# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Walter, Marc' _publ_contact_author_email marc.walter@tu-bs.de _publ_author_name 'Marc Welter' data_mima05 _database_code_depnum_ccdc_archive 'CCDC 884305' #TrackingRef '- mima05.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H54 Fe' _chemical_formula_weight 614.70 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' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1411(2) _cell_length_b 15.4986(2) _cell_length_c 21.3658(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.712(2) _cell_angle_gamma 90.00 _cell_volume 3288.21(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21852 _cell_measurement_theta_min 3.5461 _cell_measurement_theta_max 75.6913 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 3.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81888 _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 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45481 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 75.88 _reflns_number_total 6830 _reflns_number_gt 5867 _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. ; _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^)+(0.0538P)^2^+0.1983P] 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 6830 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Fe Fe 0.51483(2) 0.421854(14) 0.198117(10) 0.01411(7) Uani 1 1 d . . . C1 C 0.60663(16) 0.51544(9) 0.26116(7) 0.0180(3) Uani 1 1 d . . . C2 C 0.47617(16) 0.54378(9) 0.22867(7) 0.0172(3) Uani 1 1 d . . . H2 H 0.4052 0.5602 0.2492 0.021 Uiso 1 1 calc R . . C3 C 0.46758(15) 0.54398(9) 0.16120(7) 0.0162(3) Uani 1 1 d . . . C4 C 0.59863(15) 0.51924(9) 0.15104(7) 0.0163(3) Uani 1 1 d . . . C6 C 0.82406(16) 0.48296(10) 0.21445(8) 0.0220(3) Uani 1 1 d . . . H6 H 0.8838 0.4734 0.2542 0.026 Uiso 1 1 calc R . . C7 C 0.86964(17) 0.47752(10) 0.15874(9) 0.0242(3) Uani 1 1 d . . . H7 H 0.9622 0.4657 0.1604 0.029 Uiso 1 1 calc R . . C8 C 0.78215(17) 0.48905(10) 0.09811(8) 0.0229(3) Uani 1 1 d . . . H8 H 0.8167 0.4828 0.0602 0.028 Uiso 1 1 calc R . . C9 C 0.64935(16) 0.50895(9) 0.09367(7) 0.0185(3) Uani 1 1 d . . . H9 H 0.5914 0.5159 0.0531 0.022 Uiso 1 1 calc R . . C5 C 0.68550(16) 0.50314(9) 0.21254(7) 0.0178(3) Uani 1 1 d . . . C10 C 0.56927(15) 0.29854(9) 0.17593(7) 0.0163(3) Uani 1 1 d . . . C11 C 0.54279(16) 0.30102(9) 0.23899(7) 0.0180(3) Uani 1 1 d . . . H11 H 0.6057 0.2853 0.2766 0.022 Uiso 1 1 calc R . . C12 C 0.40892(16) 0.33034(9) 0.23794(8) 0.0191(3) Uani 1 1 d . . . C13 C 0.34578(16) 0.34061(9) 0.17153(8) 0.0176(3) Uani 1 1 d . . . C14 C 0.44563(15) 0.32276(9) 0.13331(7) 0.0160(3) Uani 1 1 d . . . C15 C 0.41117(16) 0.33168(9) 0.06544(7) 0.0193(3) Uani 1 1 d . . . H15 H 0.4774 0.3233 0.0403 0.023 Uiso 1 1 calc R . . C16 C 0.28210(17) 0.35241(10) 0.03710(8) 0.0228(3) Uani 1 1 d . . . H16 H 0.2586 0.3581 -0.0081 0.027 Uiso 1 1 calc R . . C17 C 0.18171(17) 0.36563(10) 0.07439(8) 0.0248(3) Uani 1 1 d . . . H17 H 0.0920 0.3782 0.0533 0.030 Uiso 1 1 calc R . . C18 C 0.21138(16) 0.36067(9) 0.13939(8) 0.0221(3) Uani 1 1 d . . . H18 H 0.1432 0.3705 0.1632 0.027 Uiso 1 1 calc R . . C19 C 0.64932(17) 0.51647(10) 0.33300(7) 0.0211(3) Uani 1 1 d . . . H19 H 0.5658 0.5085 0.3504 0.025 Uiso 1 1 calc R . . C20 C 0.70581(17) 0.60607(10) 0.35507(8) 0.0235(3) Uani 1 1 d . . . H20A H 0.7872 0.6173 0.3375 0.028 Uiso 1 1 calc R . . H20B H 0.6381 0.6506 0.3381 0.028 Uiso 1 1 calc R . . C21 C 0.7418(2) 0.61291(11) 0.42800(8) 0.0321(4) Uani 1 1 d . . . H21A H 0.7845 0.6696 0.4402 0.039 Uiso 1 1 calc R . . H21B H 0.6584 0.6097 0.4452 0.039 Uiso 1 1 calc R . . C22 C 0.83747(19) 0.54133(11) 0.45750(8) 0.0280(4) Uani 1 1 d . . . H22A H 0.8527 0.5451 0.5047 0.034 Uiso 1 1 calc R . . H22B H 0.9253 0.5489 0.4448 0.034 Uiso 1 1 calc R . . C23 C 0.7800(2) 0.45294(11) 0.43587(8) 0.0317(4) Uani 1 1 d . . . H23A H 0.6969 0.4430 0.4524 0.038 Uiso 1 1 calc R . . H23B H 0.8459 0.4077 0.4537 0.038 Uiso 1 1 calc R . . C24 C 0.7479(2) 0.44631(11) 0.36289(8) 0.0324(4) Uani 1 1 d . . . H24A H 0.8323 0.4518 0.3466 0.039 Uiso 1 1 calc R . . H24B H 0.7086 0.3889 0.3501 0.039 Uiso 1 1 calc R . . C25 C 0.35304(15) 0.57540(9) 0.11049(7) 0.0168(3) Uani 1 1 d . . . H25 H 0.3379 0.5328 0.0746 0.020 Uiso 1 1 calc R . . C26 C 0.39102(16) 0.66298(9) 0.08449(7) 0.0190(3) Uani 1 1 d . . . H26A H 0.4116 0.7048 0.1201 0.023 Uiso 1 1 calc R . . H26B H 0.4733 0.6557 0.0668 0.023 Uiso 1 1 calc R . . C27 C 0.27847(17) 0.69912(10) 0.03260(8) 0.0237(3) Uani 1 1 d . . . H27A H 0.3046 0.7570 0.0198 0.028 Uiso 1 1 calc R . . H27B H 0.2660 0.6612 -0.0054 0.028 Uiso 1 1 calc R . . C28 C 0.14601(17) 0.70578(10) 0.05557(8) 0.0251(3) Uani 1 1 d . . . H28A H 0.0738 0.7244 0.0197 0.030 Uiso 1 1 calc R . . H28B H 0.1546 0.7499 0.0896 0.030 Uiso 1 1 calc R . . C29 C 0.10762(16) 0.61924(10) 0.08138(8) 0.0244(3) Uani 1 1 d . . . H29A H 0.0246 0.6263 0.0985 0.029 Uiso 1 1 calc R . . H29B H 0.0891 0.5766 0.0462 0.029 Uiso 1 1 calc R . . C30 C 0.22100(16) 0.58581(10) 0.13422(8) 0.0203(3) Uani 1 1 d . . . H30A H 0.1945 0.5294 0.1496 0.024 Uiso 1 1 calc R . . H30B H 0.2351 0.6266 0.1706 0.024 Uiso 1 1 calc R . . C31 C 0.69394(15) 0.26405(9) 0.15675(7) 0.0182(3) Uani 1 1 d . . . H31 H 0.7237 0.3063 0.1271 0.022 Uiso 1 1 calc R . . C32 C 0.80880(17) 0.25097(10) 0.21435(8) 0.0246(3) Uani 1 1 d . . . H32A H 0.7765 0.2146 0.2462 0.030 Uiso 1 1 calc R . . H32B H 0.8352 0.3076 0.2344 0.030 Uiso 1 1 calc R . . C33 C 0.93217(17) 0.20852(12) 0.19672(10) 0.0323(4) Uani 1 1 d . . . H33A H 0.9707 0.2475 0.1684 0.039 Uiso 1 1 calc R . . H33B H 1.0015 0.1988 0.2360 0.039 Uiso 1 1 calc R . . C34 C 0.89524(18) 0.12264(11) 0.16292(9) 0.0278(4) Uani 1 1 d . . . H34A H 0.9758 0.0976 0.1503 0.033 Uiso 1 1 calc R . . H34B H 0.8641 0.0818 0.1925 0.033 Uiso 1 1 calc R . . C35 C 0.78462(18) 0.13521(11) 0.10382(8) 0.0253(3) Uani 1 1 d . . . H35A H 0.7591 0.0786 0.0835 0.030 Uiso 1 1 calc R . . H35B H 0.8187 0.1718 0.0726 0.030 Uiso 1 1 calc R . . C36 C 0.66069(16) 0.17769(10) 0.12107(7) 0.0200(3) Uani 1 1 d . . . H36A H 0.6207 0.1378 0.1483 0.024 Uiso 1 1 calc R . . H36B H 0.5928 0.1880 0.0814 0.024 Uiso 1 1 calc R . . C37 C 0.34962(18) 0.33027(10) 0.29706(8) 0.0230(3) Uani 1 1 d . . . H37 H 0.4265 0.3369 0.3343 0.028 Uiso 1 1 calc R . . C38 C 0.2496(2) 0.40120(12) 0.30276(10) 0.0376(5) Uani 1 1 d . . . H38A H 0.1723 0.3976 0.2662 0.045 Uiso 1 1 calc R . . H38B H 0.2932 0.4581 0.3011 0.045 Uiso 1 1 calc R . . C39 C 0.1986(2) 0.39367(12) 0.36532(10) 0.0352(4) Uani 1 1 d . . . H39A H 0.2748 0.4019 0.4019 0.042 Uiso 1 1 calc R . . H39B H 0.1317 0.4397 0.3670 0.042 Uiso 1 1 calc R . . C40 C 0.13404(19) 0.30571(11) 0.37090(9) 0.0311(4) Uani 1 1 d . . . H40A H 0.1071 0.3013 0.4128 0.037 Uiso 1 1 calc R . . H40B H 0.0520 0.2999 0.3370 0.037 Uiso 1 1 calc R . . C41 C 0.2311(2) 0.23384(11) 0.36463(10) 0.0324(4) Uani 1 1 d . . . H41A H 0.1844 0.1778 0.3647 0.039 Uiso 1 1 calc R . . H41B H 0.3066 0.2350 0.4021 0.039 Uiso 1 1 calc R . . C42 C 0.28731(16) 0.24093(9) 0.30376(8) 0.0203(3) Uani 1 1 d . . . H42A H 0.2140 0.2303 0.2662 0.024 Uiso 1 1 calc R . . H42B H 0.3568 0.1960 0.3043 0.024 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 Fe 0.01723(12) 0.01196(11) 0.01374(11) 0.00069(8) 0.00453(8) 0.00002(8) C1 0.0237(8) 0.0130(6) 0.0168(7) -0.0003(5) 0.0028(6) -0.0013(5) C2 0.0226(8) 0.0128(6) 0.0170(7) 0.0001(5) 0.0063(6) 0.0001(5) C3 0.0205(7) 0.0117(6) 0.0169(7) 0.0007(5) 0.0053(6) -0.0002(5) C4 0.0190(7) 0.0116(6) 0.0186(7) 0.0014(5) 0.0047(6) -0.0012(5) C6 0.0187(8) 0.0185(7) 0.0274(8) 0.0032(6) 0.0015(6) -0.0012(6) C7 0.0188(8) 0.0184(7) 0.0367(9) 0.0043(6) 0.0087(7) 0.0011(6) C8 0.0268(9) 0.0169(7) 0.0291(8) 0.0012(6) 0.0149(7) 0.0004(6) C9 0.0238(8) 0.0146(6) 0.0185(7) 0.0012(5) 0.0077(6) -0.0010(5) C5 0.0202(7) 0.0125(6) 0.0200(7) 0.0003(5) 0.0026(6) -0.0030(5) C10 0.0204(7) 0.0119(6) 0.0170(7) 0.0002(5) 0.0046(6) 0.0004(5) C11 0.0246(8) 0.0132(6) 0.0167(7) 0.0027(5) 0.0053(6) 0.0004(5) C12 0.0261(8) 0.0126(6) 0.0209(7) 0.0015(5) 0.0101(6) -0.0008(5) C13 0.0196(7) 0.0116(6) 0.0227(7) -0.0007(5) 0.0070(6) -0.0025(5) C14 0.0196(7) 0.0115(6) 0.0176(7) -0.0005(5) 0.0053(6) -0.0015(5) C15 0.0246(8) 0.0151(7) 0.0181(7) -0.0001(5) 0.0039(6) -0.0004(6) C16 0.0293(9) 0.0165(7) 0.0196(7) -0.0006(6) -0.0024(6) -0.0006(6) C17 0.0201(8) 0.0178(7) 0.0333(9) -0.0020(6) -0.0017(7) -0.0005(6) C18 0.0189(8) 0.0160(7) 0.0321(9) -0.0020(6) 0.0067(6) -0.0014(5) C19 0.0265(8) 0.0197(7) 0.0161(7) -0.0001(6) 0.0017(6) -0.0021(6) C20 0.0291(9) 0.0169(7) 0.0217(8) -0.0007(6) -0.0014(6) 0.0026(6) C21 0.0428(11) 0.0257(8) 0.0240(9) -0.0059(7) -0.0027(8) 0.0065(7) C22 0.0329(9) 0.0278(8) 0.0202(8) -0.0017(6) -0.0020(7) 0.0025(7) C23 0.0462(11) 0.0242(8) 0.0204(8) 0.0027(7) -0.0035(7) 0.0003(7) C24 0.0514(12) 0.0197(8) 0.0207(8) -0.0009(6) -0.0055(8) 0.0061(8) C25 0.0192(7) 0.0154(7) 0.0161(7) 0.0008(5) 0.0039(6) 0.0008(5) C26 0.0201(7) 0.0173(7) 0.0194(7) 0.0030(6) 0.0039(6) -0.0002(5) C27 0.0267(8) 0.0206(7) 0.0227(8) 0.0056(6) 0.0025(6) 0.0014(6) C28 0.0224(8) 0.0207(7) 0.0301(9) 0.0034(6) 0.0007(7) 0.0052(6) C29 0.0189(8) 0.0222(8) 0.0315(9) 0.0021(6) 0.0038(7) 0.0016(6) C30 0.0203(8) 0.0183(7) 0.0232(8) 0.0014(6) 0.0068(6) 0.0012(6) C31 0.0188(7) 0.0157(7) 0.0209(7) 0.0013(6) 0.0058(6) 0.0010(5) C32 0.0223(8) 0.0210(8) 0.0286(8) -0.0030(6) 0.0004(7) 0.0023(6) C33 0.0183(8) 0.0302(9) 0.0460(11) -0.0033(8) 0.0010(7) 0.0025(6) C34 0.0230(8) 0.0268(8) 0.0339(9) 0.0002(7) 0.0068(7) 0.0077(6) C35 0.0295(9) 0.0234(8) 0.0246(8) -0.0003(6) 0.0094(7) 0.0083(6) C36 0.0215(8) 0.0185(7) 0.0202(7) -0.0018(6) 0.0044(6) 0.0025(6) C37 0.0321(9) 0.0177(7) 0.0225(8) -0.0006(6) 0.0134(7) -0.0027(6) C38 0.0541(13) 0.0238(8) 0.0441(11) 0.0069(8) 0.0319(10) 0.0079(8) C39 0.0489(12) 0.0251(9) 0.0402(11) -0.0025(7) 0.0289(9) -0.0003(8) C40 0.0324(10) 0.0314(9) 0.0339(9) 0.0012(7) 0.0173(8) -0.0016(7) C41 0.0445(11) 0.0222(8) 0.0375(10) 0.0055(7) 0.0252(9) -0.0011(7) C42 0.0233(8) 0.0168(7) 0.0229(8) 0.0007(6) 0.0099(6) -0.0009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C11 2.0614(14) . ? Fe C2 2.0626(14) . ? Fe C12 2.0640(15) . ? Fe C1 2.0678(15) . ? Fe C3 2.0690(14) . ? Fe C10 2.0709(14) . ? Fe C4 2.0878(14) . ? Fe C14 2.0913(14) . ? Fe C13 2.1099(15) . ? Fe C5 2.1122(15) . ? C1 C2 1.433(2) . ? C1 C5 1.447(2) . ? C1 C19 1.508(2) . ? C2 C3 1.426(2) . ? C3 C4 1.441(2) . ? C3 C25 1.500(2) . ? C4 C9 1.431(2) . ? C4 C5 1.447(2) . ? C6 C7 1.364(2) . ? C6 C5 1.432(2) . ? C7 C8 1.425(2) . ? C8 C9 1.366(2) . ? C10 C11 1.427(2) . ? C10 C14 1.442(2) . ? C10 C31 1.504(2) . ? C11 C12 1.427(2) . ? C12 C13 1.442(2) . ? C12 C37 1.505(2) . ? C13 C18 1.430(2) . ? C13 C14 1.451(2) . ? C14 C15 1.428(2) . ? C15 C16 1.364(2) . ? C16 C17 1.429(2) . ? C17 C18 1.362(2) . ? C19 C24 1.527(2) . ? C19 C20 1.539(2) . ? C20 C21 1.530(2) . ? C21 C22 1.523(2) . ? C22 C23 1.523(2) . ? C23 C24 1.530(2) . ? C25 C30 1.534(2) . ? C25 C26 1.5447(19) . ? C26 C27 1.527(2) . ? C27 C28 1.524(2) . ? C28 C29 1.530(2) . ? C29 C30 1.529(2) . ? C31 C32 1.527(2) . ? C31 C36 1.543(2) . ? C32 C33 1.527(2) . ? C33 C34 1.524(2) . ? C34 C35 1.522(2) . ? C35 C36 1.529(2) . ? C37 C38 1.518(2) . ? C37 C42 1.541(2) . ? C38 C39 1.532(2) . ? C39 C40 1.528(2) . ? C40 C41 1.510(2) . ? C41 C42 1.526(2) . ? 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 C11 Fe C2 135.80(6) . . ? C11 Fe C12 40.49(6) . . ? C2 Fe C12 110.54(6) . . ? C11 Fe C1 110.87(6) . . ? C2 Fe C1 40.59(6) . . ? C12 Fe C1 114.62(6) . . ? C11 Fe C3 173.64(6) . . ? C2 Fe C3 40.39(6) . . ? C12 Fe C3 133.33(6) . . ? C1 Fe C3 69.24(6) . . ? C11 Fe C10 40.39(6) . . ? C2 Fe C10 174.03(6) . . ? C12 Fe C10 69.23(6) . . ? C1 Fe C10 133.69(6) . . ? C3 Fe C10 143.99(6) . . ? C11 Fe C4 145.73(6) . . ? C2 Fe C4 67.18(6) . . ? C12 Fe C4 172.80(6) . . ? C1 Fe C4 68.49(6) . . ? C3 Fe C4 40.57(6) . . ? C10 Fe C4 113.80(6) . . ? C11 Fe C14 67.18(6) . . ? C2 Fe C14 145.34(6) . . ? C12 Fe C14 68.62(6) . . ? C1 Fe C14 173.02(6) . . ? C3 Fe C14 113.50(6) . . ? C10 Fe C14 40.53(6) . . ? C4 Fe C14 109.07(6) . . ? C11 Fe C13 66.81(6) . . ? C2 Fe C13 115.83(6) . . ? C12 Fe C13 40.40(6) . . ? C1 Fe C13 145.87(6) . . ? C3 Fe C13 109.31(6) . . ? C10 Fe C13 68.12(6) . . ? C4 Fe C13 133.60(6) . . ? C14 Fe C13 40.39(6) . . ? C11 Fe C5 116.22(6) . . ? C2 Fe C5 67.06(6) . . ? C12 Fe C5 146.03(6) . . ? C1 Fe C5 40.48(6) . . ? C3 Fe C5 68.25(6) . . ? C10 Fe C5 109.59(6) . . ? C4 Fe C5 40.31(6) . . ? C14 Fe C5 133.59(6) . . ? C13 Fe C5 172.84(6) . . ? C2 C1 C5 106.45(13) . . ? C2 C1 C19 122.43(14) . . ? C5 C1 C19 130.24(14) . . ? C2 C1 Fe 69.51(8) . . ? C5 C1 Fe 71.41(8) . . ? C19 C1 Fe 131.97(10) . . ? C3 C2 C1 110.58(13) . . ? C3 C2 Fe 70.05(8) . . ? C1 C2 Fe 69.90(8) . . ? C2 C3 C4 106.41(13) . . ? C2 C3 C25 127.60(13) . . ? C4 C3 C25 125.47(13) . . ? C2 C3 Fe 69.56(8) . . ? C4 C3 Fe 70.41(8) . . ? C25 C3 Fe 131.14(10) . . ? C9 C4 C3 131.39(14) . . ? C9 C4 C5 119.99(14) . . ? C3 C4 C5 108.61(13) . . ? C9 C4 Fe 125.75(10) . . ? C3 C4 Fe 69.01(8) . . ? C5 C4 Fe 70.75(8) . . ? C7 C6 C5 119.53(15) . . ? C6 C7 C8 121.78(15) . . ? C9 C8 C7 120.97(15) . . ? C8 C9 C4 119.10(15) . . ? C6 C5 C1 133.68(15) . . ? C6 C5 C4 118.46(14) . . ? C1 C5 C4 107.81(13) . . ? C6 C5 Fe 130.10(11) . . ? C1 C5 Fe 68.11(8) . . ? C4 C5 Fe 68.94(8) . . ? C11 C10 C14 106.45(13) . . ? C11 C10 C31 126.63(14) . . ? C14 C10 C31 126.28(13) . . ? C11 C10 Fe 69.45(8) . . ? C14 C10 Fe 70.50(8) . . ? C31 C10 Fe 131.93(10) . . ? C10 C11 C12 110.76(13) . . ? C10 C11 Fe 70.16(8) . . ? C12 C11 Fe 69.85(8) . . ? C11 C12 C13 106.35(13) . . ? C11 C12 C37 121.82(14) . . ? C13 C12 C37 130.73(15) . . ? C11 C12 Fe 69.66(8) . . ? C13 C12 Fe 71.51(8) . . ? C37 C12 Fe 132.56(11) . . ? C18 C13 C12 133.30(14) . . ? C18 C13 C14 118.51(14) . . ? C12 C13 C14 108.15(13) . . ? C18 C13 Fe 129.98(10) . . ? C12 C13 Fe 68.09(8) . . ? C14 C13 Fe 69.11(8) . . ? C15 C14 C10 131.98(14) . . ? C15 C14 C13 119.89(14) . . ? C10 C14 C13 108.12(13) . . ? C15 C14 Fe 125.55(10) . . ? C10 C14 Fe 68.97(8) . . ? C13 C14 Fe 70.49(8) . . ? C16 C15 C14 119.24(15) . . ? C15 C16 C17 120.94(15) . . ? C18 C17 C16 121.69(15) . . ? C17 C18 C13 119.57(15) . . ? C1 C19 C24 116.53(13) . . ? C1 C19 C20 109.49(12) . . ? C24 C19 C20 110.06(14) . . ? C21 C20 C19 111.82(14) . . ? C22 C21 C20 111.79(14) . . ? C21 C22 C23 110.93(15) . . ? C22 C23 C24 111.02(15) . . ? C19 C24 C23 111.35(15) . . ? C3 C25 C30 113.30(12) . . ? C3 C25 C26 109.39(12) . . ? C30 C25 C26 108.95(12) . . ? C27 C26 C25 112.29(13) . . ? C28 C27 C26 111.64(13) . . ? C27 C28 C29 111.22(13) . . ? C30 C29 C28 110.78(13) . . ? C29 C30 C25 111.57(13) . . ? C10 C31 C32 111.92(13) . . ? C10 C31 C36 109.35(12) . . ? C32 C31 C36 109.72(12) . . ? C31 C32 C33 112.80(14) . . ? C34 C33 C32 111.00(14) . . ? C35 C34 C33 110.49(14) . . ? C34 C35 C36 111.02(13) . . ? C35 C36 C31 112.62(13) . . ? C12 C37 C38 117.03(14) . . ? C12 C37 C42 108.65(12) . . ? C38 C37 C42 110.49(14) . . ? C37 C38 C39 111.37(15) . . ? C40 C39 C38 111.22(16) . . ? C41 C40 C39 110.73(15) . . ? C40 C41 C42 112.67(15) . . ? C41 C42 C37 112.03(13) . . ? 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 C11 Fe C1 C2 -137.24(9) . . . . ? C12 Fe C1 C2 -93.35(9) . . . . ? C3 Fe C1 C2 35.96(8) . . . . ? C10 Fe C1 C2 -177.51(8) . . . . ? C4 Fe C1 C2 79.60(9) . . . . ? C14 Fe C1 C2 150.3(4) . . . . ? C13 Fe C1 C2 -58.11(14) . . . . ? C5 Fe C1 C2 116.40(12) . . . . ? C11 Fe C1 C5 106.36(9) . . . . ? C2 Fe C1 C5 -116.40(12) . . . . ? C12 Fe C1 C5 150.26(9) . . . . ? C3 Fe C1 C5 -80.44(9) . . . . ? C10 Fe C1 C5 66.10(11) . . . . ? C4 Fe C1 C5 -36.80(8) . . . . ? C14 Fe C1 C5 33.9(5) . . . . ? C13 Fe C1 C5 -174.51(10) . . . . ? C11 Fe C1 C19 -21.53(17) . . . . ? C2 Fe C1 C19 115.71(18) . . . . ? C12 Fe C1 C19 22.37(17) . . . . ? C3 Fe C1 C19 151.67(17) . . . . ? C10 Fe C1 C19 -61.79(18) . . . . ? C4 Fe C1 C19 -164.69(17) . . . . ? C14 Fe C1 C19 -94.0(5) . . . . ? C13 Fe C1 C19 57.6(2) . . . . ? C5 Fe C1 C19 -127.89(19) . . . . ? C5 C1 C2 C3 3.98(16) . . . . ? C19 C1 C2 C3 174.22(13) . . . . ? Fe C1 C2 C3 -58.30(10) . . . . ? C5 C1 C2 Fe 62.28(10) . . . . ? C19 C1 C2 Fe -127.48(14) . . . . ? C11 Fe C2 C3 -172.43(9) . . . . ? C12 Fe C2 C3 -133.66(9) . . . . ? C1 Fe C2 C3 122.07(12) . . . . ? C10 Fe C2 C3 139.7(5) . . . . ? C4 Fe C2 C3 38.99(9) . . . . ? C14 Fe C2 C3 -51.85(14) . . . . ? C13 Fe C2 C3 -89.88(10) . . . . ? C5 Fe C2 C3 82.92(9) . . . . ? C11 Fe C2 C1 65.49(12) . . . . ? C12 Fe C2 C1 104.27(9) . . . . ? C3 Fe C2 C1 -122.07(12) . . . . ? C10 Fe C2 C1 17.6(6) . . . . ? C4 Fe C2 C1 -83.08(9) . . . . ? C14 Fe C2 C1 -173.92(10) . . . . ? C13 Fe C2 C1 148.04(9) . . . . ? C5 Fe C2 C1 -39.16(9) . . . . ? C1 C2 C3 C4 -2.93(16) . . . . ? Fe C2 C3 C4 -61.14(9) . . . . ? C1 C2 C3 C25 -174.97(13) . . . . ? Fe C2 C3 C25 126.82(15) . . . . ? C1 C2 C3 Fe 58.21(10) . . . . ? C11 Fe C3 C2 56.0(6) . . . . ? C12 Fe C3 C2 68.64(12) . . . . ? C1 Fe C3 C2 -36.13(9) . . . . ? C10 Fe C3 C2 -173.43(10) . . . . ? C4 Fe C3 C2 -116.91(12) . . . . ? C14 Fe C3 C2 150.81(9) . . . . ? C13 Fe C3 C2 107.50(9) . . . . ? C5 Fe C3 C2 -79.70(9) . . . . ? C11 Fe C3 C4 172.9(5) . . . . ? C2 Fe C3 C4 116.91(12) . . . . ? C12 Fe C3 C4 -174.45(9) . . . . ? C1 Fe C3 C4 80.78(9) . . . . ? C10 Fe C3 C4 -56.51(13) . . . . ? C14 Fe C3 C4 -92.28(9) . . . . ? C13 Fe C3 C4 -135.59(9) . . . . ? C5 Fe C3 C4 37.21(9) . . . . ? C11 Fe C3 C25 -66.6(6) . . . . ? C2 Fe C3 C25 -122.63(17) . . . . ? C12 Fe C3 C25 -53.99(17) . . . . ? C1 Fe C3 C25 -158.76(15) . . . . ? C10 Fe C3 C25 63.95(18) . . . . ? C4 Fe C3 C25 120.46(17) . . . . ? C14 Fe C3 C25 28.18(15) . . . . ? C13 Fe C3 C25 -15.13(15) . . . . ? C5 Fe C3 C25 157.68(15) . . . . ? C2 C3 C4 C9 -179.68(14) . . . . ? C25 C3 C4 C9 -7.4(2) . . . . ? Fe C3 C4 C9 119.74(16) . . . . ? C2 C3 C4 C5 0.70(15) . . . . ? C25 C3 C4 C5 172.96(13) . . . . ? Fe C3 C4 C5 -59.88(10) . . . . ? C2 C3 C4 Fe 60.58(9) . . . . ? C25 C3 C4 Fe -127.15(14) . . . . ? C11 Fe C4 C9 54.77(19) . . . . ? C2 Fe C4 C9 -165.44(15) . . . . ? C12 Fe C4 C9 -92.5(5) . . . . ? C1 Fe C4 C9 150.59(15) . . . . ? C3 Fe C4 C9 -126.62(17) . . . . ? C10 Fe C4 C9 20.97(15) . . . . ? C14 Fe C4 C9 -22.43(15) . . . . ? C13 Fe C4 C9 -60.84(16) . . . . ? C5 Fe C4 C9 113.64(17) . . . . ? C11 Fe C4 C3 -178.61(10) . . . . ? C2 Fe C4 C3 -38.82(9) . . . . ? C12 Fe C4 C3 34.2(5) . . . . ? C1 Fe C4 C3 -82.79(9) . . . . ? C10 Fe C4 C3 147.60(9) . . . . ? C14 Fe C4 C3 104.19(9) . . . . ? C13 Fe C4 C3 65.78(11) . . . . ? C5 Fe C4 C3 -119.74(12) . . . . ? C11 Fe C4 C5 -58.88(14) . . . . ? C2 Fe C4 C5 80.92(9) . . . . ? C12 Fe C4 C5 153.9(4) . . . . ? C1 Fe C4 C5 36.95(9) . . . . ? C3 Fe C4 C5 119.74(12) . . . . ? C10 Fe C4 C5 -92.67(9) . . . . ? C14 Fe C4 C5 -136.08(9) . . . . ? C13 Fe C4 C5 -174.48(8) . . . . ? C5 C6 C7 C8 -1.8(2) . . . . ? C6 C7 C8 C9 2.2(2) . . . . ? C7 C8 C9 C4 0.7(2) . . . . ? C3 C4 C9 C8 176.45(15) . . . . ? C5 C4 C9 C8 -4.0(2) . . . . ? Fe C4 C9 C8 -90.90(17) . . . . ? C7 C6 C5 C1 -178.45(15) . . . . ? C7 C6 C5 C4 -1.5(2) . . . . ? C7 C6 C5 Fe 84.06(18) . . . . ? C2 C1 C5 C6 173.78(15) . . . . ? C19 C1 C5 C6 4.6(3) . . . . ? Fe C1 C5 C6 -125.19(17) . . . . ? C2 C1 C5 C4 -3.43(15) . . . . ? C19 C1 C5 C4 -172.63(14) . . . . ? Fe C1 C5 C4 57.60(10) . . . . ? C2 C1 C5 Fe -61.03(10) . . . . ? C19 C1 C5 Fe 129.77(16) . . . . ? C9 C4 C5 C6 4.3(2) . . . . ? C3 C4 C5 C6 -175.99(13) . . . . ? Fe C4 C5 C6 125.20(13) . . . . ? C9 C4 C5 C1 -177.95(13) . . . . ? C3 C4 C5 C1 1.72(16) . . . . ? Fe C4 C5 C1 -57.09(10) . . . . ? C9 C4 C5 Fe -120.86(13) . . . . ? C3 C4 C5 Fe 58.81(10) . . . . ? C11 Fe C5 C6 37.42(17) . . . . ? C2 Fe C5 C6 168.66(17) . . . . ? C12 Fe C5 C6 75.59(19) . . . . ? C1 Fe C5 C6 129.40(19) . . . . ? C3 Fe C5 C6 -147.52(16) . . . . ? C10 Fe C5 C6 -6.04(16) . . . . ? C4 Fe C5 C6 -110.08(18) . . . . ? C14 Fe C5 C6 -45.22(18) . . . . ? C13 Fe C5 C6 -76.1(5) . . . . ? C11 Fe C5 C1 -91.98(9) . . . . ? C2 Fe C5 C1 39.26(9) . . . . ? C12 Fe C5 C1 -53.82(14) . . . . ? C3 Fe C5 C1 83.07(9) . . . . ? C10 Fe C5 C1 -135.44(9) . . . . ? C4 Fe C5 C1 120.52(12) . . . . ? C14 Fe C5 C1 -174.63(9) . . . . ? C13 Fe C5 C1 154.5(4) . . . . ? C11 Fe C5 C4 147.50(8) . . . . ? C2 Fe C5 C4 -81.26(9) . . . . ? C12 Fe C5 C4 -174.34(10) . . . . ? C1 Fe C5 C4 -120.52(12) . . . . ? C3 Fe C5 C4 -37.45(8) . . . . ? C10 Fe C5 C4 104.04(9) . . . . ? C14 Fe C5 C4 64.85(11) . . . . ? C13 Fe C5 C4 34.0(5) . . . . ? C2 Fe C10 C11 53.0(6) . . . . ? C12 Fe C10 C11 -35.96(9) . . . . ? C1 Fe C10 C11 68.75(12) . . . . ? C3 Fe C10 C11 -172.54(10) . . . . ? C4 Fe C10 C11 151.10(9) . . . . ? C14 Fe C10 C11 -116.97(12) . . . . ? C13 Fe C10 C11 -79.47(9) . . . . ? C5 Fe C10 C11 107.79(9) . . . . ? C11 Fe C10 C14 116.97(12) . . . . ? C2 Fe C10 C14 169.9(5) . . . . ? C12 Fe C10 C14 81.01(9) . . . . ? C1 Fe C10 C14 -174.28(8) . . . . ? C3 Fe C10 C14 -55.57(13) . . . . ? C4 Fe C10 C14 -91.93(9) . . . . ? C13 Fe C10 C14 37.51(8) . . . . ? C5 Fe C10 C14 -135.23(8) . . . . ? C11 Fe C10 C31 -121.32(18) . . . . ? C2 Fe C10 C31 -68.4(6) . . . . ? C12 Fe C10 C31 -157.28(16) . . . . ? C1 Fe C10 C31 -52.57(17) . . . . ? C3 Fe C10 C31 66.14(18) . . . . ? C4 Fe C10 C31 29.78(16) . . . . ? C14 Fe C10 C31 121.71(17) . . . . ? C13 Fe C10 C31 159.22(16) . . . . ? C5 Fe C10 C31 -13.53(16) . . . . ? C14 C10 C11 C12 -3.05(16) . . . . ? C31 C10 C11 C12 -174.27(13) . . . . ? Fe C10 C11 C12 58.11(10) . . . . ? C14 C10 C11 Fe -61.15(9) . . . . ? C31 C10 C11 Fe 127.63(15) . . . . ? C2 Fe C11 C10 -173.16(9) . . . . ? C12 Fe C11 C10 122.26(13) . . . . ? C1 Fe C11 C10 -133.85(9) . . . . ? C3 Fe C11 C10 136.4(5) . . . . ? C4 Fe C11 C10 -51.75(14) . . . . ? C14 Fe C11 C10 38.93(9) . . . . ? C13 Fe C11 C10 82.99(9) . . . . ? C5 Fe C11 C10 -89.87(10) . . . . ? C2 Fe C11 C12 64.58(12) . . . . ? C1 Fe C11 C12 103.90(10) . . . . ? C3 Fe C11 C12 14.2(6) . . . . ? C10 Fe C11 C12 -122.26(13) . . . . ? C4 Fe C11 C12 -174.01(10) . . . . ? C14 Fe C11 C12 -83.33(10) . . . . ? C13 Fe C11 C12 -39.27(9) . . . . ? C5 Fe C11 C12 147.87(9) . . . . ? C10 C11 C12 C13 4.25(16) . . . . ? Fe C11 C12 C13 62.53(9) . . . . ? C10 C11 C12 C37 173.48(13) . . . . ? Fe C11 C12 C37 -128.23(14) . . . . ? C10 C11 C12 Fe -58.28(10) . . . . ? C2 Fe C12 C11 -137.74(9) . . . . ? C1 Fe C12 C11 -93.82(10) . . . . ? C3 Fe C12 C11 -177.86(9) . . . . ? C10 Fe C12 C11 35.88(9) . . . . ? C4 Fe C12 C11 152.0(4) . . . . ? C14 Fe C12 C11 79.46(9) . . . . ? C13 Fe C12 C11 116.14(12) . . . . ? C5 Fe C12 C11 -58.63(14) . . . . ? C11 Fe C12 C13 -116.14(12) . . . . ? C2 Fe C12 C13 106.12(9) . . . . ? C1 Fe C12 C13 150.03(8) . . . . ? C3 Fe C12 C13 65.99(11) . . . . ? C10 Fe C12 C13 -80.26(9) . . . . ? C4 Fe C12 C13 35.9(5) . . . . ? C14 Fe C12 C13 -36.68(8) . . . . ? C5 Fe C12 C13 -174.77(10) . . . . ? C11 Fe C12 C37 115.0(2) . . . . ? C2 Fe C12 C37 -22.72(18) . . . . ? C1 Fe C12 C37 21.20(18) . . . . ? C3 Fe C12 C37 -62.84(19) . . . . ? C10 Fe C12 C37 150.91(18) . . . . ? C4 Fe C12 C37 -93.0(5) . . . . ? C14 Fe C12 C37 -165.52(18) . . . . ? C13 Fe C12 C37 -128.8(2) . . . . ? C5 Fe C12 C37 56.4(2) . . . . ? C11 C12 C13 C18 173.76(15) . . . . ? C37 C12 C13 C18 5.9(3) . . . . ? Fe C12 C13 C18 -124.93(17) . . . . ? C11 C12 C13 C14 -3.74(15) . . . . ? C37 C12 C13 C14 -171.65(14) . . . . ? Fe C12 C13 C14 57.57(10) . . . . ? C11 C12 C13 Fe -61.31(10) . . . . ? C37 C12 C13 Fe 130.78(16) . . . . ? C11 Fe C13 C18 168.21(17) . . . . ? C2 Fe C13 C18 36.98(17) . . . . ? C12 Fe C13 C18 128.86(18) . . . . ? C1 Fe C13 C18 74.84(19) . . . . ? C3 Fe C13 C18 -6.38(16) . . . . ? C10 Fe C13 C18 -147.91(16) . . . . ? C4 Fe C13 C18 -45.32(18) . . . . ? C14 Fe C13 C18 -110.28(18) . . . . ? C5 Fe C13 C18 -75.3(5) . . . . ? C11 Fe C13 C12 39.35(8) . . . . ? C2 Fe C13 C12 -91.88(9) . . . . ? C1 Fe C13 C12 -54.02(14) . . . . ? C3 Fe C13 C12 -135.24(9) . . . . ? C10 Fe C13 C12 83.23(9) . . . . ? C4 Fe C13 C12 -174.18(9) . . . . ? C14 Fe C13 C12 120.86(12) . . . . ? C5 Fe C13 C12 155.9(4) . . . . ? C11 Fe C13 C14 -81.51(9) . . . . ? C2 Fe C13 C14 147.26(8) . . . . ? C12 Fe C13 C14 -120.86(12) . . . . ? C1 Fe C13 C14 -174.88(10) . . . . ? C3 Fe C13 C14 103.90(9) . . . . ? C10 Fe C13 C14 -37.63(8) . . . . ? C4 Fe C13 C14 64.96(11) . . . . ? C5 Fe C13 C14 35.0(5) . . . . ? C11 C10 C14 C15 179.95(15) . . . . ? C31 C10 C14 C15 -8.8(2) . . . . ? Fe C10 C14 C15 119.48(16) . . . . ? C11 C10 C14 C13 0.62(15) . . . . ? C31 C10 C14 C13 171.88(13) . . . . ? Fe C10 C14 C13 -59.85(10) . . . . ? C11 C10 C14 Fe 60.47(9) . . . . ? C31 C10 C14 Fe -128.27(14) . . . . ? C18 C13 C14 C15 4.6(2) . . . . ? C12 C13 C14 C15 -177.47(13) . . . . ? Fe C13 C14 C15 -120.52(13) . . . . ? C18 C13 C14 C10 -175.97(12) . . . . ? C12 C13 C14 C10 1.96(15) . . . . ? Fe C13 C14 C10 58.90(10) . . . . ? C18 C13 C14 Fe 125.12(13) . . . . ? C12 C13 C14 Fe -56.94(10) . . . . ? C11 Fe C14 C15 -166.11(15) . . . . ? C2 Fe C14 C15 54.52(18) . . . . ? C12 Fe C14 C15 150.06(15) . . . . ? C1 Fe C14 C15 -91.0(5) . . . . ? C3 Fe C14 C15 20.77(15) . . . . ? C10 Fe C14 C15 -127.31(17) . . . . ? C4 Fe C14 C15 -22.67(15) . . . . ? C13 Fe C14 C15 113.37(17) . . . . ? C5 Fe C14 C15 -60.96(16) . . . . ? C11 Fe C14 C10 -38.80(8) . . . . ? C2 Fe C14 C10 -178.17(10) . . . . ? C12 Fe C14 C10 -82.63(9) . . . . ? C1 Fe C14 C10 36.3(5) . . . . ? C3 Fe C14 C10 148.08(8) . . . . ? C4 Fe C14 C10 104.64(9) . . . . ? C13 Fe C14 C10 -119.32(12) . . . . ? C5 Fe C14 C10 66.35(11) . . . . ? C11 Fe C14 C13 80.52(9) . . . . ? C2 Fe C14 C13 -58.85(13) . . . . ? C12 Fe C14 C13 36.69(9) . . . . ? C1 Fe C14 C13 155.7(4) . . . . ? C3 Fe C14 C13 -92.60(9) . . . . ? C10 Fe C14 C13 119.32(12) . . . . ? C4 Fe C14 C13 -136.04(9) . . . . ? C5 Fe C14 C13 -174.33(9) . . . . ? C10 C14 C15 C16 177.18(15) . . . . ? C13 C14 C15 C16 -3.5(2) . . . . ? Fe C14 C15 C16 -89.96(17) . . . . ? C14 C15 C16 C17 0.3(2) . . . . ? C15 C16 C17 C18 2.0(2) . . . . ? C16 C17 C18 C13 -0.8(2) . . . . ? C12 C13 C18 C17 -179.70(15) . . . . ? C14 C13 C18 C17 -2.4(2) . . . . ? Fe C13 C18 C17 83.36(18) . . . . ? C2 C1 C19 C24 148.45(15) . . . . ? C5 C1 C19 C24 -43.8(2) . . . . ? Fe C1 C19 C24 57.7(2) . . . . ? C2 C1 C19 C20 -85.87(18) . . . . ? C5 C1 C19 C20 81.84(19) . . . . ? Fe C1 C19 C20 -176.65(12) . . . . ? C1 C19 C20 C21 176.05(14) . . . . ? C24 C19 C20 C21 -54.64(19) . . . . ? C19 C20 C21 C22 54.4(2) . . . . ? C20 C21 C22 C23 -54.7(2) . . . . ? C21 C22 C23 C24 56.1(2) . . . . ? C1 C19 C24 C23 -178.41(15) . . . . ? C20 C19 C24 C23 56.2(2) . . . . ? C22 C23 C24 C19 -57.5(2) . . . . ? C2 C3 C25 C30 -16.7(2) . . . . ? C4 C3 C25 C30 172.68(13) . . . . ? Fe C3 C25 C30 78.33(16) . . . . ? C2 C3 C25 C26 105.07(16) . . . . ? C4 C3 C25 C26 -65.55(18) . . . . ? Fe C3 C25 C26 -159.90(11) . . . . ? C3 C25 C26 C27 -179.84(12) . . . . ? C30 C25 C26 C27 -55.49(17) . . . . ? C25 C26 C27 C28 54.74(18) . . . . ? C26 C27 C28 C29 -54.01(18) . . . . ? C27 C28 C29 C30 55.53(19) . . . . ? C28 C29 C30 C25 -58.02(17) . . . . ? C3 C25 C30 C29 179.12(12) . . . . ? C26 C25 C30 C29 57.11(16) . . . . ? C11 C10 C31 C32 -14.3(2) . . . . ? C14 C10 C31 C32 176.19(14) . . . . ? Fe C10 C31 C32 80.31(17) . . . . ? C11 C10 C31 C36 107.52(16) . . . . ? C14 C10 C31 C36 -62.02(18) . . . . ? Fe C10 C31 C36 -157.90(11) . . . . ? C10 C31 C32 C33 174.89(13) . . . . ? C36 C31 C32 C33 53.31(18) . . . . ? C31 C32 C33 C34 -56.2(2) . . . . ? C32 C33 C34 C35 56.8(2) . . . . ? C33 C34 C35 C36 -56.63(19) . . . . ? C34 C35 C36 C31 55.57(18) . . . . ? C10 C31 C36 C35 -176.13(13) . . . . ? C32 C31 C36 C35 -53.02(17) . . . . ? C11 C12 C37 C38 147.58(16) . . . . ? C13 C12 C37 C38 -46.1(2) . . . . ? Fe C12 C37 C38 56.8(2) . . . . ? C11 C12 C37 C42 -86.48(18) . . . . ? C13 C12 C37 C42 79.84(19) . . . . ? Fe C12 C37 C42 -177.30(12) . . . . ? C12 C37 C38 C39 -179.50(16) . . . . ? C42 C37 C38 C39 55.5(2) . . . . ? C37 C38 C39 C40 -57.4(2) . . . . ? C38 C39 C40 C41 55.8(2) . . . . ? C39 C40 C41 C42 -54.0(2) . . . . ? C40 C41 C42 C37 53.2(2) . . . . ? C12 C37 C42 C41 177.06(15) . . . . ? C38 C37 C42 C41 -53.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 72.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.648 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.047 _iucr_refine_instructions_details ; TITL mima05 in P2(1)/c CELL 1.54184 10.1411 15.4986 21.3658 90.000 101.712 90.000 ZERR 4.00 0.0002 0.0002 0.0004 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H FE UNIT 168 216 4 SIZE 0.05 0.05 0.03 TEMP -173 ACTA 145 CONF FMAP 2 PLAN 10 L.S. 4 OMIT -4 0 8 OMIT -6 9 3 OMIT 2 3 1 OMIT -10 3 20 OMIT 4 10 19 OMIT -9 3 22 WGHT 0.053800 0.198300 FVAR 2.75306 FE 3 0.514828 0.421854 0.198117 11.00000 0.01723 0.01196 = 0.01374 0.00069 0.00453 0.00002 C1 1 0.606626 0.515439 0.261165 11.00000 0.02368 0.01302 = 0.01680 -0.00030 0.00284 -0.00127 C2 1 0.476171 0.543778 0.228665 11.00000 0.02259 0.01283 = 0.01703 0.00013 0.00632 0.00012 AFIX 43 H2 2 0.405237 0.560161 0.249197 11.00000 -1.20000 AFIX 0 C3 1 0.467579 0.543978 0.161200 11.00000 0.02054 0.01170 = 0.01689 0.00065 0.00526 -0.00018 C4 1 0.598626 0.519240 0.151043 11.00000 0.01901 0.01156 = 0.01859 0.00142 0.00467 -0.00124 C6 1 0.824056 0.482959 0.214453 11.00000 0.01870 0.01848 = 0.02745 0.00319 0.00148 -0.00124 AFIX 43 H6 2 0.883813 0.473425 0.254238 11.00000 -1.20000 AFIX 0 C7 1 0.869641 0.477520 0.158738 11.00000 0.01880 0.01843 = 0.03671 0.00434 0.00867 0.00106 AFIX 43 H7 2 0.962219 0.465727 0.160408 11.00000 -1.20000 AFIX 0 C8 1 0.782149 0.489050 0.098105 11.00000 0.02679 0.01689 = 0.02906 0.00118 0.01488 0.00038 AFIX 43 H8 2 0.816684 0.482802 0.060216 11.00000 -1.20000 AFIX 0 C9 1 0.649353 0.508953 0.093668 11.00000 0.02381 0.01455 = 0.01855 0.00121 0.00766 -0.00104 AFIX 43 H9 2 0.591449 0.515873 0.053052 11.00000 -1.20000 AFIX 0 C5 1 0.685503 0.503139 0.212539 11.00000 0.02015 0.01254 = 0.02003 0.00035 0.00257 -0.00299 C10 1 0.569269 0.298537 0.175935 11.00000 0.02040 0.01191 = 0.01705 0.00018 0.00463 0.00040 C11 1 0.542789 0.301022 0.238988 11.00000 0.02459 0.01320 = 0.01665 0.00274 0.00526 0.00042 AFIX 43 H11 2 0.605680 0.285308 0.276556 11.00000 -1.20000 AFIX 0 C12 1 0.408918 0.330337 0.237935 11.00000 0.02605 0.01258 = 0.02091 0.00152 0.01014 -0.00083 C13 1 0.345781 0.340608 0.171530 11.00000 0.01955 0.01159 = 0.02267 -0.00074 0.00699 -0.00251 C14 1 0.445634 0.322764 0.133314 11.00000 0.01959 0.01153 = 0.01765 -0.00045 0.00532 -0.00151 C15 1 0.411167 0.331677 0.065438 11.00000 0.02464 0.01512 = 0.01811 -0.00010 0.00391 -0.00038 AFIX 43 H15 2 0.477354 0.323266 0.040295 11.00000 -1.20000 AFIX 0 C16 1 0.282105 0.352409 0.037103 11.00000 0.02928 0.01653 = 0.01961 -0.00063 -0.00237 -0.00063 AFIX 43 H16 2 0.258625 0.358137 -0.008062 11.00000 -1.20000 AFIX 0 C17 1 0.181712 0.365635 0.074394 11.00000 0.02012 0.01784 = 0.03333 -0.00200 -0.00174 -0.00047 AFIX 43 H17 2 0.091987 0.378214 0.053308 11.00000 -1.20000 AFIX 0 C18 1 0.211376 0.360665 0.139393 11.00000 0.01885 0.01600 = 0.03206 -0.00196 0.00666 -0.00140 AFIX 43 H18 2 0.143245 0.370457 0.163224 11.00000 -1.20000 AFIX 0 C19 1 0.649324 0.516468 0.332999 11.00000 0.02649 0.01970 = 0.01610 -0.00012 0.00173 -0.00214 AFIX 13 H19 2 0.565800 0.508475 0.350448 11.00000 -1.20000 AFIX 0 C20 1 0.705809 0.606065 0.355074 11.00000 0.02911 0.01690 = 0.02166 -0.00066 -0.00137 0.00256 AFIX 23 H20A 2 0.787235 0.617323 0.337461 11.00000 -1.20000 H20B 2 0.638053 0.650643 0.338071 11.00000 -1.20000 AFIX 0 C21 1 0.741828 0.612908 0.428000 11.00000 0.04278 0.02566 = 0.02401 -0.00594 -0.00265 0.00649 AFIX 23 H21A 2 0.784482 0.669568 0.440154 11.00000 -1.20000 H21B 2 0.658411 0.609696 0.445232 11.00000 -1.20000 AFIX 0 C22 1 0.837467 0.541332 0.457503 11.00000 0.03292 0.02778 = 0.02021 -0.00171 -0.00198 0.00248 AFIX 23 H22A 2 0.852713 0.545103 0.504681 11.00000 -1.20000 H22B 2 0.925323 0.548885 0.444761 11.00000 -1.20000 AFIX 0 C23 1 0.780014 0.452939 0.435872 11.00000 0.04624 0.02421 = 0.02044 0.00272 -0.00353 0.00031 AFIX 23 H23A 2 0.696882 0.442996 0.452402 11.00000 -1.20000 H23B 2 0.845942 0.407730 0.453743 11.00000 -1.20000 AFIX 0 C24 1 0.747926 0.446306 0.362888 11.00000 0.05141 0.01966 = 0.02069 -0.00086 -0.00553 0.00611 AFIX 23 H24A 2 0.832278 0.451777 0.346637 11.00000 -1.20000 H24B 2 0.708591 0.388930 0.350123 11.00000 -1.20000 AFIX 0 C25 1 0.353037 0.575405 0.110493 11.00000 0.01921 0.01538 = 0.01608 0.00078 0.00387 0.00083 AFIX 13 H25 2 0.337945 0.532793 0.074601 11.00000 -1.20000 AFIX 0 C26 1 0.391024 0.662975 0.084492 11.00000 0.02014 0.01725 = 0.01943 0.00305 0.00389 -0.00025 AFIX 23 H26A 2 0.411603 0.704829 0.120147 11.00000 -1.20000 H26B 2 0.473277 0.655667 0.066775 11.00000 -1.20000 AFIX 0 C27 1 0.278473 0.699125 0.032604 11.00000 0.02675 0.02059 = 0.02270 0.00560 0.00253 0.00141 AFIX 23 H27A 2 0.304620 0.757041 0.019816 11.00000 -1.20000 H27B 2 0.265999 0.661216 -0.005438 11.00000 -1.20000 AFIX 0 C28 1 0.146013 0.705780 0.055574 11.00000 0.02239 0.02075 = 0.03010 0.00345 0.00066 0.00515 AFIX 23 H28A 2 0.073779 0.724371 0.019665 11.00000 -1.20000 H28B 2 0.154573 0.749947 0.089637 11.00000 -1.20000 AFIX 0 C29 1 0.107623 0.619239 0.081377 11.00000 0.01895 0.02220 = 0.03155 0.00209 0.00383 0.00157 AFIX 23 H29A 2 0.024559 0.626320 0.098479 11.00000 -1.20000 H29B 2 0.089096 0.576641 0.046155 11.00000 -1.20000 AFIX 0 C30 1 0.220995 0.585812 0.134223 11.00000 0.02031 0.01830 = 0.02324 0.00138 0.00679 0.00122 AFIX 23 H30A 2 0.194542 0.529411 0.149619 11.00000 -1.20000 H30B 2 0.235068 0.626605 0.170631 11.00000 -1.20000 AFIX 0 C31 1 0.693940 0.264050 0.156747 11.00000 0.01876 0.01570 = 0.02089 0.00125 0.00581 0.00101 AFIX 13 H31 2 0.723732 0.306314 0.127076 11.00000 -1.20000 AFIX 0 C32 1 0.808797 0.250969 0.214354 11.00000 0.02228 0.02102 = 0.02858 -0.00299 0.00036 0.00229 AFIX 23 H32A 2 0.776549 0.214568 0.246248 11.00000 -1.20000 H32B 2 0.835183 0.307641 0.234407 11.00000 -1.20000 AFIX 0 C33 1 0.932166 0.208522 0.196718 11.00000 0.01830 0.03021 = 0.04598 -0.00329 0.00101 0.00253 AFIX 23 H33A 2 0.970699 0.247507 0.168390 11.00000 -1.20000 H33B 2 1.001480 0.198847 0.235954 11.00000 -1.20000 AFIX 0 C34 1 0.895242 0.122639 0.162920 11.00000 0.02300 0.02679 = 0.03389 0.00023 0.00678 0.00769 AFIX 23 H34A 2 0.975797 0.097567 0.150320 11.00000 -1.20000 H34B 2 0.864107 0.081846 0.192508 11.00000 -1.20000 AFIX 0 C35 1 0.784616 0.135213 0.103821 11.00000 0.02950 0.02338 = 0.02455 -0.00034 0.00942 0.00830 AFIX 23 H35A 2 0.759087 0.078558 0.083550 11.00000 -1.20000 H35B 2 0.818747 0.171809 0.072604 11.00000 -1.20000 AFIX 0 C36 1 0.660688 0.177692 0.121075 11.00000 0.02147 0.01845 = 0.02023 -0.00180 0.00437 0.00255 AFIX 23 H36A 2 0.620738 0.137765 0.148265 11.00000 -1.20000 H36B 2 0.592757 0.188002 0.081450 11.00000 -1.20000 AFIX 0 C37 1 0.349618 0.330273 0.297061 11.00000 0.03207 0.01766 = 0.02245 -0.00060 0.01341 -0.00271 AFIX 13 H37 2 0.426538 0.336950 0.334291 11.00000 -1.20000 AFIX 0 C38 1 0.249573 0.401202 0.302763 11.00000 0.05412 0.02376 = 0.04407 0.00687 0.03188 0.00786 AFIX 23 H38A 2 0.172272 0.397649 0.266167 11.00000 -1.20000 H38B 2 0.293162 0.458077 0.301093 11.00000 -1.20000 AFIX 0 C39 1 0.198593 0.393674 0.365320 11.00000 0.04886 0.02505 = 0.04017 -0.00250 0.02891 -0.00030 AFIX 23 H39A 2 0.274791 0.401940 0.401935 11.00000 -1.20000 H39B 2 0.131658 0.439669 0.366998 11.00000 -1.20000 AFIX 0 C40 1 0.134035 0.305707 0.370899 11.00000 0.03236 0.03142 = 0.03388 0.00118 0.01725 -0.00163 AFIX 23 H40A 2 0.107064 0.301287 0.412792 11.00000 -1.20000 H40B 2 0.052026 0.299897 0.336987 11.00000 -1.20000 AFIX 0 C41 1 0.231074 0.233844 0.364631 11.00000 0.04450 0.02224 = 0.03750 0.00547 0.02518 -0.00107 AFIX 23 H41A 2 0.184354 0.177771 0.364721 11.00000 -1.20000 H41B 2 0.306636 0.234970 0.402128 11.00000 -1.20000 AFIX 0 C42 1 0.287309 0.240927 0.303765 11.00000 0.02326 0.01683 = 0.02291 0.00074 0.00993 -0.00089 AFIX 23 H42A 2 0.214025 0.230295 0.266249 11.00000 -1.20000 H42B 2 0.356846 0.195961 0.304252 11.00000 -1.20000 HKLF 4 ; # Attachment '- mima13.cif' data_mima13 _database_code_depnum_ccdc_archive 'CCDC 884306' #TrackingRef '- mima13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 Fe' _chemical_formula_weight 510.56 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.3520(4) _cell_length_b 9.6436(2) _cell_length_c 17.7391(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.946(4) _cell_angle_gamma 90.00 _cell_volume 2798.62(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 32590 _cell_measurement_theta_min 2.1547 _cell_measurement_theta_max 29.2718 _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95739 _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 '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 109058 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.88 _reflns_number_total 6673 _reflns_number_gt 