Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Kaden, Thomas' 'Alberto, Roger' 'Baumeister, Jan M.' 'Ortner, Kirsten' 'Spingler, Bernhard' _publ_contact_author_name 'Prof Thomas Kaden' _publ_contact_author_address ; Department of Chemistry University of Basel Spitalstrasse 51 CH-4056 Basel SWITZERLAND ; _publ_contact_author_email 'TH.KADEN@UNIBAS.CH' _publ_section_title ; Central vs. peripheral Ag(I) coordination in NS3-open chain and cage ligands ; data_jb260899_[Cu(4)PF6] _database_code_CSD 186809 _audit_creation_method SHELXL-97 _chemical_name_systematic '[Copper(I)(tris(2-benzylsulfanyl-ethyl)-amin)]PF6' _chemical_name_common [Cu(NS3Ph)]PF6 _chemical_melting_point ? _chemical_formula_moiety [Cu(NS3Ph)]PF6 _chemical_formula_sum 'C27 H33 Cu F6 N P S3' _chemical_formula_weight 676.23 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' 'Cu' 'Cu' 0.3201 1.2651 '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 9.0477(6) _cell_length_b 11.6121(8) _cell_length_c 14.9961(11) _cell_angle_alpha 107.744(8) _cell_angle_beta 98.854(8) _cell_angle_gamma 93.950(8) _cell_volume 1471.43(18) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 343 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.066 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6807 _exptl_absorpt_correction_T_max 0.8274 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method '/f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 50-200 _diffrn_standards_interval_count 'every image' _diffrn_standards_interval_time 3.3 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16579 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 30.31 _reflns_number_total 8014 _reflns_number_gt 5709 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1999)' _computing_cell_refinement 'IPDS (Stoe, 1999)' _computing_data_reduction 'X-RED (Stoe, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Zortep (Zsolnai, 1994), Platon (Spek, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0951P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8014 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1491 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.15853(4) 0.11260(3) 0.72758(2) 0.03196(11) Uani 1 1 d . . . N N 0.2052(3) 0.00738(19) 0.82522(16) 0.0326(5) Uani 1 1 d . . . S1 S 0.15147(9) -0.05590(6) 0.60171(5) 0.03538(16) Uani 1 1 d . . . S2 S 0.37461(8) 0.24012(5) 0.79921(5) 0.03248(15) Uani 1 1 d . . . S3 S -0.04783(8) 0.17262(6) 0.78940(6) 0.03945(17) Uani 1 1 d . . . C1 C 0.1781(4) -0.1231(2) 0.7673(2) 0.0371(6) Uani 1 1 d . . . H1A H 0.0688 -0.1514 0.7548 0.045 Uiso 1 1 calc R . . H1B H 0.2310 -0.1710 0.8038 0.045 Uiso 1 1 calc R . . C2 C 0.2321(4) -0.1464(2) 0.67272(19) 0.0370(6) Uani 1 1 d . . . H2A H 0.2059 -0.2339 0.6354 0.044 Uiso 1 1 calc R . . H2B H 0.3433 -0.1282 0.6855 0.044 Uiso 1 1 calc R . . C3 C -0.0408(4) -0.1337(3) 0.5584(2) 0.0441(7) Uani 1 1 d . . . H3A H -0.0854 -0.1393 0.6135 0.053 Uiso 1 1 calc R . . H3B H -0.1020 -0.0844 0.5272 0.053 Uiso 1 1 calc R . . C4 C 0.3648(4) 0.0439(3) 0.8729(2) 0.0368(6) Uani 1 1 d . . . H4A H 0.4298 -0.0009 0.8303 0.044 Uiso 1 1 calc R . . H4B H 0.3807 0.0206 0.9316 0.044 Uiso 1 1 calc R . . C5 C 0.4119(4) 0.1807(3) 0.89880(19) 0.0370(6) Uani 1 1 d . . . H5A H 0.5212 0.1984 0.9256 0.044 Uiso 1 1 calc R . . H5B H 0.3580 0.2245 0.9492 0.044 Uiso 1 1 calc R . . C6 C 0.5269(3) 0.1857(3) 0.7356(2) 0.0367(6) Uani 1 1 d . . . H6A H 0.6257 0.2173 0.7785 0.044 Uiso 1 1 calc R . . H6B H 0.5169 0.0955 0.7150 0.044 Uiso 1 1 calc R . . C7 C 0.1016(4) 0.0372(3) 0.8939(2) 0.0392(6) Uani 1 1 d . . . H7A H 0.1469 0.1116 0.9470 0.047 Uiso 1 1 calc R . . H7B H 0.0898 -0.0301 0.9208 0.047 Uiso 1 1 calc R . . C8 C -0.0541(4) 0.0577(3) 0.8492(2) 0.0420(7) Uani 1 1 d . . . H8A H -0.1151 0.0829 0.8997 0.050 Uiso 1 1 calc R . . H8B H -0.1052 -0.0203 0.8026 0.050 Uiso 1 1 calc R . . C9 C 0.0193(4) 0.3129(3) 0.8896(3) 0.0450(7) Uani 1 1 d . . . H9A H 0.1113 0.3002 0.9288 0.054 Uiso 1 1 calc R . . H9B H 0.0472 0.3792 0.8642 0.054 Uiso 1 1 calc R . . C11 C -0.0492(4) -0.2602(3) 0.4887(2) 0.0480(8) Uani 1 1 d . . . C12 C -0.1433(7) -0.3530(4) 0.4989(5) 0.0916(18) Uani 1 1 d . . . H12 H -0.1974 -0.3369 0.5500 0.110 Uiso 1 1 calc R . . C13 C -0.1580(9) -0.4686(5) 0.4346(6) 0.141(3) Uani 1 1 d . . . H13 H -0.2220 -0.5322 0.4419 0.169 Uiso 1 1 calc R . . C14 C -0.0811(9) -0.4929(5) 0.3600(4) 0.109(2) Uani 1 1 d . . . H14 H -0.0954 -0.5721 0.3144 0.131 Uiso 1 1 calc R . . C15 C 0.0164(8) -0.4026(5) 0.3513(3) 0.0892(17) Uani 1 1 d . . . H15 H 0.0726 -0.4198 0.3012 0.107 Uiso 1 1 calc R . . C16 C 0.0324(6) -0.2858(4) 0.4161(3) 0.0724(13) Uani 1 1 d . . . H16 H 0.1000 -0.2233 0.4103 0.087 Uiso 1 1 calc R . . C21 C 0.5190(3) 0.2287(2) 0.6500(2) 0.0363(6) Uani 1 1 d . . . C22 C 0.4646(4) 0.1480(3) 0.5591(2) 0.0422(7) Uani 1 1 d . . . H22 H 0.4274 0.0663 0.5512 0.051 Uiso 1 1 calc R . . C23 C 0.4641(4) 0.1853(3) 0.4797(2) 0.0492(8) Uani 1 1 d . . . H23 H 0.4267 0.1293 0.4179 0.059 Uiso 1 1 calc R . . C24 C 0.5177(5) 0.3038(3) 0.4902(2) 0.0562(9) Uani 1 1 d . . . H24 H 0.5190 0.3289 0.4357 0.067 Uiso 1 1 calc R . . C25 C 0.5691(6) 0.3855(3) 0.5798(3) 0.0630(11) Uani 1 1 d . . . H25 H 0.6048 0.4672 0.5868 0.076 Uiso 1 1 calc R . . C26 C 0.5694(5) 0.3492(3) 0.6602(2) 0.0512(8) Uani 1 1 d . . . H26 H 0.6038 0.4064 0.7219 0.061 Uiso 1 1 calc R . . C31 C -0.0946(3) 0.3517(2) 0.9513(2) 0.0366(6) Uani 1 1 d . . . C32 C -0.0956(4) 0.3202(3) 1.0338(3) 0.0526(9) Uani 1 1 d . . . H32 H -0.0227 0.2721 1.0513 0.063 Uiso 1 1 calc R . . C33 C -0.2017(5) 0.3582(3) 1.0905(3) 0.0599(10) Uani 1 1 d . . . H33 H -0.2006 0.3361 1.1466 0.072 Uiso 1 1 calc R . . C34 C -0.3089(4) 0.4278(3) 1.0665(3) 0.0506(8) Uani 1 1 d . . . H34 H -0.3821 0.4528 1.1053 0.061 Uiso 1 1 calc R . . C35 C -0.3086(4) 0.4609(3) 0.9850(2) 0.0425(7) Uani 1 1 d . . . H35 H -0.3807 0.5103 0.9685 0.051 Uiso 1 1 calc R . . C36 C -0.2045(3) 0.4225(2) 0.9282(2) 0.0361(6) Uani 1 1 d . . . H36 H -0.2070 0.4444 0.8719 0.043 Uiso 1 1 calc R . . P P -0.34460(10) -0.24707(6) 0.80827(5) 0.03818(18) Uani 1 1 d . . . F1 F -0.4226(6) -0.1710(4) 0.8888(2) 0.154(2) Uani 1 1 d . . . F2 F -0.2755(6) -0.3268(4) 0.7273(3) 0.1352(17) Uani 1 1 d . . . F3 F -0.3647(3) -0.1468(2) 0.75602(19) 0.0763(8) Uani 1 1 d . . . F4 F -0.3279(3) -0.3441(2) 0.8631(2) 0.0815(8) Uani 1 1 d . . . F5 F -0.1848(4) -0.1836(3) 0.8645(3) 0.1171(15) Uani 1 1 d . . . F6 F -0.5033(4) -0.3127(3) 0.7493(3) 0.1115(13) 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 Cu 0.0299(2) 0.03094(16) 0.03795(18) 0.01535(13) 0.00531(13) 0.00500(12) N 0.0392(14) 0.0282(9) 0.0320(10) 0.0115(8) 0.0072(9) 0.0046(9) S1 0.0378(4) 0.0339(3) 0.0336(3) 0.0128(2) 0.0018(3) 0.0005(3) S2 0.0317(4) 0.0285(3) 0.0368(3) 0.0093(2) 0.0072(3) 0.0040(2) S3 0.0285(4) 0.0339(3) 0.0572(4) 0.0156(3) 0.0092(3) 0.0051(3) C1 0.0472(18) 0.0271(11) 0.0402(14) 0.0152(10) 0.0077(12) 0.0070(11) C2 0.0423(17) 0.0323(12) 0.0359(13) 0.0106(10) 0.0042(11) 0.0107(11) C3 0.0384(18) 0.0442(15) 0.0479(16) 0.0196(13) -0.0041(13) -0.0025(12) C4 0.0406(17) 0.0388(13) 0.0327(12) 0.0150(10) 0.0028(11) 0.0086(11) C5 0.0373(16) 0.0399(13) 0.0315(12) 0.0092(10) 0.0039(11) 0.0046(11) C6 0.0310(15) 0.0406(13) 0.0443(15) 0.0166(11) 0.0162(11) 0.0103(11) C7 0.0460(19) 0.0376(13) 0.0398(14) 0.0174(11) 0.0154(12) 0.0049(12) C8 0.0400(18) 0.0335(13) 0.0549(17) 0.0138(12) 0.0181(14) 0.0012(11) C9 0.0279(15) 0.0318(13) 0.071(2) 0.0119(13) 0.0064(14) 0.0023(10) C11 0.0434(19) 0.0467(16) 0.0470(16) 0.0167(13) -0.0114(14) -0.0049(13) C12 0.078(4) 0.053(2) 0.131(5) 0.003(3) 0.045(3) -0.018(2) C13 0.137(7) 0.064(3) 0.186(8) -0.027(4) 0.084(6) -0.044(3) C14 0.131(6) 0.069(3) 0.086(4) -0.018(3) 0.007(4) -0.040(3) C15 0.135(5) 0.079(3) 0.0348(18) 0.0001(19) 0.009(2) -0.013(3) C16 0.109(4) 0.063(2) 0.0358(17) 0.0129(16) 0.006(2) -0.022(2) C21 0.0375(16) 0.0354(12) 0.0392(14) 0.0140(11) 0.0109(11) 0.0076(11) C22 0.0464(19) 0.0361(13) 0.0444(15) 0.0075(11) 0.0187(13) 0.0079(12) C23 0.055(2) 0.0496(17) 0.0403(15) 0.0062(13) 0.0159(14) 0.0125(15) C24 0.078(3) 0.0570(19) 0.0419(17) 0.0223(15) 0.0190(17) 0.0181(18) C25 0.093(3) 0.0397(16) 0.060(2) 0.0232(15) 0.015(2) 0.0003(17) C26 0.069(3) 0.0377(15) 0.0430(16) 0.0113(13) 0.0063(16) -0.0007(14) C31 0.0292(15) 0.0256(11) 0.0518(16) 0.0113(10) 0.0014(12) 0.0010(9) C32 0.061(2) 0.0373(14) 0.061(2) 0.0239(14) -0.0009(17) 0.0104(14) C33 0.092(3) 0.0417(16) 0.0521(19) 0.0233(15) 0.0170(19) 0.0026(17) C34 0.055(2) 0.0356(14) 0.061(2) 0.0103(14) 0.0227(17) 0.0005(13) C35 0.0366(17) 0.0349(13) 0.0526(17) 0.0104(12) 0.0052(13) 0.0046(11) C36 0.0336(15) 0.0299(11) 0.0425(14) 0.0116(10) 0.0005(11) 0.0038(10) P 0.0461(5) 0.0346(3) 0.0339(3) 0.0131(3) 0.0032(3) 0.0043(3) F1 0.266(6) 0.171(4) 0.0677(18) 0.052(2) 0.065(3) 0.166(4) F2 0.173(4) 0.157(4) 0.083(2) 0.017(2) 0.057(2) 0.089(3) F3 0.0813(18) 0.0740(15) 0.0783(15) 0.0527(13) -0.0195(13) -0.0122(12) F4 0.0774(19) 0.0807(16) 0.117(2) 0.0720(17) 0.0221(16) 0.0205(13) F5 0.096(2) 0.099(2) 0.150(3) 0.089(2) -0.070(2) -0.0495(17) F6 0.076(2) 0.125(3) 0.133(3) 0.075(2) -0.031(2) -0.0332(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 Cu N 2.188(2) . ? Cu S1 2.2561(8) . ? Cu S3 2.2692(9) . ? Cu S2 2.2701(8) . ? N C7 1.478(4) . ? N C4 1.480(4) . ? N C1 1.480(3) . ? S1 C2 1.822(3) . ? S1 C3 1.828(3) . ? S2 C5 1.824(3) . ? S2 C6 1.834(3) . ? S3 C8 1.823(3) . ? S3 C9 1.836(3) . ? C1 C2 1.524(4) . ? C3 C11 1.510(5) . ? C4 C5 1.529(4) . ? C6 C21 1.507(4) . ? C7 C8 1.531(5) . ? C9 C31 1.492(5) . ? C11 C16 1.379(6) . ? C11 C12 1.387(6) . ? C12 C13 1.377(7) . ? C13 C14 1.375(9) . ? C14 C15 1.373(8) . ? C15 C16 1.389(6) . ? C21 C22 1.390(4) . ? C21 C26 1.397(4) . ? C22 C23 1.385(5) . ? C23 C24 1.380(5) . ? C24 C25 1.375(5) . ? C25 C26 1.394(5) . ? C31 C32 1.393(5) . ? C31 C36 1.402(4) . ? C32 C33 1.386(6) . ? C33 C34 1.379(5) . ? C34 C35 1.389(5) . ? C35 C36 1.374(5) . ? P F2 1.534(3) . ? P F1 1.560(3) . ? P F5 1.563(3) . ? P F6 1.572(3) . ? P F4 1.587(2) . ? P F3 1.595(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 N Cu S1 90.48(6) . . ? N Cu S3 90.75(7) . . ? S1 Cu S3 123.45(3) . . ? N Cu S2 90.71(7) . . ? S1 Cu S2 121.93(3) . . ? S3 Cu S2 114.58(3) . . ? C7 N C4 111.8(2) . . ? C7 N C1 111.5(2) . . ? C4 N C1 111.3(2) . . ? C7 N Cu 107.54(16) . . ? C4 N Cu 107.13(16) . . ? C1 N Cu 107.31(16) . . ? C2 S1 C3 101.22(14) . . ? C2 S1 Cu 94.84(9) . . ? C3 S1 Cu 110.54(12) . . ? C5 S2 C6 100.70(13) . . ? C5 S2 Cu 94.82(10) . . ? C6 S2 Cu 109.28(10) . . ? C8 S3 C9 102.14(15) . . ? C8 S3 Cu 94.04(11) . . ? C9 S3 Cu 105.86(11) . . ? N C1 C2 112.3(2) . . ? C1 C2 S1 113.49(19) . . ? C11 C3 S1 113.3(2) . . ? N C4 C5 112.5(2) . . ? C4 C5 S2 114.34(19) . . ? C21 C6 S2 109.41(19) . . ? N C7 C8 113.0(2) . . ? C7 C8 S3 113.6(2) . . ? C31 C9 S3 113.2(2) . . ? C16 C11 C12 119.4(4) . . ? C16 C11 C3 122.4(3) . . ? C12 C11 C3 118.1(4) . . ? C13 C12 C11 119.7(5) . . ? C14 C13 C12 120.7(6) . . ? C15 C14 C13 119.9(5) . . ? C14 C15 C16 119.7(5) . . ? C11 C16 C15 120.4(4) . . ? C22 C21 C26 118.8(3) . . ? C22 C21 C6 120.4(3) . . ? C26 C21 C6 120.8(3) . . ? C23 C22 C21 120.7(3) . . ? C24 C23 C22 120.1(3) . . ? C25 C24 C23 119.9(3) . . ? C24 C25 C26 120.5(3) . . ? C25 C26 C21 119.9(3) . . ? C32 C31 C36 117.6(3) . . ? C32 C31 C9 121.8(3) . . ? C36 C31 C9 120.6(3) . . ? C33 C32 C31 120.7(3) . . ? C34 C33 C32 120.8(3) . . ? C33 C34 C35 119.2(3) . . ? C36 C35 C34 120.2(3) . . ? C35 C36 C31 121.5(3) . . ? F2 P F1 176.9(3) . . ? F2 P F5 91.0(3) . . ? F1 P F5 91.8(3) . . ? F2 P F6 87.4(3) . . ? F1 P F6 89.7(3) . . ? F5 P F6 178.4(2) . . ? F2 P F4 90.9(2) . . ? F1 P F4 88.11(18) . . ? F5 P F4 87.96(15) . . ? F6 P F4 92.28(17) . . ? F2 P F3 91.2(2) . . ? F1 P F3 89.79(18) . . ? F5 P F3 92.22(14) . . ? F6 P F3 87.60(15) . . ? F4 P F3 177.89(17) . . ? 