Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'J. D. G. Correia' 'Angela Domingos' 'Isabel Santos' 'Hartmut Spies' _publ_contact_author_name 'Prof Isabel Santos' _publ_contact_author_address ; Prof Isabel Santos Departamento de Quimica ITN Estrada Nacional 10 2686-953 Sacavem Codex PORTUGAL ; _publ_contact_author_email 'isantos@itn.pt' data_relsph _database_code_CSD 158068 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [Re(O)(k3-PNO)(SC6H5)] _chemical_formula_analytical ? _chemical_formula_sum 'C27 H23 N O3 P Re S' _chemical_formula_weight 658.69 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' '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 9.2050(8) _cell_length_b 11.9708(10) _cell_length_c 24.627(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.989(10) _cell_angle_gamma 90.00 _cell_volume 2703.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.7 _cell_measurement_theta_max 14.0 _exptl_crystal_description 'irregular-plate' _exptl_crystal_colour 'brown-yellow' _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method ? _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 4.658 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.4287 _exptl_absorpt_correction_T_max 0.9998 _exptl_special_details ; Crystals were obtained by slow diffusion of hexane on a solution of the complex in dichloromethane ; _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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 6225 _diffrn_reflns_av_R_equivalents 0.1185 _diffrn_reflns_av_sigmaI/netI 0.0997 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.93 _reflns_number_total 5857 _reflns_number_observed 2987 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 software(Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software(Enraf-Nonius,1989)' _computing_data_reduction 'process-MolEN(Fair,1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP(Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1305 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^)+(0.0526P)^2^+38.3517P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4552 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1777 _refine_ls_R_factor_obs 0.0798 _refine_ls_wR_factor_all 0.2848 _refine_ls_wR_factor_obs 0.1547 _refine_ls_goodness_of_fit_all 1.182 _refine_ls_goodness_of_fit_obs 1.305 _refine_ls_restrained_S_all 1.706 _refine_ls_restrained_S_obs 1.305 _refine_ls_shift/esd_max 0.000 _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 0.05708(6) 0.25099(9) 0.22647(3) 0.0360(2) Uani 1 d . . S1 S -0.0498(5) 0.1196(4) 0.2781(2) 0.0423(10) Uani 1 d . . P1 P -0.1047(5) 0.1823(3) 0.1530(2) 0.0334(10) Uani 1 d . . O1 O 0.2158(13) 0.1985(10) 0.2148(6) 0.055(4) Uani 1 d . . O2 O 0.0706(14) 0.3482(9) 0.2897(5) 0.047(3) Uani 1 d . . O3 O -0.0504(15) 