Cl 0.5000 0.0000 0.1157(2) 0.0331(6) Uani 1 2 d S . . O27 O 0.5488(7) 0.0870(7) 0.1737(6) 0.068(3) Uani 1 1 d . . . O28 O 0.5868(8) -0.0518(10) 0.0643(7) 0.086(3) Uani 1 1 d . . . O29 O -0.0087(12) 0.1636(10) 0.6293(8) 0.126(5) Uani 1 1 d . . . O30 O 0.1624(9) -0.0090(11) 0.6659(7) 0.114(5) 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 0.025(3) 0.017(3) 0.042(4) -0.004(3) -0.002(3) 0.002(3) C2 0.030(4) 0.026(5) 0.026(4) -0.003(3) -0.007(3) 0.002(3) C3 0.025(4) 0.020(4) 0.027(4) -0.001(3) 0.000(4) -0.002(3) C4 0.016(3) 0.019(4) 0.026(4) -0.002(3) -0.003(3) -0.004(3) C5 0.023(4) 0.023(4) 0.027(4) 0.001(3) -0.003(3) -0.008(3) C6 0.024(4) 0.031(4) 0.028(4) -0.007(4) 0.002(3) -0.004(3) C7 0.021(3) 0.022(4) 0.022(3) 0.001(3) -0.002(3) -0.003(3) C8 0.039(4) 0.021(4) 0.041(5) 0.003(4) -0.010(4) 0.012(3) N9 0.014(3) 0.016(3) 0.030(3) 0.000(3) -0.002(2) 0.004(2) C10 0.019(3) 0.015(4) 0.032(5) -0.004(3) -0.006(3) 0.008(3) C11 0.020(4) 0.020(4) 0.026(4) -0.004(3) -0.002(3) 0.006(3) N12 0.019(3) 0.009(3) 0.030(3) -0.002(2) 0.001(3) 0.003(2) C13 0.021(3) 0.017(4) 0.023(3) -0.001(3) -0.002(3) -0.001(3) C14 0.020(3) 0.044(5) 0.037(5) -0.009(4) -0.001(4) 0.009(3) C15 0.020(3) 0.012(3) 0.025(4) -0.005(3) -0.002(3) 0.001(3) C16 0.022(4) 0.024(4) 0.022(4) -0.005(3) -0.003(3) 0.003(3) C17 0.017(3) 0.023(4) 0.033(5) -0.009(3) 0.001(3) -0.001(3) N18 0.018(3) 0.019(3) 0.041(4) -0.001(3) -0.005(3) -0.003(2) C19 0.032(4) 0.020(4) 0.034(4) 0.006(3) -0.010(4) -0.006(3) C20 0.026(4) 0.024(4) 0.025(4) 0.002(3) 0.003(3) -0.006(3) Ag21 0.0163(3) 0.0160(3) 0.0216(3) 0.000 0.000 0.0050(3) Ag22 0.0157(3) 0.0153(4) 0.0634(6) 0.000 0.000 0.0002(3) Cl23 0.0374(15) 0.0204(13) 0.0415(13) 0.000 0.000 0.0007(13) O24 0.057(4) 0.046(5) 0.109(8) -0.022(5) -0.016(5) -0.015(4) O25 0.102(6) 0.074(7) 0.082(6) 0.044(5) -0.024(6) 0.012(6) Cl26 0.0192(11) 0.0382(17) 0.0419(14) 0.000 0.000 -0.0019(12) O27 0.047(4) 0.061(5) 0.097(7) -0.019(5) -0.015(4) -0.018(4) O28 0.069(6) 0.103(7) 0.087(7) -0.025(6) 0.038(5) 0.015(6) O29 0.242(16) 0.060(6) 0.076(8) -0.022(6) 0.010(8) 0.017(7) O30 0.058(5) 0.210(15) 0.075(8) -0.008(8) 0.016(5) 0.009(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 N1 C6 1.335(11) . ? N1 C2 1.351(10) . ? N1 Ag22 2.386(6) 3_744 ? C2 C3 1.386(12) . ? C2 H2 0.9500 . ? C3 C4 1.367(11) . ? C3 H3 0.9500 . ? C4 C5 1.399(11) . ? C4 C7 1.510(11) . ? C5 C6 1.392(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N9 1.270(9) . ? C7 C8 1.496(11) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N9 C10 1.463(9) . ? N9 Ag21 2.325(6) . ? C10 C11 1.512(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N12 1.466(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N12 C13 1.272(9) . ? N12 Ag21 2.337(6) . ? C13 C14 1.495(11) . ? C13 C15 1.507(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.378(11) . ? C15 C16 1.382(11) . ? C16 C17 1.384(10) . ? C16 H16 0.9500 . ? C17 N18 1.344(10) . ? C17 H17 0.9500 . ? N18 C19 1.330(10) . ? N18 Ag22 2.382(6) . ? C19 C20 1.403(11) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? Ag21 N9 2.325(6) 2_755 ? Ag21 N12 2.337(6) 2_755 ? Ag22 N18 2.382(6) 2_855 ? Ag22 N1 2.386(6) 4_545 ? Ag22 N1 2.386(6) 3_755 ? Cl23 O25 1.401(8) 2_765 ? Cl23 O25 1.401(8) . ? Cl23 O24 1.437(8) 2_765 ? Cl23 O24 1.437(8) . ? Cl26 O28 1.397(8) . ? Cl26 O28 1.397(8) 2_655 ? Cl26 O27 1.441(8) . ? Cl26 O27 1.441(8) 2_655 ? 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 C6 N1 C2 117.4(7) . . ? C6 N1 Ag22 120.3(5) . 3_744 ? C2 N1 Ag22 122.3(5) . 3_744 ? N1 C2 C3 122.0(8) . . ? N1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C4 C3 C2 120.5(8) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 117.9(7) . . ? C3 C4 C7 119.7(7) . . ? C5 C4 C7 122.5(7) . . ? C6 C5 C4 118.4(8) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? N1 C6 C5 123.6(8) . . ? N1 C6 H6 118.2 . . ? C5 C6 H6 118.2 . . ? N9 C7 C8 126.7(7) . . ? N9 C7 C4 115.2(6) . . ? C8 C7 C4 118.0(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 N9 C10 121.4(6) . . ? C7 N9 Ag21 125.3(5) . . ? C10 N9 Ag21 109.4(4) . . ? N9 C10 C11 111.3(7) . . ? N9 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N9 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N12 C11 C10 109.4(7) . . ? N12 C11 H11A 109.8 . . ? C10 C11 H11A 109.8 . . ? N12 C11 H11B 109.8 . . ? C10 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? C13 N12 C11 120.5(6) . . ? C13 N12 Ag21 125.4(5) . . ? C11 N12 Ag21 110.1(4) . . ? N12 C13 C14 126.5(7) . . ? N12 C13 C15 115.9(6) . . ? C14 C13 C15 117.5(6) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 117.9(7) . . ? C20 C15 C13 122.9(7) . . ? C16 C15 C13 119.1(7) . . ? C15 C16 C17 119.9(8) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? N18 C17 C16 122.6(7) . . ? N18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C19 N18 C17 117.5(6) . . ? C19 N18 Ag22 120.5(5) . . ? C17 N18 Ag22 122.0(5) . . ? N18 C19 C20 123.2(7) . . ? N18 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C15 C20 C19 118.9(7) . . ? C15 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? N9 Ag21 N9 115.9(3) . 2_755 ? N9 Ag21 N12 145.4(2) . 2_755 ? N9 Ag21 N12 75.3(2) 2_755 2_755 ? N9 Ag21 N12 75.3(2) . . ? N9 Ag21 N12 145.4(2) 2_755 . ? N12 Ag21 N12 115.0(3) 2_755 . ? N18 Ag22 N18 159.2(4) 2_855 . ? N18 Ag22 N1 92.0(2) 2_855 4_545 ? N18 Ag22 N1 91.9(2) . 4_545 ? N18 Ag22 N1 91.9(2) 2_855 3_755 ? N18 Ag22 N1 92.0(2) . 3_755 ? N1 Ag22 N1 158.2(4) 4_545 3_755 ? O25 Cl23 O25 112.1(10) 2_765 . ? O25 Cl23 O24 110.1(6) 2_765 2_765 ? O25 Cl23 O24 108.8(6) . 2_765 ? O25 Cl23 O24 108.8(6) 2_765 . ? O25 Cl23 O24 110.1(6) . . ? O24 Cl23 O24 106.9(8) 2_765 . ? O28 Cl26 O28 113.3(10) . 2_655 ? O28 Cl26 O27 110.4(6) . . ? O28 Cl26 O27 108.2(6) 2_655 . ? O28 Cl26 O27 108.2(6) . 2_655 ? O28 Cl26 O27 110.4(6) 2_655 2_655 ? O27 Cl26 O27 106.1(8) . 2_655 ? 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 C6 N1 C2 C3 -4.1(11) . . . . ? Ag22 N1 C2 C3 176.5(6) 3_744 . . . ? N1 C2 C3 C4 1.3(12) . . . . ? C2 C3 C4 C5 2.6(11) . . . . ? C2 C3 C4 C7 -177.2(7) . . . . ? C3 C4 C5 C6 -3.5(10) . . . . ? C7 C4 C5 C6 176.3(6) . . . . ? C2 N1 C6 C5 3.1(11) . . . . ? Ag22 N1 C6 C5 -177.5(6) 3_744 . . . ? C4 C5 C6 N1 0.7(11) . . . . ? C3 C4 C7 N9 41.6(10) . . . . ? C5 C4 C7 N9 -138.2(7) . . . . ? C3 C4 C7 C8 -137.9(7) . . . . ? C5 C4 C7 C8 42.2(10) . . . . ? C8 C7 N9 C10 1.5(12) . . . . ? C4 C7 N9 C10 -177.9(6) . . . . ? C8 C7 N9 Ag21 -153.8(6) . . . . ? C4 C7 N9 Ag21 26.8(9) . . . . ? C7 N9 C10 C11 159.0(7) . . . . ? Ag21 N9 C10 C11 -42.2(7) . . . . ? N9 C10 C11 N12 57.0(9) . . . . ? C10 C11 N12 C13 160.3(7) . . . . ? C10 C11 N12 Ag21 -40.9(8) . . . . ? C11 N12 C13 C14 0.2(12) . . . . ? Ag21 N12 C13 C14 -155.1(6) . . . . ? C11 N12 C13 C15 -177.1(6) . . . . ? Ag21 N12 C13 C15 27.5(9) . . . . ? N12 C13 C15 C20 -137.9(8) . . . . ? C14 C13 C15 C20 44.5(10) . . . . ? N12 C13 C15 C16 40.6(10) . . . . ? C14 C13 C15 C16 -137.0(8) . . . . ? C20 C15 C16 C17 2.9(11) . . . . ? C13 C15 C16 C17 -175.7(7) . . . . ? C15 C16 C17 N18 0.0(12) . . . . ? C16 C17 N18 C19 -2.6(11) . . . . ? C16 C17 N18 Ag22 177.2(6) . . . . ? C17 N18 C19 C20 2.2(11) . . . . ? Ag22 N18 C19 C20 -177.6(6) . . . . ? C16 C15 C20 C19 -3.2(11) . . . . ? C13 C15 C20 C19 175.3(7) . . . . ? N18 C19 C20 C15 0.6(12) . . . . ? C7 N9 Ag21 N9 27.6(6) . . . 2_755 ? C10 N9 Ag21 N9 -130.2(5) . . . 2_755 ? C7 N9 Ag21 N12 -74.4(7) . . . 2_755 ? C10 N9 Ag21 N12 127.8(5) . . . 2_755 ? C7 N9 Ag21 N12 172.5(6) . . . . ? C10 N9 Ag21 N12 14.8(5) . . . . ? C13 N12 Ag21 N9 172.0(6) . . . . ? C11 N12 Ag21 N9 14.4(5) . . . . ? C13 N12 Ag21 N9 -73.5(7) . . . 2_755 ? C11 N12 Ag21 N9 129.0(5) . . . 2_755 ? C13 N12 Ag21 N12 27.2(5) . . . 2_755 ? C11 N12 Ag21 N12 -130.3(5) . . . 2_755 ? C19 N18 Ag22 N18 157.9(6) . . . 2_855 ? C17 N18 Ag22 N18 -21.9(5) . . . 2_855 ? C19 N18 Ag22 N1 57.2(6) . . . 4_545 ? C17 N18 Ag22 N1 -122.6(6) . . . 4_545 ? C19 N18 Ag22 N1 -101.4(6) . . . 3_755 ? C17 N18 Ag22 N1 78.8(6) . . . 3_755 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.880 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.108 #====END=========================================================== data_Compound-5 _database_code_CSD 171384 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H51 Cl Cu N14 O4.50' _chemical_formula_weight 1115.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.6180(7) _cell_length_b 21.5640(9) _cell_length_c 18.8540(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.419(2) _cell_angle_gamma 90.00 _cell_volume 5531.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9806 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 25.42 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'red-yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 0.505 _exptl_absorpt_correction_type ? _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 0.71070 _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 degree 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 9806 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1468 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.42 _reflns_number_total 9806 _reflns_number_gt 4585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+9.7310P] 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 9806 _refine_ls_number_parameters 699 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1977 _refine_ls_R_factor_gt 0.0879 _refine_ls_wR_factor_ref 0.2485 _refine_ls_wR_factor_gt 0.1911 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.001 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 Cu Cu 0.42716(6) 0.08395(4) 0.11681(4) 0.0436(3) Uani 1 1 d . . . N1 N 0.0048(4) 0.1709(3) 0.4114(3) 0.0476(16) Uani 1 1 d . . . N2 N 0.0581(4) 0.1601(3) 0.3498(3) 0.0466(16) Uani 1 1 d . . . N3 N -0.1347(4) 0.2257(3) 0.2786(3) 0.0411(14) Uani 1 1 d . . . N4 N -0.1013(4) 0.2797(3) 0.3140(3) 0.0437(15) Uani 1 1 d . . . C5 C -0.0863(5) 0.1813(3) 0.3948(3) 0.0398(17) Uani 1 1 d . . . C6 C -0.1254(4) 0.1773(3) 0.3188(3) 0.0349(16) Uani 1 1 d . . . C7 C -0.1552(5) 0.1952(3) 0.4515(3) 0.0414(17) Uani 1 1 d . . . C8 C -0.1285(6) 0.1820(4) 0.5216(4) 0.057(2) Uani 1 1 d . . . H8 H -0.0675 0.1623 0.5327 0.069 Uiso 1 1 calc R . . C9 C -0.1893(6) 0.1972(4) 0.5755(4) 0.059(2) Uani 1 1 d . . . H9 H -0.1702 0.1888 0.6235 0.070 Uiso 1 1 calc R . . C10 C -0.2801(7) 0.2253(4) 0.5580(4) 0.065(2) Uani 1 1 d . . . H10 H -0.3223 0.2368 0.5946 0.077 Uiso 1 1 calc R . . C11 C -0.3084(6) 0.2363(4) 0.4883(4) 0.061(2) Uani 1 1 d . . . H11 H -0.3704 0.2547 0.4770 0.073 Uiso 1 1 calc R . . C12 C -0.2469(5) 0.2207(4) 0.4347(4) 0.049(2) Uani 1 1 d . . . H12 H -0.2673 0.2274 0.3865 0.059 Uiso 1 1 calc R . . C13 C -0.1498(5) 0.1165(4) 0.2909(4) 0.0418(18) Uani 1 1 d . . . C14 C -0.1736(5) 0.1072(4) 0.2191(4) 0.0458(18) Uani 1 1 d . . . H14 H -0.1801 0.1418 0.1881 0.055 Uiso 1 1 calc R . . C15 C -0.1881(5) 0.0475(4) 0.1922(4) 0.055(2) Uani 1 1 d . . . H15 H -0.2039 0.0420 0.1431 0.066 Uiso 1 1 calc R . . C16 C -0.1800(5) -0.0030(4) 0.2355(5) 0.058(2) Uani 1 1 d . . . H16 H -0.1890 -0.0435 0.2164 0.070 Uiso 1 1 calc R . . C17 C -0.1590(7) 0.0047(4) 0.3064(5) 0.073(3) Uani 1 1 d . . . H17 H -0.1544 -0.0303 0.3370 0.087 Uiso 1 1 calc R . . C18 C -0.1442(6) 0.0641(4) 0.3338(4) 0.063(2) Uani 1 1 d . . . H18 H -0.1300 0.0690 0.3833 0.076 Uiso 1 1 calc R . . C19 C 0.1486(5) 0.1469(4) 0.3632(4) 0.049(2) Uani 1 1 d . . . H19 H 0.1735 0.1441 0.4109 0.058 Uiso 1 1 calc R . . C20 C 0.2133(5) 0.1360(3) 0.3043(4) 0.0405(17) Uani 1 1 d . . . C21 C 0.3130(5) 0.1265(4) 0.3181(4) 0.048(2) Uani 1 1 d . . . H21 H 0.3401 0.1271 0.3654 0.058 Uiso 1 1 calc R . . C22 C 0.3717(5) 0.1159(4) 0.2613(4) 0.0473(19) Uani 1 1 d . . . H22 H 0.4400 0.1096 0.2712 0.057 Uiso 1 1 calc R . . N23 N 0.3396(4) 0.1141(3) 0.1939(3) 0.0447(15) Uani 1 1 d . . . C24 C 0.2423(5) 0.1237(4) 0.1814(4) 0.052(2) Uani 1 1 d . . . H24 H 0.2165 0.1230 0.1338 0.062 Uiso 1 1 calc R . . C25 C 0.1795(5) 0.1343(4) 0.2349(4) 0.053(2) Uani 1 1 d . . . H25 H 0.1115 0.1406 0.2238 0.063 Uiso 1 1 calc R . . C26 C -0.1122(5) 0.3288(4) 0.2769(4) 0.0399(17) Uani 1 1 d . . . H26 H -0.1449 0.3268 0.2314 0.048 Uiso 1 1 calc R . . C27 C -0.0748(4) 0.3883(3) 0.3039(3) 0.0335(16) Uani 1 1 d . . . C28 C -0.0900(5) 0.4415(3) 0.2644(4) 0.0391(17) Uani 1 1 d . . . H28 H -0.1273 0.4406 0.2207 0.047 Uiso 1 1 calc R . . C29 C -0.0492(5) 0.4964(3) 0.2904(4) 0.0405(17) Uani 1 1 d . . . H29 H -0.0603 0.5330 0.2630 0.049 Uiso 1 1 calc R . . N30 N 0.0049(4) 0.5015(3) 0.3515(3) 0.0414(15) Uani 1 1 d . . . C31 C 0.0172(5) 0.4488(4) 0.3898(4) 0.0430(18) Uani 1 1 d . . . H31 H 0.0534 0.4509 0.4340 0.052 Uiso 1 1 calc R . . C32 C -0.0201(5) 0.3923(4) 0.3680(4) 0.0423(18) Uani 1 1 d . . . H32 H -0.0087 0.3563 0.3963 0.051 Uiso 1 1 calc R . . N33 N 0.8984(4) 0.2163(3) -0.1049(3) 0.0466(16) Uani 1 1 d . . . N34 N 0.8290(4) 0.1840(3) -0.0651(3) 0.0498(16) Uani 1 1 d . . . N35 N 0.9262(4) 0.0700(3) -0.1552(3) 0.0432(15) Uani 1 1 d . . . N36 N 1.0170(4) 0.0841(3) -0.1189(3) 0.0448(15) Uani 1 1 d . . . C37 C 0.9254(5) 0.1843(4) -0.1576(4) 0.0423(18) Uani 1 1 d . . . C38 C 0.8813(5) 0.1209(4) -0.1751(3) 0.0387(17) Uani 1 1 d . . . C39 C 0.7886(5) 0.1180(4) -0.2176(4) 0.0417(18) Uani 1 1 d . . . C40 C 0.7573(6) 0.0625(4) -0.2476(4) 0.057(2) Uani 1 1 d . . . H40 H 0.7948 0.0258 -0.2394 0.069 Uiso 1 1 calc R . . C41 C 0.6709(6) 0.0603(5) -0.2896(4) 0.069(3) Uani 1 1 d . . . H41 H 0.6488 0.0221 -0.3096 0.082 Uiso 1 1 calc R . . C42 C 0.6175(6) 0.1137(6) -0.3020(4) 0.070(3) Uani 1 1 d . . . H42 H 0.5592 0.1124 -0.3314 0.085 Uiso 1 1 calc R . . C43 C 0.6479(5) 0.1685(5) -0.2723(4) 0.063(3) Uani 1 1 d . . . H43 H 0.6101 0.2050 -0.2808 0.076 Uiso 1 1 calc R . . C44 C 0.7332(5) 0.1715(4) -0.2302(4) 0.052(2) Uani 1 1 d . . . H44 H 0.7540 0.2099 -0.2098 0.063 Uiso 1 1 calc R . . C45 C 0.9985(5) 0.2084(4) -0.2068(4) 0.0438(19) Uani 1 1 d . . . C46 C 1.0382(5) 0.2668(4) -0.1966(4) 0.052(2) Uani 1 1 d . . . H46 H 1.0173 0.2918 -0.1586 0.063 Uiso 1 1 calc R . . C47 C 1.1084(5) 0.2895(4) -0.2415(5) 0.060(2) Uani 1 1 d . . . H47 H 1.1350 0.3298 -0.2345 0.072 Uiso 1 1 calc R . . C48 C 1.1391(6) 0.2526(5) -0.2966(4) 0.066(3) Uani 1 1 d . . . H48 H 1.1869 0.2679 -0.3274 0.079 Uiso 1 1 calc R . . C49 C 1.1008(5) 0.1937(5) -0.3071(4) 0.060(2) Uani 1 1 d . . . H49 H 1.1234 0.1683 -0.3442 0.072 Uiso 1 1 calc R . . C50 C 1.0300(5) 0.1723(4) -0.2637(4) 0.054(2) Uani 1 1 d . . . H50 H 1.0018 0.1325 -0.2722 0.064 Uiso 1 1 calc R . . C51 C 0.7645(5) 0.2186(4) -0.0396(3) 0.0416(17) Uani 1 1 d . . . H51 H 0.7652 0.2620 -0.0483 0.050 Uiso 1 1 calc R . . C52 C 0.6880(5) 0.1911(3) 0.0040(3) 0.0390(17) Uani 1 1 d . . . C53 C 0.6010(5) 0.2212(4) 0.0157(4) 0.050(2) Uani 1 1 d . . . H53 H 0.5904 0.2625 -0.0004 0.060 Uiso 1 1 calc R . . C54 C 0.5289(5) 0.1898(4) 0.0518(4) 0.0481(19) Uani 1 1 d . . . H54 H 0.4689 0.2109 0.0590 0.058 Uiso 1 1 calc R . . N55 N 0.5378(4) 0.1322(3) 0.0771(3) 0.0411(14) Uani 1 1 d . . . C56 C 0.6259(5) 0.1049(4) 0.0672(4) 0.052(2) Uani 1 1 d . . . H56 H 0.6365 0.0642 0.0851 0.062 Uiso 1 1 calc R . . C57 C 0.7004(5) 0.1332(4) 0.0328(4) 0.051(2) Uani 1 1 d . . . H57 H 0.7614 0.1124 0.0289 0.061 Uiso 1 1 calc R . . C58 C 1.0534(5) 0.0383(4) -0.0842(3) 0.0386(17) Uani 1 1 d . . . H58 H 1.0207 -0.0007 -0.0850 0.046 Uiso 1 1 calc R . . C59 C 1.1455(5) 0.0460(3) -0.0432(3) 0.0369(16) Uani 1 1 d . . . C60 C 1.1733(5) 0.0049(3) 0.0093(4) 0.0420(18) Uani 1 1 d . . . H60 H 1.1326 -0.0297 0.0181 0.050 Uiso 1 1 calc R . . C61 C 1.2583(5) 0.0128(4) 0.0493(4) 0.0444(19) Uani 1 1 d . . . H61 H 1.2750 -0.0168 0.0852 0.053 Uiso 1 1 calc R . . N62 N 1.3201(4) 0.0614(3) 0.0395(3) 0.0411(15) Uani 1 1 d . . . C63 C 1.2926(5) 0.1014(3) -0.0114(4) 0.0411(18) Uani 1 1 d . . . H63 H 1.3338 0.1361 -0.0190 0.049 Uiso 1 1 calc R . . C64 C 1.2081(5) 0.0956(3) -0.0539(3) 0.0414(18) Uani 1 1 d . . . H64 H 1.1929 0.1252 -0.0900 0.050 Uiso 1 1 calc R . . Cl65 Cl 0.82864(18) 0.37897(12) 0.05783(11) 0.0686(7) Uani 1 1 d . . . O66 O 0.9154(7) 0.3740(6) 0.0909(6) 0.187(5) Uani 1 1 d . . . O67 O 0.8369(7) 0.3858(5) -0.0102(3) 0.158(4) Uani 1 1 d . . . O68 O 0.7699(7) 0.3279(4) 0.0723(6) 0.164(4) Uani 1 1 d . . . O69 O 0.7841(10) 0.4320(6) 0.0891(8) 0.234(7) Uani 1 1 d . . . N70 N 1.0033(7) 0.1159(4) 0.0673(4) 0.090(3) Uani 1 1 d . . . C71 C 0.9852(6) 0.1654(6) 0.0823(5) 0.076(3) Uani 1 1 d . . . C72 C 0.9573(7) 0.2292(4) 0.1064(8) 0.126(5) Uani 1 1 d . . . H72A H 0.8858 0.2340 0.1017 0.188 Uiso 1 1 calc R . . H72B H 0.9887 0.2603 0.0769 0.188 Uiso 1 1 calc R . . H72C H 0.9792 0.2349 0.1561 0.188 Uiso 1 1 calc R . . N73 N 0.9310(6) 0.5791(5) 0.1348(5) 0.100(3) Uani 1 1 d . . . C74 C 0.9113(7) 0.5712(5) 0.0763(5) 0.074(3) Uani 1 1 d . . . C75 C 0.8881(8) 0.5625(5) 0.0017(5) 0.090(3) Uani 1 1 d . . . H75A H 0.9483 0.5659 -0.0248 0.135 Uiso 1 1 calc R . . H75B H 0.8411 0.5942 -0.0149 0.135 Uiso 1 1 calc R . . H75C H 0.8592 0.5213 -0.0061 0.135 Uiso 1 1 calc R . . O76 O 0.4955(12) 0.5106(8) -0.0300(7) 0.107(5) Uiso 0.50 1 d P . . C77 C 0.5874(13) 0.4986(9) -0.0309(10) 0.172(7) Uiso 1 1 d . . . C78 C 0.6180(17) 0.5155(12) -0.0959(14) 0.250(10) Uiso 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 Cu 0.0390(5) 0.0520(6) 0.0402(5) 0.0043(5) 0.0058(4) 0.0037(4) N1 0.046(4) 0.062(5) 0.036(3) -0.002(3) 0.005(3) 0.007(3) N2 0.042(4) 0.062(5) 0.036(3) -0.005(3) 0.008(3) 0.003(3) N3 0.042(3) 0.042(4) 0.039(3) -0.006(3) 0.000(3) 0.002(3) N4 0.045(3) 0.044(4) 0.042(4) -0.007(3) 0.005(3) -0.004(3) C5 0.041(4) 0.044(5) 0.035(4) -0.001(3) 0.007(3) 0.005(3) C6 0.031(3) 0.039(5) 0.034(4) -0.005(4) 0.003(3) -0.001(3) C7 0.051(4) 0.042(5) 0.031(4) 0.000(3) 0.003(3) -0.003(3) C8 0.052(5) 0.070(6) 0.050(5) 0.002(4) 0.012(4) -0.010(4) C9 0.066(5) 0.076(7) 0.034(4) 0.011(4) 0.011(4) -0.007(5) C10 0.087(6) 0.057(6) 0.053(5) -0.002(4) 0.033(5) 0.000(5) C11 0.062(5) 0.067(7) 0.055(5) 0.009(4) 0.023(4) 0.016(4) C12 0.057(5) 0.055(6) 0.036(4) 0.011(4) 0.015(4) 0.003(4) C13 0.043(4) 0.047(5) 0.035(4) -0.004(4) 0.002(3) -0.004(3) C14 0.047(4) 0.040(5) 0.051(5) -0.006(4) 0.004(3) 0.006(3) C15 0.055(5) 0.060(6) 0.049(5) -0.017(5) -0.005(4) 0.004(4) C16 0.055(5) 0.054(6) 0.067(6) -0.011(5) 0.010(4) -0.006(4) C17 0.113(8) 0.043(6) 0.062(6) 0.008(5) 0.006(5) -0.007(5) C18 0.100(7) 0.044(6) 0.046(5) -0.004(4) -0.001(5) -0.007(5) C19 0.043(4) 0.062(6) 0.041(4) 0.002(4) -0.003(3) -0.001(4) C20 0.044(4) 0.043(5) 0.034(4) 0.003(3) 0.001(3) 0.005(3) C21 0.044(4) 0.063(6) 0.038(4) -0.001(4) -0.003(3) 0.007(4) C22 0.035(4) 0.065(6) 0.042(5) -0.006(4) 0.000(3) 0.001(3) N23 0.038(3) 0.049(4) 0.047(4) 0.003(3) 0.004(3) 0.007(3) C24 0.036(4) 0.076(6) 0.043(4) 0.002(4) 0.007(3) 0.008(4) C25 0.046(4) 0.073(6) 0.039(5) 0.002(4) 0.000(3) 0.013(4) C26 0.039(4) 0.044(5) 0.037(4) -0.001(4) 0.003(3) 0.004(3) C27 0.035(4) 0.035(4) 0.031(4) -0.006(3) 0.012(3) -0.002(3) C28 0.041(4) 0.038(5) 0.039(4) -0.005(4) 0.004(3) -0.002(3) C29 0.047(4) 0.028(5) 0.047(4) 0.005(3) 0.010(3) 0.006(3) N30 0.040(3) 0.054(5) 0.030(3) -0.001(3) 0.004(3) 0.007(3) C31 0.042(4) 0.050(5) 0.038(4) -0.003(4) 0.005(3) 0.001(4) C32 0.044(4) 0.050(5) 0.033(4) -0.002(4) 0.006(3) -0.002(3) N33 0.046(3) 0.054(4) 0.040(4) 0.009(3) 0.007(3) -0.001(3) N34 0.055(4) 0.050(4) 0.046(4) 0.004(3) 0.015(3) 0.002(3) N35 0.037(3) 0.054(5) 0.038(3) 0.001(3) 0.001(3) -0.004(3) N36 0.045(3) 0.046(4) 0.044(3) -0.001(3) -0.002(3) 0.001(3) C37 0.035(4) 0.057(6) 0.034(4) 0.012(4) -0.003(3) 0.000(3) C38 0.043(4) 0.041(5) 0.033(4) 0.004(3) 0.004(3) -0.002(3) C39 0.035(4) 0.052(5) 0.038(4) 0.003(4) 0.000(3) -0.011(3) C40 0.060(5) 0.066(6) 0.046(5) 0.007(4) 0.001(4) -0.011(4) C41 0.059(5) 0.086(8) 0.060(6) 0.011(5) -0.008(4) -0.027(5) C42 0.039(5) 0.125(10) 0.047(5) 0.024(6) 0.000(4) -0.013(6) C43 0.033(4) 0.114(9) 0.041(5) 0.028(5) -0.004(4) -0.001(5) C44 0.042(4) 0.072(6) 0.044(4) 0.015(4) 0.004(3) 0.007(4) C45 0.032(4) 0.053(6) 0.047(4) 0.019(4) 0.008(3) 0.002(3) C46 0.038(4) 0.063(6) 0.056(5) 0.013(4) 0.005(4) -0.002(4) C47 0.049(5) 0.064(6) 0.066(6) 0.016(5) -0.006(4) -0.007(4) C48 0.047(5) 0.104(9) 0.048(5) 0.026(5) 0.009(4) -0.001(5) C49 0.043(4) 0.079(7) 0.060(5) 0.009(5) 0.016(4) 0.003(4) C50 0.041(4) 0.068(6) 0.052(5) 0.006(4) 0.002(4) 0.004(4) C51 0.046(4) 0.039(5) 0.040(4) 0.003(3) 0.006(3) -0.004(3) C52 0.050(4) 0.032(5) 0.035(4) 0.004(3) 0.002(3) 0.000(3) C53 0.043(4) 0.054(6) 0.055(5) 0.006(4) 0.007(4) 0.009(4) C54 0.039(4) 0.051(6) 0.054(5) -0.003(4) 0.001(3) 0.006(4) N55 0.050(3) 0.040(4) 0.034(3) 0.004(3) 0.000(3) 0.002(3) C56 0.046(4) 0.047(5) 0.063(5) 0.013(4) 0.012(4) 0.012(4) C57 0.045(4) 0.049(5) 0.059(5) 0.012(4) 0.016(4) 0.008(4) C58 0.040(4) 0.041(5) 0.035(4) 0.000(3) 0.006(3) 0.003(3) C59 0.040(4) 0.038(5) 0.032(4) -0.004(3) 0.001(3) 0.001(3) C60 0.037(4) 0.042(5) 0.047(4) 0.006(4) 0.004(3) -0.002(3) C61 0.046(4) 0.054(5) 0.034(4) 0.006(4) 0.006(3) 0.003(4) N62 0.044(3) 0.043(4) 0.036(3) 0.004(3) 0.006(3) 0.004(3) C63 0.048(4) 0.038(5) 0.038(4) -0.003(3) 0.007(3) 0.000(3) C64 0.045(4) 0.046(5) 0.033(4) 0.007(3) -0.001(3) 0.001(3) Cl65 0.0929(17) 0.0661(17) 0.0465(13) -0.0070(11) -0.0002(11) -0.0159(13) O66 0.125(7) 0.266(14) 0.161(9) 0.073(9) -0.080(7) -0.068(8) O67 0.204(9) 0.236(12) 0.035(4) -0.001(5) 0.006(5) -0.082(8) O68 0.160(8) 0.090(7) 0.251(11) -0.023(7) 0.128(8) -0.052(6) O69 0.268(15) 0.138(11) 0.296(17) -0.110(11) 0.012(12) 0.045(10) N70 0.143(8) 0.043(5) 0.089(6) -0.009(5) 0.045(5) 0.017(5) C71 0.062(6) 0.104(10) 0.064(6) 0.008(6) 0.003(5) -0.006(6) C72 0.078(7) 0.037(6) 0.266(16) -0.059(8) 0.065(9) -0.012(5) N73 0.117(7) 0.108(8) 0.072(6) 0.019(5) -0.022(5) -0.038(6) C74 0.081(6) 0.084(8) 0.057(6) 0.019(5) -0.014(5) -0.023(5) C75 0.123(8) 0.089(9) 0.058(6) 0.003(6) -0.009(6) -0.016(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 Cu N55 2.001(6) . ? Cu N23 2.026(5) . ? Cu N30 2.080(6) 2_545 ? Cu N62 2.076(6) 1_455 ? N1 C5 1.286(8) . ? N1 N2 1.414(7) . ? N2 C19 1.279(8) . ? N3 C6 1.291(8) . ? N3 N4 1.408(8) . ? N4 C26 1.275(9) . ? C5 C7 1.483(9) . ? C5 C6 1.510(9) . ? C6 C13 1.447(10) . ? C7 C8 1.385(10) . ? C7 C12 1.389(9) . ? C8 C9 1.376(10) . ? C9 C10 1.404(11) . ? C10 C11 1.373(11) . ? C11 C12 1.381(9) . ? C13 C14 1.393(10) . ? C13 C18 1.390(11) . ? C14 C15 1.393(10) . ? C15 C16 1.363(11) . ? C16 C17 1.366(11) . ? C17 C18 1.393(11) . ? C19 C20 1.467(9) . ? C20 C25 1.368(9) . ? C20 C21 1.387(9) . ? C21 C22 1.384(9) . ? C22 N23 1.327(8) . ? N23 C24 1.352(8) . ? C24 C25 1.370(9) . ? C26 C27 1.464(9) . ? C27 C28 1.378(9) . ? C27 C32 1.395(9) . ? C28 C29 1.388(9) . ? C29 N30 1.346(9) . ? N30 C31 1.354(9) . ? N30 Cu 2.080(6) 2 ? C31 C32 1.377(10) . ? N33 C37 1.277(9) . ? N33 N34 1.415(7) . ? N34 C51 1.263(8) . ? N35 C38 1.304(9) . ? N35 N36 1.419(7) . ? N36 C58 1.275(8) . ? C37 C45 1.483(9) . ? C37 C38 1.525(10) . ? C38 C39 1.467(9) . ? C39 C40 1.383(10) . ? C39 C44 1.395(10) . ? C40 C41 1.392(11) . ? C41 C42 1.377(13) . ? C42 C43 1.364(13) . ? C43 C44 1.381(10) . ? C45 C46 1.380(10) . ? C45 C50 1.408(10) . ? C46 C47 1.392(10) . ? C47 C48 1.386(12) . ? C48 C49 1.385(12) . ? C49 C50 1.371(10) . ? C51 C52 1.478(9) . ? C52 C57 1.369(10) . ? C52 C53 1.378(9) . ? C53 C54 1.395(10) . ? C54 N55 1.333(9) . ? N55 C56 1.357(8) . ? C56 C57 1.370(9) . ? C58 C59 1.454(9) . ? C59 C60 1.371(9) . ? C59 C64 1.386(9) . ? C60 C61 1.365(9) . ? C61 N62 1.362(9) . ? N62 C63 1.332(8) . ? N62 Cu 2.076(6) 1_655 ? C63 C64 1.380(9) . ? Cl65 O67 1.302(7) . ? Cl65 O66 1.317(8) . ? Cl65 O68 1.396(7) . ? Cl65 O69 1.433(10) . ? N70 C71 1.135(12) . ? C71 C72 1.502(14) . ? N73 C74 1.137(11) . ? C74 C75 1.442(13) . ? O76 O76 1.22(3) 3_665 ? O76 C77 1.28(2) . ? O76 C77 1.66(2) 3_665 ? C77 C78 1.36(3) . ? C77 O76 1.66(2) 3_665 ? 