Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ebbe Nordlander' _publ_contact_author_address ; Chemical Center Lund University Box 124 Lund SE-221 00 SWEDEN ; _publ_contact_author_email EBBE.NORDLANDER@INORG.LU.SE _publ_section_title ; Tetranuclear iron(III) complexes of a new octadentate pyridine-carboxylate ligand and their catalytic activity in alkane oxidation by hydrogen peroxide ; loop_ _publ_author_name 'Ebbe Nordlander' 'Elena A. Gutkina' 'Shaen Mkoyan' C.Pierpont 'Albert A. Shteinman' ; V.V.Strelets ; 'Vladimir M. Trukhan' data_diiron _database_code_depnum_ccdc_archive 'CCDC 255394' _audit_creation_method SHELXL _chemical_name_systematic ; {[Fe2O(L)(PhCO2)]2}(ClO4)4 2H2O 2CH3CN ; _chemical_name_common '((Fe2O(L)(PhCO2))2)(ClO4)4 2H2O 2CH3CN' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H92 Cl4 Fe4 N14 O32' _chemical_formula_weight 2271.00 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.685(1) _cell_length_b 14.468(2) _cell_length_c 15.666(2) _cell_angle_alpha 72.65(1) _cell_angle_beta 68.65(2) _cell_angle_gamma 64.34(3) _cell_volume 2567.9(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1170 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker SMART CCD' _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 22692 _diffrn_reflns_av_R_equivalents 0.2369 _diffrn_reflns_av_sigmaI/netI 1.3946 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 31.95 _reflns_number_total 15478 _reflns_number_gt 1949 _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 ? _computing_publication_material ? _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^)+(0.0202P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef na _refine_ls_number_reflns 15478 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3358 _refine_ls_R_factor_gt 0.0984 _refine_ls_wR_factor_ref 0.2029 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 0.778 _refine_ls_restrained_S_all 0.778 _refine_ls_shift/su_max 0.354 _refine_ls_shift/su_mean 0.010 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 -0.29343(15) 0.25017(15) 0.20896(12) 0.0451(6) Uani 1 1 d . . . Fe2 Fe -0.21561(15) 0.26748(15) 0.36509(11) 0.0451(6) Uani 1 1 d . . . O5 O -0.2716(6) 0.4213(6) 0.3070(5) 0.045(2) Uani 1 1 d . . . O2 O -0.4290(6) 0.2528(6) 0.3144(5) 0.053(3) Uani 1 1 d . . . O4 O -0.3312(6) 0.4043(6) 0.1973(5) 0.052(3) Uani 1 1 d . . . O1 O -0.1863(5) 0.2139(6) 0.2664(4) 0.043(2) Uani 1 1 d . . . O3 O -0.3788(6) 0.2782(6) 0.4243(5) 0.053(3) Uani 