#------------------------------------------------------------------------------ #$Date: 2020-06-03 06:44:06 +0300 (Wed, 03 Jun 2020) $ #$Revision: 252563 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/75/7157527.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_7157527 loop_ _publ_author_name 'Yang, Yong' 'Niu, Chuang' 'Chen, Muqing' 'Yang, Shangfeng' 'Wang, Guan-Wu' _publ_section_title ; Electrochemical regioselective alkylations of [60]fulleroindoline with bulky alkyl bromides ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D0OB00876A _journal_year 2020 _chemical_formula_sum 'C96 H31 N O S2' _chemical_formula_weight 1278.34 _chemical_name_common C60-derivative _chemical_name_systematic C60-derivative _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-04-16 deposited with the CCDC. 2020-06-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.62 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.205 _cell_length_b 23.555 _cell_length_c 23.364 _cell_measurement_reflns_used 9603 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 50.084 _cell_measurement_theta_min 4.368 _cell_volume 5589.214 _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measurement_device_type 'CCD MX300-HE' _diffrn_measurement_method phi_scans _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_unetI/netI 0.0434 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.971 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 9603 _diffrn_reflns_point_group_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 25.042 _diffrn_reflns_theta_max 25.042 _diffrn_reflns_theta_min 2.184 _diffrn_source 'SSRF,Beamline BL17B' _exptl_absorpt_coefficient_mu 0.160 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour Black _exptl_crystal_density_diffrn 1.519 _exptl_crystal_description Block _exptl_crystal_F_000 2616 _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 1.660 _refine_diff_density_min -1.617 _refine_diff_density_rms 0.102 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 888 _refine_ls_number_reflns 9603 _refine_ls_number_restraints 36 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.1196 _refine_ls_R_factor_gt 0.1151 _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^)+(0.0944P)^2^+36.0052P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2902 _refine_ls_wR_factor_ref 0.2931 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8906 _reflns_number_total 9603 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ob00876a2.cif _cod_data_source_block lz-1 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 5589.2 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7157527 _shelx_shelxl_version_number 2014/7 _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 0.6390 _shelx_estimated_absorpt_t_max 0.7449 _shelx_res_file ; lz-1.res created by SHELXL-2014/7 TITL lz-1_a.res in P2(1)/n REM Old TITL lz-1 in P2 #3 REM SHELXT solution in P2(1)/n REM R1 0.200, Rweak 0.037, Alpha 0.067, Orientation as input REM Formula found by SHELXT: C96 N4 CELL 0.71073 10.205 23.555 23.364 90 95.62 90 ZERR 4 0 0 0 0 0 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O S UNIT 384 124 4 4 8 SIMU 0.01 0.02 2 C85 C86 C87 C88 C89 C84 L.S. 60 0 0 PLAN 20 list 4 fmap 2 53 acta REM REM REM WGHT 0.094400 36.005199 FVAR 0.56536 S2 5 0.511730 0.403593 0.860846 11.00000 0.06322 S1 5 0.560060 0.426831 0.735096 11.00000 0.08674 O1 4 0.844661 0.733648 0.879445 11.00000 0.04414 0.03051 = 0.04309 -0.00509 -0.00126 0.00279 N1 3 0.871733 0.654480 0.828135 11.00000 0.04026 0.02841 = 0.03233 -0.00268 -0.00141 0.00201 C8 1 0.605561 0.574100 0.659707 11.00000 0.03252 0.02363 = 0.03109 -0.00217 0.00154 -0.00075 C75 1 0.916351 0.533396 0.736813 11.00000 0.03648 0.03027 = 0.03476 -0.00126 0.00391 -0.00205 AFIX 43 H75 2 0.872135 0.518649 0.703394 11.00000 -1.20000 AFIX 0 C3 1 0.755271 0.722117 0.761929 11.00000 0.02875 0.02577 = 0.03406 -0.00261 0.00069 -0.00173 C6 1 0.753855 0.648087 0.630216 11.00000 0.02913 0.02832 = 0.03712 -0.00264 0.00995 0.00099 C26 1 0.414213 0.566677 0.708580 11.00000 0.03676 0.02316 = 0.03156 -0.00093 0.00587 -0.00309 C10 1 0.524238 0.583591 0.748396 11.00000 0.03602 0.02489 = 0.02879 0.00311 0.00850 0.00231 C25 1 0.463911 0.561902 0.653354 11.00000 0.03565 0.02022 = 0.03372 -0.00035 0.00651 0.00001 C20 1 0.727677 0.693001 0.590598 11.00000 0.03605 0.03304 = 0.03285 0.00112 0.01196 -0.00116 C29 1 0.378964 0.641867 0.798266 11.00000 0.03731 0.03398 = 0.02961 0.00085 0.00848 -0.00008 C9 1 0.639217 0.587239 0.715760 11.00000 0.03601 0.02397 = 0.02820 -0.00223 0.00664 -0.00048 C21 1 0.618659 0.676971 0.549537 11.00000 0.03946 0.03379 = 0.02947 -0.00080 0.01148 0.00187 C44 1 0.254592 0.601073 0.610027 11.00000 0.03096 0.03103 = 0.03868 -0.00757 0.00145 -0.00666 C74 1 0.875193 0.583507 0.759922 11.00000 0.03367 0.02806 = 0.03234 -0.00109 0.00361 -0.00309 C4 1 0.799950 0.717337 0.706301 11.00000 0.02745 0.02717 = 0.03832 -0.00094 0.00070 -0.00078 C5 1 0.790048 