# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_walter_temp _database_code_depnum_ccdc_archive 'CCDC 743654' #TrackingRef 'walter_temp.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H74 I2 Mn2 O2' _chemical_formula_sum 'C42 H74 I2 Mn2 O2' _chemical_formula_weight 974.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 '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 9.2320(4) _cell_length_b 9.9138(4) _cell_length_c 13.3547(5) _cell_angle_alpha 105.125(2) _cell_angle_beta 102.783(2) _cell_angle_gamma 100.418(2) _cell_volume 1113.13(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3677 _cell_measurement_theta_min 3.57 _cell_measurement_theta_max 65.40 _exptl_crystal_description block _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 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 498 _exptl_absorpt_coefficient_mu 15.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3023 _exptl_absorpt_correction_T_max 0.5069 _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15296 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 71.87 _reflns_number_total 4115 _reflns_number_gt 3895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The THF ring is disordered; all carbons were refined isotropically on two alternative sets of sites. Appropriate restraints were employed to improve refinement stability. ; _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^)+(0.0327P)^2^+2.3564P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4115 _refine_ls_number_parameters 223 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.074 _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 I1 I 0.35823(3) 0.60930(2) 0.444386(16) 0.02460(8) Uani 1 1 d . . . Mn1 Mn 0.51430(6) 0.41385(5) 0.34632(4) 0.01522(11) Uani 1 1 d . . . C1 C 0.5214(4) 0.2018(3) 0.2053(2) 0.0171(6) Uani 1 1 d . . . C2 C 0.3891(4) 0.1622(3) 0.2428(2) 0.0162(6) Uani 1 1 d . . . C3 C 0.2863(4) 0.2463(3) 0.2122(2) 0.0172(6) Uani 1 1 d . . . H3 H 0.1899 0.2427 0.2271 0.021 Uiso 1 1 calc R . . C4 C 0.3477(4) 0.3349(3) 0.1570(2) 0.0162(6) Uani 1 1 d . . . C5 C 0.4926(4) 0.3090(3) 0.1545(2) 0.0161(6) Uani 1 1 d . . . H5 H 0.5614 0.3560 0.1235 0.019 Uiso 1 1 calc R . . C11 C 0.6662(4) 0.1447(4) 0.2047(3) 0.0228(7) Uani 1 1 d . . . C12 C 0.6242(5) -0.0168(4) 0.1398(3) 0.0340(9) Uani 1 1 d . . . H12A H 0.5703 -0.0310 0.0644 0.051 Uiso 1 1 calc R . . H12B H 0.5575 -0.0718 0.1710 0.051 Uiso 1 1 calc R . . H12C H 0.7181 -0.0505 0.1427 0.051 Uiso 1 1 calc R . . C13 C 0.7695(4) 0.1705(4) 0.3192(3) 0.0275(8) Uani 1 1 d . . . H13A H 0.7118 0.1208 0.3582 0.041 Uiso 1 1 calc R . . H13B H 0.8030 0.2743 0.3582 0.041 Uiso 1 1 calc R . . H13C H 0.8596 0.1328 0.3139 0.041 Uiso 1 1 calc R . . C14 C 0.7675(5) 0.2235(5) 0.1493(3) 0.0368(9) Uani 1 1 d . . . H14A H 0.8596 0.1872 0.1507 0.055 Uiso 1 1 calc R . . H14B H 0.7976 0.3274 0.1879 0.055 Uiso 1 1 calc R . . H14C H 0.7097 0.2060 0.0742 0.055 Uiso 1 1 calc R . . C21 C 0.3285(4) 0.0386(3) 0.2853(3) 0.0246(7) Uani 1 1 d . . . C22 C 0.2257(5) -0.0888(4) 0.1862(3) 0.0356(9) Uani 1 1 d . . . H22A H 0.2869 -0.1210 0.1377 0.053 Uiso 1 1 calc R . . H22B H 0.1414 -0.0574 0.1477 0.053 Uiso 1 1 calc R . . H22C H 0.1836 -0.1687 0.2104 0.053 Uiso 1 1 calc R . . C23 C 0.2286(5) 0.0860(4) 0.3594(3) 0.0354(9) Uani 1 1 d . . . H23A H 0.1937 0.0078 0.3875 0.053 Uiso 1 1 calc R . . H23B H 0.1394 0.1083 0.3181 0.053 Uiso 1 1 calc R . . H23C H 0.2891 0.1721 0.4198 0.053 Uiso 1 1 calc R . . C24 C 0.4494(5) -0.0162(4) 0.3513(3) 0.0332(9) Uani 1 1 d . . . H24A H 0.5157 -0.0504 0.3076 0.050 Uiso 1 1 calc R . . H24B H 0.3981 -0.0957 0.3721 0.050 Uiso 1 1 calc R . . H24C H 0.5117 0.0627 0.4165 0.050 Uiso 1 1 calc R . . C41 C 0.2621(4) 0.4198(4) 0.0943(3) 0.0211(7) Uani 1 1 d . . . C42 C 0.2123(5) 0.3301(4) -0.0270(3) 0.0334(9) Uani 1 1 d . . . H42A H 0.3034 0.3155 -0.0503 0.050 Uiso 1 1 calc R . . H42B H 0.1578 0.3818 -0.0697 0.050 Uiso 1 1 calc R . . H42C H 0.1443 0.2362 -0.0379 0.050 Uiso 1 1 calc R . . C43 C 0.1207(5) 0.4437(5) 0.1296(3) 0.0365(9) Uani 1 1 d . . . H43A H 0.0481 0.3502 0.1130 0.055 Uiso 1 1 calc R . . H43B H 0.0720 0.5026 0.0909 0.055 Uiso 1 1 calc R . . H43C H 0.1509 0.4936 0.2076 0.055 Uiso 1 1 calc R . . C44 C 0.3640(5) 0.5664(4) 0.1075(3) 0.0321(8) Uani 1 1 d . . . H44A H 0.3913 0.6277 0.1829 0.048 Uiso 1 1 calc R . . H44B H 0.3085 0.6127 0.0605 0.048 Uiso 1 1 calc R . . H44C H 0.4576 0.5531 0.0876 0.048 Uiso 1 1 calc R . . O1 O 0.7211(3) 0.5814(3) 0.36399(19) 0.0257(5) Uani 1 1 d D . . C61 C 0.7174(10) 0.6739(10) 0.2977(8) 0.042(2) Uiso 0.579(11) 1 d PDU A 1 H61A H 0.6210 0.7058 0.2885 0.050 Uiso 0.579(11) 1 calc PR A 1 H61B H 0.7265 0.6243 0.2256 0.050 Uiso 0.579(11) 1 calc PR A 1 C62 C 0.8624(7) 0.8075(7) 0.3629(5) 0.0286(17) Uiso 0.579(11) 1 d PDU A 1 H62A H 0.8914 0.8678 0.3184 0.034 Uiso 0.579(11) 1 calc PR A 1 H62B H 0.8502 0.8681 0.4307 0.034 Uiso 0.579(11) 1 calc PR A 1 C63 C 0.9681(8) 0.7127(8) 0.3816(6) 0.0349(19) Uiso 0.579(11) 1 d PDU A 1 H63A H 1.0717 0.7694 0.4287 0.042 Uiso 0.579(11) 1 calc PR A 1 H63B H 0.9767 0.6509 0.3129 0.042 Uiso 0.579(11) 1 calc PR A 1 C64 C 0.8761(7) 0.6199(8) 0.4416(6) 0.0236(17) Uiso 0.579(11) 1 d PDU A 1 H64A H 0.9138 0.5336 0.4458 0.028 Uiso 0.579(11) 1 calc PR A 1 H64B H 0.8795 0.6789 0.5148 0.028 Uiso 0.579(11) 1 calc PR A 1 C61' C 0.7070(8) 0.7106(9) 0.3274(7) 0.0144(19) Uiso 0.421(11) 1 d PDU A 2 H61C H 0.6874 0.7889 0.3819 0.017 Uiso 0.421(11) 1 calc PR A 2 H61D H 0.6294 0.6858 0.2567 0.017 Uiso 0.421(11) 1 calc PR A 2 C62' C 0.8902(11) 0.7475(12) 0.3189(8) 0.040(3) Uiso 0.421(11) 1 d PDU A 2 H62C H 0.9114 0.6671 0.2672 0.048 Uiso 0.421(11) 1 calc PR A 2 H62D H 0.9195 0.8387 0.3024 0.048 Uiso 0.421(11) 1 calc PR A 2 C63' C 0.9596(10) 0.7604(9) 0.4330(7) 0.026(2) Uiso 0.421(11) 1 d PDU A 2 H63C H 0.9231 0.8276 0.4849 0.031 Uiso 0.421(11) 1 calc PR A 2 H63D H 1.0732 0.7840 0.4540 0.031 Uiso 0.421(11) 1 calc PR A 2 C64' C 0.8818(10) 0.5949(11) 0.4116(11) 0.032(3) Uiso 0.421(11) 1 d PDU A 2 H64C H 0.9236 0.5312 0.3613 0.039 Uiso 0.421(11) 1 calc PR A 2 H64D H 0.8977 0.5708 0.4800 0.039 Uiso 0.421(11) 1 calc PR A 2 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 I1 0.03853(15) 0.02239(12) 0.01622(11) 0.00572(8) 0.00790(8) 0.01618(9) Mn1 0.0187(3) 0.0128(2) 0.0137(2) 0.00398(18) 0.00445(18) 0.00319(18) C1 0.0193(17) 0.0181(15) 0.0138(14) 0.0031(12) 0.0041(12) 0.0080(12) C2 0.0200(17) 0.0114(14) 0.0142(14) 0.0010(11) 0.0042(12) 0.0017(11) C3 0.0135(16) 0.0155(14) 0.0188(15) 0.0007(12) 0.0043(12) 0.0015(11) C4 0.0184(16) 0.0150(14) 0.0124(13) 0.0014(11) 0.0017(11) 0.0054(12) C5 0.0179(16) 0.0180(15) 0.0138(14) 0.0056(12) 0.0052(11) 0.0062(12) C11 0.0245(19) 0.0288(18) 0.0199(16) 0.0075(13) 0.0081(13) 0.0163(14) C12 0.043(2) 0.035(2) 0.0231(17) 0.0019(15) 0.0037(16) 0.0256(18) C13 0.0235(19) 0.0341(19) 0.0248(17) 0.0077(15) 0.0024(14) 0.0148(15) C14 0.027(2) 0.059(3) 0.042(2) 0.025(2) 0.0199(17) 0.0249(19) C21 0.033(2) 0.0149(15) 0.0251(17) 0.0078(13) 0.0096(15) -0.0003(13) C22 0.044(2) 0.0169(17) 0.036(2) 0.0074(15) 0.0030(18) -0.0046(15) C23 0.040(2) 0.032(2) 0.040(2) 0.0166(17) 0.0211(18) 0.0022(17) C24 0.049(3) 0.0220(17) 0.0292(19) 0.0145(15) 0.0085(17) 0.0051(16) C41 0.0245(18) 0.0223(16) 0.0170(15) 0.0064(13) 0.0016(13) 0.0115(13) C42 0.040(2) 0.034(2) 0.0201(17) 0.0026(15) -0.0041(15) 0.0182(17) C43 0.035(2) 0.050(2) 0.036(2) 0.0196(18) 0.0102(17) 0.0275(19) C44 0.041(2) 0.0274(19) 0.033(2) 0.0175(16) 0.0079(17) 0.0144(16) O1 0.0236(13) 0.0248(12) 0.0261(12) 0.0111(10) 0.0030(10) -0.0001(10) _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 I1 Mn1 2.8401(5) . ? I1 Mn1 2.8682(5) 2_666 ? Mn1 O1 2.216(2) . ? Mn1 C3 2.432(3) . ? Mn1 C2 2.433(3) . ? Mn1 C5 2.448(3) . ? Mn1 C1 2.451(3) . ? Mn1 C4 2.487(3) . ? Mn1 I1 2.8683(5) 2_666 ? C1 C5 1.435(4) . ? C1 C2 1.448(5) . ? C1 C11 1.544(4) . ? C2 C3 1.434(4) . ? C2 C21 1.546(4) . ? C3 C4 1.407(5) . ? C3 H3 0.9500 . ? C4 C5 1.413(5) . ? C4 C41 1.533(4) . ? C5 H5 0.9500 . ? C11 C12 1.539(5) . ? C11 C13 1.541(5) . ? C11 C14 1.541(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 C24 1.533(5) . ? C21 C23 1.540(5) . ? C21 C22 1.544(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C41 C43 1.519(5) . ? C41 C44 1.525(5) . ? C41 C42 1.549(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? O1 C61 1.430(7) . ? O1 C64' 1.446(9) . ? O1 C64 1.486(6) . ? O1 C61' 1.502(7) . ? C61 C62 1.595(9) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.498(9) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.617(8) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C61' C62' 1.700(10) . ? C61' H61C 0.9900 . ? C61' H61D 0.9900 . ? C62' C63' 1.479(11) . ? C62' H62C 0.9900 . ? C62' H62D 0.9900 . ? C63' C64' 1.590(10) . ? C63' H63C 0.9900 . ? C63' H63D 0.9900 . ? C64' H64C 0.9900 . ? C64' H64D 0.9900 . ? 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 Mn1 I1 Mn1 91.853(14) . 2_666 ? O1 Mn1 C3 142.08(10) . . ? O1 Mn1 C2 139.06(10) . . ? C3 Mn1 C2 34.27(10) . . ? O1 Mn1 C5 90.29(10) . . ? C3 Mn1 C5 55.03(11) . . ? C2 Mn1 C5 56.38(10) . . ? O1 Mn1 C1 104.59(10) . . ? C3 Mn1 C1 56.42(11) . . ? C2 Mn1 C1 34.49(11) . . ? C5 Mn1 C1 34.08(10) . . ? O1 Mn1 C4 109.16(10) . . ? C3 Mn1 C4 33.23(11) . . ? C2 Mn1 C4 56.70(10) . . ? C5 Mn1 C4 33.26(10) . . ? C1 Mn1 C4 56.60(10) . . ? O1 Mn1 I1 95.69(7) . . ? C3 Mn1 I1 95.94(8) . . ? C2 Mn1 I1 123.13(8) . . ? C5 Mn1 I1 129.15(7) . . ? C1 Mn1 I1 152.12(8) . . ? C4 Mn1 I1 98.89(7) . . ? O1 Mn1 I1 91.70(6) . 2_666 ? C3 Mn1 I1 124.63(8) . 2_666 ? C2 Mn1 I1 101.20(7) . 2_666 ? C5 Mn1 I1 142.23(7) . 2_666 ? C1 Mn1 I1 109.82(7) . 2_666 ? C4 Mn1 I1 157.03(7) . 2_666 ? I1 Mn1 I1 88.146(14) . 2_666 ? C5 C1 C2 106.2(3) . . ? C5 C1 C11 120.7(3) . . ? C2 C1 C11 132.9(3) . . ? C5 C1 Mn1 72.83(17) . . ? C2 C1 Mn1 72.09(17) . . ? C11 C1 Mn1 123.4(2) . . ? C3 C2 C1 106.4(3) . . ? C3 C2 C21 117.8(3) . . ? C1 C2 C21 134.6(3) . . ? C3 C2 Mn1 72.80(17) . . ? C1 C2 Mn1 73.42(17) . . ? C21 C2 Mn1 127.9(2) . . ? C4 C3 C2 110.7(3) . . ? C4 C3 Mn1 75.52(18) . . ? C2 C3 Mn1 72.92(17) . . ? C4 C3 H3 124.7 . . ? C2 C3 H3 124.7 . . ? Mn1 C3 H3 118.5 . . ? C3 C4 C5 106.1(3) . . ? C3 C4 C41 126.3(3) . . ? C5 C4 C41 126.6(3) . . ? C3 C4 Mn1 71.25(17) . . ? C5 C4 Mn1 71.86(17) . . ? C41 C4 Mn1 130.1(2) . . ? C4 C5 C1 110.6(3) . . ? C4 C5 Mn1 74.88(17) . . ? C1 C5 Mn1 73.09(17) . . ? C4 C5 H5 124.7 . . ? C1 C5 H5 124.7 . . ? Mn1 C5 H5 119.0 . . ? C12 C11 C13 109.7(3) . . ? C12 C11 C14 106.2(3) . . ? C13 C11 C14 105.6(3) . . ? C12 C11 C1 111.4(3) . . ? C13 C11 C1 113.0(3) . . ? C14 C11 C1 110.5(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C21 C23 105.5(3) . . ? C24 C21 C22 108.8(3) . . ? C23 C21 C22 107.9(3) . . ? C24 C21 C2 116.7(3) . . ? C23 C21 C2 110.4(3) . . ? C22 C21 C2 107.3(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C43 C41 C44 108.5(3) . . ? C43 C41 C4 111.6(3) . . ? C44 C41 C4 112.1(3) . . ? C43 C41 C42 109.2(3) . . ? C44 C41 C42 108.0(3) . . ? C4 C41 C42 107.3(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C61 O1 C64' 105.8(5) . . ? C61 O1 C64 109.9(4) . . ? C64' O1 C64 16.9(5) . . ? C61 O1 C61' 19.5(4) . . ? C64' O1 C61' 108.6(5) . . ? C64 O1 C61' 106.7(4) . . ? C61 O1 Mn1 121.3(3) . . ? C64' O1 Mn1 130.5(4) . . ? C64 O1 Mn1 128.8(3) . . ? C61' O1 Mn1 120.9(3) . . ? O1 C61 C62 103.9(5) . . ? O1 C61 H61A 111.0 . . ? C62 C61 H61A 111.0 . . ? O1 C61 H61B 111.0 . . ? C62 C61 H61B 111.0 . . ? H61A C61 H61B 109.0 . . ? C63 C62 C61 93.3(6) . . ? C63 C62 H62A 113.0 . . ? C61 C62 H62A 113.0 . . ? C63 C62 H62B 113.0 . . ? C61 C62 H62B 113.0 . . ? H62A C62 H62B 110.4 . . ? C62 C63 C64 99.1(5) . . ? C62 C63 H63A 111.9 . . ? C64 C63 H63A 111.9 . . ? C62 C63 H63B 111.9 . . ? C64 C63 H63B 111.9 . . ? H63A C63 H63B 109.6 . . ? O1 C64 C63 97.9(4) . . ? O1 C64 H64A 112.2 . . ? C63 C64 H64A 112.2 . . ? O1 C64 H64B 112.2 . . ? C63 C64 H64B 112.2 . . ? H64A C64 H64B 109.8 . . ? O1 C61' C62' 94.1(5) . . ? O1 C61' H61C 112.9 . . ? C62' C61' H61C 112.9 . . ? O1 C61' H61D 112.9 . . ? C62' C61' H61D 112.9 . . ? H61C C61' H61D 110.3 . . ? C63' C62' C61' 94.1(7) . . ? C63' C62' H62C 112.9 . . ? C61' C62' H62C 112.9 . . ? C63' C62' H62D 112.9 . . ? C61' C62' H62D 112.9 . . ? H62C C62' H62D 110.3 . . ? C62' C63' C64' 91.1(7) . . ? C62' C63' H63C 113.4 . . ? C64' C63' H63C 113.4 . . ? C62' C63' H63D 113.4 . . ? C64' C63' H63D 113.4 . . ? H63C C63' H63D 110.7 . . ? O1 C64' C63' 103.4(6) . . ? O1 C64' H64C 111.1 . . ? C63' C64' H64C 111.1 . . ? O1 C64' H64D 111.1 . . ? C63' C64' H64D 111.1 . . ? H64C C64' H64D 109.1 . . ? 