#------------------------------------------------------------------------------ #$Date: 2021-12-07 05:42:17 +0200 (Tue, 07 Dec 2021) $ #$Revision: 271204 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061029.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_7061029 loop_ _publ_author_name 'Dekhtiarenko, Maksym' 'Allain, Magali' 'Carr\'e, Vincent' 'Aubriet, Fr\'ed\'eric' 'Voitenko, Zoia' 'Sall\'e, Marc' 'Goeb, S\'ebastien' _publ_section_title ; Comparing the self-assembly processes of two redox-active exTTF-based regioisomer ligands ; _journal_issue 45 _journal_name_full 'New Journal of Chemistry' _journal_page_first 21015 _journal_page_last 21019 _journal_paper_doi 10.1039/D1NJ04555E _journal_volume 45 _journal_year 2021 _chemical_formula_moiety 'C44 H32 N4 S8' _chemical_formula_sum 'C44 H32 N4 S8' _chemical_formula_weight 873.21 _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2018-06-14T11:50:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2021-09-13 deposited with the CCDC. 2021-10-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.8500(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.6654(2) _cell_length_b 14.8503(2) _cell_length_c 20.1186(3) _cell_measurement_reflns_used 11855 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 76.227 _cell_measurement_theta_min 2.919 _cell_volume 4077.72(10) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_molecular_graphics 'DIAMOND 3.2k (Crystal Impact GbR, 2014)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2016/4 (Sheldrick, 2016)' _computing_structure_solution 'SHELXS-2013/1 (Sheldrick, 2013)' _diffrn_ambient_temperature 150.00(10) _diffrn_detector_area_resol_mean 5.199 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_device_type 'SuperNova, Single source at offset, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_unetI/netI 0.0288 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 17395 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 75 _diffrn_reflns_theta_max 76.421 _diffrn_reflns_theta_min 3.238 _exptl_absorpt_coefficient_mu 4.358 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.4944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.422 _exptl_crystal_description prism _exptl_crystal_F_000 1808 _exptl_crystal_size_max 0.371 _exptl_crystal_size_mid 0.223 _exptl_crystal_size_min 0.201 _refine_diff_density_max 0.789 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.071 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 509 _refine_ls_number_reflns 8328 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+4.5311P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1314 _refine_ls_wR_factor_ref 0.1359 _reflns_Friedel_coverage 0 _reflns_number_gt 7702 _reflns_number_total 8328 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj04555e2.cif _cod_data_source_block md054 _cod_depositor_comments 'Adding full bibliography for 7061029.cif.' _cod_original_cell_volume 4077.70(10) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7061029 _shelx_res_file ; TITL MD054 in P2(1)/c shelx.res created by SHELXL-2016/4 at 10:29:27 on 14-Jun-2018 CELL 1.54184 13.6654 14.8503 20.1186 90.000 92.850 90.000 ZERR 4.00 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N S UNIT 176 128 16 32 MERG 2 OMIT 14 8 5 OMIT 11 12 8 OMIT -10 9 16 OMIT -14 9 6 OMIT 10 13 7 OMIT 11 12 7 OMIT -9 9 17 OMIT 10 13 8 FMAP 2 PLAN 20 ACTA 150 BOND $H L.S. 4 WGHT 0.069800 4.531100 FVAR 2.74308 C1 1 0.336087 0.430414 0.989559 11.00000 0.03165 0.02139 = 0.02192 0.00248 0.00175 0.00299 C2 1 0.478346 0.369584 1.070553 11.00000 0.03479 0.04351 = 0.03174 0.00124 -0.00675 0.00990 C3 1 0.461145 0.453022 1.091900 11.00000 0.02999 0.04186 = 0.02908 -0.00120 -0.00336 0.00351 C4 1 0.627207 0.251183 1.046422 11.00000 0.04497 0.04006 = 0.09588 0.02162 0.02063 0.01473 AFIX 137 H4A 2 0.587281 0.212172 1.018351 11.00000 -1.50000 H4B 2 0.682533 0.218197 1.064885 11.00000 -1.50000 H4C 2 0.649698 0.300790 1.020661 11.00000 -1.50000 AFIX 0 C5 1 0.420343 0.520808 1.213685 11.00000 0.08241 0.10285 = 0.03695 -0.01742 0.01900 -0.04033 AFIX 137 H5A 2 0.372411 0.559892 1.192388 11.00000 -1.50000 H5B 2 0.444006 0.547123 1.255004 11.00000 -1.50000 H5C 2 0.390977 0.463477 1.222141 11.00000 -1.50000 AFIX 0 C6 1 0.265300 0.440619 0.940540 11.00000 0.02716 0.02054 = 0.01986 0.00281 0.00350 0.00134 C7 1 0.242279 0.371655 0.889440 11.00000 0.02210 0.02146 = 0.02146 0.00038 0.00166 0.00277 C8 1 0.234296 0.280461 0.904796 11.00000 0.02537 0.02337 = 0.02131 0.00219 0.00178 0.00247 AFIX 43 H8 2 0.242338 0.262578 0.949032 11.00000 -1.20000 AFIX 0 C9 1 0.214671 0.215131 0.856135 11.00000 0.02278 0.02216 = 0.02516 0.00079 0.00369 0.00248 C10 1 0.200517 0.242836 0.789619 11.00000 0.02230 0.02271 = 0.02394 -0.00163 0.00388 0.00086 C11 1 0.203658 0.334705 0.774687 11.00000 0.02351 0.02660 = 0.01944 0.00109 0.00408 0.00097 AFIX 43 H11 2 0.191567 0.352879 0.730809 11.00000 -1.20000 AFIX 0 C12 1 0.224235 0.400093 0.823103 11.00000 0.02075 0.02140 = 0.02190 0.00182 0.00399 0.00060 C13 1 0.226585 0.497424 0.808803 11.00000 0.02306 0.02251 = 0.02139 0.00259 -0.00113 -0.00023 C14 1 0.192991 0.555002 0.863068 11.00000 0.02304 0.02072 = 0.02251 0.00229 0.00108 -0.00069 C15 1 0.141436 0.635080 0.852460 11.00000 0.02736 0.02261 = 0.02406 0.00479 -0.00195 0.00024 AFIX 43 H15 2 0.129152 0.654866 0.808986 11.00000 -1.20000 AFIX 0 C16 1 0.107423 0.686892 0.904565 11.00000 0.02538 0.02006 = 0.02740 0.00250 -0.00231 0.00213 C17 1 0.124618 0.656133 0.970459 11.00000 0.02492 0.02074 = 0.02597 0.00125 0.00076 0.00162 C18 1 0.173805 0.575019 0.981263 11.00000 0.02628 0.02230 = 0.02164 0.00354 0.00080 0.00236 AFIX 43 H18 2 0.182468 0.553297 1.024512 11.00000 -1.20000 AFIX 0 C19 1 0.210426 0.525405 0.929381 11.00000 0.02297 0.01842 = 0.02391 0.00262 -0.00004 0.00172 C20 1 0.264898 0.531991 0.753169 11.00000 0.02710 0.02798 = 0.02228 0.00431 -0.00089 -0.00268 C21 1 0.373547 0.549819 0.649921 11.00000 0.03683 0.05351 = 0.03094 0.00877 0.00755 -0.01160 C22 1 0.360071 0.633834 0.672240 11.00000 0.04529 0.04901 = 0.03464 0.01459 0.00334 -0.01493 C23 1 0.390797 0.421469 0.550763 11.00000 0.06046 0.07324 = 0.04471 -0.00376 0.02459 0.00181 AFIX 137 H23A 2 0.389536 0.374577 0.583555 11.00000 -1.50000 H23B 2 0.425831 0.400909 0.513453 11.00000 -1.50000 H23C 2 0.324935 0.436817 0.536202 11.00000 -1.50000 AFIX 0 C24 1 0.520415 0.742568 0.694533 11.00000 0.04697 0.04353 = 0.14656 0.01606 0.01176 -0.01207 AFIX 137 H24A 2 0.501720 0.746069 0.739830 11.00000 -1.50000 H24B 2 0.555409 0.796155 0.683519 11.00000 -1.50000 H24C 2 0.561710 0.691017 0.689280 11.00000 -1.50000 AFIX 0 C25 1 0.213088 0.119915 0.878654 11.00000 0.02780 0.02105 = 0.02536 0.00093 -0.00116 0.00058 C26 1 0.277648 0.056260 0.855564 11.00000 0.03603 0.02687 = 0.04143 0.00166 0.01179 0.00410 AFIX 43 H26 2 0.318895 0.070894 0.821784 11.00000 -1.20000 AFIX 0 C27 1 0.280168 -0.029151 0.883196 11.00000 0.04134 0.02384 = 0.05260 0.00143 0.00875 0.00804 AFIX 43 H27 2 0.324969 -0.070208 0.867544 11.00000 -1.20000 AFIX 0 C28 1 0.158013 0.004477 0.951218 11.00000 0.04042 0.02927 = 0.03503 0.00651 0.00526 -0.00188 AFIX 43 H28 2 0.115138 -0.013034 0.983293 11.00000 -1.20000 AFIX 0 C29 1 0.151399 0.091807 0.927414 11.00000 0.03374 0.02586 = 0.03079 0.00258 0.00367 0.00277 AFIX 43 H29 2 0.105900 0.131460 0.943973 11.00000 -1.20000 AFIX 0 C30 1 0.177855 0.179741 0.733676 11.00000 0.03196 0.02383 = 0.02257 -0.00098 0.00245 0.00562 C31 1 0.228813 0.186368 0.675523 11.00000 0.04433 0.03077 = 0.03139 -0.00135 0.01203 0.00507 AFIX 43 H31 2 0.279199 0.228017 0.672396 11.00000 -1.20000 AFIX 0 C32 1 0.203581 0.130375 0.622657 11.00000 0.06442 0.03866 = 0.03037 -0.00531 0.01386 0.01253 AFIX 43 H32 2 0.237835 0.136489 0.584110 11.00000 -1.20000 AFIX 0 C33 1 0.084768 0.062286 0.679110 11.00000 0.04709 0.02939 = 0.03661 -0.00667 -0.00403 0.00142 AFIX 43 H33 2 0.035328 0.019442 0.680872 11.00000 -1.20000 AFIX 0 C34 1 0.103326 0.116070 0.734748 11.00000 0.03272 0.02796 = 0.02803 -0.00289 0.00120 0.00125 AFIX 43 H34 2 0.066528 0.109630 0.772119 11.00000 -1.20000 AFIX 0 C35 1 0.096418 0.705862 1.031059 11.00000 0.02331 0.02328 = 0.02573 0.00288 0.00064 0.00737 C36 1 0.045007 0.662674 1.079787 11.00000 0.02933 0.02859 = 0.03621 0.00268 0.00768 0.00306 AFIX 43 H36 2 0.024274 0.603457 1.073756 11.00000 -1.20000 AFIX 0 C37 1 0.025037 0.708760 1.137334 11.00000 0.03457 0.03859 = 0.03575 0.00451 0.01269 0.00662 AFIX 43 H37 2 -0.009657 0.678761 1.169216 11.00000 -1.20000 AFIX 0 C38 1 0.102770 0.834694 1.102986 11.00000 0.03371 0.02826 = 0.03333 -0.00365 -0.00099 0.00453 AFIX 43 H38 2 0.123256 0.893658 1.110707 11.00000 -1.20000 AFIX 0 C39 1 0.126003 0.794550 1.043711 11.00000 0.02881 0.02296 = 0.02805 0.00227 0.00030 0.00328 AFIX 43 H39 2 0.160825 0.826170 1.012731 11.00000 -1.20000 AFIX 0 C40 1 0.050286 0.769530 0.887208 11.00000 0.03730 0.02089 = 0.02746 -0.00264 -0.01088 0.00382 C41 1 -0.033866 0.793356 0.918881 11.00000 0.03859 0.03510 = 0.03438 -0.00466 -0.00979 0.01234 AFIX 43 H41 2 -0.056703 0.757520 0.952709 11.00000 -1.20000 AFIX 0 C42 1 -0.083648 0.871481 0.899424 11.00000 0.05230 0.04419 = 0.04079 -0.01469 -0.01792 0.02445 AFIX 43 H42 2 -0.139847 0.886188 0.921304 11.00000 -1.20000 AFIX 0 C43 1 0.023007 0.902651 0.821153 11.00000 0.07437 0.02676 = 0.04387 0.00718 -0.02112 -0.00025 AFIX 43 H43 2 0.043579 0.940054 0.787498 11.00000 -1.20000 AFIX 0 C44 1 0.077699 0.825458 0.835968 11.00000 0.05049 0.02584 = 0.03838 0.00507 -0.00915 0.00118 AFIX 43 H44 2 0.131981 0.811487 0.811832 11.00000 -1.20000 AFIX 0 N1 3 0.222358 -0.056311 0.930888 11.00000 0.04155 0.02448 = 0.04184 0.00534 -0.00091 0.00080 N2 3 0.133216 0.067986 0.623201 11.00000 0.06963 0.03488 = 0.03219 -0.01211 0.00189 0.00884 N3 3 0.052504 0.793750 1.149984 11.00000 0.03773 0.04120 = 0.03188 -0.00428 0.00667 0.00984 N4 3 -0.056487 0.926102 0.852019 11.00000 0.07278 0.03141 = 0.04744 -0.00942 -0.02648 0.01782 S1 4 0.409900 0.333102 0.999708 11.00000 0.03685 0.03078 = 0.03156 -0.00263 -0.00774 0.01095 S2 4 0.370946 0.515296 1.047440 11.00000 0.03451 0.02654 = 0.02999 -0.00091 -0.00554 0.00117 S3 4 0.557370 0.292451 1.111613 11.00000 0.07782 0.07230 = 0.04570 -0.00777 -0.02602 0.04274 S4 4 0.520033 0.505808 1.160751 11.00000 0.03959 0.05657 = 0.03962 -0.01208 -0.01121 0.00315 S5 4 0.314034 0.463920 0.691091 11.00000 0.03796 0.03814 = 0.02862 -0.00065 0.01350 -0.00797 S6 4 0.283471 0.647280 0.738513 11.00000 0.04044 0.02902 = 0.02996 0.00977 -0.00095 -0.00616 S7 4 0.451162 0.519486 0.586654 11.00000 0.05440 0.08699 = 0.05211 0.00023 0.03042 -0.02000 S8 4 0.411550 0.732098 0.639661 11.00000 0.08227 0.05768 = 0.05919 0.02506 0.01395 -0.02569 HKLF 4 REM MD054 in P2(1)/c REM R1 = 0.0490 for 7702 Fo > 4sig(Fo) and 0.0538 for all 8328 data REM 509 parameters refined using 0 restraints END WGHT 0.0698 4.5310 REM Highest difference peak 0.789, deepest hole -0.702, 1-sigma level 0.071 Q1 1 0.4610 0.6910 0.6354 11.00000 0.05 0.79 Q2 1 0.4009 0.5369 0.5625 11.00000 0.05 0.77 Q3 1 0.5179 0.2209 1.1553 11.00000 0.05 0.66 Q4 1 0.4767 0.5616 0.6061 11.00000 0.05 0.59 Q5 1 0.2819 0.4159 0.9880 11.00000 0.05 0.50 Q6 1 0.4147 0.7634 0.6728 11.00000 0.05 0.45 Q7 1 0.5176 0.2520 1.0914 11.00000 0.05 0.41 Q8 1 0.2722 0.6200 1.1925 11.00000 0.05 0.41 Q9 1 0.3980 0.5904 0.6736 11.00000 0.05 0.40 Q10 1 0.4499 0.3236 1.0446 11.00000 0.05 0.39 Q11 1 0.1035 0.6809 1.0004 11.00000 0.05 0.39 Q12 1 0.1928 0.2050 0.7640 11.00000 0.05 0.35 Q13 1 0.3336 0.7858 0.6537 11.00000 0.05 0.35 Q14 1 0.4614 0.4595 1.2061 11.00000 0.05 0.35 Q15 1 0.1216 0.6562 0.8805 11.00000 0.05 0.35 Q16 1 0.2078 0.2293 0.8246 11.00000 0.05 0.35 Q17 1 0.2545 0.4062 0.9175 11.00000 0.05 0.34 Q18 1 0.3635 0.7290 0.6163 11.00000 0.05 0.34 Q19 1 0.4759 0.4604 0.5844 11.00000 0.05 0.33 Q20 1 0.2249 0.3616 0.7995 11.00000 0.05 0.33 ; _shelx_res_checksum 25225 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_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 C1 C 0.33609(17) 0.43041(15) 0.98956(11) 0.0250(4) Uani 1 1 d . . . . . C2 C 0.47835(19) 0.3696(2) 1.07055(13) 0.0370(6) Uani 1 1 d . . . . . C3 C 0.46115(18) 0.45302(19) 1.09190(12) 0.0338(5) Uani 1 1 d . . . . . C4 C 0.6272(2) 0.2512(2) 1.0464(2) 0.0597(10) Uani 1 1 d . . . . . H4A H 0.587281 0.212172 1.018351 0.09 Uiso 1 1 calc R U . . . H4B H 0.682533 0.218197 1.064885 0.09 Uiso 1 1 calc R U . . . H4C H 0.649698 0.30079 1.020661 0.09 Uiso 1 1 calc R U . . . C5 C 0.4203(3) 0.5208(3) 1.21368(17) 0.0735(13) Uani 1 1 d . . . . . H5A H 0.372411 0.559892 1.192388 0.11 Uiso 1 1 calc R U . . . H5B H 0.444006 0.547123 1.255004 0.11 Uiso 1 1 calc R U . . . H5C H 0.390977 0.463477 1.222141 0.11 Uiso 1 1 calc R U . . . C6 C 0.26530(16) 0.44062(14) 0.94054(10) 0.0224(4) Uani 1 1 d . . . . . C7 C 0.24228(15) 0.37166(14) 0.88944(10) 0.0217(4) Uani 1 1 d . . . . . C8 C 0.23430(16) 0.28046(15) 0.90480(11) 0.0233(4) Uani 1 1 d . . . . . H8 H 0.242338 0.262578 0.949032 0.028 Uiso 1 1 calc R U . . . C9 C 0.21467(16) 0.21513(15) 0.85613(11) 0.0233(4) Uani 1 1 d . . . . . C10 C 0.20052(15) 0.24284(15) 0.78962(11) 0.0229(4) Uani 1 1 d . . . . . C11 C 0.20366(15) 0.33471(15) 0.77469(11) 0.0231(4) Uani 1 1 d . . . . . H11 H 0.191567 0.352879 0.730809 0.028 Uiso 1 1 calc R U . . . C12 C 0.22424(15) 0.40009(14) 0.82310(10) 0.0213(4) Uani 1 1 d . . . . . C13 C 0.22659(16) 0.49742(15) 0.80880(11) 0.0224(4) Uani 1 1 d . . . . . C14 C 0.19299(15) 0.55500(14) 0.86307(11) 0.0221(4) Uani 1 1 d . . . . . C15 C 0.14144(16) 0.63508(15) 0.85246(11) 0.0248(4) Uani 1 1 d . . . . . H15 H 0.129152 0.654866 0.808986 0.03 Uiso 1 1 calc R U . . . C16 C 0.10742(16) 0.68689(15) 0.90457(11) 0.0244(4) Uani 1 1 d . . . . . C17 C 0.12462(16) 0.65613(15) 0.97046(11) 0.0239(4) Uani 1 1 d . . . . . C18 C 0.17380(16) 0.57502(15) 0.98126(11) 0.0234(4) Uani 1 1 d . . . . . H18 H 0.182468 0.553297 1.024512 0.028 Uiso 1 1 calc R U . . . C19 C 0.21043(15) 0.52540(14) 0.92938(11) 0.0218(4) Uani 1 1 d . . . . . C20 C 0.26490(16) 0.53199(16) 0.75317(11) 0.0259(4) Uani 1 1 d . . . . . C21 C 0.3735(2) 0.5498(2) 0.64992(13) 0.0402(6) Uani 1 1 d . . . . . C22 C 0.3601(2) 0.6338(2) 0.67224(14) 0.0429(6) Uani 1 1 d . . . . . C23 C 0.3908(3) 0.4215(3) 0.55076(17) 0.0587(9) Uani 1 1 d . . . . . H23A H 0.389536 0.374577 0.583555 0.088 Uiso 1 1 calc R U . . . H23B H 0.425831 0.400909 0.513453 0.088 Uiso 1 1 calc R U . . . H23C H 0.324935 0.436817 0.536202 0.088 Uiso 1 1 calc R U . . . C24 C 0.5204(3) 0.7426(3) 0.6945(3) 0.0788(14) Uani 1 1 d . . . . . H24A H 0.50172 0.746069 0.73983 0.118 Uiso 1 1 calc R U . . . H24B H 0.555409 0.796155 0.683519 0.118 Uiso 1 1 calc R U . . . H24C H 0.56171 0.691017 0.68928 0.118 Uiso 1 1 calc R U . . . C25 C 0.21309(16) 0.11992(15) 0.87865(11) 0.0248(4) Uani 1 1 d . . . . . C26 C 0.27765(19) 0.05626(17) 0.85556(14) 0.0344(5) Uani 1 1 d . . . . . H26 H 0.318895 0.070894 0.821784 0.041 Uiso 1 1 calc R U . . . C27 C 0.2802(2) -0.02915(17) 0.88320(15) 0.0390(6) Uani 1 1 d . . . . . H27 H 0.324969 -0.070208 0.867544 0.047 Uiso 1 1 calc R U . . . C28 C 0.1580(2) 0.00448(17) 0.95122(13) 0.0348(5) Uani 1 1 d . . . . . H28 H 0.115138 -0.013034 0.983293 0.042 Uiso 1 1 calc R U . . . C29 C 0.15140(18) 0.09181(16) 0.92741(12) 0.0301(5) Uani 1 1 d . . . . . H29 H 0.1059 0.13146 0.943973 0.036 Uiso 1 1 calc R U . . . C30 C 0.17785(17) 0.17974(15) 0.73368(11) 0.0261(4) Uani 1 1 d . . . . . C31 C 0.2288(2) 0.18637(18) 0.67552(13) 0.0352(5) Uani 1 1 d . . . . . H31 H 0.279199 0.228017 0.672396 0.042 Uiso 1 1 calc R U . . . C32 C 0.2036(2) 0.1304(2) 0.62266(14) 0.0441(7) Uani 1 1 d . . . . . H32 H 0.237835 0.136489 0.58411 0.053 Uiso 1 1 calc R U . . . C33 C 0.0848(2) 0.06229(18) 0.67911(13) 0.0379(6) Uani 1 1 d . . . . . H33 H 0.035328 0.019442 0.680872 0.045 Uiso 1 1 calc R U . . . C34 C 0.10333(18) 0.11607(16) 0.73475(12) 0.0296(5) Uani 1 1 d . . . . . H34 H 0.066528 0.10963 0.772119 0.035 Uiso 1 1 calc R U . . . C35 C 0.09642(16) 0.70586(15) 1.03106(11) 0.0241(4) Uani 1 1 d . . . . . C36 C 0.04501(18) 0.66267(17) 1.07979(13) 0.0312(5) Uani 1 1 d . . . . . H36 H 0.024274 0.603457 1.073756 0.037 Uiso 1 1 calc R U . . . C37 C 0.02504(19) 0.70876(19) 1.13733(13) 0.0359(6) Uani 1 1 d . . . . . H37 H -0.009657 0.678761 1.169216 0.043 Uiso 1 1 calc R U . . . C38 C 0.10277(18) 0.83469(17) 1.10299(13) 0.0319(5) Uani 1 1 d . . . . . H38 H 0.123256 0.893658 1.110707 0.038 Uiso 1 1 calc R U . . . C39 C 0.12600(17) 0.79455(15) 1.04371(12) 0.0266(4) Uani 1 1 d . . . . . H39 H 0.160825 0.82617 1.012731 0.032 Uiso 1 1 calc R U . . . C40 C 0.05029(18) 0.76953(15) 0.88721(12) 0.0290(5) Uani 1 1 d . . . . . C41 C -0.0339(2) 0.79336(18) 0.91888(13) 0.0364(6) Uani 1 1 d . . . . . H41 H -0.056703 0.75752 0.952709 0.044 Uiso 1 1 calc R U . . . C42 C -0.0836(2) 0.8715(2) 0.89942(15) 0.0464(7) Uani 1 1 d . . . . . H42 H -0.139847 0.886188 0.921304 0.056 Uiso 1 1 calc R U . . . C43 C 0.0230(3) 0.90265(19) 0.82115(16) 0.0491(8) Uani 1 1 d . . . . . H43 H 0.043579 0.940054 0.787498 0.059 Uiso 1 1 calc R U . . . C44 C 0.0777(2) 0.82546(17) 0.83597(14) 0.0386(6) Uani 1 1 d . . . . . H44 H 0.131981 0.811487 0.811832 0.046 Uiso 1 1 calc R U . . . N1 N 0.22236(17) -0.05631(14) 0.93089(12) 0.0361(5) Uani 1 1 d . . . . . N2 N 0.1332(2) 0.06799(16) 0.62320(12) 0.0456(6) Uani 