# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1476 data_rese3b #[Re(CO)3{MeC(CH2SeMe)3}]CF3SO3 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Mar 16 15:45:04 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 12.584(1) _cell_length_b 15.216(1) _cell_length_c 12.4563(8) _cell_angle_alpha 99.144(7) _cell_angle_beta 98.605(6) _cell_angle_gamma 101.545(7) _cell_volume 2266.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 571.2 _cell_measurement_reflns_used 24 _cell_measurement_2theta_min 20.3 _cell_measurement_2theta_max 26.4 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'XDIM' _exptl_crystal_colour 'colourlessXDIM' _exptl_crystal_size_max 0.470 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 2.258 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 770.41 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H18 F3 O6 S Re Se3 ' _chemical_formula_moiety '?' _chemical_formula_structural '[Re(CO)3{MeC(CH2SeMe)3}]CF3SO3' _chemical_compound_source 'CH2Cl2/pet ether' _exptl_crystal_F_000 1432.00 _exptl_absorpt_coefficient_mu 10.322 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.276 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 571.2 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -3.38 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 1 4 0 1 4 -3 0 4 _diffrn_reflns_number 8347 _reflns_number_total 7951 _reflns_number_observed 4114 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 3.82 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_2theta_min ? _diffrn_reflns_2theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.05000 _diffrn_orient_matrix_UB_12 -0.02857 _diffrn_orient_matrix_UB_13 0.04650 _diffrn_orient_matrix_UB_21 0.02571 _diffrn_orient_matrix_UB_22 -0.05795 _diffrn_orient_matrix_UB_23 -0.01621 _diffrn_orient_matrix_UB_31 0.06047 _diffrn_orient_matrix_UB_32 0.02243 _diffrn_orient_matrix_UB_33 0.06654 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.003 0.002 'International Tables' H 0 72 0.000 0.000 'International Tables' O 0 24 0.011 0.006 'International Tables' Re 0 4 -1.018 7.231 'International Tables' F 0 12 0.017 0.010 'International Tables' S 0 4 0.125 0.123 'International Tables' Se 0 12 -0.093 2.226 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Re(1) 0.21083(7) 0.38063(7) 0.41428(8) 0.0450(3) Uij ? ? Re(2) -0.46216(7) 0.25132(7) -0.06542(7) 0.0538(3) Uij ? ? Se(1) 0.2454(2) 0.2205(2) 0.4284(2) 0.0490(7) Uij ? ? Se(2) 0.1046(2) 0.3693(2) 0.5752(2) 0.0525(7) Uij ? ? Se(3) 0.0272(2) 0.2997(2) 0.2805(2) 0.0485(7) Uij ? ? Se(4) -0.3683(2) 0.1174(2) -0.0446(2) 0.0555(7) Uij ? ? Se(5) -0.5839(2) 0.1502(2) -0.2466(2) 0.0547(7) Uij ? ? Se(6) -0.3225(2) 0.3085(2) -0.1850(2) 0.0666(8) Uij ? ? S(1) 0.6260(5) 0.1984(5) 0.3458(6) 0.062(2) Uij ? ? S(2) 0.0256(6) 0.1169(6) 0.8023(5) 0.077(2) Uij ? ? F(1) 0.670(2) 0.378(2) 0.362(2) 0.049(8) Uij ? ? F(2) 0.653(4) 0.363(4) 0.393(4) 0.13(2) Uij ? ? F(3) 0.545(3) 0.330(2) 0.449(2) 0.061(9) Uij ? ? F(4) 0.507(4) 0.298(3) 0.436(4) 0.13(2) Uij ? ? F(5) 0.493(4) 0.295(3) 0.288(4) 0.12(2) Uij ? ? F(6) 0.522(2) 0.314(2) 0.262(2) 0.057(8) Uij ? ? F(7) 0.168(2) 0.208(2) 0.971(2) 0.23(1) Uij ? ? F(9) 0.143(2) 0.063(2) 0.953(2) 0.15(1) Uij ? ? F(11) 0.031(2) 0.137(2) 1.012(1) 0.23(1) Uij ? ? O(1) 0.429(1) 0.460(1) 0.579(1) 0.074(6) Uij ? ? O(2) 0.327(1) 0.393(1) 0.217(1) 0.092(7) Uij ? ? O(3) 0.160(1) 0.567(1) 0.402(1) 0.076(6) Uij ? ? O(4) -0.583(2) 0.405(2) -0.091(2) 0.14(1) Uij ? ? O(5) -0.618(1) 0.168(2) 0.082(1) 0.118(9) Uij ? ? O(6) -0.307(2) 0.386(1) 0.135(1) 0.101(7) Uij ? ? O(7) 0.529(1) 0.132(1) 0.344(2) 0.114(8) Uij ? ? O(8) 0.669(1) 0.193(1) 0.249(1) 0.087(7) Uij ? ? O(9) 0.707(2) 0.212(1) 0.442(2) 0.111(8) Uij ? ? O(10) 0.104(2) 0.112(2) 0.734(2) 0.083(9) Uij ? ? O(11) -0.063(3) 0.043(3) 0.790(3) 0.14(1) Uij ? ? O(12) -0.019(2) 0.199(2) 0.808(2) 0.086(9) Uij ? ? O(13) 0.135(6) 0.155(5) 0.780(6) 0.10(2) Uij ? ? O(14) -0.011(7) 0.019(6) 0.757(6) 0.12(2) Uij ? ? O(15) -0.054(7) 0.154(6) 0.813(7) 0.11(2) Uij ? ? C(1) 0.348(2) 0.430(2) 0.514(2) 0.055(8) Uij ? ? C(2) 0.285(2) 0.386(1) 0.297(2) 0.069(8) Uij ? ? C(3) 0.180(2) 0.495(2) 0.407(2) 0.051(7) Uij ? ? C(4) -0.540(2) 0.347(2) -0.084(2) 0.09(1) Uij ? ? C(5) -0.561(2) 0.202(2) 0.031(2) 0.09(1) Uij ? ? C(6) -0.366(2) 0.333(2) 0.065(2) 0.071(9) Uij ? ? C(7) -0.083(2) 0.089(1) 0.463(2) 0.055(7) Uij ? ? C(8) 0.001(2) 0.174(1) 0.450(1) 0.043(6) Uij ? ? C(9) -0.006(2) 0.252(1) 0.539(2) 0.046(6) Uij ? ? C(10) -0.038(2) 0.187(1) 0.331(2) 0.050(7) Uij ? ? C(11) 0.115(2) 0.147(1) 0.464(2) 0.049(7) Uij ? ? C(12) 0.209(2) 0.345(2) 0.692(2) 0.081(9) Uij ? ? C(13) 0.236(2) 0.160(2) 0.277(2) 0.074(9) Uij ? ? C(14) -0.076(2) 0.372(2) 0.319(2) 0.071(9) Uij ? ? C(15) -0.328(2) 0.046(2) -0.387(2) 0.064(8) Uij ? ? C(16) -0.366(2) 0.106(2) -0.294(2) 0.054(7) Uij ? ? C(17) -0.487(2) 0.101(2) -0.339(2) 0.062(8) Uij ? ? C(18) -0.350(2) 0.059(1) -0.193(2) 0.047(6) Uij ? ? C(19) -0.291(2) 0.201(2) -0.276(2) 0.057(8) Uij ? ? C(20) -0.216(2) 0.169(2) 0.021(2) 0.09(1) Uij ? ? C(21) -0.409(2) 0.351(2) -0.303(2) 0.09(1) Uij ? ? C(22) -0.654(2) 0.035(2) -0.211(2) 0.077(9) Uij ? ? C(24) 0.580(2) 0.301(2) 0.360(2) 0.09(1) Uij ? ? C(25) 0.089(3) 0.131(4) 0.943(3) 0.12(2) Uij ? ? H(1) -0.1554 0.1002 0.4556 0.0650 Uiso ? ? H(2) -0.0828 0.0370 0.4106 0.0650 Uiso ? ? H(3) -0.0642 0.0761 0.5365 0.0650 Uiso ? ? H(4) -0.0050 0.2280 0.6074 0.0574 Uiso ? ? H(5) -0.0768 0.2650 0.5207 0.0574 Uiso ? ? H(6) -0.1185 0.1829 0.3203 0.0589 Uiso ? ? H(7) -0.0301 0.1355 0.2783 0.0589 Uiso ? ? H(8) 0.1015 0.0857 0.4208 0.0582 Uiso ? ? H(9) 0.1322 0.1416 0.5411 0.0582 Uiso ? ? H(10) 0.1734 0.3347 0.7547 0.0893 Uiso ? ? H(11) 0.2369 0.2948 0.6685 0.0893 Uiso ? ? H(12) 0.2693 0.3985 0.7199 0.0893 Uiso ? ? H(13) 0.1683 0.1611 0.2293 0.0810 Uiso ? ? H(14) 0.2959 0.1883 0.2440 0.0810 Uiso ? ? H(15) 0.2389 0.0964 0.2712 0.0810 Uiso ? ? H(16) -0.0785 0.3808 0.3957 0.0773 Uiso ? ? H(17) -0.0559 0.4327 0.3008 0.0773 Uiso ? ? H(18) -0.1496 0.3448 0.2780 0.0773 Uiso ? ? H(19) -0.3734 -0.0159 -0.4017 0.0758 Uiso ? ? H(20) -0.3388 0.0684 -0.4549 0.0758 Uiso ? ? H(21) -0.2540 0.0440 -0.3674 0.0758 Uiso ? ? H(22) -0.5206 0.0372 -0.3673 0.0765 Uiso ? ? H(23) -0.4882 0.1311 -0.4018 0.0765 Uiso ? ? H(24) -0.2776 0.0461 -0.1847 0.0546 Uiso ? ? H(25) -0.4024 -0.0009 -0.2123 0.0546 Uiso ? ? H(26) -0.2880 0.2155 -0.3485 0.0666 Uiso ? ? H(27) -0.2188 0.1965 -0.2443 0.0666 Uiso ? ? H(28) -0.1738 0.1228 0.0254 0.0911 Uiso ? ? H(29) -0.1804 0.2115 -0.0191 0.0911 Uiso ? ? H(30) -0.2076 0.2023 0.0966 0.0911 Uiso ? ? H(31) -0.4348 0.4038 -0.2740 0.1024 Uiso ? ? H(32) -0.3687 0.3655 -0.3587 0.1024 Uiso ? ? H(33) -0.4754 0.3039 -0.3392 0.1024 Uiso ? ? H(34) -0.7050 0.0417 -0.1612 0.0890 Uiso ? ? H(35) -0.6918 -0.0107 -0.2741 0.0890 Uiso ? ? H(36) -0.5985 0.0068 -0.1712 0.0890 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.0406(5) 0.0383(6) 0.0564(6) 0.0070(4) 0.0110(4) 0.0107(5) Re(2) 0.0490(5) 0.0657(8) 0.0428(5) 0.0124(5) 0.0031(4) 0.0049(5) Se(1) 0.045(1) 0.046(2) 0.060(1) 0.015(1) 0.015(1) 0.015(1) Se(2) 0.055(1) 0.049(2) 0.050(1) 0.009(1) 0.013(1) 0.001(1) Se(3) 0.051(1) 0.050(2) 0.044(1) 0.007(1) 0.006(1) 0.013(1) Se(4) 0.056(1) 0.075(2) 0.041(1) 0.017(1) 0.013(1) 0.021(1) Se(5) 0.046(1) 0.063(2) 0.050(1) 0.012(1) 0.001(1) 0.007(1) Se(6) 0.067(2) 0.065(2) 0.058(2) -0.005(1) 0.005(1) 0.013(1) S(1) 0.064(4) 0.052(5) 0.073(4) 0.010(3) 0.019(4) 0.018(4) S(2) 0.073(4) 0.084(6) 0.062(4) 0.000(4) 0.011(4) 0.008(4) F(7) 0.20(3) 0.22(4) 0.18(3) 0.01(2) -0.11(2) -0.02(2) F(9) 0.12(1) 0.24(3) 0.14(2) 0.09(2) 0.05(1) 0.09(2) F(11) 0.18(2) 0.52(5) 0.06(1) 0.20(3) 0.05(1) 0.06(2) O(1) 0.049(9) 0.06(1) 0.10(1) 0.000(9) -0.008(10) 0.02(1) O(2) 0.09(1) 0.10(2) 0.10(1) 0.03(1) 0.05(1) 0.03(1) O(3) 0.07(1) 0.05(1) 0.10(1) 0.01(1) 0.01(1) 0.02(1) O(4) 0.14(2) 0.13(2) 0.14(2) 0.08(2) -0.04(2) -0.02(2) O(5) 0.07(1) 0.20(3) 0.08(1) 0.01(1) 0.05(1) 0.02(1) O(6) 0.12(2) 0.09(2) 0.06(1) -0.01(1) -0.01(1) 0.00(1) O(7) 0.09(1) 0.07(1) 0.17(2) -0.02(1) 0.05(1) 0.02(1) O(8) 0.12(1) 0.06(1) 0.09(1) 0.03(1) 0.05(1) 0.01(1) O(9) 0.10(1) 0.11(2) 0.13(2) 0.04(1) 0.00(1) 0.07(1) C(1) 0.04(1) 0.06(2) 0.06(2) 0.01(1) 0.00(1) 0.01(1) C(2) 0.06(1) 0.01(1) 0.12(2) -0.02(1) 0.03(2) -0.03(1) C(3) 0.04(1) 0.05(2) 0.06(1) 0.00(1) 0.01(1) 0.01(1) C(4) 0.08(2) 0.10(3) 0.07(2) 0.04(2) -0.02(2) -0.02(2) C(5) 0.05(1) 0.16(3) 0.04(1) 0.01(2) 0.01(1) -0.03(2) C(6) 0.07(2) 0.09(2) 0.05(1) 0.01(2) 0.00(1) 0.02(1) C(7) 0.06(1) 0.04(2) 0.07(2) 0.00(1) 0.01(1) 0.02(1) C(8) 0.05(1) 0.05(1) 0.04(1) 0.01(1) 0.02(1) 0.02(1) C(9) 0.06(1) 0.03(1) 0.05(1) 0.00(1) 0.02(1) 0.01(1) C(10) 0.06(1) 0.03(1) 0.06(1) 0.01(1) 0.01(1) 0.01(1) C(11) 0.06(1) 0.03(1) 0.06(1) 0.00(1) 0.01(1) 0.01(1) C(12) 0.09(2) 0.09(2) 0.04(1) 0.01(2) -0.03(1) 0.02(1) C(13) 0.07(2) 0.07(2) 0.08(2) 0.01(1) 0.04(1) 0.00(1) C(14) 0.07(1) 0.06(2) 0.10(2) 0.03(1) 0.00(1) 0.03(2) C(15) 0.06(1) 0.08(2) 0.05(1) 0.02(1) 0.01(1) 0.00(1) C(16) 0.05(1) 0.06(2) 0.05(1) 0.01(1) 0.02(1) 0.01(1) C(17) 0.06(1) 0.09(2) 0.04(1) 0.03(1) 0.00(1) 0.01(1) C(18) 0.04(1) 0.05(2) 0.04(1) 0.01(1) 0.005(10) 0.01(1) C(19) 0.06(1) 0.08(2) 0.04(1) 0.02(1) 0.02(1) 0.03(1) C(20) 0.06(1) 0.15(3) 0.07(2) 0.03(2) 0.00(1) 0.04(2) C(21) 0.12(2) 0.07(2) 0.09(2) 0.02(2) 0.00(2) 0.06(2) C(22) 0.06(1) 0.07(2) 0.09(2) -0.01(1) 0.02(1) 0.00(2) C(24) 0.06(2) 0.11(3) 0.08(2) 0.01(2) 0.02(2) -0.03(2) C(25) 0.11(3) 0.22(5) 0.07(2) 0.10(3) 0.00(2) 0.03(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4114 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0475 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0547 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.280 _refine_ls_shift/esd_max 0.0030 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.37 _refine_diff_density_max 1.51 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re(1) Se(1) 2.588(3) ? ? yes Re(1) Se(2) 2.579(2) ? ? yes Re(1) Se(3) 2.587(2) ? ? yes Re(1) C(1) 1.91(2) ? ? yes Re(1) C(2) 1.86(2) ? ? yes Re(1) C(3) 1.86(3) ? ? yes Re(2) Se(4) 2.579(3) ? ? yes Re(2) Se(5) 2.594(2) ? ? yes Re(2) Se(6) 2.578(3) ? ? yes Re(2) C(4) 1.93(3) ? ? yes Re(2) C(5) 1.98(3) ? ? yes Re(2) C(6) 1.95(3) ? ? yes Se(1) C(11) 1.95(2) ? ? yes Se(1) C(13) 1.93(2) ? ? yes Se(2) C(9) 1.97(2) ? ? yes Se(2) C(12) 1.94(2) ? ? yes Se(3) C(10) 1.99(2) ? ? yes Se(3) C(14) 1.93(2) ? ? yes Se(4) C(18) 1.98(2) ? ? yes Se(4) C(20) 1.92(2) ? ? yes Se(5) C(17) 1.97(2) ? ? yes Se(5) C(22) 1.95(3) ? ? yes Se(6) C(19) 1.98(2) ? ? yes Se(6) C(21) 1.97(3) ? ? yes S(1) O(7) 1.41(2) ? ? yes