[Fe2(m-O2CArTol)2(O2CArTol)2(4-Etpy)2] (8) data_082703sad _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H86 Fe2 N2 O8' _chemical_formula_weight 1531.39 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 10.775(3) _cell_length_b 24.890(8) _cell_length_c 15.118(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.178(6) _cell_angle_gamma 90.00 _cell_volume 3894(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 856 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 21.50 _exptl_crystal_description Rod _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.434 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.561650 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 31640 _diffrn_reflns_av_R_equivalents 0.0873 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.39 _reflns_number_total 7957 _reflns_number_gt 5580 _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^)+(0.0722P)^2^+2.5966P] 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 7957 _refine_ls_number_parameters 500 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1099 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.072 _refine_ls_shift/su_mean 0.002 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 0.65979(5) 0.95071(2) 0.51345(4) 0.02525(16) Uani 1 1 d . . . N1 N 0.8321(3) 0.99128(12) 0.5862(2) 0.0286(7) Uani 1 1 d . . . O1 O 0.5772(2) 0.95663(10) 0.61734(17) 0.0318(6) Uani 1 1 d . . . O2 O 0.6138(2) 1.00137(10) 0.40914(17) 0.0302(6) Uani 1 1 d . . . O3 O 0.7541(2) 0.87892(10) 0.50986(18) 0.0331(6) Uani 1 1 d . . . O4 O 0.5434(2) 0.87219(10) 0.46762(18) 0.0333(6) Uani 1 1 d . . . C1 C 0.8914(4) 1.02957(15) 0.5506(3) 0.0333(9) Uani 1 1 d . . . H1A H 0.8502 1.0423 0.4903 0.040 Uiso 1 1 calc R . . C2 C 1.0084(4) 1.05138(16) 0.5969(3) 0.0366(9) Uani 1 1 d . . . H2A H 1.0467 1.0782 0.5682 0.044 Uiso 1 1 calc R . . C3 C 1.0711(4) 1.03430(15) 0.6857(3) 0.0332(9) Uani 1 1 d . . . C4 C 1.0084(4) 0.99562(18) 0.7225(3) 0.0431(11) Uani 1 1 d . . . H4A H 1.0462 0.9828 0.7833 0.052 Uiso 1 1 calc R . . C5 C 0.8913(4) 0.97554(18) 0.6716(3) 0.0418(10) Uani 1 1 d . . . H5A H 0.8506 0.9490 0.6990 0.050 Uiso 1 1 calc R . . C6 C 1.2012(4) 1.0576(2) 0.7360(3) 0.0495(12) Uani 1 1 d . . . H6A H 1.2667 1.0428 0.7079 0.059 Uiso 1 1 calc R . . H6B H 1.1980 1.0969 0.7258 0.059 Uiso 1 1 calc R . . C7 C 1.2458(4) 1.0474(2) 0.8377(3) 0.0563(13) Uani 1 1 d . . . H7A H 1.3305 1.0642 0.8635 0.084 Uiso 1 1 calc R . . H7B H 1.2527 1.0086 0.8491 0.084 Uiso 1 1 calc R . . H7C H 1.1834 1.0628 0.8670 0.084 Uiso 1 1 calc R . . C8 C 0.6515(3) 0.85002(14) 0.4903(2) 0.0259(8) Uani 1 1 d . . . C9 C 0.6667(3) 0.78994(14) 0.4984(3) 0.0288(8) Uani 1 1 d . . . C10 C 0.7385(4) 0.76755(15) 0.5829(3) 0.0332(9) Uani 1 1 d . . . C11 C 0.7539(4) 0.71206(17) 0.5900(3) 0.0436(11) Uani 1 1 d . . . H11A H 0.8026 0.6966 0.6465 0.052 Uiso 1 1 calc R . . C12 C 0.6991(5) 0.67937(17) 0.5158(3) 0.0503(12) Uani 1 1 d . . . H12A H 0.7105 0.6416 0.5214 0.060 Uiso 1 1 calc R . . C13 C 0.6282(4) 0.70123(16) 0.4340(3) 0.0429(10) Uani 1 1 d . . . H13A H 0.5913 0.6782 0.3834 0.051 Uiso 1 1 calc R . . C14 C 0.6090(4) 0.75661(15) 0.4236(3) 0.0335(9) Uani 1 1 d . . . C15 C 0.7945(4) 0.79958(16) 0.6673(3) 0.0343(9) Uani 1 1 d . . . C16 C 0.7220(4) 0.83548(16) 0.7030(3) 0.0380(10) Uani 1 1 d . . . H16A H 0.6337 0.8412 0.6709 0.046 Uiso 1 1 calc R . . C17 C 0.7755(4) 0.86280(17) 0.7836(3) 0.0423(10) Uani 1 1 d . . . H17A H 0.7233 0.8869 0.8065 0.051 Uiso 1 1 calc R . . C18 C 0.9050(4) 0.85588(18) 0.8326(3) 0.0446(11) Uani 1 1 d . . . C19 C 0.9769(4) 0.82006(18) 0.7970(3) 0.0452(11) Uani 1 1 d . . . H19A H 1.0654 0.8147 0.8287 0.054 Uiso 1 1 calc R . . C20 C 0.9235(4) 0.79201(17) 0.7170(3) 0.0395(10) Uani 1 1 d . . . H20A H 0.9752 0.7672 0.6953 0.047 Uiso 1 1 calc R . . C21 C 0.9640(6) 0.8857(2) 0.9208(3) 0.0686(16) Uani 1 1 d . . . H21A H 1.0531 0.8736 0.9472 0.103 Uiso 1 1 calc R . . H21B H 0.9136 0.8788 0.9645 0.103 Uiso 1 1 calc R . . H21C H 0.9636 0.9244 0.9080 0.103 Uiso 1 1 calc R . . C22 C 0.5339(4) 0.77568(15) 0.3310(3) 0.0336(9) Uani 1 1 d . . . C23 C 0.5820(4) 0.81299(16) 0.2810(3) 0.0378(10) Uani 1 1 d . . . H23A H 0.6614 0.8307 0.3091 0.045 Uiso 1 1 calc R . . C24 C 0.5161(4) 0.82477(17) 0.1911(3) 0.0440(11) Uani 1 1 d . . . H24A H 0.5514 0.8502 0.1580 0.053 Uiso 1 1 calc R . . C25 C 0.3988(5) 0.80016(17) 0.1477(3) 0.0434(11) Uani 1 1 d . . . C26 C 0.3500(4) 0.76341(17) 0.1978(3) 0.0437(11) Uani 1 1 d . . . H26A H 0.2700 0.7462 0.1699 0.052 Uiso 1 1 calc R . . C27 C 0.4157(4) 0.75143(16) 0.2877(3) 0.0404(10) Uani 1 1 d . . . H27A H 0.3799 0.7262 0.3208 0.049 Uiso 1 1 calc R . . C28 C 0.3280(5) 0.8144(2) 0.0488(3) 0.0637(14) Uani 1 1 d . . . H28A H 0.2502 0.7921 0.0281 0.096 Uiso 1 1 calc R . . H28B H 0.3847 0.8078 0.0093 0.096 Uiso 1 1 calc R . . H28C H 0.3033 0.8524 0.0452 0.096 Uiso 1 1 calc R . . C29 C 0.4782(4) 0.97060(14) 0.6392(2) 0.0273(8) Uani 1 1 d . . . C30 C 0.4673(3) 0.95404(14) 0.7333(2) 0.0248(7) Uani 1 1 d . . . C31 