# 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 ? _publ_contact_author_name 'Kari Rissanen' _publ_contact_author_email kari.t.rissanen@jyu.fi loop_ _publ_author_name K.Raatikainen J.Huuskonen K.Rissanen data_I _database_code_depnum_ccdc_archive 'CCDC 809073' #TrackingRef '- CS_KR_110124_XRD.cif' _audit_creation_date 2010-06-24T10:45:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C48 H48 Fe N6 O12, C6 H14 O, C2 H3 N, 2(Cl O4)' _chemical_formula_sum 'C56 H65 Cl2 Fe N7 O21' _chemical_formula_weight 1298.9 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 14.9147(2) _cell_length_b 24.5620(4) _cell_length_c 16.5450(2) _cell_angle_alpha 90 _cell_angle_beta 94.7070(10) _cell_angle_gamma 90 _cell_volume 6040.57(15) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5307 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 28.283 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.9158 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.79574E-2 _diffrn_orient_matrix_ub_12 -0.382596E-1 _diffrn_orient_matrix_ub_13 -0.199784E-1 _diffrn_orient_matrix_ub_21 -0.631211E-1 _diffrn_orient_matrix_ub_22 0 _diffrn_orient_matrix_ub_23 0.162396E-1 _diffrn_orient_matrix_ub_31 -0.218705E-1 _diffrn_orient_matrix_ub_32 0.139204E-1 _diffrn_orient_matrix_ub_33 -0.549095E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.099 _diffrn_reflns_av_unetI/netI 0.0582 _diffrn_reflns_number 70828 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 10625 _reflns_number_gt 7712 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0359P)^2^+16.1400P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10625 _refine_ls_number_parameters 795 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.063 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.968 _refine_diff_density_min -0.66 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.10310(4) 0.37253(2) 0.28392(3) 0.01730(14) Uani 1 1 d . . . C1 C 0.2962(4) 0.3844(2) -0.0793(4) 0.0636(18) Uani 1 1 d . . . H1A H 0.2391 0.4043 -0.0817 0.095 Uiso 1 1 calc R . . H1B H 0.3264 0.3916 -0.1286 0.095 Uiso 1 1 calc R . . H1C H 0.3348 0.3963 -0.0318 0.095 Uiso 1 1 calc R . . C2 C 0.2787(3) 0.3255(2) -0.0731(3) 0.0386(12) Uani 1 1 d . . . H2A H 0.2376 0.3132 -0.1195 0.046 Uiso 1 1 calc R . . H2B H 0.3356 0.3048 -0.0731 0.046 Uiso 1 1 calc R . . O3 O 0.2377(2) 0.31687(11) 0.00245(16) 0.0285(7) Uani 1 1 d . . . C4 C 0.2286(3) 0.26584(18) 0.0261(3) 0.0310(10) Uani 1 1 d . . . O5 O 0.2453(3) 0.22673(13) -0.0133(2) 0.0571(11) Uani 1 1 d . . . C6 C 0.1903(3) 0.26252(16) 0.1069(2) 0.0223(9) Uani 1 1 d . . . C7 C 0.1672(3) 0.21265(17) 0.1380(2) 0.0283(10) Uani 1 1 d . . . H7 H 0.1765 0.18 0.1091 0.034 Uiso 1 1 calc R . . C8 C 0.1302(3) 0.21132(16) 0.2119(2) 0.0248(9) Uani 1 1 d . . . H8 H 0.1142 0.1776 0.2347 0.03 Uiso 1 1 calc R . . C9 C 0.1165(3) 0.25971(15) 0.2524(2) 0.0187(8) Uani 1 1 d . . . N10 N 0.1408(2) 0.30878(12) 0.22262(18) 0.0187(7) Uani 1 1 d . . . C11 C 0.1780(3) 0.30939(16) 0.1514(2) 0.0193(8) Uani 1 1 d . . . H11 H 0.1967 0.3433 0.1307 0.023 Uiso 1 1 calc R . . C12 C 0.0752(3) 0.26339(15) 0.3300(2) 0.0202(8) Uani 1 1 d . . . C13 C 0.0452(3) 0.21832(16) 0.3701(2) 0.0269(10) Uani 1 1 d . . . H13 H 0.0513 0.1828 0.3484 0.032 Uiso 1 1 calc R . . C14 C 0.0062(3) 0.22579(16) 0.4421(2) 0.0297(10) Uani 1 1 d . . . H14 H -0.0157 0.1955 0.4703 0.036 Uiso 1 1 calc R . . C15 C -0.0004(3) 0.27796(16) 0.4726(2) 0.0248(9) Uani 1 1 d . . . C16 C 0.0310(3) 0.32150(16) 0.4295(2) 0.0213(9) Uani 1 1 d . . . H16 H 0.0271 0.3572 0.4511 0.026 Uiso 1 1 calc R . . N17 N 0.0668(2) 0.31503(12) 0.35828(18) 0.0189(7) Uani 1 1 d . . . C18 C -0.0420(3) 0.28401(17) 0.5518(3) 0.0358(11) Uani 1 1 d . . . O19 O -0.0674(3) 0.24574(14) 0.5881(2) 0.0787(16) Uani 1 1 d . . . O20 O -0.04348(19) 0.33479(11) 0.57728(15) 0.0242(6) Uani 1 1 d . . . C21 C -0.0839(3) 0.34401(18) 0.6541(2) 0.0298(10) Uani 1 1 d . . . H21A H -0.057 0.3769 0.6808 0.036 Uiso 1 1 calc R . . H21B H -0.0705 0.3126 0.6907 0.036 Uiso 1 1 calc R . . C22 C -0.1835(3) 0.3512(2) 0.6404(3) 0.0459(13) Uani 1 1 d . . . H22A H -0.1969 0.3795 0.5995 0.069 Uiso 1 1 calc R . . H22B H -0.2077 0.3619 0.6913 0.069 Uiso 1 1 calc R . . H22C H -0.2111 0.3168 0.6214 0.069 Uiso 1 1 calc R . . C23 C 0.5297(5) 0.2206(2) 0.5149(4) 0.076(2) Uani 1 1 d . . . H23A H 0.4964 0.2252 0.5631 0.114 Uiso 1 1 calc R . . H23B H 0.5815 0.1967 0.5279 0.114 Uiso 1 1 calc R . . H23C H 0.4902 0.2043 0.4712 0.114 Uiso 1 1 calc R . . C24 C 0.5618(3) 0.2749(2) 0.4881(3) 0.0517(15) Uani 1 1 d . . . H24A H 0.6093 0.2885 0.5284 0.062 Uiso 1 1 calc R . . H24B H 0.5884 0.2708 0.4356 0.062 Uiso 1 1 calc R . . O25 O 0.4885(2) 0.31477(13) 0.47910(18) 0.0380(8) Uani 1 1 d . . . C26 C 0.4338(3) 0.31194(18) 0.4117(2) 0.0290(10) Uani 1 1 d . . . O27 O 0.4403(2) 0.27935(14) 0.35803(19) 0.0433(9) Uani 1 1 d . . . C28 C 0.3613(3) 0.35395(16) 0.4109(2) 0.0230(9) Uani 1 1 d . . . C29 C 0.3619(3) 0.39608(17) 0.4664(2) 0.0289(10) Uani 1 1 d . . . H29 H 0.411 0.4005 0.5062 0.035 Uiso 1 1 calc R . . C30 C 0.2901(3) 0.43168(17) 0.4632(2) 0.0280(10) Uani 1 1 d . . . H30 H 0.29 0.4614 0.5 0.034 Uiso 1 1 calc R . . C31 C 0.2180(3) 0.42382(15) 0.4057(2) 0.0209(9) Uani 1 1 d . . . N32 N 0.2170(2) 0.38183(12) 0.35127(18) 0.0192(7) Uani 1 1 d . . . C33 C 0.2884(3) 0.34859(16) 0.3543(2) 0.0211(9) Uani 1 1 d . . . H33 H 0.289 0.32 0.3157 0.025 Uiso 1 1 calc R . . C34 C 0.1361(3) 0.45694(15) 0.3990(2) 0.0195(8) Uani 1 1 d . . . C35 C 0.1256(3) 0.50505(15) 0.4404(2) 0.0225(9) Uani 1 1 d . . . H35 H 0.1736 0.5191 0.4756 0.027 Uiso 1 1 calc R . . C36 C 0.0449(3) 0.53257(16) 0.4301(2) 0.0254(9) Uani 1 1 d . . . H36 H 0.0367 0.5659 0.4578 0.03 Uiso 1 1 calc R . . C37 C -0.0238(3) 0.51085(15) 0.3788(2) 0.0211(9) Uani 1 1 d . . . C38 C -0.0095(3) 0.46257(15) 0.3384(2) 0.0203(9) Uani 1 1 d . . . H38 H -0.0568 0.4481 0.3028 0.024 Uiso 1 1 calc R . . N39 N 0.0683(2) 0.43566(12) 0.34771(18) 0.0188(7) Uani 1 1 d . . . C40 C -0.1117(3) 0.54027(16) 0.3665(2) 0.0251(9) Uani 1 1 d . . . O41 O -0.1294(2) 0.58130(11) 0.40282(17) 0.0317(7) Uani 1 1 d . . . O42 O -0.16757(19) 0.51532(11) 0.31150(17) 0.0280(7) Uani 1 1 d . . . C43 C -0.2536(3) 0.54161(19) 0.2908(3) 0.0358(11) Uani 1 1 d . . . H43A H -0.2445 0.5792 0.2714 0.043 Uiso 1 1 calc R . . H43B H -0.2891 0.5432 0.3388 0.043 Uiso 1 1 calc R . . C44 C -0.3013(3) 0.5080(2) 0.2254(3) 0.0448(13) Uani 1 1 d . . . H44A H -0.2672 0.5086 0.1772 0.067 Uiso 1 1 calc R . . H44B H -0.3615 0.5229 0.2117 0.067 Uiso 1 1 calc R . . H44C H -0.3064 0.4704 0.2443 0.067 Uiso 1 1 calc R . . C45 C 0.4214(4) 0.5702(2) -0.0421(3) 0.0531(15) Uani 1 1 d . . . H45A H 0.4185 0.5362 -0.0733 0.08 Uiso 1 1 calc R . . H45B H 0.4787 0.5885 -0.0488 0.08 Uiso 1 1 calc R . . H45C H 0.3715 0.594 -0.0616 0.08 Uiso 1 1 calc R . . C46 C 0.4148(4) 0.5576(2) 0.0461(3) 0.0521(14) Uani 1 1 d . . . H46A H 0.4656 0.5342 0.0668 0.063 Uiso 1 1 calc R . . H46B H 0.4166 0.5917 0.0782 0.063 Uiso 1 1 calc R . . O47 O 0.3298(2) 0.52953(13) 0.05268(19) 0.0411(8) Uani 1 1 d . . . C48 C 0.3194(3) 0.50524(19) 0.1235(3) 0.0390(12) Uani 1 1 d . . . O49 O 0.3754(3) 0.50432(18) 0.1797(2) 0.0664(13) Uani 1 1 d . . . C50 C 0.2298(3) 0.47795(16) 0.1229(2) 0.0273(9) Uani 1 1 d . . . C51 C 0.1669(3) 0.47829(16) 0.0569(2) 0.0270(9) Uani 1 1 d . . . H51 H 0.1792 0.4967 0.0085 0.032 Uiso 1 1 calc R . . C52 C -0.2389(3) 0.30256(18) 0.1995(3) 0.0296(10) Uani 1 1 d . . . C522 C 0.0862(3) 0.45173(16) 0.0615(2) 0.0270(10) Uani 1 1 d . . . H522 H 0.0419 0.4522 0.0168 0.032 Uiso 1 1 calc R . . C53 C 0.0703(3) 0.42425(15) 0.1324(2) 0.0205(9) Uani 1 1 d . . . N54 N 0.1331(2) 0.42211(12) 0.19710(18) 0.0207(7) Uani 1 1 d . . . C55 C 0.2101(3) 0.44940(16) 0.1921(2) 0.0258(9) Uani 1 1 d . . . H55 H 0.2533 0.4493 0.2377 0.031 Uiso 1 1 calc R . . C56 C -0.0129(3) 0.39475(15) 0.1443(2) 0.0206(8) Uani 1 1 d . . . C57 C -0.0866(3) 0.39291(17) 0.0881(2) 0.0267(9) Uani 1 1 d . . . H57 H -0.0858 0.4116 0.038 0.032 Uiso 1 1 calc R . . C58 C -0.1617(3) 0.36350(17) 0.1057(2) 0.0279(10) Uani 1 1 d . . . H58 H -0.213 0.3618 0.0677 0.033 Uiso 1 1 calc R . . C59 C -0.1615(3) 0.33661(16) 0.1792(2) 0.0243(9) Uani 1 1 d . . . C60 C -0.0857(3) 0.34098(15) 0.2337(2) 0.0216(9) Uani 1 1 d . . . H60 H -0.086 0.3235 0.2849 0.026 Uiso 1 1 calc R . . N61 N -0.0122(2) 0.36877(12) 0.21707(18) 0.0197(7) Uani 1 1 d . . . O63 O -0.3115(2) 0.30424(14) 0.16216(19) 0.0421(8) Uani 1 1 d . . . O64 O -0.21700(19) 0.26972(12) 0.26172(18) 0.0326(7) Uani 1 1 d . . . C65 C -0.2905(3) 0.2381(2) 0.2910(3) 0.0404(12) Uani 1 1 d . . . H65A H -0.3171 0.2137 0.2479 0.048 Uiso 1 1 calc R . . H65B H -0.3381 0.2625 0.3083 0.048 Uiso 1 1 calc R . . C66 C -0.2498(4) 0.2052(2) 0.3622(3) 0.0580(16) Uani 1 1 d . . . H66A H -0.204 0.1806 0.3438 0.087 Uiso 1 1 calc R . . H66B H -0.297 0.184 0.3854 0.087 Uiso 1 1 calc R . . H66C H -0.2219 0.2299 0.4035 0.087 Uiso 1 1 calc R . . Cl67 Cl -0.01312(8) 0.56363(4) 0.16318(6) 0.0277(2) Uani 1 1 d . . . O68 O 0.0601(2) 0.54160(12) 0.21459(17) 0.0374(8) Uani 1 1 d . . . O69 O -0.0675(2) 0.52038(11) 0.12693(17) 0.0351(7) Uani 1 1 d . . . O70 O -0.0682(2) 0.59763(11) 0.21075(17) 0.0360(8) Uani 1 1 d . . . O71 O 0.0220(2) 0.59639(11) 0.10052(16) 0.0324(7) Uani 1 1 d . . . Cl72 Cl -0.24114(8) 0.38556(5) 0.40347(7) 0.0447(3) Uani 1 1 d . . . O73 O -0.1467(2) 0.39236(16) 0.4134(2) 0.0541(10) Uani 1 1 d . . . O74 O -0.2658(6) 0.3377(2) 0.4403(3) 0.162(4) Uani 1 1 d . . . O75 O -0.2806(3) 0.4325(2) 0.4396(3) 0.100(2) Uani 1 1 d . . . O76 O -0.2708(3) 0.38321(16) 0.3195(2) 0.0608(11) Uani 1 1 d . . . N77 N -0.6225(3) 0.3590(3) 0.1639(3) 0.0746(16) Uani 1 1 d . . . C78 C -0.5569(3) 0.3693(2) 0.1978(3) 0.0444(12) Uani 1 1 d . . . C79 C -0.4725(4) 0.3825(3) 0.2416(3) 0.0642(18) Uani 1 1 d . . . H79A H -0.4736 0.3709 0.2982 0.096 Uiso 1 1 calc R . . H79B H -0.4625 0.4219 0.2397 0.096 Uiso 1 1 calc R . . H79C H -0.4237 0.3636 0.2169 0.096 Uiso 1 1 calc R . . C80 C -0.6091(4) 0.3169(3) 0.6752(4) 0.0732(19) Uani 1 1 d . . . H80A H -0.6554 0.3332 0.7064 0.11 Uiso 1 1 calc R . . H80B H -0.5976 0.2794 0.6936 0.11 Uiso 1 1 calc R . . H80C H -0.6299 0.3167 0.6175 0.11 Uiso 1 1 calc R . . C81 C -0.5250(4) 0.3491(3) 0.6876(4) 0.0638(16) Uani 1 1 d . . . H81 H -0.4774 0.3313 0.6575 0.077 Uiso 1 1 calc R . . C82 C -0.4938(4) 0.3517(3) 0.7745(3) 0.0676(18) Uani 1 1 d . . . H82A H -0.435 0.3696 0.7811 0.101 Uiso 1 1 calc R . . H82B H -0.4887 0.3147 0.7967 0.101 Uiso 1 1 calc R . . H82C H -0.5372 0.3724 0.8036 0.101 Uiso 1 1 calc R . . O83 O -0.5451(3) 0.40352(17) 0.6518(2) 0.0639(11) Uani 1 1 d . . . C84 C -0.4717(4) 0.4441(3) 0.6517(4) 0.0687(18) Uani 1 1 d . . . H84 H -0.4514 0.4518 0.7097 0.082 Uiso 1 1 calc R . . C85 C -0.3934(5) 0.4259(3) 0.6132(6) 0.106(3) Uani 1 1 d . . . H85A H -0.4096 0.4201 0.5553 0.159 Uiso 1 1 calc R . . H85B H -0.3715 0.3917 0.6382 0.159 Uiso 1 1 calc R . . H85C H -0.3461 0.4536 0.6202 0.159 Uiso 1 1 calc R . . C86 C -0.5160(5) 0.4931(3) 0.6192(4) 0.0755(19) Uani 1 1 d . . . H86A H -0.5296 0.4891 0.5606 0.113 Uiso 1 1 calc R . . H86B H -0.4762 0.5245 0.6301 0.113 Uiso 1 1 calc R . . H86C H -0.572 0.4988 0.6452 0.113 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 0.0243(3) 0.0133(3) 0.0144(3) -0.0008(2) 0.0026(2) -0.0017(2) C1 0.090(5) 0.047(3) 0.059(4) 0.021(3) 0.043(3) 0.005(3) C2 0.041(3) 0.052(3) 0.024(2) 0.003(2) 0.013(2) -0.007(2) O3 0.0398(18) 0.0277(16) 0.0199(14) -0.0009(12) 0.0130(12) -0.0023(14) C4 0.042(3) 0.028(2) 0.025(2) -0.0049(19) 0.0123(19) 0.001(2) O5 0.099(3) 0.0297(19) 0.048(2) -0.0079(17) 0.043(2) 0.0013(19) C6 0.027(2) 0.019(2) 0.022(2) -0.0026(17) 0.0044(17) -0.0016(17) C7 0.038(3) 0.021(2) 0.028(2) -0.0060(18) 0.0091(19) -0.0014(19) C8 0.033(2) 0.018(2) 0.024(2) -0.0011(17) 0.0087(18) -0.0003(18) C9 0.022(2) 0.0139(19) 0.0203(19) -0.0008(16) -0.0011(16) -0.0039(16) N10 0.0222(18) 0.0180(16) 0.0159(16) -0.0030(13) 0.0018(13) -0.0002(14) C11 0.021(2) 0.0185(19) 0.0182(19) -0.0008(16) 0.0014(16) -0.0012(16) C12 0.026(2) 0.0159(19) 0.0186(19) -0.0014(16) 0.0025(16) -0.0018(17) C13 0.041(3) 0.015(2) 0.025(2) -0.0016(17) 0.0096(19) -0.0027(19) C14 0.047(3) 0.016(2) 0.028(2) 0.0019(18) 0.014(2) -0.007(2) C15 0.033(2) 0.022(2) 0.021(2) -0.0028(17) 0.0097(18) -0.0029(18) C16 0.027(2) 0.018(2) 0.019(2) -0.0020(16) 0.0032(16) -0.0004(17) N17 0.0235(18) 0.0154(16) 0.0179(16) -0.0002(13) 0.0021(13) -0.0019(14) C18 0.057(3) 0.022(2) 0.032(2) -0.004(2) 0.021(2) -0.007(2) O19 0.161(5) 0.0255(19) 0.061(2) -0.0103(18) 0.078(3) -0.029(2) O20 0.0327(17) 0.0232(15) 0.0177(14) -0.0001(12) 0.0079(12) -0.0002(13) C21 0.046(3) 0.028(2) 0.017(2) -0.0012(18) 0.0086(19) 0.001(2) C22 0.039(3) 0.058(3) 0.043(3) 0.002(3) 0.017(2) 0.009(3) C23 0.081(5) 0.057(4) 0.083(5) 0.016(3) -0.038(4) 0.020(4) C24 0.037(3) 0.065(4) 0.050(3) -0.008(3) -0.013(2) 0.022(3) O25 0.0302(18) 0.0442(19) 0.0379(18) -0.0057(15) -0.0068(14) 0.0084(15) C26 0.028(2) 0.036(2) 0.023(2) 0.007(2) 0.0025(18) -0.003(2) O27 0.052(2) 0.046(2) 0.0307(18) -0.0085(16) -0.0012(15) 0.0212(17) C28 0.027(2) 0.022(2) 0.021(2) 0.0057(17) 0.0056(17) -0.0018(18) C29 0.030(2) 0.033(2) 0.023(2) 0.0034(19) -0.0027(18) -0.004(2) C30 0.036(3) 0.026(2) 0.021(2) -0.0041(18) -0.0004(18) -0.001(2) C31 0.028(2) 0.019(2) 0.0160(19) -0.0013(16) 0.0067(16) -0.0080(17) N32 0.0275(19) 0.0148(16) 0.0159(16) 0.0022(13) 0.0049(13) -0.0018(14) C33 0.028(2) 0.018(2) 0.0173(19) 0.0030(16) 0.0053(16) 0.0002(18) C34 0.027(2) 0.0175(19) 0.0141(18) -0.0004(16) 0.0034(16) -0.0039(17) C35 0.032(2) 0.020(2) 0.0161(19) -0.0014(16) 0.0031(16) -0.0018(18) C36 0.040(3) 0.019(2) 0.018(2) -0.0017(17) 0.0060(18) -0.0004(19) C37 0.030(2) 0.0165(19) 0.018(2) 0.0033(16) 0.0084(17) -0.0005(17) C38 0.031(2) 0.0149(19) 0.0154(19) 0.0036(16) 0.0037(16) -0.0032(17) N39 0.0253(18) 0.0173(16) 0.0144(16) 0.0011(13) 0.0057(13) -0.0004(14) C40 0.037(3) 0.018(2) 0.021(2) 0.0021(18) 0.0091(18) -0.0032(19) O41 0.0408(19) 0.0237(16) 0.0312(16) -0.0048(13) 0.0063(13) 0.0089(14) O42 0.0296(17) 0.0224(15) 0.0320(16) 0.0000(13) 0.0018(13) 0.0043(13) C43 0.029(3) 0.038(3) 0.040(3) 0.001(2) 0.000(2) 0.003(2) C44 0.043(3) 0.037(3) 0.052(3) 0.005(2) -0.009(2) 0.000(2) C45 0.045(3) 0.061(4) 0.056(3) 0.018(3) 0.020(3) -0.007(3) C46 0.053(3) 0.051(3) 0.054(3) 0.011(3) 0.015(3) -0.024(3) O47 0.043(2) 0.0432(19) 0.0388(18) 0.0147(16) 0.0118(15) -0.0117(16) C48 0.049(3) 0.035(3) 0.034(3) 0.005(2) 0.008(2) -0.012(2) O49 0.065(3) 0.090(3) 0.041(2) 0.022(2) -0.0110(19) -0.046(2) C50 0.036(3) 0.020(2) 0.028(2) 0.0023(18) 0.0095(19) -0.0018(19) C51 0.040(3) 0.020(2) 0.022(2) 0.0049(17) 0.0087(18) 0.002(2) C52 0.030(3) 0.032(2) 0.025(2) -0.010(2) -0.0001(19) -0.006(2) C522 0.039(3) 0.023(2) 0.019(2) 0.0001(17) 0.0031(18) 0.006(2) C53 0.028(2) 0.0136(19) 0.021(2) -0.0022(16) 0.0036(17) 0.0038(17) N54 0.0269(19) 0.0160(16) 0.0195(17) -0.0022(13) 0.0045(14) -0.0002(14) C55 0.032(2) 0.021(2) 0.024(2) 0.0005(17) 0.0019(18) -0.0032(19) C56 0.030(2) 0.0164(19) 0.0152(19) -0.0002(16) 0.0003(16) 0.0054(17) C57 0.033(2) 0.024(2) 0.023(2) -0.0005(18) 0.0027(18) 0.0042(19) C58 0.029(2) 0.029(2) 0.024(2) -0.0071(18) -0.0049(18) 0.0033(19) C59 0.024(2) 0.023(2) 0.026(2) -0.0070(18) 0.0016(17) 0.0023(18) C60 0.025(2) 0.016(2) 0.023(2) -0.0019(16) 0.0031(17) 0.0015(17) N61 0.0240(18) 0.0151(16) 0.0202(16) -0.0044(14) 0.0036(13) 0.0007(14) O63 0.0321(19) 0.057(2) 0.0362(18) -0.0052(16) -0.0031(15) -0.0091(16) O64 0.0270(17) 0.0328(17) 0.0382(18) -0.0004(14) 0.0036(13) -0.0082(14) C65 0.031(3) 0.046(3) 0.045(3) -0.002(2) 0.006(2) -0.015(2) C66 0.054(4) 0.059(4) 0.062(4) 0.019(3) 0.011(3) -0.019(3) Cl67 0.0482(7) 0.0164(5) 0.0194(5) 0.0010(4) 0.0083(4) 0.0037(5) O68 0.057(2) 0.0297(17) 0.0253(16) 0.0033(13) -0.0003(14) 0.0093(15) O69 0.055(2) 0.0200(15) 0.0306(17) -0.0039(13) 0.0073(14) -0.0016(14) O70 0.057(2) 0.0205(15) 0.0330(17) -0.0017(13) 0.0177(15) 0.0048(15) O71 0.055(2) 0.0215(15) 0.0227(15) 0.0029(12) 0.0138(14) -0.0020(14) Cl72 0.0436(7) 0.0577(8) 0.0342(6) -0.0184(6) 0.0131(5) -0.0245(6) O73 0.035(2) 0.066(3) 0.059(2) -0.003(2) -0.0073(17) 0.0043(18) O74 0.309(9) 0.123(5) 0.059(3) -0.014(3) 0.048(4) -0.161(6) O75 0.045(3) 0.155(5) 0.101(4) -0.100(4) 0.007(2) 0.001(3) O76 0.057(2) 0.073(3) 0.049(2) -0.032(2) -0.0185(18) 0.019(2) N77 0.042(3) 0.111(5) 0.070(4) 0.011(3) -0.002(3) -0.013(3) C78 0.030(3) 0.058(3) 0.047(3) 0.012(3) 0.008(2) -0.002(3) C79 0.042(3) 0.097(5) 0.053(3) 0.010(3) 0.004(3) -0.021(3) C80 0.068(4) 0.067(4) 0.085(5) -0.010(4) 0.014(4) -0.022(4) C81 0.054(4) 0.063(4) 0.074(4) -0.006(3) 0.003(3) 0.001(3) C82 0.075(4) 0.080(5) 0.048(3) 0.017(3) 0.007(3) 0.012(4) O83 0.059(3) 0.069(3) 0.064(3) 0.000(2) 0.005(2) -0.007(2) C84 0.056(4) 0.075(5) 0.074(4) -0.029(4) -0.005(3) -0.023(3) C85 0.049(4) 0.096(6) 0.181(9) 0.027(6) 0.059(5) 0.010(4) C86 0.082(5) 0.067(4) 0.081(5) -0.002(4) 0.026(4) -0.014(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N54 1.962(3) . ? Fe1 N32 1.967(3) . ? Fe1 N61 1.969(3) . ? Fe1 N39 1.969(3) . ? Fe1 N10 1.972(3) . ? Fe1 N17 1.978(3) . ? C1 C2 1.474(7) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 O3 1.451(5) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? O3 C4 1.324(5) . ? C4 O5 1.199(5) . ? C4 C6 1.498(5) . ? C6 C7 1.383(6) . ? C6 C11 1.387(5) . ? C7 C8 1.383(6) . ? C7 H7 0.95 . ? C8 C9 1.388(5) . ? C8 H8 0.95 . ? C9 N10 1.362(5) . ? C9 C12 1.472(5) . ? N10 C11 1.344(5) . ? C11 H11 0.95 . ? C12 N17 1.361(5) . ? C12 C13 1.384(5) . ? C13 C14 1.379(6) . ? C13 H13 0.95 . ? C14 C15 1.384(5) . ? C14 H14 0.95 . ? C15 C16 1.389(5) . ? C15 C18 1.501(6) . ? C16 N17 1.341(5) . ? C16 H16 0.95 . ? C18 O19 1.194(5) . ? C18 O20 1.318(5) . ? O20 C21 1.468(5) . ? C21 C22 1.495(6) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C24 1.497(8) . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 O25 1.466(6) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? O25 C26 1.327(5) . ? C26 O27 1.206(5) . ? C26 C28 1.494(6) . ? C28 C33 1.382(5) . ? C28 C29 1.383(6) . ? C29 C30 1.380(6) . ? C29 H29 0.95 . ? C30 C31 1.389(6) . ? C30 H30 0.95 . ? C31 N32 1.369(5) . ? C31 C34 1.464(6) . ? N32 C33 1.340(5) . ? C33 H33 0.95 . ? C34 N39 1.370(5) . ? C34 C35 1.381(5) . ? C35 C36 1.378(6) . ? C35 H35 0.95 . ? C36 C37 1.384(6) . ? C36 H36 0.95 . ? C37 C38 1.386(5) . ? C37 C40 1.496(6) . ? C38 N39 1.333(5) . ? C38 H38 0.95 . ? C40 O41 1.214(5) . ? C40 O42 1.331(5) . ? O42 C43 1.452(5) . ? C43 C44 1.494(6) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? C45 C46 1.502(7) . ? C45 H45A 0.98 . ? C45 H45B 0.98 . ? C45 H45C 0.98 . ? C46 O47 1.455(6) . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? O47 C48 1.335(5) . ? C48 O49 1.199(6) . ? C48 C50 1.494(6) . ? C50 C51 1.381(6) . ? C50 C55 1.394(6) . ? C51 C522 1.377(6) . ? C51 H51 0.95 . ? C52 O63 1.202(5) . ? C52 O64 1.327(5) . ? C52 C59 1.486(6) . ? C522 C53 1.391(5) . ? C522 H522 0.95 . ? C53 N54 1.363(5) . ? C53 C56 1.464(6) . ? N54 C55 1.339(5) . ? C55 H55 0.95 . ? C56 N61 1.362(5) . ? C56 C57 1.381(5) . ? C57 C58 1.383(6) . ? C57 H57 0.95 . ? C58 C59 1.383(6) . ? C58 H58 0.95 . ? C59 C60 1.392(5) . ? C60 N61 1.339(5) . ? C60 H60 0.95 . ? O64 C65 1.458(5) . ? C65 C66 1.512(7) . ? C65 H65A 0.99 . ? C65 H65B 0.99 . ? C66 H66A 0.98 . ? C66 H66B 0.98 . ? C66 H66C 0.98 . ? Cl67 O68 1.434(3) . ? Cl67 O69 1.438(3) . ? Cl67 O71 1.444(3) . ? Cl67 O70 1.448(3) . ? Cl72 O74 1.388(5) . ? Cl72 O73 1.414(4) . ? Cl72 O76 1.424(4) . ? Cl72 O75 1.445(4) . ? N77 C78 1.116(6) . ? C78 C79 1.438(7) . ? C79 H79A 0.98 . ? C79 H79B 0.98 . ? C79 H79C 0.98 . ? C80 C81 1.484(8) . ? C80 H80A 0.98 . ? C80 H80B 0.98 . ? C80 H80C 0.98 . ? C81 C82 1.477(8) . ? C81 O83 1.482(7) . ? C81 H81 1 . ? C82 H82A 0.98 . ? C82 H82B 0.98 . ? C82 H82C 0.98 . ? O83 C84 1.482(7) . ? C84 C85 1.445(9) . ? C84 C86 1.455(9) . ? C84 H84 1 . ? C85 H85A 0.98 . ? C85 H85B 0.98 . ? C85 H85C 0.98 . ? C86 H86A 0.98 . ? C86 H86B 0.98 . ? C86 H86C 0.98 . ? 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 N54 Fe1 N32 96.01(13) . . ? N54 Fe1 N61 81.88(13) . . ? N32 Fe1 N61 175.97(13) . . ? N54 Fe1 N39 89.40(13) . . ? N32 Fe1 N39 81.85(13) . . ? N61 Fe1 N39 94.67(13) . . ? N54 Fe1 N10 91.42(13) . . ? N32 Fe1 N10 96.58(13) . . ? N61 Fe1 N10 86.93(13) . . ? N39 Fe1 N10 178.29(13) . . ? N54 Fe1 N17 171.47(13) . . ? N32 Fe1 N17 89.91(13) . . ? N61 Fe1 N17 92.56(13) . . ? N39 Fe1 N17 97.53(12) . . ? N10 Fe1 N17 81.78(13) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O3 C2 C1 107.1(4) . . ? O3 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O3 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? C4 O3 C2 117.0(3) . . ? O5 C4 O3 124.5(4) . . ? O5 C4 C6 123.6(4) . . ? O3 C4 C6 111.8(3) . . ? C7 C6 C11 119.4(4) . . ? C7 C6 C4 120.3(4) . . ? C11 C6 C4 120.3(4) . . ? C8 C7 C6 118.6(4) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C7 C8 C9 119.5(4) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? N10 C9 C8 122.0(3) . . ? N10 C9 C12 113.8(3) . . ? C8 C9 C12 124.2(3) . . ? C11 N10 C9 117.9(3) . . ? C11 N10 Fe1 126.7(3) . . ? C9 N10 Fe1 114.9(2) . . ? N10 C11 C6 122.6(4) . . ? N10 C11 H11 118.7 . . ? C6 C11 H11 118.7 . . ? N17 C12 C13 122.5(3) . . ? N17 C12 C9 114.5(3) . . ? C13 C12 C9 123.0(3) . . ? C14 C13 C12 118.9(4) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 119.1(4) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C14 C15 C16 119.2(4) . . ? C14 C15 C18 117.2(4) . . ? C16 C15 C18 123.6(4) . . ? N17 C16 C15 122.4(4) . . ? N17 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C16 N17 C12 117.8(3) . . ? C16 N17 Fe1 127.6(3) . . ? C12 N17 Fe1 114.4(2) . . ? O19 C18 O20 124.7(4) . . ? O19 C18 C15 122.1(4) . . ? O20 C18 C15 113.1(3) . . ? C18 O20 C21 116.3(3) . . ? O20 C21 C22 111.1(3) . . ? O20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? O20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O25 C24 C23 111.8(5) . . ? O25 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? O25 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 107.9 . . ? C26 O25 C24 116.8(4) . . ? O27 C26 O25 124.9(4) . . ? O27 C26 C28 123.6(4) . . ? O25 C26 C28 111.5(4) . . ? C33 C28 C29 118.9(4) . . ? C33 C28 C26 118.0(4) . . ? C29 C28 C26 123.1(4) . . ? C30 C29 C28 119.1(4) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C31 119.6(4) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? N32 C31 C30 121.4(4) . . ? N32 C31 C34 113.9(3) . . ? C30 C31 C34 124.7(3) . . ? C33 N32 C31 118.0(3) . . ? C33 N32 Fe1 126.7(3) . . ? C31 N32 Fe1 115.0(3) . . ? N32 C33 C28 123.1(4) . . ? N32 C33 H33 118.5 . . ? C28 C33 H33 118.5 . . ? N39 C34 C35 121.7(4) . . ? N39 C34 C31 113.8(3) . . ? C35 C34 C31 124.5(4) . . ? C36 C35 C34 119.5(4) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C35 C36 C37 118.8(4) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C36 C37 C38 119.3(4) . . ? C36 C37 C40 119.7(3) . . ? C38 C37 C40 121.0(4) . . ? N39 C38 C37 122.4(4) . . ? N39 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? C38 N39 C34 118.3(3) . . ? C38 N39 Fe1 126.4(3) . . ? C34 N39 Fe1 114.8(3) . . ? O41 C40 O42 124.8(4) . . ? O41 C40 C37 123.9(4) . . ? O42 C40 C37 111.3(3) . . ? C40 O42 C43 116.6(3) . . ? O42 C43 C44 106.5(4) . . ? O42 C43 H43A 110.4 . . ? C44 C43 H43A 110.4 . . ? O42 C43 H43B 110.4 . . ? C44 C43 H43B 110.4 . . ? H43A C43 H43B 108.6 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O47 C46 C45 107.3(4) . . ? O47 C46 H46A 110.2 . . ? C45 C46 H46A 110.2 . . ? O47 C46 H46B 110.3 . . ? C45 C46 H46B 110.3 . . ? H46A C46 H46B 108.5 . . ? C48 O47 C46 116.3(4) . . ? O49 C48 O47 124.4(5) . . ? O49 C48 C50 124.2(4) . . ? O47 C48 C50 111.3(4) . . ? C51 C50 C55 118.5(4) . . ? C51 C50 C48 123.5(4) . . ? C55 C50 C48 118.0(4) . . ? C522 C51 C50 119.6(4) . . ? C522 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? O63 C52 O64 125.0(4) . . ? O63 C52 C59 123.2(4) . . ? O64 C52 C59 111.8(4) . . ? C51 C522 C53 119.1(4) . . ? C51 C522 H522 120.5 . . ? C53 C522 H522 120.5 . . ? N54 C53 C522 121.9(4) . . ? N54 C53 C56 114.2(3) . . ? C522 C53 C56 123.9(4) . . ? C55 N54 C53 118.0(3) . . ? C55 N54 Fe1 127.2(3) . . ? C53 N54 Fe1 114.6(3) . . ? N54 C55 C50 122.8(4) . . ? N54 C55 H55 118.6 . . ? C50 C55 H55 118.6 . . ? N61 C56 C57 121.8(4) . . ? N61 C56 C53 113.9(3) . . ? C57 C56 C53 124.3(3) . . ? C56 C57 C58 119.3(4) . . ? C56 C57 H57 120.4 . . ? C58 C57 H57 120.4 . . ? C59 C58 C57 119.4(4) . . ? C59 C58 H58 120.3 . . ? C57 C58 H58 120.3 . . ? C58 C59 C60 118.4(4) . . ? C58 C59 C52 121.5(4) . . ? C60 C59 C52 120.1(4) . . ? N61 C60 C59 122.8(4) . . ? N61 C60 H60 118.6 . . ? C59 C60 H60 118.6 . . ? C60 N61 C56 118.3(3) . . ? C60 N61 Fe1 126.9(3) . . ? C56 N61 Fe1 114.7(3) . . ? C52 O64 C65 116.0(3) . . ? O64 C65 C66 106.2(4) . . ? O64 C65 H65A 110.5 . . ? C66 C65 H65A 110.5 . . ? O64 C65 H65B 110.5 . . ? C66 C65 H65B 110.5 . . ? H65A C65 H65B 108.7 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O68 Cl67 O69 110.17(19) . . ? O68 Cl67 O71 109.42(19) . . ? O69 Cl67 O71 109.74(17) . . ? O68 Cl67 O70 109.48(18) . . ? O69 Cl67 O70 109.10(19) . . ? O71 Cl67 O70 108.92(17) . . ? O74 Cl72 O73 110.3(4) . . ? O74 Cl72 O76 108.8(3) . . ? O73 Cl72 O76 110.2(2) . . ? O74 Cl72 O75 111.2(4) . . ? O73 Cl72 O75 107.0(2) . . ? O76 Cl72 O75 109.4(3) . . ? N77 C78 C79 179.8(7) . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C81 C80 H80A 109.5 . . ? C81 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C81 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C82 C81 O83 112.8(5) . . ? C82 C81 C80 110.6(6) . . ? O83 C81 C80 106.5(5) . . ? C82 C81 H81 108.9 . . ? O83 C81 H81 108.9 . . ? C80 C81 H81 108.9 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 O83 C81 118.8(5) . . ? C85 C84 C86 116.9(7) . . ? C85 C84 O83 114.6(6) . . ? C86 C84 O83 104.1(5) . . ? C85 C84 H84 106.9 . . ? C86 C84 H84 106.9 . . ? O83 C84 H84 106.9 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 O3 C4 -170.2(4) . . . . ? C2 O3 C4 O5 -6.1(7) . . . . ? C2 O3 C4 C6 176.8(4) . . . . ? O5 C4 C6 C7 -3.8(7) . . . . ? O3 C4 C6 C7 173.3(4) . . . . ? O5 C4 C6 C11 175.9(5) . . . . ? O3 C4 C6 C11 -7.0(6) . . . . ? C11 C6 C7 C8 1.7(6) . . . . ? C4 C6 C7 C8 -178.6(4) . . . . ? C6 C7 C8 C9 0.6(6) . . . . ? C7 C8 C9 N10 -1.8(6) . . . . ? C7 C8 C9 C12 178.0(4) . . . . ? C8 C9 N10 C11 0.7(5) . . . . ? C12 C9 N10 C11 -179.2(3) . . . . ? C8 C9 N10 Fe1 173.6(3) . . . . ? C12 C9 N10 Fe1 -6.3(4) . . . . ? N54 Fe1 N10 C11 4.3(3) . . . . ? N32 Fe1 N10 C11 -91.9(3) . . . . ? N61 Fe1 N10 C11 86.1(3) . . . . ? N39 Fe1 N10 C11 -115(4) . . . . ? N17 Fe1 N10 C11 179.1(3) . . . . ? N54 Fe1 N10 C9 -167.9(3) . . . . ? N32 Fe1 N10 C9 95.9(3) . . . . ? N61 Fe1 N10 C9 -86.1(3) . . . . ? N39 Fe1 N10 C9 73(5) . . . . ? N17 Fe1 N10 C9 6.9(3) . . . . ? C9 N10 C11 C6 1.7(5) . . . . ? Fe1 N10 C11 C6 -170.3(3) . . . . ? C7 C6 C11 N10 -2.9(6) . . . . ? C4 C6 C11 N10 177.4(4) . . . . ? N10 C9 C12 N17 1.0(5) . . . . ? C8 C9 C12 N17 -178.9(4) . . . . ? N10 C9 C12 C13 179.5(4) . . . . ? C8 C9 C12 C13 -0.4(6) . . . . ? N17 C12 C13 C14 -0.8(6) . . . . ? C9 C12 C13 C14 -179.2(4) . . . . ? C12 C13 C14 C15 -1.0(7) . . . . ? C13 C14 C15 C16 1.0(7) . . . . ? C13 C14 C15 C18 -179.1(4) . . . . ? C14 C15 C16 N17 0.9(6) . . . . ? C18 C15 C16 N17 -179.0(4) . . . . ? C15 C16 N17 C12 -2.6(6) . . . . ? C15 C16 N17 Fe1 173.2(3) . . . . ? C13 C12 N17 C16 2.6(6) . . . . ? C9 C12 N17 C16 -178.9(3) . . . . ? C13 C12 N17 Fe1 -173.8(3) . . . . ? C9 C12 N17 Fe1 4.7(4) . . . . ? N54 Fe1 N17 C16 -144.9(8) . . . . ? N32 Fe1 N17 C16 81.0(3) . . . . ? N61 Fe1 N17 C16 -95.8(3) . . . . ? N39 Fe1 N17 C16 -0.7(3) . . . . ? N10 Fe1 N17 C16 177.7(3) . . . . ? N54 Fe1 N17 C12 31.1(11) . . . . ? N32 Fe1 N17 C12 -103.0(3) . . . . ? N61 Fe1 N17 C12 80.2(3) . . . . ? N39 Fe1 N17 C12 175.3(3) . . . . ? N10 Fe1 N17 C12 -6.3(3) . . . . ? C14 C15 C18 O19 1.1(8) . . . . ? C16 C15 C18 O19 -179.0(5) . . . . ? C14 C15 C18 O20 178.3(4) . . . . ? C16 C15 C18 O20 -1.7(7) . . . . ? O19 C18 O20 C21 -3.2(7) . . . . ? C15 C18 O20 C21 179.6(4) . . . . ? C18 O20 C21 C22 -86.3(5) . . . . ? C23 C24 O25 C26 -79.2(6) . . . . ? C24 O25 C26 O27 -0.2(7) . . . . ? C24 O25 C26 C28 178.9(4) . . . . ? O27 C26 C28 C33 13.1(6) . . . . ? O25 C26 C28 C33 -165.9(4) . . . . ? O27 C26 C28 C29 -170.1(4) . . . . ? O25 C26 C28 C29 10.9(6) . . . . ? C33 C28 C29 C30 -0.5(6) . . . . ? C26 C28 C29 C30 -177.2(4) . . . . ? C28 C29 C30 C31 1.5(6) . . . . ? C29 C30 C31 N32 -0.9(6) . . . . ? C29 C30 C31 C34 176.6(4) . . . . ? C30 C31 N32 C33 -0.7(5) . . . . ? C34 C31 N32 C33 -178.5(3) . . . . ? C30 C31 N32 Fe1 173.0(3) . . . . ? C34 C31 N32 Fe1 -4.8(4) . . . . ? N54 Fe1 N32 C33 -98.3(3) . . . . ? N61 Fe1 N32 C33 -156.5(17) . . . . ? N39 Fe1 N32 C33 173.2(3) . . . . ? N10 Fe1 N32 C33 -6.1(3) . . . . ? N17 Fe1 N32 C33 75.6(3) . . . . ? N54 Fe1 N32 C31 88.7(3) . . . . ? N61 Fe1 N32 C31 30(2) . . . . ? N39 Fe1 N32 C31 0.1(2) . . . . ? N10 Fe1 N32 C31 -179.2(3) . . . . ? N17 Fe1 N32 C31 -97.5(3) . . . . ? C31 N32 C33 C28 1.8(5) . . . . ? Fe1 N32 C33 C28 -171.1(3) . . . . ? C29 C28 C33 N32 -1.2(6) . . . . ? C26 C28 C33 N32 175.7(3) . . . . ? N32 C31 C34 N39 8.8(5) . . . . ? C30 C31 C34 N39 -168.9(4) . . . . ? N32 C31 C34 C35 -171.9(3) . . . . ? C30 C31 C34 C35 10.4(6) . . . . ? N39 C34 C35 C36 0.0(6) . . . . ? C31 C34 C35 C36 -179.2(4) . . . . ? C34 C35 C36 C37 0.5(6) . . . . ? C35 C36 C37 C38 -0.8(6) . . . . ? C35 C36 C37 C40 -179.6(3) . . . . ? C36 C37 C38 N39 0.7(6) . . . . ? C40 C37 C38 N39 179.5(3) . . . . ? C37 C38 N39 C34 -0.2(5) . . . . ? C37 C38 N39 Fe1 -171.3(3) . . . . ? C35 C34 N39 C38 -0.2(5) . . . . ? C31 C34 N39 C38 179.1(3) . . . . ? C35 C34 N39 Fe1 172.0(3) . . . . ? C31 C34 N39 Fe1 -8.7(4) . . . . ? N54 Fe1 N39 C38 80.2(3) . . . . ? N32 Fe1 N39 C38 176.3(3) . . . . ? N61 Fe1 N39 C38 -1.6(3) . . . . ? N10 Fe1 N39 C38 -161(4) . . . . ? N17 Fe1 N39 C38 -94.9(3) . . . . ? N54 Fe1 N39 C34 -91.3(3) . . . . ? N32 Fe1 N39 C34 4.9(2) . . . . ? N61 Fe1 N39 C34 -173.1(3) . . . . ? N10 Fe1 N39 C34 28(5) . . . . ? N17 Fe1 N39 C34 93.7(3) . . . . ? C36 C37 C40 O41 -4.7(6) . . . . ? C38 C37 C40 O41 176.6(4) . . . . ? C36 C37 C40 O42 176.0(3) . . . . ? C38 C37 C40 O42 -2.7(5) . . . . ? O41 C40 O42 C43 3.9(6) . . . . ? C37 C40 O42 C43 -176.8(3) . . . . ? C40 O42 C43 C44 176.8(4) . . . . ? C45 C46 O47 C48 166.9(4) . . . . ? C46 O47 C48 O49 -1.7(8) . . . . ? C46 O47 C48 C50 180.0(4) . . . . ? O49 C48 C50 C51 -178.3(5) . . . . ? O47 C48 C50 C51 0.0(6) . . . . ? O49 C48 C50 C55 -0.2(7) . . . . ? O47 C48 C50 C55 178.2(4) . . . . ? C55 C50 C51 C522 1.4(6) . . . . ? C48 C50 C51 C522 179.6(4) . . . . ? C50 C51 C522 C53 -1.1(6) . . . . ? C51 C522 C53 N54 -1.1(6) . . . . ? C51 C522 C53 C56 179.9(4) . . . . ? C522 C53 N54 C55 2.8(5) . . . . ? C56 C53 N54 C55 -178.1(3) . . . . ? C522 C53 N54 Fe1 -171.5(3) . . . . ? C56 C53 N54 Fe1 7.6(4) . . . . ? N32 Fe1 N54 C55 1.8(3) . . . . ? N61 Fe1 N54 C55 178.4(3) . . . . ? N39 Fe1 N54 C55 83.6(3) . . . . ? N10 Fe1 N54 C55 -94.9(3) . . . . ? N17 Fe1 N54 C55 -132.0(9) . . . . ? N32 Fe1 N54 C53 175.5(3) . . . . ? N61 Fe1 N54 C53 -7.9(3) . . . . ? N39 Fe1 N54 C53 -102.7(3) . . . . ? N10 Fe1 N54 C53 78.8(3) . . . . ? N17 Fe1 N54 C53 41.7(10) . . . . ? C53 N54 C55 C50 -2.4(6) . . . . ? Fe1 N54 C55 C50 171.1(3) . . . . ? C51 C50 C55 N54 0.3(6) . . . . ? C48 C50 C55 N54 -177.9(4) . . . . ? N54 C53 C56 N61 -2.0(5) . . . . ? C522 C53 C56 N61 177.1(4) . . . . ? N54 C53 C56 C57 177.7(4) . . . . ? C522 C53 C56 C57 -3.2(6) . . . . ? N61 C56 C57 C58 -0.6(6) . . . . ? C53 C56 C57 C58 179.7(4) . . . . ? C56 C57 C58 C59 0.1(6) . . . . ? C57 C58 C59 C60 1.1(6) . . . . ? C57 C58 C59 C52 -177.4(4) . . . . ? O63 C52 C59 C58 -14.5(6) . . . . ? O64 C52 C59 C58 163.8(4) . . . . ? O63 C52 C59 C60 167.0(4) . . . . ? O64 C52 C59 C60 -14.6(5) . . . . ? C58 C59 C60 N61 -2.0(6) . . . . ? C52 C59 C60 N61 176.5(4) . . . . ? C59 C60 N61 C56 1.5(5) . . . . ? C59 C60 N61 Fe1 -173.8(3) . . . . ? C57 C56 N61 C60 -0.2(5) . . . . ? C53 C56 N61 C60 179.5(3) . . . . ? C57 C56 N61 Fe1 175.7(3) . . . . ? C53 C56 N61 Fe1 -4.6(4) . . . . ? N54 Fe1 N61 C60 -177.7(3) . . . . ? N32 Fe1 N61 C60 -119.1(18) . . . . ? N39 Fe1 N61 C60 -89.0(3) . . . . ? N10 Fe1 N61 C60 90.4(3) . . . . ? N17 Fe1 N61 C60 8.8(3) . . . . ? N54 Fe1 N61 C56 6.8(3) . . . . ? N32 Fe1 N61 C56 65.5(19) . . . . ? N39 Fe1 N61 C56 95.6(3) . . . . ? N10 Fe1 N61 C56 -85.0(3) . . . . ? N17 Fe1 N61 C56 -166.7(3) . . . . ? O63 C52 O64 C65 -6.9(6) . . . . ? C59 C52 O64 C65 174.7(3) . . . . ? C52 O64 C65 C66 -178.8(4) . . . . ? C82 C81 O83 C84 61.3(7) . . . . ? C80 C81 O83 C84 -177.1(5) . . . . ? C81 O83 C84 C85 55.8(8) . . . . ? C81 O83 C84 C86 -175.3(5) . . . . ? data_V2 _database_code_depnum_ccdc_archive 'CCDC 809074' #TrackingRef '- CS_KR_110124_XRD.cif' _audit_creation_date 2010-06-23T13:30:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C78 H84 Fe N15 O9, 4(Cl O4), C2 F3 O2, H2 O, C' _chemical_formula_sum 'C81 H86 Cl4 F3 Fe N15 O28' _chemical_formula_weight 1972.3 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6922(14) _cell_length_b 18.3992(14) _cell_length_c 19.312(2) _cell_angle_alpha 110.059(4) _cell_angle_beta 91.044(6) _cell_angle_gamma 94.961(6) _cell_volume 4547.