# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1551 data_global _publ_requested_journal ' ChemComm' _publ_contact_author_name ; Michael A. Reynolds, Ilia A. Guzei and Robert J. Angelici ; _publ_contact_author_address ; Ames Laboratory and the Department of Chemistry Iowa State University, Ames, IA 50011, USA ; _publ_contact_author_email Angelici@iastate.edu _publ_section_title ; Organometallic models of catalytic hydrodesulfurization: Re2(CO)10-promoted cleavage of C-S bonds in benzothiophene ; _publ_section_references ; All software and sources of the scattering factors are contained in the SHELXTL (version 5.10) program library (G. Sheldrick, Siemens XRD, Madison, WI). The absorption corrections were applied by using program DIFABS (Walker, N. and Stuart, D. in Acta Cryst. 1983, A39, 158) for 1 and SADABS (Blessing, R.H. Acta Cryst. 1995, A51, 33-38) for 2 and 3. ; data_ang02 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H6 O7 Re2 S' _chemical_formula_weight 702.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.167(1) _cell_length_b 12.544(1) _cell_length_c 16.019(2) _cell_angle_alpha 73.34(2) _cell_angle_beta 86.47(3) _cell_angle_gamma 71.06(2) _cell_volume 1668.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 15.0 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 14.659 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.729 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'DIFABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CAD4' _diffrn_measurement_method 'theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 5258 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 23.39 _reflns_number_total 4337 _reflns_number_gt 3571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4' _computing_cell_refinement 'CAD4' _computing_data_reduction 'XCAD4PC' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP' _computing_publication_material 'XCIF' _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^)+(0.0564P)^2^+4.5969P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4337 _refine_ls_number_parameters 451 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.003 _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 -1.18632(5) 0.32969(3) 0.50425(3) 0.02750(14) Uani 1 1 d . . . Re2 Re -0.95986(5) 0.25611(3) 0.64491(3) 0.02768(14) Uani 1 1 d . . . S1 S -0.9263(3) 0.3570(2) 0.49457(18) 0.0288(6) Uani 1 1 d . . . O1 O -1.3437(10) 0.5640(7) 0.3705(6) 0.056(2) Uani 1 1 d . . . O2 O -1.3228(9) 0.4721(7) 0.6355(6) 0.049(2) Uani 1 1 d . . . O3 O -1.1014(12) 0.2113(10) 0.3521(7) 0.073(3) Uani 1 1 d . . . O4 O -1.4780(10) 0.2575(8) 0.5347(6) 0.058(3) Uani 1 1 d . . . O5 O -0.9766(10) 0.4656(7) 0.7137(6) 0.050(2) Uani 1 1 d . . . O6 O -1.0607(11) 0.1300(8) 0.8186(6) 0.062(3) Uani 1 1 d . . . O7 O -0.6359(10) 0.1394(8) 0.7178(7) 0.070(3) Uani 1 1 d . . . C1 C -1.2852(12) 0.4786(10) 0.4210(8) 0.036(3) Uani 1 1 d . . . C2 C -1.2620(12) 0.4177(10) 0.5916(9) 0.037(3) Uani 1 1 d . . . C3 C -1.1357(14) 0.2547(11) 0.4081(8) 0.042(3) Uani 1 1 d . . . C4 C -1.3725(13) 0.2857(9) 0.5256(8) 0.041(3) Uani 1 1 d . . . C5 C -0.9715(12) 0.3880(10) 0.6890(7) 0.031(3) Uani 1 1 d . . . C6 C -1.0249(13) 0.1770(10) 0.7538(8) 0.039(3) Uani 1 1 d . . . C7 C -0.7555(13) 0.1843(11) 0.6899(8) 0.040(3) Uani 1 1 d . . . C8 C -1.0584(11) 0.1578(9) 0.5825(7) 0.030(2) Uani 1 1 d U . . H8A H -1.1186 0.1118 0.6196 0.036 Uiso 1 1 calc R . . C9 C -0.9049(12) 0.0996(9) 0.5767(7) 0.034(3) Uani 1 1 d U . . H9A H -0.8667 0.0201 0.6164 0.041 Uiso 1 1 calc R . . C10 C -0.8057(12) 0.1257(9) 0.5008(8) 0.036(3) Uani 1 1 d U . . C11 C -0.7081(14) 0.0333(10) 0.4720(9) 0.051(3) Uani 1 1 d . . . H11A H -0.7009 -0.0434 0.5028 0.062 Uiso 1 1 calc R . . C12 C -0.6223(15) 0.0529(11) 0.3996(9) 0.052(3) Uani 1 1 d . . . H12A H -0.5573 -0.0097 0.3812 0.063 Uiso 1 1 calc R . . C13 C -0.6340(13) 0.1651(13) 0.3552(8) 0.051(3) Uani 1 1 d . . . H13A H -0.5762 0.1789 0.3059 0.061 Uiso 1 1 calc R . . C14 C -0.7278(13) 0.2576(11) 0.3808(8) 0.042(3) Uani 1 1 d . . . H14A H -0.7353 0.3341 0.3491 0.050 Uiso 1 1 calc R . . C15 C -0.8108(11) 0.2373(9) 0.4536(8) 0.033(3) Uani 1 1 d . . . Re3 Re -2.52398(4) 0.67409(3) 0.11181(3) 0.02736(14) Uani 1 1 d . . . Re4 Re -2.73200(4) 0.75983(3) -0.03801(3) 0.02689(14) Uani 1 1 d . . . S2 S -2.4663(3) 0.6344(2) -0.03321(18) 0.0272(6) Uani 1 1 d . . . O1' O -2.3529(15) 0.4232(8) 0.2221(7) 0.091(4) Uani 1 1 d . . . O2' O -2.6243(10) 0.7706(7) 0.2688(6) 0.047(2) Uani 1 1 d . . . O3' O -2.7974(11) 0.5735(9) 0.1576(7) 0.068(3) Uani 1 1 d . . . O4' O -2.2189(12) 0.7337(11) 0.1115(8) 0.086(4) Uani 1 1 d . . . O5' O -2.8708(10) 0.5711(7) -0.0487(7) 0.062(3) Uani 1 1 d . . . O6' O -3.0576(9) 0.8997(7) 0.0000(6) 0.048(2) Uani 1 1 d . . . O7' O -2.7941(14) 0.8823(9) -0.2299(6) 0.077(3) Uani 1 1 d . . . C1' C -2.4109(15) 0.5153(11) 0.1803(8) 0.045(3) Uani 1 1 d . . . C2' C -2.5851(13) 0.7320(9) 0.2122(8) 0.036(3) Uani 1 1 d . . . C3' C -2.7078(13) 0.6177(10) 0.1317(8) 0.039(3) Uani 1 1 d . . . C4' C -2.3267(15) 0.7168(12) 0.1083(9) 0.052(3) Uani 1 1 d . . . C5' C -2.8166(12) 0.6376(9) -0.0426(8) 0.037(3) Uani 1 1 d . . . C6' C -2.9361(13) 0.8515(9) -0.0142(7) 0.035(3) Uani 1 1 d . . . C7' C -2.7711(13) 0.8317(10) -0.1579(10) 0.045(3) Uani 1 1 d . . . C8' C -2.6276(12) 0.8507(9) 0.0313(7) 0.032(2) Uani 1 1 d U . . H8'A H -2.6999 0.9050 0.0599 0.038 Uiso 1 1 calc R . . C9' C -2.5925(12) 0.8986(9) -0.0505(7) 0.032(2) Uani 1 1 d U . . H9'A H -2.6529 0.9812 -0.0759 0.038 Uiso 1 1 calc R . . C10' C -2.4489(12) 0.8563(9) -0.0950(7) 0.032(2) Uani 1 1 d U . . C11' C -2.3773(13) 0.9363(9) -0.1439(7) 0.038(3) Uani 1 1 d . . . H11B H -2.4270 1.0164 -0.1530 0.045 Uiso 1 1 calc R . . C12' C -2.2359(15) 0.8991(11) -0.1785(9) 0.054(4) Uani 1 1 d . . . H12B H -2.1908 0.9542 -0.2102 0.064 Uiso 1 1 calc R . . C13' C -2.1608(14) 0.7833(12) -0.1673(8) 0.047(3) Uani 1 1 d . . . H13B H -2.0645 0.7596 -0.1909 0.056 Uiso 1 1 calc R . . C14' C -2.2263(12) 0.7001(10) -0.1210(7) 0.036(3) Uani 1 1 d . . . H14B H -2.1750 0.6206 -0.1137 0.043 Uiso 1 1 calc R . . C15' C -2.3720(11) 0.7372(8) -0.0848(7) 0.027(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0313(2) 0.0274(2) 0.0212(3) -0.00455(19) -0.00334(18) -0.00723(18) Re2 0.0320(2) 0.0299(2) 0.0177(3) -0.00361(19) -0.00235(18) -0.00750(18) S1 0.0335(13) 0.0250(13) 0.0256(16) -0.0062(12) 0.0017(11) -0.0071(11) O1 0.055(5) 0.040(5) 0.052(6) 0.010(5) -0.018(5) -0.005(4) O2 0.050(5) 0.050(5) 0.049(6) -0.022(5) 0.009(4) -0.015(4) O3 0.088(7) 0.096(8) 0.045(7) -0.038(6) -0.003(6) -0.026(6) O4 0.049(5) 0.074(6) 0.075(7) -0.037(6) 0.011(5) -0.036(5) O5 0.071(6) 0.050(5) 0.036(5) -0.017(5) 0.006(4) -0.026(5) O6 0.073(6) 0.065(6) 0.040(6) 0.002(5) 0.008(5) -0.027(5) O7 0.045(5) 0.073(6) 0.079(8) -0.015(6) -0.030(5) 0.000(5) C1 0.032(6) 0.033(6) 0.034(7) -0.010(6) -0.001(5) 0.003(5) C2 0.033(6) 0.030(6) 0.048(8) -0.013(6) -0.005(6) -0.006(5) C3 0.058(7) 0.056(8) 0.012(6) -0.009(6) -0.004(5) -0.018(6) C4 0.042(7) 0.030(6) 0.049(9) -0.015(6) 0.011(6) -0.010(5) C5 0.038(6) 0.042(7) 0.013(6) 0.000(5) 0.010(5) -0.021(5) C6 0.043(6) 0.048(7) 0.022(7) 0.001(6) -0.011(5) -0.015(6) C7 0.038(7) 0.055(7) 0.026(7) -0.013(6) -0.007(5) -0.008(6) C8 0.034(3) 0.031(3) 0.027(4) -0.006(3) -0.002(3) -0.013(3) C9 0.038(3) 0.034(3) 0.032(4) -0.010(3) -0.002(3) -0.011(3) C10 0.036(3) 0.036(4) 0.033(4) -0.011(3) 0.001(3) -0.009(3) C11 0.052(7) 0.034(7) 0.047(9) -0.005(6) -0.017(7) 0.010(6) C12 0.061(8) 0.045(8) 0.040(8) -0.021(7) -0.001(7) 0.006(6) C13 0.042(7) 0.082(10) 0.025(7) -0.027(7) 0.012(6) -0.005(7) C14 0.041(6) 0.051(7) 0.031(7) -0.010(6) 0.002(6) -0.012(6) C15 0.030(5) 0.031(6) 0.033(7) -0.008(5) -0.011(5) -0.005(5) Re3 0.0324(2) 0.0256(2) 0.0184(3) -0.00032(19) -0.00386(18) -0.00617(18) Re4 0.0292(2) 0.0224(2) 0.0253(3) -0.00393(19) -0.00728(18) -0.00413(18) S2 0.0330(13) 0.0207(12) 0.0238(15) -0.0034(11) -0.0002(11) -0.0055(11) O1' 0.152(11) 0.037(6) 0.042(7) 0.008(5) -0.025(7) 0.012(6) O2' 0.066(5) 0.051(5) 0.029(5) -0.017(4) 0.006(4) -0.021(4) O3' 0.069(6) 0.101(8) 0.060(7) -0.032(6) 0.028(5) -0.059(6) O4' 0.055(6) 0.136(10) 0.076(8) -0.016(7) 0.001(6) -0.056(7) O5' 0.048(5) 0.038(5) 0.100(8) -0.008(5) -0.033(5) -0.016(4) O6' 0.036(5) 0.046(5) 0.059(6) -0.021(5) 0.003(4) -0.002(4) O7' 0.129(9) 0.063(6) 0.032(6) 0.012(5) -0.032(6) -0.037(7) C1' 0.063(8) 0.037(7) 0.025(7) -0.010(6) 0.004(6) -0.001(6) C2' 0.048(7) 0.027(6) 0.028(7) 0.004(6) -0.001(6) -0.017(5) C3' 0.042(6) 0.043(7) 0.027(7) -0.012(6) 0.010(5) -0.008(6) C4' 0.043(7) 0.056(8) 0.057(10) -0.021(7) 0.005(7) -0.014(6) C5' 0.033(6) 0.018(5) 0.049(8) -0.003(5) -0.018(5) 0.004(5) C6' 0.036(7) 0.033(6) 0.029(7) -0.007(5) -0.013(5) -0.003(5) C7' 0.045(7) 0.028(6) 0.063(10) -0.014(7) -0.011(7) -0.009(5) C8' 0.035(3) 0.029(3) 0.032(4) -0.007(3) -0.004(3) -0.012(3) C9' 0.036(3) 0.028(3) 0.033(4) -0.010(3) -0.002(3) -0.010(3) C10' 0.035(3) 0.030(3) 0.030(4) -0.007(3) -0.004(3) -0.011(3) C11' 0.056(7) 0.028(6) 0.027(7) 0.007(5) -0.010(6) -0.022(5) C12' 0.054(8) 0.053(8) 0.052(9) 0.009(7) -0.020(7) -0.032(7) C13' 0.043(6) 0.068(9) 0.022(7) 0.007(6) -0.003(5) -0.025(7) C14' 0.038(6) 0.048(7) 0.018(6) -0.002(5) -0.004(5) -0.014(5) C15' 0.032(5) 0.029(5) 0.022(6) -0.001(5) -0.009(5) -0.013(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 C1 1.927(12) . ? Re1 C4 1.940(12) . ? Re1 C2 1.982(14) . ? Re1 C3 1.983(13) . ? Re1 C8 2.142(10) . ? Re1 S1 2.506(2) . ? Re1 Re2 2.8945(7) . ? Re2 C7 1.881(11) . ? Re2 C6 1.910(13) . ? Re2 C5 1.947(12) . ? Re2 C8 2.208(10) . ? Re2 C9 2.413(11) . ? Re2 S1 2.431(3) . ? S1 C15 1.805(11) . ? O1 C1 1.128(13) . ? O2 C2 1.119(13) . ? O3 C3 1.154(14) . ? O4 C4 1.122(13) . ? O5 C5 1.138(13) . ? O6 C6 1.124(14) . ? O7 C7 1.111(13) . ? C8 C9 1.370(14) . ? C9 C10 1.498(16) . ? C10 C15 1.374(15) . ? C10 C11 1.392(17) . ? C11 C12 1.369(18) . ? C12 C13 1.355(18) . ? C13 C14 1.356(17) . ? C14 C15 1.359(16) . ? Re3 C2' 1.929(14) . ? Re3 C1' 1.947(12) . ? Re3 C3' 2.005(12) . ? Re3 C4' 2.040(13) . ? Re3 C8' 2.150(10) . ? Re3 S2 2.503(3) . ? Re3 Re4 2.8818(7) . ? Re4 C7' 1.874(15) . ? Re4 C6' 1.932(12) . ? Re4 C5' 1.950(11) . ? Re4 C8' 2.239(10) . ? Re4 S2 2.425(3) . ? Re4 C9' 2.433(9) . ? S2 C15' 1.766(9) . ? O1' C1' 1.126(14) . ? O2' C2' 1.132(14) . ? O3' C3' 1.130(13) . ? O4' C4' 1.083(14) . ? O5' C5' 1.128(12) . ? O6' C6' 1.126(13) . ? O7' C7' 1.140(15) . ? C8' C9' 1.343(15) . ? C9' C10' 1.473(15) . ? C10' C15' 1.395(14) . ? C10' C11' 1.402(14) . ? C11' C12' 1.368(18) . ? C12' C13' 1.354(18) . ? C13' C14' 1.381(15) . ? C14' C15' 1.412(15) . ? 