# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1415 data_sjp3 #'[MnCl(CO)~3~{o-C~6~H~4~(PPh~2~)~2~}]' #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jan 25 13:48:15 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 16.858(2) _cell_length_b 10.915(4) _cell_length_c 17.615(4) _cell_angle_alpha 90 _cell_angle_beta 116.72(1) _cell_angle_gamma 90 _cell_volume 2895(1) _cell_formula_units_Z 4 _cell_measurement_temperature 150.1 _cell_measurement_reflns_used 24 _cell_measurement_2theta_min 20.3 _cell_measurement_2theta_max 29.0 #------------------------------------------------------------------------------ _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 'hexplate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.350 _exptl_crystal_size_min 0.220 _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 620.89 _chemical_formula_analytical ? _chemical_formula_sum 'C33 H24 Cl Mn O3 P2 ' _chemical_formula_moiety 'C33 H24 Cl Mn O3 P2 ' _chemical_formula_structural '[MnCl(CO)~3~{o-C~6~H~4~(PPh~2~)~2~}]' _chemical_compound_source 'diffusion of pet ether into CHCl~3~ solution' _exptl_crystal_F_000 1272.00 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.905 #------------------------------------------------------------------------------ _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_% -0.64 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 4 -2 3 3 -3 2 3 -4 _diffrn_reflns_number 5575 _reflns_number_total 5385 _reflns_number_observed 2708 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_2theta_min ? _diffrn_reflns_2theta_max 25.02 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.03505 _diffrn_orient_matrix_UB_12 0.00203 _diffrn_orient_matrix_UB_13 -0.03312 _diffrn_orient_matrix_UB_21 -0.05421 _diffrn_orient_matrix_UB_22 0.02650 _diffrn_orient_matrix_UB_23 -0.05172 _diffrn_orient_matrix_UB_31 0.01557 _diffrn_orient_matrix_UB_32 0.08768 _diffrn_orient_matrix_UB_33 0.01639 #------------------------------------------------------------------------------ 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 0 132 0.003 0.002 'International Tables' H 0 96 0.000 0.000 'International Tables' O 0 12 0.011 0.006 'International Tables' P 0 8 0.102 0.094 'International Tables' Cl 0 4 0.148 0.159 'International Tables' Mn 0 4 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) 0.03210(6) 0.10428(8) 0.29799(5) 0.0252(2) Uij ? ? Cl(1) 0.12716(10) -0.0523(1) 0.29071(9) 0.0341(5) Uij ? ? P(1) 0.14399(10) 0.1354(1) 0.43506(9) 0.0263(4) Uij ? ? P(2) 0.11887(10) 0.2381(1) 0.26486(9) 0.0244(4) Uij ? ? O(1) -0.0879(3) 0.2949(4) 0.3041(3) 0.043(1) Uij ? ? O(2) -0.0650(3) -0.0844(5) 0.3434(3) 0.062(2) Uij ? ? O(3) -0.0970(3) 0.0635(4) 0.1193(3) 0.053(2) Uij ? ? C(1) -0.0389(4) 0.2222(6) 0.3038(3) 0.030(2) Uij ? ? C(2) -0.0254(4) -0.0089(6) 0.3290(4) 0.037(2) Uij ? ? C(3) -0.0448(4) 0.0797(5) 0.1883(4) 0.033(2) Uij ? ? C(4) 0.2458(3) 0.1726(5) 0.4251(3) 0.027(2) Uij ? ? C(5) 0.3306(4) 0.1555(6) 0.4898(3) 0.034(2) Uij ? ? C(6) 0.4039(4) 0.1849(6) 0.4769(4) 0.040(2) Uij ? ? C(7) 0.3905(4) 0.2341(6) 0.3993(4) 0.039(2) Uij ? ? C(8) 0.3070(4) 0.2517(6) 0.3349(3) 0.031(2) Uij ? ? C(9) 0.2332(3) 0.2213(5) 0.3466(3) 0.026(2) Uij ? ? C(10) 0.1295(4) 0.2649(6) 0.4939(3) 0.030(2) Uij ? ? C(11) 0.0550(4) 0.2621(6) 0.5087(4) 0.036(2) Uij ? ? C(12) 0.0442(4) 0.3531(7) 0.5586(4) 0.047(2) Uij ? ? C(13) 0.1037(5) 0.4442(7) 0.5919(4) 0.057(2) Uij ? ? C(14) 0.1787(4) 0.4468(6) 0.5772(4) 0.048(2) Uij ? ? C(15) 0.1903(4) 0.3578(6) 0.5274(4) 0.038(2) Uij ? ? C(16) 0.1778(4) 0.0132(6) 0.5154(4) 0.031(2) Uij ? ? C(17) 0.1617(4) -0.1085(6) 0.4929(4) 0.037(2) Uij ? ? C(18) 0.1876(4) -0.2002(6) 0.5539(4) 0.047(2) Uij ? ? C(19) 0.2323(4) -0.1691(7) 0.6393(5) 0.052(3) Uij ? ? C(20) 0.2498(4) -0.0470(8) 0.6637(4) 0.050(2) Uij ? ? C(21) 0.2222(4) 0.0428(6) 0.6030(4) 0.042(2) Uij ? ? C(22) 0.0934(3) 0.4003(5) 0.2671(3) 0.026(2) Uij ? ? C(23) 0.1535(4) 0.4860(6) 0.3217(4) 0.033(2) Uij ? ? C(24) 0.1280(4) 0.6061(6) 0.3200(4) 0.040(2) Uij ? ? C(25) 0.0439(4) 0.6428(6) 0.2635(4) 0.042(2) Uij ? ? C(26) -0.0163(4) 0.5600(6) 0.2094(4) 0.038(2) Uij ? ? C(27) 0.0090(4) 0.4392(5) 0.2111(4) 0.032(2) Uij ? ? C(28) 0.1249(3) 0.2246(5) 0.1633(3) 0.024(2) Uij ? ? C(29) 0.1486(3) 0.3260(5) 0.1298(3) 0.030(2) Uij ? ? C(30) 0.1533(4) 0.3126(6) 0.0527(4) 0.035(2) Uij ? ? C(31) 0.1355(4) 0.2016(6) 0.0112(3) 0.036(2) Uij ? ? C(32) 0.1103(4) 0.1017(6) 0.0441(3) 0.034(2) Uij ? ? C(33) 0.1068(3) 0.1140(5) 0.1211(3) 0.031(2) Uij ? ? H(1) 0.3334 0.0978 0.5412 0.0472 Uiso ? ? H(2) 0.4669 0.1697 0.5282 0.0472 Uiso ? ? H(3) 0.4439 0.2568 0.3886 0.0472 Uiso ? ? H(4) 0.2953 0.2832 0.2784 0.0472 Uiso ? ? H(5) 0.0108 0.1711 0.4869 0.0472 Uiso ? ? H(6) -0.0128 0.3622 0.5677 0.0472 Uiso ? ? H(7) 0.1079 0.5174 0.6329 0.0472 Uiso ? ? H(8) 0.2254 0.5183 0.5923 0.0472 Uiso ? ? H(9) 0.2484 0.3588 0.5189 0.0472 Uiso ? ? H(10) 0.1235 -0.1387 0.4276 0.0472 Uiso ? ? H(11) 0.1843 -0.3041 0.5308 0.0472 Uiso ? ? H(12) 0.2504 -0.2331 0.6818 0.0472 Uiso ? ? H(13) 0.2904 -0.0283 0.7291 0.0472 Uiso ? ? H(14) 0.2433 0.1466 0.6205 0.0472 Uiso ? ? H(15) 0.2154 0.4608 0.3734 0.0472 Uiso ? ? H(16) 0.1833 0.6663 0.3685 0.0472 Uiso ? ? H(17) 0.0188 0.7310 0.2582 0.0472 Uiso ? ? H(18) -0.0812 0.5886 0.1641 0.0472 Uiso ? ? H(19) -0.0404 0.3724 0.1676 0.0472 Uiso ? ? H(20) 0.1719 0.4098 0.1611 0.0472 Uiso ? ? H(21) 0.1653 0.3818 0.0237 0.0472 Uiso ? ? H(22) 0.1310 0.1972 -0.0546 0.0472 Uiso ? ? H(23) 0.1085 0.0153 0.0169 0.0472 Uiso ? ? H(24) 0.0777 0.0325 0.1290 0.0472 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) 0.0232(5) 0.0285(5) 0.0268(5) -0.0008(5) 0.0139(4) -0.0022(4) Cl(1) 0.0368(9) 0.0304(9) 0.0402(9) 0.0030(7) 0.0218(8) -0.0013(7) P(1) 0.0257(8) 0.0302(9) 0.0251(8) 0.0005(7) 0.0132(7) 0.0001(7) P(2) 0.0222(8) 0.0288(9) 0.0225(8) -0.0013(7) 0.0104(7) -0.0017(7) O(1) 0.036(3) 0.043(3) 0.056(3) 0.011(2) 0.028(2) -0.001(2) O(2) 0.051(3) 0.058(3) 0.093(4) -0.002(3) 0.046(3) 0.019(3) O(3) 0.035(3) 0.080(4) 0.038(3) -0.004(3) 0.011(2) -0.021(3) C(1) 0.027(4) 0.038(4) 0.024(3) -0.009(3) 0.009(3) 0.002(3) C(2) 0.035(4) 0.037(4) 0.046(4) 0.005(3) 0.025(3) 0.003(3) C(3) 0.028(4) 0.037(4) 0.040(4) -0.003(3) 0.021(3) -0.005(3) C(4) 0.025(3) 0.031(4) 0.028(3) 0.000(3) 0.016(3) 0.001(3) C(5) 0.031(4) 0.044(4) 0.029(3) 0.002(3) 0.014(3) 0.003(3) C(6) 0.026(4) 0.060(5) 0.030(4) 0.001(3) 