0.5254(11) 0.1217(6) 0.064(4) Uani 1 d . . N1 N 0.0137(14) 0.4006(12) 0.1879(6) 0.041(3) Uani 1 d . . C1 C 0.0039(22) 0.4958(16) 0.2276(9) 0.061(6) Uani 1 d . . H1A H -0.0959(22) 0.5056(16) 0.2366(9) 0.073 Uiso 1 calc R . H1B H 0.0367(22) 0.5649(16) 0.2121(9) 0.073 Uiso 1 calc R . C2 C 0.1020(25) 0.4641(16) 0.2780(8) 0.061(6) Uani 1 d . . H2A H 0.2036(25) 0.4727(16) 0.2712(8) 0.074 Uiso 1 calc R . H2B H 0.0821(25) 0.5113(16) 0.3085(8) 0.074 Uiso 1 calc R . C3 C -0.0129(19) 0.4287(15) 0.1361(9) 0.047(5) Uani 1 d . . C4 C 0.0138(18) 0.1267(13) 0.3457(7) 0.038(4) Uani 1 d . . C5 C 0.1610(18) 0.1480(16) 0.3621(8) 0.050(5) Uani 1 d . . H5 H 0.2259(18) 0.1629(16) 0.3361(8) 0.060 Uiso 1 calc R . C6 C 0.2093(27) 0.1467(18) 0.4164(10) 0.074(7) Uani 1 d . . H6 H 0.3064(27) 0.1644(18) 0.4262(10) 0.089 Uiso 1 calc R . C7 C 0.1231(29) 0.1211(20) 0.4568(9) 0.071(7) Uani 1 d . . H7 H 0.1602(29) 0.1196(20) 0.4931(9) 0.085 Uiso 1 calc R . C8 C -0.0214(28) 0.0974(20) 0.4417(11) 0.077(7) Uani 1 d . . H8 H -0.0841(28) 0.0774(20) 0.4678(11) 0.092 Uiso 1 calc R . C9 C -0.0704(23) 0.1037(17) 0.3880(8) 0.056(5) Uani 1 d . . H9 H -0.1693(23) 0.0914(17) 0.3791(8) 0.067 Uiso 1 calc R . C10 C -0.2856(16) 0.2342(15) 0.1505(7) 0.037(4) Uani 1 d . . C11 C -0.0313(16) 0.2314(15) 0.0928(6) 0.033(4) Uani 1 d . . C12 C -0.1134(21) 0.0320(14) 0.1471(8) 0.049(5) Uani 1 d . . C101 C -0.3717(20) 0.2474(25) 0.1020(8) 0.074(6) Uani 1 d . . H101 H -0.3342(20) 0.2260(25) 0.0697(8) 0.089 Uiso 1 calc R . C102 C -0.5116(23) 0.2914(24) 0.0996(10) 0.089(10) Uani 1 d . . H102 H -0.5677(23) 0.2971(24) 0.0664(10) 0.107 Uiso 1 calc R . C103 C -0.5636(21) 0.3251(18) 0.1453(10) 0.061(6) Uani 1 d . . H103 H -0.6576(21) 0.3539(18) 0.1443(10) 0.073 Uiso 1 calc R . C104 C -0.4854(22) 0.3181(22) 0.1909(10) 0.076(7) Uani 1 d . . H104 H -0.5229(22) 0.3433(22) 0.2226(10) 0.091 Uiso 1 calc R . C105 C -0.3457(19) 0.2737(13) 0.1938(7) 0.046(5) Uani 1 d . . H105 H -0.2917(19) 0.2713(13) 0.2275(7) 0.056 Uiso 1 calc R . C111 C 0.0121(17) 0.3454(15) 0.0920(9) 0.046(5) Uani 1 d . . C112 C 0.0643(19) 0.3825(17) 0.0432(9) 0.051(5) Uani 1 d . . H112 H 0.0835(19) 0.4586(17) 0.0409(9) 0.062 Uiso 1 calc R . C113 C 0.0892(19) 0.3214(18) 0.0003(8) 0.049(5) Uani 1 d . . H113 H 0.1347(19) 0.3496(18) -0.0291(8) 0.059 Uiso 1 calc R . C114 C 0.0426(21) 0.2135(16) 0.0026(8) 0.049(5) Uani 1 d . . H114 H 0.0502(21) 0.1675(16) -0.0275(8) 0.059 Uiso 1 calc R . C115 C -0.0151(22) 0.1700(18) 0.0477(8) 0.057(5) Uani 1 d . . H115 H -0.0441(22) 0.0955(18) 0.0471(8) 0.068 Uiso 1 calc R . C121 C 0.0181(25) -0.0267(17) 0.1466(9) 0.062(6) Uani 1 d . . H121 H 0.1059(25) 0.0111(17) 0.1450(9) 0.075 Uiso 1 calc R . C122 C 0.0145(30) -0.1427(18) 0.1485(9) 0.074(7) Uani 1 d . . H122 H 0.1011(30) -0.1828(18) 0.1490(9) 0.089 Uiso 1 calc R . C123 C -0.1111(35) -0.1971(16) 0.1495(9) 0.081(9) Uani 1 d . . H123 H -0.1108(35) -0.2748(16) 0.1500(9) 0.097 Uiso 1 calc R . C124 C -0.2384(31) -0.1424(18) 0.1499(11) 0.077(8) Uani 1 d . . H124 H -0.3248(31) -0.1825(18) 0.1504(11) 0.093 Uiso 1 calc R . C125 C -0.2419(23) -0.0259(17) 0.1495(9) 0.058(5) Uani 1 d . . H125 H -0.3297(23) 0.0121(17) 0.1508(9) 0.070 Uiso 1 calc R . C1S C 0.6044(40) 0.9280(33) 0.0101(16) 0.128(12) Uiso 1 d . . C2S C 0.4546(88) 0.9431(65) 0.0329(28) 0.289(37) Uiso 1 d . . C3S C 0.3430(57) 0.9766(47) 0.0513(21) 0.192(21) Uiso 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 0.0421(3) 0.0271(3) 0.0379(3) 0.0066(5) -0.0012(2) -0.0039(5) S1 0.050(2) 0.032(2) 0.044(3) 0.011(2) -0.004(2) -0.010(2) P1 0.044(2) 0.020(2) 0.036(2) 0.001(2) 0.002(2) -0.003(2) O1 0.043(7) 0.034(7) 0.087(11) -0.013(7) -0.001(7) -0.005(6) O2 0.071(8) 0.027(6) 0.044(7) -0.008(6) 0.010(6) -0.019(6) O3 0.072(9) 0.040(8) 0.081(12) 0.029(8) 0.015(8) 0.017(7) N1 0.039(8) 0.040(8) 0.043(9) 0.011(7) 0.000(6) -0.005(7) C1 0.069(13) 0.032(10) 0.082(17) 0.010(11) 0.011(12) 0.005(9) C2 0.100(16) 0.032(10) 0.048(12) 0.001(9) -0.011(11) -0.028(11) C3 0.041(10) 0.030(9) 0.067(14) 0.011(10) -0.008(9) -0.009(8) C4 0.050(10) 0.018(8) 0.045(10) 0.003(7) 0.007(8) 0.009(7) C5 0.037(9) 0.051(12) 0.063(13) 0.014(10) 0.000(9) -0.003(8) C6 0.101(18) 0.044(13) 0.068(16) 0.012(12) -0.042(14) 0.013(12) C7 0.112(20) 0.071(16) 0.030(11) 0.014(11) 0.005(12) 0.008(15) C8 0.092(18) 0.061(15) 0.084(19) 0.032(14) 0.041(15) 0.011(13) C9 0.069(13) 0.054(13) 0.046(12) 0.014(11) 0.013(10) 0.000(11) C10 0.036(7) 0.029(11) 0.045(9) 0.000(8) 0.006(6) -0.011(8) C11 0.039(8) 0.038(13) 0.022(7) 0.000(8) 0.006(6) 0.003(8) C12 0.060(12) 0.021(9) 0.061(13) 0.014(9) -0.015(10) -0.012(8) C101 0.066(12) 0.098(17) 0.058(12) 0.033(20) 0.004(9) -0.003(18) C102 0.055(13) 0.137(28) 0.071(16) 0.048(17) -0.023(11) 0.019(14) C103 0.044(11) 0.055(13) 0.085(18) 0.004(13) 0.009(11) 0.004(10) C104 0.047(12) 0.113(21) 0.067(16) 0.020(15) 0.005(11) -0.005(13) C105 0.057(10) 0.035(13) 0.046(10) -0.018(8) -0.004(8) 0.010(8) C111 0.032(9) 0.036(10) 0.069(14) 0.024(10) 0.001(9) -0.002(8) C112 0.042(10) 0.043(11) 0.068(15) 0.010(11) -0.001(9) 0.000(9) C113 0.042(11) 0.063(15) 0.043(12) 0.015(11) 0.009(9) -0.025(10) C114 0.065(13) 0.043(11) 0.038(11) -0.013(8) 0.002(10) 0.022(9) C115 0.079(14) 0.051(13) 0.039(12) 0.001(10) 0.001(10) 0.013(11) C121 0.078(15) 0.036(11) 0.068(16) 0.005(11) -0.021(12) -0.002(11) C122 0.134(22) 0.044(13) 0.041(13) 0.003(10) -0.008(13) 0.021(14) C123 0.174(28) 0.010(9) 0.059(15) -0.010(10) 0.013(17) -0.032(15) C124 0.116(20) 0.027(11) 0.092(20) -0.011(12) 0.030(16) -0.038(13) C125 0.067(13) 0.039(11) 0.071(15) 0.008(11) 0.016(11) -0.007(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 O1 