Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author ; Prof Alan Welch Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS ; _publ_contact_author_phone '0131 451-3217' _publ_contact_author_fax '0131 451 3180' _publ_contact_author_email A.J.Welch@hw.ac.uk _publ_requested_coeditor_name ? _publ_section_title ; New 13-vertex metallacarborane sandwich compounds, synthetic and structural studies ; loop_ _publ_author_name _publ_author_address D.Ellis ; Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS UK ; R.McIntosh ; Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS UK ; G.M.Rosair ; Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS UK ; A.J.Welch ; Department of Chemistry Heriot-Watt University Edinburgh EH14 4AS UK ; F.Teixidor ; Departament de Quimica Universitat Automona de Barcelona - CSIC Campus de Bellaterra 08193 Bellaterra Barcelona Spain ; C.Vinas ; Departament de Quimica Universitat Automona de Barcelona - CSIC Campus de Bellaterra 08193 Bellaterra Barcelona Spain ; ; S.Esquirolea ; ; Departament de Quimica Universitat Automona de Barcelona - CSIC Campus de Bellaterra 08193 Bellaterra Barcelona Spain ; _publ_contact_author_name 'Prof Alan Welch' #====================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 663037' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H24 B20 Co, C10 H16 N' _chemical_formula_sum 'C14 H40 B20 Co N' _chemical_formula_weight 497.60 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 17.4900(11) _cell_length_b 7.5085(5) _cell_length_c 20.7590(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.622(3) _cell_angle_gamma 90.00 _cell_volume 2687.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9326 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 32.98 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 63218 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 33.06 _reflns_number_total 10109 _reflns_number_gt 8290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0598P)^2^+0.0601P] 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 10109 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 Co4 Co 0.703164(7) 0.974251(17) 0.026317(6) 0.01009(4) Uani 1 1 d . . . C1A C 0.68792(5) 0.83156(13) 0.10967(5) 0.01331(16) Uani 1 1 d . . . H1A H 0.6867(7) 0.7076(18) 0.1146(6) 0.016 Uiso 1 1 d . . . B2A B 0.60974(6) 0.92410(16) 0.08933(5) 0.01480(19) Uani 1 1 d . . . H2A H 0.5575(7) 0.8446(18) 0.0750(6) 0.018 Uiso 1 1 d . . . B3A B 0.76702(6) 0.92075(15) 0.12837(5) 0.01403(18) Uani 1 1 d . . . H3A H 0.8188(7) 0.8425(17) 0.1408(6) 0.017 Uiso 1 1 d . . . B5A B 0.67692(6) 0.97195(14) 0.17536(6) 0.01364(19) Uani 1 1 d . . . H5A H 0.6720(7) 0.8917(18) 0.2148(6) 0.016 Uiso 1 1 d . . . B6A B 0.61141(6) 1.14820(14) 0.05357(5) 0.01313(18) Uani 1 1 d . . . H6A H 0.5649(7) 1.1773(17) 0.0133(6) 0.016 Uiso 1 1 d . . . B7A B 0.77867(6) 1.14426(14) 0.09663(5) 0.01304(18) Uani 1 1 d . . . H7A H 0.8342(7) 1.1661(18) 0.0835(6) 0.016 Uiso 1 1 d . . . B8A B 0.76605(6) 1.11678(15) 0.17847(5) 0.01393(19) Uani 1 1 d . . . H8A H 0.8121(7) 1.1096(17) 0.2204(6) 0.017 Uiso 1 1 d . . . B9A B 0.59572(6) 1.12141(15) 0.13462(5) 0.01386(19) Uani 1 1 d . . . H9A H 0.5389(7) 1.1248(17) 0.1477(6) 0.017 Uiso 1 1 d . . . C10A C 0.69805(5) 1.24742(12) 0.06012(5) 0.01268(16) Uani 1 1 d . . . H10A H 0.7047(6) 1.3288(19) 0.0261(6) 0.015 Uiso 1 1 d . . . B11A B 0.67609(6) 1.20906(15) 0.18683(5) 0.01466(19) Uani 1 1 d . . . H11A H 0.6682(7) 1.2600(18) 0.2324(6) 0.018 Uiso 1 1 d . . . B12A B 0.63733(6) 1.31754(15) 0.11186(5) 0.01424(19) Uani 1 1 d . . . H12A H 0.6084(7) 1.4452(18) 0.1019(6) 0.017 Uiso 1 1 d . . . B13A B 0.73767(6) 1.31527(15) 0.13790(5) 0.01434(19) Uani 1 1 d . . . H13A H 0.7681(8) 1.4469(18) 0.1451(6) 0.017 Uiso 1 1 d . . . C1B C 0.61732(5) 0.91278(13) -0.05275(4) 0.01311(16) Uani 1 1 d . . . H1B H 0.5670(7) 0.9292(18) -0.0541(6) 0.016 Uiso 1 1 d . . . B2B B 0.64951(6) 0.73019(15) -0.03046(5) 0.0159(2) Uani 1 1 d . . . H2B H 0.6024(7) 0.6167(18) -0.0176(6) 0.019 Uiso 1 1 d . . . B3B B 0.66169(6) 1.06895(15) -0.07650(5) 0.01382(18) Uani 1 1 d . . . H3B H 0.6310(7) 1.1999(17) -0.0896(6) 0.017 Uiso 1 1 d . . . B5B B 0.65559(6) 0.83146(15) -0.12008(5) 0.01507(19) Uani 1 1 d . . . H5B H 0.6097(7) 0.8028(18) -0.1632(6) 0.018 Uiso 1 1 d . . . B6B B 0.75392(6) 0.71805(14) 0.00044(6) 0.01493(19) Uani 1 1 d . . . H6B H 0.7711(7) 0.6333(17) 0.0449(6) 0.018 Uiso 1 1 d . . . B7B B 0.76617(6) 1.08011(15) -0.04846(5) 0.01330(18) Uani 1 1 d . . . H7B H 0.7912(7) 1.2161(19) -0.0347(6) 0.016 Uiso 1 1 d . . . B8B B 0.72978(6) 1.01015(15) -0.12876(6) 0.01433(19) Uani 1 1 d . . . H8B H 0.7285(7) 1.0991(18) -0.1695(6) 0.017 Uiso 1 1 d . . . B9B B 0.71697(6) 0.64047(15) -0.07881(6) 0.0162(2) Uani 1 1 d . . . H9B H 0.7058(8) 0.5057(17) -0.0889(7) 0.019 Uiso 1 1 d . . . C10B C 0.80675(5) 0.89734(13) -0.01074(5) 0.01342(16) Uani 1 1 d . . . H10B H 0.8498(7) 0.9192(19) 0.0206(6) 0.016 Uiso 1 1 d . . . B11B B 0.75125(6) 0.78226(16) -0.13467(6) 0.0161(2) Uani 1 1 d . . . H11B H 0.7581(7) 0.7264(18) -0.1804(7) 0.019 Uiso 1 1 d . . . B12B B 0.81226(6) 0.71707(15) -0.06079(6) 0.0164(2) Uani 1 1 d . . . H12B H 0.8636(7) 0.6335(18) -0.0546(6) 0.020 Uiso 1 1 d . . . B13B B 0.81942(6) 0.93316(16) -0.09012(5) 0.01563(19) Uani 1 1 d . . . H13B H 0.8775(8) 0.9838(17) -0.0960(7) 0.019 Uiso 1 1 d . . . C101 C 0.49142(6) 0.82999(14) 0.24115(5) 0.01814(19) Uani 1 1 d . . . H10D H 0.5463 0.8420 0.2356 0.022 Uiso 1 1 calc R . . H10C H 0.4590 0.8776 0.2012 0.022 Uiso 1 1 calc R . . C102 C 0.47863(6) 0.94263(14) 0.29806(5) 0.01654(18) Uani 1 1 d . . . C103 C 0.54037(7) 0.97522(15) 0.34879(6) 0.0244(2) Uani 1 1 d . . . H103 H 0.5898 0.9249 0.3471 0.029 Uiso 1 1 calc R . . C104 C 0.52993(7) 1.08082(17) 0.40171(6) 0.0284(2) Uani 1 1 d . . . H104 H 0.5720 1.1005 0.4363 0.034 Uiso 1 1 calc R . . C105 C 0.45840(7) 1.15732(15) 0.40405(6) 0.0240(2) Uani 1 1 d . . . H105 H 0.4512 1.2287 0.4404 0.029 Uiso 1 1 calc R . . C106 C 0.39715(6) 1.12942(14) 0.35312(5) 0.0202(2) Uani 1 1 d . . . H106 H 0.3482 1.1832 0.3543 0.024 Uiso 1 1 calc R . . C107 C 0.40727(6) 1.02300(13) 0.30039(5) 0.01663(18) Uani 1 1 d . . . H107 H 0.3652 1.0049 0.2657 0.020 Uiso 1 1 calc R . . C108 C 0.38787(5) 0.60203(14) 0.24149(5) 0.01875(19) Uani 1 1 d . . . H10G H 0.3773 0.4740 0.2430 0.028 Uiso 1 1 calc R . . H10F H 0.3610 0.6514 0.2001 0.028 Uiso 1 1 calc R . . H10E H 0.3693 0.6614 0.2780 0.028 Uiso 1 1 calc R . . C109 C 0.50158(7) 0.53956(15) 0.19090(6) 0.0243(2) Uani 1 1 d . . . H10J H 0.5574 0.5596 0.1941 0.036 Uiso 1 1 calc R . . H10I H 0.4744 0.5877 0.1494 0.036 Uiso 1 1 calc R . . H10H H 0.4914 0.4115 0.1928 0.036 Uiso 1 1 calc R . . C110 C 0.51378(6) 0.55370(15) 0.30949(6) 0.0223(2) Uani 1 1 d . . . H10M H 0.4949 0.6111 0.3462 0.033 Uiso 1 1 calc R . . H10L H 0.5697 0.5736 0.3133 0.033 Uiso 1 1 calc R . . H10K H 0.5034 0.4255 0.3102 0.033 Uiso 1 1 calc R . . N1 N 0.47310(4) 0.63139(11) 0.24668(4) 0.01551(16) 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 Co4 0.01007(7) 0.01005(7) 0.01004(7) -0.00016(4) 0.00131(4) -0.00038(4) C1A 0.0166(4) 0.0122(4) 0.0116(4) 0.0011(3) 0.0039(3) -0.0004(3) B2A 0.0151(4) 0.0147(5) 0.0149(5) 0.0007(4) 0.0032(4) -0.0016(4) B3A 0.0149(4) 0.0143(5) 0.0126(4) 0.0007(4) 0.0014(3) 0.0008(4) B5A 0.0136(4) 0.0152(5) 0.0123(5) 0.0009(4) 0.0027(4) -0.0005(3) B6A 0.0121(4) 0.0132(4) 0.0140(5) -0.0002(4) 0.0019(3) 0.0003(3) B7A 0.0122(4) 0.0131(4) 0.0135(5) -0.0007(4) 0.0012(3) -0.0008(3) B8A 0.0131(4) 0.0158(5) 0.0124(5) -0.0016(4) 0.0007(3) -0.0002(3) B9A 0.0130(4) 0.0153(5) 0.0135(5) 0.0004(4) 0.0028(3) 0.0004(3) C10A 0.0132(4) 0.0117(4) 0.0132(4) 0.0000(3) 0.0023(3) 0.0001(3) B11A 0.0143(4) 0.0161(5) 0.0138(5) -0.0011(4) 0.0027(3) -0.0003(3) B12A 0.0148(4) 0.0139(5) 0.0143(5) -0.0011(4) 0.0035(3) 0.0013(3) B13A 0.0145(4) 0.0142(5) 0.0145(5) -0.0023(4) 0.0027(3) -0.0013(3) C1B 0.0117(4) 0.0162(4) 0.0113(4) -0.0019(3) 0.0014(3) -0.0017(3) B2B 0.0180(5) 0.0146(5) 0.0152(5) -0.0013(4) 0.0031(4) -0.0021(4) B3B 0.0128(4) 0.0170(5) 0.0115(4) -0.0003(4) 0.0013(3) -0.0002(3) B5B 0.0156(4) 0.0165(5) 0.0129(5) -0.0019(4) 0.0017(3) -0.0021(4) B6B 0.0180(5) 0.0119(4) 0.0150(5) -0.0001(4) 0.0028(4) 0.0013(4) B7B 0.0135(4) 0.0136(4) 0.0129(4) 0.0008(4) 0.0025(3) -0.0007(3) B8B 0.0143(4) 0.0169(5) 0.0119(5) 0.0001(4) 0.0024(4) -0.0003(3) B9B 0.0198(5) 0.0138(5) 0.0152(5) -0.0017(4) 0.0031(4) -0.0006(4) C10B 0.0127(4) 0.0146(4) 0.0130(4) -0.0003(3) 0.0022(3) 0.0012(3) B11B 0.0167(4) 0.0179(5) 0.0140(5) -0.0021(4) 0.0035(4) -0.0004(4) B12B 0.0188(5) 0.0161(5) 0.0145(5) -0.0021(4) 0.0032(4) 0.0023(4) B13B 0.0153(4) 0.0180(5) 0.0141(5) -0.0017(4) 0.0041(4) -0.0006(4) C101 0.0194(4) 0.0164(4) 0.0202(5) 0.0005(4) 0.0078(4) -0.0022(3) C102 0.0155(4) 0.0152(4) 0.0191(5) 0.0001(4) 0.0034(3) -0.0019(3) C103 0.0167(5) 0.0225(5) 0.0315(6) -0.0034(4) -0.0028(4) -0.0006(4) C104 0.0291(6) 0.0242(5) 0.0275(6) -0.0042(5) -0.0083(4) -0.0027(4) C105 0.0349(6) 0.0172(5) 0.0200(5) -0.0039(4) 0.0051(4) -0.0028(4) C106 0.0224(5) 0.0164(5) 0.0231(5) 0.0000(4) 0.0073(4) 0.0009(4) C107 0.0168(4) 0.0165(4) 0.0164(5) 0.0012(4) 0.0020(3) -0.0001(3) C108 0.0133(4) 0.0199(5) 0.0232(5) -0.0017(4) 0.0033(3) -0.0016(3) C109 0.0263(5) 0.0230(5) 0.0264(6) -0.0067(4) 0.0126(4) 0.0012(4) C110 0.0174(4) 0.0238(5) 0.0249(5) 0.0058(4) 0.0014(4) 0.0020(4) N1 0.0139(3) 0.0154(4) 0.0181(4) -0.0004(3) 0.0051(3) 0.0004(3) _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 Co4 C1B 2.0826(9) . ? Co4 C1A 2.0897(9) . ? Co4 C10B 2.1618(9) . ? Co4 C10A 2.1745(9) . ? Co4 B7B 2.1972(11) . ? Co4 B7A 2.2044(10) . ? Co4 B6A 2.2147(10) . ? Co4 B6B 2.2218(11) . ? Co4 B3B 2.2517(11) . ? Co4 B3A 2.2596(11) . ? Co4 B2A 2.2885(11) . ? Co4 B2B 2.2931(11) . ? C1A B3A 1.5276(14) . ? C1A B2A 1.5289(14) . ? C1A B5A 1.7594(15) . ? C1A H1A 0.937(14) . ? B2A B9A 1.7933(16) . ? B2A B6A 1.8414(16) . ? B2A B5A 1.9993(16) . ? B2A H2A 1.090(12) . ? B3A B8A 1.8040(16) . ? B3A B7A 1.8267(16) . ? B3A B5A 2.0239(15) . ? B3A H3A 1.074(12) . ? B5A B11A 1.7966(15) . ? B5A B8A 1.8929(15) . ? B5A B9A 1.8947(15) . ? B5A H5A 1.031(13) . ? B6A C10A 1.6736(14) . ? B6A B9A 1.7611(15) . ? B6A B12A 1.7616(15) . ? B6A H6A 1.087(12) . ? B7A C10A 1.6748(14) . ? B7A B13A 1.7613(15) . ? B7A B8A 1.7616(15) . ? B7A H7A 1.064(12) . ? B8A B13A 1.7427(16) . ? B8A B11A 1.7541(15) . ? B8A H8A 1.084(12) . ? B9A B12A 1.7426(16) . ? B9A B11A 1.7533(15) . ? B9A H9A 1.074(12) . ? C10A B12A 1.7145(14) . ? C10A B13A 1.7241(14) . ? C10A H10A 0.957(13) . ? B11A B12A 1.7867(16) . ? B11A B13A 1.7869(15) . ? B11A H11A 1.051(13) . ? B12A B13A 1.7478(15) . ? B12A H12A 1.088(13) . ? B13A H13A 1.121(13) . ? C1B B2B 1.5243(15) . ? C1B B3B 1.5324(15) . ? C1B B5B 1.7571(14) . ? C1B H1B 0.885(13) . ? B2B B9B 1.8025(16) . ? B2B B6B 1.8340(15) . ? B2B B5B 2.0290(16) . ? B2B H2B 1.246(13) . ? B3B B8B 1.7949(16) . ? B3B B7B 1.8247(14) . ? B3B B5B 1.9943(16) . ? B3B H3B 1.132(13) . ? B5B B11B 1.7879(15) . ? B5B B8B 1.8960(16) . ? B5B B9B 1.9067(16) . ? B5B H5B 1.119(12) . ? B6B C10B 1.6707(15) . ? B6B B12B 1.7580(16) . ? B6B B9B 1.7631(16) . ? B6B H6B 1.119(13) . ? B7B C10B 1.6776(15) . ? B7B B13B 1.7612(16) . ? B7B B8B 1.7621(16) . ? B7B H7B 1.129(14) . ? B8B B13B 1.7364(16) . ? B8B B11B 1.7605(16) . ? B8B H8B 1.075(13) . ? B9B B12B 1.7436(16) . ? B9B B11B 1.7521(16) . ? B9B H9B 1.045(13) . ? C10B B12B 1.7188(15) . ? C10B B13B 1.7201(15) . ? C10B H10B 0.924(12) . ? B11B B12B 1.7841(16) . ? B11B B13B 1.7866(16) . ? B11B H11B 1.064(13) . ? B12B B13B 1.7448(17) . ? B12B H12B 1.085(13) . ? B13B H13B 1.110(14) . ? C101 C102 1.4997(15) . ? C101 N1 1.5336(13) . ? C101 H10D 0.9900 . ? C101 H10C 0.9900 . ? C102 C107 1.3945(14) . ? C102 C103 1.3981(15) . ? C103 C104 1.3915(18) . ? C103 H103 0.9500 . ? C104 C105 1.3848(17) . ? C104 H104 0.9500 . ? C105 C106 1.3896(15) . ? C105 H105 0.9500 . ? C106 C107 1.3901(15) . ? C106 H106 0.9500 . ? C107 H107 0.9500 . ? C108 N1 1.4928(12) . ? C108 H10G 0.9800 . ? C108 H10F 0.9800 . ? C108 H10E 0.9800 . ? C109 N1 1.5023(14) . ? C109 H10J 0.9800 . ? C109 H10I 0.9800 . ? C109 H10H 0.9800 . ? C110 N1 1.4955(14) . ? C110 H10M 0.9800 . ? C110 H10L 0.9800 . ? C110 H10K 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1B Co4 C1A 111.34(4) . . ? C1B Co4 C10B 101.36(4) . . ? C1A Co4 C10B 112.84(4) . . ? C1B Co4 C10A 113.60(4) . . ? C1A Co4 C10A 101.45(4) . . ? C10B Co4 C10A 116.68(4) . . ? C1B Co4 B7B 84.49(4) . . ? C1A Co4 B7B 156.77(4) . . ? C10B Co4 B7B 45.26(4) . . ? C10A Co4 B7B 86.52(4) . . ? C1B Co4 B7A 157.42(4) . . ? C1A Co4 B7A 83.91(4) . . ? C10B Co4 B7A 86.87(4) . . ? C10A Co4 B7A 44.97(4) . . ? B7B Co4 B7A 86.71(4) . . ? C1B Co4 B6A 82.78(4) . . ? C1A Co4 B6A 83.84(4) . . ? C10B Co4 B6A 159.16(4) . . ? C10A Co4 B6A 44.82(4) . . ? B7B Co4 B6A 115.95(4) . . ? B7A Co4 B6A 82.46(4) . . ? C1B Co4 B6B 83.23(4) . . ? C1A Co4 B6B 82.40(4) . . ? C10B Co4 B6B 44.78(4) . . ? C10A Co4 B6B 159.12(4) . . ? B7B Co4 B6B 82.79(4) . . ? B7A Co4 B6B 116.24(4) . . ? B6A Co4 B6B 155.26(4) . . ? C1B Co4 B3B 41.18(4) . . ? C1A Co4 B3B 151.80(4) . . ? C10B Co4 B3B 84.46(4) . . ? C10A Co4 B3B 89.08(4) . . ? B7B Co4 B3B 48.41(4) . . ? B7A Co4 B3B 120.48(4) . . ? B6A Co4 B3B 85.61(4) . . ? B6B Co4 B3B 97.05(4) . . ? C1B Co4 B3A 151.37(4) . . ? C1A Co4 B3A 40.89(4) . . ? C10B Co4 B3A 88.50(4) . . ? C10A Co4 B3A 84.59(4) . . ? B7B Co4 B3A 119.94(4) . . ? B7A Co4 B3A 48.29(4) . . ? B6A Co4 B3A 97.53(4) . . ? B6B Co4 B3A 85.29(4) . . ? B3B Co4 B3A 167.24(4) . . ? C1B Co4 B2A 85.67(4) . . ? C1A Co4 B2A 40.56(4) . . ? C10B Co4 B2A 151.68(4) . . ? C10A Co4 B2A 84.20(4) . . ? B7B Co4 B2A 162.49(4) . . ? B7A Co4 B2A 97.05(4) . . ? B6A Co4 B2A 48.24(4) . . ? B6B Co4 B2A 110.37(4) . . ? B3B Co4 B2A 116.50(4) . . ? B3A Co4 B2A 73.92(4) . . ? C1B Co4 B2B 40.41(4) . . ? C1A Co4 B2B 85.30(4) . . ? C10B Co4 B2B 84.20(4) . . ? C10A Co4 B2B 152.17(4) . . ? B7B Co4 B2B 97.84(4) . . ? B7A Co4 B2B 162.08(4) . . ? B6A Co4 B2B 110.54(4) . . ? B6B Co4 B2B 47.90(4) . . ? B3B Co4 B2B 74.08(4) . . ? B3A Co4 B2B 115.82(4) . . ? B2A Co4 B2B 83.82(4) . . ? B3A C1A B2A 126.95(9) . . ? B3A C1A B5A 75.65(7) . . ? B2A C1A B5A 74.52(7) . . ? B3A C1A Co4 75.54(6) . . ? B2A C1A Co4 76.73(6) . . ? B5A C1A Co4 112.35(6) . . ? B3A C1A H1A 116.4(8) . . ? B2A C1A H1A 116.5(7) . . ? B5A C1A H1A 120.2(8) . . ? Co4 C1A H1A 127.5(8) . . ? C1A B2A B9A 115.15(8) . . ? C1A B2A B6A 116.93(8) . . ? B9A B2A B6A 57.94(6) . . ? C1A B2A B5A 58.00(6) . . ? B9A B2A B5A 59.65(6) . . ? B6A B2A B5A 98.59(7) . . ? C1A B2A Co4 62.72(5) . . ? B9A B2A Co4 109.69(6) . . ? B6A B2A Co4 63.78(5) . . ? B5A B2A Co4 96.42(5) . . ? C1A B2A H2A 119.8(7) . . ? B9A B2A H2A 114.5(7) . . ? B6A B2A H2A 117.3(7) . . ? B5A B2A H2A 133.1(7) . . ? Co4 B2A H2A 125.4(7) . . ? C1A B3A B8A 114.13(8) . . ? C1A B3A B7A 117.51(8) . . ? B8A B3A B7A 58.05(6) . . ? C1A B3A B5A 57.37(6) . . ? B8A B3A B5A 58.94(6) . . ? B7A B3A B5A 98.17(7) . . ? C1A B3A Co4 63.57(5) . . ? B8A B3A Co4 110.16(6) . . ? B7A B3A Co4 64.28(5) . . ? B5A B3A Co4 96.63(5) . . ? C1A B3A H3A 120.8(7) . . ? B8A B3A H3A 113.3(7) . . ? B7A B3A H3A 116.7(7) . . ? B5A B3A H3A 132.9(7) . . ? Co4 B3A H3A 126.0(7) . . ? C1A B5A B11A 134.49(8) . . ? C1A B5A B8A 100.05(7) . . ? B11A B5A B8A 56.70(6) . . ? C1A B5A B9A 100.36(7) . . ? B11A B5A B9A 56.64(6) . . ? B8A B5A B9A 103.09(7) . . ? C1A B5A B2A 47.48(5) . . ? B11A B5A B2A 106.25(7) . . ? B8A B5A B2A 119.43(7) . . ? B9A B5A B2A 54.76(6) . . ? C1A B5A B3A 46.99(5) . . ? B11A B5A B3A 106.04(7) . . ? B8A B5A B3A 54.72(5) . . ? B9A B5A B3A 118.90(7) . . ? B2A B5A B3A 85.64(6) . . ? C1A B5A H5A 107.4(7) . . ? B11A B5A H5A 118.1(7) . . ? B8A B5A H5A 119.1(7) . . ? B9A B5A H5A 123.0(7) . . ? B2A B5A H5A 119.3(7) . . ? B3A B5A H5A 116.5(7) . . ? C10A B6A B9A 104.87(7) . . ? C10A B6A B12A 59.82(6) . . ? B9A B6A B12A 59.30(6) . . ? C10A B6A B2A 116.68(7) . . ? B9A B6A B2A 59.66(6) . . ? B12A B6A B2A 113.72(8) . . ? C10A B6A Co4 66.32(5) . . ? B9A B6A Co4 114.33(6) . . ? B12A B6A Co4 119.13(6) . . ? B2A B6A Co4 67.98(5) . . ? C10A B6A H6A 121.6(7) . . ? B9A B6A H6A 122.8(7) . . ? B12A B6A H6A 117.2(7) . . ? B2A B6A H6A 115.7(7) . . ? Co4 B6A H6A 113.8(7) . . ? C10A B7A B13A 60.17(6) . . ? C10A B7A B8A 105.00(7) . . ? B13A B7A B8A 59.30(6) . . ? C10A B7A B3A 116.86(7) . . ? B13A B7A B3A 114.53(8) . . ? B8A B7A B3A 60.33(6) . . ? C10A B7A Co4 66.57(5) . . ? B13A B7A Co4 119.78(6) . . ? B8A B7A Co4 114.39(6) . . ? B3A B7A Co4 67.43(5) . . ? C10A B7A H7A 123.2(7) . . ? B13A B7A H7A 118.4(7) . . ? B8A B7A H7A 122.2(7) . . ? B3A B7A H7A 113.3(7) . . ? Co4 B7A H7A 113.0(7) . . ? B13A B8A B11A 61.46(6) . . ? B13A B8A B7A 60.34(6) . . ? B11A B8A B7A 107.95(7) . . ? B13A B8A B3A 116.65(8) . . ? B11A B8A B3A 118.32(8) . . ? B7A B8A B3A 61.62(6) . . ? B13A B8A B5A 107.97(7) . . ? B11A B8A B5A 58.88(6) . . ? B7A B8A B5A 105.64(7) . . ? B3A B8A B5A 66.34(6) . . ? B13A B8A H8A 123.0(7) . . ? B11A B8A H8A 119.9(7) . . ? B7A B8A H8A 125.7(6) . . ? B3A B8A H8A 110.2(7) . . ? B5A B8A H8A 119.7(7) . . ? B12A B9A B11A 61.47(6) . . ? B12A B9A B6A 60.37(6) . . ? B11A B9A B6A 108.11(7) . . ? B12A B9A B2A 117.14(8) . . ? B11A B9A B2A 117.93(8) . . ? B6A B9A B2A 62.40(6) . . ? B12A B9A B5A 107.80(7) . . ? B11A B9A B5A 58.86(6) . . ? B6A B9A B5A 105.62(7) . . ? B2A B9A B5A 65.59(6) . . ? B12A B9A H9A 119.7(7) . . ? B11A B9A H9A 121.0(7) . . ? B6A B9A H9A 122.5(7) . . ? B2A B9A H9A 111.5(7) . . ? B5A B9A H9A 123.9(7) . . ? B6A C10A B7A 120.89(8) . . ? B6A C10A B12A 62.64(6) . . ? B7A C10A B12A 114.92(8) . . ? B6A C10A B13A 115.11(7) . . ? B7A C10A B13A 62.40(6) . . ? B12A C10A B13A 61.10(6) . . ? B6A C10A Co4 68.86(5) . . ? B7A C10A Co4 68.46(5) . . ? B12A C10A Co4 123.71(6) . . ? B13A C10A Co4 123.31(6) . . ? B6A C10A H10A 116.4(7) . . ? B7A C10A H10A 115.6(7) . . ? B12A C10A H10A 115.6(8) . . ? B13A C10A H10A 115.1(8) . . ? Co4 C10A H10A 110.3(8) . . ? B9A B11A B8A 115.48(8) . . ? B9A B11A B12A 58.97(6) . . ? B8A B11A B12A 108.05(8) . . ? B9A B11A B13A 108.26(8) . . ? B8A B11A B13A 58.95(6) . . ? B12A B11A B13A 58.56(6) . . ? B9A B11A B5A 64.50(6) . . ? B8A B11A B5A 64.42(6) . . ? B12A B11A B5A 110.28(8) . . ? B13A B11A B5A 110.36(8) . . ? B9A B11A H11A 118.8(7) . . ? B8A B11A H11A 119.2(7) . . ? B12A B11A H11A 122.1(7) . . ? B13A B11A H11A 122.1(7) . . ? B5A B11A H11A 119.0(7) . . ? C10A B12A B9A 103.93(7) . . ? C10A B12A B13A 59.72(6) . . ? B9A B12A B13A 110.56(8) . . ? C10A B12A B6A 57.54(6) . . ? B9A B12A B6A 60.34(6) . . ? B13A B12A B6A 109.59(7) . . ? C10A B12A B11A 102.77(7) . . ? B9A B12A B11A 59.56(6) . . ? B13A B12A B11A 60.73(6) . . ? B6A B12A B11A 106.61(8) . . ? C10A B12A H12A 118.0(7) . . ? B9A B12A H12A 126.5(7) . . ? B13A B12A H12A 118.6(7) . . ? B6A B12A H12A 116.6(7) . . ? B11A B12A H12A 131.6(7) . . ? C10A B13A B8A 103.73(7) . . ? C10A B13A B12A 59.18(6) . . ? B8A B13A B12A 110.36(8) . . ? C10A B13A B7A 57.43(6) . . ? B8A B13A B7A 60.36(6) . . ? B12A B13A B7A 109.03(7) . . ? C10A B13A B11A 102.38(7) . . ? B8A B13A B11A 59.58(6) . . ? B12A B13A B11A 60.71(6) . . ? B7A B13A B11A 106.51(8) . . ? C10A B13A H13A 119.5(7) . . ? B8A B13A H13A 126.8(7) . . ? B12A B13A H13A 117.5(7) . . ? B7A B13A H13A 119.0(7) . . ? B11A B13A H13A 129.5(7) . . ? B2B C1B B3B 127.21(8) . . ? B2B C1B B5B 76.02(7) . . ? B3B C1B B5B 74.29(7) . . ? B2B C1B Co4 77.24(6) . . ? B3B C1B Co4 75.34(5) . . ? B5B C1B Co4 112.56(6) . . ? B2B C1B H1B 116.8(9) . . ? B3B C1B H1B 115.9(9) . . ? B5B C1B H1B 122.1(8) . . ? Co4 C1B H1B 125.2(8) . . ? C1B B2B B9B 114.21(8) . . ? C1B B2B B6B 116.52(8) . . ? B9B B2B B6B 57.99(6) . . ? C1B B2B B5B 57.18(6) . . ? B9B B2B B5B 59.34(6) . . ? B6B B2B B5B 97.91(7) . . ? C1B B2B Co4 62.35(5) . . ? B9B B2B Co4 109.58(6) . . ? B6B B2B Co4 64.01(5) . . ? B5B B2B Co4 95.29(5) . . ? C1B B2B H2B 117.2(6) . . ? B9B B2B H2B 112.5(6) . . ? B6B B2B H2B 123.2(6) . . ? B5B B2B H2B 126.3(6) . . ? Co4 B2B H2B 131.7(6) . . ? C1B B3B B8B 115.41(8) . . ? C1B B3B B7B 117.81(8) . . ? B8B B3B B7B 58.26(6) . . ? C1B B3B B5B 58.01(6) . . ? B8B B3B B5B 59.77(6) . . ? B7B B3B B5B 99.24(7) . . ? C1B B3B Co4 63.48(5) . . ? B8B B3B Co4 110.74(6) . . ? B7B B3B Co4 64.23(5) . . ? B5B B3B Co4 97.59(6) . . ? C1B B3B H3B 119.8(6) . . ? B8B B3B H3B 113.8(6) . . ? B7B B3B H3B 116.5(6) . . ? B5B B3B H3B 132.9(6) . . ? Co4 B3B H3B 124.6(6) . . ? C1B B5B B11B 134.28(8) . . ? C1B B5B B8B 100.80(7) . . ? B11B B5B B8B 57.00(6) . . ? C1B B5B B9B 99.47(7) . . ? B11B B5B B9B 56.51(6) . . ? B8B B5B B9B 103.42(7) . . ? C1B B5B B3B 47.70(5) . . ? B11B B5B B3B 106.31(7) . . ? B8B B5B B3B 54.88(5) . . ? B9B B5B B3B 119.03(7) . . ? C1B B5B B2B 46.80(5) . . ? B11B B5B B2B 105.77(7) . . ? B8B B5B B2B 119.60(7) . . ? B9B B5B B2B 54.41(6) . . ? B3B B5B B2B 85.77(6) . . ? C1B B5B H5B 112.7(6) . . ? B11B B5B H5B 113.0(6) . . ? B8B B5B H5B 118.1(7) . . ? B9B B5B H5B 119.3(7) . . ? B3B B5B H5B 120.8(7) . . ? B2B B5B H5B 121.4(7) . . ? C10B B6B B12B 60.11(6) . . ? C10B B6B B9B 105.16(8) . . ? B12B B6B B9B 59.36(6) . . ? C10B B6B B2B 116.92(8) . . ? B12B B6B B2B 114.31(8) . . ? B9B B6B B2B 60.11(6) . . ? C10B B6B Co4 65.71(5) . . ? B12B B6B Co4 118.82(7) . . ? B9B B6B Co4 114.37(7) . . ? B2B B6B Co4 68.09(5) . . ? C10B B6B H6B 119.6(6) . . ? B12B B6B H6B 119.0(6) . . ? B9B B6B H6B 125.9(7) . . ? B2B B6B H6B 115.5(6) . . ? Co4 B6B H6B 110.8(7) . . ? C10B B7B B13B 59.97(6) . . ? C10B B7B B8B 104.80(8) . . ? B13B B7B B8B 59.05(6) . . ? C10B B7B B3B 115.74(8) . . ? B13B B7B B3B 113.46(8) . . ? B8B B7B B3B 60.03(6) . . ? C10B B7B Co4 66.26(5) . . ? B13B B7B Co4 119.28(7) . . ? B8B B7B Co4 114.59(6) . . ? B3B B7B Co4 67.36(5) . . ? C10B B7B H7B 120.4(6) . . ? B13B B7B H7B 118.5(6) . . ? B8B B7B H7B 124.9(6) . . ? B3B B7B H7B 116.6(6) . . ? Co4 B7B H7B 111.6(6) . . ? B13B B8B B11B 61.44(7) . . ? B13B B8B B7B 60.45(6) . . ? B11B B8B B7B 107.95(8) . . ? B13B B8B B3B 116.21(8) . . ? B11B B8B B3B 116.87(8) . . ? B7B B8B B3B 61.72(6) . . ? B13B B8B B5B 107.45(8) . . ? B11B B8B B5B 58.41(6) . . ? B7B B8B B5B 105.41(7) . . ? B3B B8B B5B 65.35(6) . . ? B13B B8B H8B 117.9(6) . . ? B11B B8B H8B 121.7(7) . . ? B7B B8B H8B 121.0(7) . . ? B3B B8B H8B 113.2(7) . . ? B5B B8B H8B 126.2(7) . . ? B12B B9B B11B 61.38(6) . . ? B12B B9B B6B 60.17(6) . . ? B11B B9B B6B 107.71(8) . . ? B12B B9B B2B 116.65(8) . . ? B11B B9B B2B 118.01(8) . . ? B6B B9B B2B 61.90(6) . . ? B12B B9B B5B 107.13(8) . . ? B11B B9B B5B 58.32(6) . . ? B6B B9B B5B 105.18(7) . . ? B2B B9B B5B 66.26(6) . . ? B12B B9B H9B 120.1(8) . . ? B11B B9B H9B 121.9(8) . . ? B6B B9B H9B 122.3(8) . . ? B2B B9B H9B 110.8(8) . . ? B5B B9B H9B 124.5(8) . . ? B6B C10B B7B 121.56(7) . . ? B6B C10B B12B 62.47(6) . . ? B7B C10B B12B 115.10(8) . . ? B6B C10B B13B 114.96(8) . . ? B7B C10B B13B 62.43(6) . . ? B12B C10B B13B 60.98(6) . . ? B6B C10B Co4 69.51(5) . . ? B7B C10B Co4 68.48(5) . . ? B12B C10B Co4 124.09(6) . . ? B13B C10B Co4 123.30(6) . . ? B6B C10B H10B 116.8(8) . . ? B7B C10B H10B 114.5(9) . . ? B12B C10B H10B 116.4(8) . . ? B13B C10B H10B 115.2(8) . . ? Co4 C10B H10B 109.6(8) . . ? B9B B11B B8B 116.36(8) . . ? B9B B11B B12B 59.08(6) . . ? B8B B11B B12B 108.10(8) . . ? B9B B11B B13B 108.38(8) . . ? B8B B11B B13B 58.61(6) . . ? B12B B11B B13B 58.50(6) . . ? B9B B11B B5B 65.17(6) . . ? B8B B11B B5B 64.59(6) . . ? B12B B11B B5B 110.69(8) . . ? B13B B11B B5B 110.11(8) . . ? B9B B11B H11B 117.0(7) . . ? B8B B11B H11B 120.2(7) . . ? B12B B11B H11B 121.3(7) . . ? B13B B11B H11B 123.2(7) . . ? B5B B11B H11B 118.7(7) . . ? C10B B12B B9B 103.96(7) . . ? C10B B12B B13B 59.55(6) . . ? B9B B12B B13B 110.71(8) . . ? C10B B12B B6B 57.43(6) . . ? B9B B12B B6B 60.46(6) . . ? B13B B12B B6B 109.42(8) . . ? C10B B12B B11B 102.57(8) . . ? B9B B12B B11B 59.55(6) . . ? B13B B12B B11B 60.82(6) . . ? B6B B12B B11B 106.52(7) . . ? C10B B12B H12B 120.9(7) . . ? B9B B12B H12B 125.2(7) . . ? B13B B12B H12B 118.2(7) . . ? B6B B12B H12B 119.1(7) . . ? B11B B12B H12B 128.6(7) . . ? C10B B13B B8B 104.10(7) . . ? C10B B13B B12B 59.48(6) . . ? B8B B13B B12B 111.03(8) . . ? C10B B13B B7B 57.60(6) . . ? B8B B13B B7B 60.50(6) . . ? B12B B13B B7B 109.67(8) . . ? C10B B13B B11B 102.42(8) . . ? B8B B13B B11B 59.94(6) . . ? B12B B13B B11B 60.68(7) . . ? B7B B13B B11B 106.83(7) . . ? C10B B13B H13B 115.2(8) . . ? B8B B13B H13B 127.4(7) . . ? B12B B13B H13B 118.5(7) . . ? B7B B13B H13B 114.1(7) . . ? B11B B13B H13B 134.7(7) . . ? C102 C101 N1 115.40(8) . . ? C102 C101 H10D 108.4 . . ? N1 C101 H10D 108.4 . . ? C102 C101 H10C 108.4 . . ? N1 C101 H10C 108.4 . . ? H10D C101 H10C 107.5 . . ? C107 C102 C103 118.76(10) . . ? C107 C102 C101 121.57(9) . . ? C103 C102 C101 119.60(9) . . ? C104 C103 C102 120.51(10) . . ? C104 C103 H103 119.7 . . ? C102 C103 H103 119.7 . . ? C105 C104 C103 120.17(10) . . ? C105 C104 H104 119.9 . . ? C103 C104 H104 119.9 . . ? C104 C105 C106 119.79(10) . . ? C104 C105 H105 120.1 . . ? C106 C105 H105 120.1 . . ? C105 C106 C107 120.15(10) . . ? C105 C106 H106 119.9 . . ? C107 C106 H106 119.9 . . ? C106 C107 C102 120.57(10) . . ? C106 C107 H107 119.7 . . ? C102 C107 H107 119.7 . . ? N1 C108 H10G 109.5 . . ? N1 C108 H10F 109.5 . . ? H10G C108 H10F 109.5 . . ? N1 C108 H10E 109.5 . . ? H10G C108 H10E 109.5 . . ? H10F C108 H10E 109.5 . . ? N1 C109 H10J 109.5 . . ? N1 C109 H10I 109.5 . . ? H10J C109 H10I 109.5 . . ? N1 C109 H10H 109.5 . . ? H10J C109 H10H 109.5 . . ? H10I C109 H10H 109.5 . . ? N1 C110 H10M 109.5 . . ? N1 C110 H10L 109.5 . . ? H10M C110 H10L 109.5 . . ? N1 C110 H10K 109.5 . . ? H10M C110 H10K 109.5 . . ? H10L C110 H10K 109.5 . . ? C108 N1 C110 109.22(8) . . ? C108 N1 C109 109.41(8) . . ? C110 N1 C109 108.79(8) . . ? C108 N1 C101 110.91(8) . . ? C110 N1 C101 111.69(8) . . ? C109 N1 C101 106.75(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.273 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.068 #===end data_3 _database_code_depnum_ccdc_archive 'CCDC 663038' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H78 B20 K2 N2 Ni O12' _chemical_formula_weight 1036.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.2433(6) _cell_length_b 42.477(3) _cell_length_c 15.4794(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.627(4) _cell_angle_gamma 90.00 _cell_volume 5383.