[Fe2(m-O2CArTol)2(O2CArTol)2(2-(4-ClBn)py)2] (2) data_082202sad2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H88 Cl2 Fe2 N2 O8' _chemical_formula_weight 1724.40 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' '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca 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' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.751(3) _cell_length_b 23.133(5) _cell_length_c 27.455(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8734(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1019 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.13 _exptl_crystal_description Block _exptl_crystal_colour Mint_green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3600 _exptl_absorpt_coefficient_mu 0.455 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.807705 _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 72872 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9955 _reflns_number_gt 9104 _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^)+(0.0518P)^2^+10.6191P] 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 9955 _refine_ls_number_parameters 554 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.1667 _refine_ls_wR_factor_gt 0.1635 _refine_ls_goodness_of_fit_ref 1.340 _refine_ls_restrained_S_all 1.340 _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 0.13871(3) 0.474348(16) 0.033169(13) 0.02248(11) Uani 1 1 d . . . N1 N 0.18141(17) 0.38755(10) 0.01577(9) 0.0281(5) Uani 1 1 d . . . O1 O 0.12841(15) 0.50405(9) -0.03507(7) 0.0317(4) Uani 1 1 d . . . O2 O 0.01051(14) 0.45792(9) 0.06218(8) 0.0321(4) Uani 1 1 d . . . O3 O 0.26553(14) 0.48786(9) 0.07200(7) 0.0308(4) Uani 1 1 d . . . O4 O 0.16072(14) 0.55851(9) 0.07697(8) 0.0328(5) Uani 1 1 d . . . C1 C 0.1887(2) 0.34509(13) 0.04939(11) 0.0304(6) Uani 1 1 d . . . C2 C 0.2182(3) 0.28981(14) 0.03680(12) 0.0404(7) Uani 1 1 d . . . H2A H 0.2226 0.2606 0.0610 0.048 Uiso 1 1 calc R . . C3 C 0.2411(3) 0.27741(15) -0.01073(13) 0.0443(8) Uani 1 1 d . . . H3A H 0.2611 0.2396 -0.0198 0.053 Uiso 1 1 calc R . . C4 C 0.2347(3) 0.32047(15) -0.04481(12) 0.0429(8) Uani 1 1 d . . . H4A H 0.2510 0.3131 -0.0779 0.051 Uiso 1 1 calc R . . C5 C 0.2043(2) 0.37459(14) -0.03044(11) 0.0360(7) Uani 1 1 d . . . H5A H 0.1992 0.4041 -0.0544 0.043 Uiso 1 1 calc R . . C6 C 0.1610(2) 0.35980(14) 0.10105(11) 0.0360(7) Uani 1 1 d . . . H6A H 0.0915 0.3502 0.1060 0.043 