#------------------------------------------------------------------------------ #$Date: 2018-02-14 06:19:12 +0200 (Wed, 14 Feb 2018) $ #$Revision: 206409 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/01/7230148.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_7230148 loop_ _publ_author_name 'Song, Xiaoxian' 'Yu, Hanbo' 'Zhang, Yuewei' 'Miao, Yang' 'Ye, Kaiqi' 'Wang, Yue' _publ_section_title ; Regulatable morphology and self-assembly of one-dimensional luminescent crystals based on alkyl-fluoro-substituted dithienophenazines ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C8CE00021B _journal_year 2018 _chemical_formula_sum 'C32 H37 F2 N2 S2' _chemical_formula_weight 551.75 _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' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-12-20 deposited with the CCDC. 2018-02-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.8960(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.89080(10) _cell_length_b 37.3867(9) _cell_length_c 15.8515(4) _cell_measurement_reflns_used 9968 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 21.51 _cell_measurement_theta_min 2.22 _cell_volume 2883.13(12) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.951 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measurement_device_type MX300 _diffrn_radiation_wavelength 0.6229 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_unetI/netI 0.0612 _diffrn_reflns_Laue_measured_fraction_full 0.951 _diffrn_reflns_Laue_measured_fraction_max 0.951 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 34697 _diffrn_reflns_point_group_measured_fraction_full 0.952 _diffrn_reflns_point_group_measured_fraction_max 0.952 _diffrn_reflns_theta_full 24.738 _diffrn_reflns_theta_max 24.738 _diffrn_reflns_theta_min 1.291 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 0.156 _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.271 _exptl_crystal_description needle _exptl_crystal_F_000 1172 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.428 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.051 _refine_ls_abs_structure_details ; Flack x determined using 4229 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.42(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 689 _refine_ls_number_reflns 9384 _refine_ls_number_restraints 525 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0498 _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^)+(0.0611P)^2^+2.0248P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1352 _refine_ls_wR_factor_ref 0.1363 _reflns_Friedel_coverage 0.969 _reflns_Friedel_fraction_full 0.953 _reflns_Friedel_fraction_max 0.953 _reflns_number_gt 9012 _reflns_number_total 9384 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8ce00021b2.cif _cod_data_source_block 1_a _cod_database_code 7230148 _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_res_file ; 1_a.res created by SHELXL-2014/7 TITL 1_a.res in P2(1) CELL 0.71073 4.8908 37.3867 15.8515 90.000 95.896 90.000 ZERR 4 0.0001 0.0009 0.0004 0.000 0.001 0.000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H N F S UNIT 128 148 8 8 8 omit 2 -2 1 omit -3 10 9 delu 0.01 0.005 C63 C64 DFIX 1.4 0.008 C64 C65 L.S. 20 ACTA BOND $H FMAP 2 PLAN 20 LIST 6 isor C60 0.008 ISOR C64 0.008 ISOR C65 0.008 SIMU WGHT 0.061100 2.024800 FVAR 0.85396 C1 1 1.378831 0.842494 0.469407 11.00000 0.12326 0.03832 = 0.08472 -0.00777 0.04823 -0.00345 AFIX 137 H1A 2 1.483989 0.863656 0.461120 11.00000 -1.50000 H1AB 2 1.336382 0.841514 0.527161 11.00000 -1.50000 H1AC 2 1.211292 0.843050 0.432126 11.00000 -1.50000 AFIX 0 C2 1 1.542945 0.810031 0.450331 11.00000 0.09496 0.03364 = 0.07251 -0.00149 0.02995 -0.00750 AFIX 23 H2A 2 1.710142 0.809480 0.488944 11.00000 -1.20000 H2AB 2 1.595482 0.812054 0.393159 11.00000 -1.20000 AFIX 0 C3 1 1.389959 0.775258 0.458010 11.00000 0.06520 0.03593 = 0.05784 0.00046 0.01528 0.00364 AFIX 23 H3A 2 1.223363 0.775856 0.419139 11.00000 -1.20000 H3AB 2 1.335909 0.773452 0.515045 11.00000 -1.20000 AFIX 0 C4 1 1.552193 0.742111 0.439726 11.00000 0.06059 0.03024 = 0.06340 -0.00282 0.01530 -0.00357 AFIX 23 H4A 2 1.718343 0.741325 0.478770 11.00000 -1.20000 H4AB 2 1.606617 0.743819 0.382720 11.00000 -1.20000 AFIX 0 C5 1 1.392026 0.707214 0.447637 11.00000 0.04948 0.03254 = 0.05928 -0.00105 0.01257 -0.00522 AFIX 23 H5A 2 1.339080 0.705332 0.504788 11.00000 -1.20000 H5AB 2 1.225177 0.708010 0.408899 11.00000 -1.20000 AFIX 0 C6 1 1.557033 0.674074 0.428332 11.00000 0.05199 0.02549 = 0.05530 -0.00308 0.00876 -0.00386 AFIX 23 H6A 2 1.617252 0.676520 0.372191 11.00000 -1.20000 H6AB 2 1.719737 0.672746 0.468721 11.00000 -1.20000 AFIX 0 C7 1 1.396534 0.639582 0.432091 11.00000 0.04553 0.03082 = 0.04619 0.00250 0.00680 -0.00207 AFIX 23 H7A 2 1.248861 0.639167 0.386306 11.00000 -1.20000 H7AB 2 1.315249 0.638405 0.485323 11.00000 -1.20000 AFIX 0 C8 1 1.583885 0.607044 0.424516 11.00000 0.04104 0.02816 = 0.04526 0.00081 -0.00319 -0.00132 AFIX 23 H8A 2 1.653616 0.607624 0.369414 11.00000 -1.20000 H8AB 2 1.740046 0.608951 0.467246 11.00000 -1.20000 AFIX 0 C9 1 1.446014 0.571782 0.434687 11.00000 0.04409 0.02464 = 0.04128 -0.00196 0.00345 0.00094 C10 1 1.501242 0.546875 0.496510 11.00000 0.03926 0.03030 = 0.03279 -0.00192 0.00149 -0.00263 AFIX 43 H10 2 1.639893 0.549522 0.540809 11.00000 -1.20000 AFIX 0 C11 1 1.326802 0.516341 0.487070 11.00000 0.03856 0.02429 = 0.03059 -0.00268 0.00424 0.00249 C12 1 1.139085 0.518617 0.416066 11.00000 0.04008 0.02005 = 0.03136 0.00409 0.00402 0.00176 C13 1 0.946185 0.490876 0.394134 11.00000 0.03784 0.02510 = 0.02706 -0.00232 0.00174 0.00228 C14 1 0.941586 0.460732 0.444971 11.00000 0.03619 0.02372 = 0.02995 0.00010 0.00287 0.00168 C15 1 1.132573 0.457396 0.519226 11.00000 0.03825 0.02292 = 0.02672 -0.00119 0.00424 0.00183 C16 1 1.331461 0.485158 0.540640 11.00000 0.03827 0.02431 = 0.03079 -0.00103 0.00681 0.00433 C17 1 1.512796 0.452985 0.655219 11.00000 0.04448 0.03087 = 0.02527 -0.00210 0.00727 0.00470 C18 1 1.713125 0.448398 0.725616 11.00000 0.04815 0.04124 = 0.03013 -0.00141 -0.00035 0.00379 AFIX 43 H18 2 1.847620 0.465643 0.739043 11.00000 -1.20000 AFIX 0 C19 1 1.704109 0.418445 0.772658 11.00000 0.04949 0.04961 = 0.02515 0.00321 -0.00166 0.01044 C20 1 1.506896 0.391976 0.754598 11.00000 0.06687 0.03854 = 0.03185 0.01178 0.00492 0.01251 C21 1 1.312622 0.394960 0.687569 11.00000 0.05419 0.03189 = 0.03665 0.00532 0.00291 0.00423 AFIX 43 H21 2 1.180669 0.377227 0.676118 11.00000 -1.20000 AFIX 0 C22 1 1.314938 0.425806 0.635110 11.00000 0.04549 0.02876 = 0.02880 0.00061 0.00627 0.00716 C23 1 0.734344 0.435859 0.411787 11.00000 0.04072 0.02480 = 0.03155 0.00038 0.00178 -0.00442 AFIX 43 H23 2 0.699777 0.414385 0.438338 11.00000 -1.20000 AFIX 0 C24 1 0.594537 0.446605 0.338422 11.00000 0.03775 0.01896 = 0.03650 -0.00128 0.00483 0.00073 C25 1 0.369792 0.428200 0.283369 11.00000 0.03880 0.02598 = 0.03616 -0.00214 -0.00495 -0.00365 AFIX 23 H25A 2 0.425932 0.425737 0.226719 11.00000 -1.20000 H25B 2 0.206785 0.443132 0.279405 11.00000 -1.20000 AFIX 0 C26 1 0.296494 0.391289 0.315567 11.00000 0.04385 0.02530 = 0.03620 0.00040 0.00376 0.00229 AFIX 23 H26A 2 0.458755 0.376215 0.319926 11.00000 -1.20000 H26B 2 0.236563 0.393588 0.371778 11.00000 -1.20000 AFIX 0 C27 1 0.070012 0.373646 0.256858 11.00000 0.04240 0.03689 = 0.03970 -0.00707 -0.00016 -0.00487 AFIX 23 H27A 2 -0.085214 0.389883 0.249041 11.00000 -1.20000 H27B 2 0.136613 0.370112 0.201897 11.00000 -1.20000 AFIX 0 C28 1 -0.029786 0.337956 0.287661 11.00000 0.04425 0.03600 = 0.05405 -0.00345 0.00539 -0.00667 AFIX 23 H28A 2 -0.075654 0.340980 0.345331 11.00000 -1.20000 H28B 2 -0.197722 0.331615 0.252937 11.00000 -1.20000 AFIX 0 C29 1 0.169978 0.306912 0.286317 11.00000 0.04799 0.03766 = 0.05086 -0.00277 0.01022 -0.00271 AFIX 23 H29A 2 0.228501 0.304811 0.229884 11.00000 -1.20000 H29B 2 0.331426 0.311928 0.325338 11.00000 -1.20000 AFIX 0 C30 1 0.046515 0.271654 0.310527 11.00000 0.04866 0.03760 = 0.06359 -0.00336 0.00957 -0.00733 AFIX 23 H30A 2 -0.005395 0.273791 0.367749 11.00000 -1.20000 H30B 2 -0.120349 0.267566 0.273161 11.00000 -1.20000 AFIX 0 C31 1 0.226175 0.239799 0.306960 11.00000 0.05978 0.04838 = 0.06467 0.00215 0.00863 0.00036 AFIX 23 H31A 2 0.390926 0.243309 0.345639 11.00000 -1.20000 H31B 2 0.281627 0.237680 0.250151 11.00000 -1.20000 AFIX 0 C32 1 0.089372 0.205319 0.329660 11.00000 0.10888 0.03893 = 0.08791 0.00404 -0.00063 0.00519 AFIX 137 H32A 2 -0.058542 0.199861 0.287008 11.00000 -1.50000 H32B 2 0.018341 0.207963 0.383566 11.00000 -1.50000 H32C 2 0.221501 0.186253 0.332811 11.00000 -1.50000 AFIX 0 C33 1 -0.222574 0.159126 0.096832 11.00000 0.13810 0.03255 = 0.09646 0.00375 0.03698 0.00682 AFIX 137 H33A 2 -0.323120 0.137035 0.092703 11.00000 -1.50000 H33B 2 -0.124647 0.161126 0.152303 11.00000 -1.50000 H33C 2 -0.094346 0.159546 0.054874 11.00000 -1.50000 AFIX 0 C34 1 -0.418606 0.189825 0.082190 11.00000 0.08406 0.03686 = 0.09591 0.00372 0.01584 -0.00478 AFIX 23 H34A 2 -0.532676 0.190842 0.128707 11.00000 -1.20000 H34B 2 -0.538361 0.185394 0.030598 11.00000 -1.20000 AFIX 0 C35 1 -0.280817 0.225658 0.074714 11.00000 0.06982 0.03610 = 0.06367 -0.00128 0.00852 -0.00857 AFIX 23 H35A 2 -0.160767 0.224332 0.029761 11.00000 -1.20000 H35B 2 -0.167042 0.230543 0.127233 11.00000 -1.20000 AFIX 0 C36 1 -0.479587 0.256589 0.056268 11.00000 0.05841 0.03394 = 0.07374 0.00776 0.00203 -0.00663 AFIX 23 H36A 2 -0.602588 0.257527 0.100481 11.00000 -1.20000 H36B 2 -0.590292 0.251960 0.003051 11.00000 -1.20000 AFIX 0 C37 1 -0.341963 0.292821 0.050789 11.00000 0.06073 0.03449 = 0.05959 0.00433 