Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Egold, Hans' ; Fachbereich Chemie und Chemietechnik Universitat Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; 'Schwarze, Detlef' ; Fachbereich Chemie und Chemietechnik Universitat Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; 'Florke, Ulrich' ; Fachbereich Chemie und Chemietechnik Universitat Paderborn Warburgerstr. 100 D-33098 Paderborn, FRG ; _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Dr Hans Egold' _publ_contact_author_address ; Anorganische und Analytische Chemistry Universität Paderborn Warburgerstr. 100, D-33098 Paderbor Paderborn 33098 GERMANY ; _publ_contact_author_email HE@CHEMIE.UNI-PADERBORN.DE _publ_contact_author_fax '+49 5251 60 3423' _publ_contact_author_phone '+49 5251 60 2496' _publ_section_title ; Substitution reactivity of hydrido sulfido bridged Dirhenium Cluster Complexes Re~2~(\m-H)(\m-SR)(CO~8~) (R = organic residue) ; _publ_contact_letter ; Please find below 6 data sets in CIF format as supplementary crystallographic data in connection with submission of our manuscript entitled "see below" for publication in Dalton Transactions. The data have already been deposited with the CCDC, the allocated CCDC deposition numbers are CCDC-169418 for 3a 139434 for 3c 169419 for 3g 169420 for 4a 169421 for 5 169422 for 7. Thank you very much! ; data_3a _database_code_CSD 169418 _audit_creation_method SHELXL _chemical_name_systematic ; \m-hydrido-\m-naphthylthiolato-ax-acetonitrile- heptacarbonyl-dirhenium ; _chemical_formula_moiety 'C19 H11 N O7 Re2 S' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H11 N O7 Re2 S' _chemical_formula_weight 769.75 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' '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 'P 2(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 9.845(4) _cell_length_b 13.269(4) _cell_length_c 16.632(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.11(2) _cell_angle_gamma 90.00 _cell_volume 2124.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.5 _cell_measurement_theta_max 17.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.407 _exptl_crystal_density_method ? _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 11.524 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.141 _exptl_absorpt_correction_T_max 0.575 _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 4796 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.56 _reflns_number_total 4657 _reflns_number_observed 3603 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker XSCANS (Bruker, 1996)' _computing_cell_refinement 'Bruker XSCANS (Bruker, 1996)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w==1/[\s^2^(Fo^2^)+(0.0722P)^2^] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00054(13) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4657 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_obs 0.0434 _refine_ls_wR_factor_all 0.1156 _refine_ls_wR_factor_obs 0.1043 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_obs 1.062 _refine_ls_restrained_S_all 1.028 _refine_ls_restrained_S_obs 1.062 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 1.04382(4) -0.29556(3) -0.06991(2) 0.02637(13) Uani 1 d . . Re2 Re 1.33353(4) -0.24146(3) 0.03546(2) 0.02535(13) Uani 1 d . . S1 S 1.2538(2) -0.4030(2) -0.03331(13) 0.0250(5) Uani 1 d . . C1 C 1.0926(11) -0.2279(8) -0.1685(6) 0.029(2) Uani 1 d . . O1 O 1.1073(9) -0.1891(6) -0.2256(4) 0.045(2) Uani 1 d . . C2 C 0.8832(12) -0.2079(9) -0.0871(6) 0.037(2) Uani 1 d . . O2 O 0.7860(9) -0.1594(8) -0.0974(5) 0.063(3) Uani 1 d . . C3 C 0.9405(11) -0.3982(9) -0.1404(7) 0.040(3) Uani 1 d . . O3 O 0.8856(8) -0.4562(7) -0.1847(5) 0.058(2) Uani 1 d . . C4 C 0.9856(12) -0.3484(9) 0.0306(6) 0.038(2) Uani 1 d . . O4 O 0.9478(9) -0.3709(8) 0.0870(5) 0.057(2) Uani 1 d . . C5 C 1.2872(12) -0.2840(9) 0.1360(6) 0.035(2) Uani 1 d . . O5 O 1.2631(10) -0.3079(8) 0.1975(5) 0.057(2) Uani 1 d . . C6 C 1.5269(11) -0.2775(9) 0.0772(6) 0.039(3) Uani 1 d . . O6 O 1.6375(8) -0.3031(6) 0.0993(5) 0.043(2) Uani 1 d . . C7 C 1.3670(11) -0.1097(8) 0.0823(6) 0.034(2) Uani 1 d . . O7 O 1.3857(9) -0.0301(7) 0.1098(5) 0.056(2) Uani 1 d . . N1 N 1.3879(10) -0.1955(6) -0.0777(5) 0.032(2) Uani 1 d . . C8 C 1.4194(11) -0.1795(8) -0.1372(6) 0.033(2) Uani 1 d . . C9 C 1.4540(13) -0.1643(9) -0.2170(6) 0.042(3) Uani 1 d . . H9A H 1.5262(63) -0.1137(47) -0.2124(12) 0.063 Uiso 1 calc R . H9B H 1.3720(25) -0.1420(61) -0.2560(14) 0.063 Uiso 1 calc R . H9C H 1.4868(83) -0.2272(18) -0.2358(24) 0.063 Uiso 1 calc R . C11 C 1.3368(9) -0.4206(7) -0.1181(5) 0.024(2) Uani 1 d . . C12 C 1.2658(10) -0.4250(7) -0.1982(5) 0.025(2) Uani 1 d . . H12 H 1.1686(10) -0.4184(7) -0.2103(5) 0.030 Uiso 1 calc R . C13 C 1.3358(10) -0.4393(7) -0.2626(5) 0.024(2) Uani 1 d . . C14 C 1.2654(12) -0.4417(8) -0.3465(6) 0.038(3) Uani 1 d . . H14 H 1.1680(12) -0.4368(8) -0.3602(6) 0.046 Uiso 1 calc R . C15 C 1.3390(13) -0.4513(9) -0.4078(6) 0.043(3) Uani 1 d . . H15 H 1.2916(13) -0.4519(9) -0.4631(6) 0.052 Uiso 1 calc R . C16 C 1.4825(13) -0.4601(10) -0.3888(6) 0.047(3) Uani 1 d . . H16 H 1.5312(13) -0.4650(10) -0.4316(6) 0.056 Uiso 1 calc R . C17 C 1.5534(12) -0.4616(10) -0.3102(6) 0.043(3) Uani 1 d . . H17 H 1.6503(12) -0.4702(10) -0.2988(6) 0.051 Uiso 1 calc R . C18 C 1.4838(11) -0.4504(8) -0.2447(6) 0.030(2) Uani 1 d . . C19 C 1.5517(10) -0.4484(8) -0.1608(6) 0.033(2) Uani 1 d . . H19 H 1.6485(10) -0.4575(8) -0.1469(6) 0.040 Uiso 1 calc R . C20 C 1.4825(11) -0.4340(8) -0.1005(6) 0.034(2) Uani 1 d . . H20 H 1.5316(11) -0.4327(8) -0.0455(6) 0.041 Uiso 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 Re1 0.0180(2) 0.0368(2) 0.0239(2) -0.00240(15) 0.00351(13) 0.0037(2) Re2 0.0206(2) 0.0345(2) 0.0204(2) -0.00257(14) 0.00298(14) 0.0013(2) S1 0.0193(11) 0.0312(12) 0.0246(10) 0.0008(9) 0.0052(8) 0.0023(9) C1 0.025(5) 0.034(5) 0.029(5) -0.001(4) 0.007(4) 0.001(4) O1 0.052(5) 0.054(5) 0.031(4) 0.009(3) 0.010(4) 0.007(4) C2 0.034(6) 0.047(6) 0.029(5) -0.010(4) 0.002(4) 0.009(5) O2 0.039(5) 0.090(7) 0.055(5) -0.005(5) -0.001(4) 0.029(5) C3 0.028(6) 0.044(6) 0.044(6) -0.001(5) -0.001(5) -0.005(5) O3 0.034(5) 0.074(6) 0.062(5) -0.022(5) 0.003(4) -0.017(5) C4 0.030(6) 0.047(7) 0.039(6) 0.000(5) 0.010(5) -0.001(5) O4 0.039(5) 0.085(7) 0.053(5) 0.006(5) 0.023(4) -0.002(5) C5 0.031(6) 0.048(6) 0.027(5) 0.000(4) 0.012(4) -0.005(5) O5 0.056(6) 0.085(7) 0.031(4) 0.006(4) 0.008(4) -0.002(5) C6 0.027(6) 0.057(7) 0.033(5) -0.011(5) 0.006(4) 0.018(5) O6 0.027(4) 0.054(5) 0.046(4) -0.004(4) 0.005(3) 0.003(4) C7 0.025(5) 0.038(6) 0.035(5) -0.003(4) -0.001(4) 0.000(4) O7 0.050(5) 0.050(5) 0.064(5) -0.025(4) 0.002(4) 0.003(4) N1 0.036(5) 0.034(5) 0.027(4) 0.001(3) 0.009(4) 0.000(4) C8 0.030(6) 0.033(5) 0.033(5) 0.004(4) 0.002(4) -0.003(4) C9 0.049(7) 0.041(6) 0.037(5) -0.003(5) 0.012(5) -0.002(6) C11 0.016(4) 0.031(5) 0.028(4) 0.001(4) 0.014(3) -0.005(4) C12 0.020(5) 0.027(5) 0.027(4) -0.008(4) 0.000(4) 0.000(4) C13 0.029(5) 0.020(4) 0.025(4) -0.001(3) 0.007(4) -0.005(4) C14 0.035(6) 0.045(6) 0.027(5) -0.001(4) -0.011(4) 0.002(5) C15 0.057(8) 0.052(7) 0.021(5) -0.006(4) 0.010(5) -0.003(6) C16 0.050(7) 0.068(8) 0.024(5) -0.006(5) 0.012(5) -0.006(7) C17 0.032(6) 0.068(8) 0.032(5) -0.015(5) 0.016(4) -0.003(6) C18 0.028(5) 0.036(5) 0.028(4) -0.008(4) 0.013(4) -0.007(4) C19 0.021(5) 0.048(6) 0.027(5) -0.003(4) -0.002(4) 0.008(5) C20 0.027(5) 0.049(6) 0.027(5) -0.004(4) 0.005(4) 0.010(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 1.935(11) . ? Re1 C3 1.941(11) . ? Re1 C4 2.004(11) . ? Re1 C1 2.014(10) . ? Re1 S1 2.480(2) . ? Re1 Re2 3.1023(12) . ? Re2 C5 1.908(10) . ? Re2 C7 1.914(11) . ? Re2 C6 1.944(10) . ? Re2 N1 2.150(8) . ? Re2 S1 2.478(2) . ? S1 C11 1.788(9) . ? C1 O1 1.116(12) . ? C2 O2 1.136(13) . ? C3 O3 1.122(12) . ? C4 O4 1.120(13) . ? C5 O5 1.143(12) . ? C6 O6 1.127(13) . ? C7 O7 1.151(13) . ? N1 C8 1.118(13) . ? C8 C9 1.451(14) . ? C11 C12 1.370(12) . ? C11 C20 1.413(13) . ? C12 C13 1.402(13) . ? C13 C14 1.423(11) . ? C13 C18 1.432(13) . ? C14 C15 1.37(2) . ? C15 C16 1.39(2) . ? C16 C17 1.347(14) . ? C17 C18 1.411(13) . ? C18 C19 1.416(12) . ? C19 C20 1.339(14) . ? 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 91.4(5) . . ? C2 Re1 C4 88.0(5) . . ? C3 Re1 C4 93.0(5) . . ? C2 Re1 C1 86.5(4) . . ? C3 Re1 C1 90.3(4) . . ? C4 Re1 C1 173.7(4) . . ? C2 Re1 S1 174.3(3) . . ? C3 Re1 S1 92.8(3) . . ? C4 Re1 S1 87.9(3) . . ? C1 Re1 S1 97.3(3) . . ? C2 Re1 Re2 124.8(3) . . ? C3 Re1 Re2 143.8(3) . . ? C4 Re1 Re2 90.0(3) . . ? C1 Re1 Re2 90.5(3) . . ? S1 Re1 Re2 51.24(6) . . ? C5 Re2 C7 88.1(5) . . ? C5 Re2 C6 90.6(5) . . ? C7 Re2 C6 90.4(5) . . ? C5 Re2 N1 179.1(4) . . ? C7 Re2 N1 92.5(4) . . ? C6 Re2 N1 88.7(4) . . ? C5 Re2 S1 92.1(3) . . ? C7 Re2 S1 171.3(3) . . ? C6 Re2 S1 98.3(3) . . ? N1 Re2 S1 87.4(2) . . ? C5 Re2 Re1 93.8(3) . . ? C7 Re2 Re1 120.0(3) . . ? C6 Re2 Re1 149.3(3) . . ? N1 Re2 Re1 86.5(2) . . ? S1 Re2 Re1 51.29(5) . . ? C11 S1 Re2 108.9(3) . . ? C11 S1 Re1 112.1(3) . . ? Re2 S1 Re1 77.47(7) . . ? O1 C1 Re1 173.8(9) . . ? O2 C2 Re1 177.6(11) . . ? O3 C3 Re1 175.7(11) . . ? O4 C4 Re1 174.6(11) . . ? O5 C5 Re2 177.8(10) . . ? O6 C6 Re2 176.3(10) . . ? O7 C7 Re2 179.2(9) . . ? C8 N1 Re2 174.3(9) . . ? N1 C8 C9 176.0(12) . . ? C12 C11 C20 119.1(9) . . ? C12 C11 S1 123.3(7) . . ? C20 C11 S1 117.6(7) . . ? C11 C12 C13 121.1(9) . . ? C12 C13 C14 122.4(9) . . ? C12 C13 C18 119.7(8) . . ? C14 C13 C18 117.9(9) . . ? C15 C14 C13 120.3(10) . . ? C14 C15 C16 120.7(10) . . ? C17 C16 C15 121.2(11) . . ? C16 C17 C18 120.8(11) . . ? C17 C18 C19 123.9(10) . . ? C17 C18 C13 119.2(9) . . ? C19 C18 C13 116.9(8) . . ? C20 C19 C18 122.1(9) . . ? C19 C20 C11 121.0(9) . . ? _refine_diff_density_max 1.082 _refine_diff_density_min -0.980 _refine_diff_density_rms 0.262 #==END data_3g _database_code_CSD 169419 _audit_creation_method SHELXL _chemical_name_systematic ; \m-hydrido-\m-naphthylthiolato-ax-triphenylphosphine- heptacarbonyl-dirhenium ; _chemical_formula_moiety 'C35 H23 O7 P Re2 S, C7 H8' _chemical_formula_sum 'C42 H31 O7 P Re2 S' _chemical_formula_weight 1083.09 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' 'P' 'P' 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.030(6) _cell_length_b 12.673(6) _cell_length_c 15.972(6) _cell_angle_alpha 76.24(2) _cell_angle_beta 71.27(2) _cell_angle_gamma 67.31(2) _cell_volume 1934.