[Fe2(m-O2CArTol)2(O2CArTol)2(2-Etpy)2] (6) data_050503sad _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C101 H92 Cl5 Fe2 N2 O8' _chemical_formula_weight 1750.72 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' 'Cl' 'Cl' 0.1484 0.1585 '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' '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' _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 15.219(2) _cell_length_b 10.8186(16) _cell_length_c 29.434(4) _cell_angle_alpha 90.00 _cell_angle_beta 117.387(6) _cell_angle_gamma 90.00 _cell_volume 4303.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1008 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 21.33 _exptl_crystal_description Rod _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1826 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.761074 _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 34613 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.38 _reflns_number_total 8807 _reflns_number_gt 7051 _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^)+(0.0757P)^2^+5.7656P] 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 8807 _refine_ls_number_parameters 583 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.1999 _refine_ls_wR_factor_gt 0.1886 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.220 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.02085(4) 0.66417(5) 0.54612(2) 0.02156(17) Uani 1 1 d . . . N1 N -0.0819(2) 0.8124(3) 0.51116(12) 0.0244(7) Uani 1 1 d . . . O1 O -0.0619(2) 0.5219(3) 0.54236(12) 0.0312(7) Uani 1 1 d . . . O2 O 0.0750(2) 0.6602(3) 0.49543(11) 0.0317(7) Uani 1 1 d . . . O3 O 0.1026(2) 0.7638(3) 0.60999(10) 0.0295(7) Uani 1 1 d . . . O4 O 0.1699(2) 0.5794(3) 0.62239(11) 0.0347(7) Uani 1 1 d . . . C1 C -0.0814(3) 0.8704(4) 0.47097(15) 0.0288(9) Uani 1 1 d . . . H1A H -0.0492 0.8311 0.4539 0.019(10) Uiso 1 1 d R . . C2 C -0.1252(3) 0.9837(4) 0.45309(16) 0.0324(10) Uani 1 1 d . . . H2A H -0.1242 1.0211 0.4241 0.034(12) Uiso 1 1 d R . . C3 C -0.1711(3) 1.0406(4) 0.47855(16) 0.0362(11) Uani 1 1 d . . . H3A H -0.1980 1.1213 0.4691 0.036(13) Uiso 1 1 d R . . C4 C -0.1762(3) 0.9796(4) 0.51813(17) 0.0352(10) Uani 1 1 d . . . H4B H -0.2109 1.0157 0.5346 0.028(11) Uiso 1 1 d R . . C5 C -0.1319(3) 0.8650(4) 0.53398(15) 0.0279(9) Uani 1 1 d . . . C6 C -0.1340(3) 0.7950(4) 0.57775(17) 0.0338(10) Uani 1 1 d . . . H6A H -0.1464 0.7066 0.5683 0.023(11) Uiso 1 1 d R . . H6B H -0.0681 0.8014 0.6079 0.035(13) Uiso 1 1 d R . . C7 C -0.2115(4) 0.8398(5) 0.59295(19) 0.0424(12) Uani 1 1 d . . . H7A H -0.2084 0.7901 0.6215 0.056(16) Uiso 1 1 d R . . H7B H -0.1989 0.9267 0.6033 0.047(15) Uiso 1 1 d R . . H7C H -0.2774 0.8318 0.5637 0.066(18) Uiso 1 1 d R . . C8 C 0.1656(3) 0.6836(4) 0.63820(16) 0.0257(9) Uani 1 1 d . . . C9 C 0.2340(3) 0.7232(4) 0.69268(15) 0.0266(9) Uani 1 1 d . . . C10 C 0.1958(3) 0.7426(4) 0.72734(15) 0.0283(9) Uani 1 1 d . . . C11 C 0.2591(4) 0.7843(4) 0.77633(16) 0.0356(10) Uani 1 1 d . . . H11A H 0.2339 0.7978 0.8001 0.041(13) Uiso 1 1 d R . . C12 C 0.3579(4) 0.8065(5) 0.79114(17) 0.0387(11) Uani 1 1 d . . . H12A H 0.3999 0.8369 0.8245 0.042(14) Uiso 1 1 d R . . C13 C 0.3948(3) 0.7840(5) 0.75729(17) 0.0374(11) Uani 1 1 d . . . H13A H 0.4632 0.7974 0.7679 0.042(14) Uiso 1 1 d R . . C14 C 0.3345(3) 0.7420(4) 0.70788(16) 0.0306(9) Uani 1 1 d . . . C15 C 0.0921(3) 0.7106(4) 0.71591(16) 0.0326(10) Uani 1 1 d . . . C16 C 0.0499(3) 0.5983(4) 0.69349(16) 0.0349(10) Uani 1 1 d . . . H16A H 0.0860 0.5433 0.6831 0.033(12) Uiso 1 1 d R . . C17 C -0.0434(4) 0.5656(5) 0.68637(17) 0.0389(11) Uani 1 1 d . . . H17A H -0.0716 0.4896 0.6700 0.029(12) Uiso 1 1 d R . . C18 C -0.0965(3) 0.6418(5) 0.70242(17) 0.0370(11) Uani 1 1 d . . . C19 C -0.0547(4) 0.7534(5) 0.72489(19) 0.0437(12) Uani 1 1 d . . . H19A H -0.0906 0.8075 0.7357 0.039(13) Uiso 1 1 d R . . C20 C 0.0377(4) 0.7879(5) 0.73155(18) 0.0373(11) Uani 1 1 d . . . H20A H 0.0648 0.8651 0.7471 0.027(11) Uiso 1 1 d R . . C21 C -0.1978(4) 0.6049(6) 0.6952(2) 0.0511(14) Uani 1 1 d . . . H21A H -0.1914 0.5615 0.7258 0.077 Uiso 1 1 calc R . . H21B H -0.2293 0.5502 0.6654 0.077 Uiso 1 1 calc R . . H21C H -0.2385 0.6790 0.6896 0.077 Uiso 1 1 calc R . . C22 C 0.3803(3) 0.7202(4) 0.67328(17) 0.0328(10) Uani 1 1 d . . . C23 C 0.3487(3) 0.7815(5) 0.62756(18) 0.0410(12) Uani 1 1 d . . . H23A H 0.2941 0.8366 0.6164 0.051(15) Uiso 1 1 d R . . C24 C 0.3962(4) 0.7643(6) 0.59785(19) 0.0500(14) Uani 1 1 d . . . H24A H 0.3730 0.8073 0.5663 0.045(14) Uiso 1 1 d R . . C25 C 0.4762(3) 0.6862(6) 0.6127(2) 0.0514(15) Uani 1 1 d . . . C26 C 0.5077(4) 0.6251(6) 0.6585(2) 0.0563(15) Uani 1 1 d . . . H26A H 0.5631 0.5714 0.6697 0.09(2) Uiso 1 1 d R . . C27 C 0.4608(4) 0.6403(5) 0.6890(2) 0.0460(13) Uani 1 1 d . . . H27A H 0.4836 0.5968 0.7204 