Uiso 1 1 calc R . . H6B H 0.1684 0.4020 0.1059 0.043 Uiso 1 1 calc R . . C7 C 0.2205(2) 0.32866(13) 0.13911(11) 0.0347(6) Uani 1 1 d . . . C8 C 0.1813(3) 0.28633(18) 0.16829(15) 0.0577(10) Uani 1 1 d . . . H8A H 0.1151 0.2757 0.1642 0.069 Uiso 1 1 calc R . . C9 C 0.2368(4) 0.2588(2) 0.20357(16) 0.0667(12) Uani 1 1 d . . . H9A H 0.2093 0.2292 0.2232 0.080 Uiso 1 1 calc R . . C10 C 0.3309(3) 0.27479(16) 0.20970(13) 0.0490(9) Uani 1 1 d . . . C11 C 0.3725(3) 0.31581(17) 0.18102(15) 0.0540(9) Uani 1 1 d . . . H11A H 0.4389 0.3260 0.1852 0.065 Uiso 1 1 calc R . . C12 C 0.3167(3) 0.34265(16) 0.14550(14) 0.0472(8) Uani 1 1 d . . . H12A H 0.3456 0.3712 0.1253 0.057 Uiso 1 1 calc R . . Cl1 Cl 0.39958(10) 0.24195(6) 0.25564(4) 0.0776(4) Uani 1 1 d . . . C13 C 0.0791(2) 0.53437(11) -0.06385(10) 0.0259(5) Uani 1 1 d . . . C14 C 0.1333(2) 0.56520(13) -0.10385(10) 0.0295(6) Uani 1 1 d . . . C15 C 0.1414(2) 0.62580(14) -0.10272(11) 0.0338(6) Uani 1 1 d . . . C16 C 0.1949(3) 0.65262(17) -0.13962(13) 0.0495(9) Uani 1 1 d . . . H16A H 0.2010 0.6935 -0.1395 0.059 Uiso 1 1 calc R . . C17 C 0.2390(3) 0.62125(19) -0.17620(14) 0.0586(11) Uani 1 1 d . . . H17A H 0.2755 0.6405 -0.2007 0.070 Uiso 1 1 calc R . . C18 C 0.2300(3) 0.56190(18) -0.17726(13) 0.0506(9) Uani 1 1 d . . . H18A H 0.2605 0.5405 -0.2026 0.061 Uiso 1 1 calc R . . C19 C 0.1767(2) 0.53296(15) -0.14153(11) 0.0361(7) Uani 1 1 d . . . C20 C 0.0994(2) 0.66171(13) -0.06335(12) 0.0338(6) Uani 1 1 d . . . C21 C 0.1025(2) 0.64495(12) -0.01458(11) 0.0324(6) Uani 1 1 d . . . H21A H 0.1293 0.6084 -0.0064 0.039 Uiso 1 1 calc R . . C22 C 0.0677(2) 0.68014(14) 0.02223(12) 0.0385(7) Uani 1 1 d . . . H22A H 0.0706 0.6673 0.0551 0.046 Uiso 1 1 calc R . . C23 C 0.0284(3) 0.73402(14) 0.01180(15) 0.0448(8) Uani 1 1 d . . . C24 C 0.0233(3) 0.75065(15) -0.03651(15) 0.0476(9) Uani 1 1 d . . . H24A H -0.0049 0.7869 -0.0445 0.057 Uiso 1 1 calc R . . C25 C 0.0582(2) 0.71591(14) -0.07342(14) 0.0431(8) Uani 1 1 d . . . H25A H 0.0543 0.7289 -0.1062 0.052 Uiso 1 1 calc R . . C26 C -0.0046(3) 0.77342(17) 0.05205(18) 0.0631(11) Uani 1 1 d . . . H26A H 0.0350 0.8086 0.0519 0.095 Uiso 1 1 calc R . . H26B H 0.0026 0.7537 0.0834 0.095 Uiso 1 1 calc R . . H26C H -0.0731 0.7836 0.0470 0.095 Uiso 1 1 calc R . . C27 C 0.1649(2) 0.46923(15) -0.14611(10) 0.0361(7) Uani 1 1 d . . . C28 C 0.0747(2) 0.44266(15) -0.14190(11) 0.0389(7) Uani 1 1 d . . . H28A H 0.0193 0.4651 -0.1335 0.047 Uiso 1 1 calc R . . C29 C 0.0645(3) 0.38388(16) -0.14978(12) 0.0449(8) Uani 1 1 d . . . H29A H 0.0020 0.3666 -0.1468 0.054 Uiso 1 1 calc R . . C30 C 0.1437(3) 0.34961(17) -0.16200(12) 0.0504(9) Uani 1 1 d . . . C31 C 0.2337(3) 0.37599(18) -0.16553(12) 0.0511(9) Uani 1 1 d . . . H31A H 0.2891 0.3533 -0.1734 0.061 Uiso 1 1 calc R . . C32 C 0.2447(3) 0.43455(17) -0.15784(12) 0.0462(8) Uani 1 1 d . . . H32A H 0.3074 0.4515 -0.1605 0.055 Uiso 1 1 calc R . . C33 C 0.1316(4) 0.28582(19) -0.17106(17) 0.0691(13) Uani 1 1 d . . . H33A H 0.1911 0.2704 -0.1858 0.104 Uiso 1 1 calc R . . H33B H 0.0767 0.2795 -0.1932 0.104 Uiso 1 1 calc R . . H33C H 0.1192 0.2661 -0.1401 0.104 Uiso 1 1 calc R . . C34 C 0.2411(2) 0.53756(12) 0.08762(10) 0.0279(6) Uani 1 1 d . . . C35 C 0.3110(2) 0.57083(13) 0.11969(11) 0.0331(6) Uani 1 1 d . . . C36 C 0.2912(2) 0.57484(14) 0.16948(12) 0.0376(7) Uani 1 1 d . . . C37 C 0.3526(3) 0.60819(16) 0.19862(14) 0.0500(9) Uani 1 1 d . . . H37A H 0.3394 0.6119 0.2324 0.060 Uiso 1 1 calc R . . C38 C 0.4319(3) 0.63573(17) 0.17887(15) 0.0570(10) Uani 1 1 d . . . H38A H 0.4721 0.6591 0.1990 0.068 Uiso 1 1 calc R . . C39 C 0.4534(3) 0.62979(15) 0.13039(14) 0.0478(9) Uani 1 1 d . . . H39A H 0.5099 0.6478 0.1176 0.057 Uiso 1 1 calc R . . C40 C 0.3934(2) 0.59754(13) 0.09951(12) 0.0367(7) Uani 1 1 d . . . C41 C 0.2099(2) 0.54221(15) 0.19247(11) 0.0384(7) Uani 1 1 d . . . C42 C 0.2010(3) 0.48312(16) 0.18598(11) 0.0431(8) Uani 1 1 d . . . H42A H 0.2468 0.4633 0.1662 0.052 Uiso 1 1 calc R . . C43 C 0.1262(3) 0.4524(2) 0.20795(13) 0.0547(10) Uani 1 1 d . . . H43A H 0.1213 0.4119 0.2028 0.066 Uiso 1 1 calc R . . C44 C 0.0592(3) 0.4797(2) 0.23708(13) 0.0599(11) Uani 1 1 d . . . C45 C 0.0691(3) 0.5381(2) 0.24423(14) 0.0655(13) Uani 1 1 d . . . H45A H 0.0241 0.5576 0.2647 0.079 Uiso 1 1 calc R . . C46 C 0.1434(3) 0.5694(2) 0.22232(14) 0.0539(10) Uani 1 1 d . . . H46A H 0.1483 0.6098 0.2279 0.065 Uiso 1 1 calc R . . C47 C -0.0224(4) 0.4462(3) 0.26047(17) 0.095(2) Uani 1 1 d . . . H47A H -0.0771 0.4723 0.2670 0.142 Uiso 1 1 calc R . . H47B H 0.0003 0.4293 0.2912 0.142 Uiso 1 1 calc R . . H47C H -0.0436 0.4153 0.2385 0.142 Uiso 1 1 calc R . . C48 C 0.4191(2) 0.59136(13) 0.04722(12) 0.0366(7) Uani 1 1 d . . . C49 C 0.3492(2) 0.59799(16) 0.01071(13) 0.0421(8) Uani 1 1 d . . . H49A H 0.2853 0.6100 0.0191 0.050 Uiso 1 1 calc R . . C50 C 0.3720(2) 0.58737(17) -0.03737(13) 0.0462(8) Uani 