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 C4 94.6(5) . . ? C1 Re1 C2 84.2(5) . . ? C4 Re1 C2 85.6(5) . . ? C1 Re1 C3 89.7(5) . . ? C4 Re1 C3 90.6(5) . . ? C2 Re1 C3 172.6(5) . . ? C1 Re1 C8 172.3(4) . . ? C4 Re1 C8 88.8(4) . . ? C2 Re1 C8 103.0(4) . . ? C3 Re1 C8 83.3(5) . . ? C1 Re1 S1 94.4(3) . . ? C4 Re1 S1 171.0(4) . . ? C2 Re1 S1 94.8(3) . . ? C3 Re1 S1 89.9(3) . . ? C8 Re1 S1 82.3(3) . . ? C1 Re1 Re2 133.2(3) . . ? C4 Re1 Re2 119.5(4) . . ? C2 Re1 Re2 68.8(3) . . ? C3 Re1 Re2 118.6(3) . . ? C8 Re1 Re2 49.3(3) . . ? S1 Re1 Re2 52.92(6) . . ? C7 Re2 C6 88.0(5) . . ? C7 Re2 C5 88.6(5) . . ? C6 Re2 C5 90.6(5) . . ? C7 Re2 C8 117.8(4) . . ? C6 Re2 C8 87.9(4) . . ? C5 Re2 C8 153.5(4) . . ? C7 Re2 C9 85.5(4) . . ? C6 Re2 C9 97.7(4) . . ? C5 Re2 C9 169.6(4) . . ? C8 Re2 C9 34.1(4) . . ? C7 Re2 S1 102.6(4) . . ? C6 Re2 S1 168.2(3) . . ? C5 Re2 S1 94.5(3) . . ? C8 Re2 S1 82.8(3) . . ? C9 Re2 S1 78.4(3) . . ? C7 Re2 Re1 150.9(4) . . ? C6 Re2 Re1 113.0(3) . . ? C5 Re2 Re1 110.2(3) . . ? C8 Re2 Re1 47.3(3) . . ? C9 Re2 Re1 72.3(3) . . ? S1 Re2 Re1 55.31(6) . . ? C15 S1 Re2 102.1(4) . . ? C15 S1 Re1 102.3(3) . . ? Re2 S1 Re1 71.77(7) . . ? O1 C1 Re1 177.9(11) . . ? O2 C2 Re1 171.0(10) . . ? O3 C3 Re1 177.8(11) . . ? O4 C4 Re1 176.4(11) . . ? O5 C5 Re2 178.8(9) . . ? O6 C6 Re2 178.8(10) . . ? O7 C7 Re2 178.2(12) . . ? C9 C8 Re1 126.4(8) . . ? C9 C8 Re2 81.1(6) . . ? Re1 C8 Re2 83.4(3) . . ? C8 C9 C10 126.6(10) . . ? C8 C9 Re2 64.7(6) . . ? C10 C9 Re2 107.8(7) . . ? C15 C10 C11 116.9(11) . . ? C15 C10 C9 123.8(10) . . ? C11 C10 C9 119.2(10) . . ? C12 C11 C10 121.5(12) . . ? C13 C12 C11 118.7(12) . . ? C12 C13 C14 121.7(12) . . ? C15 C14 C13 119.2(12) . . ? C14 C15 C10 122.0(11) . . ? C14 C15 S1 120.7(8) . . ? C10 C15 S1 117.3(9) . . ? C2' Re3 C1' 94.3(5) . . ? C2' Re3 C3' 86.5(4) . . ? C1' Re3 C3' 84.6(5) . . ? C2' Re3 C4' 89.6(5) . . ? C1' Re3 C4' 88.9(5) . . ? C3' Re3 C4' 172.2(5) . . ? C2' Re3 C8' 88.0(4) . . ? C1' Re3 C8' 174.4(5) . . ? C3' Re3 C8' 100.6(4) . . ? C4' Re3 C8' 86.0(5) . . ? C2' Re3 S2 170.3(3) . . ? C1' Re3 S2 95.4(4) . . ? C3' Re3 S2 95.2(3) . . ? C4' Re3 S2 89.9(4) . . ? C8' Re3 S2 82.2(3) . . ? C2' Re3 Re4 119.8(3) . . ? C1' Re3 Re4 131.6(4) . . ? C3' Re3 Re4 66.2(3) . . ? C4' Re3 Re4 121.6(4) . . ? C8' Re3 Re4 50.3(3) . . ? S2 Re3 Re4 52.96(6) . . ? C7' Re4 C6' 90.4(5) . . ? C7' Re4 C5' 91.4(5) . . ? C6' Re4 C5' 88.5(4) . . ? C7' Re4 C8' 115.1(4) . . ? C6' Re4 C8' 90.1(4) . . ? C5' Re4 C8' 153.5(4) . . ? C7' Re4 S2 102.0(4) . . ? C6' Re4 S2 167.3(3) . . ? C5' Re4 S2 93.8(3) . . ? C8' Re4 S2 82.3(3) . . ? C7' Re4 C9' 83.6(4) . . ? C6' Re4 C9' 100.7(4) . . ? C5' Re4 C9' 169.6(5) . . ? C8' Re4 C9' 33.1(4) . . ? S2 Re4 C9' 78.4(3) . . ? C7' Re4 Re3 149.3(3) . . ? C6' Re4 Re3 112.0(3) . . ? C5' Re4 Re3 109.1(3) . . ? C8' Re4 Re3 47.6(3) . . ? S2 Re4 Re3 55.48(7) . . ? C9' Re4 Re3 72.2(3) . . ? C15' S2 Re4 101.8(3) . . ? C15' S2 Re3 102.1(4) . . ? Re4 S2 Re3 71.56(7) . . ? O1' C1' Re3 176.2(13) . . ? O2' C2' Re3 177.0(10) . . ? O3' C3' Re3 166.9(11) . . ? O4' C4' Re3 175.2(13) . . ? O5' C5' Re4 176.4(9) . . ? O6' C6' Re4 176.2(9) . . ? O7' C7' Re4 175.3(10) . . ? C9' C8' Re3 127.5(9) . . ? C9' C8' Re4 81.4(6) . . ? Re3 C8' Re4 82.1(3) . . ? C8' C9' C10' 127.3(10) . . ? C8' C9' Re4 65.5(5) . . ? C10' C9' Re4 106.7(6) . . ? C15' C10' C11' 117.4(10) . . ? C15' C10' C9' 122.6(9) . . ? C11' C10' C9' 119.9(10) . . ? C12' C11' C10' 121.4(11) . . ? C13' C12' C11' 121.0(11) . . ? C12' C13' C14' 120.5(12) . . ? C13' C14' C15' 119.2(11) . . ? C10' C15' C14' 120.6(9) . . ? C10' C15' S2 118.9(8) . . ? C14' C15' S2 120.4(8) . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 23.39 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 1.211 _refine_diff_density_min -1.845 _refine_diff_density_rms 0.247 #===END data_ang16 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H24 O7 P2 Re2 S' _chemical_formula_weight 854.80 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.1110(4) _cell_length_b 27.1151(13) _cell_length_c 12.3490(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.0860(10) _cell_angle_gamma 90.00 _cell_volume 2655.