# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_FeCAB2b #TrackingRef 'web_deposit_cif_file_0_AndreFleckhaus_1355498170.FeCAB2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C26 H26 Fe N10), 4(F6 P), 0.22(C2), 0.4(N), 0.38(C)' _chemical_formula_sum 'C52.82 H52 F24 Fe2 N20.40 P4' _chemical_formula_weight 1664.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.2230(6) _cell_length_b 11.5332(3) _cell_length_c 29.2642(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.996(3) _cell_angle_gamma 90.00 _cell_volume 6741.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28857 _cell_measurement_theta_min 2.4815 _cell_measurement_theta_max 28.9007 _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3360 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_T_min 0.66018 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1829 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 148320 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.94 _reflns_number_total 16747 _reflns_number_gt 11589 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'Bruker SHELXTL (Sheldrick, 2008) and WinGX (Farrugia, 1999)' _computing_structure_refinement 'Bruker SHELXTL (Sheldrick, 2008) and WinGX (Farrugia, 1999)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+8.2577P] 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 16747 _refine_ls_number_parameters 949 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1727 _refine_ls_wR_factor_gt 0.1555 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 0.94544(2) 0.11204(4) 0.197795(15) 0.03542(12) Uani 1 1 d . . . Fe2 Fe 0.20296(2) 0.33078(4) 0.439218(15) 0.03785(12) Uani 1 1 d . . . P1 P 0.86253(5) 0.61033(10) 0.30183(4) 0.0572(3) Uani 1 1 d . . . P2 P 0.85698(6) 0.20103(12) 0.44335(4) 0.0679(3) Uani 1 1 d . . . P3 P 0.52066(5) 0.19141(10) 0.43074(4) 0.0562(3) Uani 1 1 d . . . P4 P 0.28369(6) 0.83059(9) 0.32984(4) 0.0575(3) Uani 1 1 d . . . F1 F 0.92768(14) 0.6896(3) 0.31653(11) 0.0991(10) Uani 1 1 d . . . F2 F 0.81692(14) 0.7117(2) 0.31754(10) 0.0798(7) Uani 1 1 d . . . F3 F 0.87296(16) 0.5580(2) 0.35296(9) 0.0872(8) Uani 1 1 d . . . F4 F 0.85288(14) 0.6634(3) 0.25126(9) 0.1044(11) Uani 1 1 d . . . F5 F 0.90804(17) 0.5085(3) 0.28670(12) 0.1160(12) Uani 1 1 d . . . F6 F 0.79681(14) 0.5330(2) 0.28808(10) 0.0823(8) Uani 1 1 d . . . F7 F 0.92645(17) 0.2504(3) 0.46843(13) 0.1242(13) Uani 1 1 d . . . F8 F 0.86094(16) 0.2817(3) 0.40001(11) 0.0973(9) Uani 1 1 d . . . F9 F 0.89490(19) 0.1026(3) 0.41977(12) 0.1137(11) Uani 1 1 d . . . F10 F 0.81880(19) 0.3019(3) 0.46487(12) 0.1216(12) Uani 1 1 d . . . F11 F 0.85246(19) 0.1180(3) 0.48610(11) 0.1209(12) Uani 1 1 d . . . F12 F 0.78731(16) 0.1503(3) 0.41727(11) 0.1068(11) Uani 1 1 d . . . F13 F 0.5047(2) 0.1565(5) 0.37863(12) 0.1598(18) Uani 1 1 d . . . F14 F 0.50735(19) 0.0630(3) 0.44379(15) 0.1227(13) Uani 1 1 d . . . F15 F 0.44485(15) 0.2272(3) 0.42989(15) 0.1187(12) Uani 1 1 d . . . F16 F 0.53729(15) 0.3201(3) 0.41605(13) 0.1054(11) Uani 1 1 d . . . F17 F 0.59733(14) 0.1597(3) 0.43054(12) 0.0996(10) Uani 1 1 d . . . F18 F 0.5399(2) 0.2247(3) 0.48264(10) 0.1232(13) Uani 1 1 d . . . F19 F 0.21718(15) 0.7549(3) 0.31669(14) 0.1195(13) Uani 1 1 d . . . F20 F 0.32727(17) 0.7264(3) 0.31517(12) 0.1021(10) Uani 1 1 d . . . F21 F 0.29337(17) 0.7803(3) 0.38003(10) 0.1137(12) Uani 1 1 d . . . F22 F 0.2729(2) 0.8806(3) 0.27912(10) 0.1274(14) Uani 1 1 d . . . F23 F 0.24037(17) 0.9359(3) 0.34449(12) 0.1110(11) Uani 1 1 d . . . F24 F 0.34953(16) 0.9061(3) 0.34241(12) 0.1032(10) Uani 1 1 d . . . N1 N 1.03504(14) 0.1136(3) 0.11891(10) 0.0462(7) Uani 1 1 d . . . N2 N 0.96419(14) 0.2512(3) 0.12166(9) 0.0452(7) Uani 1 1 d . . . N3 N 0.90133(13) 0.2551(2) 0.17843(9) 0.0386(6) Uani 1 1 d . . . N4 N 0.85006(14) 0.2327(3) 0.24019(10) 0.0445(6) Uani 1 1 d . . . N5 N 0.87113(15) 0.0833(3) 0.28409(10) 0.0483(7) Uani 1 1 d . . . N6 N 0.82354(14) -0.0093(3) 0.13646(10) 0.0536(8) Uani 1 1 d . . . N7 N 0.89965(16) -0.1155(3) 0.17562(11) 0.0518(7) Uani 1 1 d . . . N8 N 0.98833(14) -0.0324(2) 0.21831(10) 0.0436(6) Uani 1 1 d . . . N9 N 1.06787(14) 0.0806(3) 0.25741(10) 0.0527(8) Uani 1 1 d . . . N10 N 1.05969(16) 0.2658(3) 0.25280(11) 0.0579(8) Uani 1 1 d . . . N11 N 0.25967(13) 0.3674(2) 0.34621(9) 0.0406(6) Uani 1 1 d . . . N12 N 0.29091(13) 0.2184(2) 0.38772(9) 0.0413(6) Uani 1 1 d . . . N13 N 0.25363(14) 0.1907(2) 0.45518(9) 0.0404(6) Uani 1 1 d . . . N14 N 0.20373(17) 0.1906(3) 0.51825(10) 0.0546(8) Uani 1 1 d . . . N15 N 0.13423(17) 0.3261(3) 0.52874(11) 0.0592(8) Uani 1 1 d . . . N16 N 0.08889(18) 0.1624(4) 0.39414(12) 0.0709(11) Uani 1 1 d . . . N17 N 0.07287(15) 0.3472(4) 0.38883(11) 0.0642(10) Uani 1 1 d . . . N18 N 0.15275(14) 0.4704(3) 0.42205(10) 0.0476(7) Uani 1 1 d . . . N19 N 0.24230(16) 0.5622(3) 0.45935(11) 0.0524(7) Uani 1 1 d . . . N20 N 0.32663(15) 0.4645(3) 0.49331(11) 0.0542(8) Uani 1 1 d . . . N21 N 0.9945(7) 0.8919(14) 0.4164(11) 0.105(8) Uani 0.40(3) 1 d P . . C1 C 0.98747(16) 0.1483(3) 0.14328(11) 0.0408(7) Uani 1 1 d . . . C2 C 1.04205(19) 0.1917(4) 0.08355(13) 0.0566(10) Uani 1 1 d . . . H2 H 1.0721 0.1848 0.0627 0.068 Uiso 1 1 calc R . . C3 C 0.99853(19) 0.2774(4) 0.08477(13) 0.0549(9) Uani 1 1 d . . . H3 H 0.9921 0.3415 0.0653 0.066 Uiso 1 1 calc R . . C4 C 0.91489(17) 0.3113(3) 0.14017(12) 0.0439(8) Uani 1 1 d . . . C5 C 0.8824(2) 0.4129(3) 0.12398(13) 0.0554(9) Uani 1 1 d . . . H5 H 0.8924 0.4498 0.0976 0.066 Uiso 1 1 calc R . . C6 C 0.8345(2) 0.4576(3) 0.14857(15) 0.0628(11) Uani 1 1 d . . . H6 H 0.8114 0.5247 0.1382 0.075 Uiso 1 1 calc R . . C7 C 0.8210(2) 0.4034(3) 0.18813(14) 0.0565(9) Uani 1 1 d . . . H7 H 0.7897 0.4340 0.2050 0.068 Uiso 1 1 calc R . . C8 C 0.85532(17) 0.3021(3) 0.20200(12) 0.0444(8) Uani 1 1 d . . . C9 C 0.8116(2) 0.2451(4) 0.27565(14) 0.0591(10) Uani 1 1 d . . . H9 H 0.7830 0.3060 0.2798 0.071 Uiso 1 1 calc R . . C10 C 0.8242(2) 0.1521(4) 0.30217(14) 0.0601(10) Uani 1 1 d . . . H10 H 0.8052 0.1353 0.3283 0.072 Uiso 1 1 calc R . . C11 C 0.88794(16) 0.1315(3) 0.24552(11) 0.0405(7) Uani 1 1 d . . . C12 C 1.0773(2) 0.0104(4) 0.12993(15) 0.0615(10) Uani 1 1 d . . . H12A H 1.1074 0.0028 0.1078 0.092 Uiso 1 1 calc R . . H12B H 1.0495 -0.0574 0.1288 0.092 Uiso 1 1 calc R . . H12C H 1.1026 0.0183 0.1604 0.092 Uiso 1 1 calc R . . C13 C 0.8938(2) -0.0312(4) 0.30267(14) 0.0646(11) Uani 1 1 d . . . H13A H 0.8753 -0.0463 0.3303 0.097 Uiso 1 1 calc R . . H13B H 0.9418 -0.0319 0.3097 0.097 Uiso 1 1 calc R . . H13C H 0.8792 -0.0899 0.2801 0.097 Uiso 1 1 calc R . . C14 C 0.88193(17) -0.0005(3) 0.16515(11) 0.0445(8) Uani 1 1 d . . . C15 C 0.8047(2) -0.1256(5) 0.12932(17) 0.0769(14) Uani 1 1 d . . . H15 H 0.7662 -0.1522 0.1107 0.092 Uiso 1 1 calc R . . C16 C 0.8516(3) -0.1916(4) 0.15377(18) 0.0751(13) Uani 1 1 d . . . H16 H 0.8521 -0.2721 0.1558 0.090 Uiso 1 1 calc R . . C17 C 0.95969(19) -0.1352(3) 0.20507(14) 0.0514(9) Uani 1 1 d . . . C18 C 0.9883(2) -0.2407(4) 0.22011(18) 0.0710(13) Uani 1 1 d . . . H18 H 0.9679 -0.3106 0.2102 0.085 Uiso 1 1 calc R . . C19 C 1.0475(3) -0.2383(5) 0.2499(2) 0.0853(16) Uani 1 1 d . . . H19 H 1.0676 -0.3078 0.2606 0.102 Uiso 1 1 calc R . . C20 C 1.0782(2) -0.1349(5) 0.26457(16) 0.0716(13) Uani 1 1 d . . . H20 H 1.1183 -0.1337 0.2850 0.086 Uiso 1 1 calc R . . C21 C 1.04725(18) -0.0333(4) 0.24783(13) 0.0511(9) Uani 1 1 d . . . C22 C 1.02633(17) 0.1687(3) 0.23794(11) 0.0440(8) Uani 1 1 d . . . C23 C 1.1259(2) 0.1246(5) 0.28338(14) 0.0727(13) Uani 1 1 d . . . H23 H 1.1612 0.0823 0.2995 0.087 Uiso 1 1 calc R . . C24 C 1.1208(2) 0.2387(6) 0.28049(15) 0.0778(14) Uani 1 1 d . . . H24 H 1.1522 0.2918 0.2944 0.093 Uiso 1 1 calc R . . C25 C 0.7835(2) 0.0879(4) 0.11522(14) 0.0704(12) Uani 1 1 d . . . H25A H 0.7445 0.0587 0.0956 0.106 Uiso 1 1 calc R . . H25B H 0.8097 0.1332 0.0972 0.106 Uiso 1 1 calc R . . H25C H 0.7699 0.1356 0.1390 0.106 Uiso 1 1 calc R . . C26 C 1.0368(2) 