#------------------------------------------------------------------------------ #$Date: 2019-11-08 00:58:48 +0200 (Fri, 08 Nov 2019) $ #$Revision: 224380 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/92/7049258.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_7049258 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 'C42 H34 Dy2 F12 N6 O18 S4' _chemical_formula_weight 1591.99 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _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 90 _cell_angle_beta 96.515(12) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.5623(12) _cell_length_b 11.9207(13) _cell_length_c 19.877(3) _cell_measurement_reflns_used 2834 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.9481 _cell_measurement_theta_min 3.3328 _cell_volume 2722.0(6) _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 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.933 _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_unetI/netI 0.0817 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.933 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 20931 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.933 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 28.010 _diffrn_reflns_theta_min 3.340 _exptl_absorpt_coefficient_mu 2.994 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.39071 _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 1.942 _exptl_crystal_description block _exptl_crystal_F_000 1552 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _refine_diff_density_max 1.949 _refine_diff_density_min -1.473 _refine_diff_density_rms 0.154 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 380 _refine_ls_number_reflns 6131 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0584 _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^)+(0.0511P)^2^+3.5275P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1195 _refine_ls_wR_factor_ref 0.1419 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4129 _reflns_number_total 6131 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00058e2.cif _cod_data_source_block 4 _cod_depositor_comments 'Adding full bibliography for 7049253--7049258.cif.' _cod_database_code 7049258 _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 ; exp_13444.res created by SHELXL-2014/7 TITL exp_13444_a.res in P2(1)/n REM Old TITL exp_13444 in P21/n #14 REM SHELXT solution in P2(1)/n REM R1 0.189, Rweak 0.059, Alpha 0.066, Orientation as input REM Formula found by SHELXT: C29 N9 Dy O1 CELL 0.71073 11.5623 11.9207 19.8775 90 96.515 90 ZERR 2 0.0012 0.0013 0.0027 0 0.012 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Dy F N O S UNIT 84 68 4 24 12 36 8 L.S. 