Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_requested_category FI _publ_contact_author_name 'Kenji Nomiya' _publ_contact_author_address ; Department of Materials Science, Faculty of Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; _publ_contact_letter ; Dear Sir: Here we deposit our revised cif file containing CCDC294754, CCDC296440 and CCDC637149 for the article to Dalton Trans entitled Synthesis, reactivity and structure of a light-stable silver(I) cluster with an Ag4S4 core having tridentate 4N-morpholyl 2-acetylpyridine thiosemicarbazone ligands : Use of water-soluble silver(I) carboxylates as silver(I) source. Sincerely, Keji Nomiya ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' +81-463/59-4111 (Ext. 2717) ' _publ_contact_author_fax ' +81-463/58-9684 ' _publ_contact_author_email nomiya@chem.kanagawa-u.ac.jp _publ_section_title ; Synthesis, reaction and structure of a highly light-stable silver(I) cluster with an Ag4S4N4 core having a tridentate 4N-morpholyl 2-acetylpyridine thiosemicarbazone ligand: Use of water-soluble silver(I) carboxylates as silver(I) source ; loop_ _publ_author_name _publ_author_address 'Kuniaki Onodera' ; Department of Materials Science, Faculty of Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; 'Noriko Chikaraishi Kasuga' ; Department of Materials Science, Faculty of Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; 'Tomomi Takashima' ; Department of Materials Science, Faculty of Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; 'Akihiko Hara' ; Department of Materials Science, Faculty of Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; 'Akifumi Amano' ; Department of Materials Science, Faculty of Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; 'Hideyuki Murakami' ; Department of Materials Science, Faculty of Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; ; K.Nomiya ; ; Department of Materials Science, Faculty of Science, Kanagawa University Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). SIR97. J. Appl. Cryst., 32, 115-119. Farrugia, L. J. (1999). WinGX ver.1.64.00. J. Appl. Cryst., 32, 837-838. Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. MSC and Rigaku (2001). Crystal Structure. Version 2.00. Molecular Structure Corporation, The Woodlands, TX, USA. Rigaku, Tokyo, Japan. Rigaku (1998). PROCESS-AUTO. Rigaku, Tokyo, Japan. Sheldrick, G. M. (1997). SHELX-97. University of G\"ottingen, Germany. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. ; data_CCDC294754 _database_code_depnum_ccdc_archive 'CCDC 294754' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H60 Ag4 N16 O4 S4' _chemical_formula_sum 'C50 H62 Ag4 Cl6 N16 O4 S4' _chemical_formula_weight 1723.6 _chemical_compound_source 'local laboratory' 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.997(4) _cell_length_b 11.983(5) _cell_length_c 13.481(6) _cell_angle_alpha 73.203(6) _cell_angle_beta 87.140(6) _cell_angle_gamma 85.074(6) _cell_volume 1539.7(11) _cell_formula_units_Z 1 _cell_measurement_temperature 90 _cell_measurement_reflns_used 6437 _cell_measurement_theta_min 2.551 _cell_measurement_theta_max 28.297 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.86 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 1.708 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_process_details 'XPREP Bruker AXS 2000' _exptl_special_details ; SADABS, Sheldrick 1996 ; _diffrn_ambient_temperature 90 _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 8.366 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20898 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.36 _reflns_number_total 7602 _reflns_number_gt 6942 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL ' _computing_publication_material 'WinGX (Farrugia, 1999) ' _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^)+(0.0511P)^2^+0.0863P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0044(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7602 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.2665(3) 0.0363(2) 0.76408(19) 0.0242(5) Uani 1 1 d . . . H1 H -0.2365 0.0632 0.8167 0.029 Uiso 1 1 calc R . . C2 C -0.3718(3) -0.0349(2) 0.7869(2) 0.0261(5) Uani 1 1 d . . . H2 H -0.4110 -0.0562 0.8530 0.031 Uiso 1 1 calc R . . C3 C -0.4174(3) -0.0738(2) 0.7088(2) 0.0261(5) Uani 1 1 d . . . H3 H -0.4884 -0.1218 0.7213 0.031 Uiso 1 1 calc R . . C4 C -0.3558(3) -0.0402(2) 0.61122(19) 0.0236(5) Uani 1 1 d . . . H4 H -0.3849 -0.0658 0.5577 0.028 Uiso 1 1 calc R . . C5 C -0.2501(2) 0.03222(19) 0.59401(18) 0.0185(4) Uani 1 1 d . . . C6 C -0.1829(2) 0.07349(19) 0.49075(17) 0.0174(4) Uani 1 1 d . . . C7 C -0.2040(3) 0.0176(2) 0.40696(19) 0.0254(5) Uani 1 1 d . . . H7A H -0.1223 0.0159 0.3667 0.038 Uiso 1 1 calc R . . H7B H -0.2741 0.0620 0.3629 0.038 Uiso 1 1 calc R . . H7C H -0.2291 -0.0607 0.4377 0.038 Uiso 1 1 calc R . . C8 C 0.0428(2) 0.27013(19) 0.36774(17) 0.0160(4) Uani 1 1 d . . . C9 C 0.0297(3) 0.2746(2) 0.18753(18) 0.0240(5) Uani 1 1 d . . . H9A H -0.0637 0.2591 0.2043 0.029 Uiso 1 1 calc R . . H9B H 0.0795 0.2017 0.1866 0.029 Uiso 1 1 calc R . . C10 C 0.0409(2) 0.3630(2) 0.08207(18) 0.0240(5) Uani 1 1 d . . . H10A H 0.0075 0.3314 0.0302 0.029 Uiso 1 1 calc R . . H10B H -0.0150 0.4334 0.0820 0.029 Uiso 1 1 calc R . . C11 C 0.2208(3) 0.4425(2) 0.13031(18) 0.0222(5) Uani 1 1 d . . . H11A H 0.1638 0.5125 0.1295 0.027 Uiso 1 1 calc R . . H11B H 0.3116 0.4652 0.1117 0.027 Uiso 1 1 calc R . . C12 C 0.2188(2) 0.3589(2) 0.23881(18) 0.0190(4) Uani 1 1 d . . . H12A H 0.2820 0.2919 0.2420 0.023 Uiso 1 1 calc R . . H12B H 0.2458 0.3977 0.2878 0.023 Uiso 1 1 calc R . . C13 C 0.1984(2) 0.4996(2) 0.69070(18) 0.0219(5) Uani 1 1 d . . . H13 H 0.1205 0.4599 0.7025 0.026 Uiso 1 1 calc R . . C14 C 0.2615(3) 0.5129(2) 0.77566(18) 0.0250(5) Uani 1 1 d . . . H14 H 0.2275 0.4824 0.8427 0.030 Uiso 1 1 calc R . . C15 C 0.3763(3) 0.5729(2) 0.75749(19) 0.0269(5) Uani 1 1 d . . . H15 H 0.4206 0.5843 0.8124 0.032 Uiso 1 1 calc R . . C16 C 0.4251(3) 0.6161(2) 0.65633(19) 0.0239(5) Uani 1 1 d . . . H16 H 0.5026 0.6563 0.6428 0.029 Uiso 1 1 calc R . . C17 C 0.3563(2) 0.59837(19) 0.57561(17) 0.0174(4) Uani 1 1 d . . . C18 C 0.4038(2) 0.6454(2) 0.46630(17) 0.0182(4) Uani 1 1 d . . . C19 C 0.5228(3) 0.7180(3) 0.4425(2) 0.0302(6) Uani 1 1 d . . . H19A H 0.5437 0.7379 0.3695 0.045 Uiso 1 1 calc R . . H19B H 0.5986 0.6743 0.4801 0.045 Uiso 1 1 calc R . . H19C H 0.5023 0.7882 0.4627 0.045 Uiso 1 1 calc R . . C20 C 0.2856(2) 0.68315(19) 0.22656(17) 0.0164(4) Uani 1 1 d . . . C21 C 0.2455(2) 0.7786(2) 0.03842(17) 0.0202(5) Uani 1 1 d . . . H21A H 0.2544 0.8614 0.0269 0.024 Uiso 1 1 calc R . . H21B H 0.1520 0.7637 0.0551 0.024 Uiso 1 1 calc R . . C22 C 0.2900(2) 0.7439(2) -0.05912(18) 0.0226(5) Uani 1 1 d . . . H22A H 0.2735 0.6627 -0.0489 0.027 Uiso 1 1 calc R . . H22B H 0.2368 0.7911 -0.1167 0.027 Uiso 1 1 calc R . . C23 C 0.5091(2) 0.6930(2) 0.00052(18) 0.0227(5) Uani 1 1 d . . . H23A H 0.6028 0.7059 -0.0174 0.027 Uiso 1 1 calc R . . H23B H 0.4983 0.6105 0.0122 0.027 Uiso 1 1 calc R . . C24 C 0.4723(2) 0.7255(2) 0.09942(18) 0.0209(5) Uani 1 1 d . . . H24A H 0.5260 0.6760 0.1557 0.025 Uiso 1 1 calc R . . H24B H 0.4904 0.8061 0.0905 0.025 Uiso 1 1 calc R . . C25 C 0.1614(3) 0.1284(2) 0.8420(2) 0.0298(6) Uani 1 1 d . . . N1 N -0.2049(2) 0.06922(17) 0.67086(15) 0.0201(4) Uani 1 1 d . . . N2 N -0.10966(19) 0.16061(16) 0.47672(14) 0.0172(4) Uani 1 1 d . . . N3 N -0.0528(2) 0.19920(17) 0.37936(14) 0.0181(4) Uani 1 1 d . . . N4 N 0.08369(19) 0.31993(17) 0.26641(14) 0.0185(4) Uani 1 1 d . . . N5 N 0.24364(19) 0.54068(17) 0.59290(15) 0.0184(4) Uani 1 1 d . . . N6 N 0.33569(19) 0.62308(17) 0.39686(14) 0.0172(4) Uani 1 1 d . . . N7 N 0.3788(2) 0.66860(17) 0.29503(14) 0.0178(4) Uani 1 1 d . . . N8 N 0.32940(19) 0.71041(17) 0.12444(14) 0.0179(4) Uani 1 1 d . . . O1 O 0.17564(17) 0.39235(15) 0.05505(13) 0.0221(3) Uani 1 1 d . . . O2 O 0.42867(17) 0.75901(16) -0.08413(13) 0.0232(4) Uani 1 1 d . . . S1 S 0.12343(6) 0.30120(5) 0.46895(4) 0.01695(12) Uani 1 1 d . . . S2 S 0.11256(5) 0.66704(5) 0.25214(4) 0.01629(12) Uani 1 1 