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 'Schroder, Martin' 'Blake, Alexander J.' 'Brammer, L.' 'Brooks, Neil R.' 'Champness, Neil' 'Cunningham, John W.' 'Hubberstey, Peter' 'Rodger, Colin S.' 'Teat, Simon J.' 'Wilson, Claire' _publ_contact_author_name 'Prof Martin Schroder' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham Notts NG7 2RD UNITED KINGDOM ; _publ_contact_author_email 'M.SCHRODER@NOTTINGHAM.AC.UK' _publ_section_title ; Bridging mode flexibility of 1,3-dithiacyclohexane in silver(I) co-ordination polymers ; data_14no22 _database_code_CSD 187162 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3-dithiacyclohexane silver(I) nitrate ; _chemical_name_common [Ag(1,3-[6]aneS2)NO3] _chemical_formula_moiety 'C4 H8 Ag N O3 S2' _chemical_formula_sum 'C4 H8 Ag N O3 S2' _chemical_formula_weight 290.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 6.8622(4) _cell_length_b 7.9021(5) _cell_length_c 15.9619(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.1210(10) _cell_angle_gamma 90.00 _cell_volume 865.54(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7530 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 28.79 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 2.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.320 _exptl_absorpt_correction_T_max 0.492 _exptl_absorpt_process_details 'SADABS (Bruker, 1999b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 8776 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.0081 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 28.80 _reflns_number_total 2066 _reflns_number_gt 2058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999a)' _computing_data_reduction 'SAINT (Bruker, 1999a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _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 w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+3.121P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0374(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2066 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 1.320 _refine_ls_restrained_S_all 1.320 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.21563(4) -0.01404(4) -0.003086(16) 0.02216(12) Uani 1 1 d . . . S1 S 0.21293(13) 0.05481(13) -0.15231(5) 0.0243(2) Uani 1 1 d . . . C2 C -0.0231(6) 0.0111(5) -0.1967(2) 0.0257(8) Uani 1 1 d . . . H2A H -0.0426 -0.1130 -0.1974 0.031 Uiso 1 1 calc R . . H2B H -0.0238 0.0505 -0.2556 0.031 Uiso 1 1 calc R . . S3 S -0.22678(13) 0.10681(13) -0.14320(6) 0.0242(2) Uani 1 1 d . . . C4 C -0.1551(6) 0.3277(6) -0.1444(3) 0.0358(10) Uani 1 1 d . . . H4A H -0.1538 0.3673 -0.2033 0.043 Uiso 1 1 calc R . . H4B H -0.2551 0.3942 -0.1143 0.043 Uiso 1 1 calc R . . C5 C 0.0421(7) 0.3649(5) -0.1055(3) 0.0361(9) Uani 1 1 d . . . H5A H 0.0437 0.3220 -0.0472 0.043 Uiso 1 1 calc R . . H5B H 0.0616 0.4890 -0.1034 0.043 Uiso 1 1 calc R . . C6 C 0.2099(6) 0.2851(6) -0.1537(3) 0.0324(9) Uani 1 1 d . . . H6A H 0.3342 0.3269 -0.1299 0.039 Uiso 1 1 calc R . . H6B H 0.2031 0.3235 -0.2127 0.039 Uiso 1 1 calc R . . N1 N 0.4693(5) 0.2802(4) 0.0847(2) 0.0269(7) Uani 1 1 d . . . O1 O 0.4813(4) 0.2096(4) 0.01294(17) 0.0273(6) Uani 1 1 d . . . O2 O 0.3085(5) 0.2833(4) 0.1213(2) 0.0417(8) Uani 1 1 d . . . O3 O 0.6172(6) 0.3420(6) 0.1170(2) 0.0559(11) 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 0.01936(17) 0.02869(18) 0.01844(16) 0.00170(10) 0.00130(9) 0.00005(10) S1 0.0206(4) 0.0345(5) 0.0177(4) 0.0002(3) 0.0027(3) -0.0011(4) C2 0.0253(18) 0.037(2) 0.0146(15) -0.0019(14) -0.0010(13) -0.0046(15) S3 0.0202(4) 0.0314(5) 0.0209(4) 0.0031(3) -0.0007(3) -0.0017(3) C4 0.031(2) 0.029(2) 0.047(2) 0.0126(18) -0.0043(18) 0.0024(17) C5 0.041(2) 0.0209(19) 0.046(2) 0.0047(17) -0.0045(19) -0.0038(17) C6 0.0284(19) 0.036(2) 0.032(2) 0.0108(17) -0.0039(16) -0.0116(17) N1 0.0301(16) 0.0200(15) 0.0307(16) -0.0051(13) 0.0059(13) -0.0029(13) O1 0.0271(13) 0.0299(14) 0.0250(13) -0.0069(11) 0.0006(11) 0.0001(11) O2 0.0388(17) 0.0374(17) 0.0489(19) -0.0078(15) 0.0200(15) 0.0023(14) O3 0.049(2) 0.069(3) 0.050(2) -0.0280(19) 0.0064(17) -0.030(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 2.551(3) . y Ag1 O1 2.596(3) 3_655 y Ag1 S1 2.4433(9) . y Ag1 S3 2.4484(9) 3 y Ag1 Ag1 2.9695(6) 3 y S1 C2 1.800(4) . ? S1 C6 1.820(5) . ? C2 S3 1.805(4) . ? S3 C4 1.814(5) . ? S3 Ag1 2.4484(9) 3 ? C4 C5 1.517(6) . ? C5 C6 1.523(7) . ? N1 O3 1.238(5) . ? N1 O2 1.250(5) . ? N1 O1 1.277(4) . ? O1 Ag1 2.596(3) 3_655 ? 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 Ag1 S3 175.24(4) . 3 y S1 Ag1 O1 86.99(7) . . y S3 Ag1 O1 95.21(7) 3 . y S1 Ag1 O1 94.47(6) . 3_655 y S3 Ag1 O1 81.73(7) 3 3_655 y O1 Ag1 O1 81.13(10) . 3_655 y S1 Ag1 Ag1 90.58(2) . 3 y S3 Ag1 Ag1 91.14(2) 3 3 y O1 Ag1 Ag1 131.06(6) . 3 y O1 Ag1 Ag1 147.69(7) 3_655 3 y C2 S1 C6 100.16(19) . . ? C2 S1 Ag1 110.25(12) . . ? C6 S1 Ag1 103.58(14) . . ? S1 C2 S3 115.5(2) . . ? C2 S3 C4 100.8(2) . . ? C2 S3 Ag1 107.65(13) . 3 ? C4 S3 Ag1 106.89(16) . 3 ? C5 C4 S3 115.1(3) . . ? C4 C5 C6 112.8(4) . . ? C5 C6 S1 114.6(3) . . ? O3 N1 O2 121.4(4) . . ? O3 N1 O1 119.4(3) . . ? O2 N1 O1 119.1(3) . . ? N1 O1 Ag1 110.2(2) . . ? N1 O1 Ag1 111.6(2) . 3_655 ? Ag1 O1 Ag1 98.87(10) . 