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 S1 Cu N C7 -131.99(17) . . . . ? S3 Cu N C7 -8.53(17) . . . . ? S2 Cu N C7 106.07(17) . . . . ? S1 Cu N C4 107.70(16) . . . . ? S3 Cu N C4 -128.83(16) . . . . ? S2 Cu N C4 -14.24(16) . . . . ? S1 Cu N C1 -11.97(18) . . . . ? S3 Cu N C1 111.50(18) . . . . ? S2 Cu N C1 -133.91(18) . . . . ? N Cu S1 C2 -12.47(13) . . . . ? S3 Cu S1 C2 -103.68(11) . . . . ? S2 Cu S1 C2 78.66(11) . . . . ? N Cu S1 C3 91.43(12) . . . . ? S3 Cu S1 C3 0.22(11) . . . . ? S2 Cu S1 C3 -177.44(10) . . . . ? N Cu S2 C5 -9.91(11) . . . . ? S1 Cu S2 C5 -100.91(10) . . . . ? S3 Cu S2 C5 81.24(10) . . . . ? N Cu S2 C6 93.21(11) . . . . ? S1 Cu S2 C6 2.21(10) . . . . ? S3 Cu S2 C6 -175.64(10) . . . . ? N Cu S3 C8 -15.04(12) . . . . ? S1 Cu S3 C8 76.03(11) . . . . ? S2 Cu S3 C8 -106.16(11) . . . . ? N Cu S3 C9 88.80(13) . . . . ? S1 Cu S3 C9 179.87(11) . . . . ? S2 Cu S3 C9 -2.32(12) . . . . ? C7 N C1 C2 156.4(2) . . . . ? C4 N C1 C2 -78.0(3) . . . . ? Cu N C1 C2 38.9(3) . . . . ? N C1 C2 S1 -55.2(3) . . . . ? C3 S1 C2 C1 -74.3(2) . . . . ? Cu S1 C2 C1 37.8(2) . . . . ? C2 S1 C3 C11 -68.0(2) . . . . ? Cu S1 C3 C11 -167.60(19) . . . . ? C7 N C4 C5 -77.7(3) . . . . ? C1 N C4 C5 156.9(2) . . . . ? Cu N C4 C5 39.8(3) . . . . ? N C4 C5 S2 -53.9(3) . . . . ? C6 S2 C5 C4 -75.8(2) . . . . ? Cu S2 C5 C4 34.9(2) . . . . ? C5 S2 C6 C21 -178.5(2) . . . . ? Cu S2 C6 C21 82.4(2) . . . . ? C4 N C7 C8 153.2(2) . . . . ? C1 N C7 C8 -81.5(3) . . . . ? Cu N C7 C8 35.9(3) . . . . ? N C7 C8 S3 -54.6(3) . . . . ? C9 S3 C8 C7 -67.8(2) . . . . ? Cu S3 C8 C7 39.4(2) . . . . ? C8 S3 C9 C31 -70.3(2) . . . . ? Cu S3 C9 C31 -168.08(19) . . . . ? S1 C3 C11 C16 -43.8(4) . . . . ? S1 C3 C11 C12 136.3(4) . . . . ? C16 C11 C12 C13 -2.2(9) . . . . ? C3 C11 C12 C13 177.7(6) . . . . ? C11 C12 C13 C14 -0.4(13) . . . . ? C12 C13 C14 C15 2.7(14) . . . . ? C13 C14 C15 C16 -2.4(11) . . . . ? C12 C11 C16 C15 2.5(7) . . . . ? C3 C11 C16 C15 -177.4(4) . . . . ? C14 C15 C16 C11 -0.2(8) . . . . ? S2 C6 C21 C22 -104.9(3) . . . . ? S2 C6 C21 C26 76.6(4) . . . . ? C26 C21 C22 C23 1.7(5) . . . . ? C6 C21 C22 C23 -176.7(3) . . . . ? C21 C22 C23 C24 -0.1(5) . . . . ? C22 C23 C24 C25 -1.2(6) . . . . ? C23 C24 C25 C26 0.8(7) . . . . ? C24 C25 C26 C21 0.9(7) . . . . ? C22 C21 C26 C25 -2.1(6) . . . . ? C6 C21 C26 C25 176.4(4) . . . . ? S3 C9 C31 C32 95.1(3) . . . . ? S3 C9 C31 C36 -85.3(3) . . . . ? C36 C31 C32 C33 -0.2(5) . . . . ? C9 C31 C32 C33 179.4(3) . . . . ? C31 C32 C33 C34 0.2(6) . . . . ? C32 C33 C34 C35 -0.7(6) . . . . ? C33 C34 C35 C36 1.3(5) . . . . ? C34 C35 C36 C31 -1.3(4) . . . . ? C32 C31 C36 C35 0.8(4) . . . . ? C9 C31 C36 C35 -178.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 30.31 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 0.973 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.097 #===END data_jb030400_[Ag(4)PF6] _database_code_CSD 186810 _audit_creation_method SHELXL-97 _chemical_name_systematic '[Silver(I)(tris(2-benzylsulfanyl-ethyl)-amin)]PF6' _chemical_name_common [Ag(NS3Ph)]PF6 _chemical_melting_point ? _chemical_formula_moiety [Ag(NS3Ph)]PF6 _chemical_formula_sum 'C27 H33 Ag F6 N P S3' _chemical_formula_weight 720.56 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' 'S' 'S' 0.1246 0.1234 '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0859(12) _cell_length_b 11.6960(6) _cell_length_c 18.1530(13) _cell_angle_alpha 90.00 _cell_angle_beta 110.803(8) _cell_angle_gamma 90.00 _cell_volume 2994.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 570 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _exptl_crystal_description colourless _exptl_crystal_colour block _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.992 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'STOE IPDS' _diffrn_measurement_method '/f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 50-200 _diffrn_standards_interval_count 'every image' _diffrn_standards_interval_time 3.8 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5830 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5830 _reflns_number_gt 3975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1999)' _computing_cell_refinement 'IPDS (Stoe, 1999)' _computing_data_reduction 'X-RED (Stoe, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Zortep (Zsolnai, 1994), Platon (Spek, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5830 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.894 _refine_ls_shift/su_max 0.005 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.248510(19) 0.25901(2) 0.310219(17) 0.04123(9) Uani 1 1 d . . . S1 S 0.14794(7) 0.18444(9) 0.17242(7) 0.0512(2) Uani 1 1 d . . . S2 S 0.42580(7) 0.30318(8) 0.33993(6) 0.0439(2) Uani 1 1 d . . . S3 S 0.16556(6) 0.41681(8) 0.36127(6) 0.0427(2) Uani 1 1 d . . . N N 0.2463(2) 0.4356(2) 0.21806(18) 0.0382(6) Uani 1 1 d . . . C1 C 0.1823(3) 0.4042(3) 0.1380(2) 0.0477(9) Uani 1 1 d . . . H1A H 0.2191 0.3644 0.1102 0.057 Uiso 1 1 calc R . . H1B H 0.1555 0.4747 0.1082 0.057 Uiso 1 1 calc R . . C2 C 0.1017(3) 0.3274(4) 0.1395(2) 0.0492(9) Uani 1 1 d . . . H2A H 0.0526 0.3231 0.0862 0.059 Uiso 1 1 calc R . . H2B H 0.0723 0.3595 0.1758 0.059 Uiso 1 1 calc R . . C3 C 0.0436(3) 0.1154(4) 0.1823(3) 0.0641(12) Uani 1 1 d . . . H3A H -0.0131 0.1375 0.1367 0.077 Uiso 1 1 calc R . . H3B H 0.0510 0.0315 0.1802 0.077 Uiso 1 1 calc R . . C4 C 0.3445(3) 0.4544(3) 0.2212(3) 0.0457(9) Uani 1 1 d . . . H4A H 0.3758 0.5111 0.2628 0.055 Uiso 1 1 calc R . . H4B H 0.3429 0.4863 0.1702 0.055 Uiso 1 1 calc R . . C5 C 0.4022(3) 0.3442(3) 0.2381(2) 0.0428(8) Uani 1 1 d . . . H5A H 0.4627 0.3561 0.2293 0.051 Uiso 1 1 calc R . . H5B H 0.3665 0.2828 0.2022 0.051 Uiso 1 1 calc R . . C6 C 0.4853(3) 0.1654(3) 0.3459(3) 0.0513(10) Uani 1 1 d . . . H6A H 0.5353 0.1733 0.3227 0.062 Uiso 1 1 calc R . . H6B H 0.5166 0.1443 0.4020 0.062 Uiso 1 1 calc R . . C7 C 0.2095(3) 0.5338(3) 0.2490(2) 0.0435(8) Uani 1 1 d . . . H7A H 0.1396 0.5361 0.2235 0.052 Uiso 1 1 calc R . . H7B H 0.2352 0.6052 0.2352 0.052 Uiso 1 1 calc R . . C8 C 0.2355(3) 0.5287(3) 0.3384(2) 0.0456(9) Uani 1 1 d . . . H8A H 0.2221 0.6032 0.3581 0.055 Uiso 1 1 calc R . . H8B H 0.3039 0.5120 0.3642 0.055 Uiso 1 1 calc R . . C9 C 0.2152(3) 0.4122(4) 0.4690(2) 0.0538(10) Uani 1 1 d . . . H9A H 0.2213 0.4914 0.4895 0.065 Uiso 1 1 calc R . . H9B H 0.1704 0.3712 0.4884 0.065 Uiso 1 1 calc R . . C11 C 0.0273(3) 0.1449(3) 0.2561(2) 0.0462(9) Uani 1 1 d . . . C12 C -0.0326(3) 0.2356(3) 0.2586(3) 0.0507(10) Uani 1 1 d . . . H12 H -0.0646 0.2780 0.2121 0.061 Uiso 1 1 calc R . . C13 C -0.0454(3) 0.2637(4) 0.3283(3) 0.0608(11) Uani 1 1 d . . . H13 H -0.0854 0.3259 0.3292 0.073 Uiso 1 1 calc R . . C14 C -0.0010(4) 0.2030(5) 0.3956(3) 0.0690(13) Uani 1 1 d . . . H14 H -0.0107 0.2227 0.4430 0.083 Uiso 1 1 calc R . . C15 C 0.0570(3) 0.1145(5) 0.3949(3) 0.0698(14) Uani 1 1 d . . . H15 H 0.0875 0.0722 0.4418 0.084 Uiso 1 1 calc R . . C16 C 0.0723(3) 0.0852(4) 0.3259(3) 0.0608(12) Uani 1 1 d . . . H16 H 0.1138 0.0239 0.3264 0.073 Uiso 1 1 calc R . . C21 C 0.4188(3) 0.0705(3) 0.3040(2) 0.0433(8) Uani 1 1 d . . . C22 C 0.4079(3) 0.0400(3) 0.2271(2) 0.0482(9) Uani 1 1 d . . . H22 H 0.4427 0.0795 0.2005 0.058 Uiso 1 1 calc R . . C23 C 0.3466(3) -0.0477(3) 0.1890(3) 0.0518(10) Uani 1 1 d . . . H23 H 0.3398 -0.0678 0.1365 0.062 Uiso 1 1 calc R . . C24 C 0.2958(3) -0.1054(4) 0.2268(3) 0.0579(11) Uani 1 1 d . . . H24 H 0.2545 -0.1658 0.2007 0.070 Uiso 1 1 calc R . . C25 C 0.3047(3) -0.0755(4) 0.3031(3) 0.0601(11) Uani 1 1 d . . . H25 H 0.2692 -0.1147 0.3292 0.072 Uiso 1 1 calc R . . C26 C 0.3659(3) 0.0122(3) 0.3408(3) 0.0530(10) Uani 1 1 d . . . H26 H 0.3717 0.0329 0.3930 0.064 Uiso 1 1 calc R . . C31 C 0.3108(3) 0.3546(3) 0.5016(2) 0.0443(9) Uani 1 1 d . . . C32 C 0.3172(3) 0.2361(3) 0.5064(2) 0.0486(9) Uani 1 1 d . . . H32 H 0.2608 0.1917 0.4891 0.058 Uiso 1 1 calc R . . C33 C 0.4041(4) 0.1819(4) 0.5360(3) 0.0615(11) Uani 1 1 d . . . H33 H 0.4071 0.1009 0.5401 0.074 Uiso 1 1 calc R . . C34 C 0.4864(3) 0.2455(5) 0.5594(3) 0.0687(13) Uani 1 1 d . . . H34 H 0.5463 0.2084 0.5786 0.082 Uiso 1 1 calc R . . C35 C 0.4813(3) 0.3641(5) 0.5548(3) 0.0642(12) Uani 1 1 d . . . H35 H 0.5378 0.4083 0.5709 0.077 Uiso 1 1 calc R . . C36 C 0.3933(3) 0.4184(4) 0.5265(2) 0.0541(10) Uani 1 1 d . . . H36 H 0.3901 0.4995 0.5244 0.065 Uiso 1 1 calc R . . P P 0.22698(7) -0.30438(8) 0.00549(6) 0.0429(2) Uani 1 1 d . . . F1 F 0.2635(2) -0.3155(3) 0.09821(16) 0.0862(9) Uani 1 1 d . . . F2 F 0.1897(2) -0.2939(3) -0.08717(16) 0.0925(10) Uani 1 1 d . . . F3 F 0.2835(2) -0.4169(2) 0.00187(19) 0.0869(9) Uani 1 1 d . . . F4 F 0.1697(2) -0.1918(2) 0.0091(2) 0.0858(9) Uani 1 1 d . . . F5 F 0.1364(2) -0.3782(2) -0.00035(19) 0.0802(8) Uani 1 1 d . . . F6 F 0.3161(2) -0.2279(3) 0.0121(2) 0.0894(9) 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 Ag 0.04545(15) 0.03567(14) 0.04209(15) 0.00271(13) 0.01496(11) 0.00220(13) S1 0.0543(6) 0.0457(5) 0.0549(6) -0.0131(5) 0.0211(5) -0.0087(4) S2 0.0423(5) 0.0413(5) 0.0429(5) -0.0072(4) 0.0088(4) 0.0054(4) S3 0.0395(5) 0.0456(5) 0.0424(5) -0.0034(4) 