#------------------------------------------------------------------------------ #$Date: 2019-12-13 11:48:22 +0200 (Fri, 13 Dec 2019) $ #$Revision: 245059 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556564.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_1556564 loop_ _publ_author_name 'Cosquer, G.' 'Kamila, M.' 'Li, Z.-Y.' 'Breedlove, B.K.' 'Yamashita, M.' _publ_section_title ; Photo-Modulation of Single-Molecule Magnetic Dynamics of a Dysprosium Dinuclear Complex via a Diarylethene Bridge ; _journal_name_full Inorganics _journal_page_first 9 _journal_paper_doi 10.3390/inorganics6010009 _journal_volume 6 _journal_year 2018 _chemical_formula_sum 'C72 H50 Dy2 F36 N4 O12 S2' _chemical_formula_weight 2236.28 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _cell_angle_alpha 71.022(8) _cell_angle_beta 79.601(9) _cell_angle_gamma 70.806(7) _cell_formula_units_Z 2 _cell_length_a 11.7047(3) _cell_length_b 19.61640(10) _cell_length_c 20.8522(2) _cell_measurement_reflns_used 6801 _cell_measurement_temperature 96.1(2) _cell_measurement_theta_max 24.0914 _cell_measurement_theta_min 3.1099 _cell_volume 4261.3(3) _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution SIR-92 _diffrn_ambient_temperature 96.1(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.760 _diffrn_measured_fraction_theta_max 0.760 _diffrn_measurement_device_type ; Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_unetI/netI 0.0470 _diffrn_reflns_Laue_measured_fraction_full 0.760 _diffrn_reflns_Laue_measured_fraction_max 0.760 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 13349 _diffrn_reflns_point_group_measured_fraction_full 0.760 _diffrn_reflns_point_group_measured_fraction_max 0.760 _diffrn_reflns_theta_full 24.133 _diffrn_reflns_theta_max 24.133 _diffrn_reflns_theta_min 4.022 _exptl_absorpt_coefficient_mu 1.926 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7368 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 2188 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.417 _refine_diff_density_min -1.128 _refine_diff_density_rms 0.095 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1191 _refine_ls_number_reflns 10338 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.978 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0365 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0658P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.0963 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8283 _reflns_number_total 10338 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file Inorganics-2018-6-9.cif _cod_data_source_block 2-close _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 built-in table derived from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated on 2014-11-21. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_database_code 1556564 _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 ; /home/goulven/wingx/00/shelx.res created by SHELXL-2014/7 TITL shelx in P -1 CELL 0.71073 11.7047 19.6164 20.8522 71.022 79.601 70.806 ZERR 2.00 0.0003 0.0001 0.0002 0.008 0.009 0.007 LATT 1 SFAC C H N O F S DY UNIT 144 100 8 24 72 4 4 MERG 2 FMAP 2 PLAN 25 ACTA L.S. 40 WGHT 0.065800 FVAR 3.59177 0.49435 0.46776 C1 1 0.451881 1.190293 1.036351 11.00000 0.04257 0.03856 = 0.02630 -0.01166 -0.00871 -0.01664 AFIX 43 H1 2 0.466334 1.236697 1.015206 11.00000 -1.20000 AFIX 0 C2 1 0.473957 1.155252 1.104438 11.00000 0.05406 0.05055 = 0.02593 -0.01079 -0.00760 -0.02770 AFIX 43 H2 2 0.499276 1.178546 1.129330 11.00000 -1.20000 AFIX 0 C3 1 0.457359 1.085741 1.133571 11.00000 0.07367 0.05538 = 0.02436 -0.00373 -0.01702 -0.03049 AFIX 43 H3 2 0.473586 1.060387 1.178638 11.00000 -1.20000 AFIX 0 C4 1 0.416726 1.052998 1.096572 11.00000 0.05756 0.04169 = 0.02939 -0.00461 -0.00656 -0.02482 AFIX 43 H4 2 0.406325 1.005320 1.116176 11.00000 -1.20000 AFIX 0 C5 1 0.391477 1.091758 1.029845 11.00000 0.02460 0.03288 = 0.02314 -0.01046 0.00078 -0.01153 C6 1 0.342016 1.061887 0.986711 11.00000 0.02134 0.02705 = 0.02286 -0.00883 0.00111 -0.00896 C7 1 0.316096 0.993887 1.010457 11.00000 0.03277 0.03597 = 0.02606 -0.00802 -0.00249 -0.01344 AFIX 43 H5 2 0.334579 0.962927 1.053968 11.00000 -1.20000 AFIX 0 C8 1 0.262758 0.971475 0.969916 11.00000 0.03756 0.03429 = 0.02763 -0.00506 -0.00325 -0.02156 AFIX 43 H6 2 0.245028 0.925655 0.986011 11.00000 -1.20000 AFIX 0 C9 1 0.235783 1.018158 0.904699 11.00000 0.03228 0.02480 = 0.02794 -0.00609 -0.00690 -0.01193 C10 1 0.269754 1.084369 0.883132 11.00000 0.03277 0.02490 = 0.02630 -0.00610 -0.01158 -0.00725 AFIX 43 H7 2 0.255649 1.115136 0.839050 11.00000 -1.20000 AFIX 0 C11 1 0.172796 0.998929 0.861118 11.00000 0.03354 0.02556 = 0.02881 -0.00324 -0.00762 -0.01514 C12 1 0.141295 1.038211 0.796824 11.00000 0.04625 0.03859 = 0.03223 -0.00276 -0.00382 -0.03149 AFIX 43 H8 2 0.160866 1.082551 0.772969 11.00000 -1.20000 AFIX 0 C13 1 0.076065 1.006410 0.768694 11.00000 0.05404 0.03766 = 0.02903 -0.00028 -0.01149 -0.03010 PART 1 C14A 1 0.022555 0.948486 0.825034 -21.00000 0.03127 0.02649 = 0.02521 -0.01086 -0.00100 -0.01163 C15A 1 -0.105509 0.982014 0.855590 -21.00000 0.04181 0.04130 = 0.03110 -0.01464 -0.01263 -0.01592 AFIX 33 H9A 2 -0.104261 1.020198 0.874629 -21.00000 -1.50000 H11A 2 -0.160874 1.003839 0.820569 -21.00000 -1.50000 H10A 2 -0.131337 0.942933 0.890648 -21.00000 -1.50000 AFIX 0 PART 2 C14B 1 0.088198 0.922318 0.810119 21.00000 0.04491 0.02668 = 0.03408 -0.01055 -0.01021 -0.01118 C21B 1 -0.136400 0.968364 0.844942 21.00000 0.03718 0.04978 = 0.03119 -0.01928 -0.00236 -0.01678 AFIX 33 H18B 2 -0.212987 0.960182 0.845209 21.00000 -1.50000 H20B 2 -0.120013 0.960051 0.890790 21.00000 -1.50000 H19B 2 -0.139307 1.019201 0.819015 21.00000 -1.50000 AFIX 0 PART 0 C16 1 0.033091 1.028794 0.705918 11.00000 0.03097 0.02821 = 0.02491 -0.00548 -0.00216 -0.01531 C17 1 0.042414 1.095505 0.646613 11.00000 0.04303 0.03930 = 0.03324 -0.00270 -0.00595 -0.02487 AFIX 23 H13 2 0.123044 1.101655 0.639869 11.00000 -1.20000 H12 2 -0.016700 1.141354 0.653004 11.00000 -1.20000 AFIX 0 C18 1 0.015609 1.075889 0.586575 11.00000 0.07747 0.06067 = 0.02801 0.00350 -0.01546 -0.04776 AFIX 23 H15 2 0.090354 1.050269 0.564756 11.00000 -1.20000 H14 2 -0.025051 1.121229 0.553182 11.00000 -1.20000 AFIX 0 C19 1 -0.066513 1.024268 0.616121 11.00000 0.04719 0.04234 = 0.03094 -0.00737 -0.00916 -0.02409 AFIX 23 H16 2 -0.151559 1.053030 0.614427 11.00000 -1.20000 H17 2 -0.049860 0.986996 0.591822 11.00000 -1.20000 AFIX 0 C20 1 -0.032773 0.987294 0.689367 11.00000 0.02581 0.02963 = 0.02581 -0.00868 -0.00526 -0.00752 PART 1 C21A 1 0.160529 0.849182 0.767546 -21.00000 0.01970 0.02299 = 0.05879 -0.01641 -0.01491 -0.00593 AFIX 33 H18A 2 0.160047 0.811039 0.748234 -21.00000 -1.50000 H19A 2 0.191846 0.886636 0.733528 -21.00000 -1.50000 H20A 2 0.210947 0.826702 0.804925 -21.00000 -1.50000 AFIX 0 C22A 1 0.027972 0.886978 0.793571 -21.00000 0.04572 0.02269 = 0.03935 -0.00698 -0.01129 -0.02331 PART 2 