0.3843(4) 0.24028(18) 0.0782(14) Uani 1 1 d . . . H26A H 1.0689 0.4390 0.2553 0.117 Uiso 1 1 calc R . . H26B H 0.9943 0.3974 0.2500 0.117 Uiso 1 1 calc R . . H26C H 1.0324 0.3939 0.2074 0.117 Uiso 1 1 calc R . . C27 C 0.25078(15) 0.3157(3) 0.38621(10) 0.0371(7) Uani 1 1 d . . . C28 C 0.30286(19) 0.3026(3) 0.32338(13) 0.0521(9) Uani 1 1 d . . . H28 H 0.3157 0.3211 0.2951 0.062 Uiso 1 1 calc R . . C29 C 0.32266(19) 0.2096(3) 0.34909(12) 0.0507(9) Uani 1 1 d . . . H29 H 0.3516 0.1514 0.3425 0.061 Uiso 1 1 calc R . . C30 C 0.29437(17) 0.1473(3) 0.42693(11) 0.0422(7) Uani 1 1 d . . . C31 C 0.33268(19) 0.0487(3) 0.43740(13) 0.0526(9) Uani 1 1 d . . . H31 H 0.3610 0.0217 0.4176 0.063 Uiso 1 1 calc R . . C32 C 0.3276(2) -0.0086(3) 0.47836(14) 0.0595(10) Uani 1 1 d . . . H32 H 0.3529 -0.0750 0.4863 0.071 Uiso 1 1 calc R . . C33 C 0.2847(2) 0.0325(3) 0.50770(14) 0.0597(10) Uani 1 1 d . . . H33 H 0.2804 -0.0059 0.5350 0.072 Uiso 1 1 calc R . . C34 C 0.24888(19) 0.1328(3) 0.49468(12) 0.0477(8) Uani 1 1 d . . . C35 C 0.17493(18) 0.2911(3) 0.49867(12) 0.0488(8) Uani 1 1 d . . . C36 C 0.1813(3) 0.1648(4) 0.55990(14) 0.0724(13) Uani 1 1 d . . . H36 H 0.1935 0.1017 0.5792 0.087 Uiso 1 1 calc R . . C37 C 0.1388(3) 0.2494(4) 0.56625(15) 0.0771(14) Uani 1 1 d . . . H37 H 0.1159 0.2563 0.5913 0.092 Uiso 1 1 calc R . . C38 C 0.2318(2) 0.4812(3) 0.33009(13) 0.0538(9) Uani 1 1 d . . . H38A H 0.2450 0.4992 0.3008 0.081 Uiso 1 1 calc R . . H38B H 0.2485 0.5397 0.3522 0.081 Uiso 1 1 calc R . . H38C H 0.1838 0.4785 0.3268 0.081 Uiso 1 1 calc R . . C39 C 0.0912(3) 0.4284(5) 0.52316(18) 0.0865(15) Uani 1 1 d . . . H39A H 0.0675 0.4344 0.5490 0.130 Uiso 1 1 calc R . . H39B H 0.0598 0.4216 0.4951 0.130 Uiso 1 1 calc R . . H39C H 0.1182 0.4964 0.5217 0.130 Uiso 1 1 calc R . . C40 C 0.12030(17) 0.2635(4) 0.40585(12) 0.0508(9) Uani 1 1 d . . . C41 C 0.0239(3) 0.1820(7) 0.37045(18) 0.097(2) Uani 1 1 d . . . H41 H -0.0066 0.1248 0.3589 0.116 Uiso 1 1 calc R . . C42 C 0.0132(2) 0.2956(7) 0.36729(18) 0.0928(19) Uani 1 1 d . . . H42 H -0.0257 0.3330 0.3537 0.111 Uiso 1 1 calc R . . C43 C 0.09045(19) 0.4629(4) 0.39637(14) 0.0622(11) Uani 1 1 d . . . C44 C 0.0535(3) 0.5609(6) 0.38201(18) 0.0932(18) Uani 1 1 d . . . H44 H 0.0107 0.5552 0.3650 0.112 Uiso 1 1 calc R . . C45 C 0.0823(3) 0.6678(6) 0.3939(2) 0.102(2) Uani 1 1 d . . . H45 H 0.0586 0.7348 0.3841 0.122 Uiso 1 1 calc R . . C46 C 0.1455(3) 0.6781(4) 0.41982(18) 0.0843(15) Uani 1 1 d . . . H46 H 0.1644 0.7501 0.4279 0.101 Uiso 1 1 calc R . . C47 C 0.1790(2) 0.5760(3) 0.43313(13) 0.0546(9) Uani 1 1 d . . . C48 C 0.26616(17) 0.4495(3) 0.46736(11) 0.0434(8) Uani 1 1 d . . . C49 C 0.2889(3) 0.6428(4) 0.48047(17) 0.0732(13) Uani 1 1 d . . . H49 H 0.2846 0.7231 0.4800 0.088 Uiso 1 1 calc R . . C50 C 0.3407(2) 0.5817(4) 0.50131(16) 0.0702(13) Uani 1 1 d . . . H50 H 0.3796 0.6118 0.5183 0.084 Uiso 1 1 calc R . . C51 C 0.1186(3) 0.0483(5) 0.4043(2) 0.102(2) Uani 1 1 d . . . H51A H 0.0868 -0.0105 0.3927 0.153 Uiso 1 1 calc R . . H51B H 0.1309 0.0395 0.4371 0.153 Uiso 1 1 calc R . . H51C H 0.1578 0.0408 0.3897 0.153 Uiso 1 1 calc R . . C52 C 0.3733(2) 0.3710(5) 0.50997(16) 0.0757(13) Uani 1 1 d . . . H52A H 0.4130 0.4034 0.5277 0.113 Uiso 1 1 calc R . . H52B H 0.3851 0.3291 0.4840 0.113 Uiso 1 1 calc R . . H52C H 0.3525 0.3192 0.5291 0.113 Uiso 1 1 calc R . . C53 C 0.9902(7) 0.9201(19) 0.4497(13) 0.098(12) Uani 0.39(4) 1 d P . . C54 C 0.9819(11) 0.9562(19) 0.4997(11) 0.147(12) Uani 0.43(2) 1 d P . . 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 0.0326(2) 0.0400(2) 0.0331(2) 0.00016(19) 0.00325(17) -0.00148(18) Fe2 0.0340(2) 0.0448(3) 0.0341(2) -0.0023(2) 0.00319(18) -0.00446(19) P1 0.0554(6) 0.0667(7) 0.0496(5) 0.0043(5) 0.0089(5) 0.0082(5) P2 0.0655(7) 0.0767(8) 0.0622(7) 0.0004(6) 0.0123(5) -0.0007(6) P3 0.0559(6) 0.0591(6) 0.0519(6) -0.0068(5) 0.0031(5) -0.0053(5) P4 0.0633(6) 0.0542(6) 0.0518(6) 0.0027(5) -0.0009(5) 0.0091(5) F1 0.0676(18) 0.111(2) 0.112(2) 0.0242(19) -0.0063(16) -0.0154(16) F2 0.0822(18) 0.0637(15) 0.095(2) 0.0004(14) 0.0195(15) 0.0126(13) F3 0.121(2) 0.0813(18) 0.0574(15) 0.0165(13) 0.0085(15) 0.0123(17) F4 0.0769(19) 0.175(3) 0.0627(16) 0.0380(19) 0.0141(14) 0.000(2) F5 0.099(2) 0.140(3) 0.110(2) -0.028(2) 0.0179(19) 0.052(2) F6 0.0780(17) 0.0762(17) 0.0924(19) -0.0137(15) 0.0126(14) -0.0098(14) F7 0.092(2) 0.137(3) 0.131(3) 0.001(2) -0.025(2) -0.013(2) F8 0.108(2) 0.094(2) 0.092(2) 0.0211(17) 0.0250(18) -0.0066(18) F9 0.135(3) 0.099(2) 0.111(3) 0.000(2) 0.030(2) 0.030(2) F10 0.122(3) 0.143(3) 0.103(2) -0.025(2) 0.028(2) 0.038(2) F11 0.127(3) 0.153(3) 0.080(2) 0.043(2) 0.0089(19) -0.017(2) F12 0.090(2) 0.134(3) 0.090(2) 0.021(2) -0.0029(17) -0.036(2) F13 0.178(4) 0.217(5) 0.069(2) -0.043(3) -0.025(2) 0.006(4) F14 0.129(3) 0.0653(18) 0.180(4) -0.003(2) 0.042(3) -0.0312(19) F15 0.0638(18) 0.108(2) 0.189(4) -0.019(2) 0.033(2) -0.0090(17) F16 0.080(2) 0.080(2) 0.152(3) 0.041(2) 0.0073(19) 0.0042(16) F17 0.0721(18) 0.102(2) 0.127(3) 0.0206(19) 0.0242(17) 0.0169(16) F18 0.167(3) 0.144(3) 0.0602(17) -0.0307(19) 0.0205(19) -0.035(3) F19 0.080(2) 0.085(2) 0.175(3) 0.006(2) -0.035(2) -0.0031(16) F20 0.112(2) 0.082(2) 0.114(2) -0.0100(18) 0.0250(19) 0.0271(18) F21 0.103(2) 0.164(3) 0.0742(19) 0.049(2) 0.0139(17) 0.025(2) F22 0.211(4) 0.104(2) 0.0575(17) 0.0179(17) -0.010(2) 0.012(3) F23 0.109(2) 0.098(2) 0.121(3) -0.025(2) 0.002(2) 0.0452(19) F24 0.089(2) 0.097(2) 0.123(3) -0.0152(19) 0.0135(18) -0.0204(18) N1 0.0367(14) 0.0589(18) 0.0443(15) -0.0056(14) 0.0107(12) -0.0044(13) N2 0.0488(16) 0.0524(17) 0.0338(14) 0.0061(13) 0.0048(12) -0.0031(13) N3 0.0355(14) 0.0454(15) 0.0341(13) -0.0018(12) 0.0027(11) -0.0034(11) N4 0.0451(16) 0.0486(16) 0.0413(15) -0.0049(13) 0.0111(12) -0.0004(13) N5 0.0526(17) 0.0564(18) 0.0371(15) -0.0022(13) 0.0108(13) -0.0125(14) N6 0.0377(15) 0.076(2) 0.0468(17) -0.0178(16) 0.0063(13) -0.0098(15) N7 0.0530(18) 0.0466(17) 0.0588(19) -0.0088(15) 0.0179(15) -0.0085(14) N8 0.0392(15) 0.0476(16) 0.0451(15) 0.0063(13) 0.0099(12) 0.0025(12) N9 0.0362(15) 0.080(2) 0.0401(16) 0.0091(15) -0.0014(12) -0.0008(15) N10 0.0471(18) 0.073(2) 0.0530(18) -0.0138(16) 0.0071(14) -0.0206(16) N11 0.0395(15) 0.0444(15) 0.0367(14) 0.0011(12) 0.0026(11) -0.0054(12) N12 0.0405(15) 0.0452(15) 0.0380(14) 0.0018(12) 0.0056(11) 0.0014(12) N13 0.0423(15) 0.0412(15) 0.0367(14) -0.0006(12) 0.0029(11) -0.0068(12) N14 0.069(2) 0.0552(19) 0.0404(16) 0.0018(14) 0.0116(15) -0.0145(16) N15 0.064(2) 0.069(2) 0.0493(18) -0.0125(16) 0.0236(16) -0.0141(17) N16 0.064(2) 0.093(3) 0.056(2) -0.013(2) 0.0099(17) -0.041(2) N17 0.0301(15) 0.106(3) 0.0547(19) -0.0116(19) 0.0013(13) -0.0046(17) N18 0.0384(15) 0.0635(19) 0.0412(15) -0.0012(14) 0.0071(12) 0.0067(14) N19 0.062(2) 0.0459(17) 0.0511(18) -0.0073(14) 0.0130(15) -0.0067(15) N20 0.0445(17) 0.070(2) 0.0473(17) -0.0088(15) 0.0052(13) -0.0154(15) N21 0.081(9) 0.105(10) 0.138(19) -0.010(10) 0.044(9) -0.005(7) C1 0.0358(16) 0.0485(18) 0.0360(16) -0.0033(14) -0.0007(13) -0.0052(14) C2 0.050(2) 0.079(3) 0.045(2) 0.0003(19) 0.0173(17) -0.012(2) C3 0.055(2) 0.066(2) 0.046(2) 0.0114(18) 0.0132(17) -0.0111(19) C4 0.0438(18) 0.0453(19) 0.0408(17) 0.0021(15) 0.0007(14) -0.0022(15) C5 0.063(2) 0.050(2) 0.051(2) 0.0108(17) 0.0015(18) -0.0006(18) C6 0.068(3) 0.046(2) 0.069(3) 0.0052(19) -0.007(2) 0.0124(19) C7 0.055(2) 0.052(2) 0.060(2) -0.0091(19) 0.0037(18) 0.0129(18) C8 0.0415(18) 0.0459(18) 0.0445(18) -0.0088(15) 0.0031(14) -0.0007(15) C9 0.060(2) 0.069(3) 0.053(2) -0.013(2) 0.0235(19) 0.000(2) C10 0.064(2) 0.073(3) 0.049(2) -0.011(2) 0.0248(19) -0.014(2) C11 0.0377(17) 0.0481(18) 0.0343(16) -0.0048(14) 0.0014(13) -0.0105(14) C12 0.050(2) 0.067(3) 0.070(3) -0.007(2) 0.0188(19) 0.0060(19) C13 0.081(3) 0.060(2) 0.055(2) 0.007(2) 0.018(2) -0.010(2) C14 0.0390(18) 0.056(2) 0.0409(17) -0.0087(16) 0.0127(14) -0.0069(15) C15 0.064(3) 0.091(4) 0.077(3) -0.034(3) 