d . . . Cl1A Cl 0.0552(2) 0.01451(17) 0.86080(16) 0.0275(4) Uani 0.80 1 d P . . Cl1B Cl 0.0900(15) -0.0026(14) 0.8488(14) 0.039(5) Uiso 0.08 1 d P . . Cl1C Cl 0.0470(18) 0.0237(14) 0.8787(10) 0.025(3) Uiso 0.12 1 d P . . Cl2A Cl 0.32198(9) 0.07962(9) 0.79693(7) 0.0346(2) Uani 0.80 1 d P . . Cl2B Cl 0.2601(9) 0.1852(9) 0.7543(6) 0.022(2) Uiso 0.08 1 d P . . Cl2C Cl 0.2809(7) 0.1488(8) 0.7639(5) 0.0239(12) Uiso 0.12 1 d P . . Cl3A Cl 0.18125(11) 0.17231(17) 0.95061(13) 0.0538(4) Uani 0.80 1 d P . . Cl3B Cl 0.2282(13) 0.1054(12) 0.9790(10) 0.033(4) Uiso 0.08 1 d P . . Cl3C Cl 0.2117(9) 0.1266(8) 0.9761(5) 0.0111(15) Uiso 0.12 1 d P . . Ag1 Ag -0.062415(17) 0.241651(14) 0.607509(12) 0.01772(7) Uani 1 1 d . . . Ag2 Ag 0.144300(17) 0.510562(14) 0.441568(13) 0.01893(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0278(13) 0.0258(12) 0.0191(11) -0.0061(9) 0.0018(9) -0.0054(10) C2 0.0288(13) 0.0237(12) 0.0242(12) -0.0049(10) 0.0061(10) -0.0042(10) C3 0.0219(12) 0.0250(12) 0.0298(13) -0.0036(10) 0.0023(10) -0.0088(10) C4 0.0256(12) 0.0220(11) 0.0238(12) -0.0051(9) -0.0020(9) -0.0089(10) C5 0.0186(11) 0.0150(10) 0.0215(11) -0.0042(8) -0.0014(8) -0.0017(8) C6 0.0201(11) 0.0147(10) 0.0178(10) -0.0046(8) -0.0026(8) -0.0020(8) C7 0.0349(14) 0.0232(12) 0.0210(11) -0.0079(9) -0.0005(10) -0.0137(10) C8 0.0171(10) 0.0146(10) 0.0167(10) -0.0046(8) -0.0024(8) -0.0009(8) C9 0.0248(12) 0.0302(13) 0.0195(11) -0.0077(10) -0.0028(9) -0.0118(10) C10 0.0214(12) 0.0335(13) 0.0173(11) -0.0070(10) 0.0000(9) -0.0045(10) C11 0.0233(12) 0.0255(12) 0.0215(11) -0.0115(9) 0.0069(9) -0.0092(9) C12 0.0165(11) 0.0239(11) 0.0198(11) -0.0106(9) 0.0013(8) -0.0047(9) C13 0.0207(11) 0.0232(12) 0.0212(11) -0.0051(9) 0.0002(9) -0.0028(9) C14 0.0249(12) 0.0326(13) 0.0161(11) -0.0060(10) -0.0019(9) 0.0026(10) C15 0.0273(13) 0.0384(14) 0.0177(11) -0.0115(10) -0.0071(9) -0.0002(11) C16 0.0214(12) 0.0307(13) 0.0215(12) -0.0088(10) -0.0052(9) -0.0048(10) C17 0.0167(10) 0.0183(10) 0.0172(10) -0.0055(8) -0.0030(8) 0.0007(8) C18 0.0149(10) 0.0198(11) 0.0192(11) -0.0040(9) -0.0017(8) -0.0029(8) C19 0.0290(13) 0.0419(15) 0.0206(12) -0.0052(11) -0.0038(10) -0.0186(12) C20 0.0148(10) 0.0177(10) 0.0186(10) -0.0080(8) 0.0009(8) -0.0026(8) C21 0.0160(10) 0.0281(12) 0.0179(11) -0.0085(9) -0.0017(8) -0.0010(9) C22 0.0188(11) 0.0332(13) 0.0192(11) -0.0116(10) 0.0019(9) -0.0081(10) C23 0.0185(11) 0.0287(13) 0.0220(11) -0.0089(10) 0.0040(9) -0.0043(9) C24 0.0171(11) 0.0259(12) 0.0207(11) -0.0079(9) 0.0018(8) -0.0044(9) C25 0.0254(13) 0.0278(13) 0.0378(15) -0.0098(11) -0.0102(11) -0.0031(10) N1 0.0223(10) 0.0193(9) 0.0202(9) -0.0072(8) 0.0015(8) -0.0050(8) N2 0.0176(9) 0.0174(9) 0.0165(9) -0.0041(7) -0.0001(7) -0.0037(7) N3 0.0207(9) 0.0181(9) 0.0165(9) -0.0058(7) 0.0006(7) -0.0042(7) N4 0.0175(9) 0.0228(10) 0.0169(9) -0.0067(7) 0.0000(7) -0.0076(8) N5 0.0176(9) 0.0196(9) 0.0189(9) -0.0065(7) -0.0026(7) -0.0025(7) N6 0.0165(9) 0.0200(9) 0.0159(9) -0.0057(7) 0.0004(7) -0.0033(7) N7 0.0163(9) 0.0216(9) 0.0158(9) -0.0053(7) -0.0006(7) -0.0026(7) N8 0.0137(9) 0.0243(10) 0.0164(9) -0.0063(7) -0.0004(7) -0.0036(7) O1 0.0211(8) 0.0275(9) 0.0206(8) -0.0110(7) 0.0042(6) -0.0056(7) O2 0.0199(8) 0.0330(9) 0.0186(8) -0.0090(7) 0.0038(6) -0.0093(7) S1 0.0177(3) 0.0178(3) 0.0166(3) -0.0056(2) -0.0023(2) -0.0045(2) S2 0.0137(2) 0.0208(3) 0.0166(3) -0.0084(2) 0.00022(19) -0.0033(2) Cl1A 0.0210(8) 0.0333(8) 0.0319(9) -0.0131(7) -0.0015(8) -0.0081(6) Cl2A 0.0245(4) 0.0502(6) 0.0390(5) -0.0277(4) 0.0087(3) -0.0111(4) Cl3A 0.0272(5) 0.0934(11) 0.0680(8) -0.0660(8) 0.0049(5) -0.0091(6) Ag1 0.01892(11) 0.01929(11) 0.01743(10) -0.00908(7) -0.00083(7) -0.00152(7) Ag2 0.02000(11) 0.01802(11) 0.02022(11) -0.00621(7) -0.00199(7) -0.00594(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.339(3) . ? C1 C2 1.379(4) . ? C1 H1 0.9300 . ? C2 C3 1.378(4) . ? C2 H2 0.9300 . ? C3 C4 1.388(4) . ? C3 H3 0.9300 . ? C4 C5 1.393(3) . ? C4 H4 0.9300 . ? C5 N1 1.349(3) . ? C5 C6 1.483(3) . ? C6 N2 1.290(3) . ? C6 C7 1.501(3) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N3 1.306(3) . ? C8 N4 1.380(3) . ? C8 S1 1.762(2) . ? C9 N4 1.469(3) . ? C9 C10 1.514(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O1 1.425(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O1 1.428(3) . ? C11 C12 1.515(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N4 1.463(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N5 1.337(3) . ? C13 C14 1.389(3) . ? C13 H13 0.9300 . ? C14 C15 1.380(4) . ? C14 H14 0.9300 . ? C15 C16 1.391(4) . ? C15 H15 0.9300 . ? C16 C17 1.391(3) . ? C16 H16 0.9300 . ? C17 N5 1.347(3) . ? C17 C18 1.487(3) . ? C18 N6 1.285(3) . ? C18 C19 1.500(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N7 1.309(3) . ? C20 N8 1.378(3) . ? C20 S2 1.763(2) . ? C21 N8 1.466(3) . ? C21 C22 1.525(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 O2 1.425(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 O2 1.426(3) . ? C23 C24 1.513(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N8 1.465(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 Cl2B 1.539(9) . ? C25 Cl2C 1.540(6) . ? C25 Cl1C 1.720(17) . ? C25 Cl3A 1.719(3) . ? C25 Cl1A 1.754(3) . ? C25 Cl1B 1.756(18) . ? C25 Cl2A 1.799(3) . ? C25 Cl3C 1.895(8) . ? C25 Cl3B 1.932(13) . ? N1 Ag1 2.528(2) . ? N2 N3 1.371(3) . ? N2 Ag1 2.329(2) . ? N5 Ag2 2.443(2) . ? N6 N7 1.384(3) . ? N6 Ag2 2.387(2) . ? S1 Ag2 2.4537(12) . ? S1 Ag1 2.5614(9) . ? S2 Ag1 2.4568(10) 2_566 ? S2 Ag2 2.7109(10) . ? Ag1 S2 2.4568(9) 2_566 ? Ag1 Ag2 2.9027(12) 2_566 ? Ag2 Ag1 2.9027(12) 2_566 ? Ag2 Ag2 3.2111(11) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.9(2) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 118.1(2) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 119.0(2) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 119.6(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 121.2(2) . . ? N1 C5 C6 116.8(2) . . ? C4 C5 C6 121.9(2) . . ? N2 C6 C5 116.6(2) . . ? N2 C6 C7 122.6(2) . . ? C5 C6 C7 120.7(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N4 114.93(19) . . ? N3 C8 S1 125.57(17) . . ? N4 C8 S1 119.47(16) . . ? N4 C9 C10 109.7(2) . . ? N4 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? N4 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? O1 C10 C9 112.1(2) . . ? O1 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? O1 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? O1 C11 C12 112.44(19) . . ? O1 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? O1 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N4 C12 C11 109.82(19) . . ? N4 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? N4 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N5 C13 C14 123.6(2) . . ? N5 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C15 C14 C13 117.9(2) . . ? C15 C14 H14 121.1 . . ? C13 C14 H14 121.1 . . ? C14 C15 C16 119.4(2) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 119.0(2) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? N5 C17 C16 121.7(2) . . ? N5 C17 C18 117.7(2) . . ? C16 C17 C18 120.6(2) . . ? N6 C18 C17 116.4(2) . . ? N6 C18 C19 123.9(2) . . ? C17 C18 C19 119.7(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N7 C20 N8 115.9(2) . . ? N7 C20 S2 126.75(17) . . ? N8 C20 S2 117.32(16) . . ? N8 C21 C22 109.1(2) . . ? N8 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? N8 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? O2 C22 C21 112.04(19) . . ? O2 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? O2 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? O2 C23 C24 112.5(2) . . ? O2 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? O2 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? N8 C24 C23 109.20(19) . . ? N8 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? N8 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? C1 N1 C5 118.1(2) . . ? C1 N1 Ag1 125.36(16) . . ? C5 N1 Ag1 113.72(15) . . ? C6 N2 N3 115.19(18) . . ? C6 N2 Ag1 123.71(15) . . ? N3 N2 Ag1 120.98(14) . . ? C8 N3 N2 116.92(18) . . ? C8 N4 C12 122.25(19) . . ? C8 N4 C9 116.57(18) . . ? C12 N4 C9 112.38(18) . . ? C13 N5 C17 118.3(2) . . ? C13 N5 Ag2 124.99(16) . . ? C17 N5 Ag2 116.58(15) . . ? C18 N6 N7 116.31(19) . . ? C18 N6 Ag2 121.65(15) . . ? N7 N6 Ag2 122.03(13) . . ? C20 N7 N6 114.55(19) . . ? C20 N8 C21 123.06(19) . . ? C20 N8 C24 119.23(19) . . ? C21 N8 C24 111.32(18) . . ? C10 O1 C11 108.12(18) . . ? C22 O2 C23 110.36(17) . . ? C8 S1 Ag2 113.55(7) . . ? C8 S1 Ag1 96.93(8) . . ? Ag2 S1 Ag1 106.61(2) . . ? C20 S2 Ag1 103.16(7) . 