10 PLAN 20 TEMP 19.85 BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 REM REM REM WGHT 0.051100 3.527500 FVAR 0.23705 DY1 3 0.587884 0.452641 0.580926 11.00000 0.03336 0.03718 = 0.04471 0.00420 -0.00533 -0.00204 S1 7 0.592651 0.507604 0.761162 11.00000 0.06495 0.05256 = 0.05350 -0.00568 0.00125 -0.01045 S2 7 0.726136 0.267450 0.466547 11.00000 0.05025 0.06137 = 0.05540 -0.00081 0.00329 -0.00055 O2 6 0.401769 0.463968 0.526718 11.00000 0.03221 0.03927 = 0.04097 0.01108 -0.00443 -0.00225 O1 6 0.781619 0.482018 0.625008 11.00000 0.03456 0.03980 = 0.05517 0.00270 -0.00687 -0.00253 N1 5 0.471471 0.291293 0.604997 11.00000 0.03231 0.03860 = 0.04115 -0.00032 -0.00474 -0.00221 N3 5 0.804685 0.312420 0.670626 11.00000 0.03311 0.04105 = 0.05222 0.00748 -0.00723 0.00189 AFIX 43 H3 2 0.847327 0.260255 0.690349 11.00000 -1.20000 AFIX 0 N2 5 0.687803 0.299107 0.652782 11.00000 0.03714 0.03435 = 0.04620 0.00135 -0.00433 -0.00014 O4 6 0.536870 0.475422 0.695071 11.00000 0.05686 0.04326 = 0.05419 -0.00940 0.00323 -0.00120 O3 6 0.567535 0.649328 0.598258 11.00000 0.04744 0.03278 = 0.08050 0.00638 -0.01493 -0.00912 O8 6 0.666784 0.259818 0.399701 11.00000 0.07145 0.09539 = 0.05859 -0.00414 -0.00155 -0.00401 F2 4 0.799138 0.120514 0.556791 11.00000 0.18966 0.09418 = 0.10742 0.01153 -0.02695 0.06533 O7 6 0.650737 0.310155 0.514149 11.00000 0.09723 0.06061 = 0.05834 0.00740 0.01984 0.02990 C11 1 0.848079 0.411351 0.655471 11.00000 0.02953 0.04541 = 0.04543 -0.00368 -0.00328 0.00211 F3 4 0.817114 0.070816 0.456545 11.00000 0.15353 0.10933 = 0.13907 -0.03192 0.02695 0.05939 C12 1 0.972684 0.436223 0.674999 11.00000 0.03206 0.05465 = 0.04609 -0.00555 0.00130 0.00076 C1 1 0.318151 0.389117 0.541051 11.00000 0.03988 0.03926 = 0.04272 0.00181 0.00246 -0.00209 F5 4 0.571641 0.426966 0.880495 11.00000 0.11604 0.15088 = 0.05079 0.01127 -0.00543 -0.03251 C2 1 0.202580 0.397436 0.519382 11.00000 0.03984 0.05357 = 0.05311 0.01201 -0.01005 -0.00477 AFIX 43 H2 2 0.175311 0.459288 0.493818 11.00000 -1.20000 AFIX 0 O5 6 0.715694 0.482592 0.771974 11.00000 0.05481 0.11371 = 0.08366 -0.01971 -0.00220 -0.00114 C5 1 0.357285 0.296384 0.581825 11.00000 0.03599 0.03843 = 0.04070 -0.00344 -0.00083 -0.00255 C9 1 0.511461 0.204998 0.643258 11.00000 0.04292 0.03802 = 0.04090 0.00297 -0.00004 -0.00205 F6 4 0.559455 0.308105 0.803357 11.00000 0.21311 0.06602 = 0.10553 0.01998 0.03459 -0.00307 C17 1 1.015713 0.533941 0.652537 11.00000 0.04012 0.07629 = 0.05023 0.01638 -0.00317 -0.01155 AFIX 43 H17 2 0.966552 0.583668 0.627101 11.00000 -1.20000 AFIX 0 O9 6 0.838295 0.315494 0.472987 11.00000 0.05113 0.11560 = 0.12456 0.01343 -0.00760 -0.01603 C8 1 0.438302 0.117812 0.660371 11.00000 