#------------------------------------------------------------------------------ #$Date: 2025-03-13 03:52:03 +0200 (Thu, 13 Mar 2025) $ #$Revision: 298422 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/04/7160405.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_7160405 loop_ _publ_author_name 'Kou, Cai-Lan' 'Yang, Long' 'Sun, Ling-Zhi' 'Li, Meng' 'Luo, Xi' 'Guo, Hongbo' 'Xie, Jian-Bo' _publ_section_title ; Highly Enantio-Selective Synthesis of Aza-Spirocyclic Indanones via Rhodium Catalysis† ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D5OB00291E _journal_year 2025 _chemical_absolute_configuration ad _chemical_formula_moiety 'C20 H21 N O3 S' _chemical_formula_sum 'C20 H21 N O3 S' _chemical_formula_weight 355.44 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-05-20 _audit_creation_method ; Olex2 1.5 (compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396) ; _audit_update_record ; 2025-01-06 deposited with the CCDC. 2025-03-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.368(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.3191(6) _cell_length_b 11.9918(7) _cell_length_c 12.3216(6) _cell_measurement_reflns_used 8708 _cell_measurement_temperature 150.00 _cell_measurement_theta_max 56.942 _cell_measurement_theta_min 3.120 _cell_volume 1820.21(16) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 150.00 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_unetI/netI 0.0749 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.971 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 11193 _diffrn_reflns_point_group_measured_fraction_full 0.808 _diffrn_reflns_point_group_measured_fraction_max 0.780 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 56.953 _diffrn_reflns_theta_min 3.120 _diffrn_source_current 2.86 _diffrn_source_power 0.1997996 _diffrn_source_voltage 69.86 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.129 _exptl_absorpt_correction_T_max 0.7512 _exptl_absorpt_correction_T_min 0.6120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1448 before and 0.0857 after correction. The Ratio of minimum to maximum transmission is 0.8147. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.297 _exptl_crystal_description block _exptl_crystal_F_000 752 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.233 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.051 _refine_ls_abs_structure_details ; Flack x determined using 1793 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.096(14) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 453 _refine_ls_number_reflns 5822 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0411 _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^)+(0.0538P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1052 _refine_ls_wR_factor_ref 0.1081 _reflns_Friedel_coverage 0.529 _reflns_Friedel_fraction_full 0.612 _reflns_Friedel_fraction_max 0.568 _reflns_number_gt 5397 _reflns_number_total 5822 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d5ob00291e3.cif _cod_data_source_block 11 _cod_database_code 7160405 _shelx_shelxl_version_number 2019/1 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27), C37(H37), C38(H38), C39(H39), C40(H40) 2.