2_566 ? C20 S2 Ag2 95.07(8) . . ? Ag1 S2 Ag2 68.14(3) 2_566 . ? N2 Ag1 S2 156.62(5) . 2_566 ? N2 Ag1 N1 67.07(7) . . ? S2 Ag1 N1 99.18(5) 2_566 . ? N2 Ag1 S1 74.64(5) . . ? S2 Ag1 S1 124.00(3) 2_566 . ? N1 Ag1 S1 135.64(5) . . ? N2 Ag1 Ag2 112.82(5) . 2_566 ? S2 Ag1 Ag2 60.09(2) 2_566 2_566 ? N1 Ag1 Ag2 128.93(5) . 2_566 ? S1 Ag1 Ag2 85.888(19) . 2_566 ? N6 Ag2 N5 67.54(7) . . ? N6 Ag2 S1 130.68(5) . . ? N5 Ag2 S1 109.73(5) . . ? N6 Ag2 S2 70.36(5) . . ? N5 Ag2 S2 127.35(5) . . ? S1 Ag2 S2 121.48(2) . . ? N6 Ag2 Ag1 69.60(5) . 2_566 ? N5 Ag2 Ag1 84.32(5) . 2_566 ? S1 Ag2 Ag1 158.162(19) . 2_566 ? S2 Ag2 Ag1 51.771(18) . 2_566 ? N6 Ag2 Ag2 145.15(5) . 2_566 ? N5 Ag2 Ag2 90.39(5) . 2_566 ? S1 Ag2 Ag2 81.196(16) . 2_566 ? S2 Ag2 Ag2 107.77(2) . 2_566 ? Ag1 Ag2 Ag2 82.100(13) 2_566 2_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.7(4) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C2 C3 C4 C5 -0.3(4) . . . . ? C3 C4 C5 N1 0.9(4) . . . . ? C3 C4 C5 C6 -178.3(2) . . . . ? N1 C5 C6 N2 -15.3(3) . . . . ? C4 C5 C6 N2 164.0(2) . . . . ? N1 C5 C6 C7 166.5(2) . . . . ? C4 C5 C6 C7 -14.2(3) . . . . ? N4 C9 C10 O1 57.2(3) . . . . ? O1 C11 C12 N4 -56.5(3) . . . . ? N5 C13 C14 C15 0.7(4) . . . . ? C13 C14 C15 C16 -0.7(4) . . . . ? C14 C15 C16 C17 0.4(4) . . . . ? C15 C16 C17 N5 0.2(4) . . . . ? C15 C16 C17 C18 178.7(2) . . . . ? N5 C17 C18 N6 -2.6(3) . . . . ? C16 C17 C18 N6 178.8(2) . . . . ? N5 C17 C18 C19 175.4(2) . . . . ? C16 C17 C18 C19 -3.2(3) . . . . ? N8 C21 C22 O2 -56.8(3) . . . . ? O2 C23 C24 N8 56.6(3) . . . . ? C2 C1 N1 C5 1.3(4) . . . . ? C2 C1 N1 Ag1 161.0(2) . . . . ? C4 C5 N1 C1 -1.4(3) . . . . ? C6 C5 N1 C1 177.9(2) . . . . ? C4 C5 N1 Ag1 -163.35(18) . . . . ? C6 C5 N1 Ag1 15.9(2) . . . . ? C5 C6 N2 N3 -177.84(19) . . . . ? C7 C6 N2 N3 0.3(3) . . . . ? C5 C6 N2 Ag1 6.1(3) . . . . ? C7 C6 N2 Ag1 -175.67(17) . . . . ? N4 C8 N3 N2 -171.07(19) . . . . ? S1 C8 N3 N2 11.2(3) . . . . ? C6 N2 N3 C8 -166.4(2) . . . . ? Ag1 N2 N3 C8 9.7(3) . . . . ? N3 C8 N4 C12 -153.5(2) . . . . ? S1 C8 N4 C12 24.4(3) . . . . ? N3 C8 N4 C9 -8.5(3) . . . . ? S1 C8 N4 C9 169.37(17) . . . . ? C11 C12 N4 C8 -162.0(2) . . . . ? C11 C12 N4 C9 51.7(3) . . . . ? C10 C9 N4 C8 159.5(2) . . . . ? C10 C9 N4 C12 -52.1(3) . . . . ? C14 C13 N5 C17 -0.1(4) . . . . ? C14 C13 N5 Ag2 176.40(18) . . . . ? C16 C17 N5 C13 -0.3(3) . . . . ? C18 C17 N5 C13 -178.9(2) . . . . ? C16 C17 N5 Ag2 -177.11(18) . . . . ? C18 C17 N5 Ag2 4.3(3) . . . . ? C17 C18 N6 N7 178.97(19) . . . . ? C19 C18 N6 N7 1.0(3) . . . . ? C17 C18 N6 Ag2 -0.5(3) . . . . ? C19 C18 N6 Ag2 -178.48(19) . . . . ? N8 C20 N7 N6 -170.04(19) . . . . ? S2 C20 N7 N6 7.9(3) . . . . ? C18 N6 N7 C20 -155.9(2) . . . . ? Ag2 N6 N7 C20 23.6(2) . . . . ? N7 C20 N8 C21 -151.8(2) . . . . ? S2 C20 N8 C21 30.1(3) . . . . ? N7 C20 N8 C24 -2.3(3) . . . . ? S2 C20 N8 C24 179.56(16) . . . . ? C22 C21 N8 C20 -152.3(2) . . . . ? C22 C21 N8 C24 56.1(3) . . . . ? C23 C24 N8 C20 151.1(2) . . . . ? C23 C24 N8 C21 -56.1(3) . . . . ? C9 C10 O1 C11 -60.9(3) . . . . ? C12 C11 O1 C10 60.6(3) . . . . ? C21 C22 O2 C23 57.3(3) . . . . ? C24 C23 O2 C22 -57.4(3) . . . . ? N3 C8 S1 Ag2 -133.39(18) . . . . ? N4 C8 S1 Ag2 48.9(2) . . . . ? N3 C8 S1 Ag1 -21.9(2) . . . . ? N4 C8 S1 Ag1 160.47(17) . . . . ? N7 C20 S2 Ag1 41.4(2) . . . 2_566 ? N8 C20 S2 Ag1 -140.73(16) . . . 2_566 ? N7 C20 S2 Ag2 -27.3(2) . . . . ? N8 C20 S2 Ag2 150.56(16) . . . . ? C6 N2 Ag1 S2 -55.7(2) . . . 2_566 ? N3 N2 Ag1 S2 128.49(15) . . . 2_566 ? C6 N2 Ag1 N1 1.45(17) . . . . ? N3 N2 Ag1 N1 -174.33(18) . . . . ? C6 N2 Ag1 S1 158.56(19) . . . . ? N3 N2 Ag1 S1 -17.23(15) . . . . ? C6 N2 Ag1 Ag2 -122.76(18) . . . 2_566 ? N3 N2 Ag1 Ag2 61.45(17) . . . 2_566 ? C1 N1 Ag1 N2 -169.9(2) . . . . ? C5 N1 Ag1 N2 -9.40(15) . . . . ? C1 N1 Ag1 S2 -9.6(2) . . . 2_566 ? C5 N1 Ag1 S2 150.86(15) . . . 2_566 ? C1 N1 Ag1 S1 157.68(17) . . . . ? C5 N1 Ag1 S1 -41.85(19) . . . . ? C1 N1 Ag1 Ag2 -68.4(2) . . . 2_566 ? C5 N1 Ag1 Ag2 92.12(16) . . . 2_566 ? C8 S1 Ag1 N2 16.12(9) . . . . ? Ag2 S1 Ag1 N2 133.27(5) . . . . ? C8 S1 Ag1 S2 -148.24(7) . . . 2_566 ? Ag2 S1 Ag1 S2 -31.09(3) . . . 2_566 ? C8 S1 Ag1 N1 46.95(10) . . . . ? Ag2 S1 Ag1 N1 164.10(7) . . . . ? C8 S1 Ag1 Ag2 -98.90(7) . . . 2_566 ? Ag2 S1 Ag1 Ag2 18.25(2) . . . 2_566 ? C18 N6 Ag2 N5 1.94(17) . . . . ? N7 N6 Ag2 N5 -177.53(18) . . . . ? C18 N6 Ag2 S1 -95.32(18) . . . . ? N7 N6 Ag2 S1 85.22(17) . . . . ? C18 N6 Ag2 S2 149.57(19) . . . . ? N7 N6 Ag2 S2 -29.90(15) . . . . ? C18 N6 Ag2 Ag1 94.19(18) . . . 2_566 ? N7 N6 Ag2 Ag1 -85.27(16) . . . 2_566 ? C18 N6 Ag2 Ag2 56.4(2) . . . 2_566 ? N7 N6 Ag2 Ag2 -123.02(14) . . . 2_566 ? C13 N5 Ag2 N6 -179.8(2) . . . . ? C17 N5 Ag2 N6 -3.21(15) . . . . ? C13 N5 Ag2 S1 -52.87(19) . . . . ? C17 N5 Ag2 S1 123.73(15) . . . . ? C13 N5 Ag2 S2 140.82(17) . . . . ? C17 N5 Ag2 S2 -42.58(18) . . . . ? C13 N5 Ag2 Ag1 109.93(19) . . . 2_566 ? C17 N5 Ag2 Ag1 -73.46(16) . . . 2_566 ? C13 N5 Ag2 Ag2 27.91(19) . . . 2_566 ? C17 N5 Ag2 Ag2 -155.48(16) . . . 2_566 ? C8 S1 Ag2 N6 -106.97(10) . . . . ? Ag1 S1 Ag2 N6 147.52(6) . . . . ? C8 S1 Ag2 N5 176.15(9) . . . . ? Ag1 S1 Ag2 N5 70.64(6) . . . . ? C8 S1 Ag2 S2 -16.60(9) . . . . ? Ag1 S1 Ag2 S2 -122.10(3) . . . . ? C8 S1 Ag2 Ag1 48.41(10) . . . 2_566 ? Ag1 S1 Ag2 Ag1 -57.10(5) . . . 2_566 ? C8 S1 Ag2 Ag2 88.90(9) . . . 2_566 ? Ag1 S1 Ag2 Ag2 -16.600(17) . . . 2_566 ? C20 S2 Ag2 N6 23.11(9) . . . . ? Ag1 S2 Ag2 N6 -79.05(5) 2_566 . . . ? C20 S2 Ag2 N5 61.60(10) . . . . ? Ag1 S2 Ag2 N5 -40.56(6) 2_566 . . . ? C20 S2 Ag2 S1 -103.26(8) . . . . ? Ag1 S2 Ag2 S1 154.58(2) 2_566 . . . ? C20 S2 Ag2 Ag1 102.16(7) . . . 2_566 ? C20 S2 Ag2 Ag2 166.30(7) . . . 2_566 ? Ag1 S2 Ag2 Ag2 64.138(15) 2_566 . . 2_566 ? S1 Ag1 Ag2 S1 -53.77(5) . . 2_566 2_566 ? S1 Ag1 Ag2 S2 -133.49(2) . . 2_566 2_566 ? Ag2 Ag2 Ag1 S1 -13.384(14) . 2_566 . . ? Ag2 Ag2 Ag1 S2 120.10(2) . 2_566 . 2_566 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.491 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.214 data_CCDC296440 _database_code_depnum_ccdc_archive 'CCDC 296440' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H60 Ag2 N8 O2 P2 S2' _chemical_formula_sum 'C60 H60 Ag2 N8 O2 P2 S2' _chemical_formula_weight 1266.99 _chemical_compound_source 'local laboratory' 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.005(11) _cell_length_b 11.477(11) _cell_length_c 12.859(13) _cell_angle_alpha 70.353(2) _cell_angle_beta 76.622(2) _cell_angle_gamma 65.256(2) _cell_volume 1381(2) _cell_formula_units_Z 1 _cell_measurement_temperature 90 _cell_measurement_reflns_used 6203 _cell_measurement_theta_min 2.263 _cell_measurement_theta_max 28.294 _exptl_crystal_description rod _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.52 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_process_details 'XPREP Bruker AXS 2000' _exptl_special_details ; ; _diffrn_ambient_temperature 90 _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 8.366 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18103 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.30 _reflns_number_total 6839 _reflns_number_gt 6326 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL ' _computing_publication_material 'WinGX (Farrugia, 1999) ' _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^)+(0.0478P)^2^+0.0542P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6839 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.29864(18) 0.63571(18) 0.72784(15) 0.0237(3) Uani 1 1 d . . . H1 H 0.2815 0.6027 0.6782 0.028 Uiso 1 1 calc R . . C2 C 0.33272(18) 0.74733(17) 0.68561(15) 0.0241(4) Uani 1 1 d . . . H2 H 0.3403 0.7872 0.6096 0.029 Uiso 1 1 calc