# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1889 data_bpmns4_[Mn(CO)3([12]S4)]CF3SO3 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Jun 9 14:29:40 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.4610(9) _cell_length_b 11.593(2) _cell_length_c 9.372(1) _cell_angle_alpha 93.56(1) _cell_angle_beta 96.581(10) _cell_angle_gamma 72.653(9) _cell_volume 974.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150.1 _cell_measurement_reflns_used 25 _cell_measurement_2theta_min 49.2 _cell_measurement_2theta_max 49.8 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.420 _exptl_crystal_size_min 0.360 _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 528.49 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H16 F3 Mn O6 S5 ' _chemical_formula_moiety '[Mn(CO)3([12]aneS4)]CF3SO3?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 536.00 _exptl_absorpt_coefficient_mu 1.268 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.884 #------------------------------------------------------------------------------ _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 2 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.48 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 4 -1 0 4 -4 _diffrn_reflns_number 3655 _reflns_number_total 3427 _reflns_number_observed 3119 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.01078 _diffrn_orient_matrix_UB_12 0.02722 _diffrn_orient_matrix_UB_13 0.10297 _diffrn_orient_matrix_UB_21 0.11063 _diffrn_orient_matrix_UB_22 -0.03341 _diffrn_orient_matrix_UB_23 0.00243 _diffrn_orient_matrix_UB_31 0.00565 _diffrn_orient_matrix_UB_32 0.07948 _diffrn_orient_matrix_UB_33 -0.03064 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 24 0.003 0.002 'International Tables' H 0 32 0.000 0.000 'International Tables' F 0 6 0.017 0.010 'International Tables' O 0 12 0.011 0.006 'International Tables' S 0 10 0.125 0.123 'International Tables' Mn 0 2 0.337 0.728 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Mn(1) 0.14262(4) 0.05577(3) 0.28997(4) 0.0168(1) Uij ? ? S(1) 0.36761(7) 0.10748(6) 0.35850(7) 0.0198(2) Uij ? ? S(2) 0.03043(7) 0.20740(6) 0.45394(7) 0.0216(2) Uij ? ? S(3) 0.01377(7) 0.19212(6) 0.10712(7) 0.0198(2) Uij ? ? S(4) 0.35103(8) 0.13935(6) -0.00664(7) 0.0251(2) Uij ? ? S(5) 0.23391(8) -0.41630(6) 0.23664(7) 0.0241(2) Uij ? ? F(1) 0.4745(2) -0.3576(2) 0.1993(3) 0.0689(8) Uij ? ? F(2) 0.4491(3) -0.3789(2) 0.4189(3) 0.0695(7) Uij ? ? F(3) 0.5183(2) -0.5349(2) 0.2785(2) 0.0490(6) Uij ? ? O(1) 0.2679(2) -0.1267(2) 0.5129(2) 0.0293(5) Uij ? ? O(2) -0.1184(2) -0.0381(2) 0.2435(2) 0.0289(5) Uij ? ? O(3) 0.2818(2) -0.1262(2) 0.0708(2) 0.0299(6) Uij ? ? O(4) 0.1556(2) -0.2892(2) 0.2421(2) 0.0371(6) Uij ? ? O(5) 0.2387(2) -0.4730(2) 0.0957(2) 0.0360(6) Uij ? ? O(6) 0.2038(2) -0.4864(2) 0.3450(2) 0.0384(6) Uij ? ? C(1) 0.3268(3) 0.1795(3) 0.5334(3) 0.0262(7) Uij ? ? C(2) 0.1765(3) 0.2747(3) 0.5261(3) 0.0272(8) Uij ? ? C(3) -0.0956(3) 0.3292(3) 0.3459(3) 0.0307(8) Uij ? ? C(4) -0.1436(3) 0.2808(3) 0.2001(3) 0.0277(7) Uij ? ? C(5) 0.0874(3) 0.3134(2) 0.0689(3) 0.0228(7) Uij ? ? C(6) 0.1973(3) 0.2738(2) -0.0437(3) 0.0262(7) Uij ? ? C(7) 0.4693(3) 0.1926(2) 0.1307(3) 0.0255(7) Uij ? ? C(8) 0.4114(3) 0.2294(2) 0.2770(3) 0.0221(7) Uij ? ? C(9) 0.2190(3) -0.0551(2) 0.4275(3) 0.0213(7) Uij ? ? C(10) -0.0182(3) -0.0006(2) 0.2617(3) 0.0211(7) Uij ? ? C(11) 0.2306(3) -0.0555(2) 0.1543(3) 0.0219(7) Uij ? ? C(12) 0.4286(4) -0.4216(3) 0.2852(4) 0.0383(9) Uij ? ? H(1) 0.3274 0.1196 0.5982 0.0315 Uiso ? ? H(2) 0.4016 0.2168 0.5675 0.0315 Uiso ? ? H(3) 0.1769 0.3373 0.4656 0.0327 Uiso ? ? H(4) 0.1576 0.3074 0.6199 0.0327 Uiso ? ? H(5) -0.1811 0.3662 0.3948 0.0369 Uiso ? ? H(6) -0.0462 0.3874 0.3327 0.0369 Uiso ? ? H(7) -0.1992 0.3472 0.1427 0.0332 Uiso ? ? H(8) -0.2046 0.2312 0.2132 0.0332 Uiso ? ? H(9) 0.0074 0.3803 0.0344 0.0273 Uiso ? ? H(10) 0.1366 0.3370 0.1548 0.0273 Uiso ? ? H(11) 0.2376 0.3383 -0.0541 0.0314 Uiso ? ? H(12) 0.1436 0.2596 -0.1317 0.0314 Uiso ? ? H(13) 0.5603 0.1298 0.1453 0.0306 Uiso ? ? H(14) 0.4876 0.2612 0.0947 0.0306 Uiso ? ? H(15) 0.3238 0.2960 0.2655 0.0265 Uiso ? ? H(16) 0.4853 0.2529 0.3391 0.0265 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) 0.0161(2) 0.0173(2) 0.0177(2) -0.0057(2) 0.0030(2) -0.0003(2) S(1) 0.0177(3) 0.0195(3) 0.0228(3) -0.0068(3) 0.0001(3) 0.0012(3) S(2) 0.0229(3) 0.0224(3) 0.0199(3) -0.0059(3) 0.0068(3) -0.0008(3) S(3) 0.0182(3) 0.0220(3) 0.0191(3) -0.0059(3) 0.0014(2) 