# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2220 # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF, VERSION DEC95) data_global _publ_contact_letter ; Please find below 4 data set(s) in CIF format for our manuscript Thank you very much! ; _publ_contact_author ; Dr Ulrich Fl\"orke Anorganische und Analytische Chemie Universit\"at Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; _publ_contact_author_email uf@chemie.uni-paderborn.de _publ_contact_author_fax '+49 5251 60 3423' _publ_contact_author_phone '+49 5251 60 2496' _publ_section_title ; The syntheses of novel sulfur centred spirocyclic cluster complexes starting from Re~2~(\m-H)(\m-SH)(CO)~8~. ; loop_ _publ_author_name _publ_author_address 'Egold, Hans' ;Fachbereich Chemie und Chemietechnik Universit\"at Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; 'Schwarze, Detlef' ;Fachbereich Chemie und Chemietechnik Universit\"at Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; 'Schraa, Markus' ;Fachbereich Chemie und Chemietechnik Universit\"at Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; 'Fl\"orke, Ulrich' ;Fachbereich Chemie und Chemietechnik Universit\"at Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H2 O16 Re4 S' _chemical_formula_sum 'C16 H2 O16 Re4 S' _chemical_formula_weight 1227.04 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' 'Re' 'Re' -1.0185 7.2310 '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 17.424(2) _cell_length_b 9.424(1) _cell_length_c 16.739(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.03(2) _cell_angle_gamma 90.00 _cell_volume 2547.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.074 _cell_measurement_theta_max 22.319 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_density_diffrn 3.199 _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 19.096 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.247 _exptl_absorpt_correction_T_max 0.676 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 2 _diffrn_reflns_number 3606 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2932 _reflns_number_gt 2074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00032(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2932 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _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 Re1 Re 0.07104(2) 0.55649(5) 0.21484(2) 0.03458(13) Uani 1 1 d . . . Re2 Re -0.06437(2) 0.14739(5) 0.15506(2) 0.03634(14) Uani 1 1 d . . . S1 S 0.0000 0.3518(4) 0.2500 0.0327(7) Uani 1 2 d S . . O1 O 0.1925(4) 0.4099(9) 0.1464(5) 0.057(2) Uani 1 1 d . . . C1 C 0.1471(6) 0.4629(12) 0.1714(6) 0.040(2) Uani 1 1 d . . . O2 O -0.0634(6) 0.5676(13) 0.0294(5) 0.094(4) Uani 1 1 d . . . C2 C -0.0148(6) 0.5664(13) 0.0972(7) 0.046(3) Uani 1 1 d . . . O3 O 0.2132(5) 0.5426(12) 0.3965(6) 0.086(3) Uani 1 1 d . . . C3 C 0.1602(7) 0.5483(14) 0.3325(8) 0.053(3) Uani 1 1 d . . . O4 O 0.1291(5) 0.8551(10) 0.1868(7) 0.081(3) Uani 1 1 d . . . C4 C 0.1088(6) 0.7428(12) 0.1977(7) 0.042(2) Uani 1 1 d . . . O5 O 0.0733(6) 0.1261(12) 0.0783(6) 0.088(3) Uani 1 1 d . . . C5 C 0.0247(7) 0.1361(14) 0.1086(6) 0.054(3) Uani 1 1 d . . . O6 O -0.2083(5) 0.1739(11) 0.2219(6) 0.079(3) Uani 1 1 d . . . C6 C -0.1559(6) 0.1626(13) 0.1995(7) 0.048(3) Uani 1 1 d . . . O7 O -0.1269(6) -0.1504(11) 0.0843(6) 0.077(3) Uani 1 1 d . . . C7 C -0.1042(7) -0.0395(14) 0.1082(7) 0.055(3) Uani 1 1 d . . . O8 O -0.1701(5) 0.2867(11) -0.0164(5) 0.082(3) Uani 1 1 d . . . C8 C -0.1308(6) 0.2382(13) 0.0495(6) 0.047(3) Uani 1 1 d . . . H1 H 0.0000 0.663(14) 0.2500 0.080 Uiso 1 2 d S . . H2 H 0.0000 0.040(16) 0.2500 0.080 Uiso 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 Re1 0.02957(19) 0.0328(2) 0.0412(2) 0.0009(2) 0.01301(15) -0.00116(18) Re2 0.0336(2) 0.0333(3) 0.0389(2) -0.0029(2) 0.00994(16) -0.00206(18) S1 0.0283(14) 0.0279(19) 0.0392(17) 0.000 0.0095(13) 0.000 O1 0.049(4) 0.062(6) 0.066(5) -0.011(5) 0.029(4) 0.008(4) C1 0.039(5) 0.039(6) 0.043(6) -0.003(5) 0.015(4) -0.007(5) O2 0.084(6) 0.145(11) 0.039(5) 0.003(6) 0.006(4) 0.035(7) C2 0.049(6) 0.042(7) 0.049(6) 0.009(6) 0.020(5) 0.005(6) O3 0.053(5) 0.115(9) 0.063(5) -0.006(6) -0.010(4) 0.007(6) C3 0.047(6) 0.052(8) 0.060(7) 0.006(7) 0.020(5) 0.000(6) O4 0.081(6) 0.040(5) 0.135(8) 0.019(6) 0.055(6) -0.006(5) C4 0.038(5) 0.029(6) 0.063(7) 0.000(6) 0.024(5) 0.008(5) O5 0.089(6) 0.101(9) 0.100(7) 0.005(7) 0.066(6) 0.009(6) C5 0.061(6) 0.065(9) 0.035(5) 0.001(6) 0.018(5) -0.006(7) O6 0.050(4) 0.086(8) 0.112(7) -0.008(6) 0.042(5) -0.008(5) C6 0.042(5) 0.042(7) 0.048(6) -0.003(6) 0.001(5) 0.002(6) O7 0.102(7) 0.052(6) 0.076(6) -0.015(5) 0.032(5) -0.014(6) C7 0.052(6) 0.043(8) 0.062(7) -0.009(7) 0.013(5) -0.015(6) O8 0.074(5) 0.087(8) 0.058(5) 0.015(6) -0.006(4) 0.002(6) C8 0.043(5) 0.052(8) 0.035(5) 0.001(6) 0.004(4) 0.002(6) _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 Re1 C4 1.933(11) . ? Re1 C1 1.946(10) . ? Re1 C2 1.979(11) . ? Re1 C3 2.001(12) . ? Re1 S1 2.479(3) . ? Re1 Re1 3.1145(8) 2 ? Re2 C8 1.913(10) . ? Re2 C7 1.947(13) . ? Re2 C5 1.983(11) . ? Re2 C6 2.002(12) . ? Re2 S1 2.482(3) . ? Re2 Re2 3.1282(11) 2 ? S1 Re1 2.479(3) 2 ? S1 Re2 2.482(3) 2 ? O1 C1 1.139(11) . ? O2 C2 1.133(11) . ? O3 C3 1.122(12) . ? O4 C4 1.152(13) . ? O5 C5 1.143(12) . ? O6 C6 1.116(12) . ? O7 C7 1.135(14) . ? O8 C8 1.152(11) . ? 