0.05889 0.03939 = 0.05353 0.00799 -0.00656 -0.00470 AFIX 43 H8 2 0.468048 0.058128 0.687079 11.00000 -1.20000 AFIX 0 C10 1 0.636575 0.209547 0.666945 11.00000 0.03913 0.04537 = 0.05111 0.01096 -0.00259 0.00304 AFIX 43 H10 2 0.675394 0.150858 0.690648 11.00000 -1.20000 AFIX 0 O6 6 0.562216 0.613316 0.783204 11.00000 0.12856 0.04528 = 0.08018 -0.00981 -0.00363 -0.00293 C13 1 1.046537 0.363679 0.713714 11.00000 0.04476 0.05899 = 0.08193 -0.00537 -0.01563 0.00624 AFIX 43 H13 2 1.017918 0.297385 0.730121 11.00000 -1.20000 AFIX 0 C14 1 1.161819 0.390292 0.727615 11.00000 0.03935 0.07677 = 0.10289 -0.00585 -0.01866 0.00583 AFIX 43 H14 2 1.211301 0.341318 0.753433 11.00000 -1.20000 AFIX 0 F4 4 0.420264 0.415846 0.814011 11.00000 0.06171 0.24267 = 0.11152 0.06099 0.00388 -0.03231 C15 1 1.204844 0.485544 0.704762 11.00000 0.03339 0.11749 = 0.07553 -0.01067 0.00094 -0.00919 AFIX 43 H15 2 1.283759 0.501458 0.714202 11.00000 -1.20000 AFIX 0 C6 1 0.278625 0.212040 0.597650 11.00000 0.04594 0.04567 = 0.05406 0.00219 -0.00225 -0.01072 C18 1 0.646242 0.736647 0.624180 11.00000 0.08375 0.06200 = 0.09717 -0.00520 -0.01724 -0.01310 AFIX 23 H18A 2 0.642892 0.743474 0.672547 11.00000 -1.20000 H18B 2 0.724908 0.714760 0.617448 11.00000 -1.20000 AFIX 0 C7 1 0.323359 0.122485 0.637128 11.00000 0.05677 0.04285 = 0.07206 0.00966 -0.00253 -0.01704 AFIX 43 H7 2 0.274024 0.065119 0.647746 11.00000 -1.20000 AFIX 0 F1 4 0.649284 0.069396 0.490259 11.00000 0.14052 0.07484 = 0.20333 0.02591 0.01213 -0.02250 C21 1 0.746828 0.124650 0.494964 11.00000 0.09091 0.06101 = 0.09868 -0.02156 0.00068 0.02220 C3 1 0.124765 0.315490 0.534689 11.00000 0.03329 0.07953 = 0.06718 0.01488 0.00122 -0.00796 AFIX 43 H3A 2 0.046454 0.323409 0.518647 11.00000 -1.20000 AFIX 0 C16 1 1.133250 0.559393 0.667645 11.00000 0.05694 0.10964 = 0.06239 0.01912 0.00569 -0.03069 AFIX 43 H16 2 1.162856 0.626225 0.652574 11.00000 -1.20000 AFIX 0 C20 1 0.532958 0.411072 0.817120 11.00000 0.05669 0.07215 = 0.06293 0.00298 -0.00319 -0.00951 C4 1 0.159044 0.224571 0.572136 11.00000 0.04335 0.06682 = 0.06495 0.00524 0.00235 -0.01798 AFIX 43 H4 2 0.105043 0.170428 0.581251 11.00000 -1.20000 AFIX 0 C19 1 0.622623 0.842243 0.593909 11.00000 0.11216 0.05827 = 0.12998 0.00424 -0.00821 -0.02545 AFIX 137 H19A 2 0.600787 0.832762 0.546198 11.00000 -1.50000 H19B 2 0.690911 0.888456 0.601051 11.00000 -1.50000 H19C 2 0.560074 0.877482 0.613847 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_13444_a.res in P2(1)/n REM R1 = 0.0584 for 4129 Fo > 4sig(Fo) and 0.0952 for all 6131 data REM 380 parameters refined using 0 restraints END WGHT 0.0511 3.5276 REM Highest difference peak 1.949, deepest hole -1.473, 1-sigma level 