#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/42/2204280.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2204280 loop_ _publ_author_name 'K. Ravikumar' 'G. Y. S. K. Swamy' 'Sadagopan Raghavan' 'Ch. Naveen Kumar' _publ_section_title N-[(1S,2S,3R)-2-Bromo-3-(tert-butyldiphenylsiloxy)-1-phenyl-4-(phenylsulfinyl)butyl]benzenesulfonamide _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o1880 _journal_page_last o1882 _journal_paper_doi 10.1107/S1600536804023694 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'C39 H42 Br N O4 S2 Si' _chemical_formula_moiety 'C39 H42 Br N O4 S2 Si' _chemical_formula_sum 'C39 H42 Br N O4 S2 Si' _chemical_formula_weight 760.86 _chemical_name_systematic ; N-[(1S,2S,3R)-3-(tert-Butyldiphenylsiloxy)-2-bromo-1-phenyl-4- (phenylsulfinyl)butyl]benzenesulfonamide ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 91.2630(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 20.0567(11) _cell_length_b 8.2412(5) _cell_length_c 23.8154 _cell_measurement_reflns_used 3196 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.61 _cell_measurement_theta_min 2.61 _cell_volume 3935.5(3) _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2003)' _computing_publication_material 'SHELXL97 and PARST (Nardelli, 1995)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.928 _diffrn_measured_fraction_theta_max 0.895 _diffrn_measurement_device 'Bruker SMART APEX' _diffrn_measurement_device_type 'Bruker SMART APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 24266 _diffrn_reflns_theta_full 25.0 _diffrn_reflns_theta_max 28.01 _diffrn_reflns_theta_min 1.71 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type none _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1584 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.555 _refine_diff_density_min -0.241 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 437 _refine_ls_number_reflns 9091 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.953 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0543 _refine_ls_shift/su_max <0.014 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.072P)^2^+0.603P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1091 _refine_ls_wR_factor_ref 0.1302 _reflns_number_gt 5188 _reflns_number_total 9091 