Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 _publ_section_title ; Synthesis, structure and reactivity of ferrio-chloro-phosphanes, -arsanes and -stibanes [(CO)~2~(/h^5^-C~5~Me~5~)FePn(Cl)R] (Pn = P,As, Sb); R = tetramethylcyclopentadienyl, 2,7-di-tert-butyl-fluorenyl, 2,7-di-tert-butyl- 9-trimethylsilylfluorenyl) as precursor to novel metallo-phosphaalkenes, -arsaalkenes, and -stibaalkenes. ; _publ_contact_author_name 'Prof Lothar Weber' _publ_contact_author_address ; Fakultat fur Chemie der Universitat Bielefeld Universitats str. 25 Bielefeld D-33615 GERMANY ; _publ_contact_author_email LOTHAR.WEBER@UNI-BIELEFELD.DE _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name _publ_author_address 'Weber, Lothar' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Pumpenmeier, Lars' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Stammler, Hans-Georg' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; 'Neumann, Beate' ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; #========================================================================= data_compound2b _database_code_depnum_ccdc_archive 'CCDC 225075' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H28 As Cl Fe O2' _chemical_formula_sum 'C21 H28 As Cl Fe O2' _chemical_formula_weight 478.65 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' As As 0.0499 2.0058 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5320(2) _cell_length_b 13.3380(3) _cell_length_c 19.0760(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.9860(12) _cell_angle_gamma 90.00 _cell_volume 2115.33(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5063 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 2.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5325 _exptl_absorpt_correction_T_max 0.9100 _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 100(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59514 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4850 _reflns_number_gt 4384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD ' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1997)' _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^)+(0.0436P)^2^+0.3558P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4850 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 As1 As 0.26867(5) 0.91959(2) 0.126269(15) 0.02327(10) Uani 0.9385(14) 1 d P A 1 As1B As 0.1858(8) 0.8851(4) 0.1195(3) 0.0264(16) Uiso 0.0615(14) 1 d P A 2 Fe1 Fe 0.31451(5) 0.79596(3) 0.217527(19) 0.02273(10) Uani 1 1 d . . . Cl1 Cl 0.00397(10) 0.95637(6) 0.10622(4) 0.03685(19) Uani 0.9385(14) 1 d P A 1 Cl1B Cl 0.3408(16) 1.0239(9) 0.1291(7) 0.041(3) Uiso 0.0615(14) 1 d P A 2 O1 O 0.0888(3) 0.64703(19) 0.14282(12) 0.0484(6) Uani 1 1 d . . . O2 O 0.6114(3) 0.72858(17) 0.18290(11) 0.0389(5) Uani 1 1 d . . . C1 C 0.2636(4) 0.9100(2) 0.28869(14) 0.0276(6) Uani 1 1 d . A . C2 C 0.1736(3) 0.8217(2) 0.29332(13) 0.0283(6) Uani 1 1 d . A . C3 C 0.2863(4) 0.7410(2) 0.31757(14) 0.0291(6) Uani 1 1 d . A . C4 C 0.4435(4) 0.7793(2) 0.32540(13) 0.0268(6) Uani 1 1 d . A . C5 C 0.4300(4) 0.8844(2) 0.30625(14) 0.0273(6) Uani 1 1 d . A . C6 C 0.1970(4) 1.0139(2) 0.27644(16) 0.0376(7) Uani 1 1 d . . . H6A H 0.1903 1.0437 0.3226 0.056 Uiso 1 1 calc R A . H6B H 0.0894 1.0112 0.2447 0.056 Uiso 1 1 calc R . . H6C H 0.2677 1.0547 0.2540 0.056 Uiso 1 1 calc R . . C7 C -0.0059(4) 0.8142(3) 0.28298(17) 0.0402(7) Uani 1 1 d . . . H7A H -0.0363 0.8308 0.3282 0.060 Uiso 1 1 calc R A . H7B H -0.0406 0.7458 0.2686 0.060 Uiso 1 1 calc R . . H7C H -0.0577 0.8613 0.2454 0.060 Uiso 1 1 calc R . . C8 C 0.2451(4) 0.6361(2) 0.33557(16) 0.0388(8) Uani 1 1 d . . . H8A H 0.2402 0.6327 0.3864 0.058 Uiso 1 1 calc R A . H8B H 0.3277 0.5898 0.3267 0.058 Uiso 1 1 calc R . . H8C H 0.1404 0.6173 0.3054 0.058 Uiso 1 1 calc R . . C9 C 0.5974(4) 0.7230(2) 0.35429(15) 0.0366(7) Uani 1 1 d . . . H9A H 0.6273 0.7297 0.4068 0.055 Uiso 1 1 calc R A . H9B H 0.6832 0.7506 0.3334 0.055 Uiso 1 1 calc R . . H9C H 0.5819 0.6519 0.3415 0.055 Uiso 1 1 calc R . . C10 C 0.5669(4) 0.9565(2) 0.31030(17) 0.0377(7) Uani 1 1 d . . . H10A H 0.5953 0.9863 0.3585 0.057 Uiso 1 1 calc R A . H10B H 0.5346 1.0096 0.2744 0.057 Uiso 1 1 calc R . . H10C H 0.6601 0.9207 0.3006 0.057 Uiso 1 1 calc R . . C11 C 0.1789(4) 0.7073(2) 0.16787(14) 0.0324(7) Uani 1 1 d . A . C12 C 0.4894(4) 0.7559(2) 0.19147(14) 0.0273(6) Uani 1 1 d . A . C13 C 0.2606(3) 0.8581(2) 0.02814(14) 0.0267(6) Uani 1 1 d . . . H13A H 0.2351 0.9116 -0.0094 0.032 Uiso 1 1 calc R A 1 C14 C 0.1536(4) 0.7702(2) 0.00511(14) 0.0283(6) Uani 1 1 d . A . C15 C 0.2472(3) 0.6897(2) 0.00057(13) 0.0257(6) Uani 1 1 d . . . C16 C 0.4169(3) 0.7193(2) 0.01770(13) 0.0260(6) Uani 1 1 d . A . C17 C 0.4271(3) 0.8192(2) 0.03162(14) 0.0260(6) Uani 1 1 d . A . C18 C -0.0281(4) 0.7736(2) -0.01290(17) 0.0375(7) Uani 1 1 d . . . H18A H -0.0707 0.7065 -0.0269 0.056 Uiso 1 1 calc R A . H18B H -0.0655 0.8203 -0.0528 0.056 Uiso 1 1 calc R . . H18C H -0.0660 0.7961 0.0293 0.056 Uiso 1 1 calc R . . C19 C 0.1930(4) 0.5833(2) -0.01892(16) 0.0344(6) Uani 1 1 d . A . H19A H 0.0754 0.5798 -0.0280 0.052 Uiso 1 1 calc R . . H19B H 0.2401 0.5384 0.0209 0.052 Uiso 1 1 calc R . . H19C H 0.2282 0.5629 -0.0623 0.052 Uiso 1 1 calc R . . C20 C 0.5518(4) 0.6463(2) 0.01929(15) 0.0313(6) Uani 1 1 d . . . H20A H 0.6549 0.6819 0.0317 0.047 Uiso 1 1 calc R A . H20B H 0.5394 0.6151 -0.0282 0.047 Uiso 1 1 calc R . . H20C H 0.5491 0.5944 0.0553 0.047 Uiso 1 1 calc R . . C21 C 0.5767(4) 0.8823(2) 0.04956(16) 0.0327(6) Uani 1 1 d . . . H21A H 0.6706 0.8407 0.0482 0.049 Uiso 1 1 calc R A . H21B H 0.5883 0.9109 0.0978 0.049 Uiso 1 1 calc R . . H21C H 0.5686 0.9367 0.0143 0.049 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 As1 0.0285(2) 0.02193(15) 0.02004(13) 0.00005(11) 0.00676(13) 0.00250(16) Fe1 0.0242(2) 0.02637(19) 0.01789(17) -0.00033(13) 0.00522(16) -0.00065(17) Cl1 0.0346(4) 0.0463(4) 0.0286(4) -0.0028(3) 0.0049(3) 0.0161(4) O1 0.0597(16) 0.0560(14) 0.0303(11) -0.0073(10) 0.0117(11) -0.0298(13) O2 0.0355(12) 0.0531(13) 0.0279(10) 0.0011(9) 0.0063(9) 0.0150(10) C1 0.0330(15) 0.0335(14) 0.0178(12) -0.0016(11) 0.0087(11) 0.0033(12) C2 0.0270(14) 0.0425(16) 0.0167(12) -0.0034(11) 0.0072(11) -0.0010(12) C3 0.0365(15) 0.0342(15) 0.0178(12) -0.0004(10) 0.0084(11) -0.0028(13) C4 0.0302(14) 0.0340(13) 0.0154(11) -0.0008(10) 0.0038(11) 0.0014(13) C5 0.0314(15) 0.0326(14) 0.0182(11) -0.0039(10) 0.0064(11) -0.0056(12) C6 0.0509(19) 