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 N55 Cu N23 125.2(2) . . ? N55 Cu N30 102.7(2) . 2_545 ? N23 Cu N30 109.6(2) . 2_545 ? N55 Cu N62 112.1(2) . 1_455 ? N23 Cu N62 99.3(2) . 1_455 ? N30 Cu N62 107.0(2) 2_545 1_455 ? C5 N1 N2 110.7(5) . . ? C19 N2 N1 113.5(6) . . ? C6 N3 N4 111.6(6) . . ? C26 N4 N3 113.6(6) . . ? N1 C5 C7 119.6(6) . . ? N1 C5 C6 121.2(5) . . ? C7 C5 C6 119.2(6) . . ? N3 C6 C13 120.2(6) . . ? N3 C6 C5 122.2(6) . . ? C13 C6 C5 117.6(6) . . ? C8 C7 C12 119.8(6) . . ? C8 C7 C5 119.9(6) . . ? C12 C7 C5 120.3(6) . . ? C9 C8 C7 120.9(8) . . ? C8 C9 C10 118.7(7) . . ? C11 C10 C9 120.5(7) . . ? C12 C11 C10 120.3(8) . . ? C11 C12 C7 119.7(7) . . ? C14 C13 C18 116.9(7) . . ? C14 C13 C6 121.7(7) . . ? C18 C13 C6 121.3(7) . . ? C13 C14 C15 120.7(7) . . ? C16 C15 C14 121.0(8) . . ? C15 C16 C17 119.8(8) . . ? C16 C17 C18 119.7(8) . . ? C13 C18 C17 121.9(8) . . ? N2 C19 C20 119.4(6) . . ? C25 C20 C21 117.7(6) . . ? C25 C20 C19 122.6(6) . . ? C21 C20 C19 119.7(6) . . ? C20 C21 C22 118.1(6) . . ? N23 C22 C21 124.6(6) . . ? C22 N23 C24 116.4(6) . . ? C22 N23 Cu 121.1(4) . . ? C24 N23 Cu 121.7(5) . . ? N23 C24 C25 122.3(7) . . ? C20 C25 C24 120.9(7) . . ? N4 C26 C27 120.4(7) . . ? C28 C27 C32 118.7(7) . . ? C28 C27 C26 119.9(6) . . ? C32 C27 C26 121.3(7) . . ? C27 C28 C29 118.1(7) . . ? N30 C29 C28 124.6(7) . . ? C31 N30 C29 116.1(6) . . ? C31 N30 Cu 121.3(5) . 2 ? C29 N30 Cu 122.5(5) . 2 ? N30 C31 C32 123.2(7) . . ? C31 C32 C27 119.3(7) . . ? C37 N33 N34 111.6(6) . . ? C51 N34 N33 113.7(6) . . ? C38 N35 N36 110.3(6) . . ? C58 N36 N35 113.2(6) . . ? N33 C37 C45 121.4(7) . . ? N33 C37 C38 121.9(6) . . ? C45 C37 C38 116.7(6) . . ? N35 C38 C39 120.3(7) . . ? N35 C38 C37 121.1(6) . . ? C39 C38 C37 118.6(6) . . ? C40 C39 C44 119.5(7) . . ? C40 C39 C38 120.2(7) . . ? C44 C39 C38 120.3(7) . . ? C39 C40 C41 120.1(9) . . ? C42 C41 C40 119.7(9) . . ? C43 C42 C41 120.4(8) . . ? C42 C43 C44 120.7(9) . . ? C43 C44 C39 119.6(8) . . ? C46 C45 C50 118.8(7) . . ? C46 C45 C37 120.2(7) . . ? C50 C45 C37 121.1(7) . . ? C45 C46 C47 120.7(8) . . ? C46 C47 C48 119.4(8) . . ? C49 C48 C47 120.7(7) . . ? C50 C49 C48 119.6(8) . . ? C49 C50 C45 120.8(8) . . ? N34 C51 C52 119.4(7) . . ? C57 C52 C53 117.3(6) . . ? C57 C52 C51 120.6(6) . . ? C53 C52 C51 122.0(7) . . ? C52 C53 C54 118.4(7) . . ? N55 C54 C53 124.9(7) . . ? C54 N55 C56 114.9(6) . . ? C54 N55 Cu 124.0(5) . . ? C56 N55 Cu 120.7(5) . . ? N55 C56 C57 123.3(7) . . ? C52 C57 C56 120.8(7) . . ? N36 C58 C59 119.5(7) . . ? C60 C59 C64 116.7(6) . . ? C60 C59 C58 121.0(6) . . ? C64 C59 C58 122.3(6) . . ? C61 C60 C59 121.4(7) . . ? N62 C61 C60 122.3(7) . . ? C63 N62 C61 116.1(6) . . ? C63 N62 Cu 121.5(5) . 1_655 ? C61 N62 Cu 120.3(5) . 1_655 ? N62 C63 C64 124.1(7) . . ? C63 C64 C59 119.3(7) . . ? O67 Cl65 O66 111.3(7) . . ? O67 Cl65 O68 110.9(6) . . ? O66 Cl65 O68 110.7(7) . . ? O67 Cl65 O69 111.8(9) . . ? O66 Cl65 O69 104.9(8) . . ? O68 Cl65 O69 107.0(7) . . ? N70 C71 C72 176.0(11) . . ? N73 C74 C75 178.5(11) . . ? O76 O76 C77 82.9(18) 3_665 . ? O76 O76 C77 50.0(12) 3_665 3_665 ? C77 O76 C77 132.9(13) . 3_665 ? O76 C77 C78 107.1(19) . . ? O76 C77 O76 47.1(13) . 3_665 ? C78 C77 O76 154(2) . 3_665 ? 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 C5 N1 N2 C19 -177.3(7) . . . . ? C6 N3 N4 C26 -177.8(5) . . . . ? N2 N1 C5 C7 -178.6(6) . . . . ? N2 N1 C5 C6 3.8(10) . . . . ? N4 N3 C6 C13 -176.1(5) . . . . ? N4 N3 C6 C5 2.0(8) . . . . ? N1 C5 C6 N3 -96.2(9) . . . . ? C7 C5 C6 N3 86.2(8) . . . . ? N1 C5 C6 C13 81.9(8) . . . . ? C7 C5 C6 C13 -95.7(8) . . . . ? N1 C5 C7 C8 -16.0(11) . . . . ? C6 C5 C7 C8 161.7(7) . . . . ? N1 C5 C7 C12 164.8(7) . . . . ? C6 C5 C7 C12 -17.6(10) . . . . ? C12 C7 C8 C9 -3.8(12) . . . . ? C5 C7 C8 C9 176.9(7) . . . . ? C7 C8 C9 C10 1.2(12) . . . . ? C8 C9 C10 C11 1.2(13) . . . . ? C9 C10 C11 C12 -1.1(13) . . . . ? C10 C11 C12 C7 -1.5(12) . . . . ? C8 C7 C12 C11 4.0(12) . . . . ? C5 C7 C12 C11 -176.7(7) . . . . ? N3 C6 C13 C14 6.9(10) . . . . ? C5 C6 C13 C14 -171.3(6) . . . . ? N3 C6 C13 C18 -177.3(7) . . . . ? C5 C6 C13 C18 4.5(9) . . . . ? C18 C13 C14 C15 -1.9(10) . . . . ? C6 C13 C14 C15 174.1(6) . . . . ? C13 C14 C15 C16 0.5(11) . . . . ? C14 C15 C16 C17 1.1(12) . . . . ? C15 C16 C17 C18 -1.1(13) . . . . ? C14 C13 C18 C17 1.8(12) . . . . ? C6 C13 C18 C17 -174.2(7) . . . . ? C16 C17 C18 C13 -0.3(14) . . . . ? N1 N2 C19 C20 -178.6(6) . . . . ? N2 C19 C20 C25 -5.6(12) . . . . ? N2 C19 C20 C21 175.0(7) . . . . ? C25 C20 C21 C22 0.1(11) . . . . ? C19 C20 C21 C22 179.5(7) . . . . ? C20 C21 C22 N23 -0.3(13) . . . . ? C21 C22 N23 C24 0.4(12) . . . . ? C21 C22 N23 Cu -169.4(6) . . . . ? N55 Cu N23 C22 -75.2(6) . . . . ? N30 Cu N23 C22 47.2(6) 2_545 . . . ? N62 Cu N23 C22 159.2(6) 1_455 . . . ? N55 Cu N23 C24 115.5(6) . . . . ? N30 Cu N23 C24 -122.1(6) 2_545 . . . ? N62 Cu N23 C24 -10.2(6) 1_455 . . . ? C22 N23 C24 C25 -0.5(12) . . . . ? Cu N23 C24 C25 169.3(6) . . . . ? C21 C20 C25 C24 -0.2(12) . . . . ? C19 C20 C25 C24 -179.6(8) . . . . ? N23 C24 C25 C20 0.4(13) . . . . ? N3 N4 C26 C27 -175.5(5) . . . . ? N4 C26 C27 C28 -177.7(6) . . . . ? N4 C26 C27 C32 4.9(9) . . . . ? C32 C27 C28 C29 0.5(9) . . . . ? C26 C27 C28 C29 -176.9(6) . . . . ? C27 C28 C29 N30 0.3(10) . . . . ? C28 C29 N30 C31 -1.5(9) . . . . ? C28 C29 N30 Cu 175.1(5) . . . 2 ? C29 N30 C31 C32 1.8(9) . . . . ? Cu N30 C31 C32 -174.8(5) 2 . . . ? N30 C31 C32 C27 -1.0(10) . . . . ? C28 C27 C32 C31 -0.2(9) . . . . ? C26 C27 C32 C31 177.2(6) . . . . ? C37 N33 N34 C51 -144.8(6) . . . . ? C38 N35 N36 C58 164.8(6) . . . . ? N34 N33 C37 C45 -179.5(6) . . . . ? N34 N33 C37 C38 3.2(9) . . . . ? N36 N35 C38 C39 176.2(5) . . . . ? N36 N35 C38 C37 -1.3(8) . . . . ? N33 C37 C38 N35 -98.2(8) . . . . ? C45 C37 C38 N35 84.3(8) . . . . ? N33 C37 C38 C39 84.3(8) . . . . ? C45 C37 C38 C39 -93.2(7) . . . . ? N35 C38 C39 C40 -11.6(10) . . . . ? C37 C38 C39 C40 165.9(6) . . . . ? N35 C38 C39 C44 170.6(6) . . . . ? C37 C38 C39 C44 -11.9(9) . . . . ? C44 C39 C40 C41 -0.3(11) . . . . ? C38 C39 C40 C41 -178.1(7) . . . . ? C39 C40 C41 C42 0.9(12) . . . . ? C40 C41 C42 C43 -1.2(12) . . . . ? C41 C42 C43 C44 0.8(12) . . . . ? C42 C43 C44 C39 -0.2(11) . . . . ? C40 C39 C44 C43 -0.1(10) . . . . ? C38 C39 C44 C43 177.7(6) . . . . ? N33 C37 C45 C46 -0.7(10) . . . . ? C38 C37 C45 C46 176.8(6) . . . . ? N33 C37 C45 C50 178.3(7) . . . . ? C38 C37 C45 C50 -4.3(9) . . . . ? C50 C45 C46 C47 -0.3(11) . . . . ? C37 C45 C46 C47 178.6(6) . . . . ? C45 C46 C47 C48 -0.5(11) . . . . ? C46 C47 C48 C49 -0.1(12) . . . . ? C47 C48 C49 C50 1.6(12) . . . . ? C48 C49 C50 C45 -2.5(12) . . . . ? C46 C45 C50 C49 1.9(11) . . . . ? C37 C45 C50 C49 -177.1(7) . . . . ? N33 N34 C51 C52 -179.3(6) . . . . ? N34 C51 C52 C57 17.7(10) . . . . ? N34 C51 C52 C53 -160.6(7) . . . . ? C57 C52 C53 C54 -4.2(11) . . . . ? C51 C52 C53 C54 174.2(6) . . . . ? C52 C53 C54 N55 0.9(11) . . . . ? C53 C54 N55 C56 1.8(10) . . . . ? C53 C54 N55 Cu -171.2(6) . . . . ? N23 Cu N55 C54 -52.6(6) . . . . ? N30 Cu N55 C54 -178.0(5) 2_545 . . . ? N62 Cu N55 C54 67.5(6) 1_455 . . . ? N23 Cu N55 C56 134.7(5) . . . . ? N30 Cu N55 C56 9.3(6) 2_545 . . . ? N62 Cu N55 C56 -105.2(5) 1_455 . . . ? C54 N55 C56 C57 -1.2(11) . . . . ? Cu N55 C56 C57 172.1(6) . . . . ? C53 C52 C57 C56 4.8(11) . . . . ? C51 C52 C57 C56 -173.5(7) . . . . ? N55 C56 C57 C52 -2.1(12) . . . . ? N35 N36 C58 C59 -178.9(5) . . . . ? N36 C58 C59 C60 161.8(6) . . . . ? N36 C58 C59 C64 -16.6(10) . . . . ? C64 C59 C60 C61 0.3(10) . . . . ? C58 C59 C60 C61 -178.2(6) . . . . ? C59 C60 C61 N62 0.0(11) . . . . ? C60 C61 N62 C63 0.3(10) . . . . ? C60 C61 N62 Cu 164.0(5) . . . 1_655 ? C61 N62 C63 C64 -0.9(10) . . . . ? Cu N62 C63 C64 -164.4(5) 1_655 . . . ? N62 C63 C64 C59 1.2(10) . . . . ? C60 C59 C64 C63 -0.8(10) . . . . ? C58 C59 C64 C63 177.6(6) . . . . ? O76 O76 C77 C78 179(2) 3_665 . . . ? C77 O76 C77 C78 179(2) 3_665 . . . ? C77 O76 C77 O76 0.005(3) 3_665 . . 3_665 ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.42 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.843 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.080 #=======END====================================================== data_Compound-6 _database_code_CSD 171385 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H54 Ag Cl N14 O4' _chemical_formula_weight 1214.52 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' '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 'triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6820(3) _cell_length_b 12.8320(3) _cell_length_c 21.3680(5) _cell_angle_alpha 75.0060(9) _cell_angle_beta 73.0780(10) _cell_angle_gamma 64.3650(14) _cell_volume 2963.55(12) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 12725 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 27.91 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type multi-scan _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 0.71070 _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 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 12725 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.91 _reflns_number_total 12725 _reflns_number_gt 9982 _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^)+(0.0686P)^2^+2.6522P] 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 12725 _refine_ls_number_parameters 762 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.019 _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 Ag Ag 0.808847(19) -0.051469(19) 0.204435(11) 0.02617(8) Uani 1 1 d . . . N1 N 1.1775(2) -0.1333(2) 0.50726(11) 0.0226(5) Uani 1 1 d . . . N2 N 1.1088(2) -0.1432(2) 0.46970(12) 0.0238(5) Uani 1 1 d . . . N3 N 1.3440(2) -0.3830(2) 0.45337(12) 0.0236(5) Uani 1 1 d . . . N4 N 1.3945(2) -0.3025(2) 0.41414(12) 0.0249(5) Uani 1 1 d . . . C5 C 1.2575(2) -0.2327(2) 0.52548(13) 0.0195(5) Uani 1 1 d . . . C6 C 1.2758(2) -0.3464(2) 0.50757(13) 0.0207(5) Uani 1 1 d . . . C7 C 1.3366(2) -0.2373(2) 0.56626(13) 0.0193(5) Uani 1 1 d . . . C8 C 1.3130(2) -0.1406(2) 0.59411(13) 0.0222(5) Uani 1 1 d . . . H8 H 1.2444 -0.0713 0.5880 0.027 Uiso 1 1 calc R . . C9 C 1.3893(3) -0.1453(2) 0.63051(14) 0.0251(6) Uani 1 1 d . . . H9 H 1.3726 -0.0789 0.6492 0.030 Uiso 1 1 calc R . . C10 C 1.4898(3) -0.2457(3) 0.64011(14) 0.0272(6) Uani 1 1 d . . . H10 H 1.5418 -0.2482 0.6652 0.033 Uiso 1 1 calc R . . C11 C 1.5136(3) -0.3422(3) 0.61293(15) 0.0271(6) Uani 1 1 d . . . H11 H 1.5823 -0.4114 0.6193 0.032 Uiso 1 1 calc R . . C12 C 1.4371(2) -0.3382(2) 0.57607(14) 0.0235(6) Uani 1 1 d . . . H12 H 1.4539 -0.4049 0.5576 0.028 Uiso 1 1 calc R . . C13 C 1.2189(2) -0.4211(2) 0.55633(13) 0.0209(5) Uani 1 1 d . . . C14 C 1.2700(3) -0.5418(2) 0.55860(14) 0.0252(6) Uani 1 1 d . . . H14 H 1.3416 -0.5765 0.5281 0.030 Uiso 1 1 calc R . . C15 C 1.2169(3) -0.6121(3) 0.60524(15) 0.0291(6) Uani 1 1 d . . . H15 H 1.2522 -0.6945 0.6066 0.035 Uiso 1 1 calc R . . C16 C 1.1124(3) -0.5619(3) 0.64983(15) 0.0294(6) Uani 1 1 d . . . H16 H 1.0770 -0.6103 0.6821 0.035 Uiso 1 1 calc R . . C17 C 1.0594(3) -0.4419(3) 0.64763(15) 0.0288(6) Uani 1 1 d . . . H17 H 0.9869 -0.4078 0.6776 0.035 Uiso 1 1 calc R . . C18 C 1.1126(2) -0.3711(2) 0.60142(14) 0.0235(6) Uani 1 1 d . . . H18 H 1.0770 -0.2887 0.6003 0.028 Uiso 1 1 calc R . . C19 C 1.0849(3) -0.0589(2) 0.42208(14) 0.0239(6) Uani 1 1 d . . . H19 H 1.1121 0.0021 0.4158 0.029 Uiso 1 1 calc R . . C20 C 1.0155(2) -0.0557(2) 0.37683(14) 0.0225(6) Uani 1 1 d . . . C21 C 0.9563(2) -0.1310(2) 0.38964(14) 0.0230(6) Uani 1 1 d . . . H21 H 0.9576 -0.1855 0.4294 0.028 Uiso 1 1 calc R . . C22 C 0.8960(3) -0.1255(2) 0.34385(14) 0.0236(6) Uani 1 1 d . . . H22 H 0.8563 -0.1775 0.3531 0.028 Uiso 1 1 calc R . . N23 N 0.8905(2) -0.0503(2) 0.28686(11) 0.0233(5) Uani 1 1 d . . . C24 C 0.9453(3) 0.0230(3) 0.27555(15) 0.0316(7) Uani 1 1 d . . . H24 H 0.9413 0.0775 0.2357 0.038 Uiso 1 1 calc R . . C25 C 1.0080(3) 0.0240(3) 0.31884(15) 0.0313(7) Uani 1 1 d . . . H25 H 1.0451 0.0783 0.3088 0.038 Uiso 1 1 calc R . . C26 C 1.4691(2) -0.3406(2) 0.36239(14) 0.0242(6) Uani 1 1 d . . . H26 H 1.4827 -0.4143 0.3530 0.029 Uiso 1 1 calc R . . C27 C 1.5340(3) -0.2699(2) 0.31749(13) 0.0235(6) Uani 1 1 d . . . C28 C 1.4995(3) -0.1532(3) 0.32229(15) 0.0286(6) Uani 1 1 d . . . H28 H 1.4278 -0.1147 0.3516 0.034 Uiso 1 1 calc R . . C29 C 1.5703(3) -0.0941(3) 0.28407(15) 0.0302(6) Uani 1 1 d . . . H29 H 1.5449 -0.0139 0.2870 0.036 Uiso 1 1 calc R . . N30 N 1.6740(2) -0.1444(2) 0.24260(12) 0.0258(5) Uani 1 1 d . . . C31 C 1.7035(3) -0.2551(3) 0.23601(14) 0.0277(6) Uani 1 1 d . . . H31 H 1.7740 -0.2905 0.2051 0.033 Uiso 1 1 calc R . . C32 C 1.6369(3) -0.3206(3) 0.27178(14) 0.0272(6) Uani 1 1 d . . . H32 H 1.6610 -0.3988 0.2652 0.033 Uiso 1 1 calc R . . N33 N 0.4038(2) 0.4674(2) -0.06827(12) 0.0267(5) Uani 1 1 d . . . N34 N 0.4476(2) 0.3930(2) -0.01250(12) 0.0294(6) Uani 1 1 d . . . N35 N 0.2104(2) 0.3467(2) 0.00360(12) 0.0273(5) Uani 1 1 d . . . N36 N 0.1470(2) 0.4605(2) 0.01904(12) 0.0299(5) Uani 1 1 d . . . C37 C 0.3271(3) 0.4429(2) -0.08308(14) 0.0228(6) Uani 1 1 d . . . C38 C 0.2968(3) 0.3379(2) -0.04687(14) 0.0235(6) Uani 1 1 d . . . C39 C 0.3702(3) 0.2238(2) -0.06971(13) 0.0231(6) Uani 1 1 d . . . C40 C 0.4693(3) 0.2109(3) -0.12170(16) 0.0317(7) Uani 1 1 d . . . H40 H 0.4897 0.2765 -0.1430 0.038 Uiso 1 1 calc R . . C41 C 0.5384(3) 0.1030(3) -0.14243(17) 0.0364(7) Uani 1 1 d . . . H41 H 0.6063 0.0948 -0.1776 0.044 Uiso 1 1 calc R . . C42 C 0.5091(3) 0.0078(3) -0.11241(17) 0.0348(7) Uani 1 1 d . . . H42 H 0.5564 -0.0660 -0.1268 0.042 Uiso 1 1 calc R . . C43 C 0.4111(3) 0.0199(3) -0.06151(18) 0.0427(8) Uani 1 1 d . . . H43 H 0.3911 -0.0460 -0.0407 0.051 Uiso 1 1 calc R . . C44 C 0.3413(3) 0.1266(3) -0.04021(17) 0.0387(8) Uani 1 1 d . . . H44 H 0.2732 0.1338 -0.0053 0.046 Uiso 1 1 calc R . . C45 C 0.2694(3) 0.5159(2) -0.13928(13) 0.0223(5) Uani 1 1 d . . . C46 C 0.1668(3) 0.5082(2) -0.14626(14) 0.0264(6) Uani 1 1 d . . . H46 H 0.1345 0.4564 -0.1150 0.032 Uiso 1 1 calc R . . C47 C 0.1120(3) 0.5765(3) -0.19897(15) 0.0292(6) Uani 1 1 d . . . H47 H 0.0429 0.5706 -0.2040 0.035 Uiso 1 1 calc R . . C48 C 0.1580(3) 0.6525(3) -0.24373(15) 0.0307(7) Uani 1 1 d . . . H48 H 0.1196 0.7000 -0.2792 0.037 Uiso 1 1 calc R . . C49 C 0.2594(3) 0.6601(3) -0.23742(16) 0.0355(7) Uani 1 1 d . . . H49 H 0.2915 0.7117 -0.2690 0.043 Uiso 1 1 calc R . . C50 C 0.3149(3) 0.5926(3) -0.18505(15) 0.0309(7) Uani 1 1 d . . . H50 H 0.3841 0.5990 -0.1806 0.037 Uiso 1 1 calc R . . C51 C 0.5594(3) 0.3575(3) -0.01866(15) 0.0296(6) Uani 1 1 d . . . H51 H 0.6060 0.3821 -0.0585 0.035 Uiso 1 1 calc R . . C52 C 0.6175(3) 0.2782(2) 0.03557(15) 0.0267(6) Uani 1 1 d . . . C53 C 0.5522(3) 0.2604(3) 0.09951(15) 0.0303(6) Uani 1 1 d . . . H53 H 0.4684 0.3035 0.1101 0.036 Uiso 1 1 calc R . . C54 C 0.6111(3) 0.1795(3) 0.14697(15) 0.0311(6) Uani 1 1 d . . . H54 H 0.5660 0.1682 0.1904 0.037 Uiso 1 1 calc R . . N55 N 0.7298(2) 0.1151(2) 0.13504(12) 0.0287(5) Uani 1 1 d . . . C56 C 0.7918(3) 0.1340(3) 0.07371(17) 0.0345(7) Uani 1 1 d . . . H56 H 0.8756 0.0900 0.0645 0.041 Uiso 1 1 calc R . . C57 C 0.7396(3) 0.2147(3) 0.02311(16) 0.0345(7) Uani 1 1 d . . . H57 H 0.7871 0.2262 -0.0195 0.041 Uiso 1 1 calc R . . C58 C 0.1494(3) 0.4711(3) 0.07599(15) 0.0292(6) Uani 1 1 d . . . H58 H 0.1927 0.4052 0.1039 0.035 Uiso 1 1 calc R . . C59 C 0.0849(3) 0.5858(3) 0.09862(14) 0.0255(6) Uani 1 1 d . . . C60 C 0.0110(3) 0.6828(3) 0.06236(14) 0.0284(6) Uani 1 1 d . . . H60 H 0.0017 0.6778 0.0208 0.034 Uiso 1 1 calc R . . C61 C -0.0485(3) 0.7867(3) 0.08809(14) 0.0286(6) Uani 1 1 d . . . H61 H -0.1000 0.8520 0.0635 0.034 Uiso 1 1 calc R . . N62 N -0.0376(2) 0.8005(2) 0.14579(12) 0.0270(5) Uani 1 1 d . . . C63 C 0.0358(3) 0.7078(3) 0.17915(15) 0.0302(6) Uani 1 1 d . . . H63 H 0.0464 0.7164 0.2195 0.036 Uiso 1 1 calc R . . C64 C 0.0975(3) 0.5998(3) 0.15812(15) 0.0306(6) Uani 1 1 d . . . H64 H 0.1477 0.5359 0.1840 0.037 Uiso 1 1 calc R . . Cl65 Cl 0.24709(7) 0.18297(7) 0.26662(4) 0.03247(17) Uani 1 1 d . . . O66 O 0.1668(2) 0.1897(2) 0.33004(13) 0.0525(7) Uani 1 1 d . . . O67 O 0.3587(2) 0.1775(2) 0.27292(15) 0.0527(7) Uani 1 1 d . . . O68 O 0.1939(3) 0.2840(3) 0.22155(15) 0.0633(8) Uani 1 1 d . . . O69 O 0.2661(3) 0.0778(3) 0.24594(17) 0.0662(9) Uani 1 1 d . . . N70 N 0.3625(3) 0.1375(3) 0.54040(17) 0.0564(9) Uani 1 1 d . . . C71 C 0.3538(3) 0.1037(3) 0.49878(18) 0.0399(8) Uani 1 1 d . . . C72 C 0.3461(4) 0.0561(4) 0.44660(19) 0.0583(12) Uani 1 1 d . . . H72A H 0.4234 -0.0053 0.4320 0.087 Uiso 1 1 calc R . . H72B H 0.3248 0.1185 0.4092 0.087 Uiso 1 1 calc R . . H72C H 0.2848 0.0229 0.4632 0.087 Uiso 1 1 calc R . . N73 N 0.1039(4) 0.0097(4) 0.0713(2) 0.0700(11) Uani 1 1 d . A . C74 C 0.1072(3) 0.0729(3) 0.09728(18) 0.0429(8) Uani 1 1 d . . . C75A C 0.1332(10) 0.1426(12) 0.1317(7) 0.050(3) Uani 0.50 1 d P A 1 H75A H 0.1734 0.0913 0.1676 0.074 Uiso 0.50 1 calc PR A 1 H75B H 0.0583 0.2031 0.1499 0.074 Uiso 0.50 1 calc PR A 1 H75C H 0.1852 0.1797 0.1002 0.074 Uiso 0.50 1 calc PR A 1 C75B C 0.0798(11) 0.1776(10) 0.1237(6) 0.049(3) Uani 0.50 1 d P A 2 H75D H 0.1221 0.2245 0.0924 0.074 Uiso 0.50 1 calc PR A 2 H75E H 0.1054 0.1550 0.1661 0.074 Uiso 0.50 1 calc PR A 2 H75F H -0.0065 0.2236 0.1306 0.074 Uiso 0.50 1 calc PR A 2 C76 C 0.1273(5) 0.5324(6) 0.4151(3) 0.0857(18) Uani 1 1 d . . . H76A H 0.1522 0.5583 0.4457 0.129 Uiso 1 1 calc R . . H76B H 0.1434 0.4487 0.4282 0.129 Uiso 1 1 calc R . . H76C H 0.0416 0.5765 0.4165 0.129 Uiso 1 1 calc R . . C77 C 0.1930(4) 0.5522(4) 0.3491(2) 0.0541(10) Uani 1 1 d . . . C78 C 0.2443(4) 0.4616(4) 0.3113(2) 0.0579(11) Uani 1 1 d . . . H78 H 0.2273 0.3931 0.3279 0.069 Uiso 1 1 calc R . . C79 C 0.3200(4) 0.4697(4) 0.2498(2) 0.0636(12) Uani 1 1 d . . . H79 H 0.3531 0.4070 0.2250 0.076 Uiso 1 1 calc R . . C80 C 0.3483(4) 0.5707(5) 0.2234(2) 0.0687(13) Uani 1 1 d . . . H80 H 0.4009 0.5744 0.1817 0.082 Uiso 1 1 calc R . . C81 C 0.3001(4) 0.6620(5) 0.2581(3) 0.0756(15) Uani 1 1 d . . . H81 H 0.3149 0.7314 0.2404 0.091 Uiso 1 1 calc R . . C82 C 0.2242(4) 0.6485(4) 0.3239(3) 0.0645(12) Uani 1 1 d . . . H82 H 0.1953 0.7084 0.3503 0.077 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 0.02848(13) 0.02506(12) 0.02659(12) -0.00505(8) -0.00948(9) -0.00882(10) N1 0.0248(12) 0.0212(11) 0.0238(12) -0.0063(9) -0.0073(10) -0.0078(10) N2 0.0241(12) 0.0222(11) 0.0269(12) -0.0061(9) -0.0097(10) -0.0065(10) N3 0.0249(12) 0.0203(11) 0.0259(12) -0.0047(9) -0.0029(10) -0.0099(10) N4 0.0280(13) 0.0251(12) 0.0240(12) -0.0061(9) -0.0018(10) -0.0133(11) C5 0.0200(13) 0.0189(12) 0.0188(12) -0.0037(10) -0.0032(10) -0.0069(11) C6 0.0202(13) 0.0174(12) 0.0251(14) -0.0043(10) -0.0079(11) -0.0050(11) C7 0.0210(13) 0.0194(12) 0.0182(12) -0.0029(10) -0.0045(10) -0.0083(11) C8 0.0233(14) 0.0181(12) 0.0226(13) -0.0023(10) -0.0049(11) -0.0062(11) C9 0.0332(16) 0.0223(13) 0.0247(14) -0.0044(11) -0.0092(12) -0.0127(13) C10 0.0290(15) 0.0304(15) 0.0279(15) -0.0025(12) -0.0097(12) -0.0153(14) C11 0.0233(14) 0.0226(14) 0.0357(16) -0.0050(12) -0.0111(12) -0.0058(12) C12 0.0241(14) 0.0187(12) 0.0291(15) -0.0067(11) -0.0058(11) -0.0076(12) C13 0.0240(14) 0.0211(13) 0.0210(13) -0.0048(10) -0.0069(11) -0.0095(12) C14 0.0266(15) 0.0211(13) 0.0277(15) -0.0076(11) -0.0037(12) -0.0081(12) C15 0.0327(16) 0.0219(13) 0.0345(16) -0.0052(12) -0.0054(13) -0.0126(13) C16 0.0307(16) 0.0307(15) 0.0301(15) 0.0001(12) -0.0066(12) -0.0175(14) C17 0.0247(15) 0.0327(15) 0.0293(15) -0.0082(12) -0.0037(12) -0.0107(13) C18 0.0222(14) 0.0216(13) 0.0274(14) -0.0067(11) -0.0061(11) -0.0067(12) C19 0.0260(15) 0.0209(13) 0.0266(14) -0.0047(11) -0.0079(11) -0.0085(12) C20 0.0228(14) 0.0218(13) 0.0242(14) -0.0068(11) -0.0058(11) -0.0073(12) C21 0.0259(14) 0.0189(12) 0.0241(14) -0.0015(10) -0.0074(11) -0.0081(12) C22 0.0246(14) 0.0208(13) 0.0252(14) -0.0046(11) -0.0036(11) -0.0091(12) N23 0.0265(12) 0.0249(12) 0.0213(11) -0.0038(9) -0.0072(9) -0.0111(11) C24 0.0440(18) 0.0369(16) 0.0230(14) 0.0045(12) -0.0118(13) -0.0257(16) C25 0.0415(18) 0.0346(16) 0.0290(16) 0.0038(12) -0.0136(13) -0.0257(15) C26 0.0237(14) 0.0223(13) 0.0262(14) -0.0074(11) -0.0035(11) -0.0077(12) C27 0.0259(14) 0.0234(13) 0.0216(13) -0.0052(11) -0.0041(11) -0.0094(12) C28 0.0258(15) 0.0252(14) 0.0309(16) -0.0099(12) 0.0010(12) -0.0076(13) C29 0.0308(16) 0.0230(14) 0.0359(17) -0.0109(12) -0.0024(13) -0.0088(13) N30 0.0248(12) 0.0269(12) 0.0268(12) -0.0063(10) -0.0041(10) -0.0106(11) C31 0.0282(15) 0.0277(14) 0.0263(15) -0.0103(12) 0.0004(12) -0.0104(13) C32 0.0287(15) 0.0236(13) 0.0284(15) -0.0087(11) 0.0000(12) -0.0105(13) N33 0.0361(14) 0.0191(11) 0.0283(13) 0.0005(9) -0.0149(11) -0.0108(11) N34 0.0410(16) 0.0230(12) 0.0301(13) 0.0003(10) -0.0174(11) -0.0136(12) N35 0.0363(14) 0.0218(11) 0.0218(12) -0.0033(9) -0.0028(10) -0.0114(11) N36 0.0357(14) 0.0219(12) 0.0280(13) -0.0062(10) -0.0003(11) -0.0102(11) C37 0.0281(15) 0.0164(12) 0.0234(14) -0.0042(10) -0.0053(11) -0.0075(12) C38 0.0286(15) 0.0196(13) 0.0227(14) -0.0014(10) -0.0090(11) -0.0084(12) C39 0.0283(15) 0.0195(13) 0.0227(14) -0.0032(10) -0.0078(11) -0.0087(12) C40 0.0362(17) 0.0227(14) 0.0353(17) -0.0062(12) -0.0027(14) -0.0125(14) C41 0.0337(17) 0.0289(16) 0.0424(19) -0.0139(14) 0.0007(14) -0.0091(14) C42 0.0389(18) 0.0255(15) 0.0412(18) -0.0116(13) -0.0069(15) -0.0108(14) C43 0.056(2) 0.0237(15) 0.047(2) -0.0071(14) 0.0016(17) -0.0209(16) C44 0.049(2) 0.0273(15) 0.0366(18) -0.0089(13) 0.0044(15) -0.0186(15) C45 0.0265(14) 0.0168(12) 0.0229(13) -0.0054(10) -0.0047(11) -0.0066(12) C46 0.0307(15) 0.0225(13) 0.0267(15) -0.0030(11) -0.0060(12) -0.0113(13) C47 0.0301(16) 0.0292(15) 0.0302(16) -0.0034(12) -0.0118(13) -0.0103(14) C48 0.0364(17) 0.0250(14) 0.0281(15) 0.0009(12) -0.0125(13) -0.0085(14) C49 0.0400(19) 0.0317(16) 0.0330(17) 0.0050(13) -0.0083(14) -0.0173(15) C50 0.0335(17) 0.0281(15) 0.0318(16) 