0.015(2) -0.035(3) C16 0.079(3) 0.063(3) 0.088(3) -0.027(3) 0.028(3) -0.026(2) C17 0.051(2) 0.047(2) 0.061(2) 0.0037(17) 0.0221(18) 0.0020(16) C18 0.080(3) 0.050(2) 0.092(3) 0.013(2) 0.039(3) 0.010(2) C19 0.080(3) 0.073(3) 0.108(4) 0.036(3) 0.033(3) 0.033(3) C20 0.053(2) 0.092(3) 0.071(3) 0.037(3) 0.016(2) 0.027(2) C21 0.0394(18) 0.067(2) 0.048(2) 0.0168(18) 0.0103(15) 0.0088(17) C22 0.0377(17) 0.060(2) 0.0348(16) 0.0005(15) 0.0059(13) -0.0050(16) C23 0.041(2) 0.123(4) 0.050(2) 0.011(3) -0.0047(17) -0.007(2) C24 0.049(2) 0.124(5) 0.056(3) -0.012(3) -0.0061(19) -0.029(3) C25 0.045(2) 0.111(4) 0.052(2) -0.003(2) -0.0026(18) -0.001(2) C26 0.079(3) 0.063(3) 0.091(3) -0.020(3) 0.007(3) -0.023(2) C27 0.0309(15) 0.0436(17) 0.0345(15) -0.0005(13) -0.0018(12) -0.0092(13) C28 0.052(2) 0.064(2) 0.0425(19) -0.0014(17) 0.0129(16) -0.0043(18) C29 0.052(2) 0.056(2) 0.046(2) -0.0018(17) 0.0119(16) 0.0028(17) C30 0.0425(18) 0.0444(18) 0.0376(17) 0.0012(14) -0.0003(14) -0.0024(14) C31 0.052(2) 0.049(2) 0.054(2) -0.0035(17) 0.0011(17) 0.0039(17) C32 0.067(3) 0.047(2) 0.060(2) 0.0058(18) -0.007(2) 0.0060(18) C33 0.076(3) 0.051(2) 0.048(2) 0.0121(18) -0.0020(19) -0.008(2) C34 0.060(2) 0.0460(19) 0.0367(17) 0.0028(15) 0.0046(16) -0.0108(16) C35 0.050(2) 0.056(2) 0.0398(18) -0.0091(16) 0.0062(15) -0.0155(17) C36 0.106(4) 0.068(3) 0.048(2) 0.002(2) 0.024(2) -0.019(3) C37 0.106(4) 0.084(3) 0.049(2) -0.005(2) 0.036(2) -0.017(3) C38 0.061(2) 0.047(2) 0.052(2) 0.0073(17) 0.0049(18) -0.0049(17) C39 0.095(4) 0.096(4) 0.078(3) -0.007(3) 0.044(3) 0.013(3) C40 0.0380(18) 0.076(3) 0.0389(18) -0.0073(18) 0.0085(14) -0.0138(18) C41 0.056(3) 0.158(6) 0.076(3) -0.027(4) 0.008(2) -0.056(4) C42 0.036(2) 0.166(6) 0.073(3) -0.026(4) 0.001(2) -0.016(3) C43 0.043(2) 0.093(3) 0.050(2) -0.001(2) 0.0054(17) 0.019(2) C44 0.067(3) 0.132(5) 0.076(3) 0.002(3) -0.004(2) 0.049(3) C45 0.117(5) 0.096(4) 0.089(4) 0.014(3) 0.008(4) 0.064(4) C46 0.115(4) 0.065(3) 0.076(3) 0.005(2) 0.023(3) 0.031(3) C47 0.068(3) 0.049(2) 0.048(2) -0.0001(17) 0.0135(18) 0.0111(18) C48 0.0429(18) 0.054(2) 0.0347(16) -0.0038(15) 0.0090(14) -0.0087(15) C49 0.093(4) 0.058(3) 0.075(3) -0.024(2) 0.032(3) -0.031(3) C50 0.062(3) 0.084(3) 0.066(3) -0.022(2) 0.013(2) -0.035(2) C51 0.135(5) 0.084(4) 0.086(4) -0.010(3) 0.010(3) -0.061(4) C52 0.044(2) 0.115(4) 0.064(3) -0.006(3) -0.0064(19) 0.003(2) C53 0.053(8) 0.112(14) 0.13(3) 0.024(14) 0.011(9) 0.036(8) C54 0.12(2) 0.17(3) 0.142(19) 0.01(2) 0.008(16) 0.052(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 N3 1.919(3) . ? Fe1 N8 1.930(3) . ? Fe1 C11 1.965(3) . ? Fe1 C14 1.965(3) . ? Fe1 C1 1.966(3) . ? Fe1 C22 1.970(3) . ? Fe2 N18 1.928(3) . ? Fe2 N13 1.931(3) . ? Fe2 C40 1.960(3) . ? Fe2 C27 1.960(3) . ? Fe2 C48 1.964(3) . ? Fe2 C35 1.966(4) . ? P1 F4 1.585(3) . ? P1 F5 1.597(3) . ? P1 F3 1.597(3) . ? P1 F6 1.599(3) . ? P1 F2 1.600(3) . ? P1 F1 1.606(3) . ? P2 F10 1.581(3) . ? P2 F8 1.585(3) . ? P2 F7 1.586(3) . ? P2 F9 1.587(3) . ? P2 F11 1.589(3) . ? P2 F12 1.604(3) . ? P3 F18 1.556(3) . ? P3 F13 1.561(3) . ? P3 F14 1.563(3) . ? P3 F15 1.584(3) . ? P3 F17 1.594(3) . ? P3 F16 1.595(3) . ? P4 F21 1.562(3) . ? P4 F22 1.576(3) . ? P4 F24 1.585(3) . ? P4 F20 1.589(3) . ? P4 F23 1.595(3) . ? P4 F19 1.599(3) . ? N1 C1 1.345(4) . ? N1 C2 1.396(5) . ? N1 C12 1.472(5) . ? N2 C4 1.392(4) . ? N2 C1 1.392(4) . ? N2 C3 1.405(4) . ? N3 C8 1.355(4) . ? N3 C4 1.358(4) . ? N4 C11 1.391(4) . ? N4 C8 1.392(4) . ? N4 C9 1.399(4) . ? N5 C11 1.348(4) . ? N5 C10 1.402(5) . ? N5 C13 1.474(5) . ? N6 C14 1.341(4) . ? N6 C15 1.401(6) . ? N6 C25 1.464(5) . ? N7 C16 1.389(5) . ? N7 C17 1.393(5) . ? N7 C14 1.396(5) . ? N8 C17 1.350(5) . ? N8 C21 1.358(4) . ? N9 C22 1.383(5) . ? N9 C23 1.391(5) . ? N9 C21 1.393(5) . ? N10 C22 1.345(5) . ? N10 C24 1.403(6) . ? N10 C26 1.471(6) . ? N11 C27 1.351(4) . ? N11 C28 1.397(5) . ? N11 C38 1.476(4) . ? N12 C27 1.381(4) . ? N12 C29 1.388(4) . ? N12 C30 1.403(4) . ? N13 C30 1.351(4) . ? N13 C34 1.352(4) . ? N14 C35 1.381(5) . ? N14 C34 1.397(5) . ? N14 C36 1.398(5) . ? N15 C35 1.357(5) . ? N15 C37 1.402(6) . ? N15 C39 1.459(6) . ? N16 C40 1.346(5) . ? N16 C41 1.405(7) . ? N16 C51 1.459(7) . ? N17 C43 1.390(6) . ? N17 C40 1.397(5) . ? N17 C42 1.404(6) . ? N18 C47 1.347(5) . ? N18 C43 1.365(5) . ? N19 C48 1.393(5) . ? N19 C47 1.395(5) . ? N19 C49 1.397(5) . ? N20 C48 1.346(4) . ? N20 C50 1.393(5) . ? N20 C52 1.466(6) . ? N21 C53 1.04(2) . ? C2 C3 1.328(6) . ? C4 C5 1.389(5) . ? C5 C6 1.393(6) . ? C6 C7 1.380(6) . ? C7 C8 1.388(5) . ? C9 C10 1.325(6) . ? C15 C16 1.334(7) . ? C17 C18 1.389(6) . ? C18 C19 1.368(7) . ? C19 C20 1.380(7) . ? C20 C21 1.382(5) . ? C23 C24 1.322(7) . ? C28 C29 1.335(5) . ? C30 C31 1.384(5) . ? C31 C32 1.387(5) . ? C32 C33 1.395(6) . ? C33 C34 1.387(5) . ? C36 C37 1.333(7) . ? C41 C42 1.328(9) . ? C43 C44 1.384(7) . ? C44 C45 1.385(8) . ? C45 C46 1.385(8) . ? C46 C47 1.384(6) . ? C49 C50 1.330(7) . ? C53 C54 1.55(5) . ? C54 C54 1.24(4) 3_776 ? 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 N3 Fe1 N8 178.63(12) . . ? N3 Fe1 C11 79.17(13) . . ? N8 Fe1 C11 99.48(13) . . ? N3 Fe1 C14 100.72(14) . . ? N8 Fe1 C14 79.00(14) . . ? C11 Fe1 C14 90.39(13) . . ? N3 Fe1 C1 79.48(13) . . ? N8 Fe1 C1 101.88(13) . . ? C11 Fe1 C1 158.62(15) . . ? C14 Fe1 C1 94.51(13) . . ? N3 Fe1 C22 101.27(13) . . ? N8 Fe1 C22 79.03(14) . . ? C11 Fe1 C22 93.82(13) . . ? C14 Fe1 C22 158.01(16) . . ? C1 Fe1 C22 89.39(13) . . ? N18 Fe2 N13 178.86(12) . . ? N18 Fe2 C40 80.06(15) . . ? N13 Fe2 C40 99.68(15) . . ? N18 Fe2 C27 99.96(13) . . ? N13 Fe2 C27 78.94(12) . . ? C40 Fe2 C27 93.35(13) . . ? N18 Fe2 C48 78.97(14) . . ? N13 Fe2 C48 101.31(13) . . ? C40 Fe2 C48 158.99(17) . . ? C27 Fe2 C48 91.41(13) . . ? N18 Fe2 C35 102.23(14) . . ? N13 Fe2 C35 78.87(14) . . ? C40 Fe2 C35 90.41(14) . . ? C27 Fe2 C35 157.81(15) . . ? C48 Fe2 C35 92.86(14) . . ? F4 P1 F5 91.0(2) . . ? F4 P1 F3 179.3(2) . . ? F5 P1 F3 89.10(18) . . ? F4 P1 F6 90.27(17) . . ? F5 P1 F6 90.71(18) . . ? F3 P1 F6 90.43(16) . . ? F4 P1 F2 89.64(17) . . ? F5 P1 F2 179.36(19) . . ? F3 P1 F2 90.26(15) . . ? F6 P1 F2 89.21(15) . . ? F4 P1 F1 90.36(17) . . ? F5 P1 F1 90.5(2) . . ? F3 P1 F1 88.94(17) . . ? F6 P1 F1 178.64(18) . . ? F2 P1 F1 89.59(17) . . ? F10 P2 F8 88.6(2) . . ? F10 P2 F7 90.2(2) . . ? F8 P2 F7 90.4(2) . . ? F10 P2 F9 177.6(2) . . ? F8 P2 F9 89.07(18) . . ? F7 P2 F9 90.3(2) . . ? F10 P2 F11 92.2(2) . . ? F8 P2 F11 178.8(2) . . ? F7 P2 F11 90.4(2) . . ? F9 P2 F11 90.2(2) . . ? F10 P2 F12 90.6(2) . . ? F8 P2 F12 89.10(17) . . ? F7 P2 F12 179.0(2) . . ? F9 P2 F12 88.9(2) . . ? F11 P2 F12 90.01(19) . . ? F18 P3 F13 177.4(3) . . ? F18 P3 F14 91.2(2) . . ? F13 P3 F14 88.7(3) . . ? F18 P3 F15 92.6(2) . . ? F13 P3 F15 90.0(2) . . ? F14 P3 F15 92.7(2) . . ? F18 P3 F17 88.0(2) . . ? F13 P3 F17 89.4(2) . . ? F14 P3 F17 89.32(19) . . ? F15 P3 F17 177.9(2) . . ? F18 P3 F16 90.1(2) . . ? F13 P3 F16 89.8(2) . . ? F14 P3 F16 177.0(2) . . ? F15 P3 F16 89.88(18) . . ? F17 P3 F16 88.08(17) . . ? F21 P4 F22 179.2(2) . . ? F21 P4 F24 90.5(2) . . ? F22 P4 F24 90.3(2) . . ? F21 P4 F20 88.85(19) . . ? F22 P4 F20 91.3(2) . . ? F24 P4 F20 89.82(19) . . ? F21 P4 F23 91.3(2) . . ? F22 P4 F23 88.5(2) . . ? F24 P4 F23 89.77(19) . . ? F20 P4 F23 179.6(2) . . ? F21 P4 F19 90.0(2) . . ? F22 P4 F19 89.2(2) . . ? F24 P4 F19 179.5(2) . . ? F20 P4 F19 90.19(19) . . ? F23 P4 F19 90.21(19) . . ? C1 N1 C2 111.4(3) . . ? C1 N1 C12 124.3(3) . . ? C2 N1 C12 124.2(3) . . ? C4 N2 C1 117.4(3) . . ? C4 N2 C3 131.5(3) . . ? C1 N2 C3 111.1(3) . . ? C8 N3 C4 118.2(3) . . ? C8 N3 Fe1 121.2(2) . . ? C4 N3 Fe1 120.6(2) . . ? C11 N4 C8 117.5(3) . . ? C11 N4 C9 111.3(3) . . ? C8 N4 C9 131.1(3) . . ? C11 N5 C10 110.9(3) . . ? C11 N5 C13 125.0(3) . . ? C10 N5 C13 123.9(3) . . ? C14 N6 C15 111.0(4) . . ? C14 N6 C25 125.6(3) . . ? C15 N6 C25 123.4(4) . . ? C16 N7 C17 131.4(4) . . ? C16 N7 C14 