S(1) O(8) 1.40(1) ? ? yes S(1) O(9) 1.42(2) ? ? yes S(1) C(24) 1.77(3) ? ? yes S(2) O(10) 1.40(3) ? ? yes S(2) O(11) 1.39(4) ? ? yes S(2) O(12) 1.46(3) ? ? yes S(2) O(13) 1.47(7) ? ? yes S(2) O(14) 1.45(8) ? ? yes S(2) O(15) 1.26(9) ? ? yes S(2) C(25) 1.77(3) ? ? yes F(1) C(24) 1.46(4) ? ? yes F(2) C(24) 1.15(5) ? ? yes F(3) C(24) 1.30(4) ? ? yes F(4) C(24) 1.41(5) ? ? yes F(5) C(24) 1.28(5) ? ? yes F(6) C(24) 1.38(4) ? ? yes F(7) C(25) 1.34(5) ? ? yes F(9) C(25) 1.35(4) ? ? yes F(11) C(25) 1.20(3) ? ? yes O(1) C(1) 1.15(2) ? ? yes O(2) C(2) 1.20(2) ? ? yes O(3) C(3) 1.19(3) ? ? yes O(4) C(4) 1.13(3) ? ? yes O(5) C(5) 1.13(3) ? ? yes O(6) C(6) 1.15(3) ? ? yes C(8) C(9) 1.51(3) ? ? yes C(8) C(10) 1.55(3) ? ? yes C(8) C(11) 1.56(3) ? ? yes C(15) C(16) 1.55(3) ? ? yes C(16) C(17) 1.52(3) ? ? yes C(16) C(18) 1.55(3) ? ? yes C(16) C(19) 1.52(3) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se(1) Re(1) Se(2) 87.94(8) ? ? ? yes Se(1) Re(1) Se(3) 87.96(8) ? ? ? yes Se(1) Re(1) C(1) 87.2(7) ? ? ? yes Se(1) Re(1) C(2) 91.2(7) ? ? ? yes Se(1) Re(1) C(3) 177.4(6) ? ? ? yes Se(2) Re(1) Se(3) 87.76(7) ? ? ? yes Se(2) Re(1) C(1) 91.9(6) ? ? ? yes Se(2) Re(1) C(2) 178.6(6) ? ? ? yes Se(2) Re(1) C(3) 89.7(6) ? ? ? yes Se(3) Re(1) C(1) 175.1(7) ? ? ? yes Se(3) Re(1) C(2) 91.1(7) ? ? ? yes Se(3) Re(1) C(3) 90.9(6) ? ? ? yes C(1) Re(1) C(2) 89.2(9) ? ? ? yes C(1) Re(1) C(3) 94.0(9) ? ? ? yes C(2) Re(1) C(3) 91.1(10) ? ? ? yes Se(4) Re(2) Se(5) 87.68(8) ? ? ? yes Se(4) Re(2) Se(6) 89.08(8) ? ? ? yes Se(4) Re(2) C(4) 176.8(9) ? ? ? yes Se(4) Re(2) C(5) 86.8(9) ? ? ? yes Se(4) Re(2) C(6) 93.7(8) ? ? ? yes Se(5) Re(2) Se(6) 87.09(8) ? ? ? yes Se(5) Re(2) C(4) 89.9(7) ? ? ? yes Se(5) Re(2) C(5) 94.2(6) ? ? ? yes Se(5) Re(2) C(6) 176.1(7) ? ? ? yes Se(6) Re(2) C(4) 92.9(10) ? ? ? yes Se(6) Re(2) C(5) 175.6(9) ? ? ? yes Se(6) Re(2) C(6) 89.3(7) ? ? ? yes C(4) Re(2) C(5) 91(1) ? ? ? yes C(4) Re(2) C(6) 88(1) ? ? ? yes C(5) Re(2) C(6) 89.5(9) ? ? ? yes Re(1) Se(1) C(11) 108.7(6) ? ? ? yes Re(1) Se(1) C(13) 105.1(8) ? ? ? yes C(11) Se(1) C(13) 100.1(9) ? ? ? yes Re(1) Se(2) C(9) 108.5(5) ? ? ? yes Re(1) Se(2) C(12) 104.3(7) ? ? ? yes C(9) Se(2) C(12) 100.1(10) ? ? ? yes Re(1) Se(3) C(10) 108.8(6) ? ? ? yes Re(1) Se(3) C(14) 104.7(7) ? ? ? yes C(10) Se(3) C(14) 98.8(9) ? ? ? yes Re(2) Se(4) C(18) 108.9(6) ? ? ? yes Re(2) Se(4) C(20) 107.7(9) ? ? ? yes C(18) Se(4) C(20) 99.3(9) ? ? ? yes Re(2) Se(5) C(17) 108.5(6) ? ? ? yes Re(2) Se(5) C(22) 107.5(7) ? ? ? yes C(17) Se(5) C(22) 97.1(10) ? ? ? yes Re(2) Se(6) C(19) 108.6(6) ? ? ? yes Re(2) Se(6) C(21) 104.9(8) ? ? ? yes C(19) Se(6) C(21) 98(1) ? ? ? yes O(7) S(1) O(8) 116(1) ? ? ? yes O(7) S(1) O(9) 113(1) ? ? ? yes O(7) S(1) C(24) 102(1) ? ? ? yes O(8) S(1) O(9) 113(1) ? ? ? yes O(8) S(1) C(24) 105(1) ? ? ? yes O(9) S(1) C(24) 103(1) ? ? ? yes O(10) S(2) O(11) 119(1) ? ? ? yes O(10) S(2) O(12) 115(1) ? ? ? yes O(10) S(2) O(15) 139(4) ? ? ? yes O(10) S(2) C(25) 110(1) ? ? ? yes O(11) S(2) O(12) 107(2) ? ? ? yes O(11) S(2) O(13) 149(3) ? ? ? yes O(11) S(2) C(25) 102(2) ? ? ? yes O(12) S(2) O(13) 98(3) ? ? ? yes O(12) S(2) O(14) 138(3) ? ? ? yes O(12) S(2) C(25) 99(1) ? ? ? yes O(13) S(2) O(14) 111(4) ? ? ? yes O(13) S(2) O(15) 129(5) ? ? ? yes O(13) S(2) C(25) 88(3) ? ? ? yes O(14) S(2) O(15) 112(4) ? ? ? yes O(14) S(2) C(25) 107(3) ? ? ? yes O(15) S(2) C(25) 100(3) ? ? ? yes Re(1) C(1) O(1) 176(1) ? ? ? yes Re(1) C(2) O(2) 175(2) ? ? ? yes Re(1) C(3) O(3) 179(2) ? ? ? yes Re(2) C(4) O(4) 177(2) ? ? ? yes Re(2) C(5) O(5) 174(2) ? ? ? yes Re(2) C(6) O(6) 173(2) ? ? ? yes C(7) C(8) C(9) 105(1) ? ? ? yes C(7) C(8) C(10) 104(1) ? ? ? yes C(7) C(8) C(11) 105(1) ? ? ? yes C(9) C(8) C(10) 113(1) ? ? ? yes C(9) C(8) C(11) 114(1) ? ? ? yes C(10) C(8) C(11) 112(1) ? ? ? yes Se(2) C(9) C(8) 121(1) ? ? ? yes Se(3) C(10) C(8) 120(1) ? ? ? yes Se(1) C(11) C(8) 122(1) ? ? ? yes C(15) C(16) C(17) 104(1) ? ? ? yes C(15) C(16) C(18) 104(1) ? ? ? yes C(15) C(16) C(19) 105(1) ? ? ? yes C(17) C(16) C(18) 112(1) ? ? ? yes C(17) C(16) C(19) 114(2) ? ? ? yes C(18) C(16) C(19) 113(1) ? ? ? yes Se(5) C(17) C(16) 122(1) ? ? ? yes Se(4) C(18) C(16) 121(1) ? ? ? yes Se(6) C(19) C(16) 121(1) ? ? ? yes S(1) C(24) F(1) 110(1) ? ? ? yes S(1) C(24) F(2) 110(3) ? ? ? yes S(1) C(24) F(3) 119(2) ? ? ? yes S(1) C(24) F(4) 108(2) ? ? ? yes S(1) C(24) F(5) 111(2) ? ? ? yes S(1) C(24) F(6) 112(2) ? ? ? yes F(1) C(24) F(2) 19(3) ? ? ? yes F(1) C(24) F(3) 101(2) ? ? ? yes F(1) C(24) F(4) 125(3) ? ? ? yes F(1) C(24) F(5) 114(3) ? ? ? yes F(1) C(24) F(6) 91(2) ? ? ? yes F(2) C(24) F(3) 85(3) ? ? ? yes F(2) C(24) F(4) 109(3) ? ? ? yes F(2) C(24) F(5) 127(5) ? ? ? yes F(2) C(24) F(6) 108(4) ? ? ? yes F(3) C(24) F(4) 24(2) ? ? ? yes F(3) C(24) F(5) 99(3) ? ? ? yes F(3) C(24) F(6) 116(2) ? ? ? yes F(4) C(24) F(5) 85(2) ? ? ? yes F(4) C(24) F(6) 107(2) ? ? ? yes F(5) C(24) F(6) 24(2) ? ? ? yes S(2) C(25) F(7) 109(3) ? ? ? yes S(2) C(25) F(9) 108(2) ? ? ? yes S(2) C(25) F(11) 117(2) ? ? ? yes F(7) C(25) F(9) 104(3) ? ? ? yes F(7) C(25) F(11) 105(3) ? ? ? yes F(9) C(25) F(11) 110(3) ? ? ? yes #------------------------------------------------------------------------------ _publ_contact_author ; De G. Reid Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [Re(CO)3{MeC(CH2SeMe)3}]CF3SO3 ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_sdose3 #[Mn(CO)~3~{MeC(CH~2~SeMe)~3~}]CF~3~SO~3~' #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jan 25 14:18:04 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.403(3) _cell_length_b 12.139(5) _cell_length_c 9.124(4) _cell_angle_alpha 100.15(3) _cell_angle_beta 94.76(4) _cell_angle_gamma 80.92(3) _cell_volume 1010.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 20 _cell_measurement_2theta_min 22.3 _cell_measurement_2theta_max 31.1 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 2.100 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 639.14 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H18 F3 Mn O6 S Se3 ' _chemical_formula_moiety '?' _chemical_formula_structural '[Mn(CO)~3~{MeC(CH~2~SeMe)~3~}]CF~3~SO~3~' _chemical_compound_source 'diffusion of pet ether into CHCl~3~ soln' _exptl_crystal_F_000 616.00 _exptl_absorpt_coefficient_mu 6.127 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.419 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150.0 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -5.39 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 3 -1 3 2 0 4 2 -1 _diffrn_reflns_number 3800 _reflns_number_total 3563 _reflns_number_observed 2538 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_2theta_max 25.05 _diffrn_reflns_2theta_min ? _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.10442 _diffrn_orient_matrix_UB_12 -0.03062 _diffrn_orient_matrix_UB_13 -0.01087 _diffrn_orient_matrix_UB_21 -0.01588 _diffrn_orient_matrix_UB_22 -0.00931 _diffrn_orient_matrix_UB_23 -0.11097 _diffrn_orient_matrix_UB_31 0.02193 _diffrn_orient_matrix_UB_32 0.07831 _diffrn_orient_matrix_UB_33 0.00253 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 24 0.003 0.002 'International Tables' H 0 36 0.000 0.000 'International Tables' O 0 12 0.011 0.006 'International Tables' Se 0 6 -0.093 2.226 'International Tables' F 0 6 0.017 0.010 'International Tables' S 0 2 0.125 0.123 'International Tables' Mn 0 2 0.337 0.728 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Se(1) 0.55369(7) 0.74509(6) 0.75977(8) 0.0226(2) Uij ? ? Se(2) 0.91974(8) 0.70452(7) 0.70951(9) 0.0271(2) Uij ? ? Se(3) 0.68305(7) 0.90145(6) 0.53295(8) 0.0209(2) Uij ? ? Mn(1) 0.7404(1) 0.87013(9) 0.7905(1) 0.0211(3) Uij ? ? S(1) 0.7988(2) 0.2885(2) 0.7195(2) 0.0288(5) Uij ? ? F(1) 0.7630(6) 0.4162(4) 0.9818(6) 0.056(2) Uij ? ? F(2) 0.5957(6) 0.3131(5) 0.9073(6) 0.059(2) Uij ? ? F(3) 0.8044(6) 0.2367(5) 0.9877(6) 0.063(2) Uij ? ? O(1) 0.9864(6) 1.0005(5) 0.8314(6) 0.038(2) Uij ? ? O(2) 0.5368(6) 1.0770(5) 0.8872(7) 0.046(2) Uij ? ? O(3) 0.7836(6) 0.8338(6) 1.1020(6) 0.047(2) Uij ? ? O(4) 0.9498(6) 0.2984(5) 0.7435(7) 0.046(2) Uij ? ? O(5) 0.7133(6) 0.3782(4) 0.6525(6) 0.037(2) Uij ? ? O(6) 0.7662(6) 0.1765(4) 0.6616(7) 0.045(2) Uij ? ? C(1) 0.8892(8) 0.9523(7) 0.8145(8) 0.028(2) Uij ? ? C(2) 0.6154(8) 0.9953(7) 0.8474(8) 0.030(2) Uij ? ? C(3) 0.7695(8) 0.8468(7) 0.9813(9) 0.033(2) Uij ? ? C(4) 0.6709(8) 0.5506(7) 0.3301(9) 0.033(2) Uij ? ? C(5) 0.6908(8) 0.6459(6) 0.4656(8) 0.025(2) Uij ? ? C(6) 0.5850(7) 0.6320(6) 0.5760(8) 0.024(2) Uij ? ? C(7) 0.8492(8) 0.6198(6) 0.5196(9) 0.032(2) Uij ? ? C(8) 0.6515(8) 0.7571(6) 0.4053(8) 0.024(2) Uij ? ? C(9) 0.3728(8) 0.8301(7) 0.6967(9) 0.033(2) Uij ? ? C(10) 0.9046(9) 0.5947(7) 0.837(1) 0.039(3) Uij ? ? C(11) 0.8642(8) 0.9218(6) 0.4630(9) 0.030(2) Uij ? ? C(12) 0.7383(10) 0.3140(7) 0.9090(10) 0.039(3) Uij ? ? H(1) 0.7251 0.5580 0.2383 0.0447 Uiso ? ? H(2) 0.7192 0.4745 0.3672 0.0447 Uiso ? ? H(3) 0.5767 0.5616 0.2796 0.0380 Uiso ? ? H(4) 0.6089 0.5570 0.5998 0.0380 Uiso ? ? H(5) 0.4748 0.6420 0.5329 0.0447 Uiso ? ? H(6) 0.9102 0.6323 0.4415 0.0447 Uiso ? ? H(7) 0.8751 0.5403 0.5243 0.0447 Uiso ? ? H(8) 0.6951 0.7691 0.3188 0.0380 Uiso ? ? H(9) 0.5284 0.7665 0.3685 0.0447 Uiso ? ? H(10) 0.3847 0.8628 0.6108 0.0389 Uiso ? ? H(11) 0.2995 0.7832 0.6727 0.0389 Uiso ? ? H(12) 0.3404 0.8913 0.7747 0.0389 Uiso ? ? H(13) 0.9355 0.6218 0.9389 0.0463 Uiso ? ? H(14) 0.8069 0.5811 0.8373 0.0463 Uiso ? ? H(15) 0.9634 0.5242 0.8052 0.0463 Uiso ? ? H(16) 0.8546 0.9263 0.3585 0.0349 Uiso ? ? H(17) 0.9377 0.8601 0.4775 0.0349 Uiso ? ? H(18) 0.8955 0.9903 0.5152 0.0349 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Se(1) 0.0222(4) 0.0291(4) 0.0187(4) -0.0078(3) 0.0026(3) 0.0058(3) Se(2) 0.0203(4) 0.0303(4) 0.0310(5) -0.0050(3) -0.0020(3) 0.0067(4) Se(3) 0.0225(4) 0.0255(4) 0.0158(4) -0.0052(3) 0.0015(3) 0.0049(3) Mn(1) 0.0233(6) 0.0267(6) 0.0147(6) -0.0087(5) 0.0008(4) 0.0029(5) S(1) 0.035(1) 0.027(1) 0.022(1) -0.0012(8) 0.0001(8) 0.0025(9) F(1) 0.090(4) 0.047(3) 0.034(3) -0.029(3) 0.014(3) -0.014(3) F(2) 0.056(3) 0.076(4) 0.051(4) -0.024(3) 0.020(3) 0.004(3) F(3) 0.096(5) 0.064(4) 0.031(3) -0.014(3) -0.007(3) 0.019(3) O(1) 0.038(3) 0.049(4) 0.031(4) -0.025(3) -0.002(3) 0.007(3) O(2) 0.049(4) 0.035(4) 0.053(4) 0.000(3) 0.027(3) 0.004(3) O(3) 0.050(4) 0.083(5) 0.018(3) -0.029(3) -0.007(3) 0.021(3) O(4) 0.031(3) 0.055(4) 0.051(4) 0.000(3) 0.008(3) 0.009(3) O(5) 0.046(3) 0.035(3) 0.029(3) 0.003(3) -0.005(3) 0.011(3) O(6) 0.071(4) 0.026(3) 0.035(4) -0.010(3) -0.006(3) 0.000(3) C(1) 0.030(4) 0.037(5) 0.018(4) -0.007(4) -0.003(3) 0.007(4) C(2) 0.039(5) 0.035(5) 