#------------------------------------------------------------------------------ #$Date: 2019-04-11 02:03:38 +0300 (Thu, 11 Apr 2019) $ #$Revision: 214595 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/96/7049649.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_7049649 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 tropolone ligand: structure, magnetic property and theoretical elucidation ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT00364A _journal_year 2019 _chemical_formula_moiety 'C31 H21 Dy N6 O8' _chemical_formula_sum 'C31 H21 Dy N6 O8' _chemical_formula_weight 768.04 _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 ; 2019-01-16 deposited with the CCDC. 2019-04-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.10(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.674(6) _cell_length_b 17.476(9) _cell_length_c 12.846(6) _cell_measurement_reflns_used 5144 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 25.22 _cell_measurement_theta_min 2.44 _cell_volume 2829(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 0.984 _diffrn_measured_fraction_theta_max 0.984 _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 0.0392 _diffrn_reflns_av_unetI/netI 0.0399 _diffrn_reflns_Laue_measured_fraction_full 0.984 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 16663 _diffrn_reflns_point_group_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 25.017 _diffrn_reflns_theta_max 25.017 _diffrn_reflns_theta_min 1.975 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 2.707 _exptl_absorpt_correction_T_max 0.631 _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_crystal_density_diffrn 1.803 _exptl_crystal_description block _exptl_crystal_F_000 1516 _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.170 _refine_diff_density_max 0.970 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.079 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 415 _refine_ls_number_reflns 4915 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0290 _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^)+(0.0288P)^2^+0.7241P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.0639 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3992 _reflns_number_total 4915 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00364a2.cif _cod_data_source_block AAA _cod_database_code 7049649 _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 0.507 _shelx_estimated_absorpt_t_max 0.656 _shelx_res_file ; AAA.res created by SHELXL-2014/7 TITL AAA in P1 #1 New: P21/c New: P21/n CELL 0.71073 12.6740 17.4760 12.8460 90.000 96.100 90.000 ZERR 4 0.0060 0.0090 0.0060 0.000 0.040 0.000 LATT 1 SYMM 0.50000 - X , 0.50000 + Y , 0.50000 - Z SFAC C H Dy N O UNIT 124 84 4 24 32 omit 1 7 1 omit 8 2 1 omit 4 2 0 omit -3 7 5 omit 3 7 1 omit 4 10 2 omit 3 5 4 omit 9 3 2 omit 1 8 1 omit 1 2 0 omit 3 4 0 omit 0 2 1 omit -3 50.04 L.S. 16 FMAP 2 PLAN -20 ACTA BOND $H TEMP 23 size 0.29 0.19 0.17 CONF HTAB WGHT 0.028800 