data_c:\x-ray\kcm\maxushex\kcmjorge _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H27 S3 Sb' _chemical_formula_weight 389.27 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' 'S' 'S' 0.1246 0.1234 '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 Hexagonal _symmetry_space_group_name_H-M P63 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' _cell_length_a 10.3430(2) _cell_length_b 10.3430(2) _cell_length_c 9.7560(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 903.85(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14357 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 1.852 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.686 _exptl_absorpt_correction_T_max 0.866 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19393 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0509 _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 -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 30.02 _reflns_number_total 1761 _reflns_number_gt 1273 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (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^)+(0.0370P)^2^+0.1725P] 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 0.009(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.22(6) _refine_ls_number_reflns 1761 _refine_ls_number_parameters 99 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.0000 0.0000 0.53171(7) 0.02598(15) Uani 0.75 3 d SP . 1 S1 S -0.08255(13) 0.13920(12) 0.39236(16) 0.0340(3) Uani 0.75 1 d P A 1 C1 C -0.0314(7) 0.3114(6) 0.4906(7) 0.0328(11) Uani 0.75 1 d P A 1 C2 C -0.0680(7) 0.4045(6) 0.3964(8) 0.0534(13) Uani 0.75 1 d P A 1 H2A H -0.0066 0.4294 0.3135 0.080 Uiso 0.75 1 calc PR A 1 H2B H -0.0473 0.4967 0.4434 0.080 Uiso 0.75 1 calc PR A 1 H2C H -0.1738 0.3479 0.3712 0.080 Uiso 0.75 1 calc PR A 1 C3 C -0.1221(9) 0.2724(9) 0.6182(6) 0.0482(16) Uani 0.75 1 d P A 1 H3A H -0.0938 0.2153 0.6792 0.072 Uiso 0.75 1 calc PR A 1 H3B H -0.2282 0.2122 0.5951 0.072 Uiso 0.75 1 calc PR A 1 H3C H -0.1039 0.3641 0.6645 0.072 Uiso 0.75 1 calc PR A 1 C4 C 0.1371(5) 0.3961(6) 0.5231(8) 0.0477(12) Uani 0.75 1 d P A 1 H4A H 0.1939 0.4206 0.4374 0.072 Uiso 0.75 1 calc PR A 1 H4B H 0.1616 0.3331 0.5799 0.072 Uiso 0.75 1 calc PR A 1 H4C H 0.1627 0.4883 0.5726 0.072 Uiso 0.75 1 calc PR A 1 Sb1A Sb 0.0000 0.0000 0.36703(9) 0.0178(3) Uani 0.25 3 d SP . 2 S1A S -0.0795(4) 0.1426(3) 0.5066(3) 0.0203(6) Uani 0.25 1 d P B 2 C1A C -0.0216(15) 0.3176(15) 0.4069(19) 0.022(3) Uani 0.25 1 d P B 2 C2A C -0.065(2) 0.4043(19) 0.5023(17) 0.041(4) Uani 0.25 1 d P B 2 H2A1 H -0.0058 0.4281 0.5866 0.062 Uiso 0.25 1 calc PR B 2 H2A2 H -0.1713 0.3442 0.5248 0.062 Uiso 0.25 1 calc PR B 2 H2A3 H -0.0459 0.4970 0.4576 0.062 Uiso 0.25 1 calc PR B 2 C3A C -0.1150(16) 0.2758(17) 0.2675(12) 0.026(3) Uani 0.25 1 d P B 2 H3A1 H -0.2220 0.2203 0.2886 0.039 Uiso 0.25 1 calc PR B 2 H3A2 H -0.0891 0.2140 0.2106 0.039 Uiso 0.25 1 calc PR B 2 H3A3 H -0.0913 0.3675 0.2180 0.039 Uiso 0.25 1 calc PR B 2 C4A C 0.1460(17) 0.4022(15) 0.3768(16) 0.032(3) Uani 0.25 1 d P B 2 H4A1 H 0.2016 0.4245 0.4631 0.049 Uiso 0.25 1 calc PR B 2 H4A2 H 0.1725 0.4957 0.3292 0.049 Uiso 0.25 1 calc PR B 2 H4A3 H 0.1713 0.3408 0.3187 0.049 Uiso 0.25 1 calc PR B 2 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 0.02563(17) 0.02563(17) 0.0267(2) 0.000 0.000 0.01282(8) S1 0.0391(7) 0.0335(6) 0.0344(8) -0.0061(7) -0.0097(7) 0.0219(6) C1 0.038(3) 0.023(3) 0.039(3) -0.003(2) -0.004(3) 0.017(2) C2 0.058(4) 0.041(3) 0.067(4) 0.016(4) 0.007(4) 0.029(3) C3 0.058(5) 0.045(4) 0.046(4) -0.005(2) 0.008(2) 0.028(4) C4 0.034(2) 0.037(3) 0.063(3) -0.017(3) -0.004(3) 0.011(2) Sb1A 0.0194(5) 0.0194(5) 0.0147(7) 0.000 0.000 0.0097(2) S1A 0.0289(16) 0.0253(15) 0.0133(19) 0.0035(12) 0.0068(12) 0.0185(13) C1A 0.028(8) 0.016(6) 0.027(7) -0.002(8) -0.008(8) 0.015(6) C2A 0.076(12) 0.048(10) 0.023(8) 0.010(6) 0.013(7) 0.049(10) C3A 0.028(6) 0.038(7) 0.012(7) 0.009(6) 0.003(5) 0.017(6) C4A 0.040(8) 0.022(7) 0.030(8) -0.006(6) 0.001(6) 0.011(6) _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 S1 2.4248(14) 3 ? Sb1 S1 2.4248(14) 5 ? Sb1 S1 2.4248(14) . ? S1 C1 1.852(6) . ? C1 C3 1.489(9) . ? C1 C2 1.510(8) . ? C1 C4 1.541(7) . ? Sb1A S1A 2.432(3) 5 ? Sb1A S1A 2.432(3) . ? Sb1A S1A 2.432(3) 3 ? S1A C1A 1.870(15) . ? C1A C2A 1.51(2) . ? C1A C4A 1.53(2) . ? C1A C3A 1.60(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Sb1 S1 91.63(6) 3 5 ? S1 Sb1 S1 91.63(6) 3 . ? S1 Sb1 S1 91.63(6) 5 . ? C1 S1 Sb1 105.4(2) . . ? C3 C1 C2 110.9(6) . . ? C3 C1 C4 111.2(6) . . ? C2 C1 C4 109.6(5) . . ? C3 C1 S1 109.5(4) . . ? C2 C1 S1 104.8(4) . . ? C4 C1 S1 110.5(4) . . ? S1A Sb1A S1A 91.72(10) 5 . ? S1A Sb1A S1A 91.72(10) 5 3 ? S1A Sb1A S1A 91.72(10) . 3 ? C1A S1A Sb1A 104.7(5) . . ? C2A C1A C4A 111.5(13) . . ? C2A C1A C3A 111.5(12) . . ? C4A C1A C3A 110.5(14) . . ? C2A C1A S1A 102.0(12) . . ? C4A C1A S1A 112.1(10) . . ? C3A C1A S1A 108.9(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.644 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.078