Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_General _journal_coden_Cambridge 186 _audit_creation_date 'Thu Oct 4 20:37:48 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Dr. Tomoyuki Mochida ' _publ_contact_author_address ; Department of Chemistry, Faculty of Science, Toho University Miyama 2-2-1, Funabashi, Chiba, 274-8510, Japan ; _publ_contact_author_email ' mochida@chem.sci.toho-u.ac.jp ' _publ_contact_author_fax ' +81-47-472-4406 ' _publ_contact_author_phone ' +81-47-472-4406 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Dalton Trans.' _publ_requested_category ' FM ' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; Coordination polymer complexes of 4,4'-Dipyridyldisulfide and AgX (X=PF6-, C104-,OTs-,NO3-,BF4-) with twisted rhomboid network, 2-D sheet, and 1-D chain structures ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name 'Horikoshi, Ryo' 'Maki, Noriko' 'Mochida, Tomoyuki' 'Moriyama, Hiroshi' 'Yamada, Sachiko' _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_compound_3 _database_code_CSD 172107 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C17 H15 Ag N2 O3 S3 ' _chemical_formula_moiety 'C17 H15 Ag N2 O3 S3 ' _chemical_formula_weight 499.37 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.611(6) _cell_length_b 9.640(3) _cell_length_c 18.684(3) _cell_angle_alpha 90 _cell_angle_beta 94.06(2) _cell_angle_gamma 90 _cell_volume 1906(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.402 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.559 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 4888 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_theta_max 27.51 _diffrn_measured_fraction_theta_max 0.9984 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.9984 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.51 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4380 _reflns_number_gt 2630 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1123 _refine_ls_wR_factor_ref 0.3051 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4603 _refine_ls_number_parameters 235 _refine_ls_goodness_of_fit_ref 3.066 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0048 _refine_diff_density_max 3.08 _refine_diff_density_min -0.93 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag(1) Ag 0.3998(1) 0.39996(10) 0.02339(5) 0.0750(3) Uani 1.00 d . . . S(1) S 0.3100(4) 0.1385(4) 0.1199(2) 0.082(1) Uani 1.00 d . . . S(2) S 0.3996(4) 0.1990(3) 0.2114(2) 0.090(1) Uani 1.00 d . . . S(3) S -0.2189(3) 0.4844(3) 0.1175(2) 0.0674(9) Uani 1.00 d . . . O(1) O -0.189(1) 0.542(1) 0.1875(5) 0.098(3) Uani 1.00 d . . . O(2) O -0.3537(9) 0.468(1) 0.1022(6) 0.105(4) Uani 1.00 d . . . O(3) O -0.1577(9) 0.5566(9) 0.0622(5) 0.079(3) Uani 1.00 d . . . N(1) N 0.5130(10) -0.2378(9) 0.0373(5) 0.057(3) Uani 1.00 d . . . N(2) N 0.1808(9) 0.0142(8) 0.3910(5) 0.055(3) Uani 1.00 d . . . C(1) C 0.562(1) -0.180(1) 0.0943(6) 0.074(4) Uani 1.00 d . . . C(2) C 0.495(1) -0.065(1) 0.1283(6) 0.076(4) Uani 1.00 d . . . C(3) C 0.391(1) -0.017(1) 0.0901(7) 0.060(3) Uani 1.00 d . . . C(4) C 0.345(1) -0.073(1) 0.0334(8) 0.077(4) Uani 1.00 d . . . C(5) C 0.407(1) -0.181(1) 0.0081(7) 0.078(4) Uani 1.00 d . . . C(6) C 0.117(1) 0.059(1) 0.3313(7) 0.066(4) Uani 1.00 d . . . C(7) C 0.173(2) 0.115(1) 0.2737(6) 0.089(5) Uani 1.00 d . . . C(8) C 0.306(1) 0.122(1) 0.2778(6) 0.063(4) Uani 1.00 d . . . C(9) C 0.372(1) 0.077(1) 0.3383(9) 0.083(5) Uani 1.00 d . . . C(10) C 0.310(1) 0.026(1) 0.3927(7) 0.071(4) Uani 1.00 d . . . C(11) C -0.1540(10) 0.313(1) 0.1239(5) 0.057(3) Uani 1.00 d . . . C(12) C -0.073(1) 0.270(1) 0.0729(6) 0.060(3) Uani 1.00 d . . . C(13) C -0.029(1) 0.134(1) 0.0759(7) 0.067(4) Uani 1.00 d . . . C(14) C -0.064(1) 0.043(1) 0.1255(6) 0.067(4) Uani 1.00 d . . . C(15) C -0.015(2) -0.100(1) 0.1304(9) 0.113(6) Uani 1.00 d . . . C(16) C -0.146(2) 0.091(2) 0.1736(6) 0.086(5) Uani 1.00 d . . . C(17) C -0.192(1) 0.219(2) 0.1731(5) 0.079(4) Uani 1.00 d . . . H(1) H 0.6432 -0.2150 0.1160 0.0760 Uiso 1.00 calc . . . H(2) H 0.5214 -0.0266 0.1745 0.0760 Uiso 1.00 calc . . . H(3) H 0.2720 -0.0355 0.0078 0.0760 Uiso 1.00 calc . . . H(4) H 0.3740 -0.2223 -0.0374 0.0760 Uiso 1.00 calc . . . H(5) H 0.0275 0.0464 0.3271 0.0760 Uiso 1.00 calc . . . H(6) H 0.1268 0.1496 0.2326 0.0760 Uiso 1.00 calc . . . H(7) H 0.4616 0.0838 0.3400 0.0760 Uiso 1.00 calc . . . H(8) H 0.3573 -0.0020 0.4361 0.0760 Uiso 1.00 calc . . . H(9) H -0.0516 0.3339 0.0357 0.0760 Uiso 1.00 calc . . . H(10) H 0.0309 0.1061 0.0410 0.0760 Uiso 1.00 