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6464 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 23.18 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.771 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details 'SADABS, (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 50097 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_sigmaI/netI 0.1445 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -53 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 27.67 _reflns_number_total 12497 _reflns_number_gt 6331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1525P)^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 12497 _refine_ls_number_parameters 688 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1588 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.2408 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _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 Ni4 Ni 0.45616(8) 0.368433(15) 0.20524(4) 0.02313(19) Uani 1 1 d . . . C1A C 0.5724(7) 0.33073(12) 0.2614(3) 0.0275(11) Uani 1 1 d . . . H1 H 0.689(7) 0.3272(12) 0.265(3) 0.033 Uiso 1 1 d . . . B2A B 0.4633(8) 0.31732(14) 0.1810(4) 0.0269(13) Uani 1 1 d . . . H2 H 0.582(6) 0.3555(12) 0.397(3) 0.032 Uiso 1 1 d . . . B3A B 0.5004(7) 0.34659(14) 0.3369(4) 0.0258(13) Uani 1 1 d . . . H3 H 0.513(6) 0.3121(12) 0.125(3) 0.031 Uiso 1 1 d . . . B5A B 0.4506(8) 0.30024(14) 0.2979(4) 0.0287(13) Uani 1 1 d . . . H5 H 0.525(6) 0.2815(12) 0.328(3) 0.034 Uiso 1 1 d . . . B6A B 0.2539(7) 0.33349(14) 0.1612(3) 0.0231(12) Uani 1 1 d . . . H6 H 0.203(6) 0.3381(11) 0.087(3) 0.028 Uiso 1 1 d . . . B7A B 0.2833(7) 0.36023(14) 0.3236(3) 0.0234(12) Uani 1 1 d . . . H7 H 0.274(6) 0.3833(12) 0.360(3) 0.028 Uiso 1 1 d . . . B8A B 0.3348(7) 0.32475(14) 0.3765(4) 0.0267(13) Uani 1 1 d . . . H8 H 0.361(6) 0.3266(12) 0.444(3) 0.032 Uiso 1 1 d . . . B9A B 0.2925(7) 0.29448(14) 0.2020(4) 0.0260(13) Uani 1 1 d . . . H9 H 0.277(6) 0.2734(12) 0.157(3) 0.031 Uiso 1 1 d . . . C10A C 0.1590(6) 0.35118(12) 0.2383(3) 0.0231(11) Uani 1 1 d . . . H10 H 0.079(6) 0.3680(12) 0.213(3) 0.028 Uiso 1 1 d . . . B11A B 0.2398(7) 0.29402(15) 0.3100(3) 0.0273(13) Uani 1 1 d . . . H11 H 0.2083 0.2712 0.3404 0.033 Uiso 1 1 calc R . . B12A B 0.1126(7) 0.31283(13) 0.2231(3) 0.0240(12) Uani 1 1 d . . . H12 H -0.015(6) 0.3072(12) 0.186(3) 0.029 Uiso 1 1 d . . . B13A B 0.1353(8) 0.32955(14) 0.3280(4) 0.0263(13) Uani 1 1 d . . . H13 H 0.028(6) 0.3319(12) 0.372(3) 0.032 Uiso 1 1 d . . . C1B C 0.3476(6) 0.41218(12) 0.1992(3) 0.0237(11) Uani 1 1 d . . . H1E H 0.234(6) 0.4195(12) 0.224(3) 0.028 Uiso 1 1 d . . . B2B B 0.3302(8) 0.40032(14) 0.1056(4) 0.0263(13) Uani 1 1 d . . . H2E H 0.208(6) 0.3988(12) 0.071(3) 0.032 Uiso 1 1 d . . . B3B B 0.5091(7) 0.41698(14) 0.2558(4) 0.0255(13) Uani 1 1 d . . . H3E H 0.513(6) 0.4272(12) 0.321(3) 0.031 Uiso 1 1 d . . . B5B B 0.4420(7) 0.44026(15) 0.1378(4) 0.0282(13) Uani 1 1 d . . . H5E H 0.373(6) 0.4656(12) 0.140(3) 0.034 Uiso 1 1 d . . . B6B B 0.5034(8) 0.37791(15) 0.0699(4) 0.0296(14) Uani 1 1 d . . . H6E H 0.478(6) 0.3540(12) 0.027(3) 0.036 Uiso 1 1 d . . . B7B B 0.6935(7) 0.39762(15) 0.2238(4) 0.0275(13) Uani 1 1 d . . . H7E H 0.764(6) 0.3873(12) 0.281(3) 0.033 Uiso 1 1 d . . . B8B B 0.6586(7) 0.43784(15) 0.1991(4) 0.0277(13) Uani 1 1 d . . . H8E H 0.699(6) 0.4585(12) 0.240(3) 0.033 Uiso 1 1 d . . . B9B B 0.4635(8) 0.41772(16) 0.0354(4) 0.0330(15) Uani 1 1 d . . . H9E H 0.395(6) 0.4283(12) -0.027(4) 0.040 Uiso 1 1 d . . . C10B C 0.6858(7) 0.37993(14) 0.1295(3) 0.0319(13) Uani 1 1 d . . . H10E H 0.758(6) 0.3593(13) 0.129(3) 0.038 Uiso 1 1 d . . . B11B B 0.6253(8) 0.44151(16) 0.0850(4) 0.0345(15) Uani 1 1 d . . . H11E H 0.6550 0.4643 0.0540 0.041 Uiso 1 1 calc R . . B12B B 0.6623(8) 0.40318(16) 0.0402(4) 0.0350(15) Uani 1 1 d . . . H12E H 0.743(9) 0.3970(17) -0.030(5) 0.09(3) Uiso 1 1 d . . . B13B B 0.7801(8) 0.41606(15) 0.1363(4) 0.0325(14) Uani 1 1 d . . . H13E H 0.920(6) 0.4184(13) 0.132(3) 0.039 Uiso 1 1 d . . . N2 N 0.7066(6) 0.53662(12) 0.3245(4) 0.0445(13) Uani 1 1 d . . . N1 N -0.3577(6) 0.41640(11) 0.6646(3) 0.0395(12) Uani 1 1 d . . . C1S C -0.5460(6) 0.41142(14) 0.5200(3) 0.0321(12) Uani 1 1 d . . . H1S3 H -0.6582 0.4169 0.5294 0.048 Uiso 1 1 calc R . . H1S2 H -0.5428 0.3897 0.4990 0.048 Uiso 1 1 calc R . . H1S1 H -0.5085 0.4257 0.4768 0.048 Uiso 1 1 calc R . . C2S C -0.4413(7) 0.41436(13) 0.6005(4) 0.0323(12) Uani 1 1 d . . . C3S C 0.6216(7) 0.53473(14) 0.2606(4) 0.0368(14) Uani 1 1 d . . . C4S C 0.5112(7) 0.53218(14) 0.1798(3) 0.0375(14) Uani 1 1 d . . . H4S3 H 0.5279 0.5118 0.1523 0.056 Uiso 1 1 calc R . . H4S2 H 0.5340 0.5492 0.1404 0.056 Uiso 1 1 calc R . . H4S1 H 0.3979 0.5337 0.1928 0.056 Uiso 1 1 calc R . . K1 K -0.03452(13) 0.44126(3) 0.67279(6) 0.0233(3) Uani 1 1 d . . . O1A O 0.0833(4) 0.43183(8) 0.8476(2) 0.0285(8) Uani 1 1 d . . . O2A O 0.0834(4) 0.38107(8) 0.7265(2) 0.0280(8) Uani 1 1 d . . . O3A O 0.0408(4) 0.39796(8) 0.5485(2) 0.0250(8) Uani 1 1 d . . . O4A O -0.1760(4) 0.44843(8) 0.4996(2) 0.0238(8) Uani 1 1 d . . . O5A O -0.1685(4) 0.49938(8) 0.6143(2) 0.0236(8) Uani 1 1 d . . . O6A O -0.0908(4) 0.48676(8) 0.7953(2) 0.0252(8) Uani 1 1 d . . . C11A C 0.0784(5) 0.39926(9) 0.8716(2) 0.0332(13) Uani 1 1 d . . . H11X H -0.0364 0.3920 0.8678 0.040 Uiso 1 1 calc R . . H11Y H 0.1288 0.3965 0.9323 0.040 Uiso 1 1 calc R . . C12A C 0.1687(5) 0.38044(9) 0.8121(2) 0.0345(13) Uani 1 1 d R . . H11B H 0.2797 0.3892 0.8112 0.041 Uiso 1 1 calc R . . H11A H 0.1793 0.3584 0.8330 0.041 Uiso 1 1 calc R . . C13A C 0.1734(7) 0.36673(13) 0.6637(3) 0.0316(12) Uani 1 1 d . . . H12B H 0.2041 0.3450 0.6819 0.038 Uiso 1 1 calc R . . H12A H 0.2747 0.3788 0.6589 0.038 Uiso 1 1 calc R . . C14A C 0.0704(7) 0.36615(12) 0.5776(3) 0.0297(12) Uani 1 1 d . . . H13B H 0.1272 0.3544 0.5348 0.036 Uiso 1 1 calc R . . H13A H -0.0346 0.3555 0.5833 0.036 Uiso 1 1 calc R . . C15A C -0.0636(6) 0.39866(12) 0.4672(3) 0.0272(12) Uani 1 1 d . . . H14B H -0.1706 0.3891 0.4745 0.033 Uiso 1 1 calc R . . H14A H -0.0133 0.3865 0.4227 0.033 Uiso 1 1 calc R . . C16A C -0.0867(6) 0.43207(12) 0.4388(3) 0.0271(11) Uani 1 1 d . . . H15B H 0.0209 0.4422 0.4366 0.032 Uiso 1 1 calc R . . H15A H -0.1477 0.4329 0.3799 0.032 Uiso 1 1 calc R . . C17A C -0.2223(6) 0.47967(12) 0.4704(3) 0.0267(11) Uani 1 1 d . . . H16B H -0.3046 0.4785 0.4186 0.032 Uiso 1 1 calc R . . H16A H -0.1257 0.4911 0.4542 0.032 Uiso 1 1 calc R . . C18A C -0.2919(6) 0.49654(12) 0.5428(3) 0.0281(12) Uani 1 1 d . . . H17B H -0.3307 0.5177 0.5231 0.034 Uiso 1 1 calc R . . H17A H -0.3858 0.4846 0.5605 0.034 Uiso 1 1 calc R . . C19A C -0.2204(6) 0.51883(12) 0.6819(3) 0.0258(11) Uani 1 1 d . . . H18B H -0.3257 0.5111 0.6985 0.031 Uiso 1 1 calc R . . H18A H -0.2358 0.5408 0.6610 0.031 Uiso 1 1 calc R . . C20A C -0.0924(6) 0.51770(12) 0.7587(3) 0.0294(12) Uani 1 1 d . . . H19B H 0.0159 0.5227 0.7404 0.035 Uiso 1 1 calc R . . H19A H -0.1169 0.5334 0.8025 0.035 Uiso 1 1 calc R . . C21A C 0.0133(7) 0.48464(13) 0.8744(3) 0.0353(13) Uani 1 1 d . . . H20B H -0.0251 0.4992 0.9177 0.042 Uiso 1 1 calc R . . H20A H 0.1256 0.4908 0.8648 0.042 Uiso 1 1 calc R . . C22A C 0.0133(8) 0.45202(14) 0.9073(3) 0.0384(14) Uani 1 1 d . . . H21B H 0.0777 0.4508 0.9653 0.046 Uiso 1 1 calc R . . H21A H -0.0999 0.4453 0.9131 0.046 Uiso 1 1 calc R . . K2 K 0.44174(13) 0.21926(3) 0.24659(6) 0.0222(3) Uani 1 1 d . . . O1B O 0.1862(4) 0.17940(8) 0.2940(2) 0.0230(7) Uani 1 1 d . . . O2B O 0.4521(4) 0.19182(8) 0.41611(19) 0.0244(8) Uani 1 1 d . . . O3B O 0.7220(4) 0.22385(8) 0.36778(19) 0.0231(7) Uani 1 1 d . . . O4B O 0.7575(4) 0.22608(8) 0.1889(2) 0.0234(7) Uani 1 1 d . . . O5B O 0.4746(4) 0.22519(8) 0.06736(19) 0.0249(8) Uani 1 1 d . . . O6B O 0.2345(4) 0.18619(8) 0.1172(2) 0.0242(8) Uani 1 1 d . . . C11B C 0.2054(6) 0.16514(13) 0.3786(3) 0.0298(12) Uani 1 1 d . . . H11C H 0.2679 0.1453 0.3771 0.036 Uiso 1 1 calc R . . H11D H 0.0969 0.1602 0.3968 0.036 Uiso 1 1 calc R . . C12B C 0.2933(6) 0.18730(13) 0.4411(3) 0.0266(12) Uani 1 1 d . . . H12C H 0.2344 0.2076 0.4403 0.032 Uiso 1 1 calc R . . H12D H 0.3007 0.1786 0.5007 0.032 Uiso 1 1 calc R . . C13B C 0.5511(6) 0.21176(12) 0.4745(3) 0.0255(11) Uani 1 1 d . . . H13C H 0.5469 0.2048 0.5353 0.031 Uiso 1 1 calc R . . H13D H 0.5114 0.2337 0.4689 0.031 Uiso 1 1 calc R . . C14B C 0.7220(6) 0.20966(12) 0.4515(3) 0.0239(11) Uani 1 1 d . . . H14C H 0.7979 0.2209 0.4951 0.029 Uiso 1 1 calc R . . H14D H 0.7568 0.1874 0.4497 0.029 Uiso 1 1 calc R . . C15B C 0.8776(6) 0.22094(13) 0.3349(3) 0.0277(12) Uani 1 1 d . . . H15C H 0.8994 0.1986 0.3219 0.033 Uiso 1 1 calc R . . H15D H 0.9659 0.2286 0.3786 0.033 Uiso 1 1 calc R . . C16B C 0.8722(6) 0.24019(13) 0.2539(3) 0.0300(12) Uani 1 1 d . . . H16C H 0.8384 0.2620 0.2655 0.036 Uiso 1 1 calc R . . H16D H 0.9817 0.2409 0.2336 0.036 Uiso 1 1 calc R . . C17B C 0.7449(6) 0.24355(12) 0.1097(3) 0.0286(12) Uani 1 1 d . . . H17C H 0.8545 0.2462 0.0904 0.034 Uiso 1 1 calc R . . H17D H 0.6996 0.2647 0.1189 0.034 Uiso 1 1 calc R . . C18B C 0.6360(6) 0.22636(13) 0.0417(3) 0.0303(12) Uani 1 1 d . . . H18C H 0.6340 0.2373 -0.0148 0.036 Uiso 1 1 calc R . . H18D H 0.6775 0.2047 0.0350 0.036 Uiso 1 1 calc R . . C19B C 0.3629(6) 0.20979(12) 0.0040(3) 0.0281(12) Uani 1 1 d . . . H19C H 0.4082 0.1893 -0.0116 0.034 Uiso 1 1 calc R . . H19D H 0.3446 0.2228 -0.0492 0.034 Uiso 1 1 calc R . . C20B C 0.2053(6) 0.20491(12) 0.0409(3) 0.0284(12) Uani 1 1 d . . . H20C H 0.1588 0.2255 0.0553 0.034 Uiso 1 1 calc R . . H20D H 0.1261 0.1942 -0.0023 0.034 Uiso 1 1 calc R . . C21B C 0.0890(6) 0.17335(13) 0.1444(3) 0.0296(12) Uani 1 1 d . . . H21C H 0.0383 0.1585 0.1000 0.035 Uiso 1 1 calc R . . H21D H 0.0099 0.1904 0.1516 0.035 Uiso 1 1 calc R . . C22B C 0.1310(6) 0.15657(12) 0.2289(3) 0.0286(12) Uani 1 1 d . . . H22C H 0.0338 0.1454 0.2454 0.034 Uiso 1 1 calc R . . H22D H 0.2180 0.1409 0.2233 0.034 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 Ni4 0.0310(4) 0.0228(4) 0.0149(3) -0.0024(3) 0.0000(3) 0.0005(3) C1A 0.024(3) 0.031(3) 0.027(3) 0.003(2) 0.000(2) 0.003(2) B2A 0.034(3) 0.023(3) 0.024(3) 0.000(2) 0.004(3) 0.003(3) B3A 0.035(3) 0.024(3) 0.017(3) 0.001(2) -0.002(2) -0.001(3) B5A 0.034(3) 0.024(3) 0.027(3) -0.003(2) -0.003(3) 0.005(3) B6A 0.029(3) 0.024(3) 0.016(3) 0.000(2) 0.002(2) 0.000(2) B7A 0.031(3) 0.025(3) 0.016(3) -0.004(2) 0.007(2) 0.003(2) B8A 0.033(3) 0.028(3) 0.020(3) 0.007(2) 0.004(2) -0.001(3) B9A 0.034(3) 0.024(3) 0.019(3) -0.004(2) 0.001(2) 0.003(3) C10A 0.028(3) 0.023(3) 0.018(2) 0.001(2) 0.003(2) -0.001(2) B11A 0.035(3) 0.033(3) 0.015(3) 0.002(2) 0.005(2) -0.008(3) B12A 0.033(3) 0.021(3) 0.018(3) 0.000(2) 0.003(2) -0.002(2) B13A 0.037(4) 0.026(3) 0.016(3) 0.000(2) 0.003(2) -0.003(3) C1B 0.031(3) 0.021(3) 0.020(2) 0.003(2) 0.007(2) 0.001(2) B2B 0.030(3) 0.027(3) 0.022(3) 0.002(2) 0.002(2) -0.005(3) B3B 0.036(3) 0.022(3) 0.019(3) -0.003(2) 0.002(2) -0.005(3) B5B 0.028(3) 0.034(4) 0.022(3) 0.005(3) 0.000(2) -0.003(3) B6B 0.034(3) 0.036(4) 0.020(3) -0.004(3) 0.008(3) -0.006(3) B7B 0.026(3) 0.030(3) 0.026(3) -0.006(3) 0.001(3) -0.004(3) B8B 0.031(3) 0.029(3) 0.023(3) -0.003(3) 0.003(2) -0.003(3) B9B 0.040(4) 0.040(4) 0.020(3) 0.002(3) 0.004(3) -0.018(3) C10B 0.029(3) 0.034(3) 0.034(3) -0.010(2) 0.008(2) -0.003(2) B11B 0.044(4) 0.035(4) 0.025(3) -0.001(3) 0.007(3) -0.010(3) B12B 0.038(4) 0.040(4) 0.029(3) -0.007(3) 0.009(3) -0.013(3) B13B 0.031(4) 0.034(4) 0.034(3) -0.007(3) 0.010(3) -0.005(3) N2 0.032(3) 0.050(3) 0.052(3) 0.009(3) 0.003(3) 0.002(2) N1 0.041(3) 0.038(3) 0.039(3) 0.007(2) 0.005(2) -0.001(2) C1S 0.031(3) 0.040(3) 0.025(3) 0.003(2) 0.001(2) 0.004(2) C2S 0.034(3) 0.034(3) 0.030(3) 0.003(2) 0.006(3) 0.000(2) C3S 0.037(3) 0.037(4) 0.038(3) 0.003(3) 0.011(3) -0.004(3) C4S 0.042(3) 0.040(4) 0.031(3) 0.000(3) 0.005(3) -0.009(3) K1 0.0268(6) 0.0255(6) 0.0167(5) -0.0013(4) -0.0011(4) 0.0027(5) O1A 0.036(2) 0.034(2) 0.0150(16) -0.0004(15) 0.0014(15) -0.0005(16) O2A 0.030(2) 0.031(2) 0.0217(17) 0.0023(15) -0.0023(15) 0.0013(16) O3A 0.0290(19) 0.0238(19) 0.0211(17) -0.0023(14) -0.0012(15) 0.0018(15) O4A 0.033(2) 0.0226(19) 0.0158(16) 0.0002(13) 0.0038(14) 0.0012(15) O5A 0.0251(18) 0.0236(19) 0.0218(17) -0.0028(14) 0.0005(14) 0.0025(14) O6A 0.0283(19) 0.029(2) 0.0176(16) -0.0048(14) -0.0014(14) -0.0019(15) C11A 0.044(3) 0.036(3) 0.018(2) 0.008(2) -0.004(2) -0.012(3) C12A 0.042(3) 0.030(3) 0.028(3) 0.010(2) -0.011(2) -0.002(3) C13A 0.032(3) 0.030(3) 0.033(3) 0.004(2) 0.005(2) 0.009(2) C14A 0.037(3) 0.023(3) 0.030(3) -0.004(2) 0.007(2) 0.004(2) C15A 0.026(3) 0.036(3) 0.019(2) -0.011(2) -0.003(2) 0.002(2) C16A 0.032(3) 0.032(3) 0.018(2) -0.002(2) 0.005(2) 0.001(2) C17A 0.032(3) 0.023(3) 0.022(2) 0.003(2) -0.006(2) 0.000(2) C18A 0.027(3) 0.025(3) 0.031(3) 0.004(2) -0.002(2) 0.003(2) C19A 0.032(3) 0.021(3) 0.025(3) -0.003(2) 0.006(2) 0.004(2) C20A 0.036(3) 0.024(3) 0.031(3) -0.009(2) 0.013(2) -0.002(2) C21A 0.041(3) 0.040(4) 0.022(3) -0.013(2) -0.007(2) 0.008(3) C22A 0.051(4) 0.046(4) 0.019(3) -0.005(2) 0.005(3) 0.010(3) K2 0.0227(6) 0.0289(6) 0.0147(5) 0.0016(4) 0.0005(4) -0.0012(4) O1B 0.0272(19) 0.0233(19) 0.0186(16) 0.0034(14) 0.0027(14) -0.0022(14) O2B 0.0261(19) 0.032(2) 0.0153(16) -0.0002(14) 0.0043(14) 0.0003(15) O3B 0.0203(18) 0.032(2) 0.0161(16) 0.0017(14) 0.0005(13) 0.0038(15) O4B 0.0246(18) 0.0264(19) 0.0198(16) 0.0053(14) 0.0049(14) -0.0005(15) O5B 0.0260(19) 0.034(2) 0.0143(15) -0.0048(14) 0.0019(14) 0.0034(15) O6B 0.0264(19) 0.027(2) 0.0180(16) 0.0018(14) -0.0010(14) 0.0004(15) C11B 0.030(3) 0.034(3) 0.027(3) 0.012(2) 0.010(2) 0.001(2) C12B 0.026(3) 0.040(3) 0.015(2) 0.008(2) 0.004(2) 0.005(2) C13B 0.029(3) 0.033(3) 0.013(2) -0.002(2) -0.001(2) 0.001(2) C14B 0.032(3) 0.029(3) 0.009(2) -0.0007(19) -0.005(2) 0.002(2) C15B 0.021(3) 0.035(3) 0.027(3) -0.006(2) 0.002(2) -0.001(2) C16B 0.023(3) 0.032(3) 0.036(3) -0.005(2) 0.004(2) -0.008(2) C17B 0.028(3) 0.032(3) 0.027(3) 0.012(2) 0.010(2) 0.001(2) C18B 0.036(3) 0.038(3) 0.019(2) 0.010(2) 0.011(2) 0.008(2) C19B 0.042(3) 0.029(3) 0.013(2) -0.001(2) 0.001(2) 0.009(2) C20B 0.035(3) 0.030(3) 0.018(2) 0.002(2) -0.007(2) 0.004(2) C21B 0.027(3) 0.030(3) 0.032(3) -0.006(2) 0.002(2) -0.003(2) C22B 0.034(3) 0.022(3) 0.030(3) -0.002(2) 0.007(2) -0.006(2) _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 Ni4 C1A 2.012(5) . ? Ni4 C1B 2.060(5) . ? Ni4 B2A 2.205(6) . ? Ni4 B6B 2.212(6) . ? Ni4 B2B 2.219(6) . ? Ni4 B3A 2.231(6) . ? Ni4 B3B 2.231(6) . ? Ni4 B6A 2.277(6) . ? Ni4 B7B 2.306(6) . ? Ni4 C10B 2.389(5) . ? Ni4 B7A 2.472(5) . ? C1A B3A 1.527(8) . ? C1A B2A 1.557(8) . ? C1A B5A 1.770(8) . ? C1A H1 0.96(5) . ? B2A B9A 1.770(9) . ? B2A B6A 1.850(8) . ? B2A B5A 1.963(8) . ? B2A H3 1.03(5) . ? B3A B8A 1.815(8) . ? B3A B7A 1.870(8) . ? B3A B5A 2.086(8) . ? B3A H2 1.15(5) . ? B5A B11A 1.789(9) . ? B5A B9A 1.876(8) . ? B5A B8A 1.935(9) . ? B5A K2 3.530(6) . ? B5A H5 1.08(5) . ? B6A C10A 1.679(7) . ? B6A B9A 1.789(8) . ? B6A B12A 1.817(8) . ? B6A H6 1.19(5) . ? B7A C10A 1.621(7) . ? B7A B8A 1.745(8) . ? B7A B13A 1.792(8) . ? B7A H7 1.14(5) . ? B8A B13A 1.740(9) . ? B8A B11A 1.787(8) . ? B8A H8 1.04(5) . ? B9A B12A 1.739(8) . ? B9A B11A 1.776(8) . ? B9A K2 3.465(6) . ? B9A H9 1.14(5) . ? C10A B12A 1.684(8) . ? C10A B13A 1.694(7) . ? C10A H10 1.02(5) . ? B11A B13A 1.775(9) . ? B11A B12A 1.795(8) . ? B11A H11 1.1200 . ? B12A B13A 1.762(8) . ? B12A H12 1.16(5) . ? B13A H13 1.18(5) . ? C1B B3B 1.521(8) . ? C1B B2B 1.524(7) . ? C1B B5B 1.761(8) . ? C1B H1E 1.10(5) . ? B2B B9B 1.791(8) . ? B2B B6B 1.853(9) . ? B2B B5B 1.967(9) . ? B2B H2E 1.08(5) . ? B3B B8B 1.824(8) . ? B3B B7B 1.846(9) . ? B3B B5B 2.095(8) . ? B3B H3E 1.09(5) . ? B5B B11B 1.801(9) . ? B5B B9B 1.877(9) . ? B5B B8B 1.926(8) . ? B5B H5E 1.22(5) . ? B6B C10B 1.673(8) . ? B6B B9B 1.792(9) . ? B6B B12B 1.794(9) . ? B6B H6E 1.22(5) . ? B7B C10B 1.637(8) . ? B7B B8B 1.767(9) . ? B7B B13B 1.784(9) . ? B7B H7E 1.10(5) . ? B8B B13B 1.740(9) . ? B8B B11B 1.763(8) . ? B8B H8E 1.11(5) . ? B9B B12B 1.745(10) . ? B9B B11B 1.776(9) . ? B9B H9E 1.16(5) . ? C10B B12B 1.692(9) . ? C10B B13B 1.718(8) . ? C10B H10E 1.06(6) . ? B11B B13B 1.787(10) . ? B11B B12B 1.809(9) . ? B11B H11E 1.1200 . ? B12B B13B 1.767(9) . ? B12B H12E 1.36(7) . ? B13B H13E 1.17(5) . ? N2 C3S 1.147(7) . ? N2 K1 2.857(5) 3_666 ? N1 C2S 1.145(7) . ? N1 K1 2.855(5) . ? C1S C2S 1.436(7) . ? C1S H1S3 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S1 0.9800 . ? C3S C4S 1.463(8) . ? C4S H4S3 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S1 0.9800 . ? K1 O6A 2.783(3) . ? K1 O3A 2.783(3) . ? K1 O1A 2.796(3) . ? K1 O5A 2.811(3) . ? K1 O4A 2.814(3) . ? K1 O2A 2.826(4) . ? K1 N2 2.857(5) 3_666 ? O1A C22A 1.430(6) . ? O1A C11A 1.434(5) . ? O2A C13A 1.426(6) . ? O2A C12A 1.426(5) . ? O3A C14A 1.436(6) . ? O3A C15A 1.441(5) . ? O4A C16A 1.439(6) . ? O4A C17A 1.439(6) . ? O5A C18A 1.419(6) . ? O5A C19A 1.436(5) . ? O6A C21A 1.415(6) . ? O6A C20A 1.431(6) . ? C11A C12A 1.4831 . ? C11A H11X 0.9900 . ? C11A H11Y 0.9900 . ? C12A H11B 0.9900 . ? C12A H11A 0.9900 . ? C13A C14A 1.495(7) . ? C13A H12B 0.9900 . ? C13A H12A 0.9900 . ? C14A H13B 0.9900 . ? C14A H13A 0.9900 . ? C15A C16A 1.491(7) . ? C15A H14B 0.9900 . ? C15A H14A 0.9900 . ? C16A H15B 0.9900 . ? C16A H15A 0.9900 . ? C17A C18A 1.499(7) . ? C17A H16B 0.9900 . ? C17A H16A 0.9900 . ? C18A H17B 0.9900 . ? C18A H17A 0.9900 . ? C19A C20A 1.497(7) . ? C19A H18B 0.9900 . ? C19A H18A 0.9900 . ? C20A H19B 0.9900 . ? C20A H19A 0.9900 . ? C21A C22A 1.477(8) . ? C21A H20B 0.9900 . ? C21A H20A 0.9900 . ? C22A H21B 0.9900 . ? C22A H21A 0.9900 . ? K2 O3B 2.810(3) . ? K2 O5B 2.830(3) . ? K2 O6B 2.849(3) . ? K2 O4B 2.862(3) . ? K2 O1B 2.863(3) . ? K2 O2B 2.863(3) . ? K2 H5 2.97(5) . ? K2 H9 2.94(5) . ? O1B C22B 1.434(6) . ? O1B C11B 1.436(5) . ? O2B C12B 1.421(6) . ? O2B C13B 1.425(6) . ? O3B C14B 1.429(5) . ? O3B C15B 1.440(6) . ? O4B C17B 1.427(5) . ? O4B C16B 1.430(6) . ? O5B C19B 1.424(6) . ? O5B C18B 1.433(6) . ? O6B C20B 1.420(6) . ? O6B C21B 1.425(6) . ? C11B C12B 1.478(7) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C13B C14B 1.495(7) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B C16B 1.493(7) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? C17B C18B 1.492(7) . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? C19B C20B 1.492(7) . ? C19B H19C 0.9900 . ? C19B H19D 0.9900 . ? C20B H20C 0.9900 . ? C20B H20D 0.9900 . ? C21B C22B 1.494(7) . ? C21B H21C 0.9900 . ? C21B H21D 0.9900 . ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A Ni4 C1B 157.0(2) . . ? C1A Ni4 B2A 43.0(2) . . ? C1B Ni4 B2A 154.2(2) . . ? C1A Ni4 B6B 115.3(2) . . ? C1B Ni4 B6B 85.2(2) . . ? B2A Ni4 B6B 90.4(2) . . ? C1A Ni4 B2B 161.4(2) . . ? C1B Ni4 B2B 41.5(2) . . ? B2A Ni4 B2B 120.2(2) . . ? B6B Ni4 B2B 49.4(2) . . ? C1A Ni4 B3A 41.8(2) . . ? C1B Ni4 B3A 116.2(2) . . ? B2A Ni4 B3A 75.0(2) . . ? B6B Ni4 B3A 155.9(2) . . ? B2B Ni4 B3A 154.6(2) . . ? C1A Ni4 B3B 121.3(2) . . ? C1B Ni4 B3B 41.3(2) . . ? B2A Ni4 B3B 164.1(2) . . ? B6B Ni4 B3B 96.6(2) . . ? B2B Ni4 B3B 74.7(2) . . ? B3A Ni4 B3B 93.4(2) . . ? C1A Ni4 B6A 84.6(2) . . ? C1B Ni4 B6A 106.0(2) . . ? B2A Ni4 B6A 48.7(2) . . ? B6B Ni4 B6A 92.2(2) . . ? B2B Ni4 B6A 85.5(2) . . ? B3A Ni4 B6A 92.3(2) . . ? B3B Ni4 B6A 144.5(2) . . ? C1A Ni4 B7B 91.1(2) . . ? C1B Ni4 B7B 83.0(2) . . ? B2A Ni4 B7B 120.8(2) . . ? B6B Ni4 B7B 77.3(2) . . ? B2B Ni4 B7B 94.6(2) . . ? B3A Ni4 B7B 93.6(2) . . ? B3B Ni4 B7B 48.0(2) . . ? B6A Ni4 B7B 165.7(2) . . ? C1A Ni4 C10B 90.6(2) . . ? C1B Ni4 C10B 99.1(2) . . ? B2A Ni4 C10B 94.6(2) . . ? B6B Ni4 C10B 42.4(2) . . ? B2B Ni4 C10B 82.4(2) . . ? B3A Ni4 C10B 118.6(2) . . ? B3B Ni4 C10B 81.3(2) . . ? B6A Ni4 C10B 125.47(19) . . ? B7B Ni4 C10B 40.77(19) . . ? C1A Ni4 B7A 81.6(2) . . ? C1B Ni4 B7A 82.90(19) . . ? B2A Ni4 B7A 90.9(2) . . ? B6B Ni4 B7A 155.1(2) . . ? B2B Ni4 B7A 109.7(2) . . ? B3A Ni4 B7A 46.5(2) . . ? B3B Ni4 B7A 88.6(2) . . ? B6A Ni4 B7A 70.44(19) . . ? B7B Ni4 B7A 122.5(2) . . ? C10B Ni4 B7A 161.74(19) . . ? B3A C1A B2A 122.3(5) . . ? B3A C1A B5A 78.1(4) . . ? B2A C1A B5A 72.0(4) . . ? B3A C1A Ni4 76.8(3) . . ? B2A C1A Ni4 75.1(3) . . ? B5A C1A Ni4 117.5(3) . . ? B3A C1A H1 119(3) . . ? B2A C1A H1 118(3) . . ? B5A C1A H1 118(3) . . ? Ni4 C1A H1 125(3) . . ? C1A B2A B9A 116.9(4) . . ? C1A B2A B6A 116.0(4) . . ? B9A B2A B6A 59.2(3) . . ? C1A B2A B5A 59.0(3) . . ? B9A B2A B5A 60.1(3) . . ? B6A B2A B5A 98.2(4) . . ? C1A B2A Ni4 61.8(3) . . ? B9A B2A Ni4 118.1(4) . . ? B6A B2A Ni4 67.7(3) . . ? B5A B2A Ni4 101.6(3) . . ? C1A B2A H3 121(3) . . ? B9A B2A H3 116(3) . . ? B6A B2A H3 113(3) . . ? B5A B2A H3 141(3) . . ? Ni4 B2A H3 112(3) . . ? C1A B3A B8A 114.0(4) . . ? C1A B3A B7A 120.2(4) . . ? B8A B3A B7A 56.5(3) . . ? C1A B3A B5A 56.1(3) . . ? B8A B3A B5A 59.0(3) . . ? B7A B3A B5A 96.1(4) . . ? C1A B3A Ni4 61.4(3) . . ? B8A B3A Ni4 118.1(3) . . ? B7A B3A Ni4 73.5(3) . . ? B5A B3A Ni4 97.0(3) . . ? C1A B3A H2 122(3) . . ? B8A B3A H2 107(3) . . ? B7A B3A H2 117(3) . . ? B5A B3A H2 129(3) . . ? Ni4 B3A H2 128(3) . . ? C1A B5A B11A 137.3(5) . . ? C1A B5A B9A 102.2(4) . . ? B11A B5A B9A 57.9(3) . . ? C1A B5A B8A 98.4(4) . . ? B11A B5A B8A 57.2(3) . . ? B9A B5A B8A 102.7(4) . . ? C1A B5A B2A 49.0(3) . . ? B11A B5A B2A 107.8(4) . . ? B9A B5A B2A 54.9(3) . . ? B8A B5A B2A 117.6(4) . . ? C1A B5A B3A 45.7(3) . . ? B11A B5A B3A 105.7(4) . . ? B9A B5A B3A 116.6(4) . . ? B8A B5A B3A 53.5(3) . . ? B2A B5A B3A 83.6(3) . . ? C1A B5A K2 129.7(3) . . ? B11A B5A K2 83.4(3) . . ? B9A B5A K2 72.5(3) . . ? B8A B5A K2 131.8(3) . . ? B2A B5A K2 98.9(3) . . ? B3A B5A K2 169.5(3) . . ? C1A B5A H5 111(3) . . ? B11A B5A H5 111(3) . . ? B9A B5A H5 124(3) . . ? B8A B5A H5 115(3) . . ? B2A B5A H5 126(3) . . ? B3A B5A H5 119(3) . . ? K2 B5A H5 51(3) . . ? C10A B6A B9A 104.0(4) . . ? C10A B6A B12A 57.4(3) . . ? B9A B6A B12A 57.7(3) . . ? C10A B6A B2A 123.4(4) . . ? B9A B6A B2A 58.2(3) . . ? B12A B6A B2A 112.1(4) . . ? C10A B6A Ni4 83.1(3) . . ? B9A B6A Ni4 113.8(3) . . ? B12A B6A Ni4 130.4(3) . . ? B2A B6A Ni4 63.6(3) . . ? C10A B6A H6 118(2) . . ? B9A B6A H6 121(2) . . ? B12A B6A H6 114(2) . . ? B2A B6A H6 116(2) . . ? Ni4 B6A H6 110(2) . . ? C10A B7A B8A 105.9(4) . . ? C10A B7A B13A 59.3(3) . . ? B8A B7A B13A 58.9(3) . . ? C10A B7A B3A 121.6(4) . . ? B8A B7A B3A 60.2(3) . . ? B13A B7A B3A 114.7(4) . . ? C10A B7A Ni4 78.1(3) . . ? B8A B7A Ni4 109.9(3) . . ? B13A B7A Ni4 125.7(3) . . ? B3A B7A Ni4 59.9(2) . . ? C10A B7A H7 122(2) . . ? B8A B7A H7 122(2) . . ? B13A B7A H7 121(2) . . ? B3A B7A H7 109(2) . . ? Ni4 B7A H7 109(2) . . ? B13A B8A B7A 61.9(3) . . ? B13A B8A B11A 60.4(3) . . ? B7A B8A B11A 107.1(4) . . ? B13A B8A B3A 120.3(4) . . ? B7A B8A B3A 63.3(3) . . ? B11A B8A B3A 118.4(4) . . ? B13A B8A B5A 107.6(4) . . ? B7A B8A B5A 106.3(4) . . ? B11A B8A B5A 57.3(3) . . ? B3A B8A B5A 67.5(3) . . ? B13A B8A H8 120(3) . . ? B7A B8A H8 114(3) . . ? B11A B8A H8 131(3) . . ? B3A B8A H8 103(3) . . ? B5A B8A H8 127(3) . . ? B12A B9A B2A 120.1(4) . . ? B12A B9A B11A 61.4(3) . . ? B2A B9A B11A 117.7(4) . . ? B12A B9A B6A 62.0(3) . . ? B2A B9A B6A 62.7(3) . . ? B11A B9A B6A 106.8(4) . . ? B12A B9A B5A 108.8(4) . . ? B2A B9A B5A 65.1(3) . . ? B11A B9A B5A 58.6(3) . . ? B6A B9A B5A 103.8(4) . . ? B12A B9A K2 131.8(3) . . ? B2A B9A K2 105.7(3) . . ? B11A B9A K2 85.5(3) . . ? B6A B9A K2 165.8(3) . . ? B5A B9A K2 76.4(3) . . ? B12A B9A H9 115(2) . . ? B2A B9A H9 111(2) . . ? B11A B9A H9 123(3) . . ? B6A B9A H9 121(3) . . ? B5A B9A H9 128(3) . . ? K2 B9A H9 54(2) . . ? B7A C10A B6A 112.5(4) . . ? B7A C10A B12A 117.1(4) . . ? B6A C10A B12A 65.4(3) . . ? B7A C10A B13A 65.4(3) . . ? B6A C10A B13A 116.6(4) . . ? B12A C10A B13A 62.9(3) . . ? B7A C10A H10 118(3) . . ? B6A C10A H10 112(3) . . ? B12A C10A H10 120(3) . . ? B13A C10A H10 124(3) . . ? B13A B11A B9A 108.3(4) . . ? B13A B11A B8A 58.5(3) . . ? B9A B11A B8A 113.3(4) . . ? B13A B11A B12A 59.1(3) . . ? B9A B11A B12A 58.3(3) . . ? B8A B11A B12A 106.6(4) . . ? B13A B11A B5A 112.7(4) . . ? B9A B11A B5A 63.5(3) . . ? B8A B11A B5A 65.5(3) . . ? B12A B11A B5A 110.3(4) . . ? B13A B11A H11 121.9 . . ? B9A B11A H11 119.9 . . ? B8A B11A H11 119.8 . . ? B12A B11A H11 123.8 . . ? B5A B11A H11 116.5 . . ? C10A B12A B9A 106.0(4) . . ? C10A B12A B13A 58.9(3) . . ? B9A B12A B13A 110.6(4) . . ? C10A B12A B11A 102.9(4) . . ? B9A B12A B11A 60.3(3) . . ? B13A B12A B11A 59.9(3) . . ? C10A B12A B6A 57.2(3) . . ? B9A B12A B6A 60.3(3) . . ? B13A B12A B6A 106.6(4) . . ? B11A B12A B6A 104.8(4) . . ? C10A B12A H12 116(3) . . ? B9A B12A H12 124(2) . . ? B13A B12A H12 122(2) . . ? B11A B12A H12 134(3) . . ? B6A B12A H12 116(2) . . ? C10A B13A B8A 103.0(4) . . ? C10A B13A B12A 58.3(3) . . ? B8A B13A B12A 110.2(4) . . ? C10A B13A B11A 103.2(4) . . ? B8A B13A B11A 61.1(3) . . ? B12A B13A B11A 61.0(3) . . ? C10A B13A B7A 55.3(3) . . ? B8A B13A B7A 59.2(3) . . ? B12A B13A B7A 105.0(4) . . ? B11A B13A B7A 105.5(4) . . ? C10A B13A H13 126(2) . . ? B8A B13A H13 119(2) . . ? B12A B13A H13 124(2) . . ? B11A B13A H13 125(2) . . ? B7A B13A H13 121(2) . . ? B3B C1B B2B 124.9(5) . . ? B3B C1B B5B 78.9(4) . . ? B2B C1B B5B 73.2(4) . . ? B3B C1B Ni4 75.4(3) . . ? B2B C1B Ni4 74.8(3) . . ? B5B C1B Ni4 114.8(3) . . ? B3B C1B H1E 119(3) . . ? B2B C1B H1E 116(3) . . ? B5B C1B H1E 116(3) . . ? Ni4 C1B H1E 129(3) . . ? C1B B2B B9B 116.3(5) . . ? C1B B2B B6B 117.5(4) . . ? B9B B2B B6B 58.9(4) . . ? C1B B2B B5B 59.0(3) . . ? B9B B2B B5B 59.7(3) . . ? B6B B2B B5B 99.5(4) . . ? C1B B2B Ni4 63.7(3) . . ? B9B B2B Ni4 113.8(4) . . ? B6B B2B Ni4 65.1(3) . . ? B5B B2B Ni4 100.5(3) . . ? C1B B2B H2E 118(3) . . ? B9B B2B H2E 109(3) . . ? B6B B2B H2E 122(3) . . ? B5B B2B H2E 124(3) . . ? Ni4 B2B H2E 130(3) . . ? C1B B3B B8B 112.5(4) . . ? C1B B3B B7B 118.6(4) . . ? B8B B3B B7B 57.6(3) . . ? C1B B3B B5B 55.6(3) . . ? B8B B3B B5B 58.4(3) . . ? B7B B3B B5B 96.8(4) . . ? C1B B3B Ni4 63.3(3) . . ? B8B B3B Ni4 113.3(3) . . ? B7B B3B Ni4 68.1(3) . . ? B5B B3B Ni4 96.3(3) . . ? C1B B3B H3E 121(3) . . ? B8B B3B H3E 107(3) . . ? B7B B3B H3E 119(3) . . ? B5B B3B H3E 126(3) . . ? Ni4 B3B H3E 132(3) . . ? C1B B5B B11B 135.4(5) . . ? C1B B5B B9B 101.5(4) . . ? B11B B5B B9B 57.7(3) . . ? C1B B5B B8B 98.1(4) . . ? B11B B5B B8B 56.4(3) . . ? B9B B5B B8B 102.5(4) . . ? C1B B5B B2B 47.9(3) . . ? B11B B5B B2B 107.7(4) . . ? B9B B5B B2B 55.5(3) . . ? B8B B5B B2B 117.3(4) . . ? C1B B5B B3B 45.5(3) . . ? B11B B5B B3B 105.0(4) . . ? B9B B5B B3B 117.0(4) . . ? B8B B5B B3B 53.8(3) . . ? B2B B5B B3B 83.3(3) . . ? C1B B5B H5E 110(2) . . ? B11B B5B H5E 114(2) . . ? B9B B5B H5E 125(2) . . ? B8B B5B H5E 116(2) . . ? B2B B5B H5E 124(2) . . ? B3B B5B H5E 118(2) . . ? C10B B6B B9B 103.8(4) . . ? C10B B6B B12B 58.3(4) . . ? B9B B6B B12B 58.2(4) . . ? C10B B6B B2B 118.9(4) . . ? B9B B6B B2B 58.8(3) . . ? B12B B6B B2B 112.3(5) . . ? C10B B6B Ni4 74.5(3) . . ? B9B B6B Ni4 114.0(4) . . ? B12B B6B Ni4 124.4(4) . . ? B2B B6B Ni4 65.5(2) . . ? C10B B6B H6E 116(2) . . ? B9B B6B H6E 127(2) . . ? B12B B6B H6E 116(2) . . ? B2B B6B H6E 120(2) . . ? Ni4 B6B H6E 109(2) . . ? C10B B7B B8B 105.2(4) . . ? C10B B7B B13B 60.1(3) . . ? B8B B7B B13B 58.7(3) . . ? C10B B7B B3B 119.7(4) . . ? B8B B7B B3B 60.6(3) . . ? B13B B7B B3B 115.0(4) . . ? C10B B7B Ni4 72.3(3) . . ? B8B B7B Ni4 112.2(4) . . ? B13B B7B Ni4 123.3(4) . . ? B3B B7B Ni4 63.9(3) . . ? C10B B7B H7E 120(3) . . ? B8B B7B H7E 128(3) . . ? B13B B7B H7E 125(3) . . ? B3B B7B H7E 110(3) . . ? Ni4 B7B H7E 104(3) . . ? B13B B8B B11B 61.3(4) . . ? B13B B8B B7B 61.2(4) . . ? B11B B8B B7B 107.8(4) . . ? B13B B8B B3B 118.4(4) . . ? B11B B8B B3B 119.3(4) . . ? B7B B8B B3B 61.8(3) . . ? B13B B8B B5B 108.3(4) . . ? B11B B8B B5B 58.2(3) . . ? B7B B8B B5B 106.1(4) . . ? B3B B8B B5B 67.9(3) . . ? B13B B8B H8E 126(3) . . ? B11B B8B H8E 121(3) . . ? B7B B8B H8E 127(3) . . ? B3B B8B H8E 106(3) . . ? B5B B8B H8E 116(3) . . ? B12B B9B B11B 61.8(4) . . ? B12B B9B B2B 117.9(5) . . ? B11B B9B B2B 117.1(4) . . ? B12B B9B B6B 60.9(4) . . ? B11B B9B B6B 107.8(5) . . ? B2B B9B B6B 62.3(3) . . ? B12B B9B B5B 108.9(4) . . ? B11B B9B B5B 59.0(3) . . ? B2B B9B B5B 64.8(3) . . ? B6B B9B B5B 105.2(4) . . ? B12B B9B H9E 123(3) . . ? B11B B9B H9E 114(3) . . ? B2B B9B H9E 113(3) . . ? B6B B9B H9E 132(3) . . ? B5B B9B H9E 115(3) . . ? B7B C10B B6B 117.1(4) . . ? B7B C10B B12B 116.7(5) . . ? B6B C10B B12B 64.4(4) . . ? B7B C10B B13B 64.2(4) . . ? B6B C10B B13B 116.8(5) . . ? B12B C10B B13B 62.4(4) . . ? B7B C10B Ni4 66.9(3) . . ? B6B C10B Ni4 63.1(3) . . ? B12B C10B Ni4 119.9(4) . . ? B13B C10B Ni4 122.1(3) . . ? B7B C10B H10E 115(3) . . ? B6B C10B H10E 115(3) . . ? B12B C10B H10E 119(3) . . ? B13B C10B H10E 119(3) . . ? Ni4 C10B H10E 108(3) . . ? B8B B11B B9B 113.9(4) . . ? B8B B11B B13B 58.7(4) . . ? B9B B11B B13B 108.0(5) . . ? B8B B11B B5B 65.4(3) . . ? B9B B11B B5B 63.3(4) . . ? B13B B11B B5B 111.9(4) . . ? B8B B11B B12B 106.9(5) . . ? B9B B11B B12B 58.2(4) . . ? B13B B11B B12B 58.8(4) . . ? B5B B11B B12B 109.6(4) . . ? B8B B11B H11E 119.3 . . ? B9B B11B H11E 119.8 . . ? B13B B11B H11E 122.3 . . ? B5B B11B H11E 117.1 . . ? B12B B11B H11E 124.0 . . ? C10B B12B B9B 105.0(4) . . ? C10B B12B B13B 59.5(3) . . ? B9B B12B B13B 110.4(5) . . ? C10B B12B B6B 57.3(3) . . ? B9B B12B B6B 60.8(4) . . ? B13B B12B B6B 108.4(4) . . ? C10B B12B B11B 102.8(4) . . ? B9B B12B B11B 59.9(4) . . ? B13B B12B B11B 60.0(4) . . ? B6B B12B B11B 106.3(4) . . ? C10B B12B H12E 121(3) . . ? B9B B12B H12E 125(3) . . ? B13B B12B H12E 117(3) . . ? B6B B12B H12E 122(3) . . ? B11B B12B H12E 127(3) . . ? C10B B13B B8B 102.9(4) . . ? C10B B13B B12B 58.1(3) . . ? B8B B13B B12B 109.8(5) . . ? C10B B13B B7B 55.7(3) . . ? B8B B13B B7B 60.2(3) . . ? B12B B13B B7B 105.9(4) . . ? C10B B13B B11B 102.6(4) . . ? B8B B13B B11B 60.0(3) . . ? B12B B13B B11B 61.2(4) . . ? B7B B13B B11B 106.0(4) . . ? C10B B13B H13E 121(3) . . ? B8B B13B H13E 129(3) . . ? B12B B13B H13E 115(3) . . ? B7B B13B H13E 125(3) . . ? B11B B13B H13E 126(3) . . ? C3S N2 K1 121.2(4) . 3_666 ? C2S N1 K1 122.1(4) . . ? C2S C1S H1S3 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S3 C1S H1S2 109.5 . . ? C2S C1S H1S1 109.5 . . ? H1S3 C1S H1S1 109.5 . . ? H1S2 C1S H1S1 109.5 . . ? N1 C2S C1S 179.4(6) . . ? N2 C3S C4S 179.2(7) . . ? C3S C4S H4S3 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S3 C4S H4S2 109.5 . . ? C3S C4S H4S1 109.5 . . ? H4S3 C4S H4S1 109.5 . . ? H4S2 C4S H4S1 109.5 . . ? O6A K1 O3A 176.15(11) . . ? O6A K1 O1A 60.47(10) . . ? O3A K1 O1A 119.59(10) . . ? O6A K1 O5A 61.27(9) . . ? O3A K1 O5A 117.94(10) . . ? O1A K1 O5A 121.14(10) . . ? O6A K1 O4A 119.36(10) . . ? O3A K1 O4A 60.93(9) . . ? O1A K1 O4A 175.48(11) . . ? O5A K1 O4A 59.60(9) . . ? O6A K1 O2A 120.43(10) . . ? O3A K1 O2A 60.58(10) . . ? O1A K1 O2A 61.08(10) . . ? O5A K1 O2A 176.58(10) . . ? O4A K1 O2A 117.96(10) . . ? O6A K1 N1 93.37(12) . . ? O3A K1 N1 90.37(12) . . ? O1A K1 N1 102.00(13) . . ? O5A K1 N1 88.88(12) . . ? O4A K1 N1 73.48(12) . . ? O2A K1 N1 88.05(12) . . ? O6A K1 N2 89.64(13) . 3_666 ? O3A K1 N2 86.62(13) . 3_666 ? O1A K1 N2 79.09(13) . 3_666 ? O5A K1 N2 92.98(13) . 3_666 ? O4A K1 N2 105.41(13) . 3_666 ? O2A K1 N2 90.03(13) . 3_666 ? N1 K1 N2 176.95(15) . 