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 17 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method ? _exptl_crystal_F_000 1038 _exptl_absorpt_coefficient_mu 6.398 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.683 _exptl_absorpt_correction_T_max 0.880 _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 8955 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.56 _reflns_number_total 8652 _reflns_number_observed 7317 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker XSCANS (Bruker, 1996)' _computing_cell_refinement 'Bruker XSCANS (Bruker, 1996)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w==1/[\s^2^(Fo^2^)+(0.0579P)^2^+2.7484P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(2) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8652 _refine_ls_number_parameters 480 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_obs 0.0355 _refine_ls_wR_factor_all 0.0927 _refine_ls_wR_factor_obs 0.0873 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 1.050 _refine_ls_restrained_S_obs 1.079 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.72054(2) -0.47419(2) -0.129529(12) 0.02235(8) Uani 1 d . . Re2 Re 0.87101(2) -0.29431(2) -0.209961(13) 0.02856(8) Uani 1 d . . S1 S 0.75008(13) -0.36195(11) -0.28022(8) 0.0268(3) Uani 1 d . . P1 P 0.91004(14) -0.64658(11) -0.18736(8) 0.0238(3) Uani 1 d . . C1 C 0.5664(6) -0.3510(5) -0.0713(3) 0.0286(11) Uani 1 d . . O1 O 0.4774(5) -0.2835(4) -0.0327(3) 0.0435(11) Uani 1 d . . C2 C 0.5994(6) -0.5403(5) -0.1424(3) 0.0298(11) Uani 1 d . . O2 O 0.5258(4) -0.5775(4) -0.1534(3) 0.0435(10) Uani 1 d . . C3 C 0.7258(5) -0.5577(4) -0.0119(3) 0.0273(11) Uani 1 d . . O3 O 0.7259(5) -0.6050(4) 0.0583(3) 0.0415(10) Uani 1 d . . C4 C 0.6979(6) -0.1735(5) -0.1607(4) 0.0366(13) Uani 1 d . . O4 O 0.6021(5) -0.1002(4) -0.1352(4) 0.0560(13) Uani 1 d . . C5 C 0.9532(6) -0.2641(5) -0.1319(4) 0.0386(14) Uani 1 d . . O5 O 0.9980(5) -0.2440(5) -0.0851(3) 0.0514(12) Uani 1 d . . C6 C 0.9146(7) -0.1773(6) -0.3051(4) 0.046(2) Uani 1 d . . O6 O 0.9407(7) -0.1101(5) -0.3623(4) 0.074(2) Uani 1 d . . C7 C 1.0488(6) -0.4036(6) -0.2683(4) 0.0394(14) Uani 1 d . . O7 O 1.1529(5) -0.4574(5) -0.3054(4) 0.0613(14) Uani 1 d . . C11 C 0.8592(5) -0.7750(4) -0.1416(3) 0.0258(10) Uani 1 d D . C12 C 0.7948(6) -0.8137(5) -0.1833(4) 0.0338(12) Uani 1 d D . H12 H 0.7833(6) -0.7776(5) -0.2402(4) 0.041 Uiso 1 calc R . C13 C 0.7472(7) -0.9042(5) -0.1428(4) 0.0405(14) Uani 1 d D . H13 H 0.7028(7) -0.9286(5) -0.1718(4) 0.049 Uiso 1 calc R . C14 C 0.7649(7) -0.9592(5) -0.0590(4) 0.0410(14) Uani 1 d D . H14 H 0.7330(7) -1.0212(5) -0.0315(4) 0.049 Uiso 1 calc R . C15 C 0.8290(6) -0.9229(5) -0.0166(4) 0.0383(13) Uani 1 d D . H15 H 0.8414(6) -0.9602(5) 0.0400(4) 0.046 Uiso 1 calc R . C16 C 0.8758(6) -0.8305(5) -0.0573(4) 0.0313(11) Uani 1 d D . H16 H 0.9190(6) -0.8054(5) -0.0276(4) 0.038 Uiso 1 calc R . C21 C 1.0696(6) -0.6918(5) -0.1572(3) 0.0288(11) Uani 1 d D . C22 C 1.0988(6) -0.6238(5) -0.1148(4) 0.0362(13) Uani 1 d D . H22 H 1.0339(6) -0.5520(5) -0.1005(4) 0.043 Uiso 1 calc R . C23 C 1.2222(7) -0.6605(6) -0.0935(4) 0.0443(15) Uani 1 d D . H23 H 1.2402(7) -0.6130(6) -0.0653(4) 0.053 Uiso 1 calc R . C24 C 1.3184(7) -0.7650(6) -0.1129(4) 0.046(2) Uani 1 d D . H24 H 1.4025(7) -0.7886(6) -0.0991(4) 0.055 Uiso 1 calc R . C25 C 1.2899(6) -0.8363(6) -0.1534(4) 0.047(2) Uani 1 d D . H25 H 1.3547(6) -0.9087(6) -0.1661(4) 0.057 Uiso 1 calc R . C26 C 1.1679(6) -0.8009(5) -0.1746(4) 0.0365(13) Uani 1 d D . H26 H 1.1494(6) -0.8499(5) -0.2010(4) 0.044 Uiso 1 calc R . C31 C 0.9559(6) -0.6439(4) -0.3080(3) 0.0288(11) Uani 1 d D . C32 C 1.0887(6) -0.6639(5) -0.3613(4) 0.0347(12) Uani 1 d D . H32 H 1.1595(6) -0.6772(5) -0.3352(4) 0.042 Uiso 1 calc R . C33 C 1.1170(7) -0.6643(5) -0.4520(4) 0.044(2) Uani 1 d D . H33 H 1.2069(7) -0.6780(5) -0.4872(4) 0.052 Uiso 1 calc R . C34 C 1.0144(8) -0.6446(6) -0.4914(4) 0.050(2) Uani 1 d D . H34 H 1.0342(8) -0.6462(6) -0.5530(4) 0.060 Uiso 1 calc R . C35 C 0.8834(8) -0.6228(6) -0.4400(4) 0.044(2) Uani 1 d D . H35 H 0.8132(8) -0.6096(6) -0.4666(4) 0.053 Uiso 1 calc R . C36 C 0.8534(6) -0.6199(5) -0.3497(4) 0.0351(12) Uani 1 d D . H36 H 0.7625(6) -0.6015(5) -0.3158(4) 0.042 Uiso 1 calc R . C40 C 0.6035(6) -0.2414(4) -0.2974(3) 0.0274(11) Uani 1 d D . C41 C 0.4745(6) -0.2382(5) -0.2535(3) 0.0300(11) Uani 1 d D . H41 H 0.4597(6) -0.2984(5) -0.2086(3) 0.036 Uiso 1 calc R . C42 C 0.3611(6) -0.1438(5) -0.2753(3) 0.0298(11) Uani 1 d D . C43 C 0.2273(6) -0.1386(6) -0.2308(4) 0.0427(14) Uani 1 d D . H43 H 0.2110(6) -0.1964(6) -0.1840(4) 0.051 Uiso 1 calc R . C44 C 0.1197(7) -0.0494(6) -0.2553(5) 0.0439(15) Uani 1 d D . H44 H 0.0303(7) -0.0461(6) -0.2245(5) 0.053 Uiso 1 calc R . C45 C 0.1424(7) 0.0360(5) -0.3252(4) 0.0423(15) Uani 1 d D . H45 H 0.0684(7) 0.0952(5) -0.3429(4) 0.051 Uiso 1 calc R . C46 C 0.2710(6) 0.0340(5) -0.3679(4) 0.0385(14) Uani 1 d D . H46 H 0.2851(6) 0.0927(5) -0.4145(4) 0.046 Uiso 1 calc R . C47 C 0.3837(6) -0.0544(5) -0.3436(4) 0.0320(12) Uani 1 d D . C48 C 0.5186(6) -0.0590(5) -0.3861(4) 0.0375(13) Uani 1 d D . H48 H 0.5349(6) 0.0017(5) -0.4298(4) 0.045 Uiso 1 calc R . C49 C 0.6267(6) -0.1504(5) -0.3652(4) 0.0346(12) Uani 1 d D . H49 H 0.7160(6) -0.1529(5) -0.3955(4) 0.042 Uiso 1 calc R . C50 C 0.4984(17) -0.5977(18) -0.5859(17) 0.219(13) Uani 1 d D . H50A H 0.4458(187) -0.5244(58) -0.5631(54) 0.329 Uiso 1 calc R . H50B H 0.4396(175) -0.6252(93) -0.6025(105) 0.329 Uiso 1 calc R . H50C H 0.5705(19) -0.5876(142) -0.6378(60) 0.329 Uiso 1 calc R . C51 C 0.5560(16) -0.6794(15) -0.5190(13) 0.127(6) Uani 1 d D . C52 C 0.4792(27) -0.6715(28) -0.4313(21) 0.225(15) Uani 1 d D . H52 H 0.3895(27) -0.6200(28) -0.4177(21) 0.269 Uiso 1 calc R . C53 C 0.5437(42) -0.7475(35) -0.3596(16) 0.255(22) Uani 1 d D . H53 H 0.5024(42) -0.7371(35) -0.2993(16) 0.306 Uiso 1 calc R . C54 C 0.6664(31) -0.8336(21) -0.3849(15) 0.216(15) Uani 1 d D . H54 H 0.7011(31) -0.8885(21) -0.3398(15) 0.259 Uiso 1 calc R . C55 C 0.7351(22) -0.8435(15) -0.4647(10) 0.146(7) Uani 1 d D . H55 H 0.8217(22) -0.8997(15) -0.4790(10) 0.175 Uiso 1 calc R . C56 C 0.6740(16) -0.7648(14) -0.5316(9) 0.112(4) Uani 1 d D . H56 H 0.7226(16) -0.7745(14) -0.5911(9) 0.135 Uiso 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 Re1 0.02072(12) 0.02329(11) 0.02392(11) -0.00206(7) -0.00696(7) -0.00790(8) Re2 0.02637(13) 0.03033(13) 0.03323(12) 0.00163(8) -0.01204(9) -0.01381(9) S1 0.0269(6) 0.0288(6) 0.0263(6) -0.0002(5) -0.0097(5) -0.0108(5) P1 0.0234(6) 0.0250(6) 0.0243(6) -0.0034(5) -0.0078(5) -0.0080(5) C1 0.029(3) 0.026(3) 0.032(3) -0.001(2) -0.009(2) -0.011(2) O1 0.039(3) 0.033(2) 0.049(2) -0.009(2) -0.003(2) -0.007(2) C2 0.028(3) 0.031(3) 0.031(3) -0.004(2) -0.007(2) -0.011(2) O2 0.034(2) 0.051(3) 0.058(3) -0.015(2) -0.013(2) -0.021(2) C3 0.021(3) 0.027(3) 0.031(3) -0.009(2) -0.004(2) -0.004(2) O3 0.045(3) 0.040(2) 0.030(2) 0.004(2) -0.009(2) -0.009(2) C4 0.036(3) 0.031(3) 0.052(3) -0.006(2) -0.017(3) -0.016(3) O4 0.042(3) 0.041(3) 0.090(4) -0.019(2) -0.018(3) -0.013(2) C5 0.031(3) 0.043(3) 0.035(3) 0.004(2) -0.010(2) -0.010(3) O5 0.051(3) 0.074(3) 0.053(3) -0.005(2) -0.029(2) -0.035(3) C6 0.053(4) 0.050(4) 0.050(4) 0.007(3) -0.025(3) -0.032(3) O6 0.094(5) 0.083(4) 0.064(3) 0.036(3) -0.040(3) -0.061(4) C7 0.035(3) 0.040(3) 0.045(3) 0.000(3) -0.010(3) -0.018(3) O7 0.040(3) 0.061(3) 0.067(3) -0.013(3) 0.001(2) -0.010(2) C11 0.021(2) 0.024(2) 0.031(2) -0.006(2) -0.005(2) -0.006(2) C12 0.039(3) 0.030(3) 0.036(3) -0.001(2) -0.014(2) -0.015(2) C13 0.048(4) 0.036(3) 0.050(3) -0.006(3) -0.015(3) -0.024(3) C14 0.040(3) 0.032(3) 0.049(3) 0.002(2) -0.008(3) -0.018(3) C15 0.042(3) 0.035(3) 0.036(3) 0.003(2) -0.013(2) -0.014(3) C16 0.031(3) 0.030(3) 0.036(3) -0.001(2) -0.014(2) -0.012(2) C21 0.028(3) 0.032(3) 0.027(2) -0.001(2) -0.008(2) -0.011(2) C22 0.036(3) 0.034(3) 0.039(3) -0.003(2) -0.012(2) -0.012(2) C23 0.041(4) 0.051(4) 0.055(4) -0.008(3) -0.024(3) -0.020(3) C24 0.029(3) 0.060(4) 0.050(4) 0.000(3) -0.020(3) -0.014(3) C25 0.028(3) 0.051(4) 0.055(4) -0.003(3) -0.017(3) -0.002(3) C26 0.027(3) 0.040(3) 0.042(3) -0.010(2) -0.010(2) -0.007(2) C31 0.031(3) 0.023(3) 0.031(3) -0.005(2) -0.008(2) -0.008(2) C32 0.032(3) 0.033(3) 0.033(3) -0.002(2) -0.005(2) -0.009(2) C33 0.040(4) 0.041(3) 0.033(3) -0.005(2) 0.004(2) -0.006(3) C34 0.069(5) 0.047(4) 0.027(3) -0.005(2) -0.010(3) -0.015(3) C35 0.060(4) 0.042(4) 0.035(3) -0.004(2) -0.021(3) -0.014(3) C36 0.040(3) 0.036(3) 0.030(3) -0.002(2) -0.013(2) -0.011(2) C40 0.032(3) 0.027(3) 0.027(2) -0.001(2) -0.014(2) -0.010(2) C41 0.031(3) 0.028(3) 0.034(3) 0.003(2) -0.014(2) -0.013(2) C42 0.029(3) 0.030(3) 0.036(3) -0.007(2) -0.013(2) -0.009(2) C43 0.034(3) 0.048(4) 0.048(3) -0.002(3) -0.015(3) -0.013(3) C44 0.029(3) 0.044(4) 0.059(4) -0.011(3) -0.013(3) -0.010(3) C45 0.035(3) 0.035(3) 0.056(4) -0.012(3) -0.022(3) 0.001(3) C46 0.042(4) 0.027(3) 0.042(3) -0.004(2) -0.019(3) -0.002(2) C47 0.033(3) 0.032(3) 0.032(3) -0.004(2) -0.012(2) -0.009(2) C48 0.045(4) 0.033(3) 0.030(3) 0.007(2) -0.013(2) -0.012(3) C49 