0.0137(4) 0.0007(4) N 0.0389(16) 0.0356(15) 0.0396(16) 0.0005(13) 0.0131(13) 0.0018(12) C1 0.050(2) 0.055(2) 0.037(2) 0.0058(17) 0.0137(17) 0.0014(18) C2 0.045(2) 0.061(2) 0.035(2) -0.0012(18) 0.0067(17) -0.0046(19) C3 0.068(3) 0.053(2) 0.072(3) -0.015(2) 0.025(2) -0.019(2) C4 0.044(2) 0.0401(19) 0.056(2) 0.0010(17) 0.0215(18) -0.0025(16) C5 0.0399(19) 0.0417(19) 0.050(2) -0.0039(16) 0.0191(17) -0.0003(15) C6 0.045(2) 0.051(2) 0.048(2) -0.0058(18) 0.0039(18) 0.0098(18) C7 0.046(2) 0.0351(18) 0.048(2) 0.0071(16) 0.0151(18) 0.0087(16) C8 0.050(2) 0.0303(17) 0.055(2) -0.0084(16) 0.0176(19) 0.0011(16) C9 0.060(2) 0.060(2) 0.048(2) -0.0074(19) 0.026(2) 0.003(2) C11 0.039(2) 0.0395(19) 0.054(2) 0.0022(17) 0.0092(18) -0.0096(16) C12 0.0366(18) 0.043(2) 0.064(3) 0.0139(19) 0.0065(17) -0.0027(17) C13 0.051(2) 0.051(2) 0.087(3) -0.004(2) 0.033(2) -0.010(2) C14 0.071(3) 0.076(3) 0.065(3) -0.003(3) 0.029(3) -0.023(3) C15 0.065(3) 0.075(3) 0.060(3) 0.023(3) 0.010(2) -0.017(3) C16 0.046(2) 0.042(2) 0.084(4) 0.014(2) 0.010(2) -0.0021(18) C21 0.0411(19) 0.0400(19) 0.042(2) -0.0006(16) 0.0068(16) 0.0114(16) C22 0.049(2) 0.048(2) 0.049(2) -0.0043(18) 0.0191(19) 0.0066(17) C23 0.050(2) 0.048(2) 0.053(3) -0.0122(19) 0.0127(19) 0.0035(18) C24 0.052(2) 0.046(2) 0.069(3) -0.005(2) 0.014(2) 0.0004(19) C25 0.065(3) 0.043(2) 0.078(3) 0.011(2) 0.033(2) 0.006(2) C26 0.065(3) 0.047(2) 0.045(2) 0.0057(18) 0.018(2) 0.013(2) C31 0.052(2) 0.051(2) 0.033(2) -0.0051(16) 0.0180(17) -0.0026(17) C32 0.059(2) 0.050(2) 0.0358(19) -0.0028(17) 0.0154(17) -0.0113(19) C33 0.086(3) 0.054(2) 0.044(2) 0.009(2) 0.023(2) 0.009(2) C34 0.060(3) 0.095(4) 0.048(2) 0.017(3) 0.015(2) 0.019(3) C35 0.051(3) 0.088(4) 0.046(3) 0.003(2) 0.007(2) -0.014(2) C36 0.066(3) 0.054(2) 0.039(2) -0.0049(18) 0.015(2) -0.017(2) P 0.0483(5) 0.0384(5) 0.0374(5) 0.0050(4) 0.0096(4) 0.0020(4) F1 0.125(2) 0.084(2) 0.0391(15) 0.0046(14) 0.0168(15) -0.0027(18) F2 0.120(2) 0.103(2) 0.0394(15) 0.0124(15) 0.0090(15) 0.010(2) F3 0.103(2) 0.0649(17) 0.093(2) 0.0041(15) 0.0353(18) 0.0358(16) F4 0.091(2) 0.0451(14) 0.121(3) 0.0072(15) 0.0378(19) 0.0168(14) F5 0.0721(17) 0.0614(16) 0.102(2) 0.0032(15) 0.0252(16) -0.0157(13) F6 0.0678(18) 0.087(2) 0.110(2) 0.0218(18) 0.0276(17) -0.0165(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag S1 2.5737(11) . ? Ag S3 2.5797(10) . ? Ag S2 2.5858(10) . ? S1 C2 1.829(4) . ? S1 C3 1.833(4) . ? S2 C5 1.819(4) . ? S2 C6 1.829(4) . ? S3 C8 1.819(4) . ? S3 C9 1.831(4) . ? N C7 1.471(4) . ? N C1 1.478(5) . ? N C4 1.478(4) . ? C1 C2 1.519(5) . ? C3 C11 1.488(6) . ? C4 C5 1.525(5) . ? C6 C21 1.508(5) . ? C7 C8 1.529(6) . ? C9 C31 1.510(6) . ? C11 C16 1.393(6) . ? C11 C12 1.404(5) . ? C12 C13 1.384(6) . ? C13 C14 1.365(7) . ? C14 C15 1.359(7) . ? C15 C16 1.395(7) . ? C21 C22 1.391(5) . ? C21 C26 1.389(6) . ? C22 C23 1.390(6) . ? C23 C24 1.374(6) . ? C24 C25 1.389(7) . ? C25 C26 1.387(6) . ? C31 C36 1.382(5) . ? C31 C32 1.389(6) . ? C32 C33 1.382(6) . ? C33 C34 1.378(7) . ? C34 C35 1.391(7) . ? C35 C36 1.394(6) . ? P F2 1.578(3) . ? P F1 1.579(3) . ? P F3 1.582(3) . ? P F6 1.583(3) . ? P F5 1.588(3) . ? P F4 1.589(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 S1 Ag S3 113.45(3) . . ? S1 Ag S2 118.65(3) . . ? S3 Ag S2 112.32(3) . . ? C2 S1 C3 101.2(2) . . ? C2 S1 Ag 91.86(13) . . ? C3 S1 Ag 106.54(16) . . ? C5 S2 C6 101.93(18) . . ? C5 S2 Ag 91.51(12) . . ? C6 S2 Ag 106.61(14) . . ? C8 S3 C9 102.41(19) . . ? C8 S3 Ag 92.18(12) . . ? C9 S3 Ag 107.25(13) . . ? C7 N C1 111.5(3) . . ? C7 N C4 112.2(3) . . ? C1 N C4 111.8(3) . . ? N C1 C2 112.1(3) . . ? C1 C2 S1 109.4(3) . . ? C11 C3 S1 114.1(3) . . ? N C4 C5 112.0(3) . . ? C4 C5 S2 108.6(3) . . ? C21 C6 S2 113.2(3) . . ? N C7 C8 112.7(3) . . ? C7 C8 S3 108.6(3) . . ? C31 C9 S3 113.7(3) . . ? C16 C11 C12 117.5(4) . . ? C16 C11 C3 121.3(4) . . ? C12 C11 C3 121.3(4) . . ? C13 C12 C11 120.6(4) . . ? C14 C13 C12 120.8(4) . . ? C15 C14 C13 120.0(5) . . ? C14 C15 C16 120.5(4) . . ? C11 C16 C15 120.7(4) . . ? C22 C21 C26 118.3(4) . . ? C22 C21 C6 121.0(4) . . ? C26 C21 C6 120.7(4) . . ? C21 C22 C23 120.6(4) . . ? C24 C23 C22 120.3(4) . . ? C23 C24 C25 120.1(4) . . ? C26 C25 C24 119.4(4) . . ? C25 C26 C21 121.4(4) . . ? C36 C31 C32 118.9(4) . . ? C36 C31 C9 120.8(4) . . ? C32 C31 C9 120.3(4) . . ? C33 C32 C31 121.2(4) . . ? C34 C33 C32 119.8(4) . . ? C33 C34 C35 119.7(4) . . ? C34 C35 C36 120.1(4) . . ? C31 C36 C35 120.3(4) . . ? F2 P F1 179.5(2) . . ? F2 P F3 90.77(18) . . ? F1 P F3 89.22(17) . . ? F2 P F6 90.50(19) . . ? F1 P F6 89.99(18) . . ? F3 P F6 91.02(18) . . ? F2 P F5 89.93(18) . . ? F1 P F5 89.58(18) . . ? F3 P F5 90.45(17) . . ? F6 P F5 178.46(18) . . ? F2 P F4 89.25(18) . . ? F1 P F4 90.76(18) . . ? F3 P F4 179.68(18) . . ? F6 P F4 89.30(17) . . ? F5 P F4 89.23(16) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.060 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.086 #===END data_jb291199_[Cu(5)PF6] _database_code_CSD 186811 _audit_creation_method SHELXL-97 _chemical_name_systematic '[Copper(I)(tris(2-vinylsulfanyl-ethyl)-amin)]PF6' _chemical_name_common [Cu(NS3vinyl)]PF6 _chemical_melting_point ? _chemical_formula_moiety [Cu(NS3vinyl)]PF6 _chemical_formula_sum 'C12 H21 Cu F6 N P S3' _chemical_formula_weight 483.99 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' 'S' 'S' 0.1246 0.1234 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3903(10) _cell_length_b 15.3514(8) _cell_length_c 10.2517(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.405(9) _cell_angle_gamma 90.00 _cell_volume 1949.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 358 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.573 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6055 _exptl_absorpt_correction_T_max 0.7210 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Stoe IPDS' _diffrn_measurement_method '/f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 50-200 _diffrn_standards_interval_count 'every image' _diffrn_standards_interval_time 5.7 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3770 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.91 _reflns_number_total 3770 _reflns_number_gt 2734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1999)' _computing_cell_refinement 'IPDS (Stoe, 1999)' _computing_data_reduction 'X-RED (Stoe, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Zortep (Zsolnai, 1994), Platon (Spek, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0749P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3770 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.113 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.23264(3) 0.72896(3) 0.20042(4) 0.03386(16) Uani 1 1 d . . . N N 0.2580(2) 0.8092(2) 0.3770(3) 0.0346(7) Uani 1 1 d . . . S1 S 0.07440(8) 0.79909(7) 0.15606(12) 0.0491(3) Uani 1 1 d . . . S2 S 0.23145(8) 0.60728(6) 0.32709(10) 0.0429(3) Uani 1 1 d . . . S3 S 0.39238(8) 0.77655(8) 0.12232(10) 0.0458(3) Uani 1 1 d . . . C1 C 0.1734(3) 0.8776(3) 0.3741(4) 0.0449(9) Uani 1 1 d . . . H1A H 0.1977 0.9269 0.3198 0.054 Uiso 1 1 calc R . . H1B H 0.1635 0.8997 0.4637 0.054 Uiso 1 1 calc R . . C2 C 0.0652(3) 0.8441(3) 0.3194(5) 0.0520(11) Uani 1 1 d . . . H2A H 0.0125 0.8927 0.3176 0.062 Uiso 1 1 calc R . . H2B H 0.0377 0.7987 0.3785 0.062 Uiso 1 1 calc R . . C3 C 0.1056(5) 0.8941(3) 0.0666(6) 0.0701(16) Uani 1 1 d . . . H3 H 0.0744 0.9477 0.0927 0.084 Uiso 1 1 calc R . . C4 C 0.1683(6) 0.8947(4) -0.0321(6) 0.087(2) Uani 1 1 d . . . H4A H 0.2007 0.8422 -0.0604 0.104 Uiso 1 1 calc R . . H4B H 0.1822 0.9478 -0.0764 0.104 Uiso 1 1 calc R . . C5 C 0.2492(3) 0.7519(3) 0.4909(4) 0.0448(9) Uani 1 1 d . . . H5A H 0.1722 0.7462 0.5132 0.054 Uiso 1 1 calc R . . H5B H 0.2878 0.7789 0.5664 0.054 Uiso 1 1 calc R . . C6 C 0.2958(3) 0.6617(3) 0.4673(4) 0.0457(10) Uani 1 1 d . . . H6A H 0.2864 0.6255 0.5461 0.055 Uiso 1 1 calc R . . H6B H 0.3742 0.6669 0.4525 0.055 Uiso 1 1 calc R . . C7 C 0.0983(4) 0.5950(3) 0.3855(5) 0.0559(12) Uani 1 1 d . . . H7 H 0.0894 0.5891 0.4768 0.067 Uiso 1 1 calc R . . C8 C 0.0129(4) 0.5937(3) 0.3102(7) 0.0734(16) Uani 1 1 d . . . H8A H 0.0195 0.5995 0.2185 0.088 Uiso 1 1 calc R . . H8B H -0.0563 0.5870 0.3467 0.088 Uiso 1 1 calc R . . C9 C 0.3676(3) 0.8480(3) 0.3713(4) 0.0443(10) Uani 1 1 d . . . H9A H 0.4210 0.8066 0.4092 0.053 Uiso 1 1 calc R . . H9B H 0.3701 0.9018 0.4247 0.053 Uiso 1 1 calc R . . C10 C 0.3985(3) 0.8699(3) 0.2320(5) 0.0502(11) Uani 1 1 d . . . H10A H 0.4727 0.8938 0.2333 0.060 Uiso 1 1 calc R . . H10B H 0.3493 0.9158 0.1976 0.060 Uiso 1 1 calc R . . C11 C 0.4964(3) 0.7100(3) 0.1912(4) 0.0488(10) Uani 1 1 d . . . H11 H 0.5527 0.7371 0.2409 0.059 Uiso 1 1 calc R . . C12 C 0.4988(4) 0.6253(4) 0.1764(5) 0.0586(12) Uani 1 1 d . . . H12A H 0.4433 0.5968 0.1270 0.070 Uiso 1 1 calc R . . H12B H 0.5561 0.5923 0.2150 0.070 Uiso 1 1 calc R . . P P 0.27445(9) 1.08013(8) -0.34890(10) 0.0466(3) Uani 1 1 d . . . F11 F 0.2897(10) 1.1753(7) -0.3553(10) 0.0770(8) Uani 0.351(7) 1 d P A 1 F12 F 0.2281(5) 1.1795(4) -0.3254(5) 0.0770(8) Uani 0.649(7) 1 d P A 2 F21 F 0.3283(11) 0.9972(8) -0.3773(11) 0.0770(8) Uani 0.326(8) 1 d P A 1 F22 F 0.2794(5) 0.9722(4) -0.3479(5) 0.0770(8) Uani 0.674(8) 1 d P A 2 F3 F 0.2072(3) 1.0759(2) -0.4820(3) 0.0903(11) Uani 1 1 d . A . F4 F 0.3413(2) 1.0833(2) -0.2132(3) 0.0696(9) Uani 1 1 d . A . F5 F 0.1695(2) 1.0594(3) -0.2661(3) 0.0856(10) Uani 1 1 d . A . F61 F 0.3673(6) 1.1300(5) -0.4247(6) 0.0770(8) Uani 0.496(6) 1 d P A 1 F62 F 0.3862(6) 1.0705(5) -0.4223(6) 0.0770(8) Uani 0.504(6) 1 d P A 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 Cu 0.0321(2) 0.0356(3) 0.0337(2) 0.00029(19) -0.00252(17) 0.00008(19) N 0.0273(15) 0.0389(16) 0.0374(16) -0.0050(13) 0.0000(12) 0.0000(13) S1 0.0381(5) 0.0447(6) 0.0634(7) -0.0012(5) -0.0198(5) 0.0022(4) S2 0.0455(5) 0.0329(5) 0.0505(6) 0.0044(4) 0.0037(4) 0.0019(4) S3 0.0390(5) 0.0591(6) 0.0396(5) 0.0099(5) 0.0082(4) -0.0003(5) C1 0.035(2) 0.041(2) 0.058(3) -0.0123(19) 0.0014(18) 0.0044(17) C2 0.034(2) 0.052(3) 0.070(3) -0.011(2) -0.0013(19) 0.0083(18) C3 0.090(4) 0.053(3) 0.066(4) 0.009(3) -0.039(3) 0.005(3) C4 0.129(6) 0.061(3) 0.068(4) 0.019(3) -0.044(4) -0.014(3) C5 0.042(2) 0.060(3) 0.033(2) -0.0055(18) 0.0018(16) 0.0018(18) C6 0.045(2) 0.056(3) 0.037(2) 0.0113(19) 0.0011(17) 0.0025(19) C7 0.055(3) 0.046(3) 0.067(3) -0.001(2) 0.011(2) -0.015(2) C8 0.057(3) 0.054(3) 0.109(5) -0.008(3) -0.002(3) -0.014(2) C9 0.0309(19) 0.047(2) 0.055(2) -0.0130(19) -0.0056(17) -0.0040(16) C10 0.035(2) 0.044(2) 0.071(3) 0.010(2) 0.000(2) -0.0091(17) C11 0.032(2) 0.067(3) 0.048(2) -0.002(2) 0.0085(17) 0.0039(19) C12 0.046(2) 0.076(3) 0.054(3) -0.003(2) -0.001(2) 0.015(2) P 0.0426(6) 0.0599(7) 0.0370(6) -0.0036(5) -0.0075(4) -0.0055(5) F11 0.083(2) 0.0786(18) 0.0698(16) -0.0018(14) 0.0076(14) 0.0014(16) F12 0.083(2) 0.0786(18) 0.0698(16) -0.0018(14) 0.0076(14) 0.0014(16) F21 0.083(2) 0.0786(18) 0.0698(16) -0.0018(14) 0.0076(14) 0.0014(16) F22 0.083(2) 0.0786(18) 0.0698(16) -0.0018(14) 0.0076(14) 0.0014(16) F3 0.119(3) 0.088(2) 0.0612(19) 0.0057(16) -0.0503(19) -0.006(2) F4 0.0377(13) 0.129(3) 0.0418(14) -0.0172(15) -0.0044(11) -0.0057(14) F5 0.0442(15) 0.124(3) 0.088(2) 0.009(2) -0.0060(15) -0.0115(17) F61 0.083(2) 0.0786(18) 0.0698(16) -0.0018(14) 0.0076(14) 0.0014(16) F62 0.083(2) 0.0786(18) 0.0698(16) -0.0018(14) 0.0076(14) 0.0014(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 Cu N 2.206(3) . ? Cu S1 2.2730(11) . ? Cu S3 2.2738(11) . ? Cu S2 2.2752(11) . ? N C5 1.468(5) . ? N C9 1.485(5) . ? N C1 1.485(5) . ? S1 C3 1.771(6) . ? S1 C2 1.818(5) . ? S2 C7 1.778(5) . ? S2 C6 1.828(4) . ? S3 C11 1.777(4) . ? S3 C10 1.822(5) . ? C1 C2 1.529(6) . ? C3 C4 1.290(9) . ? C5 C6 1.523(6) . ? C7 C8 1.294(7) . ? C9 C10 1.525(6) . ? C11 C12 1.310(7) . ? P F21 1.470(11) . ? P F11 1.475(10) . ? P F3 1.583(3) . ? P F62 1.599(7) . ? P F5 1.602(3) . ? P F4 1.602(3) . ? P F61 1.600(7) . ? P F12 1.649(6) . ? P F22 1.659(6) . ? F11 F61 1.396(13) . ? 