1 1 d . . . O7 O -0.1424(7) 0.4934(7) 0.0828(5) 0.052(3) Uani 1 1 d . . . N1 N -0.1702(9) 0.2179(9) 0.0774(7) 0.056(3) Uani 1 1 d . . . C9 C -0.3156(12) 0.5641(12) 0.1865(9) 0.045(4) Uani 1 1 d . . . N3 N -0.3963(8) 0.3039(8) 0.1156(6) 0.045(3) Uani 1 1 d . . . C10 C -0.2350(11) 0.5825(13) 0.1093(10) 0.052(4) Uani 1 1 d . . . O6 O -0.4938(8) 0.6324(9) 0.2952(7) 0.084(4) Uani 1 1 d . . . N2 N -0.2580(10) 0.0914(9) 0.2073(8) 0.050(3) Uani 1 1 d . . . C14 C -0.4107(13) 0.6497(13) 0.2186(10) 0.053(4) Uani 1 1 d . . . C8 C -0.3054(10) 0.4562(10) 0.2334(7) 0.040(3) Uani 1 1 d . . . C6 C -0.7583(12) 0.3075(12) 0.4896(11) 0.081(5) Uani 1 1 d . . . H6A H -0.8146 0.3041 0.4722 0.097 Uiso 1 1 calc R . . C25 C -0.5066(10) 0.3614(9) 0.1360(8) 0.041(3) Uani 1 1 d . . . H25A H -0.5439 0.3769 0.1957 0.049 Uiso 1 1 calc R . . C29 C -0.3461(10) 0.2857(10) 0.0269(9) 0.043(4) Uani 1 1 d . . . C2 C -0.5648(11) 0.2859(10) 0.4582(9) 0.053(4) Uani 1 1 d . . . C30 C -0.1547(16) 0.0387(13) 0.1640(9) 0.056(4) Uani 1 1 d . . . C17 C -0.1064(10) 0.2906(11) 0.0386(8) 0.064(4) Uani 1 1 d . . . H17A H -0.0840 0.2965 0.0882 0.077 Uiso 1 1 calc R . . H17B H -0.0382 0.2601 -0.0081 0.077 Uiso 1 1 calc R . . C16 C -0.1708(9) 0.3979(9) -0.0041(7) 0.049(4) Uani 1 1 d . . . H16A H -0.2481 0.4202 0.0341 0.059 Uiso 1 1 calc R . . H16B H -0.1716 0.3957 -0.0651 0.059 Uiso 1 1 calc R . . C28 C -0.3966(13) 0.3175(12) -0.0453(10) 0.077(5) Uani 1 1 d . . . C1 C -0.4459(10) 0.2718(9) 0.3957(9) 0.044(4) Uani 1 1 d . . . C19 C -0.0914(10) 0.1091(11) 0.1015(9) 0.076(5) Uani 1 1 d . . . H19A H -0.0426 0.1107 0.1326 0.091 Uiso 1 1 calc R . . H19B H -0.0443 0.0810 0.0448 0.091 Uiso 1 1 calc R . . C7 C -0.6497(11) 0.2891(11) 0.4267(9) 0.071(5) Uani 1 1 d . . . H7A H -0.6353 0.2796 0.3666 0.085 Uiso 1 1 calc R . . C27 C -0.5125(14) 0.3752(12) -0.0160(10) 0.082(6) Uani 1 1 d . . . H27A H -0.5548 0.3990 -0.0583 0.098 Uiso 1 1 calc R . . C15 C -0.1197(10) 0.4766(10) -0.0135(8) 0.066(4) Uani 1 1 d . . . H15A H -0.0393 0.4502 -0.0426 0.079 Uiso 1 1 calc R . . H15B H -0.1540 0.5415 -0.0512 0.079 Uiso 1 1 calc R . . C18 C -0.2218(10) 0.2209(10) 0.0053(8) 0.069(5) Uani 1 1 d . . . H18A H -0.1837 0.2497 -0.0554 0.082 Uiso 1 1 calc R . . H18B H -0.2107 0.1506 0.0033 0.082 Uiso 1 1 calc R . . C11 C -0.2421(13) 0.6842(14) 0.0659(9) 0.075(5) Uani 1 1 d . . . H11A H -0.1844 0.6959 0.0150 0.089 Uiso 1 1 calc R . . C26 C -0.5659(11) 0.3979(10) 0.0718(9) 0.069(5) Uani 1 1 d . . . H26A