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7386 _cell_measurement_theta_min 6.323 _cell_measurement_theta_max 63.691 _cell_measurement_wavelength 1.54184 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.206 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.555154E-1 _diffrn_orient_matrix_ub_12 -0.2235E-3 _diffrn_orient_matrix_ub_13 -0.344667E-1 _diffrn_orient_matrix_ub_21 -0.449835E-1 _diffrn_orient_matrix_ub_22 0.121647E-1 _diffrn_orient_matrix_ub_23 0.418314E-1 _diffrn_orient_matrix_ub_31 0.168174E-1 _diffrn_orient_matrix_ub_32 0.56857E-1 _diffrn_orient_matrix_ub_33 0.104411E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_unetI/netI 0.0943 _diffrn_reflns_number 12686 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 6.35 _diffrn_reflns_theta_max 63.32 _diffrn_reflns_theta_full 57.5 _diffrn_measured_fraction_theta_full 0.946 _diffrn_measured_fraction_theta_max 0.855 _reflns_number_total 12686 _reflns_number_gt 7274 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1210P)^2^+33.5712P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 12686 _refine_ls_number_parameters 1232 _refine_ls_number_restraints 249 _refine_ls_R_factor_all 0.1969 _refine_ls_R_factor_gt 0.1204 _refine_ls_wR_factor_ref 0.3305 _refine_ls_wR_factor_gt 0.2774 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.236 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.097 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.19160(12) 0.52483(9) 0.76239(9) 0.0454(5) Uani 1 1 d . . . C1 C 0.1352(8) 0.0239(6) 0.6566(6) 0.054(3) Uani 1 1 d . . . C2 C 0.1616(9) -0.0498(7) 0.6165(7) 0.065(3) Uani 1 1 d . . . H2 H 0.1738 -0.0848 0.6414 0.078 Uiso 1 1 calc R . . C3 C 0.1703(10) -0.0728(7) 0.5406(7) 0.070(4) Uani 1 1 d . . . H3 H 0.1909 -0.1224 0.514 0.084 Uiso 1 1 calc R . . C4 C 0.1492(9) -0.0236(7) 0.5046(7) 0.068(3) Uani 1 1 d . . . H4 H 0.1533 -0.0403 0.4525 0.081 Uiso 1 1 calc R . . C5 C 0.1218(9) 0.0502(7) 0.5418(7) 0.061(3) Uani 1 1 d . . . C6 C 0.1133(8) 0.0725(6) 0.6175(6) 0.051(3) Uani 1 1 d . . . C7 C 0.1010(9) 0.1044(7) 0.5012(7) 0.066(3) Uani 1 1 d . . . H7A H 0.0889 0.1554 0.5377 0.079 Uiso 1 1 calc R . . H7B H 0.0403 0.0832 0.4695 0.079 Uiso 1 1 calc R . . N8 N 0.1836(7) 0.1168(6) 0.4536(5) 0.065(3) Uani 1 1 d . . . H8 H 0.1842 0.0714 0.413 0.078 Uiso 1 1 calc R . . C9 C 0.1625(10) 0.1808(8) 0.4258(8) 0.079(4) Uani 1 1 d . . . H9A H 0.0967 0.1687 0.4001 0.095 Uiso 1 1 calc R . . H9B H 0.1625 0.2302 0.468 0.095 Uiso 1 1 calc R . . C10 C 0.2384(9) 0.1898(8) 0.3739(7) 0.071(4) Uani 1 1 d . . . H10A H 0.2371 0.1409 0.3311 0.085 Uiso 1 1 calc R . . H10B H 0.2235 0.2317 0.3553 0.085 Uiso 1 1 calc R . . N11 N 0.3365(7) 0.2086(5) 0.4116(5) 0.061(3) Uani 1 1 d . . . C12 C 0.3594(9) 0.1457(7) 0.4370(7) 0.067(3) Uani 1 1 d . . . H12A H 0.4261 0.1574 0.4612 0.081 Uiso 1 1 calc R . . H12B H 0.3579 0.0966 0.3944 0.081 Uiso 1 1 calc R . . C13 C 0.2855(8) 0.1365(7) 0.4909(7) 0.063(3) Uani 1 1 d . . . H13A H 0.2875 0.1855 0.5338 0.075 Uiso 1 1 calc R . . H13B H 0.3017 0.0946 0.5091 0.075 Uiso 1 1 calc R . . C14 C 0.4073(9) 0.2240(7) 0.3620(6) 0.063(3) Uani 1 1 d . . . H14A H 0.3903 0.2695 0.3497 0.076 Uiso 1 1 calc R . . H14B H 0.4035 0.1786 0.3156 0.076 Uiso 1 1 calc R . . C15 C 0.5124(9) 0.2399(7) 0.3958(7) 0.061(3) Uani 1 1 d . . . C16 C 0.5833(12) 0.1920(8) 0.3627(8) 0.080(4) Uani 1 1 d . . . H16 H 0.5668 0.1494 0.3183 0.096 Uiso 1 1 calc R . . C17 C 0.6762(12) 0.2053(11) 0.3931(10) 0.098(5) Uani 1 1 d . . . H17 H 0.7244 0.1724 0.3692 0.117 Uiso 1 1 calc R . . C18 C 0.7016(11) 0.2655(10) 0.4578(10) 0.089(4) Uani 1 1 d . . . H18 H 0.7664 0.2727 0.4791 0.107 Uiso 1 1 calc R . . C19 C 0.6336(8) 0.3162(7) 0.4926(7) 0.060(3) Uani 1 1 d . . . C20 C 0.5400(8) 0.3023(7) 0.4602(7) 0.056(3) Uani 1 1 d . . . C21 C 0.6623(10) 0.3839(8) 0.5618(7) 0.073(4) Uani 1 1 d . . . H21A H 0.6037 0.4117 0.5792 0.088 Uiso 1 1 calc R . . H21B H 0.7111 0.4204 0.5501 0.088 Uiso 1 1 calc R . . N22 N 0.7054(7) 0.3614(6) 0.6239(6) 0.071(3) Uani 1 1 d . . . H22 H 0.7622 0.3379 0.6077 0.086 Uiso 1 1 calc R . . C23 C 0.7334(10) 0.4326(7) 0.6879(7) 0.073(4) Uani 1 1 d . . . H23A H 0.6749 0.4612 0.7033 0.088 Uiso 1 1 calc R . . H23B H 0.7827 0.4667 0.6734 0.088 Uiso 1 1 calc R . . C24 C 0.7752(9) 0.4144(8) 0.7520(8) 0.079(4) Uani 1 1 d . . . H24A H 0.8369 0.3898 0.7384 0.095 Uiso 1 1 calc R . . H24B H 0.7904 0.4631 0.7947 0.095 Uiso 1 1 calc R . . N25 N 0.7048(7) 0.3618(6) 0.7724(6) 0.067(3) Uani 1 1 d . . . C26 C 0.6841(9) 0.2895(7) 0.7105(7) 0.068(3) Uani 1 1 d . . . H26A H 0.6385 0.2531 0.7251 0.081 Uiso 1 1 calc R . . H26B H 0.7456 0.265 0.6959 0.081 Uiso 1 1 calc R . . C27 C 0.6385(9) 0.3058(7) 0.6463(7) 0.067(3) Uani 1 1 d . . . H27A H 0.6247 0.2566 0.6041 0.08 Uiso 1 1 calc R . . H27B H 0.5754 0.3281 0.6604 0.08 Uiso 1 1 calc R . . C28 C 0.7444(9) 0.3489(8) 0.8392(7) 0.072(4) Uani 1 1 d . . . H28A H 0.8083 0.3273 0.8278 0.086 Uiso 1 1 calc R . . H28B H 0.757 0.4 0.8792 0.086 Uiso 1 1 calc R . . C29 C 0.6813(9) 0.2964(8) 0.8675(7) 0.068(3) Uani 1 1 d . . . C30 C 0.7169(10) 0.2324(9) 0.8777(10) 0.097(5) Uani 1 1 d . . . H30 H 0.7821 0.2214 0.8653 0.116 Uiso 1 1 calc R . . C31 C 0.6606(11) 0.1845(11) 0.9052(11) 0.118(7) Uani 1 1 d . . . H31 H 0.688 0.1421 0.9133 0.141 Uiso 1 1 calc R . . C32 C 0.5670(9) 0.1969(9) 0.9209(9) 0.093(5) Uani 1 1 d . . . H32 H 0.5278 0.1617 0.9375 0.112 Uiso 1 1 calc R . . C33 C 0.5265(8) 0.2612(7) 0.9130(7) 0.065(3) Uani 1 1 d . . . C34 C 0.5857(9) 0.3108(7) 0.8877(7) 0.067(3) Uani 1 1 d . . . C35 C 0.4202(8) 0.2719(6) 0.9291(7) 0.061(3) Uani 1 1 d . . . H35A H 0.4008 0.3157 0.915 0.073 Uiso 1 1 calc R . . H35B H 0.4123 0.2854 0.9828 0.073 Uiso 1 1 calc R . . N36 N 0.3533(6) 0.1992(6) 0.8878(5) 0.061(3) Uani 1 1 d . . . H36 H 0.3641 0.1618 0.9086 0.073 Uiso 1 1 calc R . . C37 C 0.2477(8) 0.2149(7) 0.8963(6) 0.061(3) Uani 1 1 d . . . H37A H 0.235 0.2562 0.8762 0.073 Uiso 1 1 calc R . . H37B H 0.2341 0.2337 0.9493 0.073 Uiso 1 1 calc R . . C38 C 0.1802(9) 0.1429(7) 0.8566(6) 0.063(3) Uani 1 1 d . . . H38A H 0.1913 0.1018 0.8773 0.075 Uiso 1 1 calc R . . H38B H 0.1111 0.1546 0.8635 0.075 Uiso 1 1 calc R . . N39 N 0.1984(6) 0.1158(5) 0.7788(5) 0.054(2) Uani 1 1 d . . . C40 C 0.2994(9) 0.0959(7) 0.7688(7) 0.064(3) Uani 1 1 d . . . H40A H 0.3115 0.0761 0.7155 0.077 Uiso 1 1 calc R . . H40B H 0.3095 0.0542 0.789 0.077 Uiso 1 1 calc R . . C41 C 0.3709(9) 0.1660(7) 0.8074(7) 0.066(3) Uani 1 1 d . . . H41A H 0.4387 0.1509 0.8011 0.08 Uiso 1 1 calc R . . H41B H 0.3641 0.206 0.7846 0.08 Uiso 1 1 calc R . . C42 C 0.1267(9) 0.0484(6) 0.7382(6) 0.058(3) Uani 1 1 d . . . H42A H 0.0594 0.0625 0.7505 0.07 Uiso 1 1 calc R . . H42B H 0.1378 0.0042 0.7546 0.07 Uiso 1 1 calc R . . N43 N 0.0831(6) 0.1469(5) 0.6581(5) 0.051(2) Uani 1 1 d . . . H43 H 0.0216 0.1509 0.6702 0.062 Uiso 1 1 calc R . . C44 C 0.1464(10) 0.2105(6) 0.6779(6) 0.056(3) Uani 1 1 d . . . O45 O 0.2283(6) 0.2124(4) 0.6550(5) 0.066(2) Uani 1 1 d . . . C46 C 0.1103(8) 0.2844(6) 0.7291(6) 0.052(3) Uani 1 1 d . . . C47 C 0.0437(8) 0.2891(6) 0.7830(6) 0.053(3) Uani 1 1 d . . . H47 H 0.0114 0.2437 0.7883 0.064 Uiso 1 1 calc R . . C48 C 0.0260(8) 0.3624(6) 0.8286(6) 0.053(3) Uani 1 1 d . . . H48 H -0.0183 0.3672 0.8669 0.063 Uiso 1 1 calc R . . C49 C 0.0700(7) 0.4282(6) 0.8204(6) 0.045(3) Uani 1 1 d . . . N50 N 0.1350(6) 0.4235(5) 0.7659(5) 0.050(2) Uani 1 1 d . . . C51 C 0.1533(7) 0.3528(7) 0.7232(6) 0.050(3) Uani 1 1 d . . . H51 H 0.1991 0.3488 0.686 0.059 Uiso 1 1 calc R . . C52 C 0.0610(8) 0.5066(7) 0.8681(6) 0.051(3) Uani 1 1 d . . . C53 C -0.0084(8) 0.5266(7) 0.9226(6) 0.054(3) Uani 1 1 d . . . H53 H -0.0542 0.4877 0.9288 0.065 Uiso 1 1 calc R . . C54 C -0.0092(8) 0.6030(7) 0.9668(6) 0.054(3) Uani 1 1 d . . . H54 H -0.057 0.6178 1.0028 0.064 Uiso 1 1 calc R . . C55 C 0.0606(8) 0.6586(7) 0.9585(7) 0.056(3) Uani 1 1 d . . . C56 C 0.1245(8) 0.6362(6) 0.9039(6) 0.046(3) Uani 1 1 d . . . H56 H 0.1712 0.6747 0.8982 0.055 Uiso 1 1 calc R . . N57 N 0.1254(6) 0.5626(5) 0.8574(5) 0.048(2) Uani 1 1 d . . . C58 C 0.0570(10) 0.7411(8) 1.0073(8) 0.066(3) Uani 1 1 d . . . O59 O 0.0145(7) 0.7605(5) 1.0642(6) 0.083(3) Uani 1 1 d . . . O60 O 0.1073(6) 0.7898(5) 0.9811(5) 0.072(2) Uani 1 1 d . B . C61 C 0.1082(13) 0.8716(8) 1.0238(10) 0.098(5) Uani 1 1 d . . . H61A H 0.143 0.8833 1.0724 0.117 Uiso 0.58 1 calc PR A 1 H61B H 0.0402 0.8857 1.0321 0.117 Uiso 0.58 1 calc PR A 1 H61C H 0.1087 0.8773 1.0767 0.117 Uiso 0.42 1 calc PR A 2 H61D H 0.1707 0.8983 1.0158 0.117 Uiso 0.42 1 calc PR A 2 C62A C 0.159(2) 0.9159(14) 0.9827(16) 0.108(10) Uani 0.58 1 d P B 1 H62A H 0.1582 0.9716 1.0101 0.129 Uiso 0.58 1 calc PR B 1 H62B H 0.1246 0.9029 0.9342 0.129 Uiso 0.58 1 calc PR B 1 H62C H 0.2264 0.9028 0.9762 0.129 Uiso 0.58 1 calc PR B 1 C62B C 0.035(3) 0.909(2) 1.010(3) 0.120(15) Uani 0.42 1 d P B 2 H62D H 0.045 0.9638 1.0409 0.145 Uiso 0.42 1 calc PR B 2 H62E H -0.0276 0.8858 1.0212 0.145 Uiso 0.42 1 calc PR B 2 H62F H 0.0327 0.9039 0.9578 0.145 Uiso 0.42 1 calc PR B 2 N63 N 0.4694(6) 0.3558(5) 0.4907(5) 0.051(2) Uani 1 1 d . . . H63 H 0.4623 0.3925 0.4719 0.061 Uiso 1 1 calc R . . C64 C 0.4118(8) 0.3536(7) 0.5473(6) 0.054(3) Uani 1 1 d . . . O65 O 0.4222(5) 0.3096(4) 0.5811(4) 0.0549(19) Uani 1 1 d . . . C66 C 0.3319(7) 0.4075(6) 0.5644(6) 0.048(3) Uani 1 1 d . . . C67 C 0.2831(8) 0.4288(7) 0.5113(6) 0.056(3) Uani 1 1 d . . . H67 H 0.3009 0.413 0.4614 0.067 Uiso 1 1 calc R . . C68 C 0.2062(8) 0.4749(7) 0.5365(6) 0.059(3) Uani 1 1 d . . . H68 H 0.1683 0.4895 0.5026 0.071 Uiso 1 1 calc R . . C69 C 0.1848(8) 0.4996(6) 0.6103(6) 0.050(3) Uani 1 1 d . . . N70 N 0.2362(6) 0.4815(5) 0.6616(4) 0.045(2) Uani 1 1 d . . . C71 C 0.3087(8) 0.4364(6) 0.6375(6) 0.049(3) Uani 1 1 d . . . H71 H 0.3464 0.4236 0.6727 0.059 Uiso 1 1 calc R . . C72 C 0.0974(8) 0.5384(6) 0.6385(6) 0.052(3) Uani 1 1 d . . . C73 C 0.0392(8) 0.5721(6) 0.5992(6) 0.055(3) Uani 1 1 d . . . H73 H 0.0552 0.5702 0.551 0.065 Uiso 1 1 calc R . . C74 C -0.0408(9) 0.6078(7) 0.6313(7) 0.061(3) Uani 1 1 d . . . H74 H -0.0783 0.6336 0.6066 0.073 Uiso 1 1 calc R . . C75 C -0.0664(7) 0.6061(6) 0.6994(6) 0.052(3) Uani 1 1 d . . . C76 C -0.0053(7) 0.5708(6) 0.7339(6) 0.045(3) Uani 1 1 d . . . H76 H -0.0231 0.5686 0.7805 0.054 Uiso 1 1 calc R . . N77 N 0.0754(7) 0.5403(5) 0.7067(5) 0.049(2) Uani 1 1 d . . . C78 C -0.1476(8) 0.6484(8) 0.7374(7) 0.062(3) Uani 1 1 d . . . O79 O -0.1786(6) 0.7012(6) 0.7213(5) 0.087(3) Uani 1 1 d . . . O80 O -0.1753(6) 0.6294(5) 0.7942(5) 0.069(2) Uani 1 1 d . . . C81 C -0.2420(10) 0.6793(10) 0.8437(9) 0.091(5) Uani 1 1 d . . . H81A H -0.2821 0.6488 0.8683 0.109 Uiso 1 1 calc R . . H81B H -0.2869 0.6988 0.8149 0.109 Uiso 1 1 calc R . . C82 C -0.1827(13) 0.7468(12) 0.9009(9) 0.120(6) Uani 1 1 d . . . H82A H -0.227 0.7795 0.9346 0.18 Uiso 1 1 calc R . . H82B H -0.1446 0.7777 0.8764 0.18 Uiso 1 1 calc R . . H82C H -0.1379 0.7272 0.929 0.18 Uiso 1 1 calc R . . N83 N 0.5481(6) 0.3817(5) 0.8861(5) 0.058(2) Uani 1 1 d . . . H83 H 0.5658 0.4256 0.9223 0.069 Uiso 1 1 calc R . . C84 C 0.4868(8) 0.3824(8) 0.8306(7) 0.056(3) Uani 1 1 d . . . O85 O 0.4549(6) 0.3242(5) 0.7806(5) 0.062(2) Uani 1 1 d . . . C86 C 0.4556(8) 0.4604(6) 0.8368(6) 0.048(3) Uani 1 1 d . . . C87 C 0.5129(8) 0.5319(7) 0.8639(6) 0.053(3) Uani 1 1 d . . . H87 H 0.5768 0.5355 0.8856 0.063 Uiso 1 1 calc R . . C88 C 0.4753(8) 0.5969(7) 0.8588(6) 0.054(3) Uani 1 1 d . . . H88 H 0.5138 0.6457 0.876 0.065 Uiso 1 1 calc R . . C89 C 0.3811(7) 0.5908(6) 0.8286(5) 0.043(2) Uani 1 1 d . . . N90 N 0.3223(6) 0.5228(5) 0.8067(4) 0.044(2) Uani 1 1 d . . . C91 C 0.3591(7) 0.4589(6) 0.8107(6) 0.048(3) Uani 1 1 d . . . H91 H 0.3183 0.4112 0.7952 0.057 Uiso 1 1 calc R . . C92 C 0.3370(8) 0.6549(6) 0.8149(6) 0.050(3) Uani 1 1 d . . . C93 C 0.3808(8) 0.7304(7) 0.8357(6) 0.057(3) Uani 1 1 d . . . H93 H 0.4445 0.7437 0.8594 0.068 Uiso 1 1 calc R . . C94 C 0.3309(9) 0.7858(7) 0.8217(7) 0.062(3) Uani 1 1 d . . . H94 H 0.3592 0.8382 0.8368 0.075 Uiso 1 1 calc R . . C95 C 0.2390(8) 0.7648(6) 0.7854(6) 0.051(3) Uani 1 1 d . . . C96 C 0.2025(8) 0.6878(6) 0.7635(6) 0.051(3) Uani 1 1 d . . . H96 H 0.1407 0.6731 0.7368 0.061 Uiso 1 1 calc R . . N97 N 0.2480(6) 0.6321(5) 0.7772(5) 0.050(2) Uani 1 1 d . . . C98 C 0.1802(9) 0.8231(7) 0.7717(7) 0.064(3) Uani 1 1 d . . . O99 O 0.2120(6) 0.8871(5) 0.7748(5) 0.070(2) Uani 1 1 d . . . O100 O 0.0853(6) 0.7949(5) 0.7548(5) 0.076(3) Uani 1 1 d . . . C101 C 0.0176(10) 0.8443(8) 0.7383(9) 0.083(4) Uani 1 1 d . . . H10C H -0.0375 0.8108 0.7057 0.099 Uiso 1 1 calc R . . H10D H 0.0521 0.8744 0.7107 0.099 Uiso 1 1 calc R . . C102 C -0.0222(12) 0.8982(11) 0.8032(11) 0.123(7) Uani 1 1 d . . . H10E H -0.0675 0.9289 0.7879 0.184 Uiso 1 1 calc R . . H10F H 0.0315 0.9331 0.8349 0.184 Uiso 1 1 calc R . . H10G H -0.0574 0.869 0.8306 0.184 Uiso 1 1 calc R . . Cl1A Cl 0.2654(2) 0.45955(18) 0.98657(16) 0.0643(8) Uani 1 1 d D . . O2A O 0.2493(6) 0.4343(6) 1.0481(4) 0.105(4) Uani 1 1 d D . . O3A O 0.2368(6) 0.3974(4) 0.9190(4) 0.087(3) Uani 1 1 d D . . O4A O 0.3678(5) 0.4837(5) 0.9866(4) 0.082(3) Uani 1 1 d D . . O5A O 0.2082(7) 0.5229(5) 0.9937(5) 0.102(3) Uani 1 1 d D . . Cl1B Cl 0.9611(3) 0.3249(2) 0.5506(2) 0.0948(12) Uani 1 1 d DU . . O2B O 0.9604(6) 0.2810(5) 0.4704(4) 0.090(3) Uani 1 1 d DU . . O3B O 1.0611(5) 0.3344(7) 0.5820(6) 0.134(4) Uani 1 1 d DU . . O4B O 0.9205(6) 0.4008(4) 0.5624(5) 0.088(3) Uani 1 1 d DU . . O5B O 0.8935(7) 0.2839(6) 0.5869(6) 0.127(4) Uani 1 1 d DU . . Cl1C Cl 0.5327(3) 0.5682(2) 0.66361(18) 0.0815(10) Uani 1 1 d D . . O2C O 0.5161(5) 0.5040(4) 0.6893(4) 0.074(2) Uani 1 1 d D C . O3C O 0.4926(14) 0.6356(6) 0.7087(9) 0.106(6) Uani 0.586(11) 1 d PDU C 1 O4C O 0.6387(7) 0.5889(8) 0.6651(9) 0.099(5) Uani 0.586(11) 1 d PDU C 1 O5C O 0.5053(12) 0.5390(8) 0.5864(5) 0.085(5) Uani 0.586(11) 1 d PDU C 1 O6C O 0.5870(16) 0.5517(10) 0.6001(9) 0.101(6) Uani 0.414(11) 1 d PDU C 2 O7C O 0.4377(9) 0.5905(11) 0.6457(12) 0.092(6) Uani 0.414(11) 1 d PDU C 2 O8C O 0.5690(17) 0.6349(8) 0.7262(8) 0.108(7) Uani 0.414(11) 1 d PDU C 2 Cl1D Cl 0.1594(4) -0.0621(3) 0.2819(3) 0.154(2) Uani 1 1 d D . . O2D O 0.1729(14) -0.0560(9) 0.2072(6) 0.263(12) Uani 1 1 d DU . . O3D O 0.1069(7) -0.1379(5) 0.2689(7) 0.136(5) Uani 1 1 d DU . . O4D O 0.2621(8) -0.0589(11) 0.3096(12) 0.356(18) Uani 1 1 d DU . . O5D O 0.1061(7) -0.0022(5) 0.3304(5) 0.111(4) Uani 1 1 d DU . . O1E O 0.3565(8) 0.1045(6) 0.9699(6) 0.106(4) Uani 1 1 d D . . C2E C 0.3868(12) 0.1351(11) 1.0330(10) 0.091(5) Uani 1 1 d D . . O3E O 0.4160(7) 0.2055(7) 1.0652(6) 0.101(3) Uani 1 1 d D . . C4E C 0.3790(10) 0.0859(10) 1.0789(9) 0.211(7) Uani 1 1 d DU . . F5E F 0.3861(11) 0.0099(8) 1.0452(8) 0.217(6) Uani 1 1 d DU . . F6E F 0.2945(11) 0.0867(9) 1.1130(9) 0.232(7) Uani 1 1 d DU . . F7E F 0.4473(11) 0.1064(8) 1.1342(8) 0.231(7) Uani 1 1 d DU . . O1F O 0.4379(11) 0.1780(9) 0.6432(8) 0.160(5) Uani 1 1 d . . . H1FA H 0.48 0.225 0.6595 0.5 Uiso 1 1 d . . . H1FB H 0.3708 0.19 0.646 0.5 Uiso 1 1 d . . . C103 C 0.580(4) 0.101(4) 0.534(3) 0.092(17) Uiso 0.25 1 d P D 1 C104 C 0.485(4) 0.042(3) 0.528(3) 0.081 Uiso 0.25 1 d P . 