0.724100 FVAR 0.09231 DY1 3 0.485343 0.302601 0.227337 11.00000 0.03832 0.03052 = 0.02699 0.00064 0.00821 -0.00385 O1 5 0.522573 0.406045 0.340809 11.00000 0.06309 0.03872 = 0.04050 -0.00100 0.01382 -0.01246 O2 5 0.521523 0.418229 0.142663 11.00000 0.05322 0.03375 = 0.04335 0.00151 0.00489 -0.00666 O3 5 0.658320 0.277909 0.376403 11.00000 0.06097 0.06705 = 0.04438 0.00365 0.01378 -0.01478 O4 5 0.680160 0.318168 0.221313 11.00000 0.04838 0.06415 = 0.03364 0.00349 0.00062 0.00058 O5 5 0.812878 0.319535 0.343736 11.00000 0.04246 0.07344 = 0.06280 -0.00140 -0.00623 -0.00508 O6 5 0.338296 0.339046 0.084909 11.00000 0.05359 0.05009 = 0.05052 0.01262 0.00338 -0.00137 O7 5 0.311401 0.365080 0.243959 11.00000 0.05750 0.05514 = 0.06197 -0.00801 0.01356 0.00201 O8 5 0.185738 0.384053 0.117867 11.00000 0.05733 0.09671 = 0.13831 0.02261 -0.00876 0.02097 N1 4 0.534363 0.246301 0.057618 11.00000 0.03786 0.03947 = 0.02833 0.00009 0.00397 -0.00550 N2 4 0.558008 0.159454 0.236114 11.00000 0.03934 0.04073 = 0.04078 0.00169 0.00748 0.00708 N3 4 0.335868 0.198809 0.202883 11.00000 0.03941 0.03113 = 0.03413 0.00100 0.00171 0.00074 N4 4 0.425327 0.248105 0.393787 11.00000 0.04368 0.04115 = 0.02864 -0.00145 0.00712 -0.00720 N5 4 0.719439 0.305052 0.315256 11.00000 0.03974 0.04116 = 0.04155 -0.00432 0.00459 -0.00205 N6 4 0.275455 0.363253 0.147233 11.00000 0.04230 0.03912 = 0.08092 0.00953 0.00449 -0.00117 C1 1 0.560000 0.468354 0.307946 11.00000 0.03229 0.03745 = 0.04335 -0.00047 0.00875 0.00522 C2 1 0.596160 0.524804 0.381727 11.00000 0.04922 0.03855 = 0.04832 -0.00147 0.00826 0.00433 AFIX 43 H2 2 0.585706 0.512893 0.450440 11.00000 -1.20000 AFIX 0 C3 1 0.644916 0.595456 0.369682 11.00000 0.05219 0.03894 = 0.06300 -0.00886 -0.00160 0.00565 AFIX 43 H3 2 0.663764 0.622125 0.431517 11.00000 -1.20000 AFIX 0 C4 1 0.669317 0.631627 0.279822 11.00000 0.05528 0.03500 = 0.07430 0.00207 0.00247 -0.00293 AFIX 43 H4 2 0.703134 0.678768 0.288642 11.00000 -1.20000 AFIX 0 C5 1 0.649017 0.605486 0.178192 11.00000 0.05359 0.03600 = 0.06558 0.01161 0.00683 -0.00020 AFIX 43 H5 2 0.671067 0.637716 0.127112 11.00000 -1.20000 AFIX 0 C6 1 0.600460 0.538065 0.141094 11.00000 0.04937 0.03827 = 0.04786 0.00948 0.00853 0.00369 AFIX 43 H6 2 0.592440 0.533391 0.068568 11.00000 -1.20000 AFIX 0 C7 1 0.560913 0.474939 0.195302 11.00000 0.03514 0.03685 = 0.04398 0.00506 0.00184 0.00784 C8 1 0.532367 0.289296 -0.026917 11.00000 0.04789 0.04898 = 0.03455 0.00213 0.00350 -0.00490 AFIX 43 H8 2 0.512118 0.340228 -0.022286 11.00000 -1.20000 AFIX 0 C9 1 0.559244 0.262162 -0.123642 11.00000 0.05213 0.06936 = 0.03279 0.00139 0.00674 -0.01048 AFIX 43 H9 2 0.556429 0.294451 -0.181418 11.00000 -1.20000 AFIX 0 C10 1 0.589475 0.187795 -0.131327 11.00000 0.04698 0.07978 = 0.03896 -0.01714 0.00611 -0.00642 AFIX 43 H10 2 0.607969 0.168979 -0.194632 11.00000 -1.20000 AFIX 0 C11 1 0.592703 0.139949 -0.044491 11.00000 0.04376 0.05895 = 0.04364 -0.00932 0.00975 0.00389 C12 1 0.566039 