#------------------------------------------------------------------------------ #$Date: 2019-10-08 03:56:03 +0300 (Tue, 08 Oct 2019) $ #$Revision: 219140 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234434.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_7234434 loop_ _publ_author_name 'Wang, Juan' 'Yang, Mingfang' 'Sun, Juan' 'Li, Hui' 'Liu, Jinjin' 'Wang, Qinglun' 'Li, Licun' 'Ma, Yue' 'Zhao, Bin' 'Cheng, Peng' _publ_section_title ; Enhancing the energy barrier of dysprosium(iii) single-molecule magnets by tuning the magnetic interactions through different N-oxide bridging ligands ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C9CE01378D _journal_year 2019 _chemical_formula_moiety 'C38 H14 Dy2 F36 N4 O14' _chemical_formula_sum 'C38 H14 Dy2 F36 N4 O14' _chemical_formula_weight 1759.53 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-03-05 deposited with the CCDC. 2019-09-30 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.89(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.823(4) _cell_length_b 12.791(3) _cell_length_c 22.346(4) _cell_measurement_reflns_used 9102 _cell_measurement_temperature 113 _cell_measurement_theta_max 27.99 _cell_measurement_theta_min 3.065 _cell_volume 5778(2) _computing_cell_refinement ; CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015) ; _computing_data_collection ; CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015) ; _computing_data_reduction ; CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015) ; _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 113 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Rigaku Pilatus 200K' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_unetI/netI 0.0765 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 21137 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.483 _diffrn_reflns_theta_min 3.067 _exptl_absorpt_coefficient_mu 2.744 _exptl_absorpt_correction_T_max 0.760 _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorles _exptl_crystal_density_diffrn 2.023 _exptl_crystal_description block _exptl_crystal_F_000 3352 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.835 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 505 _refine_ls_number_reflns 6628 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.998 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0531 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.0956 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4048 _reflns_number_total 6628 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce01378d2.cif _cod_data_source_block shelxl _cod_database_code 7234434 _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 ; shelxl.res created by SHELXL-2014/7 TITL shelxl in Cc New: C2/c New: C2/c CELL 0.71073 20.823 12.791 22.346 90 103.89 90 ZERR 4 0.004 0.003 0.004 0 0.03 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Dy F N O UNIT 152 56 8 144 16 56 L.S. 5 PLAN -20 BOND $H CONF fmap 2 acta REM REM REM WGHT 0.028000 FVAR 0.78557 DY1 3 0.304027 0.264601 0.089551 11.00000 0.06012 