H -0.6424 0.4382 0.0876 0.083 Uiso 1 1 calc R . . C5 C -0.7826(12) 0.3302(11) 0.5757(11) 0.080(5) Uani 1 1 d . . . H5A H -0.8555 0.3458 0.6149 0.095 Uiso 1 1 calc R . . C22 C -0.6496(11) 0.5913(11) 0.3702(8) 0.083(5) Uani 1 1 d . . . H22A H -0.6357 0.5175 0.3881 0.099 Uiso 1 1 calc R . . H22B H -0.7185 0.6246 0.3509 0.099 Uiso 1 1 calc R . . C13 C -0.4184(15) 0.7494(13) 0.1741(11) 0.090(6) Uani 1 1 d . . . H13A H -0.4818 0.8052 0.1962 0.108 Uiso 1 1 calc R . . C4 C -0.6971(13) 0.3294(11) 0.6034(10) 0.078(5) Uani 1 1 d . . . H4A H -0.7118 0.3416 0.6627 0.093 Uiso 1 1 calc R . . C12 C -0.3372(15) 0.7680(13) 0.0998(12) 0.095(6) Uani 1 1 d . . . H12A H -0.3438 0.8359 0.0711 0.114 Uiso 1 1 calc R . . C33 C -0.2874(16) -0.0688(15) 0.2741(12) 0.108(7) Uani 1 1 d . . . H33A H -0.3349 -0.1045 0.3117 0.130 Uiso 1 1 calc R . . C31 C -0.1049(14) -0.0669(15) 0.1698(11) 0.093(6) Uani 1 1 d . . . H31A H -0.0304 -0.1002 0.1383 0.111 Uiso 1 1 calc R . . C21 C -0.6686(9) 0.6344(11) 0.4572(8) 0.075(5) Uani 1 1 d . . . H21A H -0.6300 0.5771 0.4988 0.090 Uiso 1 1 calc R . . H21B H -0.6315 0.6842 0.4369 0.090 Uiso 1 1 calc R . . N4 N -0.7821(9) 0.6836(10) 0.5103(7) 0.071(4) Uani 1 1 d . . . N6 N -0.8260(9) 0.8812(9) 0.5380(8) 0.077(4) Uani 1 1 d . . . H6B H -0.8245 0.8291 0.5826 0.093 Uiso 1 1 calc R . . N5 N -0.9449(8) 0.7099(8) 0.6753(7) 0.053(3) Uani 1 1 d . . . H5B H -0.8883 0.7288 0.6595 0.063 Uiso 1 1 calc R . . C38 C -1.1226(11) 0.7172(13) 0.7798(9) 0.079(5) Uani 1 1 d . . . H38A H -1.1809 0.7404 0.8315 0.095 Uiso 1 1 calc R . . C36 C -1.0377(13) 0.6136(12) 0.6584(11) 0.081(5) Uani 1 1 d . . . H36A H -1.0382 0.5663 0.6295 0.097 Uiso 1 1 calc R . . C37 C -1.1256(13) 0.6523(12) 0.7314(12) 0.089(6) Uani 1 1 d . . . H37A H -1.1890 0.6348 0.7492 0.107 Uiso 1 1 calc R . . C39 C -1.0315(12) 0.7450(10) 0.7487(9) 0.057(4) Uani 1 1 d . . . H39A H -1.0284 0.7898 0.7789 0.069 Uiso 1 1 calc R . . C23 C -0.8552(12) 0.7781(13) 0.4595(9) 0.084(6) Uani 1 1 d . . . H23A H -0.8399 0.7685 0.3966 0.100 Uiso 1 1 calc R . . H23B H -0.9341 0.7896 0.4908 0.100 Uiso 1 1 calc R . . C44 C -0.8301(14) 0.8684(14) 0.4576(10) 0.095(6) Uani 1 1 d . . . C40 C -0.8238(15) 0.9640(16) 0.5573(14) 0.144(9) Uani 1 1 d . . . H40A H -0.7584 0.9431 0.5793 0.173 Uiso 1 1 calc R . . H40B H -0.8905 0.9911 0.6066 0.173 Uiso 1 1 calc R . . C24 C -0.8461(12) 0.6066(12) 0.5530(9) 0.080(5) Uani 1 1 d . . . H24A H -0.8701 0.5977 0.5057 0.096 Uiso 1 1 calc R . . H24B H -0.7970 0.5392 