Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Daniel Miguel' _publ_contact_author_address ; Departamento de Quimica Inorganica Universidad de Valladolid Facultad de Ciencias Prado de la Magdalena s/n Valladolid E-47005 SPAIN ; _publ_contact_author_phone +34-983-184096 _publ_contact_author_fax +34-983-423013 _publ_contact_author_email dmsj@qi.uva.es _publ_section_title ; Building of dithiocarbamate and dithiocarbimate ligands within a heterobimetallic core ; loop_ _publ_author_name _publ_author_address 'Jing Li' ; State Key Laboratory of Elemento-Organic Chemistry. Nankai University 300071 Tianjin CHINA RP ; 'Daniel Miguel' ; Departamento de Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Dolores Morales' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Quimica Universidad de Oviedo C/ Julian Claveria s/n 33071 Oviedo (ASTURIAS) SPAIN ; 'Victor Riera' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Quimica Universidad de Oviedo C/ Julian Claveria s/n 33071 Oviedo (ASTURIAS) SPAIN ; 'Angel Aguirre-Perez' ; Departamento de Quimica Fisica y Analitica Facultad de Quimica Universidad de Oviedo C/ Julian Claveria s/n 33071 Oviedo (ASTURIAS) SPAIN ; ; S.Garcia-Granda ; ; Departamento de Quimica Fisica y Analitica Facultad de Quimica Universidad de Oviedo C/ Julian Claveria s/n 33071 Oviedo (ASTURIAS) SPAIN ; #-------------------------- data section of block --------------------------- data_Compound_3a(mrdtc) _database_code_CSD 208877 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H28 Mn N O6 P Re S3' _chemical_formula_sum 'C19 H28 Mn N O6 P Re S3' _chemical_formula_weight 734.71 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' Mn Mn 0.3368 0.7283 '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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3336(16) _cell_length_b 10.872(2) _cell_length_c 15.337(4) _cell_angle_alpha 72.04(3) _cell_angle_beta 86.19(2) _cell_angle_gamma 65.948(18) _cell_volume 1348.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.96 _cell_measurement_theta_max 18.88 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 5.275 _exptl_absorpt_correction_type 'empirical psi-scan' _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _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 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '1 h' _diffrn_standards_decay_% 2.89 _diffrn_reflns_number 5145 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.0891 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4722 _reflns_number_gt 2668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'CRYSDA (Beurskens et al, 1992)' _computing_data_reduction 'DATAR (local program)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1998)' _computing_publication_material 'SHELXTL (Sheldrick, 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^)+(0.0681P)^2^+1.7822P] 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 4722 _refine_ls_number_parameters 259 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1510 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1957 _refine_ls_wR_factor_gt 0.1604 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.105 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.12654(8) 1.28371(7) 0.36418(5) 0.0464(3) Uani 1 1 d . . . Mn1 Mn 0.2401(2) 1.2156(2) 0.14608(13) 0.0339(5) Uani 1 1 d . . . S1 S 0.3291(4) 1.1045(4) 0.2989(3) 0.0399(8) Uani 1 1 d . . . S2 S -0.0053(5) 1.3621(4) 0.2076(3) 0.0448(9) Uani 1 1 d . . . S3 S -0.0663(5) 1.1773(5) 0.3704(3) 0.0524(10) Uani 1 1 d . . . N1 N -0.2227(16) 1.2560(16) 0.2108(9) 0.059(4) Uani 1 1 d . . . C1 C 0.2368(18) 1.0311(15) 0.2425(9) 0.043(3) Uani 1 1 d . . . H1 H 0.1298 1.0526 0.2626 0.052 Uiso 1 1 calc R . . C2 C -0.1155(17) 1.2634(14) 0.2576(10) 0.044(4) Uani 1 1 d . . . C3 C 0.261(2) 1.3754(19) 0.3427(13) 0.063(5) Uani 1 1 d . . . O3 O 0.3482(18) 1.4326(15) 0.3275(12) 0.098(5) Uani 1 1 d . . . C11 C -0.260(2) 1.330(3) 0.1097(11) 