R . . C3 C 0.35505(19) 0.79722(18) 0.75980(15) 0.0277(4) Uani 1 1 d . . . H3 H 0.3780 0.8721 0.7345 0.033 Uiso 1 1 calc R . . C4 C 0.34307(19) 0.73501(18) 0.87280(15) 0.0253(4) Uani 1 1 d . . . H4 H 0.3568 0.7683 0.9240 0.030 Uiso 1 1 calc R . . C5 C 0.31005(15) 0.62177(16) 0.90834(14) 0.0172(3) Uani 1 1 d . . . C6 C 0.29893(15) 0.54875(15) 1.02762(13) 0.0163(3) Uani 1 1 d . . . C7 C 0.35641(17) 0.57285(17) 1.11026(15) 0.0215(3) Uani 1 1 d . . . H7A H 0.3938 0.4906 1.1652 0.032 Uiso 1 1 calc R . . H7B H 0.2864 0.6363 1.1456 0.032 Uiso 1 1 calc R . . H7C H 0.4257 0.6071 1.0726 0.032 Uiso 1 1 calc R . . C8 C 0.16310(15) 0.32130(15) 1.19933(13) 0.0152(3) Uani 1 1 d . . . C9 C 0.26119(18) 0.24743(18) 1.37577(15) 0.0246(4) Uani 1 1 d . . . H9A H 0.2041 0.2912 1.4320 0.029 Uiso 1 1 calc R . . H9B H 0.3152 0.2989 1.3310 0.029 Uiso 1 1 calc R . . C10 C 0.35175(18) 0.10837(19) 1.43059(15) 0.0278(4) Uani 1 1 d . . . H10A H 0.4154 0.0689 1.3742 0.033 Uiso 1 1 calc R . . H10B H 0.4025 0.1129 1.4806 0.033 Uiso 1 1 calc R . . C11 C 0.2017(2) 0.01782(18) 1.41906(15) 0.0285(4) Uani 1 1 d . . . H11A H 0.1521 -0.0389 1.4613 0.034 Uiso 1 1 calc R . . H11B H 0.2628 -0.0223 1.3621 0.034 Uiso 1 1 calc R . . C12 C 0.10451(18) 0.15388(17) 1.36481(14) 0.0226(3) Uani 1 1 d . . . H12A H 0.0581 0.1462 1.3133 0.027 Uiso 1 1 calc R . . H12B H 0.0379 0.1911 1.4209 0.027 Uiso 1 1 calc R . . C13 C 0.37276(15) 0.18217(15) 0.82357(13) 0.0153(3) Uani 1 1 d . . . C14 C 0.47096(16) 0.22480(17) 0.83219(15) 0.0208(3) Uani 1 1 d . . . H14 H 0.4506 0.3148 0.8222 0.025 Uiso 1 1 calc R . . C15 C 0.59915(17) 0.13235(18) 0.85580(15) 0.0236(4) Uani 1 1 d . . . H15 H 0.6648 0.1613 0.8598 0.028 Uiso 1 1 calc R . . C16 C 0.63002(16) -0.00252(17) 0.87347(14) 0.0211(3) Uani 1 1 d . . . H16 H 0.7157 -0.0638 0.8898 0.025 Uiso 1 1 calc R . . C17 C 0.53272(16) -0.04546(16) 0.86674(14) 0.0203(3) Uani 1 1 d . . . H17 H 0.5529 -0.1359 0.8787 0.024 Uiso 1 1 calc R . . C18 C 0.40440(16) 0.04650(16) 0.84204(14) 0.0182(3) Uani 1 1 d . . . H18 H 0.3393 0.0169 0.8379 0.022 Uiso 1 1 calc R . . C19 C 0.22816(16) 0.39598(16) 0.64886(13) 0.0163(3) Uani 1 1 d . . . C20 C 0.11357(18) 0.49739(17) 0.60299(14) 0.0219(3) Uani 1 1 d . . . H20 H 0.0305 0.5131 0.6456 0.026 Uiso 1 1 calc R . . C21 C 0.1223(2) 0.57520(18) 0.49411(15) 0.0279(4) Uani 1 1 d . . . H21 H 0.0450 0.6410 0.4636 0.033 Uiso 1 1 calc R . . C22 C 0.2465(2) 0.5547(2) 0.43090(15) 0.0314(4) Uani 1 1 d . . . H22 H 0.2530 0.6083 0.3589 0.038 Uiso 1 1 calc R . . C23 C 0.3601(2) 0.4544(2) 0.47540(16) 0.0316(4) Uani 1 1 d . . . H23 H 0.4432 0.4402 0.4329 0.038 Uiso 1 1 calc R . . C24 C 0.35153(18) 0.37430(18) 0.58323(14) 0.0239(3) Uani 1 1 d . . . H24 H 0.4286 0.3057 0.6118 0.029 Uiso 1 1 calc R . . C25 C 0.10752(15) 0.21509(15) 0.79547(13) 0.0155(3) Uani 1 1 d . . . C26 C 0.12837(16) 0.15617(16) 0.71070(14) 0.0190(3) Uani 1 1 d . . . H26 H 0.1906 0.1689 0.6496 0.023 Uiso 1 1 calc R . . C27 C 0.05673(17) 0.07858(18) 0.71697(15) 0.0227(3) Uani 1 1 d . . . H27 H 0.0712 0.0393 0.6604 0.027 Uiso 1 1 calc R . . C28 C -0.03640(17) 0.05978(18) 0.80778(16) 0.0244(4) Uani 1 1 d . . . H28 H -0.0834 0.0067 0.8126 0.029 Uiso 1 1 calc R . . C29 C -0.05959(17) 0.11979(18) 0.89128(15) 0.0234(3) Uani 1 1 d . . . H29 H -0.1232 0.1082 0.9515 0.028 Uiso 1 1 calc R . . C30 C 0.01230(16) 0.19766(17) 0.88539(14) 0.0198(3) Uani 1 1 d . . . H30 H -0.0035 0.2379 0.9416 0.024 Uiso 1 1 calc R . . N1 N 0.28892(14) 0.57287(14) 0.83571(12) 0.0201(3) Uani 1 1 d . . . N2 N 0.23677(13) 0.46646(13) 1.05579(11) 0.0157(3) Uani 1 1 d . . . N3 N 0.23486(13) 0.39790(13) 1.16616(11) 0.0171(3) Uani 1 1 d . . . N4 N 0.17803(15) 0.24119(14) 1.30576(12) 0.0219(3) Uani 1 1 d . . . O1 O 0.27769(14) 0.02568(13) 1.49129(10) 0.0302(3) Uani 1 1 d . . . P1 P 0.20640(4) 0.30879(4) 0.79562(3) 0.01345(8) Uani 1 1 d . . . S1 S 0.05510(4) 0.31184(4) 1.12558(3) 0.01501(8) Uani 1 1 d . . . Ag1 Ag 0.126116(11) 0.443484(11) 0.925271(9) 0.01538(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0278(9) 0.0229(8) 0.0217(8) -0.0026(7) -0.0048(7) -0.0123(7) C2 0.0278(9) 0.0174(8) 0.0214(8) -0.0016(6) 0.0018(7) -0.0081(7) C3 0.0378(10) 0.0180(8) 0.0273(9) -0.0071(7) 0.0071(8) -0.0150(8) C4 0.0329(9) 0.0217(8) 0.0247(9) -0.0108(7) 0.0050(7) -0.0141(7) C5 0.0133(7) 0.0148(7) 0.0218(8) -0.0055(6) 0.0001(6) -0.0043(6) C6 0.0133(7) 0.0143(7) 0.0200(7) -0.0058(6) -0.0013(6) -0.0033(6) C7 0.0205(8) 0.0217(8) 0.0249(8) -0.0074(7) -0.0035(6) -0.0090(6) C8 0.0151(7) 0.0128(7) 0.0154(7) -0.0050(6) -0.0025(5) -0.0016(5) C9 0.0300(9) 0.0245(9) 0.0198(8) -0.0009(7) -0.0109(7) -0.0104(7) C10 0.0271(9) 0.0302(10) 0.0190(8) -0.0025(7) -0.0050(7) -0.0059(8) C11 0.0408(11) 0.0191(8) 0.0205(8) -0.0021(7) -0.0009(7) -0.0101(8) C12 0.0297(9) 0.0198(8) 0.0177(8) -0.0012(6) -0.0017(7) -0.0119(7) C13 0.0141(7) 0.0158(7) 0.0148(7) -0.0064(6) -0.0020(5) -0.0024(6) C14 0.0191(8) 0.0156(7) 0.0289(9) -0.0085(7) -0.0064(7) -0.0038(6) C15 0.0161(7) 0.0243(9) 0.0334(9) -0.0113(7) -0.0071(7) -0.0052(6) C16 0.0154(7) 0.0209(8) 0.0230(8) -0.0090(7) -0.0034(6) 0.0001(6) C17 0.0203(8) 0.0151(7) 0.0224(8) -0.0073(6) -0.0011(6) -0.0026(6) C18 0.0179(7) 0.0168(7) 0.0213(8) -0.0076(6) -0.0026(6) -0.0057(6) C19 0.0203(7) 0.0159(7) 0.0158(7) -0.0060(6) -0.0029(6) -0.0077(6) C20 0.0239(8) 0.0199(8) 0.0204(8) -0.0056(6) -0.0044(6) -0.0056(7) C21 0.0380(10) 0.0204(8) 0.0221(9) -0.0037(7) -0.0102(8) -0.0058(8) C22 0.0521(12) 0.0284(10) 0.0160(8) -0.0033(7) -0.0022(8) -0.0199(9) C23 0.0351(10) 0.0406(11) 0.0210(9) -0.0109(8) 0.0075(7) -0.0194(9) C24 0.0220(8) 0.0275(9) 0.0214(8) -0.0084(7) -0.0001(7) -0.0082(7) C25 0.0136(7) 0.0150(7) 0.0176(7) -0.0043(6) -0.0038(6) -0.0039(6) C26 0.0192(7) 0.0217(8) 0.0176(7) -0.0072(6) -0.0013(6) -0.0081(6) C27 0.0242(8) 0.0253(9) 0.0239(8) -0.0111(7) -0.0047(7) -0.0098(7) C28 0.0192(8) 0.0249(9) 0.0330(9) -0.0085(7) -0.0055(7) -0.0100(7) C29 0.0165(7) 0.0279(9) 0.0258(8) -0.0080(7) 0.0019(6) -0.0097(7) C30 0.0168(7) 0.0233(8) 0.0205(8) -0.0089(6) -0.0016(6) -0.0064(6) N1 0.0220(7) 0.0203(7) 0.0194(7) -0.0010(5) -0.0047(5) -0.0113(6) N2 0.0154(6) 0.0136(6) 0.0164(6) -0.0036(5) -0.0023(5) -0.0040(5) N3 0.0187(6) 0.0161(6) 0.0158(6) -0.0020(5) -0.0047(5) -0.0061(5) N4 0.0284(7) 0.0211(7) 0.0171(7) 0.0017(6) -0.0080(6) -0.0127(6) O1 0.0381(7) 0.0238(7) 0.0185(6) 0.0032(5) -0.0076(5) -0.0064(6) P1 0.01294(18) 0.01343(18) 0.01428(18) -0.00544(14) -0.00206(14) -0.00355(14) S1 0.01595(17) 0.01294(17) 0.01592(17) -0.00367(14) -0.00300(14) -0.00466(14) Ag1 0.01567(7) 0.01598(7) 0.01497(7) -0.00657(5) -0.00203(4) -0.00428(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.334(2) . ? C1 C2 1.385(2) . ? C1 H1 0.9300 . ? C2 C3 1.376(3) . ? C2 H2 0.9300 . ? C3 C4 1.390(3) . ? C3 H3 0.9300 . ? C4 C5 1.396(2) . ? C4 H4 0.9300 . ? C5 N1 1.343(2) . ? C5 C6 1.485(2) . ? C6 N2 1.299(2) . ? C6 C7 1.504(2) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N3 1.323(2) . ? C8 N4 1.370(2) . ? C8 S1 1.7386(16) . ? C9 N4 1.460(2) . ? C9 C10 1.508(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O1 1.424(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O1 1.431(2) . ? C11 C12 1.511(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N4 1.455(2) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.392(2) . ? C13 C14 1.398(2) . ? C13 P1 1.8218(16) . ? C14 C15 1.392(2) . ? C14 H14 0.9300 . ? C15 C16 1.386(2) . ? C15 H15 0.9300 . ? C16 C17 1.382(2) . ? C16 H16 0.9300 . ? C17 C18 1.394(2) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.395(2) . ? C19 C20 1.395(2) . ? C19 P1 1.8281(16) . ? C20 C21 1.391(2) . ? C20 H20 0.9300 . ? C21 C22 1.389(3) . ? C21 H21 0.9300 . ? C22 C23 1.378(3) . ? C22 H22 0.9300 . ? C23 C24 1.390(3) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.391(2) . ? C25 C26 1.396(2) . ? C25 P1 1.8228(16) . ? C26 C27 1.390(2) . ? C26 H26 0.9300 . ? C27 C28 1.387(2) . ? C27 H27 0.9300 . ? C28 C29 1.384(3) . ? C28 H28 0.9300 . ? C29 C30 1.396(2) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? N1 Ag1 2.6198(14) . ? N2 N3 1.3722(18) . ? N2 Ag1 2.4252(13) . ? P1 Ag1 2.4203(4) . ? S1 Ag1 