3_666 ? C22A O1A C11A 112.6(4) . . ? C22A O1A K1 114.7(3) . . ? C11A O1A K1 111.8(2) . . ? C13A O2A C12A 112.7(4) . . ? C13A O2A K1 112.0(3) . . ? C12A O2A K1 113.9(2) . . ? C14A O3A C15A 110.9(4) . . ? C14A O3A K1 116.6(3) . . ? C15A O3A K1 115.6(3) . . ? C16A O4A C17A 112.2(4) . . ? C16A O4A K1 112.5(3) . . ? C17A O4A K1 117.7(3) . . ? C18A O5A C19A 111.7(4) . . ? C18A O5A K1 113.3(3) . . ? C19A O5A K1 114.2(3) . . ? C21A O6A C20A 112.2(4) . . ? C21A O6A K1 114.4(3) . . ? C20A O6A K1 111.3(3) . . ? O1A C11A C12A 109.1(2) . . ? O1A C11A H11X 109.9 . . ? C12A C11A H11X 109.9 . . ? O1A C11A H11Y 109.9 . . ? C12A C11A H11Y 109.9 . . ? H11X C11A H11Y 108.3 . . ? O2A C12A C11A 109.8(2) . . ? O2A C12A H11B 109.7 . . ? C11A C12A H11B 109.7 . . ? O2A C12A H11A 109.7 . . ? C11A C12A H11A 109.7 . . ? H11B C12A H11A 108.2 . . ? O2A C13A C14A 109.2(4) . . ? O2A C13A H12B 109.8 . . ? C14A C13A H12B 109.8 . . ? O2A C13A H12A 109.8 . . ? C14A C13A H12A 109.8 . . ? H12B C13A H12A 108.3 . . ? O3A C14A C13A 108.8(4) . . ? O3A C14A H13B 109.9 . . ? C13A C14A H13B 109.9 . . ? O3A C14A H13A 109.9 . . ? C13A C14A H13A 109.9 . . ? H13B C14A H13A 108.3 . . ? O3A C15A C16A 108.7(4) . . ? O3A C15A H14B 110.0 . . ? C16A C15A H14B 110.0 . . ? O3A C15A H14A 110.0 . . ? C16A C15A H14A 110.0 . . ? H14B C15A H14A 108.3 . . ? O4A C16A C15A 108.9(4) . . ? O4A C16A H15B 109.9 . . ? C15A C16A H15B 109.9 . . ? O4A C16A H15A 109.9 . . ? C15A C16A H15A 109.9 . . ? H15B C16A H15A 108.3 . . ? O4A C17A C18A 108.5(4) . . ? O4A C17A H16B 110.0 . . ? C18A C17A H16B 110.0 . . ? O4A C17A H16A 110.0 . . ? C18A C17A H16A 110.0 . . ? H16B C17A H16A 108.4 . . ? O5A C18A C17A 108.8(4) . . ? O5A C18A H17B 109.9 . . ? C17A C18A H17B 109.9 . . ? O5A C18A H17A 109.9 . . ? C17A C18A H17A 109.9 . . ? H17B C18A H17A 108.3 . . ? O5A C19A C20A 108.6(4) . . ? O5A C19A H18B 110.0 . . ? C20A C19A H18B 110.0 . . ? O5A C19A H18A 110.0 . . ? C20A C19A H18A 110.0 . . ? H18B C19A H18A 108.4 . . ? O6A C20A C19A 108.5(4) . . ? O6A C20A H19B 110.0 . . ? C19A C20A H19B 110.0 . . ? O6A C20A H19A 110.0 . . ? C19A C20A H19A 110.0 . . ? H19B C20A H19A 108.4 . . ? O6A C21A C22A 109.5(4) . . ? O6A C21A H20B 109.8 . . ? C22A C21A H20B 109.8 . . ? O6A C21A H20A 109.8 . . ? C22A C21A H20A 109.8 . . ? H20B C21A H20A 108.2 . . ? O1A C22A C21A 108.9(4) . . ? O1A C22A H21B 109.9 . . ? C21A C22A H21B 109.9 . . ? O1A C22A H21A 109.9 . . ? C21A C22A H21A 109.9 . . ? H21B C22A H21A 108.3 . . ? O3B K2 O5B 118.96(10) . . ? O3B K2 O6B 152.13(10) . . ? O5B K2 O6B 58.12(10) . . ? O3B K2 O4B 59.60(9) . . ? O5B K2 O4B 59.46(9) . . ? O6B K2 O4B 108.89(10) . . ? O3B K2 O1B 116.27(10) . . ? O5B K2 O1B 117.41(10) . . ? O6B K2 O1B 59.30(9) . . ? O4B K2 O1B 149.56(10) . . ? O3B K2 O2B 58.74(9) . . ? O5B K2 O2B 159.82(10) . . ? O6B K2 O2B 113.32(10) . . ? O4B K2 O2B 113.26(10) . . ? O1B K2 O2B 57.97(9) . . ? O3B K2 B9A 108.34(12) . . ? O5B K2 B9A 78.13(12) . . ? O6B K2 B9A 98.29(12) . . ? O4B K2 B9A 99.16(12) . . ? O1B K2 B9A 109.97(13) . . ? O2B K2 B9A 122.04(12) . . ? O3B K2 B5A 77.75(12) . . ? O5B K2 B5A 97.59(12) . . ? O6B K2 B5A 129.36(12) . . ? O4B K2 B5A 88.59(13) . . ? O1B K2 B5A 121.03(13) . . ? O2B K2 B5A 101.11(12) . . ? B9A K2 B5A 31.10(13) . . ? O3B K2 H5 61.6(10) . . ? O5B K2 H5 107.0(10) . . ? O6B K2 H5 145.7(10) . . ? O4B K2 H5 82.5(10) . . ? O1B K2 H5 123.9(10) . . ? O2B K2 H5 89.6(10) . . ? B9A K2 H5 47.4(10) . . ? B5A K2 H5 16.3(10) . . ? O3B K2 H9 124.2(10) . . ? O5B K2 H9 63.7(10) . . ? O6B K2 H9 81.1(10) . . ? O4B K2 H9 99.3(9) . . ? O1B K2 H9 105.6(9) . . ? O2B K2 H9 135.7(10) . . ? B9A K2 H9 18.2(10) . . ? B5A K2 H9 48.8(10) . . ? H5 K2 H9 65.0(14) . . ? C22B O1B C11B 110.4(4) . . ? C22B O1B K2 113.8(3) . . ? C11B O1B K2 118.5(3) . . ? C12B O2B C13B 112.7(3) . . ? C12B O2B K2 111.9(2) . . ? C13B O2B K2 107.1(3) . . ? C14B O3B C15B 112.2(4) . . ? C14B O3B K2 119.3(3) . . ? C15B O3B K2 117.1(3) . . ? C17B O4B C16B 111.3(4) . . ? C17B O4B K2 110.0(3) . . ? C16B O4B K2 112.0(3) . . ? C19B O5B C18B 111.9(4) . . ? C19B O5B K2 120.4(3) . . ? C18B O5B K2 118.1(3) . . ? C20B O6B C21B 113.1(4) . . ? C20B O6B K2 109.8(3) . . ? C21B O6B K2 115.9(3) . . ? O1B C11B C12B 108.8(4) . . ? O1B C11B H11C 109.9 . . ? C12B C11B H11C 109.9 . . ? O1B C11B H11D 109.9 . . ? C12B C11B H11D 109.9 . . ? H11C C11B H11D 108.3 . . ? O2B C12B C11B 107.8(4) . . ? O2B C12B H12C 110.1 . . ? C11B C12B H12C 110.1 . . ? O2B C12B H12D 110.1 . . ? C11B C12B H12D 110.1 . . ? H12C C12B H12D 108.5 . . ? O2B C13B C14B 107.4(4) . . ? O2B C13B H13C 110.2 . . ? C14B C13B H13C 110.2 . . ? O2B C13B H13D 110.2 . . ? C14B C13B H13D 110.2 . . ? H13C C13B H13D 108.5 . . ? O3B C14B C13B 106.9(4) . . ? O3B C14B H14C 110.3 . . ? C13B C14B H14C 110.3 . . ? O3B C14B H14D 110.3 . . ? C13B C14B H14D 110.3 . . ? H14C C14B H14D 108.6 . . ? O3B C15B C16B 108.0(4) . . ? O3B C15B H15C 110.1 . . ? C16B C15B H15C 110.1 . . ? O3B C15B H15D 110.1 . . ? C16B C15B H15D 110.1 . . ? H15C C15B H15D 108.4 . . ? O4B C16B C15B 108.3(4) . . ? O4B C16B H16C 110.0 . . ? C15B C16B H16C 110.0 . . ? O4B C16B H16D 110.0 . . ? C15B C16B H16D 110.0 . . ? H16C C16B H16D 108.4 . . ? O4B C17B C18B 109.2(4) . . ? O4B C17B H17C 109.8 . . ? C18B C17B H17C 109.8 . . ? O4B C17B H17D 109.8 . . ? C18B C17B H17D 109.8 . . ? H17C C17B H17D 108.3 . . ? O5B C18B C17B 108.9(4) . . ? O5B C18B H18C 109.9 . . ? C17B C18B H18C 109.9 . . ? O5B C18B H18D 109.9 . . ? C17B C18B H18D 109.9 . . ? H18C C18B H18D 108.3 . . ? O5B C19B C20B 108.8(4) . . ? O5B C19B H19C 109.9 . . ? C20B C19B H19C 109.9 . . ? O5B C19B H19D 109.9 . . ? C20B C19B H19D 109.9 . . ? H19C C19B H19D 108.3 . . ? O6B C20B C19B 108.9(4) . . ? O6B C20B H20C 109.9 . . ? C19B C20B H20C 109.9 . . ? O6B C20B H20D 109.9 . . ? C19B C20B H20D 109.9 . . ? H20C C20B H20D 108.3 . . ? O6B C21B C22B 108.9(4) . . ? O6B C21B H21C 109.9 . . ? C22B C21B H21C 109.9 . . ? O6B C21B H21D 109.9 . . ? C22B C21B H21D 109.9 . . ? H21C C21B H21D 108.3 . . ? O1B C22B C21B 108.4(4) . . ? O1B C22B H22C 110.0 . . ? C21B C22B H22C 110.0 . . ? O1B C22B H22D 110.0 . . ? C21B C22B H22D 110.0 . . ? H22C C22B H22D 108.4 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.666 _refine_diff_density_min -0.930 _refine_diff_density_rms 0.168 #===end data_4 _database_code_depnum_ccdc_archive 'CCDC 663039' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H72 B20 Fe K2 O12' _chemical_formula_weight 951.11 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 17.3264(19) _cell_length_b 17.501(2) _cell_length_c 18.566(2) _cell_angle_alpha 85.816(7) _cell_angle_beta 83.028(7) _cell_angle_gamma 60.542(7) _cell_volume 4865.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4375 _cell_measurement_theta_min 3.33 _cell_measurement_theta_max 28.18 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.533 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details 'SADABS (Sheldrick 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 141651 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.30 _reflns_number_total 23691 _reflns_number_gt 14216 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0563P)^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 23691 _refine_ls_number_parameters 1279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Fe4A Fe 0.724460(18) 0.528154(18) 0.744036(14) 0.01022(7) Uani 1 1 d . . . C1A C 0.64739(13) 0.65738(12) 0.77740(10) 0.0124(4) Uani 1 1 d . . . H1A H 0.6135(13) 0.7071(13) 0.7469(11) 0.015 Uiso 1 1 d . . . B2A B 0.74273(15) 0.63637(15) 0.78545(12) 0.0131(5) Uani 1 1 d . . . H2A H 0.7694(13) 0.6785(13) 0.7564(10) 0.016 Uiso 1 1 d . . . B3A B 0.59772(16) 0.61026(15) 0.81412(12) 0.0138(5) Uani 1 1 d . . . H3A H 0.5307(13) 0.6305(13) 0.8000(10) 0.017 Uiso 1 1 d . . . B5A B 0.64337(15) 0.67081(15) 0.86985(12) 0.0129(5) Uani 1 1 d . . . H5A H 0.6030(13) 0.7383(13) 0.8862(10) 0.015 Uiso 1 1 d . . . B6A B 0.81787(15) 0.52881(15) 0.81586(12) 0.0126(5) Uani 1 1 d . . . H6A H 0.8883(13) 0.5009(13) 0.7944(10) 0.015 Uiso 1 1 d . . . B7A B 0.66275(15) 0.49883(15) 0.84532(11) 0.0113(5) Uani 1 1 d . . . H7A H 0.6366(13) 0.4569(13) 0.8436(10) 0.014 Uiso 1 1 d . . . B8A B 0.61185(15) 0.58501(15) 0.90857(12) 0.0132(5) Uani 1 1 d . . . H8A H 0.5529(13) 0.5998(13) 0.9401(10) 0.016 Uiso 1 1 d . . . B9A B 0.76884(15) 0.61515(15) 0.87892(12) 0.0132(5) Uani 1 1 d . . . H9A H 0.8013(13) 0.6517(13) 0.8932(10) 0.016 Uiso 1 1 d . . . C10A C 0.77235(13) 0.46465(13) 0.84435(10) 0.0118(4) Uani 1 1 d . . . H10A H 0.8086(13) 0.4053(14) 0.8361(10) 0.014 Uiso 1 1 d . . . B11A B 0.69624(15) 0.59614(15) 0.94275(12) 0.0127(5) Uani 1 1 d . . . H11A H 0.6858(13) 0.6196(13) 0.9980(11) 0.015 Uiso 1 1 d . . . B12A B 0.80119(15) 0.50884(15) 0.90940(12) 0.0132(5) Uani 1 1 d . . . H12A H 0.8613(13) 0.4673(13) 0.9391(10) 0.016 Uiso 1 1 d . . . B13A B 0.70888(15) 0.49144(15) 0.92678(12) 0.0121(5) Uani 1 1 d . . . H13A H 0.7132(13) 0.4393(13) 0.9656(10) 0.015 Uiso 1 1 d . . . C1B C 0.63579(13) 0.56230(13) 0.66687(10) 0.0130(4) Uani 1 1 d . . . H1B H 0.5766(14) 0.6058(13) 0.6720(10) 0.016 Uiso 1 1 d . . . B2B B 0.65541(15) 0.47006(15) 0.68999(12) 0.0136(5) Uani 1 1 d . . . H2B H 0.6014(13) 0.4572(13) 0.7140(10) 0.016 Uiso 1 1 d . . . B3B B 0.70208(16) 0.59266(16) 0.63430(12) 0.0150(5) Uani 1 1 d . . . H3B H 0.6783(13) 0.6612(13) 0.6193(10) 0.018 Uiso 1 1 d . . . B5B B 0.68237(16) 0.50622(16) 0.58639(12) 0.0150(5) Uani 1 1 d . . . H5B H 0.6309(13) 0.5283(13) 0.5464(11) 0.018 Uiso 1 1 d . . . B6B B 0.76672(15) 0.39318(15) 0.70791(12) 0.0129(5) Uani 1 1 d . . . H6B H 0.7778(13) 0.3448(13) 0.7514(10) 0.016 Uiso 1 1 d . . . B7B B 0.81695(15) 0.52618(15) 0.65064(12) 0.0126(5) Uani 1 1 d . . . H7B H 0.8572(13) 0.5575(13) 0.6554(10) 0.015 Uiso 1 1 d . . . B8B B 0.78327(16) 0.52321(16) 0.56502(12) 0.0149(5) Uani 1 1 d . . . H8B H 0.7953(13) 0.5561(13) 0.5190(11) 0.018 Uiso 1 1 d . . . B9B B 0.73210(15) 0.38896(15) 0.62375(12) 0.0139(5) Uani 1 1 d . . . H9B H 0.7099(13) 0.3435(13) 0.6118(10) 0.017 Uiso 1 1 d . . . C10B C 0.84295(13) 0.42700(13) 0.68769(10) 0.0135(4) Uani 1 1 d . . . H10B H 0.8886(14) 0.4042(13) 0.7188(11) 0.016 Uiso 1 1 d . . . B11B B 0.79155(16) 0.41993(15) 0.55606(12) 0.0142(5) Uani 1 1 d . . . H11B H 0.7999(13) 0.3961(13) 0.5015(11) 0.017 Uiso 1 1 d . . . B12B B 0.84417(16) 0.35224(16) 0.63065(12) 0.0146(5) Uani 1 1 d . . . H12B H 0.8965(13) 0.2820(14) 0.6316(10) 0.017 Uiso 1 1 d . . . B13B B 0.87390(16) 0.43119(16) 0.59624(12) 0.0149(5) Uani 1 1 d . . . H13B H 0.9428(14) 0.4097(13) 0.5754(10) 0.018 Uiso 1 1 d . . . Fe4C Fe 0.724925(18) 1.025553(18) 0.243660(14) 0.00962(7) Uani 1 1 d . . . C1C C 0.64630(13) 1.15439(13) 0.27667(10) 0.0134(4) Uani 1 1 d . . . H1C H 0.6162(13) 1.2024(13) 0.2452(11) 0.016 Uiso 1 1 d . . . B2C B 0.74040(16) 1.13515(15) 0.28545(12) 0.0140(5) Uani 1 1 d . . . H2C H 0.7673(13) 1.1754(13) 0.2563(10) 0.017 Uiso 1 1 d . . . B3C B 0.59744(15) 1.10620(15) 0.31268(12) 0.0140(5) Uani 1 1 d . . . H3C H 0.5277(13) 1.1263(13) 0.2997(10) 0.017 Uiso 1 1 d . . . B5C B 0.64007(16) 1.16806(16) 0.36955(12) 0.0147(5) Uani 1 1 d . . . H5C H 0.6005(13) 1.2354(14) 0.3829(10) 0.018 Uiso 1 1 d . . . B6C B 0.81589(15) 1.02810(15) 0.31689(12) 0.0137(5) Uani 1 1 d . . . H6C H 0.8887(13) 0.9993(13) 0.2947(10) 0.016 Uiso 1 1 d . . . B7C B 0.66295(15) 0.99505(15) 0.34421(12) 0.0131(5) Uani 1 1 d . . . H7C H 0.6372(13) 0.9519(13) 0.3421(10) 0.016 Uiso 1 1 d . . . B8C B 0.60971(16) 1.08097(15) 0.40746(12) 0.0139(5) Uani 1 1 d . . . H8C H 0.5481(13) 1.0940(13) 0.4422(10) 0.017 Uiso 1 1 d . . . B9C B 0.76463(15) 1.11473(15) 0.38000(12) 0.0134(5) Uani 1 1 d . . . H9C H 0.7950(13) 1.1502(13) 0.3939(10) 0.016 Uiso 1 1 d . . . C10C C 0.77180(13) 0.96282(13) 0.34440(10) 0.0119(4) Uani 1 1 d . . . H10C H 0.8070(14) 0.9067(14) 0.3371(10) 0.014 Uiso 1 1 d . . . B11C B 0.69212(15) 1.09426(15) 0.44261(12) 0.0141(5) Uani 1 1 d . . . H11C H 0.6839(13) 1.1198(13) 0.4970(11) 0.017 Uiso 1 1 d . . . B12C B 0.79841(15) 1.00816(15) 0.41000(12) 0.0136(5) Uani 1 1 d . . . H12C H 0.8543(13) 0.9679(13) 0.4391(10) 0.016 Uiso 1 1 d . . . B13C B 0.70773(15) 0.98847(15) 0.42652(12) 0.0142(5) Uani 1 1 d . . . H13C H 0.7159(13) 0.9364(13) 0.4669(11) 0.017 Uiso 1 1 d . . . C1D C 0.63837(13) 1.06103(13) 0.16474(10) 0.0127(4) Uani 1 1 d . . . H1D H 0.5840(14) 1.1034(14) 0.1687(11) 0.015 Uiso 1 1 d . . . B2D B 0.65492(15) 0.96967(15) 0.18868(12) 0.0134(5) Uani 1 1 d . . . H2D H 0.5993(13) 0.9572(13) 0.2108(10) 0.016 Uiso 1 1 d . . . B3D B 0.70747(15) 1.08868(15) 0.13371(12) 0.0133(5) Uani 1 1 d . . . H3D H 0.6848(13) 1.1576(13) 0.1213(10) 0.016 Uiso 1 1 d . . . B5D B 0.68634(15) 1.00470(15) 0.08510(12) 0.0128(5) Uani 1 1 d . . . H5D H 0.6410(13) 1.0246(13) 0.0440(10) 0.015 Uiso 1 1 d . . . B6D B 0.76510(15) 0.89161(15) 0.20794(12) 0.0139(5) Uani 1 1 d . . . H6D H 0.7736(13) 0.8410(13) 0.2514(10) 0.017 Uiso 1 1 d . . . B7D B 0.82139(15) 1.02037(15) 0.15222(12) 0.0123(5) Uani 1 1 d . . . H7D H 0.8604(13) 1.0479(13) 0.1597(10) 0.015 Uiso 1 1 d . . . B8D B 0.78976(15) 1.01804(15) 0.06557(12) 0.0135(5) Uani 1 1 d . . . H8D H 0.8022(13) 1.0550(13) 0.0179(11) 0.016 Uiso 1 1 d . . . B9D B 0.73182(15) 0.88759(15) 0.12233(12) 0.0133(5) Uani 1 1 d . . . H9D H 0.7069(13) 0.8447(13) 0.1121(10) 0.016 Uiso 1 1 d . . . C10D C 0.84306(13) 0.92236(13) 0.18907(10) 0.0129(4) Uani 1 1 d . . . H10D H 0.8897(14) 0.8987(13) 0.2182(11) 0.015 Uiso 1 1 d . . . B11D B 0.79477(15) 0.91670(15) 0.05625(12) 0.0128(5) Uani 1 1 d . . . H11D H 0.8045(13) 0.8930(13) 0.0021(11) 0.015 Uiso 1 1 d . . . B12D B 0.84397(16) 0.84810(15) 0.13189(12) 0.0141(5) Uani 1 1 d . . . H12D H 0.8988(13) 0.7761(13) 0.1341(10) 0.017 Uiso 1 1 d . . . B13D B 0.87733(15) 0.92466(15) 0.09817(12) 0.0135(5) Uani 1 1 d . . . H13D H 0.9481(14) 0.8979(13) 0.0813(10) 0.016 Uiso 1 1 d . . . K1A K 0.78273(3) 0.46464(3) 1.08769(2) 0.01307(10) Uani 1 1 d . . . K1B K 0.27737(3) 0.95823(3) 0.09429(2) 0.01307(10) Uani 1 1 d . . . K1C K 0.72429(3) 0.54372(3) 0.39979(2) 0.01455(10) Uani 1 1 d . . . K1D K 0.78409(3) 0.96446(3) 0.59122(2) 0.01400(10) Uani 1 1 d . . . C11A C 0.77403(14) 0.25622(13) 1.09116(11) 0.0190(5) Uani 1 1 d . . . H11Z H 0.7846 0.2402 1.1427 0.023 Uiso 1 1 calc R . . H11Y H 0.7855 0.2033 1.0658 0.023 Uiso 1 1 calc R . . C12A C 0.92289(13) 0.22441(13) 1.06212(12) 0.0192(5) Uani 1 1 d . . . H12E H 0.9370 0.1710 1.0360 0.023 Uiso 1 1 calc R . . H12F H 0.9350 0.2078 1.1133 0.023 Uiso 1 1 calc R . . C13A C 0.97938(14) 0.26252(14) 1.02810(11) 0.0205(5) Uani 1 1 d . . . H13E H 1.0428 0.2166 1.0234 0.025 Uiso 1 1 calc R . . H13F H 0.9620 0.2860 0.9790 0.025 Uiso 1 1 calc R . . C14A C 1.02015(13) 0.37043(13) 1.04356(11) 0.0174(4) Uani 1 1 d . . . H14A H 1.0019 0.3975 0.9955 0.021 Uiso 1 1 calc R . . H14B H 1.0838 0.3251 1.0373 0.021 Uiso 1 1 calc R . . C15A C 1.00736(13) 0.43887(13) 1.09460(11) 0.0176(5) Uani 1 1 d . . . H15A H 1.0217 0.4127 1.1435 0.021 Uiso 1 1 calc R . . H15B H 1.0476 0.4630 1.0775 0.021 Uiso 1 1 calc R . . C16A C 0.90096(14) 0.57461(13) 1.14541(11) 0.0182(4) Uani 1 1 d . . . H16A H 0.9413 0.5989 1.1295 0.022 Uiso 1 1 calc R . . H16B H 0.9125 0.5504 1.1952 0.022 Uiso 1 1 calc R . . C17A C 0.80598(14) 0.64536(14) 1.14445(11) 0.0200(5) Uani 1 1 d . . . H17A H 0.7949 0.6956 1.1735 0.024 Uiso 1 1 calc R . . H17B H 0.7932 0.6663 1.0940 0.024 Uiso 1 1 calc R . . C18A C 0.65854(14) 0.67591(14) 1.18213(12) 0.0245(5) Uani 1 1 d . . . H18A H 0.6397 0.7043 1.1345 0.029 Uiso 1 1 calc R . . H18B H 0.6497 0.7215 1.2158 0.029 Uiso 1 1 calc R . . C19A C 0.60435(15) 0.63343(14) 1.21134(12) 0.0240(5) Uani 1 1 d . . . H19A H 0.6261 0.6014 1.2572 0.029 Uiso 1 1 calc R . . H19B H 0.5412 0.6787 1.2217 0.029 Uiso 1 1 calc R . . C20A C 0.55969(13) 0.53250(13) 1.18306(11) 0.0172(4) Uani 1 1 d . . . H20A H 0.4958 0.5769 1.1899 0.021 Uiso 1 1 calc R . . H20B H 0.5777 0.5016 1.2300 0.021 Uiso 1 1 calc R . . C21A C 0.57443(13) 0.46865(13) 1.12702(11) 0.0179(4) Uani 1 1 d . . . H21A H 0.5332 0.4445 1.1389 0.022 Uiso 1 1 calc R . . H21B H 0.5635 0.4980 1.0788 0.022 Uiso 1 1 calc R . . C22A C 0.67994(13) 0.32689(13) 1.08585(11) 0.0188(5) Uani 1 1 d . . . H22A H 0.6700 0.3446 1.0345 0.023 Uiso 1 1 calc R . . H22B H 0.6383 0.3053 1.1056 0.023 Uiso 1 1 calc R . . O1A O 0.66476(9) 0.39978(9) 1.12637(7) 0.0159(3) Uani 1 1 d . . . O2A O 0.83207(9) 0.28777(8) 1.05870(7) 0.0156(3) Uani 1 1 d . . . O3A O 0.96712(9) 0.33117(9) 1.07277(7) 0.0155(3) Uani 1 1 d . . . O4A O 0.91697(9) 0.50720(9) 1.09762(7) 0.0167(3) Uani 1 1 d . . . O5A O 0.74968(9) 0.61030(9) 1.17430(7) 0.0187(3) Uani 1 1 d . . . O6A O 0.61151(9) 0.57439(9) 1.15952(7) 0.0164(3) Uani 1 1 d . . . C11B C 0.51455(13) 0.86031(13) 0.04489(11) 0.0178(4) Uani 1 1 d . . . H11E H 0.4964 0.8856 -0.0036 0.021 Uiso 1 1 calc R . . H11F H 0.5774 0.8130 0.0390 0.021 Uiso 1 1 calc R . . C12B C 0.50520(13) 0.92987(13) 0.09318(11) 0.0182(5) Uani 1 1 d . . . H12G H 0.5213 0.9050 0.1422 0.022 Uiso 1 1 calc R . . H12H H 0.5456 0.9528 0.0732 0.022 Uiso 1 1 calc R . . C13B C 0.40018(14) 1.06686(13) 0.14403(11) 0.0195(5) Uani 1 1 d . . . H13G H 0.4421 1.0893 0.1280 0.023 Uiso 1 1 calc R . . H13H H 0.4103 1.0438 0.1943 0.023 Uiso 1 1 calc R . . C14B C 0.30642(14) 1.13900(14) 0.14139(12) 0.0215(5) Uani 1 1 d . . . H14C H 0.2961 1.1892 0.1702 0.026 Uiso 1 1 calc R . . H14D H 0.2954 1.1595 0.0906 0.026 Uiso 1 1 calc R . . C15B C 0.15681(14) 1.17446(14) 0.17416(13) 0.0277(5) Uani 1 1 d . . . H15C H 0.1403 1.1979 0.1249 0.033 Uiso 1 1 calc R . . H15D H 0.1485 1.2231 0.2040 0.033 Uiso 1 1 calc R . . C16B C 0.09928(15) 1.13778(15) 0.20726(13) 0.0283(6) Uani 1 1 d . . . H16C H 0.1184 1.1112 0.2553 0.034 Uiso 1 1 calc R . . H16D H 0.0367 1.1854 0.2145 0.034 Uiso 1 1 calc R . . C17B C 0.05207(14) 1.03509(14) 0.19198(11) 0.0204(5) Uani 1 1 d . . . H17C H -0.0116 1.0806 0.1967 0.024 Uiso 1 1 calc R . . H17D H 0.0691 1.0110 0.2410 0.024 Uiso 1 1 calc R . . C18B C 0.06551(13) 0.96368(14) 0.14441(12) 0.0215(5) Uani 1 1 d . . . H18C H 0.0241 0.9412 0.1624 0.026 Uiso 1 1 calc R . . H18D H 0.0536 0.9863 0.0942 0.026 Uiso 1 1 calc R . . C19B C 0.16991(14) 0.81935(14) 0.10995(11) 0.0202(5) Uani 1 1 d . . . H19C H 0.1572 0.8337 0.0587 0.024 Uiso 1 1 calc R . . H19D H 0.1300 0.7977 0.1339 0.024 Uiso 1 1 calc R . . C20B C 0.26506(14) 0.75043(13) 0.11378(11) 0.0192(5) Uani 1 1 d . . . H20C H 0.2784 0.7379 0.1650 0.023 Uiso 1 1 calc R . . H20D H 0.2762 0.6955 0.0920 0.023 Uiso 1 1 calc R . . C21B C 0.41236(13) 0.71944(13) 0.07626(11) 0.0193(5) Uani 1 1 d . . . H21C H 0.4254 0.6645 0.0533 0.023 Uiso 1 1 calc R . . H21D H 0.4273 0.7056 0.1271 0.023 Uiso 1 1 calc R . . C22B C 0.46711(14) 0.75620(14) 0.03617(11) 0.0206(5) Uani 1 1 d . . . H22C H 0.5303 0.7098 0.0291 0.025 Uiso 1 1 calc R . . H22D H 0.4460 0.7786 -0.0122 0.025 Uiso 1 1 calc R . . O1B O 0.45908(9) 0.82583(9) 0.07743(7) 0.0165(3) Uani 1 1 d . . . O2B O 0.41495(9) 0.99891(9) 0.09734(7) 0.0171(3) Uani 1 1 d . . . O3B O 0.24722(9) 1.10697(9) 0.17017(7) 0.0187(3) Uani 1 1 d . . . O4B O 0.10528(9) 1.07328(9) 0.16143(7) 0.0178(3) Uani 1 1 d . . . O5B O 0.15505(9) 0.89540(9) 0.14554(7) 0.0170(3) Uani 1 1 d . . . O6B O 0.32063(9) 0.78178(8) 0.07504(7) 0.0160(3) Uani 1 1 d . . . C11C C 0.71358(14) 0.35323(14) 0.34473(13) 0.0240(5) Uani 1 1 d . . . H11G H 0.6864 0.3226 0.3240 0.029 Uiso 1 1 calc R . . H11H H 0.7315 0.3269 0.3931 0.029 Uiso 1 1 calc R . . C12C C 0.79327(14) 0.34325(14) 0.29603(12) 0.0234(5) Uani 1 1 d . . . H12I H 0.8353 0.2803 0.2873 0.028 Uiso 1 1 calc R . . H12J H 0.7747 0.3727 0.2487 0.028 Uiso 1 1 calc R . . C13C C 0.91315(14) 0.37335(14) 0.28730(12) 0.0229(5) Uani 1 1 d . . . H13I H 0.8975 0.4017 0.2392 0.028 Uiso 1 1 calc R . . H13J H 0.9570 0.3105 0.2799 0.028 Uiso 1 1 calc R . . C14C C 0.95291(14) 0.41630(13) 0.32574(12) 0.0220(5) Uani 1 1 d . . . H14E H 0.9642 0.3913 0.3754 0.026 Uiso 1 1 calc R . . H14F H 1.0102 0.4060 0.2991 0.026 Uiso 1 1 calc R . . C15C C 0.92808(13) 0.55507(13) 0.35764(11) 0.0194(5) Uani 1 1 d . . . H15E H 0.9861 0.5412 0.3305 0.023 Uiso 1 1 calc R . . H15F H 0.9376 0.5386 0.4093 0.023 Uiso 1 1 calc R . . C16C C 0.86356(13) 0.65102(13) 0.35068(11) 0.0189(5) Uani 1 1 d . . . H16E H 0.8888 0.6860 0.3671 0.023 Uiso 1 1 calc R . . H16F H 0.8517 0.6667 0.2993 0.023 Uiso 1 1 calc R . . C17C C 0.71681(13) 0.75896(13) 0.38960(11) 0.0184(5) Uani 1 1 d . . . H17E H 0.6989 0.7739 0.3396 0.022 Uiso 1 1 calc R . . H17F H 0.7403 0.7972 0.4019 0.022 Uiso 1 1 calc R . . C18C C 0.63850(13) 0.77276(13) 0.44175(11) 0.0180(4) Uani 1 1 d . . . H18E H 0.6579 0.7517 0.4908 0.022 Uiso 1 1 calc R . . H18F H 0.5945 0.8361 0.4445 0.022 Uiso 1 1 calc R . . C19C C 0.52892(14) 0.72965(14) 0.46994(11) 0.0197(5) Uani 1 1 d . . . H19E H 0.4859 0.7916 0.4820 0.024 Uiso 1 1 calc R . . H19F H 0.5541 0.6981 0.5150 0.024 Uiso 1 1 calc R . . C20C C 0.48242(13) 0.68833(13) 0.43878(11) 0.0194(5) Uani 1 1 d . . . H20E H 0.4307 0.6951 0.4726 0.023 Uiso 1 1 calc R . . H20F H 0.4605 0.7175 0.3921 0.023 Uiso 1 1 calc R . . C21C C 0.50598(14) 0.55468(14) 0.39508(11) 0.0193(5) Uani 1 1 d . . . H21E H 0.4931 0.5777 0.3451 0.023 Uiso 1 1 calc R . . H21F H 0.4494 0.5653 0.4233 0.023 Uiso 1 1 calc R . . C22C C 0.57083(14) 0.45846(14) 0.39344(12) 0.0217(5) Uani 1 1 d . . . H22E H 0.5835 0.4355 0.4435 0.026 Uiso 1 1 calc R . . H22F H 0.5452 0.4269 0.3718 0.026 Uiso 1 1 calc R . . O1C O 0.65089(9) 0.44451(9) 0.35153(7) 0.0170(3) Uani 1 1 d . . . O2C O 0.83583(9) 0.38154(9) 0.32955(7) 0.0181(3) Uani 1 1 d . . . O3C O 0.89194(9) 0.50748(9) 0.32892(7) 0.0161(3) Uani 1 1 d . . . O4C O 0.78334(9) 0.66939(9) 0.39406(7) 0.0170(3) Uani 1 1 d . . . O5C O 0.59880(9) 0.72563(9) 0.41781(7) 0.0163(3) Uani 1 1 d . . . O6C O 0.54372(9) 0.59794(9) 0.42770(7) 0.0166(3) Uani 1 1 d . . . C11D C 0.59821(14) 1.12492(14) 0.71408(12) 0.0220(5) Uani 1 1 d . . . H11I H 0.5539 1.1864 0.7264 0.026 Uiso 1 1 calc R . . H11J H 0.6182 1.0915 0.7598 0.026 Uiso 1 1 calc R . . C12D C 0.55696(14) 1.08522(13) 0.67358(12) 0.0203(5) Uani 1 1 d . . . H12K H 0.5020 1.0911 0.7018 0.024 Uiso 1 1 calc R . . H12L H 0.5412 1.1156 0.6261 0.024 Uiso 1 1 calc R . . C13D C 0.58540(13) 0.95048(13) 0.62773(11) 0.0181(5) Uani 1 1 d . . . H13K H 0.5785 0.9703 0.5764 0.022 Uiso 1 1 calc R . . H13L H 0.5263 0.9632 0.6520 0.022 Uiso 1 1 calc R . . C14D C 0.64911(13) 0.85427(13) 0.63160(11) 0.0181(5) Uani 1 1 d . . . H14G H 0.6597 0.8353 0.6827 0.022 Uiso 1 1 calc R . . H14H H 0.6242 0.8210 0.6116 0.022 Uiso 1 1 calc R . . C15D C 0.79648(13) 0.74749(13) 0.59028(11) 0.0170(4) Uani 1 1 d . . . H15G H 0.7729 0.7116 0.5728 0.020 Uiso 1 1 calc R . . H15H H 0.8135 0.7274 0.6400 0.020 Uiso 1 1 calc R . . C16D C 0.87555(13) 0.73782(13) 0.54105(11) 0.0181(4) Uani 1 1 d . . . H16G H 0.9197 0.6748 0.5351 0.022 Uiso 1 1 calc R . . H16H H 0.8570 0.7633 0.4927 0.022 Uiso 1 1 calc R . . C17D C 0.99033(14) 0.77496(14) 0.52606(11) 0.0202(5) Uani 1 1 d . . . H17G H 0.9723 0.8033 0.4783 0.024 Uiso 1 1 calc R . . H17H H 1.0348 0.7124 0.5181 0.024 Uiso 1 1 calc R . . C18D C 1.02997(13) 0.81899(13) 0.56230(12) 0.0203(5) Uani 1 1 d . . . H18G H 1.0433 0.7939 0.6117 0.024 Uiso 1 1 calc R . . H18H H 1.0863 0.8094 0.5343 0.024 Uiso 1 1 calc R . . C19D C 1.00192(14) 0.95699(14) 0.60027(11) 0.0206(5) Uani 1 1 d . . . H19G H 1.0579 0.9491 0.5726 0.025 Uiso 1 1 calc R . . H19H H 1.0151 0.9337 0.6501 0.025 Uiso 1 1 calc R . . C20D C 0.93436(14) 1.05205(14) 0.60280(12) 0.0225(5) Uani 1 1 d . . . H20G H 0.9584 1.0852 0.6242 0.027 Uiso 1 1 calc R . . H20H H 0.9204 1.0751 0.5530 0.027 Uiso 1 1 calc R . . C21D C 0.79168(14) 1.15392(13) 0.65301(12) 0.0219(5) Uani 1 1 d . . . H21G H 0.7725 1.1804 0.6050 0.026 Uiso 1 1 calc R . . H21H H 0.8183 1.1854 0.6734 0.026 Uiso 1 1 calc R . . C22D C 0.71344(14) 1.16189(14) 0.70264(11) 0.0217(5) Uani 1 1 d . . . H22G H 0.7333 1.1322 0.7496 0.026 Uiso 1 1 calc R . . H22H H 0.6704 1.2245 0.7119 0.026 Uiso 1 1 calc R . . O1D O 0.67185(9) 1.12236(9) 0.66960(7) 0.0169(3) Uani 1 1 d . . . O2D O 0.62008(9) 0.99542(9) 0.66317(7) 0.0159(3) Uani 1 1 d . . . O3D O 0.73041(9) 0.83803(9) 0.59042(7) 0.0164(3) Uani 1 1 d . . . O4D O 0.91466(9) 0.78180(9) 0.57116(7) 0.0167(3) Uani 1 1 d . . . O5D O 0.96814(9) 0.91058(9) 0.56633(7) 0.0169(3) Uani 1 1 d . . . O6D O 0.85568(9) 1.06321(9) 0.64538(7) 0.0169(3) 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 Fe4A 0.01103(15) 0.01086(16) 0.00991(13) -0.00109(11) -0.00058(11) -0.00618(13) C1A 0.0136(10) 0.0076(10) 0.0126(9) -0.0011(8) -0.0015(8) -0.0025(9) B2A 0.0151(12) 0.0120(12) 0.0119(10) -0.0017(9) -0.0011(9) -0.0061(10) B3A 0.0151(12) 0.0146(12) 0.0112(10) -0.0035(9) -0.0007(9) -0.0065(11) B5A 0.0130(12) 0.0127(13) 0.0134(11) -0.0025(9) 0.0008(9) -0.0067(10) B6A 0.0132(12) 0.0121(12) 0.0119(10) -0.0006(9) -0.0027(9) -0.0053(10) B7A 0.0125(11) 0.0127(12) 0.0108(10) -0.0004(9) -0.0011(9) -0.0077(10) B8A 0.0118(12) 0.0167(13) 0.0127(11) -0.0024(9) 0.0013(9) -0.0084(11) B9A 0.0137(12) 0.0140(13) 0.0136(11) -0.0018(9) -0.0007(9) -0.0080(11) C10A 0.0107(10) 0.0109(11) 0.0120(9) -0.0005(8) -0.0014(8) -0.0038(9) B11A 0.0157(12) 0.0132(12) 0.0107(11) -0.0007(9) -0.0005(9) -0.0084(10) B12A 0.0128(12) 0.0145(13) 0.0143(11) -0.0006(9) -0.0017(9) -0.0081(11) B13A 0.0133(12) 0.0138(12) 0.0111(10) -0.0003(9) -0.0007(9) -0.0081(10) C1B 0.0106(10) 0.0153(11) 0.0122(9) -0.0028(8) -0.0036(8) -0.0049(9) B2B 0.0140(12) 0.0161(13) 0.0115(11) -0.0027(9) -0.0012(9) -0.0076(11) B3B 0.0184(12) 0.0153(13) 0.0127(11) -0.0005(9) -0.0031(10) -0.0090(11) B5B 0.0169(12) 0.0168(13) 0.0152(11) -0.0006(9) -0.0035(10) -0.0107(11) B6B 0.0132(12) 0.0126(12) 0.0124(11) -0.0026(9) -0.0005(9) -0.0058(10) B7B 0.0132(12) 0.0154(13) 0.0115(10) -0.0018(9) 0.0017(9) -0.0091(11) B8B 0.0190(13) 0.0167(13) 0.0116(11) -0.0002(9) -0.0008(10) -0.0109(11) B9B 0.0160(12) 0.0128(12) 0.0153(11) -0.0018(9) 0.0002(10) -0.0090(11) C10B 0.0150(11) 0.0138(11) 0.0130(9) -0.0004(8) -0.0038(8) -0.0075(9) B11B 0.0169(12) 0.0151(13) 0.0125(11) -0.0022(9) -0.0009(10) -0.0092(11) B12B 0.0184(12) 0.0145(13) 0.0119(11) -0.0020(9) -0.0009(10) -0.0087(11) B13B 0.0149(12) 0.0187(13) 0.0125(11) -0.0045(9) 0.0028(10) -0.0096(11) Fe4C 0.00960(15) 0.00972(15) 0.00973(13) -0.00108(10) -0.00040(11) -0.00486(13) C1C 0.0163(11) 0.0085(10) 0.0106(9) -0.0021(8) 0.0000(8) -0.0025(9) B2C 0.0178(12) 0.0113(12) 0.0144(11) -0.0031(9) 0.0007(10) -0.0082(11) B3C 0.0122(12) 0.0119(12) 0.0144(11) -0.0021(9) 0.0010(9) -0.0035(10) B5C 0.0160(12) 0.0137(13) 0.0149(11) -0.0025(9) 0.0001(10) -0.0076(11) B6C 0.0143(12) 0.0141(12) 0.0137(11) -0.0023(9) -0.0022(9) -0.0072(11) B7C 0.0134(12) 0.0142(12) 0.0113(11) -0.0011(9) 0.0010(9) -0.0068(11) B8C 0.0143(12) 0.0146(13) 0.0130(11) -0.0017(9) 0.0009(10) -0.0076(11) B9C 0.0131(12) 0.0157(13) 0.0143(11) -0.0019(9) -0.0017(9) -0.0090(11) C10C 0.0118(10) 0.0091(10) 0.0126(9) -0.0008(8) -0.0025(8) -0.0029(9) B11C 0.0156(12) 0.0152(13) 0.0132(11) -0.0015(9) -0.0008(10) -0.0087(11) B12C 0.0137(12) 0.0157(13) 0.0113(11) -0.0025(9) -0.0022(9) -0.0066(11) B13C 0.0160(12) 0.0137(13) 0.0126(11) -0.0012(9) 0.0007(10) -0.0074(11) C1D 0.0099(10) 0.0133(11) 0.0120(9) -0.0018(8) -0.0023(8) -0.0030(9) B2D 0.0127(12) 0.0149(13) 0.0136(11) -0.0020(9) -0.0016(9) -0.0073(10) B3D 0.0152(12) 0.0123(12) 0.0126(11) -0.0001(9) -0.0036(9) -0.0064(10) B5D 0.0128(12) 0.0134(12) 0.0131(11) -0.0012(9) -0.0011(9) -0.0070(10) B6D 0.0138(12) 0.0105(12) 0.0163(11) -0.0010(9) -0.0027(10) -0.0046(10) B7D 0.0129(12) 0.0144(12) 0.0119(11) -0.0008(9) -0.0010(9) -0.0083(10) B8D 0.0135(12) 0.0169(13) 0.0126(11) -0.0014(9) 0.0006(9) -0.0097(11) B9D 0.0156(12) 0.0126(12) 0.0130(11) -0.0021(9) -0.0024(10) -0.0074(11) C10D 0.0117(10) 0.0127(11) 0.0129(9) -0.0008(8) -0.0026(8) -0.0045(9) B11D 0.0123(12) 0.0151(13) 0.0111(11) -0.0032(9) 0.0013(9) -0.0069(10) B12D 0.0156(12) 0.0133(13) 0.0130(11) -0.0030(9) -0.0009(9) -0.0063(11) B13D 0.0124(12) 0.0161(13) 0.0119(11) -0.0032(9) -0.0003(9) -0.0068(11) K1A 0.0127(2) 0.0135(2) 0.0135(2) -0.00081(17) -0.00099(17) -0.0068(2) K1B 0.0128(2) 0.0124(2) 0.0138(2) -0.00172(17) -0.00085(17) -0.00590(19) K1C 0.0135(2) 0.0130(2) 0.0171(2) -0.00265(17) -0.00246(18) -0.0059(2) K1D 0.0122(2) 0.0136(2) 0.0162(2) -0.00210(17) -0.00015(18) -0.0064(2) C11A 0.0245(12) 0.0151(11) 0.0205(11) 0.0013(9) 0.0023(9) -0.0131(10) C12A 0.0147(11) 0.0095(11) 0.0292(11) -0.0040(9) -0.0034(9) -0.0019(9) C13A 0.0152(11) 0.0185(12) 0.0238(11) -0.0099(9) 0.0013(9) -0.0045(10) C14A 0.0111(10) 0.0187(12) 0.0200(10) 0.0015(9) 0.0008(8) -0.0060(9) C15A 0.0119(11) 0.0188(12) 0.0242(11) 0.0032(9) -0.0035(9) -0.0091(10) C16A 0.0211(11) 0.0196(12) 0.0201(10) -0.0007(9) -0.0021(9) -0.0145(10) C17A 0.0267(12) 0.0164(12) 0.0217(11) 0.0007(9) -0.0054(9) -0.0136(10) C18A 0.0188(12) 0.0139(12) 0.0360(13) -0.0094(10) -0.0034(10) -0.0029(10) C19A 0.0178(12) 0.0218(13) 0.0276(12) -0.0136(10) 0.0016(10) -0.0051(10) C20A 0.0113(10) 0.0151(11) 0.0193(10) 0.0021(8) 0.0024(8) -0.0030(9) C21A 0.0116(10) 0.0172(12) 0.0232(11) 0.0015(9) -0.0011(9) -0.0060(9) C22A 0.0188(11) 0.0172(12) 0.0246(11) -0.0032(9) 0.0007(9) -0.0122(10) O1A 0.0125(7) 0.0130(8) 0.0216(7) -0.0034(6) -0.0009(6) -0.0056(6) O2A 0.0126(7) 0.0117(7) 0.0212(7) 0.0012(6) -0.0003(6) -0.0053(6) O3A 0.0135(7) 0.0158(8) 0.0179(7) -0.0042(6) 0.0028(6) -0.0080(6) O4A 0.0141(7) 0.0154(8) 0.0216(7) -0.0024(6) -0.0033(6) -0.0072(6) O5A 0.0138(7) 0.0142(8) 0.0263(8) -0.0015(6) -0.0019(6) -0.0052(7) O6A 0.0160(7) 0.0152(8) 0.0178(7) -0.0053(6) 0.0027(6) -0.0077(6) C11B 0.0130(11) 0.0199(12) 0.0184(10) 0.0014(9) -0.0016(9) -0.0066(10) C12B 0.0142(11) 0.0193(12) 0.0222(11) 0.0022(9) -0.0050(9) -0.0087(10) C13B 0.0240(12) 0.0200(12) 0.0214(11) -0.0020(9) -0.0034(9) -0.0156(10) C14B 0.0260(12) 0.0157(12) 0.0265(11) -0.0005(9) -0.0031(10) -0.0130(11) C15B 0.0210(12) 0.0149(12) 0.0419(14) -0.0113(10) -0.0051(11) -0.0028(10) C16B 0.0187(12) 0.0283(14) 0.0332(13) -0.0178(10) 0.0018(10) -0.0064(11) C17B 0.0127(11) 0.0215(12) 0.0204(11) 0.0000(9) 0.0024(9) -0.0043(10) C18B 0.0136(11) 0.0226(12) 0.0278(12) 0.0005(9) -0.0040(9) -0.0082(10) C19B 0.0225(12) 0.0208(12) 0.0237(11) -0.0067(9) 0.0031(9) -0.0157(10) C20B 0.0249(12) 0.0129(11) 0.0222(11) -0.0008(8) 0.0016(9) -0.0118(10) C21B 0.0160(11) 0.0103(11) 0.0276(11) -0.0041(9) -0.0068(9) -0.0020(9) C22B 0.0160(11) 0.0183(12) 0.0258(11) -0.0112(9) -0.0005(9) -0.0059(10) O1B 0.0153(7) 0.0175(8) 0.0174(7) -0.0057(6) 0.0019(6) -0.0085(6) O2B 0.0139(7) 0.0152(8) 0.0224(7) -0.0048(6) -0.0029(6) -0.0063(6) O3B 0.0155(8) 0.0124(8) 0.0264(8) -0.0027(6) -0.0028(6) -0.0050(7) O4B 0.0158(8) 0.0192(8) 0.0173(7) -0.0069(6) 0.0012(6) -0.0075(7) O5B 0.0117(7) 0.0155(8) 0.0231(7) -0.0049(6) -0.0003(6) -0.0060(6) O6B 0.0136(7) 0.0110(7) 0.0211(7) 0.0011(6) 0.0002(6) -0.0048(6) C11C 0.0228(12) 0.0119(12) 0.0376(13) -0.0051(9) -0.0016(10) -0.0082(10) C12C 0.0239(12) 0.0179(12) 0.0297(12) -0.0104(9) -0.0023(10) -0.0099(10) C13C 0.0197(12) 0.0167(12) 0.0296(12) -0.0096(9) 0.0061(10) -0.0074(10) C14C 0.0134(11) 0.0132(12) 0.0337(12) -0.0038(9) 0.0014(9) -0.0026(10) C15C 0.0149(11) 0.0210(12) 0.0236(11) -0.0071(9) 0.0001(9) -0.0094(10) C16C 0.0185(11) 0.0195(12) 0.0225(11) -0.0026(9) 0.0009(9) -0.0125(10) C17C 0.0184(11) 0.0141(11) 0.0235(11) 0.0002(9) -0.0059(9) -0.0078(10) C18C 0.0190(11) 0.0122(11) 0.0215(10) -0.0047(8) -0.0034(9) -0.0058(9) C19C 0.0186(11) 0.0169(12) 