# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Hongyun Zhang' _publ_contact_author_email WZHY917@ZZU.EDU.CN _publ_section_title ; Counteranion's Effects on the Structures of Supramolecular Silver Coordination Compounds of One Asymmetric and One Biting Organic Ligands ; loop_ _publ_author_name 'Hongyun Zhang' 'Lu-Yan Meng' 'Yunyin Niu' 'Caoyuan Niu' 'Xin-Sheng Wan' 'Ben-Lai Wu' 'Xianfu Zheng' # Attachment 'all.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 706593' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H66 Ag4 As4 F24 N18 O9' _chemical_formula_weight 2550.59 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' As As 0.0499 2.0058 '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 trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 25.9571(7) _cell_length_b 25.9571(7) _cell_length_c 22.5629(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13165.5(9) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7482 _exptl_absorpt_coefficient_mu 2.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3808 _exptl_absorpt_correction_T_max 0.5634 _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 23848 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0116 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2740 _reflns_number_gt 2421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The bond lengths C13-O2 and C5-H5 were restrained to target values of 1.35(1) and 0.95(2) \%A, respectively. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+37.9821P] 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 2740 _refine_ls_number_parameters 211 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.044 _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 Ag1 Ag 0.3333 0.849046(16) -0.0833 0.05087(16) Uani 1 2 d S . . Ag2 Ag 0.3333 0.6667 0.4167 0.0502(2) Uani 1 6 d S . . C7 C 0.26386(13) 0.77401(13) 0.22637(12) 0.0325(6) Uani 1 1 d . . . H7 H 0.2885 0.7594 0.2119 0.039 Uiso 1 1 calc R . . C3 C 0.26222(14) 0.81080(13) 0.12369(12) 0.0321(6) Uani 1 1 d . . . C10 C 0.20540(15) 0.81941(14) 0.20841(13) 0.0366(7) Uani 1 1 d . . . C11 C 0.27299(14) 0.74241(15) 0.32599(14) 0.0369(7) Uani 1 1 d . . . C9 C 0.21314(14) 0.79042(14) 0.30911(12) 0.0356(7) Uani 1 1 d . . . C6 C 0.24218(14) 0.80015(13) 0.18689(12) 0.0330(6) Uani 1 1 d . . . C8 C 0.25033(13) 0.76902(13) 0.28581(12) 0.0322(6) Uani 1 1 d . . . N3 N 0.19230(12) 0.81374(12) 0.26701(11) 0.0374(6) Uani 1 1 d . . . H1 H 0.1682 0.8262 0.2793 0.045 Uiso 1 1 calc R . . O1 O 0.19840(12) 0.78835(12) 0.36166(9) 0.0492(6) Uani 1 1 d . . . C2 C 0.30148(15) 0.86771(14) 0.10392(14) 0.0398(7) Uani 1 1 d . . . H2 H 0.3158 0.9005 0.1304 0.048 Uiso 1 1 calc R . . C4 C 0.24307(16) 0.76490(14) 0.08284(13) 0.0398(7) Uani 1 1 d . . . H4 H 0.2156 0.7252 0.0942 0.048 Uiso 1 1 calc R . . C5 C 0.26436(16) 0.77748(15) 0.02533(13) 0.0409(7) Uani 1 1 d D . . H5 H 0.2514 0.7455 -0.0020 0.049 Uiso 1 1 calc RD . . C1 C 0.31973(14) 0.87667(15) 0.04548(14) 0.0400(7) Uani 1 1 d . . . H1A H 0.3460 0.9161 0.0324 0.048 Uiso 1 1 calc R . . N2 N 0.29070(15) 0.72015(16) 0.35710(13) 0.0532(8) Uani 1 1 d . . . N1 N 0.30202(12) 0.83218(12) 0.00667(11) 0.0363(6) Uani 1 1 d . . . C12 C 0.1757(2) 0.84486(19) 0.17205(15) 0.0539(9) Uani 1 1 d . . . H12A H 0.1474 0.8498 0.1967 0.081 Uiso 1 1 calc R . . H12B H 0.1545 0.8179 0.1391 0.081 Uiso 1 1 calc R . . H12C H 0.2057 0.8836 0.1564 0.081 Uiso 1 1 calc R . . As1 As 0.3333 0.6667 0.1667 0.0379(2) Uani 1 6 d S . . As2 As 0.3333 0.01620(3) 0.9167 0.0960(3) Uani 1 2 d S . . F1 F 0.31218(14) 0.70675(13) 0.12387(14) 0.0868(9) Uani 1 1 d . . . F2 F 0.2784(4) 0.0308(4) 0.9150(4) 0.256(5) Uani 1 1 d . . . F3 F 0.3839(3) -0.0040(4) 0.9169(5) 0.257(5) Uani 1 1 d . . . F4 F 0.3274(3) 0.0143(5) 0.9887(3) 0.271(5) Uani 1 1 d . . . O2 O 0.4348(7) 0.1014(7) 0.0833 0.268(7) Uani 1 2 d SDU . . C13 C 0.4512(12) 0.1366(10) 0.0338(9) 0.189(9) Uani 0.50 1 d PDU . . H13A H 0.4211 0.1477 0.0249 0.284 Uiso 0.50 1 calc PR . . H13B H 0.4548 0.1147 0.0002 0.284 Uiso 0.50 1 calc PR . . H13C H 0.4896 0.1726 0.0408 0.284 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0671(3) 0.0654(2) 0.0206(2) 0.00665(7) 0.01329(15) 0.03353(14) Ag2 0.0463(2) 0.0463(2) 0.0580(4) 0.000 0.000 0.02313(12) C7 0.0364(15) 0.0382(15) 0.0274(14) 0.0031(11) 0.0067(11) 0.0219(13) C3 0.0401(16) 0.0420(16) 0.0229(14) 0.0040(11) 0.0059(11) 0.0271(13) C10 0.0485(17) 0.0425(16) 0.0259(14) 0.0045(12) 0.0059(12) 0.0279(15) C11 0.0358(16) 0.0460(17) 0.0287(15) 0.0039(13) 0.0029(12) 0.0202(14) C9 0.0400(16) 0.0446(17) 0.0249(15) 0.0025(12) 0.0047(12) 0.0232(14) C6 0.0410(16) 0.0399(16) 0.0220(13) 0.0033(11) 0.0067(12) 0.0233(13) C8 0.0347(15) 0.0377(15) 0.0258(13) 0.0031(11) 0.0021(11) 0.0192(13) N3 0.0506(15) 0.0521(15) 0.0238(11) 0.0056(10) 0.0106(11) 0.0363(13) O1 0.0681(16) 0.0764(17) 0.0222(10) 0.0078(10) 0.0125(10) 0.0503(14) C2 0.0482(18) 0.0409(17) 0.0273(15) -0.0034(12) 0.0025(13) 0.0200(15) C4 0.0564(19) 0.0351(16) 0.0306(15) 0.0024(12) 0.0076(14) 0.0249(15) C5 0.057(2) 0.0442(17) 0.0278(15) -0.0017(13) 0.0041(14) 0.0296(16) C1 0.0417(17) 0.0439(17) 0.0317(16) 0.0048(13) 0.0072(13) 0.0194(14) N2 0.0577(19) 0.068(2) 0.0396(16) 0.0095(15) -0.0056(14) 0.0358(17) N1 0.0429(15) 0.0522(16) 0.0222(12) 0.0039(11) 0.0061(10) 0.0301(13) C12 0.079(3) 0.078(3) 0.0347(18) 0.0118(17) 0.0105(17) 0.061(2) As1 0.0296(3) 0.0296(3) 0.0544(5) 0.000 0.000 0.01479(13) As2 0.1007(6) 0.0777(4) 0.1173(7) 0.0307(3) 0.0614(6) 0.0503(3) F1 0.092(2) 0.0800(18) 0.107(2) 0.0262(16) -0.0088(17) 0.0572(16) F2 0.301(9) 0.328(9) 0.295(10) 0.134(8) 0.133(8) 0.273(8) F3 0.116(4) 0.219(7) 0.462(15) -0.002(7) 0.060(6) 0.104(5) F4 0.151(5) 0.470(15) 0.129(5) 0.037(7) 0.044(4) 0.108(8) O2 0.274(8) 0.274(8) 0.246(11) 0.018(5) -0.018(5) 0.128(8) C13 0.191(12) 0.180(12) 0.197(13) 0.033(9) -0.009(9) 0.093(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.149(2) 12_554 ? Ag1 N1 2.150(2) . ? Ag2 N2 2.548(3) 10_455 ? Ag2 N2 2.548(3) . ? Ag2 N2 2.548(3) 2_665 ? Ag2 N2 2.548(3) 3_565 ? Ag2 N2 2.549(3) 11_565 ? Ag2 N2 2.549(3) 12 ? C7 C8 1.376(4) . ? C7 C6 1.397(4) . ? C7 H7 0.9500 . ? C3 C2 1.384(4) . ? C3 C4 1.387(4) . ? C3 C6 1.496(4) . ? C10 N3 1.355(4) . ? C10 C6 1.369(4) . ? C10 C12 1.487(5) . ? C11 N2 1.142(4) . ? C11 C8 1.432(4) . ? C9 O1 1.239(4) . ? C9 N3 1.375(4) . ? C9 C8 1.433(4) . ? N3 H1 0.8800 . ? C2 C1 1.381(4) . ? C2 H2 0.9500 . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C5 N1 1.327(4) . ? C5 H5 0.9500 . ? C1 N1 1.335(4) . ? C1 H1A 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? As1 F1 1.699(2) 25_565 ? As1 F1 1.699(2) . ? As1 F1 1.699(2) 2_665 ? As1 F1 1.699(2) 3_565 ? As1 F1 1.699(2) 26_455 ? As1 F1 1.699(2) 27 ? As2 F4 1.631(7) 12_556 ? As2 F4 1.631(7) . ? As2 F3 1.639(6) 12_556 ? As2 F3 1.639(6) . ? As2 F2 1.649(6) . ? As2 F2 1.649(6) 12_556 ? O2 C13 1.370(10) . ? O2 C13 1.370(10) 16_544 ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 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 N1 Ag1 N1 178.33(14) 12_554 . ? N2 Ag2 N2 173.66(16) 10_455 . ? N2 Ag2 N2 90.08(15) 10_455 2_665 ? N2 Ag2 N2 94.75(10) . 2_665 ? N2 Ag2 N2 80.74(16) 10_455 3_565 ? N2 Ag2 N2 94.75(10) . 3_565 ? N2 Ag2 N2 94.75(10) 2_665 3_565 ? N2 Ag2 N2 94.75(10) 10_455 11_565 ? N2 Ag2 N2 90.08(15) . 11_565 ? N2 Ag2 N2 80.74(16) 2_665 11_565 ? N2 Ag2 N2 173.67(15) 3_565 11_565 ? N2 Ag2 N2 94.75(10) 10_455 12 ? N2 Ag2 N2 80.74(16) . 12 ? N2 Ag2 N2 173.66(15) 2_665 12 ? N2 Ag2 N2 90.08(15) 3_565 12 ? N2 Ag2 N2 94.75(10) 11_565 12 ? C8 C7 C6 121.4(3) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C2 C3 C4 117.3(3) . . ? C2 C3 C6 120.5(3) . . ? C4 C3 C6 122.2(3) . . ? N3 C10 C6 119.3(3) . . ? N3 C10 C12 115.4(3) . . ? C6 C10 C12 125.2(3) . . ? N2 C11 C8 178.4(4) . . ? O1 C9 N3 120.0(3) . . ? O1 C9 C8 126.0(3) . . ? N3 C9 C8 114.0(2) . . ? C10 C6 C7 118.3(3) . . ? C10 C6 C3 120.8(3) . . ? C7 C6 C3 120.7(3) . . ? C7 C8 C11 121.0(3) . . ? C7 C8 C9 120.7(3) . . ? C11 C8 C9 118.2(3) . . ? C10 N3 C9 126.1(3) . . ? C10 N3 H1 116.9 . . ? C9 N3 H1 116.9 . . ? C1 C2 C3 119.7(3) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C5 C4 C3 119.4(3) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N1 C5 C4 122.9(3) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? N1 C1 C2 122.7(3) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C11 N2 Ag2 173.9(3) . . ? C5 N1 C1 117.9(3) . . ? C5 N1 Ag1 121.3(2) . . ? C1 N1 Ag1 120.8(2) . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? F1 As1 F1 179.996(1) 25_565 . ? F1 As1 F1 89.11(16) 25_565 2_665 ? F1 As1 F1 90.89(16) . 2_665 ? F1 As1 F1 89.11(16) 25_565 3_565 ? F1 As1 F1 90.89(16) . 3_565 ? F1 As1 F1 90.89(16) 2_665 3_565 ? F1 As1 F1 90.89(16) 25_565 26_455 ? F1 As1 F1 89.11(16) . 26_455 ? F1 As1 F1 180.00(18) 2_665 26_455 ? F1 As1 F1 89.11(16) 3_565 26_455 ? F1 As1 F1 90.89(16) 25_565 27 ? F1 As1 F1 89.11(16) . 27 ? F1 As1 F1 89.11(16) 2_665 27 ? F1 As1 F1 179.997(1) 3_565 27 ? F1 As1 F1 90.89(16) 26_455 27 ? F4 As2 F4 178.1(9) 12_556 . ? F4 As2 F3 93.8(6) 12_556 12_556 ? F4 As2 F3 87.6(5) . 12_556 ? F4 As2 F3 87.6(5) 12_556 . ? F4 As2 F3 93.8(6) . . ? F3 As2 F3 87.9(5) 12_556 . ? F4 As2 F2 91.6(5) 12_556 . ? F4 As2 F2 87.1(4) . . ? F3 As2 F2 87.5(4) 12_556 . ? F3 As2 F2 175.3(5) . . ? F4 As2 F2 87.1(4) 12_556 12_556 ? F4 As2 F2 91.6(5) . 12_556 ? F3 As2 F2 175.3(5) 12_556 12_556 ? F3 As2 F2 87.5(4) . 12_556 ? F2 As2 F2 97.1(7) . 12_556 ? C13 O2 C13 121(3) . 16_544 ? O2 C13 H13A 109.5 . . ? O2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 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 N3 C10 C6 C7 1.4(5) . . . . ? C12 C10 C6 C7 -176.2(3) . . . . ? N3 C10 C6 C3 -174.2(3) . . . . ? C12 C10 C6 C3 8.1(5) . . . . ? C8 C7 C6 C10 -1.9(5) . . . . ? C8 C7 C6 C3 173.8(3) . . . . ? C2 C3 C6 C10 69.5(4) . . . . ? C4 C3 C6 C10 -111.0(4) . . . . ? C2 C3 C6 C7 -106.0(4) . . . . ? C4 C3 C6 C7 73.5(4) . . . . ? C6 C7 C8 C11 -179.7(3) . . . . ? C6 C7 C8 C9 0.3(5) . . . . ? N2 C11 C8 C7 -45(13) . . . . ? N2 C11 C8 C9 135(13) . . . . ? O1 C9 C8 C7 -179.7(3) . . . . ? N3 C9 C8 C7 1.7(4) . . . . ? O1 C9 C8 C11 0.2(5) . . . . ? N3 C9 C8 C11 -178.4(3) . . . . ? C6 C10 N3 C9 0.7(5) . . . . ? C12 C10 N3 C9 178.6(3) . . . . ? O1 C9 N3 C10 179.1(3) . . . . ? C8 C9 N3 C10 -2.2(5) . . . . ? C4 C3 C2 C1 0.1(5) . . . . ? C6 C3 C2 C1 179.7(3) . . . . ? C2 C3 C4 C5 1.1(5) . . . . ? C6 C3 C4 C5 -178.5(3) . . . . ? C3 C4 C5 N1 -1.1(5) . . . . ? C3 C2 C1 N1 -1.5(5) . . . . ? C8 C11 N2 Ag2 33(15) . . . . ? N2 Ag2 N2 C11 92(3) 10_455 . . . ? N2 Ag2 N2 C11 -48(3) 2_665 . . . ? N2 Ag2 N2 C11 47(3) 3_565 . . . ? N2 Ag2 N2 C11 -129(3) 11_565 . . . ? N2 Ag2 N2 C11 137(3) 12 . . . ? C4 C5 N1 C1 -0.1(5) . . . . ? C4 C5 N1 Ag1 -179.8(3) . . . . ? C2 C1 N1 C5 1.4(5) . . . . ? C2 C1 N1 Ag1 -178.9(3) . . . . ? N1 Ag1 N1 C5 -35.7(2) 12_554 . . . ? N1 Ag1 N1 C1 144.7(2) 12_554 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H1 O1 0.88 2.02 2.874(3) 163.0 31_565 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.784 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.085 data_2 _database_code_depnum_ccdc_archive 'CCDC 706594' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144 H108 Ag8 F48 N36 O12 Sb8' _chemical_formula_weight 5283.62 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 26.315(4) _cell_length_b 26.315(4) _cell_length_c 22.502(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13494(4) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7608 _exptl_absorpt_coefficient_mu 2.