2 C105 C 0.451(6) 0.018(4) 0.603(4) 0.12(2) Uiso 0.25 1 d P E 3 C106 C 0.532(5) 0.009(4) 0.743(4) 0.11(2) Uiso 0.25 1 d P F 4 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 0.0425(10) 0.0473(10) 0.0530(10) 0.0258(8) -0.0002(8) 0.0050(7) C1 0.058(7) 0.041(7) 0.068(8) 0.025(6) 0.002(6) 0.004(5) C2 0.078(9) 0.050(8) 0.075(9) 0.030(7) 0.020(7) 0.010(6) C3 0.097(10) 0.045(7) 0.070(9) 0.019(7) 0.021(7) 0.017(7) C4 0.078(9) 0.058(8) 0.066(8) 0.025(7) -0.009(6) -0.012(6) C5 0.077(9) 0.045(7) 0.057(8) 0.017(6) -0.012(6) -0.003(6) C6 0.050(7) 0.038(6) 0.062(8) 0.016(6) -0.003(5) 0.001(5) C7 0.064(8) 0.067(8) 0.072(8) 0.038(7) -0.012(6) -0.010(6) N8 0.078(7) 0.059(6) 0.063(6) 0.031(5) -0.015(5) -0.005(5) C9 0.075(9) 0.083(9) 0.097(10) 0.060(8) -0.019(8) -0.011(7) C10 0.073(9) 0.080(9) 0.075(9) 0.051(7) -0.019(7) -0.011(7) N11 0.064(6) 0.066(6) 0.065(6) 0.040(5) -0.001(5) 0.004(5) C12 0.077(9) 0.059(8) 0.074(8) 0.032(7) -0.003(7) 0.012(6) C13 0.068(8) 0.060(8) 0.066(8) 0.035(6) -0.018(6) -0.007(6) C14 0.076(9) 0.063(8) 0.055(7) 0.024(6) 0.003(6) 0.012(6) C15 0.076(9) 0.060(8) 0.058(8) 0.028(7) 0.009(7) 0.024(7) C16 0.101(12) 0.069(9) 0.082(10) 0.034(8) 0.023(9) 0.040(9) C17 0.074(11) 0.121(15) 0.114(14) 0.050(12) 0.035(10) 0.051(10) C18 0.071(10) 0.100(12) 0.101(12) 0.034(10) -0.005(9) 0.031(9) C19 0.037(7) 0.072(8) 0.082(9) 0.040(7) 0.009(6) 0.009(6) C20 0.056(8) 0.061(8) 0.063(8) 0.034(7) 0.022(6) 0.019(6) C21 0.072(9) 0.077(9) 0.090(10) 0.055(8) -0.007(7) 0.005(7) N22 0.056(6) 0.078(7) 0.090(8) 0.045(7) -0.009(5) -0.002(5) C23 0.078(9) 0.066(9) 0.078(9) 0.034(8) -0.021(7) -0.015(7) C24 0.062(8) 0.080(9) 0.105(11) 0.049(8) -0.021(7) -0.015(7) N25 0.061(6) 0.075(7) 0.074(7) 0.042(6) -0.016(5) -0.006(5) C26 0.051(7) 0.070(9) 0.093(10) 0.044(8) 0.001(7) 0.002(6) C27 0.058(8) 0.070(8) 0.077(9) 0.036(7) -0.001(6) -0.011(6) C28 0.049(7) 0.081(9) 0.097(10) 0.047(8) -0.007(7) 0.010(6) C29 0.044(7) 0.089(10) 0.082(9) 0.046(8) -0.010(6) 0.002(6) C30 0.051(8) 0.107(12) 0.163(15) 0.082(12) -0.006(9) 0.022(8) C31 0.066(11) 0.142(15) 0.198(19) 0.126(15) -0.012(11) 0.018(10) C32 0.045(8) 0.112(12) 0.166(15) 0.099(12) 0.003(8) 0.018(7) C33 0.050(7) 0.074(9) 0.089(9) 0.050(7) -0.009(6) 0.008(6) C34 0.069(9) 0.070(8) 0.075(8) 0.044(7) -0.022(7) -0.005(7) C35 0.068(8) 0.049(7) 0.070(8) 0.028(6) -0.009(6) 0.005(6) N36 0.051(6) 0.071(7) 0.069(7) 0.032(6) 0.004(5) 0.016(5) C37 0.064(8) 0.067(8) 0.056(7) 0.025(6) 0.004(6) 0.007(6) C38 0.062(8) 0.069(8) 0.066(8) 0.032(7) 0.012(6) 0.017(6) N39 0.052(6) 0.048(6) 0.063(6) 0.020(5) 0.004(5) 0.009(4) C40 0.064(8) 0.057(8) 0.075(8) 0.024(7) 0.009(6) 0.022(6) C41 0.064(8) 0.058(8) 0.080(9) 0.026(7) 0.009(7) 0.009(6) C42 0.076(8) 0.049(7) 0.058(7) 0.028(6) 0.004(6) 0.009(6) N43 0.050(5) 0.046(6) 0.065(6) 0.027(5) 0.003(4) 0.009(4) C44 0.068(9) 0.040(7) 0.062(8) 0.024(6) -0.005(6) -0.007(6) O45 0.061(6) 0.051(5) 0.086(6) 0.024(4) 0.011(5) 0.002(4) C46 0.055(7) 0.041(7) 0.063(7) 0.026(6) -0.015(6) 0.000(5) C47 0.048(7) 0.046(7) 0.066(8) 0.023(6) 0.008(6) 0.001(5) C48 0.050(7) 0.051(7) 0.062(7) 0.028(6) 0.002(5) 0.001(5) C49 0.040(6) 0.050(7) 0.048(6) 0.021(6) 0.002(5) 0.007(5) N50 0.051(6) 0.043(6) 0.055(6) 0.016(5) -0.012(5) 0.012(4) C51 0.035(6) 0.063(8) 0.058(7) 0.031(6) 0.001(5) 0.001(5) C52 0.040(6) 0.060(8) 0.061(7) 0.034(6) -0.005(5) -0.002(5) C53 0.055(7) 0.048(7) 0.067(8) 0.029(6) -0.001(6) 0.003(5) C54 0.046(7) 0.066(8) 0.053(7) 0.025(6) 0.008(5) 0.009(6) C55 0.047(7) 0.064(8) 0.067(8) 0.036(7) 0.008(6) 0.009(6) C56 0.050(7) 0.037(7) 0.055(7) 0.024(6) -0.009(5) -0.002(5) N57 0.043(5) 0.051(6) 0.059(6) 0.030(5) -0.007(4) 0.005(4) C58 0.063(9) 0.070(9) 0.073(9) 0.036(8) -0.004(7) 0.004(7) O59 0.087(7) 0.074(6) 0.086(7) 0.022(5) 0.026(6) 0.012(5) O60 0.077(6) 0.055(5) 0.086(6) 0.025(5) 0.005(5) 0.009(4) C61 0.105(13) 0.062(10) 0.126(14) 0.031(10) 0.013(10) 0.012(9) C62A 0.14(3) 0.059(16) 0.13(2) 0.042(16) -0.03(2) -0.003(16) C62B 0.13(4) 0.08(3) 0.17(4) 0.06(3) 0.02(3) 0.03(3) N63 0.057(6) 0.053(6) 0.052(6) 0.028(5) 0.009(5) 0.007(5) C64 0.044(7) 0.064(8) 0.056(7) 0.024(6) -0.007(5) 0.004(6) O65 0.049(4) 0.059(5) 0.069(5) 0.036(4) 0.005(4) 0.011(4) C66 0.042(6) 0.047(6) 0.058(7) 0.022(6) 0.001(5) 0.005(5) C67 0.053(7) 0.070(8) 0.047(7) 0.024(6) 0.001(5) 0.008(6) C68 0.057(8) 0.066(8) 0.064(8) 0.034(7) 0.001(6) 0.011(6) C69 0.050(7) 0.057(7) 0.044(7) 0.015(6) 0.004(5) 0.014(5) N70 0.047(5) 0.046(5) 0.047(5) 0.022(4) -0.004(4) 0.006(4) C71 0.052(7) 0.053(7) 0.047(7) 0.024(6) 0.003(5) 0.007(6) C72 0.061(7) 0.049(7) 0.051(7) 0.022(6) -0.009(6) 0.005(6) C73 0.056(7) 0.064(8) 0.051(7) 0.029(6) -0.003(6) 0.008(6) C74 0.058(8) 0.066(8) 0.067(8) 0.031(7) -0.002(6) 0.017(6) C75 0.038(6) 0.063(7) 0.061(7) 0.031(6) -0.003(5) 0.007(5) C76 0.039(6) 0.043(6) 0.057(7) 0.022(5) 0.002(5) 0.000(5) N77 0.054(6) 0.044(5) 0.051(6) 0.021(4) -0.003(4) 0.004(4) C78 0.043(7) 0.084(9) 0.076(9) 0.049(8) 0.000(6) 0.005(6) O79 0.072(6) 0.120(8) 0.105(7) 0.079(7) 0.026(5) 0.041(6) O80 0.056(5) 0.079(6) 0.085(6) 0.044(5) 0.008(4) 0.020(4) C81 0.061(9) 0.142(14) 0.108(12) 0.083(12) 0.046(9) 0.053(10) C82 0.118(15) 0.167(18) 0.072(11) 0.034(12) 0.011(10) 0.028(13) N83 0.053(6) 0.062(6) 0.068(6) 0.034(5) -0.006(5) 0.013(5) C84 0.043(7) 0.072(9) 0.067(8) 0.039(7) -0.001(6) 0.012(6) O85 0.060(5) 0.055(5) 0.072(5) 0.023(5) -0.018(4) 0.007(4) C86 0.051(7) 0.050(7) 0.051(6) 0.026(5) -0.007(5) 0.007(5) C87 0.046(7) 0.070(8) 0.048(6) 0.029(6) -0.006(5) -0.001(6) C88 0.051(7) 0.054(7) 0.066(7) 0.033(6) -0.006(6) 0.009(5) C89 0.047(6) 0.045(6) 0.038(6) 0.014(5) 0.003(5) 0.009(5) N90 0.051(5) 0.041(5) 0.044(5) 0.018(4) 0.006(4) 0.004(4) C91 0.047(7) 0.048(7) 0.050(7) 0.022(5) -0.002(5) 0.002(5) C92 0.050(7) 0.052(7) 0.054(7) 0.027(6) 0.001(5) 0.002(5) C93 0.047(7) 0.060(8) 0.072(8) 0.035(6) -0.005(6) -0.003(6) C94 0.061(8) 0.057(7) 0.079(9) 0.037(7) -0.001(6) 0.000(6) C95 0.057(7) 0.034(6) 0.071(8) 0.030(6) 0.001(6) -0.003(5) C96 0.054(7) 0.056(7) 0.052(7) 0.031(6) -0.001(5) 0.010(6) N97 0.045(5) 0.061(6) 0.051(5) 0.029(5) 0.000(4) 0.008(4) C98 0.065(9) 0.059(8) 0.078(9) 0.035(7) -0.004(6) 0.005(7) O99 0.066(5) 0.052(5) 0.103(7) 0.042(5) -0.008(5) 0.000(4) O100 0.067(6) 0.060(5) 0.116(7) 0.050(5) -0.019(5) -0.001(4) C101 0.065(9) 0.061(9) 0.143(14) 0.062(9) -0.019(9) 0.006(7) C102 0.090(12) 0.142(17) 0.180(19) 0.100(16) 0.029(12) 0.055(12) Cl1A 0.0536(18) 0.082(2) 0.070(2) 0.0440(18) -0.0049(14) 0.0004(15) O2A 0.072(6) 0.175(10) 0.101(7) 0.098(8) -0.008(5) -0.018(6) O3A 0.088(7) 0.076(6) 0.092(7) 0.030(5) -0.027(5) -0.013(5) O4A 0.047(5) 0.121(8) 0.074(6) 0.035(5) 0.002(4) -0.018(5) O5A 0.112(8) 0.124(9) 0.085(7) 0.047(6) -0.008(6) 0.058(7) Cl1B 0.087(3) 0.112(3) 0.101(3) 0.062(2) -0.016(2) -0.009(2) O2B 0.083(6) 0.124(8) 0.059(5) 0.027(5) 0.002(5) 0.015(5) O3B 0.066(6) 0.193(11) 0.143(9) 0.063(8) -0.038(6) -0.003(7) O4B 0.091(6) 0.082(6) 0.099(7) 0.041(5) 0.004(5) 0.011(5) O5B 0.107(8) 0.168(10) 0.138(9) 0.105(8) 0.005(7) -0.038(7) Cl1C 0.101(3) 0.077(2) 0.072(2) 0.0407(19) -0.0101(19) -0.0189(19) O2C 0.079(6) 0.078(6) 0.078(6) 0.045(5) 0.008(5) -0.001(5) O3C 0.131(14) 0.085(10) 0.123(12) 0.052(9) 0.067(11) 0.045(10) O4C 0.099(11) 0.102(11) 0.110(11) 0.062(9) -0.008(9) -0.023(9) O5C 0.116(12) 0.085(9) 0.071(9) 0.055(7) -0.005(8) -0.009(9) O6C 0.127(15) 0.110(12) 0.091(12) 0.066(10) 0.031(12) 0.008(12) O7C 0.117(14) 0.069(12) 0.109(13) 0.052(10) 0.023(11) 0.023(10) O8C 0.118(15) 0.100(12) 0.112(13) 0.049(11) 0.018(13) -0.008(12) Cl1D 0.146(5) 0.155(5) 0.147(5) 0.035(4) -0.020(4) 0.010(4) O2D 0.48(4) 0.219(19) 0.125(13) 0.104(13) -0.032(17) 0.06(2) O3D 0.095(8) 0.070(7) 0.200(13) 0.001(7) 0.034(8) -0.038(6) O4D 0.130(15) 0.45(4) 0.55(4) 0.30(3) -0.19(2) -0.137(19) O5D 0.113(8) 0.077(7) 0.105(8) -0.021(6) 0.049(7) 0.020(6) O1E 0.116(9) 0.110(8) 0.104(8) 0.064(7) -0.035(7) -0.023(6) C2E 0.085(11) 0.102(13) 0.088(12) 0.042(10) -0.015(9) -0.015(9) O3E 0.086(7) 0.111(9) 0.112(8) 0.053(7) -0.019(6) -0.018(6) C4E 0.226(15) 0.253(14) 0.242(14) 0.210(13) -0.062(11) -0.019(13) F5E 0.241(13) 0.224(14) 0.266(15) 0.198(13) -0.038(11) -0.006(11) F6E 0.216(14) 0.303(16) 0.258(15) 0.209(13) 0.027(11) -0.019(12) F7E 0.246(14) 0.263(14) 0.243(13) 0.195(12) -0.119(11) -0.079(11) O1F 0.156(13) 0.169(13) 0.155(12) 0.065(10) -0.016(10) -0.016(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N70 1.965(9) . ? Fe1 N90 1.978(8) . ? Fe1 N97 1.979(9) . ? Fe1 N50 1.979(9) . ? Fe1 N57 1.992(9) . ? Fe1 N77 1.999(9) . ? C1 C2 1.395(15) . ? C1 C6 1.400(14) . ? C1 C42 1.494(15) . ? C2 C3 1.390(16) . ? C2 H2 0.95 . ? C3 C4 1.362(16) . ? C3 H3 0.95 . ? C4 C5 1.390(16) . ? C4 H4 0.95 . ? C5 C6 1.387(15) . ? C5 C7 1.504(15) . ? C6 N43 1.426(13) . ? C7 N8 1.522(15) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? N8 C9 1.497(14) . ? N8 C13 1.514(14) . ? N8 H8 0.93 . ? C9 C10 1.495(17) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 N11 1.471(14) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? N11 C14 1.451(14) . ? N11 C12 1.460(13) . ? C12 C13 1.505(16) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.531(16) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.382(17) . ? C15 C20 1.392(16) . ? C16 C17 1.36(2) . ? C16 H16 0.95 . ? C17 C18 1.37(2) . ? C17 H17 0.95 . ? C18 C19 1.390(18) . ? C18 H18 0.95 . ? C19 C20 1.379(16) . ? C19 C21 1.498(17) . ? C20 N63 1.428(13) . ? C21 N22 1.522(14) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? N22 C23 1.475(15) . ? N22 C27 1.493(14) . ? N22 H22 0.93 . ? C23 C24 1.506(16) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 N25 1.460(15) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? N25 C26 1.453(15) . ? N25 C28 1.490(14) . ? C26 C27 1.508(16) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 C29 1.487(17) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 C30 1.385(17) . ? C29 C34 1.394(17) . ? C30 C31 1.37(2) . ? C30 H30 0.95 . ? C31 C32 1.343(19) . ? C31 H31 0.95 . ? C32 C33 1.402(16) . ? C32 H32 0.95 . ? C33 C34 1.385(16) . ? C33 C35 1.510(16) . ? C34 N83 1.453(14) . ? C35 N36 1.515(14) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? N36 C41 1.493(15) . ? N36 C37 1.500(14) . ? N36 H36 0.93 . ? C37 C38 1.504(16) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 N39 1.445(14) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? N39 C40 1.460(14) . ? N39 C42 1.486(14) . ? C40 C41 1.508(16) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? N43 C44 1.331(13) . ? N43 H43 0.88 . ? C44 O45 1.215(13) . ? C44 C46 1.510(16) . ? C46 C47 1.381(15) . ? C46 C51 1.384(14) . ? C47 C48 1.379(15) . ? C47 H47 0.95 . ? C48 C49 1.364(14) . ? C48 H48 0.95 . ? C49 N50 1.377(13) . ? C49 C52 1.438(15) . ? N50 C51 1.328(13) . ? C51 H51 0.95 . ? C52 N57 1.370(13) . ? C52 C53 1.407(15) . ? C53 C54 1.374(15) . ? C53 H53 0.95 . ? C54 C55 1.391(15) . ? C54 H54 0.95 . ? C55 C56 1.358(15) . ? C55 C58 1.493(18) . ? C56 N57 1.344(13) . ? C56 H56 0.95 . ? C58 O59 1.210(14) . ? C58 O60 1.323(14) . ? O60 C61 1.444(16) . ? C61 C62B 1.34(4) . ? C61 C62A 1.46(3) . ? C61 H61A 0.99 . ? C61 H61B 0.99 . ? C61 H61C 0.99 . ? C61 H61D 0.99 . ? C62A H62A 0.98 . ? C62A H62B 0.98 . ? C62A H62C 0.98 . ? C62B H62D 0.98 . ? C62B H62E 0.98 . ? C62B H62F 0.98 . ? N63 C64 1.370(13) . ? N63 H63 0.88 . ? C64 O65 1.216(12) . ? C64 C66 1.505(15) . ? C66 C71 1.381(14) . ? C66 C67 1.396(14) . ? C67 C68 1.398(15) . ? C67 H67 0.95 . ? C68 C69 1.384(15) . ? C68 H68 0.95 . ? C69 N70 1.353(12) . ? C69 C72 1.464(15) . ? N70 C71 1.335(13) . ? C71 H71 0.95 . ? C72 N77 1.345(13) . ? C72 C73 1.408(14) . ? C73 C74 1.373(15) . ? C73 H73 0.95 . ? C74 C75 1.379(15) . ? C74 H74 0.95 . ? C75 C76 1.390(14) . ? C75 C78 1.472(16) . ? C76 N77 1.319(13) . ? C76 H76 0.95 . ? C78 O79 1.221(13) . ? C78 O80 1.313(13) . ? O80 C81 1.472(15) . ? C81 C82 1.51(2) . ? C81 H81A 0.99 . ? C81 H81B 0.99 . ? C82 H82A 0.98 . ? C82 H82B 0.98 . ? C82 H82C 0.98 . ? N83 C84 1.353(13) . ? N83 H83 0.88 . ? C84 O85 1.210(13) . ? C84 C86 1.499(15) . ? C86 C87 1.397(14) . ? C86 C91 1.401(14) . ? C87 C88 1.375(14) . ? C87 H87 0.95 . ? C88 C89 1.386(14) . ? C88 H88 0.95 . ? C89 N90 1.359(12) . ? C89 C92 1.467(14) . ? N90 C91 1.342(12) . ? C91 H91 0.95 . ? C92 N97 1.364(13) . ? C92 C93 1.385(14) . ? C93 C94 1.372(15) . ? C93 H93 0.95 . ? C94 C95 1.387(15) . ? C94 H94 0.95 . ? C95 C96 1.376(14) . ? C95 C98 1.485(15) . ? C96 N97 1.342(12) . ? C96 H96 0.95 . ? C98 O99 1.201(13) . ? C98 O100 1.348(14) . ? O100 C101 1.456(13) . ? C101 C102 1.46(2) . ? C101 H10C 0.99 . ? C101 H10D 0.99 . ? C102 H10E 0.98 . ? C102 H10F 0.98 . ? C102 H10G 0.98 . ? Cl1A O3A 1.430(5) . ? Cl1A O5A 1.430(6) . ? Cl1A O2A 1.430(6) . ? Cl1A O4A 1.434(6) . ? Cl1B O3B 1.460(6) . ? Cl1B O5B 1.478(7) . ? Cl1B O2B 1.481(7) . ? Cl1B O4B 1.493(7) . ? Cl1C O6C 1.403(8) . ? Cl1C O3C 1.411(6) . ? Cl1C O5C 1.432(8) . ? Cl1C O2C 1.432(6) . ? Cl1C O8C 1.438(8) . ? Cl1C O4C 1.466(8) . ? Cl1C O7C 1.467(8) . ? Cl1D O5D 1.442(7) . ? Cl1D O3D 1.451(6) . ? Cl1D O4D 1.484(9) . ? Cl1D O2D 1.498(8) . ? O1E C2E 1.203(17) . ? C2E O3E 1.254(18) . ? C2E C4E 1.47(3) . ? C4E F7E 1.335(12) . ? C4E F5E 1.339(12) . ? C4E F6E 1.341(12) . ? O1F H1FA 0.949(14) . ? O1F H1FB 0.962(15) . ? C104 C104 1.64(11) 2_656 ? 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 N70 Fe1 N90 92.3(3) . . ? N70 Fe1 N97 94.3(3) . . ? N90 Fe1 N97 80.4(3) . . ? N70 Fe1 N50 94.8(4) . . ? N90 Fe1 N50 96.1(3) . . ? N97 Fe1 N50 170.4(4) . . ? N70 Fe1 N57 171.0(3) . . ? N90 Fe1 N57 96.0(3) . . ? N97 Fe1 N57 90.4(4) . . ? N50 Fe1 N57 81.0(4) . . ? N70 Fe1 N77 80.9(4) . . ? N90 Fe1 N77 167.8(3) . . ? N97 Fe1 N77 90.0(3) . . ? N50 Fe1 N77 94.6(3) . . ? N57 Fe1 N77 91.5(3) . . ? C2 C1 C6 117.9(11) . . ? C2 C1 C42 120.6(10) . . ? C6 C1 C42 121.4(10) . . ? C3 C2 C1 120.9(11) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 119.3(12) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 122.0(12) . . ? C3 C4 H4 119 . . ? C5 C4 H4 119 . . ? C6 C5 C4 118.0(10) . . ? C6 C5 C7 120.8(11) . . ? C4 C5 C7 121.2(11) . . ? C5 C6 C1 121.6(10) . . ? C5 C6 N43 120.3(10) . . ? C1 C6 N43 118.0(10) . . ? C5 C7 N8 113.7(10) . . ? C5 C7 H7A 108.8 . . ? N8 C7 H7A 108.8 . . ? C5 C7 H7B 108.8 . . ? N8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 N8 C13 108.1(9) . . ? C9 N8 C7 109.1(9) . . ? C13 N8 C7 115.7(9) . . ? C9 N8 H8 107.9 . . ? C13 N8 H8 107.9 . . ? C7 N8 H8 107.9 . . ? C10 C9 N8 110.1(11) . . ? C10 C9 H9A 109.6 . . ? N8 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? N8 C9 H9B 109.6 . . ? H9A C9 H9B 108.2 . . ? N11 C10 C9 110.3(10) . . ? N11 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? N11 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C14 N11 C12 113.2(9) . . ? C14 N11 C10 109.0(9) . . ? C12 N11 C10 109.5(9) . . ? N11 C12 C13 109.6(10) . . ? N11 C12 H12A 109.7 . . ? C13 C12 H12A 109.7 . . ? N11 C12 H12B 109.7 . . ? C13 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C12 C13 N8 109.8(9) . . ? C12 C13 H13A 109.7 . . ? N8 C13 H13A 109.7 . . ? C12 C13 H13B 109.7 . . ? N8 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? N11 C14 C15 112.2(9) . . ? N11 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? N11 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C20 117.8(12) . . ? C16 C15 C14 120.5(12) . . ? C20 C15 C14 121.7(11) . . ? C17 C16 C15 120.6(15) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 121.0(14) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C19 120.7(14) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 C18 117.3(13) . . ? C20 C19 C21 121.9(11) . . ? C18 C19 C21 120.8(12) . . ? C19 C20 C15 122.5(11) . . ? C19 C20 N63 119.6(11) . . ? C15 C20 N63 117.8(11) . . ? C19 C21 N22 113.9(10) . . ? C19 C21 H21A 108.8 . . ? N22 C21 H21A 108.8 . . ? C19 C21 H21B 108.8 . . ? N22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C23 N22 C27 110.2(10) . . ? C23 N22 C21 108.9(9) . . ? C27 N22 C21 113.9(9) . . ? C23 N22 H22 107.9 . . ? C27 N22 H22 107.9 . . ? C21 N22 H22 107.9 . . ? N22 C23 C24 111.7(10) . . ? N22 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? N22 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? N25 C24 C23 110.0(10) . . ? N25 C24 H24A 109.7 . . ? C23 C24 H24A 109.7 . . ? N25 C24 H24B 109.7 . . ? C23 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C26 N25 C24 109.8(10) . . ? C26 N25 C28 112.1(10) . . ? C24 N25 C28 109.3(9) . . ? N25 C26 C27 109.5(10) . . ? N25 C26 H26A 109.8 . . ? C27 C26 H26A 109.8 . . ? N25 C26 H26B 109.8 . . ? C27 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? N22 C27 C26 110.7(9) . . ? N22 C27 H27A 109.5 . . ? C26 C27 H27A 109.5 . . ? N22 C27 H27B 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C29 C28 N25 116.3(10) . . ? C29 C28 H28A 108.2 . . ? N25 C28 H28A 108.2 . . ? C29 C28 H28B 108.2 . . ? N25 C28 H28B 108.2 . . ? H28A C28 H28B 107.4 . . ? C30 C29 C34 116.9(12) . . ? C30 C29 C28 121.1(12) . . ? C34 C29 C28 122.0(11) . . ? C31 C30 C29 121.8(14) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C32 C31 C30 120.4(14) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 120.9(13) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 117.9(12) . . ? C34 C33 C35 122.8(10) . . ? C32 C33 C35 119.3(11) . . ? C33 C34 C29 121.9(11) . . ? C33 C34 N83 118.5(11) . . ? C29 C34 N83 119.4(11) . . ? C33 C35 N36 111.8(10) . . ? C33 C35 H35A 109.3 . . ? N36 C35 H35A 109.3 . . ? C33 C35 H35B 109.3 . . ? N36 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? C41 N36 C37 108.6(9) . . ? C41 N36 C35 113.9(9) . . ? C37 N36 C35 110.6(9) . . ? C41 N36 H36 107.8 . . ? C37 N36 H36 107.8 . . ? C35 N36 H36 107.8 . . ? N36 C37 C38 111.3(10) . . ? N36 C37 H37A 109.4 . . ? C38 C37 H37A 109.4 . . ? N36 C37 H37B 109.4 . . ? C38 C37 H37B 109.4 . . ? H37A C37 H37B 108 . . ? N39 C38 C37 109.8(9) . . ? N39 C38 H38A 109.7 . . ? C37 C38 H38A 109.7 . . ? N39 C38 H38B 109.7 . . ? C37 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C38 N39 C40 109.4(9) . . ? C38 N39 C42 110.1(9) . . ? C40 N39 C42 111.6(9) . . ? N39 C40 C41 110.7(9) . . ? N39 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? N39 C40 H40B 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? N36 C41 C40 111.3(10) . . ? N36 C41 H41A 109.4 . . ? C40 C41 H41A 109.4 . . ? N36 C41 H41B 109.4 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 108 . . ? N39 C42 C1 112.1(9) . . ? N39 C42 H42A 109.2 . . ? C1 C42 H42A 109.2 . . ? N39 C42 H42B 109.2 . . ? C1 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C44 N43 C6 121.0(10) . . ? C44 N43 H43 119.5 . . ? C6 N43 H43 119.5 . . ? O45 C44 N43 123.8(11) . . ? O45 C44 C46 119.6(10) . . ? N43 C44 C46 116.6(11) . . ? C47 C46 C51 118.4(11) . . ? C47 C46 C44 125.8(10) . . ? C51 C46 C44 115.7(11) . . ? C48 C47 C46 117.4(10) . . ? C48 C47 H47 121.3 . . ? C46 C47 H47 121.3 . . ? C49 C48 C47 122.0(11) . . ? C49 C48 H48 119 . . ? C47 C48 H48 119 . . ? C48 C49 N50 120.7(10) . . ? C48 C49 C52 125.9(10) . . ? N50 C49 C52 113.3(9) . . ? C51 N50 C49 116.9(9) . . ? C51 N50 Fe1 128.1(8) . . ? C49 N50 Fe1 115.0(7) . . ? N50 C51 C46 124.6(10) . . ? N50 C51 H51 117.7 . . ? C46 C51 H51 117.7 . . ? N57 C52 C53 120.8(11) . . ? N57 C52 C49 115.6(10) . . ? C53 C52 C49 123.6(10) . . ? C54 C53 C52 119.1(10) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C53 C54 C55 119.4(11) . . ? C53 C54 H54 120.3 . . ? C55 C54 H54 120.3 . . ? C56 C55 C54 118.8(11) . . ? C56 C55 C58 123.3(11) . . ? C54 C55 C58 117.8(11) . . ? N57 C56 C55 123.8(10) . . ? N57 C56 H56 118.1 . . ? C55 C56 H56 118.1 . . ? C56 N57 C52 117.9(9) . . ? C56 N57 Fe1 128.2(7) . . ? C52 N57 Fe1 113.0(8) . . ? O59 C58 O60 124.6(13) . . ? O59 C58 C55 123.9(12) . . ? O60 C58 C55 111.5(12) . . ? C58 O60 C61 116.3(11) . . ? C62B C61 O60 117(2) . . ? C62B C61 C62A 80(2) . . ? O60 C61 C62A 108.2(16) . . ? C62B C61 H61A 125.6 . . ? O60 C61 H61A 110.1 . . ? C62A C61 H61A 110.1 . . ? C62B C61 H61B 30.9 . . ? O60 C61 H61B 110.1 . . ? C62A C61 H61B 110.1 . . ? H61A C61 H61B 108.4 . . ? C62B C61 H61C 108 . . ? O60 C61 H61C 108 . . ? C62A C61 H61C 133.6 . . ? H61A C61 H61C 28.5 . . ? H61B C61 H61C 83.3 . . ? C62B C61 H61D 108 . . ? O60 C61 H61D 108 . . ? C62A C61 H61D 33 . . ? H61A C61 H61D 79.9 . . ? H61B C61 H61D 134.8 . . ? H61C C61 H61D 107.2 . . ? C61 C62A H62A 109.5 . . ? C61 C62A H62B 109.5 . . ? H62A C62A H62B 109.5 . . ? C61 C62A H62C 109.5 . . ? H62A C62A H62C 109.5 . . ? H62B C62A H62C 109.5 . . ? C61 C62B H62D 109.5 . . ? C61 C62B H62E 109.5 . . ? H62D C62B H62E 109.5 . . ? C61 C62B H62F 109.5 . . ? H62D C62B H62F 109.5 . . ? H62E C62B H62F 109.5 . . ? C64 N63 C20 124.1(9) . . ? C64 N63 H63 117.9 . . ? C20 N63 H63 117.9 . . ? O65 C64 N63 122.6(10) . . ? O65 C64 C66 121.3(10) . . ? N63 C64 C66 116.1(9) . . ? C71 C66 C67 120.4(10) . . ? C71 C66 C64 115.9(9) . . ? C67 C66 C64 123.6(10) . . ? C66 C67 C68 115.5(10) . . ? C66 C67 H67 122.2 . . ? C68 C67 H67 122.2 . . ? C69 C68 C67 120.8(10) . . ? C69 C68 H68 119.6 . . ? C67 C68 H68 119.6 . . ? N70 C69 C68 122.7(10) . . ? N70 C69 C72 113.3(9) . . ? C68 C69 C72 123.5(10) . . ? C71 N70 C69 116.7(9) . . ? C71 N70 Fe1 128.8(7) . . ? C69 N70 Fe1 114.6(7) . . ? N70 C71 C66 123.7(10) . . ? N70 C71 H71 118.2 . . ? C66 C71 H71 118.2 . . ? N77 C72 C73 121.0(11) . . ? N77 C72 C69 114.8(9) . . ? C73 C72 C69 124.1(10) . . ? C74 C73 C72 119.3(11) . . ? C74 C73 H73 120.3 . . ? C72 C73 H73 120.3 . . ? C73 C74 C75 119.7(10) . . ? C73 C74 H74 120.2 . . ? C75 C74 H74 120.2 . . ? C74 C75 C76 117.0(10) . . ? C74 C75 C78 120.8(10) . . ? C76 C75 C78 121.8(10) . . ? N77 C76 C75 124.8(10) . . ? N77 C76 H76 117.6 . . ? C75 C76 H76 117.6 . . ? C76 N77 C72 118.0(9) . . ? C76 N77 Fe1 127.5(7) . . ? C72 N77 Fe1 111.8(7) . . ? O79 C78 O80 123.9(12) . . ? O79 C78 C75 122.3(11) . . ? O80 C78 C75 113.4(10) . . ? C78 O80 C81 116.8(10) . . ? O80 C81 C82 109.4(12) . . ? O80 C81 H81A 109.8 . . ? C82 C81 H81A 109.8 . . ? O80 C81 H81B 109.8 . . ? C82 C81 H81B 109.8 . . ? H81A C81 H81B 108.2 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 N83 C34 122.2(10) . . ? C84 N83 H83 118.9 . . ? C34 N83 H83 118.9 . . ? O85 C84 N83 123.3(11) . . ? O85 C84 C86 121.1(10) . . ? N83 C84 C86 115.5(11) . . ? C87 C86 C91 118.4(10) . . ? C87 C86 C84 126.9(10) . . ? C91 C86 C84 114.7(10) . . ? C88 C87 C86 119.0(10) . . ? C88 C87 H87 120.5 . . ? C86 C87 H87 120.5 . . ? C87 C88 C89 119.7(10) . . ? C87 C88 H88 120.1 . . ? C89 C88 H88 120.1 . . ? N90 C89 C88 121.8(9) . . ? N90 C89 C92 114.0(9) . . ? C88 C89 C92 124.2(10) . . ? C91 N90 C89 118.6(9) . . ? C91 N90 Fe1 125.2(7) . . ? C89 N90 Fe1 115.9(7) . . ? N90 C91 C86 122.2(10) . . ? N90 C91 H91 118.9 . . ? C86 C91 H91 118.9 . . ? N97 C92 C93 122.5(10) . . ? N97 C92 C89 112.9(9) . . ? C93 C92 C89 124.5(10) . . ? C94 C93 C92 119.1(11) . . ? C94 C93 H93 120.4 . . ? C92 C93 H93 120.4 . . ? C93 C94 C95 119.5(11) . . ? C93 C94 H94 120.3 . . ? C95 C94 H94 120.3 . . ? C96 C95 C94 117.8(10) . . ? C96 C95 C98 120.5(10) . . ? C94 C95 C98 121.6(10) . . ? N97 C96 C95 124.5(10) . . ? N97 C96 H96 117.7 . . ? C95 C96 H96 117.7 . . ? C96 N97 C92 116.4(9) . . ? C96 N97 Fe1 126.8(7) . . ? C92 N97 Fe1 116.1(7) . . ? O99 C98 O100 123.7(11) . . ? O99 C98 C95 125.2(11) . . ? O100 C98 C95 111.2(10) . . ? C98 O100 C101 118.3(9) . . ? O100 C101 C102 114.1(13) . . ? O100 C101 H10C 108.7 . . ? C102 C101 H10C 108.7 . . ? O100 C101 H10D 108.7 . . ? C102 C101 H10D 108.7 . . ? H10C C101 H10D 107.6 . . ? C101 C102 H10E 109.5 . . ? C101 C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? C101 C102 H10G 109.5 . . ? H10E C102 H10G 109.5 . . ? H10F C102 H10G 109.5 . . ? O3A Cl1A O5A 109.6(5) . . ? O3A Cl1A O2A 110.3(5) . . ? O5A Cl1A O2A 108.5(6) . . ? O3A Cl1A O4A 109.1(5) . . ? O5A Cl1A O4A 110.4(6) . . ? O2A Cl1A O4A 108.9(4) . . ? O3B Cl1B O5B 110.7(6) . . ? O3B Cl1B O2B 108.9(5) . . ? O5B Cl1B O2B 110.5(6) . . ? O3B Cl1B O4B 112.6(6) . . ? O5B Cl1B O4B 105.0(6) . . ? O2B Cl1B O4B 109.1(5) . . ? O6C Cl1C O3C 133.3(8) . . ? O6C Cl1C O5C 47.0(10) . . ? O3C Cl1C O5C 118.3(9) . . ? O6C Cl1C O2C 113.7(6) . . ? O3C Cl1C O2C 113.0(6) . . ? O5C Cl1C O2C 106.5(6) . . ? O6C Cl1C O8C 116.9(10) . . ? O3C Cl1C O8C 45.3(10) . . ? O5C Cl1C O8C 146.3(9) . . ? O2C Cl1C O8C 107.1(8) . . ? O6C Cl1C O4C 56.4(10) . . ? O3C Cl1C O4C 106.5(8) . . ? O5C Cl1C O4C 103.1(7) . . ? O2C Cl1C O4C 108.8(5) . . ? O8C Cl1C O4C 66.2(10) . . ? O6C Cl1C O7C 107.4(9) . . ? O3C Cl1C O7C 57.2(9) . . ? O5C Cl1C O7C 66.3(9) . . ? O2C Cl1C O7C 109.0(6) . . ? O8C Cl1C O7C 101.9(9) . . ? O4C Cl1C O7C 142.2(8) . . ? O5D Cl1D O3D 109.9(7) . . ? O5D Cl1D O4D 112.8(9) . . ? O3D Cl1D O4D 111.2(8) . . ? O5D Cl1D O2D 114.2(8) . . ? O3D Cl1D O2D 105.9(6) . . ? O4D Cl1D O2D 102.4(7) . . ? O1E C2E O3E 127.2(15) . . ? O1E C2E C4E 115.8(15) . . ? O3E C2E C4E 116.7(15) . . ? F7E C4E F5E 103.5(12) . . ? F7E C4E F6E 103.5(12) . . ? F5E C4E F6E 102.8(12) . . ? F7E C4E C2E 113.7(15) . . ? F5E C4E C2E 117.0(14) . . ? F6E C4E C2E 114.7(14) . . ? H1FA O1F H1FB 109.1(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 2.9(17) . . . . ? C42 C1 C2 C3 -179.5(11) . . . . ? C1 C2 C3 C4 -2.5(19) . . . . ? C2 C3 C4 C5 2(2) . . . . ? C3 C4 C5 C6 -2.0(18) . . . . ? C3 C4 C5 C7 178.6(12) . . . . ? C4 C5 C6 C1 2.6(17) . . . . ? C7 C5 C6 C1 -178.0(10) . . . . ? C4 C5 C6 N43 -178.5(10) . . . . ? C7 C5 C6 N43 0.9(16) . . . . ? C2 C1 C6 C5 -3.0(16) . . . . ? C42 C1 C6 C5 179.4(11) . . . . ? C2 C1 C6 N43 178.0(10) . . . . ? C42 C1 C6 N43 0.4(15) . . . . ? C6 C5 C7 N8 127.3(12) . . . . ? C4 C5 C7 N8 -53.4(15) . . . . ? C5 C7 N8 C9 -171.0(10) . . . . ? C5 C7 N8 C13 -48.9(14) . . . . ? C13 N8 C9 C10 58.0(13) . . . . ? C7 N8 C9 C10 -175.4(10) . . . . ? N8 C9 C10 N11 -59.9(14) . . . . ? C9 C10 N11 C14 -174.8(10) . . . . ? C9 C10 N11 C12 60.8(14) . . . . ? C14 N11 C12 C13 177.1(10) . . . . ? C10 N11 C12 C13 -61.0(13) . . . . ? N11 C12 C13 N8 60.6(13) . . . . ? C9 N8 C13 C12 -58.4(13) . . . . ? C7 N8 C13 C12 178.9(9) . . . . ? C12 N11 C14 C15 -54.8(13) . . . . ? C10 N11 C14 C15 -176.9(10) . . . . ? N11 C14 C15 C16 118.8(12) . . . . ? N11 C14 C15 C20 -61.3(14) . . . . ? C20 C15 C16 C17 1.0(19) . . . . ? C14 C15 C16 C17 -179.1(12) . . . . ? C15 C16 C17 C18 1(2) . . . . ? C16 C17 C18 C19 -2(2) . . . . ? C17 C18 C19 C20 1(2) . . . . ? C17 C18 C19 C21 -177.6(13) . . . . ? C18 C19 C20 C15 0.9(17) . . . . ? C21 C19 C20 C15 179.7(10) . . . . ? C18 C19 C20 N63 -175.4(11) . . . . ? C21 C19 C20 N63 3.4(16) . . . . ? C16 C15 C20 C19 -2.0(17) . . . . ? C14 C15 C20 C19 178.1(10) . . . . ? C16 C15 C20 N63 174.4(10) . . . . ? C14 C15 C20 N63 -5.5(16) . . . . ? C20 C19 C21 N22 125.0(12) . . . . ? C18 C19 C21 N22 -56.3(16) . . . . ? C19 C21 N22 C23 178.4(11) . . . . ? C19 C21 N22 C27 -58.2(15) . . . . ? C27 N22 C23 C24 53.5(14) . . . . ? C21 N22 C23 C24 179.1(11) . . . . ? N22 C23 C24 N25 -56.8(16) . . . . ? C23 C24 N25 C26 60.7(14) . . . . ? C23 C24 N25 C28 -176.0(11) . . . . ? C24 N25 C26 C27 -61.8(12) . . . . ? C28 N25 C26 C27 176.5(10) . . . . ? C23 N22 C27 C26 -54.4(14) . . . . ? C21 N22 C27 C26 -177.1(11) . . . . ? N25 C26 C27 N22 58.8(14) . . . . ? C26 N25 C28 C29 -58.0(15) . . . . ? C24 N25 C28 C29 180.0(12) . . . . ? N25 C28 C29 C30 125.3(14) . . . . ? N25 C28 C29 C34 -57.3(18) . . . . ? C34 C29 C30 C31 1(2) . . . . ? C28 C29 C30 C31 178.6(16) . . . . ? C29 C30 C31 C32 2(3) . . . . ? C30 C31 C32 C33 -3(3) . . . . ? C31 C32 C33 C34 1(2) . . . . ? C31 C32 C33 C35 178.3(15) . . . . ? C32 C33 C34 C29 3(2) . . . . ? C35 C33 C34 C29 -174.7(12) . . . . ? C32 C33 C34 N83 -174.1(12) . . . . ? C35 C33 C34 N83 8.5(18) . . . . ? C30 C29 C34 C33 -3(2) . . . . ? C28 C29 C34 C33 179.0(12) . . . . ? C30 C29 C34 N83 173.2(12) . . . . ? C28 C29 C34 N83 -4.3(18) . . . . ? C34 C33 C35 N36 125.6(12) . . . . ? C32 C33 C35 N36 -51.7(16) . . . . ? C33 C35 N36 C41 -49.4(12) . . . . ? C33 C35 N36 C37 -172.0(9) . . . . ? C41 N36 C37 C38 55.3(12) . . . . ? C35 N36 C37 C38 -179.0(9) . . . . ? N36 C37 C38 N39 -60.0(12) . . . . ? C37 C38 N39 C40 61.5(12) . . . . ? C37 C38 N39 C42 -175.5(9) . . . . ? C38 N39 C40 C41 -60.6(12) . . . . ? C42 N39 C40 C41 177.3(9) . . . . ? C37 N36 C41 C40 -53.9(12) . . . . ? C35 N36 C41 C40 -177.6(9) . . . . ? N39 C40 C41 N36 57.5(13) . . . . ? C38 N39 C42 C1 173.6(9) . . . . ? C40 N39 C42 C1 -64.7(12) . . . . ? C2 C1 C42 N39 117.2(11) . . . . ? C6 C1 C42 N39 -65.3(14) . . . . ? C5 C6 N43 C44 -80.5(13) . . . . ? C1 C6 N43 C44 98.5(12) . . . . ? C6 N43 C44 O45 10.7(16) . . . . ? C6 N43 C44 C46 -172.2(9) . . . . ? O45 C44 C46 C47 -150.4(11) . . . . ? N43 C44 C46 C47 32.4(15) . . . . ? O45 C44 C46 C51 25.7(15) . . . . ? N43 C44 C46 C51 -151.6(9) . . . . ? C51 C46 C47 C48 -1.4(15) . . . . ? C44 C46 C47 C48 174.6(10) . . . . ? C46 C47 C48 C49 1.6(16) . . . . ? C47 C48 C49 N50 -0.5(16) . . . . ? C47 C48 C49 C52 -175.7(10) . . . . ? C48 C49 N50 C51 -0.9(14) . . . . ? C52 C49 N50 C51 174.8(8) . . . . ? C48 C49 N50 Fe1 180.0(8) . . . . ? C52 C49 N50 Fe1 -4.2(10) . . . . ? N70 Fe1 N50 C51 18.6(8) . . . . ? N90 Fe1 N50 C51 -74.3(8) . . . . ? N97 Fe1 N50 C51 -142(2) . . . . ? N57 Fe1 N50 C51 -169.4(9) . . . . ? N77 Fe1 N50 C51 99.8(8) . . . . ? N70 Fe1 N50 C49 -162.5(7) . . . . ? N90 Fe1 N50 C49 104.7(7) . . . . ? N97 Fe1 N50 C49 37(2) . . . . ? N57 Fe1 N50 C49 9.5(7) . . . . ? N77 Fe1 N50 C49 -81.3(7) . . . . ? C49 N50 C51 C46 1.2(14) . . . . ? Fe1 N50 C51 C46 -179.9(7) . . . . ? C47 C46 C51 N50 -0.1(15) . . . . ? C44 C46 C51 N50 -176.4(9) . . . . ? C48 C49 C52 N57 168.4(10) . . . . ? N50 C49 C52 N57 -7.1(12) . . . . ? C48 C49 C52 C53 -11.5(16) . . . . ? N50 C49 C52 C53 172.9(9) . . . . ? N57 C52 C53 C54 -1.9(15) . . . . ? C49 C52 C53 C54 178.1(10) . . . . ? C52 C53 C54 C55 -2.2(15) . . . . ? C53 C54 C55 C56 3.6(16) . . . . ? C53 C54 C55 C58 179.7(10) . . . . ? C54 C55 C56 N57 -0.9(16) . . . . ? C58 C55 C56 N57 -176.8(10) . . . . ? C55 C56 N57 C52 -3.0(14) . . . . ? C55 C56 N57 Fe1 164.8(8) . . . . ? C53 C52 N57 C56 4.4(13) . . . . ? C49 C52 N57 C56 -175.5(8) . . . . ? C53 C52 N57 Fe1 -165.2(8) . . . . ? C49 C52 N57 Fe1 14.9(10) . . . . ? N70 Fe1 N57 C56 -119(2) . . . . ? N90 Fe1 N57 C56 83.3(8) . . . . ? N97 Fe1 N57 C56 2.9(8) . . . . ? N50 Fe1 N57 C56 178.5(8) . . . . ? N77 Fe1 N57 C56 -87.1(8) . . . . ? N70 Fe1 N57 C52 50(2) . . . . ? N90 Fe1 N57 C52 -108.4(7) . . . . ? N97 Fe1 N57 C52 171.2(7) . . . . ? N50 Fe1 N57 C52 -13.2(7) . . . . ? N77 Fe1 N57 C52 81.2(7) . . . . ? C56 C55 C58 O59 -165.5(12) . . . . ? C54 C55 C58 O59 18.6(18) . . . . ? C56 C55 C58 O60 13.5(16) . . . . ? C54 C55 C58 O60 -162.4(10) . . . . ? O59 C58 O60 C61 -1.5(18) . . . . ? C55 C58 O60 C61 179.6(11) . . . . ? C58 O60 C61 C62B -87(3) . . . . ? C58 O60 C61 C62A -174.4(16) . . . . ? C19 C20 N63 C64 -85.5(13) . . . . ? C15 C20 N63 C64 98.0(12) . . . . ? C20 N63 C64 O65 6.7(17) . . . . ? C20 N63 C64 C66 -171.5(10) . . . . ? O65 C64 C66 C71 34.1(15) . . . . ? N63 C64 C66 C71 -147.7(10) . . . . ? O65 C64 C66 C67 -146.5(11) . . . . ? N63 C64 C66 C67 31.7(15) . . . . ? C71 C66 C67 C68 -5.0(16) . . . . ? C64 C66 C67 C68 175.6(10) . . . . ? C66 C67 C68 C69 2.7(16) . . . . ? C67 C68 C69 N70 0.5(18) . . . . ? C67 C68 C69 C72 -171.1(11) . . . . ? C68 C69 N70 C71 -1.5(16) . . . . ? C72 C69 N70 C71 170.9(9) . . . . ? C68 C69 N70 Fe1 179.3(9) . . . . ? C72 C69 N70 Fe1 -8.4(12) . . . . ? N90 Fe1 N70 C71 26.3(9) . . . . ? N97 Fe1 N70 C71 106.8(9) . . . . ? N50 Fe1 N70 C71 -70.0(9) . . . . ? N57 Fe1 N70 C71 -132(2) . . . . ? N77 Fe1 N70 C71 -163.9(9) . . . . ? N90 Fe1 N70 C69 -154.6(7) . . . . ? N97 Fe1 N70 C69 -74.0(8) . . . . ? N50 Fe1 N70 C69 109.1(7) . . . . ? N57 Fe1 N70 C69 47(3) . . . . ? N77 Fe1 N70 C69 15.3(7) . . . . ? C69 N70 C71 C66 -0.9(15) . . . . ? Fe1 N70 C71 C66 178.2(8) . . . . ? C67 C66 C71 N70 4.3(16) . . . . ? C64 C66 C71 N70 -176.2(9) . . . . ? N70 C69 C72 N77 -8.5(14) . . . . ? C68 C69 C72 N77 163.7(10) . . . . ? N70 C69 C72 C73 171.3(10) . . . . ? C68 C69 C72 C73 -16.4(18) . . . . ? N77 C72 C73 C74 0.4(16) . . . . ? C69 C72 C73 C74 -179.4(11) . . . . ? C72 C73 C74 C75 -3.9(17) . . . . ? C73 C74 C75 C76 3.2(16) . . . . ? C73 C74 C75 C78 175.7(11) . . . . ? C74 C75 C76 N77 1.1(16) . . . . ? C78 C75 C76 N77 -171.4(10) . . . . ? C75 C76 N77 C72 -4.5(15) . . . . ? C75 C76 N77 Fe1 155.2(8) . . . . ? C73 C72 N77 C76 3.6(15) . . . . ? C69 C72 N77 C76 -176.5(9) . . . . ? C73 C72 N77 Fe1 -159.1(8) . . . . ? C69 C72 N77 Fe1 20.7(11) . . . . ? N70 Fe1 N77 C76 179.6(9) . . . . ? N90 Fe1 N77 C76 -123.9(17) . . . . ? N97 Fe1 N77 C76 -86.0(9) . . . . ? N50 Fe1 N77 C76 85.5(9) . . . . ? N57 Fe1 N77 C76 4.4(9) . . . . ? N70 Fe1 N77 C72 -19.6(7) . . . . ? N90 Fe1 N77 C72 37(2) . . . . ? N97 Fe1 N77 C72 74.7(7) . . . . ? N50 Fe1 N77 C72 -113.8(7) . . . . ? N57 Fe1 N77 C72 165.1(7) . . . . ? C74 C75 C78 O79 -19.1(18) . . . . ? C76 C75 C78 O79 153.0(12) . . . . ? C74 C75 C78 O80 167.7(11) . . . . ? C76 C75 C78 O80 -20.2(16) . . . . ? O79 C78 O80 C81 -4.7(18) . . . . ? C75 C78 O80 C81 168.3(11) . . . . ? C78 O80 C81 C82 -86.3(14) . . . . ? C33 C34 N83 C84 -81.2(15) . . . . ? C29 C34 N83 C84 102.0(13) . . . . ? C34 N83 C84 O85 3.7(18) . . . . ? C34 N83 C84 C86 -179.3(10) . . . . ? O85 C84 C86 C87 -146.3(12) . . . . ? N83 C84 C86 C87 36.7(16) . . . . ? O85 C84 C86 C91 32.4(15) . . . . ? N83 C84 C86 C91 -144.6(10) . . . . ? C91 C86 C87 C88 -5.0(15) . . . . ? C84 C86 C87 C88 173.7(10) . . . . ? C86 C87 C88 C89 1.4(16) . . . . ? C87 C88 C89 N90 3.2(16) . . . . ? C87 C88 C89 C92 -174.7(10) . . . . ? C88 C89 N90 C91 -4.1(14) . . . . ? C92 C89 N90 C91 174.1(9) . . . . ? C88 C89 N90 Fe1 -178.4(8) . . . . ? C92 C89 N90 Fe1 -0.3(11) . . . . ? N70 Fe1 N90 C91 -76.3(8) . . . . ? N97 Fe1 N90 C91 -170.3(8) . . . . ? N50 Fe1 N90 C91 18.8(8) . . . . ? N57 Fe1 N90 C91 100.3(8) . . . . ? N77 Fe1 N90 C91 -131.8(16) . . . . ? N70 Fe1 N90 C89 97.6(7) . . . . ? N97 Fe1 N90 C89 