data_rb62 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H54 Cl2 Fe3 N13 O7' _chemical_formula_weight 887.26 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3260(8) _cell_length_b 25.3961(17) _cell_length_c 13.1400(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.149(1) _cell_angle_gamma 90.00 _cell_volume 4060.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 273 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description prisms _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 1.244 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7948 _exptl_absorpt_correction_T_max 0.8747 _exptl_absorpt_process_details 'based on measured indexed crystal faces, Bruker SHELXTL v6.12 (Bruker 1998)' _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 'SMART CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1' _diffrn_reflns_number 26429 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9205 _reflns_number_gt 8582 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Bruker SMART v5.624 (Bruker 1998)' _computing_cell_refinement 'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)' _computing_data_reduction 'Bruker SHELXTL v6.12 (Bruker 2000)' _computing_structure_solution 'Bruker SHELXTL v6.12' _computing_structure_refinement 'Bruker SHELXTL v6.12' _computing_molecular_graphics 'Bruker SHELXTL v6.12' _computing_publication_material 'Bruker SHELXTL v6.12' _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. The asymmetric unit consists of the cluster and a molecule of dichloromethane. The cluster has a disordered azide ligand at the N11 position. It was refined in two parts with their site occupation factors dependently refined. ; _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^)+(0.0208P)^2^+6.5782P] 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 9205 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.211 _refine_ls_shift/su_max 0.001 _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 0.35631(3) 0.149465(14) 0.38044(3) 0.01954(9) Uani 1 1 d . . . Fe2 Fe 0.25299(3) 0.062815(14) 0.48670(3) 0.01884(9) Uani 1 1 d . A . Fe3 Fe 0.14792(3) 0.160005(15) 0.55279(3) 0.02034(9) Uani 1 1 d . . . O1 O 0.25201(15) 0.14382(7) 0.46899(14) 0.0223(4) Uani 1 1 d . . . O2 O 0.11121(15) 0.08282(7) 0.52916(14) 0.0214(4) Uani 1 1 d . . . O3 O 0.39375(15) 0.07619(7) 0.43687(14) 0.0213(4) Uani 1 1 d . . . O4 O 0.32421(16) 0.06689(8) 0.63823(14) 0.0256(4) Uani 1 1 d . . . O5 O 0.24488(17) 0.13947(8) 0.69008(15) 0.0262(4) Uani 1 1 d . . . O6 O 0.17785(16) 0.05351(7) 0.33612(14) 0.0230(4) Uani 1 1 d . . . O7 O 0.26117(16) 0.11544(8) 0.25440(15) 0.0247(4) Uani 1 1 d . . . N1 N 0.0039(2) 0.14794(9) 0.63502(19) 0.0256(5) Uani 1 1 d . . . N2 N 0.0164(2) 0.18876(10) 0.43130(19) 0.0282(5) Uani 1 1 d . . . N3 N 0.5030(2) 0.12707(9) 0.30842(18) 0.0256(5) Uani 1 1 d . . . N4 N 0.4864(2) 0.19024(9) 0.48820(19) 0.0259(5) Uani 1 1 d . . . N5 N 0.1723(2) 0.23604(10) 0.5957(2) 0.0314(6) Uani 1 1 d . . . N6 N 0.2162(2) 0.25161(10) 0.6783(2) 0.0313(6) Uani 1 1 d . . . N7 N 0.2560(3) 0.26854(13) 0.7559(3) 0.0540(9) Uani 1 1 d . . . N8 N 0.3301(2) 0.21859(10) 0.3066(2) 0.0303(5) Uani 1 1 d . . . N9 N 0.2865(2) 0.22710(10) 0.2204(2) 0.0345(6) Uani 1 1 d . . . N10 N 0.2469(3) 0.23721(15) 0.1374(3) 0.0617(10) Uani 1 1 d . . . N11 N 0.2529(2) -0.01600(9) 0.4981(2) 0.0291(5) Uani 1 1 d . . . N12 N 0.2293(16) -0.0353(8) 0.5877(15) 0.029(4) Uiso 0.131(4) 1 d P A 2 N13 N 0.2142(18) -0.0563(9) 0.6620(17) 0.038(5) Uiso 0.131(4) 1 d P A 2 N12' N 0.2623(2) -0.04346(11) 0.4234(2) 0.0283(7) Uani 0.869(4) 1 d P A 1 N13' N 0.2707(3) -0.07096(13) 0.3554(3) 0.0432(9) Uani 0.869(4) 1 d P A 1 C1 C 0.0393(2) 0.05641(11) 0.5861(2) 0.0291(6) Uani 1 1 d . . . H1C H 0.0747 0.0239 0.6167 0.035 Uiso 1 1 calc R . . H1D H -0.0290 0.0464 0.5398 0.035 Uiso 1 1 calc R . . C2 C 0.0118(3) 0.09257(11) 0.6713(2) 0.0291(6) Uani 1 1 d . . . H2A H -0.0589 0.0817 0.6915 0.035 Uiso 1 1 calc R . . H2B H 0.0696 0.0896 0.7326 0.035 Uiso 1 1 calc R . . C3 C -0.0966(2) 0.15716(12) 0.5576(2) 0.0320(7) Uani 1 1 d . . . H3A H -0.1589 0.1663 0.5935 0.038 Uiso 1 1 calc R . . H3B H -0.1159 0.1246 0.5174 0.038 Uiso 1 1 calc R . . C4 C -0.0775(2) 0.20133(12) 0.4855(2) 0.0308(6) Uani 1 1 d . . . H4A H -0.1447 0.2068 0.4342 0.037 Uiso 1 1 calc R . . H4B H -0.0620 0.2343 0.5252 0.037 Uiso 1 1 calc R . . C5 C 0.0039(3) 0.18334(13) 0.7246(3) 0.0356(7) Uani 1 1 d . . . H5A H -0.0552 0.1730 0.7623 0.053 Uiso 1 1 calc R . . H5B H -0.0079 0.2197 0.7005 0.053 Uiso 1 1 calc R . . H5C H 0.0747 0.1807 0.7704 0.053 Uiso 1 1 calc R . . C6 C 0.0486(3) 0.23669(14) 0.3791(3) 0.0391(8) Uani 1 1 d . . . H6A H -0.0106 0.2465 0.3234 0.059 Uiso 1 1 calc R . . H6B H 0.1158 0.2296 0.3504 0.059 Uiso 1 1 calc R . . H6C H 0.0618 0.2656 0.4290 0.059 Uiso 1 1 calc R . . C7 C -0.0148(3) 0.14794(14) 0.3509(3) 0.0402(8) Uani 1 1 d . . . H7A H -0.0809 0.1593 0.3044 0.060 Uiso 1 1 calc R . . H7B H -0.0298 0.1147 0.3838 0.060 Uiso 1 1 calc R . . H7C H 0.0455 0.1430 0.3115 0.060 Uiso 1 1 calc