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 9.344 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.1598 _exptl_absorpt_correction_T_max 0.4551 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6297 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.34 _reflns_number_total 6297 _reflns_number_gt 4869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6297 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0353 _refine_ls_wR_factor_gt 0.0331 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _refine_ls_shift/su_max 0.002 _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 0.937529(18) 0.130651(5) 0.112039(12) 0.02232(4) Uani 1 1 d . . . Re2 Re 0.977927(18) 0.138819(5) 0.463344(12) 0.02002(4) Uani 1 1 d . . . S S 0.80256(11) 0.11754(3) 0.27439(7) 0.0212(2) Uani 1 1 d . . . P1 P 0.67164(13) 0.10209(4) -0.00558(8) 0.0295(2) Uani 1 1 d . . . P2 P 0.74644(13) 0.19275(4) 0.49104(9) 0.0312(3) Uani 1 1 d . . . O9 O 1.2961(3) 0.15455(10) 0.2441(2) 0.0396(7) Uani 1 1 d . . . O10 O 0.8062(4) 0.23849(10) 0.0963(3) 0.0520(9) Uani 1 1 d . . . O11 O 1.0675(4) 0.13956(11) -0.1031(2) 0.0566(9) Uani 1 1 d . . . O15 O 1.2560(3) 0.06806(10) 0.4158(2) 0.0388(7) Uani 1 1 d . . . O16 O 0.8210(3) 0.05343(11) 0.5788(2) 0.0516(9) Uani 1 1 d . . . O17 O 1.2005(3) 0.16526(10) 0.6893(2) 0.0385(7) Uani 1 1 d . . . O18 O 1.1125(4) 0.23240(10) 0.3619(2) 0.0455(8) Uani 1 1 d . . . C1 C 1.0254(4) 0.05511(13) 0.1367(3) 0.0286(9) Uani 1 1 d . . . H1 H 1.1144 0.0471 0.1005 0.034 Uiso 1 1 calc R . . C2 C 0.9770(5) 0.01756(13) 0.1939(3) 0.0312(10) Uani 1 1 d . . . H2 H 1.0462 -0.0110 0.1996 0.037 Uiso 1 1 calc R . . C3 C 0.8344(4) 0.01393(12) 0.2483(3) 0.0221(8) Uani 1 1 d . . . C4 C 0.7785(5) -0.03364(13) 0.2693(3) 0.0273(9) Uani 1 1 d . . . H4 H 0.8367 -0.0614 0.2489 0.033 Uiso 1 1 calc R . . C5 C 0.6434(5) -0.04158(14) 0.3179(3) 0.0292(9) Uani 1 1 d . . . H5 H 0.6118 -0.0743 0.3325 0.035 Uiso 1 1 calc R . . C6 C 0.5536(5) -0.00217(13) 0.3455(3) 0.0324(10) Uani 1 1 d . . . H6 H 0.4576 -0.0074 0.3769 0.039 Uiso 1 1 calc R . . C7 C 0.6052(4) 0.04509(14) 0.3269(3) 0.0305(9) Uani 1 1 d . . . H7 H 0.5422 0.0723 0.3447 0.037 Uiso 1 1 calc R . . C8 C 0.7469(4) 0.05378(12) 0.2828(3) 0.0225(8) Uani 1 1 d . . . C9 C 1.1603(5) 0.14663(13) 0.1966(3) 0.0273(9) Uani 1 1 d . . . C10 C 0.8542(5) 0.19811(15) 0.1015(3) 0.0323(10) Uani 1 1 d . . . C11 C 1.0212(5) 0.13664(14) -0.0202(3) 0.0356(10) Uani 1 1 d . . . C12 C 0.4783(5) 0.1075(2) 0.0459(4) 0.0720(17) Uani 1 1 d . . . H12A H 0.3819 0.0987 -0.0132 0.108 Uiso 1 1 calc R . . H12B H 0.4657 0.1415 0.0698 0.108 Uiso 1 1 calc R . . H12C H 0.4832 0.0851 0.1088 0.108 Uiso 1 1 calc R . . C13 C 0.6193(6) 0.13521(16) -0.1360(4) 0.0695(16) Uani 1 1 d . . . H13A H 0.6990 0.1262 -0.1823 0.104 Uiso 1 1 calc R . . H13B H 0.6259 0.1708 -0.1217 0.104 Uiso 1 1 calc R . . H13C H 0.5046 0.1266 -0.1744 0.104 Uiso 1 1 calc R . . C14 C 0.6661(5) 0.03872(13) -0.0508(3) 0.0424(11) Uani 1 1 d . . . H14A H 0.5564 0.0317 -0.0991 0.064 Uiso 1 1 calc R . . H14B H 0.6830 0.0169 0.0138 0.064 Uiso 1 1 calc R . . H14C H 0.7557 0.0331 -0.0917 0.064 Uiso 1 1 calc R . . C15 C 1.1543(5) 0.09379(13) 0.4320(3) 0.0259(9) Uani 1 1 d . . . C16 C 0.8777(5) 0.08364(14) 0.5353(3) 0.0303(9) Uani 1 1 d . . . C17 C 1.1156(5) 0.15623(13) 0.6058(3) 0.0257(9) Uani 1 1 d . . . C18 C 1.0648(5) 0.19784(13) 0.3972(3) 0.0285(9) Uani 1 1 d . . . C19 C 0.5662(5) 0.16276(16) 0.5255(4) 0.0548(13) Uani 1 1 d . . . H19A H 0.6034 0.1411 0.5895 0.082 Uiso 1 1 calc R . . H19B H 0.5082 0.1432 0.4622 0.082 Uiso 1 1 calc R . . H19C H 0.4888 0.1877 0.5437 0.082 Uiso 1 1 calc R . . C20 C 0.8072(6) 0.23673(16) 0.6023(4) 0.0674(16) Uani 1 1 d . . . H20A H 0.7108 0.2579 0.6067 0.101 Uiso 1 1 calc R . . H20B H 0.9002 0.2571 0.5881 0.101 Uiso 1 1 calc R . . H20C H 0.8436 0.2191 0.6725 0.101 Uiso 1 1 calc R . . C21 C 0.6513(6) 0.22994(16) 0.3735(4) 0.0640(15) Uani 1 1 d . . . H21A H 0.6102 0.2085 0.3096 0.096 Uiso 1 1 calc R . . H21B H 0.7353 0.2529 0.3560 0.096 Uiso 1 1 calc R . . H21C H 0.5567 0.2486 0.3910 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 0.02615(9) 0.02058(8) 0.02111(9) 0.00215(7) 0.00693(7) 0.00212(6) Re2 0.02129(8) 0.01867(7) 0.02066(8) -0.00005(6) 0.00568(6) -0.00140(6) S 0.0220(5) 0.0202(5) 0.0217(5) -0.0014(4) 0.0057(4) 0.0000(4) P1 0.0330(6) 0.0283(6) 0.0253(6) -0.0028(5) 0.0015(5) 0.0044(5) P2 0.0299(6) 0.0280(6) 0.0356(7) -0.0105(5) 0.0068(5) 0.0027(5) O9 0.0251(16) 0.0580(19) 0.0360(18) 0.0047(15) 0.0066(14) -0.0048(14) O10 0.071(2) 0.0233(16) 0.061(2) 0.0025(15) 0.0117(18) 0.0135(16) O11 0.076(2) 0.066(2) 0.035(2) 0.0113(18) 0.0273(18) 0.0049(19) O15 0.0356(17) 0.0423(17) 0.0392(18) 0.0042(14) 0.0091(14) 0.0154(14) O16 0.0418(19) 0.060(2) 0.049(2) 0.0243(17) 0.0007(16) -0.0208(16) O17 0.0454(18) 0.0423(17) 0.0243(17) -0.0020(14) -0.0005(14) -0.0097(14) O18 0.070(2) 0.0286(16) 0.0392(19) 0.0022(14) 0.0155(16) -0.0182(15) C1 0.026(2) 0.028(2) 0.035(2) -0.0009(18) 0.0134(19) 0.0052(17) C2 0.029(2) 0.027(2) 0.038(3) 0.0054(19) 0.0100(19) 0.0109(18) C3 0.022(2) 0.024(2) 0.019(2) -0.0016(16) 0.0014(16) 0.0010(16) C4 0.034(2) 0.023(2) 0.023(2) 0.0008(17) 0.0011(18) 0.0012(17) C5 0.035(2) 0.028(2) 0.021(2) -0.0002(18) -0.0036(18) -0.0120(18) C6 0.031(2) 0.034(2) 0.034(3) -0.0018(19) 0.012(2) -0.0128(19) C7 0.027(2) 0.030(2) 0.035(2) -0.0091(19) 0.0064(19) -0.0023(17) C8 0.020(2) 0.023(2) 0.024(2) -0.0008(16) 0.0026(16) -0.0033(15) C9 0.033(2) 0.025(2) 0.026(2) 0.0023(17) 0.0120(19) -0.0002(18) C10 0.033(2) 0.036(2) 0.028(2) 0.0039(19) 0.0071(19) -0.0034(19) C11 0.041(3) 0.034(2) 0.033(3) 0.001(2) 0.010(2) 0.0030(19) C12 0.030(3) 0.117(5) 0.065(4) -0.042(3) -0.003(2) 0.015(3) C13 0.096(4) 0.048(3) 0.046(3) 0.019(3) -0.026(3) -0.019(3) C14 0.044(3) 0.031(2) 0.050(3) -0.007(2) 0.004(2) 0.001(2) C15 0.028(2) 0.029(2) 0.021(2) 0.0037(17) 