Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Konietzny, Stefan' 'Reiss, Guido J.' _publ_contact_author_name 'Dr Guido J. Reiss' _publ_contact_author_address ; Chemie Anorganische Chemie Universitaetsstr. 1 D-40225 Duesseldorf D-40225 GERMANY ; _publ_contact_author_email 'REISSG@UNI-DUESSELDORF.DE' _publ_section_title ; How realistic are alternating C-C-bond lengths in s-cis-1,3-butadiene transition- metal complexes? ; data_C~9~H~12~MNO_LT _database_code_CSD 158318 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(butadiene) carbonyle manganese ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H12 Mn O' _chemical_formula_weight 191.13 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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 m' _symmetry_space_group_name_Hall 'P -4 2ab' _symmetry_Int_Tables_number 113 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 7.729(3) _cell_length_b 7.729(3) _cell_length_c 7.167(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 428.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 17.5 _cell_measurement_theta_max 20.1 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 -1.00 0.390 0.00 0.00 1.00 0.390 -1.00 -1.00 0.00 0.075 -1.00 1.00 0.00 0.075 1.00 -1.00 0.00 0.073 1.00 1.00 0.00 0.050 _exptl_crystal_description 'needle' _exptl_crystal_colour blue-violet _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 198 _exptl_absorpt_coefficient_mu 1.478 _exptl_absorpt_correction_type numerical # # '(X-RED 1.07, Stoe 1996)' # _exptl_absorpt_correction_T_min 0.7803 _exptl_absorpt_correction_T_max 0.8491 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _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 'Siemens P4 Diffractometer' _diffrn_measurement_method 'omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2007 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 4.69 _diffrn_reflns_theta_max 25.46 _reflns_number_total 445 _reflns_number_gt 440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS 2.10b (Siemens, 1994)' _computing_cell_refinement 'XSCANS 2.10b (Siemens, 1994)' _computing_data_reduction 'XSCANS 2.10b (Siemens, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0169P)^2^+0.0280P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'free' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.038(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 445 _refine_ls_number_parameters 44 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0130 _refine_ls_R_factor_gt 0.0128 _refine_ls_wR_factor_ref 0.0328 _refine_ls_wR_factor_gt 0.0328 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 Mn Mn 0.5000 1.0000 0.77766(3) 0.01379(13) Uani 1 4 d S . C1 C 0.5000 1.0000 1.0302(3) 0.0257(4) Uani 1 4 d S . O1 O 0.5000 1.0000 1.1903(2) 0.0489(5) Uani 1 4 d S . C3 C 0.70437(17) 0.92536(17) 0.60710(17) 0.0257(3) Uani 1 1 d . . C2 C 0.77617(16) 0.9783(2) 0.77891(18) 0.0312(3) Uani 1 1 d . . H1 H 0.845(3) 1.087(3) 0.787(3) 0.043(5) Uiso 1 1 d . . H3 H 0.729(2) 0.979(2) 0.4970(17) 0.028(4) Uiso 1 1 d . . H2 H 0.801(2) 0.895(2) 0.879(3) 0.032(4) Uiso 1 1 d . . 