0.017(4) -0.014(4) 0.006(3) -0.002(4) C(3) 0.031(4) 0.044(5) 0.028(5) -0.017(4) -0.004(4) 0.009(4) C(4) 0.036(5) 0.035(5) 0.025(5) -0.009(4) 0.008(4) -0.012(4) C(5) 0.033(4) 0.027(4) 0.017(4) -0.011(3) 0.002(3) 0.000(3) C(6) 0.025(4) 0.027(4) 0.021(4) -0.009(3) 0.005(3) 0.002(3) C(7) 0.027(4) 0.031(4) 0.036(5) -0.004(3) 0.010(4) -0.009(4) C(8) 0.043(4) 0.024(4) 0.010(4) -0.019(3) 0.001(3) 0.002(3) C(9) 0.025(4) 0.035(5) 0.037(5) -0.001(3) 0.003(4) 0.000(4) C(10) 0.040(5) 0.038(5) 0.043(6) -0.004(4) -0.008(4) 0.019(4) C(11) 0.037(5) 0.034(5) 0.021(4) -0.014(4) 0.007(3) -0.003(4) C(12) 0.055(6) 0.037(5) 0.029(5) -0.018(4) 0.001(4) 0.002(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2538 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0384 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0417 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.715 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.78 _refine_diff_density_max 1.15 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se(1) Mn(1) 2.464(1) ? ? yes Se(1) C(6) 1.981(7) ? ? yes Se(1) C(9) 1.945(7) ? ? yes Se(2) Mn(1) 2.459(1) ? ? yes Se(2) C(7) 1.974(8) ? ? yes Se(2) C(10) 1.946(8) ? ? yes Se(3) Mn(1) 2.449(1) ? ? yes Se(3) C(8) 1.975(7) ? ? yes Se(3) C(11) 1.934(7) ? ? yes Mn(1) C(1) 1.821(8) ? ? yes Mn(1) C(2) 1.793(8) ? ? yes Mn(1) C(3) 1.804(8) ? ? yes S(1) O(4) 1.439(6) ? ? yes S(1) O(5) 1.443(5) ? ? yes S(1) O(6) 1.440(6) ? ? yes S(1) C(12) 1.824(9) ? ? yes F(1) C(12) 1.344(9) ? ? yes F(2) C(12) 1.342(9) ? ? yes F(3) C(12) 1.327(10) ? ? yes O(1) C(1) 1.147(8) ? ? yes O(2) C(2) 1.161(9) ? ? yes O(3) C(3) 1.134(9) ? ? yes C(4) C(5) 1.558(10) ? ? yes C(5) C(6) 1.521(10) ? ? yes C(5) C(7) 1.532(10) ? ? yes C(5) C(8) 1.527(10) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Mn(1) Se(1) C(6) 109.1(2) ? ? ? yes Mn(1) Se(1) C(9) 107.9(2) ? ? ? yes C(6) Se(1) C(9) 98.9(3) ? ? ? yes Mn(1) Se(2) C(7) 109.5(2) ? ? ? yes Mn(1) Se(2) C(10) 106.2(3) ? ? ? yes C(7) Se(2) C(10) 98.1(4) ? ? ? yes Mn(1) Se(3) C(8) 109.4(2) ? ? ? yes Mn(1) Se(3) C(11) 104.7(2) ? ? ? yes C(8) Se(3) C(11) 100.2(3) ? ? ? yes Se(1) Mn(1) Se(2) 89.19(5) ? ? ? yes Se(1) Mn(1) Se(3) 89.18(4) ? ? ? yes Se(1) Mn(1) C(1) 175.3(2) ? ? ? yes Se(1) Mn(1) C(2) 93.5(2) ? ? ? yes Se(1) Mn(1) C(3) 87.6(2) ? ? ? yes Se(2) Mn(1) Se(3) 91.45(4) ? ? ? yes Se(2) Mn(1) C(1) 86.5(2) ? ? ? yes Se(2) Mn(1) C(2) 177.2(2) ? ? ? yes Se(2) Mn(1) C(3) 90.8(3) ? ? ? yes Se(3) Mn(1) C(1) 92.7(2) ? ? ? yes Se(3) Mn(1) C(2) 87.7(2) ? ? ? yes Se(3) Mn(1) C(3) 176.0(2) ? ? ? yes C(1) Mn(1) C(2) 90.9(3) ? ? ? yes C(1) Mn(1) C(3) 90.7(3) ? ? ? yes C(2) Mn(1) C(3) 90.2(4) ? ? ? yes O(4) S(1) O(5) 114.4(4) ? ? ? yes O(4) S(1) O(6) 115.5(4) ? ? ? yes O(4) S(1) C(12) 102.6(4) ? ? ? yes O(5) S(1) O(6) 115.3(3) ? ? ? yes O(5) S(1) C(12) 103.4(4) ? ? ? yes O(6) S(1) C(12) 103.0(4) ? ? ? yes Mn(1) C(1) O(1) 177.3(7) ? ? ? yes Mn(1) C(2) O(2) 178.3(7) ? ? ? yes Mn(1) C(3) O(3) 177.8(7) ? ? ? yes C(4) C(5) C(6) 104.6(6) ? ? ? yes C(4) C(5) C(7) 104.4(6) ? ? ? yes C(4) C(5) C(8) 105.9(6) ? ? ? yes C(6) C(5) C(7) 113.6(6) ? ? ? yes C(6) C(5) C(8) 112.5(6) ? ? ? yes C(7) C(5) C(8) 114.7(6) ? ? ? yes Se(1) C(6) C(5) 120.1(5) ? ? ? yes Se(2) C(7) C(5) 119.6(5) ? ? ? yes Se(3) C(8) C(5) 120.2(5) ? ? ? yes S(1) C(12) F(1) 111.1(6) ? ? ? yes S(1) C(12) F(2) 110.7(6) ? ? ? yes S(1) C(12) F(3) 111.9(6) ? ? ? yes F(1) C(12) F(2) 106.8(7) ? ? ? yes F(1) C(12) F(3) 108.0(7) ? ? ? yes F(2) C(12) F(3) 108.2(7) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' J. Chem. Soc., Dalton Trans.' _publ_contact_author ; Dr G. Reid Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [Mn(CO)~3~{MeC(CH~2~SeMe)~3~}]CF~3~SO~3`. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_jc10s3 #[Mn(CO)3([10]aneS3)]2[MnBr4] #------------------------------------------------------------------------------ _audit_creation_date 'Tue Mar 16 16:20:06 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 7.430(5) _cell_length_b 28.273(3) _cell_length_c 16.075(5) _cell_angle_alpha 90 _cell_angle_beta 95.79(4) _cell_angle_gamma 90 _cell_volume 3359(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150.1 _cell_measurement_reflns_used 20 _cell_measurement_2theta_min 14.1 _cell_measurement_2theta_max 16.1 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1041.23 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H28 Br4 Mn3 O6 S6 ' _chemical_formula_moiety '?' _chemical_formula_structural '[Mn(CO)3([10]aneS3)]2[MnBr4]' _chemical_compound_source 'CH2Cl2/Et2O' _exptl_crystal_F_000 2028.00 _exptl_absorpt_coefficient_mu 6.288 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.792 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150.1 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.07 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -6 -2 1 -8 3 0 -11 1 _diffrn_reflns_number 6547 _reflns_number_total 6056 _reflns_number_observed 2629 _reflns_observed_criterion 2.50 _diffrn_reflns_av_R_equivalents 5.39 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_2theta_min ? _diffrn_reflns_2theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.04911 _diffrn_orient_matrix_UB_12 -0.03110 _diffrn_orient_matrix_UB_13 -0.02149 _diffrn_orient_matrix_UB_21 0.03497 _diffrn_orient_matrix_UB_22 0.00789 _diffrn_orient_matrix_UB_23 -0.05684 _diffrn_orient_matrix_UB_31 0.12111 _diffrn_orient_matrix_UB_32 -0.01489 _diffrn_orient_matrix_UB_33 0.01475 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 80 0.003 0.002 'International Tables' H 0 112 0.000 0.000 'International Tables' O 0 24 0.011 0.006 'International Tables' S 0 24 0.125 0.123 'International Tables' Mn 0 12 0.337 0.728 'International Tables' Br 0 16 -0.290 2.459 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Br(1) 0.1642(2) 0.20560(5) 0.31463(7) 0.0394(4) Uij ? ? Br(2) 0.6461(2) 0.25987(4) 0.39522(7) 0.0388(4) Uij ? ? Br(3) 0.2672(2) 0.26847(5) 0.55391(7) 0.0497(4) Uij ? ? Br(4) 0.2294(2) 0.35390(5) 0.35148(8) 0.0441(4) Uij ? ? Mn(1) 0.7558(3) 0.06058(6) 0.1662(1) 0.0338(5) Uij ? ? Mn(2) 0.7909(3) 0.07855(6) 0.6036(1) 0.0476(6) Uij ? ? Mn(3) 0.3132(2) 0.27161(6) 0.4003(1) 0.0311(5) Uij ? ? S(1) 0.5189(5) 0.0577(1) 0.0588(2) 0.0396(9) Uij ? ? S(2) 0.8988(4) 0.1240(1) 0.1059(2) 0.0423(10) Uij ? ? S(3) 0.5923(4) 0.1168(1) 0.2298(2) 0.0354(9) Uij ? ? S(4) 0.9650(5) 0.1476(1) 0.6151(2) 0.048(1) Uij ? ? S(5) 0.5092(6) 0.1172(1) 0.6217(3) 0.068(1) Uij ? ? S(6) 0.7204(4) 0.0965(1) 0.4629(2) 0.0395(9) Uij ? ? O(1) 0.953(2) -0.0103(5) 0.0781(6) 0.153(6) Uij ? ? O(2) 1.047(1) 0.0605(3) 0.3060(6) 0.063(3) Uij ? ? O(3) 0.579(2) -0.0176(3) 0.2491(5) 0.077(4) Uij ? ? O(4) 1.120(1) 0.0284(3) 0.5678(6) 0.075(4) Uij ? ? O(5) 0.590(1) -0.0111(3) 0.5898(5) 0.060(3) Uij ? ? O(6) 0.866(2) 0.0570(4) 0.7827(6) 0.114(5) Uij ? ? C(1) 0.596(2) 0.0708(4) -0.0426(7) 0.031(3) Uij ? ? C(2) 0.694(2) 0.1151(4) -0.0526(7) 0.034(3) Uij ? ? C(3) 0.877(2) 0.1219(5) -0.0071(7) 0.045(3) Uij ? ? C(4) 0.767(2) 0.1781(4) 0.1225(7) 0.041(3) Uij ? ? C(5) 0.685(2) 0.1739(4) 0.2063(7) 0.039(3) Uij ? ? C(6) 0.371(2) 0.1166(5) 0.1682(7) 0.044(3) Uij ? ? C(7) 0.380(2) 0.1105(4) 0.0748(7) 0.041(3) Uij ? ? C(8) 0.648(2) 0.0139(5) 0.2175(8) 0.051(4) Uij ? ? C(9) 0.880(2) 0.0187(6) 0.1132(9) 0.069(5) Uij ? ? C(10) 0.935(2) 0.0614(4) 0.2517(8) 0.042(3) Uij ? ? C(11) 0.885(2) 0.1877(4) 0.6911(7) 0.038(3) Uij ? ? C(12) 0.688(2) 0.1985(5) 0.6802(8) 0.048(4) Uij ? ? C(13) 0.549(2) 0.1642(6) 0.6929(9) 0.073(5) Uij ? ? C(14) 0.439(2) 0.1477(5) 0.5209(9) 0.064(4) Uij ? ? C(15) 0.504(2) 0.1245(5) 0.4518(9) 0.062(4) Uij ? ? C(16) 0.874(2) 0.1446(4) 0.4460(7) 0.037(3) Uij ? ? C(17) 0.902(2) 0.1791(4) 0.5171(7) 0.037(3) Uij ? ? C(18) 0.663(2) 0.0233(5) 0.5918(8) 0.045(4) Uij ? ? C(19) 0.994(2) 0.0474(5) 0.5837(8) 0.045(4) Uij ? ? C(20) 0.830(2) 0.0666(5) 0.7124(10) 0.069(5) Uij ? ? H(1) 0.4909 0.0711 -0.0819 0.0395 Uiso ? ? H(2) 0.6726 0.0456 -0.0552 0.0395 Uiso ? ? H(3) 0.7060 0.1185 -0.1105 0.0402 Uiso ? ? H(4) 0.6196 0.1401 -0.0352 0.0402 Uiso ? ? H(5) 0.9495 0.0958 -0.0221 0.0554 Uiso ? ? H(6) 0.9250 0.1502 -0.0260 0.0554 Uiso ? ? H(7) 0.8430 0.2048 0.1242 0.0508 Uiso ? ? H(8) 0.6719 0.1812 0.0787 0.0508 Uiso ? ? H(9) 0.7765 0.1813 0.2494 0.0482 Uiso ? ? H(10) 0.5896 0.1964 0.2057 0.0482 Uiso ? ? H(11) 0.3146 0.1461 0.1773 0.0549 Uiso ? ? H(12) 0.3027 0.0917 0.1879 0.0549 Uiso ? ? H(13) 0.4355 0.1376 0.0536 0.0534 Uiso ? ? H(14) 0.2628 0.1064 0.0485 0.0534 Uiso ? ? H(15) 0.9452 0.2166 0.6879 0.0507 Uiso ? ? H(16) 0.9113 0.1739 0.7449 0.0507 Uiso ? ? H(17) 0.6692 0.2233 0.7169 0.0663 Uiso ? ? H(18) 0.6603 0.2076 0.6242 0.0663 Uiso ? ? H(19) 0.4294 0.1815 0.6919 0.0832 Uiso ? ? H(20) 0.5652 0.1509 0.7485 0.0832 Uiso ? ? H(21) 0.4798 0.1780 0.5257 0.1121 Uiso ? ? H(22) 0.3095 0.1460 0.5146 0.1121 Uiso ? ? H(23) 0.4156 0.1022 0.4322 0.0728 Uiso ? ? H(24) 0.5073 0.1495 0.4116 0.0728 Uiso ? ? H(25) 0.8288 0.1610 0.3971 0.0462 Uiso ? ? H(26) 0.9891 0.1310 0.4376 0.0462 Uiso ? ? H(27) 0.9961 0.2004 0.5067 0.0423 Uiso ? ? H(28) 0.7933 0.1960 0.5208 0.0423 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0466(8) 0.0413(8) 0.0306(6) -0.0067(7) 0.0052(6) -0.0090(6) Br(2) 0.0392(7) 0.0349(7) 0.0426(7) 0.0067(6) 0.0053(6) 0.0041(6) Br(3) 0.0550(9) 0.0661(10) 0.0295(6) -0.0160(8) 0.0109(6) -0.0080(7) Br(4) 0.0439(9) 0.0406(8) 0.0459(8) 0.0070(7) -0.0046(7) -0.0049(6) Mn(1) 0.038(1) 0.032(1) 0.034(1) 0.0099(9) 0.0173(8) 0.0079(8) Mn(2) 0.087(2) 0.026(1) 0.0334(9) 0.020(1) 0.023(1) 0.0058(9) Mn(3) 0.0347(10) 0.0329(10) 0.0258(8) 0.0006(9) 0.0036(8) -0.0048(8) S(1) 0.048(2) 0.034(2) 0.038(2) -0.013(2) 0.013(1) -0.003(2) S(2) 0.025(2) 0.050(2) 0.052(2) 0.000(2) 0.005(2) 0.022(2) S(3) 0.035(2) 0.039(2) 0.033(2) 0.010(1) 0.006(1) -0.006(1) S(4) 0.069(3) 0.035(2) 0.040(2) 0.023(1) 0.003(2) 0.006(2) S(5) 0.092(3) 0.039(2) 0.080(3) 0.011(2) 0.046(2) 0.010(2) S(6) 0.037(2) 0.044(2) 0.039(1) 0.011(2) 0.009(1) 0.020(2) O(1) 0.28(2) 0.14(1) 0.045(7) 0.14(1) 0.057(9) 0.034(7) O(2) 0.041(6) 0.082(7) 0.065(6) 0.010(6) -0.006(5) 0.033(6) O(3) 0.128(10) 0.064(7) 0.042(5) -0.038(7) 0.020(6) 0.015(5) O(4) 0.068(8) 0.066(7) 0.086(7) 0.025(6) -0.017(6) -0.035(6) O(5) 0.092(8) 0.038(6) 0.047(6) 0.001(6) 0.000(5) 0.001(5) O(6) 0.25(2) 0.062(7) 0.025(6) -0.002(9) -0.016(7) 0.000(5) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2629 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0619 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0682 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.850 _refine_ls_shift/esd_max 0.0158 