0.0343(15) 0.0289(14) -0.0035(12) 0.0118(14) 0.0090(15) C7 0.0313(16) 0.059(2) 0.0319(15) -0.0039(14) 0.0115(13) -0.0034(15) C8 0.052(2) 0.0402(17) 0.0258(14) 0.0028(12) 0.0120(14) -0.0056(15) C9 0.0357(17) 0.0470(17) 0.0243(13) 0.0005(13) 0.0011(12) 0.0084(14) C10 0.0413(18) 0.0398(16) 0.0336(15) -0.0077(13) 0.0120(14) -0.0137(14) C11 0.0397(17) 0.0394(16) 0.0193(13) 0.0001(12) 0.0094(12) -0.0088(14) C12 0.0337(16) 0.0282(14) 0.0194(12) 0.0014(10) 0.0044(11) 0.0054(12) C13 0.0320(15) 0.0298(14) 0.0192(12) 0.0026(10) 0.0079(10) 0.0059(11) C14 0.0340(15) 0.0328(14) 0.0195(12) 0.0031(11) 0.0088(11) 0.0047(12) C15 0.0320(15) 0.0283(14) 0.0182(12) 0.0000(10) 0.0086(10) 0.0030(11) C16 0.0318(15) 0.0285(13) 0.0199(12) 0.0039(10) 0.0106(11) 0.0030(11) C17 0.0291(15) 0.0298(13) 0.0205(12) 0.0028(10) 0.0084(11) 0.0021(11) C18 0.0324(16) 0.0420(17) 0.0356(16) -0.0094(13) 0.0024(13) 0.0006(13) C19 0.0400(16) 0.0283(14) 0.0341(15) -0.0016(11) 0.0065(14) -0.0011(14) C20 0.0344(15) 0.0301(14) 0.0317(14) 0.0015(11) 0.0123(13) 0.0069(13) C21 0.0327(16) 0.0320(14) 0.0377(15) 0.0022(12) 0.0170(14) 0.0009(13) _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 As1 C13 2.031(3) . ? As1 Cl1 2.2581(9) . ? As1 Fe1 2.3658(4) . ? As1B C13 2.019(6) . ? As1B Cl1B 2.259(15) . ? As1B Fe1 2.279(5) . ? Fe1 C12 1.758(3) . ? Fe1 C11 1.772(3) . ? Fe1 C2 2.106(3) . ? Fe1 C3 2.108(3) . ? Fe1 C5 2.116(3) . ? Fe1 C4 2.116(3) . ? Fe1 C1 2.147(3) . ? O1 C11 1.141(4) . ? O2 C12 1.149(3) . ? C1 C2 1.421(4) . ? C1 C5 1.425(4) . ? C1 C6 1.495(4) . ? C2 C3 1.448(4) . ? C2 C7 1.502(4) . ? C3 C4 1.412(4) . ? C3 C8 1.501(4) . ? C4 C5 1.447(4) . ? C4 C9 1.506(4) . ? C5 C10 1.502(4) . ? C13 C14 1.490(4) . ? C13 C17 1.500(4) . ? C14 C15 1.354(4) . ? C14 C18 1.511(4) . ? C15 C16 1.465(4) . ? C15 C19 1.512(4) . ? C16 C17 1.357(4) . ? C16 C20 1.502(4) . ? C17 C21 1.503(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 C13 As1 Cl1 96.09(8) . . ? C13 As1 Fe1 111.26(8) . . ? Cl1 As1 Fe1 105.65(3) . . ? C13 As1B Cl1B 85.6(4) . . ? C13 As1B Fe1 115.3(2) . . ? Cl1B As1B Fe1 101.3(4) . . ? C12 Fe1 C11 98.02(13) . . ? C12 Fe1 C2 153.53(12) . . ? C11 Fe1 C2 94.06(12) . . ? C12 Fe1 C3 115.28(12) . . ? C11 Fe1 C3 93.35(12) . . ? C2 Fe1 C3 40.18(11) . . ? C12 Fe1 C5 97.08(12) . . ? C11 Fe1 C5 158.46(12) . . ? C2 Fe1 C5 66.12(11) . . ? C3 Fe1 C5 66.24(11) . . ? C12 Fe1 C4 87.36(12) . . ? C11 Fe1 C4 125.75(12) . . ? C2 Fe1 C4 66.54(11) . . ? C3 Fe1 C4 39.05(11) . . ? C5 Fe1 C4 39.98(10) . . ? C12 Fe1 C1 134.34(12) . . ? C11 Fe1 C1 127.60(13) . . ? C2 Fe1 C1 39.01(11) . . ? C3 Fe1 C1 66.02(10) . . ? C5 Fe1 C1 39.04(11) . . ? C4 Fe1 C1 66.07(10) . . ? C12 Fe1 As1B 102.11(17) . . ? C11 Fe1 As1B 76.9(2) . . ? C2 Fe1 As1B 103.54(15) . . ? C3 Fe1 As1B 142.38(17) . . ? C5 Fe1 As1B 114.67(17) . . ? C4 Fe1 As1B 154.45(16) . . ? C1 Fe1 As1B 91.17(15) . . ? C12 Fe1 As1 90.82(9) . . ? C11 Fe1 As1 95.25(9) . . ? C2 Fe1 As1 111.48(8) . . ? C3 Fe1 As1 151.03(8) . . ? C5 Fe1 As1 99.80(8) . . ? C4 Fe1 As1 138.82(8) . . ? C1 Fe1 As1 87.01(7) . . ? As1B Fe1 As1 20.46(18) . . ? C2 C1 C5 108.1(2) . . ? C2 C1 C6 125.9(3) . . ? C5 C1 C6 125.6(3) . . ? C2 C1 Fe1 68.93(15) . . ? C5 C1 Fe1 69.30(15) . . ? C6 C1 Fe1 132.93(19) . . ? C1 C2 C3 107.9(2) . . ? C1 C2 C7 126.6(3) . . ? C3 C2 C7 125.2(3) . . ? C1 C2 Fe1 72.06(15) . . ? C3 C2 Fe1 69.98(15) . . ? C7 C2 Fe1 128.4(2) . . ? C4 C3 C2 108.2(2) . . ? C4 C3 C8 125.4(3) . . ? C2 C3 C8 126.4(3) . . ? C4 C3 Fe1 70.78(15) . . ? C2 C3 Fe1 69.84(14) . . ? C8 C3 Fe1 127.69(19) . . ? C3 C4 C5 107.7(2) . . ? C3 C4 C9 126.0(3) . . ? C5 C4 C9 126.1(3) . . ? C3 C4 Fe1 70.17(16) . . ? C5 C4 Fe1 70.01(15) . . ? C9 C4 Fe1 128.94(19) . . ? C1 C5 C4 108.1(2) . . ? C1 C5 C10 125.5(3) . . ? C4 C5 C10 126.2(3) . . ? C1 C5 Fe1 71.66(15) . . ? C4 C5 Fe1 70.01(15) . . ? C10 C5 Fe1 127.97(19) . . ? O1 C11 Fe1 172.7(2) . . ? O2 C12 Fe1 172.0(2) . . ? C14 C13 C17 104.6(2) . . ? C14 C13 As1B 95.9(3) . . ? C17 C13 As1B 120.2(2) . . ? C14 C13 As1 118.77(18) . . ? C17 C13 As1 105.27(17) . . ? As1B C13 As1 23.6(2) . . ? C15 C14 C13 108.2(2) . . ? C15 C14 C18 126.8(3) . . ? C13 C14 C18 125.0(3) . . ? C14 C15 C16 109.8(2) . . ? C14 C15 C19 127.4(3) . . ? C16 C15 C19 122.7(2) . . ? C17 C16 C15 109.0(2) . . ? C17 C16 C20 128.1(3) . . ? C15 C16 C20 122.9(2) . . ? C16 C17 C13 108.2(2) . . ? C16 C17 C21 127.5(3) . . ? C13 C17 C21 124.3(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.583 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.069 #========================================================================== data_compound2c _database_code_depnum_ccdc_archive 'CCDC 225076' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H28 Cl Fe O2 Sb' _chemical_formula_sum 'C21 H28 Cl Fe O2 Sb' _chemical_formula_weight 525.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 Orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 9.5910(13) _cell_length_b 15.1550(13) _cell_length_c 15.256(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2217.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 52 _cell_measurement_theta_min 3.65 _cell_measurement_theta_max 17.73 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 2.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.635751 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; SADABS ; _diffrn_ambient_temperature 100(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49430 _diffrn_reflns_av_R_equivalents 0.0717 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2647 _reflns_number_gt 1989 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD ' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EVALCCD (Duisenberg, 1998, Thesis. Utrecht Un' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0248P)^2^+4.5207P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2647 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.64314(3) 0.23043(2) 0.44578(2) 0.01949(16) Uani 0.50 1 d P A -1 Cl1 Cl 0.57745(14) 0.37350(10) 0.38336(9) 0.0226(3) Uani 0.50 1 d P A -1 Fe1 Fe 0.90246(6) 0.2500 0.46380(3) 0.01680(14) Uani 1 2 d S . . O1 O 0.9003(3) 0.1029(2) 0.5839(2) 0.0851(13) Uani 1 1 d . . . C1 C 0.9178(4) 0.2500 0.3238(2) 0.0221(9) Uani 1 2 d S . . C2 C 0.9829(3) 0.1735(2) 0.35982(18) 0.0226(6) Uani 1 1 d . . . C3 C 1.0935(3) 0.2030(2) 0.41656(18) 0.0217(6) Uani 1 1 d . . . C4 C 0.8115(5) 0.2500 0.2518(3) 0.0285(10) Uani 1 2 d S . . H4A H 0.8589 0.2500 0.1949 0.043 Uiso 1 2 calc SR A . H4B H 0.7530 0.3028 0.2567 0.043 