3.6(7) . . . . ? N50 Fe1 N90 C89 -167.3(7) . . . . ? N57 Fe1 N90 C89 -85.7(7) . . . . ? N77 Fe1 N90 C89 42(2) . . . . ? C89 N90 C91 C86 0.3(14) . . . . ? Fe1 N90 C91 C86 174.1(7) . . . . ? C87 C86 C91 N90 4.2(15) . . . . ? C84 C86 C91 N90 -174.6(9) . . . . ? N90 C89 C92 N97 -5.1(13) . . . . ? C88 C89 C92 N97 173.0(10) . . . . ? N90 C89 C92 C93 176.6(10) . . . . ? C88 C89 C92 C93 -5.3(17) . . . . ? N97 C92 C93 C94 3.7(17) . . . . ? C89 C92 C93 C94 -178.2(11) . . . . ? C92 C93 C94 C95 -1.6(17) . . . . ? C93 C94 C95 C96 -1.4(17) . . . . ? C93 C94 C95 C98 177.4(11) . . . . ? C94 C95 C96 N97 2.6(17) . . . . ? C98 C95 C96 N97 -176.2(10) . . . . ? C95 C96 N97 C92 -0.7(15) . . . . ? C95 C96 N97 Fe1 169.1(8) . . . . ? C93 C92 N97 C96 -2.6(15) . . . . ? C89 C92 N97 C96 179.1(9) . . . . ? C93 C92 N97 Fe1 -173.5(8) . . . . ? C89 C92 N97 Fe1 8.3(11) . . . . ? N70 Fe1 N97 C96 91.9(9) . . . . ? N90 Fe1 N97 C96 -176.5(9) . . . . ? N50 Fe1 N97 C96 -107(2) . . . . ? N57 Fe1 N97 C96 -80.4(9) . . . . ? N77 Fe1 N97 C96 11.1(9) . . . . ? N70 Fe1 N97 C92 -98.3(8) . . . . ? N90 Fe1 N97 C92 -6.7(7) . . . . ? N50 Fe1 N97 C92 62(2) . . . . ? N57 Fe1 N97 C92 89.4(8) . . . . ? N77 Fe1 N97 C92 -179.1(8) . . . . ? C96 C95 C98 O99 -164.1(12) . . . . ? C94 C95 C98 O99 17(2) . . . . ? C96 C95 C98 O100 15.7(16) . . . . ? C94 C95 C98 O100 -163.1(11) . . . . ? O99 C98 O100 C101 1(2) . . . . ? C95 C98 O100 C101 -178.9(11) . . . . ? C98 O100 C101 C102 -84.6(16) . . . . ? O1E C2E C4E F7E 152.1(14) . . . . ? O3E C2E C4E F7E -33.9(19) . . . . ? O1E C2E C4E F5E 31(2) . . . . ? O3E C2E C4E F5E -154.6(13) . . . . ? O1E C2E C4E F6E -89.1(18) . . . . ? O3E C2E C4E F6E 84.9(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8 O5D 0.93 1.93 2.742(13) 144.5 . N22 H22 O5B 0.93 2.11 3.031(16) 171.6 . N36 H36 O1E 0.93 1.83 2.731(13) 161.5 . N43 H43 O3D 0.88 2.17 3.000(13) 155.9 2_556 N63 H63 O5C 0.88 1.99 2.822(14) 157.9 2_666 N63 H63 O6C 0.88 2.12 2.964(19) 159.8 2_666 N83 H83 O4A 0.88 2.09 2.955(13) 167.3 2_667 O1F H1FB O45 0.962(15) 2.027(9) 2.988(17) 177.3(9) . data_V1 _database_code_depnum_ccdc_archive 'CCDC 809075' #TrackingRef '- CS_KR_110124_XRD.cif' _audit_creation_date 2010-06-03T09:46:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C72 H71 Fe N15 O9, 2(O4 S), O26' _chemical_formula_sum 'C72 H71 Fe N15 O43 S2' _chemical_formula_weight 1954.41 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.8873(2) _cell_length_b 24.0212(3) _cell_length_c 31.2772(4) _cell_angle_alpha 90 _cell_angle_beta 101.1260(10) _cell_angle_gamma 90 _cell_volume 10237.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 12562 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 28.283 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4040 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.130878E-1 _diffrn_orient_matrix_ub_12 -0.17558E-2 _diffrn_orient_matrix_ub_13 0.303094E-1 _diffrn_orient_matrix_ub_21 -0.722109E-1 _diffrn_orient_matrix_ub_22 0.4171E-3 _diffrn_orient_matrix_ub_23 -0.118803E-1 _diffrn_orient_matrix_ub_31 -0.1716E-3 _diffrn_orient_matrix_ub_32 -0.415908E-1 _diffrn_orient_matrix_ub_33 -0.13987E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_unetI/netI 0.0433 _diffrn_reflns_number 64949 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.17 _diffrn_reflns_theta_full 28.17 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 23401 _reflns_number_gt 20814 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1678P)^2^+10.0128P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 23401 _refine_ls_number_parameters 1250 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.091 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.232 _refine_ls_wR_factor_gt 0.2163 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.09 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.028(15) _refine_diff_density_max 1.186 _refine_diff_density_min -1.51 _refine_diff_density_rms 0.209 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.73332(3) 0.06973(2) 0.364346(18) 0.02366(13) Uani 1 1 d . . . C1 C 0.4739(3) -0.11395(15) 0.15415(12) 0.0231(7) Uani 1 1 d . . . C2 C 0.4535(3) -0.13219(16) 0.11069(13) 0.0270(8) Uani 1 1 d . . . H2 H 0.4981 -0.1564 0.1004 0.032 Uiso 1 1 calc R . . C3 C 0.3691(3) -0.11517(17) 0.08286(14) 0.0303(8) Uani 1 1 d . . . H3 H 0.3553 -0.1286 0.0537 0.036 Uiso 1 1 calc R . . C4 C 0.3042(3) -0.07881(17) 0.09676(15) 0.0297(8) Uani 1 1 d . . . H4 H 0.2468 -0.067 0.0772 0.036 Uiso 1 1 calc R . . C5 C 0.3239(3) -0.05936(16) 0.14015(13) 0.0247(7) Uani 1 1 d . . . C6 C 0.4072(3) -0.07834(15) 0.16847(13) 0.0222(7) Uani 1 1 d . . . C7 C 0.2560(3) -0.01748(16) 0.15470(14) 0.0254(7) Uani 1 1 d . . . H7A H 0.2002 -0.0101 0.1305 0.03 Uiso 1 1 calc R . . H7B H 0.2295 -0.0331 0.1794 0.03 Uiso 1 1 calc R . . N8 N 0.3071(2) 0.03519(13) 0.16831(11) 0.0243(6) Uani 1 1 d . . . C9 C 0.2411(3) 0.07387(16) 0.18463(14) 0.0249(7) Uani 1 1 d . . . H9A H 0.2147 0.056 0.2085 0.03 Uiso 1 1 calc R . . H9B H 0.1853 0.0832 0.1609 0.03 Uiso 1 1 calc R . . C10 C 0.2957(3) 0.12656(16) 0.20135(13) 0.0241(7) Uani 1 1 d . . . H10A H 0.2506 0.1524 0.2124 0.029 Uiso 1 1 calc R . . H10B H 0.3501 0.1174 0.2258 0.029 Uiso 1 1 calc R . . N11 N 0.3360(2) 0.15408(13) 0.16545(10) 0.0216(6) Uani 1 1 d . . . H11 H 0.2833 0.162 0.143 0.026 Uiso 1 1 calc R . . C12 C 0.4018(3) 0.11344(15) 0.14791(13) 0.0239(7) Uani 1 1 d . . . H12A H 0.4269 0.1306 0.1235 0.029 Uiso 1 1 calc R . . H12B H 0.4585 0.1037 0.1711 0.029 Uiso 1 1 calc R . . C13 C 0.3441(3) 0.06175(16) 0.13235(13) 0.0251(7) Uani 1 1 d . . . H13A H 0.2882 0.0716 0.1088 0.03 Uiso 1 1 calc R . . H13B H 0.3866 0.0353 0.1203 0.03 Uiso 1 1 calc R . . C14 C 0.3844(3) 0.20862(15) 0.18104(12) 0.0227(7) Uani 1 1 d . . . H14A H 0.3335 0.2345 0.1874 0.027 Uiso 1 1 calc R . . H14B H 0.4314 0.202 0.2087 0.027 Uiso 1 1 calc R . . C15 C 0.4380(3) 0.23614(15) 0.14930(13) 0.0220(7) Uani 1 1 d . . . C16 C 0.3925(3) 0.24609(17) 0.10643(13) 0.0264(7) Uani 1 1 d . . . H16 H 0.3268 0.2341 0.0966 0.032 Uiso 1 1 calc R . . C17 C 0.4415(3) 0.27338(18) 0.07762(14) 0.0299(8) Uani 1 1 d . . . H17 H 0.4094 0.2802 0.0484 0.036 Uiso 1 1 calc R . . C18 C 0.5383(3) 0.29065(18) 0.09224(14) 0.0294(8) Uani 1 1 d . . . H18 H 0.5724 0.3089 0.0727 0.035 Uiso 1 1 calc R . . C19 C 0.5854(3) 0.28137(16) 0.13503(13) 0.0249(7) Uani 1 1 d . . . C20 C 0.5346(3) 0.25567(16) 0.16363(13) 0.0229(7) Uani 1 1 d . . . C21 C 0.6929(3) 0.29752(16) 0.15028(14) 0.0277(8) Uani 1 1 d . . . H21A H 0.7169 0.3168 0.1264 0.033 Uiso 1 1 calc R . . H21B H 0.6989 0.3235 0.1752 0.033 Uiso 1 1 calc R . . N22 N 0.7529(2) 0.24802(14) 0.16340(12) 0.0261(6) Uani 1 1 d . . . C23 C 0.8549(3) 0.26475(15) 0.18141(14) 0.0252(7) Uani 1 1 d . . . H23A H 0.8556 0.2917 0.2054 0.03 Uiso 1 1 calc R . . H23B H 0.8835 0.2832 0.1585 0.03 Uiso 1 1 calc R . . C24 C 0.9156(3) 0.21450(16) 0.19823(13) 0.0251(7) Uani 1 1 d . . . H24A H 0.9839 0.2262 0.21 0.03 Uiso 1 1 calc R . . H24B H 0.8887 0.1971 0.2221 0.03 Uiso 1 1 calc R . . N25 N 0.9148(2) 0.17290(13) 0.16236(11) 0.0221(6) Uani 1 1 d . . . H25 H 0.9407 0.19 0.1404 0.026 Uiso 1 1 calc R . . C26 C 0.8097(3) 0.15698(17) 0.14382(14) 0.0267(7) Uani 1 1 d . . . H26A H 0.7801 0.1386 0.1665 0.032 Uiso 1 1 calc R . . H26B H 0.8076 0.1306 0.1194 0.032 Uiso 1 1 calc R . . C27 C 0.7525(3) 0.20929(17) 0.12785(14) 0.0280(8) Uani 1 1 d . . . H27A H 0.7821 0.2272 0.105 0.034 Uiso 1 1 calc R . . H27B H 0.6839 0.1992 0.1148 0.034 Uiso 1 1 calc R . . C28 C 0.9804(3) 0.12422(15) 0.17950(12) 0.0226(7) Uani 1 1 d . . . H28A H 0.9619 0.1105 0.2067 0.027 Uiso 1 1 calc R . . H28B H 1.0491 0.1374 0.1869 0.027 Uiso 1 1 calc R . . C29 C 0.9747(3) 0.07620(16) 0.14763(13) 0.0234(7) Uani 1 1 d . . . C30 C 0.9793(3) 0.08492(18) 0.10386(14) 0.0270(8) Uani 1 1 d . . . H30 H 0.9851 0.1217 0.0936 0.032 Uiso 1 1 calc R . . C31 C 0.9754(3) 0.04093(19) 0.07555(14) 0.0300(8) Uani 1 1 d . . . H31 H 0.9792 0.0474 0.046 0.036 Uiso 1 1 calc R . . C32 C 0.9659(3) -0.01385(19) 0.09045(14) 0.0307(8) Uani 1 1 d . . . H32 H 0.9633 -0.0443 0.0709 0.037 Uiso 1 1 calc R . . C33 C 0.9603(3) -0.02329(17) 0.13414(13) 0.0256(7) Uani 1 1 d . . . C34 C 0.9673(3) 0.02199(16) 0.16234(13) 0.0243(7) Uani 1 1 d . . . C35 C 0.9442(3) -0.08112(17) 0.14985(15) 0.0274(8) Uani 1 1 d . . . H35A H 0.9445 -0.108 0.1259 0.033 Uiso 1 1 calc R . . H35B H 0.9985 -0.091 0.1741 0.033 Uiso 1 1 calc R . . N36 N 0.8500(2) -0.08480(14) 0.16475(11) 0.0244(6) Uani 1 1 d . . . C37 C 0.8372(3) -0.14033(16) 0.18229(13) 0.0255(7) Uani 1 1 d . . . H37A H 0.895 -0.1496 0.2051 0.031 Uiso 1 1 calc R . . H37B H 0.8325 -0.1683 0.1587 0.031 Uiso 1 1 calc R . . C38 C 0.7452(3) -0.14254(16) 0.20160(13) 0.0255(7) Uani 1 1 d . . . H38A H 0.7379 -0.1801 0.2135 0.031 Uiso 1 1 calc R . . H38B H 0.7503 -0.1153 0.2257 0.031 Uiso 1 1 calc R . . N39 N 0.6571(2) -0.12920(13) 0.16678(10) 0.0226(6) Uani 1 1 d . . . H39 H 0.6537 -0.1557 0.1449 0.027 Uiso 1 1 calc R . . C40 C 0.6717(3) -0.07301(16) 0.14721(15) 0.0283(8) Uani 1 1 d . . . H40A H 0.6742 -0.0437 0.1696 0.034 Uiso 1 1 calc R . . H40B H 0.6158 -0.0649 0.1232 0.034 Uiso 1 1 calc R . . C41 C 0.7666(3) -0.07287(16) 0.12995(14) 0.0274(8) Uani 1 1 d . . . H41A H 0.7629 -0.1012 0.1067 0.033 Uiso 1 1 calc R . . H41B H 0.7757 -0.036 0.1171 0.033 Uiso 1 1 calc R . . C42 C 0.5648(3) -0.13365(15) 0.18512(13) 0.0231(7) Uani 1 1 d . . . H42A H 0.5729 -0.1114 0.2122 0.028 Uiso 1 1 calc R . . H42B H 0.5554 -0.173 0.1929 0.028 Uiso 1 1 calc R . . N43 N 0.4240(2) -0.06010(13) 0.21263(11) 0.0232(6) Uani 1 1 d . . . H43 H 0.3905 -0.0749 0.231 0.028 Uiso 1 1 calc R . . C44 C 0.4910(3) -0.02038(16) 0.22633(12) 0.0245(7) Uani 1 1 d . . . O45 O 0.5486(2) -0.00278(13) 0.20390(9) 0.0295(6) Uani 1 1 d . . . C46 C 0.4970(3) 0.00255(17) 0.27119(12) 0.0251(7) Uani 1 1 d . . . C47 C 0.5891(3) 0.01826(16) 0.29313(12) 0.0250(7) Uani 1 1 d . . . H47 H 0.6435 0.0108 0.2797 0.03 Uiso 1 1 calc R . . N48 N 0.6063(2) 0.04300(15) 0.33169(10) 0.0256(6) Uani 1 1 d . . . C49 C 0.5264(3) 0.0541(2) 0.34965(13) 0.0301(8) Uani 1 1 d . . . C50 C 0.4320(3) 0.0384(2) 0.33051(14) 0.0336(9) Uani 1 1 d . . . H50 H 0.3786 0.0461 0.3445 0.04 Uiso 1 1 calc R . . C51 C 0.4165(3) 0.0116(2) 0.29085(14) 0.0305(8) Uani 1 1 d . . . H51 H 0.3528 -0.0005 0.2773 0.037 Uiso 1 1 calc R . . C52 C 0.5505(3) 0.0867(2) 0.39002(13) 0.0334(9) Uani 1 1 d . . . N53 N 0.6470(3) 0.10359(17) 0.40015(11) 0.0311(7) Uani 1 1 d . . . C54 C 0.6748(3) 0.1344(2) 0.43636(13) 0.0329(9) Uani 1 1 d . . . H54 H 0.7409 0.1468 0.4437 0.039 Uiso 1 1 calc R . . C55 C 0.6102(3) 0.1488(2) 0.46350(14) 0.0379(10) Uani 1 1 d . . . C56 C 0.5130(4) 0.1311(3) 0.45307(16) 0.0432(12) Uani 1 1 d . . . H56 H 0.4681 0.1398 0.4715 0.052 Uiso 1 1 calc R . . C57 C 0.4837(3) 0.1011(3) 0.41587(16) 0.0428(12) Uani 1 1 d . . . H57 H 0.4171 0.09 0.4076 0.051 Uiso 1 1 calc R . . C58 C 0.6513(4) 0.1815(2) 0.50412(14) 0.0375(10) Uani 1 1 d . . . O59 O 0.5917(3) 0.17949(17) 0.53195(11) 0.0454(9) Uani 1 1 d . . . H59 H 0.6166 0.197 0.5547 0.068 Uiso 1 1 calc R . . O60 O 0.7280(3) 0.2055(2) 0.50900(12) 0.0533(11) Uani 1 1 d . . . N61 N 0.5825(2) 0.24931(14) 0.20834(10) 0.0234(6) Uani 1 1 d . . . H61 H 0.5879 0.2779 0.2262 0.028 Uiso 1 1 calc R . . C62 C 0.6191(3) 0.19918(17) 0.22272(12) 0.0244(7) Uani 1 1 d . . . O63 O 0.6032(2) 0.15628(12) 0.20165(10) 0.0304(6) Uani 1 1 d . . . C64 C 0.6800(3) 0.19763(18) 0.26753(13) 0.0269(7) Uani 1 1 d . . . C65 C 0.6751(3) 0.14826(17) 0.29028(12) 0.0244(7) Uani 1 1 d . . . H65 H 0.6291 0.1208 0.2777 0.029 Uiso 1 1 calc R . . N66 N 0.7323(2) 0.13767(14) 0.32909(10) 0.0231(6) Uani 1 1 d . . . C67 C 0.7981(3) 0.17805(18) 0.34632(13) 0.0283(8) Uani 1 1 d . . . C68 C 0.8026(3) 0.2291(2) 0.32684(15) 0.0348(9) Uani 1 1 d . . . H68 H 0.8462 0.2571 0.3407 0.042 Uiso 1 1 calc R . . C69 C 0.7421(3) 0.23933(19) 0.28634(15) 0.0320(8) Uani 1 1 d . . . H69 H 0.7438 0.2742 0.2722 0.038 Uiso 1 1 calc R . . C70 C 0.8671(3) 0.15939(18) 0.38607(13) 0.0305(8) Uani 1 1 d . . . N71 N 0.8519(2) 0.10614(15) 0.39732(11) 0.0272(7) Uani 1 1 d . . . C72 C 0.9170(3) 0.0838(2) 0.43070(13) 0.0302(8) Uani 1 1 d . . . H72 H 0.9085 0.0462 0.4386 0.036 Uiso 1 1 calc R . . C73 C 0.9963(4) 0.1140(2) 0.45402(15) 0.0366(10) Uani 1 1 d . . . C74 C 1.0065(4) 0.1687(2) 0.44311(18) 0.0494(14) Uani 1 1 d . . . H74 H 1.0579 0.1907 0.4591 0.059 Uiso 1 1 calc R . . C75 C 0.9412(4) 0.1915(2) 0.40853(17) 0.0459(12) Uani 1 1 d . . . H75 H 0.9478 0.2292 0.4004 0.055 Uiso 1 1 calc R . . C76 C 1.0683(4) 0.0858(2) 0.48792(17) 0.0433(11) Uani 1 1 d . . . O77 O 1.1358(4) 0.1097(2) 0.51011(18) 0.0770(18) Uani 1 1 d . . . O78 O 1.0494(3) 0.03239(15) 0.49220(12) 0.0445(9) Uani 1 1 d . . . H78 H 1.0992 0.0166 0.5066 0.067 Uiso 1 1 calc R . . N79 N 0.9636(2) 0.01148(14) 0.20700(11) 0.0250(6) Uani 1 1 d . . . H79 H 1.0157 -0.0016 0.2248 0.03 Uiso 1 1 calc R . . C80 C 0.8810(3) 0.02148(16) 0.22183(13) 0.0254(7) Uani 1 1 d . . . O81 O 0.8090(2) 0.04466(13) 0.20011(10) 0.0297(6) Uani 1 1 d . . . C82 C 0.8787(3) 0.00297(16) 0.26732(13) 0.0248(7) Uani 1 1 d . . . C83 C 0.8265(3) 0.03818(17) 0.29041(12) 0.0242(7) Uani 1 1 d . . . H83 H 0.8024 0.0725 0.2775 0.029 Uiso 1 1 calc R . . N84 N 0.8094(2) 0.02535(14) 0.32988(10) 0.0235(6) Uani 1 1 d . . . C85 C 0.8451(3) -0.02410(17) 0.34807(13) 0.0274(8) Uani 1 1 d . . . C86 C 0.9018(3) -0.05890(18) 0.32779(15) 0.0329(9) Uani 1 1 d . . . H86 H 0.929 -0.0919 0.342 0.039 Uiso 1 1 calc R . . C87 C 0.9193(3) -0.04581(17) 0.28673(15) 0.0310(8) Uani 1 1 d . . . H87 H 0.9578 -0.0695 0.2724 0.037 Uiso 1 1 calc R . . C88 C 0.8151(3) -0.03663(18) 0.38933(14) 0.0311(8) Uani 1 1 d . . . N89 N 0.7546(3) 0.00237(16) 0.40143(11) 0.0286(7) Uani 1 1 d . . . C90 C 0.7208(4) -0.0064(2) 0.43859(14) 0.0384(10) Uani 1 1 d . . . H90 H 0.6754 0.0194 0.4465 0.046 Uiso 1 1 calc R . . C91 C 0.7499(4) -0.0515(3) 0.46545(16) 0.0467(12) Uani 1 1 d . . . C92 C 0.8125(5) -0.0909(3) 0.4537(2) 0.0527(14) Uani 1 1 d . . . H92 H 0.8324 -0.1225 0.4714 0.063 Uiso 1 1 calc R . . C93 C 0.8452(4) -0.0826(2) 0.41484(18) 0.0442(11) Uani 1 1 d . . . H93 H 0.8886 -0.1088 0.4058 0.053 Uiso 1 1 calc R . . C94 C 0.7083(5) -0.0565(4) 0.5063(2) 0.0644(19) Uani 1 1 d . . . O95 O 0.7214(5) -0.1003(3) 0.52801(19) 0.092(2) Uani 1 1 d . . . O96 O 0.6563(4) -0.0140(3) 0.51402(16) 0.0838(19) Uani 1 1 d . . . S1A S 0.11643(6) 0.23039(3) 0.12317(3) 0.01984(17) Uani 1 1 d . . . O1A O 0.0102(2) 0.22625(12) 0.10453(10) 0.0272(6) Uani 1 1 d . . . O2A O 0.1553(2) 0.28363(11) 0.10877(9) 0.0231(5) Uani 1 1 d . . . O3A O 0.1688(2) 0.18350(11) 0.10733(10) 0.0275(6) Uani 1 1 d . . . O4A O 0.1327(2) 0.22982(12) 0.17059(9) 0.0265(6) Uani 1 1 d . . . S1B S 1.17958(12) -0.09885(7) 0.26353(5) 0.0538(3) Uani 1 1 d D . . O1B O 1.1032(2) -0.13922(14) 0.25192(14) 0.0454(9) Uani 1 1 d D . . O2B O 1.1499(3) -0.0408(2) 0.2529(2) 0.0781(17) Uani 1 1 d D . . O3B O 1.2004(5) -0.0987(3) 0.31162(18) 0.0815(16) Uani 1 1 d D . . O4B O 1.2706(3) -0.11370(18) 0.2516(2) 0.0713(15) Uani 1 1 d D . . O14A O 0.5476(6) 0.0039(4) 0.0695(2) 0.0447(17) Uani 0.5 1 d P A -1 O14B O 0.5343(8) 0.0529(6) 0.0617(3) 0.076(3) Uani 0.5 1 d P B -2 O15A O 0.3154(17) 0.0020(8) -0.0750(6) 0.130(9) Uani 0.5 1 d P C -3 O15B O 0.2616(11) -0.0186(6) -0.0835(3) 0.070(3) Uani 0.5 1 d P D -4 O16A O 0.578(4) -0.1036(18) 0.3779(15) 0.22(2) Uani 0.5 1 d P E -5 O16B O 0.5639(12) -0.0806(6) 0.3780(5) 0.068(3) Uani 0.5 1 d P F -6 O13A O 0.8065(8) -0.1870(4) 0.3075(3) 0.089(3) Uani 0.7 1 d P G -7 O13B O 0.808(3) -0.1935(17) 0.3405(15) 0.145(12) Uiso 0.3 1 d P H -8 O18 O -0.2154(11) 0.3280(6) -0.0192(3) 0.095(5) Uani 0.5 1 d P I -9 O19 O -0.0489(9) 0.3296(3) 0.2816(4) 0.100(5) Uani 0.5 1 d P J -10 O20 O 0.3754(12) 0.1342(6) 0.0140(4) 0.098(5) Uani 0.5 1 d P K -11 O21 O 0.2973(11) 0.1923(6) -0.0054(5) 0.092(4) Uani 0.5 1 d P L -12 O22 O 0.6554(12) -0.2200(6) 0.5012(6) 0.107(5) Uani 0.5 1 d P M -13 O23 O 1.0644(11) 0.0623(6) 0.3675(5) 0.088(4) Uiso 0.5 1 d P N -14 O24A O 0.3952(9) 0.1643(5) -0.0718(4) 0.072(3) Uiso 0.5 1 d P O -15 O24B O 0.3142(18) 0.1806(10) -0.0907(8) 0.145(7) Uiso 0.5 1 d P P -16 O25 O 0.5697(12) 0.2335(7) 0.3713(6) 0.107(5) Uiso 0.5 1 d P Q -17 O26 O 1.0071(14) -0.1944(7) 0.3060(6) 0.112(5) Uiso 0.5 1 d P R -18 O27A O 0.5870(10) -0.1748(6) 0.4318(4) 0.085(3) Uiso 0.5 1 d P S -19 O28B O 0.6245(14) -0.2021(8) 0.4115(6) 0.113(5) Uiso 0.5 1 d P T -20 O29 O 0.5594(12) 0.1482(7) 0.0644(5) 0.103(4) Uiso 