Electronic Supplementary Material for CrystEngComm This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Edward R.T. Tiekink' 'Yu Liu.' _publ_contact_author_name 'Dr Edward R.T. Tiekink' _publ_contact_author_address ; Department of Chemistry National University of Singapore Singapore 117543 SINGAPORE ; _publ_contact_author_email CHMTERT@NUS.EDU.SG _publ_requested_journal 'Cryst Eng. Comm.' _publ_section_title ; Supramolecular associations in binary antimony(III) dithiocarbamates: influence of ligand steric bulk, influence on coordination geometry, and competition with hydrogen-bonding ; data_Sb{S2CNMe)2}3 _database_code_depnum_ccdc_archive 'CCDC 253918' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C9.33 H18.33 Cl N3 S6 Sb' _chemical_formula_weight 522.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 26.6252(6) _cell_length_b 26.6252 _cell_length_c 14.6744(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 9009.0(5) _cell_formula_units_Z 18 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5366 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4668 _exptl_absorpt_coefficient_mu 2.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.769 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25470 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.030 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 30.0 _reflns_number_total 5864 _reflns_number_gt 4731 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.066P)^2^+14.783P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5864 _refine_ls_number_parameters 192 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_ref 0.118 _refine_ls_wR_factor_gt 0.111 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.002 _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 Sb Sb 0.534459(9) 0.451606(9) 0.116294(16) 0.03913(9) Uani 1 1 d . . . S1 S 0.61236(4) 0.44154(4) 0.19872(6) 0.0452(2) Uani 1 1 d . . . S2 S 0.65385(4) 0.53155(4) 0.05499(7) 0.0537(2) Uani 1 1 d . . . S3 S 0.53320(4) 0.37643(4) 0.00946(6) 0.04344(19) Uani 1 1 d . . . S4 S 0.44165(5) 0.40708(5) -0.02595(7) 0.0550(2) Uani 1 1 d . . . S5 S 0.46666(4) 0.36362(3) 0.21153(6) 0.04084(19) Uani 1 1 d . . . S6 S 0.49832(5) 0.47655(4) 0.29782(8) 0.0585(3) Uani 1 1 d . . . N1 N 0.72292(12) 0.51126(14) 0.1608(2) 0.0463(7) Uani 1 1 d . . . N2 N 0.45011(13) 0.32447(15) -0.1125(2) 0.0480(7) Uani 1 1 d . . . N3 N 0.41995(13) 0.37353(13) 0.3640(2) 0.0450(6) Uani 1 1 d . . . C1 C 0.66922(14) 0.49746(15) 0.1384(2) 0.0383(6) Uani 1 1 d . . . C2 C 0.7361(2) 0.4829(2) 0.2345(3) 0.0695(13) Uani 1 1 d . . . H2A H 0.7099 0.4758 0.2851 0.104 Uiso 1 1 calc R . . H2B H 0.7758 0.5077 0.2545 0.104 Uiso 1 1 calc R . . H2C H 0.7313 0.4463 0.2130 0.104 Uiso 1 1 calc R . . C3 C 0.77381(17) 0.5568(2) 0.1154(3) 0.0640(11) Uani 1 1 d . . . H3A H 0.7620 0.5692 0.0613 0.096 Uiso 1 1 calc R . . H3B H 0.7994 0.5423 0.0982 0.096 Uiso 1 1 calc R . . H3C H 0.7941 0.5895 0.1565 0.096 Uiso 1 1 calc R . . C4 C 0.47128(14) 0.36539(15) -0.0505(2) 0.0395(7) Uani 1 1 d . . . C5 C 0.4759(2) 0.2891(2) -0.1370(3) 0.0670(12) Uani 1 1 d . . . H5A H 0.4862 0.2945 -0.2011 0.101 Uiso 1 1 calc R . . H5B H 0.4481 0.2486 -0.1256 0.101 Uiso 1 1 calc R . . H5C H 0.5104 0.3008 -0.1007 0.101 Uiso 1 1 calc R . . C6 C 0.39842(18) 0.3122(2) -0.1649(3) 0.0618(11) Uani 1 1 d . . . H6A H 0.3716 0.3170 -0.1261 0.093 Uiso 1 1 calc R . . H6B H 0.3798 0.2727 -0.1874 0.093 Uiso 1 1 calc R . . H6C H 0.4095 0.3389 -0.2159 0.093 Uiso 1 1 calc R . . C7 C 0.45806(14) 0.40295(14) 0.2995(2) 0.0399(7) Uani 1 1 d . . . C8 C 0.38455(19) 0.31033(17) 0.3631(3) 0.0573(10) Uani 1 1 d . . . H8A H 0.3482 0.2989 0.3323 0.086 Uiso 1 1 calc R . . H8B H 0.3769 0.2960 0.4252 0.086 Uiso 1 1 calc R . . H8C H 0.4051 0.2942 0.3312 0.086 Uiso 1 1 calc R . . C9 C 0.4063(2) 0.4026(2) 0.4365(3) 0.0661(12) Uani 1 1 d . . . H9A H 0.4342 0.4438 0.4353 0.099 Uiso 1 1 calc R . . H9B H 0.4080 0.3867 0.4950 0.099 Uiso 1 1 calc R . . H9C H 0.3676 0.3967 0.4270 0.099 Uiso 1 1 calc R . . C10 C 0.3333 0.6667 0.3212(6) 0.336(18) Uiso 1 3 d SD . . Cl1 Cl 0.34761(15) 0.73829(7) 0.3236(3) 0.0609(8) Uiso 0.33 1 d PD . . Cl2 Cl 0.3434(2) 0.73267(16) 0.2800(4) 0.0904(13) Uiso 0.33 1 d PD . . Cl3 Cl 0.3237(5) 0.6895(4) 0.4283(5) 0.177(3) Uiso 0.33 1 d PD . . 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 Sb 0.03372(12) 0.03592(13) 0.04830(15) -0.00047(8) -0.00110(8) 0.01782(9) S1 0.0343(4) 0.0541(5) 0.0430(4) 0.0135(4) 0.0032(3) 0.0190(4) S2 0.0460(5) 0.0540(5) 0.0538(5) 0.0180(4) -0.0004(4) 0.0194(4) S3 0.0388(4) 0.0513(5) 0.0482(4) -0.0063(4) -0.0045(3) 0.0286(4) S4 0.0528(5) 0.0629(6) 0.0652(6) 0.0009(5) -0.0059(4) 0.0409(5) S5 0.0377(4) 0.0327(4) 0.0507(5) -0.0051(3) 0.0047(3) 0.0166(3) S6 0.0529(5) 0.0367(4) 0.0761(7) -0.0148(4) 0.0087(5) 0.0151(4) N1 0.0335(14) 0.0591(18) 0.0414(15) 0.0039(13) 0.0018(11) 0.0193(13) N2 0.0456(16) 0.0610(19) 0.0373(14) -0.0018(13) -0.0005(12) 0.0265(15) N3 0.0454(16) 0.0436(15) 0.0512(17) -0.0040(13) 0.0069(13) 0.0262(13) C1 0.0351(15) 0.0430(17) 0.0336(15) -0.0018(12) -0.0009(12) 0.0173(13) C2 0.053(2) 0.096(4) 0.064(3) 0.015(2) -0.007(2) 0.041(3) C3 0.0378(19) 0.064(3) 0.081(3) 0.013(2) 0.0136(19) 0.0191(18) C4 0.0343(15) 0.0472(18) 0.0389(16) 0.0070(13) 0.0037(12) 0.0219(14) C5 0.078(3) 0.080(3) 0.056(2) -0.023(2) -0.008(2) 0.049(3) C6 0.047(2) 0.087(3) 0.047(2) -0.007(2) -0.0103(17) 0.030(2) C7 0.0338(15) 0.0374(16) 0.0516(18) -0.0085(13) -0.0035(13) 0.0201(13) C8 0.061(2) 0.046(2) 0.061(2) 0.0070(17) 0.0139(19) 0.0243(19) C9 0.076(3) 0.069(3) 0.065(3) -0.004(2) 0.020(2) 0.044(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 Sb S1 2.5282(9) . ? Sb S3 2.5294(9) . ? Sb S5 2.5438(9) . ? S1 C1 1.743(3) . ? S2 C1 1.692(3) . ? S3 C4 1.759(3) . ? S4 C4 1.691(3) . ? S5 C7 1.747(3) . ? S6 C7 1.700(3) . ? N1 C1 1.327(4) . ? N1 C3 1.452(5) . ? N1 C2 1.458(5) . ? N2 C4 1.310(5) . ? N2 C6 1.464(5) . ? N2 C5 1.460(5) . ? N3 C7 1.321(4) . ? N3 C8 1.461(5) . ? N3 C9 1.464(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 Cl2 1.7480(10) . ? C10 Cl2 1.7480(10) 2_665 ? C10 Cl2 1.7481(10) 3_565 ? C10 Cl1 1.7485(10) . ? C10 Cl1 1.7485(10) 2_665 ? C10 Cl1 1.7485(10) 3_565 ? C10 Cl3 1.7493(10) . ? C10 Cl3 1.7493(10) 2_665 ? C10 Cl3 1.7493(10) 3_565 ? Cl1 Cl3 1.903(10) . ? Cl2 Cl2 2.841(6) 2_665 ? Cl2 Cl2 2.841(6) 3_565 ? Cl3 Cl3 1.333(14) 3_565 ? Cl3 Cl3 1.333(14) 2_665 ? 