#------------------------------------------------------------------------------ #$Date: 2019-11-08 00:02:33 +0200 (Fri, 08 Nov 2019) $ #$Revision: 224170 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/96/7049650.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_7049650 loop_ _publ_author_name 'Chen, Zilu' 'Yu, Shui' 'Wang, Rongdong' 'Li, Bo' 'Yin, Bing' 'Liu, Dongcheng' 'Liang, Yuning' 'Yao, Di' 'Liang, Fupei' _publ_section_title ; Three Dy(iii) single-ion magnets bearing the tropolone ligand: structure, magnetic properties and theoretical elucidation. ; _journal_issue 19 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 6627 _journal_page_last 6637 _journal_paper_doi 10.1039/c9dt00364a _journal_volume 48 _journal_year 2019 _chemical_formula_moiety 'C33 H23 Dy N2 O6, H2 O' _chemical_formula_sum 'C33 H25 Dy N2 O7' _chemical_formula_weight 724.05 _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 mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-03-02 deposited with the CCDC. 2019-04-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.405(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.044(4) _cell_length_b 23.437(10) _cell_length_c 11.989(5) _cell_measurement_reflns_used 5753 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 24.96 _cell_measurement_theta_min 2.37 _cell_volume 2733(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_unetI/netI 0.0669 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 16606 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 25.182 _diffrn_reflns_theta_max 25.182 _diffrn_reflns_theta_min 1.738 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 2.789 _exptl_absorpt_correction_T_max 0.557 _exptl_absorpt_correction_T_min 0.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.759 _exptl_crystal_description block _exptl_crystal_F_000 1436 _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.210 _refine_diff_density_max 1.317 _refine_diff_density_min -1.504 _refine_diff_density_rms 0.225 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 388 _refine_ls_number_reflns 4836 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0364 _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^)+(0.0460P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.0913 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3828 _reflns_number_total 4836 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00364a2.cif _cod_data_source_block A_b _cod_depositor_comments 'Adding full bibliography for 7049649--7049651.cif.' _cod_database_code 7049650 _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 0.509 _shelx_estimated_absorpt_t_max 0.592 _shelx_res_file ; A_b.res created by SHELXL-2014/7 TITL A_b.res in Pn New: P21/n CELL 0.71073 10.0440 23.4370 11.9890 90.000 104.405 90.000 ZERR 4 0.0040 0.0100 0.0050 0.000 0.005 0.000 LATT 1 SYMM 0.50000 - X , 0.50000 + Y , 0.50000 - Z SFAC C H Dy N O UNIT 132 100 4 8 28 L.S. 8 ACTA BOND $H FMAP 2 PLAN 20 CONF size 0.28 0.23 0.21 TEMP 23 HTAB EQIV $1 x-1/2, -y+1/2, z-1/2 HTAB C2 O6_$1 HTAB C10 O4 EQIV $2 -x, -y+1, -z+1 HTAB C15 O7_$2 HTAB O7 O5 EQIV $3 -x+1, -y+1, -z+1 HTAB O7 O7_$3 WGHT 0.046000 FVAR 0.19654 DY1 3 0.059949 0.371639 0.358863 11.00000 0.02742 0.01956 = 0.02989 0.00265 0.01390 0.00029 N1 4 -0.086338 0.369707 0.151311 11.00000 0.02948 0.02367 = 0.03883 0.00201 0.01605 0.00066 N2 4 -0.003472 0.469263 0.260698 11.00000 0.03235 0.02095 = 0.03419 0.00142 0.01430 0.00134 C1 1 -0.128472 0.320492 0.098066 11.00000 0.03587 0.02766 = 0.04624 -0.00181 0.01881 0.00363 AFIX 43 H1 2 -0.102171 0.286626 0.137881 11.00000 -1.20000 AFIX 0 C2 1 -0.210563 0.317427 -0.015126 11.00000 0.02957 0.04379 = 0.04702 -0.01533 0.01207 -0.00382 AFIX 43 H2 2 -0.239408 0.282371 -0.048941 11.00000 -1.20000 AFIX 0 C3 1 -0.247175 0.367106 -0.074558 11.00000 0.01948 0.06297 = 0.03599 -0.00685 0.00650 -0.00102 AFIX 43 H3 2 -0.302012 0.366006 -0.149491 11.00000 -1.20000 AFIX 0 C4 1 -0.202649 0.419444 -0.023310 11.00000 0.02174 0.04400 = 0.03580 0.00129 0.01248 0.00260 C5 1 -0.235952 0.472122 -0.081832 11.00000 0.03503 0.05312 = 0.03673 0.00984 0.00402 0.00751 AFIX 43 H5 2 -0.288660 0.472517 -0.157528 11.00000 -1.20000 AFIX 0 C6 1 -0.191684 0.521370 -0.028367 11.00000 0.03764 0.04975 = 0.05274 0.02995 0.01957 0.01690 AFIX 43 H6 2 -0.213638 0.555400 -0.068644 11.00000 -1.20000 AFIX 0 C7 1 -0.111905 0.523408 0.088395 11.00000 0.02874 0.02861 = 0.04607 0.01183 0.02173 0.00981 C8 1 -0.065807 0.573747 0.149572 11.00000 0.03854 0.02635 = 0.06356 0.01472 0.02549 0.00728 AFIX 43 H8 2 -0.085767 0.608933 0.113419 11.00000 -1.20000 AFIX 0 C9 1 0.006354 0.571428 0.259093 11.00000 0.04858 0.02152 = 0.05771 -0.00118 0.02451 -0.00418 AFIX 43 H9 2 0.037566 0.604752 0.299244 11.00000 -1.20000 AFIX 0 C10 1 0.034326 0.518650 0.312457 11.00000 0.03571 0.02698 = 0.03739 0.00258 0.00959 -0.00020 AFIX 43 H10 2 0.082680 0.517968 0.389438 11.00000 -1.20000 AFIX 0 C11 1 -0.077585 0.471692 0.149443 11.00000 0.02387 0.02828 = 0.03547 0.00472 0.01994 0.00428 C12 1 -0.123242 0.418731 0.090906 11.00000 0.02104 0.02757 = 0.03792 0.00633 0.01754 0.00275 O1 5 -0.105289 0.301648 0.361719 11.00000 0.03940 0.02335 = 0.04195 -0.00261 0.02630 -0.00542 O2 5 -0.119460 0.403337 0.432586 11.00000 0.04431 0.02180 = 0.06401 -0.00765 0.03537 -0.00511 C13 1 -0.208237 0.311802 0.404547 11.00000 0.03112 0.02836 = 0.02356 0.00359 0.00858 0.00124 C14 1 -0.215343 0.370091 0.446657 11.00000 0.02286 0.02666 = 0.03460 0.00439 0.01484 -0.00002 C15 1 -0.313891 0.391410 0.501419 11.00000 0.03578 0.02709 = 0.05018 -0.00485 0.01896 0.00107 AFIX 43 H15 2 -0.301832 0.429538 0.523069 11.00000 -1.20000 AFIX 0 C16 1 -0.424564 0.365707 0.528369 11.00000 0.02973 0.04305 = 0.05386 -0.00111 0.02603 0.00459 AFIX 43 H16 2 -0.473168 0.388557 