0.057(16) Uiso 1 1 d R . . C28 C 0.5274(4) 0.6649(8) 0.5800(2) 0.077(2) Uani 1 1 d . . . H28A H 0.5983 0.6817 0.6001 0.116 Uiso 1 1 calc R . . H28B H 0.4993 0.7203 0.5503 0.116 Uiso 1 1 calc R . . H28C H 0.5179 0.5789 0.5682 0.116 Uiso 1 1 calc R . . C29 C 0.0930(3) 0.5861(4) 0.46780(15) 0.0251(9) Uani 1 1 d . . . C30 C 0.1592(3) 0.6318(4) 0.44590(15) 0.0268(9) Uani 1 1 d . . . C31 C 0.2557(3) 0.5842(5) 0.46590(17) 0.0349(10) Uani 1 1 d . . . C32 C 0.3168(4) 0.6289(5) 0.44590(18) 0.0445(13) Uani 1 1 d . . . H32A H 0.3828 0.5992 0.4594 0.048(15) Uiso 1 1 d R . . C33 C 0.2843(4) 0.7154(6) 0.4077(2) 0.0517(14) Uani 1 1 d . . . H33A H 0.3277 0.7452 0.3950 0.057(16) Uiso 1 1 d R . . C34 C 0.1888(4) 0.7594(5) 0.38714(19) 0.0423(12) Uani 1 1 d . . . H34A H 0.1664 0.8177 0.3600 0.039(13) Uiso 1 1 d R . . C35 C 0.1245(3) 0.7189(4) 0.40590(16) 0.0312(10) Uani 1 1 d . . . C36 C 0.2933(3) 0.4864(4) 0.50542(17) 0.0334(10) Uani 1 1 d . . . C37 C 0.2789(3) 0.4857(5) 0.54866(17) 0.0364(11) Uani 1 1 d . . . H37A H 0.2448 0.5525 0.5545 0.031(12) Uiso 1 1 d R . . C38 C 0.3132(4) 0.3896(5) 0.58350(19) 0.0441(12) Uani 1 1 d . . . H38A H 0.3014 0.3913 0.6125 0.053(15) Uiso 1 1 d R . . C39 C 0.3638(4) 0.2911(5) 0.5769(2) 0.0477(13) Uani 1 1 d . . . C40 C 0.3821(4) 0.2939(6) 0.5350(2) 0.0533(14) Uani 1 1 d . . . H40A H 0.4189 0.2289 0.5302 0.063(17) Uiso 1 1 d R . . C41 C 0.3479(4) 0.3889(5) 0.5002(2) 0.0460(13) Uani 1 1 d . . . H41A H 0.3615 0.3882 0.4717 0.053(16) Uiso 1 1 d R . . C42 C 0.3966(5) 0.1834(6) 0.6133(3) 0.0698(18) Uani 1 1 d . . . H42A H 0.4579 0.1488 0.6154 0.105 Uiso 1 1 calc R . . H42B H 0.3450 0.1198 0.6010 0.105 Uiso 1 1 calc R . . H42C H 0.4083 0.2114 0.6473 0.105 Uiso 1 1 calc R . . C43 C 0.0211(3) 0.7660(4) 0.38096(15) 0.0303(10) Uani 1 1 d . . . C44 C -0.0603(4) 0.6916(4) 0.37020(16) 0.0327(10) Uani 1 1 d . . . H44A H -0.0503 0.6074 0.3806 0.015(9) Uiso 1 1 d R . . C45 C -0.1554(4) 0.7369(4) 0.34497(17) 0.0366(11) Uani 1 1 d . . . H45A H -0.2095 0.6830 0.3378 0.057(17) Uiso 1 1 d R . . C46 C -0.1732(4) 0.8598(5) 0.32974(17) 0.0414(12) Uani 1 1 d . . . C47 C -0.0933(4) 0.9354(5) 0.34063(18) 0.0436(12) Uani 1 1 d . . . H47A H -0.1037 1.0201 0.3312 0.053(15) Uiso 1 1 d R . . C48 C 0.0016(4) 0.8898(4) 0.36509(17) 0.0406(12) Uani 1 1 d . . . H48A H 0.0555 0.9436 0.3715 0.046(15) Uiso 1 1 d R . . C49 C -0.2771(2) 0.9094(3) 0.30195(12) 0.0601(16) Uani 