0.659920 0.687627 11.00000 0.02825 0.02724 = 0.03569 -0.00052 0.00278 -0.00172 C33 1 0.480569 0.807510 0.786197 11.00000 0.04449 0.02456 = 0.03936 -0.00836 0.00012 0.00406 C11 1 0.508316 0.618956 0.793458 11.00000 0.04036 0.02827 = 0.02696 0.00010 0.00389 -0.00180 C80 1 0.938763 0.604923 0.810987 11.00000 0.03760 0.02668 = 0.03778 -0.00296 0.00094 -0.00028 C13 1 0.532596 0.712604 0.824514 11.00000 0.04341 0.03005 = 0.02488 -0.00416 -0.00008 0.00324 C51 1 0.318688 0.844568 0.687068 11.00000 0.04476 0.02946 = 0.04497 -0.00369 0.00300 0.00617 C35 1 0.458940 0.857391 0.693395 11.00000 0.04281 0.02236 = 0.04628 -0.00287 0.00114 0.00182 C30 1 0.393969 0.700221 0.816777 11.00000 0.04398 0.03710 = 0.02597 -0.00380 0.01151 -0.00208 C2 1 0.745119 0.663969 0.790024 11.00000 0.03539 0.02530 = 0.03210 -0.00072 0.00128 -0.00115 C36 1 0.507105 0.853270 0.636832 11.00000 0.04423 0.02248 = 0.04660 0.00479 0.00506 -0.00045 C62 1 0.808577 0.565903 0.525624 11.00000 0.03888 0.03384 = 0.03250 -0.00333 0.00711 0.00120 C15 1 0.689576 0.770109 0.776297 11.00000 0.03810 0.02917 = 0.03447 -0.00526 -0.00135 -0.00445 C1 1 0.761300 0.620518 0.737657 11.00000 0.03174 0.02559 = 0.03251 -0.00225 0.00329 -0.00427 C45 1 0.206441 0.605113 0.663387 11.00000 0.02992 0.03291 = 0.04238 -0.00386 0.00230 -0.00622 C7 1 0.677790 0.594079 0.609733 11.00000 0.03332 0.03147 = 0.02632 -0.00199 0.00369 -0.00075 C58 1 0.114371 0.699623 0.638554 11.00000 0.02893 0.04216 = 0.04171 -0.00924 0.00091 -0.00067 C69 1 0.604945 0.468918 0.576911 11.00000 0.05105 0.03071 = 0.03288 -0.00248 0.00670 0.00032 AFIX 43 H69 2 0.540153 0.494392 0.562667 11.00000 -1.20000 AFIX 0 C68 1 0.733353 0.487795 0.590477 11.00000 0.05235 0.03133 = 0.02742 -0.00222 0.00754 0.00777 C17 1 0.713211 0.812627 0.682072 11.00000 0.03919 0.02417 = 0.04983 0.00065 0.00397 -0.00943 C22 1 0.576003 0.621312 0.563470 11.00000 0.04028 0.03278 = 0.02704 -0.00280 0.00256 0.00348 C24 1 0.384531 0.577888 0.604900 11.00000 0.03734 0.02786 = 0.03556 -0.00599 0.00077 -0.00154 C14 1 0.574197 0.764786 0.808726 11.00000 0.03812 0.03291 = 0.03267 -0.00879 0.00049 0.00160 C28 1 0.270339 0.626191 0.759932 11.00000 0.03402 0.03474 = 0.03930 -0.00165 0.01238 -0.00786 C46 1 0.136044 0.655867 0.678284 11.00000 0.02681 0.04043 = 0.04702 -0.00571 0.00412 -0.00279 C85 1 0.721827 0.534998 0.863619 11.00000 0.04437 0.03348 = 0.03424 0.00125 0.00659 0.00146 AFIX 43 H85 2 0.667536 0.535949 0.829257 11.00000 -1.20000 AFIX 0 C42 1 0.349099 0.651853 0.538030 11.00000 0.04474 0.03490 = 0.02585 -0.00591 -0.00118 0.00403 C52 1 0.281241 0.832300 0.627088 11.00000 0.04727 0.03187 = 0.04181 -0.00035 -0.00515 0.00916 C47 1 0.174559 0.669008 0.738288 11.00000 0.02583 0.04616 = 0.04053 -0.00275 0.00727 -0.00048 C41 1 0.390941 0.705095 0.521251 11.00000 0.04514 0.03930 = 0.03013 -0.00184 -0.00010 0.00374 C38 1 0.650782 0.792438 0.585130 11.00000 0.04456 0.02737 = 0.04143 0.00984 0.00955 -0.00227 C37 1 0.631477 0.831345 0.631155 11.00000 0.05100 0.02433 = 0.04505 0.00576 0.00479 -0.00493 C40 1 0.529123 0.717992 0.527275 11.00000 0.04629 0.03664 = 0.02883 0.00322 0.00610 0.00273 C55 1 0.320372 0.755624 0.536351 11.00000 0.04802 0.03594 = 0.03401 0.00128 -0.00521 0.00778 C12 1 0.614865 0.656914 0.824013 11.00000 0.04241 0.02823 = 0.02985 -0.00307 0.00566 -0.00266 C16 1 0.666231 0.815607 0.735932 11.00000 0.04455 0.02230 = 0.03989 -0.00563 0.00095 -0.00492 C49 1 0.166897 0.770848 0.714615 11.00000 0.04085 0.04070 = 0.03832 -0.00649 0.00770 0.00746 C19 1 0.744166 0.749775 0.607425 11.00000 0.03521 0.03354 = 0.03882 0.00581 0.01160 -0.00720 C18 1 0.782679 0.762250 0.666887 11.00000 0.03681 0.03110 = 0.04022 0.00100 0.00961 -0.00678 C32 1 0.345795 0.795974 0.780934 11.00000 0.04176 0.03607 = 0.03491 -0.00861 0.00509 0.00716 C23 1 0.444260 0.609508 0.559396 11.00000 0.04279 0.03498 = 0.02458 -0.00662 0.00332 -0.00519 C90 1 0.530425 0.634676 0.923189 11.00000 0.04704 0.03440 = 0.03247 0.00011 0.00766 0.00252 C79 1 1.043510 0.575770 0.838795 11.00000 0.04057 0.03068 = 0.05179 -0.00250 -0.00507 0.00109 AFIX 43 H79 2 1.084108 0.589191 0.873546 11.00000 -1.20000 AFIX 0 C53 1 0.396587 0.837564 0.595968 11.00000 0.04584 0.02929 = 0.04335 0.00387 0.00120 0.00187 C27 1 0.289105 0.587367 0.713955 11.00000 0.03469 0.02939 = 0.03966 -0.00260 0.00974 -0.00783 C59 1 0.130682 0.758491 0.656957 11.00000 0.03076 0.03904 = 0.04721 -0.00546 0.00165 0.00740 C57 1 0.163708 0.695353 0.582573 11.00000 0.03244 0.03987 = 0.04024 -0.00676 -0.00440 0.00325 C61 1 0.774931 0.549488 0.585095 11.00000 0.03940 0.03199 = 0.03209 -0.00571 0.00257 0.00108 AFIX 13 H61 2 0.857687 0.552973 0.609919 11.00000 -1.20000 AFIX 0 C84 1 0.727912 0.582039 0.899209 11.00000 0.05876 0.03510 = 0.03217 -0.00264 0.00213 0.00441 C31 1 0.301769 0.740554 0.796901 11.00000 0.03698 0.03838 = 0.03546 -0.00865 0.00925 0.00100 C34 1 0.537019 0.838897 0.741605 11.00000 0.04810 0.02219 = 0.04213 -0.00545 0.00167 -0.00124 C83 1 0.649109 0.637167 0.888820 