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bt6527.cif _cod_data_source_block I _cod_original_cell_volume 3935.5(4) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2204280 _cod_database_fobs_code 2204280 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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Br1 0.195690(19) 0.95253(4) 0.023403(15) 0.05495(14) Uani d . 1 Br C1 0.28804(17) 0.8661(4) 0.11533(14) 0.0435(8) Uani d . 1 C H1 0.2933 0.7989 0.1491 0.052 Uiso calc R 1 H C2 0.21916(16) 0.8219(3) 0.08976(13) 0.0399(8) Uani d . 1 C H2 0.1865 0.8496 0.1182 0.048 Uiso calc R 1 H C3 0.20969(16) 0.6399(3) 0.07746(13) 0.0378(7) Uani d . 1 C H3 0.2327 0.5784 0.1073 0.045 Uiso calc R 1 H C4 0.23618(17) 0.5846(3) 0.02171(13) 0.0398(8) Uani d . 1 C H4A 0.2809 0.6268 0.0170 0.048 Uiso calc R 1 H H4B 0.2080 0.6260 -0.0086 0.048 Uiso calc R 1 H C5 0.27878(18) 0.3485(3) -0.04644(13) 0.0428(8) Uani d . 1 C C6 0.3462(2) 0.3253(5) -0.04780(16) 0.0636(11) Uani d . 1 C H6 0.3715 0.3209 -0.0146 0.076 Uiso calc R 1 H C7 0.3764(2) 0.3082(6) -0.0991(2) 0.0868(14) Uani d . 1 C H7 0.4222 0.2920 -0.1004 0.104 Uiso calc R 1 H C8 0.3396(3) 0.3151(6) -0.14761(18) 0.0846(14) Uani d . 1 C H8 0.3604 0.3043 -0.1819 0.102 Uiso calc R 1 H C9 0.2722(3) 0.3378(6) -0.14613(18) 0.0830(14) Uani d . 1 C H9 0.2473 0.3434 -0.1795 0.100 Uiso calc R 1 H C10 0.2410(2) 0.3525(5) -0.09549(16) 0.0669(11) Uani d . 1 C H10 0.1950 0.3649 -0.0944 0.080 Uiso calc R 1 H C11 0.34747(17) 0.8285(4) 0.08009(15) 0.0490(9) Uani d . 1 C C12 0.3829(2) 0.6869(5) 0.08953(19) 0.0730(12) Uani d . 1 C H12 0.3709 0.6176 0.1184 0.088 Uiso calc R 1 H C13 0.4360(2) 0.6482(7) 0.0561(3) 0.1003(18) Uani d . 1 C H13 0.4594 0.5523 0.0625 0.120 Uiso calc R 1 H C14 0.4543(2) 0.7484(8) 0.0140(3) 0.1041(18) Uani d . 1 C H14 0.4900 0.7211 -0.0084 0.125 Uiso calc R 1 H C15 0.4202(2) 0.8896(6) 0.0047(2) 0.0861(14) Uani d . 1 C H15 0.4329 0.9588 -0.0240 0.103 Uiso calc R 1 H C16 0.3671(2) 0.9300(5) 0.03766(17) 0.0634(11) Uani d . 1 C H16 0.3443 1.0267 0.0311 0.076 Uiso calc R 1 H C17 0.4086(2) 1.1084(5) 0.18138(15) 0.0581(10) Uani d . 1 C C18 0.4539(3) 0.9992(6) 0.2014(2) 0.1008(17) Uani d . 1 C H18 0.4397 0.9068 0.2201 0.121 Uiso calc R 1 H C19 0.5217(3) 1.0263(8) 0.1938(3) 0.123(2) Uani d . 1 C H19 0.5524 0.9528 0.2089 0.147 Uiso calc R 1 H C20 0.5441(3) 1.1547(8) 0.1655(3) 0.1030(17) Uani d . 