# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- pub.cif' #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. Dr. Franc Meyer' _publ_contact_author_address ; Institut f\"ur Anorganische Chemie Georg August Universit\"at G\"ottingen Tammannstra\&se 4 D-37077 G\"ottingen Germany ; _publ_contact_author_email franc.meyer@chemie.uni-goettingen.de _publ_contact_author_fax 49(551)393063 _publ_contact_author_phone 49(551)393012 _publ_requested_coeditor_name ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Visualising the Carboxylate Shift at a Bioinspired Diiron(II) Site in the Solid State ; loop_ _publ_author_name _publ_author_address B.Burger ; Institut f\"ur Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammannstra\&se 4 D-37077 G\"ottingen Germany ; S.Dechert ; Institut f\"ur Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammannstra\&se 4 D-37077 G\"ottingen Germany ; C.Grosse ; Institut f\"ur Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammannstra\&se 4 D-37077 G\"ottingen Germany ; S.Demeshko ; Institut f\"ur Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammannstra\&se 4 D-37077 G\"ottingen Germany ; F.Meyer ; Institut f\"ur Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammannstra\&se 4 D-37077 G\"ottingen Germany ; #============================================================================== data_1at133K-bb4 _database_code_depnum_ccdc_archive 'CCDC 831479' #TrackingRef '- pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H42 Fe2 N12 O6, 2(C2 H3 N)' _chemical_formula_sum 'C35 H48 Fe2 N14 O6' _chemical_formula_weight 872.57 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 'P 21 21 21' 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 16.2959(3) _cell_length_b 18.9302(3) _cell_length_c 26.2922(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8110.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 76329 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.76 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.777 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7186 _exptl_absorpt_correction_T_max 0.8421 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76329 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 26.76 _reflns_number_total 17205 _reflns_number_gt 16628 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0309P)^2^+6.9806P] 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 0.024(8) _refine_ls_number_reflns 17205 _refine_ls_number_parameters 1046 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 0.22693(2) 0.585328(19) 0.385561(14) 0.01788(8) Uani 1 1 d . . . Fe2 Fe 0.09271(2) 0.717204(19) 0.439370(15) 0.01868(8) Uani 1 1 d . . . Fe11 Fe 0.75386(2) 0.40002(2) 0.407709(14) 0.02040(8) Uani 1 1 d . . . Fe12 Fe 0.56972(2) 0.311066(19) 0.436315(14) 0.01715(7) Uani 1 1 d . . . N1 N 0.20351(12) 0.59453(11) 0.46438(8) 0.0163(4) Uani 1 1 d . . . N2 N 0.16459(13) 0.65058(11) 0.48695(8) 0.0169(4) Uani 1 1 d . . . N3 N 0.31553(13) 0.48980(11) 0.44015(9) 0.0190(4) Uani 1 1 d . . . N4 N 0.23790(15) 0.48913(12) 0.34501(9) 0.0238(5) Uani 1 1 d . . . N5 N 0.26995(17) 0.37956(14) 0.32650(10) 0.0320(6) Uani 1 1 d . . . N6 N 0.35847(14) 0.60597(12) 0.38066(9) 0.0217(5) Uani 1 1 d . . . N7 N 0.48737(14) 0.60837(12) 0.40651(9) 0.0243(5) Uani 1 1 d . . . N8 N 0.04395(14) 0.65437(12) 0.59215(9) 0.0203(4) Uani 1 1 d . . . N9 N -0.01371(14) 0.73619(12) 0.48869(9) 0.0228(5) Uani 1 1 d . . . N10 N -0.11593(14) 0.72428(13) 0.54309(10) 0.0263(5) Uani 1 1 d . . . N11 N -0.0728(2) 0.52776(17) 0.64299(12) 0.0450(8) Uani 1 1 d . . . N12 N -0.04680(16) 0.61688(14) 0.69512(9) 0.0285(5) Uani 1 1 d . . . N21 N 0.71708(13) 0.38011(12) 0.48160(8) 0.0193(4) Uani 1 1 d . . . N22 N 0.64763(13) 0.34472(11) 0.49575(8) 0.0166(4) Uani 1 1 d . . . N23 N 0.85095(14) 0.46297(12) 0.46808(9) 0.0220(5) Uani 1 1 d . . . N24 N 0.87263(15) 0.37334(13) 0.38614(9) 0.0249(5) Uani 1 1 d . . . N25 N 1.00742(15) 0.37685(13) 0.38675(10) 0.0277(5) Uani 1 1 d . . . N26 N 0.75002(14) 0.50631(12) 0.38819(8) 0.0226(4) Uani 1 1 d . . . N27 N 0.77203(14) 0.61922(12) 0.40172(9) 0.0247(5) Uani 1 1 d . . . N28 N 0.51677(14) 0.35134(11) 0.59505(8) 0.0198(4) Uani 1 1 d . . . N29 N 0.45270(14) 0.31219(12) 0.47711(9) 0.0215(4) Uani 1 1 d . . . N30 N 0.35266(14) 0.31689(12) 0.53394(9) 0.0226(5) Uani 1 1 d . . . N31 N 0.6522(2) 0.3436(2) 0.69151(11) 0.0564(10) Uani 1 1 d . . . N32 N 0.5207(2) 0.33645(15) 0.71463(11) 0.0447(8) Uani 1 1 d . . . O1 O 0.09624(13) 0.56506(11) 0.37286(9) 0.0328(5) Uani 1 1 d . . . O2 O 0.01678(13) 0.65550(12) 0.39619(8) 0.0309(5) Uani 1 1 d . . . O3 O 0.19066(11) 0.69645(10) 0.38225(7) 0.0197(4) Uani 1 1 d . . . O4 O 0.21676(14) 0.64944(12) 0.30773(8) 0.0325(5) Uani 1 1 d . . . O5 O 0.15208(13) 0.81690(11) 0.46326(9) 0.0321(5) Uani 1 1 d . . . O6 O 0.06284(14) 0.82085(12) 0.40078(9) 0.0368(5) Uani 1 1 d . . . O11 O 0.68659(11) 0.31038(10) 0.38871(7) 0.0203(4) Uani 1 1 d . . . O12 O 0.71613(14) 0.36219(12) 0.31613(8) 0.0341(5) Uani 1 1 d . . . O13 O 0.55681(14) 0.20809(10) 0.42018(8) 0.0313(5) Uani 1 1 d . A . O14A O 0.6236(3) 0.17354(17) 0.48927(12) 0.0508(10) Uani 0.791(6) 1 d P A 1 O14B O 0.5552(11) 0.1665(6) 0.4978(5) 0.0508(10) Uani 0.209(6) 1 d P A 2 O15 O 0.56062(13) 0.41715(11) 0.40682(8) 0.0287(4) Uani 1 1 d . . . O16 O 0.50545(13) 0.33841(12) 0.35655(8) 0.0306(5) Uani 1 1 d . . . C1 C 0.20938(15) 0.57640(14) 0.54838(10) 0.0194(5) Uani 1 1 d . . . H1 H 0.2212 0.5567 0.5799 0.080 Uiso 1 1 calc R . . C2 C 0.22844(15) 0.55010(13) 0.50098(10) 0.0176(5) Uani 1 1 d . . . C3 C 0.16789(15) 0.64015(13) 0.53793(10) 0.0165(5) Uani 1 1 d . . . C4 C 0.26498(16) 0.48033(13) 0.48552(10) 0.0207(5) Uani 1 1 d . . . H4A H 0.2983 0.4618 0.5130 0.080 Uiso 1 1 calc R . . H4B H 0.2215 0.4467 0.4785 0.080 Uiso 1 1 calc R . . C5 C 0.32491(17) 0.42655(14) 0.40911(11) 0.0241(6) Uani 1 1 d . . . H5A H 0.3053 0.3858 0.4279 0.080 Uiso 1 1 calc R . . H5B H 0.3826 0.4193 0.4016 0.080 Uiso 1 1 calc R . . C6 C 0.27817(16) 0.43293(14) 0.36062(11) 0.0222(5) Uani 1 1 d . . . C7 C 0.2011(2) 0.47109(18) 0.29972(12) 0.0358(7) Uani 1 1 d . . . H7 H 0.1678 0.5004 0.2802 0.080 Uiso 1 1 calc R . . C8 C 0.2215(2) 0.40331(19) 0.28819(13) 0.0421(8) Uani 1 1 d . . . H8 H 0.2054 0.3781 0.2595 0.080 Uiso 1 1 calc R . . C9 C 0.3041(2) 0.30854(18) 0.33110(15) 0.0419(8) Uani 1 1 d . . . H9A H 0.2740 0.2826 0.3563 0.080 Uiso 1 1 calc R . . H9B H 0.3607 0.3116 0.3410 0.080 Uiso 1 1 calc R . . H9C H 0.3001 0.2847 0.2989 0.080 Uiso 1 1 calc R . . C10 C 0.39267(16) 0.52569(14) 0.45224(10) 0.0205(5) Uani 1 1 d . . . H10A H 0.4368 0.4913 0.4540 0.080 Uiso 1 1 calc R . . H10B H 0.3882 0.5485 0.4852 0.080 Uiso 1 1 calc R . . C11 C 0.41198(15) 0.57951(13) 0.41267(10) 0.0190(5) Uani 1 1 d . . . C12 C 0.40168(19) 0.65537(16) 0.35224(12) 0.0285(6) Uani 1 1 d . . . H12 H 0.3797 0.6830 0.3264 0.080 Uiso 1 1 calc R . . C13 C 0.4809(2) 0.65713(17) 0.36803(12) 0.0321(7) Uani 1 1 d . . . H13 H 0.5225 0.6857 0.3553 0.080 Uiso 1 1 calc R . . C14 C 0.56040(17) 0.59367(17) 0.43711(13) 0.0324(6) Uani 1 1 d . . . H14A H 0.5742 0.5445 0.4344 0.080 Uiso 1 1 calc R . . H14B H 0.5495 0.6051 0.4720 0.080 Uiso 1 1 calc R . . H14C H 0.6054 0.6218 0.4250 0.080 Uiso 1 1 calc R . . C15 C 0.12176(16) 0.68627(14) 0.57413(10) 0.0200(5) Uani 1 1 d . . . H15A H 0.1564 0.6962 0.6033 0.080 Uiso 1 1 calc R . . H15B H 0.1097 0.7308 0.5576 0.080 Uiso 1 1 calc R . . C16 C -0.00772(17) 0.63320(14) 0.54860(10) 0.0217(6) Uani 1 1 d . . . H16A H -0.0506 0.6014 0.5601 0.080 Uiso 1 1 calc R . . H16B H 0.0254 0.6085 0.5236 0.080 Uiso 1 1 calc R . . C17 C -0.04503(16) 0.69681(15) 0.52516(11) 0.0222(5) Uani 1 1 d . . . C18 C -0.06809(17) 0.79188(14) 0.48289(12) 0.0266(6) Uani 1 1 d . . . H18 H -0.0622 0.8285 0.4596 0.080 Uiso 1 1 calc R . . C19 C -0.13104(17) 0.78502(16) 0.51615(12) 0.0282(6) Uani 1 1 d . . . H19 H -0.1755 0.8153 0.5200 0.080 Uiso 1 1 calc R . . C20 C -0.16507(18) 0.69529(18) 0.58462(12) 0.0336(7) Uani 1 1 d . . . H20A H -0.1319 0.6917 0.6147 0.080 Uiso 1 1 calc R . . H20B H -0.1847 0.6493 0.5753 0.080 Uiso 1 1 calc R . . H20C H -0.2109 0.7259 0.5912 0.080 Uiso 1 1 calc R . . C21 C 0.05721(17) 0.59374(15) 0.62639(10) 0.0253(6) Uani 1 1 d . . . H21A H 0.1011 0.6045 0.6501 0.080 Uiso 1 1 calc R . . H21B H 0.0734 0.5527 0.6067 0.080 Uiso 1 1 calc R . . C22 C -0.01963(19) 0.57790(16) 0.65500(12) 0.0291(6) Uani 1 1 d . . . C23 C -0.1367(2) 0.5363(2) 0.67713(16) 0.0511(10) Uani 1 1 d . . . H23 H -0.1839 0.5086 0.6778 0.080 Uiso 1 1 calc R . . C24 C -0.1215(2) 0.5898(2) 0.70906(12) 0.0384(8) Uani 1 1 d . . . H24 H -0.1550 0.6054 0.7354 0.080 Uiso 1 1 calc R . . C25 C -0.0047(2) 0.67723(18) 0.71867(12) 0.0387(8) Uani 1 1 d . . . H25A H -0.0229 0.7202 0.7029 0.080 Uiso 1 1 calc R . . H25B H 0.0535 0.6723 0.7142 0.080 Uiso 1 1 calc R . . H25C H -0.0173 0.6786 0.7543 0.080 Uiso 1 1 calc R . . C26 C 0.03105(16) 0.59949(15) 0.37195(10) 0.0215(5) Uani 1 1 d . . . C27 C -0.03653(18) 0.57110(16) 0.33834(11) 0.0270(6) Uani 1 1 d . . . H27A H -0.0389 0.5206 0.3415 0.080 Uiso 1 1 calc R . . H27B H -0.0256 0.5836 0.3036 0.080 Uiso 1 1 calc R . . H27C H -0.0881 0.5911 0.3486 0.080 Uiso 1 1 calc R . . C28 C 0.19642(17) 0.70185(15) 0.33332(10) 0.0226(6) Uani 1 1 d . . . C29 C 0.1801(2) 0.77233(17) 0.30931(12) 0.0332(7) Uani 1 1 d . . . H29A H 0.1875 0.7688 0.2732 0.080 Uiso 1 1 calc R . . H29B H 0.2177 0.8066 0.3228 0.080 Uiso 1 1 calc R . . H29C H 0.1249 0.7866 0.3166 0.080 Uiso 1 1 calc R . . C30 C 0.1147(2) 0.85063(16) 0.42911(13) 0.0332(7) Uani 1 1 d . . . C31 C 0.1315(3) 0.92817(17) 0.42213(17) 0.0505(10) Uani 1 1 d . . . H31A H 0.0894 0.9486 0.4012 0.080 Uiso 1 1 calc R . . H31B H 0.1839 0.9343 0.4060 0.080 Uiso 1 1 calc R . . H31C H 0.1318 0.9511 0.4547 0.080 Uiso 1 1 calc R . . C41 C 0.72051(16) 0.36887(14) 0.56615(10) 0.0209(5) Uani 1 1 d . . . H41 H 0.7368 0.3721 0.6000 0.080 Uiso 1 1 calc R . . C42 C 0.76119(16) 0.39417(13) 0.52363(9) 0.0198(5) Uani 1 1 d . . . C43 C 0.64972(16) 0.33751(13) 0.54695(9) 0.0178(5) Uani 1 1 d . . . C44 C 0.84525(17) 0.42485(15) 0.51739(10) 0.0236(6) Uani 1 1 d . . . H44A H 0.8566 0.4572 0.5451 0.080 Uiso 1 1 calc R . . H44B H 0.8858 0.3874 0.5184 0.080 Uiso 1 1 calc R . . C45 C 0.93390(18) 0.45941(16) 0.44662(11) 0.0270(6) Uani 1 1 d . . . H45A H 0.9732 0.4501 0.4735 0.080 Uiso 1 1 calc R . . H45B H 0.9478 0.5043 0.4311 0.080 Uiso 1 1 calc R . . C46 C 0.93788(17) 0.40228(15) 0.40784(11) 0.0245(5) Uani 1 1 d . . . C47 C 0.9026(2) 0.32789(17) 0.34938(12) 0.0311(6) Uani 1 1 d . . . H47 H 0.8706 0.3003 0.3278 0.080 Uiso 1 1 calc R . . C48 C 0.9860(2) 0.32956(18) 0.34948(13) 0.0334(7) Uani 1 1 d . . . H48 H 1.0212 0.3040 0.3286 0.080 Uiso 1 1 calc R . . C49 C 1.09135(18) 0.39570(18) 0.40074(14) 0.0362(7) Uani 1 1 d . . . H49A H 1.1018 0.3811 0.4351 0.080 Uiso 1 1 calc R . . H49B H 1.0983 0.4459 0.3981 0.080 Uiso 1 1 calc R . . H49C H 1.1291 0.3725 0.3783 0.080 Uiso 1 1 calc R . . C50 C 0.81692(19) 0.53388(16) 0.47110(11) 0.0276(6) Uani 1 1 d . . . H50A H 0.8597 0.5672 0.4801 0.080 Uiso 1 1 calc R . . H50B H 0.7747 0.5356 0.4971 0.080 Uiso 1 1 calc R . . C51 C 0.78071(17) 0.55323(15) 0.42018(10) 0.0217(5) Uani 1 1 d . . . C52 C 0.72050(18) 0.54343(16) 0.34747(11) 0.0265(6) Uani 1 1 d . . . H52 H 0.6956 0.5238 0.3190 0.080 Uiso 1 1 calc R . . C53 C 0.73344(18) 0.61417(16) 0.35527(11) 0.0285(6) Uani 1 1 d . . . H53 H 0.7191 0.6511 0.3337 0.080 Uiso 1 1 calc R . . C54 C 0.7983(2) 0.68454(15) 0.42684(13) 0.0341(7) Uani 1 1 d . . . H54A H 0.8563 0.6825 0.4333 0.080 Uiso 1 1 calc R . . H54B H 0.7694 0.6898 0.4584 0.080 Uiso 1 1 calc R . . H54C H 0.7866 0.7241 0.4052 0.080 Uiso 1 1 calc R . . C55 C 0.58077(16) 0.30240(13) 0.57511(10) 0.0196(5) Uani 1 1 d . . . H55A H 0.5547 0.2687 0.5525 0.080 Uiso 1 1 calc R . . H55B H 0.6037 0.2761 0.6034 0.080 Uiso 1 1 calc R . . C56 C 0.47727(16) 0.39016(14) 0.55298(10) 0.0200(5) Uani 1 1 d . . . H56A H 0.5189 0.4130 0.5324 0.080 Uiso 1 1 calc R . . H56B H 0.4416 0.4265 0.5667 0.080 Uiso 1 1 calc R . . C57 C 0.42828(17) 0.34099(14) 0.52061(10) 0.0206(5) Uani 1 1 d . . . C58 C 0.38964(17) 0.26829(15) 0.46271(12) 0.0263(6) Uani 1 1 d . . . H58 H 0.3895 0.2407 0.4334 0.080 Uiso 1 1 calc R . . C59 C 0.32760(18) 0.27088(14) 0.49720(12) 0.0260(6) Uani 1 1 d . . . H59 H 0.2782 0.2463 0.4960 0.080 Uiso 1 1 calc R . . C60 C 0.30796(19) 0.33289(17) 0.58049(11) 0.0288(6) Uani 1 1 d . . . H60A H 0.2554 0.3100 0.5796 0.080 Uiso 1 1 calc R . . H60B H 0.3004 0.3830 0.5833 0.080 Uiso 1 1 calc R . . H60C H 0.3386 0.3161 0.6093 0.080 Uiso 1 1 calc R . . C61 C 0.55033(17) 0.40028(15) 0.63321(10) 0.0236(5) Uani 1 1 d . . . H61A H 0.5092 0.4352 0.6420 0.080 Uiso 1 1 calc R . . H61B H 0.5974 0.4248 0.6191 0.080 Uiso 1 1 calc R . . C62 C 0.5756(2) 0.36106(16) 0.67993(11) 0.0344(7) Uani 1 1 d . . . C63 C 0.6452(4) 0.3042(3) 0.73583(15) 0.0763(19) Uani 1 1 d . . . H63 H 0.6891 0.2839 0.7531 0.080 Uiso 1 1 calc R . . C64 C 0.5679(4) 0.2995(2) 0.75004(14) 0.0689(17) Uani 1 1 d . . . H64 H 0.5483 0.2758 0.7786 0.080 Uiso 1 1 calc R . . C65 C 0.4326(3) 0.3507(3) 0.71521(15) 0.0639(14) Uani 1 1 d . . . H65A H 0.4081 0.3324 0.6847 0.080 Uiso 1 1 calc R . . H65B H 0.4236 0.4008 0.7170 0.080 Uiso 1 1 calc R . . H65C H 0.4083 0.3284 0.7443 0.080 Uiso 1 1 calc R . . C66 C 0.68892(16) 0.31065(15) 0.33957(10) 0.0210(5) Uani 1 1 d . . . C67 C 0.6614(2) 0.24471(17) 0.31318(11) 0.0302(6) Uani 1 1 d . . . H67A H 0.6513 0.2548 0.2779 0.080 Uiso 1 1 calc R . . H67B H 0.6119 0.2277 0.3287 0.080 Uiso 1 1 calc R . . H67C H 0.7034 0.2093 0.3159 0.080 Uiso 1 1 calc R . . C68 C 0.5832(2) 0.16097(16) 0.44979(12) 0.0336(7) Uani 1 1 d . . . C69 C 0.57779(19) 0.08596(14) 0.43046(12) 0.0301(6) Uani 1 1 d . A . H69A H 0.5919 0.0539 0.4573 0.080 Uiso 1 1 calc R . . H69B H 0.6151 0.0798 0.4026 0.080 Uiso 1 1 calc R . . H69C H 0.5228 0.0765 0.4192 0.080 Uiso 1 1 calc R . . C70 C 0.52646(17) 0.40071(16) 0.36572(11) 0.0250(6) Uani 1 1 d . . . C71 C 0.5092(2) 0.45754(17) 0.32669(12) 0.0335(7) Uani 1 1 d . . . H71A H 0.4528 0.4549 0.3163 0.080 Uiso 1 1 calc R . . H71B H 0.5440 0.4507 0.2977 0.080 Uiso 1 1 calc R . . H71C H 0.5198 0.5031 0.3413 0.080 Uiso 1 1 calc R . . N42 N 0.2759(5) 0.6861(3) 0.67172(18) 0.0937(19) Uani 1 1 d . . . C74 C 0.3271(4) 0.6486(4) 0.6551(2) 0.079(2) Uani 1 1 d . . . C75 C 0.3877(3) 0.6019(4) 0.6357(2) 0.102(3) Uani 1 1 d . . . H75A H 0.3735 0.5883 0.6017 0.080 Uiso 1 1 calc R . . H75B H 0.3906 0.5606 0.6569 0.080 Uiso 1 1 calc R . . H75C H 0.4400 0.6252 0.6355 0.080 Uiso 1 1 calc R . . N43 N 0.2466(3) 0.5334(2) 0.16331(14) 0.0692(11) Uani 1 1 d . . . C76 C 0.2946(3) 0.5428(2) 0.19437(15) 0.0491(10) Uani 1 1 d . . . C77 C 0.3544(3) 0.5564(3) 0.23304(17) 0.0661(13) Uani 1 1 d . . . H77A H 0.3649 0.5138 0.2517 0.080 Uiso 1 1 calc R . . H77B H 0.3340 0.5920 0.2558 0.080 Uiso 1 1 calc R . . H77C H 0.4043 0.5727 0.2176 0.080 Uiso 1 1 calc R . . N44 N 0.9998(3) 0.4637(3) 0.22515(16) 0.0723(12) Uani 1 1 d . . . C78 C 0.9315(3) 0.4623(2) 0.23430(14) 0.0464(9) Uani 1 1 d . . . C79 C 0.8455(3) 0.4641(2) 0.24595(18) 0.0558(10) Uani 1 1 d . . . H79A H 0.8241 0.5101 0.2382 0.080 Uiso 1 1 calc R . . H79B H 0.8377 0.4543 0.2814 0.080 Uiso 1 1 calc R . . H79C H 0.8174 0.4293 0.2260 0.080 Uiso 1 1 calc R . . N45 N 0.6053(3) 0.6724(3) 0.26143(15) 0.0770(13) Uani 1 1 d . . . C80 C 0.5932(3) 0.6633(2) 0.21981(17) 0.0553(10) Uani 1 1 d . . . C81 C 0.5808(4) 0.6514(2) 0.16616(16) 0.0687(14) Uani 1 1 d . . . H81A H 0.5493 0.6895 0.1521 0.080 Uiso 1 1 calc R . . H81B H 0.5519 0.6077 0.1613 0.080 Uiso 1 1 calc R . . H81C H 0.6331 0.6490 0.1494 0.080 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 0.01936(18) 0.01696(17) 0.01733(16) -0.00249(14) 0.00098(14) 0.00019(14) Fe2 0.01641(17) 0.01584(16) 0.02379(18) 0.00130(15) -0.00117(15) 0.00242(13) Fe11 0.02449(19) 0.02079(18) 0.01593(16) 0.00044(14) 0.00124(15) -0.00750(15) Fe12 0.01617(17) 0.01737(16) 0.01791(16) -0.00170(14) -0.00074(14) -0.00209(13) N1 0.0168(10) 0.0135(10) 0.0185(10) -0.0003(8) 0.0019(8) 0.0027(8) N2 0.0150(10) 0.0153(10) 0.0202(10) -0.0009(8) 0.0019(8) 0.0036(8) N3 0.0155(10) 0.0163(10) 0.0251(11) -0.0047(9) 0.0024(9) 0.0009(8) N4 0.0269(13) 0.0236(11) 0.0209(10) -0.0052(9) 0.0002(9) -0.0002(10) N5 0.0318(14) 0.0271(12) 0.0370(14) -0.0158(11) -0.0026(11) 0.0038(11) N6 0.0225(11) 0.0215(11) 0.0212(11) -0.0020(9) 0.0028(9) -0.0032(9) N7 0.0184(11) 0.0240(12) 0.0306(12) -0.0073(10) 0.0024(10) -0.0032(9) N8 0.0198(11) 0.0199(11) 0.0212(11) -0.0044(9) 0.0044(9) 0.0005(8) N9 0.0189(11) 0.0179(11) 0.0317(13) -0.0057(9) -0.0001(10) 0.0045(9) N10 0.0162(11) 0.0306(13) 0.0321(13) -0.0104(11) 0.0006(9) 0.0026(9) N11 0.0456(18) 0.0448(17) 0.0447(17) -0.0089(14) 0.0222(14) -0.0140(14) N12 0.0342(14) 0.0292(13) 0.0220(12) 0.0013(10) 0.0095(10) 0.0058(11) N21 0.0158(10) 0.0267(11) 0.0155(10) 0.0001(8) -0.0010(8) -0.0049(9) N22 0.0158(10) 0.0182(10) 0.0157(10) 0.0012(8) 0.0008(8) -0.0024(8) N23 0.0219(12) 0.0253(12) 0.0187(11) 0.0057(9) -0.0005(9) -0.0085(9) N24 0.0215(11) 0.0287(12) 0.0247(11) 0.0004(10) -0.0017(10) -0.0016(9) N25 0.0213(12) 0.0273(12) 0.0345(13) 0.0116(11) -0.0017(10) 0.0003(10) N26 0.0206(11) 0.0266(11) 0.0206(10) 0.0009(9) -0.0023(9) -0.0025(9) N27 0.0215(11) 0.0219(11) 0.0307(12) 0.0014(9) -0.0043(10) -0.0031(9) N28 0.0239(11) 0.0178(10) 0.0177(10) 0.0000(9) 0.0040(9) 0.0003(9) N29 0.0185(11) 0.0214(11) 0.0246(11) -0.0028(9) 0.0025(9) -0.0010(9) N30 0.0197(11) 0.0232(11) 0.0250(11) 0.0031(10) 0.0041(9) -0.0026(9) N31 0.073(2) 0.073(2) 0.0226(14) -0.0109(15) -0.0105(15) 0.044(2) N32 0.081(2) 0.0295(14) 0.0240(13) -0.0014(11) 0.0055(14) -0.0074(15) O1 0.0195(10) 0.0233(10) 0.0555(14) -0.0074(10) -0.0055(10) 0.0000(8) O2 0.0225(10) 0.0337(11) 0.0366(12) -0.0093(9) -0.0026(9) 0.0024(9) O3 0.0206(9) 0.0210(9) 0.0175(8) 0.0048(7) 0.0003(7) -0.0009(7) O4 0.0411(13) 0.0327(11) 0.0236(10) -0.0040(9) -0.0055(9) 0.0056(10) O5 0.0329(11) 0.0229(10) 0.0406(12) 0.0051(9) 0.0053(10) 0.0035(9) O6 0.0387(12) 0.0276(11) 0.0442(13) 0.0070(10) 0.0037(11) 0.0045(10) O11 0.0179(8) 0.0260(9) 0.0170(8) -0.0046(8) -0.0012(7) -0.0010(7) O12 0.0325(12) 0.0375(12) 0.0324(11) 0.0102(10) -0.0068(9) -0.0081(10) O13 0.0398(12) 0.0181(10) 0.0361(11) 0.0024(8) 0.0034(9) -0.0003(9) O14A 0.088(3) 0.0317(15) 0.0330(16) -0.0067(12) -0.0132(18) -0.0015(18) O14B 0.088(3) 0.0317(15) 0.0330(16) -0.0067(12) -0.0132(18) -0.0015(18) O15 0.0387(12) 0.0238(10) 0.0234(9) 0.0008(8) 0.0005(9) 0.0072(9) O16 0.0244(11) 0.0290(11) 0.0384(12) 0.0001(9) 0.0003(9) 0.0025(8) C1 0.0169(12) 0.0226(13) 0.0186(12) 0.0030(10) -0.0001(9) 0.0026(10) C2 0.0136(11) 0.0172(11) 0.0219(12) 0.0033(10) 0.0033(10) 0.0012(9) C3 0.0122(11) 0.0181(12) 0.0193(12) -0.0014(10) 0.0012(9) 0.0001(9) C4 0.0187(13) 0.0158(11) 0.0275(13) 0.0042(10) 0.0043(11) 0.0025(10) C5 0.0221(13) 0.0208(13) 0.0294(14) -0.0077(11) 0.0005(11) 0.0055(10) C6 0.0148(12) 0.0241(13) 0.0277(13) -0.0090(11) 0.0049(10) -0.0009(10) C7 0.050(2) 0.0356(17) 0.0219(14) -0.0094(13) -0.0096(14) 0.0043(15) C8 0.052(2) 0.0403(18) 0.0345(17) -0.0165(15) -0.0131(15) 0.0053(17) C9 0.0387(18) 0.0285(16) 0.059(2) -0.0222(16) -0.0091(16) 0.0080(14) C10 0.0166(13) 0.0239(13) 0.0209(13) -0.0034(10) -0.0011(10) -0.0016(10) C11 0.0162(12) 0.0176(12) 0.0230(12) -0.0076(10) 0.0047(10) -0.0003(9) C12 0.0288(15) 0.0272(14) 0.0295(15) 0.0027(12) 0.0028(12) -0.0046(12) C13 0.0289(16) 0.0298(15) 0.0375(16) 0.0004(13) 0.0073(13) -0.0117(13) C14 0.0188(13) 0.0352(16) 0.0432(17) -0.0118(15) -0.0013(13) -0.0046(12) C15 0.0206(12) 0.0182(12) 0.0213(12) -0.0023(10) 0.0014(10) -0.0018(10) C16 0.0191(13) 0.0207(13) 0.0253(14) -0.0062(10) 0.0029(10) 0.0012(10) C17 0.0165(12) 0.0226(13) 0.0276(13) -0.0099(11) 0.0003(10) -0.0014(10) C18 0.0224(13) 0.0188(13) 0.0385(15) -0.0067(11) -0.0064(12) 0.0084(11) C19 0.0208(13) 0.0253(14) 0.0387(16) -0.0143(13) -0.0070(12) 0.0068(11) C20 0.0229(14) 0.0397(17) 0.0384(17) -0.0093(14) 0.0108(12) 0.0007(13) C21 0.0258(14) 0.0254(14) 0.0247(13) -0.0006(11) 0.0083(11) 0.0018(11) C22 0.0307(15) 0.0284(15) 0.0283(14) 0.0020(12) 0.0130(12) 0.0002(12) C23 0.040(2) 0.063(3) 0.051(2) -0.0031(19) 0.0217(18) -0.0171(18) C24 0.0370(17) 0.050(2) 0.0281(15) 0.0025(15) 0.0148(13) 0.0090(16) C25 0.053(2) 0.0344(18) 0.0283(16) -0.0032(14) 0.0057(15) 0.0026(15) C26 0.0191(12) 0.0242(13) 0.0211(12) 0.0056(11) 0.0018(10) -0.0049(11) C27 0.0263(15) 0.0304(15) 0.0243(14) 0.0015(12) -0.0039(11) -0.0029(12) C28 0.0208(13) 0.0275(15) 0.0196(12) 0.0008(11) -0.0044(10) -0.0048(11) C29 0.0411(18) 0.0346(17) 0.0238(14) 0.0112(13) -0.0027(13) 0.0001(14) C30 0.0313(16) 0.0247(14) 0.0434(18) 0.0038(14) 0.0116(14) 0.0065(12) C31 0.059(2) 0.0226(16) 0.070(3) 0.0105(16) -0.003(2) -0.0028(15) C41 0.0217(13) 0.0251(13) 0.0159(12) 0.0000(10) -0.0016(10) -0.0022(10) C42 0.0225(13) 0.0197(12) 0.0171(11) -0.0006(9) -0.0045(10) -0.0011(10) C43 0.0215(13) 0.0173(12) 0.0146(11) -0.0001(9) 0.0008(9) 0.0033(10) C44 0.0241(13) 0.0286(14) 0.0182(12) 0.0056(11) -0.0039(10) -0.0072(11) C45 0.0229(13) 0.0300(14) 0.0281(14) 0.0035(11) -0.0019(12) -0.0090(11) C46 0.0227(13) 0.0252(13) 0.0256(13) 0.0103(11) -0.0028(11) -0.0045(11) C47 0.0303(15) 0.0321(16) 0.0310(15) -0.0036(12) -0.0030(13) 0.0014(13) C48 0.0290(16) 0.0336(17) 0.0376(17) 0.0024(13) 0.0001(13) 0.0050(13) C49 0.0183(13) 0.0358(17) 0.054(2) 0.0080(15) -0.0020(13) -0.0029(12) C50 0.0325(16) 0.0280(15) 0.0224(14) -0.0001(12) -0.0103(12) -0.0075(12) C51 0.0188(12) 0.0240(13) 0.0224(13) 0.0009(10) -0.0029(10) -0.0046(10) C52 0.0255(14) 0.0297(15) 0.0243(13) 0.0021(11) -0.0029(11) -0.0008(12) C53 0.0271(15) 0.0294(15) 0.0290(14) 0.0073(11) -0.0034(12) -0.0002(12) C54 0.0385(17) 0.0176(13) 0.0462(18) -0.0017(13) -0.0115(14) -0.0027(12) C55 0.0229(13) 0.0177(12) 0.0182(11) 0.0014(9) 0.0031(10) 0.0011(10) C56 0.0207(12) 0.0177(12) 0.0216(13) 0.0005(10) 0.0019(10) -0.0002(10) C57 0.0201(13) 0.0186(12) 0.0232(13) 0.0019(10) 0.0006(10) -0.0012(10) C58 0.0219(14) 0.0272(14) 0.0299(15) -0.0020(12) 0.0005(11) -0.0053(11) C59 0.0231(14) 0.0183(13) 0.0366(16) 0.0022(12) 0.0021(12) -0.0059(10) C60 0.0254(14) 0.0344(16) 0.0266(14) 0.0049(12) 0.0088(11) -0.0017(12) C61 0.0273(14) 0.0241(13) 0.0192(12) -0.0030(11) 0.0022(10) 0.0020(11) C62 0.059(2) 0.0281(15) 0.0164(13) -0.0043(11) 0.0014(14) 0.0085(15) C63 0.139(5) 0.067(3) 0.0235(18) -0.0113(19) -0.015(3) 0.062(3) C64 0.157(6) 0.032(2) 0.0179(16) -0.0007(14) -0.007(2) 0.013(3) C65 0.080(3) 0.075(3) 0.036(2) -0.009(2) 0.017(2) -0.042(3) C66 0.0161(12) 0.0282(14) 0.0186(12) 0.0010(11) -0.0014(9) 0.0032(11) C67 0.0339(16) 0.0325(16) 0.0241(14) -0.0091(12) -0.0044(12) 0.0004(13) C68 0.0461(19) 0.0233(14) 0.0312(16) -0.0027(12) 0.0067(14) 0.0013(13) C69 0.0341(15) 0.0177(12) 0.0385(16) -0.0039(12) 0.0003(13) 0.0004(12) C70 0.0220(13) 0.0272(15) 0.0259(13) -0.0007(12) 0.0070(11) 0.0081(11) C71 0.0463(19) 0.0310(16) 0.0232(14) 0.0029(12) 0.0012(13) 0.0132(14) N42 0.150(6) 0.082(3) 0.049(3) 0.026(2) -0.041(3) -0.036(4) C74 0.084(4) 0.102(5) 0.052(3) 0.044(3) -0.034(3) -0.046(4) C75 0.039(3) 0.177(7) 0.090(4) 0.078(5) -0.010(3) -0.021(4) N43 0.093(3) 0.072(3) 0.0427(19) 0.0060(18) 0.003(2) -0.004(2) C76 0.066(3) 0.046(2) 0.035(2) 0.0068(16) 0.0130(19) 0.0029(19) C77 0.079(3) 0.071(3) 0.048(2) 0.008(2) -0.001(2) -0.004(3) N44 0.069(3) 0.088(3) 0.060(2) -0.015(2) 0.020(2) 0.000(2) C78 0.056(2) 0.049(2) 0.0334(18) -0.0042(15) 0.0084(17) -0.0134(19) C79 0.048(2) 0.056(3) 0.063(3) 0.002(2) -0.002(2) -0.008(2) N45 0.081(3) 0.109(4) 0.041(2) 0.008(2) -0.0055(19) 0.007(3) C80 0.059(3) 0.054(2) 0.052(2) 0.0096(19) 0.009(2) -0.011(2) C81 0.115(4) 0.049(2) 0.042(2) -0.0008(19) -0.010(3) -0.021(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 N1 2.114(2) . ? Fe1 N4 2.118(2) . ? Fe1 N6 2.183(2) . ? Fe1 O3 2.1868(18) . ? Fe1 O1 2.189(2) . ? Fe1 O4 2.385(2) . ? Fe2 O2 2.046(2) . ? Fe2 N2 2.128(2) . ? Fe2 N9 2.195(2) . ? Fe2 O5 2.212(2) . ? Fe2 O3 2.2265(19) . ? Fe2 O6 2.262(2) . ? Fe11 N21 2.068(2) . ? Fe11 N26 2.078(2) . ? Fe11 N24 2.079(2) . ? Fe11 O11 2.0809(19) . ? Fe12 O13 2.006(2) . ? Fe12 N22 2.112(2) . ? Fe12 O15 2.158(2) . ? Fe12 N29 2.188(2) . ? Fe12 O11 2.2790(18) . ? N1 C2 1.341(3) . ? N1 N2 1.371(3) . ? N2 C3 1.356(3) . ? N3 C5 1.457(3) . ? N3 C4 1.461(3) . ? N3 C10 1.464(3) . ? N4 C6 1.316(4) . ? N4 C7 1.376(4) . ? N5 C8 1.356(4) . ? N5 C6 1.358(3) . ? N5 C9 1.460(4) . ? N6 C11 1.311(4) . ? N6 C12 1.389(4) . ? N7 C11 1.354(3) . ? N7 C13 1.374(4) . ? N7 C14 1.463(4) . ? N8 C21 1.475(4) . ? N8 C16 1.477(3) . ? N8 C15 1.482(3) . ? N9 C17 1.318(4) . ? N9 C18 1.386(3) . ? N10 C17 1.352(3) . ? N10 C19 1.373(4) . ? N10 C20 1.461(4) . ? N11 C22 1.323(4) . ? N11 C23 1.385(4) . ? N12 C22 1.361(4) . ? N12 C24 1.372(4) . ? N12 C25 1.469(4) . ? N21 C42 1.345(3) . ? N21 N22 1.367(3) . ? N22 C43 1.354(3) . ? N23 C50 1.455(4) . ? N23 C45 1.466(4) . ? N23 C44 1.487(3) . ? N24 C46 1.325(4) . ? N24 C47 1.383(4) . ? N25 C46 1.350(4) . ? N25 C48 1.372(4) . ? N25 C49 1.461(4) . ? N26 C51 1.321(3) . ? N26 C52 1.368(4) . ? N27 C51 1.347(4) . ? N27 C53 1.377(4) . ? N27 C54 1.466(4) . ? N28 C61 1.471(3) . ? N28 C56 1.476(3) . ? N28 C55 1.490(3) . ? N29 C57 1.328(3) . ? N29 C58 1.375(4) . ? N30 C57 1.360(3) . ? N30 C59 1.363(4) . ? N30 C60 1.456(4) . ? N31 C62 1.327(5) . ? N31 C63 1.388(6) . ? N32 C62 1.360(5) . ? N32 C64 1.395(6) . ? N32 C65 1.461(6) . ? O1 C26 1.247(3) . ? O2 C26 1.259(4) . ? O3 C28 1.294(3) . ? O4 C28 1.244(4) . ? O5 C30 1.259(4) . ? O6 C30 1.260(4) . ? O11 C66 1.293(3) . ? O12 C66 1.236(4) . ? O13 C68 1.260(4) . ? O14A C68 1.252(5) . ? O14B C68 1.345(14) . ? O15 C70 1.255(4) . ? O16 C70 1.252(4) . ? C1 C2 1.377(4) . ? C1 C3 1.410(4) . ? C2 C4 1.505(3) . ? C3 C15 1.494(3) . ? C5 C6 1.490(4) . ? C7 C8 1.360(5) . ? C10 C11 1.490(4) . ? C12 C13 1.356(5) . ? C16 C17 1.483(4) . ? C18 C19 1.354(4) . ? C21 C22 1.491(4) . ? C23 C24 1.339(6) . ? C26 C27 1.511(4) . ? C28 C29 1.500(4) . ? C30 C31 1.504(4) . ? C41 C42 1.385(4) . ? C41 C43 1.392(4) . ? C42 C44 1.497(4) . ? C43 C55 1.501(4) . ? C45 C46 1.488(4) . ? C47 C48 1.359(5) . ? C50 C51 1.508(4) . ? C52 C53 1.371(4) . ? C56 C57 1.493(4) . ? C58 C59 1.359(4) . ? C61 C62 1.493(4) . ? C63 C64 1.318(8) . ? C66 C67 1.497(4) . ? C68 C69 1.511(4) . ? C70 C71 1.513(4) . ? N42 C74 1.179(9) . ? C74 C75 1.419(10) . ? N43 C76 1.145(6) . ? C76 C77 1.431(6) . ? N44 C78 1.139(6) . ? C78 C79 1.434(6) . ? N45 C80 1.125(6) . ? C80 C81 1.443(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N4 125.42(9) . . ? N1 Fe1 N6 102.73(8) . . ? N4 Fe1 N6 92.37(9) . . ? N1 Fe1 O3 84.89(7) . . ? N4 Fe1 O3 146.10(8) . . ? N6 Fe1 O3 95.21(8) . . ? N1 Fe1 O1 89.33(9) . . ? N4 Fe1 O1 81.64(9) . . ? N6 Fe1 O1 167.85(9) . . ? O3 Fe1 O1 84.24(7) . . ? N1 Fe1 O4 141.86(8) . . ? N4 Fe1 O4 90.66(8) . . ? N6 Fe1 O4 85.78(8) . . ? O3 Fe1 O4 57.15(7) . . ? O1 Fe1 O4 83.73(9) . . ? O2 Fe2 N2 108.71(9) . . ? O2 Fe2 N9 86.76(9) . . ? N2 Fe2 N9 100.65(9) . . ? O2 Fe2 O5 155.42(9) . . ? N2 Fe2 O5 95.63(8) . . ? N9 Fe2 O5 92.19(8) . . ? O2 Fe2 O3 87.62(8) . . ? N2 Fe2 O3 84.10(7) . . ? N9 Fe2 O3 173.58(8) . . ? O5 Fe2 O3 91.63(7) . . ? O2 Fe2 O6 96.67(9) . . ? N2 Fe2 O6 153.69(9) . . ? N9 Fe2 O6 87.30(9) . . ? O5 Fe2 O6 58.76(8) . . ? O3 Fe2 O6 90.27(8) . . ? N21 Fe11 N26 113.57(9) . . ? N21 Fe11 N24 118.81(9) . . ? N26 Fe11 N24 101.29(9) . . ? N21 Fe11 O11 85.66(8) . . ? N26 Fe11 O11 135.61(8) . . ? N24 Fe11 O11 103.11(8) . . ? O13 Fe12 N22 120.84(9) . . ? O13 Fe12 O15 145.20(8) . . ? N22 Fe12 O15 91.52(8) . . ? O13 Fe12 N29 91.24(9) . . ? N22 Fe12 N29 99.11(8) . . ? O15 Fe12 N29 96.16(8) . . ? O13 Fe12 O11 88.05(8) . . ? N22 Fe12 O11 84.59(7) . . ? O15 Fe12 O11 82.26(8) . . ? N29 Fe12 O11 176.04(8) . . ? C2 N1 N2 108.4(2) . . ? C2 N1 Fe1 126.65(17) . . ? N2 