# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name P.G.Edwards T.Albers P.Newman J.Baker S.Coles _publ_contact_author_name 'Edwards, P. G.' _publ_contact_author_email EDWARDSPG@CARDIFF.AC.UK data_s92 _database_code_depnum_ccdc_archive 'CCDC 804159' #TrackingRef '- Fig1_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H29 F2 Fe P3, C24 H20 B, 4(C2 H3 N)' _chemical_formula_sum 'C73 H62 B F2 Fe N4 P3' _chemical_formula_weight 1192.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.6204(3) _cell_length_b 14.7050(3) _cell_length_c 27.0880(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.6900(10) _cell_angle_gamma 90.00 _cell_volume 6070.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6241 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 26.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 0.381 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9812 _exptl_absorpt_correction_T_max 0.9943 _exptl_absorpt_process_details Denzo/Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37113 _diffrn_reflns_av_R_equivalents 0.1505 _diffrn_reflns_av_sigmaI/netI 0.1901 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 26.01 _reflns_number_total 11801 _reflns_number_gt 6241 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11801 _refine_ls_number_parameters 791 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1707 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.1946 _refine_ls_wR_factor_gt 0.1615 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.969 _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 0.19179(4) 0.35860(5) 0.02557(2) 0.0205(2) Uani 1 1 d . . . P1 P 0.26551(8) 0.35141(8) -0.03275(5) 0.0198(3) Uani 1 1 d . A . P2 P 0.27515(8) 0.47126(8) 0.05566(4) 0.0205(3) Uani 1 1 d . . . P3 P 0.29076(8) 0.27301(8) 0.06965(5) 0.0199(3) Uani 1 1 d . A . F1 F 0.1637(3) 0.4761(3) -0.1115(2) 0.0559(14) Uani 0.67 1 d P . . F2 F 0.1834(3) 0.6315(3) -0.00267(17) 0.0412(12) Uani 0.67 1 d P . . F3 F 0.2525(4) 0.2648(4) 0.1747(2) 0.0746(17) Uani 0.67 1 d P . . B1 B 0.7271(4) 0.1244(4) 0.1735(2) 0.0241(13) Uani 1 1 d . . . C1 C 0.3297(3) 0.4552(3) -0.03298(17) 0.0195(11) Uani 1 1 d . . . C2 C 0.3737(3) 0.4794(3) -0.07046(17) 0.0222(11) Uani 1 1 d . A . H2 H 0.3703 0.4416 -0.0993 0.027 Uiso 1 1 calc R . . C3 C 0.4225(3) 0.5587(3) -0.06546(18) 0.0255(12) Uani 1 1 d . . . H3 H 0.4522 0.5756 -0.0911 0.031 Uiso 1 1 calc R A . C4 C 0.4284(3) 0.6133(3) -0.02387(18) 0.0255(12) Uani 1 1 d . A . H4 H 0.4619 0.6676 -0.0211 0.031 Uiso 1 1 calc R . . C5 C 0.3856(3) 0.5900(3) 0.01470(18) 0.0224(11) Uani 1 1 d . . . H5 H 0.3906 0.6272 0.0439 0.027 Uiso 1 1 calc R A . C6 C 0.3356(3) 0.5110(3) 0.00903(17) 0.0207(11) Uani 1 1 d . A . C7 C 0.3614(3) 0.4336(3) 0.10895(17) 0.0210(11) Uani 1 1 d . A . C8 C 0.4207(3) 0.4908(3) 0.14035(17) 0.0236(11) Uani 1 1 d . . . H8 H 0.4166 0.5548 0.1360 0.028 Uiso 1 1 calc R . . C9 C 0.4855(3) 0.4534(3) 0.17789(17) 0.0259(12) Uani 1 1 d . . . H9 H 0.5263 0.4921 0.1993 0.031 Uiso 1 1 calc R . . C10 C 0.4916(3) 0.3610(4) 0.18448(18) 0.0279(12) Uani 1 1 d . . . H10 H 0.5360 0.3365 0.2108 0.034 Uiso 1 1 calc R . . C11 C 0.4344(3) 0.3031(3) 0.15370(17) 0.0236(11) Uani 1 1 d . A . H11 H 0.4393 0.2391 0.1583 0.028 Uiso 1 1 calc R . . C12 C 0.3686(3) 0.3403(3) 0.11533(17) 0.0215(11) Uani 1 1 d . . . C13 C 0.3615(3) 0.2258(3) 0.03010(17) 0.0203(11) Uani 1 1 d . . . C14 C 0.4271(3) 0.1617(3) 0.04655(18) 0.0229(11) Uani 1 1 d . A . H14 H 0.4349 0.1363 0.0795 0.027 Uiso 1 1 calc R . . C15 C 0.4807(3) 0.1352(3) 0.01487(19) 0.0273(12) Uani 1 1 d . . . H15 H 0.5258 0.0918 0.0261 0.033 Uiso 1 1 calc R A . C16 C 0.4687(3) 0.1718(3) -0.03318(18) 0.0268(12) Uani 1 1 d . A . H16 H 0.5049 0.1521 -0.0551 0.032 Uiso 1 1 calc R . . C17 C 0.4047(3) 0.2368(3) -0.04984(18) 0.0231(11) Uani 1 1 d . . . H17 H 0.3977 0.2629 -0.0826 0.028 Uiso 1 1 calc R A . C18 C 0.3508(3) 0.2631(3) -0.01761(18) 0.0207(11) Uani 1 1 d . A . C19 C 0.2095(3) 0.3282(3) -0.09765(18) 0.0229(11) Uani 1 1 d . . . C20 C 0.1681(3) 0.3949(4) -0.1293(2) 0.0347(13) Uani 1 1 d . A . H20 H 0.1721 0.4519 -0.1230 0.040 Uiso 0.33 1 d p . . C21 C 0.1163(4) 0.3766(4) -0.1765(2) 0.0426(15) Uani 1 1 d . . . H21 H 0.0879 0.4246 -0.1973 0.051 Uiso 1 1 calc R A . C22 C 0.1064(4) 0.2881(4) -0.1931(2) 0.0438(15) Uani 1 1 d . A . H22 H 0.0717 0.2746 -0.2257 0.053 Uiso 1 1 calc R . . C23 C 0.1472(4) 0.2188(4) -0.1620(2) 0.0473(16) Uani 1 1 d . . . H23 H 0.1411 0.1575 -0.1733 0.057 Uiso 1 1 calc R A . C24 C 0.1967(4) 0.2389(4) -0.1143(2) 0.0410(15) Uani 1 1 d . A . H24 H 0.2224 0.1908 -0.0926 0.049 Uiso 1 1 calc R . . C25 C 0.2288(3) 0.5718(3) 0.07856(18) 0.0234(11) Uani 1 1 d . . . C26 C 0.1898(3) 0.6397(3) 0.04600(19) 0.0282(12) Uani 1 1 d . . . H26 H 0.1872 0.6420 0.0131 0.030 Uiso 0.33 1 d p . . C27 C 0.1460(3) 0.7120(3) 0.0620(2) 0.0356(14) Uani 1 1 d . . . H27 H 0.1216 0.7589 0.0390 0.043 Uiso 1 1 calc R . . C28 C 0.1384(3) 0.7149(4) 0.1115(2) 0.0380(14) Uani 1 1 d . . . H28 H 0.1072 0.7635 0.1226 0.046 Uiso 1 1 calc R . . C29 C 0.1753(4) 0.6484(4) 0.1454(2) 0.0425(15) Uani 1 1 d . . . H29 H 0.1699 0.6510 0.1796 0.051 Uiso 1 1 calc R . . C30 C 0.2207(3) 0.5771(4) 0.1286(2) 0.0321(13) Uani 1 1 d . . . H30 H 0.2466 0.5312 0.1518 0.038 Uiso 1 1 calc R . . C31 C 0.2589(3) 0.1775(3) 0.10389(18) 0.0231(11) Uani 1 1 d . . . C32 C 0.2454(3) 0.1839(4) 0.15231(19) 0.0297(12) Uani 1 1 d . A . H32 H 0.2578 0.2348 0.1706 0.030 Uiso 0.33 1 d p . . C33 C 0.2093(3) 0.1155(4) 0.1756(2) 0.0358(13) Uani 1 1 d . . . H33 H 0.2010 0.1230 0.2090 0.043 Uiso 1 1 calc R A . C34 C 0.1854(3) 0.0360(4) 0.1495(2) 0.0376(14) Uani 1 1 d . A . H34 H 0.1605 -0.0123 0.1650 0.045 Uiso 1 1 calc R . . C35 C 0.1978(4) 0.0264(4) 0.1011(2) 0.0414(14) Uani 1 1 d . . . H35 H 0.1821 -0.0288 0.0832 0.050 Uiso 1 1 calc R A . C36 C 0.2331(3) 0.0969(4) 0.0783(2) 0.0386(14) Uani 1 1 d . A . H36 H 0.2398 0.0901 0.0445 0.046 Uiso 1 1 calc R . . C37 C 0.0888(5) 0.3856(6) 0.0613(2) 0.027(3) Uani 0.50 1 d PGU A 1 H37 H 0.0952 0.4097 0.0945 0.033 Uiso 0.50 1 calc PR A 1 C38 C 0.0773(5) 0.4368(4) 0.0159(3) 0.031(3) Uani 0.50 1 d PGU A 1 H38 H 0.0747 0.5012 0.0133 0.037 Uiso 0.50 1 calc PR A 1 C39 C 0.0704(6) 0.3748(6) -0.0250(2) 0.029(3) Uani 0.50 1 d PGU A 1 H39 H 0.0623 0.3905 -0.0597 0.035 Uiso 0.50 1 calc PR A 1 C40 C 0.0775(6) 0.2853(4) -0.0049(3) 0.026(3) Uani 0.50 1 d PGU A 1 H40 H 0.0752 0.2306 -0.0237 0.031 Uiso 0.50 1 calc PR A 1 C41 C 0.0889(6) 0.2919(5) 0.0485(3) 0.033(4) Uani 0.50 1 d PGU A 1 H41 H 0.0955 0.2424 0.0716 0.040 Uiso 0.50 1 calc PR A 1 C37' C 0.0817(3) 0.4176(4) 0.0421(2) 0.027(3) Uani 0.50 1 d PGU A 2 H37' H 0.0817 0.4721 