111.3(4) . . ? C17 N7 C14 117.4(3) . . ? C17 N8 C21 118.0(3) . . ? C17 N8 Fe1 121.1(2) . . ? C21 N8 Fe1 120.8(3) . . ? C22 N9 C23 111.3(4) . . ? C22 N9 C21 117.8(3) . . ? C23 N9 C21 130.9(4) . . ? C22 N10 C24 110.7(4) . . ? C22 N10 C26 124.9(3) . . ? C24 N10 C26 124.4(4) . . ? C27 N11 C28 110.8(3) . . ? C27 N11 C38 125.0(3) . . ? C28 N11 C38 124.0(3) . . ? C27 N12 C29 112.2(3) . . ? C27 N12 C30 117.0(3) . . ? C29 N12 C30 130.8(3) . . ? C30 N13 C34 118.2(3) . . ? C30 N13 Fe2 120.9(2) . . ? C34 N13 Fe2 120.9(2) . . ? C35 N14 C34 117.5(3) . . ? C35 N14 C36 111.6(4) . . ? C34 N14 C36 130.9(4) . . ? C35 N15 C37 110.4(4) . . ? C35 N15 C39 125.4(4) . . ? C37 N15 C39 124.2(4) . . ? C40 N16 C41 110.7(5) . . ? C40 N16 C51 124.5(4) . . ? C41 N16 C51 124.8(5) . . ? C43 N17 C40 117.6(3) . . ? C43 N17 C42 131.2(5) . . ? C40 N17 C42 111.2(5) . . ? C47 N18 C43 119.0(4) . . ? C47 N18 Fe2 121.4(2) . . ? C43 N18 Fe2 119.6(3) . . ? C48 N19 C47 117.5(3) . . ? C48 N19 C49 110.7(4) . . ? C47 N19 C49 131.7(4) . . ? C48 N20 C50 111.3(4) . . ? C48 N20 C52 125.0(3) . . ? C50 N20 C52 123.6(4) . . ? N1 C1 N2 103.4(3) . . ? N1 C1 Fe1 143.4(3) . . ? N2 C1 Fe1 113.1(2) . . ? C3 C2 N1 108.4(3) . . ? C2 C3 N2 105.6(3) . . ? N3 C4 C5 122.6(3) . . ? N3 C4 N2 109.4(3) . . ? C5 C4 N2 128.0(3) . . ? C4 C5 C6 117.7(4) . . ? C7 C6 C5 120.7(4) . . ? C6 C7 C8 118.1(4) . . ? N3 C8 C7 122.7(3) . . ? N3 C8 N4 108.9(3) . . ? C7 C8 N4 128.4(3) . . ? C10 C9 N4 105.8(4) . . ? C9 C10 N5 108.5(3) . . ? N5 C11 N4 103.5(3) . . ? N5 C11 Fe1 143.4(3) . . ? N4 C11 Fe1 113.1(2) . . ? N6 C14 N7 103.7(3) . . ? N6 C14 Fe1 143.0(3) . . ? N7 C14 Fe1 113.3(2) . . ? C16 C15 N6 108.2(4) . . ? C15 C16 N7 105.9(4) . . ? N8 C17 C18 122.7(4) . . ? N8 C17 N7 109.1(3) . . ? C18 C17 N7 128.2(4) . . ? C19 C18 C17 117.7(5) . . ? C18 C19 C20 121.4(4) . . ? C19 C20 C21 117.8(4) . . ? N8 C21 C20 122.4(4) . . ? N8 C21 N9 109.0(3) . . ? C20 C21 N9 128.6(4) . . ? N10 C22 N9 103.7(3) . . ? N10 C22 Fe1 142.8(3) . . ? N9 C22 Fe1 113.4(3) . . ? C24 C23 N9 106.1(4) . . ? C23 C24 N10 108.2(4) . . ? N11 C27 N12 103.3(3) . . ? N11 C27 Fe2 142.7(3) . . ? N12 C27 Fe2 114.0(2) . . ? C29 C28 N11 108.4(3) . . ? C28 C29 N12 105.3(3) . . ? N13 C30 C31 122.9(3) . . ? N13 C30 N12 109.1(3) . . ? C31 C30 N12 128.0(3) . . ? C30 C31 C32 118.0(4) . . ? C31 C32 C33 120.5(4) . . ? C34 C33 C32 117.6(4) . . ? N13 C34 C33 122.9(4) . . ? N13 C34 N14 109.0(3) . . ? C33 C34 N14 128.1(3) . . ? N15 C35 N14 103.9(3) . . ? N15 C35 Fe2 142.4(3) . . ? N14 C35 Fe2 113.6(3) . . ? C37 C36 N14 105.7(4) . . ? C36 C37 N15 108.5(4) . . ? N16 C40 N17 103.7(3) . . ? N16 C40 Fe2 143.3(3) . . ? N17 C40 Fe2 112.9(3) . . ? C42 C41 N16 108.8(4) . . ? C41 C42 N17 105.5(5) . . ? N18 C43 C44 121.6(5) . . ? N18 C43 N17 109.8(3) . . ? C44 C43 N17 128.6(4) . . ? C43 C44 C45 117.7(5) . . ? C46 C45 C44 122.0(5) . . ? C47 C46 C45 116.8(5) . . ? N18 C47 C46 123.0(4) . . ? N18 C47 N19 108.8(3) . . ? C46 C47 N19 128.2(4) . . ? N20 C48 N19 103.6(3) . . ? N20 C48 Fe2 143.2(3) . . ? N19 C48 Fe2 113.2(2) . . ? C50 C49 N19 106.2(4) . . ? C49 C50 N20 108.1(4) . . ? N21 C53 C54 177(2) . . ? C54 C54 C53 95(3) 3_776 . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.711 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.092 _database_code_depnum_ccdc_archive 'CCDC 915795' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_fecab3 #TrackingRef 'web_deposit_cif_file_1_AndreFleckhaus_1355498170.fecab3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C38 H50 Fe N10), 4(F6 P), C4 H8 O, C4 O' _chemical_formula_sum 'C84 H108 F24 Fe2 N20 O2 P4' _chemical_formula_weight 2121.48 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' O O 0.0106 0.0060 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8044(5) _cell_length_b 20.5091(5) _cell_length_c 20.5285(6) _cell_angle_alpha 112.364(3) _cell_angle_beta 95.655(3) _cell_angle_gamma 90.690(3) _cell_volume 4954.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25213 _cell_measurement_theta_min 2.5136 _cell_measurement_theta_max 28.8539 _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_T_min 0.91553 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1829 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 108517 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 28.91 _reflns_number_total 23760 _reflns_number_gt 18223 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'Bruker SHELXTL (Sheldrick, 2008) and WinGX (Farrugia, 1999)' _computing_structure_refinement 'Bruker SHELXTL (Sheldrick, 2008) and WinGX (Farrugia, 1999)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0991P)^2^+4.7881P] 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 23760 _refine_ls_number_parameters 1225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1956 _refine_ls_wR_factor_gt 0.1778 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.005 _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 0.77281(3) 0.338016(18) 0.250082(18) 0.03043(10) Uani 1 1 d . . . Fe2 Fe 0.24978(3) 0.165541(18) 0.751394(19) 0.02962(10) Uani 1 1 d . . . P1 P 0.28036(10) 0.34899(6) 0.40559(7) 0.0760(3) Uani 1 1 d . . . P2 P 0.75125(7) 0.27247(5) 0.58805(5) 0.0496(2) Uani 1 1 d . . . P3 P 0.76059(8) 0.40768(5) 0.89173(5) 0.0577(2) Uani 1 1 d . . . P4 P 0.74634(8) 0.00117(6) 0.88416(7) 0.0653(3) Uani 1 1 d . . . F1 F 0.2301(5) 0.4040(3) 0.3811(3) 0.202(3) Uani 1 1 d . . . F2 F 0.3474(4) 0.3217(2) 0.3427(3) 0.185(2) Uani 1 1 d . . . F3 F 0.3685(4) 0.4100(2) 0.4449(3) 0.170(2) Uani 1 1 d . . . F4 F 0.3490(5) 0.3009(3) 0.4365(4) 0.206(2) Uani 1 1 d . . . F5 F 0.2208(4) 0.3791(2) 0.4721(2) 0.169(2) Uani 1 1 d . . . F6 F 0.2020(4) 0.2875(2) 0.3739(4) 0.239(4) Uani 1 1 d . . . F7 F 0.6747(3) 0.25566(17) 0.51817(18) 0.1306(14) Uani 1 1 d . . . F8 F 0.8166(3) 0.32890(18) 0.57081(18) 0.1318(14) Uani 1 1 d . . . F9 F 0.8194(2) 0.21052(16) 0.54309(19) 0.1191(12) Uani 1 1 d . . . F10 F 0.8328(3) 0.28776(17) 0.65560(16) 0.1095(10) Uani 1 1 d . . . F11 F 0.6857(3) 0.21518(18) 0.60436(18) 0.1114(11) Uani 1 1 d . . . F12 F 0.6817(3) 0.3324(2) 0.6310(2) 0.1483(16) Uani 1 1 d . . . F13 F 0.8537(3) 0.4074(3) 0.8471(3) 0.1575(18) Uani 1 1 d . . . F14 F 0.7196(6) 0.4751(3) 0.8862(3) 0.212(3) Uani 1 1 d . . . F15 F 0.6942(4) 0.3664(3) 0.8202(2) 0.192(2) Uani 1 1 d . . . F16 F 0.8190(5) 0.4496(3) 0.9651(2) 0.195(2) Uani 1 1 d . . . F17 F 0.8057(4) 0.3395(2) 0.8972(2) 0.176(2) Uani 1 1 d . . . F18 F 0.6705(3) 0.4032(3) 0.9366(2) 0.1420(15) Uani 1 1 d . . . F19 F 0.7705(3) 0.0461(3) 0.8401(3) 0.1525(16) Uani 1 1 d . . . F20 F 0.6601(3) -0.0434(3) 0.8272(2) 0.194(3) Uani 1 1 d . . . F21 F 0.6598(3) 0.0541(2) 0.9206(2) 0.1296(13) Uani 1 1 d . . . F22 F 0.7209(3) -0.0377(2) 0.9349(2) 0.1405(15) Uani 1 1 d . . . F23 F 0.8329(3) 0.0477(3) 0.9464(2) 0.1436(15) Uani 1 1 d . . . F24 F 0.8361(3) -0.0467(2) 0.8509(3) 0.174(2) Uani 1 1 d . . . N1 N 0.5949(2) 0.44490(12) 0.21842(13) 0.0403(5) Uani 1 1 d . . . N2 N 0.6912(2) 0.38248(12) 0.13943(12) 0.0402(5) Uani 1 1 d . . . N3 N 0.81468(18) 0.31073(12) 0.15562(12) 0.0350(5) Uani 1 1 d . . . N4 N 0.92932(19) 0.24209(13) 0.18668(12) 0.0398(5) Uani 1 1 d . . . N5 N 0.93801(18) 0.22851(12) 0.28581(12) 0.0374(5) Uani 1 1 d . . . N6 N 0.59481(19) 0.20161(13) 0.18748(13) 0.0415(5) Uani 1 1 d . . . N7 N 0.60643(19) 0.27659(13) 0.29579(13) 0.0404(5) Uani 1 1 d . . . N8 N 0.72853(18) 0.36678(11) 0.34431(11) 0.0342(5) Uani 1 1 d . . . N9 N 0.8583(2) 0.45293(12) 0.37720(12) 0.0403(5) Uani 1 1 d . . . N10 N 0.9619(2) 0.46867(13) 0.30759(14) 0.0443(6) Uani 1 1 d . . . N11 N 0.2557(2) 0.00734(13) 0.62033(15) 0.0512(6) Uani 1 1 d . . . N12 N 0.1102(2) 0.05685(13) 0.64888(13) 0.0434(6) Uani 1 1 d . . . N13 N 0.09761(17) 0.16291(12) 0.73633(13) 0.0362(5) Uani 1 1 d . . . N14 N 0.11059(19) 0.26936(13) 0.82690(14) 0.0420(5) Uani 1 1 d . . . N15 N 0.2571(2) 0.32441(13) 0.88233(14) 0.0443(6) Uani 1 1 d . . . N16 N 0.26006(19) 