C 0.5487(4) 0.97853(15) 0.8122(3) 0.0295(8) Uani 1 1 d . . . C32 C 0.5363(4) 0.96322(15) 0.8982(3) 0.0352(9) Uani 1 1 d . . . H32A H 0.5905 0.9793 0.9522 0.042 Uiso 1 1 calc R . . C33 C 0.4468(4) 0.92518(16) 0.9064(3) 0.0387(10) Uani 1 1 d . . . H33A H 0.4388 0.9155 0.9654 0.046 Uiso 1 1 calc R . . C34 C 0.3695(4) 0.90157(16) 0.8283(3) 0.0355(9) Uani 1 1 d . . . H34A H 0.3091 0.8751 0.8346 0.043 Uiso 1 1 calc R . . C35 C 0.3761(3) 0.91478(14) 0.7410(3) 0.0276(8) Uani 1 1 d . . . C36 C 0.6447(4) 1.02043(15) 0.8071(3) 0.0314(9) Uani 1 1 d . . . C37 C 0.6167(4) 1.06210(15) 0.7432(3) 0.0347(9) Uani 1 1 d . . . H37A H 0.5335 1.0641 0.7003 0.042 Uiso 1 1 calc R . . C38 C 0.7083(4) 1.10061(16) 0.7412(3) 0.0404(10) Uani 1 1 d . . . H38A H 0.6875 1.1283 0.6962 0.049 Uiso 1 1 calc R . . C39 C 0.8299(4) 1.09955(18) 0.8036(3) 0.0415(10) Uani 1 1 d . . . C40 C 0.8580(4) 1.05834(18) 0.8679(3) 0.0429(11) Uani 1 1 d . . . H40A H 0.9408 1.0569 0.9114 0.051 Uiso 1 1 calc R . . C41 C 0.7677(4) 1.01962(17) 0.8697(3) 0.0378(10) Uani 1 1 d . . . H41A H 0.7894 0.9918 0.9143 0.045 Uiso 1 1 calc R . . C42 C 0.9285(5) 1.1425(2) 0.8018(4) 0.0605(14) Uani 1 1 d . . . H42A H 0.9737 1.1330 0.7560 0.091 Uiso 1 1 calc R . . H42B H 0.9910 1.1451 0.8627 0.091 Uiso 1 1 calc R . . H42C H 0.8846 1.1771 0.7856 0.091 Uiso 1 1 calc R . . C43 C 0.2911(4) 0.88698(14) 0.6591(3) 0.0294(8) Uani 1 1 d . . . C44 C 0.3354(4) 0.86687(15) 0.5879(3) 0.0303(8) Uani 1 1 d . . . H44A H 0.4230 0.8725 0.5890 0.036 Uiso 1 1 calc R . . C45 C 0.2548(4) 0.83885(15) 0.5154(3) 0.0371(9) Uani 1 1 d . . . H45A H 0.2877 0.8253 0.4677 0.045 Uiso 1 1 calc R . . C46 C 0.1248(4) 0.83018(16) 0.5117(3) 0.0392(10) Uani 1 1 d . . . C47 C 0.0805(4) 0.85132(17) 0.5809(3) 0.0414(10) Uani 1 1 d . . . H47A H -0.0079 0.8469 0.5785 0.050 Uiso 1 1 calc R . . C48 C 0.1607(4) 0.87894(16) 0.6542(3) 0.0347(9) Uani 1 1 d . . . H48A H 0.1271 0.8926 0.7015 0.042 Uiso 1 1 calc R . . C49 C 0.0365(5) 0.7987(2) 0.4337(4) 0.0614(14) Uani 1 1 d . . . H49A H 0.0086 0.7658 0.4580 0.092 Uiso 1 1 calc R . . H49B H 0.0828 0.7895 0.3885 0.092 Uiso 1 1 calc R . . H49C H -0.0394 0.8206 0.4040 0.092 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 0.0212(3) 0.0241(3) 0.0291(3) 0.0013(2) 0.0049(2) 0.0000(2) N1 0.0250(16) 0.0263(16) 0.0326(18) -0.0006(13) 0.0048(13) -0.0018(13) O1 0.0272(14) 0.0339(15) 0.0363(15) -0.0040(12) 0.0121(11) -0.0055(12) O2 0.0271(14) 0.0300(14) 0.0293(14) 0.0070(11) 0.0009(11) -0.0009(11) O3 0.0241(13) 