1 1 d . . . H50A H 0.3228 0.5912 -0.0614 0.055 Uiso 1 1 calc R . . C51 C 0.4648(3) 0.57124(14) -0.05142(13) 0.0425(8) Uani 1 1 d . . . C52 C 0.5357(3) 0.56763(15) -0.01559(14) 0.0448(8) Uani 1 1 d . . . H52A H 0.6006 0.5582 -0.0244 0.054 Uiso 1 1 calc R . . C53 C 0.5132(2) 0.57761(14) 0.03281(13) 0.0410(7) Uani 1 1 d . . . H53A H 0.5630 0.5750 0.0567 0.049 Uiso 1 1 calc R . . C54 C 0.4867(3) 0.5574(2) -0.10359(15) 0.0589(10) Uani 1 1 d . . . H54A H 0.4398 0.5288 -0.1156 0.088 Uiso 1 1 calc R . . H54B H 0.5527 0.5415 -0.1061 0.088 Uiso 1 1 calc R . . H54C H 0.4821 0.5926 -0.1232 0.088 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 0.01943(19) 0.0259(2) 0.02208(19) 0.00090(14) -0.00257(14) -0.00002(14) N1 0.0240(11) 0.0323(12) 0.0280(11) -0.0014(9) -0.0039(9) 0.0017(9) O1 0.0371(11) 0.0336(10) 0.0242(10) 0.0045(8) 0.0015(8) 0.0057(9) O2 0.0235(10) 0.0370(11) 0.0358(11) 0.0031(9) 0.0039(8) -0.0036(8) O3 0.0259(10) 0.0352(11) 0.0313(10) -0.0059(8) -0.0045(8) -0.0007(8) O4 0.0266(10) 0.0385(11) 0.0334(11) 0.0006(9) -0.0066(8) -0.0001(8) C1 0.0271(14) 0.0328(15) 0.0313(14) -0.0006(11) -0.0058(11) 0.0031(11) C2 0.0479(19) 0.0334(16) 0.0398(17) 0.0020(13) -0.0048(14) 0.0105(14) C3 0.0466(19) 0.0380(17) 0.0482(19) -0.0097(15) -0.0087(16) 0.0159(15) C4 0.049(2) 0.0460(19) 0.0334(16) -0.0085(14) -0.0026(14) 0.0159(15) C5 0.0404(17) 0.0399(16) 0.0277(14) 0.0025(12) -0.0045(13) 0.0078(13) C6 0.0414(17) 0.0353(15) 0.0314(15) 0.0025(12) -0.0008(13) 0.0077(13) C7 0.0406(17) 0.0326(15) 0.0308(15) 0.0011(12) -0.0013(13) 0.0015(13) C8 0.053(2) 0.066(3) 0.054(2) 0.0234(19) -0.0115(18) -0.014(2) C9 0.075(3) 0.070(3) 0.055(2) 0.031(2) -0.009(2) -0.011(2) C10 0.066(2) 0.048(2) 0.0331(17) 0.0075(14) -0.0144(16) 0.0162(18) C11 0.045(2) 0.054(2) 0.063(2) 0.0041(19) -0.0147(18) 0.0023(17) C12 0.048(2) 0.0439(19) 0.050(2) 0.0132(16) -0.0051(16) -0.0020(16) Cl1 0.0936(9) 0.0863(8) 0.0529(6) 0.0170(6) -0.0225(6) 0.0324(7) C13 0.0272(14) 0.0254(13) 0.0250(13) 0.0000(10) 0.0011(10) -0.0026(10) C14 0.0225(13) 0.0411(16) 0.0250(13) 0.0086(11) -0.0032(11) -0.0025(11) C15 0.0273(14) 0.0405(16) 0.0335(15) 0.0124(12) -0.0044(12) -0.0047(12) C16 0.051(2) 0.051(2) 0.047(2) 0.0195(16) 0.0032(17) -0.0108(17) C17 0.058(2) 0.073(3) 0.045(2) 0.0239(19) 0.0168(18) -0.015(2) C18 0.049(2) 0.071(3) 0.0322(17) 0.0083(16) 0.0140(15) -0.0037(18) C19 0.0302(15) 0.0514(19) 0.0268(14) 0.0049(13) 0.0008(12) -0.0004(13) C20 