C15B 1 0.193235 0.863362 0.780399 21.00000 0.03091 0.03248 = 0.05630 -0.00511 -0.01936 -0.01165 AFIX 33 H9B 2 0.269580 0.871873 0.780073 21.00000 -1.50000 H10B 2 0.195223 0.813282 0.808242 21.00000 -1.50000 H11B 2 0.178814 0.869058 0.734797 21.00000 -1.50000 AFIX 0 C22B 1 -0.036028 0.913745 0.812835 21.00000 0.05585 0.02491 = 0.02837 -0.00554 -0.00995 -0.01288 PART 0 C23 1 -0.055219 0.925584 0.734638 11.00000 0.03362 0.03074 = 0.03400 -0.00517 -0.01481 -0.01211 C24 1 -0.119215 0.875978 0.730865 11.00000 0.03840 0.03355 = 0.03181 -0.00293 -0.01512 -0.01857 AFIX 43 H21 2 -0.156184 0.883819 0.692130 11.00000 -1.20000 AFIX 0 C25 1 -0.122612 0.818404 0.785697 11.00000 0.03369 0.03579 = 0.03771 -0.00719 -0.01298 -0.01568 C26 1 -0.260826 0.761714 0.755156 11.00000 0.03260 0.02456 = 0.02392 -0.00143 -0.00534 -0.01093 AFIX 43 H22 2 -0.282900 0.805101 0.719139 11.00000 -1.20000 AFIX 0 C27 1 -0.178215 0.758402 0.797441 11.00000 0.02682 0.02761 = 0.03045 -0.00490 -0.00572 -0.01323 C28 1 -0.153457 0.693630 0.853008 11.00000 0.03815 0.03861 = 0.03236 -0.00728 -0.00795 -0.02425 AFIX 43 H23 2 -0.103535 0.689494 0.884920 11.00000 -1.20000 AFIX 0 C29 1 -0.201945 0.636181 0.860956 11.00000 0.03070 0.02871 = 0.02915 -0.00239 -0.00609 -0.00931 AFIX 43 H24 2 -0.182886 0.592767 0.897263 11.00000 -1.20000 AFIX 0 C30 1 -0.279471 0.643115 0.814642 11.00000 0.01846 0.02508 = 0.02489 -0.00854 0.00148 -0.00520 C31 1 -0.331152 0.582780 0.817860 11.00000 0.01571 0.02641 = 0.02512 -0.01173 0.00338 -0.00505 C32 1 -0.309314 0.514726 0.868405 11.00000 0.03196 0.02804 = 0.02737 -0.00761 -0.00484 -0.00977 AFIX 43 H25 2 -0.263488 0.506484 0.903740 11.00000 -1.20000 AFIX 0 C33 1 -0.355254 0.459105 0.866560 11.00000 0.04055 0.02720 = 0.03253 -0.00497 -0.00430 -0.01066 AFIX 43 H26 2 -0.341565 0.413620 0.900821 11.00000 -1.20000 AFIX 0 C34 1 -0.422096 0.471648 0.813099 11.00000 0.03757 0.02898 = 0.03142 -0.01013 -0.00492 -0.01377 AFIX 43 H27 2 -0.452241 0.434640 0.809866 11.00000 -1.20000 AFIX 0 C35 1 -0.442198 0.541092 0.764885 11.00000 0.02933 0.02752 = 0.02297 -0.00830 -0.00246 -0.01195 AFIX 43 H28 2 -0.488095 0.550248 0.729311 11.00000 -1.20000 AFIX 0 C36 1 0.770463 1.225690 0.863696 11.00000 0.02814 0.04389 = 0.03912 -0.01196 0.00628 -0.02395 C37 1 0.663770 1.208732 0.847501 11.00000 0.03470 0.02122 = 0.03853 -0.00500 -0.01057 -0.00851 C38 1 0.678358 1.186189 0.788064 11.00000 0.03407 0.03516 = 0.03082 -0.01019 0.00807 -0.01526 AFIX 43 H29 2 0.747374 1.188033 0.758185 11.00000 -1.20000 AFIX 0 C39 1 0.591149 1.161576 0.774202 11.00000 0.03307 0.02821 = 0.02948 -0.00986 -0.00108 -0.00578 C40 1 0.615758 1.131380 0.712121 11.00000 0.04014 0.04727 = 0.04246 -0.02339 0.00388 -0.01256 C41 1 0.464153 1.404039 0.677726 11.00000 0.07292 0.05262 = 0.02954 -0.00343 -0.01263 -0.04152 C42 1 0.393819 1.348844 0.723058 11.00000 0.04467 0.03039 = 0.02822 -0.01333 0.00622 -0.01922 C43 1 0.314162 1.331620 0.692874 11.00000 0.06356 0.03158 = 0.02392 -0.00111 -0.00717 -0.02468 AFIX 43 H30 2 0.306434 1.352712 0.646395 11.00000 -1.20000 AFIX 0 C44 1 0.246536 1.284030 0.730321 11.00000 0.03883 0.03600 = 0.02777 -0.00810 -0.00973 -0.01326 C45 1 0.164627 1.264498 0.693547 11.00000 0.05808 0.05941 = 0.02871 -0.00346 -0.00526 -0.03080 C46 1 0.267610 1.451177 0.936172 11.00000 0.04904 0.02902 = 0.04453 -0.01075 -0.01324 -0.00960 C47 1 0.243114 1.379465 0.936162 11.00000 0.03455 0.02108 = 0.02421 -0.00609 -0.00813 -0.00679 C48 1 0.128965 1.371186 0.954688 11.00000 0.02925 0.02562 = 0.03392 -0.01396 -0.00473 -0.00214 AFIX 43 H31 2 0.068840 1.407899 0.970766 11.00000 -1.20000 AFIX 0 C49 1 0.100195 1.309705 0.950219 11.00000 0.02908 0.03173 = 0.02459 -0.00221 -0.00748 -0.00997 C50 1 -0.032120 1.307601 0.968934 11.00000 0.02726 0.03949 = 0.04819 -0.01812 -0.00777 -0.00472 C51 1 -0.385251 0.598659 0.536093 11.00000 0.11675 0.08354 = 0.04485 -0.03671 0.02239 -0.05602 C52 1 -0.376489 0.657061 0.567510 11.00000 0.05216 0.04699 = 0.02591 -0.01522 -0.00004 -0.02341 C53 1 -0.304688 0.704217 0.533306 11.00000 0.06898 0.05313 = 0.02291 -0.00972 0.00926 -0.03344 AFIX 43 H32 2 -0.264320 0.700757 0.491252 11.00000 -1.20000 AFIX 0 C54 1 -0.292933 0.756324 0.561507 11.00000 0.03499 0.02984 = 0.02413 -0.00194 0.00160 -0.01260 C55 1 -0.213843 0.805890 0.525111 11.00000 0.06413 0.02683 = 0.04610 0.00328 -0.01836 -0.01776 C56 1 -0.705315 0.896354 0.513686 11.00000 0.05985 0.04855 = 0.03732 0.00067 -0.02721 -0.01977 C57 1 -0.634606 0.873919 0.576034 11.00000 0.03418 0.04357 = 0.03129 -0.00763 -0.01368 -0.01045 C58 1 -0.607450 0.930650 0.591840 11.00000 0.04970 0.03010 = 0.02558 0.00129 -0.01612 -0.01204 AFIX 43 H33 2 -0.627225 0.979432 0.562740 11.00000 -1.20000 AFIX 0 C59 1 -0.551161 0.915116 0.650595 11.00000 0.03225 0.02413 = 0.02851 -0.00291 -0.00565 -0.00683 C60 1 -0.526709 0.980265 0.665156 11.00000 0.05332 0.02753 = 0.03388 -0.00238 -0.01964 -0.00718 C61 1 -0.825544 0.639877 0.753461 11.00000 0.03124 0.06188 = 0.04576 -0.02218 0.00610 -0.02013 C62 1 -0.724399 0.664578 0.769184 11.00000 0.02603 0.03174 = 0.03970 -0.01262 -0.00161 -0.01017 C63 1 -0.709939 0.656683 0.835839 11.00000 0.03456 0.03041 = 0.03256 -0.00683 0.00547 -0.01667 AFIX 43 H34 2 -0.756147 0.631654 0.870820 11.00000 -1.20000 AFIX 0 C64 1 -0.628201 0.685165 0.851882 11.00000 0.02125 0.02184 = 0.02571 -0.00812 0.00050 -0.00129 C65 1 -0.618317 0.674445 0.927053 11.00000 0.03436 0.03267 = 0.03074 -0.00383 -0.00116 -0.01236 N1 3 0.410138 1.158999 1.000059 11.00000 0.03108 0.02780 = 0.02310 -0.00962 -0.00420 -0.00930 N2 3 0.321344 1.106142 0.922098 11.00000 0.02314 0.01950 = 0.02370 -0.00697 -0.00475 -0.00541 N3 3 -0.310275 0.707076 0.762773 11.00000 0.02374 0.02879 = 0.02195 -0.00187 -0.00077 -0.01477 N4 3 -0.399351 0.596261 0.766320 11.00000 0.02379 0.02853 = 0.02480 -0.01028 -0.00291 -0.00728 O1 4 0.572122 1.217379 0.888144 11.00000 0.02602 0.03597 = 0.02568 -0.01038 0.00253 -0.01395 O2 4 0.491524 1.157784 0.808229 11.00000 0.03591 0.03005 = 0.03218 -0.01640 0.00259 -0.01331 O3 4 0.417664 1.324135 0.784081 11.00000 0.03837 0.03121 = 0.02451 -0.00955 0.00162 -0.01671 O4 4 0.245505 1.250457 0.793695 11.00000 0.03303 0.03234 = 0.02393 -0.00459 -0.00555 -0.01425 O5 4 0.336728 1.333284 0.916802 11.00000 0.03102 0.03262 = 0.02970 -0.01435 -0.00121 -0.01209 O6 4 0.169855 1.256547 0.929011 11.00000 0.02646 0.02861 = 0.03266 -0.01225 0.00037 -0.01006 O7 4 -0.438407 0.656299 0.623126 11.00000 0.04214 0.03554 = 0.02865 -0.01321 0.00047 -0.01976 O8 4 -0.341169 0.768528 0.616922 11.00000 0.03679 0.03330 = 0.02525 -0.00353 -0.00124 -0.01643 O9 4 -0.609088 0.805732 0.607459 11.00000 0.04792 0.03089 = 0.02997 -0.00350 -0.01685 -0.01391 O10 4 -0.521011 0.853764 0.696525 11.00000 0.03255 0.02361 = 0.02551 -0.00470 -0.00631 -0.00790 O11 4 -0.660634 0.689639 0.717329 11.00000 0.02681 0.04337 = 0.03292 -0.01380 -0.00276 -0.01463 O12 4 -0.562513 0.722773 0.810985 11.00000 0.02591 0.02574 = 0.02542 -0.00841 -0.00127 -0.00978 F1 