# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 188/152 # Crystallographic data for manuscript no. 8/08116F/P2P # JCS Perkin II # "On the Stereochemistry of the Carbolithiation Reaction of Vinylsulfides" # R.W. Hoffmann, R. Koberstein, K. Harms # # This file contains four data sets : # data_kob1, data_kob2, data_kob02, data_kob03 # # This file has been sent to perkin@rsc.org a n d deposit@ccdc.cam.ac.uk # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF, VERSION DEC95) # This electronic data deposition form must be associated with CIF # output and can be used : # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.ac.uk # or via the WWW at http://www.iucr.ac.uk/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Data block identification for start of deposition data_global #------------------------------------------------------------------------- #2 Person making the deposition _publ_contact_author 'Klaus Harms' _publ_contact_author_email harms@chemie.uni-marburg.de #------------------------------------------------------------------------- #3 Publication details # Provide these details if the structure has been published, # accepted or submitted for publication # The CCDC journal deposition number, eg. 182/357, # should be included only if it has been assigned by the journal loop_ _publ_author_name Hoffmann, Reinhard W. Koberstein, Ralf Harms, Klaus _journal_name_full 'JCS Perkin II' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '?' _ccdc_journal_depnumber '?' #------------------------------------------------------------------------- #4 Chemical and physical data # Note that the units for melting point are Kelvin # The compound_id is the identifier for the compound in the published # paper, eg. 4a, II, etc. # Provide a brief description of any significant biological activity, # eg. antimalarial activity # If the compound exhibits polymorphism provide brief details, # eg. monoclinic form, low-temperature phase, etc. # For chemdiag include any ASCII file output by a chemical drawing # package # Against _type record, for example, ChemDraw # Against _records supply the chemical connectivity records #------------------------------------------------------------------------- #------------------------------------------------------------------------- #6 Include your "standard" CIF file here # It should contain the following data items: # unit cell parameters and volume, z value, space group symbol, # R-factor(s), atomic coordinates with standard deviations, # occupancy factors, bond lengths and bond angles # Other data items may be present but will not necessarily be # included in the Cambridge Structural Database # Do not include structure factors #------------------------------------------------------------------------- #SUBMISSION INFORMATION # For a journal send the form to the address specified by the journal # For a private communication to the CCDC send the form to the address # deposit@chemcrys.cam.ac.uk # If you have any problems with the form please contact the CCDC # Technical Editors : # by e-mail: teched@chemcrys.cam.ac.uk # by telephone: +44 1223 336031/2 # Following for data sets (sperated with # = = = END) data_kob1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H38 S Sn' _chemical_formula_weight 501.31 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' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.667(2) _cell_length_b 29.670(4) _cell_length_c 15.9184(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.768(11) _cell_angle_gamma 90.00 _cell_volume 5037.8(14) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 5.12 _cell_measurement_theta_max 12.60 _exptl_crystal_description regular _exptl_crystal_colour colorless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 1.106 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7879 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7445 _reflns_number_gt 6073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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 w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+8.1765P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00029(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7445 _refine_ls_number_parameters 522 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0941 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn Sn -0.15852(3) 0.117904(11) -0.186251(18) 0.04256(11) Uani 1 d . . . S S 0.12141(9) 0.10308(4) -0.23366(6) 0.0416(3) Uani 1 d . . . C1 C -0.0242(3) 0.11743(14) -0.2904(3) 0.0353(9) Uani 1 d . . . H1A H -0.0161 0.1488 -0.3108 0.042 Uiso 1 calc R . . C2 C -0.0456(3) 0.08709(14) -0.3672(2) 0.0326(9) Uani 1 d . . . H2A H 0.0382 0.0770 -0.3855 0.039 Uiso 1 calc R . . C3 C -0.1095(3) 0.10989(14) -0.4446(2) 0.0344(9) Uani 1 d . . . C4 C -0.1400(4) 0.06788(17) -0.5006(3) 0.0528(12) Uani 1 d . . . H4A H -0.2163 0.0732 -0.5340 0.063 Uiso 1 calc R . . H4B H -0.0708 0.0619 -0.5389 0.063 Uiso 1 calc R . . C5 C -0.1582(5) 0.02815(17) -0.4418(3) 0.0571(13) Uani 1 d . . . H5A H -0.1041 0.0030 -0.4581 0.069 Uiso 1 calc R . . H5B H -0.2456 0.0179 -0.4440 0.069 Uiso 1 calc R . . C6 C -0.1238(4) 0.04430(16) -0.3534(3) 0.0478(11) Uani 1 d . . . H6A H -0.0747 0.0214 -0.3232 0.057 Uiso 1 calc R . . H6B H -0.1992 0.0511 -0.3213 0.057 Uiso 1 calc R . . C7 C -0.2332(4) 0.13220(18) -0.4197(3) 0.0506(12) Uani 1 d . . . H7A H -0.2735 0.1450 -0.4692 0.076 Uiso 1 calc R . . H7B H -0.2163 0.1559 -0.3791 0.076 Uiso 1 calc R . . H7C H -0.2878 0.1098 -0.3950 0.076 Uiso 1 calc R . . C8 C -0.0205(3) 0.14295(14) -0.4866(2) 0.0324(9) Uani 1 d . . . C9 C 0.0935(4) 0.12800(15) -0.5184(3) 0.0394(10) Uani 1 d . . . H9A H 0.1138 0.0972 -0.5145 0.047 Uiso 1 calc R . . C10 C 0.1768(4) 0.15699(19) -0.5551(3) 0.0511(12) Uani 1 d . . . H10A H 0.2530 0.1458 -0.5754 0.061 Uiso 1 calc R . . C11 C 0.1506(5) 0.2014(2) -0.5625(3) 0.0659(15) Uani 1 d . . . H11A H 0.2078 0.2209 -0.5882 0.079 Uiso 1 calc R . . C12 C 0.0390(6) 0.21759(18) -0.5317(3) 0.0677(15) Uani 1 d . . . H12A H 0.0202 0.2485 -0.5360 0.081 Uiso 1 calc R . . C13 C -0.0458(4) 0.18825(17) -0.4944(3) 0.0512(12) Uani 1 d . . . H13A H -0.1219 0.1996 -0.4741 0.061 Uiso 1 calc R . . C14 C 0.2405(3) 0.11593(14) -0.3086(2) 0.0335(10) Uani 1 d . . . C15 C 0.3022(3) 0.08007(15) -0.3486(3) 0.0387(10) Uani 1 d . . . C16 C 0.3952(4) 0.09027(18) -0.4074(3) 0.0443(12) Uani 1 d . . . C17 C 0.4239(4) 0.13432(18) -0.4222(3) 0.0475(12) Uani 1 d . . . H17A H 0.4874 0.1407 -0.4609 0.057 Uiso 1 calc R . . C18 C 0.3649(4) 0.17039(16) -0.3835(3) 0.0454(11) Uani 1 d . . . C19 C 0.2711(4) 0.16104(15) -0.3249(3) 0.0393(10) Uani 1 d . . . C20 C 0.2706(4) 0.03152(16) -0.3310(3) 0.0546(13) Uani 1 d . . . H20A H 0.2499 0.0163 -0.3833 0.082 Uiso 1 calc R . . H20B H 0.1995 0.0301 -0.2938 0.082 Uiso 1 calc R . . H20C H 0.3422 0.0168 -0.3045 0.082 Uiso 1 calc R . . C21 C 0.4639(4) 0.05341(19) -0.4530(3) 0.0645(15) Uani 1 d . . . H21A H 0.5230 0.0667 -0.4916 0.097 Uiso 1 calc R . . H21B H 0.4041 0.0351 -0.4842 0.097 Uiso 1 calc R . . H21C H 0.5087 0.0347 -0.4126 0.097 Uiso 1 calc R . . C22 C 0.4017(5) 0.2180(2) -0.4043(4) 0.0751(17) Uani 1 d . . . H22A H 0.4437 0.2315 -0.3561 0.113 Uiso 1 calc R . . H22B H 0.3272 0.2353 -0.4184 0.113 Uiso 1 calc R . . H22C H 0.4578 0.2178 -0.4517 0.113 Uiso 1 calc R . . C23 C 0.2042(4) 0.19981(16) -0.2835(3) 0.0541(12) Uani 1 d . . . H23A H 0.2652 0.2220 -0.2646 0.081 Uiso 1 calc R . . H23B H 0.1579 0.1888 -0.2357 0.081 Uiso 1 calc R . . H23C H 0.1467 0.2136 -0.3236 0.081 Uiso 1 calc R . . Sn' Sn -0.65817(3) 0.114047(11) -0.007030(19) 0.04150(11) Uani 1 d . . . S' S -0.37018(9) 0.11101(4) 0.03378(7) 0.0417(3) Uani 1 d . . . C1' C -0.5142(3) 0.11952(14) 0.0930(2) 0.0344(9) Uani 1 d . . . H1'A H -0.5141 0.1512 0.1128 0.041 Uiso 1 calc R . . C2' C -0.5206(4) 0.08936(14) 0.1708(2) 0.0352(9) Uani 1 d . . . H2'A H -0.4329 0.0843 0.1896 0.042 Uiso 1 calc R . . C3' C -0.5896(4) 0.11019(15) 0.2469(2) 0.0392(10) Uani 1 d . . . C4' C -0.6029(5) 0.06763(19) 0.3040(3) 0.0636(15) Uani 1 d . . . H4'A H -0.5287 0.0643 0.3404 0.076 Uiso 1 calc R . . H4'B H -0.6769 0.0704 0.3394 0.076 Uiso 1 calc R . . C5' C -0.6158(5) 0.02775(19) 0.2467(3) 0.0695(16) Uani 1 d . . . H5'A H -0.7026 0.0169 0.2461 0.083 Uiso 1 calc R . . H5'B H -0.5611 0.0032 0.2661 0.083 