0.154 Q1 1 0.7628 0.5482 0.7425 11.00000 0.05 1.95 Q2 1 0.5530 0.3721 0.5909 11.00000 0.05 1.41 Q3 1 0.5204 0.5428 0.7593 11.00000 0.05 1.35 Q4 1 0.6188 0.5319 0.5764 11.00000 0.05 1.29 Q5 1 0.6246 0.3759 0.5799 11.00000 0.05 1.24 Q6 1 0.5525 0.5394 0.5925 11.00000 0.05 1.20 Q7 1 0.6054 0.4676 0.6281 11.00000 0.05 1.20 Q8 1 0.6085 0.5218 0.5430 11.00000 0.05 1.01 Q9 1 0.7599 0.3579 0.7403 11.00000 0.05 1.01 Q10 1 0.6038 0.3766 0.5464 11.00000 0.05 1.00 Q11 1 0.6591 0.4515 0.5547 11.00000 0.05 0.96 Q12 1 0.5655 0.4388 0.5347 11.00000 0.05 0.94 Q13 1 0.5620 0.4091 0.5487 11.00000 0.05 0.93 Q14 1 0.5427 0.5029 0.5568 11.00000 0.05 0.93 Q15 1 0.5838 0.6405 0.5799 11.00000 0.05 0.93 Q16 1 0.6575 0.5639 0.7814 11.00000 0.05 0.82 Q17 1 0.5071 0.4446 0.6123 11.00000 0.05 0.79 Q18 1 0.5044 0.6553 0.6154 11.00000 0.05 0.61 Q19 1 0.5908 0.5956 0.6267 11.00000 0.05 0.60 Q20 1 0.4402 0.5837 0.7780 11.00000 0.05 0.60 ; _shelx_res_checksum 33754 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Dy1 Dy 0.58788(3) 0.45264(3) 0.58093(2) 0.03916(14) Uani 1 1 d . . S1 S 0.5927(2) 0.50760(19) 0.76116(11) 0.0574(5) Uani 1 1 d . . S2 S 0.72614(18) 0.26745(19) 0.46655(11) 0.0559(5) Uani 1 1 d . . O2 O 0.4018(4) 0.4640(4) 0.5267(2) 0.0381(11) Uani 1 1 d . . O1 O 0.7816(4) 0.4820(4) 0.6250(3) 0.0441(12) Uani 1 1 d . . N1 N 0.4715(5) 0.2913(5) 0.6050(3) 0.0380(13) Uani 1 1 d . . N3 N 0.8047(5) 0.3124(5) 0.6706(3) 0.0431(14) Uani 1 1 d . . H3 H 0.8473 0.2603 0.6903 0.052 Uiso 1 1 calc R U N2 N 0.6878(5) 0.2991(5) 0.6528(3) 0.0399(14) Uani 1 1 d . . O4 O 0.5369(5) 0.4754(4) 0.6951(3) 0.0517(13) Uani 1 1 d . . O3 O 0.5675(4) 0.6493(4) 0.5983(3) 0.0553(14) Uani 1 1 d . . O8 O 0.6668(5) 0.2598(6) 0.3997(3) 0.0758(18) Uani 1 1 d . . F2 F 0.7991(7) 0.1205(6) 0.5568(4) 0.134(3) Uani 1 1 d . . O7 O 0.6507(6) 0.3102(5) 0.5141(3) 0.0712(18) Uani 1 1 d . . C11 C 0.8481(6) 0.4114(6) 0.6555(4) 0.0407(17) Uani 1 1 d . . F3 F 0.8171(7) 0.0708(6) 0.4565(4) 0.133(3) Uani 1 1 d . . C12 C 0.9727(6) 0.4362(6) 0.6750(4) 0.0445(18) Uani 1 1 d . . C1 C 0.3182(6) 0.3891(6) 0.5411(4) 0.0408(17) Uani 1 1 d . . F5 F 0.5716(6) 0.4270(6) 0.8805(3) 0.107(2) Uani 1 1 d . . C2 C 0.2026(6) 0.3974(7) 0.5194(4) 0.0500(19) Uani 1 1 d . . H2 H 0.1753 0.4593 0.4938 0.060 Uiso 1 1 calc R U O5 O 0.7157(5) 0.4826(6) 0.7720(3) 0.085(2) Uani 1 1 d . . C5 C 0.3573(6) 0.2964(6) 0.5818(3) 0.0388(16) Uani 1 1 d . . C9 C 0.5115(6) 0.2050(6) 0.6433(4) 0.0410(17) Uani 1 1 d . . F6 F 0.5595(8) 0.3081(5) 0.8034(3) 0.127(3) Uani 1 1 d . . C17 C 1.0157(7) 0.5339(7) 0.6525(4) 0.056(2) Uani 1 1 d . . H17 H 0.9666 0.5837 0.6271 0.067 Uiso 1 1 calc R U O9 O 0.8383(5) 0.3155(6) 0.4730(4) 0.098(2) Uani 1 1 d . . C8 C 0.4383(7) 