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.444 _exptl_absorpt_correction_T_max 0.638 _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 21868 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0129 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2500 _reflns_number_gt 2148 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0805P)^2^+32.1937P] 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 2500 _refine_ls_number_parameters 196 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 1.0000 1.0000 1.0000 0.0510(2) Uani 1 6 d S . . Sb2 Sb 1.0000 0.35151(3) 0.7500 0.1155(4) Uani 1 2 d S . . Ag1 Ag 0.84738(2) 0.3333 1.0833 0.0609(2) Uani 1 2 d S . . Ag2 Ag 0.6667 0.3333 0.5833 0.0770(3) Uani 1 6 d S . . F1 F 0.9562(2) 0.93351(19) 0.9547(2) 0.1174(15) Uani 1 1 d . . . F2 F 0.9337(6) 0.3611(6) 0.7417(6) 0.235(4) Uani 1 1 d U . . F3 F 1.0100(7) 0.3445(7) 0.6701(10) 0.283(6) Uani 1 1 d U . . F4 F 1.0514(6) 0.3263(7) 0.7507(7) 0.263(5) Uani 1 1 d U . . O1 O 0.78905(18) 0.19866(17) 0.63750(12) 0.0641(9) Uani 1 1 d . . . N1 N 0.83105(15) 0.30145(16) 0.99350(13) 0.0442(8) Uani 1 1 d . . . N2 N 0.81377(17) 0.19257(16) 0.73299(15) 0.0497(8) Uani 1 1 d . . . H2 H 0.8255 0.1683 0.7207 0.060 Uiso 1 1 calc R . . N3 N 0.7210(2) 0.2897(2) 0.6427(2) 0.0693(11) Uani 1 1 d . . . C1 C 0.7771(2) 0.2629(2) 0.97497(18) 0.0525(10) Uani 1 1 d . . . H1 H 0.7455 0.2495 1.0025 0.063 Uiso 1 1 calc R . . C2 C 0.8747(2) 0.32012(19) 0.95511(19) 0.0507(10) Uani 1 1 d . . . H2A H 0.9134 0.3472 0.9681 0.061 Uiso 1 1 calc R . . C3 C 0.76511(18) 0.2418(2) 0.91761(17) 0.0492(10) Uani 1 1 d . . . H3 H 0.7262 0.2139 0.9063 0.059 Uiso 1 1 calc R . . C4 C 0.86611(19) 0.30149(19) 0.89628(18) 0.0493(10) Uani 1 1 d . . . H4 H 0.8984 0.3161 0.8697 0.059 Uiso 1 1 calc R . . C5 C 0.81038(17) 0.26161(18) 0.87655(16) 0.0407(8) Uani 1 1 d . . . C6 C 0.80061(17) 0.24224(19) 0.81293(16) 0.0426(8) Uani 1 1 d . . . C7 C 0.77474(18) 0.26357(18) 0.77328(17) 0.0440(8) Uani 1 1 d . . . H7 H 0.7604 0.2879 0.7879 0.053 Uiso 1 1 calc R . . C8 C 0.76952(18) 0.25017(18) 0.71380(17) 0.0455(9) Uani 1 1 d . . . C9 C 0.7908(2) 0.21311(19) 0.69089(17) 0.0486(10) Uani 1 1 d . . . C10 C 0.8201(2) 0.2059(2) 0.79124(17) 0.0475(9) Uani 1 1 d . . . C11 C 0.8452(3) 0.1770(3) 0.8279(2) 0.0665(13) Uani 1 1 d . . . H11A H 0.8182 0.1555 0.8606 0.100 Uiso 1 1 calc R . . H11B H 0.8830 0.2067 0.8442 0.100 Uiso 1 1 calc R . . H11C H 0.8508 0.1495 0.8032 0.100 Uiso 1 1 calc R . . C12 C 0.7431(2) 0.27206(19) 0.67327(18) 0.0507(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.0443(3) 0.0443(3) 0.0642(5) 0.000 0.000 0.02217(13) Sb2 0.1111(6) 0.0873(4) 0.1561(8) 0.0378(3) 0.0756(6) 0.0556(3) Ag1 0.0798(3) 0.0796(4) 0.0234(3) -0.01636(19) -0.00818(10) 0.03979(19) Ag2 0.0726(4) 0.0726(4) 0.0858(7) 0.000 0.000 0.0363(2) F1 0.125(3) 0.080(3) 0.125(4) -0.037(2) -0.026(3) 0.034(2) F2 0.232(7) 0.257(8) 0.280(8) 0.009(7) 0.030(6) 0.171(7) F3 0.264(9) 0.292(10) 0.264(10) -0.017(8) 0.019(8) 0.117(8) F4 0.222(8) 0.283(9) 0.315(11) -0.010(7) 0.031(7) 0.149(7) O1 0.101(3) 0.086(2) 0.0253(13) -0.0148(14) -0.0044(15) 0.061(2) N1 0.061(2) 0.056(2) 0.0246(15) -0.0080(13) -0.0022(14) 0.0359(17) N2 0.066(2) 0.062(2) 0.0307(15) -0.0125(15) -0.0032(15) 0.0390(19) N3 0.089(3) 0.068(3) 0.050(2) 0.006(2) -0.016(2) 0.039(2) C1 0.055(2) 0.072(3) 0.035(2) -0.0060(19) 0.0048(17) 0.035(2) C2 0.056(2) 0.054(2) 0.038(2) -0.0114(17) -0.0102(17) 0.024(2) C3 0.045(2) 0.069(3) 0.0326(19) -0.0104(18) -0.0029(16) 0.028(2) C4 0.055(2) 0.057(2) 0.0305(19) -0.0075(17) 0.0039(17) 0.024(2) C5 0.052(2) 0.052(2) 0.0264(17) -0.0078(15) -0.0026(15) 0.0330(18) C6 0.048(2) 0.056(2) 0.0272(18) -0.0088(16) -0.0045(15) 0.0282(18) C7 0.053(2) 0.046(2) 0.0331(18) -0.0075(16) -0.0022(16) 0.0252(18) C8 0.054(2) 0.047(2) 0.0319(18) -0.0017(15) -0.0032(16) 0.0222(18) C9 0.062(2) 0.054(2) 0.0315(19) -0.0111(17) -0.0014(17) 0.031(2) C10 0.057(2) 0.058(2) 0.0327(19) -0.0122(17) -0.0038(17) 0.032(2) C11 0.090(4) 0.095(4) 0.044(2) -0.011(2) -0.007(2) 0.069(3) C12 0.064(3) 0.048(2) 0.032(2) -0.0031(16) -0.0041(18) 0.021(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 Sb1 F1 1.848(4) . ? Sb1 F1 1.848(4) 19_777 ? Sb1 F1 1.848(4) 3_675 ? Sb1 F1 1.848(4) 20_567 ? Sb1 F1 1.848(4) 2_765 ? Sb1 F1 1.848(4) 21_657 ? Sb2 F4 1.779(14) 5_766 ? Sb2 F4 1.779(14) . ? Sb2 F3 1.84(2) . ? Sb2 F3 1.84(2) 5_766 ? Sb2 F2 1.894(10) 5_766 ? Sb2 F2 1.894(10) . ? Ag1 N1 2.148(3) . ? Ag1 N1 2.148(3) 16_556 ? Ag2 N3 2.605(5) . ? Ag2 N3 2.605(5) 17_655 ? Ag2 N3 2.605(5) 16 ? Ag2 N3 2.605(5) 18_545 ? Ag2 N3 2.605(5) 3_665 ? Ag2 N3 2.605(5) 2_655 ? O1 C9 1.254(5) . ? N1 C2 1.321(6) . ? N1 C1 1.334(6) . ? N2 C10 1.346(5) . ? N2 C9 1.372(6) . ? N3 C12 1.140(7) . ? C1 C3 1.378(6) . ? C2 C4 1.390(6) . ? C3 C5 1.387(6) . ? C4 C5 1.382(6) . ? C5 C6 1.498(5) . ? C6 C10 1.380(6) . ? C6 C7 1.399(6) . ? C7 C8 1.373(5) . ? C8 C12 1.430(6) . ? C8 C9 1.441(6) . ? C10 C11 1.484(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 F1 Sb1 F1 180.000(2) . 19_777 ? F1 Sb1 F1 92.4(2) . 3_675 ? F1 Sb1 F1 87.6(2) 19_777 3_675 ? F1 Sb1 F1 87.6(2) . 20_567 ? F1 Sb1 F1 92.4(2) 19_777 20_567 ? F1 Sb1 F1 87.6(2) 3_675 20_567 ? F1 Sb1 F1 92.4(2) . 2_765 ? F1 Sb1 F1 87.6(2) 19_777 2_765 ? F1 Sb1 F1 92.4(2) 3_675 2_765 ? F1 Sb1 F1 180.000(2) 20_567 2_765 ? F1 Sb1 F1 87.6(2) . 21_657 ? F1 Sb1 F1 92.4(2) 19_777 21_657 ? F1 Sb1 F1 180.0(3) 3_675 21_657 ? F1 Sb1 F1 92.4(2) 20_567 21_657 ? F1 Sb1 F1 87.6(2) 2_765 21_657 ? F4 Sb2 F4 82.4(10) 5_766 . ? F4 Sb2 F3 86.8(7) 5_766 . ? F4 Sb2 F3 78.3(8) . . ? F4 Sb2 F3 78.3(8) 5_766 5_766 ? F4 Sb2 F3 86.8(7) . 5_766 ? F3 Sb2 F3 160.2(13) . 5_766 ? F4 Sb2 F2 166.8(6) 5_766 5_766 ? F4 Sb2 F2 85.5(7) . 5_766 ? F3 Sb2 F2 95.7(6) . 5_766 ? F3 Sb2 F2 96.0(7) 5_766 5_766 ? F4 Sb2 F2 85.5(7) 5_766 . ? F4 Sb2 F2 166.8(7) . . ? F3 Sb2 F2 96.0(7) . . ? F3 Sb2 F2 95.7(6) 5_766 . ? F2 Sb2 F2 107.1(8) 5_766 . ? N1 Ag1 N1 179.46(18) . 16_556 ? N3 Ag2 N3 88.6(2) . 17_655 ? N3 Ag2 N3 79.5(2) . 16 ? N3 Ag2 N3 96.09(15) 17_655 16 ? N3 Ag2 N3 173.8(2) . 18_545 ? N3 Ag2 N3 96.10(15) 17_655 18_545 ? N3 Ag2 N3 96.10(15) 16 18_545 ? N3 Ag2 N3 96.10(15) . 3_665 ? N3 Ag2 N3 79.5(2) 17_655 3_665 ? N3 Ag2 N3 173.8(2) 16 3_665 ? N3 Ag2 N3 88.6(2) 18_545 3_665 ? N3 Ag2 N3 96.10(15) . 2_655 ? N3 Ag2 N3 173.8(2) 17_655 2_655 ? N3 Ag2 N3 88.6(2) 16 2_655 ? N3 Ag2 N3 79.5(2) 18_545 2_655 ? N3 Ag2 N3 96.10(15) 3_665 2_655 ? C2 N1 C1 118.5(3) . . ? C2 N1 Ag1 120.2(3) . . ? C1 N1 Ag1 121.3(3) . . ? C10 N2 C9 126.2(4) . . ? C12 N3 Ag2 173.6(4) . . ? N1 C1 C3 122.7(4) . . ? N1 C2 C4 122.2(4) . . ? C1 C3 C5 119.5(4) . . ? C5 C4 C2 119.9(4) . . ? C4 C5 C3 117.2(4) . . ? C4 C5 C6 120.1(4) . . ? C3 C5 C6 122.7(4) . . ? C10 C6 C7 118.4(3) . . ? C10 C6 C5 120.9(3) . . ? C7 C6 C5 120.5(3) . . ? C8 C7 C6 121.7(4) . . ? C7 C8 C12 121.6(4) . . ? C7 C8 C9 120.0(4) . . ? C12 C8 C9 118.4(3) . . ? O1 C9 N2 119.9(4) . . ? O1 C9 C8 125.4(4) . . ? N2 C9 C8 114.6(3) . . ? N2 C10 C6 119.1(4) . . ? N2 C10 C11 115.9(4) . . ? C6 C10 C11 125.0(3) . . ? N3 C12 C8 177.5(5) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.265 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.097 data_3 _database_code_depnum_ccdc_archive 'CCDC 706595' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H18 Ag N7 O5' _chemical_formula_weight 592.32 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' Ag Ag -0.8971 1.1015 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.012(3) _cell_length_b 6.9639(8) _cell_length_c 15.0061(18) _cell_angle_alpha 90.00 _cell_angle_beta 116.001(2) _cell_angle_gamma 90.00 _cell_volume 2349.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 25.49 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6111 _exptl_absorpt_correction_T_max 0.9474 _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 6295 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.49 _reflns_number_total 2181 _reflns_number_gt 2036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The bond lengths N2-H10 and N4-O2 were restrained to target values of 0.88(1) and 1.25(1) \%A, respectively. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+2.9545P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00181(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2181 _refine_ls_number_parameters 188 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0563 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 O2 O -0.0203(15) 0.151(2) -0.249(4) 0.071(8) Uani 0.25 1 d PD . . O2' O -0.0037(15) 0.168(3) -0.239(2) 0.045(8) Uani 0.25 1 d P . . Ag1 Ag 0.0000 0.53979(3) -0.2500 0.04272(11) Uani 1 2 d S . . O1 O 0.22474(7) 0.4723(2) 0.53074(11) 0.0462(4) Uani 1 1 d . . . O3 O -0.03731(12) -0.1022(3) -0.2332(2) 0.0885(7) Uani 1 1 d . . . N1 N 0.04604(8) 0.5178(2) -0.08858(13) 0.0365(4) Uani 1 1 d . . . N2 N 0.20363(8) 0.3468(3) 0.37935(13) 0.0408(4) Uani 1 1 d D . . N3 N 0.15651(10) 0.9370(3) 0.48833(17) 0.0569(5) Uani 1 1 d . . . N4 N 0.0000 -0.0131(4) -0.2500 0.0549(8) Uani 1 2 d SD . . C1 C 0.04305(9) 0.3630(3) -0.03791(15) 0.0378(5) Uani 1 1 d . . . H1 H 0.0196 0.2571 -0.0740 0.045 Uiso 1 1 calc R . . C2 C 0.07221(9) 0.3497(3) 0.06367(15) 0.0382(5) Uani 1 1 d . . . H2 H 0.0683 0.2372 0.0962 0.046 Uiso 1 1 calc R . . C3 C 0.10735(9) 0.5012(3) 0.11864(15) 0.0352(4) Uani 1 1 d . . . C4 C 0.10989(9) 0.6628(3) 0.06614(15) 0.0394(5) Uani 1 1 d . . . H4 H 0.1329 0.7708 0.1004 0.047 Uiso 1 1 calc R . . C5 C 0.07898(9) 0.6657(3) -0.03551(16) 0.0406(5) Uani 1 1 d . . . H5 H 0.0811 0.7780 -0.0698 0.049 Uiso 1 1 calc R . . C6 C 0.14015(9) 0.4952(3) 0.22830(15) 0.0368(5) Uani 1 1 d . . . C7 C 0.17623(9) 0.3436(3) 0.27875(15) 0.0405(5) Uani 1 1 d . . . C8 C 0.19027(13) 0.1730(4) 0.23273(19) 0.0654(8) Uani 1 1 d . . . H8A H 0.2298 0.1240 0.2773 0.098 Uiso 1 1 calc R . . H8B H 0.1898 0.2102 0.1694 0.098 Uiso 1 1 calc R . . H8C H 0.1605 0.0728 0.2213 0.098 Uiso 1 1 calc R . . C9 C 0.13570(9) 0.6503(3) 0.28470(15) 0.0373(5) Uani 1 1 d . . . H9 H 0.1118 0.7576 0.2514 0.045 Uiso 1 1 calc R . . C10 C 0.16472(9) 0.6514(3) 0.38610(15) 0.0360(4) Uani 1 1 d . . . C11 C 0.19972(9) 0.4899(3) 0.43968(16) 0.0373(5) Uani 1 1 d . . . C12 C 0.15991(9) 0.8107(3) 0.44270(16) 0.0410(5) Uani 1 1 d . . . H10 H 0.2263(9) 0.248(2) 0.4090(16) 0.048(7) Uiso 1 1 d 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 O2 0.062(17) 0.013(4) 0.131(13) -0.002(6) 0.037(13) -0.007(6) O2' 0.06(2) 0.038(7) 0.066(13) -0.019(6) 0.049(14) -0.022(7) Ag1 0.05321(16) 0.04107(15) 0.02432(14) 0.000 0.00819(10) 0.000 O1 0.0485(9) 0.0595(10) 0.0244(8) 0.0020(7) 0.0104(7) 0.0078(7) O3 0.1121(18) 0.0743(14) 0.1031(19) 0.0203(14) 0.0693(16) 0.0150(14) N1 0.0382(9) 0.0389(9) 0.0278(9) 0.0016(7) 0.0103(7) 0.0032(7) N2 0.0450(10) 0.0444(11) 0.0256(9) 0.0052(8) 0.0086(8) 0.0109(8) N3 0.0677(14) 0.0550(13) 0.0501(13) -0.0058(10) 0.0277(11) 0.0052(10) N4 0.093(2) 0.0338(15) 0.0277(14) 0.000 0.0166(15) 0.000 C1 0.0377(10) 0.0351(11) 0.0342(11) -0.0016(9) 0.0098(9) 0.0010(8) C2 0.0407(11) 0.0351(11) 0.0356(11) 0.0057(9) 0.0140(9) 0.0035(9) C3 0.0341(10) 0.0413(11) 0.0271(10) 0.0024(8) 0.0107(8) 0.0050(8) C4 0.0419(11) 0.0397(11) 0.0303(11) -0.0007(9) 0.0101(9) -0.0058(9) C5 0.0445(11) 0.0417(12) 0.0317(11) 0.0046(9) 0.0130(9) -0.0023(9) C6 0.0365(10) 0.0421(11) 0.0280(11) 0.0033(8) 0.0108(9) 0.0004(8) C7 0.0445(11) 0.0442(12) 0.0283(10) 0.0021(9) 0.0117(9) 0.0048(9) C8 0.0833(19) 0.0620(17) 0.0351(13) -0.0013(12) 0.0113(13) 0.0300(14) C9 0.0378(10) 0.0398(11) 0.0317(11) 0.0046(9) 0.0130(9) 0.0008(9) C10 0.0350(10) 0.0411(11) 0.0312(10) 0.0000(9) 0.0139(8) -0.0007(8) C11 0.0338(10) 0.0472(12) 0.0291(11) 0.0007(9) 0.0120(9) -0.0008(9) C12 0.0405(11) 0.0471(13) 0.0342(11) 0.0020(10) 0.0153(9) 0.0005(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2 O2' 0.71(4) 2_554 ? O2 O2 1.03(6) 2_554 ? O2 N4 1.252(10) . ? O2' O2' 0.43(3) 2_554 ? O2' O2 0.71(4) 2_554 ? O2' N4 1.282(18) . ? Ag1 N1 2.1843(17) 2_554 ? Ag1 N1 2.1843(17) . ? Ag1 O2' 2.596(18) 2_554 ? O1 C11 1.234(3) . ? O3 N4 1.235(3) . ? N1 C1 1.340(3) . ? N1 C5 1.341(3) . ? N2 C7 1.357(3) . ? N2 C11 1.378(3) . ? N2 H10 0.877(10) . ? N3 C12 1.141(3) . ? N4 O3 1.235(3) 2_554 ? N4 O2 1.252(10) 2_554 ? N4 O2' 1.282(18) 2_554 ? C1 C2 1.375(3) . ? C1 H1 0.9500 . ? C2 C3 1.390(3) . ? C2 H2 0.9500 . ? C3 C4 1.391(3) . ? C3 C6 1.483(3) . ? C4 C5 1.375(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.380(3) . ? C6 C9 1.406(3) . ? C7 C8 1.491(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.369(3) . ? C9 H9 0.9500 . ? C10 C12 1.434(3) . ? C10 C11 1.436(3) . ? 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 O2' O2 O2 15.1(18) 2_554 2_554 ? O2' O2 N4 76.1(17) 2_554 . ? O2 O2 N4 65.6(14) 2_554 . ? O2' O2' O2 30(6) 2_554 2_554 ? O2' O2' N4 80.3(8) 2_554 . ? O2 O2' N4 71(2) 2_554 . ? N1 Ag1 N1 171.98(9) 2_554 . ? N1 Ag1 O2' 83.0(6) 2_554 2_554 ? N1 Ag1 O2' 89.0(6) . 2_554 ? C1 N1 C5 116.97(18) . . ? C1 N1 Ag1 123.50(14) . . ? C5 N1 Ag1 119.53(14) . . ? C7 N2 C11 126.56(18) . . ? C7 N2 H10 116.8(16) . . ? C11 N2 H10 116.6(16) . . ? O3 N4 O3 119.7(3) . 2_554 ? O3 N4 O2 144.0(16) . 2_554 ? O3 N4 O2 96.1(15) 2_554 2_554 ? O3 N4 O2 96.1(15) . . ? O3 N4 O2 144.0(16) 2_554 . ? O2 N4 O2 49(3) 2_554 . ? O3 N4 O2' 128.5(11) . 2_554 ? O3 N4 O2' 111.6(10) 2_554 2_554 ? O2 N4 O2' 17.9(14) 2_554 2_554 ? O2 N4 O2' 32.4(19) . 2_554 ? O3 N4 O2' 111.6(10) . . ? O3 N4 O2' 128.5(11) 2_554 . ? O2 N4 O2' 32.4(19) 2_554 . ? O2 N4 O2' 17.9(14) . . ? O2' N4 O2' 19.4(16) 2_554 . ? N1 C1 C2 123.29(19) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 119.81(19) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 116.88(19) . . ? C2 C3 C6 122.37(19) . . ? C4 C3 C6 120.74(19) . . ? C5 C4 C3 119.8(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 123.2(2) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C7 C6 C9 117.58(19) . . ? C7 C6 C3 122.76(19) . . ? C9 C6 C3 119.65(18) . . ? N2 C7 C6 119.19(19) . . ? N2 C7 C8 114.93(19) . . ? C6 C7 C8 125.9(2) . . ? 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 . . ? C10 C9 C6 122.00(19) . . ? C10 C9 H9 119.0 . . ? C6 C9 H9 119.0 . . ? C9 C10 C12 121.44(19) . . ? C9 C10 C11 120.93(19) . . ? C12 C10 C11 117.60(18) . . ? O1 C11 N2 120.51(19) . . ? O1 C11 C10 125.9(2) . . ? N2 C11 C10 113.59(18) . . ? N3 C12 C10 179.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N1 C1 -22.95(16) 2_554 . . . ? O2' Ag1 N1 C1 -26.7(6) 2_554 . . . ? N1 Ag1 N1 C5 157.58(16) 2_554 . . . ? O2' Ag1 N1 C5 153.9(6) 2_554 . . . ? O2' O2 N4 O3 -178(5) 2_554 . . . ? O2 O2 N4 O3 171(5) 2_554 . . . ? O2' O2 N4 O3 -4(9) 2_554 . . 2_554 ? O2 O2 N4 O3 -15(9) 2_554 . . 2_554 ? O2' O2 N4 O2 12(3) 2_554 . . 2_554 ? O2 O2 N4 O2' -12(3) 2_554 . . 2_554 ? O2' O2 N4 O2' 32(7) 2_554 . . . ? O2 O2 N4 O2' 20(4) 2_554 . . . ? O2' O2' N4 O3 -153(9) 2_554 . . . ? O2 O2' N4 O3 178(6) 2_554 . . . ? O2' O2' N4 O3 33(10) 2_554 . . 2_554 ? O2 O2' N4 O3 3(7) 2_554 . . 2_554 ? O2' O2' N4 O2 29(7) 2_554 . . 2_554 ? O2' O2' N4 O2 -121(13) 2_554 . . . ? O2 O2' N4 O2 -151(7) 2_554 . . . ? O2 O2' N4 O2' -29(7) 2_554 . . 