0.05102 = 0.07373 -0.00712 0.02329 -0.00552 PART 5 F1 4 0.433915 0.226281 0.297058 10.58600 0.22651 0.13521 = 0.12711 0.02979 -0.05371 -0.02107 PART 0 PART 1 F1AA 4 0.460871 0.201767 -0.052044 10.50060 0.12135 0.33899 = 0.10499 -0.02039 0.05784 0.03667 PART 0 PART 5 F2 4 0.352712 0.305013 0.312771 10.58600 0.22668 0.21125 = 0.09024 0.00467 0.08569 -0.03195 PART 0 PART 1 F2AA 4 0.496386 0.314209 0.015566 10.50060 0.16083 0.18195 = 0.22780 0.02033 0.11438 -0.05123 PART 0 PART 5 F3 4 0.450140 0.378525 0.326785 10.58600 0.22165 0.20999 = 0.08400 -0.01509 0.01398 -0.12757 PART 0 PART 1 F3AA 4 0.538091 0.172744 0.021435 10.50060 0.10419 0.27161 = 0.20023 0.05921 0.09803 0.06273 PART 0 F4 4 0.372325 0.636274 0.105957 11.00000 0.16001 0.07023 = 0.21100 0.02614 -0.01609 -0.01639 PART 3 F4AA 4 0.434822 -0.015800 0.214049 10.50770 0.30764 0.23848 = 0.07500 0.03168 -0.02539 0.04785 PART 0 F5 4 0.459826 0.621837 0.176096 11.00000 0.16763 0.11730 = 0.10894 -0.00993 0.00553 -0.08231 PART 3 F5AA 4 0.363715 -0.094761 0.151954 10.50770 0.20833 0.12755 = 0.24160 0.08697 0.01892 -0.01185 PART 0 F6 4 0.453837 0.561841 0.087458 11.00000 0.19723 0.14396 = 0.12949 -0.01300 0.08366 -0.08436 PART 3 F0AA 4 0.463236 -0.091898 0.141164 10.50770 0.38366 0.17758 = 0.26897 0.11499 0.21961 0.18823 PART 0 F7 4 0.207856 0.582294 0.141920 11.00000 0.21845 0.10172 = 0.32792 -0.04201 0.11663 0.03227 F8 4 0.122571 0.524660 0.097507 11.00000 0.17727 0.22568 = 0.35505 -0.00892 -0.00272 0.11932 F9 4 0.143893 0.526406 0.190546 11.00000 0.43548 0.18870 = 0.35578 0.02901 0.30658 0.13288 F10 4 0.148167 0.171035 0.249937 11.00000 0.49843 0.23958 = 0.33413 -0.04026 0.35009 -0.08303 F11 4 0.111957 0.106110 0.167922 11.00000 0.16285 0.26694 = 0.34573 0.11396 0.05941 -0.09084 F12 4 0.196451 0.057530 0.213922 11.00000 0.23261 0.20204 = 0.27910 0.10137 0.16025 0.01623 O1 6 0.355959 0.278922 0.191389 11.00000 0.09785 0.06373 = 0.07649 -0.00240 0.01318 -0.01781 O2 6 0.363931 0.420105 0.100906 11.00000 0.08070 0.06335 = 0.07087 -0.00553 0.01529 -0.01849 O3 6 0.232595 0.392940 0.106572 11.00000 0.08501 0.08257 = 0.10957 -0.00556 0.04247 0.01577 O4 6 0.228869 0.188546 0.137242 11.00000 0.08262 0.08606 = 0.10078 -0.00923 0.04336 -0.02029 O5 6 0.351445 0.102452 0.117641 11.00000 0.07967 0.06393 = 0.09630 0.00612 0.02654 0.00835 O6 6 0.387660 0.242116 0.038921 11.00000 0.07278 0.07159 = 0.09804 0.00116 0.03900 0.00524 O7 6 0.238828 0.155518 0.010094 11.00000 0.07954 0.03979 = 0.07792 -0.00343 0.01526 -0.01497 PART 4 F13 4 0.392784 -0.118016 0.111176 10.49230 0.16796 0.06421 = 0.22562 0.02025 -0.02244 -0.00012 F14 4 0.482037 -0.063882 0.164630 10.49230 0.11407 0.15894 = 0.18812 0.05699 -0.01572 0.05386 F15 4 0.401016 -0.046983 0.193002 10.49230 0.24296 0.13861 = 0.17962 0.08295 0.12399 0.09134 PART 0 PART 2 F16 4 0.511861 0.127330 -0.012606 10.49940 0.20310 0.16657 = 0.21430 -0.04803 0.14781 0.02089 PART 0 PART 6 F16' 4 0.461384 0.247570 0.305420 10.41400 0.18486 0.11542 = 0.07795 -0.01600 -0.03045 0.05714 PART 0 PART 2 F17 4 0.452719 0.258820 -0.042293 10.49940 0.13405 0.25738 = 0.14623 0.07466 0.10480 0.05123 PART 0 PART 6 F17' 4 0.368973 0.276129 0.315975 10.41400 0.15278 0.22459 = 0.12983 0.06112 -0.00217 -0.09035 PART 0 PART 2 F18 4 0.530814 0.264705 0.039870 10.49940 0.14148 0.31131 = 0.20085 -0.10063 0.08819 -0.13168 PART 0 PART 6 F18' 4 0.435056 0.395334 0.333014 10.41400 0.20833 0.07868 = 0.05397 -0.00728 0.02729 0.02419 PART 0 N1 5 0.227311 0.055142 0.019180 11.00000 0.09690 0.05215 = 0.08284 -0.00584 0.00513 -0.01264 N2 5 0.204855 -0.149331 0.040267 11.00000 0.25340 0.07124 = 0.15908 0.01322 -0.01656 -0.06315 C1 1 0.410847 0.316111 0.293892 11.00000 0.14075 0.09766 = 0.09152 0.00059 0.01728 -0.02956 C2 1 0.388729 0.347367 0.225194 11.00000 0.08975 0.08080 = 0.06234 0.00177 0.02361 -0.00393 C3 1 0.410118 0.440998 0.207909 11.00000 0.09224 0.08190 = 0.06834 -0.01354 0.01714 -0.01947 AFIX 43 H3 2 0.434815 0.485503 0.237600 11.00000 -1.20000 AFIX 0 C4 1 0.395251 0.470061 0.146440 11.00000 0.06845 0.06350 = 0.07606 -0.01240 0.02407 -0.00662 C5 1 0.420397 0.573696 0.129839 11.00000 0.11114 0.08013 = 0.08028 -0.00422 0.01232 -0.03324 C6 1 0.169562 0.509854 0.144597 11.00000 0.11675 0.13114 = 0.27270 -0.03399 0.09730 0.03914 C7 1 0.196846 0.401814 0.143413 11.00000 0.07477 0.11460 = 0.10733 -0.02084 0.02802 0.02016 C8 1 0.179014 0.325423 0.179080 11.00000 0.10197 0.14494 = 0.12218 -0.01777 0.06520 0.00879 AFIX 43 H8 2 0.156295 0.342867 0.208783 11.00000 -1.20000 AFIX 0 C9 1 0.194622 0.223310 0.171036 11.00000 0.07655 0.13119 = 0.09161 -0.00937 0.03292 -0.01904 C10 1 0.167729 0.141136 0.207723 11.00000 0.14550 0.14700 = 0.27096 0.01667 0.15422 -0.00998 C11 1 0.420895 -0.040033 0.151468 11.00000 0.12660 0.11914 = 0.12943 0.03013 0.05280 0.03601 C12 1 0.403856 0.060751 0.114771 11.00000 0.09498 0.06328 = 0.08054 -0.00442 0.01203 0.00803 C13 1 0.448480 0.094215 0.082260 11.00000 0.07700 0.09883 = 0.10176 0.00770 0.02553 0.02572 AFIX 43 H13 2 0.487750 0.057669 0.085341 11.00000 -1.20000 AFIX 0 C14 1 0.435136 0.182339 0.044858 11.00000 0.06445 0.09262 = 0.09117 -0.01495 0.03291 -0.00415 C15 1 0.482856 0.211518 0.006159 11.00000 0.08753 0.12660 = 0.13336 0.01467 0.05165 0.01569 C16 1 0.269477 -0.016462 0.010286 11.00000 0.12750 0.05494 = 0.12587 -0.01710 -0.00219 -0.00110 AFIX 43 H16 2 0.307274 0.001851 -0.002546 11.00000 -1.20000 AFIX 0 C17 1 0.256023 -0.118021 0.020452 11.00000 0.20183 0.04895 = 0.15240 -0.00502 -0.02511 -0.01251 AFIX 43 H17 2 0.285084 -0.168703 0.012833 11.00000 -1.20000 AFIX 0 C18 1 0.164385 -0.074494 0.048382 11.00000 0.20314 0.10004 = 0.11186 0.01403 0.00906 -0.07403 AFIX 43 H18 2 0.127359 -0.093397 0.062308 11.00000 -1.20000 AFIX 0 C19 1 0.173272 0.030649 0.037553 11.00000 0.12661 0.09340 = 0.08418 0.00161 0.02219 -0.04743 AFIX 43 H19 2 0.142991 0.081134 0.042890 11.00000 -1.20000 AFIX 0 HKLF 4 1 -1 0 0 0 1 0 0 0 -1 REM shelxl in Cc New: C2/c New: C2/c REM R1 = 0.0531 for 4048 Fo > 4sig(Fo) and 0.1070 for all 6593 data REM 505 parameters refined using 0 restraints END WGHT 0.0280 0.0000 REM Highest