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.17 _refine_diff_density_max 4.04 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) Mn(3) 2.510(3) ? ? yes Br(2) Mn(3) 2.505(3) ? ? yes Br(3) Mn(3) 2.528(3) ? ? yes Br(4) Mn(3) 2.513(3) ? ? yes Mn(1) S(1) 2.338(5) ? ? yes Mn(1) S(2) 2.343(5) ? ? yes Mn(1) S(3) 2.303(5) ? ? yes Mn(1) C(8) 1.79(2) ? ? yes Mn(1) C(9) 1.77(2) ? ? yes Mn(1) C(10) 1.82(2) ? ? yes Mn(2) S(4) 2.339(6) ? ? yes Mn(2) S(5) 2.405(6) ? ? yes Mn(2) S(6) 2.325(5) ? ? yes Mn(2) C(18) 1.83(2) ? ? yes Mn(2) C(19) 1.80(2) ? ? yes Mn(2) C(20) 1.78(2) ? ? yes S(1) C(1) 1.82(1) ? ? yes S(1) C(7) 1.85(2) ? ? yes S(2) C(3) 1.81(2) ? ? yes S(2) C(4) 1.85(2) ? ? yes S(3) C(5) 1.81(2) ? ? yes S(3) C(6) 1.83(2) ? ? yes S(4) C(11) 1.81(2) ? ? yes S(4) C(17) 1.83(2) ? ? yes S(5) C(13) 1.76(2) ? ? yes S(5) C(14) 1.86(2) ? ? yes S(6) C(15) 1.79(2) ? ? yes S(6) C(16) 1.82(2) ? ? yes O(1) C(9) 1.16(2) ? ? yes O(2) C(10) 1.14(2) ? ? yes O(3) C(8) 1.17(2) ? ? yes O(4) C(19) 1.13(2) ? ? yes O(5) C(18) 1.11(2) ? ? yes O(6) C(20) 1.17(2) ? ? yes C(1) C(2) 1.46(2) ? ? yes C(2) C(3) 1.49(2) ? ? yes C(4) C(5) 1.54(2) ? ? yes C(6) C(7) 1.52(2) ? ? yes C(11) C(12) 1.48(2) ? ? yes C(12) C(13) 1.45(2) ? ? yes C(14) C(15) 1.41(2) ? ? yes C(16) C(17) 1.50(2) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Mn(1) S(2) 93.4(2) ? ? ? yes S(1) Mn(1) S(3) 87.7(2) ? ? ? yes S(1) Mn(1) C(8) 88.7(6) ? ? ? yes S(1) Mn(1) C(9) 90.7(7) ? ? ? yes S(1) Mn(1) C(10) 178.0(6) ? ? ? yes S(2) Mn(1) S(3) 86.4(2) ? ? ? yes S(2) Mn(1) C(8) 176.9(6) ? ? ? yes S(2) Mn(1) C(9) 91.9(7) ? ? ? yes S(2) Mn(1) C(10) 88.6(6) ? ? ? yes S(3) Mn(1) C(8) 91.4(6) ? ? ? yes S(3) Mn(1) C(9) 177.6(7) ? ? ? yes S(3) Mn(1) C(10) 92.0(6) ? ? ? yes C(8) Mn(1) C(9) 90.3(9) ? ? ? yes C(8) Mn(1) C(10) 89.3(8) ? ? ? yes C(9) Mn(1) C(10) 89.7(9) ? ? ? yes S(4) Mn(2) S(5) 95.3(2) ? ? ? yes S(4) Mn(2) S(6) 87.9(2) ? ? ? yes S(4) Mn(2) C(18) 177.2(6) ? ? ? yes S(4) Mn(2) C(19) 87.5(6) ? ? ? yes S(4) Mn(2) C(20) 92.7(7) ? ? ? yes S(5) Mn(2) S(6) 84.5(2) ? ? ? yes S(5) Mn(2) C(18) 87.3(6) ? ? ? yes S(5) Mn(2) C(19) 175.8(6) ? ? ? yes S(5) Mn(2) C(20) 91.4(7) ? ? ? yes S(6) Mn(2) C(18) 91.3(6) ? ? ? yes S(6) Mn(2) C(19) 92.5(6) ? ? ? yes S(6) Mn(2) C(20) 175.9(7) ? ? ? yes C(18) Mn(2) C(19) 89.8(8) ? ? ? yes C(18) Mn(2) C(20) 88.3(9) ? ? ? yes C(19) Mn(2) C(20) 91.5(9) ? ? ? yes Br(1) Mn(3) Br(2) 105.4(1) ? ? ? yes Br(1) Mn(3) Br(3) 114.5(1) ? ? ? yes Br(1) Mn(3) Br(4) 115.8(1) ? ? ? yes Br(2) Mn(3) Br(3) 105.0(1) ? ? ? yes Br(2) Mn(3) Br(4) 109.1(1) ? ? ? yes Br(3) Mn(3) Br(4) 106.5(1) ? ? ? yes Mn(1) S(1) C(1) 111.9(5) ? ? ? yes Mn(1) S(1) C(7) 104.9(6) ? ? ? yes C(1) S(1) C(7) 100.9(7) ? ? ? yes Mn(1) S(2) C(3) 113.1(6) ? ? ? yes Mn(1) S(2) C(4) 107.7(5) ? ? ? yes C(3) S(2) C(4) 100.3(8) ? ? ? yes Mn(1) S(3) C(5) 107.2(5) ? ? ? yes Mn(1) S(3) C(6) 104.0(6) ? ? ? yes C(5) S(3) C(6) 103.2(8) ? ? ? yes Mn(2) S(4) C(11) 111.0(6) ? ? ? yes Mn(2) S(4) C(17) 104.3(5) ? ? ? yes C(11) S(4) C(17) 101.8(7) ? ? ? yes Mn(2) S(5) C(13) 109.4(8) ? ? ? yes Mn(2) S(5) C(14) 106.0(7) ? ? ? yes C(13) S(5) C(14) 103.3(9) ? ? ? yes Mn(2) S(6) C(15) 107.8(6) ? ? ? yes Mn(2) S(6) C(16) 103.0(5) ? ? ? yes C(15) S(6) C(16) 103.2(8) ? ? ? yes S(1) C(1) C(2) 118(1) ? ? ? yes C(1) C(2) C(3) 119(1) ? ? ? yes S(2) C(3) C(2) 118(1) ? ? ? yes S(2) C(4) C(5) 109(1) ? ? ? yes S(3) C(5) C(4) 116(1) ? ? ? yes S(3) C(6) C(7) 114(1) ? ? ? yes S(1) C(7) C(6) 108(1) ? ? ? yes Mn(1) C(8) O(3) 177(1) ? ? ? yes Mn(1) C(9) O(1) 176(2) ? ? ? yes Mn(1) C(10) O(2) 177(1) ? ? ? yes S(4) C(11) C(12) 115(1) ? ? ? yes C(11) C(12) C(13) 123(1) ? ? ? yes S(5) C(13) C(12) 119(1) ? ? ? yes S(5) C(14) C(15) 112(1) ? ? ? yes S(6) C(15) C(14) 120(1) ? ? ? yes S(6) C(16) C(17) 114(1) ? ? ? yes S(4) C(17) C(16) 110(1) ? ? ? yes Mn(2) C(18) O(5) 175(1) ? ? ? yes Mn(2) C(19) O(4) 177(1) ? ? ? yes Mn(2) C(20) O(6) 175(2) ? ? ? yes #------------------------------------------------------------------------------ _publ_contact_author ; Dr G. Reid Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [Mn(CO)3([10]aneS3)]2[MnBr4]. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_jcmns3 #[Mn(CO)3{MeS(CH2)2S(CH2)2SMe}]CF3SO3 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Mar 16 16:07:38 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 11.72(1) _cell_length_b 12.75(2) _cell_length_c 5.950(6) _cell_angle_alpha 99.04(9) _cell_angle_beta 90.2(1) _cell_angle_gamma 97.3(1) _cell_volume 871(1) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 23 _cell_measurement_2theta_min 38.9 _cell_measurement_2theta_max 44.8 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'column' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.900 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 470.39 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H14 F3 Mn O6 S4 ' _chemical_formula_moiety '?' _chemical_formula_structural '[Mn(CO)3{MeS(CH2)2S(CH2)2SMe}]CF3SO3' _chemical_compound_source 'CH2Cl2/pet ether' _exptl_crystal_F_000 476.00 _exptl_absorpt_coefficient_mu 1.241 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.669 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.27 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 4 -1 -2 3 1 -4 0 -1 _diffrn_reflns_number 3225 _reflns_number_total 3056 _reflns_number_observed 2225 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 2.47 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_2theta_min ? _diffrn_reflns_2theta_max 25.15 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.01867 _diffrn_orient_matrix_UB_12 0.06897 _diffrn_orient_matrix_UB_13 -0.04181 _diffrn_orient_matrix_UB_21 0.03857 _diffrn_orient_matrix_UB_22 -0.01599 _diffrn_orient_matrix_UB_23 -0.14880 _diffrn_orient_matrix_UB_31 -0.07457 _diffrn_orient_matrix_UB_32 -0.03744 _diffrn_orient_matrix_UB_33 -0.07133 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 20 0.003 0.002 'International Tables' H 0 28 0.000 0.000 'International Tables' F 0 6 0.017 0.010 'International Tables' O 0 12 0.011 0.006 'International Tables' S 0 8 0.125 0.123 'International Tables' Mn 0 2 0.337 0.728 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Mn(1) 0.1805(1) 0.1842(1) 0.3076(2) 0.0289(4) Uij ? ? S(1) 0.0779(2) 0.2775(2) 0.5953(4) 0.0330(7) Uij ? ? S(2) 0.2267(2) 0.3438(2) 0.1681(4) 0.0311(7) Uij ? ? S(3) 0.3448(2) 0.2433(2) 0.5587(4) 0.0332(7) Uij ? ? S(4) -0.2905(2) 0.3481(2) 0.0122(4) 0.0357(7) Uij ? ? F(1) -0.4345(5) 0.1690(5) -0.0164(9) 0.048(2) Uij ? ? F(2) -0.2726(6) 0.1516(5) -0.177(1) 0.059(2) Uij ? ? F(3) -0.2797(6) 0.1743(5) 0.187(1) 0.061(2) Uij ? ? O(1) -0.0292(7) 0.1153(6) 0.003(1) 0.046(2) Uij ? ? O(2) 0.1307(7) -0.0102(5) 0.519(1) 0.047(2) Uij ? ? O(3) 0.3112(6) 0.0702(5) -0.053(1) 0.042(2) Uij ? ? O(4) -0.3474(7) 0.3620(6) -0.193(1) 0.052(2) Uij ? ? O(5) -0.3430(7) 0.3893(6) 0.221(1) 0.054(2) Uij ? ? O(6) -0.1638(5) 0.3708(5) 0.014(1) 0.036(2) Uij ? ? C(1) 0.0529(9) 0.1442(7) 0.122(2) 0.031(3) Uij ? ? C(2) 0.1501(8) 0.0652(8) 0.435(2) 0.030(3) Uij ? ? C(3) 0.2624(9) 0.1161(7) 0.088(2) 0.033(3) Uij ? ? C(4) -0.0686(9) 0.2791(7) 0.500(2) 0.037(3) Uij ? ? C(5) 0.1383(9) 0.4150(8) 0.596(2) 0.039(3) Uij ? ? C(6) 0.1603(9) 0.4419(7) 0.360(2) 0.038(3) Uij ? ? C(7) 0.3819(8) 0.3799(7) 0.237(2) 0.031(3) Uij ? ? C(8) 0.4128(9) 0.3667(8) 0.477(2) 0.036(3) Uij ? ? C(9) 0.4515(9) 0.1551(8) 0.484(2) 0.038(3) Uij ? ? C(10) -0.3185(10) 0.2045(8) 0.003(2) 0.042(3) Uij ? ? H(1) -0.1061 0.3285 0.6020 0.0405 Uiso ? ? H(2) -0.0698 0.3001 0.3516 0.0405 Uiso ? ? H(3) -0.1119 0.2096 0.4895 0.0405 Uiso ? ? H(4) 0.0899 0.4623 0.6754 0.0442 Uiso ? ? H(5) 0.2123 0.4284 0.6802 0.0442 Uiso ? ? H(6) 0.2083 0.5098 0.3699 0.0442 Uiso ? ? H(7) 0.0876 0.4499 0.2930 0.0442 Uiso ? ? H(8) 0.4249 0.3344 0.1332 0.0316 Uiso ? ? H(9) 0.4055 0.4523 0.2152 0.0316 Uiso ? ? H(10) 0.3893 0.4263 0.5792 0.0416 Uiso ? ? H(11) 0.4945 0.3703 0.4936 0.0416 Uiso ? ? H(12) 0.4253 0.0851 0.5187 0.0413 Uiso ? ? H(13) 0.4675 0.1489 0.3267 0.0413 Uiso ? ? H(14) 0.5217 0.1814 0.5699 0.0413 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.037(1) 0.0245(8) 0.0265(8) 0.0063(7) -0.0011(6) 0.0050(6) S(1) 0.042(2) 0.032(1) 0.027(1) 0.009(1) -0.001(1) 0.0060(10) S(2) 0.038(2) 0.028(1) 0.030(1) 0.006(1) -0.001(1) 0.0084(10) S(3) 0.042(2) 0.033(1) 0.026(1) 0.009(1) -0.003(1) 0.0062(10) S(4) 0.047(2) 0.028(1) 0.033(1) 0.006(1) 0.000(1) 0.004(1) F(1) 0.047(4) 0.049(4) 0.044(3) -0.008(3) -0.009(3) 0.009(3) F(2) 0.069(5) 0.037(3) 0.067(4) 0.011(3) 0.012(4) -0.007(3) F(3) 0.067(5) 0.050(4) 0.067(4) -0.010(3) -0.028(4) 0.031(3) O(1) 0.046(5) 0.040(4) 0.049(4) 0.006(4) -0.011(4) 0.001(3) O(2) 0.064(6) 0.035(4) 0.045(4) 0.010(4) -0.001(4) 0.015(3) O(3) 0.051(5) 0.038(4) 0.039(4) 0.012(4) 0.009(4) 0.004(3) O(4) 0.063(6) 0.038(4) 0.058(5) -0.006(4) -0.017(4) 0.023(4) O(5) 0.049(5) 0.054(5) 0.052(5) -0.002(4) 0.019(4) -0.012(4) O(6) 0.014(4) 0.046(4) 0.047(4) -0.001(3) 0.007(3) 0.005(3) C(1) 0.023(6) 0.031(5) 0.041(6) 0.001(5) 0.014(5) 0.011(4) C(2) 0.026(6) 0.034(5) 0.031(5) 0.012(5) 0.000(4) 0.003(4) C(3) 0.043(7) 0.030(5) 0.029(5) 0.010(5) -0.006(5) 0.005(4) C(4) 0.041(7) 0.029(5) 0.043(6) 0.011(5) -0.003(5) 0.002(4) C(5) 0.042(7) 0.031(5) 0.042(6) 0.010(5) 0.016(5) -0.001(4) C(6) 0.042(7) 0.025(5) 0.048(6) 0.009(5) 0.006(5) 0.007(4) C(7) 0.031(6) 0.022(5) 0.039(5) -0.007(4) -0.010(4) 0.009(4) C(8) 0.035(7) 0.037(6) 0.036(5) -0.001(5) 0.000(5) 0.006(4) C(9) 0.036(7) 0.048(6) 0.033(5) 0.014(5) 0.003(5) 0.011(5) C(10) 0.050(8) 0.036(6) 0.038(6) 0.000(6) -0.012(5) 0.008(5) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2225 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0705 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0991 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 5.644 _refine_ls_shift/esd_max 0.0040 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.36 _refine_diff_density_max 0.92 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn(1) S(1) 2.352(3) ? ? yes Mn(1) S(2) 2.320(3) ? ? yes Mn(1) S(3) 2.402(4) ? ? yes Mn(1) C(1) 1.82(1) ? ? yes Mn(1) C(2) 1.797(10) ? ? yes Mn(1) C(3) 1.804(10) ? ? yes S(1) C(4) 1.81(1) ? ? yes S(1) C(5) 1.81(1) ? ? yes S(2) C(6) 1.810(10) ? ? yes S(2) C(7) 1.848(10) ? ? yes S(3) C(8) 1.809(10) ? ? yes S(3) C(9) 1.80(1) ? ? yes S(4) O(4) 1.435(7) ? ? yes S(4) O(5) 1.444(7) ? ? yes S(4) O(6) 1.476(7) ? ? yes S(4) C(10) 1.81(1) ? ? yes F(1) C(10) 1.38(1) ? ? yes F(2) C(10) 1.33(1) ? ? yes F(3) C(10) 1.32(1) ? ? yes O(1) C(1) 1.18(1) ? ? yes O(2) C(2) 1.15(1) ? ? yes O(3) C(3) 1.14(1) ? ? yes C(5) C(6) 