# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Kenji Matsumoto' _publ_contact_author_email matsuken@kochi-u.ac.jp loop_ _publ_author_name 'Tsutomu Katsuki' 'Kenji Matsumoto' H.Egami T.Oguma data_Fesalen_3Br2NpO_KM188 _database_code_depnum_ccdc_archive 'CCDC 854405' #TrackingRef ')(3-Br-2-NpO)]_KM188_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78H52Br1Fe1N2O3, C2H6O' _chemical_formula_sum 'C80 H58 Br Fe N2 O4' _chemical_formula_weight 1247.04 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.5514(16) _cell_length_b 16.0909(17) _cell_length_c 15.7159(17) _cell_angle_alpha 90.00 _cell_angle_beta 112.0170(10) _cell_angle_gamma 90.00 _cell_volume 3411.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.08 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1290 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8473 _exptl_absorpt_correction_T_max 0.9192 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 'focusing mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 39325 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.51 _reflns_number_total 15559 _reflns_number_gt 13510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.023(12) _refine_ls_number_reflns 15559 _refine_ls_number_parameters 793 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0986 _refine_ls_wR_factor_ref 0.2880 _refine_ls_wR_factor_gt 0.2757 _refine_ls_goodness_of_fit_ref 1.259 _refine_ls_restrained_S_all 1.259 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.40616(5) 0.20719(5) 0.85964(4) 0.01583(18) Uani 1 1 d . A 1 N1 N 0.3078(3) 0.2209(3) 0.9297(3) 0.0185(9) Uani 1 1 d . A 1 N2 N 0.4956(3) 0.2597(3) 0.9880(3) 0.0178(9) Uani 1 1 d . A 1 O1 O 0.2931(3) 0.2007(3) 0.7499(2) 0.0199(8) Uani 1 1 d . A 1 O2 O 0.4909(3) 0.2653(3) 0.8129(2) 0.0188(8) Uani 1 1 d . A 1 O3 O 0.4365(4) 0.0956(3) 0.8885(3) 0.0293(9) Uani 1 1 d . A 1 Br1 Br 0.36433(6) -0.01096(5) 1.00946(5) 0.0417(2) Uani 1 1 d . A 1 C1 C 0.3578(4) 0.2205(4) 1.0316(3) 0.0194(11) Uani 1 1 d . A 1 H1 H 0.3817 0.1625 1.0502 0.023 Uiso 1 1 calc R A 1 C2 C 0.2922(4) 0.2437(4) 1.0834(4) 0.0241(12) Uani 1 1 d . A 1 C3 C 0.2603(5) 0.3244(5) 1.0862(5) 0.0358(16) Uani 1 1 d . A 1 H3 H 0.2804 0.3675 1.0557 0.043 Uiso 1 1 calc R A 1 C4 C 0.1994(5) 0.3423(6) 1.1331(5) 0.0425(18) Uani 1 1 d . A 1 H4 H 0.1783 0.3977 1.1362 0.051 Uiso 1 1 calc R A 1 C5 C 0.1684(6) 0.2758(10) 1.1773(6) 0.071(4) Uani 1 1 d . A 1 H5 H 0.1263 0.2872 1.2097 0.085 Uiso 1 1 calc R A 1 C6 C 0.1984(6) 0.1978(7) 1.1731(5) 0.049(2) Uani 1 1 d . A 1 H6 H 0.1781 0.1545 1.2032 0.058 Uiso 1 1 calc R A 1 C7 C 0.2586(5) 0.1799(6) 1.1255(5) 0.0391(17) Uani 1 1 d . A 1 H7 H 0.2776 0.1240 1.1212 0.047 Uiso 1 1 calc R A 1 C8 C 0.2127(4) 0.2184(4) 0.8932(3) 0.0202(11) Uani 1 1 d . A 1 H8 H 0.1779 0.2242 0.9333 0.024 Uiso 1 1 calc R A 1 C9 C 0.1540(4) 0.2077(4) 0.7969(3) 0.0206(10) Uani 1 1 d . A 1 C10 C 0.1978(4) 0.1970(3) 0.7287(3) 0.0179(10) Uani 1 1 d . A 1 C11 C 0.1337(4) 0.1799(3) 0.6380(3) 0.0172(10) Uani 1 1 d . A 1 C12 C 0.0288(4) 0.1787(4) 0.6141(4) 0.0194(10) Uani 1 1 d . A 1 C13 C -0.0378(5) 0.1658(4) 0.5224(4) 0.0258(12) Uani 1 1 d . A 1 H13 H -0.0126 0.1570 0.4754 0.031 Uiso 1 1 calc R A 1 C14 C -0.1375(5) 0.1661(5) 0.5011(4) 0.0327(15) Uani 1 1 d . A 1 H14 H -0.1808 0.1594 0.4389 0.039 Uiso 1 1 calc R A 1 C15 C -0.1784(5) 0.1759(5) 0.5690(5) 0.0331(14) Uani 1 1 d . A 1 H15 H -0.2481 0.1738 0.5529 0.040 Uiso 1 1 calc R A 1 C16 C -0.1166(4) 0.1886(4) 0.6578(4) 0.0274(13) Uani 1 1 d . A 1 H16 H -0.1436 0.1960 0.7037 0.033 Uiso 1 1 calc R A 1 C17 C -0.0124(4) 0.1907(4) 0.6822(4) 0.0214(11) Uani 1 1 d . A 1 C18 C 0.0522(4) 0.2039(4) 0.7732(4) 0.0251(11) Uani 1 1 d . A 1 H18 H 0.0257 0.2103 0.8196 0.030 Uiso 1 1 calc R A 1 C19 C 0.1762(4) 0.1679(4) 0.5660(4) 0.0192(10) Uani 1 1 d . A 1 C20 C 0.2135(4) 0.2357(4) 0.5345(4) 0.0213(11) Uani 1 1 d . A 1 C21 C 0.2539(5) 0.2253(4) 0.4684(4) 0.0292(13) Uani 1 1 d . A 1 H21 H 0.2782 0.2724 0.4470 0.035 Uiso 1 1 calc R A 1 C22 C 0.2595(5) 0.1489(5) 0.4333(4) 0.0312(14) Uani 1 1 d . A 1 H22 H 0.2877 0.1436 0.3879 0.037 Uiso 1 1 calc R A 1 C23 C 0.2240(4) 0.0769(4) 0.4635(4) 0.0274(13) Uani 1 1 d . A 1 C24 C 0.2300(5) -0.0032(5) 0.4298(5) 0.0369(15) Uani 1 1 d . A 1 H24 H 0.2577 -0.0097 0.3843 0.044 Uiso 1 1 calc R A 1 C25 C 0.1970(6) -0.0720(5) 0.4611(5) 0.0388(17) Uani 1 1 d . A 1 H25 H 0.2021 -0.1254 0.4376 0.047 Uiso 1 1 calc R A 1 C26 C 0.1548(5) -0.0628(5) 0.5292(5) 0.0371(15) Uani 1 1 d . A 1 H26 H 0.1321 -0.1102 0.5516 0.045 Uiso 1 1 calc R A 1 C27 C 0.1470(5) 0.0144(4) 0.5623(5) 0.0292(13) Uani 1 1 d . A 1 H27 H 0.1172 0.0200 0.6063 0.035 Uiso 1 1 calc R A 1 C28 C 0.1829(4) 0.0871(4) 0.5319(4) 0.0227(11) Uani 1 1 d . A 1 C29 C 0.2135(5) 0.3217(4) 0.5729(4) 0.0245(12) Uani 1 1 d . A 1 C30 C 0.3012(5) 0.3623(4) 0.6154(4) 0.0271(12) Uani 1 1 d . A 1 H30 H 0.3617 0.3353 0.6221 0.033 Uiso 1 1 calc R A 1 C31 C 0.3034(6) 0.4427(4) 0.6489(5) 0.0339(14) Uani 1 1 d . A 1 H31 H 0.3649 0.4708 0.6766 0.041 Uiso 1 1 calc R A 1 C32 C 0.2161(6) 0.4818(5) 0.6421(6) 0.0393(16) Uani 1 1 d . A 1 H32 H 0.2176 0.5351 0.6684 0.047 Uiso 1 1 calc R A 1 C33 C 0.1249(5) 0.4415(5) 0.5955(5) 0.0370(15) Uani 1 1 d . A 1 H33 H 0.0643 0.4693 0.5861 0.044 Uiso 1 1 calc R A 1 C34 C 0.1242(5) 0.3623(4) 0.5641(4) 0.0295(13) Uani 1 1 d . A 1 H34 H 0.0629 0.3341 0.5360 0.035 Uiso 1 1 calc R A 1 C35 C 0.4495(3) 0.2755(3) 1.0546(3) 0.0150(10) Uani 1 1 d . A 1 H35 H 0.4254 0.3343 1.0451 0.018 Uiso 1 1 calc R A 1 C36 C 0.5179(4) 0.2679(4) 1.1549(3) 0.0203(11) Uani 1 1 d . A 1 C37 C 0.5441(7) 0.3389(5) 1.2097(6) 0.054(3) Uani 1 1 d . A 1 H37 H 0.5210 0.3920 1.1844 0.065 Uiso 1 1 calc R A 1 C38 C 0.6044(9) 0.3307(6) 1.3014(6) 0.077(4) Uani 1 1 d . A 1 H38 H 0.6249 0.3793 1.3380 0.092 Uiso 1 1 calc R A 1 C39 C 0.6357(8) 0.2538(7) 1.3412(5) 0.066(3) Uani 1 1 d . A 1 H39 H 0.6698 0.2485 1.4056 0.079 Uiso 1 1 calc R A 1 C40 C 0.6162(6) 0.1864(5) 1.2858(4) 0.0386(17) Uani 1 1 d . A 1 H40 H 0.6450 0.1343 1.3100 0.046 Uiso 1 1 calc R A 1 C41 C 0.5544(4) 0.1924(4) 1.1934(4) 0.0295(14) Uani 1 1 d . A 1 H41 H 0.5374 0.1437 1.1567 0.035 Uiso 1 1 calc R A 1 C42 C 0.5898(4) 0.2702(4) 1.0114(4) 0.0193(10) Uani 1 1 d . A 1 H42 H 0.6287 0.2755 1.0750 0.023 Uiso 1 1 calc R A 1 C43 C 0.6409(4) 0.2745(4) 0.9473(4) 0.0190(10) Uani 1 1 d . A 1 C44 C 0.5865(4) 0.2819(3) 0.8502(3) 0.0148(9) Uani 1 1 d . A 1 C45 C 0.6374(4) 0.3078(3) 0.7948(4) 0.0175(10) Uani 1 1 d . A 1 C46 C 0.7415(4) 0.3206(4) 0.8344(4) 0.0211(11) Uani 1 1 d . A 1 C47 C 0.7969(4) 0.3467(4) 0.7807(4) 0.0260(12) Uani 1 1 d . A 1 H47 H 0.7637 0.3579 0.7171 0.031 Uiso 1 1 calc R A 1 C48 C 0.8996(5) 0.3556(5) 0.8214(5) 0.0344(15) Uani 1 1 d . A 1 H48 H 0.9355 0.3719 0.7847 0.041 Uiso 1 1 calc R A 1 C49 C 0.9503(5) 0.3412(5) 0.9140(6) 0.0364(16) Uani 1 1 d . A 1 H49 H 1.0201 0.3481 0.9403 0.044 Uiso 1 1 calc R A 1 C50 C 0.9002(4) 0.3170(4) 0.9675(5) 0.0278(13) Uani 1 1 d . A 1 H50 H 0.9354 0.3073 1.0312 0.033 Uiso 1 1 calc R A 1 C51 C 0.7952(4) 0.3061(4) 0.9290(4) 0.0238(11) Uani 1 1 d . A 1 C52 C 0.7420(4) 0.2842(4) 0.9856(4) 0.0208(11) Uani 1 1 d . A 1 H52 H 0.7764 0.2763 1.0497 0.025 Uiso 1 1 calc R A 1 C53 C 0.5827(4) 0.3220(3) 0.6955(4) 0.0175(10) Uani 1 1 d . A 1 C54 C 0.5496(4) 0.2568(4) 0.6349(4) 0.0196(11) Uani 1 1 d . A 1 C55 C 0.4986(5) 0.2739(4) 0.5378(4) 0.0250(12) Uani 1 1 d . A 1 H55 H 0.4774 0.2289 0.4957 0.030 Uiso 1 1 calc R A 1 C56 C 0.4804(5) 0.3540(4) 0.5058(4) 0.0276(12) Uani 1 1 d . A 1 H56 H 0.4480 0.3643 0.4419 0.033 Uiso 1 1 calc R A 1 C57 C 0.5100(5) 0.4210(4) 0.5678(4) 0.0259(12) Uani 1 1 d . A 1 C58 C 0.4848(6) 0.5047(4) 0.5364(4) 0.0331(14) Uani 1 1 d . A 1 H58 H 0.4518 0.5159 0.4728 0.040 Uiso 1 1 calc R A 1 C59 C 0.5088(6) 0.5681(5) 0.5986(6) 0.0412(17) Uani 1 1 d . A 1 H59 H 0.4895 0.6232 0.5781 0.049 Uiso 1 1 calc R A 1 C60 C 0.5609(6) 0.5533(4) 0.6911(5) 0.0351(15) Uani 1 1 d . A 1 H60 H 0.5783 0.5985 0.7330 0.042 Uiso 1 1 calc R A 1 C61 C 0.5871(4) 0.4756(4) 0.7222(4) 0.0239(12) Uani 1 1 d . A 1 H61 H 0.6234 0.4671 0.7859 0.029 Uiso 1 1 calc R A 1 C62 C 0.5620(4) 0.4061(3) 0.6626(4) 0.0181(10) Uani 1 1 d . A 1 C63 C 0.5613(4) 0.1686(4) 0.6667(4) 0.0220(11) Uani 1 1 d . A 1 C64 C 0.4778(5) 0.1205(4) 0.6549(5) 0.0283(12) Uani 1 1 d . A 1 H64 H 0.4132 0.1435 0.6270 0.034 Uiso 1 1 calc R A 1 C65 C 0.4905(5) 0.0378(4) 0.6847(5) 0.0342(15) Uani 1 1 d . A 1 H65 H 0.4336 0.0051 0.6772 0.041 Uiso 1 1 calc R A 1 C66 C 0.5802(6) 0.0033(4) 0.7233(5) 0.0365(15) Uani 1 1 d . A 1 H66 H 0.5868 -0.0530 0.7428 0.044 Uiso 1 1 calc R A 1 C67 C 0.6660(5) 0.0519(4) 0.7351(5) 0.0339(14) Uani 1 1 d . A 1 H67 H 0.7302 0.0282 0.7621 0.041 Uiso 1 1 calc R A 1 C68 C 0.6548(5) 0.1341(4) 0.7067(5) 0.0321(14) Uani 1 1 d . A 1 H68 H 0.7117 0.1670 0.7147 0.039 Uiso 1 1 calc R A 1 C69 C 0.5147(5) 0.0564(4) 0.9495(4) 0.0317(14) Uani 1 1 d . A 1 C70 C 0.4958(5) 0.0031(4) 1.0136(5) 0.0303(14) Uani 1 1 d . A 1 C71 C 0.5705(6) -0.0397(5) 1.0794(5) 0.0365(15) Uani 1 1 d . A 1 H71 H 0.5570 -0.0750 1.1217 0.044 Uiso 1 1 calc R A 1 C72 C 0.6696(6) -0.0294(4) 1.0822(5) 0.0372(16) Uani 1 1 d . A 1 C73 C 0.7493(8) -0.0757(6) 1.1496(6) 0.055(2) Uani 1 1 d . A 1 H73 H 0.7356 -0.1110 1.1918 0.066 Uiso 1 1 calc R A 1 C74 C 0.8428(7) -0.0688(6) 1.1527(7) 0.059(3) Uani 1 1 d . A 1 H74 H 0.8949 -0.1010 1.1946 0.071 Uiso 1 1 calc R A 1 C75 C 0.8625(7) -0.0094(8) 1.0885(9) 0.069(3) Uani 1 1 d . A 1 H75 H 0.9285 0.0001 1.0927 0.083 Uiso 1 1 calc R A 1 C76 C 0.7852(6) 0.0312(6) 1.0239(7) 0.052(2) Uani 1 1 d . A 1 H76 H 0.7980 0.0665 0.9812 0.062 Uiso 1 1 calc R A 1 C77 C 0.6874(6) 0.0220(5) 1.0190(5) 0.0402(17) Uani 1 1 d . A 1 C78 C 0.6046(6) 0.0660(4) 0.9495(5) 0.0357(15) Uani 1 1 d . A 1 H78 H 0.6157 0.1008 0.9054 0.043 Uiso 1 1 calc R A 1 C1S C 0.8750(14) 0.1865(13) 0.2486(12) 0.111(6) Uani 1 1 d . B 1 C2S C 0.9757(15) 0.1346(16) 0.2755(17) 0.127(7) Uani 1 1 d . B 1 O1S O 0.8747(19) 0.2616(11) 0.2048(9) 0.235(13) Uani 1 1 d . B 1 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 0.0140(3) 0.0227(4) 0.0122(3) -0.0021(3) 0.0065(2) -0.0027(3) N1 0.0158(19) 0.028(3) 0.0124(18) -0.0028(17) 0.0065(15) -0.0072(18) N2 0.020(2) 0.022(2) 0.0131(19) -0.0041(17) 0.0081(16) -0.0025(18) O1 0.0142(16) 0.034(2) 0.0107(14) -0.0045(16) 0.0042(12) -0.0058(17) O2 0.0143(16) 0.026(2) 0.0168(17) -0.0014(15) 0.0065(14) -0.0051(15) O3 0.033(2) 0.024(2) 0.027(2) -0.0003(17) 0.0076(18) 0.0017(18) Br1 0.0416(4) 0.0348(4) 0.0541(4) 0.0053(3) 0.0243(3) -0.0025(3) C1 0.019(2) 0.029(3) 0.011(2) -0.001(2) 0.0056(18) -0.001(2) C2 0.017(2) 0.042(3) 0.015(2) -0.002(2) 0.009(2) -0.005(2) C3 0.026(3) 0.055(5) 0.028(3) -0.016(3) 0.013(3) 0.006(3) C4 0.024(3) 0.063(5) 0.040(4) -0.020(4) 0.012(3) -0.003(3) C5 0.030(4) 0.157(12) 0.031(4) -0.015(5) 0.019(3) -0.015(6) C6 0.045(4) 0.076(6) 0.038(4) 0.002(4) 0.031(3) -0.002(4) C7 0.030(3) 0.062(5) 0.028(3) 0.010(3) 0.014(3) -0.002(3) C8 0.018(2) 0.030(3) 0.013(2) -0.005(2) 0.0066(18) -0.006(2) C9 0.017(2) 0.029(3) 0.016(2) -0.007(2) 0.0069(18) -0.004(2) C10 0.018(2) 0.020(3) 0.017(2) -0.003(2) 0.0079(18) -0.004(2) C11 0.012(2) 0.022(2) 0.016(2) -0.0050(19) 0.0034(18) 0.0010(19) C12 0.012(2) 0.025(3) 0.021(2) -0.001(2) 0.0067(19) 0.0034(19) C13 0.022(3) 0.031(3) 0.022(3) -0.005(2) 0.005(2) 0.002(2) C14 0.022(3) 0.048(4) 0.021(3) -0.009(3) 0.000(2) 0.004(3) C15 0.018(3) 0.043(4) 0.036(3) -0.006(3) 0.007(2) 0.001(3) C16 0.021(3) 0.044(4) 0.019(2) -0.005(2) 0.009(2) -0.002(2) C17 0.017(2) 0.031(3) 0.017(2) -0.005(2) 0.0069(19) 0.000(2) C18 0.020(2) 0.036(3) 0.021(2) -0.007(3) 0.008(2) -0.001(3) C19 0.013(2) 0.025(3) 0.019(2) -0.004(2) 0.0044(19) 0.003(2) C20 0.018(2) 0.027(3) 0.017(2) 0.001(2) 0.005(2) 0.000(2) C21 0.027(3) 0.043(4) 0.019(2) 0.005(2) 0.010(2) 0.002(3) C22 0.028(3) 0.045(4) 0.021(3) -0.002(3) 0.010(2) 0.006(3) C23 0.020(3) 0.039(4) 0.023(3) -0.005(2) 0.007(2) 0.002(2) C24 0.036(3) 0.045(4) 0.034(3) -0.018(3) 0.018(3) 0.001(3) C25 0.043(4) 0.042(4) 0.027(3) -0.014(3) 0.008(3) 0.011(3) C26 0.031(3) 0.034(4) 0.044(4) -0.015(3) 0.012(3) -0.005(3) C27 0.027(3) 0.028(3) 0.035(3) -0.005(3) 0.015(3) -0.002(2) C28 0.022(3) 0.024(3) 0.020(3) -0.010(2) 0.006(2) -0.002(2) C29 0.029(3) 0.025(3) 0.021(3) 0.005(2) 0.011(2) 0.006(2) C30 0.035(3) 0.033(3) 0.016(3) 0.004(2) 0.012(2) 0.008(3) C31 0.040(4) 0.026(3) 0.037(3) 0.000(3) 0.016(3) -0.008(3) C32 0.043(4) 0.021(3) 0.056(4) -0.005(3) 0.020(3) 0.005(3) C33 0.033(3) 0.038(4) 0.038(4) 0.009(3) 0.010(3) 0.011(3) C34 0.028(3) 0.032(3) 0.028(3) 0.006(3) 0.009(2) 0.007(2) C35 0.009(2) 0.024(3) 0.008(2) -0.0028(18) -0.0004(17) 0.0019(19) C36 0.017(2) 0.033(3) 0.006(2) -0.004(2) -0.0005(18) 0.004(2) C37 0.057(5) 0.040(4) 0.039(4) -0.019(3) -0.011(4) 0.032(4) C38 0.101(8) 0.046(5) 0.041(5) -0.025(4) -0.023(5) 0.040(5) C39 0.063(6) 0.077(7) 0.026(4) -0.006(4) -0.020(4) 0.046(5) C40 0.044(4) 0.040(4) 0.021(3) 0.007(3) 0.000(3) 0.007(3) C41 0.024(3) 0.034(4) 0.022(3) 0.005(2) -0.001(2) -0.003(2) C42 0.018(2) 0.022(3) 0.019(2) -0.001(2) 0.008(2) 0.001(2) C43 0.014(2) 0.026(3) 0.018(2) -0.001(2) 0.0067(19) 0.000(2) C44 0.016(2) 0.015(2) 0.016(2) -0.0026(18) 0.0083(18) -0.0017(18) C45 0.020(2) 0.015(2) 0.023(3) -0.0056(19) 0.014(2) -0.0021(19) C46 0.017(2) 0.018(3) 0.028(3) -0.007(2) 0.010(2) -0.002(2) C47 0.019(3) 0.029(3) 0.030(3) -0.004(2) 0.009(2) -0.001(2) C48 0.028(3) 0.038(4) 0.047(4) -0.003(3) 0.026(3) -0.005(3) C49 0.021(3) 0.033(4) 0.056(4) -0.002(3) 0.016(3) -0.007(3) C50 0.015(3) 0.033(3) 0.036(3) -0.001(3) 0.010(2) -0.002(2) C51 0.019(3) 0.030(3) 0.024(3) -0.002(2) 0.010(2) 0.003(2) C52 0.015(2) 0.032(3) 0.017(2) -0.004(2) 0.0090(19) 0.000(2) C53 0.017(2) 0.017(2) 0.024(3) -0.001(2) 0.013(2) 0.0003(19) C54 0.022(3) 0.025(3) 0.015(2) -0.006(2) 0.011(2) -0.003(2) C55 0.032(3) 0.025(3) 0.022(3) -0.005(2) 0.014(2) -0.001(2) C56 0.034(3) 0.032(3) 0.020(3) -0.003(2) 0.014(2) -0.004(3) C57 0.026(3) 0.025(3) 0.030(3) 0.006(2) 0.013(2) -0.005(2) C58 0.049(4) 0.033(4) 0.021(3) 0.012(2) 0.016(3) -0.001(3) C59 0.049(4) 0.027(3) 0.049(4) 0.012(3) 0.020(3) -0.008(3) C60 0.045(4) 0.023(3) 0.036(3) -0.005(3) 0.014(3) -0.013(3) C61 0.026(3) 0.029(3) 0.020(2) 0.001(2) 0.012(2) -0.005(2) C62 0.021(2) 0.017(2) 0.020(3) 0.005(2) 0.013(2) -0.004(2) C63 0.027(3) 0.023(3) 0.020(3) -0.006(2) 0.013(2) -0.006(2) C64 0.021(3) 0.027(3) 0.038(3) 0.003(3) 0.013(2) 0.002(2) C65 0.040(4) 0.026(3) 0.042(4) 0.000(3) 0.022(3) -0.018(3) C66 0.055(4) 0.026(3) 0.038(4) 0.003(3) 0.029(3) -0.003(3) C67 0.027(3) 0.025(3) 0.050(4) 0.001(3) 0.016(3) 0.004(3) C68 0.026(3) 0.028(3) 0.049(4) -0.009(3) 0.021(3) -0.002(2) C69 0.044(4) 0.018(3) 0.023(3) -0.003(2) 0.001(3) 0.009(3) C70 0.033(3) 0.034(4) 0.037(3) -0.001(3) 0.027(3) 0.000(3) C71 0.048(4) 0.031(3) 0.033(3) -0.002(3) 0.018(3) 0.006(3) C72 0.042(4) 0.032(4) 0.030(3) -0.005(3) 0.005(3) 0.006(3) C73 0.063(6) 0.044(5) 0.046(4) -0.006(4) 0.008(4) 0.028(4) C74 0.050(5) 0.047(5) 0.058(5) -0.015(4) -0.006(4) 0.017(4) C75 0.032(4) 0.055(5) 0.104(8) -0.016(6) 0.007(4) 0.002(4) C76 0.037(4) 0.047(5) 0.071(6) -0.006(4) 0.020(4) 0.005(4) C77 0.036(4) 0.039(4) 0.044(4) -0.013(3) 0.012(3) 0.010(3) C78 0.043(4) 0.026(3) 0.039(4) -0.001(3) 0.016(3) 0.012(3) C1S 0.107(12) 0.127(15) 0.118(12) 0.047(11) 0.065(10) 0.022(10) C2S 0.089(11) 0.145(18) 0.156(17) 0.006(14) 0.057(12) 0.003(11) O1S 0.36(3) 0.125(12) 0.082(8) 0.041(8) -0.072(12) -0.056(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O3 1.864(5) . ? Fe1 O1 1.889(3) . ? Fe1 O2 1.900(4) . ? Fe1 N1 2.120(4) . ? Fe1 N2 2.123(4) . ? N1 C8 1.284(7) . ? N1 C1 1.490(6) . ? N2 C42 1.290(7) . ? N2 C35 1.463(7) . ? O1 C10 1.301(6) . ? O2 C44 1.319(6) . ? O3 C69 1.339(8) . ? Br1 C70 1.903(6) . ? C1 C2 1.515(8) . ? C1 C35 1.528(7) . ? C1 H1 1.0000 . ? C2 C3 1.384(11) . ? C2 C7 1.405(10) . ? C3 C4 1.380(10) . ? C3 H3 0.9500 . ? C4 C5 1.438(16) . ? C4 H4 0.9500 . ? C5 C6 1.338(18) . ? C5 H5 0.9500 . ? C6 C7 1.379(11) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.443(7) . ? C8 H8 0.9500 . ? C9 C18 1.387(7) . ? C9 C10 1.447(7) . ? C10 C11 1.407(7) . ? C11 C12 1.428(7) . ? C11 C19 1.492(7) . ? C12 C13 1.418(8) . ? C12 C17 1.423(8) . ? C13 C14 1.361(9) . ? C13 H13 0.9500 . ? C14 C15 1.411(10) . ? C14 H14 0.9500 . ? C15 C16 1.363(9) . ? C15 H15 0.9500 . ? C16 C17 1.419(8) . ? C16 H16 0.9500 . ? C17 C18 1.401(7) . ? C18 H18 0.9500 . ? C19 C20 1.389(8) . ? C19 C28 1.423(8) . ? C20 C21 1.383(8) . ? C20 C29 1.510(8) . ? C21 C22 1.363(10) . ? C21 H21 0.9500 . ? C22 C23 1.420(10) . ? C22 H22 0.9500 . ? C23 C24 1.408(10) . ? C23 C28 1.422(8) . ? C24 C25 1.369(12) . ? C24 H24 0.9500 . ? C25 C26 1.428(11) . ? C25 H25 0.9500 . ? C26 C27 1.367(10) . ? C26 H26 0.9500 . ? C27 C28 1.434(9) . ? C27 H27 0.9500 . ? C29 C30 1.364(10) . ? C29 C34 1.415(9) . ? C30 C31 1.393(9) . ? C30 H30 0.9500 . ? C31 C32 1.385(10) . ? C31 H31 0.9500 . ? C32 C33 1.410(11) . ? C32 H32 0.9500 . ? C33 C34 1.364(10) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.521(6) . ? C35 H35 1.0000 . ? C36 C41 1.372(9) . ? C36 C37 1.394(9) . ? C37 C38 1.384(11) . ? C37 H37 0.9500 . ? C38 C39 1.385(14) . ? C38 H38 0.9500 . ? C39 C40 1.353(12) . ? C39 H39 0.9500 . ? C40 C41 1.396(8) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.462(8) . ? C42 H42 0.9500 . ? C43 C52 1.374(7) . ? C43 C44 1.436(7) . ? C44 C45 1.402(7) . ? C45 C46 1.421(7) . ? C45 C53 1.480(8) . ? C46 C51 1.416(8) . ? C46 C47 1.431(9) . ? C47 C48 1.395(9) . ? C47 H47 0.9500 . ? C48 C49 1.382(11) . ? C48 H48 0.9500 . ? C49 C50 1.360(10) . ? C49 H49 0.9500 . ? C50 C51 1.427(8) . ? C50 H50 0.9500 . ? C51 C52 1.425(8) . ? C52 H52 0.9500 . ? C53 C54 1.377(8) . ? C53 C62 1.440(7) . ? C54 C55 1.451(8) . ? C54 C63 1.493(8) . ? C55 C56 1.373(9) . ? C55 H55 0.9500 . ? C56 C57 1.407(9) . ? C56 H56 0.9500 . ? C57 C62 1.416(8) . ? C57 C58 1.434(9) . ? C58 C59 1.365(11) . ? C58 H58 0.9500 . ? C59 C60 1.386(11) . ? C59 H59 0.9500 . ? C60 C61 1.344(10) . ? C60 H60 0.9500 . ? C61 C62 1.416(8) . ? C61 H61 0.9500 . ? C63 C68 1.382(9) . ? C63 C64 1.393(8) . ? C64 C65 1.401(9) . ? C64 H64 0.9500 . ? C65 C66 1.337(11) . ? C65 H65 0.9500 . ? C66 C67 1.425(10) . ? C66 H66 0.9500 . ? C67 C68 1.386(10) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C78 1.317(11) . ? C69 C70 1.427(10) . ? C70 C71 1.372(10) . ? C71 C72 1.436(12) . ? C71 H71 0.9500 . ? C72 C77 1.390(12) . ? C72 C73 1.448(11) . ? C73 C74 1.347(16) . ? C73 H73 0.9500 . ? C74 C75 1.492(18) . ? C74 H74 0.9500 . ? C75 C76 1.366(14) . ? C75 H75 0.9500 . ? C76 C77 1.404(12) . ? C76 H76 0.9500 . ? C77 C78 1.469(10) . ? C78 H78 0.9500 . ? C1S O1S 1.39(2) . ? C1S C2S 1.60(3) . ? 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 O3 Fe1 O1 102.4(2) . . ? O3 Fe1 O2 116.1(2) . . ? O1 Fe1 O2 98.25(16) . . ? O3 Fe1 N1 96.8(2) . . ? O1 Fe1 N1 87.34(16) . . ? O2 Fe1 N1 144.26(19) . . ? O3 Fe1 N2 98.47(19) . . ? O1 Fe1 N2 154.67(19) . . ? O2 Fe1 N2 85.17(17) . . ? N1 Fe1 N2 75.99(17) . . ? C8 N1 C1 119.4(4) . . ? C8 N1 Fe1 126.1(3) . . ? C1 N1 Fe1 113.9(3) . . ? C42 N2 C35 119.7(4) . . ? C42 N2 Fe1 122.1(4) . . ? C35 N2 Fe1 117.9(3) . . ? C10 O1 Fe1 135.8(3) . . ? C44 O2 Fe1 131.1(3) . . ? C69 O3 Fe1 133.5(4) . . ? N1 C1 C2 115.1(4) . . ? N1 C1 C35 106.4(4) . . ? C2 C1 C35 113.6(5) . . ? N1 C1 H1 107.1 . . ? C2 C1 H1 107.1 . . ? C35 C1 H1 107.1 . . ? C3 C2 C7 119.4(6) . . ? C3 C2 C1 122.3(6) . . ? C7 C2 C1 118.2(6) . . ? C4 C3 C2 120.2(8) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 118.9(9) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 120.4(8) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.6(9) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C2 120.4(8) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? N1 C8 C9 126.0(5) . . ? N1 C8 H8 117.0 . . ? C9 C8 H8 117.0 . . ? C18 C9 C8 116.1(5) . . ? C18 C9 C10 121.2(5) . . ? C8 C9 C10 122.6(5) . . ? O1 C10 C11 120.4(5) . . ? O1 C10 C9 121.9(4) . . ? C11 C10 C9 117.7(5) . . ? C10 C11 C12 120.5(5) . . ? C10 C11 C19 119.2(5) . . ? C12 C11 C19 120.3(4) . . ? C13 C12 C17 117.7(5) . . ? C13 C12 C11 121.7(5) . . ? C17 C12 C11 120.6(5) . . ? C14 C13 C12 120.6(6) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 121.8(6) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C16 C15 C14 119.2(6) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 120.5(6) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 121.3(5) . . ? C18 C17 C12 118.5(5) . . ? C16 C17 C12 120.1(5) . . ? C9 C18 C17 121.4(5) . . ? C9 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C20 C19 C28 119.4(5) . . ? C20 C19 C11 119.8(5) . . ? C28 C19 C11 120.7(5) . . ? C21 C20 C19 120.4(6) . . ? C21 C20 C29 118.3(6) . . ? C19 C20 C29 121.3(5) . . ? C22 C21 C20 121.4(6) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 121.0(6) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 122.6(6) . . ? C24 C23 C28 119.5(6) . . ? C22 C23 C28 117.9(6) . . ? C25 C24 C23 121.7(6) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 C26 119.6(7) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 119.9(7) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 121.5(6) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C23 C28 C19 119.9(6) . . ? C23 C28 C27 117.8(5) . . ? C19 C28 C27 122.3(5) . . ? C30 C29 C34 118.9(6) . . ? C30 C29 C20 119.6(6) . . ? C34 C29 C20 121.4(6) . . ? C29 C30 C31 120.9(6) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 120.2(7) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 119.2(7) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 119.7(7) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C29 120.9(6) . . ? C33 C34 H34 119.5 . . ? C29 C34 H34 119.5 . . ? N2 C35 C36 115.5(4) . . ? N2 C35 C1 108.9(4) . . ? C36 C35 C1 111.9(5) . . ? N2 C35 H35 106.7 . . ? C36 C35 H35 106.7 . . ? C1 C35 H35 106.7 . . ? C41 C36 C37 118.8(5) . . ? C41 C36 C35 121.5(5) . . ? C37 C36 C35 119.7(6) . . ? C38 C37 C36 119.1(7) . . ? C38 C37 H37 120.5 . . ? C36 C37 H37 120.5 . . ? C37 C38 C39 121.8(8) . . ? C37 C38 H38 119.1 . . ? C39 C38 H38 119.1 . . ? C40 C39 C38 118.2(7) . . ? C40 C39 H39 120.9 . . ? C38 C39 H39 120.9 . . ? C39 C40 C41 120.7(7) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C36 C41 C40 120.8(6) . . ? C36 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? N2 C42 C43 124.8(5) . . ? N2 C42 H42 117.6 . . ? C43 C42 H42 117.6 . . ? C52 C43 C44 122.0(5) . . ? C52 C43 C42 116.2(5) . . ? C44 C43 C42 121.0(5) . . ? O2 C44 C45 119.9(5) . . ? O2 C44 C43 121.7(5) . . ? C45 C44 C43 118.4(5) . . ? C44 C45 C46 119.7(5) . . ? C44 C45 C53 120.1(5) . . ? C46 C45 C53 120.2(5) . . ? C51 C46 C45 121.0(5) . . ? C51 C46 C47 117.1(5) . . ? C45 C46 C47 121.9(5) . . ? C48 C47 C46 120.2(6) . . ? C48 C47 H47 119.9 . . ? C46 C47 H47 119.9 . . ? C49 C48 C47 121.5(6) . . ? C49 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? C50 C49 C48 120.1(6) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 120.6(6) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? C46 C51 C52 118.7(5) . . ? C46 C51 C50 120.5(6) . . ? C52 C51 C50 120.7(5) . . ? C43 C52 C51 119.9(5) . . ? C43 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C54 C53 C62 119.7(5) . . ? C54 C53 C45 121.5(5) . . ? C62 C53 C45 118.8(5) . . ? C53 C54 C55 119.4(5) . . ? C53 C54 C63 121.7(5) . . ? C55 C54 C63 118.8(5) . . ? C56 C55 C54 121.1(5) . . ? C56 C55 H55 119.5 . . ? C54 C55 H55 119.5 . . ? C55 C56 C57 119.9(6) . . ? C55 C56 H56 120.1 . . ? C57 C56 H56 120.1 . . ? C56 C57 C62 120.2(6) . . ? C56 C57 C58 120.5(6) . . ? C62 C57 C58 119.2(6) . . ? C59 C58 C57 119.4(6) . . ? C59 C58 H58 120.3 . . ? C57 C58 H58 120.3 . . ? C58 C59 C60 121.0(7) . . ? C58 C59 H59 119.5 . . ? C60 C59 H59 119.5 . . ? C61 C60 C59 120.7(7) . . ? C61 C60 H60 119.6 . . ? C59 C60 H60 119.6 . . ? C60 C61 C62 121.7(6) . . ? C60 C61 H61 119.1 . . ? C62 C61 H61 119.1 . . ? C57 C62 C61 117.8(5) . . ? C57 C62 C53 119.6(5) . . ? C61 C62 C53 122.5(5) . . ? C68 C63 C64 119.9(6) . . ? C68 C63 C54 120.2(5) . . ? C64 C63 C54 119.9(5) . . ? C63 C64 C65 118.9(6) . . ? C63 C64 H64 120.5 . . ? C65 C64 H64 120.5 . . ? C66 C65 C64 122.0(6) . . ? C66 C65 H65 119.0 . . ? C64 C65 H65 119.0 . . ? C65 C66 C67 119.3(6) . . ? C65 C66 H66 120.3 . . ? C67 C66 H66 120.3 . . ? C68 C67 C66 119.4(6) . . ? C68 C67 H67 120.3 . . ? C66 C67 H67 120.3 . . ? C63 C68 C67 120.4(6) . . ? C63 C68 H68 119.8 . . ? C67 C68 H68 119.8 . . ? C78 C69 O3 121.5(7) . . ? C78 C69 C70 121.7(6) . . ? O3 C69 C70 116.8(7) . . ? C71 C70 C69 121.7(6) . . ? C71 C70 Br1 117.9(5) . . ? C69 C70 Br1 120.3(5) . . ? C70 C71 C72 118.0(7) . . ? C70 C71 H71 121.0 . . ? C72 C71 H71 121.0 . . ? C77 C72 C71 120.0(6) . . ? C77 C72 C73 121.0(8) . . ? C71 C72 C73 119.0(8) . . ? C74 C73 C72 120.4(10) . . ? C74 C73 H73 119.8 . . ? C72 C73 H73 119.8 . . ? C73 C74 C75 118.4(8) . . ? C73 C74 H74 120.8 . . ? C75 C74 H74 120.8 . . ? C76 C75 C74 119.7(9) . . ? C76 C75 H75 120.2 . . ? C74 C75 H75 120.2 . . ? C75 