0.0013(3) S(4) 0.0280(4) 0.0251(4) 0.0252(4) -0.0107(3) 0.0101(3) -0.0058(3) S(5) 0.0270(4) 0.0187(3) 0.0259(4) -0.0057(3) 0.0023(3) 0.0005(3) F(1) 0.043(1) 0.061(1) 0.113(2) -0.025(1) 0.003(1) 0.036(1) F(2) 0.072(2) 0.053(1) 0.072(2) -0.018(1) -0.033(1) -0.014(1) F(3) 0.0302(10) 0.031(1) 0.079(1) -0.0028(8) -0.0065(9) 0.0054(10) O(1) 0.029(1) 0.027(1) 0.030(1) -0.0070(9) -0.0016(9) 0.0090(9) O(2) 0.025(1) 0.034(1) 0.033(1) -0.0165(9) 0.0027(8) -0.0026(9) O(3) 0.035(1) 0.024(1) 0.034(1) -0.0110(9) 0.0175(9) -0.0089(9) O(4) 0.038(1) 0.021(1) 0.047(1) 0.0000(9) 0.006(1) 0.0025(9) O(5) 0.038(1) 0.038(1) 0.029(1) -0.0093(10) -0.0016(9) -0.0072(9) O(6) 0.051(1) 0.026(1) 0.041(1) -0.0111(10) 0.015(1) 0.0054(9) C(1) 0.033(2) 0.033(2) 0.017(1) -0.018(1) -0.001(1) 0.000(1) C(2) 0.037(2) 0.029(2) 0.021(1) -0.017(1) 0.008(1) -0.007(1) C(3) 0.027(2) 0.030(2) 0.028(2) 0.005(1) 0.007(1) 0.000(1) C(4) 0.017(1) 0.033(2) 0.028(2) 0.000(1) 0.003(1) 0.005(1) C(5) 0.024(1) 0.016(1) 0.028(1) -0.006(1) -0.002(1) 0.004(1) C(6) 0.031(2) 0.028(1) 0.023(1) -0.013(1) 0.002(1) 0.006(1) C(7) 0.021(1) 0.029(1) 0.030(2) -0.012(1) 0.007(1) -0.002(1) C(8) 0.021(1) 0.019(1) 0.028(1) -0.008(1) 0.002(1) 0.001(1) C(9) 0.018(1) 0.023(1) 0.025(1) -0.009(1) 0.003(1) -0.003(1) C(10) 0.023(1) 0.022(1) 0.017(1) -0.004(1) 0.005(1) 0.000(1) C(11) 0.019(1) 0.022(1) 0.028(1) -0.010(1) 0.003(1) 0.003(1) C(12) 0.034(2) 0.026(2) 0.053(2) -0.011(1) -0.006(2) 0.002(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3119 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0280 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0395 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.543 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.36 _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) S(1) 2.3881(7) ? ? yes Mn(1) S(2) 2.3461(7) ? ? yes Mn(1) S(3) 2.3728(7) ? ? yes Mn(1) C(9) 1.809(3) ? ? yes Mn(1) C(10) 1.815(3) ? ? yes Mn(1) C(11) 1.837(3) ? ? yes S(1) C(1) 1.821(3) ? ? yes S(1) C(8) 1.819(3) ? ? yes S(2) C(2) 1.827(3) ? ? yes S(2) C(3) 1.827(3) ? ? yes S(3) C(4) 1.819(3) ? ? yes S(3) C(5) 1.816(3) ? ? yes S(4) C(6) 1.807(3) ? ? yes S(4) C(7) 1.809(3) ? ? yes S(5) O(4) 1.439(2) ? ? yes S(5) O(5) 1.438(2) ? ? yes S(5) O(6) 1.442(2) ? ? yes S(5) C(12) 1.829(3) ? ? yes F(1) C(12) 1.317(4) ? ? yes F(2) C(12) 1.333(4) ? ? yes F(3) C(12) 1.337(3) ? ? yes O(1) C(9) 1.146(3) ? ? yes O(2) C(10) 1.147(3) ? ? yes O(3) C(11) 1.135(3) ? ? yes C(1) C(2) 1.515(4) ? ? yes C(1) H(1) 0.950 ? ? no C(1) H(2) 0.950 ? ? no C(2) H(3) 0.950 ? ? no C(2) H(4) 0.950 ? ? no C(3) C(4) 1.517(4) ? ? yes C(3) H(5) 0.950 ? ? no C(3) H(6) 0.950 ? ? no C(4) H(7) 0.950 ? ? no C(4) H(8) 0.950 ? ? no C(5) C(6) 1.520(4) ? ? yes C(5) H(9) 0.950 ? ? no C(5) H(10) 0.950 ? ? no C(6) H(11) 0.950 ? ? no C(6) H(12) 0.950 ? ? no C(7) C(8) 1.524(4) ? ? yes C(7) H(13) 0.950 ? ? no C(7) H(14) 0.950 ? ? no C(8) H(15) 0.950 ? ? no C(8) H(16) 0.950 ? ? no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Mn(1) S(2) 87.10(3) ? ? ? yes S(1) Mn(1) S(3) 104.87(3) ? ? ? yes S(1) Mn(1) C(9) 82.76(8) ? ? ? yes S(1) Mn(1) C(10) 170.65(8) ? ? ? yes S(1) Mn(1) C(11) 91.84(8) ? ? ? yes S(2) Mn(1) S(3) 86.47(2) ? ? ? yes S(2) Mn(1) C(9) 93.35(8) ? ? ? yes S(2) Mn(1) C(10) 92.76(8) ? ? ? yes S(2) Mn(1) C(11) 176.44(8) ? ? ? yes S(3) Mn(1) C(9) 172.34(8) ? ? ? yes S(3) Mn(1) C(10) 84.45(8) ? ? ? yes S(3) Mn(1) C(11) 90.53(8) ? ? ? yes C(9) Mn(1) C(10) 87.9(1) ? ? ? yes C(9) Mn(1) C(11) 89.9(1) ? ? ? yes C(10) Mn(1) C(11) 88.8(1) ? ? ? yes Mn(1) S(1) C(1) 99.63(9) ? ? ? yes Mn(1) S(1) C(8) 122.57(9) ? ? ? yes C(1) S(1) C(8) 98.8(1) ? ? ? yes Mn(1) S(2) C(2) 105.04(9) ? ? ? yes Mn(1) S(2) C(3) 106.01(9) ? ? ? yes C(2) S(2) C(3) 101.8(1) ? ? ? yes Mn(1) S(3) C(4) 99.68(9) ? ? ? yes Mn(1) S(3) C(5) 118.82(9) ? ? ? yes C(4) S(3) C(5) 98.7(1) ? ? ? yes C(6) S(4) C(7) 102.6(1) ? ? ? yes O(4) S(5) O(5) 115.6(1) ? ? ? yes O(4) S(5) O(6) 115.1(1) ? ? ? yes O(4) S(5) C(12) 103.7(1) ? ? ? yes O(5) S(5) O(6) 114.2(1) ? ? ? yes O(5) S(5) C(12) 102.0(1) ? ? ? yes O(6) S(5) C(12) 103.7(1) ? ? ? yes S(1) C(1) C(2) 112.0(2) ? ? ? yes S(1) C(1) H(1) 108.9 ? ? ? no S(1) C(1) H(2) 108.9 ? ? ? no C(2) C(1) H(1) 108.8 ? ? ? no C(2) C(1) H(2) 108.8 ? ? ? no H(1) C(1) H(2) 109.5 ? ? ? no S(2) C(2) C(1) 110.1(2) ? ? ? yes S(2) C(2) H(3) 109.3 ? ? ? no S(2) C(2) H(4) 109.3 ? ? ? no C(1) C(2) H(3) 109.3 ? ? ? no C(1) C(2) H(4) 109.3 ? ? ? no H(3) C(2) H(4) 109.5 ? ? ? no S(2) C(3) C(4) 