# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_paper _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author ;Mir Wais Hosseini Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universite Louis Pasteur, F-67000 Strasbourg, France ; _publ_contact_author_email hosseini@chimie.u-strasbg.fr _publ_contact_author_fax '33 3 90 24 13 23' _publ_contact_author_phone '33 3 90 24 13 25' _publ_requested_category FM loop_ _publ_author_name _publ_author_address D.Salazar-Mendoza ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universite Louis Pasteur, F-67000 Strasbourg, France ; S.A.Baudron ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universite Louis Pasteur, F-67000 Strasbourg, France ; M.W.Hosseini ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universite Louis Pasteur, F-67000 Strasbourg, France ; _publ_section_title ; Beyond classical coordination: silver-pi interactions in metal dipyrrin complexes ; _publ_contact_author_name 'Mir Wais Hosseini' ###Material relevant to compound 4 at 173K ######## data_e540b _database_code_depnum_ccdc_archive 'CCDC 641388' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H18 N8 Zn' _chemical_formula_sum 'C34 H18 N8 Zn' _chemical_formula_weight 603.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2840 1.4300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.2112(12) _cell_length_b 8.9839(5) _cell_length_c 15.8267(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.097(2) _cell_angle_gamma 90.00 _cell_volume 2813.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2041 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 26.93 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8386 _exptl_absorpt_correction_T_max 0.9224 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8704 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3215 _reflns_number_gt 2386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+0.8545P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3215 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.01255(11) -0.0863(3) 0.10958(15) 0.0288(5) Uani 1 1 d . . . H1 H -0.0324 -0.1159 0.0907 0.035 Uiso 1 1 calc R . . C2 C 0.05871(11) -0.1371(3) 0.07034(16) 0.0302(5) Uani 1 1 d . . . H2 H 0.0500 -0.2042 0.0227 0.036 Uiso 1 1 calc R . . C3 C 0.11855(11) -0.0683(3) 0.11608(15) 0.0273(5) Uani 1 1 d . . . H3 H 0.1586 -0.0794 0.1052 0.033 Uiso 1 1 calc R . . C4 C 0.10868(10) 0.0243(2) 0.18388(14) 0.0211(4) Uani 1 1 d . . . C5 C 0.15557(10) 0.1128(2) 0.24755(14) 0.0195(4) Uani 1 1 d . . . C6 C 0.14577(10) 0.2072(2) 0.31294(14) 0.0207(4) Uani 1 1 d . . . C7 C 0.19459(11) 0.2929(3) 0.37960(14) 0.0267(5) Uani 1 1 d . . . H7 H 0.2407 0.2955 0.3905 0.032 Uiso 1 1 calc R . . C8 C 0.16158(12) 0.3719(3) 0.42545(15) 0.0297(5) Uani 1 1 d . . . H8 H 0.1808 0.4377 0.4732 0.036 Uiso 1 1 calc R . . C9 C 0.09316(12) 0.3336(3) 0.38579(15) 0.0281(5) Uani 1 1 d . . . H9 H 0.0592 0.3720 0.4037 0.034 Uiso 1 1 calc R . . C10 C 0.22653(10) 0.1099(2) 0.24754(14) 0.0221(4) Uani 1 1 d . . . C11 C 0.27787(11) 0.0418(2) 0.31768(15) 0.0261(5) Uani 1 1 d . . . H11 H 0.2685 -0.0031 0.3648 0.031 Uiso 1 1 calc R . . C12 C 0.34389(11) 0.0405(3) 0.31759(16) 0.0286(5) Uani 1 1 d . . . C13 C 0.35917(11) 0.1113(3) 0.25002(16) 0.0324(6) Uani 1 1 d . . . H13 H 0.4033 0.1129 0.2512 0.039 Uiso 1 1 calc R . . C14 C 0.30769(11) 0.1802(3) 0.18024(16) 0.0303(5) Uani 1 1 d . . . C15 C 0.24105(11) 0.1765(3) 0.17736(15) 0.0257(5) Uani 1 1 d . . . H15 H 0.2066 0.2185 0.1287 0.031 Uiso 1 1 calc R . . C16 C 0.39565(12) -0.0393(3) 0.38892(18) 0.0382(6) Uani 1 1 d . . . C17 C 0.32243(12) 0.2576(3) 0.10954(18) 0.0411(7) Uani 1 1 d . . . N1 N 0.04110(8) 0.0087(2) 0.17664(12) 0.0241(4) Uani 1 1 d . . . N2 N 0.08280(9) 0.2352(2) 0.31911(12) 0.0237(4) Uani 1 1 d . . . N3 N 0.43513(12) -0.1068(3) 0.44364(19) 0.0583(7) Uani 1 1 d . . . N4 N 0.33295(12) 0.3212(3) 0.05387(17) 0.0606(7) Uani 1 1 d . . . Zn1 Zn 0.0000 0.12452(4) 0.2500 0.02608(13) Uani 1 2 d S . . 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 0.0174(11) 0.0353(14) 0.0291(12) -0.0010(10) 0.0029(9) -0.0054(9) C2 0.0256(12) 0.0337(13) 0.0281(12) -0.0075(10) 0.0056(9) 0.0013(10) C3 0.0207(12) 0.0303(12) 0.0326(13) -0.0017(10) 0.0116(10) 0.0035(9) C4 0.0144(10) 0.0254(11) 0.0237(11) 0.0036(9) 0.0071(8) 0.0027(9) C5 0.0138(9) 0.0224(11) 0.0224(10) 0.0047(9) 0.0064(8) 0.0012(9) C6 0.0142(10) 0.0264(11) 0.0212(11) 0.0042(9) 0.0059(8) -0.0009(9) C7 0.0183(11) 0.0330(13) 0.0263(12) 0.0004(10) 0.0051(9) -0.0046(10) C8 0.0313(13) 0.0340(13) 0.0227(12) -0.0054(10) 0.0083(10) -0.0051(11) C9 0.0293(12) 0.0341(13) 0.0259(12) 0.0014(10) 0.0159(10) 0.0027(10) C10 0.0144(10) 0.0244(11) 0.0280(12) -0.0059(9) 0.0082(9) -0.0016(9) C11 0.0197(11) 0.0287(12) 0.0294(12) -0.0035(10) 0.0084(9) -0.0011(9) C12 0.0146(10) 0.0327(13) 0.0344(13) -0.0081(10) 0.0039(9) 0.0004(9) C13 0.0144(11) 0.0434(15) 0.0411(14) -0.0146(12) 0.0120(10) -0.0042(10) C14 0.0220(12) 0.0396(14) 0.0333(13) -0.0108(11) 0.0147(10) -0.0086(10) C15 0.0193(11) 0.0290(12) 0.0286(12) -0.0020(9) 0.0085(9) -0.0016(9) C16 0.0186(12) 0.0425(16) 0.0488(16) -0.0077(13) 0.0065(11) 0.0015(11) C17 0.0245(13) 0.0593(18) 0.0444(16) -0.0101(13) 0.0183(12) -0.0116(12) N1 0.0134(9) 0.0332(10) 0.0250(10) 0.0005(8) 0.0062(7) -0.0003(8) N2 0.0153(9) 0.0325(10) 0.0246(10) 0.0000(8) 0.0088(7) -0.0002(8) N3 0.0281(13) 0.0615(17) 0.0694(18) 0.0048(14) -0.0017(12) 0.0084(12) N4 0.0410(14) 0.097(2) 0.0504(15) 0.0036(15) 0.0249(12) -0.0193(15) Zn1 0.01302(19) 0.0378(2) 0.0291(2) 0.000 0.00972(15) 0.000 _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 N1 1.326(3) . ? C1 C2 1.411(3) . ? C1 H1 0.9300 . ? C2 C3 1.362(3) . ? C2 H2 0.9300 . ? C3 C4 1.431(3) . ? C3 H3 0.9300 . ? C4 C5 1.384(3) . ? C4 N1 1.403(2) . ? C5 C6 1.410(3) . ? C5 C10 1.505(3) . ? C6 N2 1.397(3) . ? C6 C7 1.411(3) . ? C7 C8 1.373(3) . ? C7 H7 0.9300 . ? C8 C9 1.401(3) . ? C8 H8 0.9300 . ? C9 N2 1.333(3) . ? C9 H9 0.9300 . ? C10 C11 1.387(3) . ? C10 C15 1.390(3) . ? C11 C12 1.401(3) . ? C11 H11 0.9300 . ? C12 C13 1.380(3) . ? C12 C16 1.450(3) . ? C13 C14 1.388(3) . ? C13 H13 0.9300 . ? C14 C15 1.398(3) . ? C14 C17 1.444(3) . ? C15 H15 0.9300 . ? C16 N3 1.139(3) . ? C17 N4 1.138(3) . ? N1 Zn1 1.9797(17) . ? N2 Zn1 1.9715(18) . ? Zn1 N2 1.9715(18) 2 ? Zn1 N1 1.9797(17) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.8(2) . . ? N1 C1 H1 124.1 . . ? C2 C1 H1 124.1 . . ? C3 C2 C1 106.3(2) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? C2 C3 C4 107.60(19) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? C5 C4 N1 124.21(18) . . ? C5 C4 C3 128.24(19) . . ? N1 C4 C3 107.54(18) . . ? C4 C5 C6 128.51(19) . . ? C4 C5 C10 116.52(18) . . ? C6 C5 C10 114.97(18) . . ? N2 C6 C5 123.86(19) . . ? N2 C6 C7 108.18(18) . . ? C5 C6 C7 127.92(19) . . ? C8 C7 C6 107.51(19) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 106.2(2) . . ? C7 C8 H8 126.9 . . ? C9 C8 H8 126.9 . . ? N2 C9 C8 111.5(2) . . ? N2 C9 H9 124.2 . . ? C8 C9 H9 124.2 . . ? C11 C10 C15 119.58(19) . . ? C11 C10 C5 120.32(19) . . ? C15 C10 C5 120.10(19) . . ? C10 C11 C12 120.0(2) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.7(2) . . ? C13 C12 C16 120.6(2) . . ? C11 C12 C16 118.7(2) . . ? C12 C13 C14 119.0(2) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C13 C14 C15 120.8(2) . . ? C13 C14 C17 120.2(2) . . ? C15 C14 C17 119.0(2) . . ? C10 C15 C14 119.7(2) . . ? C10 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? N3 C16 C12 177.4(3) . . ? N4 C17 C14 178.3(3) . . ? C1 N1 C4 106.76(18) . . ? C1 N1 Zn1 129.56(15) . . ? C4 N1 Zn1 123.52(14) . . ? C9 N2 C6 106.60(18) . . ? C9 N2 Zn1 129.34(15) . . ? C6 N2 Zn1 123.61(14) . . ? N2 Zn1 N2 119.42(11) . 2 ? N2 Zn1 N1 95.62(7) . . ? N2 Zn1 N1 115.60(7) 2 . ? N2 Zn1 N1 115.60(7) . 2 ? N2 Zn1 N1 95.62(7) 2 2 ? N1 Zn1 N1 116.60(11) . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.545 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.066 #===END ###Material relevant to compound 4(AgOTf) at 173K ## data_e824a _database_code_depnum_ccdc_archive 'CCDC 641389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H18 Ag2 F6 N8 O6 S2 Zn, 2.5(C6 H6)' _chemical_formula_sum 'C51 H33 Ag2 F6 N8 O6 S2 Zn' _chemical_formula_weight 1313.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn' 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 17.9768(4) _cell_length_b 10.3321(2) _cell_length_c 28.9049(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.9440(10) _cell_angle_gamma 90.00 _cell_volume 5135.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5861 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.44 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2612 _exptl_absorpt_coefficient_mu 1.380 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6365 _exptl_absorpt_correction_T_max 0.9598 _exptl_absorpt_process_details sadabs _exptl_special_details ; One triflate anion shows positional disorder. I It has been modeled over two sites. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48751 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 30.06 _reflns_number_total 15035 _reflns_number_gt 8847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+3.4059P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15035 _refine_ls_number_parameters 650 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1268 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8654(3) 0.7299(4) 1.18704(16) 0.0404(11) Uani 1 1 d . . . H1 H 0.8652 0.6876 1.1586 0.048 Uiso 1 1 calc R . . C2 C 0.8155(3) 0.8340(4) 1.18945(17) 0.0438(11) Uani 1 1 d . . . H2 H 0.7775 0.8708 1.1638 0.053 Uiso 1 1 calc R . . C3 C 0.8343(3) 0.8694(4) 1.23680(17) 0.0372(10) Uani 1 1 d . . . H3 H 0.8113 0.9356 1.2495 0.045 Uiso 1 1 calc R . . C4 C 0.8963(2) 0.7862(3) 1.26376(15) 0.0297(9) Uani 1 1 d . . . C5 C 0.9358(2) 0.7924(3) 1.31195(15) 0.0274(8) Uani 1 1 d . . . C6 C 1.0014(2) 0.7178(3) 1.33770(15) 0.0273(8) Uani 1 1 d . . . C7 C 1.0452(2) 0.7306(4) 1.38642(16) 0.0313(9) Uani 1 1 d . A . H7 H 1.0346 0.7860 1.4090 0.038 Uiso 1 1 calc R . . C8 C 1.1077(3) 0.6451(4) 1.39456(17) 0.0342(9) Uani 1 1 d . A . H8 H 1.1469 0.6323 1.4234 0.041 Uiso 1 1 calc R . . C9 C 1.0990(2) 0.5817(4) 1.34987(17) 0.0349(10) Uani 1 1 d . . . H9 H 1.1327 0.5185 1.3448 0.042 Uiso 1 1 calc R . . C10 C 0.9084(2) 0.8926(3) 1.34061(15) 0.0299(9) Uani 1 1 d . . . C11 C 0.8374(2) 0.8776(4) 1.34974(15) 0.0313(9) Uani 1 1 d . . . H11 H 0.8095 0.8012 1.3411 0.038 Uiso 1 1 calc R . . C12 C 0.8078(2) 0.9768(4) 1.37185(15) 0.0303(9) Uani 1 1 d . . . C13 C 0.8489(3) 1.0913(4) 1.38581(15) 0.0313(9) Uani 1 1 d . . . H13 H 0.8288 1.1579 1.4002 0.038 Uiso 1 1 calc R . . C14 C 0.9210(3) 1.1028(3) 1.37749(16) 0.0317(9) Uani 1 1 d . . . C15 C 0.9508(3) 1.0049(4) 1.35494(16) 0.0319(9) Uani 1 1 d . . . H15 H 0.9990 1.0150 1.3495 0.038 Uiso 1 1 calc R . . C16 C 0.7329(3) 0.9611(4) 1.37989(17) 0.0362(10) Uani 1 1 d . . . C17 C 0.9640(3) 1.2214(4) 1.39161(16) 0.0341(9) Uani 1 1 d . . . C18 C 0.8850(3) 0.3427(4) 1.26416(17) 0.0385(10) Uani 1 1 d . . . H18 H 0.8747 0.3821 1.2905 0.046 Uiso 1 1 calc R . . C19 C 0.8465(3) 0.2314(4) 1.24109(19) 0.0432(11) Uani 1 1 d . . . H19 H 0.8076 0.1852 1.2491 0.052 Uiso 1 1 calc R . . C20 C 0.8783(3) 0.2051(4) 1.20447(18) 0.0407(11) Uani 1 1 d . . . H20 H 0.8650 0.1369 1.1826 0.049 Uiso 1 1 calc R . . C21 C 0.9357(2) 0.3016(3) 1.20593(15) 0.0299(9) Uani 1 1 d . . . C22 C 0.9824(2) 0.3161(3) 1.17497(15) 0.0281(8) Uani 1 1 d . . . C23 C 1.0388(2) 0.4126(3) 1.17702(15) 0.0281(8) Uani 1 1 d . . . C24 C 1.0936(2) 0.4159(4) 1.15023(15) 0.0311(9) Uani 1 1 d . . . H24 H 1.0963 0.3584 1.1260 0.037 Uiso 1 1 calc R . . C25 C 1.1426(3) 0.5210(4) 1.16687(16) 0.0348(9) Uani 1 1 d . . . H25 H 1.1846 0.5472 1.1566 0.042 Uiso 1 1 calc R . . C26 C 1.1145(2) 0.5796(4) 1.20294(16) 0.0333(9) Uani 1 1 d . . . H26 H 1.1360 0.6533 1.2201 0.040 Uiso 1 1 calc R . . C27 C 0.9712(2) 0.2208(3) 1.13443(15) 0.0294(9) Uani 1 1 d . . . C28 C 0.9467(2) 0.2649(4) 1.08704(15) 0.0306(9) Uani 1 1 d . . . H28 H 0.9370 0.3526 1.0808 0.037 Uiso 1 1 calc R . . C29 C 0.9366(2) 0.1779(4) 1.04885(15) 0.0298(9) Uani 1 1 d . . . C30 C 0.9503(3) 0.0453(4) 1.05747(16) 0.0321(9) Uani 1 1 d . . . H30 H 0.9432 -0.0130 1.0320 0.038 Uiso 1 1 calc R . . C31 C 0.9745(3) 0.0037(3) 1.10492(16) 0.0323(9) Uani 1 1 d . . . C32 C 0.9857(2) 0.0900(3) 1.14363(16) 0.0309(9) Uani 1 1 d . . . H32 H 1.0027 0.0600 1.1753 0.037 Uiso 1 1 calc R . . C33 C 0.9895(3) -0.1323(4) 1.11505(16) 0.0347(10) Uani 1 1 d . . . C34 C 0.9102(3) 0.2263(4) 1.00025(17) 0.0351(10) Uani 1 1 d . . . N8 N 0.8904(3) 0.2689(4) 0.96243(15) 0.0454(10) Uani 1 1 d . . . C35 C 1.2178(4) 0.4207(5) 1.5399(4) 0.076(2) Uani 1 1 d . . . C36 C 0.7999(3) 0.6560(6) 1.01000(19) 0.0531(14) Uani 1 1 d . . . N1 N 0.9127(2) 0.6998(3) 1.23043(12) 0.0314(8) Uani 1 1 d . . . N2 N 1.0367(2) 0.6241(3) 1.31608(13) 0.0310(8) Uani 1 1 d . . . N3 N 0.6732(3) 0.9508(4) 1.38571(17) 0.0500(11) Uani 1 1 d . . . N4 N 0.9968(2) 1.3163(3) 1.40272(16) 0.0462(10) Uani 1 1 d . . . N5 N 0.9380(2) 0.3849(3) 1.24383(13) 0.0308(7) Uani 1 1 d . . . N6 N 1.0542(2) 0.5166(3) 1.20916(13) 0.0304(7) Uani 1 1 d . . . N7 N 1.0011(3) -0.2402(3) 1.12277(15) 0.0468(10) Uani 1 1 d . . . O1A O 1.1067(3) 0.5816(5) 1.5057(2) 0.0582(8) Uani 0.674(3) 1 d P A 1 O2A O 1.1845(3) 0.6045(5) 1.5864(2) 0.0582(8) Uani 0.674(3) 1 d P A 1 O3A O 0.9032(3) 0.5800(5) 1.4358(2) 0.0582(8) Uani 0.674(3) 1 d P . 1 F1A F 1.2613(4) 0.3578(7) 1.5742(3) 0.0993(13) Uani 0.674(3) 1 d P A 1 F2A F 1.1873(4) 0.3358(6) 1.5008(3) 0.0993(13) Uani 0.674(3) 1 d P A 1 F3A F 1.2658(4) 0.4924(6) 1.5197(3) 0.0993(13) Uani 0.674(3) 1 d P A 1 O1B O 1.0772(7) 0.4693(10) 1.5226(5) 0.0582(8) Uani 0.326(3) 1 d P A 2 O2B O 1.1706(7) 0.6447(11) 1.5545(5) 0.0582(8) Uani 0.326(3) 1 d P A 2 O3B O 0.8576(7) 0.5319(10) 1.3956(5) 0.0582(8) Uani 0.326(3) 1 d P . 2 F1B F 1.2108(8) 0.2909(13) 1.5483(6) 0.0993(13) Uani 0.326(3) 1 d P A 2 F3B F 1.2876(9) 0.4398(13) 1.5818(6) 0.0993(13) Uani 0.326(3) 1 d P A 2 F2B F 1.2327(10) 0.4405(15) 1.5028(7) 0.0993(13) Uani 0.326(3) 1 d P A 2 O4 O 0.93581(17) 0.5518(3) 1.03141(12) 0.0371(7) Uani 1 1 d . . . O5 O 0.9205(2) 0.7699(3) 0.99794(13) 0.0504(9) Uani 1 1 d . . . O6 O 0.8659(2) 0.5870(3) 0.94670(12) 0.0433(8) Uani 1 1 d . . . F4 F 0.8122(2) 0.7062(3) 1.05404(12) 0.0700(10) Uani 1 1 d . . . F5 F 0.7524(2) 0.7357(4) 0.97846(13) 0.0871(13) Uani 1 1 d . . . F6 F 0.7646(2) 0.5433(4) 1.00816(14) 0.0754(10) Uani 1 1 d . . . S1 S 1.14419(7) 0.51561(10) 1.55239(5) 0.0396(3) Uani 1 1 d . . . S2 S 0.89111(6) 0.64026(9) 0.99482(4) 0.0306(2) Uani 1 1 d . . . Zn3 Zn 0.98835(3) 0.55723(4) 1.250485(19) 0.03172(12) Uani 1 1 d . . . Ag1 Ag 1.06108(2) 0.59307(3) 1.085815(12) 0.03532(10) Uani 1 1 d . . . Ag2 Ag 1.02508(2) 0.51944(3) 1.429040(15) 0.04333(11) Uani 1 1 d . . . C37 C 0.1461(3) 0.9215(4) 0.3265(2) 0.088(3) Uani 1 1 d G . . H37 H 0.1532 0.8339 0.3216 0.105 Uiso 1 1 calc R . . C38 C 0.1026(3) 0.9975(6) 0.28853(17) 0.098(3) Uani 1 1 d G . . H38 H 0.0806 0.9607 0.2582 0.118 Uiso 1 1 calc R . . C39 C 0.0920(3) 1.1283(5) 0.29581(19) 0.0989(14) Uani 1 1 d G . . H39 H 0.0630 1.1792 0.2704 0.119 Uiso 1 1 calc R . . C40 C 0.1249(3) 1.1832(4) 0.3411(2) 0.0989(14) Uani 1 1 d G . . H40 H 0.1178 1.2708 0.3460 0.119 Uiso 1 1 calc R . . C41 C 0.1683(3) 1.1072(5) 0.37907(17) 0.0989(14) Uani 1 1 d G . . H41 H 0.1903 1.1439 0.4094 0.119 Uiso 1 1 calc R . . C42 C 0.1789(3) 0.9764(5) 0.3718(2) 0.0989(14) Uani 1 1 d G . . H42 H 0.2080 0.9255 0.3972 0.119 Uiso 1 1 calc R . . C43 C 0.1934(3) 0.0035(5) 0.1084(2) 0.0570(14) Uani 1 1 d . . . H43 H 0.1837 -0.0041 0.0751 0.068 Uiso 1 1 calc R . . C44 C 0.1937(3) 0.1233(5) 0.1291(2) 0.0547(14) Uani 1 1 d . . . H44 H 0.1855 0.1971 0.1099 0.066 Uiso 1 1 calc R . . C45 C 0.2062(3) 0.1341(6) 0.1779(2) 0.0597(15) Uani 1 1 d . . . H45 H 0.2058 0.2149 0.1920 0.072 Uiso 1 1 calc R . . C46 C 0.2192(4) 0.0254(8) 