0.5769 0.096 Uiso 1 1 calc R . . C32 C -0.1744(18) -0.1190(13) 0.2261(13) 0.124(8) Uani 1 1 d . . . H32A H -0.1458 -0.1912 0.2332 0.149 Uiso 1 1 calc R . . Cl1 Cl -1.1157(4) 0.3726(4) 0.7294(3) 0.0725(13) Uani 1 1 d . . . O9 O -1.2191(9) 0.4577(9) 0.7611(7) 0.128(5) Uani 1 1 d . . . O8 O -1.0787(8) 0.3967(9) 0.6346(6) 0.115(4) Uani 1 1 d . . . C20 C -0.5638(16) 0.605(2) 0.2964(12) 0.217(15) Uani 1 1 d . . . H20A H -0.5597 0.5913 0.2406 0.260 Uiso 1 1 calc R . . C3 C -0.5909(11) 0.3108(11) 0.5440(10) 0.064(4) Uani 1 1 d . . . H3A H -0.5355 0.3151 0.5620 0.077 Uiso 1 1 calc R . . C41 C -0.820(3) 1.044(2) 0.478(2) 0.26(2) Uani 1 1 d . . . H41A H -0.8119 1.1027 0.4829 0.308 Uiso 1 1 calc R . . C35 C -0.9424(12) 0.6486(12) 0.6267(9) 0.066(4) Uani 1 1 d . . . C42 C -0.826(3) 1.039(2) 0.401(2) 0.207(17) Uani 1 1 d . . . H42A H -0.8257 1.0948 0.3530 0.248 Uiso 1 1 calc R . . C43 C -0.8350(18) 0.9508(18) 0.3864(16) 0.169(12) Uani 1 1 d . . . H43A H -0.8436 0.9494 0.3306 0.203 Uiso 1 1 calc R . . C34 C -0.3201(14) 0.0350(13) 0.2606(10) 0.076(5) Uani 1 1 d . . . H34A H -0.3938 0.0712 0.2916 0.092 Uiso 1 1 calc R . . Cl2 Cl -0.7754(5) 1.0028(5) 0.1051(4) 0.1024(18) Uani 1 1 d . . . O11 O -1.0356(7) 0.3640(8) 0.7712(6) 0.100(4) Uani 1 1 d . . . O10 O -1.1373(11) 0.2809(9) 0.7561(8) 0.164(6) Uani 1 1 d . . . N7 N -1.3898(13) 0.8505(15) 0.7530(13) 0.139(7) Uani 1 1 d . . . C45 C -0.5587(18) 0.1098(19) 0.1767(17) 0.138(10) Uani 1 1 d . . . O15 O -0.7757(13) 1.0038(12) 0.0207(10) 0.208(7) Uani 1 1 d . . . O14 O -0.8575(13) 0.9709(13) 0.1711(11) 0.226(9) Uani 1 1 d . . . C46 C -0.5075(17) 0.0823(17) 0.0938(13) 0.143(8) Uani 1 1 d . . . O13 O -0.6724(12) 0.9373(14) 0.1178(13) 0.292(12) Uani 1 1 d . . . O12 O -0.7926(18) 1.0903(16) 0.1147(13) 0.298(13) Uani 1 1 d . . . O16 O -0.4433(16) 0.011(4) 0.540(3) 0.80(6) Uani 1 1 d . . . 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 0.0453(13) 0.0542(16) 0.0400(12) -0.0150(11) -0.0125(11) -0.0166(12) Fe2 0.0444(14) 0.0566(16) 0.0368(12) -0.0102(11) -0.0172(10) -0.0142(12) O5 0.072(7) 0.043(6) 0.034(5) -0.002(4) -0.032(5) -0.022(5) O2 0.039(6) 0.092(8) 0.038(5) -0.014(5) -0.008(5) -0.034(6) O4 0.043(6) 0.075(8) 0.049(5) -0.019(5) -0.024(5) -0.016(6) O1 0.027(5) 0.054(6) 0.046(5) -0.019(4) -0.012(4) -0.005(5) O3 0.034(6) 0.085(8) 0.058(6) -0.018(5) -0.026(5) -0.023(6) O7 0.050(6) 0.076(8) 0.039(5) -0.015(5) -0.002(5) -0.035(6) N1 0.054(8) 0.047(9) 0.062(8) -0.044(7) -0.004(7) -0.001(7) C9 