Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Johannes Beck' _publ_contact_author_email J.BECK@UNI-BONN.DE loop_ _publ_author_name J.Beck J.Daniels A.Roloff N.Wagner data_C4S6-I2 _database_code_depnum_ccdc_archive 'CCDC 281527' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3,6,7-Tetrathiapentalene-2,5-bisthione - diiodine ; _chemical_name_common '1,3,6,7-Tetrathiapentalene-2,5-bisthione - diiodine' _chemical_melting_point 227 _chemical_formula_moiety ? _chemical_formula_sum 'C4 I2 S6' _chemical_formula_weight 494.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 '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 15.443(4) _cell_length_b 9.9217(14) _cell_length_c 16.375(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.78(2) _cell_angle_gamma 90.00 _cell_volume 2239.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 54.142 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.0430 _exptl_absorpt_correction_T_max 0.4553 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2839 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.49 _diffrn_reflns_theta_max 53.96 _reflns_number_total 1359 _reflns_number_gt 1132 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR92(Giaccovazzo, 1993)' _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^)+(0.0848P)^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_number_reflns 1359 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.6424(2) 0.4938(3) 0.15203(19) 0.0421(7) Uani 1 1 d . . . S2 S 0.6397(2) 0.2022(3) 0.18573(18) 0.0376(7) Uani 1 1 d . . . S3 S 0.6543(3) 0.2954(3) 0.0218(2) 0.0522(8) Uani 1 1 d . . . S4 S 0.6255(2) 0.1071(3) 0.3742(2) 0.0429(7) Uani 1 1 d . . . S5 S 0.6255(2) 0.4022(3) 0.41328(18) 0.0377(7) Uani 1 1 d . . . S6 S 0.6325(2) 0.5565(3) 0.3306(2) 0.0430(7) Uani 1 1 d . . . C1 C 0.6371(8) 0.4468(12) 0.2514(8) 0.040(3) Uani 1 1 d . . . C2 C 0.6464(9) 0.3278(13) 0.1154(8) 0.045(3) Uani 1 1 d . . . C3 C 0.6363(8) 0.3103(11) 0.2675(7) 0.036(3) Uani 1 1 d . . . C4 C 0.6284(7) 0.2710(12) 0.3461(6) 0.031(3) Uani 1 1 d . . . I1 I 0.60628(5) 0.13706(7) 0.52895(5) 0.0363(3) Uani 1 1 d . . . I2 I 0.57903(6) 0.17167(8) 0.68960(5) 0.0453(3) 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 0.0629(19) 0.0342(16) 0.0405(16) 0.0000(13) 0.0332(15) -0.0024(13) S2 0.0528(17) 0.0324(16) 0.0344(15) -0.0028(13) 0.0257(14) -0.0052(12) S3 0.082(2) 0.0452(19) 0.0419(17) 0.0047(15) 0.0391(17) 0.0039(16) S4 0.0635(19) 0.0368(16) 0.0391(16) -0.0022(13) 0.0325(15) -0.0060(14) S5 0.0475(16) 0.0368(16) 0.0317(15) -0.0015(13) 0.0205(13) 0.0012(13) S6 0.0609(19) 0.0353(16) 0.0402(16) -0.0029(13) 0.0293(15) -0.0001(13) C1 0.046(7) 0.035(6) 0.044(7) -0.002(6) 0.025(6) 0.000(5) C2 0.056(8) 0.045(8) 0.039(7) 0.007(6) 0.026(6) 0.006(6) C3 0.039(6) 0.039(7) 0.027(6) -0.004(5) 0.013(5) -0.004(5) C4 0.019(5) 0.052(7) 0.020(5) -0.001(5) 0.007(5) -0.001(5) I1 0.0398(5) 0.0361(5) 0.0360(5) 0.0002(3) 0.0198(4) -0.0048(3) I2 0.0663(6) 0.0398(5) 0.0400(5) -0.0014(3) 0.0329(4) -0.0033(4) _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 C1 1.730(12) . ? S1 C2 1.764(13) . ? S2 C2 1.731(12) . ? S2 C3 1.734(11) . ? S3 C2 1.623(11) . ? S4 C4 1.696(12) . ? S4 I1 2.698(3) . ? S5 C4 1.718(11) . ? S5 S6 2.078(4) . ? S6 C1 1.719(12) . ? C1 C3 1.381(17) . ? C3 C4 1.402(14) . ? I1 I2 2.8657(12) . ? 