# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2306 data_flei1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris(isopropoxy)stibane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H21 O3 Sb' _chemical_formula_weight 299.01 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' '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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.4207(14) _cell_length_b 9.2306(7) _cell_length_c 18.5641(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2642.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 84 _cell_measurement_theta_min 21 _cell_measurement_theta_max 23 _exptl_crystal_description Cylinder _exptl_crystal_colour Colourless _exptl_crystal_size_max 1.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 2.069 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; A numerical cylinder absorption correction did not change the intensities significantly and was thus not applied ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Turbo CAD4' _diffrn_measurement_method 'omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% None _diffrn_reflns_number 7223 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 35.89 _reflns_number_total 3858 _reflns_number_gt 2880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-Software' _computing_cell_refinement 'CAD4-Software' _computing_data_reduction 'CADSHEL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _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^)+(0.0445P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ride _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3858 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.918400(10) 0.047639(16) 0.574862(9) 0.03672(7) Uani 1 1 d . . . O1 O 0.93567(10) -0.10213(19) 0.50040(9) 0.0387(4) Uani 1 1 d . . . O2 O 0.81373(11) -0.05216(16) 0.61099(12) 0.0484(5) Uani 1 1 d . . . O3 O 0.99645(13) -0.03915(18) 0.64411(10) 0.0443(4) Uani 1 1 d . . . C1 C 0.74434(17) 0.0316(3) 0.63944(17) 0.0483(6) Uani 1 1 d . . . H1A H 0.7465 0.1308 0.6178 0.058 Uiso 1 1 calc R . . C2 C 0.86859(18) -0.1983(3) 0.47539(15) 0.0523(7) Uani 1 1 d . . . H2A H 0.8330 -0.2300 0.5176 0.063 Uiso 1 1 calc R . . C3 C 0.99183(17) -0.1896(3) 0.66198(14) 0.0437(5) Uani 1 1 d . . . H3A H 0.9413 -0.2340 0.6363 0.052 Uiso 1 1 calc R . . C12 C 0.66056(19) -0.0400(3) 0.6179(3) 0.0720(10) Uani 1 1 d . . . H12A H 0.6563 -0.0426 0.5652 0.108 Uiso 1 1 calc R . . H12B H 0.6117 0.0150 0.6376 0.108 Uiso 1 1 calc R . . H12C H 0.6592 -0.1391 0.6368 0.108 Uiso 1 1 calc R . . C22 C 0.9141(3) -0.3289(5) 0.4441(3) 0.0883(15) Uani 1 1 d . . . H22A H 0.9580 -0.3637 0.4782 0.132 Uiso 1 1 calc R . . H22B H 0.9423 -0.3019 0.3987 0.132 Uiso 1 1 calc R . . H22C H 0.8717 -0.4059 0.4351 0.132 Uiso 1 1 calc R . . C32 C 1.0741(2) -0.2625(4) 0.6370(2) 0.0762(10) Uani 1 1 d . . . H32A H 1.0774 -0.2585 0.5843 0.114 Uiso 1 1 calc R . . H32B H 1.0740 -0.3639 0.6527 0.114 Uiso 1 1 calc R . . H32C H 1.1243 -0.2125 0.6578 0.114 Uiso 1 1 calc R . . C21 C 0.8114(3) -0.1195(7) 0.4235(2) 0.0998(16) Uani 1 1 d . . . H21A H 0.7850 -0.0361 0.4477 0.150 Uiso 1 1 calc R . . H21B H 0.7658 -0.1849 0.4064 0.150 Uiso 1 1 calc R . . H21C H 0.8460 -0.0860 0.3825 0.150 Uiso 1 1 calc R . . C31 C 0.9783(3) -0.2037(4) 0.74157(17) 0.0694(9) Uani 1 1 d . . . H31A H 0.9259 -0.1505 0.7556 0.104 Uiso 1 1 calc R . . H31B H 1.0285 -0.1635 0.7671 0.104 Uiso 1 1 calc R . . H31C H 0.9716 -0.3062 0.7542 0.104 Uiso 1 1 calc R . . C11 C 0.7529(3) 0.0443(5) 0.7198(2) 0.0945(14) Uani 1 1 d . . . H11A H 0.8067 0.0957 0.7316 0.142 Uiso 1 1 calc R . . H11B H 0.7543 -0.0527 0.7412 0.142 Uiso 1 1 calc R . . H11C H 0.7034 0.0982 0.7391 0.142 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 0.03426(10) 0.03423(10) 0.04166(11) -0.00005(6) 0.00801(6) 0.00207(5) O1 0.0325(8) 0.0482(9) 0.0356(8) -0.0048(8) 0.0036(6) -0.0046(7) O2 0.0379(9) 0.0417(9) 0.0656(12) -0.0021(9) 0.0194(9) 0.0015(7) O3 0.0490(10) 0.0440(9) 0.0400(8) 0.0000(7) -0.0059(7) -0.0093(7) C1 0.0385(12) 0.0404(12) 0.0662(17) -0.0026(12) 0.0147(12) 0.0025(10) C2 0.0469(13) 0.0688(17) 0.0412(12) -0.0106(12) 0.0070(11) -0.0249(12) C3 0.0439(12) 0.0440(12) 0.0431(12) 0.0035(11) -0.0076(11) -0.0042(10) C12 0.0399(14) 0.0563(17) 0.120(3) -0.0114(19) 0.010(2) -0.0014(12) C22 0.090(3) 0.080(3) 0.096(3) -0.043(2) 0.037(2) -0.040(2) C32 0.080(2) 0.076(2) 0.073(2) 0.004(2) 0.0058(18) 0.0274(19) C21 0.060(2) 0.163(5) 0.076(2) 0.018(3) -0.0346(18) -0.034(3) C31 0.079(2) 0.080(2) 0.0498(16) 0.0168(16) 0.0011(16) -0.0014(18) C11 0.089(3) 0.127(4) 0.067(2) -0.031(2) 0.018(2) 0.007(3) _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 O3 1.9346(19) . ? Sb1 O1 1.9731(17) . ? Sb1 O2 1.9758(17) . ? O1 C2 1.440(3) . ? O2 C1 1.422(3) . ? O3 C3 1.430(3) . ? C1 C11 1.502(5) . ? C1 C12 1.506(4) . ? C1 H1A 1.0000 . ? C2 C21 1.494(5) . ? C2 C22 1.512(5) . ? C2 H2A 1.0000 . ? C3 C31 1.498(4) . ? C3 C32 1.509(4) . ? C3 H3A 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? 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 O3 Sb1 O1 95.25(8) . . ? O3 Sb1 O2 95.14(8) . . ? O1 Sb1 O2 91.23(7) . . ? C2 O1 Sb1 124.11(15) . . ? C1 O2 Sb1 119.15(14) . . ? C3 O3 Sb1 121.70(15) . . ? O2 C1 C11 110.2(3) . . ? O2 C1 C12 107.9(2) . . ? C11 C1 C12 112.0(3) . . ? O2 C1 H1A 108.9 . . ? C11 C1 H1A 108.9 . . ? C12 C1 H1A 108.9 . . ? O1 C2 C21 109.4(3) . . ? O1 C2 C22 106.4(2) . . ? C21 C2 C22 114.5(4) . . ? O1 C2 H2A 108.8 . . ? C21 C2 H2A 108.8 . . ? C22 C2 H2A 108.8 . . ? O3 C3 C31 108.7(2) . . ? O3 C3 C32 108.7(2) . . ? C31 C3 C32 112.4(3) . . ? O3 C3 H3A 109.0 . . ? C31 C3 H3A 109.0 . . ? C32 C3 H3A 109.0 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C32 H32A 109.5 . . ? C3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C3 C31 H31A 109.5 . . ? C3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Sb1 O1 C2 115.5(2) . . . . ? O2 Sb1 O1 C2 20.2(2) . . . . ? O3 Sb1 O2 C1 117.6(2) . . . . ? O1 Sb1 O2 C1 -147.0(2) . . . . ? O1 Sb1 O3 C3 -48.68(19) . . . . ? O2 Sb1 O3 C3 43.03(19) . . . . ? Sb1 O2 C1 C11 -94.3(3) . . . . ? Sb1 O2 C1 C12 143.2(2) . . . . ? Sb1 O1 C2 C21 78.6(3) . . . . ? Sb1 O1 C2 C22 -157.3(2) . . . . ? Sb1 O3 C3 C31 -122.8(2) . . . . ? Sb1 O3 C3 C32 114.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.621 _diffrn_reflns_theta_full 35.89 _diffrn_measured_fraction_theta_full 0.621 _refine_diff_density_max 1.307 _refine_diff_density_min -1.309 _refine_diff_density_rms 0.120 #===END data_flei2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chloro-bis(isopropoxy)stibane-Dimer ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H14 Cl O2 Sb' _chemical_formula_weight 275.37 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.035(2) _cell_length_b 14.884(2) _cell_length_c 8.065(1) _cell_angle_alpha 90.00 _cell_angle_beta 93.080(10) _cell_angle_gamma 90.00 _cell_volume 2041.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 80 _cell_measurement_theta_min 25 _cell_measurement_theta_max 27 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 2.915 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.7206 _exptl_absorpt_correction_T_max 0.9992 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'Nonius Turbo CAD4' _diffrn_measurement_method 'omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% None _diffrn_reflns_number 2394 _diffrn_reflns_av_R_equivalents 0.0080 _diffrn_reflns_av_sigmaI/netI 0.0117 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 26.94 _reflns_number_total 2220 _reflns_number_gt 1944 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-Software' _computing_cell_refinement 'CAD4-Software' _computing_data_reduction 'CADSHEL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _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^)+(0.0235P)^2^+7.5652P] 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 2220 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0529 _refine_ls_wR_factor_gt 0.0506 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.253891(9) 0.251699(11) 0.222206(19) 0.01959(7) Uani 1 1 d . . . Cl1 Cl 0.35170(4) 0.30982(5) 0.43749(8) 0.03101(15) Uani 1 1 d . . . O1 O 0.31615(10) 0.29037(13) 0.0312(2) 0.0219(4) Uani 1 1 d . . . O2 O 0.30256(13) 0.13433(13) 0.2191(2) 0.0306(4) Uani 1 1 d . . . C2 C 0.31745(18) 0.07829(19) 0.3619(3) 0.0303(6) Uani 1 1 d . . . H2A H 0.3095 0.1140 0.4646 0.036 Uiso 1 1 calc R . . C1 C 0.40212(15) 0.3003(2) 0.0368(4) 0.0328(6) Uani 1 1 d . . . H1A H 0.4229 0.2996 0.1552 0.039 Uiso 1 1 calc R . . C22 C 0.2610(3) 0.0014(2) 0.3534(5) 0.0554(11) Uani 1 1 d . . . H22A H 0.2071 0.0244 0.3541 0.083 Uiso 1 1 calc R . . H22B H 0.2714 -0.0379 0.4496 0.083 Uiso 1 1 calc R . . H22C H 0.2675 -0.0327 0.2511 0.083 Uiso 1 1 calc R . . C12 C 0.4382(2) 0.2255(4) -0.0541(8) 0.0875(19) Uani 1 1 d . . . H12A H 0.4281 0.1685 0.0020 0.131 Uiso 1 1 calc R . . H12B H 0.4950 0.2351 -0.0562 0.131 Uiso 1 1 calc R . . H12C H 0.4152 0.2233 -0.1681 0.131 Uiso 1 1 calc R . . C11 C 0.4204(3) 0.3876(3) -0.0381(12) 0.149(4) Uani 1 1 d . . . H11A H 0.3956 0.4359 0.0230 0.224 Uiso 1 1 calc R . . H11B H 0.4003 0.3885 -0.1543 0.224 Uiso 1 1 calc R . . H11C H 0.4775 0.3965 -0.0329 0.224 Uiso 1 1 calc R . . C21 C 0.4022(3) 0.0486(4) 0.3611(6) 0.0699(13) Uani 1 1 d . . . H21A H 0.4366 0.1015 0.3666 0.105 Uiso 1 1 calc R . . H21B H 0.4105 0.0151 0.2590 0.105 Uiso 1 1 calc R . . H21C H 0.4146 0.0100 0.4574 0.105 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 0.02277(10) 0.02220(10) 0.01395(10) 0.00063(6) 0.00244(6) -0.00205(6) Cl1 0.0309(3) 0.0403(4) 0.0214(3) -0.0039(3) -0.0026(2) -0.0063(3) O1 0.0202(9) 0.0280(9) 0.0177(8) 0.0037(7) 0.0021(7) -0.0046(7) O2 0.0514(12) 0.0219(9) 0.0187(9) 0.0009(8) 0.0033(8) 0.0035(9) C2 0.0458(17) 0.0261(14) 0.0190(12) 0.0037(10) 0.0026(11) 0.0047(12) C1 0.0184(12) 0.0510(19) 0.0290(14) 0.0007(13) 0.0023(10) -0.0106(12) C22 0.096(3) 0.0355(19) 0.0352(17) 0.0050(15) 0.0080(19) -0.0197(18) C12 0.0254(19) 0.097(4) 0.141(6) -0.042(4) 0.013(2) 0.006(2) C11 0.042(3) 0.052(3) 0.359(12) 0.054(5) 0.066(5) -0.008(2) C21 0.061(3) 0.095(4) 0.054(2) 0.018(2) 0.004(2) 0.035(3) _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 O2 1.9345(19) . ? Sb1 O1 2.0011(17) . ? Sb1 O1 2.3940(18) 7 ? Sb1 Cl1 2.4956(7) . ? O1 C1 1.470(3) . ? O1 Sb1 2.3940(18) 7 ? O2 C2 1.434(3) . ? C2 C22 1.494(5) . ? C2 C21 1.511(5) . ? C2 H2A 1.0000 . ? C1 C11 1.473(6) . ? C1 C12 1.485(6) . ? C1 H1A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Sb1 O1 90.25(8) . . ? O2 Sb1 O1 86.96(7) . 7 ? O1 Sb1 O1 71.25(7) . 7 ? O2 Sb1 Cl1 92.96(6) . . ? O1 Sb1 Cl1 94.25(5) . . ? O1 Sb1 Cl1 165.50(4) 7 . ? C1 O1 Sb1 125.00(15) . . ? C1 O1 Sb1 120.18(15) . 7 ? Sb1 O1 Sb1 108.75(7) . 7 ? C2 O2 Sb1 124.92(17) . . ? O2 C2 C22 108.9(3) . . ? O2 C2 C21 107.2(3) . . ? C22 C2 C21 112.9(3) . . ? O2 C2 H2A 109.3 . . ? C22 C2 H2A 109.3 . . ? C21 C2 H2A 109.3 . . ? O1 C1 C11 108.0(3) . . ? O1 C1 C12 110.3(3) . . ? C11 C1 C12 110.9(4) . . ? O1 C1 H1A 109.2 . . ? C11 C1 H1A 109.2 . . ? C12 C1 H1A 109.2 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Sb1 O1 C1 -65.6(2) . . . . ? O1 Sb1 O1 C1 -152.3(2) 7 . . . ? Cl1 Sb1 O1 C1 27.3(2) . . . . ? O2 Sb1 O1 Sb1 86.70(9) . . . 7 ? O1 Sb1 O1 Sb1 0.0 7 . . 7 ? Cl1 Sb1 O1 Sb1 179.68(6) . . . 7 ? O1 Sb1 O2 C2 149.3(2) . . . . ? O1 Sb1 O2 C2 -139.5(2) 7 . . . ? Cl1 Sb1 O2 C2 55.0(2) . . . . ? Sb1 O2 C2 C22 107.4(3) . . . . ? Sb1 O2 C2 C21 -130.2(3) . . . . ? Sb1 O1 C1 C11 -132.4(4) . . . . ? Sb1 O1 C1 C11 78.2(4) 7 . . . ? Sb1 O1 C1 C12 106.3(4) . . . . ? Sb1 O1 C1 C12 -43.1(4) 7 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.94 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.988 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.081 #===END