5 0.753842 1.288980 0.860212 11.00000 0.12275 0.07860 = 0.62554 -0.12268 -0.20398 -0.00161 F2 5 0.864865 1.212603 0.828842 11.00000 0.07900 0.47029 = 0.21198 -0.23987 0.06383 -0.16339 F3 5 0.801198 1.191532 0.920431 11.00000 0.20522 0.40382 = 0.11042 0.09145 -0.10159 -0.25695 F4 5 0.702097 1.153355 0.668055 11.00000 0.10983 0.10809 = 0.05626 -0.05600 0.04163 -0.06759 F5 5 0.650920 1.057048 0.731311 11.00000 0.09009 0.04397 = 0.06884 -0.03483 -0.01060 -0.01409 F6 5 0.517727 1.153591 0.679543 11.00000 0.06641 0.11196 = 0.05874 -0.05666 -0.02567 0.01795 F7 5 0.579708 1.381386 0.690791 11.00000 0.07049 0.09046 = 0.10589 0.00454 0.01187 -0.04976 F8 5 0.457288 1.419782 0.614291 11.00000 0.28107 0.21507 = 0.02673 -0.00258 -0.00204 -0.22762 F9 5 0.422550 1.467193 0.695221 11.00000 0.11429 0.05129 = 0.08811 -0.01844 -0.00240 -0.05280 F10 5 0.143662 1.311429 0.631656 11.00000 0.07872 0.06106 = 0.03538 0.00458 -0.02820 -0.03449 F11 5 0.220679 1.195774 0.684354 11.00000 0.12101 0.05670 = 0.08149 -0.01549 -0.04773 -0.03900 F12 5 0.063046 1.260846 0.727263 11.00000 0.07378 0.18394 = 0.04253 -0.01426 -0.00891 -0.08608 F13 5 0.355065 1.437283 0.974413 11.00000 0.08512 0.04565 = 0.12085 -0.03504 -0.06351 -0.00882 F14 5 0.299467 1.487939 0.873353 11.00000 0.07615 0.03744 = 0.06442 -0.01073 0.01064 -0.03077 F15 5 0.169321 1.499357 0.959205 11.00000 0.05760 0.03429 = 0.07750 -0.03345 0.00944 -0.01340 F16 5 -0.084314 1.338560 1.019988 11.00000 0.04139 0.06862 = 0.08428 -0.04567 0.02199 -0.02320 F17 5 -0.096603 1.345150 0.916010 11.00000 0.04160 0.07682 = 0.07225 0.00716 -0.02993 -0.01648 F18 5 -0.041370 1.238217 0.989742 11.00000 0.03191 0.04825 = 0.05628 -0.01806 0.00150 -0.02063 F19 5 -0.304213 0.589624 0.484709 11.00000 0.11973 0.06638 = 0.04205 -0.03043 0.01396 -0.04400 F20 5 -0.489235 0.611896 0.519302 11.00000 0.08609 0.33534 = 0.28374 -0.27458 0.01384 -0.07198 F21 5 -0.356313 0.529188 0.582428 11.00000 0.31162 0.09770 = 0.07382 -0.05053 0.06312 -0.13039 F22 5 -0.142774 0.784581 0.469990 11.00000 0.10048 0.08548 = 0.06223 -0.03186 0.04155 -0.06244 F23 5 -0.275985 0.876328 0.500610 11.00000 0.07515 0.03709 = 0.09982 0.02077 0.00128 -0.02359 F24 5 -0.132039 0.804271 0.562373 11.00000 0.06530 0.10149 = 0.05790 -0.00792 0.00145 -0.05914 F25 5 -0.655692 0.853246 0.474608 11.00000 0.14135 0.07081 = 0.05658 -0.02969 -0.05781 -0.00066 F26 5 -0.819036 0.891476 0.534606 11.00000 0.07088 0.10581 = 0.06545 0.00932 -0.04635 -0.03774 F27 5 -0.718600 0.967169 0.476002 11.00000 0.11314 0.04994 = 0.05002 0.01121 -0.05253 -0.03060 F28 5 -0.592555 0.996513 0.719158 11.00000 0.07340 0.04982 = 0.04998 -0.02908 -0.00722 -0.00923 F29 5 -0.544230 1.042767 0.613468 11.00000 0.12556 0.03121 = 0.04818 0.00982 -0.04386 -0.03361 F30 5 -0.408841 0.960388 0.677776 11.00000 0.06440 0.04259 = 0.06776 -0.01717 -0.02332 -0.02318 F31 5 -0.900009 0.697883 0.712276 11.00000 0.04350 0.10088 = 0.05888 -0.01135 -0.02138 -0.03030 F32 5 -0.778052 0.585610 0.723343 11.00000 0.05483 0.09705 = 0.09960 -0.06719 0.01233 -0.04411 F33 5 -0.894569 0.614511 0.809237 11.00000 0.04137 0.08265 = 0.06331 -0.02360 0.00371 -0.03679 F34 5 -0.695994 0.730992 0.948384 11.00000 0.06383 0.06229 = 0.03944 -0.02809 0.00311 -0.00123 F35 5 -0.642725 0.611370 0.967599 11.00000 0.08366 0.05597 = 0.03077 0.00807 -0.01325 -0.04076 F36 5 -0.508015 0.670262 0.937785 11.00000 0.04636 0.06265 = 0.03130 -0.01406 -0.00879 -0.02125 S1 6 0.126827 0.916433 0.893777 11.00000 0.05051 0.03233 = 0.03643 0.00185 -0.01887 -0.02440 S2 6 -0.042386 0.815060 0.852045 11.00000 0.05558 0.03828 = 0.03770 0.00403 -0.02104 -0.02971 DY1 7 0.369546 1.229624 0.878026 11.00000 0.02590 0.02371 = 0.02124 -0.00774 -0.00209 -0.01143 DY2 7 -0.487461 0.729460 0.697343 11.00000 0.02640 0.02472 = 0.02030 -0.00446 -0.00476 -0.01090 C66 1 0.181300 0.684838 0.459462 11.00000 0.19002 0.19472 = 0.63924 0.16572 0.11061 0.04271 AFIX 33 H35 2 0.264934 0.673466 0.441962 11.00000 -1.50000 H36 2 0.130865 0.694378 0.424111 11.00000 -1.50000 H37 2 0.160481 0.728636 0.475179 11.00000 -1.50000 AFIX 0 C67 1 0.161865 0.618957 0.517757 11.00000 0.18869 0.25706 = 0.26753 -0.06845 0.09694 -0.01832 AFIX 23 H38 2 0.191742 0.576819 0.498540 11.00000 -1.20000 H39 2 0.220895 0.610541 0.548809 11.00000 -1.20000 AFIX 0 C68 1 0.062360 0.605561 0.559886 11.00000 0.13423 0.17377 = 0.39190 0.13681 -0.06660 -0.00210 AFIX 23 H40 2 0.009786 0.601826 0.530939 11.00000 -1.20000 H41 2 0.021313 0.651865 0.572143 11.00000 -1.20000 AFIX 0 C69 1 0.057817 0.547476 0.620488 11.00000 0.09544 0.26175 = 0.28090 -0.20436 0.01340 -0.04197 AFIX 23 H42 2 0.105280 0.499959 0.611951 11.00000 -1.20000 H43 2 0.096683 0.554540 0.654210 11.00000 -1.20000 AFIX 0 C70 1 -0.046689 0.542334 0.645655 11.00000 0.20982 0.18123 = 0.76968 0.16362 -0.18420 -0.09846 AFIX 23 H44 2 -0.082408 0.533754 0.611534 11.00000 -1.20000 H45 2 -0.094036 0.591631 0.650307 11.00000 -1.20000 AFIX 0 C71 1 -0.066459 0.491734 0.705214 11.00000 0.19126 0.45726 = 0.18483 -0.08298 -0.00882 0.11493 AFIX 23 H46 2 -0.067282 0.447897 0.693558 11.00000 -1.20000 H47 2 -0.148571 0.513140 0.722716 11.00000 -1.20000 AFIX 0 C72 1 0.011337 0.461626 0.765478 11.00000 0.30589 0.19913 = 0.41669 -0.13319 0.18515 -0.07844 AFIX 33 H48 2 -0.021143 0.426433 0.801711 11.00000 -1.50000 H49 2 0.093068 0.436816 0.751573 11.00000 -1.50000 H50 2 0.010972 0.502708 0.781020 11.00000 -1.50000 AFIX 0 HKLF 4 REM shelx in P -1 REM R1 = 0.0365 for 8283 Fo > 4sig(Fo) and 0.0434 for all 10338 data REM 1191 parameters refined using 0 restraints END WGHT 0.0658 0.0000 REM Highest difference peak 1.417, deepest hole -1.128, 1-sigma level 0.095 Q1 1 0.6009 1.3118 0.7287 11.00000 0.05 1.42 Q2 1 0.8585 1.1701 0.8780 11.00000 0.05 1.25 Q3 1 0.7383 1.2566 0.9099 11.00000 0.05 1.24 Q4 1 0.8060 1.2770 0.8205 11.00000 0.05 1.21 Q5 1 -0.6579 0.7721 0.4824 11.00000 0.05 1.10 Q6 1 0.7752 1.2723 0.9392 11.00000 0.05 0.90 Q7 1 -0.4440 0.7485 0.6416 11.00000 0.05 0.79 Q8 1 0.5495 1.3620 0.6477 11.00000 0.05 0.73 Q9 1 0.2569 0.8956 0.8483 11.00000 0.05 0.69 Q10 1 -0.2571 0.8108 0.5503 11.00000 0.05 0.66 Q11 1 -0.4581 0.5749 0.5553 11.00000 0.05 0.66 Q12 1 0.8988 1.1889 0.8202 11.00000 0.05 0.64 Q13 1 -0.1588 0.8440 0.8662 11.00000 0.05 0.60 Q14 1 -0.4831 0.5864 0.5410 11.00000 0.05 0.59 Q15 1 0.7774 1.1959 0.9436 11.00000 0.05 0.58 Q16 1 -0.4787 0.6792 0.4655 11.00000 0.05 0.54 Q17 1 -0.4629 0.6707 0.7299 11.00000 0.05 0.54 Q18 1 -0.1171 1.3752 0.9751 11.00000 0.05 0.50 Q19 1 0.3602 1.4573 0.6403 11.00000 0.05 0.50 Q20 1 0.2719 1.2263 0.8724 11.00000 0.05 0.50 Q21 1 0.0203 1.3339 0.7129 11.00000 0.05 0.48 Q22 1 0.4776 1.4255 0.6016 11.00000 0.05 0.48 Q23 1 -0.5814 0.7251 0.6922 11.00000 0.05 0.48 Q24 1 -0.0039 1.1236 0.5329 11.00000 0.05 0.47 Q25 1 0.2932 1.3438 0.9272 11.00000 0.05 0.45 ; _shelx_res_checksum 20726 _shelx_hkl_file ; 0 0 4 1530.23 604.097 1 0 0 -4 1411.88 393.08 1 0 0 4 2221.78 604.492 1 0 0 7327968.0 4586.54 1 0 0 8 154.539 