0.051(10) 0.055(12) 0.044(9) 0.007(9) -0.015(8) -0.041(10) N3 0.029(7) 0.071(9) 0.039(7) -0.032(6) -0.003(6) -0.012(7) C10 0.033(10) 0.065(13) 0.064(11) -0.032(10) -0.010(9) -0.013(10) O6 0.067(8) 0.126(10) 0.056(7) -0.056(7) 0.006(6) -0.026(8) N2 0.031(8) 0.061(10) 0.051(8) -0.023(7) -0.013(7) -0.001(8) C14 0.063(13) 0.046(11) 0.054(10) -0.008(10) -0.021(10) -0.019(11) C8 0.042(9) 0.059(11) 0.027(7) -0.006(7) -0.012(7) -0.026(8) C6 0.047(11) 0.109(15) 0.087(13) -0.012(12) -0.012(10) -0.038(11) C25 0.036(9) 0.044(9) 0.050(8) -0.008(7) -0.018(8) -0.015(8) C29 0.020(8) 0.053(10) 0.054(9) -0.015(8) 0.002(8) -0.019(8) C2 0.058(10) 0.069(11) 0.044(9) -0.004(8) -0.009(8) -0.041(9) C30 0.095(15) 0.046(12) 0.035(9) -0.005(9) -0.033(10) -0.023(12) C17 0.040(10) 0.085(13) 0.060(10) -0.037(9) -0.011(8) -0.004(10) C16 0.041(9) 0.047(10) 0.042(8) 0.005(7) 0.002(7) -0.020(8) C28 0.073(12) 0.115(15) 0.070(11) 0.009(10) -0.048(11) -0.051(12) C1 0.030(9) 0.028(9) 0.062(10) 0.011(7) -0.005(8) -0.018(7) C19 0.067(12) 0.077(13) 0.065(10) -0.038(10) -0.041(9) 0.026(11) C7 0.057(10) 0.096(13) 0.070(11) 0.004(10) -0.021(10) -0.046(11) C27 0.105(15) 0.125(16) 0.045(10) 0.012(10) -0.046(12) -0.065(14) C15 0.041(9) 0.061(11) 0.085(11) -0.001(9) -0.006(9) -0.025(9) C18 0.101(13) 0.085(13) 0.053(9) -0.014(9) -0.041(10) -0.045(11) C11 0.083(14) 0.075(14) 0.066(11) -0.007(11) 0.015(10) -0.062(12) C26 0.060(11) 0.087(13) 0.074(11) -0.002(10) -0.046(10) -0.025(10) C5 0.056(12) 0.066(12) 0.096(13) -0.023(11) 0.014(11) -0.026(10) C22 0.094(13) 0.115(15) 0.062(10) -0.057(10) -0.003(10) -0.046(12) C13 0.115(17) 0.047(13) 0.068(12) -0.005(11) -0.023(12) 0.003(12) C4 0.080(13) 0.091(14) 0.072(11) -0.038(10) -0.007(11) -0.036(12) C12 0.14(2) 0.056(14) 0.095(15) 0.010(13) -0.046(14) -0.042(15) C33 0.105(16) 0.069(17) 0.145(19) -0.048(15) -0.027(15) -0.014(15) C31 0.086(15) 0.055(14) 0.119(16) -0.020(12) -0.027(13) -0.007(13) C21 0.019(8) 0.147(16) 0.063(10) -0.071(10) 0.003(8) -0.009(10) N4 0.054(9) 0.093(11) 0.056(8) -0.027(8) -0.027(8) 0.004(9) N6 0.086(10) 0.061(10) 0.081(10) 0.037(8) -0.042(8) -0.040(9) N5 0.027(7) 0.086(10) 0.043(7) -0.046(7) 0.011(6) -0.013(7) C38 0.051(11) 0.113(16) 0.061(10) -0.015(10) 0.012(9) -0.041(12) C36 0.068(12) 0.090(14) 0.111(14) -0.034(11) -0.030(11) -0.038(12) C37 0.056(12) 0.069(14) 0.125(16) -0.039(12) 0.013(11) -0.024(11) C39 0.063(11) 0.059(11) 0.053(10) -0.001(9) -0.024(9) -0.024(10) C23 0.083(13) 0.130(17) 