C76 C77 121.7(10) . . ? C75 C76 H76 119.1 . . ? C77 C76 H76 119.1 . . ? C72 C77 C76 118.6(8) . . ? C72 C77 C78 119.9(7) . . ? C76 C77 C78 121.5(8) . . ? C69 C78 C77 118.8(7) . . ? C69 C78 H78 120.6 . . ? C77 C78 H78 120.6 . . ? O1S C1S C2S 114.7(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 6.416 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.198 # Attachment ')]_KM137_2_final.cif' data_salenFe_O_Fesalen_KM137 _database_code_depnum_ccdc_archive 'CCDC 854406' #TrackingRef ')]_KM137_2_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C136 H92 Fe2 N4 O5' _chemical_formula_sum 'C136 H92 Fe2 N4 O5' _chemical_formula_weight 1973.84 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 18.3252(10) _cell_length_b 18.3252(10) _cell_length_c 37.083(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12452.8(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9890 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.34 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 0.284 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9454 _exptl_absorpt_correction_T_max 0.9586 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 'focusing mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 71059 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.51 _reflns_number_total 14313 _reflns_number_gt 12067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1565P)^2^+13.6384P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 14313 _refine_ls_number_parameters 663 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.2530 _refine_ls_wR_factor_gt 0.2318 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.34964(3) 0.46376(3) 0.022513(14) 0.01776(15) Uani 1 1 d . . . N1 N 0.3797(2) 0.5128(2) 0.07364(9) 0.0237(7) Uani 1 1 d . . . N2 N 0.3498(2) 0.37676(18) 0.05939(8) 0.0196(7) Uani 1 1 d . . . O1 O 0.33783(18) 0.56214(16) 0.00587(8) 0.0242(6) Uani 1 1 d . . . O2 O 0.25889(16) 0.42593(17) 0.00516(7) 0.0217(6) Uani 1 1 d . . . O3 O 0.43019(16) 0.43019(16) 0.0000 0.0200(8) Uani 1 2 d S . . C1 C 0.3832(3) 0.4614(3) 0.10457(11) 0.0260(9) Uani 1 1 d . . . H1 H 0.3320 0.4541 0.1132 0.031 Uiso 1 1 calc R . . C2 C 0.4272(3) 0.4864(3) 0.13670(12) 0.0350(11) Uani 1 1 d . . . C3 C 0.5015(4) 0.4881(4) 0.13648(17) 0.0525(16) Uani 1 1 d . . . H3 H 0.5273 0.4731 0.1155 0.063 Uiso 1 1 calc R . . C4 C 0.5398(4) 0.5118(4) 0.16670(19) 0.0636(19) Uani 1 1 d . . . H4 H 0.5916 0.5130 0.1660 0.076 Uiso 1 1 calc R . . C5 C 0.5043(5) 0.5332(4) 0.19736(15) 0.0604(19) Uani 1 1 d . . . H5 H 0.5308 0.5487 0.2180 0.073 Uiso 1 1 calc R . . C6 C 0.4283(5) 0.5319(5) 0.19771(15) 0.069(2) Uani 1 1 d . . . H6 H 0.4025 0.5472 0.2186 0.083 Uiso 1 1 calc R . . C7 C 0.3906(4) 0.5084(4) 0.16768(13) 0.0493(15) Uani 1 1 d . . . H7 H 0.3388 0.5073 0.1682 0.059 Uiso 1 1 calc R . . C8 C 0.3950(3) 0.5800(3) 0.07864(12) 0.0320(10) Uani 1 1 d . . . H8 H 0.4090 0.5940 0.1023 0.038 Uiso 1 1 calc R . . C9 C 0.3931(3) 0.6375(3) 0.05134(12) 0.0322(10) Uani 1 1 d . . . C10 C 0.3652(3) 0.6255(2) 0.01552(11) 0.0253(9) Uani 1 1 d . . . C11 C 0.3661(3) 0.6844(2) -0.00847(13) 0.0289(10) Uani 1 1 d . . . C12 C 0.3943(3) 0.7536(3) 0.00110(14) 0.0314(10) Uani 1 1 d . . . C13 C 0.3956(3) 0.8138(3) -0.02271(16) 0.0406(12) Uani 1 1 d . . . H13 H 0.3776 0.8080 -0.0466 0.049 Uiso 1 1 calc R . . C14 C 0.4218(4) 0.8796(3) -0.01224(17) 0.0503(16) Uani 1 1 d . . . H14 H 0.4228 0.9189 -0.0290 0.060 Uiso 1 1 calc R . . C15 C 0.4475(5) 0.8905(3) 0.0227(2) 0.072(2) Uani 1 1 d . . . H15 H 0.4651 0.9371 0.0298 0.086 Uiso 1 1 calc R . . C16 C 0.4474(5) 0.8349(3) 0.0465(2) 0.069(2) Uani 1 1 d . . . H16 H 0.4666 0.8427 0.0700 0.083 Uiso 1 1 calc R . . C17 C 0.4191(4) 0.7646(3) 0.03745(16) 0.0501(16) Uani 1 1 d . . . C18 C 0.4174(4) 0.7054(3) 0.06097(14) 0.0459(14) Uani 1 1 d . . . H18 H 0.4340 0.7125 0.0850 0.055 Uiso 1 1 calc R . . C19 C 0.3368(3) 0.6741(3) -0.04589(15) 0.0422(14) Uani 1 1 d . . . C20 C 0.3830(5) 0.6546(3) -0.07398(15) 0.065(2) Uani 1 1 d . . . C21 C 0.3573(8) 0.6479(4) -0.1093(2) 0.089(4) Uani 1 1 d . . . H21 H 0.3905 0.6351 -0.1279 0.107 Uiso 1 1 calc R . . C22 C 0.2918(6) 0.6582(4) -0.1171(3) 0.076(2) Uani 1 1 d . . . H22 H 0.2774 0.6516 -0.1415 0.091 Uiso 1 1 calc R . . C23 C 0.2384(5) 0.6788(4) -0.0923(3) 0.088(4) Uani 1 1 d . . . C24 C 0.1669(6) 0.6899(5) -0.0995(3) 0.083(3) Uani 1 1 d . . . H24 H 0.1482 0.6817 -0.1231 0.099 Uiso 1 1 calc R . . C25 C 0.1235(4) 0.7123(3) -0.0735(2) 0.0551(18) Uani 1 1 d . . . H25 H 0.0742 0.7203 -0.0805 0.066 Uiso 1 1 calc R . . C26 C 0.1380(7) 0.7259(5) -0.0378(3) 0.107(4) Uani 1 1 d . . . H26 H 0.1018 0.7424 -0.0213 0.128 Uiso 1 1 calc R . . C27 C 0.2169(4) 0.7125(4) -0.0267(3) 0.087(3) Uani 1 1 d . . . H27 H 0.2329 0.7202 -0.0027 0.105 Uiso 1 1 calc R . . C28 C 0.2630(4) 0.6893(3) -0.0528(2) 0.066(2) Uani 1 1 d . . . C29 C 0.4614(5) 0.6403(3) -0.0694(2) 0.066(2) Uani 1 1 d . . . C30 C 0.4852(5) 0.5849(3) -0.04733(18) 0.063(2) Uani 1 1 d . . . H30 H 0.4506 0.5585 -0.0334 0.076 Uiso 1 1 calc R . . C31 C 0.5583(6) 0.5670(4) -0.0449(3) 0.092(3) Uani 1 1 d . . . H31 H 0.5740 0.5301 -0.0287 0.111 Uiso 1 1 calc R . . C32 C 0.6095(8) 0.6041(7) -0.0669(4) 0.148(7) Uani 1 1 d . . . H32 H 0.6588 0.5880 -0.0674 0.177 Uiso 1 1 calc R . . C33 C 0.5897(8) 0.6606(8) -0.0865(5) 0.150(7) Uani 1 1 d . . . H33 H 0.6254 0.6897 -0.0983 0.179 Uiso 1 1 calc R . . C34 C 0.5151(8) 0.6773(5) -0.0897(3) 0.115(5) Uani 1 1 d . . . H34 H 0.5004 0.7145 -0.1060 0.137 Uiso 1 1 calc R . . C35 C 0.4078(2) 0.3878(2) 0.08696(10) 0.0234(9) Uani 1 1 d . . . H35 H 0.4544 0.3975 0.0738 0.028 Uiso 1 1 calc R . . C36 C 0.4215(2) 0.3253(2) 0.11214(11) 0.0236(9) Uani 1 1 d . . . C37 C 0.4743(2) 0.2740(3) 0.10295(12) 0.0261(9) Uani 1 1 d . . . H37 H 0.5002 0.2788 0.0809 0.031 Uiso 1 1 calc R . . C38 C 0.4894(3) 0.2157(3) 0.12583(14) 0.0327(10) Uani 1 1 d . . . H38 H 0.5260 0.1814 0.1195 0.039 Uiso 1 1 calc R . . C39 C 0.4514(3) 0.2075(3) 0.15776(14) 0.0358(11) Uani 1 1 d . . . H39 H 0.4619 0.1677 0.1733 0.043 Uiso 1 1 calc R . . C40 C 0.3983(3) 0.2573(3) 0.16687(12) 0.0329(11) Uani 1 1 d . . . H40 H 0.3721 0.2518 0.1888 0.039 Uiso 1 1 calc R . . C41 C 0.3828(3) 0.3160(3) 0.14388(12) 0.0297(10) Uani 1 1 d . . . H41 H 0.3454 0.3496 0.1501 0.036 Uiso 1 1 calc R . . C42 C 0.3093(2) 0.3203(2) 0.05894(11) 0.0203(8) Uani 1 1 d . . . H42 H 0.3227 0.2805 0.0739 0.024 Uiso 1 1 calc R . . C43 C 0.2446(2) 0.3125(2) 0.03736(10) 0.0207(8) Uani 1 1 d . . . C44 C 0.2185(2) 0.3684(2) 0.01285(10) 0.0164(7) Uani 1 1 d . . . C45 C 0.1484(2) 0.3612(2) -0.00198(10) 0.0203(8) Uani 1 1 d . . . C46 C 0.1054(2) 0.2983(2) 0.00565(10) 0.0213(8) Uani 1 1 d . . . C47 C 0.0322(2) 0.2897(3) -0.00692(12) 0.0271(9) Uani 1 1 d . . . H47 H 0.0106 0.3273 -0.0210 0.033 Uiso 1 1 calc R . . C48 C -0.0076(3) 0.2284(3) 0.00082(13) 0.0302(10) Uani 1 1 d . . . H48 H -0.0562 0.2246 -0.0079 0.036 Uiso 1 1 calc R . . C49 C 0.0221(3) 0.1706(3) 0.02152(13) 0.0324(10) Uani 1 1 d . . . H49 H -0.0056 0.1278 0.0262 0.039 Uiso 1 1 calc R . . C50 C 0.0914(3) 0.1779(3) 0.03468(12) 0.0275(9) Uani 1 1 d . . . H50 H 0.1115 0.1396 0.0489 0.033 Uiso 1 1 calc R . . C51 C 0.1340(2) 0.2408(2) 0.02773(11) 0.0229(8) Uani 1 1 d . . . C52 C 0.2023(2) 0.2508(2) 0.04301(11) 0.0222(8) Uani 1 1 d . . . H52 H 0.2211 0.2134 0.0581 0.027 Uiso 1 1 calc R . . C53 C 0.1162(2) 0.4230(2) -0.02292(11) 0.0208(8) Uani 1 1 d . . . C54 C 0.1046(2) 0.4900(2) -0.00608(11) 0.0226(8) Uani 1 1 d . . . C55 C 0.0697(2) 0.5467(2) -0.02585(12) 0.0266(9) Uani 1 1 d . . . H55 H 0.0644 0.5932 -0.0149 0.032 Uiso 1 1 calc R . . C56 C 0.0439(2) 0.5369(2) -0.05972(12) 0.0261(9) Uani 1 1 d . . . H56 H 0.0192 0.5756 -0.0716 0.031 Uiso 1 1 calc R . . C57 C 0.0536(2) 0.4689(3) -0.07754(11) 0.0253(9) Uani 1 1 d . . . C58 C 0.0246(3) 0.4551(3) -0.11262(12) 0.0313(10) Uani 1 1 d . . . H58 H -0.0058 0.4903 -0.1239 0.038 Uiso 1 1 calc R . . C59 C 0.0405(3) 0.3915(3) -0.12985(13) 0.0378(11) Uani 1 1 d . . . H59 H 0.0215 0.3829 -0.1533 0.045 Uiso 1 1 calc R . . C60 C 0.0850(3) 0.3379(3) -0.11323(13) 0.0376(12) Uani 1 1 d . . . H60 H 0.0976 0.2947 -0.1260 0.045 Uiso 1 1 calc R . . C61 C 0.1096(3) 0.3481(3) -0.07922(12) 0.0314(10) Uani 1 1 d . . . H61 H 0.1383 0.3111 -0.0682 0.038 Uiso 1 1 calc R . . C62 C 0.0937(2) 0.4129(2) -0.05947(11) 0.0233(8) Uani 1 1 d . . . C63 C 0.1267(2) 0.5034(2) 0.03155(12) 0.0240(9) Uani 1 1 d . . . C64 C 0.1725(3) 0.5630(3) 0.03928(13) 0.0292(10) Uani 1 1 d . . . H64 H 0.1883 0.5941 0.0203 0.035 Uiso 1 1 calc R . . C65 C 0.1950(3) 0.5767(3) 0.07452(15) 0.0407(12) Uani 1 1 d . . . H65 H 0.2262 0.6168 0.0795 0.049 Uiso 1 1 calc R . . C66 C 0.1718(3) 0.5318(4) 0.10219(14) 0.0439(13) Uani 1 1 d . . . H66 H 0.1879 0.5405 0.1262 0.053 Uiso 1 1 calc R . . C67 C 0.1247(3) 0.4735(3) 0.09489(13) 0.0377(12) Uani 1 1 d . . . H67 H 0.1077 0.4433 0.1140 0.045 Uiso 1 1 calc R . . C68 C 0.1030(3) 0.4601(3) 0.05977(12) 0.0295(9) Uani 1 1 d . . . H68 H 0.0711 0.4204 0.0549 0.035 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 0.0202(3) 0.0202(3) 0.0129(2) -0.0006(2) -0.0007(2) -0.0011(2) N1 0.0253(19) 0.0268(19) 0.0191(16) -0.0022(14) -0.0032(14) 0.0006(14) N2 0.0218(17) 0.0223(16) 0.0147(14) 0.0005(12) 0.0001(13) 0.0032(14) O1 0.0330(17) 0.0178(14) 0.0216(13) -0.0018(11) -0.0082(12) -0.0017(12) O2 0.0225(15) 0.0251(15) 0.0176(13) 0.0036(11) -0.0018(11) -0.0013(12) O3 0.0209(12) 0.0209(12) 0.0180(18) -0.0015(11) 0.0015(11) -0.0008(16) C1 0.031(2) 0.028(2) 0.0192(18) -0.0031(17) -0.0015(16) 0.0041(18) C2 0.046(3) 0.041(3) 0.018(2) 0.0000(18) -0.0074(19) -0.004(2) C3 0.049(4) 0.066(4) 0.043(3) -0.023(3) -0.015(3) 0.004(3) C4 0.061(4) 0.067(4) 0.062(4) -0.014(3) -0.032(4) 0.003(4) C5 0.093(6) 0.059(4) 0.030(3) -0.007(3) -0.032(3) -0.011(4) C6 0.100(6) 0.087(6) 0.022(2) -0.007(3) -0.005(3) -0.020(5) C7 0.063(4) 0.067(4) 0.019(2) -0.008(2) 0.002(2) -0.014(3) C8 0.042(3) 0.033(3) 0.0214(19) -0.0074(18) -0.0092(19) -0.002(2) C9 0.049(3) 0.022(2) 0.025(2) -0.0032(17) -0.004(2) -0.002(2) C10 0.028(2) 0.026(2) 0.0223(19) -0.0038(16) -0.0017(16) 0.0017(17) C11 0.035(3) 0.021(2) 0.031(2) -0.0002(17) -0.0085(19) -0.0030(18) C12 0.040(3) 0.020(2) 0.034(2) -0.0004(18) -0.010(2) 0.0001(18) C13 0.052(3) 0.024(2) 0.046(3) 0.000(2) -0.013(3) -0.004(2) C14 0.072(4) 0.024(3) 0.055(4) 0.006(2) -0.017(3) -0.011(3) C15 0.114(7) 0.029(3) 0.072(4) -0.004(3) -0.035(5) -0.023(4) C16 0.122(7) 0.031(3) 0.054(4) -0.003(3) -0.032(4) -0.020(4) C17 0.082(5) 0.028(3) 0.041(3) -0.004(2) -0.025(3) -0.012(3) C18 0.071(4) 0.037(3) 0.029(2) -0.010(2) -0.015(3) -0.013(3) C19 0.064(4) 0.018(2) 0.045(3) 0.010(2) -0.027(3) -0.014(2) C20 0.148(8) 0.019(3) 0.027(3) 0.006(2) -0.015(3) -0.024(4) C21 0.175(11) 0.041(4) 0.052(4) 0.026(3) -0.048(5) -0.035(5) C22 0.108(8) 0.047(4) 0.073(5) 0.027(4) -0.008(5) -0.022(5) C23 0.078(5) 0.028(3) 0.159(9) 0.050(5) -0.084(6) -0.035(3) C24 0.094(7) 0.062(5) 0.093(6) 0.020(5) -0.042(6) -0.024(5) C25 0.061(4) 0.035(3) 0.069(4) 0.022(3) -0.029(4) -0.003(3) C26 0.147(10) 0.043(4) 0.130(9) 0.023(5) 0.030(8) -0.046(6) C27 0.048(4) 0.033(3) 0.180(10) 0.048(5) -0.040(6) -0.005(3) C28 0.058(4) 0.031(3) 0.110(6) 0.039(4) -0.050(4) -0.021(3) C29 0.111(7) 0.027(3) 0.061(4) 0.009(3) 0.031(4) 0.010(3) C30 0.106(6) 0.029(3) 0.055(4) 0.008(3) 0.040(4) 0.002(3) C31 0.118(8) 0.044(4) 0.114(7) 0.022(4) 0.072(6) 0.017(4) C32 0.151(12) 0.089(8) 0.204(15) 0.075(9) 0.114(11) 0.031(7) C33 0.116(10) 0.134(11) 0.198(15) 0.106(11) 0.075(10) 0.017(8) C34 0.157(11) 0.053(5) 0.133(9) 0.055(6) 0.072(8) 0.020(6) C35 0.023(2) 0.033(2) 0.0144(17) 0.0013(16) -0.0028(15) 0.0005(17) C36 0.020(2) 0.032(2) 0.0191(18) 0.0009(16) -0.0057(15) -0.0018(17) C37 0.021(2) 0.030(2) 0.028(2) 0.0007(17) -0.0013(17) -0.0016(17) C38 0.030(2) 0.031(2) 0.037(2) 0.000(2) -0.004(2) 0.0009(19) C39 0.032(3) 0.034(3) 0.041(3) 0.014(2) -0.009(2) 0.000(2) C40 0.035(3) 0.043(3) 0.021(2) 0.0096(19) -0.0017(18) -0.006(2) C41 0.025(2) 0.044(3) 0.021(2) 0.0041(19) -0.0019(17) 0.0028(19) C42 0.019(2) 0.025(2) 0.0171(17) 0.0044(15) 0.0008(15) 0.0018(15) C43 0.020(2) 0.028(2) 0.0133(16) -0.0011(15) 0.0008(14) 0.0019(16) C44 0.0193(18) 0.0150(18) 0.0149(16) 0.0002(13) 0.0011(13) -0.0021(14) C45 0.0230(19) 0.0199(19) 0.0178(17) -0.0004(14) -0.0027(15) 0.0001(16) C46 0.021(2) 0.025(2) 0.0174(17) 0.0003(15) 0.0001(15) -0.0005(15) C47 0.023(2) 0.029(2) 0.029(2) 0.0063(18) -0.0046(18) -0.0032(18) C48 0.024(2) 0.033(2) 0.034(2) 0.0071(19) -0.0070(18) -0.0070(18) C49 0.033(2) 0.031(2) 0.033(2) 0.0062(19) 0.000(2) -0.0091(18) C50 0.031(2) 0.023(2) 0.029(2) 0.0077(17) 0.0001(18) -0.0038(17) C51 0.025(2) 0.024(2) 0.0194(18) -0.0008(15) 0.0036(15) -0.0005(16) C52 0.026(2) 0.021(2) 0.0195(18) 0.0024(15) 0.0001(16) 0.0013(16) C53 0.0199(19) 0.022(2) 0.0205(18) 0.0037(16) 0.0014(16) -0.0015(15) C54 0.022(2) 0.026(2) 0.0197(19) 0.0002(16) 0.0036(16) -0.0012(16) C55 0.025(2) 0.023(2) 0.032(2) 0.0046(18) 0.0052(18) 0.0030(17) C56 0.025(2) 0.024(2) 0.029(2) 0.0105(17) 0.0044(17) 0.0017(17) C57 0.021(2) 0.034(2) 0.0213(18) 0.0109(17) -0.0017(15) -0.0009(17) C58 0.030(2) 0.038(3) 0.027(2) 0.0093(19) -0.0051(18) -0.005(2) C59 0.043(3) 0.046(3) 0.025(2) 0.001(2) -0.018(2) -0.004(2) C60 0.052(3) 0.033(3) 0.028(2) -0.005(2) -0.007(2) 0.000(2) C61 0.036(3) 0.031(2) 0.028(2) -0.0011(19) -0.0081(18) 0.002(2) C62 0.020(2) 0.026(2) 0.0233(19) 0.0012(16) 0.0002(16) -0.0034(16) C63 0.019(2) 0.025(2) 0.028(2) -0.0045(17) 0.0034(16) 0.0040(16) C64 0.028(2) 0.028(2) 0.031(2) -0.0027(18) 0.0037(18) 0.0012(18) C65 0.039(3) 0.045(3) 0.038(3) -0.017(2) 0.000(2) 0.003(2) C66 0.048(3) 0.059(4) 0.025(2) -0.014(2) 0.000(2) 0.011(3) C67 0.040(3) 0.048(3) 0.025(2) -0.003(2) 0.008(2) 0.008(2) C68 0.026(2) 0.034(2) 0.028(2) 0.0011(19) 0.0083(17) 0.0021(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O3 1.8038(15) . ? Fe1 O2 1.913(3) . ? Fe1 O1 1.918(3) . ? Fe1 N2 2.100(3) . ? Fe1 N1 2.169(3) . ? N1 C8 1.278(6) . ? N1 C1 1.486(6) . ? N2 C42 1.273(5) . ? N2 C35 1.489(5) . ? O1 C10 1.314(5) . ? O2 C44 1.319(5) . ? O3 Fe1 1.8038(15) 7 ? C1 C2 1.509(6) . ? C1 C35 1.563(6) . ? C1 H1 1.0000 . ? C2 C3 1.362(8) . ? C2 C7 1.390(8) . ? C3 C4 1.392(8) . ? C3 H3 0.9500 . ? C4 C5 1.368(11) . ? C4 H4 0.9500 . ? C5 C6 1.391(11) . ? C5 H5 0.9500 . ? C6 C7 1.380(8) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.460(7) . ? C8 H8 0.9500 . ? C9 C18 1.369(7) . ? C9 C10 1.440(6) . ? C10 C11 1.399(6) . ? C11 C12 1.414(6) . ? C11 C19 1.500(7) . ? C12 C13 1.414(7) . ? C12 C17 1.437(7) . ? C13 C14 1.356(7) . ? C13 H13 0.9500 . ? C14 C15 1.392(9) . ? C14 H14 0.9500 . ? C15 C16 1.348(10) . ? C15 H15 0.9500 . ? C16 C17 1.427(8) . ? C16 H16 0.9500 . ? C17 C18 1.393(8) . ? C18 H18 0.9500 . ? C19 C20 1.389(11) . ? C19 C28 1.404(9) . ? C20 C21 1.398(9) . ? C20 C29 1.471(12) . ? C21 C22 1.248(15) . ? C21 H21 0.9500 . ? C22 C23 1.395(14) . ? C22 H22 0.9500 . ? C23 C24 1.353(12) . ? C23 C28 1.547(13) . ? C24 C25 1.317(13) . ? C24 H24 0.9500 . ? C25 C26 1.373(14) . ? C25 H25 0.9500 . ? C26 C27 1.523(15) . ? C26 H26 0.9500 . ? C27 C28 1.352(14) . ? C27 H27 0.9500 . ? C29 C30 1.375(10) . ? C29 C34 1.412(12) . ? C30 C31 1.382(13) . ? C30 H30 0.9500 . ? C31 C32 1.416(12) . ? C31 H31 0.9500 . ? C32 C33 1.318(16) . ? C32 H32 0.9500 . ? C33 C34 1.407(18) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.499(6) . ? C35 H35 1.0000 . ? C36 C41 1.386(6) . ? C36 C37 1.391(6) . ? C37 C38 1.392(7) . ? C37 H37 0.9500 . ? C38 C39 1.381(7) . ? C38 H38 0.9500 . ? C39 C40 1.375(7) . ? C39 H39 0.9500 . ? C40 C41 1.402(7) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.437(6) . ? C42 H42 0.9500 . ? C43 C52 1.387(6) . ? C43 C44 1.450(6) . ? C44 C45 1.403(6) . ? C45 C46 1.425(6) . ? C45 C53 1.494(6) . ? C46 C47 1.430(6) . ? C46 C51 1.433(6) . ? C47 C48 1.368(6) . ? C47 H47 0.9500 . ? C48 C49 1.416(7) . ? C48 H48 0.9500 . ? C49 C50 1.368(7) . ? C49 H49 0.9500 . ? C50 C51 1.417(6) . ? C50 H50 0.9500 . ? C51 C52 1.386(6) . ? C52 H52 0.9500 . ? C53 C54 1.394(6) . ? C53 C62 1.429(6) . ? C54 C55 1.424(6) . ? C54 C63 1.474(6) . ? C55 C56 1.354(6) . ? C55 H55 0.9500 . ? C56 C57 1.420(7) . ? C56 H56 0.9500 . ? C57 C58 1.428(6) . ? C57 C62 1.430(6) . ? C58 C59 1.361(8) . ? C58 H58 0.9500 . ? C59 C60 1.418(8) . ? C59 H59 0.9500 . ? C60 C61 1.352(7) . ? C60 H60 0.9500 . ? C61 C62 1.425(7) . ? C61 H61 0.9500 . ? C63 C68 1.384(6) . ? C63 C64 1.406(7) . ? C64 C65 1.393(7) . ? C64 H64 0.9500 . ? C65 C66 1.382(9) . ? C65 H65 0.9500 . ? C66 C67 1.400(9) . ? C66 H66 0.9500 . ? C67 C68 1.384(7) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Fe1 O2 115.60(14) . . ? O3 Fe1 O1 105.31(14) . . ? O2 Fe1 O1 97.72(13) . . ? O3 Fe1 N2 92.38(12) . . ? O2 Fe1 N2 86.85(13) . . ? O1 Fe1 N2 157.39(13) . . ? O3 Fe1 N1 109.77(13) . . ? O2 Fe1 N1 131.65(13) . . ? O1 Fe1 N1 85.44(13) . . ? N2 Fe1 N1 75.22(14) . . ? C8 N1 C1 119.3(4) . . ? C8 N1 Fe1 125.6(3) . . ? C1 N1 Fe1 115.0(3) . . ? C42 N2 C35 122.4(3) . . ? C42 N2 Fe1 127.4(3) . . ? C35 N2 Fe1 110.1(3) . . ? C10 O1 Fe1 134.4(3) . . ? C44 O2 Fe1 134.8(3) . . ? Fe1 O3 Fe1 140.6(2) . 7 ? N1 C1 C2 116.1(4) . . ? N1 C1 C35 103.7(3) . . ? C2 C1 C35 115.9(4) . . ? N1 C1 H1 106.8 . . ? C2 C1 H1 106.8 . . ? C35 C1 H1 106.8 . . ? C3 C2 C7 118.7(5) . . ? C3 C2 C1 122.4(5) . . ? C7 C2 C1 118.9(5) . . ? C2 C3 C4 120.5(6) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 121.2(7) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 118.6(6) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C7 C6 C5 119.9(7) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C2 121.1(7) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? N1 C8 C9 126.1(4) . . ? N1 C8 H8 117.0 . . ? C9 C8 H8 117.0 . . ? C18 C9 C10 119.6(5) . . ? C18 C9 C8 117.8(4) . . ? C10 C9 C8 122.5(4) . . ? O1 C10 C11 120.9(4) . . ? O1 C10 C9 121.4(4) . . ? C11 C10 C9 117.7(4) . . ? C10 C11 C12 122.5(4) . . ? C10 C11 C19 119.1(4) . . ? C12 C11 C19 118.4(4) . . ? C13 C12 C11 123.3(4) . . ? C13 C12 C17 118.1(5) . . ? C11 C12 C17 118.5(4) . . ? C14 C13 C12 121.4(5) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 120.9(6) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 120.1(6) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 121.9(6) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C18 C17 C16 124.3(5) . . ? C18 C17 C12 118.1(5) . . ? C16 C17 C12 117.5(5) . . ? C9 C18 C17 123.5(5) . . ? C9 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? C20 C19 C28 120.1(7) . . ? C20 C19 C11 120.6(6) . . ? C28 C19 C11 119.2(7) . . ? C19 C20 C21 121.4(10) . . ? C19 C20 C29 123.7(6) . . ? C21 C20 C29 114.9(9) . . ? C22 C21 C20 121.8(12) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 124.3(10) . . ? C21 C22 H22 117.9 . . ? C23 C22 H22 117.9 . . ? C24 C23 C22 126.2(11) . . ? C24 C23 C28 116.9(12) . . ? C22 C23 C28 117.0(7) . . ? C25 C24 C23 119.1(10) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 130.3(9) . . ? C24 C25 H25 114.8 . . ? C26 C25 H25 114.8 . . ? C25 C26 C27 114.5(11) . . ? C25 C26 H26 122.8 . . ? C27 C26 H26 122.8 . . ? C28 C27 C26 116.9(10) . . ? C28 C27 H27 121.5 . . ? C26 C27 H27 121.5 . . ? C27 C28 C19 122.4(7) . . ? C27 C28 C23 122.2(8) . . ? C19 C28 C23 115.4(9) . . ? C30 C29 C34 116.9(9) . . ? C30 C29 C20 120.6(7) . . ? C34 C29 C20 122.3(8) . . ? C29 C30 C31 121.4(7) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C30 C31 C32 119.5(10) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C33 C32 C31 120.9(13) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 119.0(11) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C33 C34 C29 121.8(9) . . ? C33 C34 H34 119.1 . . ? C29 C34 H34 119.1 . . ? N2 C35 C36 116.3(4) . . ? N2 C35 C1 101.5(3) . . ? C36 C35 C1 116.5(3) . . ? N2 C35 H35 107.3 . . ? C36 C35 H35 107.3 . . ? C1 C35 H35 107.3 . . ? C41 C36 C37 118.7(4) . . ? C41 C36 C35 122.5(4) . . ? C37 C36 C35 118.7(4) . . ? C36 C37 C38 120.5(4) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C39 C38 C37 120.4(5) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C40 C39 C38 119.6(5) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 120.2(5) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C36 C41 C40 120.5(5) . . ? C36 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? N2 C42 C43 124.7(4) . . ? N2 C42 H42 117.6 . . ? C43 C42 H42 117.6 . . ? C52 C43 C42 117.3(4) . . ? C52 C43 C44 119.1(4) . . ? C42 C43 C44 123.4(4) . . ? O2 C44 C45 120.2(3) . . ? O2 C44 C43 121.0(4) . . ? C45 C44 C43 118.7(4) . . ? C44 C45 C46 120.3(4) . . ? C44 C45 C53 119.6(4) . . ? C46 C45 C53 119.8(4) . . ? C45 C46 C47 122.9(4) . . ? C45 C46 C51 120.4(4) . . ? C47 C46 C51 116.6(4) . . ? C48 C47 C46 121.5(4) . . ? C48 C47 H47 119.3 . . ? C46 C47 H47 119.3 . . ? C47 C48 C49 121.6(4) . . ? C47 C48 H48 119.2 . . ? C49 C48 H48 119.2 . . ? C50 C49 C48 118.5(4) . . ? C50 C49 H49 120.7 . . ? C48 C49 H49 120.7 . . ? C49 C50 C51 121.7(4) . . ? C49 C50 H50 119.1 . . ? C51 C50 H50 119.1 . . ? C52 C51 C50 122.0(4) . . ? C52 C51 C46 117.8(4) . . ? C50 C51 C46 120.1(4) . . ? C51 C52 C43 123.4(4) . . ? C51 C52 H52 118.3 . . ? C43 C52 H52 118.3 . . ? C54 C53 C62 119.7(4) . . ? C54 C53 C45 119.6(4) . . ? C62 C53 C45 120.6(4) . . ? C53 C54 C55 118.7(4) . . ? C53 C54 C63 122.0(4) . . ? C55 C54 C63 119.3(4) . . ? C56 C55 C54 122.5(4) . . ? C56 C55 H55 118.8 . . ? C54 C55 H55 118.8 . . ? C55 C56 C57 120.3(4) . . ? C55 C56 H56 119.9 . . ? C57 C56 H56 119.9 . . ? C56 C57 C58 122.2(4) . . ? C56 C57 C62 118.4(4) . . ? C58 C57 C62 119.4(4) . . ? C59 C58 C57 120.0(4) . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C58 C59 C60 120.8(4) . . ? C58 C59 H59 119.6 . . ? C60 C59 H59 119.6 . . ? C61 C60 C59 120.1(5) . . ? C61 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C60 C61 C62 121.8(5) . . ? C60 C61 H61 119.1 . . ? C62 C61 H61 119.1 . . ? C61 C62 C53 122.4(4) . . ? C61 C62 C57 117.6(4) . . ? C53 C62 C57 120.0(4) . . ? C68 C63 C64 118.6(4) . . ? C68 C63 C54 122.2(4) . . ? C64 C63 C54 119.1(4) . . ? C65 C64 C63 120.5(5) . . ? C65 C64 H64 119.7 . . ? C63 C64 H64 119.7 . . ? C66 C65 C64 119.9(5) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C65 C66 C67 120.0(5) . . ? C65 C66 H66 120.0 . . ? C67 C66 H66 120.0 . . ? C68 C67 C66 119.7(5) . . ? C68 C67 H67 120.2 . . ? C66 C67 H67 120.2 . . ? C63 C68 C67 121.3(5) . . ? C63 C68 H68 119.4 . . ? C67 C68 H68 119.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.271 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.148 # Attachment '8251_web_deposit_cif_file_0_KenjiMatsumoto_1321546181.complex3_Fe_Jacobsen-salan-dimer_KM37_2_final.cif' data_R-Cy-24ditBuPh-FeNHsalan-diOH-dimer _database_code_depnum_ccdc_archive 'CCDC 854407' #TrackingRef '8251_web_deposit_cif_file_0_KenjiMatsumoto_1321546181.complex3_Fe_Jacobsen-salan-dimer_KM37_2_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C147 H234 Fe4 N8 O13' _chemical_formula_sum 'C147 H234 Fe4 N8 O13' _chemical_formula_weight 2544.82 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.0266(13) _cell_length_b 19.7736(19) _cell_length_c 28.953(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7457.