2_554 ? C5 N1 C1 C2 -0.7(3) . . . . ? Ag1 N1 C1 C2 179.85(15) . . . . ? N1 C1 C2 C3 -0.6(3) . . . . ? C1 C2 C3 C4 1.3(3) . . . . ? C1 C2 C3 C6 -179.68(19) . . . . ? C2 C3 C4 C5 -0.8(3) . . . . ? C6 C3 C4 C5 -179.78(19) . . . . ? C1 N1 C5 C4 1.3(3) . . . . ? Ag1 N1 C5 C4 -179.23(16) . . . . ? C3 C4 C5 N1 -0.6(3) . . . . ? C2 C3 C6 C7 50.3(3) . . . . ? C4 C3 C6 C7 -130.8(2) . . . . ? C2 C3 C6 C9 -130.8(2) . . . . ? C4 C3 C6 C9 48.2(3) . . . . ? C11 N2 C7 C6 -0.3(3) . . . . ? C11 N2 C7 C8 177.9(2) . . . . ? C9 C6 C7 N2 2.6(3) . . . . ? C3 C6 C7 N2 -178.43(19) . . . . ? C9 C6 C7 C8 -175.4(2) . . . . ? C3 C6 C7 C8 3.6(4) . . . . ? C7 C6 C9 C10 -1.5(3) . . . . ? C3 C6 C9 C10 179.54(19) . . . . ? C6 C9 C10 C12 179.86(19) . . . . ? C6 C9 C10 C11 -2.0(3) . . . . ? C7 N2 C11 O1 176.7(2) . . . . ? C7 N2 C11 C10 -3.0(3) . . . . ? C9 C10 C11 O1 -175.7(2) . . . . ? C12 C10 C11 O1 2.5(3) . . . . ? C9 C10 C11 N2 4.1(3) . . . . ? C12 C10 C11 N2 -177.76(18) . . . . ? C9 C10 C12 N3 -155(100) . . . . ? C11 C10 C12 N3 27(32) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.667 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.053 data_4 _database_code_depnum_ccdc_archive 'CCDC 706596' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H22 Ag B F4 N6 O3' _chemical_formula_weight 649.17 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' 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' _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 9.9336(7) _cell_length_b 10.1696(7) _cell_length_c 13.7544(9) _cell_angle_alpha 103.3460(10) _cell_angle_beta 91.1900(10) _cell_angle_gamma 97.5140(10) _cell_volume 1338.47(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6750 _exptl_absorpt_correction_T_max 0.8466 _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 7441 _diffrn_reflns_av_R_equivalents 0.0109 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4901 _reflns_number_gt 4486 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The bond lengths N2-H26 and N5-H27 were restrained to target value of 0.90(1) \%A. ; _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^)+(0.0513P)^2^+2.3268P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4901 _refine_ls_number_parameters 373 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _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 Ag1 Ag 0.10553(3) 0.17943(3) 0.09987(2) 0.05002(12) Uani 1 1 d . . . N1 N 0.2226(3) 0.2637(3) -0.0053(2) 0.0435(6) Uani 1 1 d . . . N2 N 0.5325(3) 0.5583(3) -0.3276(2) 0.0434(6) Uani 1 1 d D . . N3 N 0.9653(3) 0.4537(5) -0.2404(4) 0.0837(12) Uani 1 1 d . . . N4 N 0.0013(3) 0.0929(3) 0.2095(2) 0.0455(6) Uani 1 1 d . . . N5 N -0.3355(3) -0.2434(3) 0.4952(2) 0.0435(6) Uani 1 1 d D . . N6 N -0.7615(3) -0.1325(4) 0.3967(3) 0.0714(10) Uani 1 1 d . . . O1 O 0.7465(2) 0.6097(3) -0.3758(2) 0.0657(8) Uani 1 1 d . . . O2 O -0.5535(2) -0.3002(3) 0.5338(2) 0.0585(7) Uani 1 1 d . . . O3 O 0.5292(6) 0.1043(8) 0.2177(5) 0.160(2) Uani 1 1 d . . . H3 H 0.5655 0.1240 0.1673 0.241 Uiso 1 1 calc R . . B1 B 0.7746(5) 0.1962(5) 0.0083(4) 0.0594(11) Uani 1 1 d . . . F1 F 0.8273(3) 0.0757(2) -0.0041(2) 0.0762(7) Uani 1 1 d . . . F2 F 0.8715(4) 0.2956(3) 0.0651(4) 0.1406(17) Uani 1 1 d . . . F3 F 0.7527(4) 0.2293(4) -0.0775(3) 0.1153(12) Uani 1 1 d . . . F4 F 0.6637(4) 0.1992(5) 0.0592(4) 0.1564(19) Uani 1 1 d . . . C1 C 0.2004(3) 0.3802(3) -0.0287(3) 0.0466(8) Uani 1 1 d . . . H1 H 0.1265 0.4234 -0.0003 0.056 Uiso 1 1 calc R . . C2 C 0.2793(3) 0.4401(3) -0.0916(3) 0.0446(8) Uani 1 1 d . . . H2 H 0.2598 0.5232 -0.1053 0.053 Uiso 1 1 calc R . . C3 C 0.3881(3) 0.3795(3) -0.1354(2) 0.0348(6) Uani 1 1 d . . . C4 C 0.4092(3) 0.2576(3) -0.1118(2) 0.0415(7) Uani 1 1 d . . . H4 H 0.4814 0.2112 -0.1399 0.050 Uiso 1 1 calc R . . C5 C 0.3259(3) 0.2042(3) -0.0478(3) 0.0459(8) Uani 1 1 d . . . H5 H 0.3426 0.1208 -0.0330 0.055 Uiso 1 1 calc R . . C6 C 0.4807(3) 0.4396(3) -0.2014(2) 0.0347(6) Uani 1 1 d . . . C7 C 0.6202(3) 0.4270(3) -0.1953(2) 0.0390(7) Uani 1 1 d . . . H7 H 0.6511 0.3792 -0.1493 0.047 Uiso 1 1 calc R . . C8 C 0.7124(3) 0.4806(3) -0.2526(2) 0.0415(7) Uani 1 1 d . . . C9 C 0.6700(3) 0.5536(4) -0.3232(3) 0.0457(8) Uani 1 1 d . . . C10 C 0.2959(3) 0.5278(4) -0.2935(3) 0.0483(8) Uani 1 1 d . . . H10A H 0.2768 0.6139 -0.2505 0.072 Uiso 1 1 calc R . . H10B H 0.2323 0.4521 -0.2810 0.072 Uiso 1 1 calc R . . H10C H 0.2852 0.5312 -0.3638 0.072 Uiso 1 1 calc R . . C11 C 0.4392(3) 0.5066(3) -0.2708(2) 0.0366(6) Uani 1 1 d . . . C12 C 0.8539(4) 0.4663(4) -0.2461(3) 0.0538(9) Uani 1 1 d . . . C13 C 0.0064(3) -0.0369(4) 0.2127(3) 0.0477(8) Uani 1 1 d . . . H13 H 0.0715 -0.0841 0.1746 0.057 Uiso 1 1 calc R . . C14 C -0.0777(3) -0.1053(4) 0.2682(3) 0.0451(7) Uani 1 1 d . . . H14 H -0.0702 -0.1975 0.2682 0.054 Uiso 1 1 calc R . . C15 C -0.1741(3) -0.0383(3) 0.3245(2) 0.0368(6) Uani 1 1 d . . . C16 C -0.1772(3) 0.0967(3) 0.3228(3) 0.0439(7) Uani 1 1 d . . . H16 H -0.2403 0.1468 0.3611 0.053 Uiso 1 1 calc R . . C17 C -0.0887(3) 0.1587(4) 0.2654(3) 0.0486(8) Uani 1 1 d . . . H17 H -0.0920 0.2518 0.2657 0.058 Uiso 1 1 calc R . . C18 C -0.2735(3) -0.1085(3) 0.3808(2) 0.0371(6) Uani 1 1 d . . . C19 C -0.2371(3) -0.1821(3) 0.4471(2) 0.0398(7) Uani 1 1 d . . . C20 C -0.4122(3) -0.0973(3) 0.3692(2) 0.0390(7) Uani 1 1 d . . . H20 H -0.4391 -0.0443 0.3256 0.047 Uiso 1 1 calc R . . C21 C -0.5100(3) -0.1602(3) 0.4185(2) 0.0385(7) Uani 1 1 d . . . C22 C -0.4735(3) -0.2395(3) 0.4861(2) 0.0417(7) Uani 1 1 d . . . C23 C -0.0948(3) -0.1983(5) 0.4760(3) 0.0589(10) Uani 1 1 d . . . H23A H -0.0839 -0.1819 0.5490 0.088 Uiso 1 1 calc R . . H23B H -0.0302 -0.1323 0.4527 0.088 Uiso 1 1 calc R . . H23C H -0.0775 -0.2910 0.4453 0.088 Uiso 1 1 calc R . . C24 C -0.6501(3) -0.1462(4) 0.4064(3) 0.0463(8) Uani 1 1 d . . . C25 C 0.3997(6) 0.0986(8) 0.2072(6) 0.133(3) Uani 1 1 d . . . H25A H 0.3591 0.0962 0.2712 0.200 Uiso 1 1 calc R . . H25B H 0.3628 0.0161 0.1568 0.200 Uiso 1 1 calc R . . H25C H 0.3783 0.1792 0.1857 0.200 Uiso 1 1 calc R . . H26 H 0.504(4) 0.601(4) -0.373(2) 0.059(11) Uiso 1 1 d D . . H27 H -0.310(4) -0.293(3) 0.537(2) 0.059(11) Uiso 1 1 d 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 Ag1 0.04504(17) 0.06401(19) 0.05438(18) 0.03816(14) 0.02038(12) 0.00999(12) N1 0.0435(15) 0.0506(15) 0.0466(15) 0.0283(13) 0.0180(12) 0.0104(12) N2 0.0345(14) 0.0552(16) 0.0527(16) 0.0351(14) 0.0117(12) 0.0092(12) N3 0.0357(19) 0.118(3) 0.110(3) 0.053(3) 0.0096(18) 0.0114(19) N4 0.0386(14) 0.0598(17) 0.0503(16) 0.0340(14) 0.0134(12) 0.0114(12) N5 0.0355(14) 0.0586(17) 0.0458(15) 0.0318(13) 0.0085(11) 0.0041(12) N6 0.0393(18) 0.098(3) 0.081(2) 0.025(2) 0.0089(16) 0.0169(17) O1 0.0387(13) 0.093(2) 0.089(2) 0.0680(17) 0.0222(13) 0.0109(13) O2 0.0380(13) 0.0843(18) 0.0680(17) 0.0488(15) 0.0166(11) 0.0043(12) O3 0.122(4) 0.231(7) 0.166(6) 0.119(5) 0.009(4) 0.031(4) B1 0.062(3) 0.061(3) 0.064(3) 0.023(2) 0.009(2) 0.025(2) F1 0.1016(19) 0.0533(13) 0.0811(17) 0.0217(12) 0.0070(14) 0.0269(13) F2 0.123(3) 0.075(2) 0.207(4) -0.010(2) -0.060(3) 0.041(2) F3 0.144(3) 0.134(3) 0.103(2) 0.072(2) 0.013(2) 0.067(2) F4 0.120(3) 0.209(5) 0.188(4) 0.106(4) 0.098(3) 0.075(3) C1 0.0485(19) 0.0518(19) 0.0514(19) 0.0275(16) 0.0239(15) 0.0197(15) C2 0.0527(19) 0.0410(17) 0.0507(19) 0.0242(15) 0.0205(15) 0.0186(14) C3 0.0353(15) 0.0375(15) 0.0361(15) 0.0168(12) 0.0096(12) 0.0059(12) C4 0.0416(17) 0.0447(17) 0.0485(18) 0.0243(14) 0.0177(14) 0.0170(13) C5 0.0493(19) 0.0473(18) 0.053(2) 0.0308(16) 0.0184(15) 0.0146(15) C6 0.0331(15) 0.0365(15) 0.0395(16) 0.0178(12) 0.0104(12) 0.0059(12) C7 0.0365(16) 0.0415(16) 0.0449(17) 0.0218(14) 0.0069(13) 0.0050(13) C8 0.0320(15) 0.0498(18) 0.0494(18) 0.0242(15) 0.0072(13) 0.0060(13) C9 0.0352(16) 0.0548(19) 0.057(2) 0.0315(16) 0.0146(14) 0.0066(14) C10 0.0351(16) 0.063(2) 0.060(2) 0.0352(18) 0.0122(14) 0.0135(15) C11 0.0334(15) 0.0399(16) 0.0424(16) 0.0196(13) 0.0115(12) 0.0067(12) C12 0.0381(19) 0.067(2) 0.065(2) 0.0343(19) 0.0082(16) 0.0040(16) C13 0.0422(18) 0.059(2) 0.052(2) 0.0288(16) 0.0194(15) 0.0144(15) C14 0.0434(17) 0.0503(18) 0.0499(19) 0.0257(15) 0.0148(14) 0.0102(14) C15 0.0315(14) 0.0509(17) 0.0337(15) 0.0220(13) 0.0051(12) 0.0046(12) C16 0.0396(17) 0.0528(19) 0.0492(19) 0.0271(15) 0.0137(14) 0.0137(14) C17 0.0462(18) 0.054(2) 0.059(2) 0.0345(17) 0.0168(15) 0.0151(15) C18 0.0349(15) 0.0468(17) 0.0336(15) 0.0176(13) 0.0083(12) 0.0048(13) C19 0.0326(15) 0.0515(18) 0.0398(16) 0.0215(14) 0.0056(12) 0.0025(13) C20 0.0385(16) 0.0503(18) 0.0330(15) 0.0174(13) 0.0059(12) 0.0094(13) C21 0.0336(15) 0.0485(17) 0.0353(16) 0.0131(13) 0.0075(12) 0.0055(13) C22 0.0346(16) 0.0525(18) 0.0422(17) 0.0202(14) 0.0092(13) 0.0042(13) C23 0.0346(17) 0.088(3) 0.068(2) 0.051(2) 0.0013(16) 0.0021(17) C24 0.0385(18) 0.060(2) 0.0428(18) 0.0159(15) 0.0079(13) 0.0074(15) C25 0.081(4) 0.129(6) 0.172(7) -0.006(5) -0.047(4) 0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.134(3) . ? Ag1 N1 2.135(2) . ? N1 C5 1.336(4) . ? N1 C1 1.341(4) . ? N2 C11 1.356(4) . ? N2 C9 1.373(4) . ? N2 H26 0.894(10) . ? N3 C12 1.133(5) . ? N4 C17 1.337(4) . ? N4 C13 1.339(4) . ? N5 C19 1.356(4) . ? N5 C22 1.380(4) . ? N5 H27 0.899(10) . ? N6 C24 1.142(5) . ? O1 C9 1.236(4) . ? O2 C22 1.235(4) . ? O3 C25 1.284(7) . ? O3 H3 0.8400 . ? B1 F4 1.317(6) . ? B1 F3 1.320(6) . ? B1 F1 1.371(5) . ? B1 F2 1.382(6) . ? C1 C2 1.371(4) . ? C1 H1 0.9500 . ? C2 C3 1.393(4) . ? C2 H2 0.9500 . ? C3 C4 1.392(4) . ? C3 C6 1.480(4) . ? C4 C5 1.374(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C11 1.379(4) . ? C6 C7 1.411(4) . ? C7 C8 1.362(4) . ? C7 H7 0.9500 . ? C8 C12 1.435(5) . ? C8 C9 1.438(4) . ? C10 C11 1.504(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C13 C14 1.373(4) . ? C13 H13 0.9500 . ? C14 C15 1.392(4) . ? C14 H14 0.9500 . ? C15 C16 1.383(4) . ? C15 C18 1.479(4) . ? C16 C17 1.381(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.377(4) . ? C18 C20 1.406(4) . ? C19 C23 1.499(4) . ? C20 C21 1.370(4) . ? C20 H20 0.9500 . ? C21 C24 1.427(5) . ? C21 C22 1.434(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 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 N4 Ag1 N1 176.05(10) . . ? C5 N1 C1 116.9(3) . . ? C5 N1 Ag1 120.7(2) . . ? C1 N1 Ag1 122.3(2) . . ? C11 N2 C9 126.6(3) . . ? C11 N2 H26 119(3) . . ? C9 N2 H26 115(3) . . ? C17 N4 C13 117.4(3) . . ? C17 N4 Ag1 120.6(2) . . ? C13 N4 Ag1 121.0(2) . . ? C19 N5 C22 126.7(3) . . ? C19 N5 H27 118(3) . . ? C22 N5 H27 115(3) . . ? C25 O3 H3 109.5 . . ? F4 B1 F3 110.0(4) . . ? F4 B1 F1 113.6(4) . . ? F3 B1 F1 112.5(4) . . ? F4 B1 F2 106.1(5) . . ? F3 B1 F2 108.0(4) . . ? F1 B1 F2 106.2(4) . . ? N1 C1 C2 123.2(3) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 120.2(3) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 116.2(3) . . ? C4 C3 C6 120.2(3) . . ? C2 C3 C6 123.6(3) . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C5 C4 123.3(3) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C11 C6 C7 117.0(3) . . ? C11 C6 C3 124.0(3) . . ? C7 C6 C3 118.9(3) . . ? C8 C7 C6 122.6(3) . . ? C8 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? C7 C8 C12 122.1(3) . . ? C7 C8 C9 120.5(3) . . ? C12 C8 C9 117.4(3) . . ? O1 C9 N2 120.9(3) . . ? O1 C9 C8 125.2(3) . . ? N2 C9 C8 113.9(3) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C6 119.4(3) . . ? N2 C11 C10 114.0(3) . . ? C6 C11 C10 126.6(3) . . ? N3 C12 C8 179.2(4) . . ? N4 C13 C14 123.4(3) . . ? N4 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C13 C14 C15 119.4(3) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 117.2(3) . . ? C16 C15 C18 120.6(3) . . ? C14 C15 C18 122.1(3) . . ? C17 C16 C15 120.0(3) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? N4 C17 C16 122.6(3) . . ? N4 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C19 C18 C20 117.5(3) . . ? C19 C18 C15 123.3(3) . . ? C20 C18 C15 119.2(3) . . ? N5 C19 C18 119.1(3) . . ? N5 C19 C23 114.8(3) . . ? C18 C19 C23 126.1(3) . . ? C21 C20 C18 122.4(3) . . ? C21 C20 H20 118.8 . . ? C18 C20 H20 118.8 . . ? C20 C21 C24 121.4(3) . . ? C20 C21 C22 120.5(3) . . ? C24 C21 C22 118.0(3) . . ? O2 C22 N5 120.7(3) . . ? O2 C22 C21 125.6(3) . . ? N5 C22 C21 113.7(3) . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C24 C21 178.7(4) . . ? O3 C25 H25A 109.5 . . ? O3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 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 N4 Ag1 N1 C5 42.7(17) . . . . ? N4 Ag1 N1 C1 -134.5(15) . . . . ? N1 Ag1 N4 C17 128.6(15) . . . . ? N1 Ag1 N4 C13 -62.8(17) . . . . ? C5 N1 C1 C2 -1.1(5) . . . . ? Ag1 N1 C1 C2 176.2(3) . . . . ? N1 C1 C2 C3 0.5(6) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C1 C2 C3 C6 -178.0(3) . . . . ? C2 C3 C4 C5 -0.6(5) . . . . ? C6 C3 C4 C5 177.8(3) . . . . ? C1 N1 C5 C4 0.9(5) . . . . ? Ag1 N1 C5 C4 -176.4(3) . . . . ? C3 C4 C5 N1 -0.1(6) . . . . ? C4 C3 C6 C11 143.4(3) . . . . ? C2 C3 C6 C11 -38.3(5) . . . . ? C4 C3 C6 C7 -35.6(4) . . . . ? C2 C3 C6 C7 142.6(3) . . . . ? C11 C6 C7 C8 1.6(5) . . . . ? C3 C6 C7 C8 -179.3(3) . . . . ? C6 C7 C8 C12 -179.6(3) . . . . ? C6 C7 C8 C9 0.0(5) . . . . ? C11 N2 C9 O1 -176.8(4) . . . . ? C11 N2 C9 C8 2.6(5) . . . . ? C7 C8 C9 O1 177.4(4) . . . . ? C12 C8 C9 O1 -3.0(6) . . . . ? C7 C8 C9 N2 -2.0(5) . . . . ? C12 C8 C9 N2 177.6(3) . . . . ? C9 N2 C11 C6 -1.1(5) . . . . ? C9 N2 C11 C10 -179.9(3) . . . . ? C7 C6 C11 N2 -1.1(5) . . . . ? C3 C6 C11 N2 179.9(3) . . . . ? C7 C6 C11 C10 177.5(3) . . . . ? C3 C6 C11 C10 -1.5(5) . . . . ? C7 C8 C12 N3 18(40) . . . . ? C9 C8 C12 N3 -162(40) . . . . ? C17 N4 C13 C14 1.6(5) . . . . ? Ag1 N4 C13 C14 -167.4(3) . . . . ? N4 C13 C14 C15 0.1(6) . . . . ? C13 C14 C15 C16 -1.4(5) . . . . ? C13 C14 C15 C18 176.0(3) . . . . ? C14 C15 C16 C17 1.1(5) . . . . ? C18 C15 C16 C17 -176.4(3) . . . . ? C13 N4 C17 C16 -1.9(5) . . . . ? Ag1 N4 C17 C16 167.1(3) . . . . ? C15 C16 C17 N4 0.6(5) . . . . ? C16 C15 C18 C19 -130.5(4) . . . . ? C14 C15 C18 C19 52.1(5) . . . . ? C16 C15 C18 C20 47.6(4) . . . . ? C14 C15 C18 C20 -129.8(3) . . . . ? C22 N5 C19 C18 -0.7(5) . . . . ? C22 N5 C19 C23 177.0(3) . . . . ? C20 C18 C19 N5 2.1(5) . . . . ? C15 C18 C19 N5 -179.8(3) . . . . ? C20 C18 C19 C23 -175.4(3) . . . . ? C15 C18 C19 C23 2.8(6) . . . . ? C19 C18 C20 C21 -2.2(5) . . . . ? C15 C18 C20 C21 179.6(3) . . . . ? C18 C20 C21 C24 179.3(3) . . . . ? C18 C20 C21 C22 0.9(5) . . . . ? C19 N5 C22 O2 179.7(3) . . . . ? C19 N5 C22 C21 -0.5(5) . . . . ? C20 C21 C22 O2 -179.8(3) . . . . ? C24 C21 C22 O2 1.7(5) . . . . ? C20 C21 C22 N5 0.5(5) . . . . ? C24 C21 C22 N5 -178.0(3) . . . . ? C20 C21 C24 N6 -42(18) . . . . ? C22 C21 C24 N6 136(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H27 O1 0.899(10) 1.845(11) 2.743(4) 178(4) 1_446 N2 H26 O2 0.894(10) 1.927(11) 2.820(4) 177(4) 1_664 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.933 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.072 data_5 _database_code_depnum_ccdc_archive 'CCDC 706597' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Ag2 B2 F8 N8 S2' _chemical_formula_weight 869.93 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' B B 0.0013 0.0007 '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' 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' 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 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 6.2905(5) _cell_length_b 22.8069(19) _cell_length_c 10.1479(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.1730(10) _cell_angle_gamma 90.00 _cell_volume 1444.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4927 _exptl_absorpt_correction_T_max 0.7527 _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 7979 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2696 _reflns_number_gt 2412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. F Atoms of BF4- anion are disordered over two positions and all B-F bond lengths were restrained to a target value of 1.35(1) \%A. Displacement parameters for disordered F atoms were also subjected to restraints. ; _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^)+(0.0509P)^2^+3.1243P] 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 2696 _refine_ls_number_parameters 221 _refine_ls_number_restraints 428 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.106 _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 Ag1 Ag 1.31611(6) 0.541888(16) -0.08367(4) 0.05414(17) Uani 1 1 d U . 5 N1 N 1.4017(6) 0.63487(17) -0.0122(4) 0.0449(8) Uani 1 1 d U A 5 N2 N 1.0514(7) 0.57665(17) 0.0605(4) 0.0506(9) Uani 1 1 d U A 5 N3 N 0.8826(7) 0.55207(17) 0.1142(4) 0.0499(9) Uani 1 1 d U . 5 N4 N 0.5310(6) 0.51750(17) 0.2292(4) 0.0482(9) Uani 1 1 d U . 5 C1 C 1.5599(8) 0.6654(2) -0.0570(5) 0.0539(11) Uani 1 1 d U A 5 H1 H 1.6429 0.6470 -0.1171 0.065 Uiso 1 1 calc R A 5 C2 C 1.6073(9) 0.7225(2) -0.0194(6) 0.0629(13) Uani 1 1 d U A 5 H2 H 1.7208 0.7429 -0.0531 0.076 Uiso 1 1 calc R A 5 C3 C 1.4876(10) 0.7495(2) 0.0675(7) 0.0706(15) Uani 1 1 d U A 5 H3 H 1.5190 0.7885 0.0962 0.085 Uiso 1 1 calc R A 5 C4 C 1.3223(9) 0.7193(2) 0.1123(6) 0.0608(13) Uani 1 1 d U A 5 H4 H 1.2368 0.7372 0.1718 0.073 Uiso 1 1 calc R A 5 C5 C 1.2818(7) 0.66222(19) 0.0698(4) 0.0436(9) Uani 1 1 d U A 5 C6 C 1.1064(7) 0.62754(18) 0.1121(4) 0.0416(9) Uani 1 1 d U A 5 C7 C 0.8146(7) 0.58443(18) 0.2046(4) 0.0412(9) Uani 1 1 d U A 5 C8 C 0.6312(7) 0.56701(19) 0.2737(4) 0.0415(9) Uani 1 1 d U A 5 C9 C 0.5665(8) 0.5996(2) 0.3754(5) 0.0541(11) Uani 1 1 d U A 5 H9 H 0.6396 0.6346 0.4045 0.065 Uiso 1 1 calc R A 5 C10 C 0.3928(9) 0.5803(3) 0.4344(5) 0.0608(13) Uani 1 1 d U A 5 H10 H 0.3464 0.6016 0.5061 0.073 Uiso 1 1 calc R A 5 C11 C 0.2895(8) 0.5310(3) 0.3895(6) 0.0591(13) Uani 1 1 d U A 5 H11 H 0.1687 0.5175 0.4283 0.071 Uiso 1 1 calc R A 5 C12 C 0.3614(8) 0.5007(2) 0.2869(6) 0.0581(12) Uani 1 1 d U A 5 H12 H 0.2871 0.4661 0.2556 0.070 Uiso 1 1 calc R A 5 S1 S 0.95316(19) 0.64908(5) 0.23277(12) 0.0460(3) Uani 1 1 d U A 5 B1 B 0.9903(10) 0.6446(3) 0.6703(5) 0.0691(17) Uani 0.729(4) 1 d PDU B 1 F1 F 0.9958(10) 0.6675(3) 0.5460(5) 0.0809(15) Uani 0.729(4) 1 d PDU B 1 F2 F 0.7698(8) 0.6324(3) 0.6751(6) 0.1008(17) Uani 0.729(4) 1 d PDU B 1 F3 F 1.0212(10) 0.6873(3) 0.7689(5) 0.0966(16) Uani 0.729(4) 1 d PDU B 1 F4 F 1.0923(13) 0.5944(3) 0.6915(7) 0.140(3) Uani 0.729(4) 1 d PDU B 1 B1' B 0.9903(10) 0.6446(3) 0.6703(5) 0.0691(17) Uani 0.271(4) 1 d PDU B 2 F1' F 0.924(3) 0.6784(7) 0.5698(13) 0.0809(15) Uani 0.271(4) 1 d PDU B 2 F2' F 0.919(2) 0.6242(7) 0.7750(12) 0.1008(17) Uani 0.271(4) 1 d PDU B 2 F3' F 1.2162(15) 0.6484(7) 0.6952(13) 0.0966(16) Uani 0.271(4) 1 d PDU B 2 F4' F 0.993(3) 0.5891(5) 0.6032(16) 0.140(3) Uani 0.271(4) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0579(3) 0.0469(2) 0.0604(3) -0.01275(16) 0.01823(19) -0.00386(15) N1 0.046(2) 0.047(2) 0.0423(19) 0.0027(16) 0.0061(16) -0.0001(16) N2 0.053(2) 0.044(2) 0.058(2) -0.0072(17) 0.0208(18) -0.0031(17) N3 0.053(2) 0.045(2) 0.054(2) -0.0106(17) 0.0172(18) -0.0017(17) N4 0.050(2) 0.044(2) 0.053(2) 0.0003(17) 0.0139(17) 0.0001(17) C1 0.054(3) 0.060(3) 0.050(3) 0.003(2) 0.013(2) -0.001(2) C2 0.060(3) 0.059(3) 0.070(3) 0.011(3) 0.013(3) -0.013(2) C3 0.078(4) 0.046(3) 0.090(4) 0.004(3) 0.019(3) -0.007(3) C4 0.066(3) 0.041(2) 0.078(3) -0.003(2) 0.020(3) 0.002(2) C5 0.045(2) 0.040(2) 0.045(2) 0.0029(18) 0.0049(18) 0.0028(18) C6 0.043(2) 0.039(2) 0.043(2) -0.0015(18) 0.0074(18) 0.0057(18) C7 0.043(2) 0.040(2) 0.040(2) -0.0024(17) 0.0046(17) 0.0039(17) C8 0.039(2) 0.044(2) 0.041(2) 0.0025(18) 0.0024(17) 0.0055(18) C9 0.050(3) 0.060(3) 0.053(3) -0.009(2) 0.011(2) 0.003(2) C10 0.059(3) 0.071(3) 0.054(3) 0.000(2) 0.016(2) 0.014(3) C11 0.052(3) 0.066(3) 0.063(3) 0.019(3) 0.020(2) 0.011(2) C12 0.055(3) 0.050(3) 0.072(3) 0.009(2) 0.018(2) -0.002(2) S1 0.0481(6) 0.0412(6) 0.0500(6) -0.0090(5) 0.0113(5) 0.0002(5) B1 0.075(4) 0.074(4) 0.061(3) 0.014(3) 0.019(3) -0.006(3) F1 0.082(4) 0.108(4) 0.055(3) 0.006(3) 0.022(2) 0.012(3) F2 0.088(4) 0.118(4) 0.102(4) 0.009(3) 0.034(3) -0.017(3) F3 0.115(4) 0.107(4) 0.067(3) -0.012(3) 0.011(3) -0.032(3) F4 0.154(6) 0.156(5) 0.110(5) 0.031(5) 0.010(4) 0.075(5) B1' 0.075(4) 0.074(4) 0.061(3) 0.014(3) 0.019(3) -0.006(3) F1' 0.082(4) 0.108(4) 0.055(3) 0.006(3) 0.022(2) 0.012(3) F2' 0.088(4) 0.118(4) 0.102(4) 0.009(3) 0.034(3) -0.017(3) F3' 0.115(4) 0.107(4) 0.067(3) -0.012(3) 0.011(3) -0.032(3) F4' 0.154(6) 0.156(5) 0.110(5) 0.031(5) 0.010(4) 0.075(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 Ag1 N1 2.284(4) . ? Ag1 N4 2.301(4) 3_765 ? Ag1 N2 2.480(4) . ? Ag1 N3 2.481(4) 3_765 ? Ag1 Ag1 3.3024(8) 3_865 ? N1 C1 1.340(6) . ? N1 C5 1.344(6) . ? N2 C6 1.302(6) . ? N2 N3 1.372(5) . ? N3 C7 1.291(6) . ? N3 Ag1 2.481(4) 3_765 ? N4 C12 1.336(6) . ? N4 C8 1.343(6) . ? N4 Ag1 2.301(4) 3_765 ? C1 C2 1.379(8) . ? C1 H1 0.9500 . ? C2 C3 1.374(8) . ? C2 H2 0.9500 . ? C3 C4 1.371(8) . ? C3 H3 0.9500 . ? C4 C5 1.384(7) . ? C4 H4 0.9500 . ? C5 C6 1.465(6) . ? C6 S1 1.722(4) . ? C7 C8 1.478(6) . ? C7 S1 1.718(4) . ? C8 C9 1.374(6) . ? C9 C10 1.382(7) . ? C9 H9 0.9500 . ? C10 C11 1.349(8) . ? C10 H10 0.9500 . ? C11 C12 1.373(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? B1 F4 1.317(7) . ? B1 F1 1.370(6) . ? B1 F3 1.393(7) . ? B1 F2 1.421(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 N1 Ag1 N4 130.49(13) . 3_765 ? N1 Ag1 N2 70.43(13) . . ? N4 Ag1 N2 158.75(14) 3_765 . ? N1 Ag1 N3 159.55(13) . 3_765 ? N4 Ag1 N3 69.88(13) 3_765 3_765 ? N2 Ag1 N3 89.13(13) . 3_765 ? N1 Ag1 Ag1 104.57(10) . 3_865 ? N4 Ag1 Ag1 70.57(10) 3_765 3_865 ? N2 Ag1 Ag1 111.14(10) . 3_865 ? N3 Ag1 Ag1 82.76(10) 3_765 3_865 ? C1 N1 C5 117.8(4) . . ? C1 N1 Ag1 122.1(3) . . ? C5 N1 Ag1 119.9(3) . . ? C6 N2 N3 112.6(4) . . ? C6 N2 Ag1 111.0(3) . . ? N3 N2 Ag1 135.5(3) . . ? C7 N3 N2 113.0(4) . . ? C7 N3 Ag1 112.1(3) . 3_765 ? N2 N3 Ag1 134.9(3) . 3_765 ? C12 N4 C8 117.5(4) . . ? C12 N4 Ag1 122.2(3) . 3_765 ? C8 N4 Ag1 119.6(3) . 3_765 ? N1 C1 C2 122.8(5) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.8(5) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C4 C3 C2 119.2(5) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.1(5) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.2(4) . . ? N1 C5 C6 115.6(4) . . ? C4 C5 C6 122.1(4) . . ? N2 C6 C5 122.4(4) . . ? N2 C6 S1 113.3(3) . . ? C5 C6 S1 124.3(3) . . ? N3 C7 C8 122.1(4) . . ? N3 C7 S1 113.7(3) . . ? C8 C7 S1 124.2(3) . . ? N4 C8 C9 122.4(4) . . ? N4 C8 C7 115.4(4) . . ? C9 C8 C7 122.2(4) . . ? C8 C9 C10 118.5(5) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 119.5(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 119.1(5) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? N4 C12 C11 123.0(5) . . ? N4 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? C7 S1 C6 87.4(2) . . ? F4 B1 F1 114.4(6) . . ? F4 B1 F3 118.0(6) . . ? F1 B1 F3 112.2(5) . . ? F4 B1 F2 106.4(6) . . ? F1 B1 F2 104.1(5) . . ? F3 B1 F2 99.3(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 N4 Ag1 N1 C1 2.0(4) 3_765 . . . ? N2 Ag1 N1 C1 -173.7(4) . . . . ? N3 Ag1 N1 C1 -172.3(4) 3_765 . . . ? Ag1 Ag1 N1 C1 78.7(4) 3_865 . . . ? N4 Ag1 N1 C5 177.0(3) 3_765 . . . ? N2 Ag1 N1 C5 1.3(3) . . . . ? N3 Ag1 N1 C5 2.6(6) 3_765 . . . ? Ag1 Ag1 N1 C5 -106.3(3) 3_865 . . . ? N1 Ag1 N2 C6 -5.5(3) . . . . ? N4 Ag1 N2 C6 -176.4(3) 3_765 . . . ? N3 Ag1 N2 C6 174.9(3) 3_765 . . . ? Ag1 Ag1 N2 C6 93.0(3) 3_865 . . . ? N1 Ag1 N2 N3 -173.4(5) . . . . ? N4 Ag1 N2 N3 15.7(7) 3_765 . . . ? N3 Ag1 N2 N3 7.0(5) 3_765 . . . ? Ag1 Ag1 N2 N3 -74.9(5) 3_865 . . . ? C6 N2 N3 C7 -0.2(6) . . . . ? Ag1 N2 N3 C7 167.5(3) . . . . ? C6 N2 N3 Ag1 -177.7(3) . . . 3_765 ? Ag1 N2 N3 Ag1 -10.0(7) . . . 3_765 ? C5 N1 C1 C2 1.9(7) . . . . ? Ag1 N1 C1 C2 177.0(4) . . . . ? N1 C1 C2 C3 0.0(8) . . . . ? C1 C2 C3 C4 -1.2(9) . . . . ? C2 C3 C4 C5 0.6(9) . . . . ? C1 N1 C5 C4 -2.6(7) . . . . ? Ag1 N1 C5 C4 -177.7(4) . . . . ? C1 N1 C5 C6 177.9(4) . . . . ? Ag1 N1 C5 C6 2.7(5) . . . . ? C3 C4 C5 N1 1.3(8) . . . . ? C3 C4 C5 C6 -179.2(5) . . . . ? N3 N2 C6 C5 -179.7(4) . . . . ? Ag1 N2 C6 C5 9.5(5) . . . . ? N3 N2 C6 S1 0.3(5) . . . . ? Ag1 N2 C6 S1 -170.5(2) . . . . ? N1 C5 C6 N2 -8.9(6) . . . . ? C4 C5 C6 N2 171.6(5) . . . . ? N1 C5 C6 S1 171.2(3) . . . . ? C4 C5 C6 S1 -8.3(7) . . . . ? N2 N3 C7 C8 178.7(4) . . . . ? Ag1 N3 C7 C8 -3.2(5) 3_765 . . . ? N2 N3 C7 S1 0.0(5) . . . . ? Ag1 N3 C7 S1 178.11(19) 3_765 . . . ? C12 N4 C8 C9 0.7(7) . . . . ? Ag1 N4 C8 C9 -169.7(4) 3_765 . . . ? C12 N4 C8 C7 -178.7(4) . . . . ? Ag1 N4 C8 C7 10.9(5) 3_765 . . . ? N3 C7 C8 N4 -4.6(6) . . . . ? S1 C7 C8 N4 173.9(3) . . . . ? N3 C7 C8 C9 176.0(5) . . . . ? S1 C7 C8 C9 -5.4(6) . . . . ? N4 C8 C9 C10 0.4(7) . . . . ? C7 C8 C9 C10 179.8(4) . . . . ? C8 C9 C10 C11 -1.2(8) . . . . ? C9 C10 C11 C12 0.8(8) . . . . ? C8 N4 C12 C11 -1.1(8) . . . . ? Ag1 N4 C12 C11 169.1(4) 3_765 . . . ? C10 C11 C12 N4 0.4(8) . . . . ? N3 C7 S1 C6 0.1(4) . . . . ? C8 C7 S1 C6 -178.6(4) . . . . ? N2 C6 S1 C7 -0.2(4) . . . . ? C5 C6 S1 C7 179.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.331 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.086 data_6 _database_code_depnum_ccdc_archive 'CCDC 706598' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Ag2 Cl2 N8 O8 S2' _chemical_formula_weight 895.21 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' S S 0.1246 0.1234 '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' 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 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 6.3525(6) _cell_length_b 22.701(2) _cell_length_c 10.3344(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.948(2) _cell_angle_gamma 90.00 _cell_volume 1479.