1 1 d . . . H49A H -0.2854 0.9772 0.3218 0.090 Uiso 1 1 calc R . . H49B H -0.3243 0.8433 0.2978 0.090 Uiso 1 1 calc R . . H49C H -0.2893 0.9400 0.2682 0.090 Uiso 1 1 calc R . . C1S C 0.46838(19) 1.0205(2) 0.4523(2) 0.142(10) Uani 0.50 1 d PR . . H1S1 H 0.4205 1.0859 0.4326 0.171 Uiso 0.50 1 calc PR . . H1S2 H 0.4916 0.9770 0.4302 0.171 Uiso 0.50 1 calc PR . . Cl1 Cl 0.4211(2) 0.9167(3) 0.4835(2) 0.189(3) Uani 0.50 1 d PR . . C2S C -0.40514(19) 0.5299(2) 0.19029(10) 0.083(4) Uani 0.583(6) 1 d PRD A 1 H2S1 H -0.4651 0.5824 0.1751 0.100 Uiso 0.583(6) 1 calc PR A 1 H2S2 H -0.4226 0.4480 0.1988 0.100 Uiso 0.583(6) 1 calc PR A 1 Cl3 Cl -0.35001(19) 0.5159(2) 0.14822(10) 0.164(3) Uani 0.583(6) 1 d PRD A 1 Cl4 Cl -0.31287(19) 0.5982(2) 0.24266(11) 0.200(4) Uani 0.583(6) 1 d PRD A 1 C3S C -0.31937(19) 0.5166(2) 0.22116(11) 0.079(5) Uani 0.417(6) 1 d PRD A 2 H3S1 H -0.2638 0.5510 0.2523 0.095 Uiso 0.417(6) 1 calc PR A 2 H3S2 H -0.3225 0.4271 0.2272 0.095 Uiso 0.417(6) 1 calc PR A 2 Cl5 Cl -0.29212(19) 0.5315(2) 0.17501(10) 0.198(5) Uani 0.417(6) 1 d PRD A 2 Cl6 Cl -0.42843(19) 0.5837(2) 0.21548(11) 0.119(3) Uani 0.417(6) 1 d PRD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0259(3) 0.0205(3) 0.0216(3) -0.0014(2) 0.0138(2) 0.0007(2) N1 0.0233(17) 0.0262(18) 0.0223(17) 0.0001(13) 0.0095(14) 0.0002(14) O1 0.0341(17) 0.0203(15) 0.0433(18) -0.0005(13) 0.0213(14) -0.0037(12) O2 0.0424(18) 0.0321(16) 0.0316(16) 0.0033(13) 0.0264(14) 0.0067(14) O3 0.0288(16) 0.0317(16) 0.0235(14) 0.0009(12) 0.0082(13) 0.0011(13) O4 0.0431(18) 0.0309(17) 0.0363(17) -0.0081(13) 0.0235(15) -0.0013(14) C1 0.031(2) 0.029(2) 0.024(2) -0.0035(17) 0.0108(18) -0.0008(17) C2 0.035(2) 0.033(2) 0.024(2) 0.0052(18) 0.0094(19) 0.0024(19) C3 0.040(3) 0.032(2) 0.028(2) 0.0041(19) 0.009(2) 0.009(2) C4 0.036(3) 0.039(3) 0.030(2) -0.0049(19) 0.016(2) 0.011(2) C5 0.028(2) 0.031(2) 0.025(2) -0.0039(17) 0.0125(18) 0.0000(17) C6 0.038(3) 0.036(3) 0.033(2) 0.0070(19) 0.022(2) 0.009(2) C7 0.043(3) 0.051(3) 0.046(3) 0.004(2) 0.031(3) 0.007(2) C8 0.027(2) 0.027(2) 0.031(2) -0.0024(17) 0.0193(18) -0.0030(17) C9 0.032(2) 0.023(2) 0.025(2) 0.0002(16) 0.0138(18) 0.0031(17) C10 0.036(2) 0.026(2) 0.025(2) -0.0005(17) 0.0158(19) -0.0009(18) C11 0.045(3) 0.041(3) 0.024(2) -0.0025(19) 0.019(2) -0.001(2) C12 0.040(3) 0.046(3) 0.021(2) -0.0039(19) 0.007(2) -0.001(2) C13 0.029(2) 0.049(3) 0.028(2) 0.003(2) 