5044 _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 of the C2 and C19 atoms were refined freely. ; _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^)+(0.0352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6673 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _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 Fe Fe 0.737355(10) 0.343218(17) 0.522399(10) 0.00943(5) Uani 1 1 d . . . C1 C 0.75126(7) 0.44598(12) 0.42518(7) 0.0123(3) Uani 1 1 d . . . C2 C 0.71730(8) 0.31067(13) 0.39927(8) 0.0126(3) Uani 1 1 d . . . H2 H 0.7427(8) 0.2404(13) 0.3819(8) 0.012(3) Uiso 1 1 d . . . C3 C 0.64215(8) 0.29652(12) 0.40331(7) 0.0118(3) Uani 1 1 d . . . C4 C 0.62516(7) 0.43048(12) 0.42854(7) 0.0118(3) Uani 1 1 d . . . C5 C 0.69259(7) 0.52185(12) 0.44218(7) 0.0121(3) Uani 1 1 d . . . C6 C 0.68634(8) 0.66578(13) 0.45912(7) 0.0152(3) Uani 1 1 d . . . H6 H 0.7304 0.7271 0.4696 0.018 Uiso 1 1 calc R . . C7 C 0.61750(8) 0.71406(13) 0.46018(8) 0.0177(3) Uani 1 1 d . . . H7 H 0.6130 0.8101 0.4692 0.021 Uiso 1 1 calc R . . C8 C 0.55164(8) 0.62350(13) 0.44799(8) 0.0178(3) Uani 1 1 d . . . H8 H 0.5044 0.6601 0.4497 0.021 Uiso 1 1 calc R . . C9 C 0.55538(8) 0.48539(13) 0.43394(7) 0.0149(3) Uani 1 1 d . . . H9 H 0.5118 0.4259 0.4278 0.018 Uiso 1 1 calc R . . C10 C 0.82066(8) 0.50836(13) 0.41144(8) 0.0161(3) Uani 1 1 d . . . C11 C 0.88587(8) 0.58116(14) 0.49014(8) 0.0205(3) Uani 1 1 d . . . H11A H 0.8595 0.6490 0.5110 0.025 Uiso 1 1 calc R . . H11B H 0.9248 0.6287 0.4754 0.025 Uiso 1 1 calc R . . H11C H 0.9149 0.5122 0.5343 0.025 Uiso 1 1 calc R . . C12 C 0.86173(8) 0.39803(15) 0.38141(9) 0.0219(3) Uani 1 1 d . . . H12A H 0.8818 0.3225 0.4228 0.026 Uiso 1 1 calc R . . H12B H 0.9077 0.4397 0.3757 0.026 Uiso 1 1 calc R . . H12C H 0.8220 0.3614 0.3266 0.026 Uiso 1 1 calc R . . C13 C 0.78256(9) 0.61580(14) 0.33953(8) 0.0225(3) Uani 1 1 d . . . H13A H 0.7397 0.5713 0.2894 0.027 Uiso 1 1 calc R . . H13B H 0.8250 0.6523 0.3258 0.027 Uiso 1 1 calc R . . H13C H 0.7589 0.6920 0.3577 0.027 Uiso 1 1 calc R . . C14 C 0.58281(8) 0.17568(13) 0.36775(7) 0.0140(3) Uani 1 1 d . . . C15 C 0.51915(8) 0.21455(14) 0.27762(8) 0.0224(3) Uani 1 1 d . . . H15A H 0.4904 0.2991 0.2796 0.027 Uiso 1 1 calc R . . H15B H 0.4797 0.1387 0.2536 0.027 Uiso 1 1 calc R . . H15C H 0.5468 0.2305 0.2423 0.027 Uiso 1 1 calc R . . C16 C 0.62825(8) 0.04536(13) 0.36314(8) 0.0196(3) Uani 1 1 d . . . H16A H 0.6533 0.0624 0.3256 0.024 Uiso 1 1 calc R . . H16B H 0.5896 -0.0320 0.3411 0.024 Uiso 1 1 calc R . . H16C H 0.6709 0.0222 0.4198 0.024 Uiso 1 1 calc R . . C17 C 0.53769(8) 0.14431(13) 0.42084(8) 0.0179(3) Uani 1 1 d . . . H17A H 0.5761 0.1515 0.4811 0.022 Uiso 1 1 calc R . . H17B H 0.5151 0.0503 0.4083 0.022 Uiso 1 1 calc R . . H17C H 0.4932 0.2112 0.4069 0.022 Uiso 1 1 calc R . . C18 C 0.83554(7) 0.21749(12) 0.60328(7) 0.0121(3) Uani 1 1 d . . . C19 C 0.84626(8) 0.35827(13) 0.63152(7) 0.0125(3) Uani 1 1 d . . . H19 H 0.8912(8) 0.4175(13) 0.6388(7) 0.010(3) Uiso 1 1 d . . . C20 C 0.78129(7) 0.40227(12) 0.64855(7) 0.0112(3) Uani 1 1 d . . . C21 C 0.72979(7) 0.28200(12) 0.63556(7) 0.0106(2) Uani 1 1 d . . . C22 C 0.76289(7) 0.16934(12) 0.60690(7) 0.0113(2) Uani 1 1 d . . . C23 C 0.72750(8) 0.03413(12) 0.59781(7) 0.0134(3) Uani 1 1 d . . . H23 H 0.7467 -0.0403 0.5766 0.016 Uiso 1 1 calc R . . C24 C 0.66651(8) 0.01257(13) 0.61961(8) 0.0155(3) Uani 1 1 d . . . H24 H 0.6449 -0.0781 0.6157 0.019 Uiso 1 1 calc R . . C25 C 0.63432(8) 0.12372(13) 0.64835(8) 0.0158(3) Uani 1 1 d . . . H25 H 0.5918 0.1057 0.6635 0.019 Uiso 1 1 calc R . . C26 C 0.66335(7) 0.25493(13) 0.65442(7) 0.0134(3) Uani 1 1 d . . . H26 H 0.6395 0.3285 0.6712 0.016 Uiso 1 1 calc R . . C27 C 0.90126(8) 0.12593(13) 0.59867(8) 0.0162(3) Uani 1 1 d . . . C28 C 0.97352(8) 0.21368(14) 0.60510(9) 0.0212(3) Uani 1 1 d . . . H28A H 0.9541 0.2822 0.5593 0.025 Uiso 1 1 calc R . . H28B H 1.0142 0.1534 0.6003 0.025 Uiso 1 1 calc R . . H28C H 0.9984 0.2616 0.6597 0.025 Uiso 1 1 calc R . . C29 C 0.86993(8) 0.03863(14) 0.51769(8) 0.0220(3) Uani 1 1 d . . . H29A H 0.8225 -0.0158 0.5117 0.026 Uiso 1 1 calc R . . H29B H 0.9133 -0.0241 0.5210 0.026 Uiso 1 1 calc R . . H29C H 0.8540 0.1000 0.4687 0.026 Uiso 1 1 calc R . . C30 C 0.93301(8) 0.02855(14) 0.67619(8) 0.0213(3) Uani 1 1 d . . . H30A H 0.9524 0.0840 0.7280 0.026 Uiso 1 1 calc R . . H30B H 0.9781 -0.0277 0.6776 0.026 Uiso 1 1 calc R . . H30C H 0.8886 -0.0324 0.6721 0.026 Uiso 1 1 calc R . . C31 C 0.78107(8) 0.53475(12) 0.69502(7) 0.0127(3) Uani 1 1 d . . . C32 C 0.82098(8) 0.49762(13) 0.79002(7) 0.0167(3) Uani 1 1 d . . . H32A H 0.7892 0.4244 0.7998 0.020 Uiso 1 1 calc R . . H32B H 0.8222 0.5800 0.8229 0.020 Uiso 1 1 calc R . . H32C H 0.8769 0.4649 0.8077 0.020 Uiso 1 1 calc R . . C33 C 0.83183(8) 0.64765(13) 0.67985(8) 0.0168(3) Uani 1 1 d . . . H33A H 0.8880 0.6146 0.6992 0.020 Uiso 1 1 calc R . . H33B H 0.8322 0.7314 0.7113 0.020 Uiso 1 1 calc R . . H33C H 0.8077 0.6691 0.6193 0.020 Uiso 1 1 calc R . . C34 C 0.69509(8) 0.59252(13) 0.66950(8) 0.0165(3) Uani 1 1 d . . . H34A H 0.6638 0.5928 0.6077 0.020 Uiso 1 1 calc R . . H34B H 0.6994 0.6874 0.6909 0.020 Uiso 1 1 calc R . . H34C H 0.6672 0.5342 0.6936 0.020 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 Fe 0.01025(9) 0.00969(9) 0.00848(9) 0.00022(7) 0.00436(7) -0.00091(7) C1 0.0142(7) 0.0141(6) 0.0084(6) 0.0023(5) 0.0050(5) -0.0013(5) C2 0.0158(7) 0.0135(6) 0.0090(6) 0.0002(5) 0.0061(5) -0.0002(5) C3 0.0140(7) 0.0130(6) 0.0072(6) 0.0009(5) 0.0039(5) -0.0008(5) C4 0.0129(7) 0.0132(6) 0.0084(6) 0.0024(5) 0.0039(5) 0.0001(5) C5 0.0146(6) 0.0126(6) 0.0082(6) 0.0016(5) 0.0044(5) -0.0012(5) C6 0.0211(7) 0.0131(6) 0.0096(6) 0.0008(5) 0.0055(5) -0.0030(6) C7 0.0269(8) 0.0132(6) 0.0117(6) 0.0016(5) 0.0075(6) 0.0040(6) C8 0.0177(7) 0.0228(7) 0.0120(6) 0.0033(5) 0.0062(6) 0.0080(5) C9 0.0131(7) 0.0196(7) 0.0111(6) 0.0025(5) 0.0047(5) 0.0005(5) C10 0.0176(7) 0.0183(7) 0.0150(6) 0.0002(5) 0.0096(6) -0.0056(5) C11 0.0190(7) 0.0247(7) 0.0198(7) 0.0002(6) 0.0106(6) -0.0084(6) C12 0.0213(8) 0.0266(7) 0.0247(7) -0.0002(6) 0.0165(6) -0.0040(6) C13 0.0292(8) 0.0228(7) 0.0183(7) 0.0028(6) 0.0132(6) -0.0072(6) C14 0.0143(7) 0.0151(6) 0.0108(6) -0.0014(5) 0.0043(5) -0.0042(5) C15 0.0217(8) 0.0264(7) 0.0136(7) -0.0011(6) 0.0033(6) -0.0078(6) C16 0.0243(8) 0.0149(7) 0.0206(7) -0.0043(5) 0.0108(6) -0.0062(6) C17 0.0171(7) 0.0194(7) 0.0172(7) 0.0002(5) 0.0075(6) -0.0061(6) C18 0.0119(6) 0.0133(6) 0.0098(6) 0.0024(5) 0.0040(5) 0.0008(5) C19 0.0102(6) 0.0154(6) 0.0098(6) 0.0011(5) 0.0027(5) -0.0021(5) C20 0.0124(6) 0.0120(6) 0.0076(6) 0.0010(5) 0.0033(5) -0.0010(5) C21 0.0121(6) 0.0113(6) 0.0068(6) 0.0007(5) 0.0028(5) 0.0001(5) C22 0.0123(6) 0.0131(6) 0.0077(5) 0.0017(5) 0.0037(5) 0.0007(5) C23 0.0162(7) 0.0117(6) 0.0115(6) 0.0002(5) 0.0055(5) 0.0003(5) C24 0.0183(7) 0.0132(6) 0.0132(6) 0.0006(5) 0.0056(5) -0.0038(5) C25 0.0154(7) 0.0196(7) 0.0141(6) -0.0006(5) 0.0082(6) -0.0040(5) C26 0.0138(7) 0.0163(6) 0.0106(6) -0.0012(5) 0.0059(5) 0.0004(5) C27 0.0133(7) 0.0180(7) 0.0181(7) 0.0027(5) 0.0079(6) 0.0032(5) C28 0.0150(7) 0.0251(7) 0.0259(8) 0.0067(6) 0.0114(6) 0.0058(6) C29 0.0219(8) 0.0221(7) 0.0258(8) -0.0012(6) 0.0140(6) 0.0060(6) C30 0.0160(7) 0.0213(7) 0.0262(7) 0.0074(6) 0.0092(6) 0.0058(6) C31 0.0156(7) 0.0128(6) 0.0090(6) -0.0014(5) 0.0049(5) -0.0019(5) C32 0.0218(7) 0.0148(6) 0.0114(6) -0.0017(5) 0.0058(6) -0.0015(5) C33 0.0225(7) 0.0132(6) 0.0142(6) -0.0023(5) 0.0080(6) -0.0035(6) C34 0.0213(7) 0.0134(6) 0.0145(6) -0.0007(5) 0.0080(6) 0.0004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C19 2.0631(12) . ? Fe C2 2.0679(12) . ? Fe C20 2.0850(12) . ? Fe C3 2.0912(12) . ? Fe C1 2.1025(12) . ? Fe C18 2.1053(12) . ? Fe C5 2.1466(12) . ? Fe C4 2.1477(12) . ? Fe C22 2.1545(12) . ? Fe C21 2.1563(12) . ? C1 C2 1.4293(17) . ? C1 C5 1.4423(17) . ? C1 C10 1.5246(17) . ? C2 C3 1.4197(18) . ? C3 C4 1.4467(17) . ? C3 C14 1.5229(17) . ? C4 C9 1.4285(17) . ? C4 C5 1.4474(17) . ? C5 C6 1.4356(16) . ? C6 C7 1.3547(18) . ? C7 C8 1.4260(19) . ? C8 C9 1.3624(18) . ? C10 C12 1.5323(18) . ? C10 C11 1.5362(17) . ? C10 C13 1.5431(18) . ? C14 C16 1.5308(17) . ? C14 C15 1.5391(17) . ? C14 C17 1.5397(17) . ? C18 C19 1.4296(17) . ? C18 C22 1.4405(17) . ? C18 C27 1.5266(17) . ? C19 C20 1.4211(17) . ? C20 C21 1.4471(17) . ? C20 C31 1.5214(16) . ? C21 C26 1.4272(17) . ? C21 C22 1.4448(16) . ? C22 C23 1.4328(16) . ? C23 C24 1.3556(18) . ? C24 C25 1.4250(18) . ? C25 C26 1.3582(17) . ? C27 C28 1.5333(18) . ? C27 C29 1.5343(18) . ? C27 C30 1.5448(17) . ? C31 C33 1.5339(17) . ? C31 C34 1.5355(17) . ? C31 C32 1.5447(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Fe C2 129.41(5) . . ? C19 Fe C20 40.06(5) . . ? C2 Fe C20 166.49(5) . . ? C19 Fe C3 166.83(5) . . ? C2 Fe C3 39.91(5) . . ? C20 Fe C3 151.98(5) . . ? C19 Fe C1 108.09(5) . . ? C2 Fe C1 40.07(5) . . ? C20 Fe C1 128.32(5) . . ? C3 Fe C1 68.24(5) . . ? C19 Fe C18 40.10(5) . . ? C2 Fe C18 108.67(5) . . ? C20 Fe C18 68.32(5) . . ? C3 Fe C18 129.03(5) . . ? C1 Fe C18 116.48(5) . . ? C19 Fe C5 118.85(5) . . ? C2 Fe C5 65.80(5) . . ? C20 Fe C5 109.75(5) . . ? C3 Fe C5 67.02(5) . . ? C1 Fe C5 39.67(5) . . ? C18 Fe C5 150.02(5) . . ? C19 Fe C4 151.71(5) . . ? C2 Fe C4 65.88(5) . . ? C20 Fe C4 119.58(5) . . ? C3 Fe C4 39.88(5) . . ? C1 Fe C4 67.02(5) . . ? C18 Fe C4 167.89(5) . . ? C5 Fe C4 39.39(4) . . ? C19 Fe C22 65.74(5) . . ? C2 Fe C22 119.69(5) . . ? C20 Fe C22 67.01(4) . . ? C3 Fe C22 110.73(5) . . ? C1 Fe C22 150.30(5) . . ? C18 Fe C22 39.51(5) . . ? C5 Fe C22 169.44(5) . . ? C4 Fe C22 132.39(5) . . ? C19 Fe C21 65.76(5) . . ? C2 Fe C21 152.37(5) . . ? C20 Fe C21 39.86(4) . . ? C3 Fe C21 120.31(5) . . ? C1 Fe C21 167.32(5) . . ? C18 Fe C21 66.68(5) . . ? C5 Fe C21 132.07(5) . . ? C4 Fe C21 112.67(5) . . ? C22 Fe C21 39.16(4) . . ? C2 C1 C5 105.80(11) . . ? C2 C1 C10 125.66(11) . . ? C5 C1 C10 126.17(11) . . ? C2 C1 Fe 68.66(7) . . ? C5 C1 Fe 71.81(7) . . ? C10 C1 Fe 137.54(9) . . ? C3 C2 C1 111.32(11) . . ? C3 C2 Fe 70.92(7) . . ? C1 C2 Fe 71.26(7) . . ? C2 C3 C4 106.28(10) . . ? C2 C3 C14 125.54(11) . . ? C4 C3 C14 126.70(11) . . ? C2 C3 Fe 69.16(7) . . ? C4 C3 Fe 72.16(7) . . ? C14 C3 Fe 134.15(8) . . ? C9 C4 C3 132.63(11) . . ? C9 C4 C5 119.18(11) . . ? C3 C4 C5 107.91(10) . . ? C9 C4 Fe 131.83(8) . . ? C3 C4 Fe 67.95(7) . . ? C5 C4 Fe 70.26(7) . . ? C6 C5 C1 132.23(11) . . ? C6 C5 C4 118.70(11) . . ? C1 C5 C4 108.60(10) . . ? C6 C5 Fe 132.85(8) . . ? C1 C5 Fe 68.52(6) . . ? C4 C5 Fe 70.35(7) . . ? C7 C6 C5 119.91(12) . . ? C6 C7 C8 121.28(12) . . ? C9 C8 C7 121.13(13) . . ? C8 C9 C4 119.72(12) . . ? C1 C10 C12 111.08(10) . . ? C1 C10 C11 113.48(10) . . ? C12 C10 C11 109.26(11) . . ? C1 C10 C13 107.38(11) . . ? C12 C10 C13 106.78(11) . . ? C11 C10 C13 108.60(10) . . ? C3 C14 C16 110.23(10) . . ? C3 C14 C15 107.92(10) . . ? C16 C14 C15 108.66(10) . . ? C3 C14 C17 112.26(10) . . ? C16 C14 C17 109.17(10) . . ? C15 C14 C17 108.52(11) . . ? C19 C18 C22 105.88(11) . . ? C19 C18 C27 125.56(11) . . ? C22 C18 C27 125.85(11) . . ? C19 C18 Fe 68.36(7) . . ? C22 C18 Fe 72.09(7) . . ? C27 C18 Fe 138.55(9) . . ? C20 C19 C18 111.26(11) . . ? C20 C19 Fe 70.80(7) . . ? C18 C19 Fe 71.54(7) . . ? C19 C20 C21 106.09(10) . . ? C19 C20 C31 125.05(11) . . ? C21 C20 C31 126.69(11) . . ? C19 C20 Fe 69.14(7) . . ? C21 C20 Fe 72.73(7) . . ? C31 C20 Fe 135.75(8) . . ? C26 C21 C22 119.02(11) . . ? C26 C21 C20 132.45(11) . . ? C22 C21 C20 108.09(10) . . ? C26 C21 Fe 133.68(9) . . ? C22 C21 Fe 70.35(7) . . ? C20 C21 Fe 67.42(6) . . ? C23 C22 C18 132.05(11) . . ? C23 C22 C21 118.85(11) . . ? C18 C22 C21 108.57(10) . . ? C23 C22 Fe 133.27(9) . . ? C18 C22 Fe 68.40(7) . . ? C21 C22 Fe 70.49(6) . . ? C24 C23 C22 119.88(11) . . ? C23 C24 C25 121.09(12) . . ? C26 C25 C24 121.19(12) . . ? C25 C26 C21 119.86(12) . . ? C18 C27 C28 110.77(10) . . ? C18 C27 C29 113.42(11) . . ? C28 C27 C29 108.49(11) . . ? C18 C27 C30 107.00(10) . . ? C28 C27 C30 107.74(10) . . ? C29 C27 C30 109.27(11) . . ? C20 C31 C33 110.49(10) . . ? C20 C31 C34 113.55(10) . . ? C33 C31 C34 108.38(10) . . ? C20 C31 C32 106.27(10) . . ? C33 C31 C32 109.30(10) . . ? C34 C31 C32 108.76(10) . . ? 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 C19 Fe C1 C2 130.48(8) . . . . ? C20 Fe C1 C2 170.30(7) . . . . ? C3 Fe C1 C2 -36.06(7) . . . . ? C18 Fe C1 C2 87.90(8) . . . . ? C5 Fe C1 C2 -115.85(10) . . . . ? C4 Fe C1 C2 -79.32(8) . . . . ? C22 Fe C1 C2 57.92(12) . . . . ? C21 Fe C1 C2 -170.59(19) . . . . ? C19 Fe C1 C5 -113.67(7) . . . . ? C2 Fe C1 C5 115.85(10) . . . . ? C20 Fe C1 C5 -73.85(9) . . . . ? C3 Fe C1 C5 79.79(7) . . . . ? C18 Fe C1 C5 -156.25(7) . . . . ? C4 Fe C1 C5 36.53(7) . . . . ? C22 Fe C1 C5 173.77(8) . . . . ? C21 Fe C1 C5 -54.7(2) . . . . ? C19 Fe C1 C10 10.47(14) . . . . ? C2 Fe C1 C10 -120.02(16) . . . . ? C20 Fe C1 C10 50.28(15) . . . . ? C3 Fe C1 C10 -156.07(14) . . . . ? C18 Fe C1 C10 -32.11(14) . . . . ? C5 Fe C1 C10 124.13(16) . . . . ? C4 Fe C1 C10 160.66(14) . . . . ? C22 Fe C1 C10 -62.09(17) . . . . ? C21 Fe C1 C10 69.4(3) . . . . ? C5 C1 C2 C3 -2.88(14) . . . . ? C10 C1 C2 C3 -166.19(11) . . . . ? Fe C1 C2 C3 59.81(9) . . . . ? C5 C1 C2 Fe -62.69(8) . . . . ? C10 C1 C2 Fe 133.99(12) . . . . ? C19 Fe C2 C3 169.07(7) . . . . ? C20 Fe C2 C3 -156.03(19) . . . . ? C1 Fe C2 C3 -121.57(10) . . . . ? C18 Fe C2 C3 129.19(7) . . . . ? C5 Fe C2 C3 -82.53(8) . . . . ? C4 Fe C2 C3 -39.18(7) . . . . ? C22 Fe C2 C3 87.33(8) . . . . ? C21 Fe C2 C3 53.99(13) . . . . ? C19 Fe C2 C1 -69.36(9) . . . . ? C20 Fe C2 C1 -34.5(2) . . . . ? C3 Fe C2 C1 121.57(10) . . . . ? C18 Fe C2 C1 -109.24(8) . . . . ? C5 Fe C2 C1 39.03(7) . . . . ? C4 Fe C2 C1 82.39(8) . . . . ? C22 Fe C2 C1 -151.10(7) . . . . ? C21 Fe C2 C1 175.56(9) . . . . ? C1 C2 C3 C4 3.08(14) . . . . ? Fe C2 C3 C4 63.09(8) . . . . ? C1 C2 C3 C14 169.89(11) . . . . ? Fe C2 C3 C14 -130.09(12) . . . . ? C1 C2 C3 Fe -60.01(9) . . . . ? C19 Fe C3 C2 -40.0(2) . . . . ? C20 Fe C3 C2 168.35(9) . . . . ? C1 Fe C3 C2 36.20(7) . . . . ? C18 Fe C3 C2 -70.93(9) . . . . ? C5 Fe C3 C2 79.23(8) . . . . ? C4 Fe C3 C2 115.95(10) . . . . ? C22 Fe C3 C2 -111.89(7) . . . . ? C21 Fe C3 C2 -154.25(7) . . . . ? C19 Fe C3 C4 -155.9(2) . . . . ? C2 Fe C3 C4 -115.95(10) . . . . ? C20 Fe C3 C4 52.40(12) . . . . ? C1 Fe C3 C4 -79.75(7) . . . . ? C18 Fe C3 C4 173.12(7) . . . . ? C5 Fe C3 C4 -36.72(7) . . . . ? C22 Fe C3 C4 132.16(7) . . . . ? C21 Fe C3 C4 89.81(8) . . . . ? C19 Fe C3 C14 79.8(3) . . . . ? C2 Fe C3 C14 119.82(15) . . . . ? C20 Fe C3 C14 -71.83(16) . . . . ? C1 Fe C3 C14 156.02(14) . . . . ? C18 Fe C3 C14 48.89(14) . . . . ? C5 Fe C3 C14 -160.95(14) . . . . ? C4 Fe C3 C14 -124.23(15) . . . . ? C22 Fe C3 C14 7.93(14) . . . . ? C21 Fe C3 C14 -34.42(14) . . . . ? C2 C3 C4 C9 171.66(12) . . . . ? C14 C3 C4 C9 5.0(2) . . . . ? Fe C3 C4 C9 -127.24(13) . . . . ? C2 C3 C4 C5 -2.02(13) . . . . ? C14 C3 C4 C5 -168.64(11) . . . . ? Fe C3 C4 C5 59.08(8) . . . . ? C2 C3 C4 Fe -61.10(8) . . . . ? C14 C3 C4 Fe 132.28(12) . . . . ? C19 Fe C4 C9 -63.13(17) . . . . ? C2 Fe C4 C9 167.38(13) . . . . ? C20 Fe C4 C9 -26.48(14) . . . . ? C3 Fe C4 C9 128.18(15) . . . . ? C1 Fe C4 C9 -148.74(13) . . . . ? C18 Fe C4 C9 101.9(2) . . . . ? C5 Fe C4 C9 -111.97(14) . . . . ? C22 Fe C4 C9 58.35(14) . . . . ? C21 Fe C4 C9 17.50(13) . . . . ? C19 Fe C4 C3 168.69(9) . . . . ? C2 Fe C4 C3 39.21(7) . . . . ? C20 Fe C4 C3 -154.66(7) . . . . ? C1 Fe C4 C3 83.08(7) . . . . ? C18 Fe C4 C3 -26.3(2) . . . . ? C5 Fe C4 C3 119.86(10) . . . . ? C22 Fe C4 C3 -69.82(9) . . . . ? C21 Fe C4 C3 -110.68(7) . . . . ? C19 Fe C4 C5 48.84(13) . . . . ? C2 Fe C4 C5 -80.65(7) . . . . ? C20 Fe C4 C5 85.48(8) . . . . ? C3 Fe C4 C5 -119.86(10) . . . . ? C1 Fe C4 C5 -36.77(7) . . . . ? C18 Fe C4 C5 -146.2(2) . . . . ? C22 Fe C4 C5 170.32(7) . . . . ? C21 Fe C4 C5 129.47(7) . . . . ? C2 C1 C5 C6 -170.37(12) . . . . ? C10 C1 C5 C6 -7.2(2) . . . . ? Fe C1 C5 C6 129.03(13) . . . . ? C2 C1 C5 C4 1.51(13) . . . . ? C10 C1 C5 C4 164.72(11) . . . . ? Fe C1 C5 C4 -59.08(8) . . . . ? C2 C1 C5 Fe 60.59(8) . . . . ? C10 C1 C5 Fe -136.20(12) . . . . ? C9 C4 C5 C6 -1.21(16) . . . . ? C3 C4 C5 C6 173.47(10) . . . . ? Fe C4 C5 C6 -128.88(10) . . . . ? C9 C4 C5 C1 -174.37(10) . . . . ? C3 C4 C5 C1 0.31(13) . . . . ? Fe C4 C5 C1 57.96(8) . . . . ? C9 C4 C5 Fe 127.67(11) . . . . ? C3 C4 C5 Fe -57.65(8) . . . . ? C19 Fe C5 C6 -44.60(14) . . . . ? C2 Fe C5 C6 -167.76(14) . . . . ? C20 Fe C5 C6 -1.53(14) . . . . ? C3 Fe C5 C6 148.53(14) . . . . ? C1 Fe C5 C6 -128.33(16) . . . . ? C18 Fe C5 C6 -82.15(16) . . . . ? C4 Fe C5 C6 111.37(15) . . . . ? C22 Fe C5 C6 68.7(3) . . . . ? C21 Fe C5 C6 37.69(15) . . . . ? C19 Fe C5 C1 83.74(8) . . . . ? C2 Fe C5 C1 -39.43(7) . . . . ? C20 Fe C5 C1 126.80(7) . . . . ? C3 Fe C5 C1 -83.14(7) . . . . ? C18 Fe C5 C1 46.18(12) . . . . ? C4 Fe C5 C1 -120.30(10) . . . . ? C22 Fe C5 C1 -163.0(2) . . . . ? C21 Fe C5 C1 166.03(7) . . . . ? C19 Fe C5 C4 -155.96(7) . . . . ? C2 Fe C5 C4 80.87(8) . . . . ? C20 Fe C5 C4 -112.90(7) . . . . ? C3 Fe C5 C4 37.16(7) . . . . ? C1 Fe C5 C4 120.30(10) . . . . ? C18 Fe C5 C4 166.48(9) . . . . ? C22 Fe C5 C4 -42.7(3) . . . . ? C21 Fe C5 C4 -73.67(9) . . . . ? C1 C5 C6 C7 169.75(12) . . . . ? C4 C5 C6 C7 -1.48(17) . . . . ? Fe C5 C6 C7 -90.61(15) . . . . ? C5 C6 C7 C8 2.47(18) . . . . ? C6 C7 C8 C9 -0.71(19) . . . . ? C7 C8 C9 C4 -2.04(18) . . . . ? C3 C4 C9 C8 -170.17(12) . . . . ? C5 C4 C9 C8 2.94(17) . . . . ? Fe C4 C9 C8 91.83(14) . . . . ? C2 C1 C10 C12 -11.11(17) . . . . ? C5 C1 C10 C12 -171.10(11) . . . . ? Fe C1 C10 C12 85.83(14) . . . . ? C2 C1 C10 C11 -134.67(13) . . . . ? C5 C1 C10 C11 65.34(16) . . . . ? Fe C1 C10 C11 -37.73(18) . . . . ? C2 C1 C10 C13 105.31(14) . . . . ? C5 C1 C10 C13 -54.68(15) . . . . ? Fe C1 C10 C13 -157.75(11) . . . . ? C2 C3 C14 C16 25.36(16) . . . . ? C4 C3 C14 C16 -170.49(11) . . . . ? Fe C3 C14 C16 -69.47(15) . . . . ? C2 C3 C14 C15 -93.16(14) . . . . ? C4 C3 C14 C15 70.99(15) . . . . ? Fe C3 C14 C15 172.00(10) . . . . ? C2 C3 C14 C17 147.29(12) . . . . ? C4 C3 C14 C17 -48.56(16) . . . . ? Fe C3 C14 C17 52.46(16) . . . . ? C2 Fe C18 C19 129.72(7) . . . . ? C20 Fe C18 C19 -36.24(7) . . . . ? C3 Fe C18 C19 169.52(7) . . . . ? C1 Fe C18 C19 86.95(8) . . . . ? C5 Fe C18 C19 55.98(12) . . . . ? C4 Fe C18 C19 -169.0(2) . . . . ? C22 Fe C18 C19 -115.95(10) . . . . ? C21 Fe C18 C19 -79.50(8) . . . . ? C19 Fe C18 C22 115.95(10) . . . . ? C2 Fe C18 C22 -114.32(7) . . . . ? C20 Fe C18 C22 79.71(7) . . . . ? C3 Fe C18 C22 -74.53(9) . . . . ? C1 Fe C18 C22 -157.10(7) . . . . ? C5 Fe C18 C22 171.94(8) . . . . ? C4 Fe C18 C22 -53.1(2) . . . . ? C21 Fe C18 C22 36.45(7) . . . . ? C19 Fe C18 C27 -119.73(16) . . . . ? C2 Fe C18 C27 9.99(14) . . . . ? C20 Fe C18 C27 -155.97(15) . . . . ? C3 Fe C18 C27 49.79(15) . . . . ? C1 Fe C18 C27 -32.78(15) . . . . ? C5 Fe C18 C27 -63.75(17) . . . . ? C4 Fe C18 C27 71.3(3) . . . . ? C22 Fe C18 C27 124.32(16) . . . . ? C21 Fe C18 C27 160.77(14) . . . . ? C22 C18 C19 C20 -2.95(13) . . . . ? C27 C18 C19 C20 -165.08(11) . . . . ? Fe C18 C19 C20 59.87(8) . . . . ? C22 C18 C19 Fe -62.81(8) . . . . ? C27 C18 C19 Fe 135.05(12) . . . . ? C2 Fe C19 C20 168.02(7) . . . . ? C3 Fe C19 C20 -159.73(19) . . . . ? C1 Fe C19 C20 128.69(7) . . . . ? C18 Fe C19 C20 -121.41(10) . . . . ? C5 Fe C19 C20 86.81(8) . . . . ? C4 Fe C19 C20 53.75(13) . . . . ? C22 Fe C19 C20 -82.54(7) . . . . ? C21 Fe C19 C20 -39.41(7) . . . . ? C2 Fe C19 C18 -70.58(9) . . . . ? C20 Fe C19 C18 121.41(10) . . . . ? C3 Fe C19 C18 -38.3(2) . . . . ? C1 Fe C19 C18 -109.90(7) . . . . ? C5 Fe C19 C18 -151.78(7) . . . . ? C4 Fe C19 C18 175.16(9) . . . . ? C22 Fe C19 C18 38.86(7) . . . . ? C21 Fe C19 C18 82.00(8) . . . . ? C18 C19 C20 C21 3.55(13) . . . . ? Fe C19 C20 C21 63.86(8) . . . . ? C18 C19 C20 C31 167.70(11) . . . . ? Fe C19 C20 C31 -131.99(11) . . . . ? C18 C19 C20 Fe -60.31(8) . . . . ? C2 Fe C20 C19 -43.4(2) . . . . ? C3 Fe C20 C19 170.33(9) . . . . ? C1 Fe C20 C19 -71.04(9) . . . . ? C18 Fe C20 C19 36.27(7) . . . . ? C5 Fe C20 C19 -111.69(7) . . . . ? C4 Fe C20 C19 -153.93(7) . . . . ? C22 Fe C20 C19 79.11(8) . . . . ? C21 Fe C20 C19 115.40(10) . . . . ? C19 Fe C20 C21 -115.40(10) . . . . ? C2 Fe C20 C21 -158.77(19) . . . . ? C3 Fe C20 C21 54.92(13) . . . . ? C1 Fe C20 C21 173.56(7) . . . . ? C18 Fe C20 C21 -79.13(7) . . . . ? C5 Fe C20 C21 132.91(7) . . . . ? C4 Fe C20 C21 90.67(8) . . . . ? C22 Fe C20 C21 -36.29(7) . . . . ? C19 Fe C20 C31 119.32(15) . . . . ? C2 Fe C20 C31 75.9(3) . . . . ? C3 Fe C20 C31 -70.36(16) . . . . ? C1 Fe C20 C31 48.28(15) . . . . ? C18 Fe C20 C31 155.58(14) . . . . ? C5 Fe C20 C31 7.63(14) . . . . ? C4 Fe C20 C31 -34.62(14) . . . . ? C22 Fe C20 C31 -161.57(14) . . . . ? C21 Fe C20 C31 -125.28(15) . . . . ? C19 C20 C21 C26 169.25(12) . . . . ? C31 C20 C21 C26 5.4(2) . . . . ? Fe C20 C21 C26 -129.29(13) . . . . ? C19 C20 C21 C22 -2.73(13) . . . . ? C31 C20 C21 C22 -166.54(11) . . . . ? Fe C20 C21 C22 58.73(8) . . . . ? C19 C20 C21 Fe -61.46(8) . . . . ? C31 C20 C21 Fe 134.73(12) . . . . ? C19 Fe C21 C26 167.46(13) . . . . ? C2 Fe C21 C26 -62.67(17) . . . . ? C20 Fe C21 C26 127.84(15) . . . . ? C3 Fe C21 C26 -25.71(14) . . . . ? C1 Fe C21 C26 104.2(2) . . . . ? C18 Fe C21 C26 -148.55(13) . . . . ? C5 Fe C21 C26 59.61(14) . . . . ? C4 Fe C21 C26 18.31(13) . . . . ? C22 Fe C21 C26 -111.79(14) . . . . ? C19 Fe C21 C22 -80.76(7) . . . . ? C2 Fe C21 C22 49.12(13) . . . . ? C20 Fe C21 C22 -120.37(10) . . . . ? C3 Fe C21 C22 86.08(8) . . . . ? C1 Fe C21 C22 -144.0(2) . . . . ? C18 Fe C21 C22 -36.76(7) . . . . ? C5 Fe C21 C22 171.40(7) . . . . ? C4 Fe C21 C22 130.09(7) . . . . ? C19 Fe C21 C20 39.62(7) . . . . ? C2 Fe C21 C20 169.49(10) . . . . ? C3 Fe C21 C20 -153.55(7) . . . . ? C1 Fe C21 C20 -23.6(2) . . . . ? C18 Fe C21 C20 83.61(7) . . . . ? C5 Fe C21 C20 -68.23(9) . . . . ? C4 Fe C21 C20 -109.54(7) . . . . ? C22 Fe C21 C20 120.37(10) . . . . ? C19 C18 C22 C23 -170.19(12) . . . . ? C27 C18 C22 C23 -8.1(2) . . . . ? Fe C18 C22 C23 129.47(13) . . . . ? C19 C18 C22 C21 1.13(13) . . . . ? C27 C18 C22 C21 163.20(11) . . . . ? Fe C18 C22 C21 -59.21(8) . . . . ? C19 C18 C22 Fe 60.34(8) . . . . ? C27 C18 C22 Fe -137.59(12) . . . . ? C26 C21 C22 C23 0.41(16) . . . . ? C20 C21 C22 C23 173.65(10) . . . . ? Fe C21 C22 C23 -129.42(11) . . . . ? C26 C21 C22 C18 -172.24(10) . . . . ? C20 C21 C22 C18 1.00(13) . . . . ? Fe C21 C22 C18 57.93(8) . . . . ? C26 C21 C22 Fe 129.83(11) . . . . ? C20 C21 C22 Fe -56.93(8) . . . . ? C19 Fe C22 C23 -167.52(14) . . . . ? C2 Fe C22 C23 -44.52(14) . . . . ? C20 Fe C22 C23 148.60(13) . . . . ? C3 Fe C22 C23 -1.26(13) . . . . ? C1 Fe C22 C23 -83.41(15) . . . . ? C18 Fe C22 C23 -128.08(15) . . . . ? C5 Fe C22 C23 74.4(3) . . . . ? C4 Fe C22 C23 38.80(15) . . . . ? C21 Fe C22 C23 111.68(15) . . . . ? C19 Fe C22 C18 -39.44(7) . . . . ? C2 Fe C22 C18 83.56(8) . . . . ? C20 Fe C22 C18 -83.33(7) . . . . ? C3 Fe C22 C18 126.82(7) . . . . ? C1 Fe C22 C18 44.67(12) . . . . ? C5 Fe C22 C18 -157.5(2) . . . . ? C4 Fe C22 C18 166.88(7) . . . . ? C21 Fe C22 C18 -120.24(10) . . . . ? C19 Fe C22 C21 80.80(7) . . . . ? C2 Fe C22 C21 -156.20(7) . . . . ? C20 Fe C22 C21 36.91(7) . . . . ? C3 Fe C22 C21 -112.94(7) . . . . ? C1 Fe C22 C21 164.91(9) . . . . ? C18 Fe C22 C21 120.24(10) . . . . ? C5 Fe C22 C21 -37.3(3) . . . . ? C4 Fe C22 C21 -72.88(9) . . . . ? C18 C22 C23 C24 167.67(12) . . . . ? C21 C22 C23 C24 -2.93(17) . . . . ? Fe C22 C23 C24 -92.63(14) . . . . ? C22 C23 C24 C25 2.62(18) . . . . ? C23 C24 C25 C26 0.34(19) . . . . ? C24 C25 C26 C21 -2.91(18) . . . . ? C22 C21 C26 C25 2.47(17) . . . . ? C20 C21 C26 C25 -168.80(12) . . . . ? Fe C21 C26 C25 92.35(15) . . . . ? C19 C18 C27 C28 -15.39(17) . . . . ? C22 C18 C27 C28 -174.05(11) . . . . ? Fe C18 C27 C28 81.77(15) . . . . ? C19 C18 C27 C29 -137.66(12) . . . . ? C22 C18 C27 C29 63.69(16) . . . . ? Fe C18 C27 C29 -40.49(18) . . . . ? C19 C18 C27 C30 101.78(13) . . . . ? C22 C18 C27 C30 -56.88(15) . . . . ? Fe C18 C27 C30 -161.06(11) . . . . ? C19 C20 C31 C33 30.43(16) . . . . ? C21 C20 C31 C33 -168.67(11) . . . . ? Fe C20 C31 C33 -65.12(15) . . . . ? C19 C20 C31 C34 152.45(12) . . . . ? C21 C20 C31 C34 -46.66(16) . . . . ? Fe C20 C31 C34 56.90(16) . . . . ? C19 C20 C31 C32 -88.04(14) . . . . ? C21 C20 C31 C32 72.86(15) . . . . ? Fe C20 C31 C32 176.41(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.344 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.046 _iucr_refine_instructions_details ; TITL mima13 in P2(1)/c CELL 0.71073 18.3520 9.6436 17.7391 90.000 116.946 90.000 ZERR 4.00 0.0004 0.0002 0.0004 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H FE UNIT 136 184 4 SIZE 0.25 0.17 0.11 TEMP -173 SHEL 999 0.76 ACTA CONF FMAP 2 PLAN 10 L.S. 4 OMIT -6 3 1 OMIT -8 2 3 OMIT -7 3 3 OMIT 2 4 2 OMIT 0 1 7 OMIT -10 1 6 OMIT -7 1 4 OMIT -4 4 3 OMIT 6 2 1 OMIT -8 0 4 WGHT 0.035200 FVAR 2.53556 FE 3 0.737355 0.343218 0.522399 11.00000 0.01025 0.00969 = 0.00848 0.00022 0.00436 -0.00091 C1 1 0.751260 0.445978 0.425177 11.00000 0.01419 0.01407 = 0.00839 0.00227 0.00497 -0.00131 C2 1 0.717296 0.310668 0.399265 11.00000 0.01584 0.01349 = 0.00901 0.00017 0.00609 -0.00017 H2 2 0.742683 0.240420 0.381896 11.00000 0.01211 C3 1 0.642149 0.296518 0.403314 11.00000 0.01402 0.01303 = 0.00724 0.00088 0.00390 -0.00077 C4 1 0.625159 0.430477 0.428545 11.00000 0.01288 0.01319 = 0.00838 0.00242 0.00391 0.00009 C5 1 0.692589 0.521848 0.442183 11.00000 0.01463 0.01264 = 0.00824 0.00162 0.00445 -0.00118 C6 1 0.686345 0.665775 0.459116 11.00000 0.02108 0.01306 = 0.00961 0.00078 0.00546 -0.00303 AFIX 43 H6 2 0.730432 0.727071 0.469560 11.00000 -1.20000 AFIX 0 C7 1 0.617499 0.714058 0.460180 11.00000 0.02686 0.01320 = 0.01170 0.00162 0.00749 0.00395 AFIX 43 H7 2 0.613006 0.810110 0.469218 11.00000 -1.20000 AFIX 0 C8 1 0.551642 0.623497 0.447994 11.00000 0.01774 0.02282 = 0.01202 0.00325 0.00615 0.00804 AFIX 43 H8 2 0.504351 0.660089 0.449703 11.00000 -1.20000 AFIX 0 C9 1 0.555383 0.485392 0.433944 11.00000 0.01308 0.01962 = 0.01115 0.00253 0.00466 0.00048 AFIX 43 H9 2 0.511775 0.425868 0.427764 11.00000 -1.20000 AFIX 0 C10 1 0.820656 0.508361 0.411441 11.00000 0.01756 0.01830 = 0.01500 0.00018 0.00962 -0.00557 C11 1 0.885875 0.581163 0.490137 11.00000 0.01900 0.02474 = 0.01978 0.00018 0.01058 -0.00836 AFIX 137 H11A 2 0.859521 0.648989 0.510975 11.00000 -1.20000 H11B 2 0.924850 0.628709 0.475364 11.00000 -1.20000 H11C 2 0.914859 0.512232 0.534276 11.00000 -1.20000 AFIX 0 C12 1 0.861731 0.398032 0.381415 11.00000 0.02126 0.02658 = 0.02466 -0.00019 0.01648 -0.00397 AFIX 137 H12A 2 0.881816 0.322466 0.422789 11.00000 -1.20000 H12B 2 0.907671 0.439695 0.375675 11.00000 -1.20000 H12C 2 0.821975 0.361371 0.326575 11.00000 -1.20000 AFIX 0 C13 1 0.782564 0.615795 0.339527 11.00000 0.02915 0.02284 = 0.01831 0.00282 0.01323 -0.00719 AFIX 137 H13A 2 0.739663 0.571331 0.289375 11.00000 -1.20000 H13B 2 0.824963 0.652300 0.325800 11.00000 -1.20000 H13C 2 0.758875 0.691983 0.357735 11.00000 -1.20000 AFIX 0 C14 1 0.582811 0.175681 0.367751 11.00000 0.01435 0.01513 = 0.01083 -0.00143 0.00429 -0.00415 C15 1 0.519148 0.214548 0.277624 11.00000 0.02175 0.02644 = 0.01358 -0.00113 0.00331 -0.00784 AFIX 137 H15A 2 0.490441 0.299126 0.279564 11.00000 -1.20000 H15B 2 0.479711 0.138733 0.253608 11.00000 -1.20000 H15C 2 0.546752 0.230535 0.242312 11.00000 -1.20000 AFIX 0 C16 1 0.628253 0.045362 0.363141 11.00000 0.02428 0.01485 = 0.02057 -0.00434 0.01083 -0.00620 AFIX 137 H16A 2 0.653306 0.062423 0.325569 11.00000 -1.20000 H16B 2 0.589636 -0.031983 0.341073 11.00000 -1.20000 H16C 2 0.670908 0.022218 0.419830 11.00000 -1.20000 AFIX 0 C17 1 0.537690 0.144315 0.420839 11.00000 0.01707 0.01936 = 0.01716 0.00020 0.00753 -0.00610 AFIX 137 H17A 2 0.576054 0.151451 0.481076 11.00000 -1.20000 H17B 2 0.515059 0.050289 0.408322 11.00000 -1.20000 H17C 2 0.493238 0.211240 0.406909 11.00000 -1.20000 AFIX 0 C18 1 0.835538 0.217490 0.603278 11.00000 0.01194 0.01333 = 0.00983 0.00236 0.00397 0.00078 C19 1 0.846258 0.358273 0.631525 11.00000 0.01022 0.01536 = 0.00977 0.00111 0.00268 -0.00211 H19 2 0.891174 0.417507 0.638757 11.00000 0.00959 C20 1 0.781286 0.402274 0.648551 11.00000 0.01244 0.01202 = 0.00762 0.00101 0.00330 -0.00100 C21 1 0.729792 0.281996 0.635558 11.00000 0.01212 0.01128 = 0.00678 0.00073 0.00282 0.00011 C22 1 0.762887 0.169336 0.606902 11.00000 0.01231 0.01309 = 0.00766 0.00171 0.00371 0.00072 C23 1 0.727499 0.034130 0.597814 11.00000 0.01620 0.01165 = 0.01147 0.00020 0.00553 0.00028 AFIX 43 H23 2 0.746740 -0.040273 0.576551 11.00000 -1.20000 AFIX 0 C24 1 0.666511 0.012569 0.619614 11.00000 0.01825 0.01320 = 0.01322 0.00061 0.00561 -0.00379 AFIX 43 H24 2 0.644877 -0.078137 0.615671 11.00000 -1.20000 AFIX 0 C25 1 0.634317 0.123718 0.648346 11.00000 0.01537 0.01961 = 0.01408 -0.00059 0.00823 -0.00399 AFIX 43 H25 2 0.591780 0.105709 0.663522 11.00000 -1.20000 AFIX 0 C26 1 0.663347 0.254932 0.654425 11.00000 0.01376 0.01630 = 0.01063 -0.00119 0.00592 0.00043 AFIX 43 H26 2 0.639476 0.328541 0.671199 11.00000 -1.20000 AFIX 0 C27 1 0.901259 0.125928 0.598667 11.00000 0.01334 0.01805 = 0.01815 0.00274 0.00790 0.00317 C28 1 0.973525 0.213677 0.605095 11.00000 0.01504 0.02514 = 0.02589 0.00666 0.01145 0.00581 AFIX 137 H28A 2 0.954139 0.282160 0.559315 11.00000 -1.20000 H28B 2 1.014226 0.153363 0.600344 11.00000 -1.20000 H28C 2 0.998399 0.261593 0.659736 11.00000 -1.20000 AFIX 0 C29 1 0.869925 0.038629 0.517694 11.00000 0.02186 0.02205 = 0.02581 -0.00121 0.01400 0.00602 AFIX 137 H29A 2 0.822474 -0.015754 0.511665 11.00000 -1.20000 H29B 2 0.913275 -0.024115 0.520980 11.00000 -1.20000 H29C 2 0.854012 0.099995 0.468716 11.00000 -1.20000 AFIX 0 C30 1 0.933015 0.028546 0.676188 11.00000 0.01598 0.02132 = 0.02622 0.00743 0.00924 0.00582 AFIX 137 H30A 2 0.952449 0.083977 0.727992 11.00000 -1.20000 H30B 2 0.978096 -0.027722 0.677630 11.00000 -1.20000 H30C 2 0.888644 -0.032396 0.672120 11.00000 -1.20000 AFIX 0 C31 1 0.781074 0.534748 0.695023 11.00000 0.01560 0.01276 = 0.00904 -0.00138 0.00491 -0.00187 C32 1 0.820980 0.497623 0.790023 11.00000 0.02184 0.01480 = 0.01143 -0.00172 0.00578 -0.00155 AFIX 137 H32A 2 0.789160 0.424427 0.799753 11.00000 -1.20000 H32B 2 0.822175 0.579997 0.822916 11.00000 -1.20000 H32C 2 0.876923 0.464890 0.807672 11.00000 -1.20000 AFIX 0 C33 1 0.831832 0.647654 0.679850 11.00000 0.02254 0.01318 = 0.01424 -0.00235 0.00798 -0.00354 AFIX 137 H33A 2 0.887976 0.614612 0.699214 11.00000 -1.20000 H33B 2 0.832213 0.731413 0.711310 11.00000 -1.20000 H33C 2 0.807736 0.669069 0.619333 11.00000 -1.20000 AFIX 0 C34 1 0.695090 0.592521 0.669503 11.00000 0.02135 0.01339 = 0.01453 -0.00071 0.00801 0.00038 AFIX 137 H34A 2 0.663829 0.592807 0.607722 11.00000 -1.20000 H34B 2 0.699365 0.687432 0.690853 11.00000 -1.20000 H34C 2 0.667202 0.534197 0.693647 11.00000 -1.20000 HKLF 4 ; # Attachment '- mima14.cif' data_mima14 _database_code_depnum_ccdc_archive 'CCDC 884307' #TrackingRef '- mima14.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 Mn' _chemical_formula_weight 509.65 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.9709(4) _cell_length_b 9.6949(2) _cell_length_c 18.0377(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.575(2) _cell_angle_gamma 90.00 _cell_volume 2857.97(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22122 _cell_measurement_theta_min 4.5406 _cell_measurement_theta_max 75.6595 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 3.