0.0609 0.032 Uiso 0.50 1 calc PR A 2 C38' C 0.0717(3) 0.4111(4) -0.0112(2) 0.022(3) Uani 0.50 1 d PGU A 2 H38' H 0.0637 0.4606 -0.0343 0.026 Uiso 0.50 1 calc PR A 2 C39' C 0.0755(3) 0.3177(5) -0.02384(18) 0.025(3) Uani 0.50 1 d PGU A 2 H39' H 0.0706 0.2937 -0.0569 0.029 Uiso 0.50 1 calc PR A 2 C40' C 0.0880(2) 0.2664(3) 0.0216(2) 0.023(3) Uani 0.50 1 d PGU A 2 H40' H 0.0928 0.2021 0.0243 0.028 Uiso 0.50 1 calc PR A 2 C41' C 0.0918(2) 0.3282(4) 0.06236(18) 0.020(3) Uani 0.50 1 d PGU A 2 H41' H 0.0997 0.3124 0.0971 0.024 Uiso 0.50 1 calc PR A 2 C42 C 0.6289(2) 0.1032(3) 0.18440(14) 0.0238(11) Uani 1 1 d G . . C43 C 0.6060(2) 0.1364(3) 0.22794(13) 0.0293(12) Uani 1 1 d G . . H43 H 0.6483 0.1710 0.2510 0.035 Uiso 1 1 calc R . . C44 C 0.5242(3) 0.1218(3) 0.2396(2) 0.0318(13) Uani 1 1 d . . . H44 H 0.5113 0.1471 0.2694 0.038 Uiso 1 1 calc R . . C45 C 0.4616(3) 0.0694(3) 0.20677(19) 0.0290(12) Uani 1 1 d . . . H45 H 0.4057 0.0585 0.2140 0.035 Uiso 1 1 calc R . . C46 C 0.4824(3) 0.0340(3) 0.16405(19) 0.0312(13) Uani 1 1 d . . . H46 H 0.4405 -0.0017 0.1415 0.037 Uiso 1 1 calc R . . C47 C 0.5641(3) 0.0499(3) 0.15332(18) 0.0285(12) Uani 1 1 d . . . H47 H 0.5767 0.0236 0.1237 0.034 Uiso 1 1 calc R . . C48 C 0.7546(3) 0.2275(3) 0.19314(17) 0.0215(11) Uani 1 1 d . . . C49 C 0.7006(3) 0.3026(3) 0.17580(18) 0.0228(11) Uani 1 1 d . . . H49 H 0.6474 0.2921 0.1517 0.027 Uiso 1 1 calc R . . C50 C 0.7205(3) 0.3905(3) 0.19164(18) 0.0273(12) Uani 1 1 d . . . H50 H 0.6821 0.4387 0.1779 0.033 Uiso 1 1 calc R . . C51 C 0.7966(3) 0.4087(3) 0.22776(18) 0.0289(12) Uani 1 1 d . . . H51 H 0.8107 0.4690 0.2393 0.035 Uiso 1 1 calc R . . C52 C 0.8515(3) 0.3368(3) 0.24652(19) 0.0296(13) Uani 1 1 d . . . H52 H 0.9037 0.3479 0.2713 0.035 Uiso 1 1 calc R . . C53 C 0.8308(3) 0.2490(3) 0.22953(16) 0.0209(11) Uani 1 1 d . . . H53 H 0.8699 0.2013 0.2431 0.025 Uiso 1 1 calc R . . C54 C 0.7229(3) 0.1109(3) 0.11268(17) 0.0203(11) Uani 1 1 d . . . C55 C 0.7156(3) 0.1809(3) 0.07663(18) 0.0264(12) Uani 1 1 d . . . H55 H 0.7172 0.2421 0.0880 0.032 Uiso 1 1 calc R . . C56 C 0.7063(3) 0.1647(4) 0.02585(19) 0.0292(12) Uani 1 1 d . . . H56 H 0.7018 0.2146 0.0031 0.035 Uiso 1 1 calc R . . C57 C 0.7035(3) 0.0773(3) 0.00734(18) 0.0267(12) Uani 1 1 d . . . H57 H 0.6971 0.0664 -0.0279 0.032 Uiso 1 1 calc R . . C58 C 0.7102(3) 0.0057(3) 0.04102(19) 0.0277(12) Uani 1 1 d . . . H58 H 0.7075 -0.0552 0.0290 0.033 Uiso 1 1 calc R . . C59 C 0.7207(3) 0.0228(3) 0.09226(19) 0.0271(12) Uani 1 1 d . . . H59 H 0.7268 -0.0275 0.1148 0.033 Uiso 1 1 calc R . . C60 C 0.7990(3) 0.0515(3) 0.20509(17) 0.0235(11) Uani 1 1 d . . . C61 C 0.7867(3) -0.0051(3) 0.24357(19) 0.0286(12) Uani 1 1 d . . . H61 H 0.7306 -0.0065 0.2518 0.034 Uiso 1 1 calc R . . C62 C 0.8525(4) -0.0601(4) 0.27084(19) 0.0342(13) Uani 1 1 d . . . H62 H 0.8407 -0.0985 0.2968 0.041 Uiso 1 1 calc R . . C63 C 0.9358(3) -0.0591(4) 0.2603(2) 0.0344(14) Uani 1 1 d . . . H63 H 0.9814 -0.0960 0.2792 0.041 Uiso 1 1 calc R . . C64 C 0.9511(3) -0.0040(4) 0.2220(2) 0.0311(13) Uani 1 1 d . . . H64 H 1.0075 -0.0029 0.2143 0.037 Uiso 1 1 calc R . . C65 C 0.8843(3) 0.0497(3) 0.19489(19) 0.0268(12) Uani 1 1 d . . . H65 H 0.8961 0.0868 0.1684 0.032 Uiso 1 1 calc R . . N1 N 0.0033(4) 0.0937(5) -0.0605(3) 0.085(2) Uani 1 1 d . . . C66 C 0.0276(4) 0.0220(5) -0.0626(2) 0.0509(17) Uani 1 1 d . . . C67 C 0.0561(4) -0.0713(4) -0.0642(2) 0.0528(17) Uani 1 1 d . . . H67A H 0.0504 -0.1026 -0.0332 0.079 Uiso 1 1 calc R . . H67B H 0.1176 -0.0725 -0.0671 0.079 Uiso 1 1 calc R . . H67C H 0.0196 -0.1019 -0.0936 0.079 Uiso 1 1 calc R . . N2 N 0.0253(4) 0.2270(4) 0.1675(2) 0.0588(15) Uani 1 1 d . . . C68 C -0.0286(4) 0.2738(4) 0.1465(2) 0.0388(14) Uani 1 1 d . . . C69 C -0.0982(4) 0.3339(5) 0.1201(2) 0.0528(17) Uani 1 1 d . . . H69A H -0.1396 0.3457 0.1417 0.079 Uiso 1 1 calc R . . H69B H -0.1291 0.3048 0.0886 0.079 Uiso 1 1 calc R . . H69C H -0.0725 0.3914 0.1122 0.079 Uiso 1 1 calc R . . N3 N 0.3499(3) 0.3629(4) -0.19179(19) 0.0523(14) Uani 1 1 d . . . C70 C 0.3566(4) 0.2867(5) -0.1967(2) 0.0401(15) Uani 1 1 d . . . C71 C 0.3650(4) 0.1895(4) -0.2024(3) 0.0618(19) Uani 1 1 d . . . H71A H 0.4059 0.1651 -0.1726 0.093 Uiso 1 1 calc R . . H71B H 0.3873 0.1769 -0.2328 0.093 Uiso 1 1 calc R . . H71C H 0.3074 0.1607 -0.2055 0.093 Uiso 1 1 calc R . . N4 N 0.5843(4) 0.2539(4) -0.1270(2) 0.0636(16) Uani 1 1 d . . . C72 C 0.6225(4) 0.2126(4) -0.1506(2) 0.0402(15) Uani 1 1 d . . . C73 C 0.6701(4) 0.1597(4) -0.1804(2) 0.0456(15) Uani 1 1 d . . . H73A H 0.7179 0.1270 -0.1579 0.068 Uiso 1 1 calc R . . H73B H 0.6945 0.2001 -0.2026 0.068 Uiso 1 1 calc R . . H73C H 0.6303 0.1158 -0.2010 0.068 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 0.0142(4) 0.0246(4) 0.0235(4) 0.0016(3) 0.0056(3) 0.0009(3) P1 0.0168(6) 0.0228(7) 0.0203(6) -0.0002(5) 0.0049(5) 0.0003(5) P2 0.0183(7) 0.0233(7) 0.0210(7) 0.0005(6) 0.0065(5) 0.0012(5) P3 0.0176(7) 0.0231(7) 0.0201(6) 0.0012(5) 0.0063(5) 0.0008(5) F1 0.058(3) 0.047(3) 0.054(3) 0.009(3) -0.005(3) 0.006(3) F2 0.044(3) 0.048(3) 0.034(3) 0.012(2) 0.012(2) 0.011(2) F3 0.075(4) 0.088(5) 0.068(4) -0.010(4) 0.031(3) -0.018(3) B1 0.024(3) 0.027(3) 0.023(3) 0.005(3) 0.008(2) 0.001(2) C1 0.017(3) 0.021(3) 0.019(2) 0.005(2) 0.0013(19) 0.000(2) C2 0.024(3) 0.021(3) 0.023(3) -0.003(2) 0.009(2) 0.002(2) C3 0.024(3) 0.034(3) 0.020(3) 0.006(2) 0.009(2) 0.002(2) C4 0.021(3) 0.025(3) 0.030(3) 0.004(2) 0.005(2) -0.003(2) C5 0.020(3) 0.024(3) 0.021(3) -0.001(2) 0.001(2) 0.001(2) C6 0.017(2) 0.023(3) 0.021(3) 0.009(2) 0.001(2) 0.004(2) C7 0.018(3) 0.025(3) 0.021(3) -0.003(2) 0.008(2) 0.002(2) C8 0.023(3) 0.026(3) 0.023(3) -0.003(2) 0.009(2) 0.002(2) C9 0.025(3) 0.033(3) 0.019(3) -0.010(2) 0.003(2) 0.002(2) C10 0.019(3) 0.039(3) 0.024(3) -0.003(2) 0.001(2) 0.007(2) C11 0.020(3) 0.030(3) 0.021(3) 0.004(2) 0.005(2) 0.005(2) C12 0.019(3) 0.030(3) 0.018(2) 0.000(2) 0.009(2) -0.003(2) C13 0.015(2) 0.026(3) 0.021(3) 0.002(2) 0.006(2) -0.001(2) C14 0.021(3) 0.023(3) 0.022(3) 0.003(2) 0.000(2) 0.000(2) C15 0.021(3) 0.022(3) 0.037(3) -0.004(2) 0.003(2) 0.003(2) C16 0.023(3) 0.031(3) 0.030(3) -0.008(2) 0.013(2) 0.001(2) C17 0.023(3) 0.021(3) 0.025(3) -0.002(2) 0.005(2) -0.006(2) C18 0.014(2) 0.019(3) 0.030(3) -0.006(2) 0.006(2) -0.004(2) C19 0.014(3) 0.027(3) 0.029(3) 0.001(2) 0.005(2) 0.000(2) C20 0.037(3) 0.029(3) 0.036(3) -0.001(3) 0.004(3) 0.007(3) C21 0.047(4) 0.050(4) 0.028(3) 0.011(3) 0.004(3) 0.008(3) C22 0.039(3) 0.061(4) 0.028(3) -0.002(3) 0.000(3) -0.010(3) C23 0.055(4) 0.042(4) 0.038(4) -0.006(3) -0.006(3) -0.013(3) C24 0.040(3) 0.039(4) 0.038(3) -0.008(3) -0.004(3) -0.006(3) C25 0.016(3) 0.027(3) 