R . . C8 C 0.4679(2) 0.04349(11) 0.3936(2) 0.0293(6) Uani 1 1 d . . . H8A H 0.4338 0.0086 0.3766 0.035 Uiso 1 1 calc R . . H8B H 0.5355 0.0382 0.4442 0.035 Uiso 1 1 calc R . . C9 C 0.4969(3) 0.06893(11) 0.2962(2) 0.0297(6) Uani 1 1 d . . . H9A H 0.5685 0.0553 0.2828 0.036 Uiso 1 1 calc R . . H9B H 0.4404 0.0598 0.2365 0.036 Uiso 1 1 calc R . . C10 C 0.6025(2) 0.14304(12) 0.3814(2) 0.0303(6) Uani 1 1 d . . . H10A H 0.6655 0.1468 0.3437 0.036 Uiso 1 1 calc R . . H10B H 0.6210 0.1155 0.4346 0.036 Uiso 1 1 calc R . . C11 C 0.5818(2) 0.19489(12) 0.4324(2) 0.0307(6) Uani 1 1 d . . . H11A H 0.6480 0.2050 0.4815 0.037 Uiso 1 1 calc R . . H11B H 0.5673 0.2228 0.3794 0.037 Uiso 1 1 calc R . . C12 C 0.5030(3) 0.15155(13) 0.2061(2) 0.0347(7) Uani 1 1 d . . . H12A H 0.5134 0.1897 0.2143 0.052 Uiso 1 1 calc R . . H12B H 0.4327 0.1445 0.1619 0.052 Uiso 1 1 calc R . . H12C H 0.5630 0.1367 0.1744 0.052 Uiso 1 1 calc R . . C13 C 0.5163(3) 0.16010(13) 0.5853(2) 0.0348(7) Uani 1 1 d . . . H13A H 0.5377 0.1242 0.5693 0.052 Uiso 1 1 calc R . . H13B H 0.4531 0.1587 0.6220 0.052 Uiso 1 1 calc R . . H13C H 0.5780 0.1775 0.6288 0.052 Uiso 1 1 calc R . . C14 C 0.4533(3) 0.24392(12) 0.5162(3) 0.0367(7) Uani 1 1 d . . . H14A H 0.3877 0.2416 0.5494 0.055 Uiso 1 1 calc R . . H14B H 0.4370 0.2655 0.4538 0.055 Uiso 1 1 calc R . . H14C H 0.5133 0.2601 0.5638 0.055 Uiso 1 1 calc R . . C15 C 0.3065(2) 0.09940(11) 0.7065(2) 0.0249(6) Uani 1 1 d . . . C16 C 0.3625(3) 0.08863(13) 0.8171(2) 0.0332(7) Uani 1 1 d . . . C17 C 0.4849(3) 0.0806(2) 0.8177(3) 0.0754(16) Uani 1 1 d . . . H17A H 0.5175 0.1135 0.7977 0.113 Uiso 1 1 calc R . . H17B H 0.4959 0.0527 0.7688 0.113 Uiso 1 1 calc R . . H17C H 0.5202 0.0705 0.8871 0.113 Uiso 1 1 calc R . . C18 C 0.3416(5) 0.13308(17) 0.8890(3) 0.0657(14) Uani 1 1 d . . . H18A H 0.3781 0.1251 0.9591 0.099 Uiso 1 1 calc R . . H18B H 0.2624 0.1367 0.8885 0.099 Uiso 1 1 calc R . . H18C H 0.3710 0.1660 0.8657 0.099 Uiso 1 1 calc R . . C19 C 0.3140(4) 0.03704(16) 0.8509(3) 0.0548(11) Uani 1 1 d . . . H19A H 0.3501 0.0279 0.9206 0.082 Uiso 1 1 calc R . . H19B H 0.3260 0.0088 0.8031 0.082 Uiso 1 1 calc R . . H19C H 0.2350 0.0415 0.8507 0.082 Uiso 1 1 calc R . . C20 C 0.1947(2) 0.07731(11) 0.2561(2) 0.0231(5) Uani 1 1 d . . . C21 C 0.1324(3) 0.05867(13) 0.1517(2) 0.0326(7) Uani 1 1 d . . . C22 C 0.2126(4) 0.0230(2) 0.1067(3) 0.0709(14) Uani 1 1 d . . . H22A H 0.1767 0.0088 0.0404 0.106 Uiso 1 1 calc R . . H22B H 0.2349 -0.0062 0.1544 0.106 Uiso 1 1 calc R . . H22C H 0.2775 