0.24290(13) 0.63515(13) 0.0396(5) Uani 1 1 d . . . N17 N 0.40043(18) 0.21821(13) 0.68585(13) 0.0383(5) Uani 1 1 d . . . N18 N 0.40215(17) 0.16788(11) 0.76639(12) 0.0330(5) Uani 1 1 d . . . N19 N 0.37784(17) 0.11739(12) 0.84459(13) 0.0365(5) Uani 1 1 d . . . N20 N 0.22800(18) 0.09083(12) 0.86950(13) 0.0372(5) Uani 1 1 d . . . O1 O 0.1890(4) 0.2322(3) 0.0789(3) 0.1401(17) Uani 1 1 d . . . O2 O 0.7880(10) 0.9503(5) 0.5896(6) 0.247(5) Uani 1 1 d . . . C1 C 0.6739(2) 0.39826(13) 0.20976(14) 0.0354(6) Uani 1 1 d . . . C2 C 0.5655(3) 0.45510(17) 0.15540(18) 0.0513(8) Uani 1 1 d . . . H2 H 0.5132 0.4838 0.1489 0.062 Uiso 1 1 calc R . . C3 C 0.6253(3) 0.41668(17) 0.10628(17) 0.0502(8) Uani 1 1 d . . . H3 H 0.6233 0.4135 0.0598 0.060 Uiso 1 1 calc R . . C4 C 0.7690(2) 0.33670(15) 0.10935(15) 0.0412(6) Uani 1 1 d . . . C5 C 0.7960(3) 0.31909(19) 0.04103(17) 0.0571(9) Uani 1 1 d . . . H5 H 0.7632 0.3384 0.0106 0.069 Uiso 1 1 calc R . . C6 C 0.8741(3) 0.2712(2) 0.02017(18) 0.0664(10) Uani 1 1 d . . . H6 H 0.8940 0.2580 -0.0253 0.080 Uiso 1 1 calc R . . C7 C 0.9226(3) 0.2430(2) 0.06595(18) 0.0606(9) Uani 1 1 d . . . H7 H 0.9747 0.2108 0.0523 0.073 Uiso 1 1 calc R . . C8 C 0.8901(2) 0.26483(16) 0.13338(15) 0.0420(6) Uani 1 1 d . . . C9 C 0.8856(2) 0.26590(13) 0.25086(14) 0.0339(5) Uani 1 1 d . . . C10 C 1.0044(3) 0.19285(18) 0.18254(18) 0.0513(8) Uani 1 1 d . . . H10 H 1.0428 0.1703 0.1448 0.062 Uiso 1 1 calc R . . C11 C 1.0097(3) 0.18467(18) 0.24406(19) 0.0524(8) Uani 1 1 d . . . H11 H 1.0536 0.1549 0.2572 0.063 Uiso 1 1 calc R . . C12 C 0.5488(3) 0.48879(16) 0.28671(18) 0.0480(7) Uani 1 1 d . . . C13 C 0.9186(3) 0.22729(17) 0.35692(16) 0.0462(7) Uani 1 1 d . . . C14 C 0.4654(4) 0.5358(2) 0.2720(2) 0.0757(12) Uani 1 1 d . . . H14A H 0.4967 0.5669 0.2534 0.114 Uiso 1 1 calc R . . H14B H 0.4373 0.5632 0.3153 0.114 Uiso 1 1 calc R . . H14C H 0.4098 0.5069 0.2381 0.114 Uiso 1 1 calc R . . C15 C 0.4988(4) 0.4403(2) 0.3159(3) 0.0854(15) Uani 1 1 d . . . H15A H 0.4426 0.4118 0.2822 0.128 Uiso 1 1 calc R . . H15B H 0.4715 0.4678 0.3595 0.128 Uiso 1 1 calc R . . H15C H 0.5505 0.4102 0.3247 0.128 Uiso 1 1 calc R . . C16 C 0.6387(4) 0.5357(2) 0.3373(2) 0.0784(13) Uani 1 1 d . . . H16A H 0.6678 0.5655 0.3164 0.118 Uiso 1 1 calc R . . H16B H 0.6921 0.5068 0.3463 0.118 Uiso 1 1 calc R . . H16C H 0.6131 0.5643 0.3810 0.118 Uiso 1 1 calc R . . C17 C 0.8073(3) 0.1953(2) 0.3495(2) 0.0654(10) Uani 1 1 d . . . H17A H 0.8015 0.1484 0.3137 0.098 Uiso 1 1 calc R . . H17B H 0.7575 0.2239 0.3362 0.098 Uiso 1 1 calc R . . H17C H 0.7932 0.1936 0.3939 0.098 Uiso 1 1 calc R . . C18 C 0.9966(3) 0.18029(19) 0.3778(2) 0.0590(9) Uani 1 1 d . . . H18A H 1.0669 0.1996 0.3827 0.089 Uiso 1 1 calc R . . H18B H 0.9897 0.1335 0.3417 0.089 Uiso 1 1 calc R . . H18C H 0.9817 0.1784 0.4220 0.089 Uiso 1 1 calc R . . C19 C 0.9360(3) 0.3025(2) 0.41306(18) 0.0598(9) Uani 1 1 d . . . H19A H 1.0069 0.3195 0.4152 0.090 Uiso 1 1 calc R . . H19B H 0.9238 0.3025 0.4584 0.090 Uiso 1 1 calc R . . H19C H 0.8881 0.3328 0.4008 0.090 Uiso 1 1 calc R . . C20 C 0.6516(2) 0.26244(14) 0.23315(14) 0.0349(5) Uani 1 1 d . . . C21 C 0.5201(3) 0.18069(18) 0.22258(19) 0.0550(8) Uani 1 1 d . . . H21 H 0.4738 0.1412 0.2025 0.066 Uiso 1 1 calc R . . C22 C 0.5270(3) 0.22731(18) 0.2897(2) 0.0556(8) Uani 1 1 d . . . H22 H 0.4870 0.2268 0.3250 0.067 Uiso 1 1 calc R . . C23 C 0.6494(2) 0.33205(15) 0.35751(15) 0.0403(6) Uani 1 1 d . . . C24 C 0.6157(3) 0.35015(19) 0.42474(18) 0.0538(8) Uani 1 1 d . . . H24 H 0.5610 0.3245 0.4322 0.065 Uiso 1 1 calc R . . C25 C 0.6670(3) 0.4076(2) 0.47962(17) 0.0583(9) Uani 1 1 d . . . H25 H 0.6465 0.4212 0.5249 0.070 Uiso 1 1 calc R . . C26 C 0.7489(3) 0.44526(17) 0.46768(16) 0.0523(8) Uani 1 1 d . . . H26 H 0.7837 0.4840 0.5042 0.063 Uiso 1 1 calc R . . C27 C 0.7769(2) 0.42271(14) 0.39891(15) 0.0394(6) Uani 1 1 d . . . C28 C 0.8792(2) 0.42496(14) 0.30718(14) 0.0369(6) Uani 1 1 d . . . C29 C 0.9242(3) 0.51143(17) 0.41887(18) 0.0527(8) Uani 1 1 d . . . H29 H 0.9236 0.5384 0.4669 0.063 Uiso 1 1 calc R . . C30 C 0.9882(3) 0.52076(18) 0.37561(19) 0.0561(8) Uani 1 1 d . . . H30 H 1.0416 0.5559 0.3883 0.067 Uiso 1 1 calc R . . C31 C 0.6130(3) 0.15683(16) 0.11239(17) 0.0467(7) Uani 1 1 d . . . C32 C 1.0216(3) 0.46606(18) 0.24650(19) 0.0561(8) Uani 1 1 d . . . C33 C 0.6009(4) 0.2016(2) 0.06736(19) 0.0686(11) Uani 1 1 d . . . H33A H 0.5314 0.2187 0.0682 0.103 Uiso 1 1 calc R . . H33B H 0.6121 0.1733 0.0194 0.103 Uiso 1 1 calc R . . H33C H 0.6516 0.2409 0.0862 0.103 Uiso 1 1 calc R . . C34 C 0.7214(3) 0.1266(2) 0.1148(2) 0.0678(11) Uani 1 1 d . . . H34A H 0.7233 0.0993 0.1438 0.102 Uiso 1 1 calc R . . H34B H 0.7742 0.1647 0.1345 0.102 Uiso 1 1 calc R . . H34C H 0.7347 0.0971 0.0677 0.102 Uiso 1 1 calc R . . C35 C 0.5316(3) 0.09420(18) 0.0799(2) 0.0618(9) Uani 1 1 d . . . H35A H 0.5376 0.0651 0.1072 0.093 Uiso 1 1 calc R . . H35B H 0.5442 0.0668 0.0320 0.093 Uiso 1 1 calc R . . H35C H 0.4623 0.1115 0.0802 0.093 Uiso 1 1 calc R . . C36 C 1.0697(4) 0.3943(2) 0.2178(3) 0.0883(15) Uani 1 1 d . . . H36A H 1.1171 0.3890 0.2546 0.132 Uiso 1 1 calc R . . H36B H 1.1075 0.3911 0.1787 0.132 Uiso 1 1 calc R . . H36C H 1.0149 0.3575 0.2022 0.132 Uiso 1 1 calc R . . C37 C 1.1123(4) 0.5223(2) 0.2722(3) 0.0857(14) Uani 1 1 d . . . H37A H 1.1601 0.5138 0.3068 0.129 Uiso 1 1 calc R . . H37B H 1.0850 0.5682 0.2932 0.129 Uiso 1 1 calc R . . H37C H 1.1486 0.5202 0.2328 0.129 Uiso 1 1 calc R . . C38 C 0.9456(4) 0.4789(3) 0.1918(2) 0.0822(13) Uani 1 1 d . . . H38A H 0.9179 0.5247 0.2127 0.123 Uiso 1 1 calc R . . H38B H 0.8890 0.4434 0.1759 0.123 Uiso 1 1 calc R . . H38C H 0.9816 0.4768 0.1523 0.123 Uiso 1 1 calc R . . C39 C 0.2177(2) 0.06781(15) 0.66740(16) 0.0399(6) Uani 1 1 d . . . C40 C 0.1719(3) -0.03756(19) 0.5753(2) 0.0666(10) Uani 1 1 d . . . H40 H 0.1784 -0.0811 0.5392 0.080 Uiso 1 1 calc R . . C41 C 0.0824(3) -0.00756(19) 0.5929(2) 0.0634(10) Uani 1 1 d . . . H41 H 0.0150 -0.0257 0.5721 0.076 Uiso 1 1 calc R . . C42 C 0.0432(2) 0.10807(17) 0.68546(17) 0.0444(7) Uani 1 1 d . . . C43 C -0.0658(3) 0.1052(2) 0.6709(2) 0.0574(9) Uani 1 1 d . . . H43 H -0.1018 0.0660 0.6358 0.069 Uiso 1 1 calc R . . C44 C -0.1180(3) 0.1627(2) 0.7105(2) 0.0655(10) Uani 1 1 d . . . H44 H -0.1905 0.1627 0.7009 0.079 Uiso 1 1 calc R . . C45 C -0.0657(3) 0.2198(2) 0.7638(2) 0.0570(9) Uani 1 1 d . . . H45 H -0.1010 0.2585 0.7907 0.068 Uiso 1 1 calc R . . C46 C 0.0434(2) 0.21711(16) 0.77554(16) 0.0419(6) Uani 1 1 d . . . C47 C 0.2190(2) 0.26223(14) 0.82864(15) 0.0363(6) Uani 1 1 d . . . C48 C 0.0840(3) 0.33293(18) 0.8773(2) 0.0579(9) Uani 1 1 d . . . H48 H 0.0168 0.3484 0.8855 0.070 Uiso 1 1 calc R . . C49 C 0.1735(3) 0.36660(19) 0.9109(2) 0.0618(9) Uani 1 1 d . . . H49 H 0.1807 0.4109 0.9475 0.074 Uiso 1 1 calc R . . C50 C 0.3687(3) -0.0131(2) 0.6156(2) 0.0720(12) Uani 1 1 d . . . C51 C 0.3716(3) 0.35168(17) 0.90304(19) 0.0533(8) Uani 1 1 d . . . C52 C 0.4310(4) 0.0421(3) 0.6010(3) 0.109(2) Uani 1 1 d . . . H52A H 0.4020 0.0443 0.5570 0.164 Uiso 1 1 calc R . . H52B H 0.5030 0.0297 0.5980 0.164 Uiso 1 1 calc R . . H52C H 0.4276 0.0873 0.6387 0.164 Uiso 1 1 calc R . . C53 C 0.3746(5) -0.0845(3) 0.5533(3) 0.109(2) Uani 1 1 d . . . H53A H 0.3356 -0.1205 0.5613 0.164 Uiso 1 1 calc R . . H53B H 0.4467 -0.0965 0.5499 0.164 Uiso 1 1 calc R . . H53C H 0.3452 -0.0809 0.5100 0.164 Uiso 1 1 calc R . . C54 C 0.4093(4) -0.0204(3) 0.6851(3) 0.0999(18) Uani 1 1 d . . . H54A H 0.3668 -0.0560 0.6914 0.150 Uiso 1 1 calc R . . H54B H 0.4056 0.0238 0.7240 0.150 Uiso 1 1 calc R . . H54C H 0.4809 -0.0338 0.6833 0.150 Uiso 1 1 calc R . . C55 C 0.4096(3) 0.3618(2) 0.8391(2) 0.0721(11) Uani 1 1 d . . . H55A H 0.3671 0.3949 0.8274 0.108 Uiso 1 1 calc R . . H55B H 0.4039 0.3173 0.7995 0.108 Uiso 1 1 calc R . . H55C H 0.4816 0.3795 0.8503 0.108 Uiso 1 1 calc R . . C56 C 0.3801(4) 0.4239(2) 0.9660(2) 0.0781(12) Uani 1 1 d . . . H56A