0.171533 0.050754 11.00000 0.03579 0.04087 = 0.04322 -0.01015 0.00534 0.00099 C13 1 0.622346 0.060241 -0.048089 11.00000 0.06825 0.06811 = 0.06285 -0.02433 0.01057 0.01488 AFIX 43 H13 2 0.640338 0.039331 -0.110393 11.00000 -1.20000 AFIX 0 C14 1 0.624192 0.016017 0.037616 11.00000 0.06974 0.05649 = 0.08594 -0.02386 0.00856 0.00755 AFIX 43 H14 2 0.641006 -0.035585 0.032972 11.00000 -1.20000 AFIX 0 C15 1 0.600812 0.046664 0.136000 11.00000 0.05019 0.04147 = 0.06699 -0.00951 0.00639 0.00470 C16 1 0.573355 0.125650 0.143532 11.00000 0.03781 0.03844 = 0.05012 -0.00052 0.00525 0.00604 C17 1 0.607622 0.003414 0.228534 11.00000 0.07524 0.03941 = 0.09086 0.00520 0.01098 0.00887 AFIX 43 H17 2 0.621317 -0.048818 0.226596 11.00000 -1.20000 AFIX 0 C18 1 0.594206 0.037893 0.320745 11.00000 0.08085 0.05121 = 0.07381 0.02360 0.01054 0.01527 AFIX 43 H18 2 0.600179 0.009836 0.382608 11.00000 -1.20000 AFIX 0 C19 1 0.571440 0.115598 0.321736 11.00000 0.04882 0.05597 = 0.04834 0.01478 0.00905 0.01225 AFIX 43 H19 2 0.565139 0.138587 0.386074 11.00000 -1.20000 AFIX 0 C20 1 0.291142 0.174667 0.110144 11.00000 0.04455 0.03934 = 0.03873 -0.00263 0.00047 -0.00200 AFIX 43 H20 2 0.309193 0.198951 0.050099 11.00000 -1.20000 AFIX 0 C21 1 0.218166 0.114341 0.099169 11.00000 0.04655 0.04782 = 0.05700 -0.01493 -0.00547 -0.00369 AFIX 43 H21 2 0.187025 0.100256 0.033129 11.00000 -1.20000 AFIX 0 C22 1 0.193163 0.076575 0.185390 11.00000 0.03931 0.04006 = 0.08098 -0.00605 0.00385 -0.00743 AFIX 43 H22 2 0.147602 0.034742 0.178462 11.00000 -1.20000 AFIX 0 C23 1 0.236201 0.100762 0.285142 11.00000 0.03573 0.03337 = 0.06397 0.00861 0.01012 -0.00020 C24 1 0.307549 0.162728 0.290630 11.00000 0.03019 0.03116 = 0.03802 0.00676 0.00592 0.00299 C25 1 0.210022 0.066045 0.380791 11.00000 0.04606 0.04205 = 0.08428 0.01640 0.01700 -0.00809 AFIX 43 H25 2 0.163056 0.025019 0.377630 11.00000 -1.20000 AFIX 0 C26 1 0.252066 0.091795 0.473867 11.00000 0.05012 0.05352 = 0.07019 0.02799 0.02116 -0.00193 AFIX 43 H26 2 0.232391 0.069276 0.534494 11.00000 -1.20000 AFIX 0 C27 1 0.326570 0.153170 0.482117 11.00000 0.04273 0.05065 = 0.04174 0.01831 0.01489 0.00717 C28 1 0.354513 0.189642 0.390588 11.00000 0.03202 0.03596 = 0.03858 0.00721 0.01150 0.00319 C29 1 0.378896 0.176948 0.578557 11.00000 0.06717 0.06434 = 0.04381 0.01888 0.02053 0.00962 AFIX 43 H29 2 0.363654 0.153823 0.640425 11.00000 -1.20000 AFIX 0 C30 1 0.451931 0.233974 0.580790 11.00000 0.07256 0.06556 = 0.02713 0.00303 0.00893 0.00565 AFIX 43 H30 2 0.488515 0.249267 0.643956 11.00000 -1.20000 AFIX 0 C31 1 0.471654 0.269585 0.486901 11.00000 0.05499 0.05164 = 0.03820 -0.00788 0.00858 -0.00697 AFIX 43 H31 2 0.519398 0.310137 0.489955 11.00000 -1.20000 AFIX 0 HKLF 4 REM AAA in P1 #1 New: P21/c New: P21/n REM R1 = 0.0290 for 3992 Fo > 4sig(Fo) and 0.0413 for all 4915 data REM 415 parameters refined using 0 restraints END WGHT 0.0286 0.7569 REM Instructions for potential hydrogen bonds HTAB C8 O2 HTAB C19 N4 HTAB C31 O1 REM