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82982 _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 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37822 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.93 _diffrn_reflns_theta_max 75.85 _reflns_number_total 5934 _reflns_number_gt 5248 _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 of the C2 and C19 atoms were refined freely. ; _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^)+(0.0466P)^2^+0.2818P] 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 5934 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.002 _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 Mn Mn 0.736485(12) 0.33569(2) 0.516236(11) 0.02221(7) Uani 1 1 d . . . C1 C 0.74416(8) 0.46150(13) 0.40261(7) 0.0219(2) Uani 1 1 d . . . C2 C 0.71040(8) 0.32721(12) 0.38095(7) 0.0201(2) Uani 1 1 d . . . H2 H 0.7348(9) 0.2552(16) 0.3629(9) 0.022(4) Uiso 1 1 d . . . C3 C 0.63393(7) 0.31523(12) 0.38711(7) 0.0195(2) Uani 1 1 d . . . C4 C 0.61729(7) 0.45025(13) 0.40998(7) 0.0207(2) Uani 1 1 d . . . C5 C 0.68537(8) 0.54026(13) 0.41976(7) 0.0222(2) Uani 1 1 d . . . C6 C 0.68193(9) 0.68102(13) 0.44090(8) 0.0272(3) Uani 1 1 d . . . H6 H 0.7264 0.7411 0.4489 0.033 Uiso 1 1 calc R . . C7 C 0.61445(9) 0.72962(14) 0.44976(8) 0.0304(3) Uani 1 1 d . . . H7 H 0.6123 0.8240 0.4630 0.036 Uiso 1 1 calc R . . C8 C 0.54819(9) 0.64243(14) 0.43964(8) 0.0286(3) Uani 1 1 d . . . H8 H 0.5021 0.6791 0.4459 0.034 Uiso 1 1 calc R . . C9 C 0.54911(8) 0.50523(14) 0.42092(7) 0.0253(3) Uani 1 1 d . . . H9 H 0.5044 0.4473 0.4153 0.030 Uiso 1 1 calc R . . C10 C 0.82191(8) 0.51486(14) 0.39749(8) 0.0267(3) Uani 1 1 d . . . C11 C 0.88269(9) 0.57323(15) 0.48009(8) 0.0312(3) Uani 1 1 d . . . H11A H 0.8564 0.6479 0.4971 0.037 Uiso 1 1 calc R . . H11B H 0.9311 0.6091 0.4745 0.037 Uiso 1 1 calc R . . H11C H 0.8992 0.4998 0.5211 0.037 Uiso 1 1 calc R . . C12 C 0.86436(9) 0.39963(16) 0.37167(9) 0.0332(3) Uani 1 1 d . . . H12A H 0.8787 0.3243 0.4115 0.040 Uiso 1 1 calc R . . H12B H 0.9142 0.4358 0.3692 0.040 Uiso 1 1 calc R . . H12C H 0.8274 0.3650 0.3178 0.040 Uiso 1 1 calc R . . C13 C 0.79918(10) 0.63008(16) 0.33337(9) 0.0351(3) Uani 1 1 d . . . H13A H 0.7629 0.5930 0.2799 0.042 Uiso 1 1 calc R . . H13B H 0.8490 0.6663 0.3309 0.042 Uiso 1 1 calc R . . H13C H 0.7711 0.7044 0.3484 0.042 Uiso 1 1 calc R . . C14 C 0.57633(7) 0.19164(13) 0.36189(7) 0.0212(2) Uani 1 1 d . . . C15 C 0.50031(8) 0.22613(15) 0.28359(8) 0.0299(3) Uani 1 1 d . . . H15A H 0.4715 0.3047 0.2938 0.036 Uiso 1 1 calc R . . H15B H 0.4638 0.1460 0.2671 0.036 Uiso 1 1 calc R . . H15C H 0.5172 0.2496 0.2400 0.036 Uiso 1 1 calc R . . C16 C 0.61876(8) 0.06617(13) 0.34527(8) 0.0268(3) Uani 1 1 d . . . H16A H 0.6340 0.0869 0.3002 0.032 Uiso 1 1 calc R . . H16B H 0.5814 -0.0129 0.3307 0.032 Uiso 1 1 calc R . . H16C H 0.6681 0.0442 0.3943 0.032 Uiso 1 1 calc R . . C17 C 0.54977(8) 0.15293(14) 0.43016(8) 0.0260(3) Uani 1 1 d . . . H17A H 0.5983 0.1346 0.4806 0.031 Uiso 1 1 calc R . . H17B H 0.5154 0.0702 0.4143 0.031 Uiso 1 1 calc R . . H17C H 0.5187 0.2293 0.4390 0.031 Uiso 1 1 calc R . . C18 C 0.84211(7) 0.17678(13) 0.61334(7) 0.0209(2) Uani 1 1 d . . . C19 C 0.85118(7) 0.31776(13) 0.63623(7) 0.0210(2) Uani 1 1 d . . . H19 H 0.8968(10) 0.3727(17) 0.6406(9) 0.027(4) Uiso 1 1 d . . . C20 C 0.78445(7) 0.36561(13) 0.65322(7) 0.0203(2) Uani 1 1 d . . . C21 C 0.73432(7) 0.24561(12) 0.64569(7) 0.0193(2) Uani 1 1 d . . . C22 C 0.76895(7) 0.13035(13) 0.61961(7) 0.0199(2) Uani 1 1 d . . . C23 C 0.73025(7) -0.00055(12) 0.60793(7) 0.0220(2) Uani 1 1 d . . . H23 H 0.7506 -0.0759 0.5881 0.026 Uiso 1 1 calc R . . C24 C 0.66334(8) -0.01795(13) 0.62536(7) 0.0235(2) Uani 1 1 d . . . H24 H 0.6381 -0.1060 0.6181 0.028 Uiso 1 1 calc R . . C25 C 0.63154(8) 0.09306(14) 0.65381(7) 0.0244(3) Uani 1 1 d . . . H25 H 0.5861 0.0779 0.6669 0.029 Uiso 1 1 calc R . . C26 C 0.66505(7) 0.22249(13) 0.66294(7) 0.0225(2) Uani 1 1 d . . . H26 H 0.6420 0.2966 0.6808 0.027 Uiso 1 1 calc R . . C27 C 0.90351(8) 0.08796(14) 0.59688(8) 0.0261(3) Uani 1 1 d . . . C28 C 0.97590(8) 0.17542(15) 0.60041(10) 0.0323(3) Uani 1 1 d . . . H28A H 0.9561 0.2478 0.5588 0.039 Uiso 1 1 calc R . . H28B H 1.0150 0.1166 0.5903 0.039 Uiso 1 1 calc R . . H28C H 1.0029 0.2178 0.6544 0.039 Uiso 1 1 calc R . . C29 C 0.86409(9) 0.01930(15) 0.51259(9) 0.0336(3) Uani 1 1 d . . . H29A H 0.8163 -0.0344 0.5085 0.040 Uiso 1 1 calc R . . H29B H 0.9039 -0.0420 0.5053 0.040 Uiso 1 1 calc R . . H29C H 0.8469 0.0905 0.4702 0.040 Uiso 1 1 calc R . . C30 C 0.93630(8) -0.02423(15) 0.66326(10) 0.0345(3) Uani 1 1 d . . . H30A H 0.9607 0.0195 0.7171 0.041 Uiso 1 1 calc R . . H30B H 0.9779 -0.0792 0.6548 0.041 Uiso 1 1 calc R . . H30C H 0.8912 -0.0842 0.6600 0.041 Uiso 1 1 calc R . . C31 C 0.78117(8) 0.50354(12) 0.69239(7) 0.0222(2) Uani 1 1 d . . . C32 C 0.81061(8) 0.48002(13) 0.78477(7) 0.0258(3) Uani 1 1 d . . . H32A H 0.7744 0.4137 0.7944 0.031 Uiso 1 1 calc R . . H32B H 0.8096 0.5677 0.8114 0.031 Uiso 1 1 calc R . . H32C H 0.8666 0.4437 0.8073 0.031 Uiso 1 1 calc R . . C33 C 0.83734(9) 0.60952(14) 0.67824(8) 0.0289(3) Uani 1 1 d . . . H33A H 0.8938 0.5756 0.7023 0.035 Uiso 1 1 calc R . . H33B H 0.8343 0.6973 0.7038 0.035 Uiso 1 1 calc R . . H33C H 0.8198 0.6234 0.6196 0.035 Uiso 1 1 calc R . . C34 C 0.69443(9) 0.56512(14) 0.65769(8) 0.0294(3) Uani 1 1 d . . . H34A H 0.6754 0.5791 0.5988 0.035 Uiso 1 1 calc R . . H34B H 0.6953 0.6538 0.6841 0.035 Uiso 1 1 calc R . . H34C H 0.6573 0.5017 0.6680 0.035 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 Mn 0.02349(11) 0.02480(11) 0.01620(10) 0.00059(7) 0.00612(8) -0.00097(8) C1 0.0256(6) 0.0201(6) 0.0191(5) 0.0004(5) 0.0084(5) -0.0033(5) C2 0.0237(6) 0.0201(6) 0.0172(5) 0.0000(4) 0.0091(5) -0.0009(5) C3 0.0223(6) 0.0186(6) 0.0168(5) 0.0001(4) 0.0075(4) -0.0006(4) C4 0.0249(6) 0.0196(6) 0.0162(5) 0.0017(4) 0.0071(5) 0.0014(5) C5 0.0287(6) 0.0193(6) 0.0170(5) 0.0008(4) 0.0078(5) -0.0019(5) C6 0.0370(7) 0.0196(6) 0.0211(6) 0.0010(5) 0.0084(5) -0.0027(5) C7 0.0463(8) 0.0198(6) 0.0209(6) 0.0008(5) 0.0098(6) 0.0068(6) C8 0.0345(7) 0.0289(7) 0.0209(6) 0.0020(5) 0.0099(5) 0.0105(5) C9 0.0260(6) 0.0279(7) 0.0200(6) 0.0022(5) 0.0074(5) 0.0045(5) C10 0.0282(6) 0.0277(7) 0.0246(6) 0.0010(5) 0.0115(5) -0.0085(5) C11 0.0311(7) 0.0342(7) 0.0275(6) -0.0001(6) 0.0112(6) -0.0119(6) C12 0.0312(7) 0.0383(8) 0.0354(7) -0.0028(6) 0.0191(6) -0.0090(6) C13 0.0413(8) 0.0351(8) 0.0283(7) 0.0046(6) 0.0139(6) -0.0122(6) C14 0.0221(6) 0.0214(6) 0.0188(5) -0.0005(4) 0.0073(5) -0.0027(5) C15 0.0298(7) 0.0315(7) 0.0210(6) -0.0008(5) 0.0033(5) -0.0052(6) C16 0.0315(7) 0.0200(6) 0.0310(6) -0.0041(5) 0.0152(5) -0.0055(5) C17 0.0264(6) 0.0278(7) 0.0250(6) -0.0001(5) 0.0117(5) -0.0055(5) C18 0.0199(6) 0.0211(6) 0.0200(5) 0.0017(4) 0.0067(5) -0.0003(4) C19 0.0190(6) 0.0216(6) 0.0198(5) 0.0018(4) 0.0054(5) -0.0030(5) C20 0.0229(6) 0.0193(6) 0.0169(5) 0.0011(4) 0.0064(4) -0.0011(4) C21 0.0198(5) 0.0197(6) 0.0158(5) 0.0006(4) 0.0049(4) -0.0007(4) C22 0.0200(5) 0.0199(6) 0.0176(5) 0.0011(4) 0.0057(4) -0.0002(4) C23 0.0231(6) 0.0185(6) 0.0225(6) -0.0002(5) 0.0075(5) -0.0003(5) C24 0.0237(6) 0.0211(6) 0.0235(6) 0.0006(5) 0.0077(5) -0.0043(5) C25 0.0227(6) 0.0277(6) 0.0236(6) -0.0003(5) 0.0105(5) -0.0040(5) C26 0.0225(6) 0.0245(6) 0.0206(5) -0.0008(5) 0.0090(5) 0.0002(5) C27 0.0228(6) 0.0231(6) 0.0332(7) 0.0026(5) 0.0125(5) 0.0026(5) C28 0.0252(6) 0.0330(7) 0.0421(8) 0.0071(6) 0.0175(6) 0.0029(5) C29 0.0345(7) 0.0313(7) 0.0408(8) -0.0049(6) 0.0216(6) 0.0041(6) C30 0.0247(6) 0.0298(7) 0.0479(8) 0.0116(6) 0.0141(6) 0.0057(5) C31 0.0275(6) 0.0185(6) 0.0189(5) 0.0001(4) 0.0078(5) -0.0013(5) C32 0.0337(7) 0.0220(6) 0.0194(6) -0.0009(5) 0.0088(5) -0.0029(5) C33 0.0395(7) 0.0208(6) 0.0270(6) -0.0025(5) 0.0146(6) -0.0062(5) C34 0.0346(7) 0.0224(6) 0.0276(6) 0.0005(5) 0.0094(6) 0.0042(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn C20 2.2717(12) . ? Mn C2 2.2869(12) . ? Mn C19 2.2918(12) . ? Mn C3 2.3001(12) . ? Mn C1 2.4378(12) . ? Mn C4 2.4659(12) . ? Mn C18 2.5058(12) . ? Mn C21 2.5084(12) . ? Mn C5 2.5448(12) . ? Mn C22 2.6221(12) . ? C1 C2 1.4208(17) . ? C1 C5 1.4377(18) . ? C1 C10 1.5283(17) . ? C2 C3 1.4289(17) . ? C3 C4 1.4407(17) . ? C3 C14 1.5240(16) . ? C4 C9 1.4231(18) . ? C4 C5 1.4526(17) . ? C5 C6 1.4251(18) . ? C6 C7 1.371(2) . ? C7 C8 1.409(2) . ? C8 C9 1.3742(19) . ? C10 C12 1.531(2) . ? C10 C13 1.5360(19) . ? C10 C11 1.5426(18) . ? C14 C16 1.5301(17) . ? C14 C15 1.5389(17) . ? C14 C17 1.5408(17) . ? C18 C19 1.4175(17) . ? C18 C22 1.4379(17) . ? C18 C27 1.5231(17) . ? C19 C20 1.4326(17) . ? C20 C21 1.4429(17) . ? C20 C31 1.5250(17) . ? C21 C26 1.4208(17) . ? C21 C22 1.4494(17) . ? C22 C23 1.4202(17) . ? C23 C24 1.3738(18) . ? C24 C25 1.4114(18) . ? C25 C26 1.3718(18) . ? C27 C28 1.5318(18) . ? C27 C29 1.5365(19) . ? C27 C30 1.5417(18) . ? C31 C33 1.5342(18) . ? C31 C34 1.5384(18) . ? C31 C32 1.5413(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Mn C2 169.07(4) . . ? C20 Mn C19 36.59(4) . . ? C2 Mn C19 135.21(5) . . ? C20 Mn C3 153.41(5) . . ? C2 Mn C3 36.30(4) . . ? C19 Mn C3 167.67(4) . . ? C20 Mn C1 136.22(4) . . ? C2 Mn C1 34.82(4) . . ? C19 Mn C1 119.26(4) . . ? C3 Mn C1 59.57(4) . . ? C20 Mn C4 127.01(4) . . ? C2 Mn C4 57.35(4) . . ? C19 Mn C4 156.57(4) . . ? C3 Mn C4 34.97(4) . . ? C1 Mn C4 57.03(4) . . ? C20 Mn C18 58.92(4) . . ? C2 Mn C18 118.90(4) . . ? C19 Mn C18 34.00(4) . . ? C3 Mn C18 135.22(4) . . ? C1 Mn C18 127.16(4) . . ? C4 Mn C18 168.77(4) . . ? C20 Mn C21 34.69(4) . . ? C2 Mn C21 154.84(4) . . ? C19 Mn C21 56.67(4) . . ? C3 Mn C21 126.62(4) . . ? C1 Mn C21 170.08(4) . . ? C4 Mn C21 122.38(4) . . ? C18 Mn C21 55.65(4) . . ? C20 Mn C5 120.67(4) . . ? C2 Mn C5 56.14(4) . . ? C19 Mn C5 129.20(4) . . ? C3 Mn C5 57.68(4) . . ? C1 Mn C5 33.45(4) . . ? C4 Mn C5 33.66(4) . . ? C18 Mn C5 155.54(4) . . ? C21 Mn C5 140.08(4) . . ? C20 Mn C22 56.77(4) . . ? C2 Mn C22 128.15(4) . . ? C19 Mn C22 54.84(4) . . ? C3 Mn C22 120.15(4) . . ? C1 Mn C22 154.70(4) . . ? C4 Mn C22 139.39(4) . . ? C18 Mn C22 32.47(4) . . ? C21 Mn C22 32.72(4) . . ? C5 Mn C22 171.22(4) . . ? C2 C1 C5 106.13(11) . . ? C2 C1 C10 126.16(12) . . ? C5 C1 C10 127.26(11) . . ? C2 C1 Mn 66.78(7) . . ? C5 C1 Mn 77.36(7) . . ? C10 C1 Mn 126.37(8) . . ? C1 C2 C3 111.57(11) . . ? C1 C2 Mn 78.41(7) . . ? C3 C2 Mn 72.35(7) . . ? C2 C3 C4 105.62(10) . . ? C2 C3 C14 126.62(11) . . ? C4 C3 C14 127.14(11) . . ? C2 C3 Mn 71.35(7) . . ? C4 C3 Mn 78.82(7) . . ? C14 C3 Mn 121.92(8) . . ? C9 C4 C3 132.31(12) . . ? C9 C4 C5 119.24(11) . . ? C3 C4 C5 108.42(11) . . ? C9 C4 Mn 125.49(8) . . ? C3 C4 Mn 66.21(6) . . ? C5 C4 Mn 76.15(7) . . ? C6 C5 C1 133.13(12) . . ? C6 C5 C4 118.66(12) . . ? C1 C5 C4 108.18(11) . . ? C6 C5 Mn 127.35(8) . . ? C1 C5 Mn 69.19(7) . . ? C4 C5 Mn 70.19(7) . . ? C7 C6 C5 119.95(13) . . ? C6 C7 C8 121.31(13) . . ? C9 C8 C7 121.11(13) . . ? C8 C9 C4 119.71(13) . . ? C1 C10 C12 110.81(11) . . ? C1 C10 C13 109.16(11) . . ? C12 C10 C13 108.17(12) . . ? C1 C10 C11 111.32(11) . . ? C12 C10 C11 108.62(12) . . ? C13 C10 C11 108.68(11) . . ? C3 C14 C16 110.58(10) . . ? C3 C14 C15 109.67(10) . . ? C16 C14 C15 108.51(10) . . ? C3 C14 C17 110.52(10) . . ? C16 C14 C17 107.96(10) . . ? C15 C14 C17 109.55(11) . . ? C19 C18 C22 106.09(11) . . ? C19 C18 C27 126.66(11) . . ? C22 C18 C27 126.77(11) . . ? C19 C18 Mn 64.70(7) . . ? C22 C18 Mn 78.22(7) . . ? C27 C18 Mn 127.66(8) . . ? C18 C19 C20 111.68(11) . . ? C18 C19 Mn 81.30(7) . . ? C20 C19 Mn 70.94(7) . . ? C19 C20 C21 105.32(10) . . ? C19 C20 C31 125.46(11) . . ? C21 C20 C31 127.42(11) . . ? C19 C20 Mn 72.47(7) . . ? C21 C20 Mn 81.66(7) . . ? C31 C20 Mn 123.06(8) . . ? C26 C21 C20 132.55(11) . . ? C26 C21 C22 118.88(11) . . ? C20 C21 C22 108.45(11) . . ? C26 C21 Mn 127.81(8) . . ? C20 C21 Mn 63.65(6) . . ? C22 C21 Mn 77.95(7) . . ? C23 C22 C18 132.49(12) . . ? C23 C22 C21 119.15(11) . . ? C18 C22 C21 108.31(10) . . ? C23 C22 Mn 128.51(8) . . ? C18 C22 Mn 69.31(7) . . ? C21 C22 Mn 69.32(6) . . ? C24 C23 C22 119.80(12) . . ? C23 C24 C25 120.99(11) . . ? C26 C25 C24 121.15(12) . . ? C25 C26 C21 119.92(12) . . ? C18 C27 C28 110.52(11) . . ? C18 C27 C29 111.38(11) . . ? C28 C27 C29 108.36(12) . . ? C18 C27 C30 108.75(11) . . ? C28 C27 C30 108.33(11) . . ? C29 C27 C30 109.44(12) . . ? C20 C31 C33 110.81(11) . . ? C20 C31 C34 112.31(10) . . ? C33 C31 C34 107.33(11) . . ? C20 C31 C32 108.01(10) . . ? C33 C31 C32 108.98(10) . . ? C34 C31 C32 109.35(11) . . ? 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 C20 Mn C1 C2 170.05(7) . . . . ? C19 Mn C1 C2 128.26(7) . . . . ? C3 Mn C1 C2 -37.59(7) . . . . ? C4 Mn C1 C2 -78.85(8) . . . . ? C18 Mn C1 C2 88.41(8) . . . . ? C21 Mn C1 C2 -168.6(2) . . . . ? C5 Mn C1 C2 -113.96(10) . . . . ? C22 Mn C1 C2 59.31(12) . . . . ? C20 Mn C1 C5 -75.99(9) . . . . ? C2 Mn C1 C5 113.96(10) . . . . ? C19 Mn C1 C5 -117.78(7) . . . . ? C3 Mn C1 C5 76.37(7) . . . . ? C4 Mn C1 C5 35.12(7) . . . . ? C18 Mn C1 C5 -157.63(7) . . . . ? C21 Mn C1 C5 -54.7(3) . . . . ? C22 Mn C1 C5 173.27(8) . . . . ? C20 Mn C1 C10 51.27(13) . . . . ? C2 Mn C1 C10 -118.78(14) . . . . ? C19 Mn C1 C10 9.47(12) . . . . ? C3 Mn C1 C10 -156.37(12) . . . . ? C4 Mn C1 C10 162.37(12) . . . . ? C18 Mn C1 C10 -30.37(12) . . . . ? C21 Mn C1 C10 72.6(3) . . . . ? C5 Mn C1 C10 127.26(14) . . . . ? C22 Mn C1 C10 -59.47(15) . . . . ? C5 C1 C2 C3 -2.61(13) . . . . ? C10 C1 C2 C3 -175.39(11) . . . . ? Mn C1 C2 C3 65.55(8) . . . . ? C5 C1 C2 Mn -68.16(8) . . . . ? C10 C1 C2 Mn 119.06(12) . . . . ? C20 Mn C2 C1 -39.1(3) . . . . ? C19 Mn C2 C1 -76.51(9) . . . . ? C3 Mn C2 C1 117.32(10) . . . . ? C4 Mn C2 C1 77.83(8) . . . . ? C18 Mn C2 C1 -114.50(7) . . . . ? C21 Mn C2 C1 175.42(9) . . . . ? C5 Mn C2 C1 37.35(7) . . . . ? C22 Mn C2 C1 -152.14(7) . . . . ? C20 Mn C2 C3 -156.4(2) . . . . ? C19 Mn C2 C3 166.17(7) . . . . ? C1 Mn C2 C3 -117.32(10) . . . . ? C4 Mn C2 C3 -39.49(7) . . . . ? C18 Mn C2 C3 128.18(7) . . . . ? C21 Mn C2 C3 58.10(13) . . . . ? C5 Mn C2 C3 -79.98(7) . . . . ? C22 Mn C2 C3 90.54(8) . . . . ? C1 C2 C3 C4 2.76(13) . . . . ? Mn C2 C3 C4 72.12(8) . . . . ? C1 C2 C3 C14 174.25(11) . . . . ? Mn C2 C3 C14 -116.39(11) . . . . ? C1 C2 C3 Mn -69.36(9) . . . . ? C20 Mn C3 C2 170.23(9) . . . . ? C19 Mn C3 C2 -52.1(2) . . . . ? C1 Mn C3 C2 36.04(7) . . . . ? C4 Mn C3 C2 110.88(10) . . . . ? C18 Mn C3 C2 -77.70(9) . . . . ? C21 Mn C3 C2 -153.28(7) . . . . ? C5 Mn C3 C2 75.38(7) . . . . ? C22 Mn C3 C2 -114.58(7) . . . . ? C20 Mn C3 C4 59.35(12) . . . . ? C2 Mn C3 C4 -110.88(10) . . . . ? C19 Mn C3 C4 -162.97(19) . . . . ? C1 Mn C3 C4 -74.85(7) . . . . ? C18 Mn C3 C4 171.41(7) . . . . ? C21 Mn C3 C4 95.84(8) . . . . ? C5 Mn C3 C4 -35.51(7) . . . . ? C22 Mn C3 C4 134.53(7) . . . . ? C20 Mn C3 C14 -67.66(14) . . . . ? C2 Mn C3 C14 122.11(13) . . . . ? C19 Mn C3 C14 70.0(2) . . . . ? C1 Mn C3 C14 158.14(11) . . . . ? C4 Mn C3 C14 -127.01(13) . . . . ? C18 Mn C3 C14 44.40(12) . . . . ? C21 Mn C3 C14 -31.17(11) . . . . ? C5 Mn C3 C14 -162.52(11) . . . . ? C22 Mn C3 C14 7.52(11) . . . . ? C2 C3 C4 C9 176.01(12) . . . . ? C14 C3 C4 C9 4.6(2) . . . . ? Mn C3 C4 C9 -117.18(13) . . . . ? C2 C3 C4 C5 -1.80(13) . . . . ? C14 C3 C4 C5 -173.23(11) . . . . ? Mn C3 C4 C5 65.01(8) . . . . ? C2 C3 C4 Mn -66.81(8) . . . . ? C14 C3 C4 Mn 121.77(12) . . . . ? C20 Mn C4 C9 -25.07(13) . . . . ? C2 Mn C4 C9 167.16(13) . . . . ? C19 Mn C4 C9 -62.94(17) . . . . ? C3 Mn C4 C9 126.10(14) . . . . ? C1 Mn C4 C9 -151.13(12) . . . . ? C18 Mn C4 C9 93.4(2) . . . . ? C21 Mn C4 C9 17.10(13) . . . . ? C5 Mn C4 C9 -116.23(14) . . . . ? C22 Mn C4 C9 54.84(13) . . . . ? C20 Mn C4 C3 -151.17(7) . . . . ? C2 Mn C4 C3 41.06(7) . . . . ? C19 Mn C4 C3 170.96(10) . . . . ? C1 Mn C4 C3 82.77(8) . . . . ? C18 Mn C4 C3 -32.7(2) . . . . ? C21 Mn C4 C3 -109.00(7) . . . . ? C5 Mn C4 C3 117.67(10) . . . . ? C22 Mn C4 C3 -71.26(9) . . . . ? C20 Mn C4 C5 91.17(8) . . . . ? C2 Mn C4 C5 -76.60(7) . . . . ? C19 Mn C4 C5 53.29(14) . . . . ? C3 Mn C4 C5 -117.67(10) . . . . ? C1 Mn C4 C5 -34.90(7) . . . . ? C18 Mn C4 C5 -150.36(19) . . . . ? C21 Mn C4 C5 133.33(7) . . . . ? C22 Mn C4 C5 171.07(7) . . . . ? C2 C1 C5 C6 -176.82(13) . . . . ? C10 C1 C5 C6 -4.1(2) . . . . ? Mn C1 C5 C6 122.23(14) . . . . ? C2 C1 C5 C4 1.38(13) . . . . ? C10 C1 C5 C4 174.06(11) . . . . ? Mn C1 C5 C4 -59.57(8) . . . . ? C2 C1 C5 Mn 60.95(8) . . . . ? C10 C1 C5 Mn -126.37(12) . . . . ? C9 C4 C5 C6 0.63(17) . . . . ? C3 C4 C5 C6 178.78(10) . . . . ? Mn C4 C5 C6 -122.55(10) . . . . ? C9 C4 C5 C1 -177.87(10) . . . . ? C3 C4 C5 C1 0.27(13) . . . . ? Mn C4 C5 C1 58.95(8) . . . . ? C9 C4 C5 Mn 123.18(11) . . . . ? C3 C4 C5 Mn -58.67(8) . . . . ? C20 Mn C5 C6 -0.35(14) . . . . ? C2 Mn C5 C6 -167.97(14) . . . . ? C19 Mn C5 C6 -44.21(14) . . . . ? C3 Mn C5 C6 148.41(13) . . . . ? C1 Mn C5 C6 -129.05(15) . . . . ? C4 Mn C5 C6 111.50(14) . . . . ? C18 Mn C5 C6 -81.95(16) . . . . ? C21 Mn C5 C6 38.30(15) . . . . ? C22 Mn C5 C6 70.1(3) . . . . ? C20 Mn C5 C1 128.70(7) . . . . ? C2 Mn C5 C1 -38.92(7) . . . . ? C19 Mn C5 C1 84.83(8) . . . . ? C3 Mn C5 C1 -82.54(8) . . . . ? C4 Mn C5 C1 -119.46(10) . . . . ? C18 Mn C5 C1 47.09(13) . . . . ? C21 Mn C5 C1 167.35(7) . . . . ? C22 Mn C5 C1 -160.9(2) . . . . ? C20 Mn C5 C4 -111.84(7) . . . . ? C2 Mn C5 C4 80.53(7) . . . . ? C19 Mn C5 C4 -155.71(7) . . . . ? C3 Mn C5 C4 36.92(7) . . . . ? C1 Mn C5 C4 119.46(10) . . . . ? C18 Mn C5 C4 166.55(9) . . . . ? C21 Mn C5 C4 -73.19(9) . . . . ? C22 Mn C5 C4 -41.4(3) . . . . ? C1 C5 C6 C7 176.57(13) . . . . ? C4 C5 C6 C7 -1.48(18) . . . . ? Mn C5 C6 C7 -87.55(14) . . . . ? C5 C6 C7 C8 1.02(19) . . . . ? C6 C7 C8 C9 0.3(2) . . . . ? C7 C8 C9 C4 -1.21(19) . . . . ? C3 C4 C9 C8 -176.93(12) . . . . ? C5 C4 C9 C8 0.70(17) . . . . ? Mn C4 C9 C8 94.26(13) . . . . ? C2 C1 C10 C12 -4.52(17) . . . . ? C5 C1 C10 C12 -175.80(12) . . . . ? Mn C1 C10 C12 81.56(13) . . . . ? C2 C1 C10 C13 114.50(14) . . . . ? C5 C1 C10 C13 -56.77(16) . . . . ? Mn C1 C10 C13 -159.41(9) . . . . ? C2 C1 C10 C11 -125.53(13) . . . . ? C5 C1 C10 C11 63.20(17) . . . . ? Mn C1 C10 C11 -39.44(15) . . . . ? C2 C3 C14 C16 12.26(16) . . . . ? C4 C3 C14 C16 -178.05(11) . . . . ? Mn C3 C14 C16 -77.37(12) . . . . ? C2 C3 C14 C15 -107.37(14) . . . . ? C4 C3 C14 C15 62.32(15) . . . . ? Mn C3 C14 C15 163.00(9) . . . . ? C2 C3 C14 C17 131.75(12) . . . . ? C4 C3 C14 C17 -58.56(16) . . . . ? Mn C3 C14 C17 42.12(13) . . . . ? C20 Mn C18 C19 -38.47(7) . . . . ? C2 Mn C18 C19 129.15(7) . . . . ? C3 Mn C18 C19 170.50(7) . . . . ? C1 Mn C18 C19 88.46(8) . . . . ? C4 Mn C18 C19 -163.43(19) . . . . ? C21 Mn C18 C19 -79.81(8) . . . . ? C5 Mn C18 C19 58.02(13) . . . . ? C22 Mn C18 C19 -114.31(10) . . . . ? C20 Mn C18 C22 75.84(7) . . . . ? C2 Mn C18 C22 -116.54(7) . . . . ? C19 Mn C18 C22 114.31(10) . . . . ? C3 Mn C18 C22 -75.19(9) . . . . ? C1 Mn C18 C22 -157.22(7) . . . . ? C4 Mn C18 C22 -49.1(2) . . . . ? C21 Mn C18 C22 34.51(7) . . . . ? C5 Mn C18 C22 172.33(9) . . . . ? C20 Mn C18 C27 -156.47(12) . . . . ? C2 Mn C18 C27 11.16(12) . . . . ? C19 Mn C18 C27 -117.99(14) . . . . ? C3 Mn C18 C27 52.51(13) . . . . ? C1 Mn C18 C27 -29.53(12) . . . . ? C4 Mn C18 C27 78.6(2) . . . . ? C21 Mn C18 C27 162.20(12) . . . . ? C5 Mn C18 C27 -59.97(16) . . . . ? C22 Mn C18 C27 127.70(14) . . . . ? C22 C18 C19 C20 -2.80(14) . . . . ? C27 C18 C19 C20 -175.23(11) . . . . ? Mn C18 C19 C20 65.40(8) . . . . ? C22 C18 C19 Mn -68.20(8) . . . . ? C27 C18 C19 Mn 119.38(12) . . . . ? C20 Mn C19 C18 116.63(10) . . . . ? C2 Mn C19 C18 -74.52(9) . . . . ? C3 Mn C19 C18 -33.0(2) . . . . ? C1 Mn C19 C18 -114.05(7) . . . . ? C4 Mn C19 C18 171.97(9) . . . . ? C21 Mn C19 C18 76.55(8) . . . . ? C5 Mn C19 C18 -153.05(7) . . . . ? C22 Mn C19 C18 36.76(7) . . . . ? C2 Mn C19 C20 168.85(7) . . . . ? C3 Mn C19 C20 -149.63(19) . . . . ? C1 Mn C19 C20 129.32(7) . . . . ? C4 Mn C19 C20 55.34(14) . . . . ? C18 Mn C19 C20 -116.63(10) . . . . ? C21 Mn C19 C20 -40.08(7) . . . . ? C5 Mn C19 C20 90.32(8) . . . . ? C22 Mn C19 C20 -79.87(7) . . . . ? C18 C19 C20 C21 3.90(13) . . . . ? Mn C19 C20 C21 75.87(8) . . . . ? C18 C19 C20 C31 169.51(11) . . . . ? Mn C19 C20 C31 -118.52(11) . . . . ? C18 C19 C20 Mn -71.97(9) . . . . ? C2 Mn C20 C19 -45.9(3) . . . . ? C3 Mn C20 C19 166.05(9) . . . . ? C1 Mn C20 C19 -77.27(9) . . . . ? C4 Mn C20 C19 -155.82(7) . . . . ? C18 Mn C20 C19 35.71(7) . . . . ? C21 Mn C20 C19 109.05(10) . . . . ? C5 Mn C20 C19 -115.72(7) . . . . ? C22 Mn C20 C19 74.19(7) . . . . ? C2 Mn C20 C21 -155.0(2) . . . . ? C19 Mn C20 C21 -109.05(10) . . . . ? C3 Mn C20 C21 57.00(13) . . . . ? C1 Mn C20 C21 173.68(7) . . . . ? C4 Mn C20 C21 95.13(8) . . . . ? C18 Mn C20 C21 -73.34(7) . . . . ? C5 Mn C20 C21 135.24(7) . . . . ? C22 Mn C20 C21 -34.86(7) . . . . ? C2 Mn C20 C31 75.4(3) . . . . ? C19 Mn C20 C31 121.35(13) . . . . ? C3 Mn C20 C31 -72.60(14) . . . . ? C1 Mn C20 C31 44.08(13) . . . . ? C4 Mn C20 C31 -34.47(12) . . . . ? C18 Mn C20 C31 157.06(11) . . . . ? C21 Mn C20 C31 -129.60(14) . . . . ? C5 Mn C20 C31 5.63(12) . . . . ? C22 Mn C20 C31 -164.46(12) . . . . ? C19 C20 C21 C26 172.55(12) . . . . ? C31 C20 C21 C26 7.3(2) . . . . ? Mn C20 C21 C26 -118.29(13) . . . . ? C19 C20 C21 C22 -3.42(13) . . . . ? C31 C20 C21 C22 -168.65(11) . . . . ? Mn C20 C21 C22 65.74(8) . . . . ? C19 C20 C21 Mn -69.16(8) . . . . ? C31 C20 C21 Mn 125.60(13) . . . . ? C20 Mn C21 C26 124.81(14) . . . . ? C2 Mn C21 C26 -66.07(16) . . . . ? C19 Mn C21 C26 167.21(13) . . . . ? C3 Mn C21 C26 -27.30(13) . . . . ? C1 Mn C21 C26 98.6(2) . . . . ? C4 Mn C21 C26 15.16(12) . . . . ? C18 Mn C21 C26 -151.59(12) . . . . ? C5 Mn C21 C26 54.08(13) . . . . ? C22 Mn C21 C26 -117.36(13) . . . . ? C2 Mn C21 C20 169.12(10) . . . . ? C19 Mn C21 C20 42.40(7) . . . . ? C3 Mn C21 C20 -152.11(7) . . . . ? C1 Mn C21 C20 -26.2(3) . . . . ? C4 Mn C21 C20 -109.64(8) . . . . ? C18 Mn C21 C20 83.61(8) . . . . ? C5 Mn C21 C20 -70.72(9) . . . . ? C22 Mn C21 C20 117.83(10) . . . . ? C20 Mn C21 C22 -117.83(10) . . . . ? C2 Mn C21 C22 51.29(13) . . . . ? C19 Mn C21 C22 -75.43(7) . . . . ? C3 Mn C21 C22 90.05(8) . . . . ? C1 Mn C21 C22 -144.1(2) . . . . ? C4 Mn C21 C22 132.52(7) . . . . ? C18 Mn C21 C22 -34.23(7) . . . . ? C5 Mn C21 C22 171.44(7) . . . . ? C19 C18 C22 C23 -177.14(12) . . . . ? C27 C18 C22 C23 -4.7(2) . . . . ? Mn C18 C22 C23 123.83(13) . . . . ? C19 C18 C22 C21 0.54(13) . . . . ? C27 C18 C22 C21 172.95(11) . . . . ? Mn C18 C22 C21 -58.49(8) . . . . ? C19 C18 C22 Mn 59.04(8) . . . . ? C27 C18 C22 Mn -128.55(12) . . . . ? C26 C21 C22 C23 3.27(16) . . . . ? C20 C21 C22 C23 179.88(10) . . . . ? Mn C21 C22 C23 -123.47(10) . . . . ? C26 C21 C22 C18 -174.77(10) . . . . ? C20 C21 C22 C18 1.84(13) . . . . ? Mn C21 C22 C18 58.49(8) . . . . ? C26 C21 C22 Mn 126.74(10) . . . . ? C20 C21 C22 Mn -56.65(8) . . . . ? C20 Mn C22 C23 148.41(13) . . . . ? C2 Mn C22 C23 -43.64(13) . . . . ? C19 Mn C22 C23 -167.04(13) . . . . ? C3 Mn C22 C23 -0.43(13) . . . . ? C1 Mn C22 C23 -82.27(14) . . . . ? C4 Mn C22 C23 38.44(14) . . . . ? C18 Mn C22 C23 -128.48(14) . . . . ? C21 Mn C22 C23 111.41(14) . . . . ? C5 Mn C22 C23 72.7(3) . . . . ? C20 Mn C22 C18 -83.11(8) . . . . ? C2 Mn C22 C18 84.85(8) . . . . ? C19 Mn C22 C18 -38.56(7) . . . . ? C3 Mn C22 C18 128.05(7) . . . . ? C1 Mn C22 C18 46.21(12) . . . . ? C4 Mn C22 C18 166.93(7) . . . . ? C21 Mn C22 C18 -120.10(10) . . . . ? C5 Mn C22 C18 -158.8(2) . . . . ? C20 Mn C22 C21 36.99(7) . . . . ? C2 Mn C22 C21 -155.05(7) . . . . ? C19 Mn C22 C21 81.54(8) . . . . ? C3 Mn C22 C21 -111.85(7) . . . . ? C1 Mn C22 C21 166.32(9) . . . . ? C4 Mn C22 C21 -72.97(9) . . . . ? C18 Mn C22 C21 120.10(10) . . . . ? C5 Mn C22 C21 -38.7(3) . . . . ? C18 C22 C23 C24 174.20(12) . . . . ? C21 C22 C23 C24 -3.28(17) . . . . ? Mn C22 C23 C24 -89.10(14) . . . . ? C22 C23 C24 C25 0.84(18) . . . . ? C23 C24 C25 C26 1.72(19) . . . . ? C24 C25 C26 C21 -1.68(18) . . . . ? C20 C21 C26 C25 -176.44(12) . . . . ? C22 C21 C26 C25 -0.81(17) . . . . ? Mn C21 C26 C25 96.45(13) . . . . ? C19 C18 C27 C28 -5.40(18) . . . . ? C22 C18 C27 C28 -176.30(12) . . . . ? Mn C18 C27 C28 78.95(13) . . . . ? C19 C18 C27 C29 -125.91(13) . . . . ? C22 C18 C27 C29 63.19(16) . . . . ? Mn C18 C27 C29 -41.57(15) . . . . ? C19 C18 C27 C30 113.40(14) . . . . ? C22 C18 C27 C30 -57.50(16) . . . . ? Mn C18 C27 C30 -162.26(9) . . . . ? C19 C20 C31 C33 24.67(16) . . . . ? C21 C20 C31 C33 -172.90(11) . . . . ? Mn C20 C31 C33 -66.62(13) . . . . ? C19 C20 C31 C34 144.70(12) . . . . ? C21 C20 C31 C34 -52.86(16) . . . . ? Mn C20 C31 C34 53.42(13) . . . . ? C19 C20 C31 C32 -94.63(14) . . . . ? C21 C20 C31 C32 67.81(15) . . . . ? Mn C20 C31 C32 174.08(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 72.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.267 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.038 _iucr_refine_instructions_details ; TITL mima14 in P2(1)/c CELL 1.54184 17.9709 9.6949 18.0377 90.000 114.575 90.000 ZERR 4.00 0.0004 0.0002 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H MN UNIT 136 184 4 SIZE 0.11 0.05 0.03 TEMP -173 ACTA 145 CONF FMAP 2 PLAN 10 L.S. 8 OMIT -7 3 6 OMIT -8 2 3 OMIT 1 2 2 WGHT 0.046600 0.281800 FVAR 4.10809 MN 3 0.736485 0.335692 0.516236 11.00000 0.02349 0.02480 = 0.01620 0.00059 0.00612 -0.00097 C1 1 0.744162 0.461503 0.402609 11.00000 0.02561 0.02012 = 0.01914 0.00044 0.00838 -0.00331 C2 1 0.710403 0.327209 0.380950 11.00000 0.02372 0.02008 = 0.01718 -0.00001 0.00914 -0.00094 H2 2 0.734829 0.255215 0.362863 11.00000 0.02237 C3 1 0.633927 0.315232 0.387111 11.00000 0.02231 0.01862 = 0.01685 0.00009 0.00754 -0.00063 C4 1 0.617288 0.450253 0.409978 11.00000 0.02491 0.01964 = 0.01621 0.00166 0.00710 0.00139 C5 1 0.685370 0.540263 0.419760 11.00000 0.02869 0.01928 = 0.01701 0.00076 0.00777 -0.00186 C6 1 0.681931 0.681018 0.440904 11.00000 0.03700 0.01964 = 0.02109 0.00100 0.00835 -0.00274 AFIX 43 H6 2 0.726367 0.741119 0.448853 11.00000 -1.20000 AFIX 0 C7 1 0.614452 0.729616 0.449761 11.00000 0.04630 0.01978 = 0.02088 0.00082 0.00979 0.00684 AFIX 43 H7 2 0.612328 0.823956 0.462990 11.00000 -1.20000 AFIX 0 C8 1 0.548189 0.642435 0.439636 11.00000 0.03446 0.02888 = 0.02086 0.00203 0.00990 0.01055 AFIX 43 H8 2 0.502095 0.679118 0.445854 11.00000 -1.20000 AFIX 0 C9 1 0.549111 0.505227 0.420918 11.00000 0.02600 0.02791 = 0.01996 0.00216 0.00741 0.00454 AFIX 43 H9 2 0.504430 0.447323 0.415304 11.00000 -1.20000 AFIX 0 C10 1 0.821910 0.514862 0.397485 11.00000 0.02823 0.02770 = 0.02463 0.00102 0.01153 -0.00852 C11 1 0.882690 0.573233 0.480090 11.00000 0.03112 0.03420 = 0.02746 -0.00005 0.01124 -0.01194 AFIX 137 H11A 2 0.856431 0.647852 0.497088 11.00000 -1.20000 H11B 2 0.931089 0.609129 0.474519 11.00000 -1.20000 H11C 2 0.899163 0.499800 0.521139 11.00000 -1.20000 AFIX 0 C12 1 0.864362 0.399631 0.371667 11.00000 0.03120 0.03832 = 0.03541 -0.00277 0.01914 -0.00905 AFIX 137 H12A 2 0.878698 0.324342 0.411454 11.00000 -1.20000 H12B 2 0.914187 0.435812 0.369167 11.00000 -1.20000 H12C 2 0.827385 0.364954 0.317850 11.00000 -1.20000 AFIX 0 C13 1 0.799182 0.630083 0.333368 11.00000 0.04135 0.03506 = 0.02829 0.00463 0.01393 -0.01224 AFIX 137 H13A 2 0.762920 0.592981 0.279941 11.00000 -1.20000 H13B 2 0.849001 0.666347 0.330891 11.00000 -1.20000 H13C 2 0.771126 0.704435 0.348363 11.00000 -1.20000 AFIX 0 C14 1 0.576329 0.191635 0.361891 11.00000 0.02210 0.02140 = 0.01880 -0.00047 0.00729 -0.00268 C15 1 0.500308 0.226128 0.283589 11.00000 0.02980 0.03150 = 0.02104 -0.00079 0.00330 -0.00516 AFIX 137 H15A 2 0.471529 0.304709 0.293757 11.00000 -1.20000 H15B 2 0.463755 0.146034 0.267119 11.00000 -1.20000 H15C 2 0.517226 0.249609 0.240027 11.00000 -1.20000 AFIX 0 C16 1 0.618763 0.066172 0.345266 11.00000 0.03151 0.02003 = 0.03105 -0.00412 0.01517 -0.00552 AFIX 137 H16A 2 0.633963 0.086872 0.300199 11.00000 -1.20000 H16B 2 0.581434 -0.012921 0.330679 11.00000 -1.20000 H16C 2 0.668070 0.044206 0.394273 11.00000 -1.20000 AFIX 0 C17 1 0.549769 0.152933 0.430162 11.00000 0.02642 0.02779 = 0.02498 -0.00013 0.01173 -0.00547 AFIX 137 H17A 2 0.598348 0.134645 0.480586 11.00000 -1.20000 H17B 2 0.515364 0.070196 0.414289 11.00000 -1.20000 H17C 2 0.518700 0.229341 0.439033 11.00000 -1.20000 AFIX 0 C18 1 0.842107 0.176780 0.613342 11.00000 0.01988 0.02111 = 0.02003 0.00168 0.00665 -0.00031 C19 1 0.851178 0.317764 0.636229 11.00000 0.01899 0.02157 = 0.01981 0.00180 0.00537 -0.00300 H19 2 0.896787 0.372696 0.640628 11.00000 0.02731 C20 1 0.784454 0.365608 0.653216 11.00000 0.02285 0.01934 = 0.01690 0.00109 0.00643 -0.00112 C21 1 0.734316 0.245611 0.645686 11.00000 0.01982 0.01970 = 0.01578 0.00061 0.00492 -0.00065 C22 1 0.768949 0.130351 0.619607 11.00000 0.02005 0.01994 = 0.01757 0.00110 0.00565 -0.00022 C23 1 0.730248 -0.000554 0.607933 11.00000 0.02314 0.01851 = 0.02250 -0.00025 0.00754 -0.00027 AFIX 43 H23 2 0.750567 -0.075869 0.588134 11.00000 -1.20000 AFIX 0 C24 1 0.663338 -0.017948 0.625356 11.00000 0.02375 0.02114 = 0.02346 0.00057 0.00768 -0.00431 AFIX 43 H24 2 0.638095 -0.106009 0.618146 11.00000 -1.20000 AFIX 0 C25 1 0.631540 0.093060 0.653810 11.00000 0.02273 0.02771 = 0.02357 -0.00027 0.01052 -0.00396 AFIX 43 H25 2 0.586143 0.077880 0.666866 11.00000 -1.20000 AFIX 0 C26 1 0.665051 0.222492 0.662940 11.00000 0.02248 0.02445 = 0.02057 -0.00077 0.00904 0.00019 AFIX 43 H26 2 0.641971 0.296582 0.680778 11.00000 -1.20000 AFIX 0 C27 1 0.903514 0.087963 0.596883 11.00000 0.02283 0.02312 = 0.03316 0.00262 0.01251 0.00255 C28 1 0.975902 0.175424 0.600409 11.00000 0.02516 0.03299 = 0.04214 0.00709 0.01749 0.00289 AFIX 137 H28A 2 0.956122 0.247810 0.558792 11.00000 -1.20000 H28B 2 1.015041 0.116620 0.590256 11.00000 -1.20000 H28C 2 1.002856 0.217797 0.654434 11.00000 -1.20000 AFIX 0 C29 1 0.864093 0.019298 0.512591 11.00000 0.03450 0.03128 = 0.04085 -0.00492 0.02156 0.00410 AFIX 137 H29A 2 0.816336 -0.034388 0.508515 11.00000 -1.20000 H29B 2 0.903910 -0.041995 0.505318 11.00000 -1.20000 H29C 2 0.846890 0.090481 0.470177 11.00000 -1.20000 AFIX 0 C30 1 0.936305 -0.024230 0.663259 11.00000 0.02471 0.02980 = 0.04790 0.01157 0.01408 0.00574 AFIX 137 H30A 2 0.960686 0.019479 0.717087 11.00000 -1.20000 H30B 2 0.977890 -0.079236 0.654836 11.00000 -1.20000 H30C 2 0.891182 -0.084248 0.660046 11.00000 -1.20000 AFIX 0 C31 1 0.781173 0.503544 0.692386 11.00000 0.02748 0.01848 = 0.01886 0.00011 0.00776 -0.00129 C32 1 0.810609 0.480018 0.784774 11.00000 0.03368 0.02201 = 0.01944 -0.00095 0.00881 -0.00291 AFIX 137 H32A 2 0.774401 0.413685 0.794358 11.00000 -1.20000 H32B 2 0.809568 0.567675 0.811383 11.00000 -1.20000 H32C 2 0.866573 0.443735 0.807321 11.00000 -1.20000 AFIX 0 C33 1 0.837342 0.609515 0.678243 11.00000 0.03952 0.02083 = 0.02696 -0.00246 0.01457 -0.00620 AFIX 137 H33A 2 0.893826 0.575605 0.702343 11.00000 -1.20000 H33B 2 0.834258 0.697264 0.703792 11.00000 -1.20000 H33C 2 0.819821 0.623371 0.619560 11.00000 -1.20000 AFIX 0 C34 1 0.694430 0.565116 0.657688 11.00000 0.03459 0.02245 = 0.02762 0.00055 0.00944 0.00416 AFIX 137 H34A 2 0.675353 0.579136 0.598829 11.00000 -1.20000 H34B 2 0.695342 0.653781 0.684144 11.00000 -1.20000 H34C 2 0.657336 0.501654 0.667985 11.00000 -1.20000 HKLF 4 ; # Attachment '- mima17.cif' data_mima17 _database_code_depnum_ccdc_archive 'CCDC 884308' #TrackingRef '- mima17.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H54 Mn' _chemical_formula_weight 613.79 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3587(6) _cell_length_b 15.8419(6) _cell_length_c 16.6359(6) _cell_angle_alpha 99.248(4) _cell_angle_beta 92.509(2) _cell_angle_gamma 101.347(4) _cell_volume 3396.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19819 _cell_measurement_theta_min 3.3765 _cell_measurement_theta_max 75.6770 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 3.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97123 _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 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35598 _diffrn_reflns_av_R_equivalents 0.0869 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 76.19 _reflns_number_total 13623 _reflns_number_gt 10618 _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. ; _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^)+(0.1310P)^2^+3.2535P] 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 13623 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.2185 _refine_ls_wR_factor_gt 0.2008 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Mn Mn 0.21118(4) 0.41953(3) 0.30498(3) 0.02774(15) Uani 1 1 d . . . C1 C 0.1735(3) 0.2875(2) 0.21358(19) 0.0276(6) Uani 1 1 d . . . C2 C 0.2428(3) 0.2820(2) 0.2792(2) 0.0263(6) Uani 1 1 d . . . H2 H 0.3116 0.2758 0.2738 0.032 Uiso 1 1 calc R . . C3 C 0.1950(3) 0.2872(2) 0.3539(2) 0.0265(6) Uani 1 1 d . . . C4 C 0.0915(3) 0.2928(2) 0.33461(19) 0.0258(6) Uani 1 1 d . . . C5 C 0.0777(3) 0.2916(2) 0.2474(2) 0.0281(7) Uani 1 1 d . . . C6 C -0.0203(3) 0.2936(2) 0.2125(2) 0.0323(7) Uani 1 1 d . . . H6 H -0.0312 0.2923 0.1555 0.039 Uiso 1 1 calc R . . C7 C -0.0994(3) 0.2975(3) 0.2624(3) 0.0382(8) Uani 1 1 d . . . H7 H -0.1652 0.2983 0.2389 0.046 Uiso 1 1 calc R . . C8 C -0.0854(3) 0.3002(3) 0.3481(3) 0.0387(8) Uani 1 1 d . . . H8 H -0.1415 0.3035 0.3808 0.046 Uiso 1 1 calc R . . C9 C 0.0077(3) 0.2983(2) 0.3838(2) 0.0325(7) Uani 1 1 d . . . H9 H 0.0166 0.3007 0.4411 0.039 Uiso 1 1 calc R . . C10 C 0.1602(2) 0.5526(2) 0.33961(19) 0.0250(6) Uani 1 1 d . . . C11 C 0.2377(2) 0.5591(2) 0.28248(19) 0.0249(6) Uani 1 1 d . . . H11 H 0.2270 0.5673 0.2277 0.030 Uiso 1 1 calc R . . C12 C 0.3327(3) 0.5515(2) 0.3193(2) 0.0261(6) Uani 1 1 d . . . C13 C 0.3167(3) 0.5446(2) 0.4034(2) 0.0282(7) Uani 1 1 d . . . C14 C 0.2102(3) 0.5446(2) 0.4153(2) 0.0276(6) Uani 1 1 d . . . C15 C 0.1741(3) 0.5392(2) 0.4938(2) 0.0318(7) Uani 1 1 d . . . H15 H 0.1041 0.5382 0.5025 0.038 Uiso 1 1 calc R . . C17 C 0.3457(3) 0.5353(3) 0.5449(2) 0.0354(8) Uani 1 1 d . . . H17 H 0.3903 0.5330 0.5902 0.042 Uiso 1 1 calc R . . C16 C 0.2414(3) 0.5354(3) 0.5564(2) 0.0367(8) Uani 1 1 d . . . H16 H 0.2177 0.5327 0.6091 0.044 Uiso 1 1 calc R . . C18 C 0.3843(3) 0.5385(2) 0.4700(2) 0.0301(7) Uani 1 1 d . . . H18 H 0.4541 0.5367 0.4628 0.036 Uiso 1 1 calc R . . C19 C 0.2006(3) 0.2807(2) 0.1252(2) 0.0291(7) Uani 1 1 d . . . H19 H 0.2768 0.2884 0.1264 0.035 Uiso 1 1 calc R . . C20 C 0.1563(3) 0.1896(2) 0.0756(2) 0.0314(7) Uani 1 1 d . . . H20A H 0.1801 0.1451 0.1028 0.038 Uiso 1 1 calc R . . H20B H 0.0806 0.1783 0.0744 0.038 Uiso 1 1 calc R . . C21 C 0.1884(3) 0.1810(3) -0.0118(2) 0.0372(8) Uani 1 1 d . . . H21A H 0.2632 0.1840 -0.0108 0.045 Uiso 1 1 calc R . . H21B H 0.1537 0.1232 -0.0428 0.045 Uiso 1 1 calc R . . C22 C 0.1620(3) 0.2523(3) -0.0551(2) 0.0386(8) Uani 1 1 d . . . H22A H 0.0867 0.2444 -0.0633 0.046 Uiso 1 1 calc R . . H22B H 0.1898 0.2475 -0.1095 0.046 Uiso 1 1 calc R . . C23 C 0.2067(3) 0.3428(3) -0.0051(2) 0.0375(8) Uani 1 1 d . . . H23A H 0.1843 0.3878 -0.0325 0.045 Uiso 1 1 calc R . . H23B H 0.2824 0.3534 -0.0030 0.045 Uiso 1 1 calc R . . C24 C 0.1727(3) 0.3516(2) 0.0821(2) 0.0322(7) Uani 1 1 d . . . H24A H 0.2060 0.4097 0.1133 0.039 Uiso 1 1 calc R . . H24B H 0.0977 0.3473 0.0804 0.039 Uiso 1 1 calc R . . C25 C 0.2407(3) 0.2804(2) 0.43694(19) 0.0263(6) Uani 1 1 d . . . H25 H 0.2202 0.3257 0.4784 0.032 Uiso 1 1 calc R . . C26 C 0.1971(3) 0.1897(2) 0.4588(2) 0.0324(7) Uani 1 1 d . . . H26A H 0.1217 0.1812 0.4591 0.039 Uiso 1 1 calc R . . H26B H 0.2129 0.1435 0.4167 0.039 Uiso 1 1 calc R . . C27 C 0.2423(3) 0.1808(3) 0.5429(2) 0.0350(8) Uani 1 1 d . . . H27A H 0.2199 0.2225 0.5857 0.042 Uiso 1 1 calc R . . H27B H 0.2159 0.1210 0.5535 0.042 Uiso 1 1 calc R . . C28 C 0.3582(3) 0.1984(2) 0.5475(2) 0.0345(7) Uani 1 1 d . . . H28A H 0.3806 0.1523 0.5092 0.041 Uiso 1 1 calc R . . H28B H 0.3847 0.1961 0.6034 0.041 Uiso 1 1 calc R . . C29 C 0.4025(3) 0.2876(2) 0.5259(2) 0.0343(7) Uani 1 1 d . . . H29A H 0.4778 0.2953 0.5257 0.041 Uiso 1 1 calc R . . H29B H 0.3872 0.3340 0.5681 0.041 Uiso 1 1 calc R . . C30 C 0.3579(3) 0.2967(2) 0.4425(2) 0.0289(7) Uani 1 1 d . . . H30A H 0.3799 0.2546 0.3997 0.035 Uiso 1 1 calc R . . H30B H 0.3854 0.3563 0.4319 0.035 Uiso 1 1 calc R . . C31 C 0.0510(3) 0.5646(2) 0.3303(2) 0.0279(6) Uani 1 1 d . . . H31 H 0.0094 0.5256 0.3636 0.033 Uiso 1 1 calc R . . C32 C 0.0028(3) 0.5388(2) 0.2423(2) 0.0321(7) Uani 1 1 d . . . H32A H 0.0017 0.4762 0.2226 0.038 Uiso 1 1 calc R . . H32B H 0.0451 0.5733 0.2067 0.038 Uiso 1 1 calc R . . C33 C -0.1070(3) 0.5548(3) 0.2363(2) 0.0408(9) Uani 1 1 d . . . H33A H -0.1339 0.5421 0.1783 0.049 Uiso 1 1 calc R . . H33B H -0.1515 0.5144 0.2659 0.049 Uiso 1 1 calc R . . C34 C -0.1108(3) 0.6492(3) 0.2726(3) 0.0489(10) Uani 1 1 d . . . H34A H -0.0725 0.6893 0.2393 0.059 Uiso 1 1 calc R . . H34B H -0.1828 0.6563 0.2705 0.059 Uiso 1 1 calc R . . C35 C -0.0650(3) 0.6737(3) 0.3602(3) 0.0446(9) Uani 1 1 d . . . H35A H -0.1072 0.6378 0.3948 0.054 Uiso 1 1 calc R . . H35B H -0.0648 0.7359 0.3809 0.054 Uiso 1 1 calc R . . C36 C 0.0445(3) 0.6586(2) 0.3653(2) 0.0350(8) Uani 1 1 d . . . H36A H 0.0721 0.6725 0.4232 0.042 Uiso 1 1 calc R . . H36B H 0.0877 0.6990 0.3351 0.042 Uiso 1 1 calc R . . C37 C 0.4348(3) 0.5582(2) 0.2821(2) 0.0298(7) Uani 1 1 d . . . H37 H 0.4848 0.5460 0.3231 0.036 Uiso 1 1 calc R . . C38 C 0.4322(3) 0.4914(3) 0.2033(2) 0.0391(8) Uani 1 1 d . . . H38A H 0.4094 0.4316 0.2149 0.047 Uiso 1 1 calc R . . H38B H 0.3821 0.5010 0.1618 0.047 Uiso 1 1 calc R . . C39 C 0.5377(3) 0.5000(3) 0.1695(3) 0.0462(10) Uani 1 1 d . . . H39A H 0.5860 0.4846 0.2089 0.055 Uiso 1 1 calc R . . H39B H 0.5329 0.4582 0.1177 0.055 Uiso 1 1 calc R . . C40 C 0.5795(3) 0.5924(3) 0.1542(3) 0.0438(9) Uani 1 1 d . . . H40A H 0.6497 0.5962 0.1363 0.053 Uiso 1 1 calc R . . H40B H 0.5361 0.6053 0.1099 0.053 Uiso 1 1 calc R . . C41 C 0.5816(3) 0.6594(3) 0.2307(2) 0.0371(8) Uani 1 1 d . . . H41A H 0.6031 0.7189 0.2178 0.045 Uiso 1 1 calc R . . H41B H 0.6323 0.6515 0.2725 0.045 Uiso 1 1 calc R . . C42 C 0.4758(3) 0.6505(2) 0.2649(2) 0.0303(7) Uani 1 1 d . . . H42A H 0.4806 0.6931 0.3162 0.036 Uiso 1 1 calc R . . H42B H 0.4270 0.6647 0.2253 0.036 Uiso 1 1 calc R . . Mn' Mn 0.30311(4) -0.07911(3) 0.21094(3) 0.02797(15) Uani 1 1 d . . . C1' C 0.3725(3) -0.1609(2) 0.29859(19) 0.0278(7) Uani 1 1 d . . . C2' C 0.2918(3) -0.2138(2) 0.24283(19) 0.0266(6) Uani 1 1 d . . . H2' H 0.2274 -0.2415 0.2579 0.032 Uiso 1 1 calc R . . C3' C 0.3219(2) -0.2193(2) 0.16074(19) 0.0245(6) Uani 1 1 d . . . C4' C 0.4255(2) -0.1713(2) 0.16640(19) 0.0249(6) Uani 1 1 d . . . C5' C 0.4564(3) -0.1352(2) 0.25107(19) 0.0267(6) Uani 1 1 d . . . C6' C 0.5561(3) -0.0837(2) 0.2733(2) 0.0311(7) Uani 1 1 d . . . H6' H 0.5769 -0.0588 0.3288 0.037 Uiso 1 1 calc R . . C7' C 0.6220(3) -0.0703(2) 0.2135(2) 0.0357(8) Uani 1 1 d . . . H7' H 0.6891 -0.0362 0.2282 0.043 Uiso 1 1 calc R . . C8' C 0.5923(3) -0.1061(2) 0.1306(2) 0.0331(7) Uani 1 1 d . . . H8' H 0.6399 -0.0960 0.0907 0.040 Uiso 1 1 calc R . . C9' C 0.4961(3) -0.1551(2) 0.1066(2) 0.0291(7) Uani 1 1 d . . . H9' H 0.4769 -0.1779 0.0505 0.035 Uiso 1 1 calc R . . C10' C 0.3445(3) 0.0516(2) 0.1638(2) 0.0266(6) Uani 1 1 d . . . C11' C 0.2662(3) 0.0535(2) 0.2196(2) 0.0294(7) Uani 1 1 d . . . H11' H 0.2753 0.0874 0.2729 0.035 Uiso 1 1 calc R . . C12' C 0.1724(3) -0.0029(2) 0.1837(2) 0.0326(7) Uani 1 1 d . . . C13' C 0.1899(3) -0.0355(2) 0.1017(2) 0.0300(7) Uani 1 1 d . . . C14' C 0.2965(3) -0.0032(2) 0.0900(2) 0.0267(6) Uani 1 1 d . . . C15' C 0.3338(3) -0.0277(2) 0.0132(2) 0.0298(7) Uani 1 1 d . . . H15' H 0.4042 -0.0093 0.0053 0.036 Uiso 1 1 calc R . . C16' C 0.2677(3) -0.0781(2) -0.0497(2) 0.0341(7) Uani 1 1 d . . . H16' H 0.2928 -0.0932 -0.1015 0.041 Uiso 1 1 calc R . . C17' C 0.1625(3) -0.1081(2) -0.0389(2) 0.0364(8) Uani 1 1 d . . . H17' H 0.1179 -0.1417 -0.0837 0.044 Uiso 1 1 calc R . . C18' C 0.1247(3) -0.0889(2) 0.0358(2) 0.0344(7) Uani 1 1 d . . . H18' H 0.0550 -0.1113 0.0432 0.041 Uiso 1 1 calc R . . C19' C 0.3752(3) -0.1427(2) 0.3909(2) 0.0295(7) Uani 1 1 d . . . H19' H 0.4489 -0.1292 0.4119 0.035 Uiso 1 1 calc R . . C20' C 0.3240(3) -0.2219(2) 0.4245(2) 0.0386(8) Uani 1 1 d . . . H20C H 0.3571 -0.2714 0.4052 0.046 Uiso 1 1 calc R . . H20D H 0.2512 -0.2386 0.4032 0.046 Uiso 1 1 calc R . . C21' C 0.3302(3) -0.2055(2) 0.5178(2) 0.0386(9) Uani 1 1 d . . . H21C H 0.2920 -0.2578 0.5369 0.046 Uiso 1 1 calc R . . H21D H 0.4026 -0.1956 0.5392 0.046 Uiso 1 1 calc R . . C22' C 0.2861(3) -0.1272(3) 0.5509(2) 0.0412(9) Uani 1 1 d . . . H22C H 0.2956 -0.1157 0.6114 0.049 Uiso 1 1 calc R . . H22D H 0.2118 -0.1396 0.5349 0.049 Uiso 1 1 calc R . . C23' C 0.3386(5) -0.0472(3) 0.5182(2) 0.0539(12) Uani 1 1 d . . . H23C H 0.4116 -0.0314 0.5391 0.065 Uiso 1 1 calc R . . H23D H 0.3063 0.0026 0.5380 0.065 Uiso 1 1 calc R . . C24' C 0.3312(5) -0.0640(3) 0.4242(3) 0.0539(12) Uani 1 1 d . . . H24C H 0.2585 -0.0740 0.4033 0.065 Uiso 1 1 calc R . . H24D H 0.3690 -0.0117 0.4048 0.065 Uiso 1 1 calc R . . C25' C 0.2613(3) -0.2707(2) 0.08399(19) 0.0270(6) Uani 1 1 d . . . H25' H 0.2673 -0.2320 0.0418 0.032 Uiso 1 1 calc R . . C26' C 0.3017(3) -0.3521(2) 0.0498(2) 0.0310(7) Uani 1 1 d . . . H26C H 0.3739 -0.3342 0.0376 0.037 Uiso 1 1 calc R . . H26D H 0.2999 -0.3902 0.0917 0.037 Uiso 1 1 calc R . . C27' C 0.2389(3) -0.4038(3) -0.0279(2) 0.0415(9) Uani 1 1 d . . . H27C H 0.2453 -0.3677 -0.0715 0.050 Uiso 1 1 calc R . . H27D H 0.2656 -0.4570 -0.0468 0.050 Uiso 1 1 calc R . . C28' C 0.1264(3) -0.4297(3) -0.0117(2) 0.0414(9) Uani 1 1 d . . . H28C H 0.0863 -0.4604 -0.0631 0.050 Uiso 1 1 calc R . . H28D H 0.1194 -0.4705 0.0280 0.050 Uiso 1 1 calc R . . C29' C 0.0843(3) -0.3501(3) 0.0218(2) 0.0366(8) Uani 1 1 d . . . H29C H 0.0128 -0.3692 0.0351 0.044 Uiso 1 1 calc R . . H29D H 0.0837 -0.3130 -0.0206 0.044 Uiso 1 1 calc R . . C30' C 0.1474(3) -0.2967(2) 0.0979(2) 0.0307(7) Uani 1 1 d . . . H30C H 0.1399 -0.3311 0.1428 0.037 Uiso 1 1 calc R . . H30D H 0.1205 -0.2431 0.1150 0.037 Uiso 1 1 calc R . . C31' C 0.4510(2) 0.1083(2) 