data_sd:fetetsbcl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H30 Cl9 Fe N4 Sb' _chemical_formula_weight 931.22 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' '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' 'Sb' 'Sb' -0.5866 1.5461 '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 9.768(2) _cell_length_b 13.585(3) _cell_length_c 14.508(3) _cell_angle_alpha 76.90(3) _cell_angle_beta 87.32(3) _cell_angle_gamma 71.77(3) _cell_volume 1780.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min -20.5 _cell_measurement_theta_max 20.5 _exptl_crystal_description Rhombohedron _exptl_crystal_colour 'Dark-purple' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method ? _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 1.870 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'Enraf-nonius Fast Area-Detector' _diffrn_measurement_method 'Ellipsoid-mask Fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'No measurable crystal decay' _diffrn_reflns_number 17182 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.7 _reflns_number_total 9071 _reflns_number_gt 7801 _reflns_threshold_expression >2sigma(I) _computing_data_collection Madnes _computing_cell_refinement Madnes _computing_data_reduction 'madnes (Messerschmitt &Pflugraph,1987)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep III (burnett, Johnson, 1996)' _computing_publication_material 'Shelxl-97' _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^)+(0.0576P)^2^+5.4668P] 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 SHELXL _refine_ls_extinction_coef 0.0008(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9071 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Fe(1 Fe -0.23871(5) 0.02041(4) 0.09616(3) 0.01300(11) Uani 1 1 d . . . Cl(1 Cl -0.47021(9) 0.08480(8) 0.07469(7) 0.02720(19) Uani 1 1 d . . . N(1) N -0.1937(3) 0.1134(2) 0.17896(19) 0.0165(5) Uani 1 1 d . . . N(2) N -0.1675(3) 0.1119(2) -0.01806(18) 0.0142(5) Uani 1 1 d . . . N(3) N -0.1858(3) -0.0986(2) 0.02224(18) 0.0137(5) Uani 1 1 d . . . N(4) N -0.2095(3) -0.0978(2) 0.21820(19) 0.0189(5) Uani 1 1 d . . . C(A1 C -0.2106(4) 0.1005(3) 0.2756(2) 0.0212(7) Uani 1 1 d . A . C(A2 C -0.1818(4) 0.2133(3) 0.1472(2) 0.0203(6) Uani 1 1 d . . . C(A3 C -0.1617(3) 0.2135(3) -0.0234(2) 0.0176(6) Uani 1 1 d . . . C(A4 C -0.1603(3) 0.0991(3) -0.1092(2) 0.0152(6) Uani 1 1 d . . . C(A5 C -0.1732(3) -0.0850(3) -0.0749(2) 0.0153(6) Uani 1 1 d . . . C(A6 C -0.1995(3) -0.1986(3) 0.0534(2) 0.0179(6) Uani 1 1 d . . . C(A7 C -0.2118(4) -0.2005(3) 0.2249(3) 0.0234(7) Uani 1 1 d . . . C(A8 C -0.2147(4) -0.0852(3) 0.3098(2) 0.0241(7) Uani 1 1 d . A . C(B1 C -0.2076(5) 0.1943(3) 0.3036(3) 0.0297(8) Uani 1 1 d . . . H(B1 H -0.2168 0.2057 0.3661 0.036 Uiso 1 1 calc R . . C(B2 C -0.1893(5) 0.2631(3) 0.2253(3) 0.0297(8) Uani 1 1 d . . . H(B2 H -0.1825 0.3320 0.2221 0.036 Uiso 1 1 calc R . . C(B3 C -0.1503(4) 0.2642(3) -0.1213(3) 0.0237(7) Uani 1 1 d . . . H(B3 H -0.1445 0.3340 -0.1443 0.028 Uiso 1 1 calc R . . C(B4 C -0.1496(4) 0.1942(3) -0.1733(2) 0.0217(7) Uani 1 1 d . . . H(B4 H -0.1431 0.2052 -0.2401 0.026 Uiso 1 1 calc R . . C(B5 C -0.1762(4) -0.1790(3) -0.1032(2) 0.0195(6) Uani 1 1 d . . . H(B5 H -0.1673 -0.1904 -0.1657 0.023 Uiso 1 1 calc R . . C(B6 C -0.1940(4) -0.2481(3) -0.0243(3) 0.0216(7) Uani 1 1 d . . . H(B6 H -0.2015 -0.3169 -0.0209 0.026 Uiso 1 1 calc R . . C(B7 C -0.2143(6) -0.2525(4) 0.3222(3) 0.0377(10) Uani 1 1 d . . . H(B7 H -0.2146 -0.3236 0.3456 0.045 Uiso 1 1 calc R . . C(B8 C -0.2163(5) -0.1817(4) 0.3744(3) 0.0359(9) Uani 1 1 d . . . H(B8 H -0.2183 -0.1936 0.4415 0.043 Uiso 1 1 calc R . . C(M1 C -0.2226(4) 0.0092(3) 0.3375(2) 0.0239(7) Uani 1 1 d . . . C(M2 C -0.1665(4) 0.2615(3) 0.0526(2) 0.0190(6) Uani 1 1 d . . . C(M3 C -0.1630(3) 0.0068(3) -0.1376(2) 0.0164(6) Uani 1 1 d . . . C(M4 C -0.2143(4) -0.2468(3) 0.1485(3) 0.0223(7) Uani 1 1 d . . . C11A C -0.2665(15) 0.0083(17) 0.4393(14) 0.029(2) Uani 0.50 1 d P A 1 H11A H -0.2516 0.0703 0.4573 0.034 Uiso 0.50 1 calc PR A 1 H11B H -0.2030 -0.0567 0.4809 0.034 Uiso 0.50 1 calc PR A 1 C12A C -0.4260(9) 0.0118(7) 0.4565(6) 0.0305(16) Uani 0.50 1 d P A 1 H12A H -0.4887 0.0693 0.4088 0.046 Uiso 0.50 1 calc PR A 1 H12B H -0.4528 0.0243 0.5198 0.046 Uiso 0.50 1 calc PR A 1 H12C H -0.4371 -0.0562 0.4519 0.046 Uiso 0.50 1 calc PR A 1 C11B C -0.2221(14) 0.0139(17) 0.4413(14) 0.029(2) Uani 0.50 1 d P A 2 H11C H -0.2707 -0.0359 0.4780 0.034 Uiso 0.50 1 calc PR A 2 H11D H -0.2785 0.0865 0.4476 0.034 Uiso 0.50 1 calc PR A 2 C12B C -0.0707(9) -0.0140(7) 0.4837(5) 0.0321(17) Uani 0.50 1 d P A 2 H12D H -0.0126 -0.0843 0.4748 0.048 Uiso 0.50 1 calc PR A 2 H12E H -0.0771 -0.0149 0.5515 0.048 Uiso 0.50 1 calc PR A 2 H12F H -0.0255 0.0392 0.4520 0.048 Uiso 0.50 1 calc PR A 2 C(21 C -0.1659(4) 0.3754(3) 0.0310(3) 0.0248(7) Uani 1 1 d . . . H(2A H -0.1088 0.3886 -0.0261 0.030 Uiso 1 1 calc R . . H(2B H -0.1197 0.3881 0.0846 0.030 Uiso 1 1 calc R . . C(22 C -0.3193(5) 0.4519(3) 0.0144(4) 0.0372(10) Uani 1 1 d . . . H(2C H -0.3683 0.4345 -0.0342 0.056 Uiso 1 1 calc R . . H(2D H -0.3161 0.5250 -0.0068 0.056 Uiso 1 1 calc R . . H(2E H -0.3719 0.4454 0.0735 0.056 Uiso 1 1 calc R . . C(31 C -0.1633(4) 0.0099(3) -0.2424(2) 0.0224(7) Uani 1 1 d . . . H(3A H -0.1141 -0.0623 -0.2529 0.027 Uiso 1 1 calc R . . H(3B H -0.1094 0.0577 -0.2757 0.027 Uiso 1 1 calc R . . C(32 C -0.3170(5) 0.0491(4) -0.2832(3) 0.0358(9) Uani 1 1 d . . . H(3C H -0.3698 0.0008 -0.2513 0.054 Uiso 1 1 calc R . . H(3D H -0.3146 0.0509 -0.3512 0.054 Uiso 1 1 calc R . . H(3E H -0.3655 0.1207 -0.2733 0.054 Uiso 1 1 calc R . . C(41 C -0.2435(5) -0.3529(3) 0.1684(3) 0.0325(9) Uani 1 1 d . . . H(4A H -0.2024 -0.3951 0.2315 0.039 Uiso 1 1 calc R . . H(4B H -0.1961 -0.3931 0.1205 0.039 Uiso 1 1 calc R . . C(42 C -0.4053(6) -0.3360(4) 0.1656(5) 0.0528(14) Uani 1 1 d . . . H(4C H -0.4504 -0.3035 0.2178 0.079 Uiso 1 1 calc R . . H(4D H -0.4222 -0.4046 0.1721 0.079 Uiso 1 1 calc R . . H(4E H -0.4472 -0.2889 0.1052 0.079 Uiso 1 1 calc R . . Sb(1 Sb -0.26385(3) 0.636640(19) -0.313255(17) 0.02313(9) Uani 1 1 d . . . Cl2A Cl -0.0985(5) 0.5718(9) -0.4274(6) 0.0389(19) Uani 0.34(2) 1 d P . . Cl2B Cl -0.0935(4) 0.5255(9) -0.3948(7) 0.065(2) Uani 0.66(2) 1 d P . . Cl(3 Cl -0.42624(17) 0.71309(12) -0.44384(8) 0.0546(4) Uani 1 1 d . . . Cl(4 Cl -0.16025(16) 0.77650(11) -0.35534(7) 0.0492(3) Uani 1 1 d . . . Cl(5 Cl -0.42506(12) 0.73222(13) -0.21739(9) 0.0513(3) Uani 1 1 d . . . Cl(6 Cl -0.09793(12) 0.55930(8) -0.18202(9) 0.0405(3) Uani 1 1 d . . . Cl(7 Cl -0.36235(18) 0.49597(11) -0.27085(13) 0.0702(5) Uani 1 1 d . . . C(5A C 0.8221(14) 0.3643(9) 0.5024(8) 0.050(3) Uani 0.482(14) 1 d P B 1 H(5A H 0.9231 0.3389 0.4826 0.059 Uiso 0.482(14) 1 calc PR B 1 H(5B H 0.8197 0.4083 0.5486 0.059 Uiso 0.482(14) 1 calc PR B 1 C(5B C 0.6721(14) 0.4096(9) 0.5058(8) 0.052(3) Uani 0.518(14) 1 d P B 2 H(5C H 0.5674 0.4196 0.5104 0.062 Uiso 0.518(14) 1 calc PR B 2 H(5D H 0.6964 0.4532 0.5448 0.062 Uiso 0.518(14) 1 calc PR B 2 Cl(8 Cl 0.7095(2) 0.44892(15) 0.39777(13) 0.0718(5) Uani 1 1 d . . . Cl(9 Cl 0.7751(3) 0.2652(2) 0.55309(12) 0.1013(8) 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 Fe(1 0.0121(2) 0.0168(2) 0.0111(2) -0.00349(15) 0.00063(15) -0.00568(16) Cl(1 0.0126(3) 0.0370(5) 0.0339(5) -0.0157(4) 0.0005(3) -0.0048(3) N(1) 0.0156(12) 0.0223(13) 0.0132(12) -0.0069(10) -0.0002(9) -0.0062(10) N(2) 0.0134(11) 0.0165(12) 0.0143(12) -0.0028(9) 0.0007(9) -0.0071(9) N(3) 0.0128(11) 0.0152(12) 0.0151(12) -0.0047(9) 0.0023(9) -0.0067(9) N(4) 0.0191(13) 0.0228(14) 0.0136(12) -0.0012(10) 0.0005(10) -0.0070(11) C(A1 0.0196(15) 0.0302(18) 0.0143(14) -0.0078(13) -0.0013(11) -0.0064(13) C(A2 0.0189(15) 0.0255(16) 0.0207(15) -0.0089(13) -0.0010(12) -0.0097(13) C(A3 0.0147(13) 0.0173(14) 