0.0199(11) -0.0047(9) 0.0041(9) -0.0065(10) C20C 0.0121(11) 0.0158(12) 0.0248(11) -0.0016(9) -0.0007(9) -0.0027(10) C21C 0.0172(11) 0.0273(13) 0.0193(10) -0.0053(9) 0.0004(9) -0.0153(10) C22C 0.0213(12) 0.0252(13) 0.0235(11) -0.0056(9) 0.0057(9) -0.0160(11) O1C 0.0162(8) 0.0156(8) 0.0201(7) -0.0024(6) 0.0004(6) -0.0086(7) O2C 0.0189(8) 0.0160(8) 0.0202(7) -0.0067(6) 0.0021(6) -0.0091(7) O3C 0.0131(7) 0.0129(8) 0.0212(7) -0.0024(6) -0.0032(6) -0.0050(6) O4C 0.0142(7) 0.0124(8) 0.0209(7) -0.0004(6) 0.0025(6) -0.0048(6) O5C 0.0159(7) 0.0154(8) 0.0183(7) -0.0050(6) 0.0010(6) -0.0081(6) O6C 0.0139(7) 0.0145(8) 0.0209(7) -0.0035(6) -0.0044(6) -0.0055(6) C11D 0.0180(12) 0.0182(12) 0.0257(12) -0.0090(9) 0.0086(10) -0.0069(10) C12D 0.0134(11) 0.0129(11) 0.0299(12) -0.0021(9) 0.0030(9) -0.0036(10) C13D 0.0143(11) 0.0197(12) 0.0236(11) -0.0047(9) 0.0003(9) -0.0106(10) C14D 0.0165(11) 0.0188(12) 0.0216(11) -0.0038(9) 0.0026(9) -0.0110(10) C15D 0.0156(11) 0.0108(11) 0.0240(11) -0.0009(8) -0.0020(9) -0.0059(9) C16D 0.0177(11) 0.0140(11) 0.0219(11) -0.0047(8) -0.0034(9) -0.0063(10) C17D 0.0161(11) 0.0170(12) 0.0235(11) -0.0020(9) 0.0066(9) -0.0066(10) C18D 0.0107(11) 0.0152(12) 0.0283(12) 0.0026(9) 0.0019(9) -0.0024(10) C19D 0.0160(11) 0.0298(13) 0.0208(11) -0.0054(9) 0.0019(9) -0.0150(10) C20D 0.0232(12) 0.0271(13) 0.0246(11) -0.0046(9) 0.0042(10) -0.0187(11) C21D 0.0225(12) 0.0140(12) 0.0314(12) -0.0025(9) -0.0041(10) -0.0100(10) C22D 0.0240(12) 0.0167(12) 0.0245(11) -0.0086(9) -0.0031(10) -0.0089(10) O1D 0.0169(8) 0.0170(8) 0.0189(7) -0.0047(6) 0.0015(6) -0.0100(7) O2D 0.0140(7) 0.0119(7) 0.0202(7) -0.0028(6) -0.0015(6) -0.0049(6) O3D 0.0123(7) 0.0122(8) 0.0227(7) -0.0002(6) 0.0027(6) -0.0054(6) O4D 0.0141(7) 0.0174(8) 0.0195(7) -0.0050(6) 0.0033(6) -0.0090(7) O5D 0.0128(7) 0.0161(8) 0.0219(7) -0.0016(6) -0.0026(6) -0.0067(7) O6D 0.0159(8) 0.0158(8) 0.0205(7) -0.0001(6) -0.0002(6) -0.0092(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 Fe4A C1B 2.0679(19) . ? Fe4A C1A 2.0772(19) . ? Fe4A C10A 2.1350(19) . ? Fe4A C10B 2.149(2) . ? Fe4A B7A 2.203(2) . ? Fe4A B7B 2.204(2) . ? Fe4A B6A 2.223(2) . ? Fe4A B6B 2.231(2) . ? Fe4A B3B 2.236(2) . ? Fe4A B3A 2.248(2) . ? Fe4A B2B 2.260(2) . ? Fe4A B2A 2.267(2) . ? C1A B2A 1.530(3) . ? C1A B3A 1.536(3) . ? C1A B5A 1.738(3) . ? C1A H1A 0.96(2) . ? B2A B6A 1.781(3) . ? B2A B9A 1.813(3) . ? B2A B5A 2.060(3) . ? B2A H2A 1.124(19) . ? B3A B8A 1.793(3) . ? B3A B7A 1.800(3) . ? B3A B5A 2.001(3) . ? B3A H3A 1.09(2) . ? B5A B11A 1.801(3) . ? B5A B8A 1.903(3) . ? B5A B9A 1.920(3) . ? B5A H5A 1.08(2) . ? B6A C10A 1.687(3) . ? B6A B12A 1.764(3) . ? B6A B9A 1.769(3) . ? B6A H6A 1.100(19) . ? B7A C10A 1.685(3) . ? B7A B13A 1.762(3) . ? B7A B8A 1.769(3) . ? B7A H7A 1.039(19) . ? B8A B13A 1.724(3) . ? B8A B11A 1.761(3) . ? B8A H8A 1.03(2) . ? B9A B12A 1.730(3) . ? B9A B11A 1.758(3) . ? B9A H9A 1.10(2) . ? C10A B13A 1.721(3) . ? C10A B12A 1.723(3) . ? C10A H10A 0.93(2) . ? B11A B12A 1.777(3) . ? B11A B13A 1.778(3) . ? B11A K1A 3.386(2) . ? B11A H11A 1.094(19) . ? B12A B13A 1.759(3) . ? B12A K1A 3.357(2) . ? B12A H12A 1.12(2) . ? B13A K1A 3.304(2) . ? B13A H13A 1.099(19) . ? C1B B2B 1.517(3) . ? C1B B3B 1.534(3) . ? C1B B5B 1.729(3) . ? C1B H1B 0.93(2) . ? B2B B6B 1.783(3) . ? B2B B9B 1.815(3) . ? B2B B5B 2.053(3) . ? B2B H2B 1.104(19) . ? B3B B8B 1.794(3) . ? B3B B7B 1.796(3) . ? B3B B5B 1.994(3) . ? B3B H3B 1.09(2) . ? B5B B11B 1.798(3) . ? B5B B8B 1.905(3) . ? B5B B9B 1.906(3) . ? B5B K1C 3.534(2) . ? B5B H5B 1.13(2) . ? B6B C10B 1.689(3) . ? B6B B9B 1.759(3) . ? B6B B12B 1.763(3) . ? B6B H6B 1.088(19) . ? B7B C10B 1.680(3) . ? B7B B8B 1.771(3) . ? B7B B13B 1.774(3) . ? B7B H7B 1.092(19) . ? B8B B13B 1.730(3) . ? B8B B11B 1.760(3) . ? B8B K1C 3.290(2) . ? B8B H8B 1.05(2) . ? B9B B12B 1.738(3) . ? B9B B11B 1.752(3) . ? B9B H9B 1.09(2) . ? C10B B13B 1.725(3) . ? C10B B12B 1.733(3) . ? C10B H10B 0.94(2) . ? B11B B12B 1.777(3) . ? B11B B13B 1.785(3) . ? B11B K1C 3.448(2) . ? B11B H11B 1.09(2) . ? B12B B13B 1.753(3) . ? B12B H12B 1.11(2) . ? B13B H13B 1.09(2) . ? Fe4C C1D 2.0655(19) . ? Fe4C C1C 2.0721(19) . ? Fe4C C10C 2.1343(19) . ? Fe4C C10D 2.146(2) . ? Fe4C B7C 2.203(2) . ? Fe4C B7D 2.206(2) . ? Fe4C B6D 2.220(2) . ? Fe4C B6C 2.221(2) . ? Fe4C B3D 2.230(2) . ? Fe4C B3C 2.241(2) . ? Fe4C B2D 2.254(2) . ? Fe4C B2C 2.264(2) . ? C1C B2C 1.521(3) . ? C1C B3C 1.535(3) . ? C1C B5C 1.741(3) . ? C1C H1C 0.94(2) . ? B2C B6C 1.782(3) . ? B2C B9C 1.824(3) . ? B2C B5C 2.069(3) . ? B2C H2C 1.10(2) . ? B3C B8C 1.795(3) . ? B3C B7C 1.800(3) . ? B3C B5C 1.994(3) . ? B3C H3C 1.13(2) . ? B5C B11C 1.794(3) . ? B5C B8C 1.907(3) . ? B5C B9C 1.913(3) . ? B5C H5C 1.06(2) . ? B6C C10C 1.682(3) . ? B6C B12C 1.758(3) . ? B6C B9C 1.773(3) . ? B6C H6C 1.14(2) . ? B7C C10C 1.682(3) . ? B7C B8C 1.767(3) . ? B7C B13C 1.768(3) . ? B7C H7C 1.05(2) . ? B8C B13C 1.729(3) . ? B8C B11C 1.759(3) . ? B8C H8C 1.106(19) . ? B9C B12C 1.728(3) . ? B9C B11C 1.756(3) . ? B9C H9C 1.05(2) . ? C10C B13C 1.720(3) . ? C10C B12C 1.721(3) . ? C10C H10C 0.88(2) . ? B11C B13C 1.777(3) . ? B11C B12C 1.778(3) . ? B11C K1D 3.450(2) . ? B11C H11C 1.10(2) . ? B12C B13C 1.755(3) . ? B12C K1D 3.402(2) . ? B12C H12C 1.06(2) . ? B13C K1D 3.395(2) . ? B13C H13C 1.10(2) . ? C1D B2D 1.521(3) . ? C1D B3D 1.537(3) . ? C1D B5D 1.720(3) . ? C1D H1D 0.86(2) . ? B2D B6D 1.780(3) . ? B2D B9D 1.826(3) . ? B2D B5D 2.067(3) . ? B2D H2D 1.115(19) . ? B3D B8D 1.794(3) . ? B3D B7D 1.796(3) . ? B3D B5D 1.978(3) . ? B3D H3D 1.09(2) . ? B5D B11D 1.794(3) . ? B5D B9D 1.907(3) . ? B5D B8D 1.907(3) . ? B5D K1B 3.389(2) 2_675 ? B5D H5D 1.08(2) . ? B6D C10D 1.676(3) . ? B6D B12D 1.762(3) . ? B6D B9D 1.773(3) . ? B6D H6D 1.120(19) . ? B7D C10D 1.676(3) . ? B7D B8D 1.771(3) . ? B7D B13D 1.779(3) . ? B7D H7D 1.03(2) . ? B8D B13D 1.726(3) . ? B8D B11D 1.753(3) . ? B8D K1B 3.243(2) 2_675 ? B8D H8D 1.121(19) . ? B9D B12D 1.741(3) . ? B9D B11D 1.756(3) . ? B9D H9D 1.07(2) . ? C10D B13D 1.724(3) . ? C10D B12D 1.730(3) . ? C10D H10D 0.93(2) . ? B11D B13D 1.776(3) . ? B11D B12D 1.783(3) . ? B11D K1B 3.381(2) 2_675 ? B11D H11D 1.079(19) . ? B12D B13D 1.753(3) . ? B12D H12D 1.15(2) . ? B13D H13D 1.09(2) . ? K1A O1A 2.7909(14) . ? K1A O4A 2.7975(14) . ? K1A O6A 2.8421(14) . ? K1A O2A 2.8514(14) . ? K1A O3A 2.8774(14) . ? K1A O5A 2.8898(15) . ? K1A H11A 2.913(19) . ? K1A H12A 2.933(19) . ? K1A H13A 2.850(19) . ? K1B O2B 2.8107(14) . ? K1B O6B 2.8363(14) . ? K1B O3B 2.8378(14) . ? K1B O4B 2.8385(14) . ? K1B O1B 2.8409(15) . ? K1B O5B 2.8733(14) . ? K1B B8D 3.243(2) 2_675 ? K1B B11D 3.381(2) 2_675 ? K1B B5D 3.389(2) 2_675 ? K1C O6C 2.7776(14) . ? K1C O3C 2.8201(14) . ? K1C O2C 2.8327(14) . ? K1C O4C 2.8369(14) . ? K1C O1C 2.8478(14) . ? K1C O5C 2.8540(14) . ? K1C C19C 3.530(2) . ? K1C H5B 3.059(19) . ? K1C H8B 2.73(2) . ? K1C H11B 2.918(19) . ? K1D O3D 2.7916(14) . ? K1D O2D 2.7970(14) . ? K1D O5D 2.8320(14) . ? K1D O1D 2.8548(14) . ? K1D O6D 2.8638(14) . ? K1D O4D 2.8864(15) . ? K1D H11C 2.977(19) . ? K1D H12C 2.945(19) . ? K1D H13C 2.89(2) . ? C11A O2A 1.425(2) . ? C11A C22A 1.495(3) . ? C11A H11Z 0.9900 . ? C11A H11Y 0.9900 . ? C12A O2A 1.417(2) . ? C12A C13A 1.494(3) . ? C12A H12E 0.9900 . ? C12A H12F 0.9900 . ? C13A O3A 1.424(2) . ? C13A H13E 0.9900 . ? C13A H13F 0.9900 . ? C14A O3A 1.434(2) . ? C14A C15A 1.495(3) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A O4A 1.426(2) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A O4A 1.424(2) . ? C16A C17A 1.497(3) . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C17A O5A 1.429(2) . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? C18A O5A 1.421(2) . ? C18A C19A 1.494(3) . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? C19A O6A 1.414(2) . ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? C20A O6A 1.428(2) . ? C20A C21A 1.490(3) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? C21A O1A 1.430(2) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? C22A O1A 1.423(2) . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C11B O1B 1.424(2) . ? C11B C12B 1.497(3) . ? C11B H11E 0.9900 . ? C11B H11F 0.9900 . ? C12B O2B 1.427(2) . ? C12B H12G 0.9900 . ? C12B H12H 0.9900 . ? C13B O2B 1.424(2) . ? C13B C14B 1.493(3) . ? C13B H13G 0.9900 . ? C13B H13H 0.9900 . ? C14B O3B 1.429(2) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B O3B 1.421(3) . ? C15B C16B 1.486(3) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B O4B 1.419(2) . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? C17B O4B 1.429(2) . ? C17B C18B 1.490(3) . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C18B O5B 1.420(2) . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? C19B O5B 1.423(2) . ? C19B C20B 1.496(3) . ? C19B H19C 0.9900 . ? C19B H19D 0.9900 . ? C20B O6B 1.428(2) . ? C20B H20C 0.9900 . ? C20B H20D 0.9900 . ? C21B O6B 1.420(2) . ? C21B C22B 1.492(3) . ? C21B H21C 0.9900 . ? C21B H21D 0.9900 . ? C22B O1B 1.426(2) . ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? C11C O1C 1.427(2) . ? C11C C12C 1.496(3) . ? C11C H11G 0.9900 . ? C11C H11H 0.9900 . ? C12C O2C 1.428(2) . ? C12C H12I 0.9900 . ? C12C H12J 0.9900 . ? C13C O2C 1.415(2) . ? C13C C14C 1.502(3) . ? C13C H13I 0.9900 . ? C13C H13J 0.9900 . ? C14C O3C 1.416(2) . ? C14C H14E 0.9900 . ? C14C H14F 0.9900 . ? C15C O3C 1.424(2) . ? C15C C16C 1.498(3) . ? C15C H15E 0.9900 . ? C15C H15F 0.9900 . ? C16C O4C 1.418(2) . ? C16C H16E 0.9900 . ? C16C H16F 0.9900 . ? C17C O4C 1.421(2) . ? C17C C18C 1.493(3) . ? C17C H17E 0.9900 . ? C17C H17F 0.9900 . ? C18C O5C 1.427(2) . ? C18C H18E 0.9900 . ? C18C H18F 0.9900 . ? C19C O5C 1.431(2) . ? C19C C20C 1.501(3) . ? C19C H19E 0.9900 . ? C19C H19F 0.9900 . ? C20C O6C 1.419(2) . ? C20C H20E 0.9900 . ? C20C H20F 0.9900 . ? C21C O6C 1.420(2) . ? C21C C22C 1.496(3) . ? C21C H21E 0.9900 . ? C21C H21F 0.9900 . ? C22C O1C 1.422(2) . ? C22C H22E 0.9900 . ? C22C H22F 0.9900 . ? C11D O1D 1.416(2) . ? C11D C12D 1.501(3) . ? C11D H11I 0.9900 . ? C11D H11J 0.9900 . ? C12D O2D 1.416(2) . ? C12D H12K 0.9900 . ? C12D H12L 0.9900 . ? C13D O2D 1.431(2) . ? C13D C14D 1.494(3) . ? C13D H13K 0.9900 . ? C13D H13L 0.9900 . ? C14D O3D 1.423(2) . ? C14D H14G 0.9900 . ? C14D H14H 0.9900 . ? C15D O3D 1.427(2) . ? C15D C16D 1.494(3) . ? C15D H15G 0.9900 . ? C15D H15H 0.9900 . ? C16D O4D 1.425(2) . ? C16D H16G 0.9900 . ? C16D H16H 0.9900 . ? C17D O4D 1.424(2) . ? C17D C18D 1.492(3) . ? C17D H17G 0.9900 . ? C17D H17H 0.9900 . ? C18D O5D 1.425(2) . ? C18D H18G 0.9900 . ? C18D H18H 0.9900 . ? C19D O5D 1.425(2) . ? C19D C20D 1.491(3) . ? C19D H19G 0.9900 . ? C19D H19H 0.9900 . ? C20D O6D 1.421(2) . ? C20D H20G 0.9900 . ? C20D H20H 0.9900 . ? C21D O6D 1.426(2) . ? C21D C22D 1.495(3) . ? C21D H21G 0.9900 . ? C21D H21H 0.9900 . ? C22D O1D 1.426(2) . ? C22D H22G 0.9900 . ? C22D H22H 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1B Fe4A C1A 85.71(8) . . ? C1B Fe4A C10A 149.85(8) . . ? C1A Fe4A C10A 100.36(8) . . ? C1B Fe4A C10B 100.30(8) . . ? C1A Fe4A C10B 150.27(7) . . ? C10A Fe4A C10B 88.99(7) . . ? C1B Fe4A B7A 106.76(8) . . ? C1A Fe4A B7A 83.96(8) . . ? C10A Fe4A B7A 45.69(8) . . ? C10B Fe4A B7A 121.03(8) . . ? C1B Fe4A B7B 84.06(8) . . ? C1A Fe4A B7B 107.46(8) . . ? C10A Fe4A B7B 121.07(8) . . ? C10B Fe4A B7B 45.38(8) . . ? B7A Fe4A B7B 165.12(9) . . ? C1B Fe4A B6A 163.00(8) . . ? C1A Fe4A B6A 82.41(8) . . ? C10A Fe4A B6A 45.49(8) . . ? C10B Fe4A B6A 84.43(8) . . ? B7A Fe4A B6A 84.09(8) . . ? B7B Fe4A B6A 87.94(8) . . ? C1B Fe4A B6B 82.03(8) . . ? C1A Fe4A B6B 162.67(8) . . ? C10A Fe4A B6B 84.57(8) . . ? C10B Fe4A B6B 45.31(8) . . ? B7A Fe4A B6B 87.90(8) . . ? B7B Fe4A B6B 83.46(8) . . ? B6A Fe4A B6B 111.98(8) . . ? C1B Fe4A B3B 41.52(8) . . ? C1A Fe4A B3B 81.93(8) . . ? C10A Fe4A B3B 168.12(8) . . ? C10B Fe4A B3B 83.64(8) . . ? B7A Fe4A B3B 146.00(8) . . ? B7B Fe4A B3B 47.70(8) . . ? B6A Fe4A B3B 124.14(8) . . ? B6B Fe4A B3B 96.68(8) . . ? C1B Fe4A B3A 81.55(8) . . ? C1A Fe4A B3A 41.36(8) . . ? C10A Fe4A B3A 83.84(8) . . ? C10B Fe4A B3A 167.97(8) . . ? B7A Fe4A B3A 47.69(8) . . ? B7B Fe4A B3A 146.36(8) . . ? B6A Fe4A B3A 97.24(8) . . ? B6B Fe4A B3A 124.03(8) . . ? B3B Fe4A B3A 104.92(8) . . ? C1B Fe4A B2B 40.72(8) . . ? C1A Fe4A B2B 116.91(8) . . ? C10A Fe4A B2B 113.46(8) . . ? C10B Fe4A B2B 83.88(8) . . ? B7A Fe4A B2B 84.17(8) . . ? B7B Fe4A B2B 98.49(8) . . ? B6A Fe4A B2B 156.06(8) . . ? B6B Fe4A B2B 46.78(8) . . ? B3B Fe4A B2B 75.07(8) . . ? B3A Fe4A B2B 90.11(8) . . ? C1B Fe4A B2A 117.39(8) . . ? C1A Fe4A B2A 40.95(8) . . ? C10A Fe4A B2A 83.67(8) . . ? C10B Fe4A B2A 113.77(8) . . ? B7A Fe4A B2A 98.48(8) . . ? B7B Fe4A B2A 84.98(8) . . ? B6A Fe4A B2A 46.71(8) . . ? B6B Fe4A B2A 156.16(8) . . ? B3B Fe4A B2A 90.78(8) . . ? B3A Fe4A B2A 75.10(8) . . ? B2B Fe4A B2A 156.37(8) . . ? B2A C1A B3A 127.70(18) . . ? B2A C1A B5A 77.89(14) . . ? B3A C1A B5A 75.06(13) . . ? B2A C1A Fe4A 76.20(12) . . ? B3A C1A Fe4A 75.31(11) . . ? B5A C1A Fe4A 113.97(13) . . ? B2A C1A H1A 116.6(12) . . ? B3A C1A H1A 115.6(12) . . ? B5A C1A H1A 120.1(12) . . ? Fe4A C1A H1A 125.8(12) . . ? C1A B2A B6A 117.64(17) . . ? C1A B2A B9A 112.59(16) . . ? B6A B2A B9A 58.98(12) . . ? C1A B2A B5A 55.56(12) . . ? B6A B2A B5A 98.97(14) . . ? B9A B2A B5A 59.02(11) . . ? C1A B2A Fe4A 62.85(10) . . ? B6A B2A Fe4A 65.35(10) . . ? B9A B2A Fe4A 110.89(13) . . ? B5A B2A Fe4A 95.43(11) . . ? C1A B2A H2A 119.6(10) . . ? B6A B2A H2A 119.8(10) . . ? B9A B2A H2A 111.5(10) . . ? B5A B2A H2A 127.9(10) . . ? Fe4A B2A H2A 130.6(10) . . ? C1A B3A B8A 114.60(16) . . ? C1A B3A B7A 118.11(17) . . ? B8A B3A B7A 59.00(12) . . ? C1A B3A B5A 57.06(12) . . ? B8A B3A B5A 59.93(12) . . ? B7A B3A B5A 100.44(14) . . ? C1A B3A Fe4A 63.34(11) . . ? B8A B3A Fe4A 111.42(13) . . ? B7A B3A Fe4A 64.84(10) . . ? B5A B3A Fe4A 97.73(12) . . ? C1A B3A H3A 119.0(10) . . ? B8A B3A H3A 114.3(10) . . ? B7A B3A H3A 117.4(10) . . ? B5A B3A H3A 131.3(10) . . ? Fe4A B3A H3A 124.9(10) . . ? C1A B5A B11A 133.18(17) . . ? C1A B5A B8A 100.66(14) . . ? B11A B5A B8A 56.69(12) . . ? C1A B5A B9A 99.06(14) . . ? B11A B5A B9A 56.27(12) . . ? B8A B5A B9A 103.26(15) . . ? C1A B5A B3A 47.88(11) . . ? B11A B5A B3A 105.46(15) . . ? B8A B5A B3A 54.61(11) . . ? B9A B5A B3A 118.69(15) . . ? C1A B5A B2A 46.55(10) . . ? B11A B5A B2A 104.61(15) . . ? B8A B5A B2A 118.59(15) . . ? B9A B5A B2A 54.04(11) . . ? B3A B5A B2A 85.31(12) . . ? C1A B5A H5A 112.9(10) . . ? B11A B5A H5A 113.8(10) . . ? B8A B5A H5A 120.0(10) . . ? B9A B5A H5A 117.7(10) . . ? B3A B5A H5A 122.6(10) . . ? B2A B5A H5A 120.7(10) . . ? C10A B6A B12A 59.87(12) . . ? C10A B6A B9A 104.13(15) . . ? B12A B6A B9A 58.65(13) . . ? C10A B6A B2A 115.80(16) . . ? B12A B6A B2A 114.61(16) . . ? B9A B6A B2A 61.41(13) . . ? C10A B6A Fe4A 64.49(10) . . ? B12A B6A Fe4A 117.75(13) . . ? B9A B6A Fe4A 114.68(13) . . ? B2A B6A Fe4A 67.94(10) . . ? C10A B6A H6A 121.9(10) . . ? B12A B6A H6A 114.2(10) . . ? B9A B6A H6A 120.9(10) . . ? B2A B6A H6A 117.2(10) . . ? Fe4A B6A H6A 117.5(10) . . ? C10A B7A B13A 59.82(12) . . ? C10A B7A B8A 103.79(15) . . ? B13A B7A B8A 58.43(12) . . ? C10A B7A B3A 114.36(16) . . ? B13A B7A B3A 112.87(16) . . ? B8A B7A B3A 60.30(12) . . ? C10A B7A Fe4A 65.02(9) . . ? B13A B7A Fe4A 118.18(13) . . ? B8A B7A Fe4A 114.49(13) . . ? B3A B7A Fe4A 67.47(10) . . ? C10A B7A H7A 123.9(11) . . ? B13A B7A H7A 113.9(11) . . ? B8A B7A H7A 119.0(10) . . ? B3A B7A H7A 117.6(11) . . ? Fe4A B7A H7A 118.8(10) . . ? B13A B8A B11A 61.35(13) . . ? B13A B8A B7A 60.58(13) . . ? B11A B8A B7A 108.26(16) . . ? B13A B8A B3A 115.13(16) . . ? B11A B8A B3A 116.82(16) . . ? B7A B8A B3A 60.70(12) . . ? B13A B8A B5A 107.44(15) . . ? B11A B8A B5A 58.72(12) . . ? B7A B8A B5A 105.45(15) . . ? B3A B8A B5A 65.45(12) . . ? B13A B8A H8A 120.0(11) . . ? B11A B8A H8A 121.0(11) . . ? B7A B8A H8A 122.6(11) . . ? B3A B8A H8A 113.2(11) . . ? B5A B8A H8A 123.9(11) . . ? B12A B9A B11A 61.24(13) . . ? B12A B9A B6A 60.52(13) . . ? B11A B9A B6A 107.96(16) . . ? B12A B9A B2A 114.66(16) . . ? B11A B9A B2A 117.94(16) . . ? B6A B9A B2A 59.61(12) . . ? B12A B9A B5A 106.91(15) . . ? B11A B9A B5A 58.45(12) . . ? B6A B9A B5A 104.88(15) . . ? B2A B9A B5A 66.94(12) . . ? B12A B9A H9A 122.2(11) . . ? B11A B9A H9A 121.3(10) . . ? B6A B9A H9A 123.9(10) . . ? B2A B9A H9A 111.3(10) . . ? B5A B9A H9A 122.3(10) . . ? B7A C10A B6A 123.05(16) . . ? B7A C10A B13A 62.31(12) . . ? B6A C10A B13A 115.54(15) . . ? B7A C10A B12A 115.78(15) . . ? B6A C10A B12A 62.28(12) . . ? B13A C10A B12A 61.43(12) . . ? B7A C10A Fe4A 69.29(10) . . ? B6A C10A Fe4A 70.02(10) . . ? B13A C10A Fe4A 124.00(13) . . ? B12A C10A Fe4A 124.59(13) . . ? B7A C10A H10A 114.0(12) . . ? B6A C10A H10A 115.6(12) . . ? B13A C10A H10A 115.7(12) . . ? B12A C10A H10A 116.4(12) . . ? Fe4A C10A H10A 108.3(12) . . ? B9A B11A B8A 116.82(16) . . ? B9A B11A B12A 58.61(13) . . ? B8A B11A B12A 108.53(16) . . ? B9A B11A B13A 108.77(16) . . ? B8A B11A B13A 58.29(12) . . ? B12A B11A B13A 59.32(12) . . ? B9A B11A B5A 65.28(13) . . ? B8A B11A B5A 64.59(13) . . ? B12A B11A B5A 110.21(15) . . ? B13A B11A B5A 109.67(15) . . ? B9A B11A K1A 117.93(12) . . ? B8A B11A K1A 114.40(12) . . ? B12A B11A K1A 73.82(10) . . ? B13A B11A K1A 72.04(10) . . ? B5A B11A K1A 175.97(14) . . ? B9A B11A H11A 118.2(10) . . ? B8A B11A H11A 119.4(10) . . ? B12A B11A H11A 120.3(10) . . ? B13A B11A H11A 121.0(10) . . ? B5A B11A H11A 121.0(10) . . ? K1A B11A H11A 55.7(10) . . ? C10A B12A B9A 104.27(15) . . ? C10A B12A B13A 59.21(12) . . ? B9A B12A B13A 110.95(17) . . ? C10A B12A B6A 57.85(12) . . ? B9A B12A B6A 60.83(13) . . ? B13A B12A B6A 109.83(16) . . ? C10A B12A B11A 102.17(15) . . ? B9A B12A B11A 60.15(13) . . ? B13A B12A B11A 60.39(13) . . ? B6A B12A B11A 107.37(16) . . ? C10A B12A K1A 123.59(12) . . ? B9A B12A K1A 120.35(12) . . ? B13A B12A K1A 73.02(10) . . ? B6A B12A K1A 176.56(14) . . ? B11A B12A K1A 75.63(10) . . ? C10A B12A H12A 121.0(10) . . ? B9A B12A H12A 124.6(10) . . ? B13A B12A H12A 118.7(10) . . ? B6A B12A H12A 118.0(10) . . ? B11A B12A H12A 128.8(10) . . ? K1A B12A H12A 58.5(10) . . ? C10A B13A B8A 104.25(15) . . ? C10A B13A B12A 59.35(12) . . ? B8A B13A B12A 111.08(16) . . ? C10A B13A B7A 57.86(12) . . ? B8A B13A B7A 60.98(13) . . ? B12A B13A B7A 110.15(15) . . ? C10A B13A B11A 102.20(15) . . ? B8A B13A B11A 60.36(13) . . ? B12A B13A B11A 60.30(13) . . ? B7A B13A B11A 107.81(16) . . ? C10A B13A K1A 126.52(12) . . ? B8A B13A K1A 119.50(12) . . ? B12A B13A K1A 76.37(10) . . ? B7A B13A K1A 173.10(13) . . ? B11A B13A K1A 77.16(10) . . ? C10A B13A H13A 120.0(10) . . ? B8A B13A H13A 125.1(10) . . ? B12A B13A H13A 118.5(10) . . ? B7A B13A H13A 117.0(10) . . ? B11A B13A H13A 129.7(10) . . ? K1A B13A H13A 56.6(10) . . ? B2B C1B B3B 127.85(19) . . ? B2B C1B B5B 78.16(14) . . ? B3B C1B B5B 75.06(14) . . ? B2B C1B Fe4A 76.47(11) . . ? B3B C1B Fe4A 75.14(11) . . ? B5B C1B Fe4A 114.26(13) . . ? B2B C1B H1B 116.7(12) . . ? B3B C1B H1B 115.4(12) . . ? B5B C1B H1B 120.5(12) . . ? Fe4A C1B H1B 125.1(12) . . ? C1B B2B B6B 117.46(17) . . ? C1B B2B B9B 112.23(16) . . ? B6B B2B B9B 58.53(12) . . ? C1B B2B B5B 55.53(12) . . ? B6B B2B B5B 98.27(14) . . ? B9B B2B B5B 58.66(12) . . ? C1B B2B Fe4A 62.81(10) . . ? B6B B2B Fe4A 65.74(10) . . ? B9B B2B Fe4A 110.99(13) . . ? B5B B2B Fe4A 95.45(11) . . ? C1B B2B H2B 120.6(10) . . ? B6B B2B H2B 118.3(10) . . ? B9B B2B H2B 113.0(10) . . ? B5B B2B H2B 131.0(10) . . ? Fe4A B2B H2B 128.0(10) . . ? C1B B3B B8B 114.71(17) . . ? C1B B3B B7B 118.32(17) . . ? B8B B3B B7B 59.14(13) . . ? C1B B3B B5B 56.93(12) . . ? B8B B3B B5B 60.11(12) . . ? B7B B3B B5B 100.63(15) . . ? C1B B3B Fe4A 63.35(10) . . ? B8B B3B Fe4A 112.01(14) . . ? B7B B3B Fe4A 65.19(10) . . ? B5B B3B Fe4A 97.91(12) . . ? C1B B3B H3B 119.9(10) . . ? B8B B3B H3B 110.3(10) . . ? B7B B3B H3B 118.2(10) . . ? B5B B3B H3B 127.3(10) . . ? Fe4A B3B H3B 129.2(10) . . ? C1B B5B B11B 133.62(17) . . ? C1B B5B B8B 100.96(14) . . ? B11B B5B B8B 56.69(12) . . ? C1B B5B B9B 99.23(14) . . ? B11B B5B B9B 56.37(12) . . ? B8B B5B B9B 103.33(15) . . ? C1B B5B B3B 48.01(11) . . ? B11B B5B B3B 105.62(15) . . ? B8B B5B B3B 54.73(11) . . ? B9B B5B B3B 118.81(15) . . ? C1B B5B B2B 46.31(11) . . ? B11B B5B B2B 105.16(15) . . ? B8B B5B B2B 118.90(15) . . ? B9B B5B B2B 54.44(11) . . ? B3B B5B B2B 85.22(12) . . ? C1B B5B K1C 140.79(13) . . ? B11B B5B K1C 72.46(10) . . ? B8B B5B K1C 66.86(9) . . ? B9B B5B K1C 119.61(12) . . ? B3B B5B K1C 103.09(11) . . ? B2B B5B K1C 171.68(12) . . ? C1B B5B H5B 110.8(10) . . ? B11B B5B H5B 115.5(10) . . ? B8B B5B H5B 120.4(10) . . ? B9B B5B H5B 118.7(10) . . ? B3B B5B H5B 121.1(10) . . ? B2B B5B H5B 119.6(10) . . ? K1C B5B H5B 56.5(10) . . ? C10B B6B B9B 104.84(15) . . ? C10B B6B B12B 60.23(12) . . ? B9B B6B B12B 59.13(13) . . ? C10B B6B B2B 116.22(16) . . ? B9B B6B B2B 61.66(13) . . ? B12B B6B B2B 115.42(16) . . ? C10B B6B Fe4A 64.78(10) . . ? B9B B6B Fe4A 114.65(14) . . ? B12B B6B Fe4A 118.32(14) . . ? B2B B6B Fe4A 67.48(10) . . ? C10B B6B H6B 118.1(10) . . ? B9B B6B H6B 124.1(10) . . ? B12B B6B H6B 113.8(10) . . ? B2B B6B H6B 119.1(10) . . ? Fe4A B6B H6B 115.1(10) . . ? C10B B7B B8B 103.94(15) . . ? C10B B7B B13B 59.85(12) . . ? B8B B7B B13B 58.41(13) . . ? C10B B7B B3B 114.57(16) . . ? B8B B7B B3B 60.38(13) . . ? B13B B7B B3B 112.93(16) . . ? C10B B7B Fe4A 65.59(10) . . ? B8B B7B Fe4A 114.46(13) . . ? B13B B7B Fe4A 118.61(13) . . ? B3B B7B Fe4A 67.11(10) . . ? C10B B7B H7B 122.0(11) . . ? B8B B7B H7B 119.6(10) . . ? B13B B7B H7B 112.5(10) . . ? B3B B7B H7B 119.5(10) . . ? Fe4A B7B H7B 119.0(10) . . ? B13B B8B B11B 61.53(13) . . ? B13B B8B B7B 60.87(13) . . ? B11B B8B B7B 108.40(16) . . ? B13B B8B B3B 115.20(16) . . ? B11B B8B B3B 116.52(16) . . ? B7B B8B B3B 60.48(12) . . ? B13B B8B B5B 107.45(16) . . ? B11B B8B B5B 58.59(13) . . ? B7B B8B B5B 105.07(15) . . ? B3B B8B B5B 65.16(13) . . ? B13B B8B K1C 123.67(13) . . ? B11B B8B K1C 79.89(11) . . ? B7B B8B K1C 171.41(14) . . ? B3B B8B K1C 118.38(13) . . ? B5B B8B K1C 80.98(10) . . ? B13B B8B H8B 117.5(11) . . ? B11B B8B H8B 120.0(11) . . ? B7B B8B H8B 122.2(11) . . ? B3B B8B H8B 115.4(11) . . ? B5B B8B H8B 125.8(11) . . ? K1C B8B H8B 49.7(11) . . ? B12B B9B B11B 61.21(13) . . ? B12B B9B B6B 60.55(13) . . ? B11B B9B B6B 107.94(16) . . ? B12B B9B B2B 115.02(16) . . ? B11B B9B B2B 118.24(16) . . ? B6B B9B B2B 59.81(12) . . ? B12B B9B B5B 107.10(15) . . ? B11B B9B B5B 58.69(12) . . ? B6B B9B B5B 104.84(15) . . ? B2B B9B B5B 66.90(13) . . ? B12B B9B H9B 120.5(11) . . ? B11B B9B H9B 120.3(10) . . ? B6B B9B H9B 123.9(10) . . ? B2B B9B H9B 112.5(10) . . ? B5B B9B H9B 123.3(11) . . ? B7B C10B B6B 122.40(16) . . ? B7B C10B B13B 62.79(13) . . ? B6B C10B B13B 114.78(15) . . ? B7B C10B B12B 115.57(15) . . ? B6B C10B B12B 62.02(12) . . ? B13B C10B B12B 60.93(12) . . ? B7B C10B Fe4A 69.03(10) . . ? B6B C10B Fe4A 69.92(10) . . ? B13B C10B Fe4A 124.08(13) . . ? B12B C10B Fe4A 124.30(13) . . ? B7B C10B H10B 115.8(12) . . ? B6B C10B H10B 114.3(12) . . ? B13B C10B H10B 116.9(12) . . ? B12B C10B H10B 115.8(12) . . ? Fe4A C10B H10B 108.3(12) . . ? B9B B11B B8B 116.66(17) . . ? B9B B11B B12B 59.01(13) . . ? B8B B11B B12B 108.36(16) . . ? B9B B11B B13B 108.76(16) . . ? B8B B11B B13B 58.40(13) . . ? B12B B11B B13B 58.97(13) . . ? B9B B11B B5B 64.94(13) . . ? B8B B11B B5B 64.73(13) . . ? B12B B11B B5B 110.27(16) . . ? B13B B11B B5B 109.83(16) . . ? B9B B11B K1C 130.32(13) . . ? B8B B11B K1C 69.94(10) . . ? B12B B11B K1C 170.55(13) . . ? B13B B11B K1C 114.21(12) . . ? B5B B11B K1C 77.73(11) . . ? B9B B11B H11B 117.2(10) . . ? B8B B11B H11B 118.1(10) . . ? B12B B11B H11B 124.3(11) . . ? B13B B11B H11B 124.8(10) . . ? B5B B11B H11B 116.2(11) . . ? K1C B11B H11B 52.6(10) . . ? C10B B12B B9B 103.86(16) . . ? C10B B12B B13B 59.30(12) . . ? B9B B12B B13B 110.91(17) . . ? C10B B12B B6B 57.75(12) . . ? B9B B12B B6B 60.32(13) . . ? B13B B12B B6B 109.71(16) . . ? C10B B12B B11B 102.20(16) . . ? B9B B12B B11B 59.78(13) . . ? B13B B12B B11B 60.76(13) . . ? B6B B12B B11B 106.67(17) . . ? C10B B12B H12B 120.9(10) . . ? B9B B12B H12B 124.6(10) . . ? B13B B12B H12B 119.1(10) . . ? B6B B12B H12B 117.8(10) . . ? B11B B12B H12B 129.4(10) . . ? C10B B13B B8B 103.80(16) . . ? C10B B13B B12B 59.76(12) . . ? B8B B13B B12B 110.85(17) . . ? C10B B13B B7B 57.36(12) . . ? B8B B13B B7B 60.71(13) . . ? B12B B13B B7B 109.89(16) . . ? C10B B13B B11B 102.17(15) . . ? B8B B13B B11B 60.07(13) . . ? B12B B13B B11B 60.27(13) . . ? B7B B13B B11B 107.16(16) . . ? C10B B13B H13B 121.7(11) . . ? B8B B13B H13B 124.3(11) . . ? B12B B13B H13B 118.8(11) . . ? B7B B13B H13B 118.4(10) . . ? B11B B13B H13B 128.4(10) . . ? C1D Fe4C C1C 84.86(8) . . ? C1D Fe4C C10C 151.26(8) . . ? C1C Fe4C C10C 100.29(8) . . ? C1D Fe4C C10D 100.15(8) . . ? C1C Fe4C C10D 152.09(8) . . ? C10C Fe4C C10D 88.47(8) . . ? C1D Fe4C B7C 107.89(8) . . ? C1C Fe4C B7C 84.16(8) . . ? C10C Fe4C B7C 45.61(8) . . ? C10D Fe4C B7C 119.38(8) . . ? C1D Fe4C B7D 84.38(8) . . ? C1C Fe4C B7D 108.97(8) . . ? C10C Fe4C B7D 119.53(8) . . ? C10D Fe4C B7D 45.27(8) . . ? B7C Fe4C B7D 163.14(8) . . ? C1D Fe4C B6D 82.09(8) . . ? C1C Fe4C B6D 161.03(8) . . ? C10C Fe4C B6D 85.01(8) . . ? C10D Fe4C B6D 45.11(8) . . ? B7C Fe4C B6D 86.82(9) . . ? B7D Fe4C B6D 83.42(8) . . ? C1D Fe4C B6C 161.51(8) . . ? C1C Fe4C B6C 82.22(8) . . ? C10C Fe4C B6C 45.37(8) . . ? C10D Fe4C B6C 85.50(8) . . ? B7C Fe4C B6C 83.93(8) . . ? B7D Fe4C B6C 87.37(8) . . ? B6D Fe4C B6C 113.39(8) . . ? C1D Fe4C B3D 41.70(8) . . ? C1C Fe4C B3D 82.47(8) . . ? C10C Fe4C B3D 166.52(8) . . ? C10D Fe4C B3D 83.37(8) . . ? B7C Fe4C B3D 147.69(8) . . ? B7D Fe4C B3D 47.77(8) . . ? B6D Fe4C B3D 96.64(8) . . ? B6C Fe4C B3D 122.91(8) . . ? C1D Fe4C B3C 81.77(8) . . ? C1C Fe4C B3C 41.47(8) . . ? C10C Fe4C B3C 83.71(8) . . ? C10D Fe4C B3C 166.11(8) . . ? B7C Fe4C B3C 47.76(8) . . ? B7D Fe4C B3C 148.24(8) . . ? B6D Fe4C B3C 122.42(8) . . ? B6C Fe4C B3C 96.99(8) . . ? B3D Fe4C B3C 106.33(8) . . ? C1D Fe4C B2D 40.93(8) . . ? C1C Fe4C B2D 115.37(8) . . ? C10C Fe4C B2D 114.35(8) . . ? C10D Fe4C B2D 83.91(8) . . ? B7C Fe4C B2D 84.01(8) . . ? B7D Fe4C B2D 99.08(8) . . ? B6D Fe4C B2D 46.87(8) . . ? B6C Fe4C B2D 157.42(8) . . ? B3D Fe4C B2D 75.51(8) . . ? B3C Fe4C B2D 88.87(8) . . ? C1D Fe4C B2C 115.86(8) . . ? C1C Fe4C B2C 40.78(8) . . ? C10C Fe4C B2C 83.80(8) . . ? C10D Fe4C B2C 115.52(8) . . ? B7C Fe4C B2C 98.71(8) . . ? B7D Fe4C B2C 85.63(8) . . ? B6D Fe4C B2C 157.92(8) . . ? B6C Fe4C B2C 46.82(8) . . ? B3D Fe4C B2C 90.04(8) . . ? B3C Fe4C B2C 75.10(8) . . ? B2D Fe4C B2C 154.62(9) . . ? B2C C1C B3C 127.87(18) . . ? B2C C1C B5C 78.38(14) . . ? B3C C1C B5C 74.66(14) . . ? B2C C1C Fe4C 76.41(12) . . ? B3C C1C Fe4C 75.18(12) . . ? B5C C1C Fe4C 113.95(13) . . ? B2C C1C H1C 113.4(12) . . ? B3C C1C H1C 118.7(12) . . ? B5C C1C H1C 121.7(12) . . ? Fe4C C1C H1C 124.3(12) . . ? C1C B2C B6C 117.32(17) . . ? C1C B2C B9C 112.09(16) . . ? B6C B2C B9C 58.88(12) . . ? C1C B2C B5C 55.54(12) . . ? B6C B2C B5C 98.32(14) . . ? B9C B2C B5C 58.48(12) . . ? C1C B2C Fe4C 62.81(10) . . ? B6C B2C Fe4C 65.31(10) . . ? B9C B2C Fe4C 110.71(13) . . ? B5C B2C Fe4C 95.20(11) . . ? C1C B2C H2C 120.4(10) . . ? B6C B2C H2C 119.0(10) . . ? B9C B2C H2C 112.4(10) . . ? B5C B2C H2C 129.8(10) . . ? Fe4C B2C H2C 129.3(10) . . ? C1C B3C B8C 115.15(17) . . ? C1C B3C B7C 118.33(17) . . ? B8C B3C B7C 58.88(12) . . ? C1C B3C B5C 57.38(12) . . ? B8C B3C B5C 60.18(12) . . ? B7C B3C B5C 100.56(15) . . ? C1C B3C Fe4C 63.35(11) . . ? B8C B3C Fe4C 111.75(13) . . ? B7C B3C Fe4C 65.02(10) . . ? B5C B3C Fe4C 98.08(12) . . ? C1C B3C H3C 120.3(10) . . ? B8C B3C H3C 111.6(10) . . ? B7C B3C H3C 116.7(10) . . ? B5C B3C H3C 129.9(10) . . ? Fe4C B3C H3C 126.8(10) . . ? C1C B5C B11C 133.23(17) . . ? C1C B5C B8C 100.87(15) . . ? B11C B5C B8C 56.65(12) . . ? C1C B5C B9C 98.92(15) . . ? B11C B5C B9C 56.45(12) . . ? B8C B5C B9C 103.47(15) . . ? C1C B5C B3C 47.96(11) . . ? B11C B5C B3C 105.50(15) . . ? B8C B5C B3C 54.74(11) . . ? B9C B5C B3C 118.77(15) . . ? C1C B5C B2C 46.08(11) . . ? B11C B5C B2C 105.00(15) . . ? B8C B5C B2C 118.74(15) . . ? B9C B5C B2C 54.34(11) . . ? B3C B5C B2C 85.03(12) . . ? C1C B5C H5C 110.4(11) . . ? B11C B5C H5C 116.2(11) . . ? B8C B5C H5C 122.7(11) . . ? B9C B5C H5C 116.9(11) . . ? B3C B5C H5C 122.5(11) . . ? B2C B5C H5C 117.6(10) . . ? C10C B6C B12C 60.01(12) . . ? C10C B6C B9C 104.18(15) . . ? B12C B6C B9C 58.59(13) . . ? C10C B6C B2C 116.06(17) . . ? B12C B6C B2C 114.97(17) . . ? B9C B6C B2C 61.72(13) . . ? C10C B6C Fe4C 64.59(10) . . ? B12C B6C Fe4C 117.99(14) . . ? B9C B6C Fe4C 114.75(14) . . ? B2C B6C Fe4C 67.87(10) . . ? C10C B6C H6C 121.0(10) . . ? B12C B6C H6C 114.6(10) . . ? B9C B6C H6C 122.1(10) . . ? B2C B6C H6C 117.2(10) . . ? Fe4C B6C H6C 116.4(10) . . ? C10C B7C B8C 103.87(15) . . ? C10C B7C B13C 59.73(12) . . ? B8C B7C B13C 58.56(13) . . ? C10C B7C B3C 113.98(16) . . ? B8C B7C B3C 60.43(13) . . ? B13C B7C B3C 112.88(16) . . ? C10C B7C Fe4C 65.03(10) . . ? B8C B7C Fe4C 114.68(14) . . ? B13C B7C Fe4C 118.18(14) . . ? B3C B7C Fe4C 67.22(10) . . ? C10C B7C H7C 124.3(11) . . ? B8C B7C H7C 118.4(11) . . ? B13C B7C H7C 113.8(11) . . ? B3C B7C H7C 117.7(11) . . ? Fe4C B7C H7C 119.0(10) . . ? B13C B8C B11C 61.27(13) . . ? B13C B8C B7C 60.75(13) . . ? B11C B8C B7C 108.21(16) . . ? B13C B8C B3C 115.03(16) . . ? B11C B8C B3C 116.20(16) . . ? B7C B8C B3C 60.69(12) . . ? B13C B8C B5C 107.09(16) . . ? B11C B8C B5C 58.41(12) . . ? B7C B8C B5C 105.23(15) . . ? B3C B8C B5C 65.08(12) . . ? B13C B8C H8C 118.0(10) . . ? B11C B8C H8C 119.7(10) . . ? B7C B8C H8C 122.8(10) . . ? B3C B8C H8C 115.7(10) . . ? B5C