0.00139 -0.00923 AFIX 23 H37A 2 -0.231376 0.297501 0.104001 11.00000 -1.20000 H37B 2 -0.219072 0.291932 0.006542 11.00000 -1.20000 AFIX 0 C38 1 -0.541152 0.323399 0.032436 11.00000 0.05313 0.03506 = 0.05157 0.00476 0.00074 -0.00664 AFIX 23 H38A 2 -0.664530 0.324218 0.076557 11.00000 -1.20000 H38B 2 -0.651227 0.318758 -0.020888 11.00000 -1.20000 AFIX 0 C39 1 -0.403652 0.359732 0.027278 11.00000 0.04737 0.03483 = 0.04314 0.00459 0.00013 -0.00315 AFIX 23 H39A 2 -0.284895 0.363913 0.079197 11.00000 -1.20000 H39B 2 -0.289785 0.359595 -0.019344 11.00000 -1.20000 AFIX 0 C40 1 -0.610705 0.390007 0.014292 11.00000 0.04326 0.03218 = 0.04369 0.00661 0.00721 -0.00456 AFIX 23 H40A 2 -0.734743 0.384969 -0.036052 11.00000 -1.20000 H40B 2 -0.719149 0.390503 0.062193 11.00000 -1.20000 AFIX 0 C41 1 -0.487218 0.426275 0.004929 11.00000 0.04012 0.02973 = 0.03360 0.00288 0.00609 -0.00062 C42 1 -0.382955 0.482407 -0.045531 11.00000 0.04057 0.02604 = 0.02768 0.00119 0.00587 0.00147 C43 1 -0.192939 0.480547 0.023870 11.00000 0.03866 0.02446 = 0.02926 0.00226 0.00516 0.00108 C44 1 -0.004595 0.508788 0.045944 11.00000 0.03941 0.02997 = 0.02701 0.00103 0.00102 0.00286 C45 1 -0.005303 0.539046 -0.004158 11.00000 0.03615 0.03024 = 0.03051 -0.00187 0.00161 0.00093 C46 1 -0.206135 0.542667 -0.077491 11.00000 0.03626 0.02938 = 0.02595 0.00193 0.00483 0.00322 C47 1 -0.397804 0.514112 -0.098786 11.00000 0.04122 0.02806 = 0.02077 0.00125 0.00390 0.00147 C48 1 -0.591222 0.546611 -0.211333 11.00000 0.04136 0.03008 = 0.02444 -0.00090 -0.00113 0.00308 C49 1 -0.789454 0.550497 -0.282737 11.00000 0.04494 0.03794 = 0.03131 -0.00165 -0.00046 -0.00144 AFIX 43 H49 2 -0.913540 0.532215 -0.298187 11.00000 -1.20000 AFIX 0 C50 1 -0.794762 0.581068 -0.327667 11.00000 0.04653 0.04240 = 0.03063 0.00409 -0.00484 0.00360 C51 1 -0.606674 0.608891 -0.306286 11.00000 0.06399 0.03282 = 0.03495 0.00649 0.00145 0.00021 C52 1 -0.412629 0.606017 -0.240056 11.00000 0.06195 0.03251 = 0.03570 0.00554 -0.00418 -0.00391 AFIX 43 H52 2 -0.288348 0.624531 -0.227138 11.00000 -1.20000 AFIX 0 C53 1 -0.399524 0.574466 -0.190133 11.00000 0.04582 0.03151 = 0.02444 0.00284 0.00523 0.00043 C54 1 0.197285 0.564445 0.028103 11.00000 0.04215 0.02786 = 0.03417 0.00062 0.00429 -0.00070 AFIX 43 H54 2 0.224846 0.586182 0.001734 11.00000 -1.20000 AFIX 0 C55 1 0.345289 0.553891 0.100644 11.00000 0.04087 0.03255 = 0.03489 0.00092 -0.00051 -0.00192 C56 1 0.572064 0.573171 0.153710 11.00000 0.04871 0.03944 = 0.03633 0.00002 -0.00176 -0.00116 AFIX 23 H56A 2 0.738564 0.558961 0.155820 11.00000 -1.20000 H56B 2 0.522413 0.575403 0.211168 11.00000 -1.20000 AFIX 0 C57 1 0.630021 0.610231 0.120020 11.00000 0.04617 0.03997 = 0.04144 0.00082 -0.00278 -0.00776 AFIX 23 H57A 2 0.698537 0.607931 0.064982 11.00000 -1.20000 H57B 2 0.459969 0.623748 0.112543 11.00000 -1.20000 AFIX 0 C58 1 0.838101 0.630459 0.179152 11.00000 0.06418 0.05426 = 0.03941 -0.00301 0.00234 -0.01966 AFIX 23 H58A 2 1.009055 0.617108 0.185005 11.00000 -1.20000 H58B 2 0.771917 0.631699 0.234704 11.00000 -1.20000 AFIX 0 C59 1 0.896241 0.668151 0.150222 11.00000 0.08257 0.05649 = 0.05679 -0.00241 0.01444 -0.01855 AFIX 23 H59A 2 0.982406 0.666588 0.097892 11.00000 -1.20000 H59B 2 0.722082 0.680401 0.137430 11.00000 -1.20000 AFIX 0 C60 1 1.070844 0.690022 0.210178 11.00000 0.14176 0.09066 = 0.08297 -0.02126 0.02794 -0.05337 AFIX 23 H60A 2 1.244476 0.677634 0.222840 11.00000 -1.20000 H60B 2 0.984520 0.691341 0.262515 11.00000 -1.20000 AFIX 0 C62 1 -0.554596 0.451412 -0.055851 11.00000 0.04003 0.02739 = 0.03397 0.00052 -0.00038 -0.00250 AFIX 43 H62 2 -0.696313 0.448727 -0.099205 11.00000 -1.20000 AFIX 0 C63 1 1.053724 0.793127 0.200047 11.00000 0.26187 0.09503 = 0.13133 0.00802 0.01058 -0.01437 AFIX 137 H63A 2 0.988460 0.800900 0.143845 11.00000 -1.50000 H63B 2 1.249741 0.795884 0.208787 11.00000 -1.50000 H63C 2 0.969787 0.807300 0.240824 11.00000 -1.50000 AFIX 0 C64 1 0.980307 0.754388 0.210531 11.00000 0.19308 0.14238 = 0.17260 0.05378 0.06224 0.02036 AFIX 23 H64A 2 0.968650 0.750756 0.270646 11.00000 -1.20000 H64B 2 0.795504 0.751416 0.182796 11.00000 -1.20000 AFIX 0 C65 1 1.130613 0.726669 0.184297 11.00000 0.18733 0.09254 = 0.14255 -0.02860 0.05580 -0.05439 AFIX 23 H65A 2 1.321967 0.731457 0.203325 11.00000 -1.20000 H65B 2 1.113230 0.727151 0.122796 11.00000 -1.20000 AFIX 0 N1 3 1.125534 0.427882 0.567214 11.00000 0.04640 0.02454 = 0.02969 0.00190 0.00052 0.00198 N2 3 1.517295 0.482805 0.607714 11.00000 0.04253 0.03194 = 0.02708 -0.00017 -0.00009 0.00238 N3 3 -0.584517 0.515947 -0.164958 11.00000 0.04471 0.02854 = 0.03030 0.00041 0.00237 -0.00112 N4 3 -0.208490 0.572335 -0.122732 11.00000 0.04309 0.03711 = 0.02617 0.00224 0.00067 -0.00312 F1 4 1.511321 0.363171 0.806029 11.00000 0.09325 0.05351 = 0.05001 0.02632 -0.01360 -0.00459 