1.51(1) ? ? yes C(7) C(8) 1.51(1) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Mn(1) S(2) 88.16(10) ? ? ? yes S(1) Mn(1) S(3) 85.2(1) ? ? ? yes S(1) Mn(1) C(1) 92.7(3) ? ? ? yes S(1) Mn(1) C(2) 89.8(3) ? ? ? yes S(1) Mn(1) C(3) 178.3(3) ? ? ? yes S(2) Mn(1) S(3) 85.73(10) ? ? ? yes S(2) Mn(1) C(1) 93.1(3) ? ? ? yes S(2) Mn(1) C(2) 175.7(3) ? ? ? yes S(2) Mn(1) C(3) 90.5(3) ? ? ? yes S(3) Mn(1) C(1) 177.6(3) ? ? ? yes S(3) Mn(1) C(2) 90.4(3) ? ? ? yes S(3) Mn(1) C(3) 93.6(3) ? ? ? yes C(1) Mn(1) C(2) 90.7(4) ? ? ? yes C(1) Mn(1) C(3) 88.5(4) ? ? ? yes C(2) Mn(1) C(3) 91.5(4) ? ? ? yes Mn(1) S(1) C(4) 110.4(3) ? ? ? yes Mn(1) S(1) C(5) 102.5(3) ? ? ? yes C(4) S(1) C(5) 101.4(5) ? ? ? yes Mn(1) S(2) C(6) 105.0(3) ? ? ? yes Mn(1) S(2) C(7) 103.7(3) ? ? ? yes C(6) S(2) C(7) 103.6(5) ? ? ? yes Mn(1) S(3) C(8) 106.3(3) ? ? ? yes Mn(1) S(3) C(9) 108.5(3) ? ? ? yes C(8) S(3) C(9) 101.8(5) ? ? ? yes O(4) S(4) O(5) 115.5(5) ? ? ? yes O(4) S(4) O(6) 115.0(4) ? ? ? yes O(4) S(4) C(10) 101.8(4) ? ? ? yes O(5) S(4) O(6) 114.8(4) ? ? ? yes O(5) S(4) C(10) 103.0(5) ? ? ? yes O(6) S(4) C(10) 104.2(5) ? ? ? yes Mn(1) C(1) O(1) 178.1(8) ? ? ? yes Mn(1) C(2) O(2) 179.2(8) ? ? ? yes Mn(1) C(3) O(3) 177.6(9) ? ? ? yes S(1) C(5) C(6) 113.4(7) ? ? ? yes S(2) C(6) C(5) 115.3(7) ? ? ? yes S(2) C(7) C(8) 112.8(7) ? ? ? yes S(3) C(8) C(7) 113.7(7) ? ? ? yes S(4) C(10) F(1) 111.5(7) ? ? ? yes S(4) C(10) F(2) 112.0(7) ? ? ? yes S(4) C(10) F(3) 112.1(7) ? ? ? yes F(1) C(10) F(2) 105.4(8) ? ? ? yes F(1) C(10) F(3) 107.1(8) ? ? ? yes F(2) C(10) F(3) 108.4(9) ? ? ? yes #------------------------------------------------------------------------------ _publ_contact_author ; Dr G. Reid Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [Mn(CO)3{MeS(CH2)2S(CH2)2SMe}]CF3SO3. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_sdomns3 #[Mn(CO)~3~{MeC(CH~2~SMe)~3~}]CF~3~SO~3~ #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jan 25 14:24:05 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.190(1) _cell_length_b 12.085(2) _cell_length_c 9.079(1) _cell_angle_alpha 98.85(1) _cell_angle_beta 94.78(1) _cell_angle_gamma 81.450(10) _cell_volume 983.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150.1 _cell_measurement_reflns_used 25 _cell_measurement_2theta_min 36.7 _cell_measurement_2theta_max 40.1 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.250 _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_meas ? _chemical_formula_weight 498.44 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H18 F3 Mn O6 S4 ' _chemical_formula_moiety '?' _chemical_formula_structural '[Mn(CO)~3~{MeC(CH~2~SMe)~3~}]CF~3~SO~3~' _chemical_compound_source 'diffusion of pet ether into CHCl~3~ soln' _exptl_crystal_F_000 508.00 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.806 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150.1 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.70 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 3 0 0 2 -3 -2 4 0 _diffrn_reflns_number 3706 _reflns_number_total 3469 _reflns_number_observed 2732 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 2.06 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_2theta_min ? _diffrn_reflns_2theta_max 25.01 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.05284 _diffrn_orient_matrix_UB_12 0.07546 _diffrn_orient_matrix_UB_13 -0.01902 _diffrn_orient_matrix_UB_21 -0.05031 _diffrn_orient_matrix_UB_22 0.00770 _diffrn_orient_matrix_UB_23 0.09530 _diffrn_orient_matrix_UB_31 0.08266 _diffrn_orient_matrix_UB_32 0.03736 _diffrn_orient_matrix_UB_33 0.05505 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 24 0.003 0.002 'International Tables' H 0 36 0.000 0.000 'International Tables' O 0 12 0.011 0.006 'International Tables' S 0 8 0.125 0.123 'International Tables' F 0 6 0.017 0.010 'International Tables' Mn 0 2 0.337 0.728 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Mn(1) 0.25949(5) 0.13604(4) 0.21790(5) 0.0225(1) Uij ? ? S(1) 0.44657(8) 0.25328(6) 0.25160(8) 0.0250(2) Uij ? ? S(2) 0.30992(8) 0.10676(6) 0.46788(7) 0.0230(2) Uij ? ? S(3) 0.08806(8) 0.29658(6) 0.28648(9) 0.0298(2) Uij ? ? S(4) 0.19637(9) -0.29062(6) 0.27662(8) 0.0295(2) Uij ? ? F(6) 0.2391(2) -0.4125(2) 0.0153(2) 0.0585(7) Uij ? ? F(7) 0.1962(3) -0.2342(2) 0.0085(2) 0.0648(8) Uij ? ? F(8) 0.4077(2) -0.3083(2) 0.0938(2) 0.0570(7) Uij ? ? O(10) 0.2838(2) -0.3795(2) 0.3464(2) 0.0397(7) Uij ? ? O(11) 0.2216(3) 0.1680(2) -0.0997(2) 0.0493(8) Uij ? ? O(12) 0.0429(2) -0.3041(2) 0.2490(3) 0.0467(7) Uij ? ? O(13) 0.0042(2) 0.0086(2) 0.1714(2) 0.0418(7) Uij ? ? O(14) 0.2280(3) -0.1785(2) 0.3358(2) 0.0458(7) Uij ? ? O(15) 0.4640(3) -0.0715(2) 0.1282(3) 0.0524(8) Uij ? ? C(15) 0.4166(3) 0.3623(2) 0.4144(3) 0.0253(8) Uij ? ? C(16) 0.3435(3) 0.2372(2) 0.5879(3) 0.0289(8) Uij ? ? C(17) 0.3234(4) 0.4433(3) 0.6600(3) 0.0382(10) Uij ? ? C(18) 0.1048(3) 0.0559(2) 0.1911(3) 0.0282(8) Uij ? ? C(19) 0.1432(3) 0.0781(2) 0.5366(3) 0.0319(9) Uij ? ? C(20) 0.2350(3) 0.1571(3) 0.0243(3) 0.0317(9) Uij ? ? C(21) 0.0997(4) 0.3987(3) 0.1630(4) 0.043(1) Uij ? ? C(22) 0.3064(3) 0.3496(2) 0.5263(3) 0.0264(8) Uij ? ? C(23) 0.1461(3) 0.3715(2) 0.4661(3) 0.0318(9) Uij ? ? C(24) 0.6198(3) 0.1740(3) 0.3081(4) 0.0382(9) Uij ? ? C(25) 0.2636(4) -0.3126(3) 0.0889(4) 0.040(1) Uij ? ? C(26) 0.3856(3) 0.0093(3) 0.1651(3) 0.0322(9) Uij ? ? H(1) 0.4215 0.4347 0.7062 0.0457 Uiso ? ? H(2) 0.3027 0.5162 0.6299 0.0457 Uiso ? ? H(3) 0.2564 0.4391 0.7344 0.0457 Uiso ? ? H(4) 0.5102 0.3683 0.4684 0.0298 Uiso ? ? H(5) 0.3839 0.4334 0.3781 0.0298 Uiso ? ? H(6) 0.2891 0.2438 0.6758 0.0343 Uiso ? ? H(7) 0.4473 0.2291 0.6212 0.0343 Uiso ? ? H(8) 0.1261 0.4521 0.4574 0.0387 Uiso ? ? H(9) 0.0860 0.3577 0.5384 0.0387 Uiso ? ? H(10) 0.0651 0.1400 0.5257 0.0375 Uiso ? ? H(11) 0.1114 0.0113 0.4793 0.0375 Uiso ? ? H(12) 0.1568 0.0685 0.6380 0.0375 Uiso ? ? H(13) 0.2002 0.4149 0.1649 0.0490 Uiso ? ? H(14) 0.0731 0.3690 0.0611 0.0490 Uiso ? ? H(15) 0.0380 0.4673 0.1900 0.0490 Uiso ? ? H(16) 0.6115 0.1438 0.3982 0.0451 Uiso ? ? H(17) 0.6489 0.1117 0.2322 0.0451 Uiso ? ? H(18) 0.6965 0.2207 0.3250 0.0451 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0257(2) 0.0283(2) 0.0155(2) -0.0067(2) 0.0023(2) 0.0056(2) S(1) 0.0228(4) 0.0326(4) 0.0219(4) -0.0058(3) 0.0029(3) 0.0087(3) S(2) 0.0270(4) 0.0263(4) 0.0173(4) -0.0050(3) 0.0021(3) 0.0067(3) S(3) 0.0225(4) 0.0325(4) 0.0354(4) -0.0043(3) -0.0016(3) 0.0089(3) S(4) 0.0335(4) 0.0285(4) 0.0255(4) -0.0002(3) 0.0001(3) 0.0051(3) F(6) 0.084(2) 0.053(1) 0.039(1) -0.026(1) 0.013(1) -0.0146(10) F(7) 0.093(2) 0.068(1) 0.038(1) -0.013(1) -0.008(1) 0.027(1) F(8) 0.051(1) 0.075(2) 0.051(1) -0.022(1) 0.016(1) 0.007(1) O(10) 0.044(1) 0.036(1) 0.039(1) 0.002(1) -0.004(1) 0.014(1) O(11) 0.048(2) 0.087(2) 0.020(1) -0.021(1) -0.002(1) 0.020(1) O(12) 0.031(1) 0.058(2) 0.051(2) -0.002(1) 0.004(1) 0.009(1) O(13) 0.046(1) 0.054(1) 0.031(1) -0.028(1) -0.004(1) 0.009(1) O(14) 0.068(2) 0.027(1) 0.039(1) -0.003(1) 0.000(1) -0.001(1) O(15) 0.060(2) 0.036(1) 0.063(2) 0.001(1) 0.035(1) 0.002(1) C(15) 0.027(2) 0.023(2) 0.028(2) -0.008(1) 0.000(1) 0.006(1) C(16) 0.038(2) 0.035(2) 0.017(1) -0.015(1) 0.001(1) 0.005(1) C(17) 0.043(2) 0.036(2) 0.037(2) -0.016(2) 0.009(2) -0.003(1) C(18) 0.038(2) 0.035(2) 0.014(1) -0.007(1) 0.002(1) 0.006(1) C(19) 0.042(2) 0.037(2) 0.022(2) -0.019(1) 0.011(1) 0.004(1) C(20) 0.028(2) 0.044(2) 0.027(2) -0.013(1) 0.001(1) 0.008(1) C(21) 0.044(2) 0.039(2) 0.050(2) -0.002(2) -0.010(2) 0.022(2) C(22) 0.029(2) 0.027(2) 0.025(2) -0.007(1) 0.006(1) 0.002(1) C(23) 0.029(2) 0.031(2) 0.035(2) -0.005(1) 0.008(1) 0.000(1) C(24) 0.026(2) 0.045(2) 0.041(2) 0.003(1) 0.002(1) 0.004(2) C(25) 0.050(2) 0.040(2) 0.033(2) -0.012(2) 0.003(2) 0.005(2) C(26) 0.040(2) 0.036(2) 0.024(2) -0.013(2) 0.011(1) 0.004(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2732 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0276 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0256 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.782 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.24 _refine_diff_density_max 0.31 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn(1) S(1) 2.3579(8) ? ? yes Mn(1) S(2) 2.3481(8) ? ? yes Mn(1) S(3) 2.3487(9) ? ? yes Mn(1) C(18) 1.816(3) ? ? yes Mn(1) C(20) 1.806(3) ? ? yes Mn(1) C(26) 1.805(3) ? ? yes S(1) C(15) 1.832(3) ? ? yes S(1) C(24) 1.810(3) ? ? yes S(2) C(16) 1.824(3) ? ? yes S(2) C(19) 1.800(3) ? ? yes S(3) C(21) 1.810(3) ? ? yes S(3) C(23) 1.819(3) ? ? yes S(4) O(10) 1.439(2) ? ? yes S(4) O(12) 1.440(2) ? ? yes S(4) O(14) 1.441(2) ? ? yes S(4) C(25) 1.828(3) ? ? yes F(6) C(25) 1.328(3) ? ? yes F(7) C(25) 1.334(4) ? ? yes F(8) C(25) 1.330(4) ? ? yes O(11) C(20) 1.147(3) ? ? yes O(13) C(18) 1.145(3) ? ? yes O(15) C(26) 1.147(4) ? ? yes C(15) C(22) 1.532(4) ? ? yes C(15) H(4) 0.961 ? ? no C(15) H(5) 0.965 ? ? no C(16) C(22) 1.528(4) ? ? yes C(16) H(6) 0.964 ? ? no C(16) H(7) 0.972 ? ? no C(17) C(22) 1.543(4) ? ? yes C(17) H(1) 0.961 ? ? no C(17) H(2) 0.951 ? ? no C(17) H(3) 0.962 ? ? no C(19) H(10) 0.966 ? ? no C(19) H(11) 0.961 ? ? no C(19) H(12) 0.942 ? ? no C(21) H(13) 0.971 ? ? no C(21) H(14) 0.964 ? ? no C(21) H(15) 0.944 ? ? no C(22) C(23) 1.528(4) ? ? yes C(23) H(8) 0.978 ? ? no C(23) H(9) 0.941 ? ? no C(24) H(16) 0.959 ? ? no C(24) H(17) 0.961 ? ? no C(24) H(18) 0.955 ? ? no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Mn(1) S(2) 88.12(3) ? ? ? yes S(1) Mn(1) S(3) 88.77(3) ? ? ? yes S(1) Mn(1) C(18) 175.40(10) ? ? ? yes S(1) Mn(1) C(20) 88.90(9) ? ? ? yes S(1) Mn(1) C(26) 93.44(10) ? ? ? yes S(2) Mn(1) S(3) 91.63(3) ? ? ? yes S(2) Mn(1) C(18) 93.45(9) ? ? ? yes S(2) Mn(1) C(20) 175.83(10) ? ? ? yes S(2) Mn(1) C(26) 88.19(9) ? ? ? yes S(3) Mn(1) C(18) 86.87(10) ? ? ? yes S(3) Mn(1) C(20) 91.2(1) ? ? ? yes S(3) Mn(1) C(26) 177.77(10) ? ? ? yes C(18) Mn(1) C(20) 89.8(1) ? ? ? yes C(18) Mn(1) C(26) 90.9(1) ? ? ? yes C(20) Mn(1) C(26) 89.1(1) ? ? ? yes Mn(1) S(1) C(15) 110.83(9) ? ? ? yes Mn(1) S(1) C(24) 109.8(1) ? ? ? yes C(15) S(1) C(24) 101.5(1) ? ? ? yes Mn(1) S(2) C(16) 111.33(9) ? ? ? yes Mn(1) S(2) C(19) 108.0(1) ? ? ? yes C(16) S(2) C(19) 102.0(1) ? ? ? yes Mn(1) S(3) C(21) 108.3(1) ? ? ? yes Mn(1) S(3) C(23) 110.37(10) ? ? ? yes C(21) S(3) C(23) 101.6(1) ? ? ? yes O(10) S(4) O(12) 114.1(1) ? ? ? yes O(10) S(4) O(14) 114.5(1) ? ? ? yes O(10) S(4) C(25) 103.2(1) ? ? ? yes O(12) S(4) O(14) 116.4(1) ? ? ? yes O(12) S(4) C(25) 103.2(1) ? ? ? yes O(14) S(4) C(25) 103.0(1) ? ? ? yes S(1) C(15) C(22) 119.0(2) ? ? ? yes S(1) C(15) H(4) 107.8 ? ? ? no