0.088(7) Uani 1 1 d . . . H11A H -0.1832 1.3670 0.0853 0.132 Uiso 1 1 calc R . . H11B H -0.3626 1.4066 0.0995 0.132 Uiso 1 1 calc R . . H11C H -0.2586 1.2644 0.0794 0.132 Uiso 1 1 calc R . . C4 C 0.2171(19) 1.186(2) 0.4878(13) 0.057(5) Uani 1 1 d . . . O4 O 0.2652(17) 1.1254(16) 0.5629(9) 0.085(4) Uani 1 1 d . . . C12 C -0.310(2) 1.174(2) 0.2547(13) 0.074(6) Uani 1 1 d . . . H12A H -0.3158 1.1204 0.2170 0.112 Uiso 1 1 calc R . . H12B H -0.4139 1.2366 0.2631 0.112 Uiso 1 1 calc R . . H12C H -0.2578 1.1112 0.3133 0.112 Uiso 1 1 calc R . . C5 C -0.030(2) 1.437(2) 0.4009(13) 0.068(5) Uani 1 1 d . . . O5 O -0.1181(18) 1.5252(17) 0.4230(11) 0.107(6) Uani 1 1 d . . . C6 C 0.270(2) 1.3753(19) 0.1100(11) 0.058(4) Uani 1 1 d . . . O6 O 0.3006(17) 1.4734(13) 0.0922(10) 0.088(5) Uani 1 1 d . . . C7 C 0.417(2) 1.1384(17) 0.0964(12) 0.055(4) Uani 1 1 d . . . O7 O 0.5322(17) 1.1012(16) 0.0557(10) 0.090(4) Uani 1 1 d . . . C8 C 0.137(2) 1.246(2) 0.0405(12) 0.060(5) Uani 1 1 d . . . O8 O 0.0774(18) 1.2631(18) -0.0302(9) 0.097(5) Uani 1 1 d . . . P1 P 0.3271(5) 0.8509(4) 0.2533(3) 0.0510(11) Uani 1 1 d . . . C21 C 0.5091(13) 0.7988(13) 0.1973(12) 0.054(4) Uani 1 1 d D . . H21 H 0.4836 0.8634 0.1343 0.065 Uiso 1 1 calc R . . C22 C 0.6364(19) 0.8223(18) 0.2346(15) 0.078(6) Uani 1 1 d D . . H22A H 0.6866 0.7460 0.2895 0.117 Uiso 1 1 calc R . . H22B H 0.5919 0.9101 0.2486 0.117 Uiso 1 1 calc R . . H22C H 0.7125 0.8258 0.1897 0.117 Uiso 1 1 calc R . . C23 C 0.560(2) 0.654(2) 0.188(2) 0.139(13) Uani 1 1 d D . . H23A H 0.6239 0.6474 0.1363 0.208 Uiso 1 1 calc R . . H23B H 0.4694 0.6384 0.1784 0.208 Uiso 1 1 calc R . . H23C H 0.6204 0.5846 0.2428 0.208 Uiso 1 1 calc R . . C31 C 0.365(3) 0.733(2) 0.3763(16) 0.140 Uiso 1 1 d D . . H31 H 0.2769 0.7044 0.3857 0.168 Uiso 1 1 calc R . . C32 C 0.505(3) 0.598(2) 0.392(2) 0.141 Uiso 1 1 d D . . H32A H 0.5187 0.5480 0.4574 0.211 Uiso 1 1 d R . . H32B H 0.4853 0.5436 0.3598 0.211 Uiso 1 1 d R . . H32C H 0.5993 0.6108 0.3728 0.211 Uiso 1 1 d R . . C33 C 0.348(3) 0.806(3) 0.4462(19) 0.142 Uiso 1 1 d D . . H33A H 0.3766 0.7359 0.5067 0.213 Uiso 1 1 d R . . H33B H 0.4170 0.8555 0.4374 0.213 Uiso 1 1 d R . . H33C H 0.2420 0.8722 0.4442 0.213 Uiso 1 1 d R . . C41 C 0.172(2) 0.833(2) 0.1797(12) 0.094(7) Uiso 1 1 d D . . H41 H 0.1846 0.7347 0.2033 0.112 Uiso 1 1 calc R . . C42 C 0.215(3) 0.857(3) 0.0822(15) 0.146 Uiso 1 1 d D . . H42A H 0.1750 0.8102 0.0535 0.219 Uiso 1 1 d R . . H42B H 0.3278 0.8210 0.0801 0.219 Uiso 1 1 d R . . H42C H 0.1705 0.9573 0.0503 0.219 Uiso 1 1 d R . . C43 C 0.005(2) 0.923(3) 0.1904(18) 0.141 Uiso 1 1 d D . . H43A H -0.0214 0.8881 0.2521 0.211 Uiso 1 1 calc R . . H43B H -0.0629 0.9181 0.1481 0.211 Uiso 1 1 calc R . . H43C H -0.0086 1.0189 0.1778 0.211 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 0.0464(4) 0.0465(4) 0.0468(4) -0.0154(3) 0.0014(3) -0.0185(3) Mn1 0.0292(12) 0.0391(12) 0.0297(11) -0.0013(9) 0.0058(9) -0.0177(10) S1 0.035(2) 0.040(2) 0.041(2) -0.0082(16) 0.0003(16) -0.0150(17) S2 0.041(2) 0.042(2) 0.045(2) -0.0017(17) -0.0003(18) -0.0185(18) S3 0.047(2) 0.069(3) 0.041(2) -0.011(2) 0.0113(19) -0.030(2) N1 0.052(9) 0.080(10) 0.050(8) -0.010(7) 0.001(7) -0.038(8) C1 0.040(9) 0.052(9) 0.035(8) -0.013(7) 0.002(7) -0.017(7) C2 0.035(8) 0.034(8) 0.050(9) -0.010(7) -0.001(7) -0.003(7) C3 0.072(13) 0.056(11) 0.073(12) -0.028(9) 0.007(10) -0.031(10) O3 0.102(12) 0.072(9) 0.136(14) -0.020(9) -0.006(10) -0.057(9) C11 0.060(13) 0.16(2) 0.037(10) -0.026(12) 0.004(9) -0.042(14) C4 0.045(10) 0.081(12) 0.067(12) -0.037(10) 0.010(9) -0.037(9) O4 0.095(11) 0.107(11) 0.045(7) -0.007(7) -0.019(7) -0.040(9) C12 0.060(12) 0.115(16) 0.068(12) -0.015(11) -0.005(10) -0.064(12) C5 0.055(12) 0.068(12) 0.078(13) -0.044(11) -0.006(10) -0.006(10) O5 0.086(11) 0.109(12) 0.106(12) -0.071(11) -0.007(9) 0.009(10) C6 0.054(11) 0.063(11) 0.047(10) 0.002(8) -0.002(8) -0.026(9) O6 0.090(10) 0.055(8) 0.107(12) 0.011(8) -0.010(9) -0.042(8) C7 