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 Mn1 I1 Mn1 O1 -91.53(6) 2_666 . . . ? Mn1 I1 Mn1 C3 124.63(8) 2_666 . . . ? Mn1 I1 Mn1 C2 102.18(9) 2_666 . . . ? Mn1 I1 Mn1 C5 173.45(10) 2_666 . . . ? Mn1 I1 Mn1 C1 131.61(16) 2_666 . . . ? Mn1 I1 Mn1 C4 158.02(8) 2_666 . . . ? Mn1 I1 Mn1 I1 0.000(1) 2_666 . . 2_666 ? O1 Mn1 C1 C5 -67.93(19) . . . . ? C3 Mn1 C1 C5 75.73(19) . . . . ? C2 Mn1 C1 C5 114.0(3) . . . . ? C4 Mn1 C1 C5 35.63(18) . . . . ? I1 Mn1 C1 C5 67.4(3) . . . . ? I1 Mn1 C1 C5 -165.20(16) 2_666 . . . ? O1 Mn1 C1 C2 178.08(17) . . . . ? C3 Mn1 C1 C2 -38.26(17) . . . . ? C5 Mn1 C1 C2 -114.0(3) . . . . ? C4 Mn1 C1 C2 -78.36(19) . . . . ? I1 Mn1 C1 C2 -46.6(3) . . . . ? I1 Mn1 C1 C2 80.81(17) 2_666 . . . ? O1 Mn1 C1 C11 48.0(3) . . . . ? C3 Mn1 C1 C11 -168.3(3) . . . . ? C2 Mn1 C1 C11 -130.1(3) . . . . ? C5 Mn1 C1 C11 115.9(3) . . . . ? C4 Mn1 C1 C11 151.6(3) . . . . ? I1 Mn1 C1 C11 -176.68(17) . . . . ? I1 Mn1 C1 C11 -49.3(3) 2_666 . . . ? C5 C1 C2 C3 0.5(3) . . . . ? C11 C1 C2 C3 -174.9(3) . . . . ? Mn1 C1 C2 C3 65.8(2) . . . . ? C5 C1 C2 C21 167.2(3) . . . . ? C11 C1 C2 C21 -8.1(6) . . . . ? Mn1 C1 C2 C21 -127.4(4) . . . . ? C5 C1 C2 Mn1 -65.4(2) . . . . ? C11 C1 C2 Mn1 119.3(3) . . . . ? O1 Mn1 C2 C3 -116.5(2) . . . . ? C5 Mn1 C2 C3 -75.72(19) . . . . ? C1 Mn1 C2 C3 -113.6(3) . . . . ? C4 Mn1 C2 C3 -35.59(18) . . . . ? I1 Mn1 C2 C3 42.4(2) . . . . ? I1 Mn1 C2 C3 137.57(17) 2_666 . . . ? O1 Mn1 C2 C1 -2.8(2) . . . . ? C3 Mn1 C2 C1 113.6(3) . . . . ? C5 Mn1 C2 C1 37.93(17) . . . . ? C4 Mn1 C2 C1 78.06(19) . . . . ? I1 Mn1 C2 C1 156.06(14) . . . . ? I1 Mn1 C2 C1 -108.78(16) 2_666 . . . ? O1 Mn1 C2 C21 131.3(3) . . . . ? C3 Mn1 C2 C21 -112.2(4) . . . . ? C5 Mn1 C2 C21 172.0(3) . . . . ? C1 Mn1 C2 C21 134.1(4) . . . . ? C4 Mn1 C2 C21 -147.8(3) . . . . ? I1 Mn1 C2 C21 -69.8(3) . . . . ? I1 Mn1 C2 C21 25.3(3) 2_666 . . . ? C1 C2 C3 C4 0.5(3) . . . . ? C21 C2 C3 C4 -168.9(3) . . . . ? Mn1 C2 C3 C4 66.7(2) . . . . ? C1 C2 C3 Mn1 -66.3(2) . . . . ? C21 C2 C3 Mn1 124.4(3) . . . . ? O1 Mn1 C3 C4 -10.0(3) . . . . ? C2 Mn1 C3 C4 -117.4(3) . . . . ? C5 Mn1 C3 C4 -37.41(18) . . . . ? C1 Mn1 C3 C4 -78.9(2) . . . . ? I1 Mn1 C3 C4 97.17(17) . . . . ? I1 Mn1 C3 C4 -170.98(15) 2_666 . . . ? O1 Mn1 C3 C2 107.4(2) . . . . ? C5 Mn1 C3 C2 80.02(19) . . . . ? C1 Mn1 C3 C2 38.51(17) . . . . ? C4 Mn1 C3 C2 117.4(3) . . . . ? I1 Mn1 C3 C2 -145.40(17) . . . . ? I1 Mn1 C3 C2 -53.5(2) 2_666 . . . ? C2 C3 C4 C5 -1.2(3) . . . . ? Mn1 C3 C4 C5 63.9(2) . . . . ? C2 C3 C4 C41 168.5(3) . . . . ? Mn1 C3 C4 C41 -126.4(3) . . . . ? C2 C3 C4 Mn1 -65.1(2) . . . . ? O1 Mn1 C4 C3 173.50(18) . . . . ? C2 Mn1 C4 C3 36.73(18) . . . . ? C5 Mn1 C4 C3 114.8(3) . . . . ? C1 Mn1 C4 C3 78.3(2) . . . . ? I1 Mn1 C4 C3 -87.26(18) . . . . ? I1 Mn1 C4 C3 19.3(3) 2_666 . . . ? O1 Mn1 C4 C5 58.67(19) . . . . ? C3 Mn1 C4 C5 -114.8(3) . . . . ? C2 Mn1 C4 C5 -78.09(19) . . . . ? C1 Mn1 C4 C5 -36.52(18) . . . . ? I1 Mn1 C4 C5 157.91(16) . . . . ? I1 Mn1 C4 C5 -95.5(2) 2_666 . . . ? O1 Mn1 C4 C41 -64.4(3) . . . . ? C3 Mn1 C4 C41 122.2(4) . . . . ? C2 Mn1 C4 C41 158.9(3) . . . . ? C5 Mn1 C4 C41 -123.0(4) . . . . ? C1 Mn1 C4 C41 -159.5(3) . . . . ? I1 Mn1 C4 C41 34.9(3) . . . . ? I1 Mn1 C4 C41 141.5(2) 2_666 . . . ? C3 C4 C5 C1 1.5(3) . . . . ? C41 C4 C5 C1 -168.1(3) . . . . ? Mn1 C4 C5 C1 65.0(2) . . . . ? C3 C4 C5 Mn1 -63.5(2) . . . . ? C41 C4 C5 Mn1 126.9(3) . . . . ? C2 C1 C5 C4 -1.2(3) . . . . ? C11 C1 C5 C4 174.8(3) . . . . ? Mn1 C1 C5 C4 -66.1(2) . . . . ? C2 C1 C5 Mn1 64.9(2) . . . . ? C11 C1 C5 Mn1 -119.1(3) . . . . ? O1 Mn1 C5 C4 -126.20(18) . . . . ? C3 Mn1 C5 C4 37.37(18) . . . . ? C2 Mn1 C5 C4 79.1(2) . . . . ? C1 Mn1 C5 C4 117.5(3) . . . . ? I1 Mn1 C5 C4 -28.6(2) . . . . ? I1 Mn1 C5 C4 140.64(15) 2_666 . . . ? O1 Mn1 C5 C1 116.25(19) . . . . ? C3 Mn1 C5 C1 -80.2(2) . . . . ? C2 Mn1 C5 C1 -38.41(18) . . . . ? C4 Mn1 C5 C1 -117.5(3) . . . . ? I1 Mn1 C5 C1 -146.17(15) . . . . ? I1 Mn1 C5 C1 23.1(2) 2_666 . . . ? C5 C1 C11 C12 -115.2(3) . . . . ? C2 C1 C11 C12 59.6(4) . . . . ? Mn1 C1 C11 C12 155.9(2) . . . . ? C5 C1 C11 C13 120.7(3) . . . . ? C2 C1 C11 C13 -64.5(5) . . . . ? Mn1 C1 C11 C13 31.8(4) . . . . ? C5 C1 C11 C14 2.6(4) . . . . ? C2 C1 C11 C14 177.4(3) . . . . ? Mn1 C1 C11 C14 -86.3(3) . . . . ? C3 C2 C21 C24 -160.4(3) . . . . ? C1 C2 C21 C24 34.0(5) . . . . ? Mn1 C2 C21 C24 -71.1(4) . . . . ? C3 C2 C21 C23 -40.1(4) . . . . ? C1 C2 C21 C23 154.3(4) . . . . ? Mn1 C2 C21 C23 49.2(4) . . . . ? C3 C2 C21 C22 77.3(4) . . . . ? C1 C2 C21 C22 -88.4(4) . . . . ? Mn1 C2 C21 C22 166.5(3) . . . . ? C3 C4 C41 C43 20.7(4) . . . . ? C5 C4 C41 C43 -171.7(3) . . . . ? Mn1 C4 C41 C43 -74.9(4) . . . . ? C3 C4 C41 C44 142.6(3) . . . . ? C5 C4 C41 C44 -49.7(4) . . . . ? Mn1 C4 C41 C44 47.1(4) . . . . ? C3 C4 C41 C42 -99.0(4) . . . . ? C5 C4 C41 C42 68.7(4) . . . . ? Mn1 C4 C41 C42 165.5(3) . . . . ? C3 Mn1 O1 C61 33.9(6) . . . . ? C2 Mn1 O1 C61 89.0(6) . . . . ? C5 Mn1 O1 C61 56.1(6) . . . . ? C1 Mn1 O1 C61 87.3(6) . . . . ? C4 Mn1 O1 C61 28.1(6) . . . . ? I1 Mn1 O1 C61 -73.4(6) . . . . ? I1 Mn1 O1 C61 -161.7(6) 2_666 . . . ? C3 Mn1 O1 C64' -125.9(8) . . . . ? C2 Mn1 O1 C64' -70.8(8) . . . . ? C5 Mn1 O1 C64' -103.8(8) . . . . ? C1 Mn1 O1 C64' -72.5(8) . . . . ? C4 Mn1 O1 C64' -131.7(8) . . . . ? I1 Mn1 O1 C64' 126.8(8) . . . . ? I1 Mn1 O1 C64' 38.5(8) 2_666 . . . ? C3 Mn1 O1 C64 -147.8(5) . . . . ? C2 Mn1 O1 C64 -92.7(5) . . . . ? C5 Mn1 O1 C64 -125.6(5) . . . . ? C1 Mn1 O1 C64 -94.3(5) . . . . ? C4 Mn1 O1 C64 -153.6(5) . . . . ? I1 Mn1 O1 C64 104.9(5) . . . . ? I1 Mn1 O1 C64 16.6(5) 2_666 . . . ? C3 Mn1 O1 C61' 56.8(5) . . . . ? C2 Mn1 O1 C61' 111.8(5) . . . . ? C5 Mn1 O1 C61' 78.9(5) . . . . ? C1 Mn1 O1 C61' 110.2(5) . . . . ? C4 Mn1 O1 C61' 51.0(5) . . . . ? I1 Mn1 O1 C61' -50.5(5) . . . . ? I1 Mn1 O1 C61' -138.8(5) 2_666 . . . ? C64' O1 C61 C62 -35.4(9) . . . . ? C64 O1 C61 C62 -18.1(8) . . . . ? C61' O1 C61 C62 65.7(13) . . . . ? Mn1 O1 C61 C62 160.5(4) . . . . ? O1 C61 C62 C63 47.7(8) . . . . ? C61 C62 C63 C64 -56.6(7) . . . . ? C61 O1 C64 C63 -16.9(7) . . . . ? C64' O1 C64 C63 61.7(16) . . . . ? C61' O1 C64 C63 -37.2(6) . . . . ? Mn1 O1 C64 C63 164.6(3) . . . . ? C62 C63 C64 O1 48.3(7) . . . . ? C61 O1 C61' C62' -62.4(13) . . . . ? C64' O1 C61' C62' 22.6(8) . . . . ? C64 O1 C61' C62' 40.2(7) . . . . ? Mn1 O1 C61' C62' -159.6(4) . . . . ? O1 C61' C62' C63' -57.0(7) . . . . ? C61' C62' C63' C64' 64.3(8) . . . . ? C61 O1 C64' C63' 36.4(10) . . . . ? C64 O1 C64' C63' -70.3(16) . . . . ? C61' O1 C64' C63' 16.1(10) . . . . ? Mn1 O1 C64' C63' -161.5(4) . . . . ? C62' C63' C64' O1 -53.6(10) . . . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 71.87 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.474 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.087 _iucr_refine_instructions_details ; TITL c07293 in P-1 CELL 1.54178 9.2320 9.9138 13.3547 105.125 102.783 100.418 ZERR 1.00 0.0004 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H O MN I UNIT 42 74 2 2 2 FMAP 2 PLAN 10 L.S. 4 MPLA 5 C1 c2 c3 c4 c5 C11 C21 C41 BOND $H CONF TEMP -173 ACTA SIZE 0.05 0.10 0.10 WGHT 0.032700 2.356400 FVAR 0.62139 0.57922 I1 5 0.358234 0.609302 0.444386 11.00000 0.03853 0.02239 = 0.01622 0.00572 0.00790 0.01618 MN1 4 0.514299 0.413848 0.346319 11.00000 0.01866 0.01283 = 0.01366 0.00398 0.00445 0.00319 C1 1 0.521375 0.201789 0.205323 11.00000 0.01930 0.01810 = 0.01383 0.00308 0.00413 0.00799 C2 1 0.389055 0.162191 0.242840 11.00000 0.02004 0.01138 = 0.01416 0.00104 0.00422 0.00172 C3 1 0.286263 0.246278 0.212194 11.00000 0.01346 0.01549 = 0.01879 0.00074 0.00435 0.00147 AFIX 43 H3 2 0.189930 0.242667 0.227109 11.00000 -1.20000 AFIX 0 C4 1 0.347703 0.334911 0.156974 11.00000 0.01842 0.01503 = 0.01243 0.00137 0.00170 0.00543 C5 1 0.492615 0.309022 0.154493 11.00000 0.01790 0.01801 = 0.01379 0.00562 0.00517 0.00617 AFIX 43 H5 2 0.561448 0.356046 0.123495 11.00000 -1.20000 AFIX 0 C11 1 0.666186 0.144676 0.204700 11.00000 0.02451 0.02877 = 0.01986 0.00754 0.00812 0.01635 C12 1 0.624229 -0.016828 0.139824 11.00000 0.04258 0.03544 = 0.02311 0.00188 0.00370 0.02563 AFIX 137 H12A 2 0.570336 -0.031041 0.064417 11.00000 -1.50000 H12B 2 0.557521 -0.071827 0.170999 11.00000 -1.50000 H12C 2 0.718109 -0.050480 0.142735 11.00000 -1.50000 AFIX 0 C13 1 0.769530 0.170474 0.319159 11.00000 0.02350 0.03414 = 0.02480 0.00774 0.00236 0.01484 AFIX 137 H13A 2 0.711771 0.120774 0.358170 11.00000 -1.50000 H13B 2 0.802967 0.274294 0.358217 11.00000 -1.50000 H13C 2 0.859576 0.132761 0.313882 11.00000 -1.50000 AFIX 0 C14 1 0.767479 0.223478 0.149324 11.00000 0.02689 0.05851 = 0.04171 0.02501 0.01994 0.02489 AFIX 137 H14A 2 0.859584 0.187152 0.150678 11.00000 -1.50000 H14B 2 0.797598 0.327417 0.187887 11.00000 -1.50000 H14C 2 0.709666 0.205976 0.074191 11.00000 -1.50000 AFIX 0 C21 1 0.328488 0.038555 0.285269 11.00000 0.03294 0.01486 = 0.02510 0.00780 0.00956 -0.00029 C22 1 0.225689 -0.088769 0.186226 11.00000 0.04376 0.01687 = 0.03643 0.00743 0.00304 -0.00462 AFIX 137 H22A 2 0.286866 -0.121034 0.137700 11.00000 -1.50000 H22B 2 0.141392 -0.057423 0.147720 11.00000 -1.50000 H22C 2 0.183555 -0.168671 0.210388 11.00000 -1.50000 AFIX 0 C23 1 0.228597 0.086026 0.359415 11.00000 0.04044 0.03163 = 0.03961 0.01655 0.02113 0.00218 AFIX 137 H23A 2 0.193730 0.007825 0.387508 11.00000 -1.50000 H23B 2 0.139369 0.108341 0.318101 11.00000 -1.50000 H23C 2 0.289108 0.172129 0.419833 11.00000 -1.50000 AFIX 0 C24 1 0.449398 -0.016151 0.351342 11.00000 0.04934 0.02199 = 0.02916 0.01447 0.00845 0.00510 AFIX 137 H24A 2 0.515715 -0.050358 0.307639 11.00000 -1.50000 H24B 2 0.398071 -0.095734 0.372066 11.00000 -1.50000 H24C 2 0.511679 0.062680 0.416546 11.00000 -1.50000 AFIX 0 C41 1 0.262123 0.419844 0.094286 11.00000 0.02445 0.02226 = 0.01697 0.00644 0.00162 0.01153 C42 1 0.212326 0.330095 -0.027039 11.00000 0.03986 0.03398 = 0.02015 0.00261 -0.00407 0.01815 AFIX 137 H42A 2 0.303369 0.315494 -0.050334 11.00000 -1.50000 H42B 2 0.157766 0.381839 -0.069699 11.00000 -1.50000 H42C 2 0.144331 0.236158 -0.037859 11.00000 -1.50000 AFIX 0 C43 1 0.120718 0.443690 0.129572 11.00000 0.03510 0.04963 = 0.03564 0.01962 0.01018 0.02755 AFIX 137 H43A 2 0.048053 0.350213 0.113036 11.00000 -1.50000 H43B 2 0.072017 0.502623 0.090869 11.00000 -1.50000 H43C 2 0.150866 0.493616 0.207575 11.00000 -1.50000 AFIX 0 C44 1 0.363971 0.566420 0.107492 11.00000 0.04133 0.02735 = 0.03343 0.01752 0.00793 0.01440 AFIX 137 H44A 2 0.391292 0.627662 0.182941 11.00000 -1.50000 H44B 2 0.308455 0.612679 0.060458 11.00000 -1.50000 H44C 2 0.457617 0.553115 0.087563 11.00000 -1.50000 AFIX 0 SAME O1 C64 C63 C62 C61 SAME O1 C61' > C64' SIMU O1 > C64' 0.02 0.04 0.9 O1 3 0.721123 0.581450 0.363990 11.00000 0.02357 0.02485 = 0.02610 0.01109 0.00304 -0.00012 PART 1 21 C61 1 0.717400 0.673931 0.297730 21.00000 0.04164 AFIX 23 H61A 2 0.621033 0.705813 0.288468 21.00000 -1.20000 H61B 2 0.726458 0.624262 0.225612 21.00000 -1.20000 AFIX 0 C62 1 0.862440 0.807467 0.362897 21.00000 0.02858 AFIX 23 H62A 2 0.891434 0.867802 0.318420 21.00000 -1.20000 H62B 2 0.850196 0.868100 0.430713 21.00000 -1.20000 AFIX 0 C63 1 0.968149 0.712692 0.381613 21.00000 0.03495 AFIX 23 H63A 2 1.071696 0.769361 0.428675 21.00000 -1.20000 H63B 2 0.976729 0.650864 0.312907 21.00000 -1.20000 AFIX 0 C64 1 0.876093 0.619890 0.441604 21.00000 0.02363 AFIX 23 H64A 2 0.913759 0.533594 0.445828 21.00000 -1.20000 H64B 2 0.879482 0.678866 0.514806 21.00000 -1.20000 AFIX 0 PART 2 -21 C61' 1 0.707021 0.710647 0.327361 -21.00000 0.01442 AFIX 23 H61C 2 0.687351 0.788916 0.381899 -21.00000 -1.20000 H61D 2 0.629399 0.685789 0.256709 -21.00000 -1.20000 AFIX 0 C62' 1 0.890207 0.747530 0.318894 -21.00000 0.04003 AFIX 23 H62C 2 0.911440 0.667132 0.267161 -21.00000 -1.20000 H62D 2 0.919472 0.838696 0.302413 -21.00000 -1.20000 AFIX 0 C63' 1 0.959628 0.760439 0.433026 -21.00000 0.02571 AFIX 23 H63C 2 0.923067 0.827565 0.484854 -21.00000 -1.20000 H63D 2 1.073223 0.783964 0.454018 -21.00000 -1.20000 AFIX 0 C64' 1 0.881817 0.594898 0.411641 -21.00000 0.03232 AFIX 23 H64C 2 0.923590 0.531198 0.361341 -21.00000 -1.20000 H64D 2 0.897702 0.570768 0.480021 -21.00000 -1.20000 HKLF 4 ; # end of cif file data_c07309 _database_code_depnum_ccdc_archive 'CCDC 743655' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H122 Mn5, 2(C5 H12)' _chemical_formula_sum 'C78 H146 Mn5' _chemical_formula_weight 1358.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.5131(8) _cell_length_b 12.7588(4) _cell_length_c 25.2896(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.339(2) _cell_angle_gamma 90.00 _cell_volume 8088.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9925 _cell_measurement_theta_min 3.53 _cell_measurement_theta_max 70.95 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2956 _exptl_absorpt_coefficient_mu 6.434 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2961 _exptl_absorpt_correction_T_max 0.5655 _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51089 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 68.22 _reflns_number_total 7315 _reflns_number_gt 6656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0422P)^2^+8.1504P] 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 7315 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.003 _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 0.983392(12) 0.31151(2) 0.320572(13) 0.02213(9) Uani 1 1 d . . . Mn2 Mn 1.0000 0.19806(3) 0.2500 0.01744(10) Uani 1 2 d S . . Mn3 Mn 1.079167(12) 0.08408(2) 0.298495(13) 0.02207(9) Uani 1 1 d . . . C1 C 0.98384(8) 0.34878(15) 0.41293(8) 0.0211(4) Uani 1 1 d . . . C2 C 1.02675(8) 0.40726(15) 0.40714(8) 0.0210(4) Uani 1 1 d . . . C3 C 1.00168(7) 0.48095(15) 0.36102(8) 0.0209(4) Uani 1 1 d . . . H3 H 1.0202 0.5308 0.3483 0.025 Uiso 1 1 calc R . . C4 C 0.94594(7) 0.46933(15) 0.33719(8) 0.0209(4) Uani 1 1 d . . . C5 C 0.93545(8) 0.38804(15) 0.36912(8) 0.0214(4) Uani 1 1 d . . . H5 H 0.9009 0.3630 0.3623 0.026 Uiso 1 1 calc R . . C11 C 1.08787(8) 0.40892(16) 0.44188(9) 0.0253(4) Uani 1 1 d . . . C12 C 1.11488(8) 0.45026(19) 0.40300(10) 0.0327(5) Uani 1 1 d . . . H12A H 1.1537 0.4433 0.4236 0.049 Uiso 1 1 calc R . . H12B H 1.1056 0.5242 0.3938 0.049 Uiso 1 1 calc R . . H12C H 1.1024 0.4094 0.3670 0.049 Uiso 1 1 calc R . . C13 C 1.11307(8) 0.30132(17) 0.46376(9) 0.0303(5) Uani 1 1 d . . . H13A H 1.1006 0.2747 0.4924 0.045 Uiso 1 1 calc R . . H13B H 1.1520 0.3081 0.4818 0.045 Uiso 1 1 calc R . . H13C H 1.1027 0.2524 0.4310 0.045 Uiso 1 1 calc R . . C14 C 1.10246(9) 0.48532(18) 0.49326(9) 0.0317(5) Uani 1 1 d . . . H14A H 1.0848 0.4633 0.5180 0.048 Uiso 1 1 calc R . . H14B H 1.0907 0.5562 0.4786 0.048 Uiso 1 1 calc R . . H14C H 1.1412 0.4851 0.5159 0.048 Uiso 1 1 calc R . . C21 C 0.98233(8) 0.26460(16) 0.45615(8) 0.0247(4) Uani 1 1 d . . . C22 C 1.00377(9) 0.15764(16) 0.44671(10) 0.0322(5) Uani 1 1 d . . . H22A H 0.9827 0.1336 0.4070 0.048 Uiso 1 1 calc R . . H22B H 1.0010 0.1064 0.4742 0.048 Uiso 1 1 calc R . . H22C H 1.0412 0.1650 0.4529 0.048 Uiso 1 1 calc R . . C23 C 1.01264(9) 0.30186(17) 0.51932(9) 0.0303(5) Uani 1 1 d . . . H23A H 1.0507 0.3086 0.5281 0.046 Uiso 1 1 calc R . . H23B H 1.0079 0.2507 0.5457 0.046 Uiso 1 1 calc R . . H23C H 0.9986 0.3700 0.5243 0.046 Uiso 1 1 calc R . . C24 C 0.92421(9) 0.24436(18) 0.44731(9) 0.0305(5) Uani 1 1 d . . . H24A H 0.9080 0.3103 0.4517 0.046 Uiso 1 1 calc R . . H24B H 0.9238 0.1939 0.4763 0.046 Uiso 1 1 calc R . . H24C H 0.9040 0.2160 0.4083 0.046 Uiso 1 1 calc R . . C41 C 0.90408(8) 0.53633(16) 0.29092(9) 0.0248(4) Uani 1 1 d . . . C42 C 0.92706(9) 0.58904(18) 0.25184(9) 0.0316(5) Uani 1 1 d . . . H42A H 0.9568 0.6346 0.2753 0.047 Uiso 1 1 calc R . . H42B H 0.8993 0.6310 0.2222 0.047 Uiso 1 1 calc R . . H42C H 0.9398 0.5353 0.2330 0.047 Uiso 1 1 calc R . . C43 C 0.88582(10) 0.6211(2) 0.32165(11) 0.0418(6) Uani 1 1 d . . . H43A H 0.8707 0.5879 0.3465 0.063 Uiso 1 1 calc R . . H43B H 0.8586 0.6651 0.2926 0.063 Uiso 1 1 calc R . . H43C H 0.9164 0.6646 0.3455 0.063 Uiso 1 1 calc R . . C44 C 0.85626(9) 0.4698(2) 0.25269(11) 0.0435(6) Uani 1 1 d . . . H44A H 0.8681 0.4154 0.2333 0.065 Uiso 1 1 calc R . . H44B H 0.8297 0.5145 0.2235 0.065 Uiso 1 1 calc R . . H44C H 0.8404 0.4368 0.2768 0.065 Uiso 1 1 calc R . . C6 C 1.14847(7) -0.01507(15) 0.29014(8) 0.0220(4) Uani 1 1 d . . . C7 C 1.17176(7) 0.04463(15) 0.34389(8) 0.0225(4) Uani 1 1 d . . . C8 C 1.14690(7) 0.00704(15) 0.37997(8) 0.0222(4) Uani 1 1 d . . . H8 H 1.1541 0.0330 0.4177 0.027 Uiso 1 1 calc R . . C9 C 1.11027(7) -0.07371(15) 0.35200(8) 0.0206(4) Uani 1 1 d . . . C10 C 1.11165(8) -0.08718(15) 0.29729(8) 0.0217(4) Uani 1 1 d . . . H10 H 1.0910 -0.1371 0.2691 0.026 Uiso 1 1 calc R . . C51 C 1.15898(8) -0.01980(17) 0.23474(9) 0.0276(4) Uani 1 1 d . . . C52 C 1.16951(10) 0.08653(18) 0.21327(10) 0.0342(5) Uani 1 1 d . . . H52A H 1.1395 0.1337 0.2068 0.051 Uiso 1 1 calc R . . H52B H 1.1735 0.0769 0.1768 0.051 Uiso 1 1 calc R . . H52C H 1.2023 0.1169 0.2425 0.051 Uiso 1 1 calc R . . C53 C 1.10968(9) -0.06537(19) 0.18410(9) 0.0353(5) Uani 1 1 d . . . H53A H 1.0784 -0.0223 0.1781 0.053 Uiso 1 1 calc R . . H53B H 1.1035 -0.1373 0.1934 0.053 Uiso 1 1 calc R . . H53C H 1.1159 -0.0654 0.1487 0.053 Uiso 1 1 calc R . . C54 C 1.20615(9) -0.09476(18) 0.24566(11) 0.0352(5) Uani 1 1 d . . . H54A H 1.2120 -0.1014 0.2101 0.053 Uiso 1 1 calc R . . H54B H 1.1980 -0.1638 0.2570 0.053 Uiso 1 1 calc R . . H54C H 1.2384 -0.0667 0.2768 0.053 Uiso 1 1 calc R . . C61 C 1.21484(8) 0.13094(16) 0.36556(9) 0.0263(4) Uani 1 1 d . . . C62 C 1.19393(9) 0.23604(17) 0.33415(10) 0.0326(5) Uani 1 1 d . . . H62A H 1.1815 0.2260 0.2922 0.049 Uiso 1 1 calc R . . H62B H 1.2227 0.2880 0.3475 0.049 Uiso 1 1 calc R . . H62C H 1.1643 0.2609 0.3429 0.049 Uiso 1 1 calc R . . C63 C 1.26611(8) 0.09770(18) 0.35982(11) 0.0340(5) Uani 1 1 d . . . H63A H 1.2782 0.0300 0.3791 0.051 Uiso 1 1 calc R . . H63B H 1.2939 0.1505 0.3781 0.051 Uiso 1 1 calc R . . H63C H 1.2590 0.0914 0.3187 0.051 Uiso 1 1 calc R . . C64 C 1.23054(9) 0.15220(18) 0.43048(10) 0.0339(5) Uani 1 1 d . . . H64A H 1.1990 0.1744 0.4362 0.051 Uiso 1 1 calc R . . H64B H 1.2576 0.2076 0.4438 0.051 Uiso 1 1 calc R . . H64C H 1.2451 0.0881 0.4527 0.051 Uiso 1 1 calc R . . C91 C 1.07797(8) -0.13651(15) 0.37759(8) 0.0226(4) Uani 1 1 d . . . C92 C 1.05921(9) -0.06468(17) 0.41407(9) 0.0291(4) Uani 1 1 d . . . H92A H 1.0386 -0.0064 0.3900 0.044 Uiso 1 1 calc R . . H92B H 1.0903 -0.0371 0.4470 0.044 Uiso 1 1 calc R . . H92C H 1.0368 -0.1047 0.4285 0.044 Uiso 1 1 calc R . . C93 C 1.02891(9) -0.18586(18) 0.33005(9) 0.0310(5) Uani 1 1 d . . . H93A H 1.0062 -0.1307 0.3050 0.047 Uiso 1 1 calc R . . H93B H 1.0088 -0.2251 0.3477 0.047 Uiso 1 1 calc R . . H93C H 1.0401 -0.2336 0.3068 0.047 Uiso 1 1 calc R . . C94 C 1.11322(9) -0.22445(18) 0.41604(10) 0.0345(5) Uani 1 1 d . . . H94A H 1.0928 -0.2650 0.4328 0.052 Uiso 1 1 calc R . . H94B H 1.1445 -0.1937 0.4473 0.052 Uiso 1 1 calc R . . H94C H 1.1248 -0.2707 0.3925 0.052 Uiso 1 1 calc R . . C100 C 1.25249(12) -0.2063(2) 0.41270(15) 0.0574(8) Uani 1 1 d . . . H10A H 1.2567 -0.2028 0.4531 0.086 Uiso 1 1 calc R . . H10B H 1.2226 -0.1616 0.3885 0.086 Uiso 1 1 calc R . . H10C H 1.2853 -0.1820 0.4103 0.086 Uiso 1 1 calc R . . C101 C 1.24124(11) -0.3194(2) 0.39124(14) 0.0510(7) Uani 1 1 d . . . H10D H 1.2071 -0.3421 0.3919 0.061 Uiso 1 1 calc R . . H10E H 1.2371 -0.3223 0.3505 0.061 Uiso 1 1 calc R . . C102 C 1.28470(9) -0.39486(19) 0.42719(11) 0.0372(5) Uani 1 1 d . . . H10F H 1.2881 -0.3929 0.4677 0.045 Uiso 1 1 calc R . . H10G H 1.3190 -0.3707 0.4274 0.045 Uiso 1 1 calc R . . C103 C 1.27525(9) -0.50755(18) 0.40586(10) 0.0352(5) Uani 1 1 d . . . H10H H 1.2432 -0.5348 0.4098 0.042 Uiso 1 1 calc R . . H10I H 1.2680 -0.5089 0.3641 0.042 Uiso 1 1 calc R . . C104 C 1.32214(10) -0.57907(19) 0.43875(10) 0.0386(5) Uani 1 1 d . . . H10J H 1.3547 -0.5493 0.4380 0.058 Uiso 1 1 calc R . . H10K H 1.3156 -0.6484 0.4204 0.058 Uiso 1 1 calc R . . H10L H 1.3264 -0.5858 0.4790 0.058 Uiso 1 1 calc R . . H100 H 1.0000 0.320(3) 0.2500 0.048(11) Uiso 1 2 d S . . H101 H 1.0501(11) 0.197(2) 0.2373(13) 0.054(9) Uiso 1 1 d . . . H102 H 1.0364(12) 0.196(2) 0.3166(13) 0.060(9) Uiso 1 1 d . . . H103 H 1.0000 0.079(3) 0.2500 0.054(12) Uiso 1 2 d S . . 