0.1178(6) 0.6604(4) 0.052(2) Uani 1 1 d . . H8 H 0.4680 0.0581 0.6871 0.062 Uiso 1 1 calc R U C10 C 0.6366(6) 0.2095(7) 0.6669(4) 0.0458(18) Uani 1 1 d . . H10 H 0.6754 0.1509 0.6906 0.055 Uiso 1 1 calc R U O6 O 0.5622(6) 0.6133(5) 0.7832(3) 0.086(2) Uani 1 1 d . . C13 C 1.0465(7) 0.3637(8) 0.7137(5) 0.064(2) Uani 1 1 d . . H13 H 1.0179 0.2974 0.7301 0.076 Uiso 1 1 calc R U C14 C 1.1618(7) 0.3903(8) 0.7276(5) 0.075(3) Uani 1 1 d . . H14 H 1.2113 0.3413 0.7534 0.090 Uiso 1 1 calc R U F4 F 0.4203(5) 0.4158(8) 0.8140(4) 0.139(3) Uani 1 1 d . . C15 C 1.2048(7) 0.4855(10) 0.7048(5) 0.076(3) Uani 1 1 d . . H15 H 1.2838 0.5015 0.7142 0.091 Uiso 1 1 calc R U C6 C 0.2786(6) 0.2120(6) 0.5977(4) 0.0492(19) Uani 1 1 d . . C18 C 0.6462(9) 0.7366(8) 0.6242(6) 0.083(3) Uani 1 1 d . . H18A H 0.6429 0.7435 0.6725 0.100 Uiso 1 1 calc R U H18B H 0.7249 0.7148 0.6174 0.100 Uiso 1 1 calc R U C7 C 0.3234(7) 0.1225(7) 0.6371(4) 0.058(2) Uani 1 1 d . . H7 H 0.2740 0.0651 0.6477 0.070 Uiso 1 1 calc R U F1 F 0.6493(8) 0.0694(6) 0.4903(5) 0.140(3) Uani 1 1 d . . C21 C 0.7468(11) 0.1246(9) 0.4950(6) 0.084(3) Uani 1 1 d . . C3 C 0.1248(7) 0.3155(7) 0.5347(4) 0.060(2) Uani 1 1 d . . H3A H 0.0465 0.3234 0.5186 0.072 Uiso 1 1 calc R U C16 C 1.1332(8) 0.5594(9) 0.6676(5) 0.076(3) Uani 1 1 d . . H16 H 1.1629 0.6262 0.6526 0.092 Uiso 1 1 calc R U C20 C 0.5330(8) 0.4111(9) 0.8171(5) 0.065(2) Uani 1 1 d . . C4 C 0.1590(7) 0.2246(7) 0.5721(4) 0.059(2) Uani 1 1 d . . H4 H 0.1050 0.1704 0.5813 0.070 Uiso 1 1 calc R U C19 C 0.6226(10) 0.8422(9) 0.5939(6) 0.102(4) Uani 1 1 d . . H19A H 0.6008 0.8328 0.5462 0.153 Uiso 1 1 calc R U H19B H 0.6909 0.8885 0.6011 0.153 Uiso 1 1 calc R U H19C H 0.5601 0.8775 0.6138 0.153 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 Dy1 0.0334(2) 0.0372(2) 0.0447(2) 0.00420(16) -0.00533(14) -0.00204(15) S1 0.0650(14) 0.0526(13) 0.0535(13) -0.0057(11) 0.0013(10) -0.0104(11) S2 0.0502(12) 0.0614(14) 0.0554(13) -0.0008(11) 0.0033(10) -0.0006(10) O2 0.032(2) 0.039(3) 0.041(3) 0.011(2) -0.004(2) -0.002(2) O1 0.035(3) 0.040(3) 0.055(3) 0.003(2) -0.007(2) -0.003(2) N1 0.032(3) 0.039(3) 0.041(3) 0.000(3) -0.005(3) -0.002(2) N3 0.033(3) 0.041(4) 0.052(4) 0.007(3) -0.007(3) 0.002(3) N2 0.037(3) 0.034(3) 0.046(4) 0.001(3) -0.004(3) 0.000(3) O4 0.057(3) 0.043(3) 0.054(3) -0.009(2) 0.003(3) -0.001(2) O3 0.047(3) 0.033(3) 0.081(4) 0.006(3) -0.015(3) -0.009(2) O8 0.071(4) 0.095(5) 0.059(4) -0.004(4) -0.002(3) -0.004(4) F2 0.190(8) 0.094(5) 0.107(6) 0.012(4) -0.027(5) 0.065(5) O7 0.097(5) 0.061(4) 0.058(4) 0.007(3) 0.020(3) 0.030(3) C11 0.030(3) 0.045(4) 0.045(4) -0.004(4) -0.003(3) 0.002(3) F3 0.154(7) 0.109(5) 0.139(6) -0.032(5) 0.027(5) 0.059(5) C12 0.032(4) 0.055(5) 0.046(4) -0.006(4) 0.001(3) 0.001(3) C1 0.040(4) 0.039(4) 0.043(4) 0.002(3) 0.002(3) -0.002(3) F5 0.116(5) 0.151(6) 0.051(3) 0.011(4) -0.005(3) -0.033(4) C2 0.040(4) 0.054(5) 0.053(5) 0.012(4) -0.010(4) -0.005(4) O5 0.055(4) 0.114(6) 0.084(5) -0.020(4) -0.002(3) -0.001(4) C5 0.036(4) 0.038(4) 0.041(4) -0.003(3) -0.001(3) -0.003(3) C9 0.043(4) 0.038(4) 0.041(4) 0.003(3) 0.000(3) -0.002(3) F6 0.213(9) 0.066(4) 0.106(5) 0.020(4) 0.035(5) -0.003(5) C17 0.040(4) 0.076(6) 0.050(5) 0.016(4) -0.003(4) -0.012(4) O9 0.051(4) 0.116(6) 0.125(6) 0.013(5) -0.008(4) -0.016(4) C8 0.059(5) 0.039(4) 0.054(5) 0.008(4) -0.007(4) -0.005(4) C10 0.039(4) 0.045(4) 0.051(5) 0.011(4) -0.003(3) 0.003(3) O6 0.129(6) 0.045(4) 0.080(5) -0.010(3) -0.004(4) -0.003(4) C13 0.045(4) 0.059(5) 0.082(6) -0.005(5) -0.016(4) 0.006(4) C14 0.039(5) 0.077(7) 0.103(8) -0.006(6) -0.019(5) 0.006(5) F4 0.062(4) 0.243(9) 0.112(5) 0.061(6) 0.004(4) -0.032(5) C15 0.033(4) 0.117(9) 0.076(7) -0.011(6) 0.001(4) -0.009(5) C6 0.046(4) 0.046(5) 0.054(5) 0.002(4) -0.002(4) -0.011(4) C18 0.084(7) 0.062(6) 0.097(8) -0.005(6) -0.017(6) -0.013(6) C7 0.057(5) 0.043(5) 0.072(6) 0.010(4) -0.003(4) -0.017(4) F1 0.141(7) 0.075(5) 0.203(9) 0.026(5) 0.012(7) -0.022(5) C21 0.091(8) 0.061(7) 0.099(9) -0.022(6) 0.001(7) 0.022(6) C3 0.033(4) 0.080(6) 0.067(6) 0.015(5) 0.001(4) -0.008(4) C16 0.057(6) 0.110(8) 0.062(6) 0.019(6) 0.006(5) -0.031(6) C20 0.057(6) 0.072(6) 0.063(6) 0.003(5) -0.003(5) -0.010(5) C4 0.043(4) 0.067(6) 0.065(6) 0.005(5) 0.002(4) -0.018(4) C19 0.112(9) 0.058(7) 0.130(10) 0.004(7) -0.008(8) -0.025(6) 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 O2 Dy1 O7 96.4(2) . . O2 Dy1 O1 166.74(17) . . O7 Dy1 O1 88.6(2) . . O2 Dy1 O2 72.13(18) . 3_666 O7 Dy1 O2 74.94(17) . 3_666 O1 Dy1 O2 97.53(16) . 3_666 O2 Dy1 O3 84.69(16) . . O7 Dy1 O3 147.5(2) . . O1 Dy1 O3 84.53(16) . . O2 Dy1 O3 74.61(18) 3_666 . O2 Dy1 O4 96.77(17) . . O7 Dy1 O4 137.92(18) . . O1 Dy1 O4 87.53(18) . . O2 Dy1 O4 147.05(16) 3_666 . O3 Dy1 O4 73.51(18) . . O2 Dy1 N1 68.17(16) . . O7 Dy1 N1 75.5(2) . . O1 Dy1 N1 125.06(17) . . O2 Dy1 N1 126.54(17) 3_666 . O3 Dy1 N1 133.22(18) . . O4 Dy1 N1 72.83(18) . . O2 Dy1 N2 130.77(17) . . O7 Dy1 N2 68.88(19) . . O1 Dy1 N2 62.49(17) . . O2 Dy1 N2 138.42(17) 3_666 . O3 Dy1 N2 132.72(18) . . O4 Dy1 N2 72.26(18) . . N1 Dy1 N2 62.70(18) . . O2 Dy1 Dy1 36.75(11) . 3_666 O7 Dy1 Dy1 84.54(14) . 3_666 O1 Dy1 Dy1 132.42(12) . 3_666 O2 Dy1 Dy1 35.39(11) 3_666 3_666 O3 Dy1 Dy1 77.11(12) . 3_666 O4 Dy1 Dy1 126.82(12) . 3_666 N1 Dy1 Dy1 98.51(13) . 3_666 N2 Dy1 Dy1 150.17(13) . 3_666 O6 S1 O5 114.8(4) . . O6 S1 O4 115.0(4) . . O5 S1 O4 114.2(4) . . O6 S1 C20 104.9(5) . . O5 S1 C20 102.5(5) . . O4 S1 C20 103.3(4) . . O9 S2 O8 116.8(4) . . O9 S2 O7 114.4(5) . . O8 S2 O7 111.6(4) . . O9 S2 C21 105.5(5) . . O8 S2 C21 105.3(5) . . O7 S2 C21 101.3(5) . . C1 O2 Dy1 120.6(4) . . C1 O2 Dy1 124.7(4) . 3_666 Dy1 O2 Dy1 107.86(18) . 3_666 C11 O1 Dy1 126.2(4) . . C9 N1 C5 119.5(6) . . C9 N1 Dy1 124.1(4) . . C5 N1 Dy1 116.1(4) . . C11 N3 N2 115.6(6) . . C11 N3 H3 122.2 . . N2 N3 H3 122.2 . . C10 N2 N3 120.9(6) . . C10 N2 Dy1 122.8(5) . . N3 N2 Dy1 116.0(4) . . S1 O4 Dy1 138.5(3) . . C18 O3 Dy1 133.9(5) . . S2 O7 Dy1 151.7(4) . . O1 C11 N3 118.7(6) . . O1 C11 C12 121.3(7) . . N3 C11 C12 120.0(6) . . C17 C12 C13 119.4(7) . . C17 C12 C11 117.8(7) . . C13 C12 C11 122.8(7) . . C2 C1 O2 125.3(6) . . C2 C1 C5 118.5(7) . . O2 C1 C5 116.2(6) . . C1 C2 C3 121.2(7) . . C1 C2 H2 119.4 . . C3 C2 H2 119.4 . . N1 C5 C1 117.9(6) . . N1 C5 C6 121.4(6) . . C1 C5 C6 120.7(6) . . N1 C9 C8 122.0(7) . . N1 C9 C10 114.8(6) . . C8 C9 C10 123.1(7) . . C12 C17 C16 120.0(8) . . C12 C17 H17 120.0 . . C16 C17 H17 120.0 . . C7 C8 C9 118.7(7) . . C7 C8 H8 120.7 . . C9 C8 H8 120.7 . . N2 C10 C9 115.3(7) . . N2 C10 H10 122.4 . . C9 C10 H10 122.4 . . C14 C13 C12 119.5(9) . . C14 C13 H13 120.2 . . C12 C13 H13 120.2 . . C15 C14 C13 121.3(9) . . C15 C14 H14 119.4 . . C13 C14 H14 119.4 . . C14 C15 C16 120.3(8) . . C14 C15 H15 119.9 . . C16 C15 H15 119.9 . . C7 C6 C5 117.6(7) . . C7 C6 C4 124.4(7) . . C5 C6 C4 117.9(7) . . C19 C18 O3 114.2(8) . . C19 C18 H18A 108.7 . . O3 C18 H18A 108.7 . . C19 C18 H18B 108.7 . . O3 C18 H18B 108.7 . . H18A C18 H18B 107.6 . . C8 C7 C6 120.7(7) . . C8 C7 H7 119.6 . . C6 C7 H7 119.6 . . F1 C21 F2 110.7(12) . . F1 C21 F3 107.1(9) . . F2 C21 F3 105.8(9) . . F1 C21 S2 111.9(8) . . F2 C21 S2 111.2(8) . . F3 C21 S2 110.0(9) . . C4 C3 C2 122.0(7) . . C4 C3 H3A 119.0 . . C2 C3 H3A 119.0 . . C15 C16 C17 119.5(9) . . C15 C16 H16 120.2 . . C17 C16 H16 120.2 . . F4 C20 F6 106.9(9) . . F4 C20 F5 105.8(9) . . F6 C20 F5 106.1(9) . . F4 C20 S1 113.4(7) . . F6 C20 S1 111.0(7) . . F5 C20 S1 113.1(7) . . C3 C4 C6 119.5(7) . . C3 C4 H4 120.2 . . C6 C4 H4 120.2 . . C18 C19 H19A 109.5 . . C18 C19 H19B 109.5 . . H19A C19 H19B 109.5 . . C18 C19 H19C 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy1 O2 2.299(4) . Dy1 O7 2.322(5) . Dy1 O1 2.337(4) . Dy1 O2 2.375(4) 3_666 Dy1 O3 2.385(5) . Dy1 O4 2.423(5) . Dy1 N1 2.426(5) . Dy1 N2 2.520(6) . Dy1 Dy1 3.7778(8) 3_666 S1 O6 1.392(6) . S1 O5 1.446(6) . S1 O4 1.448(5) . S1 C20 1.792(10) . S2 O9 1.410(6) . S2 O8 1.428(6) . S2 O7 1.450(6) . S2 C21 1.801(11) . O2 C1 1.369(8) . O2 Dy1 2.375(4) 3_666 O1 C11 1.249(8) . N1 C9 1.331(8) . N1 C5 1.349(8) . N3 C11 1.330(9) . N3 N2 1.367(7) . N3 H3 0.8600 . N2 C10 1.268(9) . O3 