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C21(H21A,H21B,H21C) ; _shelx_res_file ; TITL 11_a.res in P2(1) 11.res created by SHELXL-2019/1 at 16:43:13 on 20-May-2024 REM Old TITL 11 in P2(1) REM SHELXT solution in P2(1) REM R1 0.092, Rweak 0.030, Alpha 0.006, Orientation as input REM Flack x = 0.218 ( 0.010 ) from Parsons' quotients REM Formula found by SHELXT: C40 N2 O6 S2 CELL 1.34139 12.3191 11.9918 12.3216 90 90.368 90 ZERR 4 0.0006 0.0007 0.0006 0 0.002 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O S DISP C 0.0137 0.0067 57.1 DISP H 0 0 0.6 DISP N 0.0241 0.0134 109.9 DISP O 0.0389 0.0241 193.4 DISP S 0.2925 0.4295 3294.4 UNIT 80 84 4 12 4 L.S. 10 PLAN 5 TEMP -123.15 BOND $H LIST 6 fmap 2 MORE -1 ACTA REM REM REM WGHT 0.053800 FVAR 0.95453 S1 5 0.099764 0.338141 0.171899 11.00000 0.02226 0.03343 = 0.02351 0.00189 0.00185 -0.00124 O4 4 0.531372 0.379109 -0.061597 11.00000 0.05912 0.05603 = 0.02987 0.01973 0.01683 0.01416 O5 4 0.133811 0.442283 0.127374 11.00000 0.03096 0.03575 = 0.03800 0.01144 0.00606 0.00184 O6 4 0.011128 0.279193 0.122870 11.00000 0.02775 0.05322 = 0.03063 -0.00565 -0.00291 -0.00476 N1 3 0.205243 0.254447 0.167511 11.00000 0.02242 0.02680 = 0.02423 -0.00122 0.00280 -0.00208 C1 1 -0.009744 0.421562 0.643982 11.00000 0.06147 0.06408 = 0.02770 0.00152 0.00476 0.02386 AFIX 137 H1A 2 -0.080843 0.458142 0.645888 11.00000 -1.50000 H1B 2 0.044951 0.470679 0.676748 11.00000 -1.50000 H1C 2 -0.012879 0.351490 0.684769 11.00000 -1.50000 AFIX 0 C2 1 0.020345 0.397504 0.527791 11.00000 0.03705 0.04343 = 0.02749 0.00053 0.00173 0.01596 C3 1 -0.033344 0.315222 0.469475 11.00000 0.03572 0.04821 = 0.03570 0.00676 0.01152 -0.00021 AFIX 43 H3 2 -0.086898 0.271295 0.504487 11.00000 -1.20000 AFIX 0 C4 1 -0.010508 0.295727 0.361172 11.00000 0.03015 0.03469 = 0.03421 0.00183 0.00361 -0.00678 AFIX 43 H4 2 -0.048649 0.239667 0.322021 11.00000 -1.20000 AFIX 0 C5 1 0.069289 0.359482 0.310162 11.00000 0.01938 0.03144 = 0.02440 0.00201 0.00186 0.00348 C6 1 0.125514 0.439582 0.367674 11.00000 0.02217 0.03412 = 0.03469 -0.00193 -0.00235 -0.00079 AFIX 43 H6 2 0.181028 0.481505 0.333399 11.00000 -1.20000 AFIX 0 C7 1 0.100735 0.458961 0.476303 11.00000 0.03482 0.03863 = 0.03503 -0.00672 -0.01028 0.00779 AFIX 43 H7 2 0.139166 0.514731 0.515564 11.00000 -1.20000 AFIX 0 C8 1 0.187736 0.137407 0.197960 11.00000 0.03327 0.02656 = 0.03971 0.00051 0.00332 -0.00839 AFIX 23 H8A 2 0.117236 0.111025 0.168726 11.00000 -1.20000 H8B 2 0.186533 0.130081 0.277973 11.00000 -1.20000 AFIX 0 C9 1 0.279657 0.068065 0.151534 11.00000 0.04183 0.02400 = 0.05009 -0.00291 -0.00565 -0.00060 AFIX 23 H9A 2 0.276651 0.070918 0.071272 11.00000 -1.20000 H9B 2 0.270990 -0.010645 0.174115 11.00000 -1.20000 AFIX 0 C10 1 0.390386 0.112058 0.191370 11.00000 0.03226 0.02971 = 0.03785 0.00004 -0.00498 0.00542 AFIX 23 H10A 2 0.396159 0.102085 0.270957 11.00000 -1.20000 H10B 2 0.449181 0.068382 0.157200 11.00000 -1.20000 AFIX 0 C11 1 0.404321 0.234615 0.163643 11.00000 0.02541 0.02973 = 0.01539 -0.00159 -0.00016 0.00175 C12 1 0.308320 0.300471 0.210362 11.00000 0.02258 0.02402 = 0.02175 0.00122 0.00273 -0.00313 AFIX 23 H12A 2 0.309269 0.295376 0.290556 11.00000 -1.20000 H12B 2 0.314659 0.380041 0.189947 11.00000 -1.20000 AFIX 0 C13 1 0.412849 0.256420 0.040132 11.00000 0.03147 0.04902 = 0.01788 0.00028 0.00282 0.00734 AFIX 23 H13A 2 0.424341 0.185451 0.000798 11.00000 -1.20000 H13B 2 0.345287 0.291344 0.012537 11.00000 -1.20000 AFIX 0 C14 1 0.508116 0.333575 0.023523 11.00000 0.03712 0.03344 = 0.02968 0.00612 0.01115 0.01876 C15 1 0.565745 0.342924 0.127961 11.00000 0.02937 0.02676 = 0.03045 0.00229 0.00860 0.00638 C16 1 0.510058 0.284559 0.207102 11.00000 0.02247 0.02873 = 0.02288 -0.00381 0.00300 0.00350 C17 1 0.551158 0.279065 0.312285 11.00000 0.02911 0.04708 = 0.02374 -0.00448 0.00079 -0.00005 AFIX 43 H17 2 0.513646 0.239349 0.367216 11.00000 -1.20000 AFIX 0 C18 1 0.649476 0.333643 0.335383 11.00000 0.03244 0.06120 = 0.03613 -0.01751 -0.00311 -0.00216 AFIX 43 H18 2 0.679336 0.329461 0.406544 11.00000 -1.20000 AFIX 0 C19 1 0.703736 0.393484 0.256293 11.00000 0.02987 0.04303 = 0.06072 -0.01428 0.00249 -0.00810 AFIX 43 H19 2 0.769281 0.431209 0.274097 11.00000 -1.20000 AFIX 0 C20 1 0.662958 0.398584 0.151521 11.00000 0.03403 0.03334 = 0.05188 0.00315 0.01186 -0.00182 AFIX 43 H20 2 0.700105 0.438958 0.096794 11.00000 -1.20000 AFIX 0 S2 5 0.352595 0.657951 0.341330 11.00000 0.02228 0.03109 = 0.02555 0.00348 0.00053 -0.00328 O1 4 0.262477 0.701994 0.401259 11.00000 0.02563 0.05382 = 0.03064 -0.00196 0.00743 -0.00278 O2 4 0.394748 0.549172 0.366745 11.00000 0.03395 0.03199 = 0.03821 0.01168 -0.00609 -0.00544 O3 4 0.789925 0.576532 0.521552 11.00000 0.05768 0.06849 = 0.03941 0.02229 -0.00015 0.02429 N2 3 0.453336 0.746504 0.357809 11.00000 0.01994 0.02739 = 0.02690 0.00009 -0.00056 -0.00029 C21 1 0.219748 0.628314 -0.131447 11.00000 0.03758 0.03899 = 0.03107 -0.00310 -0.00384 0.00130 AFIX 137 H21A 2 0.283309 0.630121 -0.178836 11.00000 -1.50000 H21B 2 0.170102 0.688875 -0.151472 11.00000 -1.50000 H21C 2 0.182487 0.556578 -0.139667 11.00000 -1.50000 AFIX 0 C22 1 0.255598 0.642701 -0.015310 11.00000 0.02211 0.02970 = 0.02922 0.00393 -0.00002 -0.00329 C23 1 0.345531 0.583391 0.023729 11.00000 0.02409 0.02566 = 0.03130 -0.00372 0.00564 -0.00007 AFIX 43 H23 2 0.386160 0.538259 -0.024643 11.00000 -1.20000 AFIX 0 C24 1 0.376071 0.589560 0.131685 11.00000 0.01973 0.02346 = 0.03353 0.00427 0.00063 0.00246 AFIX 43 H24 2 0.437069 0.548649 0.157376 11.00000 -1.20000 AFIX 0 C25 1 0.316844 0.656167 0.202658 11.00000 0.02129 0.02045 = 0.02907 0.00226 -0.00037 -0.00461 C26 1 0.200220 0.711849 0.055822 11.00000 0.02033 0.02938 = 0.03363 0.00344 -0.00312 0.00215 AFIX 43 H26 2 0.141186 0.755243 0.029416 11.00000 -1.20000 AFIX 0 C27 1 0.229083 0.718919 0.164111 11.00000 0.02066 0.03438 = 0.03048 -0.00181 -0.00100 0.00357 AFIX 43 H27 2 0.189727 0.765909 0.211867 11.00000 -1.20000 AFIX 0 C28 1 0.427755 0.866561 0.350560 11.00000 0.02806 0.02706 = 0.02698 -0.00168 -0.00433 0.00532 AFIX 23 H28A 2 0.357954 0.882149 0.386929 11.00000 -1.20000 H28B 2 0.421126 0.889265 0.273554 11.00000 -1.20000 AFIX 0 C29 1 0.518920 0.931442 0.405583 11.00000 0.03630 0.02587 = 0.03368 -0.00384 -0.00646 0.00091 AFIX 23 H29A 2 0.521878 0.912059 0.483646 11.00000 -1.20000 H29B 2 0.504489 1.012411 0.399356 11.00000 -1.20000 AFIX 0 C30 1 0.628182 0.903952 0.352682 11.00000 0.03175 0.02937 = 0.03141 -0.00113 -0.00638 -0.00376 AFIX 23 H30A 2 0.627799 0.931349 0.276888 11.00000 -1.20000 H30B 2 0.687071 0.942986 0.392381 11.00000 -1.20000 AFIX 0 C31 1 0.650581 0.779196 0.353244 11.00000 0.02184 0.03396 = 0.01859 0.00187 -0.00192 0.00116 C32 1 0.554455 0.717707 0.299677 11.00000 0.02285 0.02778 = 0.02210 -0.00255 0.00043 0.00137 AFIX 23 H32A 2 0.548040 0.739858 0.222502 11.00000 -1.20000 H32B 2 0.566696 0.636175 0.302812 11.00000 -1.20000 AFIX 0 C33 1 0.672209 0.730557 0.467723 11.00000 0.02951 0.03733 = 0.01797 0.00094 -0.00372 0.00209 AFIX 23 H33A 2 0.693121 0.790546 0.518944 11.00000 -1.20000 H33B 2 0.606403 0.693063 0.495506 11.00000 -1.20000 AFIX 0 C34 1 0.763748 0.647805 0.455475 11.00000 0.03084 0.04205 = 0.02638 