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 0.02614(17) 0.01968(16) 0.02114(16) -0.00274(11) 0.01033(12) 0.00004(12) Mn2 0.0184(2) 0.0153(2) 0.01818(19) 0.000 0.00708(15) 0.000 Mn3 0.02043(17) 0.01955(16) 0.02480(16) 0.00260(12) 0.00787(12) 0.00233(11) C1 0.0271(10) 0.0184(9) 0.0195(9) -0.0032(7) 0.0112(7) -0.0005(7) C2 0.0251(10) 0.0181(9) 0.0201(9) -0.0026(7) 0.0095(8) 0.0019(7) C3 0.0221(10) 0.0171(9) 0.0231(9) -0.0016(7) 0.0088(7) -0.0005(7) C4 0.0232(10) 0.0166(9) 0.0240(9) -0.0032(7) 0.0110(8) 0.0008(7) C5 0.0224(10) 0.0193(9) 0.0240(9) -0.0019(7) 0.0109(8) -0.0001(7) C11 0.0235(10) 0.0234(10) 0.0258(10) -0.0006(8) 0.0069(8) 0.0023(8) C12 0.0226(11) 0.0368(12) 0.0376(12) 0.0019(10) 0.0114(9) -0.0004(9) C13 0.0250(11) 0.0297(12) 0.0316(11) 0.0003(9) 0.0071(8) 0.0063(8) C14 0.0288(11) 0.0286(11) 0.0302(11) -0.0043(9) 0.0045(9) -0.0017(8) C21 0.0312(11) 0.0214(10) 0.0220(9) -0.0009(8) 0.0114(8) -0.0011(8) C22 0.0444(13) 0.0189(10) 0.0342(11) 0.0010(8) 0.0171(10) 0.0015(9) C23 0.0386(12) 0.0309(12) 0.0223(10) 0.0011(8) 0.0134(9) -0.0031(9) C24 0.0381(12) 0.0305(11) 0.0261(10) 0.0015(8) 0.0164(9) -0.0062(9) C41 0.0227(10) 0.0216(10) 0.0259(10) 0.0004(8) 0.0059(8) -0.0004(8) C42 0.0285(11) 0.0326(12) 0.0285(11) 0.0087(9) 0.0066(9) 0.0000(9) C43 0.0465(14) 0.0354(13) 0.0445(14) 0.0088(11) 0.0199(11) 0.0212(11) C44 0.0300(12) 0.0377(14) 0.0436(14) 0.0106(11) -0.0043(10) -0.0077(10) C6 0.0199(9) 0.0198(10) 0.0256(10) 0.0028(7) 0.0088(7) 0.0030(7) C7 0.0193(9) 0.0194(10) 0.0271(10) 0.0019(8) 0.0078(8) 0.0040(7) C8 0.0209(9) 0.0216(10) 0.0211(9) 0.0002(7) 0.0056(7) 0.0028(7) C9 0.0202(9) 0.0176(9) 0.0223(9) 0.0037(7) 0.0069(7) 0.0044(7) C10 0.0237(10) 0.0174(9) 0.0239(9) 0.0009(7) 0.0097(8) 0.0027(7) C51 0.0304(11) 0.0264(11) 0.0297(10) 0.0013(8) 0.0160(9) 0.0006(8) C52 0.0419(13) 0.0323(12) 0.0346(11) 0.0055(9) 0.0221(10) 0.0005(9) C53 0.0430(13) 0.0415(13) 0.0251(10) -0.0025(9) 0.0177(9) -0.0026(10) C54 0.0398(13) 0.0310(12) 0.0438(13) 0.0016(10) 0.0263(11) 0.0061(9) C61 0.0193(10) 0.0245(10) 0.0325(11) 0.0007(8) 0.0081(8) -0.0018(8) C62 0.0289(11) 0.0227(11) 0.0417(12) -0.0002(9) 0.0099(9) -0.0018(8) C63 0.0225(11) 0.0321(12) 0.0447(13) 0.0009(10) 0.0111(9) -0.0013(8) C64 0.0260(11) 0.0341(12) 0.0362(12) -0.0056(9) 0.0074(9) -0.0085(9) C91 0.0259(10) 0.0194(10) 0.0230(9) 0.0004(7) 0.0105(8) -0.0005(7) C92 0.0372(12) 0.0246(11) 0.0323(11) -0.0020(8) 0.0212(9) -0.0033(8) C93 0.0329(12) 0.0338(12) 0.0292(10) -0.0043(9) 0.0157(9) -0.0105(9) C94 0.0390(13) 0.0274(11) 0.0393(12) 0.0105(9) 0.0184(10) 0.0058(9) C100 0.0528(17) 0.0364(15) 0.080(2) 0.0037(14) 0.0248(15) 0.0108(12) C101 0.0390(14) 0.0427(15) 0.0664(18) -0.0012(13) 0.0167(13) 0.0075(11) C102 0.0358(13) 0.0338(13) 0.0405(13) -0.0030(10) 0.0143(10) -0.0013(9) C103 0.0341(12) 0.0338(13) 0.0386(12) -0.0038(10) 0.0159(10) -0.0057(9) C104 0.0451(14) 0.0349(13) 0.0349(12) -0.0003(10) 0.0155(10) -0.0021(10) _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 C5 2.3527(19) . ? Mn1 C3 2.3556(19) . ? Mn1 C2 2.3569(19) . ? Mn1 C4 2.3769(18) . ? Mn1 C1 2.3787(18) . ? Mn1 Mn2 2.4823(4) . ? Mn1 H100 2.019(2) . ? Mn1 H102 2.11(3) . ? Mn2 Mn3 2.4822(4) 2_755 ? Mn2 Mn3 2.4822(4) . ? Mn2 Mn1 2.4823(4) 2_755 ? Mn2 H100 1.55(4) . ? Mn2 H101 1.54(3) . ? Mn2 H102 1.57(3) . ? Mn2 H103 1.52(4) . ? Mn3 C8 2.3493(19) . ? Mn3 C10 2.3656(19) . ? Mn3 C6 2.3690(19) . ? Mn3 C7 2.3772(19) . ? Mn3 C9 2.3795(18) . ? Mn3 H101 2.02(3) . ? Mn3 H102 2.02(3) . ? Mn3 H103 2.0125(14) . ? C1 C5 1.426(3) . ? C1 C2 1.454(3) . ? C1 C21 1.545(3) . ? C2 C3 1.434(3) . ? C2 C11 1.543(3) . ? C3 C4 1.405(3) . ? C3 H3 0.9500 . ? C4 C5 1.415(3) . ? C4 C41 1.522(3) . ? C5 H5 0.9500 . ? C11 C13 1.535(3) . ? C11 C14 1.539(3) . ? C11 C12 1.549(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 C23 1.541(3) . ? C21 C24 1.542(3) . ? C21 C22 1.544(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C41 C44 1.529(3) . ? C41 C42 1.531(3) . ? C41 C43 1.533(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C6 C10 1.434(3) . ? C6 C7 1.456(3) . ? C6 C51 1.544(3) . ? C7 C8 1.430(3) . ? C7 C61 1.543(3) . ? C8 C9 1.411(3) . ? C8 H8 0.9500 . ? C9 C10 1.410(3) . ? C9 C91 1.525(3) . ? C10 H10 0.9500 . ? C51 C52 1.533(3) . ? C51 C54 1.543(3) . ? C51 C53 1.545(3) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C61 C63 1.536(3) . ? C61 C64 1.540(3) . ? C61 C62 1.544(3) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C91 C93 1.525(3) . ? C91 C92 1.533(3) . ? C91 C94 1.539(3) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C100 C101 1.528(4) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C101 C102 1.512(3) . ? C101 H10D 0.9900 . ? C101 H10E 0.9900 . ? C102 C103 1.520(3) . ? C102 H10F 0.9900 . ? C102 H10G 0.9900 . ? C103 C104 1.518(3) . ? C103 H10H 0.9900 . ? C103 H10I 0.9900 . ? C104 H10J 0.9800 . ? C104 H10K 0.9800 . ? C104 H10L 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 C5 Mn1 C3 57.17(7) . . ? C5 Mn1 C2 58.55(7) . . ? C3 Mn1 C2 35.44(6) . . ? C5 Mn1 C4 34.82(6) . . ? C3 Mn1 C4 34.55(7) . . ? C2 Mn1 C4 59.14(6) . . ? C5 Mn1 C1 35.09(7) . . ? C3 Mn1 C1 58.42(7) . . ? C2 Mn1 C1 35.76(7) . . ? C4 Mn1 C1 58.95(7) . . ? C5 Mn1 Mn2 157.84(5) . . ? C3 Mn1 Mn2 141.06(5) . . ? C2 Mn1 Mn2 142.88(5) . . ? C4 Mn1 Mn2 147.44(5) . . ? C1 Mn1 Mn2 153.46(5) . . ? C5 Mn1 H100 145.0(9) . . ? C3 Mn1 H100 104.5(11) . . ? C2 Mn1 H100 125.6(8) . . ? C4 Mn1 H100 112.6(11) . . ? C1 Mn1 H100 161.1(9) . . ? Mn2 Mn1 H100 38.7(11) . . ? C5 Mn1 H102 149.7(8) . . ? C3 Mn1 H102 129.5(8) . . ? C2 Mn1 H102 108.2(8) . . ? C4 Mn1 H102 164.0(8) . . ? C1 Mn1 H102 117.6(8) . . ? Mn2 Mn1 H102 38.8(8) . . ? H100 Mn1 H102 65.3(12) . . ? Mn3 Mn2 Mn3 108.27(2) 2_755 . ? Mn3 Mn2 Mn1 108.230(10) 2_755 . ? Mn3 Mn2 Mn1 111.745(10) . . ? Mn3 Mn2 Mn1 111.745(10) 2_755 2_755 ? Mn3 Mn2 Mn1 108.230(10) . 2_755 ? Mn1 Mn2 Mn1 108.65(2) . 2_755 ? Mn3 Mn2 H100 125.864(11) 2_755 . ? Mn3 Mn2 H100 125.864(13) . . ? Mn1 Mn2 H100 54.327(10) . . ? Mn1 Mn2 H100 54.327(11) 2_755 . ? Mn3 Mn2 H101 124.7(11) 2_755 . ? Mn3 Mn2 H101 54.4(11) . . ? Mn1 Mn2 H101 127.1(11) . . ? Mn1 Mn2 H101 53.8(11) 2_755 . ? H100 Mn2 H101 90.6(11) . . ? Mn3 Mn2 H102 124.2(11) 2_755 . ? Mn3 Mn2 H102 54.2(11) . . ? Mn1 Mn2 H102 57.5(11) . . ? Mn1 Mn2 H102 124.0(11) 2_755 . ? H100 Mn2 H102 91.1(11) . . ? H101 Mn2 H102 89.7(15) . . ? Mn3 Mn2 H103 54.136(11) 2_755 . ? Mn3 Mn2 H103 54.136(11) . . ? Mn1 Mn2 H103 125.673(11) . . ? Mn1 Mn2 H103 125.673(10) 2_755 . ? H100 Mn2 H103 180.000(12) . . ? H101 Mn2 H103 89.4(11) . . ? H102 Mn2 H103 88.9(11) . . ? C8 Mn3 C10 57.15(7) . . ? C8 Mn3 C6 58.54(7) . . ? C10 Mn3 C6 35.26(7) . . ? C8 Mn3 C7 35.21(7) . . ? C10 Mn3 C7 58.35(7) . . ? C6 Mn3 C7 35.73(7) . . ? C8 Mn3 C9 34.70(7) . . ? C10 Mn3 C9 34.57(6) . . ? C6 Mn3 C9 58.99(7) . . ? C7 Mn3 C9 58.90(7) . . ? C8 Mn3 Mn2 153.61(5) . . ? C10 Mn3 Mn2 142.56(5) . . ? C6 Mn3 Mn2 147.50(5) . . ? C7 Mn3 Mn2 155.53(5) . . ? C9 Mn3 Mn2 144.43(5) . . ? C8 Mn3 H101 152.9(8) . . ? C10 Mn3 H101 132.8(8) . . ? C6 Mn3 H101 113.0(8) . . ? C7 Mn3 H101 121.8(8) . . ? C9 Mn3 H101 166.8(8) . . ? Mn2 Mn3 H101 38.3(8) . . ? C8 Mn3 H102 115.0(9) . . ? C10 Mn3 H102 156.1(9) . . ? C6 Mn3 H102 164.5(9) . . ? C7 Mn3 H102 130.5(9) . . ? C9 Mn3 H102 125.1(9) . . ? Mn2 Mn3 H102 39.0(9) . . ? H101 Mn3 H102 65.7(12) . . ? C8 Mn3 H103 142.2(9) . . ? C10 Mn3 H103 106.5(12) . . ? C6 Mn3 H103 129.7(9) . . ? C7 Mn3 H103 164.4(11) . . ? C9 Mn3 H103 111.5(11) . . ? Mn2 Mn3 H103 37.6(12) . . ? H101 Mn3 H103 64.4(12) . . ? H102 Mn3 H103 64.7(13) . . ? C5 C1 C2 106.15(16) . . ? C5 C1 C21 120.33(17) . . ? C2 C1 C21 133.44(17) . . ? C5 C1 Mn1 71.46(10) . . ? C2 C1 Mn1 71.30(10) . . ? C21 C1 Mn1 124.40(12) . . ? C3 C2 C1 106.25(16) . . ? C3 C2 C11 120.00(17) . . ? C1 C2 C11 133.55(17) . . ? C3 C2 Mn1 72.23(11) . . ? C1 C2 Mn1 72.93(10) . . ? C11 C2 Mn1 123.47(12) . . ? C4 C3 C2 110.72(17) . . ? C4 C3 Mn1 73.56(11) . . ? C2 C3 Mn1 72.33(10) . . ? C4 C3 H3 124.6 . . ? C2 C3 H3 124.6 . . ? Mn1 C3 H3 121.1 . . ? C3 C4 C5 106.00(16) . . ? C3 C4 C41 128.08(17) . . ? C5 C4 C41 125.64(17) . . ? C3 C4 Mn1 71.90(11) . . ? C5 C4 Mn1 71.66(10) . . ? C41 C4 Mn1 125.86(13) . . ? C4 C5 C1 110.86(17) . . ? C4 C5 Mn1 73.53(11) . . ? C1 C5 Mn1 73.45(10) . . ? C4 C5 H5 124.6 . . ? C1 C5 H5 124.6 . . ? Mn1 C5 H5 120.1 . . ? C13 C11 C14 109.89(17) . . ? C13 C11 C2 114.66(17) . . ? C14 C11 C2 109.46(16) . . ? C13 C11 C12 105.65(17) . . ? C14 C11 C12 107.09(18) . . ? C2 C11 C12 109.78(16) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C23 C21 C24 106.73(16) . . ? C23 C21 C22 110.79(17) . . ? C24 C21 C22 105.60(17) . . ? C23 C21 C1 110.97(16) . . ? C24 C21 C1 110.02(16) . . ? C22 C21 C1 112.43(16) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C4 C41 C44 110.83(17) . . ? C4 C41 C42 111.11(16) . . ? C44 C41 C42 108.20(18) . . ? C4 C41 C43 108.00(17) . . ? C44 C41 C43 109.6(2) . . ? C42 C41 C43 109.04(18) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C10 C6 C7 106.26(16) . . ? C10 C6 C51 119.71(17) . . ? C7 C6 C51 133.82(18) . . ? C10 C6 Mn3 72.24(10) . . ? C7 C6 Mn3 72.44(10) . . ? C51 C6 Mn3 124.08(13) . . ? C8 C7 C6 106.13(17) . . ? C8 C7 C61 120.80(17) . . ? C6 C7 C61 133.06(18) . . ? C8 C7 Mn3 71.33(10) . . ? C6 C7 Mn3 71.83(10) . . ? C61 C7 Mn3 122.25(13) . . ? C9 C8 C7 110.85(17) . . ? C9 C8 Mn3 73.82(10) . . ? C7 C8 Mn3 73.46(11) . . ? C9 C8 H8 124.6 . . ? C7 C8 H8 124.6 . . ? Mn3 C8 H8 119.8 . . ? C10 C9 C8 106.17(17) . . ? C10 C9 C91 127.48(17) . . ? C8 C9 C91 126.30(17) . . ? C10 C9 Mn3 72.18(11) . . ? C8 C9 Mn3 71.48(11) . . ? C91 C9 Mn3 123.37(12) . . ? C9 C10 C6 110.58(17) . . ? C9 C10 Mn3 73.25(11) . . ? C6 C10 Mn3 72.50(11) . . ? C9 C10 H10 124.7 . . ? C6 C10 H10 124.7 . . ? Mn3 C10 H10 121.1 . . ? C52 C51 C54 110.14(18) . . ? C52 C51 C6 114.85(17) . . ? C54 C51 C6 108.68(17) . . ? C52 C51 C53 105.60(18) . . ? C54 C51 C53 107.55(18) . . ? C6 C51 C53 109.76(16) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C63 C61 C64 106.52(17) . . ? C63 C61 C7 111.72(17) . . ? C64 C61 C7 109.95(17) . . ? C63 C61 C62 110.69(18) . . ? C64 C61 C62 106.07(18) . . ? C7 C61 C62 111.61(16) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C9 C91 C93 111.33(16) . . ? C9 C91 C92 109.94(16) . . ? C93 C91 C92 108.25(17) . . ? C9 C91 C94 108.99(16) . . ? C93 C91 C94 108.65(18) . . ? C92 C91 C94 109.66(17) . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C91 C93 H93A 109.5 . . ? C91 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C91 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C91 C94 H94A 109.5 . . ? C91 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C91 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C101 C100 H10A 109.5 . . ? C101 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C101 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C102 C101 C100 113.2(2) . . ? C102 C101 H10D 108.9 . . ? C100 C101 H10D 108.9 . . ? C102 C101 H10E 108.9 . . ? C100 C101 H10E 108.9 . . ? H10D C101 H10E 107.8 . . ? C101 C102 C103 114.3(2) . . ? C101 C102 H10F 108.7 . . ? C103 C102 H10F 108.7 . . ? C101 C102 H10G 108.7 . . ? C103 C102 H10G 108.7 . . ? H10F C102 H10G 107.6 . . ? C104 C103 C102 113.07(19) . . ? C104 C103 H10H 109.0 . . ? C102 C103 H10H 109.0 . . ? C104 C103 H10I 109.0 . . ? C102 C103 H10I 109.0 . . ? H10H C103 H10I 107.8 . . ? C103 C104 H10J 109.5 . . ? C103 C104 H10K 109.5 . . ? H10J C104 H10K 109.5 . . ? C103 C104 H10L 109.5 . . ? H10J C104 H10L 109.5 . . ? H10K C104 H10L 109.5 . . ? 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 C5 Mn1 Mn2 Mn3 -7.44(13) . . . 2_755 ? C3 Mn1 Mn2 Mn3 -146.15(7) . . . 2_755 ? C2 Mn1 Mn2 Mn3 154.72(8) . . . 2_755 ? C4 Mn1 Mn2 Mn3 -85.96(9) . . . 2_755 ? C1 Mn1 Mn2 Mn3 86.05(11) . . . 2_755 ? C5 Mn1 Mn2 Mn3 -126.56(13) . . . . ? C3 Mn1 Mn2 Mn3 94.72(8) . . . . ? C2 Mn1 Mn2 Mn3 35.59(8) . . . . ? C4 Mn1 Mn2 Mn3 154.92(9) . . . . ? C1 Mn1 Mn2 Mn3 -33.08(11) . . . . ? C5 Mn1 Mn2 Mn1 114.09(13) . . . 2_755 ? C3 Mn1 Mn2 Mn1 -24.62(7) . . . 2_755 ? C2 Mn1 Mn2 Mn1 -83.76(8) . . . 2_755 ? C4 Mn1 Mn2 Mn1 35.57(9) . . . 2_755 ? C1 Mn1 Mn2 Mn1 -152.42(11) . . . 