0.0281(14) 0.0310(15) 0.0424(17) 0.0086(12) -0.0066(12) -0.0065(12) C21 0.0298(14) 0.0250(13) 0.0424(16) 0.0077(12) -0.0062(13) -0.0038(11) C22 0.0367(17) 0.0357(16) 0.0431(17) 0.0032(13) -0.0018(14) -0.0055(13) C23 0.0387(18) 0.0328(16) 0.063(2) 0.0006(15) 0.0009(16) -0.0039(13) C24 0.0419(18) 0.0289(15) 0.072(2) 0.0097(16) -0.0078(17) 0.0016(14) C25 0.0421(18) 0.0354(17) 0.0516(19) 0.0155(15) -0.0114(15) -0.0050(14) C26 0.068(3) 0.040(2) 0.080(3) -0.008(2) 0.007(2) 0.0041(19) C27 0.0410(17) 0.0521(19) 0.0153(12) 0.0024(12) 0.0037(11) 0.0020(14) C28 0.0415(17) 0.0481(18) 0.0272(14) 0.0014(13) -0.0018(13) 0.0045(14) C29 0.048(2) 0.053(2) 0.0337(16) 0.0025(15) -0.0083(15) -0.0035(16) C30 0.074(3) 0.051(2) 0.0263(16) -0.0024(14) -0.0027(16) 0.0105(19) C31 0.058(2) 0.063(2) 0.0320(17) -0.0034(16) 0.0083(16) 0.0169(19) C32 0.0439(19) 0.064(2) 0.0303(16) -0.0017(15) 0.0098(14) 0.0047(17) C33 0.098(4) 0.056(2) 0.053(2) -0.010(2) -0.001(2) 0.008(2) C34 0.0281(14) 0.0334(14) 0.0223(12) 0.0015(11) -0.0024(11) -0.0056(11) C35 0.0305(15) 0.0324(15) 0.0365(15) -0.0051(12) -0.0092(12) 0.0032(12) C36 0.0392(17) 0.0357(16) 0.0379(16) -0.0077(13) -0.0105(14) 0.0052(13) C37 0.058(2) 0.051(2) 0.0412(19) -0.0140(16) -0.0152(17) 0.0005(17) C38 0.066(3) 0.046(2) 0.059(2) -0.0121(18) -0.028(2) -0.0128(19) C39 0.0443(19) 0.0386(18) 0.060(2) 0.0012(16) -0.0180(17) -0.0107(15) C40 0.0320(15) 0.0319(15) 0.0462(18) 0.0010(13) -0.0124(13) -0.0032(12) C41 0.0379(16) 0.0539(19) 0.0234(14) -0.0064(13) -0.0103(12) 0.0060(14) C42 0.051(2) 0.055(2) 0.0237(14) -0.0035(13) -0.0026(14) -0.0015(16) C43 0.064(2) 0.069(3) 0.0310(17) 0.0048(17) -0.0040(17) -0.013(2) C44 0.049(2) 0.105(4) 0.0259(17) 0.0080(19) -0.0064(15) -0.007(2) C45 0.044(2) 0.114(4) 0.039(2) -0.011(2) -0.0002(17) 0.020(2) C46 0.047(2) 0.073(3) 0.0416(19) -0.0165(18) -0.0093(16) 0.0146(19) C47 0.069(3) 0.167(6) 0.048(3) 0.020(3) 0.007(2) -0.030(4) C48 0.0318(15) 0.0309(15) 0.0470(18) 0.0052(13) -0.0052(13) -0.0081(12) C49 0.0250(15) 0.053(2) 0.0482(19) 0.0118(16) -0.0034(13) -0.0062(14) C50 0.0347(17) 0.060(2) 0.0439(19) 0.0146(16) -0.0078(14) -0.0121(15) C51 0.0413(18) 0.0364(17) 0.0497(19) 0.0089(14) 0.0025(15) -0.0137(14) C52 0.0313(16) 0.0420(18) 0.061(2) 0.0043(16) 0.0013(15) -0.0011(14) C53 0.0296(15) 0.0386(17) 0.055(2) 0.0061(15) -0.0103(14) -0.0070(13) C54 0.057(2) 0.066(3) 0.054(2) 0.0077(19) 