# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1345 data_sdote3_[Mn(CO)3{Te3)]CF3SO3 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jan 18 14:36:07 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 8.989(3) _cell_length_b 10.033(2) _cell_length_c 12.086(2) _cell_angle_alpha 90 _cell_angle_beta 104.85(1) _cell_angle_gamma 90 _cell_volume 1053.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 18 _cell_measurement_2theta_min 20.0 _cell_measurement_2theta_max 26.2 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/m ' _symmetry_Int_Tables_number 11 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' ' -x, -y, -z' ' +x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'XDIM' _exptl_crystal_colour 'pale' _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.040 _exptl_crystal_density_diffrn 2.474 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 785.06 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H18 F3 Mn O6 S Te3 ' _chemical_formula_moiety '[Mn(CO)~3~{MeC(CH~2~TeMe)~3~}]CF~3~SO~3~'' _chemical_formula_structural ? _chemical_compound_source 'CH~2~Cl~2~/petroleum ether' _exptl_crystal_F_000 724.00 _exptl_absorpt_coefficient_mu 4.847 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.848 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 150.0 _diffrn_radiation_wavelength 0.7107 _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_% -0.01 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 1 -1 2 3 -1 1 2 3 _diffrn_reflns_number 2107 _reflns_number_total 1977 _reflns_number_observed 1603 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_2theta_min ? _diffrn_reflns_2theta_max 24.99 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.01558 _diffrn_orient_matrix_UB_12 0.09436 _diffrn_orient_matrix_UB_13 0.02714 _diffrn_orient_matrix_UB_21 0.00848 _diffrn_orient_matrix_UB_22 -0.03027 _diffrn_orient_matrix_UB_23 0.08022 _diffrn_orient_matrix_UB_31 0.11372 _diffrn_orient_matrix_UB_32 -0.01067 _diffrn_orient_matrix_UB_33 0.01250 #------------------------------------------------------------------------------ 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 2 0.125 0.123 'International Tables' F 0 6 0.017 0.010 'International Tables' Te 0 6 -0.531 1.675 '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 _atom_site_occupancy_factor Te(1) 0.04480(5) 0.2500 0.40077(4) 0.0165(1) Uij ? ? 0.5 Te(2) 0.27663(4) 0.06744(4) 0.23951(3) 0.0270(1) Uij ? ? 1.0 Mn(1) 0.3333(1) 0.2500 0.39821(9) 0.0155(3) Uij ? ? 0.5 S(1) 0.1837(2) 0.2500 0.7933(2) 0.0309(6) Uij ? ? 0.5 F(1) 0.4786(7) 0.2500 0.8124(7) 0.086(3) Uij ? ? 0.5 F(2) 0.3517(9) 0.0459(8) 0.8100(7) 0.049(2) Uij ? ? 0.5 F(3) 0.405(1) 0.162(1) 0.9606(6) 0.077(3) Uij ? ? 0.5 O(1) 0.3955(5) 0.0465(4) 0.5802(3) 0.031(1) Uij ? ? 1.0 O(2) 0.6587(6) 0.2500 0.3916(5) 0.037(2) Uij ? ? 0.5 O(3) 0.1633(7) 0.2500 0.6717(5) 0.045(2) Uij ? ? 0.5 O(4) 0.212(1) 0.111(1) 0.8493(9) 0.061(3) Uij ? ? 0.5 O(5) 0.078(1) 0.182(1) 0.8331(9) 0.057(3) Uij ? ? 