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 Mn 0.01414(14) 0.01414(14) 0.01310(17) 0.000 0.000 0.0010(2) C1 0.0282(6) 0.0282(6) 0.0206(10) 0.000 0.000 -0.0020(18) O1 0.0655(8) 0.0655(8) 0.0156(8) 0.000 0.000 -0.0084(19) C3 0.0203(7) 0.0323(7) 0.0244(6) -0.0014(5) 0.0066(5) 0.0085(5) C2 0.0166(6) 0.0448(10) 0.0321(6) -0.0003(8) -0.0024(4) 0.0036(6) _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 Mn C1 1.8097(19) . ? Mn C3 2.0790(13) 2_675 ? Mn C3 2.0790(13) 7_665 ? Mn C3 2.0790(13) . ? Mn C3 2.0790(13) 8_455 ? Mn C2 2.1411(15) . ? Mn C2 2.1411(15) 8_455 ? Mn C2 2.1411(15) 2_675 ? Mn C2 2.1411(15) 7_665 ? C1 O1 1.148(3) . ? C3 C2 1.4111(18) . ? C3 C3 1.418(3) 7_665 ? C3 H3 0.912(13) . ? C2 H1 1.00(2) . ? C2 H2 0.979(19) . ? 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 C1 Mn C3 126.01(4) . 2_675 ? C1 Mn C3 126.01(4) . 7_665 ? C3 Mn C3 94.35(7) 2_675 7_665 ? C1 Mn C3 126.01(4) . . ? C3 Mn C3 107.97(8) 2_675 . ? C3 Mn C3 39.88(7) 7_665 . ? C1 Mn C3 126.01(4) . 8_455 ? C3 Mn C3 39.88(7) 2_675 8_455 ? C3 Mn C3 107.97(8) 7_665 8_455 ? C3 Mn C3 94.35(7) . 8_455 ? C1 Mn C2 89.76(3) . . ? C3 Mn C2 141.41(5) 2_675 . ? C3 Mn C2 70.50(6) 7_665 . ? C3 Mn C2 39.04(5) . . ? C3 Mn C2 109.80(6) 8_455 . ? C1 Mn C2 89.76(3) . 8_455 ? C3 Mn C2 70.50(6) 2_675 8_455 ? C3 Mn C2 141.41(5) 7_665 8_455 ? C3 Mn C2 109.80(6) . 8_455 ? C3 Mn C2 39.04(5) 8_455 8_455 ? C2 Mn C2 99.00(10) . 8_455 ? C1 Mn C2 89.76(3) . 2_675 ? C3 Mn C2 39.04(5) 2_675 2_675 ? C3 Mn C2 109.80(6) 7_665 2_675 ? C3 Mn C2 141.41(5) . 2_675 ? C3 Mn C2 70.50(6) 8_455 2_675 ? C2 Mn C2 179.52(7) . 2_675 ? C2 Mn C2 81.00(10) 8_455 2_675 ? C1 Mn C2 89.76(3) . 7_665 ? C3 Mn C2 109.80(6) 2_675 7_665 ? C3 Mn C2 39.04(5) 7_665 7_665 ? C3 Mn C2 70.50(6) . 7_665 ? C3 Mn C2 141.41(5) 8_455 7_665 ? C2 Mn C2 81.00(10) . 7_665 ? C2 Mn C2 179.52(7) 8_455 7_665 ? C2 Mn C2 99.00(10) 2_675 7_665 ? O1 C1 Mn 180.000(1) . . ? C2 C3 C3 118.88(8) . 7_665 ? C2 C3 Mn 72.86(7) . . ? C3 C3 Mn 70.06(4) 7_665 . ? C2 C3 H3 122.9(10) . . ? C3 C3 H3 117.9(10) 7_665 . ? Mn C3 H3 122.6(11) . . ? C3 C2 Mn 68.10(7) . . ? C3 C2 H1 120.2(12) . . ? Mn C2 H1 117.7(13) . . ? C3 C2 H2 121.5(10) . . ? Mn C2 H2 104.4(11) . . ? H1 C2 H2 114.2(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1C Mn C2 C1 -25.21(10) . . . . ? C2 Mn C2 C1 154.79(10) 2_675 . . . ? C2 Mn C2 C1 -130.50(9) 7_665 . . . ? C2 Mn C2 C1 116.45(9) 8_455 . . . ? C1 Mn C2 C1 79.63(12) 8_455 . . . ? C1 Mn C2 C1 -179.74(4) 2_675 . . . ? C1 Mn C2 C1 -99.97(13) 7_665 . . . ? C1C Mn C2 C2 105.29(3) . . . 7_665 ? C2 Mn C2 C2 -74.71(3) 2_675 . . 7_665 ? C2 Mn C2 C2 -113.05(5) 8_455 . . 7_665 ? C1 Mn C2 C2 130.50(9) . . . 7_665 ? C1 Mn C2 C2 -149.86(5) 8_455 . . 7_665 ? C1 Mn C2 C2 -49.23(8) 2_675 . . 7_665 ? C1 Mn C2 C2 30.53(5) 7_665 . . 7_665 ? C2 C2 C1 Mn -54.71(6) 7_665 . . . ? C1C Mn C1 C2 159.85(8) . . . . ? C2 Mn C1 C2 -40.51(16) 2_675 . . . ? C2 Mn C1 C2 31.15(8) 7_665 . . . ? C2 Mn C1 C2 -71.59(11) 8_455 . . . ? C1 Mn C1 C2 -110.43(8) 8_455 . . . ? C1 Mn C1 C2 159.85(8) 2_675 . . . ? C1 Mn C1 C2 70.05(9) 7_665 . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.46 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.220 _refine_diff_density_min -0.160 _refine_diff_density_rms 0.034 ############################################################ data_C~9~H~12~MNO_RT _database_code_CSD 158319 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H12 Mn O' _chemical_formula_weight 191.13 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' 'O' 'O' 0.0106 0.0060 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 m' _symmetry_space_group_name_Hall 'P -4 2ab' _symmetry_Int_Tables_number 113 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 7.8215(8) _cell_length_b 7.8215(8) _cell_length_c 7.2234(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 441.90(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 6.22 _cell_measurement_theta_max 26.99 _exptl_crystal_description 'needle' _exptl_crystal_colour 'blue violet' _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 198 _exptl_absorpt_coefficient_mu 1.432 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7803 _exptl_absorpt_correction_T_max 0.8491 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _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 'Stoe IPDS diffractometer' _diffrn_measurement_method 'omega-scan' _diffrn_detector_area_resol_mean 50 _diffrn_standards_number 'A maximum of 50 on each image, with I> 6I/s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 4831 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 6.22 _diffrn_reflns_theta_max 26.99 _reflns_number_total 490 _reflns_number_gt 488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS-Software, Ver.2.85 (Stoe & Cie, 1997)' _computing_cell_refinement 'IPDS-Software, Ver.2.85 (Stoe & Cie, 1997)' _computing_data_reduction 'IPDS-Software, Ver.2.85 (Stoe & Cie, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+0.0296P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'free' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 490 _refine_ls_number_parameters 43 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0203 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0527 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.007 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.5000 0.0000 0.22267(4) 0.03010(18) Uani 1 4 d S . . C1 C 0.5000 0.0000 -0.0264(4) 0.0537(6) Uani 1 4 d S . . O1 O 0.5000 0.0000 -0.1850(4) 0.1016(12) Uani 1 4 d S . . C3 C 0.2981(2) 0.0742(3) 0.3913(3) 0.0551(5) Uani 1 1 d . . . C2 C 0.2260(2) 0.0201(4) 0.2232(3) 0.0641(6) Uani 1 1 d . . . H1 H 0.149(5) -0.076(5) 0.216(5) 0.076(8) Uiso 1 1 d . . . H3 H 0.279(3) 0.014(4) 0.500(3) 0.071(6) Uiso 1 1 d . . . H2 H 0.210(4) 0.097(3) 0.140(5) 0.064(7) Uiso 1 1 d . . . 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 Mn 0.03104(19) 0.03104(19) 0.0282(2) 0.000 0.000 0.00053(18) C1 0.0625(10) 0.0625(10) 0.0363(14) 0.000 0.000 -0.002(3) O1 0.1375(19) 0.1375(19) 0.0298(11) 0.000 0.000 -0.014(4) C3 0.0428(8) 0.0712(10) 0.0512(9) -0.0035(8) 0.0123(8) 0.0161(7) C2 0.0345(7) 0.0906(17) 0.0672(11) 0.0016(18) -0.0060(6) 0.0045(9) _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 Mn C1 1.799(3) . ? Mn C3 2.0771(15) 7 ? Mn C3 2.0771(15) 2_655 ? Mn C3 2.0771(15) . ? Mn C3 2.0771(15) 8_545 ? Mn C2 2.1486(19) 8_545 ? Mn C2 2.1486(19) 7 ? Mn C2 2.1486(19) 2_655 ? Mn C2 2.1486(19) . ? C1 O1 1.146(4) . ? C3 C2 1.404(3) . ? C3 C3 1.412(4) 7 ? C3 H3 0.93(3) . ? C2 H1 0.97(4) . ? C2 H2 0.86(3) . ? 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 C1 Mn C3 125.90(6) . 7 ? C1 Mn C3 125.90(6) . 2_655 ? C3 Mn C3 94.67(12) 7 2_655 ? C1 Mn C3 125.90(6) . . ? C3 Mn C3 39.74(12) 7 . ? C3 Mn C3 108.21(11) 2_655 . ? C1 Mn C3 125.90(6) . 8_545 ? C3 Mn C3 108.21(11) 7 8_545 ? C3 Mn C3 39.74(12) 2_655 8_545 ? C3 Mn C3 94.67(12) . 8_545 ? C1 Mn C2 90.11(7) . 8_545 ? C3 Mn C2 141.04(9) 7 8_545 ? C3 Mn C2 70.39(10) 2_655 8_545 ? C3 Mn C2 109.47(11) . 8_545 ? C3 Mn C2 38.75(8) 8_545 8_545 ? C1 Mn C2 90.11(7) . 7 ? C3 Mn C2 38.75(8) 7 7 ? C3 Mn C2 109.47(11) 2_655 7 ? C3 Mn C2 70.39(10) . 7 ? C3 Mn C2 141.04(9) 8_545 7 ? C2 Mn C2 179.78(14) 8_545 7 ? C1 Mn C2 90.11(7) . 2_655 ? C3 Mn C2 109.47(11) 7 2_655 ? C3 Mn C2 38.75(8) 2_655 2_655 ? C3 Mn C2 141.04(9) . 2_655 ? C3 Mn C2 70.39(10) 8_545 2_655 ? C2 Mn C2 81.60(18) 8_545 2_655 ? C2 Mn C2 98.40(18) 7 2_655 ? C1 Mn C2 90.11(7) . . ? C3 Mn C2 70.39(10) 7 . ? C3 Mn C2 141.04(9) 2_655 . ? C3 Mn C2 38.75(8) . . ? C3 Mn C2 109.47(11) 8_545 . ? C2 Mn C2 98.40(18) 8_545 . ? C2 Mn C2 81.60(18) 7 . ? C2 Mn C2 179.78(13) 2_655 . ? O1 C1 Mn 180.0 . . ? C2 C3 C3 119.82(14) . 7 ? C2 C3 Mn 73.38(11) . . ? C3 C3 Mn 70.13(6) 7 . ? C2 C3 H3 121.0(16) . . ? C3 C3 H3 118.2(16) 7 . ? Mn C3 H3 118.7(17) . . ? C3 C2 Mn 67.87(9) . . ? C3 C2 H1 122(2) . . ? Mn C2 H1 124(2) . . ? C3 C2 H2 116.9(19) . . ? Mn C2 H2 101.2(19) . . ? H1 C2 H2 115(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Mn C1 O1 -70(100) 7 . . . ? C3 Mn C1 O1 160(100) 2_655 . . . ? C3 Mn C1 O1 -20(100) . . . . ? C3 Mn C1 O1 110(100) 8_545 . . . ? C2 Mn C1 O1 94(100) 8_545 . . . ? C2 Mn C1 O1 -86(100) 7 . . . ? C2 Mn C1 O1 176(100) 2_655 . . . ? C2 Mn C1 O1 -4(100) . . . . ? C1 Mn C3 C2 26.11(18) . . . . ? C3 Mn C3 C2 131.28(15) 7 . . . ? C3 Mn C3 C2 -153.89(18) 2_655 . . . ? C3 Mn C3 C2 -115.63(17) 8_545 . . . ? C2 Mn C3 C2 -78.9(2) 8_545 . . . ? C2 Mn C3 C2 101.3(2) 7 . . . ? C2 Mn C3 C2 -179.88(8) 2_655 . . . ? C1 Mn C3 C3 -105.17(5) . . . 7 ? C3 Mn C3 C3 74.83(5) 2_655 . . 7 ? C3 Mn C3 C3 113.09(7) 8_545 . . 7 ? C2 Mn C3 C3 149.86(9) 8_545 . . 7 ? C2 Mn C3 C3 -29.96(10) 7 . . 7 ? C2 Mn C3 C3 48.85(14) 2_655 . . 7 ? C2 Mn C3 C3 -131.28(15) . . . 7 ? C3 C3 C2 Mn 54.55(10) 7 . . . ? C1 Mn C2 C3 -159.11(14) . . . . ? C3 Mn C2 C3 -30.67(13) 7 . . . ? C3 Mn C2 C3 41.7(3) 2_655 . . . ? C3 Mn C2 C3 72.38(18) 8_545 . . . ? C2 Mn C2 C3 110.76(14) 8_545 . . . ? C2 Mn C2 C3 -69.02(17) 7 . . . ? C2 Mn C2 C3 20.89(16) 2_655 . . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.227 _refine_diff_density_min -0.140 _refine_diff_density_rms 0.029