difference peak 0.835, deepest hole -0.500, 1-sigma level 0.082 Q1 1 0.3385 0.2639 0.1399 11.00000 0.05 0.84 Q2 1 0.2704 0.2590 0.0405 11.00000 0.05 0.83 Q3 1 0.2957 0.1819 0.0681 11.00000 0.05 0.45 Q4 1 0.2917 0.3443 0.0734 11.00000 0.05 0.43 Q5 1 0.3220 0.3429 0.1142 11.00000 0.05 0.39 Q6 1 0.1001 0.2098 0.1963 11.00000 0.05 0.38 Q7 1 0.3633 0.2650 0.0903 11.00000 0.05 0.37 Q8 1 0.2437 0.2724 0.0884 11.00000 0.05 0.35 Q9 1 0.1631 0.1564 0.2685 11.00000 0.05 0.35 Q10 1 0.3775 0.2379 0.1765 11.00000 0.05 0.35 Q11 1 0.3701 0.3173 0.1807 11.00000 0.05 0.33 Q12 1 0.2068 0.2559 0.1094 11.00000 0.05 0.33 Q13 1 0.3764 0.2588 0.2232 11.00000 0.05 0.31 Q14 1 0.4207 0.0972 0.2847 11.00000 0.05 0.31 Q15 1 0.2042 0.5521 0.2075 11.00000 0.05 0.30 Q16 1 0.2399 0.2262 0.0006 11.00000 0.05 0.30 Q17 1 0.3217 0.1590 0.1102 11.00000 0.05 0.29 Q18 1 0.1002 -0.0241 0.0792 11.00000 0.05 0.29 Q19 1 0.5303 0.5366 0.0987 11.00000 0.05 0.29 Q20 1 0.2047 0.4966 0.2317 11.00000 0.05 0.28 ; _shelx_res_checksum 42118 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.30403(2) 0.26460(2) 0.08955(2) 0.06040(12) Uani 1 1 d . . . . . F1 F 0.4339(15) 0.226(2) 0.2971(14) 0.179(11) Uani 0.586 1 d . . P A 5 F1AA F 0.4609(14) 0.202(3) -0.0520(14) 0.183(14) Uani 0.5006 1 d . . P B 1 F2 F 0.3527(18) 0.305(3) 0.3128(11) 0.168(12) Uani 0.586 1 d . . P A 5 F2AA F 0.4964(17) 0.314(3) 0.0156(17) 0.179(12) Uani 0.5006 1 d . . P B 1 F3 F 0.4501(11) 0.3785(16) 0.3268(10) 0.176(10) Uani 0.586 1 d . . P A 5 F3AA F 0.5381(13) 0.173(3) 0.0214(16) 0.182(12) Uani 0.5006 1 d . . P B 1 F4 F 0.3723(3) 0.6363(3) 0.1060(3) 0.157(2) Uani 1 1 d . . . . . F4AA F 0.435(2) -0.016(2) 0.2140(12) 0.219(18) Uani 0.5077 1 d . . P C 3 F5 F 0.4598(2) 0.6218(3) 0.1761(2) 0.1360(18) Uani 1 1 d . . . . . F5AA F 0.3637(16) -0.095(2) 0.152(2) 0.198(13) Uani 0.5077 1 d . . P C 3 F6 F 0.4538(3) 0.5618(4) 0.0875(2) 0.149(2) Uani 1 1 d . . . . . F0AA F 0.463(3) -0.092(3) 0.141(2) 0.25(2) Uani 0.5077 1 d . . P C 3 F7 F 0.2079(4) 0.5823(5) 0.1419(4) 0.207(3) Uani 1 1 d . . . . . F8 F 0.1226(4) 0.5247(6) 0.0975(5) 0.264(5) Uani 1 1 d . . . . . F9 F 0.1439(6) 0.5264(6) 0.1905(4) 0.291(6) Uani 1 1 d . . . . . F10 F 0.1482(7) 0.1710(7) 0.2499(5) 0.315(7) Uani 1 1 d . . . . . F11 F 0.1120(4) 0.1061(7) 0.1679(4) 0.259(5) Uani 1 1 d . . . . . F12 F 0.1965(4) 0.0575(6) 0.2139(4) 0.221(4) Uani 1 1 d . . . . . O1 O 0.3560(2) 0.2789(3) 0.1914(2) 0.0807(12) Uani 1 1 d . . . . . O2 O 0.36393(18) 0.4201(3) 0.10091(18) 0.0721(11) Uani 1 1 d . . . . . O3 O 0.2326(2) 0.3929(3) 0.1066(2) 0.0891(13) Uani 1 1 d . . . . . O4 O 0.2289(2) 0.1885(3) 0.1372(2) 0.0862(13) Uani 1 1 d . . . . . O5 O 0.3514(2) 0.1025(3) 0.1176(2) 0.0790(12) Uani 1 1 d . . . . . O6 O 0.3877(2) 0.2421(3) 0.0389(2) 0.0777(12) Uani 1 1 d . . . . . O7 O 0.23883(16) 0.1555(2) 0.01009(16) 0.0664(11) Uani 1 1 d . . . . . F13 F 0.3928(15) -0.1180(12) 0.1112(13) 0.164(8) Uani 0.4923 1 d . . P C 4 F14 F 0.4820(11) -0.064(3) 0.1646(18) 0.163(15) Uani 0.4923 1 d . . P C 4 F15 F 0.401(2) -0.047(2) 0.1930(19) 0.175(14) Uani 0.4923 