#------------------------------------------------------------------------------ #$Date: 2021-12-03 03:36:38 +0200 (Fri, 03 Dec 2021) $ #$Revision: 270996 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/84/7158427.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7158427 loop_ _publ_author_name 'Sartucci, Jenna L.' 'Maity, Arindam' 'Mohanan, Manikandan' 'Bertke, Jeffery A.' 'Kertesz, Miklos' 'Gavvalapalli, Nagarjuna' _publ_section_title ; Molecular Tetrominoes: Selective Masking of Donor pi-face to Control Configuration of Donor-Acceptor Complex ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D1OB02293H _journal_year 2021 _chemical_absolute_configuration unk _chemical_formula_moiety 'C36 H34 S2' _chemical_formula_sum 'C36 H34 S2' _chemical_formula_weight 530.75 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary intrinsic _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-05-25 deposited with the CCDC. 2021-11-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.8779(6) _cell_length_b 14.0953(7) _cell_length_c 16.4691(7) _cell_measurement_reflns_used 9821 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.30 _cell_measurement_theta_min 2.24 _cell_volume 2757.3(2) _computing_cell_refinement 'SAINT V8.37A (Bruker, 2005)' _computing_data_collection 'APEX3 V2016.5-0 (Bruker, 2016)' _computing_data_reduction ; SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) ; _computing_molecular_graphics 'SHELXLE v932 (Hubschle, 2011)' _computing_publication_material 'XCIF V2014-2 (Bruker, 2014)' _computing_structure_refinement 'SHELX-2018-3 (Sheldrick, 2015)' _computing_structure_solution 'SHELX-2014-5 (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'Bruker D8 Quest/Photon 100' _diffrn_measurement_method 'profile data from \f and \w scans' _diffrn_radiation_monochromator 'multilayer mirrors' _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_unetI/netI 0.0096 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 172579 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.360 _diffrn_reflns_theta_min 1.902 _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_T_max 0.96301 _exptl_absorpt_correction_T_min 0.95117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2016/2 (Bruker, 2016)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1128 _exptl_crystal_size_max 0.331 _exptl_crystal_size_mid 0.322 _exptl_crystal_size_min 0.299 _refine_diff_density_max 0.493 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.050 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.45(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 344 _refine_ls_number_reflns 6860 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.108 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0335 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+1.2658P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0900 _refine_ls_wR_factor_ref 0.0901 _reflns_Friedel_coverage 0.792 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 6798 _reflns_number_total 6860 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ob02293h3.cif _cod_data_source_block B19227_a _cod_database_code 7158427 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.931 _shelx_estimated_absorpt_t_max 0.938 _shelx_res_file ; TITL B19227_a.res in P2(1)2(1)2(1) B19227_a.res created by SHELXL-2018/3 