#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Blake, Alexander J.' 'Brooks, Neil R.' 'Champness, Neil' 'Cunningham, John W.' 'Hubberstey, P.' 'Schroder, M.' 'Teat, Simon J.' 'Wilson, Claire' _publ_contact_author_name 'Prof M Schroder' _publ_contact_author_address ; Prof M Schroder Department of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; data_13no31 _database_code_CSD 156906 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4-dithiacyclohexane silver nitrite ; _chemical_name_common '1,4-dithiane silver nitrite' _chemical_formula_moiety 'C4 H8 S2 Ag N O2' _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 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 10.9407(9) _cell_length_b 7.5356(6) _cell_length_c 9.5107(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.229(1) _cell_angle_gamma 90.00 _cell_volume 766.31(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2797 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 28.7 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 3.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.606 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS (Bruker, 1999b)' _exptl_special_details ; 1,4-dithiacyclohexane silver nitrite ; _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 4874 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.79 _reflns_number_total 1800 _reflns_number_gt 1586 _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^)+(0.0379P)^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_number_reflns 1800 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 0.716194(19) 0.14060(3) 0.34886(2) 0.02016(9) Uani 1 1 d . . . S1 S 0.51305(6) -0.03647(9) 0.32284(7) 0.01699(15) Uani 1 1 d . . . S2 S 0.88599(6) -0.10441(9) 0.37061(7) 0.01613(15) Uani 1 1 d . . . C1 C 0.3944(2) 0.0929(4) 0.3833(3) 0.0168(5) Uani 1 1 d . . . H1A H 0.3609 0.1824 0.3090 0.020 Uiso 1 1 calc R . . H1B H 0.3247 0.0133 0.3931 0.020 Uiso 1 1 calc R . . C2 C 0.5584(3) -0.1870(4) 0.4745(3) 0.0181(5) Uani 1 1 d . . . H2A H 0.4854 -0.2611 0.4824 0.022 Uiso 1 1 calc R . . H2B H 0.6248 -0.2672 0.4555 0.022 Uiso 1 1 calc R . . C3 C 0.9395(3) -0.1693(4) 0.5569(3) 0.0178(6) Uani 1 1 d . . . H3A H 0.8720 -0.2365 0.5878 0.021 Uiso 1 1 calc R . . H3B H 1.0120 -0.2499 0.5641 0.021 Uiso 1 1 calc R . . C4 C 1.0228(2) 0.0145(4) 0.3406(3) 0.0173(5) Uani 1 1 d . . . H4A H 1.0938 -0.0694 0.3513 0.021 Uiso 1 1 calc R . . H4B H 1.0055 0.0596 0.2406 0.021 Uiso 1 1 calc R . . N1 N 0.7704(2) 0.4515(3) 0.5397(3) 0.0224(5) Uani 1 1 d . . . O1 O 0.7739(2) 0.4401(3) 0.4090(2) 0.0280(5) Uani 1 1 d . . . O2 O 0.74336(19) 0.3081(3) 0.5944(2) 0.0229(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 Ag1 0.02036(13) 0.02002(13) 0.02164(13) -0.00124(8) 0.00789(9) -0.00185(8) S1 0.0160(3) 0.0183(3) 0.0170(3) -0.0013(3) 0.0044(2) 0.0006(3) S2 0.0161(3) 0.0159(3) 0.0164(3) -0.0008(2) 0.0035(2) -0.0013(2) C1 0.0135(13) 0.0164(13) 0.0207(13) 0.0019(11) 0.0037(10) 0.0025(10) C2 0.0176(13) 0.0155(13) 0.0220(13) -0.0014(11) 0.0062(11) 0.0019(11) C3 0.0188(14) 0.0150(13) 0.0199(13) 0.0031(11) 0.0049(11) -0.0004(10) C4 0.0154(13) 0.0193(14) 0.0181(13) 0.0018(11) 0.0052(10) -0.0018(11) N1 0.0212(12) 0.0196(13) 0.0258(13) -0.0006(10) 0.0037(10) -0.0019(10) O1 0.0381(13) 0.0255(12) 0.0203(10) 0.0015(9) 0.0059(9) -0.0039(10) O2 0.0286(11) 0.0184(10) 0.0235(10) -0.0009(8) 0.0098(8) -0.0040(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O1 2.381(2) . y Ag1 O2 2.5301(19) 4_565 y Ag1 S1 2.5590(7) . y Ag1 S2 2.5961(7) . y Ag1 O2 2.615(2) . y S1 C1 1.811(3) . ? S1 C2 1.819(3) . ? S2 C3 1.812(3) . ? S2 C4 1.818(3) . ? C1 C2 1.518(4) 3_656 ? C2 C1 1.518(4) 3_656 ? C3 C4 1.520(4) 3_756 ? C4 C3 1.520(4) 3_756 ? N1 O1 1.255(3) . ? N1 O2 1.261(3) . ? O2 Ag1 2.5301(19) 4_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 O1 Ag1 O2 90.35(7) . 