# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1341 data_mkdmn2 #'[MnCl(CO)~3~([8]aneSe~2~)]' #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jan 5 14:57:50 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 12.274(1) _cell_length_b 12.684(1) _cell_length_c 8.611(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1340.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 423.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 36.3 _cell_measurement_theta_max 42.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'rod' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.284 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 460.95 _chemical_formula_analytical ? _chemical_formula_sum 'C9 H12 Br Mn O3 Se2 ' _chemical_formula_moiety 'C9 H12 Br Mn O3 Se2 ' _chemical_formula_structural '[MnCl(CO)~3~([8]aneSe~2~)]' _chemical_compound_source 'CHCl~3~/hexane solution at -18oC' _exptl_crystal_F_000 872.00 _exptl_absorpt_coefficient_mu 9.266 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.887 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 423.2 _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_% -0.83 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -3 -1 3 -3 0 3 -3 1 _diffrn_reflns_number 1392 _reflns_number_total 1392 _reflns_number_observed 1231 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 24.98 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.02949 _diffrn_orient_matrix_UB_12 -0.04434 _diffrn_orient_matrix_UB_13 0.08633 _diffrn_orient_matrix_UB_21 -0.01618 _diffrn_orient_matrix_UB_22 -0.06510 _diffrn_orient_matrix_UB_23 -0.06131 _diffrn_orient_matrix_UB_31 0.07420 _diffrn_orient_matrix_UB_32 0.00342 _diffrn_orient_matrix_UB_33 -0.04768 #------------------------------------------------------------------------------ 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 36 0.003 0.002 'International Tables' H 0 48 0.000 0.000 'International Tables' O 0 12 0.011 0.006 'International Tables' Mn 0 4 0.337 0.728 'International Tables' Se 0 8 -0.093 2.226 'International Tables' Br 0 4 -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) -0.17160(5) -0.29095(5) 0.08046(7) 0.0240(2) Uij ? ? Se(1) 0.08192(5) -0.17668(4) 0.16163(7) 0.0190(1) Uij ? ? Se(2) -0.10965(5) -0.01720(4) 0.00128(7) 0.0194(1) Uij ? ? Mn(1) -0.03187(6) -0.18974(7) -0.07665(10) 0.0154(2) Uij ? ? O(1) -0.1790(3) -0.2124(3) -0.3474(5) 0.029(1) Uij ? ? O(2) 0.0654(3) -0.3956(3) -0.1543(5) 0.030(1) Uij ? ? O(3) 0.1170(3) -0.0983(3) -0.3080(4) 0.029(1) Uij ? ? C(1) 0.1598(5) -0.0399(4) 0.1662(7) 0.026(1) Uij ? ? C(2) 0.1286(5) 0.0404(4) 0.0435(7) 0.030(2) Uij ? ? C(3) 0.0111(5) 0.0818(4) 0.0417(6) 0.024(1) Uij ? ? C(4) -0.1620(5) -0.0294(4) 0.2150(6) 0.025(1) Uij ? ? C(5) -0.0782(5) -0.0466(4) 0.3449(7) 0.025(2) Uij ? ? C(6) -0.0158(5) -0.1493(4) 0.3400(6) 0.022(1) Uij ? ? C(7) -0.1238(4) -0.2030(4) -0.2391(6) 0.019(1) Uij ? ? C(8) 0.0281(4) -0.3167(4) -0.1226(6) 0.019(1) Uij ? ? C(9) 0.0622(4) -0.1305(4) -0.2091(7) 0.021(2) Uij ? ? H(1) 0.2366 -0.0533 0.1567 0.0321 Uiso ? ? H(2) 0.1468 -0.0064 0.2631 0.0321 Uiso ? ? H(3) 0.1405 0.0041 -0.0570 0.0350 Uiso ? ? H(4) 0.1796 0.0963 0.0473 0.0350 Uiso ? ? H(5) 0.0000 0.1136 0.1432 0.0260 Uiso ? ? H(6) 0.0078 0.1382 -0.0329 0.0260 Uiso ? ? H(7) -0.2119 -0.0852 0.2239 0.0276 Uiso ? ? H(8) -0.2003 0.0359 0.2421 0.0276 Uiso ? ? H(9) -0.1162 -0.0397 0.4421 0.0274 Uiso ? ? H(10) -0.0279 0.0119 0.3381 0.0274 Uiso ? ? H(11) 0.0266 -0.1515 0.4322 0.0210 Uiso ? ? H(12) -0.0691 -0.2036 0.3430 0.0210 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) 0.0262(3) 0.0245(3) 0.0214(3) -0.0087(3) 0.0021(3) 0.0008(3) Se(1) 0.0211(3) 0.0199(3) 0.0161(3) 0.0024(3) -0.0035(3) -0.0019(3) Se(2) 0.0217(3) 0.0180(3) 0.0184(3) 0.0027(2) -0.0020(3) -0.0004(3) Mn(1) 0.0168(4) 0.0160(4) 0.0134(4) -0.0010(4) -0.0002(4) -0.0009(4) O(1) 0.030(2) 0.037(2) 0.020(2) -0.001(2) -0.006(2) -0.002(2) O(2) 0.046(3) 0.021(2) 0.024(2) 0.010(2) -0.003(2) -0.005(2) O(3) 0.029(2) 0.038(2) 0.018(2) -0.007(2) 0.004(2) 0.000(2) C(1) 0.021(3) 0.026(2) 0.032(3) -0.007(2) -0.005(3) -0.013(3) C(2) 0.034(3) 0.024(3) 0.031(4) -0.019(3) 0.003(3) -0.004(3) C(3) 0.038(3) 0.016(3) 0.017(3) -0.012(2) -0.003(3) 0.003(2) C(4) 0.030(3) 0.024(3) 0.022(2) 0.006(3) 0.008(2) 0.000(3) C(5) 0.035(3) 0.024(3) 0.017(3) -0.004(2) 0.007(3) 0.000(3) C(6) 0.032(3) 0.026(3) 0.009(2) -0.001(2) 0.000(2) 0.001(3) C(7) 0.017(3) 0.019(3) 0.020(3) 0.000(3) -0.001(2) 0.002(3) C(8) 0.021(3) 0.024(2) 0.013(3) 0.004(2) 0.002(2) -0.004(3) C(9) 0.016(3) 0.023(3) 0.023(3) -0.005(2) -0.001(2) -0.001(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 'correct configuration' _refine_ls_abs_structure_Flack '-0.0460(69)' _refine_ls_number_reflns 1231 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0210 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0223 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.461 _refine_ls_shift/esd_max 0.0470 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.38 _refine_diff_density_max 0.40 #------------------------------------------------------------------------------ _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) 2.534(1) ? ? yes Se(1) Mn(1) 2.488(1) ? ? yes Se(1) C(1) 1.982(6) ? ? yes Se(1) C(6) 1.980(7) ? ? yes Se(2) Mn(1) 2.480(1) ? ? yes Se(2) C(3) 1.974(7) ? ? yes Se(2) C(4) 1.956(7) ? ? yes Mn(1) C(7) 1.805(7) ? ? yes Mn(1) C(8) 1.814(7) ? ? yes Mn(1) C(9) 1.788(7) ? ? yes O(1) C(7) 1.158(8) ? ? yes O(2) C(8) 1.134(8) ? ? yes O(3) C(9) 1.160(8) ? ? yes C(1) C(2) 1.517(10) ? ? yes C(2) C(3) 1.535(10) ? ? yes C(4) C(5) 1.535(10) ? ? yes C(5) C(6) 1.512(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 Mn(1) Se(1) C(1) 110.2(2) ? ? ? yes