calc . . . H(11) H -0.0825 -0.1688 0.1258 0.0760 Uiso 1.00 calc . . . H(12) H 0.0414 -0.1196 0.0945 0.0760 Uiso 1.00 calc . . . H(13) H 0.0299 -0.1182 0.1768 0.0760 Uiso 1.00 calc . . . H(14) H -0.1757 0.0250 0.2088 0.0760 Uiso 1.00 calc . . . H(15) H -0.2532 0.2472 0.2068 0.0760 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0924(8) 0.0590(6) 0.0777(7) -0.0010(5) 0.0350(6) -0.0175(4) S(1) 0.099(3) 0.078(2) 0.069(2) 0.022(2) 0.011(2) 0.005(2) S(2) 0.135(3) 0.056(2) 0.083(2) -0.023(2) 0.036(2) -0.005(2) S(3) 0.059(2) 0.069(2) 0.073(2) 0.012(2) -0.001(1) -0.022(2) O(1) 0.110(8) 0.112(7) 0.074(6) 0.010(7) 0.018(5) -0.039(6) O(2) 0.055(6) 0.098(7) 0.159(10) 0.028(5) -0.012(6) -0.025(7) O(3) 0.091(6) 0.066(5) 0.080(6) 0.018(5) 0.008(5) -0.003(4) N(1) 0.070(6) 0.044(4) 0.057(5) 0.005(5) 0.011(5) -0.005(4) N(2) 0.068(6) 0.043(4) 0.055(5) -0.002(4) 0.012(5) 0.006(4) C(1) 0.095(10) 0.069(8) 0.057(7) -0.001(7) -0.003(7) -0.010(6) C(2) 0.10(1) 0.078(8) 0.046(6) -0.010(8) -0.005(7) -0.009(6) C(3) 0.054(7) 0.055(6) 0.073(7) 0.002(6) 0.009(6) 0.012(6) C(4) 0.063(8) 0.083(9) 0.084(9) 0.016(7) 0.005(7) -0.002(7) C(5) 0.083(10) 0.073(8) 0.080(9) -0.003(8) 0.022(8) -0.002(7) C(6) 0.065(8) 0.047(6) 0.086(9) -0.003(5) 0.013(7) -0.002(6) C(7) 0.17(2) 0.056(7) 0.039(6) 0.001(9) -0.022(8) 0.014(5) C(8) 0.089(9) 0.044(6) 0.061(7) -0.016(6) 0.034(7) -0.012(5) C(9) 0.078(9) 0.060(7) 0.12(1) -0.001(6) 0.042(9) 0.008(7) C(10) 0.068(8) 0.063(7) 0.083(8) 0.007(6) 0.017(7) 0.023(6) C(11) 0.039(6) 0.077(7) 0.054(6) 0.014(6) -0.008(5) -0.011(6) C(12) 0.051(6) 0.062(6) 0.066(7) 0.007(5) 0.001(5) 0.000(5) C(13) 0.061(7) 0.074(8) 0.068(7) 0.008(6) 0.013(6) -0.010(6) C(14) 0.070(8) 0.065(7) 0.065(7) 0.010(6) -0.012(6) 0.011(6) C(15) 0.18(2) 0.057(8) 0.10(1) 0.023(10) -0.02(1) 0.022(7) C(16) 0.10(1) 0.11(1) 0.050(7) 0.014(9) -0.006(7) 0.024(7) C(17) 0.10(1) 0.106(10) 0.028(5) 0.032(9) 0.008(6) 0.010(6) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag(1) Ag(1) 3.044(2) . 3_665 yes Ag(1) N(1) 2.175(8) . 3_655 yes Ag(1) N(2) 2.167(8) . 2_555 yes S(1) S(2) 1.984(6) . . yes S(1) C(3) 1.83(1) . . yes S(2) C(8) 1.80(1) . . yes S(3) O(1) 1.434(9) . . yes S(3) O(2) 1.447(10) . . yes S(3) O(3) 1.438(9) . . yes S(3) C(11) 1.79(1) . . yes N(1) C(1) 1.28(1) . . yes N(1) C(5) 1.33(2) . . yes N(2) C(6) 1.33(2) . . yes N(2) C(10) 1.37(2) . . yes C(1) C(2) 1.48(2) . . yes C(2) C(3) 1.35(2) . . yes C(3) C(4) 1.26(2) . . yes C(4) C(5) 1.33(2) . . yes C(6) C(7) 1.38(2) . . yes C(7) C(8) 1.41(2) . . yes C(8) C(9) 1.35(2) . . yes C(9) C(10) 1.34(2) . . yes C(11) C(12) 1.39(1) . . yes C(11) C(17) 1.37(2) . . yes C(12) C(13) 1.40(2) . . yes C(13) C(14) 1.35(2) . . yes C(14) C(15) 1.47(2) . . yes C(14) C(16) 1.38(2) . . yes C(16) C(17) 1.32(2) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag(1) Ag(1) N(1) 88.5(2) 3_665 3_655 0_555 yes Ag(1) Ag(1) N(2) 102.1(2) 3_665 2_555 0_555 yes N(1) Ag(1) N(2) 162.6(3) 3_655 2_555 0_555 yes S(2) S(1) C(3) 107.2(5) . . 0_555 yes S(1) S(2) C(8) 102.6(5) . . 0_555 yes O(1) S(3) O(2) 112.0(6) . . 0_555 yes O(1) S(3) O(3) 112.8(6) . . 0_555 yes O(1) S(3) C(11) 103.5(6) . . 0_555 yes O(2) S(3) O(3) 113.6(7) . . 0_555 yes O(2) S(3) C(11) 106.5(6) . . 0_555 yes O(3) S(3) C(11) 107.7(5) . . 0_555 yes Ag(1) N(1) C(1) 125.9(9) 3_655 . 0_555 yes Ag(1) N(1) C(5) 117.3(8) 3_655 . 0_555 yes C(1) N(1) C(5) 116(1) . . 0_555 yes Ag(1) N(2) C(6) 125.3(8) 2_545 . 0_555 yes Ag(1) N(2) C(10) 118.2(8) 2_545 . 0_555 yes C(6) N(2) C(10) 115.8(10) . . 0_555 yes N(1) C(1) C(2) 120(1) . . 0_555 yes C(1) C(2) C(3) 115(1) . . 0_555 yes S(1) C(3) C(2) 120(1) . . 0_555 yes S(1) C(3) C(4) 116(1) . . 0_555 yes C(2) C(3) C(4) 123(1) . . 0_555 yes C(3) C(4) C(5) 117(1) . . 0_555 yes N(1) C(5) C(4) 126(1) . . 0_555 yes N(2) C(6) C(7) 124(1) . . 0_555 yes C(6) C(7) C(8) 117(1) . . 0_555 yes S(2) C(8) C(7) 125(1) . . 0_555 yes S(2) C(8) C(9) 115(1) . . 0_555 yes C(7) C(8) C(9) 118(1) . . 0_555 yes C(8) C(9) C(10) 119(1) . . 0_555 yes N(2) C(10) C(9) 123(1) . . 0_555 yes S(3) C(11) C(12) 118.6(9) . . 0_555 yes S(3) C(11) C(17) 121.7(9) . . 0_555 yes C(12) C(11) C(17) 119(1) . . 0_555 yes C(11) C(12) C(13) 118(1) . . 0_555 yes C(12) C(13) C(14) 122(1) . . 0_555 yes C(13) C(14) C(15) 122(1) . . 0_555 yes C(13) C(14) C(16) 116(1) . . 0_555 yes C(15) C(14) C(16) 120(1) . . 0_555 yes C(14) C(16) C(17) 124(1) . . 0_555 yes C(11) C(17) C(16) 119(1) . . 