0.0199(15) -0.0015(12) -0.0006(11) -0.0055(11) C(A4 0.0143(13) 0.0217(15) 0.0101(12) -0.0042(11) 0.0025(10) -0.0062(11) C(A5 0.0125(13) 0.0195(14) 0.0159(14) -0.0069(11) 0.0010(10) -0.0057(11) C(A6 0.0160(14) 0.0163(14) 0.0221(15) -0.0048(12) 0.0018(11) -0.0059(11) C(A7 0.0295(18) 0.0211(16) 0.0220(16) -0.0030(13) 0.0036(13) -0.0131(14) C(A8 0.0253(17) 0.0345(19) 0.0134(14) -0.0018(13) 0.0002(12) -0.0128(14) C(B1 0.037(2) 0.034(2) 0.0192(16) -0.0126(15) -0.0033(15) -0.0071(16) C(B2 0.038(2) 0.0278(19) 0.0269(18) -0.0123(15) -0.0022(16) -0.0106(16) C(B3 0.0242(16) 0.0239(17) 0.0203(16) 0.0017(13) -0.0012(13) -0.0082(13) C(B4 0.0277(17) 0.0226(16) 0.0159(14) -0.0001(12) 0.0003(12) -0.0122(13) C(B5 0.0184(14) 0.0246(16) 0.0200(15) -0.0116(13) 0.0009(12) -0.0083(12) C(B6 0.0200(15) 0.0190(15) 0.0290(17) -0.0089(13) 0.0005(13) -0.0079(12) C(B7 0.057(3) 0.035(2) 0.0232(19) 0.0035(16) 0.0038(18) -0.024(2) C(B8 0.053(3) 0.039(2) 0.0160(16) 0.0033(15) 0.0030(16) -0.020(2) C(M1 0.0229(16) 0.0336(19) 0.0142(14) -0.0065(13) -0.0007(12) -0.0061(14) C(M2 0.0173(14) 0.0178(14) 0.0242(16) -0.0041(12) -0.0023(12) -0.0084(12) C(M3 0.0150(13) 0.0220(15) 0.0119(13) -0.0049(11) 0.0017(10) -0.0050(11) C(M4 0.0217(16) 0.0202(15) 0.0248(17) -0.0033(13) 0.0024(13) -0.0077(13) C11A 0.033(8) 0.040(3) 0.0129(18) -0.0071(19) -0.002(5) -0.010(6) C12A 0.033(4) 0.042(4) 0.027(4) -0.015(3) 0.013(3) -0.023(3) C11B 0.033(8) 0.040(3) 0.0129(18) -0.0071(19) -0.002(5) -0.010(6) C12B 0.039(4) 0.044(5) 0.015(3) -0.005(3) -0.001(3) -0.017(4) C(21 0.0274(17) 0.0198(16) 0.0294(18) -0.0070(13) -0.0013(14) -0.0093(13) C(22 0.035(2) 0.0205(18) 0.053(3) -0.0107(17) -0.0048(19) -0.0013(16) C(31 0.0289(17) 0.0298(18) 0.0114(14) -0.0049(12) 0.0019(12) -0.0130(14) C(32 0.037(2) 0.053(3) 0.0192(17) -0.0050(17) -0.0083(15) -0.0169(19) C(41 0.046(2) 0.0217(18) 0.033(2) -0.0025(15) 0.0057(17) -0.0182(17) C(42 0.053(3) 0.047(3) 0.075(4) -0.019(3) 0.020(3) -0.037(3) Sb(1 0.02828(14) 0.02529(14) 0.02220(13) -0.00817(9) 0.00280(9) -0.01553(10) Cl2A 0.055(2) 0.034(4) 0.037(3) -0.020(3) 0.0190(16) -0.0208(18) Cl2B 0.0687(16) 0.075(5) 0.075(4) -0.059(4) 0.0317(16) -0.0299(17) Cl(3 0.0755(9) 0.0761(9) 0.0274(5) 0.0073(5) -0.0175(5) -0.0555(8) Cl(4 0.0818(9) 0.0620(7) 0.0238(5) 0.0043(5) -0.0093(5) -0.0588(7) Cl(5 0.0282(5) 0.0797(9) 0.0445(6) -0.0329(6) 0.0022(4) -0.0015(5) Cl(6 0.0334(5) 0.0295(5) 0.0548(7) 0.0040(4) -0.0164(5) -0.0115(4) Cl(7 0.0742(10) 0.0443(7) 0.0964(12) 0.0219(7) -0.0423(9) -0.0447(7) C(5A 0.067(8) 0.042(6) 0.050(6) -0.002(5) 0.004(5) -0.036(5) C(5B 0.073(8) 0.051(6) 0.048(6) -0.023(5) 0.011(5) -0.036(6) Cl(8 0.0916(13) 0.0636(10) 0.0631(9) -0.0134(8) -0.0095(9) -0.0273(9) Cl(9 0.173(2) 0.1059(16) 0.0367(8) 0.0016(9) -0.0313(11) -0.0681(16) _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 Fe(1 N(3) 2.060(3) . ? Fe(1 N(4) 2.066(3) . ? Fe(1 N(2) 2.067(3) . ? Fe(1 N(1) 2.078(3) . ? Fe(1 Cl(1 2.1634(11) . ? N(1) C(A2 1.370(4) . ? N(1) C(A1 1.381(4) . ? N(2) C(A4 1.369(4) . ? N(2) C(A3 1.384(4) . ? N(3) C(A6 1.377(4) . ? N(3) C(A5 1.383(4) . ? N(4) C(A8 1.374(4) . ? N(4) C(A7 1.383(5) . ? C(A1 C(M1 1.390(5) . ? C(A1 C(B1 1.431(5) . ? C(A2 C(M2 1.403(5) . ? C(A2 C(B2 1.433(5) . ? C(A3 C(M2 1.395(5) . ? C(A3 C(B3 1.446(5) . ? C(A4 C(M3 1.412(5) . ? C(A4 C(B4 1.440(4) . ? C(A5 C(M3 1.395(4) . ? C(A5 C(B5 1.437(4) . ? C(A6 C(M4 1.409(5) . ? C(A6 C(B6 1.428(5) . ? C(A7 C(M4 1.398(5) . ? C(A7 C(B7 1.430(5) . ? C(A8 C(M1 1.408(6) . ? C(A8 C(B8 1.433(5) . ? C(B1 C(B2 1.342(6) . ? C(B3 C(B4 1.339(5) . ? C(B5 C(B6 1.348(5) . ? C(B7 C(B8 1.348(7) . ? C(M1 C11A 1.52(2) . ? C(M1 C11B 1.523(19) . ? C(M2 C(21 1.510(5) . ? C(M3 C(31 1.513(4) . ? C(M4 C(41 1.517(5) . ? C11A C12A 1.554(14) . ? C11B C12B 1.529(14) . ? C(21 C(22 1.527(6) . ? C(31 C(32 1.526(5) . ? C(41 C(42 1.525(7) . ? Sb(1 Cl(5 2.3311(14) . ? Sb(1 Cl2B 2.346(3) . ? Sb(1 Cl(7 2.3490(13) . ? Sb(1 Cl(3 2.3542(15) . ? Sb(1 Cl(4 2.3719(12) . ? Sb(1 Cl2A 2.377(5) . ? Sb(1 Cl(6 2.3815(14) . ? Cl2A Cl2B 0.686(4) . ? C(5A Cl(9 1.571(10) . ? C(5A Cl(8 1.846(12) . ? C(5B Cl(8 1.602(11) . ? C(5B Cl(9 1.884(12) . ? 