1 d . . P C 4 F16 F 0.5119(18) 0.127(2) -0.0126(17) 0.178(14) Uani 0.4994 1 d . . P B 2 F16' F 0.4614(16) 0.248(2) 0.3054(15) 0.137(11) Uani 0.414 1 d . . P A 6 F17 F 0.4527(15) 0.259(3) -0.0423(15) 0.167(13) Uani 0.4994 1 d . . P B 2 F17' F 0.369(3) 0.276(4) 0.3160(19) 0.175(19) Uani 0.414 1 d . . P A 6 F18 F 0.5308(16) 0.265(4) 0.0399(16) 0.210(19) Uani 0.4994 1 d . . P B 2 F18' F 0.4351(16) 0.3953(16) 0.3330(12) 0.114(9) Uani 0.414 1 d . . P A 6 N1 N 0.2273(3) 0.0551(4) 0.0192(2) 0.0801(15) Uani 1 1 d . . . . . N2 N 0.2049(6) -0.1493(6) 0.0403(5) 0.172(5) Uani 1 1 d . . . . . C1 C 0.4108(7) 0.3161(9) 0.2939(4) 0.112(3) Uani 1 1 d . . . . . C2 C 0.3887(3) 0.3474(5) 0.2252(3) 0.0767(17) Uani 1 1 d . . . . . C3 C 0.4101(3) 0.4410(5) 0.2079(3) 0.0812(18) Uani 1 1 d . . . . . H3 H 0.4348 0.4855 0.2376 0.097 Uiso 1 1 calc R U . . . C4 C 0.3953(3) 0.4701(4) 0.1464(3) 0.0682(16) Uani 1 1 d . . . . . C5 C 0.4204(4) 0.5737(6) 0.1298(4) 0.092(2) Uani 1 1 d . . . . . C6 C 0.1696(6) 0.5099(9) 0.1446(9) 0.165(5) Uani 1 1 d . . . . . C7 C 0.1968(3) 0.4018(7) 0.1434(4) 0.098(2) Uani 1 1 d . . . . . C8 C 0.1790(4) 0.3254(8) 0.1791(4) 0.117(3) Uani 1 1 d . . . . . H8 H 0.1563 0.3429 0.2088 0.140 Uiso 1 1 calc R U . . . C9 C 0.1946(4) 0.2233(7) 0.1710(4) 0.098(2) Uani 1 1 d . . . . . C10 C 0.1677(7) 0.1411(11) 0.2077(9) 0.170(6) Uani 1 1 d . . . . . C11 C 0.4209(7) -0.0400(10) 0.1515(8) 0.121(4) Uani 1 1 d . . . . . C12 C 0.4039(4) 0.0608(5) 0.1148(3) 0.0811(19) Uani 1 1 d . . . . . C13 C 0.4485(3) 0.0942(6) 0.0823(3) 0.092(2) Uani 1 1 d . . . . . H13 H 0.4877 0.0577 0.0853 0.110 Uiso 1 1 calc R U . . . C14 C 0.4351(3) 0.1823(6) 0.0449(3) 0.0803(18) Uani 1 1 d . . . . . C15 C 0.4829(6) 0.2115(10) 0.0062(7) 0.112(3) Uani 1 1 d . . . . . C16 C 0.2695(4) -0.0165(5) 0.0103(3) 0.108(3) Uani 1 1 d . . . . . H16 H 0.3073 0.0019 -0.0025 0.130 Uiso 1 1 calc R U . . . C17 C 0.2560(5) -0.1180(6) 0.0205(5) 0.146(5) Uani 1 1 d . . . . . H17 H 0.2851 -0.1687 0.0128 0.175 Uiso 1 1 calc R U . . . C18 C 0.1644(6) -0.0745(8) 0.0484(4) 0.143(4) Uani 1 1 d . . . . . H18 H 0.1274 -0.0934 0.0623 0.172 Uiso 1 1 calc R U . . . C19 C 0.1733(4) 0.0306(6) 0.0376(3) 0.102(2) Uani 1 1 d . . . . . H19 H 0.1430 0.0811 0.0429 0.122 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 0.06012(17) 0.05102(16) 0.0737(2) -0.00712(14) 0.02329(14) -0.00552(12) F1 0.23(3) 0.135(13) 0.127(16) 0.030(10) -0.054(13) -0.021(13) F1AA 0.121(17) 0.34(4) 0.105(13) -0.02(2) 0.058(12) 0.037(19) F2 0.23(3) 0.211(19) 0.090(12) 0.005(12) 0.086(16) -0.032(15) F2AA 0.16(2) 0.182(18) 0.23(3) 0.020(15) 0.11(2) -0.051(15) F3 0.222(17) 0.210(19) 0.084(11) -0.015(11) 0.014(11) -0.128(16) F3AA 0.104(15) 0.27(4) 0.20(3) 0.06(2) 0.098(19) 0.06(2) F4 0.160(4) 0.070(3) 0.211(6) 0.026(3) -0.016(4) -0.016(3) F4AA 0.31(3) 0.24(2) 0.075(10) 0.032(11) -0.025(15) 0.05(2) F5 0.168(4) 0.117(3) 0.109(3) -0.010(3) 0.006(3) -0.082(3) F5AA 0.21(2) 0.128(16) 0.24(3) 0.087(18) 0.019(19) -0.012(14) F6 0.197(5) 0.144(4) 0.129(4) -0.013(3) 0.084(4) -0.084(4) F0AA 0.38(6) 0.18(3) 