0.0433 0.0965 0.106 Uiso 1 1 calc R . . C23 C 0.0306(4) 0.0279(2) 0.1662(3) 0.0626(13) Uani 1 1 d . . . H23A H -0.0158 0.0495 0.2035 0.094 Uiso 1 1 calc R . . H23B H 0.0524 -0.0042 0.2058 0.094 Uiso 1 1 calc R . . H23C H -0.0104 0.0183 0.0987 0.094 Uiso 1 1 calc R . . C24 C 0.1015(4) 0.10520(17) 0.0806(3) 0.0597(12) Uani 1 1 d . . . H24A H 0.0622 0.0926 0.0143 0.090 Uiso 1 1 calc R . . H24B H 0.1682 0.1238 0.0695 0.090 Uiso 1 1 calc R . . H24C H 0.0540 0.1292 0.1120 0.090 Uiso 1 1 calc R . . Cl1 Cl 0.74321(15) 0.09462(7) 0.07904(14) 0.1025(5) Uani 1 1 d . . . Cl2 Cl 0.76958(14) 0.13337(6) -0.12492(14) 0.0985(5) Uani 1 1 d . . . C25 C 0.7744(6) 0.1458(2) 0.0115(6) 0.121(3) Uani 1 1 d . . . H25A H 0.8492 0.1579 0.0406 0.145 Uiso 1 1 calc R . . H25B H 0.7228 0.1748 0.0198 0.145 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 0.01863(18) 0.01847(18) 0.02183(19) 0.00200(14) 0.00420(14) 0.00012(14) Fe2 0.01988(18) 0.01755(17) 0.01939(18) 0.00071(14) 0.00403(14) 0.00110(14) Fe3 0.02016(19) 0.01883(18) 0.02244(19) -0.00163(15) 0.00466(14) 0.00110(14) O1 0.0219(9) 0.0201(9) 0.0253(10) 0.0009(7) 0.0048(7) 0.0007(7) O2 0.0201(9) 0.0202(9) 0.0244(9) -0.0018(7) 0.0049(7) -0.0008(7) O3 0.0188(9) 0.0204(9) 0.0253(9) 0.0026(7) 0.0058(7) 0.0031(7) O4 0.0278(10) 0.0264(10) 0.0223(10) 0.0014(8) 0.0032(8) 0.0049(8) O5 0.0299(11) 0.0258(10) 0.0225(10) -0.0032(8) 0.0026(8) -0.0005(8) O6 0.0249(10) 0.0230(9) 0.0211(9) -0.0005(7) 0.0034(7) -0.0010(8) O7 0.0260(10) 0.0257(10) 0.0218(9) 0.0008(8) 0.0017(8) -0.0031(8) N1 0.0256(12) 0.0231(11) 0.0298(12) -0.0026(10) 0.0096(10) 0.0017(9) N2 0.0250(12) 0.0312(13) 0.0284(12) -0.0011(10) 0.0039(10) 0.0082(10) N3 0.0243(12) 0.0258(12) 0.0284(12) 0.0027(10) 0.0090(10) 0.0005(10) N4 0.0244(12) 0.0241(12) 0.0294(12) -0.0003(10) 0.0052(10) -0.0030(9) N5 0.0398(15) 0.0234(12) 0.0310(13) -0.0053(10) 0.0055(11) -0.0003(11) N6 0.0268(13) 0.0255(12) 0.0419(15) -0.0078(11) 0.0067(11) -0.0001(10) N7 0.0504(19) 0.0523(19) 0.053(2) -0.0237(16) -0.0106(15) -0.0002(15) N8 0.0343(14) 0.0234(12) 0.0325(14) 0.0074(10) 0.0032(11) -0.0004(10) N9 0.0286(13) 0.0282(13) 0.0464(16) 0.0142(12) 0.0047(12) -0.0023(11) N10 0.060(2) 0.063(2) 0.054(2) 0.0328(18) -0.0161(17) -0.0085(18) N11 0.0306(13) 0.0226(12) 0.0334(13) 0.0044(10) 0.0030(10) 0.0012(10) N12' 0.0205(14) 0.0208(13) 0.0432(17) 0.0012(13) 0.0040(12) -0.0035(11) N13' 0.045(2) 0.0277(16) 0.057(2) -0.0121(15) 0.0101(16) -0.0015(14) C1 0.0285(15) 0.0228(13) 0.0392(16) -0.0030(12) 0.0148(12) -0.0029(11) C2 