0.026(3) -0.001(2) 0.003(2) 0.000(2) C26 0.028(3) 0.029(3) 0.027(3) -0.002(2) 0.003(2) 0.000(2) C27 0.035(3) 0.020(3) 0.048(4) 0.002(3) -0.001(3) 0.006(2) C28 0.032(3) 0.035(3) 0.048(4) -0.013(3) 0.013(3) 0.005(3) C29 0.048(4) 0.047(4) 0.037(3) -0.002(3) 0.019(3) 0.011(3) C30 0.033(3) 0.033(3) 0.034(3) 0.004(2) 0.016(2) 0.004(2) C31 0.017(3) 0.026(3) 0.025(3) 0.005(2) 0.002(2) 0.005(2) C32 0.035(3) 0.025(3) 0.034(3) -0.001(3) 0.018(2) 0.001(2) C33 0.040(3) 0.037(3) 0.035(3) 0.009(3) 0.019(3) 0.005(3) C34 0.029(3) 0.038(4) 0.048(4) 0.014(3) 0.013(3) 0.001(2) C35 0.051(4) 0.034(3) 0.040(4) 0.004(3) 0.011(3) -0.005(3) C36 0.044(3) 0.034(3) 0.041(3) 0.004(3) 0.016(3) -0.006(3) C37 0.012(5) 0.044(7) 0.031(6) -0.010(6) 0.015(4) -0.010(5) C38 0.022(5) 0.027(6) 0.042(6) 0.000(5) 0.001(5) -0.001(4) C39 0.015(5) 0.035(7) 0.032(6) -0.004(6) -0.004(4) 0.003(5) C40 0.018(5) 0.028(6) 0.031(6) 0.003(5) 0.007(5) -0.003(4) C41 0.026(5) 0.033(6) 0.042(7) 0.003(6) 0.010(5) -0.002(5) C37' 0.021(5) 0.029(6) 0.031(6) 0.006(5) 0.009(5) 0.004(4) C38' 0.018(5) 0.024(6) 0.026(6) 0.004(5) 0.006(4) 0.000(4) C39' 0.013(5) 0.033(6) 0.031(6) 0.004(5) 0.010(4) -0.005(5) C40' 0.017(5) 0.023(5) 0.028(6) -0.005(5) 0.002(5) -0.006(4) C41' 0.010(5) 0.026(6) 0.028(5) 0.006(5) 0.014(4) 0.001(5) C42 0.021(3) 0.022(3) 0.027(3) 0.007(2) 0.002(2) 0.005(2) C43 0.029(3) 0.026(3) 0.035(3) 0.003(2) 0.009(2) -0.004(2) C44 0.033(3) 0.035(3) 0.033(3) 0.008(2) 0.018(2) 0.009(2) C45 0.019(3) 0.034(3) 0.036(3) 0.016(3) 0.011(2) -0.001(2) C46 0.024(3) 0.035(3) 0.029(3) 0.012(3) -0.005(2) -0.004(2) C47 0.028(3) 0.038(3) 0.019(3) 0.000(2) 0.004(2) -0.007(2) C48 0.022(3) 0.027(3) 0.019(2) 0.000(2) 0.011(2) -0.004(2) C49 0.021(3) 0.025(3) 0.024(3) 0.001(2) 0.009(2) 0.002(2) C50 0.036(3) 0.026(3) 0.024(3) 0.002(2) 0.015(2) 0.008(2) C51 0.039(3) 0.023(3) 0.027(3) -0.001(2) 0.013(2) -0.006(2) C52 0.023(3) 0.039(3) 0.027(3) 0.001(2) 0.006(2) -0.010(2) C53 0.019(3) 0.028(3) 0.018(3) 0.004(2) 0.008(2) 0.000(2) C54 0.016(2) 0.021(3) 0.024(3) -0.001(2) 0.006(2) -0.0011(19) C55 0.026(3) 0.024(3) 0.030(3) -0.004(2) 0.008(2) 0.002(2) C56 0.025(3) 0.032(3) 0.033(3) 0.005(2) 0.012(2) -0.003(2) C57 0.025(3) 0.036(3) 0.019(3) -0.002(2) 0.006(2) 0.005(2) C58 0.025(3) 0.027(3) 0.031(3) -0.005(2) 0.005(2) 0.002(2) C59 0.023(3) 0.030(3) 0.029(3) 0.003(2) 0.007(2) -0.002(2) C60 0.029(3) 0.019(3) 0.023(3) -0.007(2) 0.006(2) -0.005(2) C61 0.028(3) 0.027(3) 0.030(3) -0.003(2) 0.007(2) -0.001(2) C62 0.047(4) 0.030(3) 0.025(3) 0.005(2) 0.007(2) 0.003(3) C63 0.030(3) 0.033(3) 0.035(3) -0.005(3) -0.004(2) 0.013(2) C64 0.020(3) 0.037(3) 0.035(3) -0.003(3) 0.003(2) 0.004(2) C65 0.028(3) 0.025(3) 0.029(3) -0.003(2) 0.009(2) -0.003(2) N1 0.090(5) 0.051(4) 0.117(6) -0.017(4) 0.025(4) -0.010(4) C66 0.047(4) 0.046(4) 0.060(4) -0.015(4) 0.014(3) -0.007(3) C67 0.036(3) 0.068(5) 0.058(4) -0.009(4) 0.019(3) -0.003(3) N2 0.052(4) 0.063(4) 0.065(4) -0.004(3) 0.018(3) 0.002(3) C68 0.038(4) 0.049(4) 0.034(3) -0.004(3) 0.018(3) -0.017(3) C69 0.029(3) 0.090(5) 0.043(4) 0.010(3) 0.016(3) -0.005(3) N3 0.059(4) 0.053(4) 0.051(3) -0.001(3) 0.027(3) -0.005(3) C70 0.040(4) 0.047(4) 0.038(4) -0.004(3) 0.018(3) -0.014(3) C71 0.064(5) 0.054(4) 0.071(5) -0.011(4) 0.022(4) -0.011(3) N4 0.075(4) 0.055(4) 0.068(4) -0.011(3) 0.031(3) -0.001(3) C72 0.049(4) 0.030(3) 0.039(4) 0.001(3) 0.005(3) -0.008(3) C73 0.051(4) 0.044(4) 0.044(4) 0.004(3) 0.015(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C37' 2.060(5) . ? Fe1 C38' 2.070(3) . ? Fe1 C41' 2.078(5) . ? Fe1 C41 2.090(8) . ? Fe1 C37 2.090(8) . ? Fe1 C40 2.093(8) . ? Fe1 C38 2.093(8) . ? Fe1 C39' 2.094(4) . ? Fe1 C39 2.095(8) . ? Fe1 C40' 2.098(5) . ? Fe1 P3 2.1421(13) . ? Fe1 P1 2.1522(14) . ? P1 C19 1.816(5) . ? P1 C1 1.826(5) . ? P1 C18 1.841(5) . ? P2 C25 1.814(5) . ? P2 C7 1.831(4) . ? P2 C6 1.831(5) . ? P3 C31 1.812(5) . ? P3 C12 1.824(5) . ? P3 C13 1.836(5) . ? F1 C20 1.297(7) . ? F2 C26 1.306(6) . ? F3 C32 1.329(7) . ? B1 C48 1.633(7) . ? B1 C54 1.645(7) . ? B1 C60 1.649(7) . ? B1 C42 1.655(7) . ? C1 C6 1.390(6) . ? C1 C2 1.392(6) . ? C2 C3 1.384(7) . ? C3 C4 1.369(7) . ? C4 C5 1.401(7) . ? C5 C6 1.389(6) . ? C7 C12 1.384(6) . ? C7 C8 1.393(6) . ? C8 C9 1.382(6) . ? C9 C10 1.372(7) . ? C10 C11 1.374(7) . ? C11 C12 1.402(6) . ? C13 C18 1.380(6) . ? C13 C14 1.391(6) . ? C14 C15 1.380(7) . ? C15 C16 1.383(7) . ? C16 C17 1.385(7) . ? C17 C18 1.394(7) . ? C19 C20 1.369(7) . ? C19 C24 1.388(7) . ? C20 C21 1.380(7) . ? C21 C22 1.374(8) . ? C22 C23 1.386(8) . ? C23 C24 1.383(7) . ? C25 C26 1.383(7) . ? C25 C30 1.391(7) . ? C26 C27 1.383(7) . ? C27 C28 1.373(8) . ? C28 C29 1.378(8) . ? C29 C30 1.397(7) . ? C31 C32 1.377(7) . ? C31 C36 1.387(7) . ? C32 C33 1.372(7) . ? C33 C34 1.375(8) . ? C34 C35 1.376(8) . ? C35 C36 1.380(7) . ? C37 C38 1.4200 . ? C37 C41 1.4200 . ? C38 C39 1.4200 . ? C39 C40 1.4200 . ? C40 C41 1.4200 . ? C37' C38' 1.4200 . ? C37' C41' 1.4200 . ? C38' C39' 1.4200 . ? C39' C40' 1.4200 . ? C40' C41' 1.4200 . ? C42 C43 1.3943 . ? C42 C47 1.404(6) . ? C43 C44 1.398(6) . ? C44 C45 1.399(7) . ? C45 C46 1.371(7) . ? C46 C47 1.390(7) . ? C48 C53 1.405(6) . ? C48 C49 1.406(6) . ? C49 C50 1.375(7) . ? C50 C51 1.390(7) . ? C51 C52 1.385(7) . ? C52 C53 1.385(7) . ? C54 C55 1.406(7) . ? C54 C59 1.406(6) . ? C55 C56 1.372(7) . ? C56 C57 1.378(7) . ? C57 C58 1.381(7) . ? C58 C59 1.384(7) . ? C60 C61 1.380(7) . ? C60 C65 1.420(7) . ? C61 C62 1.386(7) . ? C62 C63 1.392(8) . ? C63 C64 1.377(8) . ? C64 C65 1.384(7) . ? N1 C66 1.126(8) . ? C66 C67 1.445(9) . ? N2 C68 1.138(7) . ? C68 C69 1.459(9) . ? N3 C70 1.136(7) . ? C70 C71 1.446(9) . ? N4 C72 1.140(8) . ? C72 C73 1.441(9) . ? 