0_555 yes #------------------------------------------------------------------------------ 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 Ag(1) N(1) C(1) C(2) -176.8(8) 0_555 19_1 5_555 55_5 yes Ag(1) N(1) C(5) C(4) 173(1) 0_555 19_1 5_555 55_5 yes Ag(1) N(2) C(6) C(7) -171.3(9) 0_555 19_1 5_555 55_5 yes Ag(1) N(2) C(10) C(9) 170.4(10) 0_555 19_1 5_555 55_5 yes S(1) S(2) C(8) C(7) -40(1) 0_555 19_1 5_555 55_5 yes S(1) S(2) C(8) C(9) 144.5(9) 0_555 19_1 5_555 55_5 yes S(1) C(3) C(2) C(1) -172.4(9) 0_555 19_1 5_555 55_5 yes S(1) C(3) C(4) C(5) 175(1) 0_555 19_1 5_555 55_5 yes S(2) S(1) C(3) C(2) -2(1) 0_555 19_1 5_555 55_5 yes S(2) S(1) C(3) C(4) 178.2(10) 0_555 19_1 5_555 55_5 yes S(2) C(8) C(7) C(6) -176.8(8) 0_555 19_1 5_555 55_5 yes S(2) C(8) C(9) C(10) 175.9(10) 0_555 19_1 5_555 55_5 yes S(3) C(11) C(12) C(13) -176.6(9) 0_555 19_1 5_555 55_5 yes S(3) C(11) C(17) C(16) 176(1) 0_555 19_1 5_555 55_5 yes O(1) S(3) C(11) C(12) -127.5(10) 0_555 19_1 5_555 55_5 yes O(1) S(3) C(11) C(17) 59(1) 0_555 19_1 5_555 55_5 yes O(2) S(3) C(11) C(12) 114(1) 0_555 19_1 5_555 55_5 yes O(2) S(3) C(11) C(17) -58(1) 0_555 19_1 5_555 55_5 yes O(3) S(3) C(11) C(12) -7(1) 0_555 19_1 5_555 55_5 yes O(3) S(3) C(11) C(17) 178(1) 0_555 19_1 5_555 55_5 yes N(1) C(1) C(2) C(3) -8(1) 0_555 19_1 5_555 55_5 yes N(1) C(5) C(4) C(3) 0(2) 0_555 19_1 5_555 55_5 yes N(2) C(6) C(7) C(8) 2(1) 0_555 19_1 5_555 55_5 yes N(2) C(10) C(9) C(8) 1(2) 0_555 19_1 5_555 55_5 yes C(1) N(1) C(5) C(4) -1(1) 0_555 19_1 5_555 55_5 yes C(1) C(2) C(3) C(4) 7(1) 0_555 19_1 5_555 55_5 yes C(2) C(1) N(1) C(5) 5(1) 0_555 19_1 5_555 55_5 yes C(2) C(3) C(4) C(5) -3(2) 0_555 19_1 5_555 55_5 yes C(3) S(1) S(2) C(8) -96.2(6) 0_555 19_1 5_555 55_5 yes C(6) N(2) C(10) C(9) 0(1) 0_555 19_1 5_555 55_5 yes C(6) C(7) C(8) C(9) -1(1) 0_555 19_1 5_555 55_5 yes C(7) C(6) N(2) C(10) 0(1) 0_555 19_1 5_555 55_5 yes C(7) C(8) C(9) C(10) 0(1) 0_555 19_1 5_555 55_5 yes C(11) C(12) C(13) C(14) 1(1) 0_555 19_1 5_555 55_5 yes C(11) C(17) C(16) C(14) -2(2) 0_555 19_1 5_555 55_5 yes C(12) C(11) C(17) C(16) 3(1) 0_555 19_1 5_555 55_5 yes C(12) C(13) C(14) C(15) -178(1) 0_555 19_1 5_555 55_5 yes C(12) C(13) C(14) C(16) 0(1) 0_555 19_1 5_555 55_5 yes C(13) C(12) C(11) C(17) -3(1) 0_555 19_1 5_555 55_5 yes C(13) C(14) C(16) C(17) 1(2) 0_555 19_1 5_555 55_5 yes C(15) C(14) C(16) C(17) 179(1) 0_555 19_1 5_555 55_5 yes C(15) C(14) C(16) C(17) 179(1) 0_555 19_1 5_555 55_5 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_compound_4 _database_code_CSD 172108 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C11 H9.50 Ag N3.50 O3 S2 ' _chemical_formula_moiety ' C11 H9.50 Ag N3.50 O3 S2 ' _chemical_formula_weight 410.71 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 4.957(2) _cell_length_b 19.291(3) _cell_length_c 15.335(2) _cell_angle_alpha 90 _cell_angle_beta 91.76(2) _cell_angle_gamma 90 _cell_volume 1465.6(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.861 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.667 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.885 _exptl_absorpt_correction_T_max 0.994 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3872 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 1.0000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.0000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.52 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -9.9 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2569 _reflns_number_gt 2084 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.2607 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2874 _refine_ls_number_parameters 173 _refine_ls_goodness_of_fit_ref 3.134 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0091 _refine_diff_density_max 2.09 _refine_diff_density_min -1.21 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag(1) Ag 0.4659(2) 0.26513(5) 0.35179(8) 0.0733(4) Uani 1.00 d . . . S(1) S 1.4272(6) 0.5079(1) 0.3804(2) 0.0572(8) Uani 1.00 d . . . S(2) S 1.5112(6) 0.5400(2) 0.2587(2) 0.0596(8) Uani 1.00 d . . . O(1) O 0.400(3) 0.2820(7) 0.5466(8) 0.126(5) Uani 1.00 d . . . O(2) O 0.454(3) 0.1983(7) 0.6371(6) 0.119(5) Uani 1.00 d . . . O(3) O 0.606(4) 0.1968(9) 0.513(1) 0.196(8) Uani 1.00 d . . . N(1) N 0.856(2) 0.6962(4) 0.1863(6) 0.053(3) Uani 1.00 d . . . N(2) N 0.780(2) 0.3410(4) 0.3576(6) 0.057(3) Uani 1.00 d . . . N(3) N 0.485(2) 0.2252(6) 0.5663(7) 0.071(4) Uani 1.00 d . . . N(4) N 0.8992 0.0766 0.5769 0.0760 Uiso 0.44 d P . . C(1) C 0.865(2) 0.3737(6) 0.2856(7) 0.056(3) Uani 1.00 d . . . C(2) C 1.058(2) 0.4247(5) 0.2878(6) 0.051(3) Uani 1.00 d . . . C(3) C 1.180(2) 0.4437(5) 0.3668(6) 