0.567904 11.00000 -1.20000 AFIX 0 C17 1 -0.474392 0.311018 0.505515 11.00000 0.02690 0.04602 = 0.05209 0.00421 0.01985 -0.00264 AFIX 43 H17 2 -0.553608 0.301910 0.528611 11.00000 -1.20000 AFIX 0 C18 1 -0.418359 0.268219 0.451585 11.00000 0.03139 0.04065 = 0.04426 -0.00029 0.01498 -0.00949 AFIX 43 H18 2 -0.465713 0.233754 0.442901 11.00000 -1.20000 AFIX 0 C19 1 -0.302847 0.269087 0.408850 11.00000 0.03678 0.02657 = 0.03446 -0.00464 0.01550 -0.00779 AFIX 43 H19 2 -0.284948 0.234632 0.376949 11.00000 -1.20000 AFIX 0 O3 5 0.178718 0.330645 0.533680 11.00000 0.04137 0.02429 = 0.03642 0.00192 0.00897 0.00039 O4 5 0.177211 0.437293 0.494326 11.00000 0.04614 0.02349 = 0.03398 0.00316 0.00951 -0.00319 C20 1 0.244474 0.361374 0.618249 11.00000 0.02446 0.02865 = 0.03454 0.00687 0.01692 0.00292 C21 1 0.241738 0.422966 0.595326 11.00000 0.02490 0.03065 = 0.03216 0.00401 0.01491 0.00052 C22 1 0.299737 0.465662 0.673893 11.00000 0.04126 0.03005 = 0.03724 0.00194 0.01520 -0.00678 AFIX 43 H22 2 0.284874 0.502650 0.645432 11.00000 -1.20000 AFIX 0 C23 1 0.375365 0.461918 0.786663 11.00000 0.03391 0.04626 = 0.05397 -0.01006 0.01088 -0.01699 AFIX 43 H23 2 0.403697 0.496666 0.822142 11.00000 -1.20000 AFIX 0 C24 1 0.415850 0.413919 0.855645 11.00000 0.03156 0.06140 = 0.03980 0.00163 0.00399 -0.00215 AFIX 43 H24 2 0.465586 0.420527 0.930985 11.00000 -1.20000 AFIX 0 C25 1 0.389666 0.357553 0.823564 11.00000 0.03814 0.05167 = 0.04182 0.01337 0.01024 0.00798 AFIX 43 H25 2 0.428424 0.330701 0.879316 11.00000 -1.20000 AFIX 0 C26 1 0.313460 0.335381 0.719565 11.00000 0.03955 0.03415 = 0.03811 0.00391 0.01568 0.00674 AFIX 43 H26 2 0.307954 0.295767 0.717968 11.00000 -1.20000 AFIX 0 O5 5 0.246874 0.393975 0.282531 11.00000 0.03194 0.02246 = 0.06046 0.00122 0.03318 0.00352 O6 5 0.156376 0.292710 0.287715 11.00000 0.03349 0.02269 = 0.04372 0.00116 0.02063 -0.00116 C27 1 0.312946 0.355884 0.242600 11.00000 0.02569 0.02642 = 0.02850 0.00513 0.00993 0.00550 C28 1 0.260504 0.297298 0.245514 11.00000 0.02669 0.02543 = 0.02535 0.00004 0.00059 0.00226 C29 1 0.317546 0.248707 0.207095 11.00000 0.04120 0.02379 = 0.03296 -0.00506 0.01062 0.00216 AFIX 43 H29 2 0.273928 0.214665 0.216336 11.00000 -1.20000 AFIX 0 C30 1 0.426939 0.242788 0.158099 11.00000 0.04799 0.03224 = 0.03450 -0.00734 0.00880 0.00969 AFIX 43 H30 2 0.444152 0.205402 0.139760 11.00000 -1.20000 AFIX 0 C31 1 0.515543 0.282410 0.131366 11.00000 0.03907 0.04822 = 0.03796 -0.00398 0.01616 0.01611 AFIX 43 H31 2 0.582325 0.268950 0.096412 11.00000 -1.20000 AFIX 0 C32 1 0.513883 0.339888 0.151762 11.00000 0.03365 0.05395 = 0.03922 0.01306 0.02105 0.00986 AFIX 43 H32 2 0.581487 0.360855 0.129408 11.00000 -1.20000 AFIX 0 C33 1 0.426988 0.371199 0.200432 11.00000 0.03905 0.03138 = 0.04483 0.00342 0.02153 0.00028 AFIX 43 H33 2 0.447516 0.409941 0.206690 11.00000 -1.20000 AFIX 0 O7 5 0.402525 0.493540 0.380976 11.00000 