H 0.3565 0.4182 1.0066 0.117 Uiso 1 1 calc R . . H56B H 0.3371 0.4564 0.9536 0.117 Uiso 1 1 calc R . . H56C H 0.4519 0.4420 0.9770 0.117 Uiso 1 1 calc R . . C57 C 0.4344(3) 0.2998(2) 0.9262(2) 0.0673(10) Uani 1 1 d . . . H57A H 0.4067 0.2959 0.9664 0.101 Uiso 1 1 calc R . . H57B H 0.5068 0.3165 0.9387 0.101 Uiso 1 1 calc R . . H57C H 0.4291 0.2543 0.8879 0.101 Uiso 1 1 calc R . . C58 C 0.2915(2) 0.21339(14) 0.68336(14) 0.0335(5) Uani 1 1 d . . . C59 C 0.3474(3) 0.26319(19) 0.60913(18) 0.0520(8) Uani 1 1 d . . . H59 H 0.3445 0.2837 0.5757 0.062 Uiso 1 1 calc R . . C60 C 0.4342(3) 0.24829(18) 0.64020(18) 0.0509(8) Uani 1 1 d . . . H60 H 0.5031 0.2562 0.6332 0.061 Uiso 1 1 calc R . . C61 C 0.4626(2) 0.19598(15) 0.73259(15) 0.0381(6) Uani 1 1 d . . . C62 C 0.5719(2) 0.20181(19) 0.74394(19) 0.0526(8) Uani 1 1 d . . . H62 H 0.6113 0.2228 0.7208 0.063 Uiso 1 1 calc R . . C63 C 0.6191(2) 0.1750(2) 0.7913(2) 0.0585(9) Uani 1 1 d . . . H63 H 0.6920 0.1777 0.8000 0.070 Uiso 1 1 calc R . . C64 C 0.5594(2) 0.14396(19) 0.82595(19) 0.0499(7) Uani 1 1 d . . . H64 H 0.5908 0.1248 0.8570 0.060 Uiso 1 1 calc R . . C65 C 0.4511(2) 0.14287(15) 0.81217(16) 0.0372(6) Uani 1 1 d . . . C66 C 0.2709(2) 0.11968(13) 0.82660(14) 0.0329(5) Uani 1 1 d . . . C67 C 0.3998(2) 0.08916(17) 0.89584(18) 0.0471(7) Uani 1 1 d . . . H67 H 0.4657 0.0828 0.9153 0.056 Uiso 1 1 calc R . . C68 C 0.3066(2) 0.07311(17) 0.91136(17) 0.0471(7) Uani 1 1 d . . . H68 H 0.2957 0.0535 0.9444 0.057 Uiso 1 1 calc R . . C69 C 0.1491(3) 0.25803(19) 0.61387(19) 0.0512(8) Uani 1 1 d . . . C70 C 0.1127(2) 0.07279(16) 0.87075(17) 0.0424(6) Uani 1 1 d . . . C71 C 0.1074(3) 0.3104(2) 0.6799(2) 0.0723(11) Uani 1 1 d . . . H71A H 0.1519 0.3529 0.6987 0.108 Uiso 1 1 calc R . . H71B H 0.1066 0.2900 0.7149 0.108 Uiso 1 1 calc R . . H71C H 0.0373 0.3214 0.6678 0.108 Uiso 1 1 calc R . . C72 C 0.0842(3) 0.1880(2) 0.5791(2) 0.0719(12) Uani 1 1 d . . . H72A H 0.1152 0.1580 0.5381 0.108 Uiso 1 1 calc R . . H72B H 0.0137 0.1967 0.5650 0.108 Uiso 1 1 calc R . . H72C H 0.0830 0.1654 0.6122 0.108 Uiso 1 1 calc R . . C73 C 0.1496(3) 0.2929(2) 0.5595(2) 0.0650(10) Uani 1 1 d . . . H73A H 0.1901 0.3370 0.5803 0.097 Uiso 1 1 calc R . . H73B H 0.0788 0.3011 0.5455 0.097 Uiso 1 1 calc R . . H73C H 0.1802 0.2623 0.5186 0.097 Uiso 1 1 calc R . . C74 C 0.0725(3) 0.0174(2) 0.7988(2) 0.0665(10) Uani 1 1 d . . . H74A H 0.1128 -0.0237 0.7895 0.100 Uiso 1 1 calc R . . H74B H 0.0791 0.0360 0.7629 0.100 Uiso 1 1 calc R . . H74C H -0.0001 0.0048 0.7985 0.100 Uiso 1 1 calc R . . C75 C 0.1013(3) 0.0429(2) 0.9277(2) 0.0677(11) Uani 1 1 d . . . H75A H 0.1267 0.0778 0.9734 0.102 Uiso 1 1 calc R . . H75B H 0.1414 0.0016 0.9183 0.102 Uiso 1 1 calc R . . H75C H 0.0286 0.0304 0.9272 0.102 Uiso 1 1 calc R . . C76 C 0.0525(3) 0.1402(2) 0.8898(2) 0.0622(10) Uani 1 1 d . . . H76A H 0.0810 0.1734 0.9357 0.093 Uiso 1 1 calc R . . H76B H -0.0203 0.1292 0.8907 0.093 Uiso 1 1 calc R . . H76C H 0.0589 0.1604 0.8551 0.093 Uiso 1 1 calc R . . C77 C 0.2651(6) 0.2265(5) 0.1264(7) 0.191(5) Uani 1 1 d . . . H77A H 0.3071 0.1869 0.1031 0.229 Uiso 1 1 calc R . . H77B H 0.2334 0.2174 0.1634 0.229 Uiso 1 1 calc R . . C78 C 0.3311(7) 0.2898(5) 0.1573(5) 0.147(3) Uani 1 1 d . . . H78A H 0.4044 0.2788 0.1606 0.176 Uiso 1 1 calc R . . H78B H 0.3136 0.3179 0.2044 0.176 Uiso 1 1 calc R . . C79 C 0.3116(6) 0.3285(4) 0.1099(4) 0.130(2) Uani 1 1 d . . . H79A H 0.3737 0.3320 0.0877 0.156 Uiso 1 1 calc R . . H79B H 0.2887 0.3755 0.1352 0.156 Uiso 1 1 calc R . . C80 C 0.2245(7) 0.2818(5) 0.0559(4) 0.151(3) Uani 1 1 d . . . H80A H 0.1673 0.3104 0.0500 0.181 Uiso 1 1 calc R . . H80B H 0.2511 0.2589 0.0104 0.181 Uiso 1 1 calc R . . C81 C 0.708(2) 0.9153(15) 0.5501(9) 0.401(19) Uani 1 1 d . . . C82 C 0.711(3) 0.891(2) 0.6040(18) 0.50(3) Uani 1 1 d . . . C83 C 0.7019(9) 0.8887(6) 0.6566(6) 0.158(4) Uani 1 1 d . . . C84 C 0.760(2) 0.9592(13) 0.6624(10) 0.382(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0347(2) 0.03121(19) 0.02700(18) 0.01274(14) 0.00445(14) 0.00194(14) Fe2 0.02368(18) 0.03225(19) 0.0351(2) 0.01528(15) 0.00345(14) 0.00186(13) P1 0.0850(8) 0.0612(6) 0.0888(8) 0.0270(6) 0.0484(7) 0.0087(5) P2 0.0500(5) 0.0543(5) 0.0444(4) 0.0178(4) 0.0088(4) 0.0059(4) P3 0.0646(6) 0.0653(6) 0.0515(5) 0.0291(4) 0.0163(4) 0.0112(4) P4 0.0433(5) 0.0760(7) 0.0863(7) 0.0403(6) 0.0152(5) 0.0030(4) F1 0.294(7) 0.179(5) 0.140(4) 0.071(3) 0.008(4) 0.112(5) F2 0.238(5) 0.137(3) 0.177(4) 0.026(3) 0.150(4) 0.028(3) F3 0.132(3) 0.127(3) 0.214(5) 0.018(3) 0.049(3) -0.027(3) F4 0.203(5) 0.180(5) 0.287(7) 0.148(5) 0.026(5) 0.056(4) F5 0.245(5) 0.104(2) 0.176(4) 0.041(3) 0.158(4) 0.014(3) F6 0.122(3) 0.128(3) 0.331(8) -0.073(4) 0.067(4) -0.054(3) F7 0.174(3) 0.094(2) 0.104(2) 0.0383(18) -0.073(2) -0.012(2) F8 0.179(4) 0.110(2) 0.108(2) 0.046(2) 0.011(2) -0.063(2) F9 0.0819(19) 0.093(2) 0.138(3) -0.0113(19) 0.0359(19) 0.0203(16) F10 0.120(2) 0.107(2) 0.0872(19) 0.0334(17) -0.0385(18) -0.0079(19) F11 0.111(2) 0.122(2) 0.118(2) 0.059(2) 0.0351(19) -0.0258(19) F12 0.115(3) 0.113(3) 0.166(4) -0.010(2) 0.034(2) 0.054(2) F13 0.130(3) 0.216(4) 0.211(4) 0.155(4) 0.098(3) 0.054(3) F14 0.384(8) 0.164(4) 0.157(4) 0.111(3) 0.116(5) 0.168(5) F15 0.200(5) 0.252(6) 0.076(2) 0.017(3) -0.018(3) -0.012(4) F16 0.211(5) 0.189(5) 0.129(3) 0.025(3) -0.078(3) -0.056(4) F17 0.296(6) 0.153(3) 0.161(3) 0.117(3) 0.152(4) 0.141(4) F18 0.113(3) 0.218(4) 0.138(3) 0.100(3) 0.071(2) 0.041(3) F19 0.139(3) 0.200(4) 0.186(4) 0.142(4) 0.049(3) 0.001(3) F20 0.139(3) 0.292(6) 0.098(3) 0.024(3) -0.008(2) -0.128(4) F21 0.107(2) 0.182(4) 0.125(3) 0.078(3) 0.041(2) 0.075(3) F22 0.116(3) 0.177(4) 0.186(4) 0.138(3) 0.000(3) -0.017(3) F23 0.085(2) 0.191(4) 0.132(3) 0.042(3) -0.002(2) -0.035(2) F24 0.117(3) 0.136(3) 0.244(5) 0.029(3) 0.074(3) 0.051(3) N1 0.0437(13) 0.0363(12) 0.0436(13) 0.0188(10) 0.0038(11) 0.0044(10) N2 0.0504(14) 0.0392(12) 0.0358(12) 0.0201(10) 0.0026(10) 0.0055(10) N3 0.0405(12) 0.0359(11) 0.0316(11) 0.0157(9) 0.0066(9) 0.0031(9) N4 0.0409(13) 0.0435(13) 0.0361(12) 0.0154(10) 0.0078(10) 0.0085(10) N5 0.0360(12) 0.0398(12) 0.0393(12) 0.0188(10) 0.0029(10) 0.0047(9) N6 0.0374(12) 0.0400(12) 0.0454(13) 0.0149(11) 0.0026(10) -0.0017(10) N7 0.0399(13) 0.0418(12) 0.0431(13) 0.0190(11) 0.0107(10) 0.0002(10) N8 0.0402(12) 0.0346(11) 0.0302(11) 0.0147(9) 0.0053(9) 0.0046(9) N9 0.0490(14) 0.0335(11) 0.0341(12) 0.0086(9) 0.0024(10) 0.0006(10) N10 0.0480(14) 0.0365(12) 0.0469(14) 0.0150(11) 0.0040(11) -0.0040(10) N11 0.0571(16) 0.0378(13) 0.0515(15) 0.0084(11) 0.0094(13) -0.0029(12) N12 0.0432(14) 0.0413(13) 0.0433(13) 0.0157(11) -0.0035(11) -0.0093(10) N13 0.0284(11) 0.0438(12) 0.0424(12) 0.0235(10) 0.0028(9) 0.0006(9) N14 0.0363(12) 0.0460(13) 0.0494(14) 0.0225(11) 0.0125(11) 0.0150(10) N15 0.0468(14) 0.0358(12) 0.0483(14) 0.0130(11) 0.0088(11) 0.0067(10) N16 0.0375(12) 0.0453(13) 0.0422(13) 0.0241(11) 0.0037(10) -0.0005(10) N17 0.0310(11) 0.0462(13) 0.0453(13) 0.0250(11) 0.0083(10) 0.0014(9) N18 0.0266(10) 0.0349(11) 0.0402(12) 0.0169(9) 0.0055(9) 0.0030(8) N19 0.0290(11) 0.0412(12) 0.0457(13) 0.0244(10) 0.0019(10) 0.0041(9) N20 0.0344(12) 0.0409(12) 0.0426(13) 0.0230(10) 0.0052(10) 0.0023(9) O1 0.109(4) 0.147(4) 0.170(5) 0.073(4) -0.004(3) -0.028(3) O2 0.381(15) 0.189(7) 0.159(7) 0.052(6) 0.044(8) -0.084(8) C1 0.0394(14) 0.0308(12) 0.0362(13) 0.0136(11) 0.0025(11) -0.0003(10) C2 0.061(2) 0.0474(17) 0.0504(18) 0.0266(15) -0.0036(15) 0.0106(15) C3 0.067(2) 0.0485(17) 0.0412(16) 0.0257(14) -0.0018(15) 0.0083(15) C4 0.0519(17) 0.0408(14) 0.0339(14) 0.0174(12) 0.0051(12) 0.0027(12) C5 0.080(3) 0.064(2) 0.0375(16) 0.0290(16) 0.0109(16) 0.0138(18) C6 0.086(3) 0.083(3) 0.0368(17) 0.0255(18) 0.0258(18) 0.020(2) C7 0.073(2) 0.072(2) 0.0450(18) 0.0253(17) 0.0262(17) 0.0287(19) C8 0.0471(16) 0.0453(15) 0.0356(14) 0.0159(12) 0.0114(12) 0.0073(12) C9 0.0337(13) 0.0336(12) 0.0348(13) 