0.27(4) 0.11(3) 0.22(4) 0.19(4) F7 0.218(7) 0.102(4) 0.328(10) -0.042(5) 0.117(7) 0.032(4) F8 0.177(7) 0.226(8) 0.355(13) -0.009(7) -0.003(8) 0.119(6) F9 0.435(12) 0.189(7) 0.356(13) 0.029(7) 0.307(12) 0.133(7) F10 0.498(16) 0.240(9) 0.334(13) -0.040(8) 0.350(14) -0.083(10) F11 0.163(6) 0.267(9) 0.346(12) 0.114(9) 0.059(7) -0.091(6) F12 0.233(8) 0.202(7) 0.279(9) 0.101(7) 0.160(7) 0.016(6) O1 0.098(3) 0.064(2) 0.076(3) -0.002(2) 0.013(3) -0.018(2) O2 0.081(3) 0.063(2) 0.071(3) -0.006(2) 0.015(2) -0.018(2) O3 0.085(3) 0.083(3) 0.110(4) -0.006(3) 0.042(3) 0.016(2) O4 0.083(3) 0.086(3) 0.101(4) -0.009(3) 0.043(3) -0.020(2) O5 0.080(3) 0.064(3) 0.096(3) 0.006(2) 0.027(3) 0.008(2) O6 0.073(3) 0.072(3) 0.098(3) 0.001(2) 0.039(3) 0.005(2) O7 0.080(3) 0.040(2) 0.078(3) -0.0034(17) 0.015(2) -0.0150(16) F13 0.168(18) 0.064(7) 0.23(2) 0.020(10) -0.022(15) 0.000(9) F14 0.114(12) 0.159(18) 0.19(3) 0.057(15) -0.016(16) 0.054(12) F15 0.24(4) 0.139(19) 0.18(3) 0.08(2) 0.12(3) 0.09(2) F16 0.20(3) 0.167(14) 0.21(3) -0.048(15) 0.15(3) 0.021(15) F16' 0.18(2) 0.115(17) 0.078(9) -0.016(10) -0.030(15) 0.057(18) F17 0.134(14) 0.26(3) 0.15(2) 0.07(2) 0.105(17) 0.051(19) F17' 0.15(2) 0.22(4) 0.13(2) 0.061(19) -0.002(16) -0.09(3) F18 0.14(3) 0.31(5) 0.20(2) -0.10(3) 0.09(2) -0.13(3) F18' 0.21(2) 0.079(9) 0.054(10) -0.007(7) 0.027(11) 0.024(12) N1 0.097(4) 0.052(3) 0.083(4) -0.006(3) 0.005(3) -0.013(3) N2 0.253(12) 0.071(5) 0.159(8) 0.013(5) -0.017(8) -0.063(6) C1 0.141(10) 0.098(7) 0.092(8) 0.001(6) 0.017(8) -0.030(8) C2 0.090(5) 0.081(5) 0.062(5) 0.002(4) 0.024(4) -0.004(4) C3 0.092(5) 0.082(5) 0.068(5) -0.014(3) 0.017(4) -0.019(4) C4 0.068(4) 0.063(4) 0.076(5) -0.012(3) 0.024(4) -0.007(3) C5 0.111(6) 0.080(5) 0.080(6) -0.004(4) 0.012(5) -0.033(4) C6 0.117(9) 0.131(10) 0.273(17) -0.034(11) 0.097(10) 0.039(7) C7 0.075(5) 0.115(6) 0.107(7) -0.021(5) 0.028(5) 0.020(4) C8 0.102(6) 0.145(8) 0.122(8) -0.018(6) 0.065(5) 0.009(6) C9 0.077(5) 0.131(7) 0.092(6) -0.009(5) 0.033(4) -0.019(5) C10 0.145(11) 0.147(11) 0.271(18) 0.017(11) 0.154(12) -0.010(8) C11 0.127(10) 0.119(10) 0.129(11) 0.030(8) 0.053(10) 0.036(8) C12 0.095(5) 0.063(4) 0.081(5) -0.004(3) 0.012(4) 0.008(4) C13 0.077(5) 0.099(5) 0.102(6) 0.008(4) 0.026(4) 0.026(4) C14 0.064(4) 0.093(5) 0.091(5) -0.015(4) 0.033(4) -0.004(4) C15 0.088(7) 0.127(9) 0.133(10) 0.015(8) 0.052(8) 0.016(7) C16 0.128(6) 0.055(4) 0.126(7) -0.017(4) -0.002(5) -0.001(4) C17 0.202(11) 0.049(5) 0.152(9) -0.005(5) -0.025(8) -0.013(5) C18 0.203(11) 0.100(7) 0.112(7) 0.014(6) 0.009(7) -0.074(7) C19 0.127(6) 0.093(5) 0.084(5) 0.002(4) 0.022(5) -0.047(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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_3 O1 Dy1 O3 87.04(16) . O1 Dy1 O4 77.58(15) . O3 Dy1 O4 71.85(15) . O1 Dy1 O6 105.42(16) . O3 Dy1 O6 139.51(15) . O4 Dy1 O6 147.92(15) . O1 Dy1 O5 74.49(14) . O3 Dy1 O5 147.30(16) . O4 Dy1 O5 77.87(15) . O6 Dy1 O5 72.49(14) . O1 Dy1 O2 73.11(14) . O3 Dy1 O2 73.98(14) . O4 Dy1 O2 135.57(15) . O6 Dy1 O2 73.31(13) . O5 Dy1 O2 123.54(14) . O1 Dy1 O7 146.27(13) . O3 Dy1 O7 105.22(13) . O4 Dy1 O7 76.78(14) . O6 Dy1 O7 85.67(13) . O5 Dy1 O7 79.00(13) . O2 Dy1 O7 140.22(13) . O1 Dy1 O7 150.11(12) 7 O3 Dy1 O7 74.99(15) 7 O4 Dy1 O7 117.51(13) 7 O6 Dy1 O7 75.92(14) 7 O5 Dy1 O7 131.81(14) 7 O2 Dy1 O7 78.99(12) 7 O7 Dy1 O7 63.07(13) 7 C2 O1 Dy1 136.1(4) . C4 O2 Dy1 133.6(4) . C7 O3 Dy1 133.5(5) . C9 O4 Dy1 133.1(5) . C12 O5 Dy1 134.4(4) . C14 O6 Dy1 134.8(4) . N1 O7 Dy1 122.5(3) . N1 O7 Dy1 120.5(3) 7 Dy1 O7 Dy1 116.93(13) 7 C16 N1 C19 122.0(6) . C16 N1 O7 119.8(6) . C19 N1 O7 118.2(6) . C17 N2 C18 115.1(9) . F1 C1 F3 112(2) . F17' C1 F16' 105(4) . F17' C1 F18' 104(3) . F16' C1 F18' 102.2(18) . F1 C1 F2 104(3) . F3 C1 F2 113(2) . F17' C1 C2 116(2) . F1 C1 C2 108.4(18) . F3 C1 C2 114.6(13) . F16' C1 C2 113.0(16) . F18' C1 C2 115.1(13) . F2 C1 C2 104.8(17) . O1 C2 C3 127.8(6) . O1 C2 C1 114.2(6) . C3 C2 C1 117.9(7) . C2 C3 C4 120.4(6) . C2 C3 H3 119.8 . C4 C3 H3 119.8 . O2 C4 C3 128.4(6) . O2 C4 C5 113.3(6) . C3 C4 C5 118.2(6) . F4 C5 F5 108.1(7) . F4 C5 F6 105.4(7) . F5 C5 F6 106.5(7) . F4 C5 C4 111.5(6) . F5 C5 C4 114.2(6) . F6 C5 C4 110.7(6) . F7 C6 F8 103.1(15) . F7 C6 F9 108.2(13) . F8 C6 F9 104.6(10) . F7 C6 C7 116.1(9) . F8 C6 C7 110.1(12) . F9 C6 C7 113.5(13) . O3 C7 C8 127.7(8) . O3 C7 C6 112.8(9) . C8 C7 C6 119.5(9) . C7 C8 C9 120.0(8) . C7 C8 H8 120.0 . C9 C8 H8 120.0 . O4 C9 C8 127.8(8) . O4 C9 C10 114.9(9) . C8 C9 C10 117.3(9) . F10 C10 F12 116.7(18) . F10 C10 F11 103.1(11) . F12 C10 F11 96.0(14) . F10 C10 C9 116.8(13) . F12 C10 C9 115.7(9) . F11 C10 C9 104.0(14) . F15 C11 F14 110(3) . F15 C11 F13 108(3) . F14 C11 F13 103(2) . F0AA C11 F5AA 114(3) . F0AA C11 F4AA 110(3) . F5AA C11 F4AA 94(3) . F15 C11 C12 115.7(15) . F0AA C11 C12 118(2) . F14 C11 C12 114.7(19) . F13 C11 C12 104.7(13) . F5AA C11 C12 110.0(14) . F4AA C11 C12 108.5(17) . O5 C12 C13 127.7(6) . O5 C12 C11 115.7(9) . C13 C12 C11 116.6(9) . C12 C13 C14 120.4(6) . C12 C13 H13 119.8 . C14 C13 H13 119.8 . O6 C14 C13 127.4(7) . O6 C14 C15 113.9(7) . C13 C14 C15 118.7(7) . F3AA C15 F1AA 109(2) . F17 C15 F18 114(3) . F3AA C15 F2AA 102(2) . F1AA C15 F2AA 105(2) . F17 C15 F16 106(2) . F18 C15 F16 105(2) . F3AA C15 C14 116.3(14) . F17 C15 C14 110.4(14) . F1AA C15 C14 115.7(15) . F18 C15 C14 108.6(16) . F2AA C15 C14 107.0(15) . F16 C15 C14 112.7(15) . N1 C16 C17 117.9(8) . N1 C16 H16 121.1 . C17 C16 H16 121.1 . N2 C17 C16 124.4(10) . N2 C17 H17 117.8 . C16 C17 H17 117.8 . N2 C18 C19 124.4(11) . N2 C18 H18 117.8 . C19 C18 H18 117.8 . N1 C19 C18 116.3(8) . N1 C19 H19 121.9 . C18 C19 H19 121.9 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy1 O1 2.280(4) . Dy1 O3 2.307(4) . Dy1 O4 2.309(4) . Dy1 O6 2.311(4) . Dy1 O5 2.318(4) . Dy1 O2 2.329(3) . Dy1 O7 2.405(3) . Dy1 O7 2.417(3) 7 F1 C1 1.24(3) . F1AA C15 1.28(3) . F2 C1 1.38(3) . F2AA C15 1.35(3) . F3 C1 1.25(2) . F3AA C15 1.22(2) . F4 C5 1.293(8) . F4AA C11 1.39(4) . F5 C5 1.309(7) . F5AA C11 1.38(3) . F6 C5 1.312(8) . F0AA C11 1.17(3) . F7 C6 1.233(11) . F8 C6 1.267(16) . F9 C6 1.284(14) . F10 C10 1.177(15) . F11 C10 