0.032(3) 0.040(3) 0.030(3) 0.002(2) -0.007(2) -0.016(2) C50 0.115(14) 0.232(23) 0.384(34) -0.194(24) -0.136(19) 0.011(14) C51 0.087(10) 0.135(13) 0.193(17) -0.091(12) -0.022(10) -0.046(9) C52 0.199(24) 0.293(36) 0.225(25) -0.178(26) 0.088(23) -0.160(26) C53 0.367(47) 0.343(44) 0.127(16) -0.126(23) 0.114(24) -0.283(41) C54 0.376(41) 0.230(26) 0.122(15) -0.064(16) 0.029(20) -0.238(30) C55 0.244(21) 0.159(15) 0.092(9) -0.009(10) -0.053(12) -0.125(15) C56 0.121(12) 0.140(12) 0.097(9) -0.053(9) -0.013(8) -0.057(10) _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 1.910(6) . ? Re1 C3 1.931(5) . ? Re1 C1 1.955(5) . ? Re1 S1 2.479(2) . ? Re1 P1 2.488(2) . ? Re1 Re2 3.1238(13) . ? Re2 C6 1.936(6) . ? Re2 C5 1.935(7) . ? Re2 C4 1.991(6) . ? Re2 C7 1.994(7) . ? Re2 S1 2.465(2) . ? S1 C40 1.790(5) . ? P1 C21 1.815(6) . ? P1 C31 1.823(5) . ? P1 C11 1.837(6) . ? C1 O1 1.135(7) . ? C2 O2 1.158(7) . ? C3 O3 1.139(6) . ? C4 O4 1.136(8) . ? C5 O5 1.137(7) . ? C6 O6 1.138(8) . ? C7 O7 1.134(8) . ? C11 C12 1.385(8) . ? C11 C16 1.396(7) . ? C12 C13 1.380(8) . ? C13 C14 1.391(9) . ? C14 C15 1.371(9) . ? C15 C16 1.396(8) . ? C21 C22 1.390(8) . ? C21 C26 1.414(8) . ? C22 C23 1.386(9) . ? C23 C24 1.369(10) . ? C24 C25 1.401(10) . ? C25 C26 1.372(8) . ? C31 C36 1.391(8) . ? C31 C32 1.397(8) . ? C32 C33 1.382(8) . ? C33 C34 1.380(10) . ? C34 C35 1.370(10) . ? C35 C36 1.379(8) . ? C40 C41 1.359(8) . ? C40 C49 1.422(7) . ? C41 C42 1.430(7) . ? C42 C43 1.400(8) . ? C42 C47 1.411(8) . ? C43 C44 1.375(9) . ? C44 C45 1.392(9) . ? C45 C46 1.355(9) . ? C46 C47 1.407(8) . ? C47 C48 1.408(9) . ? C48 C49 1.372(8) . ? C50 C51 1.42(2) . ? C51 C56 1.32(2) . ? C51 C52 1.39(3) . ? C52 C53 1.49(5) . ? C53 C54 1.38(5) . ? C54 C55 1.26(2) . ? C55 C56 1.42(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 C2 Re1 C3 92.8(2) . . ? C2 Re1 C1 90.5(2) . . ? C3 Re1 C1 87.3(2) . . ? C2 Re1 S1 96.7(2) . . ? C3 Re1 S1 170.0(2) . . ? C1 Re1 S1 95.6(2) . . ? C2 Re1 P1 87.3(2) . . ? C3 Re1 P1 86.47(15) . . ? C1 Re1 P1 173.2(2) . . ? S1 Re1 P1 90.97(6) . . ? C2 Re1 Re2 146.7(2) . . ? C3 Re1 Re2 120.2(2) . . ? C1 Re1 Re2 87.4(2) . . ? S1 Re1 Re2 50.60(4) . . ? P1 Re1 Re2 97.93(5) . . ? C6 Re2 C5 93.9(3) . . ? C6 Re2 C4 88.1(3) . . ? C5 Re2 C4 88.8(3) . . ? C6 Re2 C7 86.4(3) . . ? C5 Re2 C7 91.3(3) . . ? C4 Re2 C7 174.5(2) . . ? C6 Re2 S1 98.9(2) . . ? C5 Re2 S1 167.2(2) . . ? C4 Re2 S1 90.3(2) . . ? C7 Re2 S1 90.8(2) . . ? C6 Re2 Re1 149.6(2) . . ? C5 Re2 Re1 116.2(2) . . ? C4 Re2 Re1 88.0(2) . . ? C7 Re2 Re1 96.9(2) . . ? S1 Re2 Re1 51.03(4) . . ? C40 S1 Re2 106.5(2) . . ? C40 S1 Re1 114.8(2) . . ? Re2 S1 Re1 78.37(5) . . ? C21 P1 C31 105.6(2) . . ? C21 P1 C11 101.1(2) . . ? C31 P1 C11 104.8(2) . . ? C21 P1 Re1 119.4(2) . . ? C31 P1 Re1 115.0(2) . . ? C11 P1 Re1 109.2(2) . . ? O1 C1 Re1 175.9(5) . . ? O2 C2 Re1 177.3(5) . . ? O3 C3 Re1 178.3(4) . . ? O4 C4 Re2 176.4(6) . . ? O5 C5 Re2 178.0(5) . . ? O6 C6 Re2 178.6(7) . . ? O7 C7 Re2 173.9(6) . . ? C12 C11 C16 118.3(5) . . ? C12 C11 P1 123.0(4) . . ? C16 C11 P1 118.4(4) . . ? C13 C12 C11 121.1(5) . . ? C12 C13 C14 120.1(6) . . ? C15 C14 C13 119.8(6) . . ? C14 C15 C16 120.0(5) . . ? C15 C16 C11 120.6(5) . . ? C22 C21 C26 117.7(5) . . ? C22 C21 P1 122.4(4) . . ? C26 C21 P1 119.9(4) . . ? C23 C22 C21 120.9(6) . . ? C24 C23 C22 121.0(6) . . ? C23 C24 C25 119.2(6) . . ? C26 C25 C24 120.3(6) . . ? C25 C26 C21 120.9(6) . . ? C36 C31 C32 117.9(5) . . ? C36 C31 P1 118.6(4) . . ? C32 C31 P1 123.5(4) . . ? C33 C32 C31 120.5(6) . . ? C34 C33 C32 120.5(6) . . ? C35 C34 C33 119.5(6) . . ? C34 C35 C36 120.6(6) . . ? C35 C36 C31 120.9(6) . . ? C41 C40 C49 120.2(5) . . ? C41 C40 S1 122.9(4) . . ? C49 C40 S1 116.8(4) . . ? C40 C41 C42 120.3(5) . . ? C43 C42 C47 119.0(5) . . ? C43 C42 C41 121.3(5) . . ? C47 C42 C41 119.7(5) . . ? C44 C43 C42 120.4(6) . . ? C43 C44 C45 120.5(6) . . ? C46 C45 C44 120.1(6) . . ? C45 C46 C47 121.2(6) . . ? C46 C47 C48 122.7(5) . . ? C46 C47 C42 118.8(5) . . ? C48 C47 C42 118.4(5) . . ? C49 C48 C47 121.4(5) . . ? C48 C49 C40 119.9(5) . . ? C56 C51 C50 126.8(18) . . ? C56 C51 C52 116.3(23) . . ? C50 C51 C52 116.9(22) . . ? C51 C52 C53 117.8(27) . . ? C54 C53 C52 117.5(20) . . ? C55 C54 C53 124.3(31) . . ? C54 C55 C56 116.2(23) . . ? C51 C56 C55 127.0(16) . . ? _refine_diff_density_max 0.992 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.165 #==END data_4a _database_code_CSD 169420 _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-hydrido-\m-naphthylthiolato-bis-ax-acetomitrile- hexacarbonyl-dirhenium ; _chemical_formula_moiety 'C20 H14 N2 O6 Re2 S' _chemical_formula_sum 'C20 H14 N2 O6 Re2 S' _chemical_formula_weight 782.79 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' 'N' 'N' 0.0061 0.0033 '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 13.619(3) _cell_length_b 13.340(3) _cell_length_c 14.345(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.48(2) _cell_angle_gamma 90.00 _cell_volume 2332.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 14.025 _cell_measurement_theta_max 35.003 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas not measured _exptl_crystal_density_method '?' _exptl_crystal_density_diffrn 2.229 _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 10.495 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.635 _exptl_absorpt_correction_T_max 0.882 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 16 _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_number 6189 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.0886 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5144 _reflns_number_gt 3206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS (Bruker, 1996)' _computing_cell_refinement 'Bruker XSCANS (Bruker, 1996)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0981P)^2^+8.4504P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5144 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.1941 _refine_ls_wR_factor_gt 0.1666 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.98181(5) 0.82211(5) 0.20595(5) 0.0487(2) Uani 1 1 d . . . Re2 Re 1.03347(5) 0.60140(5) 0.28070(5) 0.0491(2) Uani 1 1 d . . . S1 S 0.9719(3) 0.6699(3) 0.1022(3) 0.0498(9) Uani 1 1 d . . . N1 N 0.8176(10) 0.7853(11) 0.1761(12) 0.060(3) Uani 1 1 d . . . N2 N 1.1961(11) 0.6315(10) 0.3018(11) 0.056(3) Uani 1 1 d . . . C1 C 0.9335(14) 0.9141(13) 0.0918(14) 0.056(4) Uani 1 1 d . . . O1 O 0.9058(13) 0.9708(11) 0.0249(13) 0.090(4) Uani 1 1 d . . . C2 C 0.9811(14) 0.9251(11) 0.2984(14) 0.056(4) Uani 1 1 d . . . O2 O 0.9851(13) 0.9887(12) 0.3506(14) 0.104(5) Uani 1 1 d . . . C3 C 1.1309(14) 0.8584(13) 0.2458(14) 0.060(4) Uani 1 1 d . . . O3 O 1.2205(10) 0.8788(10) 0.2686(12) 0.081(4) Uani 1 1 d . . . C4 C 0.7351(14) 0.7702(14) 0.1746(14) 0.065(5) Uani 1 1 d . . . C5 C 0.6314(16) 0.753(2) 0.174(2) 0.123(10) Uani 1 1 d . . . H5A H 0.6425 0.7252 0.2396 0.185 Uiso 1 1 calc R . . H5B H 0.5899 0.7062 0.1191 0.185 Uiso 1 1 calc R . . H5C H 0.5920 0.8148 0.1619 0.185 Uiso 1 1 calc R . . C6 C 1.0804(16) 0.5751(14) 0.4235(18) 0.068(5) Uani 1 1 d . . . O6 O 1.1077(13) 0.5648(12) 0.5120(13) 0.091(4) Uani 1 1 d . . . C7 C 1.0472(14) 0.4656(13) 0.2561(16) 0.066(5) Uani 1 1 d . . . O7 O 1.0466(12) 0.3792(11) 0.2400(13) 0.089(4) Uani 1 1 d . . . C8 C 0.8863(14) 0.5706(12) 0.2536(15) 0.059(4) Uani 1 1 d . . . O8 O 0.7986(10) 0.5491(11) 0.2325(13) 0.086(4) Uani 1 1 d . . . C9 C 1.2810(13) 0.6426(13) 0.3033(13) 0.060(4) Uani 1 1 d . . . C10 C 1.3833(13) 0.6559(18) 0.3034(19) 0.087(7) Uani 1 1 d . . . H10A H 1.4352 0.6805 0.3701 0.130 Uiso 1 1 calc R . . H10B H 1.3762 0.7033 0.2504 0.130 Uiso 1 1 calc R . . H10C H 1.4083 0.5929 0.2896 0.130 Uiso 1 1 calc R . . C11 C 1.0808(12) 0.6643(11) 0.0658(11) 0.048(3) Uani 1 1 d . . . C12 C 1.1193(14) 0.5685(13) 0.0593(14) 0.062(4) Uani 1 1 d . . . H12 H 1.0928 0.5124 0.0792 0.074 Uiso 1 1 calc R . . C13 C 1.1991(14) 0.5580(12) 0.0220(14) 0.063(4) Uani 1 1 d . . . H13 H 1.2236 0.4945 0.0157 0.075 Uiso 1 1 calc R . . C14 C 1.2420(13) 0.6431(12) -0.0059(12) 0.058(4) Uani 1 1 d . . . C15 C 1.3257(16) 0.6339(15) -0.0355(15) 0.069(5) Uani 1 1 d . . . H15 H 1.3536 0.5709 -0.0381 0.083 Uiso 1 1 calc R . . C16 C 1.3657(18) 0.7141(17) -0.0600(18) 0.086(6) Uani 1 1 d . . . H16 H 1.4162 0.7059 -0.0867 0.103 Uiso 1 1 calc R . . C17 C 1.3344(18) 0.8130(18) -0.0469(16) 0.091(7) Uani 1 1 d . . . H17 H 1.3671 0.8689 -0.0600 0.109 Uiso 1 1 calc R . . C18 C 1.2539(15) 0.8230(13) -0.0142(14) 0.070(5) Uani 1 1 d . . . H18 H 1.2312 0.8868 -0.0061 0.084 Uiso 1 1 calc R . . C19 C 1.2053(13) 0.7385(11) 0.0070(12) 0.050(4) Uani 1 1 d . . . C20 C 1.1225(13) 0.7455(12) 0.0396(11) 0.052(4) Uani 1 1 d . . . H20 H 1.0952 0.8085 0.0432 0.063 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 Re1 0.0410(3) 0.0433(3) 0.0675(4) -0.0067(3) 0.0293(3) -0.0021(2) Re2 0.0433(3) 0.0448(3) 0.0650(4) -0.0034(3) 0.0293(3) -0.0018(3) S1 0.0436(19) 0.049(2) 0.060(2) -0.0055(18) 0.0262(17) -0.0045(16) N1 0.043(7) 0.058(8) 0.087(10) 0.000(7) 0.036(7) 0.002(6) N2 0.049(8) 0.053(8) 0.062(8) -0.001(6) 0.022(6) -0.010(6) C1 0.057(9) 0.051(9) 0.064(11) -0.012(8) 0.031(8) -0.007(7) O1 0.102(11) 0.075(10) 0.102(11) 0.016(9) 0.053(9) 0.014(8) C2 0.076(11) 0.041(8) 0.077(11) -0.026(8) 0.055(10) -0.003(7) O2 0.102(12) 0.093(11) 0.130(13) -0.032(10) 0.065(11) -0.014(9) C3 0.065(11) 0.053(9) 0.073(11) -0.018(8) 0.041(9) -0.007(8) O3 0.052(7) 0.079(9) 0.119(11) -0.012(8) 0.046(7) -0.024(6) C4 0.051(10) 0.071(12) 0.074(12) 0.022(10) 0.028(9) 0.015(8) C5 0.053(11) 0.17(3) 0.17(2) 0.05(2) 0.069(14) 0.015(14) C6 0.077(12) 0.055(10) 0.079(14) -0.006(9) 0.043(11) 0.003(9) O6 0.114(12) 0.083(10) 0.089(11) 0.000(8) 0.056(10) -0.009(8) C7 0.061(10) 0.046(9) 0.098(14) 0.001(9) 