3_655 ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.57 _refine_diff_density_min -0.58 _refine_diff_density_rms 0.114 # Supporting information for crystal structure of [Ag(1,3-dithiane)]NO3 data_l14300s _database_code_CSD 187163 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Ag N O3 S2' _chemical_formula_weight 290.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 6.9178(12) _cell_length_b 7.9633(15) _cell_length_c 15.994(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.122(4) _cell_angle_gamma 90.00 _cell_volume 881.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5275 _cell_measurement_theta_min 2.5465 _cell_measurement_theta_max 29.9525 _exptl_crystal_description needle _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 2.720 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.3121 _exptl_absorpt_correction_T_max 0.7700 _exptl_absorpt_process_details ; absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995), which is based upon the method of Blessing (Blessing, 1995). ; _exptl_special_details ; Data were collected with a Bruker SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 45s duration at a crystal-to-detector distance of 4.486 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12296 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 30.43 _reflns_number_total 2550 _reflns_number_gt 1961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0893P)^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 2550 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1430 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.28514(5) 0.51319(4) -0.00331(2) 0.04410(16) Uani 1 1 d . . . S1 S 0.71137(17) 0.55709(17) 0.15196(7) 0.0471(3) Uani 1 1 d . . . C2 C 0.4789(8) 0.5118(6) 0.1966(3) 0.0478(11) Uani 1 1 d . . . H2A H 0.4786 0.5500 0.2542 0.057 Uiso 1 1 calc R . . H2B H 0.4607 0.3910 0.1972 0.057 Uiso 1 1 calc R . . S3 S 0.27602(16) 0.60696(16) 0.14258(7) 0.0470(3) Uani 1 1 d . . . C4 C 0.3445(9) 0.8250(7) 0.1435(4) 0.0719(16) Uani 1 1 d . . . H4A H 0.2478 0.8887 0.1131 0.086 Uiso 1 1 calc R . . H4B H 0.3438 0.8645 0.2009 0.086 Uiso 1 1 calc R . . C5 C 0.5402(9) 0.8618(6) 0.1062(4) 0.0701(16) Uani 1 1 d . . . H5A H 0.5417 0.8212 0.0491 0.084 Uiso 1 1 calc R . . H5B H 0.5582 0.9826 0.1045 0.084 Uiso 1 1 calc R . . C6 C 0.7080(8) 0.7849(7) 0.1526(4) 0.0640(15) Uani 1 1 d . . . H6A H 0.7045 0.8231 0.2102 0.077 Uiso 1 1 calc R . . H6B H 0.8272 0.8254 0.1281 0.077 Uiso 1 1 calc R . . N1 N 0.0321(6) 0.2194(5) 0.0827(3) 0.0507(9) Uani 1 1 d . . . O1 O 0.0170(5) 0.2933(5) 0.0130(2) 0.0527(8) Uani 1 1 d . . . O2 O -0.1137(8) 0.1597(7) 0.1149(3) 0.1088(19) Uani 1 1 d . . . O3 O 0.1893(7) 0.2149(5) 0.1185(3) 0.0825(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 Ag1 0.0350(2) 0.0596(3) 0.0377(2) -0.00499(13) 0.00121(15) 0.00035(13) S1 0.0374(5) 0.0692(7) 0.0346(5) -0.0015(5) -0.0009(4) -0.0017(5) C2 0.049(3) 0.066(3) 0.028(2) 0.0042(17) 0.000(2) -0.007(2) S3 0.0358(5) 0.0642(7) 0.0412(5) -0.0068(5) 0.0066(4) -0.0028(5) C4 0.068(4) 0.058(3) 0.090(4) -0.030(3) 0.009(3) 0.011(3) C5 0.085(4) 0.042(2) 0.083(4) -0.010(3) 0.019(3) -0.011(3) C6 0.059(3) 0.067(3) 0.066(3) -0.026(3) 0.011(3) -0.028(3) N1 0.056(2) 0.0393(18) 0.057(2) 0.0102(17) -0.0028(19) -0.0076(16) O1 0.052(2) 0.0602(19) 0.0455(17) 0.0149(14) 0.0036(15) 0.0019(14) O2 0.098(4) 0.133(4) 0.095(3) 0.053(3) -0.004(3) -0.057(4) O3 0.077(3) 0.073(2) 0.097(3) 0.015(2) -0.038(3) 0.004(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 S1 2.4427(12) 3_665 ? Ag1 S3 2.4508(12) . ? Ag1 O1 2.565(3) . ? Ag1 Ag1 2.9818(9) 3_665 ? S1 C2 1.798(6) . ? S1 C6 1.814(6) . ? S1 Ag1 2.4427(12) 3_665 ? C2 S3 1.813(5) . ? S3 C4 1.800(6) . ? C4 C5 1.509(9) . ? C5 C6 1.507(9) . ? N1 O3 1.228(5) . ? N1 O2 1.229(6) . ? N1 O1 1.265(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ag1 S3 175.41(4) 3_665 . ? S1 Ag1 O1 87.19(8) 3_665 . ? S3 Ag1 O1 95.24(8) . . ? S1 Ag1 Ag1 90.37(3) 3_665 3_665 ? S3 Ag1 Ag1 90.88(3) . 3_665 ? O1 Ag1 Ag1 132.03(8) . 3_665 ? C2 S1 C6 100.8(2) . . ? C2 S1 Ag1 110.58(16) . 3_665 ? C6 S1 Ag1 103.60(19) . 3_665 ? S1 C2 S3 114.8(2) . . ? C4 S3 C2 101.3(3) . . ? C4 S3 Ag1 107.1(2) . . ? C2 S3 Ag1 107.77(16) . . ? C5 C4 S3 114.9(4) . . ? C6 C5 C4 114.6(5) . . ? C5 C6 S1 114.5(3) . . ? O3 N1 O2 121.3(5) . . ? O3 N1 O1 119.8(4) . . ? O2 N1 O1 118.8(5) . . ? N1 O1 Ag1 110.4(3) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.9995 _refine_diff_density_max 0.633 _refine_diff_density_min -1.594 _refine_diff_density_rms 0.213 # Deepest hole -1.59e/A**3 at 0.1731 0.4957 0.0155 [0.84 A from AG1] #Supporting information for crystal structure of [Ag(1,3-dithiane)]PF6 data_l13900sd _database_code_CSD 187164 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Ag F6 P S2' _chemical_formula_weight 373.06 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.5099(9) _cell_length_b 18.743(3) _cell_length_c 8.2518(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.404(2) _cell_angle_gamma 90.00 _cell_volume 1005.