2.6397(4) . ? S1 Ag1 2.6402(4) 2_567 ? Ag1 S1 2.6402(4) 2_567 ? Ag1 Ag1 3.046(3) 2_567 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.71(17) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 117.78(16) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 119.60(16) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 118.96(17) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.33(15) . . ? N1 C5 C6 117.01(14) . . ? C4 C5 C6 121.65(15) . . ? N2 C6 C5 117.04(14) . . ? N2 C6 C7 122.77(15) . . ? C5 C6 C7 120.18(14) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N4 113.94(14) . . ? N3 C8 S1 128.22(12) . . ? N4 C8 S1 117.84(12) . . ? N4 C9 C10 109.68(15) . . ? N4 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? N4 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? O1 C10 C9 111.99(15) . . ? O1 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? O1 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? O1 C11 C12 111.53(15) . . ? O1 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? O1 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? N4 C12 C11 109.45(15) . . ? N4 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? N4 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? C18 C13 C14 118.98(14) . . ? C18 C13 P1 123.67(12) . . ? C14 C13 P1 117.27(12) . . ? C15 C14 C13 119.93(15) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.69(16) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 119.63(15) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.11(16) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.64(15) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C24 C19 C20 118.59(15) . . ? C24 C19 P1 124.57(13) . . ? C20 C19 P1 116.68(12) . . ? C21 C20 C19 120.66(17) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 120.00(17) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 119.70(17) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 120.54(18) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C19 120.48(17) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C30 C25 C26 119.37(15) . . ? C30 C25 P1 118.44(12) . . ? C26 C25 P1 122.14(12) . . ? C27 C26 C25 120.43(15) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C28 C27 C26 119.88(16) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 120.13(16) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.17(16) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 120.00(16) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C1 N1 C5 118.59(15) . . ? C1 N1 Ag1 122.78(11) . . ? C5 N1 Ag1 111.93(10) . . ? C6 N2 N3 114.26(13) . . ? C6 N2 Ag1 122.56(11) . . ? N3 N2 Ag1 123.14(10) . . ? C8 N3 N2 115.71(13) . . ? C8 N4 C12 125.12(14) . . ? C8 N4 C9 121.59(14) . . ? C12 N4 C9 112.98(13) . . ? C10 O1 C11 110.13(13) . . ? C13 P1 C25 104.16(7) . . ? C13 P1 C19 104.07(7) . . ? C25 P1 C19 102.83(7) . . ? C13 P1 Ag1 110.41(5) . . ? C25 P1 Ag1 117.45(5) . . ? C19 P1 Ag1 116.41(5) . . ? C8 S1 Ag1 98.92(5) . . ? C8 S1 Ag1 104.19(5) . 2_567 ? Ag1 S1 Ag1 70.452(11) . 2_567 ? P1 Ag1 N2 132.52(3) . . ? P1 Ag1 N1 95.09(3) . . ? N2 Ag1 N1 64.83(4) . . ? P1 Ag1 S1 111.737(15) . . ? N2 Ag1 S1 72.60(3) . . ? N1 Ag1 S1 137.29(3) . . ? P1 Ag1 S1 120.910(14) . 2_567 ? N2 Ag1 S1 99.04(3) . 2_567 ? N1 Ag1 S1 81.16(3) . 2_567 ? S1 Ag1 S1 109.548(11) . 2_567 ? P1 Ag1 Ag1 140.026(11) . 2_567 ? N2 Ag1 Ag1 82.94(3) . 2_567 ? N1 Ag1 Ag1 120.25(3) . 2_567 ? S1 Ag1 Ag1 54.782(10) . 2_567 ? S1 Ag1 Ag1 54.766(10) 2_567 2_567 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.3(3) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? C2 C3 C4 C5 0.8(3) . . . . ? C3 C4 C5 N1 -0.5(3) . . . . ? C3 C4 C5 C6 178.51(16) . . . . ? N1 C5 C6 N2 -17.5(2) . . . . ? C4 C5 C6 N2 163.53(16) . . . . ? N1 C5 C6 C7 163.40(15) . . . . ? C4 C5 C6 C7 -15.6(2) . . . . ? N4 C9 C10 O1 -55.3(2) . . . . ? O1 C11 C12 N4 56.28(19) . . . . ? C18 C13 C14 C15 1.8(3) . . . . ? P1 C13 C14 C15 178.63(13) . . . . ? C13 C14 C15 C16 -1.5(3) . . . . ? C14 C15 C16 C17 0.5(3) . . . . ? C15 C16 C17 C18 0.2(3) . . . . ? C16 C17 C18 C13 0.2(3) . . . . ? C14 C13 C18 C17 -1.2(2) . . . . ? P1 C13 C18 C17 -177.79(12) . . . . ? C24 C19 C20 C21 0.0(3) . . . . ? P1 C19 C20 C21 175.55(14) . . . . ? C19 C20 C21 C22 -1.7(3) . . . . ? C20 C21 C22 C23 2.0(3) . . . . ? C21 C22 C23 C24 -0.5(3) . . . . ? C22 C23 C24 C19 -1.3(3) . . . . ? C20 C19 C24 C23 1.5(3) . . . . ? P1 C19 C24 C23 -173.65(14) . . . . ? C30 C25 C26 C27 -1.3(2) . . . . ? P1 C25 C26 C27 175.98(13) . . . . ? C25 C26 C27 C28 0.2(3) . . . . ? C26 C27 C28 C29 1.0(3) . . . . ? C27 C28 C29 C30 -1.1(3) . . . . ? C26 C25 C30 C29 1.2(2) . . . . ? P1 C25 C30 C29 -176.18(13) . . . . ? C28 C29 C30 C25 0.0(3) . . . . ? C2 C1 N1 C5 1.7(3) . . . . ? C2 C1 N1 Ag1 150.66(14) . . . . ? C4 C5 N1 C1 -0.7(2) . . . . ? C6 C5 N1 C1 -179.74(15) . . . . ? C4 C5 N1 Ag1 -152.89(13) . . . . ? C6 C5 N1 Ag1 28.10(16) . . . . ? C5 C6 N2 N3 177.35(13) . . . . ? C7 C6 N2 N3 -3.6(2) . . . . ? C5 C6 N2 Ag1 -5.02(19) . . . . ? C7 C6 N2 Ag1 174.09(11) . . . . ? N4 C8 N3 N2 171.72(13) . . . . ? S1 C8 N3 N2 -8.6(2) . . . . ? C6 N2 N3 C8 174.77(14) . . . . ? Ag1 N2 N3 C8 -2.85(18) . . . . ? N3 C8 N4 C12 175.95(15) . . . . ? S1 C8 N4 C12 -3.8(2) . . . . ? N3 C8 N4 C9 2.9(2) . . . . ? S1 C8 N4 C9 -176.81(13) . . . . ? C11 C12 N4 C8 132.63(17) . . . . ? C11 C12 N4 C9 -53.8(2) . . . . ? C10 C9 N4 C8 -132.91(17) . . . . ? C10 C9 N4 C12 53.3(2) . . . . ? C9 C10 O1 C11 58.8(2) . . . . ? C12 C11 O1 C10 -59.18(19) . . . . ? C18 C13 P1 C25 -1.36(15) . . . . ? C14 C13 P1 C25 -178.03(13) . . . . ? C18 C13 P1 C19 -108.77(14) . . . . ? C14 C13 P1 C19 74.56(14) . . . . ? C18 C13 P1 Ag1 125.60(13) . . . . ? C14 C13 P1 Ag1 -51.07(14) . . . . ? C30 C25 P1 C13 106.66(13) . . . . ? C26 C25 P1 C13 -70.63(14) . . . . ? C30 C25 P1 C19 -145.01(13) . . . . ? C26 C25 P1 C19 37.71(15) . . . . ? C30 C25 P1 Ag1 -15.79(14) . . . . ? C26 C25 P1 Ag1 166.93(11) . . . . ? C24 C19 P1 C13 -6.77(16) . . . . ? C20 C19 P1 C13 177.95(12) . . . . ? C24 C19 P1 C25 -115.18(15) . . . . ? C20 C19 P1 C25 69.54(14) . . . . ? C24 C19 P1 Ag1 114.96(14) . . . . ? C20 C19 P1 Ag1 -60.32(14) . . . . ? N3 C8 S1 Ag1 13.15(15) . . . . ? N4 C8 S1 Ag1 -167.15(12) . . . . ? N3 C8 S1 Ag1 -58.81(15) . . . 2_567 ? N4 C8 S1 Ag1 120.89(12) . . . 2_567 ? C13 P1 Ag1 N2 12.78(7) . . . . ? C25 P1 Ag1 N2 131.96(7) . . . . ? C19 P1 Ag1 N2 -105.54(7) . . . . ? C13 P1 Ag1 N1 72.94(6) . . . . ? C25 P1 Ag1 N1 -167.88(6) . . . . ? C19 P1 Ag1 N1 -45.38(7) . . . . ? C13 P1 Ag1 S1 -73.14(6) . . . . ? C25 P1 Ag1 S1 46.04(6) . . . . ? C19 P1 Ag1 S1 168.54(6) . . . . ? C13 P1 Ag1 S1 155.67(5) . . . 2_567 ? C25 P1 Ag1 S1 -85.15(6) . . . 2_567 ? C19 P1 Ag1 S1 37.36(6) . . . 2_567 ? C13 P1 Ag1 Ag1 -133.75(5) . . . 2_567 ? C25 P1 Ag1 Ag1 -14.57(6) . . . 2_567 ? C19 P1 Ag1 Ag1 107.94(6) . . . 2_567 ? C6 N2 Ag1 P1 86.49(12) . . . . ? N3 N2 Ag1 P1 -96.08(11) . . . . ? C6 N2 Ag1 N1 13.82(11) . . . . ? N3 N2 Ag1 N1 -168.75(12) . . . . ? C6 N2 Ag1 S1 -169.67(13) . . . . ? N3 N2 Ag1 S1 7.76(10) . . . . ? C6 N2 Ag1 S1 -61.90(12) . . . 2_567 ? N3 N2 Ag1 S1 115.53(11) . . . 2_567 ? C6 N2 Ag1 Ag1 -114.43(12) . . . 2_567 ? N3 N2 Ag1 Ag1 63.00(11) . . . 2_567 ? C1 N1 Ag1 P1 52.74(14) . . . . ? C5 N1 Ag1 P1 -156.45(10) . . . . ? C1 N1 Ag1 N2 -172.20(15) . . . . ? C5 N1 Ag1 N2 -21.39(10) . . . . ? C1 N1 Ag1 S1 -177.11(12) . . . . ? C5 N1 Ag1 S1 -26.30(13) . . . . ? C1 N1 Ag1 S1 -67.80(14) . . . 2_567 ? C5 N1 Ag1 S1 83.01(11) . . . 2_567 ? C1 N1 Ag1 Ag1 -107.75(14) . . . 2_567 ? C5 N1 Ag1 Ag1 43.06(12) . . . 2_567 ? C8 S1 Ag1 P1 121.27(5) . . . . ? Ag1 S1 Ag1 P1 -136.752(13) 2_567 . . . ? C8 S1 Ag1 N2 -8.34(6) . . . . ? Ag1 S1 Ag1 N2 93.64(3) 2_567 . . . ? C8 S1 Ag1 N1 -3.68(7) . . . . ? Ag1 S1 Ag1 N1 98.30(5) 2_567 . . . ? C8 S1 Ag1 S1 -101.98(5) . . . 2_567 ? Ag1 S1 Ag1 S1 0.0 2_567 . . 2_567 ? C8 S1 Ag1 Ag1 -101.98(5) . . . 