0.0049(18) -0.0032(18) C16 0.025(2) 0.035(2) 0.030(2) 0.0030(19) 0.0033(18) -0.0035(18) C17 0.031(2) 0.021(2) 0.028(2) 0.0020(17) 0.0136(19) -0.0014(17) C18 0.036(2) 0.026(2) 0.023(2) -0.0048(18) 0.0022(18) 0.0020(19) C19 0.035(3) 0.065(3) 0.072(4) -0.017(3) 0.026(3) 0.002(2) C20 0.050(3) 0.065(3) 0.084(4) -0.053(3) 0.006(3) 0.010(3) C21 0.065(4) 0.052(3) 0.074(4) 0.006(3) 0.012(3) 0.032(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C11 1.902(4) . ? Re1 C9 1.937(4) . ? Re1 C10 1.945(4) . ? Re1 C1 2.169(3) . ? Re1 P1 2.4594(10) . ? Re1 S 2.5027(9) . ? Re2 C17 1.934(4) . ? Re2 C15 1.980(4) . ? Re2 C18 1.992(4) . ? Re2 C16 1.998(4) . ? Re2 P2 2.4597(10) . ? Re2 S 2.5320(9) . ? S C8 1.796(3) . ? P1 C14 1.805(4) . ? P1 C13 1.815(4) . ? P1 C12 1.817(4) . ? P2 C19 1.800(4) . ? P2 C21 1.803(4) . ? P2 C20 1.808(4) . ? O9 C9 1.155(4) . ? O10 C10 1.159(4) . ? O11 C11 1.164(4) . ? O15 C15 1.130(4) . ? O16 C16 1.129(4) . ? O17 C17 1.140(4) . ? O18 C18 1.135(4) . ? C1 C2 1.343(5) . ? C2 C3 1.458(5) . ? C3 C8 1.407(4) . ? C3 C4 1.409(5) . ? C4 C5 1.373(5) . ? C5 C6 1.375(5) . ? C6 C7 1.382(5) . ? C7 C8 1.391(5) . ? 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 C11 Re1 C9 89.06(16) . . ? C11 Re1 C10 92.52(16) . . ? C9 Re1 C10 95.59(15) . . ? C11 Re1 C1 92.03(15) . . ? C9 Re1 C1 83.89(14) . . ? C10 Re1 C1 175.41(15) . . ? C11 Re1 P1 86.93(12) . . ? C9 Re1 P1 172.92(11) . . ? C10 Re1 P1 90.42(11) . . ? C1 Re1 P1 90.42(10) . . ? C11 Re1 S 173.97(12) . . ? C9 Re1 S 96.59(11) . . ? C10 Re1 S 89.02(11) . . ? C1 Re1 S 86.51(10) . . ? P1 Re1 S 87.24(3) . . ? C17 Re2 C15 91.45(15) . . ? C17 Re2 C18 89.45(15) . . ? C15 Re2 C18 94.75(15) . . ? C17 Re2 C16 89.40(15) . . ? C15 Re2 C16 90.18(15) . . ? C18 Re2 C16 174.97(15) . . ? C17 Re2 P2 92.32(11) . . ? C15 Re2 P2 176.20(11) . . ? C18 Re2 P2 85.72(11) . . ? C16 Re2 P2 89.43(11) . . ? C17 Re2 S 178.45(11) . . ? C15 Re2 S 88.20(11) . . ? C18 Re2 S 89.07(11) . . ? C16 Re2 S 92.11(11) . . ? P2 Re2 S 88.04(3) . . ? C8 S Re1 109.94(12) . . ? C8 S Re2 105.40(12) . . ? Re1 S Re2 116.76(3) . . ? C14 P1 C13 102.1(2) . . ? C14 P1 C12 102.5(2) . . ? C13 P1 C12 102.2(2) . . ? C14 P1 Re1 116.40(14) . . ? C13 P1 Re1 112.43(15) . . ? C12 P1 Re1 118.85(15) . . ? C19 P2 C21 102.2(2) . . ? C19 P2 C20 102.9(2) . . ? C21 P2 C20 104.2(2) . . ? C19 P2 Re2 116.47(15) . . ? C21 P2 Re2 115.53(15) . . ? C20 P2 Re2 113.78(15) . . ? C2 C1 Re1 131.8(3) . . ? C1 C2 C3 129.9(3) . . ? C8 C3 C4 116.4(3) . . ? C8 C3 C2 126.0(3) . . ? C4 C3 C2 117.6(3) . . ? C5 C4 C3 122.8(3) . . ? C4 C5 C6 119.9(3) . . ? C5 C6 C7 119.0(4) . . ? C6 C7 C8 121.7(3) . . ? C7 C8 C3 119.9(3) . . ? C7 C8 S 115.1(3) . . ? C3 C8 S 124.9(3) . . ? O9 C9 Re1 176.8(3) . . ? O10 C10 Re1 179.2(4) . . ? O11 C11 Re1 177.7(4) . . ? O15 C15 Re2 178.9(3) . . ? O16 C16 Re2 177.7(4) . . ? O17 C17 Re2 177.7(3) . . ? O18 C18 Re2 177.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Re1 S C8 46.7(11) . . . . ? C9 Re1 S C8 -112.84(16) . . . . ? C10 Re1 S C8 151.65(16) . . . . ? C1 Re1 S C8 -29.41(15) . . . . ? P1 Re1 S C8 61.18(12) . . . . ? C11 Re1 S Re2 166.7(11) . . . . ? C9 Re1 S Re2 7.11(11) . . . . ? C10 Re1 S Re2 -88.40(12) . . . . ? C1 Re1 S Re2 90.54(10) . . . . ? P1 Re1 S Re2 -178.87(4) . . . . ? C17 Re2 S C8 144(4) . . . . ? C15 Re2 S C8 67.22(16) . . . . ? C18 Re2 S C8 162.00(16) . . . . ? C16 Re2 S C8 -22.89(16) . . . . ? P2 Re2 S C8 -112.25(12) . . . . ? C17 Re2 S Re1 22(4) . . . . ? C15 Re2 S Re1 -55.12(11) . . . . ? C18 Re2 S Re1 39.66(11) . . . . ? C16 Re2 S Re1 -145.24(11) . . . . ? P2 Re2 S Re1 125.41(4) . . . . ? C11 Re1 P1 C14 79.01(19) . . . . ? C9 Re1 P1 C14 23.5(9) . . . . ? C10 Re1 P1 C14 171.51(19) . . . . ? C1 Re1 P1 C14 -13.00(18) . . . . ? S Re1 P1 C14 -99.49(16) . . . . ? C11 Re1 P1 C13 -38.3(2) . . . . ? C9 Re1 P1 C13 -93.9(9) . . . . ? C10 Re1 P1 C13 54.2(2) . . . . ? C1 Re1 P1 C13 -130.3(2) . . . . ? S Re1 P1 C13 143.19(19) . . . . ? C11 Re1 P1 C12 -157.6(2) . . . . ? C9 Re1 P1 C12 146.9(9) . . . . ? C10 Re1 P1 C12 -65.1(2) . . . . ? C1 Re1 P1 C12 110.4(2) . . . . ? S Re1 P1 C12 23.9(2) . . . . ? C17 Re2 P2 C19 -104.2(2) . . . . ? C15 Re2 P2 C19 69.2(16) . . . . ? C18 Re2 P2 C19 166.5(2) . . . . ? C16 Re2 P2 C19 -14.8(2) . . . . ? S Re2 P2 C19 77.28(17) . . . . ? C17 Re2 P2 C21 135.8(2) . . . . ? C15 Re2 P2 C21 -50.7(16) . . . . ? C18 Re2 P2 C21 46.5(2) . . . . ? C16 Re2 P2 C21 -134.8(2) . . . . ? S Re2 P2 C21 -42.69(18) . . . . ? C17 Re2 P2 C20 15.3(2) . . . . ? C15 Re2 P2 C20 -171.3(16) . . . . ? C18 Re2 P2 C20 -74.0(2) . . . . ? C16 Re2 P2 C20 104.7(2) . . . . ? S Re2 P2 C20 -163.21(19) . . . . ? C11 Re1 C1 C2 -157.4(4) . . . . ? C9 Re1 C1 C2 113.8(4) . . . . ? C10 Re1 C1 C2 30(2) . . . . ? P1 Re1 C1 C2 -70.4(4) . . . . ? S Re1 C1 C2 16.8(4) . . . . ? Re1 C1 C2 C3 7.9(7) . . . . ? C1 C2 C3 C8 -21.6(6) . . . . ? C1 C2 C3 C4 158.7(4) . . . . ? C8 C3 C4 C5 1.7(5) . . . . ? C2 C3 C4 C5 -178.6(3) . . . . ? C3 C4 C5 C6 1.8(6) . . . . ? C4 C5 C6 C7 -2.2(6) . . . . ? C5 C6 C7 C8 -1.1(6) . . . . ? C6 C7 C8 C3 4.7(6) . . . . ? C6 C7 C8 S -175.6(3) . . . . ? C4 C3 C8 C7 -4.8(5) . . . . ? C2 C3 C8 C7 175.5(3) . . . . ? C4 C3 C8 S 