0.0017(12) -0.0076(13) -0.0155(14) C51 0.0392(18) 0.0227(14) 0.0283(15) 0.0004(11) -0.0103(13) -0.0137(14) C52 0.0335(16) 0.0212(13) 0.0304(15) -0.0025(11) -0.0119(13) -0.0127(13) C53 0.0326(16) 0.0220(14) 0.0343(16) -0.0066(12) -0.0109(13) -0.0049(13) C54 0.0358(17) 0.0278(15) 0.0283(15) -0.0045(12) -0.0079(13) -0.0100(14) N55 0.0325(14) 0.0240(12) 0.0313(13) -0.0020(10) -0.0108(11) -0.0110(11) C56 0.0297(16) 0.0334(16) 0.0407(18) 0.0010(14) -0.0112(14) -0.0137(15) C57 0.0359(18) 0.0355(17) 0.0338(17) 0.0031(13) -0.0078(14) -0.0197(15) C58 0.0358(17) 0.0245(14) 0.0238(14) -0.0025(11) -0.0014(12) -0.0122(13) C59 0.0266(15) 0.0267(14) 0.0242(14) -0.0048(11) -0.0003(11) -0.0138(13) C60 0.0329(16) 0.0289(15) 0.0216(14) -0.0050(11) -0.0024(12) -0.0119(13) C61 0.0307(16) 0.0282(15) 0.0246(15) -0.0060(12) -0.0043(12) -0.0090(13) N62 0.0256(13) 0.0312(13) 0.0254(12) -0.0091(10) -0.0016(10) -0.0117(11) C63 0.0276(15) 0.0368(16) 0.0291(15) -0.0119(13) -0.0064(12) -0.0108(14) C64 0.0303(16) 0.0272(15) 0.0311(16) -0.0057(12) -0.0082(13) -0.0063(14) Cl65 0.0291(4) 0.0302(4) 0.0373(4) -0.0077(3) -0.0062(3) -0.0097(3) O66 0.0488(15) 0.0500(15) 0.0487(16) -0.0127(12) 0.0053(12) -0.0170(13) O67 0.0325(13) 0.0492(15) 0.081(2) -0.0151(14) -0.0180(13) -0.0136(12) O68 0.081(2) 0.0590(18) 0.0558(18) 0.0130(14) -0.0402(16) -0.0285(17) O69 0.0578(17) 0.0551(17) 0.095(2) -0.0459(17) 0.0133(16) -0.0295(15) N70 0.074(2) 0.0435(18) 0.048(2) -0.0168(15) 0.0015(17) -0.0238(18) C71 0.044(2) 0.0368(18) 0.0363(19) -0.0001(15) -0.0039(15) -0.0189(16) C72 0.077(3) 0.084(3) 0.039(2) 0.003(2) -0.018(2) -0.057(3) N73 0.072(3) 0.082(3) 0.074(3) -0.039(2) 0.008(2) -0.046(2) C74 0.0395(19) 0.050(2) 0.0398(19) -0.0087(17) 0.0009(15) -0.0230(18) C75A 0.052(7) 0.060(8) 0.038(5) -0.014(5) 0.006(5) -0.029(6) C75B 0.080(9) 0.044(7) 0.031(5) -0.014(5) 0.013(6) -0.041(7) C76 0.058(3) 0.117(5) 0.091(4) 0.007(3) -0.033(3) -0.044(3) C77 0.063(3) 0.053(2) 0.055(2) -0.0098(19) -0.022(2) -0.024(2) C78 0.055(3) 0.058(3) 0.065(3) -0.013(2) -0.026(2) -0.014(2) C79 0.052(3) 0.070(3) 0.071(3) -0.019(2) -0.025(2) -0.012(2) C80 0.051(3) 0.083(3) 0.062(3) -0.020(3) -0.022(2) -0.004(3) C81 0.054(3) 0.068(3) 0.116(5) -0.028(3) -0.029(3) -0.019(3) C82 0.046(2) 0.059(3) 0.091(4) -0.033(3) -0.020(2) -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 N55 2.268(2) . ? Ag N23 2.294(2) . ? Ag N30 2.337(2) 1_455 ? Ag N62 2.362(2) 1_645 ? N1 C5 1.289(4) . ? N1 N2 1.405(3) . ? N2 C19 1.274(4) . ? N3 C6 1.287(4) . ? N3 N4 1.411(3) . ? N4 C26 1.276(4) . ? C5 C7 1.483(4) . ? C5 C6 1.508(4) . ? C6 C13 1.473(4) . ? C7 C12 1.390(4) . ? C7 C8 1.393(4) . ? C8 C9 1.381(4) . ? C8 H8 0.9500 . ? C9 C10 1.386(4) . ? C9 H9 0.9500 . ? C10 C11 1.381(4) . ? C10 H10 0.9500 . ? C11 C12 1.395(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.391(4) . ? C13 C18 1.404(4) . ? C14 C15 1.389(4) . ? C14 H14 0.9500 . ? C15 C16 1.387(4) . ? C15 H15 0.9500 . ? C16 C17 1.383(4) . ? C16 H16 0.9500 . ? C17 C18 1.390(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.468(4) . ? C19 H19 0.9500 . ? C20 C25 1.385(4) . ? C20 C21 1.394(4) . ? C21 C22 1.379(4) . ? C21 H21 0.9500 . ? C22 N23 1.342(4) . ? C22 H22 0.9500 . ? N23 C24 1.333(4) . ? C24 C25 1.390(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.468(4) . ? C26 H26 0.9500 . ? C27 C32 1.390(4) . ? C27 C28 1.391(4) . ? C28 C29 1.375(4) . ? C28 H28 0.9500 . ? C29 N30 1.347(4) . ? C29 H29 0.9500 . ? N30 C31 1.337(4) . ? N30 Ag 2.337(2) 1_655 ? C31 C32 1.383(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? N33 C37 1.281(4) . ? N33 N34 1.406(3) . ? N34 C51 1.264(4) . ? N35 C38 1.282(4) . ? N35 N36 1.403(3) . ? N36 C58 1.269(4) . ? C37 C45 1.480(4) . ? C37 C38 1.516(4) . ? C38 C39 1.474(4) . ? C39 C40 1.394(4) . ? C39 C44 1.394(4) . ? C40 C41 1.387(4) . ? C40 H40 0.9500 . ? C41 C42 1.375(5) . ? C41 H41 0.9500 . ? C42 C43 1.373(5) . ? C42 H42 0.9500 . ? C43 C44 1.380(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.387(4) . ? C45 C46 1.398(4) . ? C46 C47 1.392(4) . ? C46 H46 0.9500 . ? C47 C48 1.375(4) . ? C47 H47 0.9500 . ? C48 C49 1.377(5) . ? C48 H48 0.9500 . ? C49 C50 1.388(4) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.469(4) . ? C51 H51 0.9500 . ? C52 C57 1.383(5) . ? C52 C53 1.396(4) . ? C53 C54 1.375(4) . ? C53 H53 0.9500 . ? C54 N55 1.350(4) . ? C54 H54 0.9500 . ? N55 C56 1.340(4) . ? C56 C57 1.387(4) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C59 1.472(4) . ? C58 H58 0.9500 . ? C59 C64 1.390(4) . ? C59 C60 1.394(4) . ? C60 C61 1.384(4) . ? C60 H60 0.9500 . ? C61 N62 1.343(4) . ? C61 H61 0.9500 . ? N62 C63 1.334(4) . ? N62 Ag 2.362(2) 1_465 ? C63 C64 1.384(4) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? Cl65 O68 1.427(3) . ? Cl65 O69 1.429(3) . ? Cl65 O67 1.430(2) . ? Cl65 O66 1.436(3) . ? N70 C71 1.136(5) . ? C71 C72 1.447(5) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? N73 C74 1.116(5) . ? C74 C75B 1.455(12) . ? C74 C75A 1.478(14) . ? C75A H75A 0.9800 . ? C75A H75B 0.9800 . ? C75A H75C 0.9800 . ? C75B H75D 0.9800 . ? C75B H75E 0.9800 . ? C75B H75F 0.9800 . ? C76 C77 1.436(7) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C82 1.389(6) . ? C77 C78 1.397(6) . ? C78 C79 1.394(7) . ? C78 H78 0.9500 . ? C79 C80 1.426(7) . ? C79 H79 0.9500 . ? C80 C81 1.364(7) . ? C80 H80 0.9500 . ? C81 C82 1.470(7) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? 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 N55 Ag N23 120.74(8) . . ? N55 Ag N30 108.70(9) . 1_455 ? N23 Ag N30 112.69(8) . 1_455 ? N55 Ag N62 111.56(9) . 1_645 ? N23 Ag N62 103.96(8) . 1_645 ? N30 Ag N62 96.38(8) 1_455 1_645 ? C5 N1 N2 112.5(2) . . ? C19 N2 N1 112.7(2) . . ? C6 N3 N4 111.4(2) . . ? C26 N4 N3 112.5(2) . . ? N1 C5 C7 119.2(2) . . ? N1 C5 C6 123.5(2) . . ? C7 C5 C6 117.4(2) . . ? N3 C6 C13 119.3(2) . . ? N3 C6 C5 122.6(2) . . ? C13 C6 C5 118.0(2) . . ? C12 C7 C8 119.0(2) . . ? C12 C7 C5 120.1(2) . . ? C8 C7 C5 120.9(2) . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.8(3) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C11 C10 C9 119.5(3) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 120.4(3) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C18 119.2(3) . . ? C14 C13 C6 120.5(2) . . ? C18 C13 C6 120.3(2) . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C18 C13 120.1(3) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? N2 C19 C20 120.3(3) . . ? N2 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C25 C20 C21 117.9(3) . . ? C25 C20 C19 119.7(2) . . ? C21 C20 C19 122.4(3) . . ? C22 C21 C20 119.2(3) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? N23 C22 C21 123.3(3) . . ? N23 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? C24 N23 C22 117.1(2) . . ? C24 N23 Ag 118.20(18) . . ? C22 N23 Ag 124.41(18) . . ? N23 C24 C25 123.6(3) . . ? N23 C24 H24 118.2 . . ? C25 C24 H24 118.2 . . ? C20 C25 C24 118.9(3) . . ? C20 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? N4 C26 C27 119.6(3) . . ? N4 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C32 C27 C28 118.1(3) . . ? C32 C27 C26 120.5(2) . . ? C28 C27 C26 121.3(3) . . ? C29 C28 C27 119.2(3) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? N30 C29 C28 123.2(3) . . ? N30 C29 H29 118.4 . . ? C28 C29 H29 118.4 . . ? C31 N30 C29 117.1(2) . . ? C31 N30 Ag 122.92(19) . 1_655 ? C29 N30 Ag 118.68(19) . 1_655 ? N30 C31 C32 123.5(3) . . ? N30 C31 H31 118.2 . . ? C32 C31 H31 118.2 . . ? C31 C32 C27 118.7(3) . . ? C31 C32 H32 120.6 . . ? C27 C32 H32 120.6 . . ? C37 N33 N34 112.8(2) . . ? C51 N34 N33 114.4(3) . . ? C38 N35 N36 113.9(2) . . ? C58 N36 N35 114.5(3) . . ? N33 C37 C45 119.4(2) . . ? N33 C37 C38 122.2(3) . . ? C45 C37 C38 118.3(2) . . ? N35 C38 C39 120.1(2) . . ? N35 C38 C37 121.0(2) . . ? C39 C38 C37 118.9(2) . . ? C40 C39 C44 118.5(3) . . ? C40 C39 C38 120.9(3) . . ? C44 C39 C38 120.7(3) . . ? C41 C40 C39 120.4(3) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C42 C41 C40 120.4(3) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 119.6(3) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 120.8(3) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C43 C44 C39 120.3(3) . . ? C43 C44 H44 119.8 . . ? C39 C44 H44 119.8 . . ? C50 C45 C46 119.2(3) . . ? C50 C45 C37 121.1(3) . . ? C46 C45 C37 119.6(2) . . ? C47 C46 C45 120.0(3) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C48 C47 C46 120.0(3) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 120.4(3) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C48 C49 C50 120.3(3) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C45 C50 C49 120.1(3) . . ? C45 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? N34 C51 C52 120.2(3) . . ? N34 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C57 C52 C53 118.2(3) . . ? C57 C52 C51 119.8(3) . . ? C53 C52 C51 121.8(3) . . ? C54 C53 C52 118.9(3) . . ? C54 C53 H53 120.5 . . ? C52 C53 H53 120.5 . . ? N55 C54 C53 123.4(3) . . ? N55 C54 H54 118.3 . . ? C53 C54 H54 118.3 . . ? C56 N55 C54 117.2(3) . . ? C56 N55 Ag 120.0(2) . . ? C54 N55 Ag 120.3(2) . . ? N55 C56 C57 123.1(3) . . ? N55 C56 H56 118.4 . . ? C57 C56 H56 118.4 . . ? C52 C57 C56 119.1(3) . . ? C52 C57 H57 120.4 . . ? C56 C57 H57 120.4 . . ? N36 C58 C59 119.9(3) . . ? N36 C58 H58 120.1 . . ? C59 C58 H58 120.1 . . ? C64 C59 C60 117.9(3) . . ? C64 C59 C58 119.6(3) . . ? C60 C59 C58 122.4(3) . . ? C61 C60 C59 118.6(3) . . ? C61 C60 H60 120.7 . . ? C59 C60 H60 120.7 . . ? N62 C61 C60 123.8(3) . . ? N62 C61 H61 118.1 . . ? C60 C61 H61 118.1 . . ? C63 N62 C61 117.0(3) . . ? C63 N62 Ag 118.67(19) . 1_465 ? C61 N62 Ag 120.1(2) . 1_465 ? N62 C63 C64 123.5(3) . . ? N62 C63 H63 118.3 . . ? C64 C63 H63 118.3 . . ? C63 C64 C59 119.2(3) . . ? C63 C64 H64 120.4 . . ? C59 C64 H64 120.4 . . ? O68 Cl65 O69 111.6(2) . . ? O68 Cl65 O67 110.68(18) . . ? O69 Cl65 O67 109.13(17) . . ? O68 Cl65 O66 108.51(18) . . ? O69 Cl65 O66 107.42(18) . . ? O67 Cl65 O66 109.45(18) . . ? N70 C71 C72 177.7(4) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N73 C74 C75B 163.1(7) . . ? N73 C74 C75A 170.1(6) . . ? C75B C74 C75A 26.5(5) . . ? C74 C75A H75A 109.5 . . ? C74 C75A H75B 109.5 . . ? C74 C75A H75C 109.5 . . ? C74 C75B H75D 109.5 . . ? C74 C75B H75E 109.5 . . ? H75D C75B H75E 109.5 . . ? C74 C75B H75F 109.5 . . ? H75D C75B H75F 109.5 . . ? H75E C75B H75F 109.5 . . ? C77 C76 H76A 109.5 . . ? C77 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C77 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C82 C77 C78 117.2(4) . . ? C82 C77 C76 124.0(5) . . ? C78 C77 C76 118.1(5) . . ? C79 C78 C77 121.3(5) . . ? C79 C78 H78 119.3 . . ? C77 C78 H78 119.3 . . ? C78 C79 C80 120.9(5) . . ? C78 C79 H79 119.5 . . ? C80 C79 H79 119.5 . . ? C81 C80 C79 120.1(5) . . ? C81 C80 H80 119.9 . . ? C79 C80 H80 119.9 . . ? C80 C81 C82 117.4(5) . . ? C80 C81 H81 121.3 . . ? C82 C81 H81 121.3 . . ? C77 C82 C81 122.9(4) . . ? C77 C82 H82 118.6 . . ? C81 C82 H82 118.6 . . ? 