2_755 ? Mn3 Mn2 Mn3 C8 -107.19(11) 2_755 . . . ? Mn1 Mn2 Mn3 C8 11.91(12) . . . . ? Mn1 Mn2 Mn3 C8 131.51(11) 2_755 . . . ? Mn3 Mn2 Mn3 C10 21.47(8) 2_755 . . . ? Mn1 Mn2 Mn3 C10 140.57(8) . . . . ? Mn1 Mn2 Mn3 C10 -99.83(8) 2_755 . . . ? Mn3 Mn2 Mn3 C6 84.75(9) 2_755 . . . ? Mn1 Mn2 Mn3 C6 -156.15(9) . . . . ? Mn1 Mn2 Mn3 C6 -36.55(9) 2_755 . . . ? Mn3 Mn2 Mn3 C7 163.32(12) 2_755 . . . ? Mn1 Mn2 Mn3 C7 -77.57(12) . . . . ? Mn1 Mn2 Mn3 C7 42.02(12) 2_755 . . . ? Mn3 Mn2 Mn3 C9 -38.39(8) 2_755 . . . ? Mn1 Mn2 Mn3 C9 80.72(8) . . . . ? Mn1 Mn2 Mn3 C9 -159.68(8) 2_755 . . . ? C3 Mn1 C1 C5 76.57(12) . . . . ? C2 Mn1 C1 C5 115.04(16) . . . . ? C4 Mn1 C1 C5 35.90(11) . . . . ? Mn2 Mn1 C1 C5 -139.08(11) . . . . ? C5 Mn1 C1 C2 -115.04(16) . . . . ? C3 Mn1 C1 C2 -38.46(11) . . . . ? C4 Mn1 C1 C2 -79.13(12) . . . . ? Mn2 Mn1 C1 C2 105.88(13) . . . . ? C5 Mn1 C1 C21 114.6(2) . . . . ? C3 Mn1 C1 C21 -168.85(18) . . . . ? C2 Mn1 C1 C21 -130.4(2) . . . . ? C4 Mn1 C1 C21 150.48(18) . . . . ? Mn2 Mn1 C1 C21 -24.5(2) . . . . ? C5 C1 C2 C3 1.6(2) . . . . ? C21 C1 C2 C3 -174.90(19) . . . . ? Mn1 C1 C2 C3 65.04(12) . . . . ? C5 C1 C2 C11 176.30(19) . . . . ? C21 C1 C2 C11 -0.2(4) . . . . ? Mn1 C1 C2 C11 -120.3(2) . . . . ? C5 C1 C2 Mn1 -63.42(12) . . . . ? C21 C1 C2 Mn1 120.1(2) . . . . ? C5 Mn1 C2 C3 -76.31(12) . . . . ? C4 Mn1 C2 C3 -35.39(11) . . . . ? C1 Mn1 C2 C3 -113.94(16) . . . . ? Mn2 Mn1 C2 C3 111.48(11) . . . . ? C5 Mn1 C2 C1 37.63(11) . . . . ? C3 Mn1 C2 C1 113.94(16) . . . . ? C4 Mn1 C2 C1 78.55(12) . . . . ? Mn2 Mn1 C2 C1 -134.58(10) . . . . ? C5 Mn1 C2 C11 169.01(18) . . . . ? C3 Mn1 C2 C11 -114.7(2) . . . . ? C4 Mn1 C2 C11 -150.07(18) . . . . ? C1 Mn1 C2 C11 131.4(2) . . . . ? Mn2 Mn1 C2 C11 -3.2(2) . . . . ? C1 C2 C3 C4 -1.5(2) . . . . ? C11 C2 C3 C4 -177.05(16) . . . . ? Mn1 C2 C3 C4 64.02(13) . . . . ? C1 C2 C3 Mn1 -65.52(12) . . . . ? C11 C2 C3 Mn1 118.93(16) . . . . ? C5 Mn1 C3 C4 -38.21(11) . . . . ? C2 Mn1 C3 C4 -118.76(16) . . . . ? C1 Mn1 C3 C4 -79.93(12) . . . . ? Mn2 Mn1 C3 C4 124.56(10) . . . . ? C5 Mn1 C3 C2 80.55(12) . . . . ? C4 Mn1 C3 C2 118.76(16) . . . . ? C1 Mn1 C3 C2 38.83(11) . . . . ? Mn2 Mn1 C3 C2 -116.68(11) . . . . ? C2 C3 C4 C5 0.7(2) . . . . ? Mn1 C3 C4 C5 64.01(13) . . . . ? C2 C3 C4 C41 174.95(18) . . . . ? Mn1 C3 C4 C41 -121.79(19) . . . . ? C2 C3 C4 Mn1 -63.26(13) . . . . ? C5 Mn1 C4 C3 114.46(16) . . . . ? C2 Mn1 C4 C3 36.31(11) . . . . ? C1 Mn1 C4 C3 78.27(12) . . . . ? Mn2 Mn1 C4 C3 -105.89(12) . . . . ? C3 Mn1 C4 C5 -114.46(16) . . . . ? C2 Mn1 C4 C5 -78.15(12) . . . . ? C1 Mn1 C4 C5 -36.19(11) . . . . ? Mn2 Mn1 C4 C5 139.65(10) . . . . ? C5 Mn1 C4 C41 -121.2(2) . . . . ? C3 Mn1 C4 C41 124.4(2) . . . . ? C2 Mn1 C4 C41 160.66(18) . . . . ? C1 Mn1 C4 C41 -157.37(18) . . . . ? Mn2 Mn1 C4 C41 18.5(2) . . . . ? C3 C4 C5 C1 0.3(2) . . . . ? C41 C4 C5 C1 -174.06(17) . . . . ? Mn1 C4 C5 C1 64.50(13) . . . . ? C3 C4 C5 Mn1 -64.17(13) . . . . ? C41 C4 C5 Mn1 121.44(18) . . . . ? C2 C1 C5 C4 -1.2(2) . . . . ? C21 C1 C5 C4 175.84(16) . . . . ? Mn1 C1 C5 C4 -64.55(13) . . . . ? C2 C1 C5 Mn1 63.31(12) . . . . ? C21 C1 C5 Mn1 -119.61(16) . . . . ? C3 Mn1 C5 C4 37.90(11) . . . . ? C2 Mn1 C5 C4 80.00(12) . . . . ? C1 Mn1 C5 C4 118.37(16) . . . . ? Mn2 Mn1 C5 C4 -112.52(14) . . . . ? C3 Mn1 C5 C1 -80.47(12) . . . . ? C2 Mn1 C5 C1 -38.37(11) . . . . ? C4 Mn1 C5 C1 -118.37(16) . . . . ? Mn2 Mn1 C5 C1 129.11(13) . . . . ? C3 C2 C11 C13 -147.73(18) . . . . ? C1 C2 C11 C13 38.2(3) . . . . ? Mn1 C2 C11 C13 -60.1(2) . . . . ? C3 C2 C11 C14 88.3(2) . . . . ? C1 C2 C11 C14 -85.8(3) . . . . ? Mn1 C2 C11 C14 175.94(13) . . . . ? C3 C2 C11 C12 -29.0(2) . . . . ? C1 C2 C11 C12 156.9(2) . . . . ? Mn1 C2 C11 C12 58.7(2) . . . . ? C5 C1 C21 C23 -123.87(19) . . . . ? C2 C1 C21 C23 52.3(3) . . . . ? Mn1 C1 C21 C23 148.76(14) . . . . ? C5 C1 C21 C24 -6.0(2) . . . . ? C2 C1 C21 C24 170.15(19) . . . . ? Mn1 C1 C21 C24 -93.35(18) . . . . ? C5 C1 C21 C22 111.4(2) . . . . ? C2 C1 C21 C22 -72.5(3) . . . . ? Mn1 C1 C21 C22 24.0(2) . . . . ? C3 C4 C41 C44 146.4(2) . . . . ? C5 C4 C41 C44 -40.4(3) . . . . ? Mn1 C4 C41 C44 51.9(2) . . . . ? C3 C4 C41 C42 26.1(3) . . . . ? C5 C4 C41 C42 -160.79(19) . . . . ? Mn1 C4 C41 C42 -68.5(2) . . . . ? C3 C4 C41 C43 -93.5(2) . . . . ? C5 C4 C41 C43 79.7(2) . . . . ? Mn1 C4 C41 C43 171.99(15) . . . . ? C8 Mn3 C6 C10 76.33(12) . . . . ? C7 Mn3 C6 C10 114.18(16) . . . . ? C9 Mn3 C6 C10 35.51(11) . . . . ? Mn2 Mn3 C6 C10 -109.85(12) . . . . ? C8 Mn3 C6 C7 -37.85(11) . . . . ? C10 Mn3 C6 C7 -114.18(16) . . . . ? C9 Mn3 C6 C7 -78.67(12) . . . . ? Mn2 Mn3 C6 C7 135.96(10) . . . . ? C8 Mn3 C6 C51 -169.36(19) . . . . ? C10 Mn3 C6 C51 114.3(2) . . . . ? C7 Mn3 C6 C51 -131.5(2) . . . . ? C9 Mn3 C6 C51 149.82(18) . . . . ? Mn2 Mn3 C6 C51 4.5(2) . . . . ? C10 C6 C7 C8 -1.3(2) . . . . ? C51 C6 C7 C8 -175.7(2) . . . . ? Mn3 C6 C7 C8 63.53(13) . . . . ? C10 C6 C7 C61 177.67(19) . . . . ? C51 C6 C7 C61 3.2(4) . . . . ? Mn3 C6 C7 C61 -117.5(2) . . . . ? C10 C6 C7 Mn3 -64.82(12) . . . . ? C51 C6 C7 Mn3 120.7(2) . . . . ? C10 Mn3 C7 C8 -76.59(12) . . . . ? C6 Mn3 C7 C8 -114.81(16) . . . . ? C9 Mn3 C7 C8 -35.86(11) . . . . ? Mn2 Mn3 C7 C8 129.58(12) . . . . ? C8 Mn3 C7 C6 114.81(16) . . . . ? C10 Mn3 C7 C6 38.22(11) . . . . ? C9 Mn3 C7 C6 78.94(12) . . . . ? Mn2 Mn3 C7 C6 -115.61(13) . . . . ? C8 Mn3 C7 C61 -115.2(2) . . . . ? C10 Mn3 C7 C61 168.20(18) . . . . ? C6 Mn3 C7 C61 130.0(2) . . . . ? C9 Mn3 C7 C61 -151.07(18) . . . . ? Mn2 Mn3 C7 C61 14.4(2) . . . . ? C6 C7 C8 C9 1.0(2) . . . . ? C61 C7 C8 C9 -178.07(16) . . . . ? Mn3 C7 C8 C9 64.90(13) . . . . ? C6 C7 C8 Mn3 -63.87(12) . . . . ? C61 C7 C8 Mn3 117.02(17) . . . . ? C10 Mn3 C8 C9 -37.89(11) . . . . ? C6 Mn3 C8 C9 -79.79(12) . . . . ? C7 Mn3 C8 C9 -118.21(16) . . . . ? Mn2 Mn3 C8 C9 107.70(13) . . . . ? C10 Mn3 C8 C7 80.32(12) . . . . ? C6 Mn3 C8 C7 38.42(11) . . . . ? C9 Mn3 C8 C7 118.21(16) . . . . ? Mn2 Mn3 C8 C7 -134.09(11) . . . . ? C7 C8 C9 C10 -0.4(2) . . . . ? Mn3 C8 C9 C10 64.33(13) . . . . ? C7 C8 C9 C91 177.05(17) . . . . ? Mn3 C8 C9 C91 -118.27(18) . . . . ? C7 C8 C9 Mn3 -64.68(13) . . . . ? C8 Mn3 C9 C10 -114.60(16) . . . . ? C6 Mn3 C9 C10 -36.23(11) . . . . ? C7 Mn3 C9 C10 -78.20(12) . . . . ? Mn2 Mn3 C9 C10 112.11(11) . . . . ? C10 Mn3 C9 C8 114.60(16) . . . . ? C6 Mn3 C9 C8 78.37(12) . . . . ? C7 Mn3 C9 C8 36.40(11) . . . . ? Mn2 Mn3 C9 C8 -133.30(10) . . . . ? C8 Mn3 C9 C91 121.8(2) . . . . ? C10 Mn3 C9 C91 -123.6(2) . . . . ? C6 Mn3 C9 C91 -159.83(18) . . . . ? C7 Mn3 C9 C91 158.20(18) . . . . ? Mn2 Mn3 C9 C91 -11.5(2) . . . . ? C8 C9 C10 C6 -0.5(2) . . . . ? C91 C9 C10 C6 -177.86(17) . . . . ? Mn3 C9 C10 C6 63.35(13) . . . . ? C8 C9 C10 Mn3 -63.85(13) . . . . ? C91 C9 C10 Mn3 118.78(19) . . . . ? C7 C6 C10 C9 1.1(2) . . . . ? C51 C6 C10 C9 176.52(16) . . . . ? Mn3 C6 C10 C9 -63.82(13) . . . . ? C7 C6 C10 Mn3 64.95(12) . . . . ? C51 C6 C10 Mn3 -119.66(17) . . . . ? C8 Mn3 C10 C9 38.04(11) . . . . ? C6 Mn3 C10 C9 118.67(16) . . . . ? C7 Mn3 C10 C9 79.93(12) . . . . ? Mn2 Mn3 C10 C9 -117.56(11) . . . . ? C8 Mn3 C10 C6 -80.63(12) . . . . ? C7 Mn3 C10 C6 -38.74(11) . . . . ? C9 Mn3 C10 C6 -118.67(16) . . . . ? Mn2 Mn3 C10 C6 123.77(10) . . . . ? C10 C6 C51 C52 145.66(19) . . . . ? C7 C6 C51 C52 -40.5(3) . . . . ? Mn3 C6 C51 C52 57.8(2) . . . . ? C10 C6 C51 C54 -90.5(2) . . . . ? C7 C6 C51 C54 83.4(3) . . . . ? Mn3 C6 C51 C54 -178.30(14) . . . . ? C10 C6 C51 C53 26.9(2) . . . . ? C7 C6 C51 C53 -159.2(2) . . . . ? Mn3 C6 C51 C53 -60.9(2) . . . . ? C8 C7 C61 C63 126.8(2) . . . . ? C6 C7 C61 C63 -52.1(3) . . . . ? Mn3 C7 C61 C63 -146.94(15) . . . . ? C8 C7 C61 C64 8.7(2) . . . . ? C6 C7 C61 C64 -170.1(2) . . . . ? Mn3 C7 C61 C64 95.02(18) . . . . ? C8 C7 C61 C62 -108.7(2) . . . . ? C6 C7 C61 C62 72.5(3) . . . . ? Mn3 C7 C61 C62 -22.4(2) . . . . ? C10 C9 C91 C93 -24.6(3) . . . . ? C8 C9 C91 C93 158.54(19) . . . . ? Mn3 C9 C91 C93 67.9(2) . . . . ? C10 C9 C91 C92 -144.55(19) . . . . ? C8 C9 C91 C92 38.6(3) . . . . ? Mn3 C9 C91 C92 -52.1(2) . . . . ? C10 C9 C91 C94 95.2(2) . . . . ? C8 C9 C91 C94 -81.6(2) . . . . ? Mn3 C9 C91 C94 -172.31(14) . . . . ? C100 C101 C102 C103 -178.5(2) . . . . ? C101 C102 C103 C104 173.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 68.22 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.442 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.052 data_mima15 _database_code_depnum_ccdc_archive 'CCDC 871127' #TrackingRef 'mima15.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H146 Mn5' _chemical_formula_weight 1358.65 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' 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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.4840(4) _cell_length_b 12.7411(2) _cell_length_c 25.2730(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.331(2) _cell_angle_gamma 90.00 _cell_volume 8064.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 53670 _cell_measurement_theta_min 2.2670 _cell_measurement_theta_max 32.6472 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2956 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97390 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 224740 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 31.00 _reflns_number_total 12829 _reflns_number_gt 8779 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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. The hydrogens at the atoms C3, C5, C20 and C22 were located in difference syntheses and refined freely, as were the hydrogens at the Mn atom. The methyl hydrogens were located in difference syntheses and refined as idealised rigid groups allowed to rotate but not tip. ; _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^)+(0.0306P)^2^] 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 12829 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _refine_ls_shift/su_max 0.007 _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 1.0000 0.198218(17) 0.2500 0.01103(5) Uani 1 2 d S . . H01 H 1.0370(6) 0.1975(11) 0.3155(6) 0.050(4) Uiso 1 1 d . . . H02 H 1.0521(5) 0.1970(10) 0.2369(6) 0.043(4) Uiso 1 1 d . . . H03 H 1.0000 0.0771(15) 0.2500 0.047(6) Uiso 1 2 d S . . H04 H 1.0000 0.3230(16) 0.2500 0.056(7) Uiso 1 2 d S . . Mn2 Mn 1.079259(6) 0.084224(13) 0.298521(7) 0.01629(4) Uani 1 1 d . . . Mn3 Mn 1.016453(7) 0.311649(13) 0.179190(7) 0.01637(4) Uani 1 1 d . . . C1 C 1.14848(4) -0.01488(8) 0.29006(5) 0.0159(2) Uani 1 1 d . . . C2 C 1.17177(4) 0.04472(8) 0.34370(5) 0.0164(2) Uani 1 1 d . . . C3 C 1.14701(4) 0.00734(8) 0.37982(5) 0.0160(2) Uani 1 1 d . . . H3 H 1.1529(4) 0.0312(9) 0.4163(5) 0.018(3) Uiso 1 1 d . . . C4 C 1.11041(4) -0.07386(8) 0.35196(4) 0.0148(2) Uani 1 1 d . . . C5 C 1.11181(4) -0.08701(9) 0.29724(5) 0.0156(2) Uani 1 1 d . . . H5 H 1.0911(5) -0.1354(10) 0.2687(5) 0.020(3) Uiso 1 1 d . . . C6 C 1.15889(5) -0.01939(9) 0.23456(5) 0.0217(2) Uani 1 1 d . . . C7 C 1.20612(5) -0.09428(10) 0.24526(6) 0.0307(3) Uani 1 1 d . . . H7A H 1.2385 -0.0658 0.2761 0.037 Uiso 1 1 calc R . . H7B H 1.2116 -0.1014 0.2095 0.037 Uiso 1 1 calc R . . H7C H 1.1983 -0.1633 0.2570 0.037 Uiso 1 1 calc R . . C8 C 1.10962(5) -0.06509(11) 0.18413(5) 0.0305(3) Uani 1 1 d . . . H8A H 1.1155 -0.0637 0.1484 0.037 Uiso 1 1 calc R . . H8B H 1.0781 -0.0230 0.1787 0.037 Uiso 1 1 calc R . . H8C H 1.1040 -0.1377 0.1932 0.037 Uiso 1 1 calc R . . C9 C 1.16922(5) 0.08705(10) 0.21295(5) 0.0281(3) Uani 1 1 d . . . H9A H 1.2025 0.1168 0.2416 0.034 Uiso 1 1 calc R . . H9B