0.009(3) -0.001(3) C(7) 0.022(3) 0.061(5) 0.037(4) -0.004(3) 0.017(3) -0.004(4) C(8) 0.021(3) 0.042(4) 0.030(3) -0.003(3) 0.012(3) 0.001(3) C(9) 0.022(3) 0.031(4) 0.023(3) 0.000(3) 0.008(2) 0.000(3) C(10) 0.031(3) 0.037(4) 0.021(3) 0.007(3) 0.011(3) 0.003(3) C(11) 0.039(4) 0.042(4) 0.029(3) 0.008(3) 0.017(3) 0.002(3) C(12) 0.048(4) 0.058(5) 0.035(4) 0.022(4) 0.018(3) 0.001(4) C(13) 0.067(5) 0.052(5) 0.029(4) 0.029(4) 0.002(4) -0.011(4) C(14) 0.050(5) 0.040(4) 0.044(4) 0.001(4) 0.012(4) -0.008(4) C(15) 0.037(4) 0.042(4) 0.032(4) 0.002(3) 0.011(3) -0.001(3) C(16) 0.031(4) 0.043(4) 0.030(3) 0.004(3) 0.022(3) 0.007(3) C(17) 0.029(3) 0.042(4) 0.044(4) -0.001(3) 0.019(3) 0.006(4) C(18) 0.039(4) 0.048(5) 0.055(5) 0.008(4) 0.022(4) 0.017(4) C(19) 0.039(4) 0.071(6) 0.056(5) 0.019(4) 0.031(4) 0.038(5) C(20) 0.037(4) 0.086(6) 0.031(4) 0.020(4) 0.018(3) 0.020(4) C(21) 0.033(4) 0.060(5) 0.039(4) 0.005(4) 0.022(3) 0.005(4) C(22) 0.027(3) 0.031(3) 0.023(3) -0.003(3) 0.014(3) 0.002(3) C(23) 0.031(4) 0.032(4) 0.030(3) -0.007(3) 0.009(3) 0.000(3) C(24) 0.045(4) 0.030(4) 0.042(4) -0.009(4) 0.018(3) -0.007(3) C(25) 0.053(4) 0.032(4) 0.059(4) 0.005(4) 0.040(4) 0.007(4) C(26) 0.030(4) 0.035(4) 0.050(4) 0.005(3) 0.020(3) 0.009(3) C(27) 0.032(4) 0.033(4) 0.032(4) -0.003(3) 0.014(3) -0.002(3) C(28) 0.015(3) 0.038(4) 0.016(3) 0.002(3) 0.005(2) 0.001(3) C(29) 0.018(3) 0.042(4) 0.025(3) -0.010(3) 0.006(3) -0.002(3) C(30) 0.027(3) 0.052(4) 0.028(3) -0.005(3) 0.014(3) 0.005(3) C(31) 0.025(3) 0.057(5) 0.024(3) -0.002(3) 0.009(3) -0.002(3) C(32) 0.032(3) 0.044(4) 0.029(3) 0.003(3) 0.016(3) -0.009(3) C(33) 0.024(3) 0.037(4) 0.029(3) -0.001(3) 0.010(3) -0.007(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 2708 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0428 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0395 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.720 _refine_ls_shift/esd_max 0.1700 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.36 _refine_diff_density_max 0.41 #------------------------------------------------------------------------------ _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) Cl(1) 2.386(2) ? ? yes Mn(1) P(1) 2.325(2) ? ? yes Mn(1) P(2) 2.320(2) ? ? yes Mn(1) C(1) 1.791(6) ? ? yes Mn(1) C(2) 1.800(6) ? ? yes Mn(1) C(3) 1.798(6) ? ? yes P(1) C(4) 1.847(5) ? ? yes P(1) C(10) 1.832(6) ? ? yes P(1) C(16) 1.839(6) ? ? yes P(2) C(9) 1.823(5) ? ? yes P(2) C(22) 1.826(6) ? ? yes P(2) C(28) 1.842(5) ? ? yes O(1) C(1) 1.148(7) ? ? yes O(2) C(2) 1.158(7) ? ? yes O(3) C(3) 1.149(6) ? ? yes C(4) C(5) 1.383(7) ? ? yes C(4) C(9) 1.406(7) ? ? yes C(5) C(6) 1.391(8) ? ? yes C(5) H(1) 1.086 ? ? no C(6) C(7) 1.389(8) ? ? yes C(6) H(2) 1.053 ? ? no C(7) C(8) 1.368(7) ? ? yes C(7) H(3) 1.029 ? ? no C(8) C(9) 1.389(7) ? ? yes C(8) H(4) 0.986 ? ? no C(10) C(11) 1.393(7) ? ? yes C(10) C(15) 1.372(8) ? ? yes C(11) C(12) 1.391(8) ? ? yes C(11) H(5) 1.197 ? ? no C(12) C(13) 1.345(9) ? ? yes C(12) H(6) 1.048 ? ? no C(13) C(14) 1.400(9) ? ? yes C(13) H(7) 1.057 ? ? no C(14) C(15) 1.380(8) ? ? yes C(14) H(8) 1.054 ? ? no C(15) H(9) 1.057 ? ? no C(16) C(17) 1.378(8) ? ? yes C(16) C(21) 1.416(8) ? ? yes C(17) C(18) 1.387(8) ? ? yes C(17) H(10) 1.088 ? ? no C(18) C(19) 1.388(9) ? ? yes C(18) H(11) 1.197 ? ? no C(19) C(20) 1.391(10) ? ? yes C(19) H(12) 0.967 ? ? no C(20) C(21) 1.369(9) ? ? yes C(20) H(13) 1.062 ? ? no C(21) H(14) 1.186 ? ? no C(22) C(23) 1.397(7) ? ? yes C(22) C(27) 1.384(7) ? ? yes C(23) C(24) 1.376(8) ? ? yes C(23) H(15) 1.068 ? ? no C(24) C(25) 1.376(8) ? ? yes C(24) H(16) 1.146 ? ? no C(25) C(26) 1.373(8) ? ? yes C(25) H(17) 1.039 ? ? no C(26) C(27) 1.381(8) ? ? yes C(26) H(18) 1.070 ? ? no C(27) H(19) 1.112 ? ? no C(28) C(29) 1.395(7) ? ? yes C(28) C(33) 1.378(7) ? ? yes C(29) C(30) 1.404(7) ? ? yes C(29) H(20) 1.049 ? ? no C(30) C(31) 1.377(8) ? ? yes C(30) H(21) 0.982 ? ? no C(31) C(32) 1.388(8) ? ? yes C(31) H(22) 1.127 ? ? no C(32) C(33) 1.390(7) ? ? yes C(32) H(23) 1.052 ? ? no C(33) H(24) 1.055 ? ? 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 Cl(1) Mn(1) P(1) 84.82(6) ? ? ? yes Cl(1) Mn(1) P(2) 85.59(6) ? ? ? yes Cl(1) Mn(1) C(1) 179.8(2) ? ? ? yes Cl(1) Mn(1) C(2) 89.5(2) ? ? ? yes Cl(1) Mn(1) C(3) 90.7(2) ? ? ? yes P(1) Mn(1) P(2) 81.97(6) ? ? ? yes P(1) Mn(1) C(1) 95.0(2) ? ? ? yes P(1) Mn(1) C(2) 94.7(2) ? ? ? yes P(1) Mn(1) C(3) 173.6(2) ? ? ? yes P(2) Mn(1) C(1) 94.3(2) ? ? ? yes P(2) Mn(1) C(2) 174.3(2) ? ? ? yes P(2) Mn(1) C(3) 93.2(2) ? ? ? yes C(1) Mn(1) C(2) 90.6(2) ? ? ? yes C(1) Mn(1) C(3) 89.5(2) ? ? ? yes C(2) Mn(1) C(3) 89.8(3) ? ? ? yes Mn(1) P(1) C(4) 106.7(2) ? ? ? yes Mn(1) P(1) C(10) 116.6(2) ? ? ? yes Mn(1) P(1) C(16) 121.3(2) ? ? ? yes C(4) P(1) C(10) 104.5(3) ? ? ? yes C(4) P(1) C(16) 104.7(2) ? ? ? yes C(10) P(1) C(16) 101.4(3) ? ? ? yes Mn(1) P(2) C(9) 107.5(2) ? ? ? yes Mn(1) P(2) C(22) 115.1(2) ? ? ? yes Mn(1) P(2) C(28) 120.7(2) ? ? ? yes C(9) P(2) C(22) 104.8(3) ? ? ? yes C(9) P(2) C(28) 104.9(2) ? ? ? yes C(22) P(2) C(28) 102.4(2) ? ? ? yes Mn(1) C(1) O(1) 176.5(5) ? ? ? yes Mn(1) C(2) O(2) 175.5(6) ? ? ? yes Mn(1) C(3) O(3) 176.9(5) ? ? ? yes P(1) C(4) C(5) 123.5(4) ? ? ? yes P(1) C(4) C(9) 116.2(4) ? ? ? yes C(5) C(4) C(9) 120.3(5) ? ? ? yes C(4) C(5) C(6) 119.9(5) ? ? ? yes C(4) C(5) H(1) 114.0 ? ? ? no C(6) C(5) H(1) 124.1 ? ? ? no C(5) C(6) C(7) 119.1(5) ? ? ? yes C(5) C(6) H(2) 116.8 ? ? ? no C(7) C(6) H(2) 124.0 ? ? ? no C(6) C(7) C(8) 121.5(5) ? ? ? yes C(6) C(7) H(3) 120.3 ? ? ? no C(8) C(7) H(3) 118.2 ? ? ? no C(7) C(8) C(9) 120.0(5) ? ? ? yes C(7) C(8) H(4) 123.4 ? ? ? no C(9) C(8) H(4) 116.6 ? ? ? no P(2) C(9) C(4) 116.9(4) ? ? ? yes P(2) C(9) C(8) 124.0(4) ? ? ? yes C(4) C(9) C(8) 119.1(5) ? ? ? yes P(1) C(10) C(11) 116.7(5) ? ? ? yes P(1) C(10) C(15) 123.4(4) ? ? ? yes C(11) C(10) C(15) 119.8(6) ? ? ? yes C(10) C(11) C(12) 119.2(6) ? ? ? yes C(10) C(11) H(5) 116.2 ? ? ? no C(12) C(11) H(5) 123.8 ? ? ? no C(11) C(12) C(13) 121.3(6) ? ? ? yes C(11) C(12) H(6) 123.6 ? ? ? no C(13) C(12) H(6) 114.7 ? ? ? no C(12) C(13) C(14) 119.4(6) ? ? ? yes C(12) C(13) H(7) 131.6 ? ? ? no C(14) C(13) H(7) 108.8 ? ? ? no C(13) C(14) C(15) 120.1(6) ? ? ? yes C(13) C(14) H(8) 127.0 ? ? ? no C(15) C(14) H(8) 112.2 ? ? ? no C(10) C(15) C(14) 120.2(6) ? ? ? yes C(10) C(15) H(9) 120.5 ? ? ? no C(14) C(15) H(9) 119.2 ? ? ? no P(1) C(16) C(17) 121.7(5) ? ? ? yes