4_565 y O1 Ag1 S1 134.28(6) . . y O2 Ag1 S1 105.24(5) 4_565 . y O1 Ag1 S2 120.43(6) . . y O2 Ag1 S2 87.59(5) 4_565 . y S1 Ag1 S2 103.24(2) . . y O1 Ag1 O2 49.73(7) . . y O2 Ag1 O2 140.01(3) 4_565 . y S1 Ag1 O2 105.67(5) . . y S2 Ag1 O2 109.14(5) . . y C1 S1 C2 100.22(12) . . ? C1 S1 Ag1 110.78(9) . . ? C2 S1 Ag1 99.39(9) . . ? C3 S2 C4 100.39(12) . . ? C3 S2 Ag1 110.32(9) . . ? C4 S2 Ag1 103.65(9) . . ? C2 C1 S1 113.77(18) 3_656 . ? C1 C2 S1 113.51(19) 3_656 . ? C4 C3 S2 114.05(19) 3_756 . ? C3 C4 S2 113.50(19) 3_756 . ? O1 N1 O2 114.1(2) . . ? N1 O1 Ag1 103.93(16) . . ? N1 O2 Ag1 110.38(17) . 4_566 ? N1 O2 Ag1 92.18(15) . . ? Ag1 O2 Ag1 156.04(9) 4_566 . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.90 _refine_diff_density_min -0.52 _refine_diff_density_rms 0.124 data_14NO31 _database_code_CSD 156907 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(1,4-dithiacyclohexane)bis(silver nitrate) ; _chemical_name_common 'tris(1,4-dithiane)bis(silver nitrate)' _chemical_formula_moiety 'C12 H24 Ag2 S6 2+, 2(N O3 -)' _chemical_formula_sum 'C12 H24 Ag2 N2 O6 S6' _chemical_formula_weight 700.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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)/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 12.395(3) _cell_length_b 12.575(2) _cell_length_c 14.335(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.561(4) _cell_angle_gamma 90.00 _cell_volume 2230.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5824 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.7 _exptl_crystal_description 'triangular prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_T_max 0.802 _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 13574 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.68 _reflns_number_total 5220 _reflns_number_gt 3544 _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^)+(0.0219P)^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_number_reflns 5220 _refine_ls_number_parameters 272 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.894 _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 -0.53311(2) -0.08504(3) 0.77796(2) 0.03203(10) Uani 1 1 d . . . Ag2 Ag 0.01184(2) -0.24710(3) 0.57001(2) 0.02686(9) Uani 1 1 d . . . S1 S -0.39843(8) -0.17240(8) 0.67470(8) 0.0245(2) Uani 1 1 d . . . C2 C -0.2999(3) -0.2278(3) 0.7597(3) 0.0303(10) Uani 1 1 d . A . H2A H -0.2794 -0.1731 0.8072 0.036 Uiso 1 1 calc R . . H2B H -0.3327 -0.2882 0.7919 0.036 Uiso 1 1 calc R . . C3 C -0.1991(3) -0.2658(3) 0.7147(3) 0.0269(10) Uani 1 1 d . . . H3A H -0.2204 -0.3135 0.6618 0.032 Uiso 1 1 calc R A . H3B H -0.1538 -0.3073 0.7609 0.032 Uiso 1 1 calc R . . S4 S -0.12075(8) -0.15693(8) 0.67274(7) 0.0229(2) Uani 1 1 d . A . C5 C -0.2186(3) -0.1012(3) 0.5872(3) 0.0251(9) Uani 1 1 d . . . H5A H -0.1854 -0.0403 0.5559 0.030 Uiso 1 1 calc R A . H5B H -0.2376 -0.1556 0.5390 0.030 Uiso 1 1 calc R . . C6 C -0.3211(3) -0.0640(3) 0.6301(3) 0.0264(9) Uani 1 1 d . A . H6A H -0.3666 -0.0251 0.5823 0.032 Uiso 1 1 calc R . . H6B H -0.3015 -0.0140 0.6817 0.032 Uiso 1 1 calc R . . S11 S 0.21355(8) -0.26840(8) 0.59174(8) 0.0244(2) Uani 1 1 d . A . C12 C 0.2772(3) -0.1413(3) 0.5734(3) 0.0291(10) Uani 1 1 d . . . H12A H 0.3560 -0.1487 0.5873 