Mn(1) Se(1) C(6) 108.1(2) ? ? ? yes C(1) Se(1) C(6) 97.1(3) ? ? ? yes Mn(1) Se(2) C(3) 108.7(2) ? ? ? yes Mn(1) Se(2) C(4) 108.1(2) ? ? ? yes C(3) Se(2) C(4) 97.5(3) ? ? ? yes Br(1) Mn(1) Se(1) 88.47(4) ? ? ? yes Br(1) Mn(1) Se(2) 92.41(4) ? ? ? yes Br(1) Mn(1) C(7) 86.8(2) ? ? ? yes Br(1) Mn(1) C(8) 86.6(2) ? ? ? yes Br(1) Mn(1) C(9) 172.1(2) ? ? ? yes Se(1) Mn(1) Se(2) 86.23(4) ? ? ? yes Se(1) Mn(1) C(7) 175.1(2) ? ? ? yes Se(1) Mn(1) C(8) 90.6(2) ? ? ? yes Se(1) Mn(1) C(9) 97.8(2) ? ? ? yes Se(2) Mn(1) C(7) 92.9(2) ? ? ? yes Se(2) Mn(1) C(8) 176.7(2) ? ? ? yes Se(2) Mn(1) C(9) 92.9(2) ? ? ? yes C(7) Mn(1) C(8) 90.1(3) ? ? ? yes C(7) Mn(1) C(9) 87.0(3) ? ? ? yes C(8) Mn(1) C(9) 88.4(3) ? ? ? yes Se(1) C(1) C(2) 116.9(5) ? ? ? yes C(1) C(2) C(3) 118.3(6) ? ? ? yes Se(2) C(3) C(2) 119.3(4) ? ? ? yes Se(2) C(4) C(5) 118.5(5) ? ? ? yes C(4) C(5) C(6) 116.2(6) ? ? ? yes Se(1) C(6) C(5) 118.7(5) ? ? ? yes Mn(1) C(7) O(1) 177.1(6) ? ? ? yes Mn(1) C(8) O(2) 178.7(6) ? ? ? yes Mn(1) C(9) O(3) 172.2(6) ? ? ? yes #------------------------------------------------------------------------------ _publ_contact_author ; Dr Gillian Reid Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; Debbie Middleton Editorial Secretary Dalton Transactions Dear Debbie, As promised this is the CIF file for the crystal structure of [MnCl(CO)~3~([8]aneSe~2~)] which is included in manuscript number 8/09853K which we recently submitted for consideration for publication in Dalton Transactions. I hope that this is satisfactory. Yours sincerely, Gill Reid ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_mkdre1 #'[ReBr(CO)~3~([8]aneSe~2~)]' #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jan 5 15:36:41 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 12.302(2) _cell_length_b 12.726(1) _cell_length_c 8.656(2) _cell_angle_alpha 90 _cell_angle_beta 90.02(1) _cell_angle_gamma 90 _cell_volume 1355.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 423.2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 14.1 _cell_measurement_theta_max 17.5 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.130 _exptl_crystal_density_diffrn 2.903 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 592.22 _chemical_formula_analytical ? _chemical_formula_sum 'C9 H12 Br O3 Re Se2 ' _chemical_formula_moiety 'C9 H12 Br O3 Re Se2 ' _chemical_formula_structural '[ReBr(CO)~3~([8]aneSe~2~)]' _chemical_compound_source 'cooling a CHCl~3~/hexane mixture' _exptl_crystal_F_000 1072.00 _exptl_absorpt_coefficient_mu 17.321 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.641 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 423.2 _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_% 0.67 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 5 -1 -1 5 -1 1 5 1 _diffrn_reflns_number 1409 _reflns_number_total 1409 _reflns_number_observed 