P(1) C(16) C(21) 120.1(5) ? ? ? yes C(17) C(16) C(21) 118.2(6) ? ? ? yes C(16) C(17) C(18) 121.4(6) ? ? ? yes C(16) C(17) H(10) 122.9 ? ? ? no C(18) C(17) H(10) 115.6 ? ? ? no C(17) C(18) C(19) 119.4(7) ? ? ? yes C(17) C(18) H(11) 118.1 ? ? ? no C(19) C(18) H(11) 121.3 ? ? ? no C(18) C(19) C(20) 120.4(6) ? ? ? yes C(18) C(19) H(12) 119.4 ? ? ? no C(20) C(19) H(12) 120.2 ? ? ? no C(19) C(20) C(21) 119.6(6) ? ? ? yes C(19) C(20) H(13) 117.6 ? ? ? no C(21) C(20) H(13) 122.5 ? ? ? no C(16) C(21) C(20) 121.0(7) ? ? ? yes C(16) C(21) H(14) 116.8 ? ? ? no C(20) C(21) H(14) 121.6 ? ? ? no P(2) C(22) C(23) 124.0(4) ? ? ? yes P(2) C(22) C(27) 117.3(4) ? ? ? yes C(23) C(22) C(27) 118.7(6) ? ? ? yes C(22) C(23) C(24) 120.0(6) ? ? ? yes C(22) C(23) H(15) 123.0 ? ? ? no C(24) C(23) H(15) 116.0 ? ? ? no C(23) C(24) C(25) 120.2(6) ? ? ? yes C(23) C(24) H(16) 112.9 ? ? ? no C(25) C(24) H(16) 126.9 ? ? ? no C(24) C(25) C(26) 120.7(6) ? ? ? yes C(24) C(25) H(17) 125.5 ? ? ? no C(26) C(25) H(17) 113.8 ? ? ? no C(25) C(26) C(27) 119.3(6) ? ? ? yes C(25) C(26) H(18) 120.9 ? ? ? no C(27) C(26) H(18) 119.8 ? ? ? no C(22) C(27) C(26) 121.1(6) ? ? ? yes C(22) C(27) H(19) 120.0 ? ? ? no C(26) C(27) H(19) 118.9 ? ? ? no P(2) C(28) C(29) 119.9(4) ? ? ? yes P(2) C(28) C(33) 119.9(4) ? ? ? yes C(29) C(28) C(33) 120.2(5) ? ? ? yes C(28) C(29) C(30) 118.6(5) ? ? ? yes C(28) C(29) H(20) 125.5 ? ? ? no C(30) C(29) H(20) 115.3 ? ? ? no C(29) C(30) C(31) 120.8(6) ? ? ? yes C(29) C(30) H(21) 122.5 ? ? ? no C(31) C(30) H(21) 116.6 ? ? ? no C(30) C(31) C(32) 120.3(5) ? ? ? yes C(30) C(31) H(22) 118.8 ? ? ? no C(32) C(31) H(22) 120.2 ? ? ? no C(31) C(32) C(33) 119.1(6) ? ? ? yes C(31) C(32) H(23) 117.8 ? ? ? no C(33) C(32) H(23) 121.6 ? ? ? no C(28) C(33) C(32) 121.0(6) ? ? ? yes C(28) C(33) H(24) 132.1 ? ? ? no C(32) C(33) H(24) 105.8 ? ? ? no #------------------------------------------------------------------------------ _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 [MnCl(CO)~3~{o-C~6~H~4~(PPh~2~)~2~}] which is included in ms no 9/00875F. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_sjp2 #'[MnCl(CO)~3~(dppe)].1/2CHCl~3~' #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jan 25 12:43:05 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 17.926(10) _cell_length_b 14.174(9) _cell_length_c 23.76(1) _cell_angle_alpha 90 _cell_angle_beta 108.25(4) _cell_angle_gamma 90 _cell_volume 5734(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 20 _cell_measurement_2theta_min 14.0 _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 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.650 _exptl_crystal_size_mid 0.580 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_meas ? _chemical_formula_weight 676.99 _chemical_formula_analytical ? _chemical_formula_sum 'C29.50 H24.50 Br Cl1.50 Mn O3 P2 ' _chemical_formula_moiety '?' _chemical_formula_structural '[MnCl(CO)~3~(dppe)].1/2CHCl~3~' _chemical_compound_source 'diffusion of pet ether into CHCl~3~ soln' _exptl_crystal_F_000 2728.00 _exptl_absorpt_coefficient_mu 2.140 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.814 #------------------------------------------------------------------------------ _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_% -3.30 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 -3 -2 5 -3 1 3 0 6 _diffrn_reflns_number 9864 _reflns_number_total 9505 _reflns_number_observed 5198 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_2theta_min ? _diffrn_reflns_2theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.03754 _diffrn_orient_matrix_UB_12 -0.05072 _diffrn_orient_matrix_UB_13 0.02037 _diffrn_orient_matrix_UB_21 0.01228 _diffrn_orient_matrix_UB_22 0.03559 _diffrn_orient_matrix_UB_23 0.03816 _diffrn_orient_matrix_UB_31 -0.04348 _diffrn_orient_matrix_UB_32 -0.03374 _diffrn_orient_matrix_UB_33 0.00962 #------------------------------------------------------------------------------ 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 0 236 0.003 0.002 'International Tables' H 0 196 0.000 0.000 'International Tables' O 0 24 0.011 0.006 'International Tables' P 0 16 0.102 0.094 'International Tables' Br 0 8 -0.290 2.459 'International Tables' Mn 0 8 0.337 0.728 'International Tables' Cl 0 12 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 Br(1) 0.02761(6) 0.13353(7) 0.30193(5) 0.0397(3) Uij ? ? Br(2) 0.49166(6) 0.76705(7) 0.26558(4) 0.0382(3) Uij ? ? Mn(1) 0.14309(8) 0.09379(10) 0.26743(6) 0.0265(4) Uij ? ? Mn(2) 0.61487(8) 0.81519(10) 0.24481(6) 0.0304(4) Uij ? ? Cl(1) 0.2141(2) 0.3135(2) 1.0100(1) 0.072(1) Uij ? ? Cl(2) 0.0454(2) 0.2954(2) 0.9711(2) 0.075(1) Uij ? ? Cl(3) 0.1382(2) 0.1815(2) 0.9183(1) 0.0471(8) Uij ? ? P(1) 0.1520(2) -0.0508(2) 0.3146(1) 0.0343(8) Uij ? ? P(2) 0.0557(2) 0.0160(2) 0.1884(1) 0.0407(8) Uij ? ? P(3) 0.5367(1) 0.9122(2) 0.1706(1) 0.0290(7) Uij ? ? P(4) 0.6146(1) 0.9433(2) 0.3065(1) 0.0282(7) Uij ? ? O(1) 0.2555(4) 0.1809(5) 0.3733(3) 0.039(2) Uij ? ? O(2) 0.2757(4) 0.0403(5) 0.2271(3) 0.045(2) Uij ? ? O(3) 0.1123(4) 0.2752(5) 0.2019(3) 0.052(2) Uij ? ? O(4) 0.7538(4) 0.8773(5) 0.2139(3) 0.047(2) Uij ? ? O(5) 0.7143(5) 0.7065(5) 0.3476(3) 0.065(3) Uij ? ? O(6) 0.5885(4) 0.6517(5) 0.1633(3) 0.038(2) Uij ? ? C(1) 0.0808(8) -0.1296(8) 0.2652(6) 0.101(5) Uij ? ? C(2) 0.045(1) -0.1032(9) 0.2131(6) 0.147(7) Uij ? ? C(3) 0.2458(6) -0.1118(6) 0.3316(4) 0.035(3) Uij ? ? C(4) 0.3161(6) -0.0623(7) 0.3554(4) 0.039(3) Uij ? ? C(5) 0.3873(6) -0.1102(8) 0.3730(5) 0.047(4) Uij ? ? C(6) 0.3895(8) -0.2042(9) 0.3650(6) 0.068(5) Uij ? ? C(7) 0.3222(9) -0.2537(8) 0.3406(6) 0.067(5) Uij ? ? C(8) 0.2490(7) -0.2089(7) 0.3233(5) 0.047(4) Uij ? ? C(9) 0.1312(6) -0.0600(7) 0.3846(5) 0.042(3) Uij ? ? C(10) 0.1911(6) -0.0537(7) 0.4381(4) 0.042(3) Uij ? ? C(11) 0.1762(7) -0.0619(8) 0.4917(5) 0.054(4) Uij ? ? C(12) 0.1014(9) -0.0765(9) 0.4933(6) 0.076(5) Uij ? ? C(13) 0.0427(8) -0.083(1) 0.4405(7) 0.124(7) Uij ? ? C(14) 0.0561(7) -0.074(1) 0.3874(6) 0.114(6) Uij ? ? C(15) -0.0436(6) 0.0621(8) 0.1559(4) 0.041(3) Uij ? ? C(16) -0.1108(8) 0.0178(10) 0.1618(5) 0.066(4) Uij ? ? C(17) -0.1833(9) 0.053(1) 0.1326(7) 0.096(7) Uij ? ? C(18) -0.1920(8) 0.132(1) 0.0994(7) 0.087(6) Uij ? ? C(19) -0.1267(7) 0.1793(9) 0.0940(5) 0.060(4) Uij ? ? C(20) -0.0523(6) 0.1443(8) 0.1226(4) 0.041(3) Uij ? ? C(21) 0.0852(6) 0.0007(7) 0.1222(4) 0.040(3) Uij ? ? C(22) 0.0615(6) -0.0785(7) 0.0857(5) 0.048(4) Uij ? ? C(23) 0.0809(6) -0.0850(9) 0.0336(5) 0.056(4) Uij ? ? C(24) 0.1232(7) -0.0163(9) 0.0176(5) 0.053(4) Uij ? ? C(25) 0.1469(6) 0.0618(8) 0.0530(4) 0.048(4) Uij ? ? C(26) 0.1275(6) 0.0705(7) 0.1049(4) 0.042(3) Uij ? ? C(27) 0.5260(5) 1.0259(6) 0.2036(4) 0.031(3) Uij ? ? C(28) 0.5295(6) 1.0139(6) 0.2681(4) 0.036(3) Uij ? ? C(29) 0.5732(5) 0.9442(6) 0.1100(4) 0.027(3) Uij ? ? C(30) 0.6165(5) 0.8812(7) 0.0873(4) 0.033(3) Uij ? ? C(31) 0.6446(6) 0.9067(7) 0.0417(4) 0.040(3) Uij ? ? C(32) 0.6303(6) 0.9962(8) 0.0170(4) 0.044(3) Uij ? ? C(33) 0.5876(6) 1.0583(7) 0.0387(4) 0.042(3) Uij ? ? C(34) 0.5581(6) 1.0334(7) 0.0839(4) 0.035(3) Uij ? ? C(35) 0.4368(5) 0.8726(6) 0.1317(4) 0.027(3) Uij ? ? C(36) 0.3718(6) 0.9103(7) 0.1441(4) 0.037(3) Uij ? ? C(37) 0.2955(6) 0.8802(7) 0.1132(4) 0.041(3) Uij ? ? C(38) 0.2865(6) 0.8090(8) 0.0711(4) 0.045(3) Uij ? ? C(39) 0.3514(6) 0.7704(6) 0.0590(4) 0.038(3) Uij ? ? C(40) 0.4259(5) 0.8019(6) 0.0892(4) 0.030(3) Uij ? ? C(41) 0.6989(6) 1.0214(7) 0.3193(4) 0.036(3) Uij ? ? C(42) 0.6918(6) 1.1165(7) 0.3087(4) 0.038(3) Uij ? ? C(43) 0.7579(6) 1.1728(7) 0.3159(5) 0.045(4) Uij ? ? C(44) 0.8308(6) 1.1336(8) 0.3333(5) 0.050(4) Uij ? ? C(45) 0.8393(6) 1.0382(9) 0.3448(5) 0.057(4) Uij ? ? C(46) 0.7739(6) 0.9804(7) 0.3384(5) 0.046(4) Uij ? ? C(47) 0.6059(5) 0.9316(6) 0.3809(4) 0.032(3) Uij ? ? C(48) 0.6048(6) 1.0140(7) 0.4132(4) 0.041(3) Uij ? ? C(49) 0.5960(6) 1.0088(8) 0.4690(4) 0.045(4) Uij ? ? C(50) 0.5892(6) 0.9237(9) 0.4938(5) 0.049(4) Uij ? ? C(51) 0.5911(6) 0.8419(8) 0.4626(5) 0.050(4) Uij ? ? C(52) 0.5994(6) 0.8462(7) 0.4066(4) 0.039(3) Uij ? ? C(53) 0.1301(6) 0.2917(7) 0.9498(4) 0.043(3) Uij ? ? C(54) 0.2112(6) 0.1488(6) 0.3337(4) 0.031(3) Uij ? ? C(55) 0.1241(6) 0.2048(7) 0.2268(4) 0.044(3) Uij ? ? C(56) 0.2231(6) 0.0618(6) 0.2426(4) 0.030(3) Uij ? ? C(57) 0.6995(6) 0.8534(6) 0.2268(4) 0.034(3) Uij ? ? C(58) 0.6749(6) 0.7474(7) 0.3081(5) 0.042(3) Uij ? ? C(59) 0.5998(6) 0.7165(7) 0.1943(4) 0.035(3) Uij ? ? H(1) 0.1049 -0.1895 0.2637 0.0924 Uiso ? ? H(2) 0.0397 -0.1437 0.2849 0.0924 Uiso ? ? H(3) -0.0128 -0.1133 0.2062 0.1262 Uiso ? ? H(4) 0.0574 -0.1475 0.1866 0.1262 Uiso ? ? H(5) 0.3155 0.0060 0.3599 0.0457 Uiso ? ? H(6) 0.4360 -0.0748 0.3911 0.0536 Uiso ? ? H(7) 0.4407 -0.2360 0.3779 0.0731 Uiso ? ? H(8) 0.3267 -0.3214 0.3347 0.0720 Uiso ? ? H(9) 0.2014 -0.2460 0.3056 0.0537 Uiso ? ? H(10) 0.2447 -0.0423 0.4381 0.0504 Uiso ? ? H(11) 0.2211 -0.0573 0.5285 0.0619 Uiso ? ? H(12) 0.0937 -0.0828 0.5326 0.0860 Uiso ? ? H(13) -0.0111 -0.0922 0.4418 0.1243 Uiso ? ? H(14) 0.0122 -0.0813 0.3490 0.1093 Uiso ? ? H(15) -0.1047 -0.0381 0.1879 0.0735 Uiso ? ? H(16) -0.2312 0.0218 0.1352 0.0934 Uiso ? ? H(17) -0.2450 0.1562 0.0790 0.0869 Uiso ? ? H(18) -0.1335 0.2365 0.0689 0.0661 Uiso ? ? H(19) -0.0062 0.1782 0.1202 0.0474 Uiso ? ? H(20) 0.0314 -0.1274 0.0968 0.0525 Uiso ? ? H(21) 0.0638 -0.1400 0.0082 0.0611 Uiso ? ? H(22) 0.1372 -0.0212 -0.0190 0.0612 Uiso ? ? H(23) 0.1773 0.1114 0.0417 0.0554 Uiso ? ? H(24) 0.1446 0.1253 0.1304 0.0493 Uiso ? ? H(25) 0.5672 1.0686 0.2024 0.0365 Uiso ? ? H(26) 0.4768 1.0557 0.1814 0.0365 Uiso ? ? H(27) 0.4812 0.9826 0.2696 0.0451 Uiso ? ? H(28) 0.5305 1.0740 0.2875 0.0451 Uiso ? ? H(29) 0.6278 0.8182 0.1045 0.0414 Uiso ? ? H(30) 0.6743 0.8606 0.0269 0.0470 Uiso ? ? H(31) 0.6505 1.0140 -0.0154 0.0510 Uiso ? ? H(32) 0.5785 1.1216 0.0221 0.0488 Uiso ? ? H(33) 0.5267 1.0781 0.0977 0.0414 Uiso ? ? H(34) 0.3804 0.9596 0.1749 0.0436 Uiso ? ? H(35) 0.2331 0.7871 0.0498 0.0511 Uiso ? ? H(36) 0.3443 0.7209 0.0292 0.0459 Uiso ? ? H(37) 0.4715 0.7742 0.0815 0.0358 Uiso ? ? H(38) 0.6396 1.1448 0.2959 0.0448 Uiso ? ? H(39) 0.7525 1.2412 0.3087 0.0522 Uiso ? ? H(40) 0.8786 1.1716 0.3385 0.0605 Uiso ? ? H(41) 0.8918 1.0088 0.3576 0.0640 Uiso ? ? H(42) 0.7802 0.9127 0.3477 0.0530 Uiso ? ? H(43) 0.6102 1.0759 0.3960 0.0485 Uiso ? ? H(44) 0.5947 1.0666 0.4914 0.0533 Uiso ? ? H(45) 0.5838 0.9206 0.5338 0.0544 Uiso ? ? H(46) 0.5889 0.7809 0.4810 0.0583 Uiso ? ? H(47) 0.5994 0.7876 0.3848 0.0446 Uiso ? ? H(48) 0.1268 0.3408 0.9202 0.0484 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) 0.0310(6) 0.0448(7) 0.0399(6) 0.0030(5) 0.0061(5) -0.0111(5) Br(2) 0.0452(7) 0.0295(6) 0.0406(6) -0.0026(5) 0.0145(5) 0.0004(5) Mn(1) 0.0273(9) 0.0265(8) 0.0223(8) -0.0010(7) 0.0029(7) 0.0005(6) Mn(2) 0.0334(9) 0.0267(8) 0.0290(8) 0.0065(7) 0.0066(7) 0.0003(7) Cl(1) 0.078(2) 0.057(2) 0.057(2) -0.008(2) -0.016(2) -0.006(2) Cl(2) 0.081(2) 0.065(2) 0.099(3) -0.007(2) 0.055(2) -0.016(2) Cl(3) 0.050(2) 0.045(2) 0.044(2) -0.003(1) 0.012(1) -0.002(1) P(1) 0.034(2) 0.031(1) 0.031(1) -0.005(1) 0.000(1) 0.007(1) P(2) 0.056(2) 0.033(2) 0.024(1) -0.014(1) -0.001(1) 0.003(1) P(3) 0.032(2) 0.026(1) 0.027(1) 0.003(1) 0.006(1) -0.001(1) P(4) 0.028(1) 0.028(1) 0.026(1) 0.005(1) 0.005(1) -0.001(1) O(1) 0.036(4) 0.043(4) 0.035(4) -0.005(4) 0.005(3) -0.005(4) O(2) 0.043(5) 0.047(5) 0.050(5) -0.002(4) 0.021(4) -0.001(4) O(3) 0.048(5) 0.035(4) 0.055(5) -0.015(4) -0.007(4) 0.011(4) O(4) 0.039(5) 0.056(5) 0.044(5) 0.006(4) 0.008(4) -0.003(4) O(5) 0.092(7) 0.055(5) 0.042(5) 0.048(5) 0.013(5) 0.008(4) O(6) 0.034(4) 0.035(4) 0.047(5) 0.002(3) 0.015(4) -0.002(4) C(1) 0.11(1) 0.043(8) 0.09(1) -0.038(8) -0.062(9) 0.036(8) C(2) 0.25(2) 0.065(10) 0.048(9) -0.09(1) -0.06(1) 0.031(8) C(3) 0.060(8) 0.026(6) 0.021(5) 0.021(5) 0.015(5) 0.011(4) C(4) 0.039(7) 0.040(6) 0.037(6) 0.003(6) 0.010(5) -0.002(5) C(5) 0.043(7) 0.054(8) 0.049(7) 0.014(6) 0.020(6) 0.012(6) C(6) 0.08(1) 0.054(9) 0.09(1) 0.026(8) 0.062(9) 0.028(8) C(7) 0.10(1) 0.031(7) 0.10(1) 0.032(8) 0.078(10) 0.024(7) C(8) 0.067(8) 0.036(7) 0.051(7) 0.003(6) 0.036(6) -0.001(5) C(9) 0.040(7) 0.034(6) 0.052(7) 0.010(5) 0.014(6) 0.027(5) C(10) 0.045(7) 0.044(7) 0.043(7) -0.006(6) 0.021(6) -0.003(5) C(11) 0.070(9) 0.057(8) 0.047(7) -0.003(7) 0.032(7) 0.000(6) C(12) 0.08(1) 0.08(1) 0.09(1) 0.030(9) 0.064(9) 0.045(9) C(13) 0.054(10) 0.22(2) 0.12(1) 0.06(1) 0.060(10) 0.13(1) C(14) 0.027(7) 0.21(2) 0.11(1) 0.011(9) 0.024(8) 0.12(1) C(15) 0.027(6) 0.075(8) 0.018(5) -0.021(6) 0.001(5) -0.015(6) C(16) 0.053(9) 0.11(1) 0.045(7) -0.045(8) 0.025(7) -0.029(7) C(17) 0.05(1) 0.16(2) 0.09(1) -0.05(1) 0.04(1) -0.08(1) C(18) 0.027(8) 0.14(2) 0.09(1) 0.00(1) 0.008(8) -0.08(1) C(19) 0.044(8) 0.084(9) 0.044(7) -0.008(7) 0.004(6) -0.038(7) C(20) 0.025(6) 