Uiso 1 calc R . . C6' C -0.5786(5) 0.04283(16) 0.1593(3) 0.0528(12) Uani 1 d . . . H6'A H -0.6523 0.0443 0.1220 0.063 Uiso 1 calc R . . H6'B H -0.5178 0.0219 0.1353 0.063 Uiso 1 calc R . . C7' C -0.7200(4) 0.12700(19) 0.2210(3) 0.0597(14) Uani 1 d . . . H7'A H -0.7122 0.1497 0.1776 0.090 Uiso 1 calc R . . H7'B H -0.7610 0.1399 0.2693 0.090 Uiso 1 calc R . . H7'C H -0.7694 0.1020 0.1995 0.090 Uiso 1 calc R . . C8' C -0.5111(4) 0.14671(16) 0.2887(2) 0.0403(11) Uani 1 d . . . C9' C -0.3914(4) 0.13733(18) 0.3209(3) 0.0508(12) Uani 1 d . . . H9'A H -0.3598 0.1078 0.3173 0.061 Uiso 1 calc R . . C10' C -0.3186(5) 0.1706(3) 0.3580(3) 0.0718(18) Uani 1 d . . . H10B H -0.2381 0.1635 0.3787 0.086 Uiso 1 calc R . . C11' C -0.3615(7) 0.2134(3) 0.3649(4) 0.090(2) Uani 1 d . . . H11B H -0.3116 0.2357 0.3908 0.108 Uiso 1 calc R . . C12' C -0.4790(7) 0.2241(2) 0.3336(4) 0.090(2) Uani 1 d . . . H12B H -0.5094 0.2537 0.3378 0.108 Uiso 1 calc R . . C13' C -0.5518(5) 0.1911(2) 0.2963(3) 0.0628(14) Uani 1 d . . . H13B H -0.6316 0.1989 0.2751 0.075 Uiso 1 calc R . . C14' C -0.2496(3) 0.12597(14) 0.1081(2) 0.0337(10) Uani 1 d . . . C15' C -0.1799(4) 0.09130(14) 0.1474(3) 0.0363(10) Uani 1 d . . . C16' C -0.0901(3) 0.10268(15) 0.2079(3) 0.0394(11) Uani 1 d . . . C17' C -0.0693(4) 0.14754(16) 0.2267(3) 0.0456(11) Uani 1 d . . . H17B H -0.0091 0.1549 0.2681 0.055 Uiso 1 calc R . . C18' C -0.1343(4) 0.18239(15) 0.1867(3) 0.0437(11) Uani 1 d . . . C19' C -0.2271(4) 0.17148(15) 0.1274(3) 0.0391(10) Uani 1 d . . . C20' C -0.1987(4) 0.04233(16) 0.1255(3) 0.0534(12) Uani 1 d . . . H20D H -0.1212 0.0300 0.1042 0.080 Uiso 1 calc R . . H20E H -0.2642 0.0396 0.0829 0.080 Uiso 1 calc R . . H20F H -0.2229 0.0258 0.1754 0.080 Uiso 1 calc R . . C21' C -0.0178(4) 0.06673(17) 0.2562(3) 0.0579(13) Uani 1 d . . . H21D H 0.0313 0.0490 0.2174 0.087 Uiso 1 calc R . . H21E H -0.0762 0.0472 0.2850 0.087 Uiso 1 calc R . . H21F H 0.0376 0.0810 0.2970 0.087 Uiso 1 calc R . . C22' C -0.1063(5) 0.23052(17) 0.2107(4) 0.0670(15) Uani 1 d . . . H22D H -0.0497 0.2310 0.2590 0.100 Uiso 1 calc R . . H22E H -0.1837 0.2458 0.2248 0.100 Uiso 1 calc R . . H22F H -0.0673 0.2458 0.1639 0.100 Uiso 1 calc R . . C23' C -0.3005(4) 0.20902(16) 0.0865(3) 0.0554(13) Uani 1 d . . . H23D H -0.2433 0.2323 0.0678 0.083 Uiso 1 calc R . . H23E H -0.3583 0.2217 0.1267 0.083 Uiso 1 calc R . . H23F H -0.3473 0.1973 0.0386 0.083 Uiso 1 calc R . . C26 C -0.1439(5) 0.05493(18) -0.1216(3) 0.0617(14) Uani 1 d . . . H26A H -0.1380 0.0603 -0.0616 0.093 Uiso 1 calc R . . H26B H -0.0695 0.0391 -0.1399 0.093 Uiso 1 calc R . . H26C H -0.2175 0.0368 -0.1340 0.093 Uiso 1 calc R . . C25 C -0.0967(5) 0.17161(18) -0.1066(3) 0.0653(15) Uani 1 d . . . H25A H -0.1261 0.1665 -0.0500 0.098 Uiso 1 calc R . . H25B H -0.1301 0.1999 -0.1275 0.098 Uiso 1 calc R . . H25C H -0.0058 0.1728 -0.1060 0.098 Uiso 1 calc R . . C26' C -0.6007(5) 0.0634(2) -0.0922(4) 0.0784(18) Uani 1 d . . . H26D H -0.6454 0.0671 -0.1453 0.118 Uiso 1 calc R . . H26E H -0.6191 0.0339 -0.0690 0.118 Uiso 1 calc R . . H26F H -0.5113 0.0660 -0.1014 0.118 Uiso 1 calc R . . C24 C -0.3493(5) 0.1326(3) -0.2195(4) 0.094(2) Uani 1 d . . . H24A H -0.3981 0.1358 -0.1688 0.142 Uiso 1 calc R . . H24B H -0.3834 0.1083 -0.2534 0.142 Uiso 1 calc R . . H24C H -0.3528 0.1605 -0.2512 0.142 Uiso 1 calc R . . C25' C -0.6549(7) 0.1783(2) -0.0656(4) 0.096(2) Uani 1 d . . . H25D H -0.6611 0.1746 -0.1261 0.144 Uiso 1 calc R . . H25E H -0.5770 0.1935 -0.0512 0.144 Uiso 1 calc R . . H25F H -0.7250 0.1961 -0.0463 0.144 Uiso 1 calc R . . C24' C -0.8471(5) 0.0975(3) 0.0250(4) 0.112(3) Uani 1 d . . . H24D H -0.8972 0.0942 -0.0259 0.168 Uiso 1 calc R . . H24E H -0.8817 0.1213 0.0593 0.168 Uiso 1 calc R . . H24F H -0.8478 0.0694 0.0562 0.168 Uiso 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 Sn 0.03549(16) 0.0539(2) 0.03845(18) 0.00158(14) 0.00713(12) 0.00081(13) S 0.0302(5) 0.0621(8) 0.0323(6) 0.0099(5) -0.0016(4) 0.0001(5) C1 0.0246(18) 0.038(3) 0.043(2) 0.0091(19) 0.0017(16) -0.0026(17) C2 0.0300(19) 0.035(3) 0.033(2) 0.0024(18) 0.0012(15) -0.0015(17) C3 0.0295(19) 0.043(3) 0.030(2) 0.0023(18) -0.0017(15) -0.0018(17) C4 0.050(3) 0.060(4) 0.047(3) -0.007(2) -0.006(2) -0.015(2) C5 0.057(3) 0.048(3) 0.066(3) -0.012(3) 0.002(2) -0.009(2) C6 0.048(3) 0.041(3) 0.054(3) 0.006(2) 0.001(2) -0.010(2) C7 0.029(2) 0.081(4) 0.042(3) 0.009(2) 0.0005(18) 0.006(2) C8 0.035(2) 0.036(3) 0.026(2) -0.0015(17) -0.0062(15) 0.0034(18) C9 0.037(2) 0.042(3) 0.039(2) 0.0010(19) 0.0053(17) -0.0018(19) C10 0.042(3) 0.070(4) 0.041(3) 0.002(2) 0.0049(19) -0.009(2) C11 0.075(4) 0.073(5) 0.050(3) 0.010(3) 0.002(3) -0.030(3) C12 0.100(4) 0.036(3) 0.067(4) 0.010(3) -0.008(3) -0.008(3) C13 0.055(3) 0.047(3) 0.051(3) 0.004(2) -0.001(2) 0.008(2) C14 0.0261(18) 0.049(3) 0.026(2) 0.0045(19) -0.0097(15) -0.0037(18) C15 0.0273(19) 0.046(3) 0.042(2) 0.001(2) -0.0087(16) 0.0011(19) C16 0.029(2) 0.069(4) 0.034(2) -0.002(2) -0.0071(17) 0.004(2) C17 0.026(2) 0.072(4) 0.045(3) 0.006(2) 0.0024(17) -0.010(2) C18 0.034(2) 0.053(3) 0.049(3) 0.005(2) -0.0083(19) -0.015(2) C19 0.030(2) 0.045(3) 0.043(2) 0.002(2) -0.0091(17) -0.0036(19) C20 0.057(3) 0.044(3) 0.063(3) 0.000(2) 0.002(2) 0.006(2) C21 0.046(3) 0.083(4) 0.065(3) -0.019(3) 0.006(2) 0.011(3) C22 0.070(4) 0.066(4) 0.089(4) 0.016(3) -0.002(3) -0.027(3) C23 0.051(3) 0.044(3) 0.068(3) -0.006(2) -0.007(2) 0.000(2) Sn' 0.03678(16) 0.0466(2) 0.04097(18) -0.00169(14) -0.00594(12) -0.00190(13) S' 0.0321(5) 0.0574(8) 0.0355(6) -0.0026(5) 0.0025(4) -0.0026(5) C1' 0.0282(19) 0.035(3) 0.040(2) -0.0005(18) -0.0006(16) -0.0021(17) C2' 0.032(2) 0.036(3) 0.037(2) 0.0058(18) -0.0018(16) -0.0056(18) C3' 0.031(2) 0.059(3) 0.027(2) 0.0068(19) 0.0024(16) -0.0059(19) C4' 0.063(3) 0.080(4) 0.048(3) 0.022(3) 0.004(2) -0.020(3) C5' 0.078(4) 0.062(4) 0.068(4) 0.026(3) -0.006(3) -0.017(3) C6' 0.059(3) 0.044(3) 0.055(3) 0.003(2) 0.000(2) -0.010(2) C7' 0.035(2) 0.101(4) 0.043(3) -0.013(3) 0.0052(19) 0.000(2) C8' 0.038(2) 0.056(3) 0.027(2) 0.004(2) 0.0025(16) -0.004(2) C9' 0.043(2) 0.072(4) 0.037(3) 0.001(2) -0.0042(19) -0.005(2) C10' 0.053(3) 0.121(6) 0.042(3) -0.013(3) 0.000(2) -0.025(3) C11' 0.093(5) 0.114(6) 0.062(4) -0.030(4) 0.010(3) -0.048(5) C12' 0.122(6) 0.067(5) 0.083(5) -0.025(4) 0.016(4) -0.015(4) C13' 0.062(3) 0.072(4) 0.054(3) -0.006(3) 0.003(2) 0.003(3) C14' 0.0275(19) 0.044(3) 0.030(2) 0.0040(18) 0.0037(15) -0.0057(17) C15' 0.033(2) 0.038(3) 0.038(2) 0.0048(19) 0.0082(17) -0.0025(18) C16' 0.0260(19) 0.046(3) 0.046(3) 0.011(2) 0.0031(17) -0.0018(18) C17' 0.032(2) 0.052(3) 0.052(3) 0.003(2) -0.0014(18) -0.012(2) C18' 0.035(2) 0.040(3) 0.056(3) 0.001(2) 0.0066(19) -0.0113(19) C19' 0.032(2) 0.040(3) 0.045(3) 0.009(2) 0.0080(17) -0.0028(19) C20' 0.054(3) 0.042(3) 0.065(3) 0.005(2) -0.002(2) 0.004(2) C21' 0.044(3) 0.062(4) 0.068(3) 0.023(3) -0.004(2) -0.005(2) C22' 0.068(3) 0.049(4) 0.084(4) -0.002(3) -0.001(3) -0.017(3) C23' 0.052(3) 0.041(3) 0.073(3) 0.014(2) 0.004(2) -0.002(2) C26 0.067(3) 0.065(4) 0.054(3) 0.005(3) 0.015(2) -0.012(3) C25 0.084(4) 0.052(4) 0.060(3) -0.011(3) 0.014(3) 0.000(3) C26' 0.077(4) 0.068(4) 0.089(4) -0.038(3) -0.021(3) 0.002(3) C24 0.041(3) 0.180(7) 0.063(4) 0.018(4) 0.016(3) 0.020(4) C25' 0.135(6) 0.053(4) 0.098(5) 0.011(3) -0.054(4) 0.001(4) C24' 0.043(3) 0.229(9) 0.065(4) 0.002(5) -0.007(3) -0.037(4) _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 Sn C25 2.135(5) . ? Sn C26 2.138(5) . ? Sn C24 2.141(5) . ? Sn C1 2.205(4) . ? S C14 1.795(4) . ? S C1 1.837(4) . ? C1 C2 1.534(6) . ? C1 H1A 0.9900 . ? C2 C6 1.536(6) . ? C2 C3 1.554(5) . ? C2 H2A 0.9900 . ? C3 C8 1.526(6) . ? C3 C7 1.533(5) . ? C3 C4 1.564(6) . ? C4 C5 1.519(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.527(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C13 1.376(6) . ? C8 C9 1.395(5) . ? C9 C10 1.373(6) . ? C9 H9A 0.9400 . ? C10 C11 1.351(8) . ? C10 H10A 0.9400 . ? C11 C12 1.380(8) . ? C11 H11A 0.9400 . ? C12 C13 1.394(7) . ? C12 H12A 0.9400 . ? C13 H13A 0.9400 . ? C14 C19 1.403(6) . ? C14 C15 1.408(6) . ? C15 C16 1.406(6) . ? C15 C20 1.507(6) . ? C16 C17 1.364(7) . ? C16 C21 1.508(7) . ? C17 C18 1.391(7) . ? C17 H17A 0.9400 . ? C18 C19 1.405(6) . ? C18 C22 1.504(7) . ? C19 C23 1.509(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? Sn' C26' 2.121(5) . ? Sn' C25' 