2_567 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.667 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.138 data_CCDC637149 _database_code_depnum_ccdc_archive 'CCDC 637149' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H60 Ag2 N8 O2 P2 S2' _chemical_formula_sum 'C60 H60 Ag2 N8 O2 P2 S2' _chemical_formula_weight 1266.96 _chemical_compound_source 'local laboratory' 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' 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.348(2) _cell_length_b 14.701(3) _cell_length_c 15.139(3) _cell_angle_alpha 105.026(2) _cell_angle_beta 102.176(2) _cell_angle_gamma 100.290(2) _cell_volume 2717.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 113 _cell_measurement_reflns_used 9091 _cell_measurement_theta_min 2.9999 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.55 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.909 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7179 _exptl_absorpt_correction_T_max 0.7472 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113 _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 dtintegrate.ref _diffrn_detector_area_resol_mean 14.892 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26421 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.35 _reflns_number_total 9872 _reflns_number_gt 8302 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL ' _computing_publication_material 'WinGX (Farrugia, 1999) ' _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^)+(0.0390P)^2^+6.8187P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9872 _refine_ls_number_parameters 688 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4194(3) 0.0420(3) 0.8388(3) 0.0330(11) Uani 1 1 d . . . H1 H 0.4030 0.0002 0.7755 0.040 Uiso 1 1 calc R . . C2 C 0.3840(4) 0.0089(4) 0.9056(4) 0.0365(11) Uani 1 1 d . . . H2 H 0.3421 -0.0556 0.8897 0.044 Uiso 1 1 calc R . . C3 C 0.4108(4) 0.0719(4) 0.9972(4) 0.0363(11) Uani 1 1 d . . . H3 H 0.3869 0.0486 1.0440 0.044 Uiso 1 1 calc R . . C4 C 0.4677(3) 0.1625(3) 1.0233(3) 0.0154(8) Uani 1 1 d . . . H4 H 0.4828 0.2035 1.0868 0.018 Uiso 1 1 calc R . . C5 C 0.5035(3) 0.1953(3) 0.9581(3) 0.0231(9) Uani 1 1 d . . . C6 C 0.5678(3) 0.2963(3) 0.9895(3) 0.0225(9) Uani 1 1 d . . . C7 C 0.5511(4) 0.3699(3) 1.0710(3) 0.0301(10) Uani 1 1 d . . . H7A H 0.5027 0.3372 1.1000 0.036 Uiso 1 1 calc R . . H7C H 0.5207 0.4181 1.0478 0.036 Uiso 1 1 calc R . . H7B H 0.6192 0.4026 1.1185 0.036 Uiso 1 1 calc R . . C8 C 0.7670(3) 0.4392(3) 0.9399(3) 0.0221(9) Uani 1 1 d . . . C9 C 0.7459(5) 0.6061(4) 0.9972(5) 0.0530(16) Uani 1 1 d . . . H9A H 0.7850 0.6402 1.0646 0.064 Uiso 1 1 calc R . . H9B H 0.6741 0.5714 0.9951 0.064 Uiso 1 1 calc R . . C10 C 0.7379(4) 0.6775(4) 0.9444(4) 0.0468(14) Uani 1 1 d . . . H10A H 0.6925 0.6434 0.8789 0.056 Uiso 1 1 calc R . . H10B H 0.7033 0.7261 0.9754 0.056 Uiso 1 1 calc R . . C11 C 0.8862(5) 0.6570(4) 0.8953(4) 0.0490(14) Uani 1 1 d . . . H11A H 0.9558 0.6919 0.8928 0.059 Uiso 1 1 calc R . . H11B H 0.8428 0.6227 0.8292 0.059 Uiso 1 1 calc R . . C12 C 0.9020(3) 0.5841(3) 0.9464(3) 0.0306(10) Uani 1 1 d . . . H12A H 0.9336 0.5354 0.9111 0.037 Uiso 1 1 calc R . . H12B H 0.9512 0.6171 1.0105 0.037 Uiso 1 1 calc R . . C13 C 0.7936(4) 0.2130(3) 1.0879(4) 0.0357(11) Uani 1 1 d . . . H13 H 0.7583 0.2638 1.0997 0.043 Uiso 1 1 calc R . . C14 C 0.8708(4) 0.2089(3) 1.1620(3) 0.0356(11) Uani 1 1 d . . . H14 H 0.8884 0.2551 1.2234 0.043 Uiso 1 1 calc R . . C15 C 0.9209(4) 0.1356(4) 1.1437(4) 0.0400(12) Uani 1 1 d . . . H15 H 0.9749 0.1301 1.1927 0.048 Uiso 1 1 calc R . . C16 C 0.8935(4) 0.0702(4) 1.0547(3) 0.0324(11) Uani 1 1 d . . . H16 H 0.9282 0.0191 1.0417 0.039 Uiso 1 1 calc R . . C17 C 0.8155(3) 0.0786(3) 0.9842(3) 0.0257(9) Uani 1 1 d . . . C18 C 0.7877(3) 0.0124(3) 0.8863(3) 0.0272(10) Uani 1 1 d . . . C19 C 0.8047(4) -0.0884(3) 0.8672(4) 0.0390(12) Uani 1 1 d . . . H19A H 0.8201 -0.1041 0.9269 0.047 Uiso 1 1 calc R . . H19B H 0.8644 -0.0916 0.8392 0.047 Uiso 1 1 calc R . . H19C H 0.7407 -0.1351 0.8229 0.047 Uiso 1 1 calc R . . C20 C 0.7015(3) 0.0217(3) 0.6596(3) 0.0263(10) Uani 1 1 d . . . C21 C 0.7991(4) -0.0759(4) 0.5695(3) 0.0384(12) Uani 1 1 d . . . H21A H 0.8242 -0.0882 0.6307 0.046 Uiso 1 1 calc R . . H21B H 0.8596 -0.0350 0.5581 0.046 Uiso 1 1 calc R . . C22 C 0.7589(4) -0.1702(3) 0.4911(3) 0.0340(11) Uani 1 1 d . . . H22A H 0.8163 -0.2042 0.4876 0.041 Uiso 1 1 calc R . . H22B H 0.7006 -0.2123 0.5041 0.041 Uiso 1 1 calc R . . C23 C 0.6375(4) -0.1077(4) 0.4069(3) 0.0338(11) Uani 1 1 d . . . H23A H 0.5786 -0.1517 0.4172 0.041 Uiso 1 1 calc R . . H23B H 0.6116 -0.0975 0.3449 0.041 Uiso 1 1 calc R . . C24 C 0.6672(4) -0.0115(3) 0.4840(3) 0.0296(10) Uani 1 1 d . . . H24A H 0.7184 0.0365 0.4696 0.035 Uiso 1 1 calc R . . H24B H 0.6035 0.0135 0.4876 0.035 Uiso 1 1 calc R . . C25 C 0.5330(3) 0.3800(3) 0.6565(3) 0.0188(8) Uani 1 1 d . . . C26 C 0.5348(3) 0.3749(3) 0.7472(3) 0.0242(9) Uani 1 1 d . . . H26 H 0.5954 0.3640 0.7848 0.029 Uiso 1 1 calc R . . C27 C 0.4486(4) 0.3854(3) 0.7833(3) 0.0318(10) Uani 1 1 d . . . H27 H 0.4508 0.3824 0.8456 0.038 Uiso 1 1 calc R . . C28 C 0.3595(3) 0.4003(3) 0.7284(3) 0.0270(10) Uani 1 1 d . . . H28 H 0.3006 0.4079 0.7530 0.032 Uiso 1 1 calc R . . C29 C 0.3570(3) 0.4040(3) 0.6376(3) 0.0261(10) Uani 1 1 d . . . H29 H 0.2957 0.4134 0.5996 0.031 Uiso 1 1 calc R . . C30 C 0.4433(3) 0.3939(3) 0.6013(3) 0.0223(9) Uani 1 1 d . . . H30 H 0.4408 0.3965 0.5389 0.027 Uiso 1 1 calc R . . C31 C 0.6003(3) 0.3175(3) 0.4875(3) 0.0188(8) Uani 1 1 d . . . C32 C 0.6073(3) 0.3710(3) 0.4245(3) 0.0221(9) Uani 1 1 d . . . H32 H 0.6385 0.4390 0.4481 0.027 Uiso 1 1 calc R . . C33 C 0.5684(3) 0.3249(3) 0.3266(3) 0.0280(10) Uani 1 1 d . . . H33 H 0.5738 0.3617 0.2838 0.034 Uiso 1 1 calc R . . C34 C 0.5223(3) 0.2263(3) 0.2917(3) 0.0288(10) Uani 1 1 d . . . H34 H 0.4956 0.1955 0.2251 0.035 Uiso 1 1 calc R . . C35 C 0.5147(3) 0.1722(3) 0.3538(3) 0.0290(10) Uani 1 1 d . . . H35 H 0.4824 0.1044 0.3297 0.035 Uiso 1 1 calc R . . C36 C 0.5543(3) 0.2170(3) 0.4510(3) 0.0233(9) Uani 1 1 d . . . H36 H 0.5502 0.1795 0.4933 0.028 Uiso 1 1 calc R . . C37 C 0.7165(3) 0.4965(3) 0.6310(3) 0.0187(8) Uani 1 1 d . . . C38 C 0.6674(3) 0.5734(3) 0.6448(3) 0.0244(9) Uani 1 1 d . . . H38 H 0.5964 0.5622 0.6489 0.029 Uiso 1 1 calc R . . C39 C 0.7218(3) 0.6662(3) 0.6526(3) 0.0275(10) Uani 1 1 d . . . H39 H 0.6877 0.7180 0.6614 0.033 Uiso 1 1 calc R . . C40 C 0.8251(3) 0.6833(3) 0.6477(3) 0.0275(10) Uani 1 1 d . . . H40 H 0.8620 0.7470 0.6530 0.033 Uiso 1 1 calc R . . C41 C 0.8749(3) 0.6084(3) 0.6351(3) 0.0262(9) Uani 1 1 d . . . H41 H 0.9459 0.6205 0.6312 0.031 Uiso 1 1 calc R . . C42 C 0.8223(3) 0.5158(3) 0.6280(3) 0.0226(9) Uani 1 1 d . . . H42 H 0.8579 0.4650 0.6211 0.027 Uiso 1 1 calc R . . C43 C 0.9085(3) 0.1987(3) 0.5306(3) 0.0186(8) Uani 1 1 d . . . C44 C 0.8328(3) 0.2216(3) 0.4663(3) 0.0249(9) Uani 1 1 d . . . H44 H 0.8008 0.2726 0.4891 0.030 Uiso 1 1 calc R . . C45 C 0.8035(3) 0.1714(3) 0.3700(3) 0.0276(10) Uani 1 1 d . . . H45 H 0.7532 0.1888 0.3270 0.033 Uiso 1 1 calc R . . C46 C 0.8480(3) 0.0959(3) 0.3368(3) 0.0289(10) Uani 1 1 d . . . H46 H 0.8270 0.0601 0.2711 0.035 Uiso 1 1 calc R . . C47 C 0.9227(3) 0.0724(3) 0.3990(3) 0.0291(10) Uani 1 1 d . . . H47 H 0.9533 0.0205 0.3758 0.035 Uiso 1 1 calc R . . C48 C 0.9537(3) 0.1237(3) 0.4951(3) 0.0250(9) Uani 1 1 d . . . H48 H 1.0062 0.1075 0.5371 0.030 Uiso 1 1 calc R . . C49 C 1.0245(3) 0.3795(3) 0.6735(3) 0.0201(8) Uani 1 1 d . . . C50 C 1.0650(3) 0.4413(3) 0.7671(3) 0.0238(9) Uani 1 1 d . . . H50 H 1.0439 0.4223 0.8171 0.029 Uiso 1 1 calc R . . C51 C 1.1356(3) 0.5302(3) 0.7871(3) 0.0294(10) Uani 1 1 d . . . H51 H 1.1638 0.5711 0.8510 0.035 Uiso 1 1 calc R . . C52 C 1.1652(3) 0.5596(3) 0.7150(3) 0.0294(10) Uani 1 1 d . . . H52 H 1.2140 0.6205 0.7292 0.035 Uiso 1 1 calc R . . C53 C 1.1238(3) 0.5005(3) 0.6217(3) 0.0278(10) Uani 1 1 d . . . H53 H 1.1423 0.5215 0.5717 0.033 Uiso 1 1 calc R . . C54 C 1.0547(3) 0.4098(3) 0.6013(3) 0.0237(9) Uani 1 1 d . . . H54 H 1.0281 0.3684 0.5375 0.028 Uiso 1 1 calc R . . C55 C 1.0165(3) 0.2073(3) 0.7229(3) 0.0187(8) Uani 1 1 d . . . C56 C 0.9760(3) 0.1622(3) 0.7824(3) 0.0246(9) Uani 1 1 d . . . H56 H 0.9048 0.1587 0.7844 0.029 Uiso 1 1 calc R . . C57 C 1.0391(4) 0.1222(3) 0.8388(3) 0.0296(10) Uani 1 1 d . . . H57 H 1.0110 0.0918 