0.0058(19) -0.011(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 2.000(2) . ? Fe1 O3 2.068(2) . ? Fe1 N1 2.146(2) . ? Fe1 O4 2.308(2) . ? Fe1 C6 3.254(3) . ? Fe1 Fe1 4.3907(11) 5_565 ? N1 C5 1.341(4) . ? N1 C1 1.352(4) . ? O1 C13 1.256(3) . ? O2 C13 1.246(3) 5_565 ? O3 C34 1.272(3) . ? O4 C34 1.242(3) . ? C1 C2 1.385(4) . ? C1 C6 1.508(4) . ? C2 C3 1.373(5) . ? C3 C4 1.370(5) . ? C4 C5 1.378(4) . ? C6 C7 1.510(4) . ? C7 C12 1.374(5) . ? C7 C8 1.375(5) . ? C8 C9 1.388(5) . ? C9 C10 1.356(6) . ? C10 C11 1.359(6) . ? C10 Cl1 1.749(3) . ? C11 C12 1.387(5) . ? C13 O2 1.245(3) 5_565 ? C13 C14 1.507(4) . ? C14 C15 1.407(4) . ? C14 C19 1.408(4) . ? C15 C16 1.397(4) . ? C15 C20 1.481(5) . ? C16 C17 1.380(6) . ? C17 C18 1.379(6) . ? C18 C19 1.396(4) . ? C19 C27 1.489(5) . ? C20 C21 1.395(4) . ? C20 C25 1.403(4) . ? C21 C22 1.383(5) . ? C22 C23 1.388(5) . ? C23 C24 1.383(5) . ? C23 C26 1.503(6) . ? C24 C25 1.380(5) . ? C27 C28 1.389(5) . ? C27 C32 1.398(5) . ? C28 C29 1.384(5) . ? C29 C30 1.388(5) . ? C30 C31 1.383(6) . ? C30 C33 1.506(6) . ? C31 C32 1.379(6) . ? C34 C35 1.514(4) . ? C35 C36 1.397(4) . ? C35 C40 1.404(5) . ? C36 C37 1.395(4) . ? C36 C41 1.489(5) . ? C37 C38 1.375(6) . ? C38 C39 1.370(6) . ? C39 C40 1.399(4) . ? C40 C48 1.485(5) . ? C41 C46 1.381(5) . ? C41 C42 1.384(5) . ? C42 C43 1.387(5) . ? C43 C44 1.373(6) . ? C44 C45 1.372(7) . ? C44 C47 1.507(6) . ? C45 C46 1.389(6) . ? C48 C53 1.389(5) . ? C48 C49 1.397(4) . ? C49 C50 1.379(5) . ? C50 C51 1.384(5) . ? C51 C52 1.388(5) . ? C51 C54 1.499(5) . ? C52 C53 1.384(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 O2 Fe1 O1 112.42(9) . . ? O2 Fe1 O3 125.10(9) . . ? O1 Fe1 O3 119.38(9) . . ? O2 Fe1 N1 98.87(9) . . ? O1 Fe1 N1 97.60(9) . . ? O3 Fe1 N1 91.46(8) . . ? O2 Fe1 O4 93.98(8) . . ? O1 Fe1 O4 101.97(8) . . ? O3 Fe1 O4 59.55(7) . . ? N1 Fe1 O4 150.38(8) . . ? O2 Fe1 C6 72.28(8) . . ? O1 Fe1 C6 145.36(8) . . ? O3 Fe1 C6 75.44(8) . . ? N1 Fe1 C6 48.69(9) . . ? O4 Fe1 C6 112.10(8) . . ? O2 Fe1 Fe1 56.14(6) . 5_565 ? O1 Fe1 Fe1 57.13(6) . 5_565 ? O3 Fe1 Fe1 154.93(6) . 5_565 ? N1 Fe1 Fe1 113.47(6) . 5_565 ? O4 Fe1 Fe1 95.86(5) . 5_565 ? C6 Fe1 Fe1 122.64(6) . 