0.041(10) 0.003(8) O7 0.080(9) 0.067(9) 0.124(12) -0.002(8) 0.049(9) 0.009(7) C8 0.057(10) 0.045(8) 0.084(12) -0.003(8) 0.038(9) 0.018(7) O8 0.050(7) 0.090(10) 0.125(12) -0.003(9) 0.047(8) -0.004(7) C9 0.048(9) 0.056(10) 0.066(11) 0.015(8) 0.015(8) -0.003(7) C10 0.041(9) 0.098(15) 0.118(17) 0.016(13) 0.033(10) -0.006(10) C11 0.045(8) 0.050(8) 0.047(8) -0.010(7) 0.019(7) -0.001(6) C12 0.059(10) 0.060(10) 0.062(11) -0.005(8) 0.023(9) -0.007(8) C13 0.068(11) 0.042(8) 0.078(12) -0.013(8) 0.033(10) 0.001(8) C14 0.051(9) 0.071(11) 0.046(9) 0.002(8) 0.015(8) 0.001(8) C15 0.082(13) 0.067(11) 0.079(12) -0.002(10) 0.054(11) -0.009(10) C16 0.089(15) 0.081(15) 0.103(16) -0.014(13) 0.055(13) 0.004(12) C17 0.102(16) 0.107(17) 0.081(13) 0.009(12) 0.056(13) -0.050(14) C18 0.091(14) 0.058(9) 0.086(13) -0.001(9) 0.062(12) 0.017(10) C19 0.063(9) 0.034(7) 0.050(9) 0.003(6) 0.022(7) 0.001(6) C20 0.064(10) 0.042(8) 0.048(9) -0.004(6) 0.022(8) 0.006(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 Re1 C3 1.910(17) . ? Re1 C1 1.91(2) . ? Re1 C2 1.913(14) . ? Re1 N1 2.138(13) . ? Re1 S1 2.485(4) . ? Re1 Re2 3.1049(11) . ? Re2 C7 1.870(17) . ? Re2 C6 1.89(2) . ? Re2 C8 1.908(18) . ? Re2 N2 2.136(14) . ? Re2 S1 2.486(4) . ? S1 C11 1.780(16) . ? N1 C4 1.13(2) . ? N2 C9 1.16(2) . ? C1 O1 1.15(2) . ? C2 O2 1.117(19) . ? C3 O3 1.147(19) . ? C4 C5 1.43(2) . ? C6 O6 1.16(2) . ? C7 O7 1.18(2) . ? C8 O8 1.13(2) . ? C9 C10 1.40(2) . ? C11 C20 1.35(2) . ? C11 C12 1.40(2) . ? C12 C13 1.42(3) . ? C13 C14 1.41(2) . ? C14 C15 1.39(2) . ? C14 C19 1.41(2) . ? C15 C16 1.32(3) . ? C16 C17 1.42(3) . ? C17 C18 1.38(3) . ? C18 C19 1.41(2) . ? C19 C20 1.40(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 C3 Re1 C1 90.4(8) . . ? C3 Re1 C2 86.8(7) . . ? C1 Re1 C2 91.5(7) . . ? C3 Re1 N1 174.5(7) . . ? C1 Re1 N1 92.7(6) . . ? C2 Re1 N1 88.6(6) . . ? C3 Re1 S1 98.8(5) . . ? C1 Re1 S1 96.0(5) . . ? C2 Re1 S1 170.5(5) . . ? N1 Re1 S1 85.4(4) . . ? C3 Re1 Re2 95.2(5) . . ? C1 Re1 Re2 147.4(5) . . ? C2 Re1 Re2 120.8(5) . . ? N1 Re1 Re2 84.7(4) . . ? S1 Re1 Re2 51.36(10) . . ? C7 Re2 C6 90.6(8) . . ? C7 Re2 C8 86.4(7) . . ? C6 Re2 C8 89.9(8) . . ? C7 Re2 N2 91.4(7) . . ? C6 Re2 N2 93.0(7) . . ? C8 Re2 N2 176.3(6) . . ? C7 Re2 S1 100.2(6) . . ? C6 Re2 S1 169.1(5) . . ? C8 Re2 S1 91.6(6) . . ? N2 Re2 S1 85.9(4) . . ? C7 Re2 Re1 151.6(6) . . ? C6 Re2 Re1 117.8(5) . . ? C8 Re2 Re1 94.5(5) . . ? N2 Re2 Re1 86.1(4) . . ? S1 Re2 Re1 51.34(9) . . ? C11 S1 Re1 112.3(5) . . ? C11 S1 Re2 110.1(5) . . ? Re1 S1 Re2 77.30(12) . . ? C4 N1 Re1 170.1(16) . . ? C9 N2 Re2 172.8(15) . . ? O1 C1 Re1 178.5(16) . . ? O2 C2 Re1 175.5(16) . . ? O3 C3 Re1 178.7(16) . . ? N1 C4 C5 179(3) . . ? O6 C6 Re2 175.9(17) . . ? O7 C7 Re2 174.0(16) . . ? O8 C8 Re2 175.9(16) . . ? N2 C9 C10 179(2) . . ? C20 C11 C12 119.7(15) . . ? C20 C11 S1 123.8(12) . . ? C12 C11 S1 116.4(12) . . ? C11 C12 C13 119.3(16) . . ? C14 C13 C12 120.7(15) . . ? C15 C14 C19 120.5(16) . . ? C15 C14 C13 120.9(16) . . ? C19 C14 C13 118.2(16) . . ? C16 C15 C14 120.2(19) . . ? C15 C16 C17 122(2) . . ? C18 C17 C16 117.7(18) . . ? C17 C18 C19 121.2(16) . . ? C20 C19 C18 122.9(14) . . ? C20 C19 C14 119.3(14) . . ? C18 C19 C14 117.8(15) . . ? C11 C20 C19 122.6(14) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.291 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.243 #==END data_5b _database_code_CSD 169421 _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-hydrido-\m-naphthylthiolato-\m-bis-diphenylphosphino- ethane-hexacarbonyl-dirhenium ; _chemical_formula_moiety 'C42 H32 O6 P2 Re2 S, C3 H6 O' _chemical_formula_sum 'C45 H38 O7 P2 Re2 S' _chemical_formula_weight 1157.15 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' 'P' 'P' 0.1023 0.0942 '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 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 16.715(4) _cell_length_b 18.225(3) _cell_length_c 15.022(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.41(1) _cell_angle_gamma 90.00 _cell_volume 4342.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 6.693 _cell_measurement_theta_max 17.456 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method '?' _exptl_crystal_density_diffrn 1.770 _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 5.741 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.569 _exptl_absorpt_correction_T_max 0.847 _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 6 _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_number 11764 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.1049 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9962 _reflns_number_gt 6019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS (Bruker, 1996)' _computing_cell_refinement 'Bruker XSCANS (Bruker, 1996)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0416P)^2^] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9962 _refine_ls_number_parameters 494 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _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 0.21730(2) 0.56838(2) 0.17637(3) 0.03552(11) Uani 1 1 d . . . Re2 Re 0.38115(2) 0.48471(2) 0.29343(3) 0.03666(11) Uani 1 1 d . . . S1 S 0.25900(14) 0.43780(12) 0.16324(16) 0.0383(5) Uani 1 1 d . . . P1 P 0.26203(15) 0.61011(13) 0.04242(17) 0.0389(6) Uani 1 1 d . . . P2 P 0.45627(14) 0.48905(13) 0.17630(17) 0.0382(6) Uani 1 1 d . . . O1 O 0.1286(5) 0.5291(5) 0.3212(5) 0.073(2) Uani 1 1 d . . . C1 C 0.1674(5) 0.5410(5) 0.2740(7) 0.043(2) Uani 1 1 d . . . O2 O 0.2029(5) 0.7261(4) 0.2365(6) 0.077(2) Uani 1 1 d . . . C2 C 0.2091(6) 0.6683(5) 0.2109(7) 0.046(2) Uani 1 1 d . . . C3 C 0.1036(6) 0.5724(5) 0.0934(7) 0.045(2) Uani 1 1 d . . . O3 O 0.0352(4) 0.5746(4) 0.0438(5) 0.068(2) Uani 1 1 d . . . O4 O 0.4677(5) 0.3396(4) 0.3696(5) 0.072(2) Uani 1 1 d . . . C4 C 0.4353(6) 0.3949(6) 0.3400(7) 0.048(3) Uani 1 1 d . . . O5 O 0.3018(5) 0.4728(5) 0.4527(5) 0.081(3) Uani 1 1 d . . . C5 C 0.3271(6) 0.4774(5) 0.3910(7) 0.051(3) Uani 1 1 d . . . O6 O 0.5150(6) 0.5734(5) 0.4391(6) 0.088(3) Uani 1 1 d . . . C6 C 0.4667(7) 0.5385(6) 0.3824(7) 0.055(3) Uani 1 1 d . . . C11 C 0.2500(7) 0.7100(5) 0.0253(6) 0.050(3) Uani 1 1 d D . . C12 C 0.3170(7) 0.7558(5) 0.0335(6) 0.057(3) Uani 1 1 d D . . H12 H 0.3711 0.7366 0.0473 0.068 Uiso 1 1 calc R . . C13 C 0.3041(9) 0.8306(7) 0.0214(8) 0.079(4) Uani 1 1 d D . . H13 H 0.3501 0.8609 0.0264 0.095 Uiso 1 1 calc R . . C14 C 0.2286(10) 0.8604(6) 0.0031(8) 0.081(4) Uani 1 1 d D . . H14 H 0.2219 0.9110 -0.0045 0.097 Uiso 1 1 calc R . . C15 C 0.1591(9) 0.8156(7) -0.0049(9) 0.089(4) Uani 1 1 d D . . H15 H 0.1055 0.8359 -0.0181 0.107 Uiso 1 1 calc R . . C16 C 0.1703(7) 0.7406(6) 0.0069(8) 0.072(3) Uani 1 1 d D . . H16 H 0.1243 0.7105 0.0026 0.087 Uiso 1 1 calc R . . C21 C 0.2019(5) 0.5758(5) -0.0721(6) 0.038(2) Uani 1 1 d D . . C22 C 0.1533(6) 0.5118(5) -0.0832(7) 0.053(3) Uani 1 1 d D . . H22 H 0.1524 0.4846 -0.0312 0.064 Uiso 1 1 calc R . . C23 C 0.1064(7) 0.4894(7) -0.1731(9) 0.073(3) Uani 1 1 d D . . H23 H 0.0746 0.4466 -0.1801 0.087 Uiso 1 1 calc R . . C24 C 0.1054(7) 0.5272(7) -0.2499(8) 0.074(4) Uani 1 1 d D . . H24 H 0.0719 0.5117 -0.3088 0.089 Uiso 1 1 calc R . . C25 C 0.1537(7) 0.5886(7) -0.2413(8) 0.067(3) Uani 1 1 d D . . H25 H 0.1536 0.6145 -0.2947 0.080 Uiso 1 1 calc R . . C26 C 0.2034(7) 0.6129(6) -0.1531(7) 0.061(3) Uani 1 1 d D . . H26 H 0.2377 0.6538 -0.1481 0.074 Uiso 1 1 calc R . . C31 C 0.3701(5) 0.5941(5) 0.0417(7) 0.048(3) Uani 1 1 d . . . H31A H 0.3749 0.6109 -0.0176 0.057 Uiso 1 1 calc R . . H31B H 0.4085 0.6231 0.0912 0.057 Uiso 1 1 calc R . . C32 C 0.3965(5) 0.5147(5) 0.0555(6) 0.042(2) Uani 1 1 d . . . H32A H 0.4305 0.5036 0.0155 0.050 Uiso 1 1 calc R . . H32B H 0.3463 0.4843 0.0349 0.050 Uiso 1 1 calc R . . C41 C 0.4998(6) 0.3997(5) 0.1590(7) 0.044(2) Uani 1 1 d D . . C42 C 0.5702(6) 0.3738(6) 0.2249(8) 0.063(3) Uani 1 1 d D . . H42 H 0.5967 0.4028 0.2767 0.076 Uiso 1 1 calc R . . C43 C 0.6034(8) 0.3056(7) 0.2169(9) 0.075(4) Uani 1 1 d D . . H43 H 0.6512 0.2888 0.2632 0.089 Uiso 1 1 calc R . . C44 C 0.5654(10) 0.2630(7) 0.1407(12) 0.091(5) Uani 1 1 d D . . H44 H 0.5883 0.2178 0.1335 0.109 Uiso 1 1 calc R . . C45 C 0.4953(9) 0.2865(7) 0.0768(10) 0.083(4) Uani 1 1 d D . . H45 H 0.4682 0.2560 0.0268 0.099 Uiso 1 1 calc R . . C46 C 0.4609(7) 0.3563(6) 0.0826(8) 0.065(3) Uani 1 1 d D . . H46 H 0.4131 0.3725 0.0359 0.078 Uiso 1 1 calc R . . C51 C 0.5463(6) 0.5521(5) 0.2017(6) 0.044(2) Uani 1 1 d D . . C52 C 0.5383(6) 0.6196(6) 0.2395(7) 0.058(3) Uani 1 1 d D . . H52 H 0.4905 0.6298 0.2564 0.070 Uiso 1 1 calc R . . C53 C 0.6002(8) 0.6720(6) 0.2527(8) 0.075(4) Uani 1 1 d D . . H53 H 0.5940 0.7175 0.2776 0.090 Uiso 1 1 calc R . . C54 C 0.6711(8) 0.6568(8) 0.2288(10) 0.095(5) Uani 1 1 d D . . H54 H 0.7127 0.6923 0.2368 0.114 Uiso 1 1 calc R . . C55 C 0.6810(7) 0.5889(8) 0.1931(9) 0.080(4) Uani 1 1 d D . . H55 H 0.7300 0.5780 0.1789 0.096 Uiso 1 1 calc R . . C56 C 0.6172(6) 0.5365(6) 0.1784(7) 0.056(3) Uani 1 1 d D . . H56 H 0.6229 0.4911 0.1528 0.067 Uiso 1 1 calc R . . C61 C 0.1911(6) 0.3812(5) 0.2078(6) 0.040(2) Uani 1 1 d D . . C62 C 0.2228(7) 0.3387(5) 0.2842(7) 0.058(3) Uani 1 1 d D . . H62 H 0.2807 0.3372 0.3143 0.070 Uiso 1 1 calc R . . C63 C 0.1680(8) 0.2962(5) 0.3191(8) 0.071(3) Uani 1 1 d D . . C64 C 0.2004(10) 0.2506(6) 0.3997(10) 0.096(5) Uani 1 1 d D . . H64 H 0.2582 0.2478 0.4299 0.115 Uiso 1 1 calc R . . C65 C 0.1453(14) 0.2108(8) 0.4324(13) 0.134(7) Uani 1 1 d D . . H65 H 0.1659 0.1803 0.4842 0.161 Uiso 1 1 calc R . . C66 C 0.0585(14) 0.2164(10) 0.3873(17) 0.157(10) Uani 1 1 d D . . H66 H 0.0216 0.1914 0.4117 0.189 Uiso 1 1 calc R . . C67 C 0.0273(12) 0.2572(8) 0.3096(15) 0.126(7) Uani 1 1 d D . . H67 H -0.0306 0.2585 0.2792 0.152 Uiso 1 1 calc R . . C68 C 0.0818(10) 0.2979(6) 0.2741(11) 0.085(4) Uani 1 1 d D . . C69 C 0.0515(7) 0.3424(7) 0.1933(10) 0.082(4) Uani 1 1 d D . . H69 H -0.0060 0.3433 0.1610 0.098 Uiso 1 1 calc R . . C70 C 0.1048(7) 0.3843(6) 0.1616(8) 0.063(3) Uani 1 1 d D . . H70 H 0.0835 0.4145 0.1096 0.076 Uiso 1 1 calc R . . H1 H 0.3355 0.5818 0.2590 0.080 Uiso 1 1 d . . . C100 C -0.070(2) 0.8882(17) -0.029(2) 0.296(19) Uiso 1 1 d D . . C101 C -0.0947(9) 0.8380(8) -0.1159(10) 0.113(5) Uiso 1 1 d D . . H10A H -0.0460 0.8112 -0.1186 0.170 Uiso 1 1 calc R . . H10B H -0.1161 0.8672 -0.1716 0.170 Uiso 1 1 calc R . . H10C H -0.1374 0.8041 -0.1118 0.170 Uiso 1 1 calc R . . C102 C -0.1525(15) 0.9234(12) -0.0340(16) 0.219(11) Uiso 1 1 d D . . H10D H -0.1444 0.9557 0.0186 0.328 Uiso 1 1 calc R . . H10E H -0.1926 0.8860 -0.0324 0.328 Uiso 1 1 calc R . . H10F H -0.1734 0.9509 -0.0912 0.328 Uiso 1 1 calc R . . O100 O -0.0219(15) 0.9286(13) 0.0031(18) 0.313(13) 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 Re1 0.03406(19) 0.03610(19) 0.0378(2) -0.00067(19) 0.01339(16) -0.00011(17) Re2 0.0371(2) 0.0415(2) 0.0324(2) 0.00368(19) 0.01235(16) 0.00292(18) S1 0.0403(12) 0.0375(12) 0.0405(13) 0.0028(11) 0.0178(11) 0.0037(11) P1 0.0369(13) 0.0378(13) 0.0433(15) 0.0054(12) 0.0148(12) 0.0029(11) P2 0.0347(12) 0.0417(13) 0.0398(14) 0.0048(12) 0.0141(11) 0.0085(11) O1 0.067(5) 0.100(6) 0.068(5) -0.008(5) 0.044(5) -0.010(5) C1 0.031(5) 0.052(6) 0.050(6) -0.003(5) 0.018(5) 0.000(4) O2 0.088(6) 0.051(5) 0.098(7) -0.029(5) 0.037(5) -0.005(4) C2 0.039(5) 0.042(6) 0.050(6) -0.005(5) 0.007(5) 0.000(5) C3 0.054(6) 0.028(5) 0.054(6) -0.010(5) 0.018(5) -0.004(5) O3 0.044(4) 0.081(6) 0.066(5) -0.017(5) 0.001(4) 0.005(4) O4 0.084(6) 0.062(5) 0.072(6) 0.021(5) 0.026(5) 0.026(4) C4 0.045(6) 0.060(7) 0.045(6) 0.005(6) 0.022(5) 0.012(5) O5 0.086(6) 0.117(7) 0.058(5) 0.013(5) 0.048(5) 0.007(5) C5 0.043(6) 0.053(6) 0.060(7) 0.018(6) 0.021(5) 0.011(5) O6 0.099(7) 0.101(7) 0.047(5) 0.005(5) 0.000(5) -0.015(6) C6 0.057(7) 0.078(8) 0.022(5) 0.002(5) -0.001(5) 0.017(6) C11 0.069(7) 0.043(6) 0.037(6) 0.003(5) 0.016(5) -0.003(6) C12 0.057(7) 0.048(6) 0.057(7) 0.007(6) 0.007(6) -0.007(5) C13 0.085(10) 0.059(8) 0.086(10) 0.008(8) 0.016(8) -0.018(7) C14 0.131(13) 0.039(7) 0.075(9) 0.010(7) 0.037(9) -0.002(8) C15 0.109(11) 0.064(8) 0.084(10) 0.029(8) 0.015(9) 0.039(8) C16 0.068(8) 0.055(7) 0.099(10) 0.023(7) 0.032(7) 0.016(6) C21 0.038(5) 0.038(5) 0.038(5) 0.013(5) 0.011(4) 0.006(4) C22 0.066(7) 0.050(6) 0.043(6) 0.002(5) 0.018(5) 0.011(6) C23 0.080(9) 0.071(8) 0.066(8) -0.016(7) 0.021(7) 0.000(7) C24 0.072(8) 0.096(10) 0.044(7) -0.014(7) 0.003(6) 0.004(8) C25 0.084(9) 0.077(8) 0.040(7) 0.007(6) 0.020(6) 0.002(7) C26 0.079(8) 0.055(7) 0.047(7) 0.005(6) 0.015(6) -0.004(6) C31 0.038(5) 0.055(6) 0.048(6) 0.023(5) 0.009(5) -0.002(5) C32 0.032(5) 0.058(6) 0.036(5) 0.007(5) 0.012(4) 0.010(5) C41 0.051(6) 0.034(5) 0.059(7) 0.012(5) 0.034(5) 0.009(5) C42 0.066(7) 0.066(7) 0.059(7) 0.010(6) 0.022(6) 0.024(6) C43 0.082(9) 0.074(9) 0.088(10) 0.024(8) 0.055(8) 0.041(7) C44 0.126(13) 0.051(8) 0.137(14) 0.016(9) 0.100(12) 0.027(9) C45 0.102(11) 0.052(8) 0.109(12) -0.005(8) 0.052(9) 0.002(7) C46 0.059(7) 0.053(7) 0.082(9) -0.004(7) 0.020(7) 0.000(6) C51 0.044(6) 0.042(6) 0.053(6) 0.010(5) 0.024(5) 0.003(5) C52 0.056(7) 0.053(7) 0.075(8) 0.001(6) 0.034(6) 0.001(6) C53 0.087(9) 0.052(7) 0.096(10) 0.001(7) 0.043(8) -0.006(7) C54 0.061(8) 0.097(11) 0.131(13) -0.007(10) 0.037(9) -0.024(8) C55 0.046(7) 0.112(11) 0.090(10) -0.002(9) 0.033(7) -0.006(8) C56 0.045(6) 0.072(7) 0.057(7) -0.003(6) 0.024(5) -0.004(6) C61 0.044(5) 0.034(5) 0.047(6) -0.003(5) 0.022(5) 0.000(4) C62 0.057(7) 0.050(6) 0.072(8) 0.013(6) 0.027(6) 0.002(5) C63 0.089(10) 0.051(7) 0.090(10) 0.013(7) 0.055(8) 0.007(7) C64 0.133(13) 0.066(8) 0.114(12) 0.020(9) 0.075(11) -0.004(9) C65 0.20(2) 0.080(11) 0.165(18) 0.054(11) 0.127(18) 0.007(14) C66 0.17(2) 0.091(14) 0.27(3) 0.013(16) 0.16(2) -0.025(15) C67 0.151(16) 0.059(9) 0.21(2) -0.011(12) 0.120(16) -0.021(10) C68 0.102(11) 0.039(6) 0.142(14) -0.003(8) 0.078(11) -0.013(7) C69 0.051(7) 0.064(8) 0.133(12) -0.022(9) 0.032(8) -0.032(6) C70 0.062(7) 0.051(7) 0.068(8) 0.003(6) 0.008(6) -0.009(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 C2 1.910(10) . ? Re1 C3 1.918(10) . ? Re1 C1 1.966(9) . ? Re1 P1 2.477(2) . ? Re1 S1 2.505(2) . ? Re1 Re2 3.1427(7) . ? Re2 C6 1.893(11) . ? Re2 C4 1.895(10) . ? Re2 C5 1.955(10) . ? Re2 P2 2.464(2) . ? Re2 S1 2.490(2) . ? S1 C61 1.811(9) . ? P1 C21 1.808(9) . ? P1 C31 1.833(9) . ? P1 C11 1.841(10) . ? P2 C32 1.834(9) . ? P2 C41 1.834(9) . ? P2 C51 1.835(9) . ? O1 C1 1.123(10) . ? O2 C2 1.137(10) . ? C3 O3 1.150(10) . ? O4 C4 1.163(11) . ? O5 C5 1.136(11) . ? O6 C6 1.160(12) . ? C11 C12 1.369(13) . ? C11 C16 1.389(13) . ? C12 C13 1.383(14) . ? C13 C14 1.320(16) . ? C14 C15 1.396(16) . ? C15 C16 1.384(15) . ? C21 C26 1.399(12) . ? C21 C22 1.400(12) . ? C22 C23 1.391(14) . ? C23 C24 1.340(15) . ? C24 C25 1.362(15) . ? C25 C26 1.395(14) . ? C31 C32 1.509(12) . ? C41 C42 1.360(13) . ? C41 C46 1.378(13) . ? C42 C43 1.382(14) . ? C43 C44 1.362(17) . ? C44 C45 1.329(17) . ? C45 C46 1.410(15) . ? C51 C56 1.366(12) . ? C51 C52 1.380(13) . ? C52 C53 1.376(14) . ? C53 C54 1.370(15) . ? C54 C55 1.379(16) . ? C55 C56 1.396(14) . ? C61 C62 1.347(12) . ? C61 C70 1.391(13) . ? C62 C63 1.421(13) . ? C63 C68 1.386(17) . ? C63 C64 1.426(16) . ? C64 C65 1.378(17) . ? C65 C66 1.40(2) . ? C66 C67 1.34(2) . ? C67 C68 1.404(17) . ? C68 C69 1.414(17) . ? C69 C70 1.368(14) . ? C100 O100 1.09(4) . ? C100 C102 1.50(3) . ? C100 C101 1.54(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 Re1 C3 89.9(4) . . ? C2 Re1 C1 87.5(4) . . ? C3 Re1 C1 85.8(4) . . ? C2 Re1 P1 89.6(3) . . ? C3 Re1 P1 87.2(3) . . ? C1 Re1 P1 172.5(3) . . ? C2 Re1 S1 166.6(3) . . ? C3 Re1 S1 103.2(3) . . ? C1 Re1 S1 90.7(3) . . ? P1 Re1 S1 93.72(7) . . ? C2 Re1 Re2 115.8(3) . . ? C3 Re1 Re2 153.2(3) . . ? C1 Re1 Re2 87.7(3) . . ? P1 Re1 Re2 99.80(6) . . ? S1 Re1 Re2 50.81(5) . . ? C6 Re2 C4 91.2(4) . . ? C6 Re2 C5 86.0(4) . . ? C4 Re2 C5 86.8(4) . . ? C6 Re2 P2 92.6(3) . . ? C4 Re2 P2 90.0(3) . . ? C5 Re2 P2 176.5(3) . . ? C6 Re2 S1 168.9(3) . . ? C4 Re2 S1 99.8(3) . . ? C5 Re2 S1 96.2(3) . . ? P2 Re2 S1 85.79(8) . . ? C6 Re2 Re1 118.3(3) . . ? C4 Re2 Re1 148.9(3) . . ? C5 Re2 Re1 85.7(3) . . ? P2 Re2 Re1 97.78(6) . . ? S1 Re2 Re1 51.22(5) . . ? C61 S1 Re2 111.1(3) . . ? C61 S1 Re1 106.9(3) . . ? Re2 S1 Re1 77.97(7) . . ? C21 P1 C31 101.1(4) . . ? C21 P1 C11 101.9(4) . . ? C31 P1 C11 102.7(4) . . ? C21 P1 Re1 116.5(3) . . ? C31 P1 Re1 120.4(3) . . ? C11 P1 Re1 111.7(3) . . ? C32 P2 C41 101.7(4) . . ? C32 P2 C51 101.6(4) . . ? C41 P2 C51 104.4(4) . . ? C32 P2 Re2 118.2(3) . . ? C41 P2 Re2 112.7(3) . . ? C51 P2 Re2 116.2(3) . . ? O1 C1 Re1 170.2(9) . . ? O2 C2 Re1 175.4(9) . . ? O3 C3 Re1 179.7(11) . . ? O4 C4 Re2 178.8(9) . . ? O5 C5 Re2 174.7(9) . . ? O6 C6 Re2 175.5(10) . . ? C12 C11 C16 118.6(10) . . ? C12 C11 P1 122.7(8) . . ? C16 C11 P1 118.6(8) . . ? C11 C12 C13 120.0(11) . . ? C14 C13 C12 122.1(12) . . ? C13 C14 C15 119.5(12) . . ? C16 C15 C14 119.5(12) . . ? C15 C16 C11 120.3(12) . . ? C26 C21 C22 117.9(9) . . ? C26 C21 P1 120.2(7) . . ? C22 C21 P1 122.0(7) . . ? C23 C22 C21 119.3(10) . . ? C24 C23 C22 122.2(12) . . ? C23 C24 C25 119.8(11) . . ? C24 C25 C26 120.5(11) . . ? C25 C26 C21 120.3(10) . . ? C32 C31 P1 113.4(6) . . ? C31 C32 P2 115.1(7) . . ? C42 C41 C46 118.5(9) . . ? C42 C41 P2 119.8(8) . . ? C46 C41 P2 121.6(8) . . ? C41 C42 C43 121.9(12) . . ? C44 C43 C42 119.4(12) . . ? C45 C44 C43 119.7(12) . . ? C44 C45 C46 122.0(13) . . ? C41 C46 C45 118.4(11) . . ? C56 C51 C52 119.8(9) . . ? C56 C51 P2 122.5(8) . . ? C52 C51 P2 117.6(7) . . ? C53 C52 C51 120.7(10) . . ? C54 C53 C52 119.7(11) . . ? C53 C54 C55 120.2(12) . . ? C54 C55 C56 119.7(11) . . ? C51 C56 C55 119.9(11) . . ? C62 C61 C70 121.0(9) . . ? C62 C61 S1 121.3(8) . . ? C70 C61 S1 117.7(8) . . ? C61 C62 C63 120.2(10) . . ? C68 C63 C62 120.0(12) . . ? C68 C63 C64 119.0(12) . . ? C62 C63 C64 121.0(12) . . ? C65 C64 C63 119.4(15) . . ? C64 C65 C66 119.8(17) . . ? C67 C66 C65 121.3(18) . . ? C66 C67 C68 120(2) . . ? C63 C68 C67 120.1(16) . . ? C63 C68 C69 117.8(11) . . ? C67 C68 C69 122.0(16) . . ? C70 C69 C68 121.6(12) . . ? C69 C70 C61 119.4(11) . . ? O100 C100 C102 106(2) . . ? O100 C100 C101 138(3) . . ? C102 C100 C101 103(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 1.004 _refine_diff_density_min -1.003 _refine_diff_density_rms 0.173 #==END data_7 _database_code_CSD 169422 _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-hydrido-\m-thiolato-bis-ax-triphenylphospine- hexacarbonyl-dirhenium ; _chemical_formula_moiety 'C42 H32 O6 P2 Re2 S' _chemical_formula_sum 'C42 H32 O6 P2 Re2 S' _chemical_formula_weight 1099.08 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' 'P' 'P' 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.615(1) _cell_length_b 10.683(1) _cell_length_c 19.747(2) _cell_angle_alpha 75.86(1) _cell_angle_beta 78.98(1) _cell_angle_gamma 68.87(1) _cell_volume 2012.