0.17150(19) 0.0259(6) Uani 1 1 d . . . H31' H 0.4976 0.0722 0.1445 0.031 Uiso 1 1 calc R . . C32' C 0.4943(3) 0.1431(2) 0.2601(2) 0.0328(7) Uani 1 1 d . . . H32C H 0.4455 0.1740 0.2895 0.039 Uiso 1 1 calc R . . H32D H 0.5018 0.0934 0.2874 0.039 Uiso 1 1 calc R . . C33' C 0.5981(3) 0.2056(3) 0.2651(2) 0.0351(8) Uani 1 1 d . . . H33C H 0.6213 0.2291 0.3232 0.042 Uiso 1 1 calc R . . H33D H 0.6490 0.1731 0.2413 0.042 Uiso 1 1 calc R . . C34' C 0.5925(3) 0.2810(2) 0.2198(2) 0.0346(7) Uani 1 1 d . . . H34C H 0.6614 0.3191 0.2226 0.041 Uiso 1 1 calc R . . H34D H 0.5460 0.3165 0.2465 0.041 Uiso 1 1 calc R . . C35' C 0.5536(3) 0.2470(2) 0.1306(2) 0.0314(7) Uani 1 1 d . . . H35C H 0.5474 0.2967 0.1029 0.038 Uiso 1 1 calc R . . H35D H 0.6032 0.2159 0.1026 0.038 Uiso 1 1 calc R . . C36' C 0.4497(3) 0.1850(2) 0.1254(2) 0.0284(7) Uani 1 1 d . . . H36C H 0.4272 0.1614 0.0672 0.034 Uiso 1 1 calc R . . H36D H 0.3990 0.2184 0.1481 0.034 Uiso 1 1 calc R . . C37' C 0.0684(3) -0.0181(3) 0.2182(3) 0.0388(8) Uani 1 1 d . . . H37' H 0.0217 -0.0646 0.1783 0.047 Uiso 1 1 calc R . . C38' C 0.0718(4) -0.0514(4) 0.3002(3) 0.0533(11) Uani 1 1 d . . . H38C H 0.0989 -0.1057 0.2929 0.064 Uiso 1 1 calc R . . H38D H 0.1186 -0.0072 0.3410 0.064 Uiso 1 1 calc R . . C39' C -0.0350(4) -0.0695(4) 0.3319(4) 0.0601(14) Uani 1 1 d . . . H39C H -0.0797 -0.1186 0.2944 0.072 Uiso 1 1 calc R . . H39D H -0.0299 -0.0868 0.3863 0.072 Uiso 1 1 calc R . . C40' C -0.0826(4) 0.0116(4) 0.3385(3) 0.0568(12) Uani 1 1 d . . . H40C H -0.1539 -0.0038 0.3536 0.068 Uiso 1 1 calc R . . H40D H -0.0438 0.0573 0.3827 0.068 Uiso 1 1 calc R . . C41' C -0.0826(4) 0.0468(3) 0.2624(4) 0.0576(13) Uani 1 1 d . . . H41C H -0.1056 0.1030 0.2724 0.069 Uiso 1 1 calc R . . H41D H -0.1325 0.0058 0.2213 0.069 Uiso 1 1 calc R . . C42' C 0.0226(3) 0.0616(3) 0.2275(3) 0.0471(10) Uani 1 1 d . . . H42C H 0.0156 0.0794 0.1735 0.057 Uiso 1 1 calc R . . H42D H 0.0696 0.1100 0.2641 0.057 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 Mn 0.0326(3) 0.0251(3) 0.0260(3) 0.00531(19) 0.0060(2) 0.0058(2) C1 0.0324(17) 0.0279(16) 0.0233(15) 0.0057(12) 0.0041(12) 0.0068(12) C2 0.0276(16) 0.0248(15) 0.0280(16) 0.0064(12) 0.0069(12) 0.0062(12) C3 0.0292(16) 0.0250(15) 0.0251(15) 0.0034(11) 0.0070(12) 0.0047(12) C4 0.0274(16) 0.0250(15) 0.0251(15) 0.0047(11) 0.0056(12) 0.0046(12) C5 0.0310(17) 0.0261(15) 0.0278(16) 0.0072(12) 0.0040(13) 0.0048(12) C6 0.0333(18) 0.0323(17) 0.0316(17) 0.0074(13) 0.0031(14) 0.0056(13) C7 0.0274(17) 0.044(2) 0.045(2) 0.0097(16) 0.0009(15) 0.0085(15) C8 0.0296(18) 0.044(2) 0.044(2) 0.0103(16) 0.0129(15) 0.0065(15) C9 0.0339(18) 0.0371(18) 0.0293(16) 0.0097(13) 0.0103(14) 0.0091(14) C10 0.0274(16) 0.0256(15) 0.0224(14) 0.0063(11) 0.0069(12) 0.0034(12) C11 0.0253(15) 0.0270(15) 0.0253(15) 0.0102(11) 0.0086(12) 0.0066(12) C12 0.0283(16) 0.0250(15) 0.0270(15) 0.0064(11) 0.0077(12) 0.0076(12) C13 0.0342(17) 0.0250(15) 0.0278(16) 0.0080(12) 0.0114(13) 0.0070(12) C14 0.0324(17) 0.0233(15) 0.0276(16) 0.0052(11) 0.0071(13) 0.0055(12) C15 0.0323(17) 0.0357(18) 0.0287(17) 0.0079(13) 0.0121(13) 0.0057(14) C17 0.042(2) 0.0382(19) 0.0270(17) 0.0077(13) -0.0006(14) 0.0093(15) C16 0.046(2) 0.0390(19) 0.0266(17) 0.0079(14) 0.0100(15) 0.0085(16) C18 0.0312(17) 0.0320(17) 0.0280(16) 0.0086(13) 0.0023(13) 0.0064(13) C19 0.0305(16) 0.0350(17) 0.0226(15) 0.0061(12) 0.0049(12) 0.0073(13) C20 0.0369(18) 0.0337(18) 0.0247(16) 0.0058(13) 0.0022(13) 0.0093(14) C21 0.044(2) 0.045(2) 0.0245(16) 0.0038(14) 0.0066(14) 0.0155(16) C22 0.049(2) 0.047(2) 0.0234(16) 0.0091(14) 0.0057(15) 0.0170(17) C23 0.046(2) 0.042(2) 0.0278(17) 0.0123(14) 0.0086(15) 0.0104(16) C24 0.0317(17) 0.0363(18) 0.0293(17) 0.0066(13) 0.0054(13) 0.0071(14) C25 0.0288(16) 0.0283(16) 0.0221(14) 0.0050(11) 0.0048(12) 0.0055(12) C26 0.0340(18) 0.0347(18) 0.0290(16) 0.0111(13) 0.0054(13) 0.0033(14) C27 0.0358(19) 0.042(2) 0.0320(17) 0.0160(14) 0.0077(14) 0.0096(15) C28 0.0379(19) 0.0360(18) 0.0326(17) 0.0094(14) 0.0020(14) 0.0120(15) C29 0.0350(18) 0.0360(18) 0.0318(17) 0.0072(14) -0.0007(14) 0.0068(14) C30 0.0285(16) 0.0319(17) 0.0261(15) 0.0061(12) 0.0034(12) 0.0046(13) C31 0.0289(16) 0.0310(16) 0.0254(15) 0.0080(12) 0.0081(12) 0.0065(13) C32 0.0313(17) 0.0401(19) 0.0263(16) 0.0062(13) 0.0056(13) 0.0099(14) C33 0.0290(18) 0.060(3) 0.0340(19) 0.0073(17) 0.0041(14) 0.0107(16) C34 0.036(2) 0.064(3) 0.056(3) 0.017(2) 0.0100(18) 0.0243(19) C35 0.035(2) 0.045(2) 0.055(2) 0.0009(18) 0.0093(17) 0.0161(16) C36 0.0279(17) 0.0348(18) 0.043(2) 0.0033(14) 0.0088(14) 0.0086(14) C37 0.0291(17) 0.0347(17) 0.0296(16) 0.0108(13) 0.0091(13) 0.0109(13) C38 0.044(2) 0.0324(18) 0.041(2) 0.0038(15) 0.0175(16) 0.0059(15) C39 0.047(2) 0.042(2) 0.051(2) 0.0037(17) 0.0258(19) 0.0112(17) C40 0.041(2) 0.051(2) 0.044(2) 0.0121(17) 0.0220(17) 0.0112(17) C41 0.0325(18) 0.039(2) 0.043(2) 0.0123(15) 0.0106(15) 0.0078(15) C42 0.0266(16) 0.0316(17) 0.0338(17) 0.0087(13) 0.0067(13) 0.0053(13) Mn' 0.0341(3) 0.0267(3) 0.0249(3) 0.00708(19) 0.0085(2) 0.0072(2) C1' 0.0341(17) 0.0268(15) 0.0232(15) 0.0058(12) 0.0060(13) 0.0058(13) C2' 0.0314(16) 0.0256(15) 0.0238(15) 0.0085(11) 0.0070(12) 0.0042(12) C3' 0.0263(15) 0.0247(15) 0.0230(15) 0.0058(11) 0.0051(12) 0.0046(12) C4' 0.0280(16) 0.0267(15) 0.0220(14) 0.0080(11) 0.0035(12) 0.0070(12) C5' 0.0328(17) 0.0294(16) 0.0182(14) 0.0052(11) 0.0043(12) 0.0056(13) C6' 0.0325(17) 0.0336(17) 0.0264(16) 0.0044(13) -0.0012(13) 0.0061(13) C7' 0.0328(18) 0.0353(18) 0.0387(19) 0.0094(14) 0.0055(15) 0.0038(14) C8' 0.0299(17) 0.0375(18) 0.0345(18) 0.0099(14) 0.0104(14) 0.0081(14) C9' 0.0295(16) 0.0324(17) 0.0272(16) 0.0081(12) 0.0082(13) 0.0071(13) C10' 0.0291(16) 0.0273(15) 0.0258(15) 0.0071(12) 0.0083(12) 0.0084(12) C11' 0.0331(17) 0.0294(16) 0.0293(16) 0.0089(12) 0.0138(13) 0.0093(13) C12' 0.0304(17) 0.0310(17) 0.0393(19) 0.0117(14) 0.0145(14) 0.0064(13) C13' 0.0304(17) 0.0286(16) 0.0338(17) 0.0124(13) 0.0065(13) 0.0063(13) C14' 0.0294(16) 0.0252(15) 0.0276(16) 0.0085(12) 0.0069(13) 0.0068(12) C15' 0.0317(17) 0.0329(17) 0.0259(15) 0.0084(12) 0.0080(13) 0.0057(13) C16' 0.040(2) 0.0343(18) 0.0282(16) 0.0049(13) 0.0057(14) 0.0087(15) C17' 0.040(2) 0.0328(18) 0.0355(18) 0.0081(14) 0.0000(15) 0.0049(15) C18' 0.0296(17) 0.0336(18) 0.0398(19) 0.0099(14) -0.0006(14) 0.0037(14) C19' 0.0320(17) 0.0329(17) 0.0224(15) 0.0065(12) 0.0047(12) 0.0017(13) C20' 0.059(2) 0.0330(18) 0.0225(16) 0.0044(13) 0.0085(15) 0.0044(16) C21' 0.058(2) 0.0344(19) 0.0223(16) 0.0073(13) 0.0113(15) 0.0031(16) C22' 0.048(2) 0.056(2) 0.0237(16) 0.0066(15) 0.0130(15) 0.0185(18) C23' 0.100(4) 0.042(2) 0.0239(18) 0.0035(15) 0.010(2) 0.025(2) C24' 0.102(4) 0.039(2) 0.0281(19) 0.0083(16) 0.017(2) 0.027(2) C25' 0.0318(17) 0.0276(16) 0.0219(14) 0.0080(11) 0.0054(12) 0.0035(12) C26' 0.0328(17) 0.0338(17) 0.0243(15) 0.0029(12) 0.0065(13) 0.0025(13) C27' 0.040(2) 0.042(2) 0.0356(19) -0.0050(15) 0.0073(16) -0.0005(16) C28' 0.040(2) 0.041(2) 0.0362(19) -0.0025(15) 0.0036(16) -0.0022(16) C29' 0.0320(18) 0.040(2) 0.0355(18) 0.0057(15) -0.0019(14) 0.0026(15) C30' 0.0312(17) 0.0321(17) 0.0275(16) 0.0039(13) 0.0019(13) 0.0049(13) C31' 0.0280(16) 0.0286(16) 0.0233(14) 0.0057(12) 0.0080(12) 0.0088(12) C32' 0.0359(18) 0.0376(18) 0.0262(16) 0.0088(13) 0.0044(13) 0.0075(14) C33' 0.0351(18) 0.0401(19) 0.0275(16) 0.0034(14) -0.0035(14) 0.0051(15) C34' 0.0319(18) 0.0347(18) 0.0355(18) 0.0037(14) 0.0008(14) 0.0054(14) C35' 0.0288(17) 0.0337(17) 0.0319(17) 0.0098(13) 0.0027(13) 0.0034(13) C36' 0.0266(16) 0.0320(17) 0.0273(15) 0.0083(12) 0.0034(12) 0.0053(13) C37' 0.0322(19) 0.038(2) 0.047(2) 0.0098(16) 0.0149(16) 0.0040(15) C38' 0.049(3) 0.062(3) 0.060(3) 0.030(2) 0.020(2) 0.019(2) C39' 0.053(3) 0.064(3) 0.078(3) 0.040(3) 0.036(3) 0.019(2) C40' 0.047(3) 0.065(3) 0.068(3) 0.021(2) 0.027(2) 0.020(2) C41' 0.040(2) 0.058(3) 0.087(4) 0.030(3) 0.034(2) 0.020(2) C42' 0.036(2) 0.048(2) 0.067(3) 0.027(2) 0.0237(19) 0.0132(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn C11 2.263(3) . ? Mn C2 2.277(3) . ? Mn C1 2.332(3) . ? Mn C10 2.334(3) . ? Mn C3 2.342(3) . ? Mn C12 2.352(3) . ? Mn C4 2.440(3) . ? Mn C5 2.451(3) . ? Mn C14 2.478(3) . ? Mn C13 2.500(4) . ? C1 C2 1.425(5) . ? C1 C5 1.429(5) . ? C1 C19 1.522(4) . ? C2 C3 1.419(4) . ? C3 C4 1.429(5) . ? C3 C25 1.515(5) . ? C4 C9 1.424(5) . ? C4 C5 1.451(5) . ? C5 C6 1.416(5) . ? C6 C7 1.377(5) . ? C7 C8 1.423(6) . ? C8 C9 1.361(6) . ? C10 C14 1.435(5) . ? C10 C11 1.436(4) . ? C10 C31 1.512(5) . ? C11 C12 1.420(5) . ? C12 C13 1.443(4) . ? C12 C37 1.514(4) . ? C13 C18 1.426(5) . ? C13 C14 1.446(5) . ? C14 C15 1.420(4) . ? C15 C16 1.363(6) . ? C17 C18 1.373(5) . ? C17 C16 1.415(6) . ? C19 C24 1.520(5) . ? C19 C20 1.534(5) . ? C20 C21 1.527(5) . ? C21 C22 1.521(5) . ? C22 C23 1.530(6) . ? C23 C24 1.533(5) . ? C25 C30 1.532(5) . ? C25 C26 1.547(4) . ? C26 C27 1.537(5) . ? C27 C28 1.514(5) . ? C28 C29 1.526(5) . ? C29 C30 1.526(5) . ? C31 C36 1.531(5) . ? C31 C32 1.532(5) . ? C32 C33 1.539(5) . ? C33 C34 1.532(7) . ? C34 C35 1.516(7) . ? C35 C36 1.528(5) . ? C37 C42 1.534(5) . ? C37 C38 1.541(5) . ? C38 C39 1.530(5) . ? C39 C40 1.526(6) . ? C40 C41 1.516(6) . ? C41 C42 1.536(5) . ? Mn' C11' 2.234(3) . ? Mn' C2' 2.259(3) . ? Mn' C10' 2.306(3) . ? Mn' C3' 2.309(3) . ? Mn' C1' 2.372(3) . ? Mn' C12' 2.376(4) . ? Mn' C4' 2.460(3) . ? Mn' C5' 2.493(4) . ? Mn' C14' 2.511(3) . ? Mn' C13' 2.576(4) . ? C1' C2' 1.425(5) . ? C1' C5' 1.432(4) . ? C1' C19' 1.514(4) . ? C2' C3' 1.434(4) . ? C3' C4' 1.433(4) . ? C3' C25' 1.505(4) . ? C4' C9' 1.420(4) . ? C4' C5' 1.442(4) . ? C5' C6' 1.416(5) . ? C6' C7' 1.372(5) . ? C7' C8' 1.412(5) . ? C8' C9' 1.369(5) . ? C10' C14' 1.428(5) . ? C10' C11' 1.429(4) . ? C10' C31' 1.514(5) . ? C11' C12' 1.430(5) . ? C12' C13' 1.425(5) . ? C12' C37' 1.517(5) . ? C13' C18' 1.416(5) . ? C13' C14' 1.449(5) . ? C14' C15' 1.415(4) . ? C15' C16' 1.374(5) . ? C16' C17' 1.421(5) . ? C17' C18' 1.372(6) . ? C19' C20' 1.509(5) . ? C19' C24' 1.517(5) . ? C20' C21' 1.529(5) . ? C21' C22' 1.511(6) . ? C22' C23' 1.516(6) . ? C23' C24' 1.538(5) . ? C25' C26' 1.531(5) . ? C25' C30' 1.534(5) . ? C26' C27' 1.530(5) . ? C27' C28' 1.525(6) . ? C28' C29' 1.516(6) . ? C29' C30' 1.521(5) . ? C31' C32' 1.533(5) . ? C31' C36' 1.541(4) . ? C32' C33' 1.527(5) . ? C33' C34' 1.524(5) . ? C34' C35' 1.526(5) . ? C35' C36' 1.525(5) . ? C37' C42' 1.497(6) . ? C37' C38' 1.541(6) . ? C38' C39' 1.532(6) . ? C39' C40' 1.532(7) . ? C40' C41' 1.463(7) . ? C41' C42' 1.534(5) . ? 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 C11 Mn C2 150.88(11) . . ? C11 Mn C1 130.67(12) . . ? C2 Mn C1 36.00(12) . . ? C11 Mn C10 36.37(10) . . ? C2 Mn C10 172.54(11) . . ? C1 Mn C10 142.84(12) . . ? C11 Mn C3 169.10(12) . . ? C2 Mn C3 35.75(11) . . ? C1 Mn C3 60.08(11) . . ? C10 Mn C3 137.71(11) . . ? C11 Mn C12 35.76(12) . . ? C2 Mn C12 126.60(12) . . ? C1 Mn C12 136.40(11) . . ? C10 Mn C12 60.12(11) . . ? C3 Mn C12 136.98(12) . . ? C11 Mn C4 148.02(11) . . ? C2 Mn C4 57.77(11) . . ? C1 Mn C4 58.44(11) . . ? C10 Mn C4 114.82(11) . . ? C3 Mn C4 34.68(11) . . ? C12 Mn C4 162.82(11) . . ? C11 Mn C5 130.90(12) . . ? C2 Mn C5 57.68(12) . . ? C1 Mn C5 34.66(11) . . ? C10 Mn C5 117.16(12) . . ? C3 Mn C5 58.17(11) . . ? C12 Mn C5 162.28(11) . . ? C4 Mn C5 34.52(11) . . ? C11 Mn C14 57.73(11) . . ? C2 Mn C14 143.47(12) . . ? C1 Mn C14 165.65(11) . . ? C10 Mn C14 34.54(11) . . ? C3 Mn C14 112.28(11) . . ? C12 Mn C14 57.80(11) . . ? C4 Mn C14 108.01(11) . . ? C5 Mn C14 131.37(11) . . ? C11 Mn C13 57.38(11) . . ? C2 Mn C13 125.12(12) . . ? C1 Mn C13 157.93(12) . . ? C10 Mn C13 57.75(11) . . ? C3 Mn C13 112.08(11) . . ? C12 Mn C13 34.43(10) . . ? C4 Mn C13 128.40(11) . . ? C5 Mn C13 161.61(11) . . ? C14 Mn C13 33.77(11) . . ? C2 C1 C5 106.4(3) . . ? C2 C1 C19 123.5(3) . . ? C5 C1 C19 129.9(3) . . ? C2 C1 Mn 69.90(18) . . ? C5 C1 Mn 77.24(19) . . ? C19 C1 Mn 122.1(2) . . ? C3 C2 C1 110.7(3) . . ? C3 C2 Mn 74.63(19) . . ? C1 C2 Mn 74.10(19) . . ? C2 C3 C4 106.6(3) . . ? C2 C3 C25 127.3(3) . . ? C4 C3 C25 125.9(3) . . ? C2 C3 Mn 69.62(18) . . ? C4 C3 Mn 76.42(19) . . ? C25 C3 Mn 123.1(2) . . ? C9 C4 C3 132.1(3) . . ? C9 C4 C5 119.7(3) . . ? C3 C4 C5 108.2(3) . . ? C9 C4 Mn 124.0(2) . . ? C3 C4 Mn 68.89(18) . . ? C5 C4 Mn 73.15(18) . . ? C6 C5 C1 132.9(3) . . ? C6 C5 C4 119.0(3) . . ? C1 C5 C4 108.1(3) . . ? C6 C5 Mn 125.8(2) . . ? C1 C5 Mn 68.10(18) . . ? C4 C5 Mn 72.33(18) . . ? C7 C6 C5 119.1(3) . . ? C6 C7 C8 121.9(4) . . ? C9 C8 C7 120.7(3) . . ? C8 C9 C4 119.6(3) . . ? C14 C10 C11 106.2(3) . . ? C14 C10 C31 124.0(3) . . ? C11 C10 C31 129.3(3) . . ? C14 C10 Mn 78.21(19) . . ? C11 C10 Mn 69.11(18) . . ? C31 C10 Mn 124.6(2) . . ? C12 C11 C10 110.6(3) . . ? C12 C11 Mn 75.53(18) . . ? C10 C11 Mn 74.52(18) . . ? C11 C12 C13 106.6(3) . . ? C11 C12 C37 127.9(3) . . ? C13 C12 C37 125.2(3) . . ? C11 C12 Mn 68.70(18) . . ? C13 C12 Mn 78.39(19) . . ? C37 C12 Mn 122.8(2) . . ? C18 C13 C12 132.1(3) . . ? C18 C13 C14 119.9(3) . . ? C12 C13 C14 108.0(3) . . ? C18 C13 Mn 126.3(2) . . ? C12 C13 Mn 67.18(18) . . ? C14 C13 Mn 72.30(19) . . ? C15 C14 C10 132.0(3) . . ? C15 C14 C13 119.4(3) . . ? C10 C14 C13 108.5(3) . . ? C15 C14 Mn 126.0(2) . . ? C10 C14 Mn 67.25(18) . . ? C13 C14 Mn 73.93(19) . . ? C16 C15 C14 119.0(3) . . ? C18 C17 C16 121.8(3) . . ? C15 C16 C17 121.7(3) . . ? C17 C18 C13 118.1(3) . . ? C24 C19 C1 114.3(3) . . ? C24 C19 C20 111.0(3) . . ? C1 C19 C20 111.7(3) . . ? C21 C20 C19 111.8(3) . . ? C22 C21 C20 112.2(3) . . ? C21 C22 C23 110.7(3) . . ? C22 C23 C24 111.8(3) . . ? C19 C24 C23 111.1(3) . . ? C3 C25 C30 112.9(3) . . ? C3 C25 C26 110.4(3) . . ? C30 C25 C26 109.6(3) . . ? C27 C26 C25 111.5(3) . . ? C28 C27 C26 111.5(3) . . ? C27 C28 C29 111.3(3) . . ? C28 C29 C30 111.4(3) . . ? C29 C30 C25 112.2(3) . . ? C10 C31 C36 110.4(3) . . ? C10 C31 C32 113.7(3) . . ? C36 C31 C32 110.6(3) . . ? C31 C32 C33 111.3(3) . . ? C34 C33 C32 111.5(3) . . ? C35 C34 C33 111.5(4) . . ? C34 C35 C36 110.2(3) . . ? C35 C36 C31 112.6(3) . . ? C12 C37 C42 111.7(3) . . ? C12 C37 C38 113.5(3) . . ? C42 C37 C38 109.2(3) . . ? C39 C38 C37 111.2(3) . . ? C40 C39 C38 112.0(3) . . ? C41 C40 C39 111.1(3) . . ? C40 C41 C42 111.2(3) . . ? C37 C42 C41 112.3(3) . . ? C11' Mn' C2' 155.55(12) . . ? C11' Mn' C10' 36.65(11) . . ? C2' Mn' C10' 167.64(12) . . ? C11' Mn' C3' 162.22(12) . . ? C2' Mn' C3' 36.58(11) . . ? C10' Mn' C3' 133.09(11) . . ? C11' Mn' C1' 137.61(12) . . ? C2' Mn' C1' 35.74(12) . . ? C10' Mn' C1' 140.23(12) . . ? C3' Mn' C1' 60.16(11) . . ? C11' Mn' C12' 35.97(13) . . ? C2' Mn' C12' 130.31(12) . . ? C10' Mn' C12' 60.17(11) . . ? C3' Mn' C12' 131.32(13) . . ? C1' Mn' C12' 147.53(12) . . ? C11' Mn' C4' 145.67(11) . . ? C2' Mn' C4' 57.96(11) . . ? C10' Mn' C4' 109.68(11) . . ? C3' Mn' C4' 34.78(11) . . ? C1' Mn' C4' 57.64(10) . . ? C12' Mn' C4' 151.94(12) . . ? C11' Mn' C5' 134.64(12) . . ? C2' Mn' C5' 57.38(11) . . ? C10' Mn' C5' 113.02(11) . . ? C3' Mn' C5' 57.97(11) . . ? C1' Mn' C5' 34.13(10) . . ? C12' Mn' C5' 170.55(12) . . ? C4' Mn' C5' 33.84(10) . . ? C11' Mn' C14' 57.17(11) . . ? C2' Mn' C14' 141.28(11) . . ? C10' Mn' C14' 34.16(11) . . ? C3' Mn' C14' 106.50(11) . . ? C1' Mn' C14' 155.72(11) . . ? C12' Mn' C14' 56.73(11) . . ? C4' Mn' C14' 99.41(10) . . ? C5' Mn' C14' 122.07(10) . . ? C11' Mn' C13' 56.30(12) . . ? C2' Mn' C13' 126.75(12) . . ? C10' Mn' C13' 56.91(11) . . ? C3' Mn' C13' 106.41(11) . . ? C1' Mn' C13' 162.45(11) . . ? C12' Mn' C13' 33.14(12) . . ? C4' Mn' C13' 118.81(11) . . ? C5' Mn' C13' 150.53(11) . . ? C14' Mn' C13' 33.06(10) . . ? C2' C1' C5' 106.6(3) . . ? C2' C1' C19' 127.6(3) . . ? C5' C1' C19' 125.5(3) . . ? C2' C1' Mn' 67.82(18) . . ? C5' C1' Mn' 77.59(19) . . ? C19' C1' Mn' 124.7(2) . . ? C1' C2' C3' 110.3(3) . . ? C1' C2' Mn' 76.44(19) . . ? C3' C2' Mn' 73.61(18) . . ? C4' C3' C2' 106.2(3) . . ? C4' C3' C25' 126.0(3) . . ? C2' C3' C25' 127.6(3) . . ? C4' C3' Mn' 78.39(19) . . ? C2' C3' Mn' 69.81(18) . . ? C25' C3' Mn' 120.8(2) . . ? C9' C4' C3' 132.4(3) . . ? C9' C4' C5' 119.2(3) . . ? C3' C4' C5' 108.5(3) . . ? C9' C4' Mn' 124.8(2) . . ? C3' C4' Mn' 66.83(17) . . ? C5' C4' Mn' 74.33(19) . . ? C6' C5' C1' 131.9(3) . . ? C6' C5' C4' 119.8(3) . . ? C1' C5' C4' 108.3(3) . . ? C6' C5' Mn' 125.4(2) . . ? C1' C5' Mn' 68.29(19) . . ? C4' C5' Mn' 71.83(19) . . ? C7' C6' C5' 119.1(3) . . ? C6' C7' C8' 121.4(3) . . ? C9' C8' C7' 121.3(3) . . ? C8' C9' C4' 119.3(3) . . ? C14' C10' C11' 106.1(3) . . ? C14' C10' C31' 124.2(3) . . ? C11' C10' C31' 128.7(3) . . ? C14' C10' Mn' 80.81(19) . . ? C11' C10' Mn' 68.95(18) . . ? C31' C10' Mn' 124.6(2) . . ? C10' C11' C12' 110.4(3) . . ? C10' C11' Mn' 74.40(19) . . ? C12' C11' Mn' 77.4(2) . . ? C13' C12' C11' 106.6(3) . . ? C13' C12' C37' 123.9(3) . . ? C11' C12' C37' 129.0(3) . . ? C13' C12' Mn' 81.2(2) . . ? C11' C12' Mn' 66.6(2) . . ? C37' C12' Mn' 123.9(2) . . ? C18' C13' C12' 132.5(3) . . ? C18' C13' C14' 119.5(3) . . ? C12' C13' C14' 108.0(3) . . ? C18' C13' Mn' 129.7(2) . . ? C12' C13' Mn' 65.7(2) . . ? C14' C13' Mn' 70.99(19) . . ? C15' C14' C10' 132.2(3) . . ? C15' C14' C13' 119.1(3) . . ? C10' C14' C13' 108.7(3) . . ? C15' C14' Mn' 126.1(2) . . ? C10' C14' Mn' 65.02(17) . . ? C13' C14' Mn' 75.95(18) . . ? C16' C15' C14' 119.7(3) . . ? C15' C16' C17' 121.3(3) . . ? C18' C17' C16' 120.6(4) . . ? C17' C18' C13' 119.8(3) . . ? C20' C19' C1' 111.7(3) . . ? C20' C19' C24' 110.5(3) . . ? C1' C19' C24' 113.6(3) . . ? C19' C20' C21' 112.2(3) . . ? C22' C21' C20' 111.5(3) . . ? C21' C22' C23' 110.4(3) . . ? C22' C23' C24' 111.3(4) . . ? C19' C24' C23' 111.2(4) . . ? C3' C25' C26' 112.7(3) . . ? C3' C25' C30' 111.1(3) . . ? C26' C25' C30' 109.9(3) . . ? C27' C26' C25' 112.0(3) . . ? C28' C27' C26' 110.4(3) . . ? C29' C28' C27' 111.1(3) . . ? C28' C29' C30' 111.9(3) . . ? C29' C30' C25' 112.4(3) . . ? C10' C31' C32' 113.7(3) . . ? C10' C31' C36' 109.2(3) . . ? C32' C31' C36' 109.9(3) . . ? C33' C32' C31' 112.0(3) . . ? C34' C33' C32' 111.5(3) . . ? C33' C34' C35' 110.8(3) . . ? C36' C35' C34' 110.1(3) . . ? C35' C36' C31' 113.1(3) . . ? C42' C37' C12' 112.4(3) . . ? C42' C37' C38' 109.9(4) . . ? C12' C37' C38' 112.3(3) . . ? C39' C38' C37' 111.2(4) . . ? C40' C39' C38' 110.9(4) . . ? C41' C40' C39' 112.7(4) . . ? C40' C41' C42' 113.3(4) . . ? C37' C42' C41' 112.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Mn C1 C2 140.98(19) . . . . ? C10 Mn C1 C2 -167.61(18) . . . . ? C3 Mn C1 C2 -36.78(18) . . . . ? C12 Mn C1 C2 91.5(2) . . . . ? C4 Mn C1 C2 -77.3(2) . . . . ? C5 Mn C1 C2 -113.0(3) . . . . ? C14 Mn C1 C2 -97.8(5) . . . . ? C13 Mn C1 C2 37.8(4) . . . . ? C11 Mn C1 C5 -106.0(2) . . . . ? C2 Mn C1 C5 113.0(3) . . . . ? C10 Mn C1 C5 -54.6(3) . . . . ? C3 Mn C1 C5 76.3(2) . . . . ? C12 Mn C1 C5 -155.50(19) . . . . ? C4 Mn C1 C5 35.72(18) . . . . ? C14 Mn C1 C5 15.3(6) . . . . ? C13 Mn C1 C5 150.9(3) . . . . ? C11 Mn C1 C19 23.4(3) . . . . ? C2 Mn C1 C19 -117.6(4) . . . . ? C10 Mn C1 C19 74.8(3) . . . . ? C3 Mn C1 C19 -154.4(3) . . . . ? C12 Mn C1 C19 -26.2(4) . . . . ? C4 Mn C1 C19 165.1(3) . . . . ? C5 Mn C1 C19 129.3(4) . . . . ? C14 Mn C1 C19 144.6(4) . . . . ? C13 Mn C1 C19 -79.8(4) . . . . ? C5 C1 C2 C3 -3.1(4) . . . . ? C19 C1 C2 C3 -177.8(3) . . . . ? Mn C1 C2 C3 66.3(2) . . . . ? C5 C1 C2 Mn -69.3(2) . . . . ? C19 C1 C2 Mn 115.9(3) . . . . ? C11 Mn C2 C3 163.8(2) . . . . ? C1 Mn C2 C3 -117.3(3) . . . . ? C10 Mn C2 C3 -31.2(10) . . . . ? C12 Mn C2 C3 121.8(2) . . . . ? C4 Mn C2 C3 -38.00(19) . . . . ? C5 Mn C2 C3 -79.1(2) . . . . ? C14 Mn C2 C3 38.3(3) . . . . ? C13 Mn C2 C3 79.0(2) . . . . ? C11 Mn C2 C1 -78.9(3) . . . . ? C10 Mn C2 C1 86.1(9) . . . . ? C3 Mn C2 C1 117.3(3) . . . . ? C12 Mn C2 C1 -120.8(2) . . . . ? C4 Mn C2 C1 79.3(2) . . . . ? C5 Mn C2 C1 38.26(18) . . . . ? C14 Mn C2 C1 155.6(2) . . . . ? C13 Mn C2 C1 -163.63(17) . . . . ? C1 C2 C3 C4 2.2(4) . . . . ? Mn C2 C3 C4 68.2(2) . . . . ? C1 C2 C3 C25 177.3(3) . . . . ? Mn C2 C3 C25 -116.7(3) . . . . ? C1 C2 C3 Mn -65.9(2) . . . . ? C11 Mn C3 C2 -134.0(6) . . . . ? C1 Mn C3 C2 37.04(19) . . . . ? C10 Mn C3 C2 174.26(19) . . . . ? C12 Mn C3 C2 -90.4(2) . . . . ? C4 Mn C3 C2 113.8(3) . . . . ? C5 Mn C3 C2 77.6(2) . . . . ? C14 Mn C3 C2 -156.51(19) . . . . ? C13 Mn C3 C2 -119.9(2) . . . . ? C11 Mn C3 C4 112.3(6) . . . . ? C2 Mn C3 C4 -113.8(3) . . . . ? C1 Mn C3 C4 -76.7(2) . . . . ? C10 Mn C3 C4 60.5(3) . . . . ? C12 Mn C3 C4 155.83(18) . . . . ? C5 Mn C3 C4 -36.17(18) . . . . ? C14 Mn C3 C4 89.7(2) . . . . ? C13 Mn C3 C4 126.29(18) . . . . ? C11 Mn C3 C25 -12.0(8) . . . . ? C2 Mn C3 C25 121.9(4) . . . . ? C1 Mn C3 C25 159.0(3) . . . . ? C10 Mn C3 C25 -63.8(3) . . . . ? C12 Mn C3 C25 31.5(3) . . . . ? C4 Mn C3 C25 -124.3(3) . . . . ? C5 Mn C3 C25 -160.5(3) . . . . ? C14 Mn C3 C25 -34.6(3) . . . . ? C13 Mn C3 C25 2.0(3) . . . . ? C2 C3 C4 C9 179.2(3) . . . . ? C25 C3 C4 C9 4.0(6) . . . . ? Mn C3 C4 C9 -117.3(4) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C25 C3 C4 C5 -175.7(3) . . . . ? Mn C3 C4 C5 63.0(2) . . . . ? C2 C3 C4 Mn -63.5(2) . . . . ? C25 C3 C4 Mn 121.3(3) . . . . ? C11 Mn C4 C9 -33.3(4) . . . . ? C2 Mn C4 C9 166.6(3) . . . . ? C1 Mn C4 C9 -150.7(3) . . . . ? C10 Mn C4 C9 -12.5(3) . . . . ? C3 Mn C4 C9 127.4(4) . . . . ? C12 Mn C4 C9 56.3(5) . . . . ? C5 Mn C4 C9 -114.9(4) . . . . ? C14 Mn C4 C9 24.0(3) . . . . ? C13 Mn C4 C9 55.0(3) . . . . ? C11 Mn C4 C3 -160.7(2) . . . . ? C2 Mn C4 C3 39.21(18) . . . . ? C1 Mn C4 C3 81.9(2) . . . . ? C10 Mn C4 C3 -139.82(18) . . . . ? C12 Mn C4 C3 -71.1(4) . . . . ? C5 Mn C4 C3 117.8(3) . . . . ? C14 Mn C4 C3 -103.33(19) . . . . ? C13 Mn C4 C3 -72.4(2) . . . . ? C11 Mn C4 C5 81.5(3) . . . . ? C2 Mn C4 C5 -78.6(2) . . . . ? C1 Mn C4 C5 -35.87(19) . . . . ? C10 Mn C4 C5 102.4(2) . . . . ? C3 Mn C4 C5 -117.8(3) . . . . ? C12 Mn C4 C5 171.2(3) . . . . ? C14 Mn C4 C5 138.91(19) . . . . ? C13 Mn C4 C5 169.85(19) . . . . ? C2 C1 C5 C6 -176.6(4) . . . . ? C19 C1 C5 C6 -2.3(6) . . . . ? Mn C1 C5 C6 119.1(4) . . . . ? C2 C1 C5 C4 2.7(4) . . . . ? C19 C1 C5 C4 177.0(3) . . . . ? Mn C1 C5 C4 -61.6(2) . . . . ? C2 C1 C5 Mn 64.3(2) . . . . ? C19 C1 C5 Mn -121.4(4) . . . . ? C9 C4 C5 C6 -1.7(5) . . . . ? C3 C4 C5 C6 178.0(3) . . . . ? Mn C4 C5 C6 -121.7(3) . . . . ? C9 C4 C5 C1 178.9(3) . . . . ? C3 C4 C5 C1 -1.4(4) . . . . ? Mn C4 C5 C1 59.0(2) . . . . ? C9 C4 C5 Mn 119.9(3) . . . . ? C3 C4 C5 Mn -60.3(2) . . . . ? C11 Mn C5 C6 -22.7(4) . . . . ? C2 Mn C5 C6 -167.8(3) . . . . ? C1 Mn C5 C6 -128.0(4) . . . . ? C10 Mn C5 C6 18.4(3) . . . . ? C3 Mn C5 C6 149.8(3) . . . . ? C12 Mn C5 C6 -58.0(5) . . . . ? C4 Mn C5 C6 113.4(4) . . . . ? C14 Mn C5 C6 57.0(3) . . . . ? C13 Mn C5 C6 87.5(5) . . . . ? C11 Mn C5 C1 105.3(2) . . . . ? C2 Mn C5 C1 -39.79(19) . . . . ? C10 Mn C5 C1 146.42(18) . . . . ? C3 Mn C5 C1 -82.3(2) . . . . ? C12 Mn C5 C1 70.0(4) . . . . ? C4 Mn C5 C1 -118.6(3) . . . . ? C14 Mn C5 C1 -175.02(18) . . . . ? C13 Mn C5 C1 -144.6(3) . . . . ? C11 Mn C5 C4 -136.13(19) . . . . ? C2 Mn C5 C4 78.8(2) . . . . ? C1 Mn C5 C4 118.6(3) . . . . ? C10 Mn C5 C4 -95.0(2) . . . . ? C3 Mn C5 C4 36.34(18) . . . . ? C12 Mn C5 C4 -171.4(3) . . . . ? C14 Mn C5 C4 -56.4(2) . . . . ? C13 Mn C5 C4 -26.0(5) . . . . ? C1 C5 C6 C7 179.8(4) . . . . ? C4 C5 C6 C7 0.6(5) . . . . ? Mn C5 C6 C7 -87.7(4) . . . . ? C5 C6 C7 C8 0.5(6) . . . . ? C6 C7 C8 C9 -0.6(6) . . . . ? C7 C8 C9 C4 -0.5(6) . . . . ? C3 C4 C9 C8 -178.0(4) . . . . ? C5 C4 C9 C8 1.7(5) . . . . ? Mn C4 C9 C8 90.6(4) . . . . ? C11 Mn C10 C14 -112.6(3) . . . . ? C2 Mn C10 C14 79.6(9) . . . . ? C1 Mn C10 C14 155.8(2) . . . . ? C3 Mn C10 C14 52.9(3) . . . . ? C12 Mn C10 C14 -75.6(2) . . . . ? C4 Mn C10 C14 85.9(2) . . . . ? C5 Mn C10 C14 124.39(19) . . . . ? C13 Mn C10 C14 -35.23(17) . . . . ? C2 Mn C10 C11 -167.8(9) . . . . ? C1 Mn C10 C11 -91.6(2) . . . . ? C3 Mn C10 C11 165.5(2) . . . . ? C12 Mn C10 C11 37.06(19) . . . . ? C4 Mn C10 C11 -161.44(19) . . . . ? C5 Mn C10 C11 -122.98(19) . . . . ? C14 Mn C10 C11 112.6(3) . . . . ? C13 Mn C10 C11 77.4(2) . . . . ? C11 Mn C10 C31 124.1(3) . . . . ? C2 Mn C10 C31 -43.7(10) . . . . ? C1 Mn C10 C31 32.5(3) . . . . ? C3 Mn C10 C31 -70.4(3) . . . . ? C12 Mn C10 C31 161.1(3) . . . . ? C4 Mn C10 C31 -37.4(3) . . . . ? C5 Mn C10 C31 1.1(3) . . . . ? C14 Mn C10 C31 -123.3(3) . . . . ? C13 Mn C10 C31 -158.5(3) . . . . ? C14 C10 C11 C12 2.6(4) . . . . ? C31 C10 C11 C12 174.2(3) . . . . ? Mn C10 C11 C12 -67.6(2) . . . . ? C14 C10 C11 Mn 70.2(2) . . . . ? C31 C10 C11 Mn -118.2(3) . . . . ? C2 Mn C11 C12 -66.6(3) . . . . ? C1 Mn C11 C12 -116.2(2) . . . . ? C10 Mn C11 C12 116.6(3) . . . . ? C3 Mn C11 C12 53.6(7) . . . . ? C4 Mn C11 C12 149.7(2) . . . . ? C5 Mn C11 C12 -162.48(18) . . . . ? C14 Mn C11 C12 78.4(2) . . . . ? C13 Mn C11 C12 38.10(18) . . . . ? C2 Mn C11 C10 176.8(2) . . . . ? C1 Mn C11 C10 127.3(2) . . . . ? C3 Mn C11 C10 -63.0(7) . . . . ? C12 Mn C11 C10 -116.6(3) . . . . ? C4 Mn C11 C10 33.1(3) . . . . ? C5 Mn C11 C10 80.9(2) . . . . ? C14 Mn C11 C10 -38.24(19) . . . . ? C13 Mn C11 C10 -78.5(2) . . . . ? C10 C11 C12 C13 -3.0(4) . . . . ? Mn C11 C12 C13 -70.0(2) . . . . ? C10 C11 C12 C37 -177.4(3) . . . . ? Mn C11 C12 C37 115.7(3) . . . . ? C10 C11 C12 Mn 67.0(2) . . . . ? C2 Mn C12 C11 146.19(18) . . . . ? C1 Mn C12 C11 99.1(2) . . . . ? C10 Mn C12 C11 -37.70(18) . . . . ? C3 Mn C12 C11 -167.11(18) . . . . ? C4 Mn C12 C11 -115.0(4) . . . . ? C5 Mn C12 C11 48.4(4) . . . . ? C14 Mn C12 C11 -78.2(2) . . . . ? C13 Mn C12 C11 -113.2(3) . . . . ? C11 Mn C12 C13 113.2(3) . . . . ? C2 Mn C12 C13 -100.6(2) . . . . ? C1 Mn C12 C13 -147.6(2) . . . . ? C10 Mn C12 C13 75.5(2) . . . . ? C3 Mn C12 C13 -53.9(3) . . . . ? C4 Mn C12 C13 -1.8(5) . . . . ? C5 Mn C12 C13 161.6(3) . . . . ? C14 Mn C12 C13 35.05(19) . . . . ? C11 Mn C12 C37 -122.2(3) . . . . ? C2 Mn C12 C37 24.0(3) . . . . ? C1 Mn C12 C37 -23.1(3) . . . . ? C10 Mn C12 C37 -159.9(3) . . . . ? C3 Mn C12 C37 70.7(3) . . . . ? C4 Mn C12 C37 122.8(4) . . . . ? C5 Mn C12 C37 -73.9(5) . . . . ? C14 Mn C12 C37 159.6(3) . . . . ? C13 Mn C12 C37 124.6(4) . . . . ? C11 C12 C13 C18 -177.6(4) . . . . ? C37 C12 C13 C18 -3.1(6) . . . . ? Mn C12 C13 C18 119.1(4) . . . . ? C11 C12 C13 C14 2.3(4) . . . . ? C37 C12 C13 C14 176.8(3) . . . . ? Mn C12 C13 C14 -61.1(2) . . . . ? C11 C12 C13 Mn 63.4(2) . . . . ? C37 C12 C13 Mn -122.1(3) . . . . ? C11 Mn C13 C18 -166.0(3) . . . . ? C2 Mn C13 C18 -21.2(3) . . . . ? C1 Mn C13 C18 -47.3(4) . . . . ? C10 Mn C13 C18 150.6(3) . . . . ? C3 Mn C13 C18 17.1(3) . . . . ? C12 Mn C13 C18 -126.4(4) . . . . ? C4 Mn C13 C18 52.9(3) . . . . ? C5 Mn C13 C18 71.4(5) . . . . ? C14 Mn C13 C18 114.5(3) . . . . ? C11 Mn C13 C12 -39.63(19) . . . . ? C2 Mn C13 C12 105.3(2) . . . . ? C1 Mn C13 C12 79.1(3) . . . . ? C10 Mn C13 C12 -83.0(2) . . . . ? C3 Mn C13 C12 143.50(19) . . . . ? C4 Mn C13 C12 179.32(18) . . . . ? C5 Mn C13 C12 -162.2(3) . . . . ? C14 Mn C13 C12 -119.1(3) . . . . ? C11 Mn C13 C14 79.4(2) . . . . ? C2 Mn C13 C14 -135.68(19) . . . . ? C1 Mn C13 C14 -161.8(3) . . . . ? C10 Mn C13 C14 36.04(18) . . . . ? C3 Mn C13 C14 -97.4(2) . . . . ? C12 Mn C13 C14 119.1(3) . . . . ? C4 Mn C13 C14 -61.6(2) . . . . ? C5 Mn C13 C14 -43.2(4) . . . . ? C11 C10 C14 C15 177.4(4) . . . . ? C31 C10 C14 C15 5.3(6) . . . . ? Mn C10 C14 C15 -118.7(4) . . . . ? C11 C10 C14 C13 -1.1(4) . . . . ? C31 C10 C14 C13 -173.3(3) . . . . ? Mn C10 C14 C13 62.8(2) . . . . ? C11 C10 C14 Mn -63.9(2) . . . . ? C31 C10 C14 Mn 123.9(3) . . . . ? C18 C13 C14 C15 0.4(5) . . . . ? C12 C13 C14 C15 -179.5(3) . . . . ? Mn C13 C14 C15 122.7(3) . . . . ? C18 C13 C14 C10 179.1(3) . . . . ? C12 C13 C14 C10 -0.7(4) . . . . ? Mn C13 C14 C10 -58.6(2) . . . . ? C18 C13 C14 Mn -122.2(3) . . . . ? C12 C13 C14 Mn 57.9(2) . . . . ? C11 Mn C14 C15 166.7(4) . . . . ? C2 Mn C14 C15 -41.2(4) . . . . ? C1 Mn C14 C15 36.8(7) . . . . ? C10 Mn C14 C15 126.4(4) . . . . ? C3 Mn C14 C15 -18.2(3) . . . . ? C12 Mn C14 C15 -150.7(4) . . . . ? C4 Mn C14 C15 18.5(3) . . . . ? C5 Mn C14 C15 48.3(4) . . . . ? C13 Mn C14 C15 -115.0(4) . . . . ? C11 Mn C14 C10 40.34(18) . . . . ? C2 Mn C14 C10 -167.6(2) . . . . ? C1 Mn C14 C10 -89.6(5) . . . . ? C3 Mn C14 C10 -144.57(18) . . . . ? C12 Mn C14 C10 82.9(2) . . . . ? C4 Mn C14 C10 -107.82(19) . . . . ? C5 Mn C14 C10 -78.1(2) . . . . ? C13 Mn C14 C10 118.6(3) . . . . ? C11 Mn C14 C13 -78.3(2) . . . . ? C2 Mn C14 C13 73.7(3) . . . . ? C1 Mn C14 C13 151.8(4) . . . . ? C10 Mn C14 C13 -118.6(3) . . . . ? C3 Mn C14 C13 96.8(2) . . . . ? C12 Mn C14 C13 -35.73(18) . . . . ? C4 Mn C14 C13 133.53(18) . . . . ? C5 Mn C14 C13 163.29(18) . . . . ? C10 C14 C15 C16 -177.4(4) . . . . ? C13 C14 C15 C16 1.0(5) . . . . ? Mn C14 C15 C16 92.0(4) . . . . ? C14 C15 C16 C17 -1.0(6) . . . . ? C18 C17 C16 C15 -0.5(6) . . . . ? C16 C17 C18 C13 1.9(6) . . . . ? C12 C13 C18 C17 178.0(4) . . . . ? C14 C13 C18 C17 -1.8(5) . . . . ? Mn C13 C18 C17 -91.1(4) . . . . ? C2 C1 C19 C24 -132.0(3) . . . . ? C5 C1 C19 C24 54.5(5) . . . . ? Mn C1 C19 C24 -46.1(4) . . . . ? C2 C1 C19 C20 101.0(4) . . . . ? C5 C1 C19 C20 -72.5(5) . . . . ? Mn C1 C19 C20 -173.1(2) . . . . ? C24 C19 C20 C21 54.5(4) . . . . ? C1 C19 C20 C21 -176.7(3) . . . . ? C19 C20 C21 C22 -54.2(4) . . . . ? C20 C21 C22 C23 53.9(4) . . . . ? C21 C22 C23 C24 -54.8(4) . . . . ? C1 C19 C24 C23 177.4(3) . . . . ? C20 C19 C24 C23 -55.2(4) . . . . ? C22 C23 C24 C19 56.0(4) . . . . ? C2 C3 C25 C30 19.1(5) . . . . ? C4 C3 C25 C30 -166.7(3) . . . . ? Mn C3 C25 C30 -69.4(3) . . . . ? C2 C3 C25 C26 -104.0(4) . . . . ? C4 C3 C25 C26 70.2(4) . . . . ? Mn C3 C25 C26 167.5(2) . . . . ? C3 C25 C26 C27 179.9(3) . . . . ? C30 C25 C26 C27 54.9(4) . . . . ? C25 C26 C27 C28 -55.7(4) . . . . ? C26 C27 C28 C29 55.2(4) . . . . ? C27 C28 C29 C30 -55.0(4) . . . . ? C28 C29 C30 C25 55.8(4) . . . . ? C3 C25 C30 C29 -178.8(3) . . . . ? C26 C25 C30 C29 -55.3(4) . . . . ? C14 C10 C31 C36 75.9(4) . . . . ? C11 C10 C31 C36 -94.3(4) . . . . ? Mn C10 C31 C36 175.4(2) . . . . ? C14 C10 C31 C32 -159.1(3) . . . . ? C11 C10 C31 C32 30.6(5) . . . . ? Mn C10 C31 C32 -59.6(3) . . . . ? C10 C31 C32 C33 -178.5(3) . . . . ? C36 C31 C32 C33 -53.6(4) . . . . ? C31 C32 C33 C34 54.4(4) . . . . ? C32 C33 C34 C35 -55.9(4) . . . . ? C33 C34 C35 C36 56.0(5) . . . . ? C34 C35 C36 C31 -56.4(5) . . . . ? C10 C31 C36 C35 -178.0(3) . . . . ? C32 C31 C36 C35 55.2(4) . . . . ? C11 C12 C37 C42 65.9(4) . . . . ? C13 C12 C37 C42 -107.4(4) . . . . ? Mn C12 C37 C42 153.3(2) . . . . ? C11 C12 C37 C38 -58.0(5) . . . . ? C13 C12 C37 C38 128.7(4) . . . . ? Mn C12 C37 C38 29.4(4) . . . . ? C12 C37 C38 C39 -178.8(3) . . . . ? C42 C37 C38 C39 55.9(4) . . . . ? C37 C38 C39 C40 -56.3(5) . . . . ? C38 C39 C40 C41 55.0(5) . . . . ? C39 C40 C41 C42 -54.1(5) . . . . ? C12 C37 C42 C41 177.5(3) . . . . ? C38 C37 C42 C41 -56.2(4) . . . . ? C40 C41 C42 C37 56.0(4) . . . . ? C11' Mn' C1' C2' 142.1(2) . . . . ? C10' Mn' C1' C2' -160.84(19) . . . . ? C3' Mn' C1' C2' -38.02(18) . . . . ? C12' Mn' C1' C2' 83.1(3) . . . . ? C4' Mn' C1' C2' -78.8(2) . . . . ? C5' Mn' C1' C2' -113.9(3) . . . . ? C14' Mn' C1' C2' -99.7(3) . . . . ? C13' Mn' C1' C2' 4.8(5) . . . . ? C11' Mn' C1' C5' -104.0(2) . . . . ? C2' Mn' C1' C5' 113.9(3) . . . . ? C10' Mn' C1' C5' -46.9(3) . . . . ? C3' Mn' C1' C5' 75.9(2) . . . . ? C12' Mn' C1' C5' -163.0(2) . . . . ? C4' Mn' C1' C5' 35.15(18) . . . . ? C14' Mn' C1' C5' 14.3(4) . . . . ? C13' Mn' C1' C5' 118.7(4) . . . . ? C11' Mn' C1' C19' 20.9(4) . . . . ? C2' Mn' C1' C19' -121.2(4) . . . . ? C10' Mn' C1' C19' 77.9(3) . . . . ? C3' Mn' C1' C19' -159.2(3) . . . . ? C12' Mn' C1' C19' -38.2(4) . . . . ? C4' Mn' C1' C19' 160.0(3) . . . . ? C5' Mn' C1' C19' 124.8(4) . . . . ? C14' Mn' C1' C19' 139.1(3) . . . . ? C13' Mn' C1' C19' -116.4(4) . . . . ? C5' C1' C2' C3' -2.2(4) . . . . ? C19' C1' C2' C3' -176.0(3) . . . . ? Mn' C1' C2' C3' 66.5(2) . . . . ? C5' C1' C2' Mn' -68.7(2) . . . . ? C19' C1' C2' Mn' 117.5(3) . . . . ? C11' Mn' C2' C1' -89.9(4) . . . . ? C10' Mn' C2' C1' 78.8(6) . . . . ? C3' Mn' C2' C1' 116.3(3) . . . . ? C12' Mn' C2' C1' -135.7(2) . . . . ? C4' Mn' C2' C1' 77.8(2) . . . . ? C5' Mn' C2' C1' 37.50(18) . . . . ? C14' Mn' C2' C1' 139.6(2) . . . . ? C13' Mn' C2' C1' -178.19(18) . . . . ? C11' Mn' C2' C3' 153.8(3) . . . . ? C10' Mn' C2' C3' -37.5(7) . . . . ? C1' Mn' C2' C3' -116.3(3) . . . . ? C12' Mn' C2' C3' 108.0(2) . . . . ? C4' Mn' C2' C3' -38.51(18) . . . . ? C5' Mn' C2' C3' -78.8(2) . . . . ? C14' Mn' C2' C3' 23.3(3) . . . . ? C13' Mn' C2' C3' 65.5(2) . . . . ? C1' C2' C3' C4' 2.4(4) . . . . ? Mn' C2' C3' C4' 70.7(2) . . . . ? C1' C2' C3' C25' 177.8(3) . . . . ? Mn' C2' C3' C25' -113.9(3) . . . . ? C1' C2' C3' Mn' -68.3(2) . . . . ? C11' Mn' C3' C4' 104.5(4) . . . . ? C2' Mn' C3' C4' -112.3(3) . . . . ? C10' Mn' C3' C4' 57.4(2) . . . . ? C1' Mn' C3' C4' -75.17(19) . . . . ? C12' Mn' C3' C4' 142.57(18) . . . . ? C5' Mn' C3' C4' -35.24(17) . . . . ? C14' Mn' C3' C4' 82.65(19) . . . . ? C13' Mn' C3' C4' 117.17(18) . . . . ? C11' Mn' C3' C2' -143.2(4) . . . . ? C10' Mn' C3' C2' 169.72(19) . . . . ? C1' Mn' C3' C2' 37.13(19) . . . . ? C12' Mn' C3' C2' -105.1(2) . . . . ? C4' Mn' C3' C2' 112.3(3) . . . . ? C5' Mn' C3' C2' 77.1(2) . . . . ? C14' Mn' C3' C2' -165.04(19) . . . . ? C13' Mn' C3' C2' -130.53(19) . . . . ? C11' Mn' C3' C25' -20.7(5) . . . . ? C2' Mn' C3' C25' 122.5(3) . . . . ? C10' Mn' C3' C25' -67.8(3) . . . . ? C1' Mn' C3' C25' 159.6(3) . . . . ? C12' Mn' C3' C25' 17.4(3) . . . . ? C4' Mn' C3' C25' -125.2(3) . . . . ? C5' Mn' C3' C25' -160.5(3) . . . . ? C14' Mn' C3' C25' -42.6(3) . . . . ? C13' Mn' C3' C25' -8.0(3) . . . . ? C2' C3' C4' C9' 178.6(4) . . . . ? C25' C3' C4' C9' 3.1(6) . . . . ? Mn' C3' C4' C9' -116.7(4) . . . . ? C2' C3' C4' C5' -1.7(4) . . . . ? C25' C3' C4' C5' -177.2(3) . . . . ? Mn' C3' C4' C5' 63.1(2) . . . . ? C2' C3' C4' Mn' -64.7(2) . . . . ? C25' C3' C4' Mn' 119.8(3) . . . . ? C11' Mn' C4' C9' -21.9(4) . . . . ? C2' Mn' C4' C9' 167.1(3) . . . . ? C10' Mn' C4' C9' -12.7(3) . . . . ? C3' Mn' C4' C9' 126.5(4) . . . . ? C1' Mn' C4' C9' -150.4(3) . . . . ? C12' Mn' C4' C9' 50.5(4) . . . . ? C5' Mn' C4' C9' -114.9(4) . . . . ? C14' Mn' C4' C9' 21.1(3) . . . . ? C13' Mn' C4' C9' 49.6(3) . . . . ? C11' Mn' C4' C3' -148.4(2) . . . . ? C2' Mn' C4' C3' 40.58(18) . . . . ? C10' Mn' C4' C3' -139.19(19) . . . . ? C1' Mn' C4' C3' 83.1(2) . . . . ? C12' Mn' C4' C3' -76.1(3) . . . . ? C5' Mn' C4' C3' 118.6(3) . . . . ? C14' Mn' C4' C3' -105.45(19) . . . . ? C13' Mn' C4' C3' -76.9(2) . . . . ? C11' Mn' C4' C5' 93.1(3) . . . . ? C2' Mn' C4' C5' -78.0(2) . . . . ? C10' Mn' C4' C5' 102.26(19) . . . . ? C3' Mn' C4' C5' -118.6(3) . . . . ? C1' Mn' C4' C5' -35.45(18) . . . . ? C12' Mn' C4' C5' 165.4(2) . . . . ? C14' Mn' C4' C5' 136.00(18) . . . . ? C13' Mn' C4' C5' 164.55(17) . . . . ? C2' C1' C5' C6' -179.2(4) . . . . ? C19' C1' C5' C6' -5.2(6) . . . . ? Mn' C1' C5' C6' 118.7(4) . . . . ? C2' C1' C5' C4' 1.1(4) . . . . ? C19' C1' C5' C4' 175.1(3) . . . . ? Mn' C1' C5' C4' -60.9(2) . . . . ? C2' C1' C5' Mn' 62.0(2) . . . . ? C19' C1' C5' Mn' -124.0(3) . . . . ? C9' C4' C5' C6' 0.4(5) . . . . ? C3' C4' C5' C6' -179.4(3) . . . . ? Mn' C4' C5' C6' -121.0(3) . . . . ? C9' C4' C5' C1' -179.8(3) . . . . ? C3' C4' C5' C1' 0.4(4) . . . . ? Mn' C4' C5' C1' 58.7(2) . . . . ? C9' C4' C5' Mn' 121.4(3) . . . . ? C3' C4' C5' Mn' -58.4(2) . . . . ? C11' Mn' C5' C6' -13.6(3) . . . . ? C2' Mn' C5' C6' -166.1(3) . . . . ? C10' Mn' C5' C6' 22.7(3) . . . . ? C3' Mn' C5' C6' 150.3(3) . . . . ? C1' Mn' C5' C6' -126.8(4) . . . . ? C12' Mn' C5' C6' -19.7(8) . . . . ? C4' Mn' C5' C6' 114.1(3) . . . . ? C14' Mn' C5' C6' 60.1(3) . . . . ? C13' Mn' C5' C6' 85.7(3) . . . . ? C11' Mn' C5' C1' 113.2(2) . . . . ? C2' Mn' C5' C1' -39.34(19) . . . . ? C10' Mn' C5' C1' 149.49(19) . . . . ? C3' Mn' C5' C1' -82.9(2) . . . . ? C12' Mn' C5' C1' 107.1(7) . . . . ? C4' Mn' C5' C1' -119.2(3) . . . . ? C14' Mn' C5' C1' -173.13(18) . . . . ? C13' Mn' C5' C1' -147.5(2) . . . . ? C11' Mn' C5' C4' -127.7(2) . . . . ? C2' Mn' C5' C4' 79.8(2) . . . . ? C10' Mn' C5' C4' -91.3(2) . . . . ? C3' Mn' C5' C4' 36.23(18) . . . . ? C1' Mn' C5' C4' 119.2(3) . . . . ? C12' Mn' C5' C4' -133.7(6) . . . . ? C14' Mn' C5' C4' -54.0(2) . . . . ? C13' Mn' C5' C4' -28.3(3) . . . . ? C1' C5' C6' C7' 179.4(4) . . . . ? C4' C5' C6' C7' -0.9(5) . . . . ? Mn' C5' C6' C7' -89.0(4) . . . . ? C5' C6' C7' C8' 0.5(6) . . . . ? C6' C7' C8' C9' 0.5(6) . . . . ? C7' C8' C9' C4' -1.0(5) . . . . ? C3' C4' C9' C8' -179.7(3) . . . . ? C5' C4' C9' C8' 0.5(5) . . . . ? Mn' C4' C9' C8' 91.1(4) . . . . ? C11' Mn' C10' C14' -111.3(3) . . . . ? C2' Mn' C10' C14' 76.5(6) . . . . ? C3' Mn' C10' C14' 46.7(3) . . . . ? C1' Mn' C10' C14' 140.1(2) . . . . ? C12' Mn' C10' C14' -73.7(2) . . . . ? C4' Mn' C10' C14' 77.4(2) . . . . ? C5' Mn' C10' C14' 