0.045(3) Uani 1.00 d . . . C(4) C 1.102(2) 0.4082(6) 0.4414(6) 0.059(3) Uani 1.00 d . . . C(5) C 0.909(2) 0.3584(6) 0.4330(7) 0.060(3) Uani 1.00 d . . . C(6) C 0.958(3) 0.6920(5) 0.2658(7) 0.061(4) Uani 1.00 d . . . C(7) C 1.153(2) 0.6457(6) 0.2926(7) 0.064(4) Uani 1.00 d . . . C(8) C 1.253(2) 0.6020(5) 0.2333(7) 0.046(3) Uani 1.00 d . . . C(9) C 1.158(3) 0.6065(7) 0.1474(7) 0.071(4) Uani 1.00 d . . . C(10) C 0.964(3) 0.6532(7) 0.1280(7) 0.071(4) Uani 1.00 d . . . C(11) C 1.1431 0.0692 0.5673 0.0760 Uiso 0.44 d P . . C(12) C 1.4227 0.0392 0.5421 0.0760 Uiso 0.44 d P . . H(1) H 0.7833 0.3620 0.2308 0.0760 Uiso 1.00 calc . . . H(2) H 1.1098 0.4457 0.2354 0.0760 Uiso 1.00 calc . . . H(3) H 1.1788 0.4188 0.4972 0.0760 Uiso 1.00 calc . . . H(4) H 0.8596 0.3339 0.4839 0.0760 Uiso 1.00 calc . . . H(5) H 0.8893 0.7231 0.3079 0.0760 Uiso 1.00 calc . . . H(6) H 1.2169 0.6437 0.3513 0.0760 Uiso 1.00 calc . . . H(7) H 1.2298 0.5777 0.1036 0.0760 Uiso 1.00 calc . . . H(8) H 0.8976 0.6557 0.0693 0.0760 Uiso 1.00 calc . . . H(9) H 1.5614 0.0707 0.5597 0.0760 Uiso 0.45 calc P . . H(10) H 1.4513 -0.0040 0.5705 0.0760 Uiso 0.45 calc P . . H(11) H 1.4253 0.0328 0.4807 0.0760 Uiso 0.45 calc P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0516(6) 0.0508(6) 0.1177(10) -0.0100(4) 0.0027(5) -0.0138(5) S(1) 0.054(2) 0.054(2) 0.062(2) -0.013(1) -0.017(1) 0.012(1) S(2) 0.039(1) 0.059(2) 0.081(2) 0.003(1) 0.007(1) 0.021(1) O(1) 0.14(1) 0.117(9) 0.120(9) 0.049(9) 0.013(8) 0.036(7) O(2) 0.16(1) 0.13(1) 0.063(6) 0.049(9) 0.019(7) 0.035(6) O(3) 0.24(2) 0.19(2) 0.16(1) 0.08(2) 0.10(1) 0.05(1) N(1) 0.047(5) 0.050(5) 0.063(6) 0.003(4) 0.005(4) 0.016(4) N(2) 0.046(5) 0.045(5) 0.078(6) 0.003(4) 0.001(4) -0.001(4) N(3) 0.079(7) 0.080(7) 0.055(6) 0.012(6) 0.004(5) -0.010(6) C(1) 0.055(7) 0.059(7) 0.053(6) -0.005(5) -0.014(5) -0.005(5) C(2) 0.053(6) 0.054(6) 0.044(5) -0.008(5) -0.002(5) 0.002(4) C(3) 0.042(5) 0.041(5) 0.053(6) 0.006(4) -0.007(5) 0.000(4) C(4) 0.064(7) 0.069(7) 0.043(6) -0.016(6) -0.013(5) 0.010(5) C(5) 0.065(7) 0.057(6) 0.057(6) -0.009(6) 0.002(6) 0.015(5) C(6) 0.085(8) 0.039(6) 0.061(7) 0.008(6) 0.014(6) -0.003(5) C(7) 0.064(7) 0.072(8) 0.055(6) 0.010(6) -0.008(6) -0.004(6) C(8) 0.030(5) 0.036(5) 0.073(7) -0.002(4) 0.008(5) 0.008(5) C(9) 0.088(9) 0.081(8) 0.044(6) 0.025(7) 0.008(6) 0.000(5) C(10) 0.085(9) 0.085(9) 0.043(6) 0.031(8) -0.006(6) 0.003(6) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag(1) N(1) 2.139(9) . . yes Ag(1) N(2) 2.145(8) . 2_645 yes S(1) S(2) 2.022(4) . . yes S(1) C(3) 1.750(10) . . yes S(2) C(8) 1.786(10) . . yes O(1) N(3) 1.21(1) . . yes O(2) N(3) 1.22(1) . . yes O(3) N(3) 1.17(2) . . yes N(1) C(1) 1.35(1) . . yes N(1) C(5) 1.35(1) . . yes N(2) C(6) 1.31(1) . . yes N(2) C(10) 1.34(1) . . yes N(4) C(11) 1.2303(5) . . yes C(1) C(2) 1.37(1) . . yes C(2) C(3) 1.39(1) . . yes C(3) C(4) 1.40(1) . . yes C(4) C(5) 1.36(2) . . yes C(6) C(7) 1.37(2) . . yes C(7) C(8) 1.35(1) . . yes C(8) C(9) 1.39(2) . . yes C(9) C(10) 1.35(2) . . yes C(11) C(12) 1.5615(5) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ag(1) N(2) 166.2(4) . 2_645 0_555 yes S(2) S(1) C(3) 105.7(4) . . 0_555 yes S(1) S(2) C(8) 103.9(4) . . 0_555 yes Ag(1) N(1) C(1) 122.0(7) . . 0_555 yes Ag(1) N(1) C(5) 122.1(7) . . 0_555 yes C(1) N(1) C(5) 115.9(9) . . 0_555 yes Ag(1) N(2) C(6) 123.7(7) 2_655 . 0_555 yes Ag(1) N(2) C(10) 120.7(7) 2_655 . 0_555 yes C(6) N(2) C(10) 115.6(9) . . 0_555 yes O(1) N(3) O(2) 123(1) . . 0_555 yes O(1) N(3) O(3) 115(1) . . 0_555 yes O(2) N(3) O(3) 120(1) . . 0_555 yes N(1) C(1) C(2) 123.2(9) . . 0_555 yes C(1) C(2) C(3) 119.8(9) . . 0_555 yes S(1) C(3) C(2) 125.2(8) . . 0_555 yes S(1) C(3) C(4) 117.3(7) . . 0_555 yes C(2) C(3) C(4) 117.5(9) . . 0_555 yes C(3) C(4) C(5) 118.7(9) . . 0_555 yes N(1) C(5) C(4) 124.8(10) . . 0_555 yes N(2) C(6) C(7) 124(1) . . 0_555 yes C(6) C(7) C(8) 118(1) . . 0_555 yes S(2) C(8) C(7) 123.2(9) . . 0_555 yes S(2) C(8) C(9) 117.9(8) . . 0_555 yes C(7) C(8) C(9) 118.8(10) . . 0_555 yes C(8) C(9) C(10) 118(1) . . 0_555 yes N(2) C(10) C(9) 124(1) . . 0_555 yes N(4) C(11) C(12) 162.769(6) . . 