0.8797 0.036 Uiso 1 1 calc R . . C58 C 1.1425(3) 0.1263(3) 0.8362(3) 0.0269(10) Uani 1 1 d . . . H58 H 1.1854 0.0989 0.8752 0.032 Uiso 1 1 calc R . . C59 C 1.1834(3) 0.1702(3) 0.7768(3) 0.0250(9) Uani 1 1 d . . . H59 H 1.2544 0.1724 0.7744 0.030 Uiso 1 1 calc R . . C60 C 1.1215(3) 0.2112(3) 0.7206(3) 0.0211(9) Uani 1 1 d . . . H60 H 1.1503 0.2420 0.6803 0.025 Uiso 1 1 calc R . . Ag1 Ag 0.71543(3) 0.20190(2) 0.84886(2) 0.02761(10) Uani 1 1 d . . . Ag2 Ag 0.76480(2) 0.28337(2) 0.69532(2) 0.02290(10) Uani 1 1 d . . . N1 N 0.4800(3) 0.1374(3) 0.8634(3) 0.0445(11) Uani 1 1 d . . . N2 N 0.6358(3) 0.3171(2) 0.9432(2) 0.0201(7) Uani 1 1 d . . . N3 N 0.6845(3) 0.4154(2) 0.9717(2) 0.0221(7) Uani 1 1 d . . . N4 N 0.8012(3) 0.5362(3) 0.9545(3) 0.0408(11) Uani 1 1 d . . . N5 N 0.7650(3) 0.1498(3) 0.9999(3) 0.0343(9) Uani 1 1 d . . . N6 N 0.7534(3) 0.0481(2) 0.8189(2) 0.0245(8) Uani 1 1 d . . . N7 N 0.7437(3) -0.0092(2) 0.7296(3) 0.0267(8) Uani 1 1 d . . . N8 N 0.7143(3) -0.0247(3) 0.5743(3) 0.0366(10) Uani 1 1 d . . . P1 P 0.65128(8) 0.37093(7) 0.61665(7) 0.0169(2) Uani 1 1 d . . . P2 P 0.93247(8) 0.26444(7) 0.65538(7) 0.0174(2) Uani 1 1 d . . . S1 S 0.83815(8) 0.36316(7) 0.88498(7) 0.0223(2) Uani 1 1 d . . . S2 S 0.62956(8) 0.11065(7) 0.66588(7) 0.0221(2) Uani 1 1 d . . . O1 O 0.8357(3) 0.7253(3) 0.9401(3) 0.0491(10) Uani 1 1 d . . . O2 O 0.7216(3) -0.1534(2) 0.4031(2) 0.0372(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 C1 0.026(2) 0.023(2) 0.037(3) -0.004(2) 0.003(2) -0.0006(19) C2 0.025(2) 0.031(3) 0.048(3) 0.012(2) 0.005(2) 0.000(2) C3 0.027(2) 0.045(3) 0.043(3) 0.021(2) 0.013(2) 0.008(2) C4 0.0156(18) 0.018(2) 0.0112(18) 0.0038(15) 0.0044(15) 0.0004(16) C5 0.017(2) 0.025(2) 0.026(2) 0.0053(18) 0.0025(17) 0.0076(17) C6 0.020(2) 0.025(2) 0.022(2) 0.0070(18) 0.0037(17) 0.0078(17) C7 0.030(2) 0.031(2) 0.030(2) 0.004(2) 0.016(2) 0.008(2) C8 0.026(2) 0.021(2) 0.018(2) 0.0062(17) 0.0027(17) 0.0067(18) C9 0.066(4) 0.021(3) 0.087(4) 0.013(3) 0.052(3) 0.017(3) C10 0.039(3) 0.031(3) 0.061(4) 0.003(3) 0.006(3) 0.014(2) C11 0.059(4) 0.045(3) 0.060(4) 0.031(3) 0.030(3) 0.017(3) C12 0.026(2) 0.023(2) 0.039(3) 0.009(2) 0.006(2) 0.0017(19) C13 0.035(3) 0.025(2) 0.042(3) 0.008(2) 0.001(2) 0.010(2) C14 0.038(3) 0.033(3) 0.034(3) 0.009(2) 0.008(2) 0.006(2) C15 0.033(3) 0.049(3) 0.038(3) 0.014(2) 0.004(2) 0.016(2) C16 0.033(2) 0.041(3) 0.027(2) 0.013(2) 0.005(2) 0.019(2) C17 0.025(2) 0.024(2) 0.032(2) 0.0143(19) 0.0097(19) 0.0044(18) C18 0.030(2) 0.026(2) 0.030(2) 0.0126(19) 0.0097(19) 0.0096(19) C19 0.055(3) 0.032(3) 0.038(3) 0.015(2) 0.013(2) 0.024(2) C20 0.027(2) 0.018(2) 0.031(2) 0.0068(18) 0.0053(19) 0.0030(18) C21 0.044(3) 0.046(3) 0.028(3) 0.008(2) 0.007(2) 0.028(2) C22 0.040(3) 0.033(3) 0.034(3) 0.012(2) 0.015(2) 0.013(2) C23 0.031(2) 0.041(3) 0.028(2) 0.006(2) 0.010(2) 0.012(2) C24 0.034(2) 0.033(3) 0.023(2) 0.0101(19) 0.0064(19) 0.014(2) C25 0.021(2) 0.0141(19) 0.021(2) 0.0037(16) 0.0059(17) 0.0044(16) C26 0.022(2) 0.029(2) 0.020(2) 0.0072(18) 0.0025(17) 0.0107(18) C27 0.037(3) 0.036(3) 0.027(2) 0.009(2) 0.017(2) 0.011(2) C28 0.024(2) 0.020(2) 0.041(3) 0.0083(19) 0.017(2) 0.0071(18) C29 0.016(2) 0.023(2) 0.038(3) 0.0100(19) 0.0033(18) 0.0046(17) C30 0.020(2) 0.027(2) 0.022(2) 0.0104(18) 0.0039(17) 0.0088(18) C31 0.0128(18) 0.023(2) 0.022(2) 0.0067(17) 0.0061(16) 0.0076(16) C32 0.021(2) 0.026(2) 0.024(2) 0.0100(18) 0.0086(17) 0.0100(18) C33 0.029(2) 0.038(3) 0.021(2) 0.014(2) 0.0059(19) 0.012(2) C34 0.019(2) 0.040(3) 0.022(2) 0.003(2) 0.0030(18) 0.0049(19) C35 0.024(2) 0.024(2) 0.032(2) 0.0008(19) 0.0085(19) -0.0005(18) C36 0.026(2) 0.022(2) 0.025(2) 0.0091(18) 0.0093(18) 0.0061(18) C37 0.020(2) 0.020(2) 0.0170(19) 0.0058(16) 0.0040(16) 0.0063(16) C38 0.022(2) 0.023(2) 0.025(2) 0.0040(18) 0.0006(18) 0.0092(18) C39 0.031(2) 0.021(2) 0.030(2) 0.0095(18) 0.0019(19) 0.0111(19) C40 0.031(2) 0.019(2) 0.027(2) 0.0087(18) 0.0016(19) -0.0009(19) C41 0.021(2) 0.030(2) 0.026(2) 0.0093(19) 0.0061(18) 0.0008(18) C42 0.022(2) 0.023(2) 0.024(2) 0.0082(18) 0.0041(17) 0.0079(17) C43 0.0130(18) 0.017(2) 0.025(2) 0.0043(17) 0.0073(16) 0.0020(16) C44 0.025(2) 0.025(2) 0.026(2) 0.0078(18) 0.0074(18) 0.0100(18) C45 0.027(2) 0.034(2) 0.024(2) 0.0116(19) 0.0042(19) 0.010(2) C46 0.029(2) 0.031(2) 0.020(2) 0.0014(19) 0.0023(19) 0.006(2) C47 0.033(2) 0.023(2) 0.029(2) -0.0004(19) 0.007(2) 0.014(2) C48 0.025(2) 0.026(2) 0.024(2) 0.0057(18) 0.0058(18) 0.0127(18) C49 0.0132(18) 0.021(2) 0.026(2) 0.0063(17) 0.0044(16) 0.0072(16) C50 0.026(2) 0.022(2) 0.023(2) 0.0057(18) 0.0066(18) 0.0065(18) C51 0.027(2) 0.027(2) 0.032(2) 0.0058(19) 0.008(2) 0.0053(19) C52 0.024(2) 0.019(2) 0.044(3) 0.008(2) 0.013(2) 0.0015(18) C53 0.026(2) 0.029(2) 0.035(3) 0.015(2) 0.015(2) 0.0083(19) C54 0.023(2) 0.025(2) 0.028(2) 0.0083(18) 0.0111(18) 0.0111(18) C55 0.018(2) 0.0144(19) 0.020(2) 0.0022(16) 0.0035(16) 0.0033(16) C56 0.020(2) 0.021(2) 0.033(2) 0.0097(19) 0.0075(18) 0.0038(17) C57 0.033(2) 0.030(2) 0.032(2) 0.017(2) 0.010(2) 0.011(2) C58 0.028(2) 0.024(2) 0.026(2) 0.0057(18) 0.0018(19) 0.0124(19) C59 0.021(2) 0.026(2) 0.024(2) 0.0011(18) 0.0024(17) 0.0101(18) C60 0.0164(19) 0.022(2) 0.024(2) 0.0040(17) 0.0063(17) 0.0056(17) Ag1 0.0353(2) 0.02032(18) 0.02902(19) 0.00601(14) 0.01274(15) 0.00898(14) Ag2 0.01942(16) 0.03050(19) 0.02849(18) 0.01711(14) 0.01040(13) 0.01377(13) N1 0.037(2) 0.050(3) 0.039(2) 0.004(2) 0.005(2) 0.011(2) N2 0.0217(17) 0.0214(18) 0.0180(17) 0.0075(14) 0.0036(14) 0.0070(14) N3 0.0293(19) 0.0139(17) 0.0224(18) 0.0037(14) 0.0080(15) 0.0054(15) N4 0.049(3) 0.020(2) 0.067(3) 0.014(2) 0.038(2) 0.0120(18) N5 0.035(2) 0.022(2) 0.039(2) 0.0076(17) 0.0006(18) 0.0067(17) N6 0.0262(19) 0.0212(18) 0.0268(19) 0.0089(15) 0.0067(16) 0.0055(15) N7 0.031(2) 0.0219(19) 0.026(2) 0.0061(16) 0.0069(16) 0.0076(16) N8 0.051(3) 0.038(2) 0.022(2) 0.0053(17) 0.0059(18) 0.027(2) P1 0.0169(5) 0.0176(5) 0.0179(5) 0.0068(4) 0.0038(4) 0.0077(4) P2 0.0153(5) 0.0173(5) 0.0207(5) 0.0060(4) 0.0057(4) 0.0059(4) S1 0.0201(5) 0.0208(5) 0.0242(5) 0.0041(4) 0.0043(4) 0.0069(4) S2 0.0229(5) 0.0200(5) 0.0226(5) 0.0051(4) 0.0061(4) 0.0055(4) O1 0.060(2) 0.037(2) 0.068(3) 0.0298(19) 0.026(2) 0.0229(18) O2 0.0385(18) 0.043(2) 0.0291(18) 0.0032(15) 0.0115(15) 0.0162(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.362(7) . ? C1 N1 1.398(6) . ? C1 H1 0.9500 . ? C2 C3 1.384(7) . ? C2 H2 0.9500 . ? C3 C4 1.321(6) . ? C3 H3 0.9500 . ? C4 C5 1.340(6) . ? C4 H4 0.9500 . ? C5 N1 1.400(6) . ? C5 C6 1.473(6) . ? C6 N2 1.300(5) . ? C6 C7 1.500(6) . ? C7 H7A 0.9800 . ? C7 H7C 0.9800 . ? C7 H7B 0.9800 . ? C8 N3 1.318(5) . ? C8 N4 1.359(6) . ? C8 S1 1.752(4) . ? C9 N4 1.465(6) . ? C9 C10 1.480(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O1 1.390(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O1 1.414(7) . ? C11 C12 1.494(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N4 1.448(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N5 1.341(6) . ? C13 C14 1.377(7) . ? C13 H13 0.9500 . ? C14 C15 1.366(7) . ? C14 H14 0.9500 . ? C15 C16 1.366(7) . ? C15 H15 0.9500 . ? C16 C17 1.371(6) . ? C16 H16 0.9500 . ? C17 N5 1.341(6) . ? C17 C18 1.473(6) . ? C18 N6 1.302(6) . ? C18 C19 1.501(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N7 1.318(6) . ? C20 N8 1.356(6) . ? C20 S2 1.750(5) . ? C21 N8 1.472(6) . ? C21 C22 1.493(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O2 1.420(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O2 1.410(6) . ? C23 C24 1.506(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N8 1.455(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.388(6) . ? C25 C26 1.390(6) . ? C25 P1 1.818(4) . ? C26 C27 1.388(6) . ? C26 H26 0.9500 . ? C27 C28 1.387(6) . ? C27 H27 0.9500 . ? C28 C29 1.383(6) . ? C28 H28 0.9500 . ? C29 C30 1.390(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.392(6) . ? C31 C36 1.404(6) . ? C31 P1 1.831(5) . ? C32 C33 1.398(6) . ? C32 H32 0.9500 . ? C33 C34 1.380(7) . ? C33 H33 0.9500 . ? C34 C35 1.387(7) . ? C34 H34 0.9500 . ? C35 C36 1.387(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.397(6) . ? C37 C42 1.401(6) . ? C37 P1 1.830(5) . ? C38 C39 1.387(6) . ? C38 H38 0.9500 . ? C39 C40 1.377(6) . ? C39 H39 0.9500 . ? C40 C41 1.377(6) . ? C40 H40 0.9500 . ? C41 C42 1.380(6) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.390(6) . ? C43 C44 1.399(6) . ? C43 P2 1.815(5) . ? C44 C45 1.386(6) . ? C44 H44 0.9500 . ? C45 C46 1.382(6) . ? C45 H45 0.9500 . ? C46 C47 1.377(6) . ? C46 H46 0.9500 . ? C47 C48 1.387(6) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.389(6) . ? C49 C50 1.400(6) . ? C49 P2 1.820(5) . ? C50 C51 1.385(6) . ? C50 H50 0.9500 . ? C51 C52 1.379(6) . ? C51 H51 0.9500 . ? C52 C53 1.384(7) . ? C52 H52 0.9500 . ? C53 C54 1.396(6) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.389(6) . ? C55 C60 1.401(6) . ? C55 P2 1.818(4) . ? C56 C57 1.383(6) . ? C56 H56 0.9500 . ? C57 C58 1.380(6) . ? C57 H57 0.9500 . ? C58 C59 1.380(6) . ? C58 H58 0.9500 . ? C59 C60 1.384(6) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? Ag1 N6 2.355(5) . ? Ag1 N2 2.462(4) . ? Ag1 S1 2.481(3) . ? Ag1 N5 2.588(5) . ? Ag1 S2 2.640(3) . ? Ag1 Ag2 3.012(3) . ? Ag1 N1 3.186(5) . ? Ag2 P1 2.470(2) . ? Ag2 P2 2.481(2) . ? Ag2 S1 2.690(3) . ? Ag2 S2 2.707(4) . ? N2 N3 1.384(5) . ? N6 N7 1.360(5) . ? 