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 C37' Fe1 C38' 40.21(7) . . ? C37' Fe1 C41' 40.14(9) . . ? C38' Fe1 C41' 67.27(12) . . ? C41 Fe1 C40 39.70(14) . . ? C37 Fe1 C40 66.64(17) . . ? C41 Fe1 C38 66.64(16) . . ? C37 Fe1 C38 39.69(13) . . ? C40 Fe1 C38 66.58(16) . . ? C37' Fe1 C39' 67.15(11) . . ? C38' Fe1 C39' 39.87(6) . . ? C41' Fe1 C39' 66.84(13) . . ? C41 Fe1 C39 66.61(17) . . ? C37 Fe1 C39 66.60(16) . . ? C40 Fe1 C39 39.65(14) . . ? C38 Fe1 C39 39.64(13) . . ? C37' Fe1 C40' 67.07(13) . . ? C38' Fe1 C40' 66.89(12) . . ? C41' Fe1 C40' 39.76(9) . . ? C39' Fe1 C40' 39.60(9) . . ? C41 Fe1 P3 93.8(2) . . ? C37 Fe1 P3 112.8(2) . . ? C40 Fe1 P3 111.4(2) . . ? C38 Fe1 P3 152.2(2) . . ? C39 Fe1 P3 150.5(2) . . ? C41 Fe1 P1 139.9(2) . . ? C37 Fe1 P1 160.0(2) . . ? C40 Fe1 P1 103.5(2) . . ? C38 Fe1 P1 121.0(2) . . ? C39 Fe1 P1 94.5(2) . . ? P3 Fe1 P1 86.75(5) . . ? C19 P1 C1 107.6(2) . . ? C19 P1 C18 104.7(2) . . ? C1 P1 C18 102.7(2) . . ? C19 P1 Fe1 119.87(16) . . ? C1 P1 Fe1 110.12(16) . . ? C18 P1 Fe1 110.42(17) . . ? C25 P2 C7 104.9(2) . . ? C25 P2 C6 106.3(2) . . ? C7 P2 C6 103.8(2) . . ? C25 P2 Fe1 120.19(15) . . ? C7 P2 Fe1 110.17(16) . . ? C6 P2 Fe1 110.19(16) . . ? C31 P3 C12 106.9(2) . . ? C31 P3 C13 105.9(2) . . ? C12 P3 C13 101.8(2) . . ? C31 P3 Fe1 119.67(15) . . ? C12 P3 Fe1 110.56(16) . . ? C13 P3 Fe1 110.49(15) . . ? C48 B1 C54 112.9(4) . . ? C48 B1 C60 109.5(4) . . ? C54 B1 C60 108.3(4) . . ? C48 B1 C42 107.7(4) . . ? C54 B1 C42 108.7(4) . . ? C60 B1 C42 109.7(4) . . ? C6 C1 C2 119.4(4) . . ? C6 C1 P1 115.4(3) . . ? C2 C1 P1 125.1(4) . . ? C3 C2 C1 119.6(4) . . ? C4 C3 C2 120.7(5) . . ? C3 C4 C5 120.9(5) . . ? C6 C5 C4 118.0(5) . . ? C5 C6 C1 121.3(4) . . ? C5 C6 P2 123.6(4) . . ? C1 C6 P2 115.1(3) . . ? C12 C7 C8 119.8(4) . . ? C12 C7 P2 115.1(3) . . ? C8 C7 P2 125.0(4) . . ? C9 C8 C7 119.4(5) . . ? C10 C9 C8 120.5(4) . . ? C9 C10 C11 121.2(4) . . ? C10 C11 C12 118.7(5) . . ? C7 C12 C11 120.4(4) . . ? C7 C12 P3 115.4(3) . . ? C11 C12 P3 124.2(4) . . ? C18 C13 C14 119.9(4) . . ? C18 C13 P3 115.6(3) . . ? C14 C13 P3 124.4(4) . . ? C15 C14 C13 119.8(5) . . ? C14 C15 C16 120.0(4) . . ? C15 C16 C17 120.9(5) . . ? C16 C17 C18 118.6(5) . . ? C13 C18 C17 120.7(4) . . ? C13 C18 P1 114.9(4) . . ? C17 C18 P1 124.3(4) . . ? C20 C19 C24 117.4(4) . . ? C20 C19 P1 122.2(4) . . ? C24 C19 P1 119.8(4) . . ? F1 C20 C19 118.8(5) . . ? F1 C20 C21 117.2(5) . . ? C19 C20 C21 122.7(5) . . ? C22 C21 C20 119.2(5) . . ? C21 C22 C23 119.6(5) . . ? C24 C23 C22 119.9(5) . . ? C23 C24 C19 121.1(5) . . ? C26 C25 C30 117.4(5) . . ? C26 C25 P2 121.6(4) . . ? C30 C25 P2 120.5(4) . . ? F2 C26 C25 120.1(5) . . ? F2 C26 C27 117.0(5) . . ? C25 C26 C27 122.3(5) . . ? C28 C27 C26 119.0(5) . . ? C27 C28 C29 121.0(5) . . ? C28 C29 C30 118.9(5) . . ? C25 C30 C29 121.4(5) . . ? C32 C31 C36 116.5(5) . . ? C32 C31 P3 123.4(4) . . ? C36 C31 P3 119.3(4) . . ? F3 C32 C33 116.6(5) . . ? F3 C32 C31 118.9(5) . . ? C33 C32 C31 123.4(5) . . ? C32 C33 C34 118.7(5) . . ? C33 C34 C35 119.8(5) . . ? C34 C35 C36 120.1(5) . . ? C35 C36 C31 121.3(5) . . ? C38 C37 C41 108.0 . . ? C38 C37 Fe1 70.3(3) . . ? C41 C37 Fe1 70.1(3) . . ? C39 C38 C37 108.0 . . ? C39 C38 Fe1 70.2(3) . . ? C37 C38 Fe1 70.0(3) . . ? C40 C39 C38 108.0 . . ? C40 C39 Fe1 70.1(3) . . ? C38 C39 Fe1 70.1(3) . . ? C41 C40 C39 108.0 . . ? C41 C40 Fe1 70.0(3) . . ? C39 C40 Fe1 70.3(3) . . ? C40 C41 C37 108.0 . . ? C40 C41 Fe1 70.3(3) . . ? C37 C41 Fe1 70.2(3) . . ? C38' C37' C41' 108.0 . . ? C38' C37' Fe1 70.28(13) . . ? C41' C37' Fe1 70.59(12) . . ? C37' C38' C39' 108.0 . . ? C37' C38' Fe1 69.51(17) . . ? C39' C38' Fe1 70.95(17) . . ? C40' C39' C38' 108.0 . . ? C40' C39' Fe1 70.37(12) . . ? C38' C39' Fe1 69.18(14) . . ? C41' C40' C39' 108.0 . . ? C41' C40' Fe1 69.34(17) . . ? C39' C40' Fe1 70.03(10) . . ? C40' C41' C37' 108.0 . . ? C40' C41' Fe1 70.90(18) . . ? C37' C41' Fe1 69.28(12) . . ? C43 C42 C47 114.7(3) . . ? C43 C42 B1 120.4(3) . . ? C47 C42 B1 124.9(4) . . ? C42 C43 C44 123.6(3) . . ? C43 C44 C45 119.2(5) . . ? C46 C45 C44 118.8(5) . . ? C45 C46 C47 120.8(5) . . ? C46 C47 C42 122.8(5) . . ? C53 C48 C49 114.2(4) . . ? C53 C48 B1 124.0(4) . . ? C49 C48 B1 121.7(4) . . ? C50 C49 C48 123.8(4) . . ? C49 C50 C51 120.0(4) . . ? C52 C51 C50 118.4(5) . . ? C51 C52 C53 120.6(4) . . ? C52 C53 C48 122.9(4) . . ? C55 C54 C59 114.2(4) . . ? C55 C54 B1 125.9(4) . . ? C59 C54 B1 119.8(4) . . ? C56 C55 C54 123.0(5) . . ? C55 C56 C57 120.9(5) . . ? C56 C57 C58 118.6(5) . . ? C57 C58 C59 119.9(5) . . ? C58 C59 C54 123.3(5) . . ? C61 C60 C65 115.3(4) . . ? C61 C60 B1 126.4(4) . . ? C65 C60 B1 118.2(4) . . ? C60 C61 C62 123.0(5) . . ? C61 C62 C63 120.1(5) . . ? C64 C63 C62 119.0(5) . . ? C63 C64 C65 120.1(5) . . ? C64 C65 C60 122.5(5) . . ? N1 C66 C67 177.7(8) . . ? N2 C68 C69 179.2(7) . . ? N3 C70 C71 179.3(7) . . ? N4 C72 C73 179.4(7) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.602 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.092 # Attachment '- Fig2_new.CIF' data_pgenumbering _database_code_depnum_ccdc_archive 'CCDC 804160' #TrackingRef '- Fig2_new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H62 As3 B F2 Fe N4' _chemical_formula_weight 1324.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' F F 0.0171 0.0103 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.6500(3) _cell_length_b 14.7771(4) _cell_length_c 27.3245(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.417(2) _cell_angle_gamma 90.00 _cell_volume 6171.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 22891 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 1.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7515 _exptl_absorpt_correction_T_max 0.9813 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '/f & /w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21135 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0976 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13900 _reflns_number_gt 9514 _reflns_threshold_expression >2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13900 _refine_ls_number_parameters 806 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.1251 _refine_ls_R_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.3029 _refine_ls_wR_factor_gt 0.2585 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.051 _refine_ls_shift/su_mean 0.036 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 0.18779(7) 0.35748(7) 0.02501(4) 0.0148(3) Uani 1 1 d . . . As1 As 0.26382(6) 0.35072(6) -0.03537(3) 0.0226(3) Uani 1 1 d . D . As2 As 0.27239(6) 0.47417(6) 0.05567(3) 0.0249(3) Uani 1 1 d . E . As3 As 0.28943(7) 0.26981(7) 0.07010(3) 0.0324(3) Uani 1 1 d . F . F1 F 0.1571(6) 0.4712(6) -0.1165(3) 0.034(3) Uani 0.610(19) 1 d P A 1 F2 F 0.1776(5) 0.6385(5) -0.0002(2) 0.034(2) Uani 0.759(19) 1 d P B 1 F3 F 0.2520(7) 0.2569(7) 0.1776(3) 0.045(3) Uani 0.63(2) 1 d P C 1 B1 B 0.7276(5) 0.1224(6) 0.1739(3) 0.0133(16) Uani 1 1 d . . . C1 C 0.3315(5) 0.4593(5) -0.0345(3) 0.0155(15) Uani 1 1 d . D . C2 C 0.3773(5) 0.4838(6) -0.0717(3) 0.0194(16) Uani 1 1 d . . . H2 H 0.3756 0.4460 -0.1000 0.023 Uiso 1 1 calc R . . C3 C 0.4242(5) 0.5626(6) -0.0665(3) 0.0200(16) Uani 1 1 d . . . H3 H 0.4535 0.5801 -0.0921 0.024 Uiso 1 1 calc R . . C4 C 0.4299(5) 0.6177(5) -0.0247(3) 0.0189(16) Uani 1 1 d . . . H4 H 0.4636 0.6717 -0.0216 0.023 Uiso 1 1 calc R . . C5 C 0.3862(5) 0.5934(5) 0.0125(3) 0.0177(15) Uani 1 1 d . G . H5 H 0.3904 0.6302 0.0415 0.021 Uiso 1 1 calc R . . C6 C 0.3365(5) 0.5154(5) 0.0070(2) 0.0135(14) Uani 1 1 d . . . C7 C 0.3623(5) 0.4340(5) 0.1101(2) 0.0144(15) Uani 1 1 d . . . C8 C 