0.035 Uiso 1 1 calc R A . H12B H 0.2653 -0.1216 0.5067 0.035 Uiso 1 1 calc R . . C13 C 0.2358(3) -0.0524(3) 0.6326(3) 0.0290(10) Uani 1 1 d . A . H13A H 0.1563 -0.0475 0.6212 0.035 Uiso 1 1 calc R . . H13B H 0.2672 0.0156 0.6125 0.035 Uiso 1 1 calc R . . S14 S 0.26724(8) -0.06895(8) 0.75649(8) 0.0254(2) Uani 1 1 d . . . C15 C 0.2071(3) -0.1978(3) 0.7762(3) 0.0275(10) Uani 1 1 d . A . H15A H 0.2224 -0.2176 0.8425 0.033 Uiso 1 1 calc R . . H15B H 0.1277 -0.1915 0.7652 0.033 Uiso 1 1 calc R . . C16 C 0.2463(3) -0.2863(3) 0.7154(3) 0.0280(10) Uani 1 1 d . . . H16A H 0.2143 -0.3542 0.7353 0.034 Uiso 1 1 calc R A . H16B H 0.3257 -0.2924 0.7259 0.034 Uiso 1 1 calc R . . C20 C -0.0425(4) -0.5269(3) 0.5987(3) 0.0312(10) Uani 1 1 d . . . H20A H -0.0521 -0.5142 0.6659 0.037 Uiso 1 1 calc R A . H20B H -0.0809 -0.5936 0.5809 0.037 Uiso 1 1 calc R . . S21 S -0.10403(8) -0.41869(9) 0.53199(8) 0.0311(3) Uani 1 1 d . A . C22 C -0.0760(3) -0.4585(3) 0.4147(3) 0.0298(10) Uani 1 1 d . . . H22A H -0.1141 -0.5261 0.3996 0.036 Uiso 1 1 calc R A . H22B H -0.1052 -0.4039 0.3702 0.036 Uiso 1 1 calc R . . C30 C -0.4637(3) 0.1071(3) 0.9540(3) 0.0218(9) Uani 1 1 d . . . H30A H -0.4169 0.1341 1.0073 0.026 Uiso 1 1 calc R . . H30B H -0.4617 0.1598 0.9028 0.026 Uiso 1 1 calc R . . S31 S -0.40751(8) -0.01736(8) 0.91457(7) 0.0201(2) Uani 1 1 d . . . C32 C -0.4224(3) -0.0998(3) 1.0163(3) 0.0231(9) Uani 1 1 d . . . H32A H -0.3965 -0.1724 1.0029 0.028 Uiso 1 1 calc R . . H32B H -0.3757 -0.0711 1.0689 0.028 Uiso 1 1 calc R . . N1 N -0.4970(3) 0.1416(3) 0.6368(3) 0.0271(8) Uani 1 1 d . . . O1 O -0.4934(2) 0.1116(2) 0.7208(2) 0.0316(7) Uani 1 1 d . . . O2 O -0.5569(3) 0.0968(4) 0.5786(3) 0.0740(13) Uani 1 1 d . . . O3 O -0.4386(3) 0.2157(3) 0.6138(2) 0.0497(9) Uani 1 1 d . . . N2 N 0.0117(2) -0.1331(2) 0.3821(2) 0.0362(9) Uani 1 1 d D . . O6 O 0.0115(3) -0.0902(3) 0.3052(2) 0.0581(10) Uani 1 1 d D A . O4 O 0.0261(6) -0.0736(4) 0.4534(3) 0.054(3) Uani 0.442(7) 1 d PD A 1 O5 O -0.0078(7) -0.2257(4) 0.3945(4) 0.055(3) Uani 0.442(7) 1 d PD A 1 O4' O 0.1015(4) -0.1419(5) 0.4264(4) 0.060(2) Uani 0.558(7) 1 d PD A 2 O5' O -0.0676(4) -0.1745(5) 0.4126(3) 0.043(2) Uani 0.558(7) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02188(16) 0.0437(2) 0.0305(2) -0.01177(17) 0.00176(14) -0.00095(15) Ag2 0.02154(15) 0.03064(17) 0.02842(19) -0.00195(15) 0.00160(13) 0.00162(14) S1 0.0206(5) 0.0275(5) 0.0254(6) -0.0082(5) 0.0027(4) -0.0022(4) C2 0.030(2) 0.034(2) 0.028(3) 0.003(2) 0.007(2) 0.0006(19) C3 0.026(2) 0.024(2) 0.031(2) 0.0078(19) 0.0038(19) 0.0041(18) S4 0.0211(5) 0.0238(5) 0.0238(6) -0.0020(5) 0.0021(4) -0.0007(4) C5 0.027(2) 0.023(2) 0.025(2) 0.0065(19) 0.0044(18) 0.0032(17) C6 0.027(2) 0.024(2) 0.028(2) 0.0014(19) 0.0029(19) 0.0039(18) S11 0.0204(5) 0.0230(5) 0.0298(6) -0.0050(5) 0.0015(4) 0.0003(4) C12 0.027(2) 0.034(2) 0.027(2) 0.004(2) 0.0030(19) -0.0056(19) C13 0.032(2) 0.022(2) 0.033(3) 0.0040(19) -0.003(2) -0.0023(18) S14 0.0228(5) 0.0251(5) 0.0284(6) -0.0058(5) 0.0016(4) 0.0005(4) C15 0.024(2) 0.032(2) 0.026(2) 0.002(2) 0.0024(19) -0.0014(18) C16 0.028(2) 0.021(2) 0.035(3) 0.004(2) -0.001(2) -0.0013(17) C20 0.049(3) 0.027(2) 0.019(2) -0.0025(19) 0.011(2) -0.012(2) S21 0.0236(5) 0.0300(6) 0.0401(7) -0.0115(5) 0.0049(5) -0.0004(5) C22 0.039(3) 0.026(2) 0.023(2) 0.0032(19) -0.009(2) -0.0023(19) C30 0.030(2) 0.018(2) 0.018(2) 0.0018(17) 0.0040(17) -0.0004(17) S31 0.0210(5) 0.0211(5) 0.0182(5) -0.0010(4) 0.0026(4) 0.0003(4) C32 0.029(2) 0.020(2) 0.020(2) 0.0012(18) 0.0014(18) 0.0027(17) N1 0.0268(19) 0.0270(19) 