F2 4 1.894624 0.412470 0.839691 11.00000 0.06441 0.06387 = 0.03695 0.01094 -0.01129 0.00788 F3 4 -0.981063 0.586721 -0.394560 11.00000 0.06430 0.05818 = 0.04319 0.01599 -0.02049 -0.00357 F4 4 -0.628899 0.638511 -0.354333 11.00000 0.09806 0.04817 = 0.05466 0.02532 -0.02348 -0.00977 S1 5 0.707645 0.488423 0.307313 11.00000 0.04068 0.02456 = 0.03302 0.00336 -0.00444 -0.00017 S2 5 1.175114 0.558069 0.361882 11.00000 0.04451 0.02300 = 0.03643 0.00468 -0.00147 -0.00020 S3 5 -0.216251 0.440530 0.077233 11.00000 0.04559 0.02810 = 0.03561 0.00742 -0.00066 0.00038 S4 5 0.240971 0.511544 0.131692 11.00000 0.04333 0.03174 = 0.03329 0.00410 -0.00451 -0.00020 HKLF 4 REM 1_a.res in P2(1) REM R1 = 0.0498 for 9012 Fo > 4sig(Fo) and 0.0512 for all 9384 data REM 689 parameters refined using 525 restraints END WGHT 0.0596 2.0598 REM Highest difference peak 0.428, deepest hole -0.290, 1-sigma level 0.051 Q1 1 1.0504 0.4902 0.3029 11.00000 0.05 0.43 Q2 1 1.1628 0.7584 0.2369 11.00000 0.05 0.38 Q3 1 0.9480 0.7329 0.1661 11.00000 0.05 0.36 Q4 1 0.6118 0.5107 0.1364 11.00000 0.05 0.34 Q5 1 0.3557 0.4900 0.3069 11.00000 0.05 0.31 Q6 1 -0.5634 0.4397 0.0778 11.00000 0.05 0.31 Q7 1 1.5336 0.5601 0.3590 11.00000 0.05 0.31 Q8 1 -0.0800 0.5099 0.1355 11.00000 0.05 0.30 Q9 1 0.8363 0.5603 0.3599 11.00000 0.05 0.29 Q10 1 0.1367 0.4391 0.0840 11.00000 0.05 0.27 Q11 1 0.8631 0.6926 0.1903 11.00000 0.05 0.25 Q12 1 -0.1272 0.2427 0.3196 11.00000 0.05 0.22 Q13 1 0.2694 0.5370 0.1228 11.00000 0.05 0.22 Q14 1 -0.3210 0.2723 0.3020 11.00000 0.05 0.20 Q15 1 1.3043 0.4781 0.6650 11.00000 0.05 0.20 Q16 1 0.9907 0.8502 0.4610 11.00000 0.05 0.20 Q17 1 0.9998 0.6083 0.1199 11.00000 0.05 0.20 Q18 1 -0.8299 0.6092 -0.2495 11.00000 0.05 0.18 Q19 1 0.8443 0.4495 0.4443 11.00000 0.05 0.18 Q20 1 -0.3212 0.4882 -0.0831 11.00000 0.05 0.18 ; _shelx_res_checksum 56585 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 C1 C 1.379(2) 0.84249(19) 0.4694(6) 0.079(3) Uani 1 1 d . U H1A H 1.4840 0.8637 0.4611 0.119 Uiso 1 1 calc R U H1AB H 1.3364 0.8415 0.5272 0.119 Uiso 1 1 calc R U H1AC H 1.2113 0.8430 0.4321 0.119 Uiso 1 1 calc R U C2 C 1.5429(18) 0.81003(16) 0.4503(5) 0.0656(19) Uani 1 1 d . U H2A H 1.7101 0.8095 0.4889 0.079 Uiso 1 1 calc R U H2AB H 1.5955 0.8121 0.3932 0.079 Uiso 1 1 calc R U C3 C 1.3900(14) 0.77526(16) 0.4580(4) 0.0524(15) Uani 1 1 d . U H3A H 1.2234 0.7759 0.4191 0.063 Uiso 1 1 calc R U H3AB H 1.3359 0.7735 0.5150 0.063 Uiso 1 1 calc R U C4 C 1.5522(14) 0.74211(15) 0.4397(4) 0.0508(14) Uani 1 1 d . U H4A H 1.7183 0.7413 0.4788 0.061 Uiso 1 1 calc R U H4AB H 1.6066 0.7438 0.3827 0.061 Uiso 1 1 calc R U C5 C 1.3920(13) 0.70721(14) 0.4476(4) 0.0466(13) Uani 1 1 d . U H5A H 1.3391 0.7053 0.5048 0.056 Uiso 1 1 calc R U H5AB H 1.2252 0.7080 0.4089 0.056 Uiso 1 1 calc R U C6 C 1.5570(13) 0.67407(14) 0.4283(4) 0.0440(13) Uani 1 1 d . U H6A H 1.6173 0.6765 0.3722 0.053 Uiso 1 1 calc R U H6AB H 1.7197 0.6727 0.4687 0.053 Uiso 1 1 calc R U C7 C 1.3965(12) 0.63958(14) 0.4321(4) 0.0407(12) Uani 1 1 d . U H7A H 1.2489 0.6392 0.3863 0.049 Uiso 1 1 calc R U H7AB H 1.3152 0.6384 0.4853 0.049 Uiso 1 1 calc R U C8 C 1.5839(11) 0.60704(13) 0.4245(4) 0.0387(12) Uani 1 1 d . U H8A H 1.6536 0.6076 0.3694 0.046 Uiso 1 1 calc R U H8AB H 1.7400 0.6090 0.4672 0.046 Uiso 1 1 calc R U C9 C 1.4460(12) 0.57178(13) 0.4347(3) 0.0367(11) Uani 1 1 d . U C10 C 1.5012(11) 0.54688(13) 0.4965(3) 0.0343(11) Uani 1 1 d . U H10 H 1.6399 0.5495 0.5408 0.041 Uiso 1 1 calc R U C11 C 1.3268(10) 0.51634(13) 0.4871(3) 0.0311(10) Uani 1 1 d . U C12 C 1.1391(11) 0.51862(12) 0.4161(3) 0.0305(10) Uani 1 1 d . U C13 C 0.9462(10) 0.49088(13) 0.3941(3) 0.0301(10) Uani 1 1 d . U C14 C 0.9416(10) 0.46073(13) 0.4450(3) 0.0300(10) Uani 1 1 d . U C15 C 1.1326(10) 0.45740(12) 0.5192(3) 0.0292(10) Uani 1 1 d . U C16 C 1.3315(10) 0.48516(13) 0.5406(3) 0.0309(10) Uani 1 1 d . U C17 C 1.5128(11) 0.45298(14) 0.6552(3) 0.0333(11) Uani 1 1 d . U C18 C 1.7131(12) 0.44840(15) 0.7256(3) 0.0401(12) Uani 1 1 d . U H18 H 1.8476 0.4656 0.7390 0.048 Uiso 1 1 calc R U C19 C 1.7041(12) 0.41845(16) 0.7727(3) 0.0418(13) Uani 1 1 d . U C20 C 1.5069(14) 0.39198(16) 0.7546(4) 0.0458(14) Uani 1 1 d . U C21 C 1.3126(12) 0.39496(15) 0.6876(3) 0.0410(12) Uani 1 1 d . U H21 H 1.1807 0.3772 0.6761 0.049 Uiso 1 1 calc R U C22 C 1.3149(11) 0.42581(14) 0.6351(3) 0.0342(11) Uani 1 1 d . U C23 C 0.7343(10) 0.43586(13) 0.4118(3) 0.0325(11) Uani 1 1 d . U H23 H 0.6998 0.4144 0.4383 0.039 Uiso 1 1 calc R U C24 C 0.5945(11) 0.44661(12) 0.3384(3) 0.0310(11) Uani 1 1 d . U C25 C 0.3698(11) 0.42820(13) 0.2834(3) 0.0343(11) Uani 1 1 d . U H25A H 0.4259 0.4257 0.2267 0.041 Uiso 1 1 calc R U H25B H 0.2068 0.4431 0.2794 0.041 Uiso 1 1 calc R U C26 C 0.2965(11) 0.39129(13) 0.3156(3) 0.0351(11) Uani 1 1 d . U H26A H 0.4588 0.3762 