0_555 yes #------------------------------------------------------------------------------ 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 Ag(1) N(1) C(1) C(2) 177.2(8) 0_555 62_1 5_555 55_5 yes Ag(1) N(1) C(5) C(4) -177.1(10) 0_555 62_1 5_555 55_5 yes S(1) S(2) C(8) C(7) 36.3(10) 0_555 62_1 5_555 55_5 yes S(1) S(2) C(8) C(9) -145.9(9) 0_555 62_1 5_555 55_5 yes S(1) C(3) C(2) C(1) -179.6(8) 0_555 62_1 5_555 55_5 yes S(1) C(3) C(4) C(5) 179.6(10) 0_555 62_1 5_555 55_5 yes S(2) S(1) C(3) C(2) -4.5(10) 0_555 62_1 5_555 55_5 yes S(2) S(1) C(3) C(4) 174.4(8) 0_555 62_1 5_555 55_5 yes S(2) C(8) C(7) C(6) 179.0(9) 0_555 62_1 5_555 55_5 yes S(2) C(8) C(9) C(10) -179(1) 0_555 62_1 5_555 55_5 yes N(1) C(1) C(2) C(3) 1(1) 0_555 62_1 5_555 55_5 yes N(1) C(5) C(4) C(3) -1(1) 0_555 62_1 5_555 55_5 yes N(2) C(6) C(7) C(8) 1(1) 0_555 62_1 5_555 55_5 yes N(2) C(10) C(9) C(8) 0(2) 0_555 62_1 5_555 55_5 yes C(1) N(1) C(5) C(4) 3(1) 0_555 62_1 5_555 55_5 yes C(1) C(2) C(3) C(4) 1(1) 0_555 62_1 5_555 55_5 yes C(2) C(1) N(1) C(5) -3(1) 0_555 62_1 5_555 55_5 yes C(2) C(3) C(4) C(5) -1(1) 0_555 62_1 5_555 55_5 yes C(3) S(1) S(2) C(8) 83.1(5) 0_555 62_1 5_555 55_5 yes C(6) N(2) C(10) C(9) 2(1) 0_555 62_1 5_555 55_5 yes C(6) C(7) C(8) C(9) 1(1) 0_555 62_1 5_555 55_5 yes C(7) C(6) N(2) C(10) -3(1) 0_555 62_1 5_555 55_5 yes C(7) C(8) C(9) C(10) -1(1) 0_555 62_1 5_555 55_5 yes C(7) C(8) C(9) C(10) -1(1) 0_555 62_1 5_555 55_5 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_compound_2 _database_code_CSD 172109 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C20 H16 Ag Cl N4 O4 S4 ' _chemical_formula_moiety 'C10 H8 Ag Cl N2 O2 S2 ' _chemical_formula_weight 647.93 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.739(3) _cell_length_b 19.527(1) _cell_length_c 11.208(1) _cell_angle_alpha 90 _cell_angle_beta 92.29(2) _cell_angle_gamma 90 _cell_volume 2348.4(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.362 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.952 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 2929 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0403 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0403 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 0.65 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2816 _reflns_number_gt 2554 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.1059 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2847 _refine_ls_number_parameters 155 _refine_ls_goodness_of_fit_ref 1.530 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0005 _refine_diff_density_max 0.60 _refine_diff_density_min -0.72 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag(1) Ag 0.0000 0.29506(1) 0.2500 0.01860(9) Uani 1.00 d S . . Cl(1) Cl 0.0000 0.36787(5) -0.2500 0.0161(2) Uani 1.00 d S . . S(1) S 0.38619(7) 0.48147(4) 0.62535(6) 0.0158(2) Uani 1.00 d . . . S(2) S 0.30037(7) 0.56990(4) 0.67125(6) 0.0172(2) Uani 1.00 d . . . O(1) O 0.0558(3) 0.4089(2) -0.1567(3) 0.0494(8) Uani 1.00 d . . . O(2) O 0.0948(2) 0.3250(1) -0.2992(2) 0.0278(6) Uani 1.00 d . . . N(1) N 0.4058(2) 0.7252(1) 0.3871(2) 0.0150(5) Uani 1.00 d . . . N(2) N 0.1270(2) 0.3573(1) 0.3769(2) 0.0152(6) Uani 1.00 d . . . C(1) C 0.2357(3) 0.3329(1) 0.4232(2) 0.0166(6) Uani 1.00 d . . . C(2) C 0.3134(3) 0.3699(1) 0.4993(2) 0.0157(6) Uani 1.00 d . . . C(3) C 0.2800(3) 0.4366(1) 0.5301(2) 0.0134(6) Uani 1.00 d . . . C(4) C 0.1683(3) 0.4624(1) 0.4829(2) 0.0136(6) Uani 1.00 d . . . C(5) C 0.0961(3) 0.4212(1) 0.4075(2) 0.0155(6) Uani 1.00 d . . . C(6) C 0.3687(2) 0.6616(1) 0.3563(2) 0.0145(6) Uani 1.00 d . . . C(7) C 0.3384(3) 0.6118(1) 0.4376(2) 0.0152(6) Uani 1.00 d . . . C(8) C 0.3437(2) 0.6286(1) 0.5585(2) 0.0143(6) Uani 1.00 d . . . C(9) C 0.3791(3) 0.6944(1) 0.5923(2) 0.0153(6) Uani 1.00 d . . . C(10) C 0.4098(3) 0.7408(1) 0.5041(3) 0.0150(6) Uani 1.00 d . . . H(1) H 0.2598 0.2877 0.4023 0.0760 Uiso 1.00 calc . . . H(2) H 0.3889 0.3504 0.5307 0.0760 Uiso 1.00 calc . . . H(3) H 0.1417 0.5077 0.5020 0.0760 Uiso 1.00 calc . . . H(4) H 0.0197 0.4394 0.3755 0.0760 Uiso 1.00 calc . . . H(5) H 0.3631 0.6503 0.2731 0.0760 Uiso 1.00 calc . . . H(6) H 0.3144 0.5671 0.4121 0.0760 Uiso 1.00 calc . . . H(7) H 0.3819 0.7076 0.6736 0.0760 Uiso 1.00 calc . . . H(8) H 0.4349 0.7858 0.5278 0.0760 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0271(2) 0.0126(2) 0.0157(2) 0.0000 -0.0040(1) 0.0000 Cl(1) 0.0146(4) 0.0158(4) 0.0177(4) 0.0000 -0.0023(3) 0.0000 S(1) 0.0154(3) 0.0162(3) 0.0154(3) -0.0014(3) -0.0037(3) 0.0010(2) S(2) 0.0221(4) 0.0173(3) 0.0127(3) -0.0036(3) 0.0046(3) -0.0027(2) O(1) 0.028(1) 0.058(2) 0.061(2) -0.006(1) -0.002(1) -0.046(2) O(2) 0.023(1) 0.031(1) 0.030(1) 0.0031(10) 0.0056(10) -0.0091(10) N(1) 0.014(1) 0.013(1) 0.018(1) -0.0007(9) -0.0001(9) -0.0008(9) N(2) 0.017(1) 0.014(1) 0.015(1) -0.0032(9) 0.0022(9) 0.0010(9) C(1) 0.022(1) 0.012(1) 0.015(1) 0.002(1) 0.004(1) 0.0026(10) C(2) 0.016(1) 0.016(1) 0.016(1) 0.004(1) 0.001(1) 0.003(1) C(3) 0.014(1) 0.015(1) 0.011(1) -0.002(1) 0.0028(10) 0.0015(10) C(4) 0.012(1) 0.013(1) 0.016(1) 0.0011(10) 0.004(1) -0.0009(9) C(5) 0.012(1) 0.019(1) 0.016(1) 0.002(1) 0.001(1) 0.0003(10) C(6) 0.012(1) 0.017(1) 0.014(1) -0.002(1) -0.0012(10) -0.002(1) C(7) 0.014(1) 0.014(1) 0.018(1) -0.003(1) 0.000(1) -0.003(1) C(8) 0.010(1) 0.017(1) 0.016(1) 0.000(1) 0.0006(10) -0.0012(10) C(9) 0.013(1) 0.018(1) 0.014(1) 0.000(1) 0.001(1) -0.005(1) C(10) 0.016(1) 0.011(1) 0.018(1) 0.0003(10) -0.001(1) -0.0029(10) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag(1) N(1) 2.282(2) . . yes Ag(1) N(1) 2.282(2) . 