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 N Cu S1 90.27(8) . . ? N Cu S3 90.10(8) . . ? S1 Cu S3 122.10(5) . . ? N Cu S2 89.58(9) . . ? S1 Cu S2 119.04(4) . . ? S3 Cu S2 118.86(4) . . ? C5 N C9 111.0(3) . . ? C5 N C1 112.0(3) . . ? C9 N C1 111.2(3) . . ? C5 N Cu 107.9(2) . . ? C9 N Cu 107.7(2) . . ? C1 N Cu 107.0(2) . . ? C3 S1 C2 100.6(3) . . ? C3 S1 Cu 107.2(2) . . ? C2 S1 Cu 93.96(14) . . ? C7 S2 C6 100.0(2) . . ? C7 S2 Cu 107.34(17) . . ? C6 S2 Cu 93.72(13) . . ? C11 S3 C10 100.9(2) . . ? C11 S3 Cu 107.73(15) . . ? C10 S3 Cu 93.37(13) . . ? N C1 C2 112.4(3) . . ? C1 C2 S1 113.0(3) . . ? C4 C3 S1 123.7(5) . . ? N C5 C6 112.5(3) . . ? C5 C6 S2 112.4(3) . . ? C8 C7 S2 123.5(5) . . ? N C9 C10 112.1(3) . . ? C9 C10 S3 113.4(3) . . ? C12 C11 S3 122.9(4) . . ? F21 P F11 142.2(8) . . ? F21 P F3 91.4(4) . . ? F11 P F3 93.9(4) . . ? F21 P F62 54.9(6) . . ? F11 P F62 87.5(5) . . ? F3 P F62 92.0(3) . . ? F21 P F5 108.1(6) . . ? F11 P F5 109.1(5) . . ? F3 P F5 91.8(2) . . ? F62 P F5 162.7(3) . . ? F21 P F4 88.3(4) . . ? F11 P F4 86.8(4) . . ? F3 P F4 179.1(2) . . ? F62 P F4 88.6(3) . . ? F5 P F4 87.44(16) . . ? F21 P F61 89.0(6) . . ? F11 P F61 53.8(5) . . ? F3 P F61 88.3(3) . . ? F62 P F61 34.3(3) . . ? F5 P F61 162.8(3) . . ? F4 P F61 92.5(3) . . ? F21 P F12 172.4(6) . . ? F11 P F12 30.3(4) . . ? F3 P F12 89.2(2) . . ? F62 P F12 117.6(4) . . ? F5 P F12 79.4(3) . . ? F4 P F12 91.1(2) . . ? F61 P F12 83.4(4) . . ? F21 P F22 28.2(5) . . ? F11 P F22 170.2(6) . . ? F3 P F22 89.0(2) . . ? F62 P F22 83.0(4) . . ? F5 P F22 80.1(3) . . ? F4 P F22 90.4(2) . . ? F61 P F22 117.0(4) . . ? F12 P F22 159.4(3) . . ? F61 F11 P 67.7(6) . . ? F11 F61 P 58.5(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.91 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.205 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.080 #===END data_jb240700_[Ag(11)Tosylat] _database_code_CSD 186812 _audit_creation_method SHELXL-97 _chemical_name_systematic 'Silver(I)(in-4,10,15-trithia-1-aza-bicyclo[5.5.5]-heptadecane)toluenesulfonate' _chemical_name_common jb240700 _chemical_melting_point ? _chemical_formula_moiety jb240700 _chemical_formula_sum 'C22 H35 Ag N2 O3 S4' _chemical_formula_weight 611.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.7597(5) _cell_length_b 15.1614(11) _cell_length_c 19.4053(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2577.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8081 _exptl_absorpt_correction_T_max 0.9139 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Stoe IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 50-200 _diffrn_standards_interval_count 'every image' _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18238 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.94 _reflns_number_total 4991 _reflns_number_gt 4775 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1999)' _computing_cell_refinement 'IPDS (Stoe, 1999)' _computing_data_reduction 'X-RED (Stoe, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Zortep (Zsolnai, 1994), Platon (Spek, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.022(15) _refine_ls_number_reflns 4991 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0531 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.138 _refine_ls_shift/su_mean 0.008 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.77726(2) 0.023001(11) 0.163798(9) 0.02559(6) Uani 1 1 d . . . S1 S 1.01570(6) 0.11817(3) 0.16425(3) 0.02114(11) Uani 1 1 d . . . S2 S 0.55757(7) 0.14345(4) 0.18247(3) 0.02524(13) Uani 1 1 d . . . S3 S 0.77325(8) -0.11644(3) 0.23782(3) 0.02395(12) Uani 1 1 d . . . C1 C 0.9892(3) 0.17907(17) 0.24441(13) 0.0269(5) Uani 1 1 d . . . H1A H 1.014(3) 0.2379(17) 0.2359(12) 0.011(6) Uiso 1 1 d . . . H1B H 0.888(5) 0.174(2) 0.2596(17) 0.040(9) Uiso 1 1 d . . . C2 C 1.0919(3) 0.13911(17) 0.30020(12) 0.0279(5) Uani 1 1 d . . . H2A H 1.082(4) 0.075(2) 0.3034(14) 0.029(7) Uiso 1 1 d . . . H2B H 1.054(3) 0.1590(18) 0.3458(15) 0.028(7) Uiso 1 1 d . . . C3 C 0.9965(3) 0.20129(17) 0.09659(14) 0.0281(5) Uani 1 1 d . . . H3A H 1.014(4) 0.169(2) 0.0595(19) 0.039(9) Uiso 1 1 d . . . H3B H 0.890(6) 0.219(3) 0.094(2) 0.063(12) Uiso 1 1 d . . . C4 C 1.1020(3) 0.28108(16) 0.10385(13) 0.0258(5) Uani 1 1 d . . . H4A H 1.055(3) 0.3209(18) 0.1389(14) 0.021(7) Uiso 1 1 d . . . H4B H 1.097(4) 0.3135(18) 0.0602(16) 0.028(7) Uiso 1 1 d . . . C5 C 0.5111(3) 0.17297(17) 0.09312(13) 0.0297(6) Uani 1 1 d . . . H5A H 0.572(4) 0.221(2) 0.0859(16) 0.028(8) Uiso 1 1 d . . . H5B H 0.537(3) 0.1272(18) 0.0655(13) 0.018(6) Uiso 1 1 d . . . C6 C 0.3452(3) 0.19616(16) 0.07774(12) 0.0256(5) Uani 1 1 d . . . H6A H 0.281(4) 0.140(2) 0.0757(15) 0.033(7) Uiso 1 1 d . . . H6B H 0.334(3) 0.2167(19) 0.0301(15) 0.027(7) Uiso 1 1 d . . . C7 C 0.4071(3) 0.06836(15) 0.21091(13) 0.0239(5) Uani 1 1 d . . . H7A H 0.329(3) 0.0754(16) 0.1813(13) 0.014(6) Uiso 1 1 d . . . H7B H 0.441(3) 0.0106(19) 0.2083(14) 0.024(7) Uiso 1 1 d . . . C8 C 0.3584(3) 0.08874(16) 0.28481(13) 0.0278(5) Uani 1 1 d . . . H8A H 0.453(5) 0.102(2) 0.3106(18) 0.050(10) Uiso 1 1 d . . . H8B H 0.314(4) 0.034(2) 0.3013(15) 0.032(8) Uiso 1 1 d . . . C9 C 0.6231(3) -0.18646(16) 0.20096(13) 0.0255(5) Uani 1 1 d . . . H9A H 0.562(3) -0.1512(18) 0.1683(15) 0.026(7) Uiso 1 1 d . . . H9B H 0.558(3) -0.2075(17) 0.2396(13) 0.017(6) Uiso 1 1 d . . . C10 C 0.6945(3) -0.26490(15) 0.16305(14) 0.0267(5) Uani 1 1 d . . . H10A H 0.780(4) -0.2420(18) 0.1353(15) 0.025(7) Uiso 1 1 d . . . H10B H 0.624(4) -0.284(2) 0.1320(16) 0.033(8) Uiso 1 1 d . . . C11 C 0.7019(3) -0.08035(15) 0.32180(13) 0.0282(5) Uani 1 1 d . . . H11A H 0.789(4) -0.053(2) 0.3404(17) 0.042(8) Uiso 1 1 d . . . H11B H 0.633(3) -0.0403(18) 0.3105(13) 0.019(6) Uiso 1 1 d . . . C12 C 0.6393(3) -0.15246(16) 0.36900(13) 0.0248(5) Uani 1 1 d . . . H12A H 0.534(4) -0.1672(18) 0.3539(14) 0.026(7) Uiso 1 1 d . . . H12B H 0.624(4) -0.126(2) 0.4150(17) 0.036(8) Uiso 1 1 d . . . C13 C 0.2671(3) 0.26195(13) 0.12618(11) 0.0198(4) Uani 1 1 d . . . H13 H 0.262(3) 0.2351(14) 0.1709(12) 0.010(5) Uiso 1 1 d . . . S4 S 0.83648(10) 0.04192(4) 0.51469(3) 0.03885(17) Uani 1 1 d . . . O1 O 0.6840(4) 0.0277(2) 0.5386(2) 0.0995(13) Uani 1 1 d . . . O2 O 0.8877(3) -0.02193(13) 0.46597(9) 0.0468(5) Uani 1 1 d . . . O3 O 0.9441(4) 0.05270(14) 0.57145(11) 0.0753(10) Uani 1 1 d . . . C21 C 0.8337(3) 0.14408(16) 0.46940(12) 0.0263(5) Uani 1 1 d . . . C22 C 0.7323(3) 0.15431(15) 0.41512(12) 0.0276(5) Uani 1 1 d . . . H22 H 0.666(4) 0.108(2) 0.4047(16) 0.035(8) Uiso 1 1 d . . . C23 C 0.7312(3) 0.23168(17) 0.37743(13) 0.0302(5) Uani 1 1 d . . . H23 H 0.671(3) 0.2348(18) 0.3392(17) 0.028(7) Uiso 1 1 d . . . C24 C 0.8309(3) 0.30039(16) 0.39330(14) 0.0305(6) Uani 1 1 d . . . C25 C 0.8279(5) 0.3853(2) 0.3519(2) 0.0499(9) Uani 1 1 d . . . H25A H 0.825(4) 0.378(2) 0.306(2) 0.051(11) Uiso 1 1 d . . . H25B H 0.915(7) 0.431(4) 0.367(3) 0.113(19) Uiso 1 1 d . . . H25C H 0.742(7) 0.415(3) 0.365(2) 0.087(15) Uiso 1 1 d . . . C26 C 0.9326(3) 0.28920(17) 0.44749(15) 0.0326(6) Uani 1 1 d . . . H26 H 1.004(4) 0.332(2) 0.4526(15) 0.028(7) Uiso 1 1 d . . . C27 C 0.9339(3) 0.21110(17) 0.48566(14) 0.0318(6) Uani 1 1 d . . . H27 H 1.000(4) 0.200(2) 0.5180(18) 0.039(9) Uiso 1 1 d . . . N1 N 1.2527(2) 0.16312(12) 0.29244(9) 0.0227(4) Uani 1 1 d . . . N2 N 0.7525(4) 0.3811(2) 0.1128(2) 0.0642(9) Uani 1 1 d . . . C31 C 0.7246(6) 0.5129(3) 0.0306(2) 0.0641(10) Uani 1 1 d . . . H31A H 0.729(5) 0.560(3) 0.052(2) 0.056(11) Uiso 1 1 d . . . H31B H 0.807(5) 0.514(2) -0.001(2) 0.053(10) Uiso 1 1 d . . . H31C H 0.622(9) 0.506(4) 0.011(3) 0.13(2) Uiso 1 1 d . . . C32 C 0.7432(4) 0.4389(2) 0.07613(18) 0.0479(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 Ag 0.02456(9) 0.02210(9) 0.03011(9) 0.00186(7) -0.00085(7) -0.00439(7) S1 0.0198(3) 0.0193(2) 0.0243(2) -0.0004(2) -0.0011(2) -0.00184(19) S2 0.0219(3) 0.0223(2) 0.0315(3) -0.0024(2) 0.0018(2) -0.0001(2) S3 0.0230(3) 0.0200(2) 0.0288(3) 0.0037(2) -0.0020(2) -0.0025(2) C1 0.0217(13) 0.0268(13) 0.0321(13) -0.0056(10) 0.0013(10) 0.0001(10) C2 0.0290(15) 0.0308(13) 0.0240(12) 0.0019(10) 0.0044(10) -0.0084(10) C3 0.0301(16) 0.0265(12) 0.0278(13) 0.0039(10) -0.0094(10) -0.0029(11) C4 0.0282(14) 0.0218(11) 0.0274(12) 0.0055(9) -0.0030(10) -0.0021(10) C5 0.0359(16) 0.0257(12) 0.0276(12) -0.0007(10) 0.0133(11) 0.0027(11) C6 0.0307(13) 0.0243(12) 0.0220(12) 0.0002(9) 0.0004(10) -0.0005(11) C7 0.0243(13) 0.0176(11) 0.0299(12) -0.0015(9) -0.0027(10) 0.0013(9) C8 0.0315(15) 0.0247(12) 0.0270(12) 0.0037(10) -0.0015(11) 0.0072(10) C9 0.0247(14) 0.0242(11) 0.0277(12) 0.0039(10) -0.0044(10) -0.0005(10) C10 0.0290(15) 0.0299(11) 0.0212(10) 0.0029(10) -0.0011(11) 0.0006(9) C11 0.0321(15) 0.0189(10) 0.0336(13) -0.0003(9) -0.0054(10) 0.0040(10) C12 0.0236(14) 0.0222(11) 0.0286(12) 0.0010(10) 0.0021(10) 0.0043(10) C13 0.0204(12) 0.0182(10) 0.0207(10) 0.0015(8) -0.0003(9) -0.0002(9) S4 0.0626(5) 0.0261(3) 0.0278(3) 