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 C4 Re1 C1 92.2(4) . . ? C4 Re1 C2 88.9(5) . . ? C1 Re1 C2 90.9(4) . . ? C4 Re1 C3 90.0(5) . . ? C1 Re1 C3 87.9(4) . . ? C2 Re1 C3 178.4(4) . . ? C4 Re1 S1 165.8(3) . . ? C1 Re1 S1 101.9(3) . . ? C2 Re1 S1 90.8(3) . . ? C3 Re1 S1 90.5(3) . . ? C4 Re1 Re1 114.8(3) . 2 ? C1 Re1 Re1 153.0(3) . 2 ? C2 Re1 Re1 88.0(3) . 2 ? C3 Re1 Re1 93.5(3) . 2 ? S1 Re1 Re1 51.08(6) . 2 ? C8 Re2 C7 91.8(5) . . ? C8 Re2 C5 87.3(4) . . ? C7 Re2 C5 90.3(5) . . ? C8 Re2 C6 91.2(4) . . ? C7 Re2 C6 90.1(5) . . ? C5 Re2 C6 178.5(5) . . ? C8 Re2 S1 102.5(4) . . ? C7 Re2 S1 165.4(4) . . ? C5 Re2 S1 93.5(4) . . ? C6 Re2 S1 86.4(3) . . ? C8 Re2 Re2 153.3(4) . 2 ? C7 Re2 Re2 114.9(4) . 2 ? C5 Re2 Re2 91.7(3) . 2 ? C6 Re2 Re2 89.4(3) . 2 ? S1 Re2 Re2 50.93(6) . 2 ? Re1 S1 Re1 77.84(11) . 2 ? Re1 S1 Re2 126.726(16) . . ? Re1 S1 Re2 127.599(15) 2 . ? Re1 S1 Re2 127.599(15) . 2 ? Re1 S1 Re2 126.726(16) 2 2 ? Re2 S1 Re2 78.14(11) . 2 ? O1 C1 Re1 179.0(10) . . ? O2 C2 Re1 177.8(12) . . ? O3 C3 Re1 176.3(10) . . ? O4 C4 Re1 178.2(9) . . ? O5 C5 Re2 176.6(11) . . ? O6 C6 Re2 177.6(11) . . ? O7 C7 Re2 177.0(11) . . ? O8 C8 Re2 176.4(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.916 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.260 #=END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H2 O18 Os3 Re2 S, 0.5 C H Cl3' _chemical_formula_sum 'C18.50 H2.50 Cl1.50 O18 Os3 Re2 S' _chemical_formula_weight 1540.94 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 '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 35.480(9) _cell_length_b 11.534(2) _cell_length_c 16.023(6) _cell_angle_alpha 90.00 _cell_angle_beta 111.67(2) _cell_angle_gamma 90.00 _cell_volume 6094(3) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 6.956 _cell_measurement_theta_max 18.920 _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5416 _exptl_absorpt_coefficient_mu 20.657 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.109 _exptl_absorpt_correction_T_max 0.435 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 'less than 1' _diffrn_reflns_number 8059 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6999 _reflns_number_gt 4855 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000080(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6999 _refine_ls_number_parameters 406 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.315356(14) -0.43678(4) -0.14527(3) 0.01640(12) Uani 1 1 d . . . Os2 Os 0.393032(15) -0.54580(4) -0.06650(3) 0.01825(12) Uani 1 1 d . . . Os3 Os 0.327167(16) -0.63083(4) -0.02358(4) 0.02094(13) Uani 1 1 d . . . Re1 Re 0.378649(16) -0.21531(4) 0.09028(3) 0.01817(12) Uani 1 1 d D . . Re2 Re 0.412558(15) -0.17831(4) -0.06071(3) 0.01793(12) Uani 1 1 d D . . S1 S 0.37524(9) -0.3487(2) -0.0348(2) 0.0159(6) Uani 1 1 d . . . O1 O 0.2487(3) -0.5763(8) -0.2852(7) 0.039(3) Uani 1 1 d . . . C1 C 0.2747(4) -0.5252(12) -0.2318(9) 0.028(3) Uani 1 1 d . . . O2 O 0.2538(3) -0.3325(10) -0.0753(8) 0.052(3) Uani 1 1 d . . . C2 C 0.2765(5) -0.3703(13) -0.1032(9) 0.034(3) Uani 1 1 d . . . O3 O 0.3090(4) -0.2567(9) -0.2901(7) 0.047(3) Uani 1 1 d . . . C3 C 0.3122(4) -0.3234(13) -0.2344(10) 0.035(4) Uani 1 1 d . . . O4 O 0.4574(3) -0.4687(9) -0.1391(8) 0.045(3) Uani 1 1 d . . . C4 C 0.4323(4) -0.4920(11) -0.1144(10) 0.029(3) Uani 1 1 d . . . O5 O 0.3925(3) -0.7900(8) -0.1388(8) 0.047(3) Uani 1 1 d . . . C5 C 0.3918(4) -0.7002(11) -0.1113(10) 0.027(3) Uani 1 1 d . . . O6 O 0.4551(3) -0.6076(11) 0.1177(8) 0.057(3) Uani 1 1 d . . . C6 C 0.4324(5) -0.5846(12) 0.0509(11) 0.036(4) Uani 1 1 d . . . O7 O 0.3584(5) -0.8603(9) 0.0733(9) 0.073(5) Uani 1 1 d . . . C7 C 0.3479(5) -0.7733(12) 0.0398(9) 0.034(4) Uani 1 1 d . . . O8 O 0.2936(4) -0.7897(9) -0.1887(7) 0.049(3) Uani 1 1 d . . . C8 C 0.3060(4) -0.7252(11) -0.1323(9) 0.026(3) Uani 1 1 d . . . O9 O 0.3754(4) -0.5163(8) 0.1569(7) 0.041(3) Uani 1 1 d . . . C9 C 0.3573(4) -0.5482(11) 0.0871(9) 0.026(3) Uani 1 1 d . . . O10 O 0.2457(4) -0.6114(10) -0.0013(11) 0.078(5) Uani 1 1 d . . . C10 C 0.2764(5) -0.6167(12) -0.0115(12) 0.040(4) Uani 1 1 d . . . O11 O 0.3980(4) -0.0184(9) 0.2290(7) 0.046(3) Uani 1 1 d . . . C11 C 0.3905(5) -0.0922(11) 0.1785(9) 0.028(3) Uani 1 1 d . . . O12 O 0.3002(3) -0.0794(9) -0.0267(7) 0.042(3) Uani 1 1 d . . . C12 C 0.3289(5) -0.1297(12) 0.0136(9) 0.030(3) Uani 1 1 d . . . O13 O 0.4542(4) -0.3490(9) 0.2193(8) 0.057(4) Uani 1 1 d . . . C13 C 0.4270(4) -0.3023(12) 0.1711(10) 0.030(3) Uani 1 1 d . . . C14 C 0.3452(5) -0.2914(11) 0.1427(10) 0.030(3) Uani 1 1 d . . . O14 O 0.3231(3) -0.3311(10) 0.1737(8) 0.050(3) Uani 1 1 d . . . O15 O 0.3372(3) -0.0299(9) -0.1704(7) 0.041(3) Uani 1 1 d . . . C15 C 0.3631(4) -0.0875(12) -0.1302(9) 0.025(3) Uani 1 1 d . . . O16 O 0.4948(3) -0.2989(9) 0.0455(7) 0.046(3) Uani 1 1 d . . . C16 C 0.4639(5) -0.2590(11) 0.0067(11) 0.034(4) Uani 1 1 d . . . O17 O 