113.66(19) . . . . ? C13' Mn' C10' C14' -34.79(18) . . . . ? C2' Mn' C10' C11' -172.2(5) . . . . ? C3' Mn' C10' C11' 158.0(2) . . . . ? C1' Mn' C10' C11' -108.6(2) . . . . ? C12' Mn' C10' C11' 37.6(2) . . . . ? C4' Mn' C10' C11' -171.3(2) . . . . ? C5' Mn' C10' C11' -135.1(2) . . . . ? C14' Mn' C10' C11' 111.3(3) . . . . ? C13' Mn' C10' C11' 76.5(2) . . . . ? C11' Mn' C10' C31' 123.2(4) . . . . ? C2' Mn' C10' C31' -49.0(7) . . . . ? C3' Mn' C10' C31' -78.8(3) . . . . ? C1' Mn' C10' C31' 14.6(3) . . . . ? C12' Mn' C10' C31' 160.8(3) . . . . ? C4' Mn' C10' C31' -48.1(3) . . . . ? C5' Mn' C10' C31' -11.9(3) . . . . ? C14' Mn' C10' C31' -125.5(3) . . . . ? C13' Mn' C10' C31' -160.3(3) . . . . ? C14' C10' C11' C12' 3.4(4) . . . . ? C31' C10' C11' C12' 172.0(3) . . . . ? Mn' C10' C11' C12' -69.8(2) . . . . ? C14' C10' C11' Mn' 73.2(2) . . . . ? C31' C10' C11' Mn' -118.2(3) . . . . ? C2' Mn' C11' C10' 176.0(3) . . . . ? C3' Mn' C11' C10' -63.7(5) . . . . ? C1' Mn' C11' C10' 115.9(2) . . . . ? C12' Mn' C11' C10' -115.7(3) . . . . ? C4' Mn' C11' C10' 14.6(3) . . . . ? C5' Mn' C11' C10' 66.0(3) . . . . ? C14' Mn' C11' C10' -38.52(19) . . . . ? C13' Mn' C11' C10' -78.3(2) . . . . ? C2' Mn' C11' C12' -68.3(4) . . . . ? C10' Mn' C11' C12' 115.7(3) . . . . ? C3' Mn' C11' C12' 52.0(4) . . . . ? C1' Mn' C11' C12' -128.4(2) . . . . ? C4' Mn' C11' C12' 130.3(2) . . . . ? C5' Mn' C11' C12' -178.31(18) . . . . ? C14' Mn' C11' C12' 77.2(2) . . . . ? C13' Mn' C11' C12' 37.38(19) . . . . ? C10' C11' C12' C13' -4.4(4) . . . . ? Mn' C11' C12' C13' -72.3(2) . . . . ? C10' C11' C12' C37' -176.6(4) . . . . ? Mn' C11' C12' C37' 115.5(4) . . . . ? C10' C11' C12' Mn' 67.9(2) . . . . ? C11' Mn' C12' C13' 112.5(3) . . . . ? C2' Mn' C12' C13' -97.8(2) . . . . ? C10' Mn' C12' C13' 74.2(2) . . . . ? C3' Mn' C12' C13' -48.8(2) . . . . ? C1' Mn' C12' C13' -147.3(2) . . . . ? C4' Mn' C12' C13' -1.3(4) . . . . ? C5' Mn' C12' C13' 119.8(7) . . . . ? C14' Mn' C12' C13' 34.03(18) . . . . ? C2' Mn' C12' C11' 149.70(19) . . . . ? C10' Mn' C12' C11' -38.33(19) . . . . ? C3' Mn' C12' C11' -161.32(18) . . . . ? C1' Mn' C12' C11' 100.2(3) . . . . ? C4' Mn' C12' C11' -113.8(3) . . . . ? C5' Mn' C12' C11' 7.3(8) . . . . ? C14' Mn' C12' C11' -78.5(2) . . . . ? C13' Mn' C12' C11' -112.5(3) . . . . ? C11' Mn' C12' C37' -122.4(4) . . . . ? C2' Mn' C12' C37' 27.3(4) . . . . ? C10' Mn' C12' C37' -160.7(4) . . . . ? C3' Mn' C12' C37' 76.3(3) . . . . ? C1' Mn' C12' C37' -22.2(5) . . . . ? C4' Mn' C12' C37' 123.8(3) . . . . ? C5' Mn' C12' C37' -115.0(6) . . . . ? C14' Mn' C12' C37' 159.2(4) . . . . ? C13' Mn' C12' C37' 125.1(4) . . . . ? C11' C12' C13' C18' -175.4(4) . . . . ? C37' C12' C13' C18' -2.7(6) . . . . ? Mn' C12' C13' C18' 122.4(4) . . . . ? C11' C12' C13' C14' 3.7(4) . . . . ? C37' C12' C13' C14' 176.4(3) . . . . ? Mn' C12' C13' C14' -58.5(2) . . . . ? C11' C12' C13' Mn' 62.2(2) . . . . ? C37' C12' C13' Mn' -125.1(4) . . . . ? C11' Mn' C13' C18' -166.8(4) . . . . ? C2' Mn' C13' C18' -16.6(4) . . . . ? C10' Mn' C13' C18' 149.0(4) . . . . ? C3' Mn' C13' C18' 17.8(3) . . . . ? C1' Mn' C13' C18' -20.1(6) . . . . ? C12' Mn' C13' C18' -126.1(4) . . . . ? C4' Mn' C13' C18' 53.2(3) . . . . ? C5' Mn' C13' C18' 70.8(4) . . . . ? C14' Mn' C13' C18' 113.0(4) . . . . ? C11' Mn' C13' C12' -40.7(2) . . . . ? C2' Mn' C13' C12' 109.5(2) . . . . ? C10' Mn' C13' C12' -85.0(2) . . . . ? C3' Mn' C13' C12' 143.9(2) . . . . ? C1' Mn' C13' C12' 106.0(4) . . . . ? C4' Mn' C13' C12' 179.28(19) . . . . ? C5' Mn' C13' C12' -163.2(2) . . . . ? C14' Mn' C13' C12' -120.9(3) . . . . ? C11' Mn' C13' C14' 80.2(2) . . . . ? C2' Mn' C13' C14' -129.6(2) . . . . ? C10' Mn' C13' C14' 35.97(19) . . . . ? C3' Mn' C13' C14' -95.2(2) . . . . ? C1' Mn' C13' C14' -133.1(4) . . . . ? C12' Mn' C13' C14' 120.9(3) . . . . ? C4' Mn' C13' C14' -59.8(2) . . . . ? C5' Mn' C13' C14' -42.2(3) . . . . ? C11' C10' C14' C15' 178.0(4) . . . . ? C31' C10' C14' C15' 8.8(6) . . . . ? Mn' C10' C14' C15' -117.1(4) . . . . ? C11' C10' C14' C13' -1.0(4) . . . . ? C31' C10' C14' C13' -170.2(3) . . . . ? Mn' C10' C14' C13' 63.9(2) . . . . ? C11' C10' C14' Mn' -64.8(2) . . . . ? C31' C10' C14' Mn' 125.9(3) . . . . ? C18' C13' C14' C15' -1.7(5) . . . . ? C12' C13' C14' C15' 179.1(3) . . . . ? Mn' C13' C14' C15' 123.8(3) . . . . ? C18' C13' C14' C10' 177.5(3) . . . . ? C12' C13' C14' C10' -1.7(4) . . . . ? Mn' C13' C14' C10' -57.0(2) . . . . ? C18' C13' C14' Mn' -125.5(3) . . . . ? C12' C13' C14' Mn' 55.3(2) . . . . ? C11' Mn' C14' C15' 166.7(3) . . . . ? C2' Mn' C14' C15' -35.3(4) . . . . ? C10' Mn' C14' C15' 125.3(4) . . . . ? C3' Mn' C14' C15' -21.1(3) . . . . ? C1' Mn' C14' C15' 31.7(5) . . . . ? C12' Mn' C14' C15' -150.0(3) . . . . ? C4' Mn' C14' C15' 13.9(3) . . . . ? C5' Mn' C14' C15' 41.1(3) . . . . ? C13' Mn' C14' C15' -115.9(4) . . . . ? C11' Mn' C14' C10' 41.4(2) . . . . ? C2' Mn' C14' C10' -160.6(2) . . . . ? C3' Mn' C14' C10' -146.33(19) . . . . ? C1' Mn' C14' C10' -93.6(3) . . . . ? C12' Mn' C14' C10' 84.7(2) . . . . ? C4' Mn' C14' C10' -111.3(2) . . . . ? C5' Mn' C14' C10' -84.2(2) . . . . ? C13' Mn' C14' C10' 118.8(3) . . . . ? C11' Mn' C14' C13' -77.3(2) . . . . ? C2' Mn' C14' C13' 80.6(3) . . . . ? C10' Mn' C14' C13' -118.8(3) . . . . ? C3' Mn' C14' C13' 94.9(2) . . . . ? C1' Mn' C14' C13' 147.6(3) . . . . ? C12' Mn' C14' C13' -34.1(2) . . . . ? C4' Mn' C14' C13' 129.9(2) . . . . ? C5' Mn' C14' C13' 157.02(19) . . . . ? C10' C14' C15' C16' -176.0(4) . . . . ? C13' C14' C15' C16' 3.0(5) . . . . ? Mn' C14' C15' C16' 96.5(4) . . . . ? C14' C15' C16' C17' -1.4(5) . . . . ? C15' C16' C17' C18' -1.5(6) . . . . ? C16' C17' C18' C13' 2.8(6) . . . . ? C12' C13' C18' C17' 177.8(4) . . . . ? C14' C13' C18' C17' -1.2(5) . . . . ? Mn' C13' C18' C17' -90.2(4) . . . . ? C2' C1' C19' C20' 36.9(5) . . . . ? C5' C1' C19' C20' -135.8(4) . . . . ? Mn' C1' C19' C20' 124.2(3) . . . . ? C2' C1' C19' C24' -88.9(5) . . . . ? C5' C1' C19' C24' 98.4(5) . . . . ? Mn' C1' C19' C24' -1.6(5) . . . . ? C1' C19' C20' C21' 177.6(3) . . . . ? C24' C19' C20' C21' -54.9(5) . . . . ? C19' C20' C21' C22' 55.5(5) . . . . ? C20' C21' C22' C23' -55.3(5) . . . . ? C21' C22' C23' C24' 55.9(6) . . . . ? C20' C19' C24' C23' 55.0(5) . . . . ? C1' C19' C24' C23' -178.5(4) . . . . ? C22' C23' C24' C19' -56.3(6) . . . . ? C4' C3' C25' C26' 68.3(4) . . . . ? C2' C3' C25' C26' -106.3(4) . . . . ? Mn' C3' C25' C26' 166.5(2) . . . . ? C4' C3' C25' C30' -167.8(3) . . . . ? C2' C3' C25' C30' 17.6(5) . . . . ? Mn' C3' C25' C30' -69.6(3) . . . . ? C3' C25' C26' C27' 179.7(3) . . . . ? C30' C25' C26' C27' 55.2(4) . . . . ? C25' C26' C27' C28' -57.0(4) . . . . ? C26' C27' C28' C29' 56.2(5) . . . . ? C27' C28' C29' C30' -55.2(4) . . . . ? C28' C29' C30' C25' 54.4(4) . . . . ? C3' C25' C30' C29' -179.0(3) . . . . ? C26' C25' C30' C29' -53.5(4) . . . . ? C14' C10' C31' C32' -166.0(3) . . . . ? C11' C10' C31' C32' 27.2(5) . . . . ? Mn' C10' C31' C32' -62.4(3) . . . . ? C14' C10' C31' C36' 70.8(4) . . . . ? C11' C10' C31' C36' -96.0(4) . . . . ? Mn' C10' C31' C36' 174.4(2) . . . . ? C10' C31' C32' C33' -175.6(3) . . . . ? C36' C31' C32' C33' -52.8(4) . . . . ? C31' C32' C33' C34' 55.7(4) . . . . ? C32' C33' C34' C35' -57.2(4) . . . . ? C33' C34' C35' C36' 56.6(4) . . . . ? C34' C35' C36' C31' -55.9(4) . . . . ? C10' C31' C36' C35' 179.1(3) . . . . ? C32' C31' C36' C35' 53.7(4) . . . . ? C13' C12' C37' C42' -104.9(4) . . . . ? C11' C12' C37' C42' 66.0(5) . . . . ? Mn' C12' C37' C42' 151.9(3) . . . . ? C13' C12' C37' C38' 130.5(4) . . . . ? C11' C12' C37' C38' -58.6(5) . . . . ? Mn' C12' C37' C38' 27.3(5) . . . . ? C42' C37' C38' C39' 56.2(5) . . . . ? C12' C37' C38' C39' -177.8(4) . . . . ? C37' C38' C39' C40' -55.2(6) . . . . ? C38' C39' C40' C41' 53.0(7) . . . . ? C39' C40' C41' C42' -51.2(7) . . . . ? C12' C37' C42' C41' -180.0(4) . . . . ? C38' C37' C42' C41' -54.1(6) . . . . ? C40' C41' C42' C37' 52.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 72.50 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.797 _refine_diff_density_min -1.272 _refine_diff_density_rms 0.086 _iucr_refine_instructions_details ; TITL mima17 in P-1 CELL 1.54184 13.358714 15.841949 16.635940 99.2475 92.5088 101.3469 ZERR 4.00 0.0006 0.0006 0.0006 0.004 0.002 0.004 LATT 1 SFAC C H Mn UNIT 168 216 4 SIZE 0.11 0.10 0.09 TEMP -173 ACTA 145 CONF FMAP 2 PLAN 10 L.S. 4 OMIT 3 -6 4 OMIT -1 6 12 OMIT 6 -6 3 OMIT 3 6 4 OMIT -1 9 4 OMIT 4 6 11 OMIT -4 6 9 OMIT -8 6 3 OMIT 4 -9 5 OMIT -9 -3 1 OMIT -1 3 13 WGHT 0.131000 3.253500 FVAR 5.00104 MOLE 1 MN 3 0.211185 0.419529 0.304981 11.00000 0.03259 0.02515 = 0.02604 0.00531 0.00604 0.00577 C1 1 0.173517 0.287471 0.213582 11.00000 0.03238 0.02790 = 0.02325 0.00571 0.00415 0.00682 C2 1 0.242848 0.282040 0.279242 11.00000 0.02761 0.02483 = 0.02799 0.00645 0.00691 0.00621 AFIX 43 H2 2 0.311631 0.275792 0.273790 11.00000 -1.20000 AFIX 0 C3 1 0.195024 0.287246 0.353896 11.00000 0.02922 0.02500 = 0.02513 0.00340 0.00695 0.00472 C4 1 0.091498 0.292768 0.334612 11.00000 0.02745 0.02505 = 0.02513 0.00473 0.00559 0.00463 C5 1 0.077698 0.291604 0.247388 11.00000 0.03097 0.02609 = 0.02777 0.00717 0.00403 0.00485 C6 1 -0.020264 0.293614 0.212540 11.00000 0.03326 0.03228 = 0.03163 0.00738 0.00305 0.00560 AFIX 43 H6 2 -0.031227 0.292311 0.155505 11.00000 -1.20000 AFIX 0 C7 1 -0.099398 0.297481 0.262401 11.00000 0.02739 0.04354 = 0.04475 0.00973 0.00091 0.00855 AFIX 43 H7 2 -0.165225 0.298328 0.238904 11.00000 -1.20000 AFIX 0 C8 1 -0.085377 0.300245 0.348134 11.00000 0.02956 0.04427 = 0.04352 0.01026 0.01288 0.00647 AFIX 43 H8 2 -0.141503 0.303464 0.380832 11.00000 -1.20000 AFIX 0 C9 1 0.007666 0.298324 0.383780 11.00000 0.03391 0.03711 = 0.02928 0.00975 0.01034 0.00912 AFIX 43 H9 2 0.016595 0.300678 0.441123 11.00000 -1.20000 AFIX 0 C10 1 0.160157 0.552586 0.339615 11.00000 0.02741 0.02556 = 0.02235 0.00628 0.00691 0.00338 C11 1 0.237721 0.559068 0.282477 11.00000 0.02530 0.02695 = 0.02534 0.01018 0.00858 0.00656 AFIX 43 H11 2 0.226952 0.567299 0.227691 11.00000 -1.20000 AFIX 0 C12 1 0.332706 0.551464 0.319277 11.00000 0.02827 0.02500 = 0.02705 0.00637 0.00765 0.00756 C13 1 0.316716 0.544561 0.403381 11.00000 0.03422 0.02503 = 0.02783 0.00800 0.01139 0.00697 C14 1 0.210159 0.544606 0.415330 11.00000 0.03241 0.02332 = 0.02760 0.00521 0.00711 0.00549 C15 1 0.174130 0.539153 0.493768 11.00000 0.03231 0.03567 = 0.02865 0.00787 0.01211 0.00569 AFIX 43 H15 2 0.104125 0.538170 0.502454 11.00000 -1.20000 AFIX 0 C17 1 0.345729 0.535324 0.544879 11.00000 0.04180 0.03821 = 0.02703 0.00767 -0.00063 0.00929 AFIX 43 H17 2 0.390311 0.533047 0.590207 11.00000 -1.20000 AFIX 0 C16 1 0.241431 0.535352 0.556389 11.00000 0.04588 0.03897 = 0.02656 0.00790 0.01000 0.00854 AFIX 43 H16 2 0.217718 0.532653 0.609111 11.00000 -1.20000 AFIX 0 C18 1 0.384324 0.538497 0.469995 11.00000 0.03123 0.03199 = 0.02804 0.00858 0.00231 0.00642 AFIX 43 H18 2 0.454073 0.536704 0.462780 11.00000 -1.20000 AFIX 0 C19 1 0.200585 0.280729 0.125168 11.00000 0.03046 0.03504 = 0.02265 0.00611 0.00486 0.00728 AFIX 13 H19 2 0.276787 0.288432 0.126433 11.00000 -1.20000 AFIX 0 C20 1 0.156273 0.189609 0.075644 11.00000 0.03689 0.03372 = 0.02471 0.00584 0.00220 0.00933 AFIX 23 H20A 2 0.180080 0.145089 0.102766 11.00000 -1.20000 H20B 2 0.080604 0.178267 0.074446 11.00000 -1.20000 AFIX 0 C21 1 0.188389 0.180997 -0.011768 11.00000 0.04394 0.04541 = 0.02449 0.00384 0.00659 0.01554 AFIX 23 H21A 2 0.263162 0.183962 -0.010802 11.00000 -1.20000 H21B 2 0.153689 0.123183 -0.042788 11.00000 -1.20000 AFIX 0 C22 1 0.162046 0.252263 -0.055100 11.00000 0.04912 0.04744 = 0.02342 0.00915 0.00571 0.01699 AFIX 23 H22A 2 0.086708 0.244373 -0.063294 11.00000 -1.20000 H22B 2 0.189828 0.247541 -0.109473 11.00000 -1.20000 AFIX 0 C23 1 0.206679 0.342830 -0.005107 11.00000 0.04569 0.04219 = 0.02782 0.01231 0.00855 0.01043 AFIX 23 H23A 2 0.184343 0.387825 -0.032452 11.00000 -1.20000 H23B 2 0.282374 0.353407 -0.002971 11.00000 -1.20000 AFIX 0 C24 1 0.172701 0.351591 0.082131 11.00000 0.03166 0.03632 = 0.02933 0.00661 0.00541 0.00707 AFIX 23 H24A 2 0.206048 0.409709 0.113313 11.00000 -1.20000 H24B 2 0.097673 0.347316 0.080384 11.00000 -1.20000 AFIX 0 C25 1 0.240718 0.280368 0.436942 11.00000 0.02883 0.02829 = 0.02208 0.00496 0.00476 0.00555 AFIX 13 H25 2 0.220232 0.325665 0.478388 11.00000 -1.20000 AFIX 0 C26 1 0.197085 0.189668 0.458844 11.00000 0.03402 0.03466 = 0.02905 0.01114 0.00541 0.00333 AFIX 23 H26A 2 0.121677 0.181171 0.459102 11.00000 -1.20000 H26B 2 0.212902 0.143526 0.416672 11.00000 -1.20000 AFIX 0 C27 1 0.242290 0.180775 0.542868 11.00000 0.03579 0.04153 = 0.03197 0.01600 0.00769 0.00961 AFIX 23 H27A 2 0.219941 0.222544 0.585728 11.00000 -1.20000 H27B 2 0.215882 0.120992 0.553463 11.00000 -1.20000 AFIX 0 C28 1 0.358153 0.198366 0.547457 11.00000 0.03787 0.03604 = 0.03258 0.00937 0.00200 0.01195 AFIX 23 H28A 2 0.380569 0.152308 0.509224 11.00000 -1.20000 H28B 2 0.384746 0.196076 0.603383 11.00000 -1.20000 AFIX 0 C29 1 0.402469 0.287591 0.525921 11.00000 0.03500 0.03598 = 0.03176 0.00725 -0.00070 0.00682 AFIX 23 H29A 2 0.477813 0.295335 0.525653 11.00000 -1.20000 H29B 2 0.387242 0.334027 0.568086 11.00000 -1.20000 AFIX 0 C30 1 0.357942 0.296744 0.442472 11.00000 0.02849 0.03191 = 0.02613 0.00610 0.00335 0.00457 AFIX 23 H30A 2 0.379880 0.254581 0.399738 11.00000 -1.20000 H30B 2 0.385432 0.356334 0.431855 11.00000 -1.20000 AFIX 0 C31 1 0.050995 0.564574 0.330277 11.00000 0.02886 0.03100 = 0.02541 0.00796 0.00805 0.00648 AFIX 13 H31 2 0.009437 0.525594 0.363649 11.00000 -1.20000 AFIX 0 C32 1 0.002799 0.538812 0.242278 11.00000 0.03129 0.04012 = 0.02627 0.00622 0.00561 0.00990 AFIX 23 H32A 2 0.001669 0.476224 0.222557 11.00000 -1.20000 H32B 2 0.045105 0.573347 0.206726 11.00000 -1.20000 AFIX 0 C33 1 -0.107039 0.554777 0.236317 11.00000 0.02898 0.06002 = 0.03398 0.00730 0.00409 0.01070 AFIX 23 H33A 2 -0.133916 0.542095 0.178289 11.00000 -1.20000 H33B 2 -0.151465 0.514412 0.265870 11.00000 -1.20000 AFIX 0 C34 1 -0.110795 0.649246 0.272556 11.00000 0.03570 0.06385 = 0.05570 0.01698 0.01001 0.02426 AFIX 23 H34A 2 -0.072540 0.689269 0.239262 11.00000 -1.20000 H34B 2 -0.182821 0.656301 0.270520 11.00000 -1.20000 AFIX 0 C35 1 -0.065001 0.673666 0.360194 11.00000 0.03450 0.04515 = 0.05538 0.00085 0.00927 0.01611 AFIX 23 H35A 2 -0.107219 0.637788 0.394805 11.00000 -1.20000 H35B 2 -0.064828 0.735889 0.380875 11.00000 -1.20000 AFIX 0 C36 1 0.044469 0.658625 0.365320 11.00000 0.02787 0.03476 = 0.04261 0.00335 0.00882 0.00856 AFIX 23 H36A 2 0.072083 0.672488 0.423186 11.00000 -1.20000 H36B 2 0.087702 0.699014 0.335052 11.00000 -1.20000 AFIX 0 C37 1 0.434790 0.558202 0.282125 11.00000 0.02913 0.03474 = 0.02957 0.01083 0.00912 0.01087 AFIX 13 H37 2 0.484757 0.546042 0.323088 11.00000 -1.20000 AFIX 0 C38 1 0.432167 0.491435 0.203305 11.00000 0.04364 0.03243 = 0.04082 0.00376 0.01749 0.00593 AFIX 23 H38A 2 0.409450 0.431553 0.214917 11.00000 -1.20000 H38B 2 0.382123 0.500960 0.161761 11.00000 -1.20000 AFIX 0 C39 1 0.537749 0.500014 0.169545 11.00000 0.04707 0.04171 = 0.05127 0.00372 0.02581 0.01124 AFIX 23 H39A 2 0.586004 0.484551 0.208864 11.00000 -1.20000 H39B 2 0.532867 0.458245 0.117723 11.00000 -1.20000 AFIX 0 C40 1 0.579534 0.592375 0.154188 11.00000 0.04097 0.05058 = 0.04376 0.01206 0.02203 0.01123 AFIX 23 H40A 2 0.649748 0.596206 0.136280 11.00000 -1.20000 H40B 2 0.536107 0.605304 0.109863 11.00000 -1.20000 AFIX 0 C41 1 0.581566 0.659441 0.230664 11.00000 0.03246 0.03884 = 0.04263 0.01226 0.01060 0.00779 AFIX 23 H41A 2 0.603124 0.718903 0.217756 11.00000 -1.20000 H41B 2 0.632296 0.651534 0.272528 11.00000 -1.20000 AFIX 0 C42 1 0.475826 0.650473 0.264928 11.00000 0.02658 0.03157 = 0.03378 0.00870 0.00670 0.00527 AFIX 23 H42A 2 0.480597 0.693081 0.316184 11.00000 -1.20000 H42B 2 0.426972 0.664746 0.225295 11.00000 -1.20000 AFIX 0 MOLE 2 MN' 3 0.303115 -0.079106 0.210945 11.00000 0.03411 0.02672 = 0.02490 0.00708 0.00849 0.00719 C1' 1 0.372461 -0.160903 0.298594 11.00000 0.03407 0.02675 = 0.02323 0.00582 0.00595 0.00578 C2' 1 0.291836 -0.213826 0.242830 11.00000 0.03142 0.02560 = 0.02380 0.00846 0.00695 0.00424 AFIX 43 H2' 2 0.227371 -0.241547 0.257874 11.00000 -1.20000 AFIX 0 C3' 1 0.321907 -0.219268 0.160738 11.00000 0.02634 0.02471 = 0.02304 0.00582 0.00508 0.00455 C4' 1 0.425493 -0.171310 0.166400 11.00000 0.02804 0.02670 = 0.02196 0.00797 0.00354 0.00696 C5' 1 0.456442 -0.135152 0.251075 11.00000 0.03278 0.02942 = 0.01823 0.00522 0.00434 0.00556 C6' 1 0.556058 -0.083708 0.273266 11.00000 0.03248 0.03363 = 0.02644 0.00445 -0.00120 0.00607 AFIX 43 H6' 2 0.576908 -0.058846 0.328761 11.00000 -1.20000 AFIX 0 C7' 1 0.622030 -0.070279 0.213495 11.00000 0.03284 0.03530 = 0.03873 0.00940 0.00550 0.00381 AFIX 43 H7' 2 0.689120 -0.036194 0.228180 11.00000 -1.20000 AFIX 0 C8' 1 0.592278 -0.106068 0.130606 11.00000 0.02987 0.03745 = 0.03445 0.00992 0.01039 0.00809 AFIX 43 H8' 2 0.639915 -0.095961 0.090695 11.00000 -1.20000 AFIX 0 C9' 1 0.496131 -0.155056 0.106589 11.00000 0.02953 0.03245 = 0.02716 0.00811 0.00819 0.00706 AFIX 43 H9' 2 0.476883 -0.177938 0.050475 11.00000 -1.20000 AFIX 0 C10' 1 0.344462 0.051581 0.163807 11.00000 0.02911 0.02732 = 0.02582 0.00706 0.00835 0.00844 C11' 1 0.266242 0.053473 0.219583 11.00000 0.03308 0.02939 = 0.02929 0.00886 0.01380 0.00928 AFIX 43 H11' 2 0.275272 0.087359 0.272935 11.00000 -1.20000 AFIX 0 C12' 1 0.172448 -0.002852 0.183746 11.00000 0.03043 0.03101 = 0.03934 0.01166 0.01452 0.00644 C13' 1 0.189892 -0.035535 0.101738 11.00000 0.03037 0.02856 = 0.03382 0.01243 0.00649 0.00625 C14' 1 0.296528 -0.003198 0.090012 11.00000 0.02944 0.02520 = 0.02760 0.00847 0.00692 0.00679 C15' 1 0.333830 -0.027652 0.013243 11.00000 0.03172 0.03287 = 0.02592 0.00839 0.00803 0.00574 AFIX 43 H15' 2 0.404237 -0.009299 0.005265 11.00000 -1.20000 AFIX 0 C16' 1 0.267684 -0.078084 -0.049709 11.00000 0.04027 0.03425 = 0.02819 0.00494 0.00574 0.00872 AFIX 43 H16' 2 0.292758 -0.093213 -0.101501 11.00000 -1.20000 AFIX 0 C17' 1 0.162477 -0.108061 -0.038855 11.00000 0.04034 0.03276 = 0.03546 0.00806 0.00005 0.00492 AFIX 43 H17' 2 0.117934 -0.141695 -0.083669 11.00000 -1.20000 AFIX 0 C18' 1 0.124684 -0.088851 0.035774 11.00000 0.02958 0.03359 = 0.03978 0.00986 -0.00055 0.00366 AFIX 43 H18' 2 0.054967 -0.111256 0.043170 11.00000 -1.20000 AFIX 0 C19' 1 0.375197 -0.142672 0.390949 11.00000 0.03204 0.03286 = 0.02239 0.00648 0.00470 0.00171 AFIX 13 H19' 2 0.448914 -0.129191 0.411887 11.00000 -1.20000 AFIX 0 C20' 1 0.323989 -0.221921 0.424476 11.00000 0.05858 0.03305 = 0.02251 0.00437 0.00847 0.00438 AFIX 23 H20C 2 0.357102 -0.271355 0.405157 11.00000 -1.20000 H20D 2 0.251172 -0.238649 0.403189 11.00000 -1.20000 AFIX 0 C21' 1 0.330160 -0.205478 0.517821 11.00000 0.05794 0.03436 = 0.02228 0.00734 0.01133 0.00312 AFIX 23 H21C 2 0.292017 -0.257824 0.536873 11.00000 -1.20000 H21D 2 0.402594 -0.195582 0.539248 11.00000 -1.20000 AFIX 0 C22' 1 0.286146 -0.127188 0.550943 11.00000 0.04774 0.05628 = 0.02372 0.00663 0.01305 0.01849 AFIX 23 H22C 2 0.295601 -0.115745 0.611352 11.00000 -1.20000 H22D 2 0.211777 -0.139576 0.534880 11.00000 -1.20000 AFIX 0 C23' 1 0.338599 -0.047211 0.518173 11.00000 0.09977 0.04217 = 0.02392 0.00346 0.00955 0.02517 AFIX 23 H23C 2 0.411566 -0.031356 0.539083 11.00000 -1.20000 H23D 2 0.306290 0.002584 0.537987 11.00000 -1.20000 AFIX 0 C24' 1 0.331190 -0.063966 0.424209 11.00000 0.10158 0.03918 = 0.02812 0.00826 0.01676 0.02744 AFIX 23 H24C 2 0.258544 -0.073970 0.403300 11.00000 -1.20000 H24D 2 0.368987 -0.011732 0.404773 11.00000 -1.20000 AFIX 0 C25' 1 0.261253 -0.270709 0.083988 11.00000 0.03185 0.02763 = 0.02189 0.00797 0.00539 0.00351 AFIX 13 H25' 2 0.267282 -0.231995 0.041765 11.00000 -1.20000 AFIX 0 C26' 1 0.301739 -0.352107 0.049816 11.00000 0.03283 0.03378 = 0.02430 0.00292 0.00649 0.00248 AFIX 23 H26C 2 0.373948 -0.334212 0.037613 11.00000 -1.20000 H26D 2 0.299894 -0.390187 0.091674 11.00000 -1.20000 AFIX 0 C27' 1 0.238867 -0.403809 -0.027882 11.00000 0.04012 0.04165 = 0.03558 -0.00496 0.00731 -0.00053 AFIX 23 H27C 2 0.245343 -0.367744 -0.071513 11.00000 -1.20000 H27D 2 0.265635 -0.456997 -0.046805 11.00000 -1.20000 AFIX 0 C28' 1 0.126422 -0.429708 -0.011671 11.00000 0.03997 0.04063 = 0.03621 -0.00255 0.00361 -0.00224 AFIX 23 H28C 2 0.086263 -0.460368 -0.063126 11.00000 -1.20000 H28D 2 0.119368 -0.470472 0.028006 11.00000 -1.20000 AFIX 0 C29' 1 0.084288 -0.350130 0.021807 11.00000 0.03199 0.03962 = 0.03546 0.00572 -0.00193 0.00257 AFIX 23 H29C 2 0.012754 -0.369239 0.035118 11.00000 -1.20000 H29D 2 0.083688 -0.312958 -0.020626 11.00000 -1.20000 AFIX 0 C30' 1 0.147380 -0.296677 0.097928 11.00000 0.03118 0.03213 = 0.02751 0.00392 0.00195 0.00490 AFIX 23 H30C 2 0.139942 -0.331127 0.142766 11.00000 -1.20000 H30D 2 0.120517 -0.243145 0.115036 11.00000 -1.20000 AFIX 0 C31' 1 0.450961 0.108281 0.171505 11.00000 0.02795 0.02855 = 0.02334 0.00574 0.00797 0.00878 AFIX 13 H31' 2 0.497630 0.072163 0.144512 11.00000 -1.20000 AFIX 0 C32' 1 0.494325 0.143134 0.260067 11.00000 0.03590 0.03756 = 0.02617 0.00880 0.00437 0.00746 AFIX 23 H32C 2 0.445529 0.173994 0.289502 11.00000 -1.20000 H32D 2 0.501775 0.093365 0.287383 11.00000 -1.20000 AFIX 0 C33' 1 0.598109 0.205561 0.265121 11.00000 0.03510 0.04009 = 0.02753 0.00337 -0.00346 0.00510 AFIX 23 H33C 2 0.621344 0.229105 0.323157 11.00000 -1.20000 H33D 2 0.649000 0.173082 0.241260 11.00000 -1.20000 AFIX 0 C34' 1 0.592532 0.281037 0.219828 11.00000 0.03191 0.03466 = 0.03553 0.00371 0.00082 0.00542 AFIX 23 H34C 2 0.661384 0.319051 0.222623 11.00000 -1.20000 H34D 2 0.546023 0.316541 0.246453 11.00000 -1.20000 AFIX 0 C35' 1 0.553642 0.247002 0.130626 11.00000 0.02883 0.03365 = 0.03192 0.00976 0.00268 0.00340 AFIX 23 H35C 2 0.547372 0.296718 0.102864 11.00000 -1.20000 H35D 2 0.603192 0.215869 0.102618 11.00000 -1.20000 AFIX 0 C36' 1 0.449663 0.185028 0.125351 11.00000 0.02664 0.03198 = 0.02729 0.00830 0.00340 0.00525 AFIX 23 H36C 2 0.427247 0.161401 0.067189 11.00000 -1.20000 H36D 2 0.398957 0.218362 0.148120 11.00000 -1.20000 AFIX 0 C37' 1 0.068425 -0.018059 0.218216 11.00000 0.03216 0.03802 = 0.04661 0.00982 0.01487 0.00396 AFIX 13 H37' 2 0.021666 -0.064610 0.178299 11.00000 -1.20000 AFIX 0 C38' 1 0.071751 -0.051392 0.300191 11.00000 0.04881 0.06219 = 0.05987 0.02998 0.01992 0.01857 AFIX 23 H38C 2 0.098870 -0.105735 0.292868 11.00000 -1.20000 H38D 2 0.118600 -0.007157 0.340951 11.00000 -1.20000 AFIX 0 C39' 1 -0.034999 -0.069494 0.331941 11.00000 0.05327 0.06416 = 0.07781 0.03958 0.03571 0.01895 AFIX 23 H39C 2 -0.079731 -0.118575 0.294401 11.00000 -1.20000 H39D 2 -0.029861 -0.086788 0.386330 11.00000 -1.20000 AFIX 0 C40' 1 -0.082572 0.011584 0.338510 11.00000 0.04678 0.06461 = 0.06798 0.02071 0.02713 0.02038 AFIX 23 H40C 2 -0.153928 -0.003769 0.353595 11.00000 -1.20000 H40D 2 -0.043845 0.057306 0.382664 11.00000 -1.20000 AFIX 0 C41' 1 -0.082620 0.046778 0.262386 11.00000 0.04044 0.05771 = 0.08730 0.02966 0.03353 0.02022 AFIX 23 H41C 2 -0.105588 0.103021 0.272380 11.00000 -1.20000 H41D 2 -0.132529 0.005821 0.221296 11.00000 -1.20000 AFIX 0 C42' 1 0.022609 0.061584 0.227516 11.00000 0.03586 0.04845 = 0.06664 0.02729 0.02375 0.01324 AFIX 23 H42C 2 0.015615 0.079407 0.173513 11.00000 -1.20000 H42D 2 0.069619 0.109988 0.264118 11.00000 -1.20000 HKLF 4 ; # Attachment '- mima29a.cif' data_mima29a _database_code_depnum_ccdc_archive 'CCDC 884309' #TrackingRef '- mima29a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 Co' _chemical_formula_weight 513.64 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' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.1912(12) _cell_length_b 9.6645(4) _cell_length_c 17.7952(10) _cell_angle_alpha 90.00 _cell_angle_beta 116.869(8) _cell_angle_gamma 90.00 _cell_volume 2790.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19959 _cell_measurement_theta_min 4.5716 _cell_measurement_theta_max 75.7794 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 4.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.56386 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31069 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.97 _diffrn_reflns_theta_max 74.47 _reflns_number_total 5697 _reflns_number_gt 5378 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _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 of the C2 and c19 atoms were refined freely. ; _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^)+(0.0413P)^2^+0.5161P] 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 5697 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.002 _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 Co Co 0.738421(11) 0.342889(19) 0.522664(11) 0.01524(7) Uani 1 1 d . . . C1 C 0.75020(7) 0.45347(13) 0.42134(7) 0.0199(2) Uani 1 1 d . . . C2 C 0.71757(8) 0.31767(13) 0.39808(7) 0.0190(2) Uani 1 1 d . . . H2 H 0.7423(10) 0.2444(17) 0.3801(10) 0.021(4) Uiso 1 1 d . . . C3 C 0.64095(7) 0.30303(13) 0.40148(7) 0.0183(2) Uani 1 1 d . . . C4 C 0.62392(7) 0.43636(13) 0.42607(7) 0.0188(2) Uani 1 1 d . . . C5 C 0.69166(8) 0.52870(13) 0.43914(7) 0.0198(2) Uani 1 1 d . . . C6 C 0.68577(9) 0.67146(13) 0.45717(8) 0.0233(3) Uani 1 1 d . . . H6 H 0.7302 0.7328 0.4678 0.028 Uiso 1 1 calc R . . C7 C 0.61594(9) 0.71898(14) 0.45895(8) 0.0259(3) Uani 1 1 d . . . H7 H 0.6116 0.8145 0.4690 0.031 Uiso 1 1 calc R . . C8 C 0.54952(8) 0.62867(15) 0.44607(8) 0.0245(3) Uani 1 1 d . . . H8 H 0.5017 0.6649 0.4478 0.029 Uiso 1 1 calc R . . C9 C 0.55331(8) 0.49076(14) 0.43132(7) 0.0220(2) Uani 1 1 d . . . H9 H 0.5092 0.4312 0.4246 0.026 Uiso 1 1 calc R . . C10 C 0.82208(8) 0.51477(14) 0.41062(8) 0.0232(3) Uani 1 1 d . . . C11 C 0.78837(10) 0.62752(16) 0.34202(9) 0.0305(3) Uani 1 1 d . . . H11A H 0.7461 0.5874 0.2897 0.046 Uiso 1 1 calc R . . H11B H 0.8334 0.6643 0.3321 0.046 Uiso 1 1 calc R . . H11C H 0.7641 0.7024 0.3606 0.046 Uiso 1 1 calc R . . C12 C 0.86266(9) 0.40420(15) 0.37983(9) 0.0288(3) Uani 1 1 d . . . H12A H 0.8820 0.3277 0.4203 0.043 Uiso 1 1 calc R . . H12B H 0.9095 0.4449 0.3747 0.043 Uiso 1 1 calc R . . H12C H 0.8224 0.3693 0.3248 0.043 Uiso 1 1 calc R . . C13 C 0.88782(8) 0.58053(15) 0.49205(8) 0.0277(3) Uani 1 1 d . . . H13A H 0.8619 0.6498 0.5126 0.041 Uiso 1 1 calc R . . H13B H 0.9300 0.6251 0.4805 0.041 Uiso 1 1 calc R . . H13C H 0.9134 0.5086 0.5349 0.041 Uiso 1 1 calc R . . C14 C 0.58218(8) 0.18128(13) 0.36867(8) 0.0199(2) Uani 1 1 d . . . C15 C 0.54238(8) 0.14715(14) 0.42641(8) 0.0244(3) Uani 1 1 d . . . H15A H 0.5848 0.1466 0.4852 0.037 Uiso 1 1 calc R . . H15B H 0.5162 0.0559 0.4117 0.037 Uiso 1 1 calc R . . H15C H 0.5007 0.2172 0.4191 0.037 Uiso 1 1 calc R . . C16 C 0.51370(8) 0.21757(15) 0.28032(8) 0.0276(3) Uani 1 1 d . . . H16A H 0.4838 0.2996 0.2840 0.041 Uiso 1 1 calc R . . H16B H 0.4754 0.1396 0.2583 0.041 Uiso 1 1 calc R . . H16C H 0.5384 0.2366 0.2425 0.041 Uiso 1 1 calc R . . C17 C 0.62781(9) 0.05269(13) 0.36144(8) 0.0252(3) Uani 1 1 d . . . H17A H 0.6510 0.0714 0.3224 0.038 Uiso 1 1 calc R . . H17B H 0.5892 -0.0251 0.3403 0.038 Uiso 1 1 calc R . . H17C H 0.6723 0.0295 0.4170 0.038 Uiso 1 1 calc R . . C18 C 0.83431(8) 0.20754(13) 0.60545(7) 0.0198(2) Uani 1 1 d . . . C19 C 0.84572(8) 0.34718(13) 0.63378(8) 0.0190(2) Uani 1 1 d . . . H19 H 0.8919(10) 0.4064(17) 0.6410(10) 0.022(4) Uiso 1 1 d . . . C20 C 0.77954(7) 0.39106(13) 0.65027(7) 0.0179(2) Uani 1 1 d . . . C21 C 0.73005(7) 0.26843(13) 0.64192(7) 0.0188(2) Uani 1 1 d . . . C22 C 0.76275(8) 0.15649(12) 0.61299(7) 0.0187(2) Uani 1 1 d . . . C23 C 0.72796(8) 0.02281(13) 0.60348(8) 0.0213(2) Uani 1 1 d . . . H23 H 0.7476 -0.0509 0.5821 0.026 Uiso 1 1 calc R . . C24 C 0.66549(8) 0.00041(13) 0.62547(8) 0.0234(3) Uani 1 1 d . . . H24 H 0.6430 -0.0898 0.6204 0.028 Uiso 1 1 calc R . . C25 C 0.63435(8) 0.10922(14) 0.65539(8) 0.0234(3) Uani 1 1 d . . . H25 H 0.5917 0.0910 0.6710 0.028 Uiso 1 1 calc R . . C26 C 0.66483(8) 0.24186(14) 0.66245(7) 0.0214(2) Uani 1 1 d . . . H26 H 0.6421 0.3150 0.6810 0.026 Uiso 1 1 calc R . . C27 C 0.89977(8) 0.11710(14) 0.59879(8) 0.0228(3) Uani 1 1 d . . . C28 C 0.86654(9) 0.03168(15) 0.51733(9) 0.0297(3) Uani 1 1 d . . . H28A H 0.8192 -0.0233 0.5122 0.045 Uiso 1 1 calc R . . H28B H 0.9099 -0.0302 0.5189 0.045 Uiso 1 1 calc R . . H28C H 0.8493 0.0940 0.4689 0.045 Uiso 1 1 calc R . . C29 C 0.97172(8) 0.20580(15) 0.60341(9) 0.0288(3) Uani 1 1 d . . . H29A H 0.9510 0.2742 0.5578 0.043 Uiso 1 1 calc R . . H29B H 1.0124 0.1463 0.5975 0.043 Uiso 1 1 calc R . . H29C H 0.9976 0.2536 0.6578 0.043 Uiso 1 1 calc R . . C30 C 0.93380(8) 0.01843(15) 0.67532(9) 0.0289(3) Uani 1 1 d . . . H30A H 0.9550 0.0727 0.7274 0.043 Uiso 1 1 calc R . . H30B H 0.9784 -0.0375 0.6746 0.043 Uiso 1 1 calc R . . H30C H 0.8896 -0.0426 0.6725 0.043 Uiso 1 1 calc R . . C31 C 0.77895(8) 0.52422(13) 0.69537(7) 0.0193(2) Uani 1 1 d . . . C32 C 0.69186(8) 0.58248(14) 0.66742(8) 0.0237(3) Uani 1 1 d . . . H32A H 0.6632 0.5886 0.6058 0.035 Uiso 1 1 calc R . . H32B H 0.6957 0.6748 0.6916 0.035 Uiso 1 1 calc R . . H32C H 0.6611 0.5212 0.6870 0.035 Uiso 1 1 calc R . . C33 C 0.81775(8) 0.48982(14) 0.79034(7) 0.0230(3) Uani 1 1 d . . . H33A H 0.7853 0.4175 0.8001 0.034 Uiso 1 1 calc R . . H33B H 0.8183 0.5731 0.8220 0.034 Uiso 1 1 calc R . . H33C H 0.8743 0.4571 0.8092 0.034 Uiso 1 1 calc R . . C34 C 0.83070(8) 0.63622(13) 0.68035(8) 0.0235(3) Uani 1 1 d . . . H34A H 0.8877 0.6041 0.7019 0.035 Uiso 1 1 calc R . . H34B H 0.8294 0.7212 0.7098 0.035 Uiso 1 1 calc R . . H34C H 0.8080 0.6548 0.6198 0.035 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 Co 0.01580(10) 0.01532(11) 0.01294(10) 0.00017(7) 0.00502(7) -0.00073(7) C1 0.0210(6) 0.0193(6) 0.0163(5) 0.0009(4) 0.0057(5) -0.0019(5) C2 0.0223(6) 0.0192(6) 0.0144(5) -0.0002(4) 0.0073(5) -0.0014(5) C3 0.0195(5) 0.0189(6) 0.0132(5) 0.0004(4) 0.0046(4) -0.0012(5) C4 0.0213(6) 0.0192(6) 0.0133(5) 0.0006(4) 0.0055(4) -0.0012(5) C5 0.0249(6) 0.0170(6) 0.0144(5) 0.0016(4) 0.0061(5) -0.0014(5) C6 0.0309(7) 0.0182(6) 0.0174(6) 0.0000(4) 0.0078(5) -0.0028(5) C7 0.0378(7) 0.0183(6) 0.0183(6) 0.0010(5) 0.0098(5) 0.0035(5) C8 0.0267(6) 0.0269(7) 0.0182(6) 0.0026(5) 0.0086(5) 0.0068(5) C9 0.0223(6) 0.0254(6) 0.0172(5) 0.0013(5) 0.0078(5) 0.0002(5) C10 0.0241(6) 0.0233(6) 0.0215(6) 0.0014(5) 0.0097(5) -0.0049(5) C11 0.0365(7) 0.0298(7) 0.0248(6) 0.0052(6) 0.0134(6) -0.0058(6) C12 0.0269(6) 0.0313(7) 0.0312(7) 0.0001(6) 0.0158(6) -0.0041(5) C13 0.0249(6) 0.0313(7) 0.0246(6) -0.0005(5) 0.0093(5) -0.0101(5) C14 0.0209(6) 0.0201(6) 0.0161(5) -0.0016(5) 0.0061(5) -0.0040(5) C15 0.0241(6) 0.0257(7) 0.0227(6) -0.0010(5) 0.0101(5) -0.0070(5) C16 0.0269(6) 0.0301(7) 0.0177(6) -0.0002(5) 0.0029(5) -0.0063(5) C17 0.0295(6) 0.0190(6) 0.0263(6) -0.0051(5) 0.0121(5) -0.0061(5) C18 0.0206(6) 0.0201(6) 0.0171(5) 0.0018(5) 0.0072(4) -0.0001(5) C19 0.0183(6) 0.0194(6) 0.0152(5) 0.0007(4) 0.0039(5) -0.0024(4) C20 0.0203(5) 0.0169(6) 0.0140(5) 0.0010(4) 0.0055(4) -0.0011(4) C21 0.0191(5) 0.0179(6) 0.0145(5) -0.0011(4) 0.0034(4) -0.0009(4) C22 0.0186(6) 0.0180(6) 0.0150(5) 0.0014(4) 0.0036(5) 0.0005(4) C23 0.0225(6) 0.0180(6) 0.0195(5) 0.0003(5) 0.0060(5) 0.0005(5) C24 0.0254(6) 0.0184(6) 0.0218(6) 0.0001(5) 0.0066(5) -0.0039(5) C25 0.0222(6) 0.0260(7) 0.0212(6) -0.0018(5) 0.0090(5) -0.0044(5) C26 0.0212(6) 0.0220(6) 0.0200(6) -0.0022(5) 0.0086(5) -0.0017(5) C27 0.0228(6) 0.0215(6) 0.0242(6) 0.0022(5) 0.0108(5) 0.0023(5) C28 0.0308(7) 0.0285(7) 0.0304(7) -0.0035(6) 0.0143(6) 0.0059(5) C29 0.0250(6) 0.0300(7) 0.0342(7) 0.0063(6) 0.0158(6) 0.0039(5) C30 0.0242(6) 0.0288(7) 0.0306(7) 0.0075(6) 0.0096(5) 0.0034(5) C31 0.0232(6) 0.0169(6) 0.0150(5) -0.0007(4) 0.0062(5) -0.0019(5) C32 0.0270(6) 0.0209(6) 0.0210(6) -0.0002(5) 0.0090(5) 0.0020(5) C33 0.0285(6) 0.0212(6) 0.0157(5) -0.0016(5) 0.0070(5) -0.0021(5) C34 0.0299(7) 0.0183(6) 0.0204(6) -0.0023(5) 0.0097(5) -0.0053(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co C19 2.0573(13) . ? Co C2 2.0876(12) . ? Co C20 2.0970(12) . ? Co C3 2.1181(12) . ? Co C18 2.1450(13) . ? Co C1 2.1883(12) . ? Co C4 2.2075(12) . ? Co C5 2.2393(12) . ? Co C21 2.3101(12) . ? Co C22 2.3198(12) . ? C1 C2 1.4227(17) . ? C1 C5 1.4382(18) . ? C1 C10 1.5239(17) . ? C2 C3 1.4292(17) . ? C3 C4 1.4388(17) . ? C3 C14 1.5180(17) . ? C4 C9 1.4296(17) . ? C4 C5 1.4525(17) . ? C5 C6 1.4315(17) . ? C6 C7 1.364(2) . ? C7 C8 1.423(2) . ? C8 C9 1.3663(19) . ? C10 C12 1.5338(19) . ? C10 C13 1.5386(18) . ? C10 C11 1.5418(18) . ? C14 C17 1.5319(18) . ? C14 C15 1.5366(17) . ? C14 C16 1.5415(17) . ? C18 C19 1.4226(18) . ? C18 C22 1.4538(17) . ? C18 C27 1.5244(17) . ? C19 C20 1.4264(17) . ? C20 C21 1.4548(17) . ? C20 C31 1.5193(17) . ? C21 C26 1.4137(17) . ? C21 C22 1.4374(17) . ? C22 C23 1.4147(17) . ? C23 C24 1.3759(19) . ? C24 C25 1.4081(19) . ? C25 C26 1.3798(19) . ? C27 C28 1.5351(19) . ? C27 C29 1.5354(18) . ? C27 C30 1.5445(18) . ? C31 C34 1.5351(17) . ? C31 C32 1.5368(17) . ? C31 C33 1.5448(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Co C2 131.38(5) . . ? C19 Co C20 40.15(5) . . ? C2 Co C20 168.69(5) . . ? C19 Co C3 167.48(5) . . ? C2 Co C3 39.73(5) . . ? C20 Co C3 150.18(5) . . ? C19 Co C18 39.51(5) . . ? C2 Co C18 111.05(5) . . ? C20 Co C18 67.07(5) . . ? C3 Co C18 129.42(5) . . ? C19 Co C1 112.23(5) . . ? C2 Co C1 38.78(5) . . ? C20 Co C1 131.61(5) . . ? C3 Co C1 66.34(5) . . ? C18 Co C1 120.77(5) . . ? C19 Co C4 153.07(5) . . ? C2 Co C4 64.29(5) . . ? C20 Co C4 120.11(5) . . ? C3 Co C4 38.79(5) . . ? C18 Co C4 166.55(5) . . ? C1 Co C4 64.40(4) . . ? C19 Co C5 122.18(5) . . ? C2 Co C5 63.68(5) . . ? C20 Co C5 112.54(5) . . ? C3 Co C5 65.04(5) . . ? C18 Co C5 153.12(5) . . ? C1 Co C5 37.89(5) . . ? C4 Co C5 38.12(4) . . ? C19 Co C21 63.33(5) . . ? C2 Co C21 152.06(5) . . ? C20 Co C21 38.16(4) . . ? C3 Co C21 120.41(4) . . ? C18 Co C21 63.25(4) . . ? C1 Co C21 168.74(5) . . ? C4 Co C21 114.33(4) . . ? C5 Co C21 134.15(4) . . ? C19 Co C22 63.17(5) . . ? C2 Co C22 122.09(5) . . ? C20 Co C22 63.84(4) . . ? C3 Co C22 111.96(5) . . ? C18 Co C22 37.75(4) . . ? C1 Co C22 153.01(5) . . ? C4 Co C22 132.43(4) . . ? C5 Co C22 168.20(5) . . ? C21 Co C22 36.17(4) . . ? C2 C1 C5 106.09(11) . . ? C2 C1 C10 126.23(11) . . ? C5 C1 C10 126.42(11) . . ? C2 C1 Co 66.78(7) . . ? C5 C1 Co 72.98(7) . . ? C10 C1 Co 134.59(9) . . ? C1 C2 C3 111.45(11) . . ? C1 C2 Co 74.44(7) . . ? C3 C2 Co 71.29(7) . . ? C2 C3 C4 105.80(11) . . ? C2 C3 C14 126.24(11) . . ? C4 C3 C14 126.88(11) . . ? C2 C3 Co 68.99(7) . . ? C4 C3 Co 73.97(7) . . ? C14 C3 Co 130.74(8) . . ? C9 C4 C3 132.26(12) . . ? C9 C4 C5 119.07(11) . . ? C3 C4 C5 108.38(11) . . ? C9 C4 Co 131.23(8) . . ? C3 C4 Co 67.25(7) . . ? C5 C4 Co 72.12(7) . . ? C6 C5 C1 132.42(12) . . ? C6 C5 C4 118.95(12) . . ? C1 C5 C4 108.25(11) . . ? C6 C5 Co 131.96(9) . . ? C1 C5 Co 69.14(7) . . ? C4 C5 Co 69.75(7) . . ? C7 C6 C5 119.63(12) . . ? C6 C7 C8 121.44(12) . . ? C9 C8 C7 121.10(12) . . ? C8 C9 C4 119.75(12) . . ? C1 C10 C12 110.64(11) . . ? C1 C10 C13 112.86(10) . . ? C12 C10 C13 109.24(11) . . ? C1 C10 C11 108.49(11) . . ? C12 C10 C11 107.03(11) . . ? C13 C10 C11 108.39(11) . . ? C3 C14 C17 110.30(10) . . ? C3 C14 C15 111.83(10) . . ? C17 C14 C15 108.60(11) . . ? C3 C14 C16 108.66(10) . . ? C17 C14 C16 108.53(10) . . ? C15 C14 C16 108.85(11) . . ? C19 C18 C22 106.42(11) . . ? C19 C18 C27 125.27(11) . . ? C22 C18 C27 125.17(11) . . ? C19 C18 Co 66.92(7) . . ? C22 C18 Co 77.66(7) . . ? C27 C18 Co 135.86(9) . . ? C18 C19 C20 110.69(11) . . ? C18 C19 Co 73.57(7) . . ? C20 C19 Co 71.42(7) . . ? C19 C20 C21 106.12(10) . . ? C19 C20 C31 124.66(11) . . ? C21 C20 C31 126.32(11) . . ? C19 C20 Co 68.43(7) . . ? C21 C20 Co 78.88(7) . . ? C31 C20 Co 132.52(8) . . ? C26 C21 C22 119.17(11) . . ? C26 C21 C20 132.41(11) . . ? C22 C21 C20 108.22(11) . . ? C26 C21 Co 134.86(9) . . ? C22 C21 Co 72.28(7) . . ? C20 C21 Co 62.96(6) . . ? C23 C22 C21 119.67(11) . . ? C23 C22 C18 132.04(12) . . ? C21 C22 C18 108.08(11) . . ? C23 C22 Co 133.74(9) . . ? C21 C22 Co 71.55(7) . . ? C18 C22 Co 64.59(7) . . ? C24 C23 C22 119.47(12) . . ? C23 C24 C25 121.01(12) . . ? C26 C25 C24 120.96(12) . . ? C25 C26 C21 119.66(12) . . ? C18 C27 C28 113.19(11) . . ? C18 C27 C29 110.65(11) . . ? C28 C27 C29 108.25(11) . . ? C18 C27 C30 107.54(10) . . ? C28 C27 C30 109.30(11) . . ? C29 C27 C30 107.78(11) . . ? C20 C31 C34 110.73(10) . . ? C20 C31 C32 113.06(10) . . ? C34 C31 C32 108.00(10) . . ? C20 C31 C33 106.66(10) . . ? C34 C31 C33 109.22(10) . . ? C32 C31 C33 109.11(10) . . ? 