at 08:30:16 on 06-Jun-2019 REM Old TITL B19227 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.119, Rweak 0.033, Alpha 0.002, Orientation as input REM Flack x = 0.464 ( 0.005 ) from Parsons' quotients REM Formula found by SHELXT: C36 S2 CELL 0.71073 11.8779 14.0953 16.4691 90.000 90.000 90.000 ZERR 4.000 0.0006 0.0007 0.0007 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H S UNIT 144 136 8 TEMP -173.150 SIZE 0.299 0.322 0.331 L.S. 20 BOND $H ACTA CONF LIST 4 FMAP 2 PLAN 20 OMIT 1 3 1 OMIT 1 3 0 OMIT 2 1 2 OMIT -2 1 1 OMIT 1 0 1 OMIT 1 0 2 OMIT 2 0 3 OMIT 1 4 0 OMIT 0 0 12 TWIN WGHT 0.046100 1.265800 BASF 0.45480 FVAR 0.38194 S1 3 0.325602 0.662405 0.807419 11.00000 0.02129 0.01741 = 0.01705 -0.00120 0.00035 0.00283 S2 3 0.365440 0.564658 0.425044 11.00000 0.02744 0.02377 = 0.01744 -0.00170 0.00139 0.00078 C1 1 0.399330 0.548400 0.808929 11.00000 0.02198 0.01814 = 0.01694 0.00004 -0.00225 0.00098 AFIX 23 H1A 2 0.478857 0.558617 0.824655 11.00000 -1.20000 H1B 2 0.364284 0.506459 0.849991 11.00000 -1.20000 AFIX 0 C2 1 0.394879 0.501129 0.727177 11.00000 0.02349 0.01364 = 0.01856 0.00015 -0.00244 0.00177 C3 1 0.488884 0.500108 0.674836 11.00000 0.01853 0.01456 = 0.02190 -0.00113 -0.00437 0.00285 C4 1 0.473889 0.474275 0.593585 11.00000 0.01894 0.01890 = 0.02099 -0.00314 -0.00107 0.00407 AFIX 43 H4 2 0.537499 0.471990 0.558672 11.00000 -1.20000 AFIX 0 C5 1 0.367863 0.451738 0.562391 11.00000 0.02272 0.01386 = 0.01781 -0.00241 -0.00276 0.00218 C6 1 0.276919 0.444876 0.616099 11.00000 0.02119 0.01320 = 0.02320 -0.00253 -0.00206 -0.00061 C7 1 0.292683 0.468372 0.698235 11.00000 0.02008 0.01568 = 0.02097 0.00074 0.00051 0.00037 AFIX 43 H7 2 0.231470 0.461575 0.734903 11.00000 -1.20000 AFIX 0 C8 1 0.352130 0.446949 0.472049 11.00000 0.02699 0.01960 = 0.01843 -0.00351 -0.00293 -0.00013 AFIX 23 H8A 2 0.276755 0.420590 0.459827 11.00000 -1.20000 H8B 2 0.409176 0.403773 0.448484 11.00000 -1.20000 AFIX 0 C9 1 0.598846 0.535919 0.700952 11.00000 0.02702 0.01631 = 0.01538 -0.00095 0.00039 0.00524 C10 1 0.684959 0.569448 0.719980 11.00000 0.02488 0.02425 = 0.01867 0.00116 0.00152 0.00712 C11 1 0.789993 0.613784 0.742092 11.00000 0.02243 0.02401 = 0.01441 -0.00035 0.00018 -0.00061 C12 1 0.883077 0.559213 0.765030 11.00000 0.02426 0.02241 = 0.02261 0.00141 -0.00098 -0.00124 AFIX 43 H12 2 0.876752 0.492078 0.767300 11.00000 -1.20000 AFIX 0 C13 1 0.984439 0.602271 0.784469 11.00000 0.02109 0.03158 = 0.02511 -0.00030 -0.00203 0.00103 AFIX 43 H13 2 1.047768 0.564572 0.798620 11.00000 -1.20000 AFIX 0 C14 1 0.993489 0.700240 0.783284 11.00000 0.02228 0.03522 = 0.02698 -0.00406 0.00335 -0.00996 AFIX 43 H14 2 1.062487 0.729705 0.797951 11.00000 -1.20000 AFIX 0 C15 1 0.902517 0.755065 0.760850 11.00000 0.03799 0.02121 = 0.02711 -0.00124 0.00402 -0.00717 AFIX 43 H15 2 0.909598 0.822176 0.759364 11.00000 -1.20000 AFIX 0 C16 1 0.800382 0.712939 0.740358 11.00000 0.02707 0.02365 = 0.02386 0.00061 0.00235 0.00262 AFIX 43 H16 2 0.737942 0.751181 0.725254 11.00000 -1.20000 AFIX 0 C17 1 0.165453 0.419336 0.587857 11.00000 0.02608 0.01620 = 0.02170 -0.00151 0.00145 -0.00046 C18 1 0.074404 0.397499 0.565623 11.00000 0.02639 0.01890 = 0.02100 0.00048 -0.00081 0.00114 C19 1 -0.035986 0.368190 0.539733 11.00000 0.02101 0.01646 = 0.02106 0.00295 -0.00204 -0.00088 C20 1 -0.130530 0.385740 0.588284 