# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jonas C. Peters' _publ_contact_author_address ;Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, California 91125 USA ; _publ_contact_author_email jpeters@caltech.edu _publ_contact_author_phone 1(626)3954036 _publ_contact_author_fax 1(626)5774088 loop_ _publ_author_name _publ_author_address M.T.Whited ;Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, California 91125 USA ; E.Rivard ;Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, California 91125 USA ; J.C.Peters ;Division of Chemistry and Chemical Engineering California Institute of Technology Pasadena, California 91125 USA ; #===END data_ear13 _database_code_depnum_ccdc_archive 'CCDC 289249' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H64 Co I N P3 Si' _chemical_formula_weight 1141.98 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.0701(10) _cell_length_b 19.1387(15) _cell_length_c 22.1493(16) _cell_angle_alpha 90.00 _cell_angle_beta 102.943(3) _cell_angle_gamma 90.00 _cell_volume 5399.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4214 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 23.93 _exptl_crystal_description blade _exptl_crystal_colour dark _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.042 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44992 _diffrn_reflns_av_R_equivalents 0.1666 _diffrn_reflns_av_sigmaI/netI 0.1807 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.06 _reflns_number_total 10823 _reflns_number_gt 5545 _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^)+(0.0000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10823 _refine_ls_number_parameters 637 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1635 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.1243 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.254 _refine_ls_restrained_S_all 1.253 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I I 0.25753(4) 0.80204(3) 0.15122(2) 0.01676(14) Uani 1 1 d . . . Co Co 0.23094(7) 0.69178(5) 0.21778(4) 0.0135(2) Uani 1 1 d . . . N N 0.1238(4) 0.6381(3) 0.1576(3) 0.0160(15) Uani 1 1 d . . . P1 P 0.22709(15) 0.60833(10) 0.28149(9) 0.0144(5) Uani 1 1 d . . . P3 P 0.20957(15) 0.76461(10) 0.29378(9) 0.0137(5) Uani 1 1 d . . . P2 P 0.40427(15) 0.66840(9) 0.23267(9) 0.0134(5) Uani 1 1 d . . . Si Si 0.02992(16) 0.59652(11) 0.18939(9) 0.0168(5) Uani 1 1 d . . . C1 C 0.1141(5) 0.6337(4) 0.0939(3) 0.0153(18) Uani 1 1 d . . . C2 C 0.1734(6) 0.5823(4) 0.0692(3) 0.0201(19) Uani 1 1 d . . . C3 C 0.1574(6) 0.5759(4) 0.0040(4) 0.0217(19) Uani 1 1 d . . . H3 H 0.1961 0.5418 -0.0127 0.026 Uiso 1 1 calc R . . C4 C 0.0863(6) 0.6185(4) -0.0366(4) 0.026(2) Uani 1 1 d . . . H4 H 0.0751 0.6132 -0.0802 0.031 Uiso 1 1 calc R . . C5 C 0.0338(6) 0.6676(4) -0.0111(4) 0.025(2) Uani 1 1 d . . . H5 H -0.0137 0.6971 -0.0385 0.030 Uiso 1 1 calc R . . C6 C 0.0445(6) 0.6778(4) 0.0516(4) 0.026(2) Uani 1 1 d . . . C7 C 0.2448(6) 0.5319(4) 0.1089(3) 0.0219(19) Uani 1 1 d . . . H7 H 0.2772 0.5570 0.1481 0.026 Uiso 1 1 calc R . . C8 C 0.1873(7) 0.4677(4) 0.1274(4) 0.038(2) Uani 1 1 d . . . H8A H 0.1351 0.4831 0.1501 0.057 Uiso 1 1 calc R . . H8B H 0.2382 0.4368 0.1537 0.057 Uiso 1 1 calc R . . H8C H 0.1521 0.4425 0.0900 0.057 Uiso 1 1 calc R . . C9 C 0.3342(6) 0.5034(4) 0.0829(4) 0.028(2) Uani 1 1 d . . . H9A H 0.3063 0.4712 0.0488 0.042 Uiso 1 1 calc R . . H9B H 0.3839 0.4785 0.1155 0.042 Uiso 1 1 calc R . . H9C H 0.3703 0.5421 0.0675 0.042 Uiso 1 1 calc R . . C10 C -0.0217(6) 0.7319(4) 0.0735(4) 0.0208(19) Uani 1 1 d . . . H10 H 0.0032 0.7367 0.1194 0.025 Uiso 1 1 calc R . . C11 C -0.0147(6) 0.8035(4) 0.0442(4) 0.032(2) Uani 1 1 d . . . H11A H 0.0592 0.8160 0.0481 0.049 Uiso 1 1 calc R . . H11B H -0.0486 0.8385 0.0654 0.049 Uiso 1 1 calc R . . H11C H -0.0502 0.8019 0.0003 0.049 Uiso 1 1 calc R . . C12 C -0.1375(6) 0.7087(4) 0.0595(4) 0.030(2) Uani 1 1 d . . . H12A H -0.1658 0.7088 0.0147 0.045 Uiso 1 1 calc R . . H12B H -0.1780 0.7410 0.0794 0.045 Uiso 1 1 calc R . . H12C H -0.1423 0.6614 0.0757 0.045 Uiso 1 1 calc R . . C13 C -0.0678(6) 0.6512(4) 0.2176(4) 0.026(2) Uani 1 1 d . . . H13A H -0.0333 0.6747 0.2560 0.038 Uiso 1 1 calc R . . H13B H -0.1245 0.6214 0.2253 0.038 Uiso 1 1 calc R . . H13C H -0.0969 0.6863 0.1861 0.038 Uiso 1 1 calc R . . C14 C -0.0516(6) 0.5326(4) 0.1355(4) 0.025(2) Uani 1 1 d . . . H14A H -0.0259 0.5297 0.0973 0.037 Uiso 1 1 calc R . . H14B H -0.1249 0.5480 0.1257 0.037 Uiso 1 1 calc R . . H14C H -0.0467 0.4865 0.1553 0.037 Uiso 1 1 calc R . . C15 C 0.1116(5) 0.5539(4) 0.2617(3) 0.0158(18) Uani 1 1 d . . . H15 H 0.0954 0.5134 0.2826 0.019 Uiso 1 1 calc R . . C16 C 0.2344(6) 0.6416(4) 0.3598(3) 0.0153(18) Uani 1 1 d U . . C17 C 0.2431(6) 0.5970(4) 0.4117(3) 0.0196(19) Uani 1 1 d . . . H17 H 0.2448 0.5477 0.4072 0.023 Uiso 1 1 calc R . . C18 C 0.2492(6) 0.6275(4) 0.4697(3) 0.0205(19) Uani 1 1 d . . . H18 H 0.2597 0.5990 0.5056 0.025 Uiso 1 1 calc R . . C19 C 0.2396(7) 0.7007(5) 0.4751(4) 0.036(2) Uani 1 1 d . . . H19 H 0.2394 0.7208 0.5143 0.044 Uiso 1 1 calc R . . C20 C 0.2307(5) 0.7432(4) 0.4238(4) 0.0190(19) Uani 1 1 d . . . H20 H 0.2258 0.7924 0.4279 0.023 Uiso 1 1 calc R . . C21 C 0.2288(5) 0.7133(3) 0.3655(3) 0.0109(17) Uani 1 1 d U . . C22 C 0.3406(5) 0.5530(4) 0.2870(3) 0.0148(17) Uani 1 1 d . . . C23 C 0.3487(6) 0.4851(4) 0.3117(3) 0.0174(18) Uani 1 1 d . . . H23 H 0.2936 0.4672 0.3289 0.021 Uiso 1 1 calc R . . C24 C 0.4345(6) 0.4443(4) 0.3114(3) 0.023(2) Uani 1 1 d . . . H24 H 0.4406 0.3994 0.3303 0.027 Uiso 1 1 calc R . . C25 C 0.5136(6) 0.4690(4) 0.2831(4) 0.022(2) Uani 1 1 d . . . H25 H 0.5711 0.4398 0.2803 0.026 Uiso 1 1 calc R . . C26 C 0.5071(6) 0.5352(4) 0.2598(3) 0.0195(19) Uani 1 1 d . . . H26 H 0.5622 0.5522 0.2422 0.023 Uiso 1 1 calc R . . C27 C 0.4235(5) 0.5782(3) 0.2609(3) 0.0145(17) Uani 1 1 d . . . C28 C 0.2812(6) 0.8453(4) 0.3212(3) 0.0148(18) Uani 1 1 d . . . C29 C 0.3719(6) 0.8444(4) 0.3669(3) 0.0209(19) Uani 1 1 d . . . H29 H 0.4004 0.8006 0.3825 0.025 Uiso 1 1 calc R . . C30 C 0.4232(6) 0.9049(4) 0.3909(3) 0.0213(19) Uani 1 1 d . . . H30 H 0.4854 0.9024 0.4227 0.026 Uiso 1 1 calc R . . C31 C 0.3836(6) 0.9688(4) 0.3683(4) 0.023(2) Uani 1 1 d . . . H31 H 0.4171 1.0107 0.3854 0.027 Uiso 1 1 calc R . . C32 C 0.2938(6) 0.9718(4) 0.3201(4) 0.027(2) Uani 1 1 d . . . H32 H 0.2683 1.0156 0.3029 0.032 Uiso 1 1 calc R . . C33 C 0.2418(6) 0.9101(4) 0.2975(3) 0.0188(18) Uani 1 1 d . . . H33 H 0.1794 0.9121 0.2658 0.023 Uiso 1 1 calc R . . C34 C 0.0736(5) 0.7954(4) 0.2810(3) 0.0133(16) Uani 1 1 d . . . C35 C 0.0120(6) 0.7897(3) 0.3251(3) 0.0162(18) Uani 1 1 d . . . H35 H 0.0419 0.7693 0.3642 0.019 Uiso 1 1 calc R . . C36 C -0.0897(5) 0.8125(4) 0.3136(3) 0.0187(18) Uani 1 1 d . . . H36 H -0.1288 0.8078 0.3448 0.022 Uiso 1 1 calc R . . C37 C -0.1365(6) 0.8423(4) 0.2571(4) 0.0210(19) Uani 1 1 d . . . H37 H -0.2076 0.8572 0.2488 0.025 Uiso 1 1 calc R . . C38 C -0.0770(6) 0.8498(4) 0.2131(4) 0.024(2) Uani 1 1 d . . . H38 H -0.1071 0.8714 0.1746 0.028 Uiso 1 1 calc R . . C39 C 0.0263(6) 0.8261(3) 0.2245(3) 0.0185(18) Uani 1 1 d . . . H39 H 0.0652 0.8309 0.1933 0.022 Uiso 1 1 calc R . . C40 C 0.4974(5) 0.7172(3) 0.2911(3) 0.0142(18) Uani 1 1 d . . . C41 C 0.5290(6) 0.7825(3) 0.2772(4) 0.0200(19) Uani 1 1 d . . . H41 H 0.5017 0.8016 0.2373 0.024 Uiso 1 1 calc R . . C42 C 0.6005(6) 0.8212(4) 0.3206(4) 0.027(2) Uani 1 1 d . . . H42 H 0.6211 0.8664 0.3102 0.033 Uiso 1 1 calc R . . C43 C 0.6413(5) 0.7941(4) 0.3783(4) 0.0241(19) Uani 1 1 d . . . H43 H 0.6900 0.8207 0.4077 0.029 Uiso 1 1 calc R . . C44 C 0.6122(6) 0.7282(4) 0.3941(4) 0.027(2) Uani 1 1 d . . . H44 H 0.6406 0.7093 0.4340 0.033 Uiso 1 1 calc R . . C45 C 0.5403(5) 0.6903(4) 0.3503(3) 0.0192(18) Uani 1 1 d . . . H45 H 0.5197 0.6450 0.3608 0.023 Uiso 1 1 calc R . . C46 C 0.4716(5) 0.6699(3) 0.1686(3) 0.0101(16) Uani 1 1 d U . . C47 C 0.5799(6) 0.6706(4) 0.1788(3) 0.0193(19) Uani 1 1 d . . . H47 H 0.6209 0.6705 0.2201 0.023 Uiso 1 1 calc R . . C48 C 0.6300(6) 0.6715(4) 0.1292(4) 0.029(2) Uani 1 1 d . . . H48 H 0.7044 0.6722 0.1367 0.034 Uiso 1 1 calc R . . C49 C 0.5698(6) 0.6713(4) 0.0685(4) 0.026(2) Uani 1 1 d . . . H49 H 0.6031 0.6714 0.0345 0.031 Uiso 1 1 calc R . . C50 C 0.4619(6) 0.6709(4) 0.0582(4) 0.025(2) Uani 1 1 d . . . H50 H 0.4205 0.6713 0.0171 0.030 Uiso 1 1 calc R . . C51 C 0.4144(6) 0.6699(3) 0.1073(3) 0.0151(17) Uani 1 1 d . . . H51 H 0.3399 0.6691 0.0994 0.018 Uiso 1 1 calc R . . C52 C 0.6372(8) 0.6395(5) 0.5577(4) 0.042(3) Uani 1 1 d . . . H52 H 0.6441 0.6718 0.5909 0.051 Uiso 1 1 calc R . . C53 C 0.7274(7) 0.6101(5) 0.5450(4) 0.044(3) Uani 1 1 d . . . H53 H 0.7944 0.6208 0.5703 0.053 Uiso 1 1 calc R . . C54 C 0.7187(7) 0.5646(4) 0.4947(4) 0.037(2) Uani 1 1 d . . . H54 H 0.7793 0.5456 0.4839 0.044 Uiso 1 1 calc R . . C55 C 0.6203(7) 0.5483(4) 0.4616(4) 0.036(2) Uani 1 1 d . . . H55 H 0.6131 0.5164 0.4280 0.044 Uiso 1 1 calc R . . C56 C 0.5300(7) 0.5769(5) 0.4754(5) 0.046(3) Uani 1 1 d . . . H56 H 0.4625 0.5647 0.4516 0.055 Uiso 1 1 calc R . . C57 C 0.5404(8) 0.6237(5) 0.5245(5) 0.052(3) Uani 1 1 d . . . H57 H 0.4801 0.6442 0.5345 0.062 Uiso 1 1 calc R . . C58 C 0.1317(7) 0.1242(4) 0.1300(4) 0.033(2) Uani 1 1 d . . . H58 H 0.1429 0.1729 0.1365 0.039 Uiso 1 1 calc R . . C59 C 0.2127(7) 0.0783(5) 0.1523(4) 0.037(2) Uani 1 1 d . . . H59 H 0.2802 0.0952 0.1722 0.044 Uiso 1 1 calc R . . C60 C 0.1947(7) 0.0083(5) 0.1454(4) 0.039(2) Uani 1 1 d . . . H60 H 0.2487 -0.0240 0.1625 0.047 Uiso 1 1 calc R . . C61 C 0.0987(7) -0.0158(5) 0.1137(5) 0.044(3) Uani 1 1 d . . . H61 H 0.0869 -0.0646 0.1077 0.052 Uiso 1 1 calc R . . C62 C 0.0196(7) 0.0309(5) 0.0905(4) 0.040(2) Uani 1 1 d . . . H62 H -0.0471 0.0147 0.0686 0.048 Uiso 1 1 calc R . . C63 C 0.0381(7) 0.1015(5) 0.0996(4) 0.035(2) Uani 1 1 d . . . H63 H -0.0162 0.1341 0.0839 0.042 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 I 0.0247(3) 0.0179(3) 0.0088(3) 0.0027(3) 0.0063(2) 0.0021(3) Co 0.0191(6) 0.0159(6) 0.0062(5) 0.0002(5) 0.0041(4) -0.0006(5) N 0.011(3) 0.027(4) 0.010(4) -0.007(3) 0.003(3) -0.004(3) P1 0.0167(11) 0.0181(12) 0.0086(11) 0.0000(9) 0.0031(9) -0.0017(9) P3 0.0163(11) 0.0154(11) 0.0098(11) 0.0013(8) 0.0035(9) 0.0004(9) P2 0.0173(11) 0.0152(11) 0.0082(11) -0.0004(8) 0.0039(9) -0.0024(9) Si 0.0179(12) 0.0220(13) 0.0105(12) -0.0029(9) 0.0033(10) -0.0040(10) C1 0.004(4) 0.028(5) 0.012(4) 0.007(4) -0.003(3) 0.001(3) C2 0.023(5) 0.020(5) 0.019(5) 0.005(4) 0.009(4) -0.001(4) C3 0.022(5) 0.020(5) 0.023(5) -0.011(4) 0.005(4) -0.003(4) C4 0.040(6) 0.034(5) 0.005(4) -0.003(4) 0.008(4) -0.003(4) C5 0.028(5) 0.030(5) 0.016(5) 0.004(4) 0.001(4) -0.014(4) C6 0.024(5) 0.033(6) 0.021(5) 0.003(4) 0.004(4) -0.002(4) C7 0.024(5) 0.027(5) 0.013(5) -0.008(4) 0.001(4) 0.001(4) C8 0.043(6) 0.041(6) 0.031(6) 0.011(4) 0.009(5) 0.014(5) C9 0.021(5) 0.028(5) 0.036(6) 0.003(4) 0.009(4) 0.002(4) C10 0.029(5) 0.015(4) 0.020(5) 0.002(3) 0.008(4) -0.002(4) C11 0.036(5) 0.027(5) 0.033(5) 0.005(5) 0.006(4) 0.012(5) C12 0.029(5) 0.037(6) 0.027(5) -0.002(4) 0.010(4) 0.005(4) C13 0.024(5) 0.028(5) 0.029(5) 0.000(4) 0.015(4) -0.008(4) C14 0.017(5) 0.031(5) 0.027(5) 0.002(4) 0.005(4) -0.005(4) C15 0.005(4) 0.022(4) 0.017(4) 0.006(3) -0.005(3) -0.006(3) C16 0.016(3) 0.023(3) 0.008(3) 0.007(3) 0.005(3) 0.000(3) C17 0.024(5) 0.016(4) 0.018(5) 0.000(4) 0.005(4) 0.001(4) C18 0.038(5) 0.018(5) 0.008(4) 0.004(3) 0.008(4) 0.001(4) C19 0.057(6) 0.042(6) 0.014(5) -0.003(5) 0.016(4) -0.011(5) C20 0.013(4) 0.023(5) 0.024(5) -0.004(4) 0.011(4) -0.008(4) C21 0.014(4) 0.016(4) 0.005(4) 0.004(3) 0.007(3) -0.001(3) C22 0.010(4) 0.022(5) 0.011(4) -0.008(3) 0.001(3) -0.002(3) C23 0.020(5) 0.019(5) 0.013(4) -0.006(3) 0.004(4) -0.004(4) C24 0.043(6) 0.018(5) 0.006(4) 0.000(3) 0.004(4) -0.003(4) C25 0.018(5) 0.011(5) 0.039(6) -0.006(4) 0.013(4) 0.005(4) C26 0.015(4) 0.032(5) 0.011(5) -0.002(4) 0.001(4) 0.002(4) C27 0.015(4) 0.009(4) 0.019(5) -0.001(3) 0.002(4) 0.004(3) C28 0.017(4) 0.013(4) 0.012(4) -0.001(3) -0.001(4) -0.003(3) C29 0.035(5) 0.017(4) 0.012(4) 0.001(3) 0.008(4) -0.009(4) C30 0.020(5) 0.030(5) 0.011(4) -0.001(4) -0.003(4) -0.013(4) C31 0.039(6) 0.009(4) 0.023(5) -0.006(4) 0.011(4) -0.011(4) C32 0.027(5) 0.019(5) 0.038(6) 0.011(4) 0.015(5) 0.004(4) C33 0.014(4) 0.025(5) 0.016(5) -0.005(4) 0.003(4) -0.004(4) C34 0.014(4) 0.013(4) 0.009(4) -0.002(3) -0.005(3) -0.007(3) C35 0.031(5) 0.014(4) 0.003(4) -0.002(3) 0.003(3) -0.002(4) C36 0.016(4) 0.028(5) 0.013(4) -0.001(4) 0.008(3) 0.001(4) C37 0.018(5) 0.020(5) 0.027(5) -0.005(4) 0.009(4) 0.005(4) C38 0.018(5) 0.040(5) 0.010(5) 0.007(4) -0.002(4) 0.005(4) C39 0.019(4) 0.026(5) 0.010(4) -0.004(3) 0.001(3) -0.004(4) C40 0.012(4) 0.016(5) 0.012(4) 0.008(3) -0.003(3) 0.003(3) C41 0.026(5) 0.014(5) 0.020(5) 0.005(3) 0.006(4) -0.005(3) C42 0.035(5) 0.020(5) 0.024(5) 0.003(4) 0.002(4) 0.000(4) C43 0.004(4) 0.027(5) 0.037(5) -0.009(4) -0.004(4) -0.008(4) C44 0.033(5) 0.035(5) 0.009(5) 0.005(4) -0.007(4) -0.003(4) C45 0.015(4) 0.019(4) 0.021(5) -0.003(4) -0.003(3) 0.001(4) C46 0.016(4) 0.013(4) 0.003(4) 0.002(3) 0.005(3) -0.003(3) C47 0.022(5) 0.028(5) 0.006(4) 0.009(3) -0.002(4) 0.001(4) C48 0.014(5) 0.038(6) 0.034(6) 0.000(4) 0.008(4) 0.000(4) C49 0.032(5) 0.036(5) 0.015(5) 0.003(4) 0.015(4) -0.005(4) C50 0.030(5) 0.029(5) 0.013(5) 0.001(4) -0.003(4) 0.000(4) C51 0.021(4) 0.013(4) 0.013(4) -0.006(3) 0.008(4) -0.002(3) C52 0.067(8) 0.040(6) 0.026(6) -0.002(4) 0.025(6) -0.023(6) C53 0.043(7) 0.051(7) 0.029(6) 0.018(5) -0.008(5) -0.023(5) C54 0.033(6) 0.045(6) 0.031(6) 0.028(5) 0.003(5) 0.005(5) C55 0.045(6) 0.039(6) 0.023(5) 0.013(4) 0.001(5) -0.005(5) C56 0.022(6) 0.065(8) 0.043(7) 0.028(6) -0.012(5) -0.013(5) C57 0.051(7) 0.056(7) 0.054(8) 0.029(6) 0.023(6) -0.003(6) C58 0.048(6) 0.018(5) 0.034(6) 0.000(4) 0.014(5) -0.004(5) C59 0.029(5) 0.062(7) 0.017(5) 0.003(5) 0.000(4) -0.001(5) C60 0.020(5) 0.054(7) 0.040(6) 0.012(5) -0.002(5) 0.007(5) C61 0.031(6) 0.030(6) 0.072(8) 0.006(5) 0.017(6) -0.009(5) C62 0.026(6) 0.050(7) 0.043(7) -0.004(5) 0.004(5) -0.010(5) C63 0.034(6) 0.036(6) 0.035(6) 0.005(5) 0.009(5) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I Co 2.6415(10) . ? Co N 1.990(6) . ? Co P1 2.139(2) . ? Co P3 2.250(2) . ? Co P2 2.260(2) . ? N C1 1.391(8) . ? N Si 1.739(6) . ? P1 C22 1.804(7) . ? P1 C15 1.806(7) . ? P1 C16 1.830(7) . ? P3 C34 1.833(7) . ? P3 C21 1.836(7) . ? P3 C28 1.837(7) . ? P2 C40 1.823(7) . ? P2 C46 1.830(7) . ? P2 C27 1.834(7) . ? Si C13 1.863(7) . ? Si C14 1.867(7) . ? Si C15 1.899(7) . ? C1 C6 1.426(10) . ? C1 C2 1.433(10) . ? C2 C3 1.418(10) . ? C2 C7 1.486(10) . ? C3 C4 1.401(10) . ? C3 H3 0.9500 . ? C4 C5 1.360(10) . ? C4 H4 0.9500 . ? C5 C6 1.379(10) . ? C5 H5 0.9500 . ? C6 C10 1.498(10) . ? C7 C9 1.516(10) . ? C7 C8 1.541(10) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.528(10) . ? C10 C12 1.540(9) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15 0.9500 . ? C16 C21 1.380(9) . ? C16 C17 1.417(9) . ? C17 C18 1.396(10) . ? C17 H17 0.9500 . ? C18 C19 1.413(10) . ? C18 H18 0.9500 . ? C19 C20 1.380(10) . ? C19 H19 0.9500 . ? C20 C21 1.409(10) . ? C20 H20 0.9500 . ? C22 C23 1.405(9) . ? C22 C27 1.423(9) . ? C23 C24 1.367(10) . ? C23 H23 0.9500 . ? C24 C25 1.406(10) . ? C24 H24 0.9500 . ? C25 C26 1.364(9) . ? C25 H25 0.9500 . ? C26 C27 1.371(9) . ? C26 H26 0.9500 . ? C28 C29 1.375(9) . ? C28 C33 1.400(9) . ? C29 C30 1.383(9) . ? C29 H29 0.9500 . ? C30 C31 1.379(10) . ? C30 H30 0.9500 . ? C31 C32 1.399(10) . ? C31 H31 0.9500 . ? C32 C33 1.399(10) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.396(9) . ? C34 C35 1.403(9) . ? C35 C36 1.368(9) . ? C35 H35 0.9500 . ? C36 C37 1.387(9) . ? C36 H36 0.9500 . ? C37 C38 1.384(10) . ? C37 H37 0.9500 . ? C38 C39 1.393(9) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.372(9) . ? C40 C45 1.404(9) . ? C41 C42 1.395(10) . ? C41 H41 0.9500 . ? C42 C43 1.371(10) . ? C42 H42 0.9500 . ? C43 C44 1.384(10) . ? C43 H43 0.9500 . ? C44 C45 1.394(9) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.383(9) . ? C46 C51 1.395(9) . ? C47 C48 1.400(11) . ? C47 H47 0.9500 . ? C48 C49 1.397(10) . ? C48 H48 0.9500 . ? C49 C50 1.377(10) . ? C49 H49 0.9500 . ? C50 C51 1.368(10) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C57 1.347(12) . ? C52 C53 1.391(12) . ? C52 H52 0.9500 . ? C53 C54 1.399(12) . ? C53 H53 0.9500 . ? C54 C55 1.365(11) . ? C54 H54 0.9500 . ? C55 C56 1.396(12) . ? C55 H55 0.9500 . ? C56 C57 1.392(13) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C63 1.330(11) . ? C58 C59 1.380(11) . ? C58 H58 0.9500 . ? C59 C60 1.363(11) . ? C59 H59 0.9500 . ? C60 C61 1.373(11) . ? C60 H60 0.9500 . ? C61 C62 1.376(11) . ? C61 H61 0.9500 . ? C62 C63 1.380(11) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? 