175.5(3) . . . . ? C2 C3 C8 S -4.2(5) . . . . ? Re1 S C8 C7 -148.9(2) . . . . ? Re2 S C8 C7 84.5(3) . . . . ? Re1 S C8 C3 30.8(3) . . . . ? Re2 S C8 C3 -95.8(3) . . . . ? C11 Re1 C9 O9 -48(6) . . . . ? C10 Re1 C9 O9 -140(6) . . . . ? C1 Re1 C9 O9 44(6) . . . . ? P1 Re1 C9 O9 8(7) . . . . ? S Re1 C9 O9 130(6) . . . . ? C11 Re1 C10 O10 -106(27) . . . . ? C9 Re1 C10 O10 -17(27) . . . . ? C1 Re1 C10 O10 66(27) . . . . ? P1 Re1 C10 O10 167(100) . . . . ? S Re1 C10 O10 80(27) . . . . ? C9 Re1 C11 O11 168(100) . . . . ? C10 Re1 C11 O11 -97(9) . . . . ? C1 Re1 C11 O11 84(9) . . . . ? P1 Re1 C11 O11 -6(9) . . . . ? S Re1 C11 O11 8(10) . . . . ? C17 Re2 C15 O15 22(17) . . . . ? C18 Re2 C15 O15 112(17) . . . . ? C16 Re2 C15 O15 -67(17) . . . . ? P2 Re2 C15 O15 -152(16) . . . . ? S Re2 C15 O15 -160(100) . . . . ? C17 Re2 C16 O16 40(9) . . . . ? C15 Re2 C16 O16 131(9) . . . . ? C18 Re2 C16 O16 -37(10) . . . . ? P2 Re2 C16 O16 -53(9) . . . . ? S Re2 C16 O16 -141(9) . . . . ? C15 Re2 C17 O17 -9(9) . . . . ? C18 Re2 C17 O17 -104(9) . . . . ? C16 Re2 C17 O17 81(9) . . . . ? P2 Re2 C17 O17 170(100) . . . . ? S Re2 C17 O17 -86(10) . . . . ? C17 Re2 C18 O18 -57(9) . . . . ? C15 Re2 C18 O18 -149(9) . . . . ? C16 Re2 C18 O18 20(10) . . . . ? P2 Re2 C18 O18 35(9) . . . . ? S Re2 C18 O18 123(9) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.802 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.133 #===END data_ang17tm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H33 O7 P3 Re2 S' _chemical_formula_weight 930.87 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' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.6900(4) _cell_length_b 25.4267(12) _cell_length_c 25.8065(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6358.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 7.862 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1409 _exptl_absorpt_correction_T_max 0.6946 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7716 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7716 _reflns_number_gt 5755 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0030P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7716 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0349 _refine_ls_wR_factor_gt 0.0327 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.002 _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 0.264353(13) 0.432837(6) 0.148372(5) 0.02310(4) Uani 1 1 d . . . Re2 Re 0.469778(13) 0.127282(5) 0.115865(5) 0.02065(4) Uani 1 1 d . . . S S 0.43661(9) 0.22343(4) 0.13375(3) 0.0274(2) Uani 1 1 d . . . P1 P 0.51668(9) 0.43011(4) 0.14115(4) 0.0334(2) Uani 1 1 d . . . P2 P 0.71747(9) 0.14964(4) 0.11343(4) 0.0274(2) Uani 1 1 d . . . P3 P 0.42309(9) 0.15472(4) 0.02617(3) 0.0253(2) Uani 1 1 d . . . O9 O 0.3016(3) 0.35856(11) 0.24400(10) 0.0482(8) Uani 1 1 d . . . O10 O -0.0538(2) 0.42886(10) 0.16004(10) 0.0444(7) Uani 1 1 d . . . O11 O 0.2784(3) 0.53055(11) 0.22076(9) 0.0425(7) Uani 1 1 d . . . O12 O 0.2554(3) 0.49813(11) 0.04598(9) 0.0469(7) Uani 1 1 d . . . O16 O 0.1599(2) 0.09869(10) 0.12189(10) 0.0414(7) Uani 1 1 d . . . O17 O 0.4991(3) 0.09543(11) 0.23121(9) 0.0437(7) Uani 1 1 d . . . O18 O 0.5581(3) 0.01742(10) 0.07933(10) 0.0452(7) Uani 1 1 d . . . C1 C 0.2784(3) 0.36596(14) 0.09426(12) 0.0258(8) Uani 1 1 d . . . H1 H 0.3046 0.3764 0.0603 0.031 Uiso 1 1 calc R . . C2 C 0.2587(3) 0.31446(14) 0.09814(12) 0.0268(8) Uani 1 1 d . . . H2 H 0.2840 0.2947 0.0684 0.032 Uiso 1 1 calc R . . C3 C 0.2033(3) 0.28317(14) 0.14175(13) 0.0251(8) Uani 1 1 d . . . C4 C 0.0778(4) 0.29649(15) 0.16538(15) 0.0382(10) Uani 1 1 d . . . H4 H 0.0279 0.3260 0.1528 0.046 Uiso 1 1 calc R . . C5 C 0.0247(4) 0.26822(16) 0.20613(16) 0.0449(11) Uani 1 1 d . . . H5 H -0.0601 0.2784 0.2216 0.054 Uiso 1 1 calc R . . C6 C 0.0948(4) 0.22518(16) 0.22428(15) 0.0437(11) Uani 1 1 d . . . H6 H 0.0596 0.2059 0.2529 0.052 Uiso 1 1 calc R . . C7 C 0.2161(4) 0.20993(15) 0.20111(13) 0.0347(9) Uani 1 1 d . . . H7 H 0.2623 0.1794 0.2133 0.042 Uiso 1 1 calc R . . C8 C 0.2728(3) 0.23826(14) 0.16020(12) 0.0239(8) Uani 1 1 d . . . C9 C 0.2858(3) 0.38481(15) 0.20843(14) 0.0307(9) Uani 1 1 d . . . C10 C 0.0638(4) 0.43017(14) 0.15440(13) 0.0293(8) Uani 1 1 d . . . C11 C 0.2728(3) 0.49474(15) 0.19367(13) 0.0280(9) Uani 1 1 d . . . C12 C 0.2565(4) 0.47577(14) 0.08442(14) 0.0308(9) Uani 1 1 d . . . C13 C 0.6059(4) 0.46905(17) 0.18938(16) 0.0604(14) Uani 1 1 d . . . H13A H 0.7058 0.4656 0.1844 0.091 Uiso 1 1 calc R . . H13B H 0.5811 0.4565 0.2241 0.091 Uiso 1 1 calc R . . H13C H 0.5792 0.5060 0.1858 0.091 Uiso 1 1 calc R . . C14 C 0.5864(4) 0.4544(2) 0.08044(17) 0.0796(17) Uani 1 1 d . . . H14A H 0.5557 0.4907 0.0749 0.119 Uiso 1 1 calc R . . H14B H 0.5537 0.4322 0.0519 0.119 Uiso 1 1 calc R . . H14C H 0.6874 0.4533 0.0817 0.119 Uiso 1 1 calc R . . C15 C 0.5948(4) 0.36565(16) 0.14804(18) 0.0613(13) Uani 1 1 d . . . H15A H 0.5583 0.3420 0.1214 0.092 Uiso 1 1 calc R . . H15B H 0.5734 0.3514 0.1824 0.092 Uiso 1 1 calc R . . H15C H 0.6951 0.3687 0.1441 0.092 Uiso 1 1 calc R . . C16 C 0.2752(4) 0.11004(14) 0.12007(13) 0.0268(8) Uani 1 1 d . . . C17 C 0.4908(3) 0.10803(14) 