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 C1 S1 C2 95.3(5) . . ? C2 S2 C3 95.8(6) . . ? C4 S4 I1 100.2(3) . . ? C4 S5 S6 96.7(4) . . ? C1 S6 S5 93.3(4) . . ? C3 C1 S6 118.0(9) . . ? C3 C1 S1 116.9(9) . . ? S6 C1 S1 125.1(7) . . ? S3 C2 S2 122.6(8) . . ? S3 C2 S1 122.3(7) . . ? S2 C2 S1 115.0(6) . . ? C1 C3 C4 117.4(10) . . ? C1 C3 S2 116.9(8) . . ? C4 C3 S2 125.6(9) . . ? C3 C4 S4 122.6(8) . . ? C3 C4 S5 114.5(9) . . ? S4 C4 S5 122.8(6) . . ? S4 I1 I2 178.02(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 53.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.017 _refine_diff_density_min -1.804 _refine_diff_density_rms 0.296 data_a,b-C4S6 _database_code_depnum_ccdc_archive 'CCDC 281528' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3,6,7-Tetrathiapentalene-2,5-bisthione ; _chemical_name_common 1,3,6,7-Tetrathiapentalene-2,5-bisthione _chemical_melting_point 199 _chemical_formula_moiety C4S6 _chemical_formula_sum 'C4 S6' _chemical_formula_weight 240.40 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.6437(12) _cell_length_b 10.4593(12) _cell_length_c 9.9010(12) _cell_angle_alpha 90.00 _cell_angle_beta 105.92(3) _cell_angle_gamma 90.00 _cell_volume 761.21(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 1.702 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.70784 _exptl_absorpt_correction_T_max 0.89600 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius Bruker kappa CCD' _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 17444 _diffrn_reflns_av_R_equivalents 0.0969 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 24.37 _reflns_number_total 1224 _reflns_number_gt 1116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack(Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0030P)^2^+4.6799P] 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 0.0077(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1224 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.309 _refine_ls_restrained_S_all 1.309 _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 0.9014(2) 0.10008(15) 0.17899(16) 0.0248(4) Uani 1 1 d . . . S2 S 0.7626(2) 0.16195(15) -0.11950(16) 0.0254(4) Uani 1 1 d . . . S3 S 0.9531(3) 0.36141(16) 0.07409(19) 0.0367(5) Uani 1 1 d . . . S4 S 0.5285(3) -0.06085(16) -0.33298(17) 0.0347(5) Uani 1 1 d . . . S5 S 0.5858(2) -0.22090(15) -0.07641(17) 0.0272(4) Uani 1 1 d . . . S6 S 0.7329(2) -0.16846(15) 0.12453(16) 0.0274(4) Uani 1 1 d . . . C1 C 0.7811(8) -0.0181(6) 0.0709(6) 0.0208(13) Uani 1 1 d . . . C2 C 0.8771(8) 0.2157(6) 0.0465(6) 0.0244(14) Uani 1 1 d . . . C3 C 0.7179(8) 0.0107(6) -0.0674(6) 0.0228(14) Uani 1 1 d . . . C4 C 0.6156(8) -0.0807(6) -0.1628(6) 0.0236(14) 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 0.0308(9) 0.0212(8) 0.0212(8) -0.0006(6) 0.0048(7) -0.0020(7) S2 0.0325(9) 0.0221(9) 0.0216(8) 0.0016(7) 0.0075(7) -0.0037(7) S3 0.0522(11) 0.0238(9) 0.0305(9) 0.0009(8) 0.0053(8) -0.0121(8) S4 0.0533(11) 0.0259(9) 0.0198(9) -0.0002(7) 0.0014(8) -0.0017(8) S5 0.0341(9) 0.0213(9) 0.0249(9) -0.0012(7) 0.0059(7) -0.0059(7) S6 0.0363(9) 0.0222(9) 0.0224(8) 0.0033(7) 0.0062(7) -0.0041(7) C1 0.026(3) 0.018(3) 0.019(3) -0.001(3) 0.009(3) 0.004(3) C2 0.020(3) 0.026(4) 0.024(3) 0.001(3) 0.002(3) 0.001(3) C3 0.024(3) 0.021(3) 0.028(3) -0.002(3) 0.016(3) -0.004(3) C4 0.027(3) 0.020(3) 0.025(3) 0.000(3) 0.010(3) 0.001(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 S1 C1 1.726(6) . ? S1 