Highest difference peak 0.970, deepest hole -0.486, 1-sigma level 0.079 Q1 1 0.4345 0.3371 0.1997 11.00000 0.05 0.97 Q2 1 0.4963 0.3479 0.2728 11.00000 0.05 0.45 Q3 1 0.3568 0.2264 0.5881 11.00000 0.05 0.41 Q4 1 0.4848 0.2673 0.2768 11.00000 0.05 0.40 Q5 1 0.4633 0.2627 0.3368 11.00000 0.05 0.35 Q6 1 0.5368 0.2504 0.1950 11.00000 0.05 0.35 Q7 1 0.4806 0.2658 0.1642 11.00000 0.05 0.34 Q8 1 0.4611 0.2555 0.2321 11.00000 0.05 0.33 Q9 1 0.5521 0.2684 0.2866 11.00000 0.05 0.33 Q10 1 0.5132 0.4445 0.3176 11.00000 0.05 0.33 Q11 1 0.4003 0.2786 0.5663 11.00000 0.05 0.33 Q12 1 0.4033 0.2974 0.1040 11.00000 0.05 0.32 Q13 1 0.1820 0.3544 0.1159 11.00000 0.05 0.31 Q14 1 0.5600 0.3233 0.2602 11.00000 0.05 0.31 Q15 1 0.6344 0.1203 0.1604 11.00000 0.05 0.29 Q16 1 0.4544 0.2540 0.0627 11.00000 0.05 0.29 Q17 1 0.7025 0.0270 0.2736 11.00000 0.05 0.28 Q18 1 0.7383 -0.0061 0.1234 11.00000 0.05 0.28 Q19 1 0.3009 0.1904 0.4729 11.00000 0.05 0.27 Q20 1 0.3557 0.1636 0.4365 11.00000 0.05 0.27 ; _shelx_res_checksum 7480 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 0.48534(2) 0.30260(2) 0.22734(2) 0.03160(7) Uani 1 1 d . . O1 O 0.5226(2) 0.40604(16) 0.3408(2) 0.0468(7) Uani 1 1 d . . O2 O 0.5215(2) 0.41823(15) 0.1427(2) 0.0435(7) Uani 1 1 d . . O3 O 0.6583(3) 0.27791(19) 0.3764(2) 0.0569(9) Uani 1 1 d . . O4 O 0.6802(2) 0.31817(17) 0.2213(2) 0.0490(8) Uani 1 1 d . . O5 O 0.8129(3) 0.31953(19) 0.3437(3) 0.0604(9) Uani 1 1 d . . O6 O 0.3383(3) 0.33905(18) 0.0849(2) 0.0516(8) Uani 1 1 d . . O7 O 0.3114(3) 0.36508(18) 0.2440(3) 0.0577(9) Uani 1 1 d . . O8 O 0.1857(3) 0.3841(2) 0.1179(4) 0.0988(14) Uani 1 1 d . . N1 N 0.5344(3) 0.24630(18) 0.0576(2) 0.0352(8) Uani 1 1 d . . N2 N 0.5580(3) 0.15945(19) 0.2361(3) 0.0401(8) Uani 1 1 d . . N3 N 0.3359(3) 0.19881(17) 0.2029(2) 0.0350(8) Uani 1 1 d . . N4 N 0.4253(3) 0.24811(18) 0.3938(2) 0.0376(8) Uani 1 1 d . . N5 N 0.7194(3) 0.30505(19) 0.3153(3) 0.0408(8) Uani 1 1 d . . N6 N 0.2755(3) 0.3633(2) 0.1472(4) 0.0543(10) Uani 1 1 d . . C1 C 0.5600(3) 0.4684(2) 0.3079(3) 0.0374(10) Uani 1 1 d . . C2 C 0.5962(4) 0.5248(2) 0.3817(3) 0.0451(11) Uani 1 1 d . . H2 H 0.5857 0.5129 0.4504 0.054 Uiso 1 1 calc R U C3 C 0.6449(4) 0.5955(3) 0.3697(4) 0.0519(12) Uani 1 1 d . . H3 H 0.6638 0.6221 0.4315 0.062 Uiso 1 1 calc R U C4 C 0.6693(4) 0.6316(3) 0.2798(4) 0.0552(13) Uani 1 1 d . . H4 H 0.7031 0.6788 0.2886 0.066 Uiso 1 1 calc R U C5 C 0.6490(4) 0.6055(2) 0.1782(4) 0.0517(12) Uani 1 1 d . . H5 H 0.6711 0.6377 0.1271 0.062 Uiso 1 1 calc R U C6 C 0.6005(4) 0.5381(2) 0.1411(4) 0.0449(11) Uani 1 1 d . . H6 H 0.5924 0.5334 0.0686 0.054 Uiso 1 1 calc R U C7 C 0.5609(3) 0.4749(2) 0.1953(3) 0.0388(10) Uani 1 1 d . . C8 C 0.5324(4) 0.2893(2) -0.0269(3) 0.0439(11) Uani 1 1 d . . H8 H 0.5121 0.3402 -0.0223 0.053 Uiso 1 1 calc R U C9 C 0.5592(4) 0.2622(3) -0.1236(3) 0.0513(12) Uani 1 1 d . . H9 H 0.5564 0.2945 -0.1814 0.062 Uiso 1 1 calc R U C10 C 0.5895(4) 0.1878(3) -0.1313(4) 0.0551(13) Uani 1 1 d . . H10 H 0.6080 