0.053(11) 0.051(10) 0.058(10) -0.009(8) 0.015(9) -0.023(9) O7 0.079(10) 0.097(11) 0.074(9) -0.013(8) 0.042(8) -0.032(9) C8 0.063(12) 0.083(13) 0.046(10) -0.011(9) 0.014(9) -0.049(11) O8 0.107(12) 0.163(15) 0.046(8) -0.033(9) -0.003(8) -0.079(11) P1 0.063(3) 0.040(2) 0.048(2) -0.0115(19) 0.022(2) -0.024(2) C21 0.047(10) 0.051(10) 0.071(11) -0.025(9) 0.015(9) -0.023(8) C22 0.062(13) 0.077(13) 0.099(16) -0.028(12) 0.004(11) -0.031(11) C23 0.075(16) 0.11(2) 0.28(4) -0.13(3) 0.05(2) -0.043(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 C3 1.852(19) . ? Re1 C4 1.918(19) . ? Re1 C5 1.926(18) . ? Re1 S3 2.488(4) . ? Re1 S2 2.507(4) . ? Re1 S1 2.514(4) . ? Mn1 C7 1.763(18) . ? Mn1 C6 1.782(18) . ? Mn1 C8 1.808(17) . ? Mn1 C1 2.103(15) . ? Mn1 S1 2.310(4) . ? Mn1 S2 2.518(5) . ? S1 C1 1.792(14) . ? S2 C2 1.757(16) . ? S3 C2 1.684(15) . ? N1 C2 1.311(19) . ? N1 C12 1.43(2) . ? N1 C11 1.50(2) . ? C1 P1 1.746(15) . ? C3 O3 1.19(2) . ? C4 O4 1.15(2) . ? C5 O5 1.11(2) . ? C6 O6 1.165(19) . ? C7 O7 1.19(2) . ? C8 O8 1.181(19) . ? P1 C21 1.806(15) . ? P1 C31 1.88(2) . ? P1 C41 2.00(2) . ? C21 C22 1.494(3) . ? C21 C23 1.495(3) . ? C31 C33 1.4831(11) . ? C31 C32 1.4832(11) . ? C41 C43 1.494(3) . ? C41 C42 1.494(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 C3 Re1 C4 89.9(8) . . ? C3 Re1 C5 90.1(8) . . ? C4 Re1 C5 91.3(8) . . ? C3 Re1 S3 172.1(6) . . ? C4 Re1 S3 98.0(5) . . ? C5 Re1 S3 90.2(6) . . ? C3 Re1 S2 101.9(6) . . ? C4 Re1 S2 166.8(5) . . ? C5 Re1 S2 94.5(5) . . ? S3 Re1 S2 70.16(13) . . ? C3 Re1 S1 86.4(6) . . ? C4 Re1 S1 94.2(5) . . ? C5 Re1 S1 173.4(6) . . ? S3 Re1 S1 92.52(13) . . ? S2 Re1 S1 80.78(13) . . ? C7 Mn1 C6 87.2(8) . . ? C7 Mn1 C8 87.6(8) . . ? C6 Mn1 C8 96.3(8) . . ? C7 Mn1 C1 99.0(7) . . ? C6 Mn1 C1 154.9(7) . . ? C8 Mn1 C1 108.2(6) . . ? C7 Mn1 S1 98.6(6) . . ? C6 Mn1 S1 107.5(5) . . ? C8 Mn1 S1 155.6(5) . . ? C1 Mn1 S1 47.6(4) . . ? C7 Mn1 S2 170.7(5) . . ? C6 Mn1 S2 83.5(6) . . ? C8 Mn1 S2 93.1(6) . . ? C1 Mn1 S2 89.6(4) . . ? S1 Mn1 S2 84.61(15) . . ? C1 S1 Mn1 60.1(5) . . ? C1 S1 Re1 110.5(5) . . ? Mn1 S1 Re1 98.01(14) . . ? C2 S2 Re1 87.2(5) . . ? C2 S2 Mn1 111.0(5) . . ? Re1 S2 Mn1 92.96(13) . . ? C2 S3 Re1 89.5(6) . . ? C2 N1 C12 120.9(14) . . ? C2 N1 C11 122.6(15) . . ? C12 N1 C11 116.5(14) . . ? P1 C1 S1 119.3(8) . . ? P1 C1 Mn1 134.4(8) . . ? S1 C1 Mn1 72.3(5) . . ? N1 C2 S3 123.9(13) . . ? N1 C2 S2 123.0(12) . . ? S3 C2 S2 113.1(8) . . ? O3 C3 Re1 178.5(17) . . ? O4 C4 Re1 176.4(15) . . ? O5 C5 Re1 179.1(16) . . ? O6 C6 Mn1 173.7(15) . . ? O7 C7 Mn1 172.5(16) . . ? O8 C8 Mn1 176.6(17) . . ? C1 P1 C21 114.5(7) . . ? C1 P1 C31 113.2(8) . . ? C21 P1 C31 108.2(9) . . ? C1 P1 C41 100.8(8) . . ? C21 P1 C41 105.8(7) . . ? C31 P1 C41 114.2(10) . . ? C22 C21 C23 114.0(3) . . ? C22 C21 P1 114.4(11) . . ? C23 C21 P1 112.3(13) . . ? C33 C31 C32 115.2(2) . . ? C33 C31 P1 115.4(18) . . ? C32 C31 P1 113.7(19) . . ? C43 C41 C42 113.9(3) . . ? C43 C41 P1 113.6(17) . . ? C42 C41 P1 109.0(17) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.976 _refine_diff_density_min -1.354 _refine_diff_density_rms 0.228 #===END data_Compound_5a_(lm140at) _database_code_CSD 208878 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H30 Mn N O6 P Re S3' _chemical_formula_weight 748.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' P P 0.1023 0.0942 '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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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 11.146(4) _cell_length_b 16.565(5) _cell_length_c 15.537(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.363(12) _cell_angle_gamma 90.00 _cell_volume 2790.