0.4216(5) 0.4917(6) 0.1416(3) 0.0211(17) Uani 1 1 d . G . H8 H 0.4174 0.5554 0.1373 0.025 Uiso 1 1 calc R . . C9 C 0.4865(5) 0.4543(6) 0.1792(3) 0.0242(18) Uani 1 1 d . . . H9 H 0.5261 0.4929 0.2009 0.029 Uiso 1 1 calc R G . C10 C 0.4936(5) 0.3612(6) 0.1851(3) 0.0211(17) Uani 1 1 d . G . H10 H 0.5385 0.3365 0.2106 0.025 Uiso 1 1 calc R . . C11 C 0.4347(5) 0.3024(6) 0.1536(3) 0.0222(17) Uani 1 1 d . . . H11 H 0.4394 0.2386 0.1574 0.027 Uiso 1 1 calc R G . C12 C 0.3701(5) 0.3409(5) 0.1170(3) 0.0141(14) Uani 1 1 d . F . C13 C 0.3632(4) 0.2219(5) 0.0293(2) 0.0121(14) Uani 1 1 d . . . C14 C 0.4286(5) 0.1580(5) 0.0457(3) 0.0162(15) Uani 1 1 d . G . H14 H 0.4359 0.1327 0.0783 0.019 Uiso 1 1 calc R . . C15 C 0.4833(5) 0.1310(5) 0.0144(3) 0.0211(17) Uani 1 1 d . . . H15 H 0.5286 0.0883 0.0256 0.025 Uiso 1 1 calc R G . C16 C 0.4709(5) 0.1675(5) -0.0337(3) 0.0194(16) Uani 1 1 d . G . H16 H 0.5068 0.1476 -0.0556 0.023 Uiso 1 1 calc R . . C17 C 0.4079(5) 0.2313(5) -0.0499(3) 0.0173(15) Uani 1 1 d . . . H17 H 0.4015 0.2566 -0.0824 0.021 Uiso 1 1 calc R G . C18 C 0.3529(5) 0.2594(5) -0.0187(3) 0.0137(14) Uani 1 1 d . D . C19 C 0.2083(5) 0.3264(6) -0.1024(3) 0.0199(16) Uani 1 1 d . . . C20 C 0.1659(7) 0.3902(7) -0.1337(3) 0.034(2) Uani 1 1 d . D 1 H20 H 0.1720 0.4516 -0.1231 0.041 Uiso 0.390(19) 1 calc PR A 1 C21 C 0.1133(7) 0.3712(7) -0.1807(3) 0.039(2) Uani 1 1 d . . . H21 H 0.0824 0.4180 -0.2008 0.047 Uiso 1 1 calc R D 1 C22 C 0.1074(6) 0.2819(7) -0.1973(3) 0.036(2) Uani 1 1 d . D . H22 H 0.0738 0.2669 -0.2296 0.043 Uiso 1 1 calc R . . C23 C 0.1511(7) 0.2154(7) -0.1661(4) 0.042(3) Uani 1 1 d . . . H23 H 0.1473 0.1543 -0.1772 0.050 Uiso 1 1 calc R D . C24 C 0.1992(7) 0.2354(7) -0.1200(3) 0.036(2) Uani 1 1 d . D . H24 H 0.2273 0.1881 -0.0991 0.043 Uiso 1 1 calc R . . C25 C 0.2266(5) 0.5800(5) 0.0802(3) 0.0168(15) Uani 1 1 d . . . C26 C 0.1865(6) 0.6463(6) 0.0480(3) 0.0250(18) Uani 1 1 d . E 1 H26 H 0.1873 0.6418 0.0134 0.030 Uiso 0.241(19) 1 calc PR B 1 C27 C 0.1456(6) 0.7187(6) 0.0645(4) 0.031(2) Uani 1 1 d . . . H27 H 0.1213 0.7653 0.0418 0.037 Uiso 1 1 calc R E 1 C28 C 0.1397(6) 0.7235(7) 0.1139(4) 0.034(2) Uani 1 1 d . E . H28 H 0.1103 0.7727 0.1255 0.041 Uiso 1 1 calc R . . C29 C 0.1772(7) 0.6558(7) 0.1468(3) 0.036(2) Uani 1 1 d . . . H29 H 0.1723 0.6579 0.1808 0.043 Uiso 1 1 calc R E . C30 C 0.2216(6) 0.5859(6) 0.1303(3) 0.0276(19) Uani 1 1 d . E . H30 H 0.2491 0.5411 0.1533 0.033 Uiso 1 1 calc R . . C31 C 0.2572(5) 0.1705(5) 0.1048(3) 0.0174(15) Uani 1 1 d . . . C32 C 0.2423(6) 0.1794(6) 0.1528(3) 0.0250(18) Uani 1 1 d . F 1 H32 H 0.2578 0.2345 0.1704 0.030 Uiso 0.37(2) 1 calc PR C 1 C33 C 0.2057(6) 0.1111(7) 0.1757(3) 0.030(2) Uani 1 1 d . . . H33 H 0.1947 0.1196 0.2082 0.036 Uiso 1 1 calc R F 1 C34 C 0.1852(6) 0.0294(7) 0.1506(3) 0.030(2) Uani 1 1 d . F . H34 H 0.1617 -0.0192 0.1663 0.036 Uiso 1 1 calc R . . C35 C 0.1995(6) 0.0193(6) 0.1024(3) 0.030(2) Uani 1 1 d . . . H35 H 0.1843 -0.0357 0.0847 0.036 Uiso 1 1 calc R F . C36 C 0.2363(6) 0.0903(6) 0.0801(3) 0.0255(18) Uani 1 1 d . F . H36 H 0.2470 0.0827 0.0474 0.031 Uiso 1 1 calc R . . C37 C 0.0848(13) 0.387(2) 0.0594(10) 0.043(3) Uani 0.50 1 d P G 1 H37 H 0.0897 0.4130 0.0917 0.051 Uiso 0.50 1 calc PR G 1 C38 C 0.0734(12) 0.4325(14) 0.0116(9) 0.032(4) Uani 0.50 1 d PU G 1 H38 H 0.0705 0.4964 0.0077 0.038 Uiso 0.50 1 calc PR G 1 C39 C 0.0677(14) 0.3769(16) -0.0250(8) 0.028(4) Uani 0.50 1 d PU G 1 H39 H 0.0612 0.3934 -0.0592 0.033 Uiso 0.50 1 calc PR G 1 C40 C 0.0724(12) 0.2892(15) -0.0070(9) 0.030(4) Uani 0.50 1 d PU G 1 H40 H 0.0671 0.2355 -0.0266 0.036 Uiso 0.50 1 calc PR G 1 C41 C 0.0868(13) 0.294(2) 0.0463(9) 0.043(3) Uani 0.50 1 d PU G 1 H41 H 0.0961 0.2440 0.0688 0.051 Uiso 0.50 1 calc PR G 1 C37' C 0.0765(11) 0.4156(15) 0.0384(8) 0.024(4) Uani 0.50 1 d PU G 2 H37' H 0.0763 0.4715 0.0555 0.029 Uiso 0.50 1 calc PR G 2 C38' C 0.0669(14) 0.403(2) -0.0129(10) 0.043(3) Uani 0.50 1 d P G 2 H38' H 0.0573 0.4503 -0.0368 0.051 Uiso 0.50 1 calc PR G 2 C39' C 0.0727(11) 0.3182(14) -0.0243(7) 0.019(3) Uani 0.50 1 d PU G 2 H39' H 0.0696 0.2946 -0.0570 0.023 Uiso 0.50 1 calc PR G 2 C40' C 0.0844(9) 0.2666(11) 0.0208(6) 0.015(3) Uani 0.50 1 d PU G 2 H40' H 0.0896 0.2025 0.0223 0.018 Uiso 0.50 1 calc PR G 2 C41' C 0.0873(9) 0.3208(11) 0.0615(6) 0.013(3) Uani 0.50 1 d PU G 2 H41' H 0.0943 0.3039 0.0956 0.015 Uiso 0.50 1 calc PR G 2 C42 C 0.6296(5) 0.1011(5) 0.1841(3) 0.0176(15) Uani 1 1 d . . . C43 C 0.6062(5) 0.1355(5) 0.2278(3) 0.0197(16) Uani 1 1 d . . . H43 H 0.6475 0.1707 0.2505 0.024 Uiso 1 1 calc R . . C44 C 0.5249(6) 0.1195(6) 0.2384(3) 0.0248(18) Uani 1 1 d . . . H44 H 0.5124 0.1426 0.2685 0.030 Uiso 1 1 calc R . . C45 C 0.4614(5) 0.0705(6) 0.2059(3) 0.0257(18) Uani 1 1 d . . . H45 H 0.4045 0.0627 0.2123 0.031 Uiso 1 1 calc R . . C46 C 0.4837(5) 0.0331(6) 0.1634(3) 0.0249(18) Uani 1 1 d . . . H46 H 0.4431 -0.0040 0.1413 0.030 Uiso 1 1 calc R . . C47 C 0.5662(6) 0.0504(6) 0.1533(3) 0.0233(17) Uani 1 1 d . . . H47 H 0.5791 0.0257 0.1236 0.028 Uiso 1 1 calc R . . C48 C 0.7550(5) 0.2255(5) 0.1929(2) 0.0136(14) Uani 1 1 d . . . C49 C 0.7002(5) 0.3011(6) 0.1756(3) 0.0199(16) Uani 1 1 d . . . H49 H 0.6468 0.2906 0.1522 0.024 Uiso 1 1 calc R . . C50 C 0.7204(6) 0.3874(5) 0.1910(3) 0.0208(16) Uani 1 1 d . . . H50 H 0.6822 0.4354 0.1774 0.025 Uiso 1 1 calc R . . C51 C 0.7974(6) 0.4067(6) 0.2269(3) 0.0230(17) Uani 1 1 d . . . H51 H 0.8110 0.4668 0.2383 0.028 Uiso 1 1 calc R . . C52 C 0.8525(5) 0.3357(6) 0.2451(3) 0.0211(17) Uani 1 1 d . . . H52 H 0.9050 0.3473 0.2691 0.025 Uiso 1 1 calc R . . C53 C 0.8325(5) 0.2477(6) 0.2289(3) 0.0175(15) Uani 1 1 d . . . H53 H 0.8719 0.2005 0.2422 0.021 Uiso 1 1 calc R . . C54 C 0.7244(5) 0.1096(5) 0.1133(3) 0.0155(15) Uani 1 1 d . . . C55 C 0.7164(5) 0.1787(6) 0.0785(3) 0.0202(16) Uani 1 1 d . . . H55 H 0.7165 0.2394 0.0899 0.024 Uiso 1 1 calc R . . C56 C 0.7080(5) 0.1629(6) 0.0263(3) 0.0212(17) Uani 1 1 d . . . H56 H 0.7030 0.2124 0.0037 0.025 Uiso 1 1 calc R . . C57 C 0.7071(5) 0.0771(6) 0.0091(3) 0.0228(17) Uani 1 1 d . . . H57 H 0.7014 0.0662 -0.0258 0.027 Uiso 1 1 calc R . . C58 C 0.7146(5) 0.0052(6) 0.0420(3) 0.0212(17) Uani 1 1 d . . . H58 H 0.7136 -0.0551 0.0299 0.025 Uiso 1 1 calc R . . C59 C 0.7239(5) 0.0219(6) 0.0938(3) 0.0201(16) Uani 1 1 d . . . H59 H 0.7300 -0.0281 0.1161 0.024 Uiso 1 1 calc R . . C60 C 0.7995(5) 0.0520(5) 0.2048(3) 0.0151(15) Uani 1 1 d . . . C61 C 0.7867(6) -0.0039(6) 0.2440(3) 0.0224(17) Uani 1 1 d . . . H61 H 0.7304 -0.0049 0.2516 0.027 Uiso 1 1 calc R . . C62 C 0.8512(6) -0.0578(6) 0.2721(3) 0.0256(18) Uani 1 1 d . . . H62 H 0.8389 -0.0946 0.2983 0.031 Uiso 1 1 