0.028(2) -0.0031(18) 0.0026(17) 0.0057(16) O1 0.0400(18) 0.0307(17) 0.0249(18) 0.0079(14) 0.0079(14) -0.0018(13) O2 0.058(2) 0.120(4) 0.043(2) -0.025(2) -0.0066(19) -0.045(2) O3 0.070(2) 0.0413(19) 0.038(2) 0.0159(17) 0.0046(18) -0.0184(18) N2 0.037(2) 0.039(2) 0.030(2) 0.003(2) -0.0114(19) -0.0039(19) O6 0.062(2) 0.066(2) 0.046(2) 0.033(2) -0.0010(19) -0.011(2) O4 0.043(5) 0.049(5) 0.069(6) 0.021(5) -0.007(4) -0.011(4) O5 0.103(8) 0.021(4) 0.040(5) 0.011(4) -0.007(5) -0.013(5) O4' 0.051(4) 0.059(5) 0.065(5) -0.005(4) -0.026(4) 0.012(4) O5' 0.054(4) 0.046(4) 0.029(4) 0.005(3) 0.001(3) -0.020(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 S14 2.4829(12) 1_455 y Ag1 S1 2.5478(11) . y Ag1 S31 2.5699(11) . y Ag1 O1 2.661(3) . y Ag2 S11 2.5145(12) . y Ag2 O5 2.527(6) . y Ag2 S4 2.5409(11) . y Ag2 O5' 2.572(5) . y Ag2 S21 2.6302(11) . y Ag2 O4' 2.740(5) . y Ag2 O4 2.761(6) . y S1 C6 1.806(4) . ? S1 C2 1.810(4) . ? C2 C3 1.518(5) . ? C3 S4 1.803(4) . ? S4 C5 1.811(4) . ? C5 C6 1.519(5) . ? S11 C16 1.808(4) . ? S11 C12 1.809(4) . ? C12 C13 1.512(5) . ? C13 S14 1.806(4) . ? S14 C15 1.812(4) . ? S14 Ag1 2.4829(12) 1_655 ? C15 C16 1.512(6) . ? C20 C22 1.504(6) 3_546 ? C20 S21 1.805(4) . ? S21 C22 1.809(4) . ? C22 C20 1.504(6) 3_546 ? C30 C32 1.502(5) 3_457 ? C30 S31 1.817(4) . ? S31 C32 1.808(4) . ? C32 C30 1.502(5) 3_457 ? N1 O2 1.220(4) . ? N1 O3 1.237(4) . ? N1 O1 1.260(4) . ? N2 O5 1.205(4) . ? N2 O5' 1.218(4) . ? N2 O6 1.226(3) . ? N2 O4' 1.253(4) . ? N2 O4 1.271(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 S14 Ag1 S1 130.32(4) 1_455 . y S14 Ag1 S31 128.27(4) 1_455 . y S1 Ag1 S31 101.40(4) . . y S14 Ag1 O1 95.04(7) 1_455 . y S1 Ag1 O1 94.69(7) . . y S31 Ag1 O1 79.16(7) . . y S11 Ag2 O5 99.7(2) . . y S11 Ag2 S4 130.52(4) . . y O5 Ag2 S4 120.3(2) . . y S11 Ag2 O5' 118.03(11) . . y O5 Ag2 O5' 23.23(17) . . y S4 Ag2 O5' 97.11(14) . . y S11 Ag2 S21 117.66(3) . . y O5 Ag2 S21 82.17(12) . . y S4 Ag2 S21 96.99(4) . . y O5' Ag2 S21 86.27(12) . . y S11 Ag2 O4' 72.41(9) . . y O5 Ag2 O4' 38.64(17) . . y S4 Ag2 O4' 121.81(13) . . y O5' Ag2 O4' 47.22(12) . . y S21 Ag2 O4' 118.83(12) . . y S11 Ag2 O4 93.35(16) . . y O5 Ag2 O4 47.07(13) . . y S4 Ag2 O4 93.79(14) . . y O5' Ag2 O4 39.12(15) . . y S21 Ag2 O4 125.29(11) . . y O4' Ag2 O4 28.28(16) . . y C6 S1 C2 100.22(19) . . ? C6 S1 Ag1 105.17(13) . . ? C2 S1 Ag1 102.36(14) . . ? C3 C2 S1 111.9(3) . . ? C2 C3 S4 112.1(3) . . ? C3 S4 C5 99.65(19) . . ? C3 S4 Ag2 103.62(13) . . ? C5 S4 Ag2 102.13(13) . . ? C6 C5 S4 112.7(3) . . ? C5 C6 S1 112.8(3) . . ? C16 S11 C12 100.33(19) . . ? C16 S11 Ag2 107.20(14) . . ? C12 S11 Ag2 109.08(14) . . ? C13 C12 S11 113.9(3) . . ? C12 C13 S14 114.0(3) . . ? C13 S14 C15 100.96(19) . . ? C13 S14 Ag1 106.49(14) . 1_655 ? C15 S14 Ag1 108.91(14) . 1_655 ? C16 C15 S14 114.8(3) . . ? C15 C16 S11 114.4(3) . . ? C22 C20 S21 114.1(3) 3_546 . ? C20 S21 C22 100.65(19) . . ? C20 S21 Ag2 107.54(14) . . ? C22 S21 Ag2 106.58(14) . . ? C20 C22 S21 113.5(3) 3_546 . ? C32 C30 S31 114.9(3) 3_457 . ? C32 S31 C30 100.52(18) . . ? C32 S31 Ag1 109.72(13) . . ? C30 S31 Ag1 107.24(13) . . ? C30 C32 S31 114.1(3) 3_457 . ? O2 N1 O3 120.4(4) . . ? O2 N1 O1 120.0(4) . . ? O3 N1 O1 119.6(4) . . ? N1 O1 Ag1 125.2(2) . . ? O5 N2 O5' 50.2(4) . . ? O5 N2 O6 124.7(3) . . ? O5' N2 O6 123.7(3) . . ? O5 N2 O4' 91.1(4) . . ? O5' N2 O4' 119.4(3) . . ? O6 N2 O4' 116.5(3) . . ? O5 N2 O4 118.0(3) . . ? O5' N2 O4 92.2(4) . . ? O6 N2 O4 117.2(3) . . ? O4' N2 O4 64.3(4) . . ? N2 O4 Ag2 90.6(3) . . ? N2 O5 Ag2 104.0(3) . . ? N2 O4' Ag2 92.0(3) . . ? N2 O5' Ag2 101.2(3) . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.06 _refine_diff_density_min -1.17 _refine_diff_density_rms 0.12 data_14OTF2 _database_code_CSD 156908 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(1,4-dithiacyclohexane)bis(silver triflate) ; _chemical_name_common tris(1,4-dithiane)bis(silver triflate) _chemical_formula_moiety 'C7 H12 Ag F3 O3 S4' _chemical_formula_sum 'C7 H12 Ag F3 O3 S4' _chemical_formula_weight 437.28 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 12.874(2) _cell_length_b 10.994(2) _cell_length_c 18.678(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.801(3) _cell_angle_gamma 90.00 _cell_volume 2619.2(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6406 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29.5 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 2.208 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68910 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _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 8101 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 29.43 _reflns_number_total 3426 _reflns_number_gt 2986 _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^)+(0.0799P)^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 'geometrically located' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3426 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.116250(14) 0.47703(2) 0.204531(11) 0.01930(11) Uani 1 1 d . . . S1 S 0.13917(5) 0.28293(7) 0.27401(4) 0.02101(16) Uani 1 1 d . . . C2 C 0.1462(2) 0.1562(3) 0.21370(16) 0.0234(6) Uani 1 1 d . . . H2A H 0.1565 0.0808 0.2428 0.028 Uiso 1 1 calc R . . H2B H 0.0782 0.1490 0.1821 0.028 Uiso 1 1 calc R . . C3 C 0.2327(2) 0.1652(3) 0.16643(16) 0.0229(5) Uani 1 1 d . . . H3A H 0.2236 0.2415 0.1382 0.027 Uiso 1 1 calc R . . H3B H 0.2256 0.0966 0.1318 0.027 Uiso 1 1 calc R . . S4 S 0.36354(5) 0.16265(6) 0.21646(4) 0.02041(16) Uani 1 1 d . . . C5 C 0.3561(2) 0.2924(3) 0.27497(15) 0.0204(5) Uani 1 1 d . . . H5A H 0.4243 0.3019 0.3060 0.024 Uiso 1 1 calc R . . H5B H 0.3442 0.3664 0.2448 0.024 Uiso 1 1 calc R . . C6 C 0.2706(2) 0.2830(3) 0.32253(15) 0.0213(5) Uani 1 1 d . . . H6A H 0.2775 0.3521 0.3568 0.026 Uiso 1 1 calc R . . H6B H 0.2811 0.2072 0.3512 0.026 Uiso 1 1 calc R . . S7 S -0.00935(5) 0.47876(6) 0.09027(4) 0.01969(17) Uani 1 1 d . . . C8 C 0.0465(2) 0.3741(3) 0.03083(15) 0.0211(5) Uani 1 1 d . . . H8A H 0.1212 0.3948 0.0302 0.025 Uiso 1 1 calc R . . H8B H 0.0432 0.2905 0.0500 0.025 Uiso 1 1 calc R . . C9 C 0.0106(2) 0.6219(3) 0.04578(14) 0.0206(5) Uani 1 1 d . . . H9A H -0.0147 0.6894 0.0740 0.025 Uiso 1 1 calc R . . H9B H 0.0865 0.6341 0.0446 0.025 Uiso 1 1 calc R . . S10 S 0.35774(5) 0.46169(6) 0.09297(4) 0.01975(16) Uani 1 1 d . . . O1 O 0.26880(17) 0.4881(2) 0.13056(13) 0.0265(5) Uani 1 1 d . . . O2 O 0.45737(19) 0.4827(3) 0.13525(15) 0.0391(6) Uani 1 1 d . . . O3 O 0.3477(2) 0.3524(2) 0.05159(15) 0.0395(6) Uani 1 1 d . . . C10 C 0.3462(2) 0.5811(3) 0.02481(16) 0.0237(6) Uani 1 1 d . . . F1 F 0.41685(15) 0.5734(2) -0.01985(12) 0.0443(6) Uani 1 1 d . . . F2 F 0.25244(15) 0.5750(3) -0.01523(12) 0.0474(6) Uani 1 1 d . . . F3 F 0.3538(2) 0.6904(2) 0.05430(14) 0.0527(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.01880(14) 0.02036(16) 0.01821(16) 0.00059(7) 0.00055(9) 0.00021(6) S1 0.0179(3) 0.0216(3) 0.0239(4) 0.0045(3) 0.0043(2) 0.0023(2) C2 0.0202(11) 0.0206(13) 0.0280(15) 0.0005(11) -0.0023(10) -0.0047(10) C3 0.0248(12) 0.0222(13) 0.0205(13) -0.0002(11) -0.0017(9) 0.0013(10) S4 0.0195(3) 