S(1) C(15) H(5) 107.6 ? ? ? no C(22) C(15) H(4) 107.6 ? ? ? no C(22) C(15) H(5) 106.9 ? ? ? no H(4) C(15) H(5) 107.3 ? ? ? no S(2) C(16) C(22) 119.2(2) ? ? ? yes S(2) C(16) H(6) 108.1 ? ? ? no S(2) C(16) H(7) 107.6 ? ? ? no C(22) C(16) H(6) 107.2 ? ? ? no C(22) C(16) H(7) 107.6 ? ? ? no H(6) C(16) H(7) 106.6 ? ? ? no C(22) C(17) H(1) 111.0 ? ? ? no C(22) C(17) H(2) 111.3 ? ? ? no C(22) C(17) H(3) 110.0 ? ? ? no H(1) C(17) H(2) 108.5 ? ? ? no H(1) C(17) H(3) 107.6 ? ? ? no H(2) C(17) H(3) 108.4 ? ? ? no Mn(1) C(18) O(13) 177.3(3) ? ? ? yes S(2) C(19) H(10) 110.0 ? ? ? no S(2) C(19) H(11) 110.3 ? ? ? no S(2) C(19) H(12) 111.3 ? ? ? no H(10) C(19) H(11) 107.2 ? ? ? no H(10) C(19) H(12) 108.8 ? ? ? no H(11) C(19) H(12) 109.2 ? ? ? no Mn(1) C(20) O(11) 178.3(3) ? ? ? yes S(3) C(21) H(13) 110.3 ? ? ? no S(3) C(21) H(14) 110.7 ? ? ? no S(3) C(21) H(15) 111.9 ? ? ? no H(13) C(21) H(14) 106.6 ? ? ? no H(13) C(21) H(15) 108.2 ? ? ? no H(14) C(21) H(15) 108.8 ? ? ? no C(15) C(22) C(16) 111.9(2) ? ? ? yes C(15) C(22) C(17) 106.4(2) ? ? ? yes C(15) C(22) C(23) 113.0(2) ? ? ? yes C(16) C(22) C(17) 106.4(2) ? ? ? yes C(16) C(22) C(23) 112.9(2) ? ? ? yes C(17) C(22) C(23) 105.6(2) ? ? ? yes S(3) C(23) C(22) 119.8(2) ? ? ? yes S(3) C(23) H(8) 106.4 ? ? ? no S(3) C(23) H(9) 108.2 ? ? ? no C(22) C(23) H(8) 106.3 ? ? ? no C(22) C(23) H(9) 107.8 ? ? ? no H(8) C(23) H(9) 107.9 ? ? ? no S(1) C(24) H(16) 110.8 ? ? ? no S(1) C(24) H(17) 110.7 ? ? ? no S(1) C(24) H(18) 111.0 ? ? ? no H(16) C(24) H(17) 107.8 ? ? ? no H(16) C(24) H(18) 108.3 ? ? ? no H(17) C(24) H(18) 108.1 ? ? ? no S(4) C(25) F(6) 111.2(2) ? ? ? yes S(4) C(25) F(7) 111.4(2) ? ? ? yes S(4) C(25) F(8) 111.3(2) ? ? ? yes F(6) C(25) F(7) 107.2(3) ? ? ? yes F(6) C(25) F(8) 107.9(3) ? ? ? yes F(7) C(25) F(8) 107.7(3) ? ? ? yes Mn(1) C(26) O(15) 178.3(3) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' J. Chem. Soc., Dalton Trans.' _publ_contact_author ; Dr G. Reid Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [Mn(CO)~3~{MeC(CH~2~SMe)~3~}]CF~3~SO~3~. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_jcp3 #[Mn(CO)3{MeC(CH2PPh2)3}]CF3SO3 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Mar 16 16:00:42 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 10.948(2) _cell_length_b 22.611(3) _cell_length_c 18.429(3) _cell_angle_alpha 90 _cell_angle_beta 97.99(1) _cell_angle_gamma 90 _cell_volume 4517(1) _cell_formula_units_Z 4 _cell_measurement_temperature 150.1 _cell_measurement_reflns_used 20 _cell_measurement_2theta_min 14.3 _cell_measurement_2theta_max 16.2 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 997.65 _chemical_formula_analytical ? _chemical_formula_sum 'C46 H41 Cl2 F3 Mn O6 P3 S ' _chemical_formula_moiety '?' _chemical_formula_structural '[Mn(CO)3{MeC(CH2PPh2)3}]CF3SO3' _chemical_compound_source 'CH2Cl2/Et2O' _exptl_crystal_F_000 2048.00 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.672 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150.1 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -8.67 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -8 0 4 -2 0 3 -5 0 _diffrn_reflns_number 8626 _reflns_number_total 8174 _reflns_number_observed 4161 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 7.59 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_2theta_min ? _diffrn_reflns_2theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.08841 _diffrn_orient_matrix_UB_12 -0.01253 _diffrn_orient_matrix_UB_13 0.00571 _diffrn_orient_matrix_UB_21 -0.02627 _diffrn_orient_matrix_UB_22 -0.04225 _diffrn_orient_matrix_UB_23 -0.00651 _diffrn_orient_matrix_UB_31 -0.00049 _diffrn_orient_matrix_UB_32 0.00376 _diffrn_orient_matrix_UB_33 -0.05411 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 184 0.003 0.002 'International Tables' H 0 164 0.000 0.000 'International Tables' O 0 24 0.011 0.006 'International Tables' Mn 0 4 0.337 0.728 'International Tables' P 0 12 0.102 0.094 'International Tables' F 0 12 0.017 0.010 'International Tables' S 0 4 0.125 0.123 'International Tables' Cl 0 8 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Mn(1) 0.19866(8) 0.09079(4) 0.34882(5) 0.0188(3) Uij ? ? Cl(1) 0.2885(2) 0.0825(1) 0.9858(1) 0.0730(8) Uij ? ? Cl(2) 0.1933(2) 0.10945(10) 0.8327(1) 0.0605(7) Uij ? ? S(1) -0.3513(2) -0.32726(8) -0.4477(1) 0.0396(6) Uij ? ? P(1) 0.2607(1) 0.01297(7) 0.27852(9) 0.0194(4) Uij ? ? P(2) 0.1764(1) 0.14618(7) 0.23934(9) 0.0200(5) Uij ? ? P(3) -0.0077(1) 0.06250(7) 0.31374(9) 0.0189(4) Uij ? ? F(1) -0.2233(5) -0.4156(2) -0.4886(3) 0.071(2) Uij ? ? F(2) -0.2232(4) -0.3392(3) -0.5569(3) 0.076(2) Uij ? ? F(3) -0.1142(4) -0.3402(3) -0.4501(3) 0.080(2) Uij ? ? O(1) 0.1123(4) 0.1815(2) 0.4461(3) 0.033(1) Uij ? ? O(2) 0.2310(4) 0.0179(2) 0.4841(3) 0.034(1) Uij ? ? O(3) 0.4523(4) 0.1315(2) 0.4020(3) 0.038(2) Uij ? ? O(4) -0.4553(5) -0.3468(2) -0.4985(3) 0.052(2) Uij ? ? O(5) -0.3373(6) -0.3551(3) -0.3770(3) 0.064(2) Uij ? ? O(6) -0.3321(5) -0.2646(2) -0.4474(3) 0.060(2) Uij ? ? C(1) 0.1438(6) 0.1486(3) 0.4050(4) 0.023(2) Uij ? ? C(2) 0.2150(6) 0.0448(3) 0.4302(4) 0.022(2) Uij ? ? C(3) 0.3556(6) 0.1157(3) 0.3787(3) 0.023(2) Uij ? ? C(4) -0.0008(6) 0.0208(3) 0.0943(3) 0.026(2) Uij ? ? C(5) 0.0556(5) 0.0428(3) 0.1710(3) 0.020(2) Uij ? ? C(6) 0.1326(5) -0.0093(3) 0.2084(3) 0.020(2) Uij ? ? C(7) 0.1365(6) 0.0979(3) 0.1600(3) 0.022(2) Uij ? ? C(8) -0.0517(5) 0.0597(3) 0.2130(3) 0.023(2) Uij ? ? C(9) 0.3130(6) -0.0542(3) 0.3289(3) 0.023(2) Uij ? ? C(10) 0.4132(6) -0.0482(3) 0.3845(4) 0.028(2) Uij ? ? C(11) 0.4621(6) -0.0973(3) 0.4222(4) 0.032(2) Uij ? ? C(12) 0.4123(6) -0.1529(3) 0.4060(4) 0.030(2) Uij ? ? C(13) 0.3148(6) -0.1596(3) 0.3504(4) 0.030(2) Uij ? ? C(14) 0.2648(6) -0.1104(3) 0.3116(4) 0.026(2) Uij ? ? C(15) 0.3902(6) 0.0208(3) 0.2256(3) 0.023(2) Uij ? ? C(16) 0.4712(6) 0.0685(3) 0.2341(4) 0.025(2) Uij ? ? C(17) 0.5688(6) 0.0718(3) 0.1916(4) 0.034(2) Uij ? ? C(18) 0.5839(6) 0.0276(3) 0.1412(4) 0.036(2) Uij ? ? C(19) 0.5042(7) -0.0205(4) 0.1338(4) 0.044(2) Uij ? ? C(20) 0.4084(6) -0.0243(3) 0.1758(4) 0.034(2) Uij ? ? C(21) 0.3083(6) 0.1892(3) 0.2169(3) 0.023(2) Uij ? ? C(22) 0.3666(6) 0.2278(3) 0.2710(4) 0.028(2) Uij ? ? C(23) 0.4620(6) 0.2636(3) 0.2549(4) 0.035(2) Uij ? ? C(24) 0.5023(7) 0.2607(3) 0.1866(5) 0.043(2) Uij ? ? C(25) 0.4450(7) 0.2231(3) 0.1326(4) 0.043(2) Uij ? ? C(26) 0.3460(6) 0.1880(3) 0.1484(4) 0.031(2) Uij ? ? C(27) 0.0606(5) 0.2055(3) 0.2305(3) 0.024(2) Uij ? ? C(28) -0.0293(6) 0.2114(3) 0.1689(3) 0.025(2) Uij ? ? C(29) -0.1169(6) 0.2564(3) 0.1665(4) 0.030(2) Uij ? ? C(30) -0.1148(6) 0.2962(3) 0.2237(4) 0.033(2) Uij ? ? C(31) -0.0227(6) 0.2923(3) 0.2833(4) 0.028(2) Uij ? ? C(32) 0.0638(6) 0.2471(3) 0.2867(3) 0.026(2) Uij ? ? C(33) -0.0676(6) -0.0090(3) 0.3422(3) 0.021(2) Uij ? ? C(34) 0.0047(6) -0.0529(3) 0.3791(3) 0.022(2) Uij ? ? C(35) -0.0493(6) -0.1038(3) 0.4031(3) 0.030(2) Uij ? ? C(36) -0.1775(6) -0.1109(3) 0.3886(3) 0.028(2) Uij ? ? C(37) -0.2488(6) -0.0686(3) 0.3489(4) 0.030(2) Uij ? ? C(38) -0.1964(6) -0.0175(3) 0.3264(4) 0.028(2) Uij ? ? C(39) -0.1185(5) 0.1106(3) 0.3498(3) 0.021(2) Uij ? ? C(40) -0.1369(6) 0.1017(3) 0.4221(4) 0.030(2) Uij ? ? C(41) -0.2157(7) 0.1374(3) 0.4557(4) 0.034(2) Uij ? ? C(42) -0.2772(6) 0.1834(3) 0.4166(4) 0.035(2) Uij ? ? C(43) -0.2584(6) 0.1936(3) 0.3449(4) 0.036(2) Uij ? ? C(44) -0.1793(6) 0.1579(3) 0.3114(4) 0.029(2) Uij ? ? C(45) -0.2216(7) -0.3560(4) -0.4879(4) 0.045(3) Uij ? ? C(46) 0.2047(10) 0.1333(4) 0.9248(6) 0.075(4) Uij ? ? H(1) 0.0756 0.0144 0.0660 0.0686 Uiso ? ? H(2) -0.0319 -0.0192 0.0905 0.0686 Uiso ? ? H(3) -0.0583 0.0500 0.0710 0.0686 Uiso ? ? H(4) 0.1669 -0.0321 0.1659 0.0686 Uiso ? ? H(5) 0.0762 -0.0362 0.2311 0.0686 Uiso ? ? H(6) 0.2202 0.0831 0.1390 0.0686 Uiso ? ? H(7) 0.0888 0.1191 0.1153 0.0686 Uiso ? ? H(8) -0.1160 0.0282 0.2094 0.0686 Uiso ? ? H(9) -0.1017 0.0982 0.1892 0.0686 Uiso ? ? H(10) 0.4502 0.0049 0.3998 0.0686 Uiso ? ? H(11) 0.5279 -0.0885 0.4646 0.0686 Uiso ? ? H(12) 0.4477 -0.1932 0.4335 0.0686 Uiso ? ? H(13) 0.2804 -0.2065 0.3463 0.0686 Uiso ? ? H(14) 0.1906 -0.1194 0.2669 0.0686 Uiso ? ? H(15) 0.4756 0.1072 0.2814 0.0686 Uiso ? ? H(16) 0.6148 0.1126 0.2008 0.0686 Uiso ? ? H(17) 0.6588 0.0292 0.1162 0.0686 Uiso ? ? H(18) 0.5219 -0.0543 0.1014 0.0686 Uiso ? ? H(19) 0.3555 -0.0675 0.1814 0.0686 Uiso ? ? H(20) 0.3295 0.2243 0.3288 0.0686 Uiso ? ? H(21) 0.4927 0.3023 0.2864 0.0686 Uiso ? ? H(22) 0.5950 0.2794 0.1653 0.0686 Uiso ? ? H(23) 0.4466 0.2135 0.0701 0.0686 Uiso ? ? H(24) 0.2989 0.1631 0.1027 0.0686 Uiso ? ? H(25) -0.0354 0.1827 0.1224 0.0686 Uiso ? ? H(26) -0.1855 0.2623 0.1208 0.0686 Uiso ? ? H(27) -0.1781 0.3344 0.2186 0.0686 Uiso ? ? H(28) -0.0251 0.3278 0.3349 0.0686 Uiso ? ? H(29) 0.1323 0.2434 0.3302 0.0686 Uiso ? ? H(30) 0.1007 -0.0435 0.3967 0.0686 Uiso ? ? H(31) 0.0014 -0.1338 0.4343 0.0686 Uiso ? ? H(32) -0.2221 -0.1537 0.4013 0.0686 Uiso ? ? H(33) -0.3529 -0.0694 0.3358 0.0686 Uiso ? ? H(34) -0.2526 0.0194 0.3002 0.0686 Uiso ? ? H(35) -0.1118 0.0633 0.4507 0.0686 Uiso ? ? H(36) -0.2140 0.1281 0.5139 0.0686 Uiso ? ? H(37) -0.3299 0.2179 0.4452 0.0686 Uiso ? ? H(38) -0.2879 0.2367 0.3173 0.0686 Uiso ? ? H(39) -0.1729 0.1815 0.2584 0.0686 Uiso ? ? H(40) 0.1226 0.1387 0.9381 0.0868 Uiso ? ? H(41) 0.2439 0.1718 0.9298 0.0868 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0175(5) 0.0204(5) 0.0188(5) -0.0020(4) 0.0031(4) -0.0002(4) Cl(1) 0.061(2) 0.109(2) 0.053(1) 0.006(1) 0.021(1) -0.026(1) Cl(2) 0.059(1) 0.059(1) 0.068(2) 0.004(1) 0.024(1) 0.015(1) S(1) 0.049(1) 0.039(1) 0.031(1) -0.0136(10) 0.0048(9) -0.0046(9) P(1) 0.0174(9) 0.0206(9) 0.0201(9) 0.0000(7) 0.0026(7) -0.0009(7) P(2) 0.0178(9) 0.0196(9) 0.0226(9) -0.0015(7) 0.0027(7) -0.0003(7) P(3) 0.0160(9) 0.0206(9) 0.0204(9) -0.0016(7) 0.0031(7) 0.0015(7) F(1) 0.073(4) 0.063(4) 0.073(4) 0.016(3) -0.001(3) -0.016(3) F(2) 0.059(3) 0.128(5) 0.045(3) 0.031(3) 0.024(3) 0.028(3) F(3) 0.041(3) 0.101(4) 0.092(4) -0.007(3) -0.013(3) -0.004(3) O(1) 0.036(3) 0.031(3) 0.033(3) -0.008(2) 0.012(2) -0.008(2) O(2) 0.045(3) 0.033(3) 0.024(3) -0.002(2) 0.006(2) 0.004(2) O(3) 0.024(3) 0.053(3) 0.034(3) -0.017(2) -0.002(2) 0.005(2) O(4) 0.035(3) 0.069(4) 0.050(3) -0.016(3) 0.001(3) -0.019(3) O(5) 0.098(5) 0.068(4) 0.027(3) -0.003(4) 0.016(3) 0.002(3) O(6) 0.069(4) 0.037(3) 0.077(4) -0.011(3) 0.017(3) -0.005(3) C(1) 0.024(4) 0.024(4) 0.021(4) -0.009(3) 0.004(3) -0.002(3) C(2) 0.020(4) 0.023(4) 0.023(4) -0.004(3) 0.003(3) -0.011(3) C(3) 0.031(4) 0.022(3) 0.017(4) -0.001(3) 0.003(3) 0.004(3) C(4) 0.032(4) 0.027(4) 0.018(4) -0.001(3) -0.004(3) -0.005(3) C(5) 