1215 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.06505 _diffrn_orient_matrix_UB_12 0.04654 _diffrn_orient_matrix_UB_13 0.01092 _diffrn_orient_matrix_UB_21 0.02387 _diffrn_orient_matrix_UB_22 0.01958 _diffrn_orient_matrix_UB_23 0.10663 _diffrn_orient_matrix_UB_31 0.04251 _diffrn_orient_matrix_UB_32 0.06022 _diffrn_orient_matrix_UB_33 -0.04311 #------------------------------------------------------------------------------ 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 Re 0 4 -1.018 7.231 'International Tables' O 0 12 0.011 0.006 'International Tables' Se 0 8 -0.093 2.226 'International Tables' Br 0 4 -0.290 2.459 'International Tables' C 0 36 0.003 0.002 'International Tables' H 0 48 0.000 0.000 '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) -0.03684(4) -0.19189(4) -0.08483(7) 0.0092(1) Uij ? ? Br(1) -0.1790(1) -0.2911(1) 0.0897(2) 0.0189(4) Uij ? ? Se(1) -0.1138(1) -0.0114(1) 0.0065(2) 0.0140(4) Uij ? ? Se(2) 0.0837(1) -0.1765(1) 0.1625(2) 0.0135(4) Uij ? ? O(1) 0.1187(9) -0.0946(10) -0.318(1) 0.029(3) Uij ? ? O(2) 0.0674(9) -0.4042(8) -0.168(1) 0.024(3) Uij ? ? O(3) -0.1885(9) -0.2138(9) -0.366(1) 0.026(3) Uij ? ? C(1) 0.062(1) -0.129(1) -0.221(2) 0.012(3) Uij ? ? C(2) 0.026(1) -0.326(1) -0.135(2) 0.015(3) Uij ? ? C(3) -0.134(1) -0.205(1) -0.257(2) 0.017(3) Uij ? ? C(4) -0.163(1) -0.027(1) 0.222(2) 0.024(4) Uij ? ? C(5) -0.078(1) -0.044(1) 0.343(2) 0.014(3) Uij ? ? C(6) -0.015(1) -0.148(1) 0.341(2) 0.015(3) Uij ? ? C(7) 0.161(1) -0.039(1) 0.164(2) 0.017(3) Uij ? ? C(8) 0.128(1) 0.038(1) 0.038(2) 0.018(4) Uij ? ? C(9) 0.011(1) 0.083(1) 0.044(2) 0.021(4) Uij ? ? H(1) -0.2029 0.0341 0.2500 0.0291 Uiso ? ? H(2) -0.2108 -0.0866 0.2270 0.0291 Uiso ? ? H(3) -0.0235 0.0109 0.3289 0.0177 Uiso ? ? H(4) -0.1084 -0.0365 0.4415 0.0177 Uiso ? ? H(5) -0.0673 -0.2025 0.3430 0.0182 Uiso ? ? H(6) 0.0285 -0.1511 0.4318 0.0182 Uiso ? ? H(7) 0.1454 -0.0056 0.2632 0.0222 Uiso ? ? H(8) 0.2367 -0.0518 0.1600 0.0222 Uiso ? ? H(9) 0.1799 0.0947 0.0413 0.0207 Uiso ? ? H(10) 0.1371 0.0015 -0.0571 0.0207 Uiso ? ? H(11) 0.0066 0.1399 -0.0267 0.0214 Uiso ? ? H(12) 0.0012 0.1126 0.1478 0.0214 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) 0.0113(3) 0.0061(3) 0.0102(3) -0.0007(2) -0.0008(3) -0.0008(3) Br(1) 0.0204(8) 0.0173(8) 0.0190(7) -0.0096(6) 0.0014(7) 0.0006(8) Se(1) 0.0160(8) 0.0091(7) 0.0169(7) 0.0030(6) -0.0012(7) -0.0004(7) Se(2) 0.0161(7) 0.0101(8) 0.0142(7) 0.0023(6) -0.0042(6) -0.0017(7) O(1) 0.022(6) 0.038(7) 0.026(6) -0.007(6) -0.005(6) -0.004(6) O(2) 0.042(7) 0.008(5) 0.021(6) 0.007(5) -0.004(6) -0.003(5) O(3) 0.015(5) 0.035(7) 0.028(6) -0.007(5) -0.007(5) -0.007(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 'correct configuration' _refine_ls_abs_structure_Flack 0.0212(98) _refine_ls_number_reflns 1215 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0325 