0.2058(2) 0.075(2) Uani 1 1 d . . . H46 H 0.2276 0.0316 0.2390 0.090 Uiso 1 1 calc R . . C47 C 0.2199(4) -0.0960(7) 0.1842(3) 0.093(3) Uani 1 1 d . . . H47 H 0.2293 -0.1706 0.2030 0.112 Uiso 1 1 calc R . . C48 C 0.2070(4) -0.1033(6) 0.1365(3) 0.082(2) Uani 1 1 d . . . H48 H 0.2074 -0.1839 0.1223 0.099 Uiso 1 1 calc R . . C49 C 1.0585(3) 0.9198(5) 1.49525(17) 0.0473(12) Uani 1 1 d . . . H49 H 1.0983 0.8659 1.4922 0.057 Uiso 1 1 calc R . . C50 C 0.9872(3) 0.8691(4) 1.49299(18) 0.0475(12) Uani 1 1 d . . . H50 H 0.9784 0.7807 1.4882 0.057 Uiso 1 1 calc R . . C51 C 0.9286(3) 0.9482(5) 1.49784(18) 0.0468(12) Uani 1 1 d . . . H51 H 0.8803 0.9133 1.4965 0.056 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 0.054(3) 0.037(2) 0.026(2) -0.0048(18) 0.006(2) -0.001(2) C2 0.052(3) 0.039(2) 0.032(3) 0.0036(19) 0.000(2) 0.005(2) C3 0.039(3) 0.0323(19) 0.039(3) -0.0009(18) 0.008(2) 0.0053(18) C4 0.033(2) 0.0244(17) 0.031(2) -0.0048(16) 0.0069(19) -0.0005(15) C5 0.028(2) 0.0215(16) 0.035(2) -0.0097(15) 0.0118(19) -0.0047(14) C6 0.030(2) 0.0239(16) 0.030(2) -0.0071(15) 0.0114(18) -0.0051(15) C7 0.034(2) 0.0269(18) 0.033(2) -0.0076(16) 0.0097(19) -0.0095(16) C8 0.031(2) 0.035(2) 0.033(2) 0.0022(18) 0.004(2) -0.0093(17) C9 0.024(2) 0.033(2) 0.045(3) -0.0021(18) 0.005(2) -0.0020(16) C10 0.034(2) 0.0261(17) 0.030(2) -0.0102(16) 0.0095(19) -0.0014(15) C11 0.036(2) 0.0262(17) 0.032(2) -0.0101(16) 0.011(2) -0.0083(16) C12 0.030(2) 0.0320(18) 0.029(2) -0.0067(16) 0.0083(18) 0.0008(16) C13 0.037(2) 0.0260(17) 0.031(2) -0.0066(16) 0.0111(19) -0.0002(16) C14 0.039(2) 0.0237(17) 0.034(2) -0.0066(16) 0.013(2) -0.0029(16) C15 0.030(2) 0.0302(18) 0.039(2) -0.0082(17) 0.015(2) -0.0042(16) C16 0.035(3) 0.034(2) 0.041(3) -0.0120(19) 0.014(2) -0.0048(18) C17 0.040(3) 0.0295(19) 0.035(2) -0.0103(17) 0.014(2) -0.0028(17) C18 0.051(3) 0.031(2) 0.036(3) 0.0000(18) 0.018(2) 0.0007(19) C19 0.052(3) 0.033(2) 0.052(3) 0.003(2) 0.027(3) -0.0024(19) C20 0.052(3) 0.0254(18) 0.045(3) -0.0029(18) 0.015(2) -0.0029(18) C21 0.036(2) 0.0232(16) 0.031(2) -0.0046(15) 0.0106(19) 0.0022(15) C22 0.034(2) 0.0224(16) 0.027(2) -0.0026(15) 0.0078(18) 0.0059(15) C23 0.029(2) 0.0248(17) 0.030(2) -0.0045(15) 0.0094(18) 0.0066(15) C24 0.032(2) 0.0328(19) 0.029(2) -0.0022(16) 0.0082(19) 0.0101(16) C25 0.028(2) 0.040(2) 0.037(2) 0.0028(19) 0.010(2) 0.0050(17) C26 0.030(2) 0.034(2) 0.034(2) -0.0064(17) 0.0060(19) -0.0033(16) C27 0.033(2) 0.0247(17) 0.030(2) -0.0068(16) 0.0087(19) 0.0021(15) C28 0.034(2) 0.0246(17) 0.034(2) -0.0045(16) 0.012(2) 0.0020(15) C29 0.032(2) 0.0292(18) 0.029(2) -0.0054(16) 0.0097(19) -0.0050(16) C30 0.036(2) 0.0308(19) 0.030(2) -0.0092(16) 0.0108(19) -0.0050(16) C31 0.037(2) 0.0239(17) 0.036(2) -0.0067(16) 0.011(2) 0.0055(16) C32 0.037(2) 0.0253(17) 0.028(2) -0.0052(16) 0.0062(19) 0.0028(16) C33 0.042(3) 0.0279(18) 0.033(2) -0.0057(17) 0.010(2) 0.0075(17) C34 0.038(3) 0.0325(19) 0.035(3) -0.0081(18) 0.011(2) -0.0065(17) N8 0.063(3) 0.0381(19) 0.033(2) -0.0063(17) 0.011(2) -0.0082(18) C35 0.036(3) 0.040(3) 0.146(8) 0.001(4) 0.018(4) 0.004(2) C36 0.051(3) 0.071(3) 0.039(3) 0.016(3) 0.017(3) 0.032(3) N1 0.038(2) 0.0298(16) 0.0259(18) -0.0078(14) 0.0081(16) -0.0005(14) N2 0.0295(19) 0.0287(15) 0.034(2) -0.0085(14) 0.0087(16) 0.0007(13) N3 0.047(3) 0.045(2) 0.064(3) -0.019(2) 0.025(2) -0.0105(19) N4 0.051(3) 0.0321(18) 0.063(3) -0.0203(18) 0.030(2) -0.0141(17) N5 0.039(2) 0.0266(15) 0.0287(19) -0.0036(13) 0.0122(17) 0.0020(14) N6 0.033(2) 0.0276(15) 0.0291(19) -0.0082(13) 0.0075(16) -0.0003(13) N7 0.063(3) 0.0332(19) 0.043(2) -0.0037(17) 0.014(2) 0.0085(18) O1A 0.0506(18) 0.0538(16) 0.066(2) -0.0059(15) 0.0112(17) -0.0008(13) O2A 0.0506(18) 0.0538(16) 0.066(2) -0.0059(15) 0.0112(17) -0.0008(13) O3A 0.0506(18) 0.0538(16) 0.066(2) -0.0059(15) 0.0112(17) -0.0008(13) F1A 0.092(3) 0.077(3) 0.142(4) 0.000(3) 0.056(3) 0.023(2) F2A 0.092(3) 0.077(3) 0.142(4) 0.000(3) 0.056(3) 0.023(2) F3A 0.092(3) 0.077(3) 0.142(4) 0.000(3) 0.056(3) 0.023(2) O1B 0.0506(18) 0.0538(16) 0.066(2) -0.0059(15) 0.0112(17) -0.0008(13) O2B 0.0506(18) 0.0538(16) 0.066(2) -0.0059(15) 0.0112(17) -0.0008(13) O3B 0.0506(18) 0.0538(16) 0.066(2) -0.0059(15) 0.0112(17) -0.0008(13) F1B 0.092(3) 0.077(3) 0.142(4) 0.000(3) 0.056(3) 0.023(2) F3B 0.092(3) 0.077(3) 0.142(4) 0.000(3) 0.056(3) 0.023(2) F2B 0.092(3) 0.077(3) 0.142(4) 0.000(3) 0.056(3) 0.023(2) O4 0.0341(17) 0.0320(14) 0.0425(19) 0.0040(13) 0.0070(15) 0.0066(12) O5 0.060(2) 0.0338(15) 0.054(2) 0.0017(15) 0.0116(19) -0.0058(15) O6 0.051(2) 0.0461(17) 0.0339(18) -0.0094(14) 0.0135(16) 0.0092(14) F4 0.085(2) 0.088(2) 0.0484(19) 0.0063(17) 0.0374(19) 0.0426(19) F5 0.071(2) 0.136(3) 0.059(2) 0.042(2) 0.026(2) 0.071(2) F6 0.047(2) 0.112(3) 0.067(2) 0.015(2) 0.0169(18) -0.0210(19) S1 0.0304(6) 0.0330(5) 0.0546(8) -0.0080(5) 0.0109(6) -0.0045(4) S2 0.0316(6) 0.0279(4) 0.0330(6) -0.0012(4) 0.0107(5) 0.0046(4) Zn3 0.0366(3) 0.0268(2) 0.0332(3) -0.00939(19) 0.0123(2) 0.00079(18) Ag1 0.0406(2) 0.03065(15) 0.03403(19) -0.00139(13) 0.00986(15) 0.00475(13) Ag2 0.0451(2) 0.03127(16) 0.0561(2) -0.00777(15) 0.01858(19) -0.01220(14) C37 0.074(5) 0.068(4) 0.150(8) 0.025(5) 0.077(6) 0.013(3) C38 0.095(6) 0.145(8) 0.065(5) -0.005(5) 0.039(5) -0.015(5) C39 0.070(3) 0.113(3) 0.122(4) 0.022(3) 0.041(3) -0.014(2) C40 0.070(3) 0.113(3) 0.122(4) 0.022(3) 0.041(3) -0.014(2) C41 0.070(3) 0.113(3) 0.122(4) 0.022(3) 0.041(3) -0.014(2) C42 0.070(3) 0.113(3) 0.122(4) 0.022(3) 0.041(3) -0.014(2) C43 0.045(3) 0.065(3) 0.057(4) -0.012(3) 0.010(3) 0.003(3) C44 0.050(3) 0.059(3) 0.056(4) 0.010(3) 0.017(3) 0.018(3) C45 0.051(4) 0.070(4) 0.055(4) -0.008(3) 0.011(3) 0.008(3) C46 0.048(4) 0.121(6) 0.049(4) 0.022(4) 0.002(3) -0.021(4) C47 0.065(5) 0.079(5) 0.104(7) 0.046(5) -0.023(4) -0.035(4) C48 0.058(4) 0.047(3) 0.115(7) -0.007(4) -0.015(4) -0.014(3) C49 0.056(3) 0.054(3) 0.031(3) -0.012(2) 0.011(2) 0.006(2) C50 0.067(4) 0.037(2) 0.036(3) -0.007(2) 0.011(3) -0.007(2) C51 0.047(3) 0.054(3) 0.039(3) -0.009(2) 0.013(2) -0.014(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 C1 N1 1.331(6) . ? C1 C2 1.416(6) . ? C1 H1 0.9300 . ? C2 C3 1.361(6) . ? C2 H2 0.9300 . ? C3 C4 1.442(6) . ? C3 H3 0.9300 . ? C4 C5 1.368(6) . ? C4 N1 1.407(5) . ? C5 C6 1.424(6) . ? C5 C10 1.496(5) . ? C6 N2 1.401(5) . ? C6 C7 1.405(6) . ? C7 C8 1.394(6) . ? C7 Ag2 2.583(4) . ? C7 H7 0.9300 . ? C8 C9 1.416(6) . ? C8 Ag2 2.397(4) . ? C8 H8 0.9300 . ? C9 N2 1.328(6) . ? C9 H9 0.9300 . ? C10 C15 1.383(5) . ? C10 C11 1.385(6) . ? C11 C12 1.392(5) . ? C11 H11 0.9300 . ? C12 C13 1.391(5) . ? C12 C16 1.442(6) . ? C13 C14 1.391(6) . ? C13 H13 0.9300 . ? C14 C15 1.392(5) . ? C14 C17 1.442(5) . ? C15 H15 0.9300 . ? C16 N3 1.138(6) . ? C17 N4 1.141(5) . ? C18 N5 1.329(5) . ? C18 C19 1.406(6) . ? C18 H18 0.9300 . ? C19 C20 1.369(6) . ? C19 H19 0.9300 . ? C20 C21 1.426(6) . ? C20 H20 0.9300 . ? C21 N5 1.385(5) . ? C21 C22 1.402(5) . ? C22 C23 1.410(5) . ? C22 C27 1.498(5) . ? C23 N6 1.394(5) . ? C23 C24 1.421(5) . ? C24 C25 1.392(6) . ? C24 Ag1 2.554(4) . ? C24 H24 0.9300 . ? C25 C26 1.419(6) . ? C25 Ag1 2.488(4) . ? C25 H25 0.9300 . ? C26 N6 1.321(5) . ? C26 H26 0.9300 . ? C27 C32 1.387(5) . ? C27 C28 1.388(6) . ? C28 C29 1.394(5) . ? C28 H28 0.9300 . ? C29 C30 1.402(6) . ? C29 C34 1.435(6) . ? C30 C31 1.381(6) . ? C30 H30 0.9300 . ? C31 C32 1.399(5) . ? C31 C33 1.445(5) . ? C32 H32 0.9300 . ? C33 N7 1.144(5) . ? C34 N8 1.135(6) . ? N8 Ag1 2.335(4) 3_767 ? C35 F2B 1.195(18) . ? C35 F1A 1.253(10) . ? C35 F1B 1.375(15) . ? C35 F3A 1.387(10) . ? C35 F2A 1.408(10) . ? C35 F3B 1.482(18) . ? C35 S1 1.767(6) . ? C36 F6 1.320(7) . ? C36 F4 1.332(6) . ? C36 F5 1.336(6) . ? C36 S2 1.824(5) . ? N1 Zn3 1.973(3) . ? N2 Zn3 1.966(4) . ? N4 Ag2 2.240(3) 1_565 ? N5 Zn3 1.981(3) . ? N6 Zn3 1.956(3) . ? N7 Ag1 2.438(4) 1_545 ? O1A S1 1.486(6) . ? O1A Ag2 2.363(6) . ? O2A S1 1.385(6) . ? O3A S1 1.410(6) 3_768 ? O3A Ag2 2.341(6) . ? O1B S1 1.347(12) . ? O2B S1 1.411(11) . ? O3B S1 1.591(13) 3_768 ? O4 S2 1.451(3) . ? O4 Ag1 2.379(3) . ? O5 S2 1.433(3) . ? O6 S2 1.440(3) . ? S1 O3A 1.410(6) 3_768 ? S1 O3B 1.591(13) 3_768 ? Ag1 N8 2.335(4) 3_767 ? Ag1 N7 2.438(4) 1_565 ? Ag2 N4 2.240(3) 1_545 ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C37 H37 0.9300 . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 C40 1.3900 . ? C39 H39 0.9300 . ? C40 C41 1.3900 . ? C40 H40 0.9300 . ? C41 C42 1.3900 . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.350(9) . ? C43 C44 1.374(7) . ? C43 H43 0.9300 . ? C44 C45 1.368(8) . ? C44 H44 0.9300 . ? C45 C46 1.362(9) . ? C45 H45 0.9300 . ? C46 C47 1.402(11) . ? C46 H46 0.9300 . ? C47 C48 1.330(11) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.369(7) . ? C49 C51 1.389(7) 3_778 ? C49 H49 0.9300 . ? C50 C51 1.372(7) . ? C50 H50 0.9300 . ? C51 C49 1.389(7) 3_778 ? C51 H51 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.8(4) . . ? N1 C1 H1 124.1 . . ? C2 C1 H1 124.1 . . ? C3 C2 C1 106.2(4) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? C2 C3 C4 108.1(4) . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? C5 C4 N1 125.2(4) . . ? C5 C4 C3 127.8(4) . . ? N1 C4 C3 106.9(4) . . ? C4 C5 C6 127.7(3) . . ? C4 C5 C10 116.0(4) . . ? C6 C5 C10 116.2(4) . . ? N2 C6 C7 108.5(4) . . ? N2 C6 C5 123.7(4) . . ? C7 C6 C5 127.6(3) . . ? C8 C7 C6 107.3(4) . . ? C8 C7 Ag2 66.5(2) . . ? C6 C7 Ag2 106.4(2) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? Ag2 C7 H7 95.6 . . ? C7 C8 C9 105.7(4) . . ? C7 C8 Ag2 81.2(2) . . ? C9 C8 Ag2 102.2(3) . . ? C7 C8 H8 127.2 . . ? C9 C8 H8 127.2 . . ? Ag2 C8 H8 87.2 . . ? N2 C9 C8 111.3(4) . . ? N2 C9 H9 124.3 . . ? C8 C9 H9 124.3 . . ? C15 C10 C11 119.6(3) . . ? C15 C10 C5 120.4(4) . . ? C11 C10 C5 119.9(3) . . ? C10 C11 C12 120.1(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 121.1(4) . . ? C13 C12 C16 119.4(3) . . ? C11 C12 C16 119.5(4) . . ? C14 C13 C12 117.8(3) . . ? C14 C13 H13 121.1 . . ? C12 C13 H13 121.1 . . ? C13 C14 C15 121.6(4) . . ? C13 C14 C17 118.2(3) . . ? C15 C14 C17 120.2(4) . . ? C10 C15 C14 119.8(4) . . ? C10 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? N3 C16 C12 178.7(6) . . ? N4 C17 C14 178.8(5) . . ? N5 C18 C19 112.1(4) . . ? N5 C18 H18 124.0 . . ? C19 C18 H18 124.0 . . ? C20 C19 C18 105.7(4) . . ? C20 C19 H19 127.2 . . ? C18 C19 H19 127.2 . . ? C19 C20 C21 107.5(4) . . ? C19 C20 H20 126.3 . . ? C21 C20 H20 126.3 . . ? N5 C21 C22 123.6(4) . . ? N5 C21 C20 108.2(4) . . ? C22 C21 C20 128.2(4) . . ? C21 C22 C23 127.2(4) . . ? C21 C22 C27 117.4(3) . . ? C23 C22 C27 115.4(3) . . ? N6 C23 C22 125.0(3) . . ? N6 C23 C24 108.0(3) . . ? C22 C23 C24 126.7(3) . . ? C25 C24 C23 107.4(3) . . ? C25 C24 Ag1 71.4(2) . . ? C23 C24 Ag1 111.5(3) . . ? C25 C24 H24 126.3 . . ? C23 C24 H24 126.3 . . ? Ag1 C24 H24 87.7 . . ? C24 C25 C26 105.2(4) . . ? C24 C25 Ag1 76.6(3) . . ? C26 C25 Ag1 109.1(3) . . ? C24 C25 H25 127.4 . . ? C26 C25 H25 127.4 . . ? Ag1 C25 H25 85.5 . . ? N6 C26 C25 111.8(4) . . ? N6 C26 H26 124.1 . . ? C25 C26 H26 124.1 . . ? C32 C27 C28 119.8(4) . . ? C32 C27 C22 121.0(4) . . ? C28 C27 C22 119.2(3) . . ? C27 C28 C29 120.0(4) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C30 121.0(4) . . ? C28 C29 C34 118.7(4) . . ? C30 C29 C34 120.4(4) . . ? C31 C30 C29 118.0(4) . . ? C31 C30 H30 121.0 . . ? C29 C30 H30 121.0 . . ? C30 C31 C32 121.7(4) . . ? C30 C31 C33 119.4(4) . . ? C32 C31 C33 118.9(4) . . ? C27 C32 C31 119.5(4) . . ? C27 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? N7 C33 C31 179.5(6) . . ? N8 C34 C29 177.5(5) . . ? C34 N8 Ag1 138.1(4) . 3_767 ? F2B C35 F1A 123.2(10) . . ? F2B C35 F1B 112.4(11) . . ? F1A C35 F1B 54.7(8) . . ? F2B C35 F3A 37.2(8) . . ? F1A C35 F3A 106.8(6) . . ? F1B C35 F3A 134.0(8) . . ? F2B C35 F2A 61.7(10) . . ? F1A C35 F2A 108.6(6) . . ? F1B C35 F2A 60.0(8) . . ? F3A C35 F2A 98.1(8) . . ? F2B C35 F3B 110.7(11) . . ? F1A C35 F3B 40.2(6) . . ? F1B C35 F3B 94.8(10) . . ? F3A C35 F3B 77.9(7) . . ? F2A C35 F3B 141.1(7) . . ? F2B C35 S1 117.7(9) . . ? F1A C35 S1 117.2(7) . . ? F1B C35 S1 113.1(7) . . ? F3A C35 S1 112.6(4) . . ? F2A C35 S1 111.7(5) . . ? F3B C35 S1 105.3(7) . . ? F6 C36 F4 109.0(4) . . ? F6 C36 F5 108.2(5) . . ? F4 C36 F5 107.9(4) . . ? F6 C36 S2 111.5(4) . . ? F4 C36 S2 110.7(4) . . ? F5 C36 S2 109.4(4) . . ? C1 N1 C4 107.0(3) . . ? C1 N1 Zn3 130.4(3) . . ? C4 N1 Zn3 122.5(3) . . ? C9 N2 C6 107.1(4) . . ? C9 N2 Zn3 129.4(3) . . ? C6 N2 Zn3 122.9(3) . . ? C17 N4 Ag2 161.5(4) . 1_565 ? C18 N5 C21 106.6(3) . . ? C18 N5 Zn3 128.2(3) . . ? C21 N5 Zn3 122.9(3) . . ? C26 N6 C23 107.5(3) . . ? C26 N6 Zn3 130.1(3) . . ? C23 N6 Zn3 122.3(3) . . ? C33 N7 Ag1 133.0(4) . 1_545 ? S1 O1A Ag2 136.1(3) . . ? S1 O3A Ag2 118.6(3) 3_768 . ? S2 O4 Ag1 125.82(17) . . ? O1B S1 O2A 150.9(5) . . ? O1B S1 O3A 54.2(6) . 3_768 ? O2A S1 O3A 121.4(4) . 3_768 ? O1B S1 O2B 126.2(7) . . ? O2A S1 O2B 40.8(5) . . ? O3A S1 O2B 150.6(5) 3_768 . ? O1B S1 O1A 59.9(6) . . ? O2A S1 O1A 110.1(3) . . ? O3A S1 O1A 113.3(3) 3_768 . ? O2B S1 O1A 70.3(6) . . ? O1B S1 O3B 103.5(7) . 3_768 ? O2A S1 O3B 71.7(5) . 3_768 ? O3A S1 O3B 51.2(5) 3_768 3_768 ? O2B S1 O3B 110.5(7) . 3_768 ? O1A S1 O3B 150.5(5) . 3_768 ? O1B S1 C35 104.8(5) . . ? O2A S1 C35 104.2(3) . . ? O3A S1 C35 101.7(3) 3_768 . ? O2B S1 C35 105.7(5) . . ? O1A S1 C35 103.7(4) . . ? O3B S1 C35 104.2(5) 3_768 . ? O5 S2 O6 115.1(2) . . ? O5 S2 O4 115.3(2) . . ? O6 S2 O4 114.51(18) . . ? O5 S2 C36 104.0(2) . . ? O6 S2 C36 102.4(2) . . ? O4 S2 C36 103.1(2) . . ? N6 Zn3 N2 119.21(14) . . ? N6 Zn3 N1 117.91(14) . . ? N2 Zn3 N1 95.40(14) . . ? N6 Zn3 N5 95.09(13) . . ? N2 Zn3 N5 118.05(14) . . ? N1 Zn3 N5 112.71(15) . . ? N8 Ag1 O4 99.29(13) 3_767 . ? N8 Ag1 N7 96.91(14) 3_767 1_565 ? O4 Ag1 N7 87.82(13) . 1_565 ? N8 Ag1 C25 121.69(15) 3_767 . ? O4 Ag1 C25 138.83(13) . . ? N7 Ag1 C25 90.75(14) 1_565 . ? N8 Ag1 C24 145.81(15) 3_767 . ? O4 Ag1 C24 108.96(12) . . ? N7 Ag1 C24 102.91(13) 1_565 . ? C25 Ag1 C24 32.02(14) . . ? N4 Ag2 O3A 98.82(17) 1_545 . ? N4 Ag2 O1A 126.21(18) 1_545 . ? O3A Ag2 O1A 100.9(2) . . ? N4 Ag2 C8 118.24(14) 1_545 . ? O3A Ag2 C8 126.73(18) . . ? O1A Ag2 C8 87.29(18) . . ? N4 Ag2 C7 132.78(15) 1_545 . ? O3A Ag2 C7 94.51(17) . . ? O1A Ag2 C7 94.75(17) . . ? C8 Ag2 C7 32.23(14) . . ? C38 C37 C42 120.0 . . ? C38 C37 H37 120.0 . . ? C42 C37 H37 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C37 120.0 . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C48 C43 C44 119.9(6) . . ? C48 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C45 C44 C43 120.1(6) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 119.4(6) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C45 C46 C47 119.7(6) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C48 C47 C46 119.4(6) . . ? C48 C47 H47 120.3 . . ? C46 C47 H47 120.3 . . ? C47 C48 C43 121.5(7) . . ? C47 C48 H48 119.2 . . ? C43 C48 H48 119.2 . . ? C50 C49 C51 119.8(5) . 3_778 ? C50 C49 H49 120.1 . . ? C51 C49 H49 120.1 3_778 . ? C49 C50 C51 120.2(4) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C50 C51 C49 120.0(5) . 3_778 ? C50 C51 H51 120.0 . . ? C49 C51 H51 120.0 3_778 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.404 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.180 #===END ###Material relevant to compound 5(AgOTf)2 at 173K ## data_e916a _database_code_depnum_ccdc_archive 'CCDC 641390' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H22 AG2 CU F6 N6 O7 S2' _chemical_formula_sum 'C34 H22 Ag2 Cu F6 N6 O7 S2' _chemical_formula_weight 1083.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6021(5) _cell_length_b 12.7762(5) _cell_length_c 13.9264(5) _cell_angle_alpha 64.995(2) _cell_angle_beta 86.600(2) _cell_angle_gamma 84.435(2) _cell_volume 1861.63(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4259 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1066 _exptl_absorpt_coefficient_mu 1.