0.0079(19) 0.001(2) C14 0.031(2) 0.033(2) 0.026(2) 0.0037(18) 0.0117(19) 0.0057(18) C15 0.038(3) 0.040(3) 0.023(2) -0.0015(18) 0.0167(19) 0.000(2) C16 0.045(3) 0.037(3) 0.030(2) -0.0005(19) 0.024(2) 0.000(2) C17 0.052(3) 0.037(3) 0.032(2) -0.003(2) 0.024(2) -0.011(2) C18 0.040(3) 0.047(3) 0.029(2) 0.005(2) 0.021(2) -0.004(2) C19 0.047(3) 0.048(3) 0.050(3) -0.005(2) 0.034(3) 0.005(2) C20 0.044(3) 0.041(3) 0.037(3) -0.011(2) 0.027(2) -0.005(2) C21 0.046(3) 0.061(4) 0.055(3) 0.006(3) 0.031(3) -0.009(3) C22 0.021(2) 0.045(3) 0.033(2) -0.006(2) 0.0119(19) 0.0001(19) C23 0.027(2) 0.065(3) 0.033(2) 0.003(2) 0.015(2) 0.008(2) C24 0.030(3) 0.090(4) 0.029(3) -0.001(3) 0.012(2) 0.003(3) C25 0.025(2) 0.088(4) 0.042(3) -0.025(3) 0.015(2) -0.006(3) C26 0.033(3) 0.072(4) 0.062(4) -0.014(3) 0.020(3) 0.013(3) C27 0.039(3) 0.053(3) 0.047(3) 0.007(2) 0.020(2) 0.014(2) C28 0.038(3) 0.148(7) 0.053(3) -0.029(4) 0.026(3) 0.003(4) C29 0.022(2) 0.030(2) 0.021(2) 0.0008(16) 0.0082(17) 0.0043(17) C30 0.034(2) 0.026(2) 0.027(2) -0.0073(16) 0.0194(19) -0.0060(17) C31 0.036(3) 0.048(3) 0.028(2) -0.010(2) 0.021(2) -0.005(2) C32 0.032(3) 0.072(4) 0.034(3) -0.003(2) 0.020(2) -0.003(2) C33 0.051(3) 0.080(4) 0.041(3) -0.003(3) 0.035(3) -0.018(3) C34 0.052(3) 0.050(3) 0.034(3) 0.000(2) 0.028(2) -0.009(2) C35 0.040(3) 0.033(2) 0.026(2) -0.0072(18) 0.020(2) -0.0092(19) C36 0.024(2) 0.047(3) 0.031(2) -0.006(2) 0.0143(19) -0.0036(19) C37 0.030(2) 0.047(3) 0.032(2) -0.002(2) 0.014(2) 0.001(2) C38 0.035(3) 0.062(3) 0.036(3) 0.002(2) 0.016(2) -0.004(2) C39 0.034(3) 0.053(3) 0.047(3) 0.005(2) 0.011(2) -0.002(2) C40 0.041(3) 0.062(4) 0.055(3) -0.005(3) 0.021(3) 0.012(3) C41 0.039(3) 0.060(3) 0.046(3) -0.003(3) 0.026(2) 0.007(2) C42 0.060(4) 0.066(4) 0.065(4) 0.014(3) 0.013(3) 0.000(3) C43 0.046(3) 0.031(2) 0.0186(19) -0.0043(17) 0.0189(19) -0.0045(19) C44 0.052(3) 0.020(2) 0.030(2) -0.0049(17) 0.022(2) -0.0057(19) C45 0.042(3) 0.038(3) 0.028(2) 0.0001(19) 0.014(2) 0.002(2) C46 0.055(3) 0.045(3) 0.026(2) 0.005(2) 0.021(2) 0.011(2) C47 0.068(4) 0.030(3) 0.037(3) 0.005(2) 0.028(3) 0.006(2) C48 0.060(3) 0.035(3) 0.030(2) -0.002(2) 0.024(2) -0.011(2) C49 0.066(4) 0.059(4) 0.055(3) 0.013(3) 0.028(3) 0.022(3) C1S 0.144(18) 0.062(10) 0.29(3) 0.038(14) 0.16(2) 0.051(11) Cl1 0.094(4) 0.171(7) 0.260(9) -0.042(6) 0.043(5) 0.027(4) C2S 0.048(7) 0.044(6) 0.116(11) 0.021(7) 0.001(7) 0.004(5) Cl3 0.296(8) 