1.638(12) . ? Re1 O2 1.940(12) . ? Re1 N1 2.051(14) . ? Re1 S1 2.296(4) . ? Re1 P1 2.387(4) . ? S1 C4 1.72(2) . ? P1 C10 1.77(2) . ? P1 C11 1.782(15) . ? P1 C12 1.81(2) . ? O2 C2 1.45(2) . ? O3 C3 1.25(2) . ? N1 C3 1.32(2) . ? N1 C1 1.51(2) . ? C1 C2 1.52(3) . ? C3 C111 1.51(3) . ? C4 C9 1.38(2) . ? C4 C5 1.40(2) . ? C5 C6 1.37(3) . ? C6 C7 1.36(3) . ? C7 C8 1.38(3) . ? C8 C9 1.36(3) . ? C10 C105 1.33(2) . ? C10 C101 1.38(2) . ? C11 C115 1.35(2) . ? C11 C111 1.42(2) . ? C12 C125 1.38(2) . ? C12 C121 1.40(3) . ? C101 C102 1.39(3) . ? C102 C103 1.32(3) . ? C103 C104 1.28(3) . ? C104 C105 1.39(3) . ? C111 C112 1.40(3) . ? C112 C113 1.32(3) . ? C113 C114 1.36(3) . ? C114 C115 1.37(3) . ? C121 C122 1.39(3) . ? C122 C123 1.33(3) . ? C123 C124 1.34(3) . ? C124 C125 1.40(3) . ? C1S C2S 1.54(7) . ? C1S C2S 1.92(7) 3_675 ? C1S C3S 1.99(6) 3_675 ? C2S C3S 1.23(8) . ? C2S C1S 1.92(7) 3_675 ? C3S C1S 1.99(6) 3_675 ? 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 O1 Re1 O2 112.0(6) . . ? O1 Re1 N1 113.2(6) . . ? O2 Re1 N1 81.1(6) . . ? O1 Re1 S1 105.4(5) . . ? O2 Re1 S1 88.1(4) . . ? N1 Re1 S1 141.2(4) . . ? O1 Re1 P1 104.0(5) . . ? O2 Re1 P1 143.9(4) . . ? N1 Re1 P1 82.3(4) . . ? S1 Re1 P1 85.1(2) . . ? C4 S1 Re1 112.1(6) . . ? C10 P1 C11 106.2(8) . . ? C10 P1 C12 108.2(9) . . ? C11 P1 C12 106.2(9) . . ? C10 P1 Re1 115.3(6) . . ? C11 P1 Re1 105.1(5) . . ? C12 P1 Re1 115.1(6) . . ? C2 O2 Re1 114.4(11) . . ? C3 N1 C1 114.7(15) . . ? C3 N1 Re1 133.0(13) . . ? C1 N1 Re1 112.3(11) . . ? N1 C1 C2 106.0(15) . . ? O2 C2 C1 106.7(15) . . ? O3 C3 N1 122.2(20) . . ? O3 C3 C111 117.7(18) . . ? N1 C3 C111 120.0(16) . . ? C9 C4 C5 114.3(18) . . ? C9 C4 S1 123.7(15) . . ? C5 C4 S1 121.8(14) . . ? C6 C5 C4 120.0(20) . . ? C7 C6 C5 123.7(22) . . ? C6 C7 C8 117.5(21) . . ? C9 C8 C7 118.6(21) . . ? C8 C9 C4 125.8(21) . . ? C105 C10 C101 113.9(17) . . ? C105 C10 P1 123.4(13) . . ? C101 C10 P1 122.4(15) . . ? C115 C11 C111 117.3(17) . . ? C115 C11 P1 125.5(15) . . ? C111 C11 P1 117.1(13) . . ? C125 C12 C121 119.6(17) . . ? C125 C12 P1 122.0(16) . . ? C121 C12 P1 117.9(14) . . ? C10 C101 C102 122.7(21) . . ? C103 C102 C101 118.8(20) . . ? C104 C103 C102 120.5(21) . . ? C103 C104 C105 121.1(23) . . ? C10 C105 C104 122.8(18) . . ? C112 C111 C11 115.7(19) . . ? C112 C111 C3 119.5(17) . . ? C11 C111 C3 124.3(16) . . ? C113 C112 C111 127.2(20) . . ? C112 C113 C114 114.4(19) . . ? C113 C114 C115 122.5(20) . . ? C11 C115 C114 122.4(20) . . ? C122 C121 C12 118.5(22) . . ? C123 C122 C121 120.9(24) . . ? C122 C123 C124 121.5(19) . . ? C123 C124 C125 120.4(21) . . ? C12 C125 C124 119.0(21) . . ? C2S C1S C2S 83.6(44) . 3_675 ? C2S C1S C3S 119.6(43) . 3_675 ? C2S C1S C3S 36.5(25) 3_675 3_675 ? C3S C2S C1S 167.6(80) . . ? C3S C2S C1S 74.6(52) . 3_675 ? C1S C2S C1S 96.4(44) . 3_675 ? C2S C3S C1S 68.9(46) . 