0.1690 -0.1946 0.066 Uiso 1 1 calc R U C11 C 0.5927(4) 0.1399(3) -0.0445(3) 0.0484(11) Uani 1 1 d . . C12 C 0.5660(3) 0.1715(2) 0.0508(3) 0.0399(10) Uani 1 1 d . . C13 C 0.6223(4) 0.0602(3) -0.0481(4) 0.0661(15) Uani 1 1 d . . H13 H 0.6403 0.0393 -0.1104 0.079 Uiso 1 1 calc R U C14 C 0.6242(4) 0.0160(3) 0.0376(5) 0.0707(16) Uani 1 1 d . . H14 H 0.6410 -0.0356 0.0330 0.085 Uiso 1 1 calc R U C15 C 0.6008(4) 0.0467(2) 0.1360(4) 0.0529(12) Uani 1 1 d . . C16 C 0.5734(3) 0.1257(2) 0.1435(3) 0.0421(10) Uani 1 1 d . . C17 C 0.6076(4) 0.0034(3) 0.2285(5) 0.0683(15) Uani 1 1 d . . H17 H 0.6213 -0.0488 0.2266 0.082 Uiso 1 1 calc R U C18 C 0.5942(5) 0.0379(3) 0.3207(5) 0.0685(15) Uani 1 1 d . . H18 H 0.6002 0.0098 0.3826 0.082 Uiso 1 1 calc R U C19 C 0.5714(4) 0.1156(3) 0.3217(4) 0.0508(12) Uani 1 1 d . . H19 H 0.5651 0.1386 0.3861 0.061 Uiso 1 1 calc R U C20 C 0.2911(3) 0.1747(2) 0.1101(3) 0.0412(10) Uani 1 1 d . . H20 H 0.3092 0.1990 0.0501 0.049 Uiso 1 1 calc R U C21 C 0.2182(4) 0.1143(2) 0.0992(4) 0.0512(12) Uani 1 1 d . . H21 H 0.1870 0.1003 0.0331 0.061 Uiso 1 1 calc R U C22 C 0.1932(4) 0.0766(3) 0.1854(4) 0.0536(13) Uani 1 1 d . . H22 H 0.1476 0.0347 0.1785 0.064 Uiso 1 1 calc R U C23 C 0.2362(3) 0.1008(2) 0.2851(4) 0.0440(11) Uani 1 1 d . . C24 C 0.3075(3) 0.1627(2) 0.2906(3) 0.0330(9) Uani 1 1 d . . C25 C 0.2100(4) 0.0660(3) 0.3808(4) 0.0567(13) Uani 1 1 d . . H25 H 0.1631 0.0250 0.3776 0.068 Uiso 1 1 calc R U C26 C 0.2521(4) 0.0918(3) 0.4739(4) 0.0569(13) Uani 1 1 d . . H26 H 0.2324 0.0693 0.5345 0.068 Uiso 1 1 calc R U C27 C 0.3266(4) 0.1532(3) 0.4821(3) 0.0443(11) Uani 1 1 d . . C28 C 0.3545(3) 0.1896(2) 0.3906(3) 0.0350(9) Uani 1 1 d . . C29 C 0.3789(4) 0.1769(3) 0.5786(4) 0.0574(14) Uani 1 1 d . . H29 H 0.3637 0.1538 0.6404 0.069 Uiso 1 1 calc R U C30 C 0.4519(4) 0.2340(3) 0.5808(3) 0.0548(13) Uani 1 1 d . . H30 H 0.4885 0.2493 0.6440 0.066 Uiso 1 1 calc R U C31 C 0.4717(4) 0.2696(3) 0.4869(3) 0.0480(11) Uani 1 1 d . . H31 H 0.5194 0.3101 0.4900 0.058 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 0.03832(12) 0.03052(10) 0.02699(11) 0.00064(8) 0.00821(8) -0.00385(9) O1 0.063(2) 0.0387(16) 0.0405(17) -0.0010(13) 0.0138(15) -0.0125(15) O2 0.0532(19) 0.0338(15) 0.0434(17) 0.0015(12) 0.0049(14) -0.0067(14) O3 0.061(2) 0.067(2) 0.0444(19) 0.0037(15) 0.0138(17) -0.0148(18) O4 0.0484(19) 0.064(2) 0.0336(17) 0.0035(14) 0.0006(14) 0.0006(16) O5 0.042(2) 0.073(2) 0.063(2) -0.0014(17) -0.0062(17) -0.0051(17) O6 0.054(2) 0.0501(18) 0.0505(19) 0.0126(15) 0.0034(17) -0.0014(17) O7 0.057(2) 0.055(2) 0.062(2) -0.0080(17) 0.0136(18) 0.0020(17) O8 0.057(3) 0.097(3) 0.138(4) 0.023(3) -0.009(2) 0.021(2) N1 0.038(2) 0.0395(19) 0.0283(19) 0.0001(14) 0.0040(15) -0.0055(16) N2 0.039(2) 0.0407(19) 0.041(2) 0.0017(16) 0.0075(17) 0.0071(17) N3 0.039(2) 0.0311(17) 0.0341(19) 0.0010(14) 0.0017(15) 0.0007(16) N4 0.044(2) 0.0412(19) 0.0286(19) -0.0015(14) 0.0071(16) -0.0072(17) N5 0.040(2) 0.0412(19) 0.042(2) -0.0043(17) 0.0046(18) -0.0021(18) N6 