0.064(8) 0.028(6) -0.004(6) -0.002(5) -0.011(6) C(21) 0.050(7) 0.032(6) 0.027(6) 0.009(5) -0.003(5) -0.007(5) C(22) 0.027(6) 0.049(7) 0.060(8) 0.000(5) 0.002(6) -0.012(6) C(23) 0.035(7) 0.070(9) 0.062(8) -0.003(7) 0.014(6) -0.032(7) C(24) 0.053(8) 0.066(8) 0.034(7) 0.011(7) 0.007(6) -0.011(6) C(25) 0.062(8) 0.047(7) 0.028(6) 0.006(6) 0.005(6) 0.005(5) C(26) 0.059(8) 0.034(6) 0.025(6) 0.001(6) -0.001(5) 0.003(5) C(27) 0.035(6) 0.026(5) 0.027(5) 0.003(5) 0.003(5) 0.004(4) C(28) 0.045(7) 0.027(5) 0.030(6) 0.004(5) 0.006(5) -0.004(5) C(29) 0.020(5) 0.026(5) 0.028(5) 0.000(4) -0.001(4) 0.000(4) C(30) 0.029(6) 0.034(6) 0.037(6) -0.002(5) 0.010(5) -0.007(5) C(31) 0.038(7) 0.052(7) 0.032(6) -0.009(6) 0.013(5) -0.013(5) C(32) 0.048(7) 0.054(7) 0.031(6) -0.008(6) 0.012(5) -0.002(6) C(33) 0.043(7) 0.045(7) 0.035(6) -0.006(6) 0.007(5) -0.001(5) C(34) 0.039(6) 0.035(6) 0.026(6) 0.000(5) 0.004(5) -0.002(5) C(35) 0.025(6) 0.025(5) 0.025(5) 0.000(5) 0.001(4) 0.004(4) C(36) 0.044(7) 0.032(6) 0.037(6) 0.006(5) 0.013(5) 0.002(5) C(37) 0.036(7) 0.041(7) 0.039(6) -0.008(5) 0.001(5) 0.002(5) C(38) 0.024(6) 0.049(7) 0.046(7) -0.007(6) -0.012(5) 0.012(6) C(39) 0.040(7) 0.027(6) 0.044(6) -0.004(5) 0.007(5) 0.006(5) C(40) 0.023(6) 0.031(6) 0.035(6) -0.005(5) 0.008(5) -0.001(5) C(41) 0.050(7) 0.029(6) 0.034(6) -0.011(5) 0.021(5) -0.004(5) C(42) 0.031(6) 0.050(7) 0.037(6) -0.015(5) 0.020(5) 0.004(5) C(43) 0.043(7) 0.043(7) 0.056(7) 0.025(6) 0.023(6) 0.000(6) C(44) 0.035(7) 0.052(7) 0.064(8) -0.012(6) 0.019(6) -0.019(6) C(45) 0.029(7) 0.075(9) 0.063(8) 0.022(7) 0.008(6) -0.008(7) C(46) 0.036(7) 0.048(7) 0.049(7) 0.006(6) 0.008(6) -0.001(6) C(47) 0.031(6) 0.029(6) 0.031(6) 0.004(5) 0.005(5) 0.001(5) C(48) 0.040(7) 0.043(6) 0.048(7) -0.002(5) 0.026(6) -0.002(5) C(49) 0.047(7) 0.058(8) 0.037(7) -0.007(6) 0.021(6) -0.016(6) C(50) 0.040(7) 0.071(9) 0.039(7) 0.004(6) 0.016(6) 0.005(6) C(51) 0.059(8) 0.050(7) 0.043(7) 0.020(6) 0.021(6) 0.016(6) C(52) 0.046(7) 0.038(6) 0.035(6) 0.011(5) 0.014(5) 0.005(5) C(53) 0.050(7) 0.041(6) 0.038(6) -0.004(6) 0.015(5) -0.004(5) C(54) 0.033(6) 0.023(6) 0.038(6) 0.000(5) 0.010(5) 0.006(5) C(55) 0.048(7) 0.037(7) 0.031(6) -0.007(6) -0.010(5) 0.000(5) C(56) 0.034(6) 0.025(6) 0.030(6) -0.009(5) 0.006(5) -0.006(4) C(57) 0.040(7) 0.027(6) 0.027(6) 0.003(5) -0.001(5) 0.003(5) C(58) 0.051(7) 0.038(7) 0.038(7) 0.020(6) 0.015(6) -0.010(5) C(59) 0.048(7) 0.028(6) 0.030(6) 0.011(5) 0.015(5) 0.005(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 5198 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0550 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0635 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.012 _refine_ls_shift/esd_max 0.0150 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.07 _refine_diff_density_max 0.76 #------------------------------------------------------------------------------ _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(1) 2.517(2) ? ? yes Br(2) Mn(2) 2.504(2) ? ? yes Mn(1) P(1) 2.317(3) ? ? yes Mn(1) P(2) 2.314(3) ? ? yes Mn(1) C(54) 1.84(1) ? ? yes Mn(1) C(55) 1.82(1) ? ? yes Mn(1) C(56) 1.77(1) ? ? yes Mn(2) P(3) 2.327(3) ? ? yes Mn(2) P(4) 2.334(3) ? ? yes Mn(2) C(57) 1.78(1) ? ? yes Mn(2) C(58) 1.83(1) ? ? yes Mn(2) C(59) 1.81(1) ? ? yes Cl(1) C(53) 1.749(10) ? ? yes Cl(2) C(53) 1.74(1) ? ? yes Cl(3) C(53) 1.758(10) ? ? yes P(1) C(1) 1.82(1) ? ? yes P(1) C(3) 1.821(10) ? ? yes P(1) C(9) 1.82(1) ? ? yes P(2) C(2) 1.82(1) ? ? yes P(2) C(15) 1.83(1) ? ? yes P(2) C(21) 1.82(1) ? ? yes P(3) C(27) 1.829(9) ? ? yes P(3) C(29) 1.817(9) ? ? yes P(3) C(35) 1.828(9) ? ? yes P(4) C(28) 1.814(9) ? ? yes P(4) C(41) 1.820(10) ? ? yes P(4) C(47) 1.832(9) ? ? yes O(1) C(54) 1.121(10) ? ? yes O(2) C(56) 1.15(1) ? ? yes O(3) C(55) 1.14(1) ? ? yes O(4) C(57) 1.16(1) ? ? yes O(5) C(58) 1.14(1) ? ? yes O(6) C(59) 1.15(1) ? ? yes C(1) C(2) 1.26(1) ? ? yes C(3) C(4) 1.40(1) ? ? yes C(3) C(8) 1.39(1) ? ? yes C(4) C(5) 1.39(1) ? ? yes C(5) C(6) 1.35(1) ? ? yes C(6) C(7) 1.36(2) ? ? yes C(7) C(8) 1.40(2) ? ? yes C(9) C(10) 1.39(1) ? ? yes C(9) C(14) 1.38(1) ? ? yes C(10) C(11) 1.39(1) ? ? yes C(11) C(12) 1.37(2) ? ? yes C(12) C(13) 1.37(2) ? ? yes C(13) C(14) 1.36(2) ? ? yes C(15) C(16) 1.40(1) ? ? yes C(15) C(20) 1.39(1) ? ? yes C(16) C(17) 1.36(2) ? ? yes C(17) C(18) 1.35(2) ? ? yes C(18) C(19) 1.39(2) ? ? yes C(19) C(20) 1.39(1) ? ? yes C(21) C(22) 1.40(1) ? ? yes C(21) C(26) 1.38(1) ? ? yes C(22) C(23) 1.39(1) ? ? yes C(23) C(24) 1.36(1) ? ? yes C(24) C(25) 1.37(1) ? ? yes C(25) C(26) 1.39(1) ? ? yes C(27) C(28) 1.52(1) ? ? yes C(29) C(30) 1.40(1) ? ? yes C(29) C(34) 1.40(1) ? ? yes C(30) C(31) 1.38(1) ? ? yes C(31) C(32) 1.39(1) ? ? yes C(32) C(33) 1.37(1) ? ? yes C(33) C(34) 1.38(1) ? ? yes C(35) C(36) 1.39(1) ? ? yes C(35) C(40) 1.39(1) ? ? yes C(36) C(37) 1.40(1) ? ? yes C(37) C(38) 1.39(1) ? ? yes C(38) C(39) 1.40(1) ? ? yes C(39) C(40) 1.38(1) ? ? yes C(41) C(42) 1.37(1) ? ? yes C(41) C(46) 1.40(1) ? ? yes C(42) C(43) 1.39(1) ? ? yes C(43) C(44) 1.36(1) ? ? yes C(44) C(45) 1.38(1) ? ? yes C(45) C(46) 1.40(1) ? ? yes C(47) C(48) 1.40(1) ? ? yes C(47) C(52) 1.38(1) ? ? yes C(48) C(49) 1.39(1) ? ? yes C(49) C(50) 1.36(1) ? ? yes C(50) C(51) 1.38(1) ? ? yes C(51) C(52) 1.39(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 Br(1) Mn(1) P(1) 88.82(9) ? ? ? yes Br(1) Mn(1) P(2) 87.36(10) ? ? ? yes Br(1) Mn(1) C(54) 91.1(3) ? ? ? yes Br(1) Mn(1) C(55) 86.7(4) ? ? ? yes Br(1) Mn(1) C(56) 178.0(3) ? ? ? yes P(1) Mn(1) P(2) 84.14(10) ? ? ? yes P(1) Mn(1) C(54) 91.9(3) ? ? ? yes P(1) Mn(1) C(55) 173.4(3) ? ? ? yes P(1) Mn(1) C(56) 89.7(3) ? ? ? yes P(2) Mn(1) C(54) 175.8(3) ? ? ? yes P(2) Mn(1) C(55) 90.8(3) ? ? ? yes P(2) Mn(1) C(56) 91.2(3) ? ? ? yes C(54) Mn(1) C(55) 93.0(4) ? ? ? yes C(54) Mn(1) C(56) 90.2(4) ? ? ? yes C(55) Mn(1) C(56) 94.6(5) ? ? ? yes Br(2) Mn(2) P(3) 87.23(9) ? ? ? yes Br(2) Mn(2) P(4) 85.01(8) ? ? ? yes Br(2) Mn(2) C(57) 176.9(3) ? ? ? yes Br(2) Mn(2) C(58) 91.3(3) ? ? ? yes Br(2) Mn(2) C(59) 87.9(3) ? ? ? yes P(3) Mn(2) P(4) 84.11(9) ? ? ? yes P(3) Mn(2) C(57) 89.7(3) ? ? ? yes P(3) Mn(2) C(58) 174.5(3) ? ? ? yes P(3) Mn(2) C(59) 91.4(3) ? ? ? yes P(4) Mn(2) C(57) 94.8(3) ? ? ? yes P(4) Mn(2) C(58) 90.5(3) ? ? ? yes P(4) Mn(2) C(59) 171.8(3) ? ? ? yes C(57) Mn(2) C(58) 91.8(4) ? ? ? yes C(57) Mn(2) C(59) 92.1(4) ? ? ? yes C(58) Mn(2) C(59) 93.8(4) ? ? ? yes