H 1.1396 0.1348 0.2075 0.034 Uiso 1 1 calc R . . H9C H 1.1722 0.0777 0.1759 0.034 Uiso 1 1 calc R . . C10 C 1.21472(4) 0.13100(9) 0.36531(5) 0.0216(2) Uani 1 1 d . . . C11 C 1.19395(5) 0.23630(9) 0.33416(6) 0.0276(3) Uani 1 1 d . . . H11A H 1.1820 0.2268 0.2922 0.033 Uiso 1 1 calc R . . H11B H 1.2227 0.2885 0.3481 0.033 Uiso 1 1 calc R . . H11C H 1.1639 0.2606 0.3424 0.033 Uiso 1 1 calc R . . C12 C 1.26611(5) 0.09804(10) 0.35964(6) 0.0287(3) Uani 1 1 d . . . H12A H 1.2785 0.0306 0.3792 0.034 Uiso 1 1 calc R . . H12B H 1.2937 0.1514 0.3776 0.034 Uiso 1 1 calc R . . H12C H 1.2589 0.0911 0.3185 0.034 Uiso 1 1 calc R . . C13 C 1.23054(5) 0.15222(10) 0.43025(5) 0.0291(3) Uani 1 1 d . . . H13A H 1.1990 0.1750 0.4361 0.035 Uiso 1 1 calc R . . H13B H 1.2578 0.2073 0.4436 0.035 Uiso 1 1 calc R . . H13C H 1.2448 0.0878 0.4524 0.035 Uiso 1 1 calc R . . C14 C 1.07822(4) -0.13620(8) 0.37769(5) 0.0167(2) Uani 1 1 d . . . C15 C 1.11338(5) -0.22396(10) 0.41620(6) 0.0298(3) Uani 1 1 d . . . H15A H 1.1252 -0.2701 0.3928 0.036 Uiso 1 1 calc R . . H15B H 1.0928 -0.2648 0.4327 0.036 Uiso 1 1 calc R . . H15C H 1.1446 -0.1930 0.4477 0.036 Uiso 1 1 calc R . . C16 C 1.05924(5) -0.06459(9) 0.41375(5) 0.0248(3) Uani 1 1 d . . . H16A H 1.0902 -0.0350 0.4460 0.030 Uiso 1 1 calc R . . H16B H 1.0376 -0.1052 0.4291 0.030 Uiso 1 1 calc R . . H16C H 1.0376 -0.0076 0.3893 0.030 Uiso 1 1 calc R . . C17 C 1.02913(5) -0.18638(10) 0.33002(5) 0.0265(3) Uani 1 1 d . . . H17A H 1.0061 -0.1313 0.3051 0.032 Uiso 1 1 calc R . . H17B H 1.0093 -0.2265 0.3478 0.032 Uiso 1 1 calc R . . H17C H 1.0405 -0.2334 0.3066 0.032 Uiso 1 1 calc R . . C18 C 1.01594(4) 0.34906(8) 0.08673(4) 0.0154(2) Uani 1 1 d . . . C19 C 0.97318(4) 0.40762(8) 0.09245(4) 0.0146(2) Uani 1 1 d . . . C20 C 0.99805(4) 0.48097(8) 0.13858(5) 0.0148(2) Uani 1 1 d . . . H20 H 0.9800(4) 0.5310(9) 0.1520(5) 0.014(3) Uiso 1 1 d . . . C21 C 1.05403(4) 0.46944(8) 0.16246(4) 0.0146(2) Uani 1 1 d . . . C22 C 1.06450(4) 0.38794(8) 0.13069(5) 0.0154(2) Uani 1 1 d . . . H22 H 1.0996(5) 0.3654(9) 0.1374(5) 0.017(3) Uiso 1 1 d . . . C23 C 1.01753(5) 0.26452(9) 0.04379(5) 0.0199(2) Uani 1 1 d . . . C24 C 1.07557(5) 0.24410(10) 0.05271(5) 0.0253(3) Uani 1 1 d . . . H24A H 1.0958 0.2161 0.0918 0.030 Uiso 1 1 calc R . . H24B H 1.0918 0.3100 0.0482 0.030 Uiso 1 1 calc R . . H24C H 1.0760 0.1932 0.0238 0.030 Uiso 1 1 calc R . . C25 C 0.99625(5) 0.15769(9) 0.05334(5) 0.0276(3) Uani 1 1 d . . . H25A H 1.0177 0.1332 0.0929 0.033 Uiso 1 1 calc R . . H25B H 0.9985 0.1066 0.0254 0.033 Uiso 1 1 calc R . . H25C H 0.9589 0.1652 0.0477 0.033 Uiso 1 1 calc R . . C26 C 0.98732(5) 0.30171(10) -0.01940(5) 0.0256(3) Uani 1 1 d . . . H26A H 0.9925 0.2508 -0.0457 0.031 Uiso 1 1 calc R . . H26B H 1.0011 0.3703 -0.0243 0.031 Uiso 1 1 calc R . . H26C H 0.9492 0.3077 -0.0284 0.031 Uiso 1 1 calc R . . C27 C 0.91206(4) 0.40922(9) 0.05797(5) 0.0193(2) Uani 1 1 d . . . C28 C 0.88684(5) 0.30177(9) 0.03628(5) 0.0251(3) Uani 1 1 d . . . H28A H 0.8996 0.2745 0.0080 0.030 Uiso 1 1 calc R . . H28B H 0.8479 0.3088 0.0178 0.030 Uiso 1 1 calc R . . H28C H 0.8969 0.2532 0.0691 0.030 Uiso 1 1 calc R . . C29 C 0.89754(5) 0.48512(10) 0.00656(5) 0.0270(3) Uani 1 1 d . . . H29A H 0.9142 0.4613 -0.0190 0.032 Uiso 1 1 calc R . . H29B H 0.9105 0.5556 0.0211 0.032 Uiso 1 1 calc R . . H29C H 0.8587 0.4869 -0.0152 0.032 Uiso 1 1 calc R . . C30 C 0.88513(5) 0.45037(10) 0.09676(6) 0.0281(3) Uani 1 1 d . . . H30A H 0.8462 0.4458 0.0756 0.034 Uiso 1 1 calc R . . H30B H 0.8955 0.5236 0.1072 0.034 Uiso 1 1 calc R . . H30C H 0.8966 0.4077 0.1321 0.034 Uiso 1 1 calc R . . C31 C 1.09582(4) 0.53618(9) 0.20892(5) 0.0188(2) Uani 1 1 d . . . C32 C 1.14373(5) 0.46989(11) 0.24715(6) 0.0396(4) Uani 1 1 d . . . H32A H 1.1319 0.4147 0.2662 0.047 Uiso 1 1 calc R . . H32B H 1.1700 0.5146 0.2767 0.047 Uiso 1 1 calc R . . H32C H 1.1600 0.4378 0.2231 0.047 Uiso 1 1 calc R . . C33 C 1.11408(6) 0.62150(11) 0.17835(6) 0.0375(3) Uani 1 1 d . . . H33A H 1.1288 0.5885 0.1531 0.045 Uiso 1 1 calc R . . H33B H 1.1416 0.6649 0.2075 0.045 Uiso 1 1 calc R . . H33C H 1.0835 0.6656 0.1550 0.045 Uiso 1 1 calc R . . C34 C 1.07284(5) 0.58854(10) 0.24801(5) 0.0271(3) Uani 1 1 d . . . H34A H 1.0423 0.6324 0.2244 0.032 Uiso 1 1 calc R . . H34B H 1.1003 0.6323 0.2769 0.032 Uiso 1 1 calc R . . H34C H 1.0611 0.5345 0.2678 0.032 Uiso 1 1 calc R . . C35 C 0.82201(6) 0.07848(10) 0.93871(6) 0.0351(3) Uani 1 1 d . . . H35A H 0.8269 0.0841 0.9793 0.042 Uiso 1 1 calc R . . H35B H 0.8151 0.1483 0.9208 0.042 Uiso 1 1 calc R . . H35C H 0.8544 0.0494 0.9372 0.042 Uiso 1 1 calc R . . C36 C 0.77521(5) 0.00709(10) 0.90601(6) 0.0325(3) Uani 1 1 d . . . H36A H 0.7432 0.0343 0.9101 0.039 Uiso 1 1 calc R . . H36B H 0.7679 0.0086 0.8642 0.039 Uiso 1 1 calc R . . C37 C 0.78457(5) -0.10516(10) 0.92706(6) 0.0341(3) Uani 1 1 d . . . H37A H 0.8188 -0.1293 0.9271 0.041 Uiso 1 1 calc R . . H37B H 0.7882 -0.1071 0.9677 0.041 Uiso 1 1 calc R . . C38 C 0.74128(6) -0.18081(12) 0.89151(8) 0.0490(4) Uani 1 1 d . . . H38A H 0.7367 -0.1774 0.8506 0.059 Uiso 1 1 calc R . . H38B H 0.7072 -0.1586 0.8927 0.059 Uiso 1 1 calc R . . C39 C 0.75270(7) -0.29391(12) 0.91239(8) 0.0556(5) Uani 1 1 d . . . H39A H 0.7852 -0.3181 0.9092 0.067 Uiso 1 1 calc R . . H39B H 0.7226 -0.3385 0.8884 0.067 Uiso 1 1 calc R . . H39C H 0.7576 -0.2980 0.9530 0.067 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 0.01196(11) 0.01003(10) 0.01157(10) 0.000 0.00532(9) 0.000 Mn2 0.01376(8) 0.01498(8) 0.01916(8) 0.00320(7) 0.00582(7) 0.00325(7) Mn3 0.02080(9) 0.01518(8) 0.01522(8) 0.00307(7) 0.00954(7) -0.00072(7) C1 0.0142(5) 0.0157(5) 0.0192(5) 0.0035(4) 0.0082(4) 0.0044(4) C2 0.0123(5) 0.0147(5) 0.0210(6) 0.0025(4) 0.0055(4) 0.0031(4) C3 0.0160(5) 0.0159(5) 0.0137(5) 0.0007(4) 0.0036(4) 0.0027(4) C4 0.0151(5) 0.0133(5) 0.0157(5) 0.0027(4) 0.0059(4) 0.0035(4) C5 0.0161(5) 0.0140(5) 0.0158(5) 0.0002(4) 0.0059(4) 0.0021(4) C6 0.0248(6) 0.0220(6) 0.0243(6) 0.0023(5) 0.0162(5) 0.0018(5) C7 0.0342(7) 0.0289(7) 0.0391(7) 0.0012(6) 0.0252(6) 0.0055(6) C8 0.0373(8) 0.0378(8) 0.0211(6) -0.0020(5) 0.0168(6) -0.0040(6) C9 0.0342(7) 0.0281(7) 0.0283(6) 0.0053(5) 0.0193(6) 0.0017(6) C10 0.0140(5) 0.0202(6) 0.0284(6) 0.0008(5) 0.0065(5) -0.0004(5) C11 0.0231(6) 0.0174(6) 0.0394(7) -0.0010(5) 0.0100(6) -0.0028(5) C12 0.0147(6) 0.0292(7) 0.0407(8) 0.0018(6) 0.0097(5) -0.0007(5) C13 0.0194(6) 0.0314(7) 0.0308(7) -0.0058(6) 0.0046(5) -0.0071(5) C14 0.0205(6) 0.0145(5) 0.0163(5) 0.0014(4) 0.0089(5) -0.0001(4) C15 0.0355(7) 0.0239(6) 0.0343(7) 0.0124(5) 0.0187(6) 0.0066(6) C16 0.0332(7) 0.0216(6) 0.0271(6) -0.0027(5) 0.0199(6) -0.0031(5) C17 0.0285(7) 0.0305(7) 0.0251(6) -0.0038(5) 0.0157(5) -0.0100(6) C18 0.0219(6) 0.0130(5) 0.0141(5) 0.0030(4) 0.0102(5) 0.0006(4) C19 0.0157(5) 0.0144(5) 0.0136(5) 0.0033(4) 0.0059(4) -0.0015(4) C20 0.0163(5) 0.0118(5) 0.0177(5) 0.0024(4) 0.0083(4) 0.0004(4) C21 0.0163(5) 0.0125(5) 0.0157(5) 0.0021(4) 0.0072(4) -0.0005(4) C22 0.0160(5) 0.0161(5) 0.0168(5) 0.0033(4) 0.0094(4) 0.0015(4) C23 0.0288(6) 0.0170(5) 0.0159(5) 0.0002(4) 0.0113(5) 0.0020(5) C24 0.0325(7) 0.0262(6) 0.0212(6) 0.0000(5) 0.0152(5) 0.0073(5) C25 0.0388(8) 0.0164(6) 0.0283(7) -0.0028(5) 0.0147(6) -0.0018(5) C26 0.0330(7) 0.0285(7) 0.0161(5) -0.0016(5) 0.0109(5) 0.0023(6) C27 0.0167(5) 0.0190(6) 0.0192(5) 0.0006(5) 0.0043(4) -0.0022(5) C28 0.0190(6) 0.0248(6) 0.0272(6) -0.0008(5) 0.0051(5) -0.0061(5) C29 0.0225(6) 0.0261(6) 0.0245(6) 0.0055(5) 0.0019(5) 0.0005(5) C30 0.0168(6) 0.0337(7) 0.0334(7) -0.0036(6) 0.0100(5) -0.0013(5) C31 0.0159(5) 0.0172(5) 0.0204(6) -0.0024(4) 0.0047(5) -0.0015(4) C32 0.0249(7) 0.0339(8) 0.0413(8) -0.0132(7) -0.0052(6) 0.0074(6) C33 0.0406(8) 0.0347(8) 0.0389(8) -0.0082(6) 0.0182(7) -0.0234(7) C34 0.0254(6) 0.0291(7) 0.0223(6) -0.0087(5) 0.0053(5) -0.0004(5) C35 0.0422(8) 0.0305(7) 0.0315(7) 0.0013(6) 0.0140(6) 0.0038(6) C36 0.0318(7) 0.0308(7) 0.0363(8) 0.0045(6) 0.0154(6) 0.0056(6) C37 0.0333(7) 0.0322(7) 0.0366(8) 0.0034(6) 0.0141(6) 0.0006(6) C38 0.0352(8) 0.0414(9) 0.0659(11) 0.0021(8) 0.0165(8) -0.0090(7) C39 0.0507(10) 0.0343(9) 0.0805(13) -0.0055(9) 0.0257(10) -0.0128(8) _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 Mn2 2.4814(2) . ? Mn1 Mn2 2.4815(2) 2_755 ? Mn1 Mn3 2.4823(2) 2_755 ? Mn1 Mn3 2.4825(2) . ? Mn1 H01 1.546(14) . ? Mn1 H02 1.596(14) . ? Mn1 H03 1.54(2) . ? Mn1 H04 1.59(2) . ? Mn2 C3 2.3444(11) . ? Mn2 C5 2.3633(11) . ? Mn2 C1 2.3654(11) . ? Mn2 C2 2.3726(10) . ? Mn2 C4 2.3793(10) . ? Mn2 H01 2.008(14) . ? Mn2 H02 2.022(13) . ? Mn2 H03 2.0140(9) . ? Mn3 C22 2.3506(11) . ? Mn3 C20 2.3528(11) . ? Mn3 C19 2.3594(10) . ? Mn3 C21 2.3764(10) . ? Mn3 C18 2.3792(10) . ? Mn3 H02 2.011(13) . ? Mn3 H04 2.0235(15) . ? C1 C5 1.4297(15) . ? C1 C2 1.4525(15) . ? C1 C6 1.5436(16) . ? C2 C3 1.4266(16) . ? C2 C10 1.5392(15) . ? C3 C4 1.4121(15) . ? C3 H3 0.920(12) . ? C4 C5 1.4092(15) . ? C4 C14 1.5201(15) . ? C5 H5 0.942(12) . ? C6 C9 1.5316(16) . ? C6 C8 1.5411(17) . ? C6 C7 1.5423(17) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.5356(16) . ? C10 C13 1.5387(17) . ? C10 C11 1.5412(16) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.5254(16) . ? C14 C17 1.5301(16) . ? C14 C15 1.5350(16) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C22 1.4279(15) . ? C18 C19 1.4489(15) . ? C18 C23 1.5424(15) . ? C19 C20 1.4295(15) . ? C19 C27 1.5411(15) . ? C20 C21 1.4099(15) . ? C20 H20 0.951(12) . ? C21 C22 1.4129(15) . ? C21 C31 1.5196(15) . ? C22 H22 0.953(12) . ? C23 C24 1.5384(17) . ? C23 C25 1.5392(16) . ? C23 C26 1.5399(15) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.5303(16) . ? C27 C29 1.5345(16) . ? C27 C30 1.5435(17) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.5272(17) . ? C31 C34 1.5276(16) . ? C31 C33 1.5332(17) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.5131(18) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.5105(18) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.507(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.522(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 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 Mn2 Mn1 Mn2 108.349(11) . 2_755 ? Mn2 Mn1 Mn3 111.595(6) . 