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 N Co P1 86.54(18) . . ? N Co P3 129.39(17) . . ? P1 Co P3 86.78(8) . . ? N Co P2 121.84(17) . . ? P1 Co P2 85.81(8) . . ? P3 Co P2 107.57(8) . . ? N Co I 101.49(17) . . ? P1 Co I 171.93(7) . . ? P3 Co I 88.66(6) . . ? P2 Co I 89.24(6) . . ? C1 N Si 118.1(5) . . ? C1 N Co 127.0(5) . . ? Si N Co 114.8(3) . . ? C22 P1 C15 107.9(3) . . ? C22 P1 C16 105.8(3) . . ? C15 P1 C16 107.1(3) . . ? C22 P1 Co 110.0(3) . . ? C15 P1 Co 114.4(2) . . ? C16 P1 Co 111.2(2) . . ? C34 P3 C21 104.2(3) . . ? C34 P3 C28 100.7(3) . . ? C21 P3 C28 101.7(3) . . ? C34 P3 Co 111.2(2) . . ? C21 P3 Co 107.4(2) . . ? C28 P3 Co 129.0(3) . . ? C40 P2 C46 100.5(3) . . ? C40 P2 C27 102.8(3) . . ? C46 P2 C27 103.1(3) . . ? C40 P2 Co 119.4(2) . . ? C46 P2 Co 121.6(2) . . ? C27 P2 Co 107.0(2) . . ? N Si C13 118.5(3) . . ? N Si C14 113.2(3) . . ? C13 Si C14 104.3(3) . . ? N Si C15 103.0(3) . . ? C13 Si C15 104.9(3) . . ? C14 Si C15 113.0(3) . . ? N C1 C6 121.9(7) . . ? N C1 C2 119.6(6) . . ? C6 C1 C2 118.4(7) . . ? C3 C2 C1 118.6(7) . . ? C3 C2 C7 118.5(7) . . ? C1 C2 C7 122.8(7) . . ? C4 C3 C2 121.9(7) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C5 C4 C3 117.4(7) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? C4 C5 C6 124.7(8) . . ? C4 C5 H5 117.6 . . ? C6 C5 H5 117.6 . . ? C5 C6 C1 118.9(8) . . ? C5 C6 C10 119.1(7) . . ? C1 C6 C10 121.8(7) . . ? C2 C7 C9 116.3(7) . . ? C2 C7 C8 113.3(6) . . ? C9 C7 C8 106.1(6) . . ? C2 C7 H7 106.9 . . ? C9 C7 H7 106.9 . . ? C8 C7 H7 106.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C11 112.9(7) . . ? C6 C10 C12 110.5(6) . . ? C11 C10 C12 108.9(6) . . ? C6 C10 H10 108.2 . . ? C11 C10 H10 108.2 . . ? C12 C10 H10 108.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si C13 H13A 109.5 . . ? Si C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si C14 H14A 109.5 . . ? Si C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P1 C15 Si 103.8(4) . . ? P1 C15 H15 128.1 . . ? Si C15 H15 128.1 . . ? C21 C16 C17 121.4(6) . . ? C21 C16 P1 116.1(5) . . ? C17 C16 P1 122.5(5) . . ? C18 C17 C16 118.2(7) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C17 C18 C19 120.3(7) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 120.5(7) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.8(7) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C16 C21 C20 119.8(6) . . ? C16 C21 P3 116.9(5) . . ? C20 C21 P3 123.2(5) . . ? C23 C22 C27 118.3(6) . . ? C23 C22 P1 124.0(6) . . ? C27 C22 P1 117.6(5) . . ? C24 C23 C22 121.2(7) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 119.7(7) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 119.5(7) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 122.1(7) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C26 C27 C22 119.1(6) . . ? C26 C27 P2 127.4(6) . . ? C22 C27 P2 113.5(5) . . ? C29 C28 C33 118.1(6) . . ? C29 C28 P3 121.7(5) . . ? C33 C28 P3 120.2(6) . . ? C28 C29 C30 122.5(7) . . ? C28 C29 H29 118.8 . . ? C30 C29 H29 118.8 . . ? C31 C30 C29 119.5(7) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 119.7(7) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C33 C32 C31 119.8(7) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C28 120.3(7) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C39 C34 C35 116.7(6) . . ? C39 C34 P3 119.6(5) . . ? C35 C34 P3 123.7(5) . . ? C36 C35 C34 122.1(7) . . ? C36 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? C35 C36 C37 120.9(7) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C38 C37 C36 118.4(7) . . ? C38 C37 H37 120.8 . . ? C36 C37 H37 120.8 . . ? C37 C38 C39 120.8(7) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C38 C39 C34 121.1(7) . . ? C38 C39 H39 119.4 . . ? C34 C39 H39 119.4 . . ? C41 C40 C45 117.8(7) . . ? C41 C40 P2 119.6(5) . . ? C45 C40 P2 122.6(5) . . ? C40 C41 C42 121.2(7) . . ? C40 C41 H41 119.4 . . ? C42 C41 H41 119.4 . . ? C43 C42 C41 120.2(7) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 120.5(7) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C43 C44 C45 118.7(7) . . ? C43 C44 H44 120.7 . . ? C45 C44 H44 120.7 . . ? C44 C45 C40 121.6(7) . . ? C44 C45 H45 119.2 . . ? C40 C45 H45 119.2 . . ? C47 C46 C51 117.8(6) . . ? C47 C46 P2 121.7(5) . . ? C51 C46 P2 120.5(5) . . ? C46 C47 C48 120.8(7) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C49 C48 C47 119.6(7) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C50 C49 C48 119.6(7) . . ? C50 C49 H49 120.2 . . ? C48 C49 H49 120.2 . . ? C51 C50 C49 120.0(7) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C46 122.2(7) . . ? C50 C51 H51 118.9 . . ? C46 C51 H51 118.9 . . ? C57 C52 C53 122.3(9) . . ? C57 C52 H52 118.8 . . ? C53 C52 H52 118.8 . . ? C52 C53 C54 119.4(9) . . ? C52 C53 H53 120.3 . . ? C54 C53 H53 120.3 . . ? C55 C54 C53 118.0(9) . . ? C55 C54 H54 121.0 . . ? C53 C54 H54 121.0 . . ? C54 C55 C56 122.2(9) . . ? C54 C55 H55 118.9 . . ? C56 C55 H55 118.9 . . ? C57 C56 C55 119.0(9) . . ? C57 C56 H56 120.5 . . ? C55 C56 H56 120.5 . . ? C52 C57 C56 119.0(10) . . ? C52 C57 H57 120.5 . . ? C56 C57 H57 120.5 . . ? C63 C58 C59 121.2(8) . . ? C63 C58 H58 119.4 . . ? C59 C58 H58 119.4 . . ? C60 C59 C58 119.1(8) . . ? C60 C59 H59 120.5 . . ? C58 C59 H59 120.5 . . ? C59 C60 C61 120.2(8) . . ? C59 C60 H60 119.9 . . ? C61 C60 H60 119.9 . . ? C60 C61 C62 119.8(9) . . ? C60 C61 H61 120.1 . . ? C62 C61 H61 120.1 . . ? C61 C62 C63 119.3(8) . . ? C61 C62 H62 120.3 . . ? C63 C62 H62 120.3 . . ? C58 C63 C62 120.3(8) . . ? C58 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 27.06 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 2.181 _refine_diff_density_min -1.397 _refine_diff_density_rms 0.173 data_mtw06 _database_code_depnum_ccdc_archive 'CCDC 289250' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56.50 H61 Cl Fe N P3 Si' _chemical_formula_weight 966.36 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Fe Fe 0.3463 0.8444 '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 10.8604(17) _cell_length_b 20.831(3) _cell_length_c 23.586(4) _cell_angle_alpha 72.318(3) _cell_angle_beta 83.313(3) _cell_angle_gamma 89.880(3) _cell_volume 5046.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5691 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 24.46 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.096 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2036 _exptl_absorpt_coefficient_mu 0.509 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19505 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.1350 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 25.08 _reflns_number_total 14316 _reflns_number_gt 8695 _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^)+(0.1202P)^2^+124.7027P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14316 _refine_ls_number_parameters 1156 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.1841 _refine_ls_R_factor_gt 0.1253 _refine_ls_wR_factor_ref 0.3269 _refine_ls_wR_factor_gt 0.2861 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.011 _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 Fe1A Fe 0.86518(14) 0.13397(8) 0.29104(7) 0.0096(4) Uani 1 1 d . . . Fe1B Fe 0.73761(14) 0.63284(8) 0.29176(7) 0.0102(4) Uani 1 1 d . . . Cl1A Cl 0.9818(3) 0.22438(14) 0.23435(13) 0.0200(7) Uani 1 1 d . . . Cl1B Cl 0.6453(3) 0.72145(14) 0.23559(13) 0.0205(7) Uani 1 1 d . . . N1A N 0.8025(8) 0.1235(5) 0.3736(4) 0.012(2) Uani 1 1 d . . . N1B N 0.7636(8) 0.6242(5) 0.3737(4) 0.011(2) Uani 1 1 d . . . P1A P 0.9287(3) 0.01826(14) 0.31750(13) 0.0111(6) Uani 1 1 d . . . P2A P 0.7164(3) 0.09487(14) 0.23535(13) 0.0118(6) Uani 1 1 d . . . P3A P 1.0397(3) 0.04238(18) 0.18231(15) 0.0232(8) Uani 1 1 d . . . P1B P 0.6636(3) 0.51625(14) 0.32003(13) 0.0115(6) Uani 1 1 d . . . P2B P 0.9124(3) 0.59429(14) 0.23429(13) 0.0122(6) Uani 1 1 d . . . P3B P 0.6100(3) 0.53436(17) 0.18694(15) 0.0218(8) Uani 1 1 d . . . Si1A Si 0.7697(3) 0.04398(16) 0.42300(14) 0.0146(7) Uani 1 1 d . . . Si1B Si 0.7772(3) 0.54475(16) 0.42205(14) 0.0148(7) Uani 1 1 d . . . C1 C 0.7967(10) 0.1802(5) 0.3969(5) 0.011(2) Uani 1 1 d . . . C2 C 0.9023(10) 0.2050(6) 0.4126(5) 0.015(3) Uani 1 1 d . . . C3 C 0.8901(11) 0.2539(6) 0.4418(5) 0.020(3) Uani 1 1 d . . . H3 H 0.9619 0.2699 0.4536 0.024 Uiso 1 1 calc R . . C4 C 0.7779(11) 0.2797(6) 0.4542(5) 0.022(3) Uani 1 1 d . . . H4 H 0.7711 0.3115 0.4758 0.026 Uiso 1 1 calc R . . C5 C 0.6727(10) 0.2584(6) 0.4343(5) 0.017(3) Uani 1 1 d . . . H5 H 0.5951 0.2774 0.4415 0.021 Uiso 1 1 calc R . . C6 C 0.6798(10) 0.2111(5) 0.4051(5) 0.012(2) Uani 1 1 d . . . C7 C 1.0327(10) 0.1817(6) 0.3972(5) 0.016(3) Uani 1 1 d . . . H7 H 1.0268 0.1577 0.3667 0.020 Uiso 1 1 calc R . . C8 C 1.1260(10) 0.2407(6) 0.3693(6) 0.022(3) Uani 1 1 d U . . H8A H 1.1379 0.2637 0.3989 0.033 Uiso 1 1 calc R . . H8B H 1.0947 0.2724 0.3345 0.033 Uiso 1 1 calc R . . H8C H 1.2054 0.2238 0.3565 0.033 Uiso 1 1 calc R . . C9 C 1.0784(12) 0.1318(6) 0.4515(5) 0.024(3) Uani 1 1 d . . . H9A H 1.1633 0.1198 0.4407 0.036 Uiso 1 1 calc R . . H9B H 1.0241 0.0912 0.4650 0.036 Uiso 1 1 calc R . . H9C H 1.0773 0.1523 0.4839 0.036 Uiso 1 1 calc R . . C10 C 0.5657(10) 0.1916(6) 0.3808(5) 0.018(3) Uani 1 1 d . . . H10 H 0.5891 0.1549 0.3627 0.021 Uiso 1 1 calc R . . C11 C 0.5315(13) 0.2523(7) 0.3311(7) 0.038(4) Uani 1 1 d . . . H11A H 0.5229 0.2914 0.3460 0.058 Uiso 1 1 calc R . . H11B H 0.4528 0.2426 0.3184 0.058 Uiso 1 1 calc R . . H11C H 0.5968 0.2622 0.2970 0.058 Uiso 1 1 calc R . . C12 C 0.4574(12) 0.1660(8) 0.4279(6) 0.035(4) Uani 1 1 d . . . H12A H 0.4211 0.2036 0.4400 0.053 Uiso 1 1 calc R . . H12B H 0.4853 0.1327 0.4628 0.053 Uiso 1 1 calc R . . H12C H 0.3950 0.1448 0.4119 0.053 Uiso 1 1 calc R . . C13 C 0.6206(12) 0.0013(7) 0.4202(6) 0.029(3) Uani 1 1 d . . . H13A H 0.5547 0.0341 0.4149 0.043 Uiso 1 1 calc R . . H13B H 0.5991 -0.0352 0.4577 0.043 Uiso 1 1 calc R . . H13C H 0.6296 -0.0173 0.3865 0.043 Uiso 1 1 calc R . . C14 C 0.7681(12) 0.0429(6) 0.5034(5) 0.024(3) Uani 1 1 d . . . H14A H 0.8439 0.0656 0.5076 0.036 Uiso 1 1 calc R . . H14B H 0.7639 -0.0039 0.5295 0.036 Uiso 1 1 calc R . . H14C H 0.6956 0.0664 0.5147 0.036 Uiso 1 1 calc R . . C15 C 0.8958(11) -0.0086(6) 0.3993(5) 0.018(3) Uani 1 1 d . . . H15A H 0.9719 -0.0033 0.4170 0.022 Uiso 1 1 calc R . . H15B H 0.8688 -0.0568 0.4141 0.022 Uiso 1 1 calc R . . C16 C 0.8153(10) -0.0304(6) 0.2932(5) 0.014(3) Uani 1 1 d . . . C17 C 0.8195(10) -0.0993(5) 0.3087(5) 0.009(2) Uani 1 1 d U . . H17 H 0.8804 -0.1211 0.3331 0.011 Uiso 1 1 calc R . . C18 C 0.7399(10) -0.1382(6) 0.2908(6) 0.019(3) Uani 1 1 d . . . H18 H 0.7449 -0.1859 0.3027 0.023 Uiso 1 1 calc R . . C19 C 0.6525(10) -0.1064(6) 0.2550(6) 0.019(3) Uani 1 1 d . . . H19 H 0.5966 -0.1322 0.2417 0.023 Uiso 1 1 calc R . . C20 C 0.6459(10) -0.0361(6) 0.2384(5) 0.015(3) Uani 1 1 d . . . H20 H 0.5847 -0.0147 0.2140 0.019 Uiso 1 1 calc R . . C21 C 0.7258(10) 0.0025(5) 0.2563(5) 0.013(2) Uani 1 1 d . . . C22 C 0.5512(9) 0.1089(5) 0.2507(5) 0.012(2) Uani 1 1 d D . . C23 C 0.4715(11) 0.0613(7) 0.2956(6) 0.032(3) Uani 1 1 d D . . H23 H 0.5054 0.0196 0.3156 0.039 Uiso 1 1 calc R . . C24 C 0.3497(13) 0.0705(6) 0.3124(6) 0.042(4) Uani 1 1 d DU . . H24 H 0.2930 0.0382 0.3402 0.050 Uiso 1 1 calc R . . C25 C 0.3256(14) 0.1343(6) 0.2821(6) 0.040(4) Uani 1 1 d DU . . H25 H 0.2520 0.1492 0.2995 0.048 Uiso 1 1 calc R . . C26 C 0.3803(16) 0.1833(7) 0.2325(6) 0.071(7) Uani 1 1 d D . . H26 H 0.3397 0.2212 0.2097 0.085 Uiso 1 1 calc R . . C27 C 0.5025(13) 0.1694(7) 0.2207(6) 0.035(3) Uani 1 1 d D . . H27 H 0.5551 0.2022 0.1910 0.042 Uiso 1 1 calc R . . C28 C 0.7396(10) 0.1250(6) 0.1526(5) 0.015(3) Uani 1 1 d . . . C29 C 0.6572(13) 0.1091(7) 0.1182(6) 0.029(3) Uani 1 1 d . . . H29 H 0.5854 0.0817 0.1375 0.035 Uiso 1 1 calc R . . C30 C 0.6766(14) 0.1319(7) 0.0577(6) 0.036(4) Uani 1 1 d . . . H30 H 0.6177 0.1217 0.0347 0.043 Uiso 1 1 calc R . . C31 C 0.7863(16) 0.1713(7) 0.0288(6) 0.045(4) Uani 1 1 d . . . H31 H 0.8040 0.1854 -0.0137 0.054 Uiso 1 1 calc R . . C32 C 0.8637(14) 0.1882(7) 0.0623(6) 0.032(3) Uani 1 1 d . . . H32 H 0.9342 0.2167 0.0431 0.039 Uiso 1 1 calc R . . C33 C 0.8445(12) 0.1655(6) 0.1235(6) 0.026(3) Uani 1 1 d . . . H33 H 0.9025 0.1773 0.1462 0.031 Uiso 1 1 calc R . . C34 C 1.0749(10) -0.0218(6) 0.3017(5) 0.016(3) Uani 1 1 d . . . C35 C 1.1331(11) -0.0643(6) 0.3472(7) 0.026(3) Uani 1 1 d . . . H35 H 1.0979 -0.0741 0.3879 0.031 Uiso 1 1 calc R . . C36 C 1.2475(13) -0.0933(7) 0.3322(8) 0.038(4) Uani 1 1 d . . . H36 H 1.2874 -0.1229 0.3632 0.045 Uiso 1 1 calc R . . C37 C 1.2991(12) -0.0795(8) 0.2751(9) 0.046(5) Uani 1 1 d . . . H37 H 1.3756 -0.0987 0.2661 0.056 Uiso 1 1 calc R . . C38 C 1.2405(11) -0.0371(7) 0.2289(7) 0.034(4) Uani 1 1 d . . . H38 H 1.2782 -0.0275 0.1887 0.040 Uiso 1 1 calc R . . C39 C 1.1285(11) -0.0086(6) 0.2403(6) 0.023(3) Uani 1 1 d . . . C40 C 0.9924(11) -0.0195(7) 0.1481(6) 0.026(3) Uani 1 1 d . . . C41 C 1.0003(14) -0.0896(8) 0.1744(7) 0.044(4) Uani 1 1 d . . . H41 H 1.0382 -0.1063 0.2102 0.052 Uiso 1 1 calc R . . C42 C 0.9520(15) -0.1359(8) 0.1479(8) 0.050(5) Uani 1 1 d . . . H42 H 0.9554 -0.1831 0.1665 0.060 Uiso 1 1 calc R . . C43 C 0.9014(15) -0.1121(9) 0.0962(9) 0.057(5) Uani 1 1 d . . . H43 H 0.8734 -0.1429 0.0775 0.069 Uiso 1 1 calc R . . C44 C 0.8897(15) -0.0434(8) 0.0698(7) 0.047(4) Uani 1 1 d . . . H44 H 0.8526 -0.0274 0.0338 0.056 Uiso 1 1 calc R . . C45 C 0.9325(13) 0.0017(8) 0.0966(7) 0.038(4) Uani 1 1 d . . . H45 H 0.9207 0.0485 0.0793 0.046 Uiso 1 1 calc R . . C46 C 1.1595(11) 0.0956(7) 0.1227(5) 0.022(3) Uani 1 1 d . . . C47 C 1.2072(19) 0.0818(10) 0.0732(8) 0.073(7) Uani 1 1 d . . . H47 H 1.1831 0.0413 0.0662 0.088 Uiso 1 1 calc R . . C48 C 1.2948(18) 0.1282(10) 0.0309(8) 0.065(6) Uani 1 1 d . . . H48 H 1.3221 0.1201 -0.0060 0.078 Uiso 1 1 calc R . . C49 C 1.3368(14) 0.1793(8) 0.0404(7) 0.043(4) Uani 1 1 d . . . H49 H 1.4052 0.2049 0.0147 0.051 Uiso 1 1 calc R . . C50 C 1.284(2) 0.1980(11) 0.0878(8) 0.077(7) Uani 1 1 d . . . H50 H 1.3054 0.2404 0.0919 0.093 Uiso 1 1 calc R . . C51 C 1.1971(19) 0.1532(11) 0.1308(8) 0.086(8) Uani 1 1 d . . . H51 H 1.1648 0.1640 0.1659 0.103 Uiso 1 1 calc R . . C52 C 0.239(2) 0.3496(11) 0.1511(13) 0.103(10) Uani 1 1 d . . . H52A H 0.2184 0.3012 0.1586 0.124 Uiso 1 1 calc R . . H52B H 0.2223 0.3578 0.1904 0.124 Uiso 1 1 calc R . . C53 C 0.371(2) 0.3556(13) 0.1372(12) 0.121(12) Uani 1 1 d . . . H53A H 0.4063 0.3145 0.1303 0.146 Uiso 1 1 calc R . . H53B H 0.4115 0.3672 0.1683 0.146 Uiso 1 1 calc R . . C54 C 0.375(5) 0.414(3) 0.0793(13) 0.398(11) Uani 1 1 d . . . H54A H 0.3729 0.4581 0.0879 0.478 Uiso 1 1 calc R . . H54B H 0.4518 0.4139 0.0521 0.478 Uiso 1 1 calc R . . C55 C 0.272(6) 0.4041(14) 0.0545(13) 0.31(4) Uani 1 1 d . . . H55A H 0.2827 0.3667 0.0368 0.374 Uiso 1 1 calc R . . H55B H 0.2517 0.4454 0.0234 0.374 Uiso 1 1 calc R . . C56 C 0.154(3) 0.3826(11) 0.1190(8) 0.078(7) Uani 1 1 d . . . H56A H 0.1225 0.4219 0.1309 0.093 Uiso 1 1 calc R . . H56B H 0.0847 0.3534 0.1158 0.093 Uiso 1 1 calc R . . C57 C 0.351(2) 0.8532(12) 0.1117(12) 0.103(10) Uani 1 1 d . . . H57 H 0.2879 0.8202 0.1160 0.124 Uiso 1 1 calc R . . C58 C 0.460(2) 0.8324(13) 0.1343(13) 0.142(15) Uani 1 1 d . . . H58 H 0.4636 0.7872 0.1592 0.170 Uiso 1 1 calc R . . C59 C 0.558(2) 0.8722(11) 0.1231(8) 0.068(6) Uani 1 1 d . . . H59 H 0.6360 0.8542 0.1333 0.082 Uiso 1 1 calc R . . C60 C 0.549(2) 0.9385(12) 0.0972(11) 0.090(8) Uani 1 1 d . . . H60 H 0.6153 0.9700 0.0933 0.108 Uiso 1 1 calc R . . C61 C 0.435(4) 0.9577(17) 0.0764(13) 0.157(19) Uani 1 1 d . . . H61 H 0.4283 1.0039 0.0546 0.188 Uiso 1 1 calc R . . C62 C 0.331(3) 0.9165(18) 0.0841(10) 0.113(12) Uani 1 1 d . . . H62 H 0.2535 0.9321 0.0710 0.136 Uiso 1 1 calc R . . C63 C 0.7591(10) 0.6802(5) 0.3957(5) 0.009(2) Uani 1 1 d . . . C64 C 0.8683(10) 0.7116(6) 0.4039(5) 0.011(2) Uani 1 1 d . . . C65 C 0.8605(11) 0.7597(6) 0.4333(5) 0.016(3) Uani 1 1 d . . . H65 H 0.9343 0.7793 0.4399 0.020 Uiso 1 1 calc R . . C66 C 0.7462(11) 0.7798(6) 0.4535(5) 0.019(3) Uani 1 1 d . . . H66 H 0.7416 0.8113 0.4755 0.023 Uiso 1 1 calc R . . C67 C 0.6400(11) 0.7538(6) 0.4413(5) 0.017(3) Uani 1 1 d U . . H67 H 0.5624 0.7699 0.4533 0.020 Uiso 1 1 calc R . . C68 C 0.6413(10) 0.7047(6) 0.4121(5) 0.013(2) Uani 1 1 d . . . C69 C 0.9979(9) 0.6928(6) 0.3811(5) 0.015(3) Uani 1 1 d . . . H69 H 0.9858 0.6578 0.3609 0.018 Uiso 1 1 calc R . . C70 C 1.0582(13) 0.7561(7) 0.3328(7) 0.039(4) Uani 1 1 d . . . H70A H 1.0694 0.7918 0.3509 0.058 Uiso 1 1 calc