Mn(1) P(1) C(1) 107.6(4) ? ? ? yes Mn(1) P(1) C(3) 116.5(3) ? ? ? yes Mn(1) P(1) C(9) 120.2(3) ? ? ? yes C(1) P(1) C(3) 105.3(6) ? ? ? yes C(1) P(1) C(9) 104.0(6) ? ? ? yes C(3) P(1) C(9) 101.7(4) ? ? ? yes Mn(1) P(2) C(2) 107.1(4) ? ? ? yes Mn(1) P(2) C(15) 119.7(3) ? ? ? yes Mn(1) P(2) C(21) 116.8(3) ? ? ? yes C(2) P(2) C(15) 106.4(7) ? ? ? yes C(2) P(2) C(21) 104.8(7) ? ? ? yes C(15) P(2) C(21) 100.7(4) ? ? ? yes Mn(2) P(3) C(27) 108.4(3) ? ? ? yes Mn(2) P(3) C(29) 117.9(3) ? ? ? yes Mn(2) P(3) C(35) 117.6(3) ? ? ? yes C(27) P(3) C(29) 103.5(4) ? ? ? yes C(27) P(3) C(35) 105.6(4) ? ? ? yes C(29) P(3) C(35) 102.4(4) ? ? ? yes Mn(2) P(4) C(28) 106.2(3) ? ? ? yes Mn(2) P(4) C(41) 114.4(3) ? ? ? yes Mn(2) P(4) C(47) 123.6(3) ? ? ? yes C(28) P(4) C(41) 105.8(5) ? ? ? yes C(28) P(4) C(47) 102.9(4) ? ? ? yes C(41) P(4) C(47) 102.2(4) ? ? ? yes P(1) C(1) C(2) 119.2(10) ? ? ? yes P(2) C(2) C(1) 121.4(10) ? ? ? yes P(1) C(3) C(4) 120.3(7) ? ? ? yes P(1) C(3) C(8) 120.8(9) ? ? ? yes C(4) C(3) C(8) 118.8(10) ? ? ? yes C(3) C(4) C(5) 120.2(9) ? ? ? yes C(4) C(5) C(6) 120(1) ? ? ? yes C(5) C(6) C(7) 120(1) ? ? ? yes C(6) C(7) C(8) 121(1) ? ? ? yes C(3) C(8) C(7) 118(1) ? ? ? yes P(1) C(9) C(10) 120.8(8) ? ? ? yes P(1) C(9) C(14) 122.4(9) ? ? ? yes C(10) C(9) C(14) 116(1) ? ? ? yes C(9) C(10) C(11) 121.4(10) ? ? ? yes C(10) C(11) C(12) 120(1) ? ? ? yes C(11) C(12) C(13) 117(1) ? ? ? yes C(12) C(13) C(14) 122(1) ? ? ? yes C(9) C(14) C(13) 120(1) ? ? ? yes P(2) C(15) C(16) 123.4(10) ? ? ? yes P(2) C(15) C(20) 117.5(7) ? ? ? yes C(16) C(15) C(20) 119(1) ? ? ? yes C(15) C(16) C(17) 119(1) ? ? ? yes C(16) C(17) C(18) 121(1) ? ? ? yes C(17) C(18) C(19) 120(1) ? ? ? yes C(18) C(19) C(20) 119(1) ? ? ? yes C(15) C(20) C(19) 119(1) ? ? ? yes P(2) C(21) C(22) 121.0(9) ? ? ? yes P(2) C(21) C(26) 120.3(7) ? ? ? yes C(22) C(21) C(26) 118.5(9) ? ? ? yes C(21) C(22) C(23) 119(1) ? ? ? yes C(22) C(23) C(24) 121(1) ? ? ? yes C(23) C(24) C(25) 119(1) ? ? ? yes C(24) C(25) C(26) 120(1) ? ? ? yes C(21) C(26) C(25) 120.8(9) ? ? ? yes P(3) C(27) C(28) 110.9(6) ? ? ? yes P(4) C(28) C(27) 109.3(7) ? ? ? yes P(3) C(29) C(30) 121.9(7) ? ? ? yes P(3) C(29) C(34) 120.6(7) ? ? ? yes C(30) C(29) C(34) 117.5(9) ? ? ? yes C(29) C(30) C(31) 121.3(9) ? ? ? yes C(30) C(31) C(32) 120.6(9) ? ? ? yes C(31) C(32) C(33) 118.6(9) ? ? ? yes C(32) C(33) C(34) 121.6(10) ? ? ? yes C(29) C(34) C(33) 120.5(9) ? ? ? yes P(3) C(35) C(36) 121.8(7) ? ? ? yes P(3) C(35) C(40) 118.7(7) ? ? ? yes C(36) C(35) C(40) 119.5(8) ? ? ? yes C(35) C(36) C(37) 121.1(9) ? ? ? yes C(36) C(37) C(38) 118.1(9) ? ? ? yes C(37) C(38) C(39) 121.0(9) ? ? ? yes C(38) C(39) C(40) 120.1(9) ? ? ? yes C(35) C(40) C(39) 120.2(9) ? ? ? yes P(4) C(41) C(42) 122.9(8) ? ? ? yes P(4) C(41) C(46) 117.6(7) ? ? ? yes C(42) C(41) C(46) 119.5(9) ? ? ? yes C(41) C(42) C(43) 120.9(10) ? ? ? yes C(42) C(43) C(44) 120.2(10) ? ? ? yes C(43) C(44) C(45) 119.7(10) ? ? ? yes C(44) C(45) C(46) 121.1(10) ? ? ? yes C(41) C(46) C(45) 118.6(10) ? ? ? yes P(4) C(47) C(48) 118.3(7) ? ? ? yes P(4) C(47) C(52) 123.5(7) ? ? ? yes C(48) C(47) C(52) 118.2(9) ? ? ? yes C(47) C(48) C(49) 120.3(9) ? ? ? yes C(48) C(49) C(50) 120.9(10) ? ? ? yes C(49) C(50) C(51) 119.3(9) ? ? ? yes C(50) C(51) C(52) 120.4(10) ? ? ? yes C(47) C(52) C(51) 120.9(9) ? ? ? yes Cl(1) C(53) Cl(2) 111.3(5) ? ? ? yes Cl(1) C(53) Cl(3) 109.9(6) ? ? ? yes Cl(2) C(53) Cl(3) 110.2(5) ? ? ? yes Mn(1) C(54) O(1) 176.9(9) ? ? ? yes Mn(1) C(55) O(3) 179.1(9) ? ? ? yes Mn(1) C(56) O(2) 179.0(9) ? ? ? yes Mn(2) C(57) O(4) 178.4(9) ? ? ? yes Mn(2) C(58) O(5) 177(1) ? ? ? yes Mn(2) C(59) O(6) 177.2(9) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' J. Chem. Sc., 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 [MnCl(CO)~3~(dppe)].1/2CHCl~3~ which is included in ms no 9/00875F.' ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_sjpmncl #[MnCl(CO)~3~{o-C~6~H~4~(PH~2~)~2~}].CH~2~Cl~2~ #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jan 25 12:28:54 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 10.296(1) _cell_length_b 10.188(1) _cell_length_c 15.5896(7) _cell_angle_alpha 90 _cell_angle_beta 91.936(5) _cell_angle_gamma 90 _cell_volume 1634.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_2theta_min 21.7 _cell_measurement_2theta_max 26.6 #------------------------------------------------------------------------------ _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 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.490 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.230 _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_meas ? _chemical_formula_weight 401.43 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H10 Cl3 Mn O3 P2 ' _chemical_formula_moiety '?' _chemical_formula_structural '[MnCl(CO)~3~{o-C~6~H~4~(PH~2~)~2~}].CH~2~Cl~2~' _chemical_compound_source 'diffusion of pet ether into CH~2~Cl~2~ soln' _exptl_crystal_F_000 800.00 _exptl_absorpt_coefficient_mu 1.490 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 293.2 _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_% -9.73 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -3 -2 1 -3 2 2 -3 1 _diffrn_reflns_number 3255 _reflns_number_total 3076 _reflns_number_observed 1727 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_2theta_min ? _diffrn_reflns_2theta_max 25.03 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.05933 _diffrn_orient_matrix_UB_12 -0.07758 _diffrn_orient_matrix_UB_13 -0.00195 _diffrn_orient_matrix_UB_21 -0.01418 _diffrn_orient_matrix_UB_22 -0.01724 _diffrn_orient_matrix_UB_23 0.06213 _diffrn_orient_matrix_UB_31 -0.07565 _diffrn_orient_matrix_UB_32 -0.05761 _diffrn_orient_matrix_UB_33 -0.01596 #------------------------------------------------------------------------------ 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 40 0.003 0.002 'International Tables' H 0 40 0.000 0.000 'International Tables' O 0 12 0.011 0.006 'International Tables' P 0 8 0.102 0.094 'International Tables' Cl 0 12 0.148 0.159 'International Tables' Mn 0 4 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) 0.25433(7) 0.17142(8) 0.11561(5) 0.0539(2) Uij ? ? Cl(1) 0.4361(1) 0.0413(1) 0.16369(9) 0.0640(4) Uij ? ? Cl(2) 0.8513(2) -0.0147(2) 0.1806(1) 0.1069(7) Uij ? ? Cl(3) 0.8172(2) 0.2419(2) 0.2559(1) 0.1314(9) Uij ? ? P(1) 0.3691(1) 0.1888(1) -0.00645(9) 