1.358(18) . F12 C10 1.217(12) . O1 C2 1.247(7) . O2 C4 1.245(6) . O3 C7 1.241(8) . O4 C9 1.239(8) . O5 C12 1.230(7) . O6 C14 1.231(7) . O7 N1 1.331(5) . O7 Dy1 2.418(3) 7 F13 C11 1.38(2) . F14 C11 1.27(3) . F15 C11 1.11(3) . F16 C15 1.35(2) . F16' C1 1.35(3) . F17 C15 1.27(3) . F17' C1 1.21(4) . F18 C15 1.29(3) . F18' C1 1.35(3) . N1 C16 1.316(8) . N1 C19 1.325(8) . N2 C17 1.311(13) . N2 C18 1.316(13) . C1 C2 1.546(10) . C2 C3 1.365(8) . C3 C4 1.384(8) . C3 H3 0.9300 . C4 C5 1.504(8) . C6 C7 1.497(12) . C7 C8 1.367(10) . C8 C9 1.368(10) . C8 H8 0.9300 . C9 C10 1.520(13) . C11 C12 1.523(11) . C12 C13 1.378(9) . C13 C14 1.391(9) . C13 H13 0.9300 . C14 C15 1.512(10) . C16 C17 1.359(10) . C16 H16 0.9300 . C17 H17 0.9300 . C18 C19 1.387(10) . C18 H18 0.9300 . C19 H19 0.9300 . 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 Dy1 O7 N1 C16 -87.6(6) . Dy1 O7 N1 C16 91.1(6) 7 Dy1 O7 N1 C19 91.9(5) . Dy1 O7 N1 C19 -89.4(6) 7 Dy1 O1 C2 C3 -6.9(11) . Dy1 O1 C2 C1 177.7(7) . F17' C1 C2 O1 -46(4) . F1 C1 C2 O1 46(2) . F3 C1 C2 O1 171.9(16) . F16' C1 C2 O1 75.3(19) . F18' C1 C2 O1 -167.8(17) . F2 C1 C2 O1 -64(2) . F17' C1 C2 C3 138(3) . F1 C1 C2 C3 -129.4(19) . F3 C1 C2 C3 -4(2) . F16' C1 C2 C3 -100.6(18) . F18' C1 C2 C3 16(2) . F2 C1 C2 C3 119.9(19) . O1 C2 C3 C4 0.7(11) . C1 C2 C3 C4 176.0(8) . Dy1 O2 C4 C3 7.3(10) . Dy1 O2 C4 C5 -174.2(5) . C2 C3 C4 O2 -1.2(11) . C2 C3 C4 C5 -179.6(6) . O2 C4 C5 F4 64.6(9) . C3 C4 C5 F4 -116.8(7) . O2 C4 C5 F5 -172.5(6) . C3 C4 C5 F5 6.2(11) . O2 C4 C5 F6 -52.4(8) . C3 C4 C5 F6 126.2(7) . Dy1 O3 C7 C8 -14.2(12) . Dy1 O3 C7 C6 168.6(7) . F7 C6 C7 O3 -40.3(18) . F8 C6 C7 O3 76.4(13) . F9 C6 C7 O3 -166.7(12) . F7 C6 C7 C8 142.2(13) . F8 C6 C7 C8 -101.1(14) . F9 C6 C7 C8 15.8(18) . O3 C7 C8 C9 -7.8(13) . C6 C7 C8 C9 169.3(10) . Dy1 O4 C9 C8 17.3(12) . Dy1 O4 C9 C10 -162.2(9) . C7 C8 C9 O4 6.2(13) . C7 C8 C9 C10 -174.3(10) . O4 C9 C10 F10 163.3(16) . C8 C9 C10 F10 -16(2) . O4 C9 C10 F12 20(2) . C8 C9 C10 F12 -159.7(14) . O4 C9 C10 F11 -83.9(11) . C8 C9 C10 F11 96.4(13) . Dy1 O5 C12 C13 -12.8(11) . Dy1 O5 C12 C11 167.5(8) . F15 C11 C12 O5 -29(4) . F0AA C11 C12 O5 166(4) . F14 C11 C12 O5 -158(2) . F13 C11 C12 O5 90(2) . F5AA C11 C12 O5 34(3) . F4AA C11 C12 O5 -69(3) . F15 C11 C12 C13 152(3) . F0AA C11 C12 C13 -14(4) . F14 C11 C12 C13 22(3) . F13 C11 C12 C13 -90(2) . F5AA C11 C12 C13 -146(3) . F4AA C11 C12 C13 112(3) . O5 C12 C13 C14 -3.2(12) . C11 C12 C13 C14 176.5(9) . Dy1 O6 C14 C13 9.9(11) . Dy1 O6 C14 C15 -170.1(7) . C12 C13 C14 O6 4.7(12) . C12 C13 C14 C15 -175.3(9) . O6 C14 C15 F3AA 162(3) . C13 C14 C15 F3AA -18(3) . O6 C14 C15 F17 -29(3) . C13 C14 C15 F17 151(2) . O6 C14 C15 F1AA -68(3) . C13 C14 C15 F1AA 112(2) . O6 C14 C15 F18 96(3) . C13 C14 C15 F18 -84(3) . O6 C14 C15 F2AA 49(2) . C13 C14 C15 F2AA -131.0(19) . O6 C14 C15 F16 -148(2) . C13 C14 C15 F16 32(3) . C19 N1 C16 C17 0.1(10) . O7 N1 C16 C17 179.6(6) . C18 N2 C17 C16 2.0(17) . N1 C16 C17 N2 -2.1(14) . C17 N2 C18 C19 -0.2(16) . C16 N1 C19 C18 1.5(10) . O7 N1 C19 C18 -178.0(6) . N2 C18 C19 N1 -1.6(13) .