0.06918 0.05329 = 0.14603 -0.02907 0.04232 -0.01503 AFIX 3 H71 2 0.361364 0.462331 0.360185 11.00000 -1.50000 H72 2 0.481775 0.483155 0.409499 11.00000 -1.50000 AFIX 0 HKLF 4 REM A_b.res in Pn New: P21/n REM R1 = 0.0364 for 3828 Fo > 4sig(Fo) and 0.0578 for all 4836 data REM 388 parameters refined using 0 restraints END WGHT 0.0428 0.0000 REM Instructions for potential hydrogen bonds HTAB C2 O6_$1 HTAB C10 O4 HTAB C15 O7_$2 HTAB O7 O5 HTAB O7 O7_$3 REM Highest difference peak 1.317, deepest hole -1.504, 1-sigma level 0.225 Q1 1 0.2007 0.3684 0.4419 11.00000 0.05 1.32 Q2 1 -0.0830 0.3704 0.2688 11.00000 0.05 1.27 Q3 1 0.0914 0.6354 0.3470 11.00000 0.05 1.02 Q4 1 0.2946 0.3655 0.4296 11.00000 0.05 0.85 Q5 1 0.0785 0.6341 0.4008 11.00000 0.05 0.81 Q6 1 0.0846 0.3380 0.5342 11.00000 0.05 0.80 Q7 1 0.2424 0.3752 0.1297 11.00000 0.05 0.72 Q8 1 0.3966 0.3062 0.9429 11.00000 0.05 0.71 Q9 1 0.5734 0.4047 0.8759 11.00000 0.05 0.70 Q10 1 -0.2285 0.6119 -0.0323 11.00000 0.05 0.69 Q11 1 0.1044 0.4060 0.4426 11.00000 0.05 0.69 Q12 1 0.1648 0.3056 0.4781 11.00000 0.05 0.69 Q13 1 0.4362 0.4496 0.9218 11.00000 0.05 0.69 Q14 1 0.0624 0.3140 0.2148 11.00000 0.05 0.68 Q15 1 0.0155 0.3718 0.4690 11.00000 0.05 0.65 Q16 1 -0.2220 0.4490 -0.2056 11.00000 0.05 0.63 Q17 1 0.5058 0.1471 0.1051 11.00000 0.05 0.63 Q18 1 0.5862 0.4181 0.2200 11.00000 0.05 0.63 Q19 1 0.2643 0.1891 0.2727 11.00000 0.05 0.62 Q20 1 -0.2722 0.4652 -0.2574 11.00000 0.05 0.61 ; _shelx_res_checksum 63641 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 0.05995(2) 0.37164(2) 0.35886(2) 0.02442(10) Uani 1 1 d . . N1 N -0.0863(4) 0.36971(16) 0.1513(4) 0.0293(10) Uani 1 1 d . . N2 N -0.0035(4) 0.46926(17) 0.2607(4) 0.0281(10) Uani 1 1 d . . C1 C -0.1285(6) 0.3205(2) 0.0981(5) 0.0351(13) Uani 1 1 d . . H1 H -0.1022 0.2866 0.1379 0.042 Uiso 1 1 calc R U C2 C -0.2106(6) 0.3174(3) -0.0151(5) 0.0397(14) Uani 1 1 d . . H2 H -0.2394 0.2824 -0.0489 0.048 Uiso 1 1 calc R U C3 C -0.2472(6) 0.3671(3) -0.0746(5) 0.0396(15) Uani 1 1 d . . H3 H -0.3020 0.3660 -0.1495 0.047 Uiso 1 1 calc R U C4 C -0.2026(5) 0.4194(2) -0.0233(5) 0.0329(13) Uani 1 1 d . . C5 C -0.2360(6) 0.4721(3) -0.0818(5) 0.0425(15) Uani 1 1 d . . H5 H -0.2887 0.4725 -0.1575 0.051 Uiso 1 1 calc R U C6 C -0.1917(6) 0.5214(3) -0.0284(5) 0.0452(16) Uani 1 1 d . . H6 H -0.2136 0.5554 -0.0686 0.054 Uiso 1 1 calc R U C7 C -0.1119(5) 0.5234(2) 0.0884(5) 0.0323(13) Uani 1 1 d . . C8 C -0.0658(6) 0.5737(2) 0.1496(5) 0.0406(15) Uani 1 1 d . . H8 H -0.0858 0.6089 0.1134 0.049 Uiso 1 1 calc R U C9 C 0.0064(6) 0.5714(2) 0.2591(5) 0.0406(15) Uani 1 1 d . . H9 H 0.0376 0.6048 0.2992 0.049 Uiso 1 1 calc R U C10 C 0.0343(6) 0.5186(2) 0.3125(5) 0.0333(13) Uani 1 1 d . . H10 H 0.0827 0.5180 0.3894 0.040 Uiso 1 1 calc R U C11 C -0.0776(5) 0.4717(2) 0.1494(4) 0.0270(12) Uani 1 1 d . . C12 C -0.1232(5) 0.4187(2) 0.0909(5) 0.0270(12) Uani 1 1 d . . O1 O -0.1053(4) 0.30165(14) 0.3617(3) 0.0320(9) Uani 1 1 d . . O2 O -0.1195(4) 0.40334(14) 0.4326(3) 0.0395(10) Uani 1 1 d . . C13 C -0.2082(5) 0.3118(2) 0.4045(4) 0.0274(12) Uani 1 1 d . . C14 C -0.2153(5) 0.3701(2) 0.4467(4) 0.0267(11) Uani 1 1 d . . C15 C -0.3139(6) 0.3914(2) 0.5014(5) 0.0362(13) Uani 1 1 d . . H15 H -0.3018 0.4295 0.5231 0.043 Uiso 1 1 calc R U C16 C -0.4246(6) 0.3657(2) 0.5284(5) 0.0395(14) Uani 1 1 d . . H16 H -0.4732 0.3886 0.5679 0.047 Uiso 1 1 calc R U C17 C -0.4744(6) 0.3110(2) 0.5055(5) 0.0399(14) Uani 1 1 d . . H17 H -0.5536 0.3019 0.5286 0.048 Uiso 1 1 calc R U C18 C -0.4184(6) 0.2682(2) 0.4516(5) 0.0378(14) Uani 1 1 d . . H18 H -0.4657 0.2338 0.4429 0.045 Uiso 1 1 calc R U C19 C -0.3028(5) 0.2691(2) 0.4089(4) 0.0314(13) Uani 1 1 d . . H19 H -0.2849 0.2346 0.3769 0.038 Uiso 1 1 calc R U O3 O 0.1787(4) 0.33064(14) 0.5337(3) 0.0341(9) Uani 1 1 d . . O4 O 0.1772(4) 0.43729(14) 0.4943(3) 0.0346(9) Uani 1 1 d . . C20 C 0.2445(5) 0.3614(2) 0.6182(5) 0.0275(12) Uani 1 1 d . . C21 C 0.2417(5) 0.4230(2) 0.5953(4) 0.0279(12) Uani 1 1 d . . C22 C 0.2997(6) 0.4657(2) 0.6739(5) 0.0352(13) Uani 1 1 d . . H22 H 0.2849 0.5027 0.6454 0.042 Uiso 1 1 calc R U C23 C 0.3754(6) 0.4619(3) 0.7867(5) 0.0447(15) Uani 1 1 d . . H23 H 0.4037 0.4967 0.8221 0.054 Uiso 1 1 calc R U C24 C 0.4158(6) 0.4139(3) 0.8556(5) 0.0451(16) Uani 1 1 d . . H24 H 0.4656 0.4205 0.9310 0.054 Uiso 1 1 calc R U C25 C 0.3897(6) 0.3576(3) 0.8236(5) 0.0438(15) Uani 1 1 d . . H25 H 0.4284 0.3307 0.8793 0.053 Uiso 1 1 calc R U C26 C 0.3135(6) 0.3354(2) 0.7196(5) 0.0362(13) Uani 1 1 d . . H26 H 0.3080 0.2958 0.7180 0.043 Uiso 1 1 calc R U O5 O 0.2469(4) 0.39397(15) 0.2825(3) 0.0345(9) Uani 1 1 d . . O6 O 0.1564(4) 0.29271(14) 0.2877(3) 0.0314(8) Uani 1 1 d . . C27 C 0.3129(5) 0.3559(2) 0.2426(4) 0.0263(12) Uani 1 1 d . . C28 C 0.2605(5) 0.2973(2) 0.2455(4) 0.0269(12) Uani 1 1 d . . C29 C 0.3175(6) 0.2487(2) 0.2071(4) 0.0324(13) Uani 1 1 d . . H29 H 0.2739 0.2147 0.2163 0.039 Uiso 1 1 calc R U C30 C 0.4269(6) 0.2428(2) 0.1581(5) 0.0385(15) Uani 1 1 d . . H30 H 0.4442 0.2054 0.1398 0.046 Uiso 1 1 calc R U C31 C 0.5155(6) 0.2824(3) 0.1314(5) 0.0406(15) Uani 1 1 d . . H31 H 0.5823 0.2690 0.0964 0.049 Uiso 1 1 calc R U C32 C 0.5139(6) 0.3399(3) 0.1518(5) 0.0402(15) Uani 1 1 d . . H32 H 0.5815 0.3609 0.1294 0.048 Uiso 1 1 calc R U C33 C 0.4270(6) 0.3712(2) 0.2004(5) 0.0365(13) Uani 1 1 d . . H33 H 0.4475 0.4099 0.2067 0.044 Uiso 1 1 calc R U O7 O 0.4025(5) 0.4935(2) 0.3810(5) 0.0868(18) Uani 1 1 d . . H71 H 0.3614 0.4623 0.3602 0.130 Uiso 1 1 d R U H72 H 0.4818 0.4832 0.4095 0.130 Uiso 1 1 d 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 0.02742(16) 0.01956(14) 0.02989(15) 0.00265(11) 0.01390(10) 0.00029(11) N1 0.029(2) 0.024(2) 0.039(3) 0.002(2) 0.016(2) 0.0007(19) N2 0.032(3) 0.021(2) 0.034(3) 0.0014(18) 0.014(2) 0.0013(19) C1 0.036(3) 0.028(3) 0.046(3) -0.002(2) 0.019(3) 0.004(3) C2 0.030(3) 0.044(3) 0.047(4) -0.015(3) 0.012(3) -0.004(3) C3 0.019(3) 0.063(4) 0.036(3) -0.007(3) 0.006(2) -0.001(3) C4 0.022(3) 0.044(3) 0.036(3) 0.001(3) 0.012(2) 0.003(3) C5 0.035(3) 0.053(4) 0.037(3) 0.010(3) 0.004(3) 0.008(3) C6 0.038(3) 0.050(4) 0.053(4) 0.030(3) 0.020(3) 0.017(3) C7 0.029(3) 0.029(3) 0.046(3) 0.012(2) 0.022(3) 0.010(2) C8 0.039(3) 0.026(3) 0.064(4) 0.015(3) 0.025(3) 0.007(3) C9 0.049(4) 0.022(3) 0.058(4) -0.001(3) 0.025(3) -0.004(3) C10 0.036(3) 0.027(3) 0.037(3) 0.003(2) 0.010(2) 0.000(2) C11 0.024(3) 0.028(3) 0.035(3) 0.005(2) 0.020(2) 0.004(2) C12 0.021(3) 0.028(3) 0.038(3) 0.006(2) 0.018(2) 0.003(2) O1 0.039(2) 0.0233(18) 0.042(2) -0.0026(16) 0.0263(18) -0.0054(17) O2 0.044(2) 0.0218(19) 0.064(3) -0.0076(18) 0.035(2) -0.0051(18) C13 0.031(3) 0.028(3) 0.024(3) 0.004(2) 0.009(2) 0.001(2) C14 0.023(3) 0.027(3) 0.035(3) 0.004(2) 0.015(2) 0.000(2) C15 0.036(3) 0.027(3) 0.050(4) -0.005(3) 0.019(3) 0.001(3) C16 0.030(3) 0.043(3) 0.054(4) -0.001(3) 0.026(3) 0.005(3) C17 0.027(3) 0.046(3) 0.052(4) 0.004(3) 0.020(3) -0.003(3) C18 0.031(3) 0.041(3) 0.044(3) 0.000(3) 0.015(3) -0.009(3) C19 0.037(3) 0.027(3) 0.034(3) -0.005(2) 0.016(2) -0.008(2) O3 0.041(2) 0.0243(18) 0.036(2) 0.0019(16) 0.0090(18) 0.0004(17) O4 0.046(2) 0.0235(18) 0.034(2) 0.0032(16) 0.0095(18) -0.0032(17) C20 0.024(3) 0.029(3) 0.035(3) 0.007(2) 0.017(2) 0.003(2) C21 0.025(3) 0.031(3) 0.032(3) 0.004(2) 0.015(2) 0.001(2) C22 0.041(3) 0.030(3) 0.037(3) 0.002(2) 0.015(3) -0.007(3) C23 0.034(3) 0.046(4) 0.054(4) -0.010(3) 0.011(3) -0.017(3) C24 0.032(3) 0.061(4) 0.040(3) 0.002(3) 0.004(3) -0.002(3) C25 0.038(4) 0.052(4) 0.042(4) 0.013(3) 0.010(3) 0.008(3) C26 0.040(3) 0.034(3) 0.038(3) 0.004(3) 0.016(3) 0.007(3) O5 0.032(2) 0.0225(17) 0.060(2) 0.0012(17) 0.0332(18) 0.0035(17) O6 0.033(2) 0.0227(18) 0.044(2) 0.0012(16) 0.0206(18) -0.0012(16) C27 0.026(3) 0.026(3) 0.028(3) 0.005(2) 0.010(2) 0.006(2) C28 0.027(3) 0.025(3) 0.025(3) 0.000(2) 0.001(2) 0.002(2) C29 0.041(3) 0.024(3) 0.033(3) -0.005(2) 0.011(3) 0.002(2) C30 0.048(4) 0.032(3) 0.034(3) -0.007(2) 0.009(3) 0.010(3) C31 0.039(4) 0.048(4) 0.038(3) -0.004(3) 0.016(3) 0.016(3) C32 0.034(3) 0.054(4) 0.039(3) 0.013(3) 0.021(3) 0.010(3) C33 0.039(3) 0.031(3) 0.045(3) 0.003(3) 0.022(3) 0.000(3) O7 0.069(4) 0.053(3) 0.146(5) -0.029(3) 0.042(4) -0.015(3) 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' 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 O2 Dy1 O4 80.15(13) O2 Dy1 O1 66.27(12) O4 Dy1 O1 133.59(13) O2 Dy1 O5 148.40(12) O4 Dy1 O5 79.03(13) O1 Dy1 O5 143.36(12) O2 Dy1 O3 93.52(14) O4 Dy1 O3 65.88(12) O1 Dy1 O3 84.53(13) O5 Dy1 O3 99.31(13) O2 Dy1 O6 145.30(12) O4 Dy1 O6 126.23(13) O1 Dy1 O6 79.10(13) O5 Dy1 O6 65.83(12) O3 Dy1 O6 80.65(13) O2 Dy1 N1 93.66(14) O4 Dy1 N1 139.28(12) O1 Dy1 N1 76.34(13) O5 Dy1 N1 86.91(14) O3 Dy1 N1 154.76(12) O6 