11.00000 0.04889 0.02776 = 0.02990 -0.00297 0.00624 0.00338 AFIX 13 H83 2 0.705498 0.667137 0.906905 11.00000 -1.20000 AFIX 0 C67 1 0.748669 0.540729 0.476215 11.00000 0.05111 0.04248 = 0.03568 -0.00616 0.00769 -0.01459 AFIX 43 H67 2 0.690600 0.510731 0.479444 11.00000 -1.20000 AFIX 0 C76 1 1.024321 0.505379 0.764039 11.00000 0.03659 0.02763 = 0.04850 0.00027 0.00762 0.00192 AFIX 43 H76 2 1.054208 0.472193 0.748106 11.00000 -1.20000 AFIX 0 C81 1 0.918495 0.695092 0.866996 11.00000 0.04005 0.02936 = 0.03537 -0.00333 0.00187 -0.00184 C48 1 0.190061 0.724585 0.756245 11.00000 0.03080 0.04602 = 0.03708 -0.00561 0.01120 0.00407 C73 1 0.829943 0.447989 0.609309 11.00000 0.05048 0.03579 = 0.03983 -0.00262 0.00363 0.01198 AFIX 43 H73 2 0.917018 0.459408 0.617424 11.00000 -1.20000 AFIX 0 C50 1 0.263116 0.814948 0.730008 11.00000 0.04130 0.03217 = 0.03996 -0.00727 0.00058 0.01092 C95 1 0.495102 0.682933 0.953102 11.00000 0.06026 0.04327 = 0.03507 -0.00094 0.01156 0.00296 AFIX 43 H95 2 0.541319 0.716618 0.949833 11.00000 -1.20000 AFIX 0 C60 1 0.188474 0.789362 0.612325 11.00000 0.04334 0.03586 = 0.04207 0.00010 -0.00382 0.00795 C39 1 0.544464 0.776784 0.546106 11.00000 0.05081 0.03423 = 0.03246 0.00650 0.00866 -0.00238 C54 1 0.415257 0.800145 0.551616 11.00000 0.05580 0.03049 = 0.03724 0.01254 0.00281 0.00895 C86 1 0.794296 0.486703 0.877828 11.00000 0.05519 0.03798 = 0.04100 -0.00308 0.00145 0.00523 AFIX 43 H86 2 0.794655 0.456909 0.851726 11.00000 -1.20000 AFIX 0 C43 1 0.233240 0.646596 0.568963 11.00000 0.03472 0.03788 = 0.03879 -0.00847 -0.00086 -0.00061 C77 1 1.088417 0.526224 0.814792 11.00000 0.03631 0.03122 = 0.05335 0.00012 0.00073 -0.00237 C82 1 1.058779 0.693370 0.892842 11.00000 0.04473 0.04062 = 0.04554 -0.00940 -0.00432 -0.00165 AFIX 137 H82A 2 1.084996 0.730502 0.906494 11.00000 -1.50000 H82B 2 1.114344 0.681456 0.864224 11.00000 -1.50000 H82C 2 1.066849 0.667050 0.924361 11.00000 -1.50000 AFIX 0 C56 1 0.208448 0.750280 0.566584 11.00000 0.04687 0.04076 = 0.03412 -0.00305 -0.00480 0.00660 C72 1 0.795593 0.391074 0.615927 11.00000 0.06867 0.03814 = 0.03956 0.00013 0.00401 0.01201 AFIX 43 H72 2 0.860525 0.364886 0.628229 11.00000 -1.20000 AFIX 0 C70 1 0.572552 0.411961 0.584524 11.00000 0.05813 0.03382 = 0.04141 -0.00719 0.01191 0.00095 AFIX 43 H70 2 0.486109 0.399821 0.576061 11.00000 -1.20000 AFIX 0 C66 1 0.773708 0.559465 0.421831 11.00000 0.05792 0.04528 = 0.03986 -0.00291 0.00556 -0.00685 AFIX 43 H66 2 0.732850 0.541998 0.389117 11.00000 -1.20000 AFIX 0 C94 1 0.391713 0.681076 0.987643 11.00000 0.05961 0.05181 = 0.04191 -0.00456 0.01543 0.01152 AFIX 43 H94 2 0.367685 0.713683 1.006482 11.00000 -1.20000 AFIX 0 C63 1 0.899407 0.608240 0.519893 11.00000 0.04486 0.05212 = 0.04453 -0.01123 0.01163 -0.01158 AFIX 43 H63 2 0.945193 0.623705 0.552596 11.00000 -1.20000 AFIX 0 C91 1 0.460339 0.584364 0.929717 11.00000 0.05791 0.03896 = 0.03896 -0.00404 0.01715 0.00044 AFIX 43 H91 2 0.482355 0.551678 0.910486 11.00000 -1.20000 AFIX 0 C93 1 0.324623 0.630910 0.994034 11.00000 0.05403 0.06389 = 0.04002 0.00194 0.01721 0.00697 AFIX 43 H93 2 0.257154 0.629555 1.018027 11.00000 -1.20000 AFIX 0 C71 1 0.669400 0.373427 0.604732 11.00000 0.08318 0.03137 = 0.03566 -0.00211 0.00966 0.00086 AFIX 43 H71 2 0.647609 0.335667 0.610541 11.00000 -1.20000 AFIX 0 C92 1 0.357250 0.583058 0.965076 11.00000 0.06236 0.05153 = 0.04276 0.00077 0.02155 -0.00705 AFIX 43 H92 2 0.310632 0.549578 0.968958 11.00000 -1.20000 AFIX 0 C65 1 0.859030 0.603864 0.416710 11.00000 0.06141 0.04516 = 0.04436 0.00067 0.01914 -0.00272 AFIX 43 H65 2 0.873368 0.617522 0.380499 11.00000 -1.20000 AFIX 0 C78 1 1.207401 0.495590 0.844460 11.00000 0.05197 0.03618 = 0.07254 -0.00496 -0.01570 0.01112 AFIX 137 H78A 2 1.283483 0.519602 0.844796 11.00000 -1.50000 H78B 2 1.222391 0.461186 0.824060 11.00000 -1.50000 H78C 2 1.191471 0.486637 0.883261 11.00000 -1.50000 AFIX 0 C1S 1 0.533252 0.414738 0.798138 11.00000 0.05817 C64 1 0.923836 0.628337 0.465592 11.00000 0.06212 0.05006 = 0.05224 -0.00706 0.02557 -0.01388 AFIX 43 H64 2 0.983073 0.657882 0.462280 11.00000 -1.20000 AFIX 0 C89 1 0.801017 0.577865 0.951264 11.00000 0.11445 0.05456 = 0.05470 -0.01926 -0.02682 0.02965 AFIX 43 H89 2 0.808400 0.609180 0.975609 11.00000 -1.20000 AFIX 0 C87 1 0.865657 0.482716 0.930406 11.00000 0.10424 0.05252 = 0.06353 -0.00792 -0.02265 0.03146 AFIX 43 H87 2 0.914317 0.450215 0.940449 11.00000 -1.20000 AFIX 0 C88 1 0.864398 0.527691 0.968393 11.00000 0.12423 0.06688 = 0.06384 -0.01630 -0.03725 0.03696 AFIX 43 H88 2 0.906075 0.524299 1.005454 11.00000 -1.20000 AFIX 0 HKLF 4 REM lz-1_a.res in P2(1)/n REM R1 = 0.1151 for 8906 Fo > 4sig(Fo) and 0.1196 for all 9603 data REM 888 parameters refined using 36 restraints END WGHT 0.0952 36.4609 REM Highest difference peak 1.660, deepest hole -1.617, 1-sigma level 0.102 Q1 1 0.6199 0.4398 0.7344 11.00000 0.05 1.66 Q2 1 0.5041 0.4185 0.7382 11.00000 0.05 1.51 Q3 1 0.9401 0.5410 0.9440 11.00000 0.05 1.09 Q4 1 0.7740 0.5599 0.3490 11.00000 0.05 0.73 Q5 1 0.9394 0.4983 0.9149 11.00000 0.05 0.63 Q6 1 0.8683 0.5982 0.9370 11.00000 0.05 0.62 Q7 1 0.1800 0.5627 0.5425 11.00000 0.05 0.47 Q8 1 0.6050 0.3768 0.7577 11.00000 0.05 0.45 Q9 1 0.5062 0.3993 0.8308 11.00000 0.05 0.45 Q10 1 0.6905 0.6787 0.5067 11.00000 0.05 0.40 Q11 1 0.7665 0.6807 0.4568 11.00000 0.05 0.40 Q12 1 0.6457 0.5770 1.0001 11.00000 0.05 0.39 Q13 1 0.3893 0.5194 0.9730 11.00000 0.05 0.35 Q14 1 0.6140 0.4826 0.7630 11.00000 0.05 0.33 Q15 1 0.6678 0.5740 0.9642 11.00000 0.05 0.32 Q16 1 0.7594 0.4403 0.5022 11.00000 0.05 0.32 Q17 1 0.8129 0.6647 0.4270 11.00000 0.05 0.32 Q18 1 0.6415 0.6822 0.6425 11.00000 0.05 0.31 Q19 1 1.2531 0.5230 0.8796 11.00000 0.05 0.31 Q20 1 0.6779 0.4787 0.5247 11.00000 0.05 0.30 ; _shelx_res_checksum 68163 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 S2 S 0.5117(2) 0.40359(9) 0.86085(9) 0.0632(5) Uiso 1 1 d . . . . . S1 S 0.5601(3) 0.42683(12) 0.73510(12) 0.0867(7) Uiso 1 1 d . . . . . O1 O 0.8447(4) 0.73365(16) 0.87944(18) 0.0396(9) Uani 1 1 d . . . . . N1 N 0.8717(5) 0.65448(19) 0.8281(2) 0.0340(10) Uani 1 1 d . . . . . C8 C 0.6056(5) 0.5741(2) 0.6597(2) 0.0292(11) Uani 1 1 d . . . . . C75 C 0.9164(5) 0.5334(2) 0.7368(2) 0.0338(12) Uani 1 1 d . . . . . H75 H 0.8721 0.5186 0.7034 0.041 Uiso 1 1 calc R U . . . C3 C 0.7553(5) 0.7221(2) 0.7619(2) 0.0297(11) Uani 1 1 d . . . . . C6 C 0.7539(5) 0.6481(2) 0.6302(2) 0.0311(11) Uani 1 1 d . . . . . C26 C 0.4142(5) 0.5667(2) 0.7086(2) 0.0303(11) Uani 1 1 d . . . . . C10 C 0.5242(5) 0.5836(2) 0.7484(2) 0.0295(11) Uani 1 1 d . . . . . C25 C 0.4639(5) 0.5619(2) 0.6534(2) 0.0297(11) Uani 1 1 d . . . . . C20 C 0.7277(5) 0.6930(2) 0.5906(2) 0.0334(12) Uani 1 1 d . . . . . C29 C 0.3790(5) 0.6419(2) 0.7983(2) 0.0333(12) Uani 1 1 d . . . . . C9 C 0.6392(5) 0.5872(2) 0.7158(2) 0.0292(11) Uani 1 1 d . . . . . C21 C 0.6187(5) 0.6770(2) 0.5495(2) 0.0337(12) Uani 1 1 d . . . . . C44 C 0.2546(5) 0.6011(2) 0.6100(2) 0.0337(12) Uani 1 1 d . . . . . C74 C 0.8752(5) 0.5835(2) 0.7599(2) 0.0313(11) Uani 1 1 d . . . . . C4 C 0.8000(5) 0.7173(2) 0.7063(2) 0.0311(11) Uani 1 1 d . . . . . C5 C 0.7900(5) 0.6599(2) 0.6876(2) 0.0304(11) Uani 1 1 d . . . . . C33 C 0.4806(6) 0.8075(2) 0.7862(3) 0.0364(13) Uani 1 1 d . . . . . C11 C 0.5083(5) 0.6190(2) 0.7935(2) 0.0318(11) Uani 1 1 d . . . . . C80 C 0.9388(6) 0.6049(2) 0.8110(2) 0.0342(12) Uani 1 1 d . . . . . C13 C 0.5326(6) 0.7126(2) 0.8245(2) 0.0330(12) Uani 1 1 d . . . . . C51 C 0.3187(6) 0.8446(2) 0.6871(3) 0.0398(13) Uani 1 1 d . . . . . C35 C 0.4589(6) 0.8574(2) 0.6934(3) 0.0374(13) Uani 1 1 d . . . . . C30 C 0.3940(6) 0.7002(2) 0.8168(2) 0.0351(12) Uani 1 1 d . . . . . C2 C 0.7451(5) 0.6640(2) 0.7900(2) 0.0311(11) Uani 1 1 d . . . . . C36 C 0.5071(6) 0.8533(2) 0.6368(3) 0.0377(13) Uani 1 1 d . . . . . C62 C 0.8086(6) 0.5659(2) 0.5256(2) 0.0348(12) Uani 1 1 d . . . . . C15 C 0.6896(6) 0.7701(2) 0.7763(2) 0.0342(12) Uani 1 1 d . . . . . C1 C 0.7613(5) 0.6205(2) 0.7377(2) 0.0299(11) Uani 1 1 d . . . . . C45 C 0.2064(5) 0.6051(2) 0.6634(3) 0.0351(12) Uani 1 1 d . . . . . C7 C 0.6778(5) 0.5941(2) 0.6097(2) 0.0303(11) Uani 1 1 d . . . . . C58 C 0.1144(5) 0.6996(3) 0.6386(3) 0.0378(13) Uani 1 1 d . . . . . C69 C 0.6049(6) 0.4689(2) 0.5769(2) 0.0380(13) Uani 1 1 d . . . . . H69 H 0.5402 0.4944 0.5627 0.046 Uiso 1 1 calc R U . . . C68 C 0.7334(6) 0.4878(2) 0.5905(2) 0.0368(13) Uani 1 1 d . . . . . C17 C 0.7132(6) 0.8126(2) 0.6821(3) 0.0378(13) Uani 1 1 d . . . . . C22 C 0.5760(6) 0.6213(2) 0.5635(2) 0.0334(12) Uani 1 1 d . . . . . C24 C 0.3845(5) 0.5779(2) 0.6049(2) 0.0338(12) Uani 1 1 d . . . . . C14 C 0.5742(6) 0.7648(2) 0.8087(2) 0.0348(12) Uani 1 1 d . . . . . C28 C 0.2703(5) 0.6262(2) 0.7599(3) 0.0354(12) Uani 1 1 d . . . . . C46 C 0.1360(5) 0.6559(3) 0.6783(3) 0.0381(13) Uani 1 1 d . . . . . C85 C 0.7218(6) 0.5350(2) 0.8636(3) 0.0372(12) Uani 1 1 d . U . . . H85 H 0.6675 0.5359 0.8293 0.045 Uiso 1 1 calc R U . . . C42 C 0.3491(6) 0.6519(2) 0.5380(2) 0.0355(12) Uani 1 1 d . . . . . C52 C 0.2812(6) 0.8323(2) 0.6271(3) 0.0409(14) Uani 1 1 d . . . . . C47 C 0.1746(5) 0.6690(3) 0.7383(3) 0.0372(13) Uani 1 1 d . . . . . C41 C 0.3909(6) 0.7051(2) 0.5213(2) 0.0384(13) Uani 1 1 d . . . . . C38 C 0.6508(6) 0.7924(2) 0.5851(3) 0.0374(13) Uani 1 1 d . . . . . C37 C 0.6315(6) 0.8313(2) 0.6312(3) 0.0401(13) Uani 1 1 d . . . . . C40 C 0.5291(6) 0.7180(2) 0.5273(2) 0.0371(13) Uani 1 1 d . . . . . C55 C 0.3204(6) 0.7556(2) 0.5364(3) 0.0399(13) Uani 1 1 d . . . . . C12 C 0.6149(6) 0.6569(2) 0.8240(2) 0.0334(12) Uani 1 1 d . . . . . C16 C 0.6662(6) 0.8156(2) 0.7359(3) 0.0358(13) Uani 1 1 d . . . . . C49 C 0.1669(6) 0.7708(3) 0.7146(3) 0.0397(13) Uani 1 1 d . . . . . C19 C 0.7442(5) 0.7498(2) 0.6074(3) 0.0353(12) Uani 1 1 d . . . . . C18 C 0.7827(6) 0.7622(2) 0.6669(3) 0.0357(12) Uani 1 1 d . . . . . C32 C 0.3458(6) 0.7960(2) 0.7809(2) 0.0375(13) Uani 1 1 d . . . . . C23 C 0.4443(6) 0.6095(2) 0.5594(2) 