11.00000 0.02739 0.02708 = 0.02348 0.00328 0.00238 0.00498 AFIX 43 H20 2 -0.122013 0.417480 0.638799 11.00000 -1.20000 AFIX 0 C21 1 -0.236282 0.357058 0.563005 11.00000 0.02111 0.02547 = 0.04753 0.01419 0.00837 0.00258 AFIX 43 H21 2 -0.299936 0.368573 0.596512 11.00000 -1.20000 AFIX 0 C22 1 -0.249689 0.311815 0.489360 11.00000 0.02061 0.02090 = 0.05678 0.00859 -0.01040 -0.00692 AFIX 43 H22 2 -0.322525 0.292532 0.472168 11.00000 -1.20000 AFIX 0 C23 1 -0.156857 0.294429 0.440337 11.00000 0.03552 0.01846 = 0.03413 -0.00147 -0.01188 -0.00432 AFIX 43 H23 2 -0.166661 0.264307 0.389222 11.00000 -1.20000 AFIX 0 C24 1 -0.050172 0.320690 0.465454 11.00000 0.02452 0.02017 = 0.02078 0.00190 0.00017 -0.00268 AFIX 43 H24 2 0.013354 0.306630 0.432538 11.00000 -1.20000 AFIX 0 C25 1 0.412892 0.734982 0.740277 11.00000 0.01818 0.01665 = 0.02088 -0.00360 -0.00128 -0.00060 AFIX 23 H25A 2 0.437330 0.791883 0.770793 11.00000 -1.20000 H25B 2 0.481372 0.698324 0.726498 11.00000 -1.20000 AFIX 0 C26 1 0.357590 0.768107 0.660425 11.00000 0.01525 0.01239 = 0.02011 -0.00132 0.00005 -0.00058 C27 1 0.439674 0.835336 0.617127 11.00000 0.02270 0.02003 = 0.02632 -0.00044 0.00216 -0.00717 AFIX 23 H27A 2 0.511013 0.801605 0.605601 11.00000 -1.20000 H27B 2 0.456818 0.890041 0.652743 11.00000 -1.20000 AFIX 0 C28 1 0.387470 0.870983 0.536927 11.00000 0.03493 0.01930 = 0.02960 0.00544 0.00356 -0.00775 AFIX 13 H28 2 0.441549 0.914652 0.509200 11.00000 -1.20000 AFIX 0 C29 1 0.361532 0.786195 0.481008 11.00000 0.02981 0.02432 = 0.02073 0.00444 0.00269 -0.00437 AFIX 23 H29A 2 0.327827 0.809296 0.429708 11.00000 -1.20000 H29B 2 0.432245 0.752449 0.467652 11.00000 -1.20000 AFIX 0 C30 1 0.279814 0.717909 0.523043 11.00000 0.02027 0.01712 = 0.01921 0.00000 -0.00213 0.00017 C31 1 0.332375 0.684700 0.603403 11.00000 0.01606 0.01457 = 0.01752 -0.00015 -0.00161 -0.00069 AFIX 23 H31A 2 0.280125 0.640241 0.630707 11.00000 -1.20000 H31B 2 0.403121 0.650106 0.591848 11.00000 -1.20000 AFIX 0 C32 1 0.247868 0.822392 0.677725 11.00000 0.02036 0.01792 = 0.02424 -0.00081 -0.00065 0.00465 AFIX 23 H32A 2 0.263810 0.877268 0.713439 11.00000 -1.20000 H32B 2 0.193998 0.780268 0.706084 11.00000 -1.20000 AFIX 0 C33 1 0.195744 0.857334 0.597513 11.00000 0.02538 0.02158 = 0.02839 0.00043 -0.00485 0.00975 AFIX 13 H33 2 0.124146 0.892017 0.609313 11.00000 -1.20000 AFIX 0 C34 1 0.278222 0.924313 0.555404 11.00000 0.04758 0.01680 = 0.03175 0.00481 -0.00570 0.00263 AFIX 23 H34A 2 0.294270 0.979309 0.590959 11.00000 -1.20000 H34B 2 0.244742 0.948247 0.504307 11.00000 -1.20000 AFIX 0 C35 1 0.170564 0.772197 0.543019 11.00000 0.02005 0.02441 = 0.02620 0.00003 -0.00571 0.00529 AFIX 23 H35A 2 0.134963 0.794280 0.492057 11.00000 -1.20000 H35B 2 0.117110 0.729201 0.570824 11.00000 -1.20000 AFIX 0 C36 1 0.248977 0.633402 0.467916 11.00000 0.02174 0.02177 = 0.02154 -0.00143 -0.00416 -0.00017 AFIX 23 H36A 2 0.202919 0.657791 0.422371 11.00000 -1.20000 H36B 2 0.200852 0.589577 0.499569 11.00000 -1.20000 AFIX 0 HKLF 4 REM B19227_a.res in P2(1)2(1)2(1) REM wR2 = 0.090145, GooF = S = 1.10844, Restrained GooF = 1.10844 for all data REM R1 = 0.033467 for 6798 Fo > 4sig(Fo) and 0.033743 for all 6860 data REM 344 parameters refined using 0 restraints END WGHT 0.0461 1.2658 REM Highest difference peak 0.493, deepest hole -0.256, 1-sigma level 0.050 Q1 1 0.3997 