0.0562(4) Uij ? ? P(2) 0.3857(1) 0.3400(1) 0.16053(9) 0.0570(4) Uij ? ? O(1) 0.0448(4) 0.3437(5) 0.0531(3) 0.102(2) Uij ? ? O(2) 0.1448(4) 0.1479(4) 0.2876(3) 0.088(2) Uij ? ? O(3) 0.1215(4) -0.0685(4) 0.0508(3) 0.091(2) Uij ? ? C(1) 0.1265(5) 0.2763(6) 0.0766(4) 0.065(2) Uij ? ? C(2) 0.1858(5) 0.1578(6) 0.2210(4) 0.066(2) Uij ? ? C(3) 0.1722(5) 0.0234(6) 0.0752(4) 0.063(2) Uij ? ? C(4) 0.5143(5) 0.2871(5) 0.0130(3) 0.052(2) Uij ? ? C(5) 0.6176(5) 0.2923(5) -0.0434(3) 0.060(2) Uij ? ? C(6) 0.7236(5) 0.3692(6) -0.0218(4) 0.064(2) Uij ? ? C(7) 0.7295(5) 0.4436(5) 0.0527(4) 0.063(2) Uij ? ? C(8) 0.6270(5) 0.4396(5) 0.1080(3) 0.058(2) Uij ? ? C(9) 0.5205(5) 0.3601(5) 0.0891(3) 0.053(2) Uij ? ? C(10) 0.7864(7) 0.1432(7) 0.1689(4) 0.095(3) Uij ? ? H(1) 0.4155 0.0926 -0.0419 0.1012 Uiso ? ? H(2) 0.3069 0.2420 -0.0695 0.1012 Uiso ? ? H(3) 0.4401 0.3203 0.2343 0.1012 Uiso ? ? H(4) 0.3319 0.4523 0.1736 0.1012 Uiso ? ? H(5) 0.6252 0.5113 0.1649 0.1012 Uiso ? ? H(6) 0.8176 0.5163 0.0806 0.1012 Uiso ? ? H(7) 0.7982 0.3687 -0.0615 0.1012 Uiso ? ? H(8) 0.5921 0.2443 -0.0996 0.1012 Uiso ? ? H(9) 0.8230 0.1831 0.1168 0.1089 Uiso ? ? H(10) 0.6940 0.1367 0.1556 0.1089 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) 0.0463(4) 0.0576(5) 0.0578(5) 0.0028(4) 0.0026(3) 0.0004(4) Cl(1) 0.0581(8) 0.0672(9) 0.0667(9) 0.0123(7) 0.0023(7) 0.0093(7) Cl(2) 0.099(1) 0.095(1) 0.128(2) 0.006(1) 0.022(1) 0.013(1) Cl(3) 0.175(2) 0.129(2) 0.091(1) 0.040(2) -0.001(1) -0.011(1) P(1) 0.0540(8) 0.0626(9) 0.0519(8) 0.0023(7) 0.0003(6) -0.0037(7) P(2) 0.0575(8) 0.0590(9) 0.0547(9) 0.0003(7) 0.0086(7) -0.0035(7) O(1) 0.063(3) 0.108(4) 0.135(4) 0.029(3) 0.000(3) 0.028(3) O(2) 0.083(3) 0.111(4) 0.073(3) 0.001(3) 0.021(2) 0.010(3) O(3) 0.083(3) 0.080(3) 0.109(4) -0.015(3) -0.002(3) -0.015(3) C(1) 0.052(3) 0.068(4) 0.076(4) 0.000(3) 0.011(3) -0.001(3) C(2) 0.053(3) 0.068(4) 0.077(4) 0.001(3) 0.014(3) 0.009(3) C(3) 0.052(3) 0.067(4) 0.071(4) 0.001(3) 0.002(3) 0.005(3) C(4) 0.051(3) 0.055(3) 0.051(3) 0.004(2) 0.001(2) 0.007(3) C(5) 0.055(3) 0.067(4) 0.058(3) 0.002(3) 0.002(3) 0.006(3) C(6) 0.051(3) 0.072(4) 0.068(4) 0.009(3) 0.015(3) 0.010(3) C(7) 0.054(3) 0.062(4) 0.074(4) -0.002(3) 0.003(3) 0.006(3) C(8) 0.053(3) 0.059(4) 0.063(4) -0.004(3) 0.002(3) 0.000(3) C(9) 0.052(3) 0.055(3) 0.053(3) 0.006(3) 0.007(2) 0.001(3) C(10) 0.101(5) 0.092(5) 0.091(5) 0.005(4) -0.007(4) 0.016(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 1727 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0389 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0405 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.714 _refine_ls_shift/esd_max 0.0020 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.27 _refine_diff_density_max 0.30 #------------------------------------------------------------------------------ _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) Cl(1) 2.393(2) ? ? yes Mn(1) P(1) 2.280(2) ? ? yes Mn(1) P(2) 2.281(2) ? ? yes Mn(1) C(1) 1.786(6) ? ? yes Mn(1) C(2) 1.814(6) ? ? yes Mn(1) C(3) 1.830(6) ? ? yes Cl(2) C(10) 1.749(7) ? ? yes Cl(3) C(10) 1.710(7) ? ? yes P(1) C(4) 1.817(5) ? ? yes P(2) C(9) 1.820(5) ? ? yes O(1) C(1) 1.136(6) ? ? yes O(2) C(2) 1.139(6) ? ? yes O(3) C(3) 1.132(6) ? ? yes C(4) C(5) 1.403(7) ? ? yes C(4) C(9) 1.400(7) ? ? yes C(5) C(6) 1.377(7) ? ? yes C(6) C(7) 1.386(7) ? ? yes C(7) C(8) 1.386(7) ? ? yes C(8) C(9) 1.387(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 Cl(1) Mn(1) P(1) 83.26(5) ? ? ? yes Cl(1) Mn(1) P(2) 82.63(6) ? ? ? yes Cl(1) Mn(1) C(1) 176.0(2) ? ? ? yes Cl(1) Mn(1) C(2) 89.9(2) ? ? ? yes Cl(1) Mn(1) C(3) 89.9(2) ? ? ? yes P(1) Mn(1) P(2) 83.06(6) ? ? ? yes P(1) Mn(1) C(1) 93.8(2) ? ? ? yes P(1) Mn(1) C(2) 171.7(2) ? ? ? yes P(1) Mn(1) C(3) 91.3(2) ? ? ? yes P(2) Mn(1) C(1) 94.4(2) ? ? ? yes P(2) Mn(1) C(2) 91.4(2) ? ? ? yes P(2) Mn(1) C(3) 171.1(2) ? ? ? yes C(1) Mn(1) C(2) 92.9(2) ? ? ? yes C(1) Mn(1) C(3) 92.8(3) ? ? ? yes C(2) Mn(1) C(3) 93.4(3) ? ? ? yes Mn(1) P(1) C(4) 110.5(2) ? ? ? yes Mn(1) P(2) C(9) 110.7(2) ? ? ? yes Mn(1) C(1) O(1) 178.8(6) ? ? ? yes Mn(1) C(2) O(2) 178.7(5) ? ? ? yes Mn(1) C(3) O(3) 179.4(5) ? ? ? yes P(1) C(4) C(5) 123.6(4) ? ? ? yes P(1) C(4) C(9) 116.6(4) ? ? ? yes C(5) C(4) C(9) 119.8(5) ? ? ? yes C(4) C(5) C(6) 118.7(5) ? ? ? yes C(5) C(6) C(7) 121.9(5) ? ? ? yes C(6) C(7) C(8) 119.5(5) ? ? ? yes C(7) C(8) C(9) 120.0(5) ? ? ? yes P(2) C(9) C(4) 116.4(4) ? ? ? yes P(2) C(9) C(8) 123.4(4) ? ? ? yes C(4) C(9) C(8) 120.2(5) ? ? ? yes Cl(2) C(10) Cl(3) 113.5(4) ? ? ? 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 [MnCl(CO)~3~{o-C~6~H~4~(PH~2~)~2~}].CH~2~Cl~2~ which is included in ms no 9/00875F. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_sjpmn #[MnBr(CO)~3~(PPhH~2~)~2~] #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jan 25 12:17:52 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 28.781(5) _cell_length_b 5.962(6) _cell_length_c 24.249(4) _cell_angle_alpha 90 _cell_angle_beta 121.99(1) _cell_angle_gamma 90 _cell_volume 3528(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 25 _cell_measurement_2theta_min 36.7 _cell_measurement_2theta_max 43.2 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, +y,1/2-z' ' -x, -y, -z' ' -x, -y, -z' ' +x, -y,1/2+z' ' +x, -y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'column' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 439.06 _chemical_formula_analytical ? _chemical_formula_sum 'C15 H14 Br Mn O3 P2 ' _chemical_formula_moiety 'C15 H14 Br Mn O3 P2 ' _chemical_formula_structural 'MnBr(CO)~3~(PPhH~2~)~2~]' _chemical_compound_source 'diffusion of pet ether into CHCl~3~ soln' _exptl_crystal_F_000 1744.00 _exptl_absorpt_coefficient_mu 3.147 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.786 #------------------------------------------------------------------------------ _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_% -2.07 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 0 -8 4 -2 -4 3 1 -7 _diffrn_reflns_number 3903 _reflns_number_total 3415 _reflns_number_observed 2366 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_2theta_min ? _diffrn_reflns_2theta_max 24.98 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.02764 _diffrn_orient_matrix_UB_12 -0.06483 _diffrn_orient_matrix_UB_13 -0.04331 _diffrn_orient_matrix_UB_21 -0.02526 _diffrn_orient_matrix_UB_22 0.12803 _diffrn_orient_matrix_UB_23 -0.00796 _diffrn_orient_matrix_UB_31 0.01662 _diffrn_orient_matrix_UB_32 0.08681 _diffrn_orient_matrix_UB_33 -0.02061 #------------------------------------------------------------------------------ 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 0 120 0.003 0.002 'International Tables' H 0 112 0.000 0.000 'International Tables' O 0 24 0.011 0.006 'International Tables' P 0 16 0.102 0.094 'International Tables' Br 0 8 -0.290 2.459 'International Tables' Mn 0 8 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 Br(1) 0.22488(2) 0.05371(7) 0.17754(2) 0.0344(1) Uij ? ? Mn(1) 0.19013(2) 0.31474(10) 0.08139(3) 0.0297(2) Uij ? ? P(1) 0.15162(4) 0.5153(2) 0.12863(5) 0.0330(3) Uij ? ? P(2) 0.27192(4) 0.5050(2) 0.14705(5) 0.0339(3) Uij ? ? O(1) 0.1510(1) 0.6459(5) -0.0235(1) 0.0446(9) Uij ? ? O(2) 0.2449(1) 0.0296(5) 0.0317(1) 0.0444(9) Uij ? ? O(3) 0.0877(1) 0.0495(5) 0.0081(1) 0.0484(9) Uij ? ? C(1) 0.1668(2) 0.5157(7) 0.0175(2) 0.034(1) Uij ? ? C(2) 0.2239(2) 0.1420(7) 0.0508(2) 0.036(1) Uij ? ? C(3) 0.1276(2) 0.1515(7) 0.0368(2) 0.035(1) Uij ? ? C(4) 0.0901(2) 0.4129(7) 0.1249(2) 0.034(1) Uij ? ? C(5) 0.0421(2) 0.5357(8) 0.0908(2) 0.047(1) Uij ? ? C(6) -0.0050(2) 0.4603(10) 0.0876(2) 0.059(2) Uij ? ? C(7) -0.0044(2) 0.2648(9) 0.1173(2) 0.054(2) Uij ? ? C(8) 0.0423(2) 0.1433(8) 0.1503(2) 0.055(2) Uij ? ? C(9) 0.0908(2) 0.2148(7) 0.1546(2) 0.045(1) Uij ? ? C(10) 0.3350(1) 0.3724(6) 0.1635(2) 0.031(1) Uij ? ? C(11) 0.3581(2) 0.4378(7) 0.1287(2) 0.043(1) Uij ? ? C(12) 0.4044(2) 0.3260(9) 0.1375(2) 0.053(1) Uij ? ? C(13) 0.4275(2) 0.1554(8) 0.1817(2) 0.051(1) Uij ? ? C(14) 0.4048(2) 0.0903(9) 0.2164(3) 0.066(2) Uij ? ? C(15) 0.3585(2) 0.1985(8) 0.2077(2) 0.053(1) Uij ? ? H(1) 0.1862 0.5828 0.1925 0.0572 Uiso ? ? H(2) 0.1361 0.7086 0.1091 0.0572 Uiso ? ? H(3) 0.2801 0.5498 0.2010 0.0572 Uiso ? ? H(4) 0.2788 0.7065 0.1349 0.0572 Uiso ? ? H(5) 0.0393 0.6786 0.0607 0.0572 Uiso ? ? H(6) -0.0435 0.5768 0.0595 0.0572 Uiso ? ? H(7) -0.0419 0.2225 0.1147 0.0572 Uiso ? ? H(8) 0.0547 0.0443 0.1796 0.0572 Uiso ? ? H(9) 0.1260 0.1162 0.1775 0.0572 Uiso ? ? H(10) 0.3441 0.5851 0.1010 0.0572 Uiso ? ? H(11) 0.4132 0.3978 0.0993 0.0572 Uiso ? ? H(12) 0.4592 0.0375 0.1774 0.0572 Uiso ? ? H(13) 0.4210 -0.0439 0.2497 0.0572 Uiso ? ? H(14) 0.3320 0.1549 0.2305 0.0572 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) 0.0345(2) 0.0332(2) 0.0345(2) 0.0035(2) 0.0178(2) 0.0053(2) Mn(1) 0.0272(3) 0.0319(3) 0.0298(3) 0.0025(3) 0.0151(3) 0.0028(3) P(1) 0.0303(5) 0.0326(6) 0.0371(6) 0.0010(5) 0.0186(5) 0.0000(5) P(2) 0.0298(5) 0.0338(6) 0.0373(6) 0.0020(5) 0.0172(5) 0.0028(5) O(1) 0.041(2) 0.048(2) 0.045(2) 0.005(1) 0.022(1) 0.013(2) O(2) 0.044(2) 0.047(2) 0.050(2) 0.004(1) 0.029(2) -0.003(2) O(3) 0.041(2) 0.053(2) 0.049(2) -0.010(2) 0.022(2) -0.009(2) C(1) 0.030(2) 0.040(2) 0.036(2) 0.001(2) 0.020(2) 0.000(2) C(2) 0.037(2) 0.036(2) 0.038(2) 0.000(2) 0.021(2) 0.004(2) C(3) 0.041(2) 0.037(2) 0.034(2) 0.006(2) 0.024(2) 0.004(2) C(4) 0.032(2) 0.036(2) 0.033(2) 0.003(2) 0.018(2) -0.005(2) C(5) 0.037(2) 0.058(3) 0.044(3) 0.009(2) 0.021(2) 0.006(2) C(6) 0.030(2) 0.083(4) 0.060(3) 0.007(3) 0.021(2) -0.001(3) C(7) 0.037(2) 0.068(3) 0.063(3) -0.014(3) 0.030(2) -0.024(3) C(8) 0.062(3) 0.046(3) 0.073(3) -0.006(3) 0.047(3) -0.004(3) C(9) 0.042(3) 0.039(3) 0.066(3) 0.005(2) 0.036(2) 0.001(2) C(10) 0.024(2) 0.034(2) 0.030(2) -0.004(2) 0.011(2) -0.001(2) C(11) 0.042(2) 0.049(3) 0.039(2) -0.001(2) 0.022(2) 0.005(2) C(12) 0.044(3) 0.073(3) 0.052(3) -0.003(3) 0.033(2) -0.001(3) C(13) 0.035(2) 0.070(3) 0.052(3) 0.012(2) 0.025(2) 0.006(3) C(14) 0.049(3) 0.077(4) 0.074(4) 0.028(3) 0.035(3) 0.038(3) C(15) 0.035(2) 0.072(3) 0.059(3) 0.017(2) 0.029(2) 0.030(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 2366 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0289 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0320 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.803 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.39 _refine_diff_density_max 0.56 #------------------------------------------------------------------------------ _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(1) 2.5273(7) ? ? yes Mn(1) P(1) 2.305(1) ? ? yes Mn(1) P(2) 2.322(1) ? ? yes Mn(1) C(1) 1.784(4) ? ? yes Mn(1) C(2) 1.823(4) ? ? yes Mn(1) C(3) 1.814(4) ? ? yes P(1) C(4) 1.830(4) ? ? yes P(2) C(10) 1.821(4) ? ? yes O(1) C(1) 1.149(4) ? ? yes O(2) C(2) 1.149(4) ? ? yes O(3) C(3) 1.151(4) ? ? yes C(4) C(5) 1.385(5) ? ? yes C(4) C(9) 1.379(6) ? ? yes C(5) C(6) 1.389(6) ? ? yes C(6) C(7) 1.366(7) ? ? yes C(7) C(8) 1.355(6) ? ? yes C(8) C(9) 1.409(6) ? ? yes C(10) C(11) 1.379(5) ? ? yes C(10) C(15) 1.382(6) ? ? yes C(11) C(12) 1.402(6) ? ? yes C(12) C(13) 1.367(6) ? ? yes C(13) C(14) 1.368(6) ? ? yes C(14) C(15) 1.391(6) ? ? 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 Br(1) Mn(1) P(1) 85.44(3) ? ? ? yes Br(1) Mn(1) P(2) 84.63(3) ? ? ? yes Br(1) Mn(1) C(1) 175.8(1) ? ? ? yes Br(1) Mn(1) C(2) 89.5(1) ? ? ? yes Br(1) Mn(1) C(3) 90.2(1) ? ? ? yes P(1) Mn(1) P(2) 89.17(4) ? ? ? yes P(1) Mn(1) C(1) 91.4(1) ? ? ? yes P(1) Mn(1) C(2) 174.9(1) ? ? ? yes P(1) Mn(1) C(3) 89.4(1) ? ? ? yes P(2) Mn(1) C(1) 92.6(1) ? ? ? yes P(2) Mn(1) C(2) 89.4(1) ? ? ? yes P(2) Mn(1) C(3) 174.7(1) ? ? ? yes C(1) Mn(1) C(2) 93.6(2) ? ? ? yes C(1) Mn(1) C(3) 92.5(2) ? ? ? yes C(2) Mn(1) C(3) 91.6(2) ? ? ? yes Mn(1) P(1) C(4) 120.7(1) ? ? ? yes Mn(1) P(2) C(10) 118.0(1) ? ? ? yes Mn(1) C(1) O(1) 178.8(3) ? ? ? yes Mn(1) C(2) O(2) 178.7(4) ? ? ? yes Mn(1) C(3) O(3) 179.4(4) ? ? ? yes P(1) C(4) C(5) 119.2(3) ? ? ? yes P(1) C(4) C(9) 120.9(3) ? ? ? yes C(5) C(4) C(9) 119.9(4) ? ? ? yes C(4) C(5) C(6) 119.8(4) ? ? ? yes C(5) C(6) C(7) 120.5(4) ? ? ? yes C(6) C(7) C(8) 119.8(4) ? ? ? yes C(7) C(8) C(9) 121.2(4) ? ? ? yes C(4) C(9) C(8) 118.7(4) ? ? ? yes P(2) C(10) C(11) 119.4(3) ? ? ? yes P(2) C(10) C(15) 121.2(3) ? ? ? yes C(11) C(10) C(15) 119.3(4) ? ? ? yes C(10) C(11) C(12) 120.0(4) ? ? ? yes C(11) C(12) C(13) 120.0(4) ? ? ? yes C(12) C(13) C(14) 120.1(4) ? ? ? yes C(13) C(14) C(15) 120.3(4) ? ? ? yes C(10) C(15) C(14) 120.1(4) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' J. Che. 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 [MnBr(CO)~3~(PPhH~2~)~2~] which is included in ms no 9/00875F. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk '