# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2163 data_s92 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H6 Br1.50 I1.50 O4 S3' _chemical_formula_weight 560.51 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.8163(3) _cell_length_b 8.7676(4) _cell_length_c 14.8481(9) _cell_angle_alpha 77.310(2) _cell_angle_beta 83.073(2) _cell_angle_gamma 84.686(2) _cell_volume 731.58(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used na _cell_measurement_theta_min na _cell_measurement_theta_max na _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 7.765 _exptl_absorpt_correction_type 'Multiscan, SORTAV' _exptl_absorpt_correction_T_min 0.3057 _exptl_absorpt_correction_T_max 0.3057 _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 'Enraf Nonius FR591 Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number 'not measured' _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% na _diffrn_reflns_number 5844 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2518 _reflns_number_gt 2333 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; DENZO and COLLECT ; _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material CIFTAB _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^)+(0.0796P)^2^+9.9956P] 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 0.0073(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2518 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1574 _refine_ls_wR_factor_gt 0.1539 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.007 _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 I1 I 0.05293(10) 0.94784(7) 0.63443(4) 0.0248(3) Uani 1 1 d . . . I2 I -0.17057(12) 0.57608(8) 0.54769(5) 0.0211(3) Uani 0.50 1 d P . . Br2 Br -0.17057(12) 0.57608(8) 0.54769(5) 0.0211(3) Uani 0.50 1 d P . . Br1 Br 0.41872(18) 0.74290(12) 0.68185(8) 0.0346(3) Uani 1 1 d . . . S1 S -0.3073(4) 1.1366(3) 0.58928(17) 0.0281(6) Uani 1 1 d . . . S2 S -0.6453(4) 1.3126(3) 0.69981(18) 0.0273(6) Uani 1 1 d . . . S3 S -0.2792(4) 1.1157(3) 0.79239(17) 0.0271(6) Uani 1 1 d . . . C1 C -0.4047(17) 1.1840(11) 0.6909(7) 0.026(2) Uani 1 1 d . . . O1 O -1.0001(11) 1.4513(8) 0.8166(5) 0.0257(15) Uani 1 1 d . . . O2 O -0.7613(12) 1.4835(8) 0.9187(5) 0.0320(16) Uani 1 1 d . . . O3 O -0.2212(12) 1.1806(8) 0.9745(5) 0.0297(15) Uani 1 1 d . . . C4 C -0.8069(17) 1.4247(11) 0.8586(7) 0.024(2) Uani 1 1 d . . . C3 C -0.4727(17) 1.2201(11) 0.8592(7) 0.025(2) Uani 1 1 d . . . C2 C -0.6372(16) 1.3131(11) 0.8146(7) 0.026(2) Uani 1 1 d . . . C6 C -0.4476(16) 1.1889(11) 0.9608(7) 0.025(2) Uani 1 1 d . . . O4 O -0.6055(12) 1.1670(9) 1.0210(5) 0.0314(16) Uani 1 1 d . . . C7 C -0.1746(17) 1.1398(13) 1.0738(8) 0.032(2) Uani 1 1 d . . . H7A H -0.2820 1.2032 1.1092 0.048 Uiso 1 1 calc R . . H7B H -0.0145 1.1610 1.0786 0.048 Uiso 1 1 calc R . . H7C H -0.1966 1.0285 1.0989 0.048 Uiso 1 1 calc R . . C5 C -1.1667(17) 1.5701(12) 0.8458(8) 0.030(2) Uani 1 1 d . . . H5A H -1.1925 1.5486 0.9138 0.045 Uiso 1 1 calc R . . H5B H -1.3139 1.5680 0.8203 0.045 Uiso 1 1 calc R . . H5C H -1.1058 1.6737 0.8230 0.045 Uiso 1 1 calc R . . 