N1 Fe1 124.85(16) . . ? C3 N2 N1 107.3(2) . . ? C3 N2 Fe2 133.57(17) . . ? N1 N2 Fe2 117.32(16) . . ? C5 N3 C4 114.6(2) . . ? C5 N3 C10 114.4(2) . . ? C4 N3 C10 111.4(2) . . ? C6 N4 C7 106.7(2) . . ? C6 N4 Fe1 125.48(19) . . ? C7 N4 Fe1 127.8(2) . . ? C8 N5 C6 107.5(3) . . ? C8 N5 C9 126.0(3) . . ? C6 N5 C9 126.4(3) . . ? C11 N6 C12 105.4(2) . . ? C11 N6 Fe1 123.15(18) . . ? C12 N6 Fe1 130.6(2) . . ? C11 N7 C13 106.8(2) . . ? C11 N7 C14 126.5(3) . . ? C13 N7 C14 126.5(2) . . ? C21 N8 C16 110.2(2) . . ? C21 N8 C15 112.8(2) . . ? C16 N8 C15 110.5(2) . . ? C17 N9 C18 105.2(2) . . ? C17 N9 Fe2 130.04(18) . . ? C18 N9 Fe2 124.4(2) . . ? C17 N10 C19 107.2(2) . . ? C17 N10 C20 125.8(3) . . ? C19 N10 C20 127.0(2) . . ? C22 N11 C23 104.7(3) . . ? C22 N12 C24 107.0(3) . . ? C22 N12 C25 126.6(3) . . ? C24 N12 C25 126.4(3) . . ? C42 N21 N22 108.4(2) . . ? C42 N21 Fe11 125.53(18) . . ? N22 N21 Fe11 125.81(16) . . ? C43 N22 N21 107.4(2) . . ? C43 N22 Fe12 136.11(18) . . ? N21 N22 Fe12 116.38(15) . . ? C50 N23 C45 114.5(2) . . ? C50 N23 C44 112.1(2) . . ? C45 N23 C44 111.8(2) . . ? C46 N24 C47 105.9(2) . . ? C46 N24 Fe11 121.9(2) . . ? C47 N24 Fe11 132.1(2) . . ? C46 N25 C48 108.2(2) . . ? C46 N25 C49 126.5(3) . . ? C48 N25 C49 125.3(3) . . ? C51 N26 C52 106.6(2) . . ? C51 N26 Fe11 118.84(18) . . ? C52 N26 Fe11 134.54(19) . . ? C51 N27 C53 107.6(2) . . ? C51 N27 C54 126.1(2) . . ? C53 N27 C54 126.3(2) . . ? C61 N28 C56 111.1(2) . . ? C61 N28 C55 111.8(2) . . ? C56 N28 C55 110.6(2) . . ? C57 N29 C58 105.2(2) . . ? C57 N29 Fe12 133.42(19) . . ? C58 N29 Fe12 120.70(18) . . ? C57 N30 C59 107.6(2) . . ? C57 N30 C60 126.9(2) . . ? C59 N30 C60 125.4(2) . . ? C62 N31 C63 104.4(4) . . ? C62 N32 C64 104.9(4) . . ? C62 N32 C65 126.1(3) . . ? C64 N32 C65 128.8(4) . . ? C26 O1 Fe1 137.75(18) . . ? C26 O2 Fe2 130.56(18) . . ? C28 O3 Fe1 95.51(16) . . ? C28 O3 Fe2 135.12(17) . . ? Fe1 O3 Fe2 109.67(8) . . ? C28 O4 Fe1 87.73(16) . . ? C30 O5 Fe2 91.1(2) . . ? C30 O6 Fe2 88.77(18) . . ? C66 O11 Fe11 102.78(17) . . ? C66 O11 Fe12 124.99(16) . . ? Fe11 O11 Fe12 107.68(8) . . ? C68 O13 Fe12 121.4(2) . . ? C70 O15 Fe12 96.26(18) . . ? C2 C1 C3 104.0(2) . . ? N1 C2 C1 110.7(2) . . ? N1 C2 C4 118.5(2) . . ? C1 C2 C4 130.6(2) . . ? N2 C3 C1 109.6(2) . . ? N2 C3 C15 121.7(2) . . ? C1 C3 C15 128.1(2) . . ? N3 C4 C2 109.6(2) . . ? N3 C5 C6 111.0(2) . . ? N4 C6 N5 110.3(3) . . ? N4 C6 C5 126.0(2) . . ? N5 C6 C5 123.7(3) . . ? C8 C7 N4 108.7(3) . . ? N5 C8 C7 106.8(3) . . ? N3 C10 C11 110.3(2) . . ? N6 C11 N7 111.9(2) . . ? N6 C11 C10 124.7(2) . . ? N7 C11 C10 123.4(2) . . ? C13 C12 N6 109.5(3) . . ? C12 C13 N7 106.4(3) . . ? N8 C15 C3 113.3(2) . . ? N8 C16 C17 109.6(2) . . ? N9 C17 N10 111.5(3) . . ? N9 C17 C16 127.1(2) . . ? N10 C17 C16 121.2(3) . . ? C19 C18 N9 109.9(3) . . ? C18 C19 N10 106.1(2) . . ? N8 C21 C22 110.0(2) . . ? N11 C22 N12 111.2(3) . . ? N11 C22 C21 125.0(3) . . ? N12 C22 C21 123.7(3) . . ? C24 C23 N11 110.8(3) . . ? C23 C24 N12 106.3(3) . . ? O1 C26 O2 126.0(3) . . ? O1 C26 C27 116.5(3) . . ? O2 C26 C27 117.5(2) . . ? O4 C28 O3 119.6(3) . . ? O4 C28 C29 121.9(3) . . ? O3 C28 C29 118.4(3) . . ? O5 C30 O6 121.3(3) . . ? O5 C30 C31 119.6(3) . . ? O6 C30 C31 119.1(3) . . ? C42 C41 C43 104.6(2) . . ? N21 C42 C41 109.8(2) . . ? N21 C42 C44 118.4(2) . . ? C41 C42 C44 131.3(2) . . ? N22 C43 C41 109.8(2) . . ? N22 C43 C55 121.1(2) . . ? C41 C43 C55 129.1(2) . . ? N23 C44 C42 109.9(2) . . ? N23 C45 C46 109.7(2) . . ? N24 C46 N25 110.4(3) . . ? N24 C46 C45 124.1(3) . . ? N25 C46 C45 125.3(3) . . ? C48 C47 N24 109.7(3) . . ? C47 C48 N25 105.7(3) . . ? N23 C50 C51 109.0(2) . . ? N26 C51 N27 110.7(2) . . ? N26 C51 C50 123.3(2) . . ? N27 C51 C50 125.9(2) . . ? N26 C52 C53 109.3(3) . . ? C52 C53 N27 105.7(2) . . ? N28 C55 C43 115.0(2) . . ? N28 C56 C57 110.5(2) . . ? N29 C57 N30 110.8(2) . . ? N29 C57 C56 125.9(2) . . ? N30 C57 C56 123.1(2) . . ? C59 C58 N29 110.5(3) . . ? C58 C59 N30 105.8(2) . . ? N28 C61 C62 110.5(2) . . ? N31 C62 N32 112.3(3) . . ? N31 C62 C61 124.9(3) . . ? N32 C62 C61 122.7(3) . . ? C64 C63 N31 110.7(4) . . ? C63 C64 N32 107.7(4) . . ? O12 C66 O11 120.8(3) . . ? O12 C66 C67 122.3(3) . . ? O11 C66 C67 116.8(3) . . ? O14A C68 O13 123.9(3) . . ? O14A C68 O14B 52.1(7) . . ? O13 C68 O14B 114.1(6) . . ? O14A C68 C69 119.2(3) . . ? O13 C68 C69 116.0(3) . . ? O14B C68 C69 111.6(6) . . ? O16 C70 O15 121.4(3) . . ? O16 C70 C71 119.2(3) . . ? O15 C70 C71 119.4(3) . . ? N42 C74 C75 178.5(6) . . ? N43 C76 C77 178.7(5) . . ? N44 C78 C79 177.2(5) . . ? N45 C80 C81 177.9(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.76 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.617 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.061 data_1at248K-bb60 _database_code_depnum_ccdc_archive 'CCDC 831480' #TrackingRef '- pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H42 Fe2 N12 O6, 2(C2 H3 N)' _chemical_formula_sum 'C35 H48 Fe2 N14 O6' _chemical_formula_weight 872.57 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 'P 21 21 21' 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 16.3776(3) _cell_length_b 19.0030(4) _cell_length_c 26.5500(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8263.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 248(2) _cell_measurement_reflns_used 96951 _cell_measurement_theta_min 1.32 _cell_measurement_theta_max 26.82 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.763 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7110 _exptl_absorpt_correction_T_max 0.8454 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 248(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 96951 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.82 _reflns_number_total 17574 _reflns_number_gt 14817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0526P)^2^+0.2591P] 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 0.014(10) _refine_ls_number_reflns 17574 _refine_ls_number_parameters 1032 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.77225(3) 0.41537(2) 0.613050(16) 0.03824(11) Uani 1 1 d . . . Fe2 Fe 0.90938(3) 0.28579(2) 0.561683(17) 0.03607(10) Uani 1 1 d . . . Fe11 Fe 0.24942(3) 0.59883(2) 0.592242(15) 0.03842(11) Uani 1 1 d . . . Fe12 Fe 0.43169(2) 0.68924(2) 0.562979(15) 0.03228(9) Uani 1 1 d . . . N1 N 0.79732(14) 0.40547(13) 0.53560(8) 0.0304(5) Uani 1 1 d . A . N2 N 0.83690(15) 0.35006(13) 0.51346(9) 0.0316(5) Uani 1 1 d . A . N3 N 0.68556(14) 0.50892(13) 0.55923(10) 0.0349(5) Uani 1 1 d . . . N4 N 0.76506(18) 0.51114(15) 0.65243(9) 0.0426(6) Uani 1 1 d . A . N5 N 0.7345(2) 0.62095(17) 0.67001(12) 0.0580(8) Uani 1 1 d . A . N6 N 0.64217(17) 0.39510(15) 0.61883(10) 0.0433(6) Uani 1 1 d . A . N7 N 0.51347(17) 0.39362(16) 0.59423(11) 0.0493(7) Uani 1 1 d . A . N8 N 0.95857(15) 0.34596(14) 0.40963(9) 0.0360(6) Uani 1 1 d . . . N9 N 1.01558(17) 0.26538(14) 0.51260(11) 0.0417(6) Uani 1 1 d . A . N10 N 1.11690(16) 0.27472(17) 0.45827(11) 0.0481(7) Uani 1 1 d . A . N11 N 1.0736(2) 0.4728(2) 0.35819(14) 0.0703(10) Uani 1 1 d . . . N12 N 1.0479(2) 0.38379(17) 0.30711(11) 0.0512(8) Uani 1 1 d . . . N21 N 0.28570(15) 0.61802(14) 0.51895(9) 0.0338(6) Uani 1 1 d . . . N22 N 0.35435(14) 0.65438(13) 0.50456(8) 0.0300(5) Uani 1 1 d . . . N23 N 0.15322(17) 0.53469(15) 0.53233(10) 0.0414(6) Uani 1 1 d . . . N24 N 0.13051(18) 0.62511(16) 0.61238(11) 0.0471(7) Uani 1 1 d . . . N25 N -0.00394(18) 0.62227(18) 0.61065(13) 0.0544(8) Uani 1 1 d . . . N26 N 0.25223(17) 0.49321(14) 0.61255(9) 0.0402(6) Uani 1 1 d . . . N27 N 0.22930(17) 0.38039(15) 0.60006(10) 0.0441(6) Uani 1 1 d . . . N28 N 0.48285(16) 0.64830(14) 0.40578(9) 0.0350(5) Uani 1 1 d . . . N29 N 0.54827(15) 0.68870(15) 0.52172(10) 0.0393(6) Uani 1 1 d . . . N30 N 0.64715(16) 0.68372(15) 0.46578(10) 0.0397(6) Uani 1 1 d . . . N31 N 0.3470(3) 0.6518(3) 0.31082(12) 0.0855(14) Uani 1 1 d . . . N32 N 0.4759(3) 0.66222(19) 0.28765(12) 0.0700(11) Uani 1 1 d . . . O1A O 0.9062(2) 0.43654(17) 0.62477(12) 0.0542(10) Uiso 0.796(6) 1 d P A 1 O2A O 0.9841(2) 0.3449(2) 0.60431(13) 0.0495(9) Uiso 0.796(6) 1 d P A 1 C26A C 0.9698(2) 0.4014(2) 0.62808(14) 0.0331(9) Uiso 0.796(6) 1 d P A 1 C27A C 1.0314(4) 0.4302(4) 0.6633(3) 0.053(2) Uiso 0.796(6) 1 d P A 1 H27A H 1.0790 0.3998 0.6637 0.080 Uiso 0.796(6) 1 calc PR A 1 H27B H 1.0083 0.4327 0.6969 0.080 Uiso 0.796(6) 1 calc PR A 1 H27C H 1.0473 0.4770 0.6525 0.080 Uiso 0.796(6) 1 calc PR A 1 O1B O 0.9668(8) 0.3878(7) 0.5882(5) 0.052(4) Uiso 0.204(6) 1 d P A 2 O2B O 1.0018(10) 0.3074(9) 0.6364(6) 0.071(5) Uiso 0.204(6) 1 d P A 2 C26B C 0.9941(12) 0.3690(12) 0.6270(7) 0.043(4) Uiso 0.204(6) 1 d P A 2 C27B C 1.0464(11) 0.4223(10) 0.6583(7) 0.020(4) Uiso 0.204(6) 1 d P A 2 H27D H 1.0665 0.3994 0.6885 0.080 Uiso 0.204(6) 1 calc PR A 2 H27E H 1.0130 0.4624 0.6676 0.080 Uiso 0.204(6) 1 calc PR A 2 H27F H 1.0923 0.4382 0.6382 0.080 Uiso 0.204(6) 1 calc PR A 2 O3 O 0.81092(13) 0.30694(13) 0.61805(8) 0.0410(5) Uani 1 1 d . A . O4 O 0.7846(2) 0.35182(16) 0.69160(9) 0.0650(8) Uani 1 1 d . A . O5A O 0.8523(3) 0.1845(3) 0.53734(16) 0.0477(14) Uiso 0.610(10) 1 d P A 3 O6A O 0.9407(3) 0.1804(2) 0.59989(18) 0.0541(15) Uiso 0.610(10) 1 d P A 3 C30A C 0.8891(5) 0.1515(5) 0.5716(3) 0.0555(19) Uiso 0.610(10) 1 d P A 3 C31A C 0.8789(6) 0.0703(5) 0.5736(4) 0.069(3) Uiso 0.610(10) 1 d P A 3 H31A H 0.8374 0.0559 0.5497 0.080 Uiso 0.610(10) 1 calc PR A 3 H31B H 0.8625 0.0564 0.6073 0.080 Uiso 0.610(10) 1 calc PR A 3 H31C H 0.9303 0.0480 0.5652 0.080 Uiso 0.610(10) 1 calc PR A 3 O5B O 0.8255(6) 0.1578(5) 0.5188(3) 0.071(3) Uiso 0.390(10) 1 d P A 4 O6B O 0.9053(7) 0.1840(6) 0.5825(4) 0.076(3) Uiso 0.390(10) 1 d P A 4 C30B C 0.8658(7) 0.1433(6) 0.5569(4) 0.048(3) Uiso 0.390(10) 1 d P A 4 C31B C 0.8557(10) 0.0759(8) 0.5844(6) 0.069(4) Uiso 0.390(10) 1 d P A 4 H31D H 0.8248 0.0432 0.5638 0.080 Uiso 0.390(10) 1 calc PR A 4 H31E H 0.8267 0.0844 0.6157 0.080 Uiso 0.390(10) 1 calc PR A 4 H31F H 0.9090 0.0561 0.5917 0.080 Uiso 0.390(10) 1 calc PR A 4 O11 O 0.31444(12) 0.68872(12) 0.61160(7) 0.0386(5) Uani 1 1 d . . . O12 O 0.28593(18) 0.63807(16) 0.68362(10) 0.0633(7) Uani 1 1 d . . . O13 O 0.44297(18) 0.79142(13) 0.57882(10) 0.0584(7) Uani 1 1 d . B . O14A O 0.3749(3) 0.8258(3) 0.51196(17) 0.0773(12) Uiso 0.737(6) 1 d P B 5 O14B O 0.4380(9) 0.8327(7) 0.5025(5) 0.0773(12) Uiso 0.263(6) 1 d P B 6 O15 O 0.44254(17) 0.58478(14) 0.59427(9) 0.0565(6) Uani 1 1 d . . . O16 O 0.49822(17) 0.66333(16) 0.64244(11) 0.0634(8) Uani 1 1 d . . . C1 C 0.79282(18) 0.42287(17) 0.45249(11) 0.0359(7) Uani 1 1 d . A . H1 H 0.7815 0.4425 0.4208 0.080 Uiso 1 1 calc R . . C2 C 0.77241(17) 0.44921(15) 0.49899(10) 0.0306(6) Uani 1 1 d . . . C3 C 0.83426(17) 0.36021(16) 0.46296(10) 0.0314(6) Uani 1 1 d . . . C4 C 0.73549(19) 0.51806(17) 0.51389(12) 0.0387(7) Uani 1 1 d . A . H4A H 0.7788 0.5524 0.5205 0.080 Uiso 1 1 calc R . . H4B H 0.7015 0.5360 0.4864 0.080 Uiso 1 1 calc R . . C5 C 0.6770(2) 0.57250(18) 0.58988(13) 0.0457(8) Uani 1 1 d . A . H5A H 0.6193 0.5796 0.5982 0.080 Uiso 1 1 calc R . . H5B H 0.6955 0.6133 0.5705 0.080 Uiso 1 1 calc R . . C6 C 0.7246(2) 0.56753(17) 0.63665(12) 0.0410(7) Uani 1 1 d . . . C7 C 0.8026(3) 0.5301(2) 0.69680(14) 0.0663(12) Uani 1 1 d . . . H7 H 0.8363 0.5010 0.7164 0.080 Uiso 1 1 calc R A . C8 C 0.7830(3) 0.5974(3) 0.70759(16) 0.0768(14) Uani 1 1 d . A . H8 H 0.7999 0.6231 0.7360 0.080 Uiso 1 1 calc R . . C9 C 0.6998(3) 0.6916(2) 0.66520(19) 0.0737(13) Uani 1 1 d . . . H9A H 0.7270 0.7165 0.6381 0.080 Uiso 1 1 calc R A . H9B H 0.7074 0.7171 0.6965 0.080 Uiso 1 1 calc R . . H9C H 0.6419 0.6880 0.6578 0.080 Uiso 1 1 calc R . . C10 C 0.60840(19) 0.47390(18) 0.54756(12) 0.0382(7) Uani 1 1 d . A . H10A H 0.6127 0.4502 0.5149 0.080 Uiso 1 1 calc R . . H10B H 0.5647 0.5090 0.5453 0.080 Uiso 1 1 calc R . . C11 C 0.58831(19) 0.42181(16) 0.58705(12) 0.0375(7) Uani 1 1 d . . . C12 C 0.5984(3) 0.3483(2) 0.64807(15) 0.0562(10) Uani 1 1 d . . . H12 H 0.6201 0.3217 0.6747 0.080 Uiso 1 1 calc R A . C13 C 0.5200(3) 0.3465(2) 0.63267(16) 0.0634(11) Uani 1 1 d . A . H13 H 0.4780 0.3182 0.6459 0.080 Uiso 1 1 calc R . . C14 C 0.4407(2) 0.4082(2) 0.56372(17) 0.0618(10) Uani 1 1 d . . . H14A H 0.4234 0.4564 0.5692 0.080 Uiso 1 1 calc R A . H14B H 0.3972 0.3764 0.5734 0.080 Uiso 1 1 calc R . . H14C H 0.4536 0.4014 0.5284 0.080 Uiso 1 1 calc R . . C15 C 0.88132(18) 0.31396(17) 0.42753(11) 0.0358(6) Uani 1 1 d . A . H15A H 0.8938 0.2695 0.4445 0.080 Uiso 1 1 calc R . . H15B H 0.8469 0.3032 0.3983 0.080 Uiso 1 1 calc R . . C16 C 1.0107(2) 0.36645(17) 0.45257(12) 0.0393(7) Uani 1 1 d . A . H16A H 1.0541 0.3979 0.4409 0.080 Uiso 1 1 calc R . . H16B H 0.9779 0.3919 0.4775 0.080 Uiso 1 1 calc R . . C17 C 1.04695(18) 0.30350(18) 0.47600(12) 0.0385(7) Uani 1 1 d . . . C18 C 1.0686(2) 0.20957(19) 0.51879(14) 0.0493(8) Uani 1 1 d . . . H18 H 1.0622 0.1733 0.5425 0.080 Uiso 1 1 calc R A . C19 C 1.1306(2) 0.2148(2) 0.48577(15) 0.0533(9) Uani 1 1 d . A . H19 H 1.1747 0.1835 0.4822 0.080 Uiso 1 1 calc R . . C20 C 1.1662(2) 0.3014(2) 0.41715(15) 0.0606(11) Uani 1 1 d . . . H20A H 1.1327 0.3058 0.3872 0.080 Uiso 1 1 calc R A . H20B H 1.2108 0.2690 0.4106 0.080 Uiso 1 1 calc R . . H20C H 1.1881 0.3471 0.4262 0.080 Uiso 1 1 calc R . . C21 C 0.9453(2) 0.40653(19) 0.37561(12) 0.0453(8) Uani 1 1 d . . . H21A H 0.9292 0.4479 0.3953 0.080 Uiso 1 1 calc R . . H21B H 0.9012 0.3957 0.3519 0.080 Uiso 1 1 calc R . . C22 C 1.0215(2) 0.4220(2) 0.34740(13) 0.0503(9) Uani 1 1 d . . . C23 C 1.1362(3) 0.4654(3) 0.3240(2) 0.0815(15) Uani 1 1 d . . . H23 H 1.1830 0.4940 0.3229 0.080 Uiso 1 1 calc R . . C24 C 1.1215(3) 0.4119(3) 0.29234(16) 0.0673(12) Uani 1 1 d . . . H24 H 1.1546 0.3966 0.2656 0.080 Uiso 1 1 calc R . . C25 C 1.0060(3) 0.3229(3) 0.28510(16) 0.0726(13) Uani 1 1 d . . . H25A H 1.0256 0.2801 0.3009 0.080 Uiso 1 1 calc R . . H25B H 1.0170 0.3210 0.2492 0.080 Uiso 1 1 calc R . . H25C H 0.9477 0.3272 0.2906 0.080 Uiso 1 1 calc R . . C28 C 0.8050(2) 0.30087(19) 0.66599(11) 0.0413(8) Uani 1 1 d . . . C29 C 0.8220(3) 0.2307(2) 0.68940(14) 0.0607(11) Uani 1 1 d . A . H29A H 0.8113 0.2330 0.7253 0.080 Uiso 1 1 calc R . . H29B H 0.8786 0.2181 0.6838 0.080 Uiso 1 1 calc R . . H29C H 0.7869 0.1954 0.6742 0.080 Uiso 1 1 calc R . . C41 C 0.28098(18) 0.62917(17) 0.43525(11) 0.0364(6) Uani 1 1 d . . . H41 H 0.2641 0.6258 0.4015 0.080 Uiso 1 1 calc R . . C42 C 0.24179(19) 0.60366(16) 0.47736(10) 0.0364(6) Uani 1 1 d . . . C43 C 0.35157(18) 0.66120(16) 0.45402(10) 0.0319(6) Uani 1 1 d . . . C44 C 0.1586(2) 0.5721(2) 0.48351(12) 0.0456(8) Uani 1 1 d . . . H44A H 0.1172 0.6093 0.4822 0.080 Uiso 1 1 calc R . . H44B H 0.1479 0.5391 0.4559 0.080 Uiso 1 1 calc R . . C45 C 0.0710(2) 0.5382(2) 0.55326(13) 0.0500(8) Uani 1 1 d . . . H45A H 0.0572 0.4933 0.5693 0.080 Uiso 1 1 calc R . . H45B H 0.0315 0.5468 0.5262 0.080 Uiso 1 1 calc R . . C46 C 0.0662(2) 0.59582(19) 0.59098(12) 0.0446(7) Uani 1 1 d . . . C47 C 0.0996(3) 0.6716(2) 0.64804(16) 0.0605(10) Uani 1 1 d . . . H47 H 0.1312 0.6996 0.6697 0.080 Uiso 1 1 calc R . . C48 C 0.0172(3) 0.6703(2) 0.64680(17) 0.0625(11) Uani 1 1 d . . . H48 H -0.0185 0.6970 0.6668 0.080 Uiso 1 1 calc R . . C49 C -0.0861(2) 0.6034(3) 0.59597(19) 0.0708(12) Uani 1 1 d . . . H49A H -0.0970 0.6210 0.5624 0.080 Uiso 1 1 calc R . . H49B H -0.1247 0.6239 0.6195 0.080 Uiso 1 1 calc R . . H49C H -0.0918 0.5526 0.5962 0.080 Uiso 1 1 calc R . . C50 C 0.1873(2) 0.4645(2) 0.53003(14) 0.0522(9) Uani 1 1 d . . . H50A H 0.2305 0.4626 0.5045 0.080 Uiso 1 1 calc R . . H50B H 0.1447 0.4306 0.5207 0.080 Uiso 1 1 calc R . . C51 C 0.2217(2) 0.44599(18) 0.58106(12) 0.0398(7) Uani 1 1 d . . . C52 C 0.2810(2) 0.4568(2) 0.65292(13) 0.0476(8) Uani 1 1 d . . . H52 H 0.3062 0.4769 0.6813 0.080 Uiso 1 1 calc R . . C53 C 0.2675(2) 0.3866(2) 0.64588(13) 0.0499(9) Uani 1 1 d . . . H53 H 0.2816 0.3499 0.6680 0.080 Uiso 1 1 calc R . . C54 C 0.2027(3) 0.3150(2) 0.57629(17) 0.0619(10) Uani 1 1 d . . . H54A H 0.1458 0.3192 0.5665 0.080 Uiso 1 1 calc R . . H54B H 0.2087 0.2764 0.5999 0.080 Uiso 1 1 calc R . . H54C H 0.2358 0.3060 0.5467 0.080 Uiso 1 1 calc R . . C55 C 0.41952(18) 0.69639(16) 0.42555(10) 0.0339(6) Uani 1 1 d . . . H55A H 0.3958 0.7224 0.3972 0.080 Uiso 1 1 calc R . . H55B H 0.4458 0.7307 0.4478 0.080 Uiso 1 1 calc R . . C56 C 0.52399(18) 0.61008(16) 0.44717(11) 0.0355(7) Uani 1 1 d . . . H56A H 0.5606 0.5743 0.4331 0.080 Uiso 1 1 calc R . . H56B H 0.4831 0.5861 0.4679 0.080 Uiso 1 1 calc R . . C57 C 0.57189(19) 0.65982(17) 0.47905(11) 0.0368(7) Uani 1 1 d . . . C58 C 0.6105(2) 0.7330(2) 0.53591(13) 0.0463(8) Uani 1 1 d . . . H58 H 0.6106 0.7613 0.5650 0.080 Uiso 1 1 calc R . . C59 C 0.6717(2) 0.72981(18) 0.50158(14) 0.0448(8) Uani 1 1 d . . . H59 H 0.7213 0.7546 0.5025 0.080 Uiso 1 1 calc R . . C60 C 0.6922(2) 0.6676(2) 0.41970(13) 0.0516(9) Uani 1 1 d . . . H60A H 0.7425 0.6946 0.4190 0.080 Uiso 1 1 calc R . . H60B H 0.6592 0.6798 0.3907 0.080 Uiso 1 1 calc R . . H60C H 0.7049 0.6178 0.4188 0.080 Uiso 1 1 calc R . . C61 C 0.4500(2) 0.59872(19) 0.36806(11) 0.0439(8) Uani 1 1 d . . . H61A H 0.4035 0.5732 0.3824 0.080 Uiso 1 1 calc R . . H61B H 0.4921 0.5643 0.3590 0.080 Uiso 1 1 calc R . . C62 C 0.4235(3) 0.6376(2) 0.32240(12) 0.0534(10) Uani 1 1 d . . . C63 C 0.3512(5) 0.6905(4) 0.26734(19) 0.112(3) Uani 1 1 d . . . H63 H 0.3057 0.7093 0.2503 0.080 Uiso 1 1 calc R . . C64 C 0.4271(5) 0.6979(3) 0.25276(16) 0.099(2) Uani 1 1 d . . . H64 H 0.4453 0.7225 0.2242 0.080 Uiso 1 1 calc R . . C65 C 0.5639(4) 0.6516(4) 0.28644(18) 0.097(2) Uani 1 1 d . . . H65A H 0.5880 0.6707 0.3169 0.080 Uiso 1 1 calc R . . H65B H 0.5867 0.6755 0.2573 0.080 Uiso 1 1 calc R . . H65C H 0.5757 0.6017 0.2843 0.080 Uiso 1 1 calc R . . C66 C 0.31229(19) 0.68934(19) 0.66027(11) 0.0382(7) Uani 1 1 d . . . C67 C 0.3396(3) 0.7552(2) 0.68570(14) 0.0546(9) Uani 1 1 d . . . H67A H 0.3386 0.7485 0.7219 0.080 Uiso 1 1 calc R . . H67B H 0.3032 0.7935 0.6767 0.080 Uiso 1 1 calc R . . H67C H 0.3947 0.7665 0.6751 0.080 Uiso 1 1 calc R . . C68 C 0.4170(3) 0.8382(2) 0.55048(14) 0.0558(9) Uani 1 1 d . . . C69 C 0.4232(2) 0.91279(18) 0.56929(15) 0.0549(9) Uani 1 1 d . B . H69A H 0.4093 0.9450 0.5423 0.080 Uiso 1 1 calc R . . H69B H 0.4785 0.9219 0.5805 0.080 Uiso 1 1 calc R . . H69C H 0.3857 0.9195 0.5972 0.080 Uiso 1 1 calc R . . C70 C 0.4767(2) 0.6012(2) 0.63441(13) 0.0463(8) Uani 1 1 d . . . C71 C 0.4930(3) 0.5455(2) 0.67339(14) 0.0596(10) Uani 1 1 d . . . H71A H 0.5476 0.5515 0.6868 0.080 Uiso 1 1 calc R . . H71B H 0.4883 0.4993 0.6580 0.080 Uiso 1 1 calc R . . H71C H 0.4534 0.5497 0.7004 0.080 Uiso 1 1 calc R . . N42 N 0.7357(7) 0.3163(6) 0.3241(3) 0.173(4) Uani 1 1 d . . . C74 C 0.6775(7) 0.3449(8) 0.3395(4) 0.159(7) Uani 1 1 d . . . C75 C 0.6130(6) 0.3894(8) 0.3588(4) 0.222(8) Uani 1 1 d . . . H75A H 0.6267 0.4045 0.3927 0.333 Uiso 1 1 calc R . . H75B H 0.5622 0.3632 0.3595 0.333 Uiso 1 1 calc R . . H75C H 0.6069 0.4303 0.3373 0.333 Uiso 1 1 calc R . . N43 N 0.7537(5) 0.4668(4) 0.8355(2) 0.137(2) Uani 1 1 d . . . C76 C 0.7030(5) 0.4597(3) 0.8054(2) 0.100(2) Uani 1 1 d . . . C77 C 0.6465(5) 0.4490(5) 0.7679(3) 0.134(3) Uani 1 1 d . . . H77A H 0.6376 0.4927 0.7498 0.080 Uiso 1 1 calc R . . H77B H 0.5955 0.4333 0.7827 0.080 Uiso 1 1 calc R . . H77C H 0.6665 0.4135 0.7448 0.080 Uiso 1 1 calc R . . N44 N 0.0046(5) 0.5412(5) 0.7747(3) 0.159(3) Uani 1 1 d . . . C78 C 0.0709(4) 0.5412(4) 0.7655(2) 0.0920(17) Uani 1 1 d . . . C79 C 0.1542(4) 0.5370(4) 0.7540(2) 0.1012(18) Uani 1 1 d . . . H79A H 0.1742 0.4903 0.7621 0.080 Uiso 1 1 calc R . . H79B H 0.1839 0.5717 0.7735 0.080 Uiso 1 1 calc R . . H79C H 0.1621 0.5460 0.7183 0.080 Uiso 1 1 calc R . . N45 N 0.6012(4) 0.8286(4) 0.7595(2) 0.144(3) Uani 1 1 d . . . C80 C 0.5907(3) 0.8377(3) 0.7184(2) 0.0836(15) Uani 1 1 d . . . C81 C 0.5805(4) 0.8479(3) 0.66500(19) 0.0966(18) Uani 1 1 d . . . H81A H 0.6331 0.8441 0.6484 0.080 Uiso 1 1 calc R . . H81B H 0.5576 0.8941 0.6588 0.080 Uiso 1 1 calc R . . H81C H 0.5439 0.8122 0.6518 0.080 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 0.0471(3) 0.0320(2) 0.0356(2) -0.00261(18) 0.00413(19) 0.0021(2) Fe2 0.0310(2) 0.0320(2) 0.0451(2) 0.00545(19) -0.00248(19) 0.00413(17) Fe11 0.0442(3) 0.0386(2) 0.03250(19) 0.00052(18) 0.00256(19) -0.0114(2) Fe12 0.0292(2) 0.0332(2) 0.0344(2) -0.00306(18) -0.00186(17) -0.00332(17) N1 0.0278(12) 0.0278(13) 0.0356(12) 0.0032(10) 0.0020(9) 0.0073(10) N2 0.0279(12) 0.0298(13) 0.0372(12) 0.0017(10) 0.0028(10) 0.0053(10) N3 0.0300(13) 0.0306(13) 0.0442(13) -0.0087(11) 0.0012(11) 0.0023(10) N4 0.0443(17) 0.0439(16) 0.0395(13) -0.0080(11) -0.0022(12) -0.0023(13) N5 0.058(2) 0.0494(18) 0.0664(19) -0.0290(15) -0.0019(16) 0.0050(15) N6 0.0449(16) 0.0393(16) 0.0456(15) -0.0007(12) 0.0043(12) -0.0025(13) N7 0.0381(15) 0.0495(18) 0.0603(17) -0.0157(15) 0.0090(13) -0.0100(13) N8 0.0329(13) 0.0366(14) 0.0387(13) -0.0051(11) 0.0045(11) 0.0029(11) N9 0.0362(14) 0.0338(15) 0.0552(16) -0.0073(12) -0.0023(12) 0.0073(11) N10 0.0302(14) 0.0543(19) 0.0600(17) -0.0214(15) -0.0006(12) 0.0074(13) N11 0.070(2) 0.065(2) 0.076(2) -0.0092(18) 0.0350(19) -0.017(2) N12 0.063(2) 0.0487(18) 0.0419(15) 0.0037(13) 0.0186(14) 0.0086(15) N21 0.0270(12) 0.0435(15) 0.0309(12) -0.0014(10) -0.0016(10) -0.0093(11) N22 0.0286(12) 0.0327(13) 0.0288(11) 0.0008(10) 0.0001(9) -0.0046(10) N23 0.0416(15) 0.0431(16) 0.0393(14) 0.0094(12) -0.0031(12) -0.0128(13) N24 0.0415(16) 0.0494(17) 0.0503(15) -0.0022(14) -0.0010(13) -0.0038(13) N25 0.0380(16) 0.058(2) 0.0672(19) 0.0230(17) 0.0004(14) 0.0037(14) N26 0.0376(14) 0.0436(15) 0.0393(12) 0.0012(11) -0.0027(12) -0.0039(12) N27 0.0394(15) 0.0384(15) 0.0544(16) 0.0010(12) -0.0049(12) -0.0039(12) N28 0.0389(14) 0.0336(14) 0.0325(12) -0.0029(11) 0.0027(11) -0.0014(11) N29 0.0308(13) 0.0430(15) 0.0442(14) -0.0025(12) 0.0019(11) -0.0051(12) N30 0.0324(14) 0.0428(15) 0.0438(14) 0.0033(12) 0.0047(11) -0.0052(12) N31 0.098(3) 0.118(4) 0.0402(17) -0.018(2) -0.0118(18) 0.053(3) N32 0.114(3) 0.055(2) 0.0415(17) 0.0001(15) 0.0059(19) -0.010(2) O3 0.0347(11) 0.0495(14) 0.0387(11) 0.0118(10) -0.0005(9) -0.0013(10) O4 0.090(2) 0.0588(18) 0.0458(13) -0.0069(13) -0.0106(14) 0.0114(16) O11 0.0327(11) 0.0488(13) 0.0342(10) -0.0076(10) -0.0039(8) -0.0014(10) O12 0.0664(18) 0.0632(18) 0.0603(15) 0.0172(14) -0.0079(14) -0.0146(14) O13 0.0703(18) 0.0369(13) 0.0678(16) 0.0042(12) 0.0105(13) 0.0024(13) O15 0.0746(18) 0.0522(15) 0.0428(12) 0.0014(12) 0.0015(13) 0.0167(14) O16 0.0494(16) 0.0554(19) 0.085(2) 0.0058(15) 0.0042(14) 0.0058(13) C1 0.0309(15) 0.0415(18) 0.0353(14) 0.0072(12) 0.0001(11) 0.0037(13) C2 0.0227(14) 0.0292(14) 0.0399(14) 0.0057(12) 0.0046(11) 0.0011(11) C3 0.0269(15) 0.0346(16) 0.0327(14) -0.0021(12) -0.0006(11) -0.0003(12) C4 0.0339(17) 0.0347(16) 0.0474(16) 0.0073(13) 0.0076(14) 0.0036(13) C5 0.0397(18) 0.0392(18) 0.0582(19) -0.0172(16) -0.0044(15) 0.0108(14) C6 0.0357(17) 0.0382(18) 0.0490(17) -0.0122(14) 0.0078(14) -0.0026(14) C7 0.088(3) 0.067(3) 0.044(2) -0.0169(19) -0.019(2) 0.005(2) C8 0.100(4) 0.072(3) 0.059(2) -0.025(2) -0.025(2) 0.005(3) C9 0.072(3) 0.054(3) 0.095(3) -0.033(2) -0.010(2) 0.010(2) C10 0.0301(16) 0.0440(19) 0.0404(16) -0.0039(13) -0.0016(12) -0.0034(13) C11 0.0342(16) 0.0323(16) 0.0461(16) -0.0124(13) 0.0084(13) -0.0037(13) C12 0.057(2) 0.045(2) 0.066(2) 0.0033(18) 0.0101(19) -0.0079(18) C13 0.064(3) 0.054(3) 0.073(3) 0.006(2) 0.018(2) -0.023(2) C14 0.0341(18) 0.067(3) 0.084(3) -0.012(2) 0.0022(19) -0.0092(18) C15 0.0370(16) 0.0338(16) 0.0365(15) -0.0060(13) 0.0030(12) -0.0003(13) C16 0.0354(17) 0.0367(18) 0.0459(17) -0.0102(14) 0.0034(13) 0.0022(13) C17 0.0266(14) 0.0410(18) 0.0478(17) -0.0164(15) 0.0018(12) 0.0018(13) C18 0.0406(18) 0.0392(19) 0.068(2) -0.0113(16) -0.0155(17) 0.0112(16) C19 0.0386(19) 0.048(2) 0.073(2) -0.0229(19) -0.0115(17) 0.0162(16) C20 0.0374(19) 0.076(3) 0.069(2) -0.020(2) 0.0177(17) 0.0008(19) C21 0.0454(19) 0.0431(19) 0.0473(17) -0.0011(15) 0.0126(14) 0.0060(16) C22 0.055(2) 0.046(2) 0.0500(19) 0.0019(16) 0.0175(16) 0.0052(18) C23 0.065(3) 0.091(4) 0.089(3) 0.004(3) 0.035(3) -0.017(3) C24 0.072(3) 0.071(3) 0.059(2) 0.005(2) 0.033(2) 0.015(2) C25 0.094(4) 0.065(3) 0.059(2) -0.006(2) 0.015(2) 0.003(3) C28 0.0390(17) 0.050(2) 0.0347(15) 0.0048(15) -0.0066(13) -0.0068(15) C29 0.080(3) 0.057(2) 0.0458(19) 0.0172(18) -0.0071(19) 0.002(2) C41 0.0350(15) 0.0438(17) 0.0304(13) -0.0009(13) -0.0055(13) -0.0049(13) C42 0.0383(16) 0.0384(16) 0.0325(13) 0.0011(12) -0.0055(12) -0.0075(14) C43 0.0331(15) 0.0319(16) 0.0307(14) -0.0016(11) 0.0012(11) 0.0015(12) C44 0.0427(18) 0.056(2) 0.0377(16) 0.0098(15) -0.0088(14) -0.0117(16) C45 0.0416(19) 0.059(2) 0.0499(19) 0.0081(16) -0.0060(16) -0.0139(17) C46 0.0380(17) 0.048(2) 0.0475(17) 0.0117(16) -0.0012(15) -0.0045(16) C47 0.058(2) 0.061(3) 0.063(2) -0.0077(19) -0.0008(19) 0.003(2) C48 0.052(2) 0.063(3) 0.072(3) -0.002(2) 0.004(2) 0.011(2) C49 0.0311(18) 0.079(3) 0.102(3) 0.022(3) -0.003(2) -0.0047(19) C50 0.055(2) 0.048(2) 0.053(2) -0.0026(17) -0.0170(17) -0.0130(18) C51 0.0364(17) 0.0389(17) 0.0443(16) 0.0021(14) -0.0035(13) -0.0052(14) C52 0.046(2) 0.056(2) 0.0415(17) 0.0068(15) -0.0059(15) -0.0019(17) C53 0.045(2) 0.054(2) 0.0508(19) 0.0142(16) -0.0056(16) -0.0015(17) C54 0.064(2) 0.038(2) 0.084(3) 0.0019(19) -0.015(2) -0.0044(18) C55 0.0371(16) 0.0320(15) 0.0325(13) 0.0019(11) 0.0015(11) 0.0020(13) C56 0.0331(15) 0.0338(16) 0.0396(16) 0.0002(13) 0.0017(12) 0.0002(13) C57 0.0323(16) 0.0379(17) 0.0403(15) 0.0052(13) 0.0022(13) -0.0022(13) C58 0.0402(19) 0.051(2) 0.0479(18) -0.0058(16) 0.0002(15) -0.0115(15) C59 0.0346(17) 0.0375(19) 0.062(2) -0.0006(16) 0.0012(15) -0.0096(14) C60 0.0429(19) 0.060(2) 0.0517(19) 0.0081(17) 0.0141(15) -0.0040(17) C61 0.050(2) 0.0418(19) 0.0399(15) -0.0071(14) 0.0003(14) 0.0034(16) C62 0.076(3) 0.050(2) 0.0339(16) -0.0111(15) -0.0015(17) 0.014(2) C63 0.167(7) 0.118(5) 0.050(3) -0.022(3) -0.022(3) 0.084(5) C64 0.198(7) 0.067(3) 0.032(2) -0.002(2) -0.010(3) 0.019(4) C65 0.114(5) 0.121(5) 0.058(3) -0.007(3) 0.020(3) -0.049(4) C66 0.0302(15) 0.0469(19) 0.0374(15) 0.0000(15) -0.0025(12) 0.0042(14) C67 0.062(2) 0.054(2) 0.0474(19) -0.0156(17) -0.0081(17) 0.0004(19) C68 0.069(3) 0.042(2) 0.056(2) -0.0006(17) 0.0064(19) 0.0020(19) C69 0.058(2) 0.0343(17) 0.072(2) -0.0053(18) -0.0006(19) 0.0014(17) C70 0.0413(18) 0.047(2) 0.0508(19) 0.0003(16) 0.0098(15) 0.0164(17) C71 0.077(3) 0.057(2) 0.0448(19) 0.0062(18) -0.0006(18) 0.019(2) N42 0.234(11) 0.182(9) 0.104(5) 0.041(5) -0.077(7) -0.067(10) C74 0.136(9) 0.242(16) 0.099(7) 0.097(9) -0.060(6) -0.075(10) C75 0.090(6) 0.40(2) 0.179(9) 0.150(12) -0.003(6) -0.003(9) N43 0.207(8) 0.121(5) 0.082(3) 0.013(3) 0.011(4) -0.001(5) C76 0.146(6) 0.087(4) 0.067(3) 0.012(3) 0.023(4) 0.014(4) C77 0.143(7) 0.166(8) 0.094(5) 0.020(5) 0.022(5) 0.014(6) N44 0.149(7) 0.190(8) 0.138(5) -0.035(5) 0.040(5) 0.019(6) C78 0.091(4) 0.114(5) 0.071(3) -0.018(3) 0.017(3) -0.005(4) C79 0.086(4) 0.108(5) 0.110(4) -0.005(4) -0.004(3) -0.017(4) N45 0.160(6) 0.198(7) 0.073(3) -0.010(4) 0.000(3) -0.026(5) C80 0.078(3) 0.103(4) 0.070(3) -0.013(3) 0.008(3) 0.012(3) C81 0.130(5) 0.079(4) 0.081(3) 0.002(3) -0.010(3) 0.019(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 N4 2.102(3) . ? Fe1 N1 2.105(2) . ? Fe1 O3 2.160(2) . ? Fe1 N6 2.170(3) . ? Fe1 O1A 2.252(3) . ? Fe2 O2A 2.010(4) . ? Fe2 O6B 2.013(11) . ? Fe2 N2 2.131(2) . ? Fe2 N9 2.208(3) . ? Fe2 O5A 2.235(5) . ? Fe2 O3 2.236(2) . ? Fe2 O1B 2.266(13) . ? Fe2 O6A 2.303(5) . ? Fe11 N21 2.067(2) . ? Fe11 O11 2.078(2) . ? Fe11 N26 2.079(3) . ? Fe11 N24 2.080(3) . ? Fe12 O13 1.995(3) . ? Fe12 N22 2.109(2) . ? Fe12 O15 2.159(3) . ? Fe12 N29 2.201(3) . ? Fe12 O11 2.314(2) . ? N1 C2 1.342(4) . ? N1 N2 1.369(3) . ? N2 C3 1.355(4) . ? N3 C10 1.461(4) . ? N3 C5 1.463(4) . ? N3 C4 1.465(4) . ? N4 C6 1.328(4) . ? N4 C7 1.377(4) . ? N5 C8 1.352(5) . ? N5 C6 1.357(4) . ? N5 C9 1.463(6) . ? N6 C11 1.322(4) . ? N6 C12 1.381(5) . ? N7 C11 1.351(4) . ? N7 C13 1.362(5) . ? N7 C14 1.467(5) . ? N8 C16 1.476(4) . ? N8 C21 1.479(4) . ? N8 C15 1.482(4) . ? N9 C17 1.316(4) . ? N9 C18 1.380(4) . ? N10 C17 1.354(4) . ? N10 C19 1.371(5) . ? N10 C20 1.449(5) . ? N11 C22 1.320(5) . ? N11 C23 1.378(5) . ? N12 C22 1.363(4) . ? N12 C24 1.375(5) . ? N12 C25 1.468(6) . ? N21 C42 1.346(4) . ? N21 N22 1.374(3) . ? N22 C43 1.349(4) . ? N23 C50 1.448(5) . ? N23 C45 1.459(5) . ? N23 C44 1.481(4) . ? N24 C46 1.320(4) . ? N24 C47 1.390(5) . ? N25 C46 1.358(5) . ? N25 C48 1.369(6) . ? N25 C49 1.446(5) . ? N26 C51 1.324(4) . ? N26 C52 1.360(4) . ? N27 C51 1.350(4) . ? N27 C53 1.373(4) . ? N27 C54 1.460(5) . ? N28 C61 1.476(4) . ? N28 C55 1.479(4) . ? N28 C56 1.480(4) . ? N29 C57 1.317(4) . ? N29 C58 1.375(4) . ? N30 C59 1.354(4) . ? N30 C57 1.360(4) . ? N30 C60 1.461(4) . ? N31 C62 1.318(6) . ? N31 C63 1.371(7) . ? N32 C62 1.343(5) . ? N32 C64 1.399(7) . ? N32 C65 1.456(7) . ? O1A C26A 1.239(5) . ? O2A C26A 1.268(6) . ? C26A C27A 1.482(8) . ? O1B C26B 1.18(2) . ? O2B C26B 1.20(3) . ? C26B C27B 1.57(3) . ? O3 C28 1.282(4) . ? O4 C28 1.229(4) . ? O5A C30A 1.259(9) . ? O6A C30A 1.258(12) . ? C30A C31A 1.552(13) . ? O5B C30B 1.238(15) . ? O6B C30B 1.216(16) . ? C30B C31B 1.484(18) . ? O11 C66 1.293(4) . ? O12 C66 1.233(4) . ? O13 C68 1.240(5) . ? O14A C68 1.256(6) . ? O14B C68 1.324(13) . ? O15 C70 1.243(4) . ? O16 C70 1.250(5) . ? C1 C2 1.374(4) . ? C1 C3 1.398(4) . ? C2 C4 1.495(4) . ? C3 C15 1.500(4) . ? C5 C6 1.469(5) . ? C7 C8 1.348(6) . ? C10 C11 1.479(5) . ? C12 C13 1.349(6) . ? C16 C17 1.473(5) . ? C18 C19 1.346(5) . ? C21 C22 1.485(5) . ? C23 C24 1.341(7) . ? C28 C29 1.497(5) . ? C41 C42 1.377(4) . ? C41 C43 1.398(4) . ? C42 C44 1.498(4) . ? C43 C55 1.502(4) . ? C45 C46 1.486(5) . ? C47 C48 1.349(6) . ? C50 C51 1.509(5) . ? C52 C53 1.365(5) . ? C56 C57 1.491(4) . ? C58 C59 1.356(5) . ? C61 C62 1.484(5) . ? C63 C64 1.309(10) . ? C66 C67 1.491(5) . ? C68 C69 1.506(5) . ? C70 C71 1.505(5) . ? N42 C74 1.171(16) . ? C74 C75 1.447(18) . ? N43 C76 1.160(10) . ? C76 C77 1.373(10) . ? N44 C78 1.112(8) . ? C78 C79 1.401(9) . ? N45 C80 1.117(7) . ? C80 C81 1.441(7) . ? 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 N4 Fe1 N1 125.03(10) . . ? N4 Fe1 O3 144.28(10) . . ? N1 Fe1 O3 85.27(9) . . ? N4 Fe1 N6 93.64(11) . . ? N1 Fe1 N6 104.16(10) . . ? O3 Fe1 N6 96.56(10) . . ? N4 Fe1 O1A 80.29(11) . . ? N1 Fe1 O1A 87.76(10) . . ? O3 Fe1 O1A 82.89(10) . . ? N6 Fe1 O1A 168.01(11) . . ? O2A Fe2 O6B 113.8(4) . . ? O2A Fe2 N2 110.92(13) . . ? O6B Fe2 N2 134.2(4) . . ? O2A Fe2 N9 87.18(12) . . ? O6B Fe2 N9 91.1(3) . . ? N2 Fe2 N9 100.65(10) . . ? O2A Fe2 O5A 153.99(15) . . ? O6B Fe2 O5A 40.4(4) . . ? N2 Fe2 O5A 94.98(13) . . ? N9 Fe2 O5A 90.43(12) . . ? O2A Fe2 O3 87.82(11) . . ? O6B Fe2 O3 88.0(3) . . ? N2 Fe2 O3 84.11(8) . . ? N9 Fe2 O3 174.07(9) . . ? O5A Fe2 O3 92.68(12) . . ? O2A Fe2 O1B 25.1(3) . . ? O6B Fe2 O1B 138.6(5) . . ? N2 Fe2 O1B 85.8(4) . . ? N9 Fe2 O1B 90.4(3) . . ? O5A Fe2 O1B 178.7(4) . . ? O3 Fe2 O1B 86.4(3) . . ? O2A Fe2 O6A 95.87(17) . . ? O6B Fe2 O6A 18.3(3) . . ? N2 Fe2 O6A 152.54(16) . . ? N9 Fe2 O6A 86.08(13) . . ? O5A Fe2 O6A 58.11(17) . . ? O3 Fe2 O6A 91.27(12) . . ? O1B Fe2 O6A 121.0(4) . . ? N21 Fe11 O11 86.58(9) . . ? N21 Fe11 N26 114.09(10) . . ? O11 Fe11 N26 135.92(10) . . ? N21 Fe11 N24 117.95(11) . . ? O11 Fe11 N24 102.64(10) . . ? N26 Fe11 N24 100.71(11) . . ? O13 Fe12 N22 121.08(11) . . ? O13 Fe12 O15 143.70(11) . . ? N22 Fe12 O15 92.50(10) . . ? O13 Fe12 N29 91.67(11) . . ? N22 Fe12 N29 98.83(9) . . ? O15 Fe12 N29 96.64(11) . . ? O13 Fe12 O11 87.91(10) . . ? N22 Fe12 O11 84.87(8) . . ? O15 Fe12 O11 81.36(9) . . ? N29 Fe12 O11 175.90(9) . . ? C2 N1 N2 108.0(2) . . ? C2 N1 Fe1 126.34(19) . . ? N2 N1 Fe1 125.47(17) . . ? C3 N2 N1 107.5(2) . . ? C3 N2 Fe2 133.93(19) . . ? N1 N2 Fe2 116.53(17) . . ? C10 N3 C5 114.3(2) . . ? C10 N3 C4 111.3(2) . . ? C5 N3 C4 114.4(3) . . ? C6 N4 C7 106.3(3) . . ? C6 N4 Fe1 124.7(2) . . ? C7 N4 Fe1 128.9(3) . . ? C8 N5 C6 107.7(3) . . ? C8 N5 C9 126.6(3) . . ? C6 N5 C9 125.7(3) . . ? C11 N6 C12 105.1(3) . . ? C11 N6 Fe1 122.8(2) . . ? C12 N6 Fe1 131.5(3) . . ? C11 N7 C13 107.2(3) . . ? C11 N7 C14 125.7(3) . . ? C13 N7 C14 127.0(3) . . ? C16 N8 C21 110.6(3) . . ? C16 N8 C15 110.7(2) . . ? C21 N8 C15 112.9(2) . . ? C17 N9 C18 105.4(3) . . ? C17 N9 Fe2 130.3(2) . . ? C18 N9 Fe2 124.0(2) . . ? C17 N10 C19 106.8(3) . . ? C17 N10 C20 126.3(3) . . ? C19 N10 C20 126.9(3) . . ? C22 N11 C23 105.2(4) . . ? C22 N12 C24 107.2(4) . . ? C22 N12 C25 125.8(3) . . ? C24 N12 C25 127.0(3) . . ? C42 N21 N22 108.1(2) . . ? C42 N21 Fe11 125.7(2) . . ? N22 N21 Fe11 125.86(17) . . ? C43 N22 N21 107.3(2) . . ? C43 N22 Fe12 136.2(2) . . ? N21 N22 Fe12 116.42(16) . . ? C50 N23 C45 114.5(3) . . ? C50 N23 C44 112.5(3) . . ? C45 N23 C44 111.5(3) . . ? C46 N24 C47 105.7(3) . . ? C46 N24 Fe11 122.4(2) . . ? C47 N24 Fe11 132.0(3) . . ? C46 N25 C48 107.6(3) . . ? C46 N25 C49 126.3(4) . . ? C48 N25 C49 126.2(4) . . ? C51 N26 C52 106.5(3) . . ? C51 N26 Fe11 118.8(2) . . ? C52 N26 Fe11 134.7(2) . . ? C51 N27 C53 107.1(3) . . ? C51 N27 C54 126.6(3) . . ? C53 N27 C54 126.3(3) . . ? C61 N28 C55 112.3(2) . . ? C61 N28 C56 110.9(2) . . ? C55 N28 C56 111.0(2) . . ? C57 N29 C58 105.9(3) . . ? C57 N29 Fe12 133.2(2) . . ? C58 N29 Fe12 120.3(2) . . ? C59 N30 C57 107.7(3) . . ? C59 N30 C60 125.0(3) . . ? C57 N30 C60 127.2(3) . . ? C62 N31 C63 105.1(5) . . ? C62 N32 C64 105.0(5) . . ? C62 N32 C65 126.7(4) . . ? C64 N32 C65 128.2(5) . . ? C26A O1A Fe1 137.0(3) . . ? C26A O2A Fe2 129.9(3) . . ? O1A C26A O2A 125.2(4) . . ? O1A C26A C27A 114.7(4) . . ? O2A C26A C27A 120.1(5) . . ? C26B O1B Fe2 99.8(14) . . ? O1B C26B O2B 121(2) . . ? O1B C26B C27B 118.4(18) . . ? O2B C26B C27B 117.6(17) . . ? C28 O3 Fe1 97.2(2) . . ? C28 O3 Fe2 134.7(2) . . ? Fe1 O3 Fe2 109.99(9) . . ? C30A O5A Fe2 91.2(6) . . ? C30A O6A Fe2 88.1(5) . . ? O6A C30A O5A 122.3(9) . . ? O6A C30A C31A 119.1(7) . . ? O5A C30A C31A 118.0(9) . . ? C30B O6B Fe2 118.3(9) . . ? O6B C30B O5B 126.9(12) . . ? O6B C30B C31B 109.4(12) . . ? O5B C30B C31B 122.3(12) . . ? C66 O11 Fe11 103.9(2) . . ? C66 O11 Fe12 125.47(18) . . ? Fe11 O11 Fe12 106.91(9) . . ? C68 O13 Fe12 122.6(3) . . ? C70 O15 Fe12 97.8(2) . . ? C2 C1 C3 104.5(2) . . ? N1 C2 C1 110.6(3) . . ? N1 C2 C4 118.3(3) . . ? C1 C2 C4 131.0(3) . . ? N2 C3 C1 109.5(3) . . ? N2 C3 C15 121.4(3) . . ? C1 C3 C15 128.6(3) . . ? N3 C4 C2 109.8(2) . . ? N3 C5 C6 111.5(3) . . ? N4 C6 N5 109.8(3) . . ? N4 C6 C5 125.7(3) . . ? N5 C6 C5 124.5(3) . . ? C8 C7 N4 108.9(4) . . ? C7 C8 N5 107.3(3) . . ? N3 C10 C11 110.3(3) . . ? N6 C11 N7 111.3(3) . . ? N6 C11 C10 124.1(3) . . ? N7 C11 C10 124.6(3) . . ? C13 C12 N6 109.9(4) . . ? C12 C13 N7 106.5(3) . . ? N8 C15 C3 113.5(2) . . ? C17 C16 N8 110.2(3) . . ? N9 C17 N10 111.4(3) . . ? N9 C17 C16 126.9(3) . . ? N10 C17 C16 121.5(3) . . ? C19 C18 N9 109.9(3) . . ? C18 C19 N10 106.5(3) . . ? N8 C21 C22 109.8(3) . . ? N11 C22 N12 110.8(3) . . ? N11 C22 C21 125.3(3) . . ? N12 C22 C21 123.8(4) . . ? C24 C23 N11 110.9(4) . . ? C23 C24 N12 105.9(3) . . ? O4 C28 O3 119.9(3) . . ? O4 C28 C29 121.5(3) . . ? O3 C28 C29 118.6(3) . . ? C42 C41 C43 104.4(3) . . ? N21 C42 C41 110.2(3) . . ? N21 C42 C44 118.6(2) . . ? C41 C42 C44 130.8(3) . . ? N22 C43 C41 109.9(3) . . ? N22 C43 C55 121.2(3) . . ? C41 C43 C55 128.8(3) . . ? N23 C44 C42 110.0(3) . . ? N23 C45 C46 109.8(3) . . ? N24 C46 N25 110.7(3) . . ? N24 C46 C45 124.0(3) . . ? N25 C46 C45 125.2(3) . . ? C48 C47 N24 109.6(4) . . ? C47 C48 N25 106.4(4) . . ? N23 C50 C51 108.7(3) . . ? N26 C51 N27 110.8(3) . . ? N26 C51 C50 123.4(3) . . ? N27 C51 C50 125.8(3) . . ? N26 C52 C53 109.5(3) . . ? C52 C53 N27 106.2(3) . . ? N28 C55 C43 115.0(2) . . ? N28 C56 C57 110.5(2) . . ? N29 C57 N30 110.5(3) . . ? N29 C57 C56 126.7(3) . . ? N30 C57 C56 122.8(3) . . ? C59 C58 N29 109.6(3) . . ? N30 C59 C58 106.4(3) . . ? N28 C61 C62 110.1(3) . . ? N31 C62 N32 112.0(4) . . ? N31 C62 C61 124.8(4) . . ? N32 C62 C61 123.2(4) . . ? C64 C63 N31 110.7(5) . . ? C63 C64 N32 107.1(5) . . ? O12 C66 O11 120.3(3) . . ? O12 C66 C67 122.7(3) . . ? O11 C66 C67 116.9(3) . . ? O13 C68 O14A 123.2(4) . . ? O13 C68 O14B 115.9(7) . . ? O14A C68 O14B 49.0(6) . . ? O13 C68 C69 116.8(3) . . ? O14A C68 C69 119.0(4) . . ? O14B C68 C69 112.1(7) . . ? O15 C70 O16 120.7(4) . . ? O15 C70 C71 119.5(4) . . ? O16 C70 C71 119.8(4) . . ? N42 C74 C75 171.6(15) . . ? N43 C76 C77 176.4(8) . . ? N44 C78 C79 176.7(9) . . ? N45 C80 C81 177.4(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.82 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.496 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.051 data_1-bb70at133K-one-crystal _database_code_depnum_ccdc_archive 'CCDC 831481' #TrackingRef '- pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H42 Fe2 N12 O6, 2(C2 H3 N)' _chemical_formula_sum 'C35 H48 Fe2 N14 O6' _chemical_formula_weight 872.57 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 'P 21 21 21' 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 16.2919(4) _cell_length_b 18.9469(4) _cell_length_c 26.2523(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8103.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 78904 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 26.83 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7661 _exptl_absorpt_correction_T_max 0.8496 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78904 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 26.83 _reflns_number_total 17246 _reflns_number_gt 15179 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0364P)^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 0.003(7) _refine_ls_number_reflns 17246 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 0.77246(2) 0.415270(19) 0.614474(13) 0.01845(8) Uani 1 1 d . . . Fe2 Fe 0.90659(2) 0.283092(19) 0.560592(14) 0.01924(8) Uani 1 1 d . . . Fe11 Fe 0.24583(2) 0.60048(2) 0.592376(13) 0.02210(8) Uani 1 1 d . . . Fe12 Fe 0.429897(19) 0.689422(19) 0.563077(13) 0.01823(7) Uani 1 1 d . . . N1 N 0.79600(11) 0.40577(11) 0.53552(7) 0.0175(4) Uani 1 1 d . . . N2 N 0.83486(12) 0.34967(11) 0.51263(8) 0.0180(4) Uani 1 1 d . . . N3 N 0.68423(11) 0.51078(11) 0.55937(8) 0.0201(4) Uani 1 1 d . . . N4 N 0.76084(13) 0.51174(12) 0.65508(8) 0.0234(5) Uani 1 1 d . . . N5 N 0.72827(14) 0.62143(13) 0.67350(9) 0.0314(5) Uani 1 1 d . . . N6 N 0.64048(12) 0.39448(11) 0.61915(8) 0.0220(4) Uani 1 1 d . . . N7 N 0.51213(12) 0.39245(12) 0.59319(9) 0.0245(5) Uani 1 1 d . . . N8 N 0.95513(12) 0.34583(11) 0.40714(8) 0.0202(4) Uani 1 1 d . . . N9 N 1.01307(12) 0.26403(11) 0.51108(8) 0.0226(5) Uani 1 1 d . . . N10 N 1.11528(12) 0.27598(12) 0.45634(8) 0.0235(5) Uani 1 1 d . . . N11 N 1.07065(15) 0.47378(14) 0.35582(10) 0.0367(6) Uani 1 1 d . . . N12 N 1.04650(14) 0.38359(13) 0.30445(8) 0.0269(5) Uani 1 1 d . . . N21 N 0.28197(12) 0.62015(11) 0.51818(8) 0.0198(4) Uani 1 1 d . . . N22 N 0.35176(12) 0.65549(11) 0.50360(8) 0.0182(4) Uani 1 1 d . . . N23 N 0.14791(12) 0.53751(12) 0.53180(8) 0.0225(5) Uani 1 1 d . . . N24 N 0.12687(13) 0.62690(12) 0.61446(9) 0.0257(5) Uani 1 1 d . . . N25 N -0.00781(13) 0.62384(13) 0.61417(9) 0.0286(5) Uani 1 1 d . . . N26 N 0.25003(12) 0.49392(12) 0.61203(8) 0.0240(4) Uani 1 1 d . . . N27 N 0.22797(13) 0.38110(12) 0.59837(8) 0.0255(5) Uani 1 1 d . . . N28 N 0.48147(12) 0.64852(11) 0.40391(8) 0.0199(4) Uani 1 1 d . . . N29 N 0.54658(12) 0.68803(12) 0.52167(8) 0.0223(4) Uani 1 1 d . . . N30 N 0.64657(12) 0.68274(12) 0.46474(8) 0.0222(4) Uani 1 1 d . . . N31 N 0.34405(18) 0.65430(17) 0.30779(9) 0.0472(8) Uani 1 1 d . . . N32 N 0.47450(17) 0.66442(14) 0.28432(9) 0.0382(6) Uani 1 1 d . . . O1 O 0.90301(11) 0.43561(10) 0.62769(8) 0.0329(5) Uani 1 1 d . . . O2 O 0.98263(11) 0.34506(11) 0.60395(7) 0.0310(4) Uani 1 1 d . . . O3 O 0.80868(10) 0.30397(9) 0.61812(6) 0.0208(4) Uani 1 1 d . . . O4 O 0.78193(12) 0.35077(11) 0.69264(7) 0.0327(4) Uani 1 1 d . . . O5 O 0.84704(11) 0.18336(11) 0.53688(8) 0.0324(4) Uani 1 1 d . . . O6 O 0.93624(12) 0.17939(11) 0.59949(8) 0.0362(5) Uani 1 1 d . . . O11 O 0.31318(9) 0.69068(10) 0.61096(6) 0.0213(4) Uani 1 1 d . . . O12 O 0.28440(12) 0.63863(11) 0.68371(7) 0.0341(5) Uani 1 1 d . . . O13 O 0.44423(12) 0.79224(10) 0.57968(7) 0.0317(4) Uani 1 1 d . A . O14A O 0.3761(2) 0.82646(15) 0.51080(11) 0.0488(9) Uani 0.828(5) 1 d P A 1 O14B O 0.4372(12) 0.8319(7) 0.5022(5) 0.0488(9) Uani 0.172(5) 1 d P A 2 O15 O 0.43921(12) 0.58341(10) 0.59308(7) 0.0308(4) Uani 1 1 d . . . O16 O 0.49434(11) 0.66260(11) 0.64305(8) 0.0330(5) Uani 1 1 d . . . C1 C 0.79017(13) 0.42354(14) 0.45117(9) 0.0199(5) Uani 1 1 d . . . H1 H 0.7783 0.4436 0.4189 0.080 Uiso 1 1 calc R . . C2 C 0.77115(13) 0.44992(13) 0.49863(9) 0.0173(5) Uani 1 1 d . . . C3 C 0.83123(13) 0.36000(13) 0.46168(9) 0.0179(5) Uani 1 1 d . . . C4 C 0.73475(15) 0.51997(13) 0.51377(10) 0.0219(5) Uani 1 1 d . . . H4A H 0.7792 0.5543 0.5207 0.080 Uiso 1 1 calc R . . H4B H 0.7007 0.5387 0.4856 0.080 Uiso 1 1 calc R . . C5 C 0.67474(15) 0.57429(14) 0.59033(10) 0.0242(5) Uani 1 1 d . . . H5A H 0.6158 0.5821 0.5975 0.080 Uiso 1 1 calc R . . H5B H 0.6954 0.6156 0.5711 0.080 Uiso 1 1 calc R . . C6 C 0.72059(15) 0.56796(14) 0.63938(10) 0.0221(5) Uani 1 1 d . . . C7 C 0.79668(18) 0.52997(17) 0.70082(11) 0.0331(7) Uani 1 1 d . . . H7 H 0.8299 0.4999 0.7211 0.080 Uiso 1 1 calc R . . C8 C 0.77698(19) 0.59738(18) 0.71219(11) 0.0402(7) Uani 1 1 d . . . H8 H 0.7937 0.6231 0.7414 0.080 Uiso 1 1 calc R . . C9 C 0.69438(19) 0.69237(18) 0.66858(13) 0.0414(8) Uani 1 1 d . . . H9A H 0.7254 0.7186 0.6428 0.080 Uiso 1 1 calc R . . H9B H 0.6983 0.7168 0.7014 0.080 Uiso 1 1 calc R . . H9C H 0.6367 0.6893 0.6583 0.080 Uiso 1 1 calc R . . C10 C 0.60723(14) 0.47466(14) 0.54741(10) 0.0215(5) Uani 1 1 d . . . H10A H 0.6120 0.4513 0.5138 0.080 Uiso 1 1 calc R . . H10B H 0.5622 0.5097 0.5454 0.080 Uiso 1 1 calc R . . C11 C 0.58729(14) 0.42115(13) 0.58692(9) 0.0200(5) Uani 1 1 d . . . C12 C 0.59708(17) 0.34583(15) 0.64773(10) 0.0279(6) Uani 1 1 d . . . H12 H 0.6193 0.3178 0.6744 0.080 Uiso 1 1 calc R . . C13 C 0.51823(17) 0.34430(15) 0.63191(11) 0.0297(6) Uani 1 1 d . . . H13 H 0.4754 0.3155 0.6450 0.080 Uiso 1 1 calc R . . C14 C 0.43938(15) 0.40773(16) 0.56240(12) 0.0326(6) Uani 1 1 d . . . H14A H 0.4252 0.4578 0.5657 0.080 Uiso 1 1 calc R . . H14B H 0.3934 0.3788 0.5743 0.080 Uiso 1 1 calc R . . H14C H 0.4509 0.3969 0.5266 0.080 Uiso 1 1 calc R . . C15 C 0.87738(14) 0.31353(14) 0.42543(9) 0.0210(5) Uani 1 1 d . . . H15A H 0.8901 0.2683 0.4426 0.080 Uiso 1 1 calc R . . H15B H 0.8419 0.3030 0.3958 0.080 Uiso 1 1 calc R . . C16 C 1.00685(15) 0.36691(14) 0.45080(9) 0.0220(5) Uani 1 1 d . . . H16A H 0.9730 0.3920 0.4764 0.080 Uiso 1 1 calc R . . H16B H 1.0506 0.3994 0.4391 0.080 Uiso 1 1 calc R . . C17 C 1.04419(14) 0.30345(14) 0.47417(9) 0.0215(5) Uani 1 1 d . . . C18 C 1.06763(15) 0.20848(14) 0.51690(10) 0.0251(6) Uani 1 1 d . . . H18 H 1.0617 0.1712 0.5408 0.080 Uiso 1 1 calc R . . C19 C 1.13014(15) 0.21517(15) 0.48379(11) 0.0270(6) Uani 1 1 d . . . H19 H 1.1756 0.1842 0.4800 0.080 Uiso 1 1 calc R . . C20 C 1.16413(16) 0.30446(16) 0.41480(11) 0.0316(6) Uani 1 1 d . . . H20A H 1.1301 0.3081 0.3841 0.080 Uiso 1 1 calc R . . H20B H 1.2107 0.2731 0.4081 0.080 Uiso 1 1 calc R . . H20C H 1.1845 0.3514 0.4242 0.080 Uiso 1 1 calc R . . C21 C 0.94136(15) 0.40624(15) 0.37285(9) 0.0252(5) Uani 1 1 d . . . H21A H 0.9244 0.4480 0.3930 0.080 Uiso 1 1 calc R . . H21B H 0.8968 0.3949 0.3485 0.080 Uiso 1 1 calc R . . C22 C 1.01861(16) 0.42262(15) 0.34421(10) 0.0266(6) Uani 1 1 d . . . C23 C 1.13472(19) 0.46594(18) 0.32191(13) 0.0400(8) Uani 1 1 d . . . H23 H 1.1822 0.4950 0.3211 0.080 Uiso 1 1 calc R . . C24 C 1.12085(18) 0.41139(18) 0.29008(11) 0.0359(7) Uani 1 1 d . . . H24 H 1.1554 0.3955 0.2633 0.080 Uiso 1 1 calc R . . C25 C 1.0056(2) 0.32183(18) 0.28154(12) 0.0384(7) Uani 1 1 d . . . H25A H 1.0282 0.2785 0.2963 0.080 Uiso 1 1 calc R . . H25B H 1.0148 0.3218 0.2447 0.080 Uiso 1 1 calc R . . H25C H 0.9465 0.3241 0.2884 0.080 Uiso 1 1 calc R . . C26 C 0.96826(14) 0.40109(15) 0.62858(9) 0.0228(5) Uani 1 1 d . . . C27 C 1.03602(16) 0.42971(16) 0.66165(10) 0.0280(6) Uani 1 1 d . . . H27A H 1.0380 0.4812 0.6585 0.080 Uiso 1 1 calc R . . H27B H 1.0886 0.4096 0.6508 0.080 Uiso 1 1 calc R . . H27C H 1.0256 0.4169 0.6972 0.080 Uiso 1 1 calc R . . C28 C 0.80260(14) 0.29877(14) 0.66682(9) 0.0217(5) Uani 1 1 d . . . C29 C 0.81865(18) 0.22812(17) 0.69095(11) 0.0329(7) Uani 1 1 d . . . H29A H 0.8106 0.2316 0.7279 0.080 Uiso 1 1 calc R . . H29B H 0.8752 0.2136 0.6838 0.080 Uiso 1 1 calc R . . H29C H 0.7806 0.1931 0.6769 0.080 Uiso 1 1 calc R . . C30 C 0.88458(17) 0.15025(15) 0.57127(12) 0.0317(7) Uani 1 1 d . . . C31 C 0.8672(2) 0.07239(17) 0.57808(16) 0.0510(9) Uani 1 1 d . . . H31A H 0.9119 0.0506 0.5974 0.080 Uiso 1 1 calc R . . H31B H 0.8628 0.0498 0.5446 0.080 Uiso 1 1 calc R . . H31C H 0.8154 0.0664 0.5966 0.080 Uiso 1 1 calc R . . C41 C 0.27786(14) 0.63149(13) 0.43339(9) 0.0207(5) Uani 1 1 d . . . H41 H 0.2608 0.6283 0.3989 0.080 Uiso 1 1 calc R . . C42 C 0.23774(15) 0.60622(13) 0.47618(9) 0.0207(5) Uani 1 1 d . . . C43 C 0.34889(15) 0.66258(13) 0.45242(9) 0.0191(5) Uani 1 1 d . . . C44 C 0.15330(15) 0.57536(15) 0.48261(9) 0.0238(5) Uani 1 1 d . . . H44A H 0.1118 0.6135 0.4816 0.080 Uiso 1 1 calc R . . H44B H 0.1417 0.5423 0.4543 0.080 Uiso 1 1 calc R . . C45 C 0.06538(16) 0.54129(15) 0.55375(10) 0.0281(6) Uani 1 1 d . . . H45A H 0.0513 0.4955 0.5696 0.080 Uiso 1 1 calc R . . H45B H 0.0249 0.5510 0.5265 0.080 Uiso 1 1 calc R . . C46 C 0.06166(15) 0.59817(15) 0.59276(10) 0.0253(5) Uani 1 1 d . . . C47 C 0.09757(17) 0.67228(16) 0.65145(11) 0.0309(6) Uani 1 1 d . . . H47 H 0.1305 0.7003 0.6734 0.080 Uiso 1 1 calc R . . C48 C 0.01413(18) 0.67049(17) 0.65138(12) 0.0344(7) Uani 1 1 d . . . H48 H -0.0217 0.6965 0.6729 0.080 Uiso 1 1 calc R . . C49 C -0.09187(16) 0.60522(17) 0.60002(12) 0.0363(7) Uani 1 1 d . . . H49A H -0.1029 0.6214 0.5652 0.080 Uiso 1 1 calc R . . H49B H -0.1304 0.6278 0.6236 0.080 Uiso 1 1 calc R . . H49C H -0.0986 0.5539 0.6017 0.080 Uiso 1 1 calc R . . C50 C 0.18197(17) 0.46608(15) 0.52910(11) 0.0282(6) Uani 1 1 d . . . H50A H 0.2245 0.4639 0.5022 0.080 Uiso 1 1 calc R . . H50B H 0.1380 0.4321 0.5204 0.080 Uiso 1 1 calc R . . C51 C 0.21906(15) 0.44711(14) 0.57982(9) 0.0216(5) Uani 1 1 d . . . C52 C 0.28010(16) 0.45684(16) 0.65232(10) 0.0280(6) Uani 1 1 d . . . H52 H 0.3061 0.4769 0.6813 0.080 Uiso 1 1 calc R . . C53 C 0.26709(16) 0.38602(16) 0.64462(10) 0.0297(6) Uani 1 1 d . . . H53 H 0.2820 0.3483 0.6666 0.080 Uiso 1 1 calc R . . C54 C 0.20132(18) 0.31562(15) 0.57326(12) 0.0346(7) Uani 1 1 d . . . H54A H 0.1420 0.3174 0.5673 0.080 Uiso 1 1 calc R . . H54B H 0.2143 0.2752 0.5951 0.080 Uiso 1 1 calc R . . H54C H 0.2299 0.3106 0.5406 0.080 Uiso 1 1 calc R . . C55 C 0.41791(14) 0.69738(13) 0.42400(9) 0.0203(5) Uani 1 1 d . . . H55A H 0.3945 0.7242 0.3951 0.080 Uiso 1 1 calc R . . H55B H 0.4448 0.7317 0.4470 0.080 Uiso 1 1 calc R . . C56 C 0.52145(14) 0.60936(13) 0.44588(9) 0.0211(5) Uani 1 1 d . . . H56A H 0.5579 0.5725 0.4316 0.080 Uiso 1 1 calc R . . H56B H 0.4792 0.5859 0.4670 0.080 Uiso 1 1 calc R . . C57 C 0.57058(15) 0.65894(13) 0.47824(9) 0.0205(5) Uani 1 1 d . . . C58 C 0.61007(15) 0.73193(15) 0.53597(10) 0.0254(6) Uani 1 1 d . . . H58 H 0.6105 0.7605 0.5657 0.080 Uiso 1 1 calc R . . C59 C 0.67179(15) 0.72850(14) 0.50150(10) 0.0255(6) Uani 1 1 d . . . H59 H 0.7225 0.7531 0.5027 0.080 Uiso 1 1 calc R . . C60 C 0.69124(16) 0.66621(16) 0.41813(10) 0.0288(6) Uani 1 1 d . . . H60A H 0.7451 0.6892 0.4189 0.080 Uiso 1 1 calc R . . H60B H 0.6601 0.6833 0.3887 0.080 Uiso 1 1 calc R . . H60C H 0.6986 0.6150 0.4155 0.080 Uiso 1 1 calc R . . C61 C 0.44733(15) 0.59973(15) 0.36569(9) 0.0235(5) Uani 1 1 d . . . H61A H 0.3999 0.5743 0.3805 0.080 Uiso 1 1 calc R . . H61B H 0.4894 0.5644 0.3563 0.080 Uiso 1 1 calc R . . C62 C 0.42062(18) 0.63816(15) 0.31932(10) 0.0297(6) Uani 1 1 d . . . C63 C 0.3489(3) 0.6934(2) 0.26389(12) 0.0587(12) Uani 1 1 d . . . H63 H 0.3031 0.7131 0.2465 0.080 Uiso 1 1 calc R . . C64 C 0.4270(3) 0.70011(18) 0.24895(12) 0.0549(11) Uani 1 1 d . . . H64 H 0.4463 0.7246 0.2197 0.080 Uiso 1 1 calc R . . C65 C 0.5626(2) 0.6519(2) 0.28315(13) 0.0547(10) Uani 1 1 d . . . H65A H 0.5875 0.6703 0.3144 0.080 Uiso 1 1 calc R . . H65B H 0.5865 0.6758 0.2536 0.080 Uiso 1 1 calc R . . H65C H 0.5730 0.6010 0.2807 0.080 Uiso 1 1 calc R . . C66 C 0.31100(14) 0.69019(15) 0.66018(9) 0.0220(5) Uani 1 1 d . . . C67 C 0.33880(18) 0.75640(16) 0.68658(11) 0.0311(6) Uani 1 1 d . . . H67A H 0.3459 0.7469 0.7230 0.080 Uiso 1 1 calc R . . H67B H 0.2975 0.7934 0.6820 0.080 Uiso 1 1 calc R . . H67C H 0.3911 0.7720 0.6720 0.080 Uiso 1 1 calc R . . C68 C 0.41553(18) 0.83878(15) 0.55028(11) 0.0315(6) Uani 1 1 d . . . C69 C 0.42132(17) 0.91454(14) 0.56930(11) 0.0315(6) Uani 1 1 d . A . H69A H 0.4068 0.9470 0.5417 0.080 Uiso 1 1 calc R . . H69B H 0.4775 0.9242 0.5806 0.080 Uiso 1 1 calc R . . H69C H 0.3834 0.9212 0.5979 0.080 Uiso 1 1 calc R . . C70 C 0.47352(15) 0.60018(15) 0.63417(10) 0.0259(6) Uani 1 1 d . . . C71 C 0.49168(18) 0.54301(17) 0.67307(11) 0.0333(7) Uani 1 1 d . . . H71A H 0.5485 0.5476 0.6849 0.080 Uiso 1 1 calc R . . H71B H 0.4840 0.4965 0.6574 0.080 Uiso 1 1 calc R . . H71C H 0.4542 0.5479 0.7021 0.080 Uiso 1 1 calc R . . N42 N 0.7199(3) 0.3158(2) 0.32964(14) 0.0787(12) Uani 1 1 d . . . C74 C 0.6715(3) 0.3531(3) 0.34593(16) 0.0627(13) Uani 1 1 d . . . C75 C 0.6108(2) 0.4007(3) 0.36569(18) 0.0815(17) Uani 1 1 d . . . H75A H 0.6037 0.4403 0.3421 0.122 Uiso 1 1 calc R . . H75B H 0.6287 0.4186 0.3989 0.122 Uiso 1 1 calc R . . H75C H 0.5585 0.3757 0.3696 0.122 Uiso 1 1 calc R . . N43 N 0.7535(2) 0.46670(19) 0.83592(12) 0.0650(9) Uani 1 1 d . . . C76 C 0.7047(2) 0.45732(19) 0.80530(13) 0.0463(9) Uani 1 1 d . . . C77 C 0.6436(3) 0.4444(3) 0.76707(15) 0.0629(11) Uani 1 1 d . . . H77A H 0.6664 0.4138 0.7406 0.094 Uiso 1 1 calc R . . H77B H 0.6266 0.4894 0.7519 0.094 Uiso 1 1 calc R . . H77C H 0.5959 0.4214 0.7827 0.094 Uiso 1 1 calc R . . N44 N 0.0017(2) 0.5379(2) 0.77464(14) 0.0745(11) Uani 1 1 d . . . C78 C 0.0696(2) 0.5387(2) 0.76538(12) 0.0466(8) Uani 1 1 d . . . C79 C 0.1560(2) 0.5362(2) 0.75434(16) 0.0553(10) Uani 1 1 d . . . H79A H 0.1861 0.5631 0.7802 0.083 Uiso 1 1 calc R . . H79B H 0.1661 0.5567 0.7207 0.083 Uiso 1 1 calc R . . H79C H 0.1746 0.4870 0.7546 0.083 Uiso 1 1 calc R . . N45 N 0.3958(2) 0.3261(2) 0.73810(12) 0.0620(9) Uani 1 1 d . . . C80 C 0.40728(19) 0.33679(18) 0.78032(13) 0.0399(7) Uani 1 1 d . . . C81 C 0.4201(2) 0.34805(19) 0.83464(12) 0.0468(8) Uani 1 1 d . . . H81A H 0.3681 0.3413 0.8528 0.070 Uiso 1 1 calc R . . H81B H 0.4400 0.3962 0.8403 0.070 Uiso 1 1 calc R . . H81C H 0.4608 0.3142 0.8473 0.070 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 0.01918(16) 0.01611(17) 0.02007(16) -0.00192(14) 0.00092(13) 0.00044(13) Fe2 0.01732(16) 0.01554(17) 0.02485(18) 0.00145(15) -0.00057(14) 0.00198(13) Fe11 0.02627(18) 0.02102(19) 0.01901(16) 0.00014(15) 0.00180(14) -0.00728(15) Fe12 0.01687(15) 0.01790(17) 0.01991(16) -0.00142(15) -0.00092(14) -0.00169(13) N1 0.0162(9) 0.0158(10) 0.0206(10) 0.0002(9) 0.0021(7) 0.0028(8) N2 0.0168(9) 0.0154(11) 0.0218(10) 0.0011(9) 0.0021(8) 0.0033(8) N3 0.0174(9) 0.0177(11) 0.0253(11) -0.0030(9) 0.0014(8) 0.0003(8) N4 0.0243(11) 0.0230(11) 0.0229(10) -0.0039(9) 0.0001(9) -0.0015(9) N5 0.0300(12) 0.0268(13) 0.0374(13) -0.0140(10) -0.0019(10) 0.0031(10) N6 0.0222(10) 0.0209(11) 0.0229(10) -0.0014(9) 0.0018(8) -0.0022(9) N7 0.0192(10) 0.0229(12) 0.0313(12) -0.0089(10) 0.0032(9) -0.0030(9) N8 0.0203(10) 0.0190(11) 0.0213(10) -0.0026(9) 0.0024(8) 0.0016(8) N9 0.0204(10) 0.0179(11) 0.0294(12) -0.0047(9) -0.0004(9) 0.0025(8) N10 0.0169(10) 0.0249(12) 0.0288(11) -0.0070(10) -0.0005(8) 0.0025(9) N11 0.0403(14) 0.0305(14) 0.0393(14) -0.0018(11) 0.0150(11) -0.0072(11) N12 0.0327(12) 0.0258(13) 0.0224(11) 0.0025(10) 0.0066(9) 0.0043(10) N21 0.0164(9) 0.0230(12) 0.0198(10) -0.0001(9) 0.0002(8) -0.0032(8) N22 0.0178(10) 0.0166(11) 0.0201(10) 0.0010(9) 0.0011(8) -0.0026(8) N23 0.0223(11) 0.0226(12) 0.0227(11) 0.0039(9) -0.0006(9) -0.0070(9) N24 0.0235(10) 0.0274(12) 0.0262(11) 0.0000(10) -0.0022(9) -0.0022(9) N25 0.0235(11) 0.0265(13) 0.0357(12) 0.0104(11) -0.0018(10) -0.0013(9) N26 0.0222(10) 0.0259(12) 0.0240(10) 0.0006(9) -0.0004(9) -0.0042(9) N27 0.0216(10) 0.0222(11) 0.0327(12) 0.0011(9) -0.0036(9) -0.0018(9) N28 0.0217(10) 0.0192(11) 0.0187(10) -0.0003(9) 0.0025(8) -0.0004(8) N29 0.0198(10) 0.0219(11) 0.0251(11) -0.0016(10) 0.0008(8) -0.0004(9) N30 0.0201(10) 0.0221(11) 0.0242(11) 0.0037(10) 0.0023(8) 0.0001(9) N31 0.0540(17) 0.065(2) 0.0230(13) -0.0097(13) -0.0065(12) 0.0276(15) N32 0.0606(17) 0.0281(14) 0.0258(12) -0.0004(11) 0.0027(12) -0.0045(12) O1 0.0190(9) 0.0236(10) 0.0562(13) -0.0072(9) -0.0037(9) 0.0012(7) O2 0.0214(9) 0.0330(11) 0.0385(11) -0.0097(9) -0.0036(8) 0.0016(8) O3 0.0210(8) 0.0192(9) 0.0223(9) 0.0030(8) -0.0009(7) -0.0006(7) O4 0.0390(11) 0.0319(12) 0.0272(10) -0.0047(9) -0.0033(8) 0.0043(9) O5 0.0329(10) 0.0231(10) 0.0412(11) 0.0027(9) 0.0056(9) 0.0039(9) O6 0.0347(11) 0.0271(11) 0.0468(12) 0.0075(10) 0.0029(9) 0.0051(9) O11 0.0187(8) 0.0250(9) 0.0201(8) -0.0047(8) -0.0016(7) -0.0008(7) O12 0.0345(11) 0.0350(12) 0.0328(11) 0.0086(9) -0.0077(9) -0.0089(9) O13 0.0366(10) 0.0198(10) 0.0387(11) 0.0005(9) 0.0023(8) 0.0020(8) O14A 0.074(2) 0.0317(15) 0.0403(15) -0.0079(12) -0.0105(16) -0.0006(15) O14B 0.074(2) 0.0317(15) 0.0403(15) -0.0079(12) -0.0105(16) -0.0006(15) O15 0.0413(11) 0.0248(10) 0.0263(9) 0.0015(9) -0.0009(9) 0.0065(9) O16 0.0253(10) 0.0309(12) 0.0427(12) 0.0008(9) 0.0016(8) 0.0032(8) C1 0.0169(11) 0.0214(13) 0.0214(12) 0.0056(10) 0.0004(9) 0.0002(9) C2 0.0121(10) 0.0161(12) 0.0238(12) 0.0048(10) 0.0030(9) 0.0001(9) C3 0.0123(11) 0.0177(13) 0.0238(12) -0.0022(10) 0.0001(9) -0.0006(9) C4 0.0201(12) 0.0171(12) 0.0286(13) 0.0040(10) 0.0030(10) 0.0039(10) C5 0.0222(12) 0.0200(13) 0.0304(14) -0.0061(11) -0.0008(10) 0.0041(10) C6 0.0157(11) 0.0230(14) 0.0276(13) -0.0082(11) 0.0044(10) -0.0023(10) C7 0.0428(17) 0.0315(17) 0.0251(14) -0.0078(12) -0.0068(12) 0.0027(13) C8 0.0455(17) 0.0413(19) 0.0337(15) -0.0150(14) -0.0106(13) 0.0059(15) C9 0.0367(16) 0.0315(17) 0.056(2) -0.0197(16) -0.0083(14) 0.0076(13) C10 0.0165(12) 0.0246(14) 0.0236(13) -0.0018(10) -0.0009(9) -0.0015(10) C11 0.0187(11) 0.0182(12) 0.0231(12) -0.0076(10) 0.0045(9) 0.0005(9) C12 0.0301(14) 0.0240(14) 0.0295(14) 0.0016(12) 0.0046(11) -0.0031(12) C13 0.0302(14) 0.0237(15) 0.0352(15) -0.0019(12) 0.0100(12) -0.0095(12) C14 0.0202(12) 0.0339(16) 0.0437(16) -0.0072(14) 0.0003(12) -0.0026(11) C15 0.0197(11) 0.0195(12) 0.0239(12) -0.0013(11) 0.0004(9) 0.0012(10) C16 0.0198(12) 0.0199(13) 0.0264(14) -0.0031(11) 0.0007(10) 0.0002(10) C17 0.0176(11) 0.0204(13) 0.0263(13) -0.0080(11) 0.0003(9) -0.0010(9) C18 0.0232(12) 0.0171(13) 0.0352(14) -0.0052(11) -0.0079(11) 0.0056(10) C19 0.0207(12) 0.0224(14) 0.0380(15) -0.0114(12) -0.0062(11) 0.0058(10) C20 0.0246(13) 0.0339(16) 0.0363(15) -0.0076(13) 0.0093(11) 0.0024(12) C21 0.0274(13) 0.0227(14) 0.0254(13) 0.0010(11) 0.0060(10) 0.0025(11) C22 0.0289(13) 0.0249(15) 0.0261(13) 0.0056(12) 0.0052(11) 0.0030(11) C23 0.0349(16) 0.0388(19) 0.0462(18) 0.0035(15) 0.0138(14) -0.0077(14) C24 0.0358(15) 0.0413(18) 0.0308(15) 0.0042(14) 0.0117(12) 0.0111(14) C25 0.0483(18) 0.0349(18) 0.0320(15) -0.0035(14) 0.0066(13) 0.0019(14) C26 0.0195(12) 0.0256(15) 0.0232(12) 0.0047(11) 0.0024(9) -0.0058(11) C27 0.0276(14) 0.0312(16) 0.0252(13) 0.0028(12) -0.0013(11) -0.0028(11) C28 0.0188(12) 0.0252(15) 0.0211(12) 0.0001(11) -0.0042(9) -0.0044(10) C29 0.0409(16) 0.0318(17) 0.0261(14) 0.0101(13) -0.0035(12) 0.0006(13) C30 0.0281(14) 0.0228(15) 0.0441(17) 0.0066(13) 0.0133(13) 0.0055(11) C31 0.060(2) 0.0245(17) 0.069(2) 0.0104(16) -0.0011(18) -0.0025(15) C41 0.0219(12) 0.0225(13) 0.0179(12) -0.0013(10) -0.0017(10) -0.0011(10) C42 0.0247(12) 0.0190(12) 0.0185(11) -0.0012(10) -0.0031(9) 0.0019(10) C43 0.0213(12) 0.0151(12) 0.0209(12) 0.0000(10) 0.0006(9) 0.0033(10) C44 0.0238(12) 0.0274(15) 0.0203(12) 0.0041(11) -0.0042(10) -0.0042(11) C45 0.0244(12) 0.0314(15) 0.0284(14) 0.0027(12) -0.0021(11) -0.0082(11) C46 0.0247(12) 0.0252(14) 0.0259(12) 0.0111(12) -0.0030(11) -0.0035(11) C47 0.0310(14) 0.0307(16) 0.0311(15) -0.0024(12) -0.0015(12) 0.0017(12) C48 0.0332(15) 0.0332(17) 0.0367(16) 0.0015(13) 0.0004(12) 0.0055(13) C49 0.0196(12) 0.0343(16) 0.0548(19) 0.0055(15) -0.0026(12) -0.0016(12) C50 0.0324(14) 0.0242(15) 0.0280(14) -0.0005(12) -0.0084(11) -0.0058(11) C51 0.0181(11) 0.0228(13) 0.0240(12) 0.0009(10) 0.0001(9) -0.0019(10) C52 0.0256(13) 0.0316(16) 0.0267(14) 0.0018(12) -0.0029(11) -0.0004(12) C53 0.0251(13) 0.0327(16) 0.0314(14) 0.0067(12) -0.0022(11) -0.0004(11) C54 0.0385(15) 0.0189(14) 0.0463(18) 0.0020(13) -0.0101(13) -0.0020(12) C55 0.0232(12) 0.0189(13) 0.0187(11) 0.0020(9) 0.0019(9) 0.0008(10) C56 0.0202(11) 0.0182(13) 0.0250(13) 0.0005(11) -0.0002(10) 0.0005(9) C57 0.0193(11) 0.0182(12) 0.0241(12) 0.0039(10) 0.0008(10) 0.0000(10) C58 0.0251(13) 0.0247(15) 0.0263(13) -0.0013(11) -0.0024(10) -0.0046(10) C59 0.0226(13) 0.0205(14) 0.0333(14) 0.0018(12) -0.0024(10) -0.0046(10) C60 0.0263(13) 0.0330(16) 0.0270(14) 0.0028(12) 0.0062(11) -0.0011(12) C61 0.0242(12) 0.0233(14) 0.0228(12) -0.0039(11) 0.0011(10) 0.0020(10) C62 0.0418(16) 0.0258(15) 0.0213(13) -0.0071(11) -0.0008(12) 0.0042(12) C63 0.090(3) 0.058(3) 0.0283(17) -0.0113(17) -0.0125(18) 0.044(2) C64 0.116(3) 0.0286(18) 0.0204(14) -0.0017(13) -0.0071(19) 0.007(2) C65 0.059(2) 0.070(3) 0.0356(17) -0.0068(18) 0.0113(16) -0.033(2) C66 0.0158(11) 0.0269(14) 0.0233(12) 0.0001(11) -0.0028(9) 0.0040(10) C67 0.0328(15) 0.0320(16) 0.0285(14) -0.0086(12) -0.0073(12) 0.0014(12) C68 0.0390(16) 0.0230(15) 0.0326(16) -0.0003(12) 0.0078(12) -0.0006(12) C69 0.0353(14) 0.0180(13) 0.0412(16) -0.0062(12) -0.0033(12) 0.0026(11) C70 0.0221(12) 0.0270(16) 0.0286(14) 0.0002(12) 0.0072(10) 0.0085(11) C71 0.0405(16) 0.0323(17) 0.0270(14) 0.0028(13) 0.0028(12) 0.0116(13) N42 0.121(4) 0.071(3) 0.044(2) 0.0177(19) -0.028(2) -0.020(3) C74 0.067(3) 0.076(3) 0.045(2) 0.028(2) -0.024(2) -0.032(2) C75 0.040(2) 0.127(5) 0.078(3) 0.055(3) -0.007(2) -0.017(3) N43 0.090(3) 0.063(2) 0.0421(17) 0.0095(16) 0.0006(19) -0.007(2) C76 0.069(2) 0.037(2) 0.0333(18) 0.0060(15) 0.0120(17) 0.0026(17) C77 0.069(3) 0.071(3) 0.049(2) 0.005(2) -0.0007(19) 0.003(2) N44 0.068(2) 0.091(3) 0.064(2) -0.015(2) 0.0198(19) -0.003(2) C78 0.059(2) 0.049(2) 0.0321(17) -0.0054(15) 0.0075(16) -0.0104(18) C79 0.048(2) 0.054(2) 0.064(2) 0.003(2) -0.0017(18) -0.0086(18) N45 0.067(2) 0.078(3) 0.0412(18) 0.0072(17) -0.0002(15) 0.0039(19) C80 0.0373(16) 0.0406(18) 0.0417(19) 0.0064(15) 0.0062(14) -0.0034(14) C81 0.061(2) 0.039(2) 0.0411(18) -0.0002(16) -0.0051(16) -0.0051(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.116(2) . ? Fe1 N4 2.124(2) . ? Fe1 O1 2.1893(18) . ? Fe1 N6 2.189(2) . ? Fe1 O3 2.1919(18) . ? Fe1 O4 2.393(2) . ? Fe2 O2 2.0516(19) . ? Fe2 N2 2.131(2) . ? Fe2 N9 2.198(2) . ? Fe2 O5 2.214(2) . ? Fe2 O3 2.2321(17) . ? Fe2 O6 2.266(2) . ? Fe11 N21 2.069(2) . ? Fe11 N24 2.084(2) . ? Fe11 N26 2.085(2) . ? Fe11 O11 2.0887(18) . ? Fe12 O13 2.0097(19) . ? Fe12 N22 2.115(2) . ? Fe12 O15 2.163(2) . ? Fe12 N29 2.190(2) . ? Fe12 O11 2.2797(16) . ? N1 C2 1.342(3) . ? N1 N2 1.375(3) . ? N2 C3 1.353(3) . ? N3 C5 1.460(3) . ? N3 C10 1.463(3) . ? N3 C4 1.463(3) . ? N4 C6 1.317(3) . ? N4 C7 1.379(3) . ? N5 C6 1.358(3) . ? N5 C8 1.367(4) . ? N5 C9 1.459(4) . ? N6 C11 1.312(3) . ? N6 C12 1.383(3) . ? N7 C11 1.350(3) . ? N7 C13 1.369(4) . ? N7 C14 1.464(3) . ? N8 C21 1.473(3) . ? N8 C16 1.478(3) . ? N8 C15 1.487(3) . ? N9 C17 1.324(3) . ? N9 C18 1.386(3) . ? N10 C17 1.353(3) . ? N10 C19 1.380(4) . ? N10 C20 1.454(3) . ? N11 C22 1.323(4) . ? N11 C23 1.380(4) . ? N12 C22 1.358(3) . ? N12 C24 1.374(4) . ? N12 C25 1.475(4) . ? N21 C42 1.343(3) . ? N21 N22 1.374(3) . ? N22 C43 1.351(3) . ? N23 C50 1.464(4) . ? N23 C45 1.465(3) . ? N23 C44 1.480(3) . ? N24 C46 1.323(3) . ? N24 C47 1.382(4) . ? N25 C46 1.354(3) . ? N25 C48 1.365(4) . ? N25 C49 1.462(3) . ? N26 C51 1.325(3) . ? N26 C52 1.361(3) . ? N27 C51 1.350(3) . ? N27 C53 1.375(3) . ? N27 C54 1.470(4) . ? N28 C61 1.473(3) . ? N28 C56 1.479(3) . ? N28 C55 1.486(3) . ? N29 C57 1.325(3) . ? N29 C58 1.379(3) . ? N30 C59 1.361(3) . ? N30 C57 1.364(3) . ? N30 C60 1.458(3) . ? N31 C62 1.319(4) . ? N31 C63 1.373(5) . ? N32 C62 1.365(4) . ? N32 C64 1.385(4) . ? N32 C65 1.455(5) . ? O1 C26 1.248(3) . ? O2 C26 1.265(3) . ? O3 C28 1.286(3) . ? O4 C28 1.243(3) . ? O5 C30 1.258(3) . ? O6 C30 1.250(4) . ? O11 C66 1.293(3) . ? O12 C66 1.235(3) . ? O13 C68 1.262(3) . ? O14A C68 1.241(4) . ? O14B C68 1.317(15) . ? O15 C70 1.256(3) . ? O16 C70 1.252(4) . ? C1 C2 1.378(3) . ? C1 C3 1.405(3) . ? C2 C4 1.507(3) . ? C3 C15 1.499(3) . ? C5 C6 1.494(4) . ? C7 C8 1.350(4) . ? C10 C11 1.486(4) . ? C12 C13 1.350(4) . ? C16 C17 1.481(4) . ? C18 C19 1.345(4) . ? C21 C22 1.499(3) . ? C23 C24 1.348(5) . ? C26 C27 1.505(4) . ? C28 C29 1.504(4) . ? C30 C31 1.513(4) . ? C41 C42 1.385(3) . ? C41 C43 1.391(3) . ? C42 C44 1.504(3) . ? C43 C55 1.502(3) . ? C45 C46 1.488(4) . ? C47 C48 1.360(4) . ? C50 C51 1.506(4) . ? C52 C53 1.373(4) . ? C56 C57 1.498(3) . ? C58 C59 1.354(4) . ? C61 C62 1.484(4) . ? C63 C64 1.338(6) . ? C66 C67 1.503(4) . ? C68 C69 1.523(4) . ? C70 C71 1.518(4) . ? N42 C74 1.141(6) . ? C74 C75 1.437(8) . ? N43 C76 1.144(5) . ? C76 C77 1.435(6) . ? N44 C78 1.133(5) . ? C78 C79 1.438(5) . ? N45 C80 1.142(4) . ? C80 C81 1.457(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N4 125.52(8) . . ? N1 Fe1 O1 89.66(8) . . ? N4 Fe1 O1 81.70(8) . . ? N1 Fe1 N6 102.58(8) . . ? N4 Fe1 N6 92.24(8) . . ? O1 Fe1 N6 167.67(8) . . ? N1 Fe1 O3 84.96(7) . . ? N4 Fe1 O3 146.08(7) . . ? O1 Fe1 O3 84.31(7) . . ? N6 Fe1 O3 95.10(7) . . ? N1 Fe1 O4 141.71(7) . . ? N4 Fe1 O4 90.85(7) . . ? O1 Fe1 O4 83.76(8) . . ? N6 Fe1 O4 85.61(7) . . ? O3 Fe1 O4 56.90(7) . . ? O2 Fe2 N2 108.67(8) . . ? O2 Fe2 N9 86.88(8) . . ? N2 Fe2 N9 100.41(8) . . ? O2 Fe2 O5 155.41(8) . . ? N2 Fe2 O5 95.67(8) . . ? N9 Fe2 O5 92.25(7) . . ? O2 Fe2 O3 87.40(7) . . ? N2 Fe2 O3 84.43(7) . . ? N9 Fe2 O3 173.47(7) . . ? O5 Fe2 O3 91.63(7) . . ? O2 Fe2 O6 96.74(8) . . ? N2 Fe2 O6 153.66(8) . . ? N9 Fe2 O6 87.47(8) . . ? O5 Fe2 O6 58.67(8) . . ? O3 Fe2 O6 90.06(7) . . ? N21 Fe11 N24 118.91(8) . . ? N21 Fe11 N26 113.46(9) . . ? N24 Fe11 N26 101.20(9) . . ? N21 Fe11 O11 85.59(7) . . ? N24 Fe11 O11 103.12(8) . . ? N26 Fe11 O11 135.83(8) . . ? O13 Fe12 N22 121.65(8) . . ? O13 Fe12 O15 144.39(8) . . ? N22 Fe12 O15 91.65(8) . . ? O13 Fe12 N29 91.06(8) . . ? N22 Fe12 N29 98.77(8) . . ? O15 Fe12 N29 96.24(8) . . ? O13 Fe12 O11 88.12(7) . . ? N22 Fe12 O11 84.73(7) . . ? O15 Fe12 O11 82.38(7) . . ? N29 Fe12 O11 176.30(7) . . ? C2 N1 N2 107.78(19) . . ? C2 N1 Fe1 126.82(16) . . ? N2 N1 Fe1 125.25(15) . . ? C3 N2 N1 107.45(19) . . ? C3 N2 Fe2 133.91(16) . . ? N1 N2 Fe2 116.86(14) . . ? C5 N3 C10 114.46(19) . . ? C5 N3 C4 114.6(2) . . ? C10 N3 C4 111.2(2) . . ? C6 N4 C7 106.3(2) . . ? C6 N4 Fe1 125.68(17) . . ? C7 N4 Fe1 127.93(19) . . ? C6 N5 C8 107.2(2) . . ? C6 N5 C9 126.4(2) . . ? C8 N5 C9 126.3(2) . . ? C11 N6 C12 105.6(2) . . ? C11 N6 Fe1 122.89(16) . . ? C12 N6 Fe1 130.73(18) . . ? C11 N7 C13 107.0(2) . . ? C11 N7 C14 126.0(2) . . ? C13 N7 C14 126.9(2) . . ? C21 N8 C16 110.5(2) . . ? C21 N8 C15 112.80(19) . . ? C16 N8 C15 110.28(19) . . ? C17 N9 C18 105.3(2) . . ? C17 N9 Fe2 129.97(17) . . ? C18 N9 Fe2 124.46(18) . . ? C17 N10 C19 106.9(2) . . ? C17 N10 C20 125.8(2) . . ? C19 N10 C20 127.2(2) . . ? C22 N11 C23 104.9(2) . . ? C22 N12 C24 107.3(2) . . ? C22 N12 C25 126.5(2) . . ? C24 N12 C25 126.2(2) . . ? C42 N21 N22 108.12(19) . . ? C42 N21 Fe11 125.79(16) . . ? N22 N21 Fe11 125.85(15) . . ? C43 N22 N21 107.27(19) . . ? C43 N22 Fe12 136.46(17) . . ? N21 N22 Fe12 116.15(14) . . ? C50 N23 C45 114.3(2) . . ? C50 N23 C44 112.5(2) . . ? C45 N23 C44 112.0(2) . . ? C46 N24 C47 106.3(2) . . ? C46 N24 Fe11 121.89(19) . . ? C47 N24 Fe11 131.77(18) . . ? C46 N25 C48 108.1(2) . . ? C46 N25 C49 126.2(2) . . ? C48 N25 C49 125.7(2) . . ? C51 N26 C52 106.7(2) . . ? C51 N26 Fe11 118.53(17) . . ? C52 N26 Fe11 134.75(18) . . ? C51 N27 C53 107.8(2) . . ? C51 N27 C54 126.0(2) . . ? C53 N27 C54 126.2(2) . . ? C61 N28 C56 111.0(2) . . ? C61 N28 C55 111.69(19) . . ? C56 N28 C55 110.79(18) . . ? C57 N29 C58 105.3(2) . . ? C57 N29 Fe12 133.48(17) . . ? C58 N29 Fe12 120.57(17) . . ? C59 N30 C57 107.5(2) . . ? C59 N30 C60 125.5(2) . . ? C57 N30 C60 126.9(2) . . ? C62 N31 C63 105.3(3) . . ? C62 N32 C64 105.7(3) . . ? C62 N32 C65 126.1(3) . . ? C64 N32 C65 128.1(3) . . ? C26 O1 Fe1 137.57(17) . . ? C26 O2 Fe2 130.71(16) . . ? C28 O3 Fe1 95.54(15) . . ? C28 O3 Fe2 135.57(15) . . ? Fe1 O3 Fe2 109.47(7) . . ? C28 O4 Fe1 87.39(15) . . ? C30 O5 Fe2 90.61(18) . . ? C30 O6 Fe2 88.42(17) . . ? C66 O11 Fe11 102.31(16) . . ? C66 O11 Fe12 125.03(14) . . ? Fe11 O11 Fe12 107.51(7) . . ? C68 O13 Fe12 120.12(18) . . ? C70 O15 Fe12 96.26(17) . . ? C2 C1 C3 103.9(2) . . ? N1 C2 C1 111.0(2) . . ? N1 C2 C4 118.5(2) . . ? C1 C2 C4 130.3(2) . . ? N2 C3 C1 109.8(2) . . ? N2 C3 C15 121.4(2) . . ? C1 C3 C15 128.2(2) . . ? N3 C4 C2 109.4(2) . . ? N3 C5 C6 111.1(2) . . ? N4 C6 N5 110.6(2) . . ? N4 C6 C5 125.7(2) . . ? N5 C6 C5 123.7(2) . . ? C8 C7 N4 109.2(3) . . ? C7 C8 N5 106.8(3) . . ? N3 C10 C11 110.9(2) . . ? N6 C11 N7 111.4(2) . . ? N6 C11 C10 124.6(2) . . ? N7 C11 C10 123.9(2) . . ? C13 C12 N6 109.5(2) . . ? C12 C13 N7 106.4(2) . . ? N8 C15 C3 113.0(2) . . ? N8 C16 C17 109.6(2) . . ? N9 C17 N10 111.3(2) . . ? N9 C17 C16 127.1(2) . . ? N10 C17 C16 121.4(2) . . ? C19 C18 N9 110.0(2) . . ? C18 C19 N10 106.4(2) . . ? N8 C21 C22 109.9(2) . . ? N11 C22 N12 111.2(2) . . ? N11 C22 C21 125.0(2) . . ? N12 C22 C21 123.6(3) . . ? C24 C23 N11 110.8(3) . . ? C23 C24 N12 105.8(2) . . ? O1 C26 O2 126.0(2) . . ? O1 C26 C27 116.5(2) . . ? O2 C26 C27 117.5(2) . . ? O4 C28 O3 120.2(2) . . ? O4 C28 C29 121.5(2) . . ? O3 C28 C29 118.3(2) . . ? O6 C30 O5 122.2(3) . . ? O6 C30 C31 119.1(3) . . ? O5 C30 C31 118.7(3) . . ? C42 C41 C43 104.3(2) . . ? N21 C42 C41 110.2(2) . . ? N21 C42 C44 118.3(2) . . ? C41 C42 C44 131.1(2) . . ? N22 C43 C41 110.1(2) . . ? N22 C43 C55 120.8(2) . . ? C41 C43 C55 129.1(2) . . ? N23 C44 C42 109.91(19) . . ? N23 C45 C46 110.1(2) . . ? N24 C46 N25 110.2(2) . . ? N24 C46 C45 124.2(2) . . ? N25 C46 C45 125.4(2) . . ? C48 C47 N24 109.2(3) . . ? C47 C48 N25 106.2(3) . . ? N23 C50 C51 109.3(2) . . ? N26 C51 N27 110.4(2) . . ? N26 C51 C50 123.9(2) . . ? N27 C51 C50 125.7(2) . . ? N26 C52 C53 109.5(2) . . ? C52 C53 N27 105.5(2) . . ? N28 C55 C43 115.1(2) . . ? N28 C56 C57 110.1(2) . . ? N29 C57 N30 110.7(2) . . ? N29 C57 C56 126.2(2) . . ? N30 C57 C56 123.0(2) . . ? C59 C58 N29 110.3(2) . . ? C58 C59 N30 106.3(2) . . ? N28 C61 C62 111.2(2) . . ? N31 C62 N32 111.7(3) . . ? N31 C62 C61 125.4(3) . . ? N32 C62 C61 122.9(3) . . ? C64 C63 N31 110.6(3) . . ? C63 C64 N32 106.8(3) . . ? O12 C66 O11 121.0(3) . . ? O12 C66 C67 122.4(2) . . ? O11 C66 C67 116.5(2) . . ? O14A C68 O13 124.8(3) . . ? O14A C68 O14B 47.1(7) . . ? O13 C68 O14B 114.7(7) . . ? O14A C68 C69 118.9(3) . . ? O13 C68 C69 115.8(2) . . ? O14B C68 C69 113.1(7) . . ? O16 C70 O15 121.3(3) . . ? O16 C70 C71 119.7(3) . . ? O15 C70 C71 119.0(3) . . ? N42 C74 C75 179.1(5) . . ? N43 C76 C77 179.1(4) . . ? N44 C78 C79 177.2(5) . . ? N45 C80 C81 177.8(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.83 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.493 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.055 data_1-bb70m60at213K-one-crystal _database_code_depnum_ccdc_archive 'CCDC 831482' #TrackingRef '- pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H42 Fe2 N12 O6, 2(C2 H3 N)' _chemical_formula_sum 'C35 H48 Fe2 N14 O6' _chemical_formula_weight 872.57 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 'P 21 21 21' 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 16.3489(3) _cell_length_b 18.9892(4) _cell_length_c 26.4822(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8221.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 94982 _cell_measurement_theta_min 1.32 _cell_measurement_theta_max 25.69 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7708 _exptl_absorpt_correction_T_max 0.8482 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94982 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.69 _reflns_number_total 15577 _reflns_number_gt 13923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0514P)^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 0.011(8) _refine_ls_number_reflns 15577 _refine_ls_number_parameters 1032 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.77297(2) 0.41508(2) 0.613558(14) 0.03150(9) Uani 1 1 d . . . Fe2 Fe 0.90884(2) 0.28462(2) 0.561027(15) 0.03075(9) Uani 1 1 d . . . Fe11 Fe 0.24842(3) 0.59946(2) 0.592291(14) 0.03328(9) Uani 1 1 d . . . Fe12 Fe 0.43151(2) 0.689173(19) 0.563077(14) 0.02794(8) Uani 1 1 d . . . N1 N 0.79734(13) 0.40540(11) 0.53557(8) 0.0273(4) Uani 1 1 d . A . N2 N 0.83643(13) 0.34994(11) 0.51300(8) 0.0281(5) Uani 1 1 d . A . N3 N 0.68556(13) 0.50941(11) 0.55935(9) 0.0305(5) Uani 1 1 d . . . N4 N 0.76378(15) 0.51113(12) 0.65361(8) 0.0366(5) Uani 1 1 d . A . N5 N 0.73251(18) 0.62051(14) 0.67173(11) 0.0491(7) Uani 1 1 d . A . N6 N 0.64209(14) 0.39453(12) 0.61910(9) 0.0357(5) Uani 1 1 d . A . N7 N 0.51356(15) 0.39294(13) 0.59402(10) 0.0392(6) Uani 1 1 d . A . N8 N 0.95740(14) 0.34605(12) 0.40871(8) 0.0314(5) Uani 1 1 d . . . N9 N 1.01500(14) 0.26515(12) 0.51176(9) 0.0351(5) Uani 1 1 d . A . N10 N 1.11664(14) 0.27560(13) 0.45717(10) 0.0388(6) Uani 1 1 d . A . N11 N 1.0720(2) 0.47345(16) 0.35686(12) 0.0585(8) Uani 1 1 d . . . N12 N 1.04688(18) 0.38383(14) 0.30609(9) 0.0440(6) Uani 1 1 d . . . N21 N 0.28457(13) 0.61904(12) 0.51878(8) 0.0297(5) Uani 1 1 d . . . N22 N 0.35394(13) 0.65475(11) 0.50431(8) 0.0270(5) Uani 1 1 d . . . N23 N 0.15149(15) 0.53598(12) 0.53214(9) 0.0355(5) Uani 1 1 d . . . N24 N 0.12941(15) 0.62608(13) 0.61320(10) 0.0388(6) Uani 1 1 d . . . N25 N -0.00504(15) 0.62278(14) 0.61208(11) 0.0440(6) Uani 1 1 d . . . N26 N 0.25152(15) 0.49330(12) 0.61229(8) 0.0352(5) Uani 1 1 d . . . N27 N 0.22906(15) 0.38072(12) 0.59937(9) 0.0387(6) Uani 1 1 d . . . N28 N 0.48297(14) 0.64789(12) 0.40530(8) 0.0301(5) Uani 1 1 d . . . N29 N 0.54807(14) 0.68815(13) 0.52183(9) 0.0342(5) Uani 1 1 d . . . N30 N 0.64755(14) 0.68319(12) 0.46552(9) 0.0338(5) Uani 1 1 d . . . N31 N 0.3466(2) 0.6526(2) 0.31001(11) 0.0733(11) Uani 1 1 d . . . N32 N 0.4762(2) 0.66296(16) 0.28681(10) 0.0593(8) Uani 1 1 d . . . O1A O 0.90535(16) 0.43588(13) 0.62577(9) 0.0456(8) Uiso 0.861(6) 1 d P A 1 O2A O 0.98422(16) 0.34492(15) 0.60403(10) 0.0413(7) Uiso 0.861(6) 1 d P A 1 C26A C 0.9696(2) 0.4013(2) 0.62799(11) 0.0288(7) Uiso 0.861(6) 1 d P A 1 C27A C 1.0331(3) 0.4297(3) 0.6628(2) 0.0420(17) Uiso 0.861(6) 1 d P A 1 H27A H 1.0803 0.3987 0.6627 0.080 Uiso 0.861(6) 1 calc PR A 1 H27B H 1.0110 0.4326 0.6967 0.080 Uiso 0.861(6) 1 calc PR A 1 H27C H 1.0495 0.4762 0.6516 0.080 Uiso 0.861(6) 1 calc PR A 1 O1B O 0.9694(11) 0.3834(11) 0.5880(7) 0.055(5) Uiso 0.139(6) 1 d P A 2 O2B O 0.9987(13) 0.3111(12) 0.6338(8) 0.069(6) Uiso 0.139(6) 1 d P A 2 C26B C 0.9950(15) 0.3703(14) 0.6287(9) 0.038(5) Uiso 0.139(6) 1 d P A 2 C27B C 1.0475(14) 0.4220(11) 0.6573(8) 0.012(6) Uiso 0.139(6) 1 d P A 2 H27D H 1.0681 0.3999 0.6878 0.080 Uiso 0.139(6) 1 calc PR A 2 H27E H 1.0151 0.4629 0.6662 0.080 Uiso 0.139(6) 1 calc PR A 2 H27F H 1.0931 0.4364 0.6363 0.080 Uiso 0.139(6) 1 calc PR A 2 O3 O 0.81071(11) 0.30527(10) 0.61782(7) 0.0345(4) Uani 1 1 d . A . O4 O 0.78432(17) 0.35098(13) 0.69165(8) 0.0547(6) Uani 1 1 d . A . O5A O 0.8512(2) 0.18385(19) 0.53743(12) 0.0386(11) Uiso 0.717(10) 1 d P A 3 O6A O 0.9400(3) 0.18016(19) 0.59978(15) 0.0486(11) Uiso 0.717(10) 1 d P A 3 C30A C 0.8886(4) 0.1511(4) 0.5717(3) 0.0465(15) Uiso 0.717(10) 1 d P A 3 C31A C 0.8768(5) 0.0712(3) 0.5748(3) 0.0634(19) Uiso 0.717(10) 1 d P A 3 H31A H 0.8352 0.0568 0.5508 0.080 Uiso 0.717(10) 1 calc PR A 3 H31B H 0.8598 0.0585 0.6087 0.080 Uiso 0.717(10) 1 calc PR A 3 H31C H 0.9280 0.0478 0.5669 0.080 Uiso 0.717(10) 1 calc PR A 3 O5B O 0.8249(7) 0.1602(6) 0.5196(4) 0.066(4) Uiso 0.283(10) 1 d P A 4 O6B O 0.9110(9) 0.1805(7) 0.5842(5) 0.065(3) Uiso 0.283(10) 1 d P A 4 C30B C 0.8679(8) 0.1427(6) 0.5576(5) 0.034(3) Uiso 0.283(10) 1 d P A 4 C31B C 0.8525(11) 0.0760(8) 0.5852(6) 0.053(4) Uiso 0.283(10) 1 d P A 4 H31D H 0.8215 0.0442 0.5638 0.080 Uiso 0.283(10) 1 calc PR A 4 H31E H 0.8216 0.0858 0.6156 0.080 Uiso 0.283(10) 1 calc PR A 4 H31F H 0.9043 0.0543 0.5940 0.080 Uiso 0.283(10) 1 calc PR A 4 O11 O 0.31430(11) 0.68929(11) 0.61155(7) 0.0334(4) Uani 1 1 d . . . O12 O 0.28595(16) 0.63858(13) 0.68379(9) 0.0538(6) Uani 1 1 d . . . O13 O 0.44340(15) 0.79157(11) 0.57902(9) 0.0482(5) Uani 1 1 d . B . O14A O 0.3756(3) 0.8259(2) 0.51139(14) 0.0653(10) Uiso 0.736(5) 1 d P B 5 O14B O 0.4350(7) 0.8321(6) 0.5026(4) 0.0653(10) Uiso 0.264(5) 1 d P B 6 O15 O 0.44149(15) 0.58422(12) 0.59400(8) 0.0471(5) Uani 1 1 d . . . O16 O 0.49709(14) 0.66309(13) 0.64278(9) 0.0526(6) Uani 1 1 d . . . C1 C 0.79199(16) 0.42303(14) 0.45224(10) 0.0312(6) Uani 1 1 d . A . H1 H 0.7804 0.4428 0.4205 0.080 Uiso 1 1 calc R . . C2 C 0.77217(15) 0.44942(13) 0.49901(9) 0.0263(5) Uani 1 1 d . . . C3 C 0.83334(15) 0.36019(13) 0.46262(10) 0.0267(5) Uani 1 1 d . . . C4 C 0.73555(17) 0.51853(14) 0.51401(11) 0.0341(6) Uani 1 1 d . A . H4A H 0.7792 0.5527 0.5207 0.080 Uiso 1 1 calc R . . H4B H 0.7016 0.5367 0.4864 0.080 Uiso 1 1 calc R . . C5 C 0.67653(18) 0.57288(15) 0.59019(12) 0.0390(7) Uani 1 1 d . A . H5A H 0.6185 0.5801 0.5980 0.080 Uiso 1 1 calc R . . H5B H 0.6958 0.6138 0.5710 0.080 Uiso 1 1 calc R . . C6 C 0.72335(17) 0.56742(14) 0.63777(11) 0.0341(6) Uani 1 1 d . . . C7 C 0.8005(2) 0.5296(2) 0.69812(12) 0.0538(9) Uani 1 1 d . . . H7 H 0.8337 0.5000 0.7178 0.080 Uiso 1 1 calc R A . C8 C 0.7816(3) 0.5967(2) 0.70932(13) 0.0634(10) Uani 1 1 d . A . H8 H 0.7991 0.6223 0.7377 0.080 Uiso 1 1 calc R . . C9 C 0.6978(2) 0.6917(2) 0.66698(16) 0.0628(10) Uani 1 1 d . . . H9A H 0.7237 0.7160 0.6390 0.080 Uiso 1 1 calc R A . H9B H 0.7073 0.7177 0.6980 0.080 Uiso 1 1 calc R . . H9C H 0.6394 0.6883 0.6608 0.080 Uiso 1 1 calc R . . C10 C 0.60839(17) 0.47433(15) 0.54772(10) 0.0321(6) Uani 1 1 d . A . H10A H 0.6125 0.4510 0.5148 0.080 Uiso 1 1 calc R . . H10B H 0.5645 0.5093 0.5458 0.080 Uiso 1 1 calc R . . C11 C 0.58836(17) 0.42127(13) 0.58733(10) 0.0318(6) Uani 1 1 d . . . C12 C 0.5982(2) 0.34711(17) 0.64797(13) 0.0462(8) Uani 1 1 d . . . H12 H 0.6199 0.3201 0.6745 0.080 Uiso 1 1 calc R A . C13 C 0.5201(2) 0.34541(19) 0.63251(14) 0.0522(9) Uani 1 1 d . A . H13 H 0.4781 0.3170 0.6456 0.080 Uiso 1 1 calc R . . C14 C 0.44062(18) 0.40785(19) 0.56349(14) 0.0519(8) Uani 1 1 d . . . H14A H 0.4238 0.4563 0.5688 0.080 Uiso 1 1 calc R A . H14B H 0.3967 0.3765 0.5734 0.080 Uiso 1 1 calc R . . H14C H 0.4532 0.4007 0.5281 0.080 Uiso 1 1 calc R . . C15 C 0.87977(16) 0.31383(14) 0.42676(10) 0.0307(6) Uani 1 1 d . A . H15A H 0.8923 0.2692 0.4436 0.080 Uiso 1 1 calc R . . H15B H 0.8450 0.3034 0.3976 0.080 Uiso 1 1 calc R . . C16 C 1.00916(17) 0.36711(14) 0.45172(10) 0.0322(6) Uani 1 1 d . A . H16A H 0.9760 0.3921 0.4768 0.080 Uiso 1 1 calc R . . H16B H 1.0524 0.3990 0.4401 0.080 Uiso 1 1 calc R . . C17 C 1.04631(16) 0.30347(15) 0.47506(11) 0.0328(6) Uani 1 1 d . . . C18 C 1.06893(18) 0.20924(15) 0.51752(12) 0.0415(7) Uani 1 1 d . . . H18 H 1.0628 0.1725 0.5410 0.080 Uiso 1 1 calc R A . C19 C 1.13097(19) 0.21535(17) 0.48469(12) 0.0436(8) Uani 1 1 d . A . H19 H 1.1756 0.1845 0.4812 0.080 Uiso 1 1 calc R . . C20 C 1.1655(2) 0.30336(19) 0.41587(13) 0.0508(8) Uani 1 1 d . . . H20A H 1.1313 0.3092 0.3862 0.080 Uiso 1 1 calc R A . H20B H 1.2096 0.2708 0.4083 0.080 Uiso 1 1 calc R . . H20C H 1.1883 0.3485 0.4255 0.080 Uiso 1 1 calc R . . C21 C 0.94345(19) 0.40617(16) 0.37463(11) 0.0391(7) Uani 1 1 d . . . H21A H 0.9268 0.4475 0.3943 0.080 Uiso 1 1 calc R . . H21B H 0.8994 0.3949 0.3509 0.080 Uiso 1 1 calc R . . C22 C 1.0205(2) 0.42238(17) 0.34606(12) 0.0428(7) Uani 1 1 d . . . C23 C 1.1347(2) 0.4656(2) 0.32286(16) 0.0647(11) Uani 1 1 d . . . H23 H 1.1814 0.4944 0.3218 0.080 Uiso 1 1 calc R . . C24 C 1.1210(2) 0.4119(2) 0.29152(13) 0.0567(9) Uani 1 1 d . . . H24 H 1.1548 0.3964 0.2651 0.080 Uiso 1 1 calc R . . C25 C 1.0053(3) 0.3226(2) 0.28387(14) 0.0610(10) Uani 1 1 d . . . H25A H 1.0237 0.2800 0.3006 0.080 Uiso 1 1 calc R . . H25B H 1.0180 0.3199 0.2481 0.080 Uiso 1 1 calc R . . H25C H 0.9466 0.3275 0.2882 0.080 Uiso 1 1 calc R . . C28 C 0.80484(18) 0.29978(16) 0.66596(10) 0.0354(6) Uani 1 1 d . . . C29 C 0.8218(2) 0.22937(18) 0.68972(12) 0.0514(9) Uani 1 1 d . A . H29A H 0.8153 0.2329 0.7260 0.080 Uiso 1 1 calc R . . H29B H 0.8773 0.2150 0.6819 0.080 Uiso 1 1 calc R . . H29C H 0.7837 0.1948 0.6766 0.080 Uiso 1 1 calc R . . C41 C 0.28014(17) 0.63017(14) 0.43480(10) 0.0315(6) Uani 1 1 d . . . H41 H 0.2633 0.6269 0.4009 0.080 Uiso 1 1 calc R . . C42 C 0.24047(17) 0.60483(14) 0.47712(9) 0.0304(6) Uani 1 1 d . . . C43 C 0.35107(16) 0.66183(13) 0.45374(9) 0.0275(5) Uani 1 1 d . . . C44 C 0.15694(18) 0.57357(16) 0.48345(11) 0.0379(7) Uani 1 1 d . . . H44A H 0.1157 0.6110 0.4823 0.080 Uiso 1 1 calc R . . H44B H 0.1459 0.5408 0.4557 0.080 Uiso 1 1 calc R . . C45 C 0.06904(19) 0.53947(17) 0.55352(11) 0.0424(7) Uani 1 1 d . . . H45A H 0.0554 0.4944 0.5695 0.080 Uiso 1 1 calc R . . H45B H 0.0293 0.5482 0.5266 0.080 Uiso 1 1 calc R . . C46 C 0.06466(18) 0.59707(16) 0.59164(11) 0.0378(6) Uani 1 1 d . . . C47 C 0.0989(2) 0.67200(19) 0.64918(13) 0.0507(8) Uani 1 1 d . . . H47 H 0.1308 0.7000 0.6708 0.080 Uiso 1 1 calc R . . C48 C 0.0169(2) 0.6704(2) 0.64851(14) 0.0526(9) Uani 1 1 d . . . H48 H -0.0186 0.6969 0.6690 0.080 Uiso 1 1 calc R . . C49 C -0.0883(2) 0.6043(2) 0.59804(16) 0.0593(10) Uani 1 1 d . . . H49A H -0.1001 0.6225 0.5646 0.080 Uiso 1 1 calc R . . H49B H -0.1262 0.6246 0.6222 0.080 Uiso 1 1 calc R . . H49C H -0.0942 0.5535 0.5980 0.080 Uiso 1 1 calc R . . C50 C 0.1855(2) 0.46503(16) 0.52984(12) 0.0440(7) Uani 1 1 d . . . H50A H 0.2283 0.4629 0.5040 0.080 Uiso 1 1 calc R . . H50B H 0.1425 0.4313 0.5208 0.080 Uiso 1 1 calc R . . C51 C 0.22086(18) 0.44641(15) 0.58056(10) 0.0342(6) Uani 1 1 d . . . C52 C 0.28084(19) 0.45647(17) 0.65260(11) 0.0393(7) Uani 1 1 d . . . H52 H 0.3063 0.4763 0.6811 0.080 Uiso 1 1 calc R . . C53 C 0.2674(2) 0.38643(17) 0.64519(11) 0.0437(7) Uani 1 1 d . . . H53 H 0.2816 0.3495 0.6671 0.080 Uiso 1 1 calc R . . C54 C 0.2023(2) 0.31543(17) 0.57491(14) 0.0529(9) Uani 1 1 d . . . H54A H 0.1444 0.3185 0.5672 0.080 Uiso 1 1 calc R . . H54B H 0.2119 0.2760 0.5974 0.080 Uiso 1 1 calc R . . H54C H 0.2329 0.3086 0.5439 0.080 Uiso 1 1 calc R . . C55 C 0.41957(17) 0.69672(13) 0.42516(9) 0.0295(6) Uani 1 1 d . . . H55A H 0.3961 0.7229 0.3967 0.080 Uiso 1 1 calc R . . H55B H 0.4461 0.7309 0.4475 0.080 Uiso 1 1 calc R . . C56 C 0.52359(16) 0.60967(14) 0.44704(10) 0.0308(6) Uani 1 1 d . . . H56A H 0.5598 0.5734 0.4331 0.080 Uiso 1 1 calc R . . H56B H 0.4822 0.5863 0.4679 0.080 Uiso 1 1 calc R . . C57 C 0.57207(17) 0.65913(14) 0.47877(10) 0.0316(6) Uani 1 1 d . . . C58 C 0.61082(18) 0.73235(16) 0.53602(12) 0.0388(7) Uani 1 1 d . . . H58 H 0.6110 0.7607 0.5651 0.080 Uiso 1 1 calc R . . C59 C 0.67211(18) 0.72888(15) 0.50175(12) 0.0379(7) Uani 1 1 d . . . H59 H 0.7220 0.7534 0.5029 0.080 Uiso 1 1 calc R . . C60 C 0.6919(2) 0.66698(18) 0.41934(11) 0.0441(7) Uani 1 1 d . . . H60A H 0.7408 0.6958 0.4175 0.080 Uiso 1 1 calc R . . H60B H 0.6573 0.6767 0.3904 0.080 Uiso 1 1 calc R . . H60C H 0.7071 0.6176 0.4193 0.080 Uiso 1 1 calc R . . C61 C 0.44932(19) 0.59911(16) 0.36750(10) 0.0374(6) Uani 1 1 d . . . H61A H 0.4025 0.5740 0.3820 0.080 Uiso 1 1 calc R . . H61B H 0.4910 0.5642 0.3584 0.080 Uiso 1 1 calc R . . C62 C 0.4229(2) 0.63738(17) 0.32160(11) 0.0460(8) Uani 1 1 d . . . C63 C 0.3516(4) 0.6916(3) 0.26643(15) 0.097(2) Uani 1 1 d . . . H63 H 0.3063 0.7109 0.2495 0.080 Uiso 1 1 calc R . . C64 C 0.4283(4) 0.6983(2) 0.25147(14) 0.0830(16) Uani 1 1 d . . . H64 H 0.4469 0.7223 0.2226 0.080 Uiso 1 1 calc R . . C65 C 0.5636(3) 0.6510(3) 0.28562(16) 0.0836(15) Uani 1 1 d . . . H65A H 0.5873 0.6646 0.3178 0.080 Uiso 1 1 calc R . . H65B H 0.5879 0.6789 0.2588 0.080 Uiso 1 1 calc R . . H65C H 0.5743 0.6015 0.2795 0.080 Uiso 1 1 calc R . . C66 C 0.31210(16) 0.68955(16) 0.65996(10) 0.0328(6) Uani 1 1 d . . . C67 C 0.3398(2) 0.75569(18) 0.68589(12) 0.0469(8) Uani 1 1 d . . . H67A H 0.3444 0.7472 0.7219 0.080 Uiso 1 1 calc R . . H67B H 0.3002 0.7928 0.6799 0.080 Uiso 1 1 calc R . . H67C H 0.3926 0.7698 0.6726 0.080 Uiso 1 1 calc R . . C68 C 0.4175(2) 0.83842(17) 0.55023(12) 0.0480(8) Uani 1 1 d . . . C69 C 0.4226(2) 0.91329(15) 0.56917(13) 0.0475(7) Uani 1 1 d . B . H69A H 0.4094 0.9455 0.5419 0.080 Uiso 1 1 calc R . . H69B H 0.4776 0.9227 0.5811 0.080 Uiso 1 1 calc R . . H69C H 0.3841 0.9198 0.5966 0.080 Uiso 1 1 calc R . . C70 C 0.47566(18) 0.60078(17) 0.63433(11) 0.0389(7) Uani 1 1 d . . . C71 C 0.4928(2) 0.54458(18) 0.67324(12) 0.0499(8) Uani 1 1 d . . . H71A H 0.5485 0.5493 0.6853 0.080 Uiso 1 1 calc R . . H71B H 0.4856 0.4985 0.6581 0.080 Uiso 1 1 calc R . . H71C H 0.4552 0.5498 0.7013 0.080 Uiso 1 1 calc R . . N42 N 0.7315(5) 0.3151(4) 0.3257(2) 0.130(2) Uani 1 1 d . . . C74 C 0.6776(5) 0.3464(5) 0.3410(3) 0.116(3) Uani 1 1 d . . . C75 C 0.6137(4) 0.3901(6) 0.3598(3) 0.168(5) Uani 1 1 d . . . H75A H 0.6316 0.4129 0.3906 0.252 Uiso 1 1 calc R . . H75B H 0.5658 0.3616 0.3667 0.252 Uiso 1 1 calc R . . H75C H 0.6003 0.4256 0.3348 0.252 Uiso 1 1 calc R . . N43 N 0.7537(4) 0.4670(3) 0.83587(17) 0.1099(17) Uani 1 1 d . . . C76 C 0.7041(4) 0.4593(3) 0.80560(18) 0.0799(14) Uani 1 1 d . . . C77 C 0.6449(4) 0.4469(4) 0.7677(2) 0.1063(19) Uani 1 1 d . . . H77A H 0.6658 0.4125 0.7439 0.159 Uiso 1 1 calc R . . H77B H 0.6331 0.4905 0.7501 0.159 Uiso 1 1 calc R . . H77C H 0.5952 0.4290 0.7831 0.159 Uiso 1 1 calc R . . N44 N 0.0039(4) 0.5404(3) 0.7748(2) 0.1230(19) Uani 1 1 d . . . C78 C 0.0706(3) 0.5400(3) 0.76556(16) 0.0736(12) Uani 1 1 d . . . C79 C 0.1547(3) 0.5368(3) 0.7539(2) 0.0852(14) Uani 1 1 d . . . H79A H 0.1799 0.4987 0.7727 0.128 Uiso 1 1 calc R . . H79B H 0.1806 0.5810 0.7629 0.128 Uiso 1 1 calc R . . H79C H 0.1615 0.5284 0.7180 0.128 Uiso 1 1 calc R . . N45 N 0.6024(3) 0.8285(3) 0.76038(17) 0.1113(17) Uani 1 1 d . . . C80 C 0.5916(3) 0.8379(2) 0.71871(17) 0.0677(11) Uani 1 1 d . . . C81 C 0.5805(3) 0.8478(2) 0.66496(16) 0.0801(13) Uani 1 1 d . . . H81A H 0.6319 0.8398 0.6477 0.120 Uiso 1 1 calc R . . H81B H 0.5621 0.8956 0.6586 0.120 Uiso 1 1 calc R . . H81C H 0.5398 0.8148 0.6526 0.120 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 0.0376(2) 0.02553(19) 0.03141(19) -0.00240(15) 0.00282(16) 0.00157(16) Fe2 0.0272(2) 0.02599(18) 0.0390(2) 0.00392(16) -0.00120(17) 0.00378(15) Fe11 0.0392(2) 0.0315(2) 0.02913(18) 0.00035(15) 0.00221(17) -0.00967(17) Fe12 0.02622(19) 0.02717(18) 0.03044(18) -0.00230(15) -0.00163(16) -0.00266(15) N1 0.0255(11) 0.0245(11) 0.0319(11) 0.0016(9) 0.0053(9) 0.0047(9) N2 0.0266(12) 0.0255(11) 0.0323(11) -0.0002(9) 0.0027(9) 0.0043(9) N3 0.0267(11) 0.0274(11) 0.0374(12) -0.0070(10) 0.0024(10) 0.0014(9) N4 0.0401(15) 0.0344(12) 0.0352(12) -0.0057(10) -0.0004(11) -0.0011(11) N5 0.0490(17) 0.0404(14) 0.0578(16) -0.0227(12) -0.0018(13) 0.0064(12) N6 0.0365(13) 0.0315(12) 0.0391(13) -0.0024(10) 0.0044(11) -0.0031(10) N7 0.0302(13) 0.0370(14) 0.0505(14) -0.0106(12) 0.0047(11) -0.0054(10) N8 0.0302(12) 0.0300(12) 0.0342(11) -0.0042(10) 0.0047(10) 0.0000(9) N9 0.0308(13) 0.0277(12) 0.0468(14) -0.0059(10) -0.0011(11) 0.0074(10) N10 0.0279(12) 0.0412(14) 0.0474(14) -0.0149(11) -0.0009(10) 0.0059(10) N11 0.061(2) 0.0509(17) 0.0636(18) -0.0071(14) 0.0260(16) -0.0139(15) N12 0.0542(17) 0.0405(14) 0.0374(13) 0.0031(11) 0.0134(12) 0.0068(12) N21 0.0234(11) 0.0370(12) 0.0287(11) -0.0002(9) -0.0016(9) -0.0065(9) N22 0.0260(12) 0.0277(11) 0.0274(11) 0.0003(9) 0.0007(9) -0.0030(9) N23 0.0337(13) 0.0354(13) 0.0374(13) 0.0068(10) -0.0029(10) -0.0097(10) N24 0.0336(13) 0.0399(14) 0.0430(13) -0.0013(11) -0.0013(11) -0.0039(11) N25 0.0343(14) 0.0427(15) 0.0548(16) 0.0161(13) 0.0002(12) 0.0022(11) N26 0.0333(13) 0.0377(12) 0.0347(11) 0.0008(10) -0.0019(10) -0.0037(10) N27 0.0353(14) 0.0322(12) 0.0486(14) 0.0023(10) -0.0058(11) -0.0024(10) N28 0.0323(12) 0.0282(11) 0.0297(11) -0.0004(9) 0.0031(10) -0.0018(9) N29 0.0291(12) 0.0365(12) 0.0370(12) -0.0013(10) 0.0022(10) -0.0023(10) N30 0.0280(12) 0.0340(12) 0.0395(12) 0.0033(11) 0.0045(10) -0.0026(10) N31 0.085(3) 0.098(3) 0.0369(16) -0.0170(17) -0.0106(16) 0.043(2) N32 0.094(3) 0.0468(17) 0.0372(15) -0.0022(13) 0.0074(16) -0.0071(17) O3 0.0325(10) 0.0375(11) 0.0336(10) 0.0081(8) 0.0004(8) 0.0000(8) O4 0.0755(18) 0.0481(14) 0.0404(12) -0.0062(10) -0.0080(11) 0.0100(12) O11 0.0289(10) 0.0409(10) 0.0304(9) -0.0063(8) -0.0034(8) -0.0020(8) O12 0.0571(15) 0.0525(14) 0.0518(13) 0.0157(11) -0.0086(11) -0.0118(12) O13 0.0584(14) 0.0288(10) 0.0575(13) 0.0014(10) 0.0074(11) 0.0016(10) O15 0.0631(15) 0.0403(11) 0.0378(11) -0.0009(9) 0.0002(11) 0.0121(11) O16 0.0421(13) 0.0442(14) 0.0715(16) 0.0021(11) 0.0022(11) 0.0045(10) C1 0.0271(14) 0.0331(14) 0.0335(14) 0.0054(11) 0.0001(11) 0.0017(11) C2 0.0196(13) 0.0255(12) 0.0339(13) 0.0050(10) 0.0044(10) 0.0002(10) C3 0.0204(13) 0.0279(13) 0.0318(13) -0.0012(11) -0.0009(10) -0.0015(10) C4 0.0300(15) 0.0282(13) 0.0441(15) 0.0064(11) 0.0068(12) 0.0028(11) C5 0.0346(16) 0.0322(15) 0.0502(17) -0.0116(13) -0.0017(13) 0.0076(12) C6 0.0275(14) 0.0330(15) 0.0417(15) -0.0109(12) 0.0058(12) -0.0022(11) C7 0.069(2) 0.055(2) 0.0373(17) -0.0094(15) -0.0165(16) 0.0036(17) C8 0.080(3) 0.060(2) 0.0504(19) -0.0247(18) -0.0203(19) 0.011(2) C9 0.061(2) 0.046(2) 0.081(3) -0.0289(19) -0.0125(19) 0.0099(17) C10 0.0273(15) 0.0361(15) 0.0329(14) -0.0026(11) -0.0008(11) -0.0028(11) C11 0.0302(14) 0.0261(13) 0.0391(14) -0.0103(11) 0.0068(12) -0.0016(11) C12 0.050(2) 0.0373(17) 0.0509(18) 0.0046(14) 0.0058(15) -0.0065(15) C13 0.052(2) 0.0430(19) 0.062(2) 0.0036(16) 0.0126(17) -0.0173(16) C14 0.0303(16) 0.0548(19) 0.071(2) -0.0109(18) 0.0014(16) -0.0079(14) C15 0.0325(14) 0.0275(13) 0.0321(14) -0.0054(11) 0.0019(11) -0.0012(11) C16 0.0292(15) 0.0303(14) 0.0372(15) -0.0067(11) 0.0031(11) -0.0001(11) C17 0.0250(14) 0.0329(15) 0.0406(15) -0.0121(12) 0.0000(11) -0.0016(11) C18 0.0362(16) 0.0319(15) 0.0565(18) -0.0066(13) -0.0133(15) 0.0088(13) C19 0.0332(16) 0.0380(16) 0.060(2) -0.0184(15) -0.0082(14) 0.0115(13) C20 0.0335(17) 0.062(2) 0.0564(19) -0.0122(17) 0.0148(14) 0.0015(15) C21 0.0422(17) 0.0360(15) 0.0390(15) 0.0002(13) 0.0105(12) 0.0052(13) C22 0.0449(18) 0.0406(17) 0.0430(16) 0.0047(13) 0.0123(14) 0.0053(14) C23 0.053(2) 0.065(3) 0.076(3) 0.003(2) 0.027(2) -0.0105(19) C24 0.059(2) 0.062(2) 0.0487(19) 0.0080(18) 0.0258(17) 0.0147(18) C25 0.080(3) 0.054(2) 0.049(2) -0.0081(17) 0.0127(19) 0.0001(19) C28 0.0332(15) 0.0396(17) 0.0335(15) 0.0022(12) -0.0068(11) -0.0054(12) C29 0.070(2) 0.047(2) 0.0365(16) 0.0139(14) -0.0059(16) 0.0019(17) C41 0.0325(14) 0.0334(14) 0.0286(13) -0.0003(11) -0.0056(12) -0.0027(11) C42 0.0321(14) 0.0306(13) 0.0285(12) -0.0013(10) -0.0035(11) -0.0011(11) C43 0.0289(14) 0.0253(13) 0.0283(13) 0.0006(10) 0.0001(10) 0.0029(11) C44 0.0364(16) 0.0431(17) 0.0341(15) 0.0066(12) -0.0071(12) -0.0087(13) C45 0.0381(16) 0.0479(17) 0.0412(16) 0.0065(13) -0.0039(14) -0.0139(14) C46 0.0349(16) 0.0395(16) 0.0389(14) 0.0122(13) -0.0015(13) -0.0047(13) C47 0.049(2) 0.0488(19) 0.054(2) -0.0047(15) -0.0001(16) 0.0040(16) C48 0.045(2) 0.055(2) 0.058(2) -0.0015(17) 0.0031(16) 0.0099(16) C49 0.0279(17) 0.060(2) 0.090(3) 0.017(2) -0.0046(17) -0.0041(15) C50 0.0483(19) 0.0386(17) 0.0450(17) -0.0029(14) -0.0137(14) -0.0105(14) C51 0.0314(15) 0.0330(14) 0.0384(15) 0.0008(12) -0.0034(12) -0.0048(12) C52 0.0352(16) 0.0476(18) 0.0351(15) 0.0018(13) -0.0026(12) -0.0013(14) C53 0.0415(18) 0.0456(17) 0.0441(17) 0.0109(13) -0.0053(14) 0.0009(14) C54 0.054(2) 0.0316(15) 0.074(2) 0.0003(16) -0.0137(17) -0.0032(15) C55 0.0331(15) 0.0263(13) 0.0292(13) 0.0014(10) 0.0029(11) 0.0010(11) C56 0.0300(14) 0.0267(13) 0.0357(14) -0.0006(11) 0.0017(11) -0.0004(11) C57 0.0283(14) 0.0301(13) 0.0365(14) 0.0060(11) 0.0014(12) -0.0020(11) C58 0.0352(16) 0.0389(16) 0.0421(16) -0.0042(13) -0.0015(13) -0.0081(12) C59 0.0318(16) 0.0289(15) 0.0529(17) 0.0014(13) 0.0005(13) -0.0084(12) C60 0.0364(17) 0.0539(19) 0.0421(17) 0.0032(14) 0.0090(13) -0.0026(14) C61 0.0436(17) 0.0348(15) 0.0339(14) -0.0062(12) 0.0015(12) 0.0020(13) C62 0.064(2) 0.0432(17) 0.0307(15) -0.0122(13) -0.0022(15) 0.0117(16) C63 0.149(5) 0.103(4) 0.039(2) -0.021(2) -0.022(3) 0.075(4) C64 0.169(6) 0.051(2) 0.0293(18) 0.0002(16) -0.010(3) 0.017(3) C65 0.097(4) 0.103(4) 0.051(2) -0.006(2) 0.015(2) -0.045(3) C66 0.0247(14) 0.0389(15) 0.0348(14) -0.0020(13) -0.0025(11) 0.0046(12) C67 0.053(2) 0.0482(19) 0.0398(17) -0.0116(14) -0.0081(15) 0.0021(16) C68 0.063(2) 0.0358(16) 0.0454(18) 0.0004(14) 0.0043(16) 0.0025(15) C69 0.0524(19) 0.0275(14) 0.063(2) -0.0059(14) -0.0021(16) 0.0016(14) C70 0.0351(16) 0.0400(18) 0.0415(16) 0.0006(13) 0.0106(13) 0.0131(13) C71 0.063(2) 0.0457(19) 0.0412(17) 0.0054(14) -0.0006(15) 0.0158(16) N42 0.176(7) 0.134(5) 0.081(3) 0.025(3) -0.054(4) -0.032(5) C74 0.095(5) 0.171(9) 0.083(4) 0.073(5) -0.040(4) -0.048(5) C75 0.067(4) 0.298(12) 0.140(6) 0.123(7) -0.008(4) -0.018(6) N43 0.162(5) 0.100(3) 0.068(3) 0.008(2) 0.008(3) -0.008(4) C76 0.120(4) 0.064(3) 0.055(3) 0.010(2) 0.021(3) 0.011(3) C77 0.118(5) 0.124(5) 0.077(3) 0.012(3) 0.003(3) 0.010(4) N44 0.111(4) 0.147(5) 0.111(4) -0.026(3) 0.032(3) 0.000(4) C78 0.081(3) 0.083(3) 0.057(2) -0.013(2) 0.014(2) -0.009(3) C79 0.071(3) 0.090(3) 0.095(3) -0.001(3) -0.008(3) -0.018(3) N45 0.126(4) 0.143(5) 0.065(3) -0.011(3) -0.004(3) -0.008(3) C80 0.066(3) 0.075(3) 0.062(3) -0.011(2) 0.006(2) 0.008(2) C81 0.108(4) 0.063(3) 0.068(3) -0.001(2) -0.011(3) 0.011(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 N1 2.111(2) . ? Fe1 N4 2.115(2) . ? Fe1 O3 2.177(2) . ? Fe1 N6 2.180(2) . ? Fe1 O1A 2.224(3) . ? Fe2 O2A 2.031(3) . ? Fe2 O6B 2.071(13) . ? Fe2 N2 2.135(2) . ? Fe2 N9 2.203(2) . ? Fe2 O5A 2.222(4) . ? Fe2 O3 2.2337(19) . ? Fe2 O1B 2.238(19) . ? Fe2 O6A 2.291(4) . ? Fe11 N21 2.068(2) . ? Fe11 O11 2.081(2) . ? Fe11 N26 2.085(2) . ? Fe11 N24 2.085(3) . ? Fe12 O13 1.999(2) . ? Fe12 N22 2.111(2) . ? Fe12 O15 2.161(2) . ? Fe12 N29 2.197(2) . ? Fe12 O11 2.3065(19) . ? N1 C2 1.344(3) . ? N1 N2 1.369(3) . ? N2 C3 1.349(3) . ? N3 C10 1.460(3) . ? N3 C4 1.463(4) . ? N3 C5 1.463(3) . ? N4 C6 1.325(4) . ? N4 C7 1.368(4) . ? N5 C8 1.356(5) . ? N5 C6 1.359(4) . ? N5 C9 1.472(5) . ? N6 C11 1.318(4) . ? N6 C12 1.382(4) . ? N7 C11 1.348(4) . ? N7 C13 1.366(4) . ? N7 C14 1.468(4) . ? N8 C21 1.473(4) . ? N8 C16 1.474(3) . ? N8 C15 1.488(3) . ? N9 C17 1.318(4) . ? N9 C18 1.388(4) . ? N10 C17 1.351(4) . ? N10 C19 1.377(4) . ? N10 C20 1.454(4) . ? N11 C22 1.316(4) . ? N11 C23 1.372(5) . ? N12 C22 1.357(4) . ? N12 C24 1.379(5) . ? N12 C25 1.470(5) . ? N21 C42 1.345(3) . ? N21 N22 1.376(3) . ? N22 C43 1.347(3) . ? N23 C50 1.459(4) . ? N23 C45 1.464(4) . ? N23 C44 1.476(4) . ? N24 C46 1.323(4) . ? N24 C47 1.384(4) . ? N25 C46 1.353(4) . ? N25 C48 1.370(5) . ? N25 C49 1.454(4) . ? N26 C51 1.323(4) . ? N26 C52 1.363(4) . ? N27 C51 1.350(4) . ? N27 C53 1.370(4) . ? N27 C54 1.466(4) . ? N28 C61 1.471(4) . ? N28 C56 1.480(3) . ? N28 C55 1.487(3) . ? N29 C57 1.326(4) . ? N29 C58 1.378(4) . ? N30 C59 1.355(4) . ? N30 C57 1.362(4) . ? N30 C60 1.454(4) . ? N31 C62 1.318(5) . ? N31 C63 1.373(6) . ? N32 C62 1.357(5) . ? N32 C64 1.393(6) . ? N32 C65 1.448(6) . ? O1A C26A 1.240(5) . ? O2A C26A 1.267(5) . ? C26A C27A 1.490(6) . ? O1B C26B 1.19(3) . ? O2B C26B 1.14(3) . ? C26B C27B 1.51(3) . ? O3 C28 1.283(3) . ? O4 C28 1.233(4) . ? O5A C30A 1.258(7) . ? O6A C30A 1.251(9) . ? C30A C31A 1.531(9) . ? O5B C30B 1.272(17) . ? O6B C30B 1.229(19) . ? C30B C31B 1.482(19) . ? O11 C66 1.282(3) . ? O12 C66 1.232(4) . ? O13 C68 1.246(4) . ? O14A C68 1.259(5) . ? O14B C68 1.298(11) . ? O15 C70 1.246(4) . ? O16 C70 1.254(4) . ? C1 C2 1.375(4) . ? C1 C3 1.399(4) . ? C2 C4 1.496(4) . ? C3 C15 1.501(4) . ? C5 C6 1.478(4) . ? C7 C8 1.345(5) . ? C10 C11 1.491(4) . ? C12 C13 1.341(5) . ? C16 C17 1.487(4) . ? C18 C19 1.341(5) . ? C21 C22 1.501(4) . ? C23 C24 1.334(6) . ? C28 C29 1.504(4) . ? C41 C42 1.381(4) . ? C41 C43 1.399(4) . ? C42 C44 1.499(4) . ? C43 C55 1.505(4) . ? C45 C46 1.490(4) . ? C47 C48 1.341(5) . ? C50 C51 1.505(4) . ? C52 C53 1.362(5) . ? C56 C57 1.489(4) . ? C58 C59 1.354(4) . ? C61 C62 1.480(4) . ? C63 C64 1.321(8) . ? C66 C67 1.501(4) . ? C68 C69 1.510(4) . ? C70 C71 1.510(4) . ? N42 C74 1.137(10) . ? C74 C75 1.423(12) . ? N43 C76 1.150(7) . ? C76 C77 1.415(8) . ? N44 C78 1.118(6) . ? C78 C79 1.411(7) . ? N45 C80 1.132(6) . ? C80 C81 1.448(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N4 125.37(9) . . ? N1 Fe1 O3 85.06(8) . . ? N4 Fe1 O3 145.07(8) . . ? N1 Fe1 N6 103.62(9) . . ? N4 Fe1 N6 92.91(9) . . ? O3 Fe1 N6 95.92(8) . . ? N1 Fe1 O1A 88.51(9) . . ? N4 Fe1 O1A 80.97(9) . . ? O3 Fe1 O1A 83.50(8) . . ? N6 Fe1 O1A 167.78(9) . . ? O2A Fe2 O6B 111.2(5) . . ? O2A Fe2 N2 110.05(10) . . ? O6B Fe2 N2 137.8(5) . . ? O2A Fe2 N9 87.05(9) . . ? O6B Fe2 N9 90.1(3) . . ? N2 Fe2 N9 100.46(9) . . ? O2A Fe2 O5A 154.16(12) . . ? O6B Fe2 O5A 43.0(4) . . ? N2 Fe2 O5A 95.61(10) . . ? N9 Fe2 O5A 91.31(10) . . ? O2A Fe2 O3 87.67(9) . . ? O6B Fe2 O3 88.9(3) . . ? N2 Fe2 O3 84.31(7) . . ? N9 Fe2 O3 173.86(8) . . ? O5A Fe2 O3 92.07(9) . . ? O2A Fe2 O1B 23.1(5) . . ? O6B Fe2 O1B 134.3(7) . . ? N2 Fe2 O1B 87.0(5) . . ? N9 Fe2 O1B 88.9(5) . . ? O5A Fe2 O1B 177.3(5) . . ? O3 Fe2 O1B 87.5(5) . . ? O2A Fe2 O6A 95.85(14) . . ? O6B Fe2 O6A 15.5(4) . . ? N2 Fe2 O6A 153.30(13) . . ? N9 Fe2 O6A 86.83(11) . . ? O5A Fe2 O6A 58.31(13) . . ? O3 Fe2 O6A 90.58(10) . . ? O1B Fe2 O6A 119.0(5) . . ? N21 Fe11 O11 86.30(8) . . ? N21 Fe11 N26 113.96(9) . . ? O11 Fe11 N26 135.87(9) . . ? N21 Fe11 N24 118.23(10) . . ? O11 Fe11 N24 102.65(9) . . ? N26 Fe11 N24 100.93(10) . . ? O13 Fe12 N22 121.01(9) . . ? O13 Fe12 O15 144.07(9) . . ? N22 Fe12 O15 92.24(9) . . ? O13 Fe12 N29 91.67(9) . . ? N22 Fe12 N29 98.73(8) . . ? O15 Fe12 N29 96.59(9) . . ? O13 Fe12 O11 87.84(8) . . ? N22 Fe12 O11 84.93(7) . . ? O15 Fe12 O11 81.53(8) . . ? N29 Fe12 O11 175.98(8) . . ? C2 N1 N2 107.9(2) . . ? C2 N1 Fe1 126.37(17) . . ? N2 N1 Fe1 125.59(16) . . ? C3 N2 N1 107.7(2) . . ? C3 N2 Fe2 133.92(17) . . ? N1 N2 Fe2 116.46(16) . . ? C10 N3 C4 111.3(2) . . ? C10 N3 C5 114.0(2) . . ? C4 N3 C5 114.6(2) . . ? C6 N4 C7 106.5(3) . . ? C6 N4 Fe1 124.92(19) . . ? C7 N4 Fe1 128.4(2) . . ? C8 N5 C6 107.7(3) . . ? C8 N5 C9 126.7(3) . . ? C6 N5 C9 125.6(3) . . ? C11 N6 C12 105.0(3) . . ? C11 N6 Fe1 122.84(19) . . ? C12 N6 Fe1 131.5(2) . . ? C11 N7 C13 106.9(3) . . ? C11 N7 C14 126.0(3) . . ? C13 N7 C14 127.0(3) . . ? C21 N8 C16 110.6(2) . . ? C21 N8 C15 112.6(2) . . ? C16 N8 C15 110.7(2) . . ? C17 N9 C18 104.9(2) . . ? C17 N9 Fe2 130.57(19) . . ? C18 N9 Fe2 124.3(2) . . ? C17 N10 C19 106.5(3) . . ? C17 N10 C20 126.1(3) . . ? C19 N10 C20 127.3(3) . . ? C22 N11 C23 104.7(3) . . ? C22 N12 C24 106.8(3) . . ? C22 N12 C25 126.3(3) . . ? C24 N12 C25 126.9(3) . . ? C42 N21 N22 108.2(2) . . ? C42 N21 Fe11 125.64(18) . . ? N22 N21 Fe11 125.91(16) . . ? C43 N22 N21 107.3(2) . . ? C43 N22 Fe12 136.31(18) . . ? N21 N22 Fe12 116.25(15) . . ? C50 N23 C45 114.1(2) . . ? C50 N23 C44 112.8(2) . . ? C45 N23 C44 111.8(2) . . ? C46 N24 C47 105.7(3) . . ? C46 N24 Fe11 122.1(2) . . ? C47 N24 Fe11 132.2(2) . . ? C46 N25 C48 107.4(3) . . ? C46 N25 C49 126.8(3) . . ? C48 N25 C49 125.8(3) . . ? C51 N26 C52 106.6(2) . . ? C51 N26 Fe11 118.69(18) . . ? C52 N26 Fe11 134.7(2) . . ? C51 N27 C53 107.4(2) . . ? C51 N27 C54 126.1(3) . . ? C53 N27 C54 126.5(3) . . ? C61 N28 C56 111.6(2) . . ? C61 N28 C55 111.9(2) . . ? C56 N28 C55 110.8(2) . . ? C57 N29 C58 105.5(2) . . ? C57 N29 Fe12 133.48(19) . . ? C58 N29 Fe12 120.33(19) . . ? C59 N30 C57 107.5(2) . . ? C59 N30 C60 125.7(2) . . ? C57 N30 C60 126.7(2) . . ? C62 N31 C63 104.9(4) . . ? C62 N32 C64 105.6(4) . . ? C62 N32 C65 126.3(3) . . ? C64 N32 C65 128.0(4) . . ? C26A O1A Fe1 137.4(2) . . ? C26A O2A Fe2 130.0(2) . . ? O1A C26A O2A 125.7(3) . . ? O1A C26A C27A 115.3(3) . . ? O2A C26A C27A 119.0(4) . . ? C26B O1B Fe2 105.8(18) . . ? O2B C26B O1B 109(3) . . ? O2B C26B C27B 124(2) . . ? O1B C26B C27B 122(2) . . ? C28 O3 Fe1 96.21(17) . . ? C28 O3 Fe2 135.12(18) . . ? Fe1 O3 Fe2 109.68(8) . . ? C30A O5A Fe2 91.0(4) . . ? C30A O6A Fe2 88.0(4) . . ? O6A C30A O5A 122.5(6) . . ? O6A C30A C31A 119.3(5) . . ? O5A C30A C31A 117.9(7) . . ? C30B O6B Fe2 112.2(10) . . ? O6B C30B O5B 128.2(12) . . ? O6B C30B C31B 108.3(13) . . ? O5B C30B C31B 121.3(13) . . ? C66 O11 Fe11 103.52(18) . . ? C66 O11 Fe12 125.42(16) . . ? Fe11 O11 Fe12 107.02(8) . . ? C68 O13 Fe12 122.2(2) . . ? C70 O15 Fe12 97.2(2) . . ? C2 C1 C3 104.4(2) . . ? N1 C2 C1 110.5(2) . . ? N1 C2 C4 118.5(2) . . ? C1 C2 C4 130.8(2) . . ? N2 C3 C1 109.6(2) . . ? N2 C3 C15 121.5(2) . . ? C1 C3 C15 128.4(2) . . ? N3 C4 C2 109.7(2) . . ? N3 C5 C6 111.4(2) . . ? N4 C6 N5 109.5(3) . . ? N4 C6 C5 125.8(2) . . ? N5 C6 C5 124.7(3) . . ? C8 C7 N4 109.4(3) . . ? C7 C8 N5 106.8(3) . . ? N3 C10 C11 110.5(2) . . ? N6 C11 N7 111.5(2) . . ? N6 C11 C10 124.3(2) . . ? N7 C11 C10 124.2(3) . . ? C13 C12 N6 109.9(3) . . ? C12 C13 N7 106.6(3) . . ? N8 C15 C3 113.2(2) . . ? N8 C16 C17 109.6(2) . . ? N9 C17 N10 111.9(3) . . ? N9 C17 C16 126.6(2) . . ? N10 C17 C16 121.3(3) . . ? C19 C18 N9 110.1(3) . . ? C18 C19 N10 106.6(3) . . ? N8 C21 C22 109.7(2) . . ? N11 C22 N12 111.3(3) . . ? N11 C22 C21 125.3(3) . . ? N12 C22 C21 123.3(3) . . ? C24 C23 N11 111.5(3) . . ? C23 C24 N12 105.5(3) . . ? O4 C28 O3 120.3(3) . . ? O4 C28 C29 121.4(3) . . ? O3 C28 C29 118.3(3) . . ? C42 C41 C43 104.3(2) . . ? N21 C42 C41 110.1(2) . . ? N21 C42 C44 118.4(2) . . ? C41 C42 C44 131.0(2) . . ? N22 C43 C41 110.0(2) . . ? N22 C43 C55 121.2(2) . . ? C41 C43 C55 128.7(2) . . ? N23 C44 C42 110.1(2) . . ? N23 C45 C46 109.9(2) . . ? N24 C46 N25 110.5(3) . . ? N24 C46 C45 124.0(3) . . ? N25 C46 C45 125.2(3) . . ? C48 C47 N24 109.7(3) . . ? C47 C48 N25 106.6(3) . . ? N23 C50 C51 109.0(2) . . ? N26 C51 N27 110.5(2) . . ? N26 C51 C50 123.7(3) . . ? N27 C51 C50 125.8(3) . . ? C53 C52 N26 109.4(3) . . ? C52 C53 N27 106.2(3) . . ? N28 C55 C43 115.0(2) . . ? N28 C56 C57 110.6(2) . . ? N29 C57 N30 110.5(2) . . ? N29 C57 C56 126.2(2) . . ? N30 C57 C56 123.3(2) . . ? C59 C58 N29 109.8(3) . . ? C58 C59 N30 106.7(2) . . ? N28 C61 C62 111.0(2) . . ? N31 C62 N32 111.8(3) . . ? N31 C62 C61 125.1(3) . . ? N32 C62 C61 123.1(3) . . ? C64 C63 N31 111.1(4) . . ? C63 C64 N32 106.6(4) . . ? O12 C66 O11 121.2(3) . . ? O12 C66 C67 121.8(3) . . ? O11 C66 C67 116.9(3) . . ? O13 C68 O14A 123.4(3) . . ? O13 C68 O14B 117.0(6) . . ? O14A C68 O14B 46.3(5) . . ? O13 C68 C69 116.8(3) . . ? O14A C68 C69 118.7(3) . . ? O14B C68 C69 113.5(5) . . ? O15 C70 O16 121.1(3) . . ? O15 C70 C71 119.3(3) . . ? O16 C70 C71 119.6(3) . . ? N42 C74 C75 175.8(9) . . ? N43 C76 C77 177.3(6) . . ? N44 C78 C79 177.9(6) . . ? N45 C80 C81 177.6(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.589 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.049 data_1-bb70m25at248K-one-crystal _database_code_depnum_ccdc_archive 'CCDC 831483' #TrackingRef '- pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H42 Fe2 N12 O6, 2(C2 H3 N)' _chemical_formula_sum 'C35 H48 Fe2 N14 O6' _chemical_formula_weight 872.57 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 'P 21 21 21' 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 16.3877(4) _cell_length_b 19.0209(4) _cell_length_c 26.5783(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8284.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 248(2) _cell_measurement_reflns_used 98806 _cell_measurement_theta_min 1.32 _cell_measurement_theta_max 25.71 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7817 _exptl_absorpt_correction_T_max 0.8669 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 248(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 98806 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.71 _reflns_number_total 15703 _reflns_number_gt 13393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0467P)^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 0.007(9) _refine_ls_number_reflns 15703 _refine_ls_number_parameters 1032 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.77252(3) 0.41521(2) 0.613088(16) 0.03866(11) Uani 1 1 d . . . Fe2 Fe 0.90951(3) 0.28556(2) 0.561508(17) 0.03635(10) Uani 1 1 d . . . Fe11 Fe 0.24958(3) 0.59881(2) 0.592224(15) 0.03873(11) Uani 1 1 d . . . Fe12 Fe 0.43202(2) 0.68911(2) 0.563012(15) 0.03260(9) Uani 1 1 d . . . N1 N 0.79768(13) 0.40533(12) 0.53546(8) 0.0314(5) Uani 1 1 d . A . N2 N 0.83708(14) 0.35023(12) 0.51344(9) 0.0323(5) Uani 1 1 d . A . N3 N 0.68586(14) 0.50889(12) 0.55920(9) 0.0352(5) Uani 1 1 d . . . N4 N 0.76544(17) 0.51116(13) 0.65259(9) 0.0426(6) Uani 1 1 d . A . N5 N 0.7348(2) 0.62083(15) 0.67035(11) 0.0575(8) Uani 1 1 d . A . N6 N 0.64204(16) 0.39476(13) 0.61891(10) 0.0430(6) Uani 1 1 d . A . N7 N 0.51407(16) 0.39347(15) 0.59432(11) 0.0477(7) Uani 1 1 d . A . N8 N 0.95832(15) 0.34604(13) 0.40966(9) 0.0367(5) Uani 1 1 d . . . N9 N 1.01553(16) 0.26541(13) 0.51241(10) 0.0416(6) Uani 1 1 d . A . N10 N 1.11686(16) 0.27480(15) 0.45807(11) 0.0469(7) Uani 1 1 d . A . N11 N 1.0732(2) 0.47296(18) 0.35771(13) 0.0681(9) Uani 1 1 d . . . N12 N 1.04764(19) 0.38368(16) 0.30710(10) 0.0522(7) Uani 1 1 d . . . N21 N 0.28587(14) 0.61830(13) 0.51892(8) 0.0343(5) Uani 1 1 d . . . N22 N 0.35460(14) 0.65437(12) 0.50459(8) 0.0313(5) Uani 1 1 d . . . N23 N 0.15319(16) 0.53491(14) 0.53223(10) 0.0417(6) Uani 1 1 d . . . N24 N 0.13035(16) 0.62534(14) 0.61238(11) 0.0452(6) Uani 1 1 d . . . N25 N -0.00396(17) 0.62229(16) 0.61069(12) 0.0527(7) Uani 1 1 d . . . N26 N 0.25229(16) 0.49304(13) 0.61237(9) 0.0404(6) Uani 1 1 d . . . N27 N 0.22972(17) 0.38032(13) 0.59988(10) 0.0449(6) Uani 1 1 d . . . N28 N 0.48327(15) 0.64802(12) 0.40586(9) 0.0347(5) Uani 1 1 d . . . N29 N 0.54837(15) 0.68859(14) 0.52192(9) 0.0398(6) Uani 1 1 d . . . N30 N 0.64766(15) 0.68352(14) 0.46591(9) 0.0405(6) Uani 1 1 d . . . N31 N 0.3469(3) 0.6513(2) 0.31106(12) 0.0854(13) Uani 1 1 d . . . N32 N 0.4760(3) 0.66263(18) 0.28782(11) 0.0688(10) Uani 1 1 d . . . O1A O 0.90638(19) 0.43613(15) 0.62472(11) 0.0534(10) Uiso 0.806(6) 1 d P A 1 O2A O 0.98433(18) 0.34483(18) 0.60404(12) 0.0495(9) Uiso 0.806(6) 1 d P A 1 C26A C 0.9701(2) 0.4009(2) 0.62788(13) 0.0334(9) Uiso 0.806(6) 1 d P A 1 C27A C 1.0317(4) 0.4293(3) 0.6635(2) 0.050(2) Uiso 0.806(6) 1 d P A 1 H27A H 1.0792 0.3989 0.6638 0.080 Uiso 0.806(6) 1 calc PR A 1 H27B H 1.0084 0.4315 0.6970 0.080 Uiso 0.806(6) 1 calc PR A 1 H27C H 1.0477 0.4761 0.6530 0.080 Uiso 0.806(6) 1 calc PR A 1 O1B O 0.9669(8) 0.3866(8) 0.5880(5) 0.058(4) Uiso 0.194(6) 1 d P A 2 O2B O 1.0005(9) 0.3089(9) 0.6356(5) 0.069(5) Uiso 0.194(6) 1 d P A 2 C26B C 0.9967(12) 0.3691(12) 0.6285(7) 0.045(4) Uiso 0.194(6) 1 d P A 2 C27B C 1.0475(12) 0.4230(9) 0.6573(7) 0.019(5) Uiso 0.194(6) 1 d P A 2 H27D H 1.0685 0.4016 0.6878 0.080 Uiso 0.194(6) 1 calc PR A 2 H27E H 1.0136 0.4630 0.6660 0.080 Uiso 0.194(6) 1 calc PR A 2 H27F H 1.0926 0.4385 0.6365 0.080 Uiso 0.194(6) 1 calc PR A 2 O3 O 0.81134(12) 0.30650(11) 0.61811(8) 0.0411(5) Uani 1 1 d . A . O4 O 0.78516(19) 0.35156(14) 0.69148(9) 0.0657(7) Uani 1 1 d . A . O5A O 0.8524(2) 0.1839(2) 0.53743(15) 0.0471(14) Uiso 0.623(10) 1 d P A 3 O6A O 0.9404(3) 0.1803(2) 0.59974(18) 0.0560(15) Uiso 0.623(10) 1 d P A 3 C30A C 0.8897(5) 0.1511(5) 0.5720(3) 0.0561(19) Uiso 0.623(10) 1 d P A 3 C31A C 0.8791(6) 0.0707(4) 0.5736(3) 0.066(2) Uiso 0.623(10) 1 d P A 3 H31A H 0.8376 0.0567 0.5496 0.080 Uiso 0.623(10) 1 calc PR A 3 H31B H 0.8626 0.0565 0.6072 0.080 Uiso 0.623(10) 1 calc PR A 3 H31C H 0.9304 0.0482 0.5651 0.080 Uiso 0.623(10) 1 calc PR A 3 O5B O 0.8251(5) 0.1580(5) 0.5190(3) 0.070(3) Uiso 0.377(10) 1 d P A 4 O6B O 0.9068(7) 0.1840(6) 0.5826(4) 0.075(3) Uiso 0.377(10) 1 d P A 4 C30B C 0.8665(7) 0.1431(6) 0.5570(4) 0.043(3) Uiso 0.377(10) 1 d P A 4 C31B C 0.8529(10) 0.0759(7) 0.5845(6) 0.072(4) Uiso 0.377(10) 1 d P A 4 H31D H 0.8220 0.0439 0.5634 0.080 Uiso 0.377(10) 1 calc PR A 4 H31E H 0.8227 0.0851 0.6152 0.080 Uiso 0.377(10) 1 calc PR A 4 H31F H 0.9052 0.0549 0.5927 0.080 Uiso 0.377(10) 1 calc PR A 4 O11 O 0.31450(12) 0.68871(11) 0.61172(7) 0.0389(5) Uani 1 1 d . . . O12 O 0.28645(17) 0.63818(14) 0.68367(10) 0.0636(7) Uani 1 1 d . . . O13 O 0.44323(16) 0.79128(12) 0.57886(9) 0.0579(6) Uani 1 1 d . B . O14A O 0.3754(3) 0.8252(2) 0.51193(16) 0.0763(12) Uiso 0.727(5) 1 d P B 5 O14B O 0.4374(8) 0.8322(6) 0.5027(4) 0.0763(12) Uiso 0.273(5) 1 d P B 6 O15 O 0.44251(16) 0.58461(13) 0.59421(9) 0.0560(6) Uani 1 1 d . . . O16 O 0.49842(16) 0.66318(15) 0.64244(11) 0.0645(7) Uani 1 1 d . . . C1 C 0.79305(17) 0.42302(15) 0.45271(11) 0.0351(7) Uani 1 1 d . A . H1 H 0.7819 0.4428 0.4210 0.080 Uiso 1 1 calc R . . C2 C 0.77275(16) 0.44919(14) 0.49906(10) 0.0301(6) Uani 1 1 d . . . C3 C 0.83402(17) 0.36034(15) 0.46310(11) 0.0314(6) Uani 1 1 d . . . C4 C 0.73553(19) 0.51804(15) 0.51403(11) 0.0390(7) Uani 1 1 d . A . H4A H 0.7787 0.5525 0.5206 0.080 Uiso 1 1 calc R . . H4B H 0.7015 0.5359 0.4865 0.080 Uiso 1 1 calc R . . C5 C 0.6771(2) 0.57214(17) 0.59014(13) 0.0465(8) Uani 1 1 d . A . H5A H 0.6194 0.5790 0.5984 0.080 Uiso 1 1 calc R . . H5B H 0.6955 0.6131 0.5709 0.080 Uiso 1 1 calc R . . C6 C 0.72467(19) 0.56697(16) 0.63689(12) 0.0403(7) Uani 1 1 d . . . C7 C 0.8025(3) 0.5300(2) 0.69672(14) 0.0647(11) Uani 1 1 d . . . H7 H 0.8358 0.5005 0.7163 0.080 Uiso 1 1 calc R A . C8 C 0.7840(3) 0.5970(2) 0.70768(15) 0.0752(13) Uani 1 1 d . A . H8 H 0.8018 0.6226 0.7359 0.080 Uiso 1 1 calc R . . C9 C 0.6995(3) 0.6913(2) 0.66577(18) 0.0744(12) Uani 1 1 d . . . H9A H 0.7279 0.7172 0.6396 0.080 Uiso 1 1 calc R A . H9B H 0.7051 0.7160 0.6975 0.080 Uiso 1 1 calc R . . H9C H 0.6422 0.6875 0.6571 0.080 Uiso 1 1 calc R . . C10 C 0.60886(18) 0.47390(17) 0.54761(11) 0.0382(7) Uani 1 1 d . A . H10A H 0.6131 0.4502 0.5150 0.080 Uiso 1 1 calc R . . H10B H 0.5651 0.5089 0.5454 0.080 Uiso 1 1 calc R . . C11 C 0.58863(19) 0.42137(15) 0.58735(11) 0.0378(7) Uani 1 1 d . . . C12 C 0.5980(2) 0.34817(19) 0.64807(14) 0.0559(9) Uani 1 1 d . . . H12 H 0.6195 0.3216 0.6748 0.080 Uiso 1 1 calc R A . C13 C 0.5204(3) 0.3465(2) 0.63274(16) 0.0631(10) Uani 1 1 d . A . H13 H 0.4784 0.3183 0.6459 0.080 Uiso 1 1 calc R . . C14 C 0.4414(2) 0.4083(2) 0.56392(16) 0.0623(10) Uani 1 1 d . . . H14A H 0.4241 0.4564 0.5696 0.080 Uiso 1 1 calc R A . H14B H 0.3979 0.3764 0.5734 0.080 Uiso 1 1 calc R . . H14C H 0.4543 0.4019 0.5286 0.080 Uiso 1 1 calc R . . C15 C 0.88117(18) 0.31399(16) 0.42737(11) 0.0368(6) Uani 1 1 d . A . H15A H 0.8936 0.2694 0.4442 0.080 Uiso 1 1 calc R . . H15B H 0.8468 0.3034 0.3982 0.080 Uiso 1 1 calc R . . C16 C 1.01055(19) 0.36655(16) 0.45252(11) 0.0383(7) Uani 1 1 d . A . H16A H 1.0539 0.3980 0.4408 0.080 Uiso 1 1 calc R . . H16B H 0.9779 0.3918 0.4776 0.080 Uiso 1 1 calc R . . C17 C 1.04693(17) 0.30336(16) 0.47571(12) 0.0385(7) Uani 1 1 d . . . C18 C 1.0690(2) 0.20963(17) 0.51841(14) 0.0498(8) Uani 1 1 d . . . H18 H 1.0628 0.1733 0.5421 0.080 Uiso 1 1 calc R A . C19 C 1.1305(2) 0.21483(19) 0.48571(14) 0.0523(9) Uani 1 1 d . A . H19 H 1.1746 0.1836 0.4823 0.080 Uiso 1 1 calc R . . C20 C 1.1660(2) 0.3016(2) 0.41685(14) 0.0617(10) Uani 1 1 d . . . H20A H 1.1329 0.3043 0.3866 0.080 Uiso 1 1 calc R A . H20B H 1.2118 0.2703 0.4110 0.080 Uiso 1 1 calc R . . H20C H 1.1862 0.3480 0.4253 0.080 Uiso 1 1 calc R . . C21 C 0.9449(2) 0.40618(17) 0.37559(12) 0.0451(8) Uani 1 1 d . . . H21A H 0.9284 0.4475 0.3952 0.080 Uiso 1 1 calc R . . H21B H 0.9009 0.3951 0.3519 0.080 Uiso 1 1 calc R . . C22 C 1.0213(2) 0.42211(18) 0.34719(13) 0.0498(8) Uani 1 1 d . . . C23 C 1.1357(3) 0.4653(3) 0.32368(18) 0.0780(13) Uani 1 1 d . . . H23 H 1.1825 0.4938 0.3226 0.080 Uiso 1 1 calc R . . C24 C 1.1211(3) 0.4119(2) 0.29225(15) 0.0685(11) Uani 1 1 d . . . H24 H 1.1542 0.3968 0.2655 0.080 Uiso 1 1 calc R . . C25 C 1.0055(3) 0.3229(2) 0.28509(15) 0.0719(12) Uani 1 1 d . . . H25A H 1.0253 0.2801 0.3007 0.080 Uiso 1 1 calc R . . H25B H 1.0161 0.3212 0.2492 0.080 Uiso 1 1 calc R . . H25C H 0.9473 0.3272 0.2908 0.080 Uiso 1 1 calc R . . C28 C 0.80528(19) 0.30059(18) 0.66569(11) 0.0414(7) Uani 1 1 d . . . C29 C 0.8226(3) 0.2303(2) 0.68923(13) 0.0602(10) Uani 1 1 d . A . H29A H 0.8145 0.2333 0.7253 0.080 Uiso 1 1 calc R . . H29B H 0.8786 0.2170 0.6823 0.080 Uiso 1 1 calc R . . H29C H 0.7860 0.1954 0.6753 0.080 Uiso 1 1 calc R . . C41 C 0.28139(18) 0.62943(15) 0.43528(11) 0.0369(6) Uani 1 1 d . . . H41 H 0.2646 0.6261 0.4015 0.080 Uiso 1 1 calc R . . C42 C 0.24188(18) 0.60384(15) 0.47751(10) 0.0355(6) Uani 1 1 d . . . C43 C 0.35178(18) 0.66137(14) 0.45416(10) 0.0321(6) Uani 1 1 d . . . C44 C 0.1588(2) 0.57238(18) 0.48369(12) 0.0448(8) Uani 1 1 d . . . H44A H 0.1175 0.6096 0.4824 0.080 Uiso 1 1 calc R . . H44B H 0.1481 0.5395 0.4561 0.080 Uiso 1 1 calc R . . C45 C 0.0709(2) 0.53820(19) 0.55330(13) 0.0497(8) Uani 1 1 d . . . H45A H 0.0575 0.4933 0.5694 0.080 Uiso 1 1 calc R . . H45B H 0.0313 0.5466 0.5263 0.080 Uiso 1 1 calc R . . C46 C 0.0663(2) 0.59624(17) 0.59115(12) 0.0445(7) Uani 1 1 d . . . C47 C 0.0994(3) 0.6717(2) 0.64783(15) 0.0603(10) Uani 1 1 d . . . H47 H 0.1309 0.7000 0.6693 0.080 Uiso 1 1 calc R . . C48 C 0.0178(2) 0.6699(2) 0.64687(15) 0.0617(10) Uani 1 1 d . . . H48 H -0.0178 0.6964 0.6672 0.080 Uiso 1 1 calc R . . C49 C -0.0860(2) 0.6035(2) 0.59625(18) 0.0719(12) Uani 1 1 d . . . H49A H -0.0977 0.6225 0.5632 0.080 Uiso 1 1 calc R . . H49B H -0.1243 0.6226 0.6205 0.080 Uiso 1 1 calc R . . H49C H -0.0911 0.5527 0.5954 0.080 Uiso 1 1 calc R . . C50 C 0.1872(2) 0.46426(18) 0.53022(13) 0.0520(9) Uani 1 1 d . . . H50A H 0.2302 0.4621 0.5047 0.080 Uiso 1 1 calc R . . H50B H 0.1444 0.4306 0.5210 0.080 Uiso 1 1 calc R . . C51 C 0.22166(19) 0.44587(16) 0.58082(11) 0.0396(7) Uani 1 1 d . . . C52 C 0.2813(2) 0.45654(19) 0.65271(12) 0.0467(8) Uani 1 1 d . . . H52 H 0.3069 0.4765 0.6810 0.080 Uiso 1 1 calc R . . C53 C 0.2673(2) 0.38645(18) 0.64565(12) 0.0496(8) Uani 1 1 d . . . H53 H 0.2809 0.3497 0.6678 0.080 Uiso 1 1 calc R . . C54 C 0.2030(2) 0.31513(18) 0.57579(16) 0.0613(10) Uani 1 1 d . . . H54A H 0.1459 0.3191 0.5666 0.080 Uiso 1 1 calc R . . H54B H 0.2100 0.2762 0.5990 0.080 Uiso 1 1 calc R . . H54C H 0.2354 0.3068 0.5458 0.080 Uiso 1 1 calc R . . C55 C 0.41986(18) 0.69633(14) 0.42559(10) 0.0341(6) Uani 1 1 d . . . H55A H 0.3962 0.7223 0.3973 0.080 Uiso 1 1 calc R . . H55B H 0.4462 0.7307 0.4478 0.080 Uiso 1 1 calc R . . C56 C 0.52423(18) 0.60984(15) 0.44735(11) 0.0358(6) Uani 1 1 d . . . H56A H 0.5606 0.5740 0.4333 0.080 Uiso 1 1 calc R . . H56B H 0.4832 0.5861 0.4681 0.080 Uiso 1 1 calc R . . C57 C 0.57222(18) 0.65940(15) 0.47913(11) 0.0370(7) Uani 1 1 d . . . C58 C 0.6107(2) 0.73282(18) 0.53599(13) 0.0461(8) Uani 1 1 d . . . H58 H 0.6109 0.7611 0.5650 0.080 Uiso 1 1 calc R . . C59 C 0.6719(2) 0.72960(16) 0.50175(13) 0.0447(8) Uani 1 1 d . . . H59 H 0.7214 0.7545 0.5027 0.080 Uiso 1 1 calc R . . C60 C 0.6924(2) 0.6677(2) 0.41967(13) 0.0516(9) Uani 1 1 d . . . H60A H 0.7411 0.6965 0.4180 0.080 Uiso 1 1 calc R . . H60B H 0.6579 0.6775 0.3908 0.080 Uiso 1 1 calc R . . H60C H 0.7077 0.6184 0.4195 0.080 Uiso 1 1 calc R . . C61 C 0.4503(2) 0.59885(17) 0.36808(11) 0.0432(7) Uani 1 1 d . . . H61A H 0.4039 0.5733 0.3825 0.080 Uiso 1 1 calc R . . H61B H 0.4923 0.5645 0.3590 0.080 Uiso 1 1 calc R . . C62 C 0.4235(3) 0.63700(19) 0.32250(12) 0.0532(9) Uani 1 1 d . . . C63 C 0.3517(5) 0.6905(3) 0.26767(18) 0.111(2) Uani 1 1 d . . . H63 H 0.3064 0.7098 0.2509 0.080 Uiso 1 1 calc R . . C64 C 0.4276(5) 0.6975(2) 0.25257(16) 0.0959(19) Uani 1 1 d . . . H64 H 0.4457 0.7213 0.2237 0.080 Uiso 1 1 calc R . . C65 C 0.5636(3) 0.6520(3) 0.28645(17) 0.0949(17) Uani 1 1 d . . . H65A H 0.5877 0.6697 0.3173 0.080 Uiso 1 1 calc R . . H65B H 0.5864 0.6770 0.2579 0.080 Uiso 1 1 calc R . . H65C H 0.5753 0.6022 0.2832 0.080 Uiso 1 1 calc R . . C66 C 0.31230(18) 0.68917(17) 0.65997(11) 0.0376(7) Uani 1 1 d . . . C67 C 0.3397(2) 0.75500(19) 0.68576(13) 0.0552(9) Uani 1 1 d . . . H67A H 0.3386 0.7480 0.7219 0.080 Uiso 1 1 calc R . . H67B H 0.3034 0.7933 0.6769 0.080 Uiso 1 1 calc R . . H67C H 0.3948 0.7664 0.6752 0.080 Uiso 1 1 calc R . . C68 C 0.4179(3) 0.83777(19) 0.55047(14) 0.0570(9) Uani 1 1 d . . . C69 C 0.4229(2) 0.91272(16) 0.56917(15) 0.0558(9) Uani 1 1 d . B . H69A H 0.4095 0.9447 0.5420 0.080 Uiso 1 1 calc R . . H69B H 0.4778 0.9223 0.5810 0.080 Uiso 1 1 calc R . . H69C H 0.3846 0.9193 0.5966 0.080 Uiso 1 1 calc R . . C70 C 0.4763(2) 0.60108(19) 0.63443(13) 0.0470(8) Uani 1 1 d . . . C71 C 0.4931(3) 0.5454(2) 0.67325(14) 0.0585(10) Uani 1 1 d . . . H71A H 0.5473 0.5523 0.6871 0.080 Uiso 1 1 calc R . . H71B H 0.4899 0.4994 0.6577 0.080 Uiso 1 1 calc R . . H71C H 0.4531 0.5488 0.7000 0.080 Uiso 1 1 calc R . . N42 N 0.7350(6) 0.3165(5) 0.3247(3) 0.156(3) Uani 1 1 d . . . C74 C 0.6786(6) 0.3443(7) 0.3388(4) 0.146(5) Uani 1 1 d . . . C75 C 0.6145(5) 0.3861(7) 0.3575(3) 0.206(6) Uani 1 1 d . . . H75A H 0.6312 0.4076 0.3890 0.310 Uiso 1 1 calc R . . H75B H 0.5668 0.3570 0.3632 0.310 Uiso 1 1 calc R . . H75C H 0.6015 0.4226 0.3333 0.310 Uiso 1 1 calc R . . N43 N 0.7535(5) 0.4672(3) 0.8356(2) 0.135(2) Uani 1 1 d . . . C76 C 0.7036(5) 0.4597(3) 0.8054(2) 0.101(2) Uani 1 1 d . . . C77 C 0.6461(5) 0.4479(4) 0.7671(2) 0.130(2) Uani 1 1 d . . . H77A H 0.6677 0.4141 0.7433 0.196 Uiso 1 1 calc R . . H77B H 0.6347 0.4918 0.7499 0.196 Uiso 1 1 calc R . . H77C H 0.5962 0.4297 0.7818 0.196 Uiso 1 1 calc R . . N44 N 0.0046(5) 0.5419(4) 0.7744(2) 0.151(3) Uani 1 1 d . . . C78 C 0.0709(4) 0.5409(3) 0.76552(19) 0.0874(15) Uani 1 1 d . . . C79 C 0.1546(3) 0.5375(3) 0.7538(2) 0.1004(17) Uani 1 1 d . . . H79A H 0.1800 0.5002 0.7732 0.151 Uiso 1 1 calc R . . H79B H 0.1804 0.5820 0.7619 0.151 Uiso 1 1 calc R . . H79C H 0.1612 0.5279 0.7182 0.151 Uiso 1 1 calc R . . N45 N 0.6014(4) 0.8291(4) 0.7593(2) 0.137(2) Uani 1 1 d . . . C80 C 0.5905(3) 0.8382(3) 0.7184(2) 0.0832(14) Uani 1 1 d . . . C81 C 0.5807(4) 0.8473(3) 0.66508(19) 0.0977(17) Uani 1 1 d . . . H81A H 0.6328 0.8402 0.6485 0.147 Uiso 1 1 calc R . . H81B H 0.5611 0.8944 0.6582 0.147 Uiso 1 1 calc R . . H81C H 0.5416 0.8133 0.6525 0.147 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 0.0489(3) 0.0303(2) 0.0368(2) -0.00259(18) 0.00408(19) 0.00226(19) Fe2 0.0322(2) 0.0309(2) 0.0460(2) 0.00520(19) -0.00186(19) 0.00429(17) Fe11 0.0457(3) 0.0368(2) 0.0337(2) 0.00053(17) 0.00259(19) -0.0112(2) Fe12 0.0307(2) 0.0316(2) 0.0355(2) -0.00302(17) -0.00177(18) -0.00309(16) N1 0.0288(12) 0.0304(12) 0.0349(12) 0.0025(10) 0.0043(10) 0.0052(10) N2 0.0310(13) 0.0287(12) 0.0371(13) 0.0012(10) 0.0029(10) 0.0048(10) N3 0.0311(13) 0.0312(12) 0.0432(14) -0.0072(11) 0.0024(11) 0.0021(10) N4 0.0480(17) 0.0403(14) 0.0396(13) -0.0072(11) -0.0012(12) -0.0011(13) N5 0.060(2) 0.0472(16) 0.0654(19) -0.0276(14) -0.0051(16) 0.0073(14) N6 0.0464(16) 0.0363(14) 0.0465(15) -0.0025(12) 0.0053(13) -0.0026(12) N7 0.0381(15) 0.0454(16) 0.0597(17) -0.0136(14) 0.0063(13) -0.0073(12) N8 0.0347(14) 0.0345(13) 0.0409(13) -0.0060(11) 0.0058(11) 0.0024(10) N9 0.0374(15) 0.0319(14) 0.0556(17) -0.0064(12) -0.0030(13) 0.0080(11) N10 0.0320(14) 0.0494(17) 0.0593(17) -0.0202(14) -0.0025(12) 0.0072(12) N11 0.071(2) 0.060(2) 0.074(2) -0.0088(16) 0.0322(18) -0.0161(18) N12 0.062(2) 0.0508(17) 0.0433(15) 0.0039(13) 0.0198(14) 0.0086(14) N21 0.0288(13) 0.0416(14) 0.0324(12) -0.0013(10) -0.0014(10) -0.0079(10) N22 0.0306(13) 0.0312(12) 0.0321(12) -0.0002(10) 0.0003(10) -0.0043(10) N23 0.0410(15) 0.0413(15) 0.0429(14) 0.0078(12) -0.0041(12) -0.0126(12) N24 0.0397(15) 0.0467(15) 0.0493(15) -0.0003(13) 0.0001(13) -0.0034(12) N25 0.0409(17) 0.0519(17) 0.0653(19) 0.0214(15) -0.0009(14) 0.0022(13) N26 0.0395(14) 0.0416(13) 0.0402(13) 0.0016(11) -0.0015(12) -0.0053(12) N27 0.0442(16) 0.0370(13) 0.0537(16) 0.0012(11) -0.0055(13) -0.0028(12) N28 0.0389(14) 0.0312(13) 0.0339(12) -0.0014(11) 0.0030(11) -0.0013(10) N29 0.0341(14) 0.0408(14) 0.0444(14) -0.0015(12) 0.0028(11) -0.0034(11) N30 0.0347(14) 0.0424(14) 0.0445(14) 0.0026(12) 0.0057(12) -0.0029(12) N31 0.098(3) 0.117(3) 0.0405(18) -0.0181(19) -0.0096(18) 0.051(3) N32 0.111(3) 0.0542(19) 0.0410(17) -0.0030(14) 0.0063(19) -0.008(2) O3 0.0364(11) 0.0463(12) 0.0404(12) 0.0107(10) 0.0011(9) -0.0001(10) O4 0.092(2) 0.0575(16) 0.0473(14) -0.0085(12) -0.0119(14) 0.0135(15) O11 0.0341(11) 0.0464(12) 0.0364(11) -0.0074(10) -0.0050(9) -0.0018(9) O12 0.0696(18) 0.0594(16) 0.0618(15) 0.0169(13) -0.0091(14) -0.0132(13) O13 0.0710(17) 0.0337(12) 0.0689(16) 0.0021(11) 0.0100(13) 0.0020(11) O15 0.0752(17) 0.0482(13) 0.0445(13) -0.0009(11) -0.0014(13) 0.0162(13) O16 0.0522(16) 0.0524(17) 0.089(2) 0.0075(14) 0.0053(14) 0.0073(12) C1 0.0306(16) 0.0375(16) 0.0373(15) 0.0073(12) 0.0008(12) 0.0011(12) C2 0.0224(14) 0.0284(13) 0.0397(15) 0.0043(11) 0.0048(12) 0.0004(11) C3 0.0238(15) 0.0323(15) 0.0381(15) -0.0009(12) -0.0014(12) -0.0008(11) C4 0.0334(17) 0.0332(15) 0.0505(17) 0.0069(13) 0.0055(14) 0.0023(13) C5 0.0418(19) 0.0380(17) 0.060(2) -0.0159(15) -0.0046(16) 0.0106(14) C6 0.0337(17) 0.0375(17) 0.0495(17) -0.0106(13) 0.0065(14) -0.0016(13) C7 0.086(3) 0.064(3) 0.044(2) -0.0140(18) -0.0190(19) 0.003(2) C8 0.100(3) 0.071(3) 0.055(2) -0.026(2) -0.021(2) 0.007(3) C9 0.072(3) 0.054(2) 0.097(3) -0.034(2) -0.013(2) 0.009(2) C10 0.0307(17) 0.0427(17) 0.0413(17) -0.0029(13) -0.0007(13) -0.0021(13) C11 0.0343(16) 0.0340(15) 0.0451(16) -0.0135(13) 0.0083(14) -0.0021(13) C12 0.063(3) 0.0421(19) 0.063(2) 0.0047(17) 0.0087(19) -0.0091(18) C13 0.062(3) 0.052(2) 0.075(3) 0.006(2) 0.017(2) -0.0197(19) C14 0.0368(19) 0.065(2) 0.085(3) -0.014(2) 0.0031(19) -0.0112(17) C15 0.0385(16) 0.0338(14) 0.0380(16) -0.0046(13) 0.0011(12) -0.0008(13) C16 0.0355(17) 0.0350(16) 0.0443(18) -0.0095(13) 0.0046(13) 0.0001(13) C17 0.0272(15) 0.0401(17) 0.0482(17) -0.0159(14) 0.0005(13) 0.0003(13) C18 0.046(2) 0.0369(17) 0.067(2) -0.0085(15) -0.0157(18) 0.0103(15) C19 0.0379(19) 0.048(2) 0.071(2) -0.0236(18) -0.0084(17) 0.0153(15) C20 0.0359(19) 0.080(3) 0.069(2) -0.021(2) 0.0177(17) 0.0012(18) C21 0.049(2) 0.0402(17) 0.0460(17) -0.0009(14) 0.0122(14) 0.0069(15) C22 0.055(2) 0.0434(19) 0.0510(19) 0.0035(15) 0.0176(17) 0.0054(17) C23 0.065(3) 0.081(3) 0.089(3) 0.005(3) 0.033(2) -0.014(2) C24 0.077(3) 0.073(3) 0.056(2) 0.008(2) 0.032(2) 0.016(2) C25 0.092(3) 0.064(3) 0.060(2) -0.007(2) 0.015(2) 0.002(2) C28 0.0411(18) 0.047(2) 0.0363(17) 0.0053(14) -0.0080(13) -0.0069(14) C29 0.080(3) 0.055(2) 0.0451(19) 0.0163(17) -0.0077(18) 0.002(2) C41 0.0377(16) 0.0412(16) 0.0317(14) -0.0008(13) -0.0055(14) -0.0038(13) C42 0.0385(16) 0.0353(15) 0.0328(14) -0.0004(12) -0.0057(13) -0.0029(13) C43 0.0356(16) 0.0292(14) 0.0313(14) 0.0000(11) 0.0022(12) 0.0020(12) C44 0.0431(19) 0.051(2) 0.0404(17) 0.0093(14) -0.0082(14) -0.0095(15) C45 0.0411(19) 0.060(2) 0.0477(19) 0.0074(15) -0.0058(16) -0.0147(16) C46 0.0405(18) 0.0469(18) 0.0460(17) 0.0138(15) -0.0034(15) -0.0044(15) C47 0.058(3) 0.058(2) 0.064(2) -0.0062(18) 0.0004(19) 0.0036(19) C48 0.052(2) 0.064(3) 0.069(3) -0.002(2) 0.0058(19) 0.0109(19) C49 0.0327(19) 0.076(3) 0.107(3) 0.024(3) -0.003(2) -0.0024(19) C50 0.057(2) 0.0441(19) 0.055(2) -0.0029(16) -0.0161(17) -0.0108(16) C51 0.0374(17) 0.0379(16) 0.0434(17) -0.0005(13) -0.0030(13) -0.0050(13) C52 0.0430(19) 0.055(2) 0.0421(17) 0.0045(15) -0.0047(15) -0.0021(16) C53 0.045(2) 0.052(2) 0.0509(19) 0.0133(15) -0.0050(16) -0.0010(16) C54 0.061(2) 0.0365(17) 0.086(3) 0.0004(18) -0.017(2) -0.0043(17) C55 0.0385(16) 0.0293(14) 0.0346(14) 0.0009(11) 0.0028(12) 0.0009(12) C56 0.0351(16) 0.0321(15) 0.0401(16) 0.0005(12) 0.0023(13) -0.0002(12) C57 0.0327(17) 0.0367(15) 0.0415(16) 0.0068(13) 0.0024(13) -0.0014(13) C58 0.0405(19) 0.0490(19) 0.0487(18) -0.0051(15) -0.0014(15) -0.0107(15) C59 0.0360(18) 0.0372(18) 0.061(2) 0.0008(16) 0.0007(15) -0.0106(14) C60 0.042(2) 0.059(2) 0.053(2) 0.0047(16) 0.0111(15) -0.0024(16) C61 0.052(2) 0.0376(17) 0.0396(16) -0.0074(14) 0.0018(14) 0.0026(15) C62 0.072(3) 0.052(2) 0.0348(17) -0.0136(15) -0.0032(18) 0.0134(19) C63 0.172(7) 0.112(5) 0.049(3) -0.023(3) -0.026(3) 0.085(5) C64 0.190(7) 0.064(3) 0.034(2) -0.0011(19) -0.009(3) 0.020(4) C65 0.106(4) 0.118(4) 0.060(3) -0.006(3) 0.017(3) -0.048(4) C66 0.0288(15) 0.0440(17) 0.0400(17) -0.0039(14) -0.0029(12) 0.0046(14) C67 0.061(2) 0.056(2) 0.0480(19) -0.0137(16) -0.0079(17) 0.0005(18) C68 0.069(3) 0.0416(19) 0.060(2) 0.0044(17) 0.008(2) 0.0042(18) C69 0.064(2) 0.0286(15) 0.074(2) -0.0052(16) 0.0000(19) 0.0028(16) C70 0.0429(19) 0.047(2) 0.051(2) 0.0006(16) 0.0133(16) 0.0168(16) C71 0.077(3) 0.051(2) 0.048(2) 0.0047(17) 0.0003(18) 0.0185(19) N42 0.197(8) 0.162(7) 0.108(5) 0.036(4) -0.075(6) -0.043(7) C74 0.107(7) 0.219(12) 0.112(6) 0.096(8) -0.049(6) -0.055(7) C75 0.087(5) 0.369(17) 0.163(8) 0.145(10) -0.007(5) -0.007(8) N43 0.201(7) 0.116(4) 0.086(3) 0.014(3) 0.008(4) -0.005(5) C76 0.152(6) 0.082(4) 0.070(4) 0.015(3) 0.026(4) 0.014(4) C77 0.144(6) 0.153(7) 0.094(4) 0.015(4) 0.005(4) 0.014(5) N44 0.141(6) 0.182(7) 0.130(5) -0.036(4) 0.040(4) 0.006(5) C78 0.093(4) 0.101(4) 0.069(3) -0.021(3) 0.018(3) -0.007(3) C79 0.079(4) 0.107(4) 0.115(4) -0.008(3) -0.001(3) -0.020(3) N45 0.158(6) 0.177(6) 0.077(3) -0.013(4) 0.001(3) -0.017(5) C80 0.085(3) 0.098(4) 0.067(3) -0.014(3) 0.005(3) 0.011(3) C81 0.134(5) 0.077(3) 0.082(3) -0.004(3) -0.014(3) 0.018(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 N4 2.109(2) . ? Fe1 N1 2.112(2) . ? Fe1 O3 2.168(2) . ? Fe1 N6 2.179(3) . ? Fe1 O1A 2.251(3) . ? Fe2 O6B 2.013(11) . ? Fe2 O2A 2.013(3) . ? Fe2 N2 2.134(2) . ? Fe2 N9 2.207(3) . ? Fe2 O3 2.238(2) . ? Fe2 O5A 2.241(5) . ? Fe2 O1B 2.253(14) . ? Fe2 O6A 2.302(5) . ? Fe11 N21 2.071(2) . ? Fe11 O11 2.080(2) . ? Fe11 N26 2.082(2) . ? Fe11 N24 2.088(3) . ? Fe12 O13 1.997(2) . ? Fe12 N22 2.111(2) . ? Fe12 O15 2.161(2) . ? Fe12 N29 2.197(2) . ? Fe12 O11 2.321(2) . ? N1 C2 1.341(3) . ? N1 N2 1.363(3) . ? N2 C3 1.353(4) . ? N3 C10 1.460(4) . ? N3 C4 1.461(4) . ? N3 C5 1.464(4) . ? N4 C6 1.322(4) . ? N4 C7 1.368(4) . ? N5 C8 1.357(5) . ? N5 C6 1.367(4) . ? N5 C9 1.466(5) . ? N6 C11 1.314(4) . ? N6 C12 1.381(4) . ? N7 C11 1.345(4) . ? N7 C13 1.361(5) . ? N7 C14 1.466(5) . ? N8 C21 1.476(4) . ? N8 C16 1.477(4) . ? N8 C15 1.480(4) . ? N9 C17 1.318(4) . ? N9 C18 1.385(4) . ? N10 C17 1.352(4) . ? N10 C19 1.375(5) . ? N10 C20 1.452(5) . ? N11 C22 1.318(5) . ? N11 C23 1.373(5) . ? N12 C22 1.362(4) . ? N12 C24 1.376(5) . ? N12 C25 1.468(5) . ? N21 C42 1.344(3) . ? N21 N22 1.373(3) . ? N22 C43 1.348(4) . ? N23 C50 1.456(4) . ? N23 C45 1.461(4) . ? N23 C44 1.477(4) . ? N24 C46 1.314(4) . ? N24 C47 1.387(5) . ? N25 C46 1.357(4) . ? N25 C48 1.369(5) . ? N25 C49 1.443(5) . ? N26 C51 1.327(4) . ? N26 C52 1.363(4) . ? N27 C51 1.352(4) . ? N27 C53 1.369(4) . ? N27 C54 1.463(4) . ? N28 C61 1.475(4) . ? N28 C56 1.481(4) . ? N28 C55 1.483(4) . ? N29 C57 1.325(4) . ? N29 C58 1.376(4) . ? N30 C59 1.354(4) . ? N30 C57 1.365(4) . ? N30 C60 1.462(4) . ? N31 C62 1.320(5) . ? N31 C63 1.375(7) . ? N32 C62 1.351(5) . ? N32 C64 1.395(6) . ? N32 C65 1.450(6) . ? O1A C26A 1.244(5) . ? O2A C26A 1.262(6) . ? C26A C27A 1.485(7) . ? O1B C26B 1.23(3) . ? O2B C26B 1.16(2) . ? C26B C27B 1.53(3) . ? O3 C28 1.273(4) . ? O4 C28 1.232(4) . ? O5A C30A 1.267(9) . ? O6A C30A 1.242(11) . ? C30A C31A 1.541(12) . ? O5B C30B 1.248(14) . ? O6B C30B 1.227(15) . ? C30B C31B 1.490(17) . ? O11 C66 1.283(3) . ? O12 C66 1.231(4) . ? O13 C68 1.235(4) . ? O14A C68 1.261(5) . ? O14B C68 1.313(12) . ? O15 C70 1.244(4) . ? O16 C70 1.254(4) . ? C1 C2 1.370(4) . ? C1 C3 1.396(4) . ? C2 C4 1.499(4) . ? C3 C15 1.509(4) . ? C5 C6 1.470(5) . ? C7 C8 1.342(6) . ? C10 C11 1.491(4) . ? C12 C13 1.336(6) . ? C16 C17 1.476(4) . ? C18 C19 1.335(5) . ? C21 C22 1.493(5) . ? C23 C24 1.336(6) . ? C28 C29 1.503(5) . ? C41 C42 1.384(4) . ? C41 C43 1.397(4) . ? C42 C44 1.496(4) . ? C43 C55 1.504(4) . ? C45 C46 1.495(5) . ? C47 C48 1.337(6) . ? C50 C51 1.500(5) . ? C52 C53 1.366(5) . ? C56 C57 1.490(4) . ? C58 C59 1.355(5) . ? C61 C62 1.479(5) . ? C63 C64 1.313(9) . ? C66 C67 1.496(5) . ? C68 C69 1.512(5) . ? C70 C71 1.504(5) . ? N42 C74 1.128(13) . ? C74 C75 1.409(15) . ? N43 C76 1.155(9) . ? C76 C77 1.403(9) . ? N44 C78 1.111(7) . ? C78 C79 1.409(8) . ? N45 C80 1.116(6) . ? C80 C81 1.437(7) . ? 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 N4 Fe1 N1 125.03(10) . . ? N4 Fe1 O3 144.21(9) . . ? N1 Fe1 O3 85.30(8) . . ? N4 Fe1 N6 93.74(10) . . ? N1 Fe1 N6 104.18(10) . . ? O3 Fe1 N6 96.51(9) . . ? N4 Fe1 O1A 80.34(11) . . ? N1 Fe1 O1A 87.69(10) . . ? O3 Fe1 O1A 82.77(9) . . ? N6 Fe1 O1A 168.03(10) . . ? O6B Fe2 O2A 113.2(4) . . ? O6B Fe2 N2 135.1(4) . . ? O2A Fe2 N2 110.62(12) . . ? O6B Fe2 N9 90.9(3) . . ? O2A Fe2 N9 87.12(11) . . ? N2 Fe2 N9 100.60(9) . . ? O6B Fe2 O3 88.2(3) . . ? O2A Fe2 O3 87.75(10) . . ? N2 Fe2 O3 84.26(8) . . ? N9 Fe2 O3 173.92(9) . . ? O6B Fe2 O5A 40.7(3) . . ? O2A Fe2 O5A 153.87(14) . . ? N2 Fe2 O5A 95.39(12) . . ? N9 Fe2 O5A 90.59(11) . . ? O3 Fe2 O5A 92.59(11) . . ? O6B Fe2 O1B 137.8(5) . . ? O2A Fe2 O1B 24.8(4) . . ? N2 Fe2 O1B 85.8(4) . . ? N9 Fe2 O1B 90.3(3) . . ? O3 Fe2 O1B 86.4(3) . . ? O5A Fe2 O1B 178.3(4) . . ? O6B Fe2 O6A 17.6(3) . . ? O2A Fe2 O6A 96.04(16) . . ? N2 Fe2 O6A 152.63(15) . . ? N9 Fe2 O6A 86.37(12) . . ? O3 Fe2 O6A 90.94(12) . . ? O5A Fe2 O6A 57.83(16) . . ? O1B Fe2 O6A 120.8(4) . . ? N21 Fe11 O11 86.58(9) . . ? N21 Fe11 N26 114.14(10) . . ? O11 Fe11 N26 136.01(9) . . ? N21 Fe11 N24 117.84(10) . . ? O11 Fe11 N24 102.48(9) . . ? N26 Fe11 N24 100.81(11) . . ? O13 Fe12 N22 121.00(10) . . ? O13 Fe12 O15 143.81(10) . . ? N22 Fe12 O15 92.41(9) . . ? O13 Fe12 N29 91.68(10) . . ? N22 Fe12 N29 98.89(9) . . ? O15 Fe12 N29 96.75(10) . . ? O13 Fe12 O11 87.82(9) . . ? N22 Fe12 O11 84.87(8) . . ? O15 Fe12 O11 81.31(9) . . ? N29 Fe12 O11 175.87(8) . . ? C2 N1 N2 108.2(2) . . ? C2 N1 Fe1 126.14(18) . . ? N2 N1 Fe1 125.47(17) . . ? C3 N2 N1 107.3(2) . . ? C3 N2 Fe2 134.01(19) . . ? N1 N2 Fe2 116.72(17) . . ? C10 N3 C4 111.3(2) . . ? C10 N3 C5 114.1(2) . . ? C4 N3 C5 114.7(2) . . ? C6 N4 C7 106.6(3) . . ? C6 N4 Fe1 124.5(2) . . ? C7 N4 Fe1 128.9(2) . . ? C8 N5 C6 107.3(3) . . ? C8 N5 C9 127.0(3) . . ? C6 N5 C9 125.7(3) . . ? C11 N6 C12 104.9(3) . . ? C11 N6 Fe1 122.7(2) . . ? C12 N6 Fe1 131.8(2) . . ? C11 N7 C13 107.0(3) . . ? C11 N7 C14 125.9(3) . . ? C13 N7 C14 127.0(3) . . ? C21 N8 C16 110.8(2) . . ? C21 N8 C15 112.8(2) . . ? C16 N8 C15 111.0(2) . . ? C17 N9 C18 104.9(3) . . ? C17 N9 Fe2 130.5(2) . . ? C18 N9 Fe2 124.3(2) . . ? C17 N10 C19 106.6(3) . . ? C17 N10 C20 126.2(3) . . ? C19 N10 C20 127.2(3) . . ? C22 N11 C23 105.3(3) . . ? C22 N12 C24 107.0(3) . . ? C22 N12 C25 125.8(3) . . ? C24 N12 C25 127.2(3) . . ? C42 N21 N22 108.4(2) . . ? C42 N21 Fe11 125.43(19) . . ? N22 N21 Fe11 125.89(17) . . ? C43 N22 N21 107.3(2) . . ? C43 N22 Fe12 136.1(2) . . ? N21 N22 Fe12 116.45(16) . . ? C50 N23 C45 114.0(3) . . ? C50 N23 C44 112.9(3) . . ? C45 N23 C44 111.8(3) . . ? C46 N24 C47 105.5(3) . . ? C46 N24 Fe11 122.4(2) . . ? C47 N24 Fe11 132.1(2) . . ? C46 N25 C48 106.8(3) . . ? C46 N25 C49 126.7(3) . . ? C48 N25 C49 126.4(3) . . ? C51 N26 C52 106.5(3) . . ? C51 N26 Fe11 118.9(2) . . ? C52 N26 Fe11 134.6(2) . . ? C51 N27 C53 107.4(3) . . ? C51 N27 C54 126.0(3) . . ? C53 N27 C54 126.6(3) . . ? C61 N28 C56 111.2(2) . . ? C61 N28 C55 112.1(2) . . ? C56 N28 C55 111.0(2) . . ? C57 N29 C58 105.7(3) . . ? C57 N29 Fe12 133.2(2) . . ? C58 N29 Fe12 120.5(2) . . ? C59 N30 C57 107.6(3) . . ? C59 N30 C60 125.3(3) . . ? C57 N30 C60 126.9(3) . . ? C62 N31 C63 104.5(5) . . ? C62 N32 C64 105.5(5) . . ? C62 N32 C65 126.6(4) . . ? C64 N32 C65 127.7(4) . . ? C26A O1A Fe1 137.1(3) . . ? C26A O2A Fe2 130.0(3) . . ? O1A C26A O2A 125.2(4) . . ? O1A C26A C27A 114.7(4) . . ? O2A C26A C27A 120.1(4) . . ? C26B O1B Fe2 102.0(14) . . ? O2B C26B O1B 116(2) . . ? O2B C26B C27B 123.3(19) . . ? O1B C26B C27B 118.4(18) . . ? C28 O3 Fe1 97.0(2) . . ? C28 O3 Fe2 135.1(2) . . ? Fe1 O3 Fe2 109.83(9) . . ? C30A O5A Fe2 90.9(5) . . ? C30A O6A Fe2 88.8(5) . . ? O6A C30A O5A 122.3(8) . . ? O6A C30A C31A 120.1(7) . . ? O5A C30A C31A 117.1(8) . . ? C30B O6B Fe2 117.7(9) . . ? O6B C30B O5B 126.8(11) . . ? O6B C30B C31B 110.6(11) . . ? O5B C30B C31B 120.7(11) . . ? C66 O11 Fe11 103.90(19) . . ? C66 O11 Fe12 125.52(18) . . ? Fe11 O11 Fe12 106.75(8) . . ? C68 O13 Fe12 122.5(2) . . ? C70 O15 Fe12 97.7(2) . . ? C2 C1 C3 104.4(2) . . ? N1 C2 C1 110.4(2) . . ? N1 C2 C4 118.4(2) . . ? C1 C2 C4 130.9(3) . . ? N2 C3 C1 109.6(2) . . ? N2 C3 C15 121.4(2) . . ? C1 C3 C15 128.4(3) . . ? N3 C4 C2 109.9(2) . . ? N3 C5 C6 111.6(3) . . ? N4 C6 N5 109.6(3) . . ? N4 C6 C5 126.0(3) . . ? N5 C6 C5 124.4(3) . . ? C8 C7 N4 109.5(4) . . ? C7 C8 N5 107.0(3) . . ? N3 C10 C11 110.4(2) . . ? N6 C11 N7 111.4(3) . . ? N6 C11 C10 124.2(3) . . ? N7 C11 C10 124.3(3) . . ? C13 C12 N6 110.0(3) . . ? C12 C13 N7 106.6(3) . . ? N8 C15 C3 113.4(2) . . ? C17 C16 N8 109.9(2) . . ? N9 C17 N10 111.6(3) . . ? N9 C17 C16 126.7(3) . . ? N10 C17 C16 121.6(3) . . ? C19 C18 N9 110.2(3) . . ? C18 C19 N10 106.7(3) . . ? N8 C21 C22 110.0(3) . . ? N11 C22 N12 110.8(3) . . ? N11 C22 C21 125.7(3) . . ? N12 C22 C21 123.5(3) . . ? C24 C23 N11 111.1(4) . . ? C23 C24 N12 105.9(3) . . ? O4 C28 O3 120.3(3) . . ? O4 C28 C29 121.2(3) . . ? O3 C28 C29 118.5(3) . . ? C42 C41 C43 104.3(2) . . ? N21 C42 C41 109.9(3) . . ? N21 C42 C44 118.7(2) . . ? C41 C42 C44 130.9(3) . . ? N22 C43 C41 110.0(3) . . ? N22 C43 C55 121.3(3) . . ? C41 C43 C55 128.6(3) . . ? N23 C44 C42 110.2(2) . . ? N23 C45 C46 109.6(3) . . ? N24 C46 N25 111.1(3) . . ? N24 C46 C45 124.0(3) . . ? N25 C46 C45 124.8(3) . . ? C48 C47 N24 109.7(4) . . ? C47 C48 N25 106.9(4) . . ? N23 C50 C51 109.1(3) . . ? N26 C51 N27 110.5(3) . . ? N26 C51 C50 123.5(3) . . ? N27 C51 C50 126.0(3) . . ? N26 C52 C53 109.3(3) . . ? C52 C53 N27 106.3(3) . . ? N28 C55 C43 115.1(2) . . ? N28 C56 C57 110.5(2) . . ? N29 C57 N30 110.3(3) . . ? N29 C57 C56 126.6(3) . . ? N30 C57 C56 123.0(3) . . ? C59 C58 N29 109.8(3) . . ? N30 C59 C58 106.5(3) . . ? N28 C61 C62 110.8(3) . . ? N31 C62 N32 111.9(4) . . ? N31 C62 C61 124.9(4) . . ? N32 C62 C61 123.2(4) . . ? C64 C63 N31 111.4(5) . . ? C63 C64 N32 106.6(5) . . ? O12 C66 O11 121.0(3) . . ? O12 C66 C67 121.9(3) . . ? O11 C66 C67 117.1(3) . . ? O13 C68 O14A 123.2(4) . . ? O13 C68 O14B 116.8(6) . . ? O14A C68 O14B 48.3(5) . . ? O13 C68 C69 117.1(3) . . ? O14A C68 C69 118.4(4) . . ? O14B C68 C69 112.4(6) . . ? O15 C70 O16 120.8(3) . . ? O15 C70 C71 119.6(3) . . ? O16 C70 C71 119.6(3) . . ? N42 C74 C75 172.9(13) . . ? N43 C76 C77 176.7(8) . . ? N44 C78 C79 178.2(7) . . ? N45 C80 C81 176.5(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.597 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.048 data_1-bb70m2at271K-one-crystal _database_code_depnum_ccdc_archive 'CCDC 831484' #TrackingRef '- pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H42 Fe2 N12 O6, 2(C2 H3 N)' _chemical_formula_sum 'C35 H48 Fe2 N14 O6' _chemical_formula_weight 872.57 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 'P 21 21 21' 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 16.4147(4) _cell_length_b 19.0401(5) _cell_length_c 26.6275(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8322.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 271(2) _cell_measurement_reflns_used 96150 _cell_measurement_theta_min 1.31 _cell_measurement_theta_max 25.71 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7807 _exptl_absorpt_correction_T_max 0.8668 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 271(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 96150 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.71 _reflns_number_total 15791 _reflns_number_gt 13086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0547P)^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 0.010(10) _refine_ls_number_reflns 15791 _refine_ls_number_parameters 1032 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.77214(3) 0.41537(2) 0.612756(18) 0.04444(13) Uani 1 1 d . . . Fe2 Fe 0.90983(3) 0.28630(2) 0.561898(19) 0.04115(12) Uani 1 1 d . . . Fe11 Fe 0.25024(3) 0.59836(3) 0.592171(17) 0.04358(12) Uani 1 1 d . . . Fe12 Fe 0.43216(3) 0.68916(2) 0.562966(17) 0.03692(11) Uani 1 1 d . . . N1 N 0.79738(15) 0.40552(13) 0.53555(9) 0.0340(6) Uani 1 1 d . A . N2 N 0.83743(16) 0.35014(14) 0.51369(10) 0.0366(6) Uani 1 1 d . A . N3 N 0.68576(15) 0.50848(13) 0.55907(11) 0.0400(6) Uani 1 1 d . . . N4 N 0.76629(19) 0.51122(15) 0.65182(10) 0.0478(7) Uani 1 1 d . A . N5 N 0.7362(2) 0.62093(18) 0.66931(13) 0.0642(9) Uani 1 1 d . A . N6 N 0.64214(19) 0.39524(15) 0.61885(11) 0.0490(7) Uani 1 1 d . A . N7 N 0.51415(19) 0.39367(18) 0.59467(13) 0.0556(8) Uani 1 1 d . A . N8 N 0.95903(17) 0.34603(14) 0.41023(10) 0.0412(6) Uani 1 1 d . . . N9 N 1.01554(18) 0.26563(15) 0.51294(12) 0.0474(7) Uani 1 1 d . A . N10 N 1.11696(18) 0.27435(17) 0.45877(13) 0.0533(8) Uani 1 1 d . A . N11 N 1.0744(3) 0.4725(2) 0.35856(15) 0.0770(12) Uani 1 1 d . . . N12 N 1.0483(2) 0.38381(18) 0.30762(12) 0.0587(9) Uani 1 1 d . . . N21 N 0.28631(16) 0.61746(15) 0.51909(9) 0.0390(6) Uani 1 1 d . . . N22 N 0.35520(16) 0.65405(14) 0.50475(9) 0.0352(6) Uani 1 1 d . . . N23 N 0.15459(18) 0.53407(15) 0.53216(11) 0.0458(7) Uani 1 1 d . . . N24 N 0.13092(18) 0.62480(17) 0.61197(12) 0.0513(7) Uani 1 1 d . . . N25 N -0.0033(2) 0.62173(19) 0.60962(14) 0.0603(9) Uani 1 1 d . . . N26 N 0.25278(18) 0.49285(15) 0.61253(10) 0.0456(6) Uani 1 1 d . . . N27 N 0.23000(18) 0.38009(15) 0.60025(11) 0.0496(7) Uani 1 1 d . . . N28 N 0.48317(17) 0.64820(14) 0.40612(10) 0.0401(6) Uani 1 1 d . . . N29 N 0.54855(17) 0.68890(16) 0.52187(11) 0.0451(7) Uani 1 1 d . . . N30 N 0.64739(17) 0.68401(16) 0.46599(11) 0.0450(7) Uani 1 1 d . . . N31 N 0.3477(3) 0.6511(3) 0.31179(14) 0.0932(15) Uani 1 1 d . . . N32 N 0.4755(3) 0.6623(2) 0.28815(13) 0.0773(12) Uani 1 1 d . . . O1A O 0.9068(2) 0.43638(19) 0.62410(13) 0.0599(12) Uiso 0.762(6) 1 d P A 1 O2A O 0.9842(2) 0.3447(2) 0.60416(15) 0.0552(11) Uiso 0.762(6) 1 d P A 1 C26A C 0.9701(3) 0.4012(3) 0.62808(16) 0.0377(11) Uiso 0.762(6) 1 d P A 1 C27A C 1.0305(5) 0.4293(4) 0.6640(3) 0.056(2) Uiso 0.762(6) 1 d P A 1 H27A H 1.0776 0.3994 0.6645 0.080 Uiso 0.762(6) 1 calc PR A 1 H27B H 1.0069 0.4310 0.6970 0.080 Uiso 0.762(6) 1 calc PR A 1 H27C H 1.0462 0.4758 0.6540 0.080 Uiso 0.762(6) 1 calc PR A 1 O1B O 0.9663(7) 0.3883(7) 0.5889(5) 0.060(4) Uiso 0.238(6) 1 d P A 2 O2B O 1.0025(9) 0.3074(8) 0.6363(5) 0.078(5) Uiso 0.238(6) 1 d P A 2 C26B C 0.9965(11) 0.3694(11) 0.6273(7) 0.048(4) Uiso 0.238(6) 1 d P A 2 C27B C 1.0471(11) 0.4233(9) 0.6577(7) 0.027(4) Uiso 0.238(6) 1 d P A 2 H27D H 1.0673 0.4014 0.6877 0.080 Uiso 0.238(6) 1 calc PR A 2 H27E H 1.0132 0.4625 0.6666 0.080 Uiso 0.238(6) 1 calc PR A 2 H27F H 1.0920 0.4394 0.6377 0.080 Uiso 0.238(6) 1 calc PR A 2 O3 O 0.81119(14) 0.30747(13) 0.61824(9) 0.0469(6) Uani 1 1 d . A . O4 O 0.7848(2) 0.35209(17) 0.69141(10) 0.0746(9) Uani 1 1 d . A . O5A O 0.8529(3) 0.1842(3) 0.53720(19) 0.0533(18) Uiso 0.564(11) 1 d P A 3 O6A O 0.9404(4) 0.1807(3) 0.5998(2) 0.0606(18) Uiso 0.564(11) 1 d P A 3 C30A C 0.8897(6) 0.1513(6) 0.5722(4) 0.062(2) Uiso 0.564(11) 1 d P A 3 C31A C 0.8810(7) 0.0702(5) 0.5729(4) 0.072(3) Uiso 0.564(11) 1 d P A 3 H31A H 0.8400 0.0562 0.5493 0.080 Uiso 0.564(11) 1 calc PR A 3 H31B H 0.8655 0.0551 0.6060 0.080 Uiso 0.564(11) 1 calc PR A 3 H31C H 0.9321 0.0491 0.5640 0.080 Uiso 0.564(11) 1 calc PR A 3 O5B O 0.8252(5) 0.1561(5) 0.5187(3) 0.077(3) Uiso 0.436(11) 1 d P A 4 O6B O 0.9046(6) 0.1856(5) 0.5817(4) 0.080(3) Uiso 0.436(11) 1 d P A 4 C30B C 0.8656(7) 0.1438(6) 0.5563(4) 0.052(3) Uiso 0.436(11) 1 d P A 4 C31B C 0.8548(10) 0.0760(7) 0.5842(5) 0.079(4) Uiso 0.436(11) 1 d P A 4 H31D H 0.8243 0.0437 0.5639 0.080 Uiso 0.436(11) 1 calc PR A 4 H31E H 0.8259 0.0847 0.6150 0.080 Uiso 0.436(11) 1 calc PR A 4 H31F H 0.9072 0.0563 0.5917 0.080 Uiso 0.436(11) 1 calc PR A 4 O11 O 0.31460(13) 0.68826(13) 0.61186(8) 0.0445(5) Uani 1 1 d . . . O12 O 0.2866(2) 0.63811(17) 0.68357(11) 0.0700(8) Uani 1 1 d . . . O13 O 0.44272(19) 0.79108(13) 0.57883(11) 0.0650(7) Uani 1 1 d . B . O14A O 0.3753(3) 0.8254(3) 0.51229(19) 0.0862(14) Uiso 0.736(6) 1 d P B 5 O14B O 0.4396(9) 0.8324(7) 0.5027(5) 0.0862(14) Uiso 0.264(6) 1 d P B 6 O15 O 0.44310(19) 0.58500(15) 0.59447(10) 0.0643(7) Uani 1 1 d . . . O16 O 0.49915(18) 0.66333(17) 0.64212(13) 0.0719(9) Uani 1 1 d . . . C1 C 0.79373(19) 0.42293(18) 0.45287(12) 0.0393(7) Uani 1 1 d . A . H1 H 0.7831 0.4426 0.4216 0.080 Uiso 1 1 calc R . . C2 C 0.77268(18) 0.44883(16) 0.49929(12) 0.0340(7) Uani 1 1 d . . . C3 C 0.83464(19) 0.36049(17) 0.46332(12) 0.0350(7) Uani 1 1 d . . . C4 C 0.7356(2) 0.51757(18) 0.51386(13) 0.0448(8) Uani 1 1 d . A . H4A H 0.7783 0.5516 0.5203 0.080 Uiso 1 1 calc R . . H4B H 0.7021 0.5351 0.4866 0.080 Uiso 1 1 calc R . . C5 C 0.6774(2) 0.57189(19) 0.59005(15) 0.0520(9) Uani 1 1 d . A . H5A H 0.6947 0.6124 0.5708 0.080 Uiso 1 1 calc R . . H5B H 0.6205 0.5784 0.5988 0.080 Uiso 1 1 calc R . . C6 C 0.7258(2) 0.56744(18) 0.63601(14) 0.0464(8) Uani 1 1 d . . . C7 C 0.8042(3) 0.5305(3) 0.69562(16) 0.0742(13) Uani 1 1 d . . . H7 H 0.8380 0.5018 0.7147 0.080 Uiso 1 1 calc R A . C8 C 0.7848(3) 0.5969(3) 0.70660(17) 0.0849(15) Uani 1 1 d . A . H8 H 0.8017 0.6219 0.7347 0.080 Uiso 1 1 calc R . . C9 C 0.7008(3) 0.6911(3) 0.6649(2) 0.0832(15) Uani 1 1 d . . . H9A H 0.7278 0.7164 0.6385 0.080 Uiso 1 1 calc R A . H9B H 0.7075 0.7158 0.6961 0.080 Uiso 1 1 calc R . . H9C H 0.6438 0.6872 0.6573 0.080 Uiso 1 1 calc R . . C10 C 0.6091(2) 0.47344(19) 0.54759(13) 0.0430(8) Uani 1 1 d . A . H10A H 0.6134 0.4498 0.5155 0.080 Uiso 1 1 calc R . . H10B H 0.5659 0.5080 0.5452 0.080 Uiso 1 1 calc R . . C11 C 0.5888(2) 0.42169(17) 0.58713(13) 0.0429(8) Uani 1 1 d . . . C12 C 0.5983(3) 0.3488(2) 0.64815(17) 0.0639(11) Uani 1 1 d . . . H12 H 0.6196 0.3227 0.6746 0.080 Uiso 1 1 calc R A . C13 C 0.5208(3) 0.3471(2) 0.63298(18) 0.0698(12) Uani 1 1 d . A . H13 H 0.4794 0.3192 0.6461 0.080 Uiso 1 1 calc R . . C14 C 0.4419(2) 