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0425 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.300 _refine_ls_shift/esd_max 0.0023 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.42 _refine_diff_density_max 1.10 #------------------------------------------------------------------------------ _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) Br(1) 2.633(2) ? ? yes Re(1) Se(1) 2.607(2) ? ? yes Re(1) Se(2) 2.611(2) ? ? yes Re(1) C(1) 1.88(2) ? ? yes Re(1) C(2) 1.92(2) ? ? yes Re(1) C(3) 1.92(2) ? ? yes Se(1) C(4) 1.97(2) ? ? yes Se(1) C(9) 1.98(2) ? ? yes Se(2) C(6) 2.00(2) ? ? yes Se(2) C(7) 1.99(2) ? ? yes O(1) C(1) 1.18(2) ? ? yes O(2) C(2) 1.16(2) ? ? yes O(3) C(3) 1.15(2) ? ? yes C(4) C(5) 1.50(3) ? ? yes C(5) C(6) 1.53(2) ? ? yes C(7) C(8) 1.53(2) ? ? yes C(8) C(9) 1.55(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 Br(1) Re(1) Se(1) 90.41(6) ? ? ? yes Br(1) Re(1) Se(2) 86.72(6) ? ? ? yes Br(1) Re(1) C(1) 175.7(5) ? ? ? yes Br(1) Re(1) C(2) 88.4(5) ? ? ? yes Br(1) Re(1) C(3) 89.4(5) ? ? ? yes Se(1) Re(1) Se(2) 83.77(6) ? ? ? yes Se(1) Re(1) C(1) 92.9(5) ? ? ? yes Se(1) Re(1) C(2) 175.1(5) ? ? ? yes Se(1) Re(1) C(3) 94.9(5) ? ? ? yes Se(2) Re(1) C(1) 96.5(5) ? ? ? yes Se(2) Re(1) C(2) 91.4(5) ? ? ? yes Se(2) Re(1) C(3) 175.9(5) ? ? ? yes C(1) Re(1) C(2) 88.6(7) ? ? ? yes C(1) Re(1) C(3) 87.5(7) ? ? ? yes C(2) Re(1) C(3) 89.9(7) ? ? ? yes Re(1) Se(1) C(4) 108.1(6) ? ? ? yes Re(1) Se(1) C(9) 107.7(5) ? ? ? yes C(4) Se(1) C(9) 98.1(7) ? ? ? yes Re(1) Se(2) C(6) 107.8(5) ? ? ? yes Re(1) Se(2) C(7) 110.2(5) ? ? ? yes C(6) Se(2) C(7) 97.1(7) ? ? ? yes Re(1) C(1) O(1) 172(1) ? ? ? yes Re(1) C(2) O(2) 176(1) ? ? ? yes Re(1) C(3) O(3) 176(1) ? ? ? yes Se(1) C(4) C(5) 117(1) ? ? ? yes C(4) C(5) C(6) 118(1) ? ? ? yes Se(2) C(6) C(5) 118(1) ? ? ? yes Se(2) C(7) C(8) 115(1) ? ? ? yes C(7) C(8) C(9) 117(1) ? ? ? yes Se(1) C(9) C(8) 119(1) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_contact_author ; Dr Gillian Reid Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; Debbie Middleton Editorial Secretary Dalton Transactions Dear Debbie, Here is the CIF file for the crystal structure of [ReBr(CO)3([8]aneSe2)] which is included in the manuscript which we submitted for consideration for publication in Dalton Transactions (ms 8/09853K). I hope that this is satisfactory. Yours sincerely, Gill Reid ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_mkdw #'[W(CO)~4~([8]aneSe~2~)]' #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jan 5 17:04:31 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 12.861(2) _cell_length_b 9.978(1) _cell_length_c 10.715(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1375.