3_675 ? _refine_diff_density_max 1.815 _refine_diff_density_min -1.768 _refine_diff_density_rms 0.211 #===END data_reopnssph _database_code_CSD 158069 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [Re(O)(k3-PNS)(SC6H5)].0.5C6H14 _chemical_formula_analytical ? _chemical_formula_sum 'C30 H30 N O2 P Re S2' _chemical_formula_weight 717.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' '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 9.4660(9) _cell_length_b 11.9835(10) _cell_length_c 24.510(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.612(9) _cell_angle_gamma 90.00 _cell_volume 2755.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.4 _cell_measurement_theta_max 12.0 _exptl_crystal_description irregular _exptl_crystal_colour 'brown-orange' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method ? _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 4.648 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.9109 _exptl_absorpt_correction_T_max 0.9998 _exptl_special_details ; Crystals were obtained by layering a solution of the complex in dichoromethane with hexane ' ; _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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 6392 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.1377 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.09 _reflns_number_total 6026 _reflns_number_observed 3258 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 software(Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software(Enraf-Nonius,1989)' _computing_data_reduction 'process-MolEN(Fair,1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP(Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1006 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^)+(0.0432P)^2^+33.2212P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5020 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1793 _refine_ls_R_factor_obs 0.0844 _refine_ls_wR_factor_all 0.2886 _refine_ls_wR_factor_obs 0.1402 _refine_ls_goodness_of_fit_all 1.089 _refine_ls_goodness_of_fit_obs 1.172 _refine_ls_restrained_S_all 1.775 _refine_ls_restrained_S_obs 1.172 _refine_ls_shift/esd_max 0.000 _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 0.06331(7) 0.23685(4) 0.22836(3) 0.0377(2) Uani 1 d . . P1 P -0.0985(5) 0.3165(3) 0.1544(2) 0.0388(10) Uani 1 d . . S1 S -0.0202(5) 0.3834(3) 0.2760(2) 0.0508(12) Uani 1 d . . S2 S 0.0707(5) 0.1289(3) 0.3050(2) 0.0543(12) Uani 1 d . . O1 O 0.2248(12) 0.2688(9) 0.2164(5) 0.061(3) Uani 1 d . . O2 O -0.0733(14) -0.0196(9) 0.1158(6) 0.066(4) Uani 1 d . . N1 N -0.0053(13) 0.0905(10) 0.1885(6) 0.042(3) Uani 1 d . . C1 C 0.0767(17) -0.0074(9) 0.2766(6) 0.069(6) Uani 1 d . . H1A H 0.1730(17) -0.0247(9) 0.2698(6) 0.082 Uiso 1 calc R . H1B H 0.0482(17) -0.0621(9) 