2_555 yes Ag(1) N(2) 2.318(2) . 5_445 yes Ag(1) N(2) 2.318(2) . 6_545 yes Cl(1) O(1) 1.430(2) . . yes Cl(1) O(1) 1.430(2) . 2_554 yes Cl(1) O(2) 1.444(2) . . yes Cl(1) O(2) 1.444(2) . 2_554 yes S(1) S(2) 2.033(1) . . yes S(1) C(3) 1.764(3) . . yes S(2) C(8) 1.782(3) . . yes N(1) C(1) 1.345(4) . . yes N(1) C(5) 1.338(4) . . yes N(2) C(6) 1.344(4) . . yes N(2) C(10) 1.346(4) . . yes C(1) C(2) 1.375(4) . . yes C(2) C(3) 1.398(4) . . yes C(3) C(4) 1.387(4) . . yes C(4) C(5) 1.383(4) . . yes C(6) C(7) 1.380(4) . . yes C(7) C(8) 1.393(4) . . yes C(8) C(9) 1.388(4) . . yes C(9) C(10) 1.390(4) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ag(1) N(1) 115.6(1) . 2_555 0_555 yes N(1) Ag(1) N(2) 99.56(8) . 5_445 0_555 yes N(1) Ag(1) N(2) 117.47(8) . 6_545 0_555 yes N(1) Ag(1) N(2) 117.47(8) 2_555 5_445 0_555 yes N(1) Ag(1) N(2) 99.56(8) 2_555 6_545 0_555 yes N(2) Ag(1) N(2) 107.8(1) 5_445 6_545 0_555 yes O(1) Cl(1) O(1) 111.8(3) . 2_554 0_555 yes O(1) Cl(1) O(2) 108.9(1) . . 0_555 yes O(1) Cl(1) O(2) 109.1(2) . 2_554 0_555 yes O(1) Cl(1) O(2) 109.1(2) 2_554 . 0_555 yes O(1) Cl(1) O(2) 108.9(1) 2_554 2_554 0_555 yes O(2) Cl(1) O(2) 109.1(2) . 2_554 0_555 yes S(2) S(1) C(3) 106.65(10) . . 0_555 yes S(1) S(2) C(8) 103.45(9) . . 0_555 yes Ag(1) N(1) C(1) 122.6(2) . . 0_555 yes Ag(1) N(1) C(5) 120.5(2) . . 0_555 yes C(1) N(1) C(5) 116.9(2) . . 0_555 yes Ag(1) N(2) C(6) 120.4(2) 5_555 . 0_555 yes Ag(1) N(2) C(10) 121.0(2) 5_555 . 0_555 yes C(6) N(2) C(10) 117.2(2) . . 0_555 yes N(1) C(1) C(2) 123.3(3) . . 0_555 yes C(1) C(2) C(3) 119.2(3) . . 0_555 yes S(1) C(3) C(2) 116.5(2) . . 0_555 yes S(1) C(3) C(4) 125.4(2) . . 0_555 yes C(2) C(3) C(4) 118.1(2) . . 0_555 yes C(3) C(4) C(5) 118.5(2) . . 0_555 yes N(1) C(5) C(4) 124.1(3) . . 0_555 yes N(2) C(6) C(7) 123.8(2) . . 0_555 yes C(6) C(7) C(8) 118.4(2) . . 0_555 yes S(2) C(8) C(7) 122.5(2) . . 0_555 yes S(2) C(8) C(9) 118.5(2) . . 0_555 yes C(7) C(8) C(9) 118.9(3) . . 0_555 yes C(8) C(9) C(10) 118.6(2) . . 0_555 yes N(2) C(10) C(9) 123.0(3) . . 0_555 yes #------------------------------------------------------------------------------ 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 Ag(1) N(1) C(1) C(2) 179.7(2) 0_555 23_1 5_555 55_5 yes Ag(1) N(1) C(5) C(4) -179.4(2) 0_555 23_1 5_555 55_5 yes Ag(1) N(1) C(1) C(2) 179.7(2) 0_555 23_1 5_555 55_5 yes Ag(1) N(1) C(5) C(4) -179.4(2) 0_555 23_1 5_555 55_5 yes S(1) S(2) C(8) C(7) 46.1(2) 0_555 23_1 5_555 55_5 yes S(1) S(2) C(8) C(9) -136.8(2) 0_555 23_1 5_555 55_5 yes S(1) C(3) C(2) C(1) -178.6(2) 0_555 23_1 5_555 55_5 yes S(1) C(3) C(4) C(5) 178.8(2) 0_555 23_1 5_555 55_5 yes S(2) S(1) C(3) C(2) -172.1(2) 0_555 23_1 5_555 55_5 yes S(2) S(1) C(3) C(4) 8.7(3) 0_555 23_1 5_555 55_5 yes S(2) C(8) C(7) C(6) 177.2(2) 0_555 23_1 5_555 55_5 yes S(2) C(8) C(9) C(10) -178.4(2) 0_555 23_1 5_555 55_5 yes N(1) Ag(1) N(1) C(1) -154.2(2) 0_555 23_1 5_555 55_5 yes N(1) Ag(1) N(1) C(5) 24.9(2) 0_555 23_1 5_555 55_5 yes N(1) C(1) C(2) C(3) -0.8(4) 0_555 23_1 5_555 55_5 yes N(1) C(5) C(4) C(3) 0.2(4) 0_555 23_1 5_555 55_5 yes N(2) Ag(1) N(2) C(6) -26.2(2) 0_555 23_1 5_555 55_5 yes N(2) Ag(1) N(2) C(10) 139.9(2) 0_555 23_1 5_555 55_5 yes N(2) C(6) C(7) C(8) 1.4(4) 0_555 23_1 5_555 55_5 yes N(2) C(10) C(9) C(8) 0.7(4) 0_555 23_1 5_555 55_5 yes C(1) N(1) C(5) C(4) -0.3(4) 0_555 23_1 5_555 55_5 yes C(1) C(2) C(3) C(4) 0.6(4) 0_555 23_1 5_555 55_5 yes C(2) C(1) N(1) C(5) 0.6(4) 0_555 23_1 5_555 55_5 yes C(2) C(3) C(4) C(5) -0.3(4) 0_555 23_1 5_555 55_5 yes C(3) S(1) S(2) C(8) -90.3(1) 0_555 23_1 5_555 55_5 yes C(6) N(2) C(10) C(9) 0.7(4) 0_555 23_1 5_555 55_5 yes C(6) C(7) C(8) C(9) 0.1(4) 0_555 23_1 5_555 55_5 yes C(7) C(6) N(2) C(10) -1.8(4) 0_555 23_1 5_555 55_5 yes C(7) C(8) C(9) C(10) -1.1(4) 0_555 23_1 5_555 55_5 yes C(7) C(8) C(9) C(10) -1.1(4) 0_555 23_1 5_555 55_5 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_compound_1 _database_code_CSD 172110 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C20 H16 Ag F6 N4 P S4 ' _chemical_formula_moiety 'C10 H8 Ag F3 N2 P S2 ' _chemical_formula_weight 693.45 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.068(6) _cell_length_b 19.811(5) _cell_length_c 11.485(6) _cell_angle_alpha 90 _cell_angle_beta 95.30(4) _cell_angle_gamma 90 _cell_volume 2507(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.262 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.749 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3121 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 1.0381 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.0381 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.94 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2999 _reflns_number_gt 2149 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1196 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3032 _refine_ls_number_parameters 164 _refine_ls_goodness_of_fit_ref 1.376 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0005 _refine_diff_density_max 0.72 _refine_diff_density_min -0.72 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag(1) Ag 1.0000 0.20834(2) 0.7500 0.0643(1) Uani 1.00 d S . . S(1) S 0.7990(1) 0.42786(5) 1.15373(8) 0.0584(3) Uani 1.00 d . . . S(2) S 0.88140(9) 0.51570(5) 1.11675(8) 0.0535(3) Uani 1.00 d . . . P(1) P 0.5000 0.38390(6) 0.7500 0.0437(3) Uani 1.00 d S . . F(1) F 0.5478(2) 0.3848(1) 0.8859(2) 0.0653(7) Uani 1.00 d . . . F(2) F 0.5962(3) 0.4410(1) 0.7268(2) 0.0773(8) Uani 1.00 d . . . F(3) F 0.5956(3) 0.3276(1) 0.7262(2) 0.0855(9) Uani 1.00 d . . . N(1) N 0.9112(3) 0.2791(1) 0.8803(3) 0.0487(8) Uani 1.00 d . . . N(2) N 0.8728(3) 0.1416(1) 0.6299(2) 0.0478(8) Uani 1.00 d . . . C(1) C 0.9137(4) 0.2631(2) 0.9940(4) 0.055(1) Uani 1.00 d . . . C(2) C 0.8799(4) 0.3075(2) 1.0785(3) 0.055(1) Uani 1.00 d . . . C(3) C 0.8444(3) 0.3717(2) 1.0455(3) 0.0440(9) Uani 1.00 d . . . C(4) C 0.8413(3) 0.3892(2) 0.9279(3) 0.0464(9) Uani 1.00 d . . . C(5) C 0.8745(3) 0.3418(2) 0.8502(3) 0.0475(9) Uani 1.00 d . . . C(6) C 0.7651(4) 0.1638(2) 0.5813(3) 0.054(1) Uani 1.00 d . . . C(7) C 0.6889(3) 0.1256(2) 0.5063(3) 0.0503(10) Uani 1.00 d . . . C(8) C 0.7230(3) 0.0605(2) 0.4795(3) 0.0396(8) Uani 1.00 d . . . C(9) C 0.8331(3) 0.0368(1) 0.5294(3) 0.0405(8) Uani 1.00 d . . . C(10) C 0.9038(3) 0.0788(2) 0.6025(3) 0.0437(9) Uani 1.00 d . . . H(1) H 0.9397 0.2186 1.0171 0.0760 Uiso 1.00 calc . . . H(2) H 0.8828 0.2933 1.1580 0.0760 Uiso 1.00 calc . . . H(3) H 0.8168 0.4332 0.9019 0.0760 Uiso 1.00 calc . . . H(4) H 0.8713 0.3532 0.7683 0.0760 Uiso 1.00 calc . . . H(5) H 0.7415 0.2092 0.5996 0.0760 Uiso 1.00 calc . . . H(6) H 0.6131 0.1445 0.4724 0.0760 Uiso 1.00 calc . . . H(7) H 0.8594 -0.0079 0.5131 0.0760 Uiso 1.00 calc . . . H(8) H 0.9807 0.0624 0.6364 0.0760 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag(1) 0.0860(4) 0.0405(2) 0.0633(3) 0.0000 -0.0100(2) 0.0000 S(1) 0.0716(7) 0.0640(6) 0.0422(5) 0.0153(5) 0.0185(4) 0.0115(4) S(2) 0.0520(5) 0.0579(5) 0.0485(5) 0.0069(4) -0.0073(4) -0.0052(4) P(1) 0.0531(7) 0.0377(6) 0.0405(6) 0.0000 0.0051(5) 0.0000 F(1) 0.085(2) 0.068(1) 0.042(1) -0.005(1) -0.002(1) 0.0051(10) F(2) 0.096(2) 0.079(2) 0.060(1) -0.036(1) 0.020(1) 0.001(1) F(3) 0.089(2) 0.077(2) 0.090(2) 0.039(1) 0.001(2) -0.014(1) N(1) 0.047(2) 0.039(1) 0.058(2) 0.003(1) 0.000(1) 0.002(1) N(2) 0.056(2) 0.041(1) 0.047(1) -0.005(1) 0.006(1) 0.004(1) C(1) 0.059(2) 0.041(2) 0.065(2) 0.003(2) 0.005(2) 0.016(2) C(2) 0.059(2) 0.056(2) 0.049(2) 0.003(2) 0.005(2) 0.017(2) C(3) 0.038(2) 0.050(2) 0.045(2) 0.005(1) 0.008(1) 0.009(1) C(4) 0.049(2) 0.046(2) 0.045(2) 0.013(1) 0.005(1) 0.012(1) C(5) 0.048(2) 0.052(2) 0.043(2) 0.010(1) 0.002(1) 0.007(1) C(6) 0.067(2) 0.039(2) 0.057(2) 0.009(2) 0.007(2) 0.006(2) C(7) 0.047(2) 0.050(2) 0.052(2) 0.006(2) -0.001(2) 0.008(2) C(8) 0.040(2) 0.045(2) 0.035(2) -0.004(1) 0.007(1) 0.006(1) C(9) 0.042(2) 0.039(2) 0.041(2) -0.002(1) 0.007(1) 0.002(1) C(10) 0.041(2) 0.049(2) 0.042(2) -0.003(1) 0.006(1) 0.004(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag(1) N(1) 2.333(3) . . yes Ag(1) N(1) 2.333(3) . 2_756 yes Ag(1) N(2) 2.297(3) . . yes Ag(1) N(2) 2.297(3) . 2_756 yes S(1) S(2) 2.028(2) . . yes S(1) C(3) 1.776(4) . . yes S(2) C(8) 1.763(3) . 6_656 yes P(1) F(1) 1.601(2) . . yes P(1) F(1) 1.601(2) . 2_656 yes P(1) F(2) 1.592(2) . . yes P(1) F(2) 1.592(2) . 2_656 yes P(1) F(3) 1.579(2) . . yes P(1) F(3) 1.579(2) . 