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 6.995 _cell_measurement_theta_max 17.556 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 6.187 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.440 _exptl_absorpt_correction_T_max 0.980 _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 'Bruker P4' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% 7 _diffrn_reflns_number 10631 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9164 _reflns_number_gt 6842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS (Bruker, 1996)' _computing_cell_refinement 'Bruker XSCANS (Bruker, 1996)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0432P)^2^+1.4356P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9164 _refine_ls_number_parameters 481 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.039 _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 0.57954(2) 0.46876(2) 0.219942(11) 0.03721(7) Uani 1 1 d D . . Re2 Re 0.83730(2) 0.49341(2) 0.268177(11) 0.04033(7) Uani 1 1 d D . . S1 S 0.82384(16) 0.38295(17) 0.17344(8) 0.0504(4) Uani 1 1 d . . . P1 P 0.53162(14) 0.69255(14) 0.13619(7) 0.0357(3) Uani 1 1 d . . . P2 P 0.89932(15) 0.28305(15) 0.36051(8) 0.0404(3) Uani 1 1 d . . . O1 O 0.3081(5) 0.5841(5) 0.3077(3) 0.0743(14) Uani 1 1 d . . . C1 C 0.4085(7) 0.5417(6) 0.2733(3) 0.0508(15) Uani 1 1 d . . . O2 O 0.5970(6) 0.1874(5) 0.3122(3) 0.0820(16) Uani 1 1 d . . . C2 C 0.5985(7) 0.2899(6) 0.2795(3) 0.0500(15) Uani 1 1 d . . . O3 O 0.4406(6) 0.3873(5) 0.1235(3) 0.0717(14) Uani 1 1 d . . . C3 C 0.4954(7) 0.4178(6) 0.1588(3) 0.0492(14) Uani 1 1 d . . . O4 O 0.7643(6) 0.6488(5) 0.3895(3) 0.0740(14) Uani 1 1 d . . . C4 C 0.7962(7) 0.5908(6) 0.3426(3) 0.0514(15) Uani 1 1 d . . . O5 O 0.8251(5) 0.7738(5) 0.1777(3) 0.0778(15) Uani 1 1 d . . . C5 C 0.8187(6) 0.6692(7) 0.2071(3) 0.0504(15) Uani 1 1 d . . . O6 O 1.1433(5) 0.4530(7) 0.2366(3) 0.0954(19) Uani 1 1 d . . . C6 C 1.0289(7) 0.4664(7) 0.2505(4) 0.0611(17) Uani 1 1 d . . . C11 C 0.4787(5) 0.8460(5) 0.1743(3) 0.0384(12) Uani 1 1 d D . . C12 C 0.4163(6) 0.9749(6) 0.1347(3) 0.0525(15) Uani 1 1 d D . . H12 H 0.3999 0.9825 0.0891 0.063 Uiso 1 1 calc R . . C13 C 0.3794(7) 1.0896(6) 0.1628(4) 0.0630(18) Uani 1 1 d D . . H13 H 0.3393 1.1749 0.1358 0.076 Uiso 1 1 calc R . . C14 C 0.4011(8) 1.0800(7) 0.2308(4) 0.0651(19) Uani 1 1 d D . . H14 H 0.3755 1.1584 0.2497 0.078 Uiso 1 1 calc R . . C15 C 0.4603(8) 0.9546(7) 0.2703(4) 0.0650(19) Uani 1 1 d D . . H15 H 0.4747 0.9470 0.3163 0.078 Uiso 1 1 calc R . . C16 C 0.4990(6) 0.8386(6) 0.2412(3) 0.0493(14) Uani 1 1 d D . . H16 H 0.5399 0.7536 0.2682 0.059 Uiso 1 1 calc R . . C21 C 0.6660(5) 0.7102(6) 0.0653(3) 0.0433(13) Uani 1 1 d D . . C22 C 0.7253(6) 0.6042(7) 0.0268(3) 0.0553(16) Uani 1 1 d D . . H22 H 0.6959 0.5287 0.0382 0.066 Uiso 1 1 calc R . . C23 C 0.8266(7) 0.6116(8) -0.0276(3) 0.070(2) Uani 1 1 d D . . H23 H 0.8657 0.5413 -0.0529 0.084 Uiso 1 1 calc R . . C24 C 0.8696(8) 0.7240(10) -0.0444(4) 0.085(3) Uani 1 1 d D . . H24 H 0.9386 0.7286 -0.0809 0.102 Uiso 1 1 calc R . . C25 C 0.8124(7) 0.8281(8) -0.0083(4) 0.068(2) Uani 1 1 d D . . H25 H 0.8421 0.9034 -0.0203 0.082 Uiso 1 1 calc R . . C26 C 0.7094(6) 0.8222(7) 0.0466(3) 0.0500(15) Uani 1 1 d D . . H26 H 0.6697 0.8941 0.0708 0.060 Uiso 1 1 calc R . . C31 C 0.3884(6) 0.7304(5) 0.0866(3) 0.0423(13) Uani 1 1 d D . . C32 C 0.2630(7) 0.7301(7) 0.1240(4) 0.0668(19) Uani 1 1 d D . . H32 H 0.2531 0.7084 0.1728 0.080 Uiso 1 1 calc R . . C33 C 0.1515(8) 0.7633(9) 0.0863(6) 0.094(3) Uani 1 1 d D . . H33 H 0.0665 0.7661 0.1103 0.112 Uiso 1 1 calc R . . C34 C 0.1680(8) 0.7916(10) 0.0143(6) 0.093(3) Uani 1 1 d D . . H34 H 0.0947 0.8085 -0.0099 0.111 Uiso 1 1 calc R . . C35 C 0.2878(8) 0.7955(9) -0.0223(4) 0.088(3) Uani 1 1 d D . . H35 H 0.2961 0.8190 -0.0711 0.106 Uiso 1 1 calc R . . C36 C 0.3984(7) 0.7642(8) 0.0137(4) 0.068(2) Uani 1 1 d D . . H36 H 0.4814 0.7658 -0.0116 0.082 Uiso 1 1 calc R . . C41 C 0.9320(6) 0.1185(6) 0.3377(3) 0.0476(14) Uani 1 1 d D . . C42 C 0.8751(7) 0.0235(7) 0.3769(4) 0.0610(17) Uani 1 1 d D . . H42 H 0.8155 0.0415 0.4171 0.073 Uiso 1 1 calc R . . C43 C 0.9080(9) -0.1010(7) 0.3555(5) 0.084(3) Uani 1 1 d D . . H43 H 0.8696 -0.1659 0.3822 0.101 Uiso 1 1 calc R . . C44 C 0.9941(10) -0.1296(8) 0.2971(5) 0.086(3) Uani 1 1 d D . . H44 H 1.0139 -0.2127 0.2835 0.103 Uiso 1 1 calc R . . C45 C 1.0519(9) -0.0350(8) 0.2581(4) 0.085(3) Uani 1 1 d D . . H45 H 1.1117 -0.0547 0.2181 0.102 Uiso 1 1 calc R . . C46 C 1.0227(7) 0.0882(7) 0.2773(3) 0.0624(18) Uani 1 1 d D . . H46 H 1.0627 0.1516 0.2504 0.075 Uiso 1 1 calc R . . C51 C 0.7803(6) 0.2851(5) 0.4414(3) 0.0440(13) Uani 1 1 d D . . C52 C 0.6425(6) 0.3389(6) 0.4379(3) 0.0500(14) Uani 1 1 d D . . H52 H 0.6098 0.3750 0.3944 0.060 Uiso 1 1 calc R . . C53 C 0.5532(7) 0.3399(7) 0.4976(4) 0.0599(17) Uani 1 1 d D . . H53 H 0.4603 0.3744 0.4941 0.072 Uiso 1 1 calc R . . C54 C 0.5988(9) 0.2902(7) 0.5635(4) 0.069(2) Uani 1 1 d D . . H54 H 0.5376 0.2923 0.6041 0.083 Uiso 1 1 calc R . . C55 C 0.7356(9) 0.2382(8) 0.5674(4) 0.076(2) Uani 1 1 d D . . H55 H 0.7675 0.2052 0.6112 0.092 Uiso 1 1 calc R . . C56 C 0.8272(8) 0.2336(7) 0.5076(3) 0.0618(18) Uani 1 1 d D . . H56 H 0.9200 0.1963 0.5112 0.074 Uiso 1 1 calc R . . C61 C 1.0573(6) 0.2580(6) 0.3949(3) 0.0485(14) Uani 1 1 d D . . C62 C 1.0768(8) 0.3646(7) 0.4143(4) 0.077(2) Uani 1 1 d D . . H62 H 1.0102 0.4503 0.4087 0.093 Uiso 1 1 calc R . . C63 C 1.1950(10) 0.3459(10) 0.4422(5) 0.098(3) Uani 1 1 d D . . H63 H 1.2079 0.4189 0.4542 0.118 Uiso 1 1 calc R . . C64 C 1.2922(9) 0.2184(10) 0.4517(4) 0.087(3) Uani 1 1 d D . . H64 H 1.3706 0.2053 0.4708 0.105 Uiso 1 1 calc R . . C65 C 1.2752(8) 0.1123(10) 0.4337(4) 0.085(3) Uani 1 1 d D . . H65 H 1.3418 0.0267 0.4401 0.102 Uiso 1 1 calc R . . C66 C 1.1576(7) 0.1309(8) 0.4054(4) 0.0675(19) Uani 1 1 d D . . H66 H 1.1462 0.0571 0.3933 0.081 Uiso 1 1 calc R . . H1 H 0.657(4) 0.517(7) 0.279(3) 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 Re1 0.04321(14) 0.04028(12) 0.03099(12) -0.00913(9) -0.00242(10) -0.01653(10) Re2 0.04294(14) 0.04779(14) 0.03168(12) -0.00206(9) -0.00508(10) -0.01982(10) S1 0.0470(8) 0.0628(9) 0.0362(8) -0.0167(7) -0.0020(7) -0.0087(7) P1 0.0372(7) 0.0427(7) 0.0281(7) -0.0083(6) -0.0013(6) -0.0145(6) P2 0.0437(8) 0.0426(8) 0.0364(8) -0.0069(6) -0.0065(6) -0.0154(6) O1 0.062(3) 0.091(4) 0.070(3) -0.033(3) 0.024(3) -0.030(3) C1 0.063(4) 0.054(4) 0.039(3) -0.009(3) -0.001(3) -0.026(3) O2 0.102(4) 0.057(3) 0.096(4) 0.010(3) -0.036(3) -0.040(3) C2 0.063(4) 0.050(3) 0.043(3) -0.007(3) -0.011(3) -0.024(3) O3 0.099(4) 0.076(3) 0.059(3) -0.023(3) -0.020(3) -0.039(3) C3 0.061(4) 0.047(3) 0.043(3) -0.011(3) -0.008(3) -0.019(3) O4 0.101(4) 0.071(3) 0.062(3) -0.026(3) -0.005(3) -0.036(3) C4 0.067(4) 0.046(3) 0.049(4) -0.005(3) -0.004(3) -0.031(3) O5 0.090(4) 0.081(3) 0.071(3) 0.025(3) -0.031(3) -0.053(3) C5 0.053(4) 0.065(4) 0.037(3) 0.002(3) -0.006(3) -0.032(3) O6 0.053(3) 0.132(5) 0.095(5) 0.004(4) -0.003(3) -0.043(3) C6 0.059(4) 0.080(5) 0.047(4) 0.001(3) -0.010(3) -0.033(4) C11 0.038(3) 0.041(3) 0.040(3) -0.011(2) 0.000(2) -0.019(2) C12 0.064(4) 0.051(3) 0.044(3) -0.004(3) -0.013(3) -0.020(3) C13 0.070(5) 0.045(3) 0.075(5) -0.010(3) -0.021(4) -0.014(3) C14 0.080(5) 0.047(4) 0.072(5) -0.025(3) -0.006(4) -0.020(3) C15 0.093(6) 0.057(4) 0.047(4) -0.015(3) -0.008(4) -0.024(4) C16 0.065(4) 0.043(3) 0.038(3) -0.009(2) -0.005(3) -0.015(3) C21 0.033(3) 0.063(4) 0.031(3) -0.008(3) -0.003(2) -0.013(3) C22 0.049(4) 0.072(4) 0.034(3) -0.012(3) -0.005(3) -0.006(3) C23 0.055(4) 0.090(5) 0.041(4) -0.013(4) 0.003(3) 0.001(4) C24 0.049(4) 0.131(8) 0.047(4) 0.000(5) 0.009(3) -0.015(5) C25 0.041(4) 0.101(6) 0.054(4) 0.008(4) 0.002(3) -0.033(4) C26 0.038(3) 0.070(4) 0.041(3) 0.000(3) -0.006(3) -0.023(3) C31 0.035(3) 0.047(3) 0.047(3) -0.014(3) -0.006(3) -0.011(2) C32 0.045(4) 0.087(5) 0.063(5) -0.010(4) 0.001(3) -0.023(4) C33 0.037(4) 0.115(7) 0.128(9) -0.014(6) -0.006(5) -0.032(4) C34 0.053(5) 0.126(8) 0.112(8) -0.035(6) -0.035(5) -0.024(5) C35 0.061(5) 0.142(8) 0.064(5) -0.040(5) -0.023(4) -0.015(5) C36 0.060(4) 0.105(6) 0.045(4) -0.022(4) -0.012(3) -0.026(4) C41 0.047(3) 0.040(3) 0.053(4) -0.009(3) -0.011(3) -0.007(3) C42 0.060(4) 0.061(4) 0.069(5) -0.015(3) -0.006(4) -0.027(3) C43 0.096(6) 0.058(4) 0.112(7) -0.018(5) -0.023(6) -0.036(4) C44 0.101(7) 0.065(5) 0.100(7) -0.042(5) -0.024(6) -0.013(5) C45 0.099(6) 0.075(5) 0.070(5) -0.039(4) -0.021(5) 0.006(5) C46 0.071(5) 0.061(4) 0.048(4) -0.016(3) -0.011(3) -0.008(3) C51 0.060(4) 0.038(3) 0.033(3) -0.007(2) -0.003(3) -0.016(3) C52 0.054(4) 0.060(4) 0.038(3) -0.007(3) -0.004(3) -0.023(3) C53 0.059(4) 0.069(4) 0.053(4) -0.018(3) 0.007(3) -0.026(3) C54 0.084(6) 0.070(4) 0.046(4) -0.011(3) 0.013(4) -0.026(4) C55 0.094(6) 0.074(5) 0.040(4) 0.001(3) -0.006(4) -0.012(4) C56 0.068(4) 0.065(4) 0.039(3) -0.005(3) -0.009(3) -0.008(3) C61 0.045(3) 0.056(4) 0.044(3) -0.004(3) -0.010(3) -0.017(3) C62 0.094(6) 0.058(4) 0.094(6) -0.006(4) -0.054(5) -0.025(4) C63 0.123(8) 0.089(6) 0.111(8) -0.001(5) -0.069(7) -0.054(6) C64 0.078(6) 0.123(8) 0.073(6) -0.010(5) -0.035(5) -0.041(6) C65 0.064(5) 0.106(6) 0.084(6) -0.033(5) -0.032(4) -0.004(5) C66 0.061(4) 0.079(5) 0.070(5) -0.028(4) -0.017(4) -0.018(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 Re1 C3 1.907(6) . ? Re1 C1 1.914(6) . ? Re1 C2 1.947(6) . ? Re1 S1 2.4891(16) . ? Re1 P1 2.4946(14) . ? Re1 Re2 3.1783(4) . ? Re2 C4 1.899(6) . ? Re2 C6 1.923(7) . ? Re2 C5 1.934(6) . ? Re2 P2 2.4897(15) . ? Re2 S1 2.4929(16) . ? P1 C21 1.825(6) . ? P1 C11 1.830(5) . ? P1 C31 1.835(6) . ? P2 C41 1.817(6) . ? P2 C61 1.835(6) . ? P2 C51 1.837(6) . ? O1 C1 1.153(7) . ? O2 C2 1.131(7) . ? O3 C3 1.154(7) . ? O4 C4 1.168(7) . ? O5 C5 1.145(7) . ? O6 C6 1.156(8) . ? C11 C16 1.357(8) . ? C11 C12 1.400(8) . ? C12 C13 1.366(8) . ? C13 C14 1.378(10) . ? C14 C15 1.367(9) . ? C15 C16 1.387(8) . ? C21 C26 1.376(8) . ? C21 C22 1.407(8) . ? C22 C23 1.378(9) . ? C23 C24 1.379(12) . ? C24 C25 1.360(11) . ? C25 C26 1.392(8) . ? C31 C36 1.390(9) . ? C31 C32 1.393(8) . ? C32 C33 1.409(11) . ? C33 C34 1.370(12) . ? C34 C35 1.346(11) . ? C35 C36 1.383(10) . ? C41 C42 1.368(8) . ? C41 C46 1.407(9) . ? C42 C43 1.397(9) . ? C43 C44 1.352(12) . ? C44 C45 1.370(12) . ? C45 C46 1.369(9) . ? C51 C52 1.374(8) . ? C51 C56 1.399(8) . ? C52 C53 1.363(8) . ? C53 C54 1.389(10) . ? C54 C55 1.365(11) . ? C55 C56 1.377(9) . ? C61 C62 1.378(9) . ? C61 C66 1.388(9) . ? C62 C63 1.395(10) . ? C63 C64 1.375(12) . ? C64 C65 1.346(11) . ? C65 C66 1.394(10) . ? 