#------------------------------------------------------------------------------ #$Date: 2019-11-08 00:58:48 +0200 (Fri, 08 Nov 2019) $ #$Revision: 224380 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/92/7049253.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_7049253 loop_ _publ_author_name 'Yang, Zhao-Fu' 'Tian, Yong-Mei' 'Zhang, Wan-Ying' 'Chen, Peng' 'Li, Hong-Feng' 'Zhang, Yi-Quan' 'Sun, Wen-Bin' _publ_section_title ; High local coordination symmetry around the spin center and the alignment between magnetic and symmetric axes together play a crucial role in single-molecule magnet performance. ; _journal_issue 15 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 4931 _journal_page_last 4940 _journal_paper_doi 10.1039/c9dt00058e _journal_volume 48 _journal_year 2019 _chemical_formula_sum 'C58 H54 Dy2 F6 N6 O12 S2' _chemical_formula_weight 1530.19 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-01-30 deposited with the CCDC. 2019-03-06 downloaded from the CCDC. ; _cell_angle_alpha 99.306(7) _cell_angle_beta 96.452(7) _cell_angle_gamma 105.332(7) _cell_formula_units_Z 1 _cell_length_a 11.1327(9) _cell_length_b 11.7050(11) _cell_length_c 12.3830(10) _cell_measurement_reflns_used 5627 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 1.00000 _cell_measurement_theta_min 0.73398 _cell_volume 1515.2(2) _computing_cell_refinement 'CrysAlis PRO (Agilent, 2011)' _computing_data_collection 'CrysAlis PRO (Agilent, 2011)' _computing_data_reduction 'CrysAlis PRO (Agilent, 2011)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'CrysAlis PRO (Agilent, 2011)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_unetI/netI 0.0963 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 17350 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.484 _diffrn_reflns_theta_min 3.022 _diffrn_source '\w scans' _exptl_absorpt_coefficient_mu 2.599 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.677 _exptl_crystal_description block _exptl_crystal_F_000 758 _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 2.508 _refine_diff_density_min -1.510 _refine_diff_density_rms 0.159 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 394 _refine_ls_number_reflns 6919 _refine_ls_number_restraints 10 _refine_ls_restrained_S_all 1.016 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0536 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0590P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1208 _refine_ls_wR_factor_ref 0.1369 