0.4151(4) -0.2542(9) -0.2443(7) 0.044(3) Uani 1 1 d . . . C17 C 0.4150(4) -0.2282(12) -0.1760(10) 0.029(3) Uani 1 1 d . . . O18 O 0.4599(3) 0.0461(8) -0.0575(7) 0.043(3) Uani 1 1 d . . . C18 C 0.4430(4) -0.0383(11) -0.0590(10) 0.029(3) Uani 1 1 d . . . C100 C -0.0112(16) -0.554(3) -0.247(4) 0.108(14) Uani 0.50 1 d PDU . . Cl1 Cl 0.0000 -0.4109(8) -0.2500 0.125(4) Uani 1 2 d SDU . . Cl2 Cl 0.0220(3) -0.6186(7) -0.1537(6) 0.132(3) Uani 1 1 d DU . . H2 H 0.412(5) -0.135(14) 0.049(8) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0092(2) 0.0183(2) 0.0206(2) -0.0007(2) 0.0042(2) 0.00205(19) Os2 0.0098(2) 0.0163(2) 0.0281(3) -0.0009(2) 0.0064(2) 0.0023(2) Os3 0.0162(3) 0.0162(2) 0.0311(3) 0.0015(2) 0.0095(2) -0.0014(2) Re1 0.0183(3) 0.0159(2) 0.0199(2) -0.0001(2) 0.0067(2) 0.0002(2) Re2 0.0120(2) 0.0168(2) 0.0247(3) 0.0034(2) 0.0065(2) -0.0009(2) S1 0.0128(15) 0.0119(14) 0.0237(15) -0.0015(12) 0.0077(13) -0.0011(11) O1 0.024(6) 0.034(6) 0.050(7) -0.014(5) 0.001(5) -0.006(5) C1 0.027(8) 0.033(8) 0.035(8) -0.002(6) 0.023(7) 0.012(7) O2 0.042(7) 0.062(8) 0.067(8) -0.006(6) 0.039(7) 0.014(6) C2 0.032(9) 0.039(8) 0.023(7) -0.002(7) 0.001(7) -0.008(7) O3 0.056(8) 0.050(7) 0.039(6) 0.025(6) 0.022(6) 0.014(6) C3 0.024(8) 0.038(8) 0.038(9) -0.012(7) 0.006(7) 0.008(7) O4 0.032(6) 0.044(6) 0.075(8) 0.012(6) 0.037(6) 0.006(5) C4 0.026(8) 0.017(6) 0.049(9) 0.000(6) 0.018(7) -0.001(6) O5 0.038(7) 0.029(6) 0.062(7) -0.023(5) 0.003(6) 0.007(5) C5 0.009(6) 0.023(7) 0.049(9) -0.006(6) 0.011(6) 0.001(5) O6 0.030(7) 0.070(8) 0.049(7) 0.020(6) -0.010(6) 0.000(6) C6 0.030(9) 0.027(8) 0.052(10) -0.004(7) 0.018(8) 0.001(7) O7 0.096(11) 0.020(6) 0.069(9) 0.016(6) -0.011(8) -0.001(7) C7 0.037(9) 0.028(8) 0.027(7) -0.001(6) 0.001(7) 0.002(7) O8 0.055(8) 0.036(6) 0.046(7) -0.020(5) 0.007(6) -0.008(6) C8 0.025(8) 0.022(7) 0.028(7) 0.008(6) 0.007(6) -0.002(6) O9 0.060(8) 0.022(5) 0.036(6) 0.006(5) 0.009(6) 0.004(5) C9 0.033(8) 0.017(6) 0.029(7) 0.000(6) 0.011(7) 0.004(6) O10 0.043(8) 0.045(7) 0.171(15) -0.006(9) 0.069(10) 0.006(6) C10 0.032(9) 0.016(7) 0.074(12) 0.007(7) 0.023(9) 0.008(7) O11 0.068(9) 0.028(6) 0.041(6) -0.010(5) 0.019(6) -0.002(6) C11 0.040(9) 0.014(6) 0.024(7) 0.009(6) 0.006(7) -0.001(6) O12 0.033(6) 0.051(7) 0.041(6) -0.003(5) 0.012(5) 0.022(6) C12 0.038(9) 0.031(8) 0.032(8) 0.003(6) 0.023(7) 0.006(7) O13 0.042(8) 0.043(7) 0.064(8) 0.028(6) -0.005(7) 0.005(6) C13 0.028(8) 0.024(7) 0.038(8) 0.002(6) 0.012(7) -0.008(6) C14 0.035(9) 0.019(7) 0.041(8) 0.005(6) 0.019(8) 0.005(6) O14 0.047(7) 0.057(7) 0.067(8) 0.025(6) 0.045(7) 0.010(6) O15 0.007(5) 0.043(6) 0.065(7) 0.021(6) 0.002(5) 0.009(5) C15 0.017(7) 0.036(8) 0.030(7) 0.007(6) 0.019(6) -0.003(6) O16 0.029(6) 0.044(6) 0.050(7) 0.010(5) -0.003(5) 0.012(6) C16 0.048(10) 0.012(6) 0.056(10) 0.005(6) 0.037(9) 0.012(7) O17 0.066(8) 0.043(6) 0.032(6) 0.009(5) 0.030(6) 0.001(6) C17 0.017(7) 0.036(8) 0.037(8) 0.007(7) 0.011(6) 0.000(6) O18 0.016(5) 0.027(5) 0.072(8) 0.019(5) 0.001(5) -0.010(5) C18 0.005(6) 0.025(7) 0.057(10) -0.009(7) 0.012(6) 0.003(6) C100 0.11(3) 0.076(13) 0.12(2) -0.001(19) 0.02(2) -0.019(17) Cl1 0.071(6) 0.068(5) 0.206(11) 0.000 0.017(7) 0.000 Cl2 0.149(8) 0.123(6) 0.127(6) 0.028(5) 0.057(6) 0.025(6) _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 Os1 C1 1.888(15) . ? Os1 C2 1.905(17) . ? Os1 C3 1.909(16) . ? Os1 S1 2.430(3) . ? Os1 Os2 2.8637(10) . ? Os1 Os3 2.8956(9) . ? Os2 C5 1.914(13) . ? Os2 C4 1.926(14) . ? Os2 C6 1.936(17) . ? Os2 S1 2.462(3) . ? Os2 Os3 2.8431(9) . ? Os3 C10 1.888(16) . ? Os3 C7 1.929(14) . ? Os3 C9 1.948(14) . ? Os3 C8 1.954(14) . ? Re1 C14 1.903(14) . ? Re1 C11 1.936(14) . ? Re1 C13 1.995(15) . ? Re1 C12 2.001(15) . ? Re1 S1 2.494(3) . ? Re1 Re2 3.1036(11) . ? Re2 C18 1.938(13) . ? Re2 C17 1.967(15) . ? Re2 C16 1.974(16) . ? Re2 C15 1.994(14) . ? Re2 S1 2.489(3) . ? O1 C1 1.161(16) . ? O2 C2 1.142(18) . ? O3 C3 1.152(17) . ? O4 C4 1.129(16) . ? O5 C5 1.130(15) . ? O6 C6 1.108(17) . ? O7 C7 1.134(16) . ? O8 C8 1.127(15) . ? O9 C9 1.127(15) . ? O10 C10 1.162(18) . ? O11 C11 1.138(15) . ? O12 C12 1.140(16) . ? O13 C13 1.127(16) . ? C14 O14 1.166(16) . ? O15 C15 1.124(15) . ? O16 C16 1.139(17) . ? O17 C17 1.137(16) . ? O18 C18 1.139(15) . ? C100 Cl2 1.67(6) 2_554 ? C100 Cl2 1.70(4) . ? C100 Cl1 1.70(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 C1 Os1 C2 91.2(6) . . ? C1 Os1 C3 90.2(6) . . ? C2 Os1 C3 98.0(6) . . ? C1 Os1 S1 170.5(4) . . ? C2 Os1 S1 97.2(4) . . ? C3 Os1 S1 93.0(4) . . ? C1 Os1 Os2 115.9(4) . . ? C2 Os1 Os2 136.5(4) . . ? C3 Os1 Os2 114.3(4) . . ? S1 Os1 Os2 54.70(7) . . ? C1 Os1 Os3 87.6(4) . . ? C2 Os1 Os3 90.9(4) . . ? C3 Os1 Os3 170.9(4) . . ? S1 Os1 Os3 87.84(7) . . ? Os2 Os1 Os3 59.16(2) . . ? C5 Os2 C4 94.0(6) . . ? C5 Os2 C6 93.3(6) . . ? C4 Os2 C6 95.4(6) . . ? C5 Os2 S1 164.6(4) . . ? C4 Os2 S1 93.6(4) . . ? C6 Os2 S1 99.2(4) . . ? C5 Os2 Os3 82.1(4) . . ? C4 Os2 Os3 171.2(4) . . ? C6 Os2 Os3 92.7(5) . . ? S1 Os2 Os3 88.41(7) . . ? C5 Os2 Os1 111.0(4) . . ? C4 Os2 Os1 113.8(4) . . ? C6 Os2 Os1 139.5(4) . . ? S1 Os2 Os1 53.64(7) . . ? Os3 Os2 Os1 60.98(2) . . ? C10 Os3 C7 