2_755 ? Mn2 Mn1 Mn3 108.270(6) 2_755 2_755 ? Mn2 Mn1 Mn3 108.268(6) . . ? Mn2 Mn1 Mn3 111.596(6) 2_755 . ? Mn3 Mn1 Mn3 108.792(11) 2_755 . ? Mn2 Mn1 H01 53.9(5) . . ? Mn2 Mn1 H01 125.6(5) 2_755 . ? Mn3 Mn1 H01 57.7(5) 2_755 . ? Mn3 Mn1 H01 122.8(5) . . ? Mn2 Mn1 H02 54.3(5) . . ? Mn2 Mn1 H02 124.8(5) 2_755 . ? Mn3 Mn1 H02 126.9(5) 2_755 . ? Mn3 Mn1 H02 53.9(5) . . ? H01 Mn1 H02 88.4(7) . . ? Mn2 Mn1 H03 54.174(6) . . ? Mn2 Mn1 H03 54.174(6) 2_755 . ? Mn3 Mn1 H03 125.604(6) 2_755 . ? Mn3 Mn1 H03 125.604(6) . . ? H01 Mn1 H03 89.7(5) . . ? H02 Mn1 H03 89.4(5) . . ? Mn2 Mn1 H04 125.826(7) . . ? Mn2 Mn1 H04 125.826(6) 2_755 . ? Mn3 Mn1 H04 54.396(6) 2_755 . ? Mn3 Mn1 H04 54.396(6) . . ? H01 Mn1 H04 90.3(5) . . ? H02 Mn1 H04 90.6(5) . . ? H03 Mn1 H04 180.000(4) . . ? C3 Mn2 C5 57.16(4) . . ? C3 Mn2 C1 58.55(4) . . ? C5 Mn2 C1 35.20(4) . . ? C3 Mn2 C2 35.20(4) . . ? C5 Mn2 C2 58.27(4) . . ? C1 Mn2 C2 35.70(4) . . ? C3 Mn2 C4 34.78(4) . . ? C5 Mn2 C4 34.57(4) . . ? C1 Mn2 C4 58.98(4) . . ? C2 Mn2 C4 58.91(4) . . ? C3 Mn2 Mn1 153.67(3) . . ? C5 Mn2 Mn1 142.54(3) . . ? C1 Mn2 Mn1 147.44(3) . . ? C2 Mn2 Mn1 155.57(3) . . ? C4 Mn2 Mn1 144.42(3) . . ? C3 Mn2 H01 115.7(4) . . ? C5 Mn2 H01 157.3(4) . . ? C1 Mn2 H01 164.0(4) . . ? C2 Mn2 H01 130.5(4) . . ? C4 Mn2 H01 126.3(4) . . ? Mn1 Mn2 H01 38.5(4) . . ? C3 Mn2 H02 151.6(4) . . ? C5 Mn2 H02 131.9(4) . . ? C1 Mn2 H02 111.4(4) . . ? C2 Mn2 H02 120.3(4) . . ? C4 Mn2 H02 166.2(4) . . ? Mn1 Mn2 H02 39.9(4) . . ? H01 Mn2 H02 65.9(6) . . ? C3 Mn2 H03 141.6(4) . . ? C5 Mn2 H03 105.7(5) . . ? C1 Mn2 H03 129.0(4) . . ? C2 Mn2 H03 163.6(5) . . ? C4 Mn2 H03 110.7(5) . . ? Mn1 Mn2 H03 38.4(6) . . ? H01 Mn2 H03 65.6(6) . . ? H02 Mn2 H03 66.4(6) . . ? C22 Mn3 C20 57.27(4) . . ? C22 Mn3 C19 58.51(4) . . ? C20 Mn3 C19 35.32(4) . . ? C22 Mn3 C21 34.78(4) . . ? C20 Mn3 C21 34.69(4) . . ? C19 Mn3 C21 59.07(4) . . ? C22 Mn3 C18 35.14(4) . . ? C20 Mn3 C18 58.31(4) . . ? C19 Mn3 C18 35.60(4) . . ? C21 Mn3 C18 58.86(4) . . ? C22 Mn3 Mn1 157.67(3) . . ? C20 Mn3 Mn1 141.08(3) . . ? C19 Mn3 Mn1 143.10(3) . . ? C21 Mn3 Mn1 147.39(3) . . ? C18 Mn3 Mn1 153.58(3) . . ? C22 Mn3 H02 117.9(4) . . ? C20 Mn3 H02 159.3(4) . . ? C19 Mn3 H02 163.5(4) . . ? C21 Mn3 H02 128.8(4) . . ? C18 Mn3 H02 131.5(4) . . ? Mn1 Mn3 H02 39.9(4) . . ? C22 Mn3 H04 144.1(5) . . ? C20 Mn3 H04 103.5(6) . . ? C19 Mn3 H04 125.0(4) . . ? C21 Mn3 H04 111.7(6) . . ? C18 Mn3 H04 160.3(5) . . ? Mn1 Mn3 H04 39.7(6) . . ? H02 Mn3 H04 68.3(6) . . ? C5 C1 C2 106.26(9) . . ? C5 C1 C6 119.72(10) . . ? C2 C1 C6 133.81(10) . . ? C5 C1 Mn2 72.32(6) . . ? C2 C1 Mn2 72.42(6) . . ? C6 C1 Mn2 123.99(7) . . ? C3 C2 C1 106.25(9) . . ? C3 C2 C10 120.65(10) . . ? C1 C2 C10 133.09(10) . . ? C3 C2 Mn2 71.32(6) . . ? C1 C2 Mn2 71.88(6) . . ? C10 C2 Mn2 122.17(7) . . ? C4 C3 C2 110.80(10) . . ? C4 C3 Mn2 73.96(6) . . ? C2 C3 Mn2 73.48(6) . . ? C4 C3 H3 122.5(7) . . ? C2 C3 H3 126.7(7) . . ? Mn2 C3 H3 119.3(7) . . ? C5 C4 C3 105.94(10) . . ? C5 C4 C14 127.86(10) . . ? C3 C4 C14 126.15(10) . . ? C5 C4 Mn2 72.10(6) . . ? C3 C4 Mn2 71.26(6) . . ? C14 C4 Mn2 123.26(7) . . ? C4 C5 C1 110.73(10) . . ? C4 C5 Mn2 73.34(6) . . ? C1 C5 Mn2 72.48(6) . . ? C4 C5 H5 125.4(7) . . ? C1 C5 H5 123.9(7) . . ? Mn2 C5 H5 120.2(7) . . ? C9 C6 C8 105.57(10) . . ? C9 C6 C7 110.12(10) . . ? C8 C6 C7 107.49(10) . . ? C9 C6 C1 114.96(10) . . ? C8 C6 C1 109.68(9) . . ? C7 C6 C1 108.74(9) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C13 106.33(10) . . ? C12 C10 C2 111.84(10) . . ? C13 C10 C2 110.01(10) . . ? C12 C10 C11 110.60(10) . . ? C13 C10 C11 105.91(10) . . ? C2 C10 C11 111.83(9) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C4 C14 C16 110.22(9) . . ? C4 C14 C17 111.17(9) . . ? C16 C14 C17 108.22(10) . . ? C4 C14 C15 109.06(9) . . ? C16 C14 C15 109.74(9) . . ? C17 C14 C15 108.38(10) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C22 C18 C19 106.28(9) . . ? C22 C18 C23 120.10(10) . . ? C19 C18 C23 133.56(10) . . ? C22 C18 Mn3 71.33(6) . . ? C19 C18 Mn3 71.45(6) . . ? C23 C18 Mn3 124.11(7) . . ? C20 C19 C18 106.44(9) . . ? C20 C19 C27 119.75(9) . . ? C18 C19 C27 133.66(10) . . ? C20 C19 Mn3 72.09(6) . . ? C18 C19 Mn3 72.94(6) . . ? C27 C19 Mn3 123.17(7) . . ? C21 C20 C19 110.60(10) . . ? C21 C20 Mn3 73.57(6) . . ? C19 C20 Mn3 72.59(6) . . ? C21 C20 H20 123.6(7) . . ? C19 C20 H20 125.8(7) . . ? Mn3 C20 H20 120.6(7) . . ? C20 C21 C22 105.97(9) . . ? C20 C21 C31 128.05(10) . . ? C22 C21 C31 125.76(10) . . ? C20 C21 Mn3 71.74(6) . . ? C22 C21 Mn3 71.61(6) . . ? C31 C21 Mn3 125.55(7) . . ? C21 C22 C18 110.69(10) . . ? C21 C22 Mn3 73.61(6) . . ? C18 C22 Mn3 73.53(6) . . ? C21 C22 H22 123.3(7) . . ? C18 C22 H22 125.9(7) . . ? Mn3 C22 H22 121.9(7) . . ? C24 C23 C25 105.39(10) . . ? C24 C23 C26 106.71(9) . . ? C25 C23 C26 110.94(10) . . ? C24 C23 C18 110.06(9) . . ? C25 C23 C18 112.61(9) . . ? C26 C23 C18 110.81(9) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 109.82(9) . . ? C28 C27 C19 114.71(9) . . ? C29 C27 C19 109.26(9) . . ? C28 C27 C30 105.45(9) . . ? C29 C27 C30 107.34(10) . . ? C19 C27 C30 109.97(9) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C21 C31 C32 111.07(9) . . ? C21 C31 C34 111.21(9) . . ? C32 C31 C34 108.12(10) . . ? C21 C31 C33 107.90(9) . . ? C32 C31 C33 109.57(11) . . ? C34 C31 C33 108.95(10) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C35 113.18(11) . . ? C37 C36 H36A 108.9 . . ? C35 C36 H36A 108.9 . . ? C37 C36 H36B 108.9 . . ? C35 C36 H36B 108.9 . . ? H36A C36 H36B 107.8 . . ? C38 C37 C36 114.67(12) . . ? C38 C37 H37A 108.6 . . ? C36 C37 H37A 108.6 . . ? C38 C37 H37B 108.6 . . ? C36 C37 H37B 108.6 . . ? H37A C37 H37B 107.6 . . ? C37 C38 C39 113.53(13) . . ? C37 C38 H38A 108.9 . . ? C39 C38 H38A 108.9 . . ? C37 C38 H38B 108.9 . . ? C39 C38 H38B 108.9 . . ? H38A C38 H38B 107.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? 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 Mn2 Mn1 Mn2 C3 -107.26(6) 2_755 . . . ? Mn3 Mn1 Mn2 C3 11.85(7) 2_755 . . . ? Mn3 Mn1 Mn2 C3 131.55(6) . . . . ? Mn2 Mn1 Mn2 C5 21.59(4) 2_755 . . . ? Mn3 Mn1 Mn2 C5 140.70(4) 2_755 . . . ? Mn3 Mn1 Mn2 C5 -99.60(5) . . . . ? Mn2 Mn1 Mn2 C1 84.67(5) 2_755 . . . ? Mn3 Mn1 Mn2 C1 -156.22(5) 2_755 . . . ? Mn3 Mn1 Mn2 C1 -36.52(5) . . . . ? Mn2 Mn1 Mn2 C2 163.08(7) 2_755 . . . ? Mn3 Mn1 Mn2 C2 -77.81(7) 2_755 . . . ? Mn3 Mn1 Mn2 C2 41.90(7) . . . . ? Mn2 Mn1 Mn2 C4 -38.24(4) 2_755 . . . ? Mn3 Mn1 Mn2 C4 80.87(5) 2_755 . . . ? Mn3 Mn1 Mn2 C4 -159.43(5) . . . . ? Mn2 Mn1 Mn3 C22 -7.58(7) . . . . ? Mn2 Mn1 Mn3 C22 -126.74(7) 2_755 . . . ? Mn3 Mn1 Mn3 C22 113.87(7) 2_755 . . . ? Mn2 Mn1 Mn3 C20 -146.16(4) . . . . ? Mn2 Mn1 Mn3 C20 94.68(4) 2_755 . . . ? Mn3 Mn1 Mn3 C20 -24.72(4) 2_755 . . . ? Mn2 Mn1 Mn3 C19 154.75(4) . . . . ? Mn2 Mn1 Mn3 C19 35.59(5) 2_755 . . . ? Mn3 Mn1 Mn3 C19 -83.81(4) 2_755 . . . ? Mn2 Mn1 Mn3 C21 -85.70(5) . . . . ? Mn2 Mn1 Mn3 C21 155.14(5) 2_755 . . . ? Mn3 Mn1 Mn3 C21 35.75(5) 2_755 . . . ? Mn2 Mn1 Mn3 C18 86.02(6) . . . . ? Mn2 Mn1 Mn3 C18 -33.14(6) 2_755 . . . ? Mn3 Mn1 Mn3 C18 -152.54(6) 2_755 . . . ? C3 Mn2 C1 C5 76.37(7) . . . . ? C2 Mn2 C1 C5 114.16(9) . . . . ? C4 Mn2 C1 C5 35.46(6) . . . . ? Mn1 Mn2 C1 C5 -109.80(7) . . . . ? C3 Mn2 C1 C2 -37.79(6) . . . . ? C5 Mn2 C1 C2 -114.16(9) . . . . ? C4 Mn2 C1 C2 -78.71(6) . . . . ? Mn1 Mn2 C1 C2 136.04(6) . . . . ? C3 Mn2 C1 C6 -169.26(11) . . . . ? C5 Mn2 C1 C6 114.37(11) . . . . ? C2 Mn2 C1 C6 -131.47(12) . . . . ? C4 Mn2 C1 C6 149.83(10) . . . . ? Mn1 Mn2 C1 C6 4.57(12) . . . . ? C5 C1 C2 C3 -1.41(11) . . . . ? C6 C1 C2 C3 -175.93(11) . . . . ? Mn2 C1 C2 C3 63.48(7) . . . . ? C5 C1 C2 C10 177.65(11) . . . . ? C6 C1 C2 C10 3.1(2) . . . . ? Mn2 C1 C2 C10 -117.46(12) . . . . ? C5 C1 C2 Mn2 -64.89(7) . . . . ? C6 C1 C2 Mn2 120.58(12) . . . . ? C5 Mn2 C2 C3 -76.74(7) . . . . ? C1 Mn2 C2 C3 -114.93(9) . . . . ? C4 Mn2 C2 C3 -36.00(6) . . . . ? Mn1 Mn2 C2 C3 129.70(7) . . . . ? C3 Mn2 C2 C1 114.93(9) . . . . ? C5 Mn2 C2 C1 38.19(6) . . . . ? C4 Mn2 C2 C1 78.93(6) . . . . ? Mn1 Mn2 C2 C1 -115.38(7) . . . . ? C3 Mn2 C2 C10 -115.03(11) . . . . ? C5 Mn2 C2 C10 168.23(10) . . . . ? C1 Mn2 C2 C10 130.04(12) . . . . ? C4 Mn2 C2 C10 -151.03(10) . . . . ? Mn1 Mn2 C2 C10 14.66(14) . . . . ? C1 C2 C3 C4 1.25(12) . . . . ? C10 C2 C3 C4 -177.95(9) . . . . ? Mn2 C2 C3 C4 65.11(8) . . . . ? C1 C2 C3 Mn2 -63.86(7) . . . . ? C10 C2 C3 Mn2 116.94(9) . . . . ? C5 Mn2 C3 C4 -37.92(6) . . . . ? C1 Mn2 C3 C4 -79.73(7) . . . . ? C2 Mn2 C3 C4 -118.07(9) . . . . ? Mn1 Mn2 C3 C4 107.77(7) . . . . ? C5 Mn2 C3 C2 80.15(7) . . . . ? C1 Mn2 C3 C2 38.34(6) . . . . ? C4 Mn2 C3 C2 118.07(9) . . . . ? Mn1 Mn2 C3 C2 -134.16(6) . . . . ? C2 C3 C4 C5 -0.56(12) . . . . ? Mn2 C3 C4 C5 64.24(7) . . . . ? C2 C3 C4 C14 177.20(10) . . . . ? Mn2 C3 C4 C14 -117.99(10) . . . . ? C2 C3 C4 Mn2 -64.81(8) . . . . ? C3 Mn2 C4 C5 -114.48(9) . . . . ? C1 Mn2 C4 C5 -36.11(6) . . . . ? C2 Mn2 C4 C5 -78.04(7) . . . . ? Mn1 Mn2 C4 C5 112.07(6) . . . . ? C5 Mn2 C4 C3 114.48(9) . . . . ? C1 Mn2 C4 C3 78.38(7) . . . . ? C2 Mn2 C4 C3 36.44(6) . . . . ? Mn1 Mn2 C4 C3 -133.44(6) . . . . ? C3 Mn2 C4 C14 121.50(11) . . . . ? C5 Mn2 C4 C14 -124.02(11) . . . . ? C1 Mn2 C4 C14 -160.13(10) . . . . ? C2 Mn2 C4 C14 157.94(10) . . . . ? Mn1 Mn2 C4 C14 -11.95(11) . . . . ? C3 C4 C5 C1 -0.37(12) . . . . ? C14 C4 C5 C1 -178.08(10) . . . . ? Mn2 C4 C5 C1 63.31(8) . . . . ? C3 C4 C5 Mn2 -63.68(7) . . . . ? C14 C4 C5 Mn2 118.61(11) . . . . ? C2 C1 C5 C4 1.13(12) . . . . ? C6 C1 C5 C4 176.58(9) . . . . ? Mn2 C1 C5 C4 -63.83(8) . . . . ? C2 C1 C5 Mn2 64.96(7) . . . . ? C6 C1 C5 Mn2 -119.59(9) . . . . ? C3 Mn2 C5 C4 38.16(6) . . . . ? C1 Mn2 C5 C4 118.81(9) . . . . ? C2 Mn2 C5 C4 80.05(7) . . . . ? Mn1 Mn2 C5 C4 -117.57(6) . . . . ? C3 Mn2 C5 C1 -80.65(7) . . . . ? C2 Mn2 C5 C1 -38.76(6) . . . . ? C4 Mn2 C5 C1 -118.81(9) . . . . ? Mn1 Mn2 C5 C1 123.62(6) . . . . ? C5 C1 C6 C9 145.54(11) . . . . ? C2 C1 C6 C9 -40.52(17) . . . . ? Mn2 C1 C6 C9 57.65(13) . . . . ? C5 C1 C6 C8 26.79(14) . . . . ? C2 C1 C6 C8 -159.27(12) . . . . ? Mn2 C1 C6 C8 -61.10(12) . . . . ? C5 C1 C6 C7 -90.50(12) . . . . ? C2 C1 C6 C7 83.45(15) . . . . ? Mn2 C1 C6 C7 -178.39(8) . . . . ? C3 C2 C10 C12 126.79(11) . . . . ? C1 C2 C10 C12 -52.16(16) . . . . ? Mn2 C2 C10 C12 -147.05(8) . . . . ? C3 C2 C10 C13 8.87(14) . . . . ? C1 C2 C10 C13 -170.08(11) . . . . ? Mn2 C2 C10 C13 95.02(10) . . . . ? C3 C2 C10 C11 -108.53(12) . . . . ? C1 C2 C10 C11 72.52(15) . . . . ? Mn2 C2 C10 C11 -22.38(13) . . . . ? C5 C4 C14 C16 -144.03(11) . . . . ? C3 C4 C14 C16 38.69(14) . . . . ? Mn2 C4 C14 C16 -51.50(11) . . . . ? C5 C4 C14 C17 -24.03(15) . . . . ? C3 C4 C14 C17 158.70(10) . . . . ? Mn2 C4 C14 C17 68.51(11) . . . . ? C5 C4 C14 C15 95.42(13) . . . . ? C3 C4 C14 C15 -81.85(13) . . . . ? Mn2 C4 C14 C15 -172.04(8) . . . . ? C20 Mn3 C18 C22 76.89(7) . . . . ? C19 Mn3 C18 C22 115.18(9) . . . . ? C21 Mn3 C18 C22 36.01(6) . . . . ? Mn1 Mn3 C18 C22 -138.79(6) . . . . ? C22 Mn3 C18 C19 -115.18(9) . . . . ? C20 Mn3 C18 C19 -38.29(6) . . . . ? C21 Mn3 C18 C19 -79.17(6) . . . . ? Mn1 Mn3 C18 C19 106.03(7) . . . . ? C22 Mn3 C18 C23 114.23(11) . . . . ? C20 Mn3 C18 C23 -168.88(10) . . . . ? C19 Mn3 C18 C23 -130.59(12) . . . . ? C21 Mn3 C18 C23 150.24(10) . . . . ? Mn1 Mn3 C18 C23 -24.56(13) . . . . ? C22 C18 C19 C20 1.51(11) . . . . ? C23 C18 C19 C20 -175.40(11) . . . . ? Mn3 C18 C19 C20 64.79(7) . . . . ? C22 C18 C19 C27 176.84(11) . . . . ? C23 C18 C19 C27 -0.1(2) . . . . ? Mn3 C18 C19 C27 -119.88(12) . . . . ? C22 C18 C19 Mn3 -63.28(7) . . . . ? C23 C18 C19 Mn3 119.81(12) . . . . ? C22 Mn3 C19 C20 -76.57(7) . . . . ? C21 Mn3 C19 C20 -35.67(6) . . . . ? C18 Mn3 C19 C20 -114.22(9) . . . . ? Mn1 Mn3 C19 C20 111.20(6) . . . . ? C22 Mn3 C19 C18 37.65(6) . . . . ? C20 Mn3 C19 C18 114.22(9) . . . . ? C21 Mn3 C19 C18 78.55(6) . . . . ? Mn1 Mn3 C19 C18 -134.58(5) . . . . ? C22 Mn3 C19 C27 169.11(10) . . . . ? C20 Mn3 C19 C27 -114.31(11) . . . . ? C21 Mn3 C19 C27 -149.99(10) . . . . ? C18 Mn3 C19 C27 131.46(11) . . . . ? Mn1 Mn3 C19 C27 -3.12(11) . . . . ? C18 C19 C20 C21 -1.12(12) . . . . ? C27 C19 C20 C21 -177.23(9) . . . . ? Mn3 C19 C20 C21 64.25(8) . . . . ? C18 C19 C20 Mn3 -65.37(7) . . . . ? C27 C19 C20 Mn3 118.52(9) . . . . ? C22 Mn3 C20 C21 -38.09(6) . . . . ? C19 Mn3 C20 C21 -118.48(9) . . . . ? C18 Mn3 C20 C21 -79.88(7) . . . . ? Mn1 Mn3 C20 C21 124.53(6) . . . . ? C22 Mn3 C20 C19 