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5158 _reflns_number_total 6919 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00058e2.cif _cod_data_source_block 5 _cod_depositor_comments 'Adding full bibliography for 7049253--7049258.cif.' _cod_database_code 7049253 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.763 _shelx_estimated_absorpt_t_max 0.781 _shelx_res_file ; yzf-247-666.res created by SHELXL-2014/7 TITL yzf-247-666_a.res in P-1 REM Old TITL yzf-247-666 in P1 REM SHELXT solution in P-1 REM R1 0.128, Rweak 0.004, Alpha 0.045, Orientation as input REM Formula found by SHELXT: C27 N6 O4 Dy S F4 CELL 0.71073 11.1327 11.705 12.383 99.306 96.452 105.332 ZERR 1 0.0009 0.0011 0.001 0.007 0.007 0.007 LATT 1 SFAC C H Dy F N O S UNIT 58 54 2 6 6 12 2 DFIX 0.85 0.01 O1 H1 DANG 1.923173 0.02 C26 H1 DANG 2.940276 0.02 Dy01 H1 L.S. 5 PLAN 5 SIZE 0.1 0.11 0.1 TEMP 19.85 list 4 fmap 2 ACTA delu 0.01 0.005 c23 c24 isor 0.005 c24 WGHT 0.059000 FVAR 0.35096 DY01 3 0.508539 0.625408 0.414066 11.00000 0.03934 0.03346 = 0.03573 0.01163 0.00447 0.00493 S1 7 0.296303 0.296520 0.078047 11.00000 0.07587 0.09721 = 0.07573 -0.01194 0.01527 0.00188 O5 6 0.622964 0.553615 0.551215 11.00000 0.03293 0.03640 = 0.03996 0.01402 -0.00169 0.00404 O4 6 0.691521 0.649314 0.339604 11.00000 0.04627 0.05964 = 0.04995 0.00502 0.01332 0.00435 O3 6 0.468364 0.482067 0.249471 11.00000 0.04794 0.05599 = 0.04392 0.00345 0.01275 0.00153 O1 6 0.402088 0.698950 0.555654 11.00000 0.04768 0.04477 = 0.06313 0.00466 0.01793 0.00692 H1 2 0.431580 0.770817 0.593970 11.00000 -1.50000 O2 6 0.357219 0.665147 0.289191 11.00000 0.05947 0.04230 = 0.05199 0.01794 -0.00400 0.00867 N008 5 0.684472 0.786904 0.539903 11.00000 0.04190 0.03500 = 0.03387 0.01231 0.00503 0.00571 N009 5 0.533010 0.843810 0.395518 11.00000 0.04354 0.03401 = 0.04099 0.00988 0.00001 0.00476 N00A 5 0.445689 0.870867 0.323523 11.00000 0.05177 0.04580 = 0.04365 0.02289 0.00335 0.01125 O6 6 0.474189 0.897356 0.714357 11.00000 0.12349 0.03695 = 0.05901 0.01297 0.00925 0.01079 AFIX 147 H6 2 0.510605 0.965199 0.705858 11.00000 -1.50000 AFIX 0 C16 1 0.733519 0.624489 0.609697 11.00000 0.03897 0.04254 = 0.03423 0.01291 0.01078 0.00817 C19 1 0.727981 0.592834 0.258690 11.00000 0.04086 0.05342 = 0.05367 0.02830 0.01511 0.01243 C7 1 0.358974 0.770181 0.273495 11.00000 0.04700 0.04013 = 0.04558 0.01852 0.00937 0.01040 C6 1 0.259670 0.777806 0.184887 11.00000 0.04208 0.05250 = 0.04450 0.02140 0.01040 0.01397 C23 1 0.490223 0.315532 -0.027005 11.00000 0.05750 0.03466 = 0.03249 0.00503 0.00417 0.01425 AFIX 43 H23A 2 0.570607 0.338452 -0.045571 11.00000 -1.20000 AFIX 0 C15 1 0.816428 0.584251 0.672152 11.00000 0.04007 0.04436 = 0.05098 0.01818 0.00893 0.01046 AFIX 43 H15 2 0.795749 0.503517 0.678448 11.00000 -1.20000 AFIX 0 C17 1 0.768691 0.749425 0.603050 11.00000 0.03819 0.03976 = 0.03353 0.00786 0.00415 0.00360 C20 1 0.657046 0.500080 0.175675 11.00000 0.05239 0.05282 = 0.04761 0.01202 0.01868 0.01487 AFIX 43 H20 2 0.695781 0.467911 0.120411 11.00000 -1.20000 AFIX 0 F3 4 0.913295 0.750228 0.269004 11.00000 0.07283 0.08185 = 0.22018 0.01256 0.04830 -0.01557 C21 1 0.526732 0.452388 0.172211 11.00000 0.06198 0.04182 = 0.04040 0.01259 0.01190 0.01623 C8 1 0.625662 0.931072 0.451262 11.00000 0.06358 0.03412 = 0.05369 0.01552 0.00043 0.01279 AFIX 43 H8 2 0.634294 1.010469 0.443654 11.00000 -1.20000 AFIX 0 C14 1 0.932400 0.663775 0.726785 11.00000 0.04372 0.05798 = 0.06100 0.02475 0.00125 0.01475 AFIX 43 H14 2 0.986934 0.633852 0.769003 11.00000 -1.20000 AFIX 0 C9 1 0.715751 0.901429 0.526032 11.00000 0.04782 0.03576 = 0.04661 0.00790 0.00289 0.00439 C13 1 0.969205 0.782670 0.721130 11.00000 0.03845 0.05314 = 0.05852 0.00996 -0.00585 0.00527 AFIX 43 H13 2 1.046914 0.833203 0.758736 11.00000 -1.20000 AFIX 0 C12 1 0.886846 0.826911 0.657108 11.00000 0.04212 0.04402 = 0.04606 0.00775 0.00337 0.00542 C22 1 0.451470 0.360802 0.075923 11.00000 0.05813 0.04523 = 0.04630 0.01626 0.00931 0.01520 C5 1 0.236343 0.887231 0.176011 11.00000 0.05881 0.05742 = 0.04894 0.01492 0.00095 0.01439 AFIX 43 H5 2 0.283056 0.957388 0.225954 11.00000 -1.20000 AFIX 0 C1 1 0.190753 0.675033 0.109273 11.00000 0.05381 0.05978 = 0.05459 0.01992 0.00529 0.00499 AFIX 43 H1A 2 0.205289 0.601082 0.113473 11.00000 -1.20000 AFIX 0 C10 1 0.832206 0.984723 0.577422 11.00000 0.06264 0.03709 = 0.06334 0.01781 -0.00640 -0.00503 AFIX 43 H10 2 0.851677 1.064121 0.567130 11.00000 -1.20000 AFIX 0 C11 1 0.915883 0.948362 0.642101 11.00000 0.05409 0.04647 = 0.05945 0.01368 -0.00759 -0.00498 AFIX 43 H11 2 0.992608 1.003271 0.676753 11.00000 -1.20000 AFIX 0 C26 1 0.274253 0.647838 0.577051 11.00000 0.06409 0.05669 = 0.06650 0.00357 0.02486 0.01582 AFIX 23 H26A 2 0.274548 0.658161 0.656407 11.00000 -1.20000 H26B 2 0.245523 0.561937 0.545463 11.00000 -1.20000 AFIX 0 F1 4 0.909690 0.584237 0.178474 11.00000 0.08142 0.16913 = 0.19216 -0.04051 0.07924 -0.00034 C2 1 0.099776 0.682568 0.027051 11.00000 0.06196 0.08763 = 0.05239 0.02144 0.00223 0.00796 AFIX 43 H2 2 0.053149 0.613220 -0.023950 11.00000 -1.20000 AFIX 0 C4 1 0.145206 0.892747 0.094407 11.00000 0.07109 0.08097 = 0.06389 0.03245 0.00694 0.04136 AFIX 43 H4 2 0.129765 0.966325 0.090172 11.00000 -1.20000 AFIX 0 C3 1 0.077440 0.791760 0.019856 11.00000 0.06382 0.10639 = 0.04359 0.03143 0.00065 0.02729 AFIX 43 H3 2 0.016276 0.796059 -0.035790 11.00000 -1.20000 AFIX 0 C24 1 0.384299 0.231679 -0.092067 11.00000 0.08920 0.07361 = 0.06775 0.00967 0.01708 0.01838 AFIX 43 H24 2 0.387451 0.191334 -0.162376 11.00000 -1.20000 AFIX 0 F2 4 0.929812 0.610039 0.347128 11.00000 0.05931 0.29441 = 0.17223 0.11219 -0.00472 0.03370 C18 1 0.870992 0.635360 0.264880 11.00000 0.05244 0.08926 = 0.07749 0.01082 0.01725 0.00355 C25 1 0.278256 0.211569 -0.049546 11.00000 0.08467 0.06516 = 0.07291 -0.01379 -0.00654 0.00435 AFIX 43 H25 2 0.202339 0.156664 -0.086097 11.00000 -1.20000 AFIX 0 C28 1 0.469141 0.899656 0.828253 11.00000 0.08542 0.11329 = 0.09957 0.05599 0.00486 0.00234 AFIX 23 H28A 2 0.509270 0.841229 0.850845 11.00000 -1.20000 H28B 2 0.519351 0.978858 0.869428 11.00000 -1.20000 AFIX 0 C27 1 0.187638 0.708258 0.527884 11.00000 0.08002 0.10219 = 0.09779 0.02621 0.01388 0.03534 AFIX 137 H27A 2 0.194946 0.706242 0.451132 11.00000 -1.50000 H27B 2 0.209023 0.790730 0.566608 11.00000 -1.50000 H27C 2 0.102480 0.667189 0.533858 11.00000 -1.50000 AFIX 0 C29 1 0.349559 0.875587 0.860319 11.00000 0.11343 0.14404 = 0.15165 0.00356 0.06205 0.03048 AFIX 137 H29A 2 0.303601 0.925171 0.830226 11.00000 -1.50000 H29B 2 0.358898 0.893208 0.939781 11.00000 -1.50000 H29C 2 0.304303 0.791902 0.832903 11.00000 -1.50000 AFIX 0 HKLF 4 REM yzf-247-666_a.res in P-1 REM R1 = 0.0536 for 5158 Fo > 4sig(Fo) and 0.0804 for all 6919 data REM 394 parameters refined using 10 restraints END WGHT 0.0590 0.0000 REM Highest difference peak 2.508, deepest hole -1.510, 1-sigma level 0.159 Q1 1 0.5271 0.8756 0.2440 11.00000 0.05 2.51 Q2 1 0.5991 0.6332 0.4117 11.00000 0.05 1.71 Q3 1 0.4371 0.6432 0.4548 11.00000 0.05 1.60 Q4 1 0.4249 0.6020 0.3801 11.00000 0.05 1.55 Q5 1 0.4399 0.5848 0.3593 11.00000 0.05 1.43 ; _shelx_res_checksum 35263 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 Dy01 Dy 0.50854(3) 0.62541(2) 0.41407(2) 0.03685(12) Uani 1 1 d D . S1 S 0.2963(2) 0.2965(3) 0.0780(2) 0.0906(8) Uani 1 1 d . . O5 O 0.6230(4) 0.5536(4) 0.5512(3) 0.0375(10) Uani 1 1 d . . O4 O 0.6915(4) 0.6493(4) 0.3396(4) 0.0543(12) Uani 1 1 d . . O3 O 0.4684(4) 0.4821(4) 0.2495(4) 0.0523(12) Uani 1 1 d . . O1 O 0.4021(4) 0.6989(4) 0.5557(4) 0.0531(12) Uani 