Uiso 0.50 1 calc PR . . H4C H 0.7530 0.1972 0.2567 0.043 Uiso 0.50 1 calc PR . . C5 C 0.9510(4) 0.0802(2) 0.3364(2) 0.0362(8) Uani 1 1 d . . . H5A H 0.8519 0.0748 0.3215 0.054 Uiso 1 1 calc R A . H5B H 0.9723 0.0418 0.3864 0.054 Uiso 1 1 calc R . . H5C H 1.0077 0.0625 0.2859 0.054 Uiso 1 1 calc R . . C6 C 1.1966(3) 0.1446(2) 0.4620(2) 0.0294(7) Uani 1 1 d . . . H6A H 1.2784 0.1363 0.4244 0.044 Uiso 1 1 calc R A . H6B H 1.1535 0.0872 0.4740 0.044 Uiso 1 1 calc R . . H6C H 1.2253 0.1720 0.5173 0.044 Uiso 1 1 calc R . . C7 C 0.8927(4) 0.1630(2) 0.5389(2) 0.0386(9) Uani 1 1 d . A . C8 C 0.5407(4) 0.2500 0.5747(3) 0.0230(9) Uani 1 2 d S . . H8 H 0.4370 0.2500 0.5681 0.028 Uiso 1 2 calc SR A . C9 C 0.5872(3) 0.1721(2) 0.62646(19) 0.0280(7) Uani 1 1 d . A . C10 C 0.6594(3) 0.2018(2) 0.6963(2) 0.0324(8) Uani 1 1 d . . . C11 C 0.5527(4) 0.0787(2) 0.6033(2) 0.0387(8) Uani 1 1 d . . . H11A H 0.6012 0.0624 0.5492 0.058 Uiso 1 1 calc R A . H11B H 0.4518 0.0731 0.5947 0.058 Uiso 1 1 calc R . . H11C H 0.5824 0.0396 0.6509 0.058 Uiso 1 1 calc R . . C12 C 0.7314(4) 0.1476(3) 0.7659(2) 0.0525(11) Uani 1 1 d . A . H12A H 0.6854 0.1571 0.8225 0.079 Uiso 1 1 calc R . . H12B H 0.8293 0.1656 0.7701 0.079 Uiso 1 1 calc R . . H12C H 0.7263 0.0849 0.7504 0.079 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 Sb1 0.01649(16) 0.0246(4) 0.01737(16) -0.00216(14) -0.00206(12) -0.00108(14) Cl1 0.0188(6) 0.0289(7) 0.0200(6) 0.0039(6) -0.0011(5) 0.0096(6) Fe1 0.0152(3) 0.0205(3) 0.0147(3) 0.000 -0.0003(2) 0.000 O1 0.068(2) 0.084(2) 0.104(3) 0.074(2) 0.0579(19) 0.0492(19) C1 0.021(2) 0.033(2) 0.0125(18) 0.000 0.0004(16) 0.000 C2 0.0216(14) 0.0310(17) 0.0153(13) -0.0040(12) 0.0027(11) 0.0035(13) C3 0.0155(13) 0.0324(16) 0.0171(13) 0.0000(12) 0.0033(11) 0.0004(13) C4 0.026(2) 0.044(3) 0.0162(19) 0.000 -0.0003(17) 0.000 C5 0.0393(19) 0.0314(19) 0.0379(18) -0.0123(16) -0.0046(15) 0.0054(15) C6 0.0216(15) 0.0400(19) 0.0267(16) 0.0040(15) 0.0013(12) 0.0080(13) C7 0.0311(17) 0.042(2) 0.043(2) 0.0196(18) 0.0182(15) 0.0170(16) C8 0.0130(18) 0.036(2) 0.020(2) 0.000 -0.0002(15) 0.000 C9 0.0209(14) 0.0405(19) 0.0225(15) 0.0081(14) 0.0051(12) -0.0009(14) C10 0.0172(15) 0.056(2) 0.0239(15) 0.0075(15) 0.0050(12) -0.0001(14) C11 0.0382(19) 0.041(2) 0.0370(19) 0.0127(17) 0.0030(15) -0.0031(16) C12 0.040(2) 0.089(3) 0.0288(19) 0.020(2) -0.0037(16) 0.003(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 Sb1 C8 2.218(4) . ? Sb1 Cl1 2.4505(14) . ? Sb1 Fe1 2.5198(7) . ? Fe1 C7 1.749(3) 8_565 ? Fe1 C7 1.750(3) . ? Fe1 C3 2.094(3) 8_565 ? Fe1 C3 2.094(3) . ? Fe1 C2 2.111(3) . ? Fe1 C2 2.111(3) 8_565 ? Fe1 C1 2.141(4) . ? Fe1 Sb1 2.5198(7) 8_565 ? O1 C7 1.142(4) . ? C1 C2 1.428(4) . ? C1 C2 1.428(4) 8_565 ? C1 C4 1.499(6) . ? C2 C3 1.440(4) . ? C2 C5 1.490(4) . ? C3 C3 1.424(6) 8_565 ? C3 C6 1.497(4) . ? C8 C9 1.489(4) . ? C8 C9 1.489(4) 8_565 ? C8 Sb1 2.218(4) 8_565 ? C9 C10 1.348(4) . ? C9 C11 1.495(5) . ? C10 C10 1.462(7) 8_565 ? C10 C12 1.510(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 C8 Sb1 Cl1 96.45(6) . . ? C8 Sb1 Fe1 108.95(10) . . ? Cl1 Sb1 Fe1 101.07(4) . . ? C7 Fe1 C7 97.8(3) 8_565 . ? C7 Fe1 C3 90.93(13) 8_565 8_565 ? C7 Fe1 C3 121.92(14) . 8_565 ? C7 Fe1 C3 121.92(14) 8_565 . ? C7 Fe1 C3 90.93(13) . . ? C3 Fe1 C3 39.76(16) 8_565 . ? C7 Fe1 C2 157.80(13) 8_565 . ? C7 Fe1 C2 95.62(14) . . ? C3 Fe1 C2 66.94(11) 8_565 . ? C3 Fe1 C2 40.06(11) . . ? C7 Fe1 C2 95.62(14) 8_565 8_565 ? C7 Fe1 C2 157.81(13) . 8_565 ? C3 Fe1 C2 40.06(11) 8_565 8_565 ? C3 Fe1 C2 66.94(11) . 8_565 ? C2 Fe1 C2 66.65(17) . 8_565 ? C7 Fe1 C1 131.09(13) 8_565 . ? C7 Fe1 C1 131.09(13) . . ? C3 Fe1 C1 66.20(13) 8_565 . ? C3 Fe1 C1 66.20(13) . . ? C2 Fe1 C1 39.22(10) . . ? C2 Fe1 C1 39.22(10) 8_565 . ? C7 Fe1 Sb1 96.15(11) 8_565 . ? C7 Fe1 Sb1 85.97(12) . . ? C3 Fe1 Sb1 150.03(8) 8_565 . ? C3 Fe1 Sb1 141.84(8) . . ? C2 Fe1 Sb1 102.37(8) . . ? C2 Fe1 Sb1 110.09(8) 8_565 . ? C1 Fe1 Sb1 87.65(11) . . ? C7 Fe1 Sb1 85.97(12) 8_565 8_565 ? C7 Fe1 Sb1 96.15(11) . 8_565 ? C3 Fe1 Sb1 141.84(8) 8_565 8_565 ? C3 Fe1 Sb1 150.03(8) . 8_565 ? C2 Fe1 Sb1 110.10(8) . 8_565 ? C2 Fe1 Sb1 102.37(8) 8_565 8_565 ? C1 Fe1 Sb1 87.65(11) . 8_565 ? Sb1 Fe1 Sb1 13.519(17) . 8_565 ? C2 C1 C2 108.7(3) . 8_565 ? C2 C1 C4 125.45(17) . . ? C2 C1 C4 125.45(17) 8_565 . ? C2 C1 Fe1 69.26(18) . . ? C2 C1 Fe1 69.26(18) 8_565 . ? C4 C1 Fe1 133.2(3) . . ? C1 C2 C3 107.5(3) . . ? C1 C2 C5 126.1(3) . . ? C3 C2 C5 126.2(3) . . ? C1 C2 Fe1 71.52(19) . . ? C3 C2 Fe1 69.32(16) . . ? C5 C2 Fe1 128.8(2) . . ? C3 C3 C2 108.11(17) 8_565 . ? C3 C3 C6 126.26(18) 8_565 . ? C2 C3 C6 125.5(3) . . ? C3 C3 Fe1 70.12(8) 8_565 . ? C2 C3 Fe1 70.62(16) . . ? C6 C3 Fe1 128.3(2) . . ? O1 C7 Fe1 172.2(3) . . ? C9 C8 C9 104.9(4) . 8_565 ? C9 C8 Sb1 116.4(2) . 8_565 ? C9 C8 Sb1 103.42(19) 8_565 8_565 ? C9 C8 Sb1 103.42(19) . . ? C9 C8 Sb1 116.4(2) 8_565 . ? Sb1 C8 Sb1 15.37(3) 8_565 . ? C10 C9 C8 108.0(3) . . ? C10 C9 C11 128.0(3) . . ? C8 C9 C11 124.0(3) . . ? C9 C10 C10 109.5(2) . 8_565 ? C9 C10 C12 127.6(4) . . ? C10 C10 C12 122.9(2) 8_565 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.680 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.102 #======================================================= data_compound5b _database_code_depnum_ccdc_archive 'CCDC 225077' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 As Cl Fe O2 Si' _chemical_formula_sum 'C36 H48 As Cl Fe O2 Si' _chemical_formula_weight 707.05 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' As As 0.0499 2.0058 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 11.02200(10) _cell_length_b 11.2850(2) _cell_length_c 14.8930(2) _cell_angle_alpha 79.9290(7) _cell_angle_beta 77.8490(7) _cell_angle_gamma 76.9570(6) _cell_volume 1748.37(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7682 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 1.511 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6948 _exptl_absorpt_correction_T_max 0.7833 _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 100(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43827 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7820 _reflns_number_gt 6764 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD ' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0405P)^2^+0.6773P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7820 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 As1 As 0.856525(15) 0.676378(15) 0.362082(11) 0.01940(6) Uani 1 1 d . . . Fe1 