data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr J Rawson' _publ_contact_author_email JMR31@CAM.AC.UK loop_ _publ_author_name J.Rawson A.Alberola A.Bond R.D.Farley S.M.Humphrey ; G.D.McManus ; D.M.Murphy data_jr0331 _database_code_depnum_ccdc_archive 'CCDC 274884' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H2 N S3, H O4 S' _chemical_formula_sum 'C4 H3 N O4 S4' _chemical_formula_weight 257.31 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' _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 6.7711(3) _cell_length_b 16.1514(6) _cell_length_c 7.6578(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.331(3) _cell_angle_gamma 90.00 _cell_volume 836.06(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6033 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.113 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8781 _exptl_absorpt_correction_T_max 0.9781 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 6373 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1450 _reflns_number_gt 1244 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+1.4351P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1450 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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 S1 S 0.80922(15) 0.08849(7) 0.07437(14) 0.0271(3) Uani 1 1 d . . . S2 S 0.65602(15) -0.04901(6) 0.23096(14) 0.0263(3) Uani 1 1 d . . . S3 S 0.26835(16) 0.15372(6) 0.28483(16) 0.0311(3) Uani 1 1 d . . . N1 N 0.8287(5) -0.0075(2) 0.1259(5) 0.0271(8) Uani 1 1 d . . . C1 C 0.4706(6) 0.1776(3) 0.1762(6) 0.0291(10) Uani 1 1 d . . . H1 H 0.4993 0.2308 0.1313 0.035 Uiso 1 1 calc R . . C2 C 0.5877(6) 0.1086(2) 0.1626(5) 0.0231(9) Uani 1 1 d . . . C3 C 0.5057(6) 0.0369(2) 0.2438(5) 0.0222(9) Uani 1 1 d . . . C4 C 0.3288(6) 0.0526(2) 0.3162(6) 0.0249(9) Uani 1 1 d . . . H4 H 0.2522 0.0131 0.3747 0.030 Uiso 1 1 calc R . . S4 S 0.84575(15) 0.16288(6) 0.58192(13) 0.0232(3) Uani 1 1 d . . . O1 O 0.8239(5) 0.23996(19) 0.4854(4) 0.0340(8) Uani 1 1 d . . . O2 O 1.0021(4) 0.18087(19) 0.7371(4) 0.0316(7) Uani 1 1 d . . . H2A H 0.9472 0.2061 0.8170 0.047 Uiso 1 1 calc R . . O4 O 0.6640(4) 0.13912(18) 0.6581(4) 0.0326(7) Uani 1 1 d . . . O5 O 0.9338(5) 0.09782(18) 0.4848(4) 0.0316(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0188(6) 0.0294(6) 0.0336(6) 0.0031(4) 0.0076(4) -0.0008(4) S2 0.0215(6) 0.0241(6) 0.0342(6) 0.0034(4) 0.0087(4) 0.0029(4) S3 0.0203(6) 0.0244(6) 0.0494(7) 0.0001(4) 0.0101(5) 0.0016(4) N1 0.0172(17) 0.0304(19) 0.034(2) -0.0001(15) 0.0058(14) 0.0010(14) C1 0.020(2) 0.026(2) 0.042(3) 