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8123 _exptl_absorpt_correction_T_max 0.9647 _exptl_absorpt_process_details sadabs _exptl_special_details ; One triflate anions shows positional disorder. It has been modeled over two positions. The hydrogen atoms of the water molecule bound to Ag2 have not been introduced but are taken into account in the formula of the compound. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30358 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8318 _reflns_number_gt 4432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1339P)^2^+4.9617P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0056(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8318 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1478 _refine_ls_R_factor_gt 0.0833 _refine_ls_wR_factor_ref 0.2666 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3543(8) 0.5166(8) 0.5286(8) 0.046(2) Uani 1 1 d . . . H1 H 0.4152 0.4619 0.5332 0.055 Uiso 1 1 calc R . . C2 C 0.3501(8) 0.5893(8) 0.5829(7) 0.046(2) Uani 1 1 d . . . H2 H 0.4057 0.5917 0.6272 0.055 Uiso 1 1 calc R . . C3 C 0.2459(8) 0.6557(8) 0.5562(7) 0.043(2) Uani 1 1 d . . . H3 H 0.2174 0.7113 0.5800 0.052 Uiso 1 1 calc R . . C4 C 0.1903(8) 0.6239(7) 0.4861(7) 0.039(2) Uani 1 1 d . . . C5 C 0.0845(8) 0.6719(7) 0.4353(7) 0.0362(19) Uani 1 1 d . . . C6 C 0.0416(7) 0.6446(7) 0.3570(7) 0.0360(19) Uani 1 1 d . . . C7 C -0.0723(8) 0.6796(8) 0.3127(8) 0.045(2) Uani 1 1 d . A . H7 H -0.1300 0.7255 0.3294 0.054 Uiso 1 1 calc R . . C8 C -0.0799(8) 0.6317(9) 0.2402(7) 0.046(2) Uani 1 1 d . A . H8 H -0.1430 0.6389 0.1990 0.056 Uiso 1 1 calc R . . C9 C 0.0294(8) 0.5696(8) 0.2426(7) 0.041(2) Uani 1 1 d . . . H9 H 0.0491 0.5296 0.2008 0.050 Uiso 1 1 calc R . . C10 C 0.0133(7) 0.7570(7) 0.4649(7) 0.0368(19) Uani 1 1 d . . . C11 C -0.0291(9) 0.7229(8) 0.5687(7) 0.046(2) Uani 1 1 d . . . H11 H -0.0078 0.6489 0.6194 0.055 Uiso 1 1 calc R . . C12 C -0.1031(8) 0.7982(8) 0.5977(7) 0.043(2) Uani 1 1 d . . . H12 H -0.1328 0.7747 0.6665 0.051 Uiso 1 1 calc R . . C13 C -0.1314(7) 0.9107(8) 0.5197(7) 0.040(2) Uani 1 1 d . . . C14 C -0.0849(8) 0.9447(8) 0.4181(7) 0.045(2) Uani 1 1 d . . . H14 H -0.1017 1.0199 0.3676 0.055 Uiso 1 1 calc R . . C15 C -0.0143(9) 0.8684(7) 0.3916(7) 0.044(2) Uani 1 1 d . . . H15 H 0.0155 0.8923 0.3228 0.052 Uiso 1 1 calc R . . C16 C -0.2075(8) 0.9876(9) 0.5485(8) 0.048(2) Uani 1 1 d . . . C17 C 0.2637(9) 0.5747(8) 0.1215(8) 0.050(2) Uani 1 1 d . . . H17 H 0.2152 0.6401 0.1134 0.060 Uiso 1 1 calc R . . C18 C 0.3198(9) 0.5537(9) 0.0360(8) 0.053(3) Uani 1 1 d . . . H18 H 0.3142 0.6020 -0.0359 0.063 Uiso 1 1 calc R . . C19 C 0.3816(9) 0.4519(9) 0.0790(8) 0.050(2) Uani 1 1 d . . . H19 H 0.4269 0.4160 0.0425 0.060 Uiso 1 1 calc R . . C20 C 0.3655(8) 0.4078(8) 0.1918(7) 0.041(2) Uani 1 1 d . . . C21 C 0.4183(8) 0.3078(7) 0.2675(7) 0.040(2) Uani 1 1 d . . . C22 C 0.4003(7) 0.2708(7) 0.3783(7) 0.0376(19) Uani 1 1 d . . . C23 C 0.4424(8) 0.1627(8) 0.4586(8) 0.045(2) Uani 1 1 d . . . H23 H 0.4883 0.1044 0.4482 0.054 Uiso 1 1 calc R . . C24 C 0.4025(7) 0.1602(8) 0.5554(8) 0.043(2) Uani 1 1 d . . . H24 H 0.4144 0.1000 0.6221 0.051 Uiso 1 1 calc R . . C25 C 0.3400(8) 0.2683(8) 0.5311(7) 0.045(2) Uani 1 1 d . . . H25 H 0.3043 0.2909 0.5816 0.054 Uiso 1 1 calc R . . C26 C 0.5011(8) 0.2334(8) 0.2333(7) 0.044(2) Uani 1 1 d . . . C27 C 0.4621(10) 0.1634(9) 0.1892(9) 0.061(3) Uani 1 1 d . . . H27 H 0.3833 0.1620 0.1811 0.074 Uiso 1 1 calc R . . C28 C 0.5430(10) 0.0960(10) 0.1577(9) 0.062(3) Uani 1 1 d . . . H28 H 0.5181 0.0488 0.1286 0.074 Uiso 1 1 calc R . . C29 C 0.6600(10) 0.0981(8) 0.1693(8) 0.053(3) Uani 1 1 d . . . C30 C 0.6974(9) 0.1666(9) 0.2147(9) 0.057(3) Uani 1 1 d . . . H30 H 0.7760 0.1672 0.2241 0.068 Uiso 1 1 calc R . . C31 C 0.6184(9) 0.2326(9) 0.2452(8) 0.053(3) Uani 1 1 d . . . H31 H 0.6440 0.2787 0.2751 0.063 Uiso 1 1 calc R . . C32 C 0.7432(10) 0.0259(9) 0.1401(9) 0.059(3) Uani 1 1 d . . . C33 C 0.5664(12) 0.7568(13) 0.1449(12) 0.078(4) Uani 1 1 d . . . C34 C -0.085(2) 0.6760(15) -0.0746(13) 0.110(3) Uani 1 1 d . . . N1 N 0.2600(6) 0.5359(6) 0.4695(6) 0.0422(18) Uani 1 1 d . . . N2 N 0.1010(7) 0.5752(6) 0.3125(6) 0.0438(18) Uani 1 1 d . . . N3 N -0.2697(8) 1.0522(7) 0.5671(7) 0.057(2) Uani 1 1 d . . . N4 N 0.2909(6) 0.4881(6) 0.2133(6) 0.0385(17) Uani 1 1 d . . . N5 N 0.3382(6) 0.3348(6) 0.4265(6) 0.0411(17) Uani 1 1 d . . . N6 N 0.8125(9) -0.0335(8) 0.1223(7) 0.062(2) Uani 1 1 d . . . O1 O 0.4372(7) 0.8344(7) 0.2581(6) 0.0676(7) Uani 1 1 d . . . O2 O 0.3475(7) 0.7893(7) 0.1299(6) 0.0676(7) Uani 1 1 d . . . O3 O 0.4294(7) 0.6315(7) 0.2914(6) 0.0676(7) Uani 1 1 d . . . O5 O 0.0096(9) 0.8526(9) -0.2036(6) 0.081(3) Uani 1 1 d . . . O7 O 0.1351(7) 0.8986(7) 0.1526(6) 0.064(2) Uani 1 1 d . A . F1 F 0.5750(9) 0.6861(10) 0.1009(9) 0.129(4) Uani 1 1 d . . . F2 F 0.5793(8) 0.8638(8) 0.0701(6) 0.101(3) Uani 1 1 d . . . F3 F 0.6534(7) 0.7294(9) 0.2150(7) 0.110(3) Uani 1 1 d . . . O4A O 0.046(2) 0.798(2) -0.0206(17) 0.086(3) Uani 0.438(8) 1 d P A 1 O6A O -0.152(2) 0.855(2) -0.0946(17) 0.086(3) Uani 0.438(8) 1 d P A 1 F4A F -0.150(3) 0.635(2) 0.018(2) 0.110(3) Uani 0.438(8) 1 d P A 1 F5A F 0.033(2) 0.6074(18) -0.0875(15) 0.110(3) Uani 0.438(8) 1 d P A 1 F6A F -0.140(3) 0.654(2) -0.1418(17) 0.110(3) Uani 0.438(8) 1 d P A 1 O4B O 0.0841(16) 0.7344(16) -0.0292(13) 0.086(3) Uani 0.562(8) 1 d P A 2 O6B O -0.0873(16) 0.8641(15) -0.0467(13) 0.086(3) Uani 0.562(8) 1 d P A 2 F4B F -0.101(2) 0.6015(17) 0.0196(17) 0.110(3) Uani 0.562(8) 1 d P A 2 F5B F -0.065(2) 0.6209(15) -0.1276(13) 0.110(3) Uani 0.562(8) 1 d P A 2 F6B F -0.1985(18) 0.7349(14) -0.1393(12) 0.110(3) Uani 0.562(8) 1 d P A 2 S1 S 0.4298(3) 0.7524(3) 0.2146(3) 0.0676(7) Uani 1 1 d . . . S2 S -0.0219(3) 0.8019(3) -0.0987(3) 0.0696(9) Uani 1 1 d . A . Cu1 Cu 0.25264(10) 0.48754(9) 0.35405(9) 0.0400(3) Uani 1 1 d . . . Ag1 Ag 0.39383(7) 0.78946(7) 0.44185(6) 0.0503(3) Uani 1 1 d . . . Ag2 Ag -0.03874(8) 0.84114(8) 0.12020(7) 0.0679(3) 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 C1 0.032(5) 0.050(5) 0.051(6) -0.018(4) -0.006(4) 0.011(4) C2 0.045(5) 0.049(5) 0.047(5) -0.025(4) -0.006(4) 0.004(4) C3 0.049(5) 0.040(5) 0.043(5) -0.022(4) 0.001(4) 0.001(4) C4 0.036(5) 0.037(5) 0.045(5) -0.019(4) 0.002(4) 0.007(4) C5 0.037(5) 0.035(4) 0.037(4) -0.017(4) 0.013(4) -0.004(4) C6 0.032(4) 0.042(5) 0.041(5) -0.025(4) 0.002(4) -0.004(4) C7 0.032(5) 0.052(5) 0.055(6) -0.029(5) 0.000(4) 0.009(4) C8 0.032(5) 0.064(6) 0.046(5) -0.027(5) 0.000(4) 0.000(4) C9 0.040(5) 0.044(5) 0.046(5) -0.024(4) -0.003(4) -0.005(4) C10 0.030(4) 0.040(5) 0.044(5) -0.023(4) 0.010(4) -0.002(4) C11 0.052(6) 0.035(5) 0.043(5) -0.013(4) 0.011(4) 0.004(4) C12 0.044(5) 0.044(5) 0.036(5) -0.016(4) 0.013(4) 0.006(4) C13 0.032(4) 0.044(5) 0.050(5) -0.026(4) 0.003(4) 0.006(4) C14 0.048(5) 0.042(5) 0.033(5) -0.007(4) 0.000(4) 0.011(4) C15 0.051(6) 0.034(5) 0.041(5) -0.013(4) 0.000(4) 0.001(4) C16 0.038(5) 0.055(6) 0.049(5) -0.023(5) -0.003(4) 0.008(4) C17 0.050(6) 0.039(5) 0.052(6) -0.013(4) 0.012(5) 0.001(4) C18 0.050(6) 0.063(6) 0.041(5) -0.020(5) -0.001(5) 0.006(5) C19 0.048(6) 0.055(6) 0.045(5) -0.021(5) 0.006(4) 0.003(5) C20 0.044(5) 0.036(5) 0.043(5) -0.016(4) 0.005(4) -0.007(4) C21 0.039(5) 0.037(5) 0.046(5) -0.021(4) 0.002(4) 0.001(4) C22 0.033(4) 0.037(5) 0.044(5) -0.018(4) -0.005(4) 0.001(4) C23 0.039(5) 0.033(5) 0.059(6) -0.016(4) 0.010(4) -0.005(4) C24 0.030(5) 0.043(5) 0.049(5) -0.013(4) 0.007(4) -0.006(4) C25 0.040(5) 0.054(6) 0.044(5) -0.024(5) 0.005(4) -0.003(4) C26 0.045(5) 0.044(5) 0.045(5) -0.022(4) 0.002(4) 0.005(4) C27 0.054(6) 0.062(7) 0.082(8) -0.046(6) 0.007(6) 0.007(5) C28 0.064(7) 0.060(7) 0.075(7) -0.045(6) -0.003(6) 0.013(6) C29 0.066(7) 0.039(5) 0.051(6) -0.020(4) 0.001(5) 0.013(5) C30 0.045(6) 0.054(6) 0.064(7) -0.022(5) -0.004(5) 0.012(5) C31 0.043(6) 0.059(6) 0.057(6) -0.029(5) -0.003(5) 0.012(5) C32 0.061(7) 0.055(6) 0.058(6) -0.027(5) -0.007(5) 0.023(5) C33 0.075(9) 0.092(10) 0.085(9) -0.057(8) -0.007(7) 0.001(8) C34 0.174(11) 0.095(6) 