0.3021(6) 0.082 Uiso 1 calc R . C2 C -0.0241(17) -0.0112(9) 0.2230(6) 0.071(6) Uani 1 d R . H2A H -0.0055(17) -0.0778(9) 0.2026(6) 0.085 Uiso 1 calc R . H2B H -0.1217(17) -0.0147(9) 0.2309(6) 0.085 Uiso 1 calc R . C3 C -0.0280(17) 0.0694(12) 0.1351(8) 0.044(4) Uani 1 d . . C4 C 0.0307(19) 0.3759(12) 0.3465(7) 0.045(4) Uani 1 d . . C5 C -0.0621(21) 0.3966(14) 0.3835(9) 0.057(5) Uani 1 d . . H5 H -0.1566(21) 0.4104(14) 0.3694(9) 0.069 Uiso 1 calc R . C6 C -0.0276(32) 0.3989(19) 0.4388(12) 0.093(8) Uani 1 d . . H6 H -0.0972(32) 0.4111(19) 0.4616(12) 0.112 Uiso 1 calc R . C7 C 0.1199(45) 0.3818(21) 0.4618(12) 0.119(13) Uani 1 d . . H7 H 0.1492(45) 0.3840(21) 0.4995(12) 0.143 Uiso 1 calc R . C8 C 0.2118(32) 0.3627(16) 0.4257(11) 0.098(10) Uani 1 d . . H8 H 0.3070(32) 0.3516(16) 0.4397(11) 0.118 Uiso 1 calc R . C9 C 0.1759(19) 0.3583(13) 0.3706(9) 0.064(6) Uani 1 d . . H9 H 0.2455(19) 0.3439(13) 0.3481(9) 0.077 Uiso 1 calc R . C10 C -0.2785(16) 0.2644(13) 0.1492(7) 0.042(4) Uani 1 d . . C11 C -0.0316(16) 0.2675(14) 0.0934(7) 0.045(4) Uani 1 d . . C12 C -0.1046(16) 0.4672(11) 0.1503(6) 0.032(3) Uani 1 d . . C101 C -0.3619(19) 0.2588(18) 0.1005(8) 0.071(5) Uani 1 d . . H101 H -0.3285(19) 0.2834(18) 0.0685(8) 0.086 Uiso 1 calc R . C102 C -0.4996(23) 0.2154(20) 0.0985(9) 0.081(7) Uani 1 d . . H102 H -0.5568(23) 0.2107(20) 0.0646(9) 0.098 Uiso 1 calc R . C103 C -0.5514(20) 0.1808(16) 0.1434(10) 0.066(6) Uani 1 d . . H103 H -0.6440(20) 0.1534(16) 0.1405(10) 0.079 Uiso 1 calc R . C104 C -0.4698(22) 0.1849(15) 0.1942(10) 0.074(6) Uani 1 d . . H104 H -0.5054(22) 0.1601(15) 0.2256(10) 0.089 Uiso 1 calc R . C105 C -0.3313(16) 0.2276(13) 0.1970(7) 0.050(4) Uani 1 d . . H105 H -0.2738(16) 0.2317(13) 0.2307(7) 0.060 Uiso 1 calc R . C111 C 0.0047(18) 0.1545(13) 0.0933(7) 0.047(4) Uani 1 d . . C112 C 0.0640(19) 0.1170(17) 0.0474(8) 0.061(5) Uani 1 d . . H112 H 0.0882(19) 0.0420(17) 0.0457(8) 0.073 Uiso 1 calc R . C113 C 0.0887(24) 0.1862(21) 0.0043(9) 0.077(7) Uani 1 d . . H113 H 0.1284(24) 0.1577(21) -0.0255(9) 0.092 Uiso 1 calc R . C114 C 0.0544(27) 0.2954(17) 0.0062(10) 0.082(8) Uani 1 d . . H114 H 0.0691(27) 0.3436(17) -0.0222(10) 0.099 Uiso 1 calc R . C115 C -0.0028(21) 0.3331(15) 0.0514(8) 0.059(5) Uani 1 d . . H115 H -0.0230(21) 0.4088(15) 0.0532(8) 0.071 Uiso 1 calc R . C121 C -0.2290(20) 0.5254(13) 0.1446(9) 0.065(6) Uani 1 d . . H121 H -0.3159(20) 0.4884(13) 0.1428(9) 0.078 Uiso 1 calc R . C122 C -0.2240(22) 0.6417(15) 0.1416(9) 0.074(7) Uani 1 d . . H122 H -0.3082(22) 0.6824(15) 0.1389(9) 0.088 Uiso 1 calc R . C123 C -0.1002(25) 0.6953(16) 0.1424(8) 0.068(6) Uani 1 d . . H123 H -0.1003(25) 0.7726(16) 0.1388(8) 0.081 Uiso 1 calc R . C124 C 0.0257(22) 0.6399(14) 0.1483(8) 0.067(6) Uani 1 d . . H124 H 0.1117(22) 0.6781(14) 0.1502(8) 0.080 Uiso 1 calc R . C125 C 