316.413 1 0 0 8 285.079 674.713 1 0 0 9 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316985.00 3562.56 1 12 1 4 300.936 2073.09 1 12 1 5 841.923 1875.71 1 12 2 -332510.50 3883.63 1 12 2 -241559.60 3992.13 1 12 2 -184746.90 5016.69 1 12 2 0 1605.52 1247.93 1 12 2 1 481.332 1506.90 1 12 2 223150.70 5768.10 1 12 2 326518.00 3152.40 1 12 2 454916.90 3818.80 1 12 2 529285.00 3589.76 1 12 2 642096.00 4506.34 1 12 3 -311151.00 2449.00 1 12 3 -2 1954.61 1419.26 1 12 3 -1 3950.42 3954.79 1 12 3 0 7878.71 2175.26 1 12 3 1142449.0 6765.76 1 12 3 212226.20 2365.07 1 12 3 328141.80 3363.10 1 12 3 4-2.99734 1001.66 1 12 3 5 7187.51 2397.38 1 12 3 697197.40 5705.32 1 12 3 7 3255.77 1772.22 1 12 4 -4 623.825 1405.31 1 12 4 -3 3418.65 1899.72 1 12 4 -299345.50 5559.73 1 12 4 -152916.80 3626.67 1 12 4 021108.70 3083.44 1 12 4 1 842.141 1757.80 1 12 4 211152.10 2361.68 1 12 4 388358.00 6377.40 1 12 4 470952.40 4989.20 1 12 4 536817.80 3379.53 1 12 4 619334.00 5269.57 1 12 4 7 927.434 1397.91 1 12 5 -435600.00 3142.24 1 12 5 -3 2258.52 2426.67 1 12 5 -2 2869.48 2593.69 1 12 5 -117062.00 2770.71 1 12 5 0 9738.53 5571.93 1 12 5 1151841.0 7414.21 1 12 5 2 4441.72 2161.68 1 12 5 320264.80 3298.18 1 12 5 4 15.7044 1463.22 1 12 5 515489.50 3822.46 1 12 5 690364.60 5309.14 1 12 5 718083.70 2598.96 1 12 5 839847.50 3391.06 1 12 6 -5-108.385 1110.63 1 12 6 -4 1022.03 1697.84 1 12 6 -3 378.505 1705.66 1 12 6 -288537.40 5285.79 1 12 6 -163939.10 6279.05 1 12 6 0 6886.01 2305.55 1 12 6 1 174.616 1324.94 1 12 6 2 2462.53 2236.02 1 12 6 351280.90 3947.39 1 12 6 4 6564.47 2242.36 1 12 6 516586.30 2630.28 1 12 6 6 -128.37 1197.64 1 12 6 7 2584.37 2686.36 1 12 6 875056.40 4896.13 1 12 6 9 8963.32 4960.65 1 12 7 -5 3026.49 1969.80 1 12 7 -464844.70 4406.70 1 12 7 -316182.10 2608.25 1 12 7 -2 447.396 1339.13 1 12 7 -1 6069.27 2148.57 1 12 7 034823.00 4616.50 1 12 7 1146146.0 7135.14 1 12 7 2 1968.81 1688.03 1 12 7 360843.50 4241.60 1 12 7 417191.80 6217.37 1 12 7 552412.50 4042.53 1 12 7 617317.90 3040.50 1 12 7 770996.60 4752.85 1 12 7 881948.70 5750.95 1 12 7 9 1434.66 1669.73 1 12 8 -4 485.784 1349.90 1 12 8 -3 2419.11 1911.90 1 12 8 -266732.40 4431.73 1 12 8 -1 2398.46 2376.98 1 12 8 058347.70 4380.94 1 12 8 1 159.529 1673.83 1 12 8 2 641.912 1604.74 1 12 8 337631.70 3963.59 1 12 8 4 732.219 2358.25 1 12 8 540267.00 3471.94 1 12 8 6 665.867 2180.28 1 12 8 7 7899.48 2559.94 1 12 8 825881.60 3245.56 1 12 8 9 7877.34 2480.90 1 -12 -9 444751.40 5520.69 1 12 9 -126860.10 4292.35 1 12 9 057536.30 4720.83 1 12 9 164917.10 8404.95 1 12 9 213406.40 3194.25 1 12 9 3 6296.51 4199.72 1 12 9 4 2979.44 2261.04 1 12 9 539383.90 3710.94 1 12 9 613899.00 2791.65 1 12 9 736760.20 3614.77 1 12 9 830555.10 3362.73 1 12 9 1015985.20 3312.01 1 -12 -10 3 2276.77 2460.26 1 -12 -10 1 3293.72 3904.90 1 12 10 1 4353.88 3003.49 1 12 10 2 5396.32 2500.04 1 12 10 3129383.0 8151.75 1 12 10 4 2027.82 2120.59 1 12 10 5131791.0 7569.13 1 12 10 6 951.657 2233.36 1 12 10 7 4209.04 2062.25 1 12 10 821097.30 3182.92 1 12 10 910253.20 6399.15 1 -12 -11 -119186.90 5205.64 1 12 11 322797.30 5758.08 1 12 11 4 709.86 2186.85 1 12 11 532811.10 4235.86 1 12 11 6 4810.56 2720.52 1 12 11 7114032.0 6677.66 1 12 11 824273.70 3124.36 1 12 12 6 6962.49 2792.37 1 12 12 6 7618.13 2103.81 1 12 12 719639.80 2986.99 1 12 12 842047.50 3514.93 1 12 12 971217.60 4425.71 1 12 12 11 3646.24 1533.65 1 12 12 12 2387.13 1976.20 1 12 13 6 785.077 1497.37 1 12 13 778998.00 5036.87 1 12 13 814708.50 2896.06 1 12 13 9 1862.75 1216.73 1 12 13 1016554.30 2543.68 1 12 13 11 2063.72 1188.61 1 12 13 1275235.70 4422.51 1 12 13 13 4869.28 1547.03 1 12 14 7 2177.07 1743.65 1 12 14 8 4938.33 1776.90 1 12 14 9129794.0 6534.57 1 12 14 1062561.70 4146.91 1 12 14 1114209.00 2629.42 1 12 14 12 3841.79 1724.22 1 12 15 748841.50 4633.45 1 12 15 8 199.147 1604.50 1 12 15 9 4005.41 1896.46 1 0 0 0 0.00 0.00 1 ; _shelx_hkl_checksum 24426 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4519(5) 1.1903(3) 1.0364(2) 0.0332(14) Uani 1 1 d . . . . . H1 H 0.4663 1.2367 1.0152 0.040 Uiso 1 1 calc R U . . . C2 C 0.4740(6) 1.1553(4) 1.1044(3) 0.0398(16) Uani 1 1 d . . . . . H2 H 0.4993 1.1785 1.1293 0.048 Uiso 1 1 calc R U . . . C3 C 0.4574(6) 1.0857(4) 1.1336(3) 0.0483(18) Uani 1 1 d . . . . . H3 H 0.4736 1.0604 1.1786 0.058 Uiso 1 1 calc R U . . . C4 C 0.4167(6) 1.0530(4) 1.0966(3) 0.0412(16) Uani 1 1 d . . . . . H4 H 0.4063 1.0053 1.1162 0.049 Uiso 1 1 calc R U . . . C5 C 0.3915(5) 1.0918(3) 1.0298(2) 0.0258(13) Uani 1 1 d . . . . . C6 C 0.3420(5) 1.0619(3) 0.9867(2) 0.0232(12) Uani 1 1 d . . . . . C7 C 0.3161(5) 0.9939(3) 1.0105(3) 0.0309(14) Uani 1 1 d . . . . . H5 H 0.3346 0.9629 1.0540 0.037 Uiso 1 1 calc R U . . . C8 C 0.2628(5) 0.9715(3) 0.9699(2) 0.0312(14) Uani 1 1 d . . . . . H6 H 0.2450 0.9257 0.9860 0.037 Uiso 1 1 calc R U . . . C9 C 0.2358(5) 1.0182(3) 0.9047(2) 0.0272(13) Uani 1 1 d . . . . . C10 C 0.2698(5) 1.0844(3) 0.8831(2) 0.0274(13) Uani 1 1 d . . . . . H7 H 0.2556 1.1151 0.8390 0.033 Uiso 1 1 calc R U . . . C11 C 0.1728(5) 0.9989(3) 0.8611(2) 0.0281(13) Uani 1 1 d . . . . . C12 C 0.1413(5) 1.0382(3) 0.7968(3) 0.0359(15) Uani 1 1 d . . . . . H8 H 0.1609 1.0826 0.7730 0.043 Uiso 1 1 calc R U . . . C13 C 0.0761(6) 1.0064(3) 0.7687(3) 0.0372(15) Uani 1 1 d . . . . . C14A C 0.023(2) 0.9485(11) 0.8250(7) 0.026(5) Uani 0.51(3) 1 d . . P A 1 C15A C -0.106(2) 0.9820(12) 0.8556(10) 0.035(5) Uani 0.51(3) 1 d . . P A 1 H9A H -0.1043 1.0202 0.8746 0.052 Uiso 0.51(3) 1 calc R U P A 1 H11A H -0.1609 1.0038 0.8206 0.052 Uiso 0.51(3) 1 calc R U P A 1 H10A H -0.1313 0.9429 0.8906 0.052 Uiso 0.51(3) 1 calc R U P A 1 C14B C 0.088(3) 0.9223(11) 0.8101(9) 0.034(6) Uani 0.49(3) 1 d . . P A 2 C21B C -0.136(2) 0.9684(13) 0.8449(11) 0.036(5) Uani 0.49(3) 1 d . . P A 2 H18B H -0.2130 0.9602 0.8452 0.055 Uiso 0.49(3) 1 calc R U P A 2 H20B H -0.1200 0.9601 0.8908 0.055 Uiso 0.49(3) 1 calc R U P A 2 H19B H -0.1393 1.0192 0.8190 0.055 Uiso 0.49(3) 1 calc R U P A 2 C16 C 0.0331(5) 1.0288(3) 0.7059(2) 0.0269(13) Uani 1 1 d . . . . . C17 C 0.0424(6) 1.0955(3) 0.6466(3) 0.0368(15) Uani 1 1 d . . . . . H13 H 0.1230 1.1017 0.6399 0.044 Uiso 1 1 calc R U . . . H12 H -0.0167 1.1414 0.6530 0.044 Uiso 1 1 calc R U . . . C18 C 0.0156(7) 1.0759(4) 0.5866(3) 0.0509(19) Uani 1 1 d . . . . . H15 H 0.0904 1.0503 0.5648 0.061 Uiso 1 1 calc R U . . . H14 H -0.0251 1.1212 0.5532 0.061 Uiso 1 1 calc R U . . . C19 C -0.0665(6) 1.0243(3) 0.6161(3) 0.0373(15) Uani 1 1 d . . . . . H16 H -0.1516 1.0530 0.6144 0.045 Uiso 1 1 calc R U . . . H17 H -0.0499 0.9870 0.5918 0.045 Uiso 1 1 calc R U . . . C20 C -0.0328(5) 0.9873(3) 0.6894(2) 0.0266(13) Uani 1 1 d . . . . . C21A C 0.1605(18) 0.8492(9) 0.7675(9) 0.031(4) Uani 0.51(3) 1 d . . P A 1 H18A H 0.1600 0.8110 0.7482 0.047 Uiso 0.51(3) 1 calc R U P A 1 H19A H 0.1918 0.8866 0.7335 0.047 Uiso 0.51(3) 1 calc R U P A 1 H20A H 0.2109 0.8267 0.8049 0.047 Uiso 0.51(3) 1 calc R U P A 1 C22A C 0.028(2) 0.8870(11) 0.7936(9) 0.032(6) Uani 0.51(3) 1 d . . P A 1 C15B C 0.1932(18) 0.8634(11) 0.7804(10) 0.039(5) Uani 0.49(3) 1 d . . P A 2 H9B H 0.2696 0.8719 0.7801 0.059 Uiso 0.49(3) 1 calc R U P A 2 H10B H 0.1952 0.8133 0.8082 0.059 Uiso 0.49(3) 1 calc R U P A 2 H11B H 0.1788 0.8691 0.7348 0.059 Uiso 0.49(3) 1 calc R U P A 2 C22B C -0.036(2) 0.9137(12) 0.8128(9) 0.036(6) Uani 0.49(3) 1 d . . P A 2 C23 C -0.0552(5) 0.9256(3) 0.7346(3) 0.0315(14) Uani 1 1 d . . . . . C24 C -0.1192(5) 0.8760(3) 0.7309(3) 0.0325(14) Uani 1 1 d . . . . . H21 H -0.1562 0.8838 0.6921 0.039 Uiso 1 1 calc R U . . . C25 C -0.1226(5) 0.8184(3) 0.7857(3) 0.0338(14) Uani 1 1 d . . . . . C26 C -0.2608(5) 0.7617(3) 0.7552(2) 0.0273(13) Uani 1 1 d . . . . . H22 H -0.2829 0.8051 0.7191 0.033 Uiso 1 1 calc R U . . . C27 C -0.1782(5) 0.7584(3) 0.7974(2) 0.0273(13) Uani 1 1 d . . . . . C28 C -0.1535(5) 0.6936(3) 0.8530(3) 0.0330(14) Uani 1 1 d . . . . . H23 H -0.1035 0.6895 0.8849 0.040 Uiso 1 1 calc R U . . . C29 C -0.2019(5) 0.6362(3) 0.8610(3) 0.0304(14) Uani 1 1 d . . . . . H24 H -0.1829 0.5928 0.8973 0.036 Uiso 1 1 calc R U . . . C30 C -0.2795(5) 0.6431(3) 0.8146(2) 0.0232(12) Uani 1 1 d . . . . . C31 C -0.3312(5) 0.5828(3) 0.8179(2) 0.0223(12) Uani 1 1 d . . . . . C32 C -0.3093(5) 0.5147(3) 0.8684(2) 0.0286(13) Uani 1 1 d . . . . . H25 H -0.2635 0.5065 0.9037 0.034 Uiso 1 1 calc R U . . . C33 C -0.3553(5) 0.4591(3) 0.8666(3) 0.0339(14) Uani 1 1 d . . . . . H26 H -0.3416 0.4136 0.9008 0.041 Uiso 1 1 calc R U . . . C34 C -0.4221(5) 0.4716(3) 0.8131(2) 0.0309(14) Uani 1 1 d . . . . . H27 H -0.4522 0.4346 0.8099 0.037 Uiso 1 1 calc R U . . . C35 C -0.4422(5) 0.5411(3) 0.7649(2) 0.0253(13) Uani 1 1 d . . . . . H28 H -0.4881 0.5502 0.7293 0.030 Uiso 1 1 calc R U . . . C36 C 0.7705(6) 1.2257(4) 0.8637(3) 0.0348(15) Uani 1 1 d . . . . . C37 C 0.6638(6) 1.2087(3) 0.8475(3) 0.0313(14) Uani 1 1 d . . . . . C38 C 0.6784(5) 1.1862(3) 0.7881(3) 0.0333(14) Uani 1 1 d . . . . . H29 H 0.7474 1.1880 0.7582 0.040 Uiso 1 1 calc R U . . . C39 C 0.5911(6) 1.1616(3) 0.7742(3) 0.0308(14) Uani 1 1 d . . . . . C40 C 0.6158(6) 1.1314(4) 0.7121(3) 0.0416(16) Uani 1 1 d . . . . . C41 C 0.4642(7) 1.4040(4) 0.6777(3) 0.0467(18) Uani 1 1 d . . . . . C42 C 0.3938(5) 1.3488(3) 0.7231(3) 0.0323(14) Uani 1 1 d . . . . . C43 C 0.3142(6) 1.3316(3) 0.6929(3) 0.0381(16) Uani 1 1 d . . . . . H30 H 0.3064 1.3527 0.6464 0.046 Uiso 1 1 calc R U . . . C44 C 0.2465(5) 1.2840(3) 0.7303(3) 0.0329(14) Uani 1 1 d . . . . . C45 C 0.1646(7) 1.2645(4) 0.6935(3) 0.0473(18) Uani 1 1 d . . . . . C46 C 0.2676(6) 1.4512(3) 0.9362(3) 0.0400(16) Uani 1 1 d . . . . . C47 C 0.2431(6) 1.3795(3) 0.9362(2) 0.0263(13) Uani 1 1 d . . . . . C48 C 0.1290(5) 1.3712(3) 0.9547(3) 0.0294(13) Uani 1 1 d . . . . . H31 H 0.0688 1.4079 0.9708 0.035 Uiso 1 1 calc R U . . . C49 C 0.1002(5) 1.3097(3) 0.9502(2) 0.0289(14) Uani 1 1 d . . . . . C50 C -0.0321(5) 1.3076(4) 0.9689(3) 0.0375(15) Uani 1 1 d . . . . . C51 C -0.3853(9) 0.5987(5) 0.5361(4) 0.074(3) Uani 1 1 d . . . . . C52 C -0.3765(6) 0.6571(4) 0.5675(3) 0.0386(16) Uani 1 1 d . . . . . C53 C -0.3047(6) 0.7042(4) 0.5333(3) 0.0464(17) Uani 1 1 d . . . . . H32 H -0.2643 0.7008 0.4913 0.056 Uiso 1 1 calc R U . . . C54 C -0.2929(5) 0.7563(3) 0.5615(3) 0.0308(14) Uani 1 1 d . . . . . C55 C -0.2138(6) 0.8059(3) 0.5251(3) 0.0461(17) Uani 1 1 d . . . . . C56 C -0.7053(7) 0.8964(4) 0.5137(3) 0.0477(18) Uani 1 1 d . . . . . C57 C -0.6346(5) 0.8739(4) 0.5760(3) 0.0359(15) Uani 1 1 d . . . . . C58 C -0.6074(5) 0.9306(3) 0.5918(3) 0.0356(15) Uani 1 1 d . . . . . H33 H -0.6272 0.9794 0.5627 0.043 Uiso 1 1 calc R U . . . C59 C -0.5512(5) 0.9151(3) 0.6506(3) 0.0294(13) Uani 1 1 d . . . . . C60 C -0.5267(6) 0.9803(3) 0.6652(3) 0.0389(16) Uani 1 1 d . . . . . C61 C -0.8255(6) 0.6399(4) 0.7535(3) 0.0441(17) Uani 1 1 d . . . . . C62 C -0.7244(5) 0.6646(3) 0.7692(3) 0.0316(14) Uani 1 1 d . . . . . C63 C -0.7099(5) 0.6567(3) 0.8358(3) 0.0323(14) Uani 1 1 d . . . . . H34 H -0.7561 0.6317 0.8708 0.039 Uiso 1 1 calc R U . . . C64 C -0.6282(5) 0.6852(3) 0.8519(2) 0.0242(12) Uani 1 1 d . . . . . C65 C -0.6183(6) 0.6744(3) 0.9271(3) 0.0335(14) Uani 1 1 d . . . . . N1 N 0.4101(4) 1.1590(2) 1.0001(2) 0.0263(11) Uani 1 1 d . . . . . N2 N 0.3213(4) 1.1061(2) 0.92210(19) 0.0217(10) Uani 1 1 d . . . . . N3 N -0.3103(4) 0.7071(2) 0.76277(19) 0.0245(10) Uani 1 1 d . . . . . N4 N -0.3994(4) 0.5963(2) 0.76632(19) 0.0250(10) Uani 1 1 d . . . . . O1 O 0.5721(3) 1.2174(2) 0.88814(17) 0.0282(9) Uani 1 1 d . . . . . O2 O 0.4915(4) 1.1578(2) 0.80823(17) 0.0306(9) Uani 1 1 d . . . . . O3 O 0.4177(3) 1.3241(2) 0.78408(16) 0.0298(9) Uani 1 1 d . . . . . O4 O 0.2455(3) 1.2505(2) 0.79370(16) 0.0290(9) Uani 1 1 d . . . . . O5 O 0.3367(4) 1.3333(2) 0.91680(17) 0.0292(9) Uani 1 1 d . . . . . O6 O 0.1699(3) 1.2565(2) 0.92901(17) 0.0282(9) Uani 1 1 d . . . . . O7 O -0.4384(4) 0.6563(2) 0.62313(17) 0.0327(9) Uani 1 1 d . . . . . O8 O -0.3412(3) 0.7685(2) 0.61692(16) 0.0316(9) Uani 1 1 d . . . . . O9 O -0.6091(4) 0.8057(2) 0.60746(17) 0.0351(10) Uani 1 1 d . . . . . O10 O -0.5210(3) 0.85376(19) 0.69653(16) 0.0273(9) Uani 1 1 d . . . . . O11 O -0.6606(3) 0.6896(2) 0.71733(17) 0.0324(9) Uani 1 1 d . . . . . O12 O -0.5625(3) 0.72277(19) 0.81099(16) 0.0249(8) Uani 1 1 d . . . . . F1 F 0.7538(7) 1.2890(4) 0.8602(7) 0.254(7) Uani 1 1 d . . . . . F2 F 0.8649(6) 1.2126(7) 0.8288(4) 0.206(5) Uani 1 1 d . . . . . F3 F 0.8012(8) 1.1915(6) 0.9204(3) 0.226(6) Uani 1 1 d . . . . . F4 F 0.7021(4) 1.1534(3) 0.66806(19) 0.0805(15) Uani 1 1 d . . . . . F5 F 0.6509(4) 1.0570(2) 0.73131(19) 0.0637(12) Uani 1 1 d . . . . . F6 F 0.5177(4) 1.1536(3) 0.67954(19) 0.0793(15) Uani 1 1 d . . . . . F7 F 0.5797(5) 1.3814(3) 0.6908(3) 0.0930(16) Uani 1 1 d . . . . . F8 F 0.4573(7) 1.4198(4) 0.61429(19) 0.144(3) Uani 1 1 d . . . . . F9 F 0.4225(5) 1.4672(2) 0.6952(2) 0.0784(13) Uani 1 1 d . . . . . F10 F 0.1437(4) 1.3114(2) 0.63166(15) 0.0562(10) Uani 1 1 d . . . . . F11 F 0.2207(4) 1.1958(2) 0.6844(2) 0.0787(14) Uani 1 1 d . . . . . F12 F 0.0630(4) 1.2608(3) 0.72726(19) 0.0916(17) Uani 1 1 d . . . . . F13 F 0.3551(4) 1.4373(2) 0.9744(2) 0.0762(14) Uani 1 1 d . . . . . F14 F 0.2995(4) 1.4879(2) 0.87335(19) 0.0589(11) Uani 1 1 d . . . . . F15 F 0.1693(4) 1.4994(2) 0.95921(19) 0.0540(10) Uani 1 1 d . . . . . F16 F -0.0843(3) 1.3386(2) 1.0200(2) 0.0605(11) Uani 1 1 d . . . . . F17 F -0.0966(3) 1.3451(2) 0.91601(19) 0.0676(12) Uani 1 1 d . . . . . F18 F -0.0414(3) 1.2382(2) 0.98974(16) 0.0431(9) Uani 1 1 d . . . . . F19 F -0.3042(4) 0.5896(2) 0.48471(18) 0.0707(13) Uani 1 1 d . . . . . F20 F -0.4892(6) 0.6119(5) 0.5193(4) 0.189(4) Uani 1 1 d . . . . . F21 F -0.3563(8) 0.5292(3) 0.5824(3) 0.147(3) Uani 1 1 d . . . . . F22 F -0.1428(4) 0.7846(3) 0.4700(2) 0.0774(14) Uani 1 1 d . . . . . F23 F -0.2760(4) 0.8763(2) 0.5006(2) 0.0802(14) Uani 1 1 d . . . . . F24 F -0.1320(4) 0.8043(3) 0.56237(18) 0.0706(12) Uani 1 1 d . . . . . F25 F -0.6557(5) 0.8532(3) 0.4746(2) 0.0877(17) Uani 1 1 d . . . . . F26 F -0.8190(4) 0.8915(3) 0.5346(2) 0.0807(14) Uani 1 1 d . . . . . F27 F -0.7186(4) 0.9672(2) 0.47600(17) 0.0695(13) Uani 1 1 d . . . . . F28 F -0.5926(4) 0.9965(2) 0.71916(17) 0.0559(11) Uani 1 1 d . . . . . F29 F -0.5442(4) 1.04277(19) 0.61347(17) 0.0659(12) Uani 1 1 d . . . . . F30 F -0.4088(4) 0.9604(2) 0.67778(18) 0.0535(10) Uani 1 1 d . . . . . F31 F -0.9000(3) 0.6979(3) 0.71228(19) 0.0659(12) Uani 1 1 d . . . . . F32 F -0.7781(4) 0.5856(3) 0.7233(2) 0.0708(13) Uani 1 1 d . . . . . F33 F -0.8946(3) 0.6145(2) 0.80924(18) 0.0580(10) Uani 1 1 d . . . . . F34 F -0.6960(4) 0.7310(2) 0.94838(16) 0.0571(11) Uani 1 1 d . . . . . F35 F -0.6427(4) 0.6114(2) 0.96760(15) 0.0556(10) Uani 1 1 d . . . . . F36 F -0.5080(3) 0.6703(2) 0.93778(15) 0.0445(9) Uani 1 1 d . . . . . S1 S 0.12683(15) 0.91643(8) 0.89378(7) 0.0375(4) Uani 1 1 d . . . . . S2 S -0.04239(15) 0.81506(9) 0.85205(7) 0.0412(4) Uani 1 1 d . . . . . Dy1 Dy 0.36955(2) 1.22962(2) 0.87803(2) 0.02218(10) Uani 1 1 d . . . . . Dy2 Dy -0.48746(2) 0.72946(2) 0.69734(2) 0.02304(10) Uani 1 1 d . . . . . C66 C 0.181(2) 0.6848(14) 0.4595(19) 0.46(3) Uani 1 1 d . . . . . H35 H 0.2649 0.6735 0.4420 0.688 Uiso 1 1 calc R U . . . H36 H 0.1309 0.6944 0.4241 0.688 Uiso 1 1 calc R U . . . H37 H 0.1605 0.7286 0.4752 0.688 Uiso 1 1 calc R U . . . C67 C 0.162(2) 0.6190(16) 0.5178(12) 0.267(13) Uani 1 1 d . . . . . H38 H 0.1917 0.5768 0.4985 0.320 Uiso 1 1 calc R U . . . H39 H 0.2209 0.6105 0.5488 0.320 Uiso 1 1 calc R U . . . C68 C 0.062(2) 0.6056(11) 0.5599(16) 0.294(18) Uani 1 1 d . . . . . H40 H 0.0098 0.6018 0.5309 0.352 Uiso 1 1 calc R U . . . H41 H 0.0213 0.6519 0.5721 0.352 Uiso 1 1 calc R U . . . C69 C 0.0578(14) 0.5475(13) 0.6205(11) 0.187(9) Uani 1 1 d . . . . . H42 H 0.1053 0.5000 0.6120 0.224 Uiso 1 1 calc R U . . . H43 H 0.0967 0.5545 0.6542 0.224 Uiso 1 1 calc R U . . . C70 C -0.047(3) 0.5423(14) 0.646(3) 0.43(3) Uani 1 1 d . . . . . H44 H -0.0824 0.5338 0.6115 0.519 Uiso 1 1 calc R U . . . H45 H -0.0940 0.5916 0.6503 0.519 Uiso 1 1 calc R U . . . C71 C -0.066(2) 0.492(2) 0.7052(12) 0.33(3) Uani 1 1 d . . . . . H46 H -0.0673 0.4479 0.6936 0.402 Uiso 1 1 calc R U . . . H47 H -0.1486 0.5131 0.7227 0.402 Uiso 1 1 calc R U . . . C72 C 0.011(3) 0.4616(14) 0.7655(17) 0.324(17) Uani 1 1 d . . . . . H48 H -0.0211 0.4264 0.8017 0.485 Uiso 1 1 calc R U . . . H49 H 0.0931 0.4368 0.7516 0.485 Uiso 1 1 calc R U . . . H50 H 0.0110 0.5027 0.7810 0.485 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 C1 0.043(4) 0.039(4) 0.026(3) -0.012(3) -0.009(3) -0.017(3) C2 0.054(4) 0.051(4) 0.026(3) -0.011(3) -0.008(3) -0.028(4) C3 0.074(5) 0.055(5) 0.024(3) -0.004(3) -0.017(3) -0.030(4) C4 0.058(5) 0.042(4) 0.029(3) -0.005(3) -0.007(3) -0.025(3) C5 0.025(3) 0.033(3) 0.023(3) -0.010(3) 0.001(2) -0.012(3) C6 0.021(3) 0.027(3) 0.023(3) -0.009(2) 0.001(2) -0.009(3) C7 0.033(4) 0.036(4) 0.026(3) -0.008(3) -0.002(2) -0.013(3) C8 0.038(4) 0.034(3) 0.028(3) -0.005(3) -0.003(3) -0.022(3) C9 0.032(4) 0.025(3) 0.028(3) -0.006(2) -0.007(2) -0.012(3) C10 0.033(4) 0.025(3) 0.026(3) -0.006(2) -0.012(2) -0.007(3) C11 0.034(4) 0.026(3) 0.029(3) -0.003(2) -0.008(2) -0.015(3) C12 0.046(4) 0.039(4) 0.032(3) -0.003(3) -0.004(3) -0.031(3) C13 0.054(4) 0.038(4) 0.029(3) 0.000(3) -0.011(3) -0.030(3) C14A 0.031(13) 0.026(10) 0.025(7) -0.011(6) -0.001(8) -0.012(9) C15A 0.042(13) 0.041(11) 0.031(9) -0.015(7) -0.013(8) -0.016(8) C14B 0.045(14) 0.027(10) 0.034(8) -0.011(7) -0.010(9) -0.011(10) C21B 0.037(12) 0.050(12) 0.031(9) -0.019(8) -0.002(8) -0.017(9) C16 0.031(4) 0.028(3) 0.025(3) -0.005(2) -0.002(2) -0.015(3) C17 0.043(4) 0.039(4) 0.033(3) -0.003(3) -0.006(3) -0.025(3) C18 0.077(5) 0.061(5) 0.028(3) 0.003(3) -0.015(3) -0.048(4) C19 0.047(4) 0.042(4) 0.031(3) -0.007(3) -0.009(3) -0.024(3) C20 0.026(3) 0.030(3) 0.026(3) -0.009(3) -0.005(2) -0.008(3) C21A 0.020(10) 0.023(8) 0.059(9) -0.016(6) -0.015(7) -0.006(6) C22A 0.046(14) 0.023(9) 0.039(8) -0.007(7) -0.011(8) -0.023(9) C15B 0.031(11) 0.032(10) 0.056(10) -0.005(7) -0.019(8) -0.012(8) C22B 0.056(14) 0.025(10) 0.028(8) -0.006(7) -0.010(9) -0.013(11) C23 0.034(4) 0.031(3) 0.034(3) -0.005(3) -0.015(3) -0.012(3) C24 0.038(4) 0.034(3) 0.032(3) -0.003(3) -0.015(3) -0.019(3) C25 0.034(4) 0.036(4) 0.038(3) -0.007(3) -0.013(3) -0.016(3) C26 0.033(4) 0.025(3) 0.024(3) -0.001(2) -0.005(2) -0.011(3) C27 0.027(3) 0.028(3) 0.030(3) -0.005(2) -0.006(2) -0.013(3) C28 0.038(4) 0.039(4) 0.032(3) -0.007(3) -0.008(3) -0.024(3) C29 0.031(4) 0.029(3) 0.029(3) -0.002(2) -0.006(3) -0.009(3) C30 0.018(3) 0.025(3) 0.025(3) -0.009(2) 0.001(2) -0.005(2) C31 0.016(3) 0.026(3) 0.025(3) -0.012(2) 0.003(2) -0.005(2) C32 0.032(4) 0.028(3) 0.027(3) -0.008(3) -0.005(2) -0.010(3) C33 0.041(4) 0.027(3) 0.033(3) -0.005(3) -0.004(3) -0.011(3) C34 0.038(4) 0.029(3) 0.031(3) -0.010(3) -0.005(3) -0.014(3) C35 0.029(3) 0.028(3) 0.023(3) -0.008(2) -0.002(2) -0.012(3) C36 0.028(4) 0.044(4) 0.039(3) -0.012(3) 0.006(3) -0.024(3) C37 0.035(4) 0.021(3) 0.039(3) -0.005(3) -0.011(3) -0.009(3) C38 0.034(4) 0.035(4) 0.031(3) -0.010(3) 0.008(3) -0.015(3) C39 0.033(4) 0.028(3) 0.029(3) -0.010(3) -0.001(3) -0.006(3) C40 0.040(4) 0.047(4) 0.042(3) -0.023(3) 0.004(3) -0.013(4) C41 0.073(6) 0.053(5) 0.030(3) -0.003(3) -0.013(3) -0.042(4) C42 0.045(4) 0.030(3) 0.028(3) -0.013(3) 0.006(3) -0.019(3) C43 0.064(5) 0.032(4) 0.024(3) -0.001(3) -0.007(3) -0.025(3) C44 0.039(4) 0.036(4) 0.028(3) -0.008(3) -0.010(3) -0.013(3) C45 0.058(5) 0.059(5) 0.029(3) -0.003(3) -0.005(3) -0.031(4) C46 0.049(5) 0.029(4) 0.045(4) -0.011(3) -0.013(3) -0.010(3) C47 0.035(4) 0.021(3) 0.024(3) -0.006(2) -0.008(3) -0.007(3) C48 0.029(4) 0.026(3) 0.034(3) -0.014(3) -0.005(3) -0.002(3) C49 0.029(4) 0.032(4) 0.025(3) -0.002(3) -0.007(3) -0.010(3) C50 0.027(4) 0.039(4) 0.048(4) -0.018(3) -0.008(3) -0.005(3) C51 0.117(8) 0.084(7) 0.045(4) -0.037(5) 0.022(5) -0.056(6) C52 0.052(4) 0.047(4) 0.026(3) -0.015(3) 0.000(3) -0.023(3) C53 0.069(5) 0.053(4) 0.023(3) -0.010(3) 0.009(3) -0.033(4) C54 0.035(4) 0.030(3) 0.024(3) -0.002(3) 0.002(3) -0.013(3) C55 0.064(5) 0.027(4) 0.046(4) 0.003(3) -0.018(4) -0.018(3) C56 0.060(5) 0.049(5) 0.037(3) 0.001(3) -0.027(3) -0.020(4) C57 0.034(4) 0.044(4) 0.031(3) -0.008(3) -0.014(3) -0.010(3) C58 0.050(4) 0.030(3) 0.026(3) 0.001(3) -0.016(3) -0.012(3) C59 0.032(4) 0.024(3) 0.029(3) -0.003(3) -0.006(3) -0.007(3) C60 0.053(5) 0.028(4) 0.034(3) -0.002(3) -0.020(3) -0.007(3) C61 0.031(4) 0.062(5) 0.046(4) -0.022(4) 0.006(3) -0.020(4) C62 0.026(4) 0.032(3) 0.040(3) -0.013(3) -0.002(3) -0.010(3) C63 0.035(4) 0.030(3) 0.033(3) -0.007(3) 0.005(3) -0.017(3) C64 0.021(3) 0.022(3) 0.026(3) -0.008(2) 0.000(2) -0.001(3) C65 0.034(4) 0.033(4) 0.031(3) -0.004(3) -0.001(3) -0.012(3) N1 0.031(3) 0.028(3) 0.023(2) -0.010(2) -0.004(2) -0.009(2) N2 0.023(3) 0.019(2) 0.024(2) -0.0070(19) -0.0048(19) -0.005(2) N3 0.024(3) 0.029(3) 