R . . H70B H 1.0044 0.7716 0.3010 0.058 Uiso 1 1 calc R . . H70C H 1.1390 0.7450 0.3156 0.058 Uiso 1 1 calc R . . C71 C 1.0769(12) 0.6643(8) 0.4285(6) 0.033(3) Uani 1 1 d . . . H71A H 1.1504 0.6456 0.4120 0.050 Uiso 1 1 calc R . . H71B H 1.0303 0.6285 0.4609 0.050 Uiso 1 1 calc R . . H71C H 1.1028 0.6998 0.4444 0.050 Uiso 1 1 calc R . . C72 C 0.5198(10) 0.6812(6) 0.3971(5) 0.017(3) Uani 1 1 d U . . H72 H 0.5412 0.6573 0.3666 0.020 Uiso 1 1 calc R . . C73 C 0.4393(11) 0.7376(7) 0.3707(6) 0.027(3) Uani 1 1 d . . . H73A H 0.4144 0.7613 0.4000 0.041 Uiso 1 1 calc R . . H73B H 0.3654 0.7196 0.3597 0.041 Uiso 1 1 calc R . . H73C H 0.4853 0.7691 0.3348 0.041 Uiso 1 1 calc R . . C74 C 0.4499(11) 0.6299(6) 0.4530(6) 0.024(3) Uani 1 1 d . . . H74A H 0.4353 0.6503 0.4854 0.036 Uiso 1 1 calc R . . H74B H 0.4997 0.5899 0.4659 0.036 Uiso 1 1 calc R . . H74C H 0.3702 0.6167 0.4434 0.036 Uiso 1 1 calc R . . C75 C 0.9299(12) 0.5022(6) 0.4164(6) 0.026(3) Uani 1 1 d . . . H75A H 0.9439 0.4930 0.3779 0.038 Uiso 1 1 calc R . . H75B H 0.9278 0.4598 0.4492 0.038 Uiso 1 1 calc R . . H75C H 0.9973 0.5319 0.4193 0.038 Uiso 1 1 calc R . . C76 C 0.7425(12) 0.5424(7) 0.5022(5) 0.023(3) Uani 1 1 d . . . H76A H 0.8113 0.5643 0.5135 0.035 Uiso 1 1 calc R . . H76B H 0.7320 0.4954 0.5278 0.035 Uiso 1 1 calc R . . H76C H 0.6661 0.5661 0.5073 0.035 Uiso 1 1 calc R . . C77 C 0.6627(10) 0.4902(6) 0.4014(5) 0.014(2) Uani 1 1 d . . . H77A H 0.6852 0.4424 0.4158 0.017 Uiso 1 1 calc R . . H77B H 0.5785 0.4944 0.4207 0.017 Uiso 1 1 calc R . . C78 C 0.7883(10) 0.4684(6) 0.2941(5) 0.012(2) Uani 1 1 d U . . C79 C 0.7766(11) 0.3997(6) 0.3106(6) 0.022(3) Uani 1 1 d . . . H79 H 0.7049 0.3777 0.3360 0.026 Uiso 1 1 calc R . . C80 C 0.8667(10) 0.3613(6) 0.2911(6) 0.018(3) Uani 1 1 d . . . H80 H 0.8572 0.3135 0.3035 0.022 Uiso 1 1 calc R . . C81 C 0.9699(10) 0.3931(6) 0.2535(5) 0.017(3) Uani 1 1 d . . . H81 H 1.0319 0.3674 0.2395 0.020 Uiso 1 1 calc R . . C82 C 0.9834(10) 0.4640(6) 0.2360(5) 0.014(2) Uani 1 1 d . . . H82 H 1.0546 0.4859 0.2100 0.017 Uiso 1 1 calc R . . C83 C 0.8955(9) 0.5016(5) 0.2559(5) 0.010(2) Uani 1 1 d . . . C84 C 1.0706(10) 0.6107(6) 0.2476(5) 0.019(3) Uani 1 1 d D . . C85 C 1.1356(11) 0.5638(7) 0.2871(6) 0.030(3) Uani 1 1 d DU . . H85 H 1.0998 0.5197 0.3055 0.037 Uiso 1 1 calc R . . C86 C 1.2508(12) 0.5787(6) 0.3006(6) 0.041(4) Uani 1 1 d DU . . H86 H 1.2988 0.5467 0.3260 0.049 Uiso 1 1 calc R . . C87 C 1.2872(13) 0.6442(6) 0.2736(6) 0.036(3) Uani 1 1 d DU . . H87 H 1.3597 0.6584 0.2861 0.043 Uiso 1 1 calc R . . C88 C 1.2336(16) 0.6936(8) 0.2302(7) 0.070(5) Uani 1 1 d DU . . H88 H 1.2726 0.7366 0.2102 0.084 Uiso 1 1 calc R . . C89 C 1.1224(13) 0.6755(7) 0.2190(6) 0.034(3) Uani 1 1 d DU . . H89 H 1.0785 0.7072 0.1911 0.041 Uiso 1 1 calc R . . C90 C 0.9263(10) 0.6248(6) 0.1521(5) 0.015(3) Uani 1 1 d . . . C91 C 0.8325(12) 0.6621(6) 0.1247(6) 0.025(3) Uani 1 1 d . . . H91 H 0.7635 0.6733 0.1481 0.030 Uiso 1 1 calc R . . C92 C 0.8398(14) 0.6834(6) 0.0621(6) 0.030(3) Uani 1 1 d . . . H92 H 0.7769 0.7106 0.0431 0.036 Uiso 1 1 calc R . . C93 C 0.9334(13) 0.6661(8) 0.0288(6) 0.036(4) Uani 1 1 d . . . H93 H 0.9339 0.6789 -0.0135 0.043 Uiso 1 1 calc R . . C94 C 1.0299(14) 0.6299(8) 0.0546(6) 0.037(4) Uani 1 1 d . . . H94 H 1.0981 0.6201 0.0298 0.045 Uiso 1 1 calc R . . C95 C 1.0278(10) 0.6075(6) 0.1168(5) 0.017(3) Uani 1 1 d . . . H95 H 1.0927 0.5814 0.1350 0.020 Uiso 1 1 calc R . . C96 C 0.5245(10) 0.4746(5) 0.3076(5) 0.016(3) Uani 1 1 d . . . C97 C 0.4440(12) 0.4333(6) 0.3558(7) 0.030(3) Uani 1 1 d . . . H97 H 0.4630 0.4257 0.3956 0.035 Uiso 1 1 calc R . . C98 C 0.3375(11) 0.4032(7) 0.3465(8) 0.036(4) Uani 1 1 d . . . H98 H 0.2850 0.3753 0.3799 0.043 Uiso 1 1 calc R . . C99 C 0.3079(12) 0.4130(7) 0.2911(8) 0.038(4) Uani 1 1 d . . . H99 H 0.2344 0.3926 0.2852 0.045 Uiso 1 1 calc R . . C100 C 0.3883(12) 0.4548(7) 0.2406(7) 0.037(4) Uani 1 1 d . . . H100 H 0.3658 0.4630 0.2014 0.044 Uiso 1 1 calc R . . C101 C 0.4982(10) 0.4834(6) 0.2483(6) 0.020(3) Uani 1 1 d U . . C102 C 0.6781(11) 0.4698(6) 0.1554(6) 0.022(3) Uani 1 1 d . . . C103 C 0.6578(11) 0.4008(6) 0.1833(6) 0.028(3) Uani 1 1 d . . . H103 H 0.6013 0.3853 0.2189 0.034 Uiso 1 1 calc R . . C104 C 0.7201(13) 0.3539(7) 0.1594(7) 0.037(4) Uani 1 1 d . . . H104 H 0.7046 0.3070 0.1787 0.044 Uiso 1 1 calc R . . C105 C 0.8048(14) 0.3758(8) 0.1073(6) 0.040(4) Uani 1 1 d . . . H105 H 0.8475 0.3443 0.0910 0.048 Uiso 1 1 calc R . . C106 C 0.8246(18) 0.4435(9) 0.0805(8) 0.063(6) Uani 1 1 d . . . H106 H 0.8799 0.4592 0.0445 0.076 Uiso 1 1 calc R . . C107 C 0.7635(17) 0.4908(8) 0.1056(7) 0.051(5) Uani 1 1 d . . . H107 H 0.7823 0.5376 0.0875 0.061 Uiso 1 1 calc R . . C108 C 0.5139(13) 0.5813(8) 0.1295(6) 0.041(4) Uani 1 1 d . . . C109 C 0.483(4) 0.562(2) 0.0856(17) 0.31(4) Uani 1 1 d . . . H109 H 0.5068 0.5189 0.0821 0.366 Uiso 1 1 calc R . . C110 C 0.412(6) 0.604(3) 0.043(2) 0.47(6) Uani 1 1 d . . . H110 H 0.3906 0.5878 0.0119 0.563 Uiso 1 1 calc R . . C111 C 0.3749(19) 0.6616(13) 0.0440(9) 0.084(8) Uani 1 1 d . . . H111 H 0.3335 0.6902 0.0130 0.101 Uiso 1 1 calc R . . C112 C 0.397(2) 0.6769(12) 0.0873(11) 0.095(9) Uani 1 1 d . . . H112 H 0.3647 0.7176 0.0921 0.114 Uiso 1 1 calc R . . C113 C 0.468(2) 0.6372(12) 0.1321(10) 0.111(11) Uani 1 1 d . . . H113 H 0.4822 0.6529 0.1647 0.133 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 Fe1A 0.0077(8) 0.0107(8) 0.0120(9) -0.0067(7) 0.0017(6) -0.0017(6) Fe1B 0.0081(8) 0.0111(9) 0.0140(9) -0.0078(7) -0.0014(6) -0.0001(6) Cl1A 0.0229(16) 0.0154(15) 0.0221(16) -0.0086(13) 0.0038(12) -0.0077(12) Cl1B 0.0252(16) 0.0155(15) 0.0224(16) -0.0070(13) -0.0061(12) 0.0083(12) N1A 0.0137(49) 0.0170(52) 0.0123(50) -0.0139(42) 0.0019(38) -0.0056(39) N1B 0.005(5) 0.019(5) 0.015(5) -0.014(4) -0.002(4) 0.002(4) P1A 0.0093(15) 0.0087(15) 0.0181(16) -0.0072(13) -0.0044(12) 0.0013(11) P2A 0.0092(15) 0.0121(15) 0.0166(16) -0.0075(13) -0.0030(12) 0.0003(12) P3A 0.0137(17) 0.035(2) 0.0259(19) -0.0197(16) 0.0065(13) -0.0065(14) P1B 0.0077(14) 0.0112(15) 0.0179(16) -0.0092(13) 0.0026(12) -0.0028(11) P2B 0.0105(15) 0.0115(15) 0.0151(16) -0.0056(13) 0.0007(12) -0.0010(12) P3B 0.0213(18) 0.0258(19) 0.0255(19) -0.0158(15) -0.0105(14) 0.0072(14) Si1A 0.0169(17) 0.0165(17) 0.0108(17) -0.0059(14) 0.0021(13) -0.0038(13) Si1B 0.0175(17) 0.0151(17) 0.0134(17) -0.0061(14) -0.0030(13) -0.0009(13) C1 0.014(6) 0.013(6) 0.005(6) -0.001(5) 0.003(4) -0.001(5) C2 0.009(6) 0.019(7) 0.017(6) -0.009(5) 0.003(5) -0.001(5) C3 0.017(6) 0.030(7) 0.022(7) -0.017(6) -0.012(5) 0.005(5) C4 0.027(7) 0.023(7) 0.022(7) -0.017(6) 0.001(5) 0.003(6) C5 0.010(6) 0.029(7) 0.018(6) -0.016(6) 0.000(5) 0.009(5) C6 0.015(6) 0.009(6) 0.012(6) -0.004(5) -0.003(5) -0.007(5) C7 0.011(6) 0.019(7) 0.028(7) -0.017(6) -0.013(5) 0.005(5) C8 0.006(5) 0.028(6) 0.030(6) -0.006(5) -0.001(5) 0.005(5) C9 0.028(7) 0.026(7) 0.024(7) -0.014(6) -0.011(6) -0.002(6) C10 0.010(6) 0.026(7) 0.025(7) -0.019(6) -0.008(5) 0.006(5) C11 0.028(8) 0.046(9) 0.043(9) -0.012(8) -0.016(7) -0.005(7) C12 0.020(7) 0.052(10) 0.039(9) -0.027(8) 0.010(6) -0.009(7) C13 0.025(7) 0.025(7) 0.034(8) -0.011(6) 0.013(6) -0.012(6) C14 0.034(8) 0.025(7) 0.010(6) -0.003(5) 0.003(5) 0.000(6) C15 0.023(7) 0.015(6) 0.020(7) -0.007(5) -0.014(5) -0.001(5) C16 0.007(6) 0.028(7) 0.009(6) -0.010(5) 0.004(4) -0.005(5) C17 0.011(4) 0.007(4) 0.011(4) -0.004(3) 0.003(3) 0.004(3) C18 0.011(6) 0.008(6) 0.036(8) -0.007(6) 0.007(5) -0.003(5) C19 0.005(6) 0.022(7) 0.033(7) -0.012(6) -0.002(5) 0.000(5) C20 0.006(6) 0.014(6) 0.026(7) -0.005(5) -0.004(5) -0.001(5) C21 0.013(6) 0.010(6) 0.017(6) -0.005(5) 0.000(5) -0.001(5) C22 0.007(6) 0.017(6) 0.018(6) -0.012(5) -0.007(5) 0.001(5) C23 0.013(7) 0.052(9) 0.048(9) -0.037(8) -0.010(6) 0.005(6) C24 0.029(7) 0.048(7) 0.062(8) -0.037(6) -0.003(6) -0.004(6) C25 0.059(6) 0.027(5) 0.036(5) -0.024(4) 0.025(4) 0.001(4) C26 0.114(17) 0.072(13) 0.040(10) -0.024(10) -0.047(11) 0.083(13) C27 0.035(9) 0.030(8) 0.040(9) -0.008(7) -0.009(7) 0.017(7) C28 0.010(6) 0.014(6) 0.020(7) -0.005(5) -0.001(5) 0.006(5) C29 0.037(8) 0.034(8) 0.015(7) -0.003(6) -0.005(6) -0.001(6) C30 0.048(9) 0.035(9) 0.025(8) -0.005(7) -0.019(7) -0.007(7) C31 0.096(14) 0.028(8) 0.005(7) -0.002(6) 0.007(7) -0.022(8) C32 0.049(9) 0.021(7) 0.021(8) 0.005(6) -0.012(6) -0.009(6) C33 0.036(8) 0.012(7) 0.027(8) -0.003(6) -0.003(6) -0.008(6) C34 0.010(6) 0.017(6) 0.025(7) -0.013(5) -0.008(5) -0.003(5) C35 0.020(7) 0.017(7) 0.050(9) -0.022(7) -0.009(6) -0.003(5) C36 0.026(8) 0.022(8) 0.075(12) -0.020(8) -0.031(8) 0.000(6) C37 0.001(6) 0.053(10) 0.108(15) -0.061(11) 0.002(8) -0.002(6) C38 0.004(6) 0.046(9) 0.069(11) -0.047(8) 0.001(6) 0.005(6) C39 0.010(6) 0.025(7) 0.041(8) -0.020(6) -0.008(6) -0.004(5) C40 0.010(6) 0.036(8) 0.033(8) -0.019(7) 0.010(5) -0.001(6) C41 0.033(9) 0.053(11) 0.051(10) -0.027(9) 0.001(7) -0.004(7) C42 0.047(10) 0.041(10) 0.083(13) -0.043(10) -0.035(9) 0.008(8) C43 0.044(10) 0.071(13) 0.087(14) -0.065(12) -0.018(10) 0.003(9) C44 0.058(11) 0.054(11) 0.050(10) -0.043(9) -0.025(8) 0.012(8) C45 0.033(8) 0.045(9) 0.046(10) -0.029(8) -0.006(7) 0.001(7) C46 0.012(6) 0.039(8) 0.023(7) -0.020(6) 0.003(5) -0.007(6) C47 0.092(15) 0.085(14) 0.052(12) -0.052(11) 0.035(10) -0.052(12) C48 0.076(14) 0.075(14) 0.041(11) -0.026(10) 0.027(9) -0.023(11) C49 0.031(9) 0.045(10) 0.045(10) -0.012(8) 0.019(7) -0.014(7) C50 0.099(16) 0.079(14) 0.053(12) -0.026(11) 0.016(11) -0.063(13) C51 0.089(15) 0.125(18) 0.048(11) -0.055(12) 0.047(10) -0.099(14) C52 0.086(18) 0.059(15) 0.14(2) -0.025(15) 0.087(17) -0.026(13) C53 0.092(17) 0.13(2) 0.17(3) -0.12(2) 0.082(18) -0.088(16) C54 0.41(3) 0.70(5) 0.06(2) -0.13(3) 0.11(3) -0.515 C55 0.81(12) 0.061(18) 0.08(2) 0.025(15) -0.22(5) -0.12(4) C56 0.13(2) 0.071(15) 0.039(12) -0.039(11) 0.008(12) -0.034(14) C57 0.11(2) 0.072(16) 0.12(2) 0.006(15) -0.099(18) 0.019(14) C58 0.070(16) 0.12(2) 0.16(3) 0.10(2) -0.067(17) -0.055(15) C59 0.081(15) 0.086(16) 0.038(11) -0.024(11) 0.004(9) -0.015(12) C60 0.092(18) 0.065(15) 0.106(19) -0.037(14) 0.049(15) -0.022(13) C61 0.16(3) 0.14(3) 0.09(2) 0.055(19) 0.05(2) 0.11(3) C62 0.09(2) 0.19(3) 0.040(13) -0.017(17) -0.008(13) 0.09(2) C63 0.012(6) 0.004(5) 0.012(6) -0.004(5) -0.001(4) 0.001(4) C64 0.007(6) 0.016(6) 0.010(6) -0.003(5) 0.002(4) -0.005(5) C65 0.019(6) 0.020(7) 0.011(6) -0.007(5) -0.002(5) -0.011(5) C66 0.029(7) 0.017(7) 0.018(7) -0.017(5) 0.003(5) -0.006(5) C67 0.018(5) 0.016(5) 0.022(6) -0.016(5) 0.005(4) 0.004(4) C68 0.012(6) 0.019(6) 0.011(6) -0.007(5) -0.001(5) 0.002(5) C69 0.002(5) 0.023(7) 0.026(7) -0.015(6) -0.001(5) -0.002(5) C70 0.029(8) 0.032(8) 0.048(10) -0.010(7) 0.018(7) 0.001(6) C71 0.020(7) 0.052(10) 0.035(8) -0.022(7) -0.013(6) 0.008(6) C72 0.011(5) 0.012(5) 0.029(6) -0.015(5) 0.011(4) -0.007(4) C73 0.012(6) 0.039(8) 0.037(8) -0.019(7) -0.011(6) 0.002(6) C74 0.009(6) 0.028(7) 0.037(8) -0.015(6) 0.006(5) -0.008(5) C75 0.027(7) 0.026(7) 0.025(7) -0.007(6) -0.011(6) 0.009(6) C76 0.029(7) 0.030(8) 0.012(6) -0.005(6) -0.007(5) 0.000(6) C77 0.012(6) 0.012(6) 0.017(6) -0.005(5) 0.006(5) 0.004(5) C78 0.004(5) 0.018(6) 0.014(5) -0.006(4) 0.000(4) 0.003(4) C79 0.010(6) 0.021(7) 0.036(8) -0.012(6) 0.004(5) -0.002(5) C80 0.012(6) 0.014(6) 0.034(7) -0.012(6) -0.007(5) 0.000(5) C81 0.013(6) 0.019(7) 0.023(7) -0.014(6) -0.001(5) 0.002(5) C82 0.010(6) 0.016(6) 0.012(6) 0.000(5) 0.002(4) -0.001(5) C83 0.006(5) 0.005(5) 0.020(6) -0.003(5) -0.007(5) 0.001(4) C84 0.013(6) 0.029(7) 0.018(7) -0.011(6) -0.002(5) -0.006(5) C85 0.016(6) 0.041(7) 0.044(7) -0.029(6) -0.001(5) -0.002(5) C86 0.017(6) 0.066(8) 0.048(7) -0.029(6) -0.007(5) 0.000(6) C87 0.040(4) 0.036(4) 0.037(4) -0.014(2) -0.013(2) 0.002(2) C88 0.082(9) 0.068(9) 0.059(9) -0.017(7) -0.007(7) -0.057(7) C89 0.042(7) 0.031(7) 0.021(6) 0.006(5) -0.010(5) -0.017(6) C90 0.009(6) 0.015(6) 0.020(7) -0.007(5) 0.003(5) -0.001(5) C91 0.031(8) 0.018(7) 0.027(8) -0.010(6) 0.000(6) 0.004(6) C92 0.051(9) 0.017(7) 0.024(8) -0.001(6) -0.017(7) 0.006(6) C93 0.038(9) 0.051(10) 0.011(7) 0.002(7) -0.007(6) -0.013(7) C94 0.041(9) 0.054(10) 0.022(8) -0.022(7) 0.009(6) 0.007(7) C95 0.012(6) 0.017(6) 0.019(7) -0.004(5) 0.004(5) 0.005(5) C96 0.009(6) 0.009(6) 0.031(7) -0.011(5) 0.001(5) 0.001(5) C97 0.027(8) 0.022(7) 0.044(9) -0.020(7) 0.007(6) 0.000(6) C98 0.007(6) 0.028(8) 0.077(12) -0.027(8) 0.007(7) -0.012(6) C99 0.008(7) 0.037(9) 0.092(13) -0.049(9) -0.021(8) 0.011(6) C100 0.021(8) 0.044(9) 0.062(11) -0.037(8) -0.013(7) 0.007(7) C101 0.009(5) 0.018(6) 0.037(6) -0.012(5) -0.001(5) 0.006(4) C102 0.016(6) 0.034(8) 0.026(7) -0.016(6) -0.014(5) 0.005(6) C103 0.016(7) 0.023(8) 0.047(9) -0.017(7) 0.002(6) -0.002(5) C104 0.038(9) 0.033(8) 0.041(9) -0.015(7) -0.002(7) 0.009(7) C105 0.050(10) 0.047(10) 0.034(9) -0.030(8) 0.000(7) -0.004(8) C106 0.088(14) 0.057(12) 0.040(10) -0.022(9) 0.031(9) -0.034(10) C107 0.079(13) 0.041(10) 0.030(9) -0.015(8) 0.011(8) -0.014(9) C108 0.025(8) 0.081(12) 0.036(9) -0.041(9) -0.026(6) 0.041(8) C109 0.45(7) 0.42(6) 0.25(4) -0.32(5) -0.32(5) 0.40(6) C110 0.71(11) 0.69(10) 0.30(5) -0.43(7) -0.46(7) 0.67(10) C111 0.073(14) 0.14(2) 0.041(12) -0.022(13) -0.023(10) 0.078(14) C112 0.12(2) 0.093(17) 0.097(19) -0.061(15) -0.043(16) 0.084(16) C113 0.17(2) 0.123(19) 0.103(18) -0.090(16) -0.105(18) 0.136(19) _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 Fe1A N1A 1.933(9) . ? Fe1A Cl1A 2.242(3) . ? Fe1A P1A 2.420(3) . ? Fe1A P2A 2.480(3) . ? Fe1B N1B 1.939(9) . ? Fe1B Cl1B 2.233(3) . ? Fe1B P1B 2.427(3) . ? Fe1B P2B 2.478(3) . ? N1A C1 1.445(13) . ? N1A Si1A 1.720(10) . ? N1B C63 1.412(13) . ? N1B Si1B 1.719(10) . ? P1A C15 1.830(12) . ? P1A C16 1.842(11) . ? P1A C34 1.845(11) . ? P2A C22 1.829(11) . ? P2A C21 1.841(11) . ? P2A C28 1.846(12) . ? P3A C40 1.820(13) . ? P3A C39 1.831(13) . ? P3A C46 1.880(12) . ? P1B C77 1.827(11) . ? P1B C78 1.837(11) . ? P1B C96 1.839(11) . ? P2B C84 1.834(12) . ? P2B C90 1.835(12) . ? P2B C83 1.846(10) . ? P3B C101 1.833(12) . ? P3B C102 1.839(12) . ? P3B C108 1.844(13) . ? Si1A C13 1.866(12) . ? Si1A C14 1.887(12) . ? Si1A C15 1.890(12) . ? Si1B C76 1.869(12) . ? Si1B C77 1.887(11) . ? Si1B C75 1.888(12) . ? C1 C2 1.392(16) . ? C1 C6 1.442(16) . ? C2 C3 1.392(16) . ? C2 C7 1.534(15) . ? C3 C4 1.366(17) . ? C3 H3 0.9500 . ? C4 C5 1.405(17) . ? C4 H4 0.9500 . ? C5 C6 1.360(15) . ? C5 H5 0.9500 . ? C6 C10 1.529(15) . ? C7 C9 1.518(17) . ? C7 C8 1.526(16) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.498(17) . ? C10 C11 1.520(18) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.372(15) . ? C16 C21 1.415(16) . ? C17 C18 1.372(16) . ? C17 H17 0.9500 . ? C18 C19 1.376(17) . ? C18 H18 0.9500 . ? C19 C20 1.400(16) . ? C19 H19 0.9500 . ? C20 C21 1.370(16) . ? C20 H20 0.9500 . ? C22 C27 1.383(17) . ? C22 C23 1.416(18) . ? C23 C24 1.366(19) . ? C23 H23 0.9500 . ? C24 C25 1.346(9) . ? C24 H24 0.9500 . ? C25 C26 1.371(10) . ? C25 H25 0.9500 . ? C26 C27 1.37(2) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.379(18) . ? C28 C33 1.397(17) . ? C29 C30 1.351(18) . ? C29 H29 0.9500 . ? C30 C31 1.43(2) . ? C30 H30 0.9500 . ? C31 C32 1.33(2) . ? C31 H31 0.9500 . ? C32 C33 1.365(18) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.384(17) . ? C34 C39 1.440(17) . ? C35 C36 1.436(19) . ? C35 H35 0.9500 . ? C36 C37 1.34(2) . ? C36 H36 0.9500 . ? C37 C38 1.40(2) . ? C37 H37 0.9500 . ? C38 C39 1.385(17) . ? C38 H38 0.9500 . ? C40 C45 1.40(2) . ? C40 C41 1.41(2) . ? C41 C42 1.43(2) . ? C41 H41 0.9500 . ? C42 C43 1.35(2) . ? C42 H42 0.9500 . ? C43 C44 1.39(2) . ? C43 H43 0.9500 . ? C44 C45 1.39(2) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.333(19) . ? C46 C51 1.34(2) . ? C47 C48 1.43(2) . ? C47 H47 0.9500 . ? C48 C49 1.25(2) . ? C48 H48 0.9500 . ? C49 C50 1.36(2) . ? C49 H49 0.9500 . ? C50 C51 1.41(2) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C56 1.32(3) . ? C52 C53 1.42(3) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.53(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.37(6) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.81(6) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C62 1.31(3) . ? C57 C58 1.36(3) . ? C57 H57 0.9500 . ? C58 C59 1.31(3) . ? C58 H58 0.9500 . ? C59 C60 1.34(3) . ? C59 H59 0.9500 . ? C60 C61 1.40(4) . ? C60 H60 0.9500 . ? C61 C62 1.38(5) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.416(15) . ? C63 C68 1.431(15) . ? C64 C65 1.380(15) . ? C64 C69 1.539(15) . ? C65 C66 1.386(17) . ? C65 H65 0.9500 . ? C66 C67 1.371(16) . ? C66 H66 0.9500 . ? C67 C68 1.396(15) . ? C67 H67 0.9500 . ? C68 C72 1.525(16) . ? C69 C71 1.470(17) . ? C69 C70 1.543(18) . ? C69 H69 1.0000 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.487(17) . ? C72 C74 1.541(16) . ? C72 H72 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.366(16) . ? C78 C83 1.423(15) . ? C79 C80 1.388(16) . ? C79 H79 0.9500 . ? C80 C81 1.377(16) . ? C80 H80 0.9500 . ? C81 C82 1.411(16) . ? C81 H81 0.9500 . ? C82 C83 1.364(15) . ? C82 H82 0.9500 . ? C84 C85 1.384(19) . ? C84 C89 1.399(18) . ? C85 C86 1.385(18) . ? C85 H85 0.9500 . ? C86 C87 1.356(9) . ? C86 H86 0.9500 . ? C87 C88 1.394(10) . ? C87 H87 0.9500 . ? C88 C89 1.34(2) . ? C88 H88 0.9500 . ? C89 H89 0.9500 . ? C90 C91 1.380(17) . ? C90 C95 1.416(15) . ? C91 C92 1.400(18) . ? C91 H91 0.9500 . ? C92 C93 1.33(2) . ? C92 H92 0.9500 . ? C93 C94 1.38(2) . ? C93 H93 0.9500 . ? C94 C95 1.396(18) . ? C94 H94 0.9500 . ? C95 H95 0.9500 . ? C96 C97 1.405(17) . ? C96 C101 1.417(17) . ? C97 C98 1.387(18) . ? C97 H97 0.9500 . ? C98 C99 1.34(2) . ? C98 H98 0.9500 . ? C99 C100 1.44(2) . ? C99 H99 0.9500 . ? C100 C101 1.390(18) . ? C100 H100 0.9500 . ? C102 C107 1.37(2) . ? C102 C103 1.393(18) . ? C103 C104 1.405(18) . ? C103 H103 0.9500 . ? C104 C105 1.40(2) . ? C104 H104 0.9500 . ? C105 C106 1.36(2) . ? C105 H105 0.9500 . ? C106 C107 1.42(2) . ? C106 H106 0.9500 . ? C107 H107 0.9500 . ? C108 C113 1.28(2) . ? C108 C109 1.30(3) . ? C109 C110 1.41(4) . ? C109 H109 0.9500 . ? C110 C111 1.27(4) . ? C110 H110 0.9500 . ? C111 C112 1.21(3) . ? C111 H111 0.9500 . ? C112 C113 1.43(3) . ? C112 H112 0.9500 . ? C113 H113 0.9500 . ? 