calc R . . C63 C 0.9353(6) -0.0571(6) 0.2616(3) 0.0274(19) Uani 1 1 d . . . H63 H 0.9807 -0.0933 0.2806 0.033 Uiso 1 1 calc R . . C64 C 0.9508(6) -0.0035(6) 0.2233(3) 0.0261(18) Uani 1 1 d . . . H64 H 1.0074 -0.0026 0.2160 0.031 Uiso 1 1 calc R . . C65 C 0.8855(5) 0.0486(6) 0.1958(3) 0.0202(16) Uani 1 1 d . . . H65 H 0.8983 0.0842 0.1693 0.024 Uiso 1 1 calc R . . N1 N 0.0067(8) 0.0921(8) -0.0584(5) 0.072(3) Uani 1 1 d . . . C66 C 0.0280(7) 0.0195(8) -0.0616(4) 0.039(2) Uani 1 1 d . . . C67 C 0.0522(7) -0.0739(7) -0.0654(4) 0.039(2) Uani 1 1 d . . . H67A H 0.0348 -0.1089 -0.0388 0.059 Uiso 1 1 calc R . . H67B H 0.1157 -0.0782 -0.0621 0.059 Uiso 1 1 calc R . . H67C H 0.0226 -0.0979 -0.0981 0.059 Uiso 1 1 calc R . . N2 N 0.0224(6) 0.2306(7) 0.1658(3) 0.043(2) Uani 1 1 d . . . C68 C -0.0310(6) 0.2753(6) 0.1459(3) 0.028(2) Uani 1 1 d . . . C69 C -0.1006(7) 0.3333(8) 0.1193(4) 0.041(3) Uani 1 1 d . . . H69A H -0.0772 0.3940 0.1159 0.062 Uiso 1 1 calc R . . H69B H -0.1471 0.3371 0.1382 0.062 Uiso 1 1 calc R . . H69C H -0.1244 0.3081 0.0860 0.062 Uiso 1 1 calc R . . N3 N 0.3515(7) 0.3651(6) -0.1920(3) 0.046(2) Uani 1 1 d . . . C70 C 0.3567(6) 0.2895(8) -0.1976(3) 0.038(2) Uani 1 1 d . . . C71 C 0.3644(8) 0.1897(8) -0.2057(5) 0.051(3) Uani 1 1 d . . . H71A H 0.3778 0.1789 -0.2386 0.076 Uiso 1 1 calc R . . H71B H 0.3090 0.1600 -0.2041 0.076 Uiso 1 1 calc R . . H71C H 0.4114 0.1648 -0.1796 0.076 Uiso 1 1 calc R . . N4 N 0.5840(7) 0.2547(7) -0.1268(4) 0.053(2) Uani 1 1 d . . . C72 C 0.6194(7) 0.2128(7) -0.1511(4) 0.037(2) Uani 1 1 d . . . C73 C 0.6638(7) 0.1598(6) -0.1833(4) 0.035(2) Uani 1 1 d . . . H73A H 0.6209 0.1225 -0.2060 0.053 Uiso 1 1 calc R . . H73B H 0.7077 0.1206 -0.1626 0.053 Uiso 1 1 calc R . . H73C H 0.6926 0.2007 -0.2030 0.053 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 0.0121(5) 0.0162(6) 0.0162(5) 0.0014(4) 0.0032(4) 0.0014(4) As1 0.0256(5) 0.0207(5) 0.0207(5) 0.0001(3) 0.0035(3) 0.0002(3) As2 0.0294(5) 0.0231(5) 0.0227(5) -0.0001(3) 0.0064(3) 0.0014(4) As3 0.0354(6) 0.0303(6) 0.0314(5) 0.0006(4) 0.0069(4) 0.0004(4) F1 0.044(6) 0.018(5) 0.034(5) 0.002(3) -0.010(4) 0.009(4) F2 0.041(5) 0.033(4) 0.027(4) 0.008(3) 0.005(3) 0.009(3) F3 0.061(7) 0.039(6) 0.043(6) -0.016(4) 0.029(5) -0.014(5) B1 0.015(4) 0.012(4) 0.013(4) 0.001(3) 0.003(3) -0.001(3) C1 0.020(4) 0.010(4) 0.014(3) 0.002(3) -0.001(3) -0.002(3) C2 0.023(4) 0.023(4) 0.013(3) 0.002(3) 0.005(3) 0.006(3) C3 0.024(4) 0.022(4) 0.017(4) 0.005(3) 0.012(3) -0.004(3) C4 0.016(4) 0.017(4) 0.022(4) 0.002(3) 0.001(3) -0.007(3) C5 0.022(4) 0.016(4) 0.015(3) -0.004(3) 0.003(3) 0.002(3) C6 0.015(3) 0.017(4) 0.010(3) 0.000(3) 0.007(3) 0.001(3) C7 0.018(4) 0.017(4) 0.010(3) -0.004(3) 0.006(3) 0.003(3) C8 0.024(4) 0.016(4) 0.025(4) -0.008(3) 0.009(3) 0.000(3) C9 0.020(4) 0.036(5) 0.016(4) -0.010(3) 0.001(3) 0.001(4) C10 0.020(4) 0.030(5) 0.013(3) -0.002(3) 0.001(3) 0.005(3) C11 0.024(4) 0.022(4) 0.020(4) 0.008(3) 0.002(3) 0.011(3) C12 0.013(3) 0.014(4) 0.015(3) -0.003(3) 0.001(3) -0.001(3) C13 0.010(3) 0.012(4) 0.013(3) -0.001(3) 0.001(2) -0.002(3) C14 0.011(3) 0.017(4) 0.020(4) 0.001(3) 0.002(3) -0.001(3) C15 0.019(4) 0.013(4) 0.033(4) -0.003(3) 0.009(3) 0.003(3) C16 0.017(4) 0.019(4) 0.023(4) -0.005(3) 0.007(3) -0.001(3) C17 0.019(4) 0.020(4) 0.014(3) -0.004(3) 0.003(3) 0.000(3) C18 0.011(3) 0.014(4) 0.015(3) 0.001(3) 0.001(3) 0.001(3) C19 0.021(4) 0.023(4) 0.014(3) 0.002(3) 0.002(3) 0.002(3) C20 0.048(6) 0.028(5) 0.023(4) 0.006(4) 0.002(4) 0.011(4) C21 0.042(6) 0.045(6) 0.027(5) 0.015(4) -0.002(4) 0.014(5) C22 0.037(5) 0.044(6) 0.023(4) 0.005(4) 0.000(4) -0.005(5) C23 0.052(6) 0.033(6) 0.035(5) -0.008(4) -0.004(4) -0.009(5) C24 0.048(6) 0.026(5) 0.025(4) 0.006(4) -0.013(4) -0.001(4) C25 0.016(4) 0.014(4) 0.021(4) 0.002(3) 0.004(3) 0.002(3) C26 0.034(5) 0.023(4) 0.015(4) -0.003(3) -0.002(3) -0.003(4) C27 0.027(5) 0.015(4) 0.042(5) 0.001(4) -0.011(4) -0.003(4) C28 0.032(5) 0.028(5) 0.043(5) -0.009(4) 0.010(4) 0.010(4) C29 0.041(6) 0.043(6) 0.025(5) 0.000(4) 0.012(4) 0.014(5) C30 0.040(5) 0.021(5) 0.024(4) -0.001(3) 0.013(4) 0.003(4) C31 0.020(4) 0.012(4) 0.021(4) 0.005(3) 0.006(3) 0.003(3) C32 0.029(5) 0.022(4) 0.025(4) -0.006(3) 0.006(3) 0.004(4) C33 0.040(5) 0.036(5) 0.016(4) 0.007(4) 0.012(3) 0.009(4) C34 0.027(5) 0.035(5) 0.033(5) 0.014(4) 0.013(4) 0.002(4) C35 0.032(5) 0.023(5) 0.040(5) 0.000(4) 0.018(4) -0.007(4) C36 0.033(5) 0.022(5) 0.023(4) -0.002(3) 0.009(3) 0.001(4) C37 0.020(3) 0.076(3) 0.033(3) -0.0365(13) 0.0101(14) -0.0004(12) C38 0.032(4) 0.032(4) 0.032(4) 0.0003(13) 0.0071(15) 0.0005(13) C39 0.027(4) 0.028(4) 0.027(4) 0.0163(13) 0.0059(15) 0.0002(13) C40 0.030(4) 0.030(4) 0.030(4) -0.0001(13) 0.0063(15) -0.0002(13) C41 0.020(3) 0.076(3) 0.033(3) -0.0365(13) 0.0101(14) -0.0004(12) C37' 0.024(4) 0.035(4) 0.015(4) -0.0088(13) 0.0058(15) 0.0004(13) C38' 0.020(3) 0.076(3) 0.033(3) -0.0365(13) 0.0101(14) -0.0004(12) C39' 0.019(4) 0.020(4) 0.019(4) 0.0006(13) 0.0039(14) -0.0005(13) C40' 0.015(3) 0.015(3) 0.015(3) 0.0002(12) 0.0036(14) -0.0002(12) C41' 0.013(3) 0.013(3) 0.013(3) 0.0001(12) 0.0034(13) 0.0000(12) C42 0.018(4) 0.016(4) 0.017(3) 0.011(3) 0.000(3) 0.001(3) C43 0.022(4) 0.019(4) 0.021(4) 0.002(3) 0.009(3) -0.002(3) C44 0.036(5) 0.015(4) 0.026(4) 0.009(3) 0.014(4) 0.002(4) C45 0.017(4) 0.026(5) 0.036(5) 0.012(4) 0.009(3) -0.001(3) C46 0.016(4) 0.031(5) 0.025(4) 0.009(4) -0.001(3) -0.001(4) C47 0.030(4) 0.024(4) 0.017(4) 0.005(3) 0.006(3) -0.007(4) C48 0.016(4) 0.018(4) 0.009(3) -0.002(3) 0.007(3) -0.001(3) C49 0.019(4) 0.024(4) 0.019(4) 0.000(3) 0.009(3) 0.007(3) C50 0.034(5) 0.010(4) 0.021(4) 0.002(3) 0.012(3) 0.005(3) C51 0.031(5) 0.014(4) 0.026(4) -0.006(3) 0.010(3) -0.005(3) C52 0.017(4) 0.028(5) 0.018(4) -0.006(3) 0.003(3) -0.013(3) C53 0.020(4) 0.018(4) 0.015(3) 0.002(3) 0.004(3) 0.000(3) C54 0.013(3) 0.018(4) 0.014(3) -0.002(3) 0.002(3) 0.002(3) C55 0.026(4) 0.017(4) 0.019(4) -0.002(3) 0.010(3) 0.002(3) C56 0.023(4) 0.021(4) 0.021(4) 0.000(3) 0.007(3) 0.006(3) C57 0.017(4) 0.030(5) 0.021(4) 0.000(3) 0.005(3) -0.003(3) C58 0.026(4) 0.016(4) 0.020(4) -0.010(3) 0.002(3) 0.003(3) C59 0.025(4) 0.020(4) 0.017(4) -0.001(3) 0.008(3) 0.001(3) C60 0.018(4) 0.013(4) 0.014(3) -0.001(3) 0.004(3) -0.002(3) C61 0.028(4) 0.016(4) 0.024(4) -0.003(3) 0.007(3) 0.000(3) C62 0.035(5) 0.020(4) 0.019(4) 0.003(3) -0.001(3) 0.003(4) C63 0.032(5) 0.019(4) 0.025(4) -0.004(3) -0.009(3) 0.010(4) C64 0.020(4) 0.022(4) 0.032(4) -0.004(4) -0.003(3) 0.000(3) C65 0.020(4) 0.018(4) 0.022(4) -0.004(3) 0.002(3) -0.002(3) N1 0.078(8) 0.045(7) 0.091(8) -0.024(6) 0.015(6) 0.010(6) C66 0.036(6) 0.038(6) 0.043(6) -0.007(5) 