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 5.101 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.786630 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(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 11992 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.29 _reflns_number_total 4028 _reflns_number_gt 3422 _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^)+(0.0278P)^2^+0.3069P] 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 4028 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.706805(16) 0.270181(11) 0.603599(11) 0.04373(8) Uani 0.7858(7) 1 d P . . Mn1 Mn 0.706805(16) 0.270181(11) 0.603599(11) 0.04373(8) Uani 0.2142(7) 1 d P . . Mn2 Mn 1.03998(3) 0.27456(2) 0.67318(2) 0.04464(16) Uani 0.7858(7) 1 d P . . Re2 Re 1.03998(3) 0.27456(2) 0.67318(2) 0.04464(16) Uani 0.2142(7) 1 d P . . S1 S 0.86315(9) 0.25631(6) 0.74015(6) 0.0432(2) Uani 1 1 d . . . S2 S 0.88726(9) 0.33510(6) 0.55090(6) 0.0519(3) Uani 1 1 d . . . S3 S 0.89503(15) 0.51843(8) 0.59028(10) 0.0960(5) Uani 1 1 d . . . P1 P 0.68884(8) 0.37059(6) 0.80739(6) 0.0428(2) Uani 1 1 d . . . N1 N 1.0252(3) 0.3999(2) 0.6863(2) 0.0610(9) Uani 1 1 d . . . C1 C 0.7647(3) 0.3444(2) 0.7224(2) 0.0414(8) Uani 1 1 d . . . H1 H 0.8117 0.3909 0.7092 0.050 Uiso 1 1 calc R . . C2 C 0.9434(4) 0.4193(2) 0.6175(3) 0.0561(11) Uani 1 1 d . . . C3 C 0.7242(4) 0.1874(3) 0.5236(3) 0.0575(10) Uani 1 1 d . . . O3 O 0.7364(3) 0.1354(2) 0.4781(2) 0.0839(10) Uani 1 1 d . . . C4 C 0.5842(5) 0.3238(3) 0.5192(3) 0.0763(13) Uani 1 1 d . . . O4 O 0.5071(3) 0.3558(3) 0.4690(2) 0.1157(14) Uani 1 1 d . . . C5 C 0.5831(4) 0.2074(3) 0.6328(3) 0.0632(12) Uani 1 1 d . . . O5 O 0.5072(3) 0.1650(2) 0.6460(2) 0.0967(12) Uani 1 1 d . . . C6 C 1.0264(3) 0.1708(3) 0.6398(2) 0.0529(10) Uani 1 1 d . . . O6 O 1.0210(3) 0.1046(2) 0.6173(2) 0.0768(9) Uani 1 1 d . . . C7 C 1.1405(4) 0.2441(3) 0.7771(3) 0.0658(12) Uani 1 1 d . . . O7 O 1.2026(4) 0.2171(3) 0.8394(3) 0.1062(13) Uani 1 1 d . . . C8 C 1.1719(4) 0.2878(3) 0.6243(3) 0.0636(12) Uani 1 1 d . . . O8 O 1.2563(3) 0.2929(2) 0.5961(2) 0.0988(12) Uani 1 1 d . . . C10 C 0.7632(6) 0.5053(4) 0.5027(4) 0.132(3) Uani 1 1 d . . . H10A H 0.7839 0.4720 0.4577 0.198 Uiso 1 1 calc R . . H10B H 0.7350 0.5569 0.4781 0.198 Uiso 1 1 calc R . . H10C H 0.6990 0.4798 0.5249 0.198 Uiso 1 1 calc R . . C11 C 1.0887(5) 0.4596(3) 0.7519(4) 0.0973(18) Uani 1 1 d . . . H11A H 1.0338 0.5050 0.7515 0.117 Uiso 1 1 calc R . . H11B H 1.1030 0.4351 0.8101 0.117 Uiso 1 1 calc R . . C12 C 1.2005(6) 0.4887(5) 0.7397(5) 0.178(4) Uani 1 1 d . . . H12A H 1.2427 0.5170 0.7919 0.266 Uiso 1 1 calc R . . H12B H 1.1857 0.5249 0.6901 0.266 Uiso 1 1 calc R . . H12C H 1.2504 0.4444 0.7287 0.266 Uiso 1 1 calc R . . C21 C 0.7957(4) 0.3755(3) 0.9168(3) 0.0697(13) Uani 1 1 d . . . H21 H 0.8039 0.3197 0.9383 0.084 Uiso 1 1 calc R . . C22 C 0.9231(4) 0.4014(4) 0.9149(3) 0.0970(18) Uani 1 1 d . . . H22A H 0.9218 0.4566 0.8961 0.145 Uiso 1 1 calc R . . H22B H 0.9539 0.3679 0.8744 0.145 Uiso 1 1 calc R . . H22C H 0.9757 0.3963 0.9730 0.145 Uiso 1 1 calc R . . C23 C 0.7454(5) 0.4228(4) 0.9857(3) 0.1019(19) Uani 1 1 d . . . H23A H 0.8043 0.4212 1.0416 0.153 Uiso 1 1 calc R . . H23B H 0.6693 0.3989 0.9919 0.153 Uiso 1 1 calc R . . H23C H 0.7310 0.4778 0.9668 0.153 Uiso 1 1 calc R . . C31 C 0.6163(4) 0.4679(2) 0.7773(3) 0.0627(12) Uani 1 1 d . . . H31 H 0.5721 0.4817 0.8230 0.075 Uiso 1 1 calc R . . C32 C 0.5205(5) 0.4638(3) 0.6900(3) 0.0982(18) Uani 1 1 d . . . H32A H 0.4805 0.5153 0.6778 0.147 Uiso 1 1 calc R . . H32B H 0.4603 0.4233 0.6937 0.147 Uiso 1 1 calc R . . H32C H 0.5602 0.4502 0.6432 0.147 Uiso 1 1 calc R . . C33 C 0.7081(5) 0.5352(3) 0.7764(4) 0.1008(18) Uani 1 1 d . . . H33A H 0.7555 0.5231 0.7336 0.151 Uiso 1 1 calc R . . H33B H 0.7624 0.5401 0.8339 0.151 Uiso 1 1 calc R . . H33C H 0.6647 0.5851 0.7609 0.151 Uiso 1 1 calc R . . C41 C 0.4772(4) 0.3318(4) 0.8684(4) 0.1047(19) Uani 1 1 d . . . H41A H 0.4078 0.2961 0.8607 0.157 Uiso 1 1 calc R . . H41B H 0.4494 0.3848 0.8476 0.157 Uiso 1 1 calc R . . H41C H 0.5178 0.3345 0.9299 0.157 Uiso 1 1 calc R . . C42 C 0.6158(5) 0.2181(3) 0.8510(3) 0.0910(17) Uani 1 1 d . . . H42A H 0.5486 0.1805 0.8431 0.136 Uiso 1 1 calc R . . H42B H 0.6545 0.2224 0.9128 0.136 Uiso 1 1 calc R . . H42C H 0.6749 0.1995 0.8193 0.136 Uiso 1 1 calc R . . C43 C 0.5671(4) 0.3004(3) 0.8158(3) 0.0622(11) Uani 1 1 d . . . H43 H 0.5187 0.2915 0.7553 0.075 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 0.04630(12) 0.04236(13) 0.04203(11) -0.00225(8) 0.00920(8) 0.00106(8) Mn1 0.04630(12) 0.04236(13) 0.04203(11) -0.00225(8) 0.00920(8) 0.00106(8) Mn2 0.0410(2) 0.0468(3) 0.0484(2) -0.00532(16) 0.01507(17) 0.00053(16) Re2 0.0410(2) 0.0468(3) 0.0484(2) -0.00532(16) 0.01507(17) 0.00053(16) S1 0.0466(5) 0.0412(6) 0.0445(5) 0.0010(4) 0.0159(4) 0.0067(4) S2 0.0657(6) 0.0468(6) 0.0475(5) 0.0023(4) 0.0217(5) 0.0016(5) S3 0.1389(13) 0.0393(8) 0.1289(12) 0.0117(7) 0.0705(11) 0.0038(7) P1 0.0457(5) 0.0389(6) 0.0480(5) -0.0006(4) 0.0196(5) 0.0041(4) N1 0.060(2) 0.055(2) 0.076(2) -0.0189(19) 0.031(2) -0.0136(18) C1 0.045(2) 0.035(2) 0.047(2) 0.0016(16) 0.0176(17) 0.0030(16) C2 0.075(3) 0.035(2) 0.073(3) 0.004(2) 0.046(3) -0.004(2) C3 0.055(2) 0.064(3) 0.053(2) 0.001(2) 0.012(2) -0.008(2) O3 0.101(3) 0.073(2) 0.082(2) -0.0294(19) 0.030(2) -0.0045(19) C4 0.080(3) 0.079(4) 0.068(3) 0.002(3) 0.012(3) 0.010(3) O4 0.104(3) 0.129(4) 0.097(3) 0.017(2) -0.012(2) 0.044(3) C5 0.062(3) 0.068(3) 0.060(3) -0.016(2) 0.016(2) -0.004(2) O5 0.085(2) 0.108(3) 0.106(3) -0.026(2) 0.040(2) -0.044(2) C6 0.045(2) 0.066(3) 0.053(2) 0.008(2) 0.0243(19) 0.006(2) O6 0.094(2) 0.053(2) 0.097(2) -0.0025(18) 0.0493(19) 0.0005(17) C7 0.051(3) 0.088(4) 0.059(3) -0.012(2) 0.013(2) 0.000(2) O7 0.083(3) 0.149(4) 0.075(2) 0.004(2) -0.006(2) 0.010(2) C8 0.057(3) 0.056(3) 0.083(3) -0.010(2) 0.027(2) -0.004(2) O8 0.078(2) 0.111(3) 0.126(3) 0.002(2) 0.062(2) -0.009(2) C10 0.183(7) 0.088(5) 0.130(5) 0.051(4) 0.048(5) 0.052(5) C11 0.098(4) 0.077(4) 0.126(4) -0.054(3) 0.046(4) -0.036(3) C12 0.100(5) 0.223(10) 0.221(9) -0.131(8) 0.061(5) -0.078(6) C21 0.072(3) 0.087(4) 0.052(3) -0.011(2) 0.020(2) 0.008(2) C22 0.063(3) 0.157(6) 0.068(3) -0.030(3) 0.011(3) -0.007(3) C23 0.101(4) 0.146(6) 0.064(3) -0.032(3) 0.031(3) 0.011(4) C31 0.075(3) 0.046(3) 0.079(3) 0.009(2) 0.043(3) 0.016(2) C32 0.095(4) 0.104(5) 0.100(4) 0.032(3) 0.030(3) 0.049(3) C33 0.141(5) 0.040(3) 0.145(5) 0.004(3) 0.082(4) 0.007(3) C41 0.093(4) 0.109(5) 0.139(5) -0.019(4) 0.082(4) -0.027(3) C42 0.126(5) 0.055(4) 0.103(4) 0.013(3) 0.050(4) -0.012(3) C43 0.067(3) 0.058(3) 0.072(3) -0.001(2) 0.036(2) -0.012(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 C5 1.865(5) . ? Re1 C4 1.883(5) . ? Re1 C3 1.890(5) . ? Re1 C1 2.187(3) . ? Re1 S1 2.4252(12) . ? Re1 S2 2.5755(12) . ? Mn2 C6 1.792(5) . ? Mn2 C7 1.811(5) . ? Mn2 C8 1.818(5) . ? Mn2 N1 2.096(4) . ? Mn2 S1 2.4507(12) . ? Mn2 S2 2.4532(12) . ? S1 C1 1.807(3) . ? S2 C2 1.763(4) . ? S3 C2 1.750(4) . ? S3 C10 1.770(7) . ? P1 C1 1.779(3) . ? P1 C43 1.815(4) . ? P1 C31 1.815(4) . ? P1 C21 1.838(4) . ? N1 C2 1.274(5) . ? N1 C11 1.478(5) . ? C3 O3 1.143(5) . ? C4 O4 1.148(5) . ? C5 O5 1.154(5) . ? C6 O6 1.148(5) . ? C7 O7 1.144(5) . ? C8 O8 1.128(5) . ? C11 C12 1.390(7) . ? C21 C22 1.491(6) . ? C21 C23 1.534(6) . ? C31 C33 1.516(6) . ? C31 C32 1.523(6) . ? C41 C43 1.523(6) . ? C42 C43 1.521(6) . ? 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 C5 Re1 C4 88.5(2) . . ? C5 Re1 C3 87.09(17) . . ? C4 Re1 C3 93.01(19) . . ? C5 Re1 C1 101.44(15) . . ? C4 Re1 C1 110.36(18) . . ? C3 Re1 C1 155.13(15) . . ? C5 Re1 S1 98.98(13) . . ? C4 Re1 S1 155.89(15) . . ? C3 Re1 S1 110.14(12) . . ? C1 Re1 S1 45.77(9) . . ? C5 Re1 S2 170.33(13) . . ? C4 Re1 S2 94.36(15) . . ? C3 Re1 S2 83.55(12) . . ? C1 Re1 S2 86.21(9) . . ? S1 Re1 S2 82.05(4) . . ? C6 Mn2 C7 89.10(19) . . ? C6 Mn2 C8 90.97(17) . . ? C7 Mn2 C8 90.7(2) . . ? C6 Mn2 N1 167.16(17) . . ? C7 Mn2 N1 103.63(18) . . ? C8 Mn2 N1 90.60(16) . . ? C6 Mn2 S1 88.98(11) . . ? C7 Mn2 S1 88.85(14) . . ? C8 Mn2 S1 179.56(15) . . ? N1 Mn2 S1 89.55(9) . . ? C6 Mn2 S2 99.85(12) . . ? C7 Mn2 S2 168.47(14) . . ? C8 Mn2 