0.18871(14) 0.0290(9) Uani 1 1 d . . . C18 C 0.5215(3) 0.05842(15) 0.09369(13) 0.0284(9) Uani 1 1 d . . . C19 C 0.8117(4) 0.12572(18) 0.16888(13) 0.0501(12) Uani 1 1 d . . . H19A H 0.9085 0.1365 0.1662 0.075 Uiso 1 1 calc R . . H19B H 0.8063 0.0873 0.1700 0.075 Uiso 1 1 calc R . . H19C H 0.7715 0.1404 0.2006 0.075 Uiso 1 1 calc R . . C20 C 0.7696(4) 0.21771(16) 0.11266(16) 0.0574(13) Uani 1 1 d . . . H20A H 0.8704 0.2199 0.1154 0.086 Uiso 1 1 calc R . . H20B H 0.7274 0.2361 0.1420 0.086 Uiso 1 1 calc R . . H20C H 0.7396 0.2341 0.0802 0.086 Uiso 1 1 calc R . . C21 C 0.8144(4) 0.12230(18) 0.05998(14) 0.0567(14) Uani 1 1 d . . . H21A H 0.7791 0.1365 0.0273 0.085 Uiso 1 1 calc R . . H21B H 0.8047 0.0839 0.0599 0.085 Uiso 1 1 calc R . . H21C H 0.9120 0.1316 0.0637 0.085 Uiso 1 1 calc R . . C22 C 0.4532(4) 0.10548(15) -0.02347(13) 0.0382(10) Uani 1 1 d . . . H22A H 0.4009 0.0736 -0.0152 0.057 Uiso 1 1 calc R . . H22B H 0.5518 0.0971 -0.0249 0.057 Uiso 1 1 calc R . . H22C H 0.4231 0.1191 -0.0571 0.057 Uiso 1 1 calc R . . C23 C 0.5099(4) 0.21247(14) 0.00104(12) 0.0348(9) Uani 1 1 d . . . H23A H 0.6095 0.2060 -0.0002 0.052 Uiso 1 1 calc R . . H23B H 0.4911 0.2426 0.0237 0.052 Uiso 1 1 calc R . . H23C H 0.4760 0.2200 -0.0340 0.052 Uiso 1 1 calc R . . C24 C 0.2434(3) 0.17138(15) 0.01573(13) 0.0385(10) Uani 1 1 d . . . H24A H 0.2314 0.1846 -0.0196 0.058 Uiso 1 1 calc R . . H24B H 0.2154 0.1985 0.0405 0.058 Uiso 1 1 calc R . . H24C H 0.1863 0.1400 0.0206 0.058 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 0.02256(7) 0.02094(8) 0.02580(7) 0.00104(7) -0.00170(6) 0.00112(6) Re2 0.01983(7) 0.01852(7) 0.02360(7) 0.00253(7) 0.00147(6) 0.00186(6) S 0.0279(5) 0.0209(5) 0.0334(5) -0.0005(4) 0.0036(4) 0.0020(4) P1 0.0233(5) 0.0333(6) 0.0437(6) -0.0057(5) -0.0006(5) 0.0001(5) P2 0.0212(5) 0.0345(6) 0.0265(5) 0.0033(5) -0.0006(4) 0.0006(4) P3 0.0262(5) 0.0257(6) 0.0238(5) 0.0005(4) 0.0000(4) -0.0003(4) O9 0.0608(19) 0.046(2) 0.0383(17) 0.0100(14) -0.0093(14) 0.0066(15) O10 0.0241(14) 0.0474(19) 0.0618(19) 0.0078(15) 0.0057(13) 0.0038(14) O11 0.0504(18) 0.0344(18) 0.0426(17) -0.0098(14) 0.0053(14) -0.0028(14) O12 0.0599(18) 0.0430(19) 0.0377(16) 0.0136(14) 0.0017(15) 0.0068(16) O16 0.0260(14) 0.0452(19) 0.0529(18) 0.0050(15) 0.0016(14) -0.0041(13) O17 0.0479(18) 0.055(2) 0.0278(14) 0.0145(14) 0.0008(13) 0.0044(14) O18 0.0489(18) 0.0236(17) 0.0633(19) -0.0047(14) 0.0103(14) 0.0075(14) C1 0.0270(19) 0.028(2) 0.0229(18) 0.0026(16) -0.0070(15) 0.0051(18) C2 0.0271(19) 0.026(2) 0.0279(19) -0.0053(17) -0.0059(16) 0.0042(17) C3 0.0239(19) 0.020(2) 0.032(2) -0.0078(17) -0.0017(16) -0.0013(15) C4 0.027(2) 0.021(2) 0.067(3) -0.006(2) -0.002(2) 0.0002(17) C5 0.032(2) 0.029(3) 0.074(3) -0.016(2) 0.021(2) -0.001(2) C6 0.053(3) 0.033(3) 0.046(3) -0.006(2) 0.024(2) -0.008(2) C7 0.045(2) 0.027(2) 0.033(2) -0.0009(18) 0.0077(19) 0.0036(19) C8 0.0242(19) 0.022(2) 0.026(2) -0.0055(16) 0.0006(15) 0.0006(16) C9 0.030(2) 0.030(3) 0.032(2) -0.0051(18) -0.0038(17) 0.0025(18) C10 0.035(2) 0.025(2) 0.028(2) 0.0021(18) -0.0029(17) 0.0013(18) C11 0.027(2) 0.028(2) 0.029(2) 0.0030(18) 0.0016(17) 0.0030(18) C12 0.032(2) 0.026(2) 0.034(2) -0.0037(18) 0.0016(18) 0.0005(18) C13 0.031(2) 0.058(3) 0.092(4) -0.033(3) -0.009(2) -0.003(2) C14 0.041(3) 0.128(5) 0.070(4) 0.018(3) 0.020(2) 0.002(3) C15 0.031(2) 0.044(3) 0.109(4) -0.018(3) -0.015(3) 0.010(2) C16 0.033(2) 0.023(2) 0.0241(19) 0.0018(16) 0.0026(17) 0.0023(17) C17 0.024(2) 0.027(2) 0.036(2) -0.0009(18) 0.0060(17) 0.0019(17) C18 0.0229(19) 0.028(2) 0.034(2) 0.0067(18) 0.0050(16) 0.0015(18) C19 0.030(2) 0.082(4) 0.038(2) 0.014(2) -0.0026(19) 0.005(2) C20 0.031(2) 0.048(3) 0.093(4) 0.012(3) -0.004(2) -0.009(2) C21 0.027(2) 0.102(4) 0.041(3) -0.015(3) 0.0073(19) -0.003(2) C22 0.045(2) 0.042(3) 0.027(2) -0.0063(19) 0.0027(19) -0.003(2) C23 0.044(2) 0.034(2) 0.027(2) 0.0058(17) 0.0017(17) -0.0054(19) C24 0.034(2) 0.048(3) 0.033(2) 0.0054(19) -0.0075(18) 0.003(2) _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 C10 1.951(4) . ? Re1 C11 1.962(4) . ? Re1 C12 1.980(4) . ? Re1 C9 1.984(4) . ? Re1 C1 2.205(3) . ? Re1 P1 2.4531(9) . ? Re2 C18 1.909(4) . ? Re2 C16 1.939(4) . ? Re2 C17 1.953(4) . ? Re2 P3 2.4596(9) . ? Re2 P2 2.4674(9) . ? Re2 S 2.5086(9) . ? S C8 1.769(3) . ? P1 C13 1.810(4) . ? P1 C14 1.814(4) . ? P1 C15 1.814(4) . ? P2 C19 1.803(3) . ? P2 C21 1.808(4) . ? P2 C20 1.803(4) . ? P3 C24 1.812(3) . ? P3 C23 1.812(3) . ? P3 C22 1.815(3) . ? O9 C9 1.145(4) . ? O10 C10 1.149(4) . ? O11 C11 1.149(4) . ? O12 C12 1.144(4) . ? O16 C16 1.154(4) . ? O17 C17 1.145(4) . ? O18 C18 1.162(4) . ? C1 C2 1.327(4) . ? C2 C3 1.479(4) . ? C3 C4 1.402(4) . ? C3 C8 1.409(4) . ? C4 C5 1.374(5) . ? C5 C6 1.371(5) . ? C6 C7 1.375(4) . ? C7 C8 1.391(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 C10 Re1 C11 91.26(14) . . ? C10 Re1 C12 92.71(14) . . ? C11 Re1 C12 93.21(15) . . ? C10 Re1 C9 91.17(14) . . ? C11 Re1 C9 91.37(14) . . ? C12 Re1 C9 173.93(14) . . ? C10 Re1 C1 94.89(13) . . ? C11 Re1 C1 173.44(13) . . ? C12 Re1 C1 84.24(14) . . ? C9 Re1 C1 90.79(14) . . ? C10 Re1 P1 176.38(11) . . ? C11 Re1 P1 91.51(10) . . ? C12 Re1 P1 