0.3199 0.042 Uiso 1 1 calc R U H26B H 0.2366 0.3936 0.3718 0.042 Uiso 1 1 calc R U C27 C 0.0700(12) 0.37365(14) 0.2569(4) 0.0400(12) Uani 1 1 d . U H27A H -0.0852 0.3899 0.2490 0.048 Uiso 1 1 calc R U H27B H 0.1366 0.3701 0.2019 0.048 Uiso 1 1 calc R U C28 C -0.0298(12) 0.33796(15) 0.2877(4) 0.0447(13) Uani 1 1 d . U H28A H -0.0757 0.3410 0.3453 0.054 Uiso 1 1 calc R U H28B H -0.1977 0.3316 0.2529 0.054 Uiso 1 1 calc R U C29 C 0.1700(12) 0.30691(14) 0.2863(4) 0.0451(13) Uani 1 1 d . U H29A H 0.2285 0.3048 0.2299 0.054 Uiso 1 1 calc R U H29B H 0.3314 0.3119 0.3253 0.054 Uiso 1 1 calc R U C30 C 0.0465(13) 0.27165(15) 0.3105(4) 0.0497(14) Uani 1 1 d . U H30A H -0.0054 0.2738 0.3677 0.060 Uiso 1 1 calc R U H30B H -0.1203 0.2676 0.2732 0.060 Uiso 1 1 calc R U C31 C 0.2262(14) 0.23980(17) 0.3070(4) 0.0575(15) Uani 1 1 d . U H31A H 0.3909 0.2433 0.3456 0.069 Uiso 1 1 calc R U H31B H 0.2816 0.2377 0.2502 0.069 Uiso 1 1 calc R U C32 C 0.089(2) 0.20532(19) 0.3297(6) 0.079(2) Uani 1 1 d . U H32A H -0.0585 0.1999 0.2870 0.119 Uiso 1 1 calc R U H32B H 0.0183 0.2080 0.3836 0.119 Uiso 1 1 calc R U H32C H 0.2215 0.1863 0.3328 0.119 Uiso 1 1 calc R U C33 C -0.223(2) 0.15913(19) 0.0968(6) 0.087(3) Uani 1 1 d . U H33A H -0.3231 0.1370 0.0927 0.131 Uiso 1 1 calc R U H33B H -0.1246 0.1611 0.1523 0.131 Uiso 1 1 calc R U H33C H -0.0943 0.1595 0.0549 0.131 Uiso 1 1 calc R U C34 C -0.4186(18) 0.18983(18) 0.0822(6) 0.072(2) Uani 1 1 d . U H34A H -0.5327 0.1908 0.1287 0.086 Uiso 1 1 calc R U H34B H -0.5384 0.1854 0.0306 0.086 Uiso 1 1 calc R U C35 C -0.2808(15) 0.22566(16) 0.0747(4) 0.0564(16) Uani 1 1 d . U H35A H -0.1608 0.2243 0.0298 0.068 Uiso 1 1 calc R U H35B H -0.1670 0.2305 0.1272 0.068 Uiso 1 1 calc R U C36 C -0.4796(14) 0.25659(16) 0.0563(5) 0.0557(15) Uani 1 1 d . U H36A H -0.6026 0.2575 0.1005 0.067 Uiso 1 1 calc R U H36B H -0.5903 0.2520 0.0031 0.067 Uiso 1 1 calc R U C37 C -0.3420(13) 0.29282(15) 0.0508(4) 0.0519(14) Uani 1 1 d . U H37A H -0.2314 0.2975 0.1040 0.062 Uiso 1 1 calc R U H37B H -0.2191 0.2919 0.0065 0.062 Uiso 1 1 calc R U C38 C -0.5412(13) 0.32340(15) 0.0324(4) 0.0469(13) Uani 1 1 d . U H38A H -0.6645 0.3242 0.0766 0.056 Uiso 1 1 calc R U H38B H -0.6512 0.3188 -0.0209 0.056 Uiso 1 1 calc R U C39 C -0.4037(12) 0.35973(14) 0.0273(4) 0.0421(12) Uani 1 1 d . U H39A H -0.2849 0.3639 0.0792 0.051 Uiso 1 1 calc R U H39B H -0.2898 0.3596 -0.0193 0.051 Uiso 1 1 calc R U C40 C -0.6107(11) 0.39001(14) 0.0143(4) 0.0395(12) Uani 1 1 d . U H40A H -0.7347 0.3850 -0.0361 0.047 Uiso 1 1 calc R U H40B H -0.7191 0.3905 0.0622 0.047 Uiso 1 1 calc R U C41 C -0.4872(11) 0.42628(14) 0.0049(3) 0.0343(11) Uani 1 1 d . U C42 C -0.3830(11) 0.48241(13) -0.0455(3) 0.0313(10) Uani 1 1 d . U C43 C -0.1929(11) 0.48055(12) 0.0239(3) 0.0307(10) Uani 1 1 d . U C44 C -0.0046(10) 0.50879(14) 0.0459(3) 0.0323(10) Uani 1 1 d . U C45 C -0.0053(11) 0.53905(14) -0.0042(3) 0.0324(11) Uani 1 1 d . U C46 C -0.2061(11) 0.54267(13) -0.0775(3) 0.0304(10) Uani 1 1 d . U C47 C -0.3978(10) 0.51411(13) -0.0988(3) 0.0300(10) Uani 1 1 d . U C48 C -0.5912(11) 0.54661(13) -0.2113(3) 0.0323(11) Uani 1 1 d . U C49 C -0.7895(12) 0.55050(14) -0.2827(3) 0.0384(12) Uani 1 1 d . U H49 H -0.9135 0.5322 -0.2982 0.046 Uiso 1 1 calc R U C50 C -0.7948(12) 0.58107(15) -0.3277(3) 0.0405(12) Uani 1 1 d . U C51 C -0.6067(14) 0.60889(15) -0.3063(4) 0.0442(13) Uani 1 1 d . U C52 C -0.4126(13) 0.60602(15) -0.2401(4) 0.0440(13) Uani 1 1 d . U H52 H -0.2883 0.6245 -0.2271 0.053 Uiso 1 1 calc R U C53 C -0.3995(11) 0.57447(13) -0.1901(3) 0.0338(11) Uani 1 1 d . U C54 C 0.1973(11) 0.56444(13) 0.0281(3) 0.0347(11) Uani 1 1 d . U H54 H 0.2248 0.5862 0.0017 0.042 Uiso 1 1 calc R U C55 C 0.3453(12) 0.55389(14) 0.1006(3) 0.0364(11) Uani 1 1 d . U C56 C 0.5721(12) 0.57317(16) 0.1537(3) 0.0419(12) Uani 1 1 d . U H56A H 0.7386 0.5590 0.1558 0.050 Uiso 1 1 calc R U H56B H 0.5224 0.5754 0.2112 0.050 Uiso 1 1 calc R U C57 C 0.6300(13) 0.61023(15) 0.1200(4) 0.0430(13) Uani 1 1 d . U H57A H 0.6985 0.6079 0.0650 0.052 Uiso 1 1 calc R U H57B H 0.4600 0.6237 0.1125 0.052 Uiso 1 1 calc R U C58 C 0.8381(15) 0.63046(17) 0.1792(4) 0.0528(16) Uani 1 1 d . U H58A H 1.0091 0.6171 0.1850 0.063 Uiso 1 1 calc R U H58B H 0.7719 0.6317 0.2347 0.063 Uiso 1 1 calc R U C59 C 0.8962(17) 0.66815(19) 0.1502(4) 0.0648(19) Uani 1 1 d . U H59A H 0.9824 0.6666 0.0979 0.078 Uiso 1 1 calc R U H59B H 0.7221 0.6804 0.1374 0.078 Uiso 1 1 calc R U C60 C 1.071(2) 0.6900(3) 0.2102(6) 0.104(3) Uani 1 1 d . U H60A H 1.2445 0.6776 0.2228 0.125 Uiso 1 1 calc R U H60B H 0.9845 0.6913 0.2625 0.125 Uiso 1 1 calc R U C62 C -0.5546(11) 0.45141(13) -0.0559(3) 0.0341(11) Uani 1 1 d . U H62 H -0.6963 0.4487 -0.0992 0.041 Uiso 1 1 calc R U C63 C 1.054(4) 0.7931(4) 0.2000(9) 0.163(6) Uani 1 1 d . U H63A H 0.9885 0.8009 0.1438 0.245 Uiso 1 1 calc R U H63B H 1.2497 0.7959 0.2088 0.245 Uiso 1 1 calc R U H63C H 0.9698 0.8073 0.2408 0.245 Uiso 1 1 calc R U C64 C 0.980(4) 0.7544(4) 0.2105(11) 0.166(6) Uani 1 1 d D U H64A H 0.9687 0.7508 0.2706 0.200 Uiso 1 1 calc R U H64B H 0.7955 0.7514 0.1828 0.200 Uiso 1 1 calc R U C65 C 1.131(3) 0.7267(3) 0.1843(9) 0.138(4) Uani 1 1 d D U H65A H 1.3220 0.7315 0.2033 0.166 Uiso 1 1 calc R U H65B H 1.1132 0.7272 0.1228 0.166 Uiso 1 1 calc R U N1 N 1.1255(9) 0.42788(11) 0.5672(3) 0.0338(9) Uani 1 1 d . U N2 N 1.5173(9) 0.48280(11) 0.6077(3) 0.0341(9) Uani 1 1 d . U N3 N -0.5845(9) 0.51595(11) -0.1650(3) 0.0346(9) Uani 1 1 d . U N4 N -0.2085(9) 0.57233(12) -0.1227(3) 0.0357(10) Uani 1 1 d . U F1 F 1.5113(9) 0.36317(10) 0.8060(2) 0.0670(11) Uani 1 1 d . U F2 F 1.8946(8) 0.41247(10) 0.8397(2) 0.0562(9) Uani 1 1 d . U F3 F -0.9811(8) 0.58672(10) -0.3946(2) 0.0570(9) Uani 1 1 d . U F4 F -0.6289(10) 0.63851(10) -0.3543(2) 0.0691(12) Uani 1 1 d . U S1 S 0.7076(3) 0.48842(3) 0.30731(8) 0.0333(3) Uani 1 1 d . U S2 S 1.1751(3) 0.55807(3) 0.36188(8) 0.0350(3) Uani 1 1 d . U S3 S -0.2163(3) 0.44053(3) 0.07723(8) 0.0368(3) Uani 1 1 d . U S4 S 0.2410(3) 0.51154(3) 0.13169(8) 0.0367(3) Uani 1 1 d . 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 C1 0.123(7) 0.038(4) 0.085(5) -0.008(3) 0.048(5) -0.003(4) C2 0.095(5) 0.034(3) 0.073(5) -0.001(3) 0.030(4) -0.007(3) C3 0.065(4) 0.036(3) 0.058(4) 0.000(3) 0.015(3) 0.004(3) C4 0.061(4) 0.030(3) 0.063(4) -0.003(3) 0.015(3) -0.004(2) C5 0.049(3) 0.033(3) 0.059(4) -0.001(2) 0.013(3) -0.005(2) C6 0.052(3) 0.025(3) 0.055(3) -0.003(2) 0.009(3) -0.004(2) C7 0.046(3) 0.031(3) 0.046(3) 0.003(2) 0.007(2) -0.002(2) C8 0.041(3) 0.028(3) 0.045(3) 0.001(2) -0.003(2) -0.001(2) C9 0.044(3) 0.025(2) 0.041(3) -0.002(2) 0.003(2) 0.001(2) C10 0.039(3) 0.030(3) 0.033(3) -0.0019(19) 0.001(2) -0.0026(19) C11 0.039(3) 0.024(2) 0.031(2) -0.0027(18) 0.0042(19) 0.0025(19) C12 0.040(3) 0.020(2) 0.031(2) 0.0041(18) 0.0040(19) 0.0018(18) C13 0.038(3) 0.025(2) 0.027(2) -0.0023(19) 0.0017(19) 0.002(2) C14 0.036(3) 0.024(2) 0.030(2) 0.0001(18) 0.0029(19) 0.0017(19) C15 0.038(3) 0.023(2) 0.027(2) -0.0012(19) 0.0042(19) 0.0018(19) C16 0.038(3) 0.024(2) 0.031(2) -0.0010(19) 0.007(2) 0.0043(19) C17 0.044(3) 0.031(3) 0.025(2) -0.0021(19) 0.007(2) 0.005(2) C18 0.048(3) 0.041(3) 0.030(3) -0.001(2) 0.000(2) 0.004(2) C19 0.049(3) 0.050(3) 0.025(3) 0.003(2) -0.002(2) 0.010(3) C20 0.067(4) 0.039(3) 0.032(3) 0.012(2) 0.005(2) 0.013(3) C21 0.054(3) 0.032(3) 0.037(3) 0.005(2) 0.003(2) 0.004(2) C22 0.045(3) 0.029(3) 0.029(3) 0.001(2) 0.006(2) 0.007(2) C23 0.041(3) 0.025(2) 0.032(3) 0.0004(19) 0.002(2) -0.004(2) C24 0.038(3) 0.019(2) 0.036(3) -0.0013(18) 0.005(2) 0.0007(18) C25 0.039(3) 0.026(2) 0.036(3) -0.0021(19) -0.005(2) -0.0037(19) C26 0.044(3) 0.025(2) 0.036(3) 0.000(2) 0.004(2) 0.002(2) C27 0.042(3) 0.037(3) 0.040(3) -0.007(2) 0.000(2) -0.005(2) C28 0.044(3) 0.036(3) 0.054(3) -0.003(2) 0.005(2) -0.007(2) C29 0.048(3) 0.038(3) 0.051(3) -0.003(2) 0.010(2) -0.003(2) C30 0.049(3) 0.038(3) 0.064(4) -0.003(3) 0.010(3) -0.007(2) C31 0.060(4) 0.048(3) 0.065(4) 0.002(3) 0.009(3) 0.000(3) C32 0.109(7) 0.039(4) 0.088(6) 0.004(3) -0.001(5) 0.005(4) C33 0.138(8) 0.033(3) 0.096(6) 0.004(4) 0.037(6) 0.007(4) C34 0.084(5) 0.037(3) 0.096(6) 0.004(3) 0.016(4) -0.005(3) C35 0.070(4) 0.036(3) 0.064(4) -0.001(3) 0.009(3) -0.009(3) C36 0.058(4) 0.034(3) 0.074(4) 0.008(3) 0.002(3) -0.007(3) C37 0.061(4) 0.034(3) 0.060(4) 0.004(3) 0.001(3) -0.009(3) C38 0.053(4) 0.035(3) 0.052(3) 0.005(2) 0.001(3) -0.007(2) C39 0.047(3) 0.035(3) 0.043(3) 0.005(2) 0.000(2) -0.003(2) C40 0.043(3) 0.032(3) 0.044(3) 0.007(2) 0.007(2) -0.005(2) C41 0.040(3) 0.030(2) 0.034(3) 0.003(2) 0.006(2) -0.001(2) C42 0.041(3) 0.026(2) 0.028(2) 0.0012(19) 0.006(2) 0.0015(19) C43 0.039(3) 0.024(2) 0.029(2) 0.0023(18) 0.005(2) 0.0011(19) C44 0.039(3) 0.030(3) 0.027(2) 0.001(2) 0.0010(19) 0.003(2) C45 0.036(3) 0.030(3) 0.031(2) -0.002(2) 0.002(2) 0.001(2) C46 0.036(3) 0.029(2) 0.026(2) 0.0019(19) 0.0048(19) 0.003(2) C47 0.041(3) 0.028(2) 0.021(2) 0.0013(18) 0.0039(19) 0.001(2) C48 0.041(3) 0.030(3) 0.024(2) -0.0009(18) -0.001(2) 0.003(2) C49 0.045(3) 0.038(3) 0.031(3) -0.002(2) 0.000(2) -0.001(2) C50 0.047(3) 0.042(3) 0.031(3) 0.004(2) -0.005(2) 0.004(2) C51 0.064(4) 0.033(3) 0.035(3) 0.006(2) 0.001(2) 0.000(2) C52 0.062(4) 0.033(3) 0.036(3) 0.006(2) -0.004(2) -0.004(2) C53 0.046(3) 0.032(3) 0.024(2) 0.0028(19) 0.005(2) 0.000(2) C54 0.042(3) 0.028(3) 0.034(3) 0.001(2) 0.004(2) -0.001(2) C55 0.041(3) 0.033(3) 0.035(3) 0.001(2) -0.001(2) -0.002(2) C56 0.049(3) 0.039(3) 0.036(3) 0.000(2) -0.002(2) -0.001(2) C57 0.046(3) 0.040(3) 0.041(3) 0.001(2) -0.003(2) -0.008(2) C58 0.064(4) 0.054(4) 0.039(3) -0.003(3) 0.002(3) -0.020(3) C59 0.083(5) 0.056(4) 0.057(4) -0.002(3) 