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 N(3) Fe(1 N(4) 87.15(11) . . ? N(3) Fe(1 N(2) 87.20(11) . . ? N(4) Fe(1 N(2) 153.83(11) . . ? N(3) Fe(1 N(1) 154.48(10) . . ? N(4) Fe(1 N(1) 86.84(12) . . ? N(2) Fe(1 N(1) 87.34(11) . . ? N(3) Fe(1 Cl(1 102.39(8) . . ? N(4) Fe(1 Cl(1 104.44(9) . . ? N(2) Fe(1 Cl(1 101.73(8) . . ? N(1) Fe(1 Cl(1 103.13(8) . . ? C(A2 N(1) C(A1 106.0(3) . . ? C(A2 N(1) Fe(1 126.1(2) . . ? C(A1 N(1) Fe(1 125.6(2) . . ? C(A4 N(2) C(A3 105.9(3) . . ? C(A4 N(2) Fe(1 125.9(2) . . ? C(A3 N(2) Fe(1 125.5(2) . . ? C(A6 N(3) C(A5 105.2(3) . . ? C(A6 N(3) Fe(1 126.1(2) . . ? C(A5 N(3) Fe(1 126.0(2) . . ? C(A8 N(4) C(A7 105.4(3) . . ? C(A8 N(4) Fe(1 126.8(2) . . ? C(A7 N(4) Fe(1 126.5(2) . . ? N(1) C(A1 C(M1 125.8(3) . . ? N(1) C(A1 C(B1 109.5(3) . . ? C(M1 C(A1 C(B1 124.7(3) . . ? N(1) C(A2 C(M2 125.8(3) . . ? N(1) C(A2 C(B2 109.8(3) . . ? C(M2 C(A2 C(B2 124.4(3) . . ? N(2) C(A3 C(M2 126.2(3) . . ? N(2) C(A3 C(B3 109.5(3) . . ? C(M2 C(A3 C(B3 124.3(3) . . ? N(2) C(A4 C(M3 125.6(3) . . ? N(2) C(A4 C(B4 110.0(3) . . ? C(M3 C(A4 C(B4 124.4(3) . . ? N(3) C(A5 C(M3 125.8(3) . . ? N(3) C(A5 C(B5 110.0(3) . . ? C(M3 C(A5 C(B5 124.2(3) . . ? N(3) C(A6 C(M4 125.1(3) . . ? N(3) C(A6 C(B6 110.5(3) . . ? C(M4 C(A6 C(B6 124.3(3) . . ? N(4) C(A7 C(M4 125.5(3) . . ? N(4) C(A7 C(B7 110.0(3) . . ? C(M4 C(A7 C(B7 124.5(3) . . ? N(4) C(A8 C(M1 125.7(3) . . ? N(4) C(A8 C(B8 110.2(3) . . ? C(M1 C(A8 C(B8 124.0(3) . . ? C(B2 C(B1 C(A1 107.4(3) . . ? C(B1 C(B2 C(A2 107.3(3) . . ? C(B4 C(B3 C(A3 107.1(3) . . ? C(B3 C(B4 C(A4 107.5(3) . . ? C(B6 C(B5 C(A5 107.1(3) . . ? C(B5 C(B6 C(A6 107.2(3) . . ? C(B8 C(B7 C(A7 107.3(4) . . ? C(B7 C(B8 C(A8 107.1(3) . . ? C(A1 C(M1 C(A8 124.0(3) . . ? C(A1 C(M1 C11A 121.9(8) . . ? C(A8 C(M1 C11A 113.6(8) . . ? C(A1 C(M1 C11B 113.7(8) . . ? C(A8 C(M1 C11B 121.7(8) . . ? C11A C(M1 C11B 17.7(6) . . ? C(A3 C(M2 C(A2 124.3(3) . . ? C(A3 C(M2 C(21 117.9(3) . . ? C(A2 C(M2 C(21 117.7(3) . . ? C(A5 C(M3 C(A4 123.9(3) . . ? C(A5 C(M3 C(31 117.9(3) . . ? C(A4 C(M3 C(31 118.0(3) . . ? C(A7 C(M4 C(A6 124.2(3) . . ? C(A7 C(M4 C(41 118.0(3) . . ? C(A6 C(M4 C(41 117.7(3) . . ? C(M1 C11A C12A 113.5(10) . . ? C(M1 C11B C12B 113.3(11) . . ? C(M2 C(21 C(22 110.7(3) . . ? C(M3 C(31 C(32 110.9(3) . . ? C(M4 C(41 C(42 110.4(4) . . ? Cl(5 Sb(1 Cl2B 173.7(3) . . ? Cl(5 Sb(1 Cl(7 90.93(7) . . ? Cl2B Sb(1 Cl(7 85.6(3) . . ? Cl(5 Sb(1 Cl(3 91.44(6) . . ? Cl2B Sb(1 Cl(3 93.8(2) . . ? Cl(7 Sb(1 Cl(3 89.82(5) . . ? Cl(5 Sb(1 Cl(4 89.69(6) . . ? Cl2B Sb(1 Cl(4 93.7(3) . . ? Cl(7 Sb(1 Cl(4 178.98(5) . . ? Cl(3 Sb(1 Cl(4 90.96(5) . . ? Cl(5 Sb(1 Cl2A 169.0(3) . . ? Cl2B Sb(1 Cl2A 16.68(11) . . ? Cl(7 Sb(1 Cl2A 99.0(3) . . ? Cl(3 Sb(1 Cl2A 83.94(18) . . ? Cl(4 Sb(1 Cl2A 80.4(3) . . ? Cl(5 Sb(1 Cl(6 88.95(5) . . ? Cl2B Sb(1 Cl(6 85.8(2) . . ? Cl(7 Sb(1 Cl(6 90.44(5) . . ? Cl(3 Sb(1 Cl(6 179.52(5) . . ? Cl(4 Sb(1 Cl(6 88.77(5) . . ? Cl2A Sb(1 Cl(6 95.63(18) . . ? Cl2B Cl2A Sb(1 79.1(5) . . ? Cl2A Cl2B Sb(1 84.3(6) . . ? Cl(9 C(5A Cl(8 114.7(7) . . ? Cl(8 C(5B Cl(9 111.3(6) . . ? C(5B Cl(8 C(5A 47.4(6) . . ? C(5A Cl(9 C(5B 46.9(6) . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 29.95 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.46 _refine_diff_density_min -1.71 _refine_diff_density_rms 0.147 #_refine_diff_density_max #; #1.46 at o.92 \%A from Cl(9 #1.28 at 0.74 \%A from Sb(1 #1.26 at 0.94 \%A from C(5a #1.09 at 1.02 \%A from Sb(1 #1.02 at 1.15 \%A from Sb(1 #1.00 at 2.10 \%A from Sb(1 #; #_refine_diff_density_min #; #-1.71 at 0.08 \%A from Sb(1 #; #_refine_diff_density_rms 0.147 #=====END data_sd:fetprclsbcl6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H38 Cl9 Fe N4 Sb' _chemical_formula_weight 987.32 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' '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' 'Sb' 'Sb' -0.5866 1.5461 '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 10.0407(1) _cell_length_b 14.4882(6) _cell_length_c 15.7601(9) _cell_angle_alpha 111.079(5) _cell_angle_beta 103.848(7) _cell_angle_gamma 101.504(5) _cell_volume 1971.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min -20.5 _cell_measurement_theta_max 20.5 _exptl_crystal_description Rhombohedron _exptl_crystal_colour 'Dark purple' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method ? _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.694 _exptl_absorpt_correction_type Refdelf _exptl_absorpt_correction_T_min 0.5730 _exptl_absorpt_correction_T_max 0.7281 _exptl_absorpt_process_details 'Stuart & Walker, 1983)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-nonius Fast Area-Detector' _diffrn_measurement_method 'Ellipsoid-mask Fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'No measurable crystal decay' _diffrn_reflns_number 19282 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.82 _reflns_number_total 9979 _reflns_number_gt 8908 _reflns_threshold_expression >2sigma(I) _computing_data_collection Madnes _computing_cell_refinement Madnes _computing_data_reduction 'madnes (Messerschmitt & Pflugraph, 1987)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep III (burnett, Johnson, 1996)' _computing_publication_material 'Shelxl-97' _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_weighting_scheme_details 'w=1/[\s^2^(Fo^2^)+(0.0853P)^2^+2.3858P] 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 SHELXL _refine_ls_extinction_coef 0.0153(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9979 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.23787(4) 0.02952(3) 0.06908(2) 0.01027(10) Uani 1 d . . . Cl1 Cl 0.47041(7) 0.09086(6) 0.10837(5) 0.02117(15) Uani 1 d . . . N1 N 0.1618(2) 0.10457(17) -0.01262(15) 0.0125(4) Uani 1 d . . . N2 N 0.1787(2) -0.10056(17) -0.05956(16) 0.0134(4) Uani 1 d . . . N3 N 0.2116(2) -0.07114(17) 0.13374(16) 0.0146(4) Uani 1 d . . . N4 N 0.1985(2) 0.13490(17) 0.18165(15) 0.0124(4) Uani 1 d . . . C(M1 C 0.1719(3) 0.2668(2) 0.11903(19) 0.0155(5) Uani 1 d . . . C(M2 C 0.1466(3) -0.0189(2) -0.17372(18) 0.0147(5) Uani 1 d . . . C(M3 C 0.2072(3) -0.2318(2) 0.0035(2) 0.0203(5) Uani 1 d . . . C(M4 C 0.2264(3) 0.0524(2) 0.29454(19) 0.0162(5) Uani 1 d . . . C(A1 C 0.1584(3) 0.2051(2) 0.02317(19) 0.0145(5) Uani 1 d . . . C(A2 C 0.1476(3) 0.0767(2) -0.10887(18) 0.0136(4) Uani 1 d . . . C(A3 C 0.1609(3) -0.1020(2) -0.14869(18) 0.0148(5) Uani 1 d . . . C(A4 C 0.1919(3) -0.1969(2) -0.0689(2) 0.0176(5) Uani 1 d . . . C(A5 C 0.2127(3) -0.1722(2) 0.0979(2) 0.0188(5) Uani 1 d . . . C(A6 C 0.2189(3) -0.0446(2) 0.2285(2) 0.0166(5) Uani 1 d . . . C(A7 C 0.2205(3) 0.1370(2) 0.27171(18) 0.0151(5) Uani 1 d . . . C(A8 C 0.1927(3) 0.2326(2) 0.19257(18) 0.0137(4) Uani 1 d . . . C(B1 C 0.1427(3) 0.2417(2) -0.0512(2) 0.0200(5) Uani 1 d . . . H(B1 H 0.1384 0.3087 -0.0445 0.024 Uiso 1 calc R . . C(B2 C 0.1354(3) 0.1624(2) -0.1324(2) 0.0190(5) Uani 1 d . . . H(B2 H 0.1241 0.1631 -0.1937 0.023 Uiso 1 calc R . . C(B3 C 0.1607(3) -0.2001(2) -0.21541(19) 0.0196(5) Uani 1 d . . . H(B3 H 0.1480 -0.2205 -0.2820 0.023 Uiso 1 calc R . . C(B4 C 0.1819(3) -0.2580(2) -0.1661(2) 0.0219(6) Uani 1 d . . . H(B4 H 0.1889 -0.3264 -0.1910 0.026 Uiso 1 calc R . . C(B5 C 0.2194(3) -0.2094(2) 0.1710(2) 0.0232(6) Uani 1 d . . . H(B5 H 0.2215 -0.2770 0.1642 0.028 Uiso 1 calc R . . C(B6 C 0.2222(3) -0.1323(2) 0.2508(2) 0.0227(6) Uani 1 d . . . H(B6 H 0.2258 -0.1349 0.3106 0.027 Uiso 1 calc R . . C(B7 C 0.2318(3) 0.2378(2) 0.33990(19) 0.0191(5) Uani 1 d . . . H(B7 H 0.2495 0.2593 0.4072 0.023 Uiso 1 calc R . . C(B8 C 0.2127(3) 0.2966(2) 0.2910(2) 0.0189(5) Uani 1 d . . . H(B8 H 0.2126 0.3668 0.3169 0.023 Uiso 1 calc R . . C(11 C 0.1714(3) 0.3773(2) 0.1461(2) 0.0186(5) Uani 1 d . . . H(1A H 0.1262 0.3971 0.1966 0.022 Uiso 1 calc R . . H(1B H 0.1123 0.3822 0.0888 0.022 Uiso 1 calc R . . C(12 C 0.3237(3) 0.4535(2) 0.1837(2) 0.0236(6) Uani 1 d . . . H(1C H 0.3823 0.4500 0.2421 0.028 Uiso 1 calc R . . H(1D H 0.3698 0.4331 0.1339 0.028 Uiso 1 calc R . . C(13 C 0.3207(4) 0.5645(3) 0.2086(3) 0.0321(7) Uani 1 d . . . H(1E H 0.2611 0.5677 0.1512 0.048 Uiso 1 calc R . . H(1F H 0.4193 0.6113 0.2303 0.048 Uiso 1 calc R . . H(1G H 0.2797 0.5861 0.2603 0.048 Uiso 1 calc R . . C(21 C 0.1330(3) -0.0366(2) -0.27652(19) 0.0188(5) Uani 1 d . . . H(2A H 0.0941 0.0158 -0.2908 0.023 Uiso 1 calc R . . H(2B H 0.0629 -0.1064 -0.3213 0.023 Uiso 1 calc R . . C(22 C 0.2777(3) -0.0296(3) -0.2953(2) 0.0268(6) Uani 1 d . . . H(2C H 0.3148 -0.0838 -0.2832 0.032 Uiso 1 calc R . . H(2D H 0.2605 -0.0446 -0.3641 0.032 Uiso 1 calc R . . C(23 C 0.3915(4) 0.0757(3) -0.2328(3) 0.0339(8) Uani 1 d . . . H(2E H 0.3562 0.1297 -0.2450 0.051 Uiso 1 calc R . . H(2F H 0.4802 0.0755 -0.2485 0.051 Uiso 1 calc R . . H(2G H 0.4118 0.0901 -0.1645 0.051 Uiso 1 calc R . . C(31 C 0.2218(5) -0.3393(2) -0.0194(3) 0.0342(8) Uani 1 d . . . H(3A H 0.1559 -0.3751 0.0049 0.041 Uiso 1 calc R A 1 H(3B H 0.1869 -0.3788 -0.0906 0.041 Uiso 1 calc R A 1 C32A C 0.3592(11) -0.3467(8) 0.0171(9) 0.0257(14) Uani 0.509(8) d P B 1 H32A H 0.3514 -0.4195 0.0064 0.031 Uiso 0.509(8) calc PR B 1 H32B H 0.4021 -0.3017 0.0875 0.031 Uiso 0.509(8) calc PR B 1 C33A C 0.4546(8) -0.3119(7) -0.0353(6) 0.0392(19) Uani 0.509(8) d P B 1 H33A H 0.4078 -0.3536 -0.1052 0.059 Uiso 0.509(8) calc PR B 1 H33B H 0.5486 -0.3218 -0.0143 0.059 Uiso 0.509(8) calc PR B 1 H33C H 0.4684 -0.2381 -0.0199 0.059 Uiso 0.509(8) calc PR B 1 C32B C 0.3993(12) -0.3265(9) 0.0095(9) 0.0257(14) Uani 0.491(8) d P B 2 H32C H 0.4406 -0.2953 -0.0287 0.031 Uiso 0.491(8) calc PR B 2 H32D H 0.4494 -0.2787 0.0788 0.031 Uiso 0.491(8) calc PR B 2 C33B C 0.4256(9) -0.4311(6) -0.0100(6) 0.0357(19) Uani 0.491(8) d P B 2 H33D H 0.3851 -0.4621 0.0278 0.054 Uiso 0.491(8) calc PR B 2 H33E H 0.5298 -0.4206 0.0085 0.054 Uiso 0.491(8) calc PR B 2 H33F H 0.3789 -0.4779 -0.0790 0.054 Uiso 0.491(8) calc PR B 2 C(41 C 0.2468(3) 0.0698(2) 0.3977(2) 0.0203(5) Uani 1 d . . . H(4A H 0.1990 0.0036 0.3987 0.024 Uiso 1 calc R . . H(4B H 0.2001 0.1215 0.4261 0.024 Uiso 1 calc R . . C(42 C 0.4070(3) 0.1088(3) 0.4593(2) 0.0231(6) Uani 1 d . . . H(4C H 0.4526 0.0554 0.4332 0.028 Uiso 1 calc R . . H(4D H 0.4561 0.1729 0.4556 0.028 Uiso 1 calc R . . C(43 C 0.4262(4) 0.1314(4) 0.5636(2) 0.0361(8) Uani 1 d . . . H(4E H 0.3948 0.1916 0.5925 0.054 Uiso 1 calc R . . H(4F H 0.5283 0.1467 0.5994 0.054 Uiso 1 calc R . . H(4G H 0.3679 0.0706 0.5667 0.054 Uiso 1 calc R . . Sb(1 Sb 0.956135(19) 0.663187(14) 0.363571(12) 0.01772(8) Uani 1 d . . . Cl(2 Cl 0.70589(10) 0.58033(11) 0.30939(9) 0.0532(3) Uani 1 d . . . Cl(3 Cl 0.91839(12) 0.82530(8) 0.38609(8) 0.0429(2) Uani 1 d . . . Cl(4 Cl 0.96877(11) 0.69160(7) 0.52256(6) 0.0361(2) Uani 1 d . . . Cl(5 Cl 0.94337(11) 0.62697(8) 0.20241(6) 0.0377(2) Uani 1 d . . . Cl(6 Cl 0.99945(10) 0.50329(6) 0.34263(6) 0.03241(18) Uani 1 d . . . Cl(7 Cl 1.20642(8) 0.74833(6) 0.42024(6) 0.02907(17) Uani 1 d . . . Cl(8 Cl 1.42263(11) 0.58968(7) 0.46924(6) 0.0380(2) Uani 1 d . . . Cl(9 Cl 1.40350(11) 0.69185(8) 0.66159(7) 0.0444(2) Uani 1 d . . . C(1) C 1.3278(5) 0.5834(3) 0.5492(3) 0.0409(9) Uani 1 d . . . H(1H H 1.2263 0.5782 0.5194 0.049 Uiso 1 calc R . . H(1I H 1.3273 0.5196 0.5591 0.049 Uiso 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 0.01001(17) 0.00954(17) 0.01139(17) 0.00489(13) 0.00313(12) 0.00319(13) Cl1 0.0105(3) 0.0235(3) 0.0232(3) 0.0059(3) 0.0040(2) 0.0022(2) N1 0.0132(9) 0.0132(10) 0.0131(9) 0.0070(8) 0.0045(7) 0.0053(8) N2 0.0115(9) 0.0124(10) 0.0143(9) 0.0052(8) 0.0029(7) 0.0026(8) N3 0.0150(10) 0.0129(10) 0.0173(10) 0.0079(8) 0.0049(8) 0.0053(8) N4 0.0125(9) 0.0141(10) 0.0123(9) 0.0057(8) 0.0049(7) 0.0063(8) C(M1 0.0148(11) 0.0151(11) 0.0168(11) 0.0067(9) 0.0037(9) 0.0071(9) C(M2 0.0110(10) 0.0175(12) 0.0143(11) 0.0063(9) 0.0033(9) 0.0037(9) C(M3 0.0220(13) 0.0126(12) 0.0245(13) 0.0086(10) 0.0046(10) 0.0047(10) C(M4 0.0111(11) 0.0252(13) 0.0172(11) 0.0136(10) 0.0058(9) 0.0060(10) C(A1 0.0147(11) 0.0141(11) 0.0166(11) 0.0075(9) 0.0058(9) 0.0058(9) C(A2 0.0111(10) 0.0180(12) 0.0144(11) 0.0095(9) 0.0048(9) 0.0046(9) C(A3 0.0101(10) 0.0155(11) 0.0134(10) 0.0028(9) 0.0014(8) 0.0026(9) C(A4 0.0161(12) 0.0116(11) 0.0189(12) 0.0035(9) 0.0021(9) 0.0024(9) C(A5 0.0188(12) 0.0145(12) 0.0249(13) 0.0114(10) 0.0057(10) 0.0053(10) C(A6 0.0142(11) 0.0189(12) 0.0208(12) 0.0143(10) 0.0050(9) 0.0041(9) C(A7 0.0139(11) 0.0195(12) 0.0135(11) 0.0085(9) 0.0050(9) 0.0052(9) C(A8 0.0124(11) 0.0145(11) 0.0150(11) 0.0062(9) 0.0050(9) 0.0057(9) C(B1 0.0269(14) 0.0175(12) 0.0209(12) 0.0131(11) 0.0069(11) 0.0103(11) C(B2 0.0233(13) 0.0199(12) 0.0161(11) 0.0108(10) 0.0058(10) 0.0068(10) C(B3 0.0195(12) 0.0157(12) 0.0143(11) -0.0006(9) 0.0027(9) 0.0034(10) C(B4 0.0214(13) 0.0138(12) 0.0220(13) 0.0012(10) 0.0029(10) 0.0056(10) C(B5 0.0236(14) 0.0217(13) 0.0324(15) 0.0198(12) 0.0088(12) 0.0091(11) C(B6 0.0225(13) 0.0276(15) 0.0279(14) 0.0216(12) 0.0086(11) 0.0097(11) C(B7 0.0211(13) 0.0233(13) 0.0141(11) 0.0065(10) 0.0081(10) 0.0096(11) C(B8 0.0206(13) 0.0190(12) 0.0178(12) 0.0061(10) 0.0078(10) 0.0094(10) C(11 0.0211(13) 0.0150(12) 0.0216(12) 0.0075(10) 0.0065(10) 0.0110(10) C(12 0.0259(14) 0.0154(12) 0.0309(15) 0.0108(11) 0.0093(12) 0.0080(11) C(13 0.0398(19) 0.0166(14) 0.0410(18) 0.0127(13) 0.0140(15) 0.0099(13) C(21 0.0170(12) 0.0266(14) 0.0118(11) 0.0081(10) 0.0036(9) 0.0065(10) C(22 0.0248(14) 0.0387(17) 0.0195(13) 0.0128(13) 0.0120(11) 0.0095(13) C(23 0.0213(15) 0.048(2) 0.0288(16) 0.0183(15) 0.0079(12) 0.0001(14) C(31 0.056(2) 0.0138(13) 0.0327(16) 0.0101(12) 0.0111(16) 0.0150(14) C32A 0.029(5) 0.020(4) 0.038(3) 0.019(2) 0.016(3) 0.012(3) C33A 0.029(4) 0.047(4) 0.044(4) 0.018(4) 0.009(3) 0.024(3) C32B 0.029(5) 0.020(4) 0.038(3) 0.019(2) 0.016(3) 0.012(3) C33B 0.046(4) 0.033(4) 0.038(4) 0.014(3) 0.017(3) 0.030(3) C(41 0.0178(12) 0.0298(14) 0.0171(12) 0.0143(11) 0.0062(10) 0.0072(11) C(42 0.0203(13) 0.0344(16) 0.0195(12) 0.0166(12) 0.0067(10) 0.0089(12) C(43 0.0265(16) 0.062(2) 0.0223(15) 0.0222(16) 0.0050(12) 0.0151(16) Sb(1 0.01738(12) 0.01832(12) 0.01713(11) 0.00785(8) 0.00598(7) 0.00434(8) Cl(2 0.0188(4) 0.0769(8) 0.0626(7) 0.0445(6) 0.0030(4) -0.0025(4) Cl(3 0.0495(5) 0.0399(5) 0.0600(6) 0.0293(5) 0.0267(5) 0.0316(4) Cl(4 0.0481(5) 0.0397(4) 0.0207(3) 0.0088(3) 0.0189(3) 0.0135(4) Cl(5 0.0482(5) 0.0409(5) 0.0210(3) 0.0163(3) 0.0091(3) 0.0052(4) Cl(6 0.0485(5) 0.0150(3) 0.0267(4) 0.0047(3) 0.0092(3) 0.0081(3) Cl(7 0.0197(3) 0.0286(4) 0.0377(4) 0.0173(3) 0.0063(3) 0.0035(3) Cl(8 0.0480(5) 0.0323(4) 0.0322(4) 0.0117(3) 0.0086(4) 0.0195(4) Cl(9 0.0334(4) 0.0443(5) 0.0390(5) 0.0012(4) 0.0121(4) 0.0098(4) C(1) 0.041(2) 0.0330(19) 0.0354(18) 0.0087(15) 0.0078(16) 0.0019(16) _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 N2 2.060(2) . ? Fe1 N4 2.064(2) . ? Fe1 N3 2.069(2) . ? Fe1 N1 2.071(2) . ? Fe1 Cl1 2.1700(7) . ? N1 C(A1 1.370(3) . ? N1 C(A2 1.385(3) . ? N2 C(A3 1.365(3) . ? N2 C(A4 1.386(3) . ? N3 C(A5 1.370(3) . ? N3 C(A6 1.382(3) . ? N4 C(A7 1.371(3) . ? N4 C(A8 1.378(3) . ? C(M1 C(A8 1.403(4) . ? C(M1 C(A1 1.408(4) . ? C(M1 C(11 1.504(4) . ? C(M2 C(A2 1.391(4) . ? C(M2 C(A3 1.417(4) . ? C(M2 C(21 1.513(4) . ? C(M3 C(A4 1.394(4) . ? C(M3 C(A5 1.407(4) . ? C(M3 C(31 1.513(4) . ? C(M4 C(A6 1.390(4) . ? C(M4 C(A7 1.404(4) . ? C(M4 C(41 1.508(4) . ? C(A1 C(B1 1.440(4) . ? C(A2 C(B2 1.436(4) . ? C(A3 C(B3 1.432(4) . ? C(A4 C(B4 1.434(4) . ? C(A5 C(B5 1.432(4) . ? C(A6 C(B6 1.438(4) . ? C(A7 C(B7 1.430(4) . ? C(A8 C(B8 1.431(4) . ? C(B1 C(B2 1.351(4) . ? C(B3 C(B4 1.347(4) . ? C(B5 C(B6 1.337(5) . ? C(B7 C(B8 1.351(4) . ? C(11 C(12 1.526(4) . ? C(12 C(13 1.521(4) . ? C(21 C(22 1.542(4) . ? C(22 C(23 1.512(5) . ? C(31 C32A 1.402(11) . ? C(31 C32B 1.684(12) . ? C32A C33A 1.529(12) . ? C32B C33B 1.525(13) . ? C(41 C(42 1.531(4) . ? C(42 C(43 1.511(4) . ? Sb(1 Cl(2 2.3486(9) . ? Sb(1 Cl(7 2.3519(8) . ? Sb(1 Cl(4 2.3557(8) . ? Sb(1 Cl(6 2.3634(8) . ? Sb(1 Cl(5 2.3668(8) . ? Sb(1 Cl(3 2.3677(9) . ? Cl(8 C(1) 1.768(4) . ? Cl(9 C(1) 1.749(4) . ? 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 N2 Fe1 N4 154.26(9) . . ? N2 Fe1 N3 87.15(9) . . ? N4 Fe1 N3 86.91(9) . . ? N2 Fe1 N1 87.00(9) . . ? N4 Fe1 N1 87.16(8) . . ? N3 Fe1 N1 153.35(9) . . ? N2 Fe1 Cl1 103.53(7) . . ? N4 Fe1 Cl1 102.21(6) . . ? N3 Fe1 Cl1 104.01(7) . . ? N1 Fe1 Cl1 102.64(6) . . ? C(A1 N1 C(A2 105.8(2) . . ? C(A1 N1 Fe1 125.75(17) . . ? C(A2 N1 Fe1 125.79(17) . . ? C(A3 N2 C(A4 105.5(2) . . ? C(A3 N2 Fe1 126.42(18) . . ? C(A4 N2 Fe1 125.54(17) . . ? C(A5 N3 C(A6 105.8(2) . . ? C(A5 N3 Fe1 126.44(19) . . ? C(A6 N3 Fe1 126.60(18) . . ? C(A7 N4 C(A8 105.4(2) . . ? C(A7 N4 Fe1 125.77(17) . . ? C(A8 N4 Fe1 125.75(17) . . ? C(A8 C(M1 C(A1 123.7(2) . . ? C(A8 C(M1 C(11 117.6(2) . . ? C(A1 C(M1 C(11 118.6(2) . . ? C(A2 C(M2 C(A3 123.6(2) . . ? C(A2 C(M2 C(21 119.5(2) . . ? C(A3 C(M2 C(21 116.9(2) . . ? C(A4 C(M3 C(A5 123.8(3) . . ? C(A4 C(M3 C(31 118.6(3) . . ? C(A5 C(M3 C(31 117.5(3) . . ? C(A6 C(M4 C(A7 123.8(2) . . ? C(A6 C(M4 C(41 118.6(2) . . ? C(A7 C(M4 C(41 117.6(3) . . ? N1 C(A1 C(M1 126.1(2) . . ? N1 C(A1 C(B1 110.3(2) . . ? C(M1 C(A1 C(B1 123.6(2) . . ? N1 C(A2 C(M2 125.9(2) . . ? N1 C(A2 C(B2 109.7(2) . . ? C(M2 C(A2 C(B2 124.5(2) . . ? N2 C(A3 C(M2 126.0(2) . . ? N2 C(A3 C(B3 110.5(2) . . ? C(M2 C(A3 C(B3 123.5(2) . . ? N2 C(A4 C(M3 125.8(2) . . ? N2 C(A4 C(B4 109.8(2) . . ? C(M3 C(A4 C(B4 124.4(3) . . ? N3 C(A5 C(M3 125.9(3) . . ? N3 C(A5 C(B5 109.7(3) . . ? C(M3 C(A5 C(B5 124.4(3) . . ? N3 C(A6 C(M4 126.0(2) . . ? N3 C(A6 C(B6 109.7(2) . . ? C(M4 C(A6 C(B6 124.3(3) . . ? N4 C(A7 C(M4 125.7(2) . . ? N4 C(A7 C(B7 110.2(2) . . ? C(M4 C(A7 C(B7 124.1(2) . . ? N4 C(A8 C(M1 125.7(2) . . ? N4 C(A8 C(B8 110.4(2) . . ? C(M1 C(A8 C(B8 123.8(2) . . ? C(B2 C(B1 C(A1 106.8(2) . . ? C(B1 C(B2 C(A2 107.4(2) . . ? C(B4 C(B3 C(A3 107.2(2) . . ? C(B3 C(B4 C(A4 107.0(2) . . ? C(B6 C(B5 C(A5 107.9(3) . . ? C(B5 C(B6 C(A6 106.9(3) . . ? C(B8 C(B7 C(A7 107.4(2) . . ? C(B7 C(B8 C(A8 106.6(2) . . ? C(M1 C(11 C(12 112.0(2) . . ? C(13 C(12 C(11 111.2(3) . . ? C(M2 C(21 C(22 113.2(2) . . ? C(23 C(22 C(21 113.3(3) . . ? C32A C(31 C(M3 118.1(5) . . ? C32A C(31 C32B 16.0(5) . . ? C(M3 C(31 C32B 107.7(4) . . ? C(31 C32A C33A 108.5(7) . . ? C33B C32B C(31 111.7(7) . . ? C(M4 C(41 C(42 111.7(2) . . ? C(43 C(42 C(41 111.2(3) . . ? Cl(2 Sb(1 Cl(7 179.00(4) . . ? Cl(2 Sb(1 Cl(4 89.74(4) . . ? Cl(7 Sb(1 Cl(4 89.49(3) . . ? Cl(2 Sb(1 Cl(6 90.52(4) . . ? Cl(7 Sb(1 Cl(6 90.09(3) . . ? Cl(4 Sb(1 Cl(6 88.12(3) . . ? Cl(2 Sb(1 Cl(5 89.84(4) . . ? Cl(7 Sb(1 Cl(5 90.95(3) . . ? Cl(4 Sb(1 Cl(5 177.46(3) . . ? Cl(6 Sb(1 Cl(5 89.38(3) . . ? Cl(2 Sb(1 Cl(3 90.76(4) . . ? Cl(7 Sb(1 Cl(3 88.63(3) . . ? Cl(4 Sb(1 Cl(3 91.78(4) . . ? Cl(6 Sb(1 Cl(3 178.72(4) . . ? Cl(5 Sb(1 Cl(3 90.73(4) . . ? Cl(9 C(1) Cl(8 112.8(2) . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 29.82 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.73 _refine_diff_density_min -1.78 _refine_diff_density_rms 0.179 #_refine_diff_density_max #; #1.73 at 0.76 \%A from Sb(1 #1.24 at 1.13 \%A from Sb(1 #1.20 at 0.92 \%A from Sb(1 #1.18 at 0.83 \%A from Cl(5 #1.18 at 1.08 \%A from Sb(1 #1.15 at 1.18 \%A from Sb(1 #1.10 at 0.90 \%A from Sb(1 #1.04 at 0.90 \%A from Cl(2 #1.00 at 0.83 \%A from Cl(3 #; #_refine_diff_density_min #; #-1.78 at 0.04 \%A from Sb(1 #; #_refine_diff_density_rms 0.179 #====END