0.0045(18) 0.0071(19) -0.0037(17) C2 0.0143(19) 0.027(2) 0.028(2) 0.0005(16) 0.0017(16) -0.0015(16) C3 0.017(2) 0.023(2) 0.026(2) -0.0010(16) 0.0005(16) 0.0008(16) C4 0.019(2) 0.022(2) 0.034(2) 0.0010(16) 0.0037(17) -0.0006(16) S4 0.0208(6) 0.0218(5) 0.0277(6) 0.0000(4) 0.0078(4) 0.0000(4) O1 0.0361(18) 0.0286(16) 0.0384(18) 0.0089(13) 0.0120(14) 0.0035(13) O2 0.0226(16) 0.0390(17) 0.0332(17) -0.0048(13) 0.0023(13) 0.0018(13) O4 0.0226(17) 0.0270(15) 0.049(2) -0.0005(14) 0.0146(14) -0.0041(13) O5 0.0332(18) 0.0271(16) 0.0357(17) -0.0063(13) 0.0118(13) 0.0044(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 N1 1.603(4) . ? S1 C2 1.712(4) . ? S2 N1 1.604(4) . ? S2 C3 1.727(4) . ? S3 C1 1.688(4) . ? S3 C4 1.697(4) . ? C1 C2 1.375(6) . ? C1 H1 0.9500 . ? C2 C3 1.442(6) . ? C3 C4 1.373(6) . ? C4 H4 0.9500 . ? S4 O5 1.437(3) . ? S4 O4 1.444(3) . ? S4 O1 1.451(3) . ? S4 O2 1.572(3) . ? O2 H2A 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 S1 C2 98.52(19) . . ? N1 S2 C3 98.15(19) . . ? C1 S3 C4 95.4(2) . . ? S1 N1 S2 118.4(2) . . ? C2 C1 S3 109.9(3) . . ? C2 C1 H1 125.1 . . ? S3 C1 H1 125.1 . . ? C1 C2 C3 112.4(4) . . ? C1 C2 S1 134.9(3) . . ? C3 C2 S1 112.7(3) . . ? C4 C3 C2 113.1(4) . . ? C4 C3 S2 134.7(3) . . ? C2 C3 S2 112.2(3) . . ? C3 C4 S3 109.2(3) . . ? C3 C4 H4 125.4 . . ? S3 C4 H4 125.4 . . ? O5 S4 O4 113.82(18) . . ? O5 S4 O1 113.39(19) . . ? O4 S4 O1 111.70(19) . . ? O5 S4 O2 104.17(18) . . ? O4 S4 O2 107.23(18) . . ? O1 S4 O2 105.70(18) . . ? S4 O2 H2A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.566 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.123 data_jr9918 _database_code_depnum_ccdc_archive 'CCDC 274885' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H2 N O2 S4, As F6' _chemical_formula_sum 'C4 H2 As F6 N O2 S4' _chemical_formula_weight 413.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 15.7052(10) _cell_length_b 8.2312(6) _cell_length_c 10.9601(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1416.84(17) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 3.046 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7504 _exptl_absorpt_correction_T_max 0.8626 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Rigaku AFC-7R' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 2336 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2336 _reflns_number_gt 1812 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1343P)^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 mixed _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 0.52(3) _refine_ls_number_reflns 2336 _refine_ls_number_parameters 170 _refine_ls_number_restraints 98 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1900 _refine_ls_wR_factor_gt 0.1744 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 3.929 _refine_ls_shift/su_mean 0.172 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.4915(2) 0.3042(4) 0.1714(3) 0.0643(8) Uani 1 1 d . . . S2 S 0.4025(2) 0.4805(4) 0.3424(3) 0.0630(8) Uani 1 1 d . . . S3 S 0.63259(17) 0.7246(4) 0.2606(4) 0.0626(8) Uani 1 1 d . . . N1 N 0.4100(8) 0.3239(11) 0.2582(10) 0.074(3) Uani 1 1 d . . . C1 C 0.6163(7) 0.5403(14) 0.1782(10) 0.053(3) Uani 1 1 d . . . H1 H 0.6537 0.4956 0.1188 0.063 Uiso 1 1 calc R . . C2 C 0.5434(7) 0.4769(13) 0.2138(9) 0.054(3) Uani 1 1 d . . . C3 C 0.4975(7) 0.5725(13) 0.3033(9) 0.057(3) Uani 1 1 d . . . C4 C 0.5355(7) 0.7070(11) 0.3396(9) 0.045(2) Uani 1 1 d . . . H4 H 0.5141 0.7815 0.3983 0.054 Uiso 1 1 calc R . . As1 As 0.36921(5) 0.84528(10) 0.01257(12) 0.0480(4) Uani 1 1 d D . . F3 F 0.3230(8) 0.7768(13) 0.1414(9) 0.135(4) Uani 1 1 d D A . F5 F 0.4170(6) 0.9185(12) -0.1175(8) 0.121(4) Uani 1 1 d D A . F1 F 0.3863(18) 1.031(2) 0.0802(16) 0.093(2) Uiso 0.33 1 d PD A 1 F2 F 0.4659(11) 0.753(3) 0.043(2) 0.093(2) Uiso 0.33 1 d PD B 1 F4 F 0.2745(10) 0.929(3) -0.031(2) 0.093(2) Uiso 0.33 1 d PD A 1 F6 F 0.3504(18) 0.667(2) -0.065(2) 0.093(2) Uiso 0.33 1 d PD A 1 F1A F 0.2747(10) 0.830(4) -0.0628(15) 0.093(2) Uiso 0.33 1 d PD A 2 F2A F 0.3552(15) 1.0541(16) 0.016(3) 0.093(2) Uiso 0.33 1 d PD C 2 F4A F 0.3912(17) 0.6431(17) 0.028(3) 0.093(2) Uiso 0.33 1 d PD A 2 F6A F 0.4597(12) 0.883(4) 0.096(2) 0.093(2) Uiso 0.33 1 d PD A 2 F1B F 0.4338(15) 0.679(2) 0.003(2) 0.093(2) Uiso 0.33 1 d PD A 3 F6B F 0.3205(14) 1.027(2) 0.049(2) 0.093(2) Uiso 0.33 1 d PD A 3 F4B F 0.4285(17) 0.951(3) 0.1187(17) 0.093(2) Uiso 0.33 1 d PD A 3 F2B F 0.3060(17) 0.748(4) -0.0912(18) 0.093(2) Uiso 0.33 1 d PD A 3 O1S O 0.3883(4) 0.7261(9) 0.5010(10) 0.061(2) Uani 1 1 d . . . O2SA O 0.352(4) 0.994(9) 0.418(7) 0.127(5) Uiso 0.207(5) 1 d P . . O2SB O 0.2722(11) 0.8782(18) 0.6085(18) 0.127(5) Uiso 0.793(5) 1 d P . . S1SA S 0.3135(2) 0.8342(5) 0.4728(4) 0.0627(10) Uani 0.793(5) 1 d P D 1 S1SB S 0.3577(8) 0.9132(19) 0.5367(14) 0.0627(10) Uani 0.207(5) 1 d P D 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 S1 0.071(2) 0.0533(16) 0.0682(17) -0.0032(15) 0.0046(16) -0.0082(14) S2 0.0609(19) 0.0658(19) 0.0622(17) -0.0030(15) 0.0064(14) -0.0072(15) S3 0.0580(17) 0.0630(18) 0.0668(18) -0.0083(16) 0.0065(15) -0.0115(12) N1 0.097(8) 0.060(6) 0.065(7) -0.001(5) 0.006(7) -0.026(5) C1 0.047(6) 0.056(7) 