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 N1A Fe1A Cl1A 121.8(3) . . ? N1A Fe1A P1A 91.0(3) . . ? Cl1A Fe1A P1A 125.94(12) . . ? N1A Fe1A P2A 113.8(3) . . ? Cl1A Fe1A P2A 113.27(12) . . ? P1A Fe1A P2A 84.06(10) . . ? N1B Fe1B Cl1B 121.9(3) . . ? N1B Fe1B P1B 91.5(3) . . ? Cl1B Fe1B P1B 125.70(12) . . ? N1B Fe1B P2B 114.0(3) . . ? Cl1B Fe1B P2B 112.89(12) . . ? P1B Fe1B P2B 84.05(10) . . ? C1 N1A Si1A 118.5(7) . . ? C1 N1A Fe1A 121.4(7) . . ? Si1A N1A Fe1A 119.7(5) . . ? C63 N1B Si1B 119.6(7) . . ? C63 N1B Fe1B 121.9(7) . . ? Si1B N1B Fe1B 118.3(5) . . ? C15 P1A C16 104.6(5) . . ? C15 P1A C34 105.0(5) . . ? C16 P1A C34 101.7(5) . . ? C15 P1A Fe1A 102.0(4) . . ? C16 P1A Fe1A 107.4(4) . . ? C34 P1A Fe1A 133.4(4) . . ? C22 P2A C21 104.2(5) . . ? C22 P2A C28 101.4(5) . . ? C21 P2A C28 105.8(5) . . ? C22 P2A Fe1A 118.8(3) . . ? C21 P2A Fe1A 106.5(4) . . ? C28 P2A Fe1A 118.8(4) . . ? C40 P3A C39 101.8(6) . . ? C40 P3A C46 102.3(5) . . ? C39 P3A C46 104.9(6) . . ? C77 P1B C78 104.2(5) . . ? C77 P1B C96 105.0(5) . . ? C78 P1B C96 101.8(5) . . ? C77 P1B Fe1B 101.7(4) . . ? C78 P1B Fe1B 107.4(4) . . ? C96 P1B Fe1B 133.7(4) . . ? C84 P2B C90 101.2(5) . . ? C84 P2B C83 104.7(5) . . ? C90 P2B C83 106.4(5) . . ? C84 P2B Fe1B 118.1(3) . . ? C90 P2B Fe1B 118.4(4) . . ? C83 P2B Fe1B 106.7(4) . . ? C101 P3B C102 101.4(6) . . ? C101 P3B C108 104.6(7) . . ? C102 P3B C108 103.1(6) . . ? N1A Si1A C13 117.4(6) . . ? N1A Si1A C14 111.9(5) . . ? C13 Si1A C14 105.6(6) . . ? N1A Si1A C15 103.7(5) . . ? C13 Si1A C15 105.4(6) . . ? C14 Si1A C15 112.8(5) . . ? N1B Si1B C76 111.9(5) . . ? N1B Si1B C77 104.7(5) . . ? C76 Si1B C77 111.5(5) . . ? N1B Si1B C75 118.2(5) . . ? C76 Si1B C75 105.9(6) . . ? C77 Si1B C75 104.5(5) . . ? C2 C1 C6 119.1(10) . . ? C2 C1 N1A 120.9(9) . . ? C6 C1 N1A 119.9(9) . . ? C3 C2 C1 119.0(10) . . ? C3 C2 C7 118.6(10) . . ? C1 C2 C7 122.3(10) . . ? C4 C3 C2 122.0(11) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 118.9(11) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 121.4(10) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C1 119.0(10) . . ? C5 C6 C10 120.5(10) . . ? C1 C6 C10 120.5(9) . . ? C9 C7 C8 110.7(9) . . ? C9 C7 C2 111.6(10) . . ? C8 C7 C2 112.4(9) . . ? C9 C7 H7 107.3 . . ? C8 C7 H7 107.3 . . ? C2 C7 H7 107.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 111.0(11) . . ? C12 C10 C6 113.5(10) . . ? C11 C10 C6 108.3(10) . . ? C12 C10 H10 108.0 . . ? C11 C10 H10 108.0 . . ? C6 C10 H10 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1A C13 H13A 109.5 . . ? Si1A C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1A C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1A C14 H14A 109.5 . . ? Si1A C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1A C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P1A C15 Si1A 109.8(6) . . ? P1A C15 H15A 109.7 . . ? Si1A C15 H15A 109.7 . . ? P1A C15 H15B 109.7 . . ? Si1A C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C21 118.8(10) . . ? C17 C16 P1A 120.3(9) . . ? C21 C16 P1A 120.9(8) . . ? C18 C17 C16 123.1(11) . . ? C18 C17 H17 118.5 . . ? C16 C17 H17 118.5 . . ? C17 C18 C19 118.3(11) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C18 C19 C20 120.0(11) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 121.5(11) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C16 118.4(10) . . ? C20 C21 P2A 121.7(9) . . ? C16 C21 P2A 119.9(8) . . ? C27 C22 C23 117.9(11) . . ? C27 C22 P2A 119.8(9) . . ? C23 C22 P2A 122.1(9) . . ? C24 C23 C22 125.2(13) . . ? C24 C23 H23 117.4 . . ? C22 C23 H23 117.4 . . ? C25 C24 C23 106.8(14) . . ? C25 C24 H24 126.6 . . ? C23 C24 H24 126.6 . . ? C24 C25 C26 136.1(14) . . ? C24 C25 H25 111.9 . . ? C26 C25 H25 111.9 . . ? C25 C26 C27 109.8(12) . . ? C25 C26 H26 125.1 . . ? C27 C26 H26 125.1 . . ? C26 C27 C22 121.9(13) . . ? C26 C27 H27 119.0 . . ? C22 C27 H27 119.0 . . ? C29 C28 C33 118.5(11) . . ? C29 C28 P2A 122.5(9) . . ? C33 C28 P2A 119.0(9) . . ? C30 C29 C28 121.2(13) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 119.5(13) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 118.9(12) . . ? C32 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? C31 C32 C33 121.9(13) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C32 C33 C28 119.9(12) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C35 C34 C39 119.6(11) . . ? C35 C34 P1A 121.6(9) . . ? C39 C34 P1A 118.8(9) . . ? C34 C35 C36 119.0(13) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C37 C36 C35 121.3(14) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C36 C37 C38 120.0(13) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 121.5(14) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C38 C39 C34 118.5(12) . . ? C38 C39 P3A 124.4(11) . . ? C34 C39 P3A 117.0(9) . . ? C45 C40 C41 116.9(13) . . ? C45 C40 P3A 119.4(11) . . ? C41 C40 P3A 123.3(11) . . ? C40 C41 C42 120.7(15) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C43 C42 C41 119.5(16) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C42 C43 C44 121.2(14) . . ? C42 C43 H43 119.4 . . ? C44 C43 H43 119.4 . . ? C45 C44 C43 119.4(15) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C44 C45 C40 122.1(15) . . ? C44 C45 H45 118.9 . . ? C40 C45 H45 118.9 . . ? C47 C46 C51 118.1(13) . . ? C47 C46 P3A 125.8(11) . . ? C51 C46 P3A 116.1(10) . . ? C46 C47 C48 119.5(15) . . ? C46 C47 H47 120.3 . . ? C48 C47 H47 120.2 . . ? C49 C48 C47 122.4(16) . . ? C49 C48 H48 118.8 . . ? C47 C48 H48 118.8 . . ? C48 C49 C50 119.5(15) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C49 C50 C51 118.9(17) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C46 C51 C50 120.7(16) . . ? C46 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C56 C52 C53 129(3) . . ? C56 C52 H52A 105.2 . . ? C53 C52 H52A 105.2 . . ? C56 C52 H52B 105.2 . . ? C53 C52 H52B 105.2 . . ? H52A C52 H52B 105.9 . . ? C52 C53 C54 97(3) . . ? C52 C53 H53A 112.3 . . ? C54 C53 H53A 112.3 . . ? C52 C53 H53B 112.3 . . ? C54 C53 H53B 112.3 . . ? H53A C53 H53B 109.9 . . ? C55 C54 C53 104(2) . . ? C55 C54 H54A 110.9 . . ? C53 C54 H54A 110.9 . . ? C55 C54 H54B 110.9 . . ? C53 C54 H54B 110.9 . . ? H54A C54 H54B 108.9 . . ? C54 C55 C56 102(2) . . ? C54 C55 H55A 111.3 . . ? C56 C55 H55A 111.3 . . ? C54 C55 H55B 111.3 . . ? C56 C55 H55B 111.3 . . ? H55A C55 H55B 109.2 . . ? C52 C56 C55 88(2) . . ? C52 C56 H56A 114.1 . . ? C55 C56 H56A 114.1 . . ? C52 C56 H56B 114.1 . . ? C55 C56 H56B 114.1 . . ? H56A C56 H56B 111.2 . . ? C62 C57 C58 123(3) . . ? C62 C57 H57 118.3 . . ? C58 C57 H57 118.3 . . ? C59 C58 C57 123(2) . . ? C59 C58 H58 118.7 . . ? C57 C58 H58 118.7 . . ? C58 C59 C60 120(2) . . ? C58 C59 H59 120.1 . . ? C60 C59 H59 120.1 . . ? C59 C60 C61 115(3) . . ? C59 C60 H60 122.7 . . ? C61 C60 H60 122.7 . . ? C62 C61 C60 127(3) . . ? C62 C61 H61 116.6 . . ? C60 C61 H61 116.6 . . ? C57 C62 C61 112(2) . . ? C57 C62 H62 124.1 . . ? C61 C62 H62 124.1 . . ? N1B C63 C64 121.6(9) . . ? N1B C63 C68 119.4(9) . . ? C64 C63 C68 118.9(9) . . ? C65 C64 C63 120.1(10) . . ? C65 C64 C69 118.4(9) . . ? C63 C64 C69 121.5(9) . . ? C64 C65 C66 120.9(10) . . ? C64 C65 H65 119.6 . . ? C66 C65 H65 119.6 . . ? C67 C66 C65 119.3(10) . . ? C67 C66 H66 120.3 . . ? C65 C66 H66 120.3 . . ? C66 C67 C68 122.7(10) . . ? C66 C67 H67 118.7 . . ? C68 C67 H67 118.7 . . ? C67 C68 C63 117.7(10) . . ? C67 C68 C72 119.5(10) . . ? C63 C68 C72 122.8(10) . . ? C71 C69 C64 114.3(10) . . ? C71 C69 C70 112.6(11) . . ? C64 C69 C70 107.5(10) . . ? C71 C69 H69 107.4 . . ? C64 C69 H69 107.4 . . ? C70 C69 H69 107.4 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73 C72 C68 113.2(9) . . ? C73 C72 C74 111.0(10) . . ? C68 C72 C74 110.2(10) . . ? C73 C72 H72 107.4 . . ? C68 C72 H72 107.4 . . ? C74 C72 H72 107.4 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? Si1B C75 H75A 109.5 . . ? Si1B C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? Si1B C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? Si1B C76 H76A 109.5 . . ? Si1B C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? Si1B C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? P1B C77 Si1B 109.7(6) . . ? P1B C77 H77A 109.7 . . ? Si1B C77 H77A 109.7 . . ? P1B C77 H77B 109.7 . . ? Si1B C77 H77B 109.7 . . ? H77A C77 H77B 108.2 . . ? C79 C78 C83 119.3(10) . . ? C79 C78 P1B 119.4(8) . . ? C83 C78 P1B 121.3(8) . . ? C78 C79 C80 121.7(11) . . ? C78 C79 H79 119.1 . . ? C80 C79 H79 119.1 . . ? C81 C80 C79 119.3(11) . . ? C81 C80 H80 120.3 . . ? C79 C80 H80 120.3 . . ? C80 C81 C82 119.7(10) . . ? C80 C81 H81 120.1 . . ? C82 C81 H81 120.1 . . ? C83 C82 C81 120.8(10) . . ? C83 C82 H82 119.6 . . ? C81 C82 H82 119.6 . . ? C82 C83 C78 119.2(10) . . ? C82 C83 P2B 121.5(8) . . ? C78 C83 P2B 119.4(8) . . ? C85 C84 C89 119.8(12) . . ? C85 C84 P2B 123.0(9) . . ? C89 C84 P2B 117.0(10) . . ? C84 C85 C86 122.5(13) . . ? C84 C85 H85 118.8 . . ? C86 C85 H85 118.7 . . ? C87 C86 C85 112.3(14) . . ? C87 C86 H86 123.9 . . ? C85 C86 H86 123.9 . . ? C86 C87 C88 129.3(14) . . ? C86 C87 H87 115.3 . . ? C88 C87 H87 115.3 . . ? C89 C88 C87 114.7(14) . . ? C89 C88 H88 122.7 . . ? C87 C88 H88 122.7 . . ? C88 C89 C84 120.9(13) . . ? C88 C89 H89 119.6 . . ? C84 C89 H89 119.6 . . ? C91 C90 C95 119.9(11) . . ? C91 C90 P2B 119.0(9) . . ? C95 C90 P2B 121.0(9) . . ? C90 C91 C92 119.5(12) . . ? C90 C91 H91 120.2 . . ? C92 C91 H91 120.2 . . ? C93 C92 C91 120.9(13) . . ? C93 C92 H92 119.5 . . ? C91 C92 H92 119.5 . . ? C92 C93 C94 121.1(13) . . ? C92 C93 H93 119.5 . . ? C94 C93 H93 119.5 . . ? C93 C94 C95 120.4(12) . . ? C93 C94 H94 119.8 . . ? C95 C94 H94 119.8 . . ? C94 C95 C90 118.1(11) . . ? C94 C95 H95 121.0 . . ? C90 C95 H95 121.0 . . ? C97 C96 C101 118.9(11) . . ? C97 C96 P1B 121.4(10) . . ? C101 C96 P1B 119.7(9) . . ? C98 C97 C96 121.4(14) . . ? C98 C97 H97 119.3 . . ? C96 C97 H97 119.3 . . ? C99 C98 C97 120.8(14) . . ? C99 C98 H98 119.6 . . ? C97 C98 H98 119.6 . . ? C98 C99 C100 119.4(12) . . ? C98 C99 H99 120.3 . . ? C100 C99 H99 120.3 . . ? C101 C100 C99 121.1(14) . . ? C101 C100 H100 119.4 . . ? C99 C100 H100 119.4 . . ? C100 C101 C96 118.1(12) . . ? C100 C101 P3B 124.5(11) . . ? C96 C101 P3B 117.3(8) . . ? C107 C102 C103 118.4(13) . . ? C107 C102 P3B 117.8(11) . . ? C103 C102 P3B 123.4(10) . . ? C102 C103 C104 120.7(13) . . ? C102 C103 H103 119.6 . . ? C104 C103 H103 119.6 . . ? C105 C104 C103 120.4(14) . . ? C105 C104 H104 119.8 . . ? C103 C104 H104 119.8 . . ? C106 C105 C104 118.4(14) . . ? C106 C105 H105 120.8 . . ? C104 C105 H105 120.8 . . ? C105 C106 C107 121.0(14) . . ? C105 C106 H106 119.5 . . ? C107 C106 H106 119.5 . . ? C102 C107 C106 120.9(14) . . ? C102 C107 H107 119.5 . . ? C106 C107 H107 119.5 . . ? C113 C108 C109 114.5(17) . . ? C113 C108 P3B 119.9(12) . . ? C109 C108 P3B 125.6(16) . . ? C108 C109 C110 120(3) . . ? C108 C109 H109 120.2 . . ? C110 C109 H109 120.2 . . ? C111 C110 C109 125(3) . . ? C111 C110 H110 117.5 . . ? C109 C110 H110 117.5 . . ? C112 C111 C110 114(2) . . ? C112 C111 H111 122.8 . . ? C110 C111 H111 122.8 . . ? C111 C112 C113 123.9(19) . . ? C111 C112 H112 118.0 . . ? C113 C112 H112 118.0 . . ? C108 C113 C112 122.1(17) . . ? C108 C113 H113 118.9 . . ? C112 C113 H113 118.9 . . ? _diffrn_measured_fraction_theta_max 0.799 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.799 _refine_diff_density_max 4.787 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.194 #===END data_mtw07 _database_code_depnum_ccdc_archive 'CCDC 289251' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H50 Cl Fe N P2 Si' _chemical_formula_weight 786.19 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 9.793(3) _cell_length_b 9.371(3) _cell_length_c 44.610(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.581(4) _cell_angle_gamma 90.00 _cell_volume 4080.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5083 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.575 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34419 _diffrn_reflns_av_R_equivalents 0.0769 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.24 _reflns_number_total 8533 _reflns_number_gt 6076 _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^)+(0.0000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8533 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0682 _refine_ls_goodness_of_fit_ref 1.305 _refine_ls_restrained_S_all 1.305 _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 Fe Fe 0.30973(3) 0.21878(3) 0.139802(7) 0.01435(9) Uani 1 1 d . . . Cl Cl 0.20090(6) 0.03080(6) 0.157867(14) 0.02465(16) Uani 1 1 d . . . P1 P 0.17654(6) 0.42803(6) 0.124959(14) 0.01513(15) Uani 1 1 d . . . P2 P 0.45882(6) 0.34342(6) 0.179380(14) 0.01483(15) Uani 1 1 d . . . N N 0.43716(17) 0.26402(18) 0.10965(4) 0.0150(4) Uani 1 1 d . . . Si Si 0.48119(6) 0.44055(6) 0.115263(15) 0.01521(16) Uani 1 1 d . . . C1 C 0.4928(2) 0.1715(2) 0.08842(5) 0.0133(5) Uani 1 1 d . . . C2 C 0.5800(2) 0.0563(2) 0.09829(5) 0.0146(5) Uani 1 1 d . . . C3 C 0.6357(2) -0.0293(2) 0.07674(5) 0.0168(5) Uani 1 1 d . . . H3 H 0.6935 -0.1064 0.0833 0.020 Uiso 1 1 calc R . . C4 C 0.6098(2) -0.0061(2) 0.04635(5) 0.0186(6) Uani 1 1 d . . . H4 H 0.6515 -0.0641 0.0322 0.022 Uiso 1 1 calc R . . C5 C 0.5218(2) 0.1032(2) 0.03678(5) 0.0183(6) Uani 1 1 d . . . H5 H 0.5021 0.1187 0.0158 0.022 Uiso 1 1 calc R . . C6 C 0.4615(2) 0.1910(2) 0.05714(5) 0.0152(5) Uani 1 1 d . . . C7 C 0.6138(2) 0.0264(2) 0.13134(5) 0.0166(5) Uani 1 1 d . . . H7 H 0.5517 0.0864 0.1429 0.020 Uiso 1 1 calc R . . C8 C 0.5901(3) -0.1304(2) 0.13972(6) 0.0333(7) Uani 1 1 d . . . H8A H 0.4960 -0.1579 0.1330 0.050 Uiso 1 1 calc R . . H8B H 0.6047 -0.1418 0.1616 0.050 Uiso 1 1 calc R . . H8C H 0.6545 -0.1914 0.1299 0.050 Uiso 1 1 calc R . . C9 C 0.7621(2) 0.0704(3) 0.14107(6) 0.0276(6) Uani 1 1 d . . . H9A H 0.8254 0.0144 0.1298 0.041 Uiso 1 1 calc R . . H9B H 0.7812 0.0528 0.1627 0.041 Uiso 1 1 calc R . . H9C H 0.7742 0.1722 0.1369 0.041 Uiso 1 1 calc R . . C10 C 0.3546(2) 0.3000(2) 0.04490(5) 0.0188(6) Uani 1 1 d . . . H10 H 0.3377 0.3674 0.0616 0.023 Uiso 1 1 calc R . . C11 C 0.2192(2) 0.2255(2) 0.03531(6) 0.0247(6) Uani 1 1 d . . . H11A H 0.1514 0.2967 0.0279 0.037 Uiso 1 1 calc R . . H11B H 0.1861 0.1752 0.0526 0.037 Uiso 1 1 calc R . . H11C H 0.2335 0.1568 0.0193 0.037 Uiso 1 1 calc R . . C12 C 0.4003(3) 0.3882(3) 0.01861(6) 0.0307(7) Uani 1 1 d . . . H12A H 0.4052 0.3266 0.0010 0.046 Uiso 1 1 calc R . . H12B H 0.4908 0.4294 0.0242 0.046 Uiso 1 1 calc R . . H12C H 0.3342 0.4650 0.0139 0.046 Uiso 1 1 calc R . . C13 C 0.6007(2) 0.5189(2) 0.08944(5) 0.0212(6) Uani 1 1 d . . . H13A H 0.6901 0.4721 0.0926 0.032 Uiso 1 1 calc R . . H13B H 0.6110 0.6213 0.0935 0.032 Uiso 1 1 calc R . . H13C H 0.5639 0.5047 0.0686 0.032 Uiso 1 1 calc R . . C14 C 0.5641(2) 0.4487(2) 0.15504(5) 0.0173(6) Uani 1 1 d . . . H14A H 0.6580 0.4092 0.1558 0.021 Uiso 1 1 calc R . . H14B H 0.5698 0.5490 0.1620 0.021 Uiso 1 1 calc R . . C15 C 0.3145(2) 0.5461(2) 0.11389(5) 0.0164(5) Uani 1 1 d . . . H15A H 0.3248 0.6285 0.1278 0.020 Uiso 1 1 calc R . . H15B H 0.2916 0.5828 0.0933 0.020 Uiso 1 1 calc R . . C16 C 0.5759(2) 0.2224(2) 0.20077(5) 0.0154(5) Uani 1 1 d . . . C17 C 0.5327(2) 0.0844(2) 0.20660(5) 0.0191(6) Uani 1 1 d . . . H17 H 0.4421 0.0557 0.2001 0.023 Uiso 1 1 calc R . . C18 C 0.6210(2) -0.0117(2) 0.22189(5) 0.0220(6) Uani 1 1 d . . . H18 H 0.5908 -0.1057 0.2258 0.026 Uiso 1 1 calc R . . C19 C 0.7533(2) 0.0300(3) 0.23140(5) 0.0226(6) Uani 1 1 d . . . H19 H 0.8143 -0.0361 0.2416 0.027 Uiso 1 1 calc R . . C20 C 0.7965(2) 0.1672(3) 0.22608(5) 0.0233(6) Uani 1 1 d . . . H20 H 0.8867 0.1960 0.2330 0.028 Uiso 1 1 calc R . . C21 C 0.7090(2) 0.2632(2) 0.21077(5) 0.0196(6) Uani 1 1 d . . . H21 H 0.7396 0.3572 0.2070 0.023 Uiso 1 1 calc R . . C22 C 0.4116(2) 0.4694(2) 0.20820(5) 0.0146(5) Uani 1 1 d . . . C23 C 0.4063(2) 0.4257(2) 0.23799(5) 0.0171(5) Uani 1 1 d . . . H23 H 0.4299 0.3303 0.2434 0.021 Uiso 1 1 calc R . . C24 C 0.3670(2) 0.5193(3) 0.25980(5) 0.0213(6) Uani 1 1 d . . . H24 H 0.3652 0.4883 0.2800 0.026 Uiso 1 1 calc R . . C25 C 0.3303(2) 0.6585(3) 0.25207(6) 0.0231(6) Uani 1 1 d . . . H25 H 0.3034 0.7230 0.2669 0.028 Uiso 1 1 calc R . . C26 C 0.3333(2) 0.7021(3) 0.22255(6) 0.0236(6) Uani 1 1 d . . . H26 H 0.3073 0.7969 0.2172 0.028 Uiso 1 1 calc R . . C27 C 0.3739(2) 0.6093(2) 0.20066(5) 0.0187(6) Uani 1 1 d . . . H27 H 0.3760 0.6412 0.1805 0.022 Uiso 1 1 calc R . . C28 C 0.0865(2) 0.5219(2) 0.15341(5) 0.0157(5) Uani 1 1 d . . . C29 C 0.0596(2) 0.4466(2) 0.17916(5) 0.0200(6) Uani 1 1 d . . . H29 H 0.0866 0.3495 0.1812 0.024 Uiso 1 1 calc R . . C30 C -0.0061(2) 0.5114(3) 0.20192(6) 0.0249(6) Uani 1 1 d . . . H30 H -0.0231 0.4593 0.2195 0.030 Uiso 1 1 calc R . . C31 C -0.0472(2) 0.6528(3) 0.19895(6) 0.0257(6) Uani 1 1 d . . . H31 H -0.0932 0.6974 0.2144 0.031 Uiso 1 1 calc R . . C32 C -0.0210(2) 0.7287(3) 0.17341(6) 0.0271(6) Uani 1 1 d . . . H32 H -0.0490 0.8255 0.1714 0.033 Uiso 1 1 calc R . . C33 C 0.0460(2) 0.6641(2) 0.15076(6) 0.0223(6) Uani 1 1 d . . . H33 H 0.0643 0.7171 0.1334 0.027 Uiso 1 1 calc R . . C34 C 0.0511(2) 0.4165(2) 0.09240(5) 0.0152(5) Uani 1 1 d . . . C35 C 0.0294(2) 0.5216(2) 0.07060(5) 0.0200(6) Uani 1 1 d . . . H35 H 0.0820 0.6068 0.0721 0.024 Uiso 1 1 calc R . . C36 C -0.0688(2) 0.5034(3) 0.04661(6) 0.0231(6) Uani 1 1 d . . . H36 H -0.0820 0.5753 0.0316 0.028 Uiso 1 1 calc R . . C37 C -0.1465(2) 0.3810(2) 0.04459(6) 0.0213(6) Uani 1 1 d . . . H37 H -0.2141 0.3690 0.0283 0.026 Uiso 1 1 calc R . . C38 C -0.1271(2) 0.2760(3) 0.06605(6) 0.0228(6) Uani 1 1 d . . . H38 H -0.1814 0.1919 0.0646 0.027 Uiso 1 1 calc R . . C39 C -0.0282(2) 0.2927(2) 0.08988(5) 0.0198(6) Uani 1 1 d . . . H39 H -0.0145 0.2195 0.1045 0.024 Uiso 1 1 calc R . . C40 C 0.1966(3) 0.8913(2) 0.08114(6) 0.0277(6) Uani 1 1 d . . . H40 H 0.2328 0.9054 0.1013 0.033 Uiso 1 1 calc R . . C41 C 0.0586(3) 0.9144(2) 0.07317(6) 0.0309(7) Uani 1 1 d . . . H41 H -0.0003 0.9443 0.0879 0.037 Uiso 1 1 calc R . . C42 C 0.0068(3) 0.8936(2) 0.04372(7) 0.0295(7) Uani 1 1 d . . . H42 H -0.0877 0.9099 0.0383 0.035 Uiso 1 1 calc R . . C43 C 0.0906(3) 0.8498(2) 0.02234(6) 0.0258(6) Uani 1 1 d . . . H43 H 0.0545 0.8353 0.0022 0.031 Uiso 1 1 calc R . . C44 C 0.2282(2) 0.8270(2) 0.03040(6) 0.0231(6) Uani 1 1 d . . . H44 H 0.2869 0.7966 0.0157 0.028 Uiso 1 1 calc R . . C45 C 0.2807(2) 0.8479(2) 0.05958(6) 0.0240(6) Uani 1 1 d . . . H45 H 0.3754 0.8323 0.0649 0.029 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.01616(18) 0.01379(17) 0.0134(2) 0.00133(16) 0.00311(14) -0.00114(15) Cl 0.0312(4) 0.0226(3) 0.0203(4) 0.0031(3) 0.0033(3) -0.0105(3) P1 0.0154(3) 0.0144(3) 0.0157(4) 0.0010(3) 0.0019(3) 0.0000(3) P2 0.0151(3) 0.0154(3) 0.0141(4) 0.0003(3) 0.0014(3) -0.0001(3) N 0.0164(10) 0.0125(10) 0.0165(11) -0.0008(8) 0.0038(8) -0.0009(8) Si 0.0178(4) 0.0133(3) 0.0149(4) 0.0002(3) 0.0038(3) -0.0010(3) C1 0.0109(12) 0.0136(12) 0.0158(15) -0.0017(10) 0.0035(10) -0.0073(10) C2 0.0116(12) 0.0157(12) 0.0169(15) -0.0015(11) 0.0034(10) -0.0044(10) C3 0.0131(13) 0.0161(12) 0.0211(16) -0.0022(11) 0.0004(11) -0.0003(10) C4 0.0150(13) 0.0231(14) 0.0182(16) -0.0103(12) 0.0037(11) -0.0042(11) C5 0.0172(13) 0.0228(13) 0.0149(14) -0.0024(11) 0.0019(11) -0.0071(11) C6 0.0156(13) 0.0143(12) 0.0160(15) 0.0005(11) 0.0035(11) -0.0057(10) C7 0.0196(13) 0.0155(12) 0.0147(15) -0.0010(11) 0.0020(11) 0.0024(10) C8 0.0499(18) 0.0251(15) 0.0248(17) 0.0054(12) 0.0025(14) -0.0076(13) C9 0.0250(15) 0.0336(15) 0.0244(16) 0.0014(13) 0.0023(12) 0.0026(12) C10 0.0226(14) 0.0186(13) 0.0154(14) -0.0011(11) 0.0019(11) -0.0011(11) C11 0.0197(13) 0.0231(13) 0.0308(16) -0.0007(12) -0.0007(12) 0.0019(11) C12 0.0336(16) 0.0296(15) 0.0286(17) 0.0104(13) 0.0014(13) -0.0040(12) C13 0.0237(14) 0.0186(13) 0.0220(16) 0.0000(11) 0.0060(12) -0.0026(11) C14 0.0142(13) 0.0147(13) 0.0236(15) -0.0004(11) 0.0052(11) -0.0008(10) C15 0.0214(13) 0.0135(12) 0.0143(14) 0.0000(10) 0.0000(11) -0.0024(10) C16 0.0153(12) 0.0187(12) 0.0123(14) -0.0033(11) 0.0015(10) 0.0030(10) C17 0.0204(14) 0.0218(13) 0.0153(15) -0.0002(11) 0.0019(11) -0.0009(11) C18 0.0299(15) 0.0181(13) 0.0185(15) 0.0041(11) 0.0043(12) 0.0020(11) C19 0.0209(14) 0.0281(15) 0.0185(15) 0.0025(12) -0.0012(12) 0.0094(11) C20 0.0163(13) 0.0301(15) 0.0225(16) -0.0026(12) -0.0042(12) 0.0019(11) C21 0.0234(14) 0.0165(13) 0.0186(15) -0.0043(11) -0.0002(11) -0.0019(11) C22 0.0103(12) 0.0166(12) 0.0164(15) -0.0028(11) -0.0013(10) -0.0015(10) C23 0.0132(13) 0.0180(13) 0.0199(15) -0.0005(11) -0.0007(11) -0.0028(10) C24 0.0191(14) 0.0295(15) 0.0155(15) -0.0025(12) 0.0020(11) -0.0048(11) C25 0.0150(13) 0.0299(15) 0.0246(17) -0.0135(13) 0.0030(12) 0.0003(11) C26 0.0172(13) 0.0219(14) 0.0308(18) -0.0045(13) -0.0032(12) 0.0021(11) C27 0.0168(13) 0.0228(14) 0.0161(15) -0.0030(11) -0.0015(11) -0.0004(10) C28 0.0139(13) 0.0172(13) 0.0161(15) -0.0006(11) 0.0013(11) -0.0024(10) C29 0.0209(14) 0.0184(13) 0.0208(15) -0.0007(12) 0.0016(12) -0.0014(11) C30 0.0230(15) 0.0320(16) 0.0204(16) 0.0006(12) 0.0061(12) -0.0067(12) C31 0.0193(14) 0.0326(15) 0.0261(17) -0.0116(13) 0.0075(12) -0.0009(12) C32 0.0272(15) 0.0187(13) 0.0359(18) -0.0035(13) 0.0055(13) 0.0034(11) C33 0.0241(14) 0.0213(14) 0.0220(16) 0.0027(11) 0.0040(12) 0.0024(11) C34 0.0140(13) 0.0153(12) 0.0166(14) -0.0020(11) 0.0034(10) 0.0007(10) C35 0.0217(14) 0.0142(13) 0.0237(16) 0.0002(11) -0.0009(12) -0.0034(10) C36 0.0257(14) 0.0239(14) 0.0190(16) 0.0052(11) -0.0021(12) 0.0029(11) C37 0.0149(13) 0.0277(15) 0.0205(16) -0.0067(12) -0.0039(11) 0.0032(11) C38 0.0175(13) 0.0193(13) 0.0317(17) -0.0067(13) 0.0023(12) -0.0042(11) C39 0.0205(13) 0.0164(13) 0.0227(15) 0.0016(11) 0.0028(12) 0.0000(11) C40 0.0464(19) 0.0157(14) 0.0201(16) 0.0014(12) -0.0020(14) -0.0086(12) C41 0.0464(19) 0.0139(13) 0.035(2) 0.0034(13) 0.0213(15) 0.0023(12) C42 0.0191(14) 0.0224(14) 0.046(2) 0.0099(14) -0.0022(14) 0.0012(11) C43 0.0322(16) 0.0241(14) 0.0202(16) 0.0009(12) -0.0034(13) -0.0053(12) C44 0.0229(15) 0.0222(14) 0.0253(17) -0.0003(12) 0.0084(13) -0.0035(11) C45 0.0186(14) 0.0176(13) 0.0351(19) 0.0043(12) -0.0021(13) -0.0045(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 Fe N 1.9532(17) . ? Fe Cl 2.2418(8) . ? Fe P1 2.4180(8) . ? Fe P2 2.4903(8) . ? P1 C28 1.828(2) . ? P1 C34 1.829(2) . ? P1 C15 1.844(2) . ? P2 C16 1.827(2) . ? P2 C22 1.832(2) . ? P2 C14 1.842(2) . ? N C1 1.424(3) . ? N Si 1.7228(19) . ? Si C13 1.858(2) . ? Si C14 1.893(2) . ? Si C15 1.906(2) . ? C1 C6 1.416(3) . ? C1 C2 1.425(3) . ? C2 C3 1.396(3) . ? C2 C7 1.511(3) . ? C3 C4 1.376(3) . ? C3 H3 0.9500 . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 C6 1.391(3) . ? C5 H5 0.9500 . ? C6 C10 1.532(3) . ? C7 C8 1.538(3) . ? C7 C9 1.539(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.529(3) . ? C10 C12 1.531(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.392(3) . ? C16 C21 1.397(3) . ? C17 C18 1.389(3) . ? C17 H17 0.9500 . ? C18 C19 1.387(3) . ? C18 H18 0.9500 . ? C19 C20 1.381(3) . ? C19 H19 0.9500 . ? C20 C21 1.384(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.396(3) . ? C22 C27 1.396(3) . ? C23 C24 1.387(3) . ? C23 H23 0.9500 . ? C24 C25 1.388(3) . ? C24 H24 0.9500 . ? C25 C26 1.381(3) . ? C25 H25 0.9500 . ? C26 C27 1.389(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.391(3) . ? C28 C33 1.393(3) . ? C29 C30 1.385(3) . ? C29 H29 0.9500 . ? C30 C31 1.387(3) . ? C30 H30 0.9500 . ? C31 C32 1.385(3) . ? C31 H31 0.9500 . ? C32 C33 1.387(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.389(3) . ? C34 C39 1.396(3) . ? C35 C36 1.391(3) . ? C35 H35 0.9500 . ? C36 C37 1.376(3) . ? C36 H36 0.9500 . ? C37 C38 1.376(3) . ? C37 H37 0.9500 . ? C38 C39 1.389(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.377(3) . ? C40 C41 1.387(4) . ? C40 H40 0.9500 . ? C41 C42 1.384(4) . ? C41 H41 0.9500 . ? C42 C43 1.370(3) . ? C42 H42 0.9500 . ? C43 C44 1.384(3) . ? C43 H43 0.9500 . ? C44 C45 1.375(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? 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 N Fe Cl 140.03(6) . . ? N Fe P1 89.76(5) . . ? Cl Fe P1 118.30(3) . . ? N Fe P2 90.91(6) . . ? Cl Fe P2 112.48(3) . . ? P1 Fe P2 94.98(3) . . ? C28 P1 C34 104.45(10) . . ? C28 P1 C15 107.54(10) . . ? C34 P1 C15 106.43(10) . . ? C28 P1 Fe 118.67(8) . . ? C34 P1 Fe 118.87(7) . . ? C15 P1 Fe 99.74(7) . . ? C16 P2 C22 102.51(10) . . ? C16 P2 C14 106.42(10) . . ? C22 P2 C14 104.64(10) . . ? C16 P2 Fe 112.78(8) . . ? C22 P2 Fe 129.31(7) . . ? C14 P2 Fe 99.05(8) . . ? C1 N Si 125.21(14) . . ? C1 N Fe 128.71(14) . . ? Si N Fe 105.93(9) . . ? N Si C13 116.88(10) . . ? N Si C14 105.00(9) . . ? C13 Si C14 108.73(10) . . ? N Si C15 106.84(9) . . ? C13 Si C15 110.82(10) . . ? C14 Si C15 108.14(10) . . ? C6 C1 N 120.85(19) . . ? C6 C1 C2 118.7(2) . . ? N C1 C2 120.5(2) . . ? C3 C2 C1 118.7(2) . . ? C3 C2 C7 119.9(2) . . ? C1 C2 C7 121.4(2) . . ? C4 C3 C2 122.4(2) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C4 C5 C6 121.5(2) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.8(2) . . ? C5 C6 C10 118.4(2) . . ? C1 C6 C10 121.7(2) . . ? C2 C7 C8 112.87(19) . . ? C2 C7 C9 110.70(18) . . ? C8 C7 C9 110.18(19) . . ? C2 C7 H7 107.6 . . ? C8 C7 H7 107.6 . . ? C9 C7 H7 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 109.4(2) . . ? C11 C10 C6 110.38(18) . . ? C12 C10 C6 113.55(19) . . ? C11 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C6 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si C13 H13A 109.5 . . ? Si C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C14 Si 108.21(11) . . ? P2 C14 H14A 110.1 . . ? Si C14 H14A 110.1 . . ? P2 C14 H14B 110.1 . . ? Si C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? P1 C15 Si 108.92(11) . . ? P1 C15 H15A 109.9 . . ? Si C15 H15A 109.9 . . ? P1 C15 H15B 109.9 . . ? Si C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C17 C16 C21 119.0(2) . . ? C17 C16 P2 119.12(17) . . ? C21 C16 P2 121.87(17) . . ? C18 C17 C16 120.5(2) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 119.8(2) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C18 120.1(2) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.2(2) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 120.3(2) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? C23 C22 C27 118.4(2) . . ? C23 C22 P2 120.66(17) . . ? C27 C22 P2 120.85(18) . . ? C24 C23 C22 121.1(2) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 120.0(2) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 119.3(2) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 120.9(2) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C22 120.2(2) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C29 C28 C33 119.0(2) . . ? C29 C28 P1 117.57(17) . . ? C33 C28 P1 123.46(18) . . ? C30 C29 C28 120.8(2) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 119.8(2) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 119.8(2) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 120.3(2) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C32 C33 C28 120.2(2) . . ? C32 C33 H33 119.9 . . ? C28 C33 H33 119.9 . . ? C35 C34 C39 118.7(2) . . ? C35 C34 P1 124.73(17) . . ? C39 C34 P1 116.59(18) . . ? C34 C35 C36 120.6(2) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C37 C36 C35 119.8(2) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C38 C37 C36 120.4(2) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 120.1(2) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C34 120.3(2) . . ? C38 C39 H39 119.8 . . ? C34 C39 H39 119.8 . . ? C45 C40 C41 119.5(2) . . ? C45 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C42 C41 C40 119.8(2) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C43 C42 C41 120.6(2) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 119.4(2) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C45 C44 C43 120.4(2) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C40 120.3(2) . . ? C44 C45 H45 119.8 . . ? C40 C45 H45 119.8 . . ? _diffrn_measured_fraction_theta_max 0.847 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.847 _refine_diff_density_max 0.794 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.074 #===END data_mtw12 _database_code_depnum_ccdc_archive 'CCDC 289252' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H54 Co I N O P2 Si' _chemical_formula_weight 876.73 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' I I -0.4742 1.8119 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.6071(8) _cell_length_b 21.6762(15) _cell_length_c 16.8895(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.988(2) _cell_angle_gamma 90.00 _cell_volume 4243.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7454 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 32.74 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 1.268 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77696 _diffrn_reflns_av_R_equivalents 0.0791 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 32.82 _reflns_number_total 14707 _reflns_number_gt 10132 _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^)+(0.0000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14707 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1074 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1290 _refine_ls_goodness_of_fit_ref 3.006 _refine_ls_restrained_S_all 3.