0.0074(2) 0.0089(3) 0.0126(3) O1 0.085(2) 0.0758(18) 0.138(3) 0.073(2) 0.066(2) 0.0341(17) O2 0.0839(17) 0.0241(8) 0.0325(10) -0.0045(8) -0.0102(10) 0.0104(11) O3 0.161(3) 0.0355(11) 0.0293(10) -0.0043(9) -0.0351(15) 0.0208(15) C21 0.0337(14) 0.0216(11) 0.0237(11) -0.0005(9) 0.0049(10) 0.0071(10) C22 0.0258(14) 0.0262(11) 0.0310(12) 0.0003(10) 0.0042(11) -0.0011(11) C23 0.0253(13) 0.0362(13) 0.0293(12) 0.0062(10) 0.0017(11) 0.0062(11) C24 0.0285(14) 0.0230(12) 0.0399(14) 0.0072(10) 0.0117(11) 0.0067(10) C25 0.045(2) 0.0364(16) 0.068(3) 0.0239(15) 0.0165(16) 0.0075(14) C26 0.0296(15) 0.0222(12) 0.0460(15) -0.0060(10) 0.0028(12) -0.0032(11) C27 0.0373(16) 0.0310(12) 0.0270(12) -0.0073(10) -0.0043(12) 0.0077(11) N1 0.0227(13) 0.0220(9) 0.0235(9) -0.0015(7) 0.0002(8) 0.0021(8) N2 0.043(2) 0.0486(16) 0.100(2) -0.0003(16) 0.0203(17) 0.0040(14) C31 0.072(3) 0.057(2) 0.064(2) -0.0043(18) 0.010(2) 0.005(2) C32 0.041(2) 0.0380(15) 0.0648(19) -0.0174(15) 0.0115(15) -0.0002(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag S1 2.5386(6) . ? Ag S3 2.5563(6) . ? Ag O1 2.571(4) 2_654 ? Ag S2 2.6776(6) . ? S1 C1 1.824(3) . ? S1 C3 1.828(2) . ? S2 C7 1.827(3) . ? S2 C5 1.836(3) . ? S3 C11 1.829(3) . ? S3 C9 1.835(3) . ? C1 C2 1.533(4) . ? C2 N1 1.463(3) . ? C3 C4 1.529(4) . ? C4 C13 1.537(4) 1_655 ? C5 C6 1.525(4) . ? C6 C13 1.532(3) . ? C7 C8 1.528(3) . ? C8 N1 1.467(3) 1_455 ? C9 C10 1.532(3) . ? C10 N1 1.467(3) 4_745 ? C11 C12 1.528(3) . ? C12 C13 1.538(3) 4_645 ? C13 C4 1.537(4) 1_455 ? C13 C12 1.538(3) 4_655 ? S4 O2 1.426(2) . ? S4 O1 1.431(3) . ? S4 O3 1.459(3) . ? S4 C21 1.781(3) . ? O1 Ag 2.571(4) 2_655 ? C21 C27 1.379(4) . ? C21 C22 1.387(4) . ? C22 C23 1.382(3) . ? C23 C24 1.394(4) . ? C24 C26 1.389(4) . ? C24 C25 1.517(4) . ? C26 C27 1.397(4) . ? N1 C10 1.467(3) 4_755 ? N1 C8 1.467(3) 1_655 ? N2 C32 1.133(5) . ? C31 C32 1.438(6) . ? 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 S1 Ag S3 118.65(2) . . ? S1 Ag O1 93.70(9) . 2_654 ? S3 Ag O1 106.59(9) . 2_654 ? S1 Ag S2 101.724(19) . . ? S3 Ag S2 118.57(2) . . ? O1 Ag S2 115.26(7) 2_654 . ? C1 S1 C3 104.59(13) . . ? C1 S1 Ag 100.71(9) . . ? C3 S1 Ag 108.28(9) . . ? C7 S2 C5 106.08(12) . . ? C7 S2 Ag 97.72(8) . . ? C5 S2 Ag 101.41(9) . . ? C11 S3 C9 106.00(12) . . ? C11 S3 Ag 104.95(8) . . ? C9 S3 Ag 105.62(8) . . ? C2 C1 S1 109.12(17) . . ? N1 C2 C1 113.2(2) . . ? C4 C3 S1 115.07(18) . . ? C3 C4 C13 116.4(2) . 1_655 ? C6 C5 S2 116.90(18) . . ? C5 C6 C13 117.1(2) . . ? C8 C7 S2 111.03(18) . . ? N1 C8 C7 115.2(2) 1_455 . ? C10 C9 S3 110.11(18) . . ? N1 C10 C9 115.1(2) 4_745 . ? C12 C11 S3 116.27(16) . . ? C11 C12 C13 116.7(2) . 4_645 ? C6 C13 C4 111.7(2) . 1_455 ? C6 C13 C12 110.4(2) . 4_655 ? C4 C13 C12 111.07(18) 1_455 4_655 ? O2 S4 O1 114.0(2) . . ? O2 S4 O3 111.91(15) . . ? O1 S4 O3 112.1(2) . . ? O2 S4 C21 105.52(11) . . ? O1 S4 C21 106.17(14) . . ? O3 S4 C21 106.49(14) . . ? S4 O1 Ag 103.2(2) . 2_655 ? C27 C21 C22 119.9(2) . . ? C27 C21 S4 121.3(2) . . ? C22 C21 S4 118.7(2) . . ? C23 C22 C21 120.1(3) . . ? C22 C23 C24 120.9(3) . . ? C26 C24 C23 118.6(2) . . ? C26 C24 C25 121.0(3) . . ? C23 C24 C25 120.4(3) . . ? C24 C26 C27 120.7(3) . . ? C21 C27 C26 119.9(3) . . ? C2 N1 C10 115.34(19) . 4_755 ? C2 N1 C8 115.3(2) . 1_655 ? C10 N1 C8 115.6(2) 4_755 1_655 ? N2 C32 C31 177.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S3 Ag S1 C1 -79.88(9) . . . . ? O1 Ag S1 C1 168.93(11) 2_654 . . . ? S2 Ag S1 C1 52.18(9) . . . . ? S3 Ag S1 C3 170.70(10) . . . . ? O1 Ag S1 C3 59.51(13) 2_654 . . . ? S2 Ag S1 C3 -57.25(10) . . . . ? S1 Ag S2 C7 -161.36(8) . . . . ? S3 Ag S2 C7 -29.26(8) . . . . ? O1 Ag S2 C7 98.80(13) 2_654 . . . ? S1 Ag S2 C5 90.42(10) . . . . ? S3 Ag S2 C5 -137.47(10) . . . . ? O1 Ag S2 C5 -9.41(14) 2_654 . . . ? S1 Ag S3 C11 88.94(10) . . . . ? O1 Ag S3 C11 -167.21(12) 2_654 . . . ? S2 Ag S3 C11 -35.20(10) . . . . ? S1 Ag S3 C9 -159.30(9) . . . . ? O1 Ag S3 C9 -55.44(12) 2_654 . . . ? S2 Ag S3 C9 76.57(9) . . . . ? C3 S1 C1 C2 -145.28(18) . . . . ? Ag S1 C1 C2 102.44(17) . . . . ? S1 C1 C2 N1 75.8(2) . . . . ? C1 S1 C3 C4 54.5(2) . . . . ? Ag S1 C3 C4 161.25(18) . . . . ? S1 C3 C4 C13 41.5(3) . . . 1_655 ? C7 S2 C5 C6 44.6(2) . . . . ? Ag S2 C5 C6 146.19(18) . . . . ? S2 C5 C6 C13 48.3(3) . . . . ? C5 S2 C7 C8 -138.88(18) . . . . ? Ag S2 C7 C8 116.82(16) . . . . ? S2 C7 C8 N1 80.0(3) . . . 1_455 ? C11 S3 C9 C10 -141.34(17) . . . . ? Ag S3 C9 C10 107.64(16) . . . . ? S3 C9 C10 N1 78.4(2) . . . 4_745 ? C9 S3 C11 C12 49.5(2) . . . . ? Ag S3 C11 C12 161.03(18) . . . . ? S3 C11 C12 C13 43.7(3) . . . 4_645 ? C5 C6 C13 C4 178.6(2) . . . 1_455 ? C5 C6 C13 C12 54.5(3) . . . 4_655 ? O2 S4 O1 Ag 108.98(17) . . . 2_655 ? O3 S4 O1 Ag -19.4(2) . . . 2_655 ? C21 S4 O1 Ag -135.29(12) . . . 2_655 ? O2 S4 C21 C27 -112.3(2) . . . . ? O1 S4 C21 C27 126.3(3) . . . . ? O3 S4 C21 C27 6.8(3) . . . . ? O2 S4 C21 C22 65.2(2) . . . . ? O1 S4 C21 C22 -56.2(3) . . . . ? O3 S4 C21 C22 -175.7(2) . . . . ? C27 C21 C22 C23 -0.2(4) . . . . ? S4 C21 C22 C23 -177.7(2) . . . . ? C21 C22 C23 C24 -0.2(4) . . . . ? C22 C23 C24 C26 0.6(4) . . . . ? C22 C23 C24 C25 -179.6(3) . . . . ? C23 C24 C26 C27 -0.6(4) . . . . ? C25 C24 C26 C27 179.5(3) . . . . ? C22 C21 C27 C26 0.2(4) . . . . ? S4 C21 C27 C26 177.6(2) . . . . ? C24 C26 C27 C21 0.2(4) . . . . ? C1 C2 N1 C10 99.6(2) . . . 4_755 ? C1 C2 N1 C8 -121.6(2) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.411 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.060 #===END data_Jb230301_[Ag(16)Tosylat] _database_code_CSD 186813 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (out-7-Methyl-1-aza-4,10,15-trithia-bicyclo[5.5.5]heptadecan)Ag tosylate acetonitrile ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C14 H27 N S3)Ag(C7 H7 O3 S)(C2 H3 N)' _chemical_formula_sum 'C23 H37 Ag N2 O3 S4' _chemical_formula_weight 625.66 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinc _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.1923(6) _cell_length_b 13.8066(14) _cell_length_c 11.973(1) _cell_angle_alpha 90.00 _cell_angle_beta 92.14(1) _cell_angle_gamma 90.00 _cell_volume 1353.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 489 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6420 _exptl_absorpt_correction_T_max 0.7375 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Stoe IPDS' _diffrn_measurement_method '/f oscillation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 50-200 _diffrn_standards_interval_count 'image' _diffrn_standards_interval_time 6 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18638 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.08 _reflns_number_total 6393 _reflns_number_gt 5568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1999)' _computing_cell_refinement 'IPDS (Stoe, 1999)' _computing_data_reduction 'X-RED (Stoe, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0417P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(19) _refine_ls_number_reflns 6393 _refine_ls_number_parameters 301 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.008 _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 0.61331(3) 0.776911(15) 0.41234(2) 0.03123(7) Uani 1 1 d . . . N1 N 1.1423(3) 0.89361(18) 0.5523(2) 0.0255(5) Uani 1 1 d . . . N31 N 0.6233(6) 0.8551(3) 0.7503(5) 0.0769(13) Uani 1 1 d . . . O1 O 0.7977(3) 0.69628(19) 0.2811(2) 0.0426(6) Uani 1 1 d . . . O2 O 0.6592(3) 0.7858(3) 0.1339(2) 0.0564(8) Uani 1 1 d . . . O3 O 0.6329(4) 0.6110(3) 0.1427(3) 0.0761(11) Uani 1 1 d . . . S1 S 0.74332(9) 0.94051(5) 0.41816(7) 0.02876(17) Uani 1 1 d . . . S2 S 1.27726(9) 1.12579(5) 0.47971(7) 0.02709(16) Uani 1 1 d . . . S3 S 1.32895(9) 0.71921(5) 0.35159(8) 0.02961(17) Uani 1 1 d . . . S4 S 0.73343(11) 0.69533(7) 0.16508(8) 0.0395(2) Uani 1 1 d . . . C1 C 0.8531(4) 0.9561(2) 0.5517(3) 0.0320(7) Uani 1 1 d . . . H1A H 0.9144 1.0178 0.5491 0.038 Uiso 1 1 calc R . . H1B H 0.7716 0.9629 0.6103 0.038 Uiso 1 1 calc R . . C2 C 0.9741(4) 0.8752(2) 0.5881(3) 0.0300(7) Uani 1 1 d . . . H2A H 0.9757 0.8692 0.6705 0.036 Uiso 1 1 calc R . . H2B H 0.9353 0.8128 0.5561 0.036 Uiso 1 1 calc R . . C3 C 0.9067(4) 0.9191(2) 0.3207(3) 0.0288(7) Uani 1 1 d . . . H3A H 0.9784 0.8665 0.3503 0.035 Uiso 1 1 calc R . . H3B H 0.8580 0.8974 0.2481 0.035 Uiso 1 1 calc R . . C4 C 1.0093(4) 1.0094(2) 0.3025(3) 0.0279(7) Uani 1 1 d . . . H4A H 1.0384 1.0379 0.3765 0.033 Uiso 1 1 calc R . . H4B H 0.9407 1.0572 0.2608 0.033 Uiso 1 1 calc R . . C5 C 1.3781(4) 1.1140(2) 0.3452(3) 0.0310(7) Uani 1 1 d . . . H5A H 1.4370 1.1751 0.3307 0.037 Uiso 1 1 calc R . . H5B H 1.4607 1.0618 0.3525 0.037 Uiso 1 1 calc R . . C6 C 1.2645(4) 1.0917(2) 0.2430(3) 0.0316(7) Uani 1 1 d . . . H6A H 1.3313 1.0945 0.1758 0.038 Uiso 1 1 calc R . . H6B H 1.1835 1.1447 0.2361 0.038 Uiso 1 1 calc R . . C7 C 1.3572(4) 1.0255(2) 0.5678(3) 0.0287(7) Uani 1 1 d . . . H7A H 1.4191 0.9802 0.5212 0.034 Uiso 1 1 calc R . . H7B H 1.4334 1.0518 0.6264 0.034 Uiso 1 1 calc R . . C8 C 1.2194(4) 0.9701(2) 0.6234(3) 0.0289(7) Uani 1 1 d . . . H8A H 1.2638 0.9400 0.6932 0.035 Uiso 1 1 calc R . . H8B H 1.1342 1.0170 0.6442 0.035 Uiso 1 1 calc R . . C9 C 1.2049(4) 0.7254(2) 0.4749(3) 0.0308(7) Uani 1 1 d . . . H9A H 1.0896 0.7327 0.4485 0.037 Uiso 1 1 calc R . . H9B H 1.2138 0.6619 0.5132 0.037 Uiso 1 1 calc R . . C10 C 1.2402(4) 0.8044(2) 0.5634(3) 0.0281(7) Uani 1 1 d . . . H10A H 1.2226 0.7762 0.6381 0.034 Uiso 1 1 calc R . . H10B H 1.3571 0.8222 0.5610 0.034 Uiso 1 1 calc R . . C11 C 1.2418(4) 0.8086(2) 0.2551(3) 0.0325(7) Uani 1 1 d . . . H11A H 1.2842 0.7968 0.1800 0.039 Uiso 1 1 calc R . . H11B H 1.1218 0.7998 0.2499 0.039 Uiso 1 1 calc R . . C12 C 1.2798(4) 0.9142(2) 0.2894(3) 0.0286(7) Uani 1 1 d . . . H12A H 1.3935 0.9285 0.2694 0.034 Uiso 1 1 calc R . . H12B H 1.2757 0.9185 0.3718 0.034 Uiso 1 1 calc R . . C13 C 1.1689(4) 0.9944(2) 0.2387(3) 0.0275(6) Uani 1 1 d . . . C14 C 1.1260(7) 0.9722(4) 0.1162(4) 0.0616(12) Uani 1 1 d . . . H14A H 1.0575 1.0243 0.0844 0.074 Uiso 1 1 calc R . . H14B H 1.0664 0.9107 0.1108 0.074 Uiso 1 1 calc R . . H14C H 1.2266 0.9674 0.0747 0.074 Uiso 1 1 calc R . . C21 C 0.9114(4) 0.6823(3) 0.0850(3) 0.0386(8) Uani 1 1 d . . . C22 C 1.0334(6) 0.6175(4) 0.1234(4) 0.0553(11) Uani 1 1 d . . . H22 H 1.0196 0.5814 0.1900 0.066 Uiso 1 1 calc R . . C23 C 1.1752(7) 0.6066(4) 0.0630(5) 0.0644(13) Uani 1 1 d . . . H23 H 1.2587 0.5639 0.0899 0.077 Uiso 1 1 calc R . . C24 C 1.1957(5) 0.6567(4) -0.0348(4) 0.0510(10) Uani 