0.055(7) 0.012(5) 0.010(5) 0.023(5) C2 0.064(7) 0.046(6) 0.052(6) -0.002(5) -0.007(5) 0.013(5) C3 0.055(6) 0.076(8) 0.041(5) 0.013(5) -0.001(5) 0.015(6) C4 0.070(7) 0.021(4) 0.044(5) -0.010(4) -0.007(5) -0.002(4) As1 0.0420(5) 0.0435(5) 0.0585(6) 0.0045(6) 0.0044(6) -0.0023(3) F3 0.172(10) 0.121(8) 0.112(8) 0.022(7) 0.073(7) -0.041(7) F5 0.154(9) 0.112(7) 0.096(6) 0.009(6) 0.060(7) -0.045(7) O1S 0.057(4) 0.059(4) 0.066(5) 0.004(5) -0.002(4) 0.011(3) S1SA 0.0445(18) 0.069(2) 0.074(2) 0.0219(16) -0.0044(15) 0.0025(15) S1SB 0.0445(18) 0.069(2) 0.074(2) 0.0219(16) -0.0044(15) 0.0025(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 N1 1.604(12) . ? S1 C2 1.703(12) . ? S2 N1 1.589(10) . ? S2 C3 1.728(12) . ? S3 C4 1.759(11) . ? S3 C1 1.785(13) . ? C1 C2 1.317(16) . ? C1 H1 0.9500 . ? C2 C3 1.449(14) . ? C3 C4 1.319(14) . ? C4 H4 0.9500 . ? As1 F3 1.685(7) . ? As1 F1A 1.703(14) . ? As1 F4A 1.708(13) . ? As1 F4 1.708(14) . ? As1 F2B 1.709(14) . ? As1 F1B 1.709(13) . ? As1 F6 1.718(14) . ? As1 F6A 1.720(14) . ? As1 F5 1.721(7) . ? As1 F1 1.722(14) . ? As1 F6B 1.727(14) . ? As1 F4B 1.726(14) . ? O1S S1SA 1.505(8) . ? O1S S1SB 1.660(17) . ? O2SA S1SB 1.47(7) . ? O2SA S1SA 1.57(7) . ? O2SB S1SB 1.58(2) . ? O2SB S1SA 1.66(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 S1 C2 97.8(5) . . ? N1 S2 C3 98.5(6) . . ? C4 S3 C1 93.1(5) . . ? S2 N1 S1 119.0(6) . . ? C2 C1 S3 108.1(8) . . ? C2 C1 H1 125.9 . . ? S3 C1 H1 125.9 . . ? C1 C2 C3 114.7(11) . . ? C1 C2 S1 131.7(9) . . ? C3 C2 S1 113.6(10) . . ? C4 C3 C2 115.8(11) . . ? C4 C3 S2 133.2(9) . . ? C2 C3 S2 111.0(9) . . ? C3 C4 S3 108.2(8) . . ? C3 C4 H4 125.8 . . ? S3 C4 H4 126.0 . . ? F3 As1 F1A 90.4(5) . . ? F3 As1 F4A 71.3(11) . . ? F1A As1 F4A 98.9(14) . . ? F3 As1 F4 89.6(9) . . ? F1A As1 F4 30.1(10) . . ? F4A As1 F4 126.7(12) . . ? F3 As1 F2B 98.7(9) . . ? F1A As1 F2B 30.4(11) . . ? F4A As1 F2B 74.1(15) . . ? F4 As1 F2B 59.9(14) . . ? F3 As1 F1B 92.1(5) . . ? F1A As1 F1B 115.5(14) . . ? F4A As1 F1B 26.3(9) . . ? F4 As1 F1B 145.6(14) . . ? F2B As1 F1B 85.9(15) . . ? F3 As1 F6 93.1(9) . . ? F1A As1 F6 63.2(13) . . ? F4A As1 F6 41.6(14) . . ? F4 As1 F6 93.3(13) . . ? F2B As1 F6 34.1(11) . . ? F1B As1 F6 52.3(14) . . ? F3 As1 F6A 88.3(10) . . ? F1A As1 F6A 172.6(15) . . ? F4A As1 F6A 87.6(14) . . ? F4 As1 F6A 142.6(13) . . ? F2B As1 F6A 157.0(15) . . ? F1B As1 F6A 71.8(13) . . ? F6 As1 F6A 124.1(15) . . ? F3 As1 F5 178.9(5) . . ? F1A As1 F5 90.2(5) . . ? F4A As1 F5 109.5(11) . . ? F4 As1 F5 90.4(8) . . ? F2B As1 F5 82.3(9) . . ? F1B As1 F5 88.4(6) . . ? F6 As1 F5 88.0(9) . . ? F6A As1 F5 