0.0211(3) 0.0210(3) 0.0032(3) 0.0044(2) 0.0020(2) C5 0.0184(11) 0.0197(13) 0.0218(13) 0.0005(10) -0.0018(9) -0.0020(9) C6 0.0206(11) 0.0249(14) 0.0174(13) 0.0007(10) -0.0012(9) 0.0025(10) S7 0.0165(3) 0.0250(4) 0.0171(4) -0.0002(2) 0.0005(2) -0.0003(2) C8 0.0201(11) 0.0203(13) 0.0216(13) -0.0001(10) -0.0023(9) 0.0036(9) C9 0.0226(12) 0.0206(13) 0.0173(13) -0.0019(10) -0.0013(9) 0.0016(10) S10 0.0178(3) 0.0229(3) 0.0193(4) 0.0034(2) 0.0053(2) 0.0025(2) O1 0.0242(10) 0.0303(12) 0.0275(13) 0.0048(9) 0.0124(9) 0.0006(8) O2 0.0222(11) 0.0653(19) 0.0284(14) 0.0112(11) -0.0019(9) 0.0002(10) O3 0.0553(15) 0.0219(12) 0.0444(16) -0.0036(11) 0.0179(12) 0.0038(10) C10 0.0197(11) 0.0282(15) 0.0243(15) 0.0074(11) 0.0070(10) 0.0043(10) F1 0.0375(10) 0.0597(15) 0.0421(12) 0.0249(11) 0.0279(9) 0.0209(10) F2 0.0237(9) 0.0701(16) 0.0451(13) 0.0290(12) -0.0069(8) 0.0021(10) F3 0.0862(18) 0.0232(11) 0.0546(16) 0.0029(10) 0.0312(13) -0.0050(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag S1 2.4941(8) . y Ag S4 2.5112(8) 4 y Ag S7 2.4966(8) . y Ag O1 2.553(2) . y S1 C2 1.802(3) . ? S1 C6 1.808(3) . ? C2 C3 1.515(4) . ? C3 S4 1.812(3) . ? S4 C5 1.807(3) . ? S4 Ag 2.5112(8) 4_545 ? C5 C6 1.509(4) . ? S7 C8 1.813(3) . ? S7 C9 1.814(3) . ? C8 C9 1.518(4) 5_565 ? C9 C8 1.518(4) 5_565 ? S10 O3 1.425(3) . ? S10 O2 1.431(2) . ? S10 O1 1.451(2) . ? S10 C10 1.821(3) . ? C10 F1 1.318(3) . ? C10 F3 1.319(4) . ? C10 F2 1.332(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ag S4 113.21(3) . 4 y S1 Ag S7 117.93(2) . . y S7 Ag S4 119.97(2) . 4 y S1 Ag O1 106.09(5) . . y S4 Ag O1 104.67(6) 4 . y S7 Ag O1 89.63(6) . . y C2 S1 C6 101.00(13) . . ? C2 S1 Ag 110.41(10) . . ? C6 S1 Ag 107.28(10) . . ? C3 C2 S1 114.6(2) . . ? C2 C3 S4 113.8(2) . . ? C5 S4 C3 100.25(13) . . ? C5 S4 Ag 107.20(10) . 4_545 ? C3 S4 Ag 109.28(10) . 4_545 ? C6 C5 S4 113.9(2) . . ? C5 C6 S1 114.38(19) . . ? C8 S7 C9 100.22(13) . . ? C8 S7 Ag 104.71(8) . . ? C9 S7 Ag 106.42(8) . . ? C9 C8 S7 112.20(18) 5_565 . ? C8 C9 S7 112.1(2) 5_565 . ? O3 S10 O2 116.36(18) . . ? O3 S10 O1 114.32(15) . . ? O2 S10 O1 114.05(16) . . ? O3 S10 C10 103.65(15) . . ? O2 S10 C10 104.55(15) . . ? O1 S10 C10 101.48(13) . . ? S10 O1 Ag 165.37(14) . . ? F1 C10 F3 107.7(3) . . ? F1 C10 F2 107.0(3) . . ? F3 C10 F2 106.9(3) . . ? F1 C10 S10 113.5(2) . . ? F3 C10 S10 111.7(2) . . ? F2 C10 S10 109.7(2) . . ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.856 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.170 data_14scn1 _database_code_CSD 156909 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4-dithiacyclohexane silver thiocyanate ; _chemical_name_common '1,4-dithiane silver thiocyanate' _chemical_formula_moiety 'C5 H8 Ag N S3' _chemical_formula_sum 'C5 H8 Ag N S3' _chemical_formula_weight 286.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 5.1248(3) _cell_length_b 13.0696(8) _cell_length_c 6.4077(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.046(4) _cell_angle_gamma 90.00 _cell_volume 412.46(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4677 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 280 _exptl_absorpt_coefficient_mu 3.122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.919 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details ? _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 'Enraf Nonius Kappa CCD' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time 10 _diffrn_standards_decay_% none _diffrn_reflns_number 4677 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.49 _reflns_number_total 