0.0341(12) Uani 1 1 d . . . . . C90 C 0.5304(6) 0.6347(2) 0.9232(2) 0.0377(13) Uani 1 1 d . . . . . C79 C 1.0435(6) 0.5758(2) 0.8388(3) 0.0416(14) Uani 1 1 d . . . . . H79 H 1.0841 0.5892 0.8735 0.050 Uiso 1 1 calc R U . . . C53 C 0.3966(6) 0.8376(2) 0.5960(3) 0.0397(13) Uani 1 1 d . . . . . C27 C 0.2891(5) 0.5874(2) 0.7140(2) 0.0342(12) Uani 1 1 d . . . . . C59 C 0.1307(5) 0.7585(3) 0.6570(3) 0.0391(13) Uani 1 1 d . . . . . C57 C 0.1637(5) 0.6954(3) 0.5826(3) 0.0380(13) Uani 1 1 d . . . . . C61 C 0.7749(6) 0.5495(2) 0.5851(2) 0.0346(12) Uani 1 1 d . . . . . H61 H 0.8577 0.5530 0.6099 0.041 Uiso 1 1 calc R U . . . C84 C 0.7279(7) 0.5820(3) 0.8992(3) 0.0422(13) Uani 1 1 d . U . . . C31 C 0.3018(6) 0.7406(2) 0.7969(2) 0.0366(13) Uani 1 1 d . . . . . C34 C 0.5370(6) 0.8389(2) 0.7416(3) 0.0377(13) Uani 1 1 d . . . . . C83 C 0.6491(6) 0.6372(2) 0.8888(2) 0.0354(12) Uani 1 1 d . . . . . H83 H 0.7055 0.6671 0.9069 0.042 Uiso 1 1 calc R U . . . C67 C 0.7487(6) 0.5407(3) 0.4762(3) 0.0429(14) Uani 1 1 d . . . . . H67 H 0.6906 0.5107 0.4794 0.051 Uiso 1 1 calc R U . . . C76 C 1.0243(6) 0.5054(2) 0.7640(3) 0.0373(13) Uani 1 1 d . . . . . H76 H 1.0542 0.4722 0.7481 0.045 Uiso 1 1 calc R U . . . C81 C 0.9185(6) 0.6951(2) 0.8670(2) 0.0350(12) Uani 1 1 d . . . . . C48 C 0.1901(5) 0.7246(3) 0.7562(3) 0.0374(13) Uani 1 1 d . . . . . C73 C 0.8299(6) 0.4480(2) 0.6093(3) 0.0421(14) Uani 1 1 d . . . . . H73 H 0.9170 0.4594 0.6174 0.051 Uiso 1 1 calc R U . . . C50 C 0.2631(6) 0.8149(2) 0.7300(3) 0.0380(13) Uani 1 1 d . . . . . C95 C 0.4951(7) 0.6829(3) 0.9531(3) 0.0457(15) Uani 1 1 d . . . . . H95 H 0.5413 0.7166 0.9498 0.055 Uiso 1 1 calc R U . . . C60 C 0.1885(6) 0.7894(2) 0.6123(3) 0.0410(14) Uani 1 1 d . . . . . C39 C 0.5445(6) 0.7768(2) 0.5461(2) 0.0389(13) Uani 1 1 d . . . . . C54 C 0.4153(6) 0.8001(2) 0.5516(3) 0.0413(14) Uani 1 1 d . . . . . C86 C 0.7943(6) 0.4867(3) 0.8778(3) 0.0449(14) Uani 1 1 d . U . . . H86 H 0.7947 0.4569 0.8517 0.054 Uiso 1 1 calc R U . . . C43 C 0.2332(6) 0.6466(2) 0.5690(3) 0.0374(13) Uani 1 1 d . . . . . C77 C 1.0884(6) 0.5262(2) 0.8148(3) 0.0405(14) Uani 1 1 d . . . . . C82 C 1.0588(6) 0.6934(3) 0.8928(3) 0.0442(14) Uani 1 1 d . . . . . H82A H 1.0850 0.7305 0.9065 0.066 Uiso 1 1 calc R U . . . H82B H 1.1143 0.6815 0.8642 0.066 Uiso 1 1 calc R U . . . H82C H 1.0668 0.6670 0.9244 0.066 Uiso 1 1 calc R U . . . C56 C 0.2084(6) 0.7503(3) 0.5666(3) 0.0412(14) Uani 1 1 d . . . . . C72 C 0.7956(7) 0.3911(3) 0.6159(3) 0.0489(16) Uani 1 1 d . . . . . H72 H 0.8605 0.3649 0.6282 0.059 Uiso 1 1 calc R U . . . C70 C 0.5726(7) 0.4120(3) 0.5845(3) 0.0440(14) Uani 1 1 d . . . . . H70 H 0.4861 0.3998 0.5761 0.053 Uiso 1 1 calc R U . . . C66 C 0.7737(7) 0.5595(3) 0.4218(3) 0.0476(15) Uani 1 1 d . . . . . H66 H 0.7329 0.5420 0.3891 0.057 Uiso 1 1 calc R U . . . C94 C 0.3917(7) 0.6811(3) 0.9876(3) 0.0504(16) Uani 1 1 d . . . . . H94 H 0.3677 0.7137 1.0065 0.061 Uiso 1 1 calc R U . . . C63 C 0.8994(6) 0.6082(3) 0.5199(3) 0.0467(15) Uani 1 1 d . . . . . H63 H 0.9452 0.6237 0.5526 0.056 Uiso 1 1 calc R U . . . C91 C 0.4603(7) 0.5844(3) 0.9297(3) 0.0445(15) Uani 1 1 d . . . . . H91 H 0.4824 0.5517 0.9105 0.053 Uiso 1 1 calc R U . . . C93 C 0.3246(7) 0.6309(3) 0.9940(3) 0.0518(17) Uani 1 1 d . . . . . H93 H 0.2572 0.6296 1.0180 0.062 Uiso 1 1 calc R U . . . C71 C 0.6694(8) 0.3734(3) 0.6047(3) 0.0498(17) Uani 1 1 d . . . . . H71 H 0.6476 0.3357 0.6105 0.060 Uiso 1 1 calc R U . . . C92 C 0.3572(7) 0.5831(3) 0.9651(3) 0.0511(16) Uani 1 1 d . . . . . H92 H 0.3106 0.5496 0.9690 0.061 Uiso 1 1 calc R U . . . C65 C 0.8590(7) 0.6039(3) 0.4167(3) 0.0494(16) Uani 1 1 d . . . . . H65 H 0.8734 0.6175 0.3805 0.059 Uiso 1 1 calc R U . . . C78 C 1.2074(7) 0.4956(3) 0.8445(3) 0.0550(18) Uani 1 1 d . . . . . H78A H 1.2835 0.5196 0.8448 0.083 Uiso 1 1 calc R U . . . H78B H 1.2224 0.4612 0.8241 0.083 Uiso 1 1 calc R U . . . H78C H 1.1915 0.4866 0.8833 0.083 Uiso 1 1 calc R U . . . C1S C 0.5333(7) 0.4147(3) 0.7981(3) 0.0582(18) Uiso 1 1 d . . . . . C64 C 0.9238(7) 0.6283(3) 0.4656(3) 0.0535(17) Uani 1 1 d . . . . . H64 H 0.9831 0.6579 0.4623 0.064 Uiso 1 1 calc R U . . . C89 C 0.8010(10) 0.5779(3) 0.9513(3) 0.077(2) Uani 1 1 d . U . . . H89 H 0.8084 0.6092 0.9756 0.092 Uiso 1 1 calc R U . . . C87 C 0.8657(10) 0.4827(3) 0.9304(4) 0.075(2) Uani 1 1 d . U . . . H87 H 0.9143 0.4502 0.9404 0.091 Uiso 1 1 calc R U . . . C88 C 0.8644(11) 0.5277(4) 0.9684(4) 0.088(2) Uani 1 1 d . U . . . H88 H 0.9061 0.5243 1.0055 0.106 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 O1 0.044(2) 0.031(2) 0.043(2) -0.0051(17) -0.0013(18) 0.0028(17) N1 0.040(3) 0.028(2) 0.032(3) -0.0027(19) -0.0014(19) 0.0020(19) C8 0.033(3) 0.024(2) 0.031(3) -0.002(2) 0.002(2) -0.001(2) C75 0.036(3) 0.030(3) 0.035(3) -0.001(2) 0.004(2) -0.002(2) C3 0.029(3) 0.026(3) 0.034(3) -0.003(2) 0.001(2) -0.002(2) C6 0.029(3) 0.028(3) 0.037(3) -0.003(2) 0.010(2) 0.001(2) C26 0.037(3) 0.023(2) 0.032(3) -0.001(2) 0.006(2) -0.003(2) C10 0.036(3) 0.025(2) 0.029(3) 0.003(2) 0.009(2) 0.002(2) C25 0.036(3) 0.020(2) 0.034(3) 0.000(2) 0.007(2) 0.000(2) C20 0.036(3) 0.033(3) 0.033(3) 0.001(2) 0.012(2) -0.001(2) C29 0.037(3) 0.034(3) 0.030(3) 0.001(2) 0.008(2) 0.000(2) C9 0.036(3) 0.024(2) 0.028(3) -0.002(2) 0.007(2) 0.000(2) C21 0.039(3) 0.034(3) 0.029(3) -0.001(2) 0.011(2) 0.002(2) C44 0.031(3) 0.031(3) 0.039(3) -0.008(2) 0.001(2) -0.007(2) C74 0.034(3) 0.028(3) 0.032(3) -0.001(2) 0.004(2) -0.003(2) C4 0.027(3) 0.027(3) 0.038(3) -0.001(2) 0.001(2) -0.001(2) C5 0.028(3) 0.027(3) 0.036(3) -0.001(2) 0.003(2) -0.002(2) C33 0.044(3) 0.025(3) 0.039(3) -0.008(2) 0.000(2) 0.004(2) C11 0.040(3) 0.028(3) 0.027(3) 0.000(2) 0.004(2) -0.002(2) C80 0.038(3) 0.027(3) 0.038(3) -0.003(2) 0.001(2) 0.000(2) C13 0.043(3) 0.030(3) 0.025(3) -0.004(2) 0.000(2) 0.003(2) C51 0.045(3) 0.029(3) 0.045(4) -0.004(2) 0.003(3) 0.006(2) C35 0.043(3) 0.022(3) 0.046(3) -0.003(2) 0.001(3) 0.002(2) C30 0.044(3) 0.037(3) 0.026(3) -0.004(2) 0.012(2) -0.002(2) C2 0.035(3) 0.025(3) 0.032(3) -0.001(2) 0.001(2) -0.001(2) C36 0.044(3) 0.022(3) 0.047(4) 0.005(2) 0.005(3) 0.000(2) C62 0.039(3) 0.034(3) 0.032(3) -0.003(2) 0.007(2) 0.001(2) C15 0.038(3) 0.029(3) 0.034(3) -0.005(2) -0.001(2) -0.004(2) C1 0.032(3) 0.026(3) 0.033(3) -0.002(2) 0.003(2) -0.004(2) C45 0.030(3) 0.033(3) 0.042(3) -0.004(2) 0.002(2) -0.006(2) C7 0.033(3) 0.031(3) 0.026(3) -0.002(2) 0.004(2) -0.001(2) C58 0.029(3) 0.042(3) 0.042(3) -0.009(3) 0.001(2) -0.001(2) C69 0.051(3) 0.031(3) 0.033(3) -0.002(2) 0.007(2) 0.000(2) C68 0.052(3) 0.031(3) 0.027(3) -0.002(2) 0.008(2) 0.008(3) C17 0.039(3) 0.024(3) 0.050(4) 0.001(2) 0.004(3) -0.009(2) C22 0.040(3) 0.033(3) 0.027(3) -0.003(2) 0.003(2) 0.003(2) C24 0.037(3) 0.028(3) 0.036(3) -0.006(2) 0.001(2) -0.002(2) C14 0.038(3) 0.033(3) 0.033(3) -0.009(2) 0.000(2) 0.002(2) C28 0.034(3) 0.035(3) 0.039(3) -0.002(2) 0.012(2) -0.008(2) C46 0.027(3) 0.040(3) 0.047(4) -0.006(3) 0.004(2) -0.003(2) C85 0.044(3) 0.033(3) 0.034(3) 0.001(2) 0.007(2) 0.001(2) C42 0.045(3) 0.035(3) 0.026(3) -0.006(2) -0.001(2) 0.004(2) C52 0.047(3) 0.032(3) 0.042(3) 0.000(2) -0.005(3) 0.009(3) C47 0.026(3) 0.046(3) 0.041(3) -0.003(3) 0.007(2) 0.000(2) C41 0.045(3) 0.039(3) 0.030(3) -0.002(2) 0.000(2) 0.004(3) C38 0.045(3) 0.027(3) 0.041(3) 0.010(2) 0.010(3) -0.002(2) C37 0.051(4) 0.024(3) 0.045(4) 0.006(2) 0.005(3) -0.005(2) C40 0.046(3) 0.037(3) 0.029(3) 0.003(2) 0.006(2) 0.003(2) C55 0.048(3) 0.036(3) 0.034(3) 0.001(2) -0.005(2) 0.008(3) C12 0.042(3) 0.028(3) 0.030(3) -0.003(2) 0.006(2) -0.003(2) C16 0.045(3) 0.022(3) 0.040(3) -0.006(2) 0.001(2) -0.005(2) C49 0.041(3) 0.041(3) 0.038(3) -0.006(3) 0.008(2) 0.007(3) C19 0.035(3) 0.034(3) 0.039(3) 0.006(2) 0.012(2) -0.007(2) C18 0.037(3) 0.031(3) 0.040(3) 0.001(2) 0.010(2) -0.007(2) C32 0.042(3) 0.036(3) 0.035(3) -0.009(2) 0.005(2) 0.007(2) C23 0.043(3) 0.035(3) 0.025(3) -0.007(2) 0.003(2) -0.005(2) C90 0.047(3) 0.034(3) 0.032(3) 0.000(2) 0.008(2) 0.003(2) C79 0.041(3) 0.031(3) 0.052(4) -0.002(3) -0.005(3) 0.001(2) C53 0.046(3) 0.029(3) 0.043(3) 0.004(2) 0.001(3) 0.002(2) C27 0.035(3) 0.029(3) 0.040(3) -0.003(2) 0.010(2) -0.008(2) C59 0.031(3) 0.039(3) 0.047(4) -0.005(3) 0.002(2) 0.007(2) C57 0.032(3) 0.040(3) 0.040(3) -0.007(2) -0.004(2) 0.003(2) C61 0.039(3) 0.032(3) 0.032(3) -0.006(2) 0.003(2) 0.001(2) C84 0.059(3) 0.035(3) 0.032(3) -0.003(2) 0.002(2) 0.004(3) C31 0.037(3) 0.038(3) 0.035(3) -0.009(2) 0.009(2) 0.001(2) C34 0.048(3) 0.022(3) 0.042(3) -0.005(2) 0.002(3) -0.001(2) C83 0.049(3) 0.028(3) 0.030(3) -0.003(2) 0.006(2) 0.003(2) C67 0.051(4) 0.042(3) 0.036(3) -0.006(3) 0.008(3) -0.015(3) C76 0.037(3) 0.028(3) 0.049(4) 0.000(2) 0.008(2) 0.002(2) C81 0.040(3) 0.029(3) 0.035(3) -0.003(2) 0.002(2) -0.002(2) C48 0.031(3) 0.046(3) 0.037(3) -0.006(3) 0.011(2) 0.004(2) C73 0.050(4) 0.036(3) 0.040(3) -0.003(2) 0.004(3) 0.012(3) C50 0.041(3) 0.032(3) 0.040(3) -0.007(2) 0.001(2) 0.011(2) C95 0.060(4) 0.043(3) 0.035(3) -0.001(3) 0.012(3) 0.003(3) C60 0.043(3) 0.036(3) 0.042(3) 0.000(2) -0.004(3) 0.008(3) C39 0.051(3) 0.034(3) 0.032(3) 0.007(2) 0.009(2) -0.002(3) C54 0.056(4) 0.030(3) 0.037(3) 0.013(2) 0.003(3) 0.009(3) C86 0.055(3) 0.038(3) 0.041(3) -0.003(2) 0.001(3) 0.005(3) C43 0.035(3) 0.038(3) 0.039(3) -0.008(2) -0.001(2) -0.001(2) C77 0.036(3) 0.031(3) 0.053(4) 0.000(3) 0.001(3) -0.002(2) C82 0.045(3) 0.041(3) 0.046(4) -0.009(3) -0.004(3) -0.002(3) C56 0.047(3) 0.041(3) 0.034(3) -0.003(2) -0.005(3) 0.007(3) C72 0.069(5) 0.038(3) 0.040(4) 0.000(3) 0.004(3) 0.012(3) C70 0.058(4) 0.034(3) 0.041(4) -0.007(3) 0.012(3) 0.001(3) C66 0.058(4) 0.045(4) 0.040(4) -0.003(3) 0.006(3) -0.007(3) C94 0.060(4) 0.052(4) 0.042(4) -0.005(3) 0.015(3) 0.012(3) C63 0.045(3) 0.052(4) 0.045(4) -0.011(3) 0.012(3) -0.012(3) C91 0.058(4) 0.039(3) 0.039(3) -0.004(3) 0.017(3) 0.000(3) C93 0.054(4) 0.064(4) 0.040(4) 0.002(3) 0.017(3) 0.007(3) C71 0.083(5) 0.031(3) 0.036(4) -0.002(2) 0.010(3) 0.001(3) C92 0.062(4) 0.052(4) 0.043(4) 0.001(3) 0.022(3) -0.007(3) C65 0.061(4) 0.045(4) 0.044(4) 0.001(3) 0.019(3) -0.003(3) C78 0.052(4) 0.036(3) 0.073(5) -0.005(3) -0.016(3) 0.011(3) C64 0.062(4) 0.050(4) 0.052(4) -0.007(3) 0.026(3) -0.014(3) C89 0.114(5) 0.055(4) 0.055(4) -0.019(3) -0.027(4) 0.030(4) C87 0.104(5) 0.053(4) 0.064(4) -0.008(3) -0.023(4) 0.031(4) C88 0.124(6) 0.067(4) 0.064(4) -0.016(4) -0.037(4) 0.037(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C81 N1 C80 127.6(5) . . ? C81 N1 C2 120.6(4) . . ? C80 N1 C2 111.1(4) . . ? C9 C8 C25 107.2(5) . . ? C9 C8 C7 125.2(5) . . ? C25 C8 C7 122.1(5) . . ? C74 C75 C76 119.1(5) . . ? C15 C3 C4 119.8(5) . . ? C15 C3 C2 125.3(5) . . ? C4 C3 C2 111.3(4) . . ? C5 C6 C20 119.9(5) . . ? C5 C6 C7 123.0(5) . . ? C20 C6 C7 110.9(5) . . ? C27 C26 C25 121.3(5) . . ? C27 C26 C10 120.7(5) . . ? C25 C26 C10 106.3(4) . . ? C11 C10 C26 121.5(5) . . ? C11 C10 C9 121.9(5) . . ? C26 C10 C9 107.1(4) . . ? C24 C25 C26 119.1(5) . . ? C24 C25 C8 121.6(5) . . ? C26 C25 C8 109.0(5) . . ? C19 C20 C6 121.4(5) . . ? C19 C20 C21 120.0(5) . . ? C6 C20 C21 108.8(5) . . ? C28 C29 C11 121.6(5) . . ? C28 C29 C30 119.7(5) . . ? C11 C29 C30 108.0(5) . . ? C8 C9 C10 110.5(5) . . ? C8 C9 C1 124.4(5) . . ? C10 C9 C1 121.9(5) . . ? C40 C21 C22 121.2(5) . . ? C40 C21 C20 120.0(5) . . ? C22 C21 C20 108.7(5) . . ? C45 C44 C43 120.2(5) . . ? C45 C44 C24 120.5(5) . . ? C43 C44 C24 107.8(5) . . ? C75 C74 C80 120.6(5) . . ? C75 C74 C1 127.9(5) . . ? C80 C74 C1 111.4(5) . . ? C18 C4 C5 121.0(5) . . ? C18 C4 C3 120.6(5) . . ? C5 C4 C3 109.6(5) . . ? C6 C5 C4 119.5(5) . . ? C6 C5 C1 124.1(5) . . ? C4 C5 C1 110.7(5) . . ? C32 C33 C34 119.7(5) . . ? C32 C33 C14 120.4(5) . . ? C34 C33 C14 108.8(5) . . ? C10 C11 C29 117.9(5) . . ? C10 C11 C12 125.7(5) . . ? C29 C11 C12 111.1(5) . . ? C79 C80 C74 119.8(5) . . ? C79 C80 N1 130.1(5) . . ? C74 C80 N1 109.9(5) . . ? C14 C13 C30 118.5(5) . . ? C14 C13 C12 125.1(5) . . ? C30 C13 C12 110.6(5) . . ? C50 C51 C52 120.8(6) . . ? C50 C51 C35 119.9(5) . . ? C52 C51 C35 107.7(5) . . ? C34 C35 C51 119.9(6) . . ? C34 C35 C36 119.9(5) . . ? C51 C35 C36 108.0(5) . . ? C31 C30 C13 122.0(5) . . ? C31 C30 C29 120.2(5) . . ? C13 C30 C29 107.7(5) . . ? N1 C2 C3 107.2(4) . . ? N1 C2 C1 102.0(4) . . ? C3 C2 C1 103.1(4) . . ? N1 C2 C12 113.0(4) . . ? C3 C2 C12 113.3(4) . . ? C1 C2 C12 117.1(4) . . ? C37 C36 C53 120.0(5) . . ? C37 C36 C35 120.3(5) . . ? C53 C36 C35 107.7(5) . . ? C63 C62 C67 118.4(5) . . ? C63 C62 C61 119.3(5) . . ? C67 C62 C61 122.3(5) . . ? C3 C15 C16 120.6(5) . . ? C3 C15 C14 119.5(5) . . ? C16 C15 C14 108.3(5) . . ? C74 C1 C9 113.5(4) . . ? C74 C1 C5 114.4(4) . . ? C9 C1 C5 105.4(4) . . ? C74 C1 C2 103.8(4) . . ? C9 C1 C2 116.2(4) . . ? C5 C1 C2 103.5(4) . . ? C44 C45 C27 119.0(5) . . ? C44 C45 C46 119.9(5) . . ? C27 C45 C46 107.7(5) . . ? C8 C7 C6 106.6(4) . . ? C8 C7 C22 108.7(4) . . ? C6 C7 C22 99.0(4) . . ? C8 C7 C61 116.2(4) . . ? C6 C7 C61 110.2(4) . . ? C22 C7 C61 114.6(4) . . ? C46 C58 C57 120.3(5) . . ? C46 C58 C59 120.2(5) . . ? C57 C58 C59 107.0(5) . . ? C68 C69 C70 120.5(6) . . ? C69 C68 C73 118.4(5) . . ? C69 C68 C61 123.4(5) . . ? C73 C68 C61 118.2(5) . . ? C16 C17 C18 119.0(5) . . ? C16 C17 C37 120.3(5) . . ? C18 C17 C37 107.7(5) . . ? C23 C22 C21 119.4(5) . . ? C23 C22 C7 123.2(5) . . ? C21 C22 C7 109.7(5) . . ? C25 C24 C44 120.2(5) . . ? C25 C24 C23 118.6(5) . . ? C44 C24 C23 108.3(5) . . ? C13 C14 C33 120.8(5) . . ? C13 C14 C15 120.3(5) . . ? C33 C14 C15 106.7(5) . . ? C29 C28 C27 119.3(5) . . ? C29 C28 C47 119.9(5) . . ? C27 C28 C47 108.3(5) . . ? C58 C46 C47 119.8(5) . . ? C58 C46 C45 120.0(5) . . ? C47 C46 C45 108.2(5) . . ? C86 C85 C84 121.6(6) . . ? C41 C42 C23 120.3(5) . . ? C41 C42 C43 120.3(5) . . ? C23 C42 C43 108.8(5) . . ? C60 C52 C51 119.3(6) . . ? C60 C52 C53 120.0(5) . . ? C51 C52 C53 108.6(5) . . ? C48 C47 C46 120.6(6) . . ? C48 C47 C28 119.8(5) . . ? C46 C47 C28 107.2(5) . . ? C42 C41 C40 119.2(5) . . ? C42 C41 C55 119.8(6) . . ? C40 C41 C55 108.0(5) . . ? C39 C38 C37 120.1(5) . . ? C39 C38 C19 119.6(5) . . ? C37 C38 C19 107.8(5) . . ? C36 C37 C38 120.1(6) . . ? C36 C37 C17 119.4(6) . . ? C38 C37 C17 108.0(5) . . ? C21 C40 C41 119.4(5) . . ? C21 C40 C39 119.9(5) . . ? C41 C40 C39 107.8(5) . . ? C56 C55 C54 119.8(5) . . ? C56 C55 C41 119.7(5) . . ? C54 C55 C41 108.5(5) . . ? C11 C12 C13 97.9(4) . . ? C11 C12 C83 110.7(4) . . ? C13 C12 C83 107.9(4) . . ? C11 C12 C2 114.2(4) . . ? C13 C12 C2 112.7(4) . . ? C83 C12 C2 112.5(4) . . ? C17 C16 C15 120.5(5) . . ? C17 C16 C34 120.0(5) . . ? C15 C16 C34 108.5(5) . . ? C59 C49 C50 119.9(6) . . ? C59 C49 C48 119.8(5) . . ? C50 C49 C48 107.9(5) . . ? C20 C19 C18 118.8(5) . . ? C20 C19 C38 120.4(5) . . ? C18 C19 C38 108.3(5) . . ? C4 C18 C19 119.1(5) . . ? C4 C18 C17 119.5(5) . . ? C19 C18 C17 108.1(5) . . ? C33 C32 C31 118.9(5) . . ? C33 C32 C50 119.9(6) . . ? C31 C32 C50 108.6(5) . . ? C22 C23 C42 120.4(5) . . ? C22 C23 C24 121.6(5) . . ? C42 C23 C24 106.6(5) . . ? C95 C90 C91 