Fe 0.76258(2) 0.54910(2) 0.297162(16) 0.02098(7) Uani 1 1 d . . . Cl1 Cl 0.70951(4) 0.74531(4) 0.48251(3) 0.02737(10) Uani 1 1 d . . . Si1 Si 0.90425(4) 0.95652(4) 0.34194(3) 0.02228(11) Uani 1 1 d . . . O1 O 0.77748(16) 0.65716(13) 0.10389(9) 0.0403(4) Uani 1 1 d . . . O2 O 0.51263(12) 0.69071(12) 0.36028(10) 0.0332(3) Uani 1 1 d . . . C1 C 0.79472(16) 0.40060(15) 0.40269(12) 0.0227(3) Uani 1 1 d . . . C2 C 0.70039(17) 0.38417(15) 0.35544(12) 0.0228(3) Uani 1 1 d . . . C3 C 0.75563(17) 0.37842(16) 0.26039(12) 0.0240(4) Uani 1 1 d . . . C4 C 0.88545(17) 0.39103(16) 0.24903(13) 0.0257(4) Uani 1 1 d . . . C5 C 0.90995(17) 0.40091(16) 0.33712(13) 0.0257(4) Uani 1 1 d . . . C6 C 0.77527(19) 0.40380(17) 0.50559(12) 0.0287(4) Uani 1 1 d . . . H6A H 0.7032 0.4691 0.5234 0.043 Uiso 1 1 calc R . . H6B H 0.8516 0.4198 0.5213 0.043 Uiso 1 1 calc R . . H6C H 0.7584 0.3246 0.5390 0.043 Uiso 1 1 calc R . . C7 C 0.56889(17) 0.36799(17) 0.40064(13) 0.0268(4) Uani 1 1 d . . . H7A H 0.5131 0.3927 0.3546 0.040 Uiso 1 1 calc R . . H7B H 0.5376 0.4191 0.4507 0.040 Uiso 1 1 calc R . . H7C H 0.5702 0.2816 0.4261 0.040 Uiso 1 1 calc R . . C8 C 0.69331(19) 0.35450(18) 0.18705(13) 0.0306(4) Uani 1 1 d . . . H8A H 0.7079 0.2659 0.1855 0.046 Uiso 1 1 calc R . . H8B H 0.7291 0.3948 0.1266 0.046 Uiso 1 1 calc R . . H8C H 0.6021 0.3871 0.2010 0.046 Uiso 1 1 calc R . . C9 C 0.98131(19) 0.38670(19) 0.16047(14) 0.0350(4) Uani 1 1 d . . . H9A H 1.0346 0.4469 0.1563 0.052 Uiso 1 1 calc R . . H9B H 0.9373 0.4060 0.1074 0.052 Uiso 1 1 calc R . . H9C H 1.0343 0.3044 0.1602 0.052 Uiso 1 1 calc R . . C10 C 1.03747(18) 0.40101(18) 0.35780(15) 0.0320(4) Uani 1 1 d . . . H10A H 1.0838 0.3163 0.3684 0.048 Uiso 1 1 calc R . . H10B H 1.0267 0.4405 0.4133 0.048 Uiso 1 1 calc R . . H10C H 1.0852 0.4463 0.3052 0.048 Uiso 1 1 calc R . . C11 C 0.77421(19) 0.62386(17) 0.18160(13) 0.0286(4) Uani 1 1 d . . . C12 C 0.61271(18) 0.63756(16) 0.33505(13) 0.0259(4) Uani 1 1 d . . . C13 C 0.86309(15) 0.83743(15) 0.28143(11) 0.0187(3) Uani 1 1 d . . . C14 C 0.97372(16) 0.80306(15) 0.20447(11) 0.0206(3) Uani 1 1 d . . . C15 C 1.09498(16) 0.73497(15) 0.21075(11) 0.0216(3) Uani 1 1 d . . . H15 H 1.1168 0.7031 0.2699 0.026 Uiso 1 1 calc R . . C16 C 1.18454(17) 0.71329(16) 0.13073(12) 0.0249(4) Uani 1 1 d . . . C17 C 1.14900(18) 0.76415(18) 0.04487(12) 0.0305(4) Uani 1 1 d . . . H17 H 1.2096 0.7520 -0.0101 0.037 Uiso 1 1 calc R . . C18 C 1.02908(18) 0.83136(18) 0.03726(12) 0.0290(4) Uani 1 1 d . . . H18 H 1.0078 0.8642 -0.0219 0.035 Uiso 1 1 calc R . . C19 C 0.93975(16) 0.85021(16) 0.11775(12) 0.0226(3) Uani 1 1 d . . . C20 C 0.80668(16) 0.91134(16) 0.13229(12) 0.0225(3) Uani 1 1 d . . . C21 C 0.72712(17) 0.97028(17) 0.07027(12) 0.0273(4) Uani 1 1 d . . . H21 H 0.7587 0.9788 0.0055 0.033 Uiso 1 1 calc R . . C22 C 0.60064(18) 1.01674(17) 0.10386(13) 0.0270(4) Uani 1 1 d . . . H22 H 0.5464 1.0563 0.0611 0.032 Uiso 1 1 calc R . . C23 C 0.55116(16) 1.00681(16) 0.19904(12) 0.0231(3) Uani 1 1 d . A . C24 C 0.63239(16) 0.94670(15) 0.26091(12) 0.0213(3) Uani 1 1 d . . . H24 H 0.6007 0.9381 0.3257 0.026 Uiso 1 1 calc R . . C25 C 0.75883(16) 0.89954(15) 0.22831(11) 0.0200(3) Uani 1 1 d . . . C26 C 1.31764(17) 0.63467(18) 0.13452(13) 0.0283(4) Uani 1 1 d . . . C27 C 1.34283(18) 0.5993(2) 0.23379(13) 0.0330(4) Uani 1 1 d . . . H27A H 1.4305 0.5551 0.2328 0.050 Uiso 1 1 calc R . . H27B H 1.2850 0.5464 0.2691 0.050 Uiso 1 1 calc R . . H27C H 1.3292 0.6736 0.2631 0.050 Uiso 1 1 calc R . . C28 C 1.3296(2) 0.5160(2) 0.09313(14) 0.0382(5) Uani 1 1 d . . . H28A H 1.4151 0.4668 0.0933 0.057 Uiso 1 1 calc R . . H28B H 1.3139 0.5368 0.0293 0.057 Uiso 1 1 calc R . . H28C H 1.2675 0.4689 0.1304 0.057 Uiso 1 1 calc R . . C29 C 1.4187(2) 0.7058(2) 0.07859(17) 0.0447(6) Uani 1 1 d . . . H29A H 1.4110 0.7815 0.1049 0.067 Uiso 1 1 calc R . . H29B H 1.4066 0.7263 0.0140 0.067 Uiso 1 1 calc R . . H29C H 1.5030 0.6550 0.0812 0.067 Uiso 1 1 calc R . . C30 C 0.41303(16) 1.06340(17) 0.23549(13) 0.0259(4) Uani 1 1 d . . . C31 C 0.4142(3) 1.1699(3) 0.2867(2) 0.0453(9) Uani 0.750(4) 1 d P A 1 H31A H 0.3271 1.2079 0.3111 0.068 Uiso 0.750(4) 1 calc PR A 1 H31B H 0.4555 1.2312 0.2436 0.068 Uiso 0.750(4) 1 calc PR A 1 H31C H 0.4608 1.1387 0.3380 0.068 Uiso 0.750(4) 1 calc PR A 1 C32 C 0.3366(3) 1.1183(3) 0.1575(2) 0.0438(8) Uani 0.750(4) 1 d P A 1 H32A H 0.2495 1.1531 0.1845 0.066 Uiso 0.750(4) 1 calc PR A 1 H32B H 0.3361 1.0537 0.1213 0.066 Uiso 0.750(4) 1 calc PR A 1 H32C H 0.3755 1.1830 0.1169 0.066 Uiso 0.750(4) 1 calc PR A 1 C33 C 0.3456(3) 0.9699(3) 0.3006(2) 0.0457(9) Uani 0.750(4) 1 d P A 1 H33A H 0.2579 1.0089 0.3228 0.068 Uiso 0.750(4) 1 calc PR A 1 H33B H 0.3890 0.9386 0.3535 0.068 Uiso 0.750(4) 1 calc PR A 1 H33C H 0.3461 0.9018 0.2677 0.068 Uiso 0.750(4) 1 calc PR A 1 C31B C 0.3766(8) 1.0338(8) 0.3452(6) 0.036(2) Uiso 0.250(4) 1 d P A 2 H31D H 0.3985 0.9450 0.3638 0.054 Uiso 0.250(4) 1 calc PR A 2 H31E H 0.2854 1.0624 0.3646 0.054 Uiso 0.250(4) 1 calc PR A 2 H31F H 0.4233 1.0757 0.3747 0.054 Uiso 0.250(4) 1 calc PR A 2 C32B C 0.3811(11) 1.1954(10) 0.2071(8) 0.056(3) Uiso 0.250(4) 1 d P A 2 H32D H 0.2922 1.2261 0.2326 0.085 Uiso 0.250(4) 1 calc PR A 2 H32E H 0.3944 1.2121 0.1393 0.085 Uiso 0.250(4) 1 calc PR A 2 H32F H 0.4352 1.2366 0.2303 0.085 Uiso 0.250(4) 1 calc PR A 2 C33B C 0.3316(10) 0.9897(10) 0.2007(7) 0.051(3) Uiso 0.250(4) 1 d P A 2 H33D H 0.3579 0.9019 0.2209 0.077 Uiso 0.250(4) 1 calc PR A 2 H33E H 0.3439 1.0046 0.1328 0.077 Uiso 0.250(4) 1 calc PR A 2 H33F H 0.2420 1.0166 0.2264 0.077 Uiso 0.250(4) 1 calc PR A 2 C34 C 1.02247(19) 0.88056(19) 0.41792(14) 0.0343(4) Uani 1 1 d . . . H34A H 1.0948 0.8307 0.3821 0.052 Uiso 1 1 calc R . . H34B H 0.9831 0.8279 0.4702 0.052 Uiso 1 1 calc R . . H34C H 1.0515 0.9433 0.4413 0.052 Uiso 1 1 calc R . . C35 C 0.9768(2) 1.06603(18) 0.24838(15) 0.0343(4) Uani 1 1 d . . . H35A H 0.9982 1.1295 0.2761 0.051 Uiso 1 1 calc R . . H35B H 0.9164 1.1044 0.2069 0.051 Uiso 1 1 calc R . . H35C H 1.0537 1.0216 0.2130 0.051 Uiso 1 1 calc R . . C36 C 0.76361(18) 1.04851(18) 0.40975(14) 0.0313(4) Uani 1 1 d . . . H36A H 0.7226 0.9939 0.4597 0.047 Uiso 1 1 calc R . . H36B H 0.7036 1.0903 0.3688 0.047 Uiso 1 1 calc R . . H36C H 0.7907 1.1096 0.4364 0.047 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 As1 0.02162(9) 0.01791(9) 0.01849(9) -0.00154(6) -0.00445(7) -0.00336(7) Fe1 0.02397(13) 0.01715(12) 0.02223(13) -0.00265(9) -0.00613(10) -0.00300(10) Cl1 0.0300(2) 0.0309(2) 0.0211(2) -0.00627(17) 0.00134(17) -0.00894(18) Si1 0.0227(2) 0.0186(2) 0.0257(2) -0.00475(19) -0.00550(19) -0.00193(18) O1 0.0673(11) 0.0320(8) 0.0255(7) -0.0013(6) -0.0153(7) -0.0130(7) O2 0.0256(7) 0.0279(7) 0.0457(8) -0.0069(6) -0.0085(6) -0.0012(6) C1 0.0255(9) 0.0152(7) 0.0269(9) -0.0012(7) -0.0080(7) -0.0011(6) C2 0.0258(9) 0.0158(8) 0.0253(9) -0.0017(7) -0.0038(7) -0.0024(7) C3 0.0265(9) 0.0179(8) 0.0276(9) -0.0055(7) -0.0048(7) -0.0025(7) C4 0.0275(9) 0.0184(8) 0.0290(9) -0.0043(7) -0.0008(7) -0.0032(7) C5 0.0265(9) 0.0167(8) 0.0327(9) -0.0028(7) -0.0052(7) -0.0026(7) C6 0.0347(10) 0.0251(9) 0.0260(9) -0.0004(7) -0.0104(8) -0.0031(8) C7 0.0257(9) 0.0227(9) 0.0310(9) -0.0046(7) -0.0017(7) -0.0048(7) C8 0.0368(10) 0.0272(9) 0.0302(9) -0.0085(8) -0.0078(8) -0.0057(8) C9 0.0338(10) 0.0292(10) 0.0370(11) -0.0052(8) 0.0041(8) -0.0053(8) C10 0.0251(9) 0.0248(9) 0.0454(11) -0.0031(8) -0.0108(8) -0.0009(7) C11 0.0377(10) 0.0203(8) 0.0307(10) -0.0065(7) -0.0087(8) -0.0065(8) C12 0.0305(10) 0.0203(8) 0.0300(9) -0.0007(7) -0.0117(8) -0.0072(7) C13 0.0212(8) 0.0157(7) 0.0169(7) -0.0014(6) -0.0013(6) -0.0011(6) C14 0.0214(8) 0.0194(8) 0.0199(8) -0.0036(6) -0.0013(6) -0.0032(6) C15 0.0231(8) 0.0213(8) 0.0190(8) -0.0020(6) -0.0036(6) -0.0024(7) C16 0.0230(8) 0.0240(9) 0.0241(9) -0.0039(7) -0.0014(7) 0.0005(7) C17 0.0300(10) 0.0346(10) 0.0203(9) -0.0047(8) 0.0026(7) 0.0014(8) C18 0.0319(10) 0.0325(10) 0.0175(8) -0.0012(7) -0.0026(7) 0.0010(8) C19 0.0233(8) 0.0217(8) 0.0205(8) -0.0020(7) -0.0027(7) -0.0012(7) C20 0.0234(8) 0.0208(8) 0.0221(8) -0.0022(7) -0.0034(7) -0.0027(7) C21 0.0282(9) 0.0303(9) 0.0212(8) -0.0003(7) -0.0061(7) -0.0020(8) C22 0.0291(9) 0.0259(9) 0.0259(9) 0.0003(7) -0.0102(7) -0.0029(7) C23 0.0212(8) 0.0191(8) 0.0294(9) -0.0029(7) -0.0054(7) -0.0042(7) C24 0.0211(8) 0.0198(8) 0.0226(8) -0.0033(7) -0.0026(6) -0.0041(6) C25 0.0229(8) 0.0163(8) 0.0207(8) -0.0018(6) -0.0053(7) -0.0030(6) C26 0.0224(9) 0.0297(9) 0.0271(9) -0.0047(8) -0.0007(7) 0.0037(7) C27 0.0243(9) 0.0397(11) 0.0316(10) -0.0081(8) -0.0072(8) 0.0056(8) C28 0.0377(11) 0.0376(11) 0.0341(10) -0.0123(9) -0.0088(9) 0.0115(9) C29 0.0265(10) 0.0444(13) 0.0509(14) 0.0049(11) 0.0045(9) -0.0012(9) C30 0.0187(8) 0.0267(9) 0.0323(10) -0.0054(8) -0.0072(7) -0.0011(7) C31 0.0261(14) 0.0450(17) 0.069(2) -0.0345(16) -0.0063(13) 0.0030(12) C32 0.0248(13) 0.062(2) 0.0401(16) -0.0075(14) -0.0128(12) 0.0078(13) C33 0.0229(13) 0.0391(16) 0.064(2) 0.0087(15) 0.0021(13) -0.0045(12) C34 0.0359(11) 0.0309(10) 0.0401(11) -0.0112(9) -0.0173(9) 0.0001(8) C35 0.0382(11) 0.0255(10) 0.0393(11) -0.0041(8) -0.0024(9) -0.0108(8) C36 0.0316(10) 0.0261(9) 0.0371(10) -0.0135(8) -0.0039(8) -0.0025(8) _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 As1 C13 2.0026(16) . ? As1 Cl1 2.2678(4) . ? As1 Fe1 2.3766(3) . ? Fe1 C12 1.7617(19) . ? Fe1 C11 1.7716(19) . ? Fe1 C2 2.1091(17) . ? Fe1 C1 2.1093(17) . ? Fe1 C3 2.1141(17) . ? Fe1 C4 2.1162(18) . ? Fe1 C5 2.1499(18) . ? Si1 C36 1.8659(19) . ? Si1 C35 1.866(2) . ? Si1 C34 1.868(2) . ? Si1 C13 1.9222(17) . ? O1 C11 1.148(2) . ? O2 C12 1.150(2) . ? C1 C5 1.430(3) . ? C1 C2 1.432(2) . ? C1 C6 1.508(2) . ? C2 C3 1.425(2) . ? C2 C7 1.501(2) . ? C3 C4 1.441(3) . ? C3 C8 1.497(3) . ? C4 C5 1.421(3) . ? C4 C9 1.507(3) . ? C5 C10 1.501(3) . ? C13 C25 1.504(2) . ? C13 C14 1.518(2) . ? C14 C15 1.396(2) . ? C14 C19 1.402(2) . ? C15 C16 1.397(2) . ? C16 C17 1.404(3) . ? C16 C26 1.540(2) . ? C17 C18 1.384(3) . ? C18 C19 1.396(2) . ? C19 C20 1.462(2) . ? C20 C21 1.388(2) . ? C20 C25 1.410(2) . ? C21 C22 1.392(3) . ? C22 C23 1.402(3) . ? C23 C24 1.402(2) . ? C23 C30 1.535(2) . ? C24 C25 1.390(2) . ? C26 C27 1.529(3) . ? C26 C29 1.535(3) . ? C26 C28 1.538(3) . ? C30 C32B 1.458(11) . ? C30 C33 1.516(3) . ? C30 C31 1.536(3) . ? C30 C32 1.539(3) . ? C30 C33B 1.565(11) . ? C30 C31B 1.592(8) . ? 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 C13 As1 Cl1 98.43(5) . . ? C13 As1 Fe1 111.33(5) . . ? Cl1 As1 Fe1 105.861(14) . . ? C12 Fe1 C11 94.23(9) . . ? C12 Fe1 C2 91.72(7) . . ? C11 Fe1 C2 129.49(8) . . ? C12 Fe1 C1 106.61(8) . . ? C11 Fe1 C1 155.63(8) . . ? C2 Fe1 C1 39.69(7) . . ? C12 Fe1 C3 113.90(8) . . ? C11 Fe1 C3 93.84(7) . . ? C2 Fe1 C3 39.44(7) . . ? C1 Fe1 C3 66.47(7) . . ? C12 Fe1 C4 153.73(8) . . ? C11 Fe1 C4 89.54(8) . . ? C2 Fe1 C4 66.35(7) . . ? C1 Fe1 C4 66.19(7) . . ? C3 Fe1 C4 39.85(7) . . ? C12 Fe1 C5 145.00(8) . . ? C11 Fe1 C5 120.75(8) . . ? C2 Fe1 C5 65.84(7) . . ? C1 Fe1 C5 39.23(7) . . ? C3 Fe1 C5 65.89(7) . . ? C4 Fe1 C5 38.91(7) . . ? C12 Fe1 As1 89.13(6) . . ? C11 Fe1 As1 99.84(6) . . ? C2 Fe1 As1 130.39(5) . . ? C1 Fe1 As1 93.10(5) . . ? C3 Fe1 As1 152.30(5) . . ? C4 Fe1 As1 115.85(5) . . ? C5 Fe1 As1 86.43(5) . . ? C36 Si1 C35 107.01(9) . . ? C36 Si1 C34 110.13(9) . . ? C35 Si1 C34 108.82(10) . . ? C36 Si1 C13 113.70(8) . . ? C35 Si1 C13 106.56(8) . . ? C34 Si1 C13 110.41(8) . . ? C5 C1 C2 107.95(15) . . ? C5 C1 C6 127.40(17) . . ? C2 C1 C6 124.39(16) . . ? C5 C1 Fe1 71.92(10) . . ? C2 C1 Fe1 70.14(10) . . ? C6 C1 Fe1 128.05(12) . . ? C3 C2 C1 108.23(15) . . ? C3 C2 C7 126.49(16) . . ? C1 C2 C7 125.18(16) . . ? C3 C2 Fe1 70.47(10) . . ? C1 C2 Fe1 70.16(10) . . ? C7 C2 Fe1 127.93(12) . . ? C2 C3 C4 107.53(16) . . ? C2 C3 C8 126.29(16) . . ? C4 C3 C8 126.04(16) . . ? C2 C3 Fe1 70.09(10) . . ? C4 C3 Fe1 70.16(10) . . ? C8 C3 Fe1 128.38(13) . . ? C5 C4 C3 108.20(15) . . ? C5 C4 C9 125.60(17) . . ? C3 C4 C9 126.10(17) . . ? C5 C4 Fe1 71.83(10) . . ? C3 C4 Fe1 70.00(10) . . ? C9 C4 Fe1 126.69(13) . . ? C4 C5 C1 108.01(16) . . ? C4 C5 C10 125.24(17) . . ? C1 C5 C10 126.57(17) . . ? C4 C5 Fe1 69.26(10) . . ? C1 C5 Fe1 68.85(10) . . ? C10 C5 Fe1 131.20(13) . . ? O1 C11 Fe1 169.99(16) . . ? O2 C12 Fe1 176.96(16) . . ? C25 C13 C14 102.27(13) . . ? C25 C13 Si1 108.93(11) . . ? C14 C13 Si1 107.54(11) . . ? C25 C13 As1 121.21(11) . . ? C14 C13 As1 102.25(10) . . ? Si1 C13 As1 113.00(8) . . ? C15 C14 C19 120.49(15) . . ? C15 C14 C13 129.26(15) . . ? C19 C14 C13 110.25(14) . . ? C14 C15 C16 120.54(15) . . ? C15 C16 C17 117.77(16) . . ? C15 C16 C26 122.16(16) . . ? C17 C16 C26 120.06(15) . . ? C18 C17 C16 122.50(16) . . ? C17 C18 C19 119.09(17) . . ? C18 C19 C14 119.58(16) . . ? C18 C19 C20 131.96(16) . . ? C14 C19 C20 108.45(14) . . ? C21 C20 C25 119.81(16) . . ? C21 C20 C19 131.61(16) . . ? C25 C20 C19 108.54(15) . . ? C20 C21 C22 119.40(16) . . ? C21 C22 C23 121.80(17) . . ? C24 C23 C22 118.23(16) . . ? C24 C23 