0.0222(19) 0.5240(13) 0.1515(9) 0.066(6) Uani 1 d . . H125 H 0.1072(19) 0.4841(13) 0.1546(9) 0.079 Uiso 1 calc R . C1S C 0.4287(35) 0.4665(29) 0.0008(15) 0.135(12) Uiso 1 d . . C2S C 0.4260(68) 0.5522(51) 0.0373(23) 0.254(26) Uiso 1 d . . C3S C 0.3057(45) 0.5220(34) 0.0404(16) 0.166(15) Uiso 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 0.0358(3) 0.0214(3) 0.0560(4) -0.0063(3) 0.0062(2) -0.0004(3) P1 0.041(2) 0.028(2) 0.048(3) -0.006(2) 0.009(2) 0.001(2) S1 0.060(3) 0.036(2) 0.054(3) -0.012(2) -0.003(2) 0.015(2) S2 0.054(3) 0.034(2) 0.073(3) 0.005(2) -0.001(3) 0.002(2) O1 0.063(7) 0.043(6) 0.078(8) -0.019(7) 0.014(6) -0.010(6) O2 0.077(9) 0.030(6) 0.090(10) -0.018(6) 0.011(8) -0.016(6) N1 0.032(7) 0.041(7) 0.054(9) -0.017(7) 0.010(7) -0.002(6) C1 0.102(17) 0.034(9) 0.064(14) 0.009(9) -0.010(12) 0.014(10) C2 0.108(18) 0.023(8) 0.082(16) 0.001(9) 0.011(13) -0.013(10) C3 0.036(9) 0.026(7) 0.077(14) -0.004(8) 0.031(9) -0.002(7) C4 0.067(12) 0.027(7) 0.039(10) -0.011(7) 0.003(9) -0.005(8) C5 0.066(13) 0.043(10) 0.064(14) -0.017(10) 0.016(11) -0.013(9) C6 0.114(23) 0.074(16) 0.098(23) -0.010(15) 0.040(19) -0.019(16) C7 0.236(43) 0.066(16) 0.062(19) -0.008(14) 0.047(25) -0.032(22) C8 0.139(25) 0.044(11) 0.090(19) -0.011(12) -0.068(19) -0.022(14) C9 0.049(11) 0.034(9) 0.101(17) -0.021(10) -0.024(11) -0.008(8) C10 0.043(8) 0.033(8) 0.053(10) -0.008(8) 0.013(8) 0.003(8) C11 0.040(8) 0.046(9) 0.051(10) -0.008(9) 0.015(7) -0.003(8) C12 0.037(9) 0.028(7) 0.031(9) -0.004(6) 0.009(7) -0.013(6) C101 0.058(11) 0.085(15) 0.070(13) -0.019(13) 0.007(10) -0.013(13) C102 0.067(14) 0.116(19) 0.059(14) -0.051(14) -0.001(11) -0.012(13) C103 0.038(11) 0.064(12) 0.092(17) -0.029(12) 0.000(12) -0.016(9) C104 0.062(14) 0.053(11) 0.111(19) 0.001(12) 0.030(14) 0.008(10) C105 0.034(8) 0.043(9) 0.073(12) -0.002(9) 0.002(8) 0.001(8) C111 0.050(11) 0.039(9) 0.053(12) -0.008(8) 0.008(9) 0.005(8) C112 0.055(12) 0.069(12) 0.056(14) -0.024(11) -0.001(10) 0.015(10) C113 0.074(15) 0.109(18) 0.053(15) -0.010(13) 0.030(12) -0.020(14) C114 0.125(22) 0.054(13) 0.073(17) 0.001(11) 0.035(16) -0.013(13) C115 0.079(15) 0.054(11) 0.048(13) -0.016(9) 0.020(11) 0.013(10) C121 0.058(12) 0.032(9) 0.108(18) -0.015(10) 0.025(12) 0.006(8) C122 0.060(13) 0.041(10) 0.124(20) 0.015(11) 0.026(13) 0.025(10) C123 0.095(17) 0.048(11) 0.063(14) 0.013(10) 0.020(13) -0.002(11) C124 0.067(14) 0.042(10) 0.090(17) 0.012(10) 0.008(12) -0.023(10) C125 0.041(11) 0.029(8) 0.123(19) 0.007(10) -0.004(11) 0.007(8) _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 O1 1.639(11) . ? Re1 N1 2.070(12) . ? Re1 S2 2.273(5) . ? Re1 S1 2.305(4) . ? Re1 P1 2.410(4) . ? P1 C11 1.80(2) . ? P1 C10 1.80(2) . ? P1 C12 1.809(14) . ? S1 C4 1.73(2) . ? S2 C1 1.780(12) . ? O2 C3 1.22(2) . ? N1 C3 1.32(2) . ? N1 C2 1.51(2) . ? C1 