0.020(3) 0.021(3) 0.019(3) -0.001(3) 0.007(3) 0.002(3) C(6) 0.015(3) 0.021(3) 0.024(4) -0.003(3) 0.004(3) 0.000(3) C(7) 0.024(4) 0.023(4) 0.017(3) 0.001(3) 0.003(3) 0.002(3) C(8) 0.015(3) 0.032(4) 0.023(4) -0.005(3) 0.005(3) -0.001(3) C(9) 0.017(3) 0.027(4) 0.026(4) 0.002(3) 0.010(3) 0.002(3) C(10) 0.021(4) 0.033(4) 0.029(4) 0.004(3) 0.003(3) 0.003(3) C(11) 0.025(4) 0.040(5) 0.030(4) 0.008(3) 0.005(3) 0.006(3) C(12) 0.033(4) 0.029(4) 0.032(4) 0.010(3) 0.020(3) 0.003(3) C(13) 0.034(4) 0.024(4) 0.035(4) 0.004(3) 0.012(3) 0.004(3) C(14) 0.025(4) 0.019(3) 0.034(4) 0.005(3) 0.007(3) -0.004(3) C(15) 0.024(4) 0.026(4) 0.019(3) 0.001(3) 0.004(3) -0.004(3) C(16) 0.016(3) 0.028(4) 0.032(4) 0.002(3) 0.007(3) 0.011(3) C(17) 0.027(4) 0.032(4) 0.044(5) 0.001(3) 0.007(3) 0.001(3) C(18) 0.021(4) 0.052(5) 0.037(4) 0.003(4) 0.015(3) 0.002(4) C(19) 0.036(5) 0.054(5) 0.043(5) 0.001(4) 0.008(4) -0.015(4) C(20) 0.023(4) 0.043(5) 0.042(4) -0.009(3) 0.022(3) -0.005(4) C(21) 0.019(4) 0.022(3) 0.029(4) 0.000(3) 0.006(3) 0.001(3) C(22) 0.022(4) 0.023(4) 0.039(4) 0.000(3) 0.001(3) 0.003(3) C(23) 0.027(4) 0.021(4) 0.055(5) -0.004(3) 0.002(4) 0.005(3) C(24) 0.030(4) 0.039(5) 0.062(6) -0.005(4) 0.008(4) 0.013(4) C(25) 0.040(5) 0.044(5) 0.046(5) 0.000(4) 0.012(4) 0.007(4) C(26) 0.033(4) 0.027(4) 0.035(4) -0.002(3) 0.014(3) 0.005(3) C(27) 0.013(3) 0.030(4) 0.031(4) -0.002(3) 0.005(3) 0.005(3) C(28) 0.024(4) 0.025(4) 0.027(4) 0.000(3) 0.002(3) 0.004(3) C(29) 0.022(4) 0.032(4) 0.033(4) -0.004(3) -0.003(3) 0.007(3) C(30) 0.031(4) 0.022(4) 0.047(5) 0.005(3) 0.008(4) 0.007(3) C(31) 0.027(4) 0.027(4) 0.032(4) 0.006(3) 0.006(3) 0.003(3) C(32) 0.030(4) 0.020(4) 0.026(4) 0.000(3) 0.002(3) 0.001(3) C(33) 0.023(4) 0.025(4) 0.016(3) -0.007(3) 0.007(3) -0.003(3) C(34) 0.022(4) 0.025(4) 0.020(4) -0.006(3) 0.005(3) -0.003(3) C(35) 0.040(5) 0.020(4) 0.028(4) -0.003(3) 0.001(3) 0.000(3) C(36) 0.040(5) 0.025(4) 0.021(4) -0.011(3) 0.006(3) -0.005(3) C(37) 0.025(4) 0.031(4) 0.035(4) -0.005(3) 0.007(3) -0.011(3) C(38) 0.018(4) 0.036(4) 0.030(4) -0.005(3) 0.001(3) -0.002(3) C(39) 0.016(3) 0.023(3) 0.023(4) -0.005(3) 0.001(3) -0.001(3) C(40) 0.033(4) 0.026(4) 0.031(4) -0.003(3) 0.004(3) 0.000(3) C(41) 0.035(4) 0.036(4) 0.033(4) 0.007(4) 0.011(3) -0.004(3) C(42) 0.021(4) 0.032(4) 0.053(5) 0.003(3) 0.012(4) -0.010(4) C(43) 0.027(4) 0.025(4) 0.057(5) 0.010(3) 0.014(4) 0.001(4) C(44) 0.020(4) 0.024(4) 0.042(4) -0.002(3) 0.000(3) 0.005(3) C(45) 0.038(5) 0.053(6) 0.039(5) 0.000(4) -0.008(4) 0.001(4) C(46) 0.097(8) 0.056(6) 0.081(7) 0.013(6) 0.047(6) -0.003(5) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4161 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0538 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0653 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.982 _refine_ls_shift/esd_max 0.0320 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.58 _refine_diff_density_max 0.47 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn(1) P(1) 2.341(2) ? ? yes Mn(1) P(2) 2.359(2) ? ? yes Mn(1) P(3) 2.351(2) ? ? yes Mn(1) C(1) 1.822(7) ? ? yes Mn(1) C(2) 1.814(7) ? ? yes Mn(1) C(3) 1.819(7) ? ? yes Cl(1) C(46) 1.77(1) ? ? yes Cl(2) C(46) 1.768(10) ? ? yes S(1) O(4) 1.439(5) ? ? yes S(1) O(5) 1.435(6) ? ? yes S(1) O(6) 1.432(5) ? ? yes S(1) C(45) 1.811(8) ? ? yes P(1) C(6) 1.840(6) ? ? yes P(1) C(9) 1.829(6) ? ? yes P(1) C(15) 1.837(6) ? ? yes P(2) C(7) 1.829(6) ? ? yes P(2) C(21) 1.835(6) ? ? yes P(2) C(27) 1.837(6) ? ? yes P(3) C(8) 1.853(6) ? ? yes P(3) C(33) 1.848(6) ? ? yes P(3) C(39) 1.822(6) ? ? yes F(1) C(45) 1.348(9) ? ? yes F(2) C(45) 1.324(9) ? ? yes F(3) C(45) 1.329(8) ? ? yes O(1) C(1) 1.148(7) ? ? yes O(2) C(2) 1.156(7) ? ? yes O(3) C(3) 1.143(7) ? ? yes C(4) C(5) 1.544(8) ? ? yes C(5) C(6) 1.553(8) ? ? yes C(5) C(7) 1.558(8) ? ? yes C(5) C(8) 1.543(8) ? ? yes C(9) C(10) 1.400(9) ? ? yes C(9) C(14) 1.397(9) ? ? yes C(10) C(11) 1.379(9) ? ? yes C(11) C(12) 1.386(9) ? ? yes C(12) C(13) 1.381(10) ? ? yes C(13) C(14) 1.393(9) ? ? yes C(15) C(16) 1.391(8) ? ? yes C(15) C(20) 1.405(9) ? ? yes C(16) C(17) 1.412(9) ? ? yes C(17) C(18) 1.390(10) ? ? yes C(18) C(19) 1.39(1) ? ? yes C(19) C(20) 1.391(10) ? ? yes C(21) C(22) 1.410(9) ? ? yes C(21) C(26) 1.381(9) ? ? yes C(22) C(23) 1.386(9) ? ? yes C(23) C(24) 1.39(1) ? ? yes C(24) C(25) 1.39(1) ? ? yes C(25) C(26) 1.407(10) ? ? yes C(27) C(28) 1.401(9) ? ? yes C(27) C(32) 1.396(9) ? ? yes C(28) C(29) 1.395(9) ? ? yes C(29) C(30) 1.384(9) ? ? yes C(30) C(31) 1.387(9) ? ? yes C(31) C(32) 1.388(9) ? ? yes C(33) C(34) 1.387(9) ? ? yes C(33) C(38) 1.413(9) ? ? yes C(34) C(35) 1.394(9) ? ? yes C(35) C(36) 1.400(9) ? ? yes C(36) C(37) 1.378(9) ? ? yes C(37) C(38) 1.380(9) ? ? yes C(39) C(40) 1.391(9) ? ? yes C(39) C(44) 1.398(9) ? ? yes C(40) C(41) 1.387(9) ? ? yes C(41) C(42) 1.386(10) ? ? yes C(42) C(43) 1.386(10) ? ? yes C(43) C(44) 1.389(9) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P(1) Mn(1) P(2) 85.94(6) ? ? ? yes P(1) Mn(1) P(3) 89.14(6) ? ? ? yes P(1) Mn(1) C(1) 176.8(2) ? ? ? yes P(1) Mn(1) C(2) 91.4(2) ? ? ? yes P(1) Mn(1) C(3) 93.8(2) ? ? ? yes P(2) Mn(1) P(3) 85.89(6) ? ? ? yes P(2) Mn(1) C(1) 95.9(2) ? ? ? yes P(2) Mn(1) C(2) 177.1(2) ? ? ? yes P(2) Mn(1) C(3) 94.3(2) ? ? ? yes P(3) Mn(1) C(1) 88.4(2) ? ? ? yes P(3) Mn(1) C(2) 93.0(2) ? ? ? yes P(3) Mn(1) C(3) 177.1(2) ? ? ? yes C(1) Mn(1) C(2) 86.8(3) ? ? ? yes C(1) Mn(1) C(3) 88.7(3) ? ? ? yes C(2) Mn(1) C(3) 87.0(3) ? ? ? yes O(4) S(1) O(5) 115.5(4) ? ? ? yes O(4) S(1) O(6) 114.1(4) ? ? ? yes O(4) S(1) C(45) 102.6(3) ? ? ? yes O(5) S(1) O(6) 115.7(3) ? ? ? yes O(5) S(1) C(45) 102.9(4) ? ? ? yes O(6) S(1) C(45) 103.5(4) ? ? ? yes Mn(1) P(1) C(6) 110.1(2) ? ? ? yes Mn(1) P(1) C(9) 115.9(2) ? ? ? yes Mn(1) P(1) C(15) 121.7(2) ? ? ? yes C(6) P(1) C(9) 106.4(3) ? ? ? yes C(6) P(1) C(15) 102.9(3) ? ? ? yes C(9) P(1) C(15) 98.0(3) ? ? ? yes Mn(1) P(2) C(7) 110.6(2) ? ? ? yes Mn(1) P(2) C(21) 118.9(2) ? ? ? yes Mn(1) P(2) C(27) 116.8(2) ? ? ? yes C(7) P(2) C(21) 104.2(3) ? ? ? yes C(7) P(2) C(27) 106.2(3) ? ? ? yes C(21) P(2) C(27) 98.6(3) ? ? ? yes Mn(1) P(3) C(8) 113.0(2) ? ? ? yes Mn(1) P(3) C(33) 121.7(2) ? ? ? yes Mn(1) P(3) C(39) 113.6(2) ? ? ? yes C(8) P(3) C(33) 101.6(3) ? ? ? yes C(8) P(3) C(39) 107.0(3) ? ? ? yes C(33) P(3) C(39) 98.0(3) ? ? ? yes Mn(1) C(1) O(1) 173.4(6) ? ? ? yes Mn(1) C(2) O(2) 175.7(5) ? ? ? yes Mn(1) C(3) O(3) 175.5(6) ? ? ? yes C(4) C(5) C(6) 106.6(5) ? ? ? yes C(4) C(5) C(7) 107.5(5) ? ? ? yes C(4) C(5) C(8) 107.7(5) ? ? ? yes C(6) C(5) C(7) 112.4(5) ? ? ? yes C(6) C(5) C(8) 111.7(5) ? ? ? yes C(7) C(5) C(8) 110.6(5) ? ? ? yes P(1) C(6) C(5) 114.7(4) ? ? ? yes P(2) C(7) C(5) 116.8(4) ? ? ? yes P(3) C(8) C(5) 113.6(4) ? ? ? yes P(1) C(9) C(10) 116.7(5) ? ? ? yes P(1) C(9) C(14) 123.9(5) ? ? ? yes C(10) C(9) C(14) 119.2(6) ? ? ? yes C(9) C(10) C(11) 120.0(6) ? ? ? yes C(10) C(11) C(12) 120.6(6) ? ? ? yes C(11) C(12) C(13) 120.0(6) ? ? ? yes C(12) C(13) C(14) 120.1(6) ? ? ? yes C(9) C(14) C(13) 120.1(6) ? ? ? yes P(1) C(15) C(16) 122.9(5) ? ? ? yes P(1) C(15) C(20) 117.8(5) ? ? ? yes C(16) C(15) C(20) 119.3(6) ? ? ? yes C(15) C(16) C(17) 119.9(6) ? ? ? yes C(16) C(17) C(18) 120.2(6) ? ? ? yes C(17) C(18) C(19) 119.8(6) ? ? ? yes C(18) C(19) C(20) 120.4(7) ? ? ? yes C(15) C(20) C(19) 120.4(6) ? ? ? yes P(2) C(21) C(22) 117.5(5) ? ? ? yes P(2) C(21) C(26) 122.7(5) ? ? ? yes C(22) C(21) C(26) 119.6(6) ? ? ? yes C(21) C(22) C(23) 119.5(6) ? ? ? yes C(22) C(23) C(24) 120.6(7) ? ? ? yes C(23) C(24) C(25) 120.5(7) ? ? ? yes C(24) C(25) C(26) 118.7(7) ? ? ? yes C(21) C(26) C(25) 121.0(6) ? ? ? yes P(2) C(27) C(28) 122.7(5) ? ? ? yes P(2) C(27) C(32) 118.7(5) ? ? ? yes C(28) C(27) C(32) 118.6(6) ? ? ? yes C(27) C(28) C(29) 119.9(6) ? ? ? yes C(28) C(29) C(30) 120.7(6) ? ? ? yes C(29) C(30) C(31) 119.7(6) ? ? ? yes C(30) C(31) C(32) 120.0(6) ? ? ? yes C(27) C(32) C(31) 121.0(6) ? ? ? yes P(3) C(33) C(34) 124.4(5) ? ? ? yes P(3) C(33) C(38) 116.3(5) ? ? ? yes C(34) C(33) C(38) 119.3(6) ? ? ? yes C(33) C(34) C(35) 120.5(6) ? ? ? yes C(34) C(35) C(36) 119.4(6) ? ? ? yes C(35) C(36) C(37) 120.1(6) ? ? ? yes C(36) C(37) C(38) 120.8(6) ? ? ? yes C(33) C(38) C(37) 119.8(6) ? ? ? yes P(3) C(39) C(40) 117.1(5) ? ? ? yes P(3) C(39) C(44) 124.5(5) ? ? ? yes C(40) C(39) C(44) 118.3(6) ? ? ? yes C(39) C(40) C(41) 121.7(6) ? ? ? yes C(40) C(41) C(42) 119.5(6) ? ? ? yes C(41) C(42) C(43) 119.6(6) ? ? ? yes C(42) C(43) C(44) 120.8(6) ? ? ? yes C(39) C(44) C(43) 120.1(6) ? ? ? yes S(1) C(45) F(1) 110.6(6) ? ? ? yes S(1) C(45) F(2) 112.6(5) ? ? ? yes S(1) C(45) F(3) 112.0(6) ? ? ? yes F(1) C(45) F(2) 106.2(7) ? ? ? yes F(1) C(45) F(3) 106.4(6) ? ? ? yes F(2) C(45) F(3) 108.7(7) ? ? ? yes Cl(1) C(46) Cl(2) 111.8(5) ? ? ? yes #------------------------------------------------------------------------------ _publ_contact_author ; Dr G. Reid Deoartment of Chemistry, University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [Mn(CO)3{MeC(CH2PPh2)3}]CF3SO3. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_phte3 #[Mn(CO)3{MeC(CH2TePh)3}]CF3SO3 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Mar 16 15:13:33 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 13.216(3) _cell_length_b 15.662(2) _cell_length_c 16.050(4) _cell_angle_alpha 90 _cell_angle_beta 106.73(2) _cell_angle_gamma 90 _cell_volume 3181(1) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 20 _cell_measurement_2theta_min 14.2 _cell_measurement_2theta_max 17.