0.022(2) -0.002(2) -0.0008(19) -0.015(2) N4 0.024(3) 0.029(3) 0.025(2) -0.010(2) -0.0029(19) -0.007(2) O1 0.026(2) 0.036(2) 0.0257(18) -0.0104(17) 0.0025(18) -0.0140(19) O2 0.036(3) 0.030(2) 0.0322(19) -0.0164(18) 0.0026(19) -0.013(2) O3 0.038(3) 0.031(2) 0.0245(19) -0.0095(17) 0.0016(16) -0.0167(19) O4 0.033(2) 0.032(2) 0.0239(19) -0.0046(17) -0.0056(16) -0.0142(19) O5 0.031(3) 0.033(2) 0.0297(19) -0.0144(18) -0.0012(17) -0.012(2) O6 0.026(2) 0.029(2) 0.0327(19) -0.0122(18) 0.0004(17) -0.0101(19) O7 0.042(3) 0.036(2) 0.029(2) -0.0132(18) 0.0005(18) -0.020(2) O8 0.037(3) 0.033(2) 0.025(2) -0.0035(17) -0.0012(17) -0.016(2) O9 0.048(3) 0.031(2) 0.030(2) -0.0035(19) -0.0169(19) -0.014(2) O10 0.033(2) 0.024(2) 0.0255(18) -0.0047(17) -0.0063(17) -0.0079(18) O11 0.027(2) 0.043(3) 0.033(2) -0.0138(19) -0.0028(18) -0.015(2) O12 0.026(2) 0.026(2) 0.0254(18) -0.0084(16) -0.0013(16) -0.0098(18) F1 0.123(6) 0.079(5) 0.63(2) -0.123(8) -0.204(10) -0.002(4) F2 0.079(5) 0.470(16) 0.212(7) -0.240(10) 0.064(5) -0.163(7) F3 0.205(8) 0.404(14) 0.110(5) 0.091(6) -0.102(5) -0.257(9) F4 0.110(4) 0.108(4) 0.056(2) -0.056(3) 0.042(2) -0.068(3) F5 0.090(3) 0.044(3) 0.069(2) -0.035(2) -0.011(2) -0.014(2) F6 0.066(3) 0.112(4) 0.059(2) -0.057(3) -0.026(2) 0.018(3) F7 0.070(4) 0.090(4) 0.106(4) 0.005(3) 0.012(3) -0.050(3) F8 0.281(8) 0.215(6) 0.027(2) -0.003(3) -0.002(3) -0.228(6) F9 0.114(4) 0.051(3) 0.088(3) -0.018(2) -0.002(3) -0.053(3) F10 0.079(3) 0.061(3) 0.0354(19) 0.0046(17) -0.0282(18) -0.034(2) F11 0.121(4) 0.057(3) 0.081(3) -0.015(2) -0.048(3) -0.039(3) F12 0.074(3) 0.184(5) 0.043(2) -0.014(3) -0.009(2) -0.086(4) F13 0.085(3) 0.046(2) 0.121(3) -0.035(2) -0.064(3) -0.009(2) F14 0.076(3) 0.037(2) 0.064(2) -0.0107(19) 0.011(2) -0.031(2) F15 0.058(3) 0.034(2) 0.078(2) -0.033(2) 0.009(2) -0.013(2) F16 0.041(3) 0.069(3) 0.084(3) -0.046(2) 0.022(2) -0.023(2) F17 0.042(2) 0.077(3) 0.072(2) 0.007(2) -0.030(2) -0.016(2) F18 0.032(2) 0.048(2) 0.056(2) -0.0181(18) 0.0015(16) -0.0206(17) F19 0.120(4) 0.066(3) 0.042(2) -0.030(2) 0.014(2) -0.044(3) F20 0.086(5) 0.335(11) 0.284(9) -0.275(9) 0.014(5) -0.072(6) F21 0.312(10) 0.098(5) 0.074(3) -0.051(3) 0.063(4) -0.130(6) F22 0.100(4) 0.085(3) 0.062(3) -0.032(2) 0.042(2) -0.062(3) F23 0.075(3) 0.037(3) 0.100(3) 0.021(2) 0.001(3) -0.024(2) F24 0.065(3) 0.101(4) 0.058(2) -0.008(2) 0.001(2) -0.059(3) F25 0.141(5) 0.071(3) 0.057(2) -0.030(2) -0.058(3) -0.001(3) F26 0.071(3) 0.106(4) 0.065(3) 0.009(2) -0.046(2) -0.038(3) F27 0.113(4) 0.050(3) 0.050(2) 0.0112(19) -0.053(2) -0.031(2) F28 0.073(3) 0.050(2) 0.050(2) -0.0291(19) -0.007(2) -0.009(2) F29 0.126(4) 0.031(2) 0.048(2) 0.0098(17) -0.044(2) -0.034(2) F30 0.064(3) 0.043(2) 0.068(2) -0.0172(19) -0.023(2) -0.023(2) F31 0.044(2) 0.101(3) 0.059(2) -0.011(2) -0.021(2) -0.030(2) F32 0.055(3) 0.097(3) 0.100(3) -0.067(3) 0.012(2) -0.044(3) F33 0.041(2) 0.083(3) 0.063(2) -0.024(2) 0.0037(19) -0.037(2) F34 0.064(3) 0.062(3) 0.0394(19) -0.0281(19) 0.0031(18) -0.001(2) F35 0.084(3) 0.056(3) 0.0308(17) 0.0081(17) -0.0132(18) -0.041(2) F36 0.046(2) 0.063(2) 0.0313(17) -0.0141(16) -0.0088(16) -0.0212(19) S1 0.0505(11) 0.0323(9) 0.0364(8) 0.0018(7) -0.0189(7) -0.0244(8) S2 0.0556(11) 0.0383(9) 0.0377(8) 0.0040(7) -0.0210(8) -0.0297(8) Dy1 0.02590(18) 0.02371(16) 0.02124(14) -0.00774(11) -0.00209(11) -0.01143(13) Dy2 0.02640(18) 0.02472(17) 0.02030(14) -0.00446(11) -0.00476(11) -0.01090(13) C66 0.19(2) 0.19(2) 0.64(6) 0.17(3) 0.11(3) 0.043(18) C67 0.19(2) 0.26(3) 0.27(2) -0.07(2) 0.097(19) -0.02(2) C68 0.134(18) 0.174(19) 0.39(4) 0.14(2) -0.07(2) -0.002(14) C69 0.095(12) 0.26(3) 0.28(2) -0.20(2) 0.013(14) -0.042(14) C70 0.21(3) 0.18(2) 0.77(8) 0.16(3) -0.18(4) -0.10(2) C71 0.19(3) 0.46(6) 0.18(2) -0.08(3) -0.009(18) 0.11(3) C72 0.31(4) 0.20(3) 0.42(4) -0.13(3) 0.19(3) -0.08(2) 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' 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' Dy Dy -0.1892 4.4098 '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 N1 C1 C2 122.0(5) . . C3 C2 C1 118.0(5) . . C2 C3 C4 120.2(5) . . C3 C4 C5 119.3(6) . . N1 C5 C4 121.2(5) . . N1 C5 C6 115.9(4) . . C4 C5 C6 122.9(5) . . N2 C6 C7 120.7(4) . . N2 C6 C5 116.5(4) . . C7 C6 C5 122.8(4) . . C6 C7 C8 120.3(5) . . C7 C8 C9 119.4(5) . . C10 C9 C8 116.9(5) . . C10 C9 C11 121.6(4) . . C8 C9 C11 121.5(5) . . N2 C10 C9 123.8(4) . . C12 C11 C9 128.2(5) . . C12 C11 S1 113.2(4) . . C9 C11 S1 118.6(4) . . C11 C12 C13 115.0(5) . . C16 C13 C12 131.2(5) . . C16 C13 C14A 116.0(7) . . C12 C13 C14A 111.1(6) . . C16 C13 C14B 115.4(7) . . C12 C13 C14B 111.1(6) . . C22A C14A C15A 113(2) . . C22A C14A C13 106.0(16) . . C15A C14A C13 114.6(14) . . C22A C14A S1 113.9(17) . . C15A C14A S1 106.8(9) . . C13 C14A S1 102.7(9) . . C22B C14B C13 104.7(18) . . C22B C14B C15B 114(3) . . C13 C14B C15B 114.1(15) . . C22B C14B S1 112(2) . . C13 C14B S1 103.2(10) . . C15B C14B S1 108.2(10) . . C13 C16 C20 121.0(5) . . C13 C16 C17 128.9(5) . . C20 C16 C17 110.0(4) . . C16 C17 C18 103.3(5) . . C17 C18 C19 106.4(4) . . C20 C19 C18 103.0(4) . . C23 C20 C16 121.6(4) . . C23 C20 C19 129.2(5) . . C16 C20 C19 109.3(5) . . C14A C22A C23 106.1(18) . . C14A C22A C21A 112(2) . . C23 C22A C21A 111.1(13) . . C14A C22A S2 112.4(18) . . C23 C22A S2 103.9(9) . . C21A C22A S2 110.9(11) . . C14B C22B C21B 113(3) . . C14B C22B C23 104.6(19) . . C21B C22B C23 112.5(12) . . C14B C22B S2 113.4(19) . . C21B C22B S2 111.4(13) . . C23 C22B S2 100.6(10) . . C20 C23 C24 132.0(5) . . C20 C23 C22A 115.5(7) . . C24 C23 C22A 110.2(6) . . C20 C23 C22B 115.7(7) . . C24 C23 C22B 110.6(7) . . C25 C24 C23 116.3(5) . . C24 C25 C27 129.4(5) . . C24 C25 S2 113.0(4) . . C27 C25 S2 117.5(4) . . N3 C26 C27 124.6(5) . . C26 C27 C28 115.3(5) . . C26 C27 C25 122.7(5) . . C28 C27 C25 122.0(4) . . C29 C28 C27 120.8(5) . . C28 C29 C30 119.8(5) . . N3 C30 C29 120.4(5) . . N3 C30 C31 116.5(4) . . C29 C30 C31 123.1(5) . . N4 C31 C32 120.7(5) . . N4 C31 C30 116.1(4) . . C32 C31 C30 123.1(4) . . C33 C32 C31 120.2(5) . . C32 C33 C34 119.4(5) . . C35 C34 C33 117.5(5) . . N4 C35 C34 123.9(4) . . F1 C36 F3 104.4(9) . . F1 C36 F2 101.8(8) . . F3 C36 F2 102.5(8) . . F1 C36 C37 114.5(6) . . F3 C36 C37 113.7(6) . . F2 C36 C37 118.1(6) . . O1 C37 C38 127.5(5) . . O1 C37 C36 115.5(5) . . C38 C37 C36 117.0(6) . . C39 C38 C37 120.2(6) . . O2 C39 C38 127.6(5) . . O2 C39 C40 113.9(5) . . C38 C39 C40 118.4(6) . . F6 C40 F5 107.6(5) . . F6 C40 F4 107.6(5) . . F5 C40 F4 107.0(5) . . F6 C40 C39 111.4(5) . . F5 C40 C39 110.4(5) . . F4 C40 C39 112.6(5) . . F8 C41 F9 108.4(6) . . F8 C41 F7 109.6(7) . . F9 C41 F7 102.1(5) . . F8 C41 C42 115.1(5) . . F9 C41 C42 108.4(6) . . F7 C41 C42 112.3(5) . . O3 C42 C43 127.7(5) . . O3 C42 C41 114.1(5) . . C43 C42 C41 118.2(5) . . C44 C43 C42 121.4(5) . . O4 C44 C43 127.8(5) . . O4 C44 C45 113.2(5) . . C43 C44 C45 118.9(5) . . F12 C45 F10 108.9(6) . . F12 C45 F11 106.3(6) . . F10 C45 F11 105.6(5) . . F12 C45 C44 113.2(5) . . F10 C45 C44 113.2(6) . . F11 C45 C44 109.1(5) . . F13 C46 F14 107.9(6) . . F13 C46 F15 106.5(5) . . F14 C46 F15 106.8(5) . . F13 C46 C47 112.4(5) . . F14 C46 C47 110.1(5) . . F15 C46 C47 112.9(5) . . O5 C47 C48 127.3(5) . . O5 C47 C46 112.6(5) . . C48 C47 C46 120.1(5) . . C47 C48 C49 122.1(5) . . O6 C49 C48 126.6(6) . . O6 C49 C50 115.2(5) . . C48 C49 C50 118.0(5) . . F17 C50 F18 107.8(5) . . F17 C50 F16 108.1(5) . . F18 C50 F16 106.3(5) . . F17 C50 C49 110.4(5) . . F18 C50 C49 112.6(5) . . F16 C50 C49 111.4(5) . . F20 C51 F19 110.3(7) . . F20 C51 F21 108.0(9) . . F19 C51 F21 102.8(7) . . F20 C51 C52 112.5(8) . . F19 C51 C52 113.5(7) . . F21 C51 C52 109.1(6) . . O7 C52 C53 127.3(5) . . O7 C52 C51 113.4(6) . . C53 C52 C51 119.4(6) . . C54 C53 C52 120.4(5) . . O8 C54 C53 127.9(5) . . O8 C54 C55 111.9(5) . . C53 C54 C55 120.2(5) . . F23 C55 F24 107.8(5) . . F23 C55 F22 105.7(5) . . F24 C55 F22 102.5(6) . . F23 C55 C54 112.8(6) . . F24 C55 C54 114.3(5) . . F22 C55 C54 112.9(5) . . F25 C56 F27 107.9(5) . . F25 C56 F26 108.4(6) . . F27 C56 F26 105.3(5) . . F25 C56 C57 112.2(5) . . F27 C56 C57 113.6(5) . . F26 C56 C57 109.1(5) . . O9 C57 C58 127.5(5) . . O9 C57 C56 114.5(5) . . C58 C57 C56 118.0(5) . . C59 C58 C57 121.0(5) . . O10 C59 C58 128.6(5) . . O10 C59 C60 113.4(4) . . C58 C59 C60 117.9(5) . . F28 C60 F29 108.5(5) . . F28 C60 F30 107.0(4) . . F29 C60 F30 106.1(5) . . F28 C60 C59 112.0(5) . . F29 C60 C59 113.8(4) . . F30 C60 C59 109.2(5) . . F32 C61 F31 108.7(5) . . F32 C61 F33 108.0(6) . . F31 C61 F33 106.5(5) . . F32 C61 C62 110.2(5) . . F31 C61 C62 110.2(6) . . F33 C61 C62 113.0(5) . . O11 C62 C63 126.5(5) . . O11 C62 C61 113.6(5) . . C63 C62 C61 119.8(5) . . C62 C63 C64 121.7(5) . . O12 C64 C63 127.3(5) . . O12 C64 C65 114.3(5) . . C63 C64 C65 118.4(5) . . F36 C65 F34 107.7(5) . . F36 C65 F35 107.2(4) . . F34 C65 F35 106.5(5) . . F36 C65 C64 111.4(5) . . F34 C65 C64 111.6(5) . . F35 C65 C64 112.1(5) . . C5 N1 C1 119.2(4) . . C5 N1 Dy1 122.0(3) . . C1 N1 Dy1 118.8(4) . . C10 N2 C6 118.7(4) . . C10 N2 Dy1 120.2(3) . . C6 N2 Dy1 121.0(3) . . C26 N3 C30 119.0(4) . . C26 N3 Dy2 121.2(3) . . C30 N3 Dy2 118.8(3) . . C35 N4 C31 118.2(4) . . C35 N4 Dy2 120.6(3) . . C31 N4 Dy2 119.1(3) . . C37 O1 Dy1 131.3(3) . . C39 O2 Dy1 130.1(3) . . C42 O3 Dy1 134.1(3) . . C44 O4 Dy1 133.9(4) . . C47 O5 Dy1 134.4(3) . . C49 O6 Dy1 135.0(4) . . C52 O7 Dy2 135.4(4) . . C54 O8 Dy2 135.0(4) . . C57 O9 Dy2 133.7(3) . . C59 O10 Dy2 131.7(3) . . C62 O11 Dy2 135.3(3) . . C64 O12 Dy2 131.7(3) . . C11 S1 C14B 92.6(5) . . C11 S1 C14A 91.5(5) . . C25 S2 C22A 91.2(4) . . C25 S2 C22B 93.0(5) . . O5 Dy1 O2 146.23(14) . . O5 Dy1 O4 114.02(12) . . O2 Dy1 O4 75.94(12) . . O5 Dy1 O1 81.60(13) . . O2 Dy1 O1 72.34(13) . . O4 Dy1 O1 138.95(12) . . O5 Dy1 O3 73.78(12) . . O2 Dy1 O3 79.24(13) . . O4 Dy1 O3 73.12(12) . . O1 Dy1 O3 75.91(12) . . O5 Dy1 O6 72.62(13) . . O2 Dy1 O6 139.35(13) . . O4 Dy1 O6 74.37(12) . . O1 Dy1 O6 145.24(12) . . O3 Dy1 O6 117.00(13) . . O5 Dy1 N2 136.38(13) . . O2 Dy1 N2 75.04(13) . . O4 Dy1 N2 82.74(12) . . O1 Dy1 N2 112.72(13) . . O3 Dy1 N2 148.25(12) . . O6 Dy1 N2 74.22(13) . . O5 Dy1 N1 82.50(13) . . O2 Dy1 N1 109.19(13) . . O4 Dy1 N1 143.16(14) . . O1 Dy1 N1 73.33(13) . . O3 Dy1 N1 143.40(13) . . O6 Dy1 N1 80.41(13) . . N2 Dy1 N1 64.62(13) . . O8 Dy2 O7 73.03(13) . . O8 Dy2 O11 145.91(12) . . O7 Dy2 O11 80.08(13) . . O8 Dy2 O10 76.27(13) . . O7 Dy2 O10 140.38(12) . . O11 Dy2 O10 115.39(13) . . O8 Dy2 O9 80.39(13) . . O7 Dy2 O9 77.09(13) . . O11 Dy2 O9 73.40(13) . . O10 Dy2 O9 73.60(12) . . O8 Dy2 O12 140.98(12) . . O7 Dy2 O12 139.53(13) . . O11 Dy2 O12 72.66(12) . . O10 Dy2 O12 79.37(12) . . O9 Dy2 O12 120.91(13) . . O8 Dy2 N4 109.65(13) . . O7 Dy2 N4 73.58(12) . . O11 Dy2 N4 81.54(14) . . O10 Dy2 N4 141.66(11) . . O9 Dy2 N4 144.13(13) . . O12 Dy2 N4 73.29(12) . . O8 Dy2 N3 74.32(12) . . O7 Dy2 N3 112.13(14) . . O11 Dy2 N3 136.70(12) . . O10 Dy2 N3 82.28(13) . . O9 Dy2 N3 148.50(14) . . O12 Dy2 N3 72.56(12) . . N4 Dy2 N3 64.31(13) . . C68 C67 C66 134(2) . . C67 C68 C69 129(2) . . C70 C69 C68 116(2) . . C69 C70 C71 123(3) . . C70 C71 C72 125(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 N1 1.349(6) . C1 C2 1.391(7) . C2 C3 1.363(9) . C3 C4 1.375(8) . C4 C5 1.383(7) . C5 N1 1.335(7) . C5 C6 1.497(7) . C6 N2 1.359(6) . C6 C7 1.378(8) . C7 C8 1.382(7) . C8 C9 1.394(7) . C9 C10 1.394(7) . C9 C11 1.469(7) . C10 N2 1.334(6) . C11 C12 1.359(7) . C11 S1 1.759(5) . C12 C13 1.424(7) . C13 C16 1.370(7) . C13 C14A 1.548(16) . C13 C14B 1.566(17) . C14A C22A 1.53(3) . C14A C15A 1.54(4) . C14A S1 1.866(14) . C14B C22B 1.51(4) . C14B C15B 1.58(4) . C14B S1 1.839(14) . C21B C22B 1.53(4) . C16 C20 1.438(7) . C16 C17 1.499(7) . C17 C18 1.532(7) . C18 C19 1.533(8) . C19 C20 1.524(7) . C20 C23 1.342(8) . C21A C22A 1.57(4) . C22A C23 1.541(14) . C22A S2 1.854(15) . C22B C23 1.617(16) . C22B S2 1.861(17) . C23 C24 1.437(8) . C24 C25 1.326(8) . C25 C27 1.459(8) . C25 S2 1.780(5) . C26 N3 1.332(7) . C26 C27 1.395(7) . C27 C28 1.401(7) . C28 C29 1.373(8) . C29 C30 1.387(7) . C30 N3 1.355(6) . C30 C31 1.475(7) . C31 N4 1.359(6) . C31 C32 1.384(7) . C32 C33 1.379(8) . C33 C34 1.388(7) . C34 C35 1.380(7) . C35 N4 1.344(7) . C36 F1 1.171(8) . C36 F3 1.207(7) . C36 F2 1.208(8) . C36 C37 1.511(8) . C37 O1 1.242(7) . C37 C38 1.411(7) . C38 C39 1.371(8) . C39 O2 1.262(7) . C39 C40 1.537(8) . C40 F6 1.315(7) . C40 F5 1.319(7) . C40 F4 1.321(7) . C41 F8 1.268(6) . C41 F9 1.318(8) . C41 F7 1.327(8) . C41 C42 1.544(8) . C42 O3 1.253(6) . C42 C43 1.392(8) . C43 C44 1.377(8) . C44 O4 1.270(6) . C44 C45 1.534(8) . C45 F12 1.279(8) . C45 F10 1.329(6) . C45 F11 1.351(8) . C46 F13 1.314(6) . C46 F14 1.327(7) . C46 F15 1.352(7) . C46 C47 1.525(8) . C47 O5 1.269(6) . C47 C48 1.370(8) . C48 C49 1.389(8) . C49 O6 1.248(6) . C49 C50 1.538(8) . C50 F17 1.318(6) . C50 F18 1.322(7) . C50 F16 1.348(6) . C51 F20 1.248(10) . C51 F19 1.313(8) . C51 F21 1.365(10) . C51 C52 1.530(9) . C52 O7 1.250(6) . C52 C53 1.392(9) . C53 C54 1.386(8) . C54 O8 1.252(6) . C54 C55 1.496(9) . C55 F23 1.309(7) . C55 F24 1.324(7) . C55 F22 1.388(7) . C56 F25 1.293(7) . C56 F27 1.328(7) . C56 F26 1.348(8) . C56 C57 1.532(7) . C57 O9 1.243(7) . C57 C58 1.399(8) . C58 C59 1.394(7) . C59 O10 1.258(6) . C59 C60 1.527(8) . C60 F28 1.312(7) . C60 F29 1.327(6) . C60 F30 1.355(7) . C61 F32 1.325(7) . C61 F31 1.332(7) . C61 F33 1.342(7) . C61 C62 1.538(8) . C62 O11 1.254(7) . C62 C63 1.383(7) . C63 C64 1.389(8) . C64 O12 1.261(6) . C64 C65 1.533(7) . C65 F36 1.321(7) . C65 F34 1.329(7) . C65 F35 1.339(7) . N1 Dy1 2.516(4) . N2 Dy1 2.509(4) . N3 Dy2 2.528(4) . N4 Dy2 2.506(4) . O1 Dy1 2.345(4) . O2 Dy1 2.325(4) . O3 Dy1 2.349(4) . O4 Dy1 2.331(3) . O5 Dy1 2.319(4) . O6 Dy1 2.351(4) . O7 Dy2 2.317(3) . O8 Dy2 2.307(4) . O9 Dy2 2.349(3) . O10 Dy2 2.334(3) . O11 Dy2 2.327(4) . O12 Dy2 2.351(3) . C66 C67 1.51(3) . C67 C68 1.37(3) . C68 C69 1.41(2) . C69 C70 1.26(3) . C70 C71 1.35(4) . C71 C72 1.53(4) .