0.084(3) 0.263(7) 0.055(3) 0.260(7) 0.051(4) Cl4 0.193(6) 0.096(4) 0.143(5) -0.023(3) -0.068(4) 0.030(4) C3S 0.091(14) 0.070(12) 0.084(13) -0.002(10) 0.046(11) 0.015(10) Cl5 0.283(13) 0.152(8) 0.267(12) 0.045(8) 0.218(12) -0.020(8) Cl6 0.128(5) 0.111(5) 0.164(6) 0.044(4) 0.106(5) 0.073(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.959(3) . ? Fe1 O2 2.010(3) . ? Fe1 O3 2.023(3) . ? Fe1 N1 2.143(3) . ? Fe1 C6 3.232(4) . ? Fe1 Fe1 4.3366(12) 3_566 ? N1 C1 1.342(5) . ? N1 C5 1.350(5) . ? O1 C29 1.245(5) 3_566 ? O2 C29 1.258(5) . ? O3 C8 1.276(5) . ? O4 C8 1.233(5) . ? C1 C2 1.378(6) . ? C2 C3 1.383(6) . ? C3 C4 1.372(6) . ? C4 C5 1.386(6) . ? C5 C6 1.508(6) . ? C6 C7 1.520(6) . ? C8 C9 1.518(6) . ? C9 C14 1.397(6) . ? C9 C10 1.402(6) . ? C10 C11 1.390(6) . ? C10 C15 1.496(6) . ? C11 C12 1.381(7) . ? C12 C13 1.372(7) . ? C13 C14 1.392(6) . ? C14 C22 1.494(6) . ? C15 C16 1.390(6) . ? C15 C20 1.395(6) . ? C16 C17 1.383(6) . ? C17 C18 1.381(7) . ? C18 C19 1.382(7) . ? C18 C21 1.510(6) . ? C19 C20 1.380(7) . ? C22 C23 1.374(7) . ? C22 C27 1.393(6) . ? C23 C24 1.380(6) . ? C24 C25 1.378(7) . ? C25 C26 1.374(8) . ? C25 C28 1.509(7) . ? C26 C27 1.389(7) . ? C29 O1 1.245(5) 3_566 ? C29 C30 1.508(6) . ? C30 C31 1.405(6) . ? C30 C35 1.407(6) . ? C31 C32 1.395(6) . ? C31 C36 1.479(7) . ? C32 C33 1.370(8) . ? C33 C34 1.378(8) . ? C34 C35 1.396(6) . ? C35 C43 1.488(6) . ? C36 C37 1.387(6) . ? C36 C41 1.394(7) . ? C37 C38 1.383(7) . ? C38 C39 1.381(8) . ? C39 C40 1.382(8) . ? C39 C42 1.505(8) . ? C40 C41 1.374(8) . ? C43 C44 1.387(6) . ? C43 C48 1.405(6) . ? C44 C45 1.377(6) . ? C45 C46 1.389(7) . ? C46 C47 1.376(7) . ? C46 C49 1.506(6) . ? C47 C48 1.375(7) . ? C1S Cl1 1.7970 . ? C1S Cl1 1.985(8) 3_676 ? Cl1 C1S 1.985(7) 3_676 ? C2S Cl4 1.7036 . ? C2S Cl3 1.7933 . ? C3S Cl5 1.6003 . ? C3S Cl6 1.7478 . ? 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 114.46(13) . . ? O1 Fe1 O3 125.14(12) . . ? O2 Fe1 O3 114.46(13) . . ? O1 Fe1 N1 104.63(13) . . ? O2 Fe1 N1 96.74(12) . . ? O3 Fe1 N1 92.79(12) . . ? O1 Fe1 C6 79.94(12) . . ? O2 Fe1 C6 145.67(12) . . ? O3 Fe1 C6 73.57(12) . . ? N1 Fe1 C6 48.93(12) . . ? O1 Fe1 Fe1 54.27(9) . 3_566 ? O2 Fe1 Fe1 60.65(9) . 3_566 ? O3 Fe1 Fe1 150.29(9) . 3_566 ? N1 Fe1 Fe1 116.61(9) . 3_566 ? C6 Fe1 Fe1 128.54(9) . 