0.076(4) -0.043(4) 0.004(6) -0.053(6) N1 0.030(4) 0.043(4) 0.055(5) -0.022(4) -0.001(3) 0.002(3) N2 0.050(5) 0.040(4) 0.043(4) -0.019(3) 0.005(4) -0.001(4) N3 0.051(5) 0.055(5) 0.067(6) -0.029(4) 0.006(4) 0.012(4) N4 0.040(4) 0.030(4) 0.045(4) -0.017(3) 0.001(3) 0.004(3) N5 0.037(4) 0.046(4) 0.044(4) -0.024(4) 0.005(3) 0.001(3) N6 0.070(6) 0.053(5) 0.063(6) -0.028(4) -0.001(5) 0.018(5) O1 0.0614(15) 0.0855(18) 0.0627(15) -0.0378(13) 0.0007(12) -0.0062(14) O2 0.0614(15) 0.0855(18) 0.0627(15) -0.0378(13) 0.0007(12) -0.0062(14) O3 0.0614(15) 0.0855(18) 0.0627(15) -0.0378(13) 0.0007(12) -0.0062(14) O5 0.092(7) 0.098(7) 0.052(5) -0.028(5) -0.005(4) -0.013(5) O7 0.060(5) 0.063(5) 0.067(5) -0.027(4) 0.001(4) -0.003(4) F1 0.109(7) 0.161(9) 0.165(9) -0.123(8) 0.022(7) 0.015(7) F2 0.110(7) 0.114(7) 0.074(5) -0.030(5) 0.021(5) -0.040(6) F3 0.056(5) 0.158(9) 0.110(6) -0.051(6) -0.017(4) 0.009(5) O4A 0.090(8) 0.095(7) 0.075(6) -0.041(6) -0.016(5) 0.013(6) O6A 0.090(8) 0.095(7) 0.075(6) -0.041(6) -0.016(5) 0.013(6) F4A 0.174(11) 0.095(6) 0.076(4) -0.043(4) 0.004(6) -0.053(6) F5A 0.174(11) 0.095(6) 0.076(4) -0.043(4) 0.004(6) -0.053(6) F6A 0.174(11) 0.095(6) 0.076(4) -0.043(4) 0.004(6) -0.053(6) O4B 0.090(8) 0.095(7) 0.075(6) -0.041(6) -0.016(5) 0.013(6) O6B 0.090(8) 0.095(7) 0.075(6) -0.041(6) -0.016(5) 0.013(6) F4B 0.174(11) 0.095(6) 0.076(4) -0.043(4) 0.004(6) -0.053(6) F5B 0.174(11) 0.095(6) 0.076(4) -0.043(4) 0.004(6) -0.053(6) F6B 0.174(11) 0.095(6) 0.076(4) -0.043(4) 0.004(6) -0.053(6) S1 0.0614(15) 0.0855(18) 0.0627(15) -0.0378(13) 0.0007(12) -0.0062(14) S2 0.083(2) 0.0615(18) 0.0665(19) -0.0290(15) 0.0171(16) -0.0172(16) Cu1 0.0380(6) 0.0395(6) 0.0451(6) -0.0226(5) 0.0010(5) 0.0062(5) Ag1 0.0431(5) 0.0511(5) 0.0612(5) -0.0302(4) 0.0012(3) 0.0055(3) Ag2 0.0662(6) 0.0773(6) 0.0695(6) -0.0450(5) -0.0107(5) 0.0251(5) _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 N1 1.347(12) . ? C1 C2 1.422(13) . ? C1 H1 0.9300 . ? C2 C3 1.381(13) . ? C2 Ag1 2.558(10) . ? C2 H2 0.9300 . ? C3 C4 1.411(13) . ? C3 Ag1 2.519(10) . ? C3 H3 0.9300 . ? C4 C5 1.406(12) . ? C4 N1 1.412(10) . ? C5 C6 1.407(12) . ? C5 C10 1.484(11) . ? C6 N2 1.393(11) . ? C6 C7 1.440(12) . ? C7 C8 1.395(13) . ? C7 Ag2 2.637(10) . ? C7 H7 0.9300 . ? C8 C9 1.424(12) . ? C8 Ag2 2.560(10) . ? C8 H8 0.9300 . ? C9 N2 1.344(12) . ? C9 H9 0.9300 . ? C10 C15 1.376(12) . ? C10 C11 1.394(12) . ? C11 C12 1.397(11) . ? C11 H11 0.9300 . ? C12 C13 1.410(12) . ? C12 H12 0.9300 . ? C13 C14 1.384(12) . ? C13 C16 1.424(12) . ? C14 C15 1.368(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N3 1.145(12) . ? C17 N4 1.321(12) . ? C17 C18 1.435(13) . ? C17 H17 0.9300 . ? C18 C19 1.332(13) . ? C18 H18 0.9300 . ? C19 C20 1.434(13) . ? C19 H19 0.9300 . ? C20 C21 1.380(12) . ? C20 N4 1.396(11) . ? C21 C22 1.419(12) . ? C21 C26 1.485(12) . ? C22 N5 1.389(11) . ? C22 C23 1.423(12) . ? C23 C24 1.387(13) . ? C23 Ag1 2.676(10) 2_666 ? C23 H23 0.9300 . ? C24 C25 1.409(13) . ? C24 Ag1 2.515(9) 2_666 ? C24 H24 0.9300 . ? C25 N5 1.340(12) . ? C25 H25 0.9300 . ? C26 C31 1.379(14) . ? C26 C27 1.399(14) . ? C27 C28 1.389(13) . ? C27 H27 0.9300 . ? C28 C29 1.381(16) . ? C28 H28 0.9300 . ? C29 C30 1.389(15) . ? C29 C32 1.431(13) . ? C30 C31 1.356(13) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 N6 1.140(12) . ? C33 F1 1.282(15) . ? C33 F2 1.340(17) . ? C33 F3 1.362(15) . ? C33 S1 1.801(15) . ? C34 F5B 1.22(2) . ? C34 F4B 1.27(3) . ? C34 F6A 1.30(3) . ? C34 F4A 1.38(3) . ? C34 F6B 1.58(3) . ? C34 F5A 1.59(3) . ? C34 S2 1.724(16) . ? N1 Cu1 1.961(8) . ? N2 Cu1 1.969(8) . ? N3 Ag1 2.330(8) 2_576 ? N4 Cu1 1.981(7) . ? N5 Cu1 1.973(7) . ? N6 Ag2 2.246(8) 1_645 ? O1 S1 1.426(9) . ? O1 Ag1 2.406(8) . ? O2 S1 1.449(8) . ? O3 S1 1.461(9) . ? O5 S2 1.367(9) . ? O7 Ag2 2.343(8) . ? O4A S2 1.36(2) . ? O4A Ag2 2.39(2) . ? O6A S2 1.61(2) . ? O4B S2 1.556(18) . ? O6B S2 1.428(17) . ? O6B Ag2 2.314(17) . ? Ag1 N3 2.330(8) 2_576 ? Ag1 C24 2.515(9) 2_666 ? Ag1 C23 2.676(10) 2_666 ? Ag2 N6 2.246(8) 1_465 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 112.4(8) . . ? N1 C1 H1 123.8 . . ? C2 C1 H1 123.8 . . ? C3 C2 C1 105.5(8) . . ? C3 C2 Ag1 72.7(6) . . ? C1 C2 Ag1 105.5(6) . . ? C3 C2 H2 127.3 . . ? C1 C2 H2 127.3 . . ? Ag1 C2 H2 91.4 . . ? C2 C3 C4 107.7(8) . . ? C2 C3 Ag1 75.8(6) . . ? C4 C3 Ag1 104.5(6) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? Ag1 C3 H3 89.8 . . ? C5 C4 C3 127.6(8) . . ? C5 C4 N1 122.9(8) . . ? C3 C4 N1 109.5(8) . . ? C4 C5 C6 124.0(8) . . ? C4 C5 C10 118.5(8) . . ? C6 C5 C10 117.5(8) . . ? N2 C6 C5 125.4(8) . . ? N2 C6 C7 108.8(7) . . ? C5 C6 C7 125.8(8) . . ? C8 C7 C6 107.1(7) . . ? C8 C7 Ag2 71.4(6) . . ? C6 C7 Ag2 104.7(6) . . ? C8 C7 H7 126.5 . . ? C6 C7 H7 126.5 . . ? Ag2 C7 H7 93.1 . . ? C7 C8 C9 105.3(8) . . ? C7 C8 Ag2 77.5(6) . . ? C9 C8 Ag2 102.8(6) . . ? C7 C8 H8 127.3 . . ? C9 C8 H8 127.3 . . ? Ag2 C8 H8 89.7 . . ? N2 C9 C8 112.2(8) . . ? N2 C9 H9 123.9 . . ? C8 C9 H9 123.9 . . ? C15 C10 C11 119.1(8) . . ? C15 C10 C5 121.4(8) . . ? C11 C10 C5 119.5(8) . . ? C10 C11 C12 121.1(8) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 118.0(8) . . ? C11 C12 H12 121.0 . . ? C13 C12 H12 121.0 . . ? C14 C13 C12 120.1(7) . . ? C14 C13 C16 121.5(8) . . ? C12 C13 C16 118.4(8) . . ? C15 C14 C13 120.5(8) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C10 121.1(9) . . ? C14 C15 H15 119.5 . . ? C10 C15 H15 119.5 . . ? N3 C16 C13 177.0(11) . . ? N4 C17 C18 110.4(8) . . ? N4 C17 H17 124.8 . . ? C18 C17 H17 124.8 . . ? C19 C18 C17 107.0(9) . . ? C19 C18 H18 126.5 . . ? C17 C18 H18 126.5 . . ? C18 C19 C20 107.7(9) . . ? C18 C19 H19 126.2 . . ? C20 C19 H19 126.2 . . ? C21 C20 N4 125.0(8) . . ? C21 C20 C19 127.3(8) . . ? N4 C20 C19 107.7(8) . . ? C20 C21 C22 124.1(8) . . ? C20 C21 C26 119.3(8) . . ? C22 C21 C26 116.6(8) . . ? N5 C22 C21 125.4(8) . . ? N5 C22 C23 108.5(8) . . ? C21 C22 C23 126.1(8) . . ? C24 C23 C22 107.4(8) . . ? C24 C23 Ag1 68.2(6) . 2_666 ? C22 C23 Ag1 106.1(6) . 2_666 ? C24 C23 H23 126.3 . . ? C22 C23 H23 126.3 . . ? Ag1 C23 H23 94.6 2_666 . ? C23 C24 C25 105.4(8) . . ? C23 C24 Ag1 81.0(5) . 2_666 ? C25 C24 Ag1 101.1(6) . 2_666 ? C23 C24 H24 127.3 . . ? C25 C24 H24 127.3 . . ? Ag1 C24 H24 88.3 2_666 . ? N5 C25 C24 112.1(8) . . ? N5 C25 H25 124.0 . . ? C24 C25 H25 124.0 . . ? C31 C26 C27 119.2(9) . . ? C31 C26 C21 119.8(9) . . ? C27 C26 C21 121.0(9) . . ? C28 C27 C26 118.8(11) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C29 C28 C27 120.7(11) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 119.8(9) . . ? C28 C29 C32 120.7(10) . . ? C30 C29 C32 119.4(11) . . ? C31 C30 C29 119.4(11) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C26 122.0(11) . . ? C30 C31 H31 119.0 . . ? C26 C31 H31 119.0 . . ? N6 C32 C29 176.0(12) . . ? F1 C33 F2 108.7(12) . . ? F1 C33 F3 109.6(12) . . ? F2 C33 F3 107.6(12) . . ? F1 C33 S1 111.8(11) . . ? F2 C33 S1 110.5(10) . . ? F3 C33 S1 108.7(10) . . ? F5B C34 F4B 105.7(18) . . ? F5B C34 F6A 43.0(15) . . ? F4B C34 F6A 111.2(19) . . ? F5B C34 F4A 122.0(18) . . ? F4B C34 F4A 29.3(17) . . ? F6A C34 F4A 105(2) . . ? F5B C34 F6B 89.7(16) . . ? F4B C34 F6B 115(2) . . ? F6A C34 F6B 47.7(15) . . ? F4A C34 F6B 89.7(19) . . ? F5B C34 F5A 51.0(14) . . ? F4B C34 F5A 92.1(18) . . ? F6A C34 F5A 94.0(19) . . ? F4A C34 F5A 121.3(19) . . ? F6B C34 F5A 138.1(14) . . ? F5B C34 S2 123.7(17) . . ? F4B C34 S2 120.6(15) . . ? F6A C34 S2 126.9(16) . . ? F4A C34 S2 113.8(15) . . ? F6B C34 S2 97.1(12) . . ? F5A C34 S2 94.9(13) . . ? C1 N1 C4 105.0(8) . . ? C1 N1 Cu1 124.1(6) . . ? C4 N1 Cu1 128.1(6) . . ? C9 N2 C6 106.6(7) . . ? C9 N2 Cu1 125.9(6) . . ? C6 N2 Cu1 127.2(6) . . ? C16 N3 Ag1 165.3(8) . 2_576 ? C17 N4 C20 107.3(7) . . ? C17 N4 Cu1 125.1(6) . . ? C20 N4 Cu1 126.9(6) . . ? C25 N5 C22 106.5(7) . . ? C25 N5 Cu1 126.9(6) . . ? C22 N5 Cu1 126.4(6) . . ? C32 N6 Ag2 168.4(9) . 