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5758 _cell_measurement_theta_min 2.173 _cell_measurement_theta_max 29.275 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max .3 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 2.624 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.476 _exptl_absorpt_correction_T_max 0.731 _exptl_absorpt_process_details ; absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995), which is based upon the method of Blessing (Blessing, 1995). ; _exptl_special_details ; Data were collected with a Bruker SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 25s duration at a crystal-to-detector distance of 4.501 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'Omega Scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14192 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 30.53 _reflns_number_total 2891 _reflns_number_gt 2176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 2891 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1115 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.2211 _refine_ls_wR_factor_gt 0.2097 _refine_ls_goodness_of_fit_ref 1.454 _refine_ls_restrained_S_all 1.454 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.20449(9) 0.51115(4) 0.44023(8) 0.0487(3) Uani 1 1 d . . . S1 S 0.3135(3) 0.57954(10) 0.6777(2) 0.0400(4) Uani 1 1 d . . . C2 C 0.1570(12) 0.5531(5) 0.8395(9) 0.0453(17) Uani 1 1 d . . . H2A H 0.1909 0.5042 0.8686 0.054 Uiso 1 1 calc R . . H2B H 0.1936 0.5826 0.9334 0.054 Uiso 1 1 calc R . . S3 S -0.1144(3) 0.55897(11) 0.7975(2) 0.0423(4) Uani 1 1 d . . . C4 C -0.1377(13) 0.6524(5) 0.7448(12) 0.053(2) Uani 1 1 d . . . H4A H -0.2811 0.6624 0.7147 0.064 Uiso 1 1 calc R . . H4B H -0.0994 0.6805 0.8406 0.064 Uiso 1 1 calc R . . C5 C -0.0094(15) 0.6768(5) 0.6083(12) 0.053(2) Uani 1 1 d . . . H5A H -0.0419 0.7263 0.5834 0.063 Uiso 1 1 calc R . . H5B H -0.0462 0.6487 0.5122 0.063 Uiso 1 1 calc R . . C6 C 0.2229(14) 0.6701(4) 0.6484(11) 0.0480(18) Uani 1 1 d . . . H6A H 0.2583 0.6971 0.7463 0.058 Uiso 1 1 calc R . . H6B H 0.2948 0.6915 0.5609 0.058 Uiso 1 1 calc R . . P1 P 0.4557(3) 0.36001(11) 0.7883(2) 0.0394(4) Uani 1 1 d . . . F1 F 0.4151(13) 0.2883(4) 0.6997(12) 0.111(3) Uani 1 1 d . . . F2 F 0.4221(11) 0.3995(5) 0.6164(9) 0.092(2) Uani 1 1 d . . . F3 F 0.4980(16) 0.3225(5) 0.9549(9) 0.119(3) Uani 1 1 d . . . F4 F 0.4984(12) 0.4344(4) 0.8728(12) 0.105(3) Uani 1 1 d . . . F5 F 0.6933(10) 0.3540(5) 0.7620(9) 0.088(2) Uani 1 1 d . . . F6 F 0.2175(9) 0.3693(4) 0.8091(9) 0.089(2) 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 0.0438(4) 0.0593(4) 0.0430(4) -0.0138(3) 0.0032(3) -0.0114(3) S1 0.0284(8) 0.0556(11) 0.0354(9) -0.0013(7) -0.0044(6) -0.0036(7) C2 0.048(4) 0.062(5) 0.025(3) 0.009(3) -0.008(3) -0.001(3) S3 0.0419(10) 0.0501(10) 0.0353(9) -0.0060(7) 0.0069(7) -0.0081(7) C4 0.040(4) 0.056(5) 0.061(5) -0.012(4) -0.007(4) 0.007(3) C5 0.062(5) 0.042(4) 0.053(5) 0.010(4) -0.006(4) 0.005(3) C6 0.059(5) 0.035(4) 0.051(5) -0.004(3) 0.007(4) -0.009(3) P1 0.0428(10) 0.0442(10) 0.0307(9) 0.0002(7) -0.0013(7) -0.0010(8) F1 0.120(7) 0.069(4) 0.140(7) -0.050(5) -0.027(5) 0.000(4) F2 0.079(4) 0.128(6) 0.067(4) 0.048(4) -0.012(3) -0.003(4) F3 0.154(9) 0.153(7) 0.050(4) 0.046(5) -0.005(4) -0.004(6) F4 0.084(5) 0.078(4) 0.146(7) -0.053(5) -0.053(5) 0.013(3) F5 0.047(3) 0.121(5) 0.093(5) -0.002(4) -0.004(3) 0.027(3) F6 0.048(3) 0.128(6) 0.093(5) -0.027(4) 0.019(3) -0.010(3) _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 S3 2.405(2) 3_566 ? Ag1 S1 2.4131(19) . ? Ag1 Ag1 2.9236(12) 3_566 ? S1 C2 1.796(8) . ? S1 C6 1.808(8) . ? C2 S3 1.783(8) . ? S3 C4 1.808(10) . ? S3 Ag1 2.405(2) 3_566 ? C4 C5 1.512(13) . ? C5 C6 1.534(13) . ? P1 F1 1.545(7) . ? P1 F3 1.554(7) . ? P1 F4 1.577(7) . ? P1 F5 1.579(6) . ? P1 F6 1.580(6) . ? P1 F2 1.603(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 S3 Ag1 S1 176.98(6) 3_566 . ? S3 Ag1 Ag1 90.81(5) 3_566 3_566 ? S1 Ag1 Ag1 91.82(5) . 3_566 ? C2 S1 C6 99.4(4) . . ? C2 S1 Ag1 107.7(3) . . ? C6 S1 Ag1 108.2(3) . . ? S3 C2 S1 116.0(4) . . ? C2 S3 C4 100.0(4) . . ? C2 S3 Ag1 108.4(3) . 3_566 ? C4 S3 Ag1 108.7(3) . 3_566 ? C5 C4 S3 115.5(6) . . ? C4 C5 C6 113.3(7) . . ? C5 C6 S1 114.6(6) . . ? F1 P1 F3 92.4(6) . . ? F1 P1 F4 178.0(6) . . ? F3 P1 F4 89.5(5) . . ? F1 P1 F5 90.8(5) . . ? F3 P1 F5 88.0(5) . . ? F4 P1 F5 88.6(5) . . ? F1 P1 F6 90.4(4) . . ? F3 P1 F6 94.4(5) . . ? F4 P1 F6 90.2(4) . . ? F5 P1 F6 177.2(5) . . ? F1 P1 F2 88.4(5) . . ? F3 P1 F2 177.6(5) . . ? F4 P1 F2 89.7(5) . . ? F5 P1 F2 89.7(4) . . ? F6 P1 F2 87.8(4) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.219 _refine_diff_density_min -1.627 _refine_diff_density_rms 0.251 # four residual peaks greater than 2e/A**3 lie # within 1A of Ag #Supporting information for crystal structure of [Ag(1,3-dithiane)]BF4 data_l7900sd _database_code_CSD 187165 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Ag B F4 S2' _chemical_formula_weight 314.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.3604(3) _cell_length_b 9.2890(5) _cell_length_c 15.9760(8) _cell_angle_alpha 85.8370(10) _cell_angle_beta 84.7880(10) _cell_angle_gamma 83.6270(10) _cell_volume 932.31(8) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 4120 _cell_measurement_theta_min 2.2105 _cell_measurement_theta_max 30.468 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 2.612 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.589 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details ; absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995), which is based upon the method of Blessing (Blessing, 1995). ; _exptl_special_details ; Data were collected with a Bruker SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 60s duration at a crystal-to-detector distance of 4.476 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted. ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13675 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.211 _diffrn_reflns_theta_max 30.483 _reflns_number_total 5276 _reflns_number_gt 3294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0970P)^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 5276 _refine_ls_number_parameters 217 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1218 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2172 _refine_ls_wR_factor_gt 0.1944 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_restrained_S_all 1.281 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 2.20848(8) 0.49421(7) 0.79205(3) 0.0430(2) Uani 1 1 d . . . Ag2 Ag 1.81661(9) 0.47806(8) 0.70655(4) 0.0524(2) Uani 1 1 d . . . S1 S 1.9530(3) 0.61321(19) 0.58076(11) 0.0353(4) Uani 1 1 d . . . C2 C 2.2366(10) 0.5779(8) 0.5756(4) 0.0352(14) Uani 1 1 d . . . H2A H 2.2969 0.6318 0.5249 0.042 Uiso 1 1 calc R . . H2B H 2.2757 0.4731 0.5682 0.042 Uiso 1 1 calc R . . S3 S 2.3587(2) 0.62620(19) 0.66617(11) 0.0343(4) Uani 1 1 d . . . C4 C 2.2633(12) 0.8169(8) 0.6675(5) 0.0440(17) Uani 1 1 d . . . H4A H 2.3196 0.8581 0.7153 0.053 Uiso 1 1 calc R . . H4B H 2.3196 0.8676 0.6149 0.053 Uiso 1 1 calc R . . C5 C 2.0216(12) 0.8462(9) 0.6753(6) 0.053(2) Uani 1 1 d . . . H5A H 1.9820 0.9506 0.6836 0.064 Uiso 1 1 calc R . . H5B H 1.9652 0.7907 0.7261 0.064 Uiso 1 1 calc R . . C6 C 1.9164(13) 0.8059(8) 0.5995(6) 0.054(2) Uani 1 1 d . . . H6A H 1.9740 0.8607 0.5487 0.065 Uiso 1 1 calc R . . H6B H 1.7624 0.8371 0.6076 0.065 Uiso 1 1 calc R . . S11 S 2.0503(2) 0.38121(18) 0.92141(10) 0.0310(3) Uani 1 1 d . . . C12 C 1.7678(10) 0.4252(8) 0.9226(4) 0.0344(14) Uani 1 1 d . . . H12A H 1.7354 0.5317 0.9242 0.041 Uiso 1 1 calc R . . H12B H 1.7005 0.3805 0.9750 0.041 Uiso 1 1 calc R . . S13 S 1.6494(2) 0.36676(19) 0.83415(11) 0.0349(4) Uani 1 1 d . . . C14 C 1.7324(12) 0.1742(8) 0.8431(5) 0.0446(17) Uani 1 1 d . . . H14A H 1.6682 0.1329 0.8970 0.054 Uiso 1 1 calc R . . H14B H 1.6763 0.1280 0.7970 0.054 Uiso 1 1 calc R . . C15 C 1.9706(12) 0.1355(8) 0.8394(5) 0.0476(19) Uani 1 1 d . . . H15A H 2.0360 0.1806 0.7867 0.057 Uiso 1 1 calc R . . H15B H 2.0019 0.0289 0.8374 0.057 Uiso 1 1 calc R . . C16 C 2.0731(12) 0.1849(7) 0.9146(5) 0.0410(16) Uani 1 1 d . . . H16A H 2.2254 0.1476 0.9106 0.049 Uiso 1 1 calc R . . H16B H 2.0059 0.1410 0.9673 0.049 Uiso 1 1 calc R . . B1 B 2.4731(9) 0.7874(6) 0.8785(3) 0.0421(19) Uani 1 1 d D . . F1 F 2.2912(10) 0.7176(6) 0.8850(3) 0.103(3) Uani 1 1 d D . . F2 F 2.6151(10) 0.7238(7) 0.8183(3) 0.109(3) Uani 1 1 d D . . F3 F 2.5591(8) 0.7752(6) 0.9548(3) 0.0656(14) Uani 1 1 d D . . F4 F 2.4205(8) 0.9305(4) 0.8531(3) 0.0704(15) Uani 1 1 d D . . B11 B 1.5093(12) 0.2072(7) 0.6238(4) 0.086(5) Uani 1 1 d D . . F11 F 1.6820(17) 0.2888(8) 0.6182(5) 0.328(12) Uani 1 1 d D . . F12 F 1.5797(9) 0.0683(5) 0.6464(4) 0.0831(18) Uani 1 1 d D . . F13 F 1.4267(10) 0.2184(8) 0.5474(4) 0.103(2) Uani 1 1 d D . . F14 F 1.3644(14) 0.2636(9) 0.6845(4) 0.157(4) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0346(3) 0.0623(4) 0.0344(3) -0.0036(3) -0.0053(2) -0.0127(3) Ag2 0.0382(3) 0.0841(5) 0.0386(4) -0.0032(3) -0.0085(3) -0.0198(3) S1 0.0307(8) 0.0409(9) 0.0362(9) -0.0126(7) -0.0140(7) 0.0032(7) C2 0.031(3) 0.043(4) 0.031(3) -0.003(3) -0.001(3) 0.002(3) S3 0.0234(7) 0.0444(9) 0.0357(9) -0.0032(7) -0.0081(6) -0.0016(7) C4 0.045(4) 0.049(4) 0.042(4) -0.006(3) -0.017(3) -0.010(3) C5 0.048(4) 0.050(4) 0.066(5) -0.028(4) -0.019(4) 0.005(4) C6 0.046(4) 0.044(4) 0.075(6) -0.024(4) -0.029(4) 0.016(3) S11 0.0273(7) 0.0362(8) 0.0310(8) -0.0088(6) -0.0107(6) 0.0011(6) C12 0.030(3) 0.044(4) 0.030(3) -0.007(3) -0.007(2) 0.005(3) S13 0.0234(7) 0.0465(10) 0.0365(9) -0.0070(7) -0.0100(6) -0.0015(7) C14 0.045(4) 0.048(4) 0.046(4) -0.005(3) -0.018(3) -0.011(3) C15 0.050(4) 0.043(4) 0.052(5) -0.018(3) -0.023(4) 0.009(3) C16 0.041(4) 0.034(3) 0.050(4) -0.012(3) -0.018(3) 0.007(3) B1 0.052(5) 0.040(4) 0.034(4) -0.003(3) -0.003(4) -0.004(4) F1 0.162(7) 0.112(5) 0.054(4) 0.005(3) -0.030(4) -0.093(5) F2 0.142(6) 0.113(5) 0.055(4) -0.015(3) -0.008(4) 0.077(5) F3 0.068(3) 0.087(4) 0.046(3) -0.009(3) -0.025(2) -0.006(3) F4 0.086(4) 0.037(3) 0.088(4) -0.004(2) -0.026(3) 0.004(2) B11 0.153(13) 0.061(7) 0.031(5) 0.004(5) 0.000(6) 0.039(8) F11 0.81(4) 0.160(9) 0.070(6) 0.022(6) -0.067(12) -0.296(17) F12 0.095(4) 0.043(3) 0.111(5) -0.009(3) -0.024(4) 0.009(3) F13 0.091(4) 0.145(6) 0.076(4) -0.042(4) -0.046(4) 0.033(4) F14 0.218(10) 0.144(7) 0.082(5) -0.021(5) 0.001(6) 0.101(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S11 2.4346(17) . ? Ag1 S3 2.4522(18) . ? Ag1 Ag2 2.9718(8) . ? Ag2 S13 2.4292(18) . ? Ag2 S1 2.4343(19) . ? S1 C2 1.793(7) . ? S1 C6 1.822(8) . ? C2 S3 1.810(7) . ? S3 C4 1.808(8) . ? C4 C5 1.526(10) . ? C5 C6 1.525(11) . ? S11 C12 1.796(6) . ? S11 C16 1.823(7) . ? C12 S13 1.803(7) . ? S13 C14 1.807(8) . ? C14 C15 1.515(10) . ? C15 C16 1.539(10) . ? B1 F3 1.373(6) . ? B1 F4 1.375(6) . ? B1 F2 1.377(6) . ? B1 F1 1.380(6) . ? B11 F12 1.352(6) . ? B11 