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 C3 Re1 C1 91.6(3) . . ? C3 Re1 C2 87.3(2) . . ? C1 Re1 C2 89.1(3) . . ? C3 Re1 S1 101.80(19) . . ? C1 Re1 S1 166.45(19) . . ? C2 Re1 S1 89.3(2) . . ? C3 Re1 P1 85.23(18) . . ? C1 Re1 P1 88.71(18) . . ? C2 Re1 P1 172.14(18) . . ? S1 Re1 P1 94.48(5) . . ? C3 Re1 Re2 152.12(19) . . ? C1 Re1 Re2 116.28(18) . . ? C2 Re1 Re2 93.85(18) . . ? S1 Re1 Re2 50.41(4) . . ? P1 Re1 Re2 93.87(3) . . ? C4 Re2 C6 97.6(3) . . ? C4 Re2 C5 85.2(3) . . ? C6 Re2 C5 84.7(3) . . ? C4 Re2 P2 85.81(18) . . ? C6 Re2 P2 85.7(2) . . ? C5 Re2 P2 165.78(18) . . ? C4 Re2 S1 164.6(2) . . ? C6 Re2 S1 97.6(2) . . ? C5 Re2 S1 94.18(19) . . ? P2 Re2 S1 97.42(5) . . ? C4 Re2 Re1 114.4(2) . . ? C6 Re2 Re1 147.7(2) . . ? C5 Re2 Re1 93.09(18) . . ? P2 Re2 Re1 100.63(4) . . ? S1 Re2 Re1 50.31(4) . . ? Re1 S1 Re2 79.28(4) . . ? C21 P1 C11 105.8(3) . . ? C21 P1 C31 101.4(3) . . ? C11 P1 C31 100.9(2) . . ? C21 P1 Re1 116.43(19) . . ? C11 P1 Re1 116.79(18) . . ? C31 P1 Re1 113.36(19) . . ? C41 P2 C61 102.3(3) . . ? C41 P2 C51 105.1(3) . . ? C61 P2 C51 101.2(3) . . ? C41 P2 Re2 118.9(2) . . ? C61 P2 Re2 111.8(2) . . ? C51 P2 Re2 115.28(18) . . ? O1 C1 Re1 177.4(6) . . ? O2 C2 Re1 172.9(6) . . ? O3 C3 Re1 177.6(6) . . ? O4 C4 Re2 176.2(6) . . ? O5 C5 Re2 167.5(5) . . ? O6 C6 Re2 176.8(6) . . ? C16 C11 C12 118.2(5) . . ? C16 C11 P1 121.3(4) . . ? C12 C11 P1 120.5(4) . . ? C13 C12 C11 120.4(6) . . ? C12 C13 C14 120.5(6) . . ? C15 C14 C13 119.7(6) . . ? C14 C15 C16 119.5(6) . . ? C11 C16 C15 121.7(6) . . ? C26 C21 C22 118.8(6) . . ? C26 C21 P1 123.8(5) . . ? C22 C21 P1 117.4(5) . . ? C23 C22 C21 120.4(7) . . ? C22 C23 C24 119.5(7) . . ? C25 C24 C23 120.9(7) . . ? C24 C25 C26 120.2(7) . . ? C21 C26 C25 120.3(7) . . ? C36 C31 C32 118.7(6) . . ? C36 C31 P1 122.8(5) . . ? C32 C31 P1 118.4(5) . . ? C31 C32 C33 118.7(7) . . ? C34 C33 C32 120.2(7) . . ? C35 C34 C33 121.6(8) . . ? C34 C35 C36 119.2(8) . . ? C35 C36 C31 121.6(7) . . ? C42 C41 C46 119.3(6) . . ? C42 C41 P2 123.3(5) . . ? C46 C41 P2 117.4(5) . . ? C41 C42 C43 119.1(7) . . ? C44 C43 C42 121.6(8) . . ? C43 C44 C45 119.4(7) . . ? C46 C45 C44 120.9(8) . . ? C45 C46 C41 119.7(7) . . ? C52 C51 C56 118.6(6) . . ? C52 C51 P2 120.3(4) . . ? C56 C51 P2 121.2(5) . . ? C53 C52 C51 120.8(6) . . ? C52 C53 C54 121.0(7) . . ? C55 C54 C53 118.5(7) . . ? C54 C55 C56 121.2(7) . . ? C55 C56 C51 119.9(7) . . ? C62 C61 C66 117.9(6) . . ? C62 C61 P2 120.6(5) . . ? C66 C61 P2 121.5(5) . . ? C61 C62 C63 121.0(7) . . ? C64 C63 C62 119.4(8) . . ? C65 C64 C63 120.8(8) . . ? C64 C65 C66 120.0(8) . . ? C61 C66 C65 120.9(7) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.002 _refine_diff_density_min -0.794 _refine_diff_density_rms 0.125 # END of CIF data_3c _database_code_CSD 139434 _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-hydrido-\m-naphthylthiolato-ax-pyridine-heptacarbonyl- dirhenium ; _chemical_formula_moiety 'C22 H13 N O7 Re2 S' _chemical_formula_sum 'C22 H13 N O7 Re2 S' _chemical_formula_weight 806.79 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' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 15.464(5) _cell_length_b 15.262(4) _cell_length_c 20.333(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4799(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 15.071 _cell_measurement_theta_max 33.004 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.233 _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 10.209 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_T_max 0.782 _diffrn_ambient_temperature 298(2) _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 397 _diffrn_standards_decay_% <1 _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_number 6828 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.1007 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5936 _reflns_number_gt 3548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS (Bruker, 1996)' _computing_cell_refinement 'Bruker XSCANS (Bruker, 1996)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0551P)^2^] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00031(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 5936 _refine_ls_number_parameters 594 _refine_ls_number_restraints 705 _refine_ls_R_factor_all 0.1289 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1277 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 0.988 _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 -0.27384(7) 0.49926(6) 0.62859(4) 0.0471(3) Uani 1 1 d U . . Re2 Re -0.14842(8) 0.64725(6) 0.58447(6) 0.0556(3) Uani 1 1 d U . . S1 S -0.1323(4) 0.4874(4) 0.5723(3) 0.0493(15) Uani 1 1 d U . . O1 O -0.3815(16) 0.5164(15) 0.5037(10) 0.090(7) Uani 1 1 d U . . C1 C -0.3388(14) 0.5084(15) 0.5521(13) 0.046(6) Uani 1 1 d U . . O2 O -0.3252(14) 0.3057(11) 0.6311(9) 0.081(6) Uani 1 1 d U . . C2 C -0.3075(17) 0.3825(14) 0.6301(10) 0.052(6) Uani 1 1 d U . . O3 O -0.4324(15) 0.5440(15) 0.7097(11) 0.103(8) Uani 1 1 d U . . C3 C -0.3735(18) 0.5265(19) 0.6806(13) 0.063(8) Uani 1 1 d U . . O4 O -0.0386(16) 0.6345(18) 0.7147(11) 0.114(9) Uani 1 1 d U . . C4 C -0.0795(17) 0.638(2) 0.6676(16) 0.075(9) Uani 1 1 d U . . O5 O -0.2534(14) 0.6663(14) 0.4558(11) 0.086(7) Uani 1 1 d U . . C5 C -0.2176(18) 0.6569(18) 0.5014(17) 0.065(8) Uani 1 1 d U . . O6 O -0.1900(16) 0.8384(12) 0.6179(12) 0.114(8) Uani 1 1 d U . . C6 C -0.175(2) 0.7655(15) 0.6049(14) 0.089(10) Uani 1 1 d U . . O7 O 0.0181(16) 0.6933(13) 0.5074(10) 0.094(8) Uani 1 1 d U . . C7 C -0.045(3) 0.6756(18) 0.5364(17) 0.089(10) Uani 1 1 d U . . N1 N -0.1964(12) 0.4757(14) 0.7216(9) 0.051(5) Uani 1 1 d DU . . C8 C -0.1464(13) 0.4074(13) 0.7292(12) 0.050(6) Uani 1 1 d DU . . H8 H -0.1379 0.3695 0.6940 0.060 Uiso 1 1 calc R . . C9 C -0.1074(16) 0.3908(19) 0.7861(14) 0.074(7) Uani 1 1 d DU . . H9 H -0.0702 0.3432 0.7895 0.088 Uiso 1 1 calc R . . C10 C -0.1214(17) 0.442(2) 0.8390(16) 0.082(8) Uani 1 1 d DU . . H10 H -0.0978 0.4267 0.8794 0.098 Uiso 1 1 calc R . . C11 C -0.1698(19) 0.518(2) 0.8345(13) 0.084(8) Uani 1 1 d DU . . H11 H -0.1765 0.5561 0.8697 0.100 Uiso 1 1 calc R . . C12 C -0.2078(16) 0.5325(18) 0.7736(13) 0.061(7) Uani 1 1 d DU . . H12 H -0.2419 0.5821 0.7677 0.073 Uiso 1 1 calc R . . C21 C -0.1498(13) 0.4504(12) 0.4906(10) 0.041(5) Uani 1 1 d DU . . C22 C -0.1934(12) 0.3764(12) 0.4779(10) 0.045(6) Uani 1 1 d DU . . H22 H -0.2247 0.3495 0.5113 0.055 Uiso 1 1 calc R . . C23 C -0.1924(11) 0.3394(12) 0.4156(10) 0.042(5) Uani 1 1 d DU . . C24 C -0.2406(15) 0.2567(15) 0.4018(10) 0.053(6) Uani 1 1 d DU . . H24 H -0.2718 0.2306 0.4356 0.064 Uiso 1 1 calc R . . C25 C -0.2405(16) 0.2204(13) 0.3449(13) 0.060(6) Uani 1 1 d DU . . H25 H -0.2711 0.1686 0.3386 0.072 Uiso 1 1 calc R . . C26 C -0.1966(16) 0.2561(17) 0.2934(13) 0.066(7) Uani 1 1 d DU . . H26 H -0.1976 0.2294 0.2523 0.080 Uiso 1 1 calc R . . C27 C -0.1491(16) 0.3348(16) 0.3033(11) 0.055(6) Uani 1 1 d DU . . H27 H -0.1186 0.3597 0.2686 0.066 Uiso 1 1 calc R . . C28 C -0.1482(14) 0.3732(14) 0.3631(10) 0.042(5) Uani 1 1 d DU . . C29 C -0.1014(15) 0.4508(15) 0.3773(11) 0.055(6) Uani 1 1 d DU . . H29 H -0.0694 0.4772 0.3441 0.066 Uiso 1 1 calc R . . C30 C -0.1018(15) 0.4875(15) 0.4379(12) 0.052(6) Uani 1 1 d DU . . H30 H -0.0700 0.5383 0.4453 0.062 Uiso 1 1 calc R . . Re3 Re 0.09470(7) 0.12643(6) 0.34862(6) 0.0495(3) Uani 1 1 d U . . Re4 Re -0.04158(7) -0.01002(6) 0.39437(4) 0.0455(3) Uani 1 1 d U . . S2 S 0.0986(4) -0.0357(4) 0.3395(4) 0.0566(16) Uani 1 1 d U . . O31 O -0.0026(14) 0.1512(14) 0.2155(11) 0.087(6) Uani 1 1 d U . . C31 C 0.0279(17) 0.1397(18) 0.2650(15) 0.061(7) Uani 1 1 d U . . O32 O 0.2060(14) 0.1201(14) 0.4765(10) 0.092(7) Uani 1 1 d U . . C32 C 0.1641(15) 0.1187(19) 0.4310(15) 0.063(8) Uani 1 1 d U . . O33 O 0.2579(14) 0.1838(18) 0.2749(13) 0.121(9) Uani 1 1 d U . . C33 C 0.196(2) 0.153(2) 0.304(2) 0.120(15) Uani 1 1 d U . . O34 O 0.0532(14) 0.3183(13) 0.3854(12) 0.101(7) Uani 1 1 d U . . C34 C 0.0693(16) 0.2467(14) 0.3711(12) 0.056(7) Uani 1 1 d U . . O35 O -0.1122(15) -0.1976(13) 0.4048(12) 0.099(8) Uani 1 1 d U . . C35 C -0.082(2) -0.132(2) 0.4017(13) 0.073(9) Uani 1 1 d U . . O36 O -0.1971(13) 0.0554(14) 0.4707(13) 0.100(8) Uani 1 1 d U . . C36 C -0.136(2) 0.0312(16) 0.4433(15) 0.064(8) Uani 1 1 d U . . O37 O -0.1467(12) 0.0158(14) 0.2702(11) 0.084(7) Uani 1 1 d U . . C37 C -0.1076(14) 0.0038(17) 0.3155(16) 0.056(7) Uani 1 1 d U . . N2 N 0.0351(11) -0.0348(11) 0.4851(9) 0.042(5) Uani 1 1 d DU . . C38 C 0.0352(13) 0.0204(18) 0.5340(14) 0.079(8) Uani 1 1 d DU . . H38 H 0.0063 0.0734 0.5289 0.095 Uiso 1 1 calc R . . C39 C 0.0773(18) 0.0036(19) 0.5941(15) 0.099(9) Uani 1 1 d DU . . H39 H 0.0777 0.0449 0.6277 0.119 Uiso 1 1 calc R . . C40 C 0.1182(18) -0.077(2) 0.6014(13) 0.076(8) Uani 1 1 d DU . . H40 H 0.1440 -0.0941 0.6407 0.092 Uiso 1 1 calc R . . C41 C 0.1181(16) -0.1275(16) 0.5498(13) 0.057(6) Uani 1 1 d DU . . H41 H 0.1470 -0.1808 0.5532 0.068 Uiso 1 1 calc R . . C42 C 0.0793(14) -0.1090(15) 0.4913(13) 0.051(6) Uani 1 1 d DU . . H42 H 0.0837 -0.1478 0.4562 0.062 Uiso 1 1 calc R . . C51 C 0.0841(16) -0.0836(14) 0.2591(11) 0.047(6) Uani 1 1 d DU . . C52 C 0.0254(15) -0.1389(12) 0.2426(12) 0.055(6) Uani 1 1 d DU . . H52 H -0.0183 -0.1513 0.2726 0.066 Uiso 1 1 calc R . . C53 C 0.0239(16) -0.1815(13) 0.1814(11) 0.057(6) Uani 1 1 d DU . . C54 C -0.040(2) -0.2341(18) 0.1666(15) 0.086(8) Uani 1 1 d DU . . H54 H -0.0862 -0.2431 0.1951 0.103 Uiso 1 1 calc R . . C55 C -0.035(2) -0.2773(18) 0.1036(16) 0.089(9) Uani 1 1 d DU . . H55 H -0.0753 -0.3203 0.0937 0.106 Uiso 