0.0131(11) 0.0061(10) -0.0012(10) C10 0.0461(17) 0.0582(19) 0.0525(18) 0.0212(15) 0.0176(15) 0.0181(14) C11 0.0462(18) 0.0544(18) 0.062(2) 0.0261(16) 0.0118(15) 0.0179(14) C12 0.0519(18) 0.0441(16) 0.0529(18) 0.0223(14) 0.0127(14) 0.0145(13) C13 0.0473(17) 0.0560(18) 0.0425(16) 0.0282(14) 0.0002(13) 0.0044(14) C14 0.081(3) 0.080(3) 0.079(3) 0.041(2) 0.023(2) 0.045(2) C15 0.095(3) 0.081(3) 0.110(4) 0.058(3) 0.059(3) 0.032(3) C16 0.078(3) 0.066(2) 0.066(3) -0.001(2) 0.001(2) 0.018(2) C17 0.051(2) 0.095(3) 0.071(2) 0.056(2) 0.0074(18) -0.0013(19) C18 0.067(2) 0.059(2) 0.060(2) 0.0355(18) -0.0037(18) 0.0096(17) C19 0.072(2) 0.065(2) 0.0434(18) 0.0219(16) 0.0033(16) 0.0190(18) C20 0.0344(13) 0.0346(13) 0.0378(14) 0.0163(11) 0.0035(11) 0.0036(10) C21 0.0460(18) 0.0525(18) 0.064(2) 0.0202(16) 0.0052(15) -0.0140(14) C22 0.0491(18) 0.0569(19) 0.066(2) 0.0261(17) 0.0186(16) -0.0053(15) C23 0.0442(16) 0.0424(15) 0.0375(14) 0.0177(12) 0.0093(12) 0.0043(12) C24 0.064(2) 0.0589(19) 0.0468(18) 0.0252(16) 0.0233(16) 0.0070(16) C25 0.076(2) 0.067(2) 0.0362(16) 0.0203(16) 0.0225(16) 0.0145(18) C26 0.074(2) 0.0472(17) 0.0328(15) 0.0109(13) 0.0091(15) 0.0065(15) C27 0.0494(16) 0.0348(13) 0.0329(13) 0.0115(11) 0.0049(12) 0.0067(12) C28 0.0434(15) 0.0335(13) 0.0347(13) 0.0142(11) 0.0031(11) 0.0036(11) C29 0.062(2) 0.0410(16) 0.0419(16) 0.0036(13) -0.0046(15) -0.0032(14) C30 0.058(2) 0.0453(17) 0.056(2) 0.0119(15) -0.0017(16) -0.0130(15) C31 0.0476(17) 0.0405(15) 0.0452(16) 0.0107(13) -0.0019(13) -0.0032(13) C32 0.059(2) 0.0515(18) 0.059(2) 0.0211(16) 0.0137(16) -0.0116(15) C33 0.095(3) 0.057(2) 0.0469(19) 0.0171(17) -0.0058(19) -0.019(2) C34 0.054(2) 0.061(2) 0.067(2) 0.0012(18) 0.0035(18) 0.0067(17) C35 0.062(2) 0.0486(18) 0.063(2) 0.0128(16) -0.0067(18) -0.0139(16) C36 0.084(3) 0.065(3) 0.114(4) 0.024(3) 0.053(3) 0.004(2) C37 0.083(3) 0.081(3) 0.088(3) 0.025(2) 0.018(2) -0.035(2) C38 0.096(3) 0.093(3) 0.068(3) 0.046(2) 0.003(2) -0.019(3) C39 0.0423(15) 0.0363(13) 0.0425(15) 0.0164(12) 0.0064(12) -0.0023(11) C40 0.077(3) 0.0444(18) 0.062(2) 0.0033(16) 0.003(2) -0.0129(18) C41 0.061(2) 0.0528(19) 0.064(2) 0.0136(17) -0.0112(18) -0.0188(17) C42 0.0358(15) 0.0510(16) 0.0510(17) 0.0265(14) -0.0009(13) -0.0069(12) C43 0.0353(16) 0.072(2) 0.067(2) 0.0330(19) -0.0086(15) -0.0148(15) C44 0.0268(15) 0.102(3) 0.082(3) 0.053(2) -0.0010(16) 0.0015(17) C45 0.0331(16) 0.076(2) 0.073(2) 0.039(2) 0.0119(16) 0.0150(15) C46 0.0318(14) 0.0531(17) 0.0497(16) 0.0282(14) 0.0097(12) 0.0099(12) C47 0.0356(14) 0.0391(14) 0.0398(14) 0.0200(12) 0.0078(11) 0.0084(11) C48 0.055(2) 0.0530(19) 0.066(2) 0.0182(17) 0.0221(17) 0.0242(16) C49 0.069(2) 0.0455(18) 0.063(2) 0.0080(16) 0.0204(19) 0.0180(17) C50 0.066(2) 0.0474(19) 0.086(3) 0.0025(19) 0.027(2) 0.0089(17) C51 0.0533(19) 0.0412(16) 0.0567(19) 0.0107(14) -0.0002(15) -0.0047(14) C52 0.093(4) 0.068(3) 0.143(5) 0.002(3) 0.065(4) -0.008(3) C53 0.102(4) 0.062(3) 0.120(4) -0.020(3) 0.035(3) 0.009(3) C54 0.080(3) 0.079(3) 0.118(4) 0.015(3) -0.005(3) 0.034(3) C55 0.073(3) 0.064(2) 0.076(3) 0.021(2) 0.013(2) -0.017(2) C56 0.092(3) 0.0441(19) 0.074(3) -0.0019(18) -0.002(2) -0.0038(19) C57 0.062(2) 0.055(2) 0.073(3) 0.0155(19) -0.0089(19) 0.0008(17) C58 0.0301(13) 0.0349(13) 0.0364(13) 0.0147(11) 0.0034(10) 0.0012(10) C59 0.0502(18) 0.066(2) 0.0547(19) 0.0389(17) 0.0116(15) -0.0013(15) C60 0.0427(17) 0.064(2) 0.061(2) 0.0378(17) 0.0153(15) -0.0008(14) C61 0.0307(13) 0.0429(14) 0.0449(15) 0.0208(12) 0.0072(11) 0.0010(11) C62 0.0312(15) 0.072(2) 0.067(2) 0.0395(18) 0.0094(14) -0.0007(14) C63 0.0251(14) 0.087(3) 0.075(2) 0.044(2) 0.0055(14) 0.0046(15) C64 0.0295(14) 0.067(2) 0.062(2) 0.0366(17) 0.0008(13) 0.0085(13) C65 0.0292(13) 0.0410(14) 0.0469(15) 0.0230(12) 0.0044(11) 0.0047(10) C66 0.0297(12) 0.0309(12) 0.0389(14) 0.0139(11) 0.0050(10) 0.0026(10) C67 0.0377(15) 0.0589(18) 0.0565(18) 0.0377(16) -0.0038(13) 0.0035(13) C68 0.0433(16) 0.0583(18) 0.0522(18) 0.0362(15) 0.0006(14) 0.0011(14) C69 0.0431(17) 0.066(2) 0.0566(19) 0.0390(17) -0.0019(14) 0.0035(15) C70 0.0342(14) 0.0510(16) 0.0496(16) 0.0270(14) 0.0077(12) -0.0003(12) C71 0.063(2) 0.094(3) 0.080(3) 0.054(2) 0.016(2) 0.033(2) C72 0.057(2) 0.088(3) 0.084(3) 0.055(2) -0.021(2) -0.020(2) C73 0.061(2) 0.083(3) 0.070(2) 0.054(2) -0.0080(18) -0.0027(19) C74 0.053(2) 0.073(2) 0.067(2) 0.022(2) 0.0043(18) -0.0224(18) C75 0.0443(19) 0.100(3) 0.089(3) 0.069(3) 0.0163(19) 0.0049(19) C76 0.053(2) 0.067(2) 0.082(3) 0.041(2) 0.0271(19) 0.0180(17) C77 0.087(5) 0.161(8) 0.366(16) 0.158(10) -0.022(7) -0.013(5) C78 0.123(6) 0.179(8) 0.137(6) 0.064(6) -0.006(5) 0.022(6) C79 0.121(5) 0.138(6) 0.129(6) 0.047(5) 0.027(5) -0.026(5) C80 0.137(6) 0.205(9) 0.113(5) 0.068(6) 0.002(5) -0.045(6) C81 0.41(3) 0.40(3) 0.190(16) -0.074(18) -0.134(18) 0.07(2) C82 0.69(6) 0.58(5) 0.39(4) 0.33(4) 0.27(4) 0.55(5) C83 0.150(8) 0.178(9) 0.145(8) 0.058(7) 0.032(6) 0.004(7) C84 0.50(3) 0.37(3) 0.229(19) 0.031(17) 0.15(2) -0.18(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N3 1.936(2) . ? Fe1 N8 1.941(2) . ? Fe1 C9 2.083(3) . ? Fe1 C20 2.087(3) . ? Fe1 C1 2.104(3) . ? Fe1 C28 2.109(3) . ? Fe2 N13 1.939(2) . ? Fe2 N18 1.942(2) . ? Fe2 C47 2.086(3) . ? Fe2 C39 2.090(3) . ? Fe2 C66 2.090(3) . ? Fe2 C58 2.092(3) . ? P1 F6 1.496(4) . ? P1 F1 1.524(4) . ? P1 F2 1.548(4) . ? P1 F5 1.549(3) . ? P1 F3 1.584(4) . ? P1 F4 1.593(5) . ? P2 F12 1.561(3) . ? P2 F7 1.574(3) . ? P2 F10 1.577(3) . ? P2 F8 1.585(3) . ? P2 F9 1.588(3) . ? P2 F11 1.590(3) . ? P3 F14 1.524(4) . ? P3 F16 1.531(4) . ? P3 F15 1.545(4) . ? P3 F17 1.558(3) . ? P3 F18 1.567(3) . ? P3 F13 1.573(3) . ? P4 F20 1.526(4) . ? P4 F24 1.557(4) . ? P4 F19 1.563(3) . ? P4 F22 1.586(3) . ? P4 F23 1.593(4) . ? P4 F21 1.594(3) . ? N1 C1 1.378(4) . ? N1 C2 1.404(4) . ? N1 C12 1.530(4) . ? N2 C3 1.390(4) . ? N2 C1 1.396(4) . ? N2 C4 1.399(4) . ? N3 C8 1.345(4) . ? N3 C4 1.346(4) . ? N4 C10 1.387(4) . ? N4 C9 1.397(3) . ? N4 C8 1.397(4) . ? N5 C9 1.375(4) . ? N5 C11 1.405(4) . ? N5 C13 1.514(4) . ? N6 C20 1.385(4) . ? N6 C21 1.407(4) . ? N6 C31 1.507(4) . ? N7 C22 1.388(4) . ? N7 C20 1.393(3) . ? N7 C23 1.397(4) . ? N8 C23 1.338(4) . ? N8 C27 1.350(4) . ? N9 C28 1.385(4) . ? N9 C29 1.391(4) . ? N9 C27 1.399(4) . ? N10 C28 1.376(4) . ? N10 C30 1.403(4) . ? N10 C32 1.516(4) . ? N11 C39 1.379(4) . ? N11 C40 1.409(4) . ? N11 C50 1.513(5) . ? N12 C39 1.384(4) . ? N12 C41 1.395(4) . ? N12 C42 1.397(4) . ? N13 C42 1.336(4) . ? N13 C46 1.347(4) . ? N14 C48 1.393(4) . ? N14 C46 1.393(4) . ? N14 C47 1.396(4) . ? N15 C47 1.374(4) . ? N15 C49 1.414(4) . ? N15 C51 1.523(4) . ? N16 C58 1.375(3) . ? N16 C59 1.409(4) . ? N16 C69 1.516(4) . ? N17 C58 1.392(3) . ? N17 C61 1.398(4) . ? N17 C60 1.399(4) . ? N18 C65 1.341(4) . ? N18 C61 1.346(3) . ? N19 C66 1.389(3) . ? N19 C67 1.389(4) . ? N19 C65 1.405(3) . ? N20 C66 1.383(3) . ? N20 C68 1.400(4) . ? N20 C70 1.522(4) . ? O1 C77 1.349(10) . ? O1 C80 1.364(9) . ? O2 C81 1.27(2) . ? O2 C84 1.51(2) . ? C2 C3 1.336(5) . ? C4 C5 1.389(4) . ? C5 C6 1.392(5) . ? C6 C7 1.382(5) . ? C7 C8 1.392(4) . ? C10 C11 1.331(5) . ? C12 C15 1.508(5) . ? C12 C16 1.519(5) . ? C12 C14 1.532(5) . ? C13 C17 1.530(5) . ? C13 C19 1.532(5) . ? C13 C18 1.537(4) . ? C21 C22 1.339(5) . ? C23 C24 1.400(4) . ? C24 C25 1.384(5) . ? C25 C26 1.389(5) . ? C26 C27 1.394(4) . ? C29 C30 1.329(5) . ? C31 C34 1.531(5) . ? C31 C33 1.531(5) . ? C31 C35 1.536(4) . ? C32 C38 1.514(6) . ? C32 C36 1.526(6) . ? C32 C37 1.530(5) . ? C40 C41 1.323(6) . ? C42 C43 1.393(4) . ? C43 C44 1.376(6) . ? C44 C45 1.371(6) . ? C45 C46 1.399(4) . ? C48 C49 1.315(5) . ? C50 C52 1.514(6) . ? C50 C54 1.531(7) . ? C50 C53 1.544(5) . ? C51 C55 1.526(5) . ? C51 C57 1.528(5) . ? C51 C56 1.546(5) . ? C59 C60 1.324(5) . ? C61 C62 1.392(4) . ? C62 C63 1.382(5) . ? C63 C64 1.391(5) . ? C64 C65 1.386(4) . ? C67 C68 1.334(4) . ? C69 C71 1.525(5) . ? C69 C72 1.528(5) . ? C69 C73 