1 1 d D . H1 H 0.432(4) 0.771(3) 0.594(5) 0.080 Uiso 1 1 d D U O2 O 0.3572(5) 0.6651(4) 0.2892(4) 0.0525(12) Uani 1 1 d . . N008 N 0.6845(5) 0.7869(4) 0.5399(4) 0.0374(12) Uani 1 1 d . . N009 N 0.5330(5) 0.8438(5) 0.3955(4) 0.0410(12) Uani 1 1 d . . N00A N 0.4457(5) 0.8709(5) 0.3235(5) 0.0463(14) Uani 1 1 d . . O6 O 0.4742(7) 0.8974(5) 0.7144(5) 0.0756(17) Uani 1 1 d . . H6 H 0.5106 0.9652 0.7059 0.113 Uiso 1 1 calc R U C16 C 0.7335(6) 0.6245(6) 0.6097(5) 0.0383(14) Uani 1 1 d . . C19 C 0.7280(6) 0.5928(6) 0.2587(6) 0.0469(17) Uani 1 1 d . . C7 C 0.3590(6) 0.7702(6) 0.2735(6) 0.0433(15) Uani 1 1 d . . C6 C 0.2597(6) 0.7778(6) 0.1849(6) 0.0447(15) Uani 1 1 d . . C23 C 0.4902(7) 0.3155(6) -0.0270(5) 0.0418(15) Uani 1 1 d . U H23A H 0.5706 0.3385 -0.0456 0.050 Uiso 1 1 calc R U C15 C 0.8164(6) 0.5843(6) 0.6722(6) 0.0443(15) Uani 1 1 d . . H15 H 0.7957 0.5035 0.6784 0.053 Uiso 1 1 calc R U C17 C 0.7687(6) 0.7494(6) 0.6030(5) 0.0387(14) Uani 1 1 d . . C20 C 0.6570(7) 0.5001(6) 0.1757(6) 0.0499(17) Uani 1 1 d . . H20 H 0.6958 0.4679 0.1204 0.060 Uiso 1 1 calc R U F3 F 0.9133(5) 0.7502(5) 0.2690(7) 0.132(3) Uani 1 1 d . . C21 C 0.5267(7) 0.4524(6) 0.1722(6) 0.0470(16) Uani 1 1 d . . C8 C 0.6257(7) 0.9311(6) 0.4513(6) 0.0507(17) Uani 1 1 d . . H8 H 0.6343 1.0105 0.4437 0.061 Uiso 1 1 calc R U C14 C 0.9324(7) 0.6638(7) 0.7268(6) 0.0533(18) Uani 1 1 d . . H14 H 0.9869 0.6339 0.7690 0.064 Uiso 1 1 calc R U C9 C 0.7158(6) 0.9014(6) 0.5260(6) 0.0453(16) Uani 1 1 d . . C13 C 0.9692(6) 0.7827(6) 0.7211(6) 0.0528(18) Uani 1 1 d . . H13 H 1.0469 0.8332 0.7587 0.063 Uiso 1 1 calc R U C12 C 0.8868(6) 0.8269(6) 0.6571(6) 0.0459(16) Uani 1 1 d . . C22 C 0.4515(7) 0.3608(6) 0.0759(6) 0.0489(17) Uani 1 1 d . . C5 C 0.2363(7) 0.8872(7) 0.1760(6) 0.0556(18) Uani 1 1 d . . H5 H 0.2831 0.9574 0.2260 0.067 Uiso 1 1 calc R U C1 C 0.1908(7) 0.6750(7) 0.1093(6) 0.0576(19) Uani 1 1 d . . H1A H 0.2053 0.6011 0.1135 0.069 Uiso 1 1 calc R U C10 C 0.8322(7) 0.9847(6) 0.5774(6) 0.059(2) Uani 1 1 d . . H10 H 0.8517 1.0641 0.5671 0.070 Uiso 1 1 calc R U C11 C 0.9159(7) 0.9484(6) 0.6421(7) 0.058(2) Uani 1 1 d . . H11 H 0.9926 1.0033 0.6768 0.070 Uiso 1 1 calc R U C26 C 0.2743(7) 0.6478(7) 0.5771(7) 0.063(2) Uani 1 1 d D . H26A H 0.2745 0.6582 0.6564 0.075 Uiso 1 1 calc R U H26B H 0.2455 0.5619 0.5455 0.075 Uiso 1 1 calc R U F1 F 0.9097(6) 0.5842(7) 0.1785(8) 0.159(4) Uani 1 1 d . . C2 C 0.0998(8) 0.6826(9) 0.0271(7) 0.070(2) Uani 1 1 d . . H2 H 0.0531 0.6132 -0.0240 0.084 Uiso 1 1 calc R U C4 C 0.1452(8) 0.8927(8) 0.0944(7) 0.066(2) Uani 1 1 d . . H4 H 0.1298 0.9663 0.0902 0.080 Uiso 1 1 calc R U C3 C 0.0774(8) 0.7918(9) 0.0199(7) 0.069(2) Uani 1 1 d . . H3 H 0.0163 0.7961 -0.0358 0.083 Uiso 1 1 calc R U C24 C 0.3843(9) 0.2317(8) -0.0921(8) 0.078(2) Uani 1 1 d . U H24 H 0.3875 0.1913 -0.1624 0.094 Uiso 1 1 calc R U F2 F 0.9298(6) 0.6100(10) 0.3471(8) 0.173(4) Uani 1 1 d . . C18 C 0.8710(8) 0.6354(10) 0.2649(9) 0.077(3) Uani 1 1 d . . C25 C 0.2783(10) 0.2116(8) -0.0495(8) 0.082(3) Uani 1 1 d . . H25 H 0.2023 0.1567 -0.0861 0.099 Uiso 1 1 calc R U C28 C 0.4691(10) 0.8997(11) 0.8283(10) 0.101(4) Uani 1 1 d . . H28A H 0.5093 0.8412 0.8508 0.122 Uiso 1 1 calc R U H28B H 0.5194 0.9789 0.8694 0.122 Uiso 1 1 calc R U C27 C 0.1876(9) 0.7083(9) 0.5279(9) 0.091(3) Uani 1 1 d . . H27A H 0.1949 0.7062 0.4511 0.136 Uiso 1 1 calc R U H27B H 0.2090 0.7907 0.5666 0.136 Uiso 1 1 calc R U H27C H 0.1025 0.6672 0.5339 0.136 Uiso 1 1 calc R U C29 C 0.3496(12) 0.8756(12) 0.8603(12) 0.137(5) Uani 1 1 d . . H29A H 0.3036 0.9252 0.8302 0.206 Uiso 1 1 calc R U H29B H 0.3589 0.8932 0.9398 0.206 Uiso 1 1 calc R U H29C H 0.3043 0.7919 0.8329 0.206 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 Dy01 0.03934(19) 0.03346(17) 0.03573(18) 0.01163(13) 0.00447(12) 0.00493(12) S1 0.0759(16) 0.0972(19) 0.0757(17) -0.0119(15) 0.0153(13) 0.0019(14) O5 0.033(2) 0.036(2) 0.040(2) 0.0140(19) -0.0017(18) 0.0040(18) O4 0.046(3) 0.060(3) 0.050(3) 0.005(3) 0.013(2) 0.004(2) O3 0.048(3) 0.056(3) 0.044(3) 0.003(2) 0.013(2) 0.002(2) O1 0.048(3) 0.045(3) 0.063(3) 0.005(2) 0.018(2) 0.007(2) O2 0.059(3) 0.042(3) 0.052(3) 0.018(2) -0.004(2) 0.009(2) N008 0.042(3) 0.035(3) 0.034(3) 0.012(2) 0.005(2) 0.006(2) N009 0.044(3) 0.034(3) 0.041(3) 0.010(2) 0.000(2) 0.005(2) N00A 0.052(3) 0.046(3) 0.044(3) 0.023(3) 0.003(3) 0.011(3) O6 0.123(5) 0.037(3) 0.059(4) 0.013(3) 0.009(3) 0.011(3) C16 0.039(3) 0.043(3) 0.034(3) 0.013(3) 0.011(3) 0.008(3) C19 0.041(4) 0.053(4) 0.054(4) 0.028(4) 0.015(3) 0.012(3) C7 0.047(4) 0.040(4) 0.046(4) 0.019(3) 0.009(3) 0.010(3) C6 0.042(4) 0.053(4) 0.045(4) 0.021(3) 0.010(3) 0.014(3) C23 0.058(4) 0.035(3) 0.032(3) 0.005(3) 0.004(3) 0.014(3) C15 0.040(4) 0.044(4) 0.051(4) 0.018(3) 0.009(3) 0.010(3) C17 0.038(3) 0.040(3) 0.034(3) 0.008(3) 0.004(3) 0.004(3) C20 0.052(4) 0.053(4) 0.048(4) 0.012(4) 0.019(3) 0.015(4) F3 0.073(4) 0.082(4) 0.220(9) 0.013(5) 0.048(5) -0.016(3) C21 0.062(5) 0.042(4) 0.040(4) 0.013(3) 0.012(3) 0.016(3) C8 0.064(5) 0.034(3) 0.054(4) 0.016(3) 0.000(4) 0.013(3) C14 0.044(4) 0.058(4) 0.061(5) 0.025(4) 0.001(3) 0.015(3) C9 0.048(4) 0.036(3) 0.047(4) 0.008(3) 0.003(3) 0.004(3) C13 0.038(4) 0.053(4) 0.059(5) 0.010(4) -0.006(3) 0.005(3) C12 0.042(4) 0.044(4) 0.046(4) 0.008(3) 0.003(3) 0.005(3) C22 0.058(4) 0.045(4) 0.046(4) 0.016(3) 0.009(3) 0.015(3) C5 0.059(5) 0.057(5) 0.049(4) 0.015(4) 0.001(4) 0.014(4) C1 0.054(4) 0.060(5) 0.055(5) 0.020(4) 0.005(4) 0.005(4) C10 0.063(5) 0.037(4) 0.063(5) 0.018(4) -0.006(4) -0.005(3) C11 0.054(4) 0.046(4) 0.059(5) 0.014(4) -0.008(4) -0.005(3) C26 0.064(5) 0.057(5) 0.066(5) 0.004(4) 0.025(4) 0.016(4) F1 0.081(5) 0.169(7) 0.192(8) -0.041(6) 0.079(5) 0.000(4) C2 0.062(5) 0.088(6) 0.052(5) 0.021(5) 0.002(4) 0.008(5) C4 0.071(6) 0.081(6) 0.064(5) 0.032(5) 0.007(4) 0.041(5) C3 0.064(5) 0.106(7) 0.044(4) 0.031(5) 0.001(4) 0.027(5) C24 0.089(4) 0.074(4) 0.068(4) 0.010(3) 0.017(4) 0.018(3) F2 0.059(4) 0.294(12) 0.172(8) 0.112(8) -0.005(4) 0.034(5) C18 0.052(5) 0.089(7) 0.077(7) 0.011(6) 0.017(5) 0.004(5) C25 0.085(7) 0.065(6) 0.073(6) -0.014(5) -0.007(5) 0.004(5) C28 0.085(7) 0.113(9) 0.100(9) 0.056(7) 0.005(6) 0.002(6) C27 0.080(7) 0.102(8) 0.098(8) 0.026(7) 0.014(6) 0.035(6) C29 0.113(10) 0.144(12) 0.152(13) 0.004(10) 0.062(10) 0.030(9) 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' Dy Dy -0.1892 4.4098 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O4 Dy01 O3 71.57(16) . . O4 Dy01 O2 108.18(18) . . O3 Dy01 O2 71.91(17) . . O4 Dy01 O5 127.77(16) . 2_666 O3 Dy01 O5 74.06(16) . 2_666 O2 Dy01 O5 96.83(15) . 2_666 O4 Dy01 O1 147.46(17) . . O3 Dy01 O1 140.76(17) . . O2 Dy01 O1 85.67(18) . . O5 Dy01 O1 77.27(15) 2_666 . O4 Dy01 O5 82.78(16) . . O3 Dy01 O5 106.53(16) . . O2 Dy01 O5 167.18(15) . . O5 Dy01 O5 70.76(15) 2_666 . O1 Dy01 O5 88.32(16) . . O4 Dy01 N008 69.86(16) . . O3 Dy01 N008 141.33(17) . . O2 Dy01 N008 123.52(16) . . O5 Dy01 N008 130.09(15) 2_666 . O1 Dy01 N008 77.91(16) . . O5 Dy01 N008 65.90(15) . . O4 Dy01 N009 84.54(18) . . O3 Dy01 N009 116.83(17) . . O2 Dy01 N009 61.54(16) . . O5 Dy01 N009 146.88(16) 2_666 . O1 Dy01 N009 76.39(17) . . O5 Dy01 N009 127.76(15) . . N008 Dy01 N009 62.13(16) . . O4 Dy01 Dy01 107.09(13) . 2_666 O3 Dy01 Dy01 90.54(12) . 2_666 O2 Dy01 Dy01 132.54(12) . 2_666 O5 Dy01 Dy01 35.79(10) 2_666 2_666 O1 Dy01 Dy01 81.26(12) . 2_666 O5 Dy01 Dy01 34.98(9) . 2_666 N008 Dy01 Dy01 97.94(11) . 2_666 N009 Dy01 Dy01 152.59(12) . 2_666 C25 S1 C22 91.3(4) . . C16 O5 Dy01 128.9(4) . 2_666 C16 O5 Dy01 120.4(4) . . Dy01 O5 Dy01 109.24(15) 2_666 . C19 O4 Dy01 136.1(4) . . C21 O3 Dy01 138.4(5) . . C26 O1 Dy01 129.3(4) . . C7 O2 Dy01 124.1(4) . . C9 N008 C17 119.0(6) . . C9 N008 Dy01 122.0(4) . . C17 N008 Dy01 116.6(4) . . C8 N009 N00A 118.0(5) . . C8 N009 Dy01 121.8(4) . . N00A N009 Dy01 120.2(4) . . C7 N00A N009 109.1(5) . . O5 C16 C15 124.2(6) . . O5 C16 C17 117.8(6) . . C15 C16 C17 118.0(6) . . O4 C19 C20 128.3(6) . . O4 C19 C18 112.0(7) . . C20 C19 C18 119.6(7) . . O2 C7 N00A 125.1(6) . . O2 C7 C6 116.8(6) . . N00A C7 C6 117.9(6) . . C1 C6 C5 118.9(7) . . C1 C6 C7 119.7(6) . . C5 C6 C7 121.4(6) . . C24 C23 C22 106.8(7) . . C16 C15 C14 120.3(6) . . N008 C17 C12 122.7(6) . . N008 C17 C16 116.7(5) . . C12 C17 C16 120.5(6) . . C19 C20 C21 121.2(6) . . O3 C21 C20 123.7(7) . . O3 C21 C22 116.8(6) . . C20 C21 C22 119.5(6) . . N009 C8 C9 117.3(6) . . C13 C14 C15 123.1(7) . . N008 C9 C10 121.7(6) . . N008 C9 C8 115.5(6) . . C10 C9 C8 122.8(6) . . C14 C13 C12 118.1(7) . . C13 C12 C17 119.9(6) . . C13 C12 C11 123.4(7) . . C17 C12 C11 116.6(6) . . C23 C22 C21 129.0(7) . . C23 C22 S1 112.3(5) . . C21 C22 S1 118.7(5) . . C4 C5 C6 120.7(8) . . C6 C1 C2 119.6(8) . . C11 C10 C9 119.5(6) . . C10 C11 C12 120.3(7) . . O1 C26 C27 110.2(7) . . C3 C2 C1 120.8(8) . . C3 C4 C5 120.5(8) . . C4 C3 C2 119.6(8) . . C25 C24 C23 117.0(9) . . F2 C18 F3 108.2(10) . . F2 C18 F1 104.5(10) . . F3 C18 F1 105.2(9) . . F2 C18 C19 112.7(8) . . F3 C18 C19 112.7(8) . . F1 C18 C19 113.0(8) . . C24 C25 S1 112.5(8) . . C29 C28 O6 117.3(11) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy01 O4 2.298(5) . Dy01 O3 2.337(5) . Dy01 O2 2.347(5) . Dy01 O5 2.352(4) 2_666 Dy01 O1 2.395(5) . Dy01 O5 2.399(4) . Dy01 N008 2.498(5) . Dy01 N009 2.549(5) . Dy01 Dy01 3.8732(6) 2_666 S1 C25 1.685(9) . S1 C22 1.697(8) . O5 C16 1.339(7) . O5 Dy01 2.352(4) 2_666 O4 C19 1.275(8) . O3 C21 1.269(8) . O1 C26 1.463(8) . O2 C7 1.271(7) . N008 C9 1.337(8) . N008 C17 1.359(8) . N009 C8 1.280(8) . N009 N00A 1.378(7) . N00A C7 1.316(8) . O6 C28 1.414(12) . C16 C15 1.364(9) . C16 C17 1.429(8) . C19 C20 1.365(10) . C19 C18 1.526(11) . C7 C6 1.498(9) . C6 C1 1.378(10) . C6 C5 1.391(9) . C23 C24 1.386(11) . C23 C22 1.455(9) . C15 C14 1.398(9) . C17 C12 1.406(9) . C20 C21 1.403(10) . F3 C18 1.292(11) . C21 C22 1.470(10) . C8 C9 1.436(9) . C14 C13 1.359(10) . C9 C10 1.408(9) . C13 C12 1.399(9) . C12 C11 1.420(9) . C5 C4 1.371(10) . C1 C2 1.384(11) . C10 C11 1.357(10) . C26 C27 1.473(12) . F1 C18 1.312(11) . C2 C3 1.380(11) . C4 C3 1.356(12) . C24 C25 1.326(13) . F2 C18 1.267(12) . C28 C29 1.402(14) .