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 I1 0.0264(4) 0.0252(4) 0.0224(4) -0.0090(3) 0.0034(3) 0.0014(3) I2 0.0250(4) 0.0192(4) 0.0194(4) -0.0079(3) 0.0048(3) -0.0024(3) Br2 0.0250(4) 0.0192(4) 0.0194(4) -0.0079(3) 0.0048(3) -0.0024(3) Br1 0.0294(6) 0.0361(6) 0.0337(6) -0.0048(5) 0.0021(4) 0.0087(4) S1 0.0314(13) 0.0308(13) 0.0218(12) -0.0109(10) 0.0013(10) 0.0076(10) S2 0.0290(13) 0.0294(12) 0.0230(12) -0.0080(10) -0.0018(10) 0.0056(10) S3 0.0270(12) 0.0303(13) 0.0221(12) -0.0071(10) 0.0030(9) 0.0055(10) C1 0.026(5) 0.027(5) 0.023(5) -0.005(4) 0.002(4) 0.001(4) O1 0.024(3) 0.029(4) 0.024(4) -0.009(3) -0.001(3) 0.002(3) O2 0.031(4) 0.034(4) 0.032(4) -0.014(3) -0.002(3) 0.005(3) O3 0.025(4) 0.036(4) 0.027(4) -0.006(3) 0.002(3) -0.001(3) C4 0.028(5) 0.022(5) 0.021(5) -0.004(4) 0.002(4) 0.000(4) C3 0.024(5) 0.026(5) 0.026(5) -0.009(4) 0.005(4) -0.002(4) C2 0.022(5) 0.027(5) 0.028(5) -0.007(4) 0.003(4) -0.002(4) C6 0.021(5) 0.026(5) 0.028(5) -0.009(4) -0.001(4) 0.001(4) O4 0.022(4) 0.041(4) 0.027(4) -0.006(3) 0.004(3) 0.005(3) C7 0.021(5) 0.042(6) 0.030(6) -0.004(5) -0.003(4) -0.001(4) C5 0.022(5) 0.030(5) 0.038(6) -0.011(4) -0.005(4) 0.008(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 I1 S1 2.605(2) . ? I1 Br1 2.7107(11) . ? I2 Br2 2.7173(13) 2_566 ? I2 I2 2.7173(13) 2_566 ? S1 C1 1.673(10) . ? S2 C2 1.712(10) . ? S2 C1 1.725(10) . ? S3 C1 1.718(10) . ? S3 C3 1.740(10) . ? O1 C4 1.327(12) . ? O1 C5 1.457(11) . ? O2 C4 1.190(12) . ? O3 C6 1.350(12) . ? O3 C7 1.491(13) . ? C4 C2 1.518(13) . ? C3 C2 1.337(14) . ? C3 C6 1.496(14) . ? C6 O4 1.200(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 S1 I1 Br1 178.01(7) . . ? Br2 I2 I2 0.00(3) 2_566 2_566 ? C1 S1 I1 101.2(4) . . ? C2 S2 C1 95.9(5) . . ? C1 S3 C3 95.8(5) . . ? S1 C1 S3 124.8(6) . . ? S1 C1 S2 120.6(6) . . ? S3 C1 S2 114.6(5) . . ? C4 O1 C5 115.3(8) . . ? C6 O3 C7 114.7(7) . . ? O2 C4 O1 126.8(9) . . ? O2 C4 C2 122.9(9) . . ? O1 C4 C2 110.1(8) . . ? C2 C3 C6 126.9(9) . . ? C2 C3 S3 116.0(8) . . ? C6 C3 S3 116.9(7) . . ? C3 C2 C4 123.7(9) . . ? C3 C2 S2 117.6(8) . . ? C4 C2 S2 118.5(7) . . ? O4 C6 O3 125.2(9) . . ? O4 C6 C3 124.7(9) . . ? O3 C6 C3 110.1(8) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 3.535 _refine_diff_density_min -1.847 _refine_diff_density_rms 0.272