0.0246(14) 0.0493(17) 0.0036(12) 0.0080(12) -0.0007(11) O4 0.0255(14) 0.0284(14) 0.0448(16) -0.0012(12) 0.0079(12) 0.0071(11) C1 0.030(2) 0.031(2) 0.036(2) 0.0022(17) 0.0031(17) -0.0018(17) C2 0.029(2) 0.031(2) 0.048(2) 0.0048(18) 0.0081(18) -0.0034(18) C3 0.026(2) 0.031(2) 0.041(2) -0.0098(17) 0.0064(17) 0.0000(16) C4 0.037(2) 0.048(3) 0.037(2) 0.0042(19) -0.0024(19) -0.004(2) C5 0.040(2) 0.044(2) 0.036(2) 0.0051(19) 0.0028(19) -0.012(2) C6 0.028(2) 0.058(3) 0.057(3) -0.008(2) 0.003(2) -0.010(2) C7 0.039(3) 0.053(3) 0.065(3) -0.014(2) -0.005(2) -0.004(2) C8 0.0269(19) 0.0235(18) 0.028(2) 0.0021(14) 0.0082(16) 0.0029(16) C9 0.0217(18) 0.0264(19) 0.042(2) 0.0029(16) 0.0150(17) 0.0010(15) C10 0.026(2) 0.031(2) 0.046(2) 0.0079(18) 0.0164(18) 0.0068(16) C11 0.041(2) 0.034(2) 0.056(3) 0.014(2) 0.015(2) 0.0072(19) C12 0.059(3) 0.022(2) 0.072(3) 0.003(2) 0.022(3) 0.002(2) C13 0.049(3) 0.028(2) 0.052(3) -0.0033(19) 0.015(2) -0.001(2) C14 0.033(2) 0.028(2) 0.045(2) -0.0032(17) 0.0186(18) -0.0014(17) C15 0.030(2) 0.031(2) 0.041(2) 0.0141(17) 0.0104(18) 0.0038(17) C16 0.032(2) 0.040(2) 0.041(2) 0.0082(19) 0.0090(18) 0.0087(19) C17 0.050(3) 0.041(2) 0.036(2) 0.0092(19) 0.012(2) 0.011(2) C18 0.051(3) 0.043(3) 0.034(2) 0.0113(19) 0.003(2) -0.001(2) C19 0.030(2) 0.049(3) 0.050(3) 0.021(2) 0.001(2) 0.001(2) C20 0.031(2) 0.039(2) 0.047(3) 0.011(2) 0.0086(19) 0.0077(18) C21 0.081(4) 0.063(4) 0.048(3) 0.002(3) -0.005(3) 0.002(3) C22 0.039(2) 0.026(2) 0.038(2) -0.0070(17) 0.0158(18) -0.0030(17) C23 0.037(2) 0.035(2) 0.046(3) -0.0041(18) 0.0194(19) -0.0058(18) C24 0.054(3) 0.038(2) 0.047(3) 0.003(2) 0.026(2) -0.005(2) C25 0.055(3) 0.037(2) 0.039(2) -0.0080(19) 0.014(2) 0.000(2) C26 0.050(3) 0.034(2) 0.044(3) -0.0092(19) 0.007(2) -0.008(2) C27 0.048(3) 0.027(2) 0.048(3) -0.0067(18) 0.016(2) -0.0103(19) C28 0.078(4) 0.061(3) 0.048(3) 0.000(2) 0.012(3) -0.002(3) C29 0.028(2) 0.0199(18) 0.031(2) -0.0057(15) 0.0033(16) -0.0065(15) C30 0.0242(18) 0.0209(18) 0.0281(19) 0.0014(15) 0.0052(14) 0.0046(15) C31 0.029(2) 0.0245(19) 0.032(2) -0.0002(15) 0.0038(16) 0.0042(16) C32 0.043(2) 0.030(2) 0.030(2) -0.0033(16) 0.0047(18) 0.0036(18) C33 0.053(3) 0.036(2) 0.029(2) 0.0040(17) 0.015(2) 0.006(2) C34 0.037(2) 0.026(2) 0.045(2) 0.0061(17) 0.0142(19) 0.0024(17) C35 0.0267(19) 0.0229(19) 0.032(2) 0.0001(15) 0.0071(16) 0.0056(15) C36 0.030(2) 0.029(2) 0.033(2) -0.0079(16) 0.0042(17) -0.0023(17) C37 0.034(2) 0.027(2) 0.037(2) -0.0061(16) -0.0003(17) -0.0044(17) C38 0.050(3) 0.028(2) 0.042(2) -0.0041(18) 0.010(2) -0.0057(19) C39 0.033(2) 0.040(2) 0.050(3) -0.017(2) 0.010(2) -0.0102(19) C40 0.028(2) 0.046(3) 0.048(3) -0.013(2) 0.0004(19) -0.0017(19) C41 0.035(2) 0.039(2) 0.035(2) -0.0034(18) 0.0014(18) -0.0002(19) C42 0.045(3) 0.054(3) 0.084(4) -0.017(3) 0.020(3) -0.022(2) C43 0.029(2) 0.0226(19) 0.036(2) 0.0066(15) 0.0082(17) 0.0014(16) C44 0.0258(19) 0.029(2) 0.036(2) 0.0023(16) 0.0071(16) 0.0007(16) C45 0.042(2) 0.027(2) 0.040(2) -0.0006(17) 0.0083(19) 0.0004(18) C46 0.039(2) 0.031(2) 0.041(2) 0.0054(18) 0.001(2) -0.0053(18) C47 0.028(2) 0.042(2) 0.054(3) 0.013(2) 0.010(2) -0.0059(19) C48 0.029(2) 0.036(2) 0.040(2) 0.0044(18) 0.0128(18) 0.0008(17) C49 0.050(3) 0.057(3) 0.065(3) -0.006(3) -0.005(2) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.971(2) . ? Fe1 O1 2.015(3) . ? Fe1 O3 2.064(3) . ? Fe1 N1 2.130(3) . ? Fe1 O4 2.321(3) . ? Fe1 Fe1 4.1547(14) 3_676 ? Fe1 C6 6.441(4) . ? N1 C5 1.331(5) . ? N1 C1 1.341(5) . ? O1 C29 1.251(4) . ? O2 C29 1.265(4) 3_676 ? O3 C8 1.283(4) . ? O4 C8 1.248(4) . ? C1 C2 1.372(5) . ? C2 C3 1.391(5) . ? C3 C4 1.379(6) . ? C3 C6 1.511(5) . ? C4 C5 1.376(6) . ? C6 C7 1.500(6) . ? C8 C9 1.506(5) . ? C9 C14 1.400(5) . ? C9 C10 1.411(5) . ? C10 C11 1.392(6) . ? C10 C15 1.483(6) . ? C11 C12 1.378(6) . ? C12 C13 1.372(6) . ? C13 C14 1.396(5) . ? C14 C22 1.487(6) . ? C15 C16 1.391(6) . ? C15 C20 1.397(5) . ? C16 C17 1.375(6) . ? C17 C18 1.396(6) . ? C18 C19 1.384(6) . ? C18 C21 1.504(6) . ? C19 C20 1.376(6) . ? C22 C23 1.386(5) . ? C22 C27 1.396(6) . ? C23 C24 1.379(6) . ? C24 C25 1.393(6) . ? C25 C26 1.382(6) . ? C25 C28 1.518(6) . ? C26 C27 1.379(6) . ? C29 O2 1.265(4) 3_676 ? C29 C30 1.515(5) . ? C30 C31 1.408(5) . ? C30 C35 1.414(5) . ? C31 C32 1.396(5) . ? C31 C36 1.486(5) . ? C32 C33 1.382(6) . ? C33 C34 1.373(6) . ? C34 C35 1.381(5) . ? C35 C43 1.490(5) . ? C36 C37 1.392(5) . ? C36 C41 1.397(5) . ? C37 C38 1.382(6) . ? C38 C39 1.385(6) . ? C39 C40 1.388(6) . ? C39 C42 1.512(6) . ? C40 C41 1.375(6) . ? C43 C44 1.387(5) . ? C43 C48 1.400(5) . ? C44 C45 1.382(5) . ? C45 C46 1.402(6) . ? C46 C47 1.370(6) . ? C46 C49 1.512(6) . ? C47 C48 1.383(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 O2 Fe1 O1 120.64(11) . . ? O2 Fe1 O3 123.27(11) . . ? O1 Fe1 O3 114.29(11) . . ? O2 Fe1 N1 95.64(11) . . ? O1 Fe1 N1 94.23(11) . . ? O3 Fe1 N1 93.40(11) . . ? O2 Fe1 O4 107.78(10) . . ? O1 Fe1 O4 88.56(10) . . ? O3 Fe1 O4 59.48(9) . . ? N1 Fe1 O4 150.90(10) . . ? O2 Fe1 Fe1 61.79(8) . 3_676 ? O1 Fe1 Fe1 59.94(8) . 3_676 ? O3 Fe1 Fe1 155.43(7) . 3_676 ? N1 Fe1 Fe1 110.49(9) . 3_676 ? O4 Fe1 Fe1 95.96(7) . 3_676 ? C5 N1 C1 116.4(3) . . ? C5 N1 Fe1 118.4(3) . . ? C1 N1 Fe1 125.0(3) . . ? C29 O1 Fe1 145.2(3) . . ? C29 O2 Fe1 142.8(3) 3_676 . ? C8 O3 Fe1 95.3(2) . . ? C8 O4 Fe1 84.6(2) . . ? N1 C1 C2 123.4(4) . . ? C1 C2 C3 120.1(4) . . ? C4 C3 C2 116.2(4) . . ? C4 C3 C6 123.7(4) . . ? C2 C3 C6 120.1(4) . . ? C5 C4 C3 120.3(4) . . ? N1 C5 C4 123.6(4) . . ? C7 C6 C3 116.0(4) . . ? O4 C8 O3 119.6(3) . . ? O4 C8 C9 122.2(3) . . ? O3 C8 C9 118.1(3) . . ? C14 C9 C10 120.3(3) . . ? C14 C9 C8 120.6(3) . . ? C10 C9 C8 119.0(3) . . ? C11 C10 C9 119.0(4) . . ? C11 C10 C15 117.1(4) . . ? C9 C10 C15 123.8(3) . . ? C12 C11 C10 120.5(4) . . ? C13 C12 C11 120.3(4) . . ? C12 C13 C14 121.4(4) . . ? C13 C14 C9 118.4(4) . . ? C13 C14 C22 116.5(4) . . ? C9 C14 C22 125.0(3) . . ? C16 C15 C20 117.4(4) . . ? C16 C15 C10 122.8(4) . . ? C20 C15 C10 119.8(4) . . ? C17 C16 C15 121.3(4) . . ? C16 C17 C18 121.3(4) . . ? C19 C18 C17 117.3(4) . . ? C19 C18 C21 121.2(4) . . ? C17 C18 C21 121.5(5) . . ? C20 C19 C18 121.8(4) . . ? C19 C20 C15 120.9(4) . . ? C23 C22 C27 117.7(4) . . ? C23 C22 C14 122.6(4) . . ? C27 C22 C14 119.3(4) . . ? C24 C23 C22 120.8(4) . . ? C23 C24 C25 121.4(4) . . ? C26 C25 C24 117.8(4) . . ? C26 C25 C28 122.0(4) . . ? C24 C25 C28 120.2(4) . . ? C27 C26 C25 120.9(4) . . ? C26 C27 C22 121.3(4) . . ? O1 C29 O2 126.1(4) . 3_676 ? O1 C29 C30 117.8(3) . . ? O2 C29 C30 116.1(3) 3_676 . ? C31 C30 C35 120.8(3) . . ? C31 C30 C29 119.0(3) . . ? C35 C30 C29 120.2(3) . . ? C32 C31 C30 118.2(4) . . ? C32 C31 C36 119.3(3) . . ? C30 C31 C36 122.5(3) . . ? C33 C32 C31 121.4(4) . . ? C34 C33 C32 119.1(4) . . ? C33 C34 C35 122.7(4) . . ? C34 C35 C30 117.7(3) . . ? C34 C35 C43 120.0(3) . . ? C30 C35 C43 122.2(3) . . ? C37 C36 C41 117.5(4) . . ? C37 C36 C31 122.6(3) . . ? C41 C36 C31 119.8(4) . . ? C38 C37 C36 120.9(4) . . ? C37 C38 C39 121.2(4) . . ? C38 C39 C40 118.2(4) . . ? C38 C39 C42 120.7(4) . . ? C40 C39 C42 121.1(4) . . ? C41 C40 C39 120.9(4) . . ? C40 C41 C36 121.3(4) . . ? C44 C43 C48 117.7(4) . . ? C44 C43 C35 123.2(3) . . ? C48 C43 C35 119.1(3) . . ? C45 C44 C43 121.4(4) . . ? C44 C45 C46 120.6(4) . . ? C47 C46 C45 117.8(4) . . ? C47 C46 C49 121.1(4) . . ? C45 C46 C49 121.0(4) . . ? C46 C47 C48 122.0(4) . . ? C47 C48 C43 120.5(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.079 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.083