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 C5 N1 N2 C19 -141.1(3) . . . . ? C6 N3 N4 C26 175.3(3) . . . . ? N2 N1 C5 C7 -179.3(2) . . . . ? N2 N1 C5 C6 0.7(4) . . . . ? N4 N3 C6 C13 -177.5(2) . . . . ? N4 N3 C6 C5 -1.4(4) . . . . ? N1 C5 C6 N3 87.1(4) . . . . ? C7 C5 C6 N3 -92.9(3) . . . . ? N1 C5 C6 C13 -96.8(3) . . . . ? C7 C5 C6 C13 83.1(3) . . . . ? N1 C5 C7 C12 -167.9(3) . . . . ? C6 C5 C7 C12 12.1(4) . . . . ? N1 C5 C7 C8 10.8(4) . . . . ? C6 C5 C7 C8 -169.2(2) . . . . ? C12 C7 C8 C9 0.4(4) . . . . ? C5 C7 C8 C9 -178.3(2) . . . . ? C7 C8 C9 C10 -0.2(4) . . . . ? C8 C9 C10 C11 -0.1(4) . . . . ? C9 C10 C11 C12 0.1(4) . . . . ? C8 C7 C12 C11 -0.4(4) . . . . ? C5 C7 C12 C11 178.3(3) . . . . ? C10 C11 C12 C7 0.1(4) . . . . ? N3 C6 C13 C14 25.3(4) . . . . ? C5 C6 C13 C14 -150.9(3) . . . . ? N3 C6 C13 C18 -155.2(3) . . . . ? C5 C6 C13 C18 28.6(4) . . . . ? C18 C13 C14 C15 -0.4(4) . . . . ? C6 C13 C14 C15 179.1(3) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C17 0.9(5) . . . . ? C15 C16 C17 C18 -1.4(4) . . . . ? C16 C17 C18 C13 1.0(4) . . . . ? C14 C13 C18 C17 -0.1(4) . . . . ? C6 C13 C18 C17 -179.6(2) . . . . ? N1 N2 C19 C20 179.0(2) . . . . ? N2 C19 C20 C25 -168.6(3) . . . . ? N2 C19 C20 C21 11.1(4) . . . . ? C25 C20 C21 C22 1.7(4) . . . . ? C19 C20 C21 C22 -178.0(3) . . . . ? C20 C21 C22 N23 -0.2(4) . . . . ? C21 C22 N23 C24 -1.1(4) . . . . ? C21 C22 N23 Ag 173.0(2) . . . . ? N55 Ag N23 C24 -33.3(3) . . . . ? N30 Ag N23 C24 -164.1(2) 1_455 . . . ? N62 Ag N23 C24 92.7(2) 1_645 . . . ? N55 Ag N23 C22 152.6(2) . . . . ? N30 Ag N23 C22 21.8(2) 1_455 . . . ? N62 Ag N23 C22 -81.3(2) 1_645 . . . ? C22 N23 C24 C25 0.9(5) . . . . ? Ag N23 C24 C25 -173.6(3) . . . . ? C21 C20 C25 C24 -1.8(5) . . . . ? C19 C20 C25 C24 177.8(3) . . . . ? N23 C24 C25 C20 0.5(5) . . . . ? N3 N4 C26 C27 -177.3(2) . . . . ? N4 C26 C27 C32 162.4(3) . . . . ? N4 C26 C27 C28 -13.2(4) . . . . ? C32 C27 C28 C29 -2.7(4) . . . . ? C26 C27 C28 C29 173.0(3) . . . . ? C27 C28 C29 N30 -1.4(5) . . . . ? C28 C29 N30 C31 4.4(5) . . . . ? C28 C29 N30 Ag -162.9(2) . . . 1_655 ? C29 N30 C31 C32 -3.5(4) . . . . ? Ag N30 C31 C32 163.3(2) 1_655 . . . ? N30 C31 C32 C27 -0.5(5) . . . . ? C28 C27 C32 C31 3.6(4) . . . . ? C26 C27 C32 C31 -172.2(3) . . . . ? C37 N33 N34 C51 136.2(3) . . . . ? C38 N35 N36 C58 -118.8(3) . . . . ? N34 N33 C37 C45 177.9(2) . . . . ? N34 N33 C37 C38 -4.9(4) . . . . ? N36 N35 C38 C39 -179.0(2) . . . . ? N36 N35 C38 C37 2.4(4) . . . . ? N33 C37 C38 N35 91.8(4) . . . . ? C45 C37 C38 N35 -91.0(3) . . . . ? N33 C37 C38 C39 -86.9(3) . . . . ? C45 C37 C38 C39 90.4(3) . . . . ? N35 C38 C39 C40 -175.7(3) . . . . ? C37 C38 C39 C40 3.0(4) . . . . ? N35 C38 C39 C44 5.0(4) . . . . ? C37 C38 C39 C44 -176.3(3) . . . . ? C44 C39 C40 C41 -1.2(5) . . . . ? C38 C39 C40 C41 179.5(3) . . . . ? C39 C40 C41 C42 0.7(5) . . . . ? C40 C41 C42 C43 -0.2(5) . . . . ? C41 C42 C43 C44 0.2(6) . . . . ? C42 C43 C44 C39 -0.7(6) . . . . ? C40 C39 C44 C43 1.2(5) . . . . ? C38 C39 C44 C43 -179.4(3) . . . . ? N33 C37 C45 C50 14.6(4) . . . . ? C38 C37 C45 C50 -162.7(3) . . . . ? N33 C37 C45 C46 -164.9(3) . . . . ? C38 C37 C45 C46 17.8(4) . . . . ? C50 C45 C46 C47 0.4(4) . . . . ? C37 C45 C46 C47 180.0(3) . . . . ? C45 C46 C47 C48 -0.7(4) . . . . ? C46 C47 C48 C49 1.1(5) . . . . ? C47 C48 C49 C50 -1.2(5) . . . . ? C46 C45 C50 C49 -0.5(4) . . . . ? C37 C45 C50 C49 179.9(3) . . . . ? C48 C49 C50 C45 0.9(5) . . . . ? N33 N34 C51 C52 -179.4(2) . . . . ? N34 C51 C52 C57 162.3(3) . . . . ? N34 C51 C52 C53 -14.6(4) . . . . ? C57 C52 C53 C54 -1.1(4) . . . . ? C51 C52 C53 C54 175.8(3) . . . . ? C52 C53 C54 N55 -0.3(5) . . . . ? C53 C54 N55 C56 1.1(4) . . . . ? C53 C54 N55 Ag -161.0(2) . . . . ? N23 Ag N55 C56 102.0(2) . . . . ? N30 Ag N55 C56 -125.5(2) 1_455 . . . ? N62 Ag N55 C56 -20.4(2) 1_645 . . . ? N23 Ag N55 C54 -96.4(2) . . . . ? N30 Ag N55 C54 36.1(2) 1_455 . . . ? N62 Ag N55 C54 141.2(2) 1_645 . . . ? C54 N55 C56 C57 -0.5(5) . . . . ? Ag N55 C56 C57 161.6(2) . . . . ? C53 C52 C57 C56 1.7(4) . . . . ? C51 C52 C57 C56 -175.3(3) . . . . ? N55 C56 C57 C52 -0.9(5) . . . . ? N35 N36 C58 C59 -179.1(2) . . . . ? N36 C58 C59 C64 -173.6(3) . . . . ? N36 C58 C59 C60 6.1(4) . . . . ? C64 C59 C60 C61 -1.8(4) . . . . ? C58 C59 C60 C61 178.5(3) . . . . ? C59 C60 C61 N62 1.3(5) . . . . ? C60 C61 N62 C63 0.4(4) . . . . ? C60 C61 N62 Ag -156.2(2) . . . 1_465 ? C61 N62 C63 C64 -1.6(4) . . . . ? Ag N62 C63 C64 155.3(2) 1_465 . . . ? N62 C63 C64 C59 1.1(5) . . . . ? C60 C59 C64 C63 0.7(4) . . . . ? C58 C59 C64 C63 -179.6(3) . . . . ? C82 C77 C78 C79 -2.5(6) . . . . ? C76 C77 C78 C79 -172.9(4) . . . . ? C77 C78 C79 C80 0.5(6) . . . . ? C78 C79 C80 C81 -0.9(7) . . . . ? C79 C80 C81 C82 3.0(7) . . . . ? C78 C77 C82 C81 4.8(6) . . . . ? C76 C77 C82 C81 174.7(4) . . . . ? C80 C81 C82 C77 -5.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.218 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.079 #====END=========================================================== data_Compound-7 _database_code_CSD 171386 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H62 Cl2 N16 O9 Zn' _chemical_formula_weight 1335.57 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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2480(2) _cell_length_b 21.2640(4) _cell_length_c 30.5870(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.3710(13) _cell_angle_gamma 90.00 _cell_volume 6659.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 14007 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.90 _exptl_crystal_description 'chunks' _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 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 0.516 _exptl_absorpt_correction_type multi-scan _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 0.71070 _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 '0.8 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 14007 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1342 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.90 _reflns_number_total 14007 _reflns_number_gt 7297 _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^)+(0.0959P)^2^+0.8396P] 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 14007 _refine_ls_number_parameters 896 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.1645 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.2023 _refine_ls_wR_factor_gt 0.1669 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.723 _refine_ls_shift/su_mean 0.091 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 Zn Zn 1.01030(5) 0.20928(2) 0.269066(15) 0.02270(17) Uani 1 1 d . . . N1 N 0.9016(4) -0.03129(17) 0.05002(11) 0.0270(9) Uani 1 1 d . . . N2 N 0.8905(4) 0.01579(17) 0.08192(11) 0.0282(9) Uani 1 1 d . . . N3 N 0.5925(3) 0.00608(17) 0.04932(11) 0.0254(9) Uani 1 1 d . . . N4 N 0.5992(3) -0.05159(17) 0.07229(11) 0.0292(9) Uani 1 1 d . . . C5 C 0.8011(4) -0.03327(19) 0.02337(13) 0.0216(10) Uani 1 1 d . . . C6 C 0.6923(4) 0.0146(2) 0.02566(14) 0.0261(10) Uani 1 1 d . . . C7 C 0.7973(4) -0.0811(2) -0.01168(14) 0.0246(10) Uani 1 1 d . . . C8 C 0.8914(5) -0.1285(2) -0.01221(18) 0.0447(14) Uani 1 1 d . . . H8 H 0.9562 -0.1316 0.0108 0.054 Uiso 1 1 calc R . . C9 C 0.8897(5) -0.1712(2) -0.04684(19) 0.0549(16) Uani 1 1 d . . . H9 H 0.9549 -0.2029 -0.0476 0.066 Uiso 1 1 calc R . . C10 C 0.7946(5) -0.1679(2) -0.07984(17) 0.0430(13) Uani 1 1 d . . . H10 H 0.7938 -0.1973 -0.1032 0.052 Uiso 1 1 calc R . . C11 C 0.7019(5) -0.1223(2) -0.07873(15) 0.0387(12) Uani 1 1 d . . . H11 H 0.6352 -0.1204 -0.1012 0.046 Uiso 1 1 calc R . . C12 C 0.7040(4) -0.0788(2) -0.04512(14) 0.0300(11) Uani 1 1 d . . . H12 H 0.6395 -0.0467 -0.0452 0.036 Uiso 1 1 calc R . . C13 C 0.7003(4) 0.0727(2) -0.00028(13) 0.0215(10) Uani 1 1 d . . . C14 C 0.6117(4) 0.1226(2) 0.00498(14) 0.0312(11) Uani 1 1 d . . . H14 H 0.5471 0.1197 0.0263 0.037 Uiso 1 1 calc R . . C15 C 0.6190(5) 0.1756(2) -0.02082(15) 0.0360(12) Uani 1 1 d . . . H15 H 0.5585 0.2089 -0.0174 0.043 Uiso 1 1 calc R . . C16 C 0.7136(4) 0.1805(2) -0.05154(14) 0.0300(11) Uani 1 1 d . . . H16 H 0.7179 0.2172 -0.0692 0.036 Uiso 1 1 calc R . . C17 C 0.8009(4) 0.1328(2) -0.05655(14) 0.0293(11) Uani 1 1 d . . . H17 H 0.8657 0.1363 -0.0778 0.035 Uiso 1 1 calc R . . C18 C 0.7956(4) 0.0792(2) -0.03089(13) 0.0267(10) Uani 1 1 d . . . H18 H 0.8578 0.0466 -0.0343 0.032 Uiso 1 1 calc R . . C19 C 0.9890(4) 0.0172(2) 0.10840(14) 0.0287(11) Uani 1 1 d . . . H19 H 1.0600 -0.0107 0.1046 0.034 Uiso 1 1 calc R . . C20 C 0.9931(4) 0.0623(2) 0.14522(13) 0.0273(11) Uani 1 1 d . . . C21 C 1.1054(4) 0.0679(2) 0.17200(13) 0.0291(11) Uani 1 1 d . . . H21 H 1.1808 0.0436 0.1664 0.035 Uiso 1 1 calc R . . C22 C 1.1059(4) 0.1088(2) 0.20667(14) 0.0288(11) Uani 1 1 d . . . H22 H 1.1842 0.1134 0.2241 0.035 Uiso 1 1 calc R . . N23 N 1.0011(3) 0.14284(16) 0.21719(11) 0.0234(8) Uani 1 1 d . . . C24 C 0.8916(4) 0.1361(2) 0.19139(14) 0.0266(11) Uani 1 1 d . . . H24 H 0.8161 0.1594 0.1983 0.032 Uiso 1 1 calc R . . C25 C 0.8848(4) 0.0974(2) 0.15601(14) 0.0287(11) Uani 1 1 d . . . H25 H 0.8060 0.0944 0.1387 0.034 Uiso 1 1 calc R . . C26 C 0.5100(4) -0.0551(2) 0.10017(13) 0.0264(10) Uani 1 1 d . . . H26 H 0.4497 -0.0215 0.1030 0.032 Uiso 1 1 calc R . . C27 C 0.5011(4) -0.1112(2) 0.12790(13) 0.0237(10) Uani 1 1 d . . . C28 C 0.4018(4) -0.1175(2) 0.15633(14) 0.0296(11) Uani 1 1 d . . . H28 H 0.3366 -0.0858 0.1577 0.035 Uiso 1 1 calc R . . C29 C 0.3963(4) -0.1697(2) 0.18294(14) 0.0308(11) Uani 1 1 d . . . H29 H 0.3263 -0.1730 0.2022 0.037 Uiso 1 1 calc R . . N30 N 0.4844(3) -0.21549(17) 0.18286(11) 0.0244(8) Uani 1 1 d . . . C31 C 0.5816(4) -0.2097(2) 0.15442(14) 0.0275(10) Uani 1 1 d . . . H31 H 0.6448 -0.2422 0.1534 0.033 Uiso 1 1 calc R . . C32 C 0.5930(4) -0.1591(2) 0.12706(14) 0.0270(10) Uani 1 1 d . . . H32 H 0.6631 -0.1569 0.1077 0.032 Uiso 1 1 calc R . . N33 N 0.7482(4) 0.52066(17) 0.11453(11) 0.0300(9) Uani 1 1 d . . . N34 N 0.8002(4) 0.46217(18) 0.12908(12) 0.0347(10) Uani 1 1 d . . . N35 N 1.0038(3) 0.48912(16) 0.05686(11) 0.0247(8) Uani 1 1 d . . . N36 N 1.0543(4) 0.53662(17) 0.08502(11) 0.0261(9) Uani 1 1 d . . . C37 C 0.7930(4) 0.5356(2) 0.07730(13) 0.0226(10) Uani 1 1 d . . . C38 C 0.8775(4) 0.4905(2) 0.05293(13) 0.0230(10) Uani 1 1 d . . . C39 C 0.8106(4) 0.4430(2) 0.02480(13) 0.0241(10) Uani 1 1 d . . . C40 C 0.6878(4) 0.4555(2) 0.00556(14) 0.0318(12) Uani 1 1 d . . . H40 H 0.6455 0.4943 0.0112 0.038 Uiso 1 1 calc R . . C41 C 0.6273(5) 0.4114(2) -0.02175(15) 0.0378(12) Uani 1 1 d . . . H41 H 0.5436 0.4204 -0.0348 0.045 Uiso 1 1 calc R . . C42 C 0.6859(5) 0.3552(2) -0.03029(15) 0.0353(12) Uani 1 1 d . . . H42 H 0.6436 0.3257 -0.0494 0.042 Uiso 1 1 calc R . . C43 C 0.8068(5) 0.3416(2) -0.01102(16) 0.0403(13) Uani 1 1 d . . . H43 H 0.8475 0.3025 -0.0166 0.048 Uiso 1 1 calc R . . C44 C 0.8692(4) 0.3853(2) 0.01664(15) 0.0319(11) Uani 1 1 d . . . H44 H 0.9521 0.3756 0.0300 0.038 Uiso 1 1 calc R . . C45 C 0.7588(4) 0.5969(2) 0.05749(14) 0.0252(10) Uani 1 1 d . . . C46 C 0.8052(5) 0.6120(2) 0.01657(16) 0.0444(13) Uani 1 1 d . . . H46 H 0.8564 0.5825 0.0015 0.053 Uiso 1 1 calc R . . C47 C 0.7767(5) 0.6703(3) -0.00220(18) 0.0558(16) Uani 1 1 d . . . H47 H 0.8088 0.6804 -0.0300 0.067 Uiso 1 1 calc R . . C48 C 0.7016(5) 0.7136(2) 0.01943(19) 0.0501(15) Uani 1 1 d . . . H48 H 0.6839 0.7538 0.0070 0.060 Uiso 1 1 calc R . . C49 C 0.6528(5) 0.6975(2) 0.05947(16) 0.0354(12) Uani 1 1 d . . . H49 H 0.5993 0.7265 0.0742 0.042 Uiso 1 1 calc R . . C50 C 0.6812(4) 0.6396(2) 0.07834(15) 0.0324(11) Uani 1 1 d . . . H50 H 0.6470 0.6292 0.1058 0.039 Uiso 1 1 calc R . . C51 C 0.7462(5) 0.4397(2) 0.16201(15) 0.0376(12) Uani 1 1 d . . . H51 H 0.6726 0.4601 0.1735 0.045 Uiso 1 1 calc R . . C52 C 0.7982(5) 0.3817(2) 0.18236(14) 0.0340(12) Uani 1 1 d . . . C53 C 0.9148(5) 