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 20.5 _cell_measurement_theta_max 26.8 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y,1/2-z' ' -x,1/2+y, -z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y,1/2+z' ' +x,1/2-y, +z' '1/2+x, +y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'rod' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.070 _exptl_crystal_density_diffrn 2.599 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 537.97 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H12 O4 Se2 W ' _chemical_formula_moiety 'C10 H12 O4 Se2 W ' _chemical_formula_structural '[W(CO)~4~([8]aneSe~2~)]' _chemical_compound_source 'cooling a CHCl~3~/hexane mixture' _exptl_crystal_F_000 984.00 _exptl_absorpt_coefficient_mu 13.705 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.328 #------------------------------------------------------------------------------ _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_% -1.58 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -1 -4 0 2 -4 1 -3 -3 _diffrn_reflns_number 1421 _reflns_number_total 1421 _reflns_number_observed 956 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 24.99 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.06459 _diffrn_orient_matrix_UB_12 0.04341 _diffrn_orient_matrix_UB_13 0.03263 _diffrn_orient_matrix_UB_21 0.01936 _diffrn_orient_matrix_UB_22 -0.08527 _diffrn_orient_matrix_UB_23 0.04317 _diffrn_orient_matrix_UB_31 0.03871 _diffrn_orient_matrix_UB_32 -0.02980 _diffrn_orient_matrix_UB_33 -0.07604 #------------------------------------------------------------------------------ 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 W 0 4 -0.849 6.872 'International Tables' Se 0 8 -0.093 2.226 'International Tables' O 0 16 0.011 0.006 'International Tables' C 0 40 0.003 0.002 'International Tables' H 0 48 0.000 0.000 '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 W(1) 0.11916(6) 0.2500 0.08676(7) 0.0290(2) Uij ? ? Se(1) 0.2311(1) 0.4253(1) -0.0415(1) 0.0431(4) Uij ? ? O(1) -0.084(1) 0.2500 -0.086(1) 0.071(6) Uij ? ? O(2) 0.0008(9) 0.0280(10) 0.237(1) 0.066(4) Uij ? ? O(3) 0.279(1) 0.2500 0.314(1) 0.067(5) Uij ? ? C(1) -0.007(1) 0.2500 -0.034(2) 0.042(6) Uij ? ? C(2) 0.045(1) 0.112(1) 0.181(1) 0.045(4) Uij ? ? C(3) 0.228(1) 0.2500 0.229(2) 0.040(6) Uij ? ? C(4) 0.378(1) 0.381(2) -0.004(1) 0.064(5) Uij ? ? C(5) 0.421(2) 0.2500 -0.055(2) 0.078(9) Uij ? ? C(6) 0.186(2) 0.2500 -0.260(2) 0.056(7) Uij ? ? C(7) 0.232(1) 0.381(1) -0.224(1) 0.048(4) Uij ? ? H(1) 0.4218 0.4520 -0.0360 0.0728 Uiso ? ? H(2) 0.3875 0.3775 0.0842 0.0728 Uiso ? ? H(3) 0.4105 0.2500 -0.1439 0.0801 Uiso ? ? H(4) 0.4965 0.2500 -0.0424 0.0801 Uiso ? ? H(5) 0.1174 0.2500 -0.2243 0.0568 Uiso ? ? H(6) 0.1778 0.2500 -0.3496 0.0568 Uiso ? ? H(7) 0.1969 0.4503 -0.2705 0.0550 Uiso ? ? H(8) 0.3036 0.3798 -0.2544 0.0550 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 W(1) 0.0235(4) 0.0346(4) 0.0289(4) 0.0000 0.0029(3) 0.0000 Se(1) 0.0501(9) 0.0378(8) 0.0416(8) -0.0096(7) 