0.042(3) 0.039(2) 0.081(3) 0.010(2) 0.004(2) -0.0012(19) C1 0.032(2) 0.037(2) 0.043(2) -0.0005(18) 0.0087(19) 0.0052(19) C2 0.049(3) 0.039(2) 0.048(3) -0.0015(19) 0.008(2) 0.004(2) C3 0.052(3) 0.039(2) 0.063(3) -0.009(2) -0.002(2) 0.006(2) C4 0.055(3) 0.035(2) 0.074(4) 0.002(2) 0.002(3) -0.003(2) C5 0.054(3) 0.036(2) 0.066(3) 0.012(2) 0.007(2) 0.000(2) C6 0.049(3) 0.038(2) 0.048(3) 0.0095(19) 0.009(2) 0.004(2) C7 0.035(2) 0.037(2) 0.044(3) 0.0051(19) 0.002(2) 0.0078(19) C8 0.048(3) 0.049(3) 0.035(2) 0.0021(19) 0.004(2) -0.005(2) C9 0.052(3) 0.069(3) 0.033(3) 0.001(2) 0.007(2) -0.010(3) C10 0.047(3) 0.080(4) 0.039(3) -0.017(2) 0.006(2) -0.006(3) C11 0.044(3) 0.059(3) 0.044(3) -0.009(2) 0.010(2) 0.004(2) C12 0.036(2) 0.041(2) 0.043(3) -0.0101(19) 0.005(2) 0.0010(19) C13 0.068(4) 0.068(3) 0.063(4) -0.024(3) 0.011(3) 0.015(3) C14 0.070(4) 0.056(3) 0.086(4) -0.024(3) 0.009(3) 0.008(3) C15 0.050(3) 0.041(3) 0.067(3) -0.010(2) 0.006(3) 0.005(2) C16 0.038(3) 0.038(2) 0.050(3) -0.001(2) 0.005(2) 0.006(2) C17 0.075(4) 0.039(3) 0.091(4) 0.005(3) 0.011(3) 0.009(3) C18 0.081(4) 0.051(3) 0.074(4) 0.024(3) 0.011(3) 0.015(3) C19 0.049(3) 0.056(3) 0.048(3) 0.015(2) 0.009(2) 0.012(2) C20 0.045(3) 0.039(2) 0.039(3) -0.0026(18) 0.000(2) -0.002(2) C21 0.047(3) 0.048(3) 0.057(3) -0.015(2) -0.005(2) -0.004(2) C22 0.039(3) 0.040(3) 0.081(4) -0.006(2) 0.004(3) -0.007(2) C23 0.036(2) 0.033(2) 0.064(3) 0.009(2) 0.010(2) 0.000(2) C24 0.030(2) 0.031(2) 0.038(2) 0.0068(17) 0.0059(18) 0.0030(17) C25 0.046(3) 0.042(3) 0.084(4) 0.016(3) 0.017(3) -0.008(2) C26 0.050(3) 0.054(3) 0.070(4) 0.028(3) 0.021(3) -0.002(3) C27 0.043(3) 0.051(3) 0.042(3) 0.018(2) 0.015(2) 0.007(2) C28 0.032(2) 0.036(2) 0.039(2) 0.0072(18) 0.0115(18) 0.0032(19) C29 0.067(4) 0.064(3) 0.044(3) 0.019(2) 0.021(3) 0.010(3) C30 0.073(4) 0.066(3) 0.027(2) 0.003(2) 0.009(2) 0.006(3) C31 0.055(3) 0.052(3) 0.038(3) -0.008(2) 0.009(2) -0.007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 Dy1 O2 65.77(10) O1 Dy1 O7 74.30(11) O2 Dy1 O7 83.18(11) O1 Dy1 O4 78.47(10) O2 Dy1 O4 69.58(10) O7 Dy1 O4 147.53(10) O1 Dy1 N1 141.84(10) O2 Dy1 N1 81.86(10) O7 Dy1 N1 123.06(12) O4 Dy1 N1 71.39(11) O1 Dy1 N4 79.81(10) O2 Dy1 N4 143.26(10) O7 Dy1 N4 75.18(12) O4 Dy1 N4 117.06(11) N1 Dy1 N4 134.87(11) O1 Dy1 O6 109.74(11) O2 Dy1 O6 67.60(10) O7 Dy1 O6 50.63(11) O4 Dy1 O6 126.95(10) N1 Dy1 O6 72.92(11) N4 Dy1 O6 115.97(11) O1 Dy1 N3 134.91(10) O2 Dy1 N3 135.30(10) O7 Dy1 N3 71.22(11) O4 Dy1 N3 141.11(10) N1 Dy1 N3 82.41(10) N4 Dy1 N3 64.02(10) O6 Dy1 N3 67.82(10) O1 Dy1 N2 130.81(11) O2 Dy1 N2 137.69(10) O7 Dy1 N2 135.52(11) O4 Dy1 N2 76.39(10) N1 Dy1 N2 63.62(10) N4 Dy1 N2 75.19(10) O6 Dy1 N2 119.21(11) N3 Dy1 N2 66.23(10) O1 Dy1 O3 66.39(10) O2 Dy1 O3 105.77(10) O7 Dy1 O3 130.40(11) O4 Dy1 O3 47.85(10) N1 Dy1 O3 106.54(11) N4 Dy1 O3 69.28(11) O6 Dy1 O3 173.36(9) N3 Dy1 O3 118.79(10) N2 Dy1 O3 65.31(10) O1 Dy1 N6 93.12(12) O2 Dy1 N6 75.15(10) O7 Dy1 N6 25.46(10) O4 Dy1 N6 144.13(10) N1 Dy1 