1 C C21 0.4988(3) 1.2596(8) 0.1454(3) 0.121(2) Uani d . 1 C H21 0.5133 1.3494 0.1254 0.146 Uiso calc R 1 H C22 0.4312(2) 1.2395(6) 0.1533(2) 0.1020(17) Uani d . 1 C H22 0.4012 1.3162 0.1393 0.122 Uiso calc R 1 H C23 0.6188(3) 1.1812(8) 0.1569(3) 0.154(3) Uani d . 1 C H23A 0.6426 1.1656 0.1919 0.231 Uiso calc R 1 H H23B 0.6261 1.2897 0.1437 0.231 Uiso calc R 1 H H23C 0.6346 1.1050 0.1298 0.231 Uiso calc R 1 H C24 0.13825(16) 0.6306(4) 0.19891(13) 0.0463(8) Uani d . 1 C C25 0.18754(19) 0.5316(5) 0.22251(17) 0.0640(11) Uani d . 1 C H25 0.1976 0.4343 0.2048 0.077 Uiso calc R 1 H C26 0.2221(2) 0.5727(6) 0.2715(2) 0.0856(15) Uani d . 1 C H26 0.2548 0.5040 0.2864 0.103 Uiso calc R 1 H C27 0.2076(2) 0.7152(8) 0.29746(18) 0.0876(15) Uani d . 1 C H27 0.2300 0.7425 0.3308 0.105 Uiso calc R 1 H C28 0.1614(2) 0.8172(6) 0.27563(19) 0.0846(15) Uani d . 1 C H28 0.1527 0.9152 0.2934 0.102 Uiso calc R 1 H C29 0.12676(18) 0.7756(5) 0.22655(15) 0.0639(11) Uani d . 1 C H29 0.0950 0.8470 0.2118 0.077 Uiso calc R 1 H C30 0.02064(17) 0.7197(4) 0.12197(14) 0.0470(8) Uani d . 1 C C31 -0.02497(19) 0.7504(5) 0.16391(16) 0.0670(11) Uani d . 1 C H31 -0.0188 0.7010 0.1987 0.080 Uiso calc R 1 H C32 -0.0789(2) 0.8516(6) 0.15552(19) 0.0817(14) Uani d . 1 C H32 -0.1080 0.8713 0.1846 0.098 Uiso calc R 1 H C33 -0.0896(2) 0.9233(5) 0.1040(2) 0.0779(13) Uani d . 1 C H33 -0.1264 0.9903 0.0979 0.093 Uiso calc R 1 H C34 -0.0460(2) 0.8958(5) 0.06166(18) 0.0676(11) Uani d . 1 C H34 -0.0530 0.9448 0.0268 0.081 Uiso calc R 1 H C35 0.00834(18) 0.7957(4) 0.07047(15) 0.0537(9) Uani d . 1 C H35 0.0376 0.7785 0.0413 0.064 Uiso calc R 1 H C36 0.05932(19) 0.3617(4) 0.13002(15) 0.0546(9) Uani d . 1 C C37 0.0108(3) 0.3323(6) 0.1767(2) 0.1000(17) Uani d . 1 C H37A -0.0036 0.2212 0.1758 0.150 Uiso calc R 1 H H37B -0.0271 0.4024 0.1717 0.150 Uiso calc R 1 H H37C 0.0323 0.3547 0.2123 0.150 Uiso calc R 1 H C38 0.0237(3) 0.3390(6) 0.07335(19) 0.119(2) Uani d . 1 C H38A 0.0057 0.2312 0.0710 0.179 Uiso calc R 1 H H38B 0.0547 0.3550 0.0438 0.179 Uiso calc R 1 H H38C -0.0119 0.4165 0.0696 0.179 Uiso calc R 1 H C39 0.1144(3) 0.2344(5) 0.1353(2) 0.1056(17) Uani d . 1 C H39A 0.1339 0.2380 0.1725 0.158 Uiso calc R 1 H H39B 0.1482 0.2567 0.1083 0.158 Uiso calc R 1 H H39C 0.0960 0.1287 0.1283 0.158 Uiso calc R 1 H N1 0.28566(13) 1.0346(3) 0.13554(10) 0.0448(7) Uani d . 