B8C H8C 125.2(10) . . ? B12C B9C B11C 61.37(13) . . ? B12C B9C B6C 60.28(13) . . ? B11C B9C B6C 107.73(16) . . ? B12C B9C B2C 114.40(16) . . ? B11C B9C B2C 117.99(16) . . ? B6C B9C B2C 59.40(12) . . ? B12C B9C B5C 106.87(15) . . ? B11C B9C B5C 58.33(12) . . ? B6C B9C B5C 104.69(15) . . ? B2C B9C B5C 67.18(13) . . ? B12C B9C H9C 122.1(11) . . ? B11C B9C H9C 122.0(11) . . ? B6C B9C H9C 123.4(11) . . ? B2C B9C H9C 111.0(11) . . ? B5C B9C H9C 123.0(11) . . ? B6C C10C B7C 123.15(16) . . ? B6C C10C B13C 115.58(15) . . ? B7C C10C B13C 62.60(13) . . ? B6C C10C B12C 62.20(12) . . ? B7C C10C B12C 115.87(16) . . ? B13C C10C B12C 61.35(12) . . ? B6C C10C Fe4C 70.04(10) . . ? B7C C10C Fe4C 69.37(10) . . ? B13C C10C Fe4C 124.40(13) . . ? B12C C10C Fe4C 124.57(13) . . ? B6C C10C H10C 115.7(13) . . ? B7C C10C H10C 114.0(13) . . ? B13C C10C H10C 115.0(13) . . ? B12C C10C H10C 116.0(13) . . ? Fe4C C10C H10C 108.8(13) . . ? B9C B11C B8C 117.15(16) . . ? B9C B11C B13C 108.82(16) . . ? B8C B11C B13C 58.53(13) . . ? B9C B11C B12C 58.52(13) . . ? B8C B11C B12C 108.56(16) . . ? B13C B11C B12C 59.17(13) . . ? B9C B11C B5C 65.22(13) . . ? B8C B11C B5C 64.93(13) . . ? B13C B11C B5C 110.07(16) . . ? B12C B11C B5C 110.04(16) . . ? B9C B11C K1D 116.26(12) . . ? B8C B11C K1D 116.18(12) . . ? B13C B11C K1D 73.23(10) . . ? B12C B11C K1D 73.47(10) . . ? B5C B11C K1D 176.01(14) . . ? B9C B11C H11C 113.8(10) . . ? B8C B11C H11C 123.2(10) . . ? B13C B11C H11C 123.7(10) . . ? B12C B11C H11C 118.4(11) . . ? B5C B11C H11C 120.1(10) . . ? K1D B11C H11C 55.9(10) . . ? C10C B12C B9C 104.45(15) . . ? C10C B12C B13C 59.28(12) . . ? B9C B12C B13C 111.18(17) . . ? C10C B12C B6C 57.80(12) . . ? B9C B12C B6C 61.13(13) . . ? B13C B12C B6C 109.99(16) . . ? C10C B12C B11C 102.02(15) . . ? B9C B12C B11C 60.11(13) . . ? B13C B12C B11C 60.39(13) . . ? B6C B12C B11C 107.43(16) . . ? C10C B12C K1D 125.31(12) . . ? B9C B12C K1D 119.51(12) . . ? B13C B12C K1D 74.80(10) . . ? B6C B12C K1D 174.83(14) . . ? B11C B12C K1D 76.46(10) . . ? C10C B12C H12C 119.7(11) . . ? B9C B12C H12C 126.6(11) . . ? B13C B12C H12C 116.4(10) . . ? B6C B12C H12C 119.0(11) . . ? B11C B12C H12C 128.8(11) . . ? K1D B12C H12C 56.1(10) . . ? C10C B13C B8C 103.93(16) . . ? C10C B13C B12C 59.37(12) . . ? B8C B13C B12C 111.01(17) . . ? C10C B13C B7C 57.66(12) . . ? B8C B13C B7C 60.69(13) . . ? B12C B13C B7C 109.91(16) . . ? C10C B13C B11C 102.12(15) . . ? B8C B13C B11C 60.20(13) . . ? B12C B13C B11C 60.43(13) . . ? B7C B13C B11C 107.35(16) . . ? C10C B13C K1D 125.77(12) . . ? B8C B13C K1D 119.84(12) . . ? B12C B13C K1D 75.27(10) . . ? B7C B13C K1D 174.48(13) . . ? B11C B13C K1D 76.69(10) . . ? C10C B13C H13C 120.3(10) . . ? B8C B13C H13C 127.4(10) . . ? B12C B13C H13C 115.3(11) . . ? B7C B13C H13C 120.7(10) . . ? B11C B13C H13C 127.4(10) . . ? K1D B13C H13C 54.2(10) . . ? B2D C1D B3D 127.80(18) . . ? B2D C1D B5D 79.01(14) . . ? B3D C1D B5D 74.56(14) . . ? B2D C1D Fe4C 76.22(11) . . ? B3D C1D Fe4C 74.88(11) . . ? B5D C1D Fe4C 114.07(13) . . ? B2D C1D H1D 117.6(13) . . ? B3D C1D H1D 114.6(13) . . ? B5D C1D H1D 121.2(13) . . ? Fe4C C1D H1D 124.5(13) . . ? C1D B2D B6D 116.94(17) . . ? C1D B2D B9D 111.27(16) . . ? B6D B2D B9D 58.88(12) . . ? C1D B2D B5D 54.76(12) . . ? B6D B2D B5D 97.66(14) . . ? B9D B2D B5D 58.27(11) . . ? C1D B2D Fe4C 62.85(10) . . ? B6D B2D Fe4C 65.55(10) . . ? B9D B2D Fe4C 110.98(13) . . ? B5D B2D Fe4C 94.71(11) . . ? C1D B2D H2D 121.7(10) . . ? B6D B2D H2D 118.4(10) . . ? B9D B2D H2D 111.7(10) . . ? B5D B2D H2D 130.5(10) . . ? Fe4C B2D H2D 129.6(10) . . ? C1D B3D B8D 115.18(17) . . ? C1D B3D B7D 118.72(17) . . ? B8D B3D B7D 59.10(12) . . ? C1D B3D B5D 56.95(12) . . ? B8D B3D B5D 60.53(12) . . ? B7D B3D B5D 100.98(15) . . ? C1D B3D Fe4C 63.42(10) . . ? B8D B3D Fe4C 112.32(13) . . ? B7D B3D Fe4C 65.43(10) . . ? B5D B3D Fe4C 98.07(12) . . ? C1D B3D H3D 118.6(10) . . ? B8D B3D H3D 112.5(10) . . ? B7D B3D H3D 118.1(10) . . ? B5D B3D H3D 129.1(10) . . ? Fe4C B3D H3D 126.5(10) . . ? C1D B5D B11D 134.04(17) . . ? C1D B5D B9D 99.36(14) . . ? B11D B5D B9D 56.57(12) . . ? C1D B5D B8D 101.69(14) . . ? B11D B5D B8D 56.43(12) . . ? B9D B5D B8D 103.54(15) . . ? C1D B5D B3D 48.50(11) . . ? B11D B5D B3D 105.62(15) . . ? B9D B5D B3D 119.26(15) . . ? B8D B5D B3D 54.96(11) . . ? C1D B5D B2D 46.24(11) . . ? B11D B5D B2D 105.34(15) . . ? B9D B5D B2D 54.52(11) . . ? B8D B5D B2D 119.26(14) . . ? B3D B5D B2D 85.47(12) . . ? C1D B5D K1B 140.37(13) . 2_675 ? B11D B5D K1B 74.38(10) . 2_675 ? B9D B5D K1B 120.23(11) . 2_675 ? B8D B5D K1B 69.13(9) . 2_675 ? B3D B5D K1B 104.20(10) . 2_675 ? B2D B5D K1B 170.11(11) . 2_675 ? C1D B5D H5D 113.4(10) . . ? B11D B5D H5D 112.5(10) . . ? B9D B5D H5D 117.3(10) . . ? B8D B5D H5D 118.7(10) . . ? B3D B5D H5D 122.6(10) . . ? B2D B5D H5D 121.4(10) . . ? K1B B5D H5D 51.6(10) 2_675 . ? C10D B6D B12D 60.36(12) . . ? C10D B6D B9D 104.74(15) . . ? B12D B6D B9D 59.00(13) . . ? C10D B6D B2D 116.74(16) . . ? B12D B6D B2D 115.78(16) . . ? B9D B6D B2D 61.85(13) . . ? C10D B6D Fe4C 65.11(10) . . ? B12D B6D Fe4C 118.81(14) . . ? B9D B6D Fe4C 114.71(14) . . ? B2D B6D Fe4C 67.58(10) . . ? C10D B6D H6D 119.7(10) . . ? B12D B6D H6D 112.6(10) . . ? B9D B6D H6D 121.8(10) . . ? B2D B6D H6D 118.1(10) . . ? Fe4C B6D H6D 117.1(10) . . ? C10D B7D B8D 103.67(15) . . ? C10D B7D B13D 59.78(12) . . ? B8D B7D B13D 58.18(13) . . ? C10D B7D B3D 113.87(16) . . ? B8D B7D B3D 60.38(12) . . ? B13D B7D B3D 112.45(15) . . ? C10D B7D Fe4C 65.47(10) . . ? B8D B7D Fe4C 114.37(13) . . ? B13D B7D Fe4C 118.39(13) . . ? B3D B7D Fe4C 66.79(10) . . ? C10D B7D H7D 121.0(11) . . ? B8D B7D H7D 121.6(11) . . ? B13D B7D H7D 113.7(11) . . ? B3D B7D H7D 120.4(11) . . ? Fe4C B7D H7D 117.3(11) . . ? B13D B8D B11D 61.38(13) . . ? B13D B8D B7D 61.15(13) . . ? B11D B8D B7D 108.45(16) . . ? B13D B8D B3D 115.19(16) . . ? B11D B8D B3D 115.92(16) . . ? B7D B8D B3D 60.52(12) . . ? B13D B8D B5D 107.14(15) . . ? B11D B8D B5D 58.51(12) . . ? B7D B8D B5D 104.73(15) . . ? B3D B8D B5D 64.51(12) . . ? B13D B8D K1B 125.55(13) . 2_675 ? B11D B8D K1B 79.05(10) . 2_675 ? B7D B8D K1B 172.33(14) . 2_675 ? B3D B8D K1B 115.18(12) . 2_675 ? B5D B8D K1B 77.54(10) . 2_675 ? B13D B8D H8D 120.1(10) . . ? B11D B8D H8D 122.1(10) . . ? B7D B8D H8D 121.8(10) . . ? B3D B8D H8D 113.0(10) . . ? B5D B8D H8D 124.7(10) . . ? K1B B8D H8D 52.7(10) 2_675 . ? B12D B9D B11D 61.29(13) . . ? B12D B9D B6D 60.20(13) . . ? B11D B9D B6D 107.29(16) . . ? B12D B9D B2D 114.53(16) . . ? B11D B9D B2D 118.24(16) . . ? B6D B9D B2D 59.27(12) . . ? B12D B9D B5D 106.86(15) . . ? B11D B9D B5D 58.47(12) . . ? B6D B9D B5D 104.06(15) . . ? B2D B9D B5D 67.22(12) . . ? B12D B9D H9D 121.7(11) . . ? B11D B9D H9D 123.3(10) . . ? B6D B9D H9D 122.4(11) . . ? B2D B9D H9D 110.1(10) . . ? B5D B9D H9D 124.2(11) . . ? B7D C10D B6D 122.97(16) . . ? B7D C10D B13D 63.08(13) . . ? B6D C10D B13D 115.18(15) . . ? B7D C10D B12D 116.12(15) . . ? B6D C10D B12D 62.29(13) . . ? B13D C10D B12D 60.99(12) . . ? B7D C10D Fe4C 69.26(10) . . ? B6D C10D Fe4C 69.78(10) . . ? B13D C10D Fe4C 124.45(13) . . ? B12D C10D Fe4C 124.50(13) . . ? B7D C10D H10D 113.8(12) . . ? B6D C10D H10D 116.9(12) . . ? B13D C10D H10D 113.1(12) . . ? B12D C10D H10D 114.5(12) . . ? Fe4C C10D H10D 111.0(12) . . ? B8D B11D B9D 117.25(16) . . ? B8D B11D B13D 58.56(13) . . ? B9D B11D B13D 109.01(15) . . ? B8D B11D B12D 108.59(15) . . ? B9D B11D B12D 58.92(12) . . ? B13D B11D B12D 59.03(13) . . ? B8D B11D B5D 65.05(13) . . ? B9D B11D B5D 64.96(13) . . ? B13D B11D B5D 110.07(16) . . ? B12D B11D B5D 110.07(15) . . ? B8D B11D K1B 70.35(10) . 2_675 ? B9D B11D K1B 126.81(12) . 2_675 ? B13D B11D K1B 116.85(12) . 2_675 ? B12D B11D K1B 174.18(13) . 2_675 ? B5D B11D K1B 74.89(10) . 2_675 ? B8D B11D H11D 117.8(10) . . ? B9D B11D H11D 117.2(10) . . ? B13D B11D H11D 124.1(10) . . ? B12D B11D H11D 123.9(11) . . ? B5D B11D H11D 116.8(11) . . ? K1B B11D H11D 53.9(10) 2_675 . ? C10D B12D B9D 103.84(16) . . ? C10D B12D B13D 59.34(12) . . ? B9D B12D B13D 110.80(17) . . ? C10D B12D B6D 57.35(12) . . ? B9D B12D B6D 60.80(13) . . ? B13D B12D B6D 109.50(16) . . ? C10D B12D B11D 101.57(15) . . ? B9D B12D B11D 59.79(13) . . ? B13D B12D B11D 60.29(13) . . ? B6D B12D B11D 106.60(16) . . ? C10D B12D H12D 119.0(10) . . ? B9D B12D H12D 127.3(10) . . ? B13D B12D H12D 116.7(10) . . ? B6D B12D H12D 118.7(10) . . ? B11D B12D H12D 130.3(10) . . ? C10D B13D B8D 103.56(16) . . ? C10D B13D B12D 59.67(12) . . ? B8D B13D B12D 111.23(16) . . ? C10D B13D B11D 102.09(15) . . ? B8D B13D B11D 60.06(13) . . ? B12D B13D B11D 60.69(13) . . ? C10D B13D B7D 57.14(12) . . ? B8D B13D B7D 60.67(13) . . ? B12D B13D B7D 109.85(16) . . ? B11D B13D B7D 107.08(16) . . ? C10D B13D H13D 119.0(10) . . ? B8D B13D H13D 127.8(10) . . ? B12D B13D H13D 115.7(10) . . ? B11D B13D H13D 129.5(10) . . ? B7D B13D H13D 119.1(10) . . ? O1A K1A O4A 159.93(4) . . ? O1A K1A O6A 59.99(4) . . ? O4A K1A O6A 117.77(4) . . ? O1A K1A O2A 58.95(4) . . ? O4A K1A O2A 118.84(4) . . ? O6A K1A O2A 118.93(4) . . ? O1A K1A O3A 113.99(4) . . ? O4A K1A O3A 59.50(4) . . ? O6A K1A O3A 157.54(4) . . ? O2A K1A O3A 59.36(4) . . ? O1A K1A O5A 113.84(4) . . ? O4A K1A O5A 59.26(4) . . ? O6A K1A O5A 58.58(4) . . ? O2A K1A O5A 156.58(4) . . ? O3A K1A O5A 113.00(4) . . ? O1A K1A B13A 83.26(5) . . ? O4A K1A B13A 116.60(5) . . ? O6A K1A B13A 94.18(5) . . ? O2A K1A B13A 79.99(5) . . ? O3A K1A B13A 106.91(5) . . ? O5A K1A B13A 122.68(5) . . ? O1A K1A B12A 113.27(5) . . ? O4A K1A B12A 86.25(5) . . ? O6A K1A B12A 113.79(5) . . ? O2A K1A B12A 90.89(5) . . ? O3A K1A B12A 88.61(5) . . ? O5A K1A B12A 111.68(5) . . ? B13A K1A B12A 30.61(5) . . ? O1A K1A B11A 102.70(5) . . ? O4A K1A B11A 96.62(5) . . ? O6A K1A B11A 83.57(5) . . ? O2A K1A B11A 110.44(5) . . ? O3A K1A B11A 118.58(5) . . ? O5A K1A B11A 92.72(5) . . ? B13A K1A B11A 30.80(5) . . ? B12A K1A B11A 30.55(6) . . ? O1A K1A H11A 104.9(4) . . ? O4A K1A H11A 91.9(4) . . ? O6A K1A H11A 70.4(4) . . ? O2A K1A H11A 127.3(4) . . ? O3A K1A H11A 130.2(4) . . ? O5A K1A H11A 75.4(4) . . ? B13A K1A H11A 47.4(4) . . ? B12A K1A H11A 46.6(4) . . ? B11A K1A H11A 18.1(4) . . ? O1A K1A H12A 124.1(4) . . ? O4A K1A H12A 73.4(4) . . ? O6A K1A H12A 132.0(4) . . ? O2A K1A H12A 85.2(4) . . ? O3A K1A H12A 70.1(4) . . ? O5A K1A H12A 114.1(4) . . ? B13A K1A H12A 46.8(4) . . ? B12A K1A H12A 19.0(4) . . ? B11A K1A H12A 48.5(4) . . ? H11A K1A H12A 62.5(5) . . ? O1A K1A H13A 67.2(4) . . ? O4A K1A H13A 131.6(4) . . ? O6A K1A H13A 93.8(4) . . ? O2A K1A H13A 63.8(4) . . ? O3A K1A H13A 103.7(4) . . ? O5A K1A H13A 137.0(4) . . ? B13A K1A H13A 18.8(4) . . ? B12A K1A H13A 46.2(4) . . ? B11A K1A H13A 48.8(4) . . ? H11A K1A H13A 63.8(6) . . ? H12A K1A H13A 58.4(5) . . ? O2B K1B O6B 119.44(4) . . ? O2B K1B O3B 59.53(4) . . ? O6B K1B O3B 157.11(4) . . ? O2B K1B O4B 119.05(4) . . ? O6B K1B O4B 117.51(4) . . ? O3B K1B O4B 59.61(4) . . ? O2B K1B O1B 58.86(4) . . ? O6B K1B O1B 60.59(4) . . ? O3B K1B O1B 113.62(4) . . ? O4B K1B O1B 160.36(4) . . ? O2B K1B O5B 158.35(4) . . ? O6B K1B O5B 58.38(4) . . ? O3B K1B O5B 113.11(4) . . ? O4B K1B O5B 59.17(4) . . ? O1B K1B O5B 114.63(4) . . ? O2B K1B B8D 113.16(5) . 2_675 ? O6B K1B B8D 82.10(5) . 2_675 ? O3B K1B B8D 120.13(5) . 2_675 ? O4B K1B B8D 94.09(5) . 2_675 ? O1B K1B B8D 104.61(5) . 2_675 ? O5B K1B B8D 88.30(5) . 2_675 ? O2B K1B B11D 92.44(5) . 2_675 ? O6B K1B B11D 112.18(5) . 2_675 ? O3B K1B B11D 90.55(5) . 2_675 ? O4B K1B B11D 85.14(5) . 2_675 ? O1B K1B B11D 114.07(5) . 2_675 ? O5B K1B B11D 108.43(5) . 2_675 ? B8D K1B B11D 30.60(6) 2_675 2_675 ? O2B K1B B5D 80.19(5) . 2_675 ? O6B K1B B5D 93.90(5) . 2_675 ? O3B K1B B5D 107.80(5) . 2_675 ? O4B K1B B5D 115.74(5) . 2_675 ? O1B K1B B5D 83.69(5) . 2_675 ? O5B K1B B5D 120.82(5) . 2_675 ? B8D K1B B5D 33.34(5) 2_675 2_675 ? B11D K1B B5D 30.73(5) 2_675 2_675 ? O6C K1C O3C 162.55(4) . . ? O6C K1C O2C 118.28(4) . . ? O3C K1C O2C 59.65(4) . . ? O6C K1C O4C 119.62(4) . . ? O3C K1C O4C 58.90(4) . . ? O2C K1C O4C 118.53(4) . . ? O6C K1C O1C 58.97(4) . . ? O3C K1C O1C 115.07(4) . . ? O2C K1C O1C 59.41(4) . . ? O4C K1C O1C 158.15(4) . . ? O6C K1C O5C 60.00(4) . . ? O3C K1C O5C 115.03(4) . . ? O2C K1C O5C 159.31(4) . . ? O4C K1C O5C 59.66(4) . . ? O1C K1C O5C 113.66(4) . . ? O6C K1C B8B 101.49(5) . . ? O3C K1C B8B 95.32(5) . . ? O2C K1C B8B 107.60(5) . . ? O4C K1C B8B 79.39(5) . . ? O1C K1C B8B 122.42(5) . . ? O5C K1C B8B 92.55(5) . . ? O6C K1C B11B 97.38(5) . . ? O3C K1C B11B 99.51(5) . . ? O2C K1C B11B 83.93(5) . . ? O4C K1C B11B 107.14(5) . . ? O1C K1C B11B 94.44(5) . . ? O5C K1C B11B 116.66(5) . . ? B8B K1C B11B 30.17(5) . . ? O6C K1C C19C 42.11(4) . . ? O3C K1C C19C 136.99(5) . . ? O2C K1C C19C 160.02(5) . . ? O4C K1C C19C 78.94(4) . . ? O1C K1C C19C 100.71(5) . . ? O5C K1C C19C 22.94(4) . . ? B8B K1C C19C 84.08(6) . . ? B11B K1C C19C 100.74(5) . . ? O6C K1C B5B 72.39(5) . . ? O3C K1C B5B 125.05(5) . . ? O2C K1C B5B 109.83(5) . . ? O4C K1C B5B 105.45(5) . . ? O1C K1C B5B 94.91(5) . . ? O5C K1C B5B 89.67(5) . . ? B8B K1C B5B 32.16(5) . . ? B11B K1C B5B 29.81(6) . . ? C19C K1C B5B 71.35(5) . . ? O6C K1C H5B 54.6(4) . . ? O3C K1C H5B 142.8(4) . . ? O2C K1C H5B 114.2(4) . . ? O4C K1C H5B 114.7(4) . . ? O1C K1C H5B 83.0(4) . . ? O5C K1C H5B 82.3(4) . . ? B8B K1C H5B 49.4(4) . . ? B11B K1C H5B 44.7(4) . . ? C19C K1C H5B 60.9(4) . . ? B5B K1C H5B 17.9(4) . . ? O6C K1C H8B 112.1(4) . . ? O3C K1C H8B 83.2(4) . . ? O2C K1C H8B 111.1(4) . . ? O4C K1C H8B 62.7(4) . . ? O1C K1C H8B 139.1(4) . . ? O5C K1C H8B 86.8(4) . . ? B8B K1C H8B 17.1(4) . . ? B11B K1C H8B 45.1(4) . . ? C19C K1C H8B 84.9(4) . . ? B5B K1C H8B 48.2(4) . . ? H5B K1C H8B 64.4(6) . . ? O6C K1C H11B 101.3(4) . . ? O3C K1C H11B 93.7(4) . . ? O2C K1C H11B 67.2(4) . . ? O4C K1C H11B 118.0(4) . . ? O1C K1C H11B 82.3(4) . . ? O5C K1C H11B 133.1(4) . . ? B8B K1C H11B 46.4(4) . . ? B11B K1C H11B 17.3(4) . . ? C19C K1C H11B 115.0(4) . . ? B5B K1C H11B 43.9(4) . . ? H5B K1C H11B 55.1(5) . . ? H8B K1C H11B 59.4(6) . . ? O3D K1D O2D 59.98(4) . . ? O3D K1D O5D 118.64(4) . . ? O2D K1D O5D 160.28(4) . . ? O3D K1D O1D 119.09(4) . . ? O2D K1D O1D 59.13(4) . . ? O5D K1D O1D 117.75(4) . . ? O3D K1D O6D 158.01(4) . . ? O2D K1D O6D 114.07(4) . . ? O5D K1D O6D 58.90(4) . . ? O1D K1D O6D 58.86(4) . . ? O3D K1D O4D 59.61(4) . . ? O2D K1D O4D 115.06(4) . . ? O5D K1D O4D 59.08(4) . . ? O1D K1D O4D 156.74(4) . . ? O6D K1D O4D 112.64(4) . . ? O3D K1D B13C 75.11(5) . . ? O2D K1D B13C 91.67(5) . . ? O5D K1D B13C 107.20(5) . . ? O1D K1D B13C 108.03(5) . . ? O6D K1D B13C 126.88(5) . . ? O4D K1D B13C 94.26(5) . . ? O3D K1D B12C 99.52(5) . . ? O2D K1D B12C 119.22(5) . . ? O5D K1D B12C 80.45(5) . . ? O1D K1D B12C 110.60(5) . . ? O6D K1D B12C 101.37(5) . . ? O4D K1D B12C 91.99(5) . . ? B13C K1D B12C 29.93(5) . . ? O3D K1D B11C 102.29(5) . . ? O2D K1D B11C 94.28(5) . . ? O5D K1D B11C 104.90(5) . . ? O1D K1D B11C 83.72(5) . . ? O6D K1D B11C 99.23(5) . . ? O4D K1D B11C 119.54(5) . . ? B13C K1D B11C 30.08(5) . . ? B12C K1D B11C 30.07(6) . . ? O3D K1D H11C 113.0(4) . . ? O2D K1D H11C 87.8(4) . . ? O5D K1D H11C 109.2(4) . . ? O1D K1D H11C 66.2(4) . . ? O6D K1D H11C 86.8(4) . . ? O4D K1D H11C 137.0(4) . . ? B13C K1D H11C 46.8(4) . . ? B12C K1D H11C 45.5(4) . . ? B11C K1D H11C 17.8(4) . . ? O3D K1D H12C 102.7(4) . . ? O2D K1D H12C 135.7(4) . . ? O5D K1D H12C 63.7(4) . . ? O1D K1D H12C 121.5(4) . . ? O6D K1D H12C 95.3(4) . . ? O4D K1D H12C 79.2(4) . . ? B13C K1D H12C 44.2(4) . . ? B12C K1D H12C 17.4(4) . . ? B11C K1D H12C 46.8(4) . . ? H11C K1D H12C 60.4(5) . . ? O3D K1D H13C 57.3(4) . . ? O2D K1D H13C 84.0(4) . . ? O5D K1D H13C 112.3(4) . . ? O1D K1D H13C 116.9(4) . . ? O6D K1D H13C 144.7(4) . . ? O4D K1D H13C 82.9(4) . . ? B13C K1D H13C 18.0(4) . . ? B12C K1D H13C 44.7(4) . . ? B11C K1D H13C 47.3(4) . . ? H11C K1D H13C 62.8(6) . . ? H12C K1D H13C 55.1(5) . . ? O2A C11A C22A 108.60(16) . . ? O2A C11A H11Z 110.0 . . ? C22A C11A H11Z 110.0 . . ? O2A C11A H11Y 110.0 . . ? C22A C11A H11Y 110.0 . . ? H11Z C11A H11Y 108.4 . . ? O2A C12A C13A 108.84(16) . . ? O2A C12A H12E 109.9 . . ? C13A C12A H12E 109.9 . . ? O2A C12A H12F 109.9 . . ? C13A C12A H12F 109.9 . . ? H12E C12A H12F 108.3 . . ? O3A C13A C12A 108.59(16) . . ? O3A C13A H13E 110.0 . . ? C12A C13A H13E 110.0 . . ? O3A C13A H13F 110.0 . . ? C12A C13A H13F 110.0 . . ? H13E C13A H13F 108.4 . . ? O3A C14A C15A 108.85(15) . . ? O3A C14A H14A 109.9 . . ? C15A C14A H14A 109.9 . . ? O3A C14A H14B 109.9 . . ? C15A C14A H14B 109.9 . . ? H14A C14A H14B 108.3 . . ? O4A C15A C14A 108.76(16) . . ? O4A C15A H15A 109.9 . . ? C14A C15A H15A 109.9 . . ? O4A C15A H15B 109.9 . . ? C14A C15A H15B 109.9 . . ? H15A C15A H15B 108.3 . . ? O4A C16A C17A 108.60(16) . . ? O4A C16A H16A 110.0 . . ? C17A C16A H16A 110.0 . . ? O4A C16A H16B 110.0 . . ? C17A C16A H16B 110.0 . . ? H16A C16A H16B 108.4 . . ? O5A C17A C16A 108.55(16) . . ? O5A C17A H17A 110.0 . . ? C16A C17A H17A 110.0 . . ? O5A C17A H17B 110.0 . . ? C16A C17A H17B 110.0 . . ? H17A C17A H17B 108.4 . . ? O5A C18A C19A 108.46(17) . . ? O5A C18A H18A 110.0 . . ? C19A C18A H18A 110.0 . . ? O5A C18A H18B 110.0 . . ? C19A C18A H18B 110.0 . . ? H18A C18A H18B 108.4 . . ? O6A C19A C18A 109.09(17) . . ? O6A C19A H19A 109.9 . . ? C18A C19A H19A 109.9 . . ? O6A C19A H19B 109.9 . . ? C18A C19A H19B 109.9 . . ? H19A C19A H19B 108.3 . . ? O6A C20A C21A 108.73(15) . . ? O6A C20A H20A 109.9 . . ? C21A C20A H20A 109.9 . . ? O6A C20A H20B 109.9 . . ? C21A C20A H20B 109.9 . . ? H20A C20A H20B 108.3 . . ? O1A C21A C20A 107.54(16) . . ? O1A C21A H21A 110.2 . . ? C20A C21A H21A 110.2 . . ? O1A C21A H21B 110.2 . . ? C20A C21A H21B 110.2 . . ? H21A C21A H21B 108.5 . . ? O1A C22A C11A 108.15(16) . . ? O1A C22A H22A 110.1 . . ? C11A C22A H22A 110.1 . . ? O1A C22A H22B 110.1 . . ? C11A C22A H22B 110.1 . . ? H22A C22A H22B 108.4 . . ? C22A O1A C21A 111.46(15) . . ? C22A O1A K1A 115.52(11) . . ? C21A O1A K1A 110.91(11) . . ? C12A O2A C11A 111.96(15) . . ? C12A O2A K1A 116.70(11) . . ? C11A O2A K1A 116.90(11) . . ? C13A O3A C14A 111.62(14) . . ? C13A O3A K1A 110.27(11) . . ? C14A O3A K1A 108.98(11) . . ? C16A O4A C15A 111.22(15) . . ? C16A O4A K1A 119.37(11) . . ? C15A O4A K1A 119.23(11) . . ? C18A O5A C17A 111.94(15) . . ? C18A O5A K1A 113.02(11) . . ? C17A O5A K1A 109.26(11) . . ? C19A O6A C20A 112.32(15) . . ? C19A O6A K1A 117.90(11) . . ? C20A O6A K1A 115.49(11) . . ? O1B C11B C12B 108.22(16) . . ? O1B C11B H11E 110.1 . . ? C12B C11B H11E 110.1 . . ? O1B C11B H11F 110.1 . . ? C12B C11B H11F 110.1 . . ? H11E C11B H11F 108.4 . . ? O2B C12B C11B 108.41(16) . . ? O2B C12B H12G 110.0 . . ? C11B C12B H12G 110.0 . . ? O2B C12B H12H 110.0 . . ? C11B C12B H12H 110.0 . . ? H12G C12B H12H 108.4 . . ? O2B C13B C14B 108.41(16) . . ? O2B C13B H13G 110.0 . . ? C14B C13B H13G 110.0 . . ? O2B C13B H13H 110.0 . . ? C14B C13B H13H 110.0 . . ? H13G C13B H13H 108.4 . . ? O3B C14B C13B 109.03(16) . . ? O3B C14B H14C 109.9 . . ? C13B C14B H14C 109.9 . . ? O3B C14B H14D 109.9 . . ? C13B C14B H14D 109.9 . . ? H14C C14B H14D 108.3 . . ? O3B C15B C16B 109.02(18) . . ? O3B C15B H15C 109.9 . . ? C16B C15B H15C 109.9 . . ? O3B C15B H15D 109.9 . . ? C16B C15B H15D 109.9 . . ? H15C C15B H15D 108.3 . . ? O4B C16B C15B 109.94(17) . . ? O4B C16B H16C 109.7 . . ? C15B C16B H16C 109.7 . . ? O4B C16B H16D 109.7 . . ? C15B C16B H16D 109.7 . . ? H16C C16B H16D 108.2 . . ? O4B C17B C18B 109.64(16) . . ? O4B C17B H17C 109.7 . . ? C18B C17B H17C 109.7 . . ? O4B C17B H17D 109.7 . . ? C18B C17B H17D 109.7 . . ? H17C C17B H17D 108.2 . . ? O5B C18B C17B 108.05(17) . . ? O5B C18B H18C 110.1 . . ? C17B C18B H18C 110.1 . . ? O5B C18B H18D 110.1 . . ? C17B C18B H18D 110.1 . . ? H18C C18B H18D 108.4 . . ? O5B C19B C20B 108.42(16) . . ? O5B C19B H19C 110.0 . . ? C20B C19B H19C 110.0 . . ? O5B C19B H19D 110.0 . . ? C20B C19B H19D 110.0 . . ? H19C C19B H19D 108.4 . . ? O6B C20B C19B 108.53(16) . . ? O6B C20B H20C 110.0 . . ? C19B C20B H20C 110.0 . . ? O6B C20B H20D 110.0 . . ? C19B C20B H20D 110.0 . . ? H20C C20B H20D 108.4 . . ? O6B C21B C22B 109.35(16) . . ? O6B C21B H21C 109.8 . . ? C22B C21B H21C 109.8 . . ? O6B C21B H21D 109.8 . . ? C22B C21B H21D 109.8 . . ? H21C C21B H21D 108.3 . . ? O1B C22B C21B 108.55(16) . . ? O1B C22B H22C 110.0 . . ? C21B C22B H22C 110.0 . . ? O1B C22B H22D 110.0 . . ? C21B C22B H22D 110.0 . . ? H22C C22B H22D 108.4 . . ? C11B O1B C22B 111.76(14) . . ? C11B O1B K1B 111.41(11) . . ? C22B O1B K1B 108.94(11) . . ? C13B O2B C12B 111.75(15) . . ? C13B O2B K1B 118.17(11) . . ? C12B O2B K1B 119.47(11) . . ? C15B O3B C14B 111.76(16) . . ? C15B O3B K1B 112.63(11) . . ? C14B O3B K1B 111.79(11) . . ? C16B O4B C17B 111.73(15) . . ? C16B O4B K1B 116.38(12) . . ? C17B O4B K1B 117.22(11) . . ? C18B O5B C19B 111.53(15) . . ? C18B O5B K1B 110.94(11) . . ? C19B O5B K1B 114.53(11) . . ? C21B O6B C20B 111.70(15) . . ? C21B O6B K1B 114.85(11) . . ? C20B O6B K1B 118.53(11) . . ? O1C C11C C12C 108.62(17) . . ? O1C C11C H11G 110.0 . . ? C12C C11C H11G 110.0 . . ? O1C C11C H11H 110.0 . . ? C12C C11C H11H 110.0 . . ? H11G C11C H11H 108.3 . . ? O2C C12C C11C 109.17(17) . . ? O2C C12C H12I 109.8 . . ? C11C C12C H12I 109.8 . . ? O2C C12C H12J 109.8 . . ? C11C C12C H12J 109.8 . . ? H12I C12C H12J 108.3 . . ? O2C C13C C14C 109.29(17) . . ? O2C C13C H13I 109.8 . . ? C14C C13C H13I 109.8 . . ? O2C C13C H13J 109.8 . . ? C14C C13C H13J 109.8 . . ? H13I C13C H13J 108.3 . . ? O3C C14C C13C 108.18(17) . . ? O3C C14C H14E 110.1 . . ? C13C C14C H14E 110.1 . . ? O3C C14C H14F 110.1 . . ? C13C C14C H14F 110.1 . . ? H14E C14C H14F 108.4 . . ? O3C C15C C16C 108.14(16) . . ? O3C C15C H15E 110.1 . . ? C16C C15C H15E 110.1 . . ? O3C C15C H15F 110.1 . . ? C16C C15C H15F 110.1 . . ? H15E C15C H15F 108.4 . . ? O4C C16C C15C 108.48(16) . . ? O4C C16C H16E 110.0 . . ? C15C C16C H16E 110.0 . . ? O4C C16C H16F 110.0 . . ? C15C C16C H16F 110.0 . . ? H16E C16C H16F 108.4 . . ? O4C C17C C18C 108.32(16) . . ? O4C C17C H17E 110.0 . . ? C18C C17C H17E 110.0 . . ? O4C C17C H17F 110.0 . . ? C18C C17C H17F 110.0 . . ? H17E C17C H17F 108.4 . . ? O5C C18C C17C 109.14(15) . . ? O5C C18C H18E 109.9 . . ? C17C C18C H18E 109.9 . . ? O5C C18C H18F 109.9 . . ? C17C C18C H18F 109.9 . . ? H18E C18C H18F 108.3 . . ? O5C C19C C20C 109.11(16) . . ? O5C C19C K1C 50.98(9) . . ? C20C C19C K1C 83.92(11) . . ? O5C C19C H19E 109.9 . . ? C20C C19C H19E 109.9 . . ? K1C C19C H19E 160.3 . . ? O5C C19C H19F 109.9 . . ? C20C C19C H19F 109.9 . . ? K1C C19C H19F 78.5 . . ? H19E C19C H19F 108.3 . . ? O6C C20C C19C 108.59(16) . . ? O6C C20C H20E 110.0 . . ? C19C C20C H20E 110.0 . . ? O6C C20C H20F 110.0 . . ? C19C C20C H20F 110.0 . . ? H20E C20C H20F 108.4 . . ? O6C C21C C22C 108.60(17) . . ? O6C C21C H21E 110.0 . . ? C22C C21C H21E 110.0 . . ? O6C C21C H21F 110.0 . . ? C22C C21C H21F 110.0 . . ? H21E C21C H21F 108.4 . . ? O1C C22C C21C 109.06(17) . . ? O1C C22C H22E 109.9 . . ? C21C C22C H22E 109.9 . . ? O1C C22C H22F 109.9 . . ? C21C C22C H22F 109.9 . . ? H22E C22C H22F 108.3 . . ? C22C O1C C11C 111.51(15) . . ? C22C O1C K1C 113.13(11) . . ? C11C O1C K1C 113.16(11) . . ? C13C O2C C12C 112.69(15) . . ? C13C O2C K1C 116.56(11) . . ? C12C O2C K1C 117.13(12) . . ? C14C O3C C15C 112.11(15) . . ? C14C O3C K1C 112.30(11) . . ? C15C O3C K1C 112.96(11) . . ? C16C O4C C17C 112.69(15) . . ? C16C O4C K1C 118.15(11) . . ? C17C O4C K1C 116.48(11) . . ? C18C O5C C19C 111.11(14) . . ? C18C O5C K1C 111.73(11) . . ? C19C O5C K1C 106.08(11) . . ? C20C O6C C21C 112.15(15) . . ? C20C O6C K1C 119.32(11) . . ? C21C O6C K1C 120.32(11) . . ? O1D C11D C12D 108.67(16) . . ? O1D C11D H11I 110.0 . . ? C12D C11D H11I 110.0 . . ? O1D C11D H11J 110.0 . . ? C12D C11D H11J 110.0 . . ? H11I C11D H11J 108.3 . . ? O2D C12D C11D 107.72(17) . . ? O2D C12D H12K 110.2 . . ? C11D C12D H12K 110.2 . . ? O2D C12D H12L 110.2 . . ? C11D C12D H12L 110.2 . . ? H12K C12D H12L 108.5 . . ? O2D C13D C14D 108.18(16) . . ? O2D C13D H13K 110.1 . . ? C14D C13D H13K 110.1 . . ? O2D C13D H13L 110.1 . . ? C14D C13D H13L 110.1 . . ? H13K C13D H13L 108.4 . . ? O3D C14D C13D 108.09(16) . . ? O3D C14D H14G 110.1 . . ? C13D C14D H14G 110.1 . . ? O3D C14D H14H 110.1 . . ? C13D C14D H14H 110.1 . . ? H14G C14D H14H 108.4 . . ? O3D C15D C16D 107.86(16) . . ? O3D C15D H15G 110.1 . . ? C16D C15D H15G 110.1 . . ? O3D C15D H15H 110.1 . . ? C16D C15D H15H 110.1 . . ? H15G C15D H15H 108.4 . . ? O4D C16D C15D 109.45(16) . . ? O4D C16D H16G 109.8 . . ? C15D C16D H16G 109.8 . . ? O4D C16D H16H 109.8 . . ? C15D C16D H16H 109.8 . . ? H16G C16D H16H 108.2 . . ? O4D C17D C18D 108.82(16) . . ? O4D C17D H17G 109.9 . . ? C18D C17D H17G 109.9 . . ? O4D C17D H17H 109.9 . . ? C18D C17D H17H 109.9 . . ? H17G C17D H17H 108.3 . . ? O5D C18D C17D 108.84(16) . . ? O5D C18D H18G 109.9 . . ? C17D C18D H18G 109.9 . . ? O5D C18D H18H 109.9 . . ? C17D C18D H18H 109.9 . . ? H18G C18D H18H 108.3 . . ? O5D C19D C20D 109.24(17) . . ? O5D C19D H19G 109.8 . . ? C20D C19D H19G 109.8 . . ? O5D C19D H19H 109.8 . . ? C20D C19D H19H 109.8 . . ? H19G C19D H19H 108.3 . . ? O6D C20D C19D 109.47(17) . . ? O6D C20D H20G 109.8 . . ? C19D C20D H20G 109.8 . . ? O6D C20D H20H 109.8 . . ? C19D C20D H20H 109.8 . . ? H20G C20D H20H 108.2 . . ? O6D C21D C22D 108.64(17) . . ? O6D C21D H21G 110.0 . . ? C22D C21D H21G 110.0 . . ? O6D C21D H21H 110.0 . . ? C22D C21D H21H 110.0 . . ? H21G C21D H21H 108.3 . . ? O1D C22D C21D 109.01(16) . . ? O1D C22D H22G 109.9 . . ? C21D C22D H22G 109.9 . . ? O1D C22D H22H 109.9 . . ? C21D C22D H22H 109.9 . . ? H22G C22D H22H 108.3 . . ? C11D O1D C22D 112.69(15) . . ? C11D O1D K1D 116.13(11) . . ? C22D O1D K1D 117.82(11) . . ? C12D O2D C13D 112.04(15) . . ? C12D O2D K1D 114.57(11) . . ? C13D O2D K1D 109.98(11) . . ? C14D O3D C15D 112.85(14) . . ? C14D O3D K1D 117.99(11) . . ? C15D O3D K1D 118.83(11) . . ? C17D O4D C16D 111.77(15) . . ? C17D O4D K1D 109.55(11) . . ? C16D O4D K1D 109.49(11) . . ? C19D O5D C18D 111.88(15) . . ? C19D O5D K1D 118.93(11) . . ? C18D O5D K1D 118.43(11) . . ? C20D O6D C21D 111.01(15) . . ? C20D O6D K1D 112.10(11) . . ? C21D O6D K1D 112.41(11) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.877 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.067 data_x80799 _database_code_depnum_ccdc_archive 'CCDC 663040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H24 B20 Ti, 2(C12 H24 K O6), 2(C H Cl3)' _chemical_formula_sum 'C30 H74 B20 Cl6 K2 O12 Ti' _chemical_formula_weight 1181.89 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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 13.6324(11) _cell_length_b 15.6852(13) _cell_length_c 27.643(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5910.