0.048(10) -0.036(11) -0.034(10) -0.022(13) C44 0.130(16) 0.136(18) 0.036(9) 0.051(11) -0.053(10) -0.083(15) C40 0.132(17) 0.13(2) 0.24(3) 0.049(19) -0.128(18) -0.092(17) C24 0.078(13) 0.119(16) 0.053(10) -0.030(11) -0.009(9) -0.041(13) C32 0.16(2) 0.028(13) 0.140(19) 0.008(12) -0.012(17) -0.037(15) Cl1 0.067(3) 0.104(4) 0.059(3) -0.013(3) -0.018(3) -0.042(3) O9 0.077(8) 0.171(13) 0.141(11) -0.069(10) -0.043(8) -0.012(9) O8 0.116(9) 0.221(13) 0.041(6) -0.006(8) -0.020(7) -0.103(10) C20 0.19(2) 0.50(4) 0.099(15) -0.18(2) 0.102(15) -0.28(3) C3 0.038(10) 0.076(12) 0.072(11) -0.030(10) 0.016(8) -0.029(9) C41 0.22(3) 0.22(3) 0.36(5) 0.22(4) -0.20(4) -0.17(3) C35 0.054(11) 0.088(14) 0.057(10) -0.019(10) -0.024(9) -0.017(11) C42 0.19(3) 0.13(3) 0.27(4) 0.14(3) -0.15(3) -0.08(2) C43 0.16(2) 0.18(3) 0.154(19) 0.13(2) -0.108(17) -0.11(2) C34 0.100(15) 0.042(12) 0.099(13) -0.001(11) -0.042(12) -0.032(13) Cl2 0.110(5) 0.123(5) 0.103(4) -0.043(4) -0.020(4) -0.058(4) O11 0.062(7) 0.164(11) 0.096(7) -0.049(7) -0.033(6) -0.035(7) O10 0.292(17) 0.118(11) 0.160(12) 0.052(9) -0.131(12) -0.138(13) N7 0.051(12) 0.17(2) 0.20(2) -0.068(15) -0.023(13) -0.028(13) C45 0.09(2) 0.14(2) 0.21(3) -0.08(2) -0.03(2) -0.045(19) O15 0.29(2) 0.226(18) 0.169(14) -0.085(14) -0.062(14) -0.111(16) O14 0.209(17) 0.24(2) 0.235(18) 0.113(15) -0.099(14) -0.157(16) C46 0.138(19) 0.16(2) 0.14(2) -0.080(16) 0.005(16) -0.058(17) O13 0.126(13) 0.27(2) 0.45(3) -0.092(19) -0.173(18) 0.056(14) O12 0.35(3) 0.31(3) 0.29(2) -0.24(2) -0.02(2) -0.11(2) O16 0.22(3) 0.45(4) 0.90(9) 0.28(5) 0.17(5) 0.10(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 1.801(6) . ? Fe1 O2 1.979(7) . ? Fe1 O4 2.025(8) . ? Fe1 N2 2.138(12) . ? Fe1 N3 2.144(8) . ? Fe1 N1 2.162(9) . ? Fe2 O1 1.774(6) . ? Fe2 O3 2.037(7) . ? Fe2 O5 2.048(7) . ? Fe2 N5 2.195(9) 2_466 ? Fe2 N6 2.209(11) 2_466 ? Fe2 N4 2.252(10) 2_466 ? O5 C8 1.279(10) . ? O2 C1 1.302(12) . ? O4 C8 1.279(11) . ? O3 C1 1.203(11) . ? O7 C10 1.400(13) . ? O7 C15 1.497(12) . ? N1 C19 1.501(13) . ? N1 C17 1.505(13) . ? N1 C18 1.516(11) . ? C9 C10 1.358(15) . ? C9 C14 1.407(17) . ? C9 C8 1.482(15) . ? N3 C25 1.339(12) . ? N3 C29 1.358(13) . ? C10 C11 1.402(16) . ? O6 C20 1.178(14) . ? O6 C14 1.368(14) . ? N2 C30 1.310(16) . ? N2 C34 1.328(15) . ? C14 C13 1.377(17) . ? C6 C5 1.371(16) . ? C6 C7 1.414(15) . ? C25 C26 1.362(12) . ? C29 C28 1.396(15) . ? C29 C18 1.509(14) . ? C2 C3 1.376(14) . ? C2 C7 1.397(13) . ? C2 C1 1.523(15) . ? C30 C31 