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourlessplate' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 971.28 _chemical_formula_analytical ? _chemical_formula_sum 'C27 H24 F3 Mn O6 S Te3 ' _chemical_formula_moiety '?' _chemical_formula_structural '[Mn(CO)3{MeC(CH2TePh)3}]CF3SO3' _chemical_compound_source 'CH2Cl2/pet ether' _exptl_crystal_F_000 1832.00 _exptl_absorpt_coefficient_mu 3.220 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.803 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 423.2 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.42 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 0 4 -4 1 4 -1 3 5 _diffrn_reflns_number 6097 _reflns_number_total 5832 _reflns_number_observed 2933 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 5.65 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_2theta_min ? _diffrn_reflns_2theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.03527 _diffrn_orient_matrix_UB_12 0.05708 _diffrn_orient_matrix_UB_13 -0.01077 _diffrn_orient_matrix_UB_21 -0.06557 _diffrn_orient_matrix_UB_22 -0.02744 _diffrn_orient_matrix_UB_23 -0.03771 _diffrn_orient_matrix_UB_31 -0.02644 _diffrn_orient_matrix_UB_32 -0.00809 _diffrn_orient_matrix_UB_33 0.05191 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 108 0.003 0.002 'International Tables' H 0 96 0.000 0.000 'International Tables' O 0 24 0.011 0.006 'International Tables' Mn 0 4 0.337 0.728 'International Tables' Te 0 12 -0.531 1.675 'International Tables' F 0 12 0.017 0.010 'International Tables' S 0 4 0.125 0.123 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Te1 -0.03581(7) 0.25975(5) 0.24489(5) 0.0329(2) Uij ? ? Te2 0.11698(7) 0.07962(5) 0.35690(6) 0.0315(2) Uij ? ? Te3 0.14000(7) 0.30552(5) 0.45685(5) 0.0293(2) Uij ? ? Mn1 0.1668(1) 0.2325(1) 0.3163(1) 0.0316(6) Uij ? ? S1 0.1319(3) 0.1536(2) 0.7258(2) 0.0350(10) Uij ? ? F1 0.0657(9) 0.2625(7) 0.8206(7) 0.096(4) Uij ? ? F2 -0.0135(7) 0.1400(6) 0.8062(6) 0.065(3) Uij ? ? F3 -0.0489(7) 0.2302(6) 0.7030(7) 0.084(4) Uij ? ? O1 0.2264(9) 0.3999(6) 0.2600(7) 0.060(4) Uij ? ? O2 0.3888(8) 0.1875(6) 0.4001(6) 0.047(3) Uij ? ? O3 0.1955(8) 0.1584(7) 0.1557(7) 0.061(4) Uij ? ? O4 0.1687(7) 0.2239(6) 0.6850(5) 0.040(3) Uij ? ? O5 0.2078(7) 0.1237(7) 0.8043(7) 0.062(3) Uij ? ? O6 0.0773(9) 0.0891(6) 0.6674(7) 0.066(4) Uij ? ? C1 0.201(1) 0.3353(9) 0.2821(9) 0.046(5) Uij ? ? C2 0.303(1) 0.2078(8) 0.3706(9) 0.036(4) Uij ? ? C3 0.182(1) 0.1855(9) 0.2162(9) 0.041(4) Uij ? ? C4 -0.150(1) 0.1552(9) 0.4656(9) 0.043(4) Uij ? ? C5 -0.0606(9) 0.1766(7) 0.4230(7) 0.027(3) Uij ? ? C6 -0.1204(10) 0.2102(8) 0.3310(8) 0.034(4) Uij ? ? C7 -0.0029(9) 0.0923(7) 0.4234(8) 0.028(4) Uij ? ? C8 0.0077(9) 0.2429(7) 0.4849(8) 0.028(4) Uij ? ? C9 -0.0750(10) 0.1657(8) 0.1443(8) 0.034(4) Uij ? ? C10 -0.111(1) 0.0828(9) 0.1553(9) 0.040(4) Uij ? ? C11 -0.130(1) 0.0240(8) 0.0874(9) 0.039(4) Uij ? ? C12 -0.108(1) 0.0476(9) 0.0110(10) 0.047(5) Uij ? ? C13 -0.070(1) 0.128(1) 0.0024(9) 0.050(5) Uij ? ? C14 -0.053(1) 0.1871(9) 0.0687(9) 0.042(4) Uij ? ? C15 0.2434(9) 0.0415(7) 0.4664(7) 0.027(4) Uij ? ? C16 0.252(1) 0.0705(8) 0.5508(8) 0.035(4) Uij ? ? C17 0.333(1) 0.0392(8) 0.6182(8) 0.039(4) Uij ? ? C18 0.401(1) -0.0203(9) 0.6046(10) 0.048(5) Uij ? ? C19 0.394(1) -0.0492(9) 0.522(1) 0.050(5) Uij ? ? C20 0.311(1) -0.0201(9) 0.4510(9) 0.041(4) Uij ? ? C21 0.0583(10) 0.4217(7) 0.4094(8) 0.029(4) Uij ? ? C22 -0.049(1) 0.4329(8) 0.3921(9) 0.039(4) Uij ? ? C23 -0.095(1) 0.5109(8) 0.3647(9) 0.042(4) Uij ? ? C24 -0.035(1) 0.5787(8) 0.3535(9) 0.042(4) Uij ? ? C25 0.072(1) 0.5685(8) 0.3700(9) 0.038(4) Uij ? ? C26 0.1198(10) 0.4915(9) 0.3980(8) 0.037(4) Uij ? ? C27 0.029(1) 0.198(1) 0.7659(10) 0.051(5) Uij ? ? H1 -0.1198 0.1347 0.5232 0.0517 Uiso ? ? H2 -0.1973 0.1158 0.4322 0.0517 Uiso ? ? H3 -0.1877 0.2077 0.4697 0.0517 Uiso ? ? H4 -0.1632 0.1648 0.3016 0.0385 Uiso ? ? H5 -0.1650 0.2555 0.3401 0.0385 Uiso ? ? H6 -0.0550 0.0494 0.4011 0.0320 Uiso ? ? H7 0.0309 0.0782 0.4844 0.0320 Uiso ? ? H8 0.0353 0.2155 0.5413 0.0353 Uiso ? ? H9 -0.0393 0.2876 0.4930 0.0353 Uiso ? ? H10 -0.1221 0.0668 0.2108 0.0490 Uiso ? ? H11 -0.1588 -0.0323 0.0931 0.0465 Uiso ? ? H12 -0.1183 0.0062 -0.0366 0.0548 Uiso ? ? H13 -0.0557 0.1420 -0.0509 0.0586 Uiso ? ? H14 -0.0248 0.2441 0.0618 0.0507 Uiso ? ? H15 0.2024 0.1127 0.5613 0.0420 Uiso ? ? H16 0.3410 0.0598 0.6771 0.0450 Uiso ? ? H17 0.4549 -0.0431 0.6513 0.0615 Uiso ? ? H18 0.4452 -0.0885 0.5133 0.0598 Uiso ? ? H19 0.3017 -0.0431 0.3926 0.0494 Uiso ? ? H20 -0.0930 0.3853 0.3997 0.0468 Uiso ? ? H21 -0.1712 0.5178 0.3536 0.0494 Uiso ? ? H22 -0.0673 0.6333 0.3329 0.0517 Uiso ? ? H23 0.1159 0.6168 0.3628 0.0454 Uiso ? ? H24 0.1970 0.4850 0.4097 0.0425 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Te1 0.0347(5) 0.0321(5) 0.0285(5) 0.0043(4) 0.0037(4) 0.0054(4) Te2 0.0354(5) 0.0261(4) 0.0301(5) 0.0025(4) 0.0047(4) -0.0006(4) Te3 0.0309(5) 0.0242(4) 0.0305(5) -0.0012(4) 0.0048(4) 0.0030(4) Mn1 0.033(1) 0.031(1) 0.029(1) 0.0011(9) 0.0069(9) 0.0046(9) S1 0.040(2) 0.027(2) 0.037(2) 0.000(2) 0.010(2) -0.001(2) F1 0.120(9) 0.088(8) 0.100(8) -0.014(7) 0.061(7) -0.052(7) F2 0.068(6) 0.078(7) 0.061(6) 0.013(5) 0.036(5) 0.015(5) F3 0.050(6) 0.091(8) 0.116(8) 0.029(5) 0.030(6) 0.054(7) O1 0.075(8) 0.044(7) 0.069(8) -0.001(6) 0.035(6) 0.022(6) O2 0.038(6) 0.045(6) 0.053(6) 0.009(5) 0.005(5) 0.015(5) O3 0.046(7) 0.100(9) 0.039(7) 0.008(6) 0.014(5) -0.015(6) O4 0.043(6) 0.044(6) 0.028(5) -0.006(5) 0.002(4) 0.005(4) O5 0.035(6) 0.072(7) 0.073(8) 0.006(6) 0.008(6) 0.048(6) O6 0.071(8) 0.054(7) 0.083(8) -0.027(6) 0.042(7) -0.034(6) C1 0.048(10) 0.044(9) 0.042(9) 0.001(8) 0.009(8) 0.015(7) C2 0.038(9) 0.024(7) 0.043(9) 0.000(6) 0.008(7) 0.001(6) C3 0.037(9) 0.054(10) 0.029(8) 0.005(7) 0.005(7) 0.007(7) C4 0.044(9) 0.050(9) 0.039(9) -0.006(7) 0.018(7) 0.009(7) C5 0.028(7) 0.019(7) 0.026(7) -0.009(5) -0.003(6) 0.000(5) C6 0.031(8) 0.040(8) 0.031(8) 0.003(6) 0.011(6) -0.003(6) C7 0.018(7) 0.016(6) 0.047(8) -0.004(5) 0.006(6) -0.004(6) C8 0.031(7) 0.022(7) 0.038(8) -0.005(6) 0.020(6) 0.006(6) C9 0.035(8) 0.029(7) 0.031(8) 0.006(6) 0.000(6) 0.001(6) C10 0.028(8) 0.043(8) 0.041(9) -0.001(7) -0.003(7) 0.011(7) C11 0.045(9) 0.029(8) 0.038(9) 0.006(7) 0.003(7) 0.008(7) C12 0.042(9) 0.049(9) 0.047(10) 0.014(8) 0.007(8) 0.000(8) C13 0.040(9) 0.08(1) 0.030(8) 0.012(9) 0.004(7) 0.003(8) C14 0.047(9) 0.045(9) 0.033(8) 0.005(7) 0.014(7) 0.001(7) C15 0.032(8) 0.021(6) 0.029(7) -0.004(6) 0.011(6) -0.005(5) C16 0.043(9) 0.028(7) 0.035(8) 0.005(6) 0.013(7) 0.003(6) C17 0.047(9) 0.032(7) 0.032(8) 0.005(7) 0.002(7) -0.003(6) C18 0.031(8) 0.050(10) 0.047(10) -0.011(7) -0.014(7) 0.022(8) C19 0.040(9) 0.043(9) 0.06(1) 0.008(7) 0.008(8) 0.011(8) C20 0.039(9) 0.042(9) 0.039(8) 0.004(7) 0.005(7) 0.006(7) C21 0.034(8) 0.023(7) 0.028(7) 0.003(6) 0.006(6) -0.003(6) C22 0.044(9) 0.030(8) 0.044(9) -0.007(7) 0.011(7) -0.002(6) C23 0.030(8) 0.033(8) 0.057(10) 0.001(6) 0.004(7) -0.001(7) C24 0.06(1) 0.024(7) 0.040(9) 0.003(7) 0.018(8) 0.000(7) C25 0.041(9) 0.025(7) 0.057(9) 0.002(7) 0.027(8) 0.011(7) C26 0.028(8) 0.041(8) 0.041(8) -0.010(6) 0.006(7) 0.003(7) C27 0.06(1) 0.06(1) 0.045(10) 0.011(9) 0.026(8) 0.002(9) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2933 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0439 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0457 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.359 _refine_ls_shift/esd_max 0.0090 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.54 _refine_diff_density_max 0.85 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te(1) Mn(1) 2.627(2) ? ? yes Te(1) C(6) 2.16(1) ? ? yes Te(1) C(9) 2.14(1) ? ? yes Te(2) Mn(1) 2.615(2) ? ? yes Te(2) C(7) 2.16(1) ? ? yes Te(2) C(15) 2.13(1) ? ? yes Te(3) Mn(1) 2.643(2) ? ? yes Te(3) C(8) 2.16(1) ? ? yes Te(3) C(21) 2.14(1) ? ? yes Mn(1) C(1) 1.80(1) ? ? yes Mn(1) C(2) 1.80(1) ? ? yes Mn(1) C(3) 1.83(1) ? ? yes S(1) O(4) 1.436(9) ? ? yes S(1) O(5) 1.444(10) ? ? yes S(1) O(6) 1.425(10) ? ? yes S(1) C(27) 1.80(1) ? ? yes F(1) C(27) 1.33(2) ? ? yes F(2) C(27) 1.34(2) ? ? yes F(3) C(27) 1.32(2) ? ? yes O(1) C(1) 1.15(1) ? ? yes O(2) C(2) 1.14(1) ? ? yes O(3) C(3) 1.12(2) ? ? yes C(4) C(5) 1.57(2) ? ? yes C(5) C(6) 1.55(2) ? ? yes C(5) C(7) 1.52(2) ? ? yes C(5) C(8) 1.54(2) ? ? yes C(9) C(10) 1.41(2) ? ? yes C(9) C(14) 1.37(2) ? ? yes C(10) C(11) 1.39(2) ? ? yes C(11) C(12) 1.39(2) ? ? yes C(12) C(13) 1.37(2) ? ? yes C(13) C(14) 1.38(2) ? ? yes C(15) C(16) 1.40(2) ? ? yes C(15) C(20) 1.39(2) ? ? yes C(16) C(17) 1.38(2) ? ? yes C(17) C(18) 1.35(2) ? ? yes C(18) C(19) 1.38(2) ? ? yes C(19) C(20) 1.41(2) ? ? yes C(21) C(22) 1.38(2) ? ? yes C(21) C(26) 1.40(2) ? ? yes C(22) C(23) 1.38(2) ? ? yes C(23) C(24) 1.37(2) ? ? yes C(24) C(25) 1.37(2) ? ? yes C(25) C(26) 1.38(2) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Mn(1) Te(1) C(6) 108.3(3) ? ? ? yes Mn(1) Te(1) C(9) 102.3(3) ? ? ? yes C(6) Te(1) C(9) 100.3(5) ? ? ? yes Mn(1) Te(2) C(7) 108.2(3) ? ? ? yes Mn(1) Te(2) C(15) 105.6(3) ? ? ? yes C(7) Te(2) C(15) 97.5(5) ? ? ? yes Mn(1) Te(3) C(8) 107.3(3) ? ? ? yes Mn(1) Te(3) C(21) 104.0(3) ? ? ? yes C(8) Te(3) C(21) 96.0(5) ? ? ? yes Te(1) Mn(1) Te(2) 87.68(6) ? ? ? yes Te(1) Mn(1) Te(3) 86.07(6) ? ? ? yes Te(1) Mn(1) C(1) 92.0(5) ? ? ? yes Te(1) Mn(1) C(2) 175.6(4) ? ? ? yes Te(1) Mn(1) C(3) 92.1(4) ? ? ? yes Te(2) Mn(1) Te(3) 94.49(6) ? ? ? yes Te(2) Mn(1) C(1) 176.7(5) ? ? ? yes Te(2) Mn(1) C(2) 88.4(4) ? ? ? yes Te(2) Mn(1) C(3) 87.1(4) ? ? ? yes Te(3) Mn(1) C(1) 88.8(5) ? ? ? yes Te(3) Mn(1) C(2) 92.4(4) ? ? ? yes Te(3) Mn(1) C(3) 177.5(4) ? ? ? yes C(1) Mn(1) C(2) 92.0(6) ? ? ? yes C(1) Mn(1) C(3) 89.6(6) ? ? ? yes C(2) Mn(1) C(3) 89.6(6) ? ? ? yes O(4) S(1) O(5) 113.9(5) ? ? ? yes O(4) S(1) O(6) 114.7(6) ? ? ? yes O(4) S(1) C(27) 104.7(7) ? ? ? yes O(5) S(1) O(6) 115.9(7) ? ? ? yes O(5) S(1) C(27) 102.7(7) ? ? ? yes O(6) S(1) C(27) 102.7(7) ? ? ? yes Mn(1) C(1) O(1) 177(1) ? ? ? yes Mn(1) C(2) O(2) 174(1) ? ? ? yes Mn(1) C(3) O(3) 176(1) ? ? ? yes C(4) C(5) C(6) 104.3(10) ? ? ? yes C(4) C(5) C(7) 104.7(9) ? ? ? yes C(4) C(5) C(8) 103.9(10) ? ? ? yes C(6) C(5) C(7) 114(1) ? ? ? yes C(6) C(5) C(8) 115.4(10) ? ? ? yes C(7) C(5) C(8) 112.5(10) ? ? ? yes Te(1) C(6) C(5) 121.1(8) ? ? ? yes Te(2) C(7) C(5) 121.0(8) ? ? ? yes Te(3) C(8) C(5) 122.1(8) ? ? ? yes Te(1) C(9) C(10) 123.9(10) ? ? ? yes Te(1) C(9) C(14) 115.7(10) ? ? ? yes C(10) C(9) C(14) 120(1) ? ? ? yes C(9) C(10) C(11) 120(1) ? ? ? yes C(10) C(11) C(12) 118(1) ? ? ? yes C(11) C(12) C(13) 120(1) ? ? ? yes C(12) C(13) C(14) 121(1) ? ? ? yes C(9) C(14) C(13) 119(1) ? ? ? yes Te(2) C(15) C(16) 122.2(9) ? ? ? yes Te(2) C(15) C(20) 116.1(9) ? ? ? yes C(16) C(15) C(20) 121(1) ? ? ? yes C(15) C(16) C(17) 118(1) ? ? ? yes C(16) C(17) C(18) 121(1) ? ? ? yes C(17) C(18) C(19) 121(1) ? ? ? yes C(18) C(19) C(20) 119(1) ? ? ? yes C(15) C(20) C(19) 118(1) ? ? ? yes Te(3) C(21) C(22) 124.4(9) ? ? ? yes Te(3) C(21) C(26) 117.2(9) ? ? ? yes C(22) C(21) C(26) 118(1) ? ? ? yes C(21) C(22) C(23) 120(1) ? ? ? yes C(22) C(23) C(24) 120(1) ? ? ? yes C(23) C(24) C(25) 119(1) ? ? ? yes C(24) C(25) C(26) 121(1) ? ? ? yes C(21) C(26) C(25) 119(1) ? ? ? yes S(1) C(27) F(1) 111(1) ? ? ? yes S(1) C(27) F(2) 112(1) ? ? ? yes S(1) C(27) F(3) 112(1) ? ? ? yes F(1) C(27) F(2) 108(1) ? ? ? yes F(1) C(27) F(3) 105(1) ? ? ? yes F(2) C(27) F(3) 106(1) ? ? ? yes #------------------------------------------------------------------------------ _publ_contact_author ; Dr G. Reid Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [Mn(CO)~3~{MeC(CH~2~TePh)~3~}]CF~3~SO~3~' ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk '