# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'David Tyler' _publ_contact_author_email DTYLER@UOREGON.EDU _publ_section_title ; Precursors to Dinitrogen Reduction: Structures and Reactivity of trans-[Fe(DMeOPrPE)2(?2-H2)H]+ and trans-[Fe(DMeOPrPE)2(N2)H]+ ; loop_ _publ_author_name 'David Tyler' 'Justin L. Crossland' 'Douglas M. Young' 'Lev N. Zakharov' # Attachment 'Precursors_Full_Pape_CIFs_-_revised.cif' data_justr2 _database_code_depnum_ccdc_archive 'CCDC 735060' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H103 B Fe O8 P4' _chemical_formula_weight 1142.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 10.8357(10) _cell_length_b 16.9005(16) _cell_length_c 18.2311(17) _cell_angle_alpha 90.013(2) _cell_angle_beta 105.8960(10) _cell_angle_gamma 103.852(2) _cell_volume 3109.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7905 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8839 _exptl_absorpt_correction_T_max 0.9322 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector Bruker Apex' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24706 _diffrn_reflns_av_R_equivalents 0.0130 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.00 _reflns_number_total 13266 _reflns_number_gt 11985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The H2 and H atoms corresponding one of two possible orientations of the Fe atom were found on the residual density and refined with similar occupation factor of 0.88. The second orientation of this fragment corresponding occupation factor of 0.12 was not found and these H atoms were not taken into consideration. ; _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^)+(0.0475P)^2^+1.1037P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13266 _refine_ls_number_parameters 1083 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Fe1 Fe 0.25964(18) 0.30138(6) 0.27858(4) 0.01458(17) Uani 0.880(8) 1 d P . . Fe1A Fe 0.2909(8) 0.3109(3) 0.2731(2) 0.01458(17) Uani 0.120(8) 1 d P . . P1 P 0.20574(3) 0.420919(19) 0.267955(18) 0.01419(7) Uani 1 1 d . . . P2 P 0.36671(3) 0.346474(19) 0.399268(18) 0.01468(7) Uani 1 1 d . . . P3 P 0.33280(3) 0.188779(19) 0.286742(18) 0.01499(7) Uani 1 1 d . . . P4 P 0.17751(3) 0.264088(19) 0.154833(18) 0.01494(7) Uani 1 1 d . . . O1 O -0.18512(10) 0.47611(6) 0.26191(6) 0.0257(2) Uani 1 1 d . . . O2 O 0.51684(10) 0.64622(6) 0.22377(7) 0.0306(2) Uani 1 1 d . . . O3 O 0.12320(11) 0.25921(7) 0.57107(7) 0.0337(3) Uani 1 1 d . . . O4 O 0.82726(9) 0.42016(6) 0.51642(6) 0.0239(2) Uani 1 1 d . . . O5 O 0.26464(11) 0.08425(7) 0.51042(6) 0.0312(2) Uani 1 1 d . . . O6 O 0.75503(10) 0.16947(7) 0.37425(6) 0.0307(2) Uani 1 1 d . . . O7 O -0.26916(9) 0.22282(6) 0.12102(6) 0.0241(2) Uani 1 1 d . . . O8 O 0.55132(10) 0.41821(6) 0.04288(6) 0.0270(2) Uani 1 1 d . . . C1 C 0.23204(13) 0.46402(8) 0.36545(7) 0.0174(2) Uani 1 1 d . . . C2 C 0.36635(13) 0.45463(8) 0.41249(7) 0.0174(2) Uani 1 1 d . . . C3 C 0.23837(13) 0.11914(8) 0.20142(8) 0.0190(3) Uani 1 1 d . . . C4 C 0.22446(14) 0.17046(8) 0.13252(8) 0.0196(3) Uani 1 1 d . . . C5 C 0.03700(12) 0.43003(8) 0.22134(7) 0.0168(2) Uani 1 1 d . . . C6 C -0.07176(13) 0.37459(8) 0.24997(8) 0.0189(3) Uani 1 1 d . . . C7 C -0.20221(13) 0.39911(9) 0.22426(8) 0.0226(3) Uani 1 1 d . . . C8 C -0.30138(17) 0.50577(12) 0.23890(11) 0.0338(4) Uani 1 1 d . . . C9 C 0.30600(13) 0.50376(8) 0.22697(8) 0.0180(3) Uani 1 1 d . . . C10 C 0.30926(15) 0.59132(8) 0.25040(9) 0.0238(3) Uani 1 1 d . . . C11 C 0.38567(14) 0.65500(9) 0.21008(9) 0.0261(3) Uani 1 1 d . . . C12 C 0.59637(17) 0.71281(12) 0.19657(11) 0.0386(4) Uani 1 1 d . . . C13 C 0.28595(13) 0.29737(8) 0.46992(7) 0.0193(3) Uani 1 1 d . . . C14 C 0.31840(17) 0.34177(10) 0.54838(9) 0.0306(3) Uani 1 1 d . . . C15 C 0.26178(17) 0.28585(11) 0.60269(9) 0.0327(3) Uani 1 1 d . . . C16 C 0.0652(2) 0.20448(13) 0.61870(13) 0.0453(4) Uani 1 1 d . . . C17 C 0.54082(12) 0.34695(8) 0.44486(7) 0.0171(2) Uani 1 1 d . . . C18 C 0.64080(13) 0.39380(8) 0.40545(8) 0.0206(3) Uani 1 1 d . . . C19 C 0.77961(14) 0.38356(9) 0.44049(8) 0.0235(3) Uani 1 1 d . . . C20 C 0.95529(15) 0.40920(11) 0.55403(10) 0.0323(3) Uani 1 1 d . . . C21 C 0.31977(13) 0.12293(8) 0.36570(8) 0.0184(3) Uani 1 1 d . . . C22 C 0.18148(13) 0.09769(8) 0.37727(8) 0.0219(3) Uani 1 1 d . . . C23 C 0.17639(15) 0.04170(9) 0.44190(9) 0.0280(3) Uani 1 1 d . . . C24 C 0.2644(2) 0.03638(14) 0.57418(11) 0.0446(5) Uani 1 1 d . . . C25 C 0.50576(13) 0.19963(8) 0.28672(8) 0.0190(3) Uani 1 1 d . . . C26 C 0.55077(14) 0.12172(9) 0.27884(9) 0.0254(3) Uani 1 1 d . . . C27 C 0.70006(15) 0.13927(10) 0.29689(9) 0.0260(3) Uani 1 1 d . . . C28 C 0.89547(17) 0.18715(12) 0.39619(13) 0.0427(4) Uani 1 1 d . . . C29 C -0.00262(13) 0.23537(8) 0.11157(7) 0.0182(3) Uani 1 1 d . . . C30 C -0.08231(13) 0.16474(8) 0.14495(8) 0.0207(3) Uani 1 1 d . . . C31 C -0.22947(13) 0.15117(8) 0.10613(9) 0.0225(3) Uani 1 1 d . . . C32 C -0.40094(15) 0.21870(11) 0.07822(11) 0.0326(3) Uani 1 1 d . . . C33 C 0.22565(13) 0.32955(8) 0.08167(7) 0.0192(3) Uani 1 1 d . . . C34 C 0.37531(14) 0.36437(9) 0.09676(8) 0.0222(3) Uani 1 1 d . . . C35 C 0.41513(14) 0.37600(9) 0.02326(8) 0.0248(3) Uani 1 1 d . . . C36 C 0.60383(17) 0.42043(11) -0.02078(10) 0.0333(3) Uani 1 1 d . . . B1 B 0.88356(14) 0.16802(9) 0.82291(8) 0.0162(3) Uani 1 1 d . . . C37 C 0.78898(12) 0.17011(8) 0.73513(7) 0.0168(2) Uani 1 1 d . . . C38 C 0.69713(14) 0.09912(8) 0.69527(8) 0.0219(3) Uani 1 1 d . . . C39 C 0.62107(15) 0.09753(9) 0.61995(9) 0.0276(3) Uani 1 1 d . . . C40 C 0.63260(16) 0.16812(10) 0.58082(9) 0.0304(3) Uani 1 1 d . . . C41 C 0.72126(15) 0.23941(9) 0.61784(8) 0.0269(3) Uani 1 1 d . . . C42 C 0.79750(13) 0.23968(8) 0.69302(8) 0.0200(3) Uani 1 1 d . . . C43 C 0.93375(12) 0.26074(8) 0.86552(7) 0.0163(2) Uani 1 1 d . . . C44 C 1.03524(13) 0.32055(8) 0.84830(8) 0.0197(3) Uani 1 1 d . . . C45 C 1.07539(14) 0.40049(8) 0.88031(8) 0.0211(3) Uani 1 1 d . . . C46 C 1.01586(14) 0.42400(8) 0.93249(8) 0.0209(3) Uani 1 1 d . . . C47 C 0.91746(13) 0.36649(8) 0.95192(8) 0.0201(3) Uani 1 1 d . . . C48 C 0.87749(13) 0.28663(8) 0.91882(7) 0.0171(2) Uani 1 1 d . . . C49 C 0.80030(13) 0.10559(7) 0.87227(7) 0.0168(2) Uani 1 1 d . . . C50 C 0.66395(13) 0.09594(8) 0.86227(8) 0.0215(3) Uani 1 1 d . . . C51 C 0.59371(14) 0.04381(9) 0.90426(8) 0.0244(3) Uani 1 1 d . . . C52 C 0.65768(14) -0.00124(8) 0.95915(8) 0.0222(3) Uani 1 1 d . . . C53 C 0.79263(14) 0.00807(8) 0.97219(8) 0.0209(3) Uani 1 1 d . . . C54 C 0.86142(13) 0.06008(8) 0.92942(7) 0.0185(3) Uani 1 1 d . . . C55 C 1.01312(12) 0.13495(7) 0.81872(7) 0.0167(2) Uani 1 1 d . . . C56 C 1.13440(13) 0.15579(8) 0.87645(8) 0.0202(3) Uani 1 1 d . . . C57 C 1.24283(14) 0.12552(9) 0.87463(8) 0.0235(3) Uani 1 1 d . . . C58 C 1.23371(14) 0.07257(9) 0.81462(9) 0.0250(3) Uani 1 1 d . . . C59 C 1.11575(14) 0.04993(9) 0.75679(9) 0.0246(3) Uani 1 1 d . . . C60 C 1.00859(13) 0.08091(8) 0.75922(8) 0.0205(3) Uani 1 1 d . . . H1 H 0.3888(19) 0.3478(11) 0.2597(11) 0.028(5) Uiso 0.880(8) 1 d P . . H2 H 0.144(3) 0.2414(19) 0.2963(17) 0.066(9) Uiso 0.880(8) 1 d P . . H3 H 0.129(3) 0.2788(17) 0.2980(15) 0.049(7) Uiso 0.880(8) 1 d P . . H1A H 0.2274(15) 0.5195(10) 0.3661(9) 0.021(4) Uiso 1 1 d . . . H1B H 0.1623(16) 0.4311(10) 0.3845(9) 0.023(4) Uiso 1 1 d . . . H2A H 0.4344(15) 0.4869(9) 0.3927(9) 0.019(4) Uiso 1 1 d . . . H2B H 0.3854(16) 0.4707(10) 0.4658(10) 0.025(4) Uiso 1 1 d . . . H3A H 0.2800(18) 0.0783(11) 0.1977(10) 0.033(5) Uiso 1 1 d . . . H3B H 0.1540(17) 0.0935(10) 0.2088(9) 0.023(4) Uiso 1 1 d . . . H4A H 0.3102(18) 0.1873(10) 0.1195(10) 0.030(4) Uiso 1 1 d . . . H4B H 0.1596(18) 0.1421(11) 0.0878(10) 0.032(5) Uiso 1 1 d . . . H5A H 0.0382(16) 0.4881(10) 0.2305(9) 0.023(4) Uiso 1 1 d . . . H5B H 0.0162(16) 0.4188(10) 0.1668(10) 0.025(4) Uiso 1 1 d . . . H6A H -0.0453(15) 0.3774(9) 0.3051(9) 0.020(4) Uiso 1 1 d . . . H6B H -0.0842(16) 0.3197(10) 0.2322(9) 0.024(4) Uiso 1 1 d . . . H7A H -0.2742(16) 0.3576(10) 0.2361(9) 0.025(4) Uiso 1 1 d . . . H7B H -0.2301(16) 0.4033(10) 0.1671(10) 0.025(4) Uiso 1 1 d . . . H8A H -0.3253(18) 0.5119(11) 0.1845(11) 0.037(5) Uiso 1 1 d . . . H8B H -0.2766(18) 0.5566(12) 0.2677(11) 0.038(5) Uiso 1 1 d . . . H8C H -0.379(2) 0.4666(13) 0.2510(12) 0.049(6) Uiso 1 1 d . . . H9A H 0.3945(16) 0.4965(9) 0.2392(9) 0.021(4) Uiso 1 1 d . . . H9B H 0.2706(16) 0.4938(10) 0.1712(10) 0.026(4) Uiso 1 1 d . . . H10A H 0.2240(19) 0.5993(11) 0.2399(10) 0.037(5) Uiso 1 1 d . . . H10B H 0.3507(18) 0.6016(11) 0.3058(11) 0.034(5) Uiso 1 1 d . . . H11A H 0.3860(17) 0.7114(11) 0.2274(10) 0.033(5) Uiso 1 1 d . . . H11B H 0.3459(18) 0.6487(11) 0.1540(11) 0.035(5) Uiso 1 1 d . . . H12A H 0.681(2) 0.7028(13) 0.2017(13) 0.057(6) Uiso 1 1 d . . . H12B H 0.605(2) 0.7624(14) 0.2286(12) 0.051(6) Uiso 1 1 d . . . H12C H 0.557(2) 0.7153(13) 0.1396(13) 0.054(6) Uiso 1 1 d . . . H13A H 0.1889(17) 0.2865(10) 0.4464(9) 0.026(4) Uiso 1 1 d . . . H13B H 0.3043(16) 0.2461(11) 0.4764(9) 0.025(4) Uiso 1 1 d . . . H14A H 0.2825(19) 0.3936(13) 0.5442(11) 0.045(5) Uiso 1 1 d . . . H14B H 0.413(2) 0.3577(12) 0.5716(11) 0.040(5) Uiso 1 1 d . . . H15A H 0.282(2) 0.3160(12) 0.6538(12) 0.048(6) Uiso 1 1 d . . . H15B H 0.3016(17) 0.2393(11) 0.6109(10) 0.028(4) Uiso 1 1 d . . . H16A H 0.084(2) 0.2312(14) 0.6703(14) 0.063(7) Uiso 1 1 d . . . H16B H -0.034(2) 0.1862(14) 0.5912(13) 0.061(7) Uiso 1 1 d . . . H16C H 0.103(2) 0.1542(14) 0.6230(12) 0.053(6) Uiso 1 1 d . . . H17A H 0.5445(16) 0.2911(11) 0.4479(9) 0.024(4) Uiso 1 1 d . . . H17B H 0.5631(15) 0.3669(10) 0.4963(10) 0.021(4) Uiso 1 1 d . . . H18A H 0.6150(16) 0.3755(10) 0.3537(10) 0.025(4) Uiso 1 1 d . . . H18B H 0.6430(16) 0.4535(10) 0.4075(9) 0.025(4) Uiso 1 1 d . . . H19A H 0.8396(17) 0.4084(10) 0.4104(10) 0.030(4) Uiso 1 1 d . . . H19B H 0.7809(16) 0.3248(10) 0.4433(9) 0.024(4) Uiso 1 1 d . . . H20A H 0.9522(18) 0.3514(12) 0.5556(10) 0.035(5) Uiso 1 1 d . . . H20B H 0.9827(18) 0.4360(11) 0.6047(11) 0.034(5) Uiso 1 1 d . . . H20C H 1.017(2) 0.4328(12) 0.5253(11) 0.043(5) Uiso 1 1 d . . . H21A H 0.3831(15) 0.1533(9) 0.4110(9) 0.018(4) Uiso 1 1 d . . . H21B H 0.3488(16) 0.0743(10) 0.3570(9) 0.025(4) Uiso 1 1 d . . . H22A H 0.1522(16) 0.1461(10) 0.3886(9) 0.024(4) Uiso 1 1 d . . . H22B H 0.1184(17) 0.0695(10) 0.3322(10) 0.028(4) Uiso 1 1 d . . . H23A H 0.0839(17) 0.0251(10) 0.4488(10) 0.030(4) Uiso 1 1 d . . . H23B H 0.2042(17) -0.0086(11) 0.4328(10) 0.033(5) Uiso 1 1 d . . . H24A H 0.332(2) 0.0686(12) 0.6183(12) 0.043(5) Uiso 1 1 d . . . H24B H 0.292(2) -0.0153(14) 0.5644(13) 0.060(7) Uiso 1 1 d . . . H24C H 0.174(2) 0.0230(12) 0.5836(11) 0.044(5) Uiso 1 1 d . . . H25A H 0.5215(17) 0.2367(11) 0.2451(10) 0.032(5) Uiso 1 1 d . . . H25B H 0.5588(16) 0.2303(10) 0.3329(10) 0.024(4) Uiso 1 1 d . . . H26A H 0.5099(18) 0.0956(11) 0.2269(11) 0.037(5) Uiso 1 1 d . . . H26B H 0.5249(18) 0.0833(11) 0.3131(11) 0.034(5) Uiso 1 1 d . . . H27A H 0.7281(17) 0.0896(11) 0.2900(10) 0.033(5) Uiso 1 1 d . . . H27B H 0.7334(17) 0.1786(11) 0.2648(10) 0.029(4) Uiso 1 1 d . . . H28A H 0.925(2) 0.2062(14) 0.4504(14) 0.063(7) Uiso 1 1 d . . . H28B H 0.935(3) 0.2297(16) 0.3620(15) 0.076(8) Uiso 1 1 d . . . H28C H 0.923(2) 0.1355(14) 0.3915(12) 0.055(6) Uiso 1 1 d . . . H29A H -0.0170(15) 0.2217(10) 0.0586(10) 0.022(4) Uiso 1 1 d . . . H29B H -0.0326(16) 0.2838(10) 0.1158(9) 0.024(4) Uiso 1 1 d . . . H30A H -0.0648(15) 0.1749(10) 0.2002(10) 0.022(4) Uiso 1 1 d . . . H30B H -0.0578(16) 0.1150(11) 0.1369(10) 0.028(4) Uiso 1 1 d . . . H31A H -0.2820(15) 0.1042(10) 0.1255(9) 0.019(4) Uiso 1 1 d . . . H31B H -0.2478(16) 0.1413(10) 0.0502(10) 0.022(4) Uiso 1 1 d . . . H32A H -0.4650(19) 0.1735(12) 0.0927(11) 0.039(5) Uiso 1 1 d . . . H32B H -0.4194(18) 0.2725(12) 0.0893(11) 0.039(5) Uiso 1 1 d . . . H32C H -0.4096(18) 0.2086(11) 0.0249(11) 0.034(5) Uiso 1 1 d . . . H33A H 0.1807(16) 0.3736(10) 0.0758(9) 0.026(4) Uiso 1 1 d . . . H33B H 0.1907(16) 0.2959(10) 0.0332(10) 0.026(4) Uiso 1 1 d . . . H34A H 0.4042(16) 0.4174(11) 0.1267(9) 0.026(4) Uiso 1 1 d . . . H34B H 0.4246(17) 0.3266(11) 0.1285(10) 0.031(4) Uiso 1 1 d . . . H35A H 0.4002(17) 0.3227(11) -0.0046(10) 0.029(4) Uiso 1 1 d . . . H35B H 0.3598(17) 0.4070(11) -0.0115(10) 0.031(4) Uiso 1 1 d . . . H36A H 0.5478(19) 0.4414(12) -0.0668(12) 0.041(5) Uiso 1 1 d . . . H36B H 0.6948(18) 0.4572(11) -0.0057(10) 0.031(4) Uiso 1 1 d . . . H36C H 0.6057(19) 0.3635(12) -0.0368(11) 0.043(5) Uiso 1 1 d . . . H38 H 0.6875(16) 0.0508(11) 0.7200(10) 0.026(4) Uiso 1 1 d . . . H39 H 0.5614(18) 0.0471(12) 0.5953(11) 0.036(5) Uiso 1 1 d . . . H40 H 0.5799(19) 0.1657(12) 0.5291(11) 0.042(5) Uiso 1 1 d . . . H41 H 0.7312(17) 0.2866(11) 0.5918(10) 0.031(4) Uiso 1 1 d . . . H42 H 0.8565(16) 0.2899(10) 0.7153(9) 0.024(4) Uiso 1 1 d . . . H44 H 1.0802(16) 0.3067(10) 0.8130(10) 0.027(4) Uiso 1 1 d . . . H45 H 1.1441(16) 0.4378(10) 0.8665(9) 0.024(4) Uiso 1 1 d . . . H46 H 1.0428(16) 0.4790(11) 0.9553(9) 0.026(4) Uiso 1 1 d . . . H47 H 0.8723(15) 0.3799(9) 0.9869(9) 0.020(4) Uiso 1 1 d . . . H48 H 0.8098(15) 0.2495(9) 0.9331(8) 0.013(3) Uiso 1 1 d . . . H50 H 0.6157(16) 0.1256(10) 0.8258(9) 0.023(4) Uiso 1 1 d . . . H51 H 0.5027(18) 0.0397(11) 0.8937(10) 0.032(5) Uiso 1 1 d . . . H52 H 0.6101(16) -0.0356(10) 0.9861(10) 0.026(4) Uiso 1 1 d . . . H53 H 0.8393(16) -0.0208(10) 1.0125(10) 0.026(4) Uiso 1 1 d . . . H54 H 0.9524(16) 0.0629(9) 0.9383(9) 0.019(4) Uiso 1 1 d . . . H56 H 1.1445(16) 0.1906(10) 0.9175(10) 0.024(4) Uiso 1 1 d . . . H57 H 1.3226(16) 0.1421(10) 0.9144(9) 0.024(4) Uiso 1 1 d . . . H58 H 1.3077(18) 0.0522(10) 0.8121(10) 0.030(4) Uiso 1 1 d . . . H59 H 1.1078(16) 0.0129(10) 0.7135(10) 0.029(4) Uiso 1 1 d . . . H60 H 0.9291(16) 0.0657(10) 0.7174(9) 0.024(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0175(4) 0.01232(15) 0.01286(12) -0.00053(10) 0.00076(16) 0.0058(2) Fe1A 0.0175(4) 0.01232(15) 0.01286(12) -0.00053(10) 0.00076(16) 0.0058(2) P1 0.01554(15) 0.01253(15) 0.01451(15) 0.00071(11) 0.00330(12) 0.00462(11) P2 0.01597(15) 0.01294(15) 0.01344(15) 0.00022(12) 0.00188(12) 0.00306(11) P3 0.01566(15) 0.01271(15) 0.01558(15) -0.00007(12) 0.00168(12) 0.00475(11) P4 0.01605(15) 0.01517(15) 0.01329(15) 0.00005(12) 0.00232(12) 0.00540(12) O1 0.0235(5) 0.0263(5) 0.0302(5) 0.0000(4) 0.0073(4) 0.0119(4) O2 0.0194(5) 0.0278(5) 0.0424(6) 0.0147(5) 0.0087(4) 0.0020(4) O3 0.0338(6) 0.0363(6) 0.0393(6) 0.0149(5) 0.0215(5) 0.0117(5) O4 0.0184(5) 0.0265(5) 0.0250(5) -0.0041(4) 0.0030(4) 0.0058(4) O5 0.0357(6) 0.0328(6) 0.0258(5) 0.0091(4) 0.0109(5) 0.0070(5) O6 0.0211(5) 0.0390(6) 0.0314(6) -0.0001(5) 0.0025(4) 0.0122(4) O7 0.0188(5) 0.0204(5) 0.0306(5) -0.0051(4) 0.0023(4) 0.0056(4) O8 0.0235(5) 0.0317(6) 0.0273(5) 0.0008(4) 0.0115(4) 0.0047(4) C1 0.0207(6) 0.0147(6) 0.0174(6) -0.0011(5) 0.0055(5) 0.0053(5) C2 0.0211(6) 0.0132(6) 0.0160(6) -0.0017(5) 0.0034(5) 0.0028(5) C3 0.0198(6) 0.0152(6) 0.0200(6) -0.0025(5) 0.0011(5) 0.0061(5) C4 0.0223(7) 0.0189(6) 0.0176(6) -0.0040(5) 0.0033(5) 0.0077(5) C5 0.0165(6) 0.0161(6) 0.0178(6) 0.0021(5) 0.0031(5) 0.0059(5) C6 0.0183(6) 0.0170(6) 0.0210(7) 0.0007(5) 0.0055(5) 0.0040(5) C7 0.0173(6) 0.0237(7) 0.0253(7) 0.0012(6) 0.0053(5) 0.0034(5) C8 0.0323(8) 0.0426(10) 0.0379(9) 0.0129(8) 0.0163(7) 0.0231(7) C9 0.0170(6) 0.0165(6) 0.0216(6) 0.0015(5) 0.0075(5) 0.0037(5) C10 0.0253(7) 0.0156(6) 0.0330(8) 0.0024(6) 0.0130(6) 0.0044(5) C11 0.0237(7) 0.0204(7) 0.0354(8) 0.0081(6) 0.0100(6) 0.0060(5) C12 0.0274(8) 0.0390(10) 0.0420(10) 0.0145(8) 0.0085(7) -0.0045(7) C13 0.0204(7) 0.0180(6) 0.0178(6) 0.0014(5) 0.0054(5) 0.0018(5) C14 0.0371(9) 0.0286(8) 0.0216(7) -0.0037(6) 0.0121(6) -0.0050(7) C15 0.0391(9) 0.0351(9) 0.0214(7) 0.0020(6) 0.0116(6) 0.0010(7) C16 0.0468(11) 0.0462(11) 0.0547(12) 0.0201(9) 0.0332(10) 0.0118(9) C17 0.0167(6) 0.0165(6) 0.0159(6) 0.0006(5) 0.0013(5) 0.0040(5) C18 0.0228(7) 0.0183(6) 0.0193(6) -0.0009(5) 0.0059(5) 0.0023(5) C19 0.0208(7) 0.0233(7) 0.0268(7) -0.0052(6) 0.0094(6) 0.0030(5) C20 0.0202(7) 0.0346(9) 0.0388(9) 0.0031(7) 0.0027(7) 0.0071(6) C21 0.0200(6) 0.0155(6) 0.0198(6) 0.0024(5) 0.0049(5) 0.0053(5) C22 0.0198(6) 0.0179(6) 0.0258(7) -0.0004(5) 0.0055(5) 0.0018(5) C23 0.0275(8) 0.0228(7) 0.0350(8) 0.0055(6) 0.0136(6) 0.0030(6) C24 0.0415(10) 0.0601(13) 0.0388(10) 0.0262(9) 0.0183(8) 0.0167(9) C25 0.0176(6) 0.0184(6) 0.0210(6) 0.0009(5) 0.0045(5) 0.0056(5) C26 0.0223(7) 0.0226(7) 0.0318(8) -0.0041(6) 0.0064(6) 0.0078(5) C27 0.0248(7) 0.0283(8) 0.0299(8) 0.0028(6) 0.0111(6) 0.0119(6) C28 0.0224(8) 0.0415(10) 0.0582(12) 0.0050(9) -0.0003(8) 0.0102(7) C29 0.0168(6) 0.0205(6) 0.0158(6) -0.0004(5) 0.0013(5) 0.0055(5) C30 0.0197(6) 0.0180(6) 0.0224(7) 0.0005(5) 0.0031(5) 0.0046(5) C31 0.0196(6) 0.0168(6) 0.0283(7) -0.0034(5) 0.0034(5) 0.0030(5) C32 0.0197(7) 0.0320(8) 0.0429(10) -0.0049(7) 0.0021(7) 0.0082(6) C33 0.0204(6) 0.0208(6) 0.0171(6) 0.0034(5) 0.0053(5) 0.0064(5) C34 0.0212(7) 0.0241(7) 0.0226(7) 0.0022(6) 0.0073(5) 0.0069(5) C35 0.0228(7) 0.0280(7) 0.0243(7) 0.0015(6) 0.0084(6) 0.0057(6) C36 0.0316(8) 0.0367(9) 0.0367(9) 0.0024(7) 0.0196(7) 0.0066(7) B1 0.0169(7) 0.0150(6) 0.0164(6) 0.0011(5) 0.0043(5) 0.0042(5) C37 0.0169(6) 0.0179(6) 0.0174(6) 0.0019(5) 0.0051(5) 0.0075(5) C38 0.0231(7) 0.0185(6) 0.0226(7) 0.0031(5) 0.0032(5) 0.0063(5) C39 0.0277(7) 0.0242(7) 0.0249(7) -0.0006(6) -0.0016(6) 0.0055(6) C40 0.0311(8) 0.0334(8) 0.0209(7) 0.0045(6) -0.0040(6) 0.0105(6) C41 0.0301(8) 0.0262(7) 0.0249(7) 0.0096(6) 0.0059(6) 0.0100(6) C42 0.0212(6) 0.0187(6) 0.0210(6) 0.0022(5) 0.0063(5) 0.0062(5) C43 0.0172(6) 0.0152(6) 0.0153(6) 0.0029(5) 0.0014(5) 0.0050(5) C44 0.0224(6) 0.0182(6) 0.0196(6) 0.0024(5) 0.0077(5) 0.0053(5) C45 0.0218(7) 0.0166(6) 0.0235(7) 0.0042(5) 0.0063(5) 0.0023(5) C46 0.0243(7) 0.0144(6) 0.0213(6) -0.0005(5) 0.0019(5) 0.0049(5) C47 0.0222(6) 0.0212(7) 0.0173(6) -0.0003(5) 0.0041(5) 0.0079(5) C48 0.0170(6) 0.0167(6) 0.0167(6) 0.0035(5) 0.0031(5) 0.0043(5) C49 0.0202(6) 0.0125(6) 0.0167(6) -0.0018(5) 0.0046(5) 0.0028(5) C50 0.0199(6) 0.0227(7) 0.0201(6) 0.0034(5) 0.0033(5) 0.0047(5) C51 0.0182(7) 0.0281(7) 0.0237(7) 0.0000(6) 0.0053(5) 0.0005(5) C52 0.0288(7) 0.0168(6) 0.0200(6) 0.0003(5) 0.0107(6) -0.0007(5) C53 0.0311(7) 0.0159(6) 0.0188(6) 0.0025(5) 0.0094(5) 0.0088(5) C54 0.0206(6) 0.0174(6) 0.0188(6) 0.0008(5) 0.0064(5) 0.0065(5) C55 0.0181(6) 0.0135(6) 0.0191(6) 0.0053(5) 0.0066(5) 0.0032(5) C56 0.0216(7) 0.0191(6) 0.0192(6) 0.0027(5) 0.0047(5) 0.0047(5) C57 0.0184(6) 0.0244(7) 0.0255(7) 0.0089(6) 0.0033(5) 0.0046(5) C58 0.0211(7) 0.0238(7) 0.0342(8) 0.0097(6) 0.0115(6) 0.0092(5) C59 0.0266(7) 0.0221(7) 0.0282(7) -0.0002(6) 0.0101(6) 0.0090(6) C60 0.0200(6) 0.0199(6) 0.0210(6) 0.0006(5) 0.0044(5) 0.0054(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 Fe1 P4 2.2158(6) . ? Fe1 P3 2.2203(5) . ? Fe1 P2 2.2239(5) . ? Fe1 P1 2.2278(5) . ? Fe1 H1 1.559(19) . ? Fe1 H2 1.52(3) . ? Fe1 H3 1.51(3) . ? Fe1A P4 2.207(4) . ? Fe1A P3 2.217(4) . ? Fe1A P2 2.248(4) . ? Fe1A P1 2.256(4) . ? Fe1A H1 1.183(19) . ? Fe1A H2 1.89(3) . ? Fe1A H3 1.89(3) . ? P1 C5 1.8365(13) . ? P1 C1 1.8422(13) . ? P1 C9 1.8482(13) . ? P2 C13 1.8395(14) . ? P2 C17 1.8395(13) . ? P2 C2 1.8447(13) . ? P3 C21 1.8351(13) . ? P3 C25 1.8390(14) . ? P3 C3 1.8446(13) . ? P4 C29 1.8358(13) . ? P4 C33 1.8387(14) . ? P4 C4 1.8511(13) . ? O1 C7 1.4191(17) . ? O1 C8 1.4238(18) . ? O2 C11 1.4181(17) . ? O2 C12 1.4230(18) . ? O3 C15 1.411(2) . ? O3 C16 1.423(2) . ? O4 C19 1.4216(17) . ? O4 C20 1.4251(17) . ? O5 C24 1.416(2) . ? O5 C23 1.4170(19) . ? O6 C27 1.4136(19) . ? O6 C28 1.4191(19) . ? O7 C32 1.4124(17) . ? O7 C31 1.4276(16) . ? O8 C35 1.4217(17) . ? O8 C36 1.4226(18) . ? C1 C2 1.5186(18) . ? C1 H1A 0.951(16) . ? C1 H1B 0.971(17) . ? C2 H2A 0.961(16) . ? C2 H2B 0.961(17) . ? C3 C4 1.5206(19) . ? C3 H3A 0.922(19) . ? C3 H3B 0.959(17) . ? C4 H4A 0.997(18) . ? C4 H4B 0.956(18) . ? C5 C6 1.5322(18) . ? C5 H5A 0.991(17) . ? C5 H5B 0.965(17) . ? C6 C7 1.5188(18) . ? C6 H6A 0.965(16) . ? C6 H6B 0.948(17) . ? C7 H7A 0.989(17) . ? C7 H7B 1.010(17) . ? C8 H8A 0.97(2) . ? C8 H8B 0.95(2) . ? C8 H8C 1.02(2) . ? C9 C10 1.5298(18) . ? C9 H9A 0.961(16) . ? C9 H9B 0.982(17) . ? C10 C11 1.5136(19) . ? C10 H10A 0.933(19) . ? C10 H10B 0.983(19) . ? C11 H11A 1.003(18) . ? C11 H11B 0.989(19) . ? C12 H12A 0.95(2) . ? C12 H12B 0.99(2) . ? C12 H12C 1.01(2) . ? C13 C14 1.5266(19) . ? C13 H13A 0.992(17) . ? C13 H13B 0.935(17) . ? C14 C15 1.518(2) . ? C14 H14A 1.03(2) . ? C14 H14B 0.97(2) . ? C15 H15A 1.01(2) . ? C15 H15B 0.977(18) . ? C16 H16A 0.99(2) . ? C16 H16B 1.03(2) . ? C16 H16C 1.02(2) . ? C17 C18 1.5275(18) . ? C17 H17A 0.955(17) . ? C17 H17B 0.942(17) . ? C18 C19 1.5162(19) . ? C18 H18A 0.937(17) . ? C18 H18B 1.004(17) . ? C19 H19A 0.982(18) . ? C19 H19B 0.998(17) . ? C20 H20A 0.971(19) . ? C20 H20B 0.966(19) . ? C20 H20C 0.98(2) . ? C21 C22 1.5294(19) . ? C21 H21A 0.969(16) . ? C21 H21B 0.975(17) . ? C22 C23 1.516(2) . ? C22 H22A 0.987(17) . ? C22 H22B 0.951(17) . ? C23 H23A 1.016(18) . ? C23 H23B 0.996(19) . ? C24 H24A 0.98(2) . ? C24 H24B 1.02(2) . ? C24 H24C 1.01(2) . ? C25 C26 1.5291(19) . ? C25 H25A 1.008(18) . ? C25 H25B 0.949(17) . ? C26 C27 1.514(2) . ? C26 H26A 0.981(19) . ? C26 H26B 0.948(19) . ? C27 H27A 0.977(19) . ? C27 H27B 0.957(18) . ? C28 H28A 0.98(2) . ? C28 H28B 1.04(3) . ? C28 H28C 1.00(2) . ? C29 C30 1.5282(19) . ? C29 H29A 0.955(16) . ? C29 H29B 0.961(17) . ? C30 C31 1.5175(18) . ? C30 H30A 0.979(16) . ? C30 H30B 0.963(18) . ? C31 H31A 0.986(16) . ? C31 H31B 0.990(17) . ? C32 H32A 0.99(2) . ? C32 H32B 1.008(19) . ? C32 H32C 0.961(19) . ? C33 C34 1.5330(19) . ? C33 H33A 0.974(17) . ? C33 H33B 0.980(17) . ? C34 C35 1.515(2) . ? C34 H34A 0.985(17) . ? C34 H34B 1.011(18) . ? C35 H35A 0.990(18) . ? C35 H35B 0.990(18) . ? C36 H36A 1.01(2) . ? C36 H36B 0.996(18) . ? C36 H36C 1.01(2) . ? B1 C43 1.6475(18) . ? B1 C55 1.6504(19) . ? B1 C49 1.6512(19) . ? B1 C37 1.6527(19) . ? C37 C42 1.4027(18) . ? C37 C38 1.4107(19) . ? C38 C39 1.391(2) . ? C38 H38 0.930(17) . ? C39 C40 1.388(2) . ? C39 H39 0.961(19) . ? C40 C41 1.386(2) . ? C40 H40 0.95(2) . ? C41 C42 1.3926(19) . ? C41 H41 0.927(18) . ? C42 H42 0.945(17) . ? C43 C48 1.3998(18) . ? C43 C44 1.4096(18) . ? C44 C45 1.3907(19) . ? C44 H44 0.965(17) . ? C45 C46 1.392(2) . ? C45 H45 0.946(17) . ? C46 C47 1.385(2) . ? C46 H46 0.962(17) . ? C47 C48 1.3964(18) . ? C47 H47 0.960(16) . ? C48 H48 0.939(15) . ? C49 C50 1.4070(19) . ? C49 C54 1.4079(18) . ? C50 C51 1.393(2) . ? C50 H50 0.950(17) . ? C51 C52 1.391(2) . ? C51 H51 0.937(18) . ? C52 C53 1.385(2) . ? C52 H52 0.917(17) . ? C53 C54 1.3933(19) . ? C53 H53 0.974(17) . ? C54 H54 0.944(16) . ? C55 C60 1.4008(19) . ? C55 C56 1.4069(18) . ? C56 C57 1.3973(19) . ? C56 H56 0.918(17) . ? C57 C58 1.380(2) . ? C57 H57 0.944(17) . ? C58 C59 1.385(2) . ? C58 H58 0.957(18) . ? C59 C60 1.3942(19) . ? C59 H59 0.980(17) . ? C60 H60 0.961(17) . ? 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 P4 Fe1 P3 85.37(2) . . ? P4 Fe1 P2 172.49(11) . . ? P3 Fe1 P2 93.986(19) . . ? P4 Fe1 P1 94.43(2) . . ? P3 Fe1 P1 174.09(11) . . ? P2 Fe1 P1 85.440(17) . . ? P4 Fe1 H1 86.7(7) . . ? P3 Fe1 H1 88.8(7) . . ? P2 Fe1 H1 85.8(7) . . ? P1 Fe1 H1 85.3(7) . . ? P4 Fe1 H2 91.3(11) . . ? P3 Fe1 H2 79.9(12) . . ? P2 Fe1 H2 96.0(11) . . ? P1 Fe1 H2 106.0(12) . . ? H1 Fe1 H2 168.7(13) . . ? P4 Fe1 H3 96.5(10) . . ? P3 Fe1 H3 106.2(11) . . ? P2 Fe1 H3 90.8(10) . . ? P1 Fe1 H3 79.7(11) . . ? H1 Fe1 H3 164.8(13) . . ? H2 Fe1 H3 26.5(13) . . ? P4 Fe1A P3 85.66(12) . . ? P4 Fe1A P2 168.0(5) . . ? P3 Fe1A P2 93.41(14) . . ? P4 Fe1A P1 93.90(14) . . ? P3 Fe1A P1 166.5(5) . . ? P2 Fe1A P1 84.22(13) . . ? P4 Fe1A H1 97.5(10) . . ? P3 Fe1A H1 99.9(10) . . ? P2 Fe1A H1 94.5(10) . . ? P1 Fe1A H1 93.5(10) . . ? P4 Fe1A H2 82.7(9) . . ? P3 Fe1A H2 73.2(10) . . ? P2 Fe1A H2 85.6(9) . . ? P1 Fe1A H2 93.3(10) . . ? H1 Fe1A H2 173.1(13) . . ? P4 Fe1A H3 86.8(8) . . ? P3 Fe1A H3 94.2(9) . . ? P2 Fe1A H3 81.4(8) . . ? P1 Fe1A H3 72.2(9) . . ? H1 Fe1A H3 165.5(13) . . ? H2 Fe1A H3 21.2(11) . . ? C5 P1 C1 101.15(6) . . ? C5 P1 C9 101.63(6) . . ? C1 P1 C9 102.81(6) . . ? C5 P1 Fe1 122.81(6) . . ? C1 P1 Fe1 107.35(5) . . ? C9 P1 Fe1 118.23(7) . . ? C5 P1 Fe1A 129.57(17) . . ? C1 P1 Fe1A 109.88(11) . . ? C9 P1 Fe1A 108.7(2) . . ? Fe1 P1 Fe1A 9.64(18) . . ? C13 P2 C17 101.53(6) . . ? C13 P2 C2 102.98(6) . . ? C17 P2 C2 102.63(6) . . ? C13 P2 Fe1 114.47(7) . . ? C17 P2 Fe1 123.81(6) . . ? C2 P2 Fe1 109.02(4) . . ? C13 P2 Fe1A 123.7(2) . . ? C17 P2 Fe1A 116.1(2) . . ? C2 P2 Fe1A 107.37(11) . . ? Fe1 P2 Fe1A 9.68(18) . . ? C21 P3 C25 102.02(6) . . ? C21 P3 C3 102.87(6) . . ? C25 P3 C3 102.97(6) . . ? C21 P3 Fe1 120.39(6) . . ? C25 P3 Fe1 117.40(7) . . ? C3 P3 Fe1 109.00(5) . . ? C21 P3 Fe1A 127.43(18) . . ? C25 P3 Fe1A 107.9(2) . . ? C3 P3 Fe1A 110.97(11) . . ? Fe1 P3 Fe1A 9.77(19) . . ? C29 P4 C33 98.96(6) . . ? C29 P4 C4 101.75(6) . . ? C33 P4 C4 100.77(6) . . ? C29 P4 Fe1A 129.0(2) . . ? C33 P4 Fe1A 113.9(2) . . ? C4 P4 Fe1A 108.54(11) . . ? C29 P4 Fe1 119.87(7) . . ? C33 P4 Fe1 122.01(6) . . ? C4 P4 Fe1 110.20(5) . . ? Fe1A P4 Fe1 9.80(19) . . ? C7 O1 C8 112.09(12) . . ? C11 O2 C12 110.78(12) . . ? C15 O3 C16 110.91(14) . . ? C19 O4 C20 111.58(11) . . ? C24 O5 C23 111.95(14) . . ? C27 O6 C28 111.68(13) . . ? C32 O7 C31 111.51(11) . . ? C35 O8 C36 111.90(12) . . ? C2 C1 P1 106.72(9) . . ? C2 C1 H1A 111.7(9) . . ? P1 C1 H1A 112.1(9) . . ? C2 C1 H1B 110.2(10) . . ? P1 C1 H1B 106.5(9) . . ? H1A C1 H1B 109.5(13) . . ? C1 C2 P2 107.06(8) . . ? C1 C2 H2A 109.4(9) . . ? P2 C2 H2A 107.6(9) . . ? C1 C2 H2B 112.9(10) . . ? P2 C2 H2B 110.7(10) . . ? H2A C2 H2B 109.1(13) . . ? C4 C3 P3 107.44(9) . . ? C4 C3 H3A 113.0(11) . . ? P3 C3 H3A 110.2(11) . . ? C4 C3 H3B 111.8(10) . . ? P3 C3 H3B 107.1(10) . . ? H3A C3 H3B 107.1(14) . . ? C3 C4 P4 109.58(9) . . ? C3 C4 H4A 110.5(10) . . ? P4 C4 H4A 108.1(10) . . ? C3 C4 H4B 113.0(11) . . ? P4 C4 H4B 108.4(11) . . ? H4A C4 H4B 107.1(14) . . ? C6 C5 P1 114.95(9) . . ? C6 C5 H5A 109.9(9) . . ? P1 C5 H5A 106.0(9) . . ? C6 C5 H5B 108.5(10) . . ? P1 C5 H5B 109.9(10) . . ? H5A C5 H5B 107.4(13) . . ? C7 C6 C5 112.31(11) . . ? C7 C6 H6A 107.6(9) . . ? C5 C6 H6A 109.9(9) . . ? C7 C6 H6B 109.7(10) . . ? C5 C6 H6B 109.4(10) . . ? H6A C6 H6B 107.8(13) . . ? O1 C7 C6 108.04(11) . . ? O1 C7 H7A 110.8(10) . . ? C6 C7 H7A 110.8(9) . . ? O1 C7 H7B 109.4(9) . . ? C6 C7 H7B 111.3(9) . . ? H7A C7 H7B 106.4(13) . . ? O1 C8 H8A 110.6(11) . . ? O1 C8 H8B 103.3(12) . . ? H8A C8 H8B 112.1(16) . . ? O1 C8 H8C 111.0(12) . . ? H8A C8 H8C 107.9(16) . . ? H8B C8 H8C 111.8(16) . . ? C10 C9 P1 116.79(9) . . ? C10 C9 H9A 110.2(9) . . ? P1 C9 H9A 107.8(9) . . ? C10 C9 H9B 109.6(10) . . ? P1 C9 H9B 106.1(10) . . ? H9A C9 H9B 105.8(13) . . ? C11 C10 C9 113.29(12) . . ? C11 C10 H10A 106.8(11) . . ? C9 C10 H10A 111.4(11) . . ? C11 C10 H10B 108.6(11) . . ? C9 C10 H10B 108.7(11) . . ? H10A C10 H10B 107.9(15) . . ? O2 C11 C10 109.78(12) . . ? O2 C11 H11A 110.8(10) . . ? C10 C11 H11A 110.7(10) . . ? O2 C11 H11B 106.7(11) . . ? C10 C11 H11B 111.8(11) . . ? H11A C11 H11B 107.0(14) . . ? O2 C12 H12A 109.1(14) . . ? O2 C12 H12B 107.1(12) . . ? H12A C12 H12B 110.2(18) . . ? O2 C12 H12C 109.9(12) . . ? H12A C12 H12C 104.9(18) . . ? H12B C12 H12C 115.5(17) . . ? C14 C13 P2 118.92(10) . . ? C14 C13 H13A 107.8(9) . . ? P2 C13 H13A 107.2(10) . . ? C14 C13 H13B 109.0(10) . . ? P2 C13 H13B 107.3(10) . . ? H13A C13 H13B 105.8(14) . . ? C15 C14 C13 110.89(12) . . ? C15 C14 H14A 109.7(11) . . ? C13 C14 H14A 111.0(11) . . ? C15 C14 H14B 105.8(11) . . ? C13 C14 H14B 110.6(11) . . ? H14A C14 H14B 108.6(15) . . ? O3 C15 C14 108.51(13) . . ? O3 C15 H15A 109.4(12) . . ? C14 C15 H15A 110.3(12) . . ? O3 C15 H15B 110.6(10) . . ? C14 C15 H15B 110.4(10) . . ? H15A C15 H15B 107.6(15) . . ? O3 C16 H16A 110.8(14) . . ? O3 C16 H16B 106.4(13) . . ? H16A C16 H16B 112.6(19) . . ? O3 C16 H16C 109.1(12) . . ? H16A C16 H16C 109.7(18) . . ? H16B C16 H16C 108.1(18) . . ? C18 C17 P2 115.68(9) . . ? C18 C17 H17A 110.6(10) . . ? P2 C17 H17A 106.6(10) . . ? C18 C17 H17B 110.7(10) . . ? P2 C17 H17B 108.3(10) . . ? H17A C17 H17B 104.2(13) . . ? C19 C18 C17 112.85(11) . . ? C19 C18 H18A 107.7(10) . . ? C17 C18 H18A 109.9(10) . . ? C19 C18 H18B 109.1(9) . . ? C17 C18 H18B 110.0(9) . . ? H18A C18 H18B 107.1(14) . . ? O4 C19 C18 108.72(11) . . ? O4 C19 H19A 110.1(10) . . ? C18 C19 H19A 111.4(10) . . ? O4 C19 H19B 107.5(9) . . ? C18 C19 H19B 111.8(9) . . ? H19A C19 H19B 107.3(13) . . ? O4 C20 H20A 110.0(11) . . ? O4 C20 H20B 107.7(11) . . ? H20A C20 H20B 111.7(15) . . ? O4 C20 H20C 109.8(12) . . ? H20A C20 H20C 107.0(15) . . ? H20B C20 H20C 110.7(15) . . ? C22 C21 P3 114.75(9) . . ? C22 C21 H21A 110.5(9) . . ? P3 C21 H21A 105.8(9) . . ? C22 C21 H21B 109.6(10) . . ? P3 C21 H21B 108.5(10) . . ? H21A C21 H21B 107.4(13) . . ? C23 C22 C21 112.21(12) . . ? C23 C22 H22A 108.3(9) . . ? C21 C22 H22A 110.7(9) . . ? C23 C22 H22B 107.4(10) . . ? C21 C22 H22B 110.8(10) . . ? H22A C22 H22B 107.2(14) . . ? O5 C23 C22 108.32(12) . . ? O5 C23 H23A 108.4(10) . . ? C22 C23 H23A 111.4(10) . . ? O5 C23 H23B 108.5(10) . . ? C22 C23 H23B 111.3(10) . . ? H23A C23 H23B 108.7(14) . . ? O5 C24 H24A 106.7(12) . . ? O5 C24 H24B 108.7(13) . . ? H24A C24 H24B 108.5(17) . . ? O5 C24 H24C 110.6(11) . . ? H24A C24 H24C 111.0(16) . . ? H24B C24 H24C 111.2(17) . . ? C26 C25 P3 117.90(10) . . ? C26 C25 H25A 110.7(10) . . ? P3 C25 H25A 106.8(10) . . ? C26 C25 H25B 109.8(10) . . ? P3 C25 H25B 106.0(10) . . ? H25A C25 H25B 104.7(14) . . ? C27 C26 C25 111.44(12) . . ? C27 C26 H26A 109.6(11) . . ? C25 C26 H26A 110.4(11) . . ? C27 C26 H26B 107.0(11) . . ? C25 C26 H26B 111.1(11) . . ? H26A C26 H26B 107.2(15) . . ? O6 C27 C26 107.98(12) . . ? O6 C27 H27A 108.5(10) . . ? C26 C27 H27A 111.1(10) . . ? O6 C27 H27B 109.6(10) . . ? C26 C27 H27B 111.6(10) . . ? H27A C27 H27B 108.0(14) . . ? O6 C28 H28A 106.6(14) . . ? O6 C28 H28B 111.1(14) . . ? H28A C28 H28B 112.8(19) . . ? O6 C28 H28C 108.7(13) . . ? H28A C28 H28C 107.7(18) . . ? H28B C28 H28C 109.7(18) . . ? C30 C29 P4 116.81(9) . . ? C30 C29 H29A 108.9(10) . . ? P4 C29 H29A 106.7(9) . . ? C30 C29 H29B 110.0(10) . . ? P4 C29 H29B 106.2(10) . . ? H29A C29 H29B 108.0(13) . . ? C31 C30 C29 110.58(11) . . ? C31 C30 H30A 109.7(9) . . ? C29 C30 H30A 111.2(9) . . ? C31 C30 H30B 107.7(10) . . ? C29 C30 H30B 110.2(10) . . ? H30A C30 H30B 107.3(13) . . ? O7 C31 C30 108.57(11) . . ? O7 C31 H31A 108.8(9) . . ? C30 C31 H31A 111.5(9) . . ? O7 C31 H31B 108.9(9) . . ? C30 C31 H31B 110.2(9) . . ? H31A C31 H31B 108.8(13) . . ? O7 C32 H32A 111.9(11) . . ? O7 C32 H32B 106.7(11) . . ? H32A C32 H32B 109.6(15) . . ? O7 C32 H32C 109.1(11) . . ? H32A C32 H32C 107.4(15) . . ? H32B C32 H32C 112.3(15) . . ? C34 C33 P4 114.76(9) . . ? C34 C33 H33A 110.3(10) . . ? P4 C33 H33A 109.2(10) . . ? C34 C33 H33B 109.3(10) . . ? P4 C33 H33B 106.5(10) . . ? H33A C33 H33B 106.5(13) . . ? C35 C34 C33 112.06(11) . . ? C35 C34 H34A 108.6(10) . . ? C33 C34 H34A 110.4(10) . . ? C35 C34 H34B 109.1(10) . . ? C33 C34 H34B 109.8(10) . . ? H34A C34 H34B 106.7(14) . . ? O8 C35 C34 107.67(11) . . ? O8 C35 H35A 110.6(10) . . ? C34 C35 H35A 110.9(10) . . ? O8 C35 H35B 111.1(10) . . ? C34 C35 H35B 110.4(10) . . ? H35A C35 H35B 106.2(14) . . ? O8 C36 H36A 111.9(11) . . ? O8 C36 H36B 108.2(10) . . ? H36A C36 H36B 109.1(15) . . ? O8 C36 H36C 110.2(11) . . ? H36A C36 H36C 106.7(15) . . ? H36B C36 H36C 110.8(15) . . ? C43 B1 C55 109.61(10) . . ? C43 B1 C49 109.57(10) . . ? C55 B1 C49 108.76(10) . . ? C43 B1 C37 109.49(10) . . ? C55 B1 C37 109.08(10) . . ? C49 B1 C37 110.32(10) . . ? C42 C37 C38 114.77(12) . . ? C42 C37 B1 123.77(11) . . ? C38 C37 B1 121.38(11) . . ? C39 C38 C37 122.99(13) . . ? C39 C38 H38 118.1(10) . . ? C37 C38 H38 118.9(10) . . ? C40 C39 C38 120.07(14) . . ? C40 C39 H39 120.5(11) . . ? C38 C39 H39 119.4(11) . . ? C41 C40 C39 118.93(14) . . ? C41 C40 H40 122.3(12) . . ? C39 C40 H40 118.8(12) . . ? C40 C41 C42 120.21(14) . . ? C40 C41 H41 119.6(11) . . ? C42 C41 H41 120.1(11) . . ? C41 C42 C37 123.03(13) . . ? C41 C42 H42 116.5(10) . . ? C37 C42 H42 120.5(10) . . ? C48 C43 C44 115.39(12) . . ? C48 C43 B1 123.27(11) . . ? C44 C43 B1 121.31(11) . . ? C45 C44 C43 122.79(13) . . ? C45 C44 H44 117.2(10) . . ? C43 C44 H44 120.0(10) . . ? C44 C45 C46 120.00(13) . . ? C44 C45 H45 118.8(10) . . ? C46 C45 H45 121.2(10) . . ? C47 C46 C45 118.86(12) . . ? C47 C46 H46 120.2(10) . . ? C45 C46 H46 120.9(10) . . ? C46 C47 C48 120.46(13) . . ? C46 C47 H47 122.1(9) . . ? C48 C47 H47 117.5(9) . . ? C47 C48 C43 122.49(12) . . ? C47 C48 H48 118.0(9) . . ? C43 C48 H48 119.6(9) . . ? C50 C49 C54 114.92(12) . . ? C50 C49 B1 122.59(11) . . ? C54 C49 B1 122.46(11) . . ? C51 C50 C49 122.71(13) . . ? C51 C50 H50 117.0(10) . . ? C49 C50 H50 120.2(10) . . ? C52 C51 C50 120.40(13) . . ? C52 C51 H51 121.7(11) . . ? C50 C51 H51 117.9(11) . . ? C53 C52 C51 118.73(13) . . ? C53 C52 H52 121.8(10) . . ? C51 C52 H52 119.5(11) . . ? C52 C53 C54 120.21(13) . . ? C52 C53 H53 119.3(10) . . ? C54 C53 H53 120.4(10) . . ? C53 C54 C49 123.00(13) . . ? C53 C54 H54 117.8(9) . . ? C49 C54 H54 119.2(9) . . ? C60 C55 C56 114.95(12) . . ? C60 C55 B1 122.46(11) . . ? C56 C55 B1 122.52(11) . . ? C57 C56 C55 122.77(13) . . ? C57 C56 H56 117.4(10) . . ? C55 C56 H56 119.9(10) . . ? C58 C57 C56 120.15(13) . . ? C58 C57 H57 120.4(10) . . ? C56 C57 H57 119.5(10) . . ? C57 C58 C59 119.01(13) . . ? C57 C58 H58 121.1(11) . . ? C59 C58 H58 119.9(11) . . ? C58 C59 C60 120.19(13) . . ? C58 C59 H59 120.1(10) . . ? C60 C59 H59 119.7(10) . . ? C59 C60 C55 122.91(13) . . ? C59 C60 H60 118.4(10) . . ? C55 C60 H60 118.7(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P4 Fe1 P1 C5 53.30(10) . . . . ? P3 Fe1 P1 C5 141.1(2) . . . . ? P2 Fe1 P1 C5 -134.23(6) . . . . ? P4 Fe1 P1 C1 169.57(6) . . . . ? P3 Fe1 P1 C1 -102.6(2) . . . . ? P2 Fe1 P1 C1 -17.97(8) . . . . ? P4 Fe1 P1 C9 -74.88(8) . . . . ? P3 Fe1 P1 C9 12.9(2) . . . . ? P2 Fe1 P1 C9 97.58(7) . . . . ? P4 Fe1 P1 Fe1A -83.7(6) . . . . ? P3 Fe1 P1 Fe1A 4.2(4) . . . . ? P2 Fe1 P1 Fe1A 88.8(6) . . . . ? P4 Fe1A P1 C5 37.7(4) . . . . ? P3 Fe1A P1 C5 -49.9(8) . . . . ? P2 Fe1A P1 C5 -130.43(11) . . . . ? P4 Fe1A P1 C1 162.17(18) . . . . ? P3 Fe1A P1 C1 74.5(8) . . . . ? P2 Fe1A P1 C1 -6.0(3) . . . . ? P4 Fe1A P1 C9 -86.0(3) . . . . ? P3 Fe1A P1 C9 -173.7(7) . . . . ? P2 Fe1A P1 C9 105.8(2) . . . . ? P4 Fe1A P1 Fe1 85.8(6) . . . . ? P3 Fe1A P1 Fe1 -1.8(2) . . . . ? P2 Fe1A P1 Fe1 -82.3(6) . . . . ? P4 Fe1 P2 C13 -163.74(17) . . . . ? P3 Fe1 P2 C13 -78.96(8) . . . . ? P1 Fe1 P2 C13 106.94(7) . . . . ? P4 Fe1 P2 C17 -39.05(19) . . . . ? P3 Fe1 P2 C17 45.74(10) . . . . ? P1 Fe1 P2 C17 -128.36(6) . . . . ? P4 Fe1 P2 C2 81.56(18) . . . . ? P3 Fe1 P2 C2 166.34(6) . . . . ? P1 Fe1 P2 C2 -7.76(8) . . . . ? P4 Fe1 P2 Fe1A -0.2(5) . . . . ? P3 Fe1 P2 Fe1A 84.6(6) . . . . ? P1 Fe1 P2 Fe1A -89.5(6) . . . . ? P4 Fe1A P2 C13 18.2(9) . . . . ? P3 Fe1A P2 C13 -66.9(3) . . . . ? P1 Fe1A P2 C13 99.73(18) . . . . ? P4 Fe1A P2 C17 144.7(8) . . . . ? P3 Fe1A P2 C17 59.5(3) . . . . ? P1 Fe1A P2 C17 -133.81(15) . . . . ? P4 Fe1A P2 C2 -101.2(8) . . . . ? P3 Fe1A P2 C2 173.63(18) . . . . ? P1 Fe1A P2 C2 -19.7(3) . . . . ? P4 Fe1A P2 Fe1 0.1(3) . . . . ? P3 Fe1A P2 Fe1 -85.0(6) . . . . ? P1 Fe1A P2 Fe1 81.6(6) . . . . ? P4 Fe1 P3 C21 -137.60(6) . . . . ? P2 Fe1 P3 C21 49.91(9) . . . . ? P1 Fe1 P3 C21 134.1(2) . . . . ? P4 Fe1 P3 C25 97.24(7) . . . . ? P2 Fe1 P3 C25 -75.26(8) . . . . ? P1 Fe1 P3 C25 9.0(2) . . . . ? P4 Fe1 P3 C3 -19.24(8) . . . . ? P2 Fe1 P3 C3 168.27(6) . . . . ? P1 Fe1 P3 C3 -107.5(2) . . . . ? P4 Fe1 P3 Fe1A 84.1(6) . . . . ? P2 Fe1 P3 Fe1A -88.4(6) . . . . ? P1 Fe1 P3 Fe1A -4.2(4) . . . . ? P4 Fe1A P3 C21 -133.08(12) . . . . ? P2 Fe1A P3 C21 35.0(4) . . . . ? P1 Fe1A P3 C21 -44.5(8) . . . . ? P4 Fe1A P3 C25 105.4(2) . . . . ? P2 Fe1A P3 C25 -86.5(3) . . . . ? P1 Fe1A P3 C25 -166.0(7) . . . . ? P4 Fe1A P3 C3 -6.7(3) . . . . ? P2 Fe1A P3 C3 161.39(17) . . . . ? P1 Fe1A P3 C3 82.0(8) . . . . ? P4 Fe1A P3 Fe1 -86.8(6) . . . . ? P2 Fe1A P3 Fe1 81.3(6) . . . . ? P1 Fe1A P3 Fe1 1.8(2) . . . . ? P3 Fe1A P4 C29 107.65(18) . . . . ? P2 Fe1A P4 C29 21.7(9) . . . . ? P1 Fe1A P4 C29 -58.8(3) . . . . ? P3 Fe1A P4 C33 -126.98(17) . . . . ? P2 Fe1A P4 C33 147.1(8) . . . . ? P1 Fe1A P4 C33 66.6(3) . . . . ? P3 Fe1A P4 C4 -15.6(3) . . . . ? P2 Fe1A P4 C4 -101.6(8) . . . . ? P1 Fe1A P4 C4 177.93(18) . . . . ? P3 Fe1A P4 Fe1 85.8(6) . . . . ? P2 Fe1A P4 Fe1 -0.1(3) . . . . ? P1 Fe1A P4 Fe1 -80.6(6) . . . . ? P3 Fe1 P4 C29 114.33(7) . . . . ? P2 Fe1 P4 C29 -160.32(17) . . . . ? P1 Fe1 P4 C29 -71.60(9) . . . . ? P3 Fe1 P4 C33 -120.86(6) . . . . ? P2 Fe1 P4 C33 -35.51(19) . . . . ? P1 Fe1 P4 C33 53.21(10) . . . . ? P3 Fe1 P4 C4 -3.16(9) . . . . ? P2 Fe1 P4 C4 82.19(18) . . . . ? P1 Fe1 P4 C4 170.91(6) . . . . ? P3 Fe1 P4 Fe1A -85.1(6) . . . . ? P2 Fe1 P4 Fe1A 0.2(5) . . . . ? P1 Fe1 P4 Fe1A 89.0(6) . . . . ? C5 P1 C1 C2 176.04(9) . . . . ? C9 P1 C1 C2 -79.16(10) . . . . ? Fe1 P1 C1 C2 46.23(11) . . . . ? Fe1A P1 C1 C2 36.4(3) . . . . ? P1 C1 C2 P2 -52.27(10) . . . . ? C13 P2 C2 C1 -83.98(10) . . . . ? C17 P2 C2 C1 170.84(9) . . . . ? Fe1 P2 C2 C1 37.97(11) . . . . ? Fe1A P2 C2 C1 48.0(3) . . . . ? C21 P3 C3 C4 171.46(9) . . . . ? C25 P3 C3 C4 -82.77(10) . . . . ? Fe1 P3 C3 C4 42.60(11) . . . . ? Fe1A P3 C3 C4 32.4(3) . . . . ? P3 C3 C4 P4 -44.86(11) . . . . ? C29 P4 C4 C3 -97.97(10) . . . . ? C33 P4 C4 C3 160.40(9) . . . . ? Fe1A P4 C4 C3 40.5(3) . . . . ? Fe1 P4 C4 C3 30.24(12) . . . . ? C1 P1 C5 C6 -67.95(10) . . . . ? C9 P1 C5 C6 -173.69(10) . . . . ? Fe1 P1 C5 C6 51.30(12) . . . . ? Fe1A P1 C5 C6 59.8(3) . . . . ? P1 C5 C6 C7 165.95(9) . . . . ? C8 O1 C7 C6 177.63(12) . . . . ? C5 C6 C7 O1 -67.53(14) . . . . ? C5 P1 C9 C10 67.89(11) . . . . ? C1 P1 C9 C10 -36.54(12) . . . . ? Fe1 P1 C9 C10 -154.52(9) . . . . ? Fe1A P1 C9 C10 -152.97(14) . . . . ? P1 C9 C10 C11 -176.00(10) . . . . ? C12 O2 C11 C10 -171.00(14) . . . . ? C9 C10 C11 O2 -56.89(17) . . . . ? C17 P2 C13 C14 66.22(13) . . . . ? C2 P2 C13 C14 -39.80(13) . . . . ? Fe1 P2 C13 C14 -157.99(11) . . . . ? Fe1A P2 C13 C14 -161.27(17) . . . . ? P2 C13 C14 C15 -169.98(12) . . . . ? C16 O3 C15 C14 178.27(15) . . . . ? C13 C14 C15 O3 -59.02(18) . . . . ? C13 P2 C17 C18 -172.71(10) . . . . ? C2 P2 C17 C18 -66.42(11) . . . . ? Fe1 P2 C17 C18 57.08(12) . . . . ? Fe1A P2 C17 C18 50.3(2) . . . . ? P2 C17 C18 C19 -173.34(9) . . . . ? C20 O4 C19 C18 177.18(12) . . . . ? C17 C18 C19 O4 -65.56(15) . . . . ? C25 P3 C21 C22 -176.26(10) . . . . ? C3 P3 C21 C22 -69.76(11) . . . . ? Fe1 P3 C21 C22 51.65(12) . . . . ? Fe1A P3 C21 C22 59.8(3) . . . . ? P3 C21 C22 C23 178.54(10) . . . . ? C24 O5 C23 C22 179.14(13) . . . . ? C21 C22 C23 O5 61.09(16) . . . . ? C21 P3 C25 C26 56.15(12) . . . . ? C3 P3 C25 C26 -50.27(12) . . . . ? Fe1 P3 C25 C26 -169.99(9) . . . . ? Fe1A P3 C25 C26 -167.67(14) . . . . ? P3 C25 C26 C27 -167.63(10) . . . . ? C28 O6 C27 C26 179.66(13) . . . . ? C25 C26 C27 O6 63.15(16) . . . . ? C33 P4 C29 C30 166.66(10) . . . . ? C4 P4 C29 C30 63.60(11) . . . . ? Fe1A P4 C29 C30 -62.3(2) . . . . ? Fe1 P4 C29 C30 -58.15(12) . . . . ? P4 C29 C30 C31 177.12(9) . . . . ? C32 O7 C31 C30 172.11(13) . . . . ? C29 C30 C31 O7 -62.64(15) . . . . ? C29 P4 C33 C34 -178.09(10) . . . . ? C4 P4 C33 C34 -74.21(11) . . . . ? Fe1A P4 C33 C34 41.8(2) . . . . ? Fe1 P4 C33 C34 48.03(12) . . . . ? P4 C33 C34 C35 148.63(10) . . . . ? C36 O8 C35 C34 170.44(12) . . . . ? C33 C34 C35 O8 172.40(11) . . . . ? C43 B1 C37 C42 25.71(17) . . . . ? C55 B1 C37 C42 -94.23(14) . . . . ? C49 B1 C37 C42 146.37(12) . . . . ? C43 B1 C37 C38 -157.82(12) . . . . ? C55 B1 C37 C38 82.24(15) . . . . ? C49 B1 C37 C38 -37.16(16) . . . . ? C42 C37 C38 C39 0.4(2) . . . . ? B1 C37 C38 C39 -176.41(13) . . . . ? C37 C38 C39 C40 -0.7(2) . . . . ? C38 C39 C40 C41 0.4(2) . . . . ? C39 C40 C41 C42 0.2(2) . . . . ? C40 C41 C42 C37 -0.5(2) . . . . ? C38 C37 C42 C41 0.3(2) . . . . ? B1 C37 C42 C41 176.95(13) . . . . ? C55 B1 C43 C48 -138.57(12) . . . . ? C49 B1 C43 C48 -19.29(16) . . . . ? C37 B1 C43 C48 101.82(13) . . . . ? C55 B1 C43 C44 43.42(15) . . . . ? C49 B1 C43 C44 162.70(11) . . . . ? C37 B1 C43 C44 -76.19(14) . . . . ? C48 C43 C44 C45 -1.48(19) . . . . ? B1 C43 C44 C45 176.68(12) . . . . ? C43 C44 C45 C46 0.8(2) . . . . ? C44 C45 C46 C47 0.4(2) . . . . ? C45 C46 C47 C48 -0.9(2) . . . . ? C46 C47 C48 C43 0.2(2) . . . . ? C44 C43 C48 C47 0.94(18) . . . . ? B1 C43 C48 C47 -177.18(12) . . . . ? C43 B1 C49 C50 85.80(14) . . . . ? C55 B1 C49 C50 -154.39(12) . . . . ? C37 B1 C49 C50 -34.80(16) . . . . ? C43 B1 C49 C54 -91.97(14) . . . . ? C55 B1 C49 C54 27.83(16) . . . . ? C37 B1 C49 C54 147.42(12) . . . . ? C54 C49 C50 C51 -1.55(19) . . . . ? B1 C49 C50 C51 -179.48(12) . . . . ? C49 C50 C51 C52 0.4(2) . . . . ? C50 C51 C52 C53 1.3(2) . . . . ? C51 C52 C53 C54 -1.7(2) . . . . ? C52 C53 C54 C49 0.4(2) . . . . ? C50 C49 C54 C53 1.14(19) . . . . ? B1 C49 C54 C53 179.08(12) . . . . ? C43 B1 C55 C60 -149.15(12) . . . . ? C49 B1 C55 C60 91.07(14) . . . . ? C37 B1 C55 C60 -29.29(16) . . . . ? C43 B1 C55 C56 33.98(16) . . . . ? C49 B1 C55 C56 -85.79(14) . . . . ? C37 B1 C55 C56 153.85(12) . . . . ? C60 C55 C56 C57 0.44(19) . . . . ? B1 C55 C56 C57 177.52(12) . . . . ? C55 C56 C57 C58 -0.3(2) . . . . ? C56 C57 C58 C59 -0.2(2) . . . . ? C57 C58 C59 C60 0.5(2) . . . . ? C58 C59 C60 C55 -0.3(2) . . . . ? C56 C55 C60 C59 -0.15(19) . . . . ? B1 C55 C60 C59 -177.23(13) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.457 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.048 #===END data_just3 _database_code_depnum_ccdc_archive 'CCDC 735061' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H101 B Fe N2 O8 P4' _chemical_formula_weight 1168.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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 13.466(2) _cell_length_b 15.443(3) _cell_length_c 16.219(3) _cell_angle_alpha 97.261(3) _cell_angle_beta 94.169(3) _cell_angle_gamma 104.408(3) _cell_volume 3221.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6773 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 28.19 _exptl_crystal_description block _exptl_crystal_colour ligh-yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.384 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8967 _exptl_absorpt_correction_T_max 0.9341 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector Bruker Apex' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36541 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14419 _reflns_number_gt 12000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+2.0865P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14419 _refine_ls_number_parameters 978 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1367 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Fe1 Fe 0.68649(2) 0.780987(18) 0.749919(17) 0.01978(8) Uani 1 1 d . . . P1 P 0.71370(4) 0.78121(4) 0.61590(3) 0.02279(12) Uani 1 1 d . . . P2 P 0.56695(4) 0.65175(3) 0.70186(3) 0.02200(12) Uani 1 1 d . . . P3 P 0.68148(4) 0.76376(3) 0.88414(3) 0.02392(12) Uani 1 1 d . . . P4 P 0.82570(4) 0.89487(3) 0.79727(3) 0.02274(12) Uani 1 1 d . . . N1 N 0.59465(13) 0.85088(12) 0.74820(11) 0.0248(4) Uani 1 1 d . . . N2 N 0.53769(15) 0.89205(14) 0.74657(13) 0.0357(4) Uani 1 1 d . . . O1 O 1.05711(13) 0.78743(12) 0.62195(12) 0.0428(4) Uani 1 1 d . . . O2 O 0.5458(2) 0.8931(2) 0.42663(18) 0.0907(9) Uani 1 1 d . . . O3 O 0.67524(14) 0.41328(11) 0.57069(11) 0.0407(4) Uani 1 1 d . . . O4 O 0.20331(15) 0.68586(14) 0.77078(17) 0.0637(6) Uani 1 1 d . . . O5 O 0.75618(15) 0.48572(12) 0.83697(12) 0.0456(4) Uani 1 1 d . . . O6 O 0.47259(17) 0.89150(15) 1.04008(15) 0.0630(6) Uani 1 1 d . . . O7 O 1.22333(14) 0.95582(13) 0.89098(14) 0.0542(5) Uani 1 1 d . . . O8 O 0.74191(17) 1.19086(13) 0.70961(14) 0.0576(6) Uani 1 1 d . . . B1 B 0.15789(19) 0.29810(16) 0.76089(15) 0.0264(5) Uani 1 1 d . . . C1 C 0.62382(18) 0.68221(16) 0.55030(14) 0.0297(5) Uani 1 1 d . . . C2 C 0.52542(17) 0.65894(16) 0.59289(13) 0.0278(4) Uani 1 1 d . . . C3 C 0.7883(2) 0.84938(16) 0.94947(14) 0.0329(5) Uani 1 1 d . . . C4 C 0.81311(18) 0.93350(15) 0.90715(14) 0.0294(4) Uani 1 1 d . . . C5 C 0.83930(17) 0.77820(16) 0.58132(14) 0.0276(4) Uani 1 1 d . . . C6 C 0.88175(17) 0.70135(15) 0.60699(14) 0.0285(4) Uani 1 1 d . . . C7 C 0.98808(18) 0.70624(16) 0.58026(16) 0.0342(5) Uani 1 1 d . . . C8 C 1.1585(2) 0.7972(2) 0.5993(3) 0.0588(9) Uani 1 1 d . . . C9 C 0.68046(18) 0.87300(17) 0.56725(14) 0.0308(5) Uani 1 1 d . . . C10 C 0.7064(2) 0.8805(2) 0.47822(17) 0.0483(7) Uani 1 1 d . . . H10A H 0.7816 0.9064 0.4792 0.058 Uiso 1 1 calc R . . H10B H 0.6886 0.8192 0.4452 0.058 Uiso 1 1 calc R . . C11 C 0.6497(2) 0.9387(2) 0.43586(19) 0.0563(8) Uani 1 1 d . . . H11A H 0.6614 0.9987 0.4705 0.068 Uiso 1 1 calc R . . H11B H 0.6740 0.9476 0.3806 0.068 Uiso 1 1 calc R . . C12 C 0.4866(5) 0.9389(5) 0.3803(4) 0.146(3) Uani 1 1 d . . . H12A H 0.4138 0.9052 0.3736 0.218 Uiso 1 1 calc R . . H12B H 0.5110 0.9432 0.3251 0.218 Uiso 1 1 calc R . . H12C H 0.4942 0.9998 0.4103 0.218 Uiso 1 1 calc R . . C13 C 0.61487(17) 0.54993(14) 0.69053(13) 0.0256(4) Uani 1 1 d . . . H13A H 0.676(2) 0.5647(18) 0.6673(16) 0.036(7) Uiso 1 1 d . . . H13B H 0.6301(18) 0.5354(16) 0.7463(15) 0.025(6) Uiso 1 1 d . . . C14 C 0.54472(18) 0.46471(15) 0.63835(15) 0.0308(5) Uani 1 1 d . . . C15 C 0.59828(19) 0.38942(15) 0.62457(15) 0.0323(5) Uani 1 1 d . . . C16 C 0.7219(3) 0.3419(2) 0.5494(2) 0.0555(8) Uani 1 1 d . . . C17 C 0.44514(17) 0.61308(15) 0.74662(15) 0.0279(4) Uani 1 1 d . . . C18 C 0.36926(19) 0.67069(18) 0.74041(19) 0.0388(6) Uani 1 1 d . . . C19 C 0.27398(18) 0.63389(17) 0.78187(17) 0.0391(6) Uani 1 1 d . . . H19A H 0.2420 0.5701 0.7571 0.047 Uiso 1 1 calc R . . H19B H 0.2931 0.6358 0.8423 0.047 Uiso 1 1 calc R . . C20 C 0.1044(2) 0.6447(2) 0.7906(2) 0.0604(9) Uani 1 1 d . . . H20A H 0.0585 0.6837 0.7816 0.091 Uiso 1 1 calc R . . H20B H 0.1084 0.6354 0.8493 0.091 Uiso 1 1 calc R . . H20C H 0.0773 0.5862 0.7547 0.091 Uiso 1 1 calc R . . C21 C 0.6920(2) 0.65618(16) 0.91639(15) 0.0330(5) Uani 1 1 d . . . C22 C 0.7966(2) 0.63872(18) 0.9119(2) 0.0493(7) Uani 1 1 d . . . C23 C 0.7989(3) 0.54111(17) 0.91289(17) 0.0425(6) Uani 1 1 d . . . C24 C 0.8363(3) 0.4989(3) 0.7781(2) 0.0630(8) Uani 1 1 d . . . H24A H 0.8457 0.5588 0.7610 0.095 Uiso 1 1 calc R . . H24B H 0.8145 0.4523 0.7288 0.095 Uiso 1 1 calc R . . H24C H 0.9016 0.4944 0.8058 0.095 Uiso 1 1 calc R . . C25 C 0.5675(2) 0.78436(17) 0.93061(15) 0.0337(5) Uani 1 1 d . . . C26 C 0.5650(4) 0.7824(3) 1.0234(2) 0.0869(15) Uani 1 1 d . . . H26A H 0.6272 0.8263 1.0541 0.104 Uiso 1 1 calc R . . H26B H 0.5666 0.7214 1.0355 0.104 Uiso 1 1 calc R . . C27 C 0.4698(3) 0.8051(2) 1.0544(2) 0.0719(11) Uani 1 1 d . . . H27A H 0.4068 0.7619 1.0241 0.086 Uiso 1 1 calc R . . H27B H 0.4691 0.8014 1.1148 0.086 Uiso 1 1 calc R . . C28 C 0.3953(4) 0.9254(3) 1.0773(3) 0.0994(16) Uani 1 1 d . . . H28A H 0.4021 0.9876 1.0667 0.149 Uiso 1 1 calc R . . H28B H 0.4033 0.9246 1.1377 0.149 Uiso 1 1 calc R . . H28C H 0.3272 0.8876 1.0533 0.149 Uiso 1 1 calc R . . C29 C 0.94818(16) 0.86231(15) 0.80424(14) 0.0269(4) Uani 1 1 d . . . C30 C 1.04046(17) 0.92647(16) 0.85985(14) 0.0289(4) Uani 1 1 d . . . C31 C 1.13398(18) 0.88914(16) 0.85389(17) 0.0347(5) Uani 1 1 d . . . C32 C 1.3143(2) 0.9298(3) 0.8697(3) 0.0874(14) Uani 1 1 d . . . H32A H 1.3755 0.9769 0.8959 0.131 Uiso 1 1 calc R . . H32B H 1.3150 0.9222 0.8088 0.131 Uiso 1 1 calc R . . H32C H 1.3148 0.8727 0.8897 0.131 Uiso 1 1 calc R . . C33 C 0.86010(17) 0.99941(15) 0.75100(15) 0.0288(4) Uani 1 1 d . . . C34 C 0.78452(19) 1.05826(16) 0.75881(17) 0.0343(5) Uani 1 1 d . . . C35 C 0.8126(2) 1.13595(18) 0.70812(19) 0.0429(6) Uani 1 1 d . . . C36 C 0.7573(3) 1.2518(2) 0.7823(3) 0.0723(10) Uani 1 1 d . . . H36A H 0.7068 1.2877 0.7801 0.108 Uiso 1 1 calc R . . H36B H 0.8271 1.2919 0.7880 0.108 Uiso 1 1 calc R . . H36C H 0.7488 1.2189 0.8303 0.108 Uiso 1 1 calc R . . C37 C 0.13288(17) 0.19514(15) 0.70953(14) 0.0291(4) Uani 1 1 d . . . C38 C 0.06260(18) 0.16681(15) 0.63761(15) 0.0321(5) Uani 1 1 d . . . C39 C 0.0335(2) 0.07766(17) 0.59751(18) 0.0433(6) Uani 1 1 d . . . C40 C 0.0755(3) 0.01347(18) 0.6276(2) 0.0519(8) Uani 1 1 d . . . C41 C 0.1453(3) 0.03855(18) 0.6977(2) 0.0485(7) Uani 1 1 d . . . C42 C 0.1733(2) 0.12753(17) 0.73805(17) 0.0395(6) Uani 1 1 d . . . C43 C 0.27925(18) 0.33576(17) 0.80126(15) 0.0347(5) Uani 1 1 d . . . C44 C 0.3594(2) 0.3029(2) 0.76973(19) 0.0474(7) Uani 1 1 d . . . C45 C 0.4626(2) 0.3406(3) 0.8008(2) 0.0640(10) Uani 1 1 d . . . C46 C 0.4893(3) 0.4133(3) 0.8644(2) 0.0731(13) Uani 1 1 d . . . C47 C 0.4135(3) 0.4478(2) 0.8962(2) 0.0600(10) Uani 1 1 d . . . C48 C 0.3105(2) 0.40918(19) 0.86581(17) 0.0431(6) Uani 1 1 d . . . C49 C 0.08223(16) 0.29672(14) 0.83692(13) 0.0261(4) Uani 1 1 d . . . C50 C 0.04431(18) 0.21851(15) 0.87294(14) 0.0295(4) Uani 1 1 d . . . C51 C -0.02132(19) 0.21476(18) 0.93584(15) 0.0366(5) Uani 1 1 d . . . C52 C -0.0516(2) 0.2904(2) 0.96596(16) 0.0410(6) Uani 1 1 d . . . C53 C -0.0151(2) 0.36960(18) 0.93428(15) 0.0395(6) Uani 1 1 d . . . C54 C 0.05083(19) 0.37226(16) 0.87144(15) 0.0336(5) Uani 1 1 d . . . C55 C 0.13756(17) 0.36642(13) 0.69482(13) 0.0261(4) Uani 1 1 d . . . C56 C 0.04261(19) 0.38677(15) 0.67873(14) 0.0309(5) Uani 1 1 d . . . C57 C 0.0273(2) 0.44356(17) 0.62180(15) 0.0365(5) Uani 1 1 d . . . C58 C 0.1061(2) 0.48202(16) 0.57719(15) 0.0379(6) Uani 1 1 d . . . C59 C 0.1995(2) 0.46117(16) 0.58871(14) 0.0355(5) Uani 1 1 d . . . C60 C 0.21389(18) 0.40472(15) 0.64636(14) 0.0306(5) Uani 1 1 d . . . H1 H 0.754(2) 0.7256(18) 0.7493(16) 0.040(7) Uiso 1 1 d . . . H1A H 0.657(2) 0.6340(19) 0.5453(17) 0.041(7) Uiso 1 1 d . . . H1B H 0.613(2) 0.6976(19) 0.4986(19) 0.044(8) Uiso 1 1 d . . . H2A H 0.474(2) 0.6058(18) 0.5687(16) 0.034(7) Uiso 1 1 d . . . H2B H 0.4914(19) 0.7060(17) 0.5949(15) 0.028(6) Uiso 1 1 d . . . H3A H 0.842(2) 0.8213(19) 0.9526(17) 0.043(8) Uiso 1 1 d . . . H3B H 0.768(2) 0.8599(19) 1.0021(19) 0.044(8) Uiso 1 1 d . . . H4A H 0.876(2) 0.9792(18) 0.9361(16) 0.036(7) Uiso 1 1 d . . . H4B H 0.755(2) 0.9657(17) 0.9042(15) 0.033(6) Uiso 1 1 d . . . H5A H 0.8279(19) 0.7731(16) 0.5201(16) 0.031(6) Uiso 1 1 d . . . H5B H 0.887(2) 0.8352(18) 0.6020(16) 0.033(7) Uiso 1 1 d . . . H6A H 0.8856(17) 0.7034(15) 0.6647(15) 0.020(5) Uiso 1 1 d . . . H6B H 0.836(2) 0.6407(18) 0.5827(16) 0.033(7) Uiso 1 1 d . . . H7A H 0.990(2) 0.7044(18) 0.5199(18) 0.037(7) Uiso 1 1 d . . . H7B H 1.012(2) 0.6549(19) 0.5973(16) 0.037(7) Uiso 1 1 d . . . H8A H 1.203(3) 0.852(3) 0.636(2) 0.068(10) Uiso 1 1 d . . . H8B H 1.183(3) 0.746(3) 0.617(2) 0.071(11) Uiso 1 1 d . . . H8C H 1.154(3) 0.793(2) 0.541(2) 0.068(11) Uiso 1 1 d . . . H9A H 0.607(2) 0.8585(18) 0.5710(16) 0.038(7) Uiso 1 1 d . . . H9B H 0.703(2) 0.930(2) 0.6044(18) 0.049(8) Uiso 1 1 d . . . H14A H 0.485(2) 0.4439(18) 0.6649(17) 0.037(7) Uiso 1 1 d . . . H14B H 0.523(2) 0.4786(18) 0.5890(18) 0.037(7) Uiso 1 1 d . . . H15A H 0.6320(19) 0.3807(16) 0.6759(16) 0.028(6) Uiso 1 1 d . . . H15B H 0.552(2) 0.3346(18) 0.5999(16) 0.034(7) Uiso 1 1 d . . . H16A H 0.773(3) 0.357(3) 0.520(2) 0.075(12) Uiso 1 1 d . . . H16B H 0.669(3) 0.292(3) 0.524(2) 0.067(11) Uiso 1 1 d . . . H16C H 0.757(3) 0.336(2) 0.599(2) 0.066(11) Uiso 1 1 d . . . H17A H 0.417(2) 0.559(2) 0.7184(19) 0.049(8) Uiso 1 1 d . . . H17B H 0.462(2) 0.6099(17) 0.8005(18) 0.034(7) Uiso 1 1 d . . . H18A H 0.348(2) 0.670(2) 0.681(2) 0.059(9) Uiso 1 1 d . . . H18B H 0.398(2) 0.727(2) 0.7634(19) 0.051(9) Uiso 1 1 d . . . H21A H 0.640(2) 0.6090(18) 0.8842(17) 0.035(7) Uiso 1 1 d . . . H21B H 0.671(2) 0.6523(18) 0.9693(18) 0.040(7) Uiso 1 1 d . . . H22A H 0.822(2) 0.6529(19) 0.8669(18) 0.033(8) Uiso 1 1 d . . . H22B H 0.840(4) 0.675(3) 0.965(3) 0.114(16) Uiso 1 1 d . . . H23A H 0.861(3) 0.535(2) 0.923(2) 0.063(10) Uiso 1 1 d . . . H23B H 0.748(3) 0.505(2) 0.948(2) 0.069(10) Uiso 1 1 d . . . H25A H 0.506(3) 0.740(2) 0.902(2) 0.058(9) Uiso 1 1 d . . . H25B H 0.562(2) 0.842(2) 0.9225(17) 0.044(8) Uiso 1 1 d . . . H29A H 0.9643(19) 0.8523(16) 0.7453(16) 0.028(6) Uiso 1 1 d . . . H29B H 0.931(2) 0.8044(19) 0.8231(17) 0.040(7) Uiso 1 1 d . . . H30A H 1.056(2) 0.9796(19) 0.8426(16) 0.036(7) Uiso 1 1 d . . . H30B H 1.023(2) 0.9340(18) 0.9199(17) 0.038(7) Uiso 1 1 d . . . H31A H 1.142(2) 0.8712(18) 0.7929(18) 0.040(7) Uiso 1 1 d . . . H31B H 1.127(2) 0.8402(19) 0.8803(17) 0.035(7) Uiso 1 1 d . . . H33A H 0.8687(18) 0.9792(16) 0.6924(16) 0.027(6) Uiso 1 1 d . . . H33B H 0.923(2) 1.0300(19) 0.7727(17) 0.038(7) Uiso 1 1 d . . . H34A H 0.7837(19) 1.0796(17) 0.8169(17) 0.031(6) Uiso 1 1 d . . . H34B H 0.717(2) 1.0229(18) 0.7403(16) 0.037(7) Uiso 1 1 d . . . H35A H 0.885(2) 1.1754(19) 0.7313(17) 0.043(7) Uiso 1 1 d . . . H35B H 0.7964(15) 1.1015(14) 0.6428(13) 0.012(5) Uiso 1 1 d . . . H38 H 0.0297(19) 0.2102(17) 0.6155(15) 0.028(6) Uiso 1 1 d . . . H39 H -0.011(2) 0.061(2) 0.5505(19) 0.042(8) Uiso 1 1 d . . . H40 H 0.064(3) -0.040(2) 0.603(2) 0.063(10) Uiso 1 1 d . . . H41 H 0.173(2) -0.001(2) 0.7190(19) 0.051(8) Uiso 1 1 d . . . H42 H 0.220(2) 0.1430(18) 0.7847(17) 0.034(7) Uiso 1 1 d . . . H44 H 0.344(2) 0.253(2) 0.7288(19) 0.045(8) Uiso 1 1 d . . . H45 H 0.507(3) 0.305(2) 0.777(2) 0.072(11) Uiso 1 1 d . . . H46 H 0.553(3) 0.440(3) 0.887(2) 0.078(11) Uiso 1 1 d . . . H47 H 0.426(3) 0.495(3) 0.938(2) 0.070(11) Uiso 1 1 d . . . H48 H 0.263(2) 0.4358(17) 0.8907(16) 0.031(7) Uiso 1 1 d . . . H50 H 0.0636(19) 0.1663(17) 0.8550(15) 0.029(6) Uiso 1 1 d . . . H51 H -0.045(2) 0.158(2) 0.9620(17) 0.045(8) Uiso 1 1 d . . . H52 H -0.092(2) 0.289(2) 1.0031(19) 0.050(8) Uiso 1 1 d . . . H53 H -0.036(2) 0.4244(19) 0.9572(17) 0.040(7) Uiso 1 1 d . . . H54 H 0.073(2) 0.4262(19) 0.8511(16) 0.036(7) Uiso 1 1 d . . . H56 H -0.0135(19) 0.3643(16) 0.7082(15) 0.028(6) Uiso 1 1 d . . . H57 H -0.034(2) 0.4549(18) 0.6148(17) 0.039(7) Uiso 1 1 d . . . H58 H 0.092(2) 0.5195(18) 0.5380(17) 0.038(7) Uiso 1 1 d . . . H59 H 0.253(2) 0.4899(19) 0.5608(18) 0.043(8) Uiso 1 1 d . . . H60 H 0.2788(19) 0.3924(16) 0.6518(15) 0.027(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02014(14) 0.02016(14) 0.01907(15) 0.00285(10) 0.00268(10) 0.00516(11) P1 0.0221(2) 0.0263(3) 0.0203(2) 0.0047(2) 0.00340(19) 0.0059(2) P2 0.0211(2) 0.0229(2) 0.0212(2) 0.00321(19) 0.00157(19) 0.0045(2) P3 0.0313(3) 0.0219(2) 0.0196(2) 0.00318(19) 0.0040(2) 0.0085(2) P4 0.0226(2) 0.0206(2) 0.0242(3) 0.00096(19) 0.00239(19) 0.0054(2) N1 0.0251(9) 0.0246(8) 0.0245(9) 0.0059(7) 0.0053(7) 0.0041(7) N2 0.0317(10) 0.0344(10) 0.0457(12) 0.0119(9) 0.0089(9) 0.0133(9) O1 0.0280(8) 0.0376(9) 0.0593(11) -0.0123(8) 0.0093(8) 0.0106(7) O2 0.0587(15) 0.136(3) 0.0805(18) 0.0450(18) -0.0096(13) 0.0219(16) O3 0.0503(10) 0.0349(9) 0.0393(9) 0.0025(7) 0.0141(8) 0.0145(8) O4 0.0364(10) 0.0432(11) 0.114(2) 0.0115(12) 0.0223(11) 0.0121(9) O5 0.0463(10) 0.0369(9) 0.0508(11) -0.0044(8) -0.0103(8) 0.0155(8) O6 0.0598(13) 0.0571(13) 0.0759(15) -0.0013(11) 0.0305(12) 0.0216(11) O7 0.0275(9) 0.0496(11) 0.0753(14) -0.0111(10) -0.0157(9) 0.0073(8) O8 0.0579(13) 0.0414(11) 0.0740(15) 0.0094(10) -0.0143(11) 0.0199(9) B1 0.0273(11) 0.0236(11) 0.0268(12) 0.0055(9) 0.0004(9) 0.0038(9) C1 0.0310(11) 0.0348(12) 0.0206(10) 0.0024(9) 0.0001(8) 0.0053(9) C2 0.0261(10) 0.0301(11) 0.0245(10) 0.0034(9) -0.0020(8) 0.0041(9) C3 0.0435(13) 0.0307(11) 0.0215(11) -0.0008(9) 0.0000(9) 0.0077(10) C4 0.0329(11) 0.0244(10) 0.0281(11) -0.0040(8) 0.0036(9) 0.0060(9) C5 0.0252(10) 0.0332(12) 0.0254(11) 0.0045(9) 0.0053(8) 0.0086(9) C6 0.0300(11) 0.0274(11) 0.0285(11) 0.0006(9) 0.0038(9) 0.0098(9) C7 0.0347(12) 0.0320(12) 0.0370(13) -0.0043(10) 0.0063(10) 0.0150(10) C8 0.0339(15) 0.0548(19) 0.085(3) -0.0096(18) 0.0182(16) 0.0130(14) C9 0.0317(12) 0.0361(12) 0.0293(11) 0.0124(10) 0.0056(9) 0.0130(10) C10 0.0519(16) 0.0679(18) 0.0431(15) 0.0335(14) 0.0224(12) 0.0316(14) C11 0.0527(17) 0.086(2) 0.0470(16) 0.0416(16) 0.0150(13) 0.0314(16) C12 0.106(4) 0.229(8) 0.120(4) 0.061(5) -0.033(4) 0.073(5) C13 0.0266(10) 0.0258(10) 0.0237(10) 0.0024(8) 0.0003(8) 0.0070(8) C14 0.0313(12) 0.0275(11) 0.0311(12) 0.0017(9) -0.0029(9) 0.0062(9) C15 0.0361(12) 0.0252(11) 0.0329(12) 0.0014(9) -0.0013(10) 0.0062(9) C16 0.061(2) 0.0525(19) 0.059(2) 0.0001(16) 0.0164(17) 0.0275(17) C17 0.0255(10) 0.0263(11) 0.0309(12) 0.0047(9) 0.0064(9) 0.0036(9) C18 0.0282(12) 0.0356(13) 0.0543(16) 0.0104(12) 0.0106(11) 0.0079(10) C19 0.0318(12) 0.0342(12) 0.0515(15) 0.0030(11) 0.0145(11) 0.0081(10) C20 0.0373(15) 0.0555(18) 0.080(2) -0.0129(16) 0.0166(15) 0.0059(13) C21 0.0517(15) 0.0279(11) 0.0231(11) 0.0060(9) 0.0023(10) 0.0169(11) C22 0.0411(15) 0.0296(13) 0.074(2) 0.0024(14) -0.0172(15) 0.0119(11) C23 0.0530(16) 0.0314(12) 0.0433(14) 0.0023(11) -0.0131(12) 0.0185(12) C24 0.0512(18) 0.072(2) 0.067(2) 0.0047(17) 0.0097(15) 0.0196(16) C25 0.0421(13) 0.0312(12) 0.0313(12) 0.0061(10) 0.0166(10) 0.0119(11) C26 0.134(4) 0.130(3) 0.0540(19) 0.058(2) 0.063(2) 0.103(3) C27 0.107(3) 0.072(2) 0.065(2) 0.0336(18) 0.062(2) 0.048(2) C28 0.098(3) 0.091(3) 0.126(4) 0.006(3) 0.062(3) 0.047(3) C29 0.0233(10) 0.0248(10) 0.0309(11) -0.0005(9) 0.0008(8) 0.0063(8) C30 0.0273(11) 0.0275(11) 0.0296(11) 0.0009(9) -0.0010(9) 0.0055(9) C31 0.0296(12) 0.0307(12) 0.0419(14) 0.0041(10) -0.0049(10) 0.0074(9) C32 0.0323(16) 0.085(3) 0.133(4) -0.019(3) -0.0166(19) 0.0183(17) C33 0.0261(11) 0.0239(10) 0.0357(12) 0.0050(9) 0.0037(9) 0.0046(9) C34 0.0303(12) 0.0255(11) 0.0475(15) 0.0065(10) 0.0061(10) 0.0068(9) C35 0.0422(14) 0.0327(13) 0.0560(17) 0.0148(12) 0.0003(12) 0.0110(11) C36 0.079(2) 0.057(2) 0.089(3) 0.0145(19) 0.011(2) 0.0298(19) C37 0.0321(11) 0.0263(10) 0.0311(11) 0.0077(9) 0.0123(9) 0.0077(9) C38 0.0346(12) 0.0278(11) 0.0331(12) 0.0019(9) 0.0125(9) 0.0054(9) C39 0.0451(15) 0.0340(13) 0.0437(15) -0.0066(11) 0.0175(12) -0.0003(11) C40 0.0660(19) 0.0238(12) 0.067(2) 0.0021(12) 0.0424(17) 0.0067(12) C41 0.0683(19) 0.0324(13) 0.0600(18) 0.0210(13) 0.0387(16) 0.0251(14) C42 0.0482(15) 0.0374(13) 0.0414(14) 0.0145(11) 0.0194(12) 0.0183(12) C43 0.0301(11) 0.0409(13) 0.0322(12) 0.0218(10) -0.0013(9) 0.0010(10) C44 0.0326(13) 0.070(2) 0.0451(16) 0.0302(15) 0.0067(11) 0.0118(13) C45 0.0311(14) 0.105(3) 0.065(2) 0.056(2) 0.0094(14) 0.0118(17) C46 0.0332(16) 0.101(3) 0.075(2) 0.063(2) -0.0160(16) -0.0201(18) C47 0.0501(18) 0.0592(19) 0.0537(18) 0.0308(16) -0.0217(15) -0.0206(15) C48 0.0413(14) 0.0421(14) 0.0380(13) 0.0183(11) -0.0086(11) -0.0062(12) C49 0.0256(10) 0.0257(10) 0.0234(10) 0.0015(8) -0.0041(8) 0.0030(8) C50 0.0332(11) 0.0268(11) 0.0258(11) 0.0028(8) 0.0010(9) 0.0042(9) C51 0.0393(13) 0.0394(13) 0.0271(11) 0.0059(10) 0.0024(10) 0.0027(10) C52 0.0401(14) 0.0561(16) 0.0271(12) 0.0043(11) 0.0053(10) 0.0136(12) C53 0.0451(14) 0.0453(14) 0.0293(12) -0.0047(10) -0.0018(10) 0.0205(12) C54 0.0389(13) 0.0296(12) 0.0308(12) 0.0021(9) -0.0029(9) 0.0093(10) C55 0.0328(11) 0.0196(9) 0.0225(10) 0.0008(8) -0.0024(8) 0.0030(8) C56 0.0352(12) 0.0304(11) 0.0257(11) 0.0028(9) -0.0013(9) 0.0077(9) C57 0.0441(14) 0.0380(13) 0.0300(12) 0.0028(10) -0.0041(10) 0.0188(11) C58 0.0587(16) 0.0295(12) 0.0258(11) 0.0067(9) -0.0041(10) 0.0131(11) C59 0.0463(14) 0.0297(11) 0.0258(11) 0.0053(9) 0.0010(10) 0.0012(10) C60 0.0334(12) 0.0266(11) 0.0287(11) 0.0046(9) -0.0009(9) 0.0032(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 Fe1 N1 1.8337(18) . ? Fe1 P3 2.2302(7) . ? Fe1 P1 2.2308(7) . ? Fe1 P4 2.2373(6) . ? Fe1 P2 2.2379(6) . ? Fe1 H1 1.39(3) . ? P1 C5 1.830(2) . ? P1 C9 1.838(2) . ? P1 C1 1.848(2) . ? P2 C17 1.835(2) . ? P2 C13 1.836(2) . ? P2 C2 1.840(2) . ? P3 C25 1.837(2) . ? P3 C21 1.839(2) . ? P3 C3 1.849(2) . ? P4 C33 1.835(2) . ? P4 C29 1.840(2) . ? P4 C4 1.840(2) . ? N1 N2 1.112(3) . ? O1 C7 1.417(3) . ? O1 C8 1.417(3) . ? O2 C11 1.389(4) . ? O2 C12 1.424(5) . ? O3 C15 1.413(3) . ? O3 C16 1.417(3) . ? O4 C19 1.405(3) . ? O4 C20 1.405(3) . ? O5 C23 1.402(3) . ? O5 C24 1.485(4) . ? O6 C27 1.375(4) . ? O6 C28 1.416(4) . ? O7 C31 1.411(3) . ? O7 C32 1.433(4) . ? O8 C36 1.380(4) . ? O8 C35 1.424(3) . ? B1 C37 1.641(3) . ? B1 C43 1.647(3) . ? B1 C55 1.650(3) . ? B1 C49 1.655(3) . ? C1 C2 1.523(3) . ? C1 H1A 0.95(3) . ? C1 H1B 0.91(3) . ? C2 H2A 0.95(3) . ? C2 H2B 0.95(3) . ? C3 C4 1.521(3) . ? C3 H3A 0.94(3) . ? C3 H3B 0.92(3) . ? C4 H4A 1.00(3) . ? C4 H4B 1.02(3) . ? C5 C6 1.529(3) . ? C5 H5A 0.98(3) . ? C5 H5B 0.95(3) . ? C6 C7 1.513(3) . ? C6 H6A 0.93(2) . ? C6 H6B 1.00(3) . ? C7 H7A 0.98(3) . ? C7 H7B 0.99(3) . ? C8 H8A 1.00(4) . ? C8 H8B 1.00(4) . ? C8 H8C 0.94(4) . ? C9 C10 1.522(3) . ? C9 H9A 0.97(3) . ? C9 H9B 0.97(3) . ? C10 C11 1.512(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.524(3) . ? C13 H13A 0.92(3) . ? C13 H13B 0.98(2) . ? C14 C15 1.516(3) . ? C14 H14A 0.95(3) . ? C14 H14B 0.90(3) . ? C15 H15A 0.96(3) . ? C15 H15B 0.94(3) . ? C16 H16A 0.87(4) . ? C16 H16B 0.94(4) . ? C16 H16C 0.93(4) . ? C17 C18 1.518(3) . ? C17 H17A 0.88(3) . ? C17 H17B 0.90(3) . ? C18 C19 1.510(3) . ? C18 H18A 0.98(3) . ? C18 H18B 0.88(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.503(4) . ? C21 H21A 0.95(3) . ? C21 H21B 0.93(3) . ? C22 C23 1.518(4) . ? C22 H22A 0.86(3) . ? C22 H22B 1.02(5) . ? C23 H23A 0.86(4) . ? C23 H23B 1.03(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.512(4) . ? C25 H25A 0.97(3) . ? C25 H25B 0.94(3) . ? C26 C27 1.514(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.529(3) . ? C29 H29A 1.00(2) . ? C29 H29B 0.96(3) . ? C30 C31 1.514(3) . ? C30 H30A 0.88(3) . ? C30 H30B 1.02(3) . ? C31 H31A 1.01(3) . ? C31 H31B 0.90(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.526(3) . ? C33 H33A 0.99(2) . ? C33 H33B 0.89(3) . ? C34 C35 1.526(3) . ? C34 H34A 0.96(3) . ? C34 H34B 0.94(3) . ? C35 H35A 1.03(3) . ? C35 H35B 1.10(2) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.397(3) . ? C37 C42 1.403(3) . ? C38 C39 1.393(3) . ? C38 H38 0.98(2) . ? C39 C40 1.379(4) . ? C39 H39 0.90(3) . ? C40 C41 1.371(5) . ? C40 H40 0.84(4) . ? C41 C42 1.392(4) . ? C41 H41 0.87(3) . ? C42 H42 0.92(3) . ? C43 C48 1.399(4) . ? C43 C44 1.404(4) . ? C44 C45 1.395(4) . ? C44 H44 0.92(3) . ? C45 C46 1.380(6) . ? C45 H45 0.98(4) . ? C46 C47 1.368(6) . ? C46 H46 0.88(4) . ? C47 C48 1.393(4) . ? C47 H47 0.90(4) . ? C48 H48 0.93(3) . ? C49 C54 1.403(3) . ? C49 C50 1.406(3) . ? C50 C51 1.395(3) . ? C50 H50 0.93(3) . ? C51 C52 1.375(4) . ? C51 H51 1.02(3) . ? C52 C53 1.378(4) . ? C52 H52 0.84(3) . ? C53 C54 1.397(4) . ? C53 H53 0.99(3) . ? C54 H54 0.92(3) . ? C55 C60 1.399(3) . ? C55 C56 1.405(3) . ? C56 C57 1.390(3) . ? C56 H56 0.94(3) . ? C57 C58 1.382(4) . ? C57 H57 0.89(3) . ? C58 C59 1.379(4) . ? C58 H58 0.95(3) . ? C59 C60 1.391(3) . ? C59 H59 0.93(3) . ? C60 H60 0.94(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 P3 96.04(6) . . ? N1 Fe1 P1 95.39(6) . . ? P3 Fe1 P1 168.57(2) . . ? N1 Fe1 P4 96.01(6) . . ? P3 Fe1 P4 84.48(2) . . ? P1 Fe1 P4 94.37(2) . . ? N1 Fe1 P2 94.16(6) . . ? P3 Fe1 P2 94.87(2) . . ? P1 Fe1 P2 84.26(2) . . ? P4 Fe1 P2 169.83(2) . . ? N1 Fe1 H1 178.0(11) . . ? P3 Fe1 H1 84.8(11) . . ? P1 Fe1 H1 83.8(11) . . ? P4 Fe1 H1 85.9(11) . . ? P2 Fe1 H1 84.0(11) . . ? C5 P1 C9 103.90(10) . . ? C5 P1 C1 103.39(11) . . ? C9 P1 C1 100.09(11) . . ? C5 P1 Fe1 121.14(7) . . ? C9 P1 Fe1 115.53(8) . . ? C1 P1 Fe1 110.18(7) . . ? C17 P2 C13 102.41(10) . . ? C17 P2 C2 103.61(11) . . ? C13 P2 C2 102.31(10) . . ? C17 P2 Fe1 124.54(8) . . ? C13 P2 Fe1 115.16(7) . . ? C2 P2 Fe1 106.21(8) . . ? C25 P3 C21 103.88(11) . . ? C25 P3 C3 102.35(12) . . ? C21 P3 C3 103.97(12) . . ? C25 P3 Fe1 115.26(8) . . ? C21 P3 Fe1 119.31(8) . . ? C3 P3 Fe1 110.21(8) . . ? C33 P4 C29 102.34(10) . . ? C33 P4 C4 104.23(11) . . ? C29 P4 C4 102.83(11) . . ? C33 P4 Fe1 123.42(8) . . ? C29 P4 Fe1 114.74(7) . . ? C4 P4 Fe1 107.07(8) . . ? N2 N1 Fe1 178.85(19) . . ? C7 O1 C8 112.0(2) . . ? C11 O2 C12 110.6(4) . . ? C15 O3 C16 111.5(2) . . ? C19 O4 C20 113.0(2) . . ? C23 O5 C24 107.4(2) . . ? C27 O6 C28 112.8(3) . . ? C31 O7 C32 110.6(2) . . ? C36 O8 C35 112.8(2) . . ? C37 B1 C43 112.11(19) . . ? C37 B1 C55 108.51(17) . . ? C43 B1 C55 106.96(17) . . ? C37 B1 C49 108.04(17) . . ? C43 B1 C49 109.29(18) . . ? C55 B1 C49 111.96(18) . . ? C2 C1 P1 107.55(15) . . ? C2 C1 H1A 112.1(17) . . ? P1 C1 H1A 108.0(17) . . ? C2 C1 H1B 112.7(18) . . ? P1 C1 H1B 107.5(18) . . ? H1A C1 H1B 109(2) . . ? C1 C2 P2 105.85(15) . . ? C1 C2 H2A 116.9(15) . . ? P2 C2 H2A 110.5(15) . . ? C1 C2 H2B 111.5(15) . . ? P2 C2 H2B 106.5(14) . . ? H2A C2 H2B 105(2) . . ? C4 C3 P3 108.29(16) . . ? C4 C3 H3A 113.4(18) . . ? P3 C3 H3A 104.4(18) . . ? C4 C3 H3B 113.2(18) . . ? P3 C3 H3B 108.1(18) . . ? H3A C3 H3B 109(2) . . ? C3 C4 P4 106.44(15) . . ? C3 C4 H4A 111.7(15) . . ? P4 C4 H4A 113.0(15) . . ? C3 C4 H4B 114.4(15) . . ? P4 C4 H4B 104.5(14) . . ? H4A C4 H4B 107(2) . . ? C6 C5 P1 115.07(16) . . ? C6 C5 H5A 111.1(14) . . ? P1 C5 H5A 104.0(15) . . ? C6 C5 H5B 110.2(15) . . ? P1 C5 H5B 108.0(15) . . ? H5A C5 H5B 108(2) . . ? C7 C6 C5 112.00(19) . . ? C7 C6 H6A 108.4(14) . . ? C5 C6 H6A 110.2(14) . . ? C7 C6 H6B 107.7(15) . . ? C5 C6 H6B 112.1(15) . . ? H6A C6 H6B 106(2) . . ? O1 C7 C6 108.76(17) . . ? O1 C7 H7A 109.1(16) . . ? C6 C7 H7A 113.1(16) . . ? O1 C7 H7B 108.0(16) . . ? C6 C7 H7B 109.5(16) . . ? H7A C7 H7B 108(2) . . ? O1 C8 H8A 107(2) . . ? O1 C8 H8B 107(2) . . ? H8A C8 H8B 104(3) . . ? O1 C8 H8C 107(2) . . ? H8A C8 H8C 121(3) . . ? H8B C8 H8C 110(3) . . ? C10 C9 P1 117.21(17) . . ? C10 C9 H9A 112.2(16) . . ? P1 C9 H9A 100.3(16) . . ? C10 C9 H9B 113.1(18) . . ? P1 C9 H9B 111.2(17) . . ? H9A C9 H9B 101(2) . . ? C11 C10 C9 112.6(2) . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? O2 C11 C10 106.4(3) . . ? O2 C11 H11A 110.4 . . ? C10 C11 H11A 110.4 . . ? O2 C11 H11B 110.4 . . ? C10 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P2 117.33(15) . . ? C14 C13 H13A 108.8(17) . . ? P2 C13 H13A 106.8(17) . . ? C14 C13 H13B 107.5(14) . . ? P2 C13 H13B 108.5(14) . . ? H13A C13 H13B 108(2) . . ? C15 C14 C13 112.08(19) . . ? C15 C14 H14A 108.9(16) . . ? C13 C14 H14A 110.2(16) . . ? C15 C14 H14B 110.7(17) . . ? C13 C14 H14B 108.9(18) . . ? H14A C14 H14B 106(2) . . ? O3 C15 C14 108.87(19) . . ? O3 C15 H15A 107.1(15) . . ? C14 C15 H15A 111.6(15) . . ? O3 C15 H15B 108.2(16) . . ? C14 C15 H15B 111.9(16) . . ? H15A C15 H15B 109(2) . . ? O3 C16 H16A 113(3) . . ? O3 C16 H16B 106(2) . . ? H16A C16 H16B 114(3) . . ? O3 C16 H16C 106(2) . . ? H16A C16 H16C 100(3) . . ? H16B C16 H16C 117(3) . . ? C18 C17 P2 116.32(16) . . ? C18 C17 H17A 109(2) . . ? P2 C17 H17A 104.1(19) . . ? C18 C17 H17B 109.4(17) . . ? P2 C17 H17B 106.8(17) . . ? H17A C17 H17B 111(3) . . ? C19 C18 C17 111.4(2) . . ? C19 C18 H18A 108.2(19) . . ? C17 C18 H18A 108.6(19) . . ? C19 C18 H18B 110(2) . . ? C17 C18 H18B 111(2) . . ? H18A C18 H18B 109(3) . . ? O4 C19 C18 109.7(2) . . ? O4 C19 H19A 109.7 . . ? C18 C19 H19A 109.7 . . ? O4 C19 H19B 109.7 . . ? C18 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? O4 C20 H20A 109.5 . . ? O4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P3 114.61(19) . . ? C22 C21 H21A 111.7(16) . . ? P3 C21 H21A 108.2(16) . . ? C22 C21 H21B 111.4(17) . . ? P3 C21 H21B 109.8(17) . . ? H21A C21 H21B 100(2) . . ? C21 C22 C23 115.0(3) . . ? C21 C22 H22A 112.0(19) . . ? C23 C22 H22A 105.2(19) . . ? C21 C22 H22B 105(3) . . ? C23 C22 H22B 106(3) . . ? H22A C22 H22B 113(3) . . ? O5 C23 C22 112.4(2) . . ? O5 C23 H23A 107(2) . . ? C22 C23 H23A 112(2) . . ? O5 C23 H23B 95(2) . . ? C22 C23 H23B 116.1(19) . . ? H23A C23 H23B 113(3) . . ? O5 C24 H24A 109.5 . . ? O5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 P3 117.4(2) . . ? C26 C25 H25A 107.2(19) . . ? P3 C25 H25A 109.4(19) . . ? C26 C25 H25B 105.5(17) . . ? P3 C25 H25B 108.9(17) . . ? H25A C25 H25B 108(3) . . ? C25 C26 C27 112.0(3) . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? O6 C27 C26 107.6(3) . . ? O6 C27 H27A 110.2 . . ? C26 C27 H27A 110.2 . . ? O6 C27 H27B 110.2 . . ? C26 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? O6 C28 H28A 109.5 . . ? O6 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O6 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 P4 118.14(15) . . ? C30 C29 H29A 110.8(15) . . ? P4 C29 H29A 104.9(14) . . ? C30 C29 H29B 110.5(16) . . ? P4 C29 H29B 104.2(16) . . ? H29A C29 H29B 108(2) . . ? C31 C30 C29 109.64(18) . . ? C31 C30 H30A 106.8(17) . . ? C29 C30 H30A 110.5(18) . . ? C31 C30 H30B 110.7(15) . . ? C29 C30 H30B 109.4(15) . . ? H30A C30 H30B 110(2) . . ? O7 C31 C30 109.8(2) . . ? O7 C31 H31A 109.0(16) . . ? C30 C31 H31A 109.3(15) . . ? O7 C31 H31B 109.3(17) . . ? C30 C31 H31B 110.2(17) . . ? H31A C31 H31B 109(2) . . ? O7 C32 H32A 109.5 . . ? O7 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O7 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 P4 115.50(16) . . ? C34 C33 H33A 112.9(14) . . ? P4 C33 H33A 104.5(14) . . ? C34 C33 H33B 111.5(17) . . ? P4 C33 H33B 108.1(18) . . ? H33A C33 H33B 103(2) . . ? C35 C34 C33 110.9(2) . . ? C35 C34 H34A 111.9(15) . . ? C33 C34 H34A 108.8(15) . . ? C35 C34 H34B 109.9(16) . . ? C33 C34 H34B 109.8(16) . . ? H34A C34 H34B 105(2) . . ? O8 C35 C34 113.6(2) . . ? O8 C35 H35A 109.3(15) . . ? C34 C35 H35A 108.4(16) . . ? O8 C35 H35B 101.2(11) . . ? C34 C35 H35B 103.3(11) . . ? H35A C35 H35B 121.0(19) . . ? O8 C36 H36A 109.5 . . ? O8 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O8 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C42 115.2(2) . . ? C38 C37 B1 121.81(19) . . ? C42 C37 B1 122.8(2) . . ? C39 C38 C37 122.6(2) . . ? C39 C38 H38 118.0(15) . . ? C37 C38 H38 119.4(14) . . ? C40 C39 C38 120.2(3) . . ? C40 C39 H39 118.2(19) . . ? C38 C39 H39 121.5(19) . . ? C41 C40 C39 119.1(3) . . ? C41 C40 H40 117(2) . . ? C39 C40 H40 124(2) . . ? C40 C41 C42 120.5(3) . . ? C40 C41 H41 122(2) . . ? C42 C41 H41 118(2) . . ? C41 C42 C37 122.4(3) . . ? C41 C42 H42 119.1(17) . . ? C37 C42 H42 118.5(17) . . ? C48 C43 C44 115.2(2) . . ? C48 C43 B1 121.2(2) . . ? C44 C43 B1 123.4(2) . . ? C45 C44 C43 122.3(3) . . ? C45 C44 H44 117.6(19) . . ? C43 C44 H44 120.0(19) . . ? C46 C45 C44 120.2(4) . . ? C46 C45 H45 128(2) . . ? C44 C45 H45 112(2) . . ? C47 C46 C45 119.2(3) . . ? C47 C46 H46 116(3) . . ? C45 C46 H46 125(3) . . ? C46 C47 C48 120.4(4) . . ? C46 C47 H47 123(2) . . ? C48 C47 H47 117(2) . . ? C47 C48 C43 122.7(3) . . ? C47 C48 H48 115.7(17) . . ? C43 C48 H48 121.6(17) . . ? C54 C49 C50 114.2(2) . . ? C54 C49 B1 123.73(19) . . ? C50 C49 B1 122.11(19) . . ? C51 C50 C49 123.4(2) . . ? C51 C50 H50 117.1(15) . . ? C49 C50 H50 119.5(15) . . ? C52 C51 C50 119.9(2) . . ? C52 C51 H51 119.0(16) . . ? C50 C51 H51 121.0(16) . . ? C51 C52 C53 119.2(2) . . ? C51 C52 H52 122(2) . . ? C53 C52 H52 119(2) . . ? C52 C53 C54 120.1(2) . . ? C52 C53 H53 119.0(16) . . ? C54 C53 H53 120.9(16) . . ? C53 C54 C49 123.1(2) . . ? C53 C54 H54 117.8(16) . . ? C49 C54 H54 119.1(16) . . ? C60 C55 C56 114.6(2) . . ? C60 C55 B1 121.47(19) . . ? C56 C55 B1 123.84(19) . . ? C57 C56 C55 122.6(2) . . ? C57 C56 H56 116.4(15) . . ? C55 C56 H56 121.0(15) . . ? C58 C57 C56 120.6(2) . . ? C58 C57 H57 120.7(18) . . ? C56 C57 H57 118.7(18) . . ? C59 C58 C57 118.7(2) . . ? C59 C58 H58 123.1(16) . . ? C57 C58 H58 118.1(16) . . ? C58 C59 C60 119.9(2) . . ? C58 C59 H59 118.1(17) . . ? C60 C59 H59 121.7(18) . . ? C59 C60 C55 123.4(2) . . ? C59 C60 H60 116.8(15) . . ? C55 C60 H60 119.8(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 P1 C5 147.19(10) . . . . ? P3 Fe1 P1 C5 -33.00(16) . . . . ? P4 Fe1 P1 C5 50.72(9) . . . . ? P2 Fe1 P1 C5 -119.16(9) . . . . ? N1 Fe1 P1 C9 20.35(11) . . . . ? P3 Fe1 P1 C9 -159.84(14) . . . . ? P4 Fe1 P1 C9 -76.12(9) . . . . ? P2 Fe1 P1 C9 114.00(9) . . . . ? N1 Fe1 P1 C1 -92.13(10) . . . . ? P3 Fe1 P1 C1 87.68(14) . . . . ? P4 Fe1 P1 C1 171.40(8) . . . . ? P2 Fe1 P1 C1 1.52(9) . . . . ? N1 Fe1 P2 C17 -51.54(11) . . . . ? P3 Fe1 P2 C17 44.89(10) . . . . ? P1 Fe1 P2 C17 -146.55(9) . . . . ? P4 Fe1 P2 C17 130.74(15) . . . . ? N1 Fe1 P2 C13 -179.25(9) . . . . ? P3 Fe1 P2 C13 -82.81(8) . . . . ? P1 Fe1 P2 C13 85.74(8) . . . . ? P4 Fe1 P2 C13 3.03(16) . . . . ? N1 Fe1 P2 C2 68.30(9) . . . . ? P3 Fe1 P2 C2 164.73(8) . . . . ? P1 Fe1 P2 C2 -26.71(8) . . . . ? P4 Fe1 P2 C2 -109.42(14) . . . . ? N1 Fe1 P3 C25 20.12(11) . . . . ? P1 Fe1 P3 C25 -159.69(14) . . . . ? P4 Fe1 P3 C25 115.60(10) . . . . ? P2 Fe1 P3 C25 -74.59(10) . . . . ? N1 Fe1 P3 C21 144.81(11) . . . . ? P1 Fe1 P3 C21 -35.00(17) . . . . ? P4 Fe1 P3 C21 -119.71(10) . . . . ? P2 Fe1 P3 C21 50.10(10) . . . . ? N1 Fe1 P3 C3 -95.07(10) . . . . ? P1 Fe1 P3 C3 85.12(15) . . . . ? P4 Fe1 P3 C3 0.41(9) . . . . ? P2 Fe1 P3 C3 170.21(9) . . . . ? N1 Fe1 P4 C33 -49.93(10) . . . . ? P3 Fe1 P4 C33 -145.44(9) . . . . ? P1 Fe1 P4 C33 45.97(9) . . . . ? P2 Fe1 P4 C33 127.78(15) . . . . ? N1 Fe1 P4 C29 -175.81(10) . . . . ? P3 Fe1 P4 C29 88.68(8) . . . . ? P1 Fe1 P4 C29 -79.91(8) . . . . ? P2 Fe1 P4 C29 1.90(16) . . . . ? N1 Fe1 P4 C4 70.79(10) . . . . ? P3 Fe1 P4 C4 -24.73(8) . . . . ? P1 Fe1 P4 C4 166.69(8) . . . . ? P2 Fe1 P4 C4 -111.50(14) . . . . ? P3 Fe1 N1 N2 -100(9) . . . . ? P1 Fe1 N1 N2 80(9) . . . . ? P4 Fe1 N1 N2 175(100) . . . . ? P2 Fe1 N1 N2 -5(9) . . . . ? C5 P1 C1 C2 160.80(16) . . . . ? C9 P1 C1 C2 -92.16(17) . . . . ? Fe1 P1 C1 C2 29.96(17) . . . . ? P1 C1 C2 P2 -51.00(18) . . . . ? C17 P2 C2 C1 -174.75(15) . . . . ? C13 P2 C2 C1 -68.54(17) . . . . ? Fe1 P2 C2 C1 52.57(16) . . . . ? C25 P3 C3 C4 -93.31(18) . . . . ? C21 P3 C3 C4 158.77(16) . . . . ? Fe1 P3 C3 C4 29.78(18) . . . . ? P3 C3 C4 P4 -49.15(19) . . . . ? C33 P4 C4 C3 -177.99(16) . . . . ? C29 P4 C4 C3 -71.50(18) . . . . ? Fe1 P4 C4 C3 49.76(17) . . . . ? C9 P1 C5 C6 -174.95(17) . . . . ? C1 P1 C5 C6 -70.80(18) . . . . ? Fe1 P1 C5 C6 53.12(19) . . . . ? P1 C5 C6 C7 -176.93(16) . . . . ? C8 O1 C7 C6 -179.4(3) . . . . ? C5 C6 C7 O1 63.1(3) . . . . ? C5 P1 C9 C10 39.7(2) . . . . ? C1 P1 C9 C10 -66.9(2) . . . . ? Fe1 P1 C9 C10 174.86(18) . . . . ? P1 C9 C10 C11 163.4(2) . . . . ? C12 O2 C11 C10 -174.7(4) . . . . ? C9 C10 C11 O2 -66.3(4) . . . . ? C17 P2 C13 C14 56.91(19) . . . . ? C2 P2 C13 C14 -50.23(19) . . . . ? Fe1 P2 C13 C14 -164.95(15) . . . . ? P2 C13 C14 C15 172.61(16) . . . . ? C16 O3 C15 C14 -174.7(2) . . . . ? C13 C14 C15 O3 -69.5(2) . . . . ? C13 P2 C17 C18 -162.27(19) . . . . ? C2 P2 C17 C18 -56.1(2) . . . . ? Fe1 P2 C17 C18 64.9(2) . . . . ? P2 C17 C18 C19 -178.06(19) . . . . ? C20 O4 C19 C18 166.5(3) . . . . ? C17 C18 C19 O4 -176.7(2) . . . . ? C25 P3 C21 C22 -160.5(2) . . . . ? C3 P3 C21 C22 -53.7(2) . . . . ? Fe1 P3 C21 C22 69.5(2) . . . . ? P3 C21 C22 C23 -162.6(2) . . . . ? C24 O5 C23 C22 80.6(3) . . . . ? C21 C22 C23 O5 73.7(4) . . . . ? C21 P3 C25 C26 53.3(3) . . . . ? C3 P3 C25 C26 -54.7(3) . . . . ? Fe1 P3 C25 C26 -174.3(2) . . . . ? P3 C25 C26 C27 177.1(3) . . . . ? C28 O6 C27 C26 -171.4(4) . . . . ? C25 C26 C27 O6 -61.6(5) . . . . ? C33 P4 C29 C30 62.5(2) . . . . ? C4 P4 C29 C30 -45.4(2) . . . . ? Fe1 P4 C29 C30 -161.28(15) . . . . ? P4 C29 C30 C31 -177.62(17) . . . . ? C32 O7 C31 C30 -166.9(3) . . . . ? C29 C30 C31 O7 168.2(2) . . . . ? C29 P4 C33 C34 -163.62(18) . . . . ? C4 P4 C33 C34 -56.8(2) . . . . ? Fe1 P4 C33 C34 65.3(2) . . . . ? P4 C33 C34 C35 -172.15(18) . . . . ? C36 O8 C35 C34 79.0(3) . . . . ? C33 C34 C35 O8 177.1(2) . . . . ? C43 B1 C37 C38 -145.2(2) . . . . ? C55 B1 C37 C38 -27.3(3) . . . . ? C49 B1 C37 C38 94.3(2) . . . . ? C43 B1 C37 C42 40.2(3) . . . . ? C55 B1 C37 C42 158.2(2) . . . . ? C49 B1 C37 C42 -80.2(3) . . . . ? C42 C37 C38 C39 0.8(3) . . . . ? B1 C37 C38 C39 -174.1(2) . . . . ? C37 C38 C39 C40 -1.1(4) . . . . ? C38 C39 C40 C41 0.6(4) . . . . ? C39 C40 C41 C42 0.1(4) . . . . ? C40 C41 C42 C37 -0.3(4) . . . . ? C38 C37 C42 C41 -0.1(3) . . . . ? B1 C37 C42 C41 174.8(2) . . . . ? C37 B1 C43 C48 -161.6(2) . . . . ? C55 B1 C43 C48 79.5(2) . . . . ? C49 B1 C43 C48 -41.9(3) . . . . ? C37 B1 C43 C44 24.0(3) . . . . ? C55 B1 C43 C44 -94.8(3) . . . . ? C49 B1 C43 C44 143.8(2) . . . . ? C48 C43 C44 C45 0.2(4) . . . . ? B1 C43 C44 C45 174.9(2) . . . . ? C43 C44 C45 C46 -0.5(4) . . . . ? C44 C45 C46 C47 -0.2(4) . . . . ? C45 C46 C47 C48 1.0(4) . . . . ? C46 C47 C48 C43 -1.3(4) . . . . ? C44 C43 C48 C47 0.7(4) . . . . ? B1 C43 C48 C47 -174.1(2) . . . . ? C37 B1 C49 C54 -153.5(2) . . . . ? C43 B1 C49 C54 84.3(2) . . . . ? C55 B1 C49 C54 -34.0(3) . . . . ? C37 B1 C49 C50 26.9(3) . . . . ? C43 B1 C49 C50 -95.3(2) . . . . ? C55 B1 C49 C50 146.4(2) . . . . ? C54 C49 C50 C51 1.8(3) . . . . ? B1 C49 C50 C51 -178.6(2) . . . . ? C49 C50 C51 C52 -0.3(4) . . . . ? C50 C51 C52 C53 -1.1(4) . . . . ? C51 C52 C53 C54 0.9(4) . . . . ? C52 C53 C54 C49 0.7(4) . . . . ? C50 C49 C54 C53 -2.0(3) . . . . ? B1 C49 C54 C53 178.4(2) . . . . ? C37 B1 C55 C60 -85.3(2) . . . . ? C43 B1 C55 C60 35.8(3) . . . . ? C49 B1 C55 C60 155.54(19) . . . . ? C37 B1 C55 C56 90.8(2) . . . . ? C43 B1 C55 C56 -148.0(2) . . . . ? C49 B1 C55 C56 -28.3(3) . . . . ? C60 C55 C56 C57 -2.6(3) . . . . ? B1 C55 C56 C57 -179.0(2) . . . . ? C55 C56 C57 C58 0.8(4) . . . . ? C56 C57 C58 C59 1.6(4) . . . . ? C57 C58 C59 C60 -2.1(4) . . . . ? C58 C59 C60 C55 0.1(4) . . . . ? C56 C55 C60 C59 2.2(3) . . . . ? B1 C55 C60 C59 178.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.126 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.068 #===END data_just11 _database_code_depnum_ccdc_archive 'CCDC 735062' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H100 B Cl Fe O8 P4' _chemical_formula_weight 1175.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5949(11) _cell_length_b 15.4389(13) _cell_length_c 16.0182(13) _cell_angle_alpha 97.9400(10) _cell_angle_beta 94.0320(10) _cell_angle_gamma 103.9340(10) _cell_volume 3213.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4444 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 23.07 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9161 _exptl_absorpt_correction_T_max 0.9508 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30038 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.00 _reflns_number_total 13652 _reflns_number_gt 9832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+2.0635P] 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 13652 _refine_ls_number_parameters 690 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1504 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.096 _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 Fe1 Fe 0.68793(3) 0.29200(3) 0.24900(3) 0.02454(12) Uani 1 1 d . . . Cl1 Cl 0.56991(6) 0.38105(5) 0.25004(6) 0.0332(2) Uani 1 1 d . . . P1 P 0.82796(6) 0.40861(5) 0.29553(6) 0.02546(19) Uani 1 1 d . . . P2 P 0.69726(7) 0.27499(6) 0.39033(6) 0.0280(2) Uani 1 1 d . B . P3 P 0.71081(6) 0.28262(6) 0.10633(6) 0.0275(2) Uani 1 1 d . . . P4 P 0.56476(6) 0.16165(6) 0.20265(6) 0.0286(2) Uani 1 1 d . . . O1 O 1.21898(19) 0.45742(18) 0.39219(18) 0.0493(7) Uani 1 1 d . . . O2 O 0.7383(2) 0.70251(19) 0.2149(2) 0.0667(10) Uani 1 1 d . . . O3 O 0.7371(2) -0.01398(17) 0.3501(2) 0.0590(9) Uani 1 1 d . . . O5 O 1.04734(18) 0.28612(16) 0.11669(18) 0.0463(7) Uani 1 1 d . . . O7 O 0.6798(2) -0.07656(16) 0.07115(17) 0.0433(6) Uani 1 1 d . . . O8 O 0.2028(2) 0.1892(2) 0.2769(3) 0.0980(15) Uani 1 1 d . . . B1 B 0.1546(3) 0.8037(2) 0.2643(3) 0.0298(9) Uani 1 1 d . . . C1 C 0.8176(3) 0.4475(2) 0.4070(2) 0.0304(7) Uani 1 1 d . . . H1A H 0.8808 0.4930 0.4326 0.037 Uiso 1 1 calc R . . H1B H 0.7596 0.4756 0.4118 0.037 Uiso 1 1 calc R . . C2 C 0.8010(3) 0.3656(2) 0.4524(2) 0.0326(8) Uani 1 1 d . . . H2A H 0.7826 0.3817 0.5101 0.039 Uiso 1 1 calc R . . H2B H 0.8644 0.3449 0.4573 0.039 Uiso 1 1 calc R . . C3 C 0.6174(3) 0.1829(2) 0.0461(2) 0.0352(8) Uani 1 1 d . . . H3A H 0.6000 0.1939 -0.0119 0.042 Uiso 1 1 calc R . . H3B H 0.6462 0.1296 0.0418 0.042 Uiso 1 1 calc R . . C4 C 0.5224(3) 0.1658(2) 0.0924(2) 0.0336(8) Uani 1 1 d . . . H4A H 0.4743 0.1078 0.0663 0.040 Uiso 1 1 calc R . . H4B H 0.4878 0.2150 0.0898 0.040 Uiso 1 1 calc R . . C5 C 0.9472(2) 0.3723(2) 0.2988(2) 0.0278(7) Uani 1 1 d . . . H5A H 0.9331 0.3120 0.3166 0.033 Uiso 1 1 calc R . . H5B H 0.9666 0.3647 0.2403 0.033 Uiso 1 1 calc R . . C6 C 1.0399(2) 0.4339(2) 0.3566(2) 0.0293(7) Uani 1 1 d . . . H6A H 1.0573 0.4942 0.3390 0.035 Uiso 1 1 calc R . . H6B H 1.0232 0.4415 0.4159 0.035 Uiso 1 1 calc R . . C7 C 1.1302(2) 0.3927(2) 0.3511(2) 0.0348(8) Uani 1 1 d . . . H7A H 1.1182 0.3381 0.3788 0.042 Uiso 1 1 calc R . . H7B H 1.1393 0.3746 0.2910 0.042 Uiso 1 1 calc R . . C8 C 1.3078(3) 0.4264(3) 0.3775(4) 0.0755(16) Uani 1 1 d . . . H8A H 1.3683 0.4720 0.4062 0.113 Uiso 1 1 calc R . . H8B H 1.3134 0.4163 0.3164 0.113 Uiso 1 1 calc R . . H8C H 1.3029 0.3697 0.3997 0.113 Uiso 1 1 calc R . . C9 C 0.8605(2) 0.5117(2) 0.2479(2) 0.0305(8) Uani 1 1 d . . . H9A H 0.9290 0.5479 0.2734 0.037 Uiso 1 1 calc R . . H9B H 0.8642 0.4944 0.1866 0.037 Uiso 1 1 calc R . . C10 C 0.7858(3) 0.5707(2) 0.2588(3) 0.0374(9) Uani 1 1 d . . . H10A H 0.7155 0.5329 0.2410 0.045 Uiso 1 1 calc R . . H10B H 0.7899 0.5964 0.3194 0.045 Uiso 1 1 calc R . . C11 C 0.8078(3) 0.6473(3) 0.2068(3) 0.0501(11) Uani 1 1 d . . . H11A H 0.8778 0.6853 0.2251 0.060 Uiso 1 1 calc R . . H11B H 0.8048 0.6213 0.1463 0.060 Uiso 1 1 calc R . . C12 C 0.6404(4) 0.6571(4) 0.1724(4) 0.095(2) Uani 1 1 d . . . H12A H 0.5940 0.6965 0.1805 0.142 Uiso 1 1 calc R . . H12B H 0.6140 0.6016 0.1956 0.142 Uiso 1 1 calc R . . H12C H 0.6458 0.6418 0.1117 0.142 Uiso 1 1 calc R . . C13 C 0.7204(3) 0.1705(2) 0.4188(2) 0.0360(8) Uani 1 1 d . . . H13A H 0.7332 0.1773 0.4813 0.043 Uiso 1 1 calc R . . H13B H 0.6585 0.1206 0.4002 0.043 Uiso 1 1 calc R . . C14 C 0.8105(3) 0.1451(2) 0.3795(2) 0.0378(9) Uani 1 1 d . . . H14A H 0.8022 0.1464 0.3179 0.045 Uiso 1 1 calc R . . H14B H 0.8738 0.1910 0.4041 0.045 Uiso 1 1 calc R . . C15 C 0.8220(3) 0.0524(2) 0.3932(3) 0.0437(10) Uani 1 1 d . . . H15A H 0.8853 0.0423 0.3715 0.052 Uiso 1 1 calc R . . H15B H 0.8263 0.0488 0.4546 0.052 Uiso 1 1 calc R . . C16 C 0.7429(4) -0.1025(3) 0.3617(4) 0.097(2) Uani 1 1 d . . . H16A H 0.6827 -0.1470 0.3311 0.145 Uiso 1 1 calc R . . H16B H 0.7454 -0.1068 0.4222 0.145 Uiso 1 1 calc R . . H16C H 0.8045 -0.1146 0.3397 0.145 Uiso 1 1 calc R . . C17 C 0.5845(3) 0.2907(3) 0.4392(2) 0.0395(9) Uani 1 1 d D . . H17A H 0.5760 0.3511 0.4317 0.047 Uiso 1 1 calc R A 1 H17B H 0.5245 0.2454 0.4076 0.047 Uiso 1 1 calc R A 1 C18 C 0.5828(4) 0.2834(3) 0.5322(3) 0.0637(13) Uani 0.708(4) 1 d PD B 1 H18A H 0.5907 0.2230 0.5406 0.076 Uiso 0.708(4) 1 calc PR B 1 H18B H 0.6417 0.3291 0.5648 0.076 Uiso 0.708(4) 1 calc PR B 1 C19 C 0.4873(7) 0.2967(6) 0.5668(9) 0.065(3) Uani 0.708(4) 1 d PD B 1 H19A H 0.4274 0.2493 0.5377 0.078 Uiso 0.708(4) 1 calc PR B 1 H19B H 0.4910 0.2942 0.6283 0.078 Uiso 0.708(4) 1 calc PR B 1 O4 O 0.4803(3) 0.3818(3) 0.5515(3) 0.0678(13) Uani 0.708(4) 1 d PD B 1 C20 C 0.4012(7) 0.4089(7) 0.5938(6) 0.115(3) Uani 0.708(4) 1 d PD B 1 H20A H 0.4017 0.4709 0.5861 0.172 Uiso 0.708(4) 1 calc PR B 1 H20B H 0.4124 0.4064 0.6545 0.172 Uiso 0.708(4) 1 calc PR B 1 H20C H 0.3352 0.3682 0.5700 0.172 Uiso 0.708(4) 1 calc PR B 1 C18A C 0.5828(4) 0.2834(3) 0.5322(3) 0.0637(13) Uani 0.292(4) 1 d PD B 2 H18C H 0.6505 0.3150 0.5628 0.076 Uiso 0.292(4) 1 calc PR B 2 H18D H 0.5692 0.2189 0.5390 0.076 Uiso 0.292(4) 1 calc PR B 2 C19A C 0.5022(15) 0.324(2) 0.571(2) 0.065(3) Uani 0.292(4) 1 d PD B 2 H19C H 0.5016 0.3159 0.6315 0.078 Uiso 0.292(4) 1 calc PR B 2 H19D H 0.5185 0.3895 0.5690 0.078 Uiso 0.292(4) 1 calc PR B 2 O4A O 0.4060(9) 0.2818(8) 0.5273(8) 0.0678(13) Uani 0.292(4) 1 d PD B 2 C20A C 0.3267(17) 0.3147(17) 0.5625(15) 0.115(3) Uani 0.292(4) 1 d PD B 2 H20D H 0.2624 0.2873 0.5264 0.172 Uiso 0.292(4) 1 calc PR B 2 H20E H 0.3428 0.3806 0.5660 0.172 Uiso 0.292(4) 1 calc PR B 2 H20F H 0.3202 0.2991 0.6194 0.172 Uiso 0.292(4) 1 calc PR B 2 C21 C 0.8327(3) 0.2739(2) 0.0701(2) 0.0319(8) Uani 1 1 d . . . H21A H 0.8246 0.2610 0.0074 0.038 Uiso 1 1 calc R . . H21B H 0.8831 0.3329 0.0876 0.038 Uiso 1 1 calc R . . C22 C 0.8744(3) 0.2004(2) 0.1045(2) 0.0337(8) Uani 1 1 d . . . H22A H 0.8770 0.2098 0.1671 0.040 Uiso 1 1 calc R . . H22B H 0.8278 0.1404 0.0823 0.040 Uiso 1 1 calc R . . C23 C 0.9799(3) 0.2020(2) 0.0794(2) 0.0391(9) Uani 1 1 d . . . H23A H 1.0034 0.1517 0.0993 0.047 Uiso 1 1 calc R . . H23B H 0.9785 0.1944 0.0169 0.047 Uiso 1 1 calc R . . C24 C 1.1474(3) 0.2942(3) 0.0933(3) 0.0658(14) Uani 1 1 d . . . H24A H 1.1914 0.3529 0.1204 0.099 Uiso 1 1 calc R . . H24B H 1.1458 0.2898 0.0316 0.099 Uiso 1 1 calc R . . H24C H 1.1742 0.2456 0.1117 0.099 Uiso 1 1 calc R . . C25 C 0.6789(3) 0.3749(2) 0.0591(2) 0.0342(8) Uani 1 1 d . D . H25A H 0.6073 0.3743 0.0673 0.041 Uiso 1 1 calc R . . H25B H 0.7224 0.4328 0.0905 0.041 Uiso 1 1 calc R . . C26 C 0.6913(3) 0.3727(3) -0.0348(2) 0.0438(9) Uani 1 1 d D . . H26A H 0.7649 0.3928 -0.0413 0.053 Uiso 1 1 calc R C 1 H26B H 0.6665 0.3094 -0.0640 0.053 Uiso 1 1 calc R C 1 C27 C 0.6373(4) 0.4294(4) -0.0778(3) 0.0731(16) Uani 0.741(5) 1 d PD D 1 H27A H 0.6546 0.4270 -0.1370 0.088 Uiso 0.741(5) 1 calc PR D 1 H27B H 0.5630 0.4029 -0.0800 0.088 Uiso 0.741(5) 1 calc PR D 1 O6 O 0.6580(3) 0.5156(3) -0.0418(3) 0.0591(12) Uani 0.741(5) 1 d PD D 1 C28 C 0.5924(5) 0.5636(5) -0.0834(4) 0.108(2) Uani 0.741(5) 1 d PD D 1 H28A H 0.6115 0.6275 -0.0578 0.162 Uiso 0.741(5) 1 calc PR D 1 H28B H 0.5211 0.5369 -0.0762 0.162 Uiso 0.741(5) 1 calc PR D 1 H28C H 0.6010 0.5582 -0.1440 0.162 Uiso 0.741(5) 1 calc PR D 1 C27A C 0.6373(4) 0.4294(4) -0.0778(3) 0.0731(16) Uani 0.259(5) 1 d PD D 2 H27C H 0.6913 0.4742 -0.0985 0.088 Uiso 0.259(5) 1 calc PR D 2 H27D H 0.5983 0.3892 -0.1291 0.088 Uiso 0.259(5) 1 calc PR D 2 O6A O 0.5751(9) 0.4752(7) -0.0469(7) 0.0591(12) Uani 0.259(5) 1 d PD D 2 C28A C 0.5924(5) 0.5636(5) -0.0834(4) 0.108(2) Uani 0.259(5) 1 d P D 2 H28D H 0.5517 0.6016 -0.0562 0.162 Uiso 0.259(5) 1 calc PR D 2 H28E H 0.5719 0.5501 -0.1446 0.162 Uiso 0.259(5) 1 calc PR D 2 H28F H 0.6648 0.5956 -0.0727 0.162 Uiso 0.259(5) 1 calc PR D 2 C29 C 0.6148(3) 0.0608(2) 0.1928(2) 0.0314(8) Uani 1 1 d . . . H29A H 0.6812 0.0760 0.1696 0.038 Uiso 1 1 calc R . . H29B H 0.6280 0.0471 0.2505 0.038 Uiso 1 1 calc R . . C30 C 0.5484(3) -0.0258(2) 0.1379(2) 0.0331(8) Uani 1 1 d . . . H30A H 0.4858 -0.0476 0.1650 0.040 Uiso 1 1 calc R . . H30B H 0.5278 -0.0120 0.0817 0.040 Uiso 1 1 calc R . . C31 C 0.6041(3) -0.0994(2) 0.1260(2) 0.0354(8) Uani 1 1 d . . . H31A H 0.6359 -0.1060 0.1815 0.043 Uiso 1 1 calc R . . H31B H 0.5555 -0.1577 0.1015 0.043 Uiso 1 1 calc R . . C32 C 0.7308(3) -0.1461(3) 0.0539(3) 0.0606(13) Uani 1 1 d . . . H32A H 0.7827 -0.1283 0.0158 0.091 Uiso 1 1 calc R . . H32B H 0.6814 -0.2020 0.0269 0.091 Uiso 1 1 calc R . . H32C H 0.7634 -0.1560 0.1070 0.091 Uiso 1 1 calc R . . C33 C 0.4472(3) 0.1242(2) 0.2509(3) 0.0374(9) Uani 1 1 d . . . H33A H 0.4134 0.0615 0.2234 0.045 Uiso 1 1 calc R . . H33B H 0.4658 0.1221 0.3114 0.045 Uiso 1 1 calc R . . C34 C 0.3697(3) 0.1803(3) 0.2467(3) 0.0478(10) Uani 1 1 d . . . H34A H 0.4018 0.2434 0.2739 0.057 Uiso 1 1 calc R . . H34B H 0.3475 0.1810 0.1866 0.057 Uiso 1 1 calc R . . C35 C 0.2783(3) 0.1421(3) 0.2907(4) 0.0619(14) Uani 1 1 d . . . H35A H 0.2507 0.0770 0.2682 0.074 Uiso 1 1 calc R . . H35B H 0.2986 0.1484 0.3523 0.074 Uiso 1 1 calc R . . C36 C 0.1076(3) 0.1462(3) 0.2912(3) 0.0695(15) Uani 1 1 d . . . H36A H 0.0603 0.1830 0.2794 0.104 Uiso 1 1 calc R . . H36B H 0.1077 0.1370 0.3506 0.104 Uiso 1 1 calc R . . H36C H 0.0858 0.0875 0.2541 0.104 Uiso 1 1 calc R . . C37 C 0.0792(2) 0.8004(2) 0.3402(2) 0.0285(7) Uani 1 1 d . . . C38 C 0.0450(3) 0.8754(2) 0.3756(2) 0.0353(8) Uani 1 1 d . . . H38A H 0.0669 0.9309 0.3549 0.042 Uiso 1 1 calc R . . C39 C -0.0191(3) 0.8715(3) 0.4393(2) 0.0408(9) Uani 1 1 d . . . H39A H -0.0401 0.9239 0.4610 0.049 Uiso 1 1 calc R . . C40 C -0.0529(3) 0.7923(3) 0.4715(2) 0.0432(9) Uani 1 1 d . . . H40A H -0.0981 0.7891 0.5142 0.052 Uiso 1 1 calc R . . C41 C -0.0194(3) 0.7178(3) 0.4399(2) 0.0407(9) Uani 1 1 d . . . H41A H -0.0408 0.6630 0.4618 0.049 Uiso 1 1 calc R . . C42 C 0.0450(3) 0.7226(2) 0.3767(2) 0.0337(8) Uani 1 1 d . . . H42A H 0.0673 0.6703 0.3569 0.040 Uiso 1 1 calc R . . C43 C 0.1327(3) 0.7007(2) 0.2112(2) 0.0296(7) Uani 1 1 d . . . C44 C 0.0620(3) 0.6699(2) 0.1391(2) 0.0328(8) Uani 1 1 d . . . H44A H 0.0309 0.7119 0.1167 0.039 Uiso 1 1 calc R . . C45 C 0.0353(3) 0.5807(2) 0.0990(2) 0.0401(9) Uani 1 1 d . . . H45A H -0.0141 0.5629 0.0508 0.048 Uiso 1 1 calc R . . C46 C 0.0796(3) 0.5176(2) 0.1282(3) 0.0434(10) Uani 1 1 d . . . H46A H 0.0611 0.4565 0.1008 0.052 Uiso 1 1 calc R . . C47 C 0.1512(3) 0.5451(2) 0.1979(3) 0.0432(10) Uani 1 1 d . . . H47A H 0.1836 0.5029 0.2183 0.052 Uiso 1 1 calc R . . C48 C 0.1766(3) 0.6344(2) 0.2387(2) 0.0370(8) Uani 1 1 d . . . H48A H 0.2255 0.6513 0.2872 0.044 Uiso 1 1 calc R . . C49 C 0.2743(3) 0.8438(2) 0.3054(2) 0.0317(8) Uani 1 1 d . . . C50 C 0.3554(3) 0.8155(3) 0.2713(2) 0.0404(9) Uani 1 1 d . . . H50A H 0.3411 0.7667 0.2253 0.048 Uiso 1 1 calc R . . C51 C 0.4563(3) 0.8564(3) 0.3026(3) 0.0501(11) Uani 1 1 d . . . H51A H 0.5092 0.8348 0.2781 0.060 Uiso 1 1 calc R . . C52 C 0.4806(3) 0.9277(3) 0.3686(3) 0.0520(12) Uani 1 1 d . . . H52A H 0.5498 0.9557 0.3895 0.062 Uiso 1 1 calc R . . C53 C 0.4031(3) 0.9578(3) 0.4035(3) 0.0485(11) Uani 1 1 d . . . H53A H 0.4186 1.0071 0.4490 0.058 Uiso 1 1 calc R . . C54 C 0.3017(3) 0.9163(2) 0.3726(2) 0.0379(9) Uani 1 1 d . . . H54A H 0.2494 0.9380 0.3981 0.046 Uiso 1 1 calc R . . C55 C 0.1324(3) 0.8711(2) 0.1972(2) 0.0314(8) Uani 1 1 d . . . C56 C 0.2084(3) 0.9104(2) 0.1495(2) 0.0345(8) Uani 1 1 d . . . H56A H 0.2732 0.8979 0.1567 0.041 Uiso 1 1 calc R . . C57 C 0.1934(3) 0.9670(2) 0.0920(2) 0.0389(9) Uani 1 1 d . . . H57A H 0.2474 0.9921 0.0610 0.047 Uiso 1 1 calc R . . C58 C 0.1003(3) 0.9866(2) 0.0802(2) 0.0430(10) Uani 1 1 d . . . H58A H 0.0898 1.0265 0.0422 0.052 Uiso 1 1 calc R . . C59 C 0.0222(3) 0.9473(2) 0.1245(2) 0.0390(9) Uani 1 1 d . . . H59A H -0.0428 0.9593 0.1161 0.047 Uiso 1 1 calc R . . C60 C 0.0384(3) 0.8905(2) 0.1810(2) 0.0350(8) Uani 1 1 d . . . H60A H -0.0168 0.8637 0.2100 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 Fe1 0.0250(2) 0.0247(2) 0.0237(3) 0.00735(18) 0.00269(19) 0.00388(18) Cl1 0.0296(4) 0.0324(4) 0.0403(5) 0.0119(4) 0.0054(4) 0.0090(3) P1 0.0266(4) 0.0238(4) 0.0256(5) 0.0053(3) 0.0036(3) 0.0045(3) P2 0.0303(5) 0.0292(4) 0.0247(5) 0.0089(4) 0.0045(4) 0.0051(4) P3 0.0283(4) 0.0280(4) 0.0250(5) 0.0067(3) 0.0014(4) 0.0037(3) P4 0.0267(4) 0.0274(4) 0.0300(5) 0.0078(4) 0.0008(4) 0.0021(3) O1 0.0303(14) 0.0482(16) 0.061(2) -0.0111(14) -0.0087(13) 0.0084(12) O2 0.0548(19) 0.0458(17) 0.104(3) 0.0303(17) -0.0049(18) 0.0146(14) O3 0.0449(17) 0.0309(14) 0.094(3) 0.0099(15) -0.0279(16) 0.0070(12) O5 0.0324(14) 0.0364(14) 0.065(2) -0.0111(13) 0.0088(13) 0.0085(11) O7 0.0515(16) 0.0351(14) 0.0463(17) 0.0110(12) 0.0154(13) 0.0112(12) O8 0.048(2) 0.0453(19) 0.205(5) 0.018(2) 0.043(2) 0.0128(15) B1 0.033(2) 0.0271(19) 0.026(2) 0.0055(16) -0.0036(16) 0.0044(16) C1 0.0347(19) 0.0303(18) 0.0259(19) 0.0028(14) 0.0058(14) 0.0075(14) C2 0.0374(19) 0.0356(19) 0.0231(19) 0.0039(14) 0.0045(15) 0.0059(15) C3 0.039(2) 0.037(2) 0.0243(19) 0.0040(15) -0.0040(15) 0.0022(15) C4 0.0307(18) 0.0332(18) 0.033(2) 0.0080(15) -0.0063(15) 0.0026(14) C5 0.0280(17) 0.0271(17) 0.0279(19) 0.0042(14) 0.0034(14) 0.0062(13) C6 0.0312(18) 0.0278(17) 0.0263(19) 0.0006(14) 0.0031(14) 0.0043(14) C7 0.0323(19) 0.0314(18) 0.038(2) 0.0050(15) -0.0019(16) 0.0046(15) C8 0.037(3) 0.072(3) 0.110(5) -0.010(3) -0.011(3) 0.020(2) C9 0.0302(18) 0.0287(17) 0.031(2) 0.0104(14) 0.0022(15) 0.0016(14) C10 0.0333(19) 0.0300(19) 0.052(3) 0.0161(17) 0.0088(17) 0.0077(15) C11 0.040(2) 0.037(2) 0.080(3) 0.030(2) 0.010(2) 0.0099(17) C12 0.072(4) 0.090(4) 0.130(6) 0.045(4) -0.010(4) 0.025(3) C13 0.044(2) 0.0305(18) 0.033(2) 0.0114(15) 0.0003(16) 0.0056(16) C14 0.0324(19) 0.035(2) 0.043(2) 0.0083(17) -0.0032(16) 0.0048(15) C15 0.037(2) 0.036(2) 0.055(3) 0.0109(18) -0.0136(18) 0.0060(16) C16 0.069(4) 0.038(3) 0.173(7) 0.021(3) -0.042(4) 0.008(2) C17 0.038(2) 0.047(2) 0.035(2) 0.0110(17) 0.0126(17) 0.0083(17) C18 0.080(3) 0.085(4) 0.050(3) 0.034(3) 0.034(3) 0.046(3) C19 0.082(5) 0.075(8) 0.061(4) 0.037(5) 0.042(4) 0.039(5) O4 0.069(3) 0.071(3) 0.075(3) 0.008(2) 0.033(2) 0.036(2) C20 0.130(8) 0.138(8) 0.110(8) 0.012(6) 0.059(6) 0.091(7) C18A 0.080(3) 0.085(4) 0.050(3) 0.034(3) 0.034(3) 0.046(3) C19A 0.082(5) 0.075(8) 0.061(4) 0.037(5) 0.042(4) 0.039(5) O4A 0.069(3) 0.071(3) 0.075(3) 0.008(2) 0.033(2) 0.036(2) C20A 0.130(8) 0.138(8) 0.110(8) 0.012(6) 0.059(6) 0.091(7) C21 0.0373(19) 0.0324(18) 0.0261(19) 0.0076(14) 0.0057(15) 0.0065(15) C22 0.038(2) 0.0271(17) 0.035(2) 0.0013(15) 0.0013(16) 0.0093(15) C23 0.044(2) 0.0272(18) 0.044(2) -0.0050(16) 0.0021(18) 0.0123(16) C24 0.041(2) 0.054(3) 0.099(4) -0.007(3) 0.018(2) 0.012(2) C25 0.039(2) 0.0368(19) 0.030(2) 0.0126(15) 0.0047(16) 0.0124(16) C26 0.051(2) 0.052(2) 0.036(2) 0.0194(18) 0.0145(18) 0.0197(19) C27 0.107(4) 0.096(4) 0.043(3) 0.032(3) 0.024(3) 0.062(4) O6 0.063(3) 0.054(3) 0.061(3) 0.023(2) -0.004(2) 0.013(2) C28 0.116(5) 0.136(6) 0.107(5) 0.056(5) 0.016(4) 0.077(5) C27A 0.107(4) 0.096(4) 0.043(3) 0.032(3) 0.024(3) 0.062(4) O6A 0.063(3) 0.054(3) 0.061(3) 0.023(2) -0.004(2) 0.013(2) C28A 0.116(5) 0.136(6) 0.107(5) 0.056(5) 0.016(4) 0.077(5) C29 0.0310(18) 0.0270(17) 0.034(2) 0.0053(14) -0.0028(15) 0.0044(14) C30 0.0344(19) 0.0274(17) 0.034(2) 0.0054(15) -0.0047(15) 0.0024(14) C31 0.036(2) 0.0286(18) 0.039(2) 0.0099(15) -0.0017(16) 0.0016(15) C32 0.062(3) 0.050(3) 0.078(4) 0.016(2) 0.024(3) 0.023(2) C33 0.0325(19) 0.0308(19) 0.045(2) 0.0076(16) 0.0085(17) -0.0006(15) C34 0.033(2) 0.040(2) 0.070(3) 0.013(2) 0.012(2) 0.0035(17) C35 0.043(2) 0.039(2) 0.104(4) 0.010(2) 0.028(3) 0.0062(19) C36 0.048(3) 0.063(3) 0.083(4) -0.016(3) 0.007(3) 0.001(2) C37 0.0268(17) 0.0276(17) 0.0260(18) 0.0000(14) -0.0056(14) 0.0018(13) C38 0.037(2) 0.0308(18) 0.036(2) 0.0047(15) -0.0033(16) 0.0069(15) C39 0.039(2) 0.045(2) 0.039(2) -0.0023(18) -0.0027(17) 0.0181(17) C40 0.039(2) 0.057(3) 0.034(2) 0.0052(18) 0.0071(17) 0.0117(18) C41 0.040(2) 0.039(2) 0.039(2) 0.0113(17) 0.0020(17) -0.0001(16) C42 0.0348(19) 0.0307(18) 0.033(2) 0.0039(15) 0.0007(15) 0.0044(15) C43 0.0355(19) 0.0257(17) 0.0286(19) 0.0085(14) 0.0083(15) 0.0057(14) C44 0.0366(19) 0.0288(18) 0.032(2) 0.0052(15) 0.0089(15) 0.0045(14) C45 0.041(2) 0.037(2) 0.036(2) -0.0024(16) 0.0110(17) 0.0013(16) C46 0.054(2) 0.030(2) 0.045(3) 0.0035(17) 0.022(2) 0.0066(17) C47 0.061(3) 0.034(2) 0.047(3) 0.0195(18) 0.029(2) 0.0213(18) C48 0.044(2) 0.038(2) 0.033(2) 0.0109(16) 0.0104(17) 0.0138(16) C49 0.0314(18) 0.0329(18) 0.029(2) 0.0151(15) -0.0028(15) 0.0004(14) C50 0.034(2) 0.052(2) 0.036(2) 0.0141(18) 0.0029(16) 0.0066(17) C51 0.032(2) 0.071(3) 0.050(3) 0.031(2) 0.0048(19) 0.0048(19) C52 0.030(2) 0.064(3) 0.055(3) 0.034(2) -0.0061(19) -0.0109(19) C53 0.045(2) 0.043(2) 0.047(3) 0.0158(19) -0.013(2) -0.0088(18) C54 0.035(2) 0.035(2) 0.039(2) 0.0142(16) -0.0027(17) -0.0003(15) C55 0.039(2) 0.0220(16) 0.0277(19) 0.0004(14) -0.0059(15) 0.0022(14) C56 0.041(2) 0.0268(17) 0.032(2) 0.0055(15) -0.0028(16) 0.0026(15) C57 0.052(2) 0.0320(19) 0.028(2) 0.0087(15) 0.0001(17) -0.0002(17) C58 0.062(3) 0.0306(19) 0.032(2) 0.0042(16) -0.0116(19) 0.0096(18) C59 0.051(2) 0.0339(19) 0.031(2) 0.0029(16) -0.0071(17) 0.0129(17) C60 0.039(2) 0.0325(19) 0.030(2) 0.0047(15) -0.0043(16) 0.0053(15) _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 Fe1 P4 2.2792(9) . ? Fe1 P1 2.2803(9) . ? Fe1 P2 2.3130(10) . ? Fe1 P3 2.3175(10) . ? Fe1 Cl1 2.3505(9) . ? P1 C1 1.829(3) . ? P1 C9 1.831(3) . ? P1 C5 1.839(3) . ? P2 C17 1.821(4) . ? P2 C13 1.828(3) . ? P2 C2 1.845(3) . ? P3 C21 1.823(3) . ? P3 C25 1.827(3) . ? P3 C3 1.841(3) . ? P4 C33 1.828(4) . ? P4 C4 1.833(3) . ? P4 C29 1.836(3) . ? O1 C7 1.419(4) . ? O1 C8 1.425(5) . ? O2 C11 1.418(5) . ? O2 C12 1.420(6) . ? O3 C15 1.408(4) . ? O3 C16 1.424(5) . ? O5 C24 1.418(4) . ? O5 C23 1.421(4) . ? O7 C31 1.413(4) . ? O7 C32 1.418(4) . ? O8 C36 1.357(5) . ? O8 C35 1.415(5) . ? B1 C37 1.643(5) . ? B1 C43 1.644(5) . ? B1 C49 1.648(5) . ? B1 C55 1.656(5) . ? C1 C2 1.523(4) . ? C3 C4 1.520(5) . ? C5 C6 1.538(4) . ? C6 C7 1.514(4) . ? C9 C10 1.523(5) . ? C10 C11 1.522(5) . ? C13 C14 1.523(5) . ? C14 C15 1.519(5) . ? C17 C18 1.511(5) . ? C18 C19 1.494(9) . ? C19 O4 1.393(11) . ? O4 C20 1.425(7) . ? C19A O4A 1.402(19) . ? O4A C20A 1.417(14) . ? C21 C22 1.534(4) . ? C22 C23 1.512(5) . ? C25 C26 1.523(5) . ? C26 C27 1.478(5) . ? C27 O6 1.329(6) . ? O6 C28 1.468(6) . ? C29 C30 1.536(4) . ? C30 C31 1.507(5) . ? C33 C34 1.520(5) . ? C34 C35 1.509(5) . ? C37 C42 1.401(5) . ? C37 C38 1.412(4) . ? C38 C39 1.386(5) . ? C39 C40 1.382(5) . ? C40 C41 1.381(5) . ? C41 C42 1.384(5) . ? C43 C44 1.399(5) . ? C43 C48 1.406(5) . ? C44 C45 1.387(5) . ? C45 C46 1.378(5) . ? C46 C47 1.375(5) . ? C47 C48 1.393(5) . ? C49 C50 1.399(5) . ? C49 C54 1.400(5) . ? C50 C51 1.389(5) . ? C51 C52 1.375(6) . ? C52 C53 1.374(6) . ? C53 C54 1.395(5) . ? C55 C60 1.397(5) . ? C55 C56 1.399(5) . ? C56 C57 1.391(5) . ? C57 C58 1.378(5) . ? C58 C59 1.383(5) . ? C59 C60 1.386(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P4 Fe1 P1 171.25(4) . . ? P4 Fe1 P2 95.81(4) . . ? P1 Fe1 P2 82.64(3) . . ? P4 Fe1 P3 82.86(3) . . ? P1 Fe1 P3 96.16(3) . . ? P2 Fe1 P3 163.47(4) . . ? P4 Fe1 Cl1 92.69(3) . . ? P1 Fe1 Cl1 96.06(3) . . ? P2 Fe1 Cl1 98.93(4) . . ? P3 Fe1 Cl1 97.58(3) . . ? C1 P1 C9 105.06(16) . . ? C1 P1 C5 103.65(15) . . ? C9 P1 C5 103.08(15) . . ? C1 P1 Fe1 106.61(11) . . ? C9 P1 Fe1 123.78(11) . . ? C5 P1 Fe1 112.78(10) . . ? C17 P2 C13 106.41(17) . . ? C17 P2 C2 103.21(17) . . ? C13 P2 C2 104.62(16) . . ? C17 P2 Fe1 112.31(12) . . ? C13 P2 Fe1 118.74(13) . . ? C2 P2 Fe1 110.19(11) . . ? C21 P3 C25 105.36(16) . . ? C21 P3 C3 104.62(16) . . ? C25 P3 C3 102.12(16) . . ? C21 P3 Fe1 120.67(12) . . ? C25 P3 Fe1 112.88(12) . . ? C3 P3 Fe1 109.35(12) . . ? C33 P4 C4 104.76(17) . . ? C33 P4 C29 102.26(16) . . ? C4 P4 C29 102.70(16) . . ? C33 P4 Fe1 125.55(12) . . ? C4 P4 Fe1 106.28(11) . . ? C29 P4 Fe1 112.90(11) . . ? C7 O1 C8 110.7(3) . . ? C11 O2 C12 111.6(4) . . ? C15 O3 C16 111.6(3) . . ? C24 O5 C23 112.1(3) . . ? C31 O7 C32 111.4(3) . . ? C36 O8 C35 115.0(4) . . ? C37 B1 C43 107.7(3) . . ? C37 B1 C49 109.8(3) . . ? C43 B1 C49 112.4(3) . . ? C37 B1 C55 112.3(3) . . ? C43 B1 C55 108.1(3) . . ? C49 B1 C55 106.6(3) . . ? C2 C1 P1 107.7(2) . . ? C1 C2 P2 108.3(2) . . ? C4 C3 P3 108.2(2) . . ? C3 C4 P4 106.7(2) . . ? C6 C5 P1 117.7(2) . . ? C7 C6 C5 109.9(3) . . ? O1 C7 C6 109.0(3) . . ? C10 C9 P1 114.5(2) . . ? C11 C10 C9 111.9(3) . . ? O2 C11 C10 113.0(3) . . ? C14 C13 P2 113.2(3) . . ? C15 C14 C13 113.6(3) . . ? O3 C15 C14 109.0(3) . . ? C18 C17 P2 117.2(3) . . ? C19 C18 C17 113.5(6) . . ? O4 C19 C18 105.7(7) . . ? C19 O4 C20 111.1(7) . . ? C19A O4A C20A 112.8(16) . . ? C22 C21 P3 113.6(2) . . ? C23 C22 C21 111.4(3) . . ? O5 C23 C22 108.7(3) . . ? C26 C25 P3 115.8(2) . . ? C27 C26 C25 115.0(3) . . ? O6 C27 C26 115.2(4) . . ? C27 O6 C28 111.0(5) . . ? C30 C29 P4 117.5(2) . . ? C31 C30 C29 111.9(3) . . ? O7 C31 C30 109.0(3) . . ? C34 C33 P4 117.1(3) . . ? C35 C34 C33 110.8(3) . . ? O8 C35 C34 109.2(4) . . ? C42 C37 C38 114.2(3) . . ? C42 C37 B1 122.4(3) . . ? C38 C37 B1 123.4(3) . . ? C39 C38 C37 122.8(3) . . ? C40 C39 C38 120.7(4) . . ? C39 C40 C41 118.4(4) . . ? C40 C41 C42 120.5(4) . . ? C41 C42 C37 123.4(3) . . ? C44 C43 C48 114.7(3) . . ? C44 C43 B1 122.3(3) . . ? C48 C43 B1 122.7(3) . . ? C45 C44 C43 122.8(3) . . ? C46 C45 C44 120.8(4) . . ? C47 C46 C45 118.6(3) . . ? C46 C47 C48 120.3(4) . . ? C47 C48 C43 122.8(4) . . ? C50 C49 C54 115.5(3) . . ? C50 C49 B1 123.4(3) . . ? C54 C49 B1 120.8(3) . . ? C51 C50 C49 122.0(4) . . ? C52 C51 C50 121.0(4) . . ? C53 C52 C51 118.7(4) . . ? C52 C53 C54 120.3(4) . . ? C53 C54 C49 122.4(4) . . ? C60 C55 C56 114.9(3) . . ? C60 C55 B1 124.2(3) . . ? C56 C55 B1 120.9(3) . . ? C57 C56 C55 123.1(3) . . ? C58 C57 C56 119.9(4) . . ? C57 C58 C59 118.9(3) . . ? C58 C59 C60 120.3(4) . . ? C59 C60 C55 122.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P4 Fe1 P1 C1 -107.8(3) . . . . ? P2 Fe1 P1 C1 -27.51(12) . . . . ? P3 Fe1 P1 C1 169.09(11) . . . . ? Cl1 Fe1 P1 C1 70.76(12) . . . . ? P4 Fe1 P1 C9 130.4(3) . . . . ? P2 Fe1 P1 C9 -149.23(14) . . . . ? P3 Fe1 P1 C9 47.37(14) . . . . ? Cl1 Fe1 P1 C9 -50.96(14) . . . . ? P4 Fe1 P1 C5 5.3(3) . . . . ? P2 Fe1 P1 C5 85.59(12) . . . . ? P3 Fe1 P1 C5 -77.81(12) . . . . ? Cl1 Fe1 P1 C5 -176.14(12) . . . . ? P4 Fe1 P2 C17 -70.62(14) . . . . ? P1 Fe1 P2 C17 118.04(14) . . . . ? P3 Fe1 P2 C17 -155.09(17) . . . . ? Cl1 Fe1 P2 C17 23.03(14) . . . . ? P4 Fe1 P2 C13 54.36(14) . . . . ? P1 Fe1 P2 C13 -116.97(14) . . . . ? P3 Fe1 P2 C13 -30.1(2) . . . . ? Cl1 Fe1 P2 C13 148.01(14) . . . . ? P4 Fe1 P2 C2 174.92(12) . . . . ? P1 Fe1 P2 C2 3.59(12) . . . . ? P3 Fe1 P2 C2 90.45(18) . . . . ? Cl1 Fe1 P2 C2 -91.43(12) . . . . ? P4 Fe1 P3 C21 -119.50(13) . . . . ? P1 Fe1 P3 C21 51.75(13) . . . . ? P2 Fe1 P3 C21 -33.14(19) . . . . ? Cl1 Fe1 P3 C21 148.73(13) . . . . ? P4 Fe1 P3 C25 114.73(13) . . . . ? P1 Fe1 P3 C25 -74.02(13) . . . . ? P2 Fe1 P3 C25 -158.92(17) . . . . ? Cl1 Fe1 P3 C25 22.95(13) . . . . ? P4 Fe1 P3 C3 1.79(13) . . . . ? P1 Fe1 P3 C3 173.04(13) . . . . ? P2 Fe1 P3 C3 88.14(18) . . . . ? Cl1 Fe1 P3 C3 -89.99(13) . . . . ? P1 Fe1 P4 C33 126.6(3) . . . . ? P2 Fe1 P4 C33 47.25(15) . . . . ? P3 Fe1 P4 C33 -149.32(15) . . . . ? Cl1 Fe1 P4 C33 -52.01(15) . . . . ? P1 Fe1 P4 C4 -111.1(3) . . . . ? P2 Fe1 P4 C4 169.59(12) . . . . ? P3 Fe1 P4 C4 -26.99(12) . . . . ? Cl1 Fe1 P4 C4 70.32(12) . . . . ? P1 Fe1 P4 C29 0.8(3) . . . . ? P2 Fe1 P4 C29 -78.57(13) . . . . ? P3 Fe1 P4 C29 84.86(13) . . . . ? Cl1 Fe1 P4 C29 -177.83(13) . . . . ? C9 P1 C1 C2 -174.4(2) . . . . ? C5 P1 C1 C2 -66.6(3) . . . . ? Fe1 P1 C1 C2 52.6(2) . . . . ? P1 C1 C2 P2 -49.4(3) . . . . ? C17 P2 C2 C1 -93.6(3) . . . . ? C13 P2 C2 C1 155.3(2) . . . . ? Fe1 P2 C2 C1 26.6(3) . . . . ? C21 P3 C3 C4 160.4(2) . . . . ? C25 P3 C3 C4 -90.0(3) . . . . ? Fe1 P3 C3 C4 29.8(3) . . . . ? P3 C3 C4 P4 -52.2(3) . . . . ? C33 P4 C4 C3 -171.7(2) . . . . ? C29 P4 C4 C3 -65.1(3) . . . . ? Fe1 P4 C4 C3 53.6(2) . . . . ? C1 P1 C5 C6 -43.9(3) . . . . ? C9 P1 C5 C6 65.4(3) . . . . ? Fe1 P1 C5 C6 -158.8(2) . . . . ? P1 C5 C6 C7 179.8(2) . . . . ? C8 O1 C7 C6 -171.3(4) . . . . ? C5 C6 C7 O1 169.5(3) . . . . ? C1 P1 C9 C10 -56.0(3) . . . . ? C5 P1 C9 C10 -164.3(3) . . . . ? Fe1 P1 C9 C10 66.4(3) . . . . ? P1 C9 C10 C11 -171.3(3) . . . . ? C12 O2 C11 C10 -71.9(5) . . . . ? C9 C10 C11 O2 179.2(3) . . . . ? C17 P2 C13 C14 177.6(3) . . . . ? C2 P2 C13 C14 -73.6(3) . . . . ? Fe1 P2 C13 C14 49.8(3) . . . . ? P2 C13 C14 C15 -172.4(2) . . . . ? C16 O3 C15 C14 -179.2(4) . . . . ? C13 C14 C15 O3 65.2(4) . . . . ? C13 P2 C17 C18 49.9(4) . . . . ? C2 P2 C17 C18 -59.9(4) . . . . ? Fe1 P2 C17 C18 -178.6(3) . . . . ? P2 C17 C18 C19 -179.7(5) . . . . ? C17 C18 C19 O4 -57.6(9) . . . . ? C18 C19 O4 C20 -170.5(7) . . . . ? C25 P3 C21 C22 178.9(2) . . . . ? C3 P3 C21 C22 -73.8(3) . . . . ? Fe1 P3 C21 C22 49.7(3) . . . . ? P3 C21 C22 C23 -174.6(2) . . . . ? C24 O5 C23 C22 -177.7(4) . . . . ? C21 C22 C23 O5 63.1(4) . . . . ? C21 P3 C25 C26 46.8(3) . . . . ? C3 P3 C25 C26 -62.2(3) . . . . ? Fe1 P3 C25 C26 -179.5(2) . . . . ? P3 C25 C26 C27 162.3(3) . . . . ? C25 C26 C27 O6 53.9(6) . . . . ? C26 C27 O6 C28 -173.7(5) . . . . ? C33 P4 C29 C30 60.7(3) . . . . ? C4 P4 C29 C30 -47.8(3) . . . . ? Fe1 P4 C29 C30 -161.8(2) . . . . ? P4 C29 C30 C31 172.5(3) . . . . ? C32 O7 C31 C30 -176.6(3) . . . . ? C29 C30 C31 O7 -71.8(4) . . . . ? C4 P4 C33 C34 -56.6(3) . . . . ? C29 P4 C33 C34 -163.4(3) . . . . ? Fe1 P4 C33 C34 66.4(3) . . . . ? P4 C33 C34 C35 -178.8(3) . . . . ? C36 O8 C35 C34 161.7(4) . . . . ? C33 C34 C35 O8 -173.1(4) . . . . ? C43 B1 C37 C42 28.2(4) . . . . ? C49 B1 C37 C42 -94.5(3) . . . . ? C55 B1 C37 C42 147.1(3) . . . . ? C43 B1 C37 C38 -153.1(3) . . . . ? C49 B1 C37 C38 84.2(4) . . . . ? C55 B1 C37 C38 -34.3(4) . . . . ? C42 C37 C38 C39 -1.7(5) . . . . ? B1 C37 C38 C39 179.6(3) . . . . ? C37 C38 C39 C40 0.0(5) . . . . ? C38 C39 C40 C41 1.4(5) . . . . ? C39 C40 C41 C42 -1.0(5) . . . . ? C40 C41 C42 C37 -0.8(5) . . . . ? C38 C37 C42 C41 2.1(5) . . . . ? B1 C37 C42 C41 -179.2(3) . . . . ? C37 B1 C43 C44 92.5(4) . . . . ? C49 B1 C43 C44 -146.5(3) . . . . ? C55 B1 C43 C44 -29.1(4) . . . . ? C37 B1 C43 C48 -81.7(4) . . . . ? C49 B1 C43 C48 39.4(5) . . . . ? C55 B1 C43 C48 156.8(3) . . . . ? C48 C43 C44 C45 1.4(5) . . . . ? B1 C43 C44 C45 -173.2(3) . . . . ? C43 C44 C45 C46 -1.1(6) . . . . ? C44 C45 C46 C47 -0.3(6) . . . . ? C45 C46 C47 C48 1.3(6) . . . . ? C46 C47 C48 C43 -1.0(6) . . . . ? C44 C43 C48 C47 -0.4(5) . . . . ? B1 C43 C48 C47 174.2(3) . . . . ? C37 B1 C49 C50 146.3(3) . . . . ? C43 B1 C49 C50 26.5(5) . . . . ? C55 B1 C49 C50 -91.8(4) . . . . ? C37 B1 C49 C54 -40.5(4) . . . . ? C43 B1 C49 C54 -160.3(3) . . . . ? C55 B1 C49 C54 81.4(4) . . . . ? C54 C49 C50 C51 0.4(5) . . . . ? B1 C49 C50 C51 173.9(3) . . . . ? C49 C50 C51 C52 -0.7(6) . . . . ? C50 C51 C52 C53 0.4(6) . . . . ? C51 C52 C53 C54 0.1(6) . . . . ? C52 C53 C54 C49 -0.4(6) . . . . ? C50 C49 C54 C53 0.1(5) . . . . ? B1 C49 C54 C53 -173.6(3) . . . . ? C37 B1 C55 C60 -27.1(4) . . . . ? C43 B1 C55 C60 91.6(4) . . . . ? C49 B1 C55 C60 -147.4(3) . . . . ? C37 B1 C55 C56 155.4(3) . . . . ? C43 B1 C55 C56 -85.9(4) . . . . ? C49 B1 C55 C56 35.1(4) . . . . ? C60 C55 C56 C57 1.9(5) . . . . ? B1 C55 C56 C57 179.7(3) . . . . ? C55 C56 C57 C58 0.1(5) . . . . ? C56 C57 C58 C59 -1.7(5) . . . . ? C57 C58 C59 C60 1.2(5) . . . . ? C58 C59 C60 C55 0.9(5) . . . . ? C56 C55 C60 C59 -2.4(5) . . . . ? B1 C55 C60 C59 180.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.750 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.069