0.014(3) -0.019(4) C60 0.142(7) 0.091(6) 0.083(5) -0.021(5) 0.028(5) -0.053(5) C62 0.040(3) 0.027(2) 0.034(3) 0.0005(19) 0.000(2) -0.003(2) C63 0.26(2) 0.095(8) 0.131(11) 0.008(8) 0.011(12) -0.014(11) C64 0.193(10) 0.142(8) 0.173(10) 0.054(8) 0.062(8) 0.020(8) C65 0.187(9) 0.093(6) 0.143(8) -0.029(6) 0.056(7) -0.054(7) N1 0.046(3) 0.025(2) 0.030(2) 0.0019(16) 0.0005(18) 0.0020(17) N2 0.043(2) 0.032(2) 0.027(2) -0.0002(17) -0.0001(17) 0.0024(18) N3 0.045(3) 0.029(2) 0.030(2) 0.0004(17) 0.0024(17) -0.0011(18) N4 0.043(3) 0.037(2) 0.026(2) 0.0022(18) 0.0007(18) -0.0031(18) F1 0.093(3) 0.054(2) 0.050(2) 0.0263(17) -0.0136(19) -0.005(2) F2 0.064(2) 0.064(2) 0.0370(18) 0.0109(16) -0.0113(15) 0.0079(17) F3 0.064(2) 0.058(2) 0.0432(19) 0.0160(16) -0.0205(16) -0.0036(17) F4 0.098(3) 0.048(2) 0.055(2) 0.0253(17) -0.023(2) -0.010(2) S1 0.0407(7) 0.0246(6) 0.0330(6) 0.0034(5) -0.0044(5) -0.0002(5) S2 0.0445(7) 0.0230(6) 0.0364(7) 0.0047(5) -0.0015(5) -0.0002(5) S3 0.0456(8) 0.0281(6) 0.0356(7) 0.0074(5) -0.0007(5) 0.0004(5) S4 0.0433(7) 0.0317(7) 0.0333(6) 0.0041(5) -0.0045(5) -0.0002(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' F F 0.0171 0.0103 '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 C2 C1 H1A 109.5 C2 C1 H1AB 109.5 H1A C1 H1AB 109.5 C2 C1 H1AC 109.5 H1A C1 H1AC 109.5 H1AB C1 H1AC 109.5 C1 C2 C3 113.5(6) C1 C2 H2A 108.9 C3 C2 H2A 108.9 C1 C2 H2AB 108.9 C3 C2 H2AB 108.9 H2A C2 H2AB 107.7 C2 C3 C4 114.5(5) C2 C3 H3A 108.6 C4 C3 H3A 108.6 C2 C3 H3AB 108.6 C4 C3 H3AB 108.6 H3A C3 H3AB 107.6 C3 C4 C5 113.5(5) C3 C4 H4A 108.9 C5 C4 H4A 108.9 C3 C4 H4AB 108.9 C5 C4 H4AB 108.9 H4A C4 H4AB 107.7 C6 C5 C4 112.9(5) C6 C5 H5A 109.0 C4 C5 H5A 109.0 C6 C5 H5AB 109.0 C4 C5 H5AB 109.0 H5A C5 H5AB 107.8 C7 C6 C5 113.4(5) C7 C6 H6A 108.9 C5 C6 H6A 108.9 C7 C6 H6AB 108.9 C5 C6 H6AB 108.9 H6A C6 H6AB 107.7 C6 C7 C8 110.8(5) C6 C7 H7A 109.5 C8 C7 H7A 109.5 C6 C7 H7AB 109.5 C8 C7 H7AB 109.5 H7A C7 H7AB 108.1 C9 C8 C7 114.2(5) C9 C8 H8A 108.7 C7 C8 H8A 108.7 C9 C8 H8AB 108.7 C7 C8 H8AB 108.7 H8A C8 H8AB 107.6 C10 C9 C8 128.5(5) C10 C9 S2 110.9(4) C8 C9 S2 120.5(4) C9 C10 C11 113.6(5) C9 C10 H10 123.2 C11 C10 H10 123.2 C12 C11 C10 112.2(4) C12 C11 C16 120.0(5) C10 C11 C16 127.9(5) C11 C12 C13 121.6(4) C11 C12 S2 111.4(4) C13 C12 S2 127.0(4) C14 C13 C12 120.1(4) C14 C13 S1 111.9(4) C12 C13 S1 128.0(4) C13 C14 C15 120.0(4) C13 C14 C23 111.5(4) C15 C14 C23 128.5(4) N1 C15 C14 119.0(4) N1 C15 C16 121.0(4) C14 C15 C16 120.0(4) N2 C16 C15 122.1(4) N2 C16 C11 119.5(5) C15 C16 C11 118.4(4) N2 C17 C22 121.2(5) N2 C17 C18 119.4(5) C22 C17 C18 119.4(5) C19 C18 C17 118.5(5) C19 C18 H18 120.8 C17 C18 H18 120.8 C18 C19 F2 120.7(5) C18 C19 C20 122.6(5) F2 C19 C20 116.7(5) F1 C20 C21 120.4(6) F1 C20 C19 118.4(5) C21 C20 C19 121.2(5) C20 C21 C22 118.6(6) C20 C21 H21 120.7 C22 C21 H21 120.7 N1 C22 C17 122.4(5) N1 C22 C21 117.9(5) C17 C22 C21 119.7(5) C24 C23 C14 113.6(4) C24 C23 H23 123.2 C14 C23 H23 123.2 C23 C24 C25 129.9(5) C23 C24 S1 111.3(4) C25 C24 S1 118.8(4) C24 C25 C26 113.8(4) C24 C25 H25A 108.8 C26 C25 H25A 108.8 C24 C25 H25B 108.8 C26 C25 H25B 108.8 H25A C25 H25B 107.7 C27 C26 C25 111.6(4) C27 C26 H26A 109.3 C25 C26 H26A 109.3 C27 C26 H26B 109.3 C25 C26 H26B 109.3 H26A C26 H26B 108.0 C28 C27 C26 115.0(5) C28 C27 H27A 108.5 C26 C27 H27A 108.5 C28 C27 H27B 108.5 C26 C27 H27B 108.5 H27A C27 H27B 107.5 C29 C28 C27 116.0(5) C29 C28 H28A 108.3 C27 C28 H28A 108.3 C29 C28 H28B 108.3 C27 C28 H28B 108.3 H28A C28 H28B 107.4 C30 C29 C28 112.8(5) C30 C29 H29A 109.0 C28 C29 H29A 109.0 C30 C29 H29B 109.0 C28 C29 H29B 109.0 H29A C29 H29B 107.8 C31 C30 C29 115.8(5) C31 C30 H30A 108.3 C29 C30 H30A 108.3 C31 C30 H30B 108.3 C29 C30 H30B 108.3 H30A C30 H30B 107.4 C30 C31 C32 113.4(6) C30 C31 H31A 108.9 C32 C31 H31A 108.9 C30 C31 H31B 108.9 C32 C31 H31B 108.9 H31A C31 H31B 107.7 C31 C32 H32A 109.5 C31 C32 H32B 109.5 H32A C32 H32B 109.5 C31 C32 H32C 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 C34 C33 H33A 109.5 C34 C33 H33B 109.5 H33A C33 H33B 109.5 C34 C33 H33C 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 C33 C34 C35 114.1(7) C33 C34 H34A 108.7 C35 C34 H34A 108.7 C33 C34 H34B 108.7 C35 C34 H34B 108.7 H34A C34 H34B 107.6 C34 C35 C36 114.1(6) C34 C35 H35A 108.7 C36 C35 H35A 108.7 C34 C35 H35B 108.7 C36 C35 H35B 108.7 H35A C35 H35B 107.6 C35 C36 C37 114.3(5) C35 C36 H36A 108.7 C37 C36 H36A 108.7 C35 C36 H36B 108.7 C37 C36 H36B 108.7 H36A C36 H36B 107.6 C38 C37 C36 113.9(5) C38 C37 H37A 108.8 C36 C37 H37A 108.8 C38 C37 H37B 108.8 C36 C37 H37B 108.8 H37A C37 H37B 107.7 C37 C38 C39 114.0(5) C37 C38 H38A 108.8 C39 C38 H38A 108.8 C37 C38 H38B 108.8 C39 C38 H38B 108.8 H38A C38 H38B 107.7 C40 C39 C38 112.4(5) C40 C39 H39A 109.1 C38 C39 H39A 109.1 C40 C39 H39B 109.1 C38 C39 H39B 109.1 H39A C39 H39B 107.9 C41 C40 C39 114.7(5) C41 C40 H40A 108.6 C39 C40 H40A 108.6 C41 C40 H40B 108.6 C39 C40 H40B 108.6 H40A C40 H40B 107.6 C62 C41 C40 128.6(5) C62 C41 S3 111.5(4) C40 C41 S3 119.9(4) C43 C42 C62 113.2(4) C43 C42 C47 119.9(5) C62 C42 C47 126.9(5) C42 C43 C44 122.0(4) C42 C43 S3 111.4(4) C44 C43 S3 126.6(4) C45 C44 C43 120.2(4) C45 C44 S4 111.4(4) C43 C44 S4 128.4(4) C44 C45 C54 112.2(4) C44 C45 C46 119.9(4) C54 C45 C46 127.8(5) N4 C46 C47 121.8(4) N4 C46 C45 118.8(4) C47 C46 C45 119.4(4) N3 C47 C46 121.9(4) N3 C47 C42 119.6(4) C46 C47 C42 118.5(4) N3 C48 C53 120.8(4) N3 C48 C49 119.6(5) C53 C48 C49 119.6(5) C50 C49 C48 118.9(5) C50 C49 H49 120.6 C48 C49 H49 120.6 F3 C50 C49 121.8(5) F3 C50 C51 116.6(5) C49 C50 C51 121.6(5) F4 C51 C52 121.2(5) F4 C51 C50 117.4(5) C52 C51 C50 121.4(5) C51 C52 C53 119.3(5) C51 C52 H52 120.3 C53 C52 H52 120.3 N4 C53 C48 122.1(4) N4 C53 C52 118.7(5) C48 C53 C52 119.2(5) C55 C54 C45 113.7(5) C55 C54 H54 123.2 C45 C54 H54 123.2 C54 C55 C56 129.4(5) C54 C55 S4 110.9(4) C56 C55 S4 119.7(4) C55 C56 C57 113.1(5) C55 C56 H56A 109.0 C57 C56 H56A 109.0 C55 C56 H56B 109.0 C57 C56 H56B 109.0 H56A C56 H56B 107.8 C58 C57 C56 112.0(5) C58 C57 H57A 109.2 C56 C57 H57A 109.2 C58 C57 H57B 109.2 C56 C57 H57B 109.2 H57A C57 H57B 107.9 C57 C58 C59 114.3(6) C57 C58 H58A 108.7 C59 C58 H58A 108.7 C57 C58 H58B 108.7 C59 C58 H58B 108.7 H58A C58 H58B 107.6 C60 C59 C58 116.0(7) C60 C59 H59A 108.3 C58 C59 H59A 108.3 C60 C59 H59B 108.3 C58 C59 H59B 108.3 H59A C59 H59B 107.4 C59 C60 C65 117.4(10) C59 C60 H60A 107.9 C65 C60 H60A 107.9 C59 C60 H60B 107.9 C65 C60 H60B 107.9 H60A C60 H60B 107.2 C41 C62 C42 112.4(5) C41 C62 H62 123.8 C42 C62 H62 123.8 C64 C63 H63A 109.5 C64 C63 H63B 109.5 H63A C63 H63B 109.5 C64 C63 H63C 109.5 H63A C63 H63C 109.5 H63B C63 H63C 109.5 C65 C64 C63 123.8(14) C65 C64 H64A 106.4 C63 C64 H64A 106.4 C65 C64 H64B 106.4 C63 C64 H64B 106.4 H64A C64 H64B 106.4 C64 C65 C60 119.7(12) C64 C65 H65A 107.4 C60 C65 H65A 107.4 C64 C65 H65B 107.4 C60 C65 H65B 107.4 H65A C65 H65B 106.9 C15 N1 C22 116.4(4) C16 N2 C17 116.9(5) C47 N3 C48 116.7(4) C46 N4 C53 116.6(4) C13 S1 C24 91.7(2) C12 S2 C9 91.8(2) C43 S3 C41 91.5(2) C44 S4 C55 91.8(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.503(10) C1 H1A 0.9600 C1 H1AB 0.9600 C1 H1AC 0.9600 C2 C3 1.511(9) C2 H2A 0.9700 C2 H2AB 0.9700 C3 C4 1.515(8) C3 H3A 0.9700 C3 H3AB 0.9700 C4 C5 1.534(8) C4 H4A 0.9700 C4 H4AB 0.9700 C5 C6 1.527(8) C5 H5A 0.9700 C5 H5AB 0.9700 C6 C7 1.514(7) C6 H6A 0.9700 C6 H6AB 0.9700 C7 C8 1.535(7) C7 H7A 0.9700 C7 H7AB 0.9700 C8 C9 1.497(7) C8 H8A 0.9700 C8 H8AB 0.9700 C9 C10 1.359(8) C9 S2 1.742(6) C10 C11 1.424(7) C10 H10 0.9300 C11 C12 1.380(7) C11 C16 1.441(7) C12 C13 1.421(7) C12 S2 1.725(5) C13 C14 1.387(7) C13 S1 1.713(5) C14 C15 1.431(7) C14 C23 1.435(7) C15 N1 1.343(6) C15 C16 1.439(7) C16 N2 1.329(7) C17 N2 1.347(7) C17 C22 1.417(8) C17 C18 1.418(8) C18 C19 1.349(8) C18 H18 0.9300 C19 F2 1.358(6) C19 C20 1.391(9) C20 F1 1.350(6) C20 C21 1.355(8) C21 C22 1.422(7) C21 H21 0.9300 C22 N1 1.348(7) C23 C24 1.348(7) C23 H23 0.9300 C24 C25 1.499(7) C24 S1 1.746(5) C25 C26 1.527(7) C25 H25A 0.9700 C25 H25B 0.9700 C26 C27 1.522(7) C26 H26A 0.9700 C26 H26B 0.9700 C27 C28 1.519(8) C27 H27A 0.9700 C27 H27B 0.9700 C28 C29 1.519(8) C28 H28A 0.9700 C28 H28B 0.9700 C29 C30 1.516(8) C29 H29A 0.9700 C29 H29B 0.9700 C30 C31 1.485(9) C30 H30A 0.9700 C30 H30B 0.9700 C31 C32 1.513(10) C31 H31A 0.9700 C31 H31B 0.9700 C32 H32A 0.9600 C32 H32B 0.9600 C32 H32C 0.9600 C33 C34 1.498(11) C33 H33A 0.9600 C33 H33B 0.9600 C33 H33C 0.9600 C34 C35 1.510(9) C34 H34A 0.9700 C34 H34B 0.9700 C35 C36 1.520(9) C35 H35A 0.9700 C35 H35B 0.9700 C36 C37 1.519(8) C36 H36A 0.9700 C36 H36B 0.9700 C37 C38 1.511(8) C37 H37A 0.9700 C37 H37B 0.9700 C38 C39 1.522(8) C38 H38A 0.9700 C38 H38B 0.9700 C39 C40 1.519(8) C39 H39A 0.9700 C39 H39B 0.9700 C40 C41 1.498(7) C40 H40A 0.9700 C40 H40B 0.9700 C41 C62 1.362(7) C41 S3 1.744(5) C42 C43 1.367(7) C42 C62 1.430(7) C42 C47 1.453(7) C43 C44 1.421(7) C43 S3 1.728(5) C44 C45 1.382(7) C44 S4 1.722(5) C45 C54 1.429(7) C45 C46 1.449(7) C46 N4 1.320(7) C46 C47 1.438(7) C47 N3 1.320(6) C48 N3 1.360(6) C48 C53 1.418(7) C48 C49 1.420(7) C49 C50 1.346(8) C49 H49 0.9300 C50 F3 1.342(6) C50 C51 1.407(8) C51 F4 1.342(6) C51 C52 1.345(8) C52 C53 1.418(7) C52 H52 0.9300 C53 N4 1.347(7) C54 C55 1.353(7) C54 H54 0.9300 C55 C56 1.505(8) C55 S4 1.749(5) C56 C57 1.522(8) C56 H56A 0.9700 C56 H56B 0.9700 C57 C58 1.513(8) C57 H57A 0.9700 C57 H57B 0.9700 C58 C59 1.518(9) C58 H58A 0.9700 C58 H58B 0.9700 C59 C60 1.461(11) C59 H59A 0.9700 C59 H59B 0.9700 C60 C65 1.468(14) C60 H60A 0.9700 C60 H60B 0.9700 C62 H62 0.9300 C63 C64 1.505(18) C63 H63A 0.9600 C63 H63B 0.9600 C63 H63C 0.9600 C64 C65 1.360(10) C64 H64A 0.9700 C64 H64B 0.9700 C65 H65A 0.9700 C65 H65B 0.9700