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9937 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 27.57 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 104648 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.88 _reflns_number_total 15426 _reflns_number_gt 10892 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0967P)^2^+8.8928P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.39(4) _refine_ls_number_reflns 15426 _refine_ls_number_parameters 688 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1659 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti4 Ti 0.75844(5) 0.99889(5) 0.12421(3) 0.01918(14) Uani 1 1 d . . . C1A C 0.8408(4) 1.0625(3) 0.18275(15) 0.0247(9) Uani 1 1 d . . . H1A H 0.824(4) 1.046(3) 0.2138(19) 0.030 Uiso 1 1 d . . . B2A B 0.7797(4) 1.1390(3) 0.15935(19) 0.0254(10) Uani 1 1 d . . . H2A H 0.7168 1.1656 0.1806 0.031 Uiso 1 1 calc R . . B3A B 0.9218(4) 1.0068(4) 0.15612(18) 0.0266(11) Uani 1 1 d . . . H3A H 0.953(4) 0.948(3) 0.1775(18) 0.032 Uiso 1 1 d . . . B5A B 0.9157(7) 1.1468(7) 0.1726(3) 0.080(4) Uani 1 1 d . . . H5A H 0.9736 1.1475 0.2013 0.096 Uiso 1 1 calc R . . B6A B 0.7738(4) 1.1423(4) 0.0951(2) 0.0290(12) Uani 1 1 d . . . H6A H 0.713(4) 1.169(3) 0.0756(19) 0.035 Uiso 1 1 d . . . B7A B 0.9217(4) 1.0086(4) 0.09154(19) 0.0256(11) Uani 1 1 d . . . H7A H 0.9449 0.9489 0.0725 0.031 Uiso 1 1 calc R . . B8A B 1.0077(3) 1.0706(3) 0.1230(2) 0.0270(10) Uani 1 1 d . . . H8A H 1.087(4) 1.054(3) 0.1255(19) 0.032 Uiso 1 1 d . . . B9A B 0.8563(4) 1.2106(3) 0.1263(2) 0.0262(10) Uani 1 1 d . . . H9A H 0.838(4) 1.277(3) 0.1284(18) 0.031 Uiso 1 1 d . . . C10A C 0.8395(3) 1.0708(3) 0.06654(15) 0.0303(11) Uani 1 1 d . . . H10A H 0.8058 1.0404 0.0339 0.036 Uiso 1 1 calc R . . B11A B 0.9753(4) 1.1776(4) 0.1192(4) 0.062(2) Uani 1 1 d . . . H11A H 1.038(5) 1.220(4) 0.121(3) 0.074 Uiso 1 1 d . . . B12A B 0.8788(5) 1.1858(5) 0.0685(3) 0.0476(16) Uani 1 1 d . . . H12A H 0.875(5) 1.237(4) 0.034(2) 0.057 Uiso 1 1 d . . . B13A B 0.9568(7) 1.1094(5) 0.0699(3) 0.078(4) Uani 1 1 d . . . H13A H 1.0038 1.1170 0.0369 0.093 Uiso 1 1 calc R . . C1B C 0.6005(3) 1.0159(3) 0.12173(16) 0.0216(8) Uani 1 1 d . . . H1B H 0.567(4) 1.070(3) 0.1243(19) 0.026 Uiso 1 1 d . . . B2B B 0.6128(3) 0.9745(3) 0.17327(17) 0.0204(9) Uani 1 1 d . . . H2B H 0.5963 1.0166 0.2049 0.024 Uiso 1 1 calc R . . B3B B 0.6197(4) 0.9694(4) 0.07283(17) 0.0263(11) Uani 1 1 d . . . H3B H 0.599(4) 1.004(3) 0.0408(18) 0.032 Uiso 1 1 d . . . B5B B 0.5264(3) 0.9244(3) 0.1229(2) 0.0237(9) Uani 1 1 d . . . H5B H 0.446(4) 0.947(3) 0.1249(18) 0.028 Uiso 1 1 d . . . B6B B 0.7014(3) 0.8928(3) 0.17911(18) 0.0216(10) Uani 1 1 d . . . H6B H 0.752(4) 0.887(3) 0.2096(17) 0.026 Uiso 1 1 d . . . B7B B 0.7075(4) 0.8856(4) 0.07204(19) 0.0295(12) Uani 1 1 d . . . H7B H 0.7571 0.8829 0.0398 0.035 Uiso 1 1 calc R . . B8B B 0.5810(4) 0.8605(4) 0.06963(19) 0.0275(11) Uani 1 1 d . . . H8B H 0.541(4) 0.848(3) 0.0328(18) 0.033 Uiso 1 1 d . . . B9B B 0.5749(4) 0.8648(4) 0.17849(18) 0.0234(10) Uani 1 1 d . . . H9B H 0.5297 0.8497 0.2112 0.028 Uiso 1 1 calc R . . C10B C 0.7453(3) 0.8537(3) 0.12657(18) 0.0271(9) Uani 1 1 d . . . H10B H 0.811(4) 0.824(3) 0.1361(18) 0.033 Uiso 1 1 d . . . B11B B 0.5512(3) 0.8096(3) 0.1244(2) 0.0253(10) Uani 1 1 d . . . H11B H 0.489(4) 0.765(3) 0.1226(18) 0.030 Uiso 1 1 d . . . B12B B 0.6611(4) 0.7912(4) 0.1576(2) 0.0299(12) Uani 1 1 d . . . H12B H 0.686(4) 0.733(4) 0.1799(18) 0.036 Uiso 1 1 d . . . B13B B 0.6639(4) 0.7875(4) 0.0943(2) 0.0277(11) Uani 1 1 d . . . H13B H 0.692(4) 0.727(3) 0.0796(18) 0.033 Uiso 1 1 d . . . K1 K 0.62231(7) 0.91590(7) 0.29442(3) 0.0253(2) Uani 1 1 d . . . O1 O 0.5946(2) 1.0931(2) 0.31335(11) 0.0268(7) Uani 1 1 d . . . C11 C 0.6721(4) 1.1437(3) 0.29422(17) 0.0303(10) Uani 1 1 d . . . H11C H 0.6613 1.2045 0.3022 0.036 Uiso 1 1 calc R . . H11D H 0.6746 1.1378 0.2586 0.036 Uiso 1 1 calc R . . C12 C 0.7664(4) 1.1135(3) 0.31615(17) 0.0326(11) Uani 1 1 d . . . H12C H 0.8211 1.1507 0.3057 0.039 Uiso 1 1 calc R . . H12D H 0.7621 1.1157 0.3519 0.039 Uiso 1 1 calc R . . O2 O 0.7838(2) 1.0279(2) 0.30072(11) 0.0277(7) Uani 1 1 d . . . C13 C 0.8756(3) 0.9961(4) 0.31728(16) 0.0330(11) Uani 1 1 d . . . H13C H 0.8759 0.9929 0.3530 0.040 Uiso 1 1 calc R . . H13D H 0.9292 1.0347 0.3070 0.040 Uiso 1 1 calc R . . C14 C 0.8912(3) 0.9084(4) 0.29603(17) 0.0328(11) Uani 1 1 d . . . H14A H 0.8900 0.9113 0.2603 0.039 Uiso 1 1 calc R . . H14B H 0.9557 0.8856 0.3062 0.039 Uiso 1 1 calc R . . O3 O 0.8143(2) 0.8546(2) 0.31304(12) 0.0314(7) Uani 1 1 d . . . C15 C 0.8231(4) 0.7688(3) 0.2952(2) 0.0409(13) Uani 1 1 d . . . H15A H 0.8917 0.7487 0.2980 0.049 Uiso 1 1 calc R . . H15B H 0.8035 0.7661 0.2607 0.049 Uiso 1 1 calc R . . C16 C 0.7566(4) 0.7146(4) 0.3252(2) 0.0449(14) Uani 1 1 d . . . H16A H 0.7638 0.6539 0.3160 0.054 Uiso 1 1 calc R . . H16B H 0.7733 0.7207 0.3599 0.054 Uiso 1 1 calc R . . O4 O 0.6581(2) 0.7426(2) 0.31666(14) 0.0393(9) Uani 1 1 d . . . C17 C 0.5904(4) 0.6998(4) 0.3461(3) 0.0544(18) Uani 1 1 d . . . H17A H 0.6047 0.7116 0.3806 0.065 Uiso 1 1 calc R . . H17B H 0.5956 0.6375 0.3408 0.065 Uiso 1 1 calc R . . C18 C 0.4889(4) 0.7295(3) 0.3339(3) 0.0563(18) Uani 1 1 d . . . H18A H 0.4762 0.7211 0.2990 0.068 Uiso 1 1 calc R . . H18B H 0.4401 0.6960 0.3523 0.068 Uiso 1 1 calc R . . O5 O 0.4803(2) 0.8173(2) 0.34583(13) 0.0300(7) Uani 1 1 d . . . C19 C 0.3825(4) 0.8439(3) 0.3378(2) 0.0380(12) Uani 1 1 d . . . H19A H 0.3372 0.8101 0.3582 0.046 Uiso 1 1 calc R . . H19B H 0.3645 0.8349 0.3035 0.046 Uiso 1 1 calc R . . C20 C 0.3746(4) 0.9371(3) 0.3505(2) 0.0402(13) Uani 1 1 d . . . H20A H 0.3060 0.9566 0.3466 0.048 Uiso 1 1 calc R . . H20B H 0.3944 0.9463 0.3845 0.048 Uiso 1 1 calc R . . O6 O 0.4370(2) 0.9832(2) 0.31907(13) 0.0312(7) Uani 1 1 d . . . C21 C 0.4247(4) 1.0730(3) 0.3245(2) 0.0345(11) Uani 1 1 d . . . H21A H 0.4314 1.0892 0.3589 0.041 Uiso 1 1 calc R . . H21B H 0.3586 1.0901 0.3132 0.041 Uiso 1 1 calc R . . C22 C 0.5015(4) 1.1164(3) 0.29497(18) 0.0301(10) Uani 1 1 d . . . H22A H 0.4959 1.0989 0.2607 0.036 Uiso 1 1 calc R . . H22B H 0.4930 1.1790 0.2968 0.036 Uiso 1 1 calc R . . K2 K 0.64263(7) 0.91569(7) -0.04592(4) 0.0297(2) Uani 1 1 d . . . O7 O 0.6786(2) 0.7423(2) -0.06868(14) 0.0362(8) Uani 1 1 d . . . C23 C 0.6130(4) 0.6991(4) -0.1000(3) 0.0485(15) Uani 1 1 d . . . H23A H 0.6196 0.6367 -0.0956 0.058 Uiso 1 1 calc R . . H23B H 0.6285 0.7129 -0.1341 0.058 Uiso 1 1 calc R . . C24 C 0.5112(4) 0.7260(4) -0.0885(3) 0.062(2) Uani 1 1 d . . . H24A H 0.4641 0.6936 -0.1086 0.075 Uiso 1 1 calc R . . H24B H 0.4966 0.7142 -0.0541 0.075 Uiso 1 1 calc R . . O8 O 0.5014(3) 0.8151(2) -0.09794(17) 0.0452(10) Uani 1 1 d . . . C25 C 0.4038(4) 0.8434(4) -0.0892(3) 0.060(2) Uani 1 1 d . . . H25A H 0.3868 0.8343 -0.0548 0.072 Uiso 1 1 calc R . . H25B H 0.3575 0.8101 -0.1093 0.072 Uiso 1 1 calc R . . C26 C 0.3952(4) 0.9354(4) -0.1013(2) 0.0485(15) Uani 1 1 d . . . H26A H 0.4144 0.9450 -0.1354 0.058 Uiso 1 1 calc R . . H26B H 0.3265 0.9543 -0.0972 0.058 Uiso 1 1 calc R . . O9 O 0.4578(3) 0.9832(2) -0.07009(13) 0.0384(9) Uani 1 1 d . . . C27 C 0.4461(4) 1.0730(4) -0.0771(2) 0.0450(15) Uani 1 1 d . . . H27A H 0.3793 1.0908 -0.0674 0.054 Uiso 1 1 calc R . . H27B H 0.4554 1.0874 -0.1117 0.054 Uiso 1 1 calc R . . C28 C 0.5203(5) 1.1177(4) -0.0473(2) 0.0530(17) Uani 1 1 d . . . H28A H 0.5121 1.1801 -0.0504 0.064 Uiso 1 1 calc R . . H28B H 0.5121 1.1020 -0.0128 0.064 Uiso 1 1 calc R . . O10 O 0.6163(3) 1.0927(2) -0.06401(12) 0.0381(8) Uani 1 1 d . . . C29 C 0.6937(5) 1.1441(4) -0.0453(2) 0.0511(17) Uani 1 1 d . . . H29A H 0.6960 1.1392 -0.0096 0.061 Uiso 1 1 calc R . . H29B H 0.6824 1.2046 -0.0538 0.061 Uiso 1 1 calc R . . C30 C 0.7874(5) 1.1145(4) -0.0665(2) 0.0456(14) Uani 1 1 d . . . H30A H 0.7842 1.1174 -0.1022 0.055 Uiso 1 1 calc R . . H30B H 0.8418 1.1515 -0.0554 0.055 Uiso 1 1 calc R . . O11 O 0.8038(3) 1.0291(2) -0.05137(11) 0.0360(8) Uani 1 1 d . . . C31 C 0.8963(4) 0.9952(4) -0.06723(18) 0.0406(13) Uani 1 1 d . . . H31A H 0.9502 1.0334 -0.0569 0.049 Uiso 1 1 calc R . . H31B H 0.8973 0.9913 -0.1030 0.049 Uiso 1 1 calc R . . C32 C 0.9101(3) 0.9092(4) -0.04576(18) 0.0388(13) Uani 1 1 d . . . H32A H 0.9752 0.8862 -0.0548 0.047 Uiso 1 1 calc R . . H32B H 0.9065 0.9126 -0.0100 0.047 Uiso 1 1 calc R . . O12 O 0.8349(2) 0.8553(2) -0.06364(11) 0.0296(7) Uani 1 1 d . . . C33 C 0.8411(4) 0.7710(4) -0.04505(18) 0.0361(12) Uani 1 1 d . . . H33A H 0.8189 0.7698 -0.0110 0.043 Uiso 1 1 calc R . . H33B H 0.9099 0.7507 -0.0463 0.043 Uiso 1 1 calc R . . C34 C 0.7779(4) 0.7152(4) -0.07500(19) 0.0368(12) Uani 1 1 d . . . H34A H 0.7968 0.7197 -0.1095 0.044 Uiso 1 1 calc R . . H34B H 0.7852 0.6551 -0.0648 0.044 Uiso 1 1 calc R . . C1S C 0.6689(4) 0.5522(5) 0.7803(2) 0.0590(19) Uani 1 1 d . . . H1S H 0.6175 0.5426 0.8055 0.071 Uiso 1 1 calc R . . Cl1 Cl 0.64682(14) 0.65222(17) 0.75272(7) 0.0847(7) Uani 1 1 d . . . Cl2 Cl 0.78409(12) 0.55353(15) 0.80877(6) 0.0693(5) Uani 1 1 d . . . Cl3 Cl 0.6611(2) 0.4699(2) 0.73776(9) 0.1258(12) Uani 1 1 d . . . C2S C 0.2012(6) 0.0521(4) 1.0209(2) 0.0592(18) Uani 1 1 d . . . H2S H 0.1503 0.0609 1.0464 0.071 Uiso 1 1 calc R . . Cl4 Cl 0.19964(17) 0.14044(11) 0.98167(7) 0.0759(6) Uani 1 1 d . . . Cl5 Cl 0.31675(18) 0.04026(15) 1.04949(7) 0.0842(7) Uani 1 1 d . . . Cl6 Cl 0.17242(11) -0.04152(10) 0.98877(6) 0.0487(3) 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 Ti4 0.0157(3) 0.0218(3) 0.0201(3) -0.0054(3) 0.0032(3) -0.0059(3) C1A 0.037(2) 0.023(2) 0.0135(18) -0.0017(16) 0.0018(17) 0.0007(19) B2A 0.023(2) 0.027(3) 0.027(3) -0.002(2) 0.0025(19) -0.001(2) B3A 0.026(2) 0.031(3) 0.023(2) 0.011(2) -0.0062(19) -0.014(2) B5A 0.081(6) 0.111(8) 0.047(4) 0.054(5) -0.043(4) -0.077(6) B6A 0.023(2) 0.036(3) 0.028(3) 0.011(2) -0.007(2) -0.013(2) B7A 0.020(2) 0.031(3) 0.026(2) 0.005(2) 0.0025(19) -0.001(2) B8A 0.019(2) 0.034(3) 0.027(2) 0.002(2) 0.000(2) -0.0048(19) B9A 0.025(2) 0.023(2) 0.031(2) 0.004(2) -0.001(2) -0.0067(18) C10A 0.019(2) 0.056(3) 0.0162(19) 0.000(2) 0.0049(16) 0.007(2) B11A 0.018(3) 0.035(3) 0.132(8) -0.023(5) 0.007(4) -0.011(2) B12A 0.042(4) 0.051(4) 0.050(4) 0.004(3) 0.004(3) 0.001(3) B13A 0.109(7) 0.069(5) 0.056(4) 0.046(4) -0.057(5) -0.078(5) C1B 0.0200(18) 0.022(2) 0.0231(19) -0.0001(19) -0.0004(17) -0.0004(15) B2B 0.021(2) 0.021(2) 0.020(2) -0.0018(18) 0.0011(18) -0.0016(18) B3B 0.028(2) 0.032(3) 0.019(2) 0.004(2) -0.006(2) -0.014(2) B5B 0.018(2) 0.026(2) 0.027(2) 0.001(2) -0.004(2) -0.0024(18) B6B 0.017(2) 0.021(2) 0.026(2) 0.0001(19) 0.0002(18) -0.0024(18) B7B 0.028(2) 0.036(3) 0.024(2) -0.012(2) 0.009(2) -0.014(2) B8B 0.030(3) 0.030(3) 0.023(2) 0.000(2) 0.001(2) -0.017(2) B9B 0.019(2) 0.027(3) 0.024(2) 0.004(2) -0.0030(18) -0.003(2) C10B 0.0206(19) 0.028(2) 0.032(2) -0.007(2) 0.001(2) 0.0000(17) B11B 0.020(2) 0.027(2) 0.029(2) -0.003(2) -0.001(2) -0.0092(18) B12B 0.019(2) 0.025(3) 0.046(3) -0.003(2) -0.007(2) -0.006(2) B13B 0.022(2) 0.025(3) 0.036(3) -0.009(2) 0.001(2) -0.005(2) K1 0.0244(4) 0.0267(5) 0.0248(4) -0.0001(4) -0.0007(4) 0.0040(4) O1 0.0265(15) 0.0278(17) 0.0260(15) 0.0021(14) -0.0009(13) 0.0010(13) C11 0.036(2) 0.029(2) 0.026(2) -0.0023(19) 0.007(2) -0.004(2) C12 0.031(2) 0.041(3) 0.026(2) -0.004(2) 0.001(2) -0.011(2) O2 0.0245(15) 0.0353(18) 0.0233(15) 0.0008(13) -0.0036(12) -0.0032(13) C13 0.024(2) 0.052(3) 0.023(2) 0.001(2) -0.0022(17) -0.005(2) C14 0.0174(19) 0.056(3) 0.025(2) 0.004(2) 0.0001(17) 0.005(2) O3 0.0211(15) 0.040(2) 0.0333(17) 0.0037(15) 0.0018(14) 0.0056(14) C15 0.033(3) 0.036(3) 0.053(3) 0.001(3) 0.003(2) 0.021(2) C16 0.029(3) 0.038(3) 0.068(4) 0.013(3) 0.002(3) 0.014(2) O4 0.0260(17) 0.0278(18) 0.064(2) 0.0040(17) 0.0004(17) 0.0081(15) C17 0.034(3) 0.026(3) 0.104(5) 0.022(3) 0.004(3) 0.001(2) C18 0.035(3) 0.019(3) 0.115(6) 0.003(3) -0.005(3) 0.000(2) O5 0.0202(15) 0.0184(16) 0.051(2) 0.0015(14) -0.0019(14) 0.0001(12) C19 0.022(2) 0.029(3) 0.064(3) -0.001(2) -0.006(2) 0.000(2) C20 0.026(2) 0.030(3) 0.064(3) -0.007(2) 0.011(2) 0.002(2) O6 0.0252(15) 0.0212(17) 0.047(2) -0.0024(15) 0.0034(14) 0.0022(13) C21 0.028(2) 0.023(3) 0.052(3) -0.006(2) 0.005(2) 0.005(2) C22 0.034(2) 0.021(2) 0.035(3) -0.004(2) -0.005(2) 0.0065(19) K2 0.0273(5) 0.0377(6) 0.0241(5) 0.0018(4) 0.0031(4) 0.0061(4) O7 0.0240(16) 0.0325(19) 0.052(2) 0.0003(17) 0.0056(16) 0.0054(14) C23 0.043(3) 0.027(3) 0.075(4) 0.004(3) -0.005(3) -0.002(2) C24 0.035(3) 0.028(3) 0.124(6) 0.013(4) -0.007(4) -0.007(3) O8 0.0200(16) 0.033(2) 0.082(3) 0.009(2) -0.0018(18) -0.0040(15) C25 0.019(2) 0.049(4) 0.113(6) 0.020(4) -0.003(3) -0.009(2) C26 0.023(2) 0.059(4) 0.064(4) 0.023(3) 0.000(2) 0.007(2) O9 0.0340(18) 0.043(2) 0.0378(19) 0.0139(17) 0.0074(15) 0.0203(16) C27 0.047(3) 0.043(3) 0.045(3) 0.015(3) 0.012(3) 0.031(3) C28 0.077(5) 0.041(3) 0.041(3) 0.002(3) 0.023(3) 0.026(3) O10 0.050(2) 0.035(2) 0.0296(17) -0.0048(16) 0.0080(16) 0.0060(18) C29 0.090(5) 0.034(3) 0.030(3) -0.004(2) -0.008(3) 0.005(3) C30 0.061(4) 0.045(3) 0.031(3) 0.002(2) -0.008(3) -0.021(3) O11 0.040(2) 0.047(2) 0.0212(15) 0.0005(15) 0.0002(14) -0.0127(16) C31 0.032(2) 0.060(4) 0.030(2) -0.010(3) 0.005(2) -0.018(3) C32 0.022(2) 0.066(4) 0.028(2) 0.000(3) 0.0004(19) -0.004(2) O12 0.0190(15) 0.043(2) 0.0270(16) 0.0009(15) -0.0009(13) 0.0025(14) C33 0.029(2) 0.048(3) 0.032(2) 0.003(2) 0.005(2) 0.015(2) C34 0.029(2) 0.042(3) 0.040(3) 0.008(2) 0.007(2) 0.017(2) C1S 0.029(3) 0.115(6) 0.033(3) -0.007(3) 0.001(2) -0.010(3) Cl1 0.0488(10) 0.1329(19) 0.0723(12) 0.0435(12) -0.0157(9) -0.0260(11) Cl2 0.0397(8) 0.1117(16) 0.0564(9) 0.0024(10) -0.0128(7) -0.0069(9) Cl3 0.111(2) 0.189(3) 0.0771(14) -0.0665(18) -0.0460(14) 0.041(2) C2S 0.083(5) 0.047(3) 0.048(3) -0.001(3) 0.038(3) -0.008(3) Cl4 0.1086(15) 0.0423(8) 0.0769(12) 0.0034(8) 0.0589(12) 0.0049(9) Cl5 0.1049(16) 0.0937(15) 0.0541(10) -0.0077(10) -0.0088(10) -0.0471(13) Cl6 0.0414(7) 0.0468(8) 0.0578(8) -0.0026(7) -0.0040(6) -0.0041(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 Ti4 C1B 2.171(4) . ? Ti4 C1A 2.208(4) . ? Ti4 C10A 2.244(5) . ? Ti4 C10B 2.285(4) . ? Ti4 B6B 2.382(5) . ? Ti4 B7B 2.392(5) . ? Ti4 B3A 2.398(5) . ? Ti4 B6A 2.398(6) . ? Ti4 B7A 2.406(5) . ? Ti4 B3B 2.411(5) . ? Ti4 B2A 2.420(5) . ? Ti4 B2B 2.435(5) . ? C1A B3A 1.587(7) . ? C1A B2A 1.598(7) . ? C1A B5A 1.695(8) . ? C1A H1A 0.92(5) . ? B2A B6A 1.779(7) . ? B2A B9A 1.785(7) . ? B2A B5A 1.893(10) . ? B2A H2A 1.1200 . ? B3A B7A 1.786(7) . ? B3A B8A 1.791(7) . ? B3A H3A 1.17(5) . ? B5A B11A 1.753(13) . ? B5A B9A 1.815(9) . ? B5A H5A 1.1200 . ? B6A C10A 1.637(8) . ? B6A B12A 1.747(9) . ? B6A B9A 1.777(7) . ? B6A H6A 1.07(6) . ? B7A C10A 1.639(7) . ? B7A B8A 1.755(7) . ? B7A B13A 1.757(8) . ? B7A H7A 1.1200 . ? B8A B13A 1.735(8) . ? B8A B11A 1.738(9) . ? B8A H8A 1.11(5) . ? B9A B12A 1.674(10) . ? B9A B11A 1.715(8) . ? B9A H9A 1.08(5) . ? C10A B13A 1.712(9) . ? C10A B12A 1.881(9) . ? C10A H10A 1.1200 . ? B11A B13A 1.750(13) . ? B11A B12A 1.927(12) . ? B11A H11A 1.08(7) . ? B12A B13A 1.602(13) . ? B12A H12A 1.24(6) . ? B13A H13A 1.1200 . ? C1B B3B 1.558(7) . ? C1B B2B 1.575(6) . ? C1B B5B 1.755(6) . ? C1B H1B 0.97(5) . ? B2B B6B 1.768(7) . ? B2B B9B 1.802(7) . ? B2B B5B 1.985(7) . ? B2B K1 3.475(5) . ? B2B H2B 1.1200 . ? B3B B7B 1.778(9) . ? B3B B8B 1.790(8) . ? B3B B5B 2.008(7) . ? B3B K2 3.403(5) . ? B3B H3B 1.07(5) . ? B5B B11B 1.833(7) . ? B5B B9B 1.916(7) . ? B5B B8B 1.932(8) . ? B5B H5B 1.15(5) . ? B6B C10B 1.686(7) . ? B6B B9B 1.780(7) . ? B6B B12B 1.788(7) . ? B6B K1 3.384(5) . ? B6B H6B 1.09(5) . ? B7B C10B 1.670(8) . ? B7B B13B 1.761(8) . ? B7B B8B 1.771(7) . ? B7B K2 3.411(6) . ? B7B H7B 1.1200 . ? B8B B13B 1.748(8) . ? B8B B11B 1.759(8) . ? B8B K2 3.415(5) . ? B8B H8B 1.17(5) . ? B9B B12B 1.746(8) . ? B9B B11B 1.757(8) . ? B9B K1 3.366(5) . ? B9B H9B 1.1200 . ? C10B B12B 1.737(7) . ? C10B B13B 1.762(7) . ? C10B H10B 1.04(5) . ? B11B B12B 1.781(7) . ? B11B B13B 1.781(7) . ? B11B H11B 1.10(5) . ? B12B B13B 1.750(8) . ? B12B H12B 1.15(5) . ? B13B H13B 1.10(5) . ? K1 O6 2.822(3) . ? K1 O2 2.822(3) . ? K1 O4 2.829(4) . ? K1 O3 2.836(3) . ? K1 O1 2.854(4) . ? K1 O5 2.857(3) . ? K1 H6B 2.97(5) . ? O1 C22 1.414(6) . ? O1 C11 1.423(6) . ? C11 C12 1.498(7) . ? C11 H11C 0.9900 . ? C11 H11D 0.9900 . ? C12 O2 1.428(6) . ? C12 H12C 0.9900 . ? C12 H12D 0.9900 . ? O2 C13 1.423(6) . ? C13 C14 1.510(8) . ? C13 H13C 0.9900 . ? C13 H13D 0.9900 . ? C14 O3 1.426(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? O3 C15 1.439(6) . ? C15 C16 1.493(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O4 1.433(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O4 C17 1.402(7) . ? C17 C18 1.498(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O5 1.421(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O5 C19 1.413(6) . ? C19 C20 1.507(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O6 1.414(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? O6 C21 1.425(6) . ? C21 C22 1.492(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? K2 O9 2.814(4) . ? K2 O12 2.829(3) . ? K2 O11 2.831(4) . ? K2 O7 2.835(4) . ? K2 O10 2.844(4) . ? K2 O8 2.875(4) . ? K2 C33 3.532(5) . ? K2 H3B 2.83(5) . ? K2 H8B 2.79(5) . ? O7 C23 1.417(7) . ? O7 C34 1.430(6) . ? C23 C24 1.485(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O8 1.427(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O8 C25 1.423(7) . ? C25 C26 1.486(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O9 1.425(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O9 C27 1.431(7) . ? C27 C28 1.481(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O10 1.443(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O10 C29 1.424(7) . ? C29 C30 1.479(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O11 1.422(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O11 C31 1.436(6) . ? C31 C32 1.486(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O12 1.418(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? O12 C33 1.422(6) . ? C33 C34 1.481(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C1S Cl3 1.749(7) . ? C1S Cl2 1.757(6) . ? C1S Cl1 1.769(8) . ? C1S H1S 1.0000 . ? C2S Cl4 1.759(7) . ? C2S Cl6 1.760(7) . ? C2S Cl5 1.772(8) . ? C2S H2S 1.0000 . ? 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 C1B Ti4 C1A 118.19(17) . . ? C1B Ti4 C10A 113.84(17) . . ? C1A Ti4 C10A 92.47(16) . . ? C1B Ti4 C10B 92.61(15) . . ? C1A Ti4 C10B 117.96(18) . . ? C10A Ti4 C10B 124.06(18) . . ? C1B Ti4 B6B 77.42(16) . . ? C1A Ti4 B6B 90.82(17) . . ? C10A Ti4 B6B 164.67(17) . . ? C10B Ti4 B6B 42.30(17) . . ? C1B Ti4 B7B 77.54(18) . . ? C1A Ti4 B7B 157.7(2) . . ? C10A Ti4 B7B 95.07(18) . . ? C10B Ti4 B7B 41.76(19) . . ? B6B Ti4 B7B 76.73(16) . . ? C1B Ti4 B3A 157.84(18) . . ? C1A Ti4 B3A 40.05(19) . . ? C10A Ti4 B3A 77.18(17) . . ? C10B Ti4 B3A 96.54(18) . . ? B6B Ti4 B3A 96.02(17) . . ? B7B Ti4 B3A 122.0(2) . . ? C1B Ti4 B6A 87.77(17) . . ? C1A Ti4 B6A 77.18(17) . . ? C10A Ti4 B6A 41.12(19) . . ? C10B Ti4 B6A 162.00(19) . . ? B6B Ti4 B6A 153.82(19) . . ? B7B Ti4 B6A 121.3(2) . . ? B3A Ti4 B6A 89.63(18) . . ? C1B Ti4 B7A 153.86(18) . . ? C1A Ti4 B7A 77.06(18) . . ? C10A Ti4 B7A 41.09(17) . . ? C10B Ti4 B7A 98.40(18) . . ? B6B Ti4 B7A 125.80(18) . . ? B7B Ti4 B7A 95.12(19) . . ? B3A Ti4 B7A 43.63(16) . . ? B6A Ti4 B7A 74.55(19) . . ? C1B Ti4 B3B 39.32(18) . . ? C1A Ti4 B3B 156.61(18) . . ? C10A Ti4 B3B 93.70(17) . . ? C10B Ti4 B3B 76.35(18) . . ? B6B Ti4 B3B 89.15(17) . . ? B7B Ti4 B3B 43.5(2) . . ? B3A Ti4 B3B 162.83(19) . . ? B6A Ti4 B3B 92.93(18) . . ? B7A Ti4 B3B 121.13(18) . . ? C1B Ti4 B2A 91.16(17) . . ? C1A Ti4 B2A 40.07(17) . . ? C10A Ti4 B2A 76.67(18) . . ? C10B Ti4 B2A 154.52(19) . . ? B6B Ti4 B2A 114.68(17) . . ? B7B Ti4 B2A 162.10(19) . . ? B3A Ti4 B2A 72.16(19) . . ? B6A Ti4 B2A 43.34(17) . . ? B7A Ti4 B2A 88.98(18) . . ? B3B Ti4 B2A 120.34(19) . . ? C1B Ti4 B2B 39.46(16) . . ? C1A Ti4 B2B 94.46(17) . . ? C10A Ti4 B2B 151.20(17) . . ? C10B Ti4 B2B 76.32(16) . . ? B6B Ti4 B2B 43.05(16) . . ? B7B Ti4 B2B 88.98(17) . . ? B3A Ti4 B2B 124.08(16) . . ? B6A Ti4 B2B 113.95(18) . . ? B7A Ti4 B2B 166.68(16) . . ? B3B Ti4 B2B 69.99(15) . . ? B2A Ti4 B2B 90.98(17) . . ? B3A C1A B2A 126.0(4) . . ? B3A C1A B5A 86.2(5) . . ? B2A C1A B5A 70.1(4) . . ? B3A C1A Ti4 76.4(2) . . ? B2A C1A Ti4 77.1(3) . . ? B5A C1A Ti4 122.5(3) . . ? B3A C1A H1A 116(3) . . ? B2A C1A H1A 118(3) . . ? B5A C1A H1A 122(3) . . ? Ti4 C1A H1A 115(3) . . ? C1A B2A B6A 116.7(4) . . ? C1A B2A B9A 112.1(4) . . ? B6A B2A B9A 59.8(3) . . ? C1A B2A B5A 57.3(4) . . ? B6A B2A B5A 103.6(4) . . ? B9A B2A B5A 59.0(3) . . ? C1A B2A Ti4 62.8(2) . . ? B6A B2A Ti4 67.7(3) . . ? B9A B2A Ti4 115.9(3) . . ? B5A B2A Ti4 104.7(4) . . ? C1A B2A H2A 117.9 . . ? B6A B2A H2A 118.5 . . ? B9A B2A H2A 118.7 . . ? B5A B2A H2A 128.6 . . ? Ti4 B2A H2A 117.2 . . ? C1A B3A B7A 117.1(4) . . ? C1A B3A B8A 112.6(4) . . ? B7A B3A B8A 58.8(3) . . ? C1A B3A Ti4 63.5(2) . . ? B7A B3A Ti4 68.4(2) . . ? B8A B3A Ti4 116.7(3) . . ? C1A B3A H3A 117(2) . . ? B7A B3A H3A 121(3) . . ? B8A B3A H3A 117(3) . . ? Ti4 B3A H3A 119(3) . . ? C1A B5A B11A 129.3(6) . . ? C1A B5A B9A 106.2(4) . . ? B11A B5A B9A 57.4(4) . . ? C1A B5A B2A 52.5(3) . . ? B11A B5A B2A 108.0(5) . . ? B9A B5A B2A 57.5(3) . . ? C1A B5A H5A 108.3 . . ? B11A B5A H5A 105.6 . . ? B9A B5A H5A 144.1 . . ? B2A B5A H5A 145.9 . . ? C10A B6A B12A 67.5(4) . . ? C10A B6A B9A 107.5(4) . . ? B12A B6A B9A 56.7(3) . . ? C10A B6A B2A 115.9(4) . . ? B12A B6A B2A 113.2(4) . . ? B9A B6A B2A 60.3(3) . . ? C10A B6A Ti4 64.4(3) . . ? B12A B6A Ti4 125.4(4) . . ? B9A B6A Ti4 117.3(3) . . ? B2A B6A Ti4 69.0(3) . . ? C10A B6A H6A 117(3) . . ? B12A B6A H6A 105(3) . . ? B9A B6A H6A 120(3) . . ? B2A B6A H6A 123(3) . . ? Ti4 B6A H6A 118(3) . . ? C10A B7A B8A 109.7(4) . . ? C10A B7A B13A 60.4(4) . . ? B8A B7A B13A 59.2(3) . . ? C10A B7A B3A 115.5(4) . . ? B8A B7A B3A 60.8(3) . . ? B13A B7A B3A 110.7(5) . . ? C10A B7A Ti4 64.1(2) . . ? B8A B7A Ti4 117.8(3) . . ? B13A B7A Ti4 115.9(5) . . ? B3A B7A Ti4 67.9(2) . . ? C10A B7A H7A 119.5 . . ? B8A B7A H7A 120.5 . . ? B13A B7A H7A 121.0 . . ? B3A B7A H7A 117.2 . . ? Ti4 B7A H7A 112.7 . . ? B13A B8A B11A 60.5(5) . . ? B13A B8A B7A 60.5(3) . . ? B11A B8A B7A 109.5(4) . . ? B13A B8A B3A 111.5(4) . . ? B11A B8A B3A 113.8(4) . . ? B7A B8A B3A 60.5(3) . . ? B13A B8A H8A 121(3) . . ? B11A B8A H8A 119(3) . . ? B7A B8A H8A 123(3) . . ? B3A B8A H8A 118(3) . . ? B12A B9A B11A 69.3(5) . . ? B12A B9A B6A 60.7(4) . . ? B11A B9A B6A 111.1(4) . . ? B12A B9A B2A 116.7(4) . . ? B11A B9A B2A 114.9(4) . . ? B6A B9A B2A 59.9(3) . . ? B12A B9A B5A 117.6(6) . . ? B11A B9A B5A 59.5(5) . . ? B6A B9A B5A 107.0(4) . . ? B2A B9A B5A 63.5(3) . . ? B12A B9A H9A 109(3) . . ? B11A B9A H9A 121(3) . . ? B6A B9A H9A 118(3) . . ? B2A B9A H9A 117(3) . . ? B5A B9A H9A 127(3) . . ? B6A C10A B7A 125.3(4) . . ? B6A C10A B13A 104.0(5) . . ? B7A C10A B13A 63.2(4) . . ? B6A C10A B12A 59.1(3) . . ? B7A C10A B12A 111.3(4) . . ? B13A C10A B12A 52.7(4) . . ? B6A C10A Ti4 74.5(2) . . ? B7A C10A Ti4 74.8(2) . . ? B13A C10A Ti4 126.8(3) . . ? B12A C10A Ti4 127.0(3) . . ? B6A C10A H10A 117.1 . . ? B7A C10A H10A 111.5 . . ? B13A C10A H10A 125.3 . . ? B12A C10A H10A 123.3 . . ? Ti4 C10A H10A 99.0 . . ? B9A B11A B8A 121.7(4) . . ? B9A B11A B13A 97.9(6) . . ? B8A B11A B13A 59.7(4) . . ? B9A B11A B5A 63.1(5) . . ? B8A B11A B5A 78.5(6) . . ? B13A B11A B5A 114.9(5) . . ? B9A B11A B12A 54.4(4) . . ? B8A B11A B12A 106.4(5) . . ? B13A B11A B12A 51.4(5) . . ? B5A B11A B12A 108.3(4) . . ? B9A B11A H11A 124(4) . . ? B8A B11A H11A 113(4) . . ? B13A B11A H11A 121(4) . . ? B5A B11A H11A 120(4) . . ? B12A B11A H11A 122(4) . . ? B13A B12A B9A 105.8(5) . . ? B13A B12A B6A 104.0(5) . . ? B9A B12A B6A 62.6(3) . . ? B13A B12A C10A 58.2(4) . . ? B9A B12A C10A 101.5(4) . . ? B6A B12A C10A 53.5(3) . . ? B13A B12A B11A 58.6(4) . . ? B9A B12A B11A 56.3(4) . . ? B6A B12A B11A 103.1(5) . . ? C10A B12A B11A 98.7(4) . . ? B13A B12A H12A 122(3) . . ? B9A B12A H12A 125(3) . . ? B6A B12A H12A 123(3) . . ? C10A B12A H12A 126(3) . . ? B11A B12A H12A 129(3) . . ? B12A B13A C10A 69.1(5) . . ? B12A B13A B8A 123.3(7) . . ? C10A B13A B8A 107.2(4) . . ? B12A B13A B11A 70.0(6) . . ? C10A B13A B11A 113.1(7) . . ? B8A B13A B11A 59.8(4) . . ? B12A B13A B7A 120.0(7) . . ? C10A B13A B7A 56.4(3) . . ? B8A B13A B7A 60.3(3) . . ? B11A B13A B7A 108.9(5) . . ? B12A B13A H13A 106.3 . . ? C10A B13A H13A 121.8 . . ? B8A B13A H13A 119.8 . . ? B11A B13A H13A 119.1 . . ? B7A B13A H13A 121.9 . . ? B3B C1B B2B 125.0(4) . . ? B3B C1B B5B 74.4(3) . . ? B2B C1B B5B 73.0(3) . . ? B3B C1B Ti4 78.7(3) . . ? B2B C1B Ti4 79.4(2) . . ? B5B C1B Ti4 118.0(3) . . ? B3B C1B H1B 124(3) . . ? B2B C1B H1B 110(3) . . ? B5B C1B H1B 117(3) . . ? Ti4 C1B H1B 125(3) . . ? C1B B2B B6B 117.0(4) . . ? C1B B2B B9B 115.8(3) . . ? B6B B2B B9B 59.8(3) . . ? C1B B2B B5B 57.7(3) . . ? B6B B2B B5B 100.6(3) . . ? B9B B2B B5B 60.6(3) . . ? C1B B2B Ti4 61.2(2) . . ? B6B B2B Ti4 66.9(2) . . ? B9B B2B Ti4 115.4(3) . . ? B5B B2B Ti4 99.0(2) . . ? C1B B2B K1 170.0(3) . . ? B6B B2B K1 72.2(2) . . ? B9B B2B K1 71.4(2) . . ? B5B B2B K1 126.4(2) . . ? Ti4 B2B K1 123.22(17) . . ? C1B B2B H2B 116.2 . . ? B6B B2B H2B 119.6 . . ? B9B B2B H2B 116.3 . . ? B5B B2B H2B 131.5 . . ? Ti4 B2B H2B 120.4 . . ? K1 B2B H2B 53.9 . . ? C1B B3B B7B 118.0(4) . . ? C1B B3B B8B 116.1(4) . . ? B7B B3B B8B 59.5(3) . . ? C1B B3B B5B 57.3(3) . . ? B7B B3B B5B 100.1(3) . . ? B8B B3B B5B 60.8(3) . . ? C1B B3B Ti4 62.0(2) . . ? B7B B3B Ti4 67.7(2) . . ? B8B B3B Ti4 116.3(3) . . ? B5B B3B Ti4 99.1(2) . . ? C1B B3B K2 165.5(3) . . ? B7B B3B K2 75.1(2) . . ? B8B B3B K2 75.1(2) . . ? B5B B3B K2 129.6(3) . . ? Ti4 B3B K2 122.9(2) . . ? C1B B3B H3B 116(3) . . ? B7B B3B H3B 122(3) . . ? B8B B3B H3B 111(3) . . ? B5B B3B H3B 126(3) . . ? Ti4 B3B H3B 126(3) . . ? K2 B3B H3B 50(3) . . ? C1B B5B B11B 134.2(3) . . ? C1B B5B B9B 102.4(3) . . ? B11B B5B B9B 55.9(3) . . ? C1B B5B B8B 100.9(3) . . ? B11B B5B B8B 55.6(3) . . ? B9B B5B B8B 103.0(3) . . ? C1B B5B B2B 49.3(2) . . ? B11B B5B B2B 105.3(3) . . ? B9B B5B B2B 55.0(3) . . ? B8B B5B B2B 120.8(3) . . ? C1B B5B B3B 48.3(2) . . ? B11B B5B B3B 104.1(3) . . ? B9B B5B B3B 120.4(3) . . ? B8B B5B B3B 54.0(3) . . ? B2B B5B B3B 88.2(3) . . ? C1B B5B H5B 107(2) . . ? B11B B5B H5B 118(2) . . ? B9B B5B H5B 116(3) . . ? B8B B5B H5B 124(3) . . ? B2B B5B H5B 114(2) . . ? B3B B5B H5B 122(3) . . ? C10B B6B B2B 115.3(4) . . ? C10B B6B B9B 104.2(3) . . ? B2B B6B B9B 61.0(3) . . ? C10B B6B B12B 59.9(3) . . ? B2B B6B B12B 113.9(3) . . ? B9B B6B B12B 58.6(3) . . ? C10B B6B Ti4 65.8(2) . . ? B2B B6B Ti4 70.1(2) . . ? B9B B6B Ti4 118.8(3) . . ? B12B B6B Ti4 120.7(3) . . ? C10B B6B K1 164.4(3) . . ? B2B B6B K1 77.9(2) . . ? B9B B6B K1 74.1(2) . . ? B12B B6B K1 108.1(3) . . ? Ti4 B6B K1 129.00(19) . . ? C10B B6B H6B 114(3) . . ? B2B B6B H6B 124(3) . . ? B9B B6B H6B 127(3) . . ? B12B B6B H6B 112(3) . . ? Ti4 B6B H6B 110(3) . . ? K1 B6B H6B 59(2) . . ? C10B B7B B13B 61.7(3) . . ? C10B B7B B8B 105.6(4) . . ? B13B B7B B8B 59.3(3) . . ? C10B B7B B3B 114.7(4) . . ? B13B B7B B3B 114.4(4) . . ? B8B B7B B3B 60.6(3) . . ? C10B B7B Ti4 65.7(2) . . ? B13B B7B Ti4 122.4(3) . . ? B8B B7B Ti4 118.1(3) . . ? B3B B7B Ti4 68.8(2) . . ? C10B B7B K2 169.9(3) . . ? B13B B7B K2 111.6(3) . . ? B8B B7B K2 75.1(3) . . ? B3B B7B K2 74.6(2) . . ? Ti4 B7B K2 123.3(2) . . ? C10B B7B H7B 121.4 . . ? B13B B7B H7B 116.7 . . ? B8B B7B H7B 123.3 . . ? B3B B7B H7B 116.4 . . ? Ti4 B7B H7B 109.5 . . ? K2 B7B H7B 53.2 . . ? B13B B8B B11B 61.0(3) . . ? B13B B8B B7B 60.1(3) . . ? B11B B8B B7B 107.1(4) . . ? B13B B8B B3B 114.5(4) . . ? B11B B8B B3B 117.3(4) . . ? B7B B8B B3B 59.9(3) . . ? B13B B8B B5B 106.9(4) . . ? B11B B8B B5B 59.3(3) . . ? B7B B8B B5B 103.4(3) . . ? B3B B8B B5B 65.2(3) . . ? B13B B8B K2 111.9(3) . . ? B11B B8B K2 167.7(3) . . ? B7B B8B K2 74.9(2) . . ? B3B B8B K2 74.4(2) . . ? B5B B8B K2 132.6(3) . . ? B13B B8B H8B 122(3) . . ? B11B B8B H8B 125(3) . . ? B7B B8B H8B 121(3) . . ? B3B B8B H8B 110(3) . . ? B5B B8B H8B 125(3) . . ? K2 B8B H8B 49(3) . . ? B12B B9B B11B 61.1(3) . . ? B12B B9B B6B 60.9(3) . . ? B11B B9B B6B 108.0(4) . . ? B12B B9B B2B 114.3(4) . . ? B11B B9B B2B 117.1(4) . . ? B6B B9B B2B 59.2(3) . . ? B12B B9B B5B 106.9(4) . . ? B11B B9B B5B 59.7(3) . . ? B6B B9B B5B 102.8(3) . . ? B2B B9B B5B 64.4(3) . . ? B12B B9B K1 110.1(3) . . ? B11B B9B K1 164.3(3) . . ? B6B B9B K1 75.3(2) . . ? B2B B9B K1 78.1(2) . . ? B5B B9B K1 135.5(3) . . ? B12B B9B H9B 119.9 . . ? B11B B9B H9B 118.8 . . ? B6B B9B H9B 125.3 . . ? B2B B9B H9B 115.1 . . ? B5B B9B H9B 124.1 . . ? K1 B9B H9B 52.2 . . ? B7B C10B B6B 124.0(4) . . ? B7B C10B B12B 114.3(4) . . ? B6B C10B B12B 63.0(3) . . ? B7B C10B B13B 61.7(3) . . ? B6B C10B B13B 115.2(3) . . ? B12B C10B B13B 60.0(3) . . ? B7B C10B Ti4 72.5(3) . . ? B6B C10B Ti4 71.9(2) . . ? B12B C10B Ti4 128.9(3) . . ? B13B C10B Ti4 128.5(3) . . ? B7B C10B H10B 129(3) . . ? B6B C10B H10B 104(3) . . ? B12B C10B H10B 101(3) . . ? B13B C10B H10B 114(3) . . ? Ti4 C10B H10B 112(3) . . ? B9B B11B B8B 117.8(3) . . ? B9B B11B B12B 59.1(3) . . ? B8B B11B B12B 108.8(4) . . ? B9B B11B B13B 109.5(3) . . ? B8B B11B B13B 59.2(3) . . ? B12B B11B B13B 58.9(3) . . ? B9B B11B B5B 64.5(3) . . ? B8B B11B B5B 65.0(3) . . ? B12B B11B B5B 109.0(3) . . ? B13B B11B B5B 109.9(3) . . ? B9B B11B H11B 120(3) . . ? B8B B11B H11B 115(3) . . ? B12B B11B H11B 125(3) . . ? B13B B11B H11B 121(3) . . ? B5B B11B H11B 119(3) . . ? C10B B12B B9B 103.6(4) . . ? C10B B12B B13B 60.7(3) . . ? B9B B12B B13B 111.5(4) . . ? C10B B12B B11B 102.1(4) . . ? B9B B12B B11B 59.8(3) . . ? B13B B12B B11B 60.6(3) . . ? C10B B12B B6B 57.1(3) . . ? B9B B12B B6B 60.5(3) . . ? B13B B12B B6B 110.8(4) . . ? B11B B12B B6B 106.6(4) . . ? C10B B12B H12B 121(3) . . ? B9B B12B H12B 123(3) . . ? B13B B12B H12B 120(3) . . ? B11B B12B H12B 131(3) . . ? B6B B12B H12B 116(3) . . ? B8B B13B B12B 110.8(4) . . ? B8B B13B B7B 60.6(3) . . ? B12B B13B B7B 109.2(4) . . ? B8B B13B C10B 102.6(4) . . ? B12B B13B C10B 59.3(3) . . ? B7B B13B C10B 56.6(3) . . ? B8B B13B B11B 59.8(3) . . ? B12B B13B B11B 60.6(3) . . ? B7B B13B B11B 106.5(4) . . ? C10B B13B B11B 101.1(3) . . ? B8B B13B H13B 130(3) . . ? B12B B13B H13B 114(3) . . ? B7B B13B H13B 121(3) . . ? C10B B13B H13B 119(3) . . ? B11B B13B H13B 129(3) . . ? O6 K1 O2 116.78(10) . . ? O6 K1 O4 117.47(10) . . ? O2 K1 O4 116.77(10) . . ? O6 K1 O3 155.44(11) . . ? O2 K1 O3 58.67(10) . . ? O4 K1 O3 58.37(10) . . ? O6 K1 O1 58.17(9) . . ? O2 K1 O1 59.04(9) . . ? O4 K1 O1 156.75(11) . . ? O3 K1 O1 114.80(10) . . ? O6 K1 O5 58.36(9) . . ? O2 K1 O5 146.62(10) . . ? O4 K1 O5 59.25(10) . . ? O3 K1 O5 110.60(10) . . ? O1 K1 O5 110.25(10) . . ? O6 K1 B9B 98.47(12) . . ? O2 K1 B9B 110.90(11) . . ? O4 K1 B9B 90.64(13) . . ? O3 K1 B9B 105.61(11) . . ? O1 K1 B9B 112.41(12) . . ? O5 K1 B9B 102.40(12) . . ? O6 K1 B6B 123.57(11) . . ? O2 K1 B6B 82.89(10) . . ? O4 K1 B6B 92.70(12) . . ? O3 K1 B6B 80.82(11) . . ? O1 K1 B6B 108.61(11) . . ? O5 K1 B6B 128.81(11) . . ? B9B K1 B6B 30.57(12) . . ? O6 K1 B2B 95.77(11) . . ? O2 K1 B2B 85.65(10) . . ? O4 K1 B2B 118.03(12) . . ? O3 K1 B2B 107.40(11) . . ? O1 K1 B2B 85.09(10) . . ? O5 K1 B2B 126.67(11) . . ? B9B K1 B2B 30.48(12) . . ? B6B K1 B2B 29.84(12) . . ? O6 K1 H6B 141.3(10) . . ? O2 K1 H6B 71.4(10) . . ? O4 K1 H6B 85.5(10) . . ? O3 K1 H6B 62.8(10) . . ? O1 K1 H6B 111.9(10) . . ? O5 K1 H6B 135.4(10) . . ? B9B K1 H6B 47.6(9) . . ? B6B K1 H6B 18.3(9) . . ? B2B K1 H6B 45.7(9) . . ? C22 O1 C11 112.9(4) . . ? C22 O1 K1 107.7(3) . . ? C11 O1 K1 112.1(3) . . ? O1 C11 C12 108.1(4) . . ? O1 C11 H11C 110.1 . . ? C12 C11 H11C 110.1 . . ? O1 C11 H11D 110.1 . . ? C12 C11 H11D 110.1 . . ? H11C C11 H11D 108.4 . . ? O2 C12 C11 108.6(4) . . ? O2 C12 H12C 110.0 . . ? C11 C12 H12C 110.0 . . ? O2 C12 H12D 110.0 . . ? C11 C12 H12D 110.0 . . ? H12C C12 H12D 108.3 . . ? C13 O2 C12 112.3(4) . . ? C13 O2 K1 119.2(3) . . ? C12 O2 K1 118.3(3) . . ? O2 C13 C14 108.6(4) . . ? O2 C13 H13C 110.0 . . ? C14 C13 H13C 110.0 . . ? O2 C13 H13D 110.0 . . ? C14 C13 H13D 110.0 . . ? H13C C13 H13D 108.4 . . ? O3 C14 C13 107.9(4) . . ? O3 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? O3 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? C14 O3 C15 112.3(4) . . ? C14 O3 K1 114.7(3) . . ? C15 O3 K1 109.4(3) . . ? O3 C15 C16 106.9(4) . . ? O3 C15 H15A 110.3 . . ? C16 C15 H15A 110.3 . . ? O3 C15 H15B 110.3 . . ? C16 C15 H15B 110.3 . . ? H15A C15 H15B 108.6 . . ? O4 C16 C15 107.6(4) . . ? O4 