988 _reflns_number_gt 825 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement ? _computing_data_reduction 'DENZO SCALEPACK' _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 _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^)+(0.0405P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'differnce 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_number_reflns 988 _refine_ls_number_parameters 52 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 0.11802(8) 0.2500 -0.00624(6) 0.02055(17) Uani 1 2 d S . . S1 S -0.22155(18) 0.39853(7) -0.00420(15) 0.0154(2) Uani 1 1 d . . . C2 C -0.0603(7) 0.4786(3) 0.2252(6) 0.0161(8) Uani 1 1 d . . . H2A H -0.1787 0.5383 0.2262 0.019 Uiso 1 1 calc R . . H2B H -0.0454 0.4394 0.3602 0.019 Uiso 1 1 calc R . . C3 C 0.2191(7) 0.5169(3) 0.2275(6) 0.0154(8) Uani 1 1 d . . . H3A H 0.3368 0.4573 0.2232 0.018 Uiso 1 1 calc R . . H3B H 0.2982 0.5535 0.3657 0.018 Uiso 1 1 calc R . . S4 S 0.5030(3) 0.2500 0.3506(2) 0.0192(3) Uani 1 2 d S . . C4 C 0.3443(11) 0.2500 0.5435(8) 0.0179(11) Uani 1 2 d S . . N4 N 0.2436(9) 0.2500 0.6838(8) 0.0254(11) Uani 1 2 d S . . 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 0.0261(3) 0.0167(3) 0.0200(3) 0.000 0.00840(19) 0.000 S1 0.0154(5) 0.0129(5) 0.0181(5) -0.0013(3) 0.0049(4) -0.0022(3) C2 0.0212(19) 0.0153(18) 0.0136(18) -0.0017(14) 0.0079(15) -0.0013(14) C3 0.0173(19) 0.0124(19) 0.0153(18) -0.0015(14) 0.0026(15) -0.0002(14) S4 0.0205(7) 0.0195(7) 0.0183(7) 0.000 0.0068(5) 0.000 C4 0.022(3) 0.012(3) 0.016(3) 0.000 -0.002(2) 0.000 N4 0.023(3) 0.031(3) 0.022(3) 0.000 0.007(2) 0.000 _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 N4 2.251(5) 1_554 y Ag S4 2.5743(15) . y Ag S1 2.6096(9) 4_565 ? Ag S1 2.6096(9) . y S1 C2 1.807(4) . ? S1 C3 1.811(3) 3_565 ? C2 C3 1.513(4) . ? C3 S1 1.811(3) 3_565 ? S4 C4 1.657(6) . ? C4 N4 1.154(7) . ? N4 Ag 2.251(5) 1_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag S4 116.61(12) 1_554 . y N4 Ag S1 110.99(8) 1_554 4_565 ? S4 Ag S1 110.12(3) . 4_565 ? N4 Ag S1 110.99(8) 1_554 . y S4 Ag S1 110.12(3) . . y S1 Ag S1 96.13(4) 4_565 . y C2 S1 C3 100.82(17) . 3_565 ? C2 S1 Ag 106.20(12) . . ? C3 S1 Ag 107.45(11) 3_565 . ? C3 C2 S1 114.7(2) . . ? C2 C3 S1 114.1(2) . 3_565 ? C4 S4 Ag 104.42(19) . . ? N4 C4 S4 177.3(5) . . ? C4 N4 Ag 170.5(4) . 1_556 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.57 _refine_diff_density_min -0.91 _refine_diff_density_rms 0.197 data_14so41 _database_code_CSD 156910 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(1,4-dithiacyclohexane) silver sulphate hydrate ; _chemical_name_common 'bis(1,4-dithiane) silver sulphate hydrate' _chemical_formula_moiety 'C4 H10 Ag2 O5 S3' _chemical_formula_sum 'C4 H10 Ag2 O5 S3' _chemical_formula_weight 450.04 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 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 9.655(2) _cell_length_b 14.749(2) _cell_length_c 6.9577(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 990.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 14 _cell_measurement_theta_max 16 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 4.574 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 0.752 _exptl_absorpt_process_details 'XRED (Stoe & Cie, 1997b)' _exptl_special_details ; bis(1,4-dithiacyclohexane) silver sulphate hydrate ; _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 'Stoe Stadi-4 four circle' _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 1461 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.99 _reflns_number_total 1009 _reflns_number_gt 900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (Stoe & Cie, 1997a)' _computing_cell_refinement STADI-4 _computing_data_reduction 'X-RED (Stoe & Cie, 1997b)' _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 _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^)+(0.0342P)^2^+2.3675P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'geometrically located' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1009 _refine_ls_number_parameters 75 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 1.205 _refine_ls_restrained_S_all 1.203 _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 0.73986(3) 0.62788(2) 0.15897(5) 0.01578(17) Uani 1 1 d . . . S1 S 0.54424(15) 0.7500 0.4257(2) 0.0098(3) Uani 1 2 d S . . C1 C 0.5307(5) 0.5403(3) -0.2090(6) 0.0120(9) Uani 1 1 d . . . H1A H 0.5678 0.5855 -0.3006 0.014 Uiso 1 1 calc R . . H1B H 0.4901 0.4901 -0.2847 0.014 Uiso 1 1 calc R . . C2 C 0.5826(5) 0.4157(3) 0.0893(6) 0.0129(9) Uani 1 1 d . . . H2A H 0.5411 0.3677 0.0082 0.015 Uiso 1 1 calc R . . H2B H 0.6505 0.3867 0.1762 0.015 Uiso 1 1 calc R . . S2 S 0.67225(11) 0.49626(7) -0.06408(15) 0.0119(3) Uani 1 1 d . . . O1 O 0.6957(5) 0.7500 0.3897(7) 0.0190(10) Uani 1 2 d S . . O2 O 0.4839(3) 0.6680(2) 0.3401(5) 0.0197(7) Uani 1 1 d . . . O3 O 0.5172(5) 0.7500 0.6359(6) 0.0152(10) Uani 1 2 d S . . O5 O 0.7262(5) 0.7500 -0.1021(7) 0.0180(10) Uani 1 2 d SD . . H5A H 0.673(5) 0.7500 -0.200(6) 0.027 Uiso 1 2 d SD . . H5B H 0.807(3) 0.7500 -0.150(8) 0.027 Uiso 1 2 d SD . . 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 0.0182(2) 0.0119(2) 0.0173(2) -0.00163(13) -0.00206(13) -0.00032(13) S1 0.0112(7) 0.0088(7) 0.0093(7) 0.000 -0.0002(6) 0.000 C1 0.017(2) 0.011(2) 0.0075(19) 0.0043(17) -0.0018(18) -0.0031(18) C2 0.018(2) 0.0089(19) 0.012(2) 0.0005(19) -0.0034(18) -0.0023(17) S2 0.0136(5) 0.0113(5) 0.0108(5) 0.0001(5) 0.0005(4) 0.0000(4) O1 0.013(2) 0.020(2) 0.024(3) 0.000 0.002(2) 0.000 O2 0.0218(17) 0.0162(17) 0.0211(17) -0.0082(14) 0.0003(14) -0.0065(14) O3 0.015(2) 0.023(3) 0.008(2) 0.000 0.0000(18) 0.000 O5 0.020(2) 0.021(2) 0.013(2) 0.000 -0.002(2) 0.000 _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 O1 2.450(3) . y Ag O2 2.429(3) 6_656 y Ag O5 2.561(3) . y Ag S2 2.5697(11) . y Ag S2 2.7902(11) 2_665 y S1 O2 1.468(3) 7_575 ? S1 O2 1.468(3) . ? S1 O1 1.484(5) . ? S1 O3 1.486(4) . ? C1 C2 1.520(6) 5_665 ? C1 S2 1.818(4) . ? C2 C1 1.520(6) 5_665 ? C2 S2 1.816(4) . ? S2 Ag 2.7902(11) 2_664 ? O1 Ag 2.450(3) 7_575 ? O2 Ag 2.429(3) 6_556 ? O5 Ag 2.561(3) 7_575 ? 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 Ag O1 89.30(14) 6_656 . y O2 Ag O5 83.14(13) 6_656 . y O1 Ag O5 86.49(13) . . y O2 Ag S2 115.60(9) 6_656 . y O1 Ag S2 155.08(11) . . y O5 Ag S2 95.15(8) . . y O2 Ag S2 82.14(8) 6_656 2_665 y O1 Ag S2 94.75(10) . 2_665 y O5 Ag S2 165.21(11) . 2_665 y S2 Ag S2 89.92(2) . 2_665 y O2 S1 O2 110.8(3) 7_575 . ? O2 S1 O1 108.83(18) 7_575 . ? O2 S1 O1 108.83(18) . . ? O2 S1 O3 109.24(17) 7_575 . ? O2 S1 O3 109.24(17) . . ? O1 S1 O3 109.8(3) . . ? C2 C1 S2 112.9(3) 5_665 . ? C1 C2 S2 112.7(3) 5_665 . ? C2 S2 C1 101.6(2) . . ? C2 S2 Ag 105.09(14) . . ? C1 S2 Ag 104.83(15) . . ? C2 S2 Ag 96.98(14) . 2_664 ? C1 S2 Ag 94.59(14) . 2_664 ? Ag S2 Ag 146.67(5) . 2_664 ? S1 O1 Ag 106.39(18) . 7_575 ? S1 O1 Ag 106.39(18) . . ? Ag O1 Ag 94.63(17) 7_575 . ? S1 O2 Ag 125.8(2) . 6_556 ? Ag O5 Ag 89.36(15) 7_575 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.592 _refine_diff_density_min -1.305 _refine_diff_density_rms 0.157