0.00316 -0.00412 0.00279 C35 1 0.813594 0.667677 0.348427 11.00000 0.02373 0.03884 = 0.02708 0.00141 -0.00235 0.00048 C36 1 0.752892 0.745845 0.291568 11.00000 0.01904 0.03318 = 0.02297 -0.00340 -0.00428 -0.00317 C37 1 0.784732 0.777374 0.188305 11.00000 0.02853 0.05351 = 0.02128 0.00506 -0.00345 -0.00653 AFIX 43 H37 2 0.744995 0.831948 0.148742 11.00000 -1.20000 AFIX 0 C38 1 0.876590 0.727105 0.143670 11.00000 0.03450 0.06965 = 0.02464 -0.00214 0.00520 -0.01590 AFIX 43 H38 2 0.898711 0.747576 0.072690 11.00000 -1.20000 AFIX 0 C39 1 0.935969 0.648310 0.200426 11.00000 0.02854 0.05723 = 0.04212 -0.01139 0.00629 -0.00342 AFIX 43 H39 2 0.997829 0.614950 0.168182 11.00000 -1.20000 AFIX 0 C40 1 0.905637 0.618235 0.303305 11.00000 0.02489 0.04493 = 0.04541 -0.00193 0.00050 0.00286 AFIX 43 H40 2 0.946467 0.564751 0.343173 11.00000 -1.20000 AFIX 0 HKLF 4 REM 11_a.res in P2(1) REM wR2 = 0.1081, GooF = S = 1.031, Restrained GooF = 1.031 for all data REM R1 = 0.0411 for 5397 Fo > 4sig(Fo) and 0.0451 for all 5822 data REM 453 parameters refined using 1 restraints END WGHT 0.0538 0.0000 REM Highest difference peak 0.233, deepest hole -0.336, 1-sigma level 0.051 Q1 1 0.1434 0.2722 0.1394 11.00000 0.05 0.23 Q2 1 0.3557 0.1415 0.3644 11.00000 0.05 0.22 Q3 1 -0.1342 0.3187 0.2545 11.00000 0.05 0.22 Q4 1 0.0219 0.0172 0.0457 11.00000 0.05 0.21 Q5 1 0.0604 0.3155 0.0722 11.00000 0.05 0.20 ; _shelx_res_checksum 42213 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 0.09976(5) 0.33814(8) 0.17190(6) 0.0264(2) Uani 1 1 d . . . . . O4 O 0.5314(2) 0.3791(3) -0.0616(2) 0.0483(8) Uani 1 1 d . . . . . O5 O 0.13381(18) 0.4423(2) 0.1274(2) 0.0349(6) Uani 1 1 d . . . . . O6 O 0.01113(18) 0.2792(2) 0.12287(19) 0.0372(7) Uani 1 1 d . . . . . N1 N 0.2052(2) 0.2544(3) 0.1675(2) 0.0245(6) Uani 1 1 d . . . . . C1 C -0.0097(4) 0.4216(5) 0.6440(3) 0.0511(12) Uani 1 1 d . . . . . H1A H -0.080843 0.458142 0.645888 0.077 Uiso 1 1 calc R U . . . H1B H 0.044951 0.470679 0.676748 0.077 Uiso 1 1 calc R U . . . H1C H -0.012879 0.351490 0.684769 0.077 Uiso 1 1 calc R U . . . C2 C 0.0203(3) 0.3975(4) 0.5278(3) 0.0360(9) Uani 1 1 d . . . . . C3 C -0.0333(3) 0.3152(4) 0.4695(3) 0.0398(10) Uani 1 1 d . . . . . H3 H -0.086898 0.271295 0.504487 0.048 Uiso 1 1 calc R U . . . C4 C -0.0105(3) 0.2957(3) 0.3612(3) 0.0330(8) Uani 1 1 d . . . . . H4 H -0.048649 0.239667 0.322021 0.040 Uiso 1 1 calc R U . . . C5 C 0.0693(2) 0.3595(3) 0.3102(3) 0.0251(8) Uani 1 1 d . . . . . C6 C 0.1255(3) 0.4396(3) 0.3677(3) 0.0303(8) Uani 1 1 d . . . . . H6 H 0.181028 0.481505 0.333399 0.036 Uiso 1 1 calc R U . . . C7 C 0.1007(3) 0.4590(4) 0.4763(3) 0.0362(9) Uani 1 1 d . . . . . H7 H 0.139166 0.514731 0.515564 0.043 Uiso 1 1 calc R U . . . C8 C 0.1877(3) 0.1374(3) 0.1980(3) 0.0332(8) Uani 1 1 d . . . . . H8A H 0.117236 0.111025 0.168726 0.040 Uiso 1 1 calc R U . . . H8B H 0.186533 0.130081 0.277973 0.040 Uiso 1 1 calc R U . . . C9 C 0.2797(3) 0.0681(4) 0.1515(3) 0.0387(9) Uani 1 1 d . . . . . H9A H 0.276651 0.070918 0.071272 0.046 Uiso 1 1 calc R U . . . H9B H 0.270990 -0.010645 0.174115 0.046 Uiso 1 1 calc R U . . . C10 C 0.3904(3) 0.1121(3) 0.1914(3) 0.0333(8) Uani 1 1 d . . . . . H10A H 0.396159 0.102085 0.270957 0.040 Uiso 1 1 calc R U . . . H10B H 0.449181 0.068382 0.157200 0.040 Uiso 1 1 calc R U . . . C11 C 0.4043(2) 0.2346(3) 0.1636(2) 0.0235(7) Uani 1 1 d . . . . . C12 C 0.3083(2) 0.3005(3) 0.2104(2) 0.0228(7) Uani 1 1 d . . . . . H12A H 0.309269 0.295376 