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? O4 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? C17 O4 C16 112.0(4) . . ? C17 O4 K1 118.3(3) . . ? C16 O4 K1 119.5(3) . . ? O4 C17 C18 109.1(5) . . ? O4 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? O4 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? O5 C18 C17 109.0(5) . . ? O5 C18 H18A 109.9 . . ? C17 C18 H18A 109.9 . . ? O5 C18 H18B 109.9 . . ? C17 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? C19 O5 C18 109.1(4) . . ? C19 O5 K1 113.7(3) . . ? C18 O5 K1 110.7(3) . . ? O5 C19 C20 108.5(4) . . ? O5 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? O5 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? O6 C20 C19 108.1(4) . . ? O6 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? O6 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? C20 O6 C21 111.7(4) . . ? C20 O6 K1 119.7(3) . . ? C21 O6 K1 120.0(3) . . ? O6 C21 C22 108.1(4) . . ? O6 C21 H21A 110.1 . . ? C22 C21 H21A 110.1 . . ? O6 C21 H21B 110.1 . . ? C22 C21 H21B 110.1 . . ? H21A C21 H21B 108.4 . . ? O1 C22 C21 108.4(4) . . ? O1 C22 H22A 110.0 . . ? C21 C22 H22A 110.0 . . ? O1 C22 H22B 110.0 . . ? C21 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? O9 K2 O12 156.12(10) . . ? O9 K2 O11 116.50(12) . . ? O12 K2 O11 58.79(11) . . ? O9 K2 O7 117.58(12) . . ? O12 K2 O7 58.70(10) . . ? O11 K2 O7 117.18(11) . . ? O9 K2 O10 58.54(12) . . ? O12 K2 O10 114.39(11) . . ? O11 K2 O10 58.35(12) . . ? O7 K2 O10 156.87(11) . . ? O9 K2 O8 59.21(11) . . ? O12 K2 O8 110.49(11) . . ? O11 K2 O8 146.93(11) . . ? O7 K2 O8 58.52(11) . . ? O10 K2 O8 111.33(11) . . ? O9 K2 B3B 93.07(12) . . ? O12 K2 B3B 109.57(12) . . ? O11 K2 B3B 88.13(11) . . ? O7 K2 B3B 117.87(13) . . ? O10 K2 B3B 85.21(12) . . ? O8 K2 B3B 123.83(12) . . ? O9 K2 B7B 120.75(12) . . ? O12 K2 B7B 83.04(12) . . ? O11 K2 B7B 86.36(11) . . ? O7 K2 B7B 91.98(13) . . ? O10 K2 B7B 109.63(12) . . ? O8 K2 B7B 125.15(13) . . ? B3B K2 B7B 30.26(14) . . ? O9 K2 B8B 95.57(13) . . ? O12 K2 B8B 107.76(12) . . ? O11 K2 B8B 113.59(11) . . ? O7 K2 B8B 90.39(13) . . ? O10 K2 B8B 112.40(13) . . ? O8 K2 B8B 99.43(12) . . ? B3B K2 B8B 30.44(13) . . ? B7B K2 B8B 30.07(12) . . ? O9 K2 C33 158.36(13) . . ? O12 K2 C33 22.55(11) . . ? O11 K2 C33 79.01(12) . . ? O7 K2 C33 41.62(11) . . ? O10 K2 C33 136.48(13) . . ? O8 K2 C33 99.41(12) . . ? B3B K2 C33 102.88(13) . . ? B7B K2 C33 72.89(13) . . ? B8B K2 C33 91.10(13) . . ? O9 K2 H3B 80.3(11) . . ? O12 K2 H3B 120.2(11) . . ? O11 K2 H3B 84.3(11) . . ? O7 K2 H3B 133.8(11) . . ? O10 K2 H3B 69.3(11) . . ? O8 K2 H3B 123.5(11) . . ? B3B K2 H3B 16.8(11) . . ? B7B K2 H3B 46.5(11) . . ? B8B K2 H3B 43.9(11) . . ? C33 K2 H3B 117.8(11) . . ? O9 K2 H8B 83.3(11) . . ? O12 K2 H8B 117.9(11) . . ? O11 K2 H8B 131.7(11) . . ? O7 K2 H8B 84.0(11) . . ? O10 K2 H8B 116.5(11) . . ? O8 K2 H8B 81.4(11) . . ? B3B K2 H8B 45.2(11) . . ? B7B K2 H8B 47.9(11) . . ? B8B K2 H8B 18.4(11) . . ? C33 K2 H8B 97.5(11) . . ? H3B K2 H8B 54.6(15) . . ? C23 O7 C34 112.4(4) . . ? C23 O7 K2 119.1(3) . . ? C34 O7 K2 118.4(3) . . ? O7 C23 C24 108.9(5) . . ? O7 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? O7 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? O8 C24 C23 109.1(5) . . ? O8 C24 H24A 109.9 . . ? C23 C24 H24A 109.9 . . ? O8 C24 H24B 109.9 . . ? C23 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C25 O8 C24 111.2(4) . . ? C25 O8 K2 111.7(4) . . ? C24 O8 K2 112.6(4) . . ? O8 C25 C26 109.8(5) . . ? O8 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? O8 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? O9 C26 C25 109.1(5) . . ? O9 C26 H26A 109.9 . . ? C25 C26 H26A 109.9 . . ? O9 C26 H26B 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? C26 O9 C27 111.6(4) . . ? C26 O9 K2 118.8(3) . . ? C27 O9 K2 120.1(3) . . ? O9 C27 C28 108.3(4) . . ? O9 C27 H27A 110.0 . . ? C28 C27 H27A 110.0 . . ? O9 C27 H27B 110.0 . . ? C28 C27 H27B 110.0 . . ? H27A C27 H27B 108.4 . . ? O10 C28 C27 108.2(4) . . ? O10 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? O10 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? C29 O10 C28 113.7(5) . . ? C29 O10 K2 113.3(3) . . ? C28 O10 K2 108.8(3) . . ? O10 C29 C30 108.6(4) . . ? O10 C29 H29A 110.0 . . ? C30 C29 H29A 110.0 . . ? O10 C29 H29B 110.0 . . ? C30 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? O11 C30 C29 108.4(5) . . ? O11 C30 H30A 110.0 . . ? C29 C30 H30A 110.0 . . ? O11 C30 H30B 110.0 . . ? C29 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? C30 O11 C31 113.4(4) . . ? C30 O11 K2 119.0(3) . . ? C31 O11 K2 117.7(3) . . ? O11 C31 C32 109.0(4) . . ? O11 C31 H31A 109.9 . . ? C32 C31 H31A 109.9 . . ? O11 C31 H31B 109.9 . . ? C32 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? O12 C32 C31 108.0(4) . . ? O12 C32 H32A 110.1 . . ? C31 C32 H32A 110.1 . . ? O12 C32 H32B 110.1 . . ? C31 C32 H32B 110.1 . . ? H32A C32 H32B 108.4 . . ? C32 O12 C33 112.7(4) . . ? C32 O12 K2 114.2(3) . . ? C33 O12 K2 107.7(3) . . ? O12 C33 C34 108.2(4) . . ? O12 C33 K2 49.7(2) . . ? C34 C33 K2 86.0(3) . . ? O12 C33 H33A 110.1 . . ? C34 C33 H33A 110.1 . . ? K2 C33 H33A 77.5 . . ? O12 C33 H33B 110.1 . . ? C34 C33 H33B 110.1 . . ? K2 C33 H33B 158.6 . . ? H33A C33 H33B 108.4 . . ? O7 C34 C33 107.9(4) . . ? O7 C34 H34A 110.1 . . ? C33 C34 H34A 110.1 . . ? O7 C34 H34B 110.1 . . ? C33 C34 H34B 110.1 . . ? H34A C34 H34B 108.4 . . ? Cl3 C1S Cl2 111.3(4) . . ? Cl3 C1S Cl1 110.8(3) . . ? Cl2 C1S Cl1 109.6(4) . . ? Cl3 C1S H1S 108.3 . . ? Cl2 C1S H1S 108.3 . . ? Cl1 C1S H1S 108.3 . . ? Cl4 C2S Cl6 110.1(4) . . ? Cl4 C2S Cl5 111.6(4) . . ? Cl6 C2S Cl5 109.6(4) . . ? Cl4 C2S H2S 108.5 . . ? Cl6 C2S H2S 108.5 . . ? Cl5 C2S H2S 108.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.606 _refine_diff_density_min -1.217 _refine_diff_density_rms 0.091 #===end data_7 _database_code_depnum_ccdc_archive 'CCDC 663041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H49 B20 Fe K O6.50' _chemical_formula_weight 656.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' B B 0.0013 0.0007 '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 11.1550(18) _cell_length_b 11.4338(19) _cell_length_c 13.759(2) _cell_angle_alpha 98.939(9) _cell_angle_beta 105.521(9) _cell_angle_gamma 94.770(9) _cell_volume 1656.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3773 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description NEEDLE _exptl_crystal_colour pale _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 0.616 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25741 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 24.80 _reflns_number_total 5532 _reflns_number_gt 3638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0942P)^2^+5.9631P] 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 5532 _refine_ls_number_parameters 475 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.1288 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2178 _refine_ls_wR_factor_gt 0.1837 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe4 Fe 0.30087(7) 0.13621(7) 0.64150(6) 0.0165(3) Uani 1 1 d . . . C1A C 0.1599(6) 0.0086(6) 0.6436(4) 0.0258(14) Uani 1 1 d D . . H1C H 0.065(3) -0.017(5) 0.585(4) 0.031 Uiso 1 1 d D . . B2A B 0.1662(6) 0.1054(7) 0.7364(5) 0.0231(16) Uani 1 1 d D . . H2C H 0.090(4) 0.160(4) 0.741(4) 0.028 Uiso 1 1 d D . . B3A B 0.2652(7) -0.0662(6) 0.6301(5) 0.0252(16) Uani 1 1 d D . . H3C H 0.256(6) -0.143(4) 0.566(3) 0.030 Uiso 1 1 d D . . B5A B 0.1958(7) -0.0615(7) 0.7504(6) 0.0279(17) Uani 1 1 d D . . H5C H 0.119(4) -0.125(4) 0.753(5) 0.033 Uiso 1 1 d D . . B6A B 0.3185(7) 0.1848(7) 0.8095(5) 0.0261(16) Uani 1 1 d D . . H6C H 0.322(6) 0.282(2) 0.837(4) 0.031 Uiso 1 1 d D . . B7A B 0.4249(7) 0.0012(7) 0.6960(6) 0.0287(17) Uani 1 1 d D . . H7C H 0.493(5) -0.020(5) 0.653(4) 0.034 Uiso 1 1 d D . . B8A B 0.3537(7) -0.1113(7) 0.7435(6) 0.0287(17) Uani 1 1 d D . . H8C H 0.377(6) -0.202(3) 0.728(5) 0.034 Uiso 1 1 d D . . B9A B 0.2450(7) 0.0753(7) 0.8587(5) 0.0265(16) Uani 1 1 d D . . H9C H 0.199(5) 0.105(5) 0.919(3) 0.032 Uiso 1 1 d D . . C10A C 0.4411(5) 0.1255(6) 0.7828(5) 0.0248(14) Uani 1 1 d D . . H10C H 0.524(4) 0.193(4) 0.790(5) 0.030 Uiso 1 1 d D . . B11A B 0.3313(7) -0.0469(7) 0.8608(5) 0.0266(17) Uani 1 1 d D . . H11C H 0.329(6) -0.104(4) 0.918(4) 0.032 Uiso 1 1 d D . . B12A B 0.4073(7) 0.1025(7) 0.8951(5) 0.0259(16) Uani 1 1 d D . . H12C H 0.464(5) 0.153(5) 0.971(3) 0.031 Uiso 1 1 d D . . B13A B 0.4697(7) -0.0059(7) 0.8274(6) 0.0294(17) Uani 1 1 d D . . H13C H 0.563(3) -0.030(5) 0.863(4) 0.035 Uiso 1 1 d D . . C1B C 0.3584(8) 0.1027(9) 0.5085(5) 0.056(3) Uani 1 1 d DU . . H1D H 0.396(7) 0.013(4) 0.493(6) 0.067 Uiso 1 1 d D . . B2B B 0.4541(10) 0.2009(13) 0.5745(10) 0.080(4) Uani 1 1 d DU . . H2D H 0.545(5) 0.166(8) 0.585(7) 0.096 Uiso 1 1 d D . . B3B B 0.2116(7) 0.1018(7) 0.4689(5) 0.0243(16) Uani 1 1 d DU . . H3D H 0.146(4) 0.020(3) 0.426(4) 0.029 Uiso 1 1 d D . . B5B B 0.3255(8) 0.1906(8) 0.4178(7) 0.041(2) Uani 1 1 d D . . H5D H 0.351(6) 0.160(6) 0.347(3) 0.049 Uiso 1 1 d D . . B6B B 0.4020(11) 0.3130(10) 0.6477(8) 0.070(3) Uani 1 1 d DU . . H6D H 0.4602 0.3524 0.7278 0.084 Uiso 1 1 calc RD . . B7B B 0.1452(6) 0.2132(6) 0.5400(5) 0.0214(15) Uani 1 1 d DU . . H7D H 0.047(3) 0.195(5) 0.542(4) 0.026 Uiso 1 1 d D . . B8B B 0.1733(7) 0.2353(7) 0.4232(5) 0.0244(16) Uani 1 1 d D . . H8D H 0.092(4) 0.225(5) 0.355(3) 0.029 Uiso 1 1 d D . . B9B B 0.4383(11) 0.3279(11) 0.5277(9) 0.071(3) Uani 1 1 d DU . . H9D H 0.526(5) 0.377(7) 0.525(7) 0.085 Uiso 1 1 d D . . C10B C 0.2450(8) 0.3071(6) 0.6325(5) 0.049(2) Uani 1 1 d DU . . H10D H 0.208(7) 0.341(6) 0.700(4) 0.059 Uiso 1 1 d D . . B11B B 0.3025(8) 0.3415(8) 0.4434(6) 0.039(2) Uani 1 1 d D . . H11D H 0.295(6) 0.392(5) 0.380(4) 0.046 Uiso 1 1 d D . . B12B B 0.3527(15) 0.4088(12) 0.5759(10) 0.097(4) Uani 1 1 d DU . . H12D H 0.3906 0.5057 0.6028 0.117 Uiso 1 1 calc RD . . B13B B 0.2056(13) 0.3625(8) 0.5253(7) 0.063(3) Uani 1 1 d DU . . H13D H 0.140(6) 0.429(6) 0.519(6) 0.075 Uiso 1 1 d D . . K1 K 0.0852(2) 0.3423(2) 0.90239(17) 0.0738(7) Uani 1 1 d . . . O1 O 0.0050(5) 0.4304(4) 0.7253(3) 0.0383(12) Uani 1 1 d . . . O2 O 0.2017(5) 0.5659(4) 0.8856(4) 0.0414(12) Uani 1 1 d . . . O3 O 0.3191(5) 0.4461(4) 1.0429(4) 0.0438(13) Uani 1 1 d . . . O4 O 0.1592(4) 0.2876(5) 1.1025(4) 0.0439(13) Uani 1 1 d . . . O5 O -0.0502(4) 0.1609(4) 0.9497(3) 0.0363(11) Uani 1 1 d . . . O6 O -0.1472(4) 0.2578(4) 0.7750(3) 0.0345(11) Uani 1 1 d . . . C1 C 0.0377(9) 0.5553(6) 0.7296(6) 0.056(2) Uani 1 1 d . . . H1A H -0.0121 0.6023 0.7672 0.067 Uiso 1 1 calc R . . H1B H 0.0191 0.5730 0.6593 0.067 Uiso 1 1 calc R . . C2 C 0.1742(9) 0.5884(6) 0.7833(6) 0.053(2) Uani 1 1 d . . . H2A H 0.2233 0.5413 0.7452 0.064 Uiso 1 1 calc R . . H2B H 0.1987 0.6740 0.7850 0.064 Uiso 1 1 calc R . . C3 C 0.3316(7) 0.5905(7) 0.9377(7) 0.053(2) Uani 1 1 d . . . H3A H 0.3624 0.6746 0.9386 0.064 Uiso 1 1 calc R . . H3B H 0.3786 0.5382 0.9014 0.064 Uiso 1 1 calc R . . C4 C 0.3532(7) 0.5692(6) 1.0453(6) 0.049(2) Uani 1 1 d . . . H4A H 0.4427 0.5932 1.0839 0.059 Uiso 1 1 calc R . . H4B H 0.3021 0.6177 1.0802 0.059 Uiso 1 1 calc R . . C5 C 0.3429(8) 0.4220(7) 1.1474(6) 0.051(2) Uani 1 1 d . . . H5A H 0.3016 0.4764 1.1875 0.061 Uiso 1 1 calc R . . H5B H 0.4342 0.4351 1.1822 0.061 Uiso 1 1 calc R . . C6 C 0.2922(7) 0.2972(7) 1.1409(6) 0.047(2) Uani 1 1 d . . . H6A H 0.3259 0.2432 1.0942 0.057 Uiso 1 1 calc R . . H6B H 0.3161 0.2748 1.2095 0.057 Uiso 1 1 calc R . . C7 C 0.1024(9) 0.1751(7) 1.1081(6) 0.051(2) Uani 1 1 d . . . H7A H 0.1152 0.1681 1.1809 0.061 Uiso 1 1 calc R . . H7B H 0.1419 0.1114 1.0758 0.061 Uiso 1 1 calc R . . C8 C -0.0319(8) 0.1603(7) 1.0555(6) 0.046(2) Uani 1 1 d . . . H8A H -0.0725 0.0840 1.0644 0.055 Uiso 1 1 calc R . . H8B H -0.0709 0.2261 1.0856 0.055 Uiso 1 1 calc R . . C9 C -0.1788(7) 0.1394(6) 0.8937(6) 0.0420(19) Uani 1 1 d . . . H9A H -0.2241 0.2022 0.9200 0.050 Uiso 1 1 calc R . . H9B H -0.2166 0.0612 0.9014 0.050 Uiso 1 1 calc R . . C10 C -0.1891(7) 0.1400(6) 0.7837(6) 0.0418(18) Uani 1 1 d . . . H10A H -0.1367 0.0830 0.7592 0.050 Uiso 1 1 calc R . . H10B H -0.2773 0.1158 0.7416 0.050 Uiso 1 1 calc R . . C11 C -0.1567(6) 0.2667(7) 0.6707(5) 0.0413(19) Uani 1 1 d . . . H11A H -0.2435 0.2379 0.6271 0.050 Uiso 1 1 calc R . . H11B H -0.0993 0.2167 0.6451 0.050 Uiso 1 1 calc R . . C12 C -0.1233(7) 0.3915(7) 0.6657(5) 0.046(2) Uani 1 1 d . . . H12A H -0.1337 0.3998 0.5934 0.055 Uiso 1 1 calc R . . H12B H -0.1794 0.4417 0.6929 0.055 Uiso 1 1 calc R . . O1W O -0.0014(16) 0.4633(13) 1.0322(10) 0.072(4) Uani 0.50 1 d PD . . H1W H -0.061(9) 0.470(12) 0.974(6) 0.108 Uiso 1 1 d 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 Fe4 0.0135(4) 0.0212(5) 0.0162(4) 0.0083(3) 0.0041(3) 0.0024(3) C1A 0.024(3) 0.033(4) 0.020(3) 0.012(3) 0.003(3) -0.004(3) B2A 0.019(4) 0.035(4) 0.021(4) 0.015(3) 0.010(3) 0.006(3) B3A 0.037(4) 0.017(4) 0.025(4) 0.005(3) 0.013(3) 0.005(3) B5A 0.025(4) 0.032(4) 0.026(4) 0.015(3) 0.005(3) -0.007(3) B6A 0.036(4) 0.025(4) 0.017(3) 0.005(3) 0.004(3) 0.005(3) B7A 0.020(4) 0.040(5) 0.035(4) 0.021(4) 0.012(3) 0.016(3) B8A 0.036(4) 0.022(4) 0.033(4) 0.013(3) 0.011(3) 0.014(3) B9A 0.023(4) 0.038(4) 0.024(4) 0.011(3) 0.012(3) 0.009(3) C10A 0.019(3) 0.030(4) 0.025(3) 0.014(3) 0.001(3) -0.003(3) B11A 0.026(4) 0.038(4) 0.021(4) 0.019(3) 0.007(3) 0.005(3) B12A 0.027(4) 0.029(4) 0.019(4) 0.010(3) 0.001(3) -0.001(3) B13A 0.026(4) 0.038(5) 0.033(4) 0.024(4) 0.011(3) 0.009(3) C1B 0.059(5) 0.106(7) 0.027(4) 0.036(4) 0.025(4) 0.062(5) B2B 0.043(5) 0.121(8) 0.098(7) 0.088(7) 0.020(5) 0.009(5) B3B 0.028(4) 0.034(4) 0.016(3) 0.011(3) 0.010(3) 0.012(3) B5B 0.050(5) 0.051(5) 0.046(5) 0.039(4) 0.031(4) 0.033(4) B6B 0.080(5) 0.064(5) 0.052(4) 0.038(4) -0.008(4) -0.024(4) B7B 0.022(3) 0.025(4) 0.021(3) 0.008(3) 0.008(3) 0.009(3) B8B 0.024(4) 0.033(4) 0.021(4) 0.009(3) 0.009(3) 0.013(3) B9B 0.059(5) 0.084(5) 0.074(5) 0.056(4) 0.008(4) -0.014(4) C10B 0.089(6) 0.029(4) 0.029(4) 0.010(3) 0.005(4) 0.036(4) B11B 0.046(5) 0.044(5) 0.027(4) 0.027(4) 0.004(4) 0.000(4) B12B 0.141(9) 0.071(7) 0.068(7) 0.038(6) 0.007(6) -0.026(6) B13B 0.135(10) 0.035(5) 0.043(5) 0.024(4) 0.052(6) 0.034(6) K1 0.0911(16) 0.0689(15) 0.0637(13) 0.0057(11) 0.0330(12) -0.0005(12) O1 0.063(3) 0.025(3) 0.030(3) 0.009(2) 0.014(2) 0.016(2) O2 0.062(4) 0.030(3) 0.044(3) 0.014(2) 0.031(3) 0.009(2) O3 0.046(3) 0.032(3) 0.057(3) 0.006(2) 0.022(3) 0.005(2) O4 0.037(3) 0.052(3) 0.051(3) 0.024(3) 0.018(2) 0.011(2) O5 0.042(3) 0.039(3) 0.039(3) 0.011(2) 0.029(2) 0.007(2) O6 0.033(3) 0.040(3) 0.030(3) 0.003(2) 0.009(2) 0.005(2) C1 0.113(8) 0.027(4) 0.037(4) 0.016(3) 0.026(5) 0.029(5) C2 0.103(7) 0.023(4) 0.046(5) 0.010(3) 0.044(5) 0.003(4) C3 0.046(5) 0.030(4) 0.091(7) 0.014(4) 0.032(5) -0.003(4) C4 0.045(5) 0.029(4) 0.068(6) 0.001(4) 0.014(4) 0.005(3) C5 0.051(5) 0.058(6) 0.031(4) -0.004(4) -0.006(4) 0.014(4) C6 0.051(5) 0.065(6) 0.030(4) 0.015(4) 0.012(4) 0.017(4) C7 0.093(7) 0.043(5) 0.034(4) 0.020(4) 0.037(4) 0.019(4) C8 0.076(6) 0.035(4) 0.044(4) 0.007(3) 0.046(4) 0.001(4) C9 0.036(4) 0.027(4) 0.074(6) 0.013(4) 0.032(4) 0.007(3) C10 0.028(4) 0.038(4) 0.058(5) -0.002(4) 0.017(3) -0.003(3) C11 0.027(4) 0.066(5) 0.029(4) 0.004(4) 0.005(3) 0.017(4) C12 0.055(5) 0.062(5) 0.026(4) 0.016(4) 0.011(4) 0.030(4) O1W 0.078(10) 0.063(9) 0.073(10) 0.008(7) 0.022(8) 0.012(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe4 C1A 2.063(6) . ? Fe4 C1B 2.088(7) . ? Fe4 C10B 2.111(6) . ? Fe4 C10A 2.173(6) . ? Fe4 B6B 2.209(10) . ? Fe4 B7A 2.240(7) . ? Fe4 B6A 2.242(7) . ? Fe4 B7B 2.254(7) . ? Fe4 B2B 2.272(10) . ? Fe4 B3B 2.273(7) . ? Fe4 B2A 2.279(6) . ? Fe4 B3A 2.290(7) . ? C1A B2A 1.536(9) . ? C1A B3A 1.543(10) . ? C1A B5A 1.751(9) . ? C1A H1C 1.13(2) . ? B2A B9A 1.777(10) . ? B2A B6A 1.807(10) . ? B2A B5A 1.992(10) . ? B2A H2C 1.11(2) . ? B3A B8A 1.784(10) . ? B3A B7A 1.811(11) . ? B3A B5A 2.002(10) . ? B3A H3C 1.12(2) . ? B5A B11A 1.808(10) . ? B5A B9A 1.914(11) . ? B5A B8A 1.917(11) . ? B5A H5C 1.09(2) . ? B6A C10A 1.677(10) . ? B6A B9A 1.757(10) . ? B6A B12A 1.770(10) . ? B6A H6C 1.11(2) . ? B7A C10A 1.671(10) . ? B7A B8A 1.755(10) . ? B7A B13A 1.758(10) . ? B7A H7C 1.10(2) . ? B8A B13A 1.722(11) . ? B8A B11A 1.756(10) . ? B8A H8C 1.10(2) . ? B9A B12A 1.732(10) . ? B9A B11A 1.762(10) . ? B9A H9C 1.11(2) . ? C10A B13A 1.730(9) . ? C10A B12A 1.738(9) . ? C10A H10C 1.13(2) . ? B11A B13A 1.772(10) . ? B11A B12A 1.776(10) . ? B11A H11C 1.10(2) . ? B12A B13A 1.738(11) . ? B12A H12C 1.10(2) . ? B13A H13C 1.10(2) . ? C1B B2B 1.480(16) . ? C1B B3B 1.580(11) . ? C1B B5B 1.705(10) . ? C1B H1D 1.14(2) . ? B2B B9B 1.681(15) . ? B2B B6B 1.74(2) . ? B2B H2D 1.10(2) . ? B3B B8B 1.780(10) . ? B3B B7B 1.813(9) . ? B3B B5B 1.903(11) . ? B3B H3D 1.11(2) . ? B5B B11B 1.761(12) . ? B5B B8B 1.830(10) . ? B5B B9B 2.062(16) . ? B5B H5D 1.10(2) . ? B6B B12B 1.620(16) . ? B6B C10B 1.701(15) . ? B6B B9B 1.831(16) . ? B6B H6D 1.1200 . ? B7B C10B 1.622(10) . ? B7B B8B 1.767(9) . ? B7B B13B 1.843(12) . ? B7B H7D 1.10(2) . ? B8B B11B 1.738(11) . ? B8B B13B 1.796(12) . ? B8B H8D 1.10(2) . ? B9B B12B 1.58(2) . ? B9B B11B 1.679(14) . ? B9B H9D 1.10(2) . ? C10B B13B 1.661(11) . ? C10B B12B 1.988(16) . ? C10B H10D 1.14(2) . ? B11B B13B 1.764(13) . ? B11B B12B 1.782(16) . ? B11B H11D 1.10(2) . ? B12B B13B 1.608(19) . ? B12B H12D 1.1200 . ? B13B H13D 1.10(2) . ? K1 O1W 2.532(13) . ? K1 O1W 2.608(13) 2_567 ? K1 O6 2.712(5) . ? K1 O5 2.726(5) . ? K1 O1 2.739(5) . ? K1 O3 2.833(6) . ? K1 O4 2.839(5) . ? K1 O2 2.840(5) . ? K1 C11 3.513(7) . ? K1 C10 3.515(7) . ? K1 K1 4.970(4) 2_567 ? K1 H2C 2.81(5) . ? K1 H1W 2.56(12) . ? O1 C1 1.433(9) . ? O1 C12 1.439(9) . ? O2 C3 1.417(9) . ? O2 C2 1.427(9) . ? O3 C4 1.420(8) . ? O3 C5 1.465(9) . ? O4 C7 1.407(9) . ? O4 C6 1.424(9) . ? O5 C9 1.415(8) . ? O5 C8 1.415(8) . ? O6 C10 1.423(8) . ? O6 C11 1.431(8) . ? C1 C2 1.490(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.497(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.470(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.462(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.487(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.461(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O1W O1W 1.32(3) 2_567 ? O1W K1 2.608(13) 2_567 ? O1W H1W 0.91(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 C1A Fe4 C1B 112.7(3) . . ? C1A Fe4 C10B 114.1(3) . . ? C1B Fe4 C10B 100.2(3) . . ? C1A Fe4 C10A 100.3(2) . . ? C1B Fe4 C10A 115.3(3) . . ? C10B Fe4 C10A 114.9(3) . . ? C1A Fe4 B6B 159.9(4) . . ? C1B Fe4 B6B 79.5(4) . . ? C10B Fe4 B6B 46.3(4) . . ? C10A Fe4 B6B 87.6(3) . . ? C1A Fe4 B7A 83.2(3) . . ? C1B Fe4 B7A 85.3(3) . . ? C10B Fe4 B7A 157.3(3) . . ? C10A Fe4 B7A 44.4(3) . . ? B6B Fe4 B7A 114.5(4) . . ? C1A Fe4 B6A 83.3(3) . . ? C1B Fe4 B6A 158.1(3) . . ? C10B Fe4 B6A 85.5(3) . . ? C10A Fe4 B6A 44.6(3) . . ? B6B Fe4 B6A 89.8(4) . . ? B7A Fe4 B6A 81.9(3) . . ? C1A Fe4 B7B 84.9(2) . . ? C1B Fe4 B7B 83.2(3) . . ? C10B Fe4 B7B 43.5(3) . . ? C10A Fe4 B7B 156.1(2) . . ? B6B Fe4 B7B 80.8(3) . . ? B7A Fe4 B7B 158.7(3) . . ? B6A Fe4 B7B 114.1(3) . . ? C1A Fe4 B2B 151.1(5) . . ? C1B Fe4 B2B 39.4(5) . . ? C10B Fe4 B2B 84.6(4) . . ? C10A Fe4 B2B 90.4(3) . . ? B6B Fe4 B2B 45.7(5) . . ? B7A Fe4 B2B 86.0(4) . . ? B6A Fe4 B2B 121.6(4) . . ? B7B Fe4 B2B 96.2(3) . . ? C1A Fe4 B3B 85.5(3) . . ? C1B Fe4 B3B 42.2(3) . . ? C10B Fe4 B3B 83.1(3) . . ? C10A Fe4 B3B 155.7(2) . . ? B6B Fe4 B3B 94.9(3) . . ? B7A Fe4 B3B 114.1(3) . . ? B6A Fe4 B3B 159.2(3) . . ? B7B Fe4 B3B 47.2(2) . . ? B2B Fe4 B3B 74.6(4) . . ? C1A Fe4 B2A 41.1(3) . . ? C1B Fe4 B2A 152.8(3) . . ? C10B Fe4 B2A 89.1(3) . . ? C10A Fe4 B2A 82.7(2) . . ? B6B Fe4 B2A 123.5(4) . . ? B7A Fe4 B2A 96.0(3) . . ? B6A Fe4 B2A 47.1(3) . . ? B7B Fe4 B2A 86.4(2) . . ? B2B Fe4 B2A 167.7(4) . . ? B3B Fe4 B2A 115.2(3) . . ? C1A Fe4 B3A 41.1(3) . . ? C1B Fe4 B3A 87.7(3) . . ? C10B Fe4 B3A 154.1(3) . . ? C10A Fe4 B3A 82.8(2) . . ? B6B Fe4 B3A 159.0(4) . . ? B7A Fe4 B3A 47.1(3) . . ? B6A Fe4 B3A 96.4(3) . . ? B7B Fe4 B3A 114.5(3) . . ? B2B Fe4 B3A 115.4(4) . . ? B3B Fe4 B3A 86.5(3) . . ? B2A Fe4 B3A 73.9(3) . . ? B2A C1A B3A 126.2(5) . . ? B2A C1A B5A 74.3(4) . . ? B3A C1A B5A 74.5(4) . . ? B2A C1A Fe4 77.0(4) . . ? B3A C1A Fe4 77.3(4) . . ? B5A C1A Fe4 114.2(4) . . ? B2A C1A H1C 116(3) . . ? B3A C1A H1C 117(3) . . ? B5A C1A H1C 120(3) . . ? Fe4 C1A H1C 126(3) . . ? C1A B2A B9A 116.0(5) . . ? C1A B2A B6A 117.8(5) . . ? B9A B2A B6A 58.7(4) . . ? C1A B2A B5A 57.8(4) . . ? B9A B2A B5A 60.7(4) . . ? B6A B2A B5A 100.2(4) . . ? C1A B2A Fe4 61.9(3) . . ? B9A B2A Fe4 111.9(4) . . ? B6A B2A Fe4 65.4(3) . . ? B5A B2A Fe4 97.1(3) . . ? C1A B2A H2C 124(3) . . ? B9A B2A H2C 111(3) . . ? B6A B2A H2C 112(3) . . ? B5A B2A H2C 135(3) . . ? Fe4 B2A H2C 124(3) . . ? C1A B3A B8A 115.4(5) . . ? C1A B3A B7A 116.8(5) . . ? B8A B3A B7A 58.4(4) . . ? C1A B3A B5A 57.5(4) . . ? B8A B3A B5A 60.5(4) . . ? B7A B3A B5A 99.6(5) . . ? C1A B3A Fe4 61.6(3) . . ? B8A B3A Fe4 111.3(4) . . ? B7A B3A Fe4 65.0(3) . . ? B5A B3A Fe4 96.5(4) . . ? C1A B3A H3C 126(3) . . ? B8A B3A H3C 106(3) . . ? B7A B3A H3C 114(3) . . ? B5A B3A H3C 129(3) . . ? Fe4 B3A H3C 132(3) . . ? C1A B5A B11A 133.8(5) . . ? C1A B5A B9A 100.2(5) . . ? B11A B5A B9A 56.4(4) . . ? C1A B5A B8A 100.2(5) . . ? B11A B5A B8A 56.2(4) . . ? B9A B5A B8A 102.6(5) . . ? C1A B5A B2A 47.9(3) . . ? B11A B5A B2A 105.2(5) . . ? B9A B5A B2A 54.1(4) . . ? B8A B5A B2A 119.0(4) . . ? C1A B5A B3A 48.0(3) . . ? B11A B5A B3A 105.2(5) . . ? B9A B5A B3A 119.3(5) . . ? B8A B5A B3A 54.1(4) . . ? B2A B5A B3A 86.9(4) . . ? C1A B5A H5C 113(3) . . ? B11A B5A H5C 113(3) . . ? B9A B5A H5C 116(3) . . ? B8A B5A H5C 121(3) . . ? B2A B5A H5C 119(3) . . ? B3A B5A H5C 124(3) . . ? C10A B6A B9A 104.8(5) . . ? C10A B6A B12A 60.5(4) . . ? B9A B6A B12A 58.8(4) . . ? C10A B6A B2A 115.1(5) . . ? B9A B6A B2A 59.8(4) . . ? B12A B6A B2A 113.0(5) . . ? C10A B6A Fe4 65.5(3) . . ? B9A B6A Fe4 114.4(4) . . ? B12A B6A Fe4 119.1(4) . . ? B2A B6A Fe4 67.5(3) . . ? C10A B6A H6C 122(3) . . ? B9A B6A H6C 123(3) . . ? B12A B6A H6C 118(3) . . ? B2A B6A H6C 116(3) . . ? Fe4 B6A H6C 114(3) . . ? C10A B7A B8A 105.1(5) . . ? C10A B7A B13A 60.6(4) . . ? B8A B7A B13A 58.7(4) . . ? C10A B7A B3A 115.9(5) . . ? B8A B7A B3A 60.0(4) . . ? B13A B7A B3A 113.3(5) . . ? C10A B7A Fe4 65.6(3) . . ? B8A B7A Fe4 114.7(4) . . ? B13A B7A Fe4 119.2(5) . . ? B3A B7A Fe4 67.9(3) . . ? C10A B7A H7C 124(3) . . ? B8A B7A H7C 120(3) . . ? B13A B7A H7C 117(3) . . ? B3A B7A H7C 114(3) . . ? Fe4 B7A H7C 115(3) . . ? B13A B8A B7A 60.7(4) . . ? B13A B8A B11A 61.2(4) . . ? B7A B8A B11A 108.2(5) . . ? B13A B8A B3A 116.5(5) . . ? B7A B8A B3A 61.6(4) . . ? B11A B8A B3A 117.6(5) . . ? B13A B8A B5A 107.2(5) . . ? B7A B8A B5A 105.0(5) . . ? B11A B8A B5A 58.8(4) . . ? B3A B8A B5A 65.4(4) . . ? B13A B8A H8C 117(3) . . ? B7A B8A H8C 119(3) . . ? B11A B8A H8C 123(3) . . ? B3A B8A H8C 112(3) . . ? B5A B8A H8C 129(3) . . ? B12A B9A B6A 60.9(4) . . ? B12A B9A B11A 61.1(4) . . ? B6A B9A B11A 108.2(5) . . ? B12A B9A B2A 116.4(5) . . ? B6A B9A B2A 61.5(4) . . ? B11A B9A B2A 117.2(5) . . ? B12A B9A B5A 107.3(5) . . ? B6A B9A B5A 105.2(5) . . ? B11A B9A B5A 58.8(4) . . ? B2A B9A B5A 65.2(4) . . ? B12A B9A H9C 116(3) . . ? B6A B9A H9C 118(3) . . ? B11A B9A H9C 123(3) . . ? B2A B9A H9C 113(3) . . ? B5A B9A H9C 129(3) . . ? B7A C10A B6A 122.8(5) . . ? B7A C10A B13A 62.2(4) . . ? B6A C10A B13A 114.5(5) . . ? B7A C10A B12A 114.5(5) . . ? B6A C10A B12A 62.4(4) . . ? B13A C10A B12A 60.1(4) . . ? B7A C10A Fe4 69.9(3) . . ? B6A C10A Fe4 69.9(3) . . ? B13A C10A Fe4 124.3(4) . . ? B12A C10A Fe4 124.4(4) . . ? B7A C10A H10C 115(3) . . ? B6A C10A H10C 114(3) . . ? B13A C10A H10C 118(3) . . ? B12A C10A H10C 117(3) . . ? Fe4 C10A H10C 107(3) . . ? B8A B11A B9A 116.4(5) . . ? B8A B11A B13A 58.4(4) . . ? B9A B11A B13A 108.0(5) . . ? B8A B11A B12A 108.2(5) . . ? B9A B11A B12A 58.6(4) . . ? B13A B11A B12A 58.7(4) . . ? B8A B11A B5A 65.0(4) . . ? B9A B11A B5A 64.8(4) . . ? B13A B11A B5A 109.9(5) . . ? B12A B11A B5A 110.1(5) . . ? B8A B11A H11C 118(3) . . ? B9A B11A H11C 119(3) . . ? B13A B11A H11C 123(3) . . ? B12A B11A H11C 123(3) . . ? B5A B11A H11C 118(3) . . ? B9A B12A B13A 110.9(5) . . ? B9A B12A C10A 103.3(5) . . ? B13A B12A C10A 59.7(4) . . ? B9A B12A B6A 60.2(4) . . ? B13A B12A B6A 109.6(5) . . ? C10A B12A B6A 57.1(4) . . ? B9A B12A B11A 60.3(4) . . ? B13A B12A B11A 60.5(4) . . ? C10A B12A B11A 102.3(5) . . ? B6A B12A B11A 107.1(5) . . ? B9A B12A H12C 123(3) . . ? B13A B12A H12C 121(3) . . ? C10A B12A H12C 121(3) . . ? B6A B12A H12C 117(3) . . ? B11A B12A H12C 130(3) . . ? B8A B13A C10A 103.9(5) . . ? B8A B13A B12A 111.6(5) . . ? C10A B13A B12A 60.2(4) . . ? B8A B13A B7A 60.6(4) . . ? C10A B13A B7A 57.2(4) . . ? B12A B13A B7A 110.2(5) . . ? B8A B13A B11A 60.3(4) . . ? C10A B13A B11A 102.8(5) . . ? B12A B13A B11A 60.8(4) . . ? B7A B13A B11A 107.4(5) . . ? B8A B13A H13C 121(3) . . ? C10A B13A H13C 126(3) . . ? B12A B13A H13C 120(3) . . ? B7A B13A H13C 119(3) . . ? B11A B13A H13C 125(3) . . ? B2B C1B B3B 128.3(8) . . ? B2B C1B B5B 88.4(7) . . ? B3B C1B B5B 70.7(5) . . ? B2B C1B Fe4 77.0(6) . . ? B3B C1B Fe4 75.2(4) . . ? B5B C1B Fe4 121.2(5) . . ? B2B C1B H1D 115(4) . . ? B3B C1B H1D 117(4) . . ? B5B C1B H1D 122(4) . . ? Fe4 C1B H1D 116(4) . . ? C1B B2B B9B 110.7(8) . . ? C1B B2B B6B 117.0(8) . . ? B9B B2B B6B 64.7(8) . . ? C1B B2B Fe4 63.6(4) . . ? B9B B2B Fe4 116.5(8) . . ? B6B B2B Fe4 65.2(5) . . ? C1B B2B H2D 106(5) . . ? B9B B2B H2D 118(5) . . ? B6B B2B H2D 133(5) . . ? Fe4 B2B H2D 124(5) . . ? C1B B3B B8B 111.4(6) . . ? C1B B3B B7B 116.3(6) . . ? B8B B3B B7B 58.9(4) . . ? C1B B3B B5B 57.7(4) . . ? B8B B3B B5B 59.5(4) . . ? B7B B3B B5B 105.0(5) . . ? C1B B3B Fe4 62.6(3) . . ? B8B B3B Fe4 112.0(4) . . ? B7B B3B Fe4 65.9(3) . . ? B5B B3B Fe4 104.5(4) . . ? C1B B3B H3D 123(3) . . ? B8B B3B H3D 114(3) . . ? B7B B3B H3D 115(3) . . ? B5B B3B H3D 126(3) . . ? Fe4 B3B H3D 123(3) . . ? C1B B5B B11B 124.3(7) . . ? C1B B5B B8B 103.5(5) . . ? B11B B5B B8B 57.8(4) . . ? C1B B5B B3B 51.6(4) . . ? B11B B5B B3B 107.1(5) . . ? B8B B5B B3B 56.9(4) . . ? C1B B5B B9B 86.9(6) . . ? B11B B5B B9B 51.4(5) . . ? B8B B5B B9B 98.1(6) . . ? B3B B5B B9B 112.7(6) . . ? C1B B5B H5D 116(4) . . ? B11B B5B H5D 117(4) . . ? B8B B5B H5D 125(4) . . ? B3B B5B H5D 125(4) . . ? B9B B5B H5D 120(4) . . ? B12B B6B C10B 73.5(8) . . ? B12B B6B B2B 107.7(9) . . ? C10B B6B B2B 118.1(8) . . ? B12B B6B B9B 54.1(7) . . ? C10B B6B B9B 110.9(7) . . ? B2B B6B B9B 56.1(7) . . ? B12B B6B Fe4 126.0(8) . . ? C10B B6B Fe4 63.8(4) . . ? B2B B6B Fe4 69.1(5) . . ? B9B B6B Fe4 113.0(7) . . ? B12B B6B H6D 115.3 . . ? C10B B6B H6D 113.1 . . ? B2B B6B H6D 119.9 . . ? B9B B6B H6D 127.6 . . ? Fe4 B6B H6D 111.0 . . ? C10B B7B B8B 108.0(6) . . ? C10B B7B B3B 115.8(5) . . ? B8B B7B B3B 59.6(4) . . ? C10B B7B B13B 56.9(5) . . ? B8B B7B B13B 59.6(4) . . ? B3B B7B B13B 108.8(5) . . ? C10B B7B Fe4 63.6(3) . . ? B8B B7B Fe4 113.4(4) . . ? B3B B7B Fe4 66.9(3) . . ? B13B B7B Fe4 109.2(5) . . ? C10B B7B H7D 120(3) . . ? B8B B7B H7D 119(3) . . ? B3B B7B H7D 120(3) . . ? B13B B7B H7D 120(3) . . ? Fe4 B7B H7D 121(3) . . ? B11B B8B B7B 111.8(5) . . ? B11B B8B B3B 113.8(5) . . ? B7B B8B B3B 61.5(4) . . ? B11B B8B B13B 59.8(5) . . ? B7B B8B B13B 62.3(4) . . ? B3B B8B B13B 112.4(5) . . ? B11B B8B B5B 59.1(5) . . ? B7B B8B B5B 110.1(5) . . ? B3B B8B B5B 63.6(4) . . ? B13B B8B B5B 106.4(6) . . ? B11B B8B H8D 121(3) . . ? B7B B8B H8D 118(3) . . ? B3B B8B H8D 116(3) . . ? B13B B8B H8D 122(3) . . ? B5B B8B H8D 123(3) . . ? B12B B9B B11B 66.2(8) . . ? B12B B9B B2B 112.6(9) . . ? B11B B9B B2B 119.4(8) . . ? B12B B9B B6B 56.1(7) . . ? B11B B9B B6B 106.5(8) . . ? B2B B9B B6B 59.2(7) . . ? B12B B9B B5B 109.0(8) . . ? B11B B9B B5B 55.0(5) . . ? B2B B9B B5B 72.2(7) . . ? B6B B9B B5B 105.9(6) . . ? B12B B9B H9D 114(5) . . ? B11B B9B H9D 119(5) . . ? B2B B9B H9D 115(5) . . ? B6B B9B H9D 123(5) . . ? B5B B9B H9D 127(5) . . ? B7B C10B B13B 68.3(5) . . ? B7B C10B B6B 121.0(7) . . ? B13B C10B B6B 98.5(7) . . ? B7B C10B B12B 110.0(6) . . ? B13B C10B B12B 51.3(6) . . ? B6B C10B B12B 51.4(6) . . ? B7B C10B Fe4 73.0(4) . . ? B13B C10B Fe4 124.8(5) . . ? B6B C10B Fe4 69.9(4) . . ? B12B C10B Fe4 113.2(6) . . ? B7B C10B H10D 114(4) . . ? B13B C10B H10D 120(4) . . ? B6B C10B H10D 121(4) . . ? B12B C10B H10D 124(4) . . ? Fe4 C10B H10D 111(4) . . ? B9B B11B B8B 118.9(6) . . ? B9B B11B B5B 73.6(6) . . ? B8B B11B B5B 63.1(5) . . ? B9B B11B B13B 100.6(7) . . ? B8B B11B B13B 61.7(5) . . ? B5B B11B B13B 111.0(6) . . ? B9B B11B B12B 54.3(7) . . ? B8B B11B B12B 108.3(6) . . ? B5B B11B B12B 114.5(7) . . ? B13B B11B B12B 53.9(7) . . ? B9B B11B H11D 125(4) . . ? B8B B11B H11D 113(4) . . ? B5B B11B H11D 117(4) . . ? B13B B11B H11D 120(4) . . ? B12B B11B H11D 124(4) . . ? B9B B12B B13B 112.4(10) . . ? B9B B12B B6B 69.7(9) . . ? B13B B12B B6B 104.2(9) . . ? B9B B12B B11B 59.6(7) . . ? B13B B12B B11B 62.5(6) . . ? B6B B12B B11B 111.5(10) . . ? B9B B12B C10B 108.7(8) . . ? B13B B12B C10B 53.8(6) . . ? B6B B12B C10B 55.1(6) . . ? B11B B12B C10B 101.2(7) . . ? B9B B12B H12D 115.9 . . ? B13B B12B H12D 122.8 . . ? B6B B12B H12D 119.7 . . ? B11B B12B H12D 122.3 . . ? C10B B12B H12D 128.7 . . ? B12B B13B C10B 74.9(7) . . ? B12B B13B B11B 63.6(7) . . ? C10B B13B B11B 116.8(8) . . ? B12B B13B B8B 113.8(9) . . ? C10B B13B B8B 105.0(6) . . ? B11B B13B B8B 58.4(5) . . ? B12B B13B B7B 118.2(8) . . ? C10B B13B B7B 54.8(4) . . ? B11B B13B B7B 107.1(6) . . ? B8B B13B B7B 58.1(4) . . ? B12B B13B H13D 118(5) . . ? C10B B13B H13D 119(5) . . ? B11B B13B H13D 122(5) . . ? B8B B13B H13D 118(5) . . ? B7B B13B H13D 116(5) . . ? O1W K1 O1W 29.6(6) . 