1 1 d . . . . . N3 N 0.05250(17) 0.79375(16) 1.14998(11) 0.0368(5) Uani 1 1 d . . . . . N4 N -0.0565(2) 0.92610(17) 0.85202(13) 0.0515(7) Uani 1 1 d . . . . . S1 S 0.40990(5) 0.33310(4) 0.99971(3) 0.03338(15) Uani 1 1 d . . . . . S2 S 0.37095(4) 0.51530(4) 1.04744(3) 0.03058(14) Uani 1 1 d . . . . . S3 S 0.55737(8) 0.29245(7) 1.11161(4) 0.0662(3) Uani 1 1 d . . . . . S4 S 0.52003(5) 0.50581(6) 1.16075(4) 0.04570(18) Uani 1 1 d . . . . . S5 S 0.31403(5) 0.46392(4) 0.69109(3) 0.03451(15) Uani 1 1 d . . . . . S6 S 0.28347(5) 0.64728(4) 0.73851(3) 0.03323(15) Uani 1 1 d . . . . . S7 S 0.45116(7) 0.51949(8) 0.58665(5) 0.0636(3) Uani 1 1 d . . . . . S8 S 0.41155(8) 0.73210(7) 0.63966(5) 0.0660(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0316(11) 0.0214(10) 0.0219(10) 0.0025(8) 0.0017(8) 0.0030(8) C2 0.0348(13) 0.0435(14) 0.0317(12) 0.0012(11) -0.0068(10) 0.0099(11) C3 0.0300(12) 0.0419(14) 0.0291(12) -0.0012(10) -0.0034(9) 0.0035(10) C4 0.0450(17) 0.0401(16) 0.096(3) 0.0216(17) 0.0206(17) 0.0147(13) C5 0.082(3) 0.103(3) 0.0369(16) -0.0174(19) 0.0190(17) -0.040(2) C6 0.0272(10) 0.0205(10) 0.0199(9) 0.0028(8) 0.0035(8) 0.0013(8) C7 0.0221(9) 0.0215(10) 0.0215(10) 0.0004(8) 0.0017(7) 0.0028(8) C8 0.0254(10) 0.0234(10) 0.0213(10) 0.0022(8) 0.0018(8) 0.0025(8) C9 0.0228(10) 0.0222(10) 0.0252(10) 0.0008(8) 0.0037(8) 0.0025(8) C10 0.0223(10) 0.0227(10) 0.0239(10) -0.0016(8) 0.0039(8) 0.0009(8) C11 0.0235(10) 0.0266(11) 0.0194(9) 0.0011(8) 0.0041(8) 0.0010(8) C12 0.0208(9) 0.0214(10) 0.0219(10) 0.0018(8) 0.0040(7) 0.0006(8) C13 0.0231(10) 0.0225(10) 0.0214(10) 0.0026(8) -0.0011(8) -0.0002(8) C14 0.0230(10) 0.0207(10) 0.0225(10) 0.0023(8) 0.0011(8) -0.0007(8) C15 0.0274(10) 0.0226(10) 0.0241(10) 0.0048(8) -0.0019(8) 0.0002(8) C16 0.0254(10) 0.0201(10) 0.0274(11) 0.0025(8) -0.0023(8) 0.0021(8) C17 0.0249(10) 0.0207(10) 0.0260(10) 0.0012(8) 0.0008(8) 0.0016(8) C18 0.0263(10) 0.0223(10) 0.0216(10) 0.0035(8) 0.0008(8) 0.0024(8) C19 0.0230(10) 0.0184(10) 0.0239(10) 0.0026(8) 0.0000(8) 0.0017(8) C20 0.0271(11) 0.0280(11) 0.0223(10) 0.0043(8) -0.0009(8) -0.0027(9) C21 0.0368(13) 0.0535(17) 0.0309(12) 0.0088(12) 0.0076(10) -0.0116(12) C22 0.0453(15) 0.0490(16) 0.0346(13) 0.0146(12) 0.0033(11) -0.0149(13) C23 0.060(2) 0.073(2) 0.0447(17) -0.0038(16) 0.0246(15) 0.0018(17) C24 0.0470(19) 0.0435(19) 0.147(4) 0.016(2) 0.012(2) -0.0121(15) C25 0.0278(10) 0.0210(10) 0.0254(10) 0.0009(8) -0.0012(8) 0.0006(8) C26 0.0360(13) 0.0269(12) 0.0414(14) 0.0017(10) 0.0118(11) 0.0041(10) C27 0.0413(14) 0.0238(12) 0.0526(16) 0.0014(11) 0.0087(12) 0.0080(10) C28 0.0404(13) 0.0293(12) 0.0350(13) 0.0065(10) 0.0053(10) -0.0019(10) C29 0.0337(12) 0.0259(11) 0.0308(12) 0.0026(9) 0.0037(9) 0.0028(9) C30 0.0320(11) 0.0238(10) 0.0226(10) -0.0010(8) 0.0025(8) 0.0056(9) C31 0.0443(14) 0.0308(12) 0.0314(12) -0.0014(10) 0.0120(10) 0.0051(11) C32 0.0644(19) 0.0387(14) 0.0304(13) -0.0053(11) 0.0139(12) 0.0125(13) C33 0.0471(15) 0.0294(12) 0.0366(13) -0.0067(10) -0.0040(11) 0.0014(11) C34 0.0327(12) 0.0280(11) 0.0280(11) -0.0029(9) 0.0012(9) 0.0013(9) C35 0.0233(10) 0.0233(10) 0.0257(10) 0.0029(8) 0.0006(8) 0.0074(8) C36 0.0293(11) 0.0286(11) 0.0362(13) 0.0027(10) 0.0077(10) 0.0031(9) C37 0.0346(13) 0.0386(14) 0.0357(13) 0.0045(11) 0.0127(10) 0.0066(11) C38 0.0337(12) 0.0283(11) 0.0333(12) -0.0037(9) -0.0010(10) 0.0045(9) C39 0.0288(11) 0.0230(10) 0.0280(11) 0.0023(9) 0.0003(9) 0.0033(9) C40 0.0373(12) 0.0209(10) 0.0275(11) -0.0026(8) -0.0109(9) 0.0038(9) C41 0.0386(13) 0.0351(13) 0.0344(13) -0.0047(10) -0.0098(10) 0.0123(11) C42 0.0523(17) 0.0442(16) 0.0408(15) -0.0147(13) -0.0179(13) 0.0245(13) C43 0.074(2) 0.0268(13) 0.0439(15) 0.0072(11) -0.0211(15) -0.0002(14) C44 0.0505(15) 0.0258(12) 0.0384(14) 0.0051(10) -0.0092(11) 0.0012(11) N1 0.0415(12) 0.0245(10) 0.0418(12) 0.0053(9) -0.0009(9) 0.0008(9) N2 0.0696(17) 0.0349(12) 0.0322(11) -0.0121(9) 0.0019(11) 0.0088(11) N3 0.0377(11) 0.0412(12) 0.0319(11) -0.0043(9) 0.0067(9) 0.0098(9) N4 0.0728(18) 0.0314(12) 0.0474(14) -0.0094(11) -0.0265(13) 0.0178(12) S1 0.0368(3) 0.0308(3) 0.0316(3) -0.0026(2) -0.0077(2) 0.0110(2) S2 0.0345(3) 0.0265(3) 0.0300(3) -0.0009(2) -0.0055(2) 0.0012(2) S3 0.0778(6) 0.0723(6) 0.0457(4) -0.0078(4) -0.0260(4) 0.0427(5) S4 0.0396(4) 0.0566(4) 0.0396(4) -0.0121(3) -0.0112(3) 0.0031(3) S5 0.0380(3) 0.0381(3) 0.0286(3) -0.0007(2) 0.0135(2) -0.0080(3) S6 0.0404(3) 0.0290(3) 0.0300(3) 0.0098(2) -0.0010(2) -0.0062(2) S7 0.0544(5) 0.0870(7) 0.0521(5) 0.0002(4) 0.0304(4) -0.0200(4) S8 0.0823(6) 0.0577(5) 0.0592(5) 0.0251(4) 0.0140(4) -0.0257(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C6 C1 S2 124.03(17) . . ? C6 C1 S1 123.91(18) . . ? S2 C1 S1 111.94(12) . . ? C3 C2 S1 116.9(2) . . ? C3 C2 S3 124.7(2) . . ? S1 C2 S3 118.23(16) . . ? C2 C3 S2 117.1(2) . . ? C2 C3 S4 126.0(2) . . ? S2 C3 S4 116.85(16) . . ? S3 C4 H4A 109.5 . . ? S3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S4 C5 H5A 109.5 . . ? S4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C1 C6 C7 123.4(2) . . ? C1 C6 C19 123.0(2) . . ? C7 C6 C19 113.40(18) . . ? C8 C7 C12 119.3(2) . . ? C8 C7 C6 122.45(19) . . ? C12 C7 C6 118.25(19) . . ? C7 C8 C9 122.3(2) . . ? C7 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? C8 C9 C10 118.5(2) . . ? C8 C9 C25 116.95(19) . . ? C10 C9 C25 124.5(2) . . ? C11 C10 C9 119.1(2) . . ? C11 C10 C30 117.40(19) . . ? C9 C10 C30 123.4(2) . . ? C12 C11 C10 122.5(2) . . ? C12 C11 H11 118.8 . . ? C10 C11 H11 118.8 . . ? C11 C12 C7 118.2(2) . . ? C11 C12 C13 123.51(19) . . ? C7 C12 C13 118.29(19) . . ? C20 C13 C12 122.9(2) . . ? C20 C13 C14 122.4(2) . . ? C12 C13 C14 114.36(18) . . ? C15 C14 C19 118.0(2) . . ? C15 C14 C13 123.64(19) . . ? C19 C14 C13 118.25(19) . . ? C14 C15 C16 122.6(2) . . ? C14 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C15 C16 C17 118.7(2) . . ? C15 C16 C40 117.9(2) . . ? C17 C16 C40 123.3(2) . . ? C18 C17 C16 118.9(2) . . ? C18 C17 C35 116.31(19) . . ? C16 C17 C35 124.7(2) . . ? C19 C18 C17 122.0(2) . . ? C19 C18 H18 119 . . ? C17 C18 H18 119 . . ? C18 C19 C14 119.57(19) . . ? C18 C19 C6 122.44(19) . . ? C14 C19 C6 117.97(19) . . ? C13 C20 S6 124.79(18) . . ? C13 C20 S5 122.81(18) . . ? S6 C20 S5 112.08(12) . . ? C22 C21 S5 116.5(2) . . ? C22 C21 S7 125.4(2) . . ? S5 C21 S7 118.00(19) . . ? C21 C22 S6 117.3(2) . . ? C21 C22 S8 125.6(2) . . ? S6 C22 S8 117.07(19) . . ? S7 C23 H23A 109.5 . . ? S7 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? S7 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? S8 C24 H24A 109.5 . . ? S8 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S8 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C29 116.7(2) . . ? C26 C25 C9 121.8(2) . . ? C29 C25 C9 121.3(2) . . ? C27 C26 C25 119.5(2) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? N1 C27 C26 124.2(2) . . ? N1 C27 H27 117.9 . . ? C26 C27 H27 117.9 . . ? N1 C28 C29 124.0(2) . . ? N1 C28 H28 118 . . ? C29 C28 H28 118 . . ? C28 C29 C25 119.6(2) . . ? C28 C29 H29 120.2 . . ? C25 C29 H29 120.2 . . ? C34 C30 C31 117.2(2) . . ? C34 C30 C10 122.9(2) . . ? C31 C30 C10 119.8(2) . . ? C32 C31 C30 119.2(3) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? N2 C32 C31 124.3(3) . . ? N2 C32 H32 117.8 . . ? C31 C32 H32 117.8 . . ? N2 C33 C34 124.3(3) . . ? N2 C33 H33 117.8 . . ? C34 C33 H33 117.8 . . ? C33 C34 C30 118.9(2) . . ? C33 C34 H34 120.6 . . ? C30 C34 H34 120.6 . . ? C36 C35 C39 117.3(2) . . ? C36 C35 C17 120.5(2) . . ? C39 C35 C17 122.1(2) . . ? C37 C36 C35 119.3(2) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? N3 C37 C36 124.1(2) . . ? N3 C37 H37 117.9 . . ? C36 C37 H37 117.9 . . ? N3 C38 C39 124.0(2) . . ? N3 C38 H38 118 . . ? C39 C38 H38 118 . . ? C38 C39 C35 119.1(2) . . ? C38 C39 H39 120.5 . . ? C35 C39 H39 120.5 . . ? C41 C40 C44 116.6(2) . . ? C41 C40 C16 122.7(2) . . ? C44 C40 C16 120.6(2) . . ? C40 C41 C42 119.2(3) . . ? C40 C41 H41 120.4 . . ? C42 C41 H41 120.4 . . ? N4 C42 C41 124.4(3) . . ? N4 C42 H42 117.8 . . ? C41 C42 H42 117.8 . . ? N4 C43 C44 124.1(3) . . ? N4 C43 H43 118 . . ? C44 C43 H43 118 . . ? C40 C44 C43 119.3(3) . . ? C40 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C27 N1 C28 115.9(2) . . ? C32 N2 C33 116.0(2) . . ? C37 N3 C38 116.2(2) . . ? C42 N4 C43 116.4(2) . . ? C2 S1 C1 96.87(12) . . ? C3 S2 C1 96.89(12) . . ? C2 S3 C4 102.67(15) . . ? C3 S4 C5 101.15(16) . . ? C21 S5 C20 96.89(13) . . ? C22 S6 C20 96.53(13) . . ? C21 S7 C23 102.49(14) . . ? C22 S8 C24 100.09(17) . . ? 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 C1 C6 1.355(3) . ? C1 S2 1.765(2) . ? C1 S1 1.768(2) . ? C2 C3 1.336(4) . ? C2 S1 1.751(3) . ? C2 S3 1.753(3) . ? C3 S2 1.751(3) . ? C3 S4 1.752(3) . ? C4 S3 1.769(4) . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 S4 1.784(4) . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? C6 C7 1.474(3) . ? C6 C19 1.477(3) . ? C7 C8 1.395(3) . ? C7 C12 1.410(3) . ? C8 C9 1.395(3) . ? C8 H8 0.93 . ? C9 C10 1.404(3) . ? C9 C25 1.485(3) . ? C10 C11 1.398(3) . ? C10 C30 1.485(3) . ? C11 C12 1.394(3) . ? C11 H11 0.93 . ? C12 C13 1.474(3) . ? C13 C20 1.360(3) . ? C13 C14 1.478(3) . ? C14 C15 1.393(3) . ? C14 C19 1.414(3) . ? C15 C16 1.398(3) . ? C15 H15 0.93 . ? C16 C17 1.411(3) . ? C16 C40 1.487(3) . ? C17 C18 1.391(3) . ? C17 C35 1.492(3) . ? C18 C19 1.391(3) . ? C18 H18 0.93 . ? C20 S6 1.758(2) . ? C20 S5 1.765(2) . ? C21 C22 1.342(5) . ? C21 S5 1.744(3) . ? C21 S7 1.756(3) . ? C22 S6 1.747(3) . ? C22 S8 1.761(3) . ? C23 S7 1.806(4) . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C24 S8 1.815(5) . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 C26 1.389(3) . ? C25 C29 1.389(3) . ? C26 C27 1.385(4) . ? C26 H26 0.93 . ? C27 N1 1.335(4) . ? C27 H27 0.93 . ? C28 N1 1.338(4) . ? C28 C29 1.384(3) . ? C28 H28 0.93 . ? C29 H29 0.93 . ? C30 C34 1.391(3) . ? C30 C31 1.394(3) . ? C31 C32 1.380(4) . ? C31 H31 0.93 . ? C32 N2 1.336(4) . ? C32 H32 0.93 . ? C33 N2 1.336(4) . ? C33 C34 1.388(3) . ? C33 H33 0.93 . ? C34 H34 0.93 . ? C35 C36 1.391(3) . ? C35 C39 1.397(3) . ? C36 C37 1.384(4) . ? C36 H36 0.93 . ? C37 N3 1.338(4) . ? C37 H37 0.93 . ? C38 N3 1.342(4) . ? C38 C39 1.384(3) . ? C38 H38 0.93 . ? C39 H39 0.93 . ? C40 C41 1.388(4) . ? C40 C44 1.390(4) . ? C41 C42 1.391(4) . ? C41 H41 0.93 . ? C42 N4 1.319(5) . ? C42 H42 0.93 . ? C43 N4 1.324(5) . ? C43 C44 1.393(4) . ? C43 H43 0.93 . ? C44 H44 0.93 . ?