0.6816 0.7889 11.00000 0.05 0.49 Q2 1 0.2600 0.6591 0.7982 11.00000 0.05 0.47 Q3 1 0.4281 0.5622 0.4366 11.00000 0.05 0.43 Q4 1 -0.1717 0.3450 0.5755 11.00000 0.05 0.37 Q5 1 -0.2362 0.3352 0.4391 11.00000 0.05 0.35 Q6 1 0.2911 0.5505 0.4224 11.00000 0.05 0.34 Q7 1 0.3437 0.9184 0.5533 11.00000 0.05 0.33 Q8 1 0.4394 0.4760 0.6960 11.00000 0.05 0.33 Q9 1 0.4197 0.4479 0.5875 11.00000 0.05 0.29 Q10 1 0.3345 0.4923 0.7117 11.00000 0.05 0.28 Q11 1 0.6518 0.5238 0.6974 11.00000 0.05 0.28 Q12 1 0.1182 0.5132 0.6943 11.00000 0.05 0.28 Q13 1 -0.1012 0.3034 0.4526 11.00000 0.05 0.26 Q14 1 0.2188 0.4408 0.5868 11.00000 0.05 0.26 Q15 1 -0.3596 0.3850 0.5564 11.00000 0.05 0.26 Q16 1 0.9510 0.7215 0.7450 11.00000 0.05 0.26 Q17 1 1.0310 0.5439 0.7150 11.00000 0.05 0.25 Q18 1 0.7239 0.6179 0.7078 11.00000 0.05 0.24 Q19 1 0.5539 0.4116 0.5723 11.00000 0.05 0.23 Q20 1 0.3435 0.7252 0.6350 11.00000 0.05 0.23 ; _shelx_res_checksum 75558 loop_ _space_group_symop_operation_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' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.32560(4) 0.66240(4) 0.80742(3) 0.01859(11) Uani 1 1 d . . . . . S2 S 0.36544(5) 0.56466(4) 0.42504(3) 0.02288(13) Uani 1 1 d . . . . . C1 C 0.39933(18) 0.54840(15) 0.80893(13) 0.0190(4) Uani 1 1 d . . . . . H1A H 0.478857 0.558617 0.824655 0.023 Uiso 1 1 calc R U . . . H1B H 0.364284 0.506459 0.849991 0.023 Uiso 1 1 calc R U . . . C2 C 0.39488(19) 0.50113(15) 0.72718(13) 0.0186(4) Uani 1 1 d . . . . . C3 C 0.48888(18) 0.50011(15) 0.67484(13) 0.0183(4) Uani 1 1 d . . . . . C4 C 0.47389(19) 0.47427(15) 0.59358(13) 0.0196(4) Uani 1 1 d . . . . . H4 H 0.537499 0.471990 0.558672 0.024 Uiso 1 1 calc R U . . . C5 C 0.36786(19) 0.45174(14) 0.56239(13) 0.0181(4) Uani 1 1 d . . . . . C6 C 0.27692(19) 0.44488(15) 0.61610(14) 0.0192(4) Uani 1 1 d . . . . . C7 C 0.29268(18) 0.46837(15) 0.69823(14) 0.0189(4) Uani 1 1 d . . . . . H7 H 0.231470 0.461575 0.734903 0.023 Uiso 1 1 calc R U . . . C8 C 0.3521(2) 0.44695(16) 0.47205(13) 0.0217(4) Uani 1 1 d . . . . . H8A H 0.276755 0.420590 0.459827 0.026 Uiso 1 1 calc R U . . . H8B H 0.409176 0.403773 0.448484 0.026 Uiso 1 1 calc R U . . . C9 C 0.59885(19) 0.53592(15) 0.70095(13) 0.0196(4) Uani 1 1 d . . . . . C10 C 0.6850(2) 0.56945(17) 0.71998(13) 0.0226(4) Uani 1 1 d . . . . . C11 C 0.7900(2) 0.61378(17) 0.74209(13) 0.0203(4) Uani 1 1 d . . . . . C12 C 0.8831(2) 0.55921(17) 0.76503(14) 0.0231(4) Uani 1 1 d . . . . . H12 H 0.876752 0.492078 0.767300 0.028 Uiso 1 1 calc R U . . . C13 C 0.9844(2) 0.60227(19) 0.78447(15) 0.0259(5) Uani 1 1 d . . . . . H13 H 1.047768 0.564572 0.798620 0.031 Uiso 1 1 calc R U . . . C14 C 0.9935(2) 0.70024(19) 0.78328(15) 0.0282(5) Uani 1 1 d . . . . . H14 H 1.062487 0.729705 0.797951 0.034 Uiso 1 1 calc R U . . . C15 C 0.9025(2) 0.75506(18) 0.76085(15) 0.0288(5) Uani 1 1 d . . . . . H15 H 0.909598 0.822176 0.759364 0.035 Uiso 1 1 calc R U . . . C16 C 0.8004(2) 0.71294(17) 0.74036(14) 0.0249(5) Uani 1 1 d . . . . . H16 H 0.737942 0.751181 0.725254 0.030 Uiso 1 1 calc R U . . . C17 C 0.1655(2) 0.41934(15) 0.58786(13) 0.0213(4) Uani 1 1 d . . . . . C18 C 0.0744(2) 0.39750(16) 0.56562(14) 0.0221(4) Uani 1 1 d . . . . . C19 C -0.03599(19) 0.36819(15) 0.53973(14) 0.0195(4) Uani 1 1 d . . . . . C20 C -0.1305(2) 0.38574(18) 0.58828(15) 0.0260(5) Uani 1 1 d . . . . . H20 H -0.122013 0.417480 0.638799 0.031 Uiso 1 1 calc R U . . . C21 C -0.2363(2) 0.35706(18) 0.56301(19) 0.0314(6) Uani 1 1 d . . . . . H21 H -0.299936 0.368573 0.596512 0.038 Uiso 1 1 calc R U . . . C22 C -0.2497(2) 0.31181(18) 0.4894(2) 0.0328(6) Uani 1 1 d . . . . . H22 H -0.322525 0.292532 0.472168 0.039 Uiso 1 1 calc R U . . . C23 C -0.1569(2) 0.29443(17) 0.44034(17) 0.0294(5) Uani 1 1 d . . . . . H23 H -0.166661 0.264307 0.389222 0.035 Uiso 1 1 calc R U . . . C24 C -0.0502(2) 0.32069(16) 0.46545(14) 0.0218(4) Uani 1 1 d . . . . . H24 H 0.013354 0.306630 0.432538 0.026 Uiso 1 1 calc R U . . . C25 C 0.41289(18) 0.73498(15) 0.74028(13) 0.0186(4) Uani 1 1 d . . . . . H25A H 0.437330 0.791883 0.770793 0.022 Uiso 1 1 calc R U . . . H25B H 0.481372 0.698324 0.726498 0.022 Uiso 1 1 calc R U . . . C26 C 0.35759(17) 0.76811(14) 0.66043(13) 0.0159(4) Uani 1 1 d . . . . . C27 C 0.4397(2) 0.83534(17) 0.61713(14) 0.0230(4) Uani 1 1 d . . . . . H27A H 0.511013 0.801605 0.605601 0.028 Uiso 1 1 calc R U . . . H27B H 0.456818 0.890041 0.652743 0.028 Uiso 1 1 calc R U . . . C28 C 0.3875(2) 0.87098(17) 0.53693(16) 0.0279(5) Uani 1 1 d . . . . . H28 H 0.441549 0.914652 0.509200 0.034 Uiso 1 1 calc R U . . . C29 C 0.3615(2) 0.78619(17) 0.48101(14) 0.0249(5) Uani 1 1 d . . . . . H29A H 0.327827 0.809296 0.429708 0.030 Uiso 1 1 calc R U . . . H29B H 0.432245 0.752449 0.467652 0.030 Uiso 1 1 calc R U . . . C30 C 0.27981(19) 0.71791(15) 0.52304(13) 0.0189(4) Uani 1 1 d . . . . . C31 C 0.33238(18) 0.68470(14) 0.60340(12) 0.0161(4) Uani 1 1 d . . . . . H31A H 0.280125 0.640241 0.630707 0.019 Uiso 1 1 calc R U . . . H31B H 0.403121 0.650106 0.591848 0.019 Uiso 1 1 calc R U . . . C32 C 0.24787(19) 0.82239(16) 0.67772(14) 0.0208(4) Uani 1 1 d . . . . . H32A H 0.263810 0.877268 0.713439 0.025 Uiso 1 1 calc R U . . . H32B H 0.193998 0.780268 0.706084 0.025 Uiso 1 1 calc R U . . . C33 C 0.1957(2) 0.85733(17) 0.59751(15) 0.0251(5) Uani 1 1 d . . . . . H33 H 0.124146 0.892017 0.609313 0.030 Uiso 1 1 calc R U . . . C34 C 0.2782(3) 0.92431(17) 0.55540(17) 0.0320(6) Uani 1 1 d . . . . . H34A H 0.294270 0.979309 0.590959 0.038 Uiso 1 1 calc R U . . . H34B H 0.244742 0.948247 0.504307 0.038 Uiso 1 1 calc R U . . . C35 C 0.1706(2) 0.77220(17) 0.54302(15) 0.0236(4) Uani 1 1 d . . . . . H35A H 0.134963 0.794280 0.492057 0.028 Uiso 1 1 calc R U . . . H35B H 0.117110 0.729201 0.570824 0.028 Uiso 1 1 calc R U . . . C36 C 0.2490(2) 0.63340(16) 0.46792(14) 0.0217(4) Uani 1 1 d . . . . . H36A H 0.202919 0.657791 0.422371 0.026 Uiso 1 1 calc R U . . . H36B H 0.200852 0.589577 0.499569 0.026 Uiso 1 1 calc R U . . . 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 0.0213(2) 0.0174(2) 0.0171(2) -0.00120(18) 0.00035(19) 0.00283(19) S2 0.0274(3) 0.0238(3) 0.0174(2) -0.0017(2) 0.0014(2) 0.0008(2) C1 0.0220(9) 0.0181(9) 0.0169(9) 0.0000(8) -0.0022(8) 0.0010(8) C2 0.0235(10) 0.0136(9) 0.0186(9) 0.0002(7) -0.0024(8) 0.0018(7) C3 0.0185(9) 0.0146(9) 0.0219(10) -0.0011(7) -0.0044(8) 0.0029(7) C4 0.0189(10) 0.0189(10) 0.0210(10) -0.0031(8) -0.0011(8) 0.0041(8) C5 0.0227(10) 0.0139(8) 0.0178(9) -0.0024(7) -0.0028(8) 0.0022(8) C6 0.0212(10) 0.0132(9) 0.0232(10) -0.0025(8) -0.0021(8) -0.0006(8) C7 0.0201(9) 0.0157(9) 0.0210(10) 0.0007(8) 0.0005(8) 0.0004(8) C8 0.0270(11) 0.0196(10) 0.0184(9) -0.0035(8) -0.0029(8) -0.0001(8) C9 0.0270(10) 0.0163(9) 0.0154(9) -0.0010(8) 0.0004(8) 0.0052(8) C10 0.0249(11) 0.0242(10) 0.0187(9) 0.0012(8) 0.0015(8) 0.0071(9) C11 0.0224(10) 0.0240(10) 0.0144(9) -0.0003(8) 0.0002(8) -0.0006(8) C12 0.0243(11) 0.0224(10) 0.0226(10) 0.0014(8) -0.0010(8) -0.0012(9) C13 0.0211(10) 0.0316(12) 0.0251(11) -0.0003(9) -0.0020(9) 0.0010(9) C14 0.0223(11) 0.0352(12) 0.0270(11) -0.0041(10) 0.0034(9) -0.0100(10) C15 0.0380(14) 0.0212(11) 0.0271(12) -0.0012(9) 0.0040(10) -0.0072(10) C16 0.0271(12) 0.0236(11) 0.0239(11) 0.0006(9) 0.0024(9) 0.0026(9) C17 0.0261(11) 0.0162(9) 0.0217(10) -0.0015(7) 0.0015(8) -0.0005(8) C18 0.0264(11) 0.0189(9) 0.0210(10) 0.0005(8) -0.0008(9) 0.0011(8) C19 0.0210(10) 0.0165(9) 0.0211(10) 0.0030(8) -0.0020(8) -0.0009(8) C20 0.0274(11) 0.0271(11) 0.0235(11) 0.0033(9) 0.0024(9) 0.0050(9) C21 0.0211(11) 0.0255(12) 0.0475(15) 0.0142(11) 0.0084(10) 0.0026(9) C22 0.0206(11) 0.0209(11) 0.0568(17) 0.0086(11) -0.0104(11) -0.0069(9) C23 0.0355(13) 0.0185(10) 0.0341(13) -0.0015(9) -0.0119(10) -0.0043(9) C24 0.0245(11) 0.0202(10) 0.0208(10) 0.0019(8) 0.0002(8) -0.0027(8) C25 0.0182(9) 0.0166(9) 0.0209(10) -0.0036(8) -0.0013(8) -0.0006(8) C26 0.0152(9) 0.0124(8) 0.0201(9) -0.0013(7) 0.0000(7) -0.0006(7) C27 0.0227(10) 0.0200(10) 0.0263(11) -0.0004(9) 0.0022(8) -0.0072(9) C28 0.0349(13) 0.0193(10) 0.0296(12) 0.0054(9) 0.0036(10) -0.0078(9) C29 0.0298(12) 0.0243(11) 0.0207(10) 0.0044(8) 0.0027(9) -0.0044(9) C30 0.0203(10) 0.0171(9) 0.0192(10) 0.0000(8) -0.0021(8) 0.0002(8) C31 0.0161(9) 0.0146(9) 0.0175(9) -0.0001(7) -0.0016(7) -0.0007(7) C32 0.0204(9) 0.0179(10) 0.0242(10) -0.0008(8) -0.0007(8) 0.0047(8) C33 0.0254(11) 0.0216(11) 0.0284(11) 0.0004(9) -0.0049(9) 0.0097(9) C34 0.0476(15) 0.0168(10) 0.0318(13) 0.0048(9) -0.0057(11) 0.0026(10) C35 0.0200(10) 0.0244(10) 0.0262(11) 0.0000(8) -0.0057(9) 0.0053(8) C36 0.0217(10) 0.0218(10) 0.0215(10) -0.0014(8) -0.0042(8) -0.0002(8) 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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 0.00 -1.00 0.1020 -1.00 1.00 1.00 0.1210 1.00 1.00 0.00 0.0830 0.00 -1.00 1.00 0.1630 0.00 -1.00 4.00 0.0980 0.00 1.00 0.00 0.1270 1.00 -4.00 -1.00 0.1380 2.00 -1.00 -2.00 0.1220 1.00 0.00 -1.00 0.0930 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 S1 C1 103.18(10) . . ? C36 S2 C8 104.50(11) . . ? C2 C1 S1 111.11(15) . . ? C2 C1 H1A 109.4 . . ? S1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? S1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C7 C2 C3 118.7(2) . . ? C7 C2 C1 119.2(2) . . ? C3 C2 C1 121.60(19) . . ? C4 C3 C2 119.1(2) . . ? C4 C3 C9 119.0(2) . . ? C2 C3 C9 121.52(19) . . ? C5 C4 C3 121.7(2) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 118.63(19) . . ? C4 C5 C8 119.1(2) . . ? C6 C5 C8 121.8(2) . . ? C5 C6 C7 119.3(2) . . ? C5 C6 C17 121.3(2) . . ? C7 C6 C17 119.3(2) . . ? C2 C7 C6 121.8(2) . . ? C2 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C5 C8 S2 111.48(15) . . ? C5 C8 H8A 109.3 . . ? S2 C8 H8A 109.3 . . ? C5 C8 H8B 109.3 . . ? S2 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C3 176.2(2) . . ? C9 C10 C11 178.0(3) . . ? C12 C11 C16 118.9(2) . . ? C12 C11 C10 120.9(2) . . ? C16 C11 C10 120.2(2) . . ? C13 C12 C11 120.5(2) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 120.1(2) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.1(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.6(2) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C11 119.8(2) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? C18 C17 C6 179.1(3) . . ? C17 C18 C19 178.3(3) . . ? C20 C19 C24 119.0(2) . . ? C20 C19 C18 120.7(2) . . ? C24 C19 C18 120.3(2) . . ? C21 C20 C19 120.3(2) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 120.3(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.1(2) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.4(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C19 119.9(2) . . ? C23 C24 H24 120.1 . . ? C19 C24 H24 120.1 . . ? C26 C25 S1 116.32(15) . . ? C26 C25 H25A 108.2 . . ? S1 C25 H25A 108.2 . . ? C26 C25 H25B 108.2 . . ? S1 C25 H25B 108.2 . . ? H25A C25 H25B 107.4 . . ? C31 C26 C27 108.22(17) . . ? C31 C26 C32 109.22(17) . . ? C27 C26 C32 108.49(18) . . ? C31 C26 C25 111.91(16) . . ? C27 C26 C25 108.20(17) . . ? C32 C26 C25 110.71(17) . . ? C26 C27 C28 110.08(18) . . ? C26 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? C26 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.2 . . ? C34 C28 C29 109.3(2) . . ? C34 C28 C27 109.3(2) . . ? C29 C28 C27 109.85(19) . . ? C34 C28 H28 109.5 . . ? C29 C28 H28 109.5 . . ? C27 C28 H28 109.5 . . ? C30 C29 C28 110.12(19) . . ? C30 C29 H29A 109.6 . . ? C28 C29 H29A 109.6 . . ? C30 C29 H29B 109.6 . . ? C28 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C31 108.85(18) . . ? C29 C30 C36 111.70(19) . . ? C31 C30 C36 111.62(17) . . ? C29 C30 C35 108.53(18) . . ? C31 C30 C35 108.02(18) . . ? C36 C30 C35 108.00(18) . . ? C26 C31 C30 111.91(16) . . ? C26 C31 H31A 109.2 . . ? C30 C31 H31A 109.2 . . ? C26 C31 H31B 109.2 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C26 C32 C33 109.93(18) . . ? C26 C32 H32A 109.7 . . ? C33 C32 H32A 109.7 . . ? C26 C32 H32B 109.7 . . ? C33 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C35 110.1(2) . . ? C34 C33 C32 109.2(2) . . ? C35 C33 C32 109.35(18) . . ? C34 C33 H33 109.4 . . ? C35 C33 H33 109.4 . . ? C32 C33 H33 109.4 . . ? C33 C34 C28 109.31(19) . . ? C33 C34 H34A 109.8 . . ? C28 C34 H34A 109.8 . . ? C33 C34 H34B 109.8 . . ? C28 C34 H34B 109.8 . . ? H34A C34 H34B 108.3 . . ? C33 C35 C30 110.51(19) . . ? C33 C35 H35A 109.5 . . ? C30 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C30 C36 S2 117.16(16) . . ? C30 C36 H36A 108.0 . . ? S2 C36 H36A 108.0 . . ? C30 C36 H36B 108.0 . . ? S2 C36 H36B 108.0 . . ? H36A C36 H36B 107.3 . . ? 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 C25 1.829(2) . ? S1 C1 1.830(2) . ? S2 C36 1.831(2) . ? S2 C8 1.838(2) . ? C1 C2 1.503(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.383(3) . ? C2 C3 1.411(3) . ? C3 C4 1.398(3) . ? C3 C9 1.465(3) . ? C4 C5 1.397(3) . ? C4 H4 0.9500 . ? C5 C6 1.400(3) . ? C5 C8 1.501(3) . ? C6 C7 1.405(3) . ? C6 C17 1.449(3) . ? C7 H7 0.9500 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.170(3) . ? C10 C11 1.442(3) . ? C11 C12 1.399(3) . ? C11 C16 1.403(3) . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 C14 1.385(4) . ? C13 H13 0.9500 . ? C14 C15 1.379(4) . ? C14 H14 0.9500 . ? C15 C16 1.392(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.183(3) . ? C18 C19 1.439(3) . ? C19 C20 1.401(3) . ? C19 C24 1.405(3) . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 C22 1.380(4) . ? C21 H21 0.9500 . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 C24 1.383(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.542(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C31 1.534(3) . ? C26 C27 1.535(3) . ? C26 C32 1.538(3) . ? C27 C28 1.543(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C34 1.530(4) . ? C28 C29 1.540(3) . ? C28 H28 1.0000 . ? C29 C30 1.532(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.536(3) . ? C30 C36 1.542(3) . ? C30 C35 1.542(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.540(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.527(4) . ? C33 C35 1.528(3) . ? C33 H33 1.0000 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? 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 C25 S1 C1 C2 -66.93(17) . . . . ? S1 C1 C2 C7 -67.9(2) . . . . ? S1 C1 C2 C3 103.9(2) . . . . ? C7 C2 C3 C4 5.7(3) . . . . ? C1 C2 C3 C4 -166.1(2) . . . . ? C7 C2 C3 C9 178.48(19) . . . . ? C1 C2 C3 C9 6.7(3) . . . . ? C2 C3 C4 C5 1.6(3) . . . . ? C9 C3 C4 C5 -171.33(19) . . . . ? C3 C4 C5 C6 -7.1(3) . . . . ? C3 C4 C5 C8 165.8(2) . . . . ? C4 C5 C6 C7 5.2(3) . . . . ? C8 C5 C6 C7 -167.5(2) . . . . ? C4 C5 C6 C17 -178.4(2) . . . . ? C8 C5 C6 C17 8.9(3) . . . . ? C3 C2 C7 C6 -7.6(3) . . . . ? C1 C2 C7 C6 164.3(2) . . . . ? C5 C6 C7 C2 2.1(3) . . . . ? C17 C6 C7 C2 -174.3(2) . . . . ? C4 C5 C8 S2 -67.9(2) . . . . ? C6 C5 C8 S2 104.8(2) . . . . ? C36 S2 C8 C5 -63.37(18) . . . . ? C16 C11 C12 C13 -1.0(4) . . . . ? C10 C11 C12 C13 178.6(2) . . . . ? C11 C12 C13 C14 1.6(4) . . . . ? C12 C13 C14 C15 -1.6(4) . . . . ? C13 C14 C15 C16 1.0(4) . . . . ? C14 C15 C16 C11 -0.4(4) . . . . ? C12 C11 C16 C15 0.4(4) . . . . ? C10 C11 C16 C15 -179.2(2) . . . . ? C24 C19 C20 C21 -0.4(3) . . . . ? C18 C19 C20 C21 -179.8(2) . . . . ? C19 C20 C21 C22 -0.7(4) . . . . ? C20 C21 C22 C23 0.3(4) . . . . ? C21 C22 C23 C24 1.2(4) . . . . ? C22 C23 C24 C19 -2.2(4) . . . . ? C20 C19 C24 C23 1.8(3) . . . . ? C18 C19 C24 C23 -178.7(2) . . . . ? C1 S1 C25 C26 115.81(16) . . . . ? S1 C25 C26 C31 -66.3(2) . . . . ? S1 C25 C26 C27 174.59(15) . . . . ? S1 C25 C26 C32 55.8(2) . . . . ? C31 C26 C27 C28 58.9(2) . . . . ? C32 C26 C27 C28 -59.4(2) . . . . ? C25 C26 C27 C28 -179.61(18) . . . . ? C26 C27 C28 C34 60.2(2) . . . . ? C26 C27 C28 C29 -59.8(3) . . . . ? C34 C28 C29 C30 -60.8(3) . . . . ? C27 C28 C29 C30 59.1(3) . . . . ? C28 C29 C30 C31 -58.0(2) . . . . ? C28 C29 C30 C36 178.3(2) . . . . ? C28 C29 C30 C35 59.4(2) . . . . ? C27 C26 C31 C30 -59.5(2) . . . . ? C32 C26 C31 C30 58.4(2) . . . . ? C25 C26 C31 C30 -178.67(18) . . . . ? C29 C30 C31 C26 59.2(2) . . . . ? C36 C30 C31 C26 -177.01(18) . . . . ? C35 C30 C31 C26 -58.4(2) . . . . ? C31 C26 C32 C33 -58.0(2) . . . . ? C27 C26 C32 C33 59.8(2) . . . . ? C25 C26 C32 C33 178.38(18) . . . . ? C26 C32 C33 C34 -60.8(2) . . . . ? C26 C32 C33 C35 59.8(2) . . . . ? C35 C33 C34 C28 -59.4(3) . . . . ? C32 C33 C34 C28 60.7(3) . . . . ? C29 C28 C34 C33 60.0(3) . . . . ? C27 C28 C34 C33 -60.3(3) . . . . ? C34 C33 C35 C30 59.2(2) . . . . ? C32 C33 C35 C30 -60.9(3) . . . . ? C29 C30 C35 C33 -58.6(2) . . . . ? C31 C30 C35 C33 59.3(2) . . . . ? C36 C30 C35 C33 -179.82(19) . . . . ? C29 C30 C36 S2 53.7(2) . . . . ? C31 C30 C36 S2 -68.4(2) . . . . ? C35 C30 C36 S2 172.98(16) . . . . ? C8 S2 C36 C30 114.38(17) . . . . ?