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9884 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.45 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9173 _exptl_absorpt_correction_T_max 0.9784 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 'focusing mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 39867 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0912 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.52 _reflns_number_total 16754 _reflns_number_gt 11984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+18.9667P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 7464 Friedel pairs' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 16754 _refine_ls_number_parameters 819 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1282 _refine_ls_R_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.1920 _refine_ls_wR_factor_gt 0.1792 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.51172(7) 0.55508(4) 0.07843(3) 0.02551(19) Uani 1 1 d . . . Fe2 Fe 0.49558(7) 0.58876(4) 0.18565(2) 0.02327(18) Uani 1 1 d . . . N1 N 0.3459(3) 0.5473(3) 0.07798(17) 0.0259(11) Uani 1 1 d . . . H1N H 0.3262 0.5415 0.1086 0.031 Uiso 1 1 calc R . . N2 N 0.4862(4) 0.4583(2) 0.04282(16) 0.0321(12) Uani 1 1 d . . . H2N H 0.4823 0.4680 0.0114 0.038 Uiso 1 1 calc R . . N3 N 0.6635(3) 0.5783(2) 0.19110(16) 0.0228(11) Uani 1 1 d . . . H3N H 0.6846 0.5498 0.1674 0.027 Uiso 1 1 calc R . . N4 N 0.5149(4) 0.5319(2) 0.24997(15) 0.0220(10) Uani 1 1 d . . . H4N H 0.5194 0.5643 0.2732 0.026 Uiso 1 1 calc R . . O1 O 0.4989(4) 0.60796(18) 0.02338(11) 0.0288(8) Uani 1 1 d . . . O2 O 0.6569(3) 0.5353(3) 0.07754(17) 0.0419(12) Uani 1 1 d . . . O3 O 0.5063(3) 0.63063(17) 0.12342(10) 0.0226(8) Uani 1 1 d . . . O4 O 0.5031(4) 0.50614(17) 0.14250(11) 0.0260(8) Uani 1 1 d . . . O5 O 0.5111(3) 0.67123(17) 0.21958(12) 0.0236(8) Uani 1 1 d . . . O6 O 0.3498(3) 0.5742(2) 0.19042(14) 0.0277(10) Uani 1 1 d . . . O7 O 0.7376(11) 0.4250(10) 0.1417(5) 0.104(5) Uani 0.50 1 d P . . C1 C 0.3066(5) 0.4878(3) 0.0526(2) 0.0267(14) Uani 1 1 d . . . H1 H 0.3043 0.5009 0.0192 0.032 Uiso 1 1 calc R . . C2 C 0.1991(5) 0.4652(3) 0.0654(2) 0.0370(16) Uani 1 1 d . . . H2A H 0.1505 0.5030 0.0603 0.044 Uiso 1 1 calc R . . H2B H 0.1972 0.4533 0.0986 0.044 Uiso 1 1 calc R . . C3 C 0.1656(6) 0.4046(4) 0.0370(3) 0.053(2) Uani 1 1 d . . . H3A H 0.1604 0.4179 0.0041 0.064 Uiso 1 1 calc R . . H3B H 0.0967 0.3897 0.0474 0.064 Uiso 1 1 calc R . . C4 C 0.2407(6) 0.3463(4) 0.0417(3) 0.0485(19) Uani 1 1 d . . . H4A H 0.2194 0.3089 0.0211 0.058 Uiso 1 1 calc R . . H4B H 0.2395 0.3293 0.0739 0.058 Uiso 1 1 calc R . . C5 C 0.3502(5) 0.3686(3) 0.0293(2) 0.0378(16) Uani 1 1 d . . . H5A H 0.3982 0.3309 0.0355 0.045 Uiso 1 1 calc R . . H5B H 0.3535 0.3790 -0.0041 0.045 Uiso 1 1 calc R . . C6 C 0.3841(5) 0.4303(3) 0.0565(2) 0.0287(14) Uani 1 1 d . . . H6 H 0.3883 0.4170 0.0898 0.034 Uiso 1 1 calc R . . C7 C 0.2985(5) 0.6124(3) 0.06249(19) 0.0263(13) Uani 1 1 d . . . H7A H 0.3281 0.6505 0.0803 0.032 Uiso 1 1 calc R . . H7B H 0.2236 0.6113 0.0683 0.032 Uiso 1 1 calc R . . C8 C 0.3183(4) 0.6230(3) 0.01144(19) 0.0241(13) Uani 1 1 d . . . C9 C 0.4192(5) 0.6217(3) -0.00559(19) 0.0260(13) Uani 1 1 d . . . C10 C 0.4363(5) 0.6351(3) -0.05291(18) 0.0232(13) Uani 1 1 d . . . C11 C 0.3498(5) 0.6453(3) -0.08074(18) 0.0261(13) Uani 1 1 d . . . H11 H 0.3604 0.6536 -0.1127 0.031 Uiso 1 1 calc R . . C12 C 0.2487(5) 0.6440(3) -0.0644(2) 0.0269(13) Uani 1 1 d . . . C13 C 0.2348(5) 0.6337(3) -0.0177(2) 0.0263(13) Uani 1 1 d . . . H13 H 0.1674 0.6340 -0.0053 0.032 Uiso 1 1 calc R . . C14 C 0.5447(5) 0.6412(3) -0.0725(2) 0.0284(14) Uani 1 1 d . . . C15 C 0.6077(5) 0.5763(3) -0.06441(19) 0.0311(15) Uani 1 1 d . . . H15A H 0.6097 0.5661 -0.0313 0.047 Uiso 1 1 calc R . . H15B H 0.6778 0.5829 -0.0759 0.047 Uiso 1 1 calc R . . H15C H 0.5756 0.5386 -0.0809 0.047 Uiso 1 1 calc R . . C16 C 0.5984(6) 0.7018(4) -0.0501(3) 0.048(2) Uani 1 1 d . . . H16A H 0.5660 0.7437 -0.0606 0.072 Uiso 1 1 calc R . . H16B H 0.6711 0.7019 -0.0589 0.072 Uiso 1 1 calc R . . H16C H 0.5926 0.6984 -0.0164 0.072 Uiso 1 1 calc R . . C17 C 0.5435(5) 0.6534(3) -0.1251(2) 0.0378(16) Uani 1 1 d . . . H17A H 0.5140 0.6139 -0.1406 0.057 Uiso 1 1 calc R . . H17B H 0.6138 0.6607 -0.1361 0.057 Uiso 1 1 calc R . . H17C H 0.5018 0.6934 -0.1320 0.057 Uiso 1 1 calc R . . C18 C 0.1554(5) 0.6530(3) -0.0963(2) 0.0321(15) Uani 1 1 d . . . C19 C 0.1865(6) 0.6627(4) -0.1472(2) 0.0488(19) Uani 1 1 d . . . H19A H 0.2352 0.7003 -0.1497 0.073 Uiso 1 1 calc R . . H19B H 0.1253 0.6727 -0.1657 0.073 Uiso 1 1 calc R . . H19C H 0.2187 0.6212 -0.1587 0.073 Uiso 1 1 calc R . . C20 C 0.0907(6) 0.7136(3) -0.0808(3) 0.0466(19) Uani 1 1 d . . . H20A H 0.0701 0.7075 -0.0485 0.070 Uiso 1 1 calc R . . H20B H 0.0294 0.7169 -0.1003 0.070 Uiso 1 1 calc R . . H20C H 0.1312 0.7551 -0.0838 0.070 Uiso 1 1 calc R . . C21 C 0.0871(5) 0.5900(3) -0.0939(2) 0.0338(15) Uani 1 1 d . . . H21A H 0.1269 0.5502 -0.1034 0.051 Uiso 1 1 calc R . . H21B H 0.0283 0.5956 -0.1147 0.051 Uiso 1 1 calc R . . H21C H 0.0626 0.5837 -0.0622 0.051 Uiso 1 1 calc R . . C22 C 0.5723(5) 0.4119(4) 0.0488(2) 0.0379(15) Uani 1 1 d . . . H22A H 0.5560 0.3680 0.0340 0.046 Uiso 1 1 calc R . . H22B H 0.5837 0.4036 0.0821 0.046 Uiso 1 1 calc R . . C23 C 0.6683(5) 0.4408(3) 0.0277(2) 0.0351(15) Uani 1 1 d . . . C24 C 0.7070(5) 0.5021(4) 0.0441(2) 0.0332(16) Uani 1 1 d . . . C25 C 0.8028(5) 0.5259(3) 0.0273(2) 0.0366(16) Uani 1 1 d . . . C26 C 0.8487(5) 0.4900(3) -0.0086(2) 0.0350(15) Uani 1 1 d . . . H26 H 0.9109 0.5070 -0.0211 0.042 Uiso 1 1 calc R . . C27 C 0.8088(5) 0.4308(3) -0.0271(2) 0.0323(15) Uani 1 1 d . . . C28 C 0.7188(5) 0.4073(3) -0.0077(2) 0.0352(15) Uani 1 1 d . . . H28 H 0.6903 0.3664 -0.0191 0.042 Uiso 1 1 calc R . . C29 C 0.8520(5) 0.5890(5) 0.0479(3) 0.060(2) Uani 1 1 d . . . C30 C 0.8778(6) 0.5712(7) 0.0997(3) 0.102(5) Uani 1 1 d . . . H30A H 0.9039 0.6116 0.1154 0.153 Uiso 1 1 calc R . . H30B H 0.9300 0.5356 0.1006 0.153 Uiso 1 1 calc R . . H30C H 0.8155 0.5554 0.1153 0.153 Uiso 1 1 calc R . . C31 C 0.7845(6) 0.6504(4) 0.0444(4) 0.097(4) Uani 1 1 d . . . H31A H 0.8167 0.6882 0.0608 0.146 Uiso 1 1 calc R . . H31B H 0.7175 0.6406 0.0583 0.146 Uiso 1 1 calc R . . H31C H 0.7752 0.6625 0.0119 0.146 Uiso 1 1 calc R . . C32 C 0.9544(5) 0.6051(4) 0.0249(3) 0.067(3) Uani 1 1 d . . . H32A H 0.9431 0.6150 -0.0078 0.100 Uiso 1 1 calc R . . H32B H 1.0005 0.5662 0.0280 0.100 Uiso 1 1 calc R . . H32C H 0.9854 0.6446 0.0400 0.100 Uiso 1 1 calc R . . C33 C 0.8602(6) 0.3924(3) -0.0667(2) 0.0411(17) Uani 1 1 d . . . C34 C 0.7832(7) 0.3820(5) -0.1061(3) 0.063(2) Uani 1 1 d . . . H34A H 0.7604 0.4261 -0.1177 0.094 Uiso 1 1 calc R . . H34B H 0.7239 0.3566 -0.0946 0.094 Uiso 1 1 calc R . . H34C H 0.8161 0.3567 -0.1312 0.094 Uiso 1 1 calc R . . C35 C 0.8988(7) 0.3241(4) -0.0489(3) 0.068(3) Uani 1 1 d . . . H35A H 0.9346 0.3002 -0.0738 0.102 Uiso 1 1 calc R . . H35B H 0.8404 0.2969 -0.0383 0.102 Uiso 1 1 calc R . . H35C H 0.9462 0.3315 -0.0231 0.102 Uiso 1 1 calc R . . C36 C 0.9520(5) 0.4309(3) -0.0867(2) 0.0454(18) Uani 1 1 d . . . H36A H 0.9801 0.4058 -0.1130 0.068 Uiso 1 1 calc R . . H36B H 1.0050 0.4357 -0.0629 0.068 Uiso 1 1 calc R . . H36C H 0.9297 0.4758 -0.0970 0.068 Uiso 1 1 calc R . . C37 C 0.6952(4) 0.5466(3) 0.2352(2) 0.0270(13) Uani 1 1 d . . . H37 H 0.6972 0.5832 0.2590 0.032 Uiso 1 1 calc R . . C38 C 0.8016(5) 0.5139(3) 0.2344(3) 0.0414(17) Uani 1 1 d . . . H38A H 0.8023 0.4766 0.2116 0.050 Uiso 1 1 calc R . . H38B H 0.8531 0.5479 0.2247 0.050 Uiso 1 1 calc R . . C39 C 0.8292(5) 0.4870(4) 0.2809(3) 0.053(2) Uani 1 1 d . . . H39A H 0.8343 0.5249 0.3031 0.063 Uiso 1 1 calc R . . H39B H 0.8971 0.4646 0.2793 0.063 Uiso 1 1 calc R . . C40 C 0.7494(5) 0.4364(4) 0.2980(2) 0.0412(17) Uani 1 1 d . . . H40A H 0.7672 0.4219 0.3297 0.049 Uiso 1 1 calc R . . H40B H 0.7504 0.3959 0.2779 0.049 Uiso 1 1 calc R . . C41 C 0.6417(5) 0.4668(3) 0.2979(2) 0.0335(15) Uani 1 1 d . . . H41A H 0.6379 0.5030 0.3214 0.040 Uiso 1 1 calc R . . H41B H 0.5914 0.4314 0.3064 0.040 Uiso 1 1 calc R . . C42 C 0.6135(5) 0.4960(3) 0.2506(2) 0.0238(13) Uani 1 1 d . . . H42 H 0.6106 0.4583 0.2277 0.029 Uiso 1 1 calc R . . C43 C 0.7129(5) 0.6450(3) 0.1832(2) 0.0270(13) Uani 1 1 d . . . H43A H 0.6885 0.6637 0.1535 0.032 Uiso 1 1 calc R . . H43B H 0.7881 0.6386 0.1808 0.032 Uiso 1 1 calc R . . C44 C 0.6907(5) 0.6951(3) 0.22104(18) 0.0239(13) Uani 1 1 d . . . C45 C 0.5904(5) 0.7063(3) 0.23705(19) 0.0254(13) Uani 1 1 d . . . C46 C 0.5741(5) 0.7550(3) 0.27216(18) 0.0228(12) Uani 1 1 d . . . C47 C 0.6588(5) 0.7924(3) 0.2869(2) 0.0284(14) Uani 1 1 d . . . H47 H 0.6478 0.8258 0.3099 0.034 Uiso 1 1 calc R . . C48 C 0.7586(5) 0.7842(3) 0.27012(19) 0.0261(13) Uani 1 1 d . . . C49 C 0.7723(5) 0.7335(3) 0.23758(19) 0.0259(13) Uani 1 1 d . . . H49 H 0.8395 0.7247 0.2263 0.031 Uiso 1 1 calc R . . C50 C 0.4678(5) 0.7671(3) 0.2927(2) 0.0329(15) Uani 1 1 d . . . C51 C 0.4258(5) 0.7020(3) 0.3131(2) 0.0391(16) Uani 1 1 d . . . H51A H 0.4203 0.6678 0.2888 0.059 Uiso 1 1 calc R . . H51B H 0.3578 0.7105 0.3264 0.059 Uiso 1 1 calc R . . H51C H 0.4723 0.6858 0.3373 0.059 Uiso 1 1 calc R . . C52 C 0.3967(5) 0.7929(4) 0.2544(3) 0.0452(18) Uani 1 1 d . . . H52A H 0.4197 0.8377 0.2442 0.068 Uiso 1 1 calc R . . H52B H 0.3263 0.7960 0.2662 0.068 Uiso 1 1 calc R . . H52C H 0.3986 0.7615 0.2282 0.068 Uiso 1 1 calc R . . C53 C 0.4690(5) 0.8202(3) 0.3316(2) 0.0414(18) Uani 1 1 d . . . H53A H 0.5134 0.8045 0.3567 0.062 Uiso 1 1 calc R . . H53B H 0.3991 0.8267 0.3433 0.062 Uiso 1 1 calc R . . H53C H 0.4952 0.8632 0.3195 0.062 Uiso 1 1 calc R . . C54 C 0.8498(5) 0.8265(3) 0.2866(2) 0.0352(15) Uani 1 1 d . . . C55 C 0.8160(6) 0.8857(4) 0.3171(3) 0.054(2) Uani 1 1 d . . . H55A H 0.7826 0.8682 0.3450 0.081 Uiso 1 1 calc R . . H55B H 0.7676 0.9142 0.3000 0.081 Uiso 1 1 calc R . . H55C H 0.8761 0.9126 0.3258 0.081 Uiso 1 1 calc R . . C56 C 0.9082(6) 0.8550(4) 0.2449(2) 0.051(2) Uani 1 1 d . . . H56A H 0.9673 0.8812 0.2557 0.076 Uiso 1 1 calc R . . H56B H 0.8625 0.8844 0.2270 0.076 Uiso 1 1 calc R . . H56C H 0.9320 0.8177 0.2254 0.076 Uiso 1 1 calc R . . C57 C 0.9224(6) 0.7812(4) 0.3140(3) 0.0515(19) Uani 1 1 d . . . H57A H 0.9812 0.8078 0.3247 0.077 Uiso 1 1 calc R . . H57B H 0.9465 0.7442 0.2943 0.077 Uiso 1 1 calc R . . H57C H 0.8859 0.7624 0.3407 0.077 Uiso 1 1 calc R . . C58 C 0.4217(5) 0.4915(3) 0.2608(2) 0.0324(15) Uani 1 1 d . . . H58A H 0.4339 0.4647 0.2892 0.039 Uiso 1 1 calc R . . H58B H 0.4078 0.4597 0.2352 0.039 Uiso 1 1 calc R . . C59 C 0.3305(5) 0.5363(3) 0.2679(2) 0.0290(14) Uani 1 1 d . . . C60 C 0.2958(5) 0.5752(3) 0.2303(2) 0.0252(13) Uani 1 1 d . . . C61 C 0.2045(5) 0.6126(3) 0.2352(2) 0.0251(13) Uani 1 1 d . . . C62 C 0.1585(5) 0.6154(3) 0.27851(19) 0.0264(13) Uani 1 1 d . . . H62 H 0.0988 0.6424 0.2821 0.032 Uiso 1 1 calc R . . C63 C 0.1958(5) 0.5803(3) 0.3170(2) 0.0280(13) Uani 1 1 d . . . C64 C 0.2802(4) 0.5396(3) 0.3098(2) 0.0270(13) Uani 1 1 d . . . H64 H 0.3048 0.5128 0.3347 0.032 Uiso 1 1 calc R . . C65 C 0.1527(5) 0.6460(3) 0.1931(2) 0.0305(14) Uani 1 1 d . . . C66 C 0.2225(5) 0.6983(3) 0.1704(2) 0.0359(16) Uani 1 1 d . . . H66A H 0.1922 0.7128 0.1410 0.054 Uiso 1 1 calc R . . H66B H 0.2900 0.6781 0.1647 0.054 Uiso 1 1 calc R . . H66C H 0.2300 0.7374 0.1909 0.054 Uiso 1 1 calc R . . C67 C 0.1268(5) 0.5894(4) 0.1585(2) 0.0361(15) Uani 1 1 d . . . H67A H 0.0756 0.5590 0.1721 0.054 Uiso 1 1 calc R . . H67B H 0.1891 0.5639 0.1512 0.054 Uiso 1 1 calc R . . H67C H 0.0990 0.6094 0.1301 0.054 Uiso 1 1 calc R . . C68 C 0.0506(5) 0.6811(4) 0.2055(2) 0.0421(18) Uani 1 1 d . . . H68A H 0.0633 0.7163 0.2287 0.063 Uiso 1 1 calc R . . H68B H 0.0025 0.6477 0.2180 0.063 Uiso 1 1 calc R . . H68C H 0.0212 0.7018 0.1777 0.063 Uiso 1 1 calc R . . C69 C 0.1418(5) 0.5882(3) 0.36424(19) 0.0301(14) Uani 1 1 d . . . C70 C 0.1822(6) 0.5402(4) 0.4003(2) 0.056(2) Uani 1 1 d . . . H70A H 0.2516 0.5539 0.4093 0.084 Uiso 1 1 calc R . . H70B H 0.1840 0.4943 0.3876 0.084 Uiso 1 1 calc R . . H70C H 0.1371 0.5412 0.4274 0.084 Uiso 1 1 calc R . . C71 C 0.1488(7) 0.6598(4) 0.3803(3) 0.064(2) Uani 1 1 d . . . H71A H 0.1105 0.6649 0.4093 0.096 Uiso 1 1 calc R . . H71B H 0.1197 0.6898 0.3568 0.096 Uiso 1 1 calc R . . H71C H 0.2210 0.6717 0.3855 0.096 Uiso 1 1 calc R . . C72 C 0.0261(6) 0.5715(5) 0.3584(3) 0.065(2) Uani 1 1 d . . . H72A H -0.0087 0.5761 0.3882 0.098 Uiso 1 1 calc R . . H72B H 0.0186 0.5250 0.3471 0.098 Uiso 1 1 calc R . . H72C H -0.0045 0.6029 0.3361 0.098 Uiso 1 1 calc R . . C73 C 0.9093(18) 0.424(2) 0.1146(14) 0.25(3) Uani 0.50 1 d P . . H73A H 0.9275 0.4453 0.1440 0.374 Uiso 0.50 1 calc PR . . H73B H 0.9073 0.4579 0.0901 0.374 Uiso 0.50 1 calc PR . . H73C H 0.9607 0.3893 0.1070 0.374 Uiso 0.50 1 calc PR . . C74 C 0.805(2) 0.3909(18) 0.1189(10) 0.126(12) Uani 0.50 1 d P . . C75 C 0.787(3) 0.3231(15) 0.0976(9) 0.147(14) Uani 0.50 1 d P . . H75A H 0.8080 0.2876 0.1192 0.221 Uiso 0.50 1 calc PR . . H75B H 0.8273 0.3192 0.0691 0.221 Uiso 0.50 1 calc PR . . H75C H 0.7140 0.3181 0.0904 0.221 Uiso 0.50 1 calc PR . . 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 0.0222(4) 0.0365(4) 0.0179(4) -0.0058(3) -0.0030(4) 0.0038(4) Fe2 0.0288(5) 0.0246(4) 0.0163(3) -0.0004(3) -0.0047(4) 0.0026(4) N1 0.022(3) 0.043(3) 0.013(2) 0.000(2) 0.001(2) 0.003(2) N2 0.037(3) 0.035(3) 0.024(2) -0.001(2) 0.000(2) 0.006(3) N3 0.022(3) 0.026(3) 0.020(3) -0.011(2) 0.000(2) 0.005(2) N4 0.017(3) 0.023(2) 0.026(2) -0.0016(18) -0.006(2) 0.001(2) O1 0.026(2) 0.042(2) 0.0182(17) -0.0004(15) 0.000(2) 0.003(2) O2 0.025(2) 0.064(3) 0.036(3) -0.024(3) -0.005(2) 0.012(2) O3 0.026(2) 0.0295(18) 0.0119(16) -0.0007(14) -0.0032(19) 0.002(2) O4 0.030(2) 0.0295(19) 0.0186(17) -0.0028(15) -0.009(2) 0.003(2) O5 0.023(2) 0.0248(18) 0.0235(18) -0.0037(15) -0.0017(19) 0.0010(19) O6 0.027(2) 0.038(2) 0.019(2) 0.0021(19) -0.0052(18) 0.0097(19) O7 0.065(10) 0.160(16) 0.087(11) 0.006(11) -0.013(8) -0.024(10) C1 0.033(4) 0.034(3) 0.013(3) 0.011(3) 0.001(2) -0.001(3) C2 0.027(4) 0.038(4) 0.046(4) 0.012(3) 0.005(3) -0.005(3) C3 0.042(5) 0.055(5) 0.062(5) -0.002(4) 0.003(4) -0.017(4) C4 0.044(5) 0.041(4) 0.061(5) -0.002(4) -0.002(4) -0.014(4) C5 0.040(4) 0.046(4) 0.028(3) -0.002(3) 0.001(3) -0.004(3) C6 0.039(4) 0.031(3) 0.015(3) 0.004(2) 0.001(3) 0.003(3) C7 0.027(3) 0.031(3) 0.021(3) 0.007(2) 0.001(2) 0.003(3) C8 0.026(3) 0.025(3) 0.020(3) -0.001(2) 0.002(2) -0.001(2) C9 0.029(3) 0.024(3) 0.025(3) -0.006(2) -0.001(3) -0.001(3) C10 0.033(3) 0.022(3) 0.015(3) -0.001(2) 0.002(2) -0.005(2) C11 0.048(4) 0.025(3) 0.005(2) 0.003(2) 0.002(3) -0.003(3) C12 0.033(4) 0.020(3) 0.027(3) 0.001(2) -0.003(3) 0.001(3) C13 0.027(3) 0.027(3) 0.025(3) 0.004(3) 0.002(2) 0.003(3) C14 0.037(4) 0.028(3) 0.019(3) -0.006(3) 0.011(3) -0.004(3) C15 0.041(4) 0.037(4) 0.015(3) -0.001(3) 0.006(2) 0.001(3) C16 0.048(5) 0.045(4) 0.052(5) -0.009(4) 0.025(4) -0.016(4) C17 0.046(4) 0.038(4) 0.029(3) 0.011(3) 0.016(3) 0.005(3) C18 0.041(4) 0.032(3) 0.023(3) 0.002(3) -0.012(3) -0.003(3) C19 0.054(5) 0.063(5) 0.029(4) 0.012(4) -0.013(3) -0.009(4) C20 0.055(5) 0.029(3) 0.055(5) -0.001(3) -0.028(4) 0.004(3) C21 0.039(4) 0.037(3) 0.025(3) -0.009(3) -0.007(3) -0.004(3) C22 0.035(4) 0.045(4) 0.034(4) 0.001(3) -0.001(3) 0.006(3) C23 0.032(4) 0.039(4) 0.035(4) -0.001(3) -0.001(3) 0.009(3) C24 0.018(3) 0.050(4) 0.031(4) -0.012(3) -0.005(3) 0.011(3) C25 0.023(3) 0.048(4) 0.040(4) -0.012(3) -0.007(3) 0.003(3) C26 0.026(4) 0.042(4) 0.037(4) -0.009(3) -0.006(3) 0.007(3) C27 0.033(4) 0.030(3) 0.034(4) 0.002(3) 0.005(3) 0.013(3) C28 0.040(4) 0.028(3) 0.037(4) -0.007(3) -0.004(3) 0.003(3) C29 0.020(4) 0.088(6) 0.072(5) -0.054(5) 0.008(4) -0.004(4) C30 0.036(5) 0.213(13) 0.058(6) -0.083(7) 0.009(4) -0.025(7) C31 0.036(5) 0.059(6) 0.197(12) -0.067(7) 0.022(6) -0.011(4) C32 0.028(4) 0.076(6) 0.096(7) -0.061(5) 0.013(4) -0.006(4) C33 0.049(4) 0.033(4) 0.041(4) -0.012(3) 0.016(3) 0.007(3) C34 0.069(6) 0.079(6) 0.039(4) -0.028(4) 0.009(4) -0.022(5) C35 0.076(7) 0.038(4) 0.091(7) -0.004(4) 0.045(5) 0.017(4) C36 0.052(5) 0.040(4) 0.044(4) -0.014(3) 0.010(3) -0.004(3) C37 0.023(3) 0.029(3) 0.030(3) -0.007(3) -0.006(3) 0.006(3) C38 0.023(4) 0.040(4) 0.062(5) -0.005(4) -0.003(3) 0.006(3) C39 0.027(4) 0.055(5) 0.076(6) -0.006(4) -0.014(4) 0.016(3) C40 0.032(4) 0.046(4) 0.045(4) 0.006(3) -0.016(3) 0.010(3) C41 0.031(4) 0.037(4) 0.032(3) 0.000(3) -0.010(3) 0.008(3) C42 0.030(3) 0.023(3) 0.019(3) -0.006(2) -0.004(2) 0.007(3) C43 0.026(3) 0.034(3) 0.021(3) 0.000(3) 0.004(3) -0.001(3) C44 0.036(4) 0.021(3) 0.014(3) 0.002(2) 0.004(2) 0.002(3) C45 0.034(4) 0.025(3) 0.017(3) 0.009(2) 0.000(2) 0.005(3) C46 0.039(4) 0.018(3) 0.011(3) 0.003(2) 0.004(2) 0.004(3) C47 0.038(4) 0.025(3) 0.022(3) -0.006(3) 0.004(3) 0.002(3) C48 0.037(4) 0.027(3) 0.015(3) 0.004(2) 0.001(3) -0.002(3) C49 0.025(3) 0.030(3) 0.023(3) -0.001(3) 0.001(2) 0.000(3) C50 0.032(4) 0.031(3) 0.036(4) 0.001(3) 0.005(3) 0.004(3) C51 0.042(4) 0.038(4) 0.037(4) -0.011(3) 0.010(3) 0.001(3) C52 0.039(5) 0.044(4) 0.052(5) -0.004(4) 0.006(3) 0.014(3) C53 0.044(5) 0.039(4) 0.042(4) -0.015(3) 0.015(3) 0.000(3) C54 0.038(4) 0.040(4) 0.027(3) -0.009(3) -0.002(3) -0.002(3) C55 0.049(5) 0.057(5) 0.056(5) -0.028(4) 0.002(4) -0.011(4) C56 0.051(5) 0.056(5) 0.045(4) -0.007(4) 0.000(4) -0.023(4) C57 0.052(5) 0.062(5) 0.040(4) -0.011(4) -0.009(4) 0.001(4) C58 0.029(3) 0.031(3) 0.037(4) 0.008(3) -0.003(3) 0.002(3) C59 0.022(3) 0.027(3) 0.037(4) 0.006(3) -0.009(3) 0.000(2) C60 0.027(3) 0.024(3) 0.025(3) 0.001(2) -0.003(2) -0.001(2) C61 0.026(3) 0.024(3) 0.025(3) 0.000(2) -0.004(2) 0.005(2) C62 0.028(3) 0.029(3) 0.023(3) -0.002(2) -0.001(2) 0.003(3) C63 0.029(3) 0.027(3) 0.027(3) 0.003(3) -0.001(3) -0.001(3) C64 0.029(3) 0.029(3) 0.023(3) 0.016(3) -0.007(3) -0.003(2) C65 0.021(3) 0.041(4) 0.030(3) 0.005(3) -0.002(3) 0.011(3) C66 0.029(4) 0.047(4) 0.031(4) 0.011(3) -0.001(3) 0.005(3) C67 0.024(3) 0.058(4) 0.026(3) 0.002(3) -0.006(3) 0.005(3) C68 0.030(4) 0.061(5) 0.035(4) 0.013(3) -0.001(3) 0.018(3) C69 0.032(4) 0.038(3) 0.020(3) 0.008(3) -0.001(2) -0.003(3) C70 0.064(6) 0.073(6) 0.031(4) 0.007(4) 0.006(4) 0.015(4) C71 0.091(7) 0.061(5) 0.039(4) -0.001(4) 0.028(4) -0.006(5) C72 0.045(5) 0.103(7) 0.047(5) 0.008(4) 0.012(4) -0.009(5) C73 0.045(15) 0.40(6) 0.31(5) 0.26(5) 0.06(2) 0.07(2) C74 0.086(19) 0.18(3) 0.12(2) 0.07(2) 0.044(17) 0.05(2) C75 0.21(4) 0.13(2) 0.10(2) 0.038(19) 0.04(2) 0.11(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.914(3) . ? Fe1 O2 1.931(4) . ? Fe1 O3 1.983(3) . ? Fe1 O4 2.095(3) . ? Fe1 N1 2.165(5) . ? Fe1 N2 2.199(5) . ? Fe2 O5 1.914(3) . ? Fe2 O6 1.926(4) . ? Fe2 O3 1.988(3) . ? Fe2 O4 2.059(3) . ? Fe2 N4 2.190(4) . ? Fe2 N3 2.203(5) . ? N1 C1 1.479(8) . ? N1 C7 1.497(7) . ? N1 H1N 0.9300 . ? N2 C22 1.461(8) . ? N2 C6 1.495(8) . ? N2 H2N 0.9300 . ? N3 C37 1.481(8) . ? N3 C43 1.486(7) . ? N3 H3N 0.9300 . ? N4 C42 1.467(7) . ? N4 C58 1.486(8) . ? N4 H4N 0.9300 . ? O1 C9 1.362(7) . ? O2 C24 1.339(7) . ? O5 C45 1.343(7) . ? O6 C60 1.353(7) . ? O7 C74 1.29(3) . ? C1 C2 1.517(9) . ? C1 C6 1.525(8) . ? C1 H1 1.0000 . ? C2 C3 1.517(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.518(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.536(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.518(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6 1.0000 . ? C7 C8 1.515(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.393(8) . ? C8 C9 1.404(8) . ? C9 C10 1.413(8) . ? C10 C11 1.399(8) . ? C10 C14 1.527(8) . ? C11 C12 1.400(8) . ? C11 H11 0.9500 . ? C12 C13 1.379(8) . ? C12 C18 1.536(8) . ? C13 H13 0.9500 . ? C14 C16 1.530(9) . ? C14 C15 1.542(8) . ? C14 C17 1.542(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.532(9) . ? C18 C21 1.533(9) . ? C18 C19 1.543(9) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.505(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.386(9) . ? C23 C24 1.397(9) . ? C24 C25 1.420(9) . ? C25 C26 1.392(9) . ? C25 C29 1.525(10) . ? C26 C27 1.387(9) . ? C26 H26 0.9500 . ? C27 C28 1.380(9) . ? C27 C33 1.530(8) . ? C28 H28 0.9500 . ? C29 C31 1.503(12) . ? C29 C32 1.524(10) . ? C29 C30 1.577(13) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.531(9) . ? C33 C35 1.531(10) . ? C33 C34 1.532(10) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.526(8) . ? C37 C38 1.529(8) . ? C37 H37 1.0000 . ? C38 C39 1.492(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.525(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.526(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.531(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42 1.0000 . ? C43 C44 1.504(8) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C49 1.392(8) . ? C44 C45 1.403(8) . ? C45 C46 1.416(8) . ? C46 C47 1.394(9) . ? C46 C50 1.527(8) . ? C47 C48 1.397(9) . ? C47 H47 0.9500 . ? C48 C49 1.388(8) . ? C48 C54 1.529(9) . ? C49 H49 0.9500 . ? C50 C51 1.518(9) . ? C50 C52 1.533(9) . ? C50 C53 1.540(8) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C57 1.527(10) . ? C54 C55 1.531(9) . ? C54 C56 1.534(9) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.496(8) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C64 1.381(9) . ? C59 C60 1.406(8) . ? C60 C61 1.408(8) . ? C61 C62 1.390(8) . ? C61 C65 1.541(8) . ? C62 C63 1.400(8) . ? C62 H62 0.9500 . ? C63 C64 1.379(8) . ? C63 C69 1.545(8) . ? C64 H64 0.9500 . ? C65 C66 1.526(9) . ? C65 C67 1.540(9) . ? C65 C68 1.543(8) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C71 1.493(10) . ? C69 C70 1.506(9) . ? C69 C72 1.552(10) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.51(4) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C75 1.50(4) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 100.7(2) . . ? O1 Fe1 O3 97.61(14) . . ? O2 Fe1 O3 101.32(19) . . ? O1 Fe1 O4 170.13(17) . . ? O2 Fe1 O4 88.3(2) . . ? O3 Fe1 O4 76.38(13) . . ? O1 Fe1 N1 86.94(19) . . ? O2 Fe1 N1 164.22(19) . . ? O3 Fe1 N1 91.24(18) . . ? O4 Fe1 N1 85.38(18) . . ? O1 Fe1 N2 94.11(16) . . ? O2 Fe1 N2 88.0(2) . . ? O3 Fe1 N2 163.35(17) . . ? O4 Fe1 N2 90.30(15) . . ? N1 Fe1 N2 77.6(2) . . ? O5 Fe2 O6 101.23(18) . . ? O5 Fe2 O3 95.91(14) . . ? O6 Fe2 O3 101.33(17) . . ? O5 Fe2 O4 169.16(18) . . ? O6 Fe2 O4 88.39(18) . . ? O3 Fe2 O4 77.12(13) . . ? O5 Fe2 N4 89.37(15) . . ? O6 Fe2 N4 88.58(17) . . ? O3 Fe2 N4 167.59(17) . . ? O4 Fe2 N4 95.91(15) . . ? O5 Fe2 N3 86.48(18) . . ? O6 Fe2 N3 163.74(15) . . ? O3 Fe2 N3 91.98(18) . . ? O4 Fe2 N3 85.49(18) . . ? N4 Fe2 N3 77.11(18) . . ? C1 N1 C7 113.1(4) . . ? C1 N1 Fe1 113.9(4) . . ? C7 N1 Fe1 110.7(4) . . ? C1 N1 H1N 106.2 . . ? C7 N1 H1N 106.2 . . ? Fe1 N1 H1N 106.2 . . ? C22 N2 C6 114.8(5) . . ? C22 N2 Fe1 112.1(4) . . ? C6 N2 Fe1 109.4(3) . . ? C22 N2 H2N 106.7 . . ? C6 N2 H2N 106.7 . . ? Fe1 N2 H2N 106.7 . . ? C37 N3 C43 112.8(4) . . ? C37 N3 Fe2 112.2(4) . . ? C43 N3 Fe2 109.6(3) . . ? C37 N3 H3N 107.3 . . ? C43 N3 H3N 107.3 . . ? Fe2 N3 H3N 107.3 . . ? C42 N4 C58 116.9(4) . . ? C42 N4 Fe2 111.0(3) . . ? C58 N4 Fe2 111.2(3) . . ? C42 N4 H4N 105.6 . . ? C58 N4 H4N 105.6 . . ? Fe2 N4 H4N 105.6 . . ? C9 O1 Fe1 133.5(4) . . ? C24 O2 Fe1 125.9(4) . . ? Fe1 O3 Fe2 106.50(16) . . ? Fe2 O4 Fe1 99.98(15) . . ? C45 O5 Fe2 135.6(4) . . ? C60 O6 Fe2 124.9(4) . . ? N1 C1 C2 115.6(5) . . ? N1 C1 C6 109.1(5) . . ? C2 C1 C6 111.9(5) . . ? N1 C1 H1 106.6 . . ? C2 C1 H1 106.6 . . ? C6 C1 H1 106.6 . . ? C1 C2 C3 111.5(6) . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 111.4(6) . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 111.1(6) . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 112.3(5) . . ? C6 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? C6 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? N2 C6 C5 114.7(5) . . ? N2 C6 C1 107.0(5) . . ? C5 C6 C1 111.6(5) . . ? N2 C6 H6 107.7 . . ? C5 C6 H6 107.7 . . ? C1 C6 H6 107.7 . . ? N1 C7 C8 109.9(5) . . ? N1 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N1 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C13 C8 C9 121.4(5) . . ? C13 C8 C7 118.6(5) . . ? C9 C8 C7 120.0(5) . . ? O1 C9 C8 120.0(5) . . ? O1 C9 C10 121.0(5) . . ? C8 C9 C10 119.0(6) . . ? C11 C10 C9 117.3(5) . . ? C11 C10 C14 121.3(5) . . ? C9 C10 C14 121.3(5) . . ? C10 C11 C12 124.1(5) . . ? C10 C11 H11 118.0 . . ? C12 C11 H11 118.0 . . ? C13 C12 C11 117.2(5) . . ? C13 C12 C18 120.1(6) . . ? C11 C12 C18 122.7(5) . . ? C12 C13 C8 121.0(6) . . ? C12 C13 H13 119.5 . . ? C8 C13 H13 119.5 . . ? C10 C14 C16 109.2(5) . . ? C10 C14 C15 111.7(5) . . ? C16 C14 C15 110.1(5) . . ? C10 C14 C17 111.7(5) . . ? C16 C14 C17 107.5(5) . . ? C15 C14 C17 106.6(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C21 107.7(6) . . ? C20 C18 C12 110.6(5) . . ? C21 C18 C12 109.8(5) . . ? C20 C18 C19 109.1(6) . . ? C21 C18 C19 107.2(5) . . ? C12 C18 C19 112.4(6) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 C23 110.6(5) . . ? N2 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C28 C23 C24 119.7(6) . . ? C28 C23 C22 120.9(6) . . ? C24 C23 C22 119.4(6) . . ? O2 C24 C23 119.7(6) . . ? O2 C24 C25 121.0(6) . . ? C23 C24 C25 119.2(6) . . ? C26 C25 C24 117.7(6) . . ? C26 C25 C29 122.0(6) . . ? C24 C25 C29 120.4(6) . . ? C27 C26 C25 123.9(6) . . ? C27 C26 H26 118.1 . . ? C25 C26 H26 118.1 . . ? C28 C27 C26 116.4(6) . . ? C28 C27 C33 120.6(6) . . ? C26 C27 C33 123.0(6) . . ? C27 C28 C23 122.9(6) . . ? C27 C28 H28 118.5 . . ? C23 C28 H28 118.5 . . ? C31 C29 C32 108.3(8) . . ? C31 C29 C25 112.9(6) . . ? C32 C29 C25 111.6(6) . . ? C31 C29 C30 111.6(8) . . ? C32 C29 C30 106.0(7) . . ? C25 C29 C30 106.2(8) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 C36 112.2(5) . . ? C27 C33 C35 109.2(6) . . ? C36 C33 C35 108.0(6) . . ? C27 C33 C34 109.8(6) . . ? C36 C33 C34 107.3(6) . . ? C35 C33 C34 110.4(7) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 C42 109.6(5) . . ? N3 C37 C38 114.7(5) . . ? C42 C37 C38 111.1(5) . . ? N3 C37 H37 107.0 . . ? C42 C37 H37 107.0 . . ? C38 C37 H37 107.0 . . ? C39 C38 C37 110.8(6) . . ? C39 C38 H38A 109.5 . . ? C37 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? C38 C39 C40 111.2(6) . . ? C38 C39 H39A 109.4 . . ? C40 C39 H39A 109.4 . . ? C38 C39 H39B 109.4 . . ? C40 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C39 C40 C41 111.6(6) . . ? C39 C40 H40A 109.3 . . ? C41 C40 H40A 109.3 . . ? C39 C40 H40B 109.3 . . ? C41 C40 H40B 109.3 . . ? H40A C40 H40B 108.0 . . ? C40 C41 C42 111.8(5) . . ? C40 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? C40 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 107.9 . . ? N4 C42 C37 106.9(4) . . ? N4 C42 C41 113.8(5) . . ? C37 C42 C41 109.9(5) . . ? N4 C42 H42 108.7 . . ? C37 C42 H42 108.7 . . ? C41 C42 H42 108.7 . . ? N3 C43 C44 112.9(5) . . ? N3 C43 H43A 109.0 . . ? C44 C43 H43A 109.0 . . ? N3 C43 H43B 109.0 . . ? C44 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C49 C44 C45 120.7(5) . . ? C49 C44 C43 117.5(5) . . ? C45 C44 C43 121.6(5) . . ? O5 C45 C44 120.7(5) . . ? O5 C45 C46 120.4(5) . . ? C44 C45 C46 118.9(6) . . ? C47 C46 C45 117.5(6) . . ? C47 C46 C50 121.0(5) . . ? C45 C46 C50 121.5(6) . . ? C46 C47 C48 124.7(5) . . ? C46 C47 H47 117.7 . . ? C48 C47 H47 117.7 . . ? C49 C48 C47 116.0(6) . . ? C49 C48 C54 120.5(6) . . ? C47 C48 C54 123.5(5) . . ? C48 C49 C44 122.0(6) . . ? C48 C49 H49 119.0 . . ? C44 C49 H49 119.0 . . ? C51 C50 C46 110.2(5) . . ? C51 C50 C52 110.3(6) . . ? C46 C50 C52 108.5(5) . . ? C51 C50 C53 107.3(5) . . ? C46 C50 C53 112.5(5) . . ? C52 C50 C53 108.0(5) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C57 C54 C48 108.8(5) . . ? C57 C54 C55 109.1(6) . . ? C48 C54 C55 112.0(6) . . ? C57 C54 C56 108.6(6) . . ? C48 C54 C56 110.0(5) . . ? C55 C54 C56 108.4(6) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N4 C58 C59 111.1(5) . . ? N4 C58 H58A 109.4 . . ? C59 C58 H58A 109.4 . . ? N4 C58 H58B 109.4 . . ? C59 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? C64 C59 C60 120.1(5) . . ? C64 C59 C58 121.6(5) . . ? C60 C59 C58 118.3(6) . . ? O6 C60 C59 119.0(5) . . ? O6 C60 C61 122.2(5) . . ? C59 C60 C61 118.8(6) . . ? C62 C61 C60 118.3(5) . . ? C62 C61 C65 120.5(5) . . ? C60 C61 C65 121.0(5) . . ? C61 C62 C63 123.4(6) . . ? C61 C62 H62 118.3 . . ? C63 C62 H62 118.3 . . ? C64 C63 C62 116.4(5) . . ? C64 C63 C69 123.8(5) . . ? C62 C63 C69 119.8(5) . . ? C63 C64 C59 122.6(5) . . ? C63 C64 H64 118.7 . . ? C59 C64 H64 118.7 . . ? C66 C65 C67 109.9(5) . . ? C66 C65 C61 111.7(5) . . ? C67 C65 C61 107.5(5) . . ? C66 C65 C68 108.0(5) . . ? C67 C65 C68 106.8(5) . . ? C61 C65 C68 112.7(5) . . ? 