0.290556 0.027 Uiso 1 1 calc R U . . . H12B H 0.314659 0.380041 0.189947 0.027 Uiso 1 1 calc R U . . . C13 C 0.4128(3) 0.2564(4) 0.0401(2) 0.0328(9) Uani 1 1 d . . . . . H13A H 0.424341 0.185451 0.000798 0.039 Uiso 1 1 calc R U . . . H13B H 0.345287 0.291344 0.012537 0.039 Uiso 1 1 calc R U . . . C14 C 0.5081(3) 0.3336(4) 0.0235(3) 0.0334(8) Uani 1 1 d . . . . . C15 C 0.5657(2) 0.3429(3) 0.1280(3) 0.0288(7) Uani 1 1 d . . . . . C16 C 0.5101(2) 0.2846(3) 0.2071(2) 0.0247(7) Uani 1 1 d . . . . . C17 C 0.5512(3) 0.2791(4) 0.3123(3) 0.0333(9) Uani 1 1 d . . . . . H17 H 0.513646 0.239349 0.367216 0.040 Uiso 1 1 calc R U . . . C18 C 0.6495(3) 0.3336(4) 0.3354(3) 0.0433(10) Uani 1 1 d . . . . . H18 H 0.679336 0.329461 0.406544 0.052 Uiso 1 1 calc R U . . . C19 C 0.7037(3) 0.3935(4) 0.2563(4) 0.0445(10) Uani 1 1 d . . . . . H19 H 0.769281 0.431209 0.274097 0.053 Uiso 1 1 calc R U . . . C20 C 0.6630(3) 0.3986(4) 0.1515(3) 0.0397(10) Uani 1 1 d . . . . . H20 H 0.700105 0.438958 0.096794 0.048 Uiso 1 1 calc R U . . . S2 S 0.35259(6) 0.65795(8) 0.34133(6) 0.0263(2) Uani 1 1 d . . . . . O1 O 0.26248(18) 0.7020(3) 0.40126(19) 0.0367(6) Uani 1 1 d . . . . . O2 O 0.39475(19) 0.5492(2) 0.3667(2) 0.0347(6) Uani 1 1 d . . . . . O3 O 0.7899(2) 0.5765(3) 0.5216(2) 0.0552(9) Uani 1 1 d . . . . . N2 N 0.45334(19) 0.7465(3) 0.3578(2) 0.0247(6) Uani 1 1 d . . . . . C21 C 0.2197(3) 0.6283(4) -0.1314(3) 0.0359(9) Uani 1 1 d . . . . . H21A H 0.283309 0.630121 -0.178836 0.054 Uiso 1 1 calc R U . . . H21B H 0.170102 0.688875 -0.151472 0.054 Uiso 1 1 calc R U . . . H21C H 0.182487 0.556578 -0.139667 0.054 Uiso 1 1 calc R U . . . C22 C 0.2556(2) 0.6427(3) -0.0153(3) 0.0270(7) Uani 1 1 d . . . . . C23 C 0.3455(2) 0.5834(3) 0.0237(3) 0.0270(7) Uani 1 1 d . . . . . H23 H 0.386160 0.538259 -0.024643 0.032 Uiso 1 1 calc R U . . . C24 C 0.3761(2) 0.5896(3) 0.1317(3) 0.0256(7) Uani 1 1 d . . . . . H24 H 0.437069 0.548649 0.157376 0.031 Uiso 1 1 calc R U . . . C25 C 0.3168(2) 0.6562(3) 0.2027(3) 0.0236(7) Uani 1 1 d . . . . . C26 C 0.2002(2) 0.7118(3) 0.0558(3) 0.0278(8) Uani 1 1 d . . . . . H26 H 0.141186 0.755243 0.029416 0.033 Uiso 1 1 calc R U . . . C27 C 0.2291(2) 0.7189(3) 0.1641(3) 0.0285(8) Uani 1 1 d . . . . . H27 H 0.189727 0.765909 0.211867 0.034 Uiso 1 1 calc R U . . . C28 C 0.4278(3) 0.8666(3) 0.3506(3) 0.0274(8) Uani 1 1 d . . . . . H28A H 0.357954 0.882149 0.386929 0.033 Uiso 1 1 calc R U . . . H28B H 0.421126 0.889265 0.273554 0.033 Uiso 1 1 calc R U . . . C29 C 0.5189(3) 0.9314(3) 0.4056(3) 0.0320(8) Uani 1 1 d . . . . . H29A H 0.521878 0.912059 0.483646 0.038 Uiso 1 1 calc R U . . . H29B H 0.504489 1.012411 0.399356 0.038 Uiso 1 1 calc R U . . . C30 C 0.6282(3) 0.9040(3) 0.3527(3) 0.0309(8) Uani 1 1 d . . . . . H30A H 0.627799 0.931349 0.276888 0.037 Uiso 1 1 calc R U . . . H30B H 0.687071 0.942986 0.392381 0.037 Uiso 1 1 calc R U . . . C31 C 0.6506(2) 0.7792(3) 0.3532(2) 0.0248(7) Uani 1 1 d . . . . . C32 C 0.5545(2) 0.7177(3) 0.2997(2) 0.0242(7) Uani 1 1 d . . . . . H32A H 0.548040 0.739858 0.222502 0.029 Uiso 1 1 calc R U . . . H32B H 0.566696 0.636175 0.302812 0.029 Uiso 1 1 calc R U . . . C33 C 0.6722(2) 0.7306(3) 0.4677(2) 0.0283(8) Uani 1 1 d . . . . . H33A H 0.693121 0.790546 0.518944 0.034 Uiso 1 1 calc R U . . . H33B H 0.606403 0.693063 0.495506 0.034 Uiso 1 1 calc R U . . . C34 C 0.7637(3) 0.6478(4) 0.4555(3) 0.0331(8) Uani 1 1 d . . . . . C35 C 0.8136(2) 0.6677(3) 0.3484(3) 0.0299(8) Uani 1 1 d . . . . . C36 C 0.7529(2) 0.7458(3) 0.2916(2) 0.0251(7) Uani 1 1 d . . . . . C37 C 0.7847(3) 0.7774(4) 0.1883(3) 0.0345(9) Uani 1 1 d . . . . . H37 H 0.744995 0.831948 0.148742 0.041 Uiso 1 1 calc R U . . . C38 C 0.8766(3) 0.7271(4) 0.1437(3) 0.0429(11) Uani 1 1 d . . . . . H38 H 0.898711 0.747576 0.072690 0.051 Uiso 1 1 calc R U . . . C39 C 0.9360(3) 0.6483(4) 0.2004(3) 0.0426(10) Uani 1 1 d . . . . . H39 H 0.997829 0.614950 0.168182 0.051 Uiso 1 1 calc R U . . . C40 C 0.9056(3) 0.6182(4) 0.3033(3) 0.0384(9) Uani 1 1 d . . . . . H40 H 0.946467 0.564751 0.343173 0.046 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 0.0223(3) 0.0334(5) 0.0235(4) 0.0019(4) 0.0018(3) -0.0012(3) O4 0.0591(17) 0.056(2) 0.0299(13) 0.0197(14) 0.0168(12) 0.0142(14) O5 0.0310(12) 0.0358(17) 0.0380(14) 0.0114(12) 0.0061(10) 0.0018(11) O6 0.0277(11) 0.053(2) 0.0306(12) -0.0056(12) -0.0029(10) -0.0048(11) N1 0.0224(12) 0.0268(18) 0.0242(13) -0.0012(12) 0.0028(10) -0.0021(11) C1 0.061(3) 0.064(4) 0.028(2) 0.002(2) 0.0048(18) 0.024(2) C2 0.0371(19) 0.043(3) 0.0275(18) 0.0005(17) 0.0017(14) 0.0160(17) C3 0.0357(17) 0.048(3) 0.0357(19) 0.0068(19) 0.0115(15) -0.0002(17) C4 0.0301(16) 0.035(2) 0.0342(18) 0.0018(16) 0.0036(14) -0.0068(15) C5 0.0194(13) 0.031(2) 0.0244(15) 0.0020(14) 0.0019(11) 0.0035(13) C6 0.0222(15) 0.034(2) 0.0347(18) -0.0019(16) -0.0023(13) -0.0008(14) C7 0.0348(17) 0.039(3) 0.0350(19) -0.0067(17) -0.0103(15) 0.0078(17) C8 0.0333(16) 0.027(2) 0.0397(18) 0.0005(16) 0.0033(14) -0.0084(15) C9 0.042(2) 0.024(2) 0.050(2) -0.0029(18) -0.0056(17) -0.0006(17) C10 0.0323(17) 0.030(2) 0.0378(19) 0.0000(17) -0.0050(14) 0.0054(15) C11 0.0254(14) 0.030(2) 0.0154(14) -0.0016(14) -0.0002(11) 0.0017(14) C12 0.0226(13) 0.024(2) 0.0218(15) 0.0012(13) 0.0027(11) -0.0031(12) C13 0.0315(16) 0.049(3) 0.0179(15) 0.0003(15) 0.0028(13) 0.0073(16) C14 0.0371(16) 0.033(2) 0.0297(17) 0.0061(17) 0.0112(13) 0.0188(17) C15 0.0294(15) 0.027(2) 0.0304(16) 0.0023(16) 0.0086(12) 0.0064(15) C16 0.0225(14) 0.029(2) 0.0229(15) -0.0038(14) 0.0030(12) 0.0035(14) C17 0.0291(15) 0.047(3) 0.0237(16) -0.0045(17) 0.0008(13) -0.0001(16) C18 0.0324(17) 0.061(3) 0.0361(19) -0.018(2) -0.0031(14) -0.002(2) C19 0.0299(18) 0.043(3) 0.061(3) -0.014(2) 0.0025(17) -0.0081(17) C20 0.0340(19) 0.033(3) 0.052(2) 0.0032(19) 0.0119(17) -0.0018(16) S2 0.0223(3) 0.0311(5) 0.0255(4) 0.0035(4) 0.0005(3) -0.0033(3) O1 0.0256(10) 0.0538(19) 0.0306(12) -0.0020(12) 0.0074(9) -0.0028(11) O2 0.0340(12) 0.0320(17) 0.0382(13) 0.0117(12) -0.0061(10) -0.0054(11) O3 0.0577(17) 0.068(2) 0.0394(15) 0.0223(16) -0.0002(13) 0.0243(16) N2 0.0199(12) 0.0274(18) 0.0269(14) 0.0001(12) -0.0006(10) -0.0003(11) C21 0.0376(17) 0.039(3) 0.0311(17) -0.0031(16) -0.0038(14) 0.0013(16) C22 0.0221(13) 0.030(2) 0.0292(16) 0.0039(15) 0.0000(12) -0.0033(14) C23 0.0241(15) 0.026(2) 0.0313(17) -0.0037(15) 0.0056(13) -0.0001(14) C24 0.0197(14) 0.023(2) 0.0335(17) 0.0043(15) 0.0006(12) 0.0025(13) C25 0.0213(13) 0.0204(18) 0.0291(15) 0.0023(15) -0.0004(11) -0.0046(13) C26 0.0203(14) 0.029(2) 0.0336(17) 0.0034(15) -0.0031(12) 0.0022(13) C27 0.0207(14) 0.034(2) 0.0305(17) -0.0018(16) -0.0010(12) 0.0036(14) C28 0.0281(15) 0.027(2) 0.0270(16) -0.0017(14) -0.0043(12) 0.0053(14) C29 0.0363(18) 0.026(2) 0.0337(18) -0.0038(15) -0.0065(15) 0.0009(15) C30 0.0318(17) 0.029(2) 0.0314(18) -0.0011(16) -0.0064(14) -0.0038(15) C31 0.0218(14) 0.034(2) 0.0186(14) 0.0019(14) -0.0019(11) 0.0012(14) C32 0.0228(14) 0.028(2) 0.0221(15) -0.0026(14) 0.0004(11) 0.0014(13) C33 0.0295(15) 0.037(2) 0.0180(15) 0.0009(15) -0.0037(12) 0.0021(15) C34 0.0308(16) 0.042(3) 0.0264(16) 0.0032(17) -0.0041(13) 0.0028(16) C35 0.0237(14) 0.039(2) 0.0271(16) 0.0014(16) -0.0024(12) 0.0005(15) C36 0.0190(13) 0.033(2) 0.0230(15) -0.0034(14) -0.0043(11) -0.0032(13) C37 0.0285(15) 0.054(3) 0.0213(15) 0.0051(17) -0.0034(13) -0.0065(17) C38 0.0345(18) 0.070(3) 0.0246(17) -0.002(2) 0.0052(14) -0.016(2) C39 0.0285(16) 0.057(3) 0.042(2) -0.011(2) 0.0063(15) -0.0034(18) C40 0.0249(16) 0.045(3) 0.045(2) -0.0019(19) 0.0005(14) 0.0029(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.2925 0.4295 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 S1 O6 119.66(16) . . ? O5 S1 N1 106.69(14) . . ? O5 S1 C5 107.98(17) . . ? O6 S1 N1 106.61(16) . . ? O6 S1 C5 108.21(14) . . ? N1 S1 C5 107.06(14) . . ? C8 N1 S1 117.2(2) . . ? C8 N1 C12 113.1(3) . . ? C12 N1 S1 116.0(2) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? C3 C2 C1 120.6(4) . . ? C3 C2 C7 118.7(3) . . ? C7 C2 C1 120.8(4) . . ? C2 C3 H3 119.3 . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C3 C4 H4 120.4 . . ? C3 C4 C5 119.2(3) . . ? C5 C4 H4 120.4 . . ? C4 C5 S1 120.6(3) . . ? C6 C5 S1 119.2(2) . . ? C6 C5 C4 120.2(3) . . ? C5 C6 H6 120.1 . . ? C5 C6 C7 119.8(3) . . ? C7 C6 H6 120.1 . . ? C2 C7 C6 120.7(4) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? N1 C8 H8A 110.0 . . ? N1 C8 H8B 110.0 . . ? N1 C8 C9 108.4(3) . . ? H8A C8 H8B 108.4 . . ? C9 C8 H8A 110.0 . . ? C9 C8 H8B 110.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C8 C9 C10 110.7(3) . . ? H9A C9 H9B 108.1 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? C9 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C11 C10 C9 111.2(3) . . ? C11 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C10 C11 C12 108.9(3) . . ? C10 C11 C13 113.1(3) . . ? C10 C11 C16 113.4(3) . . ? C12 C11 C13 109.8(3) . . ? C16 C11 C12 108.9(3) . . ? C16 C11 C13 102.4(2) . . ? N1 C12 C11 109.6(3) . . ? N1 C12 H12A 109.8 . . ? N1 C12 H12B 109.8 . . ? C11 C12 H12A 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? C11 C13 H13A 110.3 . . ? C11 C13 H13B 110.3 . . ? H13A C13 H13B 108.5 . . ? C14 C13 C11 107.1(3) . . ? C14 C13 H13A 110.3 . . ? C14 C13 H13B 110.3 . . ? O4 C14 C13 125.4(3) . . ? O4 C14 C15 127.2(4) . . ? C15 C14 C13 107.4(3) . . ? C16 C15 C14 109.8(3) . . ? C16 C15 C20 121.4(3) . . ? C20 C15 C14 128.7(3) . . ? C15 C16 C11 112.1(3) . . ? C15 C16 C17 120.1(3) . . ? C17 C16 C11 127.8(3) . . ? C16 C17 H17 120.8 . . ? C16 C17 C18 118.4(3) . . ? C18 C17 H17 120.8 . . ? C17 C18 H18 119.4 . . ? C19 C18 C17 121.2(4) . . ? C19 C18 H18 119.4 . . ? C18 C19 H19 119.8 . . ? C20 C19 C18 120.3(4) . . ? C20 C19 H19 119.8 . . ? C15 C20 H20 120.7 . . ? C19 C20 C15 118.5(4) . . ? C19 C20 H20 120.7 . . ? O1 S2 O2 120.03(16) . . ? O1 S2 N2 106.49(15) . . ? O1 S2 C25 108.27(14) . . ? O2 S2 N2 106.72(15) . . ? O2 S2 C25 106.73(16) . . ? N2 S2 C25 108.13(14) . . ? C28 N2 S2 117.5(2) . . ? C28 N2 C32 112.2(3) . . ? C32 N2 S2 115.2(2) . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? C23 C22 C21 119.7(3) . . ? C26 C22 C21 121.8(3) . . ? C26 C22 C23 118.5(3) . . ? C22 C23 H23 119.5 . . ? C24 C23 C22 120.9(3) . . ? C24 C23 H23 119.5 . . ? C23 C24 H24 120.2 . . ? C23 C24 C25 119.6(3) . . ? C25 C24 H24 120.2 . . ? C24 C25 S2 119.1(2) . . ? C24 C25 C27 120.1(3) . . ? C27 C25 S2 120.7(2) . . ? C22 C26 H26 119.3 . . ? C27 C26 C22 121.5(3) . . ? C27 C26 H26 119.3 . . ? C25 C27 H27 120.4 . . ? C26 C27 C25 119.3(3) . . ? C26 C27 H27 120.4 . . ? N2 C28 H28A 110.0 . . ? N2 C28 H28B 110.0 . . ? N2 C28 C29 108.4(3) . . ? H28A C28 H28B 108.4 . . ? C29 C28 H28A 110.0 . . ? C29 C28 H28B 110.0 . . ? C28 C29 H29A 109.6 . . ? C28 C29 H29B 109.6 . . ? C28 C29 C30 110.3(3) . . ? H29A C29 H29B 108.1 . . ? C30 C29 H29A 109.6 . . ? C30 C29 H29B 109.6 . . ? C29 C30 H30A 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? C31 C30 C29 111.6(3) . . ? C31 C30 H30A 109.3 . . ? C31 C30 H30B 109.3 . . ? C30 C31 C32 109.3(3) . . ? C30 C31 C33 113.9(3) . . ? C30 C31 C36 113.9(3) . . ? C32 C31 C33 109.7(3) . . ? C36 C31 C32 107.2(3) . . ? C36 C31 C33 102.5(2) . . ? N2 C32 C31 109.1(3) . . ? N2 C32 H32A 109.9 . . ? N2 C32 H32B 109.9 . . ? C31 C32 H32A 109.9 . . ? C31 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? C31 C33 H33A 110.5 . . ? C31 C33 H33B 110.5 . . ? H33A C33 H33B 108.7 . . ? C34 C33 C31 106.3(3) . . ? C34 C33 H33A 110.5 . . ? C34 C33 H33B 110.5 . . ? O3 C34 C33 125.9(3) . . ? O3 C34 C35 126.7(3) . . ? C35 C34 C33 107.3(3) . . ? C36 C35 C34 109.5(3) . . ? C36 C35 C40 121.5(3) . . ? C40 C35 C34 129.0(3) . . ? C35 C36 C31 111.7(3) . . ? C35 C36 C37 119.6(3) . . ? C37 C36 C31 128.6(3) . . ? C36 C37 H37 120.7 . . ? C36 C37 C38 118.6(4) . . ? C38 C37 H37 120.7 . . ? C37 C38 H38 119.2 . . ? C39 C38 C37 121.5(3) . . ? C39 C38 H38 119.2 . . ? C38 C39 H39 120.0 . . ? C40 C39 C38 120.0(4) . . ? C40 C39 H39 120.0 . . ? C35 C40 H40 120.6 . . ? C39 C40 C35 118.8(4) . . ? C39 C40 H40 120.6 . . ? 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 O5 1.428(3) . ? S1 O6 1.431(2) . ? S1 N1 1.643(3) . ? S1 C5 1.765(3) . ? O4 C14 1.218(4) . ? N1 C8 1.469(5) . ? N1 C12 1.479(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C2 1.509(5) . ? C2 C3 1.386(5) . ? C2 C7 1.391(6) . ? C3 H3 0.9500 . ? C3 C4 1.385(5) . ? C4 H4 0.9500 . ? C4 C5 1.398(4) . ? C5 C6 1.378(5) . ? C6 H6 0.9500 . ? C6 C7 1.394(5) . ? C7 H7 0.9500 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.520(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.540(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.519(5) . ? C11 C12 1.537(4) . ? C11 C13 1.548(4) . ? C11 C16 1.527(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.509(5) . ? C14 C15 1.470(5) . ? C15 C16 1.386(5) . ? C15 C20 1.400(5) . ? C16 C17 1.390(4) . ? C17 H17 0.9500 . ? C17 C18 1.404(5) . ? C18 H18 0.9500 . ? C18 C19 1.386(6) . ? C19 H19 0.9500 . ? C19 C20 1.384(6) . ? C20 H20 0.9500 . ? S2 O1 1.438(2) . ? S2 O2 1.438(3) . ? S2 N2 1.645(3) . ? S2 C25 1.762(3) . ? O3 C34 1.222(5) . ? N2 C28 1.476(5) . ? N2 C32 1.482(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C22 1.505(4) . ? C22 C23 1.399(4) . ? C22 C26 1.389(5) . ? C23 H23 0.9500 . ? C23 C24 1.382(5) . ? C24 H24 0.9500 . ? C24 C25 1.394(5) . ? C25 C27 1.398(4) . ? C26 H26 0.9500 . ? C26 C27 1.381(5) . ? C27 H27 0.9500 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 C29 1.522(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.535(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C30 C31 1.521(5) . ? C31 C32 1.540(4) . ? C31 C33 1.548(4) . ? C31 C36 1.529(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 C34 1.510(5) . ? C34 C35 1.478(5) . ? C35 C36 1.386(5) . ? C35 C40 1.398(5) . ? C36 C37 1.386(5) . ? C37 H37 0.9500 . ? C37 C38 1.398(5) . ? C38 H38 0.9500 . ? C38 C39 1.382(6) . ? C39 H39 0.9500 . ? C39 C40 1.372(6) . ? C40 H40 0.9500 . ?