F13 1.365(7) . ? B11 F14 1.367(7) . ? B11 F11 1.395(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S11 Ag1 S3 175.58(6) . . ? S11 Ag1 Ag2 90.89(4) . . ? S3 Ag1 Ag2 89.50(4) . . ? S13 Ag2 S1 173.38(6) . . ? S13 Ag2 Ag1 90.61(4) . . ? S1 Ag2 Ag1 92.20(4) . . ? C2 S1 C6 101.2(4) . . ? C2 S1 Ag2 106.5(2) . . ? C6 S1 Ag2 108.6(3) . . ? S1 C2 S3 115.4(3) . . ? C4 S3 C2 100.3(3) . . ? C4 S3 Ag1 109.9(3) . . ? C2 S3 Ag1 108.6(2) . . ? C5 C4 S3 113.6(5) . . ? C4 C5 C6 114.2(7) . . ? C5 C6 S1 114.6(6) . . ? C12 S11 C16 101.0(3) . . ? C12 S11 Ag1 107.3(2) . . ? C16 S11 Ag1 109.8(3) . . ? S11 C12 S13 115.0(3) . . ? C12 S13 C14 100.4(3) . . ? C12 S13 Ag2 107.9(2) . . ? C14 S13 Ag2 110.5(3) . . ? C15 C14 S13 114.5(5) . . ? C14 C15 C16 113.6(6) . . ? C15 C16 S11 114.2(5) . . ? F3 B1 F4 111.1(5) . . ? F3 B1 F2 110.1(5) . . ? F4 B1 F2 109.2(5) . . ? F3 B1 F1 109.7(5) . . ? F4 B1 F1 108.3(5) . . ? F2 B1 F1 108.4(5) . . ? F12 B11 F13 111.7(5) . . ? F12 B11 F14 110.5(5) . . ? F13 B11 F14 111.0(5) . . ? F12 B11 F11 107.8(5) . . ? F13 B11 F11 108.5(5) . . ? F14 B11 F11 107.1(6) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.934 _refine_diff_density_min -1.344 _refine_diff_density_rms 0.191 # all residual peaks greater than 1e/A**3 are # located close to Ag or disordered BF4- # Supporting information for crystal structure of [Ag(1,3-dithiane)]2.[BF4]Cl data_13bf41 _database_code_CSD 187166 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(1,3-dithicyclohexane) bis(silver) tetrafluroborate chloride ; _chemical_name_common [Ag2(1,3-[6]aneS2)(BF4)(Cl)] _chemical_formula_moiety 'C8 H16 Ag2 B Cl F4 S4' _chemical_formula_sum 'C8 H16 Ag2 B Cl F4 S4' _chemical_formula_weight 578.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.290(2) _cell_length_b 6.919(2) _cell_length_c 16.189(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1600.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8884 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28.5 _exptl_crystal_description column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 3.159 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7430 _exptl_absorpt_correction_T_max 0.9112 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68910 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area detector' _diffrn_measurement_method 'area detector scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10906 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 29.46 _reflns_number_total 2427 _reflns_number_gt 2173 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995a)' _computing_cell_refinement 'LSCELL (Clegg, 1996)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.290P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2427 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.267 _refine_ls_restrained_S_all 1.267 _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 Ag Ag 0.131091(12) 0.03567(3) 0.457525(11) 0.02044(10) Uani 1 1 d . . . Cl Cl -0.00395(5) 0.2500 0.54188(5) 0.01735(16) Uani 1 2 d S . . C1 C 0.2239(3) 0.2500 0.6351(2) 0.0239(7) Uani 1 2 d S . . H1A H 0.1597 0.2500 0.6580 0.029 Uiso 1 2 calc SR . . H1B H 0.2680 0.2500 0.6823 0.029 Uiso 1 2 calc SR . . S2 S 0.24033(5) 0.03132(10) 0.57790(4) 0.02616(16) Uani 1 1 d . . . C3 C 0.3591(2) 0.0684(5) 0.5432(2) 0.0345(7) Uani 1 1 d . . . H3A H 0.4007 0.0716 0.5920 0.041 Uiso 1 1 calc R . . H3B H 0.3779 -0.0435 0.5089 0.041 Uiso 1 1 calc R . . C4 C 0.3739(3) 0.2500 0.4941(3) 0.0388(11) Uani 1 2 d S . . H4A H 0.3304 0.2500 0.4465 0.047 Uiso 1 2 calc SR . . H4B H 0.4385 0.2500 0.4720 0.047 Uiso 1 2 calc SR . . C11 C 0.1818(2) 0.2500 0.2646(2) 0.0201(6) Uani 1 2 d S . . H11A H 0.1763 0.2500 0.2036 0.024 Uiso 1 2 calc SR . . H11B H 0.2493 0.2500 0.2783 0.024 Uiso 1 2 calc SR . . S12 S 0.13113(4) 0.03097(9) 0.30316(4) 0.02092(15) Uani 1 1 d . . . C13 C 0.01058(18) 0.0672(4) 0.27333(16) 0.0279(6) Uani 1 1 d . . . H13A H 0.0070 0.0691 0.2123 0.033 Uiso 1 1 calc R . . H13B H -0.0266 -0.0446 0.2928 0.033 Uiso 1 1 calc R . . C14 C -0.0335(2) 0.2500 0.3061(2) 0.0302(8) Uani 1 2 d S . . H14A H -0.1008 0.2500 0.2916 0.036 Uiso 1 2 calc SR . . H14B H -0.0287 0.2500 0.3671 0.036 Uiso 1 2 calc SR . . B B 0.3492(3) 0.7500 0.3582(2) 0.0232(8) Uani 1 2 d S . . F1 F 0.28165(14) 0.7500 0.42107(13) 0.0251(4) Uani 1 2 d S . . F2 F 0.43764(16) 0.7500 0.39401(16) 0.0389(6) Uani 1 2 d S . . F3 F 0.33810(12) 0.5865(3) 0.31051(12) 0.0410(4) 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 0.01690(12) 0.02202(14) 0.02240(13) 0.00040(6) -0.00287(6) -0.00232(6) Cl 0.0132(3) 0.0163(3) 0.0226(4) 0.000 0.0035(3) 0.000 C1 0.0236(16) 0.031(2) 0.0168(14) 0.000 -0.0036(12) 0.000 S2 0.0270(3) 0.0198(3) 0.0317(3) 0.0026(2) -0.0134(3) -0.0017(2) C3 0.0199(13) 0.0388(17) 0.0447(18) -0.0154(13) -0.0138(11) 0.0113(11) C4 0.0145(16) 0.072(4) 0.030(2) 0.000 -0.0014(14) 0.000 C11 0.0144(14) 0.0243(17) 0.0216(15) 0.000 0.0048(12) 0.000 S12 0.0213(3) 0.0194(3) 0.0221(3) -0.0009(2) -0.0011(2) -0.0012(2) C13 0.0209(12) 0.0383(15) 0.0245(12) 0.0016(11) -0.0071(9) -0.0108(10) C14 0.0124(14) 0.054(3) 0.0245(17) 0.000 -0.0026(13) 0.000 B 0.0117(15) 0.036(2) 0.0219(17) 0.000 0.0006(14) 0.000 F1 0.0181(9) 0.0335(12) 0.0236(10) 0.000 0.0068(8) 0.000 F2 0.0136(10) 0.0646(19) 0.0384(13) 0.000 -0.0069(9) 0.000 F3 0.0251(8) 0.0527(11) 0.0452(10) -0.0211(9) 0.0059(8) 0.0025(8) _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 S2 2.4972(7) . y Ag S12 2.4992(7) . y Ag Cl 2.6847(7) 5_556 y Ag Cl 2.7907(7) . y Ag Ag 2.9659(9) 7_565 y Cl Ag 2.6847(7) 5_556 ? Cl Ag 2.6847(7) 3_556 ? Cl Ag 2.7907(7) 7_565 ? C1 S2 1.789(2) 7_565 ? C1 S2 1.789(2) . ? S2 C3 1.806(3) . ? C3 C4 1.502(4) . ? C4 C3 1.502(4) 7_565 ? C11 S12 1.7917(18) . ? C11 S12 1.7917(18) 7_565 ? S12 C13 1.807(3) . ? C13 C14 1.510(4) . ? C14 C13 1.510(4) 7_565 ? B F3 1.379(3) . ? B F3 1.379(3) 7_575 ? B F2 1.390(4) . ? B F1 1.403(4) . ? 