1 1 calc R . . C56 C 0.0240(18) -0.2591(17) 0.0600(15) 0.072(8) Uani 1 1 d DU . . H56 H 0.0207 -0.2827 0.0179 0.087 Uiso 1 1 calc R . . C57 C 0.0896(16) -0.2055(16) 0.0764(12) 0.061(6) Uani 1 1 d DU . . H57 H 0.1353 -0.1970 0.0474 0.073 Uiso 1 1 calc R . . C58 C 0.0890(15) -0.1628(14) 0.1370(12) 0.049(5) Uani 1 1 d DU . . C59 C 0.1505(17) -0.1077(18) 0.1532(13) 0.069(7) Uani 1 1 d DU . . H59 H 0.1952 -0.0967 0.1237 0.082 Uiso 1 1 calc R . . C60 C 0.1501(18) -0.066(2) 0.2130(15) 0.080(8) Uani 1 1 d DU . . H60 H 0.1934 -0.0259 0.2231 0.096 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 Re1 0.0531(6) 0.0458(5) 0.0425(6) -0.0071(5) -0.0014(5) -0.0018(5) Re2 0.0724(8) 0.0384(5) 0.0559(6) -0.0018(5) -0.0151(6) -0.0061(5) S1 0.056(4) 0.047(3) 0.045(3) 0.003(3) 0.003(3) 0.008(3) O1 0.109(17) 0.105(16) 0.057(12) 0.010(12) -0.023(13) 0.009(14) C1 0.018 0.051(13) 0.070(16) -0.015(12) 0.022(11) 0.005(11) O2 0.133(16) 0.048(11) 0.062(11) -0.004(9) -0.001(12) -0.034(11) C2 0.093(19) 0.039(12) 0.024(11) -0.016(11) 0.007(13) 0.013(13) O3 0.115(18) 0.119(17) 0.075(14) 0.000(13) 0.041(14) 0.046(15) C3 0.062(17) 0.074(18) 0.052(16) -0.006(14) 0.043(14) 0.009(15) O4 0.105(19) 0.17(2) 0.065(14) -0.010(15) -0.040(14) -0.041(17) C4 0.035(16) 0.11(2) 0.08(2) 0.014(18) 0.002(15) -0.034(16) O5 0.075(15) 0.103(16) 0.079(14) 0.013(13) -0.029(13) -0.020(12) C5 0.041(17) 0.063(17) 0.09(2) -0.022(16) 0.018(16) 0.001(14) O6 0.16(2) 0.051(12) 0.135(19) -0.034(13) -0.024(17) 0.026(13) C6 0.15(3) 0.021(12) 0.10(2) -0.012(13) -0.03(2) 0.006(15) O7 0.113(19) 0.082(15) 0.086(15) 0.034(12) -0.021(14) -0.051(13) C7 0.14(3) 0.042(16) 0.08(2) 0.016(15) -0.01(2) -0.031(19) N1 0.038(11) 0.072(13) 0.044(11) -0.003(10) -0.003(10) -0.009(10) C8 0.049(14) 0.034(11) 0.066(15) -0.002(11) 0.000(12) 0.003(11) C9 0.075(17) 0.085(18) 0.060(15) 0.024(14) 0.003(15) 0.002(15) C10 0.065(17) 0.12(2) 0.057(15) 0.006(18) -0.004(15) -0.035(16) C11 0.079(18) 0.13(2) 0.040(13) -0.008(16) 0.010(14) -0.042(16) C12 0.050(14) 0.075(15) 0.058(14) -0.029(13) 0.012(12) -0.040(12) C21 0.066(15) 0.023(10) 0.033(11) -0.003(9) -0.003(11) 0.012(10) C22 0.076(16) 0.021(10) 0.040(11) 0.015(9) 0.018(11) -0.005(10) C23 0.052(13) 0.031(11) 0.044(11) -0.008(9) 0.020(10) -0.003(10) C24 0.071(15) 0.056(13) 0.033(11) -0.003(10) 0.021(12) -0.020(12) C25 0.090(16) 0.039(11) 0.052(13) 0.002(12) 0.004(15) -0.016(12) C26 0.069(17) 0.074(16) 0.055(14) -0.017(13) -0.017(13) -0.014(14) C27 0.063(15) 0.067(15) 0.036(12) 0.007(11) 0.015(12) 0.004(13) C28 0.041(12) 0.039(11) 0.046(12) -0.001(9) 0.019(10) -0.006(10) C29 0.064(15) 0.066(14) 0.035(11) 0.021(11) 0.013(11) -0.017(12) C30 0.054(14) 0.051(13) 0.050(12) 0.024(11) 0.009(12) -0.004(12) Re3 0.0484(6) 0.0453(5) 0.0547(6) 0.0035(6) -0.0055(6) 0.0004(5) Re4 0.0455(5) 0.0444(6) 0.0467(6) 0.0040(5) -0.0023(5) 0.0052(5) S2 0.055(4) 0.059(4) 0.055(4) -0.002(4) -0.005(4) 0.023(3) O31 0.084(15) 0.097(15) 0.079(14) 0.015(12) -0.033(13) -0.014(12) C31 0.041(16) 0.077(18) 0.066(18) 0.008(15) -0.004(14) -0.007(14) O32 0.085(16) 0.119(17) 0.072(13) 0.019(13) -0.042(12) -0.004(14) C32 0.018 0.091(19) 0.081(19) -0.022(17) -0.013(13) -0.011(14) O33 0.049(14) 0.18(3) 0.13(2) 0.017(19) -0.027(15) -0.020(16) C33 0.09(2) 0.08(2) 0.19(4) -0.09(2) -0.06(3) 0.02(2) O34 0.108(16) 0.063(13) 0.132(18) -0.012(14) -0.024(15) 0.003(12) C34 0.067(18) 0.022(11) 0.078(19) 0.008(11) -0.023(13) 0.000(11) O35 0.112(18) 0.060(13) 0.124(18) 0.013(13) -0.012(15) -0.038(12) C35 0.08(2) 0.10(2) 0.042(15) -0.013(17) 0.016(15) 0.024(19) O36 0.052(13) 0.092(16) 0.16(2) 0.014(15) 0.052(14) 0.018(12) C36 0.07(2) 0.043(15) 0.08(2) 0.022(14) -0.026(17) 0.007(14) O37 0.055(13) 0.107(16) 0.091(15) 0.037(13) -0.027(12) 0.000(12) C37 0.011(11) 0.068(16) 0.09(2) 0.025(15) 0.000(13) 0.001(12) N2 0.047(12) 0.035(9) 0.046(10) -0.003(8) -0.012(9) 0.009(9) C38 0.047(15) 0.113(19) 0.079(16) -0.024(15) 0.002(14) 0.055(14) C39 0.11(2) 0.13(2) 0.062(16) 0.000(16) -0.003(16) 0.066(17) C40 0.081(17) 0.098(18) 0.050(15) 0.024(14) 0.000(13) 0.031(15) C41 0.062(15) 0.052(14) 0.056(14) -0.004(12) -0.001(13) 0.006(12) C42 0.040(13) 0.051(13) 0.063(14) -0.011(12) -0.007(12) 0.005(11) C51 0.052(14) 0.051(13) 0.039(12) 0.003(11) -0.003(11) 0.015(12) C52 0.068(16) 0.038(12) 0.059(13) 0.008(11) 0.001(13) -0.020(12) C53 0.073(15) 0.051(13) 0.047(12) -0.006(11) -0.001(12) -0.005(12) C54 0.11(2) 0.074(17) 0.076(16) -0.013(15) -0.001(16) -0.054(16) C55 0.10(2) 0.060(15) 0.11(2) -0.013(15) 0.003(17) -0.021(15) C56 0.067(17) 0.067(16) 0.083(17) -0.006(14) 0.017(15) 0.001(14) C57 0.058(15) 0.075(15) 0.050(13) 0.000(13) -0.002(14) 0.007(13) C58 0.045(12) 0.044(12) 0.057(13) -0.013(11) -0.007(12) -0.003(10) C59 0.049(15) 0.096(18) 0.060(15) 0.007(14) 0.015(13) 0.012(14) C60 0.060(16) 0.110(19) 0.069(16) -0.008(16) 0.002(14) 0.033(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 Re1 C1 1.86(3) . ? Re1 C2 1.86(2) . ? Re1 C3 1.91(2) . ? Re1 N1 2.27(2) . ? Re1 S1 2.477(7) . ? Re1 Re2 3.1093(15) . ? Re2 C6 1.90(2) . ? Re2 C7 1.92(4) . ? Re2 C5 2.00(4) . ? Re2 C4 2.00(3) . ? Re2 S1 2.465(6) . ? S1 C21 1.77(2) . ? O1 C1 1.19(3) . ? O2 C2 1.20(3) . ? O3 C3 1.12(3) . ? O4 C4 1.15(3) . ? O5 C5 1.09(3) . ? O6 C6 1.17(3) . ? O7 C7 1.18(4) . ? N1 C8 1.31(3) . ? N1 C12 1.38(3) . ? C8 C9 1.33(3) . ? C9 C10 1.35(4) . ? C10 C11 1.37(4) . ? C11 C12 1.39(4) . ? C21 C22 1.34(3) . ? C21 C30 1.42(3) . ? C22 C23 1.39(3) . ? C23 C28 1.37(3) . ? C23 C24 1.49(3) . ? C24 C25 1.28(3) . ? C25 C26 1.36(3) . ? C26 C27 1.42(3) . ? C27 C28 1.35(3) . ? C28 C29 1.42(3) . ? C29 C30 1.35(3) . ? Re3 C33 1.85(5) . ? Re3 C34 1.93(2) . ? Re3 C32 1.99(3) . ? Re3 C31 2.00(3) . ? Re3 S2 2.482(6) . ? Re3 Re4 3.1054(15) . ? Re4 C36 1.88(3) . ? Re4 C37 1.91(3) . ? Re4 C35 1.97(4) . ? Re4 N2 2.225(17) . ? Re4 S2 2.469(7) . ? S2 C51 1.80(2) . ? O31 C31 1.13(3) . ? O32 C32 1.13(3) . ? O33 C33 1.22(5) . ? O34 C34 1.16(3) . ? O35 C35 1.11(3) . ? O36 C36 1.16(3) . ? O37 C37 1.12(3) . ? N2 C38 1.30(3) . ? N2 C42 1.33(3) . ? C38 C39 1.41(4) . ? C39 C40 1.39(3) . ? C40 C41 1.30(3) . ? C41 C42 1.36(3) . ? C51 C52 1.29(3) . ? C51 C60 1.41(4) . ? C52 C53 1.40(3) . ? C53 C54 1.31(3) . ? C53 C58 1.38(3) . ? C54 C55 1.44(4) . ? C55 C56 1.30(4) . ? C56 C57 1.34(3) . ? C57 C58 1.39(3) . ? C58 C59 1.31(3) . ? C59 C60 1.37(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 C2 86.2(10) . . ? C1 Re1 C3 90.6(11) . . ? C2 Re1 C3 88.5(11) . . ? C1 Re1 N1 175.1(9) . . ? C2 Re1 N1 89.0(9) . . ? C3 Re1 N1 89.9(10) . . ? C1 Re1 S1 95.5(6) . . ? C2 Re1 S1 100.7(7) . . ? C3 Re1 S1 169.3(9) . . ? N1 Re1 S1 84.7(5) . . ? C1 Re1 Re2 92.4(7) . . ? C2 Re1 Re2 151.3(7) . . ? C3 Re1 Re2 120.3(9) . . ? N1 Re1 Re2 91.5(5) . . ? S1 Re1 Re2 50.83(13) . . ? C6 Re2 C7 94.2(14) . . ? C6 Re2 C5 90.1(12) . . ? C7 Re2 C5 89.9(13) . . ? C6 Re2 C4 89.6(13) . . ? C7 Re2 C4 90.2(13) . . ? C5 Re2 C4 179.6(13) . . ? C6 Re2 S1 170.4(10) . . ? C7 Re2 S1 95.0(9) . . ? C5 Re2 S1 92.4(8) . . ? C4 Re2 S1 88.0(9) . . ? C6 Re2 Re1 119.7(10) . . ? C7 Re2 Re1 146.0(9) . . ? C5 Re2 Re1 87.9(8) . . ? C4 Re2 Re1 92.3(7) . . ? S1 Re2 Re1 51.18(15) . . ? C21 S1 Re2 113.2(6) . . ? C21 S1 Re1 108.7(8) . . ? Re2 S1 Re1 77.99(18) . . ? O1 C1 Re1 178(2) . . ? O2 C2 Re1 177(2) . . ? O3 C3 Re1 178(3) . . ? O4 C4 Re2 179(3) . . ? O5 C5 Re2 176(3) . . ? O6 C6 Re2 179(3) . . ? O7 C7 Re2 179(3) . . ? C8 N1 C12 119(2) . . ? C8 N1 Re1 122.5(17) . . ? C12 N1 Re1 118.2(18) . . ? N1 C8 C9 122(3) . . ? C8 C9 C10 121(3) . . ? C9 C10 C11 121(3) . . ? C10 C11 C12 115(3) . . ? N1 C12 C11 122(3) . . ? C22 C21 C30 117(2) . . ? C22 C21 S1 121.7(17) . . ? C30 C21 S1 119.9(17) . . ? C21 C22 C23 121(2) . . ? C28 C23 C22 124(2) . . ? C28 C23 C24 114.9(19) . . ? C22 C23 C24 120.8(19) . . ? C25 C24 C23 122(2) . . ? C24 C25 C26 121(2) . . ? C25 C26 C27 119(2) . . ? C28 C27 C26 120(2) . . ? C27 C28 C23 122(2) . . ? C27 C28 C29 124(2) . . ? C23 C28 C29 114(2) . . ? C30 C29 C28 122(2) . . ? C29 C30 C21 122(2) . . ? C33 Re3 C34 94.7(12) . . ? C33 Re3 C32 88.4(15) . . ? C34 Re3 C32 88.1(11) . . ? C33 Re3 C31 89.7(14) . . ? C34 Re3 C31 90.0(10) . . ? C32 Re3 C31 177.2(12) . . ? C33 Re3 S2 99.1(9) . . ? C34 Re3 S2 165.9(8) . . ? C32 Re3 S2 89.5(8) . . ? C31 Re3 S2 92.8(8) . . ? C33 Re3 Re4 149.9(9) . . ? C34 Re3 Re4 115.4(7) . . ? C32 Re3 Re4 94.2(8) . . ? C31 Re3 Re4 88.4(8) . . ? S2 Re3 Re4 50.97(17) . . ? C36 Re4 C37 89.5(11) . . ? C36 Re4 C35 91.9(11) . . ? C37 Re4 C35 90.0(11) . . ? C36 Re4 N2 91.9(9) . . ? C37 Re4 N2 176.5(9) . . ? C35 Re4 N2 86.8(10) . . ? C36 Re4 S2 167.5(8) . . ? C37 Re4 S2 96.1(7) . . ? C35 Re4 S2 99.1(8) . . ? N2 Re4 S2 83.1(5) . . ? C36 Re4 Re3 117.5(8) . . ? C37 Re4 Re3 92.1(7) . . ? C35 Re4 Re3 150.5(8) . . ? N2 Re4 Re3 90.0(4) . . ? S2 Re4 Re3 51.34(15) . . ? C51 S2 Re4 111.4(8) . . ? C51 S2 Re3 117.9(7) . . ? Re4 S2 Re3 77.69(18) . . ? O31 C31 Re3 173(2) . . ? O32 C32 Re3 175(3) . . ? O33 C33 Re3 170(3) . . ? O34 C34 Re3 179(3) . . ? O35 C35 Re4 173(3) . . ? O36 C36 Re4 176(3) . . ? O37 C37 Re4 177(3) . . ? C38 N2 C42 119(2) . . ? C38 N2 Re4 121.6(16) . . ? C42 N2 Re4 119.9(15) . . ? N2 C38 C39 123(2) . . ? C40 C39 C38 118(3) . . ? C41 C40 C39 116(3) . . ? C40 C41 C42 126(3) . . ? N2 C42 C41 119(2) . . ? C52 C51 C60 118(3) . . ? C52 C51 S2 126(2) . . ? C60 C51 S2 116(2) . . ? C51 C52 C53 123(2) . . ? C54 C53 C58 122(2) . . ? C54 C53 C52 120(3) . . ? C58 C53 C52 118(2) . . ? C53 C54 C55 116(3) . . ? C56 C55 C54 123(3) . . ? C55 C56 C57 119(3) . . ? C56 C57 C58 120(3) . . ? C59 C58 C53 120(2) . . ? C59 C58 C57 121(3) . . ? C53 C58 C57 119(2) . . ? C58 C59 C60 121(3) . . ? C59 C60 C51 120(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.982 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.239 #=END