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 Sb S3 84.24(3) . . ? S1 Sb S5 83.20(3) . . ? S3 Sb S5 83.64(3) . . ? C1 S1 Sb 94.30(11) . . ? C4 S3 Sb 94.76(12) . . ? C7 S5 Sb 95.68(12) . . ? C1 N1 C3 123.0(3) . . ? C1 N1 C2 123.0(3) . . ? C3 N1 C2 114.1(3) . . ? C4 N2 C6 121.0(3) . . ? C4 N2 C5 124.2(3) . . ? C6 N2 C5 114.8(3) . . ? C7 N3 C8 122.6(3) . . ? C7 N3 C9 121.8(3) . . ? C8 N3 C9 115.3(3) . . ? N1 C1 S2 123.1(3) . . ? N1 C1 S1 117.8(2) . . ? S2 C1 S1 119.07(19) . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 S4 123.1(3) . . ? N2 C4 S3 117.6(3) . . ? S4 C4 S3 119.3(2) . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 S6 123.3(3) . . ? N3 C7 S5 117.8(2) . . ? S6 C7 S5 119.0(2) . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Cl2 C10 Cl2 108.7(3) . 2_665 ? Cl2 C10 Cl2 108.7(3) . 3_565 ? Cl2 C10 Cl2 108.7(3) 2_665 3_565 ? Cl2 C10 Cl1 21.58(17) . . ? Cl2 C10 Cl1 120.9(3) 2_665 . ? Cl2 C10 Cl1 115.9(3) 3_565 . ? Cl2 C10 Cl1 115.9(3) . 2_665 ? Cl2 C10 Cl1 21.58(17) 2_665 2_665 ? Cl2 C10 Cl1 120.9(3) 3_565 2_665 ? Cl1 C10 Cl1 119.96(2) . 2_665 ? Cl2 C10 Cl1 120.9(3) . 3_565 ? Cl2 C10 Cl1 115.9(3) 2_665 3_565 ? Cl2 C10 Cl1 21.58(17) 3_565 3_565 ? Cl1 C10 Cl1 119.96(2) . 3_565 ? Cl1 C10 Cl1 119.96(2) 2_665 3_565 ? Cl2 C10 Cl3 86.3(4) . . ? Cl2 C10 Cl3 110.4(5) 2_665 . ? Cl2 C10 Cl3 130.4(5) 3_565 . ? Cl1 C10 Cl3 65.9(4) . . ? Cl1 C10 Cl3 90.0(5) 2_665 . ? Cl1 C10 Cl3 110.7(5) 3_565 . ? Cl2 C10 Cl3 130.4(5) . 2_665 ? Cl2 C10 Cl3 86.3(4) 2_665 2_665 ? Cl2 C10 Cl3 110.4(5) 3_565 2_665 ? Cl1 C10 Cl3 110.7(5) . 2_665 ? Cl1 C10 Cl3 65.9(4) 2_665 2_665 ? Cl1 C10 Cl3 90.0(5) 3_565 2_665 ? Cl3 C10 Cl3 44.8(5) . 2_665 ? Cl2 C10 Cl3 110.4(5) . 3_565 ? Cl2 C10 Cl3 130.4(5) 2_665 3_565 ? Cl2 C10 Cl3 86.3(4) 3_565 3_565 ? Cl1 C10 Cl3 90.0(5) . 3_565 ? Cl1 C10 Cl3 110.7(5) 2_665 3_565 ? Cl1 C10 Cl3 65.9(4) 3_565 3_565 ? Cl3 C10 Cl3 44.8(5) . 3_565 ? Cl3 C10 Cl3 44.8(5) 2_665 3_565 ? C10 Cl1 Cl3 57.07(19) . . ? C10 Cl2 Cl2 35.66(16) . 2_665 ? C10 Cl2 Cl2 35.66(16) . 3_565 ? Cl2 Cl2 Cl2 60.000(1) 2_665 3_565 ? Cl3 Cl3 Cl3 60.000(5) 3_565 2_665 ? Cl3 Cl3 C10 67.6(2) 3_565 . ? Cl3 Cl3 C10 67.6(2) 2_665 . ? Cl3 Cl3 Cl1 98.2(7) 3_565 . ? Cl3 Cl3 Cl1 124.6(2) 2_665 . ? C10 Cl3 Cl1 57.03(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.0 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.34 _refine_diff_density_min -1.16 _refine_diff_density_rms 0.113 data_Sb{S2CN(CH2)5}3 _database_code_depnum_ccdc_archive 'CCDC 253919' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C19 H31 Cl3 N3 S6 Sb' _chemical_formula_weight 721.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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 10.3916(6) _cell_length_b 11.4660(7) _cell_length_c 13.7520(9) _cell_angle_alpha 95.617(1) _cell_angle_beta 110.929(1) _cell_angle_gamma 106.614(2) _cell_volume 1429.47(15) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3878 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 29.1 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.730 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12120 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.051 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 30.1 _reflns_number_total 8164 _reflns_number_gt 6825 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.039P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8164 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.050 _refine_ls_R_factor_gt 0.039 _refine_ls_wR_factor_ref 0.090 _refine_ls_wR_factor_gt 0.085 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _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 Sb Sb 0.144681(19) 0.098904(17) 0.211741(13) 0.02501(6) Uani 1 1 d . . . Cl1 Cl 0.30233(11) 0.38448(10) 0.93368(9) 0.0612(3) Uani 1 1 d . . . Cl2 Cl 0.02333(12) 0.41662(10) 0.83403(8) 0.0621(3) Uani 1 1 d . . . Cl3 Cl 0.11564(10) 0.36803(11) 1.04542(7) 0.0581(3) Uani 1 1 d . . . S1 S 0.24965(9) -0.06634(7) 0.17775(6) 0.03592(17) Uani 1 1 d . . . S2 S 0.18965(8) 0.07315(7) 0.00796(5) 0.03141(15) Uani 1 1 d . . . S3 S 0.25826(8) 0.07121(7) 0.40091(5) 0.03209(16) Uani 1 1 d . . . S4 S -0.05655(8) -0.07668(7) 0.28191(5) 0.03292(16) Uani 1 1 d . . . S5 S 0.39240(7) 0.27176(7) 0.27393(6) 0.03092(15) Uani 1 1 d . . . S6 S 0.16123(8) 0.34519(7) 0.31525(6) 0.03416(16) Uani 1 1 d . . . N1 N 0.2451(3) -0.1393(2) -0.01286(18) 0.0309(5) Uani 1 1 d . . . N2 N 0.1063(3) -0.0929(2) 0.47652(18) 0.0301(5) Uani 1 1 d . . . N3 N 0.4332(3) 0.4997(2) 0.36582(19) 0.0316(5) Uani 1 1 d . . . C1 C 0.2273(3) -0.0528(3) 0.0476(2) 0.0257(5) Uani 1 1 d . . . C2 C 0.2353(3) -0.1345(3) -0.1213(2) 0.0385(7) Uani 1 1 d . . . H2A H 0.2247 -0.0554 -0.1370 0.046 Uiso 1 1 calc R . . H2B H 0.1482 -0.2027 -0.1728 0.046 Uiso 1 1 calc R . . C3 C 0.3705(3) -0.1459(3) -0.1328(2) 0.0371(7) Uani 1 1 d . . . H3A H 0.3580 -0.1492 -0.2073 0.044 Uiso 1 1 calc R . . H3B H 0.4555 -0.0719 -0.0882 0.044 Uiso 1 1 calc R . . C4 C 0.3995(4) -0.2616(3) -0.1006(2) 0.0417(8) Uani 1 1 d . . . H4A H 0.4917 -0.2631 -0.1041 0.050 Uiso 1 1 calc R . . H4B H 0.3200 -0.3365 -0.1500 0.050 Uiso 1 1 calc R . . C5 C 0.4094(4) -0.2611(3) 0.0123(3) 0.0397(7) Uani 1 1 d . . . H5A H 0.4226 -0.3381 0.0318 0.048 Uiso 1 1 calc R . . H5B H 0.4947 -0.1904 0.0623 0.048 Uiso 1 1 calc R . . C6 C 0.2717(4) -0.2510(3) 0.0206(3) 0.0390(7) Uani 1 1 d . . . H6A H 0.1877 -0.3255 -0.0247 0.047 Uiso 1 1 calc R . . H6B H 0.2816 -0.2470 0.0945 0.047 Uiso 1 1 calc R . . C7 C 0.1000(3) -0.0411(3) 0.3941(2) 0.0269(5) Uani 1 1 d . . . C8 C 0.2437(3) -0.0776(3) 0.5665(2) 0.0352(6) Uani 1 1 d . . . H8A H 0.2339 -0.0585 0.6340 0.042 Uiso 1 1 calc R . . H8B H 0.3238 -0.0081 0.5655 0.042 Uiso 1 1 calc R . . C9 C 0.2778(4) -0.1954(4) 0.5582(3) 0.0473(8) Uani 1 1 d . . . H9A H 0.3668 -0.1866 0.6203 0.057 Uiso 1 1 calc R . . H9B H 0.2970 -0.2095 0.4940 0.057 Uiso 1 1 calc R . . C10 C 