1 1 d . . . C25 C 1.3490(6) 0.6400(5) -0.0983(4) 0.0683(14) Uani 1 1 d . . . H25A H 1.3478 0.6818 -0.1645 0.082 Uiso 1 1 calc R . . H25B H 1.3540 0.5720 -0.1215 0.082 Uiso 1 1 calc R . . H25C H 1.4448 0.6553 -0.0500 0.082 Uiso 1 1 calc R . . C26 C 1.0780(5) 0.7231(3) -0.0686(3) 0.0489(10) Uani 1 1 d . . . H26 H 1.0932 0.7605 -0.1340 0.059 Uiso 1 1 calc R . . C27 C 0.9361(5) 0.7366(3) -0.0081(3) 0.0415(8) Uani 1 1 d . . . H27 H 0.8574 0.7835 -0.0319 0.050 Uiso 1 1 calc R . . C31 C 0.5570(6) 0.8743(3) 0.8302(5) 0.0543(11) Uani 1 1 d . . . C32 C 0.4728(7) 0.8986(4) 0.9290(5) 0.0672(14) Uani 1 1 d . . . H32A H 0.4349 0.9658 0.9241 0.081 Uiso 1 1 calc R . . H32B H 0.5471 0.8911 0.9945 0.081 Uiso 1 1 calc R . . H32C H 0.3788 0.8554 0.9360 0.081 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 0.02205(10) 0.02513(10) 0.04663(14) 0.00137(13) 0.00289(9) -0.00013(11) N1 0.0212(12) 0.0217(11) 0.0334(15) 0.0009(10) 0.0002(11) -0.0008(10) N31 0.075(3) 0.061(3) 0.096(4) 0.000(3) 0.018(3) -0.005(2) O1 0.0510(16) 0.0412(14) 0.0360(14) 0.0019(11) 0.0090(12) 0.0051(12) O2 0.0431(14) 0.081(2) 0.0449(14) 0.0009(19) 0.0007(11) 0.0215(19) O3 0.058(2) 0.078(2) 0.094(3) -0.037(2) 0.020(2) -0.0290(18) S1 0.0168(3) 0.0243(3) 0.0452(5) 0.0033(3) 0.0004(3) 0.0013(3) S2 0.0221(4) 0.0226(3) 0.0363(4) -0.0006(3) -0.0015(3) 0.0001(3) S3 0.0218(4) 0.0212(3) 0.0456(5) -0.0044(3) -0.0014(3) 0.0021(3) S4 0.0325(5) 0.0425(5) 0.0440(5) -0.0106(4) 0.0080(4) -0.0054(4) C1 0.0265(16) 0.0263(15) 0.044(2) 0.0007(14) 0.0062(14) 0.0040(12) C2 0.0278(16) 0.0264(14) 0.0360(18) 0.0047(13) 0.0037(14) -0.0018(12) C3 0.0233(15) 0.0279(15) 0.0351(18) 0.0012(13) -0.0018(14) 0.0006(12) C4 0.0243(15) 0.0256(14) 0.0335(17) 0.0012(13) -0.0016(14) -0.0001(12) C5 0.0237(15) 0.0291(15) 0.0403(19) 0.0030(14) 0.0022(14) -0.0041(12) C6 0.0279(16) 0.0312(16) 0.0359(19) 0.0077(14) 0.0030(15) 0.0005(13) C7 0.0267(16) 0.0239(14) 0.0351(18) 0.0005(12) -0.0041(14) -0.0025(12) C8 0.0292(16) 0.0263(14) 0.0310(17) 0.0016(12) -0.0010(14) -0.0026(12) C9 0.0217(15) 0.0227(15) 0.048(2) 0.0024(14) -0.0013(14) -0.0013(12) C10 0.0205(14) 0.0241(15) 0.0393(18) 0.0036(12) -0.0047(13) 0.0022(10) C11 0.0283(16) 0.0282(15) 0.0410(19) -0.0061(13) -0.0014(15) 0.0048(12) C12 0.0248(15) 0.0272(15) 0.0336(18) 0.0001(13) -0.0013(14) -0.0017(12) C13 0.0271(16) 0.0276(15) 0.0276(16) 0.0028(12) -0.0013(13) 0.0001(13) C14 0.066(3) 0.059(3) 0.060(3) 0.005(2) 0.003(3) 0.002(2) C21 0.0350(19) 0.046(2) 0.0345(19) -0.0097(16) 0.0042(16) -0.0018(15) C22 0.056(3) 0.061(3) 0.050(3) 0.005(2) 0.015(2) 0.014(2) C23 0.058(3) 0.071(3) 0.065(3) 0.001(3) 0.015(3) 0.022(2) C24 0.044(2) 0.065(3) 0.044(2) -0.006(2) 0.0092(19) 0.002(2) C25 0.051(3) 0.096(4) 0.060(3) -0.009(3) 0.018(2) -0.001(3) C26 0.050(2) 0.063(3) 0.034(2) -0.0024(19) 0.0039(18) -0.006(2) C27 0.038(2) 0.049(2) 0.037(2) -0.0032(16) 0.0001(16) -0.0017(16) C31 0.048(2) 0.043(2) 0.072(3) 0.013(2) -0.001(2) -0.0010(19) C32 0.069(3) 0.058(3) 0.075(4) 0.015(2) 0.004(3) 0.011(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 Ag1 O1 2.483(3) . ? Ag1 S1 2.4971(8) . ? Ag1 S3 2.5425(8) 1_455 ? Ag1 S2 2.5963(8) 2_746 ? N1 C10 1.474(4) . ? N1 C2 1.480(4) . ? N1 C8 1.484(4) . ? N31 C31 1.148(7) . ? O1 S4 1.467(3) . ? O2 S4 1.433(4) . ? O3 S4 1.445(3) . ? S1 C1 1.818(4) . ? S1 C3 1.832(3) . ? S2 C5 1.844(3) . ? S2 C7 1.846(3) . ? S2 Ag1 2.5963(8) 2_756 ? S3 C11 1.818(4) . ? S3 C9 1.826(4) . ? S3 Ag1 2.5425(8) 1_655 ? S4 C21 1.784(4) . ? C1 C2 1.546(5) . ? C3 C4 1.524(4) . ? C4 C13 1.553(5) . ? C5 C6 1.541(5) . ? C6 C13 1.554(5) . ? C7 C8 1.536(5) . ? C9 C10 1.541(5) . ? C11 C12 1.543(4) . ? C12 C13 1.543(4) . ? C13 C14 1.527(6) . ? C21 C27 1.365(6) . ? C21 C22 1.406(6) . ? C22 C23 1.400(6) . ? C23 C24 1.376(7) . ? C24 C26 1.380(7) . ? C24 C25 1.510(6) . ? C26 C27 1.405(6) . ? C31 C32 1.431(8) . ? 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 O1 Ag1 S1 98.87(7) . . ? O1 Ag1 S3 104.53(7) . 1_455 ? S1 Ag1 S3 132.59(3) . 1_455 ? O1 Ag1 S2 75.40(6) . 2_746 ? S1 Ag1 S2 125.03(3) . 2_746 ? S3 Ag1 S2 100.74(3) 1_455 2_746 ? C10 N1 C2 109.8(2) . . ? C10 N1 C8 109.0(3) . . ? C2 N1 C8 109.7(3) . . ? S4 O1 Ag1 113.44(15) . . ? C1 S1 C3 103.29(15) . . ? C1 S1 Ag1 109.17(11) . . ? C3 S1 Ag1 99.04(10) . . ? C5 S2 C7 105.76(15) . . ? C5 S2 Ag1 110.37(11) . 2_756 ? C7 S2 Ag1 102.11(11) . 2_756 ? C11 S3 C9 105.37(16) . . ? C11 S3 Ag1 107.66(12) . 1_655 ? C9 S3 Ag1 106.61(11) . 1_655 ? O2 S4 O3 114.8(2) . . ? O2 S4 O1 111.89(17) . . ? O3 S4 O1 111.4(2) . . ? O2 S4 C21 107.20(18) . . ? O3 S4 C21 106.90(19) . . ? O1 S4 C21 103.76(17) . . ? C2 C1 S1 117.0(2) . . ? N1 C2 C1 112.8(3) . . ? C4 C3 S1 112.3(2) . . ? C3 C4 C13 116.1(3) . . ? C6 C5 S2 115.7(2) . . ? C5 C6 C13 119.2(3) . . ? C8 C7 S2 111.7(2) . . ? N1 C8 C7 114.2(3) . . ? C10 C9 S3 119.6(2) . . ? N1 C10 C9 116.2(3) . . ? C12 C11 S3 113.7(3) . . ? C11 C12 C13 117.6(3) . . ? C14 C13 C12 110.2(3) . . ? C14 C13 C4 109.4(3) . . ? C12 C13 C4 113.4(3) . . ? C14 C13 C6 107.6(3) . . ? C12 C13 C6 108.6(3) . . ? C4 C13 C6 107.6(3) . . ? C27 C21 C22 119.5(4) . . ? C27 C21 S4 122.2(3) . . ? C22 C21 S4 118.3(3) . . ? C23 C22 C21 119.5(4) . . ? C24 C23 C22 121.1(5) . . ? C23 C24 C26 118.5(4) . . ? C23 C24 C25 118.8(5) . . ? C26 C24 C25 122.6(4) . . ? C24 C26 C27 121.3(4) . . ? C21 C27 C26 119.9(4) . . ? N31 C31 C32 179.4(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 Ag1 O1 S4 -97.02(15) . . . . ? S3 Ag1 O1 S4 41.40(16) 1_455 . . . ? S2 Ag1 O1 S4 138.94(16) 2_746 . . . ? O1 Ag1 S1 C1 -106.60(13) . . . . ? S3 Ag1 S1 C1 134.16(11) 1_455 . . . ? S2 Ag1 S1 C1 -28.26(12) 2_746 . . . ? O1 Ag1 S1 C3 0.97(13) . . . . ? S3 Ag1 S1 C3 -118.27(12) 1_455 . . . ? S2 Ag1 S1 C3 79.31(12) 2_746 . . . ? Ag1 O1 S4 O2 41.6(2) . . . . ? Ag1 O1 S4 O3 -88.5(2) . . . . ? Ag1 O1 S4 C21 156.84(16) . . . . ? C3 S1 C1 C2 -53.4(3) . . . . ? Ag1 S1 C1 C2 51.3(3) . . . . ? C10 N1 C2 C1 -165.6(3) . . . . ? C8 N1 C2 C1 74.7(3) . . . . ? S1 C1 C2 N1 91.7(3) . . . . ? C1 S1 C3 C4 -69.5(3) . . . . ? Ag1 S1 C3 C4 178.2(2) . . . . ? S1 C3 C4 C13 169.4(2) . . . . ? C7 S2 C5 C6 115.8(2) . . . . ? Ag1 S2 C5 C6 -134.5(2) 2_756 . . . ? S2 C5 C6 C13 -63.7(4) . . . . ? C5 S2 C7 C8 -131.7(2) . . . . ? Ag1 S2 C7 C8 112.8(2) 2_756 . . . ? C10 N1 C8 C7 84.4(3) . . . . ? C2 N1 C8 C7 -155.4(3) . . . . ? S2 C7 C8 N1 84.6(3) . . . . ? C11 S3 C9 C10 -82.1(3) . . . . ? Ag1 S3 C9 C10 32.1(3) 1_655 . . . ? C2 N1 C10 C9 74.5(4) . . . . ? C8 N1 C10 C9 -165.3(3) . . . . ? S3 C9 C10 N1 94.8(3) . . . . ? C9 S3 C11 C12 73.4(3) . . . . ? Ag1 S3 C11 C12 -40.1(3) 1_655 . . . ? S3 C11 C12 C13 -160.0(2) . . . . ? C11 C12 C13 C14 -39.5(4) . . . . ? C11 C12 C13 C4 83.4(4) . . . . ? C11 C12 C13 C6 -157.1(3) . . . . ? C3 C4 C13 C14 70.6(4) . . . . ? C3 C4 C13 C12 -52.7(4) . . . . ? C3 C4 C13 C6 -172.8(3) . . . . ? C5 C6 C13 C14 -157.1(3) . . . . ? C5 C6 C13 C12 -37.8(4) . . . . ? C5 C6 C13 C4 85.2(3) . . . . ? O2 S4 C21 C27 -16.6(4) . . . . ? O3 S4 C21 C27 107.0(4) . . . . ? O1 S4 C21 C27 -135.1(3) . . . . ? O2 S4 C21 C22 159.8(3) . . . . ? O3 S4 C21 C22 -76.5(4) . . . . ? O1 S4 C21 C22 41.3(4) . . . . ? C27 C21 C22 C23 -2.7(7) . . . . ? S4 C21 C22 C23 -179.3(4) . . . . ? C21 C22 C23 C24 -1.5(8) . . . . ? C22 C23 C24 C26 4.3(8) . . . . ? C22 C23 C24 C25 -178.3(5) . . . . ? C23 C24 C26 C27 -3.0(7) . . . . ? C25 C24 C26 C27 179.6(5) . . . . ? C22 C21 C27 C26 3.9(6) . . . . ? S4 C21 C27 C26 -179.6(3) . . . . ? C24 C26 C27 C21 -1.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.08 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.741 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.080 data_jb130201 _database_code_CSD 186814 _audit_creation_method SHELXL-97 _chemical_name_systematic '1-Aza-4,10,15-trithia-7(1,3,5)-benzenabicyclo[5.5.5]heptadecaphan' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H27 N S3' _chemical_formula_sum 'C18 H27 N S3' _chemical_formula_weight 353.59 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9341(6) _cell_length_b 15.0765(9) _cell_length_c 13.6182(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.668(8) _cell_angle_gamma 90.00 _cell_volume 1802.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 270 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.408 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8610 _exptl_absorpt_correction_T_max 0.9512 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'STOE IPDS' _diffrn_measurement_method '/f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28591 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 28.18 _reflns_number_total 4367 _reflns_number_gt 3413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1999)' _computing_cell_refinement 'IPDS (Stoe, 1999)' _computing_data_reduction 'X-RED (Stoe, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Zortep (Zsolnai, 1994), ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4367 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 S1 S 1.50126(5) 0.31224(3) 0.16417(4) 0.03878(13) Uani 1 1 d . . . S2 S 0.96126(5) 0.05997(3) 0.26095(3) 0.03405(12) Uani 1 1 d . . . S3 S 1.39493(5) -0.11345(3) 0.10229(4) 0.03974(13) Uani 1 1 d . . . N1 N 1.16286(15) 0.12521(10) 0.08421(11) 0.0312(3) Uani 1 1 d . . . C1 C 1.51149(17) 0.14902(11) 0.36437(12) 0.0286(3) Uani 1 1 d . . . C2 C 1.37549(18) 0.14702(11) 0.40205(12) 0.0294(3) Uani 1 1 d . . . H2A H 1.3365 0.1997 0.4224 0.035 Uiso 1 1 calc R . . C3 C 1.29752(18) 0.06777(11) 0.40961(12) 0.0299(3) Uani 1 1 d . . . C4 C 1.35734(18) -0.01101(11) 0.37889(13) 0.0313(3) Uani 1 1 d . . . H3A H 1.3066 -0.0642 0.3839 0.038 Uiso 1 1 calc R . . C5 C 1.49242(18) -0.01117(11) 0.34069(12) 0.0308(3) Uani 1 1 d . . . C6 C 1.56857(17) 0.06905(11) 0.33472(12) 0.0298(3) Uani 1 1 d . . . H4A H 1.6593 0.0692 0.3105 0.036 Uiso 1 1 calc R . . C11 C 1.59739(18) 0.23533(12) 0.35717(13) 0.0336(3) Uani 1 1 d . . . H8B H 1.6845 0.2226 0.3262 0.040 Uiso 1 1 calc R . . H8A H 1.6362 0.2562 0.4244 0.040 Uiso 1 1 calc R . . C12 C 1.5056(2) 0.31079(11) 0.29846(14) 0.0339(3) Uani 1 1 d . . . H11B H 1.5473 0.3668 0.3260 0.041 Uiso 1 1 calc R . . H11A H 1.4015 0.3072 0.3095 0.041 Uiso 1 1 calc R . . C13 C 1.40805(19) 0.20856(12) 0.12013(13) 0.0335(3) Uani 1 1 d . . . H16B H 1.4122 0.2013 0.0499 0.040 Uiso 1 1 calc R . . H16A H 1.4640 0.1598 0.1562 0.040 Uiso 1 1 calc R . . C14 C 1.24169(18) 0.20328(12) 0.13312(13) 0.0323(3) Uani 1 1 d . . . H15B H 1.2382 0.2014 0.2039 0.039 Uiso 1 1 calc R . . H15A H 1.1887 0.2564 