1.366(17) . ? C30 C19 1.516(17) . ? C17 C16 1.503(14) . ? C16 C15 1.524(13) . ? C28 C27 1.406(17) . ? C27 C26 1.365(15) . ? C11 C12 1.400(18) . ? C5 C4 1.384(15) . ? C22 C20 1.353(17) . ? C22 C21 1.555(13) . ? C13 C12 1.340(18) . ? C4 C3 1.370(14) . ? C33 C34 1.341(17) . ? C33 C32 1.41(2) . ? C31 C32 1.365(19) . ? C21 N4 1.439(12) . ? N4 C23 1.501(14) . ? N4 C24 1.559(15) . ? N4 Fe2 2.252(10) 2_466 ? N6 C40 1.335(17) . ? N6 C44 1.351(15) . ? N6 Fe2 2.209(11) 2_466 ? N5 C35 1.314(14) . ? N5 C39 1.348(13) . ? N5 Fe2 2.195(9) 2_466 ? C38 C39 1.354(14) . ? C38 C37 1.393(16) . ? C36 C37 1.366(16) . ? C36 C35 1.469(16) . ? C23 C44 1.477(18) . ? C44 C43 1.365(18) . ? C40 C41 1.43(2) . ? C24 C35 1.435(15) . ? Cl1 O8 1.372(8) . ? Cl1 O10 1.393(10) . ? Cl1 O11 1.414(7) . ? Cl1 O9 1.452(10) . ? C41 C42 1.26(4) . ? C42 C43 1.42(3) . ? Cl2 O12 1.228(16) . ? Cl2 O15 1.320(12) . ? Cl2 O13 1.364(12) . ? Cl2 O14 1.365(14) . ? N7 C45 1.23(2) 2_366 ? C45 N7 1.23(2) 2_366 ? C45 C46 1.32(2) . ? 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 102.7(3) . . ? O1 Fe1 O4 93.1(3) . . ? O2 Fe1 O4 92.1(3) . . ? O1 Fe1 N2 92.1(4) . . ? O2 Fe1 N2 90.0(4) . . ? O4 Fe1 N2 173.8(3) . . ? O1 Fe1 N3 167.9(3) . . ? O2 Fe1 N3 88.8(3) . . ? O4 Fe1 N3 82.7(3) . . ? N2 Fe1 N3 91.5(4) . . ? O1 Fe1 N1 92.5(3) . . ? O2 Fe1 N1 159.0(3) . . ? O4 Fe1 N1 101.5(4) . . ? N2 Fe1 N1 74.9(4) . . ? N3 Fe1 N1 77.4(4) . . ? O1 Fe2 O3 99.0(3) . . ? O1 Fe2 O5 97.9(3) . . ? O3 Fe2 O5 89.1(3) . . ? O1 Fe2 N5 96.0(3) . 2_466 ? O3 Fe2 N5 163.8(4) . 2_466 ? O5 Fe2 N5 82.7(3) . 2_466 ? O1 Fe2 N6 97.0(4) . 2_466 ? O3 Fe2 N6 85.5(4) . 2_466 ? O5 Fe2 N6 164.8(4) . 2_466 ? N5 Fe2 N6 98.8(4) 2_466 2_466 ? O1 Fe2 N4 169.0(4) . 2_466 ? O3 Fe2 N4 90.1(4) . 2_466 ? O5 Fe2 N4 88.4(4) . 2_466 ? N5 Fe2 N4 75.7(4) 2_466 2_466 ? N6 Fe2 N4 77.4(5) 2_466 2_466 ? C8 O5 Fe2 124.6(7) . . ? C1 O2 Fe1 124.8(7) . . ? C8 O4 Fe1 133.0(8) . . ? Fe2 O1 Fe1 120.9(4) . . ? C1 O3 Fe2 132.5(8) . . ? C10 O7 C15 115.3(9) . . ? C19 N1 C17 109.7(10) . . ? C19 N1 C18 109.6(9) . . ? C17 N1 C18 109.3(10) . . ? C19 N1 Fe1 103.3(8) . . ? C17 N1 Fe1 112.3(7) . . ? C18 N1 Fe1 112.6(7) . . ? C10 C9 C14 118.2(14) . . ? C10 C9 C8 120.6(15) . . ? C14 C9 C8 121.1(13) . . ? C25 N3 C29 116.3(10) . . ? C25 N3 Fe1 124.9(8) . . ? C29 N3 Fe1 118.6(8) . . ? C9 C10 O7 114.7(15) . . ? C9 C10 C11 121.1(14) . . ? O7 C10 C11 123.9(15) . . ? C20 O6 C14 125.7(13) . . ? C30 N2 C34 115.5(14) . . ? C30 N2 Fe1 116.0(11) . . ? C34 N2 Fe1 