1_645 ? S1 O1 Ag1 122.3(5) . . ? S2 O4A Ag2 120.0(14) . . ? S2 O6B Ag2 120.9(10) . . ? O1 S1 O2 113.9(5) . . ? O1 S1 O3 115.6(5) . . ? O2 S1 O3 115.7(5) . . ? O1 S1 C33 103.4(6) . . ? O2 S1 C33 102.2(6) . . ? O3 S1 C33 103.4(6) . . ? O4A S2 O5 122.7(11) . . ? O4A S2 O6B 73.6(12) . . ? O5 S2 O6B 122.5(8) . . ? O4A S2 O4B 36.6(10) . . ? O5 S2 O4B 111.1(8) . . ? O6B S2 O4B 108.1(10) . . ? O4A S2 O6A 113.8(13) . . ? O5 S2 O6A 104.2(9) . . ? O6B S2 O6A 41.1(9) . . ? O4B S2 O6A 143.5(10) . . ? O4A S2 C34 115.8(12) . . ? O5 S2 C34 108.5(7) . . ? O6B S2 C34 110.1(10) . . ? O4B S2 C34 92.4(10) . . ? O6A S2 C34 85.2(12) . . ? N1 Cu1 N2 90.7(3) . . ? N1 Cu1 N5 96.2(3) . . ? N2 Cu1 N5 147.1(3) . . ? N1 Cu1 N4 156.4(3) . . ? N2 Cu1 N4 94.9(3) . . ? N5 Cu1 N4 91.5(3) . . ? N3 Ag1 O1 102.7(3) 2_576 . ? N3 Ag1 C24 107.5(3) 2_576 2_666 ? O1 Ag1 C24 84.5(3) . 2_666 ? N3 Ag1 C3 89.5(3) 2_576 . ? O1 Ag1 C3 125.9(3) . . ? C24 Ag1 C3 141.6(3) 2_666 . ? N3 Ag1 C2 117.8(3) 2_576 . ? O1 Ag1 C2 125.0(3) . . ? C24 Ag1 C2 114.0(3) 2_666 . ? C3 Ag1 C2 31.6(3) . . ? N3 Ag1 C23 93.4(3) 2_576 2_666 ? O1 Ag1 C23 114.6(3) . 2_666 ? C24 Ag1 C23 30.8(3) 2_666 2_666 ? C3 Ag1 C23 117.1(3) . 2_666 ? C2 Ag1 C23 99.4(3) . 2_666 ? N6 Ag2 O6B 91.0(5) 1_465 . ? N6 Ag2 O7 110.3(3) 1_465 . ? O6B Ag2 O7 122.5(5) . . ? N6 Ag2 O4A 131.1(6) 1_465 . ? O6B Ag2 O4A 41.6(7) . . ? O7 Ag2 O4A 92.8(6) . . ? N6 Ag2 C8 111.6(3) 1_465 . ? O6B Ag2 C8 103.9(5) . . ? O7 Ag2 C8 115.0(3) . . ? O4A Ag2 C8 94.8(6) . . ? N6 Ag2 C7 97.3(3) 1_465 . ? O6B Ag2 C7 133.4(5) . . ? O7 Ag2 C7 97.2(3) . . ? O4A Ag2 C7 122.5(6) . . ? C8 Ag2 C7 31.1(3) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.585 _refine_diff_density_min -1.387 _refine_diff_density_rms 0.183 #===END ###Material relevant to compound 7(AgOTf) at 173K ## data_e902b _database_code_depnum_ccdc_archive 'CCDC 641391' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H11 Ag Cu F9 N3 O5 S, 1.5(C6 H6)' _chemical_formula_sum 'C31 H20 Ag Cu F9 N3 O5 S' _chemical_formula_weight 888.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.5627(6) _cell_length_b 12.7625(4) _cell_length_c 15.5101(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.838(2) _cell_angle_gamma 90.00 _cell_volume 3309.37(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5187 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 24.82 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5426 _exptl_absorpt_correction_T_max 0.9464 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29318 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7557 _reflns_number_gt 4836 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1085P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7557 _refine_ls_number_parameters 430 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1790 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3425(3) 0.6976(4) 0.1496(3) 0.0294(10) Uani 1 1 d . . . H1 H 0.3841 0.7389 0.1848 0.035 Uiso 1 1 calc R . . C2 C 0.2830(3) 0.6508(4) 0.1815(4) 0.0355(12) Uani 1 1 d . . . H2 H 0.2785 0.6558 0.2396 0.043 Uiso 1 1 calc R . . C3 C 0.2334(3) 0.5967(4) 0.1096(4) 0.0356(12) Uani 1 1 d . . . H3 H 0.1887 0.5576 0.1096 0.043 Uiso 1 1 calc R . . C4 C 0.2633(3) 0.6119(4) 0.0349(3) 0.0286(10) Uani 1 1 d . . . C5 C 0.2343(3) 0.5676(3) -0.0519(3) 0.0272(10) Uani 1 1 d . . . C6 C 0.2692(3) 0.5796(3) -0.1209(3) 0.0267(10) Uani 1 1 d . . . C7 C 0.2470(3) 0.5279(4) -0.2061(3) 0.0290(10) Uani 1 1 d . . . H7 H 0.2028 0.4844 -0.2290 0.035 Uiso 1 1 calc R . . C8 C 0.3031(3) 0.5539(4) -0.2490(3) 0.0321(11) Uani 1 1 d . . . H8 H 0.3049 0.5313 -0.3053 0.039 Uiso 1 1 calc R . . C9 C 0.3571(3) 0.6229(4) -0.1879(3) 0.0277(10) Uani 1 1 d . . . H9 H 0.4015 0.6529 -0.1988 0.033 Uiso 1 1 calc R . . C10 C 0.1628(4) 0.4968(5) -0.0707(6) 0.0764(11) Uani 1 1 d . . . C11 C 0.1701(4) 0.3988(5) -0.0411(6) 0.0764(11) Uani 1 1 d . . . H11 H 0.2203 0.3752 -0.0067 0.092 Uiso 1 1 calc R . . C12 C 0.1058(4) 0.3298(5) -0.0594(6) 0.0764(11) Uani 1 1 d . . . H12 H 0.1135 0.2612 -0.0383 0.092 Uiso 1 1 calc R . . C13 C 0.0338(4) 0.3619(5) -0.1068(6) 0.0764(11) Uani 1 1 d . . . C14 C 0.0253(4) 0.4614(5) -0.1418(6) 0.0764(11) Uani 1 1 d . . . H14 H -0.0244 0.4844 -0.1782 0.092 Uiso 1 1 calc R . . C15 C 0.0909(4) 0.5275(5) -0.1227(6) 0.0764(11) Uani 1 1 d . . . H15 H 0.0846 0.5948 -0.1468 0.092 Uiso 1 1 calc R . . C16 C -0.0332(4) 0.2913(5) -0.1271(5) 0.0484(15) Uani 1 1 d . . . C17 C 0.5686(4) 0.8993(5) 0.1922(4) 0.0485(15) Uani 1 1 d . . . C18 C 0.5236(3) 0.8578(4) 0.0979(3) 0.0334(11) Uani 1 1 d . . . C19 C 0.5561(3) 0.8789(4) 0.0293(4) 0.0410(13) Uani 1 1 d . . . H19 H 0.6005 0.9227 0.0405 0.049 Uiso 1 1 calc R . . C20 C 0.5235(3) 0.8354(4) -0.0565(4) 0.0344(12) Uani 1 1 d . . . C21 C 0.5691(4) 0.8516(5) -0.1246(4) 0.0478(15) Uani 1 1 d . . . C22 C 0.1961(4) 1.0119(5) -0.1200(4) 0.0480(15) Uani 1 1 d . . . N1 N 0.3311(2) 0.6748(3) 0.0621(3) 0.0270(9) Uani 1 1 d . . . N2 N 0.3367(2) 0.6393(3) -0.1136(3) 0.0260(8) Uani 1 1 d . . . N3 N -0.0851(3) 0.2352(4) -0.1418(4) 0.0564(14) Uani 1 1 d . . . O1 O 0.4634(2) 0.8032(3) 0.0946(2) 0.0327(8) Uani 1 1 d . . . O2 O 0.4622(2) 0.7796(3) -0.0839(2) 0.0330(8) Uani 1 1 d . . . O3 O 0.3106(2) 0.8831(3) -0.0554(3) 0.0460(10) Uani 1 1 d . . . O4 O 0.2071(3) 0.8954(4) 0.0166(3) 0.0660(14) Uani 1 1 d . . . O5 O 0.1795(3) 0.8129(4) -0.1295(4) 0.0716(15) Uani 1 1 d . . . F1 F 0.5256(2) 0.8967(3) 0.2477(2) 0.0677(11) Uani 1 1 d . . . F2 F 0.6342(2) 0.8439(4) 0.2290(3) 0.0761(13) Uani 1 1 d . . . F3 F 0.5921(3) 0.9990(3) 0.1881(3) 0.0781(13) Uani 1 1 d . . . F4 F 0.5965(3) 0.9506(3) -0.1211(3) 0.0842(15) Uani 1 1 d . . . F5 F 0.6335(2) 0.7895(4) -0.1047(3) 0.0798(13) Uani 1 1 d . . . F6 F 0.5263(2) 0.8323(3) -0.2086(2) 0.0576(10) Uani 1 1 d . . . F7 F 0.2360(3) 1.0905(3) -0.0693(3) 0.0832(14) Uani 1 1 d . . . F8 F 0.1190(2) 1.0307(3) -0.1329(3) 0.0637(11) Uani 1 1 d . . . F9 F 0.2084(3) 1.0164(4) -0.1998(3) 0.0982(18) Uani 1 1 d . . . S1 S 0.22679(8) 0.88563(10) -0.06541(9) 0.0374(3) Uani 1 1 d . . . Cu1 Cu 0.39302(3) 0.73008(4) -0.01272(4) 0.02631(17) Uani 1 1 d . . . Ag1 Ag 0.20829(2) 0.82354(3) 0.16351(3) 0.04085(16) Uani 1 1 d . . . C23 C 0.1102(5) 0.1001(5) 0.0896(5) 0.064(2) Uani 1 1 d D . . H23 H 0.1185 0.0417 0.0578 0.077 Uiso 1 1 calc R . . C24 C 0.1725(5) 0.1659(7) 0.1314(6) 0.076(2) Uani 1 1 d . . . H24 H 0.2233 0.1532 0.1272 0.091 Uiso 1 1 calc R . . C25 C 0.1589(5) 0.2513(6) 0.1796(6) 0.084(3) Uani 1 1 d . . . H25 H 0.2002 0.2975 0.2070 0.101 Uiso 1 1 calc R . . C26 C 0.0854(6) 0.2667(7) 0.1865(6) 0.088(3) Uani 1 1 d . . . H26 H 0.0770 0.3220 0.2216 0.106 Uiso 1 1 calc R . . C27 C 0.0240(5) 0.2049(7) 0.1446(6) 0.080(2) Uani 1 1 d . . . H27 H -0.0266 0.2187 0.1490 0.096 Uiso 1 1 calc R . . C28 C 0.0355(5) 0.1220(6) 0.0957(5) 0.072(2) Uani 1 1 d D . . H28 H -0.0075 0.0796 0.0660 0.087 Uiso 1 1 calc R . . C29 C 0.5544(5) 0.5755(6) 0.0442(6) 0.076(2) Uani 1 1 d . . . H29 H 0.5912 0.6257 0.0747 0.091 Uiso 1 1 calc R . . C30 C 0.4984(6) 0.5366(6) 0.0817(5) 0.074(3) Uani 1 1 d . . . H30 H 0.4972 0.5624 0.1374 0.089 Uiso 1 1 calc R . . C31 C 0.4449(6) 0.4615(7) 0.0397(6) 0.077(2) Uani 1 1 d . . . H31 H 0.4084 0.4353 0.0668 0.092 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 0.034(3) 0.032(2) 0.025(3) -0.003(2) 0.013(2) 0.000(2) C2 0.045(3) 0.038(3) 0.029(3) 0.002(2) 0.020(2) -0.004(2) C3 0.044(3) 0.032(2) 0.037(3) 0.003(2) 0.022(2) -0.007(2) C4 0.031(2) 0.025(2) 0.034(3) 0.001(2) 0.016(2) -0.0006(19) C5 0.027(2) 0.023(2) 0.033(3) 0.001(2) 0.012(2) 0.0013(18) C6 0.030(2) 0.023(2) 0.024(2) -0.0026(19) 0.006(2) -0.0019(19) C7 0.032(3) 0.028(2) 0.026(3) -0.003(2) 0.007(2) 0.000(2) C8 0.037(3) 0.031(2) 0.029(3) 0.002(2) 0.011(2) 0.008(2) C9 0.032(2) 0.029(2) 0.024(2) 0.0033(19) 0.009(2) 0.005(2) C10 0.0391(14) 0.0447(14) 0.128(3) 0.0270(16) -0.0004(16) -0.0085(12) C11 0.0391(14) 0.0447(14) 0.128(3) 0.0270(16) -0.0004(16) -0.0085(12) C12 0.0391(14) 0.0447(14) 0.128(3) 0.0270(16) -0.0004(16) -0.0085(12) C13 0.0391(14) 0.0447(14) 0.128(3) 0.0270(16) -0.0004(16) -0.0085(12) C14 0.0391(14) 