0.1054 0.039 Uiso 1 1 calc R . . C21 C 1.1481(2) 0.06727(13) 0.44783(13) 0.0369(4) Uani 1 1 d . . . H12B H 1.1645 0.0940 0.5137 0.044 Uiso 1 1 calc R . . H12A H 1.1169 0.0063 0.4545 0.044 Uiso 1 1 calc R . . C22 C 1.0189(2) 0.11705(13) 0.37988(15) 0.0381(4) Uani 1 1 d . . . H10B H 1.0526 0.1766 0.3678 0.046 Uiso 1 1 calc R . . H10A H 0.9322 0.1219 0.4131 0.046 Uiso 1 1 calc R . . C23 C 0.9300(2) 0.14978(13) 0.16999(16) 0.0411(4) Uani 1 1 d . . . H18B H 0.8214 0.1599 0.1505 0.049 Uiso 1 1 calc R . . H18A H 0.9753 0.2036 0.2015 0.049 Uiso 1 1 calc R . . C24 C 0.99676(19) 0.13188(14) 0.07540(14) 0.0389(4) Uani 1 1 d . . . H17B H 0.9527 0.0769 0.0462 0.047 Uiso 1 1 calc R . . H17A H 0.9616 0.1788 0.0279 0.047 Uiso 1 1 calc R . . C31 C 1.5543(2) -0.09657(12) 0.30478(16) 0.0417(4) Uani 1 1 d . . . H14B H 1.4879 -0.1448 0.3164 0.050 Uiso 1 1 calc R . . H14A H 1.6537 -0.1078 0.3454 0.050 Uiso 1 1 calc R . . C32 C 1.5701(2) -0.09864(13) 0.19474(16) 0.0410(4) Uani 1 1 d . . . H13B H 1.6394 -0.1463 0.1861 0.049 Uiso 1 1 calc R . . H13A H 1.6173 -0.0436 0.1798 0.049 Uiso 1 1 calc R . . C33 C 1.3360(2) -0.00105(12) 0.06223(14) 0.0356(4) Uani 1 1 d . . . H1B H 1.4256 0.0362 0.0673 0.043 Uiso 1 1 calc R . . H1A H 1.2860 -0.0024 -0.0074 0.043 Uiso 1 1 calc R . . C34 C 1.22735(18) 0.03986(11) 0.12476(13) 0.0313(3) Uani 1 1 d . . . H6B H 1.1449 -0.0014 0.1274 0.038 Uiso 1 1 calc R . . H6A H 1.2819 0.0489 0.1925 0.038 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 S1 0.0408(2) 0.0352(2) 0.0422(3) 0.00448(19) 0.01249(18) -0.00836(17) S2 0.0317(2) 0.0326(2) 0.0401(2) -0.00214(17) 0.01246(16) -0.00258(15) S3 0.0377(2) 0.0316(2) 0.0523(3) -0.01186(19) 0.01447(19) -0.00404(17) N1 0.0270(6) 0.0372(7) 0.0286(7) 0.0006(6) 0.0037(5) 0.0001(5) C1 0.0255(7) 0.0334(8) 0.0265(7) -0.0011(6) 0.0038(5) -0.0021(6) C2 0.0286(7) 0.0319(8) 0.0284(8) -0.0038(6) 0.0069(6) 0.0008(6) C3 0.0280(7) 0.0366(8) 0.0256(7) 0.0020(6) 0.0063(6) -0.0014(6) C4 0.0308(7) 0.0304(8) 0.0325(8) 0.0058(6) 0.0054(6) -0.0025(6) C5 0.0286(7) 0.0318(8) 0.0312(8) 0.0027(7) 0.0036(6) 0.0040(6) C6 0.0220(7) 0.0366(8) 0.0311(8) 0.0015(7) 0.0056(6) 0.0019(6) C11 0.0285(7) 0.0358(8) 0.0362(9) -0.0040(7) 0.0054(6) -0.0057(6) C12 0.0343(8) 0.0276(8) 0.0416(9) -0.0054(7) 0.0120(7) -0.0052(6) C13 0.0330(8) 0.0366(8) 0.0318(8) 0.0005(7) 0.0087(6) -0.0012(7) C14 0.0309(8) 0.0351(8) 0.0313(8) -0.0008(7) 0.0064(6) -0.0001(6) C21 0.0329(8) 0.0481(10) 0.0324(9) -0.0002(8) 0.0133(7) -0.0030(7) C22 0.0323(8) 0.0424(10) 0.0425(10) -0.0076(8) 0.0146(7) 0.0005(7) C23 0.0314(8) 0.0428(10) 0.0510(11) 0.0063(9) 0.0126(7) 0.0088(7) C24 0.0283(8) 0.0491(10) 0.0374(9) 0.0060(8) 0.0011(6) 0.0015(7) C31 0.0391(9) 0.0334(9) 0.0523(11) 0.0009(8) 0.0081(8) 0.0082(7) C32 0.0311(8) 0.0363(9) 0.0583(12) -0.0091(8) 0.0159(8) 0.0054(7) C33 0.0347(8) 0.0370(9) 0.0381(9) -0.0053(7) 0.0142(7) -0.0040(7) C34 0.0299(7) 0.0342(8) 0.0312(8) -0.0021(7) 0.0093(6) 0.0001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C13 1.8198(18) . ? S1 C12 1.822(2) . ? S2 C23 1.822(2) . ? S2 C22 1.822(2) . ? S3 C33 1.8276(19) . ? S3 C32 1.832(2) . ? N1 C14 1.467(2) . ? N1 C24 1.470(2) . ? N1 C34 1.475(2) . ? C1 C6 1.397(2) . ? C1 C2 1.404(2) . ? C1 C11 1.523(2) . ? C2 C3 1.396(2) . ? C3 C4 1.398(2) . ? C3 C21 1.520(2) . ? C4 C5 1.400(2) . ? C5 C6 1.397(2) . ? C5 C31 1.518(2) . ? C11 C12 1.537(3) . ? C13 C14 1.531(2) . ? C21 C22 1.535(3) . ? C23 C24 1.540(3) . ? C31 C32 1.531(3) . ? C33 C34 1.534(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 C13 S1 C12 104.11(8) . . ? C23 S2 C22 103.64(10) . . ? C33 S3 C32 104.74(9) . . ? C14 N1 C24 112.01(14) . . ? C14 N1 C34 114.12(13) . . ? C24 N1 C34 114.13(14) . . ? C6 C1 C2 118.28(15) . . ? C6 C1 C11 120.22(14) . . ? C2 C1 C11 121.49(15) . . ? C3 C2 C1 121.51(15) . . ? C2 C3 C4 118.77(15) . . ? C2 C3 C21 120.75(15) . . ? C4 C3 C21 120.46(15) . . ? C3 C4 C5 121.09(15) . . ? C6 C5 C4 118.86(15) . . ? C6 C5 C31 120.34(15) . . ? C4 C5 C31 120.79(16) . . ? C1 C6 C5 121.48(15) . . ? C1 C11 C12 116.04(13) . . ? C11 C12 S1 116.16(12) . . ? C14 C13 S1 113.66(12) . . ? N1 C14 C13 112.58(14) . . ? C3 C21 C22 113.65(14) . . ? C21 C22 S2 111.23(13) . . ? C24 C23 S2 113.85(13) . . ? N1 C24 C23 119.01(15) . . ? C5 C31 C32 115.96(16) . . ? C31 C32 S3 116.96(13) . . ? C34 C33 S3 112.58(12) . . ? N1 C34 C33 112.73(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.4(2) . . . . ? C11 C1 C2 C3 -179.34(15) . . . . ? C1 C2 C3 C4 0.1(2) . . . . ? C1 C2 C3 C21 -178.25(15) . . . . ? C2 C3 C4 C5 -0.3(2) . . . . ? C21 C3 C4 C5 178.04(15) . . . . ? C3 C4 C5 C6 0.8(2) . . . . ? C3 C4 C5 C31 -178.27(16) . . . . ? C2 C1 C6 C5 0.9(2) . . . . ? C11 C1 C6 C5 179.85(15) . . . . ? C4 C5 C6 C1 -1.1(2) . . . . ? C31 C5 C6 C1 177.98(16) . . . . ? C6 C1 C11 C12 125.91(17) . . . . ? C2 C1 C11 C12 -55.1(2) . . . . ? C1 C11 C12 S1 -87.44(16) . . . . ? C13 S1 C12 C11 62.33(14) . . . . ? C12 S1 C13 C14 65.11(14) . . . . ? C24 N1 C14 C13 -165.85(14) . . . . ? C34 N1 C14 C13 62.53(18) . . . . ? S1 C13 C14 N1 171.68(12) . . . . ? C2 C3 C21 C22 64.6(2) . . . . ? C4 C3 C21 C22 -113.76(19) . . . . ? C3 C21 C22 S2 67.58(18) . . . . ? C23 S2 C22 C21 -139.75(13) . . . . ? C22 S2 C23 C24 136.18(14) . . . . ? C14 N1 C24 C23 -54.2(2) . . . . ? C34 N1 C24 C23 77.4(2) . . . . ? S2 C23 C24 N1 -65.8(2) . . . . ? C6 C5 C31 C32 -59.4(2) . . . . ? C4 C5 C31 C32 119.61(19) . . . . ? C5 C31 C32 S3 -76.32(19) . . . . ? C33 S3 C32 C31 95.60(15) . . . . ? C32 S3 C33 C34 -91.26(14) . . . . ? C14 N1 C34 C33 -97.98(17) . . . . ? C24 N1 C34 C33 131.44(16) . . . . ? S3 C33 C34 N1 -172.04(11) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.18 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.885 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.055 #===END data_jb110400 _database_code_CSD 180039 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Silver(I)(1-aza-4,10,15-trithia-7(1,3,5)-benzenabicyclo[5.5.5] heptadecaphan)]PF6 ; _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Kaden, Thomas' 'Alberto, Roger' 'Baumeister, Jan M.' 'Ortner, Kirsten' 'Schubiger, P. August' 'Spingler, Bernhard' _publ_contact_author_name 'Prof Thomas Kaden' _publ_contact_author_address ; Department of Inorganic Chemistry University of Basel Spitalstrasse 51 Basel CH-4056 SWITZERLAND ; _publ_contact_author_email 'TH.KADEN@UNIBAS.CH' _publ_section_title ; Unexpected peripheral coordination of Ag(I) with a novel type of a macrobicyclic NS3-metacyclophane ; _chemical_name_common [Ag(NS3Phan)]PF6 _chemical_melting_point ? _chemical_formula_moiety [Ag(NS3Phan)]PF6 _chemical_formula_sum 'C18 H27 Ag F6 N P S3' _chemical_formula_weight 606.43 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' 'S' 'S' 0.1246 0.1234 '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2112(9) _cell_length_b 13.5373(12) _cell_length_c 13.9691(9) _cell_angle_alpha 90.00 _cell_angle_beta 115.847(7) _cell_angle_gamma 90.00 _cell_volume 2248.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 201 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.302 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8023 _exptl_absorpt_correction_T_max 0.8876 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Stoe IPDS' _diffrn_measurement_method '/f rotation scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 50-200 _diffrn_standards_interval_count 'every image' _diffrn_standards_interval_time 5 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15549 _diffrn_reflns_av_R_equivalents 0.1027 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.94 _reflns_number_total 4146 _reflns_number_gt 3158 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1999)' _computing_cell_refinement 'IPDS (Stoe, 1999)' _computing_data_reduction 'X-RED (Stoe, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Zortep (Zsolnai, 1994), Platon (Spek, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4146 _refine_ls_number_parameters 280 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.875 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.26531(2) 0.27023(2) 0.14031(3) 0.03030(10) Uani 0.90 1 d PU . . Ag2 Ag 0.2757(3) 0.2402(2) 0.1941(3) 0.0413(7) Uani 0.10 1 d PU . . N1 N 0.4449(2) 0.25161(16) 0.12700(19) 0.0276(5) Uani 1 1 d . . . S1 S 0.35403(7) 0.40124(6) -0.15117(6) 0.0368(2) Uani 1 1 d . . . S2 S 0.36999(6) 0.39813(5) 0.27623(6) 0.03029(18) Uani 1 1 d . . . S3 S 0.22333(7) 0.10141(5) 0.06157(6) 0.03191(19) Uani 1 1 d . . . C1 C 0.4608(3) 0.3008(2) 0.0381(3) 0.0340(7) Uani 1 1 d . . . H1A H 0.5337 0.3360 0.0673 0.041 Uiso 1 1 calc R . . H1B H 0.4622 0.2501 -0.0124 0.041 Uiso 1 1 calc R . . C2 C 0.3675(3) 0.3723(3) -0.0192(3) 0.0517(10) Uani 1 1 d . . . H2A H 0.3819 0.4340 0.0228 0.062 Uiso 1 1 calc R . . H2B H 0.2958 0.3440 -0.0253 0.062 Uiso 1 1 calc R . . C3 C 0.2596(3) 0.5071(2) -0.1849(3) 0.0411(8) Uani 1 1 d . . . H3A H 0.2870 0.5527 -0.1233 0.049 Uiso 1 1 calc R . . H3B H 0.2638 0.5426 -0.2450 0.049 Uiso 1 1 calc R . . C4 C 0.1358(3) 0.4828(3) -0.2153(3) 0.0451(9) Uani 1 1 d . . . H4A H 0.0915 0.5446 -0.2381 0.054 Uiso 1 1 calc R . . H4B H 0.1082 0.4376 -0.2772 0.054 Uiso 1 1 calc R . . C5 C 0.1130(2) 0.4362(2) -0.1287(3) 0.0338(7) Uani 1 1 d . . . C6 C 0.1404(2) 0.4876(2) -0.0335(3) 0.0321(7) Uani 1 1 d . . . H6 H 0.1685 0.5531 -0.0265 0.038 Uiso 1 1 calc R . . C7 C 0.1272(2) 0.4451(2) 0.0507(3) 0.0301(7) Uani 1 1 d . . . C8 C 0.0814(2) 0.3493(2) 0.0376(2) 0.0294(7) Uani 1 1 d . . . H8 H 0.0679 0.3206 0.0930 0.035 Uiso 1 1 calc R . . C9 C 0.0554(2) 0.2956(2) -0.0564(3) 0.0315(7) Uani 1 1 d . . . C10 C 0.0709(2) 0.3407(2) -0.1386(2) 0.0343(7) Uani 1 1 d . . . H10 H 0.0523 0.3054 -0.2029 0.041 Uiso 1 1 calc R . . C11 C 0.5257(2) 0.2897(2) 0.2319(2) 0.0298(7) Uani 1 1 d . . . H11A H 0.6020 0.2896 0.2349 0.036 Uiso 1 1 calc R . . H11B H 0.5267 0.2445 0.2880 0.036 Uiso 1 1 calc R . . C12 C 0.4980(2) 0.3944(2) 0.2552(2) 0.0300(7) Uani 1 1 d . . . H12A H 0.4879 0.4381 0.1949 0.036 Uiso 1 1 calc R . . H12B H 0.5621 0.4201 0.3194 0.036 Uiso 1 1 calc R . . C13 C 0.2961(3) 0.5132(2) 0.2129(3) 0.0344(7) Uani 1 1 d . . . H13A H 0.3144 0.5651 0.2679 0.041 Uiso 1 1 calc R . . H13B H 0.3234 0.5359 0.1608 0.041 Uiso 1 1 calc R . . C14 C 0.1677(3) 0.4996(2) 0.1558(3) 0.0342(7) Uani 1 1 d . . . H14A H 0.1432 0.4627 0.2032 0.041 Uiso 1 1 calc R . . H14B H 0.1315 0.5654 0.1428 0.041 Uiso 1 1 calc R . . C21 C 0.4495(2) 0.1426(2) 0.1178(2) 0.0303(7) Uani 1 1 d . . . H21A H 0.4609 