0.5 1 d P U -21 O30 O 0.8024(17) -0.2415(9) 0.3871(8) 0.133(6) Uiso 0.5 1 d P V -22 O31 O 1.1705(14) 0.0418(8) 0.3093(6) 0.115(5) Uiso 0.5 1 d P W -23 O32 O 0.2579(14) 0.2398(8) -0.0676(6) 0.118(5) Uiso 0.5 1 d P X -24 O33 O 0.2361(17) 0.1403(10) 0.4011(8) 0.144(7) Uiso 0.5 1 d P Y -25 O36 O 0.662(2) -0.2249(11) 0.3739(9) 0.086(7) Uiso 0.25 1 d P Z -26 O35 O 1.087(2) -0.0374(12) 0.4146(9) 0.091(7) Uiso 0.25 1 d P A -27 O1 O 0.6220(4) 0.0658(2) 0.14058(14) 0.0643(13) Uani 1 1 d . B -28 O2 O 0.6475(3) -0.10904(17) 0.30275(17) 0.0596(11) Uani 1 1 d . C -29 O3 O 1.1851(3) -0.02607(17) 0.53375(14) 0.0505(9) Uani 1 1 d . D -30 O4 O 0.4960(5) 0.2963(3) 0.45407(18) 0.0766(15) Uani 1 1 d . E -31 O5 O 0.1815(5) 0.2311(3) 0.26347(18) 0.0808(16) Uani 1 1 d . F -32 O6 O 0.9774(4) 0.1292(2) 0.29419(19) 0.0746(14) Uani 1 1 d . G -33 O7 O 0.4642(4) 0.1772(3) 0.2977(2) 0.0853(18) Uani 1 1 d . H -34 O8 O 0.3657(5) 0.0183(5) 0.0127(2) 0.116(3) Uani 1 1 d . I -35 O9 O 0.1590(8) 0.1379(2) 0.02686(18) 0.106(3) Uani 1 1 d . J -36 O10 O 0.2795(5) 0.1456(3) 0.3152(3) 0.110(3) Uani 1 1 d . K -37 O11 O -0.1185(5) 0.2375(4) 0.02313(19) 0.107(3) Uani 1 1 d . L -38 O12 O 0.0394(6) 0.2386(3) 0.3150(4) 0.127(4) Uani 1 1 d . M -39 O13 O 1.3599(8) -0.0765(4) 0.3747(3) 0.124(3) Uani 1 1 d . N -40 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0202(2) 0.0341(3) 0.0160(2) -0.0021(2) 0.00190(18) -0.0022(2) C1 0.0233(17) 0.0194(16) 0.0254(17) 0.0003(13) 0.0016(14) 0.0007(13) C2 0.0294(19) 0.0211(16) 0.0280(18) -0.0041(14) -0.0008(15) 0.0000(14) C3 0.034(2) 0.0264(18) 0.0276(18) -0.0036(15) -0.0024(16) -0.0015(15) C4 0.0253(19) 0.0260(18) 0.033(2) -0.0004(15) -0.0056(16) -0.0031(14) C5 0.0220(18) 0.0218(17) 0.0284(18) 0.0006(14) -0.0001(14) -0.0040(13) C6 0.0189(16) 0.0183(15) 0.0267(18) 0.0005(13) -0.0026(13) -0.0011(12) C7 0.0188(16) 0.0222(17) 0.0334(19) 0.0018(14) 0.0011(14) 0.0005(13) N8 0.0220(15) 0.0188(14) 0.0323(16) 0.0028(12) 0.0055(13) 0.0004(11) C9 0.0194(17) 0.0238(17) 0.0325(19) 0.0015(14) 0.0074(14) 0.0008(13) C10 0.0260(18) 0.0242(17) 0.0242(16) 0.0015(13) 0.0098(14) 0.0015(13) N11 0.0179(14) 0.0220(14) 0.0247(14) 0.0013(11) 0.0039(11) 0.0037(11) C12 0.0207(17) 0.0219(16) 0.0312(18) -0.0017(14) 0.0103(14) 0.0013(13) C13 0.0255(18) 0.0223(16) 0.0285(18) -0.0038(14) 0.0074(15) -0.0013(13) C14 0.0221(17) 0.0213(16) 0.0256(17) -0.0027(13) 0.0063(14) 0.0002(13) C15 0.0206(16) 0.0172(15) 0.0277(17) -0.0008(13) 0.0034(14) 0.0030(12) C16 0.0205(17) 0.0277(18) 0.0303(19) 0.0012(15) 0.0031(14) 0.0040(14) C17 0.029(2) 0.033(2) 0.0271(18) 0.0071(15) 0.0025(16) 0.0063(15) C18 0.0274(19) 0.0309(19) 0.032(2) 0.0047(16) 0.0116(16) 0.0056(15) C19 0.0216(17) 0.0212(16) 0.0317(19) 0.0015(14) 0.0043(14) 0.0021(13) C20 0.0200(17) 0.0232(16) 0.0255(17) -0.0012(13) 0.0046(14) 0.0038(13) C21 0.0229(18) 0.0253(18) 0.036(2) 0.0025(15) 0.0078(15) -0.0006(14) N22 0.0169(14) 0.0252(15) 0.0356(17) -0.0038(13) 0.0036(13) -0.0001(11) C23 0.0184(16) 0.0210(16) 0.036(2) -0.0046(14) 0.0052(15) -0.0012(12) C24 0.0227(17) 0.0242(17) 0.0291(18) -0.0060(14) 0.0067(14) -0.0034(13) N25 0.0158(13) 0.0239(15) 0.0262(15) 0.0004(12) 0.0036(11) -0.0014(11) C26 0.0184(16) 0.0272(18) 0.0327(19) -0.0059(15) 0.0000(14) -0.0024(13) C27 0.0188(17) 0.0295(19) 0.035(2) -0.0046(16) 0.0042(15) 0.0027(14) C28 0.0182(16) 0.0225(16) 0.0256(17) -0.0013(13) 0.0004(13) -0.0015(12) C29 0.0180(16) 0.0250(17) 0.0286(18) -0.0037(14) 0.0075(14) -0.0017(12) C30 0.0215(18) 0.0296(19) 0.031(2) 0.0034(15) 0.0080(15) -0.0024(14) C31 0.0271(19) 0.038(2) 0.0265(18) -0.0024(16) 0.0094(15) -0.0025(16) C32 0.030(2) 0.035(2) 0.0287(19) -0.0085(16) 0.0096(16) -0.0010(16) C33 0.0209(17) 0.0285(18) 0.0289(18) -0.0043(14) 0.0087(14) -0.0004(13) C34 0.0197(16) 0.0273(18) 0.0280(18) -0.0030(14) 0.0100(14) -0.0002(13) C35 0.0214(17) 0.0274(18) 0.035(2) -0.0052(15) 0.0087(15) 0.0004(13) N36 0.0206(15) 0.0206(14) 0.0323(16) -0.0012(12) 0.0056(13) 0.0014(11) C37 0.0213(17) 0.0220(17) 0.0318(19) 0.0011(14) 0.0013(14) -0.0004(13) C38 0.0226(17) 0.0252(17) 0.0261(17) 0.0029(14) -0.0015(14) 0.0037(13) N39 0.0219(15) 0.0207(14) 0.0238(14) 0.0004(11) 0.0014(12) 0.0014(11) C40 0.0264(19) 0.0206(17) 0.037(2) 0.0064(14) 0.0036(16) 0.0011(13) C41 0.0244(19) 0.0264(18) 0.032(2) 0.0058(15) 0.0074(16) 0.0025(14) C42 0.0200(17) 0.0231(16) 0.0258(17) 0.0005(13) 0.0032(14) -0.0015(13) N43 0.0240(15) 0.0221(14) 0.0234(15) 0.0006(11) 0.0046(12) -0.0011(11) C44 0.0247(18) 0.0260(17) 0.0208(16) -0.0031(13) -0.0005(14) -0.0006(13) O45 0.0257(14) 0.0392(16) 0.0240(13) -0.0079(11) 0.0058(11) -0.0101(11) C46 0.0218(17) 0.0313(19) 0.0217(16) -0.0037(14) 0.0029(14) -0.0021(14) C47 0.0258(18) 0.0290(18) 0.0201(16) -0.0014(14) 0.0042(14) -0.0021(14) N48 0.0220(15) 0.0366(17) 0.0170(13) -0.0023(12) 0.0007(12) -0.0024(12) C49 0.0225(18) 0.044(2) 0.0231(18) -0.0021(16) 0.0027(15) 0.0010(16) C50 0.0248(19) 0.052(3) 0.0238(18) -0.0107(17) 0.0039(15) -0.0013(17) C51 0.0205(18) 0.045(2) 0.0254(18) -0.0047(16) 0.0021(14) -0.0019(15) C52 0.0208(19) 0.056(3) 0.0215(18) -0.0043(18) 0.0000(15) -0.0063(18) N53 0.0235(16) 0.049(2) 0.0203(15) -0.0069(14) 0.0031(12) -0.0030(14) C54 0.029(2) 0.051(3) 0.0184(17) -0.0115(16) 0.0033(15) -0.0066(18) C55 0.031(2) 0.059(3) 0.0236(19) -0.0129(19) 0.0059(17) -0.0057(19) C56 0.031(2) 0.069(3) 0.033(2) -0.011(2) 0.0128(19) -0.001(2) C57 0.020(2) 0.074(4) 0.034(2) -0.016(2) 0.0045(17) -0.006(2) C58 0.041(2) 0.053(3) 0.0185(17) -0.0075(17) 0.0067(17) -0.002(2) O59 0.045(2) 0.062(2) 0.0315(16) -0.0236(16) 0.0133(15) -0.0138(17) O60 0.042(2) 0.088(3) 0.0311(17) -0.0260(18) 0.0109(15) -0.019(2) N61 0.0203(14) 0.0251(15) 0.0234(15) -0.0019(12) 0.0010(12) 0.0026(11) C62 0.0166(16) 0.0321(19) 0.0238(17) 0.0037(14) 0.0019(13) 0.0022(13) O63 0.0340(16) 0.0253(13) 0.0283(14) -0.0021(11) -0.0033(12) 0.0015(11) C64 0.0207(17) 0.034(2) 0.0246(17) 0.0005(15) 0.0019(14) 0.0025(14) C65 0.0233(17) 0.0294(18) 0.0201(16) -0.0016(14) 0.0031(13) 0.0008(14) N66 0.0194(14) 0.0307(16) 0.0185(14) -0.0018(12) 0.0022(11) 0.0006(12) C67 0.0240(18) 0.032(2) 0.0259(18) -0.0029(15) -0.0016(14) -0.0003(15) C68 0.028(2) 0.037(2) 0.035(2) -0.0023(17) -0.0039(17) -0.0046(16) C69 0.0262(19) 0.035(2) 0.033(2) 0.0032(16) 0.0011(16) -0.0007(15) C70 0.032(2) 0.033(2) 0.0239(18) -0.0011(15) -0.0018(16) 0.0006(16) N71 0.0227(16) 0.0360(18) 0.0219(15) -0.0023(13) 0.0014(12) -0.0014(13) C72 0.0252(19) 0.040(2) 0.0230(18) 0.0018(16) -0.0016(15) -0.0017(16) C73 0.031(2) 0.040(2) 0.031(2) 0.0031(18) -0.0122(17) -0.0031(18) C74 0.051(3) 0.041(3) 0.042(3) 0.005(2) -0.026(2) -0.010(2) C75 0.052(3) 0.037(2) 0.038(2) 0.001(2) -0.018(2) -0.004(2) C76 0.040(3) 0.045(3) 0.035(2) 0.011(2) -0.016(2) -0.005(2) O77 0.065(3) 0.056(3) 0.084(3) 0.024(2) -0.051(3) -0.024(2) O78 0.0338(18) 0.0430(19) 0.0471(19) 0.0112(15) -0.0159(15) -0.0092(14) N79 0.0211(15) 0.0276(16) 0.0261(15) -0.0010(12) 0.0041(12) 0.0001(12) C80 0.0277(19) 0.0242(17) 0.0251(17) -0.0028(14) 0.0075(15) -0.0023(14) O81 0.0303(15) 0.0343(15) 0.0264(13) 0.0050(11) 0.0100(11) 0.0084(12) C82 0.0238(18) 0.0263(18) 0.0243(17) -0.0024(14) 0.0046(14) 0.0006(13) C83 0.0224(17) 0.0290(18) 0.0214(16) -0.0003(14) 0.0050(14) 0.0004(13) N84 0.0209(15) 0.0280(16) 0.0209(14) -0.0006(12) 0.0022(12) -0.0024(12) C85 0.0279(19) 0.0293(19) 0.0233(17) 0.0016(14) 0.0008(15) -0.0035(14) C86 0.039(2) 0.0267(19) 0.034(2) 0.0059(16) 0.0088(18) 0.0040(16) C87 0.035(2) 0.0252(18) 0.034(2) 0.0003(16) 0.0086(17) 0.0047(15) C88 0.031(2) 0.035(2) 0.0266(19) 0.0024(16) 0.0039(16) -0.0052(16) N89 0.0229(16) 0.0400(19) 0.0222(15) 0.0002(13) 0.0025(12) -0.0066(13) C90 0.031(2) 0.061(3) 0.0223(18) 0.0052(19) 0.0032(16) -0.007(2) C91 0.047(3) 0.064(3) 0.028(2) 0.013(2) 0.006(2) -0.009(2) C92 0.064(4) 0.052(3) 0.045(3) 0.022(2) 0.016(3) 0.001(3) C93 0.052(3) 0.043(3) 0.039(3) 0.015(2) 0.011(2) 0.006(2) C94 0.057(4) 0.103(5) 0.034(3) 0.022(3) 0.010(3) -0.020(4) O95 0.101(4) 0.117(5) 0.063(3) 0.055(3) 0.029(3) -0.003(4) O96 0.066(3) 0.148(6) 0.044(2) 0.024(3) 0.029(2) 0.017(3) S1A 0.0188(4) 0.0189(4) 0.0218(4) 0.0027(3) 0.0040(3) 0.0008(3) O1A 0.0193(13) 0.0269(14) 0.0333(15) 0.0066(11) 0.0003(11) 0.0016(10) O2A 0.0279(13) 0.0189(12) 0.0234(12) 0.0035(10) 0.0073(10) -0.0017(10) O3A 0.0246(13) 0.0226(13) 0.0349(14) -0.0012(11) 0.0053(11) 0.0042(10) O4A 0.0268(14) 0.0305(14) 0.0221(13) 0.0044(10) 0.0044(11) 0.0006(10) S1B 0.0488(8) 0.0536(8) 0.0583(8) 0.0008(6) 0.0088(6) 0.0000(6) O1B 0.0295(17) 0.0274(15) 0.076(3) -0.0067(16) 0.0013(16) 0.0075(12) O2B 0.038(2) 0.074(3) 0.130(5) 0.040(3) 0.033(3) 0.010(2) O3B 0.076(4) 0.098(4) 0.066(3) -0.002(3) 0.004(3) -0.004(3) O4B 0.049(2) 0.040(2) 0.132(5) 0.002(3) 0.034(3) -0.0008(17) O14A 0.043(4) 0.067(5) 0.025(3) 0.010(3) 0.010(3) 0.016(3) O14B 0.060(6) 0.125(10) 0.046(5) -0.009(6) 0.017(4) 0.032(6) O15A 0.137(16) 0.122(13) 0.097(11) -0.061(10) -0.064(11) 0.052(11) O15B 0.095(9) 0.084(8) 0.036(5) 0.013(5) 0.022(5) 0.042(7) O16A 0.24(4) 0.22(4) 0.19(3) 0.03(3) -0.01(3) -0.14(4) O16B 0.063(6) 0.065(7) 0.064(6) 0.028(5) -0.015(5) -0.029(5) O13A 0.112(7) 0.067(5) 0.071(5) 0.014(4) -0.028(5) -0.014(4) O18 0.118(10) 0.098(9) 0.049(5) -0.028(5) -0.031(6) 0.050(8) O19 0.107(9) 0.034(4) 0.117(9) 0.034(5) -0.082(8) -0.036(5) O20 0.122(11) 0.098(9) 0.083(8) -0.033(7) 0.041(8) -0.048(8) O21 0.109(10) 0.083(8) 0.098(9) -0.037(7) 0.052(8) -0.019(7) O22 0.100(10) 0.093(9) 0.141(13) -0.049(9) 0.054(10) -0.030(8) O1 0.062(3) 0.096(4) 0.0312(19) -0.011(2) -0.0024(18) 0.024(2) O2 0.054(2) 0.041(2) 0.080(3) -0.017(2) 0.002(2) -0.0026(17) O3 0.045(2) 0.052(2) 0.048(2) 0.0101(17) -0.0081(17) 0.0042(16) O4 0.086(4) 0.079(3) 0.064(3) 0.029(3) 0.010(3) 0.015(3) O5 0.085(4) 0.102(4) 0.052(3) 0.001(3) 0.003(3) -0.011(3) O6 0.072(3) 0.070(3) 0.080(3) 0.011(3) 0.011(3) -0.022(3) O7 0.055(3) 0.092(4) 0.115(5) 0.026(4) 0.032(3) 0.013(3) O8 0.050(3) 0.218(10) 0.079(4) 0.028(5) 0.009(3) 0.027(4) O9 0.224(9) 0.047(3) 0.055(3) -0.006(2) 0.046(4) 0.009(4) O10 0.082(5) 0.099(5) 0.155(7) 0.030(5) 0.038(5) 0.019(4) O11 0.073(4) 0.188(8) 0.049(3) 0.005(4) -0.015(3) 0.003(4) O12 0.078(4) 0.075(4) 0.242(12) 0.024(5) 0.064(6) 0.000(3) O13 0.138(8) 0.138(7) 0.082(5) 0.009(4) -0.011(5) -0.004(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Fe N84 1.963(3) . ? Fe N53 1.967(4) . ? Fe N48 1.968(3) . ? Fe N66 1.968(3) . ? Fe N71 1.971(3) . ? Fe N89 1.979(4) . ? C1 C6 1.397(5) . ? C1 C2 1.404(5) . ? C1 C42 1.511(5) . ? C2 C3 1.381(6) . ? C2 H2 0.95 . ? C3 C4 1.383(6) . ? C3 H3 0.95 . ? C4 C5 1.411(6) . ? C4 H4 0.95 . ? C5 C6 1.391(5) . ? C5 C7 1.508(5) . ? C6 N43 1.425(5) . ? C7 N8 1.473(5) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? N8 C9 1.465(5) . ? N8 C13 1.469(5) . ? C9 C10 1.516(5) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 N11 1.501(5) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? N11 C14 1.510(5) . ? N11 C12 1.511(5) . ? N11 H11 0.93 . ? C12 C13 1.506(5) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.504(5) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.388(5) . ? C15 C20 1.410(5) . ? C16 C17 1.393(6) . ? C16 H16 0.95 . ? C17 C18 1.398(6) . ? C17 H17 0.95 . ? C18 C19 1.389(6) . ? C18 H18 0.95 . ? C19 C20 1.386(6) . ? C19 C21 1.527(5) . ? C20 N61 1.436(5) . ? C21 N22 1.465(5) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? N22 C27 1.449(5) . ? N22 C23 1.475(5) . ? C23 C24 1.508(5) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 N25 1.501(5) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? N25 C26 1.512(5) . ? N25 C28 1.515(5) . ? N25 H25 0.93 . ? C26 C27 1.519(6) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 C29 1.517(5) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 C34 1.391(5) . ? C29 C30 1.399(6) . ? C30 C31 1.373(6) . ? C30 H30 0.95 . ? C31 C32 1.411(6) . ? C31 H31 0.95 . ? C32 C33 1.402(6) . ? C32 H32 0.95 . ? C33 C34 1.392(5) . ? C33 C35 1.504(6) . ? C34 N79 1.430(5) . ? C35 N36 1.475(5) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? N36 C41 1.457(5) . ? N36 C37 1.466(5) . ? C37 C38 1.516(5) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 N39 1.507(5) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? N39 C42 1.506(5) . ? N39 C40 1.512(5) . ? N39 H39 0.93 . ? C40 C41 1.517(6) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? N43 C44 1.344(5) . ? N43 H43 0.88 . ? C44 O45 1.236(5) . ? C44 C46 1.494(5) . ? C46 C47 1.382(5) . ? C46 C51 1.392(6) . ? C47 N48 1.324(5) . ? C47 H47 0.95 . ? N48 C49 1.364(5) . ? C49 C50 1.384(6) . ? C49 C52 1.468(6) . ? C50 C51 1.378(6) . ? C50 H50 0.95 . ? C51 H51 0.95 . ? C52 N53 1.378(5) . ? C52 C57 1.386(6) . ? N53 C54 1.346(5) . ? C54 C55 1.392(6) . ? C54 H54 0.95 . ? C55 C56 1.393(7) . ? C55 C58 1.509(6) . ? C56 C57 1.362(7) . ? C56 H56 0.95 . ? C57 H57 0.95 . ? C58 O60 1.195(6) . ? C58 O59 1.312(6) . ? O59 H59 0.84 . ? N61 C62 1.350(5) . ? N61 H61 0.88 . ? C62 O63 1.220(5) . ? C62 C64 1.492(5) . ? C64 C69 1.377(6) . ? C64 C65 1.391(6) . ? C65 N66 1.341(5) . ? C65 H65 0.95 . ? N66 C67 1.369(5) . ? C67 C68 1.377(6) . ? C67 C70 1.485(6) . ? C68 C69 1.400(6) . ? C68 H68 0.95 . ? C69 H69 0.95 . ? C70 N71 1.354(6) . ? C70 C75 1.367(6) . ? N71 C72 1.352(5) . ? C72 C73 1.401(6) . ? C72 H72 0.95 . ? C73 C74 1.371(7) . ? C73 C76 1.474(6) . ? C74 C75 1.383(7) . ? C74 H74 0.95 . ? C75 H75 0.95 . ? C76 O77 1.199(6) . ? C76 O78 1.323(6) . ? O78 H78 0.84 . ? N79 C80 1.340(5) . ? N79 H79 0.88 . ? C80 O81 1.229(5) . ? C80 C82 1.497(5) . ? C82 C87 1.388(6) . ? C82 C83 1.402(5) . ? C83 N84 1.337(5) . ? C83 H83 0.95 . ? N84 C85 1.368(5) . ? C85 C86 1.384(6) . ? C85 C88 1.462(6) . ? C86 C87 1.388(6) . ? C86 H86 0.95 . ? C87 H87 0.95 . ? C88 N89 1.360(6) . ? C88 C93 1.380(7) . ? N89 C90 1.351(6) . ? C90 C91 1.382(8) . ? C90 H90 0.95 . ? C91 C92 1.384(9) . ? C91 C94 1.504(8) . ? C92 C93 1.391(8) . ? C92 H92 0.95 . ? C93 H93 0.95 . ? C94 O95 1.245(10) . ? C94 O96 1.301(11) . ? S1A O4A 1.457(3) . ? S1A O3A 1.477(3) . ? S1A O1A 1.482(3) . ? S1A O2A 1.492(3) . ? S1B O4B 1.430(5) . ? S1B O1B 1.431(4) . ? S1B O2B 1.474(5) . ? S1B O3B 1.476(6) . ? 