1 N H1A 0.2641 1.1064 0.1162 0.054 Uiso calc R 1 H O1 0.28760(12) 0.3162(3) 0.06379(9) 0.0549(6) Uani d . 1 O O2 0.14103(11) 0.5982(2) 0.07797(8) 0.0428(5) Uani d . 1 O O3 0.31616(15) 0.9545(3) 0.23158(10) 0.0789(8) Uani d . 1 O O4 0.29795(13) 1.2439(3) 0.20682(11) 0.0727(8) Uani d . 1 O S1 0.23776(5) 0.36527(9) 0.01921(3) 0.0443(2) Uani d . 1 S S2 0.32280(5) 1.08613(11) 0.19330(4) 0.0545(3) Uani d . 1 S Si1 0.09182(5) 0.57629(11) 0.13268(4) 0.0423(2) Uani d . 1 Si loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.0625(3) 0.03766(18) 0.0639(3) 0.00354(17) -0.01743(19) 0.00606(16) C1 0.049(2) 0.0371(17) 0.0437(19) 0.0048(15) -0.0060(17) 0.0027(14) C2 0.042(2) 0.0386(16) 0.0390(18) 0.0026(14) 0.0038(16) 0.0012(14) C3 0.0411(19) 0.0352(16) 0.0372(18) 0.0030(14) 0.0050(15) 0.0026(13) C4 0.045(2) 0.0306(15) 0.0438(19) 0.0013(14) 0.0052(16) 0.0032(13) C5 0.053(2) 0.0369(16) 0.0383(19) 0.0025(15) 0.0051(17) -0.0028(14) C6 0.059(3) 0.085(3) 0.047(2) 0.008(2) -0.001(2) -0.002(2) C7 0.066(3) 0.127(4) 0.069(3) 0.022(3) 0.017(3) 0.001(3) C8 0.106(4) 0.097(3) 0.051(3) 0.027(3) 0.024(3) 0.002(2) C9 0.094(4) 0.108(4) 0.046(3) 0.029(3) -0.010(3) -0.009(2) C10 0.066(3) 0.081(3) 0.053(3) 0.019(2) -0.004(2) -0.014(2) C11 0.040(2) 0.0418(18) 0.065(2) 0.0010(16) -0.0084(19) -0.0080(17) C12 0.058(3) 0.057(2) 0.104(3) 0.014(2) -0.010(3) 0.000(2) C13 0.055(3) 0.087(4) 0.158(6) 0.029(3) -0.005(4) -0.025(4) C14 0.057(3) 0.120(5) 0.136(5) 0.009(3) 0.027(3) -0.045(4) C15 0.063(3) 0.095(3) 0.101(4) -0.004(3) 0.024(3) -0.013(3) C16 0.054(2) 0.057(2) 0.079(3) 0.0011(19) 0.010(2) -0.007(2) C17 0.062(3) 0.055(2) 0.056(2) 0.000(2) -0.018(2) -0.0058(18) C18 0.079(4) 0.076(3) 0.146(5) 0.009(3) -0.029(3) 0.017(3) C19 0.071(4) 0.110(5) 0.185(7) 0.026(3) -0.026(4) 0.005(4) C20 0.064(4) 0.119(5) 0.125(5) -0.004(3) -0.018(3) -0.024(4) C21 0.067(4) 0.130(5) 0.166(6) -0.021(4) -0.005(4) 0.046(4) C22 0.060(3) 0.102(4) 0.143(5) -0.004(3) -0.014(3) 0.043(3) C23 0.060(4) 0.191(7) 0.210(7) -0.012(4) -0.013(4) -0.055(6) C24 0.040(2) 0.058(2) 0.041(2) -0.0033(17) 0.0067(16) 0.0007(16) C25 0.050(2) 0.068(2) 0.073(3) -0.003(2) -0.003(2) 0.010(2) C26 0.069(3) 0.109(4) 0.077(3) -0.011(3) -0.024(3) 0.025(3) C27 0.062(3) 0.150(5) 0.050(3) -0.026(3) -0.007(2) -0.010(3) C28 0.052(3) 0.125(4) 0.077(3) -0.003(3) -0.001(2) -0.046(3) C29 0.047(2) 0.085(3) 0.060(2) 0.004(2) 0.001(2) -0.023(2) C30 0.043(2) 0.0534(19) 0.045(2) 0.0003(16) -0.0013(17) -0.0084(16) C31 0.053(3) 0.096(3) 0.052(2) 0.015(2) 0.002(2) -0.007(2) C32 0.054(3) 0.118(4) 0.073(3) 0.028(3) 0.002(2) -0.019(3) C33 0.053(3) 0.086(3) 0.094(4) 0.024(2) -0.016(3) -0.012(3) C34 0.059(3) 0.072(3) 0.071(3) 0.007(2) -0.014(2) 0.005(2) C35 0.049(2) 0.058(2) 0.054(2) 0.0013(18) -0.0039(19) -0.0046(18) C36 0.061(2) 0.051(2) 0.052(2) -0.0142(19) 0.010(2) -0.0005(17) C37 0.112(4) 0.090(3) 0.100(4) -0.036(3) 0.053(3) -0.004(3) C38 0.191(6) 0.083(3) 0.082(3) -0.062(4) -0.042(4) -0.001(3) C39 0.105(4) 0.048(2) 0.165(5) -0.009(3) 0.031(4) -0.003(3) N1 0.0481(17) 0.0426(15) 0.0433(16) 0.0055(13) -0.0089(13) -0.0003(12) O1 0.0767(18) 0.0423(12) 0.0456(14) 0.0079(12) -0.0010(13) 0.0083(10) O2 0.0413(13) 0.0470(12) 0.0404(13) -0.0055(10) 0.0103(11) -0.0046(10) O3 0.101(2) 0.086(2) 0.0488(16) -0.0166(17) -0.0066(15) 0.0157(14) O4 0.078(2) 0.0722(18) 0.0678(17) 0.0126(15) -0.0040(15) -0.0278(14) S1 0.0541(6) 0.0333(4) 0.0456(5) 0.0001(4) 0.0063(4) 0.0002(3) S2 0.0635(6) 0.0573(5) 0.0422(5) -0.0011(5) -0.0059(5) -0.0056(4) Si1 0.0410(5) 0.0454(5) 0.0405(5) -0.0015(4) 0.0049(4) -0.0034(4) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N1 C1 C11 114.1(3) ? N1 C1 C2 108.5(2) ? C11 C1 C2 116.4(3) ? N1 C1 H1 105.6 ? C11 C1 H1 105.6 ? C2 C1 H1 105.6 ? C3 C2 C1 114.3(2) ? C3 C2 Br1 110.8(2) ? C1 C2 Br1 112.7(2) ? C3 C2 H2 106.1 ? C1 C2 H2 106.1 ? Br1 C2 H2 106.1 ? O2 C3 C4 107.1(2) ? O2 C3 C2 110.5(2) ? C4 C3 C2 114.6(2) ? O2 C3 H3 108.1 ? C4 C3 H3 108.1 ? C2 C3 H3 108.1 ? C3 C4 S1 109.7(2) ? C3 C4 H4A 109.7 ? S1 C4 H4A 109.7 ? C3 C4 H4B 109.7 ? S1 C4 H4B 109.7 ? H4A C4 H4B 108.2 ? C6 C5 C10 120.5(3) ? C6 C5 S1 120.4(3) ? C10 C5 S1 119.0(3) ? C5 C6 C7 119.2(4) ? C5 C6 H6 120.4 ? C7 C6 H6 120.4 ? C8 C7 C6 120.5(4) ? C8 C7 H7 119.7 ? C6 C7 H7 119.7 ? C7 C8 C9 120.2(4) ? C7 C8 H8 119.9 ? C9 C8 H8 119.9 ? C8 C9 C10 120.2(4) ? C8 C9 H9 119.9 ? C10 C9 H9 119.9 ? C5 C10 C9 119.3(4) ? C5 C10 H10 120.3 ? C9 C10 H10 120.3 ? C16 C11 C12 118.6(4) ? C16 C11 C1 121.8(3) ? C12 C11 C1 119.6(3) ? C13 C12 C11 120.1(4) ? C13 C12 H12 120.0 ? C11 C12 H12 120.0 ? C14 C13 C12 120.7(5) ? C14 C13 H13 119.7 ? C12 C13 H13 119.7 ? C13 C14 C15 119.8(5) ? C13 C14 H14 120.1 ? C15 C14 H14 120.1 ? C14 C15 C16 120.3(5) ? C14 C15 H15 119.8 ? C16 C15 H15 119.8 ? C11 C16 C15 120.5(4) ? C11 C16 H16 119.7 ? C15 C16 H16 119.7 ? C22 C17 C18 118.2(4) ? C22 C17 S2 120.2(3) ? C18 C17 S2 121.5(4) ? C17 C18 C19 119.7(5) ? C17 C18 H18 120.2 ? C19 C18 H18 120.2 ? C20 C19 C18 122.1(5) ? C20 C19 H19 118.9 ? C18 C19 H19 118.9 ? C19 C20 C21 117.4(5) ? C19 C20 C23 121.3(6) ? C21 C20 C23 121.3(6) ? C20 C21 C22 122.3(5) ? C20 C21 H21 118.8 ? C22 C21 H21 118.8 ? C17 C22 C21 120.2(5) ? C17 C22 H22 119.9 ? C21 C22 H22 119.9 ? C20 C23 H23A 109.5 ? C20 C23 H23B 109.5 ? H23A C23 H23B 109.5 ? C20 C23 H23C 109.5 ? H23A C23 H23C 109.5 ? H23B C23 H23C 109.5 ? C29 C24 C25 116.0(3) ? C29 C24 Si1 121.5(3) ? C25 C24 Si1 122.5(3) ? C26 C25 C24 122.3(4) ? C26 C25 H25 118.8 ? C24 C25 H25 118.8 ? C27 C26 C25 119.1(4) ? C27 C26 H26 120.5 ? C25 C26 H26 120.5 ? C28 C27 C26 121.0(4) ? C28 C27 H27 119.5 ? C26 C27 H27 119.5 ? C27 C28 C29 119.9(4) ? C27 C28 H28 120.1 ? C29 C28 H28 120.1 ? C24 C29 C28 121.8(4) ? C24 C29 H29 119.1 ? C28 C29 H29 119.1 ? C35 C30 C31 116.3(3) ? C35 C30 Si1 121.7(3) ? C31 C30 Si1 122.0(3) ? C32 C31 C30 122.2(4) ? C32 C31 H31 118.9 ? C30 C31 H31 118.9 ? C33 C32 C31 119.8(4) ? C33 C32 H32 120.1 ? C31 C32 H32 120.1 ? C34 C33 C32 119.7(4) ? C34 C33 H33 120.1 ? C32 C33 H33 120.1 ? C33 C34 C35 120.2(4) ? C33 C34 H34 119.9 ? C35 C34 H34 119.9 ? C34 C35 C30 121.8(4) ? C34 C35 H35 119.1 ? C30 C35 H35 119.1 ? C37 C36 C38 109.5(4) ? C37 C36 C39 107.8(4) ? C38 C36 C39 108.2(4) ? C37 C36 Si1 110.7(3) ? C38 C36 Si1 107.4(3) ? C39 C36 Si1 113.1(3) ? C36 C37 H37A 109.5 ? C36 C37 H37B 109.5 ? H37A C37 H37B 109.5 ? C36 C37 H37C 109.5 ? H37A C37 H37C 109.5 ? H37B C37 H37C 109.5 ? C36 C38 H38A 109.5 ? C36 C38 H38B 109.5 ? H38A C38 H38B 109.5 ? C36 C38 H38C 109.5 ? H38A C38 H38C 109.5 ? H38B C38 H38C 109.5 ? C36 C39 H39A 109.5 ? C36 C39 H39B 109.5 ? H39A C39 H39B 109.5 ? C36 C39 H39C 109.5 ? H39A C39 H39C 109.5 ? H39B C39 H39C 109.5 ? C1 N1 S2 120.8(2) ? C1 N1 H1A 119.6 ? S2 N1 H1A 119.6 ? C3 O2 Si1 128.76(19) ? O1 S1 C5 106.63(15) ? O1 S1 C4 104.99(14) ? C5 S1 C4 96.58(14) ? O3 S2 O4 120.62(18) ? O3 S2 N1 107.36(15) y O4 S2 N1 105.99(15) ? O3 S2 C17 106.75(18) y O4 S2 C17 106.74(17) ? N1 S2 C17 109.02(15) y O2 Si1 C30 106.84(14) y O2 Si1 C24 110.02(13) y C30 Si1 C24 109.21(15) y O2 Si1 C36 106.66(14) ? C30 Si1 C36 109.06(16) ? C24 Si1 C36 114.75(16) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Br1 C2 1.961(3) y C1 N1 1.470(4) y C1 C11 1.505(5) ? C1 C2 1.541(4) ? C1 H1 0.9800 ? C2 C3 1.539(4) ? C2 H2 0.9800 ? C3 O2 1.419(4) ? C3 C4 1.511(4) ? C3 H3 0.9800 ? C4 S1 1.809(3) y C4 H4A 0.9700 ? C4 H4B 0.9700 ? C5 C6 1.368(5) ? C5 C10 1.378(5) ? C5 S1 1.788(3) y C6 C7 1.382(5) ? C6 H6 0.9300 ? C7 C8 1.358(6) ? C7 H7 0.9300 ? C8 C9 1.367(6) ? C8 H8 0.9300 ? C9 C10 1.376(5) ? C9 H9 0.9300 ? C10 H10 0.9300 ? C11 C16 1.376(5) ? C11 C12 1.382(5) ? C12 C13 1.381(6) ? C12 H12 0.9300 ? C13 C14 1.356(7) ? C13 H13 0.9300 ? C14 C15 1.365(7) ? C14 H14 0.9300 ? C15 C16 1.378(5) ? C15 H15 0.9300 ? C16 H16 0.9300 ? C17 C22 1.354(6) ? C17 C18 1.358(5) ? C17 S2 1.760(4) y C18 C19 1.395(7) ? C18 H18 0.9300 ? C19 C20 1.337(8) ? C19 H19 0.9300 ? C20 C21 1.335(7) ? C20 C23 1.533(7) ? C21 C22 1.383(6) ? C21 H21 0.9300 ? C22 H22 0.9300 ? C23 H23A 0.9600 ? C23 H23B 0.9600 ? C23 H23C 0.9600 ? C24 C29 1.386(5) ? C24 C25 1.391(5) ? C24 Si1 1.868(3) y C25 C26 1.386(5) ? C25 H25 0.9300 ? C26 C27 1.362(6) ? C26 H26 0.9300 ? C27 C28 1.348(6) ? C27 H27 0.9300 ? C28 C29 1.389(5) ? C28 H28 0.9300 ? C29 H29 0.9300 ? C30 C35 1.395(5) ? C30 C31 1.392(5) ? C30 Si1 1.866(3) y C31 C32 1.376(5) ? C31 H31 0.9300 ? C32 C33 1.376(6) ? C32 H32 0.9300 ? C33 C34 1.368(6) ? C33 H33 0.9300 ? C34 C35 1.379(5) ? C34 H34 0.9300 ? C35 H35 0.9300 ? C36 C37 1.513(5) ? C36 C38 1.525(5) ? C36 C39 1.527(6) ? C36 Si1 1.886(3) y C37 H37A 0.9600 ? C37 H37B 0.9600 ? C37 H37C 0.9600 ? C38 H38A 0.9600 ? C38 H38B 0.9600 ? C38 H38C 0.9600 ? C39 H39A 0.9600 ? C39 H39B 0.9600 ? C39 H39C 0.9600 ? N1 S2 1.607(3) y N1 H1A 0.8600 ? O1 S1 1.498(2) y O2 Si1 1.662(2) y O3 S2 1.425(3) y O4 S2 1.431(3) y loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1A Br1 . 0.86 2.87 3.261(2) 110 C1 H1 O3 . 0.98 2.38 2.906(4) 113 C4 H4B Br1 . 0.97 2.81 3.140(3) 101 C6 H6 O1 . 0.93 2.54 2.931(4) 106 C18 H18 O3 . 0.93 2.53 2.893(6) 104 N1 H1A O1 1_565 0.86 2.19 2.883(3) 137 C25 H25 O4 1_545 0.93 2.55 3.271(5) 135 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 N1 C1 C2 C3 -168.5(2) C11 C1 C2 C3 61.1(4) N1 C1 C2 Br1 63.8(3) C11 C1 C2 Br1 -66.5(3) C1 C2 C3 O2 154.6(3) Br1 C2 C3 O2 -76.8(3) C1 C2 C3 C4 -84.3(3) Br1 C2 C3 C4 44.4(3) O2 C3 C4 S1 -69.0(3) C2 C3 C4 S1 168.1(2) C10 C5 C6 C7 1.0(6) S1 C5 C6 C7 178.2(3) C5 C6 C7 C8 0.2(7) C6 C7 C8 C9 -0.5(7) C7 C8 C9 C10 -0.6(7) C6 C5 C10 C9 -2.0(5) S1 C5 C10 C9 -179.3(3) C8 C9 C10 C5 1.8(6) N1 C1 C11 C16 -46.2(4) C2 C1 C11 C16 81.5(4) N1 C1 C11 C12 135.1(3) C2 C1 C11 C12 -97.2(4) C16 C11 C12 C13 -1.1(6) C1 C11 C12 C13 177.6(4) C11 C12 C13 C14 0.4(7) C12 C13 C14 C15 0.3(8) C13 C14 C15 C16 -0.4(8) C12 C11 C16 C15 1.1(6) C1 C11 C16 C15 -177.6(3) C14 C15 C16 C11 -0.3(7) C22 C17 C18 C19 1.4(8) S2 C17 C18 C19 -176.3(4) C17 C18 C19 C20 -2.3(10) C18 C19 C20 C21 1.3(10) C18 C19 C20 C23 -179.2(5) C19 C20 C21 C22 0.4(10) C23 C20 C21 C22 -179.1(6) C18 C17 C22 C21 0.3(8) S2 C17 C22 C21 178.0(4) C20 C21 C22 C17 -1.2(10) C29 C24 C25 C26 1.6(5) Si1 C24 C25 C26 179.6(3) C24 C25 C26 C27 -0.2(7) C25 C26 C27 C28 -1.3(7) C26 C27 C28 C29 1.4(7) C25 C24 C29 C28 -1.5(6) Si1 C24 C29 C28 -179.6(3) C27 C28 C29 C24 0.1(7) C35 C30 C31 C32 -0.7(6) Si1 C30 C31 C32 -177.6(3) C30 C31 C32 C33 1.3(7) C31 C32 C33 C34 -1.1(7) C32 C33 C34 C35 0.4(6) C33 C34 C35 C30 0.1(6) C31 C30 C35 C34 0.0(5) Si1 C30 C35 C34 176.9(3) C11 C1 N1 S2 -87.4(3) C2 C1 N1 S2 141.0(2) C4 C3 O2 Si1 159.52(19) C2 C3 O2 Si1 -75.0(3) C6 C5 S1 O1 -11.1(3) C10 C5 S1 O1 166.2(3) C6 C5 S1 C4 96.8(3) C10 C5 S1 C4 -86.0(3) C3 C4 S1 O1 -64.9(2) C3 C4 S1 C5 -174.1(2) C1 N1 S2 O3 -36.6(3) C1 N1 S2 O4 -166.8(3) C1 N1 S2 C17 78.6(3) C22 C17 S2 O3 -170.0(4) C18 C17 S2 O3 7.7(4) C22 C17 S2 O4 -39.8(4) C18 C17 S2 O4 137.9(4) C22 C17 S2 N1 74.3(4) C18 C17 S2 N1 -108.0(4) C3 O2 Si1 C30 122.7(2) C3 O2 Si1 C24 4.3(3) C3 O2 Si1 C36 -120.7(2) C35 C30 Si1 O2 13.0(3) C31 C30 Si1 O2 -170.3(3) C35 C30 Si1 C24 132.0(3) C31 C30 Si1 C24 -51.3(3) C35 C30 Si1 C36 -101.9(3) C31 C30 Si1 C36 74.8(3) C29 C24 Si1 O2 105.0(3) C25 C24 Si1 O2 -73.0(3) C29 C24 Si1 C30 -11.9(3) C25 C24 Si1 C30 170.1(3) C29 C24 Si1 C36 -134.7(3) C25 C24 Si1 C36 47.3(3) C37 C36 Si1 O2 -177.0(3) C38 C36 Si1 O2 -57.5(4) C39 C36 Si1 O2 61.9(3) C37 C36 Si1 C30 -62.0(3) C38 C36 Si1 C30 57.6(4) C39 C36 Si1 C30 177.0(3) C37 C36 Si1 C24 60.9(4) C38 C36 Si1 C24 -179.6(3) C39 C36 Si1 C24 -60.2(3) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139066996