118.3(6) . . ? C95 C90 C83 119.4(5) . . ? C91 C90 C83 122.2(5) . . ? C80 C79 C77 119.9(6) . . ? C54 C53 C52 119.9(6) . . ? C54 C53 C36 119.9(6) . . ? C52 C53 C36 108.0(5) . . ? C26 C27 C28 118.9(5) . . ? C26 C27 C45 119.9(5) . . ? C28 C27 C45 108.5(5) . . ? C49 C59 C60 120.3(6) . . ? C49 C59 C58 119.8(6) . . ? C60 C59 C58 108.0(5) . . ? C43 C57 C56 119.9(6) . . ? C43 C57 C58 119.3(5) . . ? C56 C57 C58 108.7(5) . . ? C62 C61 C68 114.2(4) . . ? C62 C61 C7 111.7(4) . . ? C68 C61 C7 114.3(5) . . ? C89 C84 C85 117.8(6) . . ? C89 C84 C83 115.7(5) . . ? C85 C84 C83 126.2(5) . . ? C30 C31 C32 119.3(5) . . ? C30 C31 C48 120.2(5) . . ? C32 C31 C48 108.0(5) . . ? C35 C34 C33 120.7(5) . . ? C35 C34 C16 120.1(5) . . ? C33 C34 C16 107.7(5) . . ? C90 C83 C84 108.5(5) . . ? C90 C83 C12 113.7(5) . . ? C84 C83 C12 117.5(4) . . ? C62 C67 C66 121.3(6) . . ? C75 C76 C77 120.8(5) . . ? O1 C81 N1 119.3(5) . . ? O1 C81 C82 120.4(5) . . ? N1 C81 C82 120.3(5) . . ? C47 C48 C31 120.1(5) . . ? C47 C48 C49 119.9(5) . . ? C31 C48 C49 107.8(5) . . ? C72 C73 C68 120.0(6) . . ? C51 C50 C49 119.7(5) . . ? C51 C50 C32 119.9(5) . . ? C49 C50 C32 107.8(5) . . ? C94 C95 C90 120.8(6) . . ? C52 C60 C56 120.1(6) . . ? C52 C60 C59 119.9(6) . . ? C56 C60 C59 108.2(5) . . ? C38 C39 C54 119.9(6) . . ? C38 C39 C40 120.1(5) . . ? C54 C39 C40 108.5(5) . . ? C53 C54 C39 120.1(6) . . ? C53 C54 C55 120.4(6) . . ? C39 C54 C55 107.2(5) . . ? C87 C86 C85 119.9(6) . . ? C57 C43 C44 120.3(5) . . ? C57 C43 C42 119.9(5) . . ? C44 C43 C42 108.5(5) . . ? C76 C77 C79 119.7(5) . . ? C76 C77 C78 120.7(5) . . ? C79 C77 C78 119.6(6) . . ? C55 C56 C57 120.4(5) . . ? C55 C56 C60 119.8(6) . . ? C57 C56 C60 108.2(5) . . ? C71 C72 C73 121.1(6) . . ? C71 C70 C69 120.1(6) . . ? C65 C66 C67 119.7(6) . . ? C93 C94 C95 120.1(6) . . ? C62 C63 C64 121.0(6) . . ? C92 C91 C90 120.3(6) . . ? C92 C93 C94 120.2(6) . . ? C72 C71 C70 119.8(6) . . ? C93 C92 C91 120.4(6) . . ? C66 C65 C64 120.0(6) . . ? S2 C1S S1 178.0(6) . . ? C65 C64 C63 119.5(6) . . ? C84 C89 C88 121.1(7) . . ? C86 C87 C88 119.1(7) . . ? C87 C88 C89 120.1(7) . . ? 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 S2 C1S 1.525(8) . ? S1 C1S 1.551(8) . ? O1 C81 1.233(7) . ? N1 C81 1.372(7) . ? N1 C80 1.430(7) . ? N1 C2 1.512(7) . ? C8 C9 1.357(7) . ? C8 C25 1.467(7) . ? C8 C7 1.515(7) . ? C75 C74 1.380(8) . ? C75 C76 1.385(8) . ? C3 C15 1.373(8) . ? C3 C4 1.423(8) . ? C3 C2 1.527(7) . ? C6 C5 1.384(8) . ? C6 C20 1.414(8) . ? C6 C7 1.542(7) . ? C26 C27 1.384(8) . ? C26 C25 1.436(7) . ? C26 C10 1.442(8) . ? C10 C11 1.365(7) . ? C10 C9 1.463(7) . ? C25 C24 1.378(8) . ? C20 C19 1.399(8) . ? C20 C21 1.446(8) . ? C29 C28 1.405(8) . ? C29 C11 1.441(8) . ? C29 C30 1.445(8) . ? C9 C1 1.518(7) . ? C21 C40 1.395(8) . ? C21 C22 1.429(8) . ? C44 C45 1.387(8) . ? C44 C43 1.441(8) . ? C44 C24 1.450(8) . ? C74 C80 1.395(8) . ? C74 C1 1.504(7) . ? C4 C18 1.402(8) . ? C4 C5 1.422(7) . ? C5 C1 1.543(7) . ? C33 C32 1.396(8) . ? C33 C34 1.443(8) . ? C33 C14 1.451(8) . ? C11 C12 1.529(7) . ? C80 C79 1.379(8) . ? C13 C14 1.363(8) . ? C13 C30 1.438(8) . ? C13 C12 1.558(7) . ? C51 C50 1.388(9) . ? C51 C52 1.445(9) . ? C51 C35 1.456(8) . ? C35 C34 1.385(8) . ? C35 C36 1.458(9) . ? C30 C31 1.385(8) . ? C2 C1 1.616(7) . ? C2 C12 1.622(8) . ? C36 C37 1.389(9) . ? C36 C53 1.452(8) . ? C62 C63 1.377(8) . ? C62 C67 1.386(8) . ? C62 C61 1.514(8) . ? C15 C16 1.432(8) . ? C15 C14 1.467(8) . ? C45 C27 1.445(8) . ? C45 C46 1.454(8) . ? C7 C22 1.562(7) . ? C7 C61 1.590(7) . ? C58 C46 1.390(9) . ? C58 C57 1.450(8) . ? C58 C59 1.456(8) . ? C69 C68 1.391(9) . ? C69 C70 1.397(8) . ? C68 C73 1.400(8) . ? C68 C61 1.522(8) . ? C17 C16 1.392(8) . ? C17 C18 1.444(8) . ? C17 C37 1.453(8) . ? C22 C23 1.367(8) . ? C24 C23 1.478(8) . ? C28 C27 1.438(8) . ? C28 C47 1.460(8) . ? C46 C47 1.452(8) . ? C85 C86 1.380(8) . ? C85 C84 1.383(8) . ? C42 C41 1.393(8) . ? C42 C23 1.446(8) . ? C42 C43 1.450(8) . ? C52 C60 1.405(9) . ? C52 C53 1.448(9) . ? C47 C48 1.379(8) . ? C41 C40 1.436(8) . ? C41 C55 1.452(8) . ? C38 C39 1.397(9) . ? C38 C37 1.441(8) . ? C38 C19 1.446(8) . ? C40 C39 1.457(8) . ? C55 C56 1.406(9) . ? C55 C54 1.448(9) . ? C12 C83 1.590(8) . ? C16 C34 1.446(8) . ? C49 C59 1.392(8) . ? C49 C50 1.450(9) . ? C49 C48 1.464(9) . ? C19 C18 1.437(8) . ? C32 C31 1.442(8) . ? C32 C50 1.460(8) . ? C90 C95 1.400(8) . ? C90 C91 1.400(8) . ? C90 C83 1.518(8) . ? C79 C77 1.392(8) . ? C53 C54 1.388(9) . ? C59 C60 1.444(9) . ? C57 C43 1.403(8) . ? C57 C56 1.434(9) . ? C84 C89 1.367(9) . ? C84 C83 1.534(8) . ? C31 C48 1.460(8) . ? C67 C66 1.392(9) . ? C76 C77 1.387(8) . ? C81 C82 1.499(8) . ? C73 C72 1.398(9) . ? C95 C94 1.390(9) . ? C60 C56 1.440(8) . ? C39 C54 1.446(9) . ? C86 C87 1.369(10) . ? C77 C78 1.520(8) . ? C72 C71 1.354(10) . ? C70 C71 1.390(9) . ? C66 C65 1.374(9) . ? C94 C93 1.381(10) . ? C63 C64 1.399(9) . ? C91 C92 1.400(9) . ? C93 C92 1.372(10) . ? C65 C64 1.388(10) . ? C89 C88 1.387(11) . ? C87 C88 1.383(11) . ?