0.007(4) -0.004(5) C67 0.040(6) 0.035(6) 0.046(6) -0.011(5) 0.016(4) 0.002(5) N2 0.051(6) 0.042(6) 0.040(5) -0.005(4) 0.019(4) 0.005(5) C68 0.037(5) 0.024(5) 0.028(4) -0.008(4) 0.018(4) -0.012(4) C69 0.039(6) 0.058(7) 0.027(5) 0.011(5) 0.007(4) -0.003(5) N3 0.062(6) 0.033(5) 0.049(5) -0.008(4) 0.027(5) -0.013(5) C70 0.029(5) 0.058(8) 0.031(5) -0.012(5) 0.017(4) -0.009(5) C71 0.056(7) 0.037(6) 0.060(7) -0.009(5) 0.017(6) -0.005(6) N4 0.064(7) 0.044(6) 0.057(6) -0.008(5) 0.026(5) -0.002(5) C72 0.048(6) 0.022(5) 0.038(5) -0.002(4) 0.006(4) -0.009(4) C73 0.049(6) 0.022(5) 0.037(5) 0.003(4) 0.014(4) 0.004(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C37' 2.045(17) . ? Fe1 C39 2.09(2) . ? Fe1 C38 2.070(19) . ? Fe1 C41 2.03(2) . ? Fe1 C39' 2.087(16) . ? Fe1 C40' 2.087(15) . ? Fe1 C41' 2.106(14) . ? Fe1 C40 2.089(19) . ? Fe1 C37 2.080(19) . ? Fe1 C38' 2.06(3) . ? Fe1 As3 2.2100(14) . ? Fe1 As2 2.2252(14) . ? As1 C19 1.886(7) . ? As1 C1 1.919(8) . ? As1 C18 1.923(7) . ? As2 C25 1.901(8) . ? As2 C7 1.910(7) . ? As2 C6 1.929(7) . ? As3 C31 1.874(7) . ? As3 C12 1.909(7) . ? As3 C13 1.905(7) . ? B1 C48 1.637(11) . ? B1 C42 1.646(11) . ? B1 C60 1.629(11) . ? B1 C54 1.657(10) . ? C1 C6 1.393(10) . ? C1 C2 1.412(11) . ? C2 C3 1.367(12) . ? C2 H2 0.9500 . ? C3 C4 1.391(11) . ? C3 H3 0.9500 . ? C4 C5 1.389(11) . ? C4 H4 0.9500 . ? C5 C6 1.381(11) . ? C5 H5 0.9500 . ? C7 C12 1.390(11) . ? C7 C8 1.409(11) . ? C8 C9 1.393(12) . ? C8 H8 0.9500 . ? C9 C10 1.388(12) . ? C9 H9 0.9500 . ? C10 C11 1.416(12) . ? C10 H10 0.9500 . ? C11 C12 1.381(10) . ? C11 H11 0.9500 . ? C13 C14 1.394(10) . ? C13 C18 1.401(10) . ? C14 C15 1.392(11) . ? C14 H14 0.9500 . ? C15 C16 1.393(12) . ? C15 H15 0.9500 . ? C16 C17 1.367(11) . ? C16 H16 0.9500 . ? C17 C18 1.399(10) . ? C17 H17 0.9500 . ? C19 C20 1.348(12) . ? C19 C24 1.424(13) . ? C20 C21 1.397(13) . ? C20 H20 0.9500 . ? C21 C22 1.391(15) . ? C21 H21 0.9500 . ? C22 C23 1.383(15) . ? C22 H22 0.9500 . ? C23 C24 1.353(13) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.389(11) . ? C25 C26 1.375(11) . ? C26 C27 1.371(13) . ? C26 H26 0.9500 . ? C27 C28 1.376(13) . ? C27 H27 0.9500 . ? C28 C29 1.387(14) . ? C28 H28 0.9500 . ? C29 C30 1.374(13) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.386(11) . ? C31 C36 1.368(12) . ? C32 C33 1.375(13) . ? C32 H32 0.9500 . ? C33 C34 1.392(14) . ? C33 H33 0.9500 . ? C34 C35 1.390(12) . ? C34 H34 0.9500 . ? C35 C36 1.397(12) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.45(3) . ? C37 C41 1.43(4) . ? C37 H37 0.9500 . ? C38 C39 1.28(3) . ? C38 H38 0.9500 . ? C39 C40 1.38(3) . ? C39 C41 2.27(4) . ? C39 H39 0.9500 . ? C40 C41 1.43(3) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C37' C41' 1.53(3) . ? C37' C38' 1.39(3) . ? C37' H37' 0.9500 . ? C38' C39' 1.29(4) . ? C38' H38' 0.9500 . ? C39' C40' 1.43(2) . ? C39' H39' 0.9500 . ? C40' C41' 1.36(2) . ? C40' H40' 0.9500 . ? C41' H41' 0.9500 . ? C42 C47 1.376(11) . ? C42 C43 1.418(11) . ? C43 C44 1.384(12) . ? C43 H43 0.9500 . ? C44 C45 1.385(13) . ? C44 H44 0.9500 . ? C45 C46 1.399(12) . ? C45 H45 0.9500 . ? C46 C47 1.399(11) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C53 1.425(10) . ? C48 C49 1.425(11) . ? C49 C50 1.359(12) . ? C49 H49 0.9500 . ? C50 C51 1.409(12) . ? C50 H50 0.9500 . ? C51 C52 1.381(12) . ? C51 H51 0.9500 . ? C52 C53 1.388(11) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C55 1.383(11) . ? C54 C59 1.400(11) . ? C55 C56 1.421(11) . ? C55 H55 0.9500 . ? C56 C57 1.352(12) . ? C56 H56 0.9500 . ? C57 C58 1.380(12) . ? C57 H57 0.9500 . ? C58 C59 1.413(11) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 C61 1.401(11) . ? C60 C65 1.421(11) . ? C61 C62 1.382(12) . ? C61 H61 0.9500 . ? C62 C63 1.407(13) . ? C62 H62 0.9500 . ? C63 C64 1.374(13) . ? C63 H63 0.9500 . ? C64 C65 1.369(12) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? N1 C66 1.132(15) . ? C66 C67 1.440(15) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? N2 C68 1.112(13) . ? C68 C69 1.452(15) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? N3 C70 1.133(14) . ? C70 C71 1.501(16) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? N4 C72 1.137(13) . ? C72 C73 1.460(14) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C37' Fe1 C39 51.6(8) . . ? C37' Fe1 C38 21.5(6) . . ? C39 Fe1 C38 35.8(8) . . ? C37' Fe1 C41 52.9(10) . . ? C39 Fe1 C41 66.7(9) . . ? C38 Fe1 C41 66.6(10) . . ? C37' Fe1 C39' 65.3(7) . . ? C39 Fe1 C39' 24.1(7) . . ? C38 Fe1 C39' 56.0(8) . . ? C41 Fe1 C39' 55.8(8) . . ? C37' Fe1 C40' 66.4(7) . . ? C39 Fe1 C40' 58.4(7) . . ? C38 Fe1 C40' 72.8(7) . . ? C41 Fe1 C40' 22.3(6) . . ? C39' Fe1 C40' 40.0(6) . . ? C37' Fe1 C41' 43.3(8) . . ? C39 Fe1 C41' 71.7(7) . . ? C38 Fe1 C41' 61.1(7) . . ? C41 Fe1 C41' 15.8(6) . . ? C39' Fe1 C41' 66.7(6) . . ? C40' Fe1 C41' 37.9(6) . . ? C37' Fe1 C40 65.5(7) . . ? C39 Fe1 C40 38.6(8) . . ? C38 Fe1 C40 63.1(8) . . ? C41 Fe1 C40 40.5(8) . . ? C39' Fe1 C40 17.6(6) . . ? C40' Fe1 C40 22.5(6) . . ? C41' Fe1 C40 53.6(7) . . ? C37' Fe1 C37 19.6(9) . . ? C39 Fe1 C37 65.9(9) . . ? C38 Fe1 C37 40.8(10) . . ? C41 Fe1 C37 40.6(11) . . ? C39' Fe1 C37 72.9(8) . . ? C40' Fe1 C37 59.5(9) . . ? C41' Fe1 C37 27.1(9) . . ? C40 Fe1 C37 66.9(8) . . ? C37' Fe1 C38' 39.6(7) . . ? C39 Fe1 C38' 13.9(8) . . ? C38 Fe1 C38' 22.0(7) . . ? C41 Fe1 C38' 66.9(12) . . ? C39' Fe1 C38' 36.3(10) . . ? C40' Fe1 C38' 64.2(10) . . ? C41' Fe1 C38' 67.9(9) . . ? C40 Fe1 C38' 47.9(11) . . ? C37 Fe1 C38' 56.2(10) . . ? C37' Fe1 As3 133.3(7) . . ? C39 Fe1 As3 151.9(6) . . ? C38 Fe1 As3 154.7(6) . . ? C41 Fe1 As3 94.6(8) . . ? C39' Fe1 As3 127.9(6) . . ? C40' Fe1 As3 96.3(4) . . ? C41' Fe1 As3 96.1(4) . . ? C40 Fe1 As3 113.8(7) . . ? C37 Fe1 As3 113.9(10) . . ? C38' Fe1 As3 160.4(9) . . ? C37' Fe1 As2 93.9(5) . . ? C39 Fe1 As2 121.2(6) . . ? C38 Fe1 As2 94.2(6) . . ? C41 Fe1 As2 133.5(7) . . ? C39' Fe1 As2 145.1(6) . . ? C40' Fe1 As2 155.6(5) . . ? C41' Fe1 As2 117.8(5) . . ? C40 Fe1 As2 157.3(6) . . ? C37 Fe1 As2 97.1(7) . . ? C38' Fe1 As2 110.2(9) . . ? As3 Fe1 As2 86.88(5) . . ? C19 As1 C1 108.0(3) . . ? C19 As1 C18 104.8(3) . . ? C1 As1 C18 102.3(3) . . ? C19 As1 Fe1 121.3(2) . . ? C1 As1 Fe1 109.5(2) . . ? C18 As1 Fe1 109.3(2) . . ? C25 As2 C7 104.5(3) . . ? C25 As2 C6 106.0(3) . . ? C7 As2 C6 103.3(3) . . ? C25 As2 Fe1 122.1(2) . . ? C7 As2 Fe1 109.4(2) . . ? C6 As2 Fe1 109.9(2) . . ? C31 As3 C12 107.6(3) . . ? C31 As3 C13 105.5(3) . . ? C12 As3 C13 101.6(3) . . ? C31 As3 Fe1 120.1(2) . . ? C12 As3 Fe1 110.2(2) . . ? C13 As3 Fe1 110.2(2) . . ? C48 B1 C42 108.3(6) . . ? C48 B1 C60 109.0(6) . . ? C42 B1 C60 110.8(6) . . ? C48 B1 C54 111.9(6) . . ? C42 