2_656 yes N(1) C(1) 1.341(5) . . yes N(1) C(5) 1.342(4) . . yes N(2) C(6) 1.343(5) . . yes N(2) C(10) 1.336(4) . . yes C(1) C(2) 1.388(6) . . yes C(2) C(3) 1.373(5) . . yes C(3) C(4) 1.391(4) . . yes C(4) C(5) 1.370(5) . . yes C(6) C(7) 1.375(5) . . yes C(7) C(8) 1.386(4) . . yes C(8) C(9) 1.381(4) . . yes C(9) C(10) 1.374(5) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Ag(1) N(1) 106.1(1) . 2_756 0_555 yes N(1) Ag(1) N(2) 117.4(1) . . 0_555 yes N(1) Ag(1) N(2) 103.42(10) . 2_756 0_555 yes N(1) Ag(1) N(2) 103.42(10) 2_756 . 0_555 yes N(1) Ag(1) N(2) 117.4(1) 2_756 2_756 0_555 yes N(2) Ag(1) N(2) 109.7(1) . 2_756 0_555 yes S(2) S(1) C(3) 103.3(1) . . 0_555 yes S(1) S(2) C(8) 106.4(1) . 6_656 0_555 yes F(1) P(1) F(1) 178.8(2) . 2_656 0_555 yes F(1) P(1) F(2) 89.4(1) . . 0_555 yes F(1) P(1) F(2) 89.7(1) . 2_656 0_555 yes F(1) P(1) F(3) 90.6(1) . . 0_555 yes F(1) P(1) F(3) 90.3(1) . 2_656 0_555 yes F(1) P(1) F(2) 89.7(1) 2_656 . 0_555 yes F(1) P(1) F(2) 89.4(1) 2_656 2_656 0_555 yes F(1) P(1) F(3) 90.3(1) 2_656 . 0_555 yes F(1) P(1) F(3) 90.6(1) 2_656 2_656 0_555 yes F(2) P(1) F(2) 89.5(2) . 2_656 0_555 yes F(2) P(1) F(3) 90.2(2) . . 0_555 yes F(2) P(1) F(3) 179.6(1) . 2_656 0_555 yes F(2) P(1) F(3) 179.6(1) 2_656 . 0_555 yes F(2) P(1) F(3) 90.2(2) 2_656 2_656 0_555 yes F(3) P(1) F(3) 90.1(2) . 2_656 0_555 yes Ag(1) N(1) C(1) 120.7(2) . . 0_555 yes Ag(1) N(1) C(5) 121.7(2) . . 0_555 yes C(1) N(1) C(5) 116.7(3) . . 0_555 yes Ag(1) N(2) C(6) 122.2(2) . . 0_555 yes Ag(1) N(2) C(10) 121.4(2) . . 0_555 yes C(6) N(2) C(10) 116.4(3) . . 0_555 yes N(1) C(1) C(2) 123.2(3) . . 0_555 yes C(1) C(2) C(3) 118.9(3) . . 0_555 yes S(1) C(3) C(2) 118.6(3) . . 0_555 yes S(1) C(3) C(4) 122.7(3) . . 0_555 yes C(2) C(3) C(4) 118.7(3) . . 0_555 yes C(3) C(4) C(5) 118.5(3) . . 0_555 yes N(1) C(5) C(4) 124.0(3) . . 0_555 yes N(2) C(6) C(7) 123.3(3) . . 0_555 yes C(6) C(7) C(8) 119.2(3) . . 0_555 yes S(2) C(8) C(7) 115.6(2) 6_646 . 0_555 yes S(2) C(8) C(9) 126.2(3) 6_646 . 0_555 yes C(7) C(8) C(9) 118.2(3) . . 0_555 yes C(8) C(9) C(10) 118.6(3) . . 0_555 yes N(2) C(10) C(9) 124.3(3) . . 0_555 yes #------------------------------------------------------------------------------ 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 Ag(1) N(1) C(1) C(2) 169.5(3) 0_555 24_1 5_555 55_5 yes Ag(1) N(1) C(5) C(4) -168.4(3) 0_555 24_1 5_555 55_5 yes Ag(1) N(1) C(1) C(2) 169.5(3) 0_555 24_1 5_555 55_5 yes Ag(1) N(1) C(5) C(4) -168.4(3) 0_555 24_1 5_555 55_5 yes Ag(1) N(2) C(6) C(7) 177.9(3) 0_555 24_1 5_555 55_5 yes Ag(1) N(2) C(10) C(9) -178.6(2) 0_555 24_1 5_555 55_5 yes Ag(1) N(2) C(6) C(7) 177.9(3) 0_555 24_1 5_555 55_5 yes Ag(1) N(2) C(10) C(9) -178.6(2) 0_555 24_1 5_555 55_5 yes S(1) C(3) C(2) C(1) 179.0(3) 0_555 24_1 5_555 55_5 yes S(1) C(3) C(4) C(5) -178.0(3) 0_555 24_1 5_555 55_5 yes S(2) S(1) C(3) C(2) 136.4(3) 0_555 24_1 5_555 55_5 yes S(2) S(1) C(3) C(4) -45.9(3) 0_555 24_1 5_555 55_5 yes N(1) Ag(1) N(1) C(1) -142.2(3) 0_555 24_1 5_555 55_5 yes N(1) Ag(1) N(1) C(5) 26.4(2) 0_555 24_1 5_555 55_5 yes N(1) Ag(1) N(2) C(6) 38.8(3) 0_555 24_1 5_555 55_5 yes N(1) Ag(1) N(2) C(10) -142.8(2) 0_555 24_1 5_555 55_5 yes N(1) Ag(1) N(2) C(6) -77.6(3) 0_555 24_1 5_555 55_5 yes N(1) Ag(1) N(2) C(10) 100.8(3) 0_555 24_1 5_555 55_5 yes N(1) C(1) C(2) C(3) -1.4(6) 0_555 24_1 5_555 55_5 yes N(1) C(5) C(4) C(3) -0.6(6) 0_555 24_1 5_555 55_5 yes N(2) Ag(1) N(1) C(1) 102.9(3) 0_555 24_1 5_555 55_5 yes N(2) Ag(1) N(1) C(5) -88.6(3) 0_555 24_1 5_555 55_5 yes N(2) Ag(1) N(1) C(1) -18.0(3) 0_555 24_1 5_555 55_5 yes N(2) Ag(1) N(1) C(5) 150.5(3) 0_555 24_1 5_555 55_5 yes N(2) Ag(1) N(2) C(6) 156.4(3) 0_555 24_1 5_555 55_5 yes N(2) Ag(1) N(2) C(10) -25.2(2) 0_555 24_1 5_555 55_5 yes N(2) C(6) C(7) C(8) 0.7(6) 0_555 24_1 5_555 55_5 yes N(2) C(10) C(9) C(8) 0.5(5) 0_555 24_1 5_555 55_5 yes C(1) N(1) C(5) C(4) 0.6(5) 0_555 24_1 5_555 55_5 yes C(1) C(2) C(3) C(4) 1.3(6) 0_555 24_1 5_555 55_5 yes C(2) C(1) N(1) C(5) 0.4(6) 0_555 24_1 5_555 55_5 yes C(2) C(3) C(4) C(5) -0.3(5) 0_555 24_1 5_555 55_5 yes C(3) S(1) S(2) C(8) 91.4(2) 0_555 24_1 5_555 55_5 yes C(6) N(2) C(10) C(9) -0.1(5) 0_555 24_1 5_555 55_5 yes C(6) C(7) C(8) C(9) -0.2(5) 0_555 24_1 5_555 55_5 yes C(7) C(6) N(2) C(10) -0.5(5) 0_555 24_1 5_555 55_5 yes C(7) C(8) C(9) C(10) -0.4(5) 0_555 24_1 5_555 55_5 yes C(7) C(8) C(9) C(10) -0.4(5) 0_555 24_1 5_555 55_5 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag #------------------------------------------------------------------------------ #------------------------------------------------------------------------------