0.3559(2) 0.17032(15) 0.0405(13) Uani 1 1 d . . . H53 H 0.9609 0.3735 0.1469 0.049 Uiso 1 1 calc R . . C54 C 0.9631(5) 0.3045(2) 0.19267(15) 0.0395(13) Uani 1 1 d . . . H54 H 1.0426 0.2868 0.1836 0.047 Uiso 1 1 calc R . . N55 N 0.9054(4) 0.27774(16) 0.22650(11) 0.0269(9) Uani 1 1 d . . . C56 C 0.7903(4) 0.3018(2) 0.23742(14) 0.0294(11) Uani 1 1 d . . . H56 H 0.7456 0.2828 0.2606 0.035 Uiso 1 1 calc R . . C57 C 0.7339(5) 0.3531(2) 0.21631(15) 0.0349(12) Uani 1 1 d . . . H57 H 0.6520 0.3688 0.2249 0.042 Uiso 1 1 calc R . . C58 C 1.1697(4) 0.5241(2) 0.09934(13) 0.0254(10) Uani 1 1 d . . . H58 H 1.2091 0.4857 0.0910 0.030 Uiso 1 1 calc R . . C59 C 1.2434(4) 0.5673(2) 0.12834(13) 0.0235(10) Uani 1 1 d . . . C60 C 1.2034(4) 0.6291(2) 0.13579(13) 0.0245(10) Uani 1 1 d . . . H60 H 1.1267 0.6449 0.1211 0.029 Uiso 1 1 calc R . . C61 C 1.2743(4) 0.6669(2) 0.16406(13) 0.0237(10) Uani 1 1 d . . . H61 H 1.2446 0.7086 0.1686 0.010(10) Uiso 1 1 calc R . . N62 N 1.3856(3) 0.64753(16) 0.18608(10) 0.0216(8) Uani 1 1 d . . . C63 C 1.4247(4) 0.5887(2) 0.17866(14) 0.0247(10) Uani 1 1 d . . . H63 H 1.5018 0.5740 0.1937 0.030 Uiso 1 1 calc R . . C64 C 1.3585(4) 0.5478(2) 0.15005(14) 0.0271(11) Uani 1 1 d . . . H64 H 1.3916 0.5068 0.1453 0.033 Uiso 1 1 calc R . . Cl65 Cl 0.49830(13) 0.31712(7) 0.33631(5) 0.0531(4) Uani 1 1 d D . . O66 O 0.4158(8) 0.2749(5) 0.3591(3) 0.047(4) Uani 0.50 1 d PD A 1 O67 O 0.5948(8) 0.2842(5) 0.3167(3) 0.074(4) Uani 0.50 1 d PD A 1 O68 O 0.5636(7) 0.3548(4) 0.3715(2) 0.058(2) Uani 0.50 1 d PD A 1 O69 O 0.4197(10) 0.3529(6) 0.3091(4) 0.121(5) Uani 0.50 1 d PD A 1 O66' O 0.4251(16) 0.2777(7) 0.3607(5) 0.172(12) Uani 0.50 1 d PD A 2 O67' O 0.4567(12) 0.3072(7) 0.2885(3) 0.133(5) Uani 0.50 1 d PD A 2 O68' O 0.6308(8) 0.3044(5) 0.3377(4) 0.086(4) Uani 0.50 1 d PD A 2 O69' O 0.4689(9) 0.3824(3) 0.3432(3) 0.069(3) Uani 0.50 1 d PD A 2 Cl70 Cl 0.4952(3) 0.0811(2) 0.20494(14) 0.0889(13) Uani 0.67 1 d PD B 3 O71 O 0.4031(4) 0.1030(3) 0.23856(18) 0.131(3) Uani 1 1 d D B 3 O72 O 0.4324(4) 0.0342(2) 0.18238(14) 0.0798(14) Uani 1 1 d D B 3 O73 O 0.5248(16) 0.1306(6) 0.1731(3) 0.179(7) Uani 0.50 1 d PD B 3 O74 O 0.6088(6) 0.0708(6) 0.2275(3) 0.186(5) Uani 1 1 d D B 3 Cl70' Cl 0.4842(5) 0.0516(3) 0.22819(19) 0.0428(13) Uani 0.33 1 d P C 4 O73' O 0.5271(10) 0.0007(6) 0.2491(4) 0.105(4) Uani 0.50 1 d P C 4 O75 O 0.5663(12) 0.3019(5) 0.1138(3) 0.213(4) Uani 1 1 d . . . C76 C 0.6330(14) 0.2326(7) 0.1137(5) 0.208(7) Uani 1 1 d . . . H76A H 0.6472 0.2182 0.1443 0.250 Uiso 1 1 calc R . . H76B H 0.5720 0.2028 0.0987 0.250 Uiso 1 1 calc R . . C77 C 0.7583(16) 0.2312(6) 0.0920(4) 0.216(8) Uani 1 1 d . . . H77A H 0.7549 0.2602 0.0670 0.323 Uiso 1 1 calc R . . H77B H 0.7750 0.1884 0.0816 0.323 Uiso 1 1 calc R . . H77C H 0.8287 0.2439 0.1128 0.323 Uiso 1 1 calc R . . C78 C 0.5321(10) 0.3327(6) 0.0799(3) 0.135(4) Uani 1 1 d . . . H78A H 0.4737 0.3056 0.0615 0.162 Uiso 1 1 calc R . . H78B H 0.6112 0.3407 0.0633 0.162 Uiso 1 1 calc R . . C79 C 0.4636(8) 0.3950(5) 0.0860(3) 0.133(4) Uani 1 1 d . . . H79A H 0.3741 0.3874 0.0948 0.199 Uiso 1 1 calc R . . H79B H 0.4615 0.4185 0.0584 0.199 Uiso 1 1 calc R . . H79C H 0.5108 0.4194 0.1088 0.199 Uiso 1 1 calc R . . N80 N 0.8227(4) 0.17187(17) 0.29112(11) 0.0266(9) Uani 1 1 d . . . C81 C 0.7277(5) 0.1543(2) 0.30381(14) 0.0300(11) Uani 1 1 d . . . C82 C 0.6048(5) 0.1335(3) 0.32117(17) 0.0557(17) Uani 1 1 d . . . H82A H 0.6162 0.0917 0.3342 0.084 Uiso 1 1 calc R . . H82B H 0.5377 0.1318 0.2974 0.084 Uiso 1 1 calc R . . H82C H 0.5779 0.1632 0.3436 0.084 Uiso 1 1 calc R . . N83 N 1.2034(4) 0.23915(18) 0.24385(11) 0.0290(9) Uani 1 1 d . . . C84 C 1.2993(5) 0.2452(3) 0.22874(17) 0.0540(16) Uani 1 1 d . . . C85 C 1.4271(6) 0.2529(6) 0.2094(3) 0.141(4) Uani 1 1 d . . . H85A H 1.4779 0.2847 0.2259 0.212 Uiso 1 1 calc R . . H85B H 1.4146 0.2663 0.1789 0.212 Uiso 1 1 calc R . . H85C H 1.4740 0.2127 0.2106 0.212 Uiso 1 1 calc R . . N86 N 0.2430(10) 0.3868(4) 0.1764(3) 0.157(4) Uani 1 1 d . . . C87 C 0.2636(15) 0.4153(5) 0.2069(4) 0.171(6) Uani 1 1 d . . . C88 C 0.2669(10) 0.4512(4) 0.2441(3) 0.127(4) Uani 1 1 d . . . H88A H 0.3245 0.4874 0.2403 0.191 Uiso 1 1 calc R . . H88B H 0.3001 0.4258 0.2689 0.191 Uiso 1 1 calc R . . H88C H 0.1787 0.4660 0.2497 0.191 Uiso 1 1 calc R . . N89 N 0.5865(5) 0.4942(2) 0.24866(15) 0.0687(16) Uani 1 1 d . . . C90 C 0.6558(6) 0.4770(3) 0.27666(19) 0.0530(15) Uani 1 1 d . . . C91 C 0.7430(5) 0.4546(2) 0.31133(16) 0.0484(14) Uani 1 1 d . . . H91A H 0.7008 0.4205 0.3270 0.073 Uiso 1 1 calc R . . H91B H 0.7642 0.4891 0.3316 0.073 Uiso 1 1 calc R . . H91C H 0.8234 0.4389 0.2989 0.073 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 Zn 0.0224(3) 0.0247(3) 0.0210(3) 0.0015(2) -0.0006(2) 0.0005(2) N1 0.030(2) 0.031(2) 0.0206(19) -0.0033(17) 0.0048(18) 0.0067(17) N2 0.031(2) 0.032(2) 0.022(2) -0.0031(17) 0.0034(19) 0.0092(18) N3 0.023(2) 0.026(2) 0.027(2) 0.0073(16) 0.0025(17) 0.0034(16) N4 0.031(2) 0.023(2) 0.033(2) 0.0088(17) 0.0046(18) 0.0041(17) C5 0.023(3) 0.024(3) 0.018(2) 0.0073(18) 0.004(2) 0.0048(19) C6 0.027(3) 0.028(3) 0.023(2) 0.001(2) -0.003(2) 0.000(2) C7 0.021(2) 0.025(3) 0.028(2) 0.003(2) 0.005(2) -0.0034(19) C8 0.035(3) 0.037(3) 0.062(4) -0.011(3) -0.011(3) 0.010(2) C9 0.051(4) 0.031(3) 0.082(4) -0.022(3) -0.005(3) 0.013(3) C10 0.042(3) 0.040(3) 0.047(3) -0.014(3) 0.005(3) -0.003(3) C11 0.039(3) 0.045(3) 0.032(3) -0.004(2) -0.001(2) -0.002(3) C12 0.025(3) 0.033(3) 0.032(3) 0.001(2) 0.004(2) 0.006(2) C13 0.018(2) 0.024(3) 0.022(2) 0.0013(18) -0.0004(19) -0.0016(19) C14 0.030(3) 0.030(3) 0.034(3) 0.002(2) 0.009(2) 0.004(2) C15 0.035(3) 0.030(3) 0.044(3) 0.004(2) 0.005(2) 0.011(2) C16 0.039(3) 0.025(3) 0.025(2) 0.005(2) -0.006(2) -0.004(2) C17 0.033(3) 0.030(3) 0.025(2) -0.003(2) 0.002(2) -0.008(2) C18 0.029(3) 0.024(3) 0.027(2) 0.003(2) 0.000(2) 0.006(2) C19 0.024(3) 0.041(3) 0.022(2) -0.002(2) 0.004(2) 0.012(2) C20 0.028(3) 0.037(3) 0.018(2) 0.002(2) 0.001(2) 0.006(2) C21 0.027(3) 0.039(3) 0.021(2) 0.000(2) 0.003(2) 0.012(2) C22 0.020(2) 0.045(3) 0.021(2) 0.000(2) 0.001(2) 0.006(2) N23 0.022(2) 0.024(2) 0.0242(19) 0.0040(16) 0.0030(17) -0.0001(16) C24 0.019(3) 0.033(3) 0.027(3) -0.004(2) -0.002(2) 0.004(2) C25 0.023(3) 0.034(3) 0.029(3) -0.001(2) -0.005(2) 0.006(2) C26 0.023(3) 0.030(3) 0.026(2) 0.003(2) 0.001(2) 0.001(2) C27 0.025(3) 0.024(3) 0.021(2) -0.0041(19) -0.002(2) 0.000(2) C28 0.028(3) 0.032(3) 0.029(3) 0.005(2) 0.005(2) 0.007(2) C29 0.028(3) 0.033(3) 0.032(3) 0.003(2) 0.009(2) 0.009(2) N30 0.023(2) 0.028(2) 0.0225(19) -0.0014(16) 0.0012(16) -0.0051(17) C31 0.025(2) 0.025(3) 0.033(3) 0.000(2) 0.010(2) 0.003(2) C32 0.021(2) 0.031(3) 0.029(2) 0.003(2) 0.008(2) 0.005(2) N33 0.036(2) 0.030(2) 0.025(2) 0.0003(17) 0.0011(18) 0.0107(18) N34 0.046(3) 0.028(2) 0.031(2) 0.0043(18) 0.004(2) 0.0113(19) N35 0.026(2) 0.025(2) 0.023(2) -0.0023(16) -0.0038(17) -0.0016(17) N36 0.028(2) 0.031(2) 0.0198(19) -0.0020(16) -0.0033(17) -0.0019(17) C37 0.021(2) 0.024(3) 0.023(2) -0.0062(19) -0.001(2) -0.0009(19) C38 0.025(3) 0.023(3) 0.021(2) 0.0023(19) -0.003(2) 0.003(2) C39 0.023(3) 0.026(3) 0.024(2) -0.002(2) 0.004(2) -0.003(2) C40 0.029(3) 0.029(3) 0.036(3) -0.009(2) -0.010(2) 0.004(2) C41 0.030(3) 0.048(3) 0.035(3) -0.009(2) -0.005(2) -0.004(2) C42 0.036(3) 0.035(3) 0.035(3) -0.012(2) 0.000(2) -0.008(2) C43 0.046(3) 0.029(3) 0.046(3) -0.010(2) 0.002(3) 0.000(2) C44 0.030(3) 0.026(3) 0.039(3) 0.001(2) -0.007(2) -0.003(2) C45 0.026(3) 0.024(3) 0.025(2) 0.000(2) -0.005(2) 0.002(2) C46 0.051(3) 0.035(3) 0.048(3) 0.012(3) 0.014(3) 0.022(3) C47 0.060(4) 0.052(4) 0.056(4) 0.024(3) 0.019(3) 0.022(3) C48 0.054(4) 0.031(3) 0.067(4) 0.021(3) 0.010(3) 0.011(3) C49 0.037(3) 0.029(3) 0.039(3) -0.006(2) -0.006(2) 0.011(2) C50 0.035(3) 0.035(3) 0.026(3) -0.006(2) -0.006(2) 0.004(2) C51 0.047(3) 0.037(3) 0.029(3) 0.003(2) 0.008(2) 0.013(2) C52 0.051(3) 0.032(3) 0.019(2) 0.004(2) 0.005(2) 0.009(2) C53 0.046(3) 0.049(3) 0.027(3) 0.013(2) 0.014(2) 0.023(3) C54 0.049(3) 0.044(3) 0.027(3) 0.006(2) 0.005(2) 0.009(3) N55 0.032(2) 0.025(2) 0.023(2) -0.0009(16) -0.0018(18) 0.0001(17) C56 0.032(3) 0.026(3) 0.030(3) 0.002(2) 0.005(2) 0.002(2) C57 0.039(3) 0.027(3) 0.038(3) 0.001(2) -0.003(2) 0.008(2) C58 0.025(3) 0.025(3) 0.025(2) -0.002(2) -0.003(2) 0.003(2) C59 0.024(3) 0.031(3) 0.016(2) 0.0032(19) 0.001(2) 0.002(2) C60 0.021(2) 0.029(3) 0.023(2) 0.002(2) 0.000(2) 0.003(2) C61 0.026(3) 0.020(2) 0.026(2) -0.0020(19) 0.001(2) 0.001(2) N62 0.020(2) 0.026(2) 0.0183(18) 0.0037(15) -0.0019(16) 0.0015(16) C63 0.023(2) 0.024(3) 0.027(2) 0.005(2) -0.007(2) -0.001(2) C64 0.024(3) 0.024(3) 0.033(3) 0.001(2) -0.002(2) 0.006(2) Cl65 0.0384(8) 0.0543(9) 0.0681(10) -0.0267(8) 0.0208(8) -0.0140(7) O66 0.029(6) 0.047(8) 0.065(9) -0.013(7) 0.022(6) -0.015(5) O67 0.025(6) 0.139(10) 0.058(7) -0.055(6) 0.012(5) 0.002(6) O68 0.046(5) 0.077(6) 0.054(5) -0.034(5) 0.021(4) -0.046(4) O69 0.099(9) 0.125(11) 0.134(11) -0.006(9) -0.037(9) 0.065(8) O66' 0.21(2) 0.137(17) 0.17(2) -0.117(15) 0.126(16) -0.142(15) O67' 0.137(11) 0.196(15) 0.063(7) -0.051(8) -0.025(7) 0.000(10) O68' 0.025(6) 0.111(10) 0.121(11) 0.022(8) 0.002(6) 0.011(6) O69' 0.082(7) 0.043(5) 0.085(7) -0.014(5) 0.046(6) 0.001(5) Cl70 0.0400(19) 0.124(4) 0.102(3) -0.077(3) -0.005(2) 0.005(2) O71 0.034(3) 0.170(5) 0.186(6) -0.133(5) -0.032(3) 0.039(3) O72 0.057(3) 0.092(4) 0.089(3) -0.039(3) -0.012(2) -0.006(2) O73 0.297(19) 0.157(14) 0.078(9) 0.007(9) -0.049(11) -0.063(13) O74 0.052(5) 0.321(14) 0.184(8) -0.134(10) -0.005(5) 0.016(6) Cl70' 0.025(2) 0.047(3) 0.056(3) -0.012(2) 0.003(2) 0.007(2) O73' 0.066(7) 0.123(10) 0.127(9) -0.007(8) 0.000(6) 0.039(7) O75 0.357(13) 0.175(9) 0.115(6) 0.006(6) 0.090(7) 0.034(9) C76 0.227(14) 0.149(12) 0.259(16) -0.072(11) 0.155(13) -0.024(11) C77 0.322(19) 0.180(13) 0.132(10) 0.027(9) -0.151(13) -0.048(13) C78 0.136(8) 0.223(13) 0.046(5) 0.034(7) 0.011(5) 0.043(9) C79 0.064(5) 0.202(12) 0.135(8) -0.034(8) 0.025(5) 0.002(6) N80 0.028(2) 0.026(2) 0.026(2) -0.0012(17) -0.0033(18) 0.0039(18) C81 0.029(3) 0.036(3) 0.025(3) 0.008(2) -0.004(2) -0.003(2) C82 0.037(3) 0.084(5) 0.046(3) 0.031(3) -0.003(3) -0.017(3) N83 0.027(2) 0.036(2) 0.024(2) 0.0055(17) 0.0043(18) -0.0036(18) C84 0.037(3) 0.082(5) 0.043(3) 0.018(3) 0.008(3) -0.012(3) C85 0.040(4) 0.261(12) 0.126(7) 0.083(8) 0.043(5) -0.007(6) N86 0.227(10) 0.118(7) 0.123(7) 0.043(6) -0.015(7) -0.087(7) C87 0.325(17) 0.104(9) 0.082(7) 0.033(6) -0.013(10) -0.126(10) C88 0.173(9) 0.118(8) 0.091(6) 0.020(6) 0.022(6) -0.073(7) N89 0.102(4) 0.062(4) 0.041(3) 0.001(3) -0.005(3) 0.046(3) C90 0.074(4) 0.043(4) 0.042(3) 0.000(3) 0.004(3) 0.021(3) C91 0.054(4) 0.044(3) 0.047(3) 0.014(3) -0.001(3) 0.006(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 Zn N23 2.124(3) . ? Zn N62 2.150(3) 2_745 ? Zn N30 2.172(3) 2_655 ? Zn N55 2.203(3) . ? Zn N80 2.212(4) . ? Zn N83 2.245(4) . ? N1 C5 1.287(5) . ? N1 N2 1.406(5) . ? N2 C19 1.268(5) . ? N3 C6 1.290(5) . ? N3 N4 1.414(5) . ? N4 C26 1.278(5) . ? C5 C7 1.477(6) . ? C5 C6 1.515(6) . ? C6 C13 1.471(6) . ? C7 C12 1.371(6) . ? C7 C8 1.396(6) . ? C8 C9 1.395(7) . ? C9 C10 1.375(7) . ? C10 C11 1.358(7) . ? C11 C12 1.383(6) . ? C13 C18 1.387(6) . ? C13 C14 1.410(6) . ? C14 C15 1.380(6) . ? C15 C16 1.381(6) . ? C16 C17 1.367(6) . ? C17 C18 1.385(6) . ? C19 C20 1.478(6) . ? C20 C21 1.390(6) . ? C20 C25 1.389(6) . ? C21 C22 1.372(6) . ? C22 N23 1.345(5) . ? N23 C24 1.352(5) . ? C24 C25 1.358(6) . ? C26 C27 1.469(6) . ? C27 C28 1.372(6) . ? C27 C32 1.389(6) . ? C28 C29 1.378(6) . ? C29 N30 1.329(5) . ? N30 C31 1.355(5) . ? N30 Zn 2.172(3) 2_645 ? C31 C32 1.370(6) . ? N33 C37 1.286(5) . ? N33 N34 1.418(5) . ? N34 C51 1.263(6) . ? N35 C38 1.295(5) . ? N35 N36 1.412(5) . ? N36 C58 1.272(5) . ? C37 C45 1.473(6) . ? C37 C38 1.510(6) . ? C38 C39 1.476(6) . ? C39 C44 1.394(6) . ? C39 C40 1.393(6) . ? C40 C41 1.386(6) . ? C41 C42 1.367(6) . ? C42 C43 1.380(7) . ? C43 C44 1.393(6) . ? C45 C50 1.381(6) . ? C45 C46 1.395(6) . ? C46 C47 1.391(7) . ? C47 C48 1.386(7) . ? C48 C49 1.385(7) . ? C49 C50 1.387(6) . ? C51 C52 1.472(6) . ? C52 C53 1.379(6) . ? C52 C57 1.392(6) . ? C53 C54 1.370(6) . ? C54 N55 1.340(6) . ? N55 C56 1.341(5) . ? C56 C57 1.382(6) . ? C58 C59 1.466(6) . ? C59 C64 1.392(6) . ? C59 C60 1.398(6) . ? C60 C61 1.367(6) . ? C61 N62 1.364(5) . ? N62 C63 1.337(5) . ? N62 Zn 2.150(3) 2_755 ? C63 C64 1.390(6) . ? Cl65 O69 1.367(8) . ? Cl65 O66' 1.367(11) . ? Cl65 O67 1.369(8) . ? Cl65 O68' 1.384(8) . ? Cl65 O66 1.434(8) . ? Cl65 O69' 1.438(7) . ? Cl65 O68 1.478(6) . ? Cl65 O67' 1.521(8) . ? Cl70 O74 1.346(7) . ? Cl70 O72 1.360(5) . ? Cl70 O73 1.474(10) . ? Cl70 O71 1.499(5) . ? Cl70' O73' 1.323(12) . ? O75 C78 1.263(10) . ? O75 C76 1.623(15) . ? C76 C77 1.470(17) . ? C78 C79 1.514(13) . ? N80 C81 1.126(5) . ? C81 C82 1.455(7) . ? N83 C84 1.111(6) . ? C84 C85 1.467(8) . ? N86 C87 1.125(11) . ? C87 C88 1.369(13) . ? N89 C90 1.149(6) . ? C90 C91 1.440(7) . ? 