91.0(9) . . ? F3 As1 F1 90.2(5) . . ? F1A As1 F1 114.1(15) . . ? F4A As1 F1 142.4(14) . . ? F4 As1 F1 84.0(13) . . ? F2B As1 F1 142.5(15) . . ? F1B As1 F1 130.3(15) . . ? F6 As1 F1 175.7(12) . . ? F6A As1 F1 58.6(13) . . ? F5 As1 F1 88.7(5) . . ? F3 As1 F6B 84.6(8) . . ? F1A As1 F6B 77.8(13) . . ? F4A As1 F6B 155.7(12) . . ? F4 As1 F6B 47.7(10) . . ? F2B As1 F6B 107.6(14) . . ? F1B As1 F6B 166.4(14) . . ? F6 As1 F6B 140.9(13) . . ? F6A As1 F6B 94.9(12) . . ? F5 As1 F6B 94.7(8) . . ? F1 As1 F6B 36.8(11) . . ? F3 As1 F4B 80.6(9) . . ? F1A As1 F4B 146.5(15) . . ? F4A As1 F4B 108.4(14) . . ? F4 As1 F4B 117.0(13) . . ? F2B As1 F4B 176.8(16) . . ? F1B As1 F4B 97.2(16) . . ? F6 As1 F4B 148.8(15) . . ? F6A As1 F4B 26.2(10) . . ? F5 As1 F4B 98.4(8) . . ? F1 As1 F4B 34.6(10) . . ? F6B As1 F4B 69.3(13) . . ? S1SA O1S S1SB 43.5(5) . . ? S1SB O2SA S1SA 46(2) . . ? S1SB O2SB S1SA 42.6(8) . . ? O1S S1SA O2SA 106(2) . . ? O1S S1SA O2SB 104.4(7) . . ? O2SA S1SA O2SB 108(3) . . ? O2SA S1SB O2SB 118(2) . . ? O2SA S1SB O1S 103(3) . . ? O2SB S1SB O1S 101.2(10) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.366 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.149 data_jr9917 _database_code_depnum_ccdc_archive 'CCDC 275393' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 Cl4 S3' _chemical_formula_weight 286.02 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5651(3) _cell_length_b 7.9392(2) _cell_length_c 8.6375(3) _cell_angle_alpha 109.214(2) _cell_angle_beta 103.151(2) _cell_angle_gamma 97.035(2) _cell_volume 465.91(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4337 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 280 _exptl_absorpt_coefficient_mu 1.869 _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 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3268 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.46 _reflns_number_total 2122 _reflns_number_gt 1955 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0052P)^2^+0.5570P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2122 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.173 _refine_ls_shift/su_max 0.229 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2763(3) 0.0354(3) 0.1861(3) 0.0226(5) Uani 1 1 d . . . C2 C 0.3392(3) 0.1726(3) 0.1371(3) 0.0210(4) Uani 1 1 d . . . C3 C 0.3111(3) 0.1108(3) -0.0454(3) 0.0210(4) Uani 1 1 d . . . C4 C 0.2281(3) -0.0705(3) -0.1236(3) 0.0223(5) Uani 1 1 d . . . S1 S 0.18172(9) -0.16950(8) 0.01683(8) 0.02594(16) Uani 1 1 d . . . S2 S 0.45030(8) 0.39190(8) 0.28327(8) 0.02708(16) Uani 1 1 d . . . S3 S 0.38226(8) 0.24748(9) -0.15163(8) 0.02698(16) Uani 1 1 d . . . Cl1 Cl 0.28379(10) 0.04728(9) 0.38785(8) 0.03490(18) Uani 1 1 d . . . Cl2 Cl 0.23725(10) 0.52639(9) 0.26888(9) 0.03959(19) Uani 1 1 d . . . Cl3 Cl 0.14549(9) 0.33462(10) -0.22507(10) 0.04096(19) Uani 1 1 d . . . Cl4 Cl 0.17056(10) -0.20072(9) -0.33574(7) 0.03472(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0229(11) 0.0261(11) 0.0184(11) 0.0070(9) 0.0056(9) 0.0075(9) C2 0.0206(11) 0.0228(11) 0.0190(11) 0.0063(9) 0.0051(9) 0.0070(9) C3 0.0220(11) 0.0240(11) 0.0190(11) 0.0084(9) 0.0070(9) 0.0087(9) C4 0.0245(11) 0.0259(11) 0.0160(10) 0.0059(9) 0.0056(9) 0.0088(9) S1 0.0295(3) 0.0231(3) 0.0241(3) 0.0086(2) 0.0069(2) 0.0037(2) S2 0.0261(3) 0.0240(3) 0.0236(3) 0.0018(2) 0.0035(2) 0.0050(2) S3 0.0265(3) 0.0335(3) 0.0283(3) 0.0173(3) 0.0113(2) 0.0096(3) Cl1 0.0447(4) 0.0434(4) 0.0211(3) 0.0151(3) 0.0125(3) 0.0109(3) Cl2 0.0405(4) 0.0316(3) 0.0414(4) 0.0053(3) 0.0088(3) 0.0172(3) Cl3 0.0323(4) 0.0533(4) 0.0520(4) 0.0353(4) 0.0117(3) 0.0176(3) Cl4 0.0436(4) 0.0334(3) 0.0178(3) 0.0007(2) 0.0048(3) 0.0073(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 C1 C2 1.364(3) . ? C1 Cl1 1.701(2) . ? C1 S1 1.723(2) . ? C2 C3 1.443(3) . ? C2 S2 1.745(2) . ? C3 C4 1.367(3) . ? C3 S3 1.746(2) . ? C4 Cl4 1.702(2) . ? C4 S1 1.722(2) . ? S2 Cl2 2.0423(9) . ? S3 Cl3 2.0407(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Cl1 127.60(19) . . ? C2 C1 S1 112.95(17) . . ? Cl1 C1 S1 119.45(14) . . ? C1 C2 C3 111.9(2) . . ? C1 C2 S2 122.61(18) . . ? C3 C2 S2 125.38(17) . . ? C4 C3 C2 111.3(2) . . ? C4 C3 S3 124.29(17) . . ? C2 C3 S3 124.40(17) . . ? C3 C4 Cl4 127.48(18) . . ? C3 C4 S1 113.26(17) . . ? Cl4 C4 S1 119.25(14) . . ? C4 S1 C1 90.59(11) . . ? C2 S2 Cl2 101.26(8) . . ? C3 S3 Cl3 101.34(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 C1 C2 C3 179.29(17) . . . . ? S1 C1 C2 C3 -0.2(2) . . . . ? Cl1 C1 C2 S2 2.3(3) . . . . ? S1 C1 C2 S2 -177.21(12) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? S2 C2 C3 C4 176.90(17) . . . . ? C1 C2 C3 S3 -177.61(17) . . . . ? S2 C2 C3 S3 -0.7(3) . . . . ? C2 C3 C4 Cl4 -179.44(17) . . . . ? S3 C3 C4 Cl4 -1.8(3) . . . . ? C2 C3 C4 S1 0.2(2) . . . . ? S3 C3 C4 S1 177.84(12) . . . . ? C3 C4 S1 C1 -0.29(18) . . . . ? Cl4 C4 S1 C1 179.39(15) . . . . ? C2 C1 S1 C4 0.29(18) . . . . ? Cl1 C1 S1 C4 -179.27(15) . . . . ? C1 C2 S2 Cl2 -98.99(19) . . . . ? C3 C2 S2 Cl2 84.45(19) . . . . ? C4 C3 S3 Cl3 87.7(2) . . . . ? C2 C3 S3 Cl3 -94.99(19) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.798 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.084