80.39(7) . . . . ? C21 Mn3 C20 C19 118.48(9) . . . . ? C18 Mn3 C20 C19 38.61(6) . . . . ? Mn1 Mn3 C20 C19 -116.99(6) . . . . ? C19 C20 C21 C22 0.26(12) . . . . ? Mn3 C20 C21 C22 63.90(7) . . . . ? C19 C20 C21 C31 175.08(10) . . . . ? Mn3 C20 C21 C31 -121.28(11) . . . . ? C19 C20 C21 Mn3 -63.64(7) . . . . ? C22 Mn3 C21 C20 114.52(9) . . . . ? C19 Mn3 C21 C20 36.33(6) . . . . ? C18 Mn3 C21 C20 78.14(7) . . . . ? Mn1 Mn3 C21 C20 -106.16(7) . . . . ? C20 Mn3 C21 C22 -114.52(9) . . . . ? C19 Mn3 C21 C22 -78.19(7) . . . . ? C18 Mn3 C21 C22 -36.38(6) . . . . ? Mn1 Mn3 C21 C22 139.32(6) . . . . ? C22 Mn3 C21 C31 -121.29(11) . . . . ? C20 Mn3 C21 C31 124.19(12) . . . . ? C19 Mn3 C21 C31 160.52(10) . . . . ? C18 Mn3 C21 C31 -157.67(10) . . . . ? Mn1 Mn3 C21 C31 18.04(12) . . . . ? C20 C21 C22 C18 0.74(12) . . . . ? C31 C21 C22 C18 -174.24(10) . . . . ? Mn3 C21 C22 C18 64.72(8) . . . . ? C20 C21 C22 Mn3 -63.99(7) . . . . ? C31 C21 C22 Mn3 121.04(10) . . . . ? C19 C18 C22 C21 -1.42(12) . . . . ? C23 C18 C22 C21 176.00(9) . . . . ? Mn3 C18 C22 C21 -64.77(8) . . . . ? C19 C18 C22 Mn3 63.36(7) . . . . ? C23 C18 C22 Mn3 -119.23(9) . . . . ? C20 Mn3 C22 C21 37.99(6) . . . . ? C19 Mn3 C22 C21 79.94(7) . . . . ? C18 Mn3 C22 C21 118.10(9) . . . . ? Mn1 Mn3 C22 C21 -112.41(8) . . . . ? C20 Mn3 C22 C18 -80.11(7) . . . . ? C19 Mn3 C22 C18 -38.16(6) . . . . ? C21 Mn3 C22 C18 -118.10(9) . . . . ? Mn1 Mn3 C22 C18 129.50(7) . . . . ? C22 C18 C23 C24 -6.32(14) . . . . ? C19 C18 C23 C24 170.25(11) . . . . ? Mn3 C18 C23 C24 -93.21(10) . . . . ? C22 C18 C23 C25 110.96(12) . . . . ? C19 C18 C23 C25 -72.47(15) . . . . ? Mn3 C18 C23 C25 24.07(13) . . . . ? C22 C18 C23 C26 -124.12(11) . . . . ? C19 C18 C23 C26 52.46(16) . . . . ? Mn3 C18 C23 C26 148.99(8) . . . . ? C20 C19 C27 C28 -147.26(10) . . . . ? C18 C19 C27 C28 37.90(17) . . . . ? Mn3 C19 C27 C28 -60.11(12) . . . . ? C20 C19 C27 C29 88.95(12) . . . . ? C18 C19 C27 C29 -85.90(14) . . . . ? Mn3 C19 C27 C29 176.10(8) . . . . ? C20 C19 C27 C30 -28.63(13) . . . . ? C18 C19 C27 C30 156.53(11) . . . . ? Mn3 C19 C27 C30 58.52(11) . . . . ? C20 C21 C31 C32 146.29(12) . . . . ? C22 C21 C31 C32 -39.84(15) . . . . ? Mn3 C21 C31 C32 52.26(13) . . . . ? C20 C21 C31 C34 25.83(15) . . . . ? C22 C21 C31 C34 -160.31(10) . . . . ? Mn3 C21 C31 C34 -68.20(12) . . . . ? C20 C21 C31 C33 -93.60(14) . . . . ? C22 C21 C31 C33 80.26(13) . . . . ? Mn3 C21 C31 C33 172.37(8) . . . . ? C35 C36 C37 C38 -173.90(13) . . . . ? C36 C37 C38 C39 177.94(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.382 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.049 _iucr_refine_instructions_details ; TITL mima15 in C2/c CELL 0.71073 27.4840 12.7411 25.2730 90.000 114.331 90.000 ZERR 4.00 0.0004 0.0002 0.0004 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H MN UNIT 312 584 20 SIZE 0.26 0.22 0.18 TEMP -173 SHEL 999 0.69 ACTA CONF FMAP 2 PLAN 10 L.S. 4 BOND $H OMIT -3 3 6 OMIT 0 4 4 OMIT -4 2 2 OMIT -7 1 4 OMIT 6 2 5 OMIT 9 1 6 OMIT -10 4 2 OMIT -7 1 10 OMIT -6 2 8 OMIT 4 4 0 OMIT -6 4 12 OMIT -12 0 4 WGHT 0.030600 FVAR 1.34979 MN1 3 1.000000 0.198218 0.250000 10.50000 0.01196 0.01003 = 0.01157 0.00000 0.00532 0.00000 H01 2 1.036965 0.197491 0.315550 11.00000 0.05037 H02 2 1.052079 0.196979 0.236915 11.00000 0.04348 H03 2 1.000000 0.077109 0.250000 10.50000 0.04731 H04 2 1.000000 0.322956 0.250000 10.50000 0.05570 MN2 3 1.079259 0.084224 0.298521 11.00000 0.01376 0.01498 = 0.01916 0.00320 0.00582 0.00325 MN3 3 1.016453 0.311649 0.179190 11.00000 0.02080 0.01518 = 0.01522 0.00307 0.00954 -0.00072 C1 1 1.148482 -0.014884 0.290056 11.00000 0.01424 0.01568 = 0.01919 0.00352 0.00823 0.00435 C2 1 1.171768 0.044724 0.343704 11.00000 0.01227 0.01469 = 0.02100 0.00251 0.00554 0.00310 C3 1 1.147008 0.007336 0.379823 11.00000 0.01596 0.01595 = 0.01365 0.00073 0.00365 0.00274 H3 2 1.152918 0.031218 0.416330 11.00000 0.01760 C4 1 1.110413 -0.073861 0.351959 11.00000 0.01509 0.01332 = 0.01572 0.00274 0.00594 0.00354 C5 1 1.111814 -0.087012 0.297242 11.00000 0.01613 0.01405 = 0.01584 0.00015 0.00586 0.00211 H5 2 1.091119 -0.135417 0.268653 11.00000 0.02050 C6 1 1.158892 -0.019392 0.234564 11.00000 0.02483 0.02196 = 0.02426 0.00234 0.01615 0.00180 C7 1 1.206117 -0.094276 0.245265 11.00000 0.03421 0.02890 = 0.03906 0.00123 0.02520 0.00554 AFIX 137 H7A 2 1.238515 -0.065755 0.276098 11.00000 -1.20000 H7B 2 1.211589 -0.101384 0.209488 11.00000 -1.20000 H7C 2 1.198253 -0.163271 0.257007 11.00000 -1.20000 AFIX 0 C8 1 1.109622 -0.065094 0.184133 11.00000 0.03733 0.03780 = 0.02106 -0.00199 0.01680 -0.00397 AFIX 137 H8A 2 1.115469 -0.063726 0.148418 11.00000 -1.20000 H8B 2 1.078093 -0.022956 0.178741 11.00000 -1.20000 H8C 2 1.103971 -0.137662 0.193172 11.00000 -1.20000 AFIX 0 C9 1 1.169222 0.087047 0.212951 11.00000 0.03417 0.02812 = 0.02830 0.00533 0.01934 0.00170 AFIX 137 H9A 2 1.202542 0.116819 0.241601 11.00000 -1.20000 H9B 2 1.139570 0.134752 0.207531 11.00000 -1.20000 H9C 2 1.172165 0.077674 0.175893 11.00000 -1.20000 AFIX 0 C10 1 1.214724 0.131000 0.365308 11.00000 0.01398 0.02016 = 0.02839 0.00077 0.00655 -0.00041 C11 1 1.193949 0.236302 0.334165 11.00000 0.02306 0.01737 = 0.03943 -0.00099 0.01004 -0.00275 AFIX 137 H11A 2 1.182041 0.226796 0.292204 11.00000 -1.20000 H11B 2 1.222663 0.288516 0.348104 11.00000 -1.20000 H11C 2 1.163932 0.260553 0.342383 11.00000 -1.20000 AFIX 0 C12 1 1.266108 0.098045 0.359635 11.00000 0.01470 0.02916 = 0.04067 0.00181 0.00973 -0.00067 AFIX 137 H12A 2 1.278476 0.030611 0.379237 11.00000 -1.20000 H12B 2 1.293712 0.151428 0.377586 11.00000 -1.20000 H12C 2 1.258927 0.091064 0.318463 11.00000 -1.20000 AFIX 0 C13 1 1.230537 0.152225 0.430245 11.00000 0.01945 0.03144 = 0.03082 -0.00575 0.00460 -0.00706 AFIX 137 H13A 2 1.199038 0.175039 0.436062 11.00000 -1.20000 H13B 2 1.257812 0.207333 0.443611 11.00000 -1.20000 H13C 2 1.244831 0.087819 0.452422 11.00000 -1.20000 AFIX 0 C14 1 1.078224 -0.136200 0.377694 11.00000 0.02046 0.01448 = 0.01629 0.00137 0.00887 -0.00014 C15 1 1.113383 -0.223959 0.416203 11.00000 0.03555 0.02389 = 0.03430 0.01244 0.01866 0.00660 AFIX 137 H15A 2 1.125238 -0.270103 0.392800 11.00000 -1.20000 H15B 2 1.092782 -0.264755 0.432739 11.00000 -1.20000 H15C 2 1.144577 -0.193048 0.447654 11.00000 -1.20000 AFIX 0 C16 1 1.059240 -0.064590 0.413753 11.00000 0.03323 0.02159 = 0.02710 -0.00271 0.01990 -0.00307 AFIX 137 H16A 2 1.090232 -0.035035 0.446038 11.00000 -1.20000 H16B 2 1.037643 -0.105166 0.429121 11.00000 -1.20000 H16C 2 1.037649 -0.007565 0.389266 11.00000 -1.20000 AFIX 0 C17 1 1.029134 -0.186380 0.330018 11.00000 0.02855 0.03047 = 0.02509 -0.00379 0.01569 -0.00996 AFIX 137 H17A 2 1.006084 -0.131328 0.305142 11.00000 -1.20000 H17B 2 1.009338 -0.226539 0.347774 11.00000 -1.20000 H17C 2 1.040541 -0.233410 0.306604 11.00000 -1.20000 AFIX 0 C18 1 1.015943 0.349059 0.086729 11.00000 0.02194 0.01296 = 0.01413 0.00295 0.01022 0.00062 C19 1 0.973176 0.407619 0.092450 11.00000 0.01572 0.01440 = 0.01357 0.00327 0.00591 -0.00148 C20 1 0.998054 0.480974 0.138585 11.00000 0.01626 0.01180 = 0.01770 0.00237 0.00826 0.00036 H20 2 0.980044 0.530995 0.151989 11.00000 0.01375 C21 1 1.054035 0.469442 0.162463 11.00000 0.01627 0.01252 = 0.01570 0.00207 0.00721 -0.00046 C22 1 1.064502 0.387941 0.130688 11.00000 0.01601 0.01605 = 0.01682 0.00331 0.00940 0.00145 H22 2 1.099612 0.365356 0.137381 11.00000 0.01703 C23 1 1.017527 0.264519 0.043786 11.00000 0.02882 0.01702 = 0.01594 0.00024 0.01127 0.00201 C24 1 1.075571 0.244102 0.052715 11.00000 0.03253 0.02624 = 0.02119 -0.00004 0.01521 0.00731 AFIX 137 H24A 2 1.095820 0.216067 0.091808 11.00000 -1.20000 H24B 2 1.091835 0.310012 0.048178 11.00000 -1.20000 H24C 2 1.076031 0.193221 0.023845 11.00000 -1.20000 AFIX 0 C25 1 0.996251 0.157693 0.053335 11.00000 0.03884 0.01637 = 0.02833 -0.00285 0.01472 -0.00177 AFIX 137 H25A 2 1.017735 0.133234 0.092934 11.00000 -1.20000 H25B 2 0.998522 0.106631 0.025441 11.00000 -1.20000 H25C 2 0.958947 0.165197 0.047710 11.00000 -1.20000 AFIX 0 C26 1 0.987321 0.301712 -0.019398 11.00000 0.03301 0.02854 = 0.01607 -0.00163 0.01086 0.00228 AFIX 137 H26A 2 0.992457 0.250811 -0.045719 11.00000 -1.20000 H26B 2 1.001114 0.370275 -0.024266 11.00000 -1.20000 H26C 2 0.949168 0.307720 -0.028420 11.00000 -1.20000 AFIX 0 C27 1 0.912064 0.409218 0.057965 11.00000 0.01672 0.01896 = 0.01920 0.00060 0.00426 -0.00220 C28 1 0.886844 0.301773 0.036276 11.00000 0.01895 0.02483 = 0.02722 -0.00083 0.00512 -0.00606 AFIX 137 H28A 2 0.899569 0.274506 0.007983 11.00000 -1.20000 H28B 2 0.847889 0.308822 0.017812 11.00000 -1.20000 H28C 2 0.896923 0.253186 0.069145 11.00000 -1.20000 AFIX 0 C29 1 0.897540 0.485119 0.006564 11.00000 0.02249 0.02614 = 0.02452 0.00552 0.00189 0.00053 AFIX 137 H29A 2 0.914152 0.461301 -0.018986 11.00000 -1.20000 H29B 2 0.910528 0.555603 0.021063 11.00000 -1.20000 H29C 2 0.858666 0.486926 -0.015211 11.00000 -1.20000 AFIX 0 C30 1 0.885125 0.450367 0.096757 11.00000 0.01684 0.03369 = 0.03340 -0.00356 0.01003 -0.00131 AFIX 137 H30A 2 0.846246 0.445840 0.075569 11.00000 -1.20000 H30B 2 0.895470 0.523639 0.107226 11.00000 -1.20000 H30C 2 0.896556 0.407749 0.132106 11.00000 -1.20000 AFIX 0 C31 1 1.095818 0.536175 0.208924 11.00000 0.01594 0.01724 = 0.02042 -0.00237 0.00470 -0.00146 C32 1 1.143731 0.469886 0.247146 11.00000 0.02490 0.03389 = 0.04127 -0.01318 -0.00517 0.00744 AFIX 137 H32A 2 1.131905 0.414720 0.266196 11.00000 -1.20000 H32B 2 1.170045 0.514643 0.276673 11.00000 -1.20000 H32C 2 1.159987 0.437757 0.223096 11.00000 -1.20000 AFIX 0 C33 1 1.114083 0.621498 0.178347 11.00000 0.04062 0.03470 = 0.03889 -0.00816 0.01822 -0.02336 AFIX 137 H33A 2 1.128802 0.588543 0.153085 11.00000 -1.20000 H33B 2 1.141580 0.664926 0.207457 11.00000 -1.20000 H33C 2 1.083541 0.665562 0.154955 11.00000 -1.20000 AFIX 0 C34 1 1.072837 0.588539 0.248005 11.00000 0.02539 0.02912 = 0.02228 -0.00872 0.00534 -0.00043 AFIX 137 H34A 2 1.042307 0.632418 0.224371 11.00000 -1.20000 H34B 2 1.100324 0.632290 0.276913 11.00000 -1.20000 H34C 2 1.061137 0.534500 0.267804 11.00000 -1.20000 AFIX 0 C35 1 0.822014 0.078484 0.938707 11.00000 0.04216 0.03048 = 0.03152 0.00127 0.01396 0.00381 AFIX 137 H35A 2 0.826851 0.084073 0.979250 11.00000 -1.20000 H35B 2 0.815071 0.148269 0.920812 11.00000 -1.20000 H35C 2 0.854435 0.049354 0.937238 11.00000 -1.20000 AFIX 0 C36 1 0.775206 0.007086 0.906006 11.00000 0.03180 0.03081 = 0.03625 0.00446 0.01542 0.00559 AFIX 23 H36A 2 0.743193 0.034297 0.910102 11.00000 -1.20000 H36B 2 0.767856 0.008622 0.864232 11.00000 -1.20000 AFIX 0 C37 1 0.784574 -0.105160 0.927057 11.00000 0.03327 0.03225 = 0.03661 0.00336 0.01411 0.00059 AFIX 23 H37A 2 0.818833 -0.129319 0.927117 11.00000 -1.20000 H37B 2 0.788173 -0.107135 0.967666 11.00000 -1.20000 AFIX 0 C38 1 0.741278 -0.180806 0.891505 11.00000 0.03521 0.04144 = 0.06592 0.00209 0.01646 -0.00900 AFIX 23 H38A 2 0.736733 -0.177371 0.850595 11.00000 -1.20000 H38B 2 0.707216 -0.158558 0.892660 11.00000 -1.20000 AFIX 0 C39 1 0.752701 -0.293907 0.912391 11.00000 0.05074 0.03433 = 0.08049 -0.00552 0.02569 -0.01280 AFIX 137 H39A 2 0.785220 -0.318068 0.909158 11.00000 -1.20000 H39B 2 0.722602 -0.338471 0.888448 11.00000 -1.20000 H39C 2 0.757636 -0.297994 0.953014 11.00000 -1.20000 HKLF 4 ; # end of cif file