0.0447(14) 0.128(3) 0.0270(16) -0.0004(16) -0.0085(12) C15 0.0391(14) 0.0447(14) 0.128(3) 0.0270(16) -0.0004(16) -0.0085(12) C16 0.040(3) 0.044(3) 0.063(4) 0.004(3) 0.018(3) -0.006(3) C17 0.052(4) 0.053(3) 0.041(4) -0.005(3) 0.014(3) -0.020(3) C18 0.038(3) 0.034(2) 0.030(3) -0.001(2) 0.013(2) -0.005(2) C19 0.043(3) 0.048(3) 0.034(3) -0.003(2) 0.015(2) -0.024(3) C20 0.037(3) 0.035(3) 0.036(3) 0.002(2) 0.019(2) -0.004(2) C21 0.046(3) 0.058(4) 0.045(4) -0.006(3) 0.024(3) -0.021(3) C22 0.048(3) 0.053(3) 0.051(4) 0.020(3) 0.026(3) 0.024(3) N1 0.033(2) 0.0249(19) 0.027(2) -0.0005(16) 0.0140(17) -0.0007(16) N2 0.029(2) 0.0269(18) 0.024(2) 0.0032(16) 0.0115(16) 0.0008(16) N3 0.035(3) 0.059(3) 0.073(4) 0.003(3) 0.013(3) -0.012(2) O1 0.0340(19) 0.0365(18) 0.0299(19) -0.0024(15) 0.0135(15) -0.0085(15) O2 0.0361(19) 0.0382(18) 0.0279(19) -0.0027(15) 0.0146(15) -0.0077(16) O3 0.040(2) 0.039(2) 0.062(3) 0.0152(19) 0.0205(19) 0.0105(17) O4 0.094(4) 0.075(3) 0.047(3) 0.028(2) 0.049(3) 0.040(3) O5 0.058(3) 0.050(3) 0.097(4) -0.013(3) 0.009(3) 0.000(2) F1 0.075(3) 0.096(3) 0.042(2) -0.027(2) 0.0322(19) -0.038(2) F2 0.054(2) 0.117(4) 0.048(2) 0.004(2) 0.0012(19) -0.005(2) F3 0.106(3) 0.067(2) 0.062(3) -0.021(2) 0.027(2) -0.053(2) F4 0.120(4) 0.084(3) 0.071(3) -0.020(2) 0.062(3) -0.068(3) F5 0.046(2) 0.132(4) 0.071(3) -0.012(3) 0.034(2) -0.001(2) F6 0.064(2) 0.084(3) 0.0300(18) -0.0113(18) 0.0233(16) -0.026(2) F7 0.072(3) 0.038(2) 0.132(4) -0.001(2) 0.021(3) 0.0023(19) F8 0.047(2) 0.067(2) 0.077(3) 0.026(2) 0.0189(19) 0.0243(18) F9 0.149(4) 0.102(3) 0.073(3) 0.059(3) 0.077(3) 0.075(3) S1 0.0400(7) 0.0376(7) 0.0379(8) 0.0094(6) 0.0169(6) 0.0069(6) Cu1 0.0293(3) 0.0264(3) 0.0254(3) 0.0000(2) 0.0117(2) -0.0034(2) Ag1 0.0349(2) 0.0492(3) 0.0376(3) -0.00272(19) 0.00981(19) -0.01023(18) C23 0.105(6) 0.047(4) 0.053(4) 0.004(3) 0.043(4) 0.016(4) C24 0.049(4) 0.093(6) 0.091(6) 0.039(5) 0.030(4) 0.024(4) C25 0.062(5) 0.066(5) 0.106(7) -0.008(5) 0.001(5) -0.012(4) C26 0.088(6) 0.076(6) 0.098(7) -0.045(5) 0.024(5) 0.001(5) C27 0.054(4) 0.088(6) 0.101(7) -0.027(5) 0.028(4) 0.003(4) C28 0.084(6) 0.064(5) 0.066(5) -0.012(4) 0.020(4) -0.024(4) C29 0.094(6) 0.052(4) 0.072(6) 0.022(4) 0.012(5) 0.039(4) C30 0.116(7) 0.070(5) 0.038(4) 0.019(4) 0.026(4) 0.065(5) C31 0.101(7) 0.073(5) 0.062(5) 0.032(4) 0.031(5) 0.049(5) _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 N1 1.342(6) . ? C1 C2 1.418(7) . ? C1 H1 0.9300 . ? C2 C3 1.373(7) . ? C2 Ag1 2.536(5) . ? C2 H2 0.9300 . ? C3 C4 1.424(7) . ? C3 H3 0.9300 . ? C4 N1 1.391(6) . ? C4 C5 1.404(7) . ? C5 C6 1.396(7) . ? C5 C10 1.501(8) . ? C6 N2 1.385(6) . ? C6 C7 1.420(6) . ? C7 C8 1.388(7) . ? C7 Ag1 2.703(5) 4_575 ? C7 H7 0.9300 . ? C8 C9 1.422(7) . ? C8 Ag1 2.382(5) 4_575 ? C8 H8 0.9300 . ? C9 N2 1.324(6) . ? C9 H9 0.9300 . ? C10 C11 1.325(9) . ? C10 C15 1.331(9) . ? C11 C12 1.392(9) . ? C11 H11 0.9300 . ? C12 C13 1.317(9) . ? C12 H12 0.9300 . ? C13 C14 1.370(9) . ? C13 C16 1.438(8) . ? C14 C15 1.385(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N3 1.127(7) . ? C17 F1 1.309(7) . ? C17 F2 1.322(7) . ? C17 F3 1.344(7) . ? C17 C18 1.529(7) . ? C18 O1 1.254(6) . ? C18 C19 1.380(7) . ? C19 C20 1.393(7) . ? C19 H19 0.9300 . ? C20 O2 1.251(6) . ? C20 C21 1.523(8) . ? C21 F6 1.314(7) . ? C21 F5 1.337(8) . ? C21 F4 1.346(7) . ? C22 F9 1.321(7) . ? C22 F8 1.329(6) . ? C22 F7 1.334(8) . ? C22 S1 1.824(6) . ? N1 Cu1 1.949(4) . ? N2 Cu1 1.955(4) . ? N3 Ag1 2.215(5) 3_565 ? O1 Cu1 1.977(3) . ? O2 Cu1 1.978(3) . ? O3 S1 1.433(4) . ? O3 Cu1 2.400(4) . ? O4 S1 1.422(4) . ? O4 Ag1 2.450(4) . ? O5 S1 1.426(5) . ? Ag1 N3 2.215(5) 3_565 ? Ag1 C8 2.382(5) 4_576 ? Ag1 C7 2.703(5) 4_576 ? C23 C28 1.372(7) . ? C23 C24 1.374(11) . ? C23 H23 0.9300 . ? C24 C25 1.384(12) . ? C24 H24 0.9300 . ? C25 C26 1.341(12) . ? C25 H25 0.9300 . ? C26 C27 1.333(11) . ? C26 H26 0.9300 . ? C27 C28 1.352(11) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.380(12) . ? C29 C31 1.388(11) 3_665 ? C29 H29 0.9300 . ? C30 C31 1.361(12) . ? C30 H30 0.9300 . ? C31 C29 1.388(11) 3_665 ? C31 H31 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.4(4) . . ? N1 C1 H1 124.3 . . ? C2 C1 H1 124.3 . . ? C3 C2 C1 106.3(5) . . ? C3 C2 Ag1 99.8(3) . . ? C1 C2 Ag1 90.4(3) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? Ag1 C2 H2 81.5 . . ? C2 C3 C4 107.0(5) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N1 C4 C5 123.3(4) . . ? N1 C4 C3 109.0(4) . . ? C5 C4 C3 127.6(4) . . ? C6 C5 C4 125.1(4) . . ? C6 C5 C10 117.1(5) . . ? C4 C5 C10 117.7(5) . . ? N2 C6 C5 124.3(4) . . ? N2 C6 C7 108.5(4) . . ? C5 C6 C7 127.0(4) . . ? C8 C7 C6 107.5(4) . . ? C8 C7 Ag1 61.7(3) . 4_575 ? C6 C7 Ag1 107.7(3) . 4_575 ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? Ag1 C7 H7 98.3 4_575 . ? C7 C8 C9 104.8(4) . . ? C7 C8 Ag1 87.5(3) . 4_575 ? C9 C8 Ag1 100.4(3) . 4_575 ? C7 C8 H8 127.6 . . ? C9 C8 H8 127.6 . . ? Ag1 C8 H8 83.6 4_575 . ? N2 C9 C8 112.0(4) . . ? N2 C9 H9 124.0 . . ? C8 C9 H9 124.0 . . ? C11 C10 C15 117.4(6) . . ? C11 C10 C5 120.9(6) . . ? C15 C10 C5 121.5(6) . . ? C10 C11 C12 122.7(6) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C13 C12 C11 119.8(6) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 118.6(6) . . ? C12 C13 C16 120.5(6) . . ? C14 C13 C16 120.7(6) . . ? C13 C14 C15 119.8(6) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C10 C15 C14 121.5(6) . . ? C10 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? N3 C16 C13 178.9(8) . . ? F1 C17 F2 107.7(5) . . ? F1 C17 F3 107.7(5) . . ? F2 C17 F3 106.7(5) . . ? F1 C17 C18 112.7(5) . . ? F2 C17 C18 110.7(5) . . ? F3 C17 C18 111.0(5) . . ? O1 C18 C19 128.3(5) . . ? O1 C18 C17 114.5(5) . . ? C19 C18 C17 117.0(5) . . ? C18 C19 C20 120.8(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? O2 C20 C19 127.7(5) . . ? O2 C20 C21 115.0(5) . . ? C19 C20 C21 117.3(5) . . ? F6 C21 F5 107.7(5) . . ? F6 C21 F4 107.7(5) . . ? F5 C21 F4 106.3(5) . . ? F6 C21 C20 113.6(5) . . ? F5 C21 C20 110.3(5) . . ? F4 C21 C20 110.9(5) . . ? F9 C22 F8 107.6(5) . . ? F9 C22 F7 108.2(6) . . ? F8 C22 F7 106.4(5) . . ? F9 C22 S1 111.3(4) . . ? F8 C22 S1 111.9(4) . . ? F7 C22 S1 111.3(4) . . ? C1 N1 C4 106.3(4) . . ? C1 N1 Cu1 125.9(3) . . ? C4 N1 Cu1 127.6(3) . . ? C9 N2 C6 107.1(4) . . ? C9 N2 Cu1 125.8(3) . . ? C6 N2 Cu1 127.0(3) . . ? C16 N3 Ag1 159.8(6) . 3_565 ? C18 O1 Cu1 126.8(3) . . ? C20 O2 Cu1 127.1(3) . . ? S1 O3 Cu1 124.1(2) . . ? S1 O4 Ag1 149.8(3) . . ? O4 S1 O5 115.5(3) . . ? O4 S1 O3 115.4(3) . . ? O5 S1 O3 114.9(3) . . ? O4 S1 C22 102.7(3) . . ? O5 S1 C22 103.1(3) . . ? O3 S1 C22 102.6(3) . . ? N1 Cu1 N2 91.39(16) . . ? N1 Cu1 O1 89.35(15) . . ? N2 Cu1 O1 170.52(15) . . ? N1 Cu1 O2 175.93(16) . . ? N2 Cu1 O2 89.39(15) . . ? O1 Cu1 O2 89.22(14) . . ? N1 Cu1 O3 93.41(15) . . ? N2 Cu1 O3 98.44(15) . . ? O1 Cu1 O3 90.94(14) . . ? O2 Cu1 O3 90.42(14) . . ? N3 Ag1 C8 142.0(2) 3_565 4_576 ? N3 Ag1 O4 104.8(2) 3_565 . ? C8 Ag1 O4 95.13(18) 4_576 . ? N3 Ag1 C2 99.83(18) 3_565 . ? C8 Ag1 C2 105.09(17) 4_576 . ? O4 Ag1 C2 106.51(16) . . ? N3 Ag1 C7 111.17(19) 3_565 4_576 ? C8 Ag1 C7 30.86(16) 4_576 4_576 ? O4 Ag1 C7 111.22(16) . 4_576 ? C2 Ag1 C7 121.63(16) . 4_576 ? C28 C23 C24 118.8(7) . . ? C28 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C23 C24 C25 119.5(7) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 119.2(7) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C27 C26 C25 121.9(8) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C26 C27 C28 119.9(8) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C23 120.6(7) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? C30 C29 C31 119.0(8) . 3_665 ? C30 C29 H29 120.5 . . ? C31 C29 H29 120.5 3_665 . ? C31 C30 C29 121.9(8) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C29 119.1(9) . 3_665 ? C30 C31 H31 120.5 . . ? C29 C31 H31 120.5 3_665 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.645 _refine_diff_density_min -1.571 _refine_diff_density_rms 0.154 #===END