S2 96.35(15) . . ? N1 Mn2 S2 67.31(11) . . ? S1 Mn2 S2 84.09(4) . . ? C1 S1 Re1 60.15(11) . . ? C1 S1 Mn2 110.80(12) . . ? Re1 S1 Mn2 95.89(4) . . ? C2 S2 Mn2 77.27(16) . . ? C2 S2 Re1 109.93(12) . . ? Mn2 S2 Re1 92.07(4) . . ? C2 S3 C10 103.0(3) . . ? C1 P1 C43 112.87(18) . . ? C1 P1 C31 106.61(17) . . ? C43 P1 C31 106.9(2) . . ? C1 P1 C21 112.31(17) . . ? C43 P1 C21 107.3(2) . . ? C31 P1 C21 110.7(2) . . ? C2 N1 C11 123.1(4) . . ? C2 N1 Mn2 103.0(3) . . ? C11 N1 Mn2 133.9(4) . . ? P1 C1 S1 117.40(19) . . ? P1 C1 Re1 131.72(19) . . ? S1 C1 Re1 74.08(12) . . ? N1 C2 S3 124.0(3) . . ? N1 C2 S2 112.4(3) . . ? S3 C2 S2 123.5(3) . . ? O3 C3 Re1 177.3(4) . . ? O4 C4 Re1 178.1(5) . . ? O5 C5 Re1 175.1(4) . . ? O6 C6 Mn2 177.8(3) . . ? O7 C7 Mn2 173.0(5) . . ? O8 C8 Mn2 176.8(4) . . ? C12 C11 N1 116.0(5) . . ? C22 C21 C23 111.8(4) . . ? C22 C21 P1 114.3(3) . . ? C23 C21 P1 113.9(3) . . ? C33 C31 C32 111.1(4) . . ? C33 C31 P1 113.2(3) . . ? C32 C31 P1 111.6(3) . . ? C42 C43 C41 109.7(4) . . ? C42 C43 P1 112.9(3) . . ? C41 C43 P1 114.5(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.409 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.060 #===END data_Compound_5c_(lm134at) _database_code_CSD 208879 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 Mn N O6 P Re S3' _chemical_formula_weight 796.78 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' 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' Mn Mn 0.3368 0.7283 '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 10.902(5) _cell_length_b 17.048(8) _cell_length_c 16.551(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.263(8) _cell_angle_gamma 90.00 _cell_volume 3044(2) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 4.682 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.689596 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(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 13339 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 23.37 _reflns_number_total 4388 _reflns_number_gt 3611 _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^)+(0.0340P)^2^+6.5513P] 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 4388 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.005 _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 0.82889(2) 0.276402(15) 0.412292(16) 0.04305(12) Uani 0.8554(12) 1 d P . . Mn1 Mn 0.82889(2) 0.276402(15) 0.412292(16) 0.04305(12) Uani 0.1446(12) 1 d P . . Mn2 Mn 0.49159(5) 0.28307(3) 0.36381(4) 0.0372(3) Uani 0.8554(12) 1 d P . . Re2 Re 0.49159(5) 0.28307(3) 0.36381(4) 0.0372(3) Uani 0.1446(12) 1 d P . . S1 S 0.66931(15) 0.26241(9) 0.29290(10) 0.0504(4) Uani 1 1 d . . . S2 S 0.64777(14) 0.34001(9) 0.47036(9) 0.0472(4) Uani 1 1 d . . . P1 P 0.84521(15) 0.36858(10) 0.21544(10) 0.0524(4) Uani 1 1 d . . . N1 N 0.5086(4) 0.4049(3) 0.3543(3) 0.0434(11) Uani 1 1 d . . . C1 C 0.7713(5) 0.3474(3) 0.3009(3) 0.0461(14) Uani 1 1 d . . . H1 H 0.7257 0.3938 0.3151 0.055 Uiso 1 1 calc R . . C3 C 0.8112(7) 0.1923(5) 0.4865(5) 0.070(2) Uani 1 1 d . . . O3 O 0.8000(6) 0.1387(4) 0.5275(4) 0.115(2) Uani 1 1 d . . . S3 S 0.65106(16) 0.51808(9) 0.43411(12) 0.0611(5) Uani 1 1 d . . . C4 C 0.9619(8) 0.2211(5) 0.3792(5) 0.079(2) Uani 1 1 d . . . O4 O 1.0472(7) 0.1865(5) 0.3649(4) 0.138(3) Uani 1 1 d . . . C5 C 0.9462(6) 0.3246(4) 0.4921(5) 0.0631(18) Uani 1 1 d . . . O5 O 1.0165(5) 0.3534(4) 0.5419(4) 0.0985(19) Uani 1 1 d . . . C6 C 0.5056(6) 0.1811(4) 0.3916(4) 0.0625(18) Uani 1 1 d . . . O6 O 0.5104(5) 0.1159(3) 0.4093(3) 0.0846(16) Uani 1 1 d . . . C7 C 0.3907(7) 0.2629(4) 0.2708(5) 0.071(2) Uani 1 1 d . . . O7 O 0.3256(7) 0.2487(4) 0.2120(4) 0.126(3) Uani 1 1 d . . . C8 C 0.3636(7) 0.2968(4) 0.4197(5) 0.0635(18) Uani 1 1 d . . . O8 O 0.2785(5) 0.3039(4) 0.4526(4) 0.0995(19) Uani 1 1 d . . . C9 C 0.5957(5) 0.4232(3) 0.4128(4) 0.0460(14) Uani 1 1 d . . . C10 C 0.7951(6) 0.5004(4) 0.4981(5) 0.073(2) Uani 1 1 d . . . H10A H 0.8501 0.4728 0.4676 0.110 