110.9(2) ? ? ? yes S(2) C(3) H(5) 109.1 ? ? ? no S(2) C(3) H(6) 109.1 ? ? ? no C(4) C(3) H(5) 109.1 ? ? ? no C(4) C(3) H(6) 109.1 ? ? ? no H(5) C(3) H(6) 109.5 ? ? ? no S(3) C(4) C(3) 112.4(2) ? ? ? yes S(3) C(4) H(7) 108.7 ? ? ? no S(3) C(4) H(8) 108.7 ? ? ? no C(3) C(4) H(7) 108.7 ? ? ? no C(3) C(4) H(8) 108.7 ? ? ? no H(7) C(4) H(8) 109.5 ? ? ? no S(3) C(5) C(6) 111.4(2) ? ? ? yes S(3) C(5) H(9) 109.0 ? ? ? no S(3) C(5) H(10) 109.0 ? ? ? no C(6) C(5) H(9) 109.0 ? ? ? no C(6) C(5) H(10) 109.0 ? ? ? no H(9) C(5) H(10) 109.5 ? ? ? no S(4) C(6) C(5) 116.4(2) ? ? ? yes S(4) C(6) H(11) 107.7 ? ? ? no S(4) C(6) H(12) 107.7 ? ? ? no C(5) C(6) H(11) 107.7 ? ? ? no C(5) C(6) H(12) 107.7 ? ? ? no H(11) C(6) H(12) 109.5 ? ? ? no S(4) C(7) C(8) 117.6(2) ? ? ? yes S(4) C(7) H(13) 107.4 ? ? ? no S(4) C(7) H(14) 107.4 ? ? ? no C(8) C(7) H(13) 107.4 ? ? ? no C(8) C(7) H(14) 107.4 ? ? ? no H(13) C(7) H(14) 109.5 ? ? ? no S(1) C(8) C(7) 112.5(2) ? ? ? yes S(1) C(8) H(15) 108.7 ? ? ? no S(1) C(8) H(16) 108.7 ? ? ? no C(7) C(8) H(15) 108.7 ? ? ? no C(7) C(8) H(16) 108.7 ? ? ? no H(15) C(8) H(16) 109.5 ? ? ? no Mn(1) C(9) O(1) 178.9(2) ? ? ? yes Mn(1) C(10) O(2) 178.9(2) ? ? ? yes Mn(1) C(11) O(3) 177.8(2) ? ? ? yes S(5) C(12) F(1) 112.2(2) ? ? ? yes S(5) C(12) F(2) 111.2(2) ? ? ? yes S(5) C(12) F(3) 111.2(2) ? ? ? yes F(1) C(12) F(2) 107.5(3) ? ? ? yes F(1) C(12) F(3) 107.2(3) ? ? ? yes F(2) C(12) F(3) 107.3(3) ? ? ? 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 ; CIF file for fac-[Mn(CO)3([12]aneS4)]CF3SO3. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_bpmns5_[Mn(CO)3([15]S5)]CF3SO3 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Jun 9 14:54:59 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 11.420(4) _cell_length_b 14.642(3) _cell_length_c 13.605(3) _cell_angle_alpha 90 _cell_angle_beta 96.55(2) _cell_angle_gamma 90 _cell_volume 2260.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 25 _cell_measurement_2theta_min 25.9 _cell_measurement_2theta_max 35.8 #------------------------------------------------------------------------------ _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 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.350 _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 588.60 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H20 F3 Mn O6 S6 ' _chemical_formula_moiety '[Mn(CO)3([15]aneS5)]CF3SO3' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1200.00 _exptl_absorpt_coefficient_mu 1.191 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.874 #------------------------------------------------------------------------------ _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_% 1.28 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 2 -4 2 -2 -4 -1 4 -3 _diffrn_reflns_number 4387 _reflns_number_total 4168 _reflns_number_observed 2847 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.01630 _diffrn_orient_matrix_UB_12 0.03908 _diffrn_orient_matrix_UB_13 -0.05716 _diffrn_orient_matrix_UB_21 0.03436 _diffrn_orient_matrix_UB_22 -0.05389 _diffrn_orient_matrix_UB_23 -0.03160 _diffrn_orient_matrix_UB_31 -0.07951 _diffrn_orient_matrix_UB_32 -0.01527 _diffrn_orient_matrix_UB_33 -0.03476 #------------------------------------------------------------------------------ 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 56 0.003 0.002 'International Tables' H 0 80 0.000 0.000 'International Tables' O 0 24 0.011 0.006 'International Tables' S 0 24 0.125 0.123 'International Tables' F 0 12 0.017 0.010 '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) 0.1300(1) 0.15861(10) 0.4140(1) 0.0246(4) Uij ? ? S(1) 0.0097(2) 0.2429(2) 0.2976(2) 0.0251(7) Uij ? ? S(2) -0.0424(2) 0.1259(2) 0.4834(2) 0.0289(7) Uij ? ? S(3) 0.1552(2) 0.2846(2) 0.5235(2) 0.0275(7) Uij ? ? S(4) 0.1393(3) 0.5309(2) 0.3359(2) 0.0327(7) Uij ? ? S(5) 0.1324(3) 0.3678(2) 0.1251(2) 0.0444(9) Uij ? ? S(6) 0.2006(2) 0.0540(2) -0.1604(2) 0.0281(7) Uij ? ? F(1) 0.1191(7) 0.0899(6) 0.0071(5) 0.075(3) Uij ? ? F(2) 0.1201(7) 0.2034(5) -0.0903(7) 0.078(3) Uij ? ? F(3) -0.0104(6) 0.0998(7) -0.1173(6) 0.081(3) Uij ? ? O(1) 0.1044(7) -0.0104(5) 0.2953(6) 0.043(2) Uij ? ? O(2) 0.2797(7) 0.0474(5) 0.5591(5) 0.038(2) Uij ? ? O(3) 0.3453(6) 0.2118(5) 0.3250(6) 0.040(2) Uij ? ? O(4) 0.3153(6) 0.0795(5) -0.1109(6) 0.040(2) Uij ? ? O(5) 0.1717(8) 0.0913(6) -0.2574(5) 0.051(3) Uij ? ? O(6) 0.1729(7) -0.0408(5) -0.1495(6) 0.044(2) Uij ? ? C(1) -0.1441(10) 0.2129(7) 0.3111(8) 