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 S2 Ag S12 141.26(2) . . y S2 Ag Cl 114.29(2) . 5_556 y S12 Ag Cl 89.67(2) . 5_556 y S2 Ag Cl 93.26(3) . . y S12 Ag Cl 119.76(2) . . y Cl Ag Cl 85.498(18) 5_556 . y S2 Ag Ag 90.691(16) . 7_565 y S12 Ag Ag 90.746(15) . 7_565 y Cl Ag Ag 137.410(15) 5_556 7_565 y Cl Ag Ag 57.900(12) . 7_565 y Ag Cl Ag 94.82(3) 5_556 3_556 y Ag Cl Ag 149.42(3) 5_556 7_565 ? Ag Cl Ag 94.502(18) 3_556 7_565 ? Ag Cl Ag 94.502(18) 5_556 . y Ag Cl Ag 149.42(3) 3_556 . y Ag Cl Ag 64.20(2) 7_565 . y S2 C1 S2 115.50(19) 7_565 . ? C1 S2 C3 99.46(16) . . ? C1 S2 Ag 108.14(11) . . ? C3 S2 Ag 110.03(10) . . ? C4 C3 S2 114.6(2) . . ? C3 C4 C3 113.6(4) . 7_565 ? S12 C11 S12 115.53(18) . 7_565 ? C11 S12 C13 100.05(14) . . ? C11 S12 Ag 109.73(11) . . ? C13 S12 Ag 105.38(9) . . ? C14 C13 S12 114.9(2) . . ? C13 C14 C13 113.8(3) 7_565 . ? F3 B F3 110.3(3) . 7_575 ? F3 B F2 109.8(2) . . ? F3 B F2 109.8(2) 7_575 . ? F3 B F1 109.1(2) . . ? F3 B F1 109.1(2) 7_575 . ? F2 B F1 108.8(3) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.97 _refine_diff_density_min -0.93 _refine_diff_density_rms 0.118 # Supporting information for crystal structure of [Ag(1,3-dithiane)]NO2 data_13no21 _database_code_CSD 187167 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3-dithiacyclohexane silver(I) nitrite ; _chemical_name_common [Ag(1,3-[6]aneS2)NO2] _chemical_formula_moiety 'C4 H8 Ag N O2 S2' _chemical_formula_sum 'C4 H8 Ag N O2 S2' _chemical_formula_weight 274.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.5119(10) _cell_length_b 13.1352(19) _cell_length_c 18.463(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1579.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3078 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 27.46 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 3.019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.517 _exptl_absorpt_correction_T_max 0.704 _exptl_absorpt_process_details 'SADABS (Bruker, 1999b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10023 _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.93 _reflns_number_total 3677 _reflns_number_gt 2984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999a)' _computing_data_reduction 'SAINT (Bruker, 1999a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick, 1994)' _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 w=1/[\s^2^(Fo^2^)+(0.0321P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _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 0.03(4) _refine_ls_number_reflns 3677 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.61381(7) -0.00628(4) 0.13724(2) 0.02439(12) Uani 1 1 d . . . Ag2 Ag 0.42371(8) 0.14917(3) 0.04368(3) 0.02179(12) Uani 1 1 d . . . S1 S 0.4666(3) 0.08250(12) 0.24651(9) 0.0279(4) Uani 1 1 d . . . C2 C 0.2301(9) 0.1469(4) 0.2225(3) 0.0219(13) Uani 1 1 d . . . H2A H 0.1262 0.0950 0.2097 0.026 Uiso 1 1 calc R . . H2B H 0.1791 0.1839 0.2656 0.026 Uiso 1 1 calc R . . S3 S 0.2511(2) 0.23535(11) 0.14899(8) 0.0216(3) Uani 1 1 d . . . C4 C 0.4445(10) 0.3199(4) 0.1861(3) 0.0256(15) Uani 1 1 d . . . H4A H 0.4708 0.3749 0.1507 0.031 Uiso 1 1 calc R . . H4B H 0.3888 0.3518 0.2305 0.031 Uiso 1 1 calc R . . C5 C 0.6464(10) 0.2696(5) 0.2046(3) 0.0260(15) Uani 1 1 d . . . H5A H 0.7466 0.3227 0.2187 0.031 Uiso 1 1 calc R . . H5B H 0.7002 0.2350 0.1609 0.031 Uiso 1 1 calc R . . C6 C 0.6290(11) 0.1923(5) 0.2655(4) 0.0334(17) Uani 1 1 d . . . H6A H 0.5745 0.2274 0.3089 0.040 Uiso 1 1 calc R . . H6B H 0.7685 0.1676 0.2775 0.040 Uiso 1 1 calc R . . S11 S 0.4440(2) -0.13019(10) 0.05033(9) 0.0237(4) Uani 1 1 d . . . C12 C 0.2277(10) -0.0833(5) -0.0009(4) 0.0290(16) Uani 1 1 d . . . H12A H 0.1842 -0.1370 -0.0353 0.035 Uiso 1 1 calc R . . H12B H 0.1122 -0.0714 0.0329 0.035 Uiso 1 1 calc R . . S13 S 0.2738(2) 0.03181(11) -0.05088(9) 0.0240(4) Uani 1 1 d . . . C14 C 0.4803(10) -0.0117(5) -0.1088(3) 0.0275(15) Uani 1 1 d . . . H14A H 0.4284 -0.0676 -0.1397 0.033 Uiso 1 1 calc R . . H14B H 0.5216 0.0449 -0.1411 0.033 Uiso 1 1 calc R . . C15 C 0.6685(10) -0.0490(5) -0.0682(3) 0.0281(16) Uani 1 1 d . . . H15A H 0.7168 0.0055 -0.0354 0.034 Uiso 1 1 calc R . . H15B H 0.7795 -0.0630 -0.1035 0.034 Uiso 1 1 calc R . . C16 C 0.6280(10) -0.1461(5) -0.0234(3) 0.0299(15) Uani 1 1 d . . . H16A H 0.7599 -0.1700 -0.0028 0.036 Uiso 1 1 calc R . . H16B H 0.5769 -0.2000 -0.0564 0.036 Uiso 1 1 calc R . . N1 N 0.9226(8) 0.1480(4) 0.0385(3) 0.0249(10) Uani 1 1 d . . . O1 O 0.7632(7) 0.1943(3) 0.0198(2) 0.0291(11) Uani 1 1 d . . . O2 O 0.8986(7) 0.0744(3) 0.0793(2) 0.0323(11) Uani 1 1 d . . . N2 N 0.9789(9) -0.1392(5) 0.1807(3) 0.0366(15) Uani 