5_565 ? C5 N1 C1 117.8(3) . . ? C5 N1 Fe1 119.0(2) . . ? C1 N1 Fe1 123.25(19) . . ? C13 O1 Fe1 145.02(19) . . ? C13 O2 Fe1 150.6(2) 5_565 . ? C34 O3 Fe1 95.04(16) . . ? C34 O4 Fe1 84.85(17) . . ? N1 C1 C2 121.5(3) . . ? N1 C1 C6 117.4(3) . . ? C2 C1 C6 121.1(3) . . ? C3 C2 C1 119.8(3) . . ? C4 C3 C2 118.9(3) . . ? C3 C4 C5 119.0(3) . . ? N1 C5 C4 123.1(3) . . ? C1 C6 C7 113.9(3) . . ? C1 C6 Fe1 70.66(16) . . ? C7 C6 Fe1 146.7(2) . . ? C12 C7 C8 118.1(3) . . ? C12 C7 C6 119.9(3) . . ? C8 C7 C6 122.1(3) . . ? C7 C8 C9 121.2(4) . . ? C10 C9 C8 119.1(4) . . ? C9 C10 C11 121.3(3) . . ? C9 C10 Cl1 119.1(3) . . ? C11 C10 Cl1 119.6(3) . . ? C10 C11 C12 119.1(4) . . ? C7 C12 C11 121.1(3) . . ? O2 C13 O1 126.2(3) 5_565 . ? O2 C13 C14 116.6(2) 5_565 . ? O1 C13 C14 117.1(2) . . ? C15 C14 C19 120.7(3) . . ? C15 C14 C13 119.7(3) . . ? C19 C14 C13 119.7(3) . . ? C16 C15 C14 117.9(3) . . ? C16 C15 C20 119.1(3) . . ? C14 C15 C20 123.0(3) . . ? C17 C16 C15 121.7(3) . . ? C18 C17 C16 120.0(3) . . ? C17 C18 C19 120.6(3) . . ? C18 C19 C14 119.0(3) . . ? C18 C19 C27 118.2(3) . . ? C14 C19 C27 122.7(3) . . ? C21 C20 C25 116.7(3) . . ? C21 C20 C15 122.2(3) . . ? C25 C20 C15 121.0(3) . . ? C22 C21 C20 121.8(3) . . ? C21 C22 C23 120.8(3) . . ? C24 C23 C22 117.9(3) . . ? C24 C23 C26 121.4(3) . . ? C22 C23 C26 120.7(4) . . ? C25 C24 C23 121.7(3) . . ? C24 C25 C20 121.1(3) . . ? C28 C27 C32 117.8(3) . . ? C28 C27 C19 121.9(3) . . ? C32 C27 C19 120.1(3) . . ? C29 C28 C27 120.8(3) . . ? C28 C29 C30 121.3(4) . . ? C31 C30 C29 117.8(3) . . ? C31 C30 C33 121.3(4) . . ? C29 C30 C33 120.9(4) . . ? C32 C31 C30 121.4(4) . . ? C31 C32 C27 120.8(4) . . ? O4 C34 O3 120.5(3) . . ? O4 C34 C35 120.3(3) . . ? O3 C34 C35 119.2(2) . . ? C36 C35 C40 121.0(3) . . ? C36 C35 C34 118.6(3) . . ? C40 C35 C34 120.4(3) . . ? C37 C36 C35 118.6(3) . . ? C37 C36 C41 119.4(3) . . ? C35 C36 C41 121.9(3) . . ? C38 C37 C36 120.7(4) . . ? C39 C38 C37 120.5(3) . . ? C38 C39 C40 121.0(4) . . ? C39 C40 C35 118.1(3) . . ? C39 C40 C48 119.8(3) . . ? C35 C40 C48 122.1(3) . . ? C46 C41 C42 117.9(4) . . ? C46 C41 C36 121.2(3) . . ? C42 C41 C36 120.9(3) . . ? C41 C42 C43 121.0(4) . . ? C44 C43 C42 121.0(4) . . ? C45 C44 C43 117.9(4) . . ? C45 C44 C47 121.2(5) . . ? C43 C44 C47 120.8(5) . . ? C44 C45 C46 121.7(4) . . ? C41 C46 C45 120.4(4) . . ? C53 C48 C49 117.5(3) . . ? C53 C48 C40 121.3(3) . . ? C49 C48 C40 121.3(3) . . ? C50 C49 C48 120.7(3) . . ? C49 C50 C51 121.6(3) . . ? C50 C51 C52 117.8(3) . . ? C50 C51 C54 120.7(3) . . ? C52 C51 C54 121.5(3) . . ? C53 C52 C51 120.8(3) . . ? C52 C53 C48 121.4(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.720 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.082