N6 97.72(13) N4 Dy1 N6 95.12(12) O6 Dy1 N6 25.23(10) N3 Dy1 N6 65.93(10) N2 Dy1 N6 130.39(11) O3 Dy1 N6 155.64(12) C1 O1 Dy1 120.7(2) C7 O2 Dy1 120.4(2) N5 O3 Dy1 90.2(2) N5 O4 Dy1 103.8(2) N6 O6 Dy1 95.2(3) N6 O7 Dy1 97.6(3) C8 N1 C12 118.0(3) C8 N1 Dy1 120.2(3) C12 N1 Dy1 121.7(2) C19 N2 C16 116.9(4) C19 N2 Dy1 125.9(3) C16 N2 Dy1 116.9(3) C20 N3 C24 117.7(3) C20 N3 Dy1 124.1(3) C24 N3 Dy1 118.0(2) C31 N4 C28 117.8(3) C31 N4 Dy1 120.7(3) C28 N4 Dy1 121.0(2) O5 N5 O3 122.1(4) O5 N5 O4 120.8(4) O3 N5 O4 117.1(4) O8 N6 O6 122.5(5) O8 N6 O7 121.3(5) O6 N6 O7 116.2(4) O8 N6 Dy1 175.4(3) O6 N6 Dy1 59.5(2) O7 N6 Dy1 56.9(2) O1 C1 C2 118.7(4) O1 C1 C7 116.1(4) C2 C1 C7 125.3(4) C3 C2 C1 131.3(4) C3 C2 H2 114.4 C1 C2 H2 114.4 C4 C3 C2 129.7(4) C4 C3 H3 115.1 C2 C3 H3 115.1 C3 C4 C5 127.1(4) C3 C4 H4 116.4 C5 C4 H4 116.4 C4 C5 C6 129.5(4) C4 C5 H5 115.3 C6 C5 H5 115.3 C5 C6 C7 130.9(4) C5 C6 H6 114.5 C7 C6 H6 114.5 O2 C7 C6 118.8(4) O2 C7 C1 115.1(4) C6 C7 C1 126.1(4) N1 C8 C9 123.4(4) N1 C8 H8 118.3 C9 C8 H8 118.3 C10 C9 C8 118.9(4) C10 C9 H9 120.6 C8 C9 H9 120.6 C9 C10 C11 120.0(4) C9 C10 H10 120.0 C11 C10 H10 120.0 C10 C11 C12 118.0(4) C10 C11 C13 122.6(4) C12 C11 C13 119.4(4) N1 C12 C11 121.7(4) N1 C12 C16 118.3(3) C11 C12 C16 120.1(4) C14 C13 C11 120.7(5) C14 C13 H13 119.7 C11 C13 H13 119.7 C13 C14 C15 121.4(5) C13 C14 H14 119.3 C15 C14 H14 119.3 C17 C15 C16 117.1(4) C17 C15 C14 123.1(5) C16 C15 C14 119.7(5) N2 C16 C15 122.5(4) N2 C16 C12 118.8(4) C15 C16 C12 118.6(4) C18 C17 C15 119.9(5) C18 C17 H17 120.0 C15 C17 H17 120.0 C17 C18 C19 119.2(5) C17 C18 H18 120.4 C19 C18 H18 120.4 N2 C19 C18 124.2(5) N2 C19 H19 117.9 C18 C19 H19 117.9 N3 C20 C21 122.8(4) N3 C20 H20 118.6 C21 C20 H20 118.6 C22 C21 C20 119.6(4) C22 C21 H21 120.2 C20 C21 H21 120.2 C21 C22 C23 119.8(4) C21 C22 H22 120.1 C23 C22 H22 120.1 C22 C23 C24 117.6(4) C22 C23 C25 123.3(4) C24 C23 C25 119.1(4) N3 C24 C23 122.3(4) N3 C24 C28 117.7(3) C23 C24 C28 120.0(4) C26 C25 C23 121.1(4) C26 C25 H25 119.5 C23 C25 H25 119.5 C25 C26 C27 121.2(4) C25 C26 H26 119.4 C27 C26 H26 119.4 C29 C27 C28 117.6(4) C29 C27 C26 122.4(4) C28 C27 C26 120.0(4) N4 C28 C27 122.5(4) N4 C28 C24 118.9(3) C27 C28 C24 118.6(4) C30 C29 C27 119.5(4) C30 C29 H29 120.2 C27 C29 H29 120.2 C29 C30 C31 119.4(4) C29 C30 H30 120.3 C31 C30 H30 120.3 N4 C31 C30 123.1(4) N4 C31 H31 118.4 C30 C31 H31 118.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Dy1 O1 2.339(3) Dy1 O2 2.363(3) Dy1 O7 2.490(3) Dy1 O4 2.493(3) Dy1 N1 2.529(3) Dy1 N4 2.530(3) Dy1 O6 2.550(3) Dy1 N3 2.617(3) Dy1 N2 2.664(4) Dy1 O3 2.787(4) Dy1 N6 2.946(5) O1 C1 1.277(5) O2 C7 1.272(5) O3 N5 1.254(4) O4 N5 1.276(4) O5 N5 1.228(5) O6 N6 1.261(5) O7 N6 1.278(5) O8 N6 1.215(5) N1 C8 1.319(5) N1 C12 1.373(5) N2 C19 1.337(5) N2 C16 1.360(5) N3 C20 1.332(5) N3 C24 1.372(5) N4 C31 1.329(5) N4 C28 1.358(5) C1 C2 1.410(6) C1 C7 1.453(6) C2 C3 1.397(6) C2 H2 0.9300 C3 C4 1.380(6) C3 H3 0.9300 C4 C5 1.381(6) C4 H4 0.9300 C5 C6 1.390(6) C5 H5 