102.3(7) . . ? C10 Os3 C9 95.0(7) . . ? C7 Os3 C9 87.9(5) . . ? C10 Os3 C8 94.2(7) . . ? C7 Os3 C8 86.6(5) . . ? C9 Os3 C8 170.1(6) . . ? C10 Os3 Os2 153.5(4) . . ? C7 Os3 Os2 103.5(5) . . ? C9 Os3 Os2 80.1(4) . . ? C8 Os3 Os2 93.2(4) . . ? C10 Os3 Os1 95.5(4) . . ? C7 Os3 Os1 160.9(5) . . ? C9 Os3 Os1 97.4(4) . . ? C8 Os3 Os1 85.3(4) . . ? Os2 Os3 Os1 59.86(2) . . ? C14 Re1 C11 91.0(6) . . ? C14 Re1 C13 90.5(6) . . ? C11 Re1 C13 89.6(6) . . ? C14 Re1 C12 86.9(6) . . ? C11 Re1 C12 89.4(6) . . ? C13 Re1 C12 177.2(6) . . ? C14 Re1 S1 102.6(4) . . ? C11 Re1 S1 166.4(4) . . ? C13 Re1 S1 89.2(4) . . ? C12 Re1 S1 92.4(4) . . ? C14 Re1 Re2 153.2(4) . . ? C11 Re1 Re2 115.2(4) . . ? C13 Re1 Re2 95.0(4) . . ? C12 Re1 Re2 87.8(4) . . ? S1 Re1 Re2 51.40(7) . . ? C18 Re2 C17 92.2(6) . . ? C18 Re2 C16 89.4(6) . . ? C17 Re2 C16 91.4(6) . . ? C18 Re2 C15 86.6(5) . . ? C17 Re2 C15 88.0(5) . . ? C16 Re2 C15 175.9(5) . . ? C18 Re2 S1 169.8(4) . . ? C17 Re2 S1 97.9(4) . . ? C16 Re2 S1 88.6(4) . . ? C15 Re2 S1 95.5(4) . . ? C18 Re2 Re1 118.6(4) . . ? C17 Re2 Re1 148.9(4) . . ? C16 Re2 Re1 93.1(4) . . ? C15 Re2 Re1 89.6(3) . . ? S1 Re2 Re1 51.54(7) . . ? Os1 S1 Os2 71.66(8) . . ? Os1 S1 Re2 125.77(13) . . ? Os2 S1 Re2 120.13(12) . . ? Os1 S1 Re1 127.84(13) . . ? Os2 S1 Re1 142.70(13) . . ? Re2 S1 Re1 77.06(8) . . ? O1 C1 Os1 177.5(12) . . ? O2 C2 Os1 177.7(14) . . ? O3 C3 Os1 177.6(14) . . ? O4 C4 Os2 173.9(12) . . ? O5 C5 Os2 176.9(13) . . ? O6 C6 Os2 179.2(16) . . ? O7 C7 Os3 176.0(14) . . ? O8 C8 Os3 172.1(12) . . ? O9 C9 Os3 169.6(11) . . ? O10 C10 Os3 177.2(16) . . ? O11 C11 Re1 178.1(13) . . ? O12 C12 Re1 176.9(12) . . ? O13 C13 Re1 177.4(14) . . ? O14 C14 Re1 175.3(12) . . ? O15 C15 Re2 174.5(11) . . ? O16 C16 Re2 175.5(13) . . ? O17 C17 Re2 177.3(13) . . ? O18 C18 Re2 177.7(11) . . ? Cl2 C100 Cl2 119(3) 2_554 . ? Cl2 C100 Cl1 112(2) 2_554 . ? Cl2 C100 Cl1 111(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.997 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.367 #=END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H2 Fe2 O22 Re4 S2, C H Cl3' _chemical_formula_sum 'C23 H3 Cl3 Fe2 O22 Re4 S2' _chemical_formula_weight 1658.22 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.214(5) _cell_length_b 18.351(4) _cell_length_c 15.578(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.49(2) _cell_angle_gamma 90.00 _cell_volume 3875.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 47 _cell_measurement_theta_min 6.002 _cell_measurement_theta_max 20.716 _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'none' _exptl_crystal_density_diffrn 2.842 _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 13.568 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.089 _exptl_absorpt_correction_T_max 0.162 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 2 _diffrn_reflns_number 10562 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8891 _reflns_number_gt 6893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00123(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8891 _refine_ls_number_parameters 512 _refine_ls_number_restraints 664 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re -0.02920(3) -0.36322(2) 0.24174(2) 0.01683(10) Uani 1 1 d DU . . Re2 Re 0.13681(3) -0.466457(19) 0.34718(2) 0.01628(10) Uani 1 1 d DU . . Re3 Re 0.48182(3) -0.35057(2) 0.12954(3) 0.02098(11) Uani 1 1 d DU . . Re4 Re 0.48537(3) -0.40586(2) 0.31802(2) 0.02090(11) Uani 1 1 d DU . . Fe1 Fe 0.18795(10) -0.39821(7) 0.10439(8) 0.0162(3) Uani 1 1 d U . . Fe2 Fe 0.22386(10) -0.28014(7) 0.19326(9) 0.0172(3) Uani 1 1 d U . . S1 S 0.13926(16) -0.37799(12) 0.22708(14) 0.0146(4) Uani 1 1 d U . . S2 S 0.34183(17) -0.36290(12) 0.19339(15) 0.0171(4) Uani 1 1 d U . . O1 O -0.1285(7) -0.4922(5) 0.1185(6) 0.048(2) Uani 1 1 d U . . C1 C -0.0893(7) -0.4475(6) 0.1630(6) 0.0241(19) Uani 1 1 d U . . O2 O -0.2132(6) -0.3552(4) 0.3071(6) 0.039(2) Uani 1 1 d U . . C2 C -0.1443(7) -0.3583(5) 0.2837(7) 0.0228(19) Uani 1 1 d U . . O3 O -0.1358(6) -0.2718(5) 0.0772(6) 0.043(2) Uani 1 1 d U . . C3 C -0.0950(7) -0.3024(6) 0.1376(7) 0.028(2) Uani 1 1 d U . . O4 O 0.0584(7) -0.2255(5) 0.3585(6) 0.049(2) Uani 1 1 d U . . C4 C 0.0269(7) -0.2762(5) 0.3178(7) 0.0239(19) Uani 1 1 d U . . O5 O 0.0568(8) -0.5863(5) 0.2048(6) 0.051(2) Uani 1 1 d U . . C5 C 0.0805(8) -0.5416(5) 0.2548(7) 0.0235(19) Uani 1 1 d U . . C6 C 0.1953(8) -0.3896(6) 0.4385(7) 0.028(2) Uani 1 1 d U . . O6 O 0.2264(8) -0.3455(5) 0.4896(6) 0.060(3) Uani 1 1 d U . . O7 O 0.3241(6) -0.5584(4) 0.3824(6) 0.0365(19) Uani 1 1 d U . . C7 C 0.2574(7) -0.5215(5) 0.3693(7) 0.0244(19) Uani 1 1 d U . . O8 O 0.0751(6) -0.5594(4) 0.4856(5) 0.0344(18) Uani 1 1 d U . . C8 C 0.0993(7) -0.5243(5) 0.4339(6) 0.0177(17) Uani 1 1 d U . . O9 O 0.2282(7) -0.5551(4) 0.1057(7) 0.053(3) Uani 1 1 d U . . C9 C 0.2105(7) -0.4945(5) 0.1038(8) 0.027(2) Uani 1 1 d U . . O10 O 0.2218(6) -0.3513(5) -0.0629(5) 0.042(2) Uani 1 1 d U . . C10 C 0.2128(7) -0.3692(6) 0.0042(6) 0.024(2) Uani 1 1 d U . . O11 O -0.0197(6) -0.3998(6) -0.0023(5) 0.046(2) Uani 1 1 d U . . C11 C 0.0624(8) -0.3991(6) 0.0403(6) 