Uiso 1 1 calc R . . H10B H 0.7806 0.4693 0.5442 0.110 Uiso 1 1 calc R . . H10C H 0.8318 0.5495 0.5168 0.110 Uiso 1 1 calc R . . C13 C 0.4349(5) 0.4610(3) 0.3048(4) 0.0448(14) Uani 1 1 d . . . C14 C 0.4037(7) 0.4460(4) 0.2228(4) 0.070(2) Uani 1 1 d . . . H14 H 0.4328 0.4009 0.2002 0.085 Uiso 1 1 calc R . . C15 C 0.3296(9) 0.4975(5) 0.1740(5) 0.092(3) Uani 1 1 d . . . H15 H 0.3094 0.4875 0.1185 0.111 Uiso 1 1 calc R . . C16 C 0.2854(8) 0.5636(5) 0.2070(6) 0.090(3) Uani 1 1 d . . . H16 H 0.2367 0.5990 0.1738 0.107 Uiso 1 1 calc R . . C17 C 0.3134(7) 0.5776(4) 0.2899(6) 0.076(2) Uani 1 1 d . . . H17 H 0.2814 0.6216 0.3126 0.091 Uiso 1 1 calc R . . C18 C 0.3883(6) 0.5267(4) 0.3386(4) 0.0573(17) Uani 1 1 d . . . H18 H 0.4077 0.5364 0.3943 0.069 Uiso 1 1 calc R . . C21 C 0.9422(9) 0.4547(6) 0.2420(5) 0.096(3) Uani 1 1 d . . . H21 H 0.9776 0.4693 0.1929 0.116 Uiso 1 1 calc R . . C22 C 1.0518(11) 0.4347(9) 0.3079(6) 0.185(7) Uani 1 1 d . . . H22A H 1.0211 0.4154 0.3557 0.277 Uiso 1 1 calc R . . H22B H 1.1007 0.4809 0.3216 0.277 Uiso 1 1 calc R . . H22C H 1.1022 0.3952 0.2876 0.277 Uiso 1 1 calc R . . C23 C 0.8670(15) 0.5250(6) 0.2638(8) 0.189(8) Uani 1 1 d . . . H23A H 0.9193 0.5705 0.2707 0.284 Uiso 1 1 calc R . . H23B H 0.8347 0.5145 0.3137 0.284 Uiso 1 1 calc R . . H23C H 0.7997 0.5342 0.2207 0.284 Uiso 1 1 calc R . . C31 C 0.7314(8) 0.3973(6) 0.1284(5) 0.094(3) Uani 1 1 d . . . H31 H 0.6805 0.4360 0.1520 0.113 Uiso 1 1 calc R . . C32 C 0.6426(10) 0.3399(8) 0.0946(6) 0.149(5) Uani 1 1 d . . . H32A H 0.6782 0.3077 0.0564 0.223 Uiso 1 1 calc R . . H32B H 0.5703 0.3658 0.0672 0.223 Uiso 1 1 calc R . . H32C H 0.6199 0.3076 0.1377 0.223 Uiso 1 1 calc R . . C33 C 0.7822(12) 0.4431(8) 0.0629(7) 0.173(6) Uani 1 1 d . . . H33A H 0.7154 0.4688 0.0288 0.259 Uiso 1 1 calc R . . H33B H 0.8237 0.4081 0.0303 0.259 Uiso 1 1 calc R . . H33C H 0.8399 0.4817 0.0876 0.259 Uiso 1 1 calc R . . C41 C 0.9480(7) 0.2912(5) 0.1902(5) 0.084(2) Uani 1 1 d . . . H41 H 1.0079 0.2832 0.2396 0.100 Uiso 1 1 calc R . . C42 C 0.8868(10) 0.2112(5) 0.1708(6) 0.113(3) Uani 1 1 d . . . H42A H 0.9491 0.1733 0.1629 0.169 Uiso 1 1 calc R . . H42B H 0.8278 0.2152 0.1220 0.169 Uiso 1 1 calc R . . H42C H 0.8453 0.1951 0.2154 0.169 Uiso 1 1 calc R . . C43 C 1.0242(10) 0.3154(8) 0.1243(7) 0.138(4) Uani 1 1 d . . . H43A H 0.9698 0.3266 0.0747 0.206 Uiso 1 1 calc R . . H43B H 1.0792 0.2735 0.1148 0.206 Uiso 1 1 calc R . . H43C H 1.0717 0.3614 0.1416 0.206 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 0.04281(17) 0.04343(17) 0.04174(17) 0.00206(12) 0.00210(11) 0.00566(12) Mn1 0.04281(17) 0.04343(17) 0.04174(17) 0.00206(12) 0.00210(11) 0.00566(12) Mn2 0.0352(4) 0.0329(4) 0.0422(4) 0.0024(3) 0.0013(3) -0.0053(2) Re2 0.0352(4) 0.0329(4) 0.0422(4) 0.0024(3) 0.0013(3) -0.0053(2) S1 0.0536(9) 0.0462(8) 0.0509(9) -0.0073(7) 0.0057(7) -0.0065(7) S2 0.0482(8) 0.0481(8) 0.0446(9) 0.0003(7) 0.0044(7) 0.0007(7) P1 0.0524(10) 0.0628(10) 0.0416(9) -0.0052(8) 0.0059(8) -0.0106(8) N1 0.045(3) 0.041(3) 0.043(3) 0.000(2) 0.004(2) 0.000(2) C1 0.045(3) 0.048(3) 0.045(3) -0.003(3) 0.004(3) -0.004(3) C3 0.073(5) 0.066(5) 0.066(5) 0.009(4) -0.003(4) 0.011(4) O3 0.132(5) 0.084(4) 0.122(5) 0.056(4) -0.004(4) -0.001(4) S3 0.0618(10) 0.0435(9) 0.0741(12) -0.0113(8) -0.0036(9) -0.0062(7) C4 0.087(6) 0.090(6) 0.059(5) 0.004(4) 0.004(4) 0.029(5) O4 0.120(5) 0.180(7) 0.115(5) 0.002(5) 0.020(4) 0.094(6) C5 0.056(4) 0.064(4) 0.069(5) 0.009(4) 0.009(4) 0.007(3) O5 0.077(4) 0.109(4) 0.100(4) -0.008(4) -0.021(3) -0.016(3) C6 0.056(4) 0.064(5) 0.066(5) 0.014(4) 0.005(3) -0.001(3) O6 0.099(4) 0.052(3) 0.101(4) 0.016(3) 0.008(3) -0.004(3) C7 0.076(5) 0.054(4) 0.075(5) 0.018(4) -0.009(4) -0.023(4) O7 0.149(6) 0.094(4) 0.110(5) 0.027(4) -0.066(5) -0.056(4) C8 0.055(4) 0.061(4) 0.074(5) 0.005(4) 0.005(4) -0.006(3) O8 0.063(3) 0.116(5) 0.125(5) 0.007(4) 0.037(4) -0.003(3) C9 0.044(3) 0.045(3) 0.049(4) -0.004(3) 0.005(3) -0.001(3) C10 0.055(4) 