1 1 d . . . O3 O 0.9258(9) -0.0586(3) 0.2108(3) 0.0396(12) Uani 1 1 d . . . O4 O 0.8520(8) -0.1700(4) 0.1342(3) 0.0460(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 Ag1 0.0255(2) 0.0266(2) 0.0210(2) 0.0000(2) -0.0019(2) 0.0042(2) Ag2 0.0245(3) 0.0236(2) 0.0173(2) 0.0005(2) 0.0006(2) 0.0004(2) S1 0.0355(11) 0.0300(9) 0.0183(9) 0.0045(7) 0.0022(7) 0.0054(7) C2 0.023(3) 0.018(3) 0.025(3) -0.002(3) 0.012(3) 0.001(3) S3 0.0193(8) 0.0265(8) 0.0190(8) 0.0001(7) -0.0008(7) 0.0008(7) C4 0.028(4) 0.023(3) 0.025(4) -0.004(3) 0.007(3) -0.007(3) C5 0.020(4) 0.038(4) 0.020(3) -0.010(3) -0.002(3) -0.011(3) C6 0.026(4) 0.054(4) 0.020(3) -0.002(3) -0.008(3) 0.003(3) S11 0.0236(9) 0.0208(7) 0.0266(9) 0.0026(7) -0.0035(8) -0.0021(6) C12 0.017(4) 0.035(4) 0.035(4) -0.005(3) -0.005(3) -0.007(3) S13 0.0231(8) 0.0278(8) 0.0212(8) -0.0017(7) -0.0065(7) 0.0021(6) C14 0.038(4) 0.031(4) 0.014(3) -0.005(3) 0.001(3) -0.005(3) C15 0.024(4) 0.041(4) 0.020(3) -0.009(3) 0.008(3) -0.002(3) C16 0.027(4) 0.029(3) 0.034(4) -0.014(3) -0.004(3) 0.004(3) N1 0.024(3) 0.027(2) 0.024(3) 0.000(2) 0.002(3) -0.003(3) O1 0.019(3) 0.036(3) 0.032(3) 0.010(2) 0.003(2) 0.000(2) O2 0.024(3) 0.038(2) 0.035(3) 0.014(2) -0.005(2) -0.001(2) N2 0.031(3) 0.045(4) 0.034(4) 0.015(3) 0.002(3) 0.004(3) O3 0.050(3) 0.040(3) 0.029(3) 0.007(2) -0.006(3) -0.005(3) O4 0.049(3) 0.051(3) 0.038(3) -0.002(3) -0.011(3) 0.012(3) _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 O2 2.389(5) . y Ag1 O3 2.538(5) . y Ag1 O4 2.652(5) . y Ag1 S1 2.520(2) . y Ag1 S11 2.539(2) . y Ag1 Ag2 2.9470(7) . y Ag2 O1 2.331(4) . y Ag2 O1 2.588(4) 4_455 y Ag2 S3 2.5149(16) . y Ag2 S13 2.5253(16) . y S1 C2 1.812(6) . ? S1 C6 1.823(7) . ? C2 S3 1.792(6) . ? S3 C4 1.813(6) . ? C4 C5 1.511(9) . ? C5 C6 1.519(9) . ? S11 C12 1.804(7) . ? S11 C16 1.826(6) . ? C12 S13 1.797(7) . ? S13 C14 1.811(6) . ? C14 C15 1.517(9) . ? C15 C16 1.543(9) . ? N1 O2 1.234(6) . ? N1 O1 1.251(6) . ? O1 Ag2 2.588(4) 4 ? N2 O3 1.244(7) . ? N2 O4 1.259(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ag1 S1 116.66(11) . . y O2 Ag1 O3 74.83(15) . . y S1 Ag1 O3 90.10(12) . . y O2 Ag1 S11 109.84(12) . . y S1 Ag1 S11 129.56(6) . . y O3 Ag1 S11 120.87(11) . . y O2 Ag1 O4 84.05(16) . . y S1 Ag1 O4 127.94(12) . . y O3 Ag1 O4 47.45(15) . . y S11 Ag1 O4 73.82(12) . . y O2 Ag1 Ag2 75.89(10) . . y S1 Ag1 Ag2 89.36(4) . . y O3 Ag1 Ag2 146.85(10) . . y S11 Ag1 Ag2 83.73(4) . . y O4 Ag1 Ag2 142.65(11) . . y O1 Ag2 S3 117.09(12) . . y O1 Ag2 S13 113.03(12) . . y S3 Ag2 S13 129.53(6) . . y O1 Ag2 O1 95.48(8) . 4_455 y S3 Ag2 O1 79.18(11) . 4_455 y S13 Ag2 O1 90.89(11) . 4_455 y O1 Ag2 Ag1 83.60(11) . . y S3 Ag2 Ag1 92.66(4) . . y S13 Ag2 Ag1 98.32(4) . . y O1 Ag2 Ag1 170.35(10) 4_455 . y C2 S1 C6 99.8(3) . . ? C2 S1 Ag1 110.1(2) . . ? C6 S1 Ag1 107.4(2) . . ? S3 C2 S1 115.0(3) . . ? C2 S3 C4 99.4(3) . . ? C2 S3 Ag2 109.15(19) . . ? C4 S3 Ag2 104.9(2) . . ? C5 C4 S3 115.0(4) . . ? C4 C5 C6 113.2(5) . . ? C5 C6 S1 115.4(4) . . ? C12 S11 C16 99.2(3) . . ? C12 S11 Ag1 116.9(2) . . ? C16 S11 Ag1 105.0(2) . . ? S13 C12 S11 115.2(3) . . ? C12 S13 C14 99.3(3) . . ? C12 S13 Ag2 102.9(2) . . ? C14 S13 Ag2 108.3(2) . . ? C15 C14 S13 114.2(4) . . ? C14 C15 C16 113.2(5) . . ? C15 C16 S11 114.7(4) . . ? O2 N1 O1 116.4(5) . . ? N1 O1 Ag2 127.6(4) . . ? N1 O1 Ag2 100.2(3) . 4 ? Ag2 O1 Ag2 132.13(19) . 4 ? N1 O2 Ag1 135.9(4) . . ? O3 N2 O4 113.3(6) . . ? N2 O3 Ag1 102.4(4) . . ? N2 O4 Ag1 96.2(4) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.91 _refine_diff_density_min -0.81 _refine_diff_density_rms 0.139 # Supporting information for crystal structure of [Ag2(1,3-dithiane)][SO4].3H2O data_13so41 _database_code_CSD 187168 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3-dithiacyclohexane bis(silver) sulphate trihydrate ; _chemical_name_common [Ag2(1,3-[6]aneS2)SO4].3H2O _chemical_formula_moiety 'C4 H14 Ag2 O7 S3' _chemical_formula_sum 'C4 H14 Ag2 O7 S3' _chemical_formula_weight 486.07 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.876(2) _cell_length_b 7.0102(5) _cell_length_c 16.8656(13) _cell_angle_alpha 90.00 _cell_angle_beta 116.449(2) _cell_angle_gamma 90.00 _cell_volume 2421.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6751 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 3.766 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.552 _exptl_absorpt_correction_T_max 0.647 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68910 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area detector' _diffrn_measurement_method 'area detector scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8132 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 29.24 _reflns_number_total 3289 _reflns_number_gt 2914 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995a)' _computing_cell_refinement 'LSCELL (Clegg, 1996)' _computing_data_reduction 'SAINT (Siemens, 1995b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+2.4467P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0032(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3289 _refine_ls_number_parameters 155 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 Ag1 Ag 0.0000 0.92082(5) 0.2500 0.01837(12) Uani 1 2 d S . . Ag2 Ag 0.0000 1.36279(4) 0.2500 0.01864(12) Uani 1 2 d S . . Ag3 Ag 