0.027(2) Uani 1 1 d U . . O12 O 0.3096(7) -0.2127(5) 0.3719(6) 0.060(3) Uani 1 1 d U . . C12 C 0.2749(8) -0.2384(5) 0.3037(7) 0.029(2) Uani 1 1 d U . . O13 O 0.0464(6) -0.1923(4) 0.1204(7) 0.049(2) Uani 1 1 d U . . C13 C 0.1117(7) -0.2293(5) 0.1487(8) 0.030(2) Uani 1 1 d U . . O14 O 0.3082(8) -0.1846(5) 0.0860(8) 0.068(3) Uani 1 1 d U . . C14 C 0.2773(9) -0.2216(5) 0.1277(8) 0.033(2) Uani 1 1 d U . . O15 O 0.6801(6) -0.3619(5) 0.0893(7) 0.049(2) Uani 1 1 d U . . C15 C 0.6061(8) -0.3588(7) 0.1027(7) 0.032(2) Uani 1 1 d U . . O16 O 0.4159(6) -0.5023(5) 0.0413(6) 0.041(2) Uani 1 1 d U . . C16 C 0.4411(8) -0.4487(6) 0.0743(7) 0.027(2) Uani 1 1 d U . . O17 O 0.4006(7) -0.2697(6) -0.0505(7) 0.060(3) Uani 1 1 d U . . C17 C 0.4274(9) -0.3002(7) 0.0163(8) 0.038(2) Uani 1 1 d U . . O18 O 0.5439(9) -0.1983(5) 0.2134(8) 0.076(4) Uani 1 1 d U . . C18 C 0.5240(10) -0.2533(6) 0.1856(9) 0.042(3) Uani 1 1 d U . . O19 O 0.4195(6) -0.4288(5) 0.4853(5) 0.046(2) Uani 1 1 d U . . C19 C 0.4402(7) -0.4216(6) 0.4217(7) 0.027(2) Uani 1 1 d U . . O20 O 0.4387(8) -0.5657(5) 0.2483(6) 0.052(2) Uani 1 1 d U . . C20 C 0.4536(8) -0.5099(6) 0.2741(7) 0.028(2) Uani 1 1 d U . . O21 O 0.5368(9) -0.2507(5) 0.3994(7) 0.070(3) Uani 1 1 d U . . C21 C 0.5166(8) -0.3044(7) 0.3645(8) 0.034(2) Uani 1 1 d U . . O22 O 0.6920(6) -0.4536(6) 0.4263(6) 0.055(3) Uani 1 1 d U . . C22 C 0.6169(8) -0.4359(7) 0.3882(7) 0.035(2) Uani 1 1 d U . . H1 H 0.030(8) -0.411(6) 0.346(9) 0.080 Uiso 1 1 d D . . H2 H 0.541(11) -0.388(7) 0.235(4) 0.080 Uiso 1 1 d D . . C100 C 0.7538(8) 0.4052(5) 0.2504(7) 0.046(3) Uani 1 1 d DU . . H100 H 0.7888 0.3849 0.2089 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.8425(3) 0.4476(2) 0.3361(3) 0.0547(9) Uani 1 1 d DU . . Cl2 Cl 0.6666(3) 0.4642(3) 0.1873(3) 0.0817(14) Uani 1 1 d DU . . Cl3 Cl 0.7046(6) 0.3330(3) 0.2891(4) 0.152(3) Uani 1 1 d DU . . 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 Re1 0.01520(18) 0.02147(19) 0.01476(18) 0.00029(14) 0.00592(14) 0.00059(14) Re2 0.01713(19) 0.01902(18) 0.01278(17) 0.00080(13) 0.00462(14) -0.00098(14) Re3 0.01781(19) 0.0267(2) 0.0213(2) 0.00153(15) 0.01025(15) -0.00122(15) Re4 0.01507(19) 0.0300(2) 0.01673(19) 0.00144(15) 0.00339(14) -0.00196(15) Fe1 0.0168(6) 0.0208(6) 0.0112(6) -0.0012(5) 0.0045(5) -0.0003(5) Fe2 0.0202(7) 0.0149(6) 0.0187(6) 0.0002(5) 0.0089(5) 0.0001(5) S1 0.0153(10) 0.0165(10) 0.0128(10) -0.0004(8) 0.0056(8) -0.0004(8) S2 0.0164(10) 0.0185(10) 0.0179(10) 0.0008(8) 0.0074(8) 0.0009(9) O1 0.048(5) 0.053(5) 0.038(5) -0.023(4) 0.004(4) -0.016(4) C1 0.021(4) 0.031(4) 0.018(4) 0.004(3) 0.003(3) 0.000(4) O2 0.030(4) 0.046(5) 0.048(5) -0.006(4) 0.023(4) -0.005(4) C2 0.020(4) 0.022(5) 0.028(5) 0.004(4) 0.009(4) 0.002(4) O3 0.039(5) 0.047(5) 0.035(4) 0.014(4) 0.000(4) 0.008(4) C3 0.021(5) 0.028(5) 0.035(5) 0.006(4) 0.008(4) 0.009(4) O4 0.056(6) 0.043(5) 0.053(6) -0.023(4) 0.023(5) -0.006(4) C4 0.025(5) 0.023(4) 0.029(5) 0.003(3) 0.015(4) -0.005(3) O5 0.078(7) 0.037(5) 0.038(5) -0.021(4) 0.018(5) -0.017(5) C5 0.026(5) 0.024(4) 0.019(4) 0.001(3) 0.006(4) -0.002(4) C6 0.024(5) 0.038(5) 0.014(4) -0.001(4) -0.005(4) -0.008(4) O6 0.083(8) 0.054(6) 0.036(5) -0.019(4) 0.007(5) -0.028(5) O7 0.026(4) 0.025(4) 0.064(6) 0.010(4) 0.023(4) 0.001(3) C7 0.021(4) 0.022(4) 0.030(5) 0.010(4) 0.008(4) -0.002(3) O8 0.039(5) 0.044(4) 0.025(4) 0.017(3) 0.018(3) 0.003(4) C8 0.016(4) 0.019(4) 0.015(4) -0.005(3) -0.001(3) 0.002(3) O9 0.040(5) 0.025(4) 0.088(7) -0.004(4) 0.012(5) 0.002(4) C9 0.016(5) 0.023(4) 0.041(6) -0.005(4) 0.006(4) -0.003(3) O10 0.041(5) 0.072(6) 0.016(3) 0.003(4) 0.012(3) -0.005(4) C10 0.017(4) 0.038(5) 0.018(4) -0.001(4) 0.007(3) 0.007(4) O11 0.025(4) 0.089(7) 0.022(4) 0.001(4) 0.003(3) 0.004(4) C11 0.025(4) 0.039(6) 0.012(4) 0.001(4) 0.000(3) -0.003(4) O12 0.069(7) 0.064(6) 0.040(5) -0.031(5) 0.007(5) -0.015(5) C12 0.031(5) 0.023(5) 0.034(5) -0.010(4) 0.012(4) -0.006(4) O13 0.020(4) 0.036(5) 0.086(7) 0.026(5) 0.009(4) 0.008(3) C13 0.020(4) 0.018(4) 0.050(6) 0.005(4) 0.008(4) 0.001(3) O14 0.090(8) 0.029(4) 0.118(9) 0.040(5) 0.083(7) 0.019(5) C14 0.051(7) 0.013(4) 0.050(6) 0.006(4) 0.037(6) 0.007(4) O15 0.032(4) 0.064(6) 0.063(6) 0.006(5) 0.031(4) 0.000(4) C15 0.023(4) 0.050(7) 0.027(5) 0.001(5) 0.015(4) -0.004(4) O16 0.044(5) 0.042(4) 0.043(5) -0.019(4) 0.024(4) -0.007(4) C16 0.026(5) 0.033(4) 0.029(5) -0.005(4) 0.019(4) 0.001(4) O17 0.057(6) 0.079(7) 0.051(5) 0.039(5) 0.027(5) 0.014(5) C17 0.039(6) 0.042(6) 0.038(5) 0.011(4) 0.022(5) 0.002(5) O18 0.112(10) 0.046(5) 0.089(8) -0.029(6) 0.056(8) -0.036(6) C18 0.057(8) 0.034(5) 0.052(7) -0.004(4) 0.043(6) -0.017(5) O19 0.035(5) 0.081(6) 0.024(4) -0.005(4) 0.014(3) -0.018(5) C19 0.019(5) 0.038(6) 0.022(4) -0.002(4) 0.002(4) -0.003(4) O20 0.074(7) 0.034(4) 0.057(6) -0.008(4) 0.032(5) -0.012(5) C20 0.025(5) 0.031(4) 0.032(5) 0.002(4) 0.015(4) 0.001(4) O21 0.102(9) 0.051(6) 0.062(7) -0.030(5) 0.030(6) -0.036(6) C21 0.029(5) 0.044(5) 0.036(5) -0.011(5) 0.019(5) -0.017(4) O22 0.018(4) 0.107(8) 0.037(5) 0.030(5) 0.006(4) 0.010(5) C22 0.022(4) 0.065(7) 0.017(5) 0.005(5) 0.006(3) -0.003(4) C100 0.058(8) 0.048(7) 