C2 1.52 . ? C3 C111 1.51(2) . ? C4 C5 1.37(2) . ? C4 C9 1.44(2) . ? C5 C6 1.35(3) . ? C6 C7 1.45(4) . ? C7 C8 1.34(4) . ? C8 C9 1.35(3) . ? C10 C101 1.34(2) . ? C10 C105 1.40(2) . ? C11 C115 1.35(2) . ? C11 C111 1.40(2) . ? C12 C121 1.36(2) . ? C12 C125 1.38(2) . ? C101 C102 1.40(3) . ? C102 C103 1.33(3) . ? C103 C104 1.38(3) . ? C104 C105 1.40(2) . ? C111 C112 1.40(2) . ? C112 C113 1.39(3) . ? C113 C114 1.35(3) . ? C114 C115 1.37(3) . ? C121 C122 1.40(2) . ? C122 C123 1.33(3) . ? C123 C124 1.36(3) . ? C124 C125 1.39(2) . ? C1S C2S 1.37(6) . ? C1S C1S 1.58(6) 3_665 ? C1S C3S 1.74(5) . ? C1S C2S 1.78(6) 3_665 ? C2S C3S 1.21(6) . ? C2S C1S 1.78(6) 3_665 ? 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 O1 Re1 N1 110.8(5) . . ? O1 Re1 S2 110.7(4) . . ? N1 Re1 S2 83.2(4) . . ? O1 Re1 S1 107.6(4) . . ? N1 Re1 S1 141.0(4) . . ? S2 Re1 S1 89.5(2) . . ? O1 Re1 P1 106.7(4) . . ? N1 Re1 P1 81.5(4) . . ? S2 Re1 P1 142.5(2) . . ? S1 Re1 P1 81.51(15) . . ? C11 P1 C10 105.1(7) . . ? C11 P1 C12 107.0(7) . . ? C10 P1 C12 108.6(7) . . ? C11 P1 Re1 103.7(6) . . ? C10 P1 Re1 114.6(6) . . ? C12 P1 Re1 116.7(5) . . ? C4 S1 Re1 113.4(6) . . ? C1 S2 Re1 101.4(5) . . ? C3 N1 C2 112.6(12) . . ? C3 N1 Re1 129.0(11) . . ? C2 N1 Re1 118.3(9) . . ? C2 C1 S2 108.5(5) . . ? N1 C2 C1 110.7(8) . . ? O2 C3 N1 123.7(16) . . ? O2 C3 C111 114.8(17) . . ? N1 C3 C111 121.5(14) . . ? C5 C4 C9 114.7(17) . . ? C5 C4 S1 122.2(15) . . ? C9 C4 S1 122.8(15) . . ? C6 C5 C4 125.3(22) . . ? C5 C6 C7 118.6(25) . . ? C8 C7 C6 116.4(28) . . ? C7 C8 C9 124.6(28) . . ? C8 C9 C4 120.4(22) . . ? C101 C10 C105 119.6(15) . . ? C101 C10 P1 121.3(13) . . ? C105 C10 P1 119.1(12) . . ? C115 C11 C111 119.3(16) . . ? C115 C11 P1 124.9(13) . . ? C111 C11 P1 115.5(13) . . ? C121 C12 C125 119.4(14) . . ? C121 C12 P1 122.6(12) . . ? C125 C12 P1 118.1(12) . . ? C10 C101 C102 119.0(19) . . ? C103 C102 C101 122.1(20) . . ? C102 C103 C104 120.9(19) . . ? C103 C104 C105 117.8(20) . . ? C104 C105 C10 120.5(17) . . ? C11 C111 C112 115.9(17) . . ? C11 C111 C3 125.7(15) . . ? C112 C111 C3 118.1(15) . . ? C113 C112 C111 123.2(19) . . ? C114 C113 C112 119.1(22) . . ? C113 C114 C115 118.0(22) . . ? C11 C115 C114 124.3(17) . . ? C12 C121 C122 118.8(17) . . ? C123 C122 C121 121.1(18) . . ? C122 C123 C124 121.6(18) . . ? C123 C124 C125 117.9(18) . . ? C12 C125 C124 121.3(17) . . ? C2S C1S C1S 73.9(34) . 3_665 ? C2S C1S C3S 43.6(32) . . ? C1S C1S C3S 117.2(36) 3_665 . ? C2S C1S C2S 121.5(36) . 3_665 ? C1S C1S C2S 47.6(24) 3_665 3_665 ? C3S C1S C2S 164.1(37) . 3_665 ? C3S C2S C1S 85.0(48) . . ? C3S C2S C1S 142.9(59) . 3_665 ? C1S C2S C1S 58.5(36) . 3_665 ? C2S C3S C1S 51.3(33) . . ? _refine_diff_density_max 2.655 _refine_diff_density_min -1.659 _refine_diff_density_rms 0.218 _eof # End of Crystallografic Information File