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 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C71 C69 C70 111.1(6) . . ? C71 C69 C63 110.1(5) . . ? C70 C69 C63 113.0(5) . . ? C71 C69 C72 107.2(7) . . ? C70 C69 C72 106.3(6) . . ? C63 C69 C72 108.9(5) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C69 C72 H72A 109.5 . . ? C69 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C69 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 H73A 109.5 . . ? C74 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C74 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? O7 C74 C75 125(3) . . ? O7 C74 C73 116(3) . . ? C75 C74 C73 120(3) . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.878 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.086 # Attachment '8252_web_deposit_cif_file_1_KenjiMatsumoto_1321546181.complex4_[(L2)Fe1(OH)2Fe(L2)]_KM187_final.cif' data_aSR_diPh_NpNp_FeNHsalan_OH2_KM187 _database_code_depnum_ccdc_archive 'CCDC 854408' #TrackingRef '8252_web_deposit_cif_file_1_KenjiMatsumoto_1321546181.complex4_[(L2)Fe1(OH)2Fe(L2)]_KM187_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C112H86Fe2N4O6, 2(H2O), CH2Cl2' _chemical_formula_sum 'C113 H92 Cl2 Fe2 N4 O8' _chemical_formula_weight 1816.51 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.5225(14) _cell_length_b 25.289(3) _cell_length_c 15.7743(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.270(2) _cell_angle_gamma 90.00 _cell_volume 4974.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9952 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 25.51 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 0.403 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8886 _exptl_absorpt_correction_T_max 0.9880 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 'focusing mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 57214 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 22598 _reflns_number_gt 17541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1764P)^2^+8.7158P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(19) _refine_ls_number_reflns 22598 _refine_ls_number_parameters 1160 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0889 _refine_ls_wR_factor_ref 0.2713 _refine_ls_wR_factor_gt 0.2473 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.71717(6) 0.18631(3) 0.47096(5) 0.02119(18) Uani 1 1 d . . . Fe2 Fe 0.62856(6) 0.13335(3) 0.30114(5) 0.02080(18) Uani 1 1 d . . . N1 N 0.6767(4) 0.11289(19) 0.5336(3) 0.0220(9) Uani 1 1 d . . . N2 N 0.6390(4) 0.21736(18) 0.5781(3) 0.0216(9) Uani 1 1 d . . . N3 N 0.6200(4) 0.2123(2) 0.2424(3) 0.0270(10) Uani 1 1 d . . . N4 N 0.4748(4) 0.1290(2) 0.2239(3) 0.0247(10) Uani 1 1 d . . . O1 O 0.8525(3) 0.18228(19) 0.5378(3) 0.0277(9) Uani 1 1 d . . . O2 O 0.7200(4) 0.25625(16) 0.4255(3) 0.0289(9) Uani 1 1 d . . . O3 O 0.7625(3) 0.14848(16) 0.3710(3) 0.0252(9) Uani 1 1 d . . . O4 O 0.5701(3) 0.17446(14) 0.3993(2) 0.0216(8) Uani 1 1 d . . . O5 O 0.6948(4) 0.11184(16) 0.2030(3) 0.0295(9) Uani 1 1 d . . . O6 O 0.5897(3) 0.06835(15) 0.3541(3) 0.0244(8) Uani 1 1 d . . . O1W O 0.9909(3) 0.1702(2) 0.2821(3) 0.0466(14) Uani 1 1 d . . . O2W O 0.9060(4) 0.5681(3) 0.7393(5) 0.071(2) Uani 1 1 d . . . C1 C 0.6423(4) 0.1233(2) 0.6201(3) 0.0197(10) Uani 1 1 d . . . H1 H 0.7084 0.1297 0.6593 0.024 Uiso 1 1 calc R . . C2 C 0.5841(4) 0.0764(2) 0.6548(4) 0.0231(11) Uani 1 1 d . . . C3 C 0.6156(6) 0.0579(3) 0.7360(4) 0.0350(14) Uani 1 1 d . . . H3 H 0.6750 0.0738 0.7681 0.042 Uiso 1 1 calc R . . C4 C 0.5606(7) 0.0158(3) 0.7713(5) 0.0468(18) Uani 1 1 d . . . H4 H 0.5816 0.0036 0.8273 0.056 Uiso 1 1 calc R . . C5 C 0.4755(6) -0.0074(3) 0.7230(5) 0.0409(16) Uani 1 1 d . . . H5 H 0.4375 -0.0357 0.7459 0.049 Uiso 1 1 calc R . . C6 C 0.4449(6) 0.0108(3) 0.6401(6) 0.0445(18) Uani 1 1 d . . . H6 H 0.3871 -0.0056 0.6069 0.053 Uiso 1 1 calc R . . C7 C 0.4981(5) 0.0520(3) 0.6074(5) 0.0354(15) Uani 1 1 d . . . H7 H 0.4763 0.0643 0.5515 0.043 Uiso 1 1 calc R . . C8 C 0.7666(5) 0.0741(2) 0.5337(4) 0.0284(13) Uani 1 1 d . . . H8A H 0.7832 0.0682 0.4743 0.034 Uiso 1 1 calc R . . H8B H 0.7429 0.0400 0.5563 0.034 Uiso 1 1 calc R . . C9 C 0.8674(5) 0.0916(3) 0.5858(4) 0.0292(13) Uani 1 1 d . . . C10 C 0.9052(5) 0.1453(2) 0.5834(4) 0.0284(13) Uani 1 1 d . . . C11 C 1.0003(5) 0.1599(3) 0.6329(4) 0.0301(13) Uani 1 1 d . . . C12 C 1.0613(5) 0.1194(3) 0.6812(4) 0.0345(14) Uani 1 1 d . . . C13 C 1.1596(5) 0.1299(4) 0.7302(4) 0.0408(15) Uani 1 1 d . . . H13 H 1.1846 0.1653 0.7351 0.049 Uiso 1 1 calc R . . C14 C 1.2183(6) 0.0914(4) 0.7698(6) 0.052(2) Uani 1 1 d . . . H14 H 1.2853 0.0997 0.8001 0.063 Uiso 1 1 calc R . . C15 C 1.1809(7) 0.0382(4) 0.7668(6) 0.059(2) Uani 1 1 d . . . H15 H 1.2222 0.0109 0.7954 0.071 Uiso 1 1 calc R . . C16 C 1.0863(6) 0.0270(3) 0.7230(5) 0.0423(17) Uani 1 1 d . . . H16 H 1.0603 -0.0083 0.7218 0.051 Uiso 1 1 calc R . . C17 C 1.0257(5) 0.0664(3) 0.6792(4) 0.0326(14) Uani 1 1 d . . . C18 C 0.9256(5) 0.0548(3) 0.6327(4) 0.0328(14) Uani 1 1 d . . . H18 H 0.8984 0.0198 0.6344 0.039 Uiso 1 1 calc R . . C19 C 1.0387(5) 0.2157(3) 0.6298(4) 0.0355(15) Uani 1 1 d . . . C20 C 1.1403(6) 0.2249(4) 0.6009(5) 0.0434(18) Uani 1 1 d . . . H20 H 1.1815 0.1957 0.5844 0.052 Uiso 1 1 calc R . . C21 C 1.1819(7) 0.2763(4) 0.5959(5) 0.058(3) Uani 1 1 d . . . H21 H 1.2493 0.2818 0.5742 0.070 Uiso 1 1 calc R . . C22 C 1.1225(7) 0.3203(4) 0.6234(6) 0.055(2) Uani 1 1 d . . . H22 H 1.1506 0.3551 0.6215 0.066 Uiso 1 1 calc R . . C23 C 1.0234(6) 0.3114(3) 0.6529(5) 0.0418(17) Uani 1 1 d . . . C24 C 0.9627(7) 0.3544(3) 0.6798(5) 0.051(2) Uani 1 1 d . . . H24 H 0.9899 0.3892 0.6743 0.061 Uiso 1 1 calc R . . C25 C 0.8650(7) 0.3481(3) 0.7140(6) 0.0506(19) Uani 1 1 d . . . H25 H 0.8256 0.3776 0.7317 0.061 Uiso 1 1 calc R . . C26 C 0.8275(6) 0.2967(3) 0.7211(5) 0.0370(15) Uani 1 1 d . . . H26 H 0.7622 0.2912 0.7461 0.044 Uiso 1 1 calc R . . C27 C 0.8825(5) 0.2531(3) 0.6930(4) 0.0308(13) Uani 1 1 d . . . H27 H 0.8527 0.2188 0.6977 0.037 Uiso 1 1 calc R . . C28 C 0.9802(5) 0.2587(3) 0.6580(4) 0.0350(14) Uani 1 1 d . . . C29 C 0.5752(4) 0.1744(2) 0.6166(4) 0.0194(10) Uani 1 1 d . . . H29 H 0.5089 0.1681 0.5775 0.023 Uiso 1 1 calc R . . C30 C 0.5411(4) 0.1877(2) 0.7036(3) 0.0204(10) Uani 1 1 d . . . C31 C 0.4334(4) 0.1906(2) 0.7171(4) 0.0250(11) Uani 1 1 d . . . H31 H 0.3804 0.1858 0.6707 0.030 Uiso 1 1 calc R . . C32 C 0.4022(5) 0.2004(2) 0.7982(4) 0.0291(13) Uani 1 1 d . . . H32 H 0.3282 0.2019 0.8067 0.035 Uiso 1 1 calc R . . C33 C 0.4784(6) 0.2080(3) 0.8664(4) 0.0323(13) Uani 1 1 d . . . H33 H 0.4570 0.2148 0.9216 0.039 Uiso 1 1 calc R . . C34 C 0.5861(5) 0.2054(2) 0.8532(4) 0.0284(12) Uani 1 1 d . . . H34 H 0.6388 0.2106 0.8998 0.034 Uiso 1 1 calc R . . C35 C 0.6181(5) 0.1955(2) 0.7729(4) 0.0252(12) Uani 1 1 d . . . H35 H 0.6923 0.1940 0.7648 0.030 Uiso 1 1 calc R . . C36 C 0.5733(5) 0.2651(2) 0.5545(4) 0.0277(12) Uani 1 1 d . . . H36A H 0.5337 0.2759 0.6032 0.033 Uiso 1 1 calc R . . H36B H 0.5201 0.2566 0.5060 0.033 Uiso 1 1 calc R . . C37 C 0.6434(4) 0.3102(2) 0.5302(4) 0.0226(11) Uani 1 1 d . . . C38 C 0.7136(5) 0.3030(2) 0.4635(4) 0.0263(12) Uani 1 1 d . . . C39 C 0.7761(5) 0.3453(2) 0.4390(4) 0.0243(11) Uani 1 1 d . . . C40 C 0.7673(5) 0.3954(2) 0.4767(4) 0.0249(12) Uani 1 1 d . . . C41 C 0.8249(5) 0.4407(2) 0.4516(4) 0.0291(13) Uani 1 1 d . . . H41 H 0.8697 0.4376 0.4064 0.035 Uiso 1 1 calc R . . C42 C 0.8171(5) 0.4886(2) 0.4912(5) 0.0326(14) Uani 1 1 d . . . H42 H 0.8577 0.5178 0.4741 0.039 Uiso 1 1 calc R . . C43 C 0.7494(6) 0.4950(2) 0.5569(4) 0.0336(14) Uani 1 1 d . . . H43 H 0.7435 0.5284 0.5836 0.040 Uiso 1 1 calc R . . C44 C 0.6916(5) 0.4524(2) 0.5821(4) 0.0320(13) Uani 1 1 d . . . H44 H 0.6466 0.4566 0.6270 0.038 Uiso 1 1 calc R . . C45 C 0.6982(5) 0.4030(2) 0.5428(4) 0.0252(12) Uani 1 1 d . . . C46 C 0.6375(5) 0.3585(2) 0.5677(4) 0.0275(12) Uani 1 1 d . . . H46 H 0.5916 0.3629 0.6119 0.033 Uiso 1 1 calc R . . C47 C 0.8549(5) 0.3350(2) 0.3751(4) 0.0252(12) Uani 1 1 d . . . C48 C 0.9502(6) 0.3111(3) 0.4007(5) 0.0386(15) Uani 1 1 d . . . H48 H 0.9642 0.3007 0.4585 0.046 Uiso 1 1 calc R . . C49 C 1.0295(6) 0.3012(4) 0.3431(6) 0.051(2) Uani 1 1 d . . . H49 H 1.0954 0.2846 0.3623 0.061 Uiso 1 1 calc R . . C50 C 1.0092(7) 0.3159(3) 0.2609(6) 0.055(2) Uani 1 1 d . . . H50 H 1.0622 0.3102 0.2226 0.066 Uiso 1 1 calc R . . C51 C 0.9100(6) 0.3398(3) 0.2304(5) 0.0436(17) Uani 1 1 d . . . C52 C 0.8871(9) 0.3534(4) 0.1423(5) 0.060(3) Uani 1 1 d . . . H52 H 0.9388 0.3467 0.1031 0.072 Uiso 1 1 calc R . . C53 C 0.7897(10) 0.3762(4) 0.1143(5) 0.064(3) Uani 1 1 d . . . H53 H 0.7759 0.3859 0.0562 0.077 Uiso 1 1 calc R . . C54 C 0.7106(8) 0.3853(3) 0.1708(5) 0.050(2) Uani 1 1 d . . . H54 H 0.6427 0.3994 0.1507 0.060 Uiso 1 1 calc R . . C55 C 0.7342(6) 0.3731(3) 0.2569(4) 0.0365(15) Uani 1 1 d . . . H55 H 0.6825 0.3809 0.2956 0.044 Uiso 1 1 calc R . . C56 C 0.8317(6) 0.3497(2) 0.2882(4) 0.0327(14) Uani 1 1 d . . . C57 C 0.5250(6) 0.2174(2) 0.1793(4) 0.0305(13) Uani 1 1 d . . . H57 H 0.5445 0.2021 0.1243 0.037 Uiso 1 1 calc R . . C58 C 0.4924(6) 0.2737(3) 0.1629(4) 0.0364(15) Uani 1 1 d . . . C59 C 0.4910(12) 0.2912(3) 0.0782(6) 0.089(4) Uani 1 1 d . . . H59 H 0.5142 0.2685 0.0355 0.107 Uiso 1 1 calc R . . C60 C 0.4550(16) 0.3425(4) 0.0575(8) 0.119(6) Uani 1 1 d . . . H60 H 0.4535 0.3550 0.0006 0.142 Uiso 1 1 calc R . . C61 C 0.4206(14) 0.3758(4) 0.1233(9) 0.118(7) Uani 1 1 d . . . H61 H 0.3929 0.4100 0.1092 0.142 Uiso 1 1 calc R . . C62 C 0.4273(9) 0.3585(4) 0.2087(7) 0.066(3) Uani 1 1 d . . . H62 H 0.4060 0.3806 0.2529 0.080 Uiso 1 1 calc R . . C63 C 0.4666(7) 0.3071(3) 0.2258(5) 0.0448(18) Uani 1 1 d . . . H63 H 0.4755 0.2952 0.2831 0.054 Uiso 1 1 calc R . . C64 C 0.7222(6) 0.2270(2) 0.2074(4) 0.0315(13) Uani 1 1 d . . . H64A H 0.7804 0.2265 0.2543 0.038 Uiso 1 1 calc R . . H64B H 0.7159 0.2637 0.1856 0.038 Uiso 1 1 calc R . . C65 C 0.7533(5) 0.1912(3) 0.1365(4) 0.0298(12) Uani 1 1 d . . . C66 C 0.7369(4) 0.1358(3) 0.1390(3) 0.0253(11) Uani 1 1 d . . . C67 C 0.7623(5) 0.1042(2) 0.0706(4) 0.0266(12) Uani 1 1 d . . . C68 C 0.8118(5) 0.1272(3) 0.0017(4) 0.0302(13) Uani 1 1 d . . . C69 C 0.8429(6) 0.0958(3) -0.0675(4) 0.0395(16) Uani 1 1 d . . . H69 H 0.8284 0.0590 -0.0697 0.047 Uiso 1 1 calc R . . C70 C 0.8941(6) 0.1197(4) -0.1308(4) 0.0466(19) Uani 1 1 d . . . H70 H 0.9158 0.0987 -0.1761 0.056 Uiso 1 1 calc R . . C71 C 0.9153(5) 0.1739(3) -0.1307(4) 0.0424(18) Uani 1 1 d . . . H71 H 0.9516 0.1892 -0.1749 0.051 Uiso 1 1 calc R . . C72 C 0.8835(5) 0.2046(3) -0.0667(5) 0.0392(16) Uani 1 1 d . . . H72 H 0.8963 0.2416 -0.0680 0.047 Uiso 1 1 calc R . . C73 C 0.8322(5) 0.1832(3) 0.0015(4) 0.0326(13) Uani 1 1 d . . . C74 C 0.7982(5) 0.2136(3) 0.0690(4) 0.0290(13) Uani 1 1 d . . . H74 H 0.8068 0.2509 0.0677 0.035 Uiso 1 1 calc R . . C75 C 0.7272(5) 0.0483(2) 0.0706(4) 0.0287(12) Uani 1 1 d . . . C76 C 0.7860(6) 0.0093(3) 0.1109(5) 0.0389(16) Uani 1 1 d . . . H76 H 0.8569 0.0170 0.1344 0.047 Uiso 1 1 calc R . . C77 C 0.7463(8) -0.0417(3) 0.1192(5) 0.050(2) Uani 1 1 d . . . H77 H 0.7904 -0.0678 0.1481 0.060 Uiso 1 1 calc R . . C78 C 0.6451(8) -0.0547(3) 0.0863(5) 0.052(2) Uani 1 1 d . . . H78 H 0.6183 -0.0894 0.0934 0.063 Uiso 1 1 calc R . . C79 C 0.5800(7) -0.0158(3) 0.0414(4) 0.0389(16) Uani 1 1 d . . . C80 C 0.4721(8) -0.0254(4) 0.0052(5) 0.055(2) Uani 1 1 d . . . H80 H 0.4422 -0.0595 0.0116 0.066 Uiso 1 1 calc R . . C81 C 0.4124(6) 0.0112(4) -0.0367(6) 0.0493(19) Uani 1 1 d . . . H81 H 0.3416 0.0030 -0.0597 0.059 Uiso 1 1 calc R . . C82 C 0.4536(7) 0.0612(4) -0.0468(6) 0.053(2) Uani 1 1 d . . . H82 H 0.4109 0.0870 -0.0779 0.064 Uiso 1 1 calc R . . C83 C 0.5561(6) 0.0746(3) -0.0125(5) 0.0380(15) Uani 1 1 d . . . H83 H 0.5822 0.1095 -0.0191 0.046 Uiso 1 1 calc R . . C84 C 0.6221(5) 0.0361(3) 0.0325(4) 0.0287(12) Uani 1 1 d . . . C85 C 0.4329(5) 0.1840(2) 0.2094(4) 0.0259(11) Uani 1 1 d . . . H85 H 0.4145 0.1984 0.2652 0.031 Uiso 1 1 calc R . . C86 C 0.3321(5) 0.1855(3) 0.1476(4) 0.0320(13) Uani 1 1 d . . . C87 C 0.2383(7) 0.2096(3) 0.1684(5) 0.0492(19) Uani 1 1 d . . . H87 H 0.2361 0.2260 0.2223 0.059 Uiso 1 1 calc R . . C88 C 0.1462(8) 0.2096(4) 0.1097(7) 0.068(3) Uani 1 1 d . . . H88 H 0.0833 0.2275 0.1232 0.081 Uiso 1 1 calc R . . C89 C 0.1474(7) 0.1845(5) 0.0348(6) 0.063(3) Uani 1 1 d . . . H89 H 0.0842 0.1834 -0.0034 0.076 Uiso 1 1 calc R . . C90 C 0.2396(8) 0.1603(5) 0.0127(6) 0.065(3) Uani 1 1 d . . . H90 H 0.2395 0.1428 -0.0406 0.078 Uiso 1 1 calc R . . C91 C 0.3330(6) 0.1613(3) 0.0682(4) 0.0438(17) Uani 1 1 d . . . H91 H 0.3970 0.1456 0.0520 0.053 Uiso 1 1 calc R . . C92 C 0.3975(5) 0.0920(2) 0.2585(4) 0.0272(12) Uani 1 1 d . . . H92A H 0.3286 0.0927 0.2222 0.033 Uiso 1 1 calc R . . H92B H 0.3835 0.1031 0.3167 0.033 Uiso 1 1 calc R . . C93 C 0.4434(4) 0.0365(2) 0.2609(4) 0.0237(11) Uani 1 1 d . . . C94 C 0.5421(5) 0.0274(2) 0.3124(4) 0.0238(11) Uani 1 1 d . . . C95 C 0.5852(5) -0.0229(2) 0.3175(4) 0.0245(12) Uani 1 1 d . . . C96 C 0.5319(5) -0.0653(2) 0.2730(4) 0.0263(12) Uani 1 1 d . . . C97 C 0.5753(6) -0.1180(2) 0.2743(4) 0.0309(13) Uani 1 1 d . . . H97 H 0.6417 -0.1249 0.3064 0.037 Uiso 1 1 calc R . . C98 C 0.5232(6) -0.1582(3) 0.2305(5) 0.0391(16) Uani 1 1 d . . . H98 H 0.5526 -0.1928 0.2335 0.047 Uiso 1 1 calc R . . C99 C 0.4255(6) -0.1485(3) 0.1805(4) 0.0364(15) Uani 1 1 d . . . H99 H 0.3902 -0.1766 0.1492 0.044 Uiso 1 1 calc R . . C100 C 0.3812(5) -0.0986(3) 0.1771(4) 0.0326(14) Uani 1 1 d . . . H100 H 0.3147 -0.0926 0.1445 0.039 Uiso 1 1 calc R . . C101 C 0.4343(5) -0.0560(2) 0.2221(4) 0.0292(13) Uani 1 1 d . . . C102 C 0.3917(5) -0.0043(2) 0.2169(4) 0.0291(13) Uani 1 1 d . . . H102 H 0.3266 0.0023 0.1827 0.035 Uiso 1 1 calc R . . C103 C 0.6918(4) -0.0304(2) 0.3682(4) 0.0265(12) Uani 1 1 d . . . C104 C 0.7824(5) -0.0088(3) 0.3382(4) 0.0327(14) Uani 1 1 d . . . H104 H 0.7761 0.0104 0.2862 0.039 Uiso 1 1 calc R . . C105 C 0.8830(6) -0.0149(3) 0.3832(5) 0.0409(17) Uani 1 1 d . . . H105 H 0.9441 0.0006 0.3615 0.049 Uiso 1 1 calc R . . C106 C 0.8952(5) -0.0421(3) 0.4565(5) 0.0404(17) Uani 1 1 d . . . H106 H 0.9648 -0.0466 0.4849 0.048 Uiso 1 1 calc R . . C107 C 0.8054(5) -0.0642(2) 0.4919(5) 0.0337(14) Uani 1 1 d . . . C108 C 0.8154(6) -0.0927(3) 0.5688(5) 0.047(2) Uani 1 1 d . . . H108 H 0.8843 -0.0977 0.5984 0.057 Uiso 1 1 calc R . . C109 C 0.7255(8) -0.1135(3) 0.6018(6) 0.055(2) Uani 1 1 d . . . H109 H 0.7327 -0.1326 0.6539 0.067 Uiso 1 1 calc R . . C110 C 0.6250(6) -0.1063(3) 0.5586(5) 0.0445(17) Uani 1 1 d . . . H110 H 0.5640 -0.1208 0.5816 0.053 Uiso 1 1 calc R . . C111 C 0.6114(5) -0.0790(2) 0.4842(4) 0.0311(13) Uani 1 1 d . . . H111 H 0.5413 -0.0740 0.4568 0.037 Uiso 1 1 calc R . . C112 C 0.7006(5) -0.0580(2) 0.4471(4) 0.0280(13) Uani 1 1 d . . . C1A C 0.7684(10) 0.6787(5) 0.5922(8) 0.030(3) Uiso 0.486(5) 1 d P B 1 C1B C 0.9066(19) 0.7958(10) 0.1209(15) 0.075(6) Uiso 0.514(5) 1 d P B 2 Cl1A Cl 0.6946(2) 0.63633(14) 0.5218(2) 0.0337(8) Uiso 0.486(5) 1 d P B 1 Cl2A Cl 0.6918(2) 0.74284(13) 0.5941(2) 0.0325(8) Uiso 0.486(5) 1 d P B 1 Cl1B Cl 0.7723(4) 0.8077(2) 0.1458(3) 0.0675(13) Uiso 0.514(5) 1 d P B 2 Cl2B Cl 0.9515(7) 0.8358(3) 0.0622(5) 0.109(2) Uiso 0.514(5) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0250(4) 0.0180(4) 0.0200(4) -0.0017(3) -0.0006(3) -0.0030(3) Fe2 0.0267(4) 0.0159(3) 0.0196(4) -0.0021(3) 0.0009(3) -0.0019(3) N1 0.024(2) 0.022(2) 0.019(2) -0.0030(18) -0.0021(18) -0.0004(18) N2 0.024(2) 0.018(2) 0.022(2) 0.0026(18) 0.0029(18) -0.0046(18) N3 0.037(3) 0.024(2) 0.019(2) -0.0007(19) 0.000(2) -0.008(2) N4 0.035(3) 0.015(2) 0.023(2) 0.0012(19) 0.0004(19) -0.002(2) O1 0.0223(19) 0.035(2) 0.025(2) -0.0005(19) -0.0037(15) -0.0055(18) O2 0.046(3) 0.019(2) 0.023(2) -0.0010(16) 0.0069(18) -0.0058(17) O3 0.0221(19) 0.028(2) 0.025(2) -0.0069(16) 0.0013(16) -0.0002(15) O4 0.029(2) 0.016(2) 0.0196(18) -0.0011(14) -0.0014(15) 0.0015(14) O5 0.043(2) 0.0195(19) 0.027(2) -0.0016(17) 0.0101(18) -0.0033(17) O6 0.034(2) 0.0150(18) 0.024(2) 0.0002(15) -0.0028(16) -0.0045(16) O1W 0.018(2) 0.080(4) 0.043(3) -0.025(3) 0.0066(19) -0.012(2) O2W 0.020(2) 0.075(4) 0.121(6) -0.040(4) 0.020(3) -0.009(3) C1 0.021(2) 0.014(3) 0.024(3) 0.002(2) -0.0045(19) -0.0006(18) C2 0.024(3) 0.015(2) 0.029(3) 0.000(2) 0.000(2) 0.001(2) C3 0.045(4) 0.023(3) 0.037(4) 0.001(3) 0.003(3) -0.005(3) C4 0.069(5) 0.027(3) 0.047(4) 0.014(3) 0.019(4) -0.003(3) C5 0.043(4) 0.025(3) 0.055(4) 0.007(3) 0.011(3) -0.006(3) C6 0.040(4) 0.031(4) 0.061(5) 0.007(3) -0.002(3) -0.009(3) C7 0.031(3) 0.028(3) 0.046(4) 0.007(3) -0.005(3) -0.007(2) C8 0.030(3) 0.022(3) 0.034(3) -0.009(2) 0.002(2) 0.003(2) C9 0.027(3) 0.035(3) 0.026(3) -0.007(3) 0.001(2) 0.006(2) C10 0.026(3) 0.033(3) 0.026(3) -0.001(2) 0.001(2) 0.001(2) C11 0.023(3) 0.042(4) 0.025(3) -0.001(3) -0.001(2) -0.002(2) C12 0.027(3) 0.050(4) 0.027(3) -0.007(3) 0.007(2) -0.002(3) C13 0.027(3) 0.057(4) 0.036(3) 0.000(3) -0.008(3) -0.003(3) C14 0.033(4) 0.062(5) 0.057(5) -0.014(4) -0.020(3) 0.009(3) C15 0.050(5) 0.066(6) 0.056(5) -0.008(4) -0.022(4) 0.031(4) C16 0.042(4) 0.041(4) 0.044(4) -0.013(3) -0.001(3) 0.015(3) C17 0.028(3) 0.043(4) 0.026(3) -0.010(3) -0.002(2) 0.007(3) C18 0.032(3) 0.031(3) 0.034(3) -0.009(3) -0.001(3) 0.005(2) C19 0.030(3) 0.047(4) 0.027(3) 0.004(3) -0.010(3) -0.015(3) C20 0.030(3) 0.063(5) 0.038(4) 0.004(3) 0.005(3) -0.012(3) C21 0.045(4) 0.088(7) 0.041(4) 0.012(4) 0.002(3) -0.036(5) C22 0.052(5) 0.057(5) 0.053(5) 0.017(4) -0.006(4) -0.021(4) C23 0.047(4) 0.040(4) 0.035(4) 0.008(3) -0.010(3) -0.014(3) C24 0.065(5) 0.028(4) 0.054(5) 0.014(3) -0.023(4) -0.012(3) C25 0.055(5) 0.033(4) 0.061(5) 0.001(4) -0.006(4) 0.000(3) C26 0.037(3) 0.030(3) 0.042(4) -0.001(3) -0.005(3) -0.002(3) C27 0.034(3) 0.030(3) 0.027(3) 0.001(2) -0.006(2) -0.008(2) C28 0.036(3) 0.034(3) 0.033(3) 0.004(3) -0.009(3) -0.006(3) C29 0.018(2) 0.015(3) 0.024(3) 0.0016(19) -0.0016(19) -0.0017(18) C30 0.025(2) 0.012(2) 0.023(2) 0.001(2) 0.0002(19) 0.000(2) C31 0.026(3) 0.023(3) 0.026(3) -0.001(2) -0.003(2) -0.004(2) C32 0.025(3) 0.033(3) 0.029(3) -0.008(2) 0.003(2) -0.006(2) C33 0.046(4) 0.027(3) 0.025(3) -0.002(2) 0.010(3) -0.007(3) C34 0.040(3) 0.023(3) 0.022(3) -0.004(2) -0.003(2) -0.004(2) C35 0.023(3) 0.023(3) 0.029(3) 0.001(2) 0.000(2) -0.003(2) C36 0.037(3) 0.021(3) 0.024(3) 0.008(2) 0.001(2) 0.002(2) C37 0.025(3) 0.019(3) 0.023(3) 0.001(2) 0.001(2) -0.001(2) C38 0.036(3) 0.021(3) 0.020(3) -0.002(2) -0.006(2) -0.002(2) C39 0.031(3) 0.020(3) 0.021(3) 0.002(2) -0.004(2) -0.002(2) C40 0.025(3) 0.019(3) 0.029(3) 0.002(2) -0.001(2) -0.002(2) C41 0.033(3) 0.018(3) 0.035(3) -0.002(2) -0.004(3) -0.005(2) C42 0.029(3) 0.021(3) 0.048(4) 0.000(3) 0.007(3) -0.003(2) C43 0.045(4) 0.020(3) 0.036(3) -0.006(2) 0.002(3) -0.001(3) C44 0.039(3) 0.024(3) 0.033(3) 0.005(2) 0.001(3) 0.000(2) C45 0.026(3) 0.023(3) 0.026(3) 0.004(2) -0.002(2) 0.002(2) C46 0.036(3) 0.023(3) 0.023(3) 0.003(2) -0.003(2) 0.005(2) C47 0.032(3) 0.018(3) 0.026(3) -0.005(2) 0.006(2) -0.006(2) C48 0.039(4) 0.038(4) 0.039(4) -0.013(3) 0.005(3) -0.003(3) C49 0.031(4) 0.058(5) 0.063(5) -0.018(4) 0.010(3) -0.014(3) C50 0.055(5) 0.048(5) 0.068(6) -0.029(4) 0.036(4) -0.023(4) C51 0.051(4) 0.036(4) 0.047(4) -0.013(3) 0.019(3) -0.015(3) C52 0.102(7) 0.049(5) 0.035(4) -0.010(4) 0.038(5) -0.028(5) C53 0.129(9) 0.041(5) 0.024(4) 0.007(3) 0.014(5) -0.002(5) C54 0.089(6) 0.032(4) 0.027(4) 0.003(3) 0.007(4) 0.003(4) C55 0.064(5) 0.023(3) 0.023(3) 0.001(2) 0.008(3) 0.001(3) C56 0.048(4) 0.024(3) 0.028(3) -0.004(2) 0.011(3) -0.015(3) C57 0.049(4) 0.022(3) 0.020(3) -0.003(2) -0.002(3) -0.004(3) C58 0.055(4) 0.023(3) 0.029(3) 0.004(3) -0.008(3) -0.009(3) C59 0.202(14) 0.020(4) 0.036(5) 0.007(3) -0.027(6) -0.001(6) C60 0.246(19) 0.037(5) 0.060(7) 0.013(5) -0.056(9) 0.006(8) C61 0.204(16) 0.022(4) 0.111(10) 0.024(5) -0.087(11) 0.007(6) C62 0.084(7) 0.032(4) 0.084(7) 0.007(4) 0.011(6) 0.004(4) C63 0.067(5) 0.025(3) 0.042(4) 0.007(3) 0.004(4) -0.002(3) C64 0.046(4) 0.024(3) 0.026(3) -0.005(2) 0.011(3) -0.012(3) C65 0.034(3) 0.027(3) 0.028(3) 0.002(3) 0.003(2) -0.001(3) C66 0.028(3) 0.026(3) 0.021(3) -0.001(2) -0.001(2) -0.003(2) C67 0.028(3) 0.026(3) 0.026(3) -0.001(2) 0.001(2) 0.006(2) C68 0.025(3) 0.038(3) 0.027(3) 0.001(3) -0.001(2) 0.002(2) C69 0.039(4) 0.051(4) 0.029(3) -0.001(3) 0.004(3) 0.010(3) C70 0.045(4) 0.072(6) 0.024(3) 0.001(3) 0.015(3) 0.014(4) C71 0.030(3) 0.070(6) 0.027(3) 0.016(3) 0.003(3) 0.009(3) C72 0.023(3) 0.056(4) 0.037(4) 0.010(3) -0.005(3) -0.001(3) C73 0.024(3) 0.047(4) 0.026(3) 0.004(3) -0.002(2) -0.003(3) C74 0.028(3) 0.033(3) 0.025(3) 0.000(2) -0.003(2) -0.007(2) C75 0.036(3) 0.027(3) 0.023(3) -0.008(2) 0.004(2) 0.005(2) C76 0.043(4) 0.031(3) 0.040(4) -0.011(3) -0.009(3) 0.011(3) C77 0.075(6) 0.031(4) 0.039(4) -0.008(3) -0.014(4) 0.011(4) C78 0.088(6) 0.028(4) 0.040(4) -0.012(3) 0.002(4) -0.009(4) C79 0.063(5) 0.033(3) 0.021(3) -0.005(3) 0.008(3) -0.002(3) C80 0.072(6) 0.063(5) 0.033(4) -0.014(4) 0.015(4) -0.031(5) C81 0.037(4) 0.057(5) 0.053(5) -0.003(4) -0.002(3) -0.010(3) C82 0.043(4) 0.065(5) 0.049(5) -0.013(4) -0.011(4) 0.005(4) C83 0.038(4) 0.040(4) 0.035(4) -0.004(3) -0.002(3) 0.004(3) C84 0.033(3) 0.034(3) 0.020(3) -0.006(2) 0.005(2) -0.001(2) C85 0.036(3) 0.017(2) 0.025(3) 0.000(2) 0.000(2) 0.005(2) C86 0.041(3) 0.023(3) 0.030(3) 0.005(3) -0.006(2) -0.001(3) C87 0.056(5) 0.047(4) 0.043(4) -0.003(3) -0.009(3) 0.016(4) C88 0.059(5) 0.069(6) 0.072(6) -0.005(5) -0.015(5) 0.033(5) C89 0.046(4) 0.088(7) 0.050(5) 0.000(5) -0.027(4) 0.022(5) C90 0.058(5) 0.094(7) 0.039(4) -0.021(5) -0.019(4) 0.015(5) C91 0.044(4) 0.060(5) 0.025(3) -0.005(3) -0.005(3) 0.010(3) C92 0.031(3) 0.021(3) 0.029(3) 0.001(2) -0.003(2) 0.003(2) C93 0.024(3) 0.017(3) 0.030(3) 0.001(2) 0.001(2) 0.002(2) C94 0.026(3) 0.017(3) 0.027(3) -0.002(2) 0.001(2) -0.005(2) C95 0.027(3) 0.021(3) 0.025(3) 0.001(2) 0.005(2) 0.001(2) C96 0.029(3) 0.018(3) 0.031(3) -0.001(2) 0.002(2) -0.004(2) C97 0.039(3) 0.024(3) 0.031(3) -0.003(2) 0.008(3) -0.003(2) C98 0.062(5) 0.016(3) 0.041(4) -0.006(3) 0.017(3) -0.005(3) C99 0.050(4) 0.025(3) 0.034(3) -0.009(3) -0.001(3) -0.009(3) C100 0.039(3) 0.030(3) 0.027(3) -0.002(3) -0.005(3) -0.014(3) C101 0.040(3) 0.019(3) 0.029(3) -0.002(2) 0.005(3) -0.006(2) C102 0.034(3) 0.024(3) 0.029(3) 0.006(2) -0.001(2) -0.004(2) C103 0.021(3) 0.016(2) 0.041(3) -0.010(2) -0.005(2) 0.004(2) C104 0.037(3) 0.027(3) 0.035(3) -0.010(3) 0.007(3) -0.001(2) C105 0.030(3) 0.032(3) 0.063(5) -0.016(3) 0.014(3) -0.002(3) C106 0.030(3) 0.030(3) 0.059(5) -0.017(3) -0.007(3) 0.007(3) C107 0.031(3) 0.023(3) 0.046(4) -0.011(3) -0.001(3) 0.009(2) C108 0.038(4) 0.037(4) 0.061(5) -0.005(3) -0.024(4) 0.015(3) C109 0.074(6) 0.041(4) 0.047(5) 0.007(4) -0.015(4) -0.002(4) C110 0.044(4) 0.043(4) 0.046(4) 0.009(3) 0.003(3) 0.002(3) C111 0.028(3) 0.026(3) 0.039(4) 0.003(3) -0.001(3) 0.000(2) C112 0.025(3) 0.018(3) 0.040(3) -0.008(2) -0.004(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.910(4) . ? Fe1 O1 1.914(4) . ? Fe1 O3 1.971(4) . ? Fe1 O4 2.092(4) . ? Fe1 N2 2.176(5) . ? Fe1 N1 2.185(5) . ? Fe2 O5 1.901(4) . ? Fe2 O6 1.927(4) . ? Fe2 O3 1.958(4) . ? Fe2 O4 2.055(4) . ? Fe2 N4 2.185(5) . ? Fe2 N3 2.199(5) . ? N1 C1 1.492(7) . ? N1 C8 1.493(7) . ? N2 C36 1.490(7) . ? N2 C29 1.508(7) . ? N3 C57 1.485(8) . ? N3 C64 1.486(8) . ? N4 C92 1.487(8) . ? N4 C85 1.496(7) . ? O1 C10 1.318(8) . ? O2 C38 1.332(7) . ? O5 C66 1.329(7) . ? O6 C94 1.337(7) . ? C1 C2 1.519(7) . ? C1 C29 1.541(7) . ? C1 H1 1.0000 . ? C2 C3 1.386(9) . ? C2 C7 1.397(8) . ? C3 C4 1.411(9) . ? C3 H3 0.9500 . ? C4 C5 1.383(11) . ? C4 H4 0.9500 . ? C5 C6 1.405(11) . ? C5 H5 0.9500 . ? C6 C7 1.363(10) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.508(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C18 1.358(9) . ? C9 C10 1.441(9) . ? C10 C11 1.413(8) . ? C11 C12 1.451(10) . ? C11 C19 1.493(9) . ? C12 C17 1.413(10) . ? C12 C13 1.417(9) . ? C13 C14 1.339(11) . ? C13 H13 0.9500 . ? C14 C15 1.425(14) . ? C14 H14 0.9500 . ? C15 C16 1.346(11) . ? C15 H15 0.9500 . ? C16 C17 1.395(10) . ? C16 H16 0.9500 . ? C17 C18 1.424(9) . ? C18 H18 0.9500 . ? C19 C28 1.405(11) . ? C19 C20 1.410(10) . ? C20 C21 1.406(12) . ? C20 H20 0.9500 . ? C21 C22 1.428(15) . ? C21 H21 0.9500 . ? C22 C23 1.384(12) . ? C22 H22 0.9500 . ? C23 C24 1.415(12) . ? C23 C28 1.444(9) . ? C24 C25 1.391(13) . ? C24 H24 0.9500 . ? C25 C26 1.388(10) . ? C25 H25 0.9500 . ? C26 C27 1.396(10) . ? C26 H26 0.9500 . ? C27 C28 1.395(10) . ? C27 H27 0.9500 . ? C29 C30 1.512(8) . ? C29 H29 1.0000 . ? C30 C31 1.387(8) . ? C30 C35 1.404(7) . ? C31 C32 1.393(8) . ? C31 H31 0.9500 . ? C32 C33 1.384(9) . ? C32 H32 0.9500 . ? C33 C34 1.385(9) . ? C33 H33 0.9500 . ? C34 C35 1.386(9) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.509(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C46 1.364(8) . ? C37 C38 1.442(8) . ? C38 C39 1.401(8) . ? C39 C40 1.407(8) . ? C39 C47 1.496(8) . ? C40 C45 1.429(9) . ? C40 C41 1.429(8) . ? C41 C42 1.371(9) . ? C41 H41 0.9500 . ? C42 C43 1.407(10) . ? C42 H42 0.9500 . ? C43 C44 1.376(9) . ? C43 H43 0.9500 . ? C44 C45 1.400(9) . ? C44 H44 0.9500 . ? C45 C46 1.433(9) . ? C46 H46 0.9500 . ? C47 C48 1.366(10) . ? C47 C56 1.424(9) . ? C48 C49 1.427(11) . ? C48 H48 0.9500 . ? C49 C50 1.351(13) . ? C49 H49 0.9500 . ? C50 C51 1.424(13) . ? C50 H50 0.9500 . ? C51 C56 1.421(10) . ? C51 C52 1.435(12) . ? C52 C53 1.384(16) . ? C52 H52 0.9500 . ? C53 C54 1.410(14) . ? C53 H53 0.9500 . ? C54 C55 1.398(10) . ? C54 H54 0.9500 . ? C55 C56 1.405(10) . ? C55 H55 0.9500 . ? C57 C58 1.495(9) . ? C57 C85 1.540(9) . ? C57 H57 1.0000 . ? C58 C63 1.364(11) . ? C58 C59 1.406(11) . ? C59 C60 1.403(14) . ? C59 H59 0.9500 . ? C60 C61 1.43(2) . ? C60 H60 0.9500 . ? C61 C62 1.413(18) . ? C61 H61 0.9500 . ? C62 C63 1.408(11) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 C65 1.518(9) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C74 1.371(9) . ? C65 C66 1.416(9) . ? C66 C67 1.402(8) . ? C67 C68 1.424(9) . ? C67 C75 1.479(9) . ? C68 C69 1.432(10) . ? C68 C73 1.439(10) . ? C69 C70 1.375(11) . ? C69 H69 0.9500 . ? C70 C71 1.394(13) . ? C70 H70 0.9500 . ? C71 C72 1.363(11) . ? C71 H71 0.9500 . ? C72 C73 1.411(9) . ? C72 H72 0.9500 . ? C73 C74 1.410(9) . ? C74 H74 0.9500 . ? C75 C76 1.355(9) . ? C75 C84 1.429(9) . ? C76 C77 1.392(11) . ? C76 H76 0.9500 . ? C77 C78 1.365(13) . ? C77 H77 0.9500 . ? C78 C79 1.424(12) . ? C78 H78 0.9500 . ? C79 C84 1.425(10) . ? C79 C80 1.439(12) . ? C80 C81 1.327(13) . ? C80 H80 0.9500 . ? C81 C82 1.380(13) . ? C81 H81 0.9500 . ? C82 C83 1.388(11) . ? C82 H82 0.9500 . ? C83 C84 1.424(9) . ? C83 H83 0.9500 . ? C85 C86 1.522(8) . ? C85 H85 1.0000 . ? C86 C87 1.388(11) . ? C86 C91 1.395(10) . ? C87 C88 1.410(12) . ? C87 H87 0.9500 . ? C88 C89 1.344(14) . ? C88 H88 0.9500 . ? C89 C90 1.379(13) . ? C89 H89 0.9500 . ? C90 C91 1.395(11) . ? C90 H90 0.9500 . ? C91 H91 0.9500 . ? C92 C93 1.516(8) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C102 1.373(8) . ? C93 C94 1.434(8) . ? C94 C95 1.382(8) . ? C95 C96 1.415(8) . ? C95 C103 1.505(8) . ? C96 C101 1.420(9) . ? C96 C97 1.438(8) . ? C97 C98 1.360(9) . ? C97 H97 0.9500 . ? C98 C99 1.415(11) . ? C98 H98 0.9500 . ? C99 C100 1.379(10) . ? C99 H99 0.9500 . ? C100 C101 1.421(8) . ? C100 H100 0.9500 . ? C101 C102 1.411(9) . ? C102 H102 0.9500 . ? C103 C104 1.381(9) . ? C103 C112 1.422(9) . ? C104 C105 1.397(10) . ? C104 H104 0.9500 . ? C105 C106 1.342(12) . ? C105 H105 0.9500 . ? C106 C107 1.415(11) . ? C106 H106 0.9500 . ? C107 C108 1.407(11) . ? C107 C112 1.441(9) . ? C108 C109 1.386(13) . ? C108 H108 0.9500 . ? C109 C110 1.387(12) . ? C109 H109 0.9500 . ? C110 C111 1.359(10) . ? C110 H110 0.9500 . ? C111 C112 1.411(9) . ? C111 H111 0.9500 . ? C1A Cl1A 1.746(13) . ? C1A Cl2A 1.885(13) . ? C1B Cl2B 1.51(2) . ? C1B Cl1B 1.79(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe1 O1 102.1(2) . . ? O2 Fe1 O3 97.62(18) . . ? O1 Fe1 O3 96.28(18) . . ? O2 Fe1 O4 88.58(17) . . ? O1 Fe1 O4 168.71(18) . . ? O3 Fe1 O4 78.58(16) . . ? O2 Fe1 N2 89.00(18) . . ? O1 Fe1 N2 91.72(18) . . ? O3 Fe1 N2 168.29(17) . . ? O4 Fe1 N2 92.00(16) . . ? O2 Fe1 N1 165.88(19) . . ? O1 Fe1 N1 86.34(18) . . ? O3 Fe1 N1 92.57(18) . . ? O4 Fe1 N1 83.87(16) . . ? N2 Fe1 N1 79.39(18) . . ? O5 Fe2 O6 104.80(18) . . ? O5 Fe2 O3 95.70(19) . . ? O6 Fe2 O3 99.20(18) . . ? O5 Fe2 O4 166.02(16) . . ? O6 Fe2 O4 89.03(17) . . ? O3 Fe2 O4 79.79(16) . . ? O5 Fe2 N4 87.67(19) . . ? O6 Fe2 N4 87.39(18) . . ? O3 Fe2 N4 171.54(18) . . ? O4 Fe2 N4 95.11(17) . . ? O5 Fe2 N3 85.69(19) . . ? O6 Fe2 N3 162.30(19) . . ? O3 Fe2 N3 93.79(18) . . ? O4 Fe2 N3 81.45(17) . . ? N4 Fe2 N3 78.70(18) . . ? C1 N1 C8 113.3(4) . . ? C1 N1 Fe1 111.3(3) . . ? C8 N1 Fe1 110.6(4) . . ? C36 N2 C29 112.5(4) . . ? C36 N2 Fe1 112.1(4) . . ? C29 N2 Fe1 110.2(3) . . ? C57 N3 C64 113.1(5) . . ? C57 N3 Fe2 111.5(3) . . ? C64 N3 Fe2 111.9(4) . . ? C92 N4 C85 114.2(5) . . ? C92 N4 Fe2 113.4(3) . . ? C85 N4 Fe2 108.5(3) . . ? C10 O1 Fe1 135.3(4) . . ? C38 O2 Fe1 130.5(4) . . ? Fe2 O3 Fe1 104.51(19) . . ? Fe2 O4 Fe1 97.06(17) . . ? C66 O5 Fe2 136.2(4) . . ? C94 O6 Fe2 124.4(4) . . ? N1 C1 C2 112.4(4) . . ? N1 C1 C29 108.5(4) . . ? C2 C1 C29 113.0(4) . . ? N1 C1 H1 107.6 . . ? C2 C1 H1 107.6 . . ? C29 C1 H1 107.6 . . ? C3 C2 C7 119.1(6) . . ? C3 C2 C1 119.4(5) . . ? C7 C2 C1 121.5(5) . . ? C2 C3 C4 120.8(7) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 118.8(7) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 120.3(6) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 120.2(7) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C2 120.9(7) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? N1 C8 C9 113.8(5) . . ? N1 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C18 C9 C10 120.0(6) . . ? C18 C9 C8 118.5(6) . . ? C10 C9 C8 121.4(6) . . ? O1 C10 C11 118.0(6) . . ? O1 C10 C9 122.3(5) . . ? C11 C10 C9 119.6(6) . . ? C10 C11 C12 118.8(6) . . ? C10 C11 C19 119.1(6) . . ? C12 C11 C19 121.9(6) . . ? C17 C12 C13 116.5(7) . . ? C17 C12 C11 120.6(6) . . ? C13 C12 C11 122.9(7) . . ? C14 C13 C12 122.1(8) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 120.4(7) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.2(7) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 121.1(8) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C17 C12 120.7(6) . . ? C16 C17 C18 121.4(7) . . ? C12 C17 C18 117.9(6) . . ? C9 C18 C17 122.9(6) . . ? C9 C18 H18 118.6 . . ? C17 C18 H18 118.6 . . ? C28 C19 C20 119.2(7) . . ? C28 C19 C11 122.8(6) . . ? C20 C19 C11 117.9(7) . . ? C21 C20 C19 121.3(8) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 119.9(7) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 118.9(8) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 119.9(7) . . ? C22 C23 C28 121.4(8) . . ? C24 C23 C28 118.6(7) . . ? C25 C24 C23 122.9(7) . . ? C25 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? C26 C25 C24 117.1(8) . . ? C26 C25 H25 121.5 . . ? C24 C25 H25 121.5 . . ? C25 C26 C27 122.3(7) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C28 C27 C26 121.4(6) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C19 123.3(6) . . ? C27 C28 C23 117.6(7) . . ? C19 C28 C23 119.2(7) . . ? N2 C29 C30 114.1(4) . . ? N2 C29 C1 108.2(4) . . ? C30 C29 C1 110.6(4) . . ? N2 C29 H29 107.9 . . ? C30 C29 H29 107.9 . . ? C1 C29 H29 107.9 . . ? C31 C30 C35 118.7(5) . . ? C31 C30 C29 120.7(5) . . ? C35 C30 C29 120.5(5) . . ? C30 C31 C32 120.6(5) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C33 C32 C31 120.4(6) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 119.3(6) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C33 C34 C35 120.8(6) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C34 C35 C30 120.2(5) . . ? C34 C35 H35 119.9 . . ? C30 C35 H35 119.9 . . ? N2 C36 C37 110.8(5) . . ? N2 C36 H36A 109.5 . . ? C37 C36 H36A 109.5 . . ? N2 C36 H36B 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? C46 C37 C38 119.3(5) . . ? C46 C37 C36 120.7(5) . . ? C38 C37 C36 119.9(5) . . ? O2 C38 C39 119.7(5) . . ? O2 C38 C37 120.3(5) . . ? C39 C38 C37 119.9(5) . . ? C38 C39 C40 120.2(6) . . ? C38 C39 C47 118.2(5) . . ? C40 C39 C47 121.5(5) . . ? C39 C40 C45 120.4(5) . . ? C39 C40 C41 122.9(6) . . ? C45 C40 C41 116.7(5) . . ? C42 C41 C40 121.6(6) . . ? C42 C41 H41 119.2 . . ? C40 C41 H41 119.2 . . ? C41 C42 C43 120.6(6) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C44 C43 C42 119.5(6) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C45 121.1(6) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C44 C45 C40 120.6(6) . . ? C44 C45 C46 121.6(6) . . ? C40 C45 C46 117.8(5) . . ? C37 C46 C45 122.2(6) . . ? C37 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C48 C47 C56 119.7(6) . . ? C48 C47 C39 119.4(6) . . ? C56 C47 C39 120.9(6) . . ? C47 C48 C49 122.0(7) . . ? C47 C48 H48 119.0 . . ? C49 C48 H48 119.0 . . ? C50 C49 C48 118.8(8) . . ? C50 C49 H49 120.6 . . ? C48 C49 H49 120.6 . . ? C49 C50 C51 121.6(7) . . ? C49 C50 H50 119.2 . . ? C51 C50 H50 119.2 . . ? C56 C51 C50 119.3(7) . . ? C56 C51 C52 119.4(8) . . ? C50 C51 C52 121.3(8) . . ? C53 C52 C51 120.0(8) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 121.1(7) . . ? C52 C53 H53 119.5 . . ? C54 C53 H53 119.5 . . ? C55 C54 C53 118.7(9) . . ? C55 C54 H54 120.6 . . ? C53 C54 H54 120.6 . . ? C54 C55 C56 122.2(7) . . ? C54 C55 H55 118.9 . . ? C56 C55 H55 118.9 . . ? C55 C56 C51 118.6(7) . . ? C55 C56 C47 122.8(6) . . ? C51 C56 C47 118.7(7) . . ? N3 C57 C58 112.8(5) . . ? N3 C57 C85 108.8(5) . . ? C58 C57 C85 112.0(6) . . ? N3 C57 H57 107.7 . . ? C58 C57 H57 107.7 . . ? C85 C57 H57 107.7 . . ? C63 C58 C59 120.8(7) . . ? C63 C58 C57 122.9(6) . . ? C59 C58 C57 116.3(7) . . ? C60 C59 C58 119.2(10) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? C59 C60 C61 119.1(10) . . ? C59 C60 H60 120.4 . . ? C61 C60 H60 120.4 . . ? C62 C61 C60 120.9(9) . . ? C62 C61 H61 119.6 . . ? C60 C61 H61 119.6 . . ? C63 C62 C61 117.2(10) . . ? C63 C62 H62 121.4 . . ? C61 C62 H62 121.4 . . ? C58 C63 C62 122.4(8) . . ? C58 C63 H63 118.8 . . ? C62 C63 H63 118.8 . . ? N3 C64 C65 114.3(5) . . ? N3 C64 H64A 108.7 . . ? C65 C64 H64A 108.7 . . ? N3 C64 H64B 108.7 . . ? C65 C64 H64B 108.7 . . ? H64A C64 H64B 107.6 . . ? C74 C65 C66 120.0(6) . . ? C74 C65 C64 118.5(6) . . ? C66 C65 C64 121.5(5) . . ? O5 C66 C67 117.3(6) . . ? O5 C66 C65 122.7(5) . . ? C67 C66 C65 120.0(5) . . ? C66 C67 C68 120.0(6) . . ? C66 C67 C75 117.2(5) . . ? C68 C67 C75 122.6(6) . . ? C67 C68 C69 121.6(6) . . ? C67 C68 C73 119.5(6) . . ? C69 C68 C73 118.9(6) . . ? C70 C69 C68 119.2(7) . . ? C70 C69 H69 120.4 . . ? C68 C69 H69 120.4 . . ? C69 C70 C71 122.1(7) . . ? C69 C70 H70 118.9 . . ? C71 C70 H70 118.9 . . ? C72 C71 C70 119.5(7) . . ? C72 C71 H71 120.2 . . ? C70 C71 H71 120.2 . . ? C71 C72 C73 122.0(8) . . ? C71 C72 H72 119.0 . . ? C73 C72 H72 119.0 . . ? C74 C73 C72 123.8(7) . . ? C74 C73 C68 118.0(6) . . ? C72 C73 C68 118.2(6) . . ? C65 C74 C73 122.4(6) . . ? C65 C74 H74 118.8 . . ? C73 C74 H74 118.8 . . ? C76 C75 C84 118.7(6) . . ? C76 C75 C67 123.1(6) . . ? C84 C75 C67 118.0(5) . . ? C75 C76 C77 122.3(7) . . ? C75 C76 H76 118.8 . . ? C77 C76 H76 118.8 . . ? C78 C77 C76 121.0(7) . . ? C78 C77 H77 119.5 . . ? C76 C77 H77 119.5 . . ? C77 C78 C79 119.4(7) . . ? C77 C78 H78 120.3 . . ? C79 C78 H78 120.3 . . ? C78 C79 C84 119.0(7) . . ? C78 C79 C80 123.7(7) . . ? C84 C79 C80 117.3(7) . . ? C81 C80 C79 123.0(8) . . ? C81 C80 H80 118.5 . . ? C79 C80 H80 118.5 . . ? C80 C81 C82 119.8(8) . . ? C80 C81 H81 120.1 . . ? C82 C81 H81 120.1 . . ? C81 C82 C83 121.4(8) . . ? C81 C82 H82 119.3 . . ? C83 C82 H82 119.3 . . ? C82 C83 C84 120.0(7) . . ? C82 C83 H83 120.0 . . ? C84 C83 H83 120.0 . . ? C83 C84 C79 118.4(6) . . ? C83 C84 C75 122.1(6) . . ? C79 C84 C75 119.5(6) . . ? N4 C85 C86 112.4(5) . . ? N4 C85 C57 107.2(5) . . ? C86 C85 C57 112.9(5) . . ? N4 C85 H85 108.1 . . ? C86 C85 H85 108.1 . . ? C57 C85 H85 108.1 . . ? C87 C86 C91 118.8(6) . . ? C87 C86 C85 122.0(6) . . ? C91 C86 C85 119.2(6) . . ? C86 C87 C88 120.2(8) . . ? C86 C87 H87 119.9 . . ? C88 C87 H87 119.9 . . ? C89 C88 C87 120.2(8) . . ? C89 C88 H88 119.9 . . ? C87 C88 H88 119.9 . . ? C88 C89 C90 120.6(7) . . ? C88 C89 H89 119.7 . . ? C90 C89 H89 119.7 . . ? C89 C90 C91 120.4(8) . . ? C89 C90 H90 119.8 . . ? C91 C90 H90 119.8 . . ? C86 C91 C90 119.7(7) . . ? C86 C91 H91 120.1 . . ? C90 C91 H91 120.1 . . ? N4 C92 C93 109.5(5) . . ? N4 C92 H92A 109.8 . . ? C93 C92 H92A 109.8 . . ? N4 C92 H92B 109.8 . . ? C93 C92 H92B 109.8 . . ? H92A C92 H92B 108.2 . . ? C102 C93 C94 120.5(5) . . ? C102 C93 C92 121.6(5) . . ? C94 C93 C92 117.9(5) . . ? O6 C94 C95 122.0(5) . . ? O6 C94 C93 118.5(5) . . ? C95 C94 C93 119.5(5) . . ? C94 C95 C96 120.4(5) . . ? C94 C95 C103 118.0(5) . . ? C96 C95 C103 121.5(5) . . ? C95 C96 C101 119.8(5) . . ? C95 C96 C97 122.4(6) . . ? C101 C96 C97 117.8(5) . . ? C98 C97 C96 121.4(6) . . ? C98 C97 H97 119.3 . . ? C96 C97 H97 119.3 . . ? C97 C98 C99 120.3(6) . . ? C97 C98 H98 119.9 . . ? C99 C98 H98 119.9 . . ? C100 C99 C98 120.2(6) . . ? C100 C99 H99 119.9 . . ? C98 C99 H99 119.9 . . ? C99 C100 C101 120.5(6) . . ? C99 C100 H100 119.8 . . ? C101 C100 H100 119.8 . . ? C102 C101 C96 119.2(5) . . ? C102 C101 C100 121.1(6) . . ? C96 C101 C100 119.7(6) . . ? C93 C102 C101 120.6(6) . . ? C93 C102 H102 119.7 . . ? C101 C102 H102 119.7 . . ? C104 C103 C112 119.6(6) . . ? C104 C103 C95 119.0(6) . . ? C112 C103 C95 121.4(5) . . ? C103 C104 C105 120.9(7) . . ? C103 C104 H104 119.6 . . ? C105 C104 H104 119.6 . . ? C106 C105 C104 121.3(7) . . ? C106 C105 H105 119.3 . . ? C104 C105 H105 119.3 . . ? C105 C106 C107 120.7(6) . . ? C105 C106 H106 119.6 . . ? C107 C106 H106 119.6 . . ? C108 C107 C106 122.1(6) . . ? C108 C107 C112 119.0(7) . . ? C106 C107 C112 119.0(7) . . ? C109 C108 C107 120.4(6) . . ? C109 C108 H108 119.8 . . ? C107 C108 H108 119.8 . . ? C108 C109 C110 119.8(8) . . ? C108 C109 H109 120.1 . . ? C110 C109 H109 120.1 . . ? C111 C110 C109 121.8(8) . . ? C111 C110 H110 119.1 . . ? C109 C110 H110 119.1 . . ? C110 C111 C112 120.5(6) . . ? C110 C111 H111 119.7 . . ? C112 C111 H111 119.7 . . ? C111 C112 C103 123.2(5) . . ? C111 C112 C107 118.4(6) . . ? C103 C112 C107 118.5(6) . . ? Cl1A C1A Cl2A 107.3(6) . . ? Cl2B C1B Cl1B 115.6(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.561 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.158 # Attachment '8253_web_deposit_cif_file_2_KenjiMatsumoto_1321546181.complex5_[(L3)Fe(OH)2Fe(L3)]_KM98_2_final.cif' data_R_diPh_3PhNp_FeNHsalan_diOH_KM98 _database_code_depnum_ccdc_archive 'CCDC 854409' #TrackingRef '8253_web_deposit_cif_file_2_KenjiMatsumoto_1321546181.complex5_[(L3)Fe(OH)2Fe(L3)]_KM98_2_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96H78Fe2N4O6, H2O, 2(C3H6O)' _chemical_formula_sum 'C102 H92 Fe2 N4 O9' _chemical_formula_weight 1629.50 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 26.435(4) _cell_length_b 12.5897(17) _cell_length_c 18.562(5) _cell_angle_alpha 90.00 _cell_angle_beta 125.3570(10) _cell_angle_gamma 90.00 _cell_volume 5038.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9907 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour 'red purple' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.341 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9197 _exptl_absorpt_correction_T_max 0.9733 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 'focusing mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 28940 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.51 _reflns_number_total 11455 _reflns_number_gt 10074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1938P)^2^+1.9933P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 11455 _refine_ls_number_parameters 569 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2520 _refine_ls_wR_factor_gt 0.2407 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.441318(18) 0.34855(4) 0.40394(3) 0.02704(16) Uani 1 1 d . A 1 N1 N 0.50401(13) 0.3578(4) 0.36422(19) 0.0343(7) Uani 1 1 d . A 1 N2 N 0.39867(19) 0.4760(4) 0.3062(3) 0.0397(9) Uani 1 1 d . A 1 O1 O 0.39690(15) 0.2431(3) 0.3143(2) 0.0373(7) Uani 1 1 d . A 1 O2 O 0.38327(12) 0.3729(3) 0.43179(17) 0.0369(7) Uani 1 1 d . A 1 O3 O 0.5000 0.2531(3) 0.5000 0.0312(9) Uani 1 2 d S . 1 O4 O 0.5000 0.4534(4) 0.5000 0.0309(9) Uani 1 2 d S . 1 C1 C 0.4857(2) 0.4432(4) 0.2959(3) 0.0398(10) Uani 1 1 d . A 1 H1 H 0.4574 0.4098 0.2364 0.048 Uiso 1 1 calc R A 1 C2 C 0.5423(2) 0.4827(5) 0.3023(4) 0.0517(12) Uani 1 1 d . A 1 C3 C 0.5936(3) 0.5197(8) 0.3800(5) 0.089(3) Uani 1 1 d . A 1 H3 H 0.5934 0.5244 0.4309 0.107 Uiso 1 1 calc R A 1 C4 C 0.6460(4) 0.5503(9) 0.3851(7) 0.112(4) Uani 1 1 d . A 1 H4 H 0.6814 0.5741 0.4401 0.135 Uiso 1 1 calc R A 1 C5 C 0.6478(4) 0.5471(9) 0.3141(8) 0.114(4) Uani 1 1 d . A 1 H5 H 0.6830 0.5722 0.3175 0.137 Uiso 1 1 calc R A 1 C6 C 0.6000(6) 0.5087(14) 0.2409(9) 0.156(7) Uani 1 1 d . . . H6 H 0.6015 0.5022 0.1912 0.187 Uiso 1 1 calc R A 1 C7 C 0.5454(4) 0.4760(12) 0.2330(6) 0.133(5) Uani 1 1 d . A 1 H7 H 0.5110 0.4492 0.1783 0.160 Uiso 1 1 calc R A 1 C8 C 0.51636(19) 0.2554(4) 0.3421(3) 0.0426(10) Uani 1 1 d . A 1 H8A H 0.5325 0.2066 0.3928 0.051 Uiso 1 1 calc R A 1 H8B H 0.5489 0.2637 0.3316 0.051 Uiso 1 1 calc R A 1 C9 C 0.45890(18) 0.2063(4) 0.2605(3) 0.0342(8) Uani 1 1 d . A 1 C10 C 0.40197(18) 0.2023(3) 0.2528(2) 0.0328(8) Uani 1 1 d . A 1 C11 C 0.35018(18) 0.1522(3) 0.1795(2) 0.0316(8) Uani 1 1 d . A 1 C12 C 0.3543(2) 0.1038(3) 0.1140(3) 0.0333(8) Uani 1 1 d . A 1 C13 C 0.3028(2) 0.0539(4) 0.0374(3) 0.0495(11) Uani 1 1 d . A 1 H13 H 0.2645 0.0494 0.0308 0.059 Uiso 1 1 calc R A 1 C14 C 0.3071(3) 0.0126(5) -0.0263(4) 0.0596(14) Uani 1 1 d . A 1 H14 H 0.2721 -0.0205 -0.0766 0.072 Uiso 1 1 calc R A 1 C15 C 0.3658(3) 0.0190(5) -0.0177(4) 0.0605(14) Uani 1 1 d . A 1 H15 H 0.3688 -0.0081 -0.0628 0.073 Uiso 1 1 calc R A 1 C16 C 0.4153(3) 0.0638(4) 0.0553(3) 0.0458(10) Uani 1 1 d . A 1 H16 H 0.4538 0.0655 0.0622 0.055 Uiso 1 1 calc R A 1 C17 C 0.4115(2) 0.1086(3) 0.1222(3) 0.0356(8) Uani 1 1 d . A 1 C18 C 0.4624(2) 0.1603(3) 0.1962(3) 0.0360(8) Uani 1 1 d . A 1 H18 H 0.5005 0.1636 0.2021 0.043 Uiso 1 1 calc R A 1 C19 C 0.29129(19) 0.1528(4) 0.1726(3) 0.0362(8) Uani 1 1 d . A 1 C20 C 0.2609(2) 0.2492(4) 0.1621(3) 0.0422(10) Uani 1 1 d . A 1 H20 H 0.2783 0.3137 0.1590 0.051 Uiso 1 1 calc R A 1 C21 C 0.2065(2) 0.2526(5) 0.1563(3) 0.0526(12) Uani 1 1 d . A 1 H21 H 0.1863 0.3186 0.1480 0.063 Uiso 1 1 calc R A 1 C22 C 0.1812(3) 0.1590(6) 0.1625(4) 0.0628(15) Uani 1 1 d . A 1 H22 H 0.1442 0.1608 0.1599 0.075 Uiso 1 1 calc R A 1 C23 C 0.2103(3) 0.0634(5) 0.1727(4) 0.0648(16) Uani 1 1 d . A 1 H23 H 0.1924 -0.0004 0.1755 0.078 Uiso 1 1 calc R A 1 C24 C 0.2651(3) 0.0585(4) 0.1789(4) 0.0509(11) Uani 1 1 d . A 1 H24 H 0.2849 -0.0079 0.1874 0.061 Uiso 1 1 calc R A 1 C25 C 0.4492(2) 0.5293(4) 0.3043(3) 0.0444(10) Uani 1 1 d . . . H25 H 0.4767 0.5739 0.3580 0.053 Uiso 1 1 calc R A 1 C26 C 0.4213(10) 0.5928(16) 0.2218(11) 0.042(4) Uani 0.43(2) 1 d P A 1 C27 C 0.3821(8) 0.5551(9) 0.1358(9) 0.038(3) Uani 0.43(2) 1 d P A 1 C28 C 0.3619(6) 0.6305(10) 0.0652(6) 0.047(4) Uani 0.43(2) 1 d P A 1 C29 C 0.3766(14) 0.7386(16) 0.0819(11) 0.093(9) Uani 0.43(2) 1 d P A 1 C30 C 0.414(2) 0.7640(15) 0.1682(12) 0.153(18) Uani 0.43(2) 1 d P A 1 C31 C 0.4278(19) 0.6996(18) 0.2343(10) 0.126(14) Uani 0.43(2) 1 d P A 1 C32 C 0.3643(3) 0.5519(5) 0.3257(4) 0.0547(13) Uani 1 1 d . A 1 H32A H 0.3470 0.6104 0.2820 0.066 Uiso 1 1 calc R A 1 H32B H 0.3934 0.5831 0.3851 0.066 Uiso 1 1 calc R A 1 C33 C 0.3118(2) 0.4955(5) 0.3220(3) 0.0472(11) Uani 1 1 d . A 1 C34 C 0.32479(19) 0.4066(4) 0.3782(3) 0.0402(9) Uani 1 1 d . A 1 C35 C 0.27875(18) 0.3575(6) 0.3800(2) 0.0489(11) Uani 1 1 d . A 1 C36 C 0.2169(2) 0.3968(5) 0.3248(3) 0.0532(13) Uani 1 1 d . A 1 C37 C 0.1668(2) 0.3458(9) 0.3204(3) 0.0707(18) Uani 1 1 d . A 1 H37 H 0.1745 0.2853 0.3559 0.085 Uiso 1 1 calc R A 1 C38 C 0.1082(3) 0.3842(10) 0.2653(6) 0.101(4) Uani 1 1 d . A 1 H38 H 0.0751 0.3479 0.2614 0.121 Uiso 1 1 calc R A 1 C39 C 0.0954(3) 0.4717(9) 0.2163(5) 0.094(3) Uani 1 1 d . A 1 H39 H 0.0538 0.4967 0.1804 0.113 Uiso 1 1 calc R A 1 C40 C 0.1420(3) 0.5288(7) 0.2160(4) 0.080(2) Uani 1 1 d . A 1 H40 H 0.1323 0.5900 0.1803 0.096 Uiso 1 1 calc R A 1 C41 C 0.2050(2) 0.4884(6) 0.2731(4) 0.0652(18) Uani 1 1 d . A 1 C42 C 0.2518(3) 0.5336(5) 0.2711(3) 0.0594(14) Uani 1 1 d . A 1 H42 H 0.2424 0.5928 0.2336 0.071 Uiso 1 1 calc R A 1 C43 C 0.2955(2) 0.2614(7) 0.4370(4) 0.069(2) Uani 1 1 d . A 1 C44 C 0.3155(4) 0.1691(6) 0.4216(6) 0.082(2) Uani 1 1 d . . . H44 H 0.3186 0.1663 0.3731 0.098 Uiso 1 1 calc R A 1 C45 C 0.3312(5) 0.0804(10) 0.4742(8) 0.132(5) Uani 1 1 d . A . H45 H 0.3435 0.0160 0.4617 0.159 Uiso 1 1 calc R . . C46 C 0.3282(5) 0.0901(16) 0.5475(9) 0.165(9) Uani 1 1 d . . . H46 H 0.3388 0.0306 0.5852 0.198 Uiso 1 1 calc R A . C47 C 0.3114(5) 0.1784(13) 0.5649(6) 0.112(4) Uani 1 1 d . A . H47 H 0.3105 0.1816 0.6153 0.134 Uiso 1 1 calc R B 1 C48 C 0.2950(4) 0.2666(11) 0.5125(5) 0.100(3) Uani 1 1 d . A 1 H48 H 0.2834 0.3303 0.5268 0.120 Uiso 1 1 calc R A 1 C26A C 0.4279(8) 0.6289(15) 0.2420(13) 0.054(4) Uani 0.57(2) 1 d P A 2 C27A C 0.3802(8) 0.607(2) 0.1515(14) 0.116(10) Uani 0.57(2) 1 d P A 2 C28A C 0.3609(9) 0.7159(19) 0.1003(15) 0.104(8) Uani 0.57(2) 1 d P A 2 C29A C 0.3918(8) 0.7931(19) 0.129(2) 0.110(8) Uani 0.57(2) 1 d P A 2 C30A C 0.4371(7) 0.8056(17) 0.2024(19) 0.133(11) Uani 0.57(2) 1 d P A 2 C31A C 0.4578(6) 0.7227(13) 0.2683(16) 0.090(7) Uani 0.57(2) 1 d P A 2 C1S C 1.0000 0.1587(12) 0.0000 0.095(3) Uiso 1 2 d S . 1 C2S C 0.9950(12) 0.222(2) 0.0682(16) 0.215(9) Uiso 1 1 d . . . C3S C 0.4905(11) 0.983(2) 0.3985(19) 0.136(9) Uiso 0.50 1 d PD . . C4S C 0.4232(10) 0.9433(19) 0.3657(16) 0.109(6) Uiso 0.50 1 d PD . . C5S C 0.5277(10) 0.938(2) 0.3668(15) 0.112(6) Uiso 0.50 1 d PD . . O1S O 1.0000 0.0712(15) 0.0000 0.169(5) Uiso 1 2 d S . . O2S O 0.5260(5) 1.0488(9) 0.4640(7) 0.079(3) Uiso 0.50 1 d P . . O1W O 0.5000 0.6780(16) 0.5000 0.186(6) Uiso 1 2 d S . . 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 0.0199(2) 0.0374(3) 0.0167(2) 0.0010(2) 0.00650(17) -0.0012(2) N1 0.0218(12) 0.053(2) 0.0233(12) -0.0052(16) 0.0102(10) -0.0088(17) N2 0.0301(18) 0.058(2) 0.0281(18) 0.0145(16) 0.0148(15) 0.0091(16) O1 0.0283(15) 0.0543(19) 0.0214(14) -0.0073(12) 0.0099(12) -0.0097(13) O2 0.0244(11) 0.059(2) 0.0227(11) 0.0065(11) 0.0111(10) 0.0043(11) O3 0.027(2) 0.031(2) 0.025(2) 0.000 0.0088(18) 0.000 O4 0.028(2) 0.035(2) 0.0194(18) 0.000 0.0080(16) 0.000 C1 0.030(2) 0.061(3) 0.0259(18) -0.0060(18) 0.0148(16) -0.0188(19) C2 0.039(2) 0.071(3) 0.050(3) -0.014(2) 0.029(2) -0.025(2) C3 0.063(4) 0.132(7) 0.058(3) -0.016(4) 0.027(3) -0.063(4) C4 0.062(4) 0.144(8) 0.099(6) 0.013(6) 0.028(4) -0.058(5) C5 0.085(6) 0.127(8) 0.161(10) -0.038(7) 0.090(7) -0.063(6) C6 0.151(10) 0.241(16) 0.152(10) -0.062(11) 0.131(10) -0.115(11) C7 0.092(6) 0.255(15) 0.074(5) -0.061(7) 0.060(5) -0.110(8) C8 0.0216(18) 0.060(3) 0.039(2) -0.014(2) 0.0133(17) -0.0033(18) C9 0.0285(18) 0.043(2) 0.0256(18) -0.0079(15) 0.0125(15) -0.0068(16) C10 0.0310(18) 0.041(2) 0.0192(15) 0.0003(14) 0.0102(14) -0.0074(15) C11 0.0296(18) 0.0288(16) 0.0248(17) 0.0018(13) 0.0090(14) -0.0073(14) C12 0.040(2) 0.0219(16) 0.0264(18) -0.0009(14) 0.0126(16) -0.0065(15) C13 0.049(3) 0.048(2) 0.035(2) -0.0138(19) 0.015(2) -0.014(2) C14 0.058(3) 0.064(3) 0.040(3) -0.026(2) 0.018(2) -0.013(2) C15 0.072(4) 0.061(3) 0.037(2) -0.014(2) 0.025(2) 0.004(3) C16 0.055(3) 0.041(2) 0.039(2) -0.0007(18) 0.026(2) 0.0036(19) C17 0.046(2) 0.0259(16) 0.0283(18) 0.0043(14) 0.0176(17) 0.0023(16) C18 0.038(2) 0.0351(19) 0.0343(19) -0.0033(15) 0.0206(17) 0.0003(16) C19 0.0301(18) 0.043(2) 0.0257(17) -0.0084(15) 0.0102(15) -0.0147(16) C20 0.034(2) 0.046(2) 0.032(2) -0.0060(17) 0.0107(17) -0.0087(18) C21 0.036(2) 0.063(3) 0.044(2) -0.017(2) 0.014(2) -0.008(2) C22 0.044(3) 0.083(4) 0.063(3) -0.025(3) 0.032(3) -0.026(3) C23 0.066(3) 0.063(3) 0.080(4) -0.024(3) 0.051(3) -0.037(3) C24 0.055(3) 0.041(2) 0.057(3) -0.010(2) 0.033(2) -0.015(2) C25 0.034(2) 0.056(3) 0.035(2) 0.0162(19) 0.0159(18) 0.0014(19) C26 0.063(9) 0.034(8) 0.026(7) -0.008(5) 0.024(6) -0.018(7) C27 0.052(7) 0.023(5) 0.023(5) 0.003(4) 0.013(5) -0.008(5) C28 0.050(7) 0.046(7) 0.021(5) 0.015(4) 0.006(4) -0.010(5) C29 0.16(2) 0.057(10) 0.029(7) 0.014(6) 0.039(10) -0.039(11) C30 0.32(5) 0.033(8) 0.026(8) 0.003(6) 0.057(15) -0.031(14) C31 0.23(3) 0.062(11) 0.024(7) -0.007(7) 0.042(12) -0.072(16) C32 0.056(3) 0.061(3) 0.050(3) 0.025(2) 0.032(2) 0.023(2) C33 0.032(2) 0.067(3) 0.033(2) 0.005(2) 0.0133(17) 0.018(2) C34 0.0298(19) 0.060(3) 0.0275(19) -0.0050(18) 0.0147(16) 0.0016(18) C35 0.0290(17) 0.089(4) 0.0239(16) -0.004(3) 0.0128(14) 0.000(3) C36 0.030(2) 0.094(4) 0.032(2) -0.019(2) 0.0160(18) -0.002(2) C37 0.0315(19) 0.134(6) 0.044(2) -0.036(4) 0.0208(19) -0.017(4) C38 0.033(3) 0.193(12) 0.069(4) -0.062(6) 0.025(3) -0.008(4) C39 0.026(3) 0.164(9) 0.068(4) -0.036(5) 0.013(3) 0.025(4) C40 0.039(3) 0.122(6) 0.058(3) -0.017(4) 0.016(3) 0.030(3) C41 0.032(2) 0.111(5) 0.041(3) -0.018(3) 0.014(2) 0.024(3) C42 0.047(3) 0.075(4) 0.039(2) 0.004(2) 0.015(2) 0.028(3) C43 0.029(2) 0.128(6) 0.036(2) 0.009(3) 0.010(2) -0.033(3) C44 0.080(5) 0.072(4) 0.087(5) 0.012(4) 0.044(4) -0.010(4) C45 0.111(8) 0.122(9) 0.106(8) 0.042(7) 0.030(6) -0.031(7) C46 0.068(6) 0.236(17) 0.116(9) 0.102(11) 0.010(6) -0.062(9) C47 0.083(6) 0.185(13) 0.061(5) 0.048(7) 0.038(4) -0.006(7) C48 0.070(4) 0.182(10) 0.048(3) 0.014(5) 0.034(3) -0.022(5) C26A 0.055(7) 0.049(10) 0.050(10) 0.022(7) 0.025(7) 0.000(7) C27A 0.065(9) 0.15(2) 0.073(12) 0.085(14) 0.008(8) -0.025(13) C28A 0.091(11) 0.109(15) 0.088(13) 0.055(13) 0.039(10) 0.005(10) C29A 0.065(9) 0.101(14) 0.14(2) 0.052(15) 0.044(11) -0.004(9) C30A 0.058(8) 0.088(12) 0.19(2) 0.092(14) 0.037(11) 0.001(7) C31A 0.043(6) 0.065(9) 0.129(15) 0.059(10) 0.030(7) 0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.906(3) . ? Fe1 O1 1.910(3) . ? Fe1 O3 1.956(3) . ? Fe1 O4 2.031(3) . ? Fe1 N1 2.172(3) . ? Fe1 N2 2.184(4) . ? N1 C8 1.446(6) . ? N1 C1 1.512(6) . ? N2 C32 1.500(7) . ? N2 C25 1.514(6) . ? O1 C10 1.327(5) . ? O2 C34 1.334(5) . ? O3 Fe1 1.956(3) 2_656 ? O4 Fe1 2.031(3) 2_656 ? C1 C2 1.515(6) . ? C1 C25 1.516(7) . ? C1 H1 1.0000 . ? C2 C7 1.339(9) . ? C2 C3 1.368(8) . ? C3 C4 1.385(10) . ? C3 H3 0.9500 . ? C4 C5 1.346(15) . ? C4 H4 0.9500 . ? C5 C6 1.301(15) . ? C5 H5 0.9500 . ? C6 C7 1.424(10) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.523(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C18 1.376(6) . ? C9 C10 1.429(6) . ? C10 C11 1.403(5) . ? C11 C12 1.419(6) . ? C11 C19 1.487(6) . ? C12 C13 1.425(6) . ? C12 C17 1.430(6) . ? C13 C14 1.354(8) . ? C13 H13 0.9500 . ? C14 C15 1.466(9) . ? C14 H14 0.9500 . ? C15 C16 1.347(8) . ? C15 H15 0.9500 . ? C16 C17 1.419(6) . ? C16 H16 0.9500 . ? C17 C18 1.408(6) . ? C18 H18 0.9500 . ? C19 C20 1.406(7) . ? C19 C24 1.413(6) . ? C20 C21 1.378(7) . ? C20 H20 0.9500 . ? C21 C22 1.394(9) . ? C21 H21 0.9500 . ? C22 C23 1.381(10) . ? C22 H22 0.9500 . ? C23 C24 1.386(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.49(2) . ? C25 C26A 1.573(15) . ? C25 H25 1.0000 . ? C26 C31 1.36(2) . ? C26 C27 1.389(18) . ? C27 C28 1.447(17) . ? C28 C29 1.40(2) . ? C29 C30 1.35(2) . ? C30 C31 1.33(2) . ? C32 C33 1.525(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C42 1.380(6) . ? C33 C34 1.430(7) . ? C34 C35 1.382(7) . ? C35 C36 1.425(7) . ? C35 C43 1.496(10) . ? C36 C41 1.414(10) . ? C36 C37 1.431(8) . ? C37 C38 1.359(11) . ? C37 H37 0.9500 . ? C38 C39 1.342(16) . ? C38 H38 0.9500 . ? C39 C40 1.429(13) . ? C39 H39 0.9500 . ? C40 C41 1.454(7) . ? C40 H40 0.9500 . ? C41 C42 1.380(10) . ? C42 H42 0.9500 . ? C43 C44 1.373(12) . ? C43 C48 1.409(10) . ? C44 C45 1.379(13) . ? C44 H44 0.9500 . ? C45 C46 1.41(2) . ? C45 H45 0.9500 . ? C46 C47 1.31(2) . ? C46 H46 0.9500 . ? C47 C48 1.371(17) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C26A C31A 1.35(2) . ? C26A C27A 1.43(3) . ? C27A C28A 1.57(3) . ? C28A C29A 1.18(3) . ? C29A C30A 1.20(4) . ? C30A C31A 1.45(2) . ? C1S O1S 1.10(2) . ? C1S C2S 1.57(3) . ? C1S C2S 1.57(3) 2_755 ? C3S O2S 1.31(3) . ? C3S C5S 1.521(18) . ? C3S C4S 1.593(18) . ? 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 O2 Fe1 O1 99.36(14) . . ? O2 Fe1 O3 100.94(9) . . ? O1 Fe1 O3 97.51(16) . . ? O2 Fe1 O4 89.03(9) . . ? O1 Fe1 O4 171.28(12) . . ? O3 Fe1 O4 78.39(11) . . ? O2 Fe1 N1 167.27(16) . . ? O1 Fe1 N1 86.95(15) . . ? O3 Fe1 N1 89.07(10) . . ? O4 Fe1 N1 85.30(10) . . ? O2 Fe1 N2 89.85(14) . . ? O1 Fe1 N2 91.47(14) . . ? O3 Fe1 N2 164.59(12) . . ? O4 Fe1 N2 90.95(16) . . ? N1 Fe1 N2 78.89(16) . . ? C8 N1 C1 114.3(3) . . ? C8 N1 Fe1 113.0(3) . . ? C1 N1 Fe1 112.7(3) . . ? C32 N2 C25 113.0(4) . . ? C32 N2 Fe1 111.2(3) . . ? C25 N2 Fe1 107.8(3) . . ? C10 O1 Fe1 134.5(3) . . ? C34 O2 Fe1 128.1(3) . . ? Fe1 O3 Fe1 104.2(2) 2_656 . ? Fe1 O4 Fe1 98.97(19) . 2_656 ? N1 C1 C2 110.2(4) . . ? N1 C1 C25 109.7(3) . . ? C2 C1 C25 114.5(4) . . ? N1 C1 H1 107.4 . . ? C2 C1 H1 107.4 . . ? C25 C1 H1 107.4 . . ? C7 C2 C3 117.3(6) . . ? C7 C2 C1 120.7(5) . . ? C3 C2 C1 121.8(5) . . ? C2 C3 C4 120.6(8) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 121.6(8) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C6 C5 C4 118.1(7) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C5 C6 C7 121.9(9) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C2 C7 C6 120.3(8) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? N1 C8 C9 112.6(4) . . ? N1 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C18 C9 C10 119.6(4) . . ? C18 C9 C8 120.3(4) . . ? C10 C9 C8 120.0(4) . . ? O1 C10 C11 118.8(4) . . ? O1 C10 C9 121.7(3) . . ? C11 C10 C9 119.5(4) . . ? C10 C11 C12 120.6(4) . . ? C10 C11 C19 117.8(4) . . ? C12 C11 C19 121.6(3) . . ? C11 C12 C13 122.8(4) . . ? C11 C12 C17 119.4(3) . . ? C13 C12 C17 117.8(4) . . ? C14 C13 C12 121.7(5) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 120.1(5) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 118.9(5) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 121.9(5) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C18 C17 C16 121.8(4) . . ? C18 C17 C12 118.5(4) . . ? C16 C17 C12 119.6(4) . . ? C9 C18 C17 122.4(4) . . ? C9 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C20 C19 C24 117.9(4) . . ? C20 C19 C11 120.2(4) . . ? C24 C19 C11 121.9(4) . . ? C21 C20 C19 121.6(5) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 119.8(5) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 119.4(5) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 121.6(5) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C23 C24 C19 119.6(5) . . ? C23 C24 H24 120.2 . . ? C19 C24 H24 120.2 . . ? C26 C25 N2 110.0(9) . . ? C26 C25 C1 104.2(8) . . ? N2 C25 C1 107.9(4) . . ? C26 C25 C26A 20.5(6) . . ? N2 C25 C26A 115.1(7) . . ? C1 C25 C26A 118.3(8) . . ? C26 C25 H25 111.5 . . ? N2 C25 H25 111.5 . . ? C1 C25 H25 111.5 . . ? C26A C25 H25 91.7 . . ? C31 C26 C27 118.1(17) . . ? C31 C26 C25 114.6(11) . . ? C27 C26 C25 126.4(14) . . ? C26 C27 C28 117.1(13) . . ? C29 C28 C27 121.9(11) . . ? C30 C29 C28 114.3(14) . . ? C31 C30 C29 125(2) . . ? C30 C31 C26 120.2(16) . . ? N2 C32 C33 110.8(5) . . ? N2 C32 H32A 109.5 . . ? C33 C32 H32A 109.5 . . ? N2 C32 H32B 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C42 C33 C34 117.8(5) . . ? C42 C33 C32 121.7(5) . . ? C34 C33 C32 120.3(4) . . ? O2 C34 C35 119.8(4) . . ? O2 C34 C33 118.5(4) . . ? C35 C34 C33 121.6(4) . . ? C34 C35 C36 119.2(6) . . ? C34 C35 C43 118.3(4) . . ? C36 C35 C43 122.4(5) . . ? C41 C36 C35 118.8(5) . . ? C41 C36 C37 119.6(6) . . ? C35 C36 C37 121.6(6) . . ? C38 C37 C36 119.9(9) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C39 C38 C37 122.1(9) . . ? C39 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? C38 C39 C40 122.4(6) . . ? C38 C39 H39 118.8 . . ? C40 C39 H39 118.8 . . ? C39 C40 C41 116.7(8) . . ? C39 C40 H40 121.7 . . ? C41 C40 H40 121.7 . . ? C42 C41 C36 120.3(5) . . ? C42 C41 C40 120.2(7) . . ? C36 C41 C40 119.3(7) . . ? C41 C42 C33 122.1(6) . . ? C41 C42 H42 119.0 . . ? C33 C42 H42 119.0 . . ? C44 C43 C48 118.2(8) . . ? C44 C43 C35 121.9(6) . . ? C48 C43 C35 119.8(9) . . ? C43 C44 C45 122.2(10) . . ? C43 C44 H44 118.9 . . ? C45 C44 H44 118.9 . . ? C44 C45 C46 116.7(14) . . ? C44 C45 H45 121.7 . . ? C46 C45 H45 121.7 . . ? C47 C46 C45 121.9(11) . . ? C47 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? C46 C47 C48 121.8(11) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C47 C48 C43 119.1(12) . . ? C47 C48 H48 120.4 . . ? C43 C48 H48 120.4 . . ? C31A C26A C27A 122.0(15) . . ? C31A C26A C25 123.1(14) . . ? C27A C26A C25 114.2(14) . . ? C26A C27A C28A 107(2) . . ? C29A C28A C27A 123(2) . . ? C28A C29A C30A 126(2) . . ? C29A C30A C31A 120.6(18) . . ? C26A C31A C30A 117.9(18) . . ? O1S C1S C2S 120.7(11) . . ? O1S C1S C2S 120.7(11) . 2_755 ? C2S C1S C2S 119(2) . 2_755 ? O2S C3S C5S 108.6(18) . . ? O2S C3S C4S 126.6(19) . . ? C5S C3S C4S 124(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.515 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.168 # Attachment '8255_web_deposit_cif_file_4_KenjiMatsumoto_1321546181.complex8_[Fe(L1)(1Br2NpO)(H2O)]_KM296_final.cif' data_Fesalan_1Br2NpO_H2O_KM296 _database_code_depnum_ccdc_archive 'CCDC 854410' #TrackingRef '8255_web_deposit_cif_file_4_KenjiMatsumoto_1321546181.complex8_[Fe(L1)(1Br2NpO)(H2O)]_KM296_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C79 H62 Br Cl2 Fe N2 O5' _chemical_formula_sum 'C79 H62 Br Cl2 Fe N2 O5' _chemical_formula_weight 1325.97 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.237(2) _cell_length_b 19.981(3) _cell_length_c 22.218(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6320.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9908 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.41 _exptl_crystal_description block _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2740 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8388 _exptl_absorpt_correction_T_max 0.9055 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 'focusing mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 36196 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.49 _reflns_number_total 14367 _reflns_number_gt 12493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+4.6062P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(6) _refine_ls_number_reflns 14367 _refine_ls_number_parameters 827 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.91600(3) 0.74874(2) 0.778356(18) 0.01466(9) Uani 1 1 d . . . O1 O 0.79462(14) 0.78473(11) 0.77625(9) 0.0190(4) Uani 1 1 d . . . O2 O 0.94688(14) 0.73566(10) 0.69472(9) 0.0185(4) Uani 1 1 d . . . O3 O 0.88442(15) 0.65721(11) 0.80518(10) 0.0233(5) Uani 1 1 d . . . O4 O 0.98013(17) 0.84815(12) 0.76255(12) 0.0221(5) Uani 1 1 d . . . O5 O 0.95321(17) 0.93756(12) 0.85687(11) 0.0311(5) Uani 1 1 d . . . N1 N 0.92919(17) 0.78344(13) 0.87205(11) 0.0165(5) Uani 1 1 d . . . N2 N 1.05673(17) 0.71562(13) 0.80136(11) 0.0148(5) Uani 1 1 d . . . C1 C 1.00306(19) 0.74297(15) 0.90270(12) 0.0162(5) Uani 1 1 d . . . H1 H 0.9788 0.6963 0.9076 0.019 Uiso 1 1 calc R . . C2 C 1.0300(2) 0.76933(16) 0.96446(13) 0.0196(6) Uani 1 1 d . . . C3 C 1.0532(3) 0.83655(19) 0.97295(16) 0.0295(8) Uani 1 1 d . . . H3 H 1.0483 0.8671 0.9403 0.035 Uiso 1 1 calc R . . C4 C 1.0835(3) 0.8590(2) 1.02863(17) 0.0386(9) Uani 1 1 d . . . H4A H 1.1000 0.9047 1.0340 0.046 Uiso 1 1 calc R . . C5 C 1.0896(3) 0.8144(2) 1.07684(16) 0.0363(9) Uani 1 1 d . . . H5 H 1.1099 0.8298 1.1151 0.044 Uiso 1 1 calc R . . C6 C 1.0664(2) 0.7491(2) 1.06897(15) 0.0343(8) Uani 1 1 d . . . H6 H 1.0706 0.7189 1.1019 0.041 Uiso 1 1 calc R . . C7 C 1.0365(3) 0.72597(18) 1.01297(15) 0.0281(7) Uani 1 1 d . . . H7 H 1.0204 0.6802 1.0080 0.034 Uiso 1 1 calc R . . C8 C 0.8372(2) 0.77982(15) 0.90273(13) 0.0183(6) Uani 1 1 d . . . H8A H 0.8458 0.7909 0.9458 0.022 Uiso 1 1 calc R . . H8B H 0.8132 0.7334 0.9002 0.022 Uiso 1 1 calc R . . C9 C 0.7653(2) 0.82706(15) 0.87569(13) 0.0167(6) Uani 1 1 d . . . C10 C 0.7435(2) 0.82211(15) 0.81273(13) 0.0179(6) Uani 1 1 d . . . C11 C 0.6641(2) 0.85500(16) 0.79035(13) 0.0195(6) Uani 1 1 d . . . C12 C 0.6099(2) 0.89687(16) 0.82832(14) 0.0208(6) Uani 1 1 d . . . C13 C 0.5279(2) 0.93019(19) 0.80837(15) 0.0295(7) Uani 1 1 d . . . H13 H 0.5083 0.9250 0.7678 0.035 Uiso 1 1 calc R . . C14 C 0.4762(3) 0.9697(2) 0.84609(17) 0.0341(8) Uani 1 1 d . . . H14 H 0.4216 0.9915 0.8314 0.041 Uiso 1 1 calc R . . C15 C 0.5033(2) 0.97829(18) 0.90676(16) 0.0302(8) Uani 1 1 d . . . H15 H 0.4674 1.0062 0.9326 0.036 Uiso 1 1 calc R . . C16 C 0.5810(2) 0.94654(16) 0.92802(14) 0.0236(6) Uani 1 1 d . . . H16 H 0.5983 0.9520 0.9690 0.028 Uiso 1 1 calc R . . C17 C 0.6368(2) 0.90536(15) 0.89009(13) 0.0180(6) Uani 1 1 d . . . C18 C 0.7148(2) 0.86864(15) 0.91195(14) 0.0183(6) Uani 1 1 d . . . H18 H 0.7323 0.8731 0.9530 0.022 Uiso 1 1 calc R . . C19 C 0.6369(2) 0.84212(17) 0.72619(14) 0.0242(7) Uani 1 1 d . . . C20 C 0.6851(2) 0.87031(18) 0.67796(14) 0.0264(7) Uani 1 1 d . . . C21 C 0.6565(3) 0.8550(2) 0.61785(15) 0.0361(9) Uani 1 1 d . . . H21 H 0.6883 0.8754 0.5850 0.043 Uiso 1 1 calc R . . C22 C 0.5849(3) 0.8120(2) 0.60676(16) 0.0434(11) Uani 1 1 d . . . H22 H 0.5661 0.8041 0.5664 0.052 Uiso 1 1 calc R . . C23 C 0.5381(3) 0.7789(2) 0.65355(17) 0.0413(10) Uani 1 1 d . . . C24 C 0.4690(3) 0.7291(3) 0.6437(2) 0.0575(14) Uani 1 1 d . . . H24 H 0.4522 0.7180 0.6035 0.069 Uiso 1 1 calc R . . C25 C 0.4262(3) 0.6968(3) 0.6896(2) 0.0610(15) Uani 1 1 d . . . H25 H 0.3807 0.6633 0.6813 0.073 Uiso 1 1 calc R . . C26 C 0.4489(3) 0.7125(3) 0.7501(2) 0.0493(11) Uani 1 1 d . . . H26 H 0.4189 0.6897 0.7823 0.059 Uiso 1 1 calc R . . C27 C 0.5148(2) 0.7610(2) 0.76157(17) 0.0360(9) Uani 1 1 d . . . H27 H 0.5286 0.7722 0.8022 0.043 Uiso 1 1 calc R . . C28 C 0.5625(2) 0.7946(2) 0.71501(16) 0.0317(8) Uani 1 1 d . . . C29 C 0.7692(2) 0.91343(17) 0.68422(15) 0.0266(7) Uani 1 1 d . . . C30 C 0.8460(3) 0.90378(18) 0.64582(15) 0.0283(7) Uani 1 1 d . . . H30 H 0.8436 0.8688 0.6169 0.034 Uiso 1 1 calc R . . C31 C 0.9246(3) 0.94331(17) 0.64868(14) 0.0285(7) Uani 1 1 d . . . H31 H 0.9750 0.9360 0.6214 0.034 Uiso 1 1 calc R . . C32 C 0.9310(3) 0.99432(18) 0.69152(17) 0.0341(8) Uani 1 1 d . . . H32 H 0.9857 1.0214 0.6944 0.041 Uiso 1 1 calc R . . C33 C 0.8554(3) 1.00429(17) 0.72957(17) 0.0390(10) Uani 1 1 d . . . H33 H 0.8587 1.0390 0.7587 0.047 Uiso 1 1 calc R . . C34 C 0.7758(3) 0.96556(18) 0.72654(16) 0.0341(8) Uani 1 1 d . . . H34 H 0.7250 0.9740 0.7532 0.041 Uiso 1 1 calc R . . C35 C 1.0886(2) 0.74069(14) 0.86075(13) 0.0162(5) Uani 1 1 d . . . H35 H 1.1119 0.7875 0.8553 0.019 Uiso 1 1 calc R . . C36 C 1.1689(2) 0.69868(15) 0.88557(13) 0.0181(6) Uani 1 1 d . . . C37 C 1.2557(2) 0.72723(18) 0.89794(15) 0.0249(7) Uani 1 1 d . . . H37 H 1.2642 0.7741 0.8936 0.030 Uiso 1 1 calc R . . C38 C 1.3299(2) 0.6874(2) 0.91658(17) 0.0347(8) Uani 1 1 d . . . H38 H 1.3887 0.7073 0.9258 0.042 Uiso 1 1 calc R . . C39 C 1.3190(3) 0.61978(19) 0.92181(16) 0.0320(8) Uani 1 1 d . . . H39 H 1.3708 0.5927 0.9334 0.038 Uiso 1 1 calc R . . C40 C 1.2329(3) 0.59063(18) 0.91033(16) 0.0295(7) Uani 1 1 d . . . H40 H 1.2254 0.5436 0.9143 0.035 Uiso 1 1 calc R . . C41 C 1.1579(2) 0.62977(17) 0.89317(14) 0.0231(7) Uani 1 1 d . . . H41 H 1.0983 0.6097 0.8865 0.028 Uiso 1 1 calc R . . C42 C 1.1255(2) 0.72561(15) 0.75276(13) 0.0176(6) Uani 1 1 d . . . H42A H 1.1885 0.7119 0.7670 0.021 Uiso 1 1 calc R . . H42B H 1.1283 0.7737 0.7423 0.021 Uiso 1 1 calc R . . C43 C 1.1003(2) 0.68593(14) 0.69755(13) 0.0163(6) Uani 1 1 d . . . C44 C 1.0094(2) 0.69478(14) 0.67030(13) 0.0161(6) Uani 1 1 d . . . C45 C 0.9893(2) 0.66103(15) 0.61696(13) 0.0162(6) Uani 1 1 d . . . C46 C 1.0545(2) 0.61524(14) 0.59191(14) 0.0182(6) Uani 1 1 d . . . C47 C 1.0367(2) 0.57984(16) 0.53771(14) 0.0247(7) Uani 1 1 d . . . H47 H 0.9795 0.5872 0.5168 0.030 Uiso 1 1 calc R . . C48 C 1.1006(3) 0.53520(16) 0.51498(14) 0.0265(7) Uani 1 1 d . . . H48 H 1.0873 0.5125 0.4784 0.032 Uiso 1 1 calc R . . C49 C 1.1848(2) 0.52272(16) 0.54483(15) 0.0253(7) Uani 1 1 d . . . H49 H 1.2283 0.4914 0.5288 0.030 Uiso 1 1 calc R . . C50 C 1.2050(2) 0.55583(15) 0.59748(14) 0.0209(6) Uani 1 1 d . . . H50 H 1.2619 0.5464 0.6182 0.025 Uiso 1 1 calc R . . C51 C 1.1420(2) 0.60372(15) 0.62116(13) 0.0181(6) Uani 1 1 d . . . C52 C 1.1625(2) 0.64131(15) 0.67419(13) 0.0185(6) Uani 1 1 d . . . H52 H 1.2212 0.6350 0.6937 0.022 Uiso 1 1 calc R . . C53 C 0.8995(2) 0.67613(14) 0.58426(13) 0.0178(6) Uani 1 1 d . . . C54 C 0.8244(2) 0.63222(16) 0.58188(14) 0.0231(6) Uani 1 1 d . . . C55 C 0.7424(2) 0.65056(19) 0.54843(17) 0.0310(8) Uani 1 1 d . . . H55 H 0.6907 0.6205 0.5471 0.037 Uiso 1 1 calc R . . C56 C 0.7365(2) 0.70924(18) 0.51880(16) 0.0302(8) Uani 1 1 d . . . H56 H 0.6806 0.7201 0.4976 0.036 Uiso 1 1 calc R . . C57 C 0.8122(2) 0.75483(18) 0.51871(13) 0.0230(6) Uani 1 1 d . . . C58 C 0.8083(3) 0.81687(17) 0.48726(15) 0.0269(7) Uani 1 1 d . . . H58 H 0.7526 0.8290 0.4664 0.032 Uiso 1 1 calc R . . C59 C 0.8837(3) 0.85921(17) 0.48674(14) 0.0269(7) Uani 1 1 d . . . H59 H 0.8801 0.9005 0.4657 0.032 Uiso 1 1 calc R . . C60 C 0.9663(2) 0.84188(17) 0.51720(15) 0.0248(7) Uani 1 1 d . . . H60 H 1.0189 0.8710 0.5158 0.030 Uiso 1 1 calc R . . C61 C 0.9720(2) 0.78294(15) 0.54920(14) 0.0202(6) Uani 1 1 d . . . H61 H 1.0282 0.7723 0.5701 0.024 Uiso 1 1 calc R . . C62 C 0.8952(2) 0.73821(15) 0.55127(13) 0.0196(6) Uani 1 1 d . . . C63 C 0.8246(2) 0.56541(17) 0.61114(15) 0.0250(7) Uani 1 1 d . . . C64 C 0.8542(2) 0.55560(18) 0.67026(16) 0.0280(7) Uani 1 1 d . . . H64 H 0.8793 0.5920 0.6926 0.034 Uiso 1 1 calc R . . C65 C 0.8470(3) 0.49258(18) 0.69685(18) 0.0344(8) Uani 1 1 d . . . H65 H 0.8662 0.4866 0.7374 0.041 Uiso 1 1 calc R . . C66 C 0.8124(3) 0.4389(2) 0.6647(2) 0.0435(10) Uani 1 1 d . . . H66 H 0.8075 0.3962 0.6832 0.052 Uiso 1 1 calc R . . C67 C 0.7847(3) 0.44757(19) 0.6056(2) 0.0414(10) Uani 1 1 d . . . H67 H 0.7619 0.4104 0.5832 0.050 Uiso 1 1 calc R . . C68 C 0.7900(3) 0.51000(18) 0.57873(18) 0.0348(8) Uani 1 1 d . . . H68 H 0.7703 0.5155 0.5382 0.042 Uiso 1 1 calc R . . C69 C 0.8049(3) 0.62733(16) 0.80771(15) 0.0278(7) Uani 1 1 d . . . C70 C 0.7846(3) 0.57946(18) 0.85045(16) 0.0295(8) Uani 1 1 d . . . C71 C 0.6981(3) 0.54368(19) 0.85348(19) 0.0403(10) Uani 1 1 d . . . C72 C 0.6785(4) 0.4931(2) 0.8962(2) 0.0540(13) Uani 1 1 d . . . H72 H 0.7250 0.4798 0.9244 0.065 Uiso 1 1 calc R . . C73 C 0.5903(5) 0.4629(2) 0.8965(3) 0.080(2) Uani 1 1 d . . . H73 H 0.5770 0.4285 0.9248 0.097 Uiso 1 1 calc R . . C74 C 0.5184(4) 0.4836(3) 0.8539(3) 0.0685(18) Uani 1 1 d . . . H74 H 0.4576 0.4641 0.8553 0.082 Uiso 1 1 calc R . . C75 C 0.5378(3) 0.5287(3) 0.8141(3) 0.0617(15) Uani 1 1 d . . . H75 H 0.4904 0.5414 0.7863 0.074 Uiso 1 1 calc R . . C76 C 0.6281(3) 0.5606(2) 0.81019(19) 0.0420(10) Uani 1 1 d . . . C77 C 0.6471(3) 0.6085(2) 0.76628(19) 0.0400(10) Uani 1 1 d . . . H77 H 0.6004 0.6187 0.7371 0.048 Uiso 1 1 calc R . . C78 C 0.7314(2) 0.64113(19) 0.76440(17) 0.0319(8) Uani 1 1 d . . . H78 H 0.7421 0.6736 0.7339 0.038 Uiso 1 1 calc R . . C79 C 0.7344(3) 0.3275(2) 0.85022(19) 0.0411(9) Uani 1 1 d . . . H79A H 0.6918 0.3385 0.8840 0.049 Uiso 1 1 calc R . . H79B H 0.7405 0.2782 0.8482 0.049 Uiso 1 1 calc R . . Br1 Br 0.87792(3) 0.563630(19) 0.910713(17) 0.03882(10) Uani 1 1 d . . . Cl1 Cl 0.68567(7) 0.35740(6) 0.78224(5) 0.0491(3) Uani 1 1 d . . . Cl2 Cl 0.84538(7) 0.36330(6) 0.86329(5) 0.0479(3) Uani 1 1 d . . . H1N1 H 0.948(3) 0.823(2) 0.8745(17) 0.025(10) Uiso 1 1 d . . . H2N2 H 1.042(3) 0.677(2) 0.8044(17) 0.022(10) Uiso 1 1 d . . . H4OA H 0.967(3) 0.876(2) 0.782(2) 0.028(11) Uiso 1 1 d . . . H4OB H 0.970(3) 0.860(2) 0.728(2) 0.034(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01271(17) 0.01902(19) 0.01224(18) -0.00193(17) -0.00094(15) 0.00223(17) O1 0.0147(9) 0.0287(11) 0.0135(10) -0.0056(9) -0.0016(8) 0.0058(8) O2 0.0170(9) 0.0238(11) 0.0147(10) -0.0043(8) -0.0016(8) 0.0051(8) O3 0.0188(10) 0.0315(12) 0.0195(10) -0.0072(9) -0.0027(9) 0.0089(9) O4 0.0289(12) 0.0202(12) 0.0171(12) -0.0005(10) 0.0026(9) 0.0032(10) O5 0.0341(13) 0.0270(12) 0.0321(13) -0.0036(11) 0.0025(11) 0.0021(11) N1 0.0143(12) 0.0196(13) 0.0154(12) -0.0021(10) -0.0023(10) 0.0016(10) N2 0.0148(12) 0.0166(13) 0.0128(12) -0.0005(10) -0.0009(9) -0.0001(9) C1 0.0150(12) 0.0205(14) 0.0132(13) 0.0002(11) -0.0020(10) 0.0002(11) C2 0.0138(13) 0.0295(16) 0.0155(15) -0.0039(12) -0.0016(11) 0.0074(11) C3 0.0301(18) 0.0355(19) 0.0229(17) -0.0045(14) -0.0031(14) -0.0070(15) C4 0.036(2) 0.045(2) 0.035(2) -0.0154(17) -0.0044(17) -0.0085(18) C5 0.0262(17) 0.061(2) 0.0216(17) -0.0139(16) -0.0127(15) 0.0117(18) C6 0.0360(19) 0.049(2) 0.0176(15) -0.0047(16) -0.0048(13) 0.0257(18) C7 0.0320(18) 0.0318(17) 0.0203(16) -0.0026(13) -0.0023(14) 0.0143(14) C8 0.0155(13) 0.0243(15) 0.0150(14) -0.0007(12) 0.0004(11) -0.0004(11) C9 0.0130(13) 0.0208(15) 0.0164(14) 0.0016(11) 0.0014(11) -0.0013(11) C10 0.0135(13) 0.0238(15) 0.0162(14) -0.0003(12) -0.0008(11) -0.0010(11) C11 0.0176(14) 0.0278(16) 0.0132(14) -0.0027(12) -0.0012(11) 0.0027(12) C12 0.0159(14) 0.0285(16) 0.0178(14) 0.0007(12) 0.0038(12) 0.0037(12) C13 0.0268(17) 0.041(2) 0.0210(16) -0.0004(15) -0.0024(13) 0.0125(15) C14 0.0295(19) 0.041(2) 0.031(2) 0.0017(16) 0.0019(15) 0.0181(16) C15 0.0274(17) 0.0362(19) 0.0271(17) -0.0055(15) 0.0099(15) 0.0115(14) C16 0.0223(15) 0.0286(16) 0.0198(15) -0.0018(12) 0.0015(13) -0.0001(14) C17 0.0146(14) 0.0221(14) 0.0173(14) -0.0009(11) 0.0024(11) -0.0005(11) C18 0.0174(13) 0.0248(15) 0.0126(13) -0.0025(12) -0.0001(12) -0.0034(11) C19 0.0197(15) 0.0377(18) 0.0151(14) -0.0052(13) -0.0012(12) 0.0124(13) C20 0.0269(17) 0.0369(18) 0.0156(15) -0.0031(13) -0.0036(13) 0.0194(14) C21 0.0291(18) 0.064(3) 0.0154(16) -0.0039(16) -0.0007(14) 0.0233(18) C22 0.0275(18) 0.083(3) 0.0197(17) -0.0148(18) -0.0082(15) 0.020(2) C23 0.0205(17) 0.071(3) 0.032(2) -0.0256(19) -0.0073(15) 0.0139(17) C24 0.026(2) 0.100(4) 0.046(3) -0.039(3) -0.0072(19) 0.002(2) C25 0.026(2) 0.086(4) 0.072(3) -0.039(3) -0.008(2) -0.008(2) C26 0.029(2) 0.069(3) 0.050(3) -0.015(2) -0.0005(19) -0.007(2) C27 0.0226(16) 0.051(2) 0.035(2) -0.0097(17) -0.0064(14) 0.0008(16) C28 0.0169(15) 0.055(2) 0.0230(17) -0.0093(16) -0.0050(13) 0.0093(14) C29 0.0342(18) 0.0272(17) 0.0184(16) 0.0044(13) 0.0018(14) 0.0149(14) C30 0.0375(19) 0.0298(17) 0.0176(15) -0.0003(13) 0.0001(14) 0.0119(15) C31 0.0348(18) 0.0315(17) 0.0191(15) 0.0054(13) 0.0055(14) 0.0096(15) C32 0.048(2) 0.0237(17) 0.0309(19) 0.0066(14) -0.0001(17) 0.0043(15) C33 0.070(3) 0.0201(16) 0.0266(19) 0.0006(14) 0.0083(18) 0.0050(17) C34 0.051(2) 0.0284(17) 0.0225(17) 0.0038(15) 0.0145(17) 0.0143(16) C35 0.0167(13) 0.0154(13) 0.0166(13) -0.0010(11) -0.0022(11) 0.0003(11) C36 0.0170(14) 0.0240(15) 0.0133(13) -0.0038(11) -0.0017(11) 0.0043(12) C37 0.0207(15) 0.0310(17) 0.0230(17) -0.0023(13) -0.0044(12) -0.0015(13) C38 0.0185(16) 0.053(2) 0.033(2) 0.0001(17) -0.0073(15) 0.0019(15) C39 0.0282(17) 0.042(2) 0.0256(18) 0.0009(15) -0.0055(14) 0.0159(15) C40 0.0359(18) 0.0293(16) 0.0233(16) -0.0002(14) -0.0034(15) 0.0125(14) C41 0.0225(16) 0.0289(17) 0.0180(15) -0.0008(12) -0.0058(12) 0.0026(13) C42 0.0145(13) 0.0225(14) 0.0157(14) 0.0000(11) -0.0027(12) -0.0005(12) C43 0.0167(14) 0.0186(13) 0.0136(13) 0.0019(11) 0.0039(11) -0.0003(11) C44 0.0194(14) 0.0173(14) 0.0115(13) 0.0010(11) 0.0020(11) 0.0014(11) C45 0.0164(14) 0.0181(14) 0.0140(13) 0.0010(11) 0.0031(11) 0.0012(11) C46 0.0213(14) 0.0192(14) 0.0140(13) 0.0004(12) 0.0048(12) 0.0000(11) C47 0.0291(17) 0.0266(17) 0.0184(15) -0.0016(13) 0.0016(13) 0.0059(13) C48 0.039(2) 0.0217(15) 0.0192(15) -0.0028(12) 0.0037(14) 0.0045(14) C49 0.0302(17) 0.0214(15) 0.0244(16) -0.0001(13) 0.0126(14) 0.0067(13) C50 0.0188(14) 0.0201(14) 0.0240(16) 0.0037(13) 0.0066(12) 0.0052(12) C51 0.0202(15) 0.0181(14) 0.0160(14) 0.0030(11) 0.0072(12) 0.0032(11) C52 0.0173(14) 0.0239(15) 0.0145(14) 0.0054(12) -0.0009(11) -0.0004(12) C53 0.0184(14) 0.0232(14) 0.0118(13) -0.0038(11) 0.0009(11) 0.0048(11) C54 0.0229(15) 0.0258(15) 0.0208(16) -0.0041(13) -0.0002(13) 0.0044(12) C55 0.0210(16) 0.0357(19) 0.0363(19) -0.0066(16) -0.0029(15) -0.0030(14) C56 0.0244(17) 0.0359(19) 0.0303(19) -0.0029(15) -0.0120(14) 0.0084(14) C57 0.0229(15) 0.0302(16) 0.0160(14) -0.0044(13) -0.0027(11) 0.0078(14) C58 0.0297(17) 0.0324(18) 0.0187(16) 0.0001(13) -0.0026(13) 0.0126(14) C59 0.0354(18) 0.0276(16) 0.0176(15) 0.0041(13) 0.0064(14) 0.0078(15) C60 0.0246(16) 0.0276(17) 0.0222(16) 0.0006(13) 0.0077(13) 0.0031(13) C61 0.0211(15) 0.0249(15) 0.0146(14) 0.0004(12) 0.0025(12) 0.0063(12) C62 0.0208(15) 0.0260(16) 0.0121(13) -0.0030(11) 0.0008(11) 0.0046(12) C63 0.0198(15) 0.0251(16) 0.0299(17) -0.0042(14) 0.0055(13) -0.0024(13) C64 0.0266(17) 0.0277(17) 0.0299(17) -0.0022(14) 0.0051(14) 0.0026(14) C65 0.037(2) 0.0297(18) 0.037(2) 0.0049(15) 0.0114(16) 0.0035(15) C66 0.044(2) 0.0246(18) 0.062(3) 0.0035(19) 0.020(2) 0.0031(17) C67 0.044(2) 0.0260(19) 0.054(3) -0.0102(17) 0.0137(19) -0.0058(16) C68 0.036(2) 0.0312(18) 0.038(2) -0.0061(16) 0.0039(16) -0.0041(15) C69 0.041(2) 0.0199(15) 0.0223(16) -0.0087(13) 0.0120(15) -0.0015(14) C70 0.0309(18) 0.0288(18) 0.0289(18) -0.0098(14) 0.0073(14) -0.0012(14) C71 0.044(2) 0.0320(19) 0.045(2) -0.0211(17) 0.0270(19) -0.0168(16) C72 0.074(3) 0.042(2) 0.046(3) -0.020(2) 0.034(2) -0.021(2) C73 0.122(5) 0.049(3) 0.071(4) -0.033(3) 0.078(4) -0.053(3) C74 0.062(3) 0.083(4) 0.061(3) -0.040(3) 0.034(3) -0.048(3) C75 0.042(3) 0.067(3) 0.076(3) -0.044(3) 0.025(2) -0.029(2) C76 0.0273(18) 0.048(2) 0.051(2) -0.029(2) 0.0134(18) -0.0129(18) C77 0.0278(18) 0.045(2) 0.047(2) -0.0245(19) -0.0030(16) -0.0006(16) C78 0.0232(17) 0.0337(19) 0.039(2) -0.0122(16) 0.0015(14) -0.0016(14) C79 0.036(2) 0.047(2) 0.040(2) 0.0002(18) 0.0015(18) -0.0051(18) Br1 0.0511(2) 0.03080(18) 0.0345(2) 0.00486(15) 0.00403(18) -0.00400(17) Cl1 0.0378(5) 0.0668(7) 0.0428(6) -0.0048(5) -0.0040(5) 0.0040(5) Cl2 0.0350(5) 0.0558(6) 0.0529(6) -0.0095(5) -0.0056(5) -0.0005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.872(2) . ? Fe1 O2 1.927(2) . ? Fe1 O3 1.975(2) . ? Fe1 N2 2.171(2) . ? Fe1 N1 2.202(2) . ? Fe1 O4 2.214(2) . ? O1 C10 1.320(4) . ? O2 C44 1.324(4) . ? O3 C69 1.281(4) . ? O4 H4OA 0.72(4) . ? O4 H4OB 0.82(5) . ? N1 C8 1.478(4) . ? N1 C1 1.491(4) . ? N1 H1N1 0.84(4) . ? N2 C42 1.471(4) . ? N2 C35 1.482(4) . ? N2 H2N2 0.80(4) . ? C1 C2 1.519(4) . ? C1 C35 1.534(4) . ? C1 H1 1.0000 . ? C2 C7 1.386(5) . ? C2 C3 1.396(5) . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.395(6) . ? C4 H4A 0.9500 . ? C5 C6 1.357(6) . ? C5 H5 0.9500 . ? C6 C7 1.394(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.517(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C18 1.362(4) . ? C9 C10 1.436(4) . ? C10 C11 1.399(4) . ? C11 C12 1.417(4) . ? C11 C19 1.499(4) . ? C12 C13 1.415(4) . ? C12 C17 1.435(4) . ? C13 C14 1.366(5) . ? C13 H13 0.9500 . ? C14 C15 1.413(5) . ? C14 H14 0.9500 . ? C15 C16 1.360(5) . ? C15 H15 0.9500 . ? C16 C17 1.421(4) . ? C16 H16 0.9500 . ? C17 C18 1.416(4) . ? C18 H18 0.9500 . ? C19 C20 1.392(5) . ? C19 C28 1.444(5) . ? C20 C21 1.429(5) . ? C20 C29 1.481(5) . ? C21 C22 1.356(6) . ? C21 H21 0.9500 . ? C22 C23 1.400(6) . ? C22 H22 0.9500 . ? C23 C24 1.417(7) . ? C23 C28 1.443(5) . ? C24 C25 1.352(8) . ? C24 H24 0.9500 . ? C25 C26 1.417(7) . ? C25 H25 0.9500 . ? C26 C27 1.373(6) . ? C26 H26 0.9500 . ? C27 C28 1.408(6) . ? C27 H27 0.9500 . ? C29 C30 1.400(5) . ? C29 C34 1.406(5) . ? C30 C31 1.371(5) . ? C30 H30 0.9500 . ? C31 C32 1.398(5) . ? C31 H31 0.9500 . ? C32 C33 1.382(6) . ? C32 H32 0.9500 . ? C33 C34 1.374(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.522(4) . ? C35 H35 1.0000 . ? C36 C37 1.389(4) . ? C36 C41 1.396(5) . ? C37 C38 1.386(5) . ? C37 H37 0.9500 . ? C38 C39 1.365(6) . ? C38 H38 0.9500 . ? C39 C40 1.381(5) . ? C39 H39 0.9500 . ? C40 C41 1.378(5) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.504(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C52 1.359(4) . ? C43 C44 1.440(4) . ? C44 C45 1.393(4) . ? C45 C46 1.417(4) . ? C45 C53 1.501(4) . ? C46 C47 1.419(4) . ? C46 C51 1.423(4) . ? C47 C48 1.370(4) . ? C47 H47 0.9500 . ? C48 C49 1.393(5) . ? C48 H48 0.9500 . ? C49 C50 1.374(5) . ? C49 H49 0.9500 . ? C50 C51 1.413(4) . ? C50 H50 0.9500 . ? C51 C52 1.428(4) . ? C52 H52 0.9500 . ? C53 C54 1.385(4) . ? C53 C62 1.442(4) . ? C54 C55 1.432(5) . ? C54 C63 1.485(5) . ? C55 C56 1.347(5) . ? C55 H55 0.9500 . ? C56 C57 1.411(5) . ? C56 H56 0.9500 . ? C57 C58 1.424(5) . ? C57 C62 1.425(4) . ? C58 C59 1.368(5) . ? C58 H58 0.9500 . ? C59 C60 1.400(5) . ? C59 H59 0.9500 . ? C60 C61 1.378(5) . ? C60 H60 0.9500 . ? C61 C62 1.412(4) . ? C61 H61 0.9500 . ? C63 C64 1.393(5) . ? C63 C68 1.409(5) . ? C64 C65 1.395(5) . ? C64 H64 0.9500 . ? C65 C66 1.379(6) . ? C65 H65 0.9500 . ? C66 C67 1.383(6) . ? C66 H66 0.9500 . ? C67 C68 1.385(6) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.378(5) . ? C69 C78 1.448(5) . ? C70 C71 1.426(5) . ? C70 Br1 1.912(4) . ? C71 C72 1.414(6) . ? C71 C76 1.426(6) . ? C72 C73 1.393(8) . ? C72 H72 0.9500 . ? C73 C74 1.453(9) . ? C73 H73 0.9500 . ? C74 C75 1.293(8) . ? C74 H74 0.9500 . ? C75 C76 1.436(5) . ? C75 H75 0.9500 . ? C76 C77 1.394(6) . ? C77 C78 1.367(5) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 Cl2 1.759(4) . ? C79 Cl1 1.766(4) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 103.80(9) . . ? O1 Fe1 O3 98.80(9) . . ? O2 Fe1 O3 102.55(9) . . ? O1 Fe1 N2 167.09(9) . . ? O2 Fe1 N2 88.57(9) . . ? O3 Fe1 N2 81.76(9) . . ? O1 Fe1 N1 88.94(9) . . ? O2 Fe1 N1 159.17(10) . . ? O3 Fe1 N1 91.47(9) . . ? N2 Fe1 N1 78.16(9) . . ? O1 Fe1 O4 91.84(9) . . ? O2 Fe1 O4 82.80(10) . . ? O3 Fe1 O4 166.48(9) . . ? N2 Fe1 O4 86.00(10) . . ? N1 Fe1 O4 80.35(10) . . ? C10 O1 Fe1 135.27(19) . . ? C44 O2 Fe1 129.19(18) . . ? C69 O3 Fe1 130.2(2) . . ? Fe1 O4 H4OA 120(3) . . ? Fe1 O4 H4OB 109(3) . . ? H4OA O4 H4OB 107(4) . . ? C8 N1 C1 112.8(2) . . ? C8 N1 Fe1 110.18(18) . . ? C1 N1 Fe1 108.73(17) . . ? C8 N1 H1N1 107(3) . . ? C1 N1 H1N1 105(3) . . ? Fe1 N1 H1N1 113(3) . . ? C42 N2 C35 113.8(2) . . ? C42 N2 Fe1 113.58(18) . . ? C35 N2 Fe1 112.86(17) . . ? C42 N2 H2N2 112(3) . . ? C35 N2 H2N2 109(3) . . ? Fe1 N2 H2N2 94(3) . . ? N1 C1 C2 113.7(2) . . ? N1 C1 C35 107.4(2) . . ? C2 C1 C35 111.0(2) . . ? N1 C1 H1 108.2 . . ? C2 C1 H1 108.2 . . ? C35 C1 H1 108.2 . . ? C7 C2 C3 118.7(3) . . ? C7 C2 C1 120.2(3) . . ? C3 C2 C1 121.0(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.9(4) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 120.0(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.5(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C2 C7 C6 120.5(3) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? N1 C8 C9 112.7(2) . . ? N1 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C18 C9 C10 120.3(3) . . ? C18 C9 C8 120.1(3) . . ? C10 C9 C8 119.2(3) . . ? O1 C10 C11 119.5(3) . . ? O1 C10 C9 121.2(3) . . ? C11 C10 C9 119.2(3) . . ? C10 C11 C12 120.4(3) . . ? C10 C11 C19 117.8(3) . . ? C12 C11 C19 121.8(3) . . ? C13 C12 C11 122.7(3) . . ? C13 C12 C17 117.7(3) . . ? C11 C12 C17 119.6(3) . . ? C14 C13 C12 121.6(3) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 120.6(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.8(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.3(3) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 122.3(3) . . ? C18 C17 C12 118.5(3) . . ? C16 C17 C12 119.1(3) . . ? C9 C18 C17 121.8(3) . . ? C9 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C20 C19 C28 119.7(3) . . ? C20 C19 C11 122.3(3) . . ? C28 C19 C11 117.8(3) . . ? C19 C20 C21 119.5(3) . . ? C19 C20 C29 124.2(3) . . ? C21 C20 C29 116.3(3) . . ? C22 C21 C20 121.3(4) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 121.5(3) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C22 C23 C24 123.2(4) . . ? C22 C23 C28 119.0(4) . . ? C24 C23 C28 117.8(4) . . ? C25 C24 C23 122.1(4) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C24 C25 C26 120.5(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 119.2(5) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 122.0(4) . . ? C26 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? C27 C28 C23 118.4(4) . . ? C27 C28 C19 122.7(3) . . ? C23 C28 C19 118.8(3) . . ? C30 C29 C34 117.2(3) . . ? C30 C29 C20 119.6(3) . . ? C34 C29 C20 123.2(3) . . ? C31 C30 C29 122.0(3) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 120.3(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 118.1(4) . . ? C33 C32 H32 120.9 . . ? C31 C32 H32 120.9 . . ? C34 C33 C32 122.1(3) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C33 C34 C29 120.4(3) . . ? C33 C34 H34 119.8 . . ? C29 C34 H34 119.8 . . ? N2 C35 C36 111.5(2) . . ? N2 C35 C1 108.0(2) . . ? C36 C35 C1 113.1(2) . . ? N2 C35 H35 108.1 . . ? C36 C35 H35 108.1 . . ? C1 C35 H35 108.1 . . ? C37 C36 C41 118.8(3) . . ? C37 C36 C35 120.9(3) . . ? C41 C36 C35 120.2(3) . . ? C38 C37 C36 120.1(3) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C39 C38 C37 120.5(3) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C38 C39 C40 120.1(3) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C41 C40 C39 120.0(3) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C36 120.4(3) . . ? C40 C41 H41 119.8 . . ? C36 C41 H41 119.8 . . ? N2 C42 C43 111.6(2) . . ? N2 C42 H42A 109.3 . . ? C43 C42 H42A 109.3 . . ? N2 C42 H42B 109.3 . . ? C43 C42 H42B 109.3 . . ? H42A C42 H42B 108.0 . . ? C52 C43 C44 120.4(3) . . ? C52 C43 C42 120.1(3) . . ? C44 C43 C42 119.5(2) . . ? O2 C44 C45 120.6(3) . . ? O2 C44 C43 120.5(3) . . ? C45 C44 C43 118.8(3) . . ? C44 C45 C46 120.8(3) . . ? C44 C45 C53 119.3(3) . . ? C46 C45 C53 119.8(3) . . ? C45 C46 C47 122.6(3) . . ? C45 C46 C51 119.9(3) . . ? C47 C46 C51 117.6(3) . . ? C48 C47 C46 121.2(3) . . ? C48 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? C47 C48 C49 120.8(3) . . ? C47 C48 H48 119.6 . . ? C49 C48 H48 119.6 . . ? C50 C49 C48 119.9(3) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 120.7(3) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? C50 C51 C46 119.7(3) . . ? C50 C51 C52 122.2(3) . . ? C46 C51 C52 118.1(3) . . ? C43 C52 C51 121.8(3) . . ? C43 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? C54 C53 C62 119.5(3) . . ? C54 C53 C45 123.3(3) . . ? C62 C53 C45 117.1(3) . . ? C53 C54 C55 119.2(3) . . ? C53 C54 C63 123.4(3) . . ? C55 C54 C63 117.4(3) . . ? C56 C55 C54 121.8(3) . . ? C56 C55 H55 119.1 . . ? C54 C55 H55 119.1 . . ? C55 C56 C57 121.0(3) . . ? C55 C56 H56 119.5 . . ? C57 C56 H56 119.5 . . ? C56 C57 C58 122.2(3) . . ? C56 C57 C62 118.8(3) . . ? C58 C57 C62 119.0(3) . . ? C59 C58 C57 120.8(3) . . ? C59 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C58 C59 C60 120.2(3) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C61 C60 C59 120.7(3) . . ? C61 C60 H60 119.7 . . ? C59 C60 H60 119.7 . . ? C60 C61 C62 120.8(3) . . ? C60 C61 H61 119.6 . . ? C62 C61 H61 119.6 . . ? C61 C62 C57 118.5(3) . . ? C61 C62 C53 121.9(3) . . ? C57 C62 C53 119.6(3) . . ? C64 C63 C68 118.5(3) . . ? C64 C63 C54 122.7(3) . . ? C68 C63 C54 118.8(3) . . ? C63 C64 C65 120.3(3) . . ? C63 C64 H64 119.9 . . ? C65 C64 H64 119.9 . . ? C66 C65 C64 120.6(4) . . ? C66 C65 H65 119.7 . . ? C64 C65 H65 119.7 . . ? C65 C66 C67 119.7(4) . . ? C65 C66 H66 120.1 . . ? C67 C66 H66 120.1 . . ? C66 C67 C68 120.4(4) . . ? C66 C67 H67 119.8 . . ? C68 C67 H67 119.8 . . ? C67 C68 C63 120.5(4) . . ? C67 C68 H68 119.8 . . ? C63 C68 H68 119.8 . . ? O3 C69 C70 122.6(4) . . ? O3 C69 C78 121.4(3) . . ? C70 C69 C78 116.0(3) . . ? C69 C70 C71 124.1(4) . . ? C69 C70 Br1 116.9(3) . . ? C71 C70 Br1 118.9(3) . . ? C72 C71 C70 124.1(4) . . ? C72 C71 C76 118.9(4) . . ? C70 C71 C76 117.0(4) . . ? C73 C72 C71 119.4(6) . . ? C73 C72 H72 120.3 . . ? C71 C72 H72 120.3 . . ? C72 C73 C74 120.5(5) . . ? C72 C73 H73 119.7 . . ? C74 C73 H73 119.7 . . ? C75 C74 C73 119.5(5) . . ? C75 C74 H74 120.2 . . ? C73 C74 H74 120.2 . . ? C74 C75 C76 122.8(6) . . ? C74 C75 H75 118.6 . . ? C76 C75 H75 118.6 . . ? C77 C76 C71 120.0(3) . . ? C77 C76 C75 121.4(5) . . ? C71 C76 C75 118.6(4) . . ? C78 C77 C76 121.3(4) . . ? C78 C77 H77 119.4 . . ? C76 C77 H77 119.4 . . ? C77 C78 C69 121.6(4) . . ? C77 C78 H78 119.2 . . ? C69 C78 H78 119.2 . . ? Cl2 C79 Cl1 110.9(2) . . ? Cl2 C79 H79A 109.5 . . ? Cl1 C79 H79A 109.5 . . ? Cl2 C79 H79B 109.5 . . ? Cl1 C79 H79B 109.5 . . ? H79A C79 H79B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.866 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.071 # Attachment '8256_web_deposit_cif_file_5_KenjiMatsumoto_1321546181.complex9_[(L3)Fe(OH)(6Br2NpO)(L3)]_KM117_final.cif' data_LFe_OH_6Br2NpO_FeL_KM117 _database_code_depnum_ccdc_archive 'CCDC 854411' #TrackingRef '8256_web_deposit_cif_file_5_KenjiMatsumoto_1321546181.complex9_[(L3)Fe(OH)(6Br2NpO)(L3)]_KM117_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'CC106H83Br1Fe2N4O6, 0.5(C10H7Br1O1)' _chemical_formula_sum 'C111 H86.50 Br1.50 Fe2 N4 O6.50' _chemical_formula_weight 1811.91 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.6693(14) _cell_length_b 25.349(3) _cell_length_c 27.020(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9362.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9864 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 24.90 _exptl_crystal_description block _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3748 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7006 _exptl_absorpt_correction_T_max 0.9237 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 'focusing mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 53205 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.50 _reflns_number_total 21307 _reflns_number_gt 15976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1937P)^2^+24.9252P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 21307 _refine_ls_number_parameters 1111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1372 _refine_ls_R_factor_gt 0.1061 _refine_ls_wR_factor_ref 0.3152 _refine_ls_wR_factor_gt 0.2848 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C4X C 0.2237(7) -0.0897(4) -0.0033(3) 0.113(6) Uani 1 1 d G . . C7Y C 0.1598(9) -0.1296(5) -0.0176(3) 0.11(2) Uiso 0.291(4) 1 d PG A 2 C8Y C 0.1249(7) -0.1652(4) 0.0173(3) 0.060(8) Uiso 0.291(4) 1 d PG A 2 C9Y C 0.1538(5) -0.1610(3) 0.0664(3) 0.069(9) Uiso 0.291(4) 1 d PG A 2 C10Y C 0.2177(7) -0.1212(4) 0.0807(3) 0.045(6) Uiso 0.291(4) 1 d PG A 2 C3X C 0.2526(7) -0.0855(4) 0.0459(3) 0.086(4) Uani 1 1 d G A . C9Z C -0.2331(6) -0.3071(4) 0.1344(4) 0.051(4) Uiso 0.50 1 d PG A 4 C4Z C -0.1628(7) -0.3202(4) 0.1695(4) 0.050(4) Uiso 0.50 1 d PG A 4 C3Z C -0.0645(7) -0.3212(4) 0.1565(4) 0.073(6) Uiso 0.50 1 d PG A 4 C2Z C -0.0363(7) -0.3092(3) 0.1084(4) 0.091(7) Uiso 0.50 1 d PG A 4 C1Z C -0.1066(8) -0.2961(4) 0.0733(3) 0.086(7) Uiso 0.50 1 d PG A 4 C10Z C -0.2049(7) -0.2950(5) 0.0863(4) 0.136(13) Uiso 0.50 1 d PG A 4 Br1Y Br 0.0348(3) -0.21697(16) 0.00080(15) 0.0744(14) Uiso 0.291(4) 1 d P A 2 Fe1 Fe 0.58742(7) 0.01918(4) 0.00698(3) 0.0295(2) Uani 1 1 d . . . Fe2 Fe 0.48181(6) 0.04558(4) 0.10692(3) 0.0269(2) Uani 1 1 d . . . N1 N 0.6584(4) -0.0486(2) 0.0447(2) 0.0310(11) Uani 1 1 d . . . N2 N 0.7396(4) 0.0326(2) -0.0105(2) 0.0351(12) Uani 1 1 d . . . N3 N 0.4401(4) 0.1194(2) 0.0716(2) 0.0303(11) Uani 1 1 d . . . N4 N 0.5228(4) 0.1052(2) 0.1632(2) 0.0306(11) Uani 1 1 d . . . O1 O 0.5734(4) -0.0263(2) -0.04831(16) 0.0347(10) Uani 1 1 d . . . O2 O 0.5507(3) 0.0863(2) -0.02150(18) 0.0359(11) Uani 1 1 d . . . O3 O 0.3532(3) 0.0379(2) 0.13171(19) 0.0344(10) Uani 1 1 d . . . O4 O 0.5561(3) -0.00585(17) 0.14375(17) 0.0302(10) Uani 1 1 d . . . O5 O 0.4607(3) 0.00535(19) 0.04233(17) 0.0322(10) Uani 1 1 d . . . O6 O 0.6108(3) 0.05962(18) 0.07194(17) 0.0309(10) Uani 1 1 d . . . O1Z O -0.3213(10) -0.3593(5) 0.2768(5) 0.055(3) Uiso 0.50 1 d P . . Br1X Br -0.0162(3) -0.13589(16) -0.09152(13) 0.186(2) Uani 0.709(4) 1 d P A 1 Br1Z Br -0.0629(4) -0.2636(2) 0.01285(19) 0.1413(15) Uiso 0.50 1 d P . . C1 C 0.7681(5) -0.0461(3) 0.0400(2) 0.0340(14) Uani 1 1 d . . . H1 H 0.7860 -0.0668 0.0098 0.041 Uiso 1 1 calc R . . C2 C 0.8176(6) -0.0720(4) 0.0826(3) 0.053(2) Uani 1 1 d . . . C3 C 0.8667(11) -0.1185(5) 0.0756(6) 0.098(5) Uani 1 1 d . . . H3 H 0.8706 -0.1347 0.0440 0.118 Uiso 1 1 calc R . . C4 C 0.912(2) -0.1418(7) 0.1185(12) 0.183(13) Uani 1 1 d . . . H4 H 0.9510 -0.1727 0.1147 0.219 Uiso 1 1 calc R . . C5 C 0.9008(15) -0.1204(8) 0.1646(7) 0.143(10) Uani 1 1 d . . . H5 H 0.9239 -0.1388 0.1929 0.172 Uiso 1 1 calc R . . C6 C 0.8555(10) -0.0720(8) 0.1700(5) 0.099(5) Uani 1 1 d . . . H6 H 0.8547 -0.0542 0.2009 0.119 Uiso 1 1 calc R . . C7 C 0.8127(8) -0.0512(6) 0.1297(3) 0.076(3) Uani 1 1 d . . . H7 H 0.7763 -0.0196 0.1340 0.091 Uiso 1 1 calc R . . C8 C 0.6177(6) -0.0997(3) 0.0269(3) 0.0364(15) Uani 1 1 d . . . H8A H 0.5457 -0.0995 0.0308 0.044 Uiso 1 1 calc R . . H8B H 0.6443 -0.1289 0.0472 0.044 Uiso 1 1 calc R . . C9 C 0.6429(6) -0.1087(3) -0.0264(3) 0.0389(16) Uani 1 1 d . . . C10 C 0.6193(5) -0.0687(3) -0.0619(3) 0.0364(15) Uani 1 1 d . . . C11 C 0.6470(5) -0.0754(3) -0.1120(3) 0.0350(14) Uani 1 1 d . . . C12 C 0.6981(7) -0.1210(3) -0.1275(3) 0.050(2) Uani 1 1 d . . . C13 C 0.7248(8) -0.1300(4) -0.1776(3) 0.056(2) Uani 1 1 d . . . H13 H 0.7100 -0.1039 -0.2017 0.067 Uiso 1 1 calc R . . C14 C 0.7710(12) -0.1749(4) -0.1920(4) 0.083(4) Uani 1 1 d . . . H14 H 0.7877 -0.1801 -0.2258 0.100 Uiso 1 1 calc R . . C15 C 0.7945(13) -0.2145(5) -0.1558(4) 0.094(5) Uani 1 1 d . . . H15 H 0.8276 -0.2458 -0.1655 0.113 Uiso 1 1 calc R . . C16 C 0.7691(9) -0.2070(4) -0.1073(4) 0.068(3) Uani 1 1 d . . . H16 H 0.7836 -0.2339 -0.0839 0.082 Uiso 1 1 calc R . . C17 C 0.7217(8) -0.1605(4) -0.0909(3) 0.057(2) Uani 1 1 d . . . C18 C 0.6939(7) -0.1530(3) -0.0419(3) 0.049(2) Uani 1 1 d . . . H18 H 0.7106 -0.1791 -0.0182 0.059 Uiso 1 1 calc R . . C19 C 0.6198(7) -0.0331(3) -0.1473(3) 0.0455(19) Uani 1 1 d . . . C20 C 0.6871(9) 0.0021(4) -0.1645(3) 0.064(3) Uani 1 1 d . . . H20 H 0.7542 -0.0012 -0.1560 0.077 Uiso 1 1 calc R . . C21 C 0.6541(12) 0.0440(5) -0.1957(4) 0.086(4) Uani 1 1 d . . . H21 H 0.6991 0.0698 -0.2071 0.103 Uiso 1 1 calc R . . C22 C 0.5584(9) 0.0469(4) -0.2090(4) 0.064(3) Uani 1 1 d . . . H22 H 0.5379 0.0746 -0.2303 0.076 Uiso 1 1 calc R . . C23 C 0.4918(8) 0.0117(5) -0.1929(3) 0.063(3) Uani 1 1 d . . . H23 H 0.4253 0.0143 -0.2030 0.075 Uiso 1 1 calc R . . C24 C 0.5218(7) -0.0288(3) -0.1613(3) 0.0477(19) Uani 1 1 d . . . H24 H 0.4753 -0.0535 -0.1492 0.057 Uiso 1 1 calc R . . C25 C 0.8008(5) 0.0114(3) 0.0307(2) 0.0353(15) Uani 1 1 d . . . H25 H 0.7847 0.0322 0.0611 0.042 Uiso 1 1 calc R . . C26 C 0.9089(5) 0.0154(4) 0.0227(3) 0.0471(19) Uani 1 1 d . . . C27 C 0.9668(7) 0.0410(4) 0.0578(5) 0.064(3) Uani 1 1 d . . . H27 H 0.9380 0.0555 0.0868 0.077 Uiso 1 1 calc R . . C28 C 1.0667(7) 0.0451(5) 0.0499(6) 0.082(4) Uani 1 1 d . . . H28 H 1.1059 0.0611 0.0748 0.098 Uiso 1 1 calc R . . C29 C 1.1091(7) 0.0278(7) 0.0095(5) 0.098(5) Uani 1 1 d . . . H29 H 1.1773 0.0327 0.0046 0.118 Uiso 1 1 calc R . . C30 C 1.0532(8) 0.0023(10) -0.0257(4) 0.137(9) Uani 1 1 d . . . H30 H 1.0829 -0.0107 -0.0551 0.165 Uiso 1 1 calc R . . C31 C 0.9513(7) -0.0044(8) -0.0180(4) 0.098(5) Uani 1 1 d . . . H31 H 0.9130 -0.0230 -0.0416 0.118 Uiso 1 1 calc R . . C32 C 0.7573(6) 0.0899(3) -0.0195(3) 0.0431(18) Uani 1 1 d . . . H32A H 0.7412 0.1098 0.0109 0.052 Uiso 1 1 calc R . . H32B H 0.8277 0.0953 -0.0265 0.052 Uiso 1 1 calc R . . C33 C 0.6990(6) 0.1118(3) -0.0615(3) 0.0441(17) Uani 1 1 d . . . C34 C 0.5942(6) 0.1101(3) -0.0591(3) 0.0369(15) Uani 1 1 d . . . C35 C 0.5396(6) 0.1372(3) -0.0945(3) 0.0396(17) Uani 1 1 d . . . C36 C 0.5879(7) 0.1620(3) -0.1351(3) 0.0481(19) Uani 1 1 d . . . C37 C 0.5330(8) 0.1848(4) -0.1754(3) 0.061(2) Uani 1 1 d . . . H37 H 0.4635 0.1839 -0.1748 0.073 Uiso 1 1 calc R . . C38 C 0.5814(9) 0.2081(4) -0.2150(4) 0.068(3) Uani 1 1 d . . . H38 H 0.5452 0.2241 -0.2410 0.082 Uiso 1 1 calc R . . C39 C 0.6850(9) 0.2077(5) -0.2164(4) 0.078(4) Uani 1 1 d . . . H39 H 0.7175 0.2240 -0.2435 0.094 Uiso 1 1 calc R . . C40 C 0.7396(9) 0.1846(4) -0.1802(4) 0.068(3) Uani 1 1 d . . . H40 H 0.8089 0.1839 -0.1825 0.081 Uiso 1 1 calc R . . C41 C 0.6903(7) 0.1610(4) -0.1382(3) 0.052(2) Uani 1 1 d . . . C42 C 0.7450(6) 0.1366(4) -0.0998(3) 0.0483(19) Uani 1 1 d . . . H42 H 0.8144 0.1376 -0.1008 0.058 Uiso 1 1 calc R . . C43 C 0.4322(6) 0.1387(3) -0.0891(3) 0.0390(16) Uani 1 1 d . . . C44 C 0.3724(7) 0.0946(4) -0.1002(3) 0.056(2) Uani 1 1 d . . . H44 H 0.4008 0.0624 -0.1112 0.067 Uiso 1 1 calc R . . C45 C 0.2718(7) 0.0990(5) -0.0946(4) 0.064(3) Uani 1 1 d . . . H45 H 0.2323 0.0696 -0.1032 0.076 Uiso 1 1 calc R . . C46 C 0.2272(6) 0.1430(4) -0.0776(3) 0.053(2) Uani 1 1 d . . . H46 H 0.1583 0.1442 -0.0732 0.064 Uiso 1 1 calc R . . C47 C 0.2855(7) 0.1866(4) -0.0670(3) 0.051(2) Uani 1 1 d . . . H47 H 0.2562 0.2180 -0.0547 0.061 Uiso 1 1 calc R . . C48 C 0.3851(7) 0.1847(3) -0.0740(3) 0.050(2) Uani 1 1 d . . . H48 H 0.4228 0.2156 -0.0684 0.060 Uiso 1 1 calc R . . C49 C 0.4688(5) 0.1677(2) 0.0999(2) 0.0301(13) Uani 1 1 d . . . H49 H 0.4115 0.1791 0.1203 0.036 Uiso 1 1 calc R . . C50 C 0.4966(4) 0.2130(2) 0.0658(2) 0.0272(12) Uani 1 1 d . . . C51 C 0.4425(6) 0.2594(3) 0.0663(3) 0.0435(17) Uani 1 1 d . . . H51 H 0.3905 0.2635 0.0892 0.052 Uiso 1 1 calc R . . C52 C 0.4640(7) 0.3003(3) 0.0333(3) 0.051(2) Uani 1 1 d . . . H52 H 0.4274 0.3321 0.0344 0.061 Uiso 1 1 calc R . . C53 C 0.5390(6) 0.2944(3) -0.0013(3) 0.0462(18) Uani 1 1 d . . . H53 H 0.5539 0.3220 -0.0238 0.055 Uiso 1 1 calc R . . C54 C 0.5917(6) 0.2474(3) -0.0023(3) 0.0426(17) Uani 1 1 d . . . H54 H 0.6425 0.2427 -0.0259 0.051 Uiso 1 1 calc R . . C55 C 0.5698(5) 0.2070(3) 0.0315(2) 0.0323(14) Uani 1 1 d . . . H55 H 0.6062 0.1751 0.0307 0.039 Uiso 1 1 calc R . . C56 C 0.3333(5) 0.1208(3) 0.0587(3) 0.0343(15) Uani 1 1 d . . . H56A H 0.3184 0.1549 0.0426 0.041 Uiso 1 1 calc R . . H56B H 0.3195 0.0925 0.0345 0.041 Uiso 1 1 calc R . . C57 C 0.2672(5) 0.1141(3) 0.1022(3) 0.0387(15) Uani 1 1 d . . . C58 C 0.2757(5) 0.0698(3) 0.1348(3) 0.0363(15) Uani 1 1 d . . . C59 C 0.2011(5) 0.0581(3) 0.1676(3) 0.0432(18) Uani 1 1 d . . . C60 C 0.1182(6) 0.0917(4) 0.1716(3) 0.050(2) Uani 1 1 d . . . C61 C 0.0367(8) 0.0788(5) 0.2024(5) 0.077(4) Uani 1 1 d . . . H61 H 0.0359 0.0466 0.2203 0.093 Uiso 1 1 calc R . . C62 C -0.0403(8) 0.1131(5) 0.2060(5) 0.078(4) Uani 1 1 d . . . H62 H -0.0935 0.1046 0.2272 0.094 Uiso 1 1 calc R . . C63 C -0.0422(8) 0.1607(5) 0.1790(5) 0.080(4) Uani 1 1 d . . . H63 H -0.0962 0.1841 0.1820 0.096 Uiso 1 1 calc R . . C64 C 0.0331(8) 0.1727(4) 0.1490(4) 0.067(3) Uani 1 1 d . . . H64 H 0.0310 0.2049 0.1311 0.081 Uiso 1 1 calc R . . C65 C 0.1145(6) 0.1396(3) 0.1431(3) 0.0474(19) Uani 1 1 d . . . C66 C 0.1895(6) 0.1490(3) 0.1093(3) 0.0457(18) Uani 1 1 d . . . H66 H 0.1877 0.1805 0.0903 0.055 Uiso 1 1 calc R . . C67 C 0.2101(5) 0.0087(4) 0.1984(3) 0.049(2) Uani 1 1 d . . . C68 C 0.2766(6) 0.0061(4) 0.2393(4) 0.058(2) Uani 1 1 d . . . H68 H 0.3168 0.0354 0.2472 0.069 Uiso 1 1 calc R . . C69 C 0.2814(8) -0.0398(5) 0.2671(4) 0.071(3) Uani 1 1 d . . . H69 H 0.3269 -0.0417 0.2936 0.085 Uiso 1 1 calc R . . C70 C 0.2243(9) -0.0815(4) 0.2580(5) 0.076(4) Uani 1 1 d . . . H70 H 0.2271 -0.1117 0.2787 0.091 Uiso 1 1 calc R . . C71 C 0.1586(9) -0.0799(4) 0.2165(4) 0.070(3) Uani 1 1 d . . . H71 H 0.1186 -0.1094 0.2089 0.084 Uiso 1 1 calc R . . C72 C 0.1546(7) -0.0352(4) 0.1882(4) 0.053(2) Uani 1 1 d . . . H72 H 0.1119 -0.0345 0.1604 0.064 Uiso 1 1 calc R . . C73 C 0.5541(5) 0.1536(3) 0.1354(2) 0.0291(13) Uani 1 1 d . . . H73 H 0.6119 0.1438 0.1147 0.035 Uiso 1 1 calc R . . C74 C 0.5840(5) 0.1990(3) 0.1682(2) 0.0325(14) Uani 1 1 d . . . C75 C 0.6746(5) 0.2238(3) 0.1613(3) 0.0375(15) Uani 1 1 d . . . H75 H 0.7171 0.2120 0.1359 0.045 Uiso 1 1 calc R . . C76 C 0.7030(6) 0.2659(3) 0.1916(3) 0.0458(18) Uani 1 1 d . . . H76 H 0.7636 0.2833 0.1860 0.055 Uiso 1 1 calc R . . C77 C 0.6416(6) 0.2823(3) 0.2300(3) 0.0411(17) Uani 1 1 d . . . H77 H 0.6611 0.3107 0.2508 0.049 Uiso 1 1 calc R . . C78 C 0.5541(7) 0.2579(3) 0.2380(3) 0.0449(18) Uani 1 1 d . . . H78 H 0.5142 0.2683 0.2651 0.054 Uiso 1 1 calc R . . C79 C 0.5226(7) 0.2168(3) 0.2057(3) 0.0417(16) Uani 1 1 d . . . H79 H 0.4596 0.2016 0.2098 0.050 Uiso 1 1 calc R . . C80 C 0.5972(6) 0.0856(3) 0.1980(3) 0.0375(16) Uani 1 1 d . . . H80A H 0.6089 0.1128 0.2236 0.045 Uiso 1 1 calc R . . H80B H 0.6593 0.0802 0.1798 0.045 Uiso 1 1 calc R . . C81 C 0.5690(5) 0.0348(3) 0.2230(3) 0.0345(15) Uani 1 1 d . . . C82 C 0.5546(5) -0.0108(3) 0.1934(2) 0.0310(13) Uani 1 1 d . . . C83 C 0.5392(5) -0.0588(3) 0.2159(3) 0.0342(14) Uani 1 1 d . . . C84 C 0.5346(5) -0.0638(3) 0.2679(3) 0.0364(15) Uani 1 1 d . . . C85 C 0.5148(6) -0.1120(3) 0.2917(3) 0.0439(17) Uani 1 1 d . . . H85 H 0.5095 -0.1433 0.2727 0.053 Uiso 1 1 calc R . . C86 C 0.5029(6) -0.1142(3) 0.3424(3) 0.050(2) Uani 1 1 d . . . H86 H 0.4885 -0.1470 0.3578 0.060 Uiso 1 1 calc R . . C87 C 0.5120(7) -0.0688(4) 0.3711(3) 0.052(2) Uani 1 1 d . . . H87 H 0.5051 -0.0710 0.4061 0.062 Uiso 1 1 calc R . . C88 C 0.5309(7) -0.0208(3) 0.3491(3) 0.0461(18) Uani 1 1 d . . . H88 H 0.5363 0.0099 0.3690 0.055 Uiso 1 1 calc R . . C89 C 0.5422(6) -0.0169(3) 0.2976(3) 0.0380(15) Uani 1 1 d . . . C90 C 0.5627(6) 0.0316(3) 0.2737(3) 