0.1120 0.1861 0.036 Uiso 1 1 calc R . . H21B H 0.5149 0.1251 0.1043 0.036 Uiso 1 1 calc R . . C22 C 0.3426(3) 0.1001(2) 0.0285(3) 0.0334(7) Uani 1 1 d . . . H22A H 0.3572 0.0313 0.0139 0.040 Uiso 1 1 calc R . . H22B H 0.3234 0.1392 -0.0371 0.040 Uiso 1 1 calc R . . C23 C 0.1016(3) 0.1146(2) -0.0684(3) 0.0425(9) Uani 1 1 d . . . H23A H 0.1279 0.1360 -0.1214 0.051 Uiso 1 1 calc R . . H23B H 0.0647 0.0494 -0.0910 0.051 Uiso 1 1 calc R . . C24 C 0.0151(3) 0.1892(2) -0.0667(3) 0.0416(9) Uani 1 1 d . . . H24A H -0.0551 0.1823 -0.1332 0.050 Uiso 1 1 calc R . . H24B H -0.0025 0.1734 -0.0064 0.050 Uiso 1 1 calc R . . P1 P 0.76636(7) 0.20128(6) 0.06155(7) 0.0316(2) Uani 1 1 d . . . F1 F 0.7523(2) 0.23654(15) 0.16406(18) 0.0549(6) Uani 1 1 d . . . F2 F 0.64753(17) 0.14451(14) 0.01982(19) 0.0529(6) Uani 1 1 d . . . F3 F 0.82941(19) 0.10356(14) 0.12325(19) 0.0567(6) Uani 1 1 d . . . F4 F 0.77732(19) 0.16409(18) -0.04168(18) 0.0600(6) Uani 1 1 d . . . F5 F 0.88423(17) 0.25818(15) 0.10335(19) 0.0562(6) Uani 1 1 d . . . F6 F 0.70131(17) 0.29853(14) -0.00039(18) 0.0523(6) 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 0.02357(14) 0.03232(16) 0.03590(19) -0.00920(13) 0.01379(14) -0.00101(11) Ag2 0.0428(16) 0.0409(16) 0.0478(18) -0.0002(14) 0.0269(16) -0.0008(12) N1 0.0294(13) 0.0282(12) 0.0238(12) 0.0015(9) 0.0103(11) 0.0022(10) S1 0.0446(5) 0.0421(4) 0.0268(4) 0.0081(3) 0.0184(4) 0.0083(3) S2 0.0302(4) 0.0354(4) 0.0268(4) -0.0035(3) 0.0139(3) 0.0010(3) S3 0.0355(4) 0.0304(4) 0.0306(4) -0.0014(3) 0.0152(3) -0.0032(3) C1 0.0299(16) 0.0417(17) 0.0345(17) 0.0006(13) 0.0178(14) 0.0033(13) C2 0.056(2) 0.069(2) 0.037(2) 0.0171(17) 0.0265(19) 0.0263(19) C3 0.057(2) 0.0354(17) 0.0360(18) 0.0089(14) 0.0247(18) 0.0060(15) C4 0.045(2) 0.051(2) 0.0354(19) 0.0105(15) 0.0139(17) 0.0154(16) C5 0.0224(15) 0.0424(17) 0.0325(17) 0.0010(13) 0.0080(13) 0.0108(13) C6 0.0245(15) 0.0309(15) 0.0411(19) -0.0017(13) 0.0146(14) 0.0036(12) C7 0.0168(13) 0.0332(15) 0.0388(18) -0.0063(13) 0.0107(13) 0.0040(11) C8 0.0175(13) 0.0349(15) 0.0366(17) -0.0034(12) 0.0124(13) 0.0012(11) C9 0.0180(13) 0.0354(16) 0.0386(18) -0.0098(13) 0.0101(13) -0.0005(11) C10 0.0222(15) 0.0454(18) 0.0288(16) -0.0100(13) 0.0051(13) 0.0049(12) C11 0.0208(14) 0.0420(17) 0.0251(15) -0.0001(12) 0.0084(13) 0.0024(12) C12 0.0221(14) 0.0382(16) 0.0270(15) -0.0024(12) 0.0083(13) -0.0019(12) C13 0.0299(16) 0.0297(15) 0.0387(18) -0.0115(13) 0.0105(15) 0.0008(12) C14 0.0271(16) 0.0344(15) 0.0418(19) -0.0109(13) 0.0156(15) 0.0020(12) C21 0.0306(16) 0.0323(15) 0.0307(16) 0.0005(12) 0.0158(14) 0.0080(12) C22 0.0409(18) 0.0317(15) 0.0298(16) -0.0022(12) 0.0174(15) 0.0054(13) C23 0.0313(17) 0.0405(18) 0.043(2) -0.0140(14) 0.0044(16) -0.0013(14) C24 0.0259(16) 0.0386(17) 0.051(2) -0.0161(15) 0.0084(16) -0.0069(13) P1 0.0279(4) 0.0318(4) 0.0387(5) -0.0023(3) 0.0178(4) -0.0005(3) F1 0.0702(15) 0.0531(12) 0.0521(13) -0.0109(10) 0.0367(12) -0.0002(10) F2 0.0392(11) 0.0426(11) 0.0805(16) -0.0137(10) 0.0294(11) -0.0094(9) F3 0.0601(14) 0.0435(11) 0.0629(14) 0.0062(10) 0.0235(12) 0.0158(10) F4 0.0534(13) 0.0848(15) 0.0497(13) -0.0130(11) 0.0299(11) 0.0026(11) F5 0.0335(11) 0.0647(13) 0.0648(14) 0.0029(11) 0.0161(11) -0.0133(9) F6 0.0469(12) 0.0403(10) 0.0617(14) 0.0072(9) 0.0163(11) 0.0015(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 Ag2 0.812(4) . ? Ag1 C8 2.464(3) . ? Ag1 N1 2.472(3) . ? Ag1 S3 2.4916(8) . ? Ag1 S2 2.4952(8) . ? Ag2 S2 2.488(3) . ? Ag2 S3 2.514(3) . ? Ag2 S1 2.730(4) 4_566 ? N1 C11 1.479(4) . ? N1 C21 1.486(3) . ? N1 C1 1.502(4) . ? S1 C2 1.816(4) . ? S1 C3 1.822(3) . ? S1 Ag2 2.730(4) 4_565 ? S2 C12 1.839(3) . ? S2 C13 1.847(3) . ? S3 C22 1.826(3) . ? S3 C23 1.835(3) . ? C1 C2 1.496(4) . ? C3 C4 1.537(5) . ? C4 C5 1.506(5) . ? C5 C10 1.390(5) . ? C5 C6 1.401(5) . ? C6 C7 1.387(5) . ? C7 C8 1.408(4) . ? C7 C14 1.517(4) . ? C8 C9 1.405(4) . ? C9 C10 1.392(5) . ? C9 C24 1.522(4) . ? C11 C12 1.534(4) . ? C13 C14 1.539(4) . ? C21 C22 1.531(4) . ? C23 C24 1.532(5) . ? P1 F4 1.592(2) . ? P1 F1 1.596(2) . ? P1 F3 1.600(2) . ? P1 F5 1.602(2) . ? P1 F6 1.604(2) . ? P1 F2 1.612(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 Ag2 Ag1 C8 118.9(3) . . ? Ag2 Ag1 N1 103.8(2) . . ? C8 Ag1 N1 137.35(10) . . ? Ag2 Ag1 S3 82.2(2) . . ? C8 Ag1 S3 99.69(7) . . ? N1 Ag1 S3 84.80(6) . . ? Ag2 Ag1 S2 80.1(2) . . ? C8 Ag1 S2 102.73(7) . . ? N1 Ag1 S2 84.05(6) . . ? S3 Ag1 S2 156.24(3) . . ? Ag1 Ag2 S2 81.1(2) . . ? Ag1 Ag2 S3 79.1(2) . . ? S2 Ag2 S3 154.59(17) . . ? Ag1 Ag2 S1 159.5(3) . 4_566 ? S2 Ag2 S1 107.28(14) . 4_566 ? S3 Ag2 S1 86.94(10) . 4_566 ? C11 N1 C21 113.1(2) . . ? C11 N1 C1 111.3(2) . . ? C21 N1 C1 110.0(2) . . ? C11 N1 Ag1 101.08(18) . . ? C21 N1 Ag1 100.68(17) . . ? C1 N1 Ag1 120.12(17) . . ? C2 S1 C3 100.66(16) . . ? C2 S1 Ag2 119.21(16) . 4_565 ? C3 S1 Ag2 111.51(13) . 4_565 ? C12 S2 C13 106.09(15) . . ? C12 S2 Ag2 102.31(12) . . ? C13 S2 Ag2 116.77(13) . . ? C12 S2 Ag1 95.89(10) . . ? C13 S2 Ag1 102.66(9) . . ? Ag2 S2 Ag1 18.76(9) . . ? C22 S3 C23 103.41(17) . . ? C22 S3 Ag1 94.00(10) . . ? C23 S3 Ag1 106.14(10) . . ? C22 S3 Ag2 101.69(12) . . ? C23 S3 Ag2 119.81(14) . . ? Ag1 S3 Ag2 18.67(9) . . ? C2 C1 N1 110.5(3) . . ? C1 C2 S1 112.1(3) . . ? C4 C3 S1 115.4(2) . . ? C5 C4 C3 115.4(3) . . ? C10 C5 C6 118.9(3) . . ? C10 C5 C4 121.4(3) . . ? C6 C5 C4 119.7(3) . . ? C7 C6 C5 121.5(3) . . ? C6 C7 C8 118.5(3) . . ? C6 C7 C14 119.8(3) . . ? C8 C7 C14 121.6(3) . . ? C9 C8 C7 120.9(3) . . ? C9 C8 Ag1 95.57(18) . . ? C7 C8 Ag1 93.74(17) . . ? C10 C9 C8 118.7(3) . . ? C10 C9 C24 120.5(3) . . ? C8 C9 C24 120.8(3) . . ? C5 C10 C9 121.5(3) . . ? N1 C11 C12 113.3(2) . . ? C11 C12 S2 112.3(2) . . ? C14 C13 S2 112.3(2) . . ? C7 C14 C13 113.8(3) . . ? N1 C21 C22 112.6(2) . . ? C21 C22 S3 112.4(2) . . ? C24 C23 S3 112.8(2) . . ? C9 C24 C23 113.2(3) . . ? F4 P1 F1 178.34(13) . . ? F4 P1 F3 89.71(13) . . ? F1 P1 F3 90.06(12) . . ? F4 P1 F5 91.40(13) . . ? F1 P1 F5 90.25(13) . . ? F3 P1 F5 90.35(12) . . ? F4 P1 F6 90.56(13) . . ? F1 P1 F6 89.64(12) . . ? F3 P1 F6 179.08(13) . . ? F5 P1 F6 90.52(11) . . ? F4 P1 F2 88.88(12) . . ? F1 P1 F2 89.47(13) . . ? F3 P1 F2 89.82(12) . . ? F5 P1 F2 179.67(14) . . ? F6 P1 F2 89.31(11) . . ? 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 C8 Ag1 Ag2 S2 -99.19(14) . . . . ? N1 Ag1 Ag2 S2 81.32(9) . . . . ? S3 Ag1 Ag2 S2 164.00(7) . . . . ? C8 Ag1 Ag2 S3 96.82(14) . . . . ? N1 Ag1 Ag2 S3 -82.68(8) . . . . ? S2 Ag1 Ag2 S3 -164.00(7) . . . . ? C8 Ag1 Ag2 S1 144.8(7) . . . 4_566 ? N1 Ag1 Ag2 S1 -34.7(8) . . . 4_566 ? S3 Ag1 Ag2 S1 47.9(7) . . . 4_566 ? S2 Ag1 Ag2 S1 -116.1(8) . . . 4_566 ? Ag2 Ag1 N1 C11 -55.0(3) . . . . ? C8 Ag1 N1 C11 125.61(17) . . . . ? S3 Ag1 N1 C11 -135.73(16) . . . . ? S2 Ag1 N1 C11 23.25(15) . . . . ? Ag2 Ag1 N1 C21 61.3(3) . . . . ? C8 Ag1 N1 C21 -118.03(18) . . . . ? S3 Ag1 N1 C21 -19.37(15) . . . . ? S2 Ag1 N1 C21 139.61(16) . . . . ? Ag2 Ag1 N1 C1 -177.9(3) . . . . ? C8 Ag1 N1 C1 2.8(3) . . . . ? S3 Ag1 N1 C1 101.46(19) . . . . ? S2 Ag1 N1 C1 -99.56(19) . . . . ? Ag1 Ag2 S2 C12 -71.6(3) . . . . ? S3 Ag2 S2 C12 -32.5(4) . . . . ? S1 Ag2 S2 C12 89.17(15) 4_566 . . . ? Ag1 Ag2 S2 C13 43.7(3) . . . . ? S3 Ag2 S2 C13 82.9(4) . . . . ? S1 Ag2 S2 C13 -155.50(15) 4_566 . . . ? S3 Ag2 S2 Ag1 39.1(3) . . . . ? S1 Ag2 S2 Ag1 160.8(3) 4_566 . . . ? Ag2 Ag1 S2 C12 111.3(3) . . . . ? C8 Ag1 S2 C12 -131.13(12) . . . . ? N1 Ag1 S2 C12 6.14(11) . . . . ? S3 Ag1 S2 C12 68.58(13) . . . . ? Ag2 Ag1 S2 C13 -140.8(3) . . . . ? C8 Ag1 S2 C13 -23.15(14) . . . . ? N1 Ag1 S2 C13 114.13(13) . . . . ? S3 Ag1 S2 C13 176.56(13) . . . . ? C8 Ag1 S2 Ag2 117.6(3) . . . . ? N1 Ag1 S2 Ag2 -105.1(2) . . . . ? S3 Ag1 S2 Ag2 -42.7(2) . . . . ? Ag2 Ag1 S3 C22 -115.3(3) . . . . ? C8 Ag1 S3 C22 126.58(13) . . . . ? N1 Ag1 S3 C22 -10.63(12) . . . . ? S2 Ag1 S3 C22 -72.92(13) . . . . ? Ag2 Ag1 S3 C23 139.5(3) . . . . ? C8 Ag1 S3 C23 21.37(16) . . . . ? N1 Ag1 S3 C23 -115.83(15) . . . . ? S2 Ag1 S3 C23 -178.12(15) . . . . ? C8 Ag1 S3 Ag2 -118.1(3) . . . . ? N1 Ag1 S3 Ag2 104.7(2) . . . . ? S2 Ag1 S3 Ag2 42.4(2) . . . . ? Ag1 Ag2 S3 C22 67.1(3) . . . . ? S2 Ag2 S3 C22 27.7(4) . . . . ? S1 Ag2 S3 C22 -97.84(13) 4_566 . . . ? Ag1 Ag2 S3 C23 -46.0(3) . . . . ? S2 Ag2 S3 C23 -85.4(4) . . . . ? S1 Ag2 S3 C23 149.11(16) 4_566 . . . ? S2 Ag2 S3 Ag1 -39.4(3) . . . . ? S1 Ag2 S3 Ag1 -164.9(3) 4_566 . . . ? C11 N1 C1 C2 -106.5(3) . . . . ? C21 N1 C1 C2 127.3(3) . . . . ? Ag1 N1 C1 C2 11.2(3) . . . . ? N1 C1 C2 S1 -160.1(2) . . . . ? C3 S1 C2 C1 -167.7(3) . . . . ? Ag2 S1 C2 C1 70.1(3) 4_565 . . . ? C2 S1 C3 C4 -75.4(3) . . . . ? Ag2 S1 C3 C4 52.0(3) 4_565 . . . ? S1 C3 C4 C5 63.2(4) . . . . ? C3 C4 C5 C10 -115.8(3) . . . . ? C3 C4 C5 C6 60.7(4) . . . . ? C10 C5 C6 C7 0.6(4) . . . . ? C4 C5 C6 C7 -176.0(3) . . . . ? C5 C6 C7 C8 -2.3(4) . . . . ? C5 C6 C7 C14 174.4(3) . . . . ? C6 C7 C8 C9 3.5(4) . . . . ? C14 C7 C8 C9 -173.1(3) . . . . ? C6 C7 C8 Ag1 102.3(2) . . . . ? C14 C7 C8 Ag1 -74.4(3) . . . . ? Ag2 Ag1 C8 C9 -119.8(3) . . . . ? N1 Ag1 C8 C9 59.5(2) . . . . ? S3 Ag1 C8 C9 -33.3(2) . . . . ? S2 Ag1 C8 C9 154.58(18) . . . . ? Ag2 Ag1 C8 C7 118.6(3) . . . . ? N1 Ag1 C8 C7 -62.1(2) . . . . ? S3 Ag1 C8 C7 -154.94(18) . . . . ? S2 Ag1 C8 C7 33.0(2) . . . . ? C7 C8 C9 C10 -2.9(4) . . . . ? Ag1 C8 C9 C10 -100.7(3) . . . . ? C7 C8 C9 C24 174.8(3) . . . . ? Ag1 C8 C9 C24 77.1(3) . . . . ? C6 C5 C10 C9 0.1(4) . . . . ? C4 C5 C10 C9 176.6(3) . . . . ? C8 C9 C10 C5 1.1(4) . . . . ? C24 C9 C10 C5 -176.7(3) . . . . ? C21 N1 C11 C12 -162.2(3) . . . . ? C1 N1 C11 C12 73.3(3) . . . . ? Ag1 N1 C11 C12 -55.4(3) . . . . ? N1 C11 C12 S2 69.3(3) . . . . ? C13 S2 C12 C11 -141.7(2) . . . . ? Ag2 S2 C12 C11 -18.9(2) . . . . ? Ag1 S2 C12 C11 -36.7(2) . . . . ? C12 S2 C13 C14 141.1(2) . . . . ? Ag2 S2 C13 C14 27.8(3) . . . . ? Ag1 S2 C13 C14 41.0(3) . . . . ? C6 C7 C14 C13 -65.6(4) . . . . ? C8 C7 C14 C13 111.1(3) . . . . ? S2 C13 C14 C7 -75.6(3) . . . . ? C11 N1 C21 C22 160.0(3) . . . . ? C1 N1 C21 C22 -74.8(3) . . . . ? Ag1 N1 C21 C22 53.0(3) . . . . ? N1 C21 C22 S3 -72.9(3) . . . . ? C23 S3 C22 C21 150.2(2) . . . . ? Ag1 S3 C22 C21 42.6(2) . . . . ? Ag2 S3 C22 C21 25.4(2) . . . . ? C22 S3 C23 C24 -136.6(3) . . . . ? Ag1 S3 C23 C24 -38.3(3) . . . . ? Ag2 S3 C23 C24 -24.5(3) . . . . ? C10 C9 C24 C23 67.6(4) . . . . ? C8 C9 C24 C23 -110.2(4) . . . . ? S3 C23 C24 C9 71.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.648 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.081