0.1518(4) -0.3077(4) 0.5527(3) 0.0566(10) Uani 1 1 d . . . H10A H 0.1439 -0.3009 0.6218 0.068 Uiso 1 1 calc R . . H10B H 0.1722 -0.3844 0.5381 0.068 Uiso 1 1 calc R . . C11 C 0.0084(4) -0.3153(3) 0.4666(3) 0.0476(8) Uani 1 1 d . . . H11A H 0.0098 -0.3378 0.3964 0.057 Uiso 1 1 calc R . . H11B H -0.0723 -0.3809 0.4712 0.057 Uiso 1 1 calc R . . C12 C -0.0178(3) -0.1931(3) 0.4769(3) 0.0384(7) Uani 1 1 d . . . H12A H -0.1081 -0.1990 0.4174 0.046 Uiso 1 1 calc R . . H12B H -0.0297 -0.1745 0.5437 0.046 Uiso 1 1 calc R . . C13 C 0.3360(3) 0.3843(3) 0.32302(19) 0.0252(5) Uani 1 1 d . . . C14 C 0.3947(4) 0.6065(3) 0.3951(3) 0.0402(7) Uani 1 1 d . . . H14A H 0.4651 0.6548 0.4668 0.048 Uiso 1 1 calc R . . H14B H 0.2967 0.5777 0.3957 0.048 Uiso 1 1 calc R . . C15 C 0.3967(4) 0.6882(3) 0.3145(3) 0.0510(9) Uani 1 1 d . . . H15A H 0.3188 0.6424 0.2444 0.061 Uiso 1 1 calc R . . H15B H 0.3776 0.7632 0.3365 0.061 Uiso 1 1 calc R . . C16 C 0.5442(4) 0.7262(4) 0.3058(3) 0.0568(10) Uani 1 1 d . . . H16A H 0.6200 0.7825 0.3729 0.068 Uiso 1 1 calc R . . H16B H 0.5397 0.7714 0.2485 0.068 Uiso 1 1 calc R . . C17 C 0.5850(4) 0.6130(4) 0.2829(3) 0.0526(10) Uani 1 1 d . . . H17A H 0.5160 0.5615 0.2119 0.063 Uiso 1 1 calc R . . H17B H 0.6838 0.6398 0.2836 0.063 Uiso 1 1 calc R . . C18 C 0.5806(3) 0.5377(3) 0.3662(3) 0.0406(7) Uani 1 1 d . . . H18A H 0.6052 0.4636 0.3509 0.049 Uiso 1 1 calc R . . H18B H 0.6528 0.5878 0.4369 0.049 Uiso 1 1 calc R . . C19 C 0.1211(3) 0.3393(3) 0.9202(2) 0.0376(7) Uani 1 1 d . . . H19 H 0.0743 0.2484 0.8891 0.045 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 Sb 0.02677(10) 0.02529(10) 0.02214(9) 0.00451(7) 0.00905(7) 0.00915(7) Cl1 0.0500(5) 0.0661(6) 0.0827(7) 0.0160(5) 0.0421(5) 0.0224(5) Cl2 0.0691(6) 0.0603(6) 0.0505(5) 0.0104(5) 0.0099(5) 0.0322(5) Cl3 0.0556(5) 0.0832(7) 0.0448(5) 0.0081(5) 0.0269(4) 0.0307(5) S1 0.0537(5) 0.0381(4) 0.0308(3) 0.0149(3) 0.0229(3) 0.0273(4) S2 0.0364(4) 0.0310(4) 0.0276(3) 0.0098(3) 0.0116(3) 0.0135(3) S3 0.0303(3) 0.0362(4) 0.0226(3) 0.0067(3) 0.0069(3) 0.0059(3) S4 0.0298(3) 0.0371(4) 0.0277(3) 0.0068(3) 0.0074(3) 0.0112(3) S5 0.0262(3) 0.0312(4) 0.0353(3) 0.0020(3) 0.0139(3) 0.0097(3) S6 0.0311(4) 0.0354(4) 0.0386(4) 0.0033(3) 0.0192(3) 0.0102(3) N1 0.0354(13) 0.0328(13) 0.0306(11) 0.0074(10) 0.0181(10) 0.0141(11) N2 0.0332(12) 0.0313(13) 0.0290(11) 0.0103(10) 0.0134(10) 0.0133(10) N3 0.0317(12) 0.0273(12) 0.0325(12) 0.0030(10) 0.0129(10) 0.0067(10) C1 0.0210(12) 0.0299(14) 0.0249(12) 0.0065(11) 0.0083(10) 0.0079(11) C2 0.0388(16) 0.052(2) 0.0252(13) 0.0043(13) 0.0114(12) 0.0207(15) C3 0.0339(15) 0.0485(19) 0.0291(14) 0.0056(13) 0.0158(12) 0.0120(14) C4 0.0410(17) 0.054(2) 0.0407(16) 0.0063(15) 0.0256(14) 0.0207(16) C5 0.0461(18) 0.0420(18) 0.0425(16) 0.0124(14) 0.0244(15) 0.0224(15) C6 0.0538(19) 0.0340(16) 0.0468(17) 0.0144(14) 0.0333(16) 0.0216(15) C7 0.0337(14) 0.0257(13) 0.0254(12) 0.0056(10) 0.0139(11) 0.0134(11) C8 0.0384(16) 0.0418(17) 0.0254(13) 0.0108(12) 0.0112(12) 0.0149(14) C9 0.051(2) 0.061(2) 0.0486(19) 0.0235(17) 0.0239(16) 0.0370(18) C10 0.077(3) 0.043(2) 0.069(3) 0.0249(19) 0.038(2) 0.033(2) C11 0.062(2) 0.0313(17) 0.053(2) 0.0127(15) 0.0300(18) 0.0116(16) C12 0.0384(16) 0.0423(18) 0.0387(16) 0.0161(14) 0.0202(14) 0.0117(14) C13 0.0280(13) 0.0287(13) 0.0194(11) 0.0067(10) 0.0095(10) 0.0099(11) C14 0.0521(19) 0.0293(16) 0.0399(16) 0.0030(13) 0.0216(15) 0.0129(14) C15 0.071(2) 0.0379(19) 0.0388(17) 0.0121(15) 0.0145(17) 0.0199(18) C16 0.071(3) 0.043(2) 0.0358(17) 0.0120(15) 0.0162(17) -0.0039(19) C17 0.0473(19) 0.057(2) 0.0351(16) -0.0019(16) 0.0205(15) -0.0097(17) C18 0.0311(15) 0.0376(17) 0.0408(16) -0.0029(14) 0.0134(13) -0.0006(13) C19 0.0383(16) 0.0374(17) 0.0370(15) 0.0032(13) 0.0155(13) 0.0141(14) _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 Sb S1 2.5241(8) . ? Sb S3 2.5385(7) . ? Sb S5 2.5424(7) . ? Cl1 C19 1.738(3) . ? Cl2 C19 1.756(3) . ? Cl3 C19 1.745(3) . ? S1 C1 1.750(3) . ? S2 C1 1.691(3) . ? S3 C7 1.740(3) . ? S4 C7 1.702(3) . ? S5 C13 1.735(3) . ? S6 C13 1.702(3) . ? N1 C1 1.328(3) . ? N1 C6 1.468(4) . ? N1 C2 1.465(3) . ? N2 C7 1.320(3) . ? N2 C12 1.464(4) . ? N2 C8 1.467(4) . ? N3 C13 1.332(3) . ? N3 C14 1.456(4) . ? N3 C18 1.465(4) . ? C2 C3 1.509(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.515(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.518(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.511(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C8 C9 1.495(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.525(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.509(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.504(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C14 C15 1.522(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.520(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.515(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 C18 1.507(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Sb S3 80.45(2) . . ? S1 Sb S5 92.01(3) . . ? S3 Sb S5 81.37(2) . . ? C1 S1 Sb 95.83(9) . . ? C7 S3 Sb 95.23(9) . . ? C13 S5 Sb 94.27(9) . . ? C1 N1 C6 123.6(2) . . ? C1 N1 C2 123.1(3) . . ? C6 N1 C2 113.3(2) . . ? C7 N2 C12 123.1(2) . . ? C7 N2 C8 123.8(2) . . ? C12 N2 C8 111.8(2) . . ? C13 N3 C14 123.3(2) . . ? C13 N3 C18 123.3(3) . . ? C14 N3 C18 112.1(2) . . ? N1 C1 S2 124.0(2) . . ? N1 C1 S1 118.4(2) . . ? S2 C1 S1 117.58(16) . . ? N1 C2 C3 110.8(2) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 111.9(3) . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 109.4(3) . . ? C3 C4 H4A 109.8 . . ? C5 C4 H4A 109.8 . . ? C3 C4 H4B 109.8 . . ? C5 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? C6 C5 C4 110.5(3) . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N1 C6 C5 110.9(2) . . ? N1 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N2 C7 S4 123.3(2) . . ? N2 C7 S3 118.6(2) . . ? S4 C7 S3 118.09(15) . . ? N2 C8 C9 109.4(3) . . ? N2 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? N2 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C8 C9 C10 111.6(3) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C9 C10 C11 111.0(3) . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 111.4(3) . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? N2 C12 C11 109.9(3) . . ? N2 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? N2 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N3 C13 S6 122.4(2) . . ? N3 C13 S5 117.9(2) . . ? S6 C13 S5 119.78(16) . . ? N3 C14 C15 109.1(3) . . ? N3 C14 H14A 109.9 . . ? C15 C14 H14A 109.9 . . ? N3 C14 H14B 109.9 . . ? C15 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C16 C15 C14 110.9(3) . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C17 111.1(3) . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C16 109.6(3) . . ? C18 C17 H17A 109.7 . . ? C16 C17 H17A 109.7 . . ? C18 C17 H17B 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? N3 C18 C17 109.3(3) . . ? N3 C18 H18A 109.8 . . ? C17 C18 H18A 109.8 . . ? N3 C18 H18B 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? Cl1 C19 Cl3 109.94(17) . . ? Cl1 C19 Cl2 110.97(18) . . ? Cl3 C19 Cl2 110.86(18) . . ? Cl1 C19 H19 108.3 . . ? Cl3 C19 H19 108.3 . . ? Cl2 C19 H19 108.3 . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 30.1 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.79 _refine_diff_density_min -0.48 _refine_diff_density_rms 0.100 data_Sb{S2CN(CH2)6}3 _database_code_depnum_ccdc_archive 'CCDC 253920' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C21 H36 N3 S6 Sb' _chemical_formula_weight 644.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M P21/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 10.9080(6) _cell_length_b 13.5802(7) _cell_length_c 18.8708(10) _cell_angle_alpha 90 _cell_angle_beta 99.305(1) _cell_angle_gamma 90 _cell_volume 2758.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1985 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 22.3 _exptl_crystal_description plate _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.298 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23109 _diffrn_reflns_av_R_equivalents 0.082 _diffrn_reflns_av_sigmaI/netI 0.107 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.9 _diffrn_reflns_theta_max 30.1 _reflns_number_total 8047 _reflns_number_gt 4663 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.046P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8047 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.135 _refine_ls_R_factor_gt 0.071 _refine_ls_wR_factor_ref 0.135 _refine_ls_wR_factor_gt 0.115 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _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 Sb Sb 0.28915(3) 0.24504(2) 0.081230(18) 0.03213(11) Uani 1 1 d . . . S1 S 0.16394(12) 0.31334(10) -0.03113(7) 0.0359(3) Uani 1 1 d . . . S2 S 0.04968(16) 0.34447(13) 0.09947(8) 0.0540(4) Uani 1 1 d . . . S3 S 0.41924(12) 0.17548(10) -0.00582(7) 0.0343(3) Uani 1 1 d . . . S4 S 0.20016(15) 0.05998(11) 0.02100(9) 0.0471(4) Uani 1 1 d . . . S5 S 0.41476(13) 0.40341(10) 0.07753(7) 0.0373(3) Uani 1 1 d . . . S6 S 0.53458(13) 0.25436(9) 0.18142(7) 0.0371(3) Uani 1 1 d . . . N1 N -0.0636(4) 0.3794(3) -0.0342(2) 0.0355(11) Uani 1 1 d . . . N2 N 0.3446(4) 0.0111(3) -0.0739(2) 0.0318(10) Uani 1 1 d . . . N3 N 0.6371(4) 0.4253(3) 0.1567(2) 0.0329(10) Uani 1 1 d . . . C1 C 0.0370(5) 0.3493(3) 0.0090(3) 0.0327(12) Uani 1 1 d . . . C2 C -0.0740(5) 0.3753(4) -0.1128(3) 0.0466(15) Uani 1 1 d . . . H2A H 0.0058 0.3944 -0.1262 0.056 Uiso 1 1 calc R . . H2B H -0.1363 0.4233 -0.1340 0.056 Uiso 1 1 calc R . . C3 C -0.1101(7) 0.2741(5) -0.1441(3) 0.063(2) Uani 1 1 d . . . H3A H -0.0341 0.2381 -0.1490 0.076 Uiso 1 1 calc R . . H3B H -0.1576 0.2827 -0.1924 0.076 Uiso 1 1 calc R . . C4 C -0.1864(9) 0.2115(6) -0.1004(4) 0.088(3) Uani 1 1 d . . . H4A H -0.2187 0.1544 -0.1293 0.106 Uiso 1 1 calc R . . H4B H -0.1315 0.1868 -0.0579 0.106 Uiso 1 1 calc R . . C5 C -0.2911(7) 0.2632(6) -0.0769(5) 0.087(3) Uani 1 1 d . . . H5A H -0.3554 0.2143 -0.0721 0.104 Uiso 1 1 calc R . . H5B H -0.3260 0.3086 -0.1152 0.104 Uiso 1 1 calc R . . C6 C -0.2654(6) 0.3216(5) -0.0068(4) 0.0628(19) Uani 1 1 d . . . H6A H -0.3443 0.3473 0.0039 0.075 Uiso 1 1 calc R . . H6B H -0.2318 0.2766 0.0321 0.075 Uiso 1 1 calc R . . C7 C -0.1761(5) 0.4066(4) -0.0074(4) 0.0518(17) Uani 1 1 d . . . H7A H -0.2178 0.4595 -0.0373 0.062 Uiso 1 1 calc R . . H7B H -0.1539 0.4321 0.0416 0.062 Uiso 1 1 calc R . . C8 C 0.3205(5) 0.0736(4) -0.0244(3) 0.0314(12) Uani 1 1 d . . . C9 C 0.4474(5) 0.0224(4) -0.1143(3) 0.0382(13) Uani 1 1 d . . . H9A H 0.4780 -0.0430 -0.1247 0.046 Uiso 1 1 calc R . . H9B H 0.5155 0.0574 -0.0844 0.046 Uiso 1 1 calc R . . C10 C 0.4122(6) 0.0773(5) -0.1836(3) 0.0523(16) Uani 1 1 d . . . H10A H 0.4836 0.0774 -0.2091 0.063 Uiso 1 1 calc R . . H10B H 0.3948 0.1459 -0.1724 0.063 Uiso 1 1 calc R . . C11 C 0.3020(8) 0.0368(7) -0.2328(4) 0.100(3) Uani 1 1 d . . . H11A H 0.2913 0.0758 -0.2770 0.120 Uiso 1 1 calc R . . H11B H 0.3225 -0.0304 -0.2456 0.120 Uiso 1 1 calc R . . C12 C 0.1873(8) 0.0336(8) -0.2088(4) 0.112(4) Uani 1 1 d . . . H12A H 0.1240 0.0278 -0.2518 0.134 Uiso 1 1 calc R . . H12B H 0.1756 0.0984 -0.1880 0.134 Uiso 1 1 calc R . . C13 C 0.1545(6) -0.0431(5) -0.1550(4) 0.070(2) Uani 1 1 d . . . H13A H 0.1241 -0.1026 -0.1815 0.084 Uiso 1 1 calc R . . H13B H 0.0863 -0.0171 -0.1325 0.084 Uiso 1 1 calc R . . C14 C 0.2588(6) -0.0712(4) -0.0971(3) 0.0527(17) Uani 1 1 d . . . H14A H 0.2242 -0.0954 -0.0555 0.063 Uiso 1 1 calc R . . H14B H 0.3058 -0.1252 -0.1144 0.063 Uiso 1 1 calc R . . C15 C 0.5399(5) 0.3655(3) 0.1417(2) 0.0297(11) Uani 1 1 d . . . C16 C 0.7465(5) 0.3935(4) 0.2078(3) 0.0469(16) Uani 1 1 d . . . H16A H 0.7931 0.3458 0.1837 0.056 Uiso 1 1 calc R . . H16B H 0.7177 0.3594 0.2478 0.056 Uiso 1 1 calc R . . C17 C 0.8336(5) 0.4744(4) 0.2379(3) 0.0471(15) Uani 1 1 d . . . H17A H 0.8982 0.4456 0.2741 0.056 Uiso 1 1 calc R . . H17B H 0.8746 0.4998 0.1991 0.056 Uiso 1 1 calc R . . C18 C 0.7762(6) 0.5612(5) 0.2720(3) 0.0543(17) Uani 1 1 d . . . H18A H 0.7112 0.5361 0.2974 0.065 Uiso 1 1 calc R . . H18B H 0.8404 0.5912 0.3079 0.065 Uiso 1 1 calc R . . C19 C 0.7209(6) 0.6402(4) 0.2209(3) 0.0538(17) Uani 1 1 d . . . H19A H 0.7864 0.6666 0.1963 0.065 Uiso 1 1 calc R . . H19B H 0.6922 0.6940 0.2487 0.065 Uiso 1 1 calc R . . C20 C 0.6141(5) 0.6077(4) 0.1649(3) 0.0474(16) Uani 1 1 d . . . H20A H 0.5880 0.6633 0.1329 0.057 Uiso 1 1 calc R . . H20B H 0.5439 0.5901 0.1889 0.057 Uiso 1 1 calc R . . C21 C 0.6439(5) 0.5207(4) 0.1199(3) 0.0411(14) Uani 1 1 d . . . H21A H 0.5853 0.5200 0.0747 0.049 Uiso 1 1 calc R . . H21B H 0.7276 0.5290 0.1083 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 Sb 0.03463(19) 0.03670(19) 0.02496(17) 0.00186(17) 0.00452(13) 0.00040(17) S1 0.0321(7) 0.0469(8) 0.0286(7) 0.0037(6) 0.0045(6) 0.0030(6) S2 0.0504(10) 0.0780(11) 0.0344(8) -0.0140(8) 0.0091(7) 0.0073(8) S3 0.0324(7) 0.0381(7) 0.0329(7) -0.0022(6) 0.0065(6) -0.0037(6) S4 0.0511(10) 0.0454(8) 0.0496(9) -0.0038(7) 0.0225(8) -0.0133(7) S5 0.0401(8) 0.0348(7) 0.0336(8) 0.0063(6) -0.0047(6) 0.0017(6) S6 0.0430(8) 0.0320(6) 0.0343(7) 0.0058(6) 0.0005(6) 0.0014(6) N1 0.033(3) 0.026(2) 0.047(3) -0.002(2) 0.004(2) 0.0012(18) N2 0.036(3) 0.031(2) 0.028(2) 0.004(2) 0.0058(19) 0.0003(19) N3 0.037(3) 0.035(2) 0.026(2) 0.006(2) 0.0038(19) -0.001(2) C1 0.030(3) 0.024(2) 0.043(3) -0.008(2) 0.001(2) 0.001(2) C2 0.035(3) 0.055(4) 0.048(4) 0.024(3) 0.001(3) 0.004(3) C3 0.064(5) 0.089(5) 0.036(3) -0.009(4) 0.006(3) -0.034(4) C4 0.117(8) 0.076(5) 0.074(6) -0.025(5) 0.023(5) -0.041(5) C5 0.052(4) 0.096(6) 0.117(7) -0.045(6) 0.030(5) -0.030(4) C6 0.045(4) 0.071(5) 0.077(5) -0.012(4) 0.025(4) -0.006(3) C7 0.040(4) 0.046(3) 0.070(5) -0.009(3) 0.010(3) 0.013(3) C8 0.034(3) 0.031(3) 0.028(3) 0.004(2) -0.001(2) 0.005(2) C9 0.037(3) 0.037(3) 0.042(3) -0.003(3) 0.010(3) 0.006(2) C10 0.047(4) 0.067(4) 0.043(4) 0.015(3) 0.008(3) 0.004(3) C11 0.080(6) 0.167(9) 0.047(5) 0.034(6) -0.012(4) -0.014(6) C12 0.050(5) 0.229(12) 0.049(5) 0.033(7) -0.011(4) 0.006(6) C13 0.050(4) 0.091(5) 0.067(5) -0.026(4) 0.001(4) -0.024(4) C14 0.060(4) 0.040(3) 0.060(4) -0.013(3) 0.020(4) -0.018(3) C15 0.036(3) 0.035(3) 0.018(2) 0.001(2) 0.003(2) 0.002(2) C16 0.043(4) 0.052(3) 0.041(3) 0.012(3) -0.008(3) -0.001(3) C17 0.039(3) 0.057(4) 0.041(3) 0.000(3) -0.007(3) -0.002(3) C18 0.061(4) 0.068(4) 0.032(3) -0.008(3) 0.002(3) -0.002(3) C19 0.073(5) 0.051(4) 0.037(4) -0.007(3) 0.009(3) 0.004(3) C20 0.045(4) 0.039(3) 0.058(4) 0.017(3) 0.010(3) 0.001(3) C21 0.047(4) 0.043(3) 0.032(3) 0.010(3) 0.001(3) -0.015(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 Sb S1 2.5069(13) . ? Sb S3 2.5215(14) . ? Sb S5 2.5571(14) . ? Sb S4 2.8623(15) . ? S1 C1 1.751(6) . ? S2 C1 1.692(6) . ? S3 C8 1.753(5) . ? S4 C8 1.690(6) . ? S5 C15 1.749(5) . ? S6 C15 1.690(5) . ? N1 C1 1.321(6) . ? N1 C2 1.470(7) . ? N1 C7 1.449(7) . ? N2 C8 1.319(6) . ? N2 C9 1.463(7) . ? N2 C14 1.478(6) . ? N3 C15 1.329(6) . ? N3 C21 1.477(6) . ? N3 C16 1.473(6) . ? C2 C3 1.522(8) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.522(10) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.468(11) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.529(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.511(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C9 C10 1.500(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.499(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.398(11) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 C13 1.537(11) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 C14 1.494(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C16 C17 1.502(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 C18 1.526(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 C19 1.503(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.506(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.521(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 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 S1 Sb S3 82.80(4) . . ? S1 Sb S5 83.50(4) . . ? S3 Sb S5 86.38(5) . . ? S1 Sb S4 83.43(5) . . ? S3 Sb S4 66.60(4) . . ? S5 Sb S4 151.21(5) . . ? C1 S1 Sb 95.65(18) . . ? C8 S3 Sb 91.95(19) . . ? C8 S4 Sb 82.18(18) . . ? C15 S5 Sb 95.44(17) . . ? C1 N1 C2 122.1(5) . . ? C1 N1 C7 122.0(5) . . ? C2 N1 C7 115.5(4) . . ? C8 N2 C9 124.0(4) . . ? C8 N2 C14 120.5(5) . . ? C9 N2 C14 115.3(4) . . ? C15 N3 C21 122.3(4) . . ? C15 N3 C16 119.7(4) . . ? C21 N3 C16 117.9(4) . . ? N1 C1 S2 123.9(4) . . ? N1 C1 S1 117.1(4) . . ? S2 C1 S1 119.0(3) . . ? N1 C2 C3 113.5(5) . . ? N1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? N1 C2 H2B 108.9 . . ? C3 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 115.0(6) . . ? C2 C3 H3A 108.5 . . ? C4 C3 H3A 108.5 . . ? C2 C3 H3B 108.5 . . ? C4 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C5 C4 C3 114.7(7) . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4B 108.6 . . ? C3 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? C4 C5 C6 117.8(7) . . ? C4 C5 H5A 107.9 . . ? C6 C5 H5A 107.9 . . ? C4 C5 H5B 107.9 . . ? C6 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? C7 C6 C5 114.7(6) . . ? C7 C6 H6A 108.6 . . ? C5 C6 H6A 108.6 . . ? C7 C6 H6B 108.6 . . ? C5 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? N1 C7 C6 113.0(5) . . ? N1 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N2 C8 S4 123.2(4) . . ? N2 C8 S3 117.6(4) . . ? S4 C8 S3 119.1(3) . . ? N2 C9 C10 113.3(4) . . ? N2 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N2 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C9 C10 C11 115.1(6) . . ? C9 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? C9 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C12 C11 C10 118.7(8) . . ? C12 C11 H11A 107.6 . . ? C10 C11 H11A 107.6 . . ? C12 C11 H11B 107.6 . . ? C10 C11 H11B 107.6 . . ? H11A C11 H11B 107.1 . . ? C11 C12 C13 123.4(8) . . ? C11 C12 H12A 106.5 . . ? C13 C12 H12A 106.5 . . ? C11 C12 H12B 106.5 . . ? C13 C12 H12B 106.5 . . ? H12A C12 H12B 106.5 . . ? C12 C13 C14 115.2(6) . . ? C12 C13 H13A 108.5 . . ? C14 C13 H13A 108.5 . . ? C12 C13 H13B 108.5 . . ? C14 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? N2 C14 C13 113.2(5) . . ? N2 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? N2 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.8 . . ? N3 C15 S6 122.3(4) . . ? N3 C15 S5 118.3(4) . . ? S6 C15 S5 119.4(3) . . ? N3 C16 C17 115.4(4) . . ? N3 C16 H16A 108.4 . . ? C17 C16 H16A 108.4 . . ? N3 C16 H16B 108.4 . . ? C17 C16 H16B 108.4 . . ? H16A C16 H16B 107.5 . . ? C18 C17 C16 116.6(5) . . ? C18 C17 H17A 108.1 . . ? C16 C17 H17A 108.1 . . ? C18 C17 H17B 108.1 . . ? C16 C17 H17B 108.1 . . ? H17A C17 H17B 107.3 . . ? C19 C18 C17 115.5(5) . . ? C19 C18 H18A 108.4 . . ? C17 C18 H18A 108.4 . . ? C19 C18 H18B 108.4 . . ? C17 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? C18 C19 C20 115.2(5) . . ? C18 C19 H19A 108.5 . . ? C20 C19 H19A 108.5 . . ? C18 C19 H19B 108.5 . . ? C20 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C19 C20 C21 114.1(5) . . ? C19 C20 H20A 108.7 . . ? C21 C20 H20A 108.7 . . ? C19 C20 H20B 108.7 . . ? C21 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? N3 C21 C20 112.8(5) . . ? N3 C21 H21A 109.0 . . ? C20 C21 H21A 109.0 . . ? N3 C21 H21B 109.0 . . ? C20 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.1 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.17 _refine_diff_density_min -0.51 _refine_diff_density_rms 0.129 data_Sb{S2CN(CH2Ph)2}3 _database_code_depnum_ccdc_archive 'CCDC 253921' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C45 H42 N3 S6 Sb' _chemical_formula_weight 938.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8634(6) _cell_length_b 13.1293(7) _cell_length_c 17.1450(9) _cell_angle_alpha 93.689(1) _cell_angle_beta 99.276(1) _cell_angle_gamma 105.504(1) _cell_volume 2098.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5366 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.993 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17755 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_av_sigmaI/netI 0.055 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.2 _diffrn_reflns_theta_max 30.0 _reflns_number_total 12028 _reflns_number_gt 9708 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.052P)^2^+0.087P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12028 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.058 _refine_ls_R_factor_gt 0.045 _refine_ls_wR_factor_ref 0.107 _refine_ls_wR_factor_gt 0.098 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _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 Sb Sb 0.137781(19) 0.203949(13) 0.220703(10) 0.02895(6) Uani 1 1 d . . . S1 S 0.33520(7) 0.36694(5) 0.28755(4) 0.03300(15) Uani 1 1 d . . . S2 S 0.04166(8) 0.35375(6) 0.31546(5) 0.04523(19) Uani 1 1 d . . . S3 S 0.32268(8) 0.16503(6) 0.14459(4) 0.03747(16) Uani 1 1 d . . . S4 S 0.13161(8) 0.28607(6) 0.06979(4) 0.03894(16) Uani 1 1 d . . . S5 S 0.24874(8) 0.10394(5) 0.32822(4) 0.03566(15) Uani 1 1 d . . . S6 S -0.00757(9) -0.02500(6) 0.21245(5) 0.0514(2) Uani 1 1 d . . . N1 N 0.2755(2) 0.50281(17) 0.38891(12) 0.0280(4) Uani 1 1 d . . . N2 N 0.3080(2) 0.21295(19) -0.00466(12) 0.0321(5) Uani 1 1 d . . . N3 N 0.1624(2) -0.10711(17) 0.31012(13) 0.0307(5) Uani 1 1 d . . . C1 C 0.2198(3) 0.4167(2) 0.33669(15) 0.0281(5) Uani 1 1 d . . . C2 C 0.4303(3) 0.5514(2) 0.41526(15) 0.0301(5) Uani 1 1 d . . . H2A H 0.4804 0.5011 0.3984 0.036 Uiso 1 1 calc R . . H2B H 0.4510 0.5621 0.4735 0.036 Uiso 1 1 calc R . . C3 C 0.4907(3) 0.6563(2) 0.38468(15) 0.0288(5) Uani 1 1 d . . . C4 C 0.4767(3) 0.6654(2) 0.30377(16) 0.0361(6) Uani 1 1 d . . . H4 H 0.4189 0.6081 0.2669 0.043 Uiso 1 1 calc R . . C5 C 0.5478(4) 0.7588(2) 0.27755(19) 0.0467(8) Uani 1 1 d . . . H5 H 0.5377 0.7646 0.2227 0.056 Uiso 1 1 calc R . . C6 C 0.6329(4) 0.8430(2) 0.3303(2) 0.0493(8) Uani 1 1 d . . . H6 H 0.6821 0.9055 0.3117 0.059 Uiso 1 1 calc R . . C7 C 0.6461(3) 0.8357(2) 0.4105(2) 0.0467(8) Uani 1 1 d . . . H7 H 0.7033 0.8936 0.4470 0.056 Uiso 1 1 calc R . . C8 C 0.5747(3) 0.7427(2) 0.43746(17) 0.0371(6) Uani 1 1 d . . . H8 H 0.5834 0.7382 0.4925 0.044 Uiso 1 1 calc R . . C9 C 0.1863(3) 0.5478(2) 0.43497(16) 0.0334(6) Uani 1 1 d . . . H9A H 0.0858 0.5218 0.4084 0.040 Uiso 1 1 calc R . . H9B H 0.2158 0.6255 0.4370 0.040 Uiso 1 1 calc R . . C10 C 0.2010(3) 0.5168(2) 0.51873(16) 0.0327(6) Uani 1 1 d . . . C11 C 0.2526(3) 0.5941(3) 0.58329(18) 0.0441(7) Uani 1 1 d . . . H11 H 0.2772 0.6663 0.5751 0.053 Uiso 1 1 calc R . . C12 C 0.2682(4) 0.5657(3) 0.66002(19) 0.0514(8) Uani 1 1 d . . . H12 H 0.3022 0.6190 0.7035 0.062 Uiso 1 1 calc R . . C13 C 0.2344(4) 0.4604(3) 0.67310(19) 0.0497(8) Uani 1 1 d . . . H13 H 0.2464 0.4413 0.7251 0.060 Uiso 1 1 calc R . . C14 C 0.1829(4) 0.3835(3) 0.60915(19) 0.0463(8) Uani 1 1 d . . . H14 H 0.1595 0.3114 0.6177 0.056 Uiso 1 1 calc R . . C15 C 0.1648(3) 0.4108(2) 0.53216(18) 0.0383(6) Uani 1 1 d . . . H15 H 0.1279 0.3573 0.4890 0.046 Uiso 1 1 calc R . . C16 C 0.2573(3) 0.2215(2) 0.06227(15) 0.0310(5) Uani 1 1 d . . . C17 C 0.2450(3) 0.2492(2) -0.07866(15) 0.0333(6) Uani 1 1 d . . . H17A H 0.1412 0.2324 -0.0816 0.040 Uiso 1 1 calc R . . H17B H 0.2615 0.2081 -0.1242 0.040 Uiso 1 1 calc R . . C18 C 0.3013(3) 0.3657(2) -0.08708(14) 0.0322(6) Uani 1 1 d . . . C19 C 0.4408(3) 0.4095(3) -0.09890(16) 0.0408(7) Uani 1 1 d . . . H19 H 0.5042 0.3672 -0.0976 0.049 Uiso 1 1 calc R . . C20 C 0.4865(4) 0.5149(3) -0.11248(18) 0.0489(8) Uani 1 1 d . . . H20 H 0.5808 0.5437 -0.1201 0.059 Uiso 1 1 calc R . . C21 C 0.3953(4) 0.5774(3) -0.11494(17) 0.0466(8) Uani 1 1 d . . . H21 H 0.4270 0.6488 -0.1248 0.056 Uiso 1 1 calc R . . C22 C 0.2566(4) 0.5361(3) -0.10299(18) 0.0456(7) Uani 1 1 d . . . H22 H 0.1939 0.5790 -0.1043 0.055 Uiso 1 1 calc R . . C23 C 0.2113(3) 0.4303(2) -0.08902(16) 0.0388(6) Uani 1 1 d . . . H23 H 0.1172 0.4021 -0.0807 0.047 Uiso 1 1 calc R . . C24 C 0.4228(3) 0.1623(2) -0.01135(16) 0.0350(6) Uani 1 1 d . . . H24A H 0.4649 0.1506 0.0419 0.042 Uiso 1 1 calc R . . H24B H 0.4981 0.2109 -0.0329 0.042 Uiso 1 1 calc R . . C25 C 0.3723(3) 0.0581(2) -0.06343(15) 0.0325(6) Uani 1 1 d . . . C26 C 0.4365(3) 0.0426(3) -0.12798(16) 0.0406(7) Uani 1 1 d . . . H26 H 0.5101 0.0984 -0.1396 0.049 Uiso 1 1 calc R . . C27 C 0.3933(4) -0.0539(3) -0.1754(2) 0.0575(10) Uani 1 1 d . . . H27 H 0.4368 -0.0628 -0.2192 0.069 Uiso 1 1 calc R . . C28 C 0.2887(4) -0.1355(3) -0.1590(2) 0.0664(12) Uani 1 1 d . . . H28 H 0.2595 -0.2009 -0.1914 0.080 Uiso 1 1 calc R . . C29 C 0.2251(4) -0.1225(3) -0.0944(3) 0.0629(11) Uani 1 1 d . . . H29 H 0.1535 -0.1796 -0.0828 0.075 Uiso 1 1 calc R . . C30 C 0.2652(3) -0.0266(3) -0.0466(2) 0.0489(8) Uani 1 1 d . . . H30 H 0.2206 -0.0185 -0.0031 0.059 Uiso 1 1 calc R . . C31 C 0.1345(3) -0.0194(2) 0.28488(15) 0.0322(5) Uani 1 1 d . . . C32 C 0.0667(3) -0.2138(2) 0.28056(17) 0.0349(6) Uani 1 1 d . . . H32A H -0.0276 -0.2071 0.2574 0.042 Uiso 1 1 calc R . . H32B H 0.0551 -0.2554 0.3257 0.042 Uiso 1 1 calc R . . C33 C 0.1182(3) -0.2740(2) 0.21913(15) 0.0300(5) Uani 1 1 d . . . C34 C 0.1709(3) -0.2270(2) 0.15580(17) 0.0394(6) Uani 1 1 d . . . H34 H 0.1830 -0.1540 0.1527 0.047 Uiso 1 1 calc R . . C35 C 0.2057(3) -0.2881(3) 0.09715(18) 0.0476(8) Uani 1 1 d . . . H35 H 0.2397 -0.2564 0.0538 0.057 Uiso 1 1 calc R . . C36 C 0.1909(3) -0.3948(3) 0.10180(18) 0.0477(8) Uani 1 1 d . . . H36 H 0.2155 -0.4355 0.0621 0.057 Uiso 1 1 calc R . . C37 C 0.1396(3) -0.4419(3) 0.16520(18) 0.0442(7) Uani 1 1 d . . . H37 H 0.1296 -0.5146 0.1688 0.053 Uiso 1 1 calc R . . C38 C 0.1034(3) -0.3817(2) 0.22315(16) 0.0348(6) Uani 1 1 d . . . H38 H 0.0682 -0.4141 0.2660 0.042 Uiso 1 1 calc R . . C39 C 0.2825(3) -0.1048(2) 0.37328(15) 0.0323(5) Uani 1 1 d . . . H39A H 0.3596 -0.0396 0.3737 0.039 Uiso 1 1 calc R . . H39B H 0.3192 -0.1653 0.3615 0.039 Uiso 1 1 calc R . . C40 C 0.2432(3) -0.1090(2) 0.45488(15) 0.0318(6) Uani 1 1 d . . . C41 C 0.1082(3) -0.1082(2) 0.46844(18) 0.0394(6) Uani 1 1 d . . . H41 H 0.0372 -0.1038 0.4261 0.047 Uiso 1 1 calc R . . C42 C 0.0785(4) -0.1139(3) 0.5453(2) 0.0490(8) Uani 1 1 d . . . H42 H -0.0131 -0.1142 0.5543 0.059 Uiso 1 1 calc R . . C43 C 0.1816(4) -0.1192(2) 0.60762(18) 0.0497(9) Uani 1 1 d . . . H43 H 0.1605 -0.1232 0.6591 0.060 Uiso 1 1 calc R . . C44 C 0.3162(4) -0.1185(2) 0.59484(18) 0.0461(8) Uani 1 1 d . . . H44 H 0.3875 -0.1210 0.6377 0.055 Uiso 1 1 calc R . . C45 C 0.3462(3) -0.1142(2) 0.51866(17) 0.0380(6) Uani 1 1 d . . . H45 H 0.4378 -0.1147 0.5101 0.046 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 Sb 0.03264(10) 0.02566(9) 0.02980(9) 0.00486(6) 0.00819(7) 0.00849(7) S1 0.0299(3) 0.0281(3) 0.0427(4) 0.0009(3) 0.0153(3) 0.0068(3) S2 0.0286(4) 0.0434(4) 0.0618(5) -0.0062(4) 0.0162(3) 0.0051(3) S3 0.0431(4) 0.0454(4) 0.0319(3) 0.0076(3) 0.0094(3) 0.0239(3) S4 0.0406(4) 0.0468(4) 0.0392(4) 0.0132(3) 0.0143(3) 0.0231(3) S5 0.0418(4) 0.0244(3) 0.0327(3) 0.0021(3) -0.0028(3) 0.0017(3) S6 0.0502(5) 0.0295(4) 0.0598(5) 0.0002(3) -0.0205(4) 0.0053(3) N1 0.0301(11) 0.0265(10) 0.0311(10) 0.0076(8) 0.0112(9) 0.0098(9) N2 0.0297(12) 0.0388(13) 0.0268(10) 0.0008(9) 0.0036(9) 0.0097(10) N3 0.0345(12) 0.0241(10) 0.0309(11) 0.0035(8) 0.0048(9) 0.0044(9) C1 0.0277(12) 0.0248(12) 0.0334(12) 0.0070(10) 0.0106(10) 0.0064(10) C2 0.0309(13) 0.0315(13) 0.0298(12) 0.0068(10) 0.0045(10) 0.0117(11) C3 0.0281(13) 0.0252(12) 0.0344(13) 0.0036(10) 0.0075(10) 0.0090(10) C4 0.0438(16) 0.0304(14) 0.0320(13) 0.0050(11) 0.0062(12) 0.0073(12) C5 0.063(2) 0.0378(16) 0.0422(16) 0.0118(13) 0.0206(15) 0.0102(15) C6 0.055(2) 0.0280(15) 0.066(2) 0.0087(14) 0.0247(17) 0.0049(14) C7 0.0426(17) 0.0301(15) 0.060(2) -0.0085(13) 0.0098(15) 0.0017(13) C8 0.0385(15) 0.0347(14) 0.0375(14) -0.0022(11) 0.0062(12) 0.0113(12) C9 0.0422(15) 0.0281(13) 0.0379(14) 0.0068(11) 0.0147(12) 0.0183(12) C10 0.0334(14) 0.0321(14) 0.0383(14) 0.0053(11) 0.0157(11) 0.0135(11) C11 0.0480(18) 0.0368(16) 0.0475(17) -0.0039(13) 0.0128(14) 0.0115(14) C12 0.052(2) 0.065(2) 0.0385(16) -0.0091(15) 0.0104(15) 0.0213(17) C13 0.0422(18) 0.080(3) 0.0387(16) 0.0162(16) 0.0185(14) 0.0284(17) C14 0.0487(18) 0.0499(19) 0.0511(18) 0.0210(15) 0.0260(15) 0.0191(15) C15 0.0413(16) 0.0361(15) 0.0407(15) 0.0059(12) 0.0165(13) 0.0105(12) C16 0.0292(13) 0.0327(13) 0.0296(12) 0.0012(10) 0.0043(10) 0.0075(11) C17 0.0290(13) 0.0403(15) 0.0260(12) 0.0019(11) 0.0004(10) 0.0052(11) C18 0.0323(14) 0.0393(15) 0.0203(11) 0.0011(10) 0.0018(10) 0.0045(11) C19 0.0361(15) 0.0488(18) 0.0339(14) 0.0000(12) 0.0083(12) 0.0061(13) C20 0.0408(17) 0.056(2) 0.0393(16) 0.0040(14) 0.0102(13) -0.0061(15) C21 0.054(2) 0.0399(17) 0.0342(15) 0.0038(13) 0.0026(14) -0.0022(15) C22 0.054(2) 0.0456(18) 0.0401(16) 0.0107(14) 0.0089(14) 0.0168(15) C23 0.0354(15) 0.0476(17) 0.0318(13) 0.0070(12) 0.0061(12) 0.0086(13) C24 0.0285(13) 0.0431(16) 0.0333(13) -0.0007(11) 0.0065(11) 0.0105(12) C25 0.0299(13) 0.0392(15) 0.0292(12) 0.0056(11) 0.0038(10) 0.0118(11) C26 0.0472(17) 0.0488(18) 0.0316(13) 0.0065(12) 0.0074(13) 0.0229(14) C27 0.072(3) 0.066(2) 0.0413(17) -0.0072(16) -0.0039(17) 0.042(2) C28 0.070(3) 0.053(2) 0.067(2) -0.0174(19) -0.028(2) 0.032(2) C29 0.044(2) 0.043(2) 0.087(3) 0.0097(19) -0.0165(19) 0.0030(16) C30 0.0379(17) 0.055(2) 0.0510(18) 0.0117(16) 0.0042(14) 0.0091(15) C31 0.0362(14) 0.0260(12) 0.0314(13) 0.0028(10) 0.0040(11) 0.0052(11) C32 0.0404(15) 0.0232(12) 0.0398(14) 0.0031(11) 0.0121(12) 0.0043(11) C33 0.0275(13) 0.0319(13) 0.0289(12) 0.0023(10) 0.0029(10) 0.0074(10) C34 0.0371(16) 0.0389(16) 0.0424(15) 0.0103(13) 0.0116(13) 0.0074(13) C35 0.0372(16) 0.069(2) 0.0377(15) 0.0091(15) 0.0124(13) 0.0123(16) C36 0.0390(17) 0.065(2) 0.0406(16) -0.0102(15) 0.0014(13) 0.0237(16) C37 0.0473(18) 0.0424(17) 0.0445(16) -0.0023(13) -0.0007(14) 0.0224(14) C38 0.0398(15) 0.0337(14) 0.0314(13) 0.0036(11) 0.0027(11) 0.0132(12) C39 0.0354(14) 0.0307(13) 0.0319(13) 0.0069(10) 0.0060(11) 0.0106(11) C40 0.0424(15) 0.0207(12) 0.0321(13) 0.0033(10) 0.0088(11) 0.0076(11) C41 0.0382(16) 0.0365(15) 0.0398(15) -0.0002(12) 0.0078(13) 0.0052(12) C42 0.054(2) 0.0410(17) 0.0492(18) -0.0034(14) 0.0241(16) 0.0017(15) C43 0.076(2) 0.0317(15) 0.0356(15) 0.0011(12) 0.0203(16) -0.0006(15) C44 0.068(2) 0.0337(15) 0.0340(15) 0.0042(12) 0.0051(15) 0.0123(15) C45 0.0496(17) 0.0286(13) 0.0372(14) 0.0039(11) 0.0073(13) 0.0136(12) _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 Sb S1 2.5341(7) . ? Sb S3 2.5435(7) . ? Sb S5 2.5980(7) . ? Sb S4 2.8643(7) . ? Sb S2 2.9135(8) . ? S1 C1 1.751(3) . ? S2 C1 1.698(3) . ? S3 C16 1.748(3) . ? S4 C16 1.694(3) . ? S5 C31 1.745(3) . ? S6 C31 1.698(3) . ? N1 C1 1.327(3) . ? N1 C2 1.470(3) . ? N1 C9 1.479(3) . ? N2 C16 1.334(3) . ? N2 C17 1.484(3) . ? N2 C24 1.473(3) . ? N3 C31 1.335(3) . ? N3 C32 1.469(3) . ? N3 C39 1.463(3) . ? C2 C3 1.511(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.388(4) . ? C3 C8 1.385(4) . ? C4 C5 1.382(4) . ? C4 H4 0.9400 . ? C5 C6 1.370(5) . ? C5 H5 0.9400 . ? C6 C7 1.372(5) . ? C6 H6 0.9400 . ? C7 C8 1.384(4) . ? C7 H7 0.9400 . ? C8 H8 0.9400 . ? C9 C10 1.513(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C15 1.385(4) . ? C10 C11 1.383(4) . ? C11 C12 1.386(5) . ? C11 H11 0.9400 . ? C12 C13 1.376(5) . ? C12 H12 0.9400 . ? C13 C14 1.372(5) . ? C13 H13 0.9400 . ? C14 C15 1.386(4) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C17 C18 1.507(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 C23 1.380(4) . ? C18 C19 1.396(4) . ? C19 C20 1.383(5) . ? C19 H19 0.9400 . ? C20 C21 1.368(5) . ? C20 H20 0.9400 . ? C21 C22 1.384(5) . ? C21 H21 0.9400 . ? C22 C23 1.390(4) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? C24 C25 1.501(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.390(4) . ? C25 C30 1.395(4) . ? C26 C27 1.384(5) . ? C26 H26 0.9400 . ? C27 C28 1.354(6) . ? C27 H27 0.9400 . ? C28 C29 1.379(6) . ? C28 H28 0.9400 . ? C29 C30 1.382(5) . ? C29 H29 0.9400 . ? C30 H30 0.9400 . ? C32 C33 1.508(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 C38 1.389(4) . ? C33 C34 1.388(4) . ? C34 C35 1.388(4) . ? C34 H34 0.9400 . ? C35 C36 1.378(5) . ? C35 H35 0.9400 . ? C36 C37 1.384(5) . ? C36 H36 0.9400 . ? C37 C38 1.379(4) . ? C37 H37 0.9400 . ? C38 H38 0.9400 . ? C39 C40 1.512(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C40 C41 1.390(4) . ? C40 C45 1.386(4) . ? C41 C42 1.397(4) . ? C41 H41 0.9400 . ? C42 C43 1.371(5) . ? C42 H42 0.9400 . ? C43 C44 1.378(5) . ? C43 H43 0.9400 . ? C44 C45 1.386(4) . ? C44 H44 0.9400 . ? C45 H45 0.9400 . ? 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 Sb S3 85.77(2) . . ? S1 Sb S5 85.18(2) . . ? S3 Sb S5 84.01(2) . . ? S1 Sb S4 91.60(2) . . ? S3 Sb S4 66.25(2) . . ? S5 Sb S4 150.25(2) . . ? S1 Sb S2 65.69(2) . . ? S3 Sb S2 149.74(2) . . ? S5 Sb S2 102.47(3) . . ? S4 Sb S2 103.05(2) . . ? C1 S1 Sb 93.09(9) . . ? C1 S2 Sb 81.84(9) . . ? C16 S3 Sb 91.70(9) . . ? C16 S4 Sb 82.38(9) . . ? C31 S5 Sb 92.50(9) . . ? C1 N1 C2 123.6(2) . . ? C1 N1 C9 121.9(2) . . ? C2 N1 C9 113.9(2) . . ? C16 N2 C17 121.1(2) . . ? C16 N2 C24 122.8(2) . . ? C17 N2 C24 116.0(2) . . ? C31 N3 C32 121.9(2) . . ? C31 N3 C39 123.2(2) . . ? C32 N3 C39 114.7(2) . . ? N1 C1 S2 122.58(19) . . ? N1 C1 S1 118.42(19) . . ? S2 C1 S1 119.00(15) . . ? N1 C2 C3 115.4(2) . . ? N1 C2 H2A 108.4 . . ? C3 C2 H2A 108.4 . . ? N1 C2 H2B 108.4 . . ? C3 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? C4 C3 C8 118.6(2) . . ? C4 C3 C2 121.3(2) . . ? C8 C3 C2 119.8(2) . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 121.0(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 119.8(3) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 119.7(3) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C3 C8 C7 121.0(3) . . ? C3 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? N1 C9 C10 110.9(2) . . ? N1 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.0 . . ? C15 C10 C11 118.8(3) . . ? C15 C10 C9 120.8(3) . . ? C11 C10 C9 120.3(3) . . ? C10 C11 C12 120.4(3) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 119.1(3) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.9(3) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C10 120.2(3) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? N2 C16 S4 121.8(2) . . ? N2 C16 S3 119.1(2) . . ? S4 C16 S3 119.10(15) . . ? N2 C17 C18 115.9(2) . . ? N2 C17 H17A 108.3 . . ? C18 C17 H17A 108.3 . . ? N2 C17 H17B 108.3 . . ? C18 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C23 C18 C19 118.3(3) . . ? C23 C18 C17 120.0(3) . . ? C19 C18 C17 121.6(3) . . ? C18 C19 C20 120.4(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 120.5(3) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 119.1(3) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C18 C23 C22 121.5(3) . . ? C18 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? N2 C24 C25 113.4(2) . . ? N2 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N2 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C30 118.4(3) . . ? C26 C25 C24 120.2(3) . . ? C30 C25 C24 121.3(3) . . ? C25 C26 C27 120.8(3) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C28 C27 C26 120.4(3) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 119.8(4) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 121.0(4) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C25 119.6(3) . . ? C29 C30 H30 120.2 . . ? C25 C30 H30 120.2 . . ? N3 C31 S6 122.0(2) . . ? N3 C31 S5 118.4(2) . . ? S6 C31 S5 119.63(16) . . ? N3 C32 C33 114.4(2) . . ? N3 C32 H32A 108.7 . . ? C33 C32 H32A 108.7 . . ? N3 C32 H32B 108.7 . . ? C33 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? C38 C33 C34 119.0(3) . . ? C38 C33 C32 118.8(2) . . ? C34 C33 C32 122.0(3) . . ? C35 C34 C33 119.8(3) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C36 C35 C34 120.7(3) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 119.7(3) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 119.8(3) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C33 120.9(3) . . ? C37 C38 H38 119.5 . . ? C33 C38 H38 119.5 . . ? N3 C39 C40 113.3(2) . . ? N3 C39 H39A 108.9 . . ? C40 C39 H39A 108.9 . . ? N3 C39 H39B 108.9 . . ? C40 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? C41 C40 C45 118.8(3) . . ? C41 C40 C39 122.8(3) . . ? C45 C40 C39 118.4(3) . . ? C40 C41 C42 119.7(3) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C43 C42 C41 120.7(3) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 119.9(3) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C45 119.8(3) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C40 C45 C44 121.0(3) . . ? C40 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.0 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.22 _refine_diff_density_min -0.45 _refine_diff_density_rms 0.098