0.5 C(1) 0.3693(6) 0.1241(6) 0.5074(4) 0.022(1) Uij ? ? 1.0 C(2) 0.5299(9) 0.2500 0.3915(6) 0.022(2) Uij ? ? 0.5 C(3) -0.009(1) 0.053(1) 0.434(1) 0.034(3) Uij ? ? 0.5 C(4) -0.0927(10) 0.2500 0.2251(7) 0.035(2) Uij ? ? 0.5 C(5) -0.0202(8) 0.2500 0.1235(6) 0.022(2) Uij ? ? 0.5 C(6) -0.1572(9) 0.2500 0.0174(7) 0.031(2) Uij ? ? 0.5 C(7) 0.0670(6) 0.1220(6) 0.1146(4) 0.026(1) Uij ? ? 1.0 C(8) 0.430(1) 0.085(1) 0.1406(9) 0.029(3) Uij ? ? 0.5 C(9) 0.203(1) -0.091(1) 0.3058(9) 0.030(3) Uij ? ? 0.5 C(10) 0.368(1) 0.168(1) 0.8469(10) 0.034(3) Uij ? ? 0.5 H(1) -0.1179 0.0426 0.4225 0.0418 Uiso ? ? ? H(2) 0.0240 -0.0076 0.3837 0.0418 Uiso ? ? ? H(3) 0.0403 0.0287 0.5110 0.0418 Uiso ? ? ? H(4) -0.1531 0.1727 0.2166 0.0420 Uiso ? ? ? H(5) -0.1531 0.3273 0.2166 0.0420 Uiso ? ? ? H(6) -0.2164 0.3281 0.0176 0.0376 Uiso ? ? ? H(7) -0.1201 0.2500 -0.0495 0.0376 Uiso ? ? ? H(8) -0.2184 0.1735 0.0190 0.0376 Uiso ? ? ? H(9) 0.0923 0.1259 0.0428 0.0304 Uiso ? ? ? H(10) -0.0035 0.0514 0.1135 0.0304 Uiso ? ? ? H(11) 0.5304 0.0627 0.1855 0.0345 Uiso ? ? ? H(12) 0.4015 0.0263 0.0774 0.0345 Uiso ? ? ? H(13) 0.4298 0.1741 0.1144 0.0345 Uiso ? ? ? H(14) 0.1220 -0.0656 0.3385 0.0356 Uiso ? ? ? H(15) 0.1680 -0.1550 0.2479 0.0356 Uiso ? ? ? H(16) 0.2858 -0.1267 0.3639 0.0356 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 Te(1) 0.0143(2) 0.0193(3) 0.0163(2) 0.0000 0.0046(2) 0.0000 Te(2) 0.0277(2) 0.0289(2) 0.0224(2) 0.0091(2) 0.0027(2) -0.0086(2) Mn(1) 0.0134(5) 0.0181(6) 0.0146(5) 0.0000 0.0030(4) 0.0000 S(1) 0.024(1) 0.046(1) 0.022(1) 0.0000 0.0070(9) 0.0000 F(1) 0.025(3) 0.125(7) 0.108(6) 0.0000 0.017(4) 0.0000 F(2) 0.053(5) 0.040(5) 0.054(5) 0.021(4) 0.013(4) 0.006(4) F(3) 0.088(7) 0.101(7) 0.030(4) 0.055(6) -0.007(4) 0.001(5) O(1) 0.034(2) 0.031(2) 0.028(2) 0.015(2) 0.011(2) 0.014(2) O(2) 0.017(3) 0.039(4) 0.056(4) 0.0000 0.013(3) 0.0000 O(3) 0.041(4) 0.072(5) 0.019(3) 0.0000 0.003(3) 0.0000 O(4) 0.063(7) 0.055(7) 0.057(6) -0.015(6) 0.001(5) 0.020(6) O(5) 0.042(5) 0.070(7) 0.068(7) 0.009(5) 0.030(5) 0.035(5) C(1) 0.013(3) 0.030(3) 0.022(3) 0.003(2) 0.005(2) -0.005(3) C(2) 0.018(4) 0.022(4) 0.023(4) 0.0000 0.003(3) 0.0000 C(3) 0.024(6) 0.024(7) 0.053(8) -0.008(5) 0.008(5) 0.016(6) C(4) 0.023(4) 0.057(6) 0.023(4) 0.0000 0.003(3) 0.0000 C(5) 0.014(4) 0.031(5) 0.018(4) 0.0000 -0.002(3) 0.0000 C(6) 0.025(4) 0.035(5) 0.030(5) 0.0000 0.000(4) 0.0000 C(7) 0.026(3) 0.025(3) 0.022(3) 0.000(2) -0.002(2) -0.004(2) C(8) 0.030(6) 0.039(7) 0.020(5) 0.002(5) 0.011(5) 0.002(5) C(9) 0.031(6) 0.030(7) 0.023(6) 0.009(5) -0.004(5) -0.001(5) C(10) 0.034(7) 0.038(8) 0.029(6) 0.000(6) 0.004(5) -0.002(6) #------------------------------------------------------------------------------ _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 1603 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0255 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0337 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.079 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.62 _refine_diff_density_max 0.48 #------------------------------------------------------------------------------ _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) 2.601(2) ? ? yes Te(1) C(3) 2.10(1) ? ? yes Te(1) C(4) 2.165(8) ? ? yes Te(2) Mn(1) 2.6063(8) ? ? yes Te(2) C(7) 2.162(5) ? ? yes Te(2) C(8) 2.05(1) ? ? yes Te(2) C(9) 1.97(1) ? ? yes Mn(1) C(1) 1.795(6) ? ? yes Mn(1) C(2) 1.790(8) ? ? yes S(1) O(3) 1.433(6) ? ? yes S(1) O(4) 1.55(1) ? ? yes S(1) O(5) 1.36(1) ? ? yes S(1) C(10) 1.81(1) ? ? yes F(1) C(10) 1.43(1) ? ? yes F(2) C(10) 1.30(2) ? ? yes F(3) C(10) 1.33(1) ? ? yes C(4) C(5) 1.53(1) ? ? yes C(5) C(6) 1.534(10) ? ? yes C(5) C(7) 1.523(7) ? ? 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(3) 106.4(3) ? ? ? yes Mn(1) Te(1) C(4) 108.0(3) ? ? ? yes C(3) Te(1) C(3) 140.9(8) ? ? ? yes C(3) Te(1) C(4) 94.8(3) ? ? ? yes Mn(1) Te(2) C(7) 107.9(2) ? ? ? yes Mn(1) Te(2) C(8) 109.5(3) ? ? ? yes Mn(1) Te(2) C(9) 106.9(3) ? ? ? yes C(7) Te(2) C(8) 99.6(3) ? ? ? yes C(7) Te(2) C(9) 99.6(3) ? ? ? yes C(8) Te(2) C(9) 130.8(5) ? ? ? yes Te(1) Mn(1) Te(2) 90.08(3) ? ? ? yes Te(1) Mn(1) C(1) 89.1(2) ? ? ? yes Te(1) Mn(1) C(2) 178.1(2) ? ? ? yes Te(2) Mn(1) Te(2*) 89.31(4) ? ? ? yes Te(2) Mn(1) C(1) 90.6(2) ? ? ? yes Te(2) Mn(1) C(1*) 179.1(2) ? ? ? yes Te(2) Mn(1) C(2) 88.6(2) ? ? ? yes Te(2) Mn(1) C(1) 179.1(2) ? ? ? yes Te(2) Mn(1) C(1*) 90.6(2) ? ? ? yes Te(2) Mn(1) C(2) 88.6(2) ? ? ? yes C(1) Mn(1) C(1*) 89.4(4) ? ? ? yes C(1) Mn(1) C(2) 92.2(2) ? ? ? yes O(3) S(1) O(4) 114.4(4) ? ? ? yes O(3) S(1) O(5) 116.6(5) ? ? ? yes O(3) S(1) C(10) 103.4(5) ? ? ? yes O(4) S(1) O(4) 129.5(8) ? ? ? yes O(4) S(1) O(5) 110.5(7) ? ? ? yes O(4) S(1) C(10) 102.8(6) ? ? ? yes O(4) S(1) O(5) 110.5(7) ? ? ? yes O(4) S(1) C(10) 102.8(6) ? ? ? yes O(5) S(1) C(10) 107.8(6) ? ? ? yes O(5) S(1) C(10) 139.6(6) ? ? ? yes O(5) S(1) C(10) 107.8(6) ? ? ? yes Mn(1) C(1) O(1) 177.6(5) ? ? ? yes Mn(1) C(2) O(2) 177.4(7) ? ? ? yes Te(1) C(4) C(5) 122.2(5) ? ? ? yes C(4) C(5) C(6) 104.8(6) ? ? ? yes C(4) C(5) C(7) 112.9(4) ? ? ? yes C(4) C(5) C(7) 112.9(4) ? ? ? yes C(6) C(5) C(7) 105.0(4) ? ? ? yes C(6) C(5) C(7) 105.0(4) ? ? ? yes C(7) C(5) C(7) 115.0(7) ? ? ? yes Te(2) C(7) C(5) 122.5(4) ? ? ? yes S(1) C(10) F(1) 106.0(7) ? ? ? yes S(1) C(10) F(2) 107.0(8) ? ? ? yes S(1) C(10) F(3) 110.8(10) ? ? ? yes F(1) C(10) F(2) 117(1) ? ? ? yes F(1) C(10) F(3) 108.7(9) ? ? ? yes F(1) C(10) O(4) 159.2(10) ? ? ? yes F(2) C(10) F(3) 106(1) ? ? ? 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 ; Dear Debbie, This is the CIF file for the crystal stucture of [Mn(CO)~3~{MeC(CH~2~TeMe)~3~}]CF~3~SO~3~ which is included in the -Dalton Communication which we have submitted for publication (9/00615J). I hope that this is OK, Gill ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' loop_ _publ_section_title ; Spectroscopic and Structural Characterisation of fac-[Mn(CO)~3~{MeC(CH~2~TeMe)~3~}]CF~3~SO~3~: the First Transition Metal Complex of a Tridentate Telluroether. ;