0.071198(12) 0.64237(3) 0.497737(16) 0.02029(11) Uani 1 1 d . . . S1 S 0.08055(3) 0.92489(10) 0.40672(4) 0.01464(16) Uani 1 1 d . . . C2 C 0.07620(15) 1.1378(4) 0.4630(2) 0.0155(5) Uani 1 1 d . . . H2A H 0.0347 1.1380 0.4682 0.019 Uiso 1 1 calc R . . H2B H 0.1126 1.1380 0.5237 0.019 Uiso 1 1 calc R . . S3 S 0.08054(3) 1.35014(9) 0.40644(5) 0.01428(16) Uani 1 1 d . . . C4 C 0.16106(15) 1.3199(5) 0.4126(2) 0.0180(5) Uani 1 1 d . . . H4A H 0.1707 1.4300 0.3836 0.022 Uiso 1 1 calc R . . H4B H 0.1938 1.3193 0.4755 0.022 Uiso 1 1 calc R . . C5 C 0.16772(15) 1.1362(4) 0.3687(2) 0.0187(6) Uani 1 1 d . . . H5A H 0.1340 1.1363 0.3062 0.022 Uiso 1 1 calc R . . H5B H 0.2109 1.1364 0.3683 0.022 Uiso 1 1 calc R . . C6 C 0.16119(14) 0.9532(4) 0.41227(19) 0.0172(5) Uani 1 1 d . . . H6A H 0.1942 0.9531 0.4751 0.021 Uiso 1 1 calc R . . H6B H 0.1704 0.8431 0.3828 0.021 Uiso 1 1 calc R . . S5 S -0.09865(3) 0.63866(9) 0.31582(5) 0.01257(16) Uani 1 1 d . . . O1 O -0.06565(12) 0.6442(3) 0.25791(15) 0.0177(4) Uani 1 1 d . . . O2 O -0.05092(11) 0.5994(3) 0.40805(14) 0.0199(4) Uani 1 1 d . . . O3 O -0.14758(10) 0.4826(3) 0.28525(13) 0.0182(4) Uani 1 1 d . . . O4 O -0.13147(12) 0.8215(3) 0.31047(16) 0.0225(5) Uani 1 1 d . . . O9 O 0.07277(13) 0.8344(4) 0.62687(18) 0.0243(5) Uani 1 1 d D . . H9B H 0.100(2) 0.742(7) 0.665(3) 0.031(11) Uiso 1 1 d D . . H9A H 0.086(3) 0.930(8) 0.639(4) 0.043(15) Uiso 1 1 d D . . O10 O -0.22625(11) 0.9849(4) 0.35133(16) 0.0261(5) Uani 1 1 d . . . O11 O 0.19664(12) 0.6321(3) 0.59505(18) 0.0257(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01854(17) 0.01785(19) 0.01393(16) 0.000 0.00293(12) 0.000 Ag2 0.01837(19) 0.01794(19) 0.01454(18) 0.000 0.00276(14) 0.000 Ag3 0.02526(17) 0.01617(16) 0.01928(16) 0.00038(7) 0.00976(11) -0.00171(7) S1 0.0165(3) 0.0121(3) 0.0135(3) 0.0004(2) 0.0050(2) -0.0002(2) C2 0.0195(13) 0.0131(13) 0.0142(12) -0.0009(9) 0.0078(11) -0.0012(9) S3 0.0145(3) 0.0133(3) 0.0135(3) -0.0005(2) 0.0048(3) 0.0009(2) C4 0.0154(12) 0.0188(13) 0.0185(13) 0.0015(11) 0.0065(10) -0.0018(11) C5 0.0166(13) 0.0210(15) 0.0200(13) 0.0004(10) 0.0094(11) 0.0012(10) C6 0.0153(12) 0.0164(13) 0.0178(12) 0.0006(10) 0.0056(10) 0.0049(10) S5 0.0120(3) 0.0121(3) 0.0136(3) 0.0002(2) 0.0057(3) 0.0001(2) O1 0.0206(10) 0.0162(10) 0.0212(10) 0.0009(7) 0.0136(9) 0.0004(7) O2 0.0181(10) 0.0238(11) 0.0153(9) 0.0010(8) 0.0051(8) -0.0052(8) O3 0.0155(9) 0.0169(10) 0.0183(9) 0.0003(8) 0.0042(7) -0.0052(8) O4 0.0229(11) 0.0149(10) 0.0315(12) -0.0012(9) 0.0136(9) 0.0060(9) O9 0.0230(11) 0.0184(11) 0.0265(12) 0.0001(9) 0.0064(10) 0.0002(9) O10 0.0179(10) 0.0326(13) 0.0251(11) -0.0052(10) 0.0073(9) -0.0019(9) O11 0.0212(12) 0.0299(13) 0.0250(12) 0.0010(9) 0.0093(10) 0.0016(8) _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 S1 2.4585(7) 2 ? Ag1 S1 2.4585(7) . y Ag1 O1 2.492(2) . y Ag1 O1 2.492(2) 2 ? Ag1 Ag2 3.0983(5) . y Ag2 S3 2.4563(7) 2 ? Ag2 S3 2.4563(7) . y Ag2 O1 2.519(2) 1_565 y Ag2 O1 2.519(2) 2_565 ? Ag3 O2 2.504(2) 5_566 y Ag3 O2 2.533(2) . y Ag3 O9 2.547(3) . y Ag3 S1 2.5724(7) . y Ag3 O11 2.596(3) . y Ag3 S3 2.6281(7) 1_545 y S1 C2 1.796(3) . ? S1 C6 1.816(3) . ? C2 S3 1.794(3) . ? S3 C4 1.811(3) . ? S3 Ag3 2.6281(7) 1_565 ? C4 C5 1.527(4) . ? C5 C6 1.519(4) . ? S5 O4 1.468(2) . ? S5 O2 1.475(2) . ? S5 O1 1.477(2) . ? S5 O3 1.484(2) . ? O1 Ag2 2.519(2) 1_545 ? O2 Ag3 2.504(2) 5_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ag1 S1 178.67(4) 2 . y S1 Ag1 O1 83.43(6) 2 . y S1 Ag1 O1 97.61(6) . . y S1 Ag1 O1 97.61(6) 2 2 ? S1 Ag1 O1 83.43(6) . 2 ? O1 Ag1 O1 77.83(10) . 2 y S1 Ag1 Ag2 89.336(18) 2 . ? S1 Ag1 Ag2 89.34(2) . . y O1 Ag1 Ag2 141.08(5) . . y O1 Ag1 Ag2 141.08(5) 2 . ? S3 Ag2 S3 175.86(3) 2 . y S3 Ag2 O1 84.58(6) 2 1_565 ? S3 Ag2 O1 98.69(6) . 1_565 y S3 Ag2 O1 98.69(6) 2 2_565 ? S3 Ag2 O1 84.58(6) . 2_565 y O1 Ag2 O1 76.88(10) 1_565 2_565 y S3 Ag2 Ag1 87.930(17) 2 . ? S3 Ag2 Ag1 87.93(2) . . y O1 Ag2 Ag1 141.56(5) 1_565 . y O1 Ag2 Ag1 141.56(5) 2_565 . ? O2 Ag3 O2 80.31(8) 5_566 . y O2 Ag3 O9 75.59(8) 5_566 . y O2 Ag3 O9 99.51(8) . . y O2 Ag3 S1 171.13(6) 5_566 . y O2 Ag3 S1 95.62(5) . . y O9 Ag3 S1 97.48(6) . . y O2 Ag3 O11 92.58(7) 5_566 . y O2 Ag3 O11 171.37(7) . . y O9 Ag3 O11 83.30(8) . . y S1 Ag3 O11 92.08(6) . . y O2 Ag3 S3 86.01(6) 5_566 1_545 y O2 Ag3 S3 85.03(6) . 1_545 y O9 Ag3 S3 159.91(6) . 1_545 y S1 Ag3 S3 101.56(2) . 1_545 y O11 Ag3 S3 89.62(6) . 1_545 y C2 S1 C6 100.15(14) . . ? C2 S1 Ag1 112.75(10) . . ? C6 S1 Ag1 108.32(10) . . ? C2 S1 Ag3 106.59(10) . . ? C6 S1 Ag3 113.96(10) . . ? Ag1 S1 Ag3 114.26(3) . . ? S3 C2 S1 112.26(16) . . ? C2 S3 C4 99.70(14) . . ? C2 S3 Ag2 114.11(10) . . ? C4 S3 Ag2 108.84(10) . . ? C2 S3 Ag3 107.25(10) . 1_565 ? C4 S3 Ag3 113.82(11) . 1_565 ? Ag2 S3 Ag3 112.54(3) . 1_565 ? C5 C4 S3 112.9(2) . . ? C6 C5 C4 115.1(3) . . ? C5 C6 S1 112.6(2) . . ? O4 S5 O2 110.23(14) . . ? O4 S5 O1 109.55(13) . . ? O2 S5 O1 110.24(13) . . ? O4 S5 O3 109.66(14) . . ? O2 S5 O3 108.57(13) . . ? O1 S5 O3 108.56(13) . . ? S5 O1 Ag1 123.60(12) . . ? S5 O1 Ag2 120.45(11) . 1_545 ? Ag1 O1 Ag2 102.64(8) . 1_545 ? S5 O2 Ag3 122.43(12) . 5_566 ? S5 O2 Ag3 135.16(13) . . ? Ag3 O2 Ag3 99.69(8) 5_566 . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.92 _refine_diff_density_min -0.73 _refine_diff_density_rms 0.173