0.0316(15) 0.0257(14) 0.0327(15) 0.0023(12) 0.0139(12) 0.0012(12) C3 0.0208(14) 0.0356(16) 0.0401(17) -0.0018(13) 0.0059(12) 0.0022(12) C4 0.0236(14) 0.0323(15) 0.0365(16) -0.0006(13) 0.0049(12) 0.0082(12) C5 0.0384(18) 0.0351(16) 0.0374(17) -0.0078(14) 0.0188(14) 0.0036(14) C6 0.0355(18) 0.0435(19) 0.0384(18) 0.0123(15) 0.0065(14) 0.0094(15) C7 0.0408(19) 0.0450(19) 0.0311(16) -0.0079(14) -0.0057(14) 0.0127(15) C8 0.0276(15) 0.0224(13) 0.0405(17) 0.0030(12) 0.0132(13) 0.0069(11) C9 0.0288(15) 0.0258(14) 0.0379(16) -0.0027(12) 0.0152(12) 0.0011(12) C10 0.0204(14) 0.0331(15) 0.0387(16) 0.0008(13) 0.0084(12) -0.0007(12) C11 0.0237(14) 0.0348(16) 0.0341(16) 0.0010(13) 0.0060(12) -0.0045(12) C12 0.0362(17) 0.0377(17) 0.0331(16) 0.0063(13) 0.0145(13) -0.0006(14) C13 0.0350(17) 0.0393(17) 0.0283(15) 0.0028(13) 0.0000(13) -0.0063(14) C14 0.0355(17) 0.0276(15) 0.0469(19) -0.0091(14) 0.0064(14) -0.0034(13) C15 0.0249(14) 0.0271(14) 0.0228(13) 0.0035(11) 0.0040(11) -0.0027(11) C16 0.0408(18) 0.0367(16) 0.0209(14) 0.0025(12) 0.0011(12) 0.0028(14) C17 0.041(2) 0.140(5) 0.040(2) 0.018(3) -0.0108(18) 0.006(3) C18 0.113(4) 0.050(2) 0.0280(19) -0.0069(17) -0.007(2) 0.006(2) C19 0.082(3) 0.048(2) 0.0353(19) 0.0144(17) 0.0114(19) 0.001(2) C20 0.0217(13) 0.0233(13) 0.0238(13) 0.0001(10) 0.0022(10) 0.0041(10) C21 0.0371(17) 0.0372(16) 0.0221(14) -0.0019(12) 0.0005(12) -0.0085(14) C22 0.076(3) 0.087(3) 0.047(2) -0.040(2) 0.000(2) 0.013(3) C23 0.062(3) 0.087(3) 0.0340(19) -0.005(2) -0.0070(18) -0.043(2) C24 0.081(3) 0.054(2) 0.035(2) 0.0110(17) -0.020(2) -0.014(2) Cl1 0.1095(13) 0.0940(11) 0.1150(13) -0.0002(10) 0.0511(10) 0.0211(10) Cl2 0.1028(12) 0.0864(10) 0.1195(13) -0.0157(9) 0.0580(10) -0.0325(9) C25 0.128(6) 0.060(3) 0.190(8) -0.068(4) 0.072(6) -0.031(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 1.8716(19) . ? Fe1 N8 2.007(2) . ? Fe1 O3 2.0291(18) . ? Fe1 O7 2.0608(19) . ? Fe1 N4 2.220(2) . ? Fe1 N3 2.243(2) . ? Fe2 O3 1.9787(19) . ? Fe2 O2 1.9834(19) . ? Fe2 N11 2.007(2) . ? Fe2 O4 2.0469(19) . ? Fe2 O6 2.0605(19) . ? Fe2 O1 2.0700(19) . ? Fe3 O1 1.8647(19) . ? Fe3 N5 2.020(2) . ? Fe3 O2 2.0245(19) . ? Fe3 O5 2.066(2) . ? Fe3 N2 2.211(2) . ? Fe3 N1 2.241(2) . ? O2 C1 1.416(3) . ? O3 C8 1.419(3) . ? O4 C15 1.264(3) . ? O5 C15 1.267(3) . ? O6 C20 1.259(3) . ? O7 C20 1.271(3) . ? N1 C5 1.482(4) . ? N1 C2 1.483(4) . ? N1 C3 1.492(4) . ? N2 C6 1.482(4) . ? N2 C7 1.486(4) . ? N2 C4 1.487(4) . ? N3 C12 1.482(4) . ? N3 C9 1.486(4) . ? N3 C10 1.488(4) . ? N4 C13 1.483(4) . ? N4 C14 1.486(4) . ? N4 C11 1.486(4) . ? N5 N6 1.200(4) . ? N6 N7 1.144(4) . ? N8 N9 1.194(4) . ? N9 N10 1.151(4) . ? N11 N12' 1.224(4) . ? N11 N12 1.350(19) . ? N12 N13 1.15(3) . ? N12' N13' 1.151(4) . ? C1 C2 1.527(4) . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.511(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.525(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.518(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.531(4) . ? C16 C18 1.520(5) . ? C16 C17 1.521(5) . ? C16 C19 1.535(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.536(4) . ? C21 C23 1.515(5) . ? C21 C24 1.517(5) . ? C21 C22 1.528(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Cl1 C25 1.654(7) . ? Cl2 C25 1.812(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? 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 N8 107.10(10) . . ? O1 Fe1 O3 80.87(8) . . ? N8 Fe1 O3 171.37(10) . . ? O1 Fe1 O7 96.21(8) . . ? N8 Fe1 O7 87.19(9) . . ? O3 Fe1 O7 88.65(8) . . ? O1 Fe1 N4 97.88(9) . . ? N8 Fe1 N4 86.83(10) . . ? O3 Fe1 N4 95.48(8) . . ? O7 Fe1 N4 165.78(9) . . ? O1 Fe1 N3 157.25(8) . . ? N8 Fe1 N3 95.53(10) . . ? O3 Fe1 N3 76.70(8) . . ? O7 Fe1 N3 87.04(9) . . ? N4 Fe1 N3 80.71(9) . . ? O3 Fe2 O2 155.14(8) . . ? O3 Fe2 N11 101.92(9) . . ? O2 Fe2 N11 102.93(9) . . ? O3 Fe2 O4 92.88(8) . . ? O2 Fe2 O4 88.52(8) . . ? N11 Fe2 O4 89.04(9) . . ? O3 Fe2 O6 89.19(8) . . ? O2 Fe2 O6 91.02(8) . . ? N11 Fe2 O6 87.22(9) . . ? O4 Fe2 O6 176.04(8) . . ? O3 Fe2 O1 77.41(7) . . ? O2 Fe2 O1 77.73(7) . . ? N11 Fe2 O1 177.83(9) . . ? O4 Fe2 O1 93.04(8) . . ? O6 Fe2 O1 90.70(7) . . ? O1 Fe3 N5 106.84(10) . . ? O1 Fe3 O2 81.60(8) . . ? N5 Fe3 O2 171.02(9) . . ? O1 Fe3 O5 95.92(8) . . ? N5 Fe3 O5 87.59(9) . . ? O2 Fe3 O5 88.49(8) . . ? O1 Fe3 N2 98.10(9) . . ? N5 Fe3 N2 86.86(10) . . ? O2 Fe3 N2 95.09(9) . . ? O5 Fe3 N2 165.89(9) . . ? O1 Fe3 N1 157.93(8) . . ? N5 Fe3 N1 95.17(10) . . ? O2 Fe3 N1 76.51(8) . . ? O5 Fe3 N1 86.38(9) . . ? N2 Fe3 N1 81.21(9) . . ? Fe3 O1 Fe1 162.82(11) . . ? Fe3 O1 Fe2 98.34(8) . . ? Fe1 O1 Fe2 98.85(8) . . ? C1 O2 Fe2 132.90(17) . . ? C1 O2 Fe3 121.39(16) . . ? Fe2 O2 Fe3 96.07(8) . . ? C8 O3 Fe2 133.37(17) . . ? C8 O3 Fe1 120.90(16) . . ? Fe2 O3 Fe1 96.77(8) . . ? C15 O4 Fe2 128.89(18) . . ? C15 O5 Fe3 126.80(18) . . ? C20 O6 Fe2 129.67(18) . . ? C20 O7 Fe1 126.26(18) . . ? C5 N1 C2 109.1(2) . . ? C5 N1 C3 110.0(2) . . ? C2 N1 C3 111.9(2) . . ? C5 N1 Fe3 113.63(18) . . ? C2 N1 Fe3 105.58(17) . . ? C3 N1 Fe3 106.60(18) . . ? C6 N2 C7 107.6(3) . . ? C6 N2 C4 109.4(2) . . ? C7 N2 C4 110.9(3) . . ? C6 N2 Fe3 112.70(19) . . ? C7 N2 Fe3 111.10(18) . . ? C4 N2 Fe3 105.22(17) . . ? C12 N3 C9 109.1(2) . . ? C12 N3 C10 110.5(2) . . ? C9 N3 C10 111.2(2) . . ? C12 N3 Fe1 113.16(18) . . ? C9 N3 Fe1 105.51(17) . . ? C10 N3 Fe1 107.24(17) . . ? C13 N4 C14 107.5(2) . . ? C13 N4 C11 110.9(2) . . ? C14 N4 C11 108.6(2) . . ? C13 N4 Fe1 111.32(18) . . ? C14 N4 Fe1 112.76(19) . . ? C11 N4 Fe1 105.70(17) . . ? N6 N5 Fe3 126.4(2) . . ? N7 N6 N5 177.1(3) . . ? N9 N8 Fe1 129.1(2) . . ? N10 N9 N8 177.2(3) . . ? N12' N11 N12 123.6(8) . . ? N12' N11 Fe2 120.5(2) . . ? N12 N11 Fe2 115.5(8) . . ? N13 N12 N11 173(2) . . ? N13' N12' N11 177.4(3) . . ? O2 C1 C2 109.5(2) . . ? O2 C1 H1C 109.8 . . ? C2 C1 H1C 109.8 . . ? O2 C1 H1D 109.8 . . ? C2 C1 H1D 109.8 . . ? H1C C1 H1D 108.2 . . ? N1 C2 C1 110.2(2) . . ? N1 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? N1 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? N1 C3 C4 110.4(2) . . ? N1 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? N2 C4 C3 110.6(2) . . ? N2 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 109.9(2) . . ? O3 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? O3 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? N3 C9 C8 110.2(2) . . ? N3 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? N3 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? N3 C10 C11 110.0(2) . . ? N3 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? N3 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N4 C11 C10 110.5(2) . . ? N4 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N3 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O4 C15 O5 124.8(3) . . ? O4 C15 C16 117.0(3) . . ? O5 C15 C16 118.2(3) . . ? C18 C16 C17 111.2(4) . . ? C18 C16 C15 111.2(3) . . ? C17 C16 C15 109.0(3) . . ? C18 C16 C19 110.0(3) . . ? C17 C16 C19 108.4(3) . . ? C15 C16 C19 106.8(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O6 C20 O7 125.0(3) . . ? O6 C20 C21 118.2(2) . . ? O7 C20 C21 116.8(2) . . ? C23 C21 C24 110.3(3) . . ? C23 C21 C22 109.9(4) . . ? C24 C21 C22 109.8(3) . . ? C23 C21 C20 110.7(3) . . ? C24 C21 C20 110.5(3) . . ? C22 C21 C20 105.4(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Cl1 C25 Cl2 114.8(3) . . ? Cl1 C25 H25A 108.6 . . ? Cl2 C25 H25A 108.6 . . ? Cl1 C25 H25B 108.6 . . ? Cl2 C25 H25B 108.6 . . ? H25A C25 H25B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.947 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.070