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I I 0.92011(3) 0.201853(11) -0.119709(13) 0.05553(11) Uani 1 1 d . . . Co Co 0.81236(4) 0.232112(17) 0.00048(2) 0.02444(10) Uani 1 1 d . . . P1 P 0.87609(8) 0.32472(4) 0.06520(5) 0.02902(18) Uani 1 1 d . . . P2 P 0.86238(8) 0.16945(4) 0.11226(5) 0.02911(19) Uani 1 1 d . . . Si1 Si 0.67886(8) 0.26271(4) 0.13636(6) 0.02699(19) Uani 1 1 d . . . N N 0.6618(2) 0.24449(12) 0.03821(17) 0.0336(7) Uani 1 1 d . . . C1 C 0.5553(3) 0.23855(16) -0.0064(3) 0.0476(11) Uani 1 1 d . . . C14 C 0.7742(3) 0.33220(15) 0.14291(19) 0.0340(7) Uani 1 1 d . . . H14A H 0.7278 0.3703 0.1351 0.041 Uiso 1 1 calc R . . H14B H 0.8157 0.3342 0.1956 0.041 Uiso 1 1 calc R . . C2 C 0.5035(4) 0.29049(17) -0.0441(2) 0.0465(10) Uani 1 1 d . . . C20 C 0.9114(5) 0.44671(18) -0.1156(3) 0.0627(14) Uani 1 1 d . . . H20 H 0.9425 0.4453 -0.1665 0.075 Uiso 1 1 calc R . . C16 C 0.8678(3) 0.39513(15) 0.0062(2) 0.0351(8) Uani 1 1 d . . . C34 C 0.8376(3) 0.08664(15) 0.1047(2) 0.0367(8) Uani 1 1 d . . . C28 C 1.0077(3) 0.17101(16) 0.1570(2) 0.0375(8) Uani 1 1 d . . . C15 C 0.7640(4) 0.19789(17) 0.1851(2) 0.0524(12) Uani 1 1 d . . . H15A H 0.8080 0.2130 0.2331 0.063 Uiso 1 1 calc R . . H15B H 0.7117 0.1645 0.2009 0.063 Uiso 1 1 calc R . . C21 C 0.9083(4) 0.39332(17) -0.0695(2) 0.0493(10) Uani 1 1 d . . . H21 H 0.9342 0.3553 -0.0903 0.059 Uiso 1 1 calc R . . C29 C 1.0324(4) 0.17105(16) 0.2384(2) 0.0477(11) Uani 1 1 d . . . H29 H 0.9712 0.1716 0.2736 0.057 Uiso 1 1 calc R . . C17 C 0.8271(3) 0.45106(16) 0.0347(2) 0.0401(8) Uani 1 1 d . . . H17 H 0.7984 0.4533 0.0863 0.048 Uiso 1 1 calc R . . C22 C 1.0213(3) 0.33144(14) 0.1104(2) 0.0330(7) Uani 1 1 d . . . C7 C 0.5636(4) 0.3523(2) -0.0453(3) 0.0572(12) Uani 1 1 d . . . H7 H 0.6291 0.3509 -0.0045 0.069 Uiso 1 1 calc R . . C18 C 0.8285(4) 0.50301(17) -0.0121(3) 0.0494(10) Uani 1 1 d . . . H18 H 0.8007 0.5409 0.0078 0.059 Uiso 1 1 calc R . . C38 C 0.8571(4) -0.00738(18) 0.0296(3) 0.0597(13) Uani 1 1 d . . . H38 H 0.8781 -0.0278 -0.0173 0.072 Uiso 1 1 calc R . . C23 C 1.0456(3) 0.34378(13) 0.1898(2) 0.0341(8) Uani 1 1 d . . . H23 H 0.9840 0.3499 0.2238 0.041 Uiso 1 1 calc R . . C33 C 1.0983(4) 0.1729(3) 0.1070(3) 0.0735(15) Uani 1 1 d . . . H33 H 1.0832 0.1743 0.0512 0.088 Uiso 1 1 calc R . . C39 C 0.8664(3) 0.05631(16) 0.0360(3) 0.0443(9) Uani 1 1 d . . . H39 H 0.8928 0.0795 -0.0073 0.053 Uiso 1 1 calc R . . C37 C 0.8177(5) -0.0403(2) 0.0914(4) 0.0780(17) Uani 1 1 d . . . H37 H 0.8118 -0.0839 0.0873 0.094 Uiso 1 1 calc R . . C8 C 0.6146(5) 0.3637(3) -0.1252(3) 0.094(2) Uani 1 1 d . . . H8A H 0.6702 0.3310 -0.1357 0.141 Uiso 1 1 calc R . . H8B H 0.6538 0.4037 -0.1244 0.141 Uiso 1 1 calc R . . H8C H 0.5528 0.3636 -0.1670 0.141 Uiso 1 1 calc R . . C27 C 1.1145(5) 0.3226(3) 0.0617(3) 0.0787(17) Uani 1 1 d . . . H27 H 1.1003 0.3127 0.0073 0.094 Uiso 1 1 calc R . . C13 C 0.5418(4) 0.2756(2) 0.1867(3) 0.0628(13) Uani 1 1 d . . . H13A H 0.5006 0.3107 0.1623 0.094 Uiso 1 1 calc R . . H13B H 0.5593 0.2841 0.2431 0.094 Uiso 1 1 calc R . . H13C H 0.4935 0.2386 0.1814 0.094 Uiso 1 1 calc R . . C19 C 0.8696(4) 0.50117(19) -0.0873(3) 0.0566(12) Uani 1 1 d . . . H19 H 0.8689 0.5373 -0.1191 0.068 Uiso 1 1 calc R . . C30 C 1.1452(5) 0.1703(2) 0.2683(3) 0.0751(18) Uani 1 1 d . . . H30 H 1.1614 0.1698 0.3240 0.090 Uiso 1 1 calc R . . C9 C 0.4861(6) 0.4067(2) -0.0244(3) 0.0810(17) Uani 1 1 d . . . H9A H 0.4234 0.4111 -0.0652 0.122 Uiso 1 1 calc R . . H9B H 0.5319 0.4447 -0.0217 0.122 Uiso 1 1 calc R . . H9C H 0.4535 0.3992 0.0271 0.122 Uiso 1 1 calc R . . C35 C 0.7966(4) 0.05248(19) 0.1673(3) 0.0587(12) Uani 1 1 d . . . H35 H 0.7759 0.0725 0.2145 0.070 Uiso 1 1 calc R . . C6 C 0.5017(4) 0.1807(2) -0.0154(5) 0.104(3) Uani 1 1 d . . . C11 C 0.5804(6) 0.0769(2) -0.0505(7) 0.179(5) Uani 1 1 d . . . H11A H 0.6191 0.0399 -0.0289 0.269 Uiso 1 1 calc R . . H11B H 0.6289 0.0965 -0.0891 0.269 Uiso 1 1 calc R . . H11C H 0.5063 0.0652 -0.0768 0.269 Uiso 1 1 calc R . . C10 C 0.5591(6) 0.1232(2) 0.0184(7) 0.164(5) Uani 1 1 d . . . H10 H 0.6362 0.1355 0.0426 0.196 Uiso 1 1 calc R . . C5 C 0.3960(5) 0.1769(2) -0.0561(6) 0.138(4) Uani 1 1 d . . . H5 H 0.3593 0.1378 -0.0608 0.165 Uiso 1 1 calc R . . C36 C 0.7862(5) -0.0113(2) 0.1600(4) 0.0847(19) Uani 1 1 d . . . H36 H 0.7575 -0.0348 0.2020 0.102 Uiso 1 1 calc R . . C24 C 1.1591(4) 0.34733(16) 0.2207(3) 0.0498(11) Uani 1 1 d . . . H24 H 1.1741 0.3552 0.2756 0.060 Uiso 1 1 calc R . . C25 C 1.2483(5) 0.3396(2) 0.1729(4) 0.0844(19) Uani 1 1 d . . . H25 H 1.3254 0.3422 0.1945 0.101 Uiso 1 1 calc R . . C31 C 1.2330(6) 0.1702(3) 0.2186(4) 0.109(3) Uani 1 1 d . . . H31 H 1.3104 0.1684 0.2398 0.131 Uiso 1 1 calc R . . C32 C 1.2116(5) 0.1727(4) 0.1383(4) 0.119(3) Uani 1 1 d . . . H32 H 1.2738 0.1743 0.1040 0.143 Uiso 1 1 calc R . . C26 C 1.2276(5) 0.3281(3) 0.0931(5) 0.102(2) Uani 1 1 d . . . H26 H 1.2903 0.3239 0.0595 0.122 Uiso 1 1 calc R . . C12 C 0.4929(9) 0.0939(3) 0.0819(8) 0.216(8) Uani 1 1 d . . . H12A H 0.4905 0.1220 0.1272 0.324 Uiso 1 1 calc R . . H12B H 0.5307 0.0553 0.0988 0.324 Uiso 1 1 calc R . . H12C H 0.4141 0.0852 0.0613 0.324 Uiso 1 1 calc R . . C3 C 0.3965(4) 0.2832(2) -0.0847(3) 0.0656(15) Uani 1 1 d . . . H3 H 0.3607 0.3182 -0.1094 0.079 Uiso 1 1 calc R . . C4 C 0.3414(4) 0.2273(3) -0.0901(4) 0.103(3) Uani 1 1 d . . . H4 H 0.2676 0.2236 -0.1167 0.124 Uiso 1 1 calc R . . O O 0.7055(3) 0.47455(13) 0.23439(19) 0.0606(9) Uani 1 1 d . . . C43 C 0.8919(6) 0.4862(3) 0.2869(4) 0.094(2) Uani 1 1 d . . . H43A H 0.9082 0.4419 0.2860 0.141 Uiso 1 1 calc R . . H43B H 0.9242 0.5040 0.3366 0.141 Uiso 1 1 calc R . . H43C H 0.9270 0.5062 0.2420 0.141 Uiso 1 1 calc R . . C40 C 0.5106(6) 0.4633(3) 0.1967(4) 0.103(2) Uani 1 1 d . . . H40A H 0.5364 0.4513 0.1446 0.154 Uiso 1 1 calc R . . H40B H 0.4514 0.4954 0.1902 0.154 Uiso 1 1 calc R . . H40C H 0.4784 0.4273 0.2228 0.154 Uiso 1 1 calc R . . C41 C 0.5981(11) 0.4846(9) 0.2400(7) 0.303(12) Uani 1 1 d . . . H41A H 0.5899 0.5300 0.2376 0.363 Uiso 1 1 calc R . . H41B H 0.5821 0.4728 0.2950 0.363 Uiso 1 1 calc R . . C42 C 0.7868(9) 0.4945(7) 0.2820(8) 0.287(10) Uani 1 1 d . . . H42A H 0.7787 0.5400 0.2790 0.345 Uiso 1 1 calc R . . H42B H 0.7616 0.4829 0.3351 0.345 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 I 0.1109(3) 0.03979(13) 0.01742(12) -0.00429(10) 0.01829(13) 0.00696(15) Co 0.0334(2) 0.02330(18) 0.0159(2) -0.00147(15) -0.00611(16) 0.00421(17) P1 0.0422(5) 0.0296(4) 0.0160(4) -0.0060(3) 0.0078(3) -0.0071(4) P2 0.0356(5) 0.0316(4) 0.0201(4) 0.0042(3) 0.0017(3) 0.0167(4) Si1 0.0227(4) 0.0240(4) 0.0344(5) -0.0007(3) 0.0025(4) 0.0051(3) N 0.0247(14) 0.0323(13) 0.0424(17) -0.0137(12) -0.0119(12) 0.0097(11) C1 0.0282(19) 0.0433(19) 0.069(3) -0.0299(19) -0.0242(18) 0.0137(16) C14 0.044(2) 0.0394(17) 0.0194(16) -0.0058(13) 0.0090(14) -0.0084(15) C2 0.046(2) 0.050(2) 0.041(2) -0.0229(17) -0.0238(18) 0.0154(18) C20 0.109(4) 0.042(2) 0.040(2) 0.0049(18) 0.036(3) -0.009(2) C16 0.047(2) 0.0348(16) 0.0239(17) -0.0028(13) 0.0087(15) -0.0073(15) C34 0.0340(19) 0.0321(16) 0.044(2) 0.0083(15) 0.0012(16) 0.0115(14) C28 0.045(2) 0.0379(17) 0.0286(18) 0.0049(14) -0.0103(16) 0.0091(16) C15 0.079(3) 0.0429(19) 0.038(2) 0.0178(17) 0.031(2) 0.034(2) C21 0.080(3) 0.0335(17) 0.037(2) -0.0054(15) 0.027(2) -0.0085(19) C29 0.077(3) 0.0329(17) 0.031(2) 0.0050(15) -0.019(2) -0.0033(19) C17 0.052(2) 0.0405(18) 0.0284(19) -0.0028(15) 0.0070(16) -0.0008(17) C22 0.039(2) 0.0249(14) 0.0357(19) -0.0091(13) 0.0069(15) 0.0012(14) C7 0.061(3) 0.065(3) 0.042(2) 0.012(2) -0.028(2) 0.004(2) C18 0.062(3) 0.0374(19) 0.050(3) 0.0007(17) 0.013(2) 0.0033(18) C38 0.058(3) 0.039(2) 0.081(3) -0.011(2) -0.003(3) 0.015(2) C23 0.045(2) 0.0237(14) 0.0331(19) 0.0072(13) -0.0002(16) -0.0015(14) C33 0.042(3) 0.129(4) 0.048(3) 0.024(3) -0.016(2) 0.009(3) C39 0.044(2) 0.0341(17) 0.054(3) 0.0011(16) -0.0020(19) 0.0158(16) C37 0.067(3) 0.031(2) 0.137(6) 0.012(3) 0.018(3) 0.008(2) C8 0.088(4) 0.134(5) 0.059(3) 0.038(3) 0.001(3) 0.046(4) C27 0.057(3) 0.101(4) 0.081(4) -0.063(3) 0.022(3) 0.000(3) C13 0.036(2) 0.056(2) 0.098(4) -0.032(3) 0.023(2) -0.0036(19) C19 0.080(3) 0.044(2) 0.047(3) 0.0119(19) 0.019(2) -0.008(2) C30 0.089(4) 0.075(3) 0.056(3) 0.027(2) -0.047(3) -0.034(3) C9 0.118(5) 0.054(3) 0.069(4) -0.009(2) -0.015(3) 0.007(3) C35 0.059(3) 0.045(2) 0.074(3) 0.018(2) 0.030(2) 0.020(2) C6 0.054(3) 0.039(2) 0.211(7) -0.046(3) -0.071(4) 0.018(2) C11 0.068(4) 0.046(3) 0.417(16) -0.069(6) -0.052(7) 0.025(3) C10 0.082(5) 0.027(2) 0.368(14) -0.037(5) -0.121(7) 0.015(3) C5 0.062(4) 0.060(3) 0.281(10) -0.079(5) -0.096(5) 0.019(3) C36 0.073(4) 0.049(3) 0.136(6) 0.029(3) 0.047(4) 0.014(2) C24 0.057(3) 0.0342(18) 0.056(3) 0.0080(17) -0.021(2) 0.0074(18) C25 0.045(3) 0.083(3) 0.123(5) -0.051(3) -0.015(3) 0.033(3) C31 0.066(4) 0.157(6) 0.097(5) 0.060(5) -0.060(4) -0.033(4) C32 0.040(3) 0.223(8) 0.091(5) 0.066(5) -0.025(3) -0.006(4) C26 0.044(3) 0.129(5) 0.134(6) -0.073(5) 0.026(3) 0.016(3) C12 0.177(10) 0.042(3) 0.410(19) -0.015(6) -0.180(12) 0.007(5) C3 0.056(3) 0.075(3) 0.061(3) -0.037(2) -0.037(2) 0.032(2) C4 0.055(3) 0.092(4) 0.155(6) -0.077(4) -0.072(4) 0.037(3) O 0.078(2) 0.0459(15) 0.056(2) -0.0006(13) -0.0122(18) -0.0079(16) C43 0.082(5) 0.076(3) 0.122(6) 0.022(4) -0.023(4) 0.008(3) C40 0.121(6) 0.076(4) 0.108(5) -0.001(4) -0.016(5) 0.015(4) C41 0.145(11) 0.59(3) 0.177(12) -0.239(17) 0.006(9) -0.048(14) C42 0.102(8) 0.47(2) 0.286(16) -0.302(17) -0.015(9) -0.036(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 I Co 2.5258(5) . ? Co N 1.910(3) . ? Co P2 2.3731(8) . ? Co P1 2.3849(9) . ? P1 C14 1.820(4) . ? P1 C22 1.820(4) . ? P1 C16 1.822(3) . ? P2 C28 1.813(4) . ? P2 C34 1.821(3) . ? P2 C15 1.829(4) . ? Si1 N 1.706(3) . ? Si1 C13 1.863(4) . ? Si1 C14 1.869(3) . ? Si1 C15 1.883(4) . ? N C1 1.419(4) . ? C1 C6 1.405(6) . ? C1 C2 1.413(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C2 C3 1.396(5) . ? C2 C7 1.511(6) . ? C20 C19 1.372(6) . ? C20 C21 1.396(5) . ? C20 H20 0.9500 . ? C16 C21 1.386(5) . ? C16 C17 1.396(5) . ? C34 C39 1.390(5) . ? C34 C35 1.395(5) . ? C28 C33 1.382(6) . ? C28 C29 1.389(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C21 H21 0.9500 . ? C29 C30 1.379(7) . ? C29 H29 0.9500 . ? C17 C18 1.377(5) . ? C17 H17 0.9500 . ? C22 C23 1.382(5) . ? C22 C27 1.405(6) . ? C7 C8 1.521(7) . ? C7 C9 1.536(7) . ? C7 H7 1.0000 . ? C18 C19 1.380(6) . ? C18 H18 0.9500 . ? C38 C37 1.363(7) . ? C38 C39 1.388(5) . ? C38 H38 0.9500 . ? C23 C24 1.394(5) . ? C23 H23 0.9500 . ? C33 C32 1.391(7) . ? C33 H33 0.9500 . ? C39 H39 0.9500 . ? C37 C36 1.384(8) . ? C37 H37 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C27 C26 1.395(8) . ? C27 H27 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C19 H19 0.9500 . ? C30 C31 1.354(9) . ? C30 H30 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C35 C36 1.392(6) . ? C35 H35 0.9500 . ? C6 C5 1.377(6) . ? C6 C10 1.511(8) . ? C11 C10 1.566(13) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C10 C12 1.494(16) . ? C10 H10 1.0000 . ? C5 C4 1.375(8) . ? C5 H5 0.9500 . ? C36 H36 0.9500 . ? C24 C25 1.355(7) . ? C24 H24 0.9500 . ? C25 C26 1.380(9) . ? C25 H25 0.9500 . ? C31 C32 1.366(8) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C26 H26 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C3 C4 1.370(7) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? O C41 1.275(12) . ? O C42 1.282(8) . ? C43 C42 1.232(11) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C40 C41 1.304(11) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 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 N Co P2 90.29(9) . . ? N Co P1 89.78(8) . . ? P2 Co P1 93.44(3) . . ? N Co I 143.57(8) . . ? P2 Co I 112.33(3) . . ? P1 Co I 115.61(3) . . ? C14 P1 C22 108.27(16) . . ? C14 P1 C16 107.59(17) . . ? C22 P1 C16 100.57(16) . . ? C14 P1 Co 101.99(11) . . ? C22 P1 Co 121.20(10) . . ? C16 P1 Co 116.62(11) . . ? C28 P2 C34 100.83(15) . . ? C28 P2 C15 108.3(2) . . ? C34 P2 C15 106.12(19) . . ? C28 P2 Co 120.31(12) . . ? C34 P2 Co 118.49(12) . . ? C15 P2 Co 101.95(11) . . ? N Si1 C13 114.82(19) . . ? N Si1 C14 106.41(15) . . ? C13 Si1 C14 111.65(17) . . ? N Si1 C15 106.51(16) . . ? C13 Si1 C15 110.7(2) . . ? C14 Si1 C15 106.3(2) . . ? C1 N Si1 126.2(3) . . ? C1 N Co 126.7(3) . . ? Si1 N Co 107.15(13) . . ? C6 C1 C2 119.1(3) . . ? C6 C1 N 120.5(3) . . ? C2 C1 N 120.4(3) . . ? P1 C14 Si1 106.90(16) . . ? P1 C14 H14A 110.3 . . ? Si1 C14 H14A 110.3 . . ? P1 C14 H14B 110.3 . . ? Si1 C14 H14B 110.3 . . ? H14A C14 H14B 108.6 . . ? C3 C2 C1 118.6(4) . . ? C3 C2 C7 119.5(4) . . ? C1 C2 C7 121.8(3) . . ? C19 C20 C21 119.9(4) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C21 C16 C17 118.7(3) . . ? C21 C16 P1 118.0(3) . . ? C17 C16 P1 123.2(3) . . ? C39 C34 C35 119.2(3) . . ? C39 C34 P2 118.7(3) . . ? C35 C34 P2 121.9(3) . . ? C33 C28 C29 118.7(4) . . ? C33 C28 P2 117.9(3) . . ? C29 C28 P2 123.5(3) . . ? P2 C15 Si1 106.79(18) . . ? P2 C15 H15A 110.4 . . ? Si1 C15 H15A 110.4 . . ? P2 C15 H15B 110.4 . . ? Si1 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? C16 C21 C20 120.7(4) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C30 C29 C28 120.3(5) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C18 C17 C16 119.8(4) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C23 C22 C27 118.0(4) . . ? C23 C22 P1 124.1(3) . . ? C27 C22 P1 117.9(3) . . ? C2 C7 C8 110.9(4) . . ? C2 C7 C9 113.7(4) . . ? C8 C7 C9 109.8(4) . . ? C2 C7 H7 107.4 . . ? C8 C7 H7 107.4 . . ? C9 C7 H7 107.4 . . ? C17 C18 C19 121.3(4) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C37 C38 C39 119.3(5) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C22 C23 C24 121.0(4) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C28 C33 C32 120.1(5) . . ? C28 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C38 C39 C34 120.9(4) . . ? C38 C39 H39 119.5 . . ? C34 C39 H39 119.5 . . ? C38 C37 C36 121.1(4) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C26 C27 C22 120.3(5) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C20 C19 C18 119.4(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C31 C30 C29 120.3(5) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C36 C35 C34 119.4(5) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C5 C6 C1 119.1(5) . . ? C5 C6 C10 120.2(5) . . ? C1 C6 C10 120.7(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 C10 C6 112.9(7) . . ? C12 C10 C11 111.6(6) . . ? C6 C10 C11 109.4(8) . . ? C12 C10 H10 107.6 . . ? C6 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? C4 C5 C6 122.7(5) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C37 C36 C35 120.0(5) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C25 C24 C23 120.5(4) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.3(5) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C30 C31 C32 120.7(5) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C31 C32 C33 119.8(6) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C25 C26 C27 119.9(5) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C4 C3 C2 122.2(4) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 118.2(4) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C41 O C42 125.9(7) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O C41 C40 129.4(10) . . ? O C41 H41A 104.9 . . ? C40 C41 H41A 104.9 . . ? O C41 H41B 104.9 . . ? C40 C41 H41B 104.9 . . ? H41A C41 H41B 105.8 . . ? C43 C42 O 133.3(9) . . ? C43 C42 H42A 103.9 . . ? O C42 H42A 103.9 . . ? C43 C42 H42B 103.9 . . ? O C42 H42B 103.9 . . ? H42A C42 H42B 105.4 . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 32.82 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 3.111 _refine_diff_density_min -2.974 _refine_diff_density_rms 0.140 #===END data_mtw21 _database_code_depnum_ccdc_archive 'CCDC 297851' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H52 Cl Co N P3 Si' _chemical_formula_weight 894.32 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' N N 0.0061 0.0033 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 12.8058(15) _cell_length_b 17.612(2) _cell_length_c 20.505(3) _cell_angle_alpha 93.701(4) _cell_angle_beta 91.736(4) _cell_angle_gamma 103.463(4) _cell_volume 4483.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2086 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 20.97 _exptl_crystal_description blade _exptl_crystal_colour brown _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.081 _exptl_crystal_size_min 0.074 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.613 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17435 _diffrn_reflns_av_R_equivalents 0.1319 _diffrn_reflns_av_sigmaI/netI 0.2188 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 23.01 _reflns_number_total 9939 _reflns_number_gt 4751 _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^)+(0.1451P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9939 _refine_ls_number_parameters 1057 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1835 _refine_ls_R_factor_gt 0.0935 _refine_ls_wR_factor_ref 0.2813 _refine_ls_wR_factor_gt 0.2331 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.004 _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 Co1A Co 0.74908(13) 0.93976(9) 0.25614(8) 0.0200(5) Uani 1 1 d . . . Co1B Co 0.78433(14) 0.44161(10) 0.24812(9) 0.0282(6) Uani 1 1 d . . . Cl1A Cl 0.7125(2) 0.81076(17) 0.27449(16) 0.0242(9) Uani 1 1 d . . . Cl1B Cl 0.8197(3) 0.32123(19) 0.23113(18) 0.0374(10) Uani 1 1 d . . . P1A P 0.7903(3) 1.06203(18) 0.24282(17) 0.0217(9) Uani 1 1 d . . . P2A P 0.8322(3) 0.92705(19) 0.15948(17) 0.0229(9) Uani 1 1 d . . . P3A P 0.8835(3) 0.96298(18) 0.33134(17) 0.0228(9) Uani 1 1 d . . . P1B P 0.7538(3) 0.55387(19) 0.2697(2) 0.0311(10) Uani 1 1 d . . . P2B P 0.8565(4) 0.4524(2) 0.3512(2) 0.0487(12) Uani 1 1 d . . . P3B P 0.6036(4) 0.3947(2) 0.2585(2) 0.0509(13) Uani 1 1 d . . . Si1A Si 0.5811(3) 1.0362(2) 0.30152(19) 0.0283(10) Uani 1 1 d . . . Si1B Si 0.9214(3) 0.5813(2) 0.1768(2) 0.0401(12) Uani 1 1 d . . . N1A N 0.5976(8) 0.9522(5) 0.2586(5) 0.021(3) Uani 1 1 d . . . N1B N 0.8438(10) 0.4838(7) 0.1690(6) 0.050(4) Uani 1 1 d . . . C1 C 0.5111(10) 0.8919(7) 0.2368(6) 0.022(3) Uani 1 1 d . . . C2 C 0.4770(10) 0.8786(7) 0.1690(7) 0.022(3) Uani 1 1 d . . . C3 C 0.3902(11) 0.8188(8) 0.1481(7) 0.030(4) Uani 1 1 d . . . H3 H 0.3688 0.8117 0.1029 0.036 Uiso 1 1 calc R . . C4 C 0.3352(11) 0.7704(8) 0.1892(7) 0.034(4) Uani 1 1 d . . . H4 H 0.2765 0.7295 0.1724 0.041 Uiso 1 1 calc R . . C5 C 0.3615(11) 0.7784(8) 0.2560(7) 0.034(4) Uani 1 1 d . . . H5 H 0.3199 0.7446 0.2848 0.040 Uiso 1 1 calc R . . C6 C 0.4532(10) 0.8390(7) 0.2807(7) 0.028(4) Uani 1 1 d . . . C7 C 0.5397(11) 0.9309(8) 0.1212(7) 0.038(4) Uani 1 1 d . . . H7 H 0.6178 0.9385 0.1337 0.045 Uiso 1 1 calc R . . C8 C 0.5228(11) 0.8977(8) 0.0496(6) 0.038(4) Uani 1 1 d . . . H8A H 0.5262 0.8425 0.0470 0.058 Uiso 1 1 calc R . . H8B H 0.5792 0.9273 0.0237 0.058 Uiso 1 1 calc R . . H8C H 0.4523 0.9019 0.0324 0.058 Uiso 1 1 calc R . . C9 C 0.5153(12) 1.0133(7) 0.1215(7) 0.042(4) Uani 1 1 d . . . H9A H 0.4398 1.0079 0.1079 0.062 Uiso 