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 C19 Co C1 C2 129.16(8) . . . . ? C20 Co C1 C2 171.32(7) . . . . ? C3 Co C1 C2 -37.32(7) . . . . ? C18 Co C1 C2 85.77(8) . . . . ? C4 Co C1 C2 -80.12(8) . . . . ? C5 Co C1 C2 -116.54(10) . . . . ? C21 Co C1 C2 -166.3(2) . . . . ? C22 Co C1 C2 54.92(13) . . . . ? C19 Co C1 C5 -114.30(7) . . . . ? C2 Co C1 C5 116.54(10) . . . . ? C20 Co C1 C5 -72.14(9) . . . . ? C3 Co C1 C5 79.22(7) . . . . ? C18 Co C1 C5 -157.69(7) . . . . ? C4 Co C1 C5 36.42(7) . . . . ? C21 Co C1 C5 -49.8(2) . . . . ? C22 Co C1 C5 171.46(9) . . . . ? C19 Co C1 C10 10.46(14) . . . . ? C2 Co C1 C10 -118.70(15) . . . . ? C20 Co C1 C10 52.62(15) . . . . ? C3 Co C1 C10 -156.02(14) . . . . ? C18 Co C1 C10 -32.93(14) . . . . ? C4 Co C1 C10 161.18(14) . . . . ? C5 Co C1 C10 124.76(15) . . . . ? C21 Co C1 C10 75.0(3) . . . . ? C22 Co C1 C10 -63.78(17) . . . . ? C5 C1 C2 C3 -0.77(14) . . . . ? C10 C1 C2 C3 -168.60(11) . . . . ? Co C1 C2 C3 62.15(8) . . . . ? C5 C1 C2 Co -62.91(8) . . . . ? C10 C1 C2 Co 129.25(12) . . . . ? C19 Co C2 C1 -73.05(9) . . . . ? C20 Co C2 C1 -35.1(3) . . . . ? C3 Co C2 C1 119.68(11) . . . . ? C18 Co C2 C1 -113.34(8) . . . . ? C4 Co C2 C1 80.41(8) . . . . ? C5 Co C2 C1 37.80(7) . . . . ? C21 Co C2 C1 174.33(9) . . . . ? C22 Co C2 C1 -154.00(7) . . . . ? C19 Co C2 C3 167.27(7) . . . . ? C20 Co C2 C3 -154.8(2) . . . . ? C18 Co C2 C3 126.98(7) . . . . ? C1 Co C2 C3 -119.68(11) . . . . ? C4 Co C2 C3 -39.26(7) . . . . ? C5 Co C2 C3 -81.88(8) . . . . ? C21 Co C2 C3 54.65(13) . . . . ? C22 Co C2 C3 86.32(8) . . . . ? C1 C2 C3 C4 1.34(13) . . . . ? Co C2 C3 C4 65.40(8) . . . . ? C1 C2 C3 C14 170.11(11) . . . . ? Co C2 C3 C14 -125.82(12) . . . . ? C1 C2 C3 Co -64.06(9) . . . . ? C19 Co C3 C2 -49.7(2) . . . . ? C20 Co C3 C2 170.34(9) . . . . ? C18 Co C3 C2 -74.83(9) . . . . ? C1 Co C3 C2 36.45(7) . . . . ? C4 Co C3 C2 114.45(10) . . . . ? C5 Co C3 C2 78.16(8) . . . . ? C21 Co C3 C2 -153.69(7) . . . . ? C22 Co C3 C2 -114.28(7) . . . . ? C19 Co C3 C4 -164.1(2) . . . . ? C2 Co C3 C4 -114.45(10) . . . . ? C20 Co C3 C4 55.89(12) . . . . ? C18 Co C3 C4 170.72(7) . . . . ? C1 Co C3 C4 -78.00(7) . . . . ? C5 Co C3 C4 -36.29(7) . . . . ? C21 Co C3 C4 91.86(8) . . . . ? C22 Co C3 C4 131.27(7) . . . . ? C19 Co C3 C14 70.7(3) . . . . ? C2 Co C3 C14 120.33(14) . . . . ? C20 Co C3 C14 -69.33(16) . . . . ? C18 Co C3 C14 45.50(13) . . . . ? C1 Co C3 C14 156.78(13) . . . . ? C4 Co C3 C14 -125.22(14) . . . . ? C5 Co C3 C14 -161.51(13) . . . . ? C21 Co C3 C14 -33.36(13) . . . . ? C22 Co C3 C14 6.05(13) . . . . ? C2 C3 C4 C9 172.20(12) . . . . ? C14 C3 C4 C9 3.5(2) . . . . ? Co C3 C4 C9 -125.77(13) . . . . ? C2 C3 C4 C5 -1.37(13) . . . . ? C14 C3 C4 C5 -170.05(11) . . . . ? Co C3 C4 C5 60.65(8) . . . . ? C2 C3 C4 Co -62.02(8) . . . . ? C14 C3 C4 Co 129.30(12) . . . . ? C19 Co C4 C9 -60.51(17) . . . . ? C2 Co C4 C9 167.24(14) . . . . ? C20 Co C4 C9 -24.56(14) . . . . ? C3 Co C4 C9 127.02(15) . . . . ? C18 Co C4 C9 94.6(2) . . . . ? C1 Co C4 C9 -149.54(14) . . . . ? C5 Co C4 C9 -113.34(15) . . . . ? C21 Co C4 C9 18.11(14) . . . . ? C22 Co C4 C9 56.21(14) . . . . ? C19 Co C4 C3 172.47(10) . . . . ? C2 Co C4 C3 40.22(7) . . . . ? C20 Co C4 C3 -151.58(7) . . . . ? C18 Co C4 C3 -32.4(2) . . . . ? C1 Co C4 C3 83.44(7) . . . . ? C5 Co C4 C3 119.64(10) . . . . ? C21 Co C4 C3 -108.91(7) . . . . ? C22 Co C4 C3 -70.81(9) . . . . ? C19 Co C4 C5 52.83(13) . . . . ? C2 Co C4 C5 -79.42(7) . . . . ? C20 Co C4 C5 88.78(8) . . . . ? C3 Co C4 C5 -119.64(10) . . . . ? C18 Co C4 C5 -152.02(18) . . . . ? C1 Co C4 C5 -36.20(7) . . . . ? C21 Co C4 C5 131.45(7) . . . . ? C22 Co C4 C5 169.55(7) . . . . ? C2 C1 C5 C6 -172.77(13) . . . . ? C10 C1 C5 C6 -5.0(2) . . . . ? Co C1 C5 C6 128.39(14) . . . . ? C2 C1 C5 C4 -0.12(13) . . . . ? C10 C1 C5 C4 167.68(11) . . . . ? Co C1 C5 C4 -58.96(8) . . . . ? C2 C1 C5 Co 58.84(8) . . . . ? C10 C1 C5 Co -133.36(12) . . . . ? C9 C4 C5 C6 0.19(17) . . . . ? C3 C4 C5 C6 174.75(10) . . . . ? Co C4 C5 C6 -127.62(11) . . . . ? C9 C4 C5 C1 -173.62(10) . . . . ? C3 C4 C5 C1 0.95(13) . . . . ? Co C4 C5 C1 58.58(8) . . . . ? C9 C4 C5 Co 127.81(11) . . . . ? C3 C4 C5 Co -57.63(8) . . . . ? C19 Co C5 C6 -43.53(14) . . . . ? C2 Co C5 C6 -167.60(14) . . . . ? C20 Co C5 C6 0.69(14) . . . . ? C3 Co C5 C6 148.15(14) . . . . ? C18 Co C5 C6 -82.73(16) . . . . ? C1 Co C5 C6 -128.90(16) . . . . ? C4 Co C5 C6 111.24(15) . . . . ? C21 Co C5 C6 39.10(15) . . . . ? C22 Co C5 C6 70.3(3) . . . . ? C19 Co C5 C1 85.38(8) . . . . ? C2 Co C5 C1 -38.69(7) . . . . ? C20 Co C5 C1 129.60(7) . . . . ? C3 Co C5 C1 -82.95(7) . . . . ? C18 Co C5 C1 46.18(13) . . . . ? C4 Co C5 C1 -119.86(10) . . . . ? C21 Co C5 C1 168.01(7) . . . . ? C22 Co C5 C1 -160.76(19) . . . . ? C19 Co C5 C4 -154.76(7) . . . . ? C2 Co C5 C4 81.17(7) . . . . ? C20 Co C5 C4 -110.54(7) . . . . ? C3 Co C5 C4 36.91(7) . . . . ? C18 Co C5 C4 166.03(9) . . . . ? C1 Co C5 C4 119.86(10) . . . . ? C21 Co C5 C4 -72.13(9) . . . . ? C22 Co C5 C4 -40.9(2) . . . . ? C1 C5 C6 C7 169.84(13) . . . . ? C4 C5 C6 C7 -2.18(17) . . . . ? Co C5 C6 C7 -90.21(15) . . . . ? C5 C6 C7 C8 2.18(19) . . . . ? C6 C7 C8 C9 -0.09(19) . . . . ? C7 C8 C9 C4 -1.95(18) . . . . ? C3 C4 C9 C8 -171.16(12) . . . . ? C5 C4 C9 C8 1.86(17) . . . . ? Co C4 C9 C8 93.02(14) . . . . ? C2 C1 C10 C12 -6.47(17) . . . . ? C5 C1 C10 C12 -171.90(11) . . . . ? Co C1 C10 C12 85.60(14) . . . . ? C2 C1 C10 C13 -129.21(13) . . . . ? C5 C1 C10 C13 65.36(16) . . . . ? Co C1 C10 C13 -37.15(18) . . . . ? C2 C1 C10 C11 110.66(14) . . . . ? C5 C1 C10 C11 -54.77(16) . . . . ? Co C1 C10 C11 -157.28(10) . . . . ? C2 C3 C14 C17 21.40(16) . . . . ? C4 C3 C14 C17 -172.15(11) . . . . ? Co C3 C14 C17 -71.16(14) . . . . ? C2 C3 C14 C15 142.37(12) . . . . ? C4 C3 C14 C15 -51.17(16) . . . . ? Co C3 C14 C15 49.81(15) . . . . ? C2 C3 C14 C16 -97.46(14) . . . . ? C4 C3 C14 C16 69.00(15) . . . . ? Co C3 C14 C16 169.99(9) . . . . ? C2 Co C18 C19 130.29(7) . . . . ? C20 Co C18 C19 -37.68(7) . . . . ? C3 Co C18 C19 171.67(7) . . . . ? C1 Co C18 C19 88.28(8) . . . . ? C4 Co C18 C19 -162.59(17) . . . . ? C5 Co C18 C19 57.24(13) . . . . ? C21 Co C18 C19 -79.71(8) . . . . ? C22 Co C18 C19 -114.06(10) . . . . ? C19 Co C18 C22 114.06(10) . . . . ? C2 Co C18 C22 -115.65(7) . . . . ? C20 Co C18 C22 76.38(7) . . . . ? C3 Co C18 C22 -74.27(9) . . . . ? C1 Co C18 C22 -157.66(7) . . . . ? C4 Co C18 C22 -48.5(2) . . . . ? C5 Co C18 C22 171.30(9) . . . . ? C21 Co C18 C22 34.35(7) . . . . ? C19 Co C18 C27 -117.53(16) . . . . ? C2 Co C18 C27 12.76(14) . . . . ? C20 Co C18 C27 -155.21(14) . . . . ? C3 Co C18 C27 54.14(15) . . . . ? C1 Co C18 C27 -29.25(15) . . . . ? C4 Co C18 C27 79.9(2) . . . . ? C5 Co C18 C27 -60.29(18) . . . . ? C21 Co C18 C27 162.76(14) . . . . ? C22 Co C18 C27 128.41(16) . . . . ? C22 C18 C19 C20 -6.23(13) . . . . ? C27 C18 C19 C20 -166.95(11) . . . . ? Co C18 C19 C20 62.20(8) . . . . ? C22 C18 C19 Co -68.42(8) . . . . ? C27 C18 C19 Co 130.85(12) . . . . ? C2 Co C19 C18 -71.57(9) . . . . ? C20 Co C19 C18 119.19(10) . . . . ? C3 Co C19 C18 -31.1(2) . . . . ? C1 Co C19 C18 -111.91(7) . . . . ? C4 Co C19 C18 171.16(9) . . . . ? C5 Co C19 C18 -153.30(7) . . . . ? C21 Co C19 C18 79.47(7) . . . . ? C22 Co C19 C18 38.79(7) . . . . ? C2 Co C19 C20 169.23(7) . . . . ? C3 Co C19 C20 -150.3(2) . . . . ? C18 Co C19 C20 -119.19(10) . . . . ? C1 Co C19 C20 128.90(7) . . . . ? C4 Co C19 C20 51.97(13) . . . . ? C5 Co C19 C20 87.50(8) . . . . ? C21 Co C19 C20 -39.72(7) . . . . ? C22 Co C19 C20 -80.41(7) . . . . ? C18 C19 C20 C21 7.20(13) . . . . ? Co C19 C20 C21 70.72(8) . . . . ? C18 C19 C20 C31 168.87(11) . . . . ? Co C19 C20 C31 -127.61(11) . . . . ? C18 C19 C20 Co -63.52(9) . . . . ? C2 Co C20 C19 -45.6(3) . . . . ? C3 Co C20 C19 167.51(9) . . . . ? C18 Co C20 C19 37.09(7) . . . . ? C1 Co C20 C19 -74.46(9) . . . . ? C4 Co C20 C19 -155.65(7) . . . . ? C5 Co C20 C19 -113.72(7) . . . . ? C21 Co C20 C19 112.46(10) . . . . ? C22 Co C20 C19 78.61(7) . . . . ? C19 Co C20 C21 -112.46(10) . . . . ? C2 Co C20 C21 -158.1(2) . . . . ? C3 Co C20 C21 55.06(13) . . . . ? C18 Co C20 C21 -75.37(7) . . . . ? C1 Co C20 C21 173.08(7) . . . . ? C4 Co C20 C21 91.89(8) . . . . ? C5 Co C20 C21 133.82(7) . . . . ? C22 Co C20 C21 -33.85(7) . . . . ? C19 Co C20 C31 117.85(14) . . . . ? C2 Co C20 C31 72.2(3) . . . . ? C3 Co C20 C31 -74.64(15) . . . . ? C18 Co C20 C31 154.93(13) . . . . ? C1 Co C20 C31 43.39(14) . . . . ? C4 Co C20 C31 -37.80(13) . . . . ? C5 Co C20 C31 4.13(13) . . . . ? C21 Co C20 C31 -129.70(15) . . . . ? C22 Co C20 C31 -163.54(13) . . . . ? C19 C20 C21 C26 169.21(13) . . . . ? C31 C20 C21 C26 7.9(2) . . . . ? Co C20 C21 C26 -127.33(13) . . . . ? C19 C20 C21 C22 -5.31(13) . . . . ? C31 C20 C21 C22 -166.59(11) . . . . ? Co C20 C21 C22 58.15(8) . . . . ? C19 C20 C21 Co -63.46(8) . . . . ? C31 C20 C21 Co 135.27(12) . . . . ? C19 Co C21 C26 165.89(14) . . . . ? C2 Co C21 C26 -64.91(17) . . . . ? C20 Co C21 C26 124.07(16) . . . . ? C3 Co C21 C26 -27.72(14) . . . . ? C18 Co C21 C26 -149.64(14) . . . . ? C1 Co C21 C26 96.6(2) . . . . ? C4 Co C21 C26 15.68(14) . . . . ? C5 Co C21 C26 55.84(15) . . . . ? C22 Co C21 C26 -113.82(15) . . . . ? C19 Co C21 C22 -80.29(8) . . . . ? C2 Co C21 C22 48.91(13) . . . . ? C20 Co C21 C22 -122.11(10) . . . . ? C3 Co C21 C22 86.10(8) . . . . ? C18 Co C21 C22 -35.83(7) . . . . ? C1 Co C21 C22 -149.6(2) . . . . ? C4 Co C21 C22 129.50(7) . . . . ? C5 Co C21 C22 169.65(7) . . . . ? C19 Co C21 C20 41.82(7) . . . . ? C2 Co C21 C20 171.02(10) . . . . ? C3 Co C21 C20 -151.80(7) . . . . ? C18 Co C21 C20 86.28(8) . . . . ? C1 Co C21 C20 -27.4(3) . . . . ? C4 Co C21 C20 -108.39(8) . . . . ? C5 Co C21 C20 -68.24(9) . . . . ? C22 Co C21 C20 122.11(10) . . . . ? C26 C21 C22 C23 1.60(17) . . . . ? C20 C21 C22 C23 176.97(10) . . . . ? Co C21 C22 C23 -130.45(11) . . . . ? C26 C21 C22 C18 -173.74(10) . . . . ? C20 C21 C22 C18 1.63(13) . . . . ? Co C21 C22 C18 54.21(8) . . . . ? C26 C21 C22 Co 132.04(11) . . . . ? C20 C21 C22 Co -52.58(8) . . . . ? C19 C18 C22 C23 -171.83(13) . . . . ? C27 C18 C22 C23 -11.1(2) . . . . ? Co C18 C22 C23 127.04(14) . . . . ? C19 C18 C22 C21 2.71(13) . . . . ? C27 C18 C22 C21 163.46(11) . . . . ? Co C18 C22 C21 -58.42(8) . . . . ? C19 C18 C22 Co 61.13(8) . . . . ? C27 C18 C22 Co -138.12(12) . . . . ? C19 Co C22 C23 -165.47(14) . . . . ? C2 Co C22 C23 -41.60(14) . . . . ? C20 Co C22 C23 149.43(14) . . . . ? C3 Co C22 C23 1.84(14) . . . . ? C18 Co C22 C23 -124.86(16) . . . . ? C1 Co C22 C23 -78.84(16) . . . . ? C4 Co C22 C23 41.48(15) . . . . ? C5 Co C22 C23 74.7(3) . . . . ? C21 Co C22 C23 113.76(15) . . . . ? C19 Co C22 C21 80.77(8) . . . . ? C2 Co C22 C21 -155.36(7) . . . . ? C20 Co C22 C21 35.67(7) . . . . ? C3 Co C22 C21 -111.92(7) . . . . ? C18 Co C22 C21 121.38(10) . . . . ? C1 Co C22 C21 167.41(9) . . . . ? C4 Co C22 C21 -72.28(9) . . . . ? C5 Co C22 C21 -39.1(2) . . . . ? C19 Co C22 C18 -40.61(7) . . . . ? C2 Co C22 C18 83.26(8) . . . . ? C20 Co C22 C18 -85.71(8) . . . . ? C3 Co C22 C18 126.71(7) . . . . ? C1 Co C22 C18 46.03(13) . . . . ? C4 Co C22 C18 166.34(7) . . . . ? C5 Co C22 C18 -160.5(2) . . . . ? C21 Co C22 C18 -121.38(10) . . . . ? C21 C22 C23 C24 -2.73(18) . . . . ? C18 C22 C23 C24 171.30(13) . . . . ? Co C22 C23 C24 -95.07(15) . . . . ? C22 C23 C24 C25 1.52(19) . . . . ? C23 C24 C25 C26 0.89(19) . . . . ? C24 C25 C26 C21 -2.02(19) . . . . ? C22 C21 C26 C25 0.77(17) . . . . ? C20 C21 C26 C25 -173.28(12) . . . . ? Co C21 C26 C25 94.42(15) . . . . ? C19 C18 C27 C28 -137.08(13) . . . . ? C22 C18 C27 C28 65.71(16) . . . . ? Co C18 C27 C28 -44.82(18) . . . . ? C19 C18 C27 C29 -15.38(17) . . . . ? C22 C18 C27 C29 -172.59(11) . . . . ? Co C18 C27 C29 76.88(15) . . . . ? C19 C18 C27 C30 102.10(14) . . . . ? C22 C18 C27 C30 -55.12(16) . . . . ? Co C18 C27 C30 -165.65(10) . . . . ? C19 C20 C31 C34 29.66(16) . . . . ? C21 C20 C31 C34 -172.36(11) . . . . ? Co C20 C31 C34 -61.91(15) . . . . ? C19 C20 C31 C32 151.01(11) . . . . ? C21 C20 C31 C32 -51.01(16) . . . . ? Co C20 C31 C32 59.43(15) . . . . ? C19 C20 C31 C33 -89.07(13) . . . . ? C21 C20 C31 C33 68.91(15) . . . . ? Co C20 C31 C33 179.35(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 74.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.291 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.040 _iucr_refine_instructions_details ; TITL mima29a in P2(1)/c CELL 1.54184 18.1912 9.6645 17.7952 90.000 116.869 90.000 ZERR 4.00 0.0012 0.0004 0.0010 0.000 0.008 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H CO UNIT 136 184 4 SIZE 0.20 0.13 0.05 TEMP -173 SHEL 999 0.80 ACTA CONF FMAP 2 PLAN 10 L.S. 8 OMIT -8 2 3 OMIT -22 0 14 OMIT -6 3 1 OMIT 5 6 14 OMIT -13 9 5 OMIT 1 11 7 OMIT -14 9 9 OMIT 2 9 12 OMIT 7 10 5 OMIT 5 8 12 OMIT 3 9 11 OMIT -22 1 5 OMIT 0 11 8 OMIT -12 10 7 OMIT 8 7 11 OMIT -17 8 7 WGHT 0.041300 0.516100 FVAR 4.09169 CO 3 0.738421 0.342889 0.522664 11.00000 0.01580 0.01532 = 0.01294 0.00017 0.00502 -0.00073 C1 1 0.750205 0.453472 0.421337 11.00000 0.02096 0.01925 = 0.01625 0.00092 0.00565 -0.00192 C2 1 0.717570 0.317668 0.398084 11.00000 0.02228 0.01920 = 0.01435 -0.00024 0.00732 -0.00141 H2 2 0.742323 0.244427 0.380059 11.00000 0.02088 C3 1 0.640948 0.303029 0.401484 11.00000 0.01949 0.01885 = 0.01322 0.00043 0.00458 -0.00123 C4 1 0.623919 0.436361 0.426066 11.00000 0.02132 0.01918 = 0.01334 0.00065 0.00552 -0.00120 C5 1 0.691660 0.528697 0.439145 11.00000 0.02485 0.01698 = 0.01438 0.00163 0.00615 -0.00140 C6 1 0.685772 0.671463 0.457172 11.00000 0.03092 0.01821 = 0.01737 -0.00003 0.00784 -0.00281 AFIX 43 H6 2 0.730231 0.732776 0.467840 11.00000 -1.20000 AFIX 0 C7 1 0.615942 0.718983 0.458946 11.00000 0.03783 0.01830 = 0.01833 0.00105 0.00983 0.00346 AFIX 43 H7 2 0.611583 0.814458 0.468997 11.00000 -1.20000 AFIX 0 C8 1 0.549518 0.628673 0.446074 11.00000 0.02668 0.02692 = 0.01819 0.00259 0.00860 0.00685 AFIX 43 H8 2 0.501735 0.664871 0.447766 11.00000 -1.20000 AFIX 0 C9 1 0.553305 0.490757 0.431319 11.00000 0.02229 0.02537 = 0.01721 0.00134 0.00783 0.00022 AFIX 43 H9 2 0.509183 0.431234 0.424576 11.00000 -1.20000 AFIX 0 C10 1 0.822082 0.514773 0.410624 11.00000 0.02415 0.02334 = 0.02148 0.00138 0.00968 -0.00491 C11 1 0.788374 0.627516 0.342020 11.00000 0.03653 0.02976 = 0.02482 0.00516 0.01344 -0.00579 AFIX 137 H11A 2 0.746128 0.587443 0.289713 11.00000 -1.50000 H11B 2 0.833442 0.664333 0.332116 11.00000 -1.50000 H11C 2 0.764126 0.702435 0.360622 11.00000 -1.50000 AFIX 0 C12 1 0.862657 0.404200 0.379831 11.00000 0.02693 0.03128 = 0.03125 0.00008 0.01581 -0.00414 AFIX 137 H12A 2 0.881989 0.327724 0.420337 11.00000 -1.50000 H12B 2 0.909516 0.444885 0.374671 11.00000 -1.50000 H12C 2 0.822390 0.369345 0.324810 11.00000 -1.50000 AFIX 0 C13 1 0.887825 0.580534 0.492048 11.00000 0.02490 0.03130 = 0.02462 -0.00052 0.00929 -0.01014 AFIX 137 H13A 2 0.861896 0.649786 0.512614 11.00000 -1.50000 H13B 2 0.930049 0.625097 0.480499 11.00000 -1.50000 H13C 2 0.913404 0.508605 0.534894 11.00000 -1.50000 AFIX 0 C14 1 0.582176 0.181276 0.368665 11.00000 0.02090 0.02009 = 0.01607 -0.00156 0.00614 -0.00400 C15 1 0.542378 0.147146 0.426405 11.00000 0.02415 0.02567 = 0.02274 -0.00096 0.01011 -0.00703 AFIX 137 H15A 2 0.584803 0.146605 0.485199 11.00000 -1.50000 H15B 2 0.516219 0.055878 0.411700 11.00000 -1.50000 H15C 2 0.500731 0.217188 0.419143 11.00000 -1.50000 AFIX 0 C16 1 0.513699 0.217566 0.280320 11.00000 0.02694 0.03007 = 0.01766 -0.00017 0.00286 -0.00632 AFIX 137 H16A 2 0.483799 0.299590 0.283970 11.00000 -1.50000 H16B 2 0.475411 0.139552 0.258310 11.00000 -1.50000 H16C 2 0.538351 0.236628 0.242513 11.00000 -1.50000 AFIX 0 C17 1 0.627812 0.052687 0.361438 11.00000 0.02952 0.01901 = 0.02633 -0.00508 0.01210 -0.00605 AFIX 137 H17A 2 0.651043 0.071443 0.322369 11.00000 -1.50000 H17B 2 0.589242 -0.025103 0.340316 11.00000 -1.50000 H17C 2 0.672345 0.029460 0.417006 11.00000 -1.50000 AFIX 0 C18 1 0.834305 0.207543 0.605450 11.00000 0.02061 0.02010 = 0.01709 0.00182 0.00723 -0.00011 C19 1 0.845716 0.347183 0.633776 11.00000 0.01827 0.01943 = 0.01519 0.00065 0.00391 -0.00245 H19 2 0.891855 0.406368 0.641005 11.00000 0.02200 C20 1 0.779537 0.391065 0.650269 11.00000 0.02033 0.01691 = 0.01398 0.00100 0.00551 -0.00113 C21 1 0.730049 0.268426 0.641918 11.00000 0.01915 0.01786 = 0.01450 -0.00114 0.00338 -0.00093 C22 1 0.762749 0.156492 0.612986 11.00000 0.01861 0.01801 = 0.01503 0.00140 0.00359 0.00046 C23 1 0.727962 0.022812 0.603484 11.00000 0.02251 0.01804 = 0.01947 0.00026 0.00596 0.00045 AFIX 43 H23 2 0.747575 -0.050901 0.582092 11.00000 -1.20000 AFIX 0 C24 1 0.665495 0.000413 0.625474 11.00000 0.02539 0.01839 = 0.02182 0.00010 0.00660 -0.00389 AFIX 43 H24 2 0.643032 -0.089835 0.620393 11.00000 -1.20000 AFIX 0 C25 1 0.634355 0.109216 0.655395 11.00000 0.02225 0.02596 = 0.02116 -0.00180 0.00900 -0.00442 AFIX 43 H25 2 0.591740 0.091027 0.670952 11.00000 -1.20000 AFIX 0 C26 1 0.664833 0.241864 0.662446 11.00000 0.02124 0.02202 = 0.02004 -0.00217 0.00858 -0.00173 AFIX 43 H26 2 0.642110 0.314973 0.681001 11.00000 -1.20000 AFIX 0 C27 1 0.899769 0.117105 0.598792 11.00000 0.02284 0.02145 = 0.02425 0.00221 0.01076 0.00232 C28 1 0.866539 0.031676 0.517330 11.00000 0.03081 0.02847 = 0.03037 -0.00345 0.01433 0.00589 AFIX 137 H28A 2 0.819238 -0.023290 0.512244 11.00000 -1.50000 H28B 2 0.909875 -0.030215 0.518874 11.00000 -1.50000 H28C 2 0.849291 0.093996 0.468865 11.00000 -1.50000 AFIX 0 C29 1 0.971718 0.205799 0.603409 11.00000 0.02504 0.02998 = 0.03417 0.00631 0.01584 0.00386 AFIX 137 H29A 2 0.951048 0.274203 0.557839 11.00000 -1.50000 H29B 2 1.012408 0.146254 0.597504 11.00000 -1.50000 H29C 2 0.997623 0.253551 0.657830 11.00000 -1.50000 AFIX 0 C30 1 0.933796 0.018432 0.675325 11.00000 0.02419 0.02879 = 0.03061 0.00749 0.00965 0.00337 AFIX 137 H30A 2 0.954972 0.072707 0.727430 11.00000 -1.50000 H30B 2 0.978434 -0.037459 0.674629 11.00000 -1.50000 H30C 2 0.889572 -0.042561 0.672478 11.00000 -1.50000 AFIX 0 C31 1 0.778945 0.524225 0.695368 11.00000 0.02320 0.01686 = 0.01501 -0.00070 0.00617 -0.00192 C32 1 0.691859 0.582476 0.667425 11.00000 0.02695 0.02091 = 0.02102 -0.00016 0.00901 0.00204 AFIX 137 H32A 2 0.663203 0.588568 0.605822 11.00000 -1.50000 H32B 2 0.695693 0.674849 0.691642 11.00000 -1.50000 H32C 2 0.661148 0.521156 0.686992 11.00000 -1.50000 AFIX 0 C33 1 0.817745 0.489817 0.790335 11.00000 0.02851 0.02124 = 0.01575 -0.00161 0.00705 -0.00210 AFIX 137 H33A 2 0.785267 0.417498 0.800090 11.00000 -1.50000 H33B 2 0.818251 0.573066 0.822009 11.00000 -1.50000 H33C 2 0.874332 0.457061 0.809151 11.00000 -1.50000 AFIX 0 C34 1 0.830697 0.636218 0.680349 11.00000 0.02988 0.01832 = 0.02042 -0.00231 0.00967 -0.00532 AFIX 137 H34A 2 0.887738 0.604131 0.701853 11.00000 -1.50000 H34B 2 0.829410 0.721207 0.709770 11.00000 -1.50000 H34C 2 0.807979 0.654809 0.619836 11.00000 -1.50000 HKLF 4 ; # Attachment '- mima34.cif' data_mima34 _database_code_depnum_ccdc_archive 'CCDC 884310' #TrackingRef '- mima34.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H52 Fe' _chemical_formula_weight 516.61 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5774(2) _cell_length_b 15.1552(2) _cell_length_c 15.4685(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.108(2) _cell_angle_gamma 90.00 _cell_volume 2931.76(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25619 _cell_measurement_theta_min 2.2011 _cell_measurement_theta_max 29.2656 _exptl_crystal_description prism _exptl_crystal_colour 'dark violet' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.534 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97581 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _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 '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 112119 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.87 _reflns_number_total 6986 _reflns_number_gt 6010 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _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 on C2, C20 and C22 were refined freely. The methyls were refined using a rigid model, others riding. ; _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^)+(0.0386P)^2^+1.4909P] 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 6986 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Fe Fe 0.460672(14) 0.299465(12) 0.756122(11) 0.01156(6) Uani 1 1 d . . . C1 C 0.29207(10) 0.29314(9) 0.74257(8) 0.0141(3) Uani 1 1 d . . . C2 C 0.33813(11) 0.21104(9) 0.72156(9) 0.0143(3) Uani 1 1 d . . . H2 H 0.3273(12) 0.1566(11) 0.7504(10) 0.015(4) Uiso 1 1 d . . . C3 C 0.40137(11) 0.21986(9) 0.65067(8) 0.0150(3) Uani 1 1 d . . . C4 C 0.39092(11) 0.31076(9) 0.62367(8) 0.0150(3) Uani 1 1 d . . . C5 C 0.32443(10) 0.35593(9) 0.68084(8) 0.0147(3) Uani 1 1 d . . . C6 C 0.29351(11) 0.44540(9) 0.66249(9) 0.0195(3) Uani 1 1 d . . . H6 H 0.2520 0.4764 0.7004 0.023 Uiso 1 1 calc R . . C7 C 0.32387(12) 0.48582(10) 0.59060(10) 0.0238(3) Uani 1 1 d . . . H7 H 0.3016 0.5447 0.5778 0.029 Uiso 1 1 calc R . . C8 C 0.38847(12) 0.44141(10) 0.53431(10) 0.0242(3) Uani 1 1 d . . . H8 H 0.4083 0.4712 0.4845 0.029 Uiso 1 1 calc R . . C9 C 0.42249(11) 0.35726(10) 0.55017(9) 0.0201(3) Uani 1 1 d . . . H9 H 0.4671 0.3294 0.5125 0.024 Uiso 1 1 calc R . . C10 C 0.20203(11) 0.30377(9) 0.80073(9) 0.0172(3) Uani 1 1 d . . . C11 C 0.09849(12) 0.32519(11) 0.74201(10) 0.0249(3) Uani 1 1 d . . . H11A H 0.1058 0.3827 0.7142 0.037 Uiso 1 1 calc R . . H11B H 0.0382 0.3269 0.7772 0.037 Uiso 1 1 calc R . . H11C H 0.0857 0.2796 0.6972 0.037 Uiso 1 1 calc R . . C12 C 0.22333(12) 0.37700(10) 0.86885(10) 0.0229(3) Uani 1 1 d . . . H12A H 0.2842 0.3604 0.9105 0.034 Uiso 1 1 calc R . . H12B H 0.1598 0.3852 0.8996 0.034 Uiso 1 1 calc R . . H12C H 0.2395 0.4322 0.8399 0.034 Uiso 1 1 calc R . . C13 C 0.18260(12) 0.21700(10) 0.84736(10) 0.0223(3) Uani 1 1 d . . . H13A H 0.1599 0.1715 0.8043 0.033 Uiso 1 1 calc R . . H13B H 0.1266 0.2257 0.8861 0.033 Uiso 1 1 calc R . . H13C H 0.2488 0.1983 0.8816 0.033 Uiso 1 1 calc R . . C14 C 0.43811(12) 0.14019(9) 0.60130(9) 0.0202(3) Uani 1 1 d . . . C15 C 0.52627(16) 0.15979(12) 0.54340(13) 0.0425(5) Uani 1 1 d . . . H15A H 0.4978 0.1975 0.4949 0.064 Uiso 1 1 calc R . . H15B H 0.5521 0.1043 0.5206 0.064 Uiso 1 1 calc R . . H15C H 0.5855 0.1901 0.5775 0.064 Uiso 1 1 calc R . . C16 C 0.33887(14) 0.10700(11) 0.54287(10) 0.0293(4) Uani 1 1 d . . . H16A H 0.2826 0.0909 0.5792 0.044 Uiso 1 1 calc R . . H16B H 0.3583 0.0552 0.5100 0.044 Uiso 1 1 calc R . . H16C H 0.3127 0.1538 0.5024 0.044 Uiso 1 1 calc R . . C17 C 0.47794(13) 0.06603(10) 0.66368(11) 0.0278(3) Uani 1 1 d . . . H17A H 0.5423 0.0856 0.6999 0.042 Uiso 1 1 calc R . . H17B H 0.4949 0.0139 0.6302 0.042 Uiso 1 1 calc R . . H17C H 0.4222 0.0511 0.7009 0.042 Uiso 1 1 calc R . . C18 C 0.56221(10) 0.39703(9) 0.81699(8) 0.0150(3) Uani 1 1 d . . . C19 C 0.62569(10) 0.33379(9) 0.77310(9) 0.0157(3) Uani 1 1 d . . . C20 C 0.60529(11) 0.24902(9) 0.80884(9) 0.0164(3) Uani 1 1 d . . . H20 H 0.6356(13) 0.1941(10) 0.7929(10) 0.013(4) Uiso 1 1 d . . . C21 C 0.53666(11) 0.25671(9) 0.87574(8) 0.0160(3) Uani 1 1 d . . . C22 C 0.51001(11) 0.34743(9) 0.87929(8) 0.0153(3) Uani 1 1 d . . . H22 H 0.4641(13) 0.3724(10) 0.9183(10) 0.015(4) Uiso 1 1 d . . . C23 C 0.55824(11) 0.49850(9) 0.81943(9) 0.0173(3) Uani 1 1 d . . . C24 C 0.56960(12) 0.54390(9) 0.73243(9) 0.0205(3) Uani 1 1 d . . . H24A H 0.6421 0.5345 0.7164 0.031 Uiso 1 1 calc R . . H24B H 0.5564 0.6073 0.7378 0.031 Uiso 1 1 calc R . . H24C H 0.5176 0.5189 0.6874 0.031 Uiso 1 1 calc R . . C25 C 0.45090(12) 0.53025(9) 0.84794(10) 0.0212(3) Uani 1 1 d . . . H25A H 0.4490 0.5949 0.8477 0.032 Uiso 1 1 calc R . . H25B H 0.4435 0.5086 0.9067 0.032 Uiso 1 1 calc R . . H25C H 0.3920 0.5075 0.8075 0.032 Uiso 1 1 calc R . . C26 C 0.64595(12) 0.53113(10) 0.88982(10) 0.0237(3) Uani 1 1 d . . . H26A H 0.7165 0.5153 0.8731 0.036 Uiso 1 1 calc R . . H26B H 0.6359 0.5034 0.9456 0.036 Uiso 1 1 calc R . . H26C H 0.6411 0.5954 0.8954 0.036 Uiso 1 1 calc R . . C27 C 0.71719(11) 0.34524(10) 0.71482(9) 0.0194(3) Uani 1 1 d . . . C28 C 0.77526(13) 0.25667(11) 0.70616(11) 0.0286(3) Uani 1 1 d . . . H28A H 0.7247 0.2130 0.6791 0.043 Uiso 1 1 calc R . . H28B H 0.8042 0.2359 0.7639 0.043 Uiso 1 1 calc R . . H28C H 0.8339 0.2647 0.6699 0.043 Uiso 1 1 calc R . . C29 C 0.68096(12) 0.37754(10) 0.62225(9) 0.0226(3) Uani 1 1 d . . . H29A H 0.7437 0.3938 0.5933 0.034 Uiso 1 1 calc R . . H29B H 0.6344 0.4291 0.6250 0.034 Uiso 1 1 calc R . . H29C H 0.6417 0.3303 0.5894 0.034 Uiso 1 1 calc R . . C30 C 0.80232(11) 0.40847(11) 0.75843(10) 0.0259(3) Uani 1 1 d . . . H30A H 0.8227 0.3895 0.8185 0.039 Uiso 1 1 calc R . . H30B H 0.7731 0.4684 0.7583 0.039 Uiso 1 1 calc R . . H30C H 0.8654 0.4077 0.7263 0.039 Uiso 1 1 calc R . . C31 C 0.52181(12) 0.18624(9) 0.94318(9) 0.0203(3) Uani 1 1 d . . . C32 C 0.48241(15) 0.09832(10) 0.90272(11) 0.0311(4) Uani 1 1 d . . . H32A H 0.4100 0.1058 0.8733 0.047 Uiso 1 1 calc R . . H32B H 0.4815 0.0537 0.9485 0.047 Uiso 1 1 calc R . . H32C H 0.5305 0.0792 0.8605 0.047 Uiso 1 1 calc R . . C33 C 0.44603(12) 0.21675(11) 1.00829(10) 0.0253(3) Uani 1 1 d . . . H33A H 0.4754 0.2695 1.0387 0.038 Uiso 1 1 calc R . . H33B H 0.4382 0.1697 1.0506 0.038 Uiso 1 1 calc R . . H33C H 0.3760 0.2306 0.9773 0.038 Uiso 1 1 calc R . . C34 C 0.63224(13) 0.17179(13) 0.99398(11) 0.0338(4) Uani 1 1 d . . . H34A H 0.6822 0.1499 0.9544 0.051 Uiso 1 1 calc R . . H34B H 0.6263 0.1285 1.0402 0.051 Uiso 1 1 calc R . . H34C H 0.6587 0.2278 1.0197 0.051 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 Fe 0.01132(10) 0.01215(10) 0.01090(9) 0.00105(7) -0.00030(7) 0.00068(7) C1 0.0119(6) 0.0171(6) 0.0129(6) -0.0008(5) -0.0006(5) 0.0004(5) C2 0.0142(6) 0.0143(6) 0.0141(6) -0.0001(5) 0.0008(5) -0.0011(5) C3 0.0152(6) 0.0157(6) 0.0137(6) -0.0013(5) 0.0003(5) -0.0005(5) C4 0.0144(6) 0.0177(6) 0.0121(6) -0.0002(5) -0.0017(5) -0.0005(5) C5 0.0132(6) 0.0163(6) 0.0136(6) -0.0003(5) -0.0034(5) 0.0002(5) C6 0.0185(7) 0.0179(7) 0.0205(7) -0.0018(5) -0.0057(5) 0.0014(5) C7 0.0257(8) 0.0165(7) 0.0264(8) 0.0053(6) -0.0094(6) -0.0015(6) C8 0.0229(7) 0.0277(8) 0.0206(7) 0.0097(6) -0.0043(6) -0.0063(6) C9 0.0176(7) 0.0257(7) 0.0162(7) 0.0022(6) -0.0012(5) -0.0027(6) C10 0.0132(6) 0.0223(7) 0.0163(6) -0.0012(5) 0.0021(5) 0.0008(5) C11 0.0145(7) 0.0344(8) 0.0256(8) -0.0009(6) 0.0005(6) 0.0024(6) C12 0.0199(7) 0.0280(8) 0.0216(7) -0.0070(6) 0.0059(6) 0.0009(6) C13 0.0180(7) 0.0283(8) 0.0210(7) 0.0014(6) 0.0049(6) -0.0030(6) C14 0.0226(7) 0.0179(7) 0.0207(7) -0.0048(5) 0.0050(6) 0.0002(5) C15 0.0505(12) 0.0302(9) 0.0530(12) -0.0131(8) 0.0341(10) -0.0020(8) C16 0.0362(9) 0.0249(8) 0.0248(8) -0.0109(6) -0.0066(7) 0.0056(7) C17 0.0324(8) 0.0203(7) 0.0292(8) -0.0070(6) -0.0033(7) 0.0089(6) C18 0.0128(6) 0.0169(6) 0.0142(6) 0.0001(5) -0.0034(5) -0.0009(5) C19 0.0113(6) 0.0189(6) 0.0162(6) 0.0033(5) -0.0016(5) 0.0009(5) C20 0.0144(6) 0.0164(7) 0.0178(6) 0.0033(5) -0.0015(5) 0.0027(5) C21 0.0146(6) 0.0187(7) 0.0135(6) 0.0037(5) -0.0034(5) -0.0003(5) C22 0.0151(6) 0.0185(7) 0.0116(6) 0.0000(5) -0.0019(5) -0.0012(5) C23 0.0169(7) 0.0152(6) 0.0185(6) -0.0005(5) -0.0038(5) -0.0016(5) C24 0.0206(7) 0.0165(7) 0.0236(7) 0.0038(5) -0.0024(6) -0.0010(5) C25 0.0230(7) 0.0164(7) 0.0234(7) -0.0029(5) -0.0005(6) 0.0012(5) C26 0.0238(7) 0.0223(7) 0.0232(7) -0.0026(6) -0.0064(6) -0.0040(6) C27 0.0138(6) 0.0225(7) 0.0222(7) 0.0055(6) 0.0031(5) 0.0023(5) C28 0.0225(8) 0.0292(8) 0.0365(9) 0.0079(7) 0.0137(7) 0.0080(6) C29 0.0201(7) 0.0282(8) 0.0201(7) 0.0048(6) 0.0046(6) -0.0005(6) C30 0.0140(7) 0.0332(8) 0.0300(8) 0.0072(7) -0.0006(6) -0.0018(6) C31 0.0213(7) 0.0220(7) 0.0172(7) 0.0081(5) -0.0005(5) 0.0003(5) C32 0.0470(10) 0.0203(8) 0.0254(8) 0.0100(6) 0.0016(7) -0.0024(7) C33 0.0247(8) 0.0333(8) 0.0180(7) 0.0084(6) 0.0023(6) -0.0025(6) C34 0.0236(8) 0.0470(10) 0.0294(9) 0.0205(8) -0.0027(7) 0.0046(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C20 2.0597(13) . ? Fe C2 2.0693(13) . ? Fe C22 2.0716(13) . ? Fe C21 2.0930(13) . ? Fe C3 2.1009(13) . ? Fe C18 2.1090(13) . ? Fe C1 2.1108(13) . ? Fe C19 2.1287(13) . ? Fe C5 2.1448(13) . ? Fe C4 2.1480(13) . ? C1 C2 1.4246(18) . ? C1 C5 1.4373(18) . ? C1 C10 1.5280(18) . ? C2 C3 1.4279(18) . ? C3 C4 1.4414(18) . ? C3 C14 1.5263(19) . ? C4 C9 1.4294(19) . ? C4 C5 1.4518(18) . ? C5 C6 1.4307(19) . ? C6 C7 1.359(2) . ? C7 C8 1.422(2) . ? C8 C9 1.359(2) . ? C10 C13 1.532(2) . ? C10 C12 1.5341(19) . ? C10 C11 1.5409(19) . ? C14 C15 1.527(2) . ? C14 C17 1.531(2) . ? C14 C16 1.545(2) . ? C18 C22 1.4350(19) . ? C18 C19 1.4602(19) . ? C18 C23 1.5393(19) . ? C19 C20 1.4326(19) . ? C19 C27 1.5452(19) . ? C20 C21 1.4211(19) . ? C21 C22 1.4177(19) . ? C21 C31 1.5182(18) . ? C23 C24 1.5317(19) . ? C23 C25 1.541(2) . ? C23 C26 1.5463(19) . ? C27 C29 1.5359(19) . ? C27 C30 1.538(2) . ? C27 C28 1.541(2) . ? C31 C33 1.530(2) . ? C31 C32 1.532(2) . ? C31 C34 1.537(2) . ? 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 C20 Fe C2 117.65(5) . . ? C20 Fe C22 66.46(5) . . ? C2 Fe C22 127.36(5) . . ? C20 Fe C21 40.01(5) . . ? C2 Fe C21 106.58(5) . . ? C22 Fe C21 39.80(5) . . ? C20 Fe C3 108.66(5) . . ? C2 Fe C3 40.04(5) . . ? C22 Fe C3 164.24(5) . . ? C21 Fe C3 126.84(5) . . ? C20 Fe C18 67.43(5) . . ? C2 Fe C18 165.56(5) . . ? C22 Fe C18 40.14(5) . . ? C21 Fe C18 67.95(5) . . ? C3 Fe C18 153.81(5) . . ? C20 Fe C1 149.09(5) . . ? C2 Fe C1 39.84(5) . . ? C22 Fe C1 107.86(5) . . ? C21 Fe C1 115.67(5) . . ? C3 Fe C1 68.09(5) . . ? C18 Fe C1 129.08(5) . . ? C20 Fe C19 39.96(5) . . ? C2 Fe C19 151.62(5) . . ? C22 Fe C19 66.93(5) . . ? C21 Fe C19 67.61(5) . . ? C3 Fe C19 119.81(5) . . ? C18 Fe C19 40.31(5) . . ? C1 Fe C19 168.35(5) . . ? C20 Fe C5 169.72(5) . . ? C2 Fe C5 65.67(5) . . ? C22 Fe C5 120.20(5) . . ? C21 Fe C5 150.09(5) . . ? C3 Fe C5 67.07(5) . . ? C18 Fe C5 111.93(5) . . ? C1 Fe C5 39.47(5) . . ? C19 Fe C5 132.97(5) . . ? C20 Fe C4 131.38(5) . . ? C2 Fe C4 65.66(5) . . ? C22 Fe C4 154.31(5) . . ? C21 Fe C4 165.84(5) . . ? C3 Fe C4 39.64(5) . . ? C18 Fe C4 122.44(5) . . ? C1 Fe C4 66.72(5) . . ? C19 Fe C4 113.08(5) . . ? C5 Fe C4 39.53(5) . . ? C2 C1 C5 106.02(11) . . ? C2 C1 C10 124.84(12) . . ? C5 C1 C10 126.97(12) . . ? C2 C1 Fe 68.51(7) . . ? C5 C1 Fe 71.54(7) . . ? C10 C1 Fe 137.43(9) . . ? C1 C2 C3 111.51(12) . . ? C1 C2 Fe 71.65(8) . . ? C3 C2 Fe 71.17(8) . . ? C2 C3 C4 105.72(11) . . ? C2 C3 C14 122.22(12) . . ? C4 C3 C14 129.36(12) . . ? C2 C3 Fe 68.79(7) . . ? C4 C3 Fe 71.94(7) . . ? C14 C3 Fe 137.85(10) . . ? C9 C4 C3 132.62(13) . . ? C9 C4 C5 118.61(12) . . ? C3 C4 C5 108.36(11) . . ? C9 C4 Fe 132.70(10) . . ? C3 C4 Fe 68.42(7) . . ? C5 C4 Fe 70.11(7) . . ? C6 C5 C1 132.00(13) . . ? C6 C5 C4 119.22(12) . . ? C1 C5 C4 108.34(11) . . ? C6 C5 Fe 132.11(10) . . ? C1 C5 Fe 68.99(7) . . ? C4 C5 Fe 70.35(7) . . ? C7 C6 C5 119.69(14) . . ? C6 C7 C8 121.07(14) . . ? C9 C8 C7 121.54(14) . . ? C8 C9 C4 119.83(14) . . ? C1 C10 C13 110.61(11) . . ? C1 C10 C12 113.23(11) . . ? C13 C10 C12 108.82(12) . . ? C1 C10 C11 107.94(11) . . ? C13 C10 C11 106.93(12) . . ? C12 C10 C11 109.11(12) . . ? C3 C14 C15 114.65(12) . . ? C3 C14 C17 111.21(12) . . ? C15 C14 C17 107.65(14) . . ? C3 C14 C16 106.35(12) . . ? C15 C14 C16 108.19(14) . . ? C17 C14 C16 108.64(12) . . ? C22 C18 C19 106.28(12) . . ? C22 C18 C23 119.24(12) . . ? C19 C18 C23 133.46(12) . . ? C22 C18 Fe 68.53(7) . . ? C19 C18 Fe 70.57(7) . . ? C23 C18 Fe 133.77(9) . . ? C20 C19 C18 106.25(12) . . ? C20 C19 C27 120.06(12) . . ? C18 C19 C27 132.50(12) . . ? C20 C19 Fe 67.42(7) . . ? C18 C19 Fe 69.12(7) . . ? C27 C19 Fe 137.08(10) . . ? C21 C20 C19 110.80(12) . . ? C21 C20 Fe 71.26(8) . . ? C19 C20 Fe 72.62(8) . . ? C22 C21 C20 105.79(12) . . ? C22 C21 C31 127.50(12) . . ? C20 C21 C31 124.84(12) . . ? C22 C21 Fe 69.29(7) . . ? C20 C21 Fe 68.73(7) . . ? C31 C21 Fe 138.35(10) . . ? C21 C22 C18 110.79(12) . . ? C21 C22 Fe 70.91(8) . . ? C18 C22 Fe 71.33(7) . . ? C24 C23 C18 114.89(11) . . ? C24 C23 C25 106.12(11) . . ? C18 C23 C25 110.52(11) . . ? C24 C23 C26 110.42(12) . . ? C18 C23 C26 108.31(11) . . ? C25 C23 C26 106.24(12) . . ? C29 C27 C30 109.51(12) . . ? C29 C27 C28 107.04(12) . . ? C30 C27 C28 105.45(12) . . ? C29 C27 C19 114.47(11) . . ? C30 C27 C19 109.93(12) . . ? C28 C27 C19 110.01(12) . . ? C21 C31 C33 111.75(12) . . ? C21 C31 C32 112.90(12) . . ? C33 C31 C32 109.55(13) . . ? C21 C31 C34 106.32(12) . . ? C33 C31 C34 107.39(13) . . ? C32 C31 C34 108.69(13) . . ? 