0.9300 C6 C7 1.424(5) C6 H6 0.9300 C8 C9 1.405(6) C8 H8 0.9300 C9 C10 1.361(7) C9 H9 0.9300 C10 C11 1.391(7) C10 H10 0.9300 C11 C12 1.416(6) C11 C13 1.445(7) C12 C16 1.431(6) C13 C14 1.343(7) C13 H13 0.9300 C14 C15 1.432(7) C14 H14 0.9300 C15 C17 1.404(7) C15 C16 1.429(6) C17 C18 1.356(7) C17 H17 0.9300 C18 C19 1.389(7) C18 H18 0.9300 C19 H19 0.9300 C20 C21 1.400(6) C20 H20 0.9300 C21 C22 1.356(6) C21 H21 0.9300 C22 C23 1.403(6) C22 H22 0.9300 C23 C24 1.408(6) C23 C25 1.440(6) C24 C28 1.436(6) C25 C26 1.334(7) C25 H25 0.9300 C26 C27 1.425(6) C26 H26 0.9300 C27 C29 1.405(7) C27 C28 1.415(5) C29 C30 1.358(7) C29 H29 0.9300 C30 C31 1.403(6) C30 H30 0.9300 C31 H31 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 Dy1 O3 N5 O5 169.9(3) Dy1 O3 N5 O4 -9.2(3) Dy1 O4 N5 O5 -168.5(3) Dy1 O4 N5 O3 10.6(4) Dy1 O6 N6 O8 -175.1(4) Dy1 O6 N6 O7 5.1(4) Dy1 O7 N6 O8 174.9(4) Dy1 O7 N6 O6 -5.3(4) Dy1 O1 C1 C2 -170.6(3) Dy1 O1 C1 C7 9.8(5) O1 C1 C2 C3 176.4(5) C7 C1 C2 C3 -4.0(8) C1 C2 C3 C4 2.0(9) C2 C3 C4 C5 0.9(9) C3 C4 C5 C6 -0.1(9) C4 C5 C6 C7 -2.6(9) Dy1 O2 C7 C6 168.1(3) Dy1 O2 C7 C1 -12.3(5) C5 C6 C7 O2 -178.3(4) C5 C6 C7 C1 2.2(8) O1 C1 C7 O2 1.7(5) C2 C1 C7 O2 -177.9(4) O1 C1 C7 C6 -178.7(4) C2 C1 C7 C6 1.6(7) C12 N1 C8 C9 1.1(6) Dy1 N1 C8 C9 179.5(3) N1 C8 C9 C10 -0.3(7) C8 C9 C10 C11 0.4(7) C9 C10 C11 C12 -1.3(7) C9 C10 C11 C13 178.9(5) C8 N1 C12 C11 -2.0(6) Dy1 N1 C12 C11 179.5(3) C8 N1 C12 C16 177.0(4) Dy1 N1 C12 C16 -1.5(5) C10 C11 C12 N1 2.2(7) C13 C11 C12 N1 -178.1(4) C10 C11 C12 C16 -176.8(4) C13 C11 C12 C16 2.9(7) C10 C11 C13 C14 -179.9(5) C12 C11 C13 C14 0.4(8) C11 C13 C14 C15 -2.3(9) C13 C14 C15 C17 -176.4(5) C13 C14 C15 C16 0.9(8) C19 N2 C16 C15 1.1(6) Dy1 N2 C16 C15 -173.0(3) C19 N2 C16 C12 -176.3(4) Dy1 N2 C16 C12 9.6(5) C17 C15 C16 N2 2.4(7) C14 C15 C16 N2 -175.0(4) C17 C15 C16 C12 179.8(4) C14 C15 C16 C12 2.4(7) N1 C12 C16 N2 -5.8(6) C11 C12 C16 N2 173.2(4) N1 C12 C16 C15 176.7(4) C11 C12 C16 C15 -4.2(6) C16 C15 C17 C18 -3.6(8) C14 C15 C17 C18 173.7(5) C15 C17 C18 C19 1.4(9) C16 N2 C19 C18 -3.5(7) Dy1 N2 C19 C18 169.9(4) C17 C18 C19 N2 2.4(8) C24 N3 C20 C21 -0.6(6) Dy1 N3 C20 C21 174.2(3) N3 C20 C21 C22 -2.0(7) C20 C21 C22 C23 3.4(7) C21 C22 C23 C24 -2.2(6) C21 C22 C23 C25 177.1(4) C20 N3 C24 C23 1.8(6) Dy1 N3 C24 C23 -173.3(3) C20 N3 C24 C28 -179.0(4) Dy1 N3 C24 C28 5.9(4) C22 C23 C24 N3 -0.4(6) C25 C23 C24 N3 -179.7(4) C22 C23 C24 C28 -179.6(4) C25 C23 C24 C28 1.1(6) C22 C23 C25 C26 -179.1(5) C24 C23 C25 C26 0.1(7) C23 C25 C26 C27 -1.7(7) C25 C26 C27 C29 -174.3(5) C25 C26 C27 C28 2.1(7) C31 N4 C28 C27 2.0(6) Dy1 N4 C28 C27 174.1(3) C31 N4 C28 C24 -176.8(4) Dy1 N4 C28 C24 -4.7(5) C29 C27 C28 N4 -3.1(6) C26 C27 C28 N4 -179.7(4) C29 C27 C28 C24 175.7(4) C26 C27 C28 C24 -0.9(6) N3 C24 C28 N4 -1.0(5) C23 C24 C28 N4 178.2(4) N3 C24 C28 C27 -179.9(3) C23 C24 C28 C27 -0.7(6) C28 C27 C29 C30 1.1(7) C26 C27 C29 C30 177.6(5) C27 C29 C30 C31 1.8(7) C28 N4 C31 C30 1.0(6) Dy1 N4 C31 C30 -171.0(3) C29 C30 C31 N4 -3.0(7)