B1 C54 108.5(6) . . ? C60 B1 C54 108.3(6) . . ? C6 C1 C2 119.0(7) . . ? C6 C1 As1 116.2(5) . . ? C2 C1 As1 124.7(6) . . ? C3 C2 C1 119.2(7) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 121.5(7) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 119.7(7) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 119.4(7) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 121.2(6) . . ? C1 C6 As2 115.2(6) . . ? C5 C6 As2 123.6(5) . . ? C12 C7 C8 119.3(7) . . ? C12 C7 As2 116.2(5) . . ? C8 C7 As2 124.5(6) . . ? C9 C8 C7 119.4(8) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 120.4(8) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.8(7) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 117.9(8) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C11 C12 C7 122.3(7) . . ? C11 C12 As3 122.3(6) . . ? C7 C12 As3 115.3(5) . . ? C14 C13 C18 119.8(6) . . ? C14 C13 As3 124.1(5) . . ? C18 C13 As3 116.0(5) . . ? C15 C14 C13 120.2(7) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.3(7) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 121.1(7) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 120.2(7) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 119.4(7) . . ? C13 C18 As1 115.5(5) . . ? C17 C18 As1 125.0(5) . . ? C20 C19 C24 116.5(8) . . ? C20 C19 As1 122.9(7) . . ? C24 C19 As1 120.0(6) . . ? C19 C20 C21 123.7(9) . . ? C19 C20 H20 118.1 . . ? C21 C20 H20 118.2 . . ? C22 C21 C20 118.4(9) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C21 C22 C23 118.9(9) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 121.4(10) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C19 121.1(9) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? C30 C25 C26 118.1(7) . . ? C30 C25 As2 120.3(6) . . ? C26 C25 As2 121.0(6) . . ? C27 C26 C25 121.8(8) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C28 C27 C26 119.8(8) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 119.4(8) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 120.2(8) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 120.7(8) . . ? C25 C30 H30 119.6 . . ? C29 C30 H30 119.7 . . ? C32 C31 C36 118.5(7) . . ? C32 C31 As3 121.5(6) . . ? C36 C31 As3 119.4(6) . . ? C31 C32 C33 122.1(8) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 118.9 . . ? C34 C33 C32 119.2(7) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 119.5(8) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C36 C35 C34 119.9(9) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C31 120.8(8) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C38 C37 C41 103.0(18) . . ? C38 C37 Fe1 69.2(11) . . ? C41 C37 Fe1 67.7(11) . . ? C38 C37 H37 127.8 . . ? C41 C37 H37 129.2 . . ? Fe1 C37 H37 126.1 . . ? C39 C38 C37 112.4(19) . . ? C39 C38 Fe1 73.0(13) . . ? C37 C38 Fe1 70.0(11) . . ? C39 C38 H38 123.5 . . ? C37 C38 H38 124.1 . . ? Fe1 C38 H38 125.0 . . ? C38 C39 C40 109.6(18) . . ? C38 C39 Fe1 71.2(12) . . ? C40 C39 Fe1 70.6(11) . . ? C38 C39 C41 72.8(14) . . ? C40 C39 C41 36.8(11) . . ? Fe1 C39 C41 55.3(7) . . ? C38 C39 H39 124.3 . . ? C40 C39 H39 126.1 . . ? Fe1 C39 H39 124.5 . . ? C41 C39 H39 162.8 . . ? C39 C40 C41 108(2) . . ? C39 C40 Fe1 70.8(12) . . ? C41 C40 Fe1 67.5(12) . . ? C39 C40 H40 125.5 . . ? C41 C40 H40 126.9 . . ? Fe1 C40 H40 127.2 . . ? C40 C41 C37 107(3) . . ? C40 C41 Fe1 72.1(13) . . ? C37 C41 Fe1 71.6(14) . . ? C40 C41 C39 35.6(13) . . ? C37 C41 C39 71.8(18) . . ? Fe1 C41 C39 58.0(9) . . ? C40 C41 H41 126.0 . . ? C37 C41 H41 126.7 . . ? Fe1 C41 H41 121.5 . . ? C39 C41 H41 161.4 . . ? C41' C37' C38' 106(2) . . ? C41' C37' Fe1 70.5(9) . . ? C38' C37' Fe1 70.9(12) . . ? C41' C37' H37' 127.5 . . ? C38' C37' H37' 127.0 . . ? Fe1 C37' H37' 123.0 . . ? C39' C38' C37' 112(3) . . ? C39' C38' Fe1 72.9(15) . . ? C37' C38' Fe1 69.5(13) . . ? C39' C38' H38' 123.4 . . ? C37' C38' H38' 124.4 . . ? Fe1 C38' H38' 125.5 . . ? C38' C39' C40' 108.1(18) . . ? C38' C39' Fe1 70.8(12) . . ? C40' C39' Fe1 70.0(9) . . ? C38' C39' H39' 125.9 . . ? C40' C39' H39' 126.0 . . ? Fe1 C39' H39' 124.7 . . ? C39' C40' C41' 111.5(14) . . ? C39' C40' Fe1 70.0(9) . . ? C41' C40' Fe1 71.8(9) . . ? C39' C40' H40' 124.1 . . ? C41' C40' H40' 124.5 . . ? Fe1 C40' H40' 125.4 . . ? C37' C41' C40' 102.8(14) . . ? C37' C41' Fe1 66.3(8) . . ? C40' C41' Fe1 70.3(9) . . ? C37' C41' H41' 128.7 . . ? C40' C41' H41' 128.5 . . ? Fe1 C41' H41' 126.5 . . ? C47 C42 C43 115.2(7) . . ? C47 C42 B1 125.3(7) . . ? C43 C42 B1 119.5(7) . . ? C44 C43 C42 122.1(8) . . ? C44 C43 H43 119.0 . . ? C42 C43 H43 118.9 . . ? C45 C44 C43 121.4(8) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C46 C45 C44 117.8(7) . . ? C46 C45 H45 121.1 . . ? C44 C45 H45 121.1 . . ? C45 C46 C47 119.8(8) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C42 C47 C46 123.7(8) . . ? C42 C47 H47 118.2 . . ? C46 C47 H47 118.1 . . ? C53 C48 C49 114.3(7) . . ? C53 C48 B1 124.0(7) . . ? C49 C48 B1 121.7(7) . . ? C50 C49 C48 123.3(8) . . ? C50 C49 H49 118.3 . . ? C48 C49 H49 118.4 . . ? C49 C50 C51 120.8(8) . . ? C49 C50 H50 119.6 . . ? C51 C50 H50 119.6 . . ? C52 C51 C50 118.2(7) . . ? C52 C51 H51 120.9 . . ? C50 C51 H51 120.9 . . ? C53 C52 C51 121.0(7) . . ? C53 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? C52 C53 C48 122.4(7) . . ? C52 C53 H53 118.8 . . ? C48 C53 H53 118.8 . . ? C55 C54 C59 115.4(7) . . ? C55 C54 B1 125.6(7) . . ? C59 C54 B1 118.9(7) . . ? C54 C55 C56 122.9(8) . . ? C54 C55 H55 118.5 . . ? C56 C55 H55 118.5 . . ? C57 C56 C55 119.7(8) . . ? C57 C56 H56 120.2 . . ? C55 C56 H56 120.2 . . ? C56 C57 C58 120.1(7) . . ? C56 C57 H57 120.0 . . ? C58 C57 H57 120.0 . . ? C57 C58 C59 119.6(7) . . ? C57 C58 H58 120.2 . . ? C59 C58 H58 120.2 . . ? C58 C59 C54 122.3(7) . . ? C58 C59 H59 118.9 . . ? C54 C59 H59 118.9 . . ? C61 C60 C65 114.0(7) . . ? C61 C60 B1 125.2(7) . . ? C65 C60 B1 120.5(6) . . ? C62 C61 C60 124.0(8) . . ? C62 C61 H61 118.0 . . ? C60 C61 H61 118.0 . . ? C61 C62 C63 119.0(8) . . ? C61 C62 H62 120.5 . . ? C63 C62 H62 120.5 . . ? C64 C63 C62 119.1(8) . . ? C64 C63 H63 120.5 . . ? C62 C63 H63 120.4 . . ? C63 C64 C65 120.6(8) . . ? C63 C64 H64 119.7 . . ? C65 C64 H64 119.7 . . ? C64 C65 C60 123.2(8) . . ? C64 C65 H65 118.4 . . ? C60 C65 H65 118.4 . . ? N1 C66 C67 177.9(13) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N2 C68 C69 179.4(10) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.4 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N3 C70 C71 179.1(11) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N4 C72 C73 178.8(12) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.320 _refine_diff_density_min -2.316 _refine_diff_density_rms 0.166