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 N23 Zn N62 94.35(13) . 2_745 ? N23 Zn N30 174.20(13) . 2_655 ? N62 Zn N30 91.14(12) 2_745 2_655 ? N23 Zn N55 89.57(13) . . ? N62 Zn N55 176.05(13) 2_745 . ? N30 Zn N55 84.92(13) 2_655 . ? N23 Zn N80 88.64(13) . . ? N62 Zn N80 90.03(13) 2_745 . ? N30 Zn N80 93.22(13) 2_655 . ? N55 Zn N80 90.51(13) . . ? N23 Zn N83 86.79(13) . . ? N62 Zn N83 88.32(13) 2_745 . ? N30 Zn N83 91.52(13) 2_655 . ? N55 Zn N83 91.46(13) . . ? N80 Zn N83 175.01(14) . . ? C5 N1 N2 112.2(3) . . ? C19 N2 N1 112.0(3) . . ? C6 N3 N4 112.2(3) . . ? C26 N4 N3 111.2(4) . . ? N1 C5 C7 118.6(4) . . ? N1 C5 C6 121.3(4) . . ? C7 C5 C6 119.9(4) . . ? N3 C6 C13 119.0(4) . . ? N3 C6 C5 122.2(4) . . ? C13 C6 C5 118.8(4) . . ? C12 C7 C8 118.5(4) . . ? C12 C7 C5 121.0(4) . . ? C8 C7 C5 120.5(4) . . ? C9 C8 C7 119.5(5) . . ? C10 C9 C8 120.7(5) . . ? C11 C10 C9 119.6(5) . . ? C10 C11 C12 120.4(5) . . ? C7 C12 C11 121.3(4) . . ? C18 C13 C14 118.5(4) . . ? C18 C13 C6 120.3(4) . . ? C14 C13 C6 121.2(4) . . ? C15 C14 C13 119.9(4) . . ? C14 C15 C16 120.5(4) . . ? C17 C16 C15 120.0(4) . . ? C16 C17 C18 120.4(4) . . ? C17 C18 C13 120.7(4) . . ? N2 C19 C20 119.9(4) . . ? C21 C20 C25 117.6(4) . . ? C21 C20 C19 120.1(4) . . ? C25 C20 C19 122.2(4) . . ? C22 C21 C20 119.1(4) . . ? N23 C22 C21 123.3(4) . . ? C22 N23 C24 117.1(4) . . ? C22 N23 Zn 121.7(3) . . ? C24 N23 Zn 121.1(3) . . ? C25 C24 N23 122.9(4) . . ? C24 C25 C20 120.0(4) . . ? N4 C26 C27 119.7(4) . . ? C28 C27 C32 117.5(4) . . ? C28 C27 C26 120.7(4) . . ? C32 C27 C26 121.8(4) . . ? C29 C28 C27 120.1(4) . . ? N30 C29 C28 123.0(4) . . ? C29 N30 C31 116.9(4) . . ? C29 N30 Zn 122.5(3) . 2_645 ? C31 N30 Zn 120.2(3) . 2_645 ? N30 C31 C32 123.2(4) . . ? C31 C32 C27 119.3(4) . . ? C37 N33 N34 110.5(4) . . ? C51 N34 N33 114.2(4) . . ? C38 N35 N36 112.4(3) . . ? C58 N36 N35 111.8(4) . . ? N33 C37 C45 119.7(4) . . ? N33 C37 C38 120.9(4) . . ? C45 C37 C38 119.4(4) . . ? N35 C38 C39 118.5(4) . . ? N35 C38 C37 124.0(4) . . ? C39 C38 C37 117.4(4) . . ? C44 C39 C40 118.7(4) . . ? C44 C39 C38 120.9(4) . . ? C40 C39 C38 120.4(4) . . ? C41 C40 C39 120.0(4) . . ? C42 C41 C40 121.2(4) . . ? C41 C42 C43 119.7(4) . . ? C42 C43 C44 120.1(5) . . ? C43 C44 C39 120.3(4) . . ? C50 C45 C46 119.1(4) . . ? C50 C45 C37 121.6(4) . . ? C46 C45 C37 119.3(4) . . ? C45 C46 C47 120.2(5) . . ? C48 C47 C46 120.4(5) . . ? C47 C48 C49 119.1(5) . . ? C50 C49 C48 120.7(5) . . ? C49 C50 C45 120.5(5) . . ? N34 C51 C52 119.4(4) . . ? C53 C52 C57 117.9(4) . . ? C53 C52 C51 121.5(4) . . ? C57 C52 C51 120.4(4) . . ? C54 C53 C52 118.9(5) . . ? N55 C54 C53 124.2(5) . . ? C54 N55 C56 116.8(4) . . ? C54 N55 Zn 121.2(3) . . ? C56 N55 Zn 121.2(3) . . ? N55 C56 C57 122.7(4) . . ? C56 C57 C52 119.4(5) . . ? N36 C58 C59 121.7(4) . . ? C64 C59 C60 116.8(4) . . ? C64 C59 C58 120.4(4) . . ? C60 C59 C58 122.8(4) . . ? C61 C60 C59 120.2(4) . . ? N62 C61 C60 123.1(4) . . ? C63 N62 C61 116.7(3) . . ? C63 N62 Zn 122.4(3) . 2_755 ? C61 N62 Zn 120.9(3) . 2_755 ? N62 C63 C64 123.4(4) . . ? C63 C64 C59 119.7(4) . . ? O69 Cl65 O66' 110.6(10) . . ? O69 Cl65 O67 115.9(7) . . ? O66' Cl65 O67 110.3(9) . . ? O69 Cl65 O68' 132.9(7) . . ? O66' Cl65 O68' 115.0(8) . . ? O67 Cl65 O68' 35.7(4) . . ? O69 Cl65 O66 107.5(6) . . ? O66' Cl65 O66 4.1(11) . . ? O67 Cl65 O66 110.0(6) . . ? O68' Cl65 O66 117.4(6) . . ? O69 Cl65 O69' 55.2(6) . . ? O66' Cl65 O69' 113.0(7) . . ? O67 Cl65 O69' 135.8(6) . . ? O68' Cl65 O69' 113.3(6) . . ? O66 Cl65 O69' 113.7(5) . . ? O69 Cl65 O68 112.3(6) . . ? O66' Cl65 O68 100.3(8) . . ? O67 Cl65 O68 106.4(4) . . ? O68' Cl65 O68 70.7(5) . . ? O66 Cl65 O68 104.1(5) . . ? O69' Cl65 O68 57.5(5) . . ? O69 Cl65 O67' 49.9(6) . . ? O66' Cl65 O67' 107.5(7) . . ? O67 Cl65 O67' 71.8(6) . . ? O68' Cl65 O67' 103.8(6) . . ? O66 Cl65 O67' 103.5(7) . . ? O69' Cl65 O67' 102.8(6) . . ? O68 Cl65 O67' 151.0(6) . . ? O74 Cl70 O72 121.5(6) . . ? O74 Cl70 O73 104.9(7) . . ? O72 Cl70 O73 107.2(5) . . ? O74 Cl70 O71 104.7(4) . . ? O72 Cl70 O71 106.1(4) . . ? O73 Cl70 O71 112.5(7) . . ? O73' Cl70' O74 125.3(10) . . ? C78 O75 C76 124.8(10) . . ? C77 C76 O75 113.4(12) . . ? O75 C78 C79 117.9(9) . . ? C81 N80 Zn 177.2(4) . . ? N80 C81 C82 178.0(6) . . ? C84 N83 Zn 169.6(5) . . ? N83 C84 C85 179.1(7) . . ? N86 C87 C88 170.6(18) . . ? N89 C90 C91 179.0(6) . . ? 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 C5 N1 N2 C19 179.3(4) . . . . ? C6 N3 N4 C26 170.6(4) . . . . ? N2 N1 C5 C7 -179.1(3) . . . . ? N2 N1 C5 C6 4.8(5) . . . . ? N4 N3 C6 C13 -179.9(3) . . . . ? N4 N3 C6 C5 0.6(5) . . . . ? N1 C5 C6 N3 -90.3(5) . . . . ? C7 C5 C6 N3 93.6(5) . . . . ? N1 C5 C6 C13 90.2(5) . . . . ? C7 C5 C6 C13 -85.9(5) . . . . ? N1 C5 C7 C12 -169.1(4) . . . . ? C6 C5 C7 C12 7.1(6) . . . . ? N1 C5 C7 C8 8.8(6) . . . . ? C6 C5 C7 C8 -175.0(4) . . . . ? C12 C7 C8 C9 1.2(7) . . . . ? C5 C7 C8 C9 -176.8(5) . . . . ? C7 C8 C9 C10 -1.4(8) . . . . ? C8 C9 C10 C11 0.3(8) . . . . ? C9 C10 C11 C12 1.1(8) . . . . ? C8 C7 C12 C11 0.2(7) . . . . ? C5 C7 C12 C11 178.1(4) . . . . ? C10 C11 C12 C7 -1.3(7) . . . . ? N3 C6 C13 C18 -170.4(4) . . . . ? C5 C6 C13 C18 9.1(6) . . . . ? N3 C6 C13 C14 9.2(6) . . . . ? C5 C6 C13 C14 -171.3(4) . . . . ? C18 C13 C14 C15 1.7(6) . . . . ? C6 C13 C14 C15 -177.9(4) . . . . ? C13 C14 C15 C16 -0.7(7) . . . . ? C14 C15 C16 C17 -0.1(7) . . . . ? C15 C16 C17 C18 -0.1(6) . . . . ? C16 C17 C18 C13 1.1(6) . . . . ? C14 C13 C18 C17 -1.9(6) . . . . ? C6 C13 C18 C17 177.7(4) . . . . ? N1 N2 C19 C20 -177.9(4) . . . . ? N2 C19 C20 C21 -174.3(4) . . . . ? N2 C19 C20 C25 9.6(7) . . . . ? C25 C20 C21 C22 -2.1(7) . . . . ? C19 C20 C21 C22 -178.4(4) . . . . ? C20 C21 C22 N23 2.3(7) . . . . ? C21 C22 N23 C24 -1.0(6) . . . . ? C21 C22 N23 Zn -176.6(3) . . . . ? N62 Zn N23 C22 -45.4(3) 2_745 . . . ? N30 Zn N23 C22 115.9(12) 2_655 . . . ? N55 Zn N23 C22 134.1(3) . . . . ? N80 Zn N23 C22 -135.3(3) . . . . ? N83 Zn N23 C22 42.7(3) . . . . ? N62 Zn N23 C24 139.2(3) 2_745 . . . ? N30 Zn N23 C24 -59.5(14) 2_655 . . . ? N55 Zn N23 C24 -41.3(3) . . . . ? N80 Zn N23 C24 49.3(3) . . . . ? N83 Zn N23 C24 -132.8(3) . . . . ? C22 N23 C24 C25 -0.4(6) . . . . ? Zn N23 C24 C25 175.2(3) . . . . ? N23 C24 C25 C20 0.6(7) . . . . ? C21 C20 C25 C24 0.7(7) . . . . ? C19 C20 C25 C24 176.9(4) . . . . ? N3 N4 C26 C27 -179.2(3) . . . . ? N4 C26 C27 C28 -176.3(4) . . . . ? N4 C26 C27 C32 4.8(6) . . . . ? C32 C27 C28 C29 0.5(6) . . . . ? C26 C27 C28 C29 -178.4(4) . . . . ? C27 C28 C29 N30 0.3(7) . . . . ? C28 C29 N30 C31 -1.1(6) . . . . ? C28 C29 N30 Zn 171.4(3) . . . 2_645 ? C29 N30 C31 C32 1.1(6) . . . . ? Zn N30 C31 C32 -171.6(3) 2_645 . . . ? N30 C31 C32 C27 -0.3(7) . . . . ? C28 C27 C32 C31 -0.5(6) . . . . ? C26 C27 C32 C31 178.4(4) . . . . ? C37 N33 N34 C51 -169.8(4) . . . . ? C38 N35 N36 C58 159.9(4) . . . . ? N34 N33 C37 C45 -175.7(3) . . . . ? N34 N33 C37 C38 5.9(5) . . . . ? N36 N35 C38 C39 -179.4(3) . . . . ? N36 N35 C38 C37 -2.7(6) . . . . ? N33 C37 C38 N35 -91.4(5) . . . . ? C45 C37 C38 N35 90.2(5) . . . . ? N33 C37 C38 C39 85.3(5) . . . . ? C45 C37 C38 C39 -93.1(5) . . . . ? N35 C38 C39 C44 25.0(6) . . . . ? C37 C38 C39 C44 -151.9(4) . . . . ? N35 C38 C39 C40 -154.5(4) . . . . ? C37 C38 C39 C40 28.7(6) . . . . ? C44 C39 C40 C41 -1.2(7) . . . . ? C38 C39 C40 C41 178.2(4) . . . . ? C39 C40 C41 C42 0.1(7) . . . . ? C40 C41 C42 C43 0.8(7) . . . . ? C41 C42 C43 C44 -0.6(7) . . . . ? C42 C43 C44 C39 -0.5(7) . . . . ? C40 C39 C44 C43 1.4(7) . . . . ? C38 C39 C44 C43 -178.1(4) . . . . ? N33 C37 C45 C50 1.2(6) . . . . ? C38 C37 C45 C50 179.6(4) . . . . ? N33 C37 C45 C46 -178.4(4) . . . . ? C38 C37 C45 C46 0.0(6) . . . . ? C50 C45 C46 C47 2.0(7) . . . . ? C37 C45 C46 C47 -178.4(5) . . . . ? C45 C46 C47 C48 -0.3(8) . . . . ? C46 C47 C48 C49 -1.6(9) . . . . ? C47 C48 C49 C50 1.7(8) . . . . ? C48 C49 C50 C45 0.0(7) . . . . ? C46 C45 C50 C49 -1.9(7) . . . . ? C37 C45 C50 C49 178.5(4) . . . . ? N33 N34 C51 C52 -175.2(4) . . . . ? N34 C51 C52 C53 9.1(7) . . . . ? N34 C51 C52 C57 -174.6(4) . . . . ? C57 C52 C53 C54 -1.2(7) . . . . ? C51 C52 C53 C54 175.2(4) . . . . ? C52 C53 C54 N55 -1.3(8) . . . . ? C53 C54 N55 C56 3.0(7) . . . . ? C53 C54 N55 Zn -166.5(4) . . . . ? N23 Zn N55 C54 -70.7(3) . . . . ? N62 Zn N55 C54 102.9(19) 2_745 . . . ? N30 Zn N55 C54 107.5(3) 2_655 . . . ? N80 Zn N55 C54 -159.3(3) . . . . ? N83 Zn N55 C54 16.1(3) . . . . ? N23 Zn N55 C56 120.3(3) . . . . ? N62 Zn N55 C56 -66(2) 2_745 . . . ? N30 Zn N55 C56 -61.5(3) 2_655 . . . ? N80 Zn N55 C56 31.7(3) . . . . ? N83 Zn N55 C56 -152.9(3) . . . . ? C54 N55 C56 C57 -2.2(6) . . . . ? Zn N55 C56 C57 167.3(3) . . . . ? N55 C56 C57 C52 -0.2(7) . . . . ? C53 C52 C57 C56 1.9(7) . . . . ? C51 C52 C57 C56 -174.5(4) . . . . ? N35 N36 C58 C59 178.5(3) . . . . ? N36 C58 C59 C64 167.9(4) . . . . ? N36 C58 C59 C60 -12.0(6) . . . . ? C64 C59 C60 C61 -1.6(6) . . . . ? C58 C59 C60 C61 178.3(4) . . . . ? C59 C60 C61 N62 0.3(6) . . . . ? C60 C61 N62 C63 0.4(6) . . . . ? C60 C61 N62 Zn -178.9(3) . . . 2_755 ? C61 N62 C63 C64 0.3(6) . . . . ? Zn N62 C63 C64 179.6(3) 2_755 . . . ? N62 C63 C64 C59 -1.7(7) . . . . ? C60 C59 C64 C63 2.2(6) . . . . ? C58 C59 C64 C63 -177.7(4) . . . . ? C78 O75 C76 C77 60.8(18) . . . . ? C76 O75 C78 C79 176.3(10) . . . . ? N23 Zn N80 C81 173(8) . . . . ? N62 Zn N80 C81 78(8) 2_745 . . . ? N30 Zn N80 C81 -13(8) 2_655 . . . ? N55 Zn N80 C81 -98(8) . . . . ? N83 Zn N80 C81 149(7) . . . . ? Zn N80 C81 C82 21(21) . . . . ? N23 Zn N83 C84 -24(2) . . . . ? N62 Zn N83 C84 71(2) 2_745 . . . ? N30 Zn N83 C84 162(2) 2_655 . . . ? N55 Zn N83 C84 -113(2) . . . . ? N80 Zn N83 C84 0(3) . . . . ? Zn N83 C84 C85 -89(64) . . . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.757 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.085 #===============END===================================