1 1 calc R . . H9B H 0.5615 1.0447 0.0911 0.062 Uiso 1 1 calc R . . H9C H 0.5292 1.0392 0.1657 0.062 Uiso 1 1 calc R . . C10 C 0.4822(10) 0.8444(7) 0.3542(6) 0.028(4) Uani 1 1 d . . . H10 H 0.5534 0.8824 0.3623 0.033 Uiso 1 1 calc R . . C11 C 0.4934(12) 0.7658(8) 0.3769(7) 0.044(4) Uani 1 1 d . . . H11A H 0.5118 0.7713 0.4240 0.065 Uiso 1 1 calc R . . H11B H 0.5504 0.7487 0.3534 0.065 Uiso 1 1 calc R . . H11C H 0.4253 0.7268 0.3680 0.065 Uiso 1 1 calc R . . C12 C 0.4031(11) 0.8729(9) 0.3956(7) 0.048(4) Uani 1 1 d . . . H12A H 0.3871 0.9195 0.3779 0.071 Uiso 1 1 calc R . . H12B H 0.4335 0.8861 0.4405 0.071 Uiso 1 1 calc R . . H12C H 0.3367 0.8317 0.3957 0.071 Uiso 1 1 calc R . . C13 C 0.6029(11) 1.0497(7) 0.3924(6) 0.033(4) Uani 1 1 d . . . H13A H 0.5616 1.0035 0.4121 0.049 Uiso 1 1 calc R . . H13B H 0.5790 1.0961 0.4088 0.049 Uiso 1 1 calc R . . H13C H 0.6795 1.0567 0.4041 0.049 Uiso 1 1 calc R . . C14 C 0.4450(10) 1.0541(8) 0.2840(7) 0.034(4) Uani 1 1 d . . . H14A H 0.4497 1.0919 0.2506 0.051 Uiso 1 1 calc R . . H14B H 0.4187 1.0749 0.3241 0.051 Uiso 1 1 calc R . . H14C H 0.3952 1.0047 0.2681 0.051 Uiso 1 1 calc R . . C15 C 0.6923(10) 1.1151(7) 0.2725(7) 0.031(4) Uani 1 1 d . . . H15 H 0.6964 1.1697 0.2731 0.037 Uiso 1 1 calc R . . C16 C 0.8063(10) 1.0777(7) 0.1556(6) 0.027(3) Uani 1 1 d . . . C17 C 0.7980(12) 1.1461(8) 0.1286(8) 0.041(4) Uani 1 1 d . . . H17 H 0.7859 1.1891 0.1552 0.049 Uiso 1 1 calc R . . C18 C 0.8075(13) 1.1502(9) 0.0633(8) 0.049(5) Uani 1 1 d . . . H18 H 0.8018 1.1972 0.0448 0.059 Uiso 1 1 calc R . . C19 C 0.8248(14) 1.0911(9) 0.0232(7) 0.056(5) Uani 1 1 d . . . H19 H 0.8307 1.0964 -0.0225 0.067 Uiso 1 1 calc R . . C20 C 0.8339(12) 1.0209(9) 0.0502(7) 0.046(4) Uani 1 1 d . . . H20 H 0.8470 0.9788 0.0229 0.055 Uiso 1 1 calc R . . C21 C 0.8238(11) 1.0139(7) 0.1161(7) 0.035(4) Uani 1 1 d . . . C22 C 0.7805(10) 0.8431(7) 0.0992(6) 0.019(3) Uani 1 1 d U . . C23 C 0.8356(12) 0.8326(8) 0.0446(7) 0.037(4) Uani 1 1 d . . . H23 H 0.9029 0.8672 0.0386 0.045 Uiso 1 1 calc R . . C24 C 0.7934(15) 0.7711(10) -0.0022(8) 0.056(5) Uani 1 1 d . . . H24 H 0.8299 0.7648 -0.0411 0.067 Uiso 1 1 calc R . . C25 C 0.6985(15) 0.7203(10) 0.0091(9) 0.056(5) Uani 1 1 d . . . H25 H 0.6700 0.6778 -0.0222 0.067 Uiso 1 1 calc R . . C26 C 0.6428(15) 0.7288(10) 0.0646(9) 0.063(5) Uani 1 1 d . . . H26 H 0.5768 0.6929 0.0714 0.076 Uiso 1 1 calc R . . C27 C 0.6862(11) 0.7922(8) 0.1113(7) 0.033(4) Uani 1 1 d . . . H27 H 0.6503 0.7990 0.1503 0.040 Uiso 1 1 calc R . . C28 C 0.9760(11) 0.9311(7) 0.1573(6) 0.026(3) Uani 1 1 d . . . C29 C 1.0534(13) 1.0013(8) 0.1587(7) 0.042(4) Uani 1 1 d . . . H29 H 1.0313 1.0493 0.1589 0.050 Uiso 1 1 calc R . . C30 C 1.1620(13) 1.0026(9) 0.1599(7) 0.048(4) Uani 1 1 d . . . H30 H 1.2144 1.0509 0.1615 0.058 Uiso 1 1 calc R . . C31 C 1.1923(13) 0.9330(10) 0.1589(7) 0.045(4) Uani 1 1 d . . . H31 H 1.2666 0.9333 0.1595 0.054 Uiso 1 1 calc R . . C32 C 1.1184(12) 0.8632(9) 0.1571(6) 0.031(4) Uani 1 1 d . . . H32 H 1.1410 0.8154 0.1547 0.037 Uiso 1 1 calc R . . C33 C 1.0123(11) 0.8623(8) 0.1586(6) 0.031(4) Uani 1 1 d . . . H33 H 0.9615 0.8138 0.1605 0.037 Uiso 1 1 calc R . . C34 C 0.9217(10) 1.1079(7) 0.2822(6) 0.026(3) Uani 1 1 d . . . C35 C 0.9793(12) 1.1823(8) 0.2735(7) 0.041(4) Uani 1 1 d . . . H35 H 0.9487 1.2135 0.2460 0.049 Uiso 1 1 calc R . . C36 C 1.0776(12) 1.2132(9) 0.3022(9) 0.054(5) Uani 1 1 d . . . H36 H 1.1138 1.2655 0.2957 0.065 Uiso 1 1 calc R . . C37 C 1.1259(12) 1.1677(9) 0.3417(8) 0.052(5) Uani 1 1 d . . . H37 H 1.1962 1.1880 0.3609 0.063 Uiso 1 1 calc R . . C38 C 1.0691(11) 1.0919(7) 0.3524(7) 0.035(4) Uani 1 1 d . . . H38 H 1.1004 1.0612 0.3801 0.042 Uiso 1 1 calc R . . C39 C 0.9673(10) 1.0607(7) 0.3231(6) 0.023(3) Uani 1 1 d . . . C40 C 0.9763(11) 0.8980(7) 0.3409(6) 0.021(3) Uani 1 1 d . . . C41 C 1.0714(12) 0.9125(8) 0.3114(7) 0.031(4) Uani 1 1 d . . . H41 H 1.0931 0.9581 0.2881 0.037 Uiso 1 1 calc R . . C42 C 1.1406(13) 0.8569(10) 0.3160(7) 0.045(4) Uani 1 1 d . . . H42 H 1.2086 0.8669 0.2968 0.054 Uiso 1 1 calc R . . C43 C 1.1065(13) 0.7918(9) 0.3476(7) 0.036(4) Uani 1 1 d . . . H43 H 1.1495 0.7546 0.3491 0.043 Uiso 1 1 calc R . . C44 C 1.0105(12) 0.7783(8) 0.3778(7) 0.037(4) Uani 1 1 d . . . H44 H 0.9880 0.7331 0.4014 0.044 Uiso 1 1 calc R . . C45 C 0.9443(11) 0.8338(8) 0.3731(7) 0.034(4) Uani 1 1 d . . . H45 H 0.8770 0.8245 0.3931 0.041 Uiso 1 1 calc R . . C46 C 0.8338(10) 0.9696(7) 0.4133(7) 0.024(3) Uani 1 1 d . . . C47 C 0.8754(11) 1.0308(8) 0.4610(7) 0.034(4) Uani 1 1 d . . . H47 H 0.9358 1.0708 0.4520 0.041 Uiso 1 1 calc R . . C48 C 0.8295(13) 1.0335(9) 0.5208(7) 0.035(4) Uani 1 1 d . . . H48 H 0.8557 1.0776 0.5510 0.042 Uiso 1 1 calc R . . C49 C 0.7494(12) 0.9761(10) 0.5375(6) 0.036(4) Uani 1 1 d . . . H49 H 0.7214 0.9775 0.5799 0.043 Uiso 1 1 calc R . . C50 C 0.7079(11) 0.9143(8) 0.4916(7) 0.035(4) Uani 1 1 d . . . H50 H 0.6497 0.8735 0.5024 0.042 Uiso 1 1 calc R . . C51 C 0.7496(11) 0.9110(8) 0.4303(7) 0.032(4) Uani 1 1 d . . . H51 H 0.7199 0.8680 0.3997 0.038 Uiso 1 1 calc R . . C52 C 0.8346(16) 0.4362(9) 0.1097(9) 0.073(6) Uani 1 1 d D . . C53 C 0.9226(13) 0.4012(8) 0.0907(8) 0.058(5) Uani 1 1 d D . . C54 C 0.9082(12) 0.3545(9) 0.0307(8) 0.064(5) Uani 1 1 d D . . H54 H 0.9642 0.3307 0.0173 0.076 Uiso 1 1 calc R . . C55 C 0.8149(13) 0.3421(9) -0.0095(7) 0.075(7) Uani 1 1 d DU . . H55 H 0.8098 0.3111 -0.0497 0.090 Uiso 1 1 calc R . . C56 C 0.7302(13) 0.3739(9) 0.0078(11) 0.083(7) Uani 1 1 d D . . H56 H 0.6680 0.3658 -0.0206 0.099 Uiso 1 1 calc R . . C57 C 0.7366(14) 0.4195(10) 0.0695(8) 0.062(5) Uani 1 1 d . . . C58 C 1.0267(11) 0.4173(8) 0.1272(8) 0.040(4) Uani 1 1 d . . . H58 H 1.0196 0.4463 0.1698 0.049 Uiso 1 1 calc R . . C59 C 1.0597(14) 0.3426(10) 0.1422(9) 0.072(6) Uani 1 1 d . . . H59A H 1.0024 0.3091 0.1649 0.108 Uiso 1 1 calc R . . H59B H 1.1259 0.3557 0.1701 0.108 Uiso 1 1 calc R . . H59C H 1.0722 0.3149 0.1013 0.108 Uiso 1 1 calc R . . C60 C 1.1160(12) 0.4679(9) 0.0913(7) 0.054(5) Uani 1 1 d . . . H60A H 1.1223 0.4418 0.0484 0.080 Uiso 1 1 calc R . . H60B H 1.1841 0.4761 0.1169 0.080 Uiso 1 1 calc R . . H60C H 1.0992 0.5187 0.0854 0.080 Uiso 1 1 calc R . . C61 C 0.6461(12) 0.4535(9) 0.0860(9) 0.057(5) Uani 1 1 d . . . H61 H 0.6341 0.4473 0.1336 0.069 Uiso 1 1 calc R . . C62 C 0.5459(18) 0.4141(11) 0.0499(10) 0.119(10) Uani 1 1 d . . . H62A H 0.5513 0.4255 0.0038 0.178 Uiso 1 1 calc R . . H62B H 0.4861 0.4329 0.0683 0.178 Uiso 1 1 calc R . . H62C H 0.5334 0.3575 0.0532 0.178 Uiso 1 1 calc R . . C63 C 0.6631(14) 0.5403(9) 0.0756(10) 0.083(7) Uani 1 1 d . . . H63A H 0.7251 0.5700 0.1030 0.124 Uiso 1 1 calc R . . H63B H 0.5988 0.5581 0.0877 0.124 Uiso 1 1 calc R . . H63C H 0.6764 0.5486 0.0295 0.124 Uiso 1 1 calc R . . C64 C 0.9371(15) 0.6251(10) 0.0939(8) 0.081(6) Uani 1 1 d . . . H64A H 0.9216 0.5829 0.0589 0.121 Uiso 1 1 calc R . . H64B H 1.0108 0.6561 0.0911 0.121 Uiso 1 1 calc R . . H64C H 0.8868 0.6589 0.0891 0.121 Uiso 1 1 calc R . . C65 C 1.0572(13) 0.6070(10) 0.2142(9) 0.070(6) Uani 1 1 d . . . H65A H 1.0551 0.5933 0.2597 0.105 Uiso 1 1 calc R . . H65B H 1.0871 0.6634 0.2128 0.105 Uiso 1 1 calc R . . H65C H 1.1025 0.5782 0.1900 0.105 Uiso 1 1 calc R . . C66 C 0.8392(10) 0.6330(8) 0.2305(7) 0.034(4) Uani 1 1 d . . . H66 H 0.8419 0.6875 0.2358 0.041 Uiso 1 1 calc R . . C67 C 0.7698(12) 0.5806(7) 0.3580(7) 0.039(4) Uani 1 1 d . . . C68 C 0.7485(12) 0.6475(8) 0.3883(9) 0.048(5) Uani 1 1 d . . . H68 H 0.7200 0.6823 0.3634 0.058 Uiso 1 1 calc R . . C69 C 0.7686(12) 0.6634(10) 0.4543(9) 0.053(5) Uani 1 1 d . . . H69 H 0.7552 0.7100 0.4745 0.063 Uiso 1 1 calc R . . C70 C 0.8072(15) 0.6144(11) 0.4916(10) 0.070(6) Uani 1 1 d . . . H70 H 0.8169 0.6259 0.5376 0.084 Uiso 1 1 calc R . . C71 C 0.8319(16) 0.5494(9) 0.4641(8) 0.073(6) Uani 1 1 d . . . H71 H 0.8615 0.5170 0.4910 0.088 Uiso 1 1 calc R . . C72 C 0.8153(15) 0.5294(10) 0.3982(8) 0.064(5) Uani 1 1 d . . . C73 C 1.0047(12) 0.4835(9) 0.3509(8) 0.044(4) Uani 1 1 d . . . C74 C 1.0628(15) 0.5467(10) 0.3889(9) 0.064(5) Uani 1 1 d . . . H74 H 1.0276 0.5752 0.4183 0.077 Uiso 1 1 calc R . . C75 C 1.1750(15) 0.5695(11) 0.3843(9) 0.062(5) Uani 1 1 d . . . H75 H 1.2156 0.6148 0.4090 0.074 Uiso 1 1 calc R . . C76 C 1.2253(16) 0.5256(13) 0.3437(11) 0.083(6) Uani 1 1 d . . . H76 H 1.3011 0.5408 0.3403 0.100 Uiso 1 1 calc R . . C77 C 1.1673(14) 0.4605(9) 0.3085(9) 0.071(6) Uani 1 1 d . . . H77 H 1.2012 0.4260 0.2843 0.085 Uiso 1 1 calc R . . C78 C 1.0599(15) 0.4476(11) 0.3096(8) 0.066(6) Uani 1 1 d . . . H78 H 1.0192 0.4093 0.2781 0.079 Uiso 1 1 calc R . . C79 C 0.8325(16) 0.3700(10) 0.4030(8) 0.054(5) Uani 1 1 d . . . C80 C 0.7529(17) 0.3542(13) 0.4444(11) 0.074(6) Uani 1 1 d . . . H80 H 0.7063 0.3888 0.4489 0.088 Uiso 1 1 calc R . . C81 C 0.7357(16) 0.2891(13) 0.4812(10) 0.075(6) Uani 1 1 d . . . H81 H 0.6776 0.2788 0.5096 0.090 Uiso 1 1 calc R . . C82 C 0.8026(18) 0.2415(10) 0.4755(9) 0.060(5) Uani 1 1 d . . . H82 H 0.7919 0.1973 0.5009 0.072 Uiso 1 1 calc R . . C83 C 0.8830(17) 0.2538(10) 0.4360(11) 0.072(6) Uani 1 1 d . . . H83 H 0.9288 0.2185 0.4331 0.087 Uiso 1 1 calc R . . C84 C 0.9014(14) 0.3187(9) 0.3980(8) 0.057(5) Uani 1 1 d . . . H84 H 0.9594 0.3277 0.3694 0.069 Uiso 1 1 calc R . . C85 C 0.6150(11) 0.5539(8) 0.2431(8) 0.044(4) Uani 1 1 d . . . C86 C 0.5780(11) 0.6189(7) 0.2352(7) 0.040(4) Uani 1 1 d . . . H86 H 0.6245 0.6693 0.2441 0.048 Uiso 1 1 calc R . . C87 C 0.4740(12) 0.6117(9) 0.2145(8) 0.054(5) Uani 1 1 d . . . H87 H 0.4498 0.6577 0.2074 0.065 Uiso 1 1 calc R . . C88 C 0.4024(14) 0.5398(10) 0.2034(10) 0.081(7) Uani 1 1 d . . . H88 H 0.3316 0.5361 0.1859 0.097 Uiso 1 1 calc R . . C89 C 0.4369(14) 0.4707(9) 0.2187(9) 0.068(6) Uani 1 1 d . . . H89 H 0.3871 0.4212 0.2154 0.082 Uiso 1 1 calc R . . C90 C 0.5468(12) 0.4769(9) 0.2388(9) 0.063(6) Uani 1 1 d . . . C91 C 0.5499(12) 0.3695(9) 0.3387(8) 0.046(4) Uani 1 1 d . . . C92 C 0.5130(14) 0.4225(10) 0.3784(9) 0.056(5) Uani 1 1 d . . . H92 H 0.5156 0.4738 0.3655 0.067 Uiso 1 1 calc R . . C93 C 0.4727(18) 0.3999(14) 0.4367(12) 0.099(8) Uani 1 1 d . . . H93 H 0.4530 0.4376 0.4661 0.119 Uiso 1 1 calc R . . C94 C 0.4598(17) 0.3252(15) 0.4543(11) 0.097(7) Uani 1 1 d . . . H94 H 0.4314 0.3107 0.4952 0.116 Uiso 1 1 calc R . . C95 C 0.4897(16) 0.2697(13) 0.4102(12) 0.086(7) Uani 1 1 d . . . H95 H 0.4793 0.2167 0.4203 0.104 Uiso 1 1 calc R . . C96 C 0.5342(13) 0.2937(9) 0.3526(8) 0.048(4) Uani 1 1 d . . . H96 H 0.5540 0.2569 0.3224 0.058 Uiso 1 1 calc R . . C97 C 0.5293(12) 0.3143(8) 0.2008(9) 0.048(5) Uani 1 1 d . . . C98 C 0.4178(14) 0.2817(10) 0.2123(8) 0.058(5) Uani 1 1 d . . . H98 H 0.3837 0.3029 0.2472 0.070 Uiso 1 1 calc R . . C99 C 0.3600(14) 0.2172(10) 0.1704(9) 0.057(5) Uani 1 1 d . . . H99 H 0.2859 0.1947 0.1751 0.069 Uiso 1 1 calc R . . C100 C 0.4163(15) 0.1898(8) 0.1236(10) 0.056(5) Uani 1 1 d . . . H100 H 0.3798 0.1460 0.0957 0.067 Uiso 1 1 calc R . . C101 C 0.5241(16) 0.2214(10) 0.1135(9) 0.065(5) Uani 1 1 d . . . H101 H 0.5588 0.2015 0.0782 0.078 Uiso 1 1 calc R . . C102 C 0.5776(14) 0.2806(9) 0.1547(8) 0.048(5) Uani 1 1 d . . . H102 H 0.6528 0.2993 0.1508 0.058 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 Co1A 0.0244(11) 0.0163(10) 0.0211(11) 0.0007(8) -0.0099(9) 0.0100(8) Co1B 0.0294(12) 0.0164(10) 0.0387(13) 0.0000(9) -0.0049(10) 0.0069(8) Cl1A 0.025(2) 0.0162(17) 0.031(2) -0.0006(15) -0.0088(17) 0.0062(14) Cl1B 0.046(2) 0.0225(19) 0.048(3) 0.0017(18) 0.000(2) 0.0177(17) P1A 0.027(2) 0.0177(19) 0.023(2) -0.0001(16) -0.0071(18) 0.0117(16) P2A 0.027(2) 0.0194(19) 0.024(2) -0.0014(17) -0.0067(18) 0.0118(16) P3A 0.026(2) 0.0167(19) 0.027(2) -0.0015(17) -0.0090(18) 0.0095(16) P1B 0.026(2) 0.0148(19) 0.052(3) -0.0016(19) -0.004(2) 0.0064(16) P2B 0.056(3) 0.036(3) 0.051(3) -0.004(2) -0.008(2) 0.009(2) P3B 0.053(3) 0.037(3) 0.061(3) 0.000(2) -0.012(2) 0.009(2) Si1A 0.033(2) 0.025(2) 0.030(2) -0.0028(19) -0.012(2) 0.0179(18) Si1B 0.045(3) 0.025(2) 0.047(3) 0.007(2) -0.001(2) 0.000(2) N1A 0.020(6) 0.022(6) 0.027(7) 0.000(5) -0.010(5) 0.018(5) N1B 0.063(10) 0.051(9) 0.044(9) 0.003(7) 0.006(7) 0.027(7) C1 0.016(8) 0.025(8) 0.027(9) -0.001(7) -0.009(7) 0.010(7) C2 0.016(8) 0.012(7) 0.042(10) -0.005(7) -0.012(7) 0.011(6) C3 0.023(9) 0.039(9) 0.032(9) 0.015(8) -0.008(8) 0.013(7) C4 0.033(10) 0.032(9) 0.038(11) -0.017(8) -0.022(8) 0.015(7) C5 0.028(9) 0.032(9) 0.049(11) 0.001(8) 0.006(8) 0.022(7) C6 0.020(8) 0.025(8) 0.040(10) -0.010(7) -0.006(8) 0.012(7) C7 0.023(9) 0.046(10) 0.041(10) -0.007(8) -0.021(8) 0.007(7) C8 0.051(10) 0.032(9) 0.030(9) -0.006(7) -0.019(8) 0.010(7) C9 0.059(11) 0.030(9) 0.040(10) 0.008(7) -0.020(8) 0.021(8) C10 0.027(9) 0.019(8) 0.033(9) 0.003(7) -0.010(7) -0.001(6) C11 0.043(10) 0.044(10) 0.042(10) 0.014(8) 0.005(8) 0.005(8) C12 0.039(10) 0.056(11) 0.045(11) -0.012(9) -0.003(9) 0.011(8) C13 0.044(9) 0.021(8) 0.035(9) -0.002(7) -0.012(8) 0.015(7) C14 0.029(9) 0.050(9) 0.034(9) -0.004(7) -0.001(7) 0.033(7) C15 0.026(8) 0.018(7) 0.053(10) 0.002(7) -0.001(7) 0.017(6) C16 0.030(9) 0.029(9) 0.024(8) 0.000(7) -0.005(7) 0.011(7) C17 0.064(11) 0.023(9) 0.042(11) 0.010(8) -0.019(9) 0.022(7) C18 0.086(13) 0.039(10) 0.033(11) 0.017(9) -0.016(10) 0.031(9) C19 0.108(15) 0.053(11) 0.019(9) 0.017(9) -0.005(9) 0.041(10) C20 0.074(13) 0.043(10) 0.028(10) 0.008(8) 0.001(9) 0.027(9) C21 0.044(10) 0.012(8) 0.046(11) 0.004(7) 0.008(8) 0.002(7) C22 0.024(7) 0.017(6) 0.019(7) -0.001(5) -0.017(6) 0.012(5) C23 0.038(10) 0.049(10) 0.035(10) -0.007(8) -0.010(8) 0.034(8) C24 0.076(14) 0.054(12) 0.049(12) -0.019(10) -0.023(11) 0.047(11) C25 0.064(13) 0.046(11) 0.049(13) -0.033(9) -0.031(11) 0.009(10) C26 0.072(14) 0.049(11) 0.059(13) -0.019(10) -0.014(11) 0.005(10) C27 0.039(10) 0.035(9) 0.032(9) -0.009(8) -0.004(8) 0.024(8) C28 0.037(9) 0.022(8) 0.018(8) 0.003(6) 0.004(7) 0.007(7) C29 0.054(12) 0.033(10) 0.041(10) 0.003(8) -0.007(9) 0.016(8) C30 0.051(12) 0.036(10) 0.053(12) -0.002(8) -0.001(9) 0.001(8) C31 0.038(10) 0.064(12) 0.031(10) 0.007(9) 0.015(8) 0.005(10) C32 0.039(10) 0.046(10) 0.015(8) -0.001(7) 0.005(7) 0.025(8) C33 0.031(10) 0.040(9) 0.028(9) -0.004(7) 0.008(7) 0.021(7) C34 0.031(9) 0.010(8) 0.036(9) -0.008(7) -0.007(7) 0.005(6) C35 0.051(11) 0.029(9) 0.041(10) -0.001(8) -0.018(9) 0.010(8) C36 0.049(11) 0.026(9) 0.086(14) 0.009(9) -0.015(11) 0.008(8) C37 0.045(11) 0.038(10) 0.067(13) 0.002(9) -0.009(9) -0.003(8) C38 0.032(9) 0.021(8) 0.051(10) -0.001(7) -0.006(8) 0.006(7) C39 0.030(9) 0.007(7) 0.034(9) 0.002(6) -0.005(7) 0.008(6) C40 0.025(9) 0.018(8) 0.023(8) -0.002(7) -0.015(7) 0.015(6) C41 0.043(10) 0.032(8) 0.025(9) -0.004(7) -0.020(8) 0.026(8) C42 0.049(11) 0.059(12) 0.026(10) -0.011(9) -0.018(8) 0.015(9) C43 0.038(11) 0.041(10) 0.034(10) -0.014(8) -0.014(8) 0.027(8) C44 0.043(11) 0.031(9) 0.042(10) 0.004(7) -0.013(9) 0.023(8) C45 0.024(9) 0.034(9) 0.046(10) 0.001(8) -0.020(8) 0.015(7) C46 0.020(8) 0.012(7) 0.043(10) 0.008(7) -0.011(7) 0.006(6) C47 0.030(9) 0.024(8) 0.048(11) -0.002(8) -0.023(8) 0.012(7) C48 0.053(12) 0.047(11) 0.011(9) -0.012(8) -0.019(8) 0.031(9) C49 0.048(11) 0.061(11) 0.004(8) 0.007(8) -0.001(8) 0.022(9) C50 0.035(9) 0.037(9) 0.040(11) 0.010(8) -0.010(9) 0.024(7) C51 0.037(10) 0.034(9) 0.029(10) -0.010(7) -0.016(8) 0.024(8) C52 0.096(17) 0.042(11) 0.079(15) -0.004(11) -0.004(13) 0.016(11) C53 0.045(11) 0.056(11) 0.070(14) -0.003(10) -0.008(10) 0.008(9) C54 0.088(15) 0.050(11) 0.057(13) -0.002(10) -0.002(12) 0.025(10) C55 0.14(2) 0.038(11) 0.024(10) -0.004(8) -0.055(12) -0.010(12) C56 0.036(12) 0.037(11) 0.16(2) -0.012(13) 0.023(13) -0.010(9) C57 0.069(14) 0.060(12) 0.055(12) -0.022(10) -0.037(11) 0.024(10) C58 0.034(10) 0.040(10) 0.050(11) -0.004(8) -0.005(9) 0.017(8) C59 0.063(13) 0.068(13) 0.086(15) 0.008(11) 0.018(11) 0.014(10) C60 0.051(12) 0.054(11) 0.050(11) -0.001(9) 0.002(9) 0.000(9) C61 0.035(11) 0.063(12) 0.067(13) 0.014(10) -0.006(10) -0.005(9) C62 0.18(2) 0.069(14) 0.115(19) -0.026(13) -0.121(18) 0.066(15) C63 0.085(15) 0.037(11) 0.126(19) 0.005(11) -0.033(13) 0.020(10) C64 0.098(16) 0.071(14) 0.069(14) -0.005(11) -0.013(12) 0.014(11) C65 0.064(13) 0.069(13) 0.074(14) -0.015(11) -0.016(11) 0.015(10) C66 0.025(8) 0.028(8) 0.055(11) 0.017(8) 0.003(8) 0.013(7) C67 0.045(10) 0.014(8) 0.054(11) -0.008(8) 0.022(9) -0.004(7) C68 0.046(11) 0.021(9) 0.074(14) -0.003(9) 0.002(10) 0.001(7) C69 0.036(11) 0.042(11) 0.070(14) -0.013(11) 0.003(10) -0.006(8) C70 0.081(15) 0.071(14) 0.061(14) -0.005(12) 0.012(11) 0.026(12) C71 0.136(19) 0.045(11) 0.050(13) -0.002(10) 0.023(12) 0.045(12) C72 0.101(15) 0.050(11) 0.038(11) -0.025(9) -0.004(11) 0.025(11) C73 0.043(11) 0.053(11) 0.040(11) 