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 C20 Fe C1 C2 -53.69(13) . . . . ? C22 Fe C1 C2 -127.52(8) . . . . ? C21 Fe C1 C2 -85.31(8) . . . . ? C3 Fe C1 C2 36.28(8) . . . . ? C18 Fe C1 C2 -166.89(8) . . . . ? C19 Fe C1 C2 170.9(2) . . . . ? C5 Fe C1 C2 116.37(11) . . . . ? C4 Fe C1 C2 79.35(8) . . . . ? C20 Fe C1 C5 -170.06(10) . . . . ? C2 Fe C1 C5 -116.37(11) . . . . ? C22 Fe C1 C5 116.12(8) . . . . ? C21 Fe C1 C5 158.32(8) . . . . ? C3 Fe C1 C5 -80.09(8) . . . . ? C18 Fe C1 C5 76.74(9) . . . . ? C19 Fe C1 C5 54.5(3) . . . . ? C4 Fe C1 C5 -37.02(7) . . . . ? C20 Fe C1 C10 64.93(18) . . . . ? C2 Fe C1 C10 118.62(17) . . . . ? C22 Fe C1 C10 -8.90(15) . . . . ? C21 Fe C1 C10 33.31(15) . . . . ? C3 Fe C1 C10 154.90(15) . . . . ? C18 Fe C1 C10 -48.27(16) . . . . ? C19 Fe C1 C10 -70.5(3) . . . . ? C5 Fe C1 C10 -125.01(17) . . . . ? C4 Fe C1 C10 -162.03(15) . . . . ? C5 C1 C2 C3 1.90(15) . . . . ? C10 C1 C2 C3 166.09(12) . . . . ? Fe C1 C2 C3 -60.25(10) . . . . ? C5 C1 C2 Fe 62.15(9) . . . . ? C10 C1 C2 Fe -133.65(13) . . . . ? C20 Fe C2 C1 152.14(8) . . . . ? C22 Fe C2 C1 71.77(9) . . . . ? C21 Fe C2 C1 110.40(8) . . . . ? C3 Fe C2 C1 -121.41(11) . . . . ? C18 Fe C2 C1 44.9(2) . . . . ? C19 Fe C2 C1 -176.15(10) . . . . ? C5 Fe C2 C1 -38.68(7) . . . . ? C4 Fe C2 C1 -82.26(8) . . . . ? C20 Fe C2 C3 -86.44(9) . . . . ? C22 Fe C2 C3 -166.81(8) . . . . ? C21 Fe C2 C3 -128.18(8) . . . . ? C18 Fe C2 C3 166.31(19) . . . . ? C1 Fe C2 C3 121.41(11) . . . . ? C19 Fe C2 C3 -54.74(14) . . . . ? C5 Fe C2 C3 82.73(8) . . . . ? C4 Fe C2 C3 39.16(8) . . . . ? C1 C2 C3 C4 -2.42(15) . . . . ? Fe C2 C3 C4 -62.96(9) . . . . ? C1 C2 C3 C14 -165.40(12) . . . . ? Fe C2 C3 C14 134.06(13) . . . . ? C1 C2 C3 Fe 60.54(10) . . . . ? C20 Fe C3 C2 111.07(8) . . . . ? C22 Fe C3 C2 41.9(2) . . . . ? C21 Fe C3 C2 70.28(9) . . . . ? C18 Fe C3 C2 -172.31(11) . . . . ? C1 Fe C3 C2 -36.10(8) . . . . ? C19 Fe C3 C2 153.43(8) . . . . ? C5 Fe C3 C2 -78.93(8) . . . . ? C4 Fe C3 C2 -115.61(11) . . . . ? C20 Fe C3 C4 -133.32(8) . . . . ? C2 Fe C3 C4 115.61(11) . . . . ? C22 Fe C3 C4 157.50(18) . . . . ? C21 Fe C3 C4 -174.11(8) . . . . ? C18 Fe C3 C4 -56.71(15) . . . . ? C1 Fe C3 C4 79.50(8) . . . . ? C19 Fe C3 C4 -90.96(9) . . . . ? C5 Fe C3 C4 36.67(8) . . . . ? C20 Fe C3 C14 -3.99(16) . . . . ? C2 Fe C3 C14 -115.06(17) . . . . ? C22 Fe C3 C14 -73.2(3) . . . . ? C21 Fe C3 C14 -44.78(17) . . . . ? C18 Fe C3 C14 72.6(2) . . . . ? C1 Fe C3 C14 -151.16(16) . . . . ? C19 Fe C3 C14 38.37(16) . . . . ? C5 Fe C3 C14 166.01(16) . . . . ? C4 Fe C3 C14 129.33(18) . . . . ? C2 C3 C4 C9 -170.32(14) . . . . ? C14 C3 C4 C9 -9.0(2) . . . . ? Fe C3 C4 C9 128.83(16) . . . . ? C2 C3 C4 C5 1.96(14) . . . . ? C14 C3 C4 C5 163.28(13) . . . . ? Fe C3 C4 C5 -58.89(9) . . . . ? C2 C3 C4 Fe 60.85(9) . . . . ? C14 C3 C4 Fe -137.83(15) . . . . ? C20 Fe C4 C9 -62.02(16) . . . . ? C2 Fe C4 C9 -168.29(15) . . . . ? C22 Fe C4 C9 65.1(2) . . . . ? C21 Fe C4 C9 -109.1(2) . . . . ? C3 Fe C4 C9 -128.74(17) . . . . ? C18 Fe C4 C9 25.33(16) . . . . ? C1 Fe C4 C9 148.00(15) . . . . ? C19 Fe C4 C9 -19.32(15) . . . . ? C5 Fe C4 C9 111.04(16) . . . . ? C20 Fe C4 C3 66.72(10) . . . . ? C2 Fe C4 C3 -39.55(8) . . . . ? C22 Fe C4 C3 -166.13(11) . . . . ? C21 Fe C4 C3 19.6(2) . . . . ? C18 Fe C4 C3 154.08(8) . . . . ? C1 Fe C4 C3 -83.26(8) . . . . ? C19 Fe C4 C3 109.42(8) . . . . ? C5 Fe C4 C3 -120.22(11) . . . . ? C20 Fe C4 C5 -173.06(8) . . . . ? C2 Fe C4 C5 80.67(8) . . . . ? C22 Fe C4 C5 -45.92(15) . . . . ? C21 Fe C4 C5 139.8(2) . . . . ? C3 Fe C4 C5 120.22(11) . . . . ? C18 Fe C4 C5 -85.71(9) . . . . ? C1 Fe C4 C5 36.96(8) . . . . ? C19 Fe C4 C5 -130.36(8) . . . . ? C2 C1 C5 C6 171.48(14) . . . . ? C10 C1 C5 C6 7.7(2) . . . . ? Fe C1 C5 C6 -128.37(15) . . . . ? C2 C1 C5 C4 -0.60(14) . . . . ? C10 C1 C5 C4 -164.35(12) . . . . ? Fe C1 C5 C4 59.55(9) . . . . ? C2 C1 C5 Fe -60.15(9) . . . . ? C10 C1 C5 Fe 136.09(13) . . . . ? C9 C4 C5 C6 -0.59(19) . . . . ? C3 C4 C5 C6 -174.12(12) . . . . ? Fe C4 C5 C6 128.03(12) . . . . ? C9 C4 C5 C1 172.67(12) . . . . ? C3 C4 C5 C1 -0.86(15) . . . . ? Fe C4 C5 C1 -58.71(9) . . . . ? C9 C4 C5 Fe -128.62(12) . . . . ? C3 C4 C5 Fe 57.85(9) . . . . ? C20 Fe C5 C6 -81.6(3) . . . . ? C2 Fe C5 C6 167.29(15) . . . . ? C22 Fe C5 C6 46.80(15) . . . . ? C21 Fe C5 C6 86.37(17) . . . . ? C3 Fe C5 C6 -148.85(15) . . . . ? C18 Fe C5 C6 2.79(15) . . . . ? C1 Fe C5 C6 128.25(17) . . . . ? C19 Fe C5 C6 -38.76(17) . . . . ? C4 Fe C5 C6 -112.08(16) . . . . ? C20 Fe C5 C1 150.2(3) . . . . ? C2 Fe C5 C1 39.04(7) . . . . ? C22 Fe C5 C1 -81.45(9) . . . . ? C21 Fe C5 C1 -41.88(14) . . . . ? C3 Fe C5 C1 82.90(8) . . . . ? C18 Fe C5 C1 -125.46(8) . . . . ? C19 Fe C5 C1 -167.01(8) . . . . ? C4 Fe C5 C1 119.67(11) . . . . ? C20 Fe C5 C4 30.5(3) . . . . ? C2 Fe C5 C4 -80.63(8) . . . . ? C22 Fe C5 C4 158.88(8) . . . . ? C21 Fe C5 C4 -161.55(10) . . . . ? C3 Fe C5 C4 -36.77(7) . . . . ? C18 Fe C5 C4 114.87(8) . . . . ? C1 Fe C5 C4 -119.67(11) . . . . ? C19 Fe C5 C4 73.33(10) . . . . ? C1 C5 C6 C7 -169.34(14) . . . . ? C4 C5 C6 C7 2.04(19) . . . . ? Fe C5 C6 C7 91.25(16) . . . . ? C5 C6 C7 C8 -1.7(2) . . . . ? C6 C7 C8 C9 -0.2(2) . . . . ? C7 C8 C9 C4 1.6(2) . . . . ? C3 C4 C9 C8 170.42(14) . . . . ? C5 C4 C9 C8 -1.2(2) . . . . ? Fe C4 C9 C8 -89.86(17) . . . . ? C2 C1 C10 C13 10.89(18) . . . . ? C5 C1 C10 C13 171.76(13) . . . . ? Fe C1 C10 C13 -84.73(16) . . . . ? C2 C1 C10 C12 133.33(14) . . . . ? C5 C1 C10 C12 -65.79(17) . . . . ? Fe C1 C10 C12 37.71(19) . . . . ? C2 C1 C10 C11 -105.77(15) . . . . ? C5 C1 C10 C11 55.10(17) . . . . ? Fe C1 C10 C11 158.60(12) . . . . ? C2 C3 C14 C15 -165.69(15) . . . . ? C4 C3 C14 C15 35.7(2) . . . . ? Fe C3 C14 C15 -72.3(2) . . . . ? C2 C3 C14 C17 -43.29(18) . . . . ? C4 C3 C14 C17 158.08(14) . . . . ? Fe C3 C14 C17 50.10(19) . . . . ? C2 C3 C14 C16 74.81(16) . . . . ? C4 C3 C14 C16 -83.82(17) . . . . ? Fe C3 C14 C16 168.20(12) . . . . ? C20 Fe C18 C22 -79.75(8) . . . . ? C2 Fe C18 C22 33.9(2) . . . . ? C21 Fe C18 C22 -36.35(8) . . . . ? C3 Fe C18 C22 -166.30(11) . . . . ? C1 Fe C18 C22 69.50(10) . . . . ? C19 Fe C18 C22 -117.27(11) . . . . ? C5 Fe C18 C22 111.33(8) . . . . ? C4 Fe C18 C22 154.51(8) . . . . ? C20 Fe C18 C19 37.52(8) . . . . ? C2 Fe C18 C19 151.15(19) . . . . ? C22 Fe C18 C19 117.27(11) . . . . ? C21 Fe C18 C19 80.93(8) . . . . ? C3 Fe C18 C19 -49.03(15) . . . . ? C1 Fe C18 C19 -173.23(7) . . . . ? C5 Fe C18 C19 -131.39(8) . . . . ? C4 Fe C18 C19 -88.22(9) . . . . ? C20 Fe C18 C23 169.76(15) . . . . ? C2 Fe C18 C23 -76.6(3) . . . . ? C22 Fe C18 C23 -110.49(16) . . . . ? C21 Fe C18 C23 -146.84(15) . . . . ? C3 Fe C18 C23 83.21(18) . . . . ? C1 Fe C18 C23 -40.99(16) . . . . ? C19 Fe C18 C23 132.24(17) . . . . ? C5 Fe C18 C23 0.84(15) . . . . ? C4 Fe C18 C23 44.02(15) . . . . ? C22 C18 C19 C20 2.14(14) . . . . ? C23 C18 C19 C20 170.07(13) . . . . ? Fe C18 C19 C20 -57.37(9) . . . . ? C22 C18 C19 C27 -164.97(13) . . . . ? C23 C18 C19 C27 3.0(2) . . . . ? Fe C18 C19 C27 135.52(15) . . . . ? C22 C18 C19 Fe 59.51(9) . . . . ? C23 C18 C19 Fe -132.56(15) . . . . ? C2 Fe C19 C20 -46.45(14) . . . . ? C22 Fe C19 C20 80.36(8) . . . . ? C21 Fe C19 C20 37.05(8) . . . . ? C3 Fe C19 C20 -83.70(9) . . . . ? C18 Fe C19 C20 118.88(11) . . . . ? C1 Fe C19 C20 145.8(2) . . . . ? C5 Fe C19 C20 -169.12(8) . . . . ? C4 Fe C19 C20 -127.60(8) . . . . ? C20 Fe C19 C18 -118.88(11) . . . . ? C2 Fe C19 C18 -165.33(10) . . . . ? C22 Fe C19 C18 -38.52(8) . . . . ? C21 Fe C19 C18 -81.83(8) . . . . ? C3 Fe C19 C18 157.41(7) . . . . ? C1 Fe C19 C18 27.0(3) . . . . ? C5 Fe C19 C18 72.00(10) . . . . ? C4 Fe C19 C18 113.51(8) . . . . ? C20 Fe C19 C27 110.46(17) . . . . ? C2 Fe C19 C27 64.01(19) . . . . ? C22 Fe C19 C27 -169.18(16) . . . . ? C21 Fe C19 C27 147.51(15) . . . . ? C3 Fe C19 C27 26.76(16) . . . . ? C18 Fe C19 C27 -130.66(17) . . . . ? C1 Fe C19 C27 -103.7(3) . . . . ? C5 Fe C19 C27 -58.66(16) . . . . ? C4 Fe C19 C27 -17.14(16) . . . . ? C18 C19 C20 C21 -2.93(15) . . . . ? C27 C19 C20 C21 166.12(12) . . . . ? Fe C19 C20 C21 -61.37(10) . . . . ? C18 C19 C20 Fe 58.45(9) . . . . ? C27 C19 C20 Fe -132.51(12) . . . . ? C2 Fe C20 C21 -82.94(9) . . . . ? C22 Fe C20 C21 38.33(8) . . . . ? C3 Fe C20 C21 -125.60(8) . . . . ? C18 Fe C20 C21 82.11(8) . . . . ? C1 Fe C20 C21 -47.30(14) . . . . ? C19 Fe C20 C21 119.95(11) . . . . ? C5 Fe C20 C21 170.7(3) . . . . ? C4 Fe C20 C21 -163.81(8) . . . . ? C2 Fe C20 C19 157.11(8) . . . . ? C22 Fe C20 C19 -81.62(8) . . . . ? C21 Fe C20 C19 -119.95(11) . . . . ? C3 Fe C20 C19 114.45(8) . . . . ? C18 Fe C20 C19 -37.84(8) . . . . ? C1 Fe C20 C19 -167.24(9) . . . . ? C5 Fe C20 C19 50.7(3) . . . . ? C4 Fe C20 C19 76.24(10) . . . . ? C19 C20 C21 C22 2.50(15) . . . . ? Fe C20 C21 C22 -59.70(9) . . . . ? C19 C20 C21 C31 -162.89(12) . . . . ? Fe C20 C21 C31 134.91(13) . . . . ? C19 C20 C21 Fe 62.20(10) . . . . ? C20 Fe C21 C22 117.35(11) . . . . ? C2 Fe C21 C22 -129.18(8) . . . . ? C3 Fe C21 C22 -168.37(8) . . . . ? C18 Fe C21 C22 36.64(8) . . . . ? C1 Fe C21 C22 -87.41(9) . . . . ? C19 Fe C21 C22 80.34(8) . . . . ? C5 Fe C21 C22 -59.32(13) . . . . ? C4 Fe C21 C22 176.12(19) . . . . ? C2 Fe C21 C20 113.47(8) . . . . ? C22 Fe C21 C20 -117.35(11) . . . . ? C3 Fe C21 C20 74.28(10) . . . . ? C18 Fe C21 C20 -80.70(8) . . . . ? C1 Fe C21 C20 155.24(8) . . . . ? C19 Fe C21 C20 -37.01(8) . . . . ? C5 Fe C21 C20 -176.67(10) . . . . ? C4 Fe C21 C20 58.8(2) . . . . ? C20 Fe C21 C31 -119.00(18) . . . . ? C2 Fe C21 C31 -5.53(16) . . . . ? C22 Fe C21 C31 123.65(18) . . . . ? C3 Fe C21 C31 -44.71(17) . . . . ? C18 Fe C21 C31 160.30(17) . . . . ? C1 Fe C21 C31 36.24(17) . . . . ? C19 Fe C21 C31 -156.00(17) . . . . ? C5 Fe C21 C31 64.3(2) . . . . ? C4 Fe C21 C31 -60.2(3) . . . . ? C20 C21 C22 C18 -1.08(15) . . . . ? C31 C21 C22 C18 163.80(13) . . . . ? Fe C21 C22 C18 -60.42(9) . . . . ? C20 C21 C22 Fe 59.34(9) . . . . ? C31 C21 C22 Fe -135.79(14) . . . . ? C19 C18 C22 C21 -0.68(15) . . . . ? C23 C18 C22 C21 -170.66(11) . . . . ? Fe C18 C22 C21 60.16(9) . . . . ? C19 C18 C22 Fe -60.84(9) . . . . ? C23 C18 C22 Fe 129.18(11) . . . . ? C20 Fe C22 C21 -38.53(8) . . . . ? C2 Fe C22 C21 69.18(10) . . . . ? C3 Fe C22 C21 36.5(2) . . . . ? C18 Fe C22 C21 -120.89(11) . . . . ? C1 Fe C22 C21 108.92(8) . . . . ? C19 Fe C22 C21 -82.21(8) . . . . ? C5 Fe C22 C21 150.25(8) . . . . ? C4 Fe C22 C21 -177.81(11) . . . . ? C20 Fe C22 C18 82.36(8) . . . . ? C2 Fe C22 C18 -169.93(8) . . . . ? C21 Fe C22 C18 120.89(11) . . . . ? C3 Fe C22 C18 157.36(18) . . . . ? C1 Fe C22 C18 -130.19(8) . . . . ? C19 Fe C22 C18 38.68(8) . . . . ? C5 Fe C22 C18 -88.86(9) . . . . ? C4 Fe C22 C18 -56.92(15) . . . . ? C22 C18 C23 C24 -154.07(12) . . . . ? C19 C18 C23 C24 39.2(2) . . . . ? Fe C18 C23 C24 -66.63(17) . . . . ? C22 C18 C23 C25 -34.04(16) . . . . ? C19 C18 C23 C25 159.26(14) . . . . ? Fe C18 C23 C25 53.40(17) . . . . ? C22 C18 C23 C26 81.97(15) . . . . ? C19 C18 C23 C26 -84.73(18) . . . . ? Fe C18 C23 C26 169.41(11) . . . . ? C20 C19 C27 C29 119.73(14) . . . . ? C18 C19 C27 C29 -74.60(19) . . . . ? Fe C19 C27 C29 31.4(2) . . . . ? C20 C19 C27 C30 -116.54(14) . . . . ? C18 C19 C27 C30 49.13(19) . . . . ? Fe C19 C27 C30 155.12(12) . . . . ? C20 C19 C27 C28 -0.83(18) . . . . ? C18 C19 C27 C28 164.84(14) . . . . ? Fe C19 C27 C28 -89.17(16) . . . . ? C22 C21 C31 C33 15.4(2) . . . . ? C20 C21 C31 C33 177.55(13) . . . . ? Fe C21 C31 C33 -85.70(17) . . . . ? C22 C21 C31 C32 139.40(15) . . . . ? C20 C21 C31 C32 -58.41(19) . . . . ? Fe C21 C31 C32 38.3(2) . . . . ? C22 C21 C31 C34 -101.51(17) . . . . ? C20 C21 C31 C34 60.68(18) . . . . ? Fe C21 C31 C34 157.43(13) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.429 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.052 _iucr_refine_instructions_details ; TITL mima34 in P2(1)/n CELL 0.71073 12.5774 15.1552 15.4685 90.000 96.108 90.000 ZERR 4.00 0.0002 0.0002 0.0002 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H FE UNIT 136 208 4 SIZE 0.19 0.17 0.15 TEMP -173 SHEL 999 0.76 ACTA CONF FMAP 2 PLAN 10 L.S. 8 WGHT 0.038600 1.490900 FVAR 2.77087 FE 3 0.460672 0.299465 0.756122 11.00000 0.01132 0.01215 = 0.01090 0.00105 -0.00030 0.00068 C1 1 0.292066 0.293139 0.742569 11.00000 0.01193 0.01706 = 0.01288 -0.00080 -0.00058 0.00038 C2 1 0.338128 0.211040 0.721564 11.00000 0.01423 0.01433 = 0.01406 -0.00012 0.00078 -0.00110 H2 2 0.327307 0.156590 0.750449 11.00000 0.01489 C3 1 0.401371 0.219861 0.650667 11.00000 0.01524 0.01572 = 0.01371 -0.00133 0.00033 -0.00055 C4 1 0.390922 0.310756 0.623673 11.00000 0.01440 0.01770 = 0.01213 -0.00018 -0.00170 -0.00046 C5 1 0.324428 0.355934 0.680843 11.00000 0.01316 0.01634 = 0.01359 -0.00033 -0.00337 0.00016 C6 1 0.293506 0.445403 0.662487 11.00000 0.01847 0.01785 = 0.02054 -0.00176 -0.00566 0.00137 AFIX 43 H6 2 0.251951 0.476420 0.700360 11.00000 -1.20000 AFIX 0 C7 1 0.323867 0.485823 0.590597 11.00000 0.02572 0.01650 = 0.02640 0.00527 -0.00945 -0.00145 AFIX 43 H7 2 0.301561 0.544701 0.577755 11.00000 -1.20000 AFIX 0 C8 1 0.388465 0.441408 0.534312 11.00000 0.02294 0.02767 = 0.02061 0.00970 -0.00433 -0.00626 AFIX 43 H8 2 0.408305 0.471248 0.484455 11.00000 -1.20000 AFIX 0 C9 1 0.422495 0.357260 0.550171 11.00000 0.01765 0.02569 = 0.01617 0.00217 -0.00123 -0.00274 AFIX 43 H9 2 0.467147 0.329424 0.512503 11.00000 -1.20000 AFIX 0 C10 1 0.202025 0.303773 0.800732 11.00000 0.01318 0.02232 = 0.01628 -0.00121 0.00205 0.00080 C11 1 0.098491 0.325187 0.742014 11.00000 0.01450 0.03437 = 0.02561 -0.00088 0.00050 0.00239 AFIX 137 H11A 2 0.105753 0.382677 0.714239 11.00000 -1.50000 H11B 2 0.038205 0.326942 0.777237 11.00000 -1.50000 H11C 2 0.085667 0.279562 0.697223 11.00000 -1.50000 AFIX 0 C12 1 0.223329 0.376999 0.868847 11.00000 0.01989 0.02802 = 0.02164 -0.00696 0.00592 0.00091 AFIX 137 H12A 2 0.284246 0.360417 0.910508 11.00000 -1.50000 H12B 2 0.159848 0.385174 0.899626 11.00000 -1.50000 H12C 2 0.239503 0.432183 0.839921 11.00000 -1.50000 AFIX 0 C13 1 0.182596 0.216998 0.847361 11.00000 0.01804 0.02830 = 0.02103 0.00144 0.00495 -0.00304 AFIX 137 H13A 2 0.159890 0.171506 0.804283 11.00000 -1.50000 H13B 2 0.126641 0.225668 0.886053 11.00000 -1.50000 H13C 2 0.248827 0.198310 0.881574 11.00000 -1.50000 AFIX 0 C14 1 0.438107 0.140192 0.601299 11.00000 0.02263 0.01790 = 0.02067 -0.00479 0.00498 0.00024 C15 1 0.526274 0.159788 0.543401 11.00000 0.05054 0.03017 = 0.05298 -0.01315 0.03409 -0.00203 AFIX 137 H15A 2 0.497804 0.197512 0.494916 11.00000 -1.50000 H15B 2 0.552109 0.104333 0.520627 11.00000 -1.50000 H15C 2 0.585496 0.190098 0.577498 11.00000 -1.50000 AFIX 0 C16 1 0.338871 0.107001 0.542875 11.00000 0.03616 0.02486 = 0.02481 -0.01085 -0.00658 0.00563 AFIX 137 H16A 2 0.282614 0.090899 0.579193 11.00000 -1.50000 H16B 2 0.358324 0.055229 0.510009 11.00000 -1.50000 H16C 2 0.312737 0.153826 0.502367 11.00000 -1.50000 AFIX 0 C17 1 0.477943 0.066030 0.663680 11.00000 0.03239 0.02031 = 0.02919 -0.00703 -0.00327 0.00893 AFIX 137 H17A 2 0.542275 0.085603 0.699920 11.00000 -1.50000 H17B 2 0.494895 0.013943 0.630194 11.00000 -1.50000 H17C 2 0.422167 0.051058 0.700868 11.00000 -1.50000 AFIX 0 C18 1 0.562212 0.397028 0.816989 11.00000 0.01278 0.01694 = 0.01418 0.00005 -0.00340 -0.00091 C19 1 0.625694 0.333795 0.773097 11.00000 0.01130 0.01887 = 0.01616 0.00333 -0.00157 0.00089 C20 1 0.605288 0.249019 0.808841 11.00000 0.01441 0.01642 = 0.01777 0.00328 -0.00148 0.00275 H20 2 0.635628 0.194115 0.792887 11.00000 0.01286 C21 1 0.536661 0.256709 0.875742 11.00000 0.01462 0.01874 = 0.01346 0.00369 -0.00342 -0.00030 C22 1 0.510006 0.347435 0.879286 11.00000 0.01509 0.01847 = 0.01158 0.00002 -0.00194 -0.00116 H22 2 0.464102 0.372411 0.918326 11.00000 0.01454 C23 1 0.558245 0.498505 0.819433 11.00000 0.01690 0.01516 = 0.01849 -0.00049 -0.00379 -0.00155 C24 1 0.569604 0.543898 0.732425 11.00000 0.02058 0.01645 = 0.02357 0.00380 -0.00238 -0.00099 AFIX 137 H24A 2 0.642079 0.534544 0.716414 11.00000 -1.50000 H24B 2 0.556444 0.607295 0.737806 11.00000 -1.50000 H24C 2 0.517557 0.518898 0.687386 11.00000 -1.50000 AFIX 0 C25 1 0.450899 0.530252 0.847943 11.00000 0.02299 0.01639 = 0.02342 -0.00292 -0.00053 0.00115 AFIX 137 H25A 2 0.448971 0.594897 0.847748 11.00000 -1.50000 H25B 2 0.443482 0.508568 0.906686 11.00000 -1.50000 H25C 2 0.391991 0.507478 0.807525 11.00000 -1.50000 AFIX 0 C26 1 0.645946 0.531134 0.889821 11.00000 0.02383 0.02225 = 0.02322 -0.00264 -0.00645 -0.00397 AFIX 137 H26A 2 0.716466 0.515306 0.873060 11.00000 -1.50000 H26B 2 0.635872 0.503395 0.945596 11.00000 -1.50000 H26C 2 0.641081 0.595381 0.895415 11.00000 -1.50000 AFIX 0 C27 1 0.717185 0.345242 0.714817 11.00000 0.01384 0.02253 = 0.02218 0.00546 0.00305 0.00232 C28 1 0.775259 0.256668 0.706164 11.00000 0.02248 0.02919 = 0.03645 0.00793 0.01367 0.00798 AFIX 137 H28A 2 0.724709 0.213002 0.679136 11.00000 -1.50000 H28B 2 0.804154 0.235935 0.763940 11.00000 -1.50000 H28C 2 0.833851 0.264733 0.669912 11.00000 -1.50000 AFIX 0 C29 1 0.680961 0.377543 0.622246 11.00000 0.02010 0.02820 = 0.02015 0.00478 0.00456 -0.00049 AFIX 137 H29A 2 0.743724 0.393840 0.593266 11.00000 -1.50000 H29B 2 0.634365 0.429074 0.624971 11.00000 -1.50000 H29C 2 0.641681 0.330326 0.589433 11.00000 -1.50000 AFIX 0 C30 1 0.802325 0.408469 0.758430 11.00000 0.01402 0.03318 = 0.02997 0.00723 -0.00058 -0.00178 AFIX 137 H30A 2 0.822749 0.389535 0.818481 11.00000 -1.50000 H30B 2 0.773099 0.468417 0.758334 11.00000 -1.50000 H30C 2 0.865366 0.407737 0.726261 11.00000 -1.50000 AFIX 0 C31 1 0.521813 0.186241 0.943181 11.00000 0.02125 0.02196 = 0.01723 0.00808 -0.00052 0.00034 C32 1 0.482411 0.098318 0.902717 11.00000 0.04698 0.02029 = 0.02542 0.00998 0.00156 -0.00238 AFIX 137 H32A 2 0.410044 0.105794 0.873282 11.00000 -1.50000 H32B 2 0.481465 0.053696 0.948482 11.00000 -1.50000 H32C 2 0.530519 0.079218 0.860502 11.00000 -1.50000 AFIX 0 C33 1 0.446031 0.216747 1.008294 11.00000 0.02466 0.03329 = 0.01805 0.00835 0.00232 -0.00250 AFIX 137 H33A 2 0.475364 0.269545 1.038679 11.00000 -1.50000 H33B 2 0.438230 0.169681 1.050603 11.00000 -1.50000 H33C 2 0.375958 0.230553 0.977305 11.00000 -1.50000 AFIX 0 C34 1 0.632243 0.171794 0.993980 11.00000 0.02364 0.04702 = 0.02941 0.02053 -0.00273 0.00464 AFIX 137 H34A 2 0.682178 0.149920 0.954430 11.00000 -1.50000 H34B 2 0.626258 0.128469 1.040244 11.00000 -1.50000 H34C 2 0.658706 0.227784 1.019657 11.00000 -1.50000 HKLF 4 ; # Attachment '- mima51.cif' data_mima51 _database_code_depnum_ccdc_archive 'CCDC 884311' #TrackingRef '- mima51.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H54 D18 Co' _chemical_formula_weight 870.22 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' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.0890(5) _cell_length_b 14.2424(5) _cell_length_c 13.4791(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.734(5) _cell_angle_gamma 90.00 _cell_volume 2350.03(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13797 _cell_measurement_theta_min 3.5032 _cell_measurement_theta_max 72.8248 _exptl_crystal_description prism _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 918 _exptl_absorpt_coefficient_mu 3.135 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.11979 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57644 _diffrn_reflns_av_R_equivalents 0.1048 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 72.98 _reflns_number_total 4662 _reflns_number_gt 3996 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _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 solvent is deutero-benzene! ; _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^)+(0.0739P)^2^+0.9666P] 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 4662 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Co Co 0.5000 0.5000 0.5000 0.01516(14) Uani 1 2 d S . . C1 C 0.39168(16) 0.61269(14) 0.47736(17) 0.0214(4) Uani 1 1 d . . . C2 C 0.49980(15) 0.64504(14) 0.49407(15) 0.0188(4) Uani 1 1 d . . . H2 H 0.5416 0.6850 0.5502 0.023 Uiso 1 1 calc R . . C3 C 0.53533(16) 0.60796(14) 0.41315(17) 0.0219(4) Uani 1 1 d . . . C4 C 0.44186(16) 0.56110(14) 0.33624(17) 0.0216(4) Uani 1 1 d . . . C5 C 0.35400(16) 0.56382(14) 0.37618(16) 0.0203(4) Uani 1 1 d . . . C6 C 0.25299(17) 0.52162(15) 0.31828(17) 0.0222(4) Uani 1 1 d . . . H6 H 0.1950 0.5217 0.3452 0.027 Uiso 1 1 calc R . . C7 C 0.23966(17) 0.48057(15) 0.22263(18) 0.0234(5) Uani 1 1 d . . . H7 H 0.1712 0.4534 0.1824 0.028 Uiso 1 1 calc R . . C8 C 0.32607(18) 0.47794(15) 0.18264(18) 0.0247(5) Uani 1 1 d . . . H8 H 0.3144 0.4492 0.1159 0.030 Uiso 1 1 calc R . . C9 C 0.42615(18) 0.51596(15) 0.23814(18) 0.0233(5) Uani 1 1 d . . . H9 H 0.4841 0.5122 0.2114 0.028 Uiso 1 1 calc R . . C10 C 0.31889(16) 0.63746(14) 0.53889(17) 0.0214(4) Uani 1 1 d . . . H10 H 0.2826 0.5784 0.5493 0.026 Uiso 1 1 calc R . . C11 C 0.38018(17) 0.67903(16) 0.64836(18) 0.0273(5) Uani 1 1 d . . . H11A H 0.4161 0.7382 0.6402 0.033 Uiso 1 1 calc R . . H11B H 0.4378 0.6347 0.6896 0.033 Uiso 1 1 calc R . . C12 C 0.3033(2) 0.69873(17) 0.70908(19) 0.0325(5) Uani 1 1 d . . . H12A H 0.2734 0.6387 0.7240 0.039 Uiso 1 1 calc R . . H12B H 0.3448 0.7288 0.7778 0.039 Uiso 1 1 calc R . . C13 C 0.20946(19) 0.76261(17) 0.64591(19) 0.0321(5) Uani 1 1 d . . . H13A H 0.1575 0.7690 0.6839 0.039 Uiso 1 1 calc R . . H13B H 0.2384 0.8258 0.6401 0.039 Uiso 1 1 calc R . . C14 C 0.14971(17) 0.72366(16) 0.53524(19) 0.0281(5) Uani 1 1 d . . . H14A H 0.0926 0.7686 0.4945 0.034 Uiso 1 1 calc R . . H14B H 0.1134 0.6639 0.5408 0.034 Uiso 1 1 calc R . . C15 C 0.22873(17) 0.70647(15) 0.47636(18) 0.0249(5) Uani 1 1 d . . . H15A H 0.2621 0.7667 0.4672 0.030 Uiso 1 1 calc R . . H15B H 0.1883 0.6804 0.4051 0.030 Uiso 1 1 calc R . . C16 C 0.64186(16) 0.62658(14) 0.39665(17) 0.0218(4) Uani 1 1 d . . . H16 H 0.6674 0.5657 0.3766 0.026 Uiso 1 1 calc R . . C17 C 0.62573(17) 0.69570(15) 0.30502(18) 0.0257(5) Uani 1 1 d . . . H17A H 0.5684 0.6715 0.2402 0.031 Uiso 1 1 calc R . . H17B H 0.6009 0.7569 0.3229 0.031 Uiso 1 1 calc R . . C18 C 0.73139(18) 0.70937(17) 0.28349(18) 0.0289(5) Uani 1 1 d . . . H18A H 0.7520 0.6495 0.2583 0.035 Uiso 1 1 calc R . . H18B H 0.7197 0.7568 0.2268 0.035 Uiso 1 1 calc R . . C19 C 0.82376(18) 0.74143(16) 0.38268(19) 0.0297(5) Uani 1 1 d . . . H19A H 0.8077 0.8054 0.4019 0.036 Uiso 1 1 calc R . . H19B H 0.8925 0.7443 0.3677 0.036 Uiso 1 1 calc R . . C20 C 0.83910(17) 0.67559(16) 0.47570(18) 0.0274(5) Uani 1 1 d . . . H20A H 0.8953 0.7016 0.5401 0.033 Uiso 1 1 calc R . . H20B H 0.8650 0.6138 0.4606 0.033 Uiso 1 1 calc R . . C21 C 0.73160(17) 0.66277(15) 0.49576(17) 0.0253(5) Uani 1 1 d . . . H21A H 0.7428 0.6177 0.5546 0.030 Uiso 1 1 calc R . . H21B H 0.7090 0.7236 0.5170 0.030 Uiso 1 1 calc R . . C91 C 0.0718(2) 0.0658(2) 0.3987(2) 0.0442(7) Uani 1 1 d . . . H91 H 0.0791 0.1029 0.4595 0.053 Uiso 1 1 calc R . . C92 C 0.0451(2) 0.10784(19) 0.3016(2) 0.0414(6) Uani 1 1 d . . . H92 H 0.0349 0.1739 0.2953 0.050 Uiso 1 1 calc R . . C93 C 0.0331(2) 0.0546(2) 0.2126(2) 0.0384(6) Uani 1 1 d . . . H93 H 0.0148 0.0838 0.1452 0.046 Uiso 1 1 calc R . . C94 C 0.0478(2) -0.0415(2) 0.2220(2) 0.0386(6) Uani 1 1 d . . . H94 H 0.0387 -0.0787 0.1610 0.046 Uiso 1 1 calc R . . C95 C 0.0758(2) -0.08356(19) 0.3210(2) 0.0395(6) Uani 1 1 d . . . H95 H 0.0866 -0.1495 0.3278 0.047 Uiso 1 1 calc R . . C96 C 0.0880(2) -0.0298(2) 0.4091(2) 0.0420(6) Uani 1 1 d . . . H96 H 0.1076 -0.0585 0.4769 0.050 Uiso 1 1 calc R . . C97 C 0.3939(2) -0.0209(2) 0.4384(2) 0.0396(6) Uani 1 1 d . . . H97 H 0.3206 -0.0353 0.3959 0.047 Uiso 1 1 calc R . . C98 C 0.4243(2) 0.07082(19) 0.4653(2) 0.0392(6) Uani 1 1 d . . . H98 H 0.3720 0.1198 0.4413 0.047 Uiso 1 1 calc R . . C99 C 0.5304(2) 0.09156(18) 0.5268(2) 0.0399(6) Uani 1 1 d . . . H99 H 0.5514 0.1549 0.5453 0.048 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 Co 0.0125(2) 0.0172(2) 0.0166(2) -0.00017(17) 0.00630(17) 0.00022(16) C1 0.0186(9) 0.0225(10) 0.0224(11) 0.0010(8) 0.0064(8) 0.0017(8) C2 0.0189(10) 0.0160(9) 0.0214(11) -0.0004(7) 0.0070(8) 0.0005(7) C3 0.0193(10) 0.0220(10) 0.0245(11) 0.0022(8) 0.0077(8) 0.0013(8) C4 0.0211(10) 0.0229(10) 0.0217(11) 0.0013(8) 0.0085(8) 0.0005(8) C5 0.0190(9) 0.0218(9) 0.0203(10) 0.0026(8) 0.0073(8) 0.0014(8) C6 0.0174(10) 0.0273(10) 0.0225(11) 0.0028(8) 0.0076(9) 0.0007(8) C7 0.0175(10) 0.0287(10) 0.0218(11) -0.0017(8) 0.0042(9) -0.0014(8) C8 0.0256(11) 0.0295(10) 0.0190(11) -0.0024(9) 0.0080(9) -0.0002(9) C9 0.0230(11) 0.0293(11) 0.0205(11) 0.0012(8) 0.0112(9) 0.0004(8) C10 0.0223(10) 0.0210(10) 0.0251(11) -0.0021(8) 0.0136(9) 0.0000(8) C11 0.0212(10) 0.0333(11) 0.0253(12) 0.0007(9) 0.0055(9) 0.0038(9) C12 0.0357(13) 0.0389(13) 0.0233(12) -0.0045(10) 0.0109(10) 0.0026(10) C13 0.0329(12) 0.0358(12) 0.0339(13) -0.0041(10) 0.0194(11) 0.0068(10) C14 0.0196(10) 0.0346(12) 0.0315(13) 0.0040(10) 0.0109(9) 0.0050(9) C15 0.0237(11) 0.0286(11) 0.0236(11) -0.0011(9) 0.0098(9) -0.0010(8) C16 0.0192(9) 0.0222(10) 0.0279(12) 0.0027(8) 0.0129(9) 0.0009(8) C17 0.0196(10) 0.0286(11) 0.0273(12) 0.0039(9) 0.0064(9) 0.0016(8) C18 0.0258(11) 0.0368(12) 0.0245(12) 0.0068(9) 0.0093(9) 0.0003(9) C19 0.0222(11) 0.0327(12) 0.0361(13) 0.0026(10) 0.0128(10) -0.0058(9) C20 0.0179(10) 0.0338(12) 0.0295(12) 0.0018(9) 0.0070(9) -0.0001(9) C21 0.0244(11) 0.0289(11) 0.0243(11) 0.0082(9) 0.0107(9) 0.0041(9) C91 0.0417(15) 0.0511(16) 0.0407(16) -0.0171(13) 0.0156(12) -0.0109(12) C92 0.0364(13) 0.0372(13) 0.0551(18) -0.0018(12) 0.0216(13) -0.0023(11) C93 0.0262(12) 0.0571(16) 0.0347(14) 0.0087(12) 0.0144(11) 0.0003(11) C94 0.0276(12) 0.0545(16) 0.0355(15) -0.0128(12) 0.0132(11) -0.0012(11) C95 0.0340(13) 0.0394(13) 0.0436(15) -0.0002(12) 0.0117(12) 0.0051(11) C96 0.0353(14) 0.0579(16) 0.0285(14) 0.0028(12) 0.0062(11) -0.0010(12) C97 0.0310(13) 0.0629(17) 0.0274(13) -0.0054(12) 0.0136(11) -0.0080(12) C98 0.0503(16) 0.0449(14) 0.0280(13) 0.0072(11) 0.0208(12) 0.0166(12) C99 0.0611(17) 0.0317(12) 0.0354(14) -0.0055(11) 0.0278(13) -0.0098(12) _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 Co C2 2.067(2) 3_666 ? Co C2 2.067(2) . ? Co C3 2.081(2) 3_666 ? Co C3 2.081(2) . ? Co C1 2.091(2) . ? Co C1 2.091(2) 3_666 ? Co C5 2.237(2) 3_666 ? Co C5 2.237(2) . ? Co C4 2.240(2) . ? Co C4 2.240(2) 3_666 ? C1 C2 1.428(3) . ? C1 C5 1.453(3) . ? C1 C10 1.510(3) . ? C2 C3 1.430(3) . ? C3 C4 1.456(3) . ? C3 C16 1.511(3) . ? C4 C9 1.418(3) . ? C4 C5 1.433(3) . ? C5 C6 1.410(3) . ? C6 C7 1.369(3) . ? C7 C8 1.415(3) . ? C8 C9 1.369(3) . ? C10 C11 1.527(3) . ? C10 C15 1.538(3) . ? C11 C12 1.532(3) . ? C12 C13 1.523(3) . ? C13 C14 1.523(3) . ? C14 C15 1.530(3) . ? C16 C21 1.523(3) . ? C16 C17 1.534(3) . ? C17 C18 1.523(3) . ? C18 C19 1.521(3) . ? C19 C20 1.521(3) . ? C20 C21 1.535(3) . ? C91 C92 1.368(4) . ? C91 C96 1.378(4) . ? C92 C93 1.380(4) . ? C93 C94 1.382(4) . ? C94 C95 1.388(4) . ? C95 C96 1.374(4) . ? C97 C99 1.373(4) 3_656 ? C97 C98 1.377(4) . ? C98 C99 1.373(4) . ? C99 C97 1.373(4) 3_656 ? 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 C2 Co C2 180.0 3_666 . ? C2 Co C3 40.32(8) 3_666 3_666 ? C2 Co C3 139.69(8) . 3_666 ? C2 Co C3 139.68(8) 3_666 . ? C2 Co C3 40.32(8) . . ? C3 Co C3 180.0 3_666 . ? C2 Co C1 139.83(7) 3_666 . ? C2 Co C1 40.17(7) . . ? C3 Co C1 112.02(8) 3_666 . ? C3 Co C1 67.98(8) . . ? C2 Co C1 40.17(7) 3_666 3_666 ? C2 Co C1 139.83(7) . 3_666 ? C3 Co C1 67.98(8) 3_666 3_666 ? C3 Co C1 112.02(8) . 3_666 ? C1 Co C1 180.00(7) . 3_666 ? C2 Co C5 64.92(7) 3_666 3_666 ? C2 Co C5 115.08(7) . 3_666 ? C3 Co C5 65.26(7) 3_666 3_666 ? C3 Co C5 114.74(8) . 3_666 ? C1 Co C5 140.95(8) . 3_666 ? C1 Co C5 39.05(8) 3_666 3_666 ? C2 Co C5 115.08(7) 3_666 . ? C2 Co C5 64.92(7) . . ? C3 Co C5 114.74(8) 3_666 . ? C3 Co C5 65.26(7) . . ? C1 Co C5 39.05(8) . . ? C1 Co C5 140.95(8) 3_666 . ? C5 Co C5 180.0 3_666 . ? C2 Co C4 114.93(8) 3_666 . ? C2 Co C4 65.07(8) . . ? C3 Co C4 140.85(8) 3_666 . ? C3 Co C4 39.15(8) . . ? C1 Co C4 65.28(8) . . ? C1 Co C4 114.72(8) 3_666 . ? C5 Co C4 142.68(7) 3_666 . ? C5 Co C4 37.32(7) . . ? C2 Co C4 65.07(8) 3_666 3_666 ? C2 Co C4 114.93(8) . 3_666 ? C3 Co C4 39.15(8) 3_666 3_666 ? C3 Co C4 140.85(8) . 3_666 ? C1 Co C4 114.72(8) . 3_666 ? C1 Co C4 65.28(8) 3_666 3_666 ? C5 Co C4 37.32(7) 3_666 3_666 ? C5 Co C4 142.68(7) . 3_666 ? C4 Co C4 180.00(11) . 3_666 ? C2 C1 C5 106.89(17) . . ? C2 C1 C10 128.37(19) . . ? C5 C1 C10 123.85(18) . . ? C2 C1 Co 69.01(11) . . ? C5 C1 Co 75.91(11) . . ? C10 C1 Co 128.77(14) . . ? C1 C2 C3 109.41(18) . . ? C1 C2 Co 70.81(11) . . ? C3 C2 Co 70.37(11) . . ? C2 C3 C4 107.11(17) . . ? C2 C3 C16 127.87(18) . . ? C4 C3 C16 124.21(19) . . ? C2 C3 Co 69.31(11) . . ? C4 C3 Co 76.34(12) . . ? C16 C3 Co 127.79(14) . . ? C9 C4 C5 119.47(19) . . ? C9 C4 C3 132.82(19) . . ? C5 C4 C3 107.70(18) . . ? C9 C4 Co 128.98(15) . . ? C5 C4 Co 71.22(12) . . ? C3 C4 Co 64.52(11) . . ? C6 C5 C4 120.04(19) . . ? C6 C5 C1 131.60(19) . . ? C4 C5 C1 108.35(17) . . ? C6 C5 Co 128.73(14) . . ? C4 C5 Co 71.46(11) . . ? C1 C5 Co 65.04(11) . . ? C7 C6 C5 119.0(2) . . ? C6 C7 C8 121.2(2) . . ? C9 C8 C7 121.4(2) . . ? C8 C9 C4 118.9(2) . . ? C1 C10 C11 113.80(17) . . ? C1 C10 C15 111.05(17) . . ? C11 C10 C15 108.69(17) . . ? C10 C11 C12 111.56(18) . . ? C13 C12 C11 111.29(19) . . ? C14 C13 C12 111.28(19) . . ? C13 C14 C15 111.07(18) . . ? C14 C15 C10 110.27(18) . . ? C3 C16 C21 113.30(18) . . ? C3 C16 C17 111.09(17) . . ? C21 C16 C17 109.43(17) . . ? C18 C17 C16 111.10(17) . . ? C19 C18 C17 111.34(19) . . ? C18 C19 C20 111.81(18) . . ? C19 C20 C21 110.91(17) . . ? C16 C21 C20 110.87(18) . . ? C92 C91 C96 120.5(3) . . ? C91 C92 C93 120.2(3) . . ? C92 C93 C94 119.7(2) . . ? C93 C94 C95 119.8(2) . . ? C96 C95 C94 120.0(3) . . ? C95 C96 C91 119.8(3) . . ? C99 C97 C98 119.9(3) 3_656 . ? C99 C98 C97 120.0(2) . . ? C97 C99 C98 120.1(2) 3_656 . ? 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 C2 Co C1 C2 180.0 3_666 . . . ? C3 Co C1 C2 142.75(12) 3_666 . . . ? C3 Co C1 C2 -37.25(12) . . . . ? C1 Co C1 C2 -126(6) 3_666 . . . ? C5 Co C1 C2 65.35(17) 3_666 . . . ? C5 Co C1 C2 -114.65(17) . . . . ? C4 Co C1 C2 -79.97(12) . . . . ? C4 Co C1 C2 100.03(12) 3_666 . . . ? C2 Co C1 C5 -65.34(17) 3_666 . . . ? C2 Co C1 C5 114.65(17) . . . . ? C3 Co C1 C5 -102.60(12) 3_666 . . . ? C3 Co C1 C5 77.40(12) . . . . ? C1 Co C1 C5 -11(6) 3_666 . . . ? C5 Co C1 C5 180.0 3_666 . . . ? C4 Co C1 C5 34.69(11) . . . . ? C4 Co C1 C5 -145.31(11) 3_666 . . . ? C2 Co C1 C10 57.0(2) 3_666 . . . ? C2 Co C1 C10 -123.0(2) . . . . ? C3 Co C1 C10 19.8(2) 3_666 . . . ? C3 Co C1 C10 -160.2(2) . . . . ? C1 Co C1 C10 111(6) 3_666 . . . ? C5 Co C1 C10 -57.7(2) 3_666 . . . ? C5 Co C1 C10 122.4(2) . . . . ? C4 Co C1 C10 157.0(2) . . . . ? C4 Co C1 C10 -23.0(2) 3_666 . . . ? C5 C1 C2 C3 -7.1(2) . . . . ? C10 C1 C2 C3 -176.49(19) . . . . ? Co C1 C2 C3 60.02(14) . . . . ? C5 C1 C2 Co -67.11(13) . . . . ? C10 C1 C2 Co 123.5(2) . . . . ? C2 Co C2 C1 47(8) 3_666 . . . ? C3 Co C2 C1 -60.15(17) 3_666 . . . ? C3 Co C2 C1 119.85(17) . . . . ? C1 Co C2 C1 180.0 3_666 . . . ? C5 Co C2 C1 -140.79(12) 3_666 . . . ? C5 Co C2 C1 39.21(12) . . . . ? C4 Co C2 C1 80.55(12) . . . . ? C4 Co C2 C1 -99.44(12) 3_666 . . . ? C2 Co C2 C3 -73(100) 3_666 . . . ? C3 Co C2 C3 180.000(1) 3_666 . . . ? C1 Co C2 C3 -119.85(17) . . . . ? C1 Co C2 C3 60.15(17) 3_666 . . . ? C5 Co C2 C3 99.36(12) 3_666 . . . ? C5 Co C2 C3 -80.64(12) . . . . ? C4 Co C2 C3 -39.29(11) . . . . ? C4 Co C2 C3 140.71(11) 3_666 . . . ? C1 C2 C3 C4 7.3(2) . . . . ? Co C2 C3 C4 67.64(14) . . . . ? C1 C2 C3 C16 177.29(19) . . . . ? Co C2 C3 C16 -122.4(2) . . . . ? C1 C2 C3 Co -60.29(14) . . . . ? C2 Co C3 C2 180.0 3_666 . . . ? C3 Co C3 C2 169(5) 3_666 . . . ? C1 Co C3 C2 37.12(11) . . . . ? C1 Co C3 C2 -142.88(11) 3_666 . . . ? C5 Co C3 C2 -100.27(12) 3_666 . . . ? C5 Co C3 C2 79.73(12) . . . . ? C4 Co C3 C2 114.55(16) . . . . ? C4 Co C3 C2 -65.45(16) 3_666 . . . ? C2 Co C3 C4 65.44(16) 3_666 . . . ? C2 Co C3 C4 -114.55(16) . . . . ? C3 Co C3 C4 54(5) 3_666 . . . ? C1 Co C3 C4 -77.43(12) . . . . ? C1 Co C3 C4 102.57(12) 3_666 . . . ? C5 Co C3 C4 145.18(11) 3_666 . . . ? C5 Co C3 C4 -34.83(11) . . . . ? C4 Co C3 C4 180.0 3_666 . . . ? C2 Co C3 C16 -57.5(2) 3_666 . . . ? C2 Co C3 C16 122.5(2) . . . . ? C3 Co C3 C16 -69(5) 3_666 . . . ? C1 Co C3 C16 159.6(2) . . . . ? C1 Co C3 C16 -20.4(2) 3_666 . . . ? C5 Co C3 C16 22.2(2) 3_666 . . . ? C5 Co C3 C16 -157.8(2) . . . . ? C4 Co C3 C16 -122.9(2) . . . . ? C4 Co C3 C16 57.1(2) 3_666 . . . ? C2 C3 C4 C9 176.5(2) . . . . ? C16 C3 C4 C9 6.1(4) . . . . ? Co C3 C4 C9 -120.6(2) . . . . ? C2 C3 C4 C5 -4.7(2) . . . . ? C16 C3 C4 C5 -175.09(18) . . . . ? Co C3 C4 C5 58.23(14) . . . . ? C2 C3 C4 Co -62.92(13) . . . . ? C16 C3 C4 Co 126.7(2) . . . . ? C2 Co C4 C9 -13.9(2) 3_666 . . . ? C2 Co C4 C9 166.1(2) . . . . ? C3 Co C4 C9 -54.3(2) 3_666 . . . ? C3 Co C4 C9 125.7(2) . . . . ? C1 Co C4 C9 -149.4(2) . . . . ? C1 Co C4 C9 30.6(2) 3_666 . . . ? C5 Co C4 C9 66.8(2) 3_666 . . . ? C5 Co C4 C9 -113.2(2) . . . . ? C4 Co C4 C9 -108(21) 3_666 . . . ? C2 Co C4 C5 99.28(12) 3_666 . . . ? C2 Co C4 C5 -80.72(12) . . . . ? C3 Co C4 C5 58.82(17) 3_666 . . . ? C3 Co C4 C5 -121.19(17) . . . . ? C1 Co C4 C5 -36.25(12) . . . . ? C1 Co C4 C5 143.75(12) 3_666 . . . ? C5 Co C4 C5 180.0 3_666 . . . ? C4 Co C4 C5 6(21) 3_666 . . . ? C2 Co C4 C3 -139.54(11) 3_666 . . . ? C2 Co C4 C3 40.47(11) . . . . ? C3 Co C4 C3 180.0 3_666 . . . ? C1 Co C4 C3 84.93(13) . . . . ? C1 Co C4 C3 -95.07(13) 3_666 . . . ? C5 Co C4 C3 -58.81(17) 3_666 . . . ? C5 Co C4 C3 121.19(17) . . . . ? C4 Co C4 C3 127(21) 3_666 . . . ? C9 C4 C5 C6 0.2(3) . . . . ? C3 C4 C5 C6 -178.80(18) . . . . ? Co C4 C5 C6 -124.64(19) . . . . ? C9 C4 C5 C1 179.36(18) . . . . ? C3 C4 C5 C1 0.4(2) . . . . ? Co C4 C5 C1 54.54(14) . . . . ? C9 C4 C5 Co 124.82(19) . . . . ? C3 C4 C5 Co -54.16(14) . . . . ? C2 C1 C5 C6 -176.9(2) . . . . ? C10 C1 C5 C6 -6.9(3) . . . . ? Co C1 C5 C6 120.6(2) . . . . ? C2 C1 C5 C4 4.1(2) . . . . ? C10 C1 C5 C4 174.07(18) . . . . ? Co C1 C5 C4 -58.41(14) . . . . ? C2 C1 C5 Co 62.48(13) . . . . ? C10 C1 C5 Co -127.5(2) . . . . ? C2 Co C5 C6 15.2(2) 3_666 . . . ? C2 Co C5 C6 -164.8(2) . . . . ? C3 Co C5 C6 -29.4(2) 3_666 . . . ? C3 Co C5 C6 150.6(2) . . . . ? C1 Co C5 C6 -124.4(2) . . . . ? C1 Co C5 C6 55.6(2) 3_666 . . . ? C5 Co C5 C6 -146(4) 3_666 . . . ? C4 Co C5 C6 114.1(2) . . . . ? C4 Co C5 C6 -65.9(2) 3_666 . . . ? C2 Co C5 C4 -98.85(12) 3_666 . . . ? C2 Co C5 C4 81.15(12) . . . . ? C3 Co C5 C4 -143.51(12) 3_666 . . . ? C3 Co C5 C4 36.49(12) . . . . ? C1 Co C5 C4 121.49(17) . . . . ? C1 Co C5 C4 -58.51(17) 3_666 . . . ? C5 Co C5 C4 100(4) 3_666 . . . ? C4 Co C5 C4 180.0 3_666 . . . ? C2 Co C5 C1 139.66(11) 3_666 . . . ? C2 Co C5 C1 -40.34(11) . . . . ? C3 Co C5 C1 95.00(13) 3_666 . . . ? C3 Co C5 C1 -85.00(13) . . . . ? C1 Co C5 C1 180.0 3_666 . . . ? C5 Co C5 C1 -22(4) 3_666 . . . ? C4 Co C5 C1 -121.49(17) . . . . ? C4 Co C5 C1 58.51(17) 3_666 . . . ? C4 C5 C6 C7 -1.7(3) . . . . ? C1 C5 C6 C7 179.3(2) . . . . ? Co C5 C6 C7 -91.3(2) . . . . ? C5 C6 C7 C8 1.5(3) . . . . ? C6 C7 C8 C9 0.2(3) . . . . ? C7 C8 C9 C4 -1.8(3) . . . . ? C5 C4 C9 C8 1.6(3) . . . . ? C3 C4 C9 C8 -179.8(2) . . . . ? Co C4 C9 C8 90.5(2) . . . . ? C2 C1 C10 C11 -18.6(3) . . . . ? C5 C1 C10 C11 173.66(19) . . . . ? Co C1 C10 C11 74.3(2) . . . . ? C2 C1 C10 C15 104.4(2) . . . . ? C5 C1 C10 C15 -63.3(2) . . . . ? Co C1 C10 C15 -162.69(15) . . . . ? C1 C10 C11 C12 -177.47(18) . . . . ? C15 C10 C11 C12 58.2(2) . . . . ? C10 C11 C12 C13 -55.9(3) . . . . ? C11 C12 C13 C14 53.6(3) . . . . ? C12 C13 C14 C15 -55.3(3) . . . . ? C13 C14 C15 C10 58.5(2) . . . . ? C1 C10 C15 C14 174.80(17) . . . . ? C11 C10 C15 C14 -59.3(2) . . . . ? C2 C3 C16 C21 20.6(3) . . . . ? C4 C3 C16 C21 -171.08(18) . . . . ? Co C3 C16 C21 -71.5(2) . . . . ? C2 C3 C16 C17 -103.1(2) . . . . ? C4 C3 C16 C17 65.3(3) . . . . ? Co C3 C16 C17 164.80(15) . . . . ? C3 C16 C17 C18 -176.16(18) . . . . ? C21 C16 C17 C18 58.0(2) . . . . ? C16 C17 C18 C19 -56.0(2) . . . . ? C17 C18 C19 C20 54.1(3) . . . . ? C18 C19 C20 C21 -54.3(3) . . . . ? C3 C16 C21 C20 177.14(17) . . . . ? C17 C16 C21 C20 -58.3(2) . . . . ? C19 C20 C21 C16 56.8(2) . . . . ? C96 C91 C92 C93 0.7(4) . . . . ? C91 C92 C93 C94 0.2(4) . . . . ? C92 C93 C94 C95 -0.8(3) . . . . ? C93 C94 C95 C96 0.6(4) . . . . ? C94 C95 C96 C91 0.3(4) . . . . ? C92 C91 C96 C95 -0.9(4) . . . . ? C99 C97 C98 C99 0.0(4) 3_656 . . . ? C97 C98 C99 C97 0.0(4) . . . 3_656 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 72.98 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.645 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.058 _iucr_refine_instructions_details ; TITL mima51 in P2(1)/c CELL 1.54184 13.089042 14.242444 13.479092 90.0000 110.7341 90.0000 ZERR 2.00 0.000500 0.000500 0.000700 0.0000 0.0050 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H Co UNIT 120.00 144.00 2.00 TEMP -173 SIZE 0.2 0.04 0.02 ACTA 150 CONF L.S. 4 FMAP 2 PLAN 10 WGHT 0.073900 0.966600 FVAR 3.85828 CO 3 0.500000 0.500000 0.500000 10.50000 0.01254 0.01723 = 0.01663 -0.00017 0.00630 0.00022 C1 1 0.391677 0.612691 0.477362 11.00000 0.01861 0.02245 = 0.02243 0.00098 0.00641 0.00166 C2 1 0.499798 0.645042 0.494069 11.00000 0.01886 0.01601 = 0.02139 -0.00043 0.00698 0.00047 AFIX 43 H2 2 0.541596 0.684985 0.550215 11.00000 -1.20000 AFIX 0 C3 1 0.535333 0.607962 0.413151 11.00000 0.01927 0.02198 = 0.02454 0.00216 0.00772 0.00128 C4 1 0.441864 0.561102 0.336239 11.00000 0.02106 0.02294 = 0.02167 0.00133 0.00855 0.00048 C5 1 0.354004 0.563823 0.376185 11.00000 0.01898 0.02179 = 0.02031 0.00264 0.00728 0.00139 C6 1 0.252990 0.521622 0.318278 11.00000 0.01737 0.02727 = 0.02250 0.00284 0.00761 0.00074 AFIX 43 H6 2 0.195028 0.521668 0.345217 11.00000 -1.20000 AFIX 0 C7 1 0.239665 0.480567 0.222628 11.00000 0.01749 0.02873 = 0.02176 -0.00168 0.00418 -0.00143 AFIX 43 H7 2 0.171223 0.453373 0.182418 11.00000 -1.20000 AFIX 0 C8 1 0.326065 0.477943 0.182639 11.00000 0.02563 0.02951 = 0.01898 -0.00242 0.00799 -0.00023 AFIX 43 H8 2 0.314392 0.449211 0.115909 11.00000 -1.20000 AFIX 0 C9 1 0.426150 0.515961 0.238141 11.00000 0.02305 0.02925 = 0.02045 0.00119 0.01115 0.00036 AFIX 43 H9 2 0.484113 0.512163 0.211374 11.00000 -1.20000 AFIX 0 C10 1 0.318892 0.637458 0.538895 11.00000 0.02234 0.02101 = 0.02513 -0.00214 0.01360 0.00005 AFIX 13 H10 2 0.282590 0.578399 0.549281 11.00000 -1.20000 AFIX 0 C11 1 0.380178 0.679029 0.648356 11.00000 0.02119 0.03330 = 0.02533 0.00070 0.00553 0.00382 AFIX 23 H11A 2 0.416079 0.738224 0.640225 11.00000 -1.20000 H11B 2 0.437803 0.634690 0.689634 11.00000 -1.20000 AFIX 0 C12 1 0.303265 0.698732 0.709077 11.00000 0.03568 0.03887 = 0.02330 -0.00446 0.01088 0.00263 AFIX 23 H12A 2 0.273433 0.638687 0.724024 11.00000 -1.20000 H12B 2 0.344819 0.728801 0.777776 11.00000 -1.20000 AFIX 0 C13 1 0.209456 0.762607 0.645906 11.00000 0.03289 0.03575 = 0.03387 -0.00408 0.01941 0.00682 AFIX 23 H13A 2 0.157477 0.769042 0.683893 11.00000 -1.20000 H13B 2 0.238392 0.825779 0.640095 11.00000 -1.20000 AFIX 0 C14 1 0.149709 0.723661 0.535241 11.00000 0.01963 0.03461 = 0.03154 0.00404 0.01093 0.00501 AFIX 23 H14A 2 0.092586 0.768640 0.494523 11.00000 -1.20000 H14B 2 0.113411 0.663939 0.540810 11.00000 -1.20000 AFIX 0 C15 1 0.228734 0.706469 0.476356 11.00000 0.02371 0.02858 = 0.02364 -0.00108 0.00982 -0.00103 AFIX 23 H15A 2 0.262097 0.766692 0.467159 11.00000 -1.20000 H15B 2 0.188277 0.680434 0.405108 11.00000 -1.20000 AFIX 0 C16 1 0.641864 0.626581 0.396647 11.00000 0.01920 0.02218 = 0.02787 0.00271 0.01291 0.00094 AFIX 13 H16 2 0.667439 0.565739 0.376600 11.00000 -1.20000 AFIX 0 C17 1 0.625725 0.695696 0.305020 11.00000 0.01963 0.02858 = 0.02727 0.00387 0.00636 0.00165 AFIX 23 H17A 2 0.568383 0.671546 0.240236 11.00000 -1.20000 H17B 2 0.600900 0.756933 0.322932 11.00000 -1.20000 AFIX 0 C18 1 0.731386 0.709374 0.283488 11.00000 0.02577 0.03677 = 0.02449 0.00684 0.00931 0.00033 AFIX 23 H18A 2 0.752013 0.649508 0.258297 11.00000 -1.20000 H18B 2 0.719682 0.756764 0.226794 11.00000 -1.20000 AFIX 0 C19 1 0.823763 0.741426 0.382677 11.00000 0.02218 0.03272 = 0.03606 0.00261 0.01279 -0.00580 AFIX 23 H19A 2 0.807685 0.805395 0.401902 11.00000 -1.20000 H19B 2 0.892466 0.744316 0.367668 11.00000 -1.20000 AFIX 0 C20 1 0.839097 0.675591 0.475701 11.00000 0.01788 0.03380 = 0.02948 0.00181 0.00697 -0.00009 AFIX 23 H20A 2 0.895330 0.701551 0.540134 11.00000 -1.20000 H20B 2 0.865042 0.613807 0.460590 11.00000 -1.20000 AFIX 0 C21 1 0.731603 0.662767 0.495761 11.00000 0.02437 0.02890 = 0.02435 0.00816 0.01071 0.00413 AFIX 23 H21A 2 0.742816 0.617729 0.554626 11.00000 -1.20000 H21B 2 0.709002 0.723597 0.517006 11.00000 -1.20000 AFIX 0 C91 1 0.071771 0.065831 0.398741 11.00000 0.04170 0.05109 = 0.04067 -0.01706 0.01556 -0.01089 AFIX 43 H91 2 0.079121 0.102860 0.459509 11.00000 -1.20000 AFIX 0 C92 1 0.045123 0.107841 0.301558 11.00000 0.03641 0.03718 = 0.05510 -0.00176 0.02161 -0.00225 AFIX 43 H92 2 0.034874 0.173908 0.295302 11.00000 -1.20000 AFIX 0 C93 1 0.033081 0.054578 0.212593 11.00000 0.02623 0.05713 = 0.03474 0.00868 0.01444 0.00031 AFIX 43 H93 2 0.014780 0.083840 0.145185 11.00000 -1.20000 AFIX 0 C94 1 0.047773 -0.041507 0.222045 11.00000 0.02763 0.05452 = 0.03548 -0.01283 0.01324 -0.00119 AFIX 43 H94 2 0.038685 -0.078679 0.160985 11.00000 -1.20000 AFIX 0 C95 1 0.075841 -0.083556 0.320984 11.00000 0.03396 0.03943 = 0.04360 -0.00021 0.01174 0.00507 AFIX 43 H95 2 0.086642 -0.149543 0.327806 11.00000 -1.20000 AFIX 0 C96 1 0.088025 -0.029801 0.409112 11.00000 0.03532 0.05793 = 0.02851 0.00278 0.00621 -0.00104 AFIX 43 H96 2 0.107585 -0.058469 0.476945 11.00000 -1.20000 AFIX 0 C97 1 0.393914 -0.020924 0.438428 11.00000 0.03100 0.06291 = 0.02744 -0.00537 0.01360 -0.00798 AFIX 43 H97 2 0.320593 -0.035347 0.395867 11.00000 -1.20000 AFIX 0 C98 1 0.424345 0.070820 0.465300 11.00000 0.05033 0.04493 = 0.02802 0.00720 0.02080 0.01665 AFIX 43 H98 2 0.372027 0.119756 0.441311 11.00000 -1.20000 AFIX 0 C99 1 0.530370 0.091563 0.526802 11.00000 0.06115 0.03170 = 0.03542 -0.00552 0.02779 -0.00980 AFIX 43 H99 2 0.551357 0.154883 0.545320 11.00000 -1.20000 HKLF 4 ; # Attachment '- mima52.cif' data_mima52 _database_code_depnum_ccdc_archive 'CCDC 884312' #TrackingRef '- mima52.