2.123(6) . ? Sn' C24' 2.142(5) . ? Sn' C1' 2.203(4) . ? S' C14' 1.791(4) . ? S' C1' 1.831(4) . ? C1' C2' 1.530(5) . ? C1' H1'A 0.9900 . ? C2' C6' 1.523(6) . ? C2' C3' 1.554(6) . ? C2' H2'A 0.9900 . ? C3' C8' 1.517(6) . ? C3' C7' 1.529(6) . ? C3' C4' 1.563(6) . ? C4' C5' 1.499(8) . ? C4' H4'A 0.9800 . ? C4' H4'B 0.9800 . ? C5' C6' 1.518(7) . ? C5' H5'A 0.9800 . ? C5' H5'B 0.9800 . ? C6' H6'A 0.9800 . ? C6' H6'B 0.9800 . ? C7' H7'A 0.9700 . ? C7' H7'B 0.9700 . ? C7' H7'C 0.9700 . ? C8' C13' 1.392(7) . ? C8' C9' 1.398(6) . ? C9' C10' 1.384(7) . ? C9' H9'A 0.9400 . ? C10' C11' 1.355(9) . ? C10' H10B 0.9400 . ? C11' C12' 1.379(9) . ? C11' H11B 0.9400 . ? C12' C13' 1.379(8) . ? C12' H12B 0.9400 . ? C13' H13B 0.9400 . ? C14' C19' 1.405(6) . ? C14' C15' 1.411(6) . ? C15' C16' 1.391(6) . ? C15' C20' 1.507(6) . ? C16' C17' 1.382(6) . ? C16' C21' 1.519(6) . ? C17' C18' 1.394(6) . ? C17' H17B 0.9400 . ? C18' C19' 1.397(6) . ? C18' C22' 1.507(7) . ? C19' C23' 1.505(6) . ? C20' H20D 0.9700 . ? C20' H20E 0.9700 . ? C20' H20F 0.9700 . ? C21' H21D 0.9700 . ? C21' H21E 0.9700 . ? C21' H21F 0.9700 . ? C22' H22D 0.9700 . ? C22' H22E 0.9700 . ? C22' H22F 0.9700 . ? C23' H23D 0.9700 . ? C23' H23E 0.9700 . ? C23' H23F 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26' H26D 0.9700 . ? C26' H26E 0.9700 . ? C26' H26F 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25' H25D 0.9700 . ? C25' H25E 0.9700 . ? C25' H25F 0.9700 . ? C24' H24D 0.9700 . ? C24' H24E 0.9700 . ? C24' H24F 0.9700 . ? 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 C25 Sn C26 110.3(2) . . ? C25 Sn C24 106.2(3) . . ? C26 Sn C24 111.1(2) . . ? C25 Sn C1 104.63(18) . . ? C26 Sn C1 108.20(17) . . ? C24 Sn C1 116.13(18) . . ? C14 S C1 103.04(17) . . ? C2 C1 S 111.8(3) . . ? C2 C1 Sn 120.8(2) . . ? S C1 Sn 100.70(18) . . ? C2 C1 H1A 107.6 . . ? S C1 H1A 107.6 . . ? Sn C1 H1A 107.6 . . ? C1 C2 C6 116.5(3) . . ? C1 C2 C3 115.8(3) . . ? C6 C2 C3 103.9(3) . . ? C1 C2 H2A 106.6 . . ? C6 C2 H2A 106.6 . . ? C3 C2 H2A 106.6 . . ? C8 C3 C7 112.2(4) . . ? C8 C3 C2 111.0(3) . . ? C7 C3 C2 110.6(3) . . ? C8 C3 C4 112.8(3) . . ? C7 C3 C4 108.6(3) . . ? C2 C3 C4 101.0(3) . . ? C5 C4 C3 107.2(4) . . ? C5 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? C5 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? C4 C5 C6 107.0(4) . . ? C4 C5 H5A 110.3 . . ? C6 C5 H5A 110.3 . . ? C4 C5 H5B 110.3 . . ? C6 C5 H5B 110.3 . . ? H5A C5 H5B 108.6 . . ? C5 C6 C2 104.6(4) . . ? C5 C6 H6A 110.8 . . ? C2 C6 H6A 110.8 . . ? C5 C6 H6B 110.8 . . ? C2 C6 H6B 110.8 . . ? H6A C6 H6B 108.9 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 116.7(4) . . ? C13 C8 C3 123.0(4) . . ? C9 C8 C3 120.3(4) . . ? C10 C9 C8 121.8(4) . . ? C10 C9 H9A 119.1 . . ? C8 C9 H9A 119.1 . . ? C11 C10 C9 120.9(5) . . ? C11 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? C10 C11 C12 119.2(5) . . ? C10 C11 H11A 120.4 . . ? C12 C11 H11A 120.4 . . ? C11 C12 C13 120.1(5) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C8 C13 C12 121.3(5) . . ? C8 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C19 C14 C15 121.7(4) . . ? C19 C14 S 119.6(3) . . ? C15 C14 S 118.7(3) . . ? C16 C15 C14 118.5(4) . . ? C16 C15 C20 119.4(4) . . ? C14 C15 C20 122.1(4) . . ? C17 C16 C15 118.9(4) . . ? C17 C16 C21 120.0(4) . . ? C15 C16 C21 121.1(5) . . ? C16 C17 C18 123.8(4) . . ? C16 C17 H17A 118.1 . . ? C18 C17 H17A 118.1 . . ? C17 C18 C19 118.3(4) . . ? C17 C18 C22 120.3(4) . . ? C19 C18 C22 121.5(5) . . ? C14 C19 C18 118.7(4) . . ? C14 C19 C23 122.3(4) . . ? C18 C19 C23 119.0(4) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26' Sn' C25' 110.4(3) . . ? C26' Sn' C24' 105.7(3) . . ? C25' Sn' C24' 109.4(3) . . ? C26' Sn' C1' 108.05(18) . . ? C25' Sn' C1' 103.6(2) . . ? C24' Sn' C1' 119.57(19) . . ? C14' S' C1' 103.06(18) . . ? C2' C1' S' 112.5(3) . . ? C2' C1' Sn' 120.2(3) . . ? S' C1' Sn' 101.49(18) . . ? C2' C1' H1'A 107.3 . . ? S' C1' H1'A 107.3 . . ? Sn' C1' H1'A 107.3 . . ? C6' C2' C1' 117.1(3) . . ? C6' C2' C3' 105.0(3) . . ? C1' C2' C3' 115.2(3) . . ? C6' C2' H2'A 106.3 . . ? C1' C2' H2'A 106.3 . . ? C3' C2' H2'A 106.3 . . ? C8' C3' C7' 112.3(4) . . ? C8' C3' C2' 111.2(3) . . ? C7' C3' C2' 110.9(3) . . ? C8' C3' C4' 112.1(3) . . ? C7' C3' C4' 109.4(4) . . ? C2' C3' C4' 100.3(4) . . ? C5' C4' C3' 107.0(4) . . ? C5' C4' H4'A 110.3 . . ? C3' C4' H4'A 110.3 . . ? C5' C4' H4'B 110.3 . . ? C3' C4' H4'B 110.3 . . ? H4'A C4' H4'B 108.6 . . ? C4' C5' C6' 107.5(4) . . ? C4' C5' H5'A 110.2 . . ? C6' C5' H5'A 110.2 . . ? C4' C5' H5'B 110.2 . . ? C6' C5' H5'B 110.2 . . ? H5'A C5' H5'B 108.5 . . ? C5' C6' C2' 105.5(4) . . ? C5' C6' H6'A 110.6 . . ? C2' C6' H6'A 110.6 . . ? C5' C6' H6'B 110.6 . . ? C2' C6' H6'B 110.6 . . ? H6'A C6' H6'B 108.8 . . ? C3' C7' H7'A 109.5 . . ? C3' C7' H7'B 109.5 . . ? H7'A C7' H7'B 109.5 . . ? C3' C7' H7'C 109.5 . . ? H7'A C7' H7'C 109.5 . . ? H7'B C7' H7'C 109.5 . . ? C13' C8' C9' 116.2(4) . . ? C13' C8' C3' 122.9(4) . . ? C9' C8' C3' 121.0(4) . . ? C10' C9' C8' 121.3(5) . . ? C10' C9' H9'A 119.4 . . ? C8' C9' H9'A 119.4 . . ? C11' C10' C9' 121.0(6) . . ? C11' C10' H10B 119.5 . . ? C9' C10' H10B 119.5 . . ? C10' C11' C12' 119.5(6) . . ? C10' C11' H11B 120.3 . . ? C12' C11' H11B 120.3 . . ? C11' C12' C13' 119.8(6) . . ? C11' C12' H12B 120.1 . . ? C13' C12' H12B 120.1 . . ? C12' C13' C8' 122.3(5) . . ? C12' C13' H13B 118.9 . . ? C8' C13' H13B 118.9 . . ? C19' C14' C15' 121.1(4) . . ? C19' C14' S' 120.1(3) . . ? C15' C14' S' 118.8(3) . . ? C16' C15' C14' 118.9(4) . . ? C16' C15' C20' 118.8(4) . . ? C14' C15' C20' 122.2(4) . . ? C17' C16' C15' 119.4(4) . . ? C17' C16' C21' 119.2(4) . . ? C15' C16' C21' 121.3(4) . . ? C16' C17' C18' 122.6(4) . . ? C16' C17' H17B 118.7 . . ? C18' C17' H17B 118.7 . . ? C17' C18' C19' 118.7(4) . . ? C17' C18' C22' 119.4(4) . . ? C19' C18' C22' 121.8(4) . . ? C18' C19' C14' 119.2(4) . . ? C18' C19' C23' 118.8(4) . . ? C14' C19' C23' 122.0(4) . . ? C15' C20' H20D 109.5 . . ? C15' C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? C15' C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? C16' C21' H21D 109.5 . . ? C16' C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C16' C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? C18' C22' H22D 109.5 . . ? C18' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C18' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C19' C23' H23D 109.5 . . ? C19' C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C19' C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? Sn C26 H26A 109.5 . . ? Sn C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Sn C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Sn C25 H25A 109.5 . . ? Sn C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Sn C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Sn' C26' H26D 109.5 . . ? Sn' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? Sn' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? Sn C24 H24A 109.5 . . ? Sn C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Sn C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Sn' C25' H25D 109.5 . . ? Sn' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? Sn' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? Sn' C24' H24D 109.5 . . ? Sn' C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? Sn' C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 S C1 C2 64.4(3) . . . . ? C14 S C1 Sn -165.99(18) . . . . ? C25 Sn C1 C2 -172.5(3) . . . . ? C26 Sn C1 C2 69.9(3) . . . . ? C24 Sn C1 C2 -55.8(4) . . . . ? C25 Sn C1 S 63.9(2) . . . . ? C26 Sn C1 S -53.7(2) . . . . ? C24 Sn C1 S -179.4(3) . . . . ? S C1 C2 C6 92.0(4) . . . . ? Sn C1 C2 C6 -26.2(5) . . . . ? S C1 C2 C3 -145.3(3) . . . . ? Sn C1 C2 C3 96.5(3) . . . . ? C1 C2 C3 C8 71.2(4) . . . . ? C6 C2 C3 C8 -159.7(3) . . . . ? C1 C2 C3 C7 -54.1(4) . . . . ? C6 C2 C3 C7 75.0(4) . . . . ? C1 C2 C3 C4 -168.9(3) . . . . ? C6 C2 C3 C4 -39.8(4) . . . . ? C8 C3 C4 C5 147.2(4) . . . . ? C7 C3 C4 C5 -87.7(4) . . . . ? C2 C3 C4 C5 28.6(4) . . . . ? C3 C4 C5 C6 -6.7(5) . . . . ? C4 C5 C6 C2 -18.5(5) . . . . ? C1 C2 C6 C5 165.5(4) . . . . ? C3 C2 C6 C5 36.9(4) . . . . ? C7 C3 C8 C13 5.0(5) . . . . ? C2 C3 C8 C13 -119.4(4) . . . . ? C4 C3 C8 C13 128.1(4) . . . . ? C7 C3 C8 C9 -175.9(4) . . . . ? C2 C3 C8 C9 59.6(5) . . . . ? C4 C3 C8 C9 -52.9(5) . . . . ? C13 C8 C9 C10 0.4(6) . . . . ? C3 C8 C9 C10 -178.7(4) . . . . ? C8 C9 C10 C11 -0.6(7) . . . . ? C9 C10 C11 C12 0.7(8) . . . . ? C10 C11 C12 C13 -0.7(8) . . . . ? C9 C8 C13 C12 -0.4(6) . . . . ? C3 C8 C13 C12 178.7(4) . . . . ? C11 C12 C13 C8 0.5(8) . . . . ? C1 S C14 C19 74.5(3) . . . . ? C1 S C14 C15 -106.5(3) . . . . ? C19 C14 C15 C16 -1.1(5) . . . . ? S C14 C15 C16 179.9(3) . . . . ? C19 C14 C15 C20 179.5(4) . . . . ? S C14 C15 C20 0.5(5) . . . . ? C14 C15 C16 C17 1.3(5) . . . . ? C20 C15 C16 C17 -179.3(4) . . . . ? C14 C15 C16 C21 -179.4(4) . . . . ? C20 C15 C16 C21 0.0(6) . . . . ? C15 C16 C17 C18 -1.1(6) . . . . ? C21 C16 C17 C18 179.5(4) . . . . ? C16 C17 C18 C19 0.7(6) . . . . ? C16 C17 C18 C22 -179.4(4) . . . . ? C15 C14 C19 C18 0.7(5) . . . . ? S C14 C19 C18 179.7(3) . . . . ? C15 C14 C19 C23 179.0(4) . . . . ? S C14 C19 C23 -2.0(5) . . . . ? C17 C18 C19 C14 -0.5(6) . . . . ? C22 C18 C19 C14 179.6(4) . . . . ? C17 C18 C19 C23 -178.8(4) . . . . ? C22 C18 C19 C23 1.3(6) . . . . ? C14' S' C1' C2' -61.0(3) . . . . ? C14' S' C1' Sn' 169.18(18) . . . . ? C26' Sn' C1' C2' -87.5(4) . . . . ? C25' Sn' C1' C2' 155.4(4) . . . . ? C24' Sn' C1' C2' 33.3(4) . . . . ? C26' Sn' C1' S' 37.4(3) . . . . ? C25' Sn' C1' S' -79.8(3) . . . . ? C24' Sn' C1' S' 158.2(3) . . . . ? S' C1' C2' C6' -88.7(4) . . . . ? Sn' C1' C2' C6' 30.7(5) . . . . ? S' C1' C2' C3' 147.2(3) . . . . ? Sn' C1' C2' C3' -93.4(4) . . . . ? C6' C2' C3' C8' 156.7(4) . . . . ? C1' C2' C3' C8' -73.0(4) . . . . ? C6' C2' C3' C7' -77.5(4) . . . . ? C1' C2' C3' C7' 52.8(5) . . . . ? C6' C2' C3' C4' 38.0(4) . . . . ? C1' C2' C3' C4' 168.3(3) . . . . ? C8' C3' C4' C5' -149.8(4) . . . . ? C7' C3' C4' C5' 84.9(5) . . . . ? C2' C3' C4' C5' -31.7(5) . . . . ? C3' C4' C5' C6' 13.9(6) . . . . ? C4' C5' C6' C2' 10.5(6) . . . . ? C1' C2' C6' C5' -160.1(4) . . . . ? C3' C2' C6' C5' -31.0(5) . . . . ? C7' C3' C8' C13' -4.4(6) . . . . ? C2' C3' C8' C13' 120.5(4) . . . . ? C4' C3' C8' C13' -128.1(5) . . . . ? C7' C3' C8' C9' 176.6(4) . . . . ? C2' C3' C8' C9' -58.4(5) . . . . ? C4' C3' C8' C9' 53.0(5) . . . . ? C13' C8' C9' C10' 0.0(6) . . . . ? C3' C8' C9' C10' 179.0(4) . . . . ? C8' C9' C10' C11' 0.5(8) . . . . ? C9' C10' C11' C12' -0.7(9) . . . . ? C10' C11' C12' C13' 0.4(10) . . . . ? C11' C12' C13' C8' 0.1(9) . . . . ? C9' C8' C13' C12' -0.3(7) . . . . ? C3' C8' C13' C12' -179.3(5) . . . . ? C1' S' C14' C19' -75.1(3) . . . . ? C1' S' C14' C15' 103.8(3) . . . . ? C19' C14' C15' C16' 1.8(6) . . . . ? S' C14' C15' C16' -177.1(3) . . . . ? C19' C14' C15' C20' -177.7(4) . . . . ? S' C14' C15' C20' 3.4(5) . . . . ? C14' C15' C16' C17' -1.4(6) . . . . ? C20' C15' C16' C17' 178.1(4) . . . . ? C14' C15' C16' C21' 176.2(4) . . . . ? C20' C15' C16' C21' -4.3(6) . . . . ? C15' C16' C17' C18' -0.7(6) . . . . ? C21' C16' C17' C18' -178.3(4) . . . . ? C16' C17' C18' C19' 2.3(6) . . . . ? C16' C17' C18' C22' -180.0(4) . . . . ? C17' C18' C19' C14' -1.9(6) . . . . ? C22' C18' C19' C14' -179.5(4) . . . . ? C17' C18' C19' C23' 177.8(4) . . . . ? C22' C18' C19' C23' 0.2(6) . . . . ? C15' C14' C19' C18' -0.1(6) . . . . ? S' C14' C19' C18' 178.8(3) . . . . ? C15' C14' C19' C23' -179.8(4) . . . . ? S' C14' C19' C23' -0.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.821 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.821 _refine_diff_density_max 0.529 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.069 # = = = END data_kob2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H32 S' _chemical_formula_weight 352.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.963(4) _cell_length_b 6.0560(10) _cell_length_c 18.185(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.210(10) _cell_angle_gamma 90.00 _cell_volume 4074.5(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 118 _cell_measurement_theta_min 20 _cell_measurement_theta_max 40 _exptl_crystal_description Regular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.404 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5708 _exptl_absorpt_correction_T_max 0.8496 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method Omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3550 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 65.28 _reflns_number_total 3492 _reflns_number_gt 2772 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 (Harms, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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 w=1/[\s^2^(Fo^2^)+(0.1046P)^2^+2.2123P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00019(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3492 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1858 _refine_ls_wR_factor_gt 0.1734 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.096494(19) 0.24450(13) 0.05209(5) 0.0819(3) Uani 1 d . . . C1 C 0.13177(7) 0.0413(5) 0.05952(16) 0.0663(7) Uani 1 d . . . H1 H 0.1194(7) -0.095(5) 0.0283(16) 0.072(8) Uiso 1 d . . . C2 C 0.15393(6) 0.1469(5) 0.01562(15) 0.0621(6) Uani 1 d . . . H2 H 0.1631(8) 0.296(5) 0.0417(17) 0.077(8) Uiso 1 d . . . C3 C 0.18630(6) 0.0110(4) 0.01140(14) 0.0618(6) Uani 1 d . . . C4 C 0.19300(8) 0.1345(6) -0.05596(17) 0.0773(8) Uani 1 d . . . H4B H 0.2063(9) 0.052(6) -0.082(2) 0.106(11) Uiso 1 d . . . H4A H 0.2046(9) 0.281(6) -0.035(2) 0.100(11) Uiso 1 d . . . C5 C 0.15594(10) 0.1851(10) -0.1179(2) 0.0971(11) Uani 1 d . . . H5A H 0.1585(13) 0.312(9) -0.143(3) 0.154(18) Uiso 1 d . . . H5B H 0.1480(11) 0.065(7) -0.153(2) 0.119(14) Uiso 1 d . . . C6 C 0.13100(9) 0.2017(6) -0.07188(17) 0.0782(8) Uani 1 d . . . H6A H 0.1106(9) 0.102(5) -0.0928(17) 0.084(9) Uiso 1 d . . . H6B H 0.1207(9) 0.349(6) -0.073(2) 0.101(11) Uiso 1 d . . . C7 C 0.15374(9) -0.0155(7) 0.14530(19) 0.0844(9) Uani 1 d . . . H7B H 0.1715(9) -0.130(6) 0.1467(17) 0.085(9) Uiso 1 d . . . H7A H 0.1390(9) -0.078(6) 0.172(2) 0.100(10) Uiso 1 d . . . H7C H 0.1657(11) 0.127(8) 0.175(2) 0.129(15) Uiso 1 d . . . C8 C 0.22101(6) 0.0182(4) 0.08540(13) 0.0584(6) Uani 1 d . . . C9 C 0.24534(7) -0.1563(5) 0.10491(16) 0.0708(7) Uani 1 d . . . H9 H 0.2397(7) -0.286(5) 0.0713(17) 0.078(9) Uiso 1 d . . . C10 C 0.27820(8) -0.1434(6) 0.16846(17) 0.0793(8) Uani 1 d . . . H10 H 0.2920(9) -0.269(5) 0.1751(19) 0.088(10) Uiso 1 d . . . C11 C 0.28776(7) 0.0418(6) 0.21438(16) 0.0756(8) Uani 1 d . . . H11 H 0.3122(8) 0.046(5) 0.2613(18) 0.087(9) Uiso 1 d . . . C12 C 0.26406(8) 0.2153(6) 0.19638(18) 0.0742(7) Uani 1 d . . . H12 H 0.2688(8) 0.346(6) 0.2238(18) 0.084(9) Uiso 1 d . . . C13 C 0.23177(8) 0.2048(5) 0.13300(17) 0.0693(7) Uani 1 d . . . H13 H 0.2169(9) 0.322(6) 0.1241(18) 0.091(10) Uiso 1 d . . . C14 C 0.17436(10) -0.2245(5) -0.0146(2) 0.0802(8) Uani 1 d . . . H14C H 0.1707(9) -0.312(6) 0.031(2) 0.093(10) Uiso 1 d . . . H14B H 0.1525(10) -0.226(5) -0.054(2) 0.097(11) Uiso 1 d . . . H14A H 0.1898(9) -0.299(6) -0.0327(19) 0.091(10) Uiso 1 d . . . C15 C 0.07450(6) 0.1321(5) 0.11181(16) 0.0700(7) Uani 1 d . . . C16 C 0.05157(6) -0.0524(5) 0.08524(16) 0.0718(7) Uani 1 d . . . C17 C 0.03375(7) -0.1305(6) 0.13241(19) 0.0818(8) Uani 1 d . . . C18 C 0.03837(8) -0.0238(7) 0.2023(2) 0.0911(10) Uani 1 d . . . H18 H 0.0264(10) -0.087(6) 0.236(2) 0.118(12) Uiso 1 d . . . C19 C 0.05991(8) 0.1609(7) 0.22841(18) 0.0868(9) Uani 1 d . . . C20 C 0.07885(7) 0.2383(5) 0.18378(18) 0.0769(8) Uani 1 d . . . C21 C 0.04599(11) -0.1632(8) 0.0077(2) 0.0926(10) Uani 1 d . . . H21B H 0.0210(11) -0.190(6) -0.023(2) 0.108(11) Uiso 1 d . . . H21A H 0.0522(12) -0.065(8) -0.029(3) 0.143(17) Uiso 1 d . . . H21C H 0.0572(13) -0.292(9) 0.016(3) 0.143(18) Uiso 1 d . . . C22 C 0.00935(12) -0.3288(9) 0.1081(4) 0.1154(14) Uani 1 d . . . H22C H -0.0138(14) -0.297(8) 0.056(3) 0.147(16) Uiso 1 d . . . H22B H 0.0232(13) -0.469(10) 0.105(3) 0.156(18) Uiso 1 d . . . H22A H 0.0017(16) -0.364(10) 0.148(4) 0.18(2) Uiso 1 d . . . C23 C 0.06152(17) 0.2722(13) 0.3040(3) 0.1259(18) Uani 1 d . . . H23C H 0.0887(16) 0.280(8) 0.339(3) 0.162(19) Uiso 1 d . . . H23B H 0.0520(15) 0.408(10) 0.295(3) 0.16(2) Uiso 1 d . . . H23A H 0.0462(15) 0.219(9) 0.328(3) 0.16(2) Uiso 1 d . . . C24 C 0.10357(12) 0.4333(9) 0.2135(3) 0.1066(13) Uani 1 d . . . H24C H 0.0946(15) 0.555(11) 0.227(3) 0.18(2) Uiso 1 d . . . H24B H 0.1250(15) 0.397(9) 0.262(3) 0.161(18) Uiso 1 d . . . H24A H 0.1116(15) 0.488(10) 0.176(3) 0.18(3) Uiso 1 d . . . 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 S1 0.0749(5) 0.0780(6) 0.0970(6) 0.0186(4) 0.0374(4) 0.0138(3) C1 0.0621(13) 0.0639(16) 0.0699(15) 0.0102(13) 0.0217(12) 0.0021(12) C2 0.0654(13) 0.0568(15) 0.0613(14) 0.0081(12) 0.0208(11) 0.0029(12) C3 0.0670(13) 0.0566(15) 0.0605(13) -0.0021(11) 0.0226(11) -0.0017(11) C4 0.0844(18) 0.088(2) 0.0632(15) 0.0070(15) 0.0321(14) 0.0047(17) C5 0.096(2) 0.127(3) 0.0659(19) 0.019(2) 0.0276(17) 0.010(2) C6 0.0748(17) 0.086(2) 0.0648(16) 0.0146(15) 0.0159(13) 0.0064(16) C7 0.0740(17) 0.106(3) 0.0762(18) 0.0313(19) 0.0319(15) 0.0157(19) C8 0.0646(13) 0.0550(14) 0.0567(12) 0.0014(10) 0.0240(10) 0.0007(11) C9 0.0759(16) 0.0667(17) 0.0665(15) -0.0036(13) 0.0231(13) 0.0089(14) C10 0.0768(17) 0.083(2) 0.0728(17) 0.0036(16) 0.0227(14) 0.0182(16) C11 0.0652(15) 0.094(2) 0.0643(15) -0.0041(15) 0.0203(12) 0.0002(15) C12 0.0693(16) 0.074(2) 0.0769(17) -0.0118(15) 0.0252(13) -0.0085(14) C13 0.0690(15) 0.0589(16) 0.0773(17) -0.0064(13) 0.0246(13) 0.0011(13) C14 0.0773(19) 0.067(2) 0.087(2) -0.0135(16) 0.0203(17) -0.0018(15) C15 0.0562(13) 0.0766(19) 0.0722(16) -0.0005(14) 0.0186(11) 0.0048(12) C16 0.0567(13) 0.0761(18) 0.0748(16) -0.0012(14) 0.0161(12) 0.0038(12) C17 0.0625(14) 0.083(2) 0.095(2) 0.0110(17) 0.0244(14) 0.0024(14) C18 0.0755(17) 0.111(3) 0.092(2) 0.021(2) 0.0384(17) 0.0126(18) C19 0.0764(17) 0.110(3) 0.0694(17) -0.0005(17) 0.0223(14) 0.0152(18) C20 0.0633(15) 0.082(2) 0.0757(17) -0.0047(14) 0.0147(13) 0.0060(13) C21 0.079(2) 0.100(3) 0.087(2) -0.020(2) 0.0171(17) 0.001(2) C22 0.082(2) 0.099(3) 0.156(4) 0.016(3) 0.034(3) -0.014(2) C23 0.125(4) 0.170(6) 0.080(2) -0.013(3) 0.036(2) 0.029(4) C24 0.089(2) 0.101(3) 0.113(3) -0.031(3) 0.020(2) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C15 1.771(3) . ? S1 C1 1.837(3) . ? C1 C7 1.512(4) . ? C1 C2 1.538(3) . ? C1 H1 1.02(3) . ? C2 C6 1.543(4) . ? C2 C3 1.559(3) . ? C2 H2 1.02(3) . ? C3 C14 1.522(4) . ? C3 C8 1.525(3) . ? C3 C4 1.543(4) . ? C4 C5 1.515(5) . ? C4 H4B 0.97(4) . ? C4 H4A 1.00(4) . ? C5 C6 1.528(5) . ? C5 H5A 0.93(5) . ? C5 H5B 0.94(4) . ? C6 H6A 0.97(3) . ? C6 H6B 0.98(4) . ? C7 H7B 0.99(3) . ? C7 H7A 0.97(4) . ? C7 H7C 1.04(5) . ? C8 C9 1.389(4) . ? C8 C13 1.389(4) . ? C9 C10 1.385(4) . ? C9 H9 0.97(3) . ? C10 C11 1.364(4) . ? C10 H10 0.92(3) . ? C11 C12 1.369(4) . ? C11 H11 1.03(3) . ? C12 C13 1.369(4) . ? C12 H12 0.92(3) . ? C13 H13 0.90(3) . ? C14 H14C 1.04(4) . ? C14 H14B 0.90(4) . ? C14 H14A 0.92(4) . ? C15 C20 1.409(4) . ? C15 C16 1.409(4) . ? C16 C17 1.389(4) . ? C16 C21 1.501(5) . ? C17 C18 1.375(5) . ? C17 C22 1.505(5) . ? C18 C19 1.381(5) . ? C18 H18 0.98(4) . ? C19 C20 1.384(5) . ? C19 C23 1.511(5) . ? C20 C24 1.503(5) . ? C21 H21B 0.96(4) . ? C21 H21A 1.00(5) . ? C21 H21C 0.89(5) . ? C22 H22C 1.06(5) . ? C22 H22B 1.02(6) . ? C22 H22A 0.91(6) . ? C23 H23C 1.03(6) . ? C23 H23B 0.89(6) . ? C23 H23A 0.94(6) . ? C24 H24C 0.90(6) . ? C24 H24B 1.00(6) . ? C24 H24A 0.92(6) . ? 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 C15 S1 C1 104.01(12) . . ? C7 C1 C2 114.0(2) . . ? C7 C1 S1 111.0(2) . . ? C2 C1 S1 105.04(18) . . ? C7 C1 H1 111.2(15) . . ? C2 C1 H1 107.5(15) . . ? S1 C1 H1 107.7(15) . . ? C1 C2 C6 113.0(2) . . ? C1 C2 C3 117.2(2) . . ? C6 C2 C3 104.1(2) . . ? C1 C2 H2 107.6(16) . . ? C6 C2 H2 105.0(16) . . ? C3 C2 H2 109.3(16) . . ? C14 C3 C8 112.0(2) . . ? C14 C3 C4 109.6(3) . . ? C8 C3 C4 108.3(2) . . ? C14 C3 C2 110.0(2) . . ? C8 C3 C2 115.9(2) . . ? C4 C3 C2 100.4(2) . . ? C5 C4 C3 105.9(2) . . ? C5 C4 H4B 108(2) . . ? C3 C4 H4B 115(2) . . ? C5 C4 H4A 106(2) . . ? C3 C4 H4A 109(2) . . ? H4B C4 H4A 112(3) . . ? C4 C5 C6 105.2(2) . . ? C4 C5 H5A 106(3) . . ? C6 C5 H5A 116(3) . . ? C4 C5 H5B 109(3) . . ? C6 C5 H5B 108(2) . . ? H5A C5 H5B 112(4) . . ? C5 C6 C2 107.1(2) . . ? C5 C6 H6A 111.8(18) . . ? C2 C6 H6A 110.8(18) . . ? C5 C6 H6B 114(2) . . ? C2 C6 H6B 107(2) . . ? H6A C6 H6B 106(3) . . ? C1 C7 H7B 108.6(18) . . ? C1 C7 H7A 112(2) . . ? H7B C7 H7A 106(3) . . ? C1 C7 H7C 109(2) . . ? H7B C7 H7C 113(3) . . ? H7A C7 H7C 109(3) . . ? C9 C8 C13 116.0(2) . . ? C9 C8 C3 121.3(2) . . ? C13 C8 C3 122.5(2) . . ? C10 C9 C8 121.4(3) . . ? C10 C9 H9 119.5(17) . . ? C8 C9 H9 118.9(17) . . ? C11 C10 C9 121.0(3) . . ? C11 C10 H10 126(2) . . ? C9 C10 H10 113(2) . . ? C10 C11 C12 118.5(3) . . ? C10 C11 H11 119.2(18) . . ? C12 C11 H11 122.3(18) . . ? C13 C12 C11 120.8(3) . . ? C13 C12 H12 115.7(19) . . ? C11 C12 H12 123.4(19) . . ? C12 C13 C8 122.3(3) . . ? C12 C13 H13 118(2) . . ? C8 C13 H13 120(2) . . ? C3 C14 H14C 110.8(19) . . ? C3 C14 H14B 111(2) . . ? H14C C14 H14B 104(3) . . ? C3 C14 H14A 113(2) . . ? H14C C14 H14A 110(3) . . ? H14B C14 H14A 107(3) . . ? C20 C15 C16 121.1(3) . . ? C20 C15 S1 118.6(2) . . ? C16 C15 S1 120.2(2) . . ? C17 C16 C15 118.5(3) . . ? C17 C16 C21 120.0(3) . . ? C15 C16 C21 121.5(3) . . ? C18 C17 C16 119.4(3) . . ? C18 C17 C22 119.5(4) . . ? C16 C17 C22 121.2(4) . . ? C17 C18 C19 123.1(3) . . ? C17 C18 H18 118(2) . . ? C19 C18 H18 119(2) . . ? C18 C19 C20 118.7(3) . . ? C18 C19 C23 118.7(4) . . ? C20 C19 C23 122.5(4) . . ? C19 C20 C15 119.2(3) . . ? C19 C20 C24 119.1(3) . . ? C15 C20 C24 121.8(3) . . ? C16 C21 H21B 112(2) . . ? C16 C21 H21A 112(3) . . ? H21B C21 H21A 100(3) . . ? C16 C21 H21C 111(3) . . ? H21B C21 H21C 107(4) . . ? H21A C21 H21C 114(4) . . ? C17 C22 H22C 111(3) . . ? C17 C22 H22B 112(3) . . ? H22C C22 H22B 114(4) . . ? C17 C22 H22A 109(4) . . ? H22C C22 H22A 108(4) . . ? H22B C22 H22A 101(4) . . ? C19 C23 H23C 105(3) . . ? C19 C23 H23B 112(4) . . ? H23C C23 H23B 110(5) . . ? C19 C23 H23A 118(4) . . ? H23C C23 H23A 117(5) . . ? H23B C23 H23A 95(4) . . ? C20 C24 H24C 118(4) . . ? C20 C24 H24B 112(3) . . ? H24C C24 H24B 104(4) . . ? C20 C24 H24A 112(4) . . ? H24C C24 H24A 101(5) . . ? H24B C24 H24A 109(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 S1 C1 C7 -50.4(3) . . . . ? C15 S1 C1 C2 -174.03(18) . . . . ? C7 C1 C2 C6 179.6(3) . . . . ? S1 C1 C2 C6 -58.7(3) . . . . ? C7 C1 C2 C3 58.5(4) . . . . ? S1 C1 C2 C3 -179.75(18) . . . . ? C1 C2 C3 C14 48.0(3) . . . . ? C6 C2 C3 C14 -77.6(3) . . . . ? C1 C2 C3 C8 -80.2(3) . . . . ? C6 C2 C3 C8 154.2(2) . . . . ? C1 C2 C3 C4 163.5(2) . . . . ? C6 C2 C3 C4 37.8(3) . . . . ? C14 C3 C4 C5 74.8(4) . . . . ? C8 C3 C4 C5 -162.7(3) . . . . ? C2 C3 C4 C5 -40.9(3) . . . . ? C3 C4 C5 C6 27.9(4) . . . . ? C4 C5 C6 C2 -3.2(5) . . . . ? C1 C2 C6 C5 -150.4(3) . . . . ? C3 C2 C6 C5 -22.1(4) . . . . ? C14 C3 C8 C9 24.3(3) . . . . ? C4 C3 C8 C9 -96.6(3) . . . . ? C2 C3 C8 C9 151.6(2) . . . . ? C14 C3 C8 C13 -161.5(3) . . . . ? C4 C3 C8 C13 77.5(3) . . . . ? C2 C3 C8 C13 -34.3(3) . . . . ? C13 C8 C9 C10 0.3(4) . . . . ? C3 C8 C9 C10 174.8(2) . . . . ? C8 C9 C10 C11 0.2(5) . . . . ? C9 C10 C11 C12 0.1(5) . . . . ? C10 C11 C12 C13 -1.1(4) . . . . ? C11 C12 C13 C8 1.7(4) . . . . ? C9 C8 C13 C12 -1.3(4) . . . . ? C3 C8 C13 C12 -175.7(2) . . . . ? C1 S1 C15 C20 110.6(2) . . . . ? C1 S1 C15 C16 -72.9(2) . . . . ? C20 C15 C16 C17 -1.2(4) . . . . ? S1 C15 C16 C17 -177.6(2) . . . . ? C20 C15 C16 C21 178.4(3) . . . . ? S1 C15 C16 C21 2.0(4) . . . . ? C15 C16 C17 C18 1.3(4) . . . . ? C21 C16 C17 C18 -178.3(3) . . . . ? C15 C16 C17 C22 -179.0(3) . . . . ? C21 C16 C17 C22 1.4(5) . . . . ? C16 C17 C18 C19 0.5(5) . . . . ? C22 C17 C18 C19 -179.2(3) . . . . ? C17 C18 C19 C20 -2.5(5) . . . . ? C17 C18 C19 C23 176.8(4) . . . . ? C18 C19 C20 C15 2.5(4) . . . . ? C23 C19 C20 C15 -176.8(4) . . . . ? C18 C19 C20 C24 -177.4(3) . . . . ? C23 C19 C20 C24 3.3(5) . . . . ? C16 C15 C20 C19 -0.7(4) . . . . ? S1 C15 C20 C19 175.7(2) . . . . ? C16 C15 C20 C24 179.2(3) . . . . ? S1 C15 C20 C24 -4.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.452 _diffrn_reflns_theta_full 65.28 _diffrn_measured_fraction_theta_full 0.452 _refine_diff_density_max 0.379 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.039 # = = = END data_kob02 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 O S' _chemical_formula_weight 444.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 '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 10.6210(10) _cell_length_b 10.9180(10) _cell_length_c 11.8420(10) _cell_angle_alpha 77.560(10) _cell_angle_beta 67.200(10) _cell_angle_gamma 81.250(10) _cell_volume 1232.58(19) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 40.0 _cell_measurement_theta_max 46.4 _exptl_crystal_description unregelm&a&sig _exptl_crystal_colour farblos _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 1.297 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6249 _exptl_absorpt_correction_T_max 0.8292 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method Omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4429 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 64.87 _reflns_number_total 4182 _reflns_number_gt 3589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 (Harms, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0685P)^2^+0.3720P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0038(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4182 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 S1 S 0.38919(5) 0.73517(4) 0.19399(4) 0.03174(16) Uani 1 1 d . . . O1 O 0.36539(14) 0.98694(13) 0.00683(12) 0.0370(3) Uani 1 1 d . . . H1A H 0.430(3) 0.934(3) 0.004(3) 0.079(10) Uiso 1 1 d . . . C1 C 0.24590(17) 0.92959(16) 0.09401(16) 0.0267(4) Uani 1 1 d . . . H1 H 0.234(2) 0.859(2) 0.0610(18) 0.035(5) Uiso 1 1 d . . . C2 C 0.26335(18) 0.87341(16) 0.21911(16) 0.0255(4) Uani 1 1 d . . . H2 H 0.1757(19) 0.8446(17) 0.2790(17) 0.022(4) Uiso 1 1 d . . . C3 C 0.31540(18) 0.96443(16) 0.27145(16) 0.0268(4) Uani 1 1 d . . . H3 H 0.407(2) 0.9857(18) 0.2100(18) 0.027(5) Uiso 1 1 d . . . C4 C 0.32818(19) 0.91688(18) 0.40146(17) 0.0317(4) Uani 1 1 d . . . C5 C 0.3474(2) 1.0428(2) 0.4309(2) 0.0405(5) Uani 1 1 d . . . H5A H 0.334(2) 1.034(2) 0.519(2) 0.051(6) Uiso 1 1 d . . . H5B H 0.439(2) 1.070(2) 0.3755(19) 0.038(6) Uiso 1 1 d . . . C6 C 0.2465(3) 1.1399(2) 0.3904(2) 0.0461(5) Uani 1 1 d . . . H6A H 0.156(3) 1.146(2) 0.462(2) 0.060(7) Uiso 1 1 d . . . H6B H 0.286(3) 1.225(3) 0.357(3) 0.070(8) Uiso 1 1 d . . . C7 C 0.2247(2) 1.08998(18) 0.2876(2) 0.0356(4) Uani 1 1 d . . . H7A H 0.249(2) 1.152(2) 0.207(2) 0.049(6) Uiso 1 1 d . . . H7B H 0.128(2) 1.0730(19) 0.3156(19) 0.036(5) Uiso 1 1 d . . . C8 C 0.45214(19) 0.82506(17) 0.40161(16) 0.0317(4) Uani 1 1 d . . . C9 C 0.4435(3) 0.7237(2) 0.4977(2) 0.0478(5) Uani 1 1 d . . . H9 H 0.355(2) 0.705(2) 0.563(2) 0.052(7) Uiso 1 1 d . . . C10 C 0.5586(3) 0.6445(3) 0.5003(2) 0.0612(7) Uani 1 1 d . . . H10 H 0.548(3) 0.576(3) 0.566(3) 0.082(9) Uiso 1 1 d . . . C11 C 0.6841(3) 0.6644(2) 0.4078(2) 0.0544(6) Uani 1 1 d . . . H11 H 0.763(3) 0.607(3) 0.408(3) 0.072(8) Uiso 1 1 d . . . C12 C 0.6953(2) 0.7642(2) 0.3115(2) 0.0446(5) Uani 1 1 d . . . H12 H 0.784(3) 0.777(2) 0.242(2) 0.057(7) Uiso 1 1 d . . . C13 C 0.5807(2) 0.8436(2) 0.30913(19) 0.0369(5) Uani 1 1 d . . . H13 H 0.592(2) 0.915(2) 0.240(2) 0.053(7) Uiso 1 1 d . . . C14 C 0.12123(18) 1.02078(16) 0.10218(16) 0.0276(4) Uani 1 1 d . . . C15 C 0.1321(2) 1.13986(18) 0.03010(19) 0.0358(4) Uani 1 1 d . . . H15 H 0.217(2) 1.168(2) -0.0190(19) 0.036(6) Uiso 1 1 d . . . C16 C 0.0143(3) 1.2178(2) 0.0335(2) 0.0456(5) Uani 1 1 d . . . H16 H 0.027(2) 1.299(2) -0.023(2) 0.056(7) Uiso 1 1 d . . . C17 C -0.1129(2) 1.1781(2) 0.1087(2) 0.0470(6) Uani 1 1 d . . . H17 H -0.198(3) 1.234(3) 0.115(3) 0.073(8) Uiso 1 1 d . . . C18 C -0.1249(2) 1.0596(2) 0.1809(2) 0.0433(5) Uani 1 1 d . . . H18 H -0.213(3) 1.029(2) 0.238(2) 0.065(8) Uiso 1 1 d . . . C19 C -0.0078(2) 0.98113(19) 0.17619(19) 0.0360(4) Uani 1 1 d . . . H19 H -0.016(2) 0.895(2) 0.227(2) 0.046(6) Uiso 1 1 d . . . C20 C 0.31250(18) 0.63678(15) 0.13931(16) 0.0282(4) Uani 1 1 d . . . C21 C 0.36698(19) 0.62569(16) 0.01234(17) 0.0315(4) Uani 1 1 d . . . C22 C 0.3057(2) 0.54634(17) -0.02733(18) 0.0360(5) Uani 1 1 d . . . C23 C 0.1959(2) 0.48233(19) 0.0580(2) 0.0400(5) Uani 1 1 d . . . H23 H 0.156(2) 0.428(2) 0.031(2) 0.054(7) Uiso 1 1 d . . . C24 C 0.1431(2) 0.49026(18) 0.1833(2) 0.0384(5) Uani 1 1 d . . . C25 C 0.20299(19) 0.56748(16) 0.22556(17) 0.0318(4) Uani 1 1 d . . . C26 C 0.4862(2) 0.6959(2) -0.0814(2) 0.0422(5) Uani 1 1 d . . . H26A H 0.536(3) 0.732(3) -0.038(3) 0.071(8) Uiso 1 1 d . . . H26B H 0.554(3) 0.644(3) -0.138(2) 0.066(8) Uiso 1 1 d . . . H26C H 0.456(3) 0.773(3) -0.134(3) 0.084(9) Uiso 1 1 d . . . C27 C 0.3567(3) 0.5315(3) -0.1621(2) 0.0541(6) Uani 1 1 d . . . H27A H 0.302(4) 0.476(4) -0.172(3) 0.107(12) Uiso 1 1 d . . . H27B H 0.358(3) 0.607(3) -0.215(3) 0.074(9) Uiso 1 1 d . . . H27C H 0.453(3) 0.499(3) -0.192(3) 0.085(10) Uiso 1 1 d . . . C28 C 0.0246(3) 0.4143(3) 0.2707(3) 0.0574(7) Uani 1 1 d . . . H28A H -0.054(3) 0.468(3) 0.315(3) 0.083(9) Uiso 1 1 d . . . H28B H 0.000(3) 0.365(3) 0.228(3) 0.093(11) Uiso 1 1 d . . . H28C H 0.045(3) 0.351(3) 0.337(3) 0.101(12) Uiso 1 1 d . . . C29 C 0.1500(3) 0.5731(2) 0.3624(2) 0.0490(6) Uani 1 1 d . . . H29A H 0.128(3) 0.492(3) 0.415(3) 0.065(8) Uiso 1 1 d . . . H29B H 0.066(3) 0.631(3) 0.387(3) 0.078(9) Uiso 1 1 d . . . H29C H 0.221(3) 0.608(3) 0.384(3) 0.078(9) Uiso 1 1 d . . . C30 C 0.1935(2) 0.8663(2) 0.49634(19) 0.0421(5) Uani 1 1 d . . . H30A H 0.180(2) 0.781(3) 0.483(2) 0.057(7) Uiso 1 1 d . . . H30B H 0.114(3) 0.924(2) 0.492(2) 0.055(7) Uiso 1 1 d . . . H30C H 0.183(2) 0.859(2) 0.584(2) 0.054(7) Uiso 1 1 d . . . 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 S1 0.0364(3) 0.0219(3) 0.0443(3) -0.00945(19) -0.0226(2) 0.00260(17) O1 0.0334(7) 0.0376(8) 0.0342(7) 0.0015(6) -0.0099(6) -0.0036(6) C1 0.0317(9) 0.0210(9) 0.0302(9) -0.0056(7) -0.0136(7) -0.0030(7) C2 0.0285(9) 0.0198(9) 0.0303(9) -0.0040(7) -0.0129(8) -0.0030(7) C3 0.0304(9) 0.0226(9) 0.0313(9) -0.0060(7) -0.0142(8) -0.0034(7) C4 0.0381(10) 0.0311(10) 0.0309(9) -0.0078(8) -0.0164(8) -0.0037(8) C5 0.0501(13) 0.0384(12) 0.0438(12) -0.0160(9) -0.0250(10) -0.0016(9) C6 0.0572(14) 0.0371(12) 0.0582(14) -0.0239(11) -0.0315(12) 0.0051(10) C7 0.0434(11) 0.0247(10) 0.0464(12) -0.0137(9) -0.0226(9) 0.0026(8) C8 0.0413(10) 0.0311(10) 0.0301(9) -0.0065(8) -0.0195(8) -0.0053(8) C9 0.0564(14) 0.0443(13) 0.0362(11) 0.0024(9) -0.0159(10) -0.0008(11) C10 0.0811(18) 0.0491(15) 0.0474(14) 0.0048(11) -0.0303(13) 0.0118(13) C11 0.0636(15) 0.0519(15) 0.0539(14) -0.0157(11) -0.0330(13) 0.0184(12) C12 0.0436(12) 0.0516(14) 0.0457(12) -0.0130(10) -0.0234(10) 0.0011(10) C13 0.0396(11) 0.0365(11) 0.0401(11) -0.0040(9) -0.0210(9) -0.0058(9) C14 0.0370(10) 0.0212(9) 0.0331(9) -0.0084(7) -0.0210(8) 0.0006(7) C15 0.0481(12) 0.0245(10) 0.0421(11) -0.0047(8) -0.0249(10) -0.0030(9) C16 0.0708(16) 0.0223(10) 0.0612(14) -0.0116(10) -0.0451(13) 0.0081(10) C17 0.0546(13) 0.0400(13) 0.0684(15) -0.0304(11) -0.0428(12) 0.0177(10) C18 0.0376(11) 0.0473(13) 0.0551(13) -0.0201(10) -0.0249(10) 0.0050(9) C19 0.0369(10) 0.0321(11) 0.0454(11) -0.0080(9) -0.0220(9) -0.0012(8) C20 0.0362(9) 0.0165(8) 0.0346(9) -0.0049(7) -0.0175(8) 0.0031(7) C21 0.0394(10) 0.0198(9) 0.0351(10) -0.0046(7) -0.0166(8) 0.0063(7) C22 0.0518(12) 0.0222(9) 0.0407(11) -0.0113(8) -0.0259(9) 0.0106(8) C23 0.0507(12) 0.0256(10) 0.0559(13) -0.0158(9) -0.0301(11) 0.0022(9) C24 0.0394(10) 0.0222(10) 0.0552(12) -0.0085(9) -0.0184(9) -0.0018(8) C25 0.0407(10) 0.0189(9) 0.0359(10) -0.0050(7) -0.0152(8) 0.0008(8) C26 0.0466(12) 0.0327(12) 0.0377(11) -0.0051(9) -0.0074(10) 0.0015(9) C27 0.0801(19) 0.0441(15) 0.0447(13) -0.0201(11) -0.0311(13) 0.0157(13) C28 0.0519(14) 0.0392(14) 0.0763(18) -0.0154(13) -0.0118(13) -0.0130(11) C29 0.0669(16) 0.0375(13) 0.0353(11) -0.0031(10) -0.0091(11) -0.0139(12) C30 0.0415(12) 0.0522(14) 0.0312(11) -0.0093(9) -0.0096(9) -0.0067(10) _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 S1 C20 1.7920(18) . ? S1 C2 1.8506(17) . ? O1 C1 1.420(2) . ? C1 C14 1.515(2) . ? C1 C2 1.546(2) . ? C2 C3 1.541(2) . ? C3 C7 1.553(2) . ? C3 C4 1.567(2) . ? C4 C8 1.529(3) . ? C4 C30 1.530(3) . ? C4 C5 1.549(3) . ? C5 C6 1.528(3) . ? C6 C7 1.542(3) . ? C8 C13 1.391(3) . ? C8 C9 1.391(3) . ? C9 C10 1.392(3) . ? C10 C11 1.370(4) . ? C11 C12 1.379(3) . ? C12 C13 1.389(3) . ? C14 C19 1.386(3) . ? C14 C15 1.387(3) . ? C15 C16 1.394(3) . ? C16 C17 1.372(3) . ? C17 C18 1.383(3) . ? C18 C19 1.388(3) . ? C20 C25 1.408(3) . ? C20 C21 1.412(3) . ? C21 C22 1.406(3) . ? C21 C26 1.504(3) . ? C22 C23 1.379(3) . ? C22 C27 1.510(3) . ? C23 C24 1.386(3) . ? C24 C25 1.399(3) . ? C24 C28 1.510(3) . ? C25 C29 1.507(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 S1 C2 102.75(8) . . ? O1 C1 C14 109.61(14) . . ? O1 C1 C2 111.04(14) . . ? C14 C1 C2 115.52(14) . . ? C3 C2 C1 114.40(14) . . ? C3 C2 S1 107.93(11) . . ? C1 C2 S1 107.68(12) . . ? C2 C3 C7 113.41(14) . . ? C2 C3 C4 117.45(15) . . ? C7 C3 C4 103.68(14) . . ? C8 C4 C30 112.39(16) . . ? C8 C4 C5 108.75(15) . . ? C30 C4 C5 109.41(17) . . ? C8 C4 C3 115.47(14) . . ? C30 C4 C3 110.03(15) . . ? C5 C4 C3 99.98(15) . . ? C6 C5 C4 105.55(16) . . ? C5 C6 C7 105.59(16) . . ? C6 C7 C3 106.24(15) . . ? C13 C8 C9 116.94(19) . . ? C13 C8 C4 121.26(17) . . ? C9 C8 C4 121.69(18) . . ? C8 C9 C10 121.3(2) . . ? C11 C10 C9 120.7(2) . . ? C10 C11 C12 119.1(2) . . ? C11 C12 C13 120.2(2) . . ? C12 C13 C8 121.8(2) . . ? C19 C14 C15 118.95(17) . . ? C19 C14 C1 119.27(16) . . ? C15 C14 C1 121.60(17) . . ? C14 C15 C16 119.9(2) . . ? C17 C16 C15 120.5(2) . . ? C16 C17 C18 120.0(2) . . ? C17 C18 C19 119.5(2) . . ? C14 C19 C18 121.0(2) . . ? C25 C20 C21 121.45(17) . . ? C25 C20 S1 118.95(13) . . ? C21 C20 S1 119.53(14) . . ? C22 C21 C20 118.16(18) . . ? C22 C21 C26 119.16(18) . . ? C20 C21 C26 122.68(18) . . ? C23 C22 C21 119.43(18) . . ? C23 C22 C27 119.4(2) . . ? C21 C22 C27 121.2(2) . . ? C22 C23 C24 123.06(18) . . ? C23 C24 C25 118.71(18) . . ? C23 C24 C28 119.5(2) . . ? C25 C24 C28 121.8(2) . . ? C24 C25 C20 119.13(17) . . ? C24 C25 C29 119.22(18) . . ? C20 C25 C29 121.64(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 49.85(19) . . . . ? C14 C1 C2 C3 -75.74(19) . . . . ? O1 C1 C2 S1 -70.11(15) . . . . ? C14 C1 C2 S1 164.30(12) . . . . ? C20 S1 C2 C3 177.97(12) . . . . ? C20 S1 C2 C1 -58.05(13) . . . . ? C1 C2 C3 C7 55.8(2) . . . . ? S1 C2 C3 C7 175.58(13) . . . . ? C1 C2 C3 C4 176.78(14) . . . . ? S1 C2 C3 C4 -63.40(17) . . . . ? C2 C3 C4 C8 76.6(2) . . . . ? C7 C3 C4 C8 -157.40(16) . . . . ? C2 C3 C4 C30 -51.9(2) . . . . ? C7 C3 C4 C30 74.09(19) . . . . ? C2 C3 C4 C5 -166.92(15) . . . . ? C7 C3 C4 C5 -40.95(18) . . . . ? C8 C4 C5 C6 163.00(17) . . . . ? C30 C4 C5 C6 -73.9(2) . . . . ? C3 C4 C5 C6 41.6(2) . . . . ? C4 C5 C6 C7 -26.3(2) . . . . ? C5 C6 C7 C3 -0.2(2) . . . . ? C2 C3 C7 C6 154.59(17) . . . . ? C4 C3 C7 C6 26.1(2) . . . . ? C30 C4 C8 C13 169.36(18) . . . . ? C5 C4 C8 C13 -69.3(2) . . . . ? C3 C4 C8 C13 42.0(2) . . . . ? C30 C4 C8 C9 -14.5(3) . . . . ? C5 C4 C8 C9 106.8(2) . . . . ? C3 C4 C8 C9 -141.85(19) . . . . ? C13 C8 C9 C10 -0.2(3) . . . . ? C4 C8 C9 C10 -176.5(2) . . . . ? C8 C9 C10 C11 0.0(4) . . . . ? C9 C10 C11 C12 -0.1(4) . . . . ? C10 C11 C12 C13 0.4(4) . . . . ? C11 C12 C13 C8 -0.7(3) . . . . ? C9 C8 C13 C12 0.6(3) . . . . ? C4 C8 C13 C12 176.90(17) . . . . ? O1 C1 C14 C19 175.87(15) . . . . ? C2 C1 C14 C19 -57.8(2) . . . . ? O1 C1 C14 C15 0.9(2) . . . . ? C2 C1 C14 C15 127.24(18) . . . . ? C19 C14 C15 C16 0.4(3) . . . . ? C1 C14 C15 C16 175.38(17) . . . . ? C14 C15 C16 C17 0.6(3) . . . . ? C15 C16 C17 C18 -0.6(3) . . . . ? C16 C17 C18 C19 -0.4(3) . . . . ? C15 C14 C19 C18 -1.4(3) . . . . ? C1 C14 C19 C18 -176.50(17) . . . . ? C17 C18 C19 C14 1.4(3) . . . . ? C2 S1 C20 C25 -76.96(15) . . . . ? C2 S1 C20 C21 106.05(14) . . . . ? C25 C20 C21 C22 2.2(3) . . . . ? S1 C20 C21 C22 179.10(12) . . . . ? C25 C20 C21 C26 -178.41(16) . . . . ? S1 C20 C21 C26 -1.5(2) . . . . ? C20 C21 C22 C23 -0.2(3) . . . . ? C26 C21 C22 C23 -179.58(17) . . . . ? C20 C21 C22 C27 178.90(18) . . . . ? C26 C21 C22 C27 -0.5(3) . . . . ? C21 C22 C23 C24 -1.2(3) . . . . ? C27 C22 C23 C24 179.71(19) . . . . ? C22 C23 C24 C25 0.5(3) . . . . ? C22 C23 C24 C28 -178.5(2) . . . . ? C23 C24 C25 C20 1.5(3) . . . . ? C28 C24 C25 C20 -179.47(19) . . . . ? C23 C24 C25 C29 -177.70(19) . . . . ? C28 C24 C25 C29 1.3(3) . . . . ? C21 C20 C25 C24 -2.9(3) . . . . ? S1 C20 C25 C24 -179.81(13) . . . . ? C21 C20 C25 C29 176.30(18) . . . . ? S1 C20 C25 C29 -0.6(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 64.87 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.282 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.047 # = = = END data_kob03 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 O S' _chemical_formula_weight 444.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.6130(10) _cell_length_b 16.0730(10) _cell_length_c 22.7180(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4970.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 40.1 _cell_measurement_theta_max 46.4 _exptl_crystal_description quaderf&ormig _exptl_crystal_colour farblos _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 1.287 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5655 _exptl_absorpt_correction_T_max 0.7829 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method Omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4225 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 65.03 _reflns_number_total 4225 _reflns_number_gt 3531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 (Harms, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0698P)^2^+1.6183P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00066(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4225 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.152 _refine_ls_shift/su_mean 0.008 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 S1 S 0.34816(3) 0.22900(3) 0.740818(18) 0.02749(16) Uani 1 1 d . . . O1 O 0.17715(11) 0.21965(8) 0.81338(6) 0.0342(3) Uani 1 1 d . . . H1A H 0.135(2) 0.2241(18) 0.8423(14) 0.070(9) Uiso 1 1 d . . . C1 C 0.17323(14) 0.29191(11) 0.77702(8) 0.0274(4) Uani 1 1 d . . . H1 H 0.1007(15) 0.3053(13) 0.7655(8) 0.027(5) Uiso 1 1 d . . . C2 C 0.22797(13) 0.27190(11) 0.71938(8) 0.0256(4) Uani 1 1 d . . . H2 H 0.2464(15) 0.3239(13) 0.6995(9) 0.033(5) Uiso 1 1 d . . . C3 C 0.17321(14) 0.21598(12) 0.67538(8) 0.0283(4) Uani 1 1 d . . . H3 H 0.2234(14) 0.1879(12) 0.6534(8) 0.026(5) Uiso 1 1 d . . . C4 C 0.11357(14) 0.26333(12) 0.62655(8) 0.0332(4) Uani 1 1 d . . . C5 C 0.0475(2) 0.19253(18) 0.60163(14) 0.0587(8) Uani 1 1 d . . . H5A H -0.006(3) 0.209(2) 0.5860(18) 0.115(14) Uiso 1 1 d . . . H5B H 0.071(3) 0.174(3) 0.5667(19) 0.118(15) Uiso 1 1 d . . . C6 C 0.0450(3) 0.12317(18) 0.64544(12) 0.0646(9) Uani 1 1 d . . . H6A H -0.007(3) 0.095(2) 0.6511(15) 0.099(12) Uiso 1 1 d . . . H6B H 0.087(3) 0.083(3) 0.6239(19) 0.135(17) Uiso 1 1 d . . . C7 C 0.10117(17) 0.15136(14) 0.69954(10) 0.0380(5) Uani 1 1 d . . . H7A H 0.1368(18) 0.1062(17) 0.7175(11) 0.055(7) Uiso 1 1 d . . . H7B H 0.055(2) 0.1749(16) 0.7287(11) 0.056(7) Uiso 1 1 d . . . C8 C 0.18232(14) 0.29892(13) 0.58002(8) 0.0331(4) Uani 1 1 d . . . C9 C 0.23769(19) 0.24690(19) 0.54357(10) 0.0521(6) Uani 1 1 d . . . H9 H 0.230(2) 0.185(2) 0.5484(12) 0.080(10) Uiso 1 1 d . . . C10 C 0.2985(2) 0.2777(2) 0.50024(11) 0.0695(9) Uani 1 1 d . . . H10 H 0.337(3) 0.243(2) 0.4752(16) 0.096(11) Uiso 1 1 d . . . C11 C 0.3077(2) 0.3617(3) 0.49204(12) 0.0754(10) Uani 1 1 d . . . H11 H 0.351(2) 0.3853(19) 0.4596(13) 0.082(9) Uiso 1 1 d . . . C12 C 0.2568(2) 0.4149(2) 0.52774(13) 0.0659(8) Uani 1 1 d . . . H12 H 0.260(2) 0.4737(19) 0.5226(13) 0.079(9) Uiso 1 1 d . . . C13 C 0.19459(17) 0.38412(15) 0.57171(10) 0.0452(5) Uani 1 1 d . . . H13 H 0.1591(17) 0.4221(14) 0.5955(10) 0.044(6) Uiso 1 1 d . . . C14 C 0.21482(13) 0.36790(11) 0.80804(8) 0.0292(4) Uani 1 1 d . . . C15 C 0.19602(16) 0.44701(12) 0.78518(9) 0.0368(5) Uani 1 1 d . . . H15 H 0.1569(17) 0.4495(15) 0.7495(10) 0.041(6) Uiso 1 1 d . . . C16 C 0.23126(17) 0.51795(13) 0.81272(10) 0.0432(5) Uani 1 1 d . . . H16 H 0.2167(18) 0.5748(16) 0.7948(11) 0.055(7) Uiso 1 1 d . . . C17 C 0.28508(18) 0.51088(15) 0.86379(11) 0.0470(6) Uani 1 1 d . . . H17 H 0.304(2) 0.5597(16) 0.8844(12) 0.061(7) Uiso 1 1 d . . . C18 C 0.30415(18) 0.43304(15) 0.88690(11) 0.0495(6) Uani 1 1 d . . . H18 H 0.3407(17) 0.4275(15) 0.9252(11) 0.051(7) Uiso 1 1 d . . . C19 C 0.26940(16) 0.36213(14) 0.85894(9) 0.0398(5) Uani 1 1 d . . . H19 H 0.2811(17) 0.3086(15) 0.8749(10) 0.045(6) Uiso 1 1 d . . . C20 C 0.41356(13) 0.23845(11) 0.67291(8) 0.0265(4) Uani 1 1 d . . . C21 C 0.44470(13) 0.31758(11) 0.65309(8) 0.0291(4) Uani 1 1 d . . . C22 C 0.49719(14) 0.32229(12) 0.60015(9) 0.0337(4) Uani 1 1 d . . . C23 C 0.51613(15) 0.24983(14) 0.56900(9) 0.0367(5) Uani 1 1 d . . . H23 H 0.5530(18) 0.2538(14) 0.5322(11) 0.044(6) Uiso 1 1 d . . . C24 C 0.48473(15) 0.17202(12) 0.58758(8) 0.0341(5) Uani 1 1 d . . . C25 C 0.43423(14) 0.16557(12) 0.64092(8) 0.0300(4) Uani 1 1 d . . . C26 C 0.42319(17) 0.39593(13) 0.68700(10) 0.0366(5) Uani 1 1 d . . . H26A H 0.369(2) 0.4310(16) 0.6689(12) 0.061(8) Uiso 1 1 d . . . H26B H 0.4015(17) 0.3849(14) 0.7264(11) 0.042(6) Uiso 1 1 d . . . H26C H 0.4811(19) 0.4298(15) 0.6908(10) 0.049(7) Uiso 1 1 d . . . C27 C 0.5310(2) 0.40492(15) 0.57589(11) 0.0456(5) Uani 1 1 d . . . H27B H 0.475(2) 0.4412(18) 0.5670(12) 0.068(8) Uiso 1 1 d . . . H27C H 0.566(2) 0.3974(17) 0.5377(12) 0.065(8) Uiso 1 1 d . . . H27A H 0.572(2) 0.4368(16) 0.6058(12) 0.062(8) Uiso 1 1 d . . . C28 C 0.5010(2) 0.09761(17) 0.54825(11) 0.0501(6) Uani 1 1 d . . . H28C H 0.543(2) 0.1109(18) 0.5120(14) 0.081(9) Uiso 1 1 d . . . H28A H 0.533(2) 0.053(2) 0.5682(15) 0.088(10) Uiso 1 1 d . . . H28B H 0.441(2) 0.0784(19) 0.5315(14) 0.080(10) Uiso 1 1 d . . . C29 C 0.4039(2) 0.08102(14) 0.66309(12) 0.0489(6) Uani 1 1 d . . . H29A H 0.393(3) 0.076(2) 0.7044(18) 0.109(12) Uiso 1 1 d . . . H29B H 0.449(2) 0.041(2) 0.6545(15) 0.089(11) Uiso 1 1 d . . . H29C H 0.353(3) 0.062(2) 0.6368(16) 0.100(12) Uiso 1 1 d . . . C30 C 0.04675(18) 0.33057(17) 0.65246(11) 0.0467(6) Uani 1 1 d . . . H30B H 0.083(2) 0.3759(18) 0.6735(12) 0.064(8) Uiso 1 1 d . . . H30C H 0.0098(19) 0.3556(15) 0.6203(11) 0.056(7) Uiso 1 1 d . . . H30A H -0.001(2) 0.3072(19) 0.6831(13) 0.075(9) Uiso 1 1 d . . . 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 S1 0.0285(3) 0.0315(3) 0.0225(3) 0.00131(17) -0.00014(17) 0.00225(18) O1 0.0437(8) 0.0293(7) 0.0296(7) 0.0055(6) 0.0102(6) 0.0012(6) C1 0.0305(10) 0.0253(9) 0.0265(9) 0.0021(7) 0.0022(8) 0.0015(8) C2 0.0271(10) 0.0257(9) 0.0241(9) 0.0027(7) 0.0005(7) 0.0005(7) C3 0.0296(9) 0.0288(10) 0.0266(9) 0.0015(8) -0.0020(8) 0.0005(8) C4 0.0316(10) 0.0374(11) 0.0305(10) 0.0027(8) -0.0060(8) -0.0024(8) C5 0.0636(17) 0.0548(16) 0.0578(17) 0.0101(13) -0.0309(14) -0.0251(14) C6 0.094(2) 0.0514(16) 0.0479(15) 0.0044(12) -0.0215(15) -0.0357(17) C7 0.0425(12) 0.0325(11) 0.0390(11) 0.0035(9) -0.0042(10) -0.0081(10) C8 0.0335(10) 0.0449(11) 0.0211(9) 0.0007(8) -0.0071(8) 0.0019(9) C9 0.0562(15) 0.0699(17) 0.0301(11) -0.0082(11) -0.0058(11) 0.0146(13) C10 0.0595(17) 0.120(3) 0.0288(12) 0.0003(16) 0.0032(12) 0.0291(18) C11 0.0472(15) 0.136(3) 0.0433(15) 0.0354(18) 0.0052(12) 0.0143(18) C12 0.0523(15) 0.077(2) 0.0684(18) 0.0379(16) -0.0013(14) -0.0042(14) C13 0.0441(12) 0.0487(13) 0.0429(12) 0.0102(11) 0.0010(10) 0.0011(11) C14 0.0311(10) 0.0305(10) 0.0261(9) -0.0025(7) 0.0059(7) 0.0023(8) C15 0.0462(12) 0.0318(11) 0.0325(11) 0.0010(8) -0.0009(9) 0.0011(9) C16 0.0537(14) 0.0292(11) 0.0469(12) -0.0027(9) 0.0048(10) -0.0003(10) C17 0.0479(13) 0.0393(12) 0.0539(14) -0.0150(11) -0.0009(11) -0.0020(10) C18 0.0527(14) 0.0493(14) 0.0466(13) -0.0127(11) -0.0148(11) 0.0063(11) C19 0.0472(13) 0.0353(11) 0.0370(11) -0.0034(9) -0.0073(9) 0.0068(10) C20 0.0252(9) 0.0295(10) 0.0248(9) -0.0002(7) -0.0015(7) 0.0014(7) C21 0.0276(9) 0.0295(10) 0.0302(9) 0.0019(8) -0.0036(8) -0.0011(8) C22 0.0311(10) 0.0386(11) 0.0314(10) 0.0049(8) -0.0024(8) -0.0030(8) C23 0.0336(10) 0.0516(13) 0.0247(10) 0.0026(9) 0.0021(8) 0.0025(9) C24 0.0335(10) 0.0402(11) 0.0285(10) -0.0043(8) -0.0004(8) 0.0066(9) C25 0.0307(10) 0.0282(10) 0.0311(10) -0.0016(8) -0.0025(8) 0.0014(8) C26 0.0372(11) 0.0291(10) 0.0436(12) -0.0020(9) 0.0025(10) -0.0036(9) C27 0.0504(14) 0.0453(13) 0.0412(13) 0.0123(11) 0.0035(11) -0.0092(11) C28 0.0596(16) 0.0512(14) 0.0393(13) -0.0126(11) 0.0043(12) 0.0114(13) C29 0.0671(17) 0.0278(12) 0.0517(15) -0.0018(10) 0.0157(14) -0.0020(11) C30 0.0372(12) 0.0584(15) 0.0444(13) 0.0152(12) 0.0048(11) 0.0147(11) _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 S1 C20 1.7877(18) . ? S1 C2 1.8411(18) . ? O1 C1 1.426(2) . ? C1 C14 1.520(3) . ? C1 C2 1.541(2) . ? C2 C3 1.537(2) . ? C3 C7 1.530(3) . ? C3 C4 1.571(3) . ? C4 C8 1.523(3) . ? C4 C30 1.530(3) . ? C4 C5 1.557(3) . ? C5 C6 1.495(4) . ? C6 C7 1.517(3) . ? C8 C13 1.392(3) . ? C8 C9 1.397(3) . ? C9 C10 1.378(4) . ? C10 C11 1.369(5) . ? C11 C12 1.367(5) . ? C12 C13 1.400(3) . ? C14 C19 1.378(3) . ? C14 C15 1.397(3) . ? C15 C16 1.386(3) . ? C16 C17 1.377(3) . ? C17 C18 1.382(3) . ? C18 C19 1.388(3) . ? C20 C25 1.407(3) . ? C20 C21 1.414(3) . ? C21 C22 1.401(3) . ? C21 C26 1.505(3) . ? C22 C23 1.387(3) . ? C22 C27 1.510(3) . ? C23 C24 1.387(3) . ? C24 C25 1.397(3) . ? C24 C28 1.509(3) . ? C25 C29 1.507(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 S1 C2 100.51(8) . . ? O1 C1 C14 111.84(15) . . ? O1 C1 C2 107.71(14) . . ? C14 C1 C2 112.44(15) . . ? C3 C2 C1 116.12(15) . . ? C3 C2 S1 112.58(12) . . ? C1 C2 S1 106.45(12) . . ? C7 C3 C2 118.32(16) . . ? C7 C3 C4 104.53(16) . . ? C2 C3 C4 115.24(15) . . ? C8 C4 C30 111.52(18) . . ? C8 C4 C5 112.15(19) . . ? C30 C4 C5 108.2(2) . . ? C8 C4 C3 110.75(15) . . ? C30 C4 C3 112.20(17) . . ? C5 C4 C3 101.61(17) . . ? C6 C5 C4 108.4(2) . . ? C5 C6 C7 107.8(2) . . ? C6 C7 C3 103.59(19) . . ? C13 C8 C9 116.3(2) . . ? C13 C8 C4 122.49(19) . . ? C9 C8 C4 121.2(2) . . ? C10 C9 C8 122.1(3) . . ? C11 C10 C9 120.5(3) . . ? C12 C11 C10 119.3(3) . . ? C11 C12 C13 120.6(3) . . ? C8 C13 C12 121.1(3) . . ? C19 C14 C15 118.17(18) . . ? C19 C14 C1 122.42(17) . . ? C15 C14 C1 119.39(17) . . ? C16 C15 C14 121.2(2) . . ? C17 C16 C15 119.8(2) . . ? C16 C17 C18 119.7(2) . . ? C17 C18 C19 120.4(2) . . ? C14 C19 C18 120.8(2) . . ? C25 C20 C21 121.63(17) . . ? C25 C20 S1 118.33(14) . . ? C21 C20 S1 120.03(14) . . ? C22 C21 C20 118.34(17) . . ? C22 C21 C26 119.57(17) . . ? C20 C21 C26 122.09(17) . . ? C23 C22 C21 119.18(18) . . ? C23 C22 C27 119.72(19) . . ? C21 C22 C27 121.09(19) . . ? C22 C23 C24 122.98(18) . . ? C23 C24 C25 118.84(18) . . ? C23 C24 C28 119.29(19) . . ? C25 C24 C28 121.8(2) . . ? C24 C25 C20 118.99(17) . . ? C24 C25 C29 119.45(18) . . ? C20 C25 C29 121.55(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 75.42(19) . . . . ? C14 C1 C2 C3 -160.92(15) . . . . ? O1 C1 C2 S1 -50.78(16) . . . . ? C14 C1 C2 S1 72.88(16) . . . . ? C20 S1 C2 C3 68.01(14) . . . . ? C20 S1 C2 C1 -163.69(12) . . . . ? C1 C2 C3 C7 -30.4(2) . . . . ? S1 C2 C3 C7 92.69(19) . . . . ? C1 C2 C3 C4 94.33(19) . . . . ? S1 C2 C3 C4 -142.62(14) . . . . ? C7 C3 C4 C8 -153.29(17) . . . . ? C2 C3 C4 C8 75.1(2) . . . . ? C7 C3 C4 C30 81.4(2) . . . . ? C2 C3 C4 C30 -50.2(2) . . . . ? C7 C3 C4 C5 -34.0(2) . . . . ? C2 C3 C4 C5 -165.6(2) . . . . ? C8 C4 C5 C6 136.4(3) . . . . ? C30 C4 C5 C6 -100.1(3) . . . . ? C3 C4 C5 C6 18.1(3) . . . . ? C4 C5 C6 C7 4.5(4) . . . . ? C5 C6 C7 C3 -26.1(3) . . . . ? C2 C3 C7 C6 167.3(2) . . . . ? C4 C3 C7 C6 37.5(2) . . . . ? C30 C4 C8 C13 11.8(3) . . . . ? C5 C4 C8 C13 133.3(2) . . . . ? C3 C4 C8 C13 -113.9(2) . . . . ? C30 C4 C8 C9 -168.9(2) . . . . ? C5 C4 C8 C9 -47.4(3) . . . . ? C3 C4 C8 C9 65.3(2) . . . . ? C13 C8 C9 C10 -2.3(3) . . . . ? C4 C8 C9 C10 178.4(2) . . . . ? C8 C9 C10 C11 1.0(4) . . . . ? C9 C10 C11 C12 0.7(4) . . . . ? C10 C11 C12 C13 -1.0(4) . . . . ? C9 C8 C13 C12 2.0(3) . . . . ? C4 C8 C13 C12 -178.7(2) . . . . ? C11 C12 C13 C8 -0.4(4) . . . . ? O1 C1 C14 C19 13.9(3) . . . . ? C2 C1 C14 C19 -107.4(2) . . . . ? O1 C1 C14 C15 -164.87(17) . . . . ? C2 C1 C14 C15 73.8(2) . . . . ? C19 C14 C15 C16 0.1(3) . . . . ? C1 C14 C15 C16 178.92(19) . . . . ? C14 C15 C16 C17 -0.6(3) . . . . ? C15 C16 C17 C18 0.5(4) . . . . ? C16 C17 C18 C19 0.0(4) . . . . ? C15 C14 C19 C18 0.4(3) . . . . ? C1 C14 C19 C18 -178.4(2) . . . . ? C17 C18 C19 C14 -0.5(4) . . . . ? C2 S1 C20 C25 -107.92(15) . . . . ? C2 S1 C20 C21 73.20(16) . . . . ? C25 C20 C21 C22 0.1(3) . . . . ? S1 C20 C21 C22 178.95(14) . . . . ? C25 C20 C21 C26 -179.88(18) . . . . ? S1 C20 C21 C26 -1.0(3) . . . . ? C20 C21 C22 C23 0.4(3) . . . . ? C26 C21 C22 C23 -179.59(18) . . . . ? C20 C21 C22 C27 178.87(19) . . . . ? C26 C21 C22 C27 -1.1(3) . . . . ? C21 C22 C23 C24 0.5(3) . . . . ? C27 C22 C23 C24 -177.9(2) . . . . ? C22 C23 C24 C25 -2.0(3) . . . . ? C22 C23 C24 C28 174.7(2) . . . . ? C23 C24 C25 C20 2.4(3) . . . . ? C28 C24 C25 C20 -174.1(2) . . . . ? C23 C24 C25 C29 -177.1(2) . . . . ? C28 C24 C25 C29 6.3(3) . . . . ? C21 C20 C25 C24 -1.5(3) . . . . ? S1 C20 C25 C24 179.59(14) . . . . ? C21 C20 C25 C29 178.0(2) . . . . ? S1 C20 C25 C29 -0.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 65.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.358 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.054 # = = = END