0.035(3) Uij ? ? C(2) -0.1540(10) 0.1317(8) 0.3764(8) 0.035(3) Uij ? ? C(3) -0.069(1) 0.2300(7) 0.5528(8) 0.036(3) Uij ? ? C(4) 0.0422(9) 0.2628(7) 0.6056(7) 0.030(3) Uij ? ? C(5) 0.1032(9) 0.3933(6) 0.4686(7) 0.029(3) Uij ? ? C(6) 0.1869(10) 0.4257(7) 0.3974(8) 0.033(3) Uij ? ? C(7) 0.0230(10) 0.4977(7) 0.2395(8) 0.035(3) Uij ? ? C(8) 0.062(1) 0.4776(8) 0.1401(8) 0.038(3) Uij ? ? C(9) 0.005(1) 0.2917(8) 0.1042(8) 0.039(3) Uij ? ? C(10) 0.0245(9) 0.2077(7) 0.1718(7) 0.030(3) Uij ? ? C(11) 0.1119(9) 0.0553(7) 0.3388(8) 0.033(3) Uij ? ? C(12) 0.2195(9) 0.0919(7) 0.5060(7) 0.027(3) Uij ? ? C(13) 0.2607(9) 0.1902(7) 0.3584(8) 0.029(3) Uij ? ? C(14) 0.101(1) 0.1131(8) -0.0876(8) 0.038(3) Uij ? ? H(1) -0.1839 0.1998 0.2475 0.0418 Uiso ? ? H(2) -0.1806 0.2637 0.3387 0.0418 Uiso ? ? H(3) -0.1477 0.0782 0.3379 0.0423 Uiso ? ? H(4) -0.2293 0.1333 0.3997 0.0423 Uiso ? ? H(5) -0.1015 0.2757 0.5082 0.0434 Uiso ? ? H(6) -0.1232 0.2169 0.5992 0.0434 Uiso ? ? H(7) 0.0710 0.2180 0.6528 0.0366 Uiso ? ? H(8) 0.0273 0.3180 0.6388 0.0366 Uiso ? ? H(9) 0.0999 0.4374 0.5194 0.0346 Uiso ? ? H(10) 0.0268 0.3854 0.4340 0.0346 Uiso ? ? H(11) 0.2623 0.4352 0.4331 0.0398 Uiso ? ? H(12) 0.1922 0.3799 0.3487 0.0398 Uiso ? ? H(13) -0.0138 0.4444 0.2612 0.0422 Uiso ? ? H(14) -0.0328 0.5460 0.2315 0.0422 Uiso ? ? H(15) 0.1164 0.5239 0.1267 0.0457 Uiso ? ? H(16) -0.0056 0.4808 0.0926 0.0457 Uiso ? ? H(17) -0.0634 0.3233 0.1184 0.0465 Uiso ? ? H(18) -0.0040 0.2726 0.0370 0.0465 Uiso ? ? H(19) -0.0328 0.1624 0.1514 0.0364 Uiso ? ? H(20) 0.1012 0.1835 0.1683 0.0364 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) 0.0308(9) 0.0190(8) 0.0254(8) 0.0011(7) 0.0089(7) -0.0026(6) S(1) 0.032(1) 0.022(1) 0.022(1) -0.001(1) 0.008(1) -0.002(1) S(2) 0.037(2) 0.021(1) 0.031(1) 0.001(1) 0.012(1) 0.001(1) S(3) 0.038(2) 0.020(1) 0.024(1) 0.004(1) 0.005(1) -0.002(1) S(4) 0.048(2) 0.021(1) 0.029(1) -0.002(1) 0.005(1) 0.002(1) S(5) 0.045(2) 0.045(2) 0.047(2) -0.006(1) 0.021(1) -0.005(1) S(6) 0.036(1) 0.024(1) 0.025(1) 0.002(1) 0.006(1) 0.000(1) F(1) 0.094(6) 0.104(7) 0.028(4) 0.034(5) 0.019(4) -0.005(4) F(2) 0.085(6) 0.040(5) 0.118(8) 0.010(4) 0.053(6) -0.017(5) F(3) 0.032(4) 0.132(8) 0.080(6) -0.002(5) 0.012(4) -0.028(6) O(1) 0.049(5) 0.031(4) 0.051(5) -0.002(4) 0.011(4) -0.013(4) O(2) 0.048(5) 0.033(4) 0.034(4) 0.005(4) 0.005(4) 0.003(4) O(3) 0.025(4) 0.037(5) 0.059(5) -0.006(4) 0.011(4) -0.009(4) O(4) 0.033(4) 0.037(4) 0.051(5) 0.004(4) 0.006(4) 0.004(4) O(5) 0.077(6) 0.054(5) 0.023(4) 0.020(5) 0.010(4) 0.009(4) O(6) 0.055(5) 0.030(4) 0.046(5) -0.001(4) 0.003(4) 0.002(4) C(1) 0.036(6) 0.028(6) 0.044(7) 0.010(5) 0.018(5) 0.005(5) C(2) 0.033(6) 0.039(6) 0.034(6) -0.007(5) 0.005(5) -0.007(5) C(3) 0.048(7) 0.029(6) 0.035(6) 0.008(5) 0.021(5) -0.005(5) C(4) 0.039(6) 0.034(6) 0.018(5) 0.002(5) 0.001(4) -0.006(4) C(5) 0.044(7) 0.017(5) 0.025(5) 0.005(5) 0.004(5) -0.003(4) C(6) 0.044(7) 0.022(5) 0.034(6) -0.002(5) 0.007(5) 0.001(5) C(7) 0.043(7) 0.033(6) 0.028(6) -0.005(5) 0.000(5) 0.002(5) C(8) 0.045(7) 0.038(6) 0.031(6) -0.009(6) 0.006(5) 0.002(5) C(9) 0.051(7) 0.041(7) 0.025(6) -0.004(6) 0.006(5) -0.007(5) C(10) 0.041(6) 0.032(6) 0.019(5) -0.006(5) 0.005(5) -0.007(4) C(11) 0.038(6) 0.026(6) 0.037(6) -0.005(5) 0.016(5) -0.004(5) C(12) 0.027(6) 0.029(6) 0.023(5) -0.001(5) 0.001(4) -0.004(5) C(13) 0.032(6) 0.026(5) 0.031(6) 0.007(5) 0.002(5) -0.006(5) C(14) 0.037(7) 0.043(7) 0.035(7) 0.005(6) 0.006(5) -0.003(5) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2847 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0718 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.1012 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 4.076 _refine_ls_shift/esd_max 0.0090 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.63 _refine_diff_density_max 1.83 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn(1) S(1) 2.329(3) ? ? yes Mn(1) S(2) 2.329(3) ? ? yes Mn(1) S(3) 2.368(3) ? ? yes Mn(1) C(11) 1.82(1) ? ? yes Mn(1) C(12) 1.81(1) ? ? yes Mn(1) C(13) 1.81(1) ? ? yes S(1) C(1) 1.84(1) ? ? yes S(1) C(10) 1.814(10) ? ? yes S(2) C(2) 1.82(1) ? ? yes S(2) C(3) 1.84(1) ? ? yes S(3) C(4) 1.83(1) ? ? yes S(3) C(5) 1.829(10) ? ? yes S(4) C(6) 1.81(1) ? ? yes S(4) C(7) 1.82(1) ? ? yes S(5) C(8) 1.82(1) ? ? yes S(5) C(9) 1.83(1) ? ? yes S(6) O(4) 1.451(8) ? ? yes S(6) O(5) 1.432(8) ? ? yes S(6) O(6) 1.435(8) ? ? yes S(6) C(14) 1.81(1) ? ? yes F(1) C(14) 1.33(1) ? ? yes F(2) C(14) 1.34(1) ? ? yes F(3) C(14) 1.30(1) ? ? yes