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 N84 Fe N53 171.35(15) . . ? N84 Fe N48 93.53(14) . . ? N53 Fe N48 81.18(14) . . ? N84 Fe N66 95.10(14) . . ? N53 Fe N66 92.12(15) . . ? N48 Fe N66 94.08(14) . . ? N84 Fe N71 92.54(14) . . ? N53 Fe N71 93.32(15) . . ? N48 Fe N71 172.39(16) . . ? N66 Fe N71 80.79(14) . . ? N84 Fe N89 80.96(14) . . ? N53 Fe N89 92.44(16) . . ? N48 Fe N89 93.14(14) . . ? N66 Fe N89 171.97(14) . . ? N71 Fe N89 92.35(15) . . ? C6 C1 C2 118.6(3) . . ? C6 C1 C42 120.7(3) . . ? C2 C1 C42 120.7(3) . . ? C3 C2 C1 120.4(4) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 120.9(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 119.1(4) . . ? C6 C5 C7 121.2(4) . . ? C4 C5 C7 119.7(4) . . ? C5 C6 C1 121.2(4) . . ? C5 C6 N43 118.5(3) . . ? C1 C6 N43 120.3(3) . . ? N8 C7 C5 111.4(3) . . ? N8 C7 H7A 109.3 . . ? C5 C7 H7A 109.3 . . ? N8 C7 H7B 109.3 . . ? C5 C7 H7B 109.3 . . ? H7A C7 H7B 108 . . ? C9 N8 C13 109.0(3) . . ? C9 N8 C7 110.3(3) . . ? C13 N8 C7 111.8(3) . . ? N8 C9 C10 110.2(3) . . ? N8 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? N8 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? N11 C10 C9 110.1(3) . . ? N11 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? N11 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.2 . . ? C10 N11 C14 110.3(3) . . ? C10 N11 C12 109.0(3) . . ? C14 N11 C12 114.5(3) . . ? C10 N11 H11 107.6 . . ? C14 N11 H11 107.6 . . ? C12 N11 H11 107.6 . . ? C13 C12 N11 109.2(3) . . ? C13 C12 H12A 109.8 . . ? N11 C12 H12A 109.8 . . ? C13 C12 H12B 109.8 . . ? N11 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? N8 C13 C12 110.7(3) . . ? N8 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? N8 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 N11 114.5(3) . . ? C15 C14 H14A 108.6 . . ? N11 C14 H14A 108.6 . . ? C15 C14 H14B 108.6 . . ? N11 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C16 C15 C20 118.5(4) . . ? C16 C15 C14 121.5(3) . . ? C20 C15 C14 119.9(3) . . ? C15 C16 C17 121.2(4) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C18 119.2(4) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 120.8(4) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 119.3(4) . . ? C20 C19 C21 120.0(4) . . ? C18 C19 C21 120.6(4) . . ? C19 C20 C15 120.9(4) . . ? C19 C20 N61 118.6(3) . . ? C15 C20 N61 120.5(3) . . ? N22 C21 C19 110.5(3) . . ? N22 C21 H21A 109.5 . . ? C19 C21 H21A 109.5 . . ? N22 C21 H21B 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C27 N22 C21 112.9(3) . . ? C27 N22 C23 109.2(3) . . ? C21 N22 C23 109.8(3) . . ? N22 C23 C24 110.2(3) . . ? N22 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? N22 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N25 C24 C23 110.4(3) . . ? N25 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? N25 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C24 N25 C26 108.8(3) . . ? C24 N25 C28 109.4(3) . . ? C26 N25 C28 114.2(3) . . ? C24 N25 H25 108.1 . . ? C26 N25 H25 108.1 . . ? C28 N25 H25 108.1 . . ? N25 C26 C27 108.8(3) . . ? N25 C26 H26A 109.9 . . ? C27 C26 H26A 109.9 . . ? N25 C26 H26B 109.9 . . ? C27 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? N22 C27 C26 110.8(3) . . ? N22 C27 H27A 109.5 . . ? C26 C27 H27A 109.5 . . ? N22 C27 H27B 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? N25 C28 C29 113.8(3) . . ? N25 C28 H28A 108.8 . . ? C29 C28 H28A 108.8 . . ? N25 C28 H28B 108.8 . . ? C29 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C34 C29 C30 119.0(4) . . ? C34 C29 C28 119.5(3) . . ? C30 C29 C28 121.5(3) . . ? C31 C30 C29 120.8(4) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 120.0(4) . . ? C30 C31 H31 120 . . ? C32 C31 H31 120 . . ? C33 C32 C31 119.9(4) . . ? C33 C32 H32 120 . . ? C31 C32 H32 120 . . ? C34 C33 C32 118.8(4) . . ? C34 C33 C35 120.7(4) . . ? C32 C33 C35 120.5(4) . . ? C29 C34 C33 121.5(4) . . ? C29 C34 N79 120.5(3) . . ? C33 C34 N79 118.0(4) . . ? N36 C35 C33 110.8(3) . . ? N36 C35 H35A 109.5 . . ? C33 C35 H35A 109.5 . . ? N36 C35 H35B 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C41 N36 C37 108.8(3) . . ? C41 N36 C35 112.2(3) . . ? C37 N36 C35 110.6(3) . . ? N36 C37 C38 110.7(3) . . ? N36 C37 H37A 109.5 . . ? C38 C37 H37A 109.5 . . ? N36 C37 H37B 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? N39 C38 C37 109.5(3) . . ? N39 C38 H38A 109.8 . . ? C37 C38 H38A 109.8 . . ? N39 C38 H38B 109.8 . . ? C37 C38 H38B 109.8 . . ? H38A C38 H38B 108.2 . . ? C42 N39 C38 110.0(3) . . ? C42 N39 C40 114.1(3) . . ? C38 N39 C40 109.2(3) . . ? C42 N39 H39 107.8 . . ? C38 N39 H39 107.8 . . ? C40 N39 H39 107.8 . . ? N39 C40 C41 109.8(3) . . ? N39 C40 H40A 109.7 . . ? C41 C40 H40A 109.7 . . ? N39 C40 H40B 109.7 . . ? C41 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? N36 C41 C40 110.7(3) . . ? N36 C41 H41A 109.5 . . ? C40 C41 H41A 109.5 . . ? N36 C41 H41B 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? N39 C42 C1 113.6(3) . . ? N39 C42 H42A 108.8 . . ? C1 C42 H42A 108.8 . . ? N39 C42 H42B 108.8 . . ? C1 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C44 N43 C6 120.1(3) . . ? C44 N43 H43 120 . . ? C6 N43 H43 120 . . ? O45 C44 N43 123.1(3) . . ? O45 C44 C46 118.8(3) . . ? N43 C44 C46 118.1(3) . . ? C47 C46 C51 118.9(4) . . ? C47 C46 C44 116.4(3) . . ? C51 C46 C44 124.6(4) . . ? N48 C47 C46 124.2(4) . . ? N48 C47 H47 117.9 . . ? C46 C47 H47 117.9 . . ? C47 N48 C49 116.4(3) . . ? C47 N48 Fe 127.3(3) . . ? C49 N48 Fe 116.2(3) . . ? N48 C49 C50 123.1(4) . . ? N48 C49 C52 113.0(4) . . ? C50 C49 C52 123.8(4) . . ? C51 C50 C49 119.2(4) . . ? C51 C50 H50 120.4 . . ? C49 C50 H50 120.4 . . ? C50 C51 C46 118.1(4) . . ? C50 C51 H51 120.9 . . ? C46 C51 H51 120.9 . . ? N53 C52 C57 121.5(4) . . ? N53 C52 C49 113.9(4) . . ? C57 C52 C49 124.6(4) . . ? C54 N53 C52 117.6(4) . . ? C54 N53 Fe 126.8(3) . . ? C52 N53 Fe 114.9(3) . . ? N53 C54 C55 122.4(4) . . ? N53 C54 H54 118.8 . . ? C55 C54 H54 118.8 . . ? C54 C55 C56 119.4(4) . . ? C54 C55 C58 117.4(4) . . ? C56 C55 C58 123.2(4) . . ? C57 C56 C55 118.5(4) . . ? C57 C56 H56 120.8 . . ? C55 C56 H56 120.8 . . ? C56 C57 C52 120.5(4) . . ? C56 C57 H57 119.7 . . ? C52 C57 H57 119.7 . . ? O60 C58 O59 126.4(4) . . ? O60 C58 C55 122.8(4) . . ? O59 C58 C55 110.8(4) . . ? C58 O59 H59 109.5 . . ? C62 N61 C20 119.6(3) . . ? C62 N61 H61 120.2 . . ? C20 N61 H61 120.2 . . ? O63 C62 N61 123.8(3) . . ? O63 C62 C64 119.8(4) . . ? N61 C62 C64 116.4(3) . . ? C69 C64 C65 119.3(4) . . ? C69 C64 C62 125.3(4) . . ? C65 C64 C62 115.3(4) . . ? N66 C65 C64 123.1(4) . . ? N66 C65 H65 118.5 . . ? C64 C65 H65 118.5 . . ? C65 N66 C67 117.1(3) . . ? C65 N66 Fe 127.1(3) . . ? C67 N66 Fe 115.8(3) . . ? N66 C67 C68 122.8(4) . . ? N66 C67 C70 112.9(4) . . ? C68 C67 C70 124.2(4) . . ? C67 C68 C69 119.1(4) . . ? C67 C68 H68 120.5 . . ? C69 C68 H68 120.5 . . ? C64 C69 C68 118.4(4) . . ? C64 C69 H69 120.8 . . ? C68 C69 H69 120.8 . . ? N71 C70 C75 122.6(4) . . ? N71 C70 C67 113.3(4) . . ? C75 C70 C67 124.1(4) . . ? C72 N71 C70 117.4(4) . . ? C72 N71 Fe 126.5(3) . . ? C70 N71 Fe 116.1(3) . . ? N71 C72 C73 122.6(4) . . ? N71 C72 H72 118.7 . . ? C73 C72 H72 118.7 . . ? C74 C73 C72 118.4(4) . . ? C74 C73 C76 122.1(4) . . ? C72 C73 C76 119.5(4) . . ? C73 C74 C75 119.4(4) . . ? C73 C74 H74 120.3 . . ? C75 C74 H74 120.3 . . ? C70 C75 C74 119.6(5) . . ? C70 C75 H75 120.2 . . ? C74 C75 H75 120.2 . . ? O77 C76 O78 123.6(4) . . ? O77 C76 C73 122.9(5) . . ? O78 C76 C73 113.5(4) . . ? C76 O78 H78 109.5 . . ? C80 N79 C34 120.1(3) . . ? C80 N79 H79 120 . . ? C34 N79 H79 120 . . ? O81 C80 N79 123.4(4) . . ? O81 C80 C82 119.7(4) . . ? N79 C80 C82 116.9(4) . . ? C87 C82 C83 119.4(4) . . ? C87 C82 C80 125.8(4) . . ? C83 C82 C80 114.7(3) . . ? N84 C83 C82 122.6(4) . . ? N84 C83 H83 118.7 . . ? C82 C83 H83 118.7 . . ? C83 N84 C85 118.0(3) . . ? C83 N84 Fe 126.3(3) . . ? C85 N84 Fe 115.7(3) . . ? N84 C85 C86 121.8(4) . . ? N84 C85 C88 113.8(4) . . ? C86 C85 C88 124.4(4) . . ? C85 C86 C87 120.3(4) . . ? C85 C86 H86 119.9 . . ? C87 C86 H86 119.9 . . ? C86 C87 C82 117.9(4) . . ? C86 C87 H87 121.1 . . ? C82 C87 H87 121.1 . . ? N89 C88 C93 121.7(4) . . ? N89 C88 C85 113.6(4) . . ? C93 C88 C85 124.7(4) . . ? C90 N89 C88 117.9(4) . . ? C90 N89 Fe 126.4(4) . . ? C88 N89 Fe 115.5(3) . . ? N89 C90 C91 122.4(5) . . ? N89 C90 H90 118.8 . . ? C91 C90 H90 118.8 . . ? C90 C91 C92 120.0(5) . . ? C90 C91 C94 117.6(6) . . ? C92 C91 C94 122.3(6) . . ? C91 C92 C93 117.6(5) . . ? C91 C92 H92 121.2 . . ? C93 C92 H92 121.2 . . ? C88 C93 C92 120.4(5) . . ? C88 C93 H93 119.8 . . ? C92 C93 H93 119.8 . . ? O95 C94 O96 126.1(6) . . ? O95 C94 C91 119.4(8) . . ? O96 C94 C91 114.4(6) . . ? O4A S1A O3A 110.17(17) . . ? O4A S1A O1A 110.30(17) . . ? O3A S1A O1A 109.52(17) . . ? O4A S1A O2A 108.76(16) . . ? O3A S1A O2A 108.79(17) . . ? O1A S1A O2A 109.27(16) . . ? O4B S1B O1B 114.4(3) . . ? O4B S1B O2B 113.6(3) . . ? O1B S1B O2B 115.0(3) . . ? O4B S1B O3B 104.9(4) . . ? O1B S1B O3B 104.5(3) . . ? O2B S1B O3B 102.6(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.1(6) . . . . ? C42 C1 C2 C3 178.3(4) . . . . ? C1 C2 C3 C4 1.7(6) . . . . ? C2 C3 C4 C5 -0.8(6) . . . . ? C3 C4 C5 C6 -1.6(6) . . . . ? C3 C4 C5 C7 176.9(4) . . . . ? C4 C5 C6 C1 3.3(6) . . . . ? C7 C5 C6 C1 -175.2(3) . . . . ? C4 C5 C6 N43 -177.5(3) . . . . ? C7 C5 C6 N43 4.0(5) . . . . ? C2 C1 C6 C5 -2.4(6) . . . . ? C42 C1 C6 C5 179.2(3) . . . . ? C2 C1 C6 N43 178.3(3) . . . . ? C42 C1 C6 N43 0.0(5) . . . . ? C6 C5 C7 N8 60.9(5) . . . . ? C4 C5 C7 N8 -117.6(4) . . . . ? C5 C7 N8 C9 -176.7(3) . . . . ? C5 C7 N8 C13 61.8(4) . . . . ? C13 N8 C9 C10 -60.5(4) . . . . ? C7 N8 C9 C10 176.3(3) . . . . ? N8 C9 C10 N11 59.4(4) . . . . ? C9 C10 N11 C14 176.1(3) . . . . ? C9 C10 N11 C12 -57.3(4) . . . . ? C10 N11 C12 C13 57.5(4) . . . . ? C14 N11 C12 C13 -178.4(3) . . . . ? C9 N8 C13 C12 61.5(4) . . . . ? C7 N8 C13 C12 -176.2(3) . . . . ? N11 C12 C13 N8 -60.2(4) . . . . ? C10 N11 C14 C15 172.8(3) . . . . ? C12 N11 C14 C15 49.4(4) . . . . ? N11 C14 C15 C16 52.7(5) . . . . ? N11 C14 C15 C20 -131.4(3) . . . . ? C20 C15 C16 C17 1.7(6) . . . . ? C14 C15 C16 C17 177.7(4) . . . . ? C15 C16 C17 C18 0.4(6) . . . . ? C16 C17 C18 C19 -0.6(6) . . . . ? C17 C18 C19 C20 -1.3(6) . . . . ? C17 C18 C19 C21 176.7(4) . . . . ? C18 C19 C20 C15 3.5(6) . . . . ? C21 C19 C20 C15 -174.5(3) . . . . ? C18 C19 C20 N61 -176.5(3) . . . . ? C21 C19 C20 N61 5.5(5) . . . . ? C16 C15 C20 C19 -3.7(5) . . . . ? C14 C15 C20 C19 -179.7(3) . . . . ? C16 C15 C20 N61 176.2(3) . . . . ? C14 C15 C20 N61 0.2(5) . . . . ? C20 C19 C21 N22 61.7(5) . . . . ? C18 C19 C21 N22 -116.4(4) . . . . ? C19 C21 N22 C27 62.6(4) . . . . ? C19 C21 N22 C23 -175.3(3) . . . . ? C27 N22 C23 C24 -60.1(4) . . . . ? C21 N22 C23 C24 175.6(3) . . . . ? N22 C23 C24 N25 58.8(4) . . . . ? C23 C24 N25 C26 -57.5(4) . . . . ? C23 C24 N25 C28 177.1(3) . . . . ? C24 N25 C26 C27 57.5(4) . . . . ? C28 N25 C26 C27 -179.9(3) . . . . ? C21 N22 C27 C26 -176.0(3) . . . . ? C23 N22 C27 C26 61.6(4) . . . . ? N25 C26 C27 N22 -60.8(4) . . . . ? C24 N25 C28 C29 172.5(3) . . . . ? C26 N25 C28 C29 50.3(4) . . . . ? N25 C28 C29 C34 -135.0(4) . . . . ? N25 C28 C29 C30 46.7(5) . . . . ? C34 C29 C30 C31 0.7(6) . . . . ? C28 C29 C30 C31 179.1(4) . . . . ? C29 C30 C31 C32 0.5(6) . . . . ? C30 C31 C32 C33 0.1(6) . . . . ? C31 C32 C33 C34 -1.9(6) . . . . ? C31 C32 C33 C35 176.4(4) . . . . ? C30 C29 C34 C33 -2.7(6) . . . . ? C28 C29 C34 C33 178.9(3) . . . . ? C30 C29 C34 N79 179.3(3) . . . . ? C28 C29 C34 N79 0.9(5) . . . . ? C32 C33 C34 C29 3.3(6) . . . . ? C35 C33 C34 C29 -175.1(4) . . . . ? C32 C33 C34 N79 -178.6(4) . . . . ? C35 C33 C34 N79 3.0(5) . . . . ? C34 C33 C35 N36 62.0(5) . . . . ? C32 C33 C35 N36 -116.3(4) . . . . ? C33 C35 N36 C41 61.5(4) . . . . ? C33 C35 N36 C37 -176.8(3) . . . . ? C41 N36 C37 C38 -61.8(4) . . . . ? C35 N36 C37 C38 174.5(3) . . . . ? N36 C37 C38 N39 59.9(4) . . . . ? C37 C38 N39 C42 177.6(3) . . . . ? C37 C38 N39 C40 -56.5(4) . . . . ? C42 N39 C40 C41 179.8(3) . . . . ? C38 N39 C40 C41 56.2(4) . . . . ? C37 N36 C41 C40 61.3(4) . . . . ? C35 N36 C41 C40 -176.0(3) . . . . ? N39 C40 C41 N36 -59.3(4) . . . . ? C38 N39 C42 C1 172.7(3) . . . . ? C40 N39 C42 C1 49.6(4) . . . . ? C6 C1 C42 N39 -133.3(4) . . . . ? C2 C1 C42 N39 48.4(5) . . . . ? C5 C6 N43 C44 -103.0(4) . . . . ? C1 C6 N43 C44 76.3(5) . . . . ? C6 N43 C44 O45 -9.0(6) . . . . ? C6 N43 C44 C46 172.3(3) . . . . ? O45 C44 C46 C47 -32.1(6) . . . . ? N43 C44 C46 C47 146.7(4) . . . . ? O45 C44 C46 C51 144.4(4) . . . . ? N43 C44 C46 C51 -36.8(6) . . . . ? C51 C46 C47 N48 -1.9(6) . . . . ? C44 C46 C47 N48 174.9(4) . . . . ? C46 C47 N48 C49 -1.4(6) . . . . ? C46 C47 N48 Fe -177.2(3) . . . . ? N84 Fe N48 C47 -17.1(4) . . . . ? N53 Fe N48 C47 169.8(4) . . . . ? N66 Fe N48 C47 78.3(4) . . . . ? N71 Fe N48 C47 125.6(10) . . . . ? N89 Fe N48 C47 -98.2(4) . . . . ? N84 Fe N48 C49 167.0(3) . . . . ? N53 Fe N48 C49 -6.1(3) . . . . ? N66 Fe N48 C49 -97.6(3) . . . . ? N71 Fe N48 C49 -50.2(12) . . . . ? N89 Fe N48 C49 85.9(3) . . . . ? C47 N48 C49 C50 3.2(7) . . . . ? Fe N48 C49 C50 179.6(4) . . . . ? C47 N48 C49 C52 -173.9(4) . . . . ? Fe N48 C49 C52 2.4(5) . . . . ? N48 C49 C50 C51 -1.8(8) . . . . ? C52 C49 C50 C51 175.0(5) . . . . ? C49 C50 C51 C46 -1.5(7) . . . . ? C47 C46 C51 C50 3.2(7) . . . . ? C44 C46 C51 C50 -173.2(4) . . . . ? N48 C49 C52 N53 4.9(6) . . . . ? C50 C49 C52 N53 -172.2(5) . . . . ? N48 C49 C52 C57 -176.5(5) . . . . ? C50 C49 C52 C57 6.3(8) . . . . ? C57 C52 N53 C54 0.4(7) . . . . ? C49 C52 N53 C54 179.0(4) . . . . ? C57 C52 N53 Fe 171.4(4) . . . . ? C49 C52 N53 Fe -10.0(5) . . . . ? N84 Fe N53 C54 126.1(9) . . . . ? N48 Fe N53 C54 178.9(4) . . . . ? N66 Fe N53 C54 -87.3(4) . . . . ? N71 Fe N53 C54 -6.4(4) . . . . ? N89 Fe N53 C54 86.1(4) . . . . ? N84 Fe N53 C52 -43.9(11) . . . . ? N48 Fe N53 C52 8.8(3) . . . . ? N66 Fe N53 C52 102.6(3) . . . . ? N71 Fe N53 C52 -176.5(3) . . . . ? N89 Fe N53 C52 -84.0(3) . . . . ? C52 N53 C54 C55 0.8(7) . . . . ? Fe N53 C54 C55 -169.0(4) . . . . ? N53 C54 C55 C56 -0.3(8) . . . . ? N53 C54 C55 C58 177.6(5) . . . . ? C54 C55 C56 C57 -1.4(9) . . . . ? C58 C55 C56 C57 -179.1(6) . . . . ? C55 C56 C57 C52 2.6(9) . . . . ? N53 C52 C57 C56 -2.2(9) . . . . ? C49 C52 C57 C56 179.4(5) . . . . ? C54 C55 C58 O60 16.8(8) . . . . ? C56 C55 C58 O60 -165.4(6) . . . . ? C54 C55 C58 O59 -163.2(5) . . . . ? C56 C55 C58 O59 14.6(8) . . . . ? C19 C20 N61 C62 -102.9(4) . . . . ? C15 C20 N61 C62 77.1(5) . . . . ? C20 N61 C62 O63 -10.1(6) . . . . ? C20 N61 C62 C64 171.5(3) . . . . ? O63 C62 C64 C69 146.6(4) . . . . ? N61 C62 C64 C69 -35.0(6) . . . . ? O63 C62 C64 C65 -30.3(5) . . . . ? N61 C62 C64 C65 148.2(4) . . . . ? C69 C64 C65 N66 -3.9(6) . . . . ? C62 C64 C65 N66 173.2(3) . . . . ? C64 C65 N66 C67 -0.1(6) . . . . ? C64 C65 N66 Fe -179.6(3) . . . . ? N84 Fe N66 C65 78.4(3) . . . . ? N53 Fe N66 C65 -96.8(3) . . . . ? N48 Fe N66 C65 -15.5(3) . . . . ? N71 Fe N66 C65 170.1(3) . . . . ? N89 Fe N66 C65 138.6(10) . . . . ? N84 Fe N66 C67 -101.2(3) . . . . ? N53 Fe N66 C67 83.6(3) . . . . ? N48 Fe N66 C67 164.9(3) . . . . ? N71 Fe N66 C67 -9.4(3) . . . . ? N89 Fe N66 C67 -41.0(12) . . . . ? C65 N66 C67 C68 4.2(6) . . . . ? Fe N66 C67 C68 -176.2(4) . . . . ? C65 N66 C67 C70 -172.0(3) . . . . ? Fe N66 C67 C70 7.6(4) . . . . ? N66 C67 C68 C69 -4.2(7) . . . . ? C70 C67 C68 C69 171.5(4) . . . . ? C65 C64 C69 C68 3.7(6) . . . . ? C62 C64 C69 C68 -173.0(4) . . . . ? C67 C68 C69 C64 0.1(7) . . . . ? N66 C67 C70 N71 0.3(5) . . . . ? C68 C67 C70 N71 -175.7(4) . . . . ? N66 C67 C70 C75 178.1(5) . . . . ? C68 C67 C70 C75 2.0(8) . . . . ? C75 C70 N71 C72 -3.8(7) . . . . ? C67 C70 N71 C72 174.0(4) . . . . ? C75 C70 N71 Fe 174.1(4) . . . . ? C67 C70 N71 Fe -8.2(5) . . . . ? N84 Fe N71 C72 -77.9(4) . . . . ? N53 Fe N71 C72 95.7(4) . . . . ? N48 Fe N71 C72 139.3(10) . . . . ? N66 Fe N71 C72 -172.7(4) . . . . ? N89 Fe N71 C72 3.1(4) . . . . ? N84 Fe N71 C70 104.4(3) . . . . ? N53 Fe N71 C70 -81.9(3) . . . . ? N48 Fe N71 C70 -38.4(12) . . . . ? N66 Fe N71 C70 9.7(3) . . . . ? N89 Fe N71 C70 -174.5(3) . . . . ? C70 N71 C72 C73 1.5(6) . . . . ? Fe N71 C72 C73 -176.1(4) . . . . ? N71 C72 C73 C74 1.7(8) . . . . ? N71 C72 C73 C76 -175.6(5) . . . . ? C72 C73 C74 C75 -2.7(9) . . . . ? C76 C73 C74 C75 174.5(6) . . . . ? N71 C70 C75 C74 2.8(9) . . . . ? C67 C70 C75 C74 -174.7(5) . . . . ? C73 C74 C75 C70 0.6(10) . . . . ? C74 C73 C76 O77 5.6(10) . . . . ? C72 C73 C76 O77 -177.2(6) . . . . ? C74 C73 C76 O78 -176.3(6) . . . . ? C72 C73 C76 O78 0.9(8) . . . . ? C29 C34 N79 C80 75.7(5) . . . . ? C33 C34 N79 C80 -102.4(4) . . . . ? C34 N79 C80 O81 -7.3(6) . . . . ? C34 N79 C80 C82 172.7(3) . . . . ? O81 C80 C82 C87 141.7(4) . . . . ? N79 C80 C82 C87 -38.3(6) . . . . ? O81 C80 C82 C83 -35.5(5) . . . . ? N79 C80 C82 C83 144.5(4) . . . . ? C87 C82 C83 N84 -3.7(6) . . . . ? C80 C82 C83 N84 173.7(4) . . . . ? C82 C83 N84 C85 0.3(6) . . . . ? C82 C83 N84 Fe -177.5(3) . . . . ? N53 Fe N84 C83 132.0(9) . . . . ? N48 Fe N84 C83 80.0(3) . . . . ? N66 Fe N84 C83 -14.4(3) . . . . ? N71 Fe N84 C83 -95.4(3) . . . . ? N89 Fe N84 C83 172.7(3) . . . . ? N53 Fe N84 C85 -45.8(11) . . . . ? N48 Fe N84 C85 -97.8(3) . . . . ? N66 Fe N84 C85 167.8(3) . . . . ? N71 Fe N84 C85 86.8(3) . . . . ? N89 Fe N84 C85 -5.2(3) . . . . ? C83 N84 C85 C86 3.5(6) . . . . ? Fe N84 C85 C86 -178.5(3) . . . . ? C83 N84 C85 C88 -174.7(3) . . . . ? Fe N84 C85 C88 3.3(4) . . . . ? N84 C85 C86 C87 -3.9(7) . . . . ? C88 C85 C86 C87 174.2(4) . . . . ? C85 C86 C87 C82 0.4(7) . . . . ? C83 C82 C87 C86 3.2(6) . . . . ? C80 C82 C87 C86 -173.8(4) . . . . ? N84 C85 C88 N89 2.0(5) . . . . ? C86 C85 C88 N89 -176.2(4) . . . . ? N84 C85 C88 C93 -176.9(5) . . . . ? C86 C85 C88 C93 4.9(7) . . . . ? C93 C88 N89 C90 -2.9(7) . . . . ? C85 C88 N89 C90 178.2(4) . . . . ? C93 C88 N89 Fe 172.6(4) . . . . ? C85 C88 N89 Fe -6.3(5) . . . . ? N84 Fe N89 C90 -178.6(4) . . . . ? N53 Fe N89 C90 -4.2(4) . . . . ? N48 Fe N89 C90 -85.5(4) . . . . ? N66 Fe N89 C90 120.3(10) . . . . ? N71 Fe N89 C90 89.2(4) . . . . ? N84 Fe N89 C88 6.3(3) . . . . ? N53 Fe N89 C88 -179.3(3) . . . . ? N48 Fe N89 C88 99.4(3) . . . . ? N66 Fe N89 C88 -54.7(12) . . . . ? N71 Fe N89 C88 -85.9(3) . . . . ? C88 N89 C90 C91 3.7(7) . . . . ? Fe N89 C90 C91 -171.2(4) . . . . ? N89 C90 C91 C92 -2.9(8) . . . . ? N89 C90 C91 C94 179.2(5) . . . . ? C90 C91 C92 C93 1.1(9) . . . . ? C94 C91 C92 C93 178.9(6) . . . . ? N89 C88 C93 C92 1.3(8) . . . . ? C85 C88 C93 C92 -180.0(5) . . . . ? C91 C92 C93 C88 -0.3(9) . . . . ? C90 C91 C94 O95 169.8(7) . . . . ? C92 C91 C94 O95 -8.1(10) . . . . ? C90 C91 C94 O96 -6.7(9) . . . . ? C92 C91 C94 O96 175.5(6) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF