[Fe2(m-O2CArTol)2(O2CArTol)2(2-Bnan)2] (5) data_071502 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H94 Fe2 N2 O8' _chemical_formula_weight 1683.57 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.774(3) _cell_length_b 23.088(5) _cell_length_c 14.488(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.498(4) _cell_angle_gamma 90.00 _cell_volume 4394.4(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4804 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 23.46 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.392 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32331 _diffrn_reflns_av_R_equivalents 0.0791 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7741 _reflns_number_gt 6081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7741 _refine_ls_number_parameters 554 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.004 _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 0.41394(3) 0.572784(16) 0.46382(3) 0.02302(12) Uani 1 1 d . . . N1 N 0.28479(18) 0.55129(10) 0.51441(19) 0.0369(7) Uani 1 1 d . . . H1A H 0.2562 0.5178 0.4835 0.044 Uiso 1 1 calc R . . H1B H 0.3097 0.5428 0.5793 0.044 Uiso 1 1 calc R . . O1 O 0.51307(15) 0.58391(9) 0.59343(14) 0.0383(5) Uani 1 1 d . . . O2 O 0.39495(17) 0.49599(9) 0.39857(15) 0.0432(6) Uani 1 1 d . . . O3 O 0.35900(14) 0.65026(8) 0.39442(14) 0.0304(5) Uani 1 1 d . . . O4 O 0.48615(14) 0.60883(8) 0.35883(14) 0.0299(5) Uani 1 1 d . . . C1 C 0.2041(2) 0.59308(12) 0.5025(2) 0.0304(7) Uani 1 1 d . . . C2 C 0.1841(2) 0.61818(12) 0.5826(2) 0.0283(7) Uani 1 1 d . . . C3 C 0.1067(2) 0.65902(12) 0.5651(2) 0.0318(7) Uani 1 1 d . . . H3A H 0.0905 0.6761 0.6183 0.038 Uiso 1 1 calc R . . C4 C 0.0527(2) 0.67532(14) 0.4721(2) 0.0410(8) Uani 1 1 d . . . H4A H 0.0002 0.7035 0.4616 0.049 Uiso 1 1 calc R . . C5 C 0.0754(2) 0.65056(16) 0.3946(2) 0.0458(9) Uani 1 1 d . . . H5A H 0.0391 0.6620 0.3305 0.055 Uiso 1 1 calc R . . C6 C 0.1502(2) 0.60945(15) 0.4099(2) 0.0405(8) Uani 1 1 d . . . H6A H 0.1651 0.5921 0.3562 0.049 Uiso 1 1 calc R . . C7 C 0.2458(2) 0.60089(13) 0.6844(2) 0.0356(8) Uani 1 1 d . . . H7A H 0.2420 0.5583 0.6907 0.043 Uiso 1 1 calc R . . H7B H 0.3180 0.6112 0.6942 0.043 Uiso 1 1 calc R . . C8 C 0.2113(2) 0.62887(13) 0.7627(2) 0.0314(7) Uani 1 1 d . . . C9 C 0.1439(2) 0.60166(14) 0.8025(2) 0.0362(8) Uani 1 1 d . . . H9A H 0.1207 0.5637 0.7815 0.043 Uiso 1 1 calc R . . C10 C 0.1094(2) 0.62847(15) 0.8722(2) 0.0420(8) Uani 1 1 d . . . H10A H 0.0653 0.6085 0.9006 0.050 Uiso 1 1 calc R . . C11 C 0.1397(3) 0.68452(16) 0.9002(2) 0.0468(9) Uani 1 1 d . . . H11A H 0.1143 0.7038 0.9462 0.056 Uiso 1 1 calc R . . C12 C 0.2070(3) 0.71243(15) 0.8612(2) 0.0484(9) Uani 1 1 d . . . H12A H 0.2278 0.7510 0.8802 0.058 Uiso 1 1 calc R . . C13 C 0.2436(2) 0.68450(14) 0.7950(2) 0.0392(8) Uani 1 1 d . . . H13A H 0.2920 0.7035 0.7707 0.047 Uiso 1 1 calc R . . C14 C 0.4095(2) 0.44677(13) 0.3698(2) 0.0289(7) Uani 1 1 d . . . C15 C 0.3278(2) 0.42147(11) 0.2870(2) 0.0259(6) Uani 1 1 d . . . C16 C 0.2347(2) 0.40617(12) 0.3023(2) 0.0311(7) Uani 1 1 d . . . C17 C 0.1592(2) 0.38258(13) 0.2251(2) 0.0400(8) Uani 1 1 d . . . H17A H 0.0965 0.3710 0.2343 0.048 Uiso 1 1 calc R . . C18 C 0.1733(3) 0.37572(14) 0.1360(2) 0.0447(9) Uani 1 1 d . . . H18A H 0.1199 0.3603 0.0840 0.054 Uiso 1 1 calc R . . C19 C 0.2642(3) 0.39106(13) 0.1214(2) 0.0396(8) Uani 1 1 d . . . H19A H 0.2732 0.3858 0.0594 0.048 Uiso 1 1 calc R . . C20 C 0.3435(2) 0.41434(11) 0.1968(2) 0.0289(7) Uani 1 1 d . . . C21 C 0.2142(2) 0.41310(11) 0.3977(2) 0.0283(7) Uani 1 1 d . . . C22 C 0.2855(2) 0.39847(12) 0.4849(2) 0.0305(7) Uani 1 1 d . . . H22A H 0.3494 0.3830 0.4849 0.037 Uiso 1 1 calc R . . C23 C 0.2646(2) 0.40606(12) 0.5717(2) 0.0332(7) Uani 1 1 d . . . H23A H 0.3155 0.3968 0.6304 0.040 Uiso 1 1 calc R . . C24 C 0.1713(2) 0.42685(13) 0.5753(2) 0.0375(8) Uani 1 1 d . . . C25 C 0.1000(2) 0.44016(13) 0.4883(3) 0.0409(8) Uani 1 1 d . . . H25A H 0.0348 0.4537 0.4883 0.049 Uiso 1 1 calc R . . C26 C 0.1209(2) 0.43425(13) 0.4011(2) 0.0389(8) Uani 1 1 d . . . H26A H 0.0707 0.4448 0.3427 0.047 Uiso 1 1 calc R . . C27 C 0.1489(3) 0.43378(16) 0.6701(3) 0.0537(10) Uani 1 1 d . . . H27A H 0.0872 0.4571 0.6602 0.080 Uiso 1 1 calc R . . H27B H 0.2063 0.4532 0.7167 0.080 Uiso 1 1 calc R . . H27C H 0.1386 0.3956 0.6950 0.080 Uiso 1 1 calc R . . C28 C 0.4373(2) 0.43366(12) 0.1747(2) 0.0296(7) Uani 1 1 d . . . C29 C 0.4819(2) 0.48715(13) 0.2041(2) 0.0308(7) Uani 1 1 d . . . H29A H 0.4588 0.5101 0.2477 0.037 Uiso 1 1 calc R . . C30 C 0.5596(2) 0.50728(14) 0.1707(2) 0.0386(8) Uani 1 1 d . . . H30A H 0.5880 0.5443 0.1910 0.046 Uiso 1 1 calc R . . C31 C 0.5975(2) 0.47505(16) 0.1083(2) 0.0427(9) Uani 1 1 d . . . C32 C 0.5564(3) 0.42028(16) 0.0828(2) 0.0460(9) Uani 1 1 d . . . H32A H 0.5826 0.3964 0.0425 0.055 Uiso 1 1 calc R . . C33 C 0.4781(3) 0.40002(14) 0.1150(2) 0.0397(8) Uani 1 1 d . . . H33A H 0.4513 0.3624 0.0962 0.048 Uiso 1 1 calc R . . C34 C 0.6775(3) 0.49909(18) 0.0670(2) 0.0579(11) Uani 1 1 d . . . H34A H 0.6445 0.5161 0.0033 0.087 Uiso 1 1 calc R . . H34B H 0.7231 0.4678 0.0604 0.087 Uiso 1 1 calc R . . H34C H 0.7169 0.5290 0.1104 0.087 Uiso 1 1 calc R . . C35 C 0.4217(2) 0.64855(12) 0.3457(2) 0.0246(6) Uani 1 1 d . . . C36 C 0.4161(2) 0.69446(12) 0.2703(2) 0.0256(7) Uani 1 1 d . . . C37 C 0.3324(2) 0.69549(12) 0.1864(2) 0.0279(7) Uani 1 1 d . . . C38 C 0.3293(2) 0.73788(12) 0.1173(2) 0.0344(7) Uani 1 1 d . . . H38A H 0.2730 0.7391 0.0601 0.041 Uiso 1 1 calc R . . C39 C 0.4062(2) 0.77814(13) 0.1303(2) 0.0372(8) Uani 1 1 d . . . H39A H 0.4030 0.8064 0.0818 0.045 Uiso 1 1 calc R . . C40 C 0.4870(2) 0.77740(12) 0.2128(2) 0.0345(8) Uani 1 1 d . . . H40A H 0.5392 0.8056 0.2216 0.041 Uiso 1 1 calc R . . C41 C 0.4940(2) 0.73558(12) 0.2846(2) 0.0287(7) Uani 1 1 d . . . C42 C 0.2470(2) 0.65336(12) 0.16987(19) 0.0279(7) Uani 1 1 d . . . C43 C 0.2622(2) 0.59414(13) 0.1683(2) 0.0361(8) Uani 1 1 d . . . H43A H 0.3292 0.5797 0.1783 0.043 Uiso 1 1 calc R . . C44 C 0.1819(3) 0.55560(13) 0.1525(2) 0.0407(8) Uani 1 1 d . . . H44A H 0.1947 0.5152 0.1525 0.049 Uiso 1 1 calc R . . C45 C 0.0834(2) 0.57499(14) 0.1365(2) 0.0372(8) Uani 1 1 d . . . C46 C 0.0677(2) 0.63416(14) 0.1362(2) 0.0386(8) Uani 1 1 d . . . H46A H 0.0005 0.6486 0.1245 0.046 Uiso 1 1 calc R . . C47 C 0.1478(2) 0.67253(13) 0.1524(2) 0.0334(7) Uani 1 1 d . . . H47A H 0.1347 0.7130 0.1516 0.040 Uiso 1 1 calc R . . C48 C -0.0045(3) 0.53333(15) 0.1214(3) 0.0562(10) Uani 1 1 d . . . H48A H 0.0208 0.4935 0.1250 0.084 Uiso 1 1 calc R . . H48B H -0.0537 0.5400 0.0576 0.084 Uiso 1 1 calc R . . H48C H -0.0377 0.5394 0.1717 0.084 Uiso 1 1 calc R . . C49 C 0.5802(2) 0.73867(12) 0.3753(2) 0.0313(7) Uani 1 1 d . . . C50 C 0.5641(2) 0.74278(13) 0.4654(2) 0.0383(8) Uani 1 1 d . . . H50A H 0.4967 0.7413 0.4696 0.046 Uiso 1 1 calc R . . C51 C 0.6446(3) 0.74897(14) 0.5487(3) 0.0492(9) Uani 1 1 d . . . H51A H 0.6314 0.7524 0.6091 0.059 Uiso 1 1 calc R . . C52 C 0.7436(3) 0.75033(15) 0.5463(3) 0.0557(11) Uani 1 1 d . . . C53 C 0.7599(3) 0.74601(14) 0.4574(3) 0.0549(11) Uani 1 1 d . . . H53A H 0.8277 0.7468 0.4541 0.066 Uiso 1 1 calc R . . C54 C 0.6802(2) 0.74051(13) 0.3726(3) 0.0436(9) Uani 1 1 d . . . H54A H 0.6940 0.7380 0.3123 0.052 Uiso 1 1 calc R . . C55 C 0.8317(3) 0.75655(19) 0.6379(3) 0.0865(16) Uani 1 1 d . . . H55A H 0.8395 0.7974 0.6573 0.130 Uiso 1 1 calc R . . H55B H 0.8943 0.7428 0.6262 0.130 Uiso 1 1 calc R . . H55C H 0.8183 0.7335 0.6896 0.130 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0243(2) 0.0198(2) 0.0252(2) 0.00223(18) 0.00799(17) 0.00150(17) N1 0.0412(16) 0.0261(14) 0.0533(18) -0.0061(12) 0.0294(14) -0.0060(12) O1 0.0288(12) 0.0598(15) 0.0233(11) 0.0003(10) 0.0032(9) 0.0048(11) O2 0.0631(16) 0.0274(12) 0.0485(15) -0.0170(11) 0.0311(12) -0.0171(11) O3 0.0320(12) 0.0300(12) 0.0336(12) 0.0087(9) 0.0163(10) 0.0051(9) O4 0.0306(12) 0.0248(11) 0.0378(12) 0.0064(9) 0.0158(10) 0.0052(9) C1 0.0239(16) 0.0286(17) 0.043(2) -0.0066(14) 0.0170(15) -0.0094(13) C2 0.0259(16) 0.0264(16) 0.0338(18) 0.0002(13) 0.0110(14) -0.0042(13) C3 0.0311(18) 0.0318(18) 0.0345(19) -0.0037(14) 0.0130(15) -0.0023(14) C4 0.0277(18) 0.048(2) 0.046(2) 0.0081(17) 0.0103(16) 0.0028(15) C5 0.0319(19) 0.070(3) 0.033(2) 0.0093(18) 0.0056(16) -0.0058(18) C6 0.037(2) 0.054(2) 0.035(2) -0.0127(17) 0.0172(16) -0.0129(17) C7 0.0328(18) 0.0348(18) 0.040(2) 0.0038(15) 0.0121(15) 0.0027(14) C8 0.0274(17) 0.0354(18) 0.0276(17) 0.0045(14) 0.0023(14) 0.0021(14) C9 0.0325(18) 0.0373(19) 0.0344(19) 0.0017(15) 0.0034(15) -0.0050(15) C10 0.0339(19) 0.057(2) 0.035(2) 0.0036(17) 0.0099(16) -0.0076(16) C11 0.052(2) 0.060(2) 0.0302(19) -0.0102(17) 0.0144(17) -0.0048(19) C12 0.072(3) 0.038(2) 0.034(2) -0.0072(16) 0.0158(19) -0.0129(18) C13 0.046(2) 0.038(2) 0.0344(19) 0.0050(15) 0.0133(16) -0.0107(16) C14 0.0333(18) 0.0334(18) 0.0245(17) -0.0031(14) 0.0156(14) -0.0074(14) C15 0.0341(17) 0.0114(14) 0.0286(16) 0.0009(12) 0.0041(13) 0.0041(12) C16 0.0291(17) 0.0239(16) 0.0352(18) 0.0012(13) 0.0019(14) 0.0020(13) C17 0.037(2) 0.0356(19) 0.041(2) 0.0016(16) 0.0021(16) -0.0036(15) C18 0.049(2) 0.038(2) 0.035(2) -0.0060(16) -0.0041(17) -0.0051(17) C19 0.053(2) 0.0346(19) 0.0260(18) -0.0032(14) 0.0048(16) 0.0012(16) C20 0.0399(18) 0.0146(15) 0.0288(17) -0.0005(12) 0.0051(14) 0.0051(13) C21 0.0264(16) 0.0186(15) 0.0389(18) 0.0003(13) 0.0085(14) -0.0068(12) C22 0.0274(17) 0.0254(16) 0.0379(19) 0.0000(14) 0.0085(14) -0.0024(13) C23 0.0364(19) 0.0267(17) 0.0363(19) 0.0026(14) 0.0107(15) -0.0028(14) C24 0.041(2) 0.0284(17) 0.047(2) -0.0075(16) 0.0193(17) -0.0120(15) C25 0.0294(18) 0.0350(19) 0.063(2) -0.0072(17) 0.0209(18) -0.0027(14) C26 0.0296(18) 0.0354(19) 0.047(2) -0.0039(16) 0.0039(15) -0.0006(14) C27 0.054(2) 0.059(2) 0.058(2) -0.011(2) 0.032(2) -0.0120(19) C28 0.0375(18) 0.0256(16) 0.0232(16) 0.0038(13) 0.0056(13) 0.0122(14) C29 0.0338(18) 0.0348(18) 0.0234(17) 0.0018(14) 0.0080(14) 0.0087(14) C30 0.039(2) 0.042(2) 0.0316(19) 0.0092(15) 0.0057(16) 0.0055(16) C31 0.036(2) 0.063(2) 0.0277(19) 0.0195(17) 0.0069(15) 0.0171(17) C32 0.055(2) 0.059(2) 0.0270(18) 0.0075(17) 0.0166(17) 0.0268(19) C33 0.054(2) 0.0335(19) 0.0287(18) 0.0015(15) 0.0088(16) 0.0143(16) C34 0.043(2) 0.089(3) 0.044(2) 0.027(2) 0.0161(18) 0.016(2) C35 0.0217(15) 0.0221(16) 0.0279(17) -0.0048(13) 0.0044(13) -0.0035(13) C36 0.0316(17) 0.0205(15) 0.0276(17) 0.0020(12) 0.0134(14) 0.0049(13) C37 0.0348(18) 0.0229(16) 0.0282(17) -0.0005(13) 0.0128(14) 0.0026(13) C38 0.045(2) 0.0309(18) 0.0271(17) 0.0033(14) 0.0101(15) 0.0051(15) C39 0.054(2) 0.0297(18) 0.0334(19) 0.0087(14) 0.0210(17) 0.0052(16) C40 0.043(2) 0.0258(17) 0.043(2) 0.0053(15) 0.0245(17) -0.0025(14) C41 0.0318(17) 0.0250(16) 0.0328(17) 0.0011(13) 0.0148(14) 0.0021(13) C42 0.0362(18) 0.0265(16) 0.0189(15) 0.0030(12) 0.0051(13) 0.0041(13) C43 0.0307(18) 0.0330(18) 0.0391(19) -0.0005(15) 0.0020(15) 0.0050(14) C44 0.052(2) 0.0252(18) 0.040(2) -0.0010(15) 0.0058(17) 0.0020(16) C45 0.043(2) 0.041(2) 0.0277(17) -0.0027(15) 0.0102(15) -0.0089(16) C46 0.0328(19) 0.046(2) 0.038(2) -0.0010(16) 0.0105(15) 0.0019(16) C47 0.0385(19) 0.0261(17) 0.0338(18) -0.0005(14) 0.0081(15) 0.0044(14) C48 0.058(3) 0.053(2) 0.059(3) -0.0048(19) 0.020(2) -0.0181(19) C49 0.0331(18) 0.0208(16) 0.0414(19) 0.0040(14) 0.0137(15) -0.0041(13) C50 0.037(2) 0.0327(18) 0.043(2) 0.0017(15) 0.0101(17) -0.0105(15) C51 0.057(2) 0.044(2) 0.042(2) 0.0031(17) 0.0082(19) -0.0200(18) C52 0.050(2) 0.038(2) 0.066(3) 0.0157(19) -0.002(2) -0.0194(18) C53 0.032(2) 0.037(2) 0.092(3) 0.016(2) 0.013(2) -0.0069(16) C54 0.039(2) 0.0353(19) 0.058(2) 0.0060(17) 0.0182(18) -0.0034(16) C55 0.066(3) 0.084(3) 0.081(3) 0.025(3) -0.020(2) -0.031(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.978(2) . ? Fe1 O2 1.989(2) . ? Fe1 O3 2.0798(19) . ? Fe1 N1 2.175(2) . ? Fe1 O4 2.2150(19) . ? Fe1 C35 2.472(3) . ? Fe1 Fe1 4.0646(10) 3_666 ? Fe1 C7 4.522(3) . ? N1 C1 1.442(4) . ? O1 C14 1.258(3) 3_666 ? O2 C14 1.247(3) . ? O3 C35 1.269(3) . ? O4 C35 1.251(3) . ? C1 C6 1.377(4) . ? C1 C2 1.398(4) . ? C2 C3 1.389(4) . ? C2 C7 1.517(4) . ? C3 C4 1.382(4) . ? C4 C5 1.377(4) . ? C5 C6 1.370(4) . ? C7 C8 1.501(4) . ? C8 C9 1.382(4) . ? C8 C13 1.393(4) . ? C9 C10 1.385(4) . ? C10 C11 1.383(4) . ? C11 C12 1.381(4) . ? C12 C13 1.372(4) . ? C14 O1 1.258(3) 3_666 ? C14 C15 1.495(4) . ? C15 C20 1.397(4) . ? C15 C16 1.410(4) . ? C16 C17 1.389(4) . ? C16 C21 1.501(4) . ? C17 C18 1.371(4) . ? C18 C19 1.378(4) . ? C19 C20 1.399(4) . ? C20 C28 1.490(4) . ? C21 C22 1.388(4) . ? C21 C26 1.389(4) . ? C22 C23 1.383(4) . ? C23 C24 1.387(4) . ? C24 C25 1.379(4) . ? C24 C27 1.504(4) . ? C25 C26 1.385(4) . ? C28 C29 1.388(4) . ? C28 C33 1.400(4) . ? C29 C30 1.381(4) . ? C30 C31 1.388(4) . ? C31 C32 1.390(5) . ? C31 C34 1.510(4) . ? C32 C33 1.378(4) . ? C35 C36 1.508(4) . ? C36 C41 1.400(4) . ? C36 C37 1.402(4) . ? C37 C38 1.391(4) . ? C37 C42 1.489(4) . ? C38 C39 1.379(4) . ? C39 C40 1.368(4) . ? C40 C41 1.401(4) . ? C41 C49 1.484(4) . ? C42 C43 1.385(4) . ? C42 C47 1.385(4) . ? C43 C44 1.384(4) . ? C44 C45 1.380(4) . ? C45 C46 1.383(4) . ? C45 C48 1.510(4) . ? C46 C47 1.379(4) . ? C49 C50 1.391(4) . ? C49 C54 1.391(4) . ? C50 C51 1.379(4) . ? C51 C52 1.375(5) . ? C52 C53 1.376(5) . ? C52 C55 1.512(5) . ? C53 C54 1.386(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 O1 Fe1 O2 121.42(9) . . ? O1 Fe1 O3 113.22(9) . . ? O2 Fe1 O3 124.06(9) . . ? O1 Fe1 N1 96.36(9) . . ? O2 Fe1 N1 87.29(9) . . ? O3 Fe1 N1 98.26(9) . . ? O1 Fe1 O4 106.18(8) . . ? O2 Fe1 O4 91.75(8) . . ? O3 Fe1 O4 61.18(7) . . ? N1 Fe1 O4 153.99(9) . . ? O1 Fe1 C35 113.83(9) . . ? O2 Fe1 C35 109.19(9) . . ? O3 Fe1 C35 30.88(8) . . ? N1 Fe1 C35 127.21(9) . . ? O4 Fe1 C35 30.32(7) . . ? O1 Fe1 Fe1 71.33(6) . 3_666 ? O2 Fe1 Fe1 50.85(7) . 3_666 ? O3 Fe1 Fe1 159.23(6) . 3_666 ? N1 Fe1 Fe1 101.37(7) . 3_666 ? O4 Fe1 Fe1 98.06(5) . 3_666 ? C35 Fe1 Fe1 128.35(7) . 3_666 ? O1 Fe1 C7 70.41(7) . . ? O2 Fe1 C7 116.21(7) . . ? O3 Fe1 C7 91.67(7) . . ? N1 Fe1 C7 31.81(8) . . ? O4 Fe1 C7 149.61(6) . . ? C35 Fe1 C7 121.71(8) . . ? Fe1 Fe1 C7 108.63(4) 3_666 . ? C1 N1 Fe1 119.05(18) . . ? C14 O1 Fe1 125.76(19) 3_666 . ? C14 O2 Fe1 163.7(2) . . ? C35 O3 Fe1 91.86(16) . . ? C35 O4 Fe1 86.26(16) . . ? C6 C1 C2 120.9(3) . . ? C6 C1 N1 118.1(3) . . ? C2 C1 N1 121.0(3) . . ? C3 C2 C1 117.5(3) . . ? C3 C2 C7 122.1(3) . . ? C1 C2 C7 120.4(3) . . ? C4 C3 C2 121.4(3) . . ? C5 C4 C3 119.7(3) . . ? C6 C5 C4 120.0(3) . . ? C5 C6 C1 120.5(3) . . ? C8 C7 C2 114.2(2) . . ? C8 C7 Fe1 160.3(2) . . ? C2 C7 Fe1 66.87(15) . . ? C9 C8 C13 117.8(3) . . ? C9 C8 C7 121.6(3) . . ? C13 C8 C7 120.6(3) . . ? C8 C9 C10 121.4(3) . . ? C11 C10 C9 119.6(3) . . ? C12 C11 C10 119.8(3) . . ? C13 C12 C11 120.0(3) . . ? C12 C13 C8 121.4(3) . . ? O2 C14 O1 124.9(3) . 3_666 ? O2 C14 C15 117.8(3) . . ? O1 C14 C15 117.2(3) 3_666 . ? C20 C15 C16 121.4(3) . . ? C20 C15 C14 120.4(3) . . ? C16 C15 C14 118.2(3) . . ? C17 C16 C15 117.9(3) . . ? C17 C16 C21 118.7(3) . . ? C15 C16 C21 123.3(3) . . ? C18 C17 C16 121.3(3) . . ? C17 C18 C19 120.5(3) . . ? C18 C19 C20 120.7(3) . . ? C15 C20 C19 118.1(3) . . ? C15 C20 C28 123.7(3) . . ? C19 C20 C28 118.1(3) . . ? C22 C21 C26 117.5(3) . . ? C22 C21 C16 122.3(3) . . ? C26 C21 C16 120.1(3) . . ? C23 C22 C21 120.9(3) . . ? C22 C23 C24 121.8(3) . . ? C25 C24 C23 117.2(3) . . ? C25 C24 C27 121.6(3) . . ? C23 C24 C27 121.2(3) . . ? C24 C25 C26 121.6(3) . . ? C25 C26 C21 121.0(3) . . ? C29 C28 C33 117.4(3) . . ? C29 C28 C20 122.2(3) . . ? C33 C28 C20 120.1(3) . . ? C30 C29 C28 120.7(3) . . ? C29 C30 C31 122.0(3) . . ? C30 C31 C32 117.3(3) . . ? C30 C31 C34 121.6(3) . . ? C32 C31 C34 121.1(3) . . ? C33 C32 C31 121.1(3) . . ? C32 C33 C28 121.4(3) . . ? O4 C35 O3 120.6(3) . . ? O4 C35 C36 120.3(2) . . ? O3 C35 C36 119.1(2) . . ? O4 C35 Fe1 63.41(15) . . ? O3 C35 Fe1 57.25(14) . . ? C36 C35 Fe1 174.8(2) . . ? C41 C36 C37 120.7(3) . . ? C41 C36 C35 120.0(3) . . ? C37 C36 C35 119.3(2) . . ? C38 C37 C36 118.4(3) . . ? C38 C37 C42 119.4(3) . . ? C36 C37 C42 122.2(3) . . ? C39 C38 C37 121.3(3) . . ? C40 C39 C38 120.1(3) . . ? C39 C40 C41 120.9(3) . . ? C36 C41 C40 118.6(3) . . ? C36 C41 C49 122.5(3) . . ? C40 C41 C49 118.8(3) . . ? C43 C42 C47 117.3(3) . . ? C43 C42 C37 122.1(3) . . ? C47 C42 C37 120.6(3) . . ? C44 C43 C42 121.3(3) . . ? C45 C44 C43 121.0(3) . . ? C44 C45 C46 117.8(3) . . ? C44 C45 C48 121.5(3) . . ? C46 C45 C48 120.7(3) . . ? C47 C46 C45 121.2(3) . . ? C46 C47 C42 121.4(3) . . ? C50 C49 C54 117.5(3) . . ? C50 C49 C41 121.6(3) . . ? C54 C49 C41 120.8(3) . . ? C51 C50 C49 121.0(3) . . ? C52 C51 C50 121.5(4) . . ? C51 C52 C53 117.7(3) . . ? C51 C52 C55 121.3(4) . . ? C53 C52 C55 121.0(4) . . ? C52 C53 C54 121.9(3) . . ? C53 C54 C49 120.4(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.451 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.054