0.029(6) -0.001(5) 0.008(5) -0.006(5) Cl1 0.051(2) 0.055(2) 0.059(2) -0.0153(17) 0.0178(17) -0.0158(16) Cl2 0.060(3) 0.104(4) 0.078(3) 0.025(3) 0.017(2) 0.040(2) Cl3 0.185(7) 0.125(5) 0.092(4) 0.052(3) -0.037(4) -0.118(5) _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 Re1 C2 1.938(10) . ? Re1 C3 1.959(10) . ? Re1 C1 1.999(10) . ? Re1 C4 2.006(10) . ? Re1 S1 2.487(2) . ? Re1 Re2 3.0863(9) . ? Re2 C8 1.916(10) . ? Re2 C7 1.929(10) . ? Re2 C5 1.980(10) . ? Re2 C6 1.998(10) . ? Re2 S1 2.485(2) . ? Re3 C17 1.935(12) . ? Re3 C15 1.940(10) . ? Re3 C18 1.998(12) . ? Re3 C16 2.005(11) . ? Re3 S2 2.488(2) . ? Re3 Re4 3.0925(8) . ? Re4 C19 1.930(11) . ? Re4 C22 1.940(11) . ? Re4 C21 1.999(12) . ? Re4 C20 2.033(11) . ? Re4 S2 2.484(2) . ? Fe1 C11 1.764(10) . ? Fe1 C10 1.782(10) . ? Fe1 C9 1.797(10) . ? Fe1 S1 2.251(3) . ? Fe1 S2 2.303(3) . ? Fe1 Fe2 2.5392(19) . ? Fe2 C13 1.797(10) . ? Fe2 C14 1.800(10) . ? Fe2 C12 1.822(10) . ? Fe2 S2 2.262(3) . ? Fe2 S1 2.308(3) . ? O1 C1 1.110(12) . ? O2 C2 1.144(12) . ? O3 C3 1.101(12) . ? O4 C4 1.139(12) . ? O5 C5 1.112(12) . ? C6 O6 1.129(13) . ? O7 C7 1.134(12) . ? O8 C8 1.160(12) . ? O9 C9 1.137(12) . ? O10 C10 1.139(12) . ? O11 C11 1.156(12) . ? O12 C12 1.131(13) . ? O13 C13 1.128(12) . ? O14 C14 1.117(13) . ? O15 C15 1.133(13) . ? O16 C16 1.117(12) . ? O17 C17 1.141(14) . ? O18 C18 1.102(14) . ? O19 C19 1.124(13) . ? O20 C20 1.097(13) . ? O21 C21 1.121(14) . ? O22 C22 1.104(13) . ? C100 Cl3 1.691(10) . ? C100 Cl2 1.716(10) . ? C100 Cl1 1.723(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 Re1 C3 90.7(4) . . ? C2 Re1 C1 89.7(4) . . ? C3 Re1 C1 85.6(4) . . ? C2 Re1 C4 89.4(4) . . ? C3 Re1 C4 92.4(4) . . ? C1 Re1 C4 177.8(4) . . ? C2 Re1 S1 165.8(3) . . ? C3 Re1 S1 102.7(3) . . ? C1 Re1 S1 96.0(3) . . ? C4 Re1 S1 85.3(3) . . ? C2 Re1 Re2 115.9(3) . . ? C3 Re1 Re2 152.7(3) . . ? C1 Re1 Re2 88.2(3) . . ? C4 Re1 Re2 94.0(3) . . ? S1 Re1 Re2 51.61(5) . . ? C8 Re2 C7 90.2(4) . . ? C8 Re2 C5 89.4(4) . . ? C7 Re2 C5 84.8(4) . . ? C8 Re2 C6 91.9(4) . . ? C7 Re2 C6 94.9(4) . . ? C5 Re2 C6 178.6(4) . . ? C8 Re2 S1 164.3(3) . . ? C7 Re2 S1 105.3(3) . . ? C5 Re2 S1 90.1(3) . . ? C6 Re2 S1 88.7(3) . . ? C8 Re2 Re1 112.7(3) . . ? C7 Re2 Re1 155.9(3) . . ? C5 Re2 Re1 87.9(3) . . ? C6 Re2 Re1 91.9(3) . . ? S1 Re2 Re1 51.67(5) . . ? C17 Re3 C15 88.9(5) . . ? C17 Re3 C18 87.5(5) . . ? C15 Re3 C18 89.5(5) . . ? C17 Re3 C16 93.0(5) . . ? C15 Re3 C16 90.1(4) . . ? C18 Re3 C16 179.3(5) . . ? C17 Re3 S2 105.0(4) . . ? C15 Re3 S2 165.6(3) . . ? C18 Re3 S2 94.4(3) . . ? C16 Re3 S2 85.8(3) . . ? C17 Re3 Re4 155.5(3) . . ? C15 Re3 Re4 115.0(3) . . ? C18 Re3 Re4 87.8(3) . . ? C16 Re3 Re4 91.9(3) . . ? S2 Re3 Re4 51.49(5) . . ? C19 Re4 C22 89.6(4) . . ? C19 Re4 C21 86.0(5) . . ? C22 Re4 C21 89.4(5) . . ? C19 Re4 C20 92.6(4) . . ? C22 Re4 C20 90.1(5) . . ? C21 Re4 C20 178.5(4) . . ? C19 Re4 S2 107.4(3) . . ? C22 Re4 S2 163.0(3) . . ? C21 Re4 S2 91.6(4) . . ? C20 Re4 S2 89.3(3) . . ? C19 Re4 Re3 158.2(3) . . ? C22 Re4 Re3 111.5(3) . . ? C21 Re4 Re3 88.7(3) . . ? C20 Re4 Re3 92.9(3) . . ? S2 Re4 Re3 51.59(6) . . ? C11 Fe1 C10 86.6(5) . . ? C11 Fe1 C9 98.0(5) . . ? C10 Fe1 C9 102.0(5) . . ? C11 Fe1 S1 88.0(3) . . ? C10 Fe1 S1 152.5(3) . . ? C9 Fe1 S1 105.5(4) . . ? C11 Fe1 S2 163.7(4) . . ? C10 Fe1 S2 92.3(3) . . ? C9 Fe1 S2 98.1(3) . . ? S1 Fe1 S2 85.48(9) . . ? C11 Fe1 Fe2 108.6(4) . . ? C10 Fe1 Fe2 99.3(3) . . ? C9 Fe1 Fe2 146.6(3) . . ? S1 Fe1 Fe2 57.25(7) . . ? S2 Fe1 Fe2 55.44(7) . . ? C13 Fe2 C14 87.0(5) . . ? C13 Fe2 C12 101.6(5) . . ? C14 Fe2 C12 99.7(5) . . ? C13 Fe2 S2 157.0(4) . . ? C14 Fe2 S2 87.8(3) . . ? C12 Fe2 S2 101.3(3) . . ? C13 Fe2 S1 91.7(3) . . ? C14 Fe2 S1 158.7(4) . . ? C12 Fe2 S1 101.5(3) . . ? S2 Fe2 S1 85.09(9) . . ? C13 Fe2 Fe1 102.9(4) . . ? C14 Fe2 Fe1 104.5(4) . . ? C12 Fe2 Fe1 146.2(3) . . ? S2 Fe2 Fe1 56.97(7) . . ? S1 Fe2 Fe1 55.08(7) . . ? Fe1 S1 Fe2 67.68(8) . . ? Fe1 S1 Re2 127.52(10) . . ? Fe2 S1 Re2 143.71(10) . . ? Fe1 S1 Re1 130.25(10) . . ? Fe2 S1 Re1 121.20(10) . . ? Re2 S1 Re1 76.73(7) . . ? Fe2 S2 Fe1 67.59(8) . . ? Fe2 S2 Re4 130.41(11) . . ? Fe1 S2 Re4 142.14(11) . . ? Fe2 S2 Re3 128.34(10) . . ? Fe1 S2 Re3 120.93(10) . . ? Re4 S2 Re3 76.92(7) . . ? O1 C1 Re1 175.4(10) . . ? O2 C2 Re1 178.9(9) . . ? O3 C3 Re1 175.6(10) . . ? O4 C4 Re1 177.8(9) . . ? O5 C5 Re2 174.0(10) . . ? O6 C6 Re2 178.5(11) . . ? O7 C7 Re2 174.8(9) . . ? O8 C8 Re2 179.0(8) . . ? O9 C9 Fe1 177.4(10) . . ? O10 C10 Fe1 175.1(9) . . ? O11 C11 Fe1 179.5(10) . . ? O12 C12 Fe2 177.7(11) . . ? O13 C13 Fe2 173.8(9) . . ? O14 C14 Fe2 178.2(12) . . ? O15 C15 Re3 177.6(11) . . ? O16 C16 Re3 177.6(11) . . ? O17 C17 Re3 176.1(11) . . ? O18 C18 Re3 176.8(14) . . ? O19 C19 Re4 175.5(9) . . ? O20 C20 Re4 177.2(10) . . ? O21 C21 Re4 172.6(11) . . ? O22 C22 Re4 178.3(11) . . ? Cl3 C100 Cl2 113.2(7) . . ? Cl3 C100 Cl1 111.3(6) . . ? Cl2 C100 Cl1 113.1(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.936 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.315 #=END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H2 O19 Os3 Re2 S' _chemical_formula_sum 'C19 H2 O19 Os3 Re2 S' _chemical_formula_weight 1509.27 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' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.805(2) _cell_length_b 28.614(6) _cell_length_c 11.870(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.120(10) _cell_angle_gamma 90.00 _cell_volume 2900.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7.696 _cell_measurement_theta_max 15.941 _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 21.566 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.175 _exptl_absorpt_correction_T_max 0.761 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 2 _diffrn_reflns_number 6354 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6144 _reflns_number_gt 3645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+36.2877P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6144 _refine_ls_number_parameters 398 _refine_ls_number_restraints 520 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1667 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.790 _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 Os1 Os 1.29751(9) 0.15502(3) 1.70480(7) 0.0369(2) Uani 1 1 d U . . Os2 Os 1.30876(9) 0.05902(3) 1.78417(7) 0.0378(2) Uani 1 1 d U . . Os3 Os 1.60539(8) 0.10703(3) 1.81381(6) 0.0371(2) Uani 1 1 d U . . Re1 Re 1.40913(9) 0.18487(3) 1.37406(7) 0.0404(2) Uani 1 1 d U . . Re2 Re 1.13024(9) 0.11615(3) 1.33239(7) 0.0394(2) Uani 1 1 d U . . S1 S 1.3349(5) 0.13001(18) 1.5135(4) 0.0363(9) Uani 1 1 d U . . O1 O 1.335(2) 0.2566(6) 1.6401(15) 0.058(4) Uani 1 1 d U . . C1 C 1.317(2) 0.2189(8) 1.6598(18) 0.042(4) Uani 1 1 d U . . O2 O 0.9471(17) 0.1428(6) 1.6056(13) 0.049(4) Uani 1 1 d U . . C2 C 1.078(2) 0.1496(8) 1.6462(16) 0.039(3) Uani 1 1 d U . . O3 O 1.258(2) 0.1931(7) 1.9359(13) 0.063(5) Uani 1 1 d U . . C3 C 1.269(2) 0.1777(8) 1.8498(18) 0.041(4) Uani 1 1 d U . . C4 C 1.091(2) 0.0469(8) 1.7451(19) 0.044(4) Uani 1 1 d U . . O4 O 0.9592(19) 0.0374(8) 1.7255(17) 0.073(5) Uani 1 1 d U . . O5 O 1.419(2) -0.0369(7) 1.8839(14) 0.063(5) Uani 1 1 d U . . C5 C 1.383(3) -0.0012(8) 1.8514(17) 0.041(4) Uani 1 1 d U . . O6 O 1.272(2) 0.0915(7) 2.0231(16) 0.067(5) Uani 1 1 d U . . C6 C 1.287(2) 0.0836(8) 1.9346(19) 0.043(4) Uani 1 1 d U . . O7 O 1.3350(19) 0.0190(6) 1.5488(14) 0.056(4) Uani 1 1 d U . . C7 C 1.328(2) 0.0376(8) 1.6312(18) 0.039(3) Uani 1 1 d U . . O8 O 1.7676(18) 0.0194(6) 1.9318(12) 0.050(4) Uani 1 1 d U . . C8 C 1.706(2) 0.0506(9) 1.886(2) 0.048(4) Uani 1 1 d U . . O9 O 1.6536(18) 0.0684(6) 1.5795(14) 0.052(4) Uani 1 1 d U . . C9 C 1.626(2) 0.0855(8) 1.6601(18) 0.039(4) Uani 1 1 d U . . O10 O 1.5801(18) 0.1453(6) 2.0513(13) 0.051(4) Uani 1 1 d U . . C10 C 1.585(2) 0.1330(8) 1.9661(17) 0.042(4) Uani 1 1 d U . . O11 O 1.9106(18) 0.1628(7) 1.8468(15) 0.056(4) Uani 1 1 d U . . C11 C 1.794(2) 0.1399(10) 1.8296(18) 0.048(4) Uani 1 1 d U . . O12 O 1.170(2) 0.2630(6) 1.3846(16) 0.062(4) Uani 1 1 d U . . C12 C 1.258(2) 0.2327(8) 1.3864(18) 0.040(3) Uani 1 1 d U . . O13 O 1.4951(19) 0.2430(7) 1.1760(16) 0.064(5) Uani 1 1 d U . . C13 C 1.458(2) 0.2218(9) 1.2464(18) 0.045(4) Uani 1 1 d U . . O14 O 1.6678(18) 0.2257(7) 1.5735(15) 0.064(5) Uani 1 1 d U . . C14 C 1.574(3) 0.2121(9) 1.497(2) 0.050(4) Uani 1 1 d U . . O15 O 1.640(2) 0.1086(8) 1.3262(17) 0.069(5) Uani 1 1 d U . . C15 C 1.556(2) 0.1335(10) 1.3422(19) 0.048(4) Uani 1 1 d U . . O16 O 1.349(2) 0.0343(6) 1.2904(14) 0.057(4) Uani 1 1 d U . . C16 C 1.271(2) 0.0657(8) 1.3075(17) 0.038(3) Uani 1 1 d U . . O17 O 0.930(2) 0.1040(9) 1.0831(15) 0.076(6) Uani 1 1 d U . . C17 C 1.006(3) 0.1099(10) 1.1776(19) 0.057(5) Uani 1 1 d U . . O18 O 0.900(2) 0.1948(6) 1.3725(16) 0.061(4) Uani 1 1 d U . . C18 C 0.988(2) 0.1689(9) 1.3627(18) 0.048(4) Uani 1 1 d U . . O19 O 0.932(2) 0.0454(7) 1.4328(17) 0.064(5) Uani 1 1 d U . . C19 C 1.006(2) 0.0712(9) 1.3953(19) 0.048(4) Uani 1 1 d U . . 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 Os1 0.0335(4) 0.0432(4) 0.0328(4) -0.0014(3) 0.0059(3) 0.0018(3) Os2 0.0335(4) 0.0461(5) 0.0335(4) 0.0006(3) 0.0077(3) -0.0011(3) Os3 0.0307(4) 0.0482(5) 0.0309(4) -0.0020(3) 0.0047(3) -0.0004(3) Re1 0.0336(4) 0.0493(5) 0.0375(4) 0.0044(4) 0.0069(3) -0.0020(3) Re2 0.0323(4) 0.0509(5) 0.0326(4) 0.0008(3) 0.0035(3) -0.0017(3) S1 0.033(2) 0.042(3) 0.033(2) 0.0003(18) 0.0049(16) 0.0005(19) O1 0.078(11) 0.046(7) 0.050(9) 0.003(7) 0.017(8) 0.010(8) C1 0.038(9) 0.045(6) 0.038(9) -0.003(6) -0.001(7) 0.002(6) O2 0.041(6) 0.057(10) 0.045(8) 0.003(7) 0.004(6) 0.014(7) C2 0.036(5) 0.054(10) 0.026(8) 0.006(7) 0.007(5) 0.000(6) O3 0.072(11) 0.081(13) 0.035(7) -0.014(8) 0.010(7) 0.009(10) C3 0.035(8) 0.050(8) 0.038(7) -0.006(7) 0.008(6) 0.012(8) C4 0.036(6) 0.050(10) 0.052(11) -0.013(9) 0.019(6) -0.003(6) O4 0.037(6) 0.096(15) 0.083(13) -0.007(11) 0.011(8) -0.002(9) O5 0.089(12) 0.061(9) 0.045(9) 0.016(8) 0.027(8) 0.025(9) C5 0.054(10) 0.045(6) 0.029(8) -0.002(6) 0.015(8) 0.001(6) O6 0.085(12) 0.068(12) 0.059(9) -0.010(9) 0.035(9) 0.008(10) C6 0.035(8) 0.051(10) 0.044(7) -0.001(6) 0.010(7) 0.002(8) O7 0.062(10) 0.061(11) 0.044(8) -0.005(7) 0.011(7) -0.014(8) C7 0.031(8) 0.043(8) 0.039(6) 