0.4085(2) 0.56423(19) 0.0701(11) Uani 1 1 d . . . H14A H 0.4236 0.4555 0.5707 0.080 Uiso 1 1 calc R A . H14B H 0.3994 0.3759 0.5727 0.080 Uiso 1 1 calc R . . H14C H 0.4552 0.4038 0.5293 0.080 Uiso 1 1 calc R . . C15 C 0.8817(2) 0.31408(18) 0.42771(12) 0.0415(7) Uani 1 1 d . A . H15A H 0.8938 0.2700 0.4444 0.080 Uiso 1 1 calc R . . H15B H 0.8479 0.3038 0.3988 0.080 Uiso 1 1 calc R . . C16 C 1.0115(2) 0.36630(19) 0.45288(13) 0.0443(8) Uani 1 1 d . A . H16A H 0.9795 0.3918 0.4775 0.080 Uiso 1 1 calc R . . H16B H 1.0546 0.3970 0.4412 0.080 Uiso 1 1 calc R . . C17 C 1.0474(2) 0.30316(19) 0.47641(13) 0.0435(8) Uani 1 1 d . . . C18 C 1.0687(2) 0.2096(2) 0.51921(16) 0.0563(10) Uani 1 1 d . . . H18 H 1.0626 0.1738 0.5427 0.080 Uiso 1 1 calc R A . C19 C 1.1300(2) 0.2148(2) 0.48645(17) 0.0604(11) Uani 1 1 d . A . H19 H 1.1734 0.1837 0.4831 0.080 Uiso 1 1 calc R . . C20 C 1.1665(2) 0.3006(3) 0.41768(16) 0.0685(12) Uani 1 1 d . . . H20A H 1.1335 0.3053 0.3881 0.080 Uiso 1 1 calc R A . H20B H 1.2101 0.2682 0.4111 0.080 Uiso 1 1 calc R . . H20C H 1.1888 0.3455 0.4266 0.080 Uiso 1 1 calc R . . C21 C 0.9462(2) 0.4061(2) 0.37627(14) 0.0518(9) Uani 1 1 d . . . H21A H 0.9299 0.4469 0.3956 0.080 Uiso 1 1 calc R . . H21B H 0.9028 0.3953 0.3528 0.080 Uiso 1 1 calc R . . C22 C 1.0226(3) 0.4221(2) 0.34804(15) 0.0563(10) Uani 1 1 d . . . C23 C 1.1366(3) 0.4651(3) 0.3245(2) 0.0871(16) Uani 1 1 d . . . H23 H 1.1828 0.4933 0.3235 0.080 Uiso 1 1 calc R . . C24 C 1.1218(3) 0.4122(3) 0.29299(18) 0.0783(14) Uani 1 1 d . . . H24 H 1.1545 0.3975 0.2665 0.080 Uiso 1 1 calc R . . C25 C 1.0059(3) 0.3234(3) 0.28566(18) 0.0802(14) Uani 1 1 d . . . H25A H 1.0323 0.2808 0.2960 0.080 Uiso 1 1 calc R . . H25B H 1.0073 0.3268 0.2497 0.080 Uiso 1 1 calc R . . H25C H 0.9503 0.3230 0.2969 0.080 Uiso 1 1 calc R . . C28 C 0.8057(2) 0.3014(2) 0.66567(13) 0.0463(8) Uani 1 1 d . . . C29 C 0.8227(3) 0.2316(2) 0.68909(16) 0.0673(12) Uani 1 1 d . A . H29A H 0.8108 0.2337 0.7244 0.080 Uiso 1 1 calc R . . H29B H 0.8790 0.2197 0.6844 0.080 Uiso 1 1 calc R . . H29C H 0.7891 0.1965 0.6736 0.080 Uiso 1 1 calc R . . C41 C 0.2816(2) 0.62895(18) 0.43569(12) 0.0414(7) Uani 1 1 d . . . H41 H 0.2647 0.6258 0.4024 0.080 Uiso 1 1 calc R . . C42 C 0.2428(2) 0.60312(17) 0.47760(11) 0.0404(7) Uani 1 1 d . . . C43 C 0.3523(2) 0.66105(17) 0.45435(11) 0.0360(7) Uani 1 1 d . . . C44 C 0.1600(2) 0.5716(2) 0.48360(13) 0.0504(9) Uani 1 1 d . . . H44A H 0.1191 0.6083 0.4823 0.080 Uiso 1 1 calc R . . H44B H 0.1496 0.5390 0.4563 0.080 Uiso 1 1 calc R . . C45 C 0.0722(2) 0.5376(2) 0.55303(15) 0.0556(10) Uani 1 1 d . . . H45A H 0.0587 0.4933 0.5690 0.080 Uiso 1 1 calc R . . H45B H 0.0333 0.5459 0.5263 0.080 Uiso 1 1 calc R . . C46 C 0.0672(2) 0.5953(2) 0.59053(14) 0.0501(9) Uani 1 1 d . . . C47 C 0.0995(3) 0.6711(2) 0.64724(17) 0.0672(11) Uani 1 1 d . . . H47 H 0.1305 0.6990 0.6686 0.080 Uiso 1 1 calc R . . C48 C 0.0183(3) 0.6697(3) 0.64586(18) 0.0689(12) Uani 1 1 d . . . H48 H -0.0170 0.6961 0.6656 0.080 Uiso 1 1 calc R . . C49 C -0.0844(2) 0.6034(3) 0.5949(2) 0.0808(14) Uani 1 1 d . . . H49A H -0.0960 0.6235 0.5627 0.080 Uiso 1 1 calc R . . H49B H -0.1223 0.6212 0.6192 0.080 Uiso 1 1 calc R . . H49C H -0.0891 0.5532 0.5930 0.080 Uiso 1 1 calc R . . C50 C 0.1884(3) 0.4640(2) 0.53031(16) 0.0593(10) Uani 1 1 d . . . H50A H 0.2313 0.4619 0.5053 0.080 Uiso 1 1 calc R . . H50B H 0.1464 0.4306 0.5210 0.080 Uiso 1 1 calc R . . C51 C 0.2223(2) 0.44555(18) 0.58107(13) 0.0446(8) Uani 1 1 d . . . C52 C 0.2812(2) 0.4564(2) 0.65268(14) 0.0526(9) Uani 1 1 d . . . H52 H 0.3063 0.4762 0.6806 0.080 Uiso 1 1 calc R . . C53 C 0.2674(2) 0.3865(2) 0.64608(14) 0.0547(9) Uani 1 1 d . . . H53 H 0.2807 0.3505 0.6682 0.080 Uiso 1 1 calc R . . C54 C 0.2031(3) 0.3149(2) 0.57664(18) 0.0691(12) Uani 1 1 d . . . H54A H 0.1467 0.3188 0.5677 0.080 Uiso 1 1 calc R . . H54B H 0.2102 0.2766 0.5997 0.080 Uiso 1 1 calc R . . H54C H 0.2349 0.3064 0.5470 0.080 Uiso 1 1 calc R . . C55 C 0.4201(2) 0.69604(16) 0.42586(12) 0.0394(7) Uani 1 1 d . . . H55A H 0.3966 0.7217 0.3979 0.080 Uiso 1 1 calc R . . H55B H 0.4461 0.7300 0.4478 0.080 Uiso 1 1 calc R . . C56 C 0.5248(2) 0.61001(17) 0.44734(12) 0.0408(7) Uani 1 1 d . . . H56A H 0.5612 0.5750 0.4333 0.080 Uiso 1 1 calc R . . H56B H 0.4847 0.5860 0.4679 0.080 Uiso 1 1 calc R . . C57 C 0.5723(2) 0.65996(18) 0.47914(12) 0.0413(8) Uani 1 1 d . . . C58 C 0.6108(2) 0.7331(2) 0.53570(15) 0.0515(9) Uani 1 1 d . . . H58 H 0.6109 0.7610 0.5643 0.080 Uiso 1 1 calc R . . C59 C 0.6714(2) 0.73006(19) 0.50182(15) 0.0503(9) Uani 1 1 d . . . H59 H 0.7203 0.7547 0.5028 0.080 Uiso 1 1 calc R . . C60 C 0.6926(2) 0.6681(2) 0.41997(15) 0.0597(11) Uani 1 1 d . . . H60A H 0.7418 0.6955 0.4191 0.080 Uiso 1 1 calc R . . H60B H 0.6597 0.6795 0.3913 0.080 Uiso 1 1 calc R . . H60C H 0.7061 0.6191 0.4193 0.080 Uiso 1 1 calc R . . C61 C 0.4506(2) 0.59862(19) 0.36856(13) 0.0491(9) Uani 1 1 d . . . H61A H 0.4048 0.5733 0.3827 0.080 Uiso 1 1 calc R . . H61B H 0.4923 0.5647 0.3597 0.080 Uiso 1 1 calc R . . C62 C 0.4241(3) 0.6372(2) 0.32296(14) 0.0591(11) Uani 1 1 d . . . C63 C 0.3509(6) 0.6892(4) 0.2684(2) 0.117(3) Uani 1 1 d . . . H63 H 0.3056 0.7071 0.2517 0.080 Uiso 1 1 calc R . . C64 C 0.4269(6) 0.6972(3) 0.25333(18) 0.107(2) Uani 1 1 d . . . H64 H 0.4446 0.7214 0.2250 0.080 Uiso 1 1 calc R . . C65 C 0.5634(4) 0.6525(4) 0.2867(2) 0.106(2) Uani 1 1 d . . . H65A H 0.5875 0.6734 0.3160 0.080 Uiso 1 1 calc R . . H65B H 0.5851 0.6743 0.2571 0.080 Uiso 1 1 calc R . . H65C H 0.5756 0.6032 0.2861 0.080 Uiso 1 1 calc R . . C66 C 0.3124(2) 0.6887(2) 0.65996(13) 0.0422(8) Uani 1 1 d . . . C67 C 0.3399(3) 0.7545(2) 0.68564(15) 0.0614(11) Uani 1 1 d . . . H67A H 0.3390 0.7476 0.7214 0.080 Uiso 1 1 calc R . . H67B H 0.3040 0.7924 0.6769 0.080 Uiso 1 1 calc R . . H67C H 0.3943 0.7657 0.6751 0.080 Uiso 1 1 calc R . . C68 C 0.4178(3) 0.8375(2) 0.55075(16) 0.0634(11) Uani 1 1 d . . . C69 C 0.4230(3) 0.91211(19) 0.56935(17) 0.0628(10) Uani 1 1 d . B . H69A H 0.4093 0.9437 0.5426 0.080 Uiso 1 1 calc R . . H69B H 0.4775 0.9216 0.5806 0.080 Uiso 1 1 calc R . . H69C H 0.3857 0.9186 0.5967 0.080 Uiso 1 1 calc R . . C70 C 0.4768(2) 0.6012(2) 0.63415(16) 0.0530(9) Uani 1 1 d . . . C71 C 0.4930(3) 0.5458(2) 0.67334(15) 0.0651(11) Uani 1 1 d . . . H71A H 0.5445 0.5549 0.6891 0.080 Uiso 1 1 calc R . . H71B H 0.4942 0.5004 0.6577 0.080 Uiso 1 1 calc R . . H71C H 0.4505 0.5469 0.6981 0.080 Uiso 1 1 calc R . . N42 N 0.7361(7) 0.3184(6) 0.3238(3) 0.172(4) Uani 1 1 d . . . C74 C 0.6777(7) 0.3432(8) 0.3381(4) 0.164(6) Uani 1 1 d . . . C75 C 0.6145(7) 0.3844(9) 0.3565(4) 0.237(8) Uani 1 1 d . . . H75A H 0.6309 0.4059 0.3875 0.356 Uiso 1 1 calc R . . H75B H 0.5675 0.3554 0.3623 0.356 Uiso 1 1 calc R . . H75C H 0.6013 0.4201 0.3324 0.356 Uiso 1 1 calc R . . N43 N 0.7536(6) 0.4668(4) 0.8352(2) 0.155(3) Uani 1 1 d . . . C76 C 0.7038(6) 0.4601(4) 0.8052(3) 0.115(3) Uani 1 1 d . . . C77 C 0.6469(6) 0.4488(6) 0.7675(3) 0.155(3) Uani 1 1 d . . . H77A H 0.6694 0.4178 0.7427 0.233 Uiso 1 1 calc R . . H77B H 0.6330 0.4928 0.7521 0.233 Uiso 1 1 calc R . . H77C H 0.5988 0.4280 0.7817 0.233 Uiso 1 1 calc R . . N44 N 0.0043(5) 0.5425(5) 0.7741(3) 0.176(4) Uani 1 1 d . . . C78 C 0.0704(5) 0.5414(4) 0.7654(2) 0.1004(19) Uani 1 1 d . . . C79 C 0.1539(4) 0.5372(4) 0.7543(3) 0.114(2) Uani 1 1 d . . . H79A H 0.1792 0.5036 0.7762 0.172 Uiso 1 1 calc R . . H79B H 0.1786 0.5824 0.7591 0.172 Uiso 1 1 calc R . . H79C H 0.1609 0.5228 0.7200 0.172 Uiso 1 1 calc R . . N45 N 0.6011(5) 0.8290(5) 0.7591(2) 0.159(3) Uani 1 1 d . . . C80 C 0.5900(4) 0.8375(3) 0.7184(2) 0.0935(17) Uani 1 1 d . . . C81 C 0.5804(5) 0.8473(3) 0.6652(2) 0.111(2) Uani 1 1 d . . . H81A H 0.6312 0.8382 0.6487 0.167 Uiso 1 1 calc R . . H81B H 0.5637 0.8947 0.6586 0.167 Uiso 1 1 calc R . . H81C H 0.5397 0.8154 0.6528 0.167 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 0.0572(3) 0.0343(2) 0.0419(2) -0.0027(2) 0.0050(2) 0.0032(2) Fe2 0.0359(2) 0.0352(2) 0.0523(3) 0.0056(2) -0.0027(2) 0.00432(19) Fe11 0.0506(3) 0.0417(3) 0.0384(2) 0.0001(2) 0.0031(2) -0.0124(2) Fe12 0.0346(2) 0.0361(2) 0.0401(2) -0.0036(2) -0.0022(2) -0.00361(19) N1 0.0336(14) 0.0307(13) 0.0378(13) 0.0025(11) 0.0033(11) 0.0057(11) N2 0.0334(14) 0.0341(14) 0.0425(15) 0.0004(11) 0.0015(12) 0.0055(11) N3 0.0345(14) 0.0350(14) 0.0505(16) -0.0091(13) 0.0020(13) 0.0022(11) N4 0.0506(19) 0.0471(17) 0.0456(16) -0.0080(13) -0.0031(14) -0.0010(14) N5 0.067(2) 0.0523(19) 0.073(2) -0.0303(16) -0.0047(19) 0.0054(17) N6 0.0529(18) 0.0412(16) 0.0528(17) -0.0019(14) 0.0058(15) -0.0028(14) N7 0.0435(18) 0.056(2) 0.068(2) -0.0172(17) 0.0067(15) -0.0113(15) N8 0.0394(16) 0.0392(15) 0.0451(15) -0.0051(13) 0.0067(13) 0.0033(12) N9 0.0405(17) 0.0374(16) 0.064(2) -0.0064(14) -0.0034(15) 0.0089(13) N10 0.0348(16) 0.056(2) 0.069(2) -0.0226(16) -0.0022(14) 0.0076(14) N11 0.080(3) 0.067(2) 0.084(3) -0.011(2) 0.037(2) -0.022(2) N12 0.071(2) 0.055(2) 0.0504(18) 0.0033(15) 0.0202(16) 0.0083(17) N21 0.0332(14) 0.0483(16) 0.0356(14) -0.0008(12) 0.0002(12) -0.0095(12) N22 0.0341(15) 0.0364(14) 0.0353(14) 0.0002(11) 0.0009(11) -0.0055(11) N23 0.0449(17) 0.0484(17) 0.0442(16) 0.0094(13) -0.0055(13) -0.0134(14) N24 0.0421(17) 0.0542(18) 0.0577(18) -0.0009(15) -0.0016(15) -0.0051(14) N25 0.0455(19) 0.060(2) 0.075(2) 0.0249(18) 0.0009(17) 0.0042(15) N26 0.0425(16) 0.0486(16) 0.0457(15) 0.0005(13) -0.0021(14) -0.0061(14) N27 0.0449(17) 0.0418(15) 0.0621(19) 0.0013(13) -0.0043(15) -0.0043(13) N28 0.0454(16) 0.0369(15) 0.0381(14) -0.0025(12) 0.0040(13) -0.0008(12) N29 0.0358(15) 0.0477(16) 0.0519(17) -0.0026(14) 0.0010(13) -0.0041(13) N30 0.0365(16) 0.0494(17) 0.0491(16) 0.0032(14) 0.0044(13) -0.0046(13) N31 0.107(4) 0.125(4) 0.047(2) -0.020(2) -0.011(2) 0.053(3) N32 0.123(4) 0.062(2) 0.046(2) -0.0031(17) 0.006(2) -0.008(2) O3 0.0416(13) 0.0551(15) 0.0441(13) 0.0130(11) 0.0007(10) -0.0007(11) O4 0.102(3) 0.069(2) 0.0524(16) -0.0083(15) -0.0110(16) 0.0148(18) O11 0.0380(12) 0.0534(14) 0.0420(13) -0.0076(11) -0.0064(10) -0.0016(11) O12 0.077(2) 0.0640(19) 0.0685(18) 0.0169(15) -0.0065(16) -0.0137(16) O13 0.080(2) 0.0380(14) 0.0764(19) 0.0018(13) 0.0117(15) 0.0022(13) O15 0.084(2) 0.0594(16) 0.0491(15) -0.0003(13) -0.0010(15) 0.0186(15) O16 0.0560(18) 0.058(2) 0.102(2) 0.0074(17) 0.0072(16) 0.0085(14) C1 0.0339(17) 0.0452(18) 0.0388(17) 0.0073(14) -0.0007(13) 0.0022(14) C2 0.0232(16) 0.0322(15) 0.0465(17) 0.0030(13) 0.0039(13) 0.0004(12) C3 0.0283(16) 0.0381(17) 0.0386(17) -0.0002(14) 0.0000(13) 0.0010(13) C4 0.0383(19) 0.0393(17) 0.057(2) 0.0073(15) 0.0072(16) 0.0021(15) C5 0.045(2) 0.043(2) 0.067(2) -0.0194(18) -0.0052(18) 0.0111(16) C6 0.042(2) 0.0412(19) 0.056(2) -0.0139(15) 0.0083(17) -0.0018(15) C7 0.098(4) 0.071(3) 0.054(3) -0.015(2) -0.021(2) 0.004(3) C8 0.109(4) 0.084(4) 0.062(3) -0.027(3) -0.025(3) 0.004(3) C9 0.086(3) 0.061(3) 0.103(4) -0.036(3) -0.016(3) 0.011(2) C10 0.0356(19) 0.048(2) 0.0456(19) -0.0062(15) -0.0005(14) -0.0015(15) C11 0.0398(19) 0.0366(17) 0.0523(19) -0.0155(15) 0.0087(16) -0.0032(15) C12 0.066(3) 0.049(2) 0.076(3) 0.005(2) 0.010(2) -0.008(2) C13 0.069(3) 0.057(3) 0.083(3) 0.007(2) 0.020(2) -0.020(2) C14 0.042(2) 0.075(3) 0.093(3) -0.015(3) 0.005(2) -0.010(2) C15 0.0450(19) 0.0378(16) 0.0418(18) -0.0066(14) 0.0010(14) -0.0003(15) C16 0.0388(19) 0.0444(19) 0.050(2) -0.0120(15) 0.0069(15) 0.0013(15) C17 0.0313(17) 0.045(2) 0.054(2) -0.0172(17) 0.0016(15) 0.0005(14) C18 0.048(2) 0.042(2) 0.079(3) -0.0115(18) -0.016(2) 0.0116(17) C19 0.042(2) 0.055(2) 0.084(3) -0.028(2) -0.009(2) 0.0161(18) C20 0.043(2) 0.089(3) 0.073(3) -0.023(2) 0.0199(19) 0.002(2) C21 0.056(2) 0.047(2) 0.053(2) -0.0009(17) 0.0156(17) 0.0080(18) C22 0.065(3) 0.051(2) 0.053(2) 0.0046(18) 0.0210(19) 0.006(2) C23 0.066(3) 0.092(4) 0.103(4) 0.001(3) 0.036(3) -0.018(3) C24 0.086(3) 0.082(3) 0.067(3) 0.007(3) 0.038(3) 0.020(3) C25 0.103(4) 0.072(3) 0.066(3) -0.009(2) 0.015(3) 0.005(3) C28 0.047(2) 0.050(2) 0.0417(19) 0.0050(17) -0.0075(15) -0.0078(17) C29 0.086(3) 0.064(3) 0.051(2) 0.017(2) -0.008(2) 0.005(2) C41 0.0406(18) 0.0486(18) 0.0350(16) -0.0003(15) -0.0050(15) -0.0054(14) C42 0.0445(19) 0.0393(17) 0.0374(16) 0.0019(13) -0.0073(15) -0.0044(15) C43 0.0372(18) 0.0355(16) 0.0354(17) -0.0001(13) 0.0032(13) -0.0003(14) C44 0.049(2) 0.055(2) 0.047(2) 0.0095(17) -0.0108(17) -0.0124(17) C45 0.046(2) 0.064(2) 0.057(2) 0.0092(18) -0.0065(18) -0.0152(18) C46 0.044(2) 0.055(2) 0.052(2) 0.0147(18) -0.0011(17) -0.0036(18) C47 0.065(3) 0.066(3) 0.071(3) -0.010(2) 0.002(2) 0.008(2) C48 0.059(3) 0.066(3) 0.082(3) -0.001(2) 0.006(2) 0.013(2) C49 0.037(2) 0.088(3) 0.118(4) 0.028(3) -0.001(2) -0.002(2) C50 0.064(3) 0.050(2) 0.063(2) -0.0018(19) -0.020(2) -0.0126(19) C51 0.044(2) 0.0416(18) 0.0484(19) -0.0009(15) -0.0054(16) -0.0049(15) C52 0.049(2) 0.060(2) 0.049(2) 0.0058(18) -0.0077(17) -0.0029(18) C53 0.052(2) 0.056(2) 0.055(2) 0.0143(17) -0.0064(18) 0.0009(18) C54 0.075(3) 0.042(2) 0.090(3) 0.001(2) -0.017(2) -0.005(2) C55 0.0444(19) 0.0348(16) 0.0390(17) 0.0013(13) 0.0031(14) 0.0005(14) C56 0.0379(18) 0.0391(18) 0.0453(19) 0.0005(14) 0.0017(14) -0.0002(14) C57 0.0375(19) 0.0425(18) 0.0439(18) 0.0067(15) 0.0037(15) -0.0017(15) C58 0.046(2) 0.056(2) 0.053(2) -0.0044(18) -0.0005(17) -0.0116(17) C59 0.038(2) 0.042(2) 0.070(2) -0.0003(18) 0.0022(18) -0.0107(16) C60 0.049(2) 0.069(3) 0.062(2) 0.009(2) 0.0148(18) -0.0036(19) C61 0.059(2) 0.043(2) 0.0452(19) -0.0080(16) 0.0024(16) 0.0027(17) C62 0.080(3) 0.057(2) 0.041(2) -0.0150(18) -0.002(2) 0.016(2) C63 0.172(7) 0.120(5) 0.060(4) -0.025(3) -0.024(4) 0.082(6) C64 0.210(8) 0.073(3) 0.037(2) -0.005(2) -0.011(4) 0.022(5) C65 0.115(5) 0.137(5) 0.067(3) -0.005(3) 0.021(3) -0.052(4) C66 0.0327(17) 0.050(2) 0.0440(19) -0.0015(17) -0.0034(14) 0.0049(16) C67 0.069(3) 0.063(3) 0.053(2) -0.0147(19) -0.008(2) 0.002(2) C68 0.078(3) 0.047(2) 0.066(3) 0.0032(19) 0.007(2) 0.004(2) C69 0.069(3) 0.0357(18) 0.083(3) -0.005(2) -0.001(2) 0.0034(18) C70 0.048(2) 0.051(2) 0.061(2) 0.0015(19) 0.0130(18) 0.0191(19) C71 0.085(3) 0.060(3) 0.051(2) 0.007(2) 0.000(2) 0.019(2) N42 0.206(10) 0.195(9) 0.117(6) 0.034(5) -0.077(7) -0.049(9) C74 0.121(8) 0.248(16) 0.122(8) 0.103(9) -0.056(7) -0.061(10) C75 0.106(7) 0.43(2) 0.178(10) 0.149(13) -0.003(7) 0.010(11) N43 0.229(9) 0.144(6) 0.091(4) 0.014(4) 0.005(5) -0.006(6) C76 0.171(8) 0.091(5) 0.083(5) 0.014(4) 0.028(5) 0.017(5) C77 0.163(8) 0.206(10) 0.097(5) 0.014(6) 0.008(6) 0.015(7) N44 0.152(7) 0.220(9) 0.157(7) -0.056(6) 0.048(6) 0.009(7) C78 0.104(5) 0.113(5) 0.084(4) -0.021(3) 0.017(4) -0.006(4) C79 0.092(5) 0.120(5) 0.131(5) -0.004(4) 0.004(4) -0.024(4) N45 0.172(7) 0.218(8) 0.086(4) -0.014(5) 0.004(4) -0.031(6) C80 0.093(4) 0.111(5) 0.076(4) -0.018(3) 0.007(3) 0.013(3) C81 0.153(6) 0.086(4) 0.094(4) 0.005(3) -0.013(4) 0.025(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 N4 2.103(3) . ? Fe1 N1 2.105(2) . ? Fe1 O3 2.157(3) . ? Fe1 N6 2.174(3) . ? Fe1 O1A 2.267(4) . ? Fe2 O6B 1.991(10) . ? Fe2 O2A 1.998(4) . ? Fe2 N2 2.130(3) . ? Fe2 N9 2.206(3) . ? Fe2 O3 2.244(2) . ? Fe2 O5A 2.255(6) . ? Fe2 O1B 2.269(12) . ? Fe2 O6A 2.305(6) . ? Fe11 N21 2.066(3) . ? Fe11 O11 2.079(2) . ? Fe11 N26 2.081(3) . ? Fe11 N24 2.090(3) . ? Fe12 O13 1.994(3) . ? Fe12 N22 2.108(3) . ? Fe12 O15 2.161(3) . ? Fe12 N29 2.202(3) . ? Fe12 O11 2.328(2) . ? N1 C2 1.333(4) . ? N1 N2 1.372(4) . ? N2 C3 1.356(4) . ? N3 C10 1.457(4) . ? N3 C4 1.466(4) . ? N3 C5 1.469(4) . ? N4 C6 1.328(5) . ? N4 C7 1.372(5) . ? N5 C8 1.354(6) . ? N5 C6 1.361(4) . ? N5 C9 1.461(6) . ? N6 C11 1.317(5) . ? N6 C12 1.381(5) . ? N7 C11 1.351(5) . ? N7 C13 1.357(6) . ? N7 C14 1.464(5) . ? N8 C21 1.473(5) . ? N8 C16 1.476(4) . ? N8 C15 1.482(4) . ? N9 C17 1.315(5) . ? N9 C18 1.389(4) . ? N10 C17 1.352(4) . ? N10 C19 1.370(6) . ? N10 C20 1.452(5) . ? N11 C22 1.311(6) . ? N11 C23 1.374(6) . ? N12 C22 1.367(5) . ? N12 C24 1.378(6) . ? N12 C25 1.467(6) . ? N21 C42 1.343(4) . ? N21 N22 1.382(4) . ? N22 C43 1.349(4) . ? N23 C50 1.446(5) . ? N23 C45 1.463(5) . ? N23 C44 1.480(4) . ? N24 C46 1.317(5) . ? N24 C47 1.388(5) . ? N25 C46 1.361(5) . ? N25 C48 1.375(6) . ? N25 C49 1.430(5) . ? N26 C51 1.328(4) . ? N26 C52 1.358(5) . ? N27 C51 1.353(5) . ? N27 C53 1.372(5) . ? N27 C54 1.460(5) . ? N28 C61 1.475(4) . ? N28 C55 1.476(4) . ? N28 C56 1.483(4) . ? N29 C57 1.323(4) . ? N29 C58 1.373(5) . ? N30 C59 1.355(5) . ? N30 C57 1.361(4) . ? N30 C60 1.464(5) . ? N31 C62 1.317(6) . ? N31 C63 1.366(8) . ? N32 C62 1.342(6) . ? N32 C64 1.392(7) . ? N32 C65 1.455(7) . ? O1A C26A 1.240(6) . ? O2A C26A 1.271(7) . ? C26A C27A 1.479(9) . ? O1B C26B 1.19(2) . ? O2B C26B 1.21(2) . ? C26B C27B 1.55(3) . ? O3 C28 1.271(4) . ? O4 C28 1.232(5) . ? O5A C30A 1.277(11) . ? O6A C30A 1.243(14) . ? C30A C31A 1.550(14) . ? O5B C30B 1.224(14) . ? O6B C30B 1.226(15) . ? C30B C31B 1.499(17) . ? O11 C66 1.281(4) . ? O12 C66 1.226(5) . ? O13 C68 1.228(5) . ? O14A C68 1.261(6) . ? O14B C68 1.332(14) . ? O15 C70 1.231(5) . ? O16 C70 1.257(5) . ? C1 C2 1.375(4) . ? C1 C3 1.393(5) . ? C2 C4 1.494(4) . ? C3 C15 1.509(4) . ? C5 C6 1.462(5) . ? C7 C8 1.336(7) . ? C10 C11 1.480(5) . ? C12 C13 1.335(7) . ? C16 C17 1.478(5) . ? C18 C19 1.335(6) . ? C21 C22 1.493(5) . ? C23 C24 1.332(8) . ? C28 C29 1.495(5) . ? C41 C42 1.375(5) . ? C41 C43 1.403(5) . ? C42 C44 1.495(5) . ? C43 C55 1.503(4) . ? C45 C46 1.487(6) . ? C47 C48 1.335(6) . ? C50 C51 1.503(5) . ? C52 C53 1.360(6) . ? C56 C57 1.493(5) . ? C58 C59 1.345(5) . ? C61 C62 1.484(5) . ? C63 C64 1.320(10) . ? C66 C67 1.497(5) . ? C68 C69 1.507(5) . ? C70 C71 1.506(6) . ? N42 C74 1.135(16) . ? C74 C75 1.390(18) . ? N43 C76 1.151(11) . ? C76 C77 1.387(11) . ? N44 C78 1.109(9) . ? C78 C79 1.405(10) . ? N45 C80 1.110(8) . ? C80 C81 1.437(8) . ? 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 N4 Fe1 N1 124.70(11) . . ? N4 Fe1 O3 143.77(10) . . ? N1 Fe1 O3 85.57(9) . . ? N4 Fe1 N6 94.09(12) . . ? N1 Fe1 N6 104.49(11) . . ? O3 Fe1 N6 96.82(10) . . ? N4 Fe1 O1A 79.95(12) . . ? N1 Fe1 O1A 87.36(12) . . ? O3 Fe1 O1A 82.48(11) . . ? N6 Fe1 O1A 168.06(12) . . ? O6B Fe2 O2A 114.4(3) . . ? O6B Fe2 N2 133.3(3) . . ? O2A Fe2 N2 111.27(14) . . ? O6B Fe2 N9 91.0(3) . . ? O2A Fe2 N9 87.23(13) . . ? N2 Fe2 N9 100.64(11) . . ? O6B Fe2 O3 88.0(3) . . ? O2A Fe2 O3 87.95(12) . . ? N2 Fe2 O3 84.14(9) . . ? N9 Fe2 O3 174.19(10) . . ? O6B Fe2 O5A 39.6(3) . . ? O2A Fe2 O5A 153.79(18) . . ? N2 Fe2 O5A 94.86(15) . . ? N9 Fe2 O5A 90.00(14) . . ? O3 Fe2 O5A 92.90(14) . . ? O6B Fe2 O1B 139.3(5) . . ? O2A Fe2 O1B 25.3(3) . . ? N2 Fe2 O1B 86.0(3) . . ? N9 Fe2 O1B 91.1(3) . . ? O3 Fe2 O1B 86.0(3) . . ? O5A Fe2 O1B 178.5(3) . . ? O6B Fe2 O6A 18.8(3) . . ? O2A Fe2 O6A 96.1(2) . . ? N2 Fe2 O6A 152.01(18) . . ? N9 Fe2 O6A 86.09(15) . . ? O3 Fe2 O6A 91.21(14) . . ? O5A Fe2 O6A 57.7(2) . . ? O1B Fe2 O6A 121.3(4) . . ? N21 Fe11 O11 86.96(10) . . ? N21 Fe11 N26 114.17(11) . . ? O11 Fe11 N26 135.97(11) . . ? N21 Fe11 N24 117.63(12) . . ? O11 Fe11 N24 102.38(11) . . ? N26 Fe11 N24 100.70(12) . . ? O13 Fe12 N22 121.10(12) . . ? O13 Fe12 O15 143.51(12) . . ? N22 Fe12 O15 92.53(11) . . ? O13 Fe12 N29 91.84(12) . . ? N22 Fe12 N29 98.85(10) . . ? O15 Fe12 N29 96.82(11) . . ? O13 Fe12 O11 87.75(11) . . ? N22 Fe12 O11 84.96(9) . . ? O15 Fe12 O11 81.08(10) . . ? N29 Fe12 O11 175.76(10) . . ? C2 N1 N2 108.3(2) . . ? C2 N1 Fe1 126.3(2) . . ? N2 N1 Fe1 125.24(19) . . ? C3 N2 N1 107.0(2) . . ? C3 N2 Fe2 134.2(2) . . ? N1 N2 Fe2 116.75(19) . . ? C10 N3 C4 111.3(3) . . ? C10 N3 C5 114.4(3) . . ? C4 N3 C5 114.6(3) . . ? C6 N4 C7 106.3(3) . . ? C6 N4 Fe1 124.4(2) . . ? C7 N4 Fe1 129.2(3) . . ? C8 N5 C6 107.3(4) . . ? C8 N5 C9 127.0(4) . . ? C6 N5 C9 125.6(4) . . ? C11 N6 C12 105.1(3) . . ? C11 N6 Fe1 122.5(2) . . ? C12 N6 Fe1 131.8(3) . . ? C11 N7 C13 107.3(4) . . ? C11 N7 C14 125.2(4) . . ? C13 N7 C14 127.4(4) . . ? C21 N8 C16 110.6(3) . . ? C21 N8 C15 112.9(3) . . ? C16 N8 C15 111.4(3) . . ? C17 N9 C18 104.9(3) . . ? C17 N9 Fe2 130.7(2) . . ? C18 N9 Fe2 124.1(3) . . ? C17 N10 C19 106.3(3) . . ? C17 N10 C20 126.6(4) . . ? C19 N10 C20 127.0(3) . . ? C22 N11 C23 105.4(4) . . ? C22 N12 C24 106.5(4) . . ? C22 N12 C25 125.9(4) . . ? C24 N12 C25 127.7(4) . . ? C42 N21 N22 108.1(2) . . ? C42 N21 Fe11 125.9(2) . . ? N22 N21 Fe11 125.68(19) . . ? C43 N22 N21 107.2(2) . . ? C43 N22 Fe12 136.1(2) . . ? N21 N22 Fe12 116.56(18) . . ? C50 N23 C45 114.2(3) . . ? C50 N23 C44 113.1(3) . . ? C45 N23 C44 111.4(3) . . ? C46 N24 C47 105.7(3) . . ? C46 N24 Fe11 122.1(3) . . ? C47 N24 Fe11 132.2(3) . . ? C46 N25 C48 106.8(3) . . ? C46 N25 C49 126.8(4) . . ? C48 N25 C49 126.4(4) . . ? C51 N26 C52 106.2(3) . . ? C51 N26 Fe11 118.9(2) . . ? C52 N26 Fe11 134.9(2) . . ? C51 N27 C53 107.2(3) . . ? C51 N27 C54 126.3(3) . . ? C53 N27 C54 126.5(3) . . ? C61 N28 C55 112.5(3) . . ? C61 N28 C56 110.8(3) . . ? C55 N28 C56 111.2(2) . . ? C57 N29 C58 105.5(3) . . ? C57 N29 Fe12 133.2(2) . . ? C58 N29 Fe12 120.7(2) . . ? C59 N30 C57 107.5(3) . . ? C59 N30 C60 125.1(3) . . ? C57 N30 C60 127.2(3) . . ? C62 N31 C63 105.2(6) . . ? C62 N32 C64 105.7(5) . . ? C62 N32 C65 126.5(4) . . ? C64 N32 C65 127.8(5) . . ? C26A O1A Fe1 137.1(3) . . ? C26A O2A Fe2 129.9(3) . . ? O1A C26A O2A 124.5(4) . . ? O1A C26A C27A 114.9(5) . . ? O2A C26A C27A 120.6(5) . . ? C26B O1B Fe2 100.5(12) . . ? O1B C26B O2B 120.0(19) . . ? O1B C26B C27B 118.1(17) . . ? O2B C26B C27B 120.0(16) . . ? C28 O3 Fe1 97.6(2) . . ? C28 O3 Fe2 134.3(2) . . ? Fe1 O3 Fe2 109.89(10) . . ? C30A O5A Fe2 90.8(6) . . ? C30A O6A Fe2 89.4(6) . . ? O6A C30A O5A 121.8(10) . . ? O6A C30A C31A 120.2(9) . . ? O5A C30A C31A 117.0(10) . . ? C30B O6B Fe2 120.1(9) . . ? O5B C30B O6B 127.6(11) . . ? O5B C30B C31B 120.5(11) . . ? O6B C30B C31B 110.3(11) . . ? C66 O11 Fe11 104.1(2) . . ? C66 O11 Fe12 125.6(2) . . ? Fe11 O11 Fe12 106.64(10) . . ? C68 O13 Fe12 122.9(3) . . ? C70 O15 Fe12 98.1(3) . . ? C2 C1 C3 104.3(3) . . ? N1 C2 C1 110.7(3) . . ? N1 C2 C4 118.5(3) . . ? C1 C2 C4 130.5(3) . . ? N2 C3 C1 109.7(3) . . ? N2 C3 C15 121.3(3) . . ? C1 C3 C15 128.4(3) . . ? N3 C4 C2 109.7(3) . . ? C6 C5 N3 111.8(3) . . ? N4 C6 N5 109.5(3) . . ? N4 C6 C5 125.7(3) . . ? N5 C6 C5 124.8(3) . . ? C8 C7 N4 109.3(4) . . ? C7 C8 N5 107.5(4) . . ? N3 C10 C11 110.5(3) . . ? N6 C11 N7 110.9(3) . . ? N6 C11 C10 124.1(3) . . ? N7 C11 C10 124.9(3) . . ? C13 C12 N6 110.0(4) . . ? C12 C13 N7 106.7(4) . . ? N8 C15 C3 113.3(3) . . ? N8 C16 C17 110.2(3) . . ? N9 C17 N10 111.9(3) . . ? N9 C17 C16 126.7(3) . . ? N10 C17 C16 121.3(3) . . ? C19 C18 N9 109.8(4) . . ? C18 C19 N10 107.2(3) . . ? N8 C21 C22 110.3(3) . . ? N11 C22 N12 111.0(4) . . ? N11 C22 C21 125.9(4) . . ? N12 C22 C21 123.1(4) . . ? C24 C23 N11 111.0(4) . . ? C23 C24 N12 106.2(4) . . ? O4 C28 O3 120.1(3) . . ? O4 C28 C29 121.1(3) . . ? O3 C28 C29 118.8(4) . . ? C42 C41 C43 104.5(3) . . ? N21 C42 C41 110.4(3) . . ? N21 C42 C44 118.5(3) . . ? C41 C42 C44 130.6(3) . . ? N22 C43 C41 109.8(3) . . ? N22 C43 C55 121.3(3) . . ? C41 C43 C55 128.8(3) . . ? N23 C44 C42 110.0(3) . . ? N23 C45 C46 109.9(3) . . ? N24 C46 N25 110.8(4) . . ? N24 C46 C45 124.2(3) . . ? N25 C46 C45 124.8(3) . . ? C48 C47 N24 109.8(4) . . ? C47 C48 N25 106.9(4) . . ? N23 C50 C51 109.1(3) . . ? N26 C51 N27 110.6(3) . . ? N26 C51 C50 123.2(3) . . ? N27 C51 C50 126.1(3) . . ? N26 C52 C53 110.0(3) . . ? C52 C53 N27 106.1(3) . . ? N28 C55 C43 115.2(3) . . ? N28 C56 C57 110.4(3) . . ? N29 C57 N30 110.4(3) . . ? N29 C57 C56 126.8(3) . . ? N30 C57 C56 122.8(3) . . ? C59 C58 N29 110.2(3) . . ? C58 C59 N30 106.5(3) . . ? N28 C61 C62 110.2(3) . . ? N31 C62 N32 111.8(4) . . ? N31 C62 C61 124.3(4) . . ? N32 C62 C61 123.9(4) . . ? C64 C63 N31 110.8(6) . . ? C63 C64 N32 106.6(5) . . ? O12 C66 O11 121.1(3) . . ? O12 C66 C67 121.9(3) . . ? O11 C66 C67 117.0(3) . . ? O13 C68 O14A 123.2(4) . . ? O13 C68 O14B 116.3(7) . . ? O14A C68 O14B 49.8(6) . . ? O13 C68 C69 117.3(4) . . ? O14A C68 C69 118.1(4) . . ? O14B C68 C69 111.6(7) . . ? O15 C70 O16 120.7(4) . . ? O15 C70 C71 119.9(4) . . ? O16 C70 C71 119.3(4) . . ? N42 C74 C75 169.8(16) . . ? N43 C76 C77 176.3(9) . . ? N44 C78 C79 177.8(9) . . ? N45 C80 C81 176.7(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.512 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.048 data_1-acetat_100at100K-synchrotron _database_code_depnum_ccdc_archive 'CCDC 831485' #TrackingRef '- pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H42 Fe2 N12 O6, 2(C2 H3 N)' _chemical_formula_sum 'C35 H48 Fe2 N14 O6' _chemical_formula_weight 872.57 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 'P 21 21 21' 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 16.264(3) _cell_length_b 18.940(4) _cell_length_c 26.215(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8075(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 62244 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 30.92 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6983 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.80000 _diffrn_radiation_type ? _diffrn_radiation_source synchrotron _diffrn_source_type 'BESSY ML Beamline 14.2' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Mar MX-225' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62244 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 30.92 _reflns_number_total 17697 _reflns_number_gt 16890 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0448P)^2^+5.7938P] 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 -0.079(7) _refine_ls_number_reflns 17697 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.228180(19) 0.584288(15) 0.385359(12) 0.00672(7) Uani 1 1 d . . . Fe2 Fe 0.094335(19) 0.717033(15) 0.439285(13) 0.00753(7) Uani 1 1 d . . . Fe11 Fe 0.75468(2) 0.399523(16) 0.407504(12) 0.01075(7) Uani 1 1 d . . . Fe12 Fe 0.570677(18) 0.310142(15) 0.436976(12) 0.00689(6) Uani 1 1 d . . . N1 N 0.20481(11) 0.59400(9) 0.46469(7) 0.0060(3) Uani 1 1 d . . . N2 N 0.16580(11) 0.65016(9) 0.48724(7) 0.0066(3) Uani 1 1 d . . . N3 N 0.31639(11) 0.48889(9) 0.44075(8) 0.0087(4) Uani 1 1 d . . . N4 N 0.23997(12) 0.48778(10) 0.34465(7) 0.0115(4) Uani 1 1 d . . . N5 N 0.27314(14) 0.37813(11) 0.32638(9) 0.0184(4) Uani 1 1 d . . . N6 N 0.36030(11) 0.60520(10) 0.38088(8) 0.0102(4) Uani 1 1 d . . . N7 N 0.48935(12) 0.60733(10) 0.40712(8) 0.0120(4) Uani 1 1 d . . . N8 N 0.04572(12) 0.65446(9) 0.59305(7) 0.0092(4) Uani 1 1 d . . . N9 N -0.01237(12) 0.73624(9) 0.48867(8) 0.0108(4) Uani 1 1 d . . . N10 N -0.11456(12) 0.72456(10) 0.54386(8) 0.0121(4) Uani 1 1 d . . . N11 N -0.07061(15) 0.52646(12) 0.64430(9) 0.0227(5) Uani 1 1 d . . . N12 N -0.04635(14) 0.61696(11) 0.69597(8) 0.0150(4) Uani 1 1 d . . . N21 N 0.71856(12) 0.37959(10) 0.48215(7) 0.0087(4) Uani 1 1 d . . . N22 N 0.64898(11) 0.34448(9) 0.49639(7) 0.0070(3) Uani 1 1 d . . . N23 N 0.85304(12) 0.46243(10) 0.46830(7) 0.0110(4) Uani 1 1 d . . . N24 N 0.87361(13) 0.37292(11) 0.38501(8) 0.0140(4) Uani 1 1 d . . . N25 N 1.00884(13) 0.37604(10) 0.38562(9) 0.0158(4) Uani 1 1 d . . . N26 N 0.75068(12) 0.50594(10) 0.38806(7) 0.0123(4) Uani 1 1 d . . . N27 N 0.77234(13) 0.61929(10) 0.40188(8) 0.0142(4) Uani 1 1 d . . . N28 N 0.51891(12) 0.35121(9) 0.59643(7) 0.0087(4) Uani 1 1 d . . . N29 N 0.45389(12) 0.31162(10) 0.47837(7) 0.0103(4) Uani 1 1 d . . . N30 N 0.35358(12) 0.31708(10) 0.53554(7) 0.0103(4) Uani 1 1 d . . . N31 N 0.65729(17) 0.34549(15) 0.69267(9) 0.0319(6) Uani 1 1 d . . . N32 N 0.52641(17) 0.33544(12) 0.71611(9) 0.0247(5) Uani 1 1 d . . . O1 O 0.09758(11) 0.56423(9) 0.37219(8) 0.0190(4) Uani 1 1 d . . . O2 O 0.01809(11) 0.65474(9) 0.39596(7) 0.0175(4) Uani 1 1 d . . . O3 O 0.19218(9) 0.69574(8) 0.38179(6) 0.0093(3) Uani 1 1 d . . . O4 O 0.21880(12) 0.64849(9) 0.30698(7) 0.0185(4) Uani 1 1 d . . . O5 O 0.15413(11) 0.81630(9) 0.46281(7) 0.0169(4) Uani 