0.0371(16) Uani 1 1 d . . . H90 H 0.5723 0.0625 0.2930 0.045 Uiso 1 1 calc R . . C91 C 0.5310(6) -0.1074(3) 0.1837(3) 0.0385(15) Uani 1 1 d . . . C92 C 0.4403(8) -0.1199(3) 0.1622(3) 0.054(2) Uani 1 1 d . . . H92 H 0.3851 -0.0983 0.1687 0.064 Uiso 1 1 calc R . . C93 C 0.4307(10) -0.1638(4) 0.1315(4) 0.072(3) Uani 1 1 d . . . H93 H 0.3697 -0.1722 0.1166 0.086 Uiso 1 1 calc R . . C94 C 0.5137(11) -0.1952(4) 0.1231(4) 0.070(3) Uani 1 1 d . . . H94 H 0.5083 -0.2257 0.1028 0.084 Uiso 1 1 calc R . . C95 C 0.6016(9) -0.1827(4) 0.1435(4) 0.070(3) Uani 1 1 d . . . H95 H 0.6573 -0.2038 0.1366 0.083 Uiso 1 1 calc R . . C96 C 0.6104(7) -0.1387(4) 0.1749(4) 0.056(2) Uani 1 1 d . . . H96 H 0.6715 -0.1308 0.1899 0.068 Uiso 1 1 calc R . . C1X C 0.3821(6) -0.0245(3) 0.0261(3) 0.0409(16) Uani 1 1 d . A . C2X C 0.3268(7) -0.0538(4) 0.0608(4) 0.057(2) Uani 1 1 d . . . H2X H 0.3419 -0.0512 0.0950 0.069 Uiso 1 1 calc R A . C8X C 0.1058(19) -0.1032(10) -0.0733(9) 0.132(11) Uani 0.709(4) 1 d P A 1 C9X C 0.1638(13) -0.0785(8) -0.1054(7) 0.084(5) Uani 0.709(4) 1 d P A 1 H9X H 0.1473 -0.0788 -0.1396 0.100 Uiso 0.709(4) 1 calc PR A 1 C10X C 0.2460(10) -0.0528(6) -0.0905(5) 0.059(3) Uani 0.709(4) 1 d P A 1 H10X H 0.2815 -0.0320 -0.1136 0.071 Uiso 0.709(4) 1 calc PR A 1 C5X C 0.2808(9) -0.0567(5) -0.0384(4) 0.074(3) Uani 1 1 d . A . C6X C 0.3615(7) -0.0265(4) -0.0239(3) 0.054(2) Uani 1 1 d . . . H6X H 0.4005 -0.0082 -0.0474 0.064 Uiso 1 1 calc R A . C5Z C -0.1957(10) -0.3387(5) 0.2186(5) 0.031(3) Uiso 0.50 1 d P . . C6Z C -0.2948(10) -0.3401(5) 0.2308(5) 0.030(3) Uiso 0.50 1 d P A . C7Z C -0.3650(14) -0.3285(7) 0.1968(7) 0.052(4) Uiso 0.50 1 d P . . C8Z C -0.3415(15) -0.3125(7) 0.1512(7) 0.055(4) Uiso 0.50 1 d P A . C7X C 0.1302(16) -0.1064(9) -0.0237(8) 0.105(8) Uani 0.709(4) 1 d P A 1 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 C4X 0.109(11) 0.153(14) 0.078(9) -0.031(9) 0.021(8) -0.078(11) C3X 0.074(7) 0.108(10) 0.075(8) 0.021(7) -0.012(6) -0.052(7) Fe1 0.0249(4) 0.0378(5) 0.0258(4) -0.0017(4) -0.0015(3) -0.0010(4) Fe2 0.0225(4) 0.0304(4) 0.0280(4) 0.0003(4) 0.0004(3) -0.0021(3) N1 0.025(3) 0.041(3) 0.027(3) -0.004(2) 0.000(2) -0.003(2) N2 0.031(3) 0.042(3) 0.032(3) 0.006(2) -0.003(2) -0.005(2) N3 0.025(3) 0.038(3) 0.028(3) 0.000(2) -0.005(2) -0.002(2) N4 0.034(3) 0.029(3) 0.029(3) 0.004(2) 0.001(2) 0.001(2) O1 0.034(2) 0.046(3) 0.024(2) -0.0034(19) -0.0050(18) 0.005(2) O2 0.027(2) 0.047(3) 0.033(2) 0.005(2) -0.0029(19) 0.001(2) O3 0.017(2) 0.041(3) 0.045(3) 0.006(2) 0.0048(18) 0.0025(18) O4 0.034(2) 0.027(2) 0.030(2) 0.0019(17) -0.0022(18) 0.0028(18) O5 0.023(2) 0.042(3) 0.032(2) -0.0038(19) -0.0037(17) -0.0070(19) O6 0.025(2) 0.035(2) 0.033(2) -0.0034(18) 0.0000(18) -0.0036(18) Br1X 0.149(2) 0.226(4) 0.182(3) 0.087(3) -0.117(2) -0.138(3) C1 0.028(3) 0.045(4) 0.028(3) -0.001(3) 0.002(2) 0.005(3) C2 0.029(4) 0.076(6) 0.054(5) 0.028(4) -0.015(3) -0.011(4) C3 0.100(10) 0.070(7) 0.125(12) 0.010(7) -0.069(9) 0.016(7) C4 0.21(2) 0.083(11) 0.25(3) 0.012(15) -0.14(2) 0.041(13) C5 0.158(16) 0.142(15) 0.130(14) 0.096(13) -0.105(13) -0.074(13) C6 0.071(7) 0.169(15) 0.059(7) 0.063(8) -0.017(6) -0.013(9) C7 0.057(6) 0.138(11) 0.033(4) 0.021(6) -0.009(4) 0.009(6) C8 0.039(4) 0.039(4) 0.031(3) 0.000(3) -0.008(3) 0.000(3) C9 0.038(4) 0.050(4) 0.029(3) -0.010(3) -0.007(3) 0.011(3) C10 0.036(3) 0.047(4) 0.026(3) -0.006(3) -0.009(3) 0.008(3) C11 0.039(4) 0.036(3) 0.030(3) -0.005(3) -0.006(3) 0.000(3) C12 0.068(6) 0.047(4) 0.036(4) -0.003(3) -0.006(4) 0.018(4) C13 0.086(7) 0.049(5) 0.034(4) -0.002(3) 0.002(4) 0.018(5) C14 0.151(12) 0.062(6) 0.037(5) -0.005(4) -0.001(6) 0.040(7) C15 0.162(14) 0.060(6) 0.060(6) -0.007(5) 0.011(8) 0.058(8) C16 0.104(8) 0.049(5) 0.051(5) -0.001(4) -0.004(6) 0.036(5) C17 0.077(6) 0.044(4) 0.051(5) -0.008(4) -0.007(5) 0.018(4) C18 0.072(6) 0.036(4) 0.041(4) -0.005(3) -0.013(4) -0.001(4) C19 0.064(5) 0.046(4) 0.026(3) -0.008(3) -0.007(3) 0.003(4) C20 0.075(6) 0.075(6) 0.042(5) 0.004(4) -0.013(5) -0.011(5) C21 0.123(11) 0.071(7) 0.064(7) 0.017(6) -0.014(7) -0.033(8) C22 0.089(8) 0.055(5) 0.047(5) -0.003(4) -0.009(5) 0.025(6) C23 0.067(6) 0.091(7) 0.031(4) -0.005(4) -0.001(4) 0.044(6) C24 0.049(4) 0.056(5) 0.037(4) -0.006(3) 0.003(3) 0.024(4) C25 0.033(3) 0.050(4) 0.023(3) 0.002(3) 0.003(3) -0.007(3) C26 0.026(3) 0.076(6) 0.039(4) 0.021(4) -0.004(3) 0.001(4) C27 0.040(5) 0.060(5) 0.093(7) -0.008(5) -0.025(5) -0.002(4) C28 0.035(5) 0.070(7) 0.141(12) 0.004(7) -0.023(6) -0.016(5) C29 0.026(4) 0.186(15) 0.083(8) 0.056(9) -0.014(5) -0.021(6) C30 0.038(5) 0.33(3) 0.041(5) 0.009(10) 0.009(4) 0.003(10) C31 0.032(4) 0.224(17) 0.038(5) 0.004(7) 0.003(4) -0.010(7) C32 0.031(4) 0.054(5) 0.044(4) 0.013(3) -0.002(3) -0.002(3) C33 0.044(4) 0.048(4) 0.040(4) 0.005(3) 0.002(3) -0.004(3) C34 0.043(4) 0.037(3) 0.030(3) 0.006(3) -0.003(3) -0.003(3) C35 0.050(4) 0.044(4) 0.026(3) -0.005(3) -0.004(3) 0.017(3) C36 0.061(5) 0.048(4) 0.035(4) 0.011(3) 0.002(4) 0.011(4) C37 0.055(5) 0.085(7) 0.042(4) 0.011(4) 0.002(4) 0.018(5) C38 0.082(7) 0.080(7) 0.042(5) 0.018(5) 0.009(5) 0.019(6) C39 0.082(7) 0.106(9) 0.045(5) 0.036(6) 0.025(5) 0.039(7) C40 0.070(6) 0.073(6) 0.059(6) 0.031(5) 0.023(5) 0.011(5) C41 0.052(5) 0.058(5) 0.045(4) 0.018(4) 0.005(4) 0.014(4) C42 0.039(4) 0.058(5) 0.048(5) 0.015(4) 0.005(3) -0.003(4) C43 0.045(4) 0.045(4) 0.027(3) 0.001(3) -0.005(3) 0.012(3) C44 0.056(5) 0.056(5) 0.055(5) -0.024(4) 0.013(4) 0.004(4) C45 0.045(5) 0.098(8) 0.049(5) -0.013(5) -0.003(4) -0.008(5) C46 0.039(4) 0.082(6) 0.039(4) -0.004(4) -0.010(3) 0.012(4) C47 0.056(5) 0.052(5) 0.044(4) -0.003(4) -0.008(4) 0.021(4) C48 0.048(5) 0.046(4) 0.056(5) -0.004(4) -0.012(4) 0.016(4) C49 0.030(3) 0.026(3) 0.034(3) 0.006(2) 0.003(3) -0.003(2) C50 0.024(3) 0.031(3) 0.026(3) 0.005(2) -0.004(2) 0.000(2) C51 0.051(4) 0.041(4) 0.038(4) 0.007(3) 0.004(3) 0.006(3) C52 0.055(5) 0.041(4) 0.057(5) 0.017(4) -0.006(4) 0.014(4) C53 0.060(5) 0.040(4) 0.039(4) 0.012(3) -0.002(4) -0.005(3) C54 0.044(4) 0.047(4) 0.036(4) 0.013(3) 0.004(3) -0.012(3) C55 0.029(3) 0.038(3) 0.030(3) 0.009(3) -0.002(3) 0.002(3) C56 0.022(3) 0.039(4) 0.042(4) 0.009(3) -0.005(3) -0.002(3) C57 0.033(3) 0.046(4) 0.038(4) -0.003(3) -0.004(3) -0.001(3) C58 0.027(3) 0.049(4) 0.032(3) -0.002(3) -0.001(3) -0.001(3) C59 0.024(3) 0.046(4) 0.059(5) 0.012(4) 0.007(3) 0.007(3) C60 0.032(4) 0.068(5) 0.052(5) 0.012(4) 0.012(3) 0.006(4) C61 0.059(6) 0.083(7) 0.090(8) 0.043(6) 0.037(6) 0.029(5) C62 0.044(5) 0.096(8) 0.095(8) 0.036(7) 0.024(5) 0.022(5) C63 0.056(6) 0.096(8) 0.089(8) 0.020(6) 0.019(5) 0.047(6) C64 0.061(6) 0.062(6) 0.079(7) 0.022(5) 0.011(5) 0.020(5) C65 0.032(4) 0.053(5) 0.057(5) 0.002(4) 0.005(3) 0.019(3) C66 0.036(4) 0.048(4) 0.053(5) 0.006(4) -0.010(4) 0.001(3) C67 0.027(3) 0.065(5) 0.054(5) 0.017(4) 0.016(3) 0.010(3) C68 0.030(4) 0.079(6) 0.063(5) 0.032(5) 0.013(4) 0.010(4) C69 0.047(5) 0.088(8) 0.078(7) 0.039(6) 0.014(5) 0.022(5) C70 0.070(7) 0.059(6) 0.098(8) 0.038(6) 0.048(6) 0.031(5) C71 0.079(7) 0.056(5) 0.075(7) 0.025(5) 0.037(6) 0.020(5) C72 0.050(5) 0.055(5) 0.055(5) 0.005(4) 0.012(4) 0.004(4) C73 0.035(3) 0.028(3) 0.024(3) 0.001(2) 0.000(2) 0.001(3) C74 0.035(3) 0.031(3) 0.032(3) 0.008(3) -0.010(3) -0.005(3) C75 0.037(4) 0.034(3) 0.042(4) 0.001(3) 0.005(3) -0.004(3) C76 0.043(4) 0.052(5) 0.042(4) 0.007(3) -0.012(3) -0.003(4) C77 0.056(5) 0.027(3) 0.040(4) -0.003(3) -0.013(3) -0.005(3) C78 0.055(5) 0.033(4) 0.046(4) -0.001(3) 0.005(4) 0.007(3) C79 0.052(4) 0.030(3) 0.044(4) 0.000(3) 0.005(4) -0.004(3) C80 0.047(4) 0.032(3) 0.034(3) 0.004(3) -0.011(3) -0.006(3) C81 0.037(4) 0.029(3) 0.038(3) 0.007(3) -0.005(3) 0.001(3) C82 0.029(3) 0.031(3) 0.033(3) 0.001(3) -0.001(2) -0.003(3) C83 0.030(3) 0.035(3) 0.037(4) 0.007(3) -0.002(3) 0.000(3) C84 0.027(3) 0.031(3) 0.051(4) 0.009(3) -0.006(3) -0.003(3) C85 0.040(4) 0.038(4) 0.054(4) 0.015(3) -0.012(3) -0.007(3) C86 0.050(5) 0.044(4) 0.057(5) 0.025(4) -0.010(4) -0.005(4) C87 0.060(5) 0.057(5) 0.039(4) 0.020(4) -0.016(4) -0.018(4) C88 0.059(5) 0.042(4) 0.036(4) 0.013(3) -0.015(4) -0.001(4) C89 0.043(4) 0.038(4) 0.033(3) 0.008(3) -0.008(3) 0.001(3) C90 0.043(4) 0.035(4) 0.034(3) 0.008(3) -0.009(3) 0.000(3) C91 0.039(4) 0.031(3) 0.045(4) 0.008(3) 0.004(3) -0.006(3) C92 0.080(6) 0.037(4) 0.045(4) 0.010(3) -0.017(4) -0.012(4) C93 0.110(9) 0.060(6) 0.045(5) 0.016(4) -0.023(6) -0.026(6) C94 0.130(11) 0.033(4) 0.048(5) 0.004(4) 0.002(6) -0.009(6) C95 0.078(7) 0.053(5) 0.078(7) -0.008(5) 0.032(6) 0.001(5) C96 0.058(5) 0.045(4) 0.067(6) 0.002(4) 0.007(4) 0.001(4) C1X 0.038(4) 0.038(4) 0.047(4) -0.004(3) -0.004(3) -0.011(3) C2X 0.059(5) 0.063(6) 0.049(5) 0.010(4) -0.009(4) -0.026(5) C8X 0.133(19) 0.145(19) 0.119(17) 0.057(15) -0.081(15) -0.099(17) C9X 0.068(10) 0.103(13) 0.080(11) 0.002(10) -0.030(9) -0.027(9) C10X 0.046(7) 0.067(8) 0.063(8) -0.010(6) -0.015(6) 0.012(6) C5X 0.077(7) 0.091(8) 0.054(6) -0.004(5) -0.021(5) -0.036(6) C6X 0.049(5) 0.075(6) 0.037(4) -0.015(4) 0.001(3) -0.022(4) C7X 0.095(13) 0.095(13) 0.125(17) 0.041(12) -0.071(13) -0.056(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C4X C7Y 1.3900 . ? C4X C3X 1.3900 . ? C4X C7X 1.455(17) . ? C4X C5X 1.487(13) . ? C7Y C8Y 1.3900 . ? C8Y C9Y 1.3900 . ? C8Y Br1Y 1.853(8) . ? C9Y C10Y 1.3900 . ? C10Y C3X 1.3900 . ? C3X C2X 1.356(11) . ? C9Z C10Z 1.3900 . ? C9Z C4Z 1.3900 . ? C9Z C8Z 1.56(2) . ? C4Z C3Z 1.3900 . ? C4Z C5Z 1.475(16) . ? C3Z C2Z 1.3900 . ? C2Z C1Z 1.3900 . ? C1Z C10Z 1.3900 . ? C1Z Br1Z 1.923(10) . ? Br1Y Br1Z 1.813(7) . ? Fe1 O1 1.897(5) . ? Fe1 O2 1.934(5) . ? Fe1 O5 2.008(5) . ? Fe1 O6 2.058(5) . ? Fe1 N2 2.159(6) . ? Fe1 N1 2.221(6) . ? Fe2 O3 1.891(4) . ? Fe2 O4 1.929(4) . ? Fe2 O6 2.033(5) . ? Fe2 O5 2.042(5) . ? Fe2 N3 2.177(6) . ? Fe2 N4 2.216(6) . ? N1 C8 1.491(9) . ? N1 C1 1.506(8) . ? N2 C25 1.493(9) . ? N2 C32 1.494(10) . ? N3 C49 1.495(8) . ? N3 C56 1.501(8) . ? N4 C80 1.471(9) . ? N4 C73 1.500(8) . ? O1 C10 1.296(9) . ? O2 C34 1.323(8) . ? O3 C58 1.335(9) . ? O4 C82 1.347(8) . ? O5 C1X 1.385(8) . ? O1Z C6Z 1.384(18) . ? Br1X C8X 1.925(17) . ? C1 C2 1.486(10) . ? C1 C25 1.546(11) . ? C1 H1 1.0000 . ? C2 C3 1.370(17) . ? C2 C7 1.378(15) . ? C3 C4 1.44(2) . ? C3 H3 0.9500 . ? C4 C5 1.37(3) . ? C4 H4 0.9500 . ? C5 C6 1.38(3) . ? C5 H5 0.9500 . ? C6 C7 1.344(14) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.497(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C18 1.386(11) . ? C9 C10 1.433(11) . ? C10 C11 1.418(10) . ? C11 C12 1.413(11) . ? C11 C19 1.483(11) . ? C12 C13 1.420(12) . ? C12 C17 1.444(12) . ? C13 C14 1.359(13) . ? C13 H13 0.9500 . ? C14 C15 1.437(15) . ? C14 H14 0.9500 . ? C15 C16 1.369(15) . ? C15 H15 0.9500 . ? C16 C17 1.418(12) . ? C16 H16 0.9500 . ? C17 C18 1.389(13) . ? C18 H18 0.9500 . ? C19 C20 1.362(14) . ? C19 C24 1.397(13) . ? C20 C21 1.428(16) . ? C20 H20 0.9500 . ? C21 C22 1.359(18) . ? C21 H21 0.9500 . ? C22 C23 1.348(16) . ? C22 H22 0.9500 . ? C23 C24 1.397(12) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.498(10) . ? C25 H25 1.0000 . ? C26 C31 1.340(15) . ? C26 C27 1.394(13) . ? C27 C28 1.386(14) . ? C27 H27 0.9500 . ? C28 C29 1.31(2) . ? C28 H28 0.9500 . ? C29 C30 1.38(2) . ? C29 H29 0.9500 . ? C30 C31 1.419(15) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.493(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C42 1.363(11) . ? C33 C34 1.435(11) . ? C34 C35 1.395(10) . ? C35 C36 1.425(11) . ? C35 C43 1.475(11) . ? C36 C41 1.402(13) . ? C36 C37 1.444(12) . ? C37 C38 1.391(13) . ? C37 H37 0.9500 . ? C38 C39 1.417(17) . ? C38 H38 0.9500 . ? C39 C40 1.363(14) . ? C39 H39 0.9500 . ? C40 C41 1.449(12) . ? C40 H40 0.9500 . ? C41 C42 1.420(12) . ? C42 H42 0.9500 . ? C43 C48 1.395(11) . ? C43 C44 1.416(12) . ? C44 C45 1.388(14) . ? C44 H44 0.9500 . ? C45 C46 1.352(15) . ? C45 H45 0.9500 . ? C46 C47 1.393(14) . ? C46 H46 0.9500 . ? C47 C48 1.374(13) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.520(8) . ? C49 C73 1.553(9) . ? C49 H49 1.0000 . ? C50 C55 1.370(9) . ? C50 C51 1.391(10) . ? C51 C52 1.397(11) . ? C51 H51 0.9500 . ? C52 C53 1.395(12) . ? C52 H52 0.9500 . ? C53 C54 1.391(12) . ? C53 H53 0.9500 . ? C54 C55 1.405(9) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.491(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C66 1.396(11) . ? C57 C58 1.432(11) . ? C58 C59 1.383(10) . ? C59 C60 1.422(11) . ? C59 C67 1.509(11) . ? C60 C61 1.429(12) . ? C60 C65 1.439(12) . ? C61 C62 1.367(14) . ? C61 H61 0.9500 . ? C62 C63 1.411(16) . ? C62 H62 0.9500 . ? C63 C64 1.344(15) . ? C63 H63 0.9500 . ? C64 C65 1.403(12) . ? C64 H64 0.9500 . ? C65 C66 1.394(12) . ? C66 H66 0.9500 . ? C67 C72 1.376(13) . ? C67 C68 1.430(13) . ? C68 C69 1.387(13) . ? C68 H68 0.9500 . ? C69 C70 1.335(18) . ? C69 H69 0.9500 . ? C70 C71 1.437(19) . ? C70 H70 0.9500 . ? C71 C72 1.367(13) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.511(9) . ? C73 H73 1.0000 . ? C74 C79 1.391(11) . ? C74 C75 1.401(10) . ? C75 C76 1.399(11) . ? C75 H75 0.9500 . ? C76 C77 1.398(12) . ? C76 H76 0.9500 . ? C77 C78 1.364(12) . ? C77 H77 0.9500 . ? C78 C79 1.425(11) . ? C78 H78 0.9500 . ? C79 H79 0.9500 . ? C80 C81 1.506(9) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 C90 1.375(10) . ? C81 C82 1.417(10) . ? C82 C83 1.377(9) . ? C83 C84 1.415(10) . ? C83 C91 1.511(10) . ? C84 C85 1.406(10) . ? C84 C89 1.438(11) . ? C85 C86 1.379(12) . ? C85 H85 0.9500 . ? C86 C87 1.394(13) . ? C86 H86 0.9500 . ? C87 C88 1.379(11) . ? C87 H87 0.9500 . ? C88 C89 1.405(10) . ? C88 H88 0.9500 . ? C89 C90 1.416(10) . ? C90 H90 0.9500 . ? C91 C96 1.365(12) . ? C91 C92 1.406(12) . ? C92 C93 1.394(14) . ? C92 H92 0.9500 . ? C93 C94 1.405(18) . ? C93 H93 0.9500 . ? C94 C95 1.360(18) . ? C94 H94 0.9500 . ? C95 C96 1.405(14) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C1X C6X 1.380(12) . ? C1X C2X 1.415(12) . ? C2X H2X 0.9500 . ? C8X C9X 1.33(3) . ? C8X C7X 1.38(3) . ? C9X C10X 1.36(2) . ? C9X H9X 0.9500 . ? C10X C5X 1.489(17) . ? C10X H10X 0.9500 . ? C5X C6X 1.399(13) . ? C6X H6X 0.9500 . ? C5Z C6Z 1.395(19) . ? C6Z C7Z 1.36(2) . ? C7Z C8Z 1.34(3) . ? 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 C7Y C4X C3X 120.0 . . ? C7Y C4X C7X 29.8(11) . . ? C3X C4X C7X 129.4(11) . . ? C7Y C4X C5X 124.1(6) . . ? C3X C4X C5X 114.7(5) . . ? C7X C4X C5X 112.5(11) . . ? C4X C7Y C8Y 120.0 . . ? C7Y C8Y C9Y 120.0 . . ? C7Y C8Y Br1Y 121.7(3) . . ? C9Y C8Y Br1Y 118.2(3) . . ? C10Y C9Y C8Y 120.0 . . ? C3X C10Y C9Y 120.0 . . ? C2X C3X C10Y 116.2(6) . . ? C2X C3X C4X 122.8(6) . . ? C10Y C3X C4X 120.0 . . ? C10Z C9Z C4Z 120.0 . . ? C10Z C9Z C8Z 123.7(9) . . ? C4Z C9Z C8Z 116.0(9) . . ? C3Z C4Z C9Z 120.0 . . ? C3Z C4Z C5Z 121.1(8) . . ? C9Z C4Z C5Z 118.6(8) . . ? C4Z C3Z C2Z 120.0 . . ? C3Z C2Z C1Z 120.0 . . ? C10Z C1Z C2Z 120.0 . . ? C10Z C1Z Br1Z 120.5(6) . . ? C2Z C1Z Br1Z 117.9(5) . . ? C1Z C10Z C9Z 120.0 . . ? Br1Z Br1Y C8Y 155.2(4) . . ? O1 Fe1 O2 101.3(2) . . ? O1 Fe1 O5 100.4(2) . . ? O2 Fe1 O5 96.8(2) . . ? O1 Fe1 O6 172.0(2) . . ? O2 Fe1 O6 86.6(2) . . ? O5 Fe1 O6 79.37(18) . . ? O1 Fe1 N2 91.2(2) . . ? O2 Fe1 N2 91.4(2) . . ? O5 Fe1 N2 164.1(2) . . ? O6 Fe1 N2 87.6(2) . . ? O1 Fe1 N1 86.3(2) . . ? O2 Fe1 N1 167.6(2) . . ? O5 Fe1 N1 91.3(2) . . ? O6 Fe1 N1 85.74(19) . . ? N2 Fe1 N1 78.5(2) . . ? O3 Fe2 O4 103.7(2) . . ? O3 Fe2 O6 171.6(2) . . ? O4 Fe2 O6 84.4(2) . . ? O3 Fe2 O5 96.9(2) . . ? O4 Fe2 O5 100.2(2) . . ? O6 Fe2 O5 79.18(18) . . ? O3 Fe2 N3 90.0(2) . . ? O4 Fe2 N3 160.9(2) . . ? O6 Fe2 N3 82.7(2) . . ? O5 Fe2 N3 91.0(2) . . ? O3 Fe2 N4 93.5(2) . . ? O4 Fe2 N4 88.5(2) . . ? O6 Fe2 N4 88.9(2) . . ? O5 Fe2 N4 164.4(2) . . ? N3 Fe2 N4 77.4(2) . . ? C8 N1 C1 112.4(6) . . ? C8 N1 Fe1 111.1(4) . . ? C1 N1 Fe1 111.4(4) . . ? C25 N2 C32 112.4(6) . . ? C25 N2 Fe1 108.7(4) . . ? C32 N2 Fe1 110.2(4) . . ? C49 N3 C56 110.8(5) . . ? C49 N3 Fe2 114.3(4) . . ? C56 N3 Fe2 112.1(4) . . ? C80 N4 C73 113.5(5) . . ? C80 N4 Fe2 112.5(4) . . ? C73 N4 Fe2 106.6(4) . . ? C10 O1 Fe1 132.6(4) . . ? C34 O2 Fe1 126.2(5) . . ? C58 O3 Fe2 134.3(5) . . ? C82 O4 Fe2 124.6(4) . . ? C1X O5 Fe1 127.8(4) . . ? C1X O5 Fe2 130.7(4) . . ? Fe1 O5 Fe2 101.40(19) . . ? Fe2 O6 Fe1 100.05(19) . . ? Br1Y Br1Z C1Z 131.3(4) . . ? C2 C1 N1 111.7(6) . . ? C2 C1 C25 114.2(6) . . ? N1 C1 C25 109.9(6) . . ? C2 C1 H1 106.9 . . ? N1 C1 H1 106.9 . . ? C25 C1 H1 106.9 . . ? C3 C2 C7 118.7(10) . . ? C3 C2 C1 119.7(10) . . ? C7 C2 C1 121.6(9) . . ? C2 C3 C4 117.0(16) . . ? C2 C3 H3 121.5 . . ? C4 C3 H3 121.5 . . ? C5 C4 C3 121.3(18) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 120.0(12) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 117.3(16) . . ? C7 C6 H6 121.3 . . ? C5 C6 H6 121.3 . . ? C6 C7 C2 125.2(14) . . ? C6 C7 H7 117.4 . . ? C2 C7 H7 117.4 . . ? N1 C8 C9 110.9(6) . . ? N1 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? C18 C9 C10 118.9(7) . . ? C18 C9 C8 122.1(7) . . ? C10 C9 C8 118.9(6) . . ? O1 C10 C11 119.9(6) . . ? O1 C10 C9 120.4(6) . . ? C11 C10 C9 119.7(6) . . ? C12 C11 C10 120.9(7) . . ? C12 C11 C19 121.7(7) . . ? C10 C11 C19 117.4(6) . . ? C11 C12 C13 122.7(7) . . ? C11 C12 C17 118.3(7) . . ? C13 C12 C17 118.9(8) . . ? C14 C13 C12 121.9(8) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 119.6(9) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 119.8(9) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 122.1(9) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C18 C17 C16 122.5(9) . . ? C18 C17 C12 119.8(8) . . ? C16 C17 C12 117.7(8) . . ? C9 C18 C17 122.5(8) . . ? C9 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C20 C19 C24 120.3(8) . . ? C20 C19 C11 121.6(8) . . ? C24 C19 C11 118.0(8) . . ? C19 C20 C21 118.3(11) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C22 C21 C20 120.0(11) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 122.0(10) . . ? C23 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C22 C23 C24 119.1(9) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C19 C24 C23 120.2(10) . . ? C19 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? N2 C25 C26 114.9(6) . . ? N2 C25 C1 107.4(5) . . ? C26 C25 C1 111.8(7) . . ? N2 C25 H25 107.5 . . ? C26 C25 H25 107.5 . . ? C1 C25 H25 107.5 . . ? C31 C26 C27 119.1(9) . . ? C31 C26 C25 121.3(8) . . ? C27 C26 C25 119.5(8) . . ? C28 C27 C26 119.3(12) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 122.6(12) . . ? C29 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? C28 C29 C30 119.1(9) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C29 C30 C31 119.8(13) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C26 C31 C30 120.0(13) . . ? C26 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 N2 113.5(7) . . ? C33 C32 H32A 108.9 . . ? N2 C32 H32A 108.9 . . ? C33 C32 H32B 108.9 . . ? N2 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C42 C33 C34 120.6(7) . . ? C42 C33 C32 120.1(7) . . ? C34 C33 C32 119.1(7) . . ? O2 C34 C35 120.8(7) . . ? O2 C34 C33 119.8(6) . . ? C35 C34 C33 119.2(7) . . ? C34 C35 C36 119.7(7) . . ? C34 C35 C43 118.5(7) . . ? C36 C35 C43 121.8(7) . . ? C41 C36 C35 120.1(7) . . ? C41 C36 C37 118.7(8) . . ? C35 C36 C37 121.0(8) . . ? C38 C37 C36 120.3(9) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 119.5(9) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C40 C39 C38 122.1(9) . . ? C40 C39 H39 119.0 . . ? C38 C39 H39 119.0 . . ? C39 C40 C41 119.1(10) . . ? C39 C40 H40 120.5 . . ? C41 C40 H40 120.5 . . ? C36 C41 C42 119.3(8) . . ? C36 C41 C40 120.2(8) . . ? C42 C41 C40 120.5(8) . . ? C33 C42 C41 120.8(8) . . ? C33 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C48 C43 C44 117.1(8) . . ? C48 C43 C35 120.7(8) . . ? C44 C43 C35 122.2(7) . . ? C45 C44 C43 119.0(8) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C46 C45 C44 123.4(10) . . ? C46 C45 H45 118.3 . . ? C44 C45 H45 118.3 . . ? C45 C46 C47 117.8(8) . . ? C45 C46 H46 121.1 . . ? C47 C46 H46 121.1 . . ? C48 C47 C46 120.7(8) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C43 121.8(9) . . ? C47 C48 H48 119.1 . . ? C43 C48 H48 119.1 . . ? N3 C49 C50 112.0(5) . . ? N3 C49 C73 108.9(5) . . ? C50 C49 C73 111.2(5) . . ? N3 C49 H49 108.2 . . ? C50 C49 H49 108.2 . . ? C73 C49 H49 108.2 . . ? C55 C50 C51 119.2(6) . . ? C55 C50 C49 120.6(6) . . ? C51 C50 C49 120.0(6) . . ? C50 C51 C52 120.6(8) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C53 C52 C51 120.1(8) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C54 C53 C52 119.0(7) . . ? C54 C53 H53 120.5 . . ? C52 C53 H53 120.5 . . ? C53 C54 C55 120.0(7) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C50 C55 C54 121.0(7) . . ? C50 C55 H55 119.5 . . ? C54 C55 H55 119.5 . . ? C57 C56 N3 113.8(6) . . ? C57 C56 H56A 108.8 . . ? N3 C56 H56A 108.8 . . ? C57 C56 H56B 108.8 . . ? N3 C56 H56B 108.8 . . ? H56A C56 H56B 107.7 . . ? C66 C57 C58 118.3(7) . . ? C66 C57 C56 119.8(7) . . ? C58 C57 C56 121.7(6) . . ? O3 C58 C59 119.8(7) . . ? O3 C58 C57 119.9(6) . . ? C59 C58 C57 120.2(7) . . ? C58 C59 C60 120.5(7) . . ? C58 C59 C67 118.1(6) . . ? C60 C59 C67 121.5(7) . . ? C59 C60 C61 121.9(8) . . ? C59 C60 C65 119.6(7) . . ? C61 C60 C65 118.5(8) . . ? C62 C61 C60 119.8(9) . . ? C62 C61 H61 120.1 . . ? C60 C61 H61 120.1 . . ? C61 C62 C63 121.4(9) . . ? C61 C62 H62 119.3 . . ? C63 C62 H62 119.3 . . ? C64 C63 C62 119.4(9) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C63 C64 C65 122.7(9) . . ? C63 C64 H64 118.6 . . ? C65 C64 H64 118.6 . . ? C66 C65 C64 123.8(8) . . ? C66 C65 C60 117.9(7) . . ? C64 C65 C60 118.1(8) . . ? C65 C66 C57 122.8(8) . . ? C65 C66 H66 118.6 . . ? C57 C66 H66 118.6 . . ? C72 C67 C68 118.0(8) . . ? C72 C67 C59 121.0(8) . . ? C68 C67 C59 121.0(8) . . ? C69 C68 C67 119.1(10) . . ? C69 C68 H68 120.4 . . ? C67 C68 H68 120.4 . . ? C70 C69 C68 122.4(11) . . ? C70 C69 H69 118.8 . . ? C68 C69 H69 118.8 . . ? C69 C70 C71 119.1(9) . . ? C69 C70 H70 120.5 . . ? C71 C70 H70 120.5 . . ? C72 C71 C70 119.1(11) . . ? C72 C71 H71 120.5 . . ? C70 C71 H71 120.5 . . ? C71 C72 C67 122.3(10) . . ? C71 C72 H72 118.9 . . ? C67 C72 H72 118.9 . . ? N4 C73 C74 114.0(5) . . ? N4 C73 C49 106.5(5) . . ? C74 C73 C49 113.0(5) . . ? N4 C73 H73 107.7 . . ? C74 C73 H73 107.7 . . ? C49 C73 H73 107.7 . . ? C79 C74 C75 119.0(7) . . ? C79 C74 C73 120.7(6) . . ? C75 C74 C73 120.2(6) . . ? C76 C75 C74 120.6(7) . . ? C76 C75 H75 119.7 . . ? C74 C75 H75 119.7 . . ? C77 C76 C75 119.6(7) . . ? C77 C76 H76 120.2 . . ? C75 C76 H76 120.2 . . ? C78 C77 C76 120.6(7) . . ? C78 C77 H77 119.7 . . ? C76 C77 H77 119.7 . . ? C77 C78 C79 120.0(8) . . ? C77 C78 H78 120.0 . . ? C79 C78 H78 120.0 . . ? C74 C79 C78 120.0(7) . . ? C74 C79 H79 120.0 . . ? C78 C79 H79 120.0 . . ? N4 C80 C81 113.4(6) . . ? N4 C80 H80A 108.9 . . ? C81 C80 H80A 108.9 . . ? N4 C80 H80B 108.9 . . ? C81 C80 H80B 108.9 . . ? H80A C80 H80B 107.7 . . ? C90 C81 C82 120.4(6) . . ? C90 C81 C80 120.8(6) . . ? C82 C81 C80 118.7(6) . . ? O4 C82 C83 121.5(6) . . ? O4 C82 C81 119.0(6) . . ? C83 C82 C81 119.5(6) . . ? C82 C83 C84 121.6(7) . . ? C82 C83 C91 118.6(6) . . ? C84 C83 C91 119.7(6) . . ? C85 C84 C83 122.7(7) . . ? C85 C84 C89 118.6(7) . . ? C83 C84 C89 118.5(6) . . ? C86 C85 C84 120.8(8) . . ? C86 C85 H85 119.6 . . ? C84 C85 H85 119.6 . . ? C85 C86 C87 120.6(7) . . ? C85 C86 H86 119.7 . . ? C87 C86 H86 119.7 . . ? C88 C87 C86 120.3(8) . . ? C88 C87 H87 119.9 . . ? C86 C87 H87 119.9 . . ? C87 C88 C89 120.8(8) . . ? C87 C88 H88 119.6 . . ? C89 C88 H88 119.6 . . ? C88 C89 C90 122.4(7) . . ? C88 C89 C84 119.0(7) . . ? C90 C89 C84 118.6(6) . . ? C81 C90 C89 121.1(7) . . ? C81 C90 H90 119.5 . . ? C89 C90 H90 119.5 . . ? C96 C91 C92 119.8(8) . . ? C96 C91 C83 121.1(7) . . ? C92 C91 C83 119.1(7) . . ? C93 C92 C91 120.6(10) . . ? C93 C92 H92 119.7 . . ? C91 C92 H92 119.7 . . ? C92 C93 C94 118.2(11) . . ? C92 C93 H93 120.9 . . ? C94 C93 H93 120.9 . . ? C95 C94 C93 121.0(9) . . ? C95 C94 H94 119.5 . . ? C93 C94 H94 119.5 . . ? C94 C95 C96 120.4(10) . . ? C94 C95 H95 119.8 . . ? C96 C95 H95 119.8 . . ? C91 C96 C95 119.9(10) . . ? C91 C96 H96 120.0 . . ? C95 C96 H96 120.0 . . ? C6X C1X O5 119.3(7) . . ? C6X C1X C2X 121.3(7) . . ? O5 C1X C2X 119.4(7) . . ? C3X C2X C1X 121.0(8) . . ? C3X C2X H2X 119.5 . . ? C1X C2X H2X 119.5 . . ? C9X C8X C7X 121.0(16) . . ? C9X C8X Br1X 123.5(14) . . ? C7X C8X Br1X 115.6(16) . . ? C8X C9X C10X 121.6(17) . . ? C8X C9X H9X 119.2 . . ? C10X C9X H9X 119.2 . . ? C9X C10X C5X 120.8(15) . . ? C9X C10X H10X 119.6 . . ? C5X C10X H10X 119.6 . . ? C6X C5X C4X 122.9(9) . . ? C6X C5X C10X 118.8(11) . . ? C4X C5X C10X 118.2(10) . . ? C1X C6X C5X 117.2(9) . . ? C1X C6X H6X 121.4 . . ? C5X C6X H6X 121.4 . . ? C6Z C5Z C4Z 121.1(12) . . ? C7Z C6Z O1Z 119.9(13) . . ? C7Z C6Z C5Z 121.3(14) . . ? O1Z C6Z C5Z 118.4(12) . . ? C8Z C7Z C6Z 121.2(17) . . ? C7Z C8Z C9Z 121.6(17) . . ? C8X C7X C4X 124.2(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 5.648 _refine_diff_density_min -1.506 _refine_diff_density_rms 0.142