126.9(11) . . ? O6 C14 C13 120.8(16) . . ? O6 C14 C9 119.0(14) . . ? C13 C14 C9 120.2(15) . . ? O5 C8 O4 124.5(12) . . ? O5 C8 C9 118.0(10) . . ? O4 C8 C9 117.5(10) . . ? C5 C6 C7 121.6(14) . . ? N3 C25 C26 121.9(11) . . ? N3 C29 C28 127.6(12) . . ? N3 C29 C18 115.5(11) . . ? C28 C29 C18 116.9(12) . . ? C3 C2 C7 119.9(13) . . ? C3 C2 C1 116.9(12) . . ? C7 C2 C1 122.6(12) . . ? N2 C30 C31 126.9(17) . . ? N2 C30 C19 112.1(15) . . ? C31 C30 C19 121.0(19) . . ? C16 C17 N1 114.8(10) . . ? C17 C16 C15 112.3(10) . . ? C29 C28 C27 111.4(13) . . ? O3 C1 O2 127.1(12) . . ? O3 C1 C2 119.6(12) . . ? O2 C1 C2 113.3(10) . . ? N1 C19 C30 111.8(12) . . ? C2 C7 C6 117.6(13) . . ? C26 C27 C28 123.0(13) . . ? O7 C15 C16 106.8(9) . . ? C29 C18 N1 111.7(10) . . ? C12 C11 C10 119.3(14) . . ? C25 C26 C27 119.7(13) . . ? C6 C5 C4 119.0(14) . . ? C20 C22 C21 115.5(12) . . ? C12 C13 C14 121.7(18) . . ? C3 C4 C5 120.4(13) . . ? C13 C12 C11 119.3(17) . . ? C34 C33 C32 114(2) . . ? C32 C31 C30 113.9(18) . . ? N4 C21 C22 118.8(9) . . ? C21 N4 C23 116.2(12) . . ? C21 N4 C24 111.6(12) . . ? C23 N4 C24 106.6(11) . . ? C21 N4 Fe2 111.2(7) . 2_466 ? C23 N4 Fe2 106.4(8) . 2_466 ? C24 N4 Fe2 104.0(7) . 2_466 ? C40 N6 C44 128.6(15) . . ? C40 N6 Fe2 118.5(12) . 2_466 ? C44 N6 Fe2 111.8(11) . 2_466 ? C35 N5 C39 123.6(12) . . ? C35 N5 Fe2 112.3(9) . 2_466 ? C39 N5 Fe2 123.7(9) . 2_466 ? C39 C38 C37 117.3(15) . . ? C37 C36 C35 118.3(14) . . ? C36 C37 C38 121.6(15) . . ? N5 C39 C38 122.1(13) . . ? C44 C23 N4 108.2(11) . . ? N6 C44 C43 116.8(19) . . ? N6 C44 C23 117.8(13) . . ? C43 C44 C23 123.8(18) . . ? N6 C40 C41 112(2) . . ? C35 C24 N4 108.3(13) . . ? C31 C32 C33 123.3(18) . . ? O8 Cl1 O10 111.5(7) . . ? O8 Cl1 O11 110.3(6) . . ? O10 Cl1 O11 110.1(7) . . ? O8 Cl1 O9 107.7(7) . . ? O10 Cl1 O9 109.1(8) . . ? O11 Cl1 O9 108.1(6) . . ? O6 C20 C22 127.0(15) . . ? C4 C3 C2 121.1(13) . . ? C42 C41 C40 123(4) . . ? N5 C35 C24 122.6(14) . . ? N5 C35 C36 116.9(13) . . ? C24 C35 C36 120.1(15) . . ? C41 C42 C43 122(3) . . ? C44 C43 C42 117(2) . . ? N2 C34 C33 126.7(18) . . ? O12 Cl2 O15 110.5(13) . . ? O12 Cl2 O13 108.8(12) . . ? O15 Cl2 O13 108.7(11) . . ? O12 Cl2 O14 107.8(13) . . ? O15 Cl2 O14 111.2(10) . . ? O13 Cl2 O14 109.8(11) . . ? N7 C45 C46 171(3) 2_366 . ? _diffrn_measured_fraction_theta_max 0.872 _diffrn_reflns_theta_full 31.95 _diffrn_measured_fraction_theta_full 0.872 _refine_diff_density_max 0.443 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.084