C2 1.756(6) . ? S2 C3 1.727(6) . ? S2 C2 1.730(6) . ? S3 C2 1.627(6) . ? S4 C4 1.646(6) . ? S5 C4 1.744(6) . ? S5 S6 2.073(2) . ? S6 C1 1.731(6) . ? C1 C3 1.355(8) . ? C3 C4 1.419(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C2 95.8(3) . . ? C3 S2 C2 96.0(3) . . ? C4 S5 S6 98.0(2) . . ? C1 S6 S5 92.9(2) . . ? C3 C1 S1 116.7(5) . . ? C3 C1 S6 117.7(5) . . ? S1 C1 S6 125.6(3) . . ? S3 C2 S2 121.9(4) . . ? S3 C2 S1 124.0(4) . . ? S2 C2 S1 114.1(4) . . ? C1 C3 C4 120.1(6) . . ? C1 C3 S2 117.4(5) . . ? C4 C3 S2 122.5(5) . . ? C3 C4 S4 126.2(5) . . ? C3 C4 S5 111.2(4) . . ? S4 C4 S5 122.5(4) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 24.37 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.444 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.107 data_a,a-C4S6 _database_code_depnum_ccdc_archive 'CCDC 281529' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,3-dithiolo-(4,5-d)-1,3-dithol-2,5-dithione ; _chemical_name_common 1,3-dithiolo-(4,5-d)-1,3-dithol-2,5-dithione _chemical_melting_point 280 _chemical_formula_moiety C4S6 _chemical_formula_sum C4S6 _chemical_formula_weight 240.40 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.8050(2) _cell_length_b 6.6377(3) _cell_length_c 10.4310(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.546(2) _cell_angle_gamma 90.00 _cell_volume 392.33(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour light-brown _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 240 _exptl_absorpt_coefficient_mu 1.651 _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 293(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 'Nonius Bruker kappa CCD' _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 10403 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 27.53 _reflns_number_total 895 _reflns_number_gt 807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack(Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0297P)^2^+0.2442P] 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 895 _refine_ls_number_parameters 46 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.19514(8) -0.18527(7) -0.02019(5) 0.03485(15) Uani 1 1 d . . . S2 S 0.66919(8) -0.20625(8) 0.14632(5) 0.03634(15) Uani 1 1 d . . . S3 S 0.31473(9) -0.51273(8) 0.17749(5) 0.04509(17) Uani 1 1 d . . . C1 C 0.3901(3) 0.0048(3) -0.03849(17) 0.0315(4) Uani 1 1 d . . . C2 C 0.3901(3) -0.3117(3) 0.10390(17) 0.0317(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 S1 0.0294(2) 0.0369(3) 0.0365(3) 0.00373(18) 0.00327(19) -0.00655(17) S2 0.0310(3) 0.0384(3) 0.0366(3) 0.00973(19) 0.00098(19) -0.00308(18) S3 0.0448(3) 0.0393(3) 0.0507(3) 0.0123(2) 0.0092(2) -0.0069(2) C1 0.0308(8) 0.0320(9) 0.0314(8) 0.0015(7) 0.0056(7) -0.0038(7) C2 0.0333(9) 0.0321(9) 0.0304(8) -0.0007(7) 0.0084(7) -0.0012(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 S1 C1 1.7329(18) . ? S1 C2 1.7389(18) . ? S2 C2 1.7321(18) . ? S2 C1 1.7330(19) 3_655 ? S3 C2 1.6452(18) . ? C1 C1 1.353(4) 3_655 ? C1 S2 1.7330(19) 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 C1 S1 C2 95.65(9) . . ? C2 S2 C1 95.92(9) . 3_655 ? C1 C1 S1 117.02(19) 3_655 . ? C1 C1 S2 116.76(19) 3_655 3_655 ? S1 C1 S2 126.22(11) . 3_655 ? S3 C2 S2 122.50(11) . . ? S3 C2 S1 122.88(11) . . ? S2 C2 S1 114.61(10) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.412 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.057