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4760 _exptl_absorpt_correction_T_max 0.8897 _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 9499 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3372 _reflns_number_gt 2828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. O toms of ClO4- anion are disordered over two positions and all Cl-O bond lengths were restrained to a target value of 1.44(1) \%A. Displacement parameters for disordered O atoms were also subjected to restraints. ; _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^)+(0.0580P)^2^+1.5746P] 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 3372 _refine_ls_number_parameters 221 _refine_ls_number_restraints 278 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.074 _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 Ag1 Ag 1.31300(5) 0.541127(14) -0.08479(3) 0.05765(14) Uani 1 1 d . . . N1 N 1.4124(5) 0.63334(14) -0.0092(3) 0.0463(7) Uani 1 1 d U . . N2 N 1.0613(5) 0.57670(14) 0.0619(3) 0.0529(7) Uani 1 1 d U . . N3 N 0.8932(6) 0.55258(15) 0.1146(3) 0.0533(8) Uani 1 1 d U . . N4 N 0.5422(5) 0.51953(14) 0.2281(3) 0.0520(7) Uani 1 1 d U . . S1 S 0.96898(15) 0.64946(4) 0.23239(9) 0.0485(2) Uani 1 1 d . . . Cl1 Cl 1.00407(19) 0.64347(5) 0.67498(10) 0.0648(3) Uani 0.736(5) 1 d PDU A 1 O1 O 1.1127(12) 0.5905(3) 0.6877(7) 0.124(2) Uani 0.736(5) 1 d PDU A 1 O2 O 1.0535(11) 0.6846(3) 0.7804(5) 0.0924(16) Uani 0.736(5) 1 d PDU A 1 O3 O 1.0149(10) 0.6730(3) 0.5528(4) 0.0754(14) Uani 0.736(5) 1 d PDU A 1 O4 O 0.7765(7) 0.6298(2) 0.6769(5) 0.0864(15) Uani 0.736(5) 1 d PDU A 1 Cl1' Cl 1.00407(19) 0.64347(5) 0.67498(10) 0.0648(3) Uani 0.264(5) 1 d PDU A 2 O1' O 0.935(3) 0.5974(6) 0.7515(16) 0.124(2) Uani 0.264(5) 1 d PDU A 2 O2' O 1.2415(13) 0.6397(7) 0.6993(12) 0.0924(16) Uani 0.264(5) 1 d PDU A 2 O3' O 0.963(3) 0.6544(8) 0.5418(9) 0.0754(14) Uani 0.264(5) 1 d PDU A 2 O4' O 0.965(3) 0.6980(5) 0.7464(15) 0.0864(15) Uani 0.264(5) 1 d PDU A 2 C1 C 1.5705(7) 0.66352(19) -0.0530(4) 0.0559(9) Uani 1 1 d U . . H1 H 1.6509 0.6449 -0.1131 0.067 Uiso 1 1 calc R . . C2 C 1.6219(7) 0.7205(2) -0.0150(5) 0.0653(11) Uani 1 1 d U . . H2 H 1.7360 0.7403 -0.0477 0.078 Uiso 1 1 calc R . . C3 C 1.5066(8) 0.7478(2) 0.0702(6) 0.0746(13) Uani 1 1 d U . . H3 H 1.5403 0.7868 0.0987 0.089 Uiso 1 1 calc R . . C4 C 1.3406(7) 0.71807(18) 0.1145(5) 0.0636(11) Uani 1 1 d U . . H4 H 1.2575 0.7365 0.1734 0.076 Uiso 1 1 calc R . . C5 C 1.2959(6) 0.66126(16) 0.0724(4) 0.0460(8) Uani 1 1 d U . . C6 C 1.1194(6) 0.62727(16) 0.1133(3) 0.0442(7) Uani 1 1 d U . . C7 C 0.8271(6) 0.58530(16) 0.2040(3) 0.0440(7) Uani 1 1 d U . . C8 C 0.6455(6) 0.56830(17) 0.2731(3) 0.0447(7) Uani 1 1 d U . . C9 C 0.5851(6) 0.6010(2) 0.3740(4) 0.0567(9) Uani 1 1 d U . . H9 H 0.6617 0.6354 0.4031 0.068 Uiso 1 1 calc R . . C10 C 0.4130(8) 0.5835(2) 0.4323(4) 0.0648(11) Uani 1 1 d U . . H10 H 0.3689 0.6055 0.5025 0.078 Uiso 1 1 calc R . . C11 C 0.3054(7) 0.5337(2) 0.3880(5) 0.0618(11) Uani 1 1 d U . . H11 H 0.1859 0.5205 0.4270 0.074 Uiso 1 1 calc R . . C12 C 0.3742(7) 0.50335(19) 0.2857(5) 0.0597(10) Uani 1 1 d U . . H12 H 0.2982 0.4691 0.2546 0.072 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 Ag1 0.0645(2) 0.0494(2) 0.0625(2) -0.01205(13) 0.02161(16) -0.00431(13) N1 0.0478(16) 0.0490(17) 0.0428(15) 0.0021(12) 0.0076(12) 0.0009(13) N2 0.0571(19) 0.0473(17) 0.0581(18) -0.0077(14) 0.0225(15) -0.0033(14) N3 0.0580(19) 0.0482(17) 0.0566(18) -0.0085(14) 0.0190(15) -0.0056(14) N4 0.0544(19) 0.0426(16) 0.0616(19) 0.0025(14) 0.0177(15) 0.0031(14) S1 0.0512(5) 0.0453(5) 0.0506(5) -0.0087(4) 0.0120(4) 0.0012(4) Cl1 0.0680(7) 0.0739(7) 0.0543(6) 0.0131(5) 0.0147(5) -0.0033(5) O1 0.142(5) 0.125(4) 0.112(4) 0.023(4) 0.041(3) 0.056(4) O2 0.098(4) 0.111(4) 0.063(3) -0.004(3) -0.012(2) -0.007(3) O3 0.081(3) 0.083(4) 0.060(2) 0.012(2) 0.002(2) -0.031(2) O4 0.079(3) 0.092(3) 0.092(3) 0.005(3) 0.027(2) -0.011(3) Cl1' 0.0680(7) 0.0739(7) 0.0543(6) 0.0131(5) 0.0147(5) -0.0033(5) O1' 0.142(5) 0.125(4) 0.112(4) 0.023(4) 0.041(3) 0.056(4) O2' 0.098(4) 0.111(4) 0.063(3) -0.004(3) -0.012(2) -0.007(3) O3' 0.081(3) 0.083(4) 0.060(2) 0.012(2) 0.002(2) -0.031(2) O4' 0.079(3) 0.092(3) 0.092(3) 0.005(3) 0.027(2) -0.011(3) C1 0.052(2) 0.062(2) 0.055(2) 0.0069(18) 0.0128(17) -0.0015(18) C2 0.059(2) 0.063(3) 0.076(3) 0.012(2) 0.015(2) -0.009(2) C3 0.073(3) 0.050(2) 0.102(4) 0.000(2) 0.017(3) -0.012(2) C4 0.068(3) 0.046(2) 0.080(3) -0.0054(19) 0.021(2) 0.0004(19) C5 0.0478(19) 0.0416(18) 0.0485(18) 0.0052(14) 0.0053(15) 0.0040(15) C6 0.0477(18) 0.0431(18) 0.0423(16) 0.0004(14) 0.0069(14) 0.0056(15) C7 0.0433(18) 0.0440(18) 0.0449(17) 0.0006(14) 0.0059(14) 0.0053(14) C8 0.0429(18) 0.0480(19) 0.0429(17) 0.0042(14) 0.0037(14) 0.0077(15) C9 0.049(2) 0.071(3) 0.052(2) -0.0092(18) 0.0125(16) 0.0004(19) C10 0.061(3) 0.083(3) 0.053(2) -0.003(2) 0.0194(18) 0.012(2) C11 0.051(2) 0.071(3) 0.067(3) 0.017(2) 0.0219(19) 0.0084(19) C12 0.057(2) 0.050(2) 0.075(3) 0.0083(19) 0.020(2) -0.0037(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.294(3) 3_765 ? Ag1 N1 2.296(3) . ? Ag1 N2 2.468(3) . ? Ag1 N3 2.498(3) 3_765 ? Ag1 Ag1 3.3459(7) 3_865 ? N1 C1 1.339(5) . ? N1 C5 1.346(5) . ? N2 C6 1.300(5) . ? N2 N3 1.370(5) . ? N3 C7 1.295(5) . ? N3 Ag1 2.498(3) 3_765 ? N4 C12 1.336(5) . ? N4 C8 1.341(5) . ? N4 Ag1 2.294(3) 3_765 ? S1 C7 1.719(4) . ? S1 C6 1.722(4) . ? Cl1 O1 1.384(5) . ? Cl1 O3 1.439(4) . ? Cl1 O2 1.440(5) . ? Cl1 O4 1.481(4) . ? C1 C2 1.379(6) . ? C1 H1 0.9500 . ? C2 C3 1.361(7) . ? C2 H2 0.9500 . ? C3 C4 1.376(7) . ? C3 H3 0.9500 . ? C4 C5 1.379(6) . ? C4 H4 0.9500 . ? C5 C6 1.465(5) . ? C7 C8 1.479(5) . ? C8 C9 1.373(5) . ? C9 C10 1.370(6) . ? C9 H9 0.9500 . ? C10 C11 1.370(7) . ? C10 H10 0.9500 . ? C11 C12 1.377(7) . ? C11 H11 0.9500 . ? C12 H12 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 N4 Ag1 N1 130.67(11) 3_765 . ? N4 Ag1 N2 158.85(12) 3_765 . ? N1 Ag1 N2 70.41(11) . . ? N4 Ag1 N3 69.78(11) 3_765 3_765 ? N1 Ag1 N3 159.55(11) . 3_765 ? N2 Ag1 N3 89.16(11) . 3_765 ? N4 Ag1 Ag1 71.85(9) 3_765 3_865 ? N1 Ag1 Ag1 100.48(8) . 3_865 ? N2 Ag1 Ag1 109.43(8) . 3_865 ? N3 Ag1 Ag1 85.29(9) 3_765 3_865 ? C1 N1 C5 117.6(3) . . ? C1 N1 Ag1 122.5(3) . . ? C5 N1 Ag1 119.5(2) . . ? C6 N2 N3 112.7(3) . . ? C6 N2 Ag1 111.5(2) . . ? N3 N2 Ag1 135.0(2) . . ? C7 N3 N2 113.0(3) . . ? C7 N3 Ag1 111.5(2) . 3_765 ? N2 N3 Ag1 135.5(2) . 3_765 ? C12 N4 C8 117.1(4) . . ? C12 N4 Ag1 121.8(3) . 3_765 ? C8 N4 Ag1 120.1(2) . 3_765 ? C7 S1 C6 87.43(17) . . ? O1 Cl1 O3 114.4(4) . . ? O1 Cl1 O2 115.5(4) . . ? O3 Cl1 O2 109.4(3) . . ? O1 Cl1 O4 107.0(4) . . ? O3 Cl1 O4 105.1(3) . . ? O2 Cl1 O4 104.5(4) . . ? N1 C1 C2 123.0(4) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 119.0(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.1(4) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 119.4(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 122.0(4) . . ? N1 C5 C6 115.5(3) . . ? C4 C5 C6 122.5(4) . . ? N2 C6 C5 122.5(3) . . ? N2 C6 S1 113.3(3) . . ? C5 C6 S1 124.2(3) . . ? N3 C7 C8 122.3(3) . . ? N3 C7 S1 113.5(3) . . ? C8 C7 S1 124.2(3) . . ? N4 C8 C9 122.7(4) . . ? N4 C8 C7 115.2(3) . . ? C9 C8 C7 122.1(4) . . ? C10 C9 C8 119.2(4) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 119.0(4) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 118.5(4) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? N4 C12 C11 123.4(4) . . ? N4 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? 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 N4 Ag1 N1 C1 4.7(4) 3_765 . . . ? N2 Ag1 N1 C1 -173.3(3) . . . . ? N3 Ag1 N1 C1 -175.5(3) 3_765 . . . ? Ag1 Ag1 N1 C1 79.7(3) 3_865 . . . ? N4 Ag1 N1 C5 177.7(2) 3_765 . . . ? N2 Ag1 N1 C5 -0.3(3) . . . . ? N3 Ag1 N1 C5 -2.4(5) 3_765 . . . ? Ag1 Ag1 N1 C5 -107.3(3) 3_865 . . . ? N4 Ag1 N2 C6 -179.7(3) 3_765 . . . ? N1 Ag1 N2 C6 -4.0(3) . . . . ? N3 Ag1 N2 C6 175.2(3) 3_765 . . . ? Ag1 Ag1 N2 C6 90.5(3) 3_865 . . . ? N4 Ag1 N2 N3 10.9(6) 3_765 . . . ? N1 Ag1 N2 N3 -173.4(4) . . . . ? N3 Ag1 N2 N3 5.8(4) 3_765 . . . ? Ag1 Ag1 N2 N3 -78.9(4) 3_865 . . . ? C6 N2 N3 C7 0.3(5) . . . . ? Ag1 N2 N3 C7 169.6(3) . . . . ? C6 N2 N3 Ag1 -177.6(3) . . . 3_765 ? Ag1 N2 N3 Ag1 -8.3(6) . . . 3_765 ? C5 N1 C1 C2 2.2(6) . . . . ? Ag1 N1 C1 C2 175.4(3) . . . . ? N1 C1 C2 C3 -0.5(7) . . . . ? C1 C2 C3 C4 -0.9(8) . . . . ? C2 C3 C4 C5 0.5(8) . . . . ? C1 N1 C5 C4 -2.5(6) . . . . ? Ag1 N1 C5 C4 -175.9(3) . . . . ? C1 N1 C5 C6 177.5(3) . . . . ? Ag1 N1 C5 C6 4.1(4) . . . . ? C3 C4 C5 N1 1.2(7) . . . . ? C3 C4 C5 C6 -178.8(4) . . . . ? N3 N2 C6 C5 179.9(3) . . . . ? Ag1 N2 C6 C5 8.0(4) . . . . ? N3 N2 C6 S1 -0.1(4) . . . . ? Ag1 N2 C6 S1 -171.98(16) . . . . ? N1 C5 C6 N2 -8.6(5) . . . . ? C4 C5 C6 N2 171.4(4) . . . . ? N1 C5 C6 S1 171.4(3) . . . . ? C4 C5 C6 S1 -8.6(5) . . . . ? C7 S1 C6 N2 -0.1(3) . . . . ? C7 S1 C6 C5 179.9(3) . . . . ? N2 N3 C7 C8 179.2(3) . . . . ? Ag1 N3 C7 C8 -2.3(4) 3_765 . . . ? N2 N3 C7 S1 -0.4(4) . . . . ? Ag1 N3 C7 S1 178.07(16) 3_765 . . . ? C6 S1 C7 N3 0.3(3) . . . . ? C6 S1 C7 C8 -179.3(3) . . . . ? C12 N4 C8 C9 0.1(6) . . . . ? Ag1 N4 C8 C9 -169.2(3) 3_765 . . . ? C12 N4 C8 C7 -178.5(3) . . . . ? Ag1 N4 C8 C7 12.2(4) 3_765 . . . ? N3 C7 C8 N4 -6.0(5) . . . . ? S1 C7 C8 N4 173.5(3) . . . . ? N3 C7 C8 C9 175.4(4) . . . . ? S1 C7 C8 C9 -5.1(5) . . . . ? N4 C8 C9 C10 0.3(6) . . . . ? C7 C8 C9 C10 178.8(4) . . . . ? C8 C9 C10 C11 -0.2(7) . . . . ? C9 C10 C11 C12 -0.3(7) . . . . ? C8 N4 C12 C11 -0.6(6) . . . . ? Ag1 N4 C12 C11 168.5(3) 3_765 . . . ? C10 C11 C12 N4 0.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.900 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.090 data_7 _database_code_depnum_ccdc_archive 'CCDC 706599' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Ag2 F12 N8 P2 S2' _chemical_formula_weight 986.25 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 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 6.4014(4) _cell_length_b 23.1239(16) _cell_length_c 10.6375(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.0630(10) _cell_angle_gamma 90.00 _cell_volume 1565.81(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 1.592 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4973 _exptl_absorpt_correction_T_max 0.7208 _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 8569 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2905 _reflns_number_gt 2649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0331P)^2^+1.2288P] 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 2905 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Ag1 Ag 1.31930(3) 0.538312(9) -0.07893(2) 0.04920(10) Uani 1 1 d . . . N1 N 1.4128(3) 0.62913(10) -0.0085(2) 0.0429(5) Uani 1 1 d . . . N2 N 1.0754(4) 0.57143(9) 0.0716(2) 0.0454(5) Uani 1 1 d . . . N3 N 0.9066(4) 0.54829(9) 0.1224(2) 0.0456(5) Uani 1 1 d . . . N4 N 0.5484(4) 0.51784(10) 0.2285(2) 0.0451(5) Uani 1 1 d . . . S1 S 0.96546(11) 0.64651(3) 0.22496(7) 0.04543(17) Uani 1 1 d . . . C1 C 1.5668(5) 0.65892(14) -0.0542(3) 0.0539(7) Uani 1 1 d . . . H1 H 1.6482 0.6402 -0.1119 0.065 Uiso 1 1 calc R . . C2 C 1.6132(5) 0.71535(15) -0.0219(4) 0.0648(9) Uani 1 1 d . . . H2 H 1.7238 0.7351 -0.0568 0.078 Uiso 1 1 calc R . . C3 C 1.4964(6) 0.74281(15) 0.0620(4) 0.0724(10) Uani 1 1 d . . . H3 H 1.5259 0.7817 0.0866 0.087 Uiso 1 1 calc R . . C4 C 1.3361(5) 0.71284(13) 0.1095(3) 0.0611(8) Uani 1 1 d . . . H4 H 1.2534 0.7307 0.1676 0.073 Uiso 1 1 calc R . . C5 C 1.2975(4) 0.65656(11) 0.0714(2) 0.0408(6) Uani 1 1 d . . . C6 C 1.1239(4) 0.62260(11) 0.1149(2) 0.0383(5) Uani 1 1 d . . . C7 C 0.8320(4) 0.58220(11) 0.2038(2) 0.0384(5) Uani 1 1 d . . . C8 C 0.6491(4) 0.56640(11) 0.2694(2) 0.0389(5) Uani 1 1 d . . . C9 C 0.5860(4) 0.59909(13) 0.3663(3) 0.0500(7) Uani 1 1 d . . . H9 H 0.6597 0.6334 0.3928 0.060 Uiso 1 1 calc R . . C10 C 0.4142(5) 0.58155(15) 0.4249(3) 0.0561(7) Uani 1 1 d . . . H10 H 0.3685 0.6034 0.4925 0.067 Uiso 1 1 calc R . . C11 C 0.3110(5) 0.53214(14) 0.3840(3) 0.0542(7) Uani 1 1 d . . . H11 H 0.1921 0.5192 0.4225 0.065 Uiso 1 1 calc R . . C12 C 0.3821(5) 0.50167(13) 0.2865(3) 0.0538(7) Uani 1 1 d . . . H12 H 0.3097 0.4674 0.2586 0.065 Uiso 1 1 calc R . . P1 P 0.99436(11) 0.64227(3) 0.66987(7) 0.04617(18) Uani 1 1 d . . . F1 F 0.9729(4) 0.70118(11) 0.7406(3) 0.1027(9) Uani 1 1 d . . . F2 F 0.7447(3) 0.63673(9) 0.64969(18) 0.0638(5) Uani 1 1 d . . . F3 F 1.0096(4) 0.58327(10) 0.5957(3) 0.1014(8) Uani 1 1 d . . . F4 F 1.2419(3) 0.64760(11) 0.6896(2) 0.0828(6) Uani 1 1 d . . . F5 F 0.9941(4) 0.67544(12) 0.5406(2) 0.0951(8) Uani 1 1 d . . . F6 F 0.9896(3) 0.60807(12) 0.7979(2) 0.0948(8) 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 Ag1 0.04991(15) 0.04162(14) 0.05826(16) -0.01076(9) 0.01595(10) -0.00160(9) N1 0.0419(12) 0.0453(12) 0.0427(12) -0.0018(10) 0.0097(10) -0.0041(10) N2 0.0511(13) 0.0396(12) 0.0484(13) -0.0050(10) 0.0189(10) -0.0037(10) N3 0.0506(13) 0.0400(12) 0.0490(13) -0.0040(10) 0.0186(11) -0.0041(10) N4 0.0451(13) 0.0378(11) 0.0545(13) -0.0002(10) 0.0143(10) -0.0004(10) S1 0.0452(4) 0.0401(3) 0.0533(4) -0.0109(3) 0.0156(3) -0.0023(3) C1 0.0468(16) 0.0634(19) 0.0529(17) -0.0021(14) 0.0123(13) -0.0063(14) C2 0.0530(18) 0.060(2) 0.083(2) 0.0056(17) 0.0163(16) -0.0158(15) C3 0.066(2) 0.0463(17) 0.108(3) -0.0093(18) 0.024(2) -0.0140(16) C4 0.0578(18) 0.0441(16) 0.085(2) -0.0104(16) 0.0231(16) -0.0044(14) C5 0.0387(13) 0.0403(13) 0.0437(14) 0.0023(11) 0.0055(11) 0.0011(11) C6 0.0394(13) 0.0373(13) 0.0389(13) -0.0003(10) 0.0078(10) 0.0032(10) C7 0.0389(13) 0.0377(13) 0.0385(13) -0.0002(10) 0.0043(10) 0.0021(10) C8 0.0366(13) 0.0406(14) 0.0397(13) 0.0045(11) 0.0046(10) 0.0037(11) C9 0.0459(15) 0.0573(17) 0.0480(15) -0.0096(13) 0.0103(12) -0.0035(13) C10 0.0508(17) 0.073(2) 0.0467(16) -0.0057(15) 0.0156(13) 0.0048(15) C11 0.0461(16) 0.0626(19) 0.0565(17) 0.0114(14) 0.0178(13) 0.0037(14) C12 0.0501(17) 0.0451(15) 0.0690(19) 0.0045(14) 0.0187(14) -0.0033(13) P1 0.0404(4) 0.0533(4) 0.0460(4) 0.0049(3) 0.0103(3) -0.0023(3) F1 0.1011(18) 0.0851(16) 0.128(2) -0.0489(15) 0.0406(16) -0.0237(14) F2 0.0431(9) 0.0751(12) 0.0733(12) 0.0077(10) 0.0056(8) 0.0019(8) F3 0.0839(16) 0.0748(14) 0.154(2) -0.0379(15) 0.0509(15) -0.0070(12) F4 0.0405(10) 0.1284(19) 0.0807(14) 0.0054(13) 0.0118(9) -0.0117(11) F5 0.0979(17) 0.123(2) 0.0650(13) 0.0370(13) 0.0114(12) -0.0247(14) F6 0.0602(12) 0.144(2) 0.0798(14) 0.0578(15) 0.0055(10) -0.0001(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.284(2) 3_765 ? Ag1 N1 2.288(2) . ? Ag1 N2 2.473(2) . ? Ag1 N3 2.485(2) 3_765 ? Ag1 Ag1 3.2390(5) 3_865 ? N1 C1 1.335(4) . ? N1 C5 1.343(3) . ? N2 C6 1.296(3) . ? N2 N3 1.367(3) . ? N3 C7 1.296(3) . ? N3 Ag1 2.485(2) 3_765 ? N4 C12 1.339(4) . ? N4 C8 1.344(3) . ? N4 Ag1 2.284(2) 3_765 ? S1 C7 1.718(3) . ? S1 C6 1.719(3) . ? C1 C2 1.374(5) . ? C1 H1 0.9500 . ? C2 C3 1.379(5) . ? C2 H2 0.9500 . ? C3 C4 1.377(5) . ? C3 H3 0.9500 . ? C4 C5 1.378(4) . ? C4 H4 0.9500 . ? C5 C6 1.475(4) . ? C7 C8 1.471(4) . ? C8 C9 1.373(4) . ? C9 C10 1.381(4) . ? C9 H9 0.9500 . ? C10 C11 1.368(5) . ? C10 H10 0.9500 . ? C11 C12 1.371(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? P1 F1 1.569(2) . ? P1 F5 1.574(2) . ? P1 F6 1.578(2) . ? P1 F4 1.5814(19) . ? P1 F3 1.584(2) . ? P1 F2 1.5953(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 N4 Ag1 N1 130.26(8) 3_765 . ? N4 Ag1 N2 158.86(8) 3_765 . ? N1 Ag1 N2 70.44(7) . . ? N4 Ag1 N3 70.34(8) 3_765 3_765 ? N1 Ag1 N3 158.08(8) . 