O(1) C(11) 1.13(1) ? ? yes O(2) C(12) 1.14(1) ? ? yes O(3) C(13) 1.16(1) ? ? yes C(1) C(2) 1.50(1) ? ? yes C(3) C(4) 1.47(2) ? ? yes C(5) C(6) 1.51(1) ? ? yes C(7) C(8) 1.50(1) ? ? yes C(9) C(10) 1.54(1) ? ? yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Mn(1) S(2) 85.7(1) ? ? ? yes S(1) Mn(1) S(3) 92.00(10) ? ? ? yes S(1) Mn(1) C(11) 92.1(4) ? ? ? yes S(1) Mn(1) C(12) 178.3(3) ? ? ? yes S(1) Mn(1) C(13) 91.8(3) ? ? ? yes S(2) Mn(1) S(3) 87.3(1) ? ? ? yes S(2) Mn(1) C(11) 90.6(3) ? ? ? yes S(2) Mn(1) C(12) 92.6(3) ? ? ? yes S(2) Mn(1) C(13) 176.9(3) ? ? ? yes S(3) Mn(1) C(11) 175.2(4) ? ? ? yes S(3) Mn(1) C(12) 88.1(3) ? ? ? yes S(3) Mn(1) C(13) 91.0(3) ? ? ? yes C(11) Mn(1) C(12) 87.7(5) ? ? ? yes C(11) Mn(1) C(13) 91.3(4) ? ? ? yes C(12) Mn(1) C(13) 90.0(5) ? ? ? yes Mn(1) S(1) C(1) 107.5(4) ? ? ? yes Mn(1) S(1) C(10) 112.3(4) ? ? ? yes C(1) S(1) C(10) 102.7(5) ? ? ? yes Mn(1) S(2) C(2) 102.3(4) ? ? ? yes Mn(1) S(2) C(3) 103.6(4) ? ? ? yes C(2) S(2) C(3) 103.2(5) ? ? ? yes Mn(1) S(3) C(4) 101.8(3) ? ? ? yes Mn(1) S(3) C(5) 114.2(3) ? ? ? yes C(4) S(3) C(5) 100.5(5) ? ? ? yes C(6) S(4) C(7) 105.2(5) ? ? ? yes C(8) S(5) C(9) 101.8(5) ? ? ? yes O(4) S(6) O(5) 115.5(5) ? ? ? yes O(4) S(6) O(6) 113.5(5) ? ? ? yes O(4) S(6) C(14) 102.4(5) ? ? ? yes O(5) S(6) O(6) 115.7(5) ? ? ? yes O(5) S(6) C(14) 103.2(5) ? ? ? yes O(6) S(6) C(14) 104.2(5) ? ? ? yes S(1) C(1) C(2) 112.7(8) ? ? ? yes S(2) C(2) C(1) 114.7(8) ? ? ? yes S(2) C(3) C(4) 109.7(8) ? ? ? yes S(3) C(4) C(3) 113.0(7) ? ? ? yes S(3) C(5) C(6) 109.6(7) ? ? ? yes S(4) C(6) C(5) 112.7(7) ? ? ? yes S(4) C(7) C(8) 115.7(8) ? ? ? yes S(5) C(8) C(7) 117.0(8) ? ? ? yes S(5) C(9) C(10) 109.8(8) ? ? ? yes S(1) C(10) C(9) 108.3(7) ? ? ? yes Mn(1) C(11) O(1) 176(1) ? ? ? yes Mn(1) C(12) O(2) 175.4(9) ? ? ? yes Mn(1) C(13) O(3) 178.1(9) ? ? ? yes S(6) C(14) F(1) 111.6(8) ? ? ? yes S(6) C(14) F(2) 109.8(8) ? ? ? yes S(6) C(14) F(3) 114.2(8) ? ? ? yes F(1) C(14) F(2) 105(1) ? ? ? yes F(1) C(14) F(3) 107.8(10) ? ? ? yes F(2) C(14) F(3) 107(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 ; CIF file for fac-[Mn(CO)3([15]aneS5)]CF3SO3. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-dicarbonyl manganese(I) 1,4,7,10-tetrathiacyclododecane . 1/2CHCl2 solvate ; _chemical_name_common ? _chemical_formula_moiety '[Mn(CO)2([12]aneS4)]CF3SO3.1/2CHCl3' _chemical_formula_sum 'C11.50 H16.50 Cl1.50 F3 Mn O5 S5' _chemical_formula_weight 560.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0952(16) _cell_length_b 15.267(3) _cell_length_c 9.6411(15) _cell_angle_alpha 90.983(17) _cell_angle_beta 90.332(14) _cell_angle_gamma 86.531(13) _cell_volume 2070.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 13.9 _cell_measurement_theta_max 17.9 _exptl_crystal_description column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.580 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.120 _exptl_crystal_density_meas 'not measured ' _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 1.383 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 1.000 _exptl_absorpt_correction_T_max 0.906 _exptl_special_details ; Mn-S distances in Mn(2) cation defixed to 2.32(3) A - S)5) and S(7) disordered to give two sites each (70:30% occupancy). H atoms on major form included in fixed, calculated positions, but those on minor component omitted. Max peak and trough <0.5 A from S(6b) - i.e. in the disordered region. ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type AFC7S _diffrn_measurement_method omege/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -1.65 _diffrn_reflns_number 7633 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.1242 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7306 _reflns_number_gt 3708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'Texsan' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+9.5568P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7306 _refine_ls_number_parameters 511 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1631 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.2092 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.094 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.82066(9) 0.00833(8) 0.25147(13) 0.0214(3) Uani 1 d . . . Mn2 Mn 0.25859(11) 0.22514(9) 0.25727(15) 0.0395(4) Uani 1 d D . . Cl1 Cl 0.98789(18) 0.44223(19) 0.7696(3) 0.0523(7) Uani 1 d . . . Cl2 Cl 0.8404(2) 0.41096(18) 0.5708(3) 0.0506(7) Uani 1 d . . . Cl3 Cl 0.9134(2) 0.2710(2) 0.7469(3) 0.0560(8) Uani 1 d . . . S1 S 0.91677(15) 0.12532(14) 0.2400(2) 0.0259(5) Uani 1 d . . . S2 S 0.75782(16) 0.07705(14) 0.4521(2) 0.0282(5) Uani 1 d . . . S3 S 0.69283(16) -0.08001(14) 0.2547(2) 0.0263(5) Uani 1 d . . . S4 S 0.72065(16) 0.09612(15) 0.1118(2) 0.0300(5) Uani 1 d . . . S5 S 0.25501(18) 0.23515(16) 0.0201(2) 0.0353(6) Uani 1 d . . . S6B S 0.3810(6) 0.3226(6) 0.2543(12) 0.060(3) Uiso 0.30 d PD . . S6A S 0.3177(2) 0.3578(2) 0.2451(4) 0.0324(8) Uani 0.70 d P . . S7 S 0.2560(2) 0.25440(18) 0.4929(3) 0.0490(8) Uani 1 d . . . S8A S 0.10189(16) 0.28677(19) 0.2483(3) 0.0278(7) Uani 0.70 d PD . . S8B S 0.1563(4) 0.3487(3) 0.2583(7) 0.0248(16) Uiso 0.30 d PD . . S9 S 0.79148(17) 0.45725(14) 0.1647(3) 0.0316(6) Uani 1 d . . . S10 S 0.57082(17) 0.21867(16) 0.7639(3) 0.0371(6) Uani 1 d . . . F1 F 0.6584(6) 0.4080(6) 0.3278(7) 0.087(3) Uani 1 d . . . F2 F 0.6070(5) 0.4618(5) 0.1353(9) 0.075(2) Uani 1 d . . . F3 F 0.6714(5) 0.3326(4) 0.1396(8) 0.0625(19) Uani 1 d . . . F4 F 0.6639(5) 0.3580(5) 0.8203(8) 0.076(2) Uani 1 d . . . F5 F 0.5158(5) 0.3848(4) 0.7851(9) 0.075(2) Uani 1 d . . . F6 F 0.6069(5) 0.3532(5) 0.6149(7) 0.074(2) Uani 1 d . . . O1 O 0.9471(5) -0.1024(5) 0.4287(8) 0.054(2) Uani 1 d . . . O2 O 0.9238(5) -0.0885(5) 0.0269(8) 0.052(2) Uani 1 d . . . O3 O 0.4316(5) 0.1092(6) 0.2577(8) 0.061(2) Uani 1 d . . . O4 O 0.1661(7) 0.0583(7) 0.2736(9) 0.075(3) Uani 1 d . . . O5 O 0.7830(5) 0.5407(4) 0.2373(8) 0.0494(19) Uani 1 d . . . O6 O 0.7966(6) 0.4629(5) 0.0181(7) 0.056(2) Uani 1 d . . . O7 O 0.8570(5) 0.3937(5) 0.2268(8) 0.054(2) Uani 1 d . . . O8 O 0.5459(6) 0.2118(5) 0.9075(8) 0.056(2) Uani 1 d . . . O9 O 0.4941(6) 0.2057(5) 0.6675(10) 0.066(2) Uani 1 d . . . O10 O 0.6605(6) 0.1753(5) 0.7252(8) 0.058(2) Uani 1 d . . . C1 C 0.8741(6) 0.1991(6) 0.3810(10) 0.032(2) Uani 1 d . . . H1A H 0.9125 0.1870 0.4630 0.080 Uiso 1 calc . . . H1B H 0.8831 0.2591 0.3548 0.080 Uiso 1 calc . . . C2 C 0.7700(7) 0.1913(6) 0.4172(10) 0.034(2) Uani 1 d . . . H2A H 0.7293 0.2100 0.3404 0.080 Uiso 1 calc . . . H2B H 0.7530 0.2273 0.4982 0.080 Uiso 1 calc . . . C3 C 0.6322(7) 0.0597(7) 0.4320(10) 0.038(2) Uani 1 d . . . H3A H 0.5978 0.0785 0.5152 0.080 Uiso 1 calc . . . H3B H 0.6057 0.0926 0.3542 0.080 Uiso 1 calc . . . C4 C 0.6255(7) -0.0383(6) 0.4064(11) 0.037(2) Uani 1 d . . . H4A H 0.5593 -0.0505 0.3938 0.080 Uiso 1 calc . . . H4B H 0.6490 -0.0694 0.4878 0.080 Uiso 1 calc . . . C5 C 0.6141(6) -0.0414(6) 0.1121(10) 0.031(2) Uani 1 d . . . H5A H 0.5910 -0.0918 0.0628 0.080 Uiso 1 calc . . . H5B H 0.5596 -0.0079 0.1509 0.080 Uiso 1 calc . . . C6 C 0.6622(7) 0.0141(6) 0.0122(11) 0.039(2) Uani 1 d . . . H6A H 0.6160 0.0418 -0.0506 0.080 Uiso 1 calc . . . H6B H 0.7083 -0.0214 -0.0420 0.080 Uiso 1 calc . . . C7 C 0.8059(7) 0.1403(7) -0.0031(10) 0.037(2) Uani 1 d . . . H7A H 0.8393 0.0933 -0.0556 0.080 Uiso 1 calc . . . H7B H 0.7741 0.1804 -0.0676 0.080 Uiso 1 calc . . . C8 C 0.8749(7) 0.1880(6) 0.0873(10) 0.033(2) Uani 1 d . . . H8A H 0.8442 0.2434 0.1186 0.080 Uiso 1 calc . . . H8B H 0.9293 0.2010 0.0320 0.080 Uiso 1 calc . . . C9 C 0.8973(7) -0.0574(6) 0.3631(10) 0.034(2) Uani 1 d . . . C10 C 0.8806(6) -0.0496(6) 0.1120(10) 0.030(2) Uani 1 d . . . C11 C 0.3410(7) 0.3173(7) -0.0215(11) 0.046(3) Uani 1 d . . . H11A H 0.3833 0.2942 -0.0941 0.080 Uiso 1 calc . . . H11B H 0.3073 0.3699 -0.0555 0.080 Uiso 1 calc . . . C12B C 0.362(3) 0.396(3) 0.098(4) 0.046(9) Uiso 0.30 d P . . C12A C 0.3963(10) 0.3391(12) 0.1006(18) 0.050(4) Uani 0.70 d P . . H12A H 0.4302 0.3913 0.0840 0.080 Uiso 0.70 calc P . . H12B H 0.4426 0.2912 0.1205 0.080 Uiso 0.70 calc P . . C13A C 0.3946(11) 0.3517(11) 0.399(2) 0.054(5) Uani 0.70 d P . . H13A H 0.4404 0.3020 0.3900 0.080 Uiso 0.70 calc P . . H13B H 0.4292 0.4046 0.4076 0.080 Uiso 0.70 calc P . . C13B C 0.370(2) 0.406(2) 0.398(3) 0.029(7) Uiso 0.30 d P . . C14 C 0.3386(9) 0.3425(8) 0.5207(12) 0.058(3) Uani 1 d . . . H14A H 0.3028 0.3974 0.5415 0.080 Uiso 1 calc . . . H14B H 0.3799 0.3285 0.5991 0.080 Uiso 1 calc . . . C15 C 0.1414(8) 0.3158(7) 0.5223(11) 0.045(3) Uani 1 d . . . H15A H 0.0962 0.2754 0.5547 0.080 Uiso 1 calc . . . H15B H 0.1496 0.3590 0.5957 0.080 Uiso 1 calc . . . C16A C 0.0985(9) 0.3636(10) 0.3932(14) 0.028(3) Uani 0.70 d P . . H16A H 0.1349 0.4136 0.3720 0.080 Uiso 0.70 calc P . . H16B H 0.0334 0.3848 0.4115 0.080 Uiso 0.70 calc P . . C16B C 0.092(3) 0.316(3) 0.407(4) 0.036(9) Uiso 0.30 d P . . C17B C 0.0882(19) 0.311(2) 0.115(3) 0.014(6) Uiso 0.30 d P . . C17A C 0.1007(9) 0.3547(9) 0.0919(13) 0.028(3) Uani 0.70 d P . . H17A H 0.0363 0.3756 0.0687 0.080 Uiso 0.70 calc P . . H17B H 0.1388 0.4049 0.1063 0.080 Uiso 0.70 calc P . . C18 C 0.1418(7) 0.2960(6) -0.0211(10) 0.038(2) Uani 1 d . . . H18A H 0.1513 0.3313 -0.1019 0.080 Uiso 1 calc . . . H18B H 0.0955 0.2538 -0.0461 0.080 Uiso 1 calc . . . C19 C 0.3663(7) 0.1567(7) 0.2594(10) 0.036(2) Uani 1 d . . . C20 C 0.1991(8) 0.1267(8) 0.2665(11) 0.046(3) Uani 1 d . . . C21 C 0.6758(8) 0.4130(7) 0.1954(12) 0.047(3) Uani 1 d . . . C22 C 0.5895(8) 0.3344(7) 0.7423(11) 0.042(3) Uani 1 d . . . C23 C 0.8860(7) 0.3852(7) 0.7364(11) 0.043(3) Uani 1 d . . . H23 H 0.8379 0.4026 0.8061 0.080 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0176(7) 0.0189(7) 0.0277(7) 0.0016(5) 0.0033(5) 0.0007(5) Mn2 0.0607(11) 0.0267(8) 0.0283(8) 0.0038(6) 0.0120(7) 0.0215(7) Cl1 0.0290(14) 0.0595(18) 0.0666(19) -0.0131(14) -0.0108(13) 0.0069(12) Cl2 0.0514(17) 0.0496(16) 0.0493(17) -0.0089(13) -0.0131(13) 0.0043(13) Cl3 0.068(2) 0.0556(18) 0.0452(16) 0.0102(13) 0.0030(14) -0.0093(15) S1 0.0200(11) 0.0271(12) 0.0309(12) 0.0017(9) 0.0031(9) -0.0037(9) S2 0.0261(12) 0.0252(11) 0.0332(13) -0.0016(9) 0.0073(10) -0.0015(9) S3 0.0275(12) 0.0182(11) 0.0334(13) -0.0005(9) 0.0079(10) -0.0024(9) S4 0.0272(12) 0.0264(12) 0.0368(13) 0.0049(10) -0.0021(10) -0.0043(9) S5 0.0406(14) 0.0347(13) 0.0288(13) 0.0023(10) 0.0088(11) 0.0140(11) S6A 0.0178(17) 0.0330(18) 0.046(2) -0.0058(15) 0.0022(14) 0.0014(14) S7 0.075(2) 0.0396(15) 0.0288(14) 0.0012(11) 0.0112(13) 0.0233(14) S8A 0.0251(17) 0.0221(16) 0.0362(19) 0.0003(14) 0.0049(14) -0.0019(13) S9 0.0354(13) 0.0205(11) 0.0390(14) -0.0020(10) 0.0050(11) -0.0015(10) S10 0.0293(13) 0.0361(14) 0.0450(15) -0.0088(11) -0.0008(11) 0.0020(11) F1 0.095(6) 0.119(7) 0.053(5) 0.011(4) 0.031(4) -0.045(5) F2 0.035(4) 0.056(4) 0.133(7) 0.013(4) -0.006(4) -0.002(3) F3 0.057(4) 0.037(4) 0.095(5) 0.005(4) -0.013(4) -0.021(3) F4 0.054(4) 0.088(6) 0.090(6) -0.010(4) -0.011(4) -0.039(4) F5 0.077(5) 0.034(4) 0.114(6) -0.009(4) 0.037(5) 0.000(3) F6 0.080(5) 0.086(5) 0.060(5) 0.018(4) 0.018(4) -0.023(4) O1 0.042(5) 0.051(5) 0.067(5) 0.019(4) -0.013(4) 0.017(4) O2 0.045(5) 0.059(5) 0.052(5) -0.022(4) 0.022(4) -0.002(4) O3 0.036(4) 0.092(6) 0.051(5) -0.013(4) 0.003(4) 0.027(4) O4 0.065(6) 0.099(8) 0.063(6) 0.016(5) 0.010(5) -0.022(6) O5 0.054(5) 0.032(4) 0.062(5) -0.019(3) 0.008(4) -0.004(3) O6 0.074(6) 0.059(5) 0.037(4) -0.009(4) 0.021(4) -0.021(4) O7 0.049(5) 0.034(4) 0.078(6) 0.009(4) -0.010(4) 0.001(4) O8 0.060(5) 0.047(5) 0.059(5) 0.000(4) 0.019(4) 0.000(4) O9 0.058(5) 0.037(4) 0.103(7) -0.006(4) -0.034(5) -0.013(4) O10 0.055(5) 0.066(5) 0.050(5) -0.010(4) 0.009(4) 0.025(4) C1 0.026(5) 0.030(5) 0.039(6) -0.003(4) 0.004(4) -0.003(4) C2 0.041(6) 0.021(5) 0.041(6) -0.006(4) 0.013(5) -0.006(4) C3 0.026(5) 0.046(6) 0.042(6) -0.020(5) 0.017(4) -0.011(4) C4 0.041(6) 0.022(5) 0.048(6) -0.005(4) 0.009(5) -0.010(4) C5 0.023(5) 0.026(5) 0.044(6) -0.003(4) -0.001(4) -0.001(4) C6 0.042(6) 0.031(5) 0.045(6) 0.008(5) -0.017(5) -0.013(5) C7 0.037(6) 0.042(6) 0.034(5) 0.009(5) 0.001(4) -0.008(5) C8 0.036(6) 0.024(5) 0.038(6) 0.010(4) -0.003(4) -0.007(4) C9 0.034(6) 0.032(5) 0.035(5) -0.006(4) 0.005(5) -0.001(4) C10 0.018(5) 0.023(5) 0.051(6) 0.006(4) 0.002(4) -0.005(4) C11 0.038(6) 0.057(7) 0.042(6) 0.017(5) 0.014(5) 0.010(5) C12A 0.019(8) 0.062(12) 0.072(12) -0.006(9) 0.018(8) -0.021(8) C13A 0.033(9) 0.040(10) 0.088(14) -0.022(9) -0.007(9) -0.004(8) C14 0.070(9) 0.064(8) 0.038(6) -0.013(6) 0.006(6) 0.012(7) C15 0.055(7) 0.037(6) 0.042(6) -0.002(5) 0.022(5) 0.005(5) C16A 0.021(7) 0.024(8) 0.041(8) 0.001(6) 0.009(6) -0.007(6) C17A 0.029(7) 0.026(8) 0.028(7) 0.015(6) -0.004(6) 0.000(6) C18 0.036(6) 0.036(5) 0.041(6) 0.011(4) 0.011(5) 0.016(4) C19 0.031(6) 0.042(6) 0.035(6) -0.007(5) -0.001(4) -0.004(5) C20 0.039(6) 0.067(8) 0.032(6) 0.017(5) 0.010(5) 0.010(6) C21 0.044(7) 0.033(6) 0.065(8) 0.018(5) -0.001(6) -0.005(5) C22 0.042(6) 0.043(6) 0.041(6) -0.010(5) 0.010(5) -0.017(5) C23 0.024(5) 0.058(7) 0.045(6) -0.014(5) 0.003(5) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C10 1.785(10) . ? Mn1 C9 1.795(10) . ? Mn1 S1 2.311(2) . ? Mn1 S3 2.316(3) . ? Mn1 S4 2.326(3) . ? Mn1 S2 2.338(3) . ? Mn2 C20 1.769(14) . ? Mn2 C19 1.791(10) . ? Mn2 S6A 2.242(4) . ? Mn2 S5 2.294(3) . ? Mn2 S8B 2.304(3) . ? Mn2 S7 2.307(3) . ? Mn2 S6B 2.347(3) . ? Mn2 S8A 2.3496(19) . ? Cl1 C23 1.749(10) . ? Cl2 C23 1.760(11) . ? Cl3 C23 1.767(11) . ? S1 C1 1.831(9) . ? S1 C8 1.845(9) . ? S2 C2 1.801(9) . ? S2 C3 1.815(10) . ? S3 C4 1.832(10) . ? S3 C5 1.844(9) . ? S4 C6 1.801(10) . ? S4 C7 1.806(10) . ? S5 C18 1.842(9) . ? S5 C11 1.847(11) . ? S6B C13B 1.86(3) . ? S6B C12B 1.90(4) . ? S6A C12A 1.794(15) . ? S6A C13A 1.835(18) . ? S6A S8B 2.292(7) . ? S7 C15 1.839(11) . ? S7 C14 1.846(14) . ? S8A C16A 1.808(14) . ? S8A C17A 1.844(13) . ? S8B C17B 1.78(3) . ? S8B C16B 1.79(4) . ? S9 O6 1.420(7) . ? S9 O7 1.434(7) . ? S9 O5 1.443(7) . ? S9 C21 1.830(11) . ? S10 O8 1.438(8) . ? S10 O10 1.439(7) . ? S10 O9 1.442(8) . ? S10 C22 1.818(11) . ? F1 C21 1.306(13) . ? F2 C21 1.325(12) . ? F3 C21 1.335(12) . ? F4 C22 1.351(12) . ? F5 C22 1.319(12) . ? F6 C22 1.294(12) . ? O1 C9 1.147(11) . ? O2 C10 1.158(11) . ? O3 C19 1.136(11) . ? O4 C20 1.171(14) . ? C1 C2 1.522(13) . ? C3 C4 1.521(13) . ? C5 C6 1.487(13) . ? C7 C8 1.513(13) . ? C11 C12A 1.45(2) . ? C13A C14 1.43(2) . ? C15 C16A 1.556(18) . ? C17A C18 1.496(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Mn1 C9 85.7(4) . . ? C10 Mn1 S1 93.0(3) . . ? C9 Mn1 S1 96.3(3) . . ? C10 Mn1 S3 95.4(3) . . ? C9 Mn1 S3 96.9(3) . . ? S1 Mn1 S3 164.80(9) . . ? C10 Mn1 S4 95.7(3) . . ? C9 Mn1 S4 178.5(3) . . ? S1 Mn1 S4 83.12(9) . . ? S3 Mn1 S4 83.47(9) . . ? C10 Mn1 S2 172.7(3) . . ? C9 Mn1 S2 87.2(3) . . ? S1 Mn1 S2 85.98(9) . . ? S3 Mn1 S2 87.20(9) . . ? S4 Mn1 S2 91.30(9) . . ? C20 Mn2 C19 86.1(5) . . ? C20 Mn2 S6A 173.5(4) . . ? C19 Mn2 S6A 100.4(3) . . ? C20 Mn2 S5 96.6(3) . . ? C19 Mn2 S5 94.0(3) . . ? S6A Mn2 S5 82.98(13) . . ? C20 Mn2 S8B 113.0(4) . . ? C19 Mn2 S8B 160.8(4) . . ? S6A Mn2 S8B 60.5(2) . . ? S5 Mn2 S8B 85.95(19) . . ? C20 Mn2 S7 95.5(4) . . ? C19 Mn2 S7 95.7(3) . . ? S6A Mn2 S7 84.04(13) . . ? S5 Mn2 S7 165.00(11) . . ? S8B Mn2 S7 81.1(2) . . ? C20 Mn2 S6B 160.9(5) . . ? C19 Mn2 S6B 74.9(4) . . ? S6A Mn2 S6B 25.5(3) . . ? S5 Mn2 S6B 86.8(3) . . ? S8B Mn2 S6B 85.9(3) . . ? S7 Mn2 S6B 84.7(3) . . ? C20 Mn2 S8A 82.0(3) . . ? C19 Mn2 S8A 167.9(3) . . ? S6A Mn2 S8A 91.55(12) . . ? S5 Mn2 S8A 85.33(11) . . ? S8B Mn2 S8A 31.3(2) . . ? S7 Mn2 S8A 87.53(12) . . ? S6B Mn2 S8A 117.0(3) . . ? C1 S1 C8 100.9(4) . . ? C1 S1 Mn1 104.0(3) . . ? C8 S1 Mn1 105.6(3) . . ? C2 S2 C3 105.8(5) . . ? C2 S2 Mn1 102.2(3) . . ? C3 S2 Mn1 101.5(3) . . ? C4 S3 C5 101.2(4) . . ? C4 S3 Mn1 103.0(3) . . ? C5 S3 Mn1 105.5(3) . . ? C6 S4 C7 106.2(5) . . ? C6 S4 Mn1 100.9(3) . . ? C7 S4 Mn1 100.7(3) . . ? C18 S5 C11 101.0(5) . . ? C18 S5 Mn2 105.5(3) . . ? C11 S5 Mn2 105.3(4) . . ? C13B S6B C12B 100.7(17) . . ? C13B S6B Mn2 112.0(11) . . ? C12B S6B Mn2 108.2(12) . . ? C12A S6A C13A 105.2(8) . . ? C12A S6A Mn2 99.8(6) . . ? C13A S6A Mn2 98.5(6) . . ? C12A S6A S8B 130.2(6) . . ? C13A S6A S8B 122.1(6) . . ? Mn2 S6A S8B 61.07(14) . . ? C15 S7 C14 100.5(5) . . ? C15 S7 Mn2 104.4(4) . . ? C14 S7 Mn2 105.4(4) . . ? C16A S8A C17A 105.4(7) . . ? C16A S8A Mn2 102.6(4) . . ? C17A S8A Mn2 103.5(4) . . ? C17B S8B C16B 103.6(16) . . ? C17B S8B S6A 121.8(9) . . ? C16B S8B S6A 126.0(12) . . ? C17B S8B Mn2 93.4(9) . . ? C16B S8B Mn2 94.0(12) . . ? S6A S8B Mn2 58.38(14) . . ? O6 S9 O7 115.6(5) . . ? O6 S9 O5 114.6(5) . . ? O7 S9 O5 114.4(5) . . ? O6 S9 C21 104.1(5) . . ? O7 S9 C21 103.2(5) . . ? O5 S9 C21 102.5(5) . . ? O8 S10 O10 115.2(5) . . ? O8 S10 O9 114.6(5) . . ? O10 S10 O9 114.8(5) . . ? O8 S10 C22 104.4(5) . . ? O10 S10 C22 103.8(5) . . ? O9 S10 C22 101.7(5) . . ? C2 C1 S1 114.0(6) . . ? C1 C2 S2 105.9(6) . . ? C4 C3 S2 106.0(7) . . ? C3 C4 S3 113.3(6) . . ? C6 C5 S3 112.9(6) . . ? C5 C6 S4 107.3(7) . . ? C8 C7 S4 106.8(6) . . ? C7 C8 S1 113.5(6) . . ? O1 C9 Mn1 176.4(9) . . ? O2 C10 Mn1 176.0(9) . . ? C12A C11 S5 110.6(8) . . ? C11 C12A S6A 109.0(9) . . ? C14 C13A S6A 110.0(10) . . ? C13A C14 S7 110.0(9) . . ? C16A C15 S7 115.0(7) . . ? C15 C16A S8A 108.4(9) . . ? C18 C17A S8A 105.6(8) . . ? C17A C18 S5 115.9(8) . . ? O3 C19 Mn2 175.8(9) . . ? O4 C20 Mn2 175.2(10) . . ? F1 C21 F2 109.5(10) . . ? F1 C21 F3 107.8(9) . . ? F2 C21 F3 105.8(9) . . ? F1 C21 S9 111.4(8) . . ? F2 C21 S9 110.7(7) . . ? F3 C21 S9 111.3(8) . . ? F6 C22 F5 108.5(10) . . ? F6 C22 F4 107.6(8) . . ? F5 C22 F4 105.9(8) . . ? F6 C22 S10 112.5(7) . . ? F5 C22 S10 111.8(7) . . ? F4 C22 S10 110.3(8) . . ? Cl1 C23 Cl2 110.1(6) . . ? Cl1 C23 Cl3 110.0(5) . . ? Cl2 C23 Cl3 110.0(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.428 _refine_diff_density_min -1.896 _refine_diff_density_rms 0.148