C18 1.439(10) . F2 C21 1.308(12) . C11 C12 1.479(9) . F3 C21 1.340(12) . C12 C17 1.362(10) . C12 C13 1.386(10) . C1 C2 1.360(9) . C1 C5 1.414(9) . F5 C20 1.302(10) . C2 C3 1.385(10) . C2 H2 0.9300 . C5 C6 1.415(9) . C9 C8 1.406(10) . C9 C10 1.471(9) . F6 C20 1.302(11) . C17 C16 1.392(11) . C17 H17 0.9300 . C8 C7 1.358(11) . C8 H8 0.9300 . C10 H10 0.9300 . C13 C14 1.368(11) . C13 H13 0.9300 . C14 C15 1.340(13) . C14 H14 0.9300 . F4 C20 1.299(10) . C15 C16 1.366(13) . C15 H15 0.9300 . C6 C7 1.390(10) . C6 C4 1.426(10) . C18 C19 1.408(13) . C18 H18A 0.9700 . C18 H18B 0.9700 . C7 H7 0.9300 . F1 C21 1.300(13) . C3 C4 1.349(11) . C3 H3A 0.9300 . C16 H16 0.9300 . C4 H4 0.9300 . C19 H19A 0.9600 . C19 H19B 0.9600 . C19 H19C 0.9600 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 C11 N3 N2 C10 -177.5(7) . C11 N3 N2 Dy1 8.5(7) . O6 S1 O4 Dy1 107.1(5) . O5 S1 O4 Dy1 -28.7(6) . C20 S1 O4 Dy1 -139.2(5) . O9 S2 O7 Dy1 31.6(9) . O8 S2 O7 Dy1 -103.8(8) . C21 S2 O7 Dy1 144.5(8) . Dy1 O1 C11 N3 -6.7(10) . Dy1 O1 C11 C12 173.7(5) . N2 N3 C11 O1 -2.1(10) . N2 N3 C11 C12 177.6(6) . O1 C11 C12 C17 -6.8(11) . N3 C11 C12 C17 173.5(7) . O1 C11 C12 C13 174.4(8) . N3 C11 C12 C13 -5.2(11) . Dy1 O2 C1 C2 170.2(6) . Dy1 O2 C1 C2 -42.2(9) 3_666 Dy1 O2 C1 C5 -9.7(8) . Dy1 O2 C1 C5 137.8(5) 3_666 O2 C1 C2 C3 177.9(7) . C5 C1 C2 C3 -2.2(12) . C9 N1 C5 C1 -179.7(6) . Dy1 N1 C5 C1 5.5(8) . C9 N1 C5 C6 0.4(10) . Dy1 N1 C5 C6 -174.5(5) . C2 C1 C5 N1 -177.6(7) . O2 C1 C5 N1 2.3(9) . C2 C1 C5 C6 2.3(11) . O2 C1 C5 C6 -177.8(6) . C5 N1 C9 C8 0.2(10) . Dy1 N1 C9 C8 174.6(5) . C5 N1 C9 C10 -178.6(6) . Dy1 N1 C9 C10 -4.2(9) . C13 C12 C17 C16 1.0(13) . C11 C12 C17 C16 -177.9(8) . N1 C9 C8 C7 -0.2(12) . C10 C9 C8 C7 178.6(8) . N3 N2 C10 C9 -178.4(6) . Dy1 N2 C10 C9 -4.9(9) . N1 C9 C10 N2 5.7(10) . C8 C9 C10 N2 -173.1(7) . C17 C12 C13 C14 -1.3(13) . C11 C12 C13 C14 177.5(8) . C12 C13 C14 C15 0.3(15) . C13 C14 C15 C16 1.0(16) . N1 C5 C6 C7 -1.0(11) . C1 C5 C6 C7 179.1(7) . N1 C5 C6 C4 179.0(7) . C1 C5 C6 C4 -1.0(11) . Dy1 O3 C18 C19 146.9(8) . C9 C8 C7 C6 -0.5(13) . C5 C6 C7 C8 1.1(12) . C4 C6 C7 C8 -178.9(8) . O9 S2 C21 F1 -178.6(9) . O8 S2 C21 F1 -54.5(10) . O7 S2 C21 F1 61.9(10) . O9 S2 C21 F2 57.0(10) . O8 S2 C21 F2 -178.9(8) . O7 S2 C21 F2 -62.5(10) . O9 S2 C21 F3 -59.8(9) . O8 S2 C21 F3 64.3(9) . O7 S2 C21 F3 -179.3(8) . C1 C2 C3 C4 0.7(14) . C14 C15 C16 C17 -1.3(16) . C12 C17 C16 C15 0.3(14) . O6 S1 C20 F4 62.1(9) . O5 S1 C20 F4 -177.6(8) . O4 S1 C20 F4 -58.7(9) . O6 S1 C20 F6 -177.6(7) . O5 S1 C20 F6 -57.3(8) . O4 S1 C20 F6 61.6(8) . O6 S1 C20 F5 -58.4(8) . O5 S1 C20 F5 61.9(8) . O4 S1 C20 F5 -179.2(7) . C2 C3 C4 C6 0.7(13) . C7 C6 C4 C3 179.4(8) . C5 C6 C4 C3 -0.5(12) .