89.46(10) . . ? C9 Re1 P1 86.43(10) . . ? C1 Re1 P1 82.44(8) . . ? C18 Re2 C16 93.70(14) . . ? C18 Re2 C17 91.79(14) . . ? C16 Re2 C17 89.48(13) . . ? C18 Re2 P3 91.51(10) . . ? C16 Re2 P3 86.44(10) . . ? C17 Re2 P3 174.91(10) . . ? C18 Re2 P2 87.04(10) . . ? C16 Re2 P2 178.23(10) . . ? C17 Re2 P2 88.89(10) . . ? P3 Re2 P2 95.14(3) . . ? C18 Re2 S 169.30(10) . . ? C16 Re2 S 94.91(10) . . ? C17 Re2 S 94.62(11) . . ? P3 Re2 S 82.71(3) . . ? P2 Re2 S 84.54(3) . . ? C8 S Re2 113.18(12) . . ? C13 P1 C14 103.3(2) . . ? C13 P1 C15 103.13(19) . . ? C14 P1 C15 103.7(2) . . ? C13 P1 Re1 114.10(13) . . ? C14 P1 Re1 115.28(14) . . ? C15 P1 Re1 115.74(13) . . ? C19 P2 C21 102.29(18) . . ? C19 P2 C20 100.99(19) . . ? C21 P2 C20 102.4(2) . . ? C19 P2 Re2 113.24(13) . . ? C21 P2 Re2 115.87(13) . . ? C20 P2 Re2 119.61(13) . . ? C24 P3 C23 101.73(17) . . ? C24 P3 C22 102.16(17) . . ? C23 P3 C22 103.41(17) . . ? C24 P3 Re2 112.52(11) . . ? C23 P3 Re2 118.77(11) . . ? C22 P3 Re2 116.04(13) . . ? C2 C1 Re1 134.8(3) . . ? C1 C2 C3 129.8(3) . . ? C4 C3 C8 117.6(3) . . ? C4 C3 C2 121.1(3) . . ? C8 C3 C2 121.3(3) . . ? C5 C4 C3 122.1(4) . . ? C6 C5 C4 119.6(4) . . ? C5 C6 C7 120.0(4) . . ? C6 C7 C8 121.4(4) . . ? C7 C8 C3 119.2(3) . . ? C7 C8 S 122.5(3) . . ? C3 C8 S 118.1(3) . . ? O9 C9 Re1 177.2(3) . . ? O10 C10 Re1 177.3(3) . . ? O11 C11 Re1 179.0(3) . . ? O12 C12 Re1 176.0(3) . . ? O16 C16 Re2 178.4(3) . . ? O17 C17 Re2 177.4(3) . . ? O18 C18 Re2 177.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C18 Re2 S C8 159.6(6) . . . . ? C16 Re2 S C8 16.10(15) . . . . ? C17 Re2 S C8 -73.77(15) . . . . ? P3 Re2 S C8 101.87(12) . . . . ? P2 Re2 S C8 -162.22(12) . . . . ? C10 Re1 P1 C13 -124.3(16) . . . . ? C11 Re1 P1 C13 15.6(2) . . . . ? C12 Re1 P1 C13 108.8(2) . . . . ? C9 Re1 P1 C13 -75.7(2) . . . . ? C1 Re1 P1 C13 -166.97(19) . . . . ? C10 Re1 P1 C14 116.4(16) . . . . ? C11 Re1 P1 C14 -103.7(2) . . . . ? C12 Re1 P1 C14 -10.5(2) . . . . ? C9 Re1 P1 C14 165.0(2) . . . . ? C1 Re1 P1 C14 73.7(2) . . . . ? C10 Re1 P1 C15 -4.8(16) . . . . ? C11 Re1 P1 C15 135.05(19) . . . . ? C12 Re1 P1 C15 -131.76(19) . . . . ? C9 Re1 P1 C15 43.8(2) . . . . ? C1 Re1 P1 C15 -47.50(19) . . . . ? C18 Re2 P2 C19 -78.44(19) . . . . ? C16 Re2 P2 C19 37(3) . . . . ? C17 Re2 P2 C19 13.42(19) . . . . ? P3 Re2 P2 C19 -169.69(16) . . . . ? S Re2 P2 C19 108.17(16) . . . . ? C18 Re2 P2 C21 39.31(19) . . . . ? C16 Re2 P2 C21 154(3) . . . . ? C17 Re2 P2 C21 131.17(19) . . . . ? P3 Re2 P2 C21 -51.94(17) . . . . ? S Re2 P2 C21 -134.08(17) . . . . ? C18 Re2 P2 C20 162.71(19) . . . . ? C16 Re2 P2 C20 -82(3) . . . . ? C17 Re2 P2 C20 -105.44(19) . . . . ? P3 Re2 P2 C20 71.45(16) . . . . ? S Re2 P2 C20 -10.69(16) . . . . ? C18 Re2 P3 C24 116.49(17) . . . . ? C16 Re2 P3 C24 22.87(17) . . . . ? C17 Re2 P3 C24 -14.0(12) . . . . ? P2 Re2 P3 C24 -156.35(14) . . . . ? S Re2 P3 C24 -72.55(14) . . . . ? C18 Re2 P3 C23 -124.90(17) . . . . ? C16 Re2 P3 C23 141.48(17) . . . . ? C17 Re2 P3 C23 104.6(12) . . . . ? P2 Re2 P3 C23 -37.74(14) . . . . ? S Re2 P3 C23 46.07(14) . . . . ? C18 Re2 P3 C22 -0.66(17) . . . . ? C16 Re2 P3 C22 -94.28(17) . . . . ? C17 Re2 P3 C22 -131.1(12) . . . . ? P2 Re2 P3 C22 86.50(14) . . . . ? S Re2 P3 C22 170.31(14) . . . . ? C10 Re1 C1 C2 -69.9(3) . . . . ? C11 Re1 C1 C2 130.6(11) . . . . ? C12 Re1 C1 C2 -162.1(4) . . . . ? C9 Re1 C1 C2 21.4(4) . . . . ? P1 Re1 C1 C2 107.7(3) . . . . ? Re1 C1 C2 C3 7.5(6) . . . . ? C1 C2 C3 C4 51.3(5) . . . . ? C1 C2 C3 C8 -130.2(4) . . . . ? C8 C3 C4 C5 1.9(5) . . . . ? C2 C3 C4 C5 -179.6(3) . . . . ? C3 C4 C5 C6 -0.7(6) . . . . ? C4 C5 C6 C7 -1.3(6) . . . . ? C5 C6 C7 C8 2.0(6) . . . . ? C6 C7 C8 C3 -0.8(5) . . . . ? C6 C7 C8 S 173.7(3) . . . . ? C4 C3 C8 C7 -1.1(5) . . . . ? C2 C3 C8 C7 -179.6(3) . . . . ? C4 C3 C8 S -175.9(2) . . . . ? C2 C3 C8 S 5.6(4) . . . . ? Re2 S C8 C7 47.3(3) . . . . ? Re2 S C8 C3 -138.1(2) . . . . ? C10 Re1 C9 O9 -127(7) . . . . ? C11 Re1 C9 O9 -35(7) . . . . ? C12 Re1 C9 O9 104(7) . . . . ? C1 Re1 C9 O9 138(7) . . . . ? P1 Re1 C9 O9 56(7) . . . . ? C11 Re1 C10 O10 -46(7) . . . . ? C12 Re1 C10 O10 -140(7) . . . . ? C9 Re1 C10 O10 45(7) . . . . ? C1 Re1 C10 O10 136(7) . . . . ? P1 Re1 C10 O10 93(7) . . . . ? C10 Re1 C11 O11 104(20) . . . . ? C12 Re1 C11 O11 -163(20) . . . . ? C9 Re1 C11 O11 13(20) . . . . ? C1 Re1 C11 O11 -96(20) . . . . ? P1 Re1 C11 O11 -73(20) . . . . ? C10 Re1 C12 O12 -116(5) . . . . ? C11 Re1 C12 O12 153(5) . . . . ? C9 Re1 C12 O12 14(6) . . . . ? C1 Re1 C12 O12 -21(5) . . . . ? P1 Re1 C12 O12 62(5) . . . . ? C18 Re2 C16 O16 -15(12) . . . . ? C17 Re2 C16 O16 -107(12) . . . . ? P3 Re2 C16 O16 76(12) . . . . ? P2 Re2 C16 O16 -130(11) . . . . ? S Re2 C16 O16 159(12) . . . . ? C18 Re2 C17 O17 -65(7) . . . . ? C16 Re2 C17 O17 29(7) . . . . ? P3 Re2 C17 O17 65(8) . . . . ? P2 Re2 C17 O17 -152(7) . . . . ? S Re2 C17 O17 123(7) . . . . ? C16 Re2 C18 O18 158(6) . . . . ? C17 Re2 C18 O18 -112(6) . . . . ? P3 Re2 C18 O18 72(6) . . . . ? P2 Re2 C18 O18 -23(6) . . . . ? S Re2 C18 O18 15(7) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.886 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.129