3_566 ? C1 N1 C5 118.3(4) . . ? C1 N1 Fe1 118.3(3) . . ? C5 N1 Fe1 122.0(3) . . ? C29 O1 Fe1 156.2(3) 3_566 . ? C29 O2 Fe1 141.1(3) . . ? C8 O3 Fe1 101.5(2) . . ? N1 C1 C2 123.7(4) . . ? C1 C2 C3 117.7(4) . . ? C4 C3 C2 119.1(4) . . ? C3 C4 C5 120.5(4) . . ? N1 C5 C4 120.5(4) . . ? N1 C5 C6 116.9(4) . . ? C4 C5 C6 122.6(4) . . ? C5 C6 C7 114.6(4) . . ? C5 C6 Fe1 70.6(2) . . ? C7 C6 Fe1 172.6(3) . . ? O4 C8 O3 122.1(4) . . ? O4 C8 C9 121.8(4) . . ? O3 C8 C9 116.1(3) . . ? C14 C9 C10 120.3(4) . . ? C14 C9 C8 119.8(4) . . ? C10 C9 C8 119.9(4) . . ? C11 C10 C9 118.8(4) . . ? C11 C10 C15 117.7(4) . . ? C9 C10 C15 123.3(4) . . ? C12 C11 C10 121.2(4) . . ? C13 C12 C11 119.3(4) . . ? C12 C13 C14 121.5(4) . . ? C13 C14 C9 118.8(4) . . ? C13 C14 C22 118.2(4) . . ? C9 C14 C22 123.0(4) . . ? C16 C15 C20 117.8(4) . . ? C16 C15 C10 121.2(4) . . ? C20 C15 C10 120.8(4) . . ? C17 C16 C15 120.8(4) . . ? C18 C17 C16 121.1(4) . . ? C19 C18 C17 118.2(4) . . ? C19 C18 C21 120.9(5) . . ? C17 C18 C21 120.9(5) . . ? C20 C19 C18 121.3(4) . . ? C19 C20 C15 120.8(5) . . ? C23 C22 C27 118.9(4) . . ? C23 C22 C14 121.9(4) . . ? C27 C22 C14 119.1(4) . . ? C22 C23 C24 120.4(5) . . ? C23 C24 C25 121.8(5) . . ? C26 C25 C24 117.6(5) . . ? C26 C25 C28 120.2(5) . . ? C24 C25 C28 122.1(6) . . ? C25 C26 C27 121.7(5) . . ? C26 C27 C22 119.6(5) . . ? O1 C29 O2 125.6(4) 3_566 . ? O1 C29 C30 117.4(4) 3_566 . ? O2 C29 C30 117.0(4) . . ? C31 C30 C35 120.9(4) . . ? C31 C30 C29 118.5(4) . . ? C35 C30 C29 120.7(4) . . ? C32 C31 C30 117.9(4) . . ? C32 C31 C36 119.2(4) . . ? C30 C31 C36 122.9(4) . . ? C33 C32 C31 121.7(5) . . ? C32 C33 C34 120.4(4) . . ? C33 C34 C35 120.5(5) . . ? C34 C35 C30 118.7(4) . . ? C34 C35 C43 118.1(4) . . ? C30 C35 C43 123.1(4) . . ? C37 C36 C41 116.8(5) . . ? C37 C36 C31 124.0(4) . . ? C41 C36 C31 119.2(4) . . ? C38 C37 C36 121.3(5) . . ? C39 C38 C37 121.3(5) . . ? C38 C39 C40 117.6(5) . . ? C38 C39 C42 121.4(5) . . ? C40 C39 C42 121.1(6) . . ? C41 C40 C39 121.3(5) . . ? C40 C41 C36 121.6(5) . . ? C44 C43 C48 116.6(4) . . ? C44 C43 C35 123.1(4) . . ? C48 C43 C35 120.3(4) . . ? C45 C44 C43 121.6(4) . . ? C44 C45 C46 121.0(5) . . ? C47 C46 C45 118.2(5) . . ? C47 C46 C49 120.7(4) . . ? C45 C46 C49 121.1(5) . . ? C48 C47 C46 120.8(5) . . ? C47 C48 C43 121.7(5) . . ? Cl1 C1S Cl1 95.1(4) . 3_676 ? C1S Cl1 C1S 84.8(4) . 3_676 ? Cl4 C2S Cl3 102.0 . . ? Cl5 C3S Cl6 118.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.952 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.082