3_765 ? N2 Ag1 N3 88.58(7) . 3_765 ? N4 Ag1 Ag1 75.71(6) 3_765 3_865 ? N1 Ag1 Ag1 100.63(6) . 3_865 ? N2 Ag1 Ag1 107.40(6) . 3_865 ? N3 Ag1 Ag1 91.45(6) 3_765 3_865 ? C1 N1 C5 117.6(2) . . ? C1 N1 Ag1 122.14(19) . . ? C5 N1 Ag1 119.89(17) . . ? C6 N2 N3 112.7(2) . . ? C6 N2 Ag1 111.66(17) . . ? N3 N2 Ag1 135.57(16) . . ? C7 N3 N2 112.9(2) . . ? C7 N3 Ag1 111.33(17) . 3_765 ? N2 N3 Ag1 135.28(16) . 3_765 ? C12 N4 C8 117.5(2) . . ? C12 N4 Ag1 122.23(19) . 3_765 ? C8 N4 Ag1 120.02(17) . 3_765 ? C7 S1 C6 87.32(12) . . ? N1 C1 C2 123.2(3) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 118.8(3) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 118.8(3) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.6(3) . . ? N1 C5 C6 115.5(2) . . ? C4 C5 C6 121.9(2) . . ? N2 C6 C5 122.3(2) . . ? N2 C6 S1 113.6(2) . . ? C5 C6 S1 124.11(19) . . ? N3 C7 C8 122.3(2) . . ? N3 C7 S1 113.46(19) . . ? C8 C7 S1 124.21(19) . . ? N4 C8 C9 122.3(2) . . ? N4 C8 C7 115.6(2) . . ? C9 C8 C7 122.1(2) . . ? C8 C9 C10 119.3(3) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 118.9(3) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 118.8(3) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? N4 C12 C11 123.3(3) . . ? N4 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? F1 P1 F5 90.23(16) . . ? F1 P1 F6 90.59(16) . . ? F5 P1 F6 178.52(14) . . ? F1 P1 F4 90.33(14) . . ? F5 P1 F4 89.23(13) . . ? F6 P1 F4 92.00(12) . . ? F1 P1 F3 178.24(16) . . ? F5 P1 F3 88.81(16) . . ? F6 P1 F3 90.34(16) . . ? F4 P1 F3 91.13(14) . . ? F1 P1 F2 89.83(13) . . ? F5 P1 F2 90.76(12) . . ? F6 P1 F2 88.01(11) . . ? F4 P1 F2 179.83(15) . . ? F3 P1 F2 88.70(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 N4 Ag1 N1 C1 0.0(3) 3_765 . . . ? N2 Ag1 N1 C1 -174.9(2) . . . . ? N3 Ag1 N1 C1 -157.4(2) 3_765 . . . ? Ag1 Ag1 N1 C1 80.2(2) 3_865 . . . ? N4 Ag1 N1 C5 172.83(18) 3_765 . . . ? N2 Ag1 N1 C5 -2.12(19) . . . . ? N3 Ag1 N1 C5 15.4(3) 3_765 . . . ? Ag1 Ag1 N1 C5 -106.96(19) 3_865 . . . ? N4 Ag1 N2 C6 -169.9(2) 3_765 . . . ? N1 Ag1 N2 C6 -0.62(18) . . . . ? N3 Ag1 N2 C6 -174.17(19) 3_765 . . . ? Ag1 Ag1 N2 C6 94.76(18) 3_865 . . . ? N4 Ag1 N2 N3 12.4(4) 3_765 . . . ? N1 Ag1 N2 N3 -178.4(3) . . . . ? N3 Ag1 N2 N3 8.1(3) 3_765 . . . ? Ag1 Ag1 N2 N3 -83.0(3) 3_865 . . . ? C6 N2 N3 C7 -0.5(3) . . . . ? Ag1 N2 N3 C7 177.19(19) . . . . ? C6 N2 N3 Ag1 170.7(2) . . . 3_765 ? Ag1 N2 N3 Ag1 -11.5(4) . . . 3_765 ? C5 N1 C1 C2 0.9(4) . . . . ? Ag1 N1 C1 C2 173.9(3) . . . . ? N1 C1 C2 C3 0.2(5) . . . . ? C1 C2 C3 C4 -0.6(6) . . . . ? C2 C3 C4 C5 -0.2(6) . . . . ? C1 N1 C5 C4 -1.7(4) . . . . ? Ag1 N1 C5 C4 -174.9(2) . . . . ? C1 N1 C5 C6 177.5(2) . . . . ? Ag1 N1 C5 C6 4.3(3) . . . . ? C3 C4 C5 N1 1.4(5) . . . . ? C3 C4 C5 C6 -177.8(3) . . . . ? N3 N2 C6 C5 -178.5(2) . . . . ? Ag1 N2 C6 C5 3.2(3) . . . . ? N3 N2 C6 S1 0.8(3) . . . . ? Ag1 N2 C6 S1 -177.50(11) . . . . ? N1 C5 C6 N2 -5.1(4) . . . . ? C4 C5 C6 N2 174.1(3) . . . . ? N1 C5 C6 S1 175.60(19) . . . . ? C4 C5 C6 S1 -5.1(4) . . . . ? C7 S1 C6 N2 -0.6(2) . . . . ? C7 S1 C6 C5 178.7(2) . . . . ? N2 N3 C7 C8 179.4(2) . . . . ? Ag1 N3 C7 C8 6.0(3) 3_765 . . . ? N2 N3 C7 S1 0.0(3) . . . . ? Ag1 N3 C7 S1 -173.39(11) 3_765 . . . ? C6 S1 C7 N3 0.3(2) . . . . ? C6 S1 C7 C8 -179.0(2) . . . . ? C12 N4 C8 C9 -0.4(4) . . . . ? Ag1 N4 C8 C9 -174.5(2) 3_765 . . . ? C12 N4 C8 C7 179.5(2) . . . . ? Ag1 N4 C8 C7 5.3(3) 3_765 . . . ? N3 C7 C8 N4 -7.8(4) . . . . ? S1 C7 C8 N4 171.46(19) . . . . ? N3 C7 C8 C9 172.0(3) . . . . ? S1 C7 C8 C9 -8.7(4) . . . . ? N4 C8 C9 C10 0.5(4) . . . . ? C7 C8 C9 C10 -179.3(3) . . . . ? C8 C9 C10 C11 -0.4(5) . . . . ? C9 C10 C11 C12 0.2(5) . . . . ? C8 N4 C12 C11 0.2(4) . . . . ? Ag1 N4 C12 C11 174.2(2) 3_765 . . . ? C10 C11 C12 N4 -0.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.503 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.061 # Attachment 'Structure 8 new.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 706600' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Ag2 As2 F12 N8 S2' _chemical_formula_weight 1074.15 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' N N 0.0061 0.0033 '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' _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 8.4118(10) _cell_length_b 8.6865(10) _cell_length_c 11.089(2) _cell_angle_alpha 86.128(7) _cell_angle_beta 77.818(12) _cell_angle_gamma 80.346(13) _cell_volume 780.37(19) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 3.599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3067 _exptl_absorpt_correction_T_max 0.5048 _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 4192 _diffrn_reflns_av_R_equivalents 0.0133 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2707 _reflns_number_gt 2403 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0574P)^2^+0.1055P] 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 2707 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Ag1 Ag 0.78054(4) -0.05249(4) 0.42334(3) 0.05265(14) Uani 1 1 d . . . S1 S 0.45096(10) 0.27915(11) 0.18991(8) 0.0402(2) Uani 1 1 d . . . N1 N 0.8949(4) 0.0654(4) 0.2327(3) 0.0415(7) Uani 1 1 d . . . N2 N 0.5779(3) 0.1445(4) 0.3646(3) 0.0413(7) Uani 1 1 d . . . N3 N 0.4132(3) 0.1792(4) 0.4132(3) 0.0420(7) Uani 1 1 d . . . N4 N 0.0722(3) 0.2265(4) 0.4621(3) 0.0412(7) Uani 1 1 d . . . C1 C 1.0524(4) 0.0460(5) 0.1758(3) 0.0469(9) Uani 1 1 d . . . H1 H 1.1286 -0.0265 0.2115 0.056 Uiso 1 1 calc R . . C2 C 1.1115(5) 0.1248(5) 0.0683(4) 0.0519(10) Uani 1 1 d . . . H2 H 1.2254 0.1076 0.0313 0.062 Uiso 1 1 calc R . . C3 C 1.0023(5) 0.2283(5) 0.0159(4) 0.0542(10) Uani 1 1 d . . . H3 H 1.0392 0.2838 -0.0588 0.065 Uiso 1 1 calc R . . C4 C 0.8363(5) 0.2518(5) 0.0731(3) 0.0458(9) Uani 1 1 d . . . H4 H 0.7584 0.3237 0.0386 0.055 Uiso 1 1 calc R . . C5 C 0.7880(4) 0.1689(4) 0.1799(3) 0.0353(7) Uani 1 1 d . . . C6 C 0.6168(4) 0.1896(4) 0.2492(3) 0.0352(7) Uani 1 1 d . . . C7 C 0.3319(4) 0.2502(4) 0.3331(3) 0.0350(7) Uani 1 1 d . . . C8 C 0.1524(4) 0.3010(4) 0.3640(3) 0.0364(7) Uani 1 1 d . . . C9 C 0.0726(5) 0.4191(5) 0.2992(4) 0.0477(9) Uani 1 1 d . . . H9 H 0.1327 0.4686 0.2294 0.057 Uiso 1 1 calc R . . C10 C -0.0944(5) 0.4652(5) 0.3359(4) 0.0540(10) Uani 1 1 d . . . H10 H -0.1510 0.5469 0.2922 0.065 Uiso 1 1 calc R . . C11 C -0.1772(5) 0.3912(5) 0.4363(4) 0.0516(10) Uani 1 1 d . . . H11 H -0.2926 0.4204 0.4640 0.062 Uiso 1 1 calc R . . C12 C -0.0899(5) 0.2731(5) 0.4969(4) 0.0501(9) Uani 1 1 d . . . H12 H -0.1481 0.2222 0.5668 0.060 Uiso 1 1 calc R . . As1 As 0.49842(4) 0.73752(4) 0.20873(3) 0.03967(14) Uani 1 1 d . . . F1 F 0.6764(3) 0.7968(3) 0.2264(3) 0.0702(7) Uani 1 1 d . . . F2 F 0.6122(4) 0.6072(3) 0.1028(2) 0.0775(8) Uani 1 1 d . . . F3 F 0.3198(3) 0.6779(3) 0.1923(3) 0.0720(7) Uani 1 1 d . . . F4 F 0.3846(3) 0.8702(3) 0.3132(2) 0.0700(7) Uani 1 1 d . . . F5 F 0.5140(3) 0.5985(3) 0.3230(2) 0.0730(7) Uani 1 1 d . . . F6 F 0.4812(4) 0.8749(3) 0.0926(3) 0.0751(8) 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 Ag1 0.0424(2) 0.0664(2) 0.0446(2) 0.01595(15) -0.00755(14) -0.00430(15) S1 0.0291(4) 0.0520(5) 0.0355(4) 0.0065(4) -0.0027(3) -0.0033(4) N1 0.0319(15) 0.0506(18) 0.0390(15) 0.0012(13) -0.0040(12) -0.0036(13) N2 0.0252(14) 0.0564(19) 0.0388(15) 0.0038(13) -0.0025(12) -0.0038(12) N3 0.0313(15) 0.0542(19) 0.0358(15) 0.0052(13) -0.0008(12) -0.0039(13) N4 0.0285(15) 0.0551(18) 0.0376(15) 0.0004(13) -0.0014(12) -0.0076(13) C1 0.0268(18) 0.063(2) 0.048(2) -0.0047(18) -0.0043(16) -0.0016(16) C2 0.0291(19) 0.070(3) 0.053(2) -0.013(2) 0.0055(17) -0.0087(17) C3 0.045(2) 0.065(3) 0.045(2) 0.0045(19) 0.0066(17) -0.0121(19) C4 0.042(2) 0.050(2) 0.0399(19) 0.0083(16) 0.0000(16) -0.0069(16) C5 0.0259(17) 0.0395(18) 0.0389(18) -0.0047(14) -0.0030(13) -0.0040(13) C6 0.0289(17) 0.0410(19) 0.0341(17) 0.0010(14) -0.0025(13) -0.0069(13) C7 0.0291(17) 0.0379(18) 0.0355(17) -0.0012(14) -0.0003(13) -0.0063(13) C8 0.0311(17) 0.0393(18) 0.0390(18) -0.0036(14) -0.0056(14) -0.0067(14) C9 0.035(2) 0.050(2) 0.056(2) 0.0104(17) -0.0063(17) -0.0090(16) C10 0.036(2) 0.059(3) 0.066(3) 0.000(2) -0.0159(19) 0.0016(17) C11 0.0282(18) 0.068(3) 0.056(2) -0.007(2) -0.0065(17) -0.0009(17) C12 0.0310(19) 0.070(3) 0.044(2) -0.0006(18) 0.0013(15) -0.0056(17) As1 0.0288(2) 0.0420(2) 0.0442(2) 0.00338(16) -0.00066(16) -0.00483(15) F1 0.0387(13) 0.0810(18) 0.0924(19) -0.0081(15) -0.0070(12) -0.0199(12) F2 0.0761(19) 0.0647(17) 0.0772(18) -0.0193(14) 0.0121(14) 0.0019(13) F3 0.0507(14) 0.0726(17) 0.101(2) 0.0011(15) -0.0257(14) -0.0207(12) F4 0.0500(14) 0.0712(16) 0.0787(17) -0.0226(14) 0.0157(12) -0.0091(11) F5 0.0648(17) 0.0792(18) 0.0693(17) 0.0316(14) -0.0128(13) -0.0094(13) F6 0.0735(18) 0.0684(17) 0.0703(16) 0.0266(13) -0.0005(14) -0.0031(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.282(3) 2_656 y Ag1 N2 2.366(3) . y Ag1 N1 2.371(3) . y Ag1 N3 2.498(3) 2_656 y S1 C6 1.714(3) . ? S1 C7 1.717(3) . ? N1 C1 1.330(5) . ? N1 C5 1.357(4) . ? N2 C6 1.303(4) . ? N2 N3 1.367(4) . ? N3 C7 1.294(4) . ? N3 Ag1 2.498(3) 2_656 ? N4 C12 1.337(5) . ? N4 C8 1.341(4) . ? N4 Ag1 2.282(3) 2_656 ? C1 C2 1.375(6) . ? C1 H1 0.9500 . ? C2 C3 1.367(6) . ? C2 H2 0.9500 . ? C3 C4 1.394(5) . ? C3 H3 0.9500 . ? C4 C5 1.366(5) . ? C4 H4 0.9500 . ? C5 C6 1.470(5) . ? C7 C8 1.474(5) . ? C8 C9 1.375(5) . ? C9 C10 1.376(5) . ? C9 H9 0.9500 . ? C10 C11 1.366(6) . ? C10 H10 0.9500 . ? C11 C12 1.380(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? As1 F5 1.700(2) . ? As1 F6 1.708(2) . ? As1 F2 1.709(2) . ? As1 F4 1.711(2) . ? As1 F1 1.715(2) . ? As1 F3 1.717(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 N4 Ag1 N2 162.55(10) 2_656 . ? N4 Ag1 N1 124.48(10) 2_656 . ? N2 Ag1 N1 71.17(10) . . ? N4 Ag1 N3 70.63(10) 2_656 2_656 ? N2 Ag1 N3 95.93(10) . 2_656 ? N1 Ag1 N3 161.21(10) . 2_656 ? C6 S1 C7 87.10(16) . . ? C1 N1 C5 117.1(3) . . ? C1 N1 Ag1 127.0(3) . . ? C5 N1 Ag1 115.8(2) . . ? C6 N2 N3 113.1(3) . . ? C6 N2 Ag1 112.5(2) . . ? N3 N2 Ag1 130.3(2) . . ? C7 N3 N2 112.0(3) . . ? C7 N3 Ag1 108.6(2) . 2_656 ? N2 N3 Ag1 133.7(2) . 2_656 ? C12 N4 C8 117.4(3) . . ? C12 N4 Ag1 122.8(3) . 2_656 ? C8 N4 Ag1 119.3(2) . 2_656 ? N1 C1 C2 123.9(4) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 118.3(3) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 118.5(4) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 122.8(3) . . ? N1 C5 C6 114.7(3) . . ? C4 C5 C6 122.5(3) . . ? N2 C6 C5 122.3(3) . . ? N2 C6 S1 113.4(2) . . ? C5 C6 S1 124.3(3) . . ? N3 C7 C8 122.2(3) . . ? N3 C7 S1 114.3(2) . . ? C8 C7 S1 123.5(2) . . ? N4 C8 C9 122.1(3) . . ? N4 C8 C7 115.2(3) . . ? C9 C8 C7 122.7(3) . . ? C8 C9 C10 119.8(4) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 118.7(4) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C12 118.7(4) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? N4 C12 C11 123.4(4) . . ? N4 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? F5 As1 F6 178.96(15) . . ? F5 As1 F2 89.86(14) . . ? F6 As1 F2 89.57(14) . . ? F5 As1 F4 90.98(14) . . ? F6 As1 F4 89.59(14) . . ? F2 As1 F4 179.15(13) . . ? F5 As1 F1 90.67(14) . . ? F6 As1 F1 90.19(15) . . ? F2 As1 F1 89.38(14) . . ? F4 As1 F1 90.48(13) . . ? F5 As1 F3 88.94(14) . . ? F6 As1 F3 90.19(14) . . ? F2 As1 F3 90.89(14) . . ? F4 As1 F3 89.25(13) . . ? F1 As1 F3 179.53(13) . . ? 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 N4 Ag1 N1 C1 -1.7(4) 2_656 . . . ? N2 Ag1 N1 C1 169.6(3) . . . . ? N3 Ag1 N1 C1 -142.0(3) 2_656 . . . ? N4 Ag1 N1 C5 -178.4(2) 2_656 . . . ? N2 Ag1 N1 C5 -7.1(2) . . . . ? N3 Ag1 N1 C5 41.3(5) 2_656 . . . ? N4 Ag1 N2 C6 170.5(3) 2_656 . . . ? N1 Ag1 N2 C6 15.0(2) . . . . ? N3 Ag1 N2 C6 -151.0(2) 2_656 . . . ? N4 Ag1 N2 N3 -34.5(5) 2_656 . . . ? N1 Ag1 N2 N3 170.1(3) . . . . ? N3 Ag1 N2 N3 4.1(3) 2_656 . . . ? C6 N2 N3 C7 -0.2(4) . . . . ? Ag1 N2 N3 C7 -155.2(3) . . . . ? C6 N2 N3 Ag1 149.3(3) . . . 2_656 ? Ag1 N2 N3 Ag1 -5.6(5) . . . 2_656 ? C5 N1 C1 C2 0.3(6) . . . . ? Ag1 N1 C1 C2 -176.4(3) . . . . ? N1 C1 C2 C3 -0.5(6) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C1 N1 C5 C4 -0.1(5) . . . . ? Ag1 N1 C5 C4 176.9(3) . . . . ? C1 N1 C5 C6 -177.9(3) . . . . ? Ag1 N1 C5 C6 -0.9(4) . . . . ? C3 C4 C5 N1 0.2(5) . . . . ? C3 C4 C5 C6 177.8(3) . . . . ? N3 N2 C6 C5 177.8(3) . . . . ? Ag1 N2 C6 C5 -22.6(4) . . . . ? N3 N2 C6 S1 -0.2(4) . . . . ? Ag1 N2 C6 S1 159.30(16) . . . . ? N1 C5 C6 N2 16.6(5) . . . . ? C4 C5 C6 N2 -161.2(4) . . . . ? N1 C5 C6 S1 -165.6(3) . . . . ? C4 C5 C6 S1 16.6(5) . . . . ? C7 S1 C6 N2 0.4(3) . . . . ? C7 S1 C6 C5 -177.6(3) . . . . ? N2 N3 C7 C8 -179.4(3) . . . . ? Ag1 N3 C7 C8 23.4(4) 2_656 . . . ? N2 N3 C7 S1 0.6(4) . . . . ? Ag1 N3 C7 S1 -156.65(16) 2_656 . . . ? C6 S1 C7 N3 -0.6(3) . . . . ? C6 S1 C7 C8 179.4(3) . . . . ? C12 N4 C8 C9 -1.0(5) . . . . ? Ag1 N4 C8 C9 -172.9(3) 2_656 . . . ? C12 N4 C8 C7 177.3(3) . . . . ? Ag1 N4 C8 C7 5.5(4) 2_656 . . . ? N3 C7 C8 N4 -21.3(5) . . . . ? S1 C7 C8 N4 158.7(3) . . . . ? N3 C7 C8 C9 157.0(4) . . . . ? S1 C7 C8 C9 -23.0(5) . . . . ? N4 C8 C9 C10 0.8(6) . . . . ? C7 C8 C9 C10 -177.4(3) . . . . ? C8 C9 C10 C11 -0.3(6) . . . . ? C9 C10 C11 C12 -0.1(6) . . . . ? C8 N4 C12 C11 0.7(6) . . . . ? Ag1 N4 C12 C11 172.2(3) 2_656 . . . ? C10 C11 C12 N4 -0.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.821 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.114 data_9 _database_code_depnum_ccdc_archive 'CCDC 706601' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H36 Ag4 N20 O13 S4' _chemical_formula_weight 1672.70 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' O O 0.0106 0.0060 '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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8745(14) _cell_length_b 14.061(2) _cell_length_c 14.463(3) _cell_angle_alpha 68.322(3) _cell_angle_beta 86.714(3) _cell_angle_gamma 88.930(3) _cell_volume 1485.7(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 826 _exptl_absorpt_coefficient_mu 1.519 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7409 _exptl_absorpt_correction_T_max 0.8754 _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 8388 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5460 _reflns_number_gt 4144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. O Atoms of NO3^-^anion are disordered over two positions and all N-O bond lengths were restrained to a target value of 1.24(1) \%A. Displacement parameters for disordered O atoms were also subjected to restraints. The bond lengths C25-O7 was restrained to target values of 1.42(1) \%A. ; _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^)+(0.0684P)^2^+3.0570P] 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 5460 _refine_ls_number_parameters 433 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1293 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.009 _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 Ag1 Ag 0.74544(7) 0.20665(3) 0.32824(4) 0.06657(19) Uani 1 1 d . . . Ag2 Ag 0.44335(7) 0.20670(3) 0.63469(4) 0.06861(19) Uani 1 1 d . . . N1 N 0.4409(6) 0.0466(4) 0.7677(3) 0.0578(12) Uani 1 1 d . . . N2 N 0.5977(6) 0.0755(3) 0.5840(3) 0.0547(11) Uani 1 1 d . . . N3 N 0.6803(6) 0.0753(3) 0.4985(3) 0.0541(11) Uani 1 1 d . . . N4 N 0.8539(6) 0.0474(4) 0.3391(3) 0.0546(11) Uani 1 1 d . . . N5 N 0.2626(6) 0.3485(4) 0.6086(4) 0.0610(12) Uani 1 1 d . . . N6 N 0.4661(6) 0.3256(3) 0.4563(3) 0.0573(12) Uani 1 1 d . . . N7 N 0.5520(6) 0.3261(4) 0.3710(4) 0.0594(12) Uani 1 1 d . . . N8 N 0.6870(7) 0.3480(4) 0.1845(4) 0.0670(13) Uani 1 1 d . . . N9 N 1.1071(7) 0.3170(4) 0.2451(4) 0.0653(13) Uani 1 1 d D . . N10 N 0.6520(9) 0.2623(4) 0.7955(5) 0.0777(16) Uani 1 1 d D . . O1 O 1.0327(6) 0.2902(4) 0.3268(4) 0.0794(13) Uani 1 1 d . A . O2 O 1.1201(16) 0.2626(9) 0.1955(10) 0.103(3) Uani 0.734(9) 1 d PD A 1 O3 O 1.211(2) 0.3828(13) 0.2149(11) 0.206(9) Uani 0.734(9) 1 d PD A 1 O2' O 1.057(5) 0.274(3) 0.191(3) 0.103(3) Uani 0.266(9) 1 d PD A 2 O3' O 1.119(3) 0.4122(7) 0.2129(19) 0.064(6) Uani 0.266(9) 1 d PD A 2 O4 O 0.7000(7) 0.2631(4) 0.7113(5) 0.0957(16) Uani 1 1 d . A . O5 O 0.7365(11) 0.2845(7) 0.8560(6) 0.105(3) Uani 0.734(9) 1 d PD A 1 O5' O 0.792(2) 0.2228(18) 0.8269(16) 0.105(3) Uani 0.266(9) 1 d PD A 2 O6 O 0.5018(9) 0.2615(4) 0.8168(4) 0.1029(18) Uani 1 1 d . A . O7 O 0.0313(12) 0.1684(9) 0.9042(8) 0.093(3) Uani 0.50 1 d PD . . H7 H -0.0399 0.2112 0.8715 0.139 Uiso 0.50 1 calc PR . . S1 S 0.7017(2) -0.10631(11) 0.62325(11) 0.0561(4) Uani 1 1 d . . . S2 S 0.4083(2) 0.49859(11) 0.32381(11) 0.0583(4) Uani 1 1 d . . . C1 C 0.3670(9) 0.0342(5) 0.8564(5) 0.0728(18) Uani 1 1 d . . . H1 H 0.3089 0.0902 0.8654 0.087 Uiso 1 1 calc R . . C2 C 0.3725(10) -0.0587(6) 0.9361(5) 0.079(2) Uani 1 1 d . . . H2 H 0.3196 -0.0656 0.9990 0.094 Uiso 1 1 calc R . . C3 C 0.4536(9) -0.1391(6) 0.9239(5) 0.0757(19) Uani 1 1 d . . . H3 H 0.4574 -0.2034 0.9773 0.091 Uiso 1 1 calc R . . C4 C 0.5303(9) -0.1253(5) 0.8322(5) 0.0671(16) Uani 1 1 d . . . H4A H 0.5901 -0.1802 0.8218 0.080 Uiso 1 1 calc R . . C5 C 0.5206(7) -0.0327(4) 0.7559(4) 0.0502(12) Uani 1 1 d . . . C6 C 0.5988(7) -0.0140(4) 0.6560(4) 0.0489(12) Uani 1 1 d . . . C7 C 0.7412(6) -0.0141(4) 0.5073(4) 0.0460(12) Uani 1 1 d . . . C8 C 0.8375(7) -0.0336(4) 0.4261(4) 0.0499(12) Uani 1 1 d . . . C9 C 0.9108(8) -0.1260(5) 0.4385(5) 0.0642(16) Uani 1 1 d . . . H9 H 0.8980 -0.1815 0.5006 0.077 Uiso 1 1 calc R . . C10 C 1.0040(8) -0.1375(5) 0.3592(5) 0.0695(17) Uani 1 1 d . . . H10 H 1.0564 -0.2011 0.3663 0.083 Uiso 1 1 calc R . . C11 C 1.0194(8) -0.0575(6) 0.2719(6) 0.0731(19) Uani 1 1 d . . . H11 H 1.0821 -0.0641 0.2165 0.088 Uiso 1 1 calc R . . C12 C 0.9429(8) 0.0347(5) 0.2636(5) 0.0676(16) Uani 1 1 d . . . H12 H 0.9546 0.0909 0.2018 0.081 Uiso 1 1 calc R . . C13 C 0.1689(9) 0.3616(5) 0.6823(5) 0.0707(17) Uani 1 1 d . . . H13 H 0.1502 0.3043 0.7427 0.085 Uiso 1 1 calc R . . C14 C 0.0968(9) 0.4546(6) 0.6758(6) 0.0752(19) Uani 1 1 d . . . H14 H 0.0295 0.4604 0.7301 0.090 Uiso 1 1 calc R . . C15 C 0.1249(8) 0.5378(5) 0.5894(5) 0.0677(17) Uani 1 1 d . . . H15 H 0.0806 0.6030 0.5834 0.081 Uiso 1 1 calc R . . C16 C 0.2183(7) 0.5249(5) 0.5118(5) 0.0596(14) Uani 1 1 d . . . H16 H 0.2377 0.5810 0.4506 0.072 Uiso 1 1 calc R . . C17 C 0.2840(7) 0.4293(4) 0.5238(4) 0.0517(13) Uani 1 1 d . . . C18 C 0.3833(7) 0.4116(4) 0.4423(4) 0.0513(13) Uani 1 1 d . . . C19 C 0.5331(7) 0.4115(4) 0.2959(4) 0.0508(12) Uani 1 1 d . . . C20 C 0.6142(8) 0.4309(4) 0.1954(4) 0.0566(14) Uani 1 1 d . . . C21 C 0.6155(9) 0.5256(5) 0.1214(5) 0.0738(18) Uani 1 1 d . . . H21 H 0.5630 0.5817 0.1332 0.089 Uiso 1 1 calc R . . C22 C 0.6931(10) 0.5396(5) 0.0296(5) 0.081(2) Uani 1 1 d . . . H22 H 0.6949 0.6050 -0.0228 0.097 Uiso 1 1 calc R . . C23 C 0.7677(10) 0.4566(6) 0.0158(5) 0.085(2) Uani 1 1 d . . . H23 H 0.8211 0.4629 -0.0467 0.103 Uiso 1 1 calc R . . C24 C 0.7634(10) 0.3629(6) 0.0956(5) 0.082(2) Uani 1 1 d . . . H24 H 0.8182 0.3062 0.0860 0.098 Uiso 1 1 calc R . . C25 C 0.0840(18) 0.1964(14) 0.9803(9) 0.098(6) Uani 0.50 1 d PD . . H25A H 0.1517 0.2593 0.9520 0.148 Uiso 0.50 1 calc PR . . H25B H 0.1534 0.1415 1.0244 0.148 Uiso 0.50 1 calc PR . . H25C H -0.0156 0.2080 1.0185 0.148 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0754(3) 0.0471(3) 0.0666(3) -0.0113(2) 0.0111(2) 0.0101(2) Ag2 0.0929(4) 0.0466(3) 0.0601(3) -0.0143(2) 0.0054(2) 0.0110(2) N1 0.071(3) 0.046(3) 0.051(3) -0.012(2) 0.002(2) -0.002(2) N2 0.065(3) 0.045(3) 0.052(3) -0.015(2) -0.002(2) 0.008(2) N3 0.060(3) 0.047(3) 0.056(3) -0.020(2) 0.000(2) 0.008(2) N4 0.056(3) 0.053(3) 0.055(3) -0.020(2) 0.002(2) 0.003(2) N5 0.067(3) 0.057(3) 0.058(3) -0.022(2) 0.006(2) 0.001(2) N6 0.069(3) 0.040(2) 0.054(3) -0.009(2) 0.006(2) 0.007(2) N7 0.067(3) 0.044(3) 0.059(3) -0.011(2) 0.006(2) 0.008(2) N8 0.074(3) 0.062(3) 0.061(3) -0.020(3) 0.006(3) 0.013(3) N9 0.065(3) 0.069(4) 0.055(3) -0.015(3) -0.004(3) 0.004(3) N10 0.088(5) 0.061(3) 0.070(4) -0.006(3) -0.015(4) -0.001(3) O1 0.088(3) 0.081(3) 0.067(3) -0.027(2) 0.010(2) 0.012(3) O2 0.145(11) 0.087(5) 0.075(4) -0.030(4) -0.019(6) 0.075(6) O3 0.184(14) 0.32(2) 0.095(8) -0.050(11) 0.027(10) -0.175(14) O2' 0.145(11) 0.087(5) 0.075(4) -0.030(4) -0.019(6) 0.075(6) O3' 0.069(12) 0.039(8) 0.081(13) -0.022(8) 0.021(11) -0.026(8) O4 0.102(4) 0.085(4) 0.110(4) -0.052(3) 0.025(3) 0.002(3) O5 0.124(6) 0.116(7) 0.083(5) -0.042(4) -0.027(5) 0.009(5) O5' 0.124(6) 0.116(7) 0.083(5) -0.042(4) -0.027(5) 0.009(5) O6 0.121(5) 0.079(4) 0.102(4) -0.030(3) 0.028(4) 0.000(3) O7 0.065(6) 0.116(9) 0.104(8) -0.050(7) 0.007(5) 0.024(6) S1 0.0673(9) 0.0435(7) 0.0525(8) -0.0123(6) -0.0042(7) 0.0136(6) S2 0.0728(10) 0.0442(7) 0.0538(8) -0.0140(6) -0.0037(7) 0.0143(7) C1 0.086(5) 0.072(4) 0.063(4) -0.031(3) 0.018(3) -0.002(3) C2 0.097(5) 0.085(5) 0.052(4) -0.024(4) 0.011(3) -0.012(4) C3 0.089(5) 0.073(4) 0.054(4) -0.012(3) 0.004(3) 0.000(4) C4 0.080(4) 0.053(4) 0.059(4) -0.010(3) -0.006(3) 0.013(3) C5 0.053(3) 0.048(3) 0.050(3) -0.019(2) -0.006(2) 0.003(2) C6 0.048(3) 0.044(3) 0.052(3) -0.015(2) -0.008(2) 0.009(2) C7 0.046(3) 0.042(3) 0.049(3) -0.014(2) -0.008(2) 0.005(2) C8 0.045(3) 0.053(3) 0.054(3) -0.022(3) -0.007(2) 0.003(2) C9 0.063(4) 0.055(3) 0.075(4) -0.024(3) -0.005(3) 0.014(3) C10 0.072(4) 0.060(4) 0.082(5) -0.034(4) -0.002(3) 0.013(3) C11 0.063(4) 0.087(5) 0.083(5) -0.051(4) 0.013(3) -0.005(4) C12 0.073(4) 0.066(4) 0.063(4) -0.025(3) 0.008(3) 0.002(3) C13 0.075(4) 0.076(4) 0.060(4) -0.027(3) 0.014(3) 0.000(3) C14 0.064(4) 0.097(5) 0.080(5) -0.052(4) 0.001(3) 0.008(4) C15 0.063(4) 0.070(4) 0.084(5) -0.045(4) -0.017(3) 0.019(3) C16 0.056(3) 0.054(3) 0.070(4) -0.026(3) -0.008(3) 0.010(3) C17 0.048(3) 0.049(3) 0.062(3) -0.025(3) -0.007(3) 0.002(2) C18 0.054(3) 0.044(3) 0.057(3) -0.020(3) -0.002(3) -0.002(2) C19 0.055(3) 0.041(3) 0.055(3) -0.016(2) -0.005(2) 0.008(2) C20 0.060(3) 0.051(3) 0.058(3) -0.019(3) -0.001(3) 0.000(3) C21 0.101(5) 0.053(4) 0.062(4) -0.016(3) 0.003(4) 0.009(3) C22 0.109(6) 0.064(4) 0.056(4) -0.008(3) 0.004(4) 0.010(4) C23 0.090(5) 0.101(6) 0.056(4) -0.021(4) 0.012(4) 0.004(4) C24 0.086(5) 0.079(5) 0.075(5) -0.027(4) 0.013(4) 0.020(4) C25 0.081(10) 0.183(19) 0.043(7) -0.055(10) -0.024(7) 0.051(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 Ag1 N4 2.335(5) . ? Ag1 N8 2.347(5) . ? Ag1 N7 2.467(5) . ? Ag1 N3 2.504(5) . ? Ag2 N1 2.360(5) . ? Ag2 N5 2.355(5) . ? Ag2 N6 2.501(5) . ? Ag2 N2 2.497(5) . ? N1 C1 1.329(7) . ? N1 C5 1.330(7) . ? N2 C6 1.304(7) . ? N2 N3 1.364(6) . ? N3 C7 1.300(7) . ? N4 C12 1.329(7) . ? N4 C8 1.350(7) . ? N5 C13 1.328(7) . ? N5 C17 1.334(7) . ? N6 C18 1.317(7) . ? N6 N7 1.370(6) . ? N7 C19 1.301(7) . ? N8 C24 1.334(8) . ? N8 C20 1.346(7) . ? N9 O3 1.186(8) . ? N9 O1 1.218(6) . ? N9 O2 1.226(7) . ? N9 O2' 1.231(10) . ? N9 O3' 1.248(9) . ? N10 O6 1.204(8) . ? N10 O4 1.251(8) . ? N10 O5' 1.256(10) . ? N10 O5 1.258(7) . ? O4 O5' 1.751(19) . ? O7 C25 1.384(9) . ? O7 H7 0.8400 . ? S1 C7 1.715(5) . ? S1 C6 1.713(5) . ? S2 C18 1.701(6) . ? S2 C19 1.704(5) . ? C1 C2 1.388(10) . ? C1 H1 0.9500 . ? C2 C3 1.351(10) . ? C2 H2 0.9500 . ? C3 C4 1.373(9) . ? C3 H3 0.9500 . ? C4 C5 1.365(8) . ? C4 H4A 0.9500 . ? C5 C6 1.469(7) . ? C7 C8 1.469(7) . ? C8 C9 1.365(8) . ? C9 C10 1.385(9) . ? C9 H9 0.9500 . ? C10 C11 1.347(10) . ? C10 H10 0.9500 . ? C11 C12 1.387(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.389(10) . ? C13 H13 0.9500 . ? C14 C15 1.370(10) . ? C14 H14 0.9500 . ? C15 C16 1.373(9) . ? C15 H15 0.9500 . ? C16 C17 1.385(8) . ? C16 H16 0.9500 . ? C17 C18 1.471(8) . ? C19 C20 1.484(8) . ? C20 C21 1.366(8) . ? C21 C22 1.376(9) . ? C21 H21 0.9500 . ? C22 C23 1.371(10) . ? C22 H22 0.9500 . ? C23 C24 1.394(10) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 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 N4 Ag1 N8 128.25(17) . . ? N4 Ag1 N7 156.21(16) . . ? N8 Ag1 N7 69.64(17) . . ? N4 Ag1 N3 69.48(15) . . ? N8 Ag1 N3 155.22(17) . . ? N7 Ag1 N3 88.98(15) . . ? N1 Ag2 N5 129.76(17) . . ? N1 Ag2 N6 155.78(16) . . ? N5 Ag2 N6 69.26(16) . . ? N1 Ag2 N2 69.09(16) . . ? N5 Ag2 N2 154.10(17) . . ? N6 Ag2 N2 88.37(15) . . ? C1 N1 C5 118.5(5) . . ? C1 N1 Ag2 121.5(4) . . ? C5 N1 Ag2 119.9(4) . . ? C6 N2 N3 112.5(4) . . ? C6 N2 Ag2 112.4(4) . . ? N3 N2 Ag2 135.0(3) . . ? C7 N3 N2 112.8(4) . . ? C7 N3 Ag1 111.9(3) . . ? N2 N3 Ag1 135.2(3) . . ? C12 N4 C8 117.9(5) . . ? C12 N4 Ag1 121.9(4) . . ? C8 N4 Ag1 120.0(4) . . ? C13 N5 C17 117.3(5) . . ? C13 N5 Ag2 122.3(4) . . ? C17 N5 Ag2 118.5(4) . . ? C18 N6 N7 112.2(4) . . ? C18 N6 Ag2 111.9(4) . . ? N7 N6 Ag2 135.8(3) . . ? C19 N7 N6 112.5(5) . . ? C19 N7 Ag1 112.4(4) . . ? N6 N7 Ag1 135.0(3) . . ? C24 N8 C20 116.0(6) . . ? C24 N8 Ag1 122.7(4) . . ? C20 N8 Ag1 118.5(4) . . ? O3 N9 O1 124.8(10) . . ? O3 N9 O2 109.2(13) . . ? O1 N9 O2 123.1(9) . . ? O3 N9 O2' 121(3) . . ? O1 N9 O2' 114(3) . . ? O2 N9 O2' 24.3(16) . . ? O3 N9 O3' 39.5(12) . . ? O1 N9 O3' 107.3(12) . . ? O2 N9 O3' 126.5(14) . . ? O2' N9 O3' 120(2) . . ? O6 N10 O4 118.9(6) . . ? O6 N10 O5' 143.8(13) . . ? O4 N10 O5' 88.6(12) . . ? O6 N10 O5 111.0(8) . . ? O4 N10 O5 128.2(8) . . ? O5' N10 O5 55.1(11) . . ? N10 O4 O5' 45.8(6) . . ? N10 O5' O4 45.6(7) . . ? C25 O7 H7 109.5 . . ? C7 S1 C6 87.4(3) . . ? C18 S2 C19 88.0(3) . . ? N1 C1 C2 121.6(6) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 119.7(6) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 118.3(6) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C5 C4 C3 119.9(6) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? N1 C5 C4 122.0(5) . . ? N1 C5 C6 115.8(5) . . ? C4 C5 C6 122.2(5) . . ? N2 C6 C5 122.8(5) . . ? N2 C6 S1 113.6(4) . . ? C5 C6 S1 123.6(4) . . ? N3 C7 C8 123.2(5) . . ? N3 C7 S1 113.6(4) . . ? C8 C7 S1 123.2(4) . . ? N4 C8 C9 122.2(5) . . ? N4 C8 C7 115.3(5) . . ? C9 C8 C7 122.4(5) . . ? C8 C9 C10 119.1(6) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C11 C10 C9 119.1(6) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 119.4(6) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? N4 C12 C11 122.3(6) . . ? N4 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? N5 C13 C14 123.4(7) . . ? N5 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C15 C14 C13 118.6(6) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 118.6(6) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? C15 C16 C17 119.3(6) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? N5 C17 C16 122.7(5) . . ? N5 C17 C18 116.1(5) . . ? C16 C17 C18 121.2(5) . . ? N6 C18 C17 122.0(5) . . ? N6 C18 S2 113.4(4) . . ? C17 C18 S2 124.6(4) . . ? N7 C19 C20 122.7(5) . . ? N7 C19 S2 113.9(4) . . ? C20 C19 S2 123.3(4) . . ? N8 C20 C21 123.5(6) . . ? N8 C20 C19 114.3(5) . . ? C21 C20 C19 122.2(5) . . ? C20 C21 C22 119.9(6) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 118.1(6) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C22 C23 C24 118.6(6) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? N8 C24 C23 123.9(7) . . ? N8 C24 H24 118.1 . . ? C23 C24 H24 118.1 . . ? O7 C25 H25A 109.5 . . ? O7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 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 N5 Ag2 N1 C1 -21.9(6) . . . . ? N6 Ag2 N1 C1 -158.5(5) . . . . ? N2 Ag2 N1 C1 178.9(5) . . . . ? N5 Ag2 N1 C5 160.9(4) . . . . ? N6 Ag2 N1 C5 24.3(7) . . . . ? N2 Ag2 N1 C5 1.7(4) . . . . ? N1 Ag2 N2 C6 -0.1(4) . . . . ? N5 Ag2 N2 C6 -141.4(4) . . . . ? N6 Ag2 N2 C6 -171.0(4) . . . . ? N1 Ag2 N2 N3 179.5(5) . . . . ? N5 Ag2 N2 N3 38.1(7) . . . . ? N6 Ag2 N2 N3 8.5(5) . . . . ? C6 N2 N3 C7 0.3(7) . . . . ? Ag2 N2 N3 C7 -179.2(4) . . . . ? C6 N2 N3 Ag1 -179.0(4) . . . . ? Ag2 N2 N3 Ag1 1.5(8) . . . . ? N4 Ag1 N3 C7 0.9(4) . . . . ? N8 Ag1 N3 C7 140.9(4) . . . . ? N7 Ag1 N3 C7 170.6(4) . . . . ? N4 Ag1 N3 N2 -179.8(5) . . . . ? N8 Ag1 N3 N2 -39.8(7) . . . . ? N7 Ag1 N3 N2 -10.1(5) . . . . ? N8 Ag1 N4 C12 22.6(6) . . . . ? N7 Ag1 N4 C12 156.2(5) . . . . ? N3 Ag1 N4 C12 -177.4(5) . . . . ? N8 Ag1 N4 C8 -162.2(4) . . . . ? N7 Ag1 N4 C8 -28.6(7) . . . . ? N3 Ag1 N4 C8 -2.2(4) . . . . ? N1 Ag2 N5 C13 19.9(6) . . . . ? N6 Ag2 N5 C13 -177.7(5) . . . . ? N2 Ag2 N5 C13 150.5(5) . . . . ? N1 Ag2 N5 C17 -176.2(4) . . . . ? N6 Ag2 N5 C17 -13.7(4) . . . . ? N2 Ag2 N5 C17 -45.6(6) . . . . ? N1 Ag2 N6 C18 153.7(4) . . . . ? N5 Ag2 N6 C18 8.1(4) . . . . ? N2 Ag2 N6 C18 174.8(4) . . . . ? N1 Ag2 N6 N7 -31.4(8) . . . . ? N5 Ag2 N6 N7 -177.0(6) . . . . ? N2 Ag2 N6 N7 -10.4(5) . . . . ? C18 N6 N7 C19 0.4(7) . . . . ? Ag2 N6 N7 C19 -174.5(4) . . . . ? C18 N6 N7 Ag1 176.7(4) . . . . ? Ag2 N6 N7 Ag1 1.8(9) . . . . ? N4 Ag1 N7 C19 -150.7(4) . . . . ? N8 Ag1 N7 C19 -8.1(4) . . . . ? N3 Ag1 N7 C19 -175.3(4) . . . . ? N4 Ag1 N7 N6 33.0(8) . . . . ? N8 Ag1 N7 N6 175.6(6) . . . . ? N3 Ag1 N7 N6 8.4(5) . . . . ? N4 Ag1 N8 C24 -23.9(7) . . . . ? N7 Ag1 N8 C24 174.2(6) . . . . ? N3 Ag1 N8 C24 -153.9(5) . . . . ? N4 Ag1 N8 C20 175.8(4) . . . . ? N7 Ag1 N8 C20 14.0(4) . . . . ? N3 Ag1 N8 C20 45.8(7) . . . . ? O6 N10 O4 O5' -155.4(14) . . . . ? O5 N10 O4 O5' 41.7(13) . . . . ? O6 N10 O5' O4 142(2) . . . . ? O5 N10 O5' O4 -140.4(11) . . . . ? C5 N1 C1 C2 0.5(10) . . . . ? Ag2 N1 C1 C2 -176.8(5) . . . . ? N1 C1 C2 C3 -0.5(11) . . . . ? C1 C2 C3 C4 0.9(11) . . . . ? C2 C3 C4 C5 -1.2(11) . . . . ? C1 N1 C5 C4 -0.8(9) . . . . ? Ag2 N1 C5 C4 176.5(5) . . . . ? C1 N1 C5 C6 179.7(5) . . . . ? Ag2 N1 C5 C6 -3.0(7) . . . . ? C3 C4 C5 N1 1.2(10) . . . . ? C3 C4 C5 C6 -179.3(6) . . . . ? N3 N2 C6 C5 178.9(5) . . . . ? Ag2 N2 C6 C5 -1.5(7) . . . . ? N3 N2 C6 S1 -0.3(6) . . . . ? Ag2 N2 C6 S1 179.3(2) . . . . ? N1 C5 C6 N2 3.0(8) . . . . ? C4 C5 C6 N2 -176.5(6) . . . . ? N1 C5 C6 S1 -177.8(4) . . . . ? C4 C5 C6 S1 2.7(8) . . . . ? C7 S1 C6 N2 0.2(4) . . . . ? C7 S1 C6 C5 -179.0(5) . . . . ? N2 N3 C7 C8 -179.1(5) . . . . ? Ag1 N3 C7 C8 0.4(6) . . . . ? N2 N3 C7 S1 -0.2(6) . . . . ? Ag1 N3 C7 S1 179.3(2) . . . . ? C6 S1 C7 N3 0.0(4) . . . . ? C6 S1 C7 C8 178.9(5) . . . . ? C12 N4 C8 C9 0.9(8) . . . . ? Ag1 N4 C8 C9 -174.5(4) . . . . ? C12 N4 C8 C7 178.6(5) . . . . ? Ag1 N4 C8 C7 3.2(6) . . . . ? N3 C7 C8 N4 -2.3(8) . . . . ? S1 C7 C8 N4 178.8(4) . . . . ? N3 C7 C8 C9 175.3(5) . . . . ? S1 C7 C8 C9 -3.5(8) . . . . ? N4 C8 C9 C10 -0.5(9) . . . . ? C7 C8 C9 C10 -178.0(5) . . . . ? C8 C9 C10 C11 -0.2(10) . . . . ? C9 C10 C11 C12 0.5(10) . . . . ? C8 N4 C12 C11 -0.6(9) . . . . ? Ag1 N4 C12 C11 174.7(5) . . . . ? C10 C11 C12 N4 -0.1(11) . . . . ? C17 N5 C13 C14 -1.5(10) . . . . ? Ag2 N5 C13 C14 162.6(5) . . . . ? N5 C13 C14 C15 -0.7(11) . . . . ? C13 C14 C15 C16 2.1(10) . . . . ? C14 C15 C16 C17 -1.3(9) . . . . ? C13 N5 C17 C16 2.4(9) . . . . ? Ag2 N5 C17 C16 -162.3(4) . . . . ? C13 N5 C17 C18 -177.9(5) . . . . ? Ag2 N5 C17 C18 17.4(6) . . . . ? C15 C16 C17 N5 -1.0(9) . . . . ? C15 C16 C17 C18 179.3(5) . . . . ? N7 N6 C18 C17 -179.0(5) . . . . ? Ag2 N6 C18 C17 -2.9(7) . . . . ? N7 N6 C18 S2 -0.7(6) . . . . ? Ag2 N6 C18 S2 175.4(2) . . . . ? N5 C17 C18 N6 -9.2(8) . . . . ? C16 C17 C18 N6 170.5(5) . . . . ? N5 C17 C18 S2 172.7(4) . . . . ? C16 C17 C18 S2 -7.6(8) . . . . ? C19 S2 C18 N6 0.6(5) . . . . ? C19 S2 C18 C17 178.9(5) . . . . ? N6 N7 C19 C20 179.7(5) . . . . ? Ag1 N7 C19 C20 2.5(7) . . . . ? N6 N7 C19 S2 0.1(7) . . . . ? Ag1 N7 C19 S2 -177.0(2) . . . . ? C18 S2 C19 N7 -0.4(5) . . . . ? C18 S2 C19 C20 180.0(5) . . . . ? C24 N8 C20 C21 0.2(10) . . . . ? Ag1 N8 C20 C21 161.7(5) . . . . ? C24 N8 C20 C19 -179.1(6) . . . . ? Ag1 N8 C20 C19 -17.5(7) . . . . ? N7 C19 C20 N8 9.6(8) . . . . ? S2 C19 C20 N8 -170.8(5) . . . . ? N7 C19 C20 C21 -169.7(6) . . . . ? S2 C19 C20 C21 9.9(9) . . . . ? N8 C20 C21 C22 0.6(11) . . . . ? C19 C20 C21 C22 179.8(6) . . . . ? C20 C21 C22 C23 -0.2(12) . . . . ? C21 C22 C23 C24 -0.9(12) . . . . ? C20 N8 C24 C23 -1.4(11) . . . . ? Ag1 N8 C24 C23 -162.1(6) . . . . ? C22 C23 C24 N8 1.8(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O5 0.84 2.00 2.782(13) 153.4 1_455 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.917 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.107 data_10 _database_code_depnum_ccdc_archive 'CCDC 706602' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Ag F6 N8 S2 Sb' _chemical_formula_weight 824.19 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' Ag Ag -0.8971 1.1015 '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' N N 0.0061 0.0033 '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' Sb Sb -0.5866 1.5461 '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' _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 7.4577(8) _cell_length_b 7.5306(8) _cell_length_c 12.8304(13) _cell_angle_alpha 101.086(2) _cell_angle_beta 92.947(2) _cell_angle_gamma 90.682(2) _cell_volume 706.01(13) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 1.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4374 _exptl_absorpt_correction_T_max 0.6949 _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 3953 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2585 _reflns_number_gt 2322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0633P)^2^+0.3498P] 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 2585 _refine_ls_number_parameters 193 _refine_ls_number_restraints 234 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.071 _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 Ag1 Ag 0.5000 0.5000 0.5000 0.0889(2) Uani 1 2 d SU . . N1 N 0.5873(4) 0.5047(4) 0.3199(3) 0.0614(7) Uani 1 1 d U . . N2 N 0.6421(4) 0.7717(4) 0.4953(2) 0.0505(6) Uani 1 1 d U . . N3 N 0.6798(4) 0.9130(4) 0.5779(2) 0.0529(6) Uani 1 1 d U . . N4 N 0.8607(4) 1.3515(4) 0.5665(2) 0.0557(6) Uani 1 1 d U . . S1 S 0.77691(10) 1.01430(11) 0.40996(7) 0.0494(2) Uani 1 1 d U . . C1 C 0.5601(6) 0.3729(6) 0.2341(4) 0.0780(11) Uani 1 1 d U . . H1 H 0.5117 0.2599 0.2431 0.094 Uiso 1 1 calc R . . C2 C 0.5989(6) 0.3937(7) 0.1342(4) 0.0848(13) Uani 1 1 d U . . H2 H 0.5795 0.2963 0.0754 0.102 Uiso 1 1 calc R . . C3 C 0.6657(6) 0.5560(7) 0.1202(4) 0.0843(13) Uani 1 1 d U . . H3 H 0.6921 0.5734 0.0512 0.101 Uiso 1 1 calc R . . C4 C 0.6946(5) 0.6947(6) 0.2068(3) 0.0668(9) Uani 1 1 d U . . H4 H 0.7410 0.8089 0.1987 0.080 Uiso 1 1 calc R . . C5 C 0.6544(4) 0.6637(4) 0.3057(3) 0.0495(7) Uani 1 1 d U . . C6 C 0.6851(4) 0.8017(4) 0.4035(2) 0.0450(6) Uani 1 1 d U . . C7 C 0.7515(4) 1.0496(4) 0.5453(2) 0.0449(6) Uani 1 1 d U . . C8 C 0.8062(4) 1.2210(4) 0.6163(3) 0.0472(6) Uani 1 1 d U . . C9 C 0.8014(5) 1.2408(5) 0.7246(3) 0.0606(8) Uani 1 1 d U . . H9 H 0.7632 1.1438 0.7564 0.073 Uiso 1 1 calc R . . C10 C 0.8542(6) 1.4073(6) 0.7862(3) 0.0736(10) Uani 1 1 d U . . H10 H 0.8516 1.4269 0.8615 0.088 Uiso 1 1 calc R . . C11 C 0.9100(5) 1.5431(6) 0.7372(3) 0.0705(10) Uani 1 1 d U . . H11 H 0.9466 1.6581 0.7778 0.085 Uiso 1 1 calc R . . C12 C 0.9118(5) 1.5097(5) 0.6284(3) 0.0626(9) Uani 1 1 d U . . H12 H 0.9515 1.6043 0.5951 0.075 Uiso 1 1 calc R . . Sb1 Sb 1.0000 1.0000 1.0000 0.07051(18) Uani 1 2 d SU . . F1 F 1.0840(5) 0.9605(4) 0.8641(2) 0.1139(11) Uani 1 1 d U . . F2 F 0.9894(7) 0.7537(4) 0.9937(3) 0.1499(17) Uani 1 1 d U . . F3 F 0.7700(6) 0.9938(9) 0.9411(4) 0.186(2) Uani 1 1 d U . . 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 Ag1 0.1092(4) 0.0753(3) 0.0928(4) 0.0515(3) -0.0170(3) -0.0422(3) N1 0.0659(17) 0.0514(16) 0.0677(18) 0.0157(14) -0.0034(14) -0.0041(13) N2 0.0562(14) 0.0419(13) 0.0569(16) 0.0189(11) 0.0030(12) -0.0069(11) N3 0.0568(14) 0.0524(15) 0.0537(15) 0.0204(12) 0.0051(11) -0.0038(12) N4 0.0577(15) 0.0507(15) 0.0597(16) 0.0147(12) -0.0002(12) -0.0075(12) S1 0.0495(4) 0.0481(4) 0.0547(5) 0.0189(3) 0.0094(3) -0.0057(3) C1 0.085(3) 0.054(2) 0.089(3) 0.003(2) -0.012(2) -0.0015(18) C2 0.090(3) 0.079(3) 0.074(3) -0.012(2) -0.004(2) 0.004(2) C3 0.088(3) 0.102(3) 0.059(2) 0.004(2) 0.015(2) -0.003(2) C4 0.066(2) 0.074(2) 0.061(2) 0.0163(18) 0.0118(16) -0.0085(18) C5 0.0428(14) 0.0489(16) 0.0588(18) 0.0150(13) 0.0034(13) 0.0019(12) C6 0.0378(13) 0.0453(16) 0.0563(17) 0.0205(13) 0.0036(12) 0.0015(11) C7 0.0398(13) 0.0462(16) 0.0520(16) 0.0176(13) 0.0038(12) 0.0021(11) C8 0.0399(14) 0.0468(16) 0.0568(17) 0.0147(13) 0.0027(12) 0.0021(11) C9 0.0646(19) 0.062(2) 0.0575(19) 0.0175(16) 0.0051(15) -0.0006(15) C10 0.082(2) 0.081(3) 0.055(2) 0.0050(19) 0.0024(18) 0.002(2) C11 0.070(2) 0.061(2) 0.073(2) -0.0017(18) -0.0032(18) -0.0006(17) C12 0.0614(19) 0.0507(19) 0.075(2) 0.0128(16) -0.0013(16) -0.0068(15) Sb1 0.1158(4) 0.0477(2) 0.0497(2) 0.01027(15) 0.01945(19) -0.00839(19) F1 0.199(3) 0.0767(17) 0.0684(16) 0.0093(13) 0.0547(19) -0.0168(18) F2 0.298(5) 0.0606(16) 0.099(2) 0.0190(15) 0.068(3) -0.001(2) F3 0.131(3) 0.278(6) 0.143(3) 0.029(4) -0.006(3) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.305(3) 2_666 ? Ag1 N2 2.305(3) . ? Ag1 N1 2.440(3) 2_666 ? Ag1 N1 2.440(3) . ? N1 C1 1.338(5) . ? N1 C5 1.340(4) . ? N2 C6 1.297(4) . ? N2 N3 1.365(4) . ? N3 C7 1.302(4) . ? N4 C12 1.338(5) . ? N4 C8 1.341(4) . ? S1 C6 1.720(3) . ? S1 C7 1.726(3) . ? C1 C2 1.365(7) . ? C1 H1 0.9500 . ? C2 C3 1.361(7) . ? C2 H2 0.9500 . ? C3 C4 1.377(6) . ? C3 H3 0.9500 . ? C4 C5 1.380(5) . ? C4 H4 0.9500 . ? C5 C6 1.472(4) . ? C7 C8 1.469(4) . ? C8 C9 1.371(5) . ? C9 C10 1.388(5) . ? C9 H9 0.9500 . ? C10 C11 1.371(6) . ? C10 H10 0.9500 . ? C11 C12 1.370(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? Sb1 F3 1.835(4) . ? Sb1 F3 1.835(4) 2_777 ? Sb1 F2 1.841(3) . ? Sb1 F2 1.841(3) 2_777 ? Sb1 F1 1.854(3) 2_777 ? Sb1 F1 1.854(3) . ? 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 Ag1 N2 180.0 2_666 . ? N2 Ag1 N1 70.01(10) 2_666 2_666 ? N2 Ag1 N1 109.99(10) . 2_666 ? N2 Ag1 N1 109.99(10) 2_666 . ? N2 Ag1 N1 70.01(10) . . ? N1 Ag1 N1 180.0 2_666 . ? C1 N1 C5 117.8(4) . . ? C1 N1 Ag1 127.0(3) . . ? C5 N1 Ag1 114.9(2) . . ? C6 N2 N3 114.3(3) . . ? C6 N2 Ag1 117.8(2) . . ? N3 N2 Ag1 127.9(2) . . ? C7 N3 N2 111.3(3) . . ? C12 N4 C8 116.5(3) . . ? C6 S1 C7 86.97(15) . . ? N1 C1 C2 122.9(4) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.0(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.5(4) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 118.4(4) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 122.3(3) . . ? N1 C5 C6 115.1(3) . . ? C4 C5 C6 122.5(3) . . ? N2 C6 C5 121.6(3) . . ? N2 C6 S1 113.1(2) . . ? C5 C6 S1 125.3(2) . . ? N3 C7 C8 123.6(3) . . ? N3 C7 S1 114.4(2) . . ? C8 C7 S1 122.0(2) . . ? N4 C8 C9 124.1(3) . . ? N4 C8 C7 114.7(3) . . ? C9 C8 C7 121.2(3) . . ? C8 C9 C10 117.8(4) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? C11 C10 C9 119.3(4) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C12 C11 C10 118.7(4) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? N4 C12 C11 123.7(4) . . ? N4 C12 H12 118.1 . . ? C11 C12 H12 118.1 . . ? F3 Sb1 F3 180.000(2) . 2_777 ? F3 Sb1 F2 90.6(3) . . ? F3 Sb1 F2 89.4(3) 2_777 . ? F3 Sb1 F2 89.4(3) . 2_777 ? F3 Sb1 F2 90.6(3) 2_777 2_777 ? F2 Sb1 F2 180.0(2) . 2_777 ? F3 Sb1 F1 91.0(2) . 2_777 ? F3 Sb1 F1 89.0(2) 2_777 2_777 ? F2 Sb1 F1 90.41(14) . 2_777 ? F2 Sb1 F1 89.59(14) 2_777 2_777 ? F3 Sb1 F1 89.0(2) . . ? F3 Sb1 F1 91.0(2) 2_777 . ? F2 Sb1 F1 89.59(14) . . ? F2 Sb1 F1 90.41(14) 2_777 . ? F1 Sb1 F1 180.000(2) 2_777 . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.502 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.197