0.077(5) 0.084(5) -0.017(4) -0.002(4) -0.013(4) C13 0.048(3) 0.041(3) 0.044(4) 0.001(3) 0.004(3) -0.001(3) C14 0.101(6) 0.049(4) 0.059(5) 0.003(4) 0.002(4) 0.002(4) C15 0.136(8) 0.070(5) 0.059(5) 0.011(4) -0.022(5) -0.002(5) C16 0.091(6) 0.062(5) 0.103(7) 0.023(5) -0.026(5) 0.001(4) C17 0.064(5) 0.058(4) 0.101(7) 0.003(4) -0.005(4) 0.012(4) C18 0.053(4) 0.056(4) 0.062(4) -0.003(3) 0.006(3) 0.003(3) C21 0.119(7) 0.114(7) 0.064(5) -0.015(5) 0.039(5) -0.062(6) C22 0.168(11) 0.279(17) 0.090(8) 0.023(9) -0.040(8) -0.166(12) C23 0.310(19) 0.099(8) 0.196(14) -0.073(9) 0.165(14) -0.103(10) C31 0.093(6) 0.126(7) 0.056(5) 0.027(5) -0.008(4) -0.022(5) C32 0.126(9) 0.217(14) 0.086(7) 0.024(8) -0.039(7) -0.048(9) C33 0.173(12) 0.239(15) 0.095(8) 0.091(9) -0.017(8) -0.071(11) C41 0.060(5) 0.122(7) 0.071(5) -0.004(5) 0.018(4) 0.019(5) C42 0.127(8) 0.092(7) 0.121(8) -0.027(6) 0.021(7) 0.033(6) C43 0.126(9) 0.178(11) 0.129(9) 0.013(8) 0.086(8) 0.030(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 C4 1.876(9) . ? Re1 C5 1.890(8) . ? Re1 C3 1.916(8) . ? Re1 C1 2.219(6) . ? Re1 S1 2.4495(18) . ? Re1 S2 2.5581(18) . ? Mn2 C7 1.793(8) . ? Mn2 C8 1.797(8) . ? Mn2 C6 1.799(8) . ? Mn2 N1 2.094(5) . ? Mn2 S1 2.431(2) . ? Mn2 S2 2.4674(17) . ? S1 C1 1.820(6) . ? S2 C9 1.756(6) . ? P1 C1 1.763(6) . ? P1 C41 1.818(8) . ? P1 C21 1.827(8) . ? P1 C31 1.827(8) . ? N1 C9 1.293(7) . ? N1 C13 1.429(7) . ? C3 O3 1.154(9) . ? S3 C9 1.745(6) . ? S3 C10 1.789(7) . ? C4 O4 1.155(9) . ? C5 O5 1.151(8) . ? C6 O6 1.148(8) . ? C7 O7 1.144(8) . ? C8 O8 1.148(8) . ? C13 C14 1.375(9) . ? C13 C18 1.381(8) . ? C14 C15 1.374(10) . ? C15 C16 1.370(12) . ? C16 C17 1.382(11) . ? C17 C18 1.372(9) . ? C21 C23 1.524(15) . ? C21 C22 1.536(14) . ? C31 C32 1.432(12) . ? C31 C33 1.506(12) . ? C41 C43 1.521(12) . ? C41 C42 1.531(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Re1 C5 87.0(3) . . ? C4 Re1 C3 88.0(3) . . ? C5 Re1 C3 89.9(3) . . ? C4 Re1 C1 99.8(3) . . ? C5 Re1 C1 115.2(3) . . ? C3 Re1 C1 153.9(3) . . ? C4 Re1 S1 101.8(2) . . ? C5 Re1 S1 159.6(2) . . ? C3 Re1 S1 108.6(2) . . ? C1 Re1 S1 45.55(14) . . ? C4 Re1 S2 173.4(2) . . ? C5 Re1 S2 92.0(2) . . ? C3 Re1 S2 85.5(2) . . ? C1 Re1 S2 86.52(16) . . ? S1 Re1 S2 81.21(6) . . ? C7 Mn2 C8 92.3(4) . . ? C7 Mn2 C6 93.1(3) . . ? C8 Mn2 C6 92.2(3) . . ? C7 Mn2 N1 100.1(2) . . ? C8 Mn2 N1 89.6(3) . . ? C6 Mn2 N1 166.6(2) . . ? C7 Mn2 S1 89.5(3) . . ? C8 Mn2 S1 177.8(2) . . ? C6 Mn2 S1 86.5(2) . . ? N1 Mn2 S1 91.28(13) . . ? C7 Mn2 S2 164.7(2) . . ? C8 Mn2 S2 95.1(2) . . ? C6 Mn2 S2 100.0(2) . . ? N1 Mn2 S2 66.65(13) . . ? S1 Mn2 S2 83.45(6) . . ? C1 S1 Mn2 111.7(2) . . ? C1 S1 Re1 60.51(18) . . ? Mn2 S1 Re1 96.86(7) . . ? C9 S2 Mn2 78.13(19) . . ? C9 S2 Re1 110.2(2) . . ? Mn2 S2 Re1 93.17(6) . . ? C1 P1 C41 113.8(3) . . ? C1 P1 C21 106.7(3) . . ? C41 P1 C21 106.5(4) . . ? C1 P1 C31 110.5(4) . . ? C41 P1 C31 112.6(4) . . ? C21 P1 C31 106.2(4) . . ? C9 N1 C13 124.1(5) . . ? C9 N1 Mn2 104.3(4) . . ? C13 N1 Mn2 131.1(4) . . ? P1 C1 S1 116.7(3) . . ? P1 C1 Re1 132.1(3) . . ? S1 C1 Re1 73.9(2) . . ? O3 C3 Re1 176.0(7) . . ? C9 S3 C10 102.2(3) . . ? O4 C4 Re1 175.0(7) . . ? O5 C5 Re1 178.6(7) . . ? O6 C6 Mn2 177.7(6) . . ? O7 C7 Mn2 178.7(6) . . ? O8 C8 Mn2 176.9(7) . . ? N1 C9 S3 124.7(4) . . ? N1 C9 S2 110.9(4) . . ? S3 C9 S2 124.3(3) . . ? C14 C13 C18 119.9(6) . . ? C14 C13 N1 118.8(5) . . ? C18 C13 N1 121.2(5) . . ? C15 C14 C13 120.1(7) . . ? C16 C15 C14 120.2(8) . . ? C15 C16 C17 119.8(7) . . ? C18 C17 C16 120.2(7) . . ? C17 C18 C13 119.8(7) . . ? C23 C21 C22 113.4(10) . . ? C23 C21 P1 112.1(7) . . ? C22 C21 P1 110.9(7) . . ? C32 C31 C33 111.8(8) . . ? C32 C31 P1 118.0(7) . . ? C33 C31 P1 115.4(7) . . ? C43 C41 C42 110.9(8) . . ? C43 C41 P1 112.7(7) . . ? C42 C41 P1 115.5(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.37 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.891 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.087 #===END