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H29 Fe I O2' _chemical_formula_weight 472.17 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' Fe Fe -1.1336 3.1974 '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 orthorhombic _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 15.3534(3) _cell_length_b 10.4548(2) _cell_length_c 12.3471(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1981.92(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 30097 _cell_measurement_theta_min 3.5768 _cell_measurement_theta_max 75.6778 _exptl_crystal_description needle _exptl_crystal_colour 'brown-violet dichroic' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 18.373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.05459 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49188 _diffrn_reflns_av_R_equivalents 0.0983 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.23 _diffrn_reflns_theta_max 75.87 _reflns_number_total 3932 _reflns_number_gt 3840 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _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. ; _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^)+(0.0479P)^2^+0.4039P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.034(5) _refine_ls_number_reflns 3932 _refine_ls_number_parameters 217 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _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 Fe Fe 0.44350(3) 0.65644(4) 0.80693(4) 0.01154(11) Uani 1 1 d . . . I I 0.372845(12) 0.633487(17) 0.99872(3) 0.02123(8) Uani 1 1 d . . . O1 O 0.58136(15) 0.4712(2) 0.8522(2) 0.0235(5) Uani 1 1 d . . . O2 O 0.55831(18) 0.8537(2) 0.8962(3) 0.0278(6) Uani 1 1 d . . . C1 C 0.43477(18) 0.7404(3) 0.6531(3) 0.0122(6) Uani 1 1 d . . . C2 C 0.35338(19) 0.7657(3) 0.7125(3) 0.0114(6) Uani 1 1 d . . . C3 C 0.3167(2) 0.6429(3) 0.7368(3) 0.0140(7) Uani 1 1 d . . . H3 H 0.2637 0.6303 0.7750 0.017 Uiso 1 1 calc R . . C4 C 0.37004(17) 0.5423(3) 0.6964(3) 0.0111(6) Uani 1 1 d . . . C5 C 0.44245(19) 0.6038(3) 0.6457(3) 0.0135(6) Uani 1 1 d . . . H5 H 0.4893 0.5602 0.6116 0.016 Uiso 1 1 calc R . . C6 C 0.49818(19) 0.8252(3) 0.5884(3) 0.0137(6) Uani 1 1 d . . . C7 C 0.5881(2) 0.7605(3) 0.5813(3) 0.0209(7) Uani 1 1 d . . . H7A H 0.5830 0.6806 0.5403 0.031 Uiso 1 1 calc R . . H7B H 0.6094 0.7420 0.6544 0.031 Uiso 1 1 calc R . . H7C H 0.6290 0.8178 0.5445 0.031 Uiso 1 1 calc R . . C8 C 0.5140(2) 0.9611(3) 0.6322(3) 0.0180(6) Uani 1 1 d . . . H8A H 0.5548 1.0062 0.5845 0.027 Uiso 1 1 calc R . . H8B H 0.5387 0.9560 0.7053 0.027 Uiso 1 1 calc R . . H8C H 0.4587 1.0078 0.6347 0.027 Uiso 1 1 calc R . . C9 C 0.4602(2) 0.8345(3) 0.4738(3) 0.0184(7) Uani 1 1 d . . . H9A H 0.4044 0.8802 0.4763 0.028 Uiso 1 1 calc R . . H9B H 0.4510 0.7483 0.4448 0.028 Uiso 1 1 calc R . . H9C H 0.5008 0.8811 0.4270 0.028 Uiso 1 1 calc R . . C10 C 0.3022(2) 0.8882(3) 0.7395(3) 0.0159(7) Uani 1 1 d . . . C11 C 0.2806(2) 0.9620(3) 0.6348(3) 0.0182(6) Uani 1 1 d . . . H11A H 0.2392 1.0306 0.6512 0.027 Uiso 1 1 calc R . . H11B H 0.2548 0.9034 0.5818 0.027 Uiso 1 1 calc R . . H11C H 0.3341 0.9990 0.6048 0.027 Uiso 1 1 calc R . . C12 C 0.3500(2) 0.9750(3) 0.8213(3) 0.0195(6) Uani 1 1 d . . . H12A H 0.4066 1.0001 0.7915 0.029 Uiso 1 1 calc R . . H12B H 0.3588 0.9284 0.8893 0.029 Uiso 1 1 calc R . . H12C H 0.3150 1.0516 0.8351 0.029 Uiso 1 1 calc R . . C13 C 0.2148(2) 0.8533(3) 0.7921(4) 0.0229(9) Uani 1 1 d . . . H13A H 0.1840 0.9316 0.8126 0.034 Uiso 1 1 calc R . . H13B H 0.2253 0.8011 0.8567 0.034 Uiso 1 1 calc R . . H13C H 0.1794 0.8047 0.7404 0.034 Uiso 1 1 calc R . . C14 C 0.3471(2) 0.4010(3) 0.6935(3) 0.0140(6) Uani 1 1 d . . . C15 C 0.4236(2) 0.3161(3) 0.7267(4) 0.0258(8) Uani 1 1 d . . . H15A H 0.4095 0.2265 0.7115 0.039 Uiso 1 1 calc R . . H15B H 0.4350 0.3265 0.8043 0.039 Uiso 1 1 calc R . . H15C H 0.4756 0.3408 0.6855 0.039 Uiso 1 1 calc R . . C16 C 0.3217(3) 0.3686(3) 0.5765(4) 0.0259(8) Uani 1 1 d . . . H16A H 0.2746 0.4253 0.5529 0.039 Uiso 1 1 calc R . . H16B H 0.3020 0.2795 0.5728 0.039 Uiso 1 1 calc R . . H16C H 0.3723 0.3801 0.5292 0.039 Uiso 1 1 calc R . . C17 C 0.2707(3) 0.3731(3) 0.7690(4) 0.0273(9) Uani 1 1 d . . . H17A H 0.2188 0.4181 0.7430 0.041 Uiso 1 1 calc R . . H17B H 0.2849 0.4024 0.8423 0.041 Uiso 1 1 calc R . . H17C H 0.2594 0.2808 0.7701 0.041 Uiso 1 1 calc R . . C18 C 0.5253(2) 0.5418(3) 0.8369(3) 0.0178(6) Uani 1 1 d . . . C19 C 0.5109(2) 0.7789(3) 0.8613(3) 0.0197(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0120(2) 0.00932(17) 0.0133(3) 0.00069(19) -0.00158(19) 0.00039(15) I 0.02586(12) 0.02383(11) 0.01400(12) 0.00297(10) 0.00237(10) 0.00437(6) O1 0.0165(11) 0.0181(11) 0.0359(15) 0.0023(10) -0.0080(10) 0.0041(9) O2 0.0336(14) 0.0174(11) 0.0325(18) -0.0003(10) -0.0152(12) -0.0065(9) C1 0.0105(13) 0.0133(13) 0.0129(15) 0.0022(11) -0.0013(11) -0.0006(10) C2 0.0097(12) 0.0125(13) 0.0121(16) 0.0014(11) -0.0019(11) 0.0008(10) C3 0.0077(13) 0.0146(14) 0.0196(19) -0.0015(11) -0.0030(12) -0.0004(10) C4 0.0098(13) 0.0111(13) 0.0124(16) 0.0001(12) -0.0028(10) 0.0010(9) C5 0.0126(14) 0.0126(13) 0.0154(16) -0.0005(12) -0.0014(12) 0.0012(10) C6 0.0122(14) 0.0112(13) 0.0177(18) 0.0006(11) -0.0002(12) -0.0013(10) C7 0.0126(15) 0.0175(14) 0.032(2) 0.0041(14) 0.0039(13) 0.0002(11) C8 0.0183(14) 0.0118(13) 0.0238(18) 0.0023(12) -0.0006(13) -0.0052(11) C9 0.0203(15) 0.0174(13) 0.017(2) 0.0011(12) 0.0030(12) -0.0025(11) C10 0.0139(15) 0.0132(12) 0.021(2) -0.0020(13) 0.0015(13) 0.0049(11) C11 0.0189(15) 0.0160(14) 0.0199(18) 0.0028(12) -0.0014(13) 0.0039(11) C12 0.0232(14) 0.0133(13) 0.0218(18) -0.0037(13) -0.0008(14) 0.0016(12) C13 0.0189(18) 0.0193(15) 0.031(3) 0.0003(14) 0.0074(16) 0.0040(11) C14 0.0127(13) 0.0092(12) 0.0200(18) 0.0006(12) 0.0002(13) -0.0020(11) C15 0.0220(17) 0.0098(14) 0.046(3) 0.0043(14) -0.0077(15) -0.0007(12) C16 0.037(2) 0.0168(15) 0.024(2) -0.0021(12) -0.0012(16) -0.0055(12) C17 0.030(2) 0.0175(15) 0.035(3) -0.0036(13) 0.0148(18) -0.0103(12) C18 0.0192(15) 0.0150(13) 0.0192(18) -0.0027(11) -0.0018(12) -0.0065(11) C19 0.0239(16) 0.0190(15) 0.0161(17) 0.0049(12) -0.0046(13) 0.0028(12) _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 Fe C18 1.775(3) . ? Fe C19 1.778(3) . ? Fe C5 2.066(3) . ? Fe C1 2.096(3) . ? Fe C3 2.135(3) . ? Fe C4 2.135(3) . ? Fe C2 2.139(3) . ? Fe I 2.6158(7) . ? O1 C18 1.150(4) . ? O2 C19 1.152(4) . ? C1 C5 1.437(4) . ? C1 C2 1.473(4) . ? C1 C6 1.540(4) . ? C2 C3 1.433(4) . ? C2 C10 1.539(4) . ? C3 C4 1.423(4) . ? C4 C5 1.429(4) . ? C4 C14 1.519(4) . ? C6 C9 1.534(5) . ? C6 C7 1.539(4) . ? C6 C8 1.540(4) . ? C10 C13 1.535(4) . ? C10 C11 1.542(5) . ? C10 C12 1.543(5) . ? C14 C17 1.526(5) . ? C14 C15 1.529(4) . ? C14 C16 1.534(5) . ? 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 C18 Fe C19 89.76(14) . . ? C18 Fe C5 91.53(14) . . ? C19 Fe C5 124.07(15) . . ? C18 Fe C1 121.15(14) . . ? C19 Fe C1 94.43(14) . . ? C5 Fe C1 40.38(11) . . ? C18 Fe C3 133.22(12) . . ? C19 Fe C3 137.01(13) . . ? C5 Fe C3 65.44(13) . . ? C1 Fe C3 66.56(12) . . ? C18 Fe C4 97.46(12) . . ? C19 Fe C4 162.03(15) . . ? C5 Fe C4 39.72(12) . . ? C1 Fe C4 67.75(12) . . ? C3 Fe C4 38.93(11) . . ? C18 Fe C2 158.70(14) . . ? C19 Fe C2 101.40(13) . . ? C5 Fe C2 67.19(12) . . ? C1 Fe C2 40.68(11) . . ? C3 Fe C2 39.18(11) . . ? C4 Fe C2 66.94(11) . . ? C18 Fe I 92.43(11) . . ? C19 Fe I 88.05(12) . . ? C5 Fe I 147.65(9) . . ? C1 Fe I 146.30(8) . . ? C3 Fe I 89.02(10) . . ? C4 Fe I 107.96(9) . . ? C2 Fe I 105.90(9) . . ? C5 C1 C2 106.2(2) . . ? C5 C1 C6 119.2(3) . . ? C2 C1 C6 133.8(3) . . ? C5 C1 Fe 68.67(18) . . ? C2 C1 Fe 71.23(18) . . ? C6 C1 Fe 132.1(2) . . ? C3 C2 C1 106.1(3) . . ? C3 C2 C10 120.0(3) . . ? C1 C2 C10 133.6(3) . . ? C3 C2 Fe 70.24(18) . . ? C1 C2 Fe 68.09(16) . . ? C10 C2 Fe 131.0(2) . . ? C4 C3 C2 111.3(3) . . ? C4 C3 Fe 70.54(17) . . ? C2 C3 Fe 70.58(17) . . ? C3 C4 C5 105.6(3) . . ? C3 C4 C14 126.4(3) . . ? C5 C4 C14 127.4(3) . . ? C3 C4 Fe 70.53(19) . . ? C5 C4 Fe 67.53(18) . . ? C14 C4 Fe 132.9(2) . . ? C4 C5 C1 110.8(3) . . ? C4 C5 Fe 72.8(2) . . ? C1 C5 Fe 70.95(19) . . ? C9 C6 C7 108.4(3) . . ? C9 C6 C8 109.0(3) . . ? C7 C6 C8 106.5(2) . . ? C9 C6 C1 105.9(2) . . ? C7 C6 C1 110.1(2) . . ? C8 C6 C1 116.7(3) . . ? C13 C10 C2 109.9(3) . . ? C13 C10 C11 106.6(3) . . ? C2 C10 C11 110.2(3) . . ? C13 C10 C12 106.2(3) . . ? C2 C10 C12 112.9(3) . . ? C11 C10 C12 110.9(3) . . ? C4 C14 C17 110.5(3) . . ? C4 C14 C15 112.3(2) . . ? C17 C14 C15 108.4(3) . . ? C4 C14 C16 107.2(3) . . ? C17 C14 C16 109.7(3) . . ? C15 C14 C16 108.6(3) . . ? O1 C18 Fe 176.0(3) . . ? O2 C19 Fe 176.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C18 Fe C1 C5 48.5(2) . . . . ? C19 Fe C1 C5 140.91(18) . . . . ? C3 Fe C1 C5 -79.09(18) . . . . ? C4 Fe C1 C5 -36.71(16) . . . . ? C2 Fe C1 C5 -116.7(2) . . . . ? I Fe C1 C5 -125.96(17) . . . . ? C18 Fe C1 C2 165.24(17) . . . . ? C19 Fe C1 C2 -102.36(19) . . . . ? C5 Fe C1 C2 116.7(2) . . . . ? C3 Fe C1 C2 37.65(17) . . . . ? C4 Fe C1 C2 80.03(18) . . . . ? I Fe C1 C2 -9.2(3) . . . . ? C18 Fe C1 C6 -62.1(3) . . . . ? C19 Fe C1 C6 30.3(3) . . . . ? C5 Fe C1 C6 -110.6(3) . . . . ? C3 Fe C1 C6 170.3(3) . . . . ? C4 Fe C1 C6 -147.3(3) . . . . ? C2 Fe C1 C6 132.7(4) . . . . ? I Fe C1 C6 123.4(2) . . . . ? C5 C1 C2 C3 -0.3(3) . . . . ? C6 C1 C2 C3 168.7(3) . . . . ? Fe C1 C2 C3 -60.3(2) . . . . ? C5 C1 C2 C10 -173.5(3) . . . . ? C6 C1 C2 C10 -4.5(6) . . . . ? Fe C1 C2 C10 126.4(4) . . . . ? C5 C1 C2 Fe 60.1(2) . . . . ? C6 C1 C2 Fe -130.9(4) . . . . ? C18 Fe C2 C3 80.6(4) . . . . ? C19 Fe C2 C3 -159.0(2) . . . . ? C5 Fe C2 C3 78.6(2) . . . . ? C1 Fe C2 C3 117.5(3) . . . . ? C4 Fe C2 C3 35.32(19) . . . . ? I Fe C2 C3 -67.8(2) . . . . ? C18 Fe C2 C1 -36.9(4) . . . . ? C19 Fe C2 C1 83.5(2) . . . . ? C5 Fe C2 C1 -38.88(17) . . . . ? C3 Fe C2 C1 -117.5(3) . . . . ? C4 Fe C2 C1 -82.18(19) . . . . ? I Fe C2 C1 174.69(15) . . . . ? C18 Fe C2 C10 -166.4(3) . . . . ? C19 Fe C2 C10 -46.0(3) . . . . ? C5 Fe C2 C10 -168.3(3) . . . . ? C1 Fe C2 C10 -129.5(4) . . . . ? C3 Fe C2 C10 113.0(4) . . . . ? C4 Fe C2 C10 148.4(3) . . . . ? I Fe C2 C10 45.2(3) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? C10 C2 C3 C4 174.4(3) . . . . ? Fe C2 C3 C4 -58.9(2) . . . . ? C1 C2 C3 Fe 58.9(2) . . . . ? C10 C2 C3 Fe -126.7(3) . . . . ? C18 Fe C3 C4 -28.4(3) . . . . ? C19 Fe C3 C4 153.1(2) . . . . ? C5 Fe C3 C4 38.72(19) . . . . ? C1 Fe C3 C4 83.1(2) . . . . ? C2 Fe C3 C4 122.2(3) . . . . ? I Fe C3 C4 -120.79(19) . . . . ? C18 Fe C3 C2 -150.5(2) . . . . ? C19 Fe C3 C2 31.0(3) . . . . ? C5 Fe C3 C2 -83.4(2) . . . . ? C1 Fe C3 C2 -39.07(19) . . . . ? C4 Fe C3 C2 -122.2(3) . . . . ? I Fe C3 C2 117.04(18) . . . . ? C2 C3 C4 C5 0.3(4) . . . . ? Fe C3 C4 C5 -58.7(2) . . . . ? C2 C3 C4 C14 -171.5(3) . . . . ? Fe C3 C4 C14 129.5(4) . . . . ? C2 C3 C4 Fe 58.9(2) . . . . ? C18 Fe C4 C3 159.6(2) . . . . ? C19 Fe C4 C3 -87.5(5) . . . . ? C5 Fe C4 C3 -117.1(3) . . . . ? C1 Fe C4 C3 -79.8(2) . . . . ? C2 Fe C4 C3 -35.53(19) . . . . ? I Fe C4 C3 64.5(2) . . . . ? C18 Fe C4 C5 -83.4(2) . . . . ? C19 Fe C4 C5 29.6(5) . . . . ? C1 Fe C4 C5 37.30(17) . . . . ? C3 Fe C4 C5 117.1(3) . . . . ? C2 Fe C4 C5 81.54(19) . . . . ? I Fe C4 C5 -178.38(15) . . . . ? C18 Fe C4 C14 37.5(3) . . . . ? C19 Fe C4 C14 150.5(4) . . . . ? C5 Fe C4 C14 120.9(3) . . . . ? C1 Fe C4 C14 158.2(3) . . . . ? C3 Fe C4 C14 -122.0(4) . . . . ? C2 Fe C4 C14 -157.6(3) . . . . ? I Fe C4 C14 -57.5(3) . . . . ? C3 C4 C5 C1 -0.4(4) . . . . ? C14 C4 C5 C1 171.2(3) . . . . ? Fe C4 C5 C1 -61.1(2) . . . . ? C3 C4 C5 Fe 60.6(2) . . . . ? C14 C4 C5 Fe -127.7(3) . . . . ? C2 C1 C5 C4 0.4(4) . . . . ? C6 C1 C5 C4 -170.5(3) . . . . ? Fe C1 C5 C4 62.2(2) . . . . ? C2 C1 C5 Fe -61.7(2) . . . . ? C6 C1 C5 Fe 127.3(3) . . . . ? C18 Fe C5 C4 99.85(18) . . . . ? C19 Fe C5 C4 -169.41(18) . . . . ? C1 Fe C5 C4 -120.0(2) . . . . ? C3 Fe C5 C4 -37.96(16) . . . . ? C2 Fe C5 C4 -80.87(18) . . . . ? I Fe C5 C4 2.9(3) . . . . ? C18 Fe C5 C1 -140.11(18) . . . . ? C19 Fe C5 C1 -49.4(2) . . . . ? C3 Fe C5 C1 82.07(17) . . . . ? C4 Fe C5 C1 120.0(2) . . . . ? C2 Fe C5 C1 39.16(16) . . . . ? I Fe C5 C1 122.92(17) . . . . ? C5 C1 C6 C9 83.3(3) . . . . ? C2 C1 C6 C9 -84.6(4) . . . . ? Fe C1 C6 C9 170.0(2) . . . . ? C5 C1 C6 C7 -33.8(4) . . . . ? C2 C1 C6 C7 158.3(3) . . . . ? Fe C1 C6 C7 52.9(4) . . . . ? C5 C1 C6 C8 -155.3(3) . . . . ? C2 C1 C6 C8 36.8(5) . . . . ? Fe C1 C6 C8 -68.5(4) . . . . ? C3 C2 C10 C13 0.3(5) . . . . ? C1 C2 C10 C13 172.8(4) . . . . ? Fe C2 C10 C13 -88.8(4) . . . . ? C3 C2 C10 C11 -116.8(3) . . . . ? C1 C2 C10 C11 55.7(5) . . . . ? Fe C2 C10 C11 154.1(2) . . . . ? C3 C2 C10 C12 118.6(3) . . . . ? C1 C2 C10 C12 -68.9(5) . . . . ? Fe C2 C10 C12 29.5(4) . . . . ? C3 C4 C14 C17 -16.6(5) . . . . ? C5 C4 C14 C17 173.4(3) . . . . ? Fe C4 C14 C17 80.3(4) . . . . ? C3 C4 C14 C15 -137.8(4) . . . . ? C5 C4 C14 C15 52.2(5) . . . . ? Fe C4 C14 C15 -41.0(4) . . . . ? C3 C4 C14 C16 102.9(4) . . . . ? C5 C4 C14 C16 -67.1(4) . . . . ? Fe C4 C14 C16 -160.2(3) . . . . ? C19 Fe C18 O1 -63(4) . . . . ? C5 Fe C18 O1 61(4) . . . . ? C1 Fe C18 O1 32(4) . . . . ? C3 Fe C18 O1 118(4) . . . . ? C4 Fe C18 O1 100(4) . . . . ? C2 Fe C18 O1 59(4) . . . . ? I Fe C18 O1 -151(4) . . . . ? C18 Fe C19 O2 15(5) . . . . ? C5 Fe C19 O2 -77(5) . . . . ? C1 Fe C19 O2 -106(5) . . . . ? C3 Fe C19 O2 -166(5) . . . . ? C4 Fe C19 O2 -99(5) . . . . ? C2 Fe C19 O2 -147(5) . . . . ? I Fe C19 O2 107(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 75.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.978 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.081 _iucr_refine_instruction_details ; TITL mima52 in Pca2(1) CELL 1.54184 15.353380 10.454840 12.347088 90.0000 90.0000 90.0000 ZERR 4.00 0.000300 0.000200 0.000300 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z+1/2 SYMM x+1/2,-y, z SYMM -x+1/2, y, z+1/2 SFAC C H O Fe I UNIT 76.00 116.00 8.00 4.00 4.00 OMIT 8 4 -12 TEMP -173 SIZE 0.12 0.03 0.015 ACTA 150 CONF MERG 2 FMAP 2 PLAN 10 L.S. 4 WGHT 0.047900 0.403900 FVAR 2.10278 FE 4 0.443500 0.656440 0.806925 11.00000 0.01199 0.00932 = 0.01333 0.00069 -0.00158 0.00039 I 5 0.372845 0.633487 0.998720 11.00000 0.02586 0.02383 = 0.01400 0.00297 0.00237 0.00437 O1 3 0.581364 0.471223 0.852217 11.00000 0.01648 0.01815 = 0.03585 0.00227 -0.00796 0.00408 O2 3 0.558310 0.853706 0.896183 11.00000 0.03362 0.01740 = 0.03248 -0.00028 -0.01520 -0.00654 C1 1 0.434767 0.740441 0.653141 11.00000 0.01045 0.01333 = 0.01288 0.00218 -0.00135 -0.00058 C2 1 0.353376 0.765653 0.712539 11.00000 0.00973 0.01246 = 0.01210 0.00137 -0.00187 0.00082 C3 1 0.316735 0.642903 0.736812 11.00000 0.00773 0.01456 = 0.01958 -0.00148 -0.00296 -0.00039 AFIX 43 H3 2 0.263695 0.630300 0.774971 11.00000 -1.20000 AFIX 0 C4 1 0.370038 0.542322 0.696390 11.00000 0.00977 0.01111 = 0.01235 0.00014 -0.00284 0.00099 C5 1 0.442453 0.603754 0.645677 11.00000 0.01256 0.01259 = 0.01537 -0.00050 -0.00142 0.00116 AFIX 43 H5 2 0.489332 0.560151 0.611636 11.00000 -1.20000 AFIX 0 C6 1 0.498182 0.825215 0.588424 11.00000 0.01219 0.01115 = 0.01767 0.00059 -0.00022 -0.00134 C7 1 0.588065 0.760502 0.581267 11.00000 0.01256 0.01754 = 0.03248 0.00409 0.00385 0.00019 AFIX 137 H7A 2 0.583001 0.680550 0.540317 11.00000 -1.50000 H7B 2 0.609379 0.741967 0.654418 11.00000 -1.50000 H7C 2 0.629034 0.817795 0.544512 11.00000 -1.50000 AFIX 0 C8 1 0.514032 0.961129 0.632204 11.00000 0.01831 0.01184 = 0.02385 0.00228 -0.00057 -0.00516 AFIX 137 H8A 2 0.554813 1.006155 0.584511 11.00000 -1.50000 H8B 2 0.538663 0.955952 0.705296 11.00000 -1.50000 H8C 2 0.458708 1.007790 0.634671 11.00000 -1.50000 AFIX 0 C9 1 0.460168 0.834543 0.473785 11.00000 0.02027 0.01742 = 0.01742 0.00113 0.00302 -0.00255 AFIX 137 H9A 2 0.404444 0.880159 0.476341 11.00000 -1.50000 H9B 2 0.450956 0.748334 0.444803 11.00000 -1.50000 H9C 2 0.500821 0.881094 0.426981 11.00000 -1.50000 AFIX 0 C10 1 0.302242 0.888160 0.739526 11.00000 0.01388 0.01324 = 0.02050 -0.00204 0.00149 0.00487 C11 1 0.280596 0.962009 0.634804 11.00000 0.01889 0.01595 = 0.01986 0.00277 -0.00139 0.00395 AFIX 137 H11A 2 0.239156 1.030629 0.651188 11.00000 -1.50000 H11B 2 0.254799 0.903366 0.581842 11.00000 -1.50000 H11C 2 0.334078 0.998961 0.604838 11.00000 -1.50000 AFIX 0 C12 1 0.350023 0.975015 0.821301 11.00000 0.02321 0.01332 = 0.02184 -0.00374 -0.00078 0.00163 AFIX 137 H12A 2 0.406638 1.000145 0.791456 11.00000 -1.50000 H12B 2 0.358808 0.928413 0.889296 11.00000 -1.50000 H12C 2 0.314960 1.051636 0.835073 11.00000 -1.50000 AFIX 0 C13 1 0.214825 0.853260 0.792083 11.00000 0.01886 0.01929 = 0.03068 0.00032 0.00735 0.00403 AFIX 137 H13A 2 0.183980 0.931649 0.812648 11.00000 -1.50000 H13B 2 0.225289 0.801117 0.856744 11.00000 -1.50000 H13C 2 0.179388 0.804731 0.740415 11.00000 -1.50000 AFIX 0 C14 1 0.347067 0.401050 0.693526 11.00000 0.01267 0.00918 = 0.02003 0.00064 0.00024 -0.00202 C15 1 0.423636 0.316081 0.726698 11.00000 0.02200 0.00979 = 0.04571 0.00432 -0.00773 -0.00072 AFIX 137 H15A 2 0.409463 0.226466 0.711494 11.00000 -1.50000 H15B 2 0.434951 0.326540 0.804308 11.00000 -1.50000 H15C 2 0.475559 0.340791 0.685548 11.00000 -1.50000 AFIX 0 C16 1 0.321699 0.368554 0.576536 11.00000 0.03693 0.01681 = 0.02391 -0.00214 -0.00118 -0.00553 AFIX 137 H16A 2 0.274568 0.425292 0.552939 11.00000 -1.50000 H16B 2 0.302020 0.279494 0.572771 11.00000 -1.50000 H16C 2 0.372306 0.380116 0.529166 11.00000 -1.50000 AFIX 0 C17 1 0.270707 0.373077 0.768979 11.00000 0.02979 0.01749 = 0.03461 -0.00363 0.01477 -0.01031 AFIX 137 H17A 2 0.218764 0.418085 0.742990 11.00000 -1.50000 H17B 2 0.284893 0.402350 0.842288 11.00000 -1.50000 H17C 2 0.259419 0.280828 0.770123 11.00000 -1.50000 AFIX 0 C18 1 0.525258 0.541812 0.836936 11.00000 0.01916 0.01501 = 0.01925 -0.00273 -0.00181 -0.00648 C19 1 0.510924 0.778930 0.861265 11.00000 0.02388 0.01902 = 0.01614 0.00488 -0.00456 0.00278 HKLF 4 ; # Attachment '- mima53.cif' data_mima53 _database_code_depnum_ccdc_archive 'CCDC 884313' #TrackingRef '- mima53.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H23 Fe I O2' _chemical_formula_weight 466.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' Fe Fe -1.1336 3.1974 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.49836(10) _cell_length_b 13.6127(2) _cell_length_c 16.3850(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1895.50(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 51952 _cell_measurement_theta_min 3.2438 _cell_measurement_theta_max 75.5866 _exptl_crystal_description prism _exptl_crystal_colour 'yellow-dark brown dichroic' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 19.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.00388 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58426 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.22 _diffrn_reflns_theta_max 75.77 _reflns_number_total 3948 _reflns_number_gt 3943 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _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. ; _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^)+(0.0301P)^2^+1.5467P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(4) _refine_ls_number_reflns 3948 _refine_ls_number_parameters 214 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0193 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0501 _refine_ls_wR_factor_gt 0.0501 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.080 _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 Fe Fe 0.25394(4) 0.54014(3) 0.76199(2) 0.00702(8) Uani 1 1 d . . . I I 0.021617(17) 0.543791(11) 0.865554(8) 0.01396(5) Uani 1 1 d . . . O1 O 0.3993(2) 0.38109(14) 0.85138(11) 0.0201(4) Uani 1 1 d . . . O2 O 0.0808(2) 0.39816(13) 0.66154(11) 0.0169(4) Uani 1 1 d . . . C1 C 0.3962(3) 0.65984(19) 0.79981(15) 0.0133(5) Uani 1 1 d . . . C2 C 0.2560(3) 0.69543(17) 0.76192(15) 0.0114(5) Uani 1 1 d . . . H2 H 0.1813 0.7366 0.7882 0.014 Uiso 1 1 calc R . . C3 C 0.2417(3) 0.66165(16) 0.68001(14) 0.0089(4) Uani 1 1 d U . . C4 C 0.3858(3) 0.60567(17) 0.66377(14) 0.0085(4) Uani 1 1 d U . . C5 C 0.4787(3) 0.60506(17) 0.73715(14) 0.0115(4) Uani 1 1 d . . . C6 C 0.6284(3) 0.5560(2) 0.73696(16) 0.0171(5) Uani 1 1 d . . . H6 H 0.6908 0.5541 0.7850 0.020 Uiso 1 1 calc R . . C7 C 0.6793(3) 0.5126(2) 0.66780(19) 0.0200(6) Uani 1 1 d . . . H7 H 0.7778 0.4796 0.6679 0.024 Uiso 1 1 calc R . . C8 C 0.5887(3) 0.51510(19) 0.59442(16) 0.0172(5) Uani 1 1 d . . . H8 H 0.6298 0.4854 0.5465 0.021 Uiso 1 1 calc R . . C9 C 0.4453(3) 0.55885(18) 0.59151(14) 0.0130(5) Uani 1 1 d . . . H9 H 0.3854 0.5585 0.5426 0.016 Uiso 1 1 calc R . . C10 C 0.4580(4) 0.69341(19) 0.88220(14) 0.0178(5) Uani 1 1 d . . . C11 C 0.5995(4) 0.7627(2) 0.86446(18) 0.0234(6) Uani 1 1 d . . . H11A H 0.5656 0.8157 0.8280 0.035 Uiso 1 1 calc R . . H11B H 0.6842 0.7252 0.8384 0.035 Uiso 1 1 calc R . . H11C H 0.6379 0.7908 0.9158 0.035 Uiso 1 1 calc R . . C12 C 0.3327(4) 0.7510(2) 0.92866(16) 0.0255(7) Uani 1 1 d . . . H12A H 0.2398 0.7095 0.9368 0.038 Uiso 1 1 calc R . . H12B H 0.3032 0.8094 0.8972 0.038 Uiso 1 1 calc R . . H12C H 0.3745 0.7712 0.9818 0.038 Uiso 1 1 calc R . . C13 C 0.5129(4) 0.6074(2) 0.93603(16) 0.0286(7) Uani 1 1 d . . . H13A H 0.5961 0.5710 0.9078 0.043 Uiso 1 1 calc R . . H13B H 0.4239 0.5635 0.9468 0.043 Uiso 1 1 calc R . . H13C H 0.5537 0.6330 0.9878 0.043 Uiso 1 1 calc R . . C14 C 0.1205(3) 0.69670(18) 0.61867(14) 0.0121(5) Uani 1 1 d . . . C15 C 0.2044(4) 0.7722(2) 0.56368(17) 0.0213(6) Uani 1 1 d . . . H15A H 0.2910 0.7400 0.5347 0.032 Uiso 1 1 calc R . . H15B H 0.2462 0.8256 0.5974 0.032 Uiso 1 1 calc R . . H15C H 0.1294 0.7989 0.5241 0.032 Uiso 1 1 calc R . . C16 C 0.0540(3) 0.6137(2) 0.56481(16) 0.0182(5) Uani 1 1 d . . . H16A H -0.0082 0.5687 0.5985 0.027 Uiso 1 1 calc R . . H16B H 0.1410 0.5777 0.5395 0.027 Uiso 1 1 calc R . . H16C H -0.0130 0.6420 0.5222 0.027 Uiso 1 1 calc R . . C17 C -0.0175(4) 0.7457(2) 0.66240(16) 0.0205(5) Uani 1 1 d . . . H17A H 0.0180 0.8071 0.6876 0.031 Uiso 1 1 calc R . . H17B H -0.0580 0.7015 0.7047 0.031 Uiso 1 1 calc R . . H17C H -0.1011 0.7599 0.6229 0.031 Uiso 1 1 calc R . . C18 C 0.3441(3) 0.4426(2) 0.81936(15) 0.0151(5) Uani 1 1 d . . . C19 C 0.1475(3) 0.45527(19) 0.70013(13) 0.0107(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.00899(16) 0.00871(16) 0.00335(14) 0.00128(14) -0.00056(12) -0.00149(15) I 0.01371(8) 0.01846(8) 0.00971(7) 0.00076(6) 0.00375(5) -0.00226(6) O1 0.0269(10) 0.0189(9) 0.0144(9) 0.0064(8) -0.0063(8) -0.0048(8) O2 0.0215(10) 0.0148(8) 0.0144(8) -0.0028(7) -0.0046(7) -0.0021(7) C1 0.0167(13) 0.0151(11) 0.0081(11) 0.0025(9) 0.0002(9) -0.0082(10) C2 0.0184(12) 0.0076(10) 0.0082(10) 0.0004(8) 0.0029(9) -0.0018(9) C3 0.0130(10) 0.0077(9) 0.0060(9) 0.0022(7) 0.0023(8) -0.0007(8) C4 0.0098(8) 0.0097(8) 0.0058(7) 0.0018(6) 0.0020(6) -0.0023(7) C5 0.0119(11) 0.0148(10) 0.0078(10) 0.0024(8) -0.0015(9) -0.0065(9) C6 0.0099(11) 0.0255(13) 0.0157(11) 0.0050(11) -0.0040(9) -0.0052(11) C7 0.0081(12) 0.0267(14) 0.0251(14) 0.0056(11) 0.0042(10) 0.0011(10) C8 0.0184(13) 0.0204(13) 0.0129(12) 0.0002(10) 0.0064(10) -0.0003(10) C9 0.0178(13) 0.0136(11) 0.0077(10) 0.0007(9) 0.0041(9) -0.0011(9) C10 0.0259(14) 0.0212(12) 0.0062(10) 0.0010(9) -0.0028(10) -0.0113(11) C11 0.0292(15) 0.0256(14) 0.0153(12) 0.0008(12) -0.0052(12) -0.0164(11) C12 0.0392(18) 0.0279(15) 0.0094(11) -0.0096(11) 0.0036(11) -0.0170(13) C13 0.046(2) 0.0288(14) 0.0108(12) 0.0061(10) -0.0140(13) -0.0149(15) C14 0.0161(12) 0.0131(11) 0.0072(11) 0.0037(9) 0.0010(9) 0.0017(9) C15 0.0274(15) 0.0191(13) 0.0175(13) 0.0129(11) 0.0011(11) 0.0015(11) C16 0.0209(14) 0.0195(12) 0.0142(12) 0.0002(10) -0.0073(10) 0.0025(11) C17 0.0210(14) 0.0220(12) 0.0184(12) 0.0020(10) 0.0013(11) 0.0097(11) C18 0.0110(11) 0.0229(14) 0.0112(11) -0.0048(10) -0.0011(9) -0.0082(11) C19 0.0119(11) 0.0124(10) 0.0077(9) 0.0048(10) 0.0038(8) 0.0037(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 Fe C19 1.783(3) . ? Fe C18 1.799(3) . ? Fe C2 2.114(2) . ? Fe C1 2.122(3) . ? Fe C3 2.133(2) . ? Fe C5 2.143(3) . ? Fe C4 2.154(2) . ? Fe I 2.6039(4) . ? O1 C18 1.093(3) . ? O2 C19 1.151(3) . ? C1 C2 1.429(4) . ? C1 C5 1.450(4) . ? C1 C10 1.519(3) . ? C2 C3 1.424(3) . ? C3 C4 1.467(3) . ? C3 C14 1.516(3) . ? C4 C9 1.437(3) . ? C4 C5 1.438(3) . ? C5 C6 1.437(4) . ? C6 C7 1.349(4) . ? C7 C8 1.428(4) . ? C8 C9 1.357(4) . ? C10 C12 1.526(4) . ? C10 C13 1.538(4) . ? C10 C11 1.556(4) . ? C14 C17 1.528(4) . ? C14 C16 1.541(3) . ? C14 C15 1.541(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 Fe C18 92.00(11) . . ? C19 Fe C2 130.66(10) . . ? C18 Fe C2 137.32(11) . . ? C19 Fe C1 162.30(10) . . ? C18 Fe C1 99.88(10) . . ? C2 Fe C1 39.42(10) . . ? C19 Fe C3 96.88(10) . . ? C18 Fe C3 157.28(11) . . ? C2 Fe C3 39.17(9) . . ? C1 Fe C3 67.43(9) . . ? C19 Fe C5 127.68(10) . . ? C18 Fe C5 91.37(10) . . ? C2 Fe C5 65.19(10) . . ? C1 Fe C5 39.74(9) . . ? C3 Fe C5 66.69(9) . . ? C19 Fe C4 96.18(9) . . ? C18 Fe C4 118.33(11) . . ? C2 Fe C4 65.25(9) . . ? C1 Fe C4 66.66(9) . . ? C3 Fe C4 40.00(9) . . ? C5 Fe C4 39.11(9) . . ? C19 Fe I 89.89(7) . . ? C18 Fe I 89.80(8) . . ? C2 Fe I 89.28(7) . . ? C1 Fe I 103.13(7) . . ? C3 Fe I 111.01(7) . . ? C5 Fe I 142.33(6) . . ? C4 Fe I 150.84(7) . . ? C2 C1 C5 105.7(2) . . ? C2 C1 C10 124.9(2) . . ? C5 C1 C10 128.1(2) . . ? C2 C1 Fe 70.00(14) . . ? C5 C1 Fe 70.94(14) . . ? C10 C1 Fe 133.45(17) . . ? C3 C2 C1 111.8(2) . . ? C3 C2 Fe 71.15(13) . . ? C1 C2 Fe 70.58(14) . . ? C2 C3 C4 105.5(2) . . ? C2 C3 C14 125.5(2) . . ? C4 C3 C14 127.6(2) . . ? C2 C3 Fe 69.68(13) . . ? C4 C3 Fe 70.76(13) . . ? C14 C3 Fe 133.99(17) . . ? C9 C4 C5 119.5(2) . . ? C9 C4 C3 132.4(2) . . ? C5 C4 C3 108.0(2) . . ? C9 C4 Fe 127.96(17) . . ? C5 C4 Fe 70.05(13) . . ? C3 C4 Fe 69.23(12) . . ? C6 C5 C4 119.1(2) . . ? C6 C5 C1 132.0(2) . . ? C4 C5 C1 108.9(2) . . ? C6 C5 Fe 126.71(17) . . ? C4 C5 Fe 70.85(13) . . ? C1 C5 Fe 69.32(14) . . ? C7 C6 C5 119.3(2) . . ? C6 C7 C8 121.6(2) . . ? C9 C8 C7 121.6(2) . . ? C8 C9 C4 118.8(2) . . ? C1 C10 C12 110.9(2) . . ? C1 C10 C13 112.7(2) . . ? C12 C10 C13 108.5(2) . . ? C1 C10 C11 106.5(2) . . ? C12 C10 C11 108.7(2) . . ? C13 C10 C11 109.5(3) . . ? C3 C14 C17 110.4(2) . . ? C3 C14 C16 113.4(2) . . ? C17 C14 C16 107.9(2) . . ? C3 C14 C15 106.4(2) . . ? C17 C14 C15 109.8(2) . . ? C16 C14 C15 108.9(2) . . ? O1 C18 Fe 177.1(2) . . ? O2 C19 Fe 177.9(2) . . ? 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 C19 Fe C1 C2 64.1(4) . . . . ? C18 Fe C1 C2 -164.43(15) . . . . ? C3 Fe C1 C2 35.26(14) . . . . ? C5 Fe C1 C2 115.4(2) . . . . ? C4 Fe C1 C2 78.86(15) . . . . ? I Fe C1 C2 -72.31(14) . . . . ? C19 Fe C1 C5 -51.3(4) . . . . ? C18 Fe C1 C5 80.13(15) . . . . ? C2 Fe C1 C5 -115.4(2) . . . . ? C3 Fe C1 C5 -80.19(14) . . . . ? C4 Fe C1 C5 -36.59(13) . . . . ? I Fe C1 C5 172.25(12) . . . . ? C19 Fe C1 C10 -176.3(3) . . . . ? C18 Fe C1 C10 -44.8(3) . . . . ? C2 Fe C1 C10 119.7(3) . . . . ? C3 Fe C1 C10 154.9(3) . . . . ? C5 Fe C1 C10 -124.9(3) . . . . ? C4 Fe C1 C10 -161.5(3) . . . . ? I Fe C1 C10 47.3(3) . . . . ? C5 C1 C2 C3 3.1(3) . . . . ? C10 C1 C2 C3 171.0(2) . . . . ? Fe C1 C2 C3 -59.34(17) . . . . ? C5 C1 C2 Fe 62.43(16) . . . . ? C10 C1 C2 Fe -129.7(2) . . . . ? C19 Fe C2 C3 -36.4(2) . . . . ? C18 Fe C2 C3 145.41(17) . . . . ? C1 Fe C2 C3 122.4(2) . . . . ? C5 Fe C2 C3 82.95(15) . . . . ? C4 Fe C2 C3 39.69(14) . . . . ? I Fe C2 C3 -125.66(14) . . . . ? C19 Fe C2 C1 -158.87(15) . . . . ? C18 Fe C2 C1 23.0(2) . . . . ? C3 Fe C2 C1 -122.4(2) . . . . ? C5 Fe C2 C1 -39.49(14) . . . . ? C4 Fe C2 C1 -82.75(15) . . . . ? I Fe C2 C1 111.89(14) . . . . ? C1 C2 C3 C4 -3.1(3) . . . . ? Fe C2 C3 C4 -62.13(15) . . . . ? C1 C2 C3 C14 -170.8(2) . . . . ? Fe C2 C3 C14 130.2(2) . . . . ? C1 C2 C3 Fe 59.00(17) . . . . ? C19 Fe C3 C2 153.02(16) . . . . ? C18 Fe C3 C2 -94.7(3) . . . . ? C1 Fe C3 C2 -35.47(15) . . . . ? C5 Fe C3 C2 -78.78(15) . . . . ? C4 Fe C3 C2 -115.6(2) . . . . ? I Fe C3 C2 60.49(15) . . . . ? C19 Fe C3 C4 -91.43(14) . . . . ? C18 Fe C3 C4 20.8(3) . . . . ? C2 Fe C3 C4 115.6(2) . . . . ? C1 Fe C3 C4 80.08(15) . . . . ? C5 Fe C3 C4 36.78(13) . . . . ? I Fe C3 C4 176.04(11) . . . . ? C19 Fe C3 C14 32.8(2) . . . . ? C18 Fe C3 C14 145.0(3) . . . . ? C2 Fe C3 C14 -120.3(3) . . . . ? C1 Fe C3 C14 -155.7(3) . . . . ? C5 Fe C3 C14 161.0(3) . . . . ? C4 Fe C3 C14 124.2(3) . . . . ? I Fe C3 C14 -59.8(2) . . . . ? C2 C3 C4 C9 -175.6(2) . . . . ? C14 C3 C4 C9 -8.3(4) . . . . ? Fe C3 C4 C9 123.0(3) . . . . ? C2 C3 C4 C5 1.9(2) . . . . ? C14 C3 C4 C5 169.2(2) . . . . ? Fe C3 C4 C5 -59.51(16) . . . . ? C2 C3 C4 Fe 61.41(15) . . . . ? C14 C3 C4 Fe -131.3(2) . . . . ? C19 Fe C4 C9 -34.9(2) . . . . ? C18 Fe C4 C9 60.8(3) . . . . ? C2 Fe C4 C9 -167.1(3) . . . . ? C1 Fe C4 C9 149.6(3) . . . . ? C3 Fe C4 C9 -128.2(3) . . . . ? C5 Fe C4 C9 112.5(3) . . . . ? I Fe C4 C9 -135.80(18) . . . . ? C19 Fe C4 C5 -147.31(15) . . . . ? C18 Fe C4 C5 -51.68(17) . . . . ? C2 Fe C4 C5 80.48(15) . . . . ? C1 Fe C4 C5 37.16(14) . . . . ? C3 Fe C4 C5 119.34(19) . . . . ? I Fe C4 C5 111.75(16) . . . . ? C19 Fe C4 C3 93.35(15) . . . . ? C18 Fe C4 C3 -171.02(14) . . . . ? C2 Fe C4 C3 -38.86(13) . . . . ? C1 Fe C4 C3 -82.19(15) . . . . ? C5 Fe C4 C3 -119.34(19) . . . . ? I Fe C4 C3 -7.6(2) . . . . ? C9 C4 C5 C6 -1.1(3) . . . . ? C3 C4 C5 C6 -178.9(2) . . . . ? Fe C4 C5 C6 122.1(2) . . . . ? C9 C4 C5 C1 177.8(2) . . . . ? C3 C4 C5 C1 -0.1(3) . . . . ? Fe C4 C5 C1 -59.08(16) . . . . ? C9 C4 C5 Fe -123.1(2) . . . . ? C3 C4 C5 Fe 59.00(15) . . . . ? C2 C1 C5 C6 176.9(2) . . . . ? C10 C1 C5 C6 9.5(4) . . . . ? Fe C1 C5 C6 -121.3(3) . . . . ? C2 C1 C5 C4 -1.8(3) . . . . ? C10 C1 C5 C4 -169.2(2) . . . . ? Fe C1 C5 C4 60.02(16) . . . . ? C2 C1 C5 Fe -61.79(16) . . . . ? C10 C1 C5 Fe 130.8(3) . . . . ? C19 Fe C5 C6 -69.9(2) . . . . ? C18 Fe C5 C6 23.7(2) . . . . ? C2 Fe C5 C6 166.8(2) . . . . ? C1 Fe C5 C6 127.6(3) . . . . ? C3 Fe C5 C6 -150.2(2) . . . . ? C4 Fe C5 C6 -112.6(3) . . . . ? I Fe C5 C6 115.2(2) . . . . ? C19 Fe C5 C4 42.72(18) . . . . ? C18 Fe C5 C4 136.31(15) . . . . ? C2 Fe C5 C4 -80.64(15) . . . . ? C1 Fe C5 C4 -119.8(2) . . . . ? C3 Fe C5 C4 -37.60(13) . . . . ? I Fe C5 C4 -132.23(12) . . . . ? C19 Fe C5 C1 162.55(15) . . . . ? C18 Fe C5 C1 -103.87(15) . . . . ? C2 Fe C5 C1 39.18(14) . . . . ? C3 Fe C5 C1 82.22(15) . . . . ? C4 Fe C5 C1 119.8(2) . . . . ? I Fe C5 C1 -12.41(19) . . . . ? C4 C5 C6 C7 0.8(4) . . . . ? C1 C5 C6 C7 -177.8(3) . . . . ? Fe C5 C6 C7 87.7(3) . . . . ? C5 C6 C7 C8 0.6(4) . . . . ? C6 C7 C8 C9 -1.8(4) . . . . ? C7 C8 C9 C4 1.5(4) . . . . ? C5 C4 C9 C8 -0.1(3) . . . . ? C3 C4 C9 C8 177.2(2) . . . . ? Fe C4 C9 C8 -86.9(3) . . . . ? C2 C1 C10 C12 13.7(3) . . . . ? C5 C1 C10 C12 178.8(2) . . . . ? Fe C1 C10 C12 -81.3(3) . . . . ? C2 C1 C10 C13 135.5(3) . . . . ? C5 C1 C10 C13 -59.4(4) . . . . ? Fe C1 C10 C13 40.5(4) . . . . ? C2 C1 C10 C11 -104.4(3) . . . . ? C5 C1 C10 C11 60.7(3) . . . . ? Fe C1 C10 C11 160.6(2) . . . . ? C2 C3 C14 C17 -19.3(3) . . . . ? C4 C3 C14 C17 175.7(2) . . . . ? Fe C3 C14 C17 76.2(3) . . . . ? C2 C3 C14 C16 -140.6(2) . . . . ? C4 C3 C14 C16 54.5(3) . . . . ? Fe C3 C14 C16 -45.0(3) . . . . ? C2 C3 C14 C15 99.7(3) . . . . ? C4 C3 C14 C15 -65.2(3) . . . . ? Fe C3 C14 C15 -164.74(19) . . . . ? C19 Fe C18 O1 37(5) . . . . ? C2 Fe C18 O1 -144(5) . . . . ? C1 Fe C18 O1 -130(5) . . . . ? C3 Fe C18 O1 -76(5) . . . . ? C5 Fe C18 O1 -91(5) . . . . ? C4 Fe C18 O1 -61(5) . . . . ? I Fe C18 O1 127(5) . . . . ? C18 Fe C19 O2 0(6) . . . . ? C2 Fe C19 O2 -178(100) . . . . ? C1 Fe C19 O2 133(6) . . . . ? C3 Fe C19 O2 159(6) . . . . ? C5 Fe C19 O2 94(6) . . . . ? C4 Fe C19 O2 119(6) . . . . ? I Fe C19 O2 -90(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 75.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.830 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.076 _iucr_refine_instructions_details ; TITL mima53 in P2(1)2(1)2(1) CELL 1.54184 8.498357 13.612668 16.384965 90.0000 90.0000 90.0000 ZERR 4.00 0.000100 0.000200 0.000200 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H O Fe I UNIT 76.00 92.00 8.00 4.00 4.00 TEMP -173 SIZE 0.12 0.1 0.02 OMIT 6 1 17 OMIT 0 6 15 OMIT 2 0 13 OMIT -2 12 13 OMIT -6 13 6 ACTA 150 CONF MERG 2 FMAP 2 PLAN 10 L.S. 4 ISOR C3 0.002 ISOR C4 0.001 WGHT 0.030100 1.546700 FVAR 3.48454 FE 4 0.253939 0.540142 0.761987 11.00000 0.00899 0.00871 = 0.00335 0.00128 -0.00056 -0.00149 I 5 0.021617 0.543791 0.865554 11.00000 0.01371 0.01846 = 0.00971 0.00076 0.00375 -0.00226 O1 3 0.399281 0.381090 0.851379 11.00000 0.02694 0.01885 = 0.01437 0.00645 -0.00633 -0.00476 O2 3 0.080797 0.398157 0.661536 11.00000 0.02148 0.01477 = 0.01437 -0.00276 -0.00464 -0.00205 C1 1 0.396222 0.659843 0.799814 11.00000 0.01666 0.01513 = 0.00808 0.00246 0.00022 -0.00823 C2 1 0.255973 0.695429 0.761915 11.00000 0.01842 0.00755 = 0.00824 0.00039 0.00290 -0.00182 AFIX 43 H2 2 0.181300 0.736634 0.788178 11.00000 -1.20000 AFIX 0 C3 1 0.241680 0.661653 0.680011 11.00000 0.01302 0.00774 = 0.00599 0.00223 0.00227 -0.00065 C4 1 0.385767 0.605666 0.663775 11.00000 0.00983 0.00973 = 0.00583 0.00176 0.00203 -0.00227 C5 1 0.478680 0.605057 0.737150 11.00000 0.01193 0.01484 = 0.00778 0.00239 -0.00146 -0.00647 C6 1 0.628373 0.556007 0.736958 11.00000 0.00994 0.02548 = 0.01574 0.00504 -0.00401 -0.00518 AFIX 43 H6 2 0.690833 0.554139 0.785018 11.00000 -1.20000 AFIX 0 C7 1 0.679282 0.512630 0.667796 11.00000 0.00811 0.02675 = 0.02514 0.00561 0.00423 0.00114 AFIX 43 H7 2 0.777792 0.479642 0.667906 11.00000 -1.20000 AFIX 0 C8 1 0.588676 0.515100 0.594425 11.00000 0.01837 0.02044 = 0.01294 0.00018 0.00635 -0.00035 AFIX 43 H8 2 0.629770 0.485393 0.546484 11.00000 -1.20000 AFIX 0 C9 1 0.445296 0.558851 0.591515 11.00000 0.01780 0.01364 = 0.00766 0.00070 0.00408 -0.00110 AFIX 43 H9 2 0.385367 0.558527 0.542572 11.00000 -1.20000 AFIX 0 C10 1 0.458006 0.693411 0.882195 11.00000 0.02591 0.02122 = 0.00619 0.00101 -0.00283 -0.01129 C11 1 0.599504 0.762713 0.864461 11.00000 0.02920 0.02563 = 0.01527 0.00079 -0.00517 -0.01635 AFIX 137 H11A 2 0.565626 0.815736 0.828019 11.00000 -1.50000 H11B 2 0.684168 0.725246 0.838381 11.00000 -1.50000 H11C 2 0.637851 0.790811 0.915811 11.00000 -1.50000 AFIX 0 C12 1 0.332654 0.751036 0.928658 11.00000 0.03918 0.02787 = 0.00938 -0.00958 0.00361 -0.01697 AFIX 137 H12A 2 0.239768 0.709504 0.936768 11.00000 -1.50000 H12B 2 0.303161 0.809448 0.897221 11.00000 -1.50000 H12C 2 0.374549 0.771153 0.981816 11.00000 -1.50000 AFIX 0 C13 1 0.512884 0.607422 0.936032 11.00000 0.04635 0.02876 = 0.01081 0.00609 -0.01403 -0.01485 AFIX 137 H13A 2 0.596061 0.570952 0.907781 11.00000 -1.50000 H13B 2 0.423865 0.563544 0.946832 11.00000 -1.50000 H13C 2 0.553690 0.632983 0.987786 11.00000 -1.50000 AFIX 0 C14 1 0.120459 0.696705 0.618673 11.00000 0.01614 0.01307 = 0.00715 0.00368 0.00100 0.00170 C15 1 0.204401 0.772166 0.563685 11.00000 0.02743 0.01912 = 0.01749 0.01291 0.00113 0.00155 AFIX 137 H15A 2 0.291049 0.739971 0.534665 11.00000 -1.50000 H15B 2 0.246160 0.825635 0.597373 11.00000 -1.50000 H15C 2 0.129364 0.798870 0.524056 11.00000 -1.50000 AFIX 0 C16 1 0.054011 0.613706 0.564813 11.00000 0.02089 0.01949 = 0.01425 0.00021 -0.00729 0.00250 AFIX 137 H16A 2 -0.008249 0.568706 0.598531 11.00000 -1.50000 H16B 2 0.141043 0.577651 0.539467 11.00000 -1.50000 H16C 2 -0.013023 0.641971 0.522186 11.00000 -1.50000 AFIX 0 C17 1 -0.017533 0.745712 0.662401 11.00000 0.02104 0.02199 = 0.01835 0.00199 0.00127 0.00970 AFIX 137 H17A 2 0.018028 0.807113 0.687601 11.00000 -1.50000 H17B 2 -0.058001 0.701550 0.704717 11.00000 -1.50000 H17C 2 -0.101149 0.759914 0.622939 11.00000 -1.50000 AFIX 0 C18 1 0.344116 0.442580 0.819360 11.00000 0.01099 0.02295 = 0.01123 -0.00479 -0.00110 -0.00820 C19 1 0.147466 0.455271 0.700132 11.00000 0.01192 0.01238 = 0.00768 0.00483 0.00380 0.00368 HKLF 4 ;