0.007(6) 0.005(6) 0.004(7) O8 0.058(9) 0.057(9) 0.033(8) 0.005(6) 0.005(6) 0.000(7) C8 0.032(7) 0.065(9) 0.048(10) 0.010(8) 0.012(8) 0.004(7) O9 0.047(8) 0.063(11) 0.047(8) -0.012(7) 0.011(6) 0.012(7) C9 0.035(8) 0.044(11) 0.042(7) -0.005(6) 0.015(7) -0.005(6) O10 0.056(9) 0.060(10) 0.039(7) -0.014(7) 0.015(7) -0.002(8) C10 0.038(9) 0.058(11) 0.030(6) -0.004(7) 0.007(5) -0.015(7) O11 0.046(8) 0.060(11) 0.061(10) 0.003(8) 0.008(7) -0.007(6) C11 0.037(6) 0.074(13) 0.032(9) 0.001(8) 0.009(6) -0.009(7) O12 0.067(11) 0.046(10) 0.076(12) 0.005(9) 0.021(9) 0.012(7) C12 0.038(8) 0.046(6) 0.041(10) 0.005(7) 0.019(7) -0.006(5) O13 0.045(9) 0.078(13) 0.069(11) 0.030(9) 0.016(8) -0.002(8) C13 0.044(10) 0.055(11) 0.041(8) -0.003(7) 0.020(7) -0.003(8) O14 0.043(8) 0.085(14) 0.060(10) -0.008(9) 0.002(6) -0.020(8) C14 0.042(9) 0.050(11) 0.052(9) 0.002(8) -0.001(7) -0.006(7) O15 0.050(9) 0.087(14) 0.074(12) 0.015(10) 0.024(8) 0.023(9) C15 0.033(7) 0.071(11) 0.041(10) 0.005(8) 0.008(7) 0.007(7) O16 0.074(11) 0.058(10) 0.042(8) -0.004(8) 0.018(7) 0.005(7) C16 0.038(8) 0.042(7) 0.031(8) 0.003(6) 0.000(6) -0.006(5) O17 0.056(10) 0.121(18) 0.043(8) -0.010(10) -0.003(7) -0.012(11) C17 0.054(11) 0.064(14) 0.040(7) 0.013(7) -0.014(7) 0.008(8) O18 0.075(11) 0.048(10) 0.065(11) 0.015(8) 0.026(9) 0.021(7) C18 0.040(7) 0.064(10) 0.040(9) 0.032(8) 0.012(7) 0.021(7) O19 0.072(11) 0.051(10) 0.077(12) 0.012(9) 0.032(9) -0.003(8) C19 0.032(8) 0.062(10) 0.045(10) 0.012(9) -0.001(6) -0.002(6) _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 Os1 C2 1.892(19) . ? Os1 C3 1.91(2) . ? Os1 C1 1.92(2) . ? Os1 S1 2.478(5) . ? Os1 Os2 2.8979(13) . ? Os1 Os3 3.0326(12) . ? Os2 C4 1.89(2) . ? Os2 C5 1.94(2) . ? Os2 C7 1.96(2) . ? Os2 C6 1.97(2) . ? Os2 Os3 2.8956(12) . ? Os3 C11 1.88(2) . ? Os3 C8 1.94(2) . ? Os3 C9 1.98(2) . ? Os3 C10 2.00(2) . ? Re1 C12 1.94(2) . ? Re1 C14 1.95(2) . ? Re1 C13 1.98(2) . ? Re1 C15 2.05(2) . ? Re1 S1 2.482(5) . ? Re1 Re2 3.0900(13) . ? Re2 C17 1.90(2) . ? Re2 C19 1.95(2) . ? Re2 C16 1.97(2) . ? Re2 C18 2.05(2) . ? Re2 S1 2.477(5) . ? O1 C1 1.12(3) . ? O2 C2 1.15(2) . ? O3 C3 1.14(2) . ? C4 O4 1.16(3) . ? O5 C5 1.11(3) . ? O6 C6 1.12(3) . ? O7 C7 1.13(3) . ? O8 C8 1.12(3) . ? O9 C9 1.15(2) . ? O10 C10 1.08(2) . ? O11 C11 1.19(3) . ? O12 C12 1.16(3) . ? O13 C13 1.14(3) . ? O14 C14 1.13(3) . ? O15 C15 1.08(3) . ? O16 C16 1.18(3) . ? O17 C17 1.17(3) . ? O18 C18 1.10(3) . ? O19 C19 1.15(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 C2 Os1 C3 90.7(8) . . ? C2 Os1 C1 97.3(9) . . ? C3 Os1 C1 88.1(10) . . ? C2 Os1 S1 89.5(6) . . ? C3 Os1 S1 176.9(7) . . ? C1 Os1 S1 88.8(6) . . ? C2 Os1 Os2 89.6(7) . . ? C3 Os1 Os2 91.8(7) . . ? C1 Os1 Os2 173.1(6) . . ? S1 Os1 Os2 91.28(13) . . ? C2 Os1 Os3 147.7(7) . . ? C3 Os1 Os3 94.0(6) . . ? C1 Os1 Os3 114.7(6) . . ? S1 Os1 Os3 87.45(11) . . ? Os2 Os1 Os3 58.40(3) . . ? C4 Os2 C5 99.1(10) . . ? C4 Os2 C7 91.6(8) . . ? C5 Os2 C7 90.3(8) . . ? C4 Os2 C6 88.4(9) . . ? C5 Os2 C6 92.4(9) . . ? C7 Os2 C6 177.3(9) . . ? C4 Os2 Os3 161.3(7) . . ? C5 Os2 Os3 99.6(7) . . ? C7 Os2 Os3 88.9(6) . . ? C6 Os2 Os3 90.2(6) . . ? C4 Os2 Os1 98.1(7) . . ? C5 Os2 Os1 162.7(7) . . ? C7 Os2 Os1 90.0(6) . . ? C6 Os2 Os1 87.3(7) . . ? Os3 Os2 Os1 63.13(3) . . ? C11 Os3 C8 94.3(10) . . ? C11 Os3 C9 88.2(9) . . ? C8 Os3 C9 90.6(10) . . ? C11 Os3 C10 89.8(9) . . ? C8 Os3 C10 92.6(10) . . ? C9 Os3 C10 176.3(9) . . ? C11 Os3 Os2 178.0(8) . . ? C8 Os3 Os2 87.7(7) . . ? C9 Os3 Os2 91.4(6) . . ? C10 Os3 Os2 90.5(5) . . ? C11 Os3 Os1 119.5(8) . . ? C8 Os3 Os1 146.2(7) . . ? C9 Os3 Os1 91.3(6) . . ? C10 Os3 Os1 87.1(6) . . ? Os2 Os3 Os1 58.47(3) . . ? C12 Re1 C14 93.6(10) . . ? C12 Re1 C13 88.0(9) . . ? C14 Re1 C13 95.6(10) . . ? C12 Re1 C15 173.7(9) . . ? C14 Re1 C15 92.1(10) . . ? C13 Re1 C15 88.6(9) . . ? C12 Re1 S1 95.6(6) . . ? C14 Re1 S1 91.3(7) . . ? C13 Re1 S1 172.0(7) . . ? C15 Re1 S1 87.2(7) . . ? C12 Re1 Re2 85.8(6) . . ? C14 Re1 Re2 142.2(7) . . ? C13 Re1 Re2 122.1(7) . . ? C15 Re1 Re2 91.5(7) . . ? S1 Re1 Re2 51.39(11) . . ? C17 Re2 C19 93.7(10) . . ? C17 Re2 C16 91.2(10) . . ? C19 Re2 C16 90.5(9) . . ? C17 Re2 C18 90.4(10) . . ? C19 Re2 C18 89.7(10) . . ? C16 Re2 C18 178.3(9) . . ? C17 Re2 S1 167.9(8) . . ? C19 Re2 S1 97.5(6) . . ? C16 Re2 S1 84.0(6) . . ? C18 Re2 S1 94.3(7) . . ? C17 Re2 Re1 117.4(8) . . ? C19 Re2 Re1 148.9(6) . . ? C16 Re2 Re1 89.1(6) . . ? C18 Re2 Re1 89.9(7) . . ? S1 Re2 Re1 51.53(12) . . ? Re2 S1 Os1 127.6(2) . . ? Re2 S1 Re1 77.08(14) . . ? Os1 S1 Re1 122.9(2) . . ? O1 C1 Os1 175.6(19) . . ? O2 C2 Os1 174(2) . . ? O3 C3 Os1 176(2) . . ? O4 C4 Os2 176(2) . . ? O5 C5 Os2 176(2) . . ? O6 C6 Os2 171(2) . . ? O7 C7 Os2 170.0(19) . . ? O8 C8 Os3 176(2) . . ? O9 C9 Os3 170.2(19) . . ? O10 C10 Os3 176(2) . . ? O11 C11 Os3 175(2) . . ? O12 C12 Re1 173.8(18) . . ? O13 C13 Re1 176(2) . . ? O14 C14 Re1 175(2) . . ? O15 C15 Re1 175(2) . . ? O16 C16 Re2 176.6(18) . . ? O17 C17 Re2 177(3) . . ? O18 C18 Re2 173(2) . . ? O19 C19 Re2 179(2) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 1.477 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.404 # End of cif