0.006(9) -0.020(9) 0.020(9) C74 0.063(14) 0.047(11) 0.085(15) -0.003(11) -0.013(12) 0.023(10) C75 0.054(14) 0.065(13) 0.056(13) 0.004(10) -0.020(10) -0.002(10) C76 0.062(14) 0.105(18) 0.097(17) 0.032(15) 0.000(14) 0.043(14) C77 0.056(14) 0.030(10) 0.115(17) -0.039(11) -0.051(12) 0.003(9) C78 0.054(14) 0.107(16) 0.030(11) -0.030(11) -0.035(10) 0.017(12) C79 0.078(14) 0.059(12) 0.033(11) 0.012(9) 0.014(10) 0.030(11) C80 0.076(16) 0.080(16) 0.077(16) -0.007(13) -0.021(13) 0.049(12) C81 0.064(15) 0.076(15) 0.077(16) -0.008(13) -0.004(12) 0.004(13) C82 0.086(16) 0.042(11) 0.043(12) 0.011(9) -0.032(12) -0.001(12) C83 0.076(16) 0.045(13) 0.099(17) 0.015(12) 0.002(14) 0.018(11) C84 0.066(13) 0.033(10) 0.064(13) -0.008(10) 0.012(10) -0.002(9) C85 0.028(9) 0.017(8) 0.079(13) -0.006(8) -0.024(9) -0.004(7) C86 0.032(10) 0.015(8) 0.071(12) -0.014(8) -0.013(9) 0.009(7) C87 0.039(11) 0.036(10) 0.095(15) 0.000(10) -0.006(10) 0.025(9) C88 0.060(13) 0.046(12) 0.135(19) -0.037(12) -0.054(12) 0.027(10) C89 0.076(14) 0.024(10) 0.098(16) -0.012(10) -0.004(12) 0.002(9) C90 0.037(11) 0.038(10) 0.112(16) -0.021(10) -0.027(11) 0.016(8) C91 0.046(11) 0.034(10) 0.060(12) 0.002(9) 0.040(9) 0.011(8) C92 0.069(13) 0.053(11) 0.055(12) 0.022(10) 0.025(11) 0.023(10) C93 0.12(2) 0.091(18) 0.11(2) 0.019(16) 0.055(17) 0.063(15) C94 0.093(18) 0.13(2) 0.091(18) 0.032(17) 0.033(14) 0.056(16) C95 0.061(14) 0.090(16) 0.12(2) 0.022(16) 0.011(14) 0.032(12) C96 0.048(11) 0.043(11) 0.047(12) 0.010(9) 0.015(9) -0.005(8) C97 0.022(10) 0.021(8) 0.096(15) -0.005(9) 0.008(9) 0.001(7) C98 0.061(14) 0.065(12) 0.048(12) -0.002(10) -0.007(10) 0.018(10) C99 0.042(11) 0.048(11) 0.080(14) 0.008(11) -0.012(11) 0.005(9) C100 0.057(14) 0.018(9) 0.087(16) 0.012(9) -0.031(12) 0.000(9) C101 0.076(16) 0.054(12) 0.063(14) 0.013(11) -0.027(12) 0.017(11) C102 0.067(12) 0.033(10) 0.049(11) -0.011(9) -0.013(10) 0.025(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1A N1A 2.004(9) . ? Co1A P1A 2.132(4) . ? Co1A P3A 2.222(4) . ? Co1A Cl1A 2.269(3) . ? Co1A P2A 2.301(4) . ? Co1B N1B 1.931(13) . ? Co1B P1B 2.125(4) . ? Co1B P2B 2.260(5) . ? Co1B Cl1B 2.277(3) . ? Co1B P3B 2.291(5) . ? P1A C34 1.827(13) . ? P1A C15 1.827(12) . ? P1A C16 1.838(14) . ? P2A C28 1.828(14) . ? P2A C21 1.841(14) . ? P2A C22 1.846(12) . ? P3A C46 1.821(14) . ? P3A C39 1.824(12) . ? P3A C40 1.847(12) . ? P1B C66 1.810(14) . ? P1B C67 1.833(15) . ? P1B C85 1.843(13) . ? P2B C72 1.800(15) . ? P2B C79 1.828(17) . ? P2B C73 1.849(16) . ? P3B C90 1.826(16) . ? P3B C91 1.843(16) . ? P3B C97 1.845(16) . ? Si1A N1A 1.730(10) . ? Si1A C13 1.868(13) . ? Si1A C14 1.870(12) . ? Si1A C15 1.884(14) . ? Si1B N1B 1.766(13) . ? Si1B C65 1.823(16) . ? Si1B C66 1.881(14) . ? Si1B C64 1.909(18) . ? N1A C1 1.385(15) . ? N1B C52 1.42(2) . ? C1 C2 1.432(17) . ? C1 C6 1.433(18) . ? C2 C3 1.378(17) . ? C2 C7 1.508(19) . ? C3 C4 1.334(18) . ? C3 H3 0.9500 . ? C4 C5 1.392(19) . ? C4 H4 0.9500 . ? C5 C6 1.444(18) . ? C5 H5 0.9500 . ? C6 C10 1.533(18) . ? C7 C8 1.535(18) . ? C7 C9 1.553(18) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.495(18) . ? C10 C11 1.526(18) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15 0.9500 . ? C16 C17 1.382(18) . ? C16 C21 1.407(18) . ? C17 C18 1.352(19) . ? C17 H17 0.9500 . ? C18 C19 1.35(2) . ? C18 H18 0.9500 . ? C19 C20 1.41(2) . ? C19 H19 0.9500 . ? C20 C21 1.371(19) . ? C20 H20 0.9500 . ? C22 C23 1.366(18) . ? C22 C27 1.366(18) . ? C23 C24 1.40(2) . ? C23 H23 0.9500 . ? C24 C25 1.37(2) . ? C24 H24 0.9500 . ? C25 C26 1.38(2) . ? C25 H25 0.9500 . ? C26 C27 1.419(19) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.392(18) . ? C28 C33 1.396(17) . ? C29 C30 1.39(2) . ? C29 H29 0.9500 . ? C30 C31 1.37(2) . ? C30 H30 0.9500 . ? C31 C32 1.364(19) . ? C31 H31 0.9500 . ? C32 C33 1.356(17) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.372(18) . ? C34 C39 1.422(17) . ? C35 C36 1.349(19) . ? C35 H35 0.9500 . ? C36 C37 1.40(2) . ? C36 H36 0.9500 . ? C37 C38 1.397(18) . ? C37 H37 0.9500 . ? C38 C39 1.392(17) . ? C38 H38 0.9500 . ? C40 C45 1.333(18) . ? C40 C41 1.354(18) . ? C41 C42 1.471(19) . ? C41 H41 0.9500 . ? C42 C43 1.34(2) . ? C42 H42 0.9500 . ? C43 C44 1.371(19) . ? C43 H43 0.9500 . ? C44 C45 1.441(18) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.379(18) . ? C46 C47 1.403(18) . ? C47 C48 1.379(19) . ? C47 H47 0.9500 . ? C48 C49 1.332(19) . ? C48 H48 0.9500 . ? C49 C50 1.387(19) . ? C49 H49 0.9500 . ? C50 C51 1.382(19) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C57 1.44(2) . ? C52 C53 1.46(2) . ? C53 C54 1.42(2) . ? C53 C58 1.47(2) . ? C54 C55 1.396(10) . ? C54 H54 0.9500 . ? C55 C56 1.378(10) . ? C55 H55 0.9500 . ? C56 C57 1.44(2) . ? C56 H56 0.9500 . ? C57 C61 1.46(2) . ? C58 C59 1.52(2) . ? C58 C60 1.519(19) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.46(2) . ? C61 C63 1.52(2) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66 0.9500 . ? C67 C68 1.384(19) . ? C67 C72 1.46(2) . ? C68 C69 1.37(2) . ? C68 H68 0.9500 . ? C69 C70 1.35(2) . ? C69 H69 0.9500 . ? C70 C71 1.35(2) . ? C70 H70 0.9500 . ? C71 C72 1.37(2) . ? C71 H71 0.9500 . ? C73 C78 1.34(2) . ? C73 C74 1.37(2) . ? C74 C75 1.41(2) . ? C74 H74 0.9500 . ? C75 C76 1.37(2) . ? C75 H75 0.9500 . ? C76 C77 1.36(2) . ? C76 H76 0.9500 . ? C77 C78 1.34(2) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C80 1.34(2) . ? C79 C84 1.40(2) . ? C80 C81 1.39(3) . ? C80 H80 0.9500 . ? C81 C82 1.33(2) . ? C81 H81 0.9500 . ? C82 C83 1.32(2) . ? C82 H82 0.9500 . ? C83 C84 1.40(2) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 C86 1.354(18) . ? C85 C90 1.428(19) . ? C86 C87 1.361(19) . ? C86 H86 0.9500 . ? C87 C88 1.38(2) . ? C87 H87 0.9500 . ? C88 C89 1.44(2) . ? C88 H88 0.9500 . ? C89 C90 1.43(2) . ? C89 H89 0.9500 . ? C91 C96 1.35(2) . ? C91 C92 1.37(2) . ? C92 C93 1.36(2) . ? C92 H92 0.9500 . ? C93 C94 1.36(3) . ? C93 H93 0.9500 . ? C94 C95 1.41(3) . ? C94 H94 0.9500 . ? C95 C96 1.38(2) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C97 C102 1.33(2) . ? C97 C98 1.44(2) . ? C98 C99 1.42(2) . ? C98 H98 0.9500 . ? C99 C100 1.35(2) . ? C99 H99 0.9500 . ? C100 C101 1.39(2) . ? C100 H100 0.9500 . ? C101 C102 1.34(2) . ? C101 H101 0.9500 . ? C102 H102 0.9500 . ? 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 N1A Co1A P1A 85.2(3) . . ? N1A Co1A P3A 132.5(3) . . ? P1A Co1A P3A 87.12(13) . . ? N1A Co1A Cl1A 96.9(3) . . ? P1A Co1A Cl1A 176.93(15) . . ? P3A Co1A Cl1A 89.81(13) . . ? N1A Co1A P2A 122.2(3) . . ? P1A Co1A P2A 85.00(14) . . ? P3A Co1A P2A 103.56(14) . . ? Cl1A Co1A P2A 95.75(13) . . ? N1B Co1B P1B 85.4(4) . . ? N1B Co1B P2B 131.0(4) . . ? P1B Co1B P2B 86.65(16) . . ? N1B Co1B Cl1B 97.1(4) . . ? P1B Co1B Cl1B 176.72(17) . . ? P2B Co1B Cl1B 90.12(15) . . ? N1B Co1B P3B 122.7(4) . . ? P1B Co1B P3B 85.42(15) . . ? P2B Co1B P3B 104.68(18) . . ? Cl1B Co1B P3B 94.88(15) . . ? C34 P1A C15 108.8(6) . . ? C34 P1A C16 104.8(6) . . ? C15 P1A C16 107.7(6) . . ? C34 P1A Co1A 110.5(4) . . ? C15 P1A Co1A 114.4(4) . . ? C16 P1A Co1A 110.0(4) . . ? C28 P2A C21 101.1(6) . . ? C28 P2A C22 99.5(6) . . ? C21 P2A C22 104.9(6) . . ? C28 P2A Co1A 122.0(4) . . ? C21 P2A Co1A 105.4(5) . . ? C22 P2A Co1A 121.2(5) . . ? C46 P3A C39 103.6(6) . . ? C46 P3A C40 101.9(6) . . ? C39 P3A C40 106.4(6) . . ? C46 P3A Co1A 110.9(4) . . ? C39 P3A Co1A 108.6(4) . . ? C40 P3A Co1A 123.6(4) . . ? C66 P1B C67 106.7(6) . . ? C66 P1B C85 105.7(6) . . ? C67 P1B C85 108.0(7) . . ? C66 P1B Co1B 115.1(5) . . ? C67 P1B Co1B 110.7(5) . . ? C85 P1B Co1B 110.3(4) . . ? C72 P2B C79 104.8(9) . . ? C72 P2B C73 105.4(8) . . ? C79 P2B C73 103.8(8) . . ? C72 P2B Co1B 109.3(6) . . ? C79 P2B Co1B 122.0(6) . . ? C73 P2B Co1B 110.2(5) . . ? C90 P3B C91 103.5(8) . . ? C90 P3B C97 103.1(7) . . ? C91 P3B C97 104.5(7) . . ? C90 P3B Co1B 103.5(6) . . ? C91 P3B Co1B 120.6(6) . . ? C97 P3B Co1B 119.1(6) . . ? N1A Si1A C13 120.9(5) . . ? N1A Si1A C14 111.7(5) . . ? C13 Si1A C14 105.5(6) . . ? N1A Si1A C15 103.2(6) . . ? C13 Si1A C15 102.9(6) . . ? C14 Si1A C15 112.4(6) . . ? N1B Si1B C65 122.1(7) . . ? N1B Si1B C66 103.0(6) . . ? C65 Si1B C66 106.0(7) . . ? N1B Si1B C64 111.3(7) . . ? C65 Si1B C64 104.0(8) . . ? C66 Si1B C64 110.3(7) . . ? C1 N1A Si1A 122.1(8) . . ? C1 N1A Co1A 121.6(7) . . ? Si1A N1A Co1A 115.5(5) . . ? C52 N1B Si1B 122.1(11) . . ? C52 N1B Co1B 121.2(10) . . ? Si1B N1B Co1B 116.4(7) . . ? N1A C1 C2 121.4(12) . . ? N1A C1 C6 121.6(11) . . ? C2 C1 C6 117.1(11) . . ? C3 C2 C1 120.7(13) . . ? C3 C2 C7 121.1(12) . . ? C1 C2 C7 118.3(11) . . ? C4 C3 C2 122.2(14) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 121.7(14) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C4 C5 C6 118.6(14) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C1 C6 C5 119.7(12) . . ? C1 C6 C10 123.0(11) . . ? C5 C6 C10 117.3(13) . . ? C2 C7 C8 114.6(11) . . ? C2 C7 C9 114.1(12) . . ? C8 C7 C9 105.5(11) . . ? C2 C7 H7 107.4 . . ? C8 C7 H7 107.4 . . ? C9 C7 H7 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 108.3(12) . . ? C12 C10 C6 113.5(11) . . ? C11 C10 C6 111.6(11) . . ? C12 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C6 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1A C13 H13A 109.5 . . ? Si1A C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1A C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1A C14 H14A 109.5 . . ? Si1A C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1A C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P1A C15 Si1A 103.8(6) . . ? P1A C15 H15 128.1 . . ? Si1A C15 H15 128.1 . . ? C17 C16 C21 120.8(13) . . ? C17 C16 P1A 123.4(11) . . ? C21 C16 P1A 115.7(10) . . ? C18 C17 C16 118.3(14) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C19 C18 C17 123.4(14) . . ? C19 C18 H18 118.3 . . ? C17 C18 H18 118.3 . . ? C18 C19 C20 118.8(14) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C21 C20 C19 119.8(14) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C16 118.8(13) . . ? C20 C21 P2A 125.7(11) . . ? C16 C21 P2A 115.4(11) . . ? C23 C22 C27 121.5(12) . . ? C23 C22 P2A 120.7(11) . . ? C27 C22 P2A 117.8(10) . . ? C22 C23 C24 120.3(15) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 118.5(16) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 C25 C26 122.1(15) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C25 C26 C27 118.6(16) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C22 C27 C26 118.9(14) . . ? C22 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C29 C28 C33 117.4(13) . . ? C29 C28 P2A 122.5(10) . . ? C33 C28 P2A 120.0(10) . . ? C30 C29 C28 121.1(13) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C31 C30 C29 118.6(14) . . ? C31 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? C32 C31 C30 121.5(15) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C33 C32 C31 119.6(13) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C28 121.5(13) . . ? C32 C33 H33 119.2 . . ? C28 C33 H33 119.2 . . ? C35 C34 C39 118.8(12) . . ? C35 C34 P1A 125.0(10) . . ? C39 C34 P1A 116.2(9) . . ? C36 C35 C34 123.1(14) . . ? C36 C35 H35 118.5 . . ? C34 C35 H35 118.5 . . ? C35 C36 C37 119.6(14) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 118.9(14) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? C39 C38 C37 121.1(13) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C38 C39 C34 118.4(11) . . ? C38 C39 P3A 126.5(10) . . ? C34 C39 P3A 115.1(9) . . ? C45 C40 C41 121.0(12) . . ? C45 C40 P3A 118.7(11) . . ? C41 C40 P3A 120.1(10) . . ? C40 C41 C42 119.1(14) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? C43 C42 C41 119.3(15) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C42 C43 C44 120.9(13) . . ? C42 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C43 C44 C45 118.9(14) . . ? C43 C44 H44 120.6 . . ? C45 C44 H44 120.6 . . ? C40 C45 C44 120.8(14) . . ? C40 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? C51 C46 C47 117.0(13) . . ? C51 C46 P3A 118.6(10) . . ? C47 C46 P3A 124.4(11) . . ? C48 C47 C46 120.8(14) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C49 C48 C47 121.9(14) . . ? C49 C48 H48 119.0 . . ? C47 C48 H48 119.0 . . ? C48 C49 C50 118.3(14) . . ? C48 C49 H49 120.9 . . ? C50 C49 H49 120.9 . . ? C51 C50 C49 121.3(14) . . ? C51 C50 H50 119.4 . . ? C49 C50 H50 119.4 . . ? C46 C51 C50 120.6(13) . . ? C46 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? N1B C52 C57 120.2(17) . . ? N1B C52 C53 120.0(17) . . ? C57 C52 C53 119.7(16) . . ? C54 C53 C52 117.0(15) . . ? C54 C53 C58 119.2(15) . . ? C52 C53 C58 123.5(16) . . ? C55 C54 C53 122.6(15) . . ? C55 C54 H54 118.7 . . ? C53 C54 H54 118.7 . . ? C56 C55 C54 121.4(16) . . ? C56 C55 H55 119.3 . . ? C54 C55 H55 119.3 . . ? C55 C56 C57 119.5(18) . . ? C55 C56 H56 120.3 . . ? C57 C56 H56 120.3 . . ? C52 C57 C56 119.6(17) . . ? C52 C57 C61 122.1(15) . . ? C56 C57 C61 118.1(15) . . ? C53 C58 C59 112.1(13) . . ? C53 C58 C60 112.3(13) . . ? C59 C58 C60 108.6(12) . . ? C53 C58 H58 107.9 . . ? C59 C58 H58 107.9 . . ? C60 C58 H58 107.9 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 C57 113.2(16) . . ? C62 C61 C63 106.4(14) . . ? C57 C61 C63 114.8(15) . . ? C62 C61 H61 107.3 . . ? C57 C61 H61 107.3 . . ? C63 C61 H61 107.3 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? Si1B C64 H64A 109.5 . . ? Si1B C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? Si1B C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Si1B C65 H65A 109.5 . . ? Si1B C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? Si1B C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? P1B C66 Si1B 103.1(7) . . ? P1B C66 H66 128.5 . . ? Si1B C66 H66 128.5 . . ? C68 C67 C72 118.2(14) . . ? C68 C67 P1B 124.9(13) . . ? C72 C67 P1B 116.8(10) . . ? C69 C68 C67 119.7(16) . . ? C69 C68 H68 120.1 . . ? C67 C68 H68 120.1 . . ? C70 C69 C68 121.8(17) . . ? C70 C69 H69 119.1 . . ? C68 C69 H69 119.1 . . ? C71 C70 C69 120.7(18) . . ? C71 C70 H70 119.6 . . ? C69 C70 H70 119.6 . . ? C70 C71 C72 121.3(18) . . ? C70 C71 H71 119.3 . . ? C72 C71 H71 119.4 . . ? C71 C72 C67 118.2(14) . . ? C71 C72 P2B 127.9(15) . . ? C67 C72 P2B 113.5(11) . . ? C78 C73 C74 116.5(16) . . ? C78 C73 P2B 120.8(13) . . ? C74 C73 P2B 122.5(14) . . ? C73 C74 C75 119.8(17) . . ? C73 C74 H74 120.1 . . ? C75 C74 H74 120.1 . . ? C76 C75 C74 119.4(18) . . ? C76 C75 H75 120.3 . . ? C74 C75 H75 120.3 . . ? C77 C76 C75 120.3(19) . . ? C77 C76 H76 119.8 . . ? C75 C76 H76 119.8 . . ? C78 C77 C76 116.7(17) . . ? C78 C77 H77 121.6 . . ? C76 C77 H77 121.6 . . ? C73 C78 C77 126.1(16) . . ? C73 C78 H78 116.9 . . ? C77 C78 H78 116.9 . . ? C80 C79 C84 117.7(16) . . ? C80 C79 P2B 124.8(16) . . ? C84 C79 P2B 117.6(15) . . ? C79 C80 C81 122.6(17) . . ? C79 C80 H80 118.7 . . ? C81 C80 H80 118.7 . . ? C82 C81 C80 118(2) . . ? C82 C81 H81 120.8 . . ? C80 C81 H81 120.8 . . ? C83 C82 C81 122.1(19) . . ? C83 C82 H82 118.9 . . ? C81 C82 H82 118.9 . . ? C82 C83 C84 120.5(18) . . ? C82 C83 H83 119.7 . . ? C84 C83 H83 119.7 . . ? C83 C84 C79 118.6(17) . . ? C83 C84 H84 120.7 . . ? C79 C84 H84 120.7 . . ? C86 C85 C90 123.0(13) . . ? C86 C85 P1B 125.0(10) . . ? C90 C85 P1B 111.7(10) . . ? C85 C86 C87 119.7(13) . . ? C85 C86 H86 120.1 . . ? C87 C86 H86 120.1 . . ? C86 C87 C88 122.3(14) . . ? C86 C87 H87 118.9 . . ? C88 C87 H87 118.9 . . ? C87 C88 C89 118.7(15) . . ? C87 C88 H88 120.7 . . ? C89 C88 H88 120.7 . . ? C90 C89 C88 119.6(15) . . ? C90 C89 H89 120.2 . . ? C88 C89 H89 120.2 . . ? C85 C90 C89 116.0(14) . . ? C85 C90 P3B 119.1(11) . . ? C89 C90 P3B 124.9(12) . . ? C96 C91 C92 121.2(15) . . ? C96 C91 P3B 116.9(12) . . ? C92 C91 P3B 121.3(13) . . ? C93 C92 C91 118.5(16) . . ? C93 C92 H92 120.8 . . ? C91 C92 H92 120.8 . . ? C94 C93 C92 122(2) . . ? C94 C93 H93 118.9 . . ? C92 C93 H93 118.9 . . ? C93 C94 C95 118(2) . . ? C93 C94 H94 120.9 . . ? C95 C94 H94 120.9 . . ? C96 C95 C94 119(2) . . ? C96 C95 H95 120.4 . . ? C94 C95 H95 120.4 . . ? C91 C96 C95 120.3(17) . . ? C91 C96 H96 119.9 . . ? C95 C96 H96 119.9 . . ? C102 C97 C98 119.9(15) . . ? C102 C97 P3B 122.2(12) . . ? C98 C97 P3B 117.5(13) . . ? C99 C98 C97 118.6(16) . . ? C99 C98 H98 120.7 . . ? C97 C98 H98 120.7 . . ? C100 C99 C98 116.2(16) . . ? C100 C99 H99 121.9 . . ? C98 C99 H99 121.9 . . ? C99 C100 C101 124.5(17) . . ? C99 C100 H100 117.8 . . ? C101 C100 H100 117.8 . . ? C102 C101 C100 118.2(18) . . ? C102 C101 H101 120.9 . . ? C100 C101 H101 120.9 . . ? C97 C102 C101 122.3(18) . . ? C97 C102 H102 118.9 . . ? C101 C102 H102 118.9 . . ? _diffrn_measured_fraction_theta_max 0.795 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.795 _refine_diff_density_max 2.294 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.131