1 1 d . . . O6 O 0.06465(12) 0.82053(9) 0.40002(7) 0.0204(4) Uani 1 1 d . . . O11 O 0.68732(9) 0.30887(8) 0.38937(6) 0.0095(3) Uani 1 1 d . . . O12 O 0.71580(12) 0.36161(10) 0.31651(7) 0.0202(4) Uani 1 1 d . . . O13 O 0.55535(12) 0.20744(9) 0.42003(7) 0.0199(4) Uani 1 1 d . A . O14A O 0.6243(2) 0.17335(12) 0.48927(10) 0.0338(8) Uani 0.874(6) 1 d P A 1 O14B O 0.5700(17) 0.1684(9) 0.4982(7) 0.0338(8) Uani 0.126(6) 1 d P A 2 O15 O 0.56189(11) 0.41661(9) 0.40721(7) 0.0178(4) Uani 1 1 d . . . O16 O 0.50675(11) 0.33748(9) 0.35684(7) 0.0191(4) Uani 1 1 d . . . C1 C 0.21063(13) 0.57662(11) 0.54918(8) 0.0083(4) Uani 1 1 d . . . H1 H 0.2228 0.5568 0.5816 0.080 Uiso 1 1 calc R . . C2 C 0.22949(13) 0.54952(10) 0.50149(8) 0.0076(4) Uani 1 1 d . . . C3 C 0.16950(13) 0.63993(11) 0.53853(8) 0.0072(4) Uani 1 1 d . . . C4 C 0.26572(14) 0.47951(11) 0.48632(9) 0.0103(4) Uani 1 1 d . . . H4A H 0.2997 0.4607 0.5145 0.080 Uiso 1 1 calc R . . H4B H 0.2211 0.4453 0.4792 0.080 Uiso 1 1 calc R . . C5 C 0.32611(14) 0.42501(11) 0.40993(9) 0.0121(4) Uani 1 1 d . . . H5A H 0.3050 0.3838 0.4292 0.080 Uiso 1 1 calc R . . H5B H 0.3852 0.4170 0.4029 0.080 Uiso 1 1 calc R . . C6 C 0.28048(14) 0.43151(11) 0.36052(9) 0.0111(4) Uani 1 1 d . . . C7 C 0.20424(18) 0.46970(14) 0.29889(10) 0.0207(5) Uani 1 1 d . . . H7 H 0.1706 0.4998 0.2787 0.080 Uiso 1 1 calc R . . C8 C 0.22465(19) 0.40198(15) 0.28712(11) 0.0261(6) Uani 1 1 d . . . H8 H 0.2086 0.3763 0.2576 0.080 Uiso 1 1 calc R . . C9 C 0.30673(18) 0.30659(14) 0.33169(12) 0.0268(6) Uani 1 1 d . . . H9A H 0.2767 0.2813 0.3585 0.080 Uiso 1 1 calc R . . H9B H 0.3651 0.3094 0.3408 0.080 Uiso 1 1 calc R . . H9C H 0.3008 0.2813 0.2993 0.080 Uiso 1 1 calc R . . C10 C 0.39402(13) 0.52447(11) 0.45299(9) 0.0093(4) Uani 1 1 d . . . H10A H 0.4389 0.4893 0.4548 0.080 Uiso 1 1 calc R . . H10B H 0.3895 0.5477 0.4867 0.080 Uiso 1 1 calc R . . C11 C 0.41366(13) 0.57860(11) 0.41307(8) 0.0085(4) Uani 1 1 d . . . C12 C 0.40351(16) 0.65399(12) 0.35223(10) 0.0153(5) Uani 1 1 d . . . H12 H 0.3811 0.6818 0.3255 0.080 Uiso 1 1 calc R . . C13 C 0.48277(16) 0.65606(13) 0.36817(10) 0.0172(5) Uani 1 1 d . . . H13 H 0.5254 0.6853 0.3551 0.080 Uiso 1 1 calc R . . C14 C 0.56160(14) 0.59277(13) 0.43815(11) 0.0186(5) Uani 1 1 d . . . H14A H 0.5772 0.5431 0.4343 0.080 Uiso 1 1 calc R . . H14B H 0.5491 0.6025 0.4740 0.080 Uiso 1 1 calc R . . H14C H 0.6071 0.6230 0.4270 0.080 Uiso 1 1 calc R . . C15 C 0.12348(13) 0.68649(11) 0.57497(9) 0.0093(4) Uani 1 1 d . . . H15A H 0.1590 0.6967 0.6047 0.080 Uiso 1 1 calc R . . H15B H 0.1110 0.7319 0.5579 0.080 Uiso 1 1 calc R . . C16 C -0.00623(14) 0.63300(11) 0.54939(9) 0.0101(4) Uani 1 1 d . . . H16A H -0.0500 0.6005 0.5612 0.080 Uiso 1 1 calc R . . H16B H 0.0276 0.6078 0.5238 0.080 Uiso 1 1 calc R . . C17 C -0.04385(14) 0.69676(11) 0.52585(9) 0.0100(4) Uani 1 1 d . . . C18 C -0.06702(14) 0.79184(11) 0.48303(9) 0.0135(5) Uani 1 1 d . . . H18 H -0.0612 0.8291 0.4591 0.080 Uiso 1 1 calc R . . C19 C -0.12965(15) 0.78542(12) 0.51648(10) 0.0141(5) Uani 1 1 d . . . H19 H -0.1750 0.8165 0.5204 0.080 Uiso 1 1 calc R . . C20 C -0.16357(15) 0.69593(13) 0.58542(10) 0.0177(5) Uani 1 1 d . . . H20A H -0.1287 0.6895 0.6156 0.080 Uiso 1 1 calc R . . H20B H -0.1867 0.6503 0.5752 0.080 Uiso 1 1 calc R . . H20C H -0.2083 0.7287 0.5935 0.080 Uiso 1 1 calc R . . C21 C 0.05907(15) 0.59374(12) 0.62761(9) 0.0133(4) Uani 1 1 d . . . H21A H 0.1037 0.6049 0.6520 0.080 Uiso 1 1 calc R . . H21B H 0.0759 0.5519 0.6075 0.080 Uiso 1 1 calc R . . C22 C -0.01835(16) 0.57762(13) 0.65624(10) 0.0159(5) Uani 1 1 d . . . C23 C -0.13454(18) 0.53439(15) 0.67799(12) 0.0261(6) Uani 1 1 d . . . H23 H -0.1821 0.5052 0.6787 0.080 Uiso 1 1 calc R . . C24 C -0.12097(17) 0.58948(14) 0.71028(10) 0.0217(5) Uani 1 1 d . . . H24 H -0.1557 0.6055 0.7370 0.080 Uiso 1 1 calc R . . C25 C -0.00537(18) 0.67828(14) 0.71905(10) 0.0222(6) Uani 1 1 d . . . H25A H -0.0281 0.7218 0.7046 0.080 Uiso 1 1 calc R . . H25B H 0.0537 0.6761 0.7120 0.080 Uiso 1 1 calc R . . H25C H -0.0144 0.6779 0.7560 0.080 Uiso 1 1 calc R . . C26 C 0.03276(14) 0.59858(12) 0.37144(9) 0.0103(4) Uani 1 1 d . . . C27 C -0.03597(15) 0.56992(13) 0.33806(9) 0.0148(5) Uani 1 1 d . . . H27A H -0.0387 0.5185 0.3416 0.080 Uiso 1 1 calc R . . H27B H -0.0251 0.5821 0.3024 0.080 Uiso 1 1 calc R . . H27C H -0.0884 0.5907 0.3487 0.080 Uiso 1 1 calc R . . C28 C 0.19804(14) 0.70068(12) 0.33298(9) 0.0110(4) Uani 1 1 d . . . C29 C 0.18248(18) 0.77168(14) 0.30850(10) 0.0200(5) Uani 1 1 d . . . H29A H 0.1897 0.7678 0.2715 0.080 Uiso 1 1 calc R . . H29B H 0.2214 0.8064 0.3221 0.080 Uiso 1 1 calc R . . H29C H 0.1262 0.7869 0.3160 0.080 Uiso 1 1 calc R . . C30 C 0.11659(16) 0.85005(12) 0.42831(11) 0.0183(5) Uani 1 1 d . . . C31 C 0.1350(2) 0.92791(14) 0.42111(14) 0.0335(7) Uani 1 1 d . . . H31A H 0.0916 0.9496 0.4004 0.080 Uiso 1 1 calc R . . H31B H 0.1880 0.9333 0.4038 0.080 Uiso 1 1 calc R . . H31C H 0.1373 0.9512 0.4545 0.080 Uiso 1 1 calc R . . C41 C 0.72294(14) 0.36825(11) 0.56697(9) 0.0108(4) Uani 1 1 d . . . H41 H 0.7401 0.3712 0.6015 0.080 Uiso 1 1 calc R . . C42 C 0.76323(14) 0.39384(11) 0.52411(8) 0.0092(4) Uani 1 1 d . . . C43 C 0.65155(14) 0.33712(11) 0.54779(8) 0.0072(4) Uani 1 1 d . . . C44 C 0.84780(14) 0.42459(12) 0.51752(9) 0.0124(4) Uani 1 1 d . . . H44A H 0.8597 0.4576 0.5458 0.080 Uiso 1 1 calc R . . H44B H 0.8893 0.3863 0.5184 0.080 Uiso 1 1 calc R . . C45 C 0.93576(15) 0.45905(13) 0.44602(10) 0.0159(5) Uani 1 1 d . . . H45A H 0.9766 0.4498 0.4732 0.080 Uiso 1 1 calc R . . H45B H 0.9494 0.5048 0.4299 0.080 Uiso 1 1 calc R . . C46 C 0.93938(15) 0.40134(12) 0.40693(9) 0.0136(4) Uani 1 1 d . . . C47 C 0.90281(17) 0.32742(13) 0.34812(10) 0.0186(5) Uani 1 1 d . . . H47 H 0.8698 0.2993 0.3262 0.080 Uiso 1 1 calc R . . C48 C 0.98643(17) 0.32915(14) 0.34811(11) 0.0204(5) Uani 1 1 d . . . H48 H 1.0222 0.3031 0.3265 0.080 Uiso 1 1 calc R . . C49 C 1.09309(16) 0.39440(14) 0.39970(12) 0.0226(6) Uani 1 1 d . . . H49A H 1.1038 0.3791 0.4348 0.080 Uiso 1 1 calc R . . H49B H 1.1005 0.4456 0.3972 0.080 Uiso 1 1 calc R . . H49C H 1.1316 0.3707 0.3766 0.080 Uiso 1 1 calc R . . C50 C 0.81889(16) 0.53424(12) 0.47097(10) 0.0155(5) Uani 1 1 d . . . H50A H 0.8629 0.5683 0.4796 0.080 Uiso 1 1 calc R . . H50B H 0.7763 0.5366 0.4979 0.080 Uiso 1 1 calc R . . C51 C 0.78182(14) 0.55290(12) 0.42020(9) 0.0111(4) Uani 1 1 d . . . C52 C 0.72007(16) 0.54361(13) 0.34755(10) 0.0160(5) Uani 1 1 d . . . H52 H 0.6940 0.5239 0.3184 0.080 Uiso 1 1 calc R . . C53 C 0.73319(15) 0.61424(13) 0.35576(10) 0.0171(5) Uani 1 1 d . . . H53 H 0.7181 0.6521 0.3339 0.080 Uiso 1 1 calc R . . C54 C 0.79891(17) 0.68450(12) 0.42716(11) 0.0207(5) Uani 1 1 d . . . H54A H 0.8579 0.6817 0.4347 0.080 Uiso 1 1 calc R . . H54B H 0.7682 0.6905 0.4590 0.080 Uiso 1 1 calc R . . H54C H 0.7884 0.7248 0.4047 0.080 Uiso 1 1 calc R . . C55 C 0.58268(14) 0.30219(11) 0.57643(8) 0.0089(4) Uani 1 1 d . . . H55A H 0.5558 0.2676 0.5535 0.080 Uiso 1 1 calc R . . H55B H 0.6064 0.2756 0.6054 0.080 Uiso 1 1 calc R . . C56 C 0.47894(14) 0.39011(11) 0.55430(9) 0.0104(4) Uani 1 1 d . . . H56A H 0.5214 0.4135 0.5332 0.080 Uiso 1 1 calc R . . H56B H 0.4425 0.4271 0.5685 0.080 Uiso 1 1 calc R . . C57 C 0.42961(14) 0.34088(11) 0.52185(9) 0.0096(4) Uani 1 1 d . . . C58 C 0.38995(14) 0.26764(12) 0.46403(9) 0.0131(5) Uani 1 1 d . . . H58 H 0.3895 0.2391 0.4342 0.080 Uiso 1 1 calc R . . C59 C 0.32818(14) 0.27108(11) 0.49852(9) 0.0131(5) Uani 1 1 d . . . H59 H 0.2773 0.2465 0.4973 0.080 Uiso 1 1 calc R . . C60 C 0.30898(15) 0.33349(13) 0.58216(9) 0.0149(5) Uani 1 1 d . . . H60A H 0.2554 0.3098 0.5816 0.080 Uiso 1 1 calc R . . H60B H 0.3008 0.3846 0.5846 0.080 Uiso 1 1 calc R . . H60C H 0.3407 0.3171 0.6117 0.080 Uiso 1 1 calc R . . C61 C 0.55310(15) 0.40046(12) 0.63463(9) 0.0118(4) Uani 1 1 d . . . H61A H 0.5107 0.4356 0.6441 0.080 Uiso 1 1 calc R . . H61B H 0.6004 0.4261 0.6197 0.080 Uiso 1 1 calc R . . C62 C 0.58053(18) 0.36181(13) 0.68123(9) 0.0176(5) Uani 1 1 d . . . C63 C 0.6523(3) 0.30635(19) 0.73686(11) 0.0426(10) Uani 1 1 d . . . H63 H 0.6982 0.2870 0.7544 0.080 Uiso 1 1 calc R . . C64 C 0.5742(3) 0.29936(15) 0.75163(11) 0.0380(9) Uani 1 1 d . . . H64 H 0.5550 0.2746 0.7808 0.080 Uiso 1 1 calc R . . C65 C 0.4382(2) 0.3478(2) 0.71753(12) 0.0381(8) Uani 1 1 d . . . H65A H 0.4128 0.3284 0.6867 0.080 Uiso 1 1 calc R . . H65B H 0.4275 0.3987 0.7193 0.080 Uiso 1 1 calc R . . H65C H 0.4147 0.3247 0.7476 0.080 Uiso 1 1 calc R . . C66 C 0.68917(13) 0.30964(12) 0.33992(9) 0.0098(4) Uani 1 1 d . . . C67 C 0.66148(16) 0.24364(13) 0.31319(9) 0.0160(5) Uani 1 1 d . . . H67A H 0.6543 0.2534 0.2767 0.080 Uiso 1 1 calc R . . H67B H 0.6091 0.2278 0.3277 0.080 Uiso 1 1 calc R . . H67C H 0.7030 0.2066 0.3176 0.080 Uiso 1 1 calc R . . C68 C 0.58508(17) 0.16081(12) 0.44955(10) 0.0190(5) Uani 1 1 d . . . C69 C 0.57877(16) 0.08509(11) 0.43057(10) 0.0168(5) Uani 1 1 d . A . H69A H 0.5949 0.0527 0.4579 0.080 Uiso 1 1 calc R . . H69B H 0.6153 0.0786 0.4012 0.080 Uiso 1 1 calc R . . H69C H 0.5220 0.0752 0.4203 0.080 Uiso 1 1 calc R . . C70 C 0.52734(15) 0.40046(13) 0.36607(9) 0.0138(5) Uani 1 1 d . . . C71 C 0.50875(18) 0.45696(14) 0.32700(10) 0.0197(5) Uani 1 1 d . . . H71A H 0.4506 0.4545 0.3174 0.080 Uiso 1 1 calc R . . H71B H 0.5430 0.4495 0.2967 0.080 Uiso 1 1 calc R . . H71C H 0.5206 0.5035 0.3416 0.080 Uiso 1 1 calc R . . N42 N 0.2824(3) 0.6838(2) 0.66960(12) 0.0545(10) Uani 1 1 d . . . C74 C 0.3304(3) 0.6454(2) 0.65313(14) 0.0418(9) Uani 1 1 d . . . C75 C 0.3903(2) 0.5963(2) 0.63287(16) 0.0521(11) Uani 1 1 d . . . H75A H 0.3963 0.5563 0.6563 0.078 Uiso 1 1 calc R . . H75B H 0.4433 0.6202 0.6290 0.078 Uiso 1 1 calc R . . H75C H 0.3716 0.5791 0.5996 0.078 Uiso 1 1 calc R . . N43 N 0.2461(2) 0.53350(16) 0.16396(11) 0.0435(7) Uani 1 1 d . . . C76 C 0.2950(2) 0.54319(16) 0.19458(11) 0.0299(7) Uani 1 1 d . . . C77 C 0.3569(3) 0.5560(2) 0.23309(14) 0.0427(8) Uani 1 1 d . . . H77A H 0.4005 0.5857 0.2188 0.064 Uiso 1 1 calc R . . H77B H 0.3803 0.5109 0.2443 0.064 Uiso 1 1 calc R . . H77C H 0.3318 0.5801 0.2623 0.064 Uiso 1 1 calc R . . N44 N 0.9989(2) 0.4640(2) 0.22555(13) 0.0506(8) Uani 1 1 d . . . C78 C 0.9308(2) 0.46233(16) 0.23438(11) 0.0302(7) Uani 1 1 d . . . C79 C 0.8440(2) 0.46359(19) 0.24536(15) 0.0380(8) Uani 1 1 d . . . H79A H 0.8249 0.5126 0.2467 0.057 Uiso 1 1 calc R . . H79B H 0.8338 0.4408 0.2783 0.057 Uiso 1 1 calc R . . H79C H 0.8142 0.4382 0.2185 0.057 Uiso 1 1 calc R . . N45 N 0.6047(2) 0.67496(17) 0.26215(11) 0.0406(7) Uani 1 1 d . . . C80 C 0.59326(18) 0.66354(15) 0.22003(11) 0.0242(6) Uani 1 1 d . . . C81 C 0.5800(2) 0.65143(16) 0.16565(12) 0.0304(7) Uani 1 1 d . . . H81A H 0.5402 0.6859 0.1526 0.046 Uiso 1 1 calc R . . H81B H 0.5587 0.6036 0.1605 0.046 Uiso 1 1 calc R . . H81C H 0.6322 0.6567 0.1474 0.046 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 0.00728(14) 0.00444(13) 0.00845(14) -0.00175(11) 0.00092(12) -0.00001(11) Fe2 0.00683(14) 0.00331(13) 0.01243(15) 0.00134(11) -0.00054(12) 0.00159(10) Fe11 0.01567(16) 0.00847(14) 0.00811(14) -0.00007(11) 0.00209(13) -0.00717(12) Fe12 0.00603(14) 0.00619(13) 0.00846(14) -0.00165(11) -0.00100(12) -0.00130(11) N1 0.0069(8) 0.0020(7) 0.0092(8) -0.0006(6) 0.0018(7) 0.0016(6) N2 0.0052(8) 0.0033(8) 0.0111(9) -0.0001(7) 0.0033(7) 0.0025(6) N3 0.0075(8) 0.0045(8) 0.0142(9) -0.0031(7) 0.0002(8) 0.0004(6) N4 0.0122(9) 0.0102(8) 0.0121(9) -0.0048(7) 0.0001(8) -0.0007(7) N5 0.0183(10) 0.0126(9) 0.0243(11) -0.0121(8) -0.0013(9) 0.0021(8) N6 0.0091(9) 0.0087(8) 0.0128(9) -0.0022(7) 0.0020(8) -0.0032(7) N7 0.0080(9) 0.0095(9) 0.0186(10) -0.0052(8) 0.0028(8) -0.0031(7) N8 0.0095(9) 0.0062(8) 0.0120(9) -0.0006(7) 0.0022(8) -0.0005(7) N9 0.0087(9) 0.0054(8) 0.0183(10) -0.0026(7) -0.0002(8) 0.0018(7) N10 0.0068(9) 0.0133(9) 0.0163(10) -0.0062(8) -0.0003(8) 0.0016(7) N11 0.0250(12) 0.0173(10) 0.0257(12) -0.0014(9) 0.0128(10) -0.0056(9) N12 0.0191(10) 0.0144(9) 0.0116(9) 0.0016(7) 0.0053(8) 0.0050(8) N21 0.0076(8) 0.0104(8) 0.0081(9) 0.0007(7) 0.0013(7) -0.0036(7) N22 0.0069(8) 0.0056(8) 0.0087(8) -0.0001(7) -0.0005(7) -0.0017(7) N23 0.0121(10) 0.0114(9) 0.0095(9) 0.0028(7) -0.0003(8) -0.0063(7) N24 0.0124(9) 0.0151(9) 0.0145(10) 0.0002(8) -0.0002(9) -0.0015(7) N25 0.0129(10) 0.0114(9) 0.0230(11) 0.0079(8) -0.0015(9) -0.0007(7) N26 0.0109(9) 0.0150(9) 0.0109(9) 0.0006(7) -0.0006(8) -0.0040(7) N27 0.0125(9) 0.0100(9) 0.0202(10) 0.0018(7) -0.0029(9) -0.0019(7) N28 0.0113(9) 0.0058(8) 0.0089(8) 0.0003(7) 0.0020(8) -0.0004(7) N29 0.0082(8) 0.0103(8) 0.0125(9) -0.0006(7) 0.0019(7) -0.0018(7) N30 0.0077(9) 0.0102(8) 0.0129(9) 0.0023(7) 0.0019(8) -0.0003(7) N31 0.0363(15) 0.0474(16) 0.0122(11) -0.0088(11) -0.0065(11) 0.0244(13) N32 0.0447(15) 0.0147(10) 0.0147(11) -0.0007(8) 0.0020(11) -0.0072(10) O1 0.0078(8) 0.0097(8) 0.0396(11) -0.0053(7) -0.0057(8) -0.0006(6) O2 0.0116(8) 0.0158(8) 0.0250(10) -0.0067(7) -0.0032(7) 0.0017(7) O3 0.0095(7) 0.0075(7) 0.0108(7) 0.0027(6) -0.0007(6) -0.0013(6) O4 0.0236(9) 0.0182(8) 0.0136(8) -0.0034(7) -0.0037(8) 0.0027(7) O5 0.0181(9) 0.0077(7) 0.0251(9) 0.0029(7) 0.0044(8) 0.0025(7) O6 0.0212(9) 0.0130(8) 0.0269(10) 0.0059(7) 0.0024(8) 0.0042(7) O11 0.0075(7) 0.0124(7) 0.0086(7) -0.0034(6) -0.0013(6) -0.0003(6) O12 0.0217(9) 0.0194(9) 0.0194(9) 0.0080(7) -0.0059(8) -0.0064(7) O13 0.0231(9) 0.0084(7) 0.0281(10) 0.0010(7) 0.0038(8) 0.0009(7) O14A 0.056(2) 0.0177(10) 0.0276(13) -0.0081(9) -0.0068(14) -0.0021(12) O14B 0.056(2) 0.0177(10) 0.0276(13) -0.0081(9) -0.0068(14) -0.0021(12) O15 0.0258(9) 0.0120(8) 0.0154(8) 0.0009(7) -0.0004(8) 0.0043(7) O16 0.0140(8) 0.0151(8) 0.0283(10) 0.0007(7) 0.0020(8) 0.0031(7) C1 0.0066(9) 0.0093(9) 0.0090(10) 0.0013(8) 0.0013(8) 0.0008(8) C2 0.0065(9) 0.0045(9) 0.0117(10) 0.0014(8) 0.0030(8) 0.0005(8) C3 0.0035(9) 0.0071(9) 0.0109(10) 0.0004(8) 0.0007(8) -0.0013(7) C4 0.0086(10) 0.0048(9) 0.0175(11) 0.0027(8) 0.0016(9) 0.0033(8) C5 0.0123(10) 0.0065(9) 0.0176(11) -0.0067(9) 0.0002(9) 0.0030(8) C6 0.0087(10) 0.0091(10) 0.0155(11) -0.0066(8) 0.0047(9) -0.0020(8) C7 0.0273(14) 0.0200(12) 0.0148(12) -0.0069(10) -0.0075(11) 0.0041(10) C8 0.0303(15) 0.0256(13) 0.0223(13) -0.0160(11) -0.0077(12) 0.0039(12) C9 0.0252(14) 0.0143(12) 0.0409(17) -0.0196(12) -0.0085(13) 0.0073(11) C10 0.0054(10) 0.0104(9) 0.0122(10) -0.0015(8) -0.0013(8) -0.0014(8) C11 0.0051(9) 0.0079(9) 0.0125(10) -0.0069(8) 0.0024(8) -0.0018(8) C12 0.0168(12) 0.0116(10) 0.0177(12) 0.0003(9) 0.0029(10) -0.0027(9) C13 0.0152(12) 0.0137(11) 0.0228(13) -0.0009(9) 0.0068(10) -0.0058(9) C14 0.0094(10) 0.0185(11) 0.0278(13) -0.0074(10) 0.0007(11) -0.0022(9) C15 0.0088(10) 0.0062(9) 0.0128(10) -0.0012(8) -0.0005(8) -0.0006(8) C16 0.0087(10) 0.0079(9) 0.0139(11) -0.0027(8) 0.0026(9) -0.0001(8) C17 0.0085(10) 0.0074(9) 0.0141(10) -0.0063(8) 0.0002(9) -0.0001(8) C18 0.0121(10) 0.0065(9) 0.0218(12) -0.0025(8) -0.0050(10) 0.0063(8) C19 0.0103(10) 0.0095(9) 0.0225(12) -0.0086(9) -0.0055(10) 0.0049(8) C20 0.0109(11) 0.0196(12) 0.0226(13) -0.0062(10) 0.0067(10) 0.0016(9) C21 0.0154(11) 0.0109(10) 0.0136(11) -0.0004(8) 0.0051(9) 0.0020(9) C22 0.0192(12) 0.0129(11) 0.0156(11) 0.0028(9) 0.0059(10) 0.0043(9) C23 0.0224(14) 0.0256(14) 0.0302(15) 0.0043(11) 0.0123(12) -0.0061(11) C24 0.0229(13) 0.0233(13) 0.0187(12) 0.0043(10) 0.0111(11) 0.0059(11) C25 0.0317(15) 0.0178(12) 0.0171(12) -0.0024(10) 0.0035(11) 0.0025(11) C26 0.0095(10) 0.0098(10) 0.0117(10) 0.0054(8) 0.0017(9) -0.0024(8) C27 0.0145(11) 0.0158(11) 0.0141(11) 0.0025(9) -0.0032(10) -0.0017(9) C28 0.0088(10) 0.0126(11) 0.0117(10) 0.0015(8) -0.0021(9) -0.0040(8) C29 0.0290(14) 0.0177(12) 0.0134(12) 0.0080(9) -0.0041(11) 0.0003(10) C30 0.0157(12) 0.0107(10) 0.0286(14) 0.0036(10) 0.0108(11) 0.0040(9) C31 0.0400(17) 0.0092(11) 0.0512(19) 0.0080(12) -0.0014(15) -0.0016(11) C41 0.0132(10) 0.0107(9) 0.0086(10) -0.0017(8) -0.0042(9) -0.0012(8) C42 0.0106(10) 0.0073(9) 0.0096(10) -0.0008(7) -0.0024(9) 0.0004(8) C43 0.0085(10) 0.0061(9) 0.0070(10) 0.0008(7) -0.0005(8) 0.0036(8) C44 0.0110(10) 0.0164(11) 0.0099(10) 0.0028(8) -0.0028(9) -0.0037(9) C45 0.0141(11) 0.0172(11) 0.0163(12) 0.0015(9) -0.0004(10) -0.0077(9) C46 0.0146(11) 0.0123(10) 0.0138(11) 0.0072(9) -0.0029(9) -0.0036(8) C47 0.0202(12) 0.0185(12) 0.0169(12) -0.0004(9) -0.0039(10) 0.0018(10) C48 0.0180(12) 0.0175(12) 0.0258(14) 0.0012(10) -0.0019(11) 0.0036(10) C49 0.0116(11) 0.0186(12) 0.0376(16) 0.0038(11) -0.0024(11) -0.0011(9) C50 0.0186(12) 0.0127(10) 0.0151(12) -0.0006(9) -0.0077(10) -0.0051(9) C51 0.0093(10) 0.0107(10) 0.0132(10) 0.0000(8) 0.0002(9) -0.0030(8) C52 0.0132(11) 0.0191(11) 0.0156(11) -0.0001(9) -0.0014(10) -0.0017(9) C53 0.0128(11) 0.0177(11) 0.0208(12) 0.0056(9) -0.0029(10) 0.0004(9) C54 0.0222(13) 0.0075(10) 0.0323(15) 0.0003(10) -0.0099(11) -0.0001(9) C55 0.0127(10) 0.0057(9) 0.0083(9) 0.0017(7) 0.0004(8) 0.0011(8) C56 0.0113(10) 0.0058(9) 0.0141(11) -0.0002(8) 0.0000(9) 0.0004(8) C57 0.0087(10) 0.0074(9) 0.0127(10) 0.0021(8) 0.0022(9) 0.0006(8) C58 0.0111(11) 0.0123(10) 0.0161(11) -0.0006(9) -0.0014(9) -0.0040(8) C59 0.0114(11) 0.0089(10) 0.0190(12) 0.0022(9) -0.0009(9) -0.0047(8) C60 0.0137(11) 0.0149(11) 0.0160(11) 0.0018(9) 0.0055(9) -0.0011(9) C61 0.0146(11) 0.0089(9) 0.0119(10) -0.0028(8) 0.0000(9) 0.0010(8) C62 0.0287(14) 0.0136(11) 0.0106(11) -0.0052(9) -0.0017(11) 0.0048(10) C63 0.071(3) 0.0415(19) 0.0149(14) -0.0095(13) -0.0116(16) 0.0392(19) C64 0.087(3) 0.0157(13) 0.0116(12) 0.0004(10) -0.0058(16) 0.0072(15) C65 0.0426(19) 0.049(2) 0.0227(15) -0.0040(14) 0.0087(15) -0.0257(16) C66 0.0058(9) 0.0119(10) 0.0118(10) -0.0022(8) -0.0034(8) 0.0024(8) C67 0.0188(12) 0.0160(11) 0.0133(11) -0.0070(9) -0.0033(10) -0.0004(9) C68 0.0244(13) 0.0087(10) 0.0237(13) -0.0011(9) 0.0089(11) -0.0013(9) C69 0.0197(12) 0.0060(9) 0.0248(13) -0.0029(9) -0.0002(10) 0.0008(9) C70 0.0119(11) 0.0155(11) 0.0140(11) 0.0006(9) 0.0061(9) 0.0076(9) C71 0.0264(14) 0.0179(12) 0.0150(12) 0.0034(9) 0.0024(11) 0.0088(10) N42 0.088(3) 0.0506(19) 0.0251(15) 0.0125(14) -0.0219(18) -0.020(2) C74 0.047(2) 0.052(2) 0.0267(17) 0.0208(17) -0.0160(17) -0.0241(19) C75 0.0248(17) 0.081(3) 0.051(2) 0.037(2) -0.0059(16) -0.0149(18) N43 0.062(2) 0.0425(16) 0.0261(14) 0.0067(12) -0.0042(16) -0.0081(15) C76 0.0474(19) 0.0233(14) 0.0190(14) 0.0042(11) 0.0131(14) 0.0026(13) C77 0.049(2) 0.047(2) 0.0319(18) 0.0037(15) 0.0025(17) 0.0057(17) N44 0.046(2) 0.061(2) 0.0454(18) -0.0078(16) 0.0181(16) -0.0033(16) C78 0.0385(19) 0.0316(15) 0.0205(14) -0.0042(11) 0.0051(14) -0.0082(13) C79 0.0312(17) 0.0362(17) 0.047(2) 0.0051(15) -0.0002(16) -0.0068(14) N45 0.0434(17) 0.0490(17) 0.0293(15) 0.0062(13) -0.0006(13) 0.0044(14) C80 0.0223(13) 0.0230(13) 0.0272(15) 0.0070(11) 0.0058(12) -0.0023(11) C81 0.0396(18) 0.0247(14) 0.0271(15) -0.0009(12) -0.0019(14) -0.0042(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.1221(19) . ? Fe1 N4 2.1253(19) . ? Fe1 O1 2.1852(18) . ? Fe1 N6 2.1881(19) . ? Fe1 O3 2.1927(16) . ? Fe1 O4 2.3924(18) . ? Fe2 O2 2.0541(18) . ? Fe2 N2 2.1296(18) . ? Fe2 N9 2.195(2) . ? Fe2 O5 2.2047(18) . ? Fe2 O3 2.2286(16) . ? Fe2 O6 2.2660(17) . ? Fe11 N21 2.0776(19) . ? Fe11 N26 2.080(2) . ? Fe11 N24 2.084(2) . ? Fe11 O11 2.0915(16) . ? Fe12 O13 2.0108(18) . ? Fe12 N22 2.1144(19) . ? Fe12 O15 2.1669(17) . ? Fe12 N29 2.188(2) . ? Fe12 O11 2.2710(16) . ? N1 C2 1.342(3) . ? N1 N2 1.372(2) . ? N2 C3 1.360(3) . ? N3 C4 1.462(3) . ? N3 C5 1.463(3) . ? N3 C10 1.467(3) . ? N4 C6 1.320(3) . ? N4 C7 1.376(3) . ? N5 C6 1.355(3) . ? N5 C8 1.373(4) . ? N5 C9 1.468(3) . ? N6 C11 1.311(3) . ? N6 C12 1.383(3) . ? N7 C11 1.355(3) . ? N7 C13 1.380(3) . ? N7 C14 1.456(3) . ? N8 C16 1.480(3) . ? N8 C21 1.480(3) . ? N8 C15 1.481(3) . ? N9 C17 1.331(3) . ? N9 C18 1.386(3) . ? N10 C17 1.350(3) . ? N10 C19 1.380(3) . ? N10 C20 1.455(3) . ? N11 C22 1.326(3) . ? N11 C23 1.372(4) . ? N12 C22 1.359(3) . ? N12 C24 1.373(3) . ? N12 C25 1.470(3) . ? N21 C42 1.346(3) . ? N21 N22 1.365(3) . ? N22 C43 1.355(3) . ? N23 C45 1.468(3) . ? N23 C50 1.471(3) . ? N23 C44 1.478(3) . ? N24 C46 1.328(3) . ? N24 C47 1.380(3) . ? N25 C46 1.348(3) . ? N25 C48 1.374(4) . ? N25 C49 1.461(3) . ? N26 C51 1.326(3) . ? N26 C52 1.373(3) . ? N27 C51 1.355(3) . ? N27 C53 1.370(3) . ? N27 C54 1.467(3) . ? N28 C61 1.477(3) . ? N28 C56 1.478(3) . ? N28 C55 1.488(3) . ? N29 C57 1.327(3) . ? N29 C58 1.384(3) . ? N30 C57 1.364(3) . ? N30 C59 1.368(3) . ? N30 C60 1.455(3) . ? N31 C62 1.321(4) . ? N31 C63 1.378(4) . ? N32 C62 1.364(4) . ? N32 C64 1.392(4) . ? N32 C65 1.455(5) . ? O1 C26 1.239(3) . ? O2 C26 1.266(3) . ? O3 C28 1.287(3) . ? O4 C28 1.247(3) . ? O5 C30 1.265(3) . ? O6 C30 1.255(3) . ? O11 C66 1.297(3) . ? O12 C66 1.238(3) . ? O13 C68 1.270(3) . ? O14A C68 1.244(4) . ? O14B C68 1.31(2) . ? O15 C70 1.254(3) . ? O16 C70 1.262(3) . ? C1 C2 1.386(3) . ? C1 C3 1.401(3) . ? C2 C4 1.505(3) . ? C3 C15 1.500(3) . ? C5 C6 1.498(3) . ? C7 C8 1.360(4) . ? C10 C11 1.500(3) . ? C12 C13 1.356(4) . ? C16 C17 1.488(3) . ? C18 C19 1.349(4) . ? C21 C22 1.497(3) . ? C23 C24 1.361(4) . ? C26 C27 1.520(3) . ? C28 C29 1.511(3) . ? C30 C31 1.517(3) . ? C41 C42 1.388(3) . ? C41 C43 1.396(3) . ? C42 C44 1.504(3) . ? C43 C55 1.502(3) . ? C45 C46 1.499(3) . ? C47 C48 1.360(4) . ? C50 C51 1.503(3) . ? C52 C53 1.372(3) . ? C56 C57 1.496(3) . ? C58 C59 1.353(4) . ? C61 C62 1.492(3) . ? C63 C64 1.334(6) . ? C66 C67 1.502(3) . ? C68 C69 1.521(3) . ? C70 C71 1.512(3) . ? N42 C74 1.151(6) . ? C74 C75 1.446(7) . ? N43 C76 1.145(5) . ? C76 C77 1.446(5) . ? N44 C78 1.131(5) . ? C78 C79 1.442(5) . ? N45 C80 1.140(4) . ? C80 C81 1.460(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N4 125.65(7) . . ? N1 Fe1 O1 89.76(7) . . ? N4 Fe1 O1 81.89(7) . . ? N1 Fe1 N6 102.29(7) . . ? N4 Fe1 N6 92.30(7) . . ? O1 Fe1 N6 167.83(8) . . ? N1 Fe1 O3 84.87(6) . . ? N4 Fe1 O3 146.17(7) . . ? O1 Fe1 O3 84.32(6) . . ? N6 Fe1 O3 94.92(6) . . ? N1 Fe1 O4 141.83(6) . . ? N4 Fe1 O4 90.66(7) . . ? O1 Fe1 O4 83.72(7) . . ? N6 Fe1 O4 85.67(7) . . ? O3 Fe1 O4 57.11(6) . . ? O2 Fe2 N2 108.32(7) . . ? O2 Fe2 N9 86.79(7) . . ? N2 Fe2 N9 100.48(7) . . ? O2 Fe2 O5 155.60(7) . . ? N2 Fe2 O5 95.81(7) . . ? N9 Fe2 O5 92.43(7) . . ? O2 Fe2 O3 87.32(7) . . ? N2 Fe2 O3 84.37(6) . . ? N9 Fe2 O3 173.32(7) . . ? O5 Fe2 O3 91.63(6) . . ? O2 Fe2 O6 96.72(7) . . ? N2 Fe2 O6 154.01(7) . . ? N9 Fe2 O6 87.48(7) . . ? O5 Fe2 O6 58.89(7) . . ? O3 Fe2 O6 90.08(6) . . ? N21 Fe11 N26 113.45(8) . . ? N21 Fe11 N24 119.01(8) . . ? N26 Fe11 N24 101.19(8) . . ? N21 Fe11 O11 85.23(7) . . ? N26 Fe11 O11 136.33(7) . . ? N24 Fe11 O11 102.91(7) . . ? O13 Fe12 N22 122.34(7) . . ? O13 Fe12 O15 144.34(7) . . ? N22 Fe12 O15 91.08(7) . . ? O13 Fe12 N29 90.82(7) . . ? N22 Fe12 N29 98.84(7) . . ? O15 Fe12 N29 96.28(7) . . ? O13 Fe12 O11 88.39(7) . . ? N22 Fe12 O11 84.54(7) . . ? O15 Fe12 O11 82.36(6) . . ? N29 Fe12 O11 176.40(7) . . ? C2 N1 N2 108.37(17) . . ? C2 N1 Fe1 126.61(14) . . ? N2 N1 Fe1 124.90(13) . . ? C3 N2 N1 107.16(17) . . ? C3 N2 Fe2 133.84(14) . . ? N1 N2 Fe2 117.32(13) . . ? C4 N3 C5 114.30(17) . . ? C4 N3 C10 111.24(18) . . ? C5 N3 C10 114.06(17) . . ? C6 N4 C7 106.53(19) . . ? C6 N4 Fe1 125.52(16) . . ? C7 N4 Fe1 127.85(17) . . ? C6 N5 C8 107.5(2) . . ? C6 N5 C9 126.4(2) . . ? C8 N5 C9 126.0(2) . . ? C11 N6 C12 105.66(19) . . ? C11 N6 Fe1 123.09(15) . . ? C12 N6 Fe1 130.48(16) . . ? C11 N7 C13 106.5(2) . . ? C11 N7 C14 126.4(2) . . ? C13 N7 C14 127.1(2) . . ? C16 N8 C21 110.11(17) . . ? C16 N8 C15 110.66(17) . . ? C21 N8 C15 112.89(18) . . ? C17 N9 C18 104.96(19) . . ? C17 N9 Fe2 130.00(15) . . ? C18 N9 Fe2 124.76(16) . . ? C17 N10 C19 107.2(2) . . ? C17 N10 C20 125.7(2) . . ? C19 N10 C20 127.1(2) . . ? C22 N11 C23 104.7(2) . . ? C22 N12 C24 107.3(2) . . ? C22 N12 C25 126.6(2) . . ? C24 N12 C25 126.0(2) . . ? C42 N21 N22 108.78(18) . . ? C42 N21 Fe11 125.50(15) . . ? N22 N21 Fe11 125.50(14) . . ? C43 N22 N21 107.25(18) . . ? C43 N22 Fe12 136.00(15) . . ? N21 N22 Fe12 116.60(14) . . ? C45 N23 C50 113.91(18) . . ? C45 N23 C44 112.27(19) . . ? C50 N23 C44 112.64(19) . . ? C46 N24 C47 106.2(2) . . ? C46 N24 Fe11 121.81(17) . . ? C47 N24 Fe11 131.98(17) . . ? C46 N25 C48 107.7(2) . . ? C46 N25 C49 126.6(2) . . ? C48 N25 C49 125.7(2) . . ? C51 N26 C52 106.35(19) . . ? C51 N26 Fe11 118.85(16) . . ? C52 N26 Fe11 134.79(16) . . ? C51 N27 C53 107.51(19) . . ? C51 N27 C54 126.0(2) . . ? C53 N27 C54 126.5(2) . . ? C61 N28 C56 110.94(17) . . ? C61 N28 C55 111.75(18) . . ? C56 N28 C55 110.75(17) . . ? C57 N29 C58 105.12(19) . . ? C57 N29 Fe12 133.59(16) . . ? C58 N29 Fe12 120.65(16) . . ? C57 N30 C59 107.30(19) . . ? C57 N30 C60 127.0(2) . . ? C59 N30 C60 125.55(19) . . ? C62 N31 C63 105.2(3) . . ? C62 N32 C64 105.5(3) . . ? C62 N32 C65 126.5(2) . . ? C64 N32 C65 127.8(3) . . ? C26 O1 Fe1 137.59(15) . . ? C26 O2 Fe2 130.53(15) . . ? C28 O3 Fe1 95.31(13) . . ? C28 O3 Fe2 135.43(15) . . ? Fe1 O3 Fe2 109.63(7) . . ? C28 O4 Fe1 87.18(14) . . ? C30 O5 Fe2 91.04(15) . . ? C30 O6 Fe2 88.49(14) . . ? C66 O11 Fe11 101.88(14) . . ? C66 O11 Fe12 124.65(14) . . ? Fe11 O11 Fe12 107.69(7) . . ? C68 O13 Fe12 119.40(17) . . ? C70 O15 Fe12 96.45(15) . . ? C2 C1 C3 104.06(19) . . ? N1 C2 C1 110.47(18) . . ? N1 C2 C4 118.71(19) . . ? C1 C2 C4 130.66(19) . . ? N2 C3 C1 109.89(19) . . ? N2 C3 C15 121.58(19) . . ? C1 C3 C15 127.9(2) . . ? N3 C4 C2 109.25(17) . . ? N3 C5 C6 110.85(18) . . ? N4 C6 N5 110.5(2) . . ? N4 C6 C5 125.88(19) . . ? N5 C6 C5 123.6(2) . . ? C8 C7 N4 109.2(2) . . ? C7 C8 N5 106.3(2) . . ? N3 C10 C11 110.17(18) . . ? N6 C11 N7 111.9(2) . . ? N6 C11 C10 124.81(19) . . ? N7 C11 C10 123.3(2) . . ? C13 C12 N6 109.6(2) . . ? C12 C13 N7 106.4(2) . . ? N8 C15 C3 112.90(17) . . ? N8 C16 C17 109.43(17) . . ? N9 C17 N10 111.4(2) . . ? N9 C17 C16 127.0(2) . . ? N10 C17 C16 121.5(2) . . ? C19 C18 N9 110.3(2) . . ? C18 C19 N10 106.2(2) . . ? N8 C21 C22 109.99(19) . . ? N11 C22 N12 111.5(2) . . ? N11 C22 C21 124.7(2) . . ? N12 C22 C21 123.6(2) . . ? C24 C23 N11 111.2(2) . . ? C23 C24 N12 105.3(2) . . ? O1 C26 O2 126.4(2) . . ? O1 C26 C27 116.6(2) . . ? O2 C26 C27 117.0(2) . . ? O4 C28 O3 120.4(2) . . ? O4 C28 C29 121.2(2) . . ? O3 C28 C29 118.3(2) . . ? O6 C30 O5 121.5(2) . . ? O6 C30 C31 119.5(2) . . ? O5 C30 C31 119.0(3) . . ? C42 C41 C43 104.39(19) . . ? N21 C42 C41 109.68(19) . . ? N21 C42 C44 118.54(19) . . ? C41 C42 C44 131.3(2) . . ? N22 C43 C41 109.90(19) . . ? N22 C43 C55 121.28(19) . . ? C41 C43 C55 128.8(2) . . ? N23 C44 C42 109.91(18) . . ? N23 C45 C46 109.86(19) . . ? N24 C46 N25 110.6(2) . . ? N24 C46 C45 124.0(2) . . ? N25 C46 C45 125.1(2) . . ? C48 C47 N24 109.2(2) . . ? C47 C48 N25 106.3(2) . . ? N23 C50 C51 109.07(19) . . ? N26 C51 N27 110.7(2) . . ? N26 C51 C50 123.9(2) . . ? N27 C51 C50 125.3(2) . . ? C53 C52 N26 109.2(2) . . ? N27 C53 C52 106.2(2) . . ? N28 C55 C43 114.91(17) . . ? N28 C56 C57 110.49(17) . . ? N29 C57 N30 111.0(2) . . ? N29 C57 C56 126.1(2) . . ? N30 C57 C56 122.9(2) . . ? C59 C58 N29 110.3(2) . . ? C58 C59 N30 106.3(2) . . ? N28 C61 C62 110.96(18) . . ? N31 C62 N32 111.8(2) . . ? N31 C62 C61 125.7(3) . . ? N32 C62 C61 122.4(2) . . ? C64 C63 N31 110.7(3) . . ? C63 C64 N32 106.8(3) . . ? O12 C66 O11 120.8(2) . . ? O12 C66 C67 122.4(2) . . ? O11 C66 C67 116.8(2) . . ? O14A C68 O13 124.9(2) . . ? O14A C68 O14B 42.1(11) . . ? O13 C68 O14B 116.5(9) . . ? O14A C68 C69 119.2(2) . . ? O13 C68 C69 115.5(2) . . ? O14B C68 C69 114.2(8) . . ? O15 C70 O16 120.9(2) . . ? O15 C70 C71 120.0(2) . . ? O16 C70 C71 119.1(2) . . ? N42 C74 C75 179.2(4) . . ? N43 C76 C77 179.5(4) . . ? N44 C78 C79 177.5(4) . . ? N45 C80 C81 177.9(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.92 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.174 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.068