1.539(4) . ? C70 C74 1.515(5) . ? C70 C76 1.528(5) . ? C70 C75 1.531(4) . ? C77 C78 1.430(11) . ? C78 C79 1.476(10) . ? C79 C80 1.521(9) . ? C81 C82 1.38(4) . ? C82 C83 1.11(3) . ? C83 C84 1.58(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 N3 Fe1 N8 178.69(10) . . ? N3 Fe1 C9 78.88(10) . . ? N8 Fe1 C9 102.43(10) . . ? N3 Fe1 C20 101.22(10) . . ? N8 Fe1 C20 78.78(10) . . ? C9 Fe1 C20 91.17(10) . . ? N3 Fe1 C1 79.31(10) . . ? N8 Fe1 C1 99.38(10) . . ? C9 Fe1 C1 158.17(11) . . ? C20 Fe1 C1 92.05(10) . . ? N3 Fe1 C28 101.00(10) . . ? N8 Fe1 C28 79.02(10) . . ? C9 Fe1 C28 92.32(10) . . ? C20 Fe1 C28 157.77(11) . . ? C1 Fe1 C28 92.82(10) . . ? N13 Fe2 N18 179.83(9) . . ? N13 Fe2 C47 78.96(11) . . ? N18 Fe2 C47 101.19(10) . . ? N13 Fe2 C39 78.93(11) . . ? N18 Fe2 C39 100.93(11) . . ? C47 Fe2 C39 157.88(12) . . ? N13 Fe2 C66 100.66(10) . . ? N18 Fe2 C66 79.26(10) . . ? C47 Fe2 C66 91.50(10) . . ? C39 Fe2 C66 92.85(11) . . ? N13 Fe2 C58 101.43(10) . . ? N18 Fe2 C58 78.66(10) . . ? C47 Fe2 C58 92.14(10) . . ? C39 Fe2 C58 91.93(11) . . ? C66 Fe2 C58 157.91(10) . . ? F6 P1 F1 102.6(4) . . ? F6 P1 F2 93.5(3) . . ? F1 P1 F2 93.5(3) . . ? F6 P1 F5 90.3(3) . . ? F1 P1 F5 87.6(3) . . ? F2 P1 F5 175.7(3) . . ? F6 P1 F3 173.5(4) . . ? F1 P1 F3 83.5(3) . . ? F2 P1 F3 88.1(3) . . ? F5 P1 F3 88.0(3) . . ? F6 P1 F4 86.9(4) . . ? F1 P1 F4 170.5(4) . . ? F2 P1 F4 85.0(3) . . ? F5 P1 F4 93.2(3) . . ? F3 P1 F4 87.0(3) . . ? F12 P2 F7 91.4(2) . . ? F12 P2 F10 91.3(2) . . ? F7 P2 F10 177.0(2) . . ? F12 P2 F8 89.1(2) . . ? F7 P2 F8 90.6(2) . . ? F10 P2 F8 88.1(2) . . ? F12 P2 F9 178.5(2) . . ? F7 P2 F9 87.4(2) . . ? F10 P2 F9 89.96(19) . . ? F8 P2 F9 91.6(2) . . ? F12 P2 F11 91.4(2) . . ? F7 P2 F11 88.9(2) . . ? F10 P2 F11 92.32(19) . . ? F8 P2 F11 179.3(2) . . ? F9 P2 F11 87.83(19) . . ? F14 P3 F16 91.3(3) . . ? F14 P3 F15 87.5(4) . . ? F16 P3 F15 175.9(3) . . ? F14 P3 F17 178.4(3) . . ? F16 P3 F17 88.2(3) . . ? F15 P3 F17 93.1(3) . . ? F14 P3 F18 91.4(3) . . ? F16 P3 F18 82.5(3) . . ? F15 P3 F18 93.6(3) . . ? F17 P3 F18 90.0(2) . . ? F14 P3 F13 92.5(3) . . ? F16 P3 F13 97.4(3) . . ? F15 P3 F13 86.5(3) . . ? F17 P3 F13 86.1(2) . . ? F18 P3 F13 176.1(2) . . ? F20 P4 F24 94.6(3) . . ? F20 P4 F19 91.9(3) . . ? F24 P4 F19 88.0(3) . . ? F20 P4 F22 91.4(3) . . ? F24 P4 F22 95.8(3) . . ? F19 P4 F22 174.7(3) . . ? F20 P4 F23 177.3(2) . . ? F24 P4 F23 87.2(3) . . ? F19 P4 F23 90.2(3) . . ? F22 P4 F23 86.4(2) . . ? F20 P4 F21 88.7(3) . . ? F24 P4 F21 176.4(3) . . ? F19 P4 F21 90.5(2) . . ? F22 P4 F21 85.5(2) . . ? F23 P4 F21 89.5(2) . . ? C1 N1 C2 110.9(2) . . ? C1 N1 C12 128.2(2) . . ? C2 N1 C12 120.5(2) . . ? C3 N2 C1 113.0(3) . . ? C3 N2 C4 126.6(3) . . ? C1 N2 C4 120.3(2) . . ? C8 N3 C4 117.3(2) . . ? C8 N3 Fe1 121.47(19) . . ? C4 N3 Fe1 121.27(19) . . ? C10 N4 C9 113.2(2) . . ? C10 N4 C8 127.4(3) . . ? C9 N4 C8 119.2(2) . . ? C9 N5 C11 111.0(2) . . ? C9 N5 C13 126.9(2) . . ? C11 N5 C13 121.8(2) . . ? C20 N6 C21 110.7(2) . . ? C20 N6 C31 127.4(2) . . ? C21 N6 C31 121.6(2) . . ? C22 N7 C20 113.2(3) . . ? C22 N7 C23 127.1(3) . . ? C20 N7 C23 119.3(2) . . ? C23 N8 C27 117.7(2) . . ? C23 N8 Fe1 121.38(19) . . ? C27 N8 Fe1 120.91(19) . . ? C28 N9 C29 112.9(3) . . ? C28 N9 C27 120.1(2) . . ? C29 N9 C27 127.0(3) . . ? C28 N10 C30 110.7(3) . . ? C28 N10 C32 128.6(2) . . ? C30 N10 C32 120.7(3) . . ? C39 N11 C40 110.2(3) . . ? C39 N11 C50 127.9(3) . . ? C40 N11 C50 121.9(3) . . ? C39 N12 C41 112.6(3) . . ? C39 N12 C42 119.8(2) . . ? C41 N12 C42 127.6(3) . . ? C42 N13 C46 117.7(3) . . ? C42 N13 Fe2 121.1(2) . . ? C46 N13 Fe2 121.1(2) . . ? C48 N14 C46 127.8(3) . . ? C48 N14 C47 112.7(3) . . ? C46 N14 C47 119.5(2) . . ? C47 N15 C49 110.5(3) . . ? C47 N15 C51 126.7(2) . . ? C49 N15 C51 122.2(3) . . ? C58 N16 C59 110.9(2) . . ? C58 N16 C69 127.4(2) . . ? C59 N16 C69 121.6(2) . . ? C58 N17 C61 119.5(2) . . ? C58 N17 C60 112.8(2) . . ? C61 N17 C60 127.7(2) . . ? C65 N18 C61 117.4(2) . . ? C65 N18 Fe2 121.05(18) . . ? C61 N18 Fe2 121.50(19) . . ? C66 N19 C67 113.1(2) . . ? C66 N19 C65 120.1(2) . . ? C67 N19 C65 126.8(2) . . ? C66 N20 C68 111.2(2) . . ? C66 N20 C70 128.1(2) . . ? C68 N20 C70 120.6(2) . . ? C77 O1 C80 107.2(6) . . ? C81 O2 C84 101.8(18) . . ? N1 C1 N2 102.0(2) . . ? N1 C1 Fe1 149.7(2) . . ? N2 C1 Fe1 108.26(18) . . ? C3 C2 N1 108.6(3) . . ? C2 C3 N2 105.4(3) . . ? N3 C4 C5 123.8(3) . . ? N3 C4 N2 110.7(2) . . ? C5 C4 N2 125.5(3) . . ? C4 C5 C6 117.0(3) . . ? C7 C6 C5 121.0(3) . . ? C6 C7 C8 117.1(3) . . ? N3 C8 C7 123.8(3) . . ? N3 C8 N4 110.7(2) . . ? C7 C8 N4 125.4(3) . . ? N5 C9 N4 101.7(2) . . ? N5 C9 Fe1 148.7(2) . . ? N4 C9 Fe1 109.61(18) . . ? C11 C10 N4 105.4(3) . . ? C10 C11 N5 108.6(3) . . ? C15 C12 C16 112.6(4) . . ? C15 C12 N1 109.5(3) . . ? C16 C12 N1 106.7(3) . . ? C15 C12 C14 109.1(3) . . ? C16 C12 C14 108.6(3) . . ? N1 C12 C14 110.3(3) . . ? N5 C13 C17 107.8(3) . . ? N5 C13 C19 108.7(3) . . ? C17 C13 C19 113.5(3) . . ? N5 C13 C18 110.2(3) . . ? C17 C13 C18 108.3(3) . . ? C19 C13 C18 108.3(3) . . ? N6 C20 N7 102.0(2) . . ? N6 C20 Fe1 148.5(2) . . ? N7 C20 Fe1 109.48(18) . . ? C22 C21 N6 108.5(3) . . ? C21 C22 N7 105.6(3) . . ? N8 C23 N7 110.9(2) . . ? N8 C23 C24 123.4(3) . . ? N7 C23 C24 125.6(3) . . ? C25 C24 C23 117.4(3) . . ? C24 C25 C26 120.6(3) . . ? C25 C26 C27 117.5(3) . . ? N8 C27 C26 123.3(3) . . ? N8 C27 N9 111.1(2) . . ? C26 C27 N9 125.6(3) . . ? N10 C28 N9 102.2(2) . . ? N10 C28 Fe1 148.9(2) . . ? N9 C28 Fe1 108.89(19) . . ? C30 C29 N9 105.6(3) . . ? C29 C30 N10 108.6(3) . . ? N6 C31 C34 107.5(3) . . ? N6 C31 C33 109.1(3) . . ? C34 C31 C33 114.0(3) . . ? N6 C31 C35 111.0(3) . . ? C34 C31 C35 107.5(3) . . ? C33 C31 C35 107.7(3) . . ? C38 C32 N10 108.1(3) . . ? C38 C32 C36 113.1(4) . . ? N10 C32 C36 107.8(3) . . ? C38 C32 C37 109.9(3) . . ? N10 C32 C37 110.7(3) . . ? C36 C32 C37 107.2(4) . . ? N11 C39 N12 102.6(2) . . ? N11 C39 Fe2 148.2(2) . . ? N12 C39 Fe2 109.2(2) . . ? C41 C40 N11 108.8(3) . . ? C40 C41 N12 105.8(3) . . ? N13 C42 C43 123.1(3) . . ? N13 C42 N12 111.0(2) . . ? C43 C42 N12 125.9(3) . . ? C44 C43 C42 117.5(3) . . ? C45 C44 C43 121.5(3) . . ? C44 C45 C46 116.8(3) . . ? N13 C46 N14 110.9(2) . . ? N13 C46 C45 123.4(3) . . ? N14 C46 C45 125.7(3) . . ? N15 C47 N14 102.1(2) . . ? N15 C47 Fe2 148.5(2) . . ? N14 C47 Fe2 109.4(2) . . ? C49 C48 N14 105.9(3) . . ? C48 C49 N15 108.9(3) . . ? N11 C50 C52 108.8(4) . . ? N11 C50 C54 107.8(3) . . ? C52 C50 C54 113.3(5) . . ? N11 C50 C53 110.0(4) . . ? C52 C50 C53 107.8(4) . . ? C54 C50 C53 109.2(4) . . ? N15 C51 C55 107.0(3) . . ? N15 C51 C57 109.2(3) . . ? C55 C51 C57 113.7(3) . . ? N15 C51 C56 110.0(3) . . ? C55 C51 C56 108.7(3) . . ? C57 C51 C56 108.3(3) . . ? N16 C58 N17 102.0(2) . . ? N16 C58 Fe2 148.4(2) . . ? N17 C58 Fe2 109.60(18) . . ? C60 C59 N16 108.7(3) . . ? C59 C60 N17 105.5(3) . . ? N18 C61 C62 123.6(3) . . ? N18 C61 N17 110.6(2) . . ? C62 C61 N17 125.7(3) . . ? C63 C62 C61 116.9(3) . . ? C62 C63 C64 121.1(3) . . ? C65 C64 C63 117.0(3) . . ? N18 C65 C64 123.8(3) . . ? N18 C65 N19 110.7(2) . . ? C64 C65 N19 125.5(3) . . ? N20 C66 N19 101.7(2) . . ? N20 C66 Fe2 149.3(2) . . ? N19 C66 Fe2 108.93(17) . . ? C68 C67 N19 105.7(3) . . ? C67 C68 N20 108.3(3) . . ? N16 C69 C71 107.8(3) . . ? N16 C69 C72 108.5(3) . . ? C71 C69 C72 114.3(3) . . ? N16 C69 C73 110.3(3) . . ? C71 C69 C73 107.8(3) . . ? C72 C69 C73 108.2(3) . . ? C74 C70 N20 108.0(2) . . ? C74 C70 C76 112.9(3) . . ? N20 C70 C76 109.0(2) . . ? C74 C70 C75 109.2(3) . . ? N20 C70 C75 110.2(3) . . ? C76 C70 C75 107.7(3) . . ? O1 C77 C78 110.6(7) . . ? C77 C78 C79 106.1(7) . . ? C78 C79 C80 101.6(6) . . ? O1 C80 C79 109.2(6) . . ? O2 C81 C82 79(2) . . ? C83 C82 C81 160(3) . . ? C82 C83 C84 67(3) . . ? O2 C84 C83 108.4(13) . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.018 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.074 _database_code_depnum_ccdc_archive 'CCDC 915796'