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 C2 C1 N1 120.0(4) . . ? C2 C1 H1 120.0 . . ? N1 C1 H1 120.0 . . ? C1 C2 C3 118.1(5) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C4 C3 C2 123.8(5) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C3 C4 C5 118.5(4) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C4 C5 N1 122.0(4) . . ? C4 C5 C6 117.3(4) . . ? N1 C5 C6 120.7(4) . . ? N2 C6 C5 117.3(4) . . ? N2 C6 C7 123.3(4) . . ? C5 C6 C7 119.4(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? H7C C7 H7B 109.5 . . ? N3 C8 N4 114.3(4) . . ? N3 C8 S1 128.5(3) . . ? N4 C8 S1 117.2(3) . . ? N4 C9 C10 109.5(5) . . ? N4 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? N4 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? O1 C10 C9 112.9(4) . . ? O1 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? O1 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? O1 C11 C12 112.1(4) . . ? O1 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? O1 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N4 C12 C11 109.5(4) . . ? N4 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? N4 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? N5 C13 C14 124.1(5) . . ? N5 C13 H13 117.9 . . ? C14 C13 H13 117.9 . . ? C15 C14 C13 117.2(5) . . ? C15 C14 H14 121.4 . . ? C13 C14 H14 121.4 . . ? C14 C15 C16 120.0(5) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 119.7(5) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N5 C17 C16 121.8(4) . . ? N5 C17 C18 117.0(4) . . ? C16 C17 C18 121.1(4) . . ? N6 C18 C17 116.3(4) . . ? N6 C18 C19 122.8(4) . . ? C17 C18 C19 120.8(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N7 C20 N8 114.1(4) . . ? N7 C20 S2 127.0(4) . . ? N8 C20 S2 118.9(3) . . ? N8 C21 C22 109.8(4) . . ? N8 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? N8 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? O2 C22 C21 110.1(4) . . ? O2 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? O2 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.2 . . ? O2 C23 C24 113.7(4) . . ? O2 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? O2 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N8 C24 C23 109.0(4) . . ? N8 C24 H24A 109.9 . . ? C23 C24 H24A 109.9 . . ? N8 C24 H24B 109.9 . . ? C23 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C30 C25 C26 119.3(4) . . ? C30 C25 P1 122.9(3) . . ? C26 C25 P1 117.8(3) . . ? C27 C26 C25 120.5(4) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C26 120.0(4) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 119.5(4) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 120.7(4) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C25 C30 C29 119.9(4) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C36 119.0(4) . . ? C32 C31 P1 123.3(3) . . ? C36 C31 P1 117.8(3) . . ? C31 C32 C33 120.1(4) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 120.3(4) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.1(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C36 120.0(4) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.5(4) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C38 C37 C42 118.6(4) . . ? C38 C37 P1 124.0(3) . . ? C42 C37 P1 117.4(3) . . ? C39 C38 C37 120.2(4) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C40 C39 C38 120.3(4) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 120.1(4) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C40 C41 C42 120.5(4) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 120.2(4) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? C48 C43 C44 118.1(4) . . ? C48 C43 P2 125.2(3) . . ? C44 C43 P2 116.5(3) . . ? C45 C44 C43 121.2(4) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C46 C45 C44 119.6(4) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C47 C46 C45 120.0(4) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.5(4) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C47 C48 C43 120.5(4) . . ? C47 C48 H48 119.7 . . ? C43 C48 H48 119.7 . . ? C54 C49 C50 118.8(4) . . ? C54 C49 P2 124.6(3) . . ? C50 C49 P2 116.6(3) . . ? C51 C50 C49 120.3(4) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C52 C51 C50 120.5(4) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C51 C52 C53 120.0(4) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C52 C53 C54 119.8(4) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C49 C54 C53 120.6(4) . . ? C49 C54 H54 119.7 . . ? C53 C54 H54 119.7 . . ? C56 C55 C60 119.0(4) . . ? C56 C55 P2 118.4(3) . . ? C60 C55 P2 122.5(3) . . ? C57 C56 C55 120.2(4) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C58 C57 C56 120.4(4) . . ? C58 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C59 C58 C57 119.9(4) . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C58 C59 C60 120.3(4) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C59 C60 C55 120.1(4) . . ? C59 C60 H60 120.0 . . ? C55 C60 H60 120.0 . . ? N6 Ag1 N2 146.12(12) . . ? N6 Ag1 S1 128.39(12) . . ? N2 Ag1 S1 75.61(12) . . ? N6 Ag1 N5 66.48(13) . . ? N2 Ag1 N5 85.39(14) . . ? S1 Ag1 N5 105.31(11) . . ? N6 Ag1 S2 73.46(10) . . ? N2 Ag1 S2 122.34(9) . . ? S1 Ag1 S2 114.43(6) . . ? N5 Ag1 S2 135.57(12) . . ? N6 Ag1 Ag2 106.96(11) . . ? N2 Ag1 Ag2 106.49(12) . . ? S1 Ag1 Ag2 57.66(6) . . ? N5 Ag1 Ag2 154.00(10) . . ? S2 Ag1 Ag2 56.78(9) . . ? N6 Ag1 N1 97.98(13) . . ? N2 Ag1 N1 58.75(13) . . ? S1 Ag1 N1 132.83(9) . . ? N5 Ag1 N1 83.59(13) . . ? S2 Ag1 N1 83.67(10) . . ? Ag2 Ag1 N1 122.39(9) . . ? P1 Ag2 P2 120.75(6) . . ? P1 Ag2 S1 114.31(8) . . ? P2 Ag2 S1 99.76(6) . . ? P1 Ag2 S2 102.99(10) . . ? P2 Ag2 S2 112.64(8) . . ? S1 Ag2 S2 105.85(6) . . ? P1 Ag2 Ag1 122.99(6) . . ? P2 Ag2 Ag1 116.20(4) . . ? S1 Ag2 Ag1 51.21(8) . . ? S2 Ag2 Ag1 54.66(6) . . ? C1 N1 C5 117.6(4) . . ? C1 N1 Ag1 126.3(3) . . ? C5 N1 Ag1 93.8(3) . . ? C6 N2 N3 112.9(3) . . ? C6 N2 Ag1 126.4(3) . . ? N3 N2 Ag1 118.4(2) . . ? C8 N3 N2 115.9(3) . . ? C8 N4 C12 125.5(4) . . ? C8 N4 C9 121.8(4) . . ? C12 N4 C9 111.9(4) . . ? C13 N5 C17 117.2(4) . . ? C13 N5 Ag1 122.7(3) . . ? C17 N5 Ag1 110.3(3) . . ? C18 N6 N7 114.8(4) . . ? C18 N6 Ag1 122.8(3) . . ? N7 N6 Ag1 122.4(3) . . ? C20 N7 N6 116.1(4) . . ? C20 N8 C24 125.4(4) . . ? C20 N8 C21 120.3(4) . . ? C24 N8 C21 112.8(4) . . ? C25 P1 C37 104.46(19) . . ? C25 P1 C31 103.72(18) . . ? C37 P1 C31 102.92(18) . . ? C25 P1 Ag2 114.74(14) . . ? C37 P1 Ag2 114.61(15) . . ? C31 P1 Ag2 114.93(14) . . ? C43 P2 C55 107.2(2) . . ? C43 P2 C49 104.56(19) . . ? C55 P2 C49 101.1(2) . . ? C43 P2 Ag2 111.21(13) . . ? C55 P2 Ag2 118.00(14) . . ? C49 P2 Ag2 113.59(15) . . ? C8 S1 Ag1 100.29(17) . . ? C8 S1 Ag2 116.29(14) . . ? Ag1 S1 Ag2 71.13(5) . . ? C20 S2 Ag1 95.52(16) . . ? C20 S2 Ag2 108.20(18) . . ? Ag1 S2 Ag2 68.56(6) . . ? C10 O1 C11 109.9(4) . . ? C23 O2 C22 109.7(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.027 _refine_diff_density_min -1.287 _refine_diff_density_rms 0.098