2_567 ? O1W K1 O6 92.6(4) . . ? O1W K1 O6 89.8(4) 2_567 . ? O1W K1 O5 80.9(4) . . ? O1W K1 O5 105.5(4) 2_567 . ? O6 K1 O5 61.86(15) . . ? O1W K1 O1 105.6(3) . . ? O1W K1 O1 78.4(3) 2_567 . ? O6 K1 O1 61.34(15) . . ? O5 K1 O1 123.02(17) . . ? O1W K1 O3 83.0(4) . . ? O1W K1 O3 85.6(4) 2_567 . ? O6 K1 O3 175.26(16) . . ? O5 K1 O3 118.75(16) . . ? O1 K1 O3 118.23(17) . . ? O1W K1 O4 65.2(3) . . ? O1W K1 O4 92.0(3) 2_567 . ? O6 K1 O4 120.34(16) . . ? O5 K1 O4 60.35(15) . . ? O1 K1 O4 170.36(16) . . ? O3 K1 O4 59.20(15) . . ? O1W K1 O2 85.3(4) . . ? O1W K1 O2 61.2(4) 2_567 . ? O6 K1 O2 118.43(17) . . ? O5 K1 O2 166.26(16) . . ? O1 K1 O2 60.32(15) . . ? O3 K1 O2 59.71(15) . . ? O4 K1 O2 114.10(16) . . ? O1W K1 C11 107.3(4) . . ? O1W K1 C11 94.8(4) 2_567 . ? O6 K1 C11 22.13(15) . . ? O5 K1 C11 81.23(17) . . ? O1 K1 C11 42.24(17) . . ? O3 K1 C11 159.24(18) . . ? O4 K1 C11 141.37(18) . . ? O2 K1 C11 102.36(18) . . ? O1W K1 C10 96.2(4) . . ? O1W K1 C10 103.6(4) 2_567 . ? O6 K1 C10 21.92(16) . . ? O5 K1 C10 42.01(16) . . ? O1 K1 C10 81.26(17) . . ? O3 K1 C10 160.08(18) . . ? O4 K1 C10 102.30(17) . . ? O2 K1 C10 140.18(18) . . ? C11 K1 C10 39.22(18) . . ? O1W K1 K1 15.0(3) . 2_567 ? O1W K1 K1 14.6(3) 2_567 2_567 ? O6 K1 K1 91.18(12) . 2_567 ? O5 K1 K1 93.45(11) . 2_567 ? O1 K1 K1 91.84(12) . 2_567 ? O3 K1 K1 84.10(11) . 2_567 ? O4 K1 K1 78.75(12) . 2_567 ? O2 K1 K1 72.88(11) . 2_567 ? C11 K1 K1 101.26(14) . 2_567 ? C10 K1 K1 100.25(14) . 2_567 ? O1W K1 H2C 158.1(11) . . ? O1W K1 H2C 150.1(10) 2_567 . ? O6 K1 H2C 67.6(9) . . ? O5 K1 H2C 81.4(12) . . ? O1 K1 H2C 73.7(10) . . ? O3 K1 H2C 117.1(9) . . ? O4 K1 H2C 115.9(11) . . ? O2 K1 H2C 111.7(12) . . ? C11 K1 H2C 57.0(8) . . ? C10 K1 H2C 61.9(10) . . ? K1 K1 H2C 158.1(8) 2_567 . ? O1W K1 H1W 20.5(8) . . ? O1W K1 H1W 23(3) 2_567 . ? O6 K1 H1W 75.6(18) . . ? O5 K1 H1W 83(3) . . ? O1 K1 H1W 87.3(16) . . ? O3 K1 H1W 99.8(18) . . ? O4 K1 H1W 84.1(14) . . ? O2 K1 H1W 84(3) . . ? C11 K1 H1W 87.6(11) . . ? C10 K1 H1W 84(2) . . ? K1 K1 H1W 16(2) 2_567 . ? H2C K1 H1W 143.1(19) . . ? C1 O1 C12 110.9(6) . . ? C1 O1 K1 117.7(4) . . ? C12 O1 K1 116.3(4) . . ? C3 O2 C2 112.3(6) . . ? C3 O2 K1 114.5(4) . . ? C2 O2 K1 114.2(4) . . ? C4 O3 C5 110.4(6) . . ? C4 O3 K1 115.5(4) . . ? C5 O3 K1 116.6(4) . . ? C7 O4 C6 110.8(6) . . ? C7 O4 K1 112.9(4) . . ? C6 O4 K1 111.4(4) . . ? C9 O5 C8 112.1(5) . . ? C9 O5 K1 114.7(4) . . ? C8 O5 K1 116.3(4) . . ? C10 O6 C11 111.5(5) . . ? C10 O6 K1 112.7(4) . . ? C11 O6 K1 112.3(4) . . ? O1 C1 C2 108.6(6) . . ? O1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? O1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.3 . . ? O2 C2 C1 110.5(6) . . ? O2 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? O2 C3 C4 109.4(6) . . ? O2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? O3 C4 C3 109.2(6) . . ? O3 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? O3 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? O3 C5 C6 108.2(6) . . ? O3 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O3 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? O4 C6 C5 107.4(6) . . ? O4 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? O4 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? O4 C7 C8 110.1(6) . . ? O4 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? O4 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.2 . . ? O5 C8 C7 109.6(6) . . ? O5 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? O5 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O5 C9 C10 108.5(5) . . ? O5 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O5 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? O6 C10 C9 107.9(6) . . ? O6 C10 K1 45.4(3) . . ? C9 C10 K1 79.5(4) . . ? O6 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? K1 C10 H10A 88.5 . . ? O6 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? K1 C10 H10B 155.0 . . ? H10A C10 H10B 108.4 . . ? O6 C11 C12 108.8(6) . . ? O6 C11 K1 45.6(3) . . ? C12 C11 K1 82.1(4) . . ? O6 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? K1 C11 H11A 155.4 . . ? O6 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? K1 C11 H11B 86.2 . . ? H11A C11 H11B 108.3 . . ? O1 C12 C11 109.3(6) . . ? O1 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? O1 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? O1W O1W K1 78.4(11) 2_567 . ? O1W O1W K1 72.0(11) 2_567 2_567 ? K1 O1W K1 150.4(6) . 2_567 ? O1W O1W H1W 51(8) 2_567 . ? K1 O1W H1W 82(8) . . ? K1 O1W H1W 80(8) 2_567 . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 24.80 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.790 _refine_diff_density_min -1.336 _refine_diff_density_rms 0.111 #===end data_8 _database_code_depnum_ccdc_archive 'CCDC 663042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H24 B20 Fe, C10 H16 N' _chemical_formula_sum 'C14 H40 B20 Fe N' _chemical_formula_weight 494.52 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 P2(1)/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 17.559(3) _cell_length_b 7.5023(12) _cell_length_c 20.871(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.765(10) _cell_angle_gamma 90.00 _cell_volume 2709.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3790 _cell_measurement_theta_min 2.807 _cell_measurement_theta_max 23.078 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 0.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.763 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details 'SADABS (Shedrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex2 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 68196 _diffrn_reflns_av_R_equivalents 0.1576 _diffrn_reflns_av_sigmaI/netI 0.1230 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 30.09 _reflns_number_total 7944 _reflns_number_gt 4578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^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 7944 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1296 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1362 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe4 Fe 0.20264(2) 0.97242(5) 0.025922(16) 0.01243(10) Uani 1 1 d . . . C1A C 0.18776(15) 0.8340(4) 0.10823(12) 0.0163(6) Uani 1 1 d . . . H1C H 0.1891(15) 0.708(4) 0.1129(12) 0.020 Uiso 1 1 d . . . B2A B 0.10893(18) 0.9267(4) 0.08955(14) 0.0165(6) Uani 1 1 d . . . H2C H 0.0570(15) 0.841(3) 0.0759(12) 0.020 Uiso 1 1 d . . . B3A B 0.26689(17) 0.9229(4) 0.12847(13) 0.0154(6) Uani 1 1 d . . . H3C H 0.3201(15) 0.838(3) 0.1422(12) 0.018 Uiso 1 1 d . . . B5A B 0.17638(17) 0.9708(4) 0.17436(14) 0.0168(6) Uani 1 1 d . . . H5C H 0.1668(15) 0.891(4) 0.2141(12) 0.020 Uiso 1 1 d . . . B6A B 0.11078(17) 1.1483(4) 0.05367(14) 0.0150(6) Uani 1 1 d . . . H6C H 0.0666(14) 1.188(3) 0.0146(12) 0.018 Uiso 1 1 d . . . B7A B 0.27845(17) 1.1443(4) 0.09720(14) 0.0155(6) Uani 1 1 d . . . H7C H 0.3342(15) 1.174(3) 0.0833(12) 0.019 Uiso 1 1 d . . . B8A B 0.26520(17) 1.1175(4) 0.17849(14) 0.0166(6) Uani 1 1 d . . . H8C H 0.3146(15) 1.116(4) 0.2191(12) 0.020 Uiso 1 1 d . . . B9A B 0.09487(17) 1.1215(4) 0.13437(14) 0.0150(6) Uani 1 1 d . . . H9C H 0.0377(15) 1.121(4) 0.1459(12) 0.018 Uiso 1 1 d . . . C10A C 0.19773(14) 1.2438(3) 0.06012(12) 0.0141(5) Uani 1 1 d . . . H10C H 0.2031(14) 1.326(4) 0.0277(12) 0.017 Uiso 1 1 d . . . B11A B 0.17525(17) 1.2102(4) 0.18629(14) 0.0168(6) Uani 1 1 d . . . H11C H 0.1679(14) 1.258(4) 0.2356(12) 0.020 Uiso 1 1 d . . . B12A B 0.13643(17) 1.3173(4) 0.11151(14) 0.0166(6) Uani 1 1 d . . . H12C H 0.1081(15) 1.444(4) 0.1035(12) 0.020 Uiso 1 1 d . . . B13A B 0.23672(17) 1.3157(4) 0.13824(14) 0.0165(6) Uani 1 1 d . . . H13C H 0.2668(15) 1.449(4) 0.1463(12) 0.020 Uiso 1 1 d . . . C1B C 0.11879(15) 0.9117(4) -0.05249(12) 0.0168(6) Uani 1 1 d . . . H1D H 0.0645(16) 0.932(4) -0.0560(12) 0.020 Uiso 1 1 d . . . B2B B 0.15093(18) 0.7266(4) -0.03142(14) 0.0195(7) Uani 1 1 d . . . H2D H 0.1041(15) 0.612(4) -0.0170(12) 0.023 Uiso 1 1 d . . . B3B B 0.16289(17) 1.0671(4) -0.07794(14) 0.0169(6) Uani 1 1 d . . . H3D H 0.1298(15) 1.198(4) -0.0935(12) 0.020 Uiso 1 1 d . . . B5B B 0.15547(18) 0.8294(4) -0.11970(14) 0.0182(6) Uani 1 1 d . . . H5D H 0.1098(15) 0.800(4) -0.1622(12) 0.022 Uiso 1 1 d . . . B6B B 0.25403(18) 0.7141(4) -0.00071(14) 0.0179(6) Uani 1 1 d . . . H6D H 0.2721(15) 0.618(4) 0.0408(12) 0.021 Uiso 1 1 d . . . B7B B 0.26650(17) 1.0792(4) -0.04965(14) 0.0153(6) Uani 1 1 d . . . H7D H 0.2887(14) 1.216(4) -0.0387(12) 0.018 Uiso 1 1 d . . . B8B B 0.23001(17) 1.0084(4) -0.12948(14) 0.0167(6) Uani 1 1 d . . . H8D H 0.2276(15) 1.105(4) -0.1743(12) 0.020 Uiso 1 1 d . . . B9B B 0.21786(18) 0.6372(4) -0.07974(15) 0.0193(7) Uani 1 1 d . . . H9D H 0.2046(15) 0.497(4) -0.0921(13) 0.023 Uiso 1 1 d . . . C10B C 0.30538(15) 0.8962(4) -0.01135(12) 0.0163(6) Uani 1 1 d . . . H10D H 0.3506(15) 0.915(4) 0.0200(13) 0.020 Uiso 1 1 d . . . B11B B 0.25204(18) 0.7799(4) -0.13510(14) 0.0181(6) Uani 1 1 d . . . H11D H 0.2581(14) 0.728(4) -0.1836(12) 0.022 Uiso 1 1 d . . . B12B B 0.31262(18) 0.7151(4) -0.06135(14) 0.0188(7) Uani 1 1 d . . . H12D H 0.3634(15) 0.623(4) -0.0557(12) 0.023 Uiso 1 1 d . . . B13B B 0.31946(18) 0.9313(4) -0.09074(14) 0.0188(7) Uani 1 1 d . . . H13D H 0.3762(15) 0.980(4) -0.1005(13) 0.023 Uiso 1 1 d . . . C1 C -0.02097(15) 0.9451(3) 0.29813(12) 0.0177(6) Uani 1 1 d . . . C2 C -0.09182(15) 1.0243(3) 0.30057(12) 0.0180(5) Uani 1 1 d . . . H2A H -0.1339 1.0051 0.2661 0.022 Uiso 1 1 calc R . . C3 C -0.10204(16) 1.1314(4) 0.35278(13) 0.0227(6) Uani 1 1 d . . . H3A H -0.1508 1.1855 0.3537 0.027 Uiso 1 1 calc R . . C4 C -0.04132(17) 1.1594(4) 0.40349(14) 0.0264(7) Uani 1 1 d . . . H4A H -0.0485 1.2307 0.4396 0.032 Uiso 1 1 calc R . . C5 C 0.03022(18) 1.0825(4) 0.40108(14) 0.0308(7) Uani 1 1 d . . . H5A H 0.0722 1.1022 0.4355 0.037 Uiso 1 1 calc R . . C6 C 0.04043(16) 0.9771(4) 0.34863(14) 0.0267(7) Uani 1 1 d . . . H6A H 0.0896 0.9263 0.3471 0.032 Uiso 1 1 calc R . . C7 C -0.00808(16) 0.8317(4) 0.24146(13) 0.0217(6) Uani 1 1 d . . . H7A H 0.0467 0.8436 0.2362 0.026 Uiso 1 1 calc R . . H7B H -0.0402 0.8797 0.2016 0.026 Uiso 1 1 calc R . . C8 C 0.01413(9) 0.5541(2) 0.30934(7) 0.0236(6) Uani 1 1 d . . . H8A H 0.0049 0.4252 0.3090 0.035 Uiso 1 1 calc R . . H8B H -0.0060 0.6082 0.3458 0.035 Uiso 1 1 calc R . . H8E H 0.0698 0.5769 0.3141 0.035 Uiso 1 1 calc R . . N1 N -0.02633(9) 0.6340(2) 0.24647(7) 0.0184(5) Uani 1 1 d R . . C10 C 0.00169(13) 0.5399(3) 0.19149(7) 0.0280(7) Uani 1 1 d R . . H10F H -0.0085 0.4120 0.1940 0.042 Uiso 1 1 d R . . H10G H 0.0574 0.5596 0.1945 0.042 Uiso 1 1 d R . . H10H H -0.0254 0.5869 0.1500 0.042 Uiso 1 1 d R . . C9 C -0.11153(14) 0.6041(4) 0.24206(13) 0.0214(6) Uani 1 1 d . . . H9A H -0.1387 0.6493 0.2003 0.032 Uiso 1 1 calc R . . H9B H -0.1298 0.6671 0.2777 0.032 Uiso 1 1 calc R . . H9E H -0.1217 0.4762 0.2453 0.032 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 Fe4 0.01333(18) 0.01090(18) 0.01281(17) 0.00031(15) 0.00154(13) -0.00033(16) C1A 0.0240(14) 0.0125(13) 0.0127(12) 0.0027(10) 0.0041(11) -0.0010(11) B2A 0.0201(15) 0.0175(16) 0.0125(14) 0.0001(12) 0.0042(12) 0.0010(12) B3A 0.0187(15) 0.0159(16) 0.0114(13) 0.0008(11) 0.0022(11) 0.0004(12) B5A 0.0185(14) 0.0166(15) 0.0155(13) -0.0012(13) 0.0036(11) -0.0023(13) B6A 0.0157(15) 0.0131(15) 0.0159(14) -0.0017(12) 0.0019(12) 0.0002(12) B7A 0.0144(14) 0.0152(15) 0.0169(15) -0.0005(12) 0.0024(12) -0.0015(12) B8A 0.0190(15) 0.0164(16) 0.0138(14) -0.0028(12) 0.0009(12) 0.0017(12) B9A 0.0148(15) 0.0158(16) 0.0148(14) -0.0012(12) 0.0037(11) 0.0013(12) C10A 0.0195(14) 0.0109(13) 0.0123(12) 0.0003(10) 0.0037(10) -0.0001(10) B11A 0.0182(15) 0.0161(16) 0.0163(14) -0.0004(12) 0.0037(12) 0.0014(12) B12A 0.0177(15) 0.0162(16) 0.0162(14) -0.0003(12) 0.0036(12) -0.0012(12) B13A 0.0191(15) 0.0151(16) 0.0150(14) -0.0003(12) 0.0018(12) -0.0005(12) C1B 0.0148(13) 0.0200(14) 0.0143(12) -0.0034(11) -0.0013(10) -0.0003(11) B2B 0.0212(16) 0.0222(17) 0.0147(14) -0.0025(13) 0.0020(12) -0.0015(13) B3B 0.0164(15) 0.0192(17) 0.0151(14) -0.0014(12) 0.0026(11) -0.0019(12) B5B 0.0211(16) 0.0174(16) 0.0163(15) -0.0005(12) 0.0037(12) -0.0027(13) B6B 0.0205(16) 0.0140(15) 0.0190(15) -0.0001(12) 0.0031(12) -0.0005(12) B7B 0.0176(15) 0.0139(15) 0.0150(14) 0.0005(12) 0.0045(12) -0.0019(12) B8B 0.0181(14) 0.0167(17) 0.0156(14) 0.0001(12) 0.0035(11) -0.0001(12) B9B 0.0225(16) 0.0146(16) 0.0206(16) 0.0014(12) 0.0033(13) 0.0002(13) C10B 0.0161(13) 0.0161(14) 0.0166(13) -0.0008(10) 0.0024(11) 0.0018(11) B11B 0.0214(16) 0.0185(16) 0.0148(14) -0.0037(12) 0.0040(12) -0.0004(13) B12B 0.0215(16) 0.0161(16) 0.0188(15) -0.0044(12) 0.0033(12) 0.0026(13) B13B 0.0216(16) 0.0213(18) 0.0145(14) -0.0035(12) 0.0058(12) -0.0019(13) C1 0.0219(14) 0.0118(14) 0.0206(13) 0.0008(11) 0.0065(11) -0.0010(11) C2 0.0226(13) 0.0139(13) 0.0175(12) 0.0018(11) 0.0029(10) -0.0014(11) C3 0.0245(15) 0.0176(15) 0.0274(15) 0.0005(12) 0.0082(12) -0.0012(12) C4 0.0370(18) 0.0195(16) 0.0227(15) -0.0027(12) 0.0048(13) -0.0036(13) C5 0.0321(17) 0.0237(17) 0.0319(17) -0.0034(13) -0.0080(14) -0.0025(13) C6 0.0201(14) 0.0212(15) 0.0369(17) -0.0023(13) -0.0003(12) 0.0023(12) C7 0.0252(15) 0.0166(15) 0.0254(15) 0.0039(12) 0.0106(12) -0.0011(12) C8 0.0199(14) 0.0233(16) 0.0265(14) 0.0063(12) 0.0011(11) 0.0020(12) N1 0.0181(11) 0.0172(12) 0.0210(12) 0.0001(9) 0.0067(9) 0.0003(9) C10 0.0302(16) 0.0261(16) 0.0311(16) -0.0076(14) 0.0147(13) 0.0009(14) C9 0.0165(14) 0.0225(15) 0.0255(15) -0.0012(12) 0.0044(11) -0.0008(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe4 C1B 2.058(2) . ? Fe4 C1A 2.062(3) . ? Fe4 C10B 2.159(3) . ? Fe4 C10A 2.164(3) . ? Fe4 B7A 2.231(3) . ? Fe4 B7B 2.233(3) . ? Fe4 B6A 2.235(3) . ? Fe4 B6B 2.247(3) . ? Fe4 B3A 2.274(3) . ? Fe4 B3B 2.275(3) . ? Fe4 B2B 2.300(3) . ? Fe4 B2A 2.309(3) . ? C1A B3A 1.534(4) . ? C1A B2A 1.539(4) . ? C1A B5A 1.758(4) . ? C1A H1C 0.95(3) . ? B2A B9A 1.775(4) . ? B2A B6A 1.826(4) . ? B2A B5A 1.984(4) . ? B2A H2C 1.11(3) . ? B3A B8A 1.798(4) . ? B3A B7A 1.809(4) . ? B3A B5A 2.022(4) . ? B3A H3C 1.13(3) . ? B5A B11A 1.814(4) . ? B5A B8A 1.899(4) . ? B5A B9A 1.902(4) . ? B5A H5C 1.06(3) . ? B6A C10A 1.671(4) . ? B6A B12A 1.756(4) . ? B6A B9A 1.765(4) . ? B6A H6C 1.07(2) . ? B7A C10A 1.671(4) . ? B7A B8A 1.763(4) . ? B7A B13A 1.771(4) . ? B7A H7C 1.09(3) . ? B8A B13A 1.739(4) . ? B8A B11A 1.759(4) . ? B8A H8C 1.11(3) . ? B9A B12A 1.742(4) . ? B9A B11A 1.758(4) . ? B9A H9C 1.07(3) . ? C10A B12A 1.734(4) . ? C10A B13A 1.743(4) . ? C10A H10C 0.93(3) . ? B11A B13A 1.779(4) . ? B11A B12A 1.785(4) . ? B11A H11C 1.12(3) . ? B12A B13A 1.755(4) . ? B12A H12C 1.07(3) . ? B13A H13C 1.13(3) . ? C1B B2B 1.535(4) . ? C1B B3B 1.543(4) . ? C1B B5B 1.752(4) . ? C1B H1D 0.96(3) . ? B2B B9B 1.803(5) . ? B2B B6B 1.817(4) . ? B2B B5B 2.012(4) . ? B2B H2D 1.26(3) . ? B3B B8B 1.780(4) . ? B3B B7B 1.817(4) . ? B3B B5B 1.979(4) . ? B3B H3D 1.16(3) . ? B5B B11B 1.817(4) . ? B5B B8B 1.910(4) . ? B5B B9B 1.914(4) . ? B5B H5D 1.11(3) . ? B6B C10B 1.672(4) . ? B6B B9B 1.761(4) . ? B6B B12B 1.761(4) . ? B6B H6D 1.13(3) . ? B7B C10B 1.675(4) . ? B7B B13B 1.761(4) . ? B7B B8B 1.763(4) . ? B7B H7D 1.11(3) . ? B8B B13B 1.739(4) . ? B8B B11B 1.765(4) . ? B8B H8D 1.18(3) . ? B9B B12B 1.744(4) . ? B9B B11B 1.754(4) . ? B9B H9D 1.10(3) . ? C10B B12B 1.731(4) . ? C10B B13B 1.736(4) . ? C10B H10D 0.95(3) . ? B11B B13B 1.782(4) . ? B11B B12B 1.784(4) . ? B11B H11D 1.11(3) . ? B12B B13B 1.745(5) . ? B12B H12D 1.12(3) . ? B13B H13D 1.11(3) . ? C1 C2 1.387(4) . ? C1 C6 1.395(4) . ? C1 C7 1.505(4) . ? C2 C3 1.390(4) . ? C2 H2A 0.9500 . ? C3 C4 1.385(4) . ? C3 H3A 0.9500 . ? C4 C5 1.391(4) . ? C4 H4A 0.9500 . ? C5 C6 1.386(4) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 N1 1.525(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N1 1.5066 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8E 0.9800 . ? N1 C10 1.4995 . ? N1 C9 1.500(3) . ? C10 H10F 0.9796 . ? C10 H10G 0.9805 . ? C10 H10H 0.9799 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9E 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1B Fe4 C1A 112.11(11) . . ? C1B Fe4 C10B 100.58(10) . . ? C1A Fe4 C10B 113.49(10) . . ? C1B Fe4 C10A 114.03(10) . . ? C1A Fe4 C10A 100.44(10) . . ? C10B Fe4 C10A 116.77(10) . . ? C1B Fe4 B7A 157.47(11) . . ? C1A Fe4 B7A 83.17(11) . . ? C10B Fe4 B7A 87.30(11) . . ? C10A Fe4 B7A 44.67(10) . . ? C1B Fe4 B7B 83.97(11) . . ? C1A Fe4 B7B 156.79(11) . . ? C10B Fe4 B7B 44.79(11) . . ? C10A Fe4 B7B 87.04(10) . . ? B7A Fe4 B7B 87.10(11) . . ? C1B Fe4 B6A 83.47(11) . . ? C1A Fe4 B6A 83.24(11) . . ? C10B Fe4 B6A 158.99(11) . . ? C10A Fe4 B6A 44.62(10) . . ? B7A Fe4 B6A 82.02(11) . . ? B7B Fe4 B6A 116.24(11) . . ? C1B Fe4 B6B 82.85(11) . . ? C1A Fe4 B6B 83.38(11) . . ? C10B Fe4 B6B 44.56(11) . . ? C10A Fe4 B6B 158.94(10) . . ? B7A Fe4 B6B 116.38(11) . . ? B7B Fe4 B6B 82.18(11) . . ? B6A Fe4 B6B 155.64(11) . . ? C1B Fe4 B3A 152.36(11) . . ? C1A Fe4 B3A 41.09(10) . . ? C10B Fe4 B3A 89.11(10) . . ? C10A Fe4 B3A 83.37(10) . . ? B7A Fe4 B3A 47.33(11) . . ? B7B Fe4 B3A 119.67(11) . . ? B6A Fe4 B3A 96.73(11) . . ? B6B Fe4 B3A 86.32(11) . . ? C1B Fe4 B3B 41.33(11) . . ? C1A Fe4 B3B 152.78(11) . . ? C10B Fe4 B3B 83.07(10) . . ? C10A Fe4 B3B 89.87(10) . . ? B7A Fe4 B3B 120.46(11) . . ? B7B Fe4 B3B 47.53(11) . . ? B6A Fe4 B3B 86.81(11) . . ? B6B Fe4 B3B 96.01(11) . . ? B3A Fe4 B3B 166.07(11) . . ? C1B Fe4 B2B 40.78(11) . . ? C1A Fe4 B2B 86.27(11) . . ? C10B Fe4 B2B 83.13(11) . . ? C10A Fe4 B2B 153.10(10) . . ? B7A Fe4 B2B 161.59(11) . . ? B7B Fe4 B2B 96.97(11) . . ? B6A Fe4 B2B 111.69(11) . . ? B6B Fe4 B2B 47.10(11) . . ? B3A Fe4 B2B 116.59(11) . . ? B3B Fe4 B2B 73.99(11) . . ? C1B Fe4 B2A 86.61(11) . . ? C1A Fe4 B2A 40.75(10) . . ? C10B Fe4 B2A 152.68(11) . . ? C10A Fe4 B2A 82.98(10) . . ? B7A Fe4 B2A 96.04(11) . . ? B7B Fe4 B2A 162.14(11) . . ? B6A Fe4 B2A 47.35(11) . . ? B6B Fe4 B2A 111.68(11) . . ? B3A Fe4 B2A 73.90(11) . . ? B3B Fe4 B2A 117.45(11) . . ? B2B Fe4 B2A 85.60(11) . . ? B3A C1A B2A 127.4(2) . . ? B3A C1A B5A 75.43(18) . . ? B2A C1A B5A 73.62(18) . . ? B3A C1A Fe4 76.91(15) . . ? B2A C1A Fe4 78.28(15) . . ? B5A C1A Fe4 114.04(17) . . ? B3A C1A H1C 113.5(16) . . ? B2A C1A H1C 118.7(16) . . ? B5A C1A H1C 120.3(16) . . ? Fe4 C1A H1C 125.6(16) . . ? C1A B2A B9A 116.0(2) . . ? C1A B2A B6A 116.0(2) . . ? B9A B2A B6A 58.68(16) . . ? C1A B2A B5A 58.27(16) . . ? B9A B2A B5A 60.51(16) . . ? B6A B2A B5A 99.48(19) . . ? C1A B2A Fe4 60.97(14) . . ? B9A B2A Fe4 110.94(18) . . ? B6A B2A Fe4 64.21(13) . . ? B5A B2A Fe4 96.47(15) . . ? C1A B2A H2C 117.9(13) . . ? B9A B2A H2C 115.4(13) . . ? B6A B2A H2C 119.4(13) . . ? B5A B2A H2C 131.6(13) . . ? Fe4 B2A H2C 124.9(13) . . ? C1A B3A B8A 114.2(2) . . ? C1A B3A B7A 116.8(2) . . ? B8A B3A B7A 58.51(16) . . ? C1A B3A B5A 57.31(16) . . ? B8A B3A B5A 59.26(16) . . ? B7A B3A B5A 98.79(19) . . ? C1A B3A Fe4 62.00(13) . . ? B8A B3A Fe4 111.06(17) . . ? B7A B3A Fe4 65.07(12) . . ? B5A B3A Fe4 96.46(14) . . ? C1A B3A H3C 119.8(13) . . ? B8A B3A H3C 114.0(13) . . ? B7A B3A H3C 118.2(13) . . ? B5A B3A H3C 131.6(13) . . ? Fe4 B3A H3C 126.1(13) . . ? C1A B5A B11A 133.7(2) . . ? C1A B5A B8A 99.91(19) . . ? B11A B5A B8A 56.49(16) . . ? C1A B5A B9A 100.35(18) . . ? B11A B5A B9A 56.41(16) . . ? B8A B5A B9A 103.1(2) . . ? C1A B5A B2A 48.11(14) . . ? B11A B5A B2A 105.6(2) . . ? B8A B5A B2A 119.9(2) . . ? B9A B5A B2A 54.31(15) . . ? C1A B5A B3A 47.26(14) . . ? B11A B5A B3A 105.6(2) . . ? B8A B5A B3A 54.49(15) . . ? B9A B5A B3A 119.4(2) . . ? B2A B5A B3A 86.90(17) . . ? C1A B5A H5C 109.9(14) . . ? B11A B5A H5C 116.3(14) . . ? B8A B5A H5C 122.0(14) . . ? B9A B5A H5C 118.1(14) . . ? B2A B5A H5C 117.1(14) . . ? B3A B5A H5C 120.9(15) . . ? C10A B6A B12A 60.71(16) . . ? C10A B6A B9A 105.2(2) . . ? B12A B6A B9A 59.32(17) . . ? C10A B6A B2A 115.9(2) . . ? B12A B6A B2A 113.3(2) . . ? B9A B6A B2A 59.22(16) . . ? C10A B6A Fe4 65.43(13) . . ? B12A B6A Fe4 119.49(18) . . ? B9A B6A Fe4 114.72(17) . . ? B2A B6A Fe4 68.45(14) . . ? C10A B6A H6C 118.6(14) . . ? B12A B6A H6C 113.2(14) . . ? B9A B6A H6C 123.3(14) . . ? B2A B6A H6C 120.3(14) . . ? Fe4 B6A H6C 115.3(14) . . ? C10A B7A B8A 104.9(2) . . ? C10A B7A B13A 60.78(16) . . ? B8A B7A B13A 58.96(17) . . ? C10A B7A B3A 116.0(2) . . ? B8A B7A B3A 60.45(16) . . ? B13A B7A B3A 114.3(2) . . ? C10A B7A Fe4 65.54(13) . . ? B8A B7A Fe4 114.50(18) . . ? B13A B7A Fe4 119.55(18) . . ? B3A B7A Fe4 67.60(13) . . ? C10A B7A H7C 121.1(13) . . ? B8A B7A H7C 123.4(13) . . ? B13A B7A H7C 116.5(14) . . ? B3A B7A H7C 116.2(14) . . ? Fe4 B7A H7C 113.6(13) . . ? B13A B8A B11A 61.14(18) . . ? B13A B8A B7A 60.76(17) . . ? B11A B8A B7A 108.1(2) . . ? B13A B8A B3A 116.4(2) . . ? B11A B8A B3A 118.6(2) . . ? B7A B8A B3A 61.04(17) . . ? B13A B8A B5A 107.9(2) . . ? B11A B8A B5A 59.32(17) . . ? B7A B8A B5A 105.30(19) . . ? B3A B8A B5A 66.26(17) . . ? B13A B8A H8C 120.4(14) . . ? B11A B8A H8C 122.3(14) . . ? B7A B8A H8C 121.7(13) . . ? B3A B8A H8C 110.3(14) . . ? B5A B8A H8C 124.0(14) . . ? B12A B9A B11A 61.31(17) . . ? B12A B9A B6A 60.09(17) . . ? B11A B9A B6A 107.7(2) . . ? B12A B9A B2A 116.6(2) . . ? B11A B9A B2A 117.9(2) . . ? B6A B9A B2A 62.09(17) . . ? B12A B9A B5A 107.6(2) . . ? B11A B9A B5A 59.26(16) . . ? B6A B9A B5A 104.9(2) . . ? B2A B9A B5A 65.19(16) . . ? B12A B9A H9C 121.1(14) . . ? B11A B9A H9C 123.2(13) . . ? B6A B9A H9C 121.4(13) . . ? B2A B9A H9C 109.6(14) . . ? B5A B9A H9C 124.3(14) . . ? B6A C10A B7A 122.5(2) . . ? B6A C10A B12A 62.06(17) . . ? B7A C10A B12A 115.0(2) . . ? B6A C10A B13A 114.6(2) . . ? B7A C10A B13A 62.44(16) . . ? B12A C10A B13A 60.63(16) . . ? B6A C10A Fe4 69.95(13) . . ? B7A C10A Fe4 69.78(14) . . ? B12A C10A Fe4 124.55(17) . . ? B13A C10A Fe4 124.63(17) . . ? B6A C10A H10C 115.4(16) . . ? B7A C10A H10C 116.7(16) . . ? B12A C10A H10C 112.9(16) . . ? B13A C10A H10C 113.8(16) . . ? Fe4 C10A H10C 111.5(16) . . ? B9A B11A B8A 115.7(2) . . ? B9A B11A B13A 108.7(2) . . ? B8A B11A B13A 58.89(17) . . ? B9A B11A B12A 58.91(16) . . ? B8A B11A B12A 108.2(2) . . ? B13A B11A B12A 59.01(16) . . ? B9A B11A B5A 64.33(17) . . ? B8A B11A B5A 64.19(17) . . ? B13A B11A B5A 109.9(2) . . ? B12A B11A B5A 109.7(2) . . ? B9A B11A H11C 118.8(13) . . ? B8A B11A H11C 117.3(13) . . ? B13A B11A H11C 123.6(14) . . ? B12A B11A H11C 125.1(13) . . ? B5A B11A H11C 116.7(14) . . ? C10A B12A B9A 103.5(2) . . ? C10A B12A B13A 59.96(16) . . ? B9A B12A B13A 110.6(2) . . ? C10A B12A B6A 57.22(16) . . ? B9A B12A B6A 60.59(17) . . ? B13A B12A B6A 109.9(2) . . ? C10A B12A B11A 102.3(2) . . ? B9A B12A B11A 59.78(17) . . ? B13A B12A B11A 60.33(17) . . ? B6A B12A B11A 107.0(2) . . ? C10A B12A H12C 120.4(14) . . ? B9A B12A H12C 125.7(15) . . ? B13A B12A H12C 118.1(14) . . ? B6A B12A H12C 118.3(14) . . ? B11A B12A H12C 129.3(14) . . ? B8A B13A C10A 102.9(2) . . ? B8A B13A B12A 110.5(2) . . ? C10A B13A B12A 59.41(16) . . ? B8A B13A B7A 60.29(17) . . ? C10A B13A B7A 56.78(15) . . ? B12A B13A B7A 109.1(2) . . ? B8A B13A B11A 59.98(17) . . ? C10A B13A B11A 102.1(2) . . ? B12A B13A B11A 60.66(17) . . ? B7A B13A B11A 106.9(2) . . ? B8A B13A H13C 126.7(13) . . ? C10A B13A H13C 120.8(13) . . ? B12A B13A H13C 117.3(13) . . ? B7A B13A H13C 119.6(13) . . ? B11A B13A H13C 128.5(13) . . ? B2B C1B B3B 126.9(2) . . ? B2B C1B B5B 75.13(19) . . ? B3B C1B B5B 73.52(19) . . ? B2B C1B Fe4 78.10(15) . . ? B3B C1B Fe4 76.91(15) . . ? B5B C1B Fe4 113.83(17) . . ? B2B C1B H1D 118.7(16) . . ? B3B C1B H1D 113.8(16) . . ? B5B C1B H1D 119.4(16) . . ? Fe4 C1B H1D 126.6(16) . . ? C1B B2B B9B 114.8(2) . . ? C1B B2B B6B 116.3(2) . . ? B9B B2B B6B 58.22(17) . . ? C1B B2B B5B 57.34(16) . . ? B9B B2B B5B 59.95(16) . . ? B6B B2B B5B 98.7(2) . . ? C1B B2B Fe4 61.12(14) . . ? B9B B2B Fe4 110.61(18) . . ? B6B B2B Fe4 64.92(14) . . ? B5B B2B Fe4 95.48(16) . . ? C1B B2B H2D 117.5(12) . . ? B9B B2B H2D 113.1(12) . . ? B6B B2B H2D 122.1(12) . . ? B5B B2B H2D 127.5(12) . . ? Fe4 B2B H2D 129.7(12) . . ? C1B B3B B8B 116.3(2) . . ? C1B B3B B7B 117.3(2) . . ? B8B B3B B7B 58.66(16) . . ? C1B B3B B5B 58.11(17) . . ? B8B B3B B5B 60.79(16) . . ? B7B B3B B5B 100.12(19) . . ? C1B B3B Fe4 61.77(13) . . ? B8B B3B Fe4 111.77(17) . . ? B7B B3B Fe4 65.02(13) . . ? B5B B3B Fe4 97.19(15) . . ? C1B B3B H3D 118.6(13) . . ? B8B B3B H3D 113.1(13) . . ? B7B B3B H3D 118.4(13) . . ? B5B B3B H3D 130.3(13) . . ? Fe4 B3B H3D 126.1(12) . . ? C1B B5B B11B 134.0(2) . . ? C1B B5B B8B 100.93(19) . . ? B11B B5B B8B 56.47(16) . . ? C1B B5B B9B 100.22(19) . . ? B11B B5B B9B 56.00(16) . . ? B8B B5B B9B 102.95(19) . . ? C1B B5B B3B 48.37(15) . . ? B11B B5B B3B 105.6(2) . . ? B8B B5B B3B 54.46(15) . . ? B9B B5B B3B 119.77(19) . . ? C1B B5B B2B 47.53(15) . . ? B11B B5B B2B 105.5(2) . . ? B8B B5B B2B 120.12(19) . . ? B9B B5B B2B 54.60(15) . . ? B3B B5B B2B 87.25(17) . . ? C1B B5B H5D 113.3(14) . . ? B11B B5B H5D 112.7(14) . . ? B8B B5B H5D 118.0(14) . . ? B9B B5B H5D 118.6(14) . . ? B3B B5B H5D 121.1(14) . . ? B2B B5B H5D 121.2(14) . . ? C10B B6B B9B 105.1(2) . . ? C10B B6B B12B 60.47(17) . . ? B9B B6B B12B 59.35(17) . . ? C10B B6B B2B 116.0(2) . . ? B9B B6B B2B 60.47(17) . . ? B12B B6B B2B 114.5(2) . . ? C10B B6B Fe4 64.94(14) . . ? B9B B6B Fe4 114.70(18) . . ? B12B B6B Fe4 118.81(19) . . ? B2B B6B Fe4 67.97(14) . . ? C10B B6B H6D 122.4(13) . . ? B9B B6B H6D 121.3(14) . . ? B12B B6B H6D 115.6(13) . . ? B2B B6B H6D 115.9(13) . . ? Fe4 B6B H6D 115.6(13) . . ? C10B B7B B13B 60.64(17) . . ? C10B B7B B8B 104.9(2) . . ? B13B B7B B8B 59.15(16) . . ? C10B B7B B3B 114.7(2) . . ? B13B B7B B3B 113.1(2) . . ? B8B B7B B3B 59.63(16) . . ? C10B B7B Fe4 65.27(13) . . ? B13B B7B Fe4 119.19(18) . . ? B8B B7B Fe4 114.46(18) . . ? B3B B7B Fe4 67.45(13) . . ? C10B B7B H7D 124.0(13) . . ? B13B B7B H7D 119.2(13) . . ? B8B B7B H7D 122.3(13) . . ? B3B B7B H7D 114.4(13) . . ? Fe4 B7B H7D 112.8(13) . . ? B13B B8B B7B 60.39(17) . . ? B13B B8B B11B 61.14(17) . . ? B7B B8B B11B 107.9(2) . . ? B13B B8B B3B 116.1(2) . . ? B7B B8B B3B 61.71(16) . . ? B11B B8B B3B 117.1(2) . . ? B13B B8B B5B 107.3(2) . . ? B7B B8B B5B 104.9(2) . . ? B11B B8B B5B 59.11(17) . . ? B3B B8B B5B 64.75(17) . . ? B13B B8B H8D 118.8(13) . . ? B7B B8B H8D 121.6(13) . . ? B11B B8B H8D 121.5(13) . . ? B3B B8B H8D 113.0(13) . . ? B5B B8B H8D 125.7(13) . . ? B12B B9B B11B 61.32(18) . . ? B12B B9B B6B 60.33(18) . . ? B11B B9B B6B 107.9(2) . . ? B12B B9B B2B 116.1(2) . . ? B11B B9B B2B 118.0(2) . . ? B6B B9B B2B 61.31(17) . . ? B12B B9B B5B 107.3(2) . . ? B11B B9B B5B 59.18(17) . . ? B6B B9B B5B 104.5(2) . . ? B2B B9B B5B 65.45(17) . . ? B12B B9B H9D 121.9(14) . . ? B11B B9B H9D 120.8(14) . . ? B6B B9B H9D 124.2(14) . . ? B2B B9B H9D 110.8(14) . . ? B5B B9B H9D 122.4(14) . . ? B6B C10B B7B 123.2(2) . . ? B6B C10B B12B 62.30(18) . . ? B7B C10B B12B 114.9(2) . . ? B6B C10B B13B 114.7(2) . . ? B7B C10B B13B 62.14(17) . . ? B12B C10B B13B 60.46(17) . . ? B6B C10B Fe4 70.50(14) . . ? B7B C10B Fe4 69.94(14) . . ? B12B C10B Fe4 125.19(17) . . ? B13B C10B Fe4 124.51(17) . . ? B6B C10B H10D 115.8(16) . . ? B7B C10B H10D 115.8(17) . . ? B12B C10B H10D 113.1(17) . . ? B13B C10B H10D 113.4(16) . . ? Fe4 C10B H10D 111.4(16) . . ? B9B B11B B8B 116.5(2) . . ? B9B B11B B13B 108.6(2) . . ? B8B B11B B13B 58.71(17) . . ? B9B B11B B12B 59.06(17) . . ? B8B B11B B12B 108.2(2) . . ? B13B B11B B12B 58.61(17) . . ? B9B B11B B5B 64.81(18) . . ? B8B B11B B5B 64.42(17) . . ? B13B B11B B5B 109.6(2) . . ? B12B B11B B5B 109.9(2) . . ? B9B B11B H11D 119.1(14) . . ? B8B B11B H11D 117.2(14) . . ? B13B B11B H11D 122.7(14) . . ? B12B B11B H11D 123.9(14) . . ? B5B B11B H11D 118.1(13) . . ? C10B B12B B9B 103.4(2) . . ? C10B B12B B13B 59.93(17) . . ? B9B B12B B13B 110.7(2) . . ? C10B B12B B6B 57.23(16) . . ? B9B B12B B6B 60.32(18) . . ? B13B B12B B6B 109.9(2) . . ? C10B B12B B11B 102.3(2) . . ? B9B B12B B11B 59.62(17) . . ? B13B B12B B11B 60.66(17) . . ? B6B B12B B11B 106.6(2) . . ? C10B B12B H12D 124.0(14) . . ? B9B B12B H12D 122.1(14) . . ? B13B B12B H12D 120.6(14) . . ? B6B B12B H12D 118.4(13) . . ? B11B B12B H12D 127.4(13) . . ? C10B B13B B8B 103.3(2) . . ? C10B B13B B12B 59.62(17) . . ? B8B B13B B12B 111.2(2) . . ? C10B B13B B7B 57.22(16) . . ? B8B B13B B7B 60.47(17) . . ? B12B B13B B7B 109.9(2) . . ? C10B B13B B11B 102.1(2) . . ? B8B B13B B11B 60.15(17) . . ? B12B B13B B11B 60.73(17) . . ? B7B B13B B11B 107.2(2) . . ? C10B B13B H13D 120.1(14) . . ? B8B B13B H13D 124.8(14) . . ? B12B B13B H13D 119.3(14) . . ? B7B B13B H13D 116.3(14) . . ? B11B B13B H13D 130.7(14) . . ? C2 C1 C6 118.8(2) . . ? C2 C1 C7 121.8(2) . . ? C6 C1 C7 119.4(2) . . ? C1 C2 C3 120.8(2) . . ? C1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 120.2(3) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 C1 120.5(3) . . ? C5 C6 H6A 119.7 . . ? C1 C6 H6A 119.7 . . ? C1 C7 N1 115.8(2) . . ? C1 C7 H7A 108.3 . . ? N1 C7 H7A 108.3 . . ? C1 C7 H7B 108.3 . . ? N1 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8E 109.5 . . ? H8A C8 H8E 109.5 . . ? H8B C8 H8E 109.5 . . ? C10 N1 C9 109.61(17) . . ? C10 N1 C8 108.2 . . ? C9 N1 C8 108.17(12) . . ? C10 N1 C7 107.78(16) . . ? C9 N1 C7 111.13(18) . . ? C8 N1 C7 111.93(12) . . ? N1 C10 H10F 109.5 . . ? N1 C10 H10G 109.4 . . ? H10F C10 H10G 109.5 . . ? N1 C10 H10H 109.5 . . ? H10F C10 H10H 109.5 . . ? H10G C10 H10H 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9E 109.5 . . ? H9A C9 H9E 109.5 . . ? H9B C9 H9E 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.502 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.102