0.0108(6) -0.0009(6) O(1) 0.038(10) 0.11(1) 0.06(1) 0.0000 -0.025(8) 0.0000 O(2) 0.070(8) 0.059(7) 0.069(7) -0.015(6) 0.021(6) 0.017(6) O(3) 0.07(1) 0.07(1) 0.056(10) 0.0000 -0.044(9) 0.0000 C(1) 0.03(1) 0.06(1) 0.04(1) 0.0000 0.017(9) 0.0000 C(2) 0.049(9) 0.056(9) 0.029(7) -0.003(8) 0.009(6) 0.012(7) C(3) 0.03(1) 0.05(1) 0.04(1) 0.0000 0.014(10) 0.0000 C(4) 0.037(9) 0.11(1) 0.043(9) -0.037(10) -0.006(7) -0.010(9) C(5) 0.01(1) 0.18(3) 0.04(1) 0.0000 0.004(9) 0.0000 C(6) 0.03(1) 0.11(2) 0.03(1) 0.0000 -0.005(9) 0.0000 C(7) 0.041(9) 0.059(10) 0.044(8) -0.002(7) 0.004(7) 0.012(7) #------------------------------------------------------------------------------ _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 956 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0352 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0398 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.976 _refine_ls_shift/esd_max 0.0012 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.83 _refine_diff_density_max 1.04 #------------------------------------------------------------------------------ _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 W(1) Se(1) 2.650(1) ? ? yes W(1) C(1) 2.08(2) ? ? yes W(1) C(2) 1.96(1) ? ? yes W(1) C(2) 1.96(1) ? ? yes W(1) C(3) 2.07(2) ? ? yes Se(1) C(4) 1.98(2) ? ? yes Se(1) C(7) 2.01(1) ? ? yes O(1) C(1) 1.13(2) ? ? yes O(2) C(2) 1.17(1) ? ? yes O(3) C(3) 1.12(2) ? ? yes C(4) C(5) 1.53(2) ? ? yes C(6) C(7) 1.49(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 Se(1) W(1) Se(1) 82.62(6) ? ? ? yes Se(1) W(1) C(1) 95.9(4) ? ? ? yes Se(1) W(1) C(2) 176.0(4) ? ? ? yes Se(1) W(1) C(2) 93.9(4) ? ? ? yes Se(1) W(1) C(3) 90.8(4) ? ? ? yes Se(1) W(1) C(1) 95.9(4) ? ? ? yes Se(1) W(1) C(2) 93.9(4) ? ? ? yes Se(1) W(1) C(2) 176.0(4) ? ? ? yes Se(1) W(1) C(3) 90.8(4) ? ? ? yes C(1) W(1) C(2) 86.4(5) ? ? ? yes C(1) W(1) C(3) 171.0(7) ? ? ? yes C(2) W(1) C(2) 89.5(8) ? ? ? yes C(2) W(1) C(3) 87.2(5) ? ? ? yes W(1) Se(1) C(4) 105.3(4) ? ? ? yes W(1) Se(1) C(7) 111.4(4) ? ? ? yes C(4) Se(1) C(7) 98.4(6) ? ? ? yes W(1) C(1) O(1) 171(1) ? ? ? yes W(1) C(2) O(2) 179(1) ? ? ? yes W(1) C(3) O(3) 173(1) ? ? ? yes Se(1) C(4) C(5) 118(1) ? ? ? yes C(4) C(5) C(4) 117(1) ? ? ? yes C(7) C(6) C(7) 123(1) ? ? ? yes Se(1) C(7) C(6) 116(1) ? ? ? yes #------------------------------------------------------------------------------ _publ_contact_author ; Dr Gillian Reid Departmnet of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; Debbie Middleton Editorial Secretary Dalton Transactions Dear Debbie, Here is the CIF file for the crystal structure of [W(CO)~4~([8]aneSe~2~)] which is included in manuscript 8/09853K which we recently submitted for consideration for publication in Dalton Transactions. I hope that this is satisfactory. Your sincerely, Gill Reid ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk '