# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Rong Cao' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian, 350002, China ; #======================================================================== _publ_contact_author_email rcao@fjirsm.ac.cn _publ_contact_author_fax +86-591-83796710 _publ_contact_author_phone +86-591-83796710 _publ_contact_letter ; Dear Sir, Please consider this CIF submission for publication in CrystEngComm. All authors have seen and approved this submission. Best wishes Rong Cao ; loop_ _publ_author_name 'Rong Cao' 'Yun Gong' #===END data_1205 _database_code_depnum_ccdc_archive 'CCDC 805812' #TrackingRef '- 10031301.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H13 Mn O8' _chemical_formula_weight 328.12 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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4984(3) _cell_length_b 7.7273(2) _cell_length_c 15.4282(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.228(2) _cell_angle_gamma 90.00 _cell_volume 1241.66(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3320 _cell_measurement_theta_min 2.4950 _cell_measurement_theta_max 28.7473 _exptl_crystal_description lamellar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.84904 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Oxford XCalibur Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5287 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2192 _reflns_number_gt 1786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (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^)+(0.0655P)^2^+0.0546P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2192 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Mn1 Mn -0.12163(4) 0.20188(5) 0.30526(3) 0.02062(18) Uani 1 1 d . . . O3 O -0.0955(2) -0.2808(3) 0.44061(14) 0.0268(5) Uani 1 1 d . . . O2 O -0.1136(2) -0.0049(3) 0.40310(15) 0.0283(5) Uani 1 1 d . . . O1 O 0.08608(19) 0.1096(3) 0.30111(14) 0.0232(5) Uani 1 1 d . . . O5 O -0.16561(19) -0.0030(3) 0.21185(14) 0.0258(5) Uani 1 1 d . . . O7 O -0.0909(2) 0.3806(3) 0.20062(14) 0.0296(5) Uani 1 1 d . . . O8 O 0.6591(2) 0.7756(3) 0.47597(17) 0.0401(6) Uani 1 1 d . . . H8 H 0.7291 0.7418 0.4644 0.060 Uiso 1 1 calc R . . O6 O -0.0463(3) 0.3843(3) 0.40319(16) 0.0419(6) Uani 1 1 d . . . C7 C -0.0593(3) -0.1491(4) 0.4021(2) 0.0211(7) Uani 1 1 d . . . C6 C 0.2442(3) -0.0465(4) 0.2479(2) 0.0328(8) Uani 1 1 d . . . H6 H 0.3013 -0.0687 0.2079 0.039 Uiso 1 1 calc R . . C1 C 0.0588(3) -0.1667(4) 0.3534(2) 0.0227(7) Uani 1 1 d . . . H1 H 0.1071 -0.2713 0.3727 0.027 Uiso 1 1 calc R . . C3 C 0.1051(3) -0.0029(4) 0.2280(2) 0.0247(7) Uani 1 1 d . . . H3 H 0.0791 0.0461 0.1698 0.030 Uiso 1 1 calc R . . C10 C 0.5831(3) 0.6352(5) 0.4894(2) 0.0301(8) Uani 1 1 d . . . C4 C 0.1462(3) -0.0051(4) 0.3684(2) 0.0262(7) Uani 1 1 d . . . H4 H 0.1556 0.0420 0.4279 0.031 Uiso 1 1 calc R . . C9 C 0.4602(3) 0.6685(5) 0.5064(2) 0.0326(8) Uani 1 1 d . . . H9 H 0.4330 0.7822 0.5113 0.039 Uiso 1 1 calc R . . C11 C 0.6229(3) 0.4652(5) 0.4836(2) 0.0323(8) Uani 1 1 d . . . H11 H 0.7063 0.4414 0.4730 0.039 Uiso 1 1 calc R . . C5 C 0.2696(3) -0.0473(4) 0.3335(2) 0.0342(8) Uani 1 1 d . . . H5 H 0.3486 -0.0696 0.3661 0.041 Uiso 1 1 calc R . . O4 O -0.17467(19) -0.2867(3) 0.19860(15) 0.0255(5) Uani 1 1 d . . . C8 C -0.1144(3) -0.1491(4) 0.21794(19) 0.0208(7) Uani 1 1 d . . . C2 C 0.0285(3) -0.1649(4) 0.2511(2) 0.0218(7) Uani 1 1 d . . . H2 H 0.0638 -0.2688 0.2267 0.026 Uiso 1 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 0.0210(3) 0.0142(3) 0.0262(3) -0.0007(2) 0.00139(19) 0.00134(17) O3 0.0317(12) 0.0206(11) 0.0284(12) 0.0055(10) 0.0049(10) -0.0038(9) O2 0.0288(12) 0.0232(12) 0.0348(13) 0.0076(10) 0.0115(10) 0.0065(9) O1 0.0219(11) 0.0177(11) 0.0298(12) 0.0003(10) 0.0020(9) -0.0002(8) O5 0.0238(11) 0.0193(11) 0.0327(13) -0.0053(9) -0.0031(10) 0.0039(9) O7 0.0307(12) 0.0242(12) 0.0345(13) 0.0054(11) 0.0060(10) 0.0031(10) O8 0.0344(14) 0.0415(15) 0.0459(16) 0.0004(12) 0.0114(12) -0.0117(11) O6 0.0593(16) 0.0232(13) 0.0377(14) -0.0083(11) -0.0146(12) 0.0063(11) C7 0.0225(16) 0.0204(15) 0.0193(16) 0.0023(13) -0.0021(13) -0.0006(12) C6 0.0206(16) 0.0284(18) 0.052(2) -0.0009(16) 0.0138(16) -0.0022(13) C1 0.0174(15) 0.0184(15) 0.0322(18) 0.0045(13) 0.0021(13) 0.0036(11) C3 0.0247(17) 0.0223(16) 0.0279(17) -0.0015(14) 0.0064(13) -0.0012(12) C10 0.0291(18) 0.043(2) 0.0182(16) 0.0033(15) 0.0038(14) -0.0075(15) C4 0.0215(17) 0.0263(17) 0.0287(18) 0.0010(14) -0.0043(14) -0.0021(12) C9 0.0340(19) 0.040(2) 0.0236(18) 0.0007(15) 0.0053(15) 0.0017(15) C11 0.0255(18) 0.047(2) 0.0255(18) 0.0011(16) 0.0077(14) -0.0039(15) C5 0.0147(16) 0.0308(19) 0.056(2) 0.0045(17) -0.0002(16) -0.0010(13) O4 0.0200(11) 0.0176(11) 0.0381(13) -0.0031(10) 0.0008(9) -0.0062(9) C8 0.0212(15) 0.0226(16) 0.0190(15) -0.0010(13) 0.0045(13) 0.0005(12) C2 0.0192(15) 0.0177(15) 0.0293(17) -0.0039(13) 0.0063(13) 0.0009(11) _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 O4 2.134(2) 2_455 ? Mn1 O6 2.143(2) . ? Mn1 O5 2.152(2) . ? Mn1 O7 2.179(2) . ? Mn1 O2 2.193(2) . ? Mn1 O1 2.303(2) . ? O3 C7 1.261(4) . ? O2 C7 1.252(4) . ? O1 C4 1.449(4) . ? O1 C3 1.458(4) . ? O5 C8 1.249(3) . ? O8 C10 1.377(4) . ? O8 H8 0.8200 . ? C7 C1 1.534(4) . ? C6 C5 1.314(5) . ? C6 C3 1.493(4) . ? C6 H6 0.9300 . ? C1 C4 1.550(4) . ? C1 C2 1.571(5) . ? C1 H1 0.9800 . ? C3 C2 1.553(4) . ? C3 H3 0.9800 . ? C10 C9 1.374(5) . ? C10 C11 1.385(5) . ? C4 C5 1.500(4) . ? C4 H4 0.9800 . ? C9 C11 1.372(5) 3_666 ? C9 H9 0.9300 . ? C11 C9 1.372(5) 3_666 ? C11 H11 0.9300 . ? C5 H5 0.9300 . ? O4 C8 1.253(3) . ? O4 Mn1 2.134(2) 2_445 ? C8 C2 1.528(4) . ? C2 H2 0.9800 . ? 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 O4 Mn1 O6 105.79(9) 2_455 . ? O4 Mn1 O5 83.22(8) 2_455 . ? O6 Mn1 O5 170.07(9) . . ? O4 Mn1 O7 101.20(8) 2_455 . ? O6 Mn1 O7 91.71(9) . . ? O5 Mn1 O7 90.54(8) . . ? O4 Mn1 O2 90.06(8) 2_455 . ? O6 Mn1 O2 90.86(9) . . ? O5 Mn1 O2 84.90(9) . . ? O7 Mn1 O2 167.29(8) . . ? O4 Mn1 O1 164.01(7) 2_455 . ? O6 Mn1 O1 87.50(9) . . ? O5 Mn1 O1 82.96(7) . . ? O7 Mn1 O1 86.95(7) . . ? O2 Mn1 O1 80.72(7) . . ? C7 O2 Mn1 128.2(2) . . ? C4 O1 C3 95.8(2) . . ? C4 O1 Mn1 119.90(17) . . ? C3 O1 Mn1 115.37(17) . . ? C8 O5 Mn1 124.1(2) . . ? C10 O8 H8 109.5 . . ? O2 C7 O3 123.2(3) . . ? O2 C7 C1 118.8(3) . . ? O3 C7 C1 118.0(3) . . ? C5 C6 C3 106.1(3) . . ? C5 C6 H6 126.9 . . ? C3 C6 H6 126.9 . . ? C7 C1 C4 110.8(3) . . ? C7 C1 C2 114.7(2) . . ? C4 C1 C2 100.6(2) . . ? C7 C1 H1 110.1 . . ? C4 C1 H1 110.1 . . ? C2 C1 H1 110.1 . . ? O1 C3 C6 101.6(3) . . ? O1 C3 C2 100.2(2) . . ? C6 C3 C2 107.0(3) . . ? O1 C3 H3 115.4 . . ? C6 C3 H3 115.4 . . ? C2 C3 H3 115.4 . . ? C9 C10 O8 117.2(3) . . ? C9 C10 C11 119.2(3) . . ? O8 C10 C11 123.6(3) . . ? O1 C4 C5 101.2(3) . . ? O1 C4 C1 100.9(2) . . ? C5 C4 C1 107.1(3) . . ? O1 C4 H4 115.3 . . ? C5 C4 H4 115.3 . . ? C1 C4 H4 115.3 . . ? C11 C9 C10 120.4(3) 3_666 . ? C11 C9 H9 119.8 3_666 . ? C10 C9 H9 119.8 . . ? C9 C11 C10 120.4(3) 3_666 . ? C9 C11 H11 119.8 3_666 . ? C10 C11 H11 119.8 . . ? C6 C5 C4 106.5(3) . . ? C6 C5 H5 126.7 . . ? C4 C5 H5 126.7 . . ? C8 O4 Mn1 121.06(18) . 2_445 ? O5 C8 O4 123.3(3) . . ? O5 C8 C2 119.5(3) . . ? O4 C8 C2 117.2(3) . . ? C8 C2 C3 112.0(2) . . ? C8 C2 C1 113.8(2) . . ? C3 C2 C1 101.1(2) . . ? C8 C2 H2 109.9 . . ? C3 C2 H2 109.9 . . ? C1 C2 H2 109.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.607 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.074 #===END #===END data_1207 _database_code_depnum_ccdc_archive 'CCDC 805813' #TrackingRef '- 10031301.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H36 Mn2 O20' _chemical_formula_weight 730.24 _chemical_absolute_configuration 'C1,C3 S- and C2,C4 R-centers' 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 Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 17.3858(5) _cell_length_b 7.7932(3) _cell_length_c 10.8696(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.685(3) _cell_angle_gamma 90.00 _cell_volume 1469.69(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2482 _cell_measurement_theta_min 2.3430 _cell_measurement_theta_max 28.7473 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 0.946 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.90625 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Oxford XCalibur Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3266 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2155 _reflns_number_gt 1972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (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^)+(0.0668P)^2^+0.0000P] 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 none _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 0.04(3) _refine_ls_number_reflns 2155 _refine_ls_number_parameters 207 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Mn1 Mn 0.28590(3) 0.24961(8) 0.87413(5) 0.02171(18) Uani 1 1 d . . . O2 O 0.39654(16) 0.7279(5) 0.8579(3) 0.0344(7) Uani 1 1 d . . . O10 O 0.56023(16) 0.7468(7) 0.8889(3) 0.0477(7) Uani 1 1 d . . . O6 O 0.36688(19) 0.0667(4) 0.8072(3) 0.0385(9) Uani 1 1 d . . . O3 O 0.37316(18) 0.4496(4) 0.8633(3) 0.0313(8) Uani 1 1 d . . . C6 C 0.2629(3) 0.5005(8) 0.4987(5) 0.0342(13) Uani 1 1 d . . . H6 H 0.2827 0.5216 0.4227 0.041 Uiso 1 1 calc R . . O1 O 0.25343(16) 0.3459(4) 0.6773(2) 0.0233(6) Uani 1 1 d . . . O7 O 0.19241(17) 0.0691(4) 0.8370(3) 0.0328(7) Uani 1 1 d . . . O9 O 0.0269(2) 0.5913(6) 0.8248(4) 0.0605(11) Uani 1 1 d . . . C4 C 0.1887(2) 0.4614(5) 0.6600(4) 0.0243(9) Uani 1 1 d . . . H4 H 0.1398 0.4157 0.6859 0.029 Uiso 1 1 calc R . . C3 C 0.3078(2) 0.4555(5) 0.6199(3) 0.0245(9) Uani 1 1 d . . . H3 H 0.3588 0.4052 0.6113 0.029 Uiso 1 1 calc R . . C1 C 0.2193(2) 0.6208(5) 0.7333(3) 0.0209(8) Uani 1 1 d . . . H1 H 0.1947 0.7255 0.6999 0.025 Uiso 1 1 calc R . . C2 C 0.3066(2) 0.6161(5) 0.7042(4) 0.0223(8) Uani 1 1 d . . . H2 H 0.3196 0.7188 0.6578 0.027 Uiso 1 1 calc R . . O11 O 0.5000 0.3309(7) 0.0000 0.0707(19) Uani 1 2 d S . . C5 C 0.1893(3) 0.5031(6) 0.5255(4) 0.0330(11) Uani 1 1 d . . . H5 H 0.1468 0.5262 0.4717 0.040 Uiso 1 1 calc R . . C11 C 0.5111(5) 0.3187(13) 0.5581(8) 0.080(2) Uani 1 1 d . . . C7 C 0.3625(2) 0.5959(5) 0.8172(4) 0.0212(8) Uani 1 1 d . . . C9 C 0.5116(5) 0.6279(14) 0.5635(9) 0.115(4) Uani 1 1 d . . . H9 H 0.5192 0.7293 0.6078 0.138 Uiso 1 1 calc R . . C10 C 0.5231(4) 0.461(2) 0.6211(7) 0.106(4) Uani 1 1 d . . . H10 H 0.5393 0.4544 0.7042 0.128 Uiso 1 1 calc R . . O8 O 0.5122(6) 0.1456(13) 0.5865(8) 0.074(3) Uani 0.50 1 d P . . H8 H 0.5028 0.0896 0.5234 0.110 Uiso 0.50 1 calc PR . . O4 O 0.20912(17) 0.4598(4) 0.9188(3) 0.0282(7) Uani 1 1 d . . . C8 C 0.2069(2) 0.6037(5) 0.8700(3) 0.0199(8) Uani 1 1 d . . . O5 O 0.19518(15) 0.7406(5) 0.9289(2) 0.0275(6) Uani 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 Mn1 0.0270(3) 0.0163(3) 0.0215(3) 0.0003(3) -0.00088(19) 0.0002(3) O2 0.0327(14) 0.0252(19) 0.0439(16) -0.0009(17) -0.0099(12) -0.0043(16) O10 0.0342(15) 0.0533(19) 0.0549(18) -0.001(3) -0.0037(13) 0.000(2) O6 0.0383(19) 0.0279(18) 0.050(2) -0.0019(17) 0.0060(16) 0.0071(14) O3 0.0293(16) 0.0291(18) 0.0339(18) 0.0089(16) -0.0107(13) -0.0083(13) C6 0.060(4) 0.025(2) 0.0174(19) 0.0010(16) 0.003(2) 0.000(2) O1 0.0333(16) 0.0167(14) 0.0199(14) 0.0006(12) 0.0013(12) 0.0012(12) O7 0.0321(17) 0.0271(17) 0.0382(18) 0.0030(15) -0.0054(13) -0.0057(13) O9 0.046(2) 0.062(3) 0.073(3) 0.003(2) -0.0013(18) -0.0012(19) C4 0.026(2) 0.024(2) 0.022(2) -0.0040(18) -0.0067(16) 0.0013(17) C3 0.032(2) 0.022(2) 0.020(2) 0.0016(18) 0.0030(17) 0.0009(18) C1 0.025(2) 0.017(2) 0.0200(19) -0.0002(16) -0.0042(15) 0.0027(16) C2 0.029(2) 0.016(2) 0.022(2) 0.0049(17) 0.0008(16) -0.0031(16) O11 0.056(4) 0.040(3) 0.112(5) 0.000 -0.033(3) 0.000 C5 0.045(3) 0.026(3) 0.026(2) -0.0040(19) -0.014(2) 0.002(2) C11 0.052(4) 0.117(7) 0.073(4) 0.012(5) 0.022(4) 0.003(4) C7 0.0197(18) 0.019(2) 0.026(2) -0.0001(18) 0.0052(15) -0.0018(16) C9 0.085(7) 0.118(8) 0.145(9) -0.065(7) 0.038(7) -0.032(6) C10 0.050(4) 0.206(12) 0.062(5) -0.026(7) -0.006(3) -0.015(6) O8 0.096(8) 0.065(7) 0.061(6) 0.007(5) 0.017(5) -0.004(6) O4 0.0376(17) 0.0232(17) 0.0244(16) 0.0027(14) 0.0078(13) 0.0060(12) C8 0.0191(17) 0.019(2) 0.021(2) -0.0004(18) -0.0033(14) 0.0020(15) O5 0.0387(13) 0.0187(14) 0.0248(13) -0.0056(18) -0.0007(10) 0.0051(17) _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 O5 2.146(2) 4_547 ? Mn1 O6 2.162(3) . ? Mn1 O7 2.168(3) . ? Mn1 O3 2.183(3) . ? Mn1 O4 2.187(3) . ? Mn1 O1 2.303(3) . ? O2 C7 1.253(5) . ? O3 C7 1.255(5) . ? C6 C5 1.330(8) . ? C6 C3 1.528(6) . ? C6 H6 0.9300 . ? O1 C4 1.444(5) . ? O1 C3 1.445(5) . ? C4 C5 1.498(6) . ? C4 C1 1.551(5) . ? C4 H4 0.9800 . ? C3 C2 1.552(6) . ? C3 H3 0.9800 . ? C1 C8 1.521(5) . ? C1 C2 1.571(5) . ? C1 H1 0.9800 . ? C2 C7 1.524(5) . ? C2 H2 0.9800 . ? C5 H5 0.9300 . ? C11 C11 1.296(17) 2_656 ? C11 C10 1.311(14) . ? C11 O8 1.383(11) . ? C9 C9 1.41(2) 2_656 ? C9 C10 1.454(14) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? O8 H8 0.8200 . ? O4 C8 1.240(5) . ? C8 O5 1.268(6) . ? O5 Mn1 2.146(2) 4_557 ? 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 O5 Mn1 O6 104.63(14) 4_547 . ? O5 Mn1 O7 103.28(12) 4_547 . ? O6 Mn1 O7 90.36(13) . . ? O5 Mn1 O3 90.82(12) 4_547 . ? O6 Mn1 O3 89.01(12) . . ? O7 Mn1 O3 165.57(11) . . ? O5 Mn1 O4 81.93(13) 4_547 . ? O6 Mn1 O4 171.22(13) . . ? O7 Mn1 O4 93.81(12) . . ? O3 Mn1 O4 85.03(13) . . ? O5 Mn1 O1 161.82(13) 4_547 . ? O6 Mn1 O1 91.62(11) . . ? O7 Mn1 O1 84.39(11) . . ? O3 Mn1 O1 81.22(10) . . ? O4 Mn1 O1 81.11(10) . . ? C7 O3 Mn1 125.8(3) . . ? C5 C6 C3 105.1(4) . . ? C5 C6 H6 127.5 . . ? C3 C6 H6 127.5 . . ? C4 O1 C3 95.8(3) . . ? C4 O1 Mn1 117.8(2) . . ? C3 O1 Mn1 117.8(2) . . ? O1 C4 C5 102.0(3) . . ? O1 C4 C1 101.2(3) . . ? C5 C4 C1 107.7(4) . . ? O1 C4 H4 114.8 . . ? C5 C4 H4 114.8 . . ? C1 C4 H4 114.8 . . ? O1 C3 C6 101.3(3) . . ? O1 C3 C2 100.8(3) . . ? C6 C3 C2 107.4(4) . . ? O1 C3 H3 115.2 . . ? C6 C3 H3 115.2 . . ? C2 C3 H3 115.2 . . ? C8 C1 C4 111.5(3) . . ? C8 C1 C2 113.2(3) . . ? C4 C1 C2 100.5(3) . . ? C8 C1 H1 110.4 . . ? C4 C1 H1 110.4 . . ? C2 C1 H1 110.4 . . ? C7 C2 C3 111.1(3) . . ? C7 C2 C1 114.5(3) . . ? C3 C2 C1 100.8(3) . . ? C7 C2 H2 110.0 . . ? C3 C2 H2 110.0 . . ? C1 C2 H2 110.0 . . ? C6 C5 C4 106.1(4) . . ? C6 C5 H5 126.9 . . ? C4 C5 H5 126.9 . . ? C11 C11 C10 122.4(7) 2_656 . ? C11 C11 O8 102.5(6) 2_656 . ? C10 C11 O8 135.0(11) . . ? O2 C7 O3 123.4(4) . . ? O2 C7 C2 117.5(3) . . ? O3 C7 C2 119.1(3) . . ? C9 C9 C10 116.3(6) 2_656 . ? C9 C9 H9 121.8 2_656 . ? C10 C9 H9 121.8 . . ? C11 C10 C9 121.3(9) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C11 O8 H8 109.5 . . ? C8 O4 Mn1 125.8(3) . . ? O4 C8 O5 123.1(4) . . ? O4 C8 C1 119.7(4) . . ? O5 C8 C1 117.2(4) . . ? C8 O5 Mn1 120.8(3) . 4_557 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.401 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.077 #======================================================================== data_10031301 _database_code_depnum_ccdc_archive 'CCDC 805814' #TrackingRef '- 10031301.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H10 Mn O7' _chemical_formula_weight 273.07 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.862(4) _cell_length_b 6.2531(18) _cell_length_c 10.122(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.938(4) _cell_angle_gamma 90.00 _cell_volume 940.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2539 _cell_measurement_theta_min 3.3747 _cell_measurement_theta_max 27.4680 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 1.422 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6397 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Oxford XCalibur Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6937 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2152 _reflns_number_gt 1974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (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^)+(0.0478P)^2^+0.6897P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2152 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Mn1 Mn 0.191178(19) 1.06230(5) 0.00453(3) 0.01526(12) Uani 1 1 d . . . O1 O 0.32683(10) 0.8882(2) 0.03470(13) 0.0168(3) Uani 1 1 d . . . O2 O 0.23737(11) 1.2321(2) 0.18358(14) 0.0252(4) Uani 1 1 d . . . C6 C 0.46612(14) 0.8177(4) 0.1254(2) 0.0224(4) Uani 1 1 d . . . H6 H 0.5276 0.8420 0.1354 0.027 Uiso 1 1 calc R . . O3 O 0.07037(12) 1.2450(3) -0.00233(18) 0.0371(4) Uani 1 1 d . . . C4 C 0.32512(13) 0.6783(3) 0.09816(19) 0.0165(4) Uani 1 1 d . . . H4 H 0.2885 0.5696 0.0529 0.020 Uiso 1 1 calc R . . C3 C 0.39168(13) 0.9829(3) 0.1254(2) 0.0179(4) Uani 1 1 d . . . H3 H 0.4105 1.1283 0.1028 0.021 Uiso 1 1 calc R . . C5 C 0.42511(15) 0.6305(4) 0.1083(2) 0.0221(4) Uani 1 1 d . . . H5 H 0.4523 0.4968 0.1035 0.027 Uiso 1 1 calc R . . O7 O 0.00000(11) 0.4924(3) 0.20030(17) 0.0282(4) Uani 1 1 d . . . C2 C 0.34154(13) 0.9622(3) 0.25897(19) 0.0154(4) Uani 1 1 d . . . H2 H 0.3855 0.9540 0.3320 0.018 Uiso 1 1 calc R . . C1 C 0.29480(13) 0.7384(3) 0.23965(18) 0.0140(4) Uani 1 1 d . . . H1 H 0.3197 0.6359 0.3036 0.017 Uiso 1 1 calc R . . O6 O 0.14791(10) 0.8313(3) 0.15609(15) 0.0220(3) Uani 1 1 d . . . O4 O 0.27492(12) 1.2206(2) 0.39720(15) 0.0269(4) Uani 1 1 d . . . C7 C 0.27833(13) 1.1524(3) 0.28060(19) 0.0160(4) Uani 1 1 d . . . O5 O 0.15546(9) 0.6511(2) 0.34389(14) 0.0193(3) Uani 1 1 d . . . C8 C 0.19235(12) 0.7407(3) 0.24746(18) 0.0143(4) Uani 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 Mn1 0.01943(18) 0.01564(18) 0.01069(17) 0.00102(10) -0.00082(12) 0.00057(11) O1 0.0218(7) 0.0177(7) 0.0107(6) 0.0002(5) -0.0005(5) -0.0003(6) O2 0.0393(9) 0.0207(7) 0.0154(7) -0.0027(6) -0.0058(6) 0.0091(6) C6 0.0164(9) 0.0323(11) 0.0187(10) -0.0018(9) 0.0039(8) 0.0011(8) O3 0.0388(10) 0.0413(10) 0.0311(9) -0.0011(8) -0.0028(8) 0.0212(8) C4 0.0211(9) 0.0139(9) 0.0145(9) -0.0018(7) 0.0002(7) 0.0006(7) C3 0.0191(9) 0.0189(9) 0.0157(9) -0.0019(7) 0.0027(7) -0.0038(8) C5 0.0240(10) 0.0250(10) 0.0175(10) -0.0006(8) 0.0049(8) 0.0087(9) O7 0.0247(8) 0.0308(8) 0.0290(9) 0.0004(7) -0.0005(7) -0.0046(7) C2 0.0164(9) 0.0180(9) 0.0117(9) -0.0022(7) 0.0001(7) -0.0002(7) C1 0.0164(9) 0.0141(8) 0.0116(9) 0.0014(7) 0.0010(7) 0.0012(7) O6 0.0176(7) 0.0289(8) 0.0195(7) 0.0102(6) -0.0012(6) 0.0002(6) O4 0.0416(9) 0.0248(8) 0.0142(7) -0.0050(6) -0.0013(7) 0.0123(7) C7 0.0194(9) 0.0143(9) 0.0143(9) -0.0013(7) 0.0002(7) -0.0021(7) O5 0.0182(7) 0.0233(7) 0.0165(7) 0.0071(6) 0.0022(5) 0.0010(6) C8 0.0162(9) 0.0128(8) 0.0141(9) 0.0001(7) 0.0007(7) -0.0001(7) _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 O3 2.1283(17) . ? Mn1 O4 2.1485(16) 4_585 ? Mn1 O5 2.1628(15) 4_575 ? Mn1 O2 2.2007(15) . ? Mn1 O6 2.2105(15) . ? Mn1 O1 2.3071(15) . ? O1 C3 1.447(2) . ? O1 C4 1.462(2) . ? O2 C7 1.251(2) . ? C6 C5 1.330(3) . ? C6 C3 1.514(3) . ? C6 H6 0.9300 . ? C4 C5 1.518(3) . ? C4 C1 1.555(3) . ? C4 H4 0.9800 . ? C3 C2 1.560(3) . ? C3 H3 0.9800 . ? C5 H5 0.9300 . ? C2 C7 1.534(3) . ? C2 C1 1.573(3) . ? C2 H2 0.9800 . ? C1 C8 1.526(3) . ? C1 H1 0.9800 . ? O6 C8 1.262(2) . ? O4 C7 1.257(2) . ? O4 Mn1 2.1485(16) 4_586 ? O5 C8 1.259(2) . ? O5 Mn1 2.1628(15) 4_576 ? 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 O3 Mn1 O4 98.03(7) . 4_585 ? O3 Mn1 O5 96.32(7) . 4_575 ? O4 Mn1 O5 98.44(6) 4_585 4_575 ? O3 Mn1 O2 91.11(6) . . ? O4 Mn1 O2 86.33(6) 4_585 . ? O5 Mn1 O2 170.49(6) 4_575 . ? O3 Mn1 O6 96.81(7) . . ? O4 Mn1 O6 160.28(6) 4_585 . ? O5 Mn1 O6 92.75(6) 4_575 . ? O2 Mn1 O6 80.45(6) . . ? O3 Mn1 O1 172.98(6) . . ? O4 Mn1 O1 81.54(6) 4_585 . ? O5 Mn1 O1 90.67(5) 4_575 . ? O2 Mn1 O1 81.87(5) . . ? O6 Mn1 O1 82.15(5) . . ? C3 O1 C4 96.01(14) . . ? C3 O1 Mn1 117.56(12) . . ? C4 O1 Mn1 117.41(11) . . ? C7 O2 Mn1 126.55(13) . . ? C5 C6 C3 105.49(18) . . ? C5 C6 H6 127.3 . . ? C3 C6 H6 127.3 . . ? O1 C4 C5 100.52(16) . . ? O1 C4 C1 101.26(14) . . ? C5 C4 C1 106.48(15) . . ? O1 C4 H4 115.5 . . ? C5 C4 H4 115.5 . . ? C1 C4 H4 115.5 . . ? O1 C3 C6 101.57(16) . . ? O1 C3 C2 101.14(15) . . ? C6 C3 C2 107.60(17) . . ? O1 C3 H3 114.9 . . ? C6 C3 H3 114.9 . . ? C2 C3 H3 114.9 . . ? C6 C5 C4 106.36(18) . . ? C6 C5 H5 126.8 . . ? C4 C5 H5 126.8 . . ? C7 C2 C3 111.21(16) . . ? C7 C2 C1 115.94(16) . . ? C3 C2 C1 100.51(15) . . ? C7 C2 H2 109.6 . . ? C3 C2 H2 109.6 . . ? C1 C2 H2 109.6 . . ? C8 C1 C4 110.76(15) . . ? C8 C1 C2 115.10(15) . . ? C4 C1 C2 101.27(14) . . ? C8 C1 H1 109.8 . . ? C4 C1 H1 109.8 . . ? C2 C1 H1 109.8 . . ? C8 O6 Mn1 130.33(13) . . ? C7 O4 Mn1 136.22(14) . 4_586 ? O2 C7 O4 125.13(19) . . ? O2 C7 C2 119.24(17) . . ? O4 C7 C2 115.57(17) . . ? C8 O5 Mn1 138.84(13) . 4_576 ? O5 C8 O6 122.59(17) . . ? O5 C8 C1 118.92(16) . . ? O6 C8 C1 118.49(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.746 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.075