C30 120.39(15) . . ? C22 C23 C30 121.35(16) . . ? C25 C24 C23 120.57(15) . . ? C24 C25 C20 120.18(15) . . ? C24 C25 C13 129.58(15) . . ? C20 C25 C13 110.19(14) . . ? C27 C26 C29 108.10(17) . . ? C27 C26 C28 108.18(16) . . ? C29 C26 C28 109.44(17) . . ? C27 C26 C16 112.04(14) . . ? C29 C26 C16 110.05(16) . . ? C28 C26 C16 108.99(16) . . ? C32B C30 C33 134.9(5) . . ? C32B C30 C23 113.3(5) . . ? C33 C30 C23 111.50(17) . . ? C32B C30 C31 50.5(5) . . ? C33 C30 C31 110.0(2) . . ? C23 C30 C31 107.46(16) . . ? C32B C30 C32 57.9(5) . . ? C33 C30 C32 108.2(2) . . ? C23 C30 C32 112.88(17) . . ? C31 C30 C32 106.7(2) . . ? C32B C30 C33B 113.0(6) . . ? C33 C30 C33B 58.3(4) . . ? C23 C30 C33B 105.4(4) . . ? C31 C30 C33B 147.1(4) . . ? C32 C30 C33B 57.3(4) . . ? C32B C30 C31B 109.9(6) . . ? C33 C30 C31B 45.5(3) . . ? C23 C30 C31B 112.2(3) . . ? C31 C30 C31B 66.7(3) . . ? C32 C30 C31B 134.1(4) . . ? C33B C30 C31B 102.5(5) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.556 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.058 #============================================================== data_compound7c _database_code_depnum_ccdc_archive 'CCDC 225078' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H65 Fe O2 Sb' _chemical_formula_sum 'C54 H65 Fe O2 Sb' _chemical_formula_weight 923.66 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' Fe Fe 0.3463 0.8444 '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' 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 10.34100(10) _cell_length_b 15.21400(10) _cell_length_c 16.2210(2) _cell_angle_alpha 89.8230(5) _cell_angle_beta 73.7590(4) _cell_angle_gamma 72.1330(5) _cell_volume 2322.43(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13518 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 0.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8883 _exptl_absorpt_correction_T_max 0.9125 _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 100(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95916 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 30.00 _reflns_number_total 13551 _reflns_number_gt 12003 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD ' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0443P)^2^+2.3569P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13551 _refine_ls_number_parameters 540 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Sb1 Sb 0.574687(12) 0.380664(8) 0.171543(7) 0.01406(4) Uani 1 1 d . . . Fe1 Fe 0.74101(3) 0.261474(18) 0.045251(17) 0.01618(6) Uani 1 1 d . . . O1 O 0.49151(19) 0.24971(14) 0.00244(11) 0.0366(4) Uani 1 1 d . . . O2 O 0.78085(18) 0.10336(11) 0.14790(10) 0.0293(3) Uani 1 1 d . . . C1 C 0.8497(2) 0.24532(15) -0.08669(13) 0.0220(4) Uani 1 1 d . . . C2 C 0.9464(2) 0.20163(15) -0.04090(13) 0.0236(4) Uani 1 1 d . . . C3 C 0.9505(2) 0.27045(16) 0.01748(13) 0.0234(4) Uani 1 1 d . . . C4 C 0.8583(2) 0.35764(14) 0.00587(13) 0.0218(4) Uani 1 1 d . . . C5 C 0.7928(2) 0.34213(14) -0.05698(13) 0.0208(4) Uani 1 1 d . . . C6 C 0.8195(3) 0.19958(18) -0.15786(14) 0.0324(5) Uani 1 1 d . . . H6A H 0.8918 0.1976 -0.2124 0.049 Uiso 1 1 calc R . . H6B H 0.7255 0.2350 -0.1625 0.049 Uiso 1 1 calc R . . H6C H 0.8214 0.1363 -0.1451 0.049 Uiso 1 1 calc R . . C7 C 1.0374(3) 0.10167(17) -0.05565(18) 0.0391(6) Uani 1 1 d . . . H7A H 0.9865 0.0638 -0.0732 0.059 Uiso 1 1 calc R . . H7B H 1.0590 0.0813 -0.0022 0.059 Uiso 1 1 calc R . . H7C H 1.1261 0.0947 -0.1012 0.059 Uiso 1 1 calc R . . C8 C 1.0520(2) 0.2536(2) 0.07079(16) 0.0395(6) Uani 1 1 d . . . H8A H 1.0500 0.1982 0.1014 0.059 Uiso 1 1 calc R . . H8B H 1.0238 0.3073 0.1127 0.059 Uiso 1 1 calc R . . H8C H 1.1483 0.2445 0.0331 0.059 Uiso 1 1 calc R . . C9 C 0.8428(3) 0.45130(17) 0.04409(16) 0.0333(5) Uani 1 1 d . . . H9A H 0.8951 0.4826 0.0005 0.050 Uiso 1 1 calc R . . H9B H 0.8811 0.4440 0.0935 0.050 Uiso 1 1 calc R . . H9C H 0.7420 0.4885 0.0632 0.050 Uiso 1 1 calc R . . C10 C 0.6939(3) 0.41701(17) -0.09133(16) 0.0329(5) Uani 1 1 d . . . H10A H 0.6308 0.4641 -0.0443 0.049 Uiso 1 1 calc R . . H10B H 0.6371 0.3901 -0.1163 0.049 Uiso 1 1 calc R . . H10C H 0.7494 0.4457 -0.1358 0.049 Uiso 1 1 calc R . . C11 C 0.5871(2) 0.25479(15) 0.02328(13) 0.0240(4) Uani 1 1 d . . . C12 C 0.7602(2) 0.16879(14) 0.11160(13) 0.0216(4) Uani 1 1 d . . . C13 C 0.37059(18) 0.34895(13) 0.22795(12) 0.0153(3) Uani 1 1 d . . . H13 H 0.3075 0.3702 0.1901 0.018 Uiso 1 1 calc R . . C14 C 0.30676(18) 0.40902(13) 0.31217(12) 0.0155(3) Uani 1 1 d . . . C15 C 0.28233(19) 0.50362(13) 0.32789(12) 0.0168(3) Uani 1 1 d . . . H15 H 0.2960 0.5405 0.2809 0.020 Uiso 1 1 calc R . . C16 C 0.2379(2) 0.54452(13) 0.41236(12) 0.0185(3) Uani 1 1 d . . . C17 C 0.2155(2) 0.48805(15) 0.48063(13) 0.0223(4) Uani 1 1 d . . . H17 H 0.1848 0.5151 0.5384 0.027 Uiso 1 1 calc R . . C18 C 0.2372(2) 0.39433(14) 0.46573(13) 0.0210(4) Uani 1 1 d . . . H18 H 0.2200 0.3579 0.5127 0.025 Uiso 1 1 calc R . . C19 C 0.28457(19) 0.35375(13) 0.38106(12) 0.0169(3) Uani 1 1 d . . . C20 C 0.31837(19) 0.25839(13) 0.34584(12) 0.0170(3) Uani 1 1 d . . . C21 C 0.3036(2) 0.17936(14) 0.38544(13) 0.0195(4) Uani 1 1 d . . . H21 H 0.2735 0.1810 0.4465 0.023 Uiso 1 1 calc R . . C22 C 0.3334(2) 0.09778(14) 0.33478(13) 0.0200(4) Uani 1 1 d . . . H22 H 0.3231 0.0440 0.3621 0.024 Uiso 1 1 calc R . . C23 C 0.37805(19) 0.09299(13) 0.24443(13) 0.0182(3) Uani 1 1 d . . . C24 C 0.39565(19) 0.17278(13) 0.20524(12) 0.0173(3) Uani 1 1 d . . . H24 H 0.4273 0.1708 0.1442 0.021 Uiso 1 1 calc R . . C25 C 0.36725(18) 0.25452(13) 0.25492(12) 0.0160(3) Uani 1 1 d . . . C26 C 0.2194(2) 0.64665(14) 0.43291(13) 0.0212(4) Uani 1 1 d . . . C27 C 0.2451(2) 0.69795(15) 0.35131(14) 0.0255(4) Uani 1 1 d . . . H27A H 0.1763 0.6964 0.3208 0.038 Uiso 1 1 calc R . . H27B H 0.3417 0.6677 0.3137 0.038 Uiso 1 1 calc R . . H27C H 0.2339 0.7625 0.3674 0.038 Uiso 1 1 calc R . . C28 C 0.3264(2) 0.65120(16) 0.48078(14) 0.0260(4) Uani 1 1 d . . . H28A H 0.4230 0.6181 0.4447 0.039 Uiso 1 1 calc R . . H28B H 0.3069 0.6222 0.5349 0.039 Uiso 1 1 calc R . . H28C H 0.3175 0.7161 0.4932 0.039 Uiso 1 1 calc R . . C29 C 0.0668(2) 0.69644(16) 0.48945(15) 0.0287(4) Uani 1 1 d . . . H29A H 0.0573 0.7605 0.5059 0.043 Uiso 1 1 calc R . . H29B H 0.0459 0.6641 0.5415 0.043 Uiso 1 1 calc R . . H29C H -0.0002 0.6964 0.4570 0.043 Uiso 1 1 calc R . . C30 C 0.4064(2) 0.00469(14) 0.18732(14) 0.0210(4) Uani 1 1 d . . . C31 C 0.3821(3) -0.07523(15) 0.24068(16) 0.0281(4) Uani 1 1 d . . . H31A H 0.2828 -0.0575 0.2763 0.042 Uiso 1 1 calc R . . H31B H 0.4445 -0.0889 0.2780 0.042 Uiso 1 1 calc R . . H31C H 0.4035 -0.1304 0.2019 0.042 Uiso 1 1 calc R . . C32 C 0.3064(2) 0.02509(15) 0.12983(15) 0.0266(4) Uani 1 1 d . . . H32A H 0.3252 -0.0311 0.0931 0.040 Uiso 1 1 calc R . . H32B H 0.3229 0.0745 0.0936 0.040 Uiso 1 1 calc R . . H32C H 0.2074 0.0448 0.1663 0.040 Uiso 1 1 calc R . . C33 C 0.5615(2) -0.02688(16) 0.12976(16) 0.0298(5) Uani 1 1 d . . . H33A H 0.6255 -0.0389 0.1661 0.045 Uiso 1 1 calc R . . H33B H 0.5779 0.0219 0.0926 0.045 Uiso 1 1 calc R . . H33C H 0.5800 -0.0837 0.0940 0.045 Uiso 1 1 calc R . . C34 C 0.64697(18) 0.36212(12) 0.29028(12) 0.0149(3) Uani 1 1 d . . . H34 H 0.5626 0.3853 0.3423 0.018 Uiso 1 1 calc R . . C35 C 0.74124(19) 0.26998(12) 0.30484(12) 0.0151(3) Uani 1 1 d . . . C36 C 0.70795(19) 0.19068(13) 0.33211(12) 0.0165(3) Uani 1 1 d . . . H36 H 0.6151 0.1879 0.3388 0.020 Uiso 1 1 calc R . . C37 C 0.8115(2) 0.11464(13) 0.34978(12) 0.0173(3) Uani 1 1 d . . . C38 C 0.9496(2) 0.11890(13) 0.33508(13) 0.0203(4) Uani 1 1 d . . . H38 H 1.0213 0.0665 0.3439 0.024 Uiso 1 1 calc R . . C39 C 0.9848(2) 0.19784(13) 0.30789(13) 0.0193(4) Uani 1 1 d . . . H39 H 1.0791 0.1992 0.2980 0.023 Uiso 1 1 calc R . . C40 C 0.87887(19) 0.27455(13) 0.29558(12) 0.0163(3) Uani 1 1 d . . . C41 C 0.87761(19) 0.36946(13) 0.28215(12) 0.0162(3) Uani 1 1 d . . . C42 C 0.9819(2) 0.41174(14) 0.27491(13) 0.0200(4) Uani 1 1 d . . . H42 H 1.0753 0.3759 0.2745 0.024 Uiso 1 1 calc R . . C43 C 0.9482(2) 0.50675(14) 0.26825(13) 0.0211(4) Uani 1 1 d . . . H43 H 1.0196 0.5352 0.2634 0.025 Uiso 1 1 calc R . . C44 C 0.8110(2) 0.56195(13) 0.26847(12) 0.0181(3) Uani 1 1 d . . . C45 C 0.70691(19) 0.51842(13) 0.27590(12) 0.0169(3) Uani 1 1 d . . . H45 H 0.6136 0.5542 0.2763 0.020 Uiso 1 1 calc R . . C46 C 0.73949(19) 0.42346(13) 0.28272(12) 0.0153(3) Uani 1 1 d . . . C47 C 0.7690(2) 0.03148(13) 0.38779(13) 0.0210(4) Uani 1 1 d . . . C48 C 0.6504(3) 0.06524(16) 0.47351(15) 0.0295(5) Uani 1 1 d . . . H48A H 0.6844 0.0942 0.5134 0.044 Uiso 1 1 calc R . . H48B H 0.6239 0.0124 0.4988 0.044 Uiso 1 1 calc R . . H48C H 0.5674 0.1106 0.4630 0.044 Uiso 1 1 calc R . . C49 C 0.7140(2) -0.01219(14) 0.32494(15) 0.0266(4) Uani 1 1 d . . . H49A H 0.6343 0.0349 0.3127 0.040 Uiso 1 1 calc R . . H49B H 0.6822 -0.0630 0.3509 0.040 Uiso 1 1 calc R . . H49C H 0.7906 -0.0363 0.2711 0.040 Uiso 1 1 calc R . . C50 C 0.8927(3) -0.04404(16) 0.40559(18) 0.0324(5) Uani 1 1 d . . . H50A H 0.9683 -0.0681 0.3514 0.049 Uiso 1 1 calc R . . H50B H 0.8595 -0.0945 0.4311 0.049 Uiso 1 1 calc R . . H50C H 0.9296 -0.0178 0.4456 0.049 Uiso 1 1 calc R . . C51 C 0.7741(2) 0.66642(13) 0.25842(13) 0.0209(4) Uani 1 1 d . . . C52 C 0.7488(3) 0.68441(16) 0.16978(16) 0.0352(5) Uani 1 1 d . . . H52A H 0.6712 0.6621 0.1656 0.053 Uiso 1 1 calc R . . H52B H 0.8356 0.6515 0.1241 0.053 Uiso 1 1 calc R . . H52C H 0.7233 0.7511 0.1633 0.053 Uiso 1 1 calc R . . C53 C 0.8929(2) 0.70397(15) 0.26471(18) 0.0317(5) Uani 1 1 d . . . H53A H 0.8642 0.7708 0.2592 0.048 Uiso 1 1 calc R . . H53B H 0.9798 0.6728 0.2183 0.048 Uiso 1 1 calc R . . H53C H 0.9107 0.6923 0.3206 0.048 Uiso 1 1 calc R . . C54 C 0.6384(2) 0.72053(14) 0.32961(15) 0.0247(4) Uani 1 1 d . . . H54A H 0.5579 0.7029 0.3232 0.037 Uiso 1 1 calc R . . H54B H 0.6195 0.7872 0.3247 0.037 Uiso 1 1 calc R . . H54C H 0.6514 0.7059 0.3862 0.037 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 Sb1 0.01120(6) 0.01500(6) 0.01590(6) 0.00342(4) -0.00359(4) -0.00440(4) Fe1 0.01404(12) 0.01793(13) 0.01557(12) 0.00277(10) -0.00226(9) -0.00558(10) O1 0.0322(9) 0.0611(12) 0.0281(8) 0.0088(8) -0.0124(7) -0.0280(9) O2 0.0398(9) 0.0210(7) 0.0228(7) 0.0043(6) -0.0051(7) -0.0071(6) C1 0.0206(9) 0.0276(10) 0.0172(9) 0.0025(7) -0.0006(7) -0.0111(8) C2 0.0187(9) 0.0240(9) 0.0205(9) 0.0037(7) 0.0027(7) -0.0037(7) C3 0.0161(8) 0.0339(11) 0.0182(9) 0.0045(8) -0.0021(7) -0.0077(8) C4 0.0180(9) 0.0241(9) 0.0207(9) -0.0004(7) 0.0024(7) -0.0102(7) C5 0.0165(8) 0.0241(9) 0.0198(9) 0.0074(7) -0.0010(7) -0.0077(7) C6 0.0398(13) 0.0419(13) 0.0205(10) 0.0000(9) -0.0033(9) -0.0251(11) C7 0.0307(12) 0.0267(11) 0.0400(14) 0.0071(10) 0.0072(10) 0.0029(9) C8 0.0192(10) 0.0709(19) 0.0274(11) 0.0078(12) -0.0082(9) -0.0117(11) C9 0.0335(12) 0.0333(12) 0.0315(12) -0.0052(9) 0.0059(9) -0.0220(10) C10 0.0266(11) 0.0351(12) 0.0337(12) 0.0159(10) -0.0076(9) -0.0065(9) C11 0.0242(10) 0.0308(10) 0.0178(9) 0.0031(8) -0.0026(7) -0.0133(8) C12 0.0216(9) 0.0212(9) 0.0175(9) -0.0018(7) -0.0003(7) -0.0055(7) C13 0.0103(7) 0.0198(8) 0.0163(8) 0.0014(6) -0.0031(6) -0.0062(6) C14 0.0099(7) 0.0208(8) 0.0162(8) 0.0012(6) -0.0036(6) -0.0056(6) C15 0.0142(8) 0.0203(8) 0.0167(8) 0.0034(7) -0.0050(6) -0.0064(7) C16 0.0145(8) 0.0215(9) 0.0187(8) 0.0001(7) -0.0027(7) -0.0068(7) C17 0.0234(9) 0.0272(10) 0.0164(8) -0.0006(7) -0.0029(7) -0.0106(8) C18 0.0223(9) 0.0251(9) 0.0167(8) 0.0045(7) -0.0040(7) -0.0105(8) C19 0.0129(8) 0.0209(8) 0.0179(8) 0.0034(7) -0.0044(6) -0.0069(7) C20 0.0133(8) 0.0207(8) 0.0182(8) 0.0030(7) -0.0058(6) -0.0060(7) C21 0.0173(8) 0.0225(9) 0.0195(9) 0.0047(7) -0.0064(7) -0.0066(7) C22 0.0169(8) 0.0199(9) 0.0246(9) 0.0060(7) -0.0079(7) -0.0063(7) C23 0.0134(8) 0.0187(8) 0.0225(9) 0.0020(7) -0.0062(7) -0.0043(7) C24 0.0131(8) 0.0203(8) 0.0184(8) 0.0012(7) -0.0039(6) -0.0058(7) C25 0.0106(7) 0.0197(8) 0.0181(8) 0.0022(7) -0.0042(6) -0.0053(6) C26 0.0200(9) 0.0209(9) 0.0210(9) -0.0018(7) -0.0028(7) -0.0073(7) C27 0.0272(10) 0.0226(9) 0.0262(10) 0.0017(8) -0.0061(8) -0.0090(8) C28 0.0276(10) 0.0285(10) 0.0249(10) 0.0002(8) -0.0065(8) -0.0143(9) C29 0.0255(10) 0.0257(10) 0.0292(11) -0.0037(8) -0.0023(9) -0.0052(8) C30 0.0187(9) 0.0186(9) 0.0268(10) 0.0004(7) -0.0085(7) -0.0058(7) C31 0.0332(11) 0.0198(9) 0.0352(12) 0.0038(8) -0.0144(9) -0.0099(8) C32 0.0288(11) 0.0252(10) 0.0304(11) 0.0024(8) -0.0143(9) -0.0099(8) C33 0.0223(10) 0.0268(10) 0.0361(12) -0.0082(9) -0.0031(9) -0.0065(8) C34 0.0122(7) 0.0155(8) 0.0179(8) 0.0013(6) -0.0046(6) -0.0057(6) C35 0.0129(7) 0.0156(8) 0.0163(8) 0.0008(6) -0.0044(6) -0.0039(6) C36 0.0150(8) 0.0182(8) 0.0184(8) 0.0016(6) -0.0062(7) -0.0070(7) C37 0.0187(8) 0.0165(8) 0.0184(8) 0.0022(6) -0.0075(7) -0.0062(7) C38 0.0173(8) 0.0161(8) 0.0263(10) 0.0028(7) -0.0073(7) -0.0030(7) C39 0.0134(8) 0.0200(9) 0.0240(9) 0.0008(7) -0.0053(7) -0.0047(7) C40 0.0136(8) 0.0173(8) 0.0180(8) 0.0012(6) -0.0044(6) -0.0051(6) C41 0.0132(8) 0.0184(8) 0.0178(8) 0.0022(6) -0.0044(6) -0.0064(6) C42 0.0129(8) 0.0222(9) 0.0261(9) 0.0035(7) -0.0058(7) -0.0072(7) C43 0.0171(8) 0.0230(9) 0.0265(10) 0.0039(7) -0.0060(7) -0.0114(7) C44 0.0179(8) 0.0177(8) 0.0199(9) 0.0015(7) -0.0043(7) -0.0085(7) C45 0.0149(8) 0.0177(8) 0.0194(8) 0.0023(7) -0.0057(7) -0.0064(7) C46 0.0143(8) 0.0176(8) 0.0160(8) 0.0016(6) -0.0050(6) -0.0073(6) C47 0.0244(9) 0.0170(8) 0.0250(9) 0.0066(7) -0.0110(8) -0.0081(7) C48 0.0350(12) 0.0284(11) 0.0274(11) 0.0089(8) -0.0070(9) -0.0153(9) C49 0.0331(11) 0.0194(9) 0.0343(11) 0.0053(8) -0.0159(9) -0.0130(8) C50 0.0309(11) 0.0224(10) 0.0490(14) 0.0159(10) -0.0194(11) -0.0087(9) C51 0.0207(9) 0.0171(8) 0.0264(10) 0.0030(7) -0.0050(7) -0.0099(7) C52 0.0547(16) 0.0222(10) 0.0297(12) 0.0085(9) -0.0131(11) -0.0132(10) C53 0.0220(10) 0.0213(10) 0.0511(14) 0.0004(9) -0.0029(10) -0.0129(8) C54 0.0221(9) 0.0184(9) 0.0327(11) 0.0025(8) -0.0067(8) -0.0067(7) _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 Sb1 C34 2.2407(18) . ? Sb1 C13 2.2509(17) . ? Sb1 Fe1 2.5654(3) . ? Fe1 C11 1.757(2) . ? Fe1 C12 1.768(2) . ? Fe1 C1 2.0958(19) . ? Fe1 C5 2.1063(19) . ? Fe1 C2 2.110(2) . ? Fe1 C3 2.133(2) . ? Fe1 C4 2.1608(19) . ? O1 C11 1.154(3) . ? O2 C12 1.149(3) . ? C1 C2 1.413(3) . ? C1 C5 1.436(3) . ? C1 C6 1.501(3) . ? C2 C3 1.432(3) . ? C2 C7 1.501(3) . ? C3 C4 1.424(3) . ? C3 C8 1.502(3) . ? C4 C5 1.428(3) . ? C4 C9 1.500(3) . ? C5 C10 1.501(3) . ? C13 C14 1.507(2) . ? C13 C25 1.508(3) . ? C14 C15 1.394(3) . ? C14 C19 1.406(3) . ? C15 C16 1.398(3) . ? C16 C17 1.411(3) . ? C16 C26 1.532(3) . ? C17 C18 1.385(3) . ? C18 C19 1.397(3) . ? C19 C20 1.461(3) . ? C20 C21 1.391(3) . ? C20 C25 1.414(3) . ? C21 C22 1.393(3) . ? C22 C23 1.403(3) . ? C23 C24 1.406(3) . ? C23 C30 1.537(3) . ? C24 C25 1.390(3) . ? C26 C27 1.535(3) . ? C26 C28 1.536(3) . ? C26 C29 1.539(3) . ? C30 C31 1.533(3) . ? C30 C33 1.539(3) . ? C30 C32 1.542(3) . ? C34 C35 1.503(2) . ? C34 C46 1.511(2) . ? C35 C36 1.391(2) . ? C35 C40 1.412(2) . ? C36 C37 1.406(3) . ? C37 C38 1.403(3) . ? C37 C47 1.536(3) . ? C38 C39 1.394(3) . ? C39 C40 1.392(3) . ? C40 C41 1.456(3) . ? C41 C42 1.395(2) . ? C41 C46 1.410(2) . ? C42 C43 1.391(3) . ? C43 C44 1.408(3) . ? C44 C45 1.406(2) . ? C44 C51 1.536(3) . ? C45 C46 1.391(3) . ? C47 C50 1.531(3) . ? C47 C49 1.537(3) . ? C47 C48 1.538(3) . ? C51 C53 1.532(3) . ? C51 C54 1.540(3) . ? C51 C52 1.541(3) . ? 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 C34 Sb1 C13 96.34(6) . . ? C34 Sb1 Fe1 112.76(5) . . ? C13 Sb1 Fe1 110.93(5) . . ? C11 Fe1 C12 96.87(10) . . ? C11 Fe1 C1 91.15(9) . . ? C12 Fe1 C1 122.81(9) . . ? C11 Fe1 C5 94.93(9) . . ? C12 Fe1 C5 159.41(8) . . ? C1 Fe1 C5 39.96(8) . . ? C11 Fe1 C2 122.63(9) . . ? C12 Fe1 C2 93.20(9) . . ? C1 Fe1 C2 39.27(8) . . ? C5 Fe1 C2 66.21(8) . . ? C11 Fe1 C3 157.04(9) . . ? C12 Fe1 C3 98.33(9) . . ? C1 Fe1 C3 66.12(8) . . ? C5 Fe1 C3 65.85(8) . . ? C2 Fe1 C3 39.45(8) . . ? C11 Fe1 C4 130.02(9) . . ? C12 Fe1 C4 133.06(9) . . ? C1 Fe1 C4 65.92(8) . . ? C5 Fe1 C4 39.08(8) . . ? C2 Fe1 C4 65.48(8) . . ? C3 Fe1 C4 38.73(8) . . ? C11 Fe1 Sb1 86.84(7) . . ? C12 Fe1 Sb1 93.11(6) . . ? C1 Fe1 Sb1 143.97(6) . . ? C5 Fe1 Sb1 104.36(6) . . ? C2 Fe1 Sb1 148.77(6) . . ? C3 Fe1 Sb1 109.33(6) . . ? C4 Fe1 Sb1 88.25(5) . . ? C2 C1 C5 107.86(18) . . ? C2 C1 C6 125.9(2) . . ? C5 C1 C6 126.2(2) . . ? C2 C1 Fe1 70.91(11) . . ? C5 C1 Fe1 70.42(11) . . ? C6 C1 Fe1 127.24(15) . . ? C1 C2 C3 108.34(18) . . ? C1 C2 C7 125.8(2) . . ? C3 C2 C7 125.7(2) . . ? C1 C2 Fe1 69.81(11) . . ? C3 C2 Fe1 71.15(11) . . ? C7 C2 Fe1 128.25(15) . . ? C4 C3 C2 107.96(18) . . ? C4 C3 C8 126.9(2) . . ? C2 C3 C8 124.6(2) . . ? C4 C3 Fe1 71.68(11) . . ? C2 C3 Fe1 69.41(11) . . ? C8 C3 Fe1 131.31(15) . . ? C3 C4 C5 107.81(18) . . ? C3 C4 C9 127.1(2) . . ? C5 C4 C9 124.7(2) . . ? C3 C4 Fe1 69.59(11) . . ? C5 C4 Fe1 68.40(11) . . ? C9 C4 Fe1 132.54(14) . . ? C4 C5 C1 107.97(18) . . ? C4 C5 C10 124.8(2) . . ? C1 C5 C10 127.0(2) . . ? C4 C5 Fe1 72.52(11) . . ? C1 C5 Fe1 69.62(11) . . ? C10 C5 Fe1 128.28(14) . . ? O1 C11 Fe1 174.91(19) . . ? O2 C12 Fe1 173.61(18) . . ? C14 C13 C25 102.97(15) . . ? C14 C13 Sb1 102.48(11) . . ? C25 C13 Sb1 122.62(12) . . ? C15 C14 C19 120.48(17) . . ? C15 C14 C13 129.33(17) . . ? C19 C14 C13 109.90(16) . . ? C14 C15 C16 120.44(17) . . ? C15 C16 C17 118.25(18) . . ? C15 C16 C26 122.39(17) . . ? C17 C16 C26 119.30(17) . . ? C18 C17 C16 121.77(18) . . ? C17 C18 C19 119.50(18) . . ? C18 C19 C14 119.54(17) . . ? C18 C19 C20 131.85(17) . . ? C14 C19 C20 108.61(16) . . ? C21 C20 C25 119.83(18) . . ? C21 C20 C19 131.60(18) . . ? C25 C20 C19 108.49(16) . . ? C20 C21 C22 119.46(18) . . ? C21 C22 C23 121.73(18) . . ? C22 C23 C24 118.24(18) . . ? C22 C23 C30 122.56(17) . . ? C24 C23 C30 119.20(17) . . ? C25 C24 C23 120.70(17) . . ? C24 C25 C20 120.01(17) . . ? C24 C25 C13 130.20(17) . . ? C20 C25 C13 109.67(16) . . ? C16 C26 C27 112.29(16) . . ? C16 C26 C28 108.40(17) . . ? C27 C26 C28 108.77(17) . . ? C16 C26 C29 109.76(16) . . ? C27 C26 C29 107.43(18) . . ? C28 C26 C29 110.17(17) . . ? C31 C30 C23 112.13(17) . . ? C31 C30 C33 108.09(18) . . ? C23 C30 C33 109.50(16) . . ? C31 C30 C32 108.32(17) . . ? C23 C30 C32 109.54(16) . . ? C33 C30 C32 109.20(18) . . ? C35 C34 C46 102.88(14) . . ? C35 C34 Sb1 121.09(12) . . ? C46 C34 Sb1 104.40(11) . . ? C36 C35 C40 120.03(16) . . ? C36 C35 C34 129.93(16) . . ? C40 C35 C34 109.74(15) . . ? C35 C36 C37 120.14(17) . . ? C38 C37 C36 118.61(17) . . ? C38 C37 C47 122.05(17) . . ? C36 C37 C47 119.29(17) . . ? C39 C38 C37 121.92(18) . . ? C40 C39 C38 118.66(17) . . ? C39 C40 C35 120.42(17) . . ? C39 C40 C41 130.58(17) . . ? C35 C40 C41 108.66(16) . . ? C42 C41 C46 119.69(17) . . ? C42 C41 C40 131.63(17) . . ? C46 C41 C40 108.55(15) . . ? C43 C42 C41 119.44(17) . . ? C42 C43 C44 121.81(17) . . ? C45 C44 C43 118.13(17) . . ? C45 C44 C51 119.74(17) . . ? C43 C44 C51 122.11(17) . . ? C46 C45 C44 120.53(17) . . ? C45 C46 C41 120.40(16) . . ? C45 C46 C34 129.91(16) . . ? C41 C46 C34 109.68(15) . . ? C50 C47 C37 112.75(17) . . ? C50 C47 C49 107.98(18) . . ? C37 C47 C49 109.86(16) . . ? C50 C47 C48 108.05(18) . . ? C37 C47 C48 108.93(16) . . ? C49 C47 C48 109.20(18) . . ? C53 C51 C44 112.17(17) . . ? C53 C51 C54 107.57(17) . . ? C44 C51 C54 110.31(16) . . ? C53 C51 C52 108.75(19) . . ? C44 C51 C52 108.93(17) . . ? C54 C51 C52 109.04(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.097 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.085 #===END