Dy1 N1 79.71(13) O2 Dy1 N2 76.26(13) O4 Dy1 N2 75.94(12) O1 Dy1 N2 122.21(13) O5 Dy1 N2 75.79(13) O3 Dy1 N2 141.68(13) O6 Dy1 N2 127.68(13) N1 Dy1 N2 63.55(12) C1 N1 C12 117.6(5) C1 N1 Dy1 121.2(3) C12 N1 Dy1 121.2(3) C10 N2 C11 116.6(4) C10 N2 Dy1 123.5(3) C11 N2 Dy1 119.9(3) N1 C1 C2 123.1(5) N1 C1 H1 118.4 C2 C1 H1 118.4 C3 C2 C1 118.5(5) C3 C2 H2 120.7 C1 C2 H2 120.7 C2 C3 C4 120.3(5) C2 C3 H3 119.9 C4 C3 H3 119.9 C3 C4 C12 117.5(5) C3 C4 C5 122.5(5) C12 C4 C5 120.0(5) C6 C5 C4 120.2(5) C6 C5 H5 119.9 C4 C5 H5 119.9 C5 C6 C7 122.3(5) C5 C6 H6 118.8 C7 C6 H6 118.8 C8 C7 C11 116.3(5) C8 C7 C6 124.8(5) C11 C7 C6 118.9(5) C9 C8 C7 120.5(5) C9 C8 H8 119.8 C7 C8 H8 119.8 C8 C9 C10 119.2(5) C8 C9 H9 120.4 C10 C9 H9 120.4 N2 C10 C9 124.1(5) N2 C10 H10 117.9 C9 C10 H10 117.9 N2 C11 C7 123.2(5) N2 C11 C12 118.2(4) C7 C11 C12 118.6(5) N1 C12 C4 122.9(5) N1 C12 C11 117.1(4) C4 C12 C11 119.9(5) C13 O1 Dy1 121.3(3) C14 O2 Dy1 122.4(3) O1 C13 C19 120.4(5) O1 C13 C14 115.0(4) C19 C13 C14 124.5(5) O2 C14 C15 118.9(5) O2 C14 C13 114.8(5) C15 C14 C13 126.3(5) C16 C15 C14 131.2(5) C16 C15 H15 114.4 C14 C15 H15 114.4 C15 C16 C17 129.6(6) C15 C16 H16 115.2 C17 C16 H16 115.2 C16 C17 C18 126.6(6) C16 C17 H17 116.7 C18 C17 H17 116.7 C19 C18 C17 129.7(5) C19 C18 H18 115.2 C17 C18 H18 115.2 C18 C19 C13 132.1(5) C18 C19 H19 114.0 C13 C19 H19 114.0 C20 O3 Dy1 121.6(3) C21 O4 Dy1 122.7(3) O3 C20 C26 119.6(5) O3 C20 C21 114.9(4) C26 C20 C21 125.5(5) O4 C21 C22 118.8(5) O4 C21 C20 114.9(4) C22 C21 C20 126.3(5) C23 C22 C21 130.6(5) C23 C22 H22 114.7 C21 C22 H22 114.7 C22 C23 C24 129.8(6) C22 C23 H23 115.1 C24 C23 H23 115.1 C25 C24 C23 126.7(6) C25 C24 H24 116.6 C23 C24 H24 116.6 C24 C25 C26 129.1(5) C24 C25 H25 115.5 C26 C25 H25 115.5 C20 C26 C25 131.8(5) C20 C26 H26 114.1 C25 C26 H26 114.1 C27 O5 Dy1 122.2(3) C28 O6 Dy1 122.1(3) O5 C27 C33 120.1(5) O5 C27 C28 114.9(5) C33 C27 C28 125.0(5) O6 C28 C29 120.3(5) O6 C28 C27 114.9(5) C29 C28 C27 124.8(5) C30 C29 C28 131.1(5) C30 C29 H29 114.5 C28 C29 H29 114.5 C29 C30 C31 131.4(5) C29 C30 H30 114.3 C31 C30 H30 114.3 C32 C31 C30 125.7(6) C32 C31 H31 117.1 C30 C31 H31 117.1 C31 C32 C33 129.6(6) C31 C32 H32 115.2 C33 C32 H32 115.2 C32 C33 C27 132.4(5) C32 C33 H33 113.8 C27 C33 H33 113.8 H71 O7 H72 102.6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Dy1 O2 2.318(4) Dy1 O4 2.333(3) Dy1 O1 2.340(3) Dy1 O5 2.343(4) Dy1 O3 2.344(4) Dy1 O6 2.345(3) Dy1 N1 2.556(4) Dy1 N2 2.579(4) N1 C1 1.335(7) N1 C12 1.360(6) N2 C10 1.324(7) N2 C11 1.357(6) C1 C2 1.404(8) C1 H1 0.9300 C2 C3 1.367(8) C2 H2 0.9300 C3 C4 1.395(8) C3 H3 0.9300 C4 C12 1.403(7) C4 C5 1.418(8) C5 C6 1.341(9) C5 H5 0.9300 C6 C7 1.430(8) C6 H6 0.9300 C7 C8 1.405(8) C7 C11 1.414(7) C8 C9 1.334(8) C8 H8 0.9300 C9 C10 1.389(7) C9 H9 0.9300 C10 H10 0.9300 C11 C12 1.443(7) O1 C13 1.286(6) O2 C14 1.282(6) C13 C19 1.390(7) C13 C14 1.464(7) C14 C15 1.408(8) C15 C16 1.372(8) C15 H15 0.9300 C16 C17 1.378(8) C16 H16 0.9300 C17 C18 1.386(8) C17 H17 0.9300 C18 C19 1.380(7) C18 H18 0.9300 C19 H19 0.9300 O3 C20 1.284(6) O4 C21 1.268(6) C20 C26 1.381(7) C20 C21 1.468(7) C21 C22 1.398(7) C22 C23 1.379(8) C22 H22 0.9300 C23 C24 1.396(9) C23 H23 0.9300 C24 C25 1.383(9) C24 H24 0.9300 C25 C26 1.391(8) C25 H25 0.9300 C26 H26 0.9300 O5 C27 1.275(6) O6 C28 1.275(6) C27 C33 1.409(8) C27 C28 1.474(7) C28 C29 1.403(7) C29 C30 1.376(8) C29 H29 0.9300 C30 C31 1.378(8) C30 H30 0.9300 C31 C32 1.370(8) C31 H31 0.9300 C32 C33 1.376(8) C32 H32 0.9300 C33 H33 0.9300 O7 H71 0.8466 O7 H72 0.8212 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2 O6 0.93 2.65 3.531(7) 158.9 4_565 C10 H10 O4 0.93 2.34 2.982(6) 126.1 . C15 H15 O7 0.93 2.49 3.267(7) 141.9 3_566 O7 H71 O5 0.85 2.05 2.892(6) 169.8 . O7 H72 O7 0.82 2.55 3.048(11) 120.2 3_666 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 C12 N1 C1 C2 -1.4(8) Dy1 N1 C1 C2 179.0(4) N1 C1 C2 C3 1.2(9) C1 C2 C3 C4 0.4(9) C2 C3 C4 C12 -1.7(8) C2 C3 C4 C5 179.0(6) C3 C4 C5 C6 179.4(6) C12 C4 C5 C6 0.0(9) C4 C5 C6 C7 -0.9(9) C5 C6 C7 C8 -178.3(6) C5 C6 C7 C11 0.5(9) C11 C7 C8 C9 0.1(8) C6 C7 C8 C9 178.9(6) C7 C8 C9 C10 -0.6(9) C11 N2 C10 C9 -2.0(8) Dy1 N2 C10 C9 176.9(4) C8 C9 C10 N2 1.7(9) C10 N2 C11 C7 1.4(7) Dy1 N2 C11 C7 -177.5(4) C10 N2 C11 C12 -178.7(5) Dy1 N2 C11 C12 2.4(6) C8 C7 C11 N2 -0.5(8) C6 C7 C11 N2 -179.4(5) C8 C7 C11 C12 179.6(5) C6 C7 C11 C12 0.7(7) C1 N1 C12 C4 0.0(8) Dy1 N1 C12 C4 179.6(4) C1 N1 C12 C11 179.8(5) Dy1 N1 C12 C11 -0.7(6) C3 C4 C12 N1 1.5(8) C5 C4 C12 N1 -179.2(5) C3 C4 C12 C11 -178.2(5) C5 C4 C12 C11 1.1(8) N2 C11 C12 N1 -1.1(7) C7 C11 C12 N1 178.8(5) N2 C11 C12 C4 178.6(5) C7 C11 C12 C4 -1.5(7) Dy1 O1 C13 C19 -177.9(3) Dy1 O1 C13 C14 2.0(6) Dy1 O2 C14 C15 174.4(4) Dy1 O2 C14 C13 -4.4(6) O1 C13 C14 O2 1.5(6) C19 C13 C14 O2 -178.7(5) O1 C13 C14 C15 -177.2(5) C19 C13 C14 C15 2.7(8) O2 C14 C15 C16 -179.2(6) C13 C14 C15 C16 -0.6(10) C14 C15 C16 C17 -2.5(11) C15 C16 C17 C18 2.3(11) C16 C17 C18 C19 0.2(10) C17 C18 C19 C13 -0.8(10) O1 C13 C19 C18 178.4(5) C14 C13 C19 C18 -1.4(9) Dy1 O3 C20 C26 -179.8(4) Dy1 O3 C20 C21 -1.5(6) Dy1 O4 C21 C22 -174.9(4) Dy1 O4 C21 C20 3.7(6) O3 C20 C21 O4 -1.4(7) C26 C20 C21 O4 176.8(5) O3 C20 C21 C22 177.0(5) C26 C20 C21 C22 -4.8(9) O4 C21 C22 C23 -179.1(6) C20 C21 C22 C23 2.5(10) C21 C22 C23 C24 -0.2(12) C22 C23 C24 C25 1.3(12) C23 C24 C25 C26 -3.2(12) O3 C20 C26 C25 -178.8(6) C21 C20 C26 C25 3.0(10) C24 C25 C26 C20 1.4(12) Dy1 O5 C27 C33 -178.3(4) Dy1 O5 C27 C28 1.5(6) Dy1 O6 C28 C29 178.1(3) Dy1 O6 C28 C27 -1.3(5) O5 C27 C28 O6 -0.1(6) C33 C27 C28 O6 179.7(5) O5 C27 C28 C29 -179.5(5) C33 C27 C28 C29 0.3(8) O6 C28 C29 C30 179.2(5) C27 C28 C29 C30 -1.4(9) C28 C29 C30 C31 0.2(10) C29 C30 C31 C32 1.4(10) C30 C31 C32 C33 -0.8(10) C31 C32 C33 C27 -1.2(11) O5 C27 C33 C32 -178.7(6) C28 C27 C33 C32 1.5(10)