#------------------------------------------------------------------------------ #$Date: 2019-11-08 00:58:48 +0200 (Fri, 08 Nov 2019) $ #$Revision: 224380 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/92/7049256.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_7049256 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 H40 Cl4 Dy2 N12 O4' _chemical_formula_weight 1243.66 _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 ; 2019-01-30 deposited with the CCDC. 2019-03-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.012(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.3353(12) _cell_length_b 15.0093(13) _cell_length_c 15.7056(9) _cell_measurement_reflns_used 3487 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.8068 _cell_measurement_theta_min 2.9367 _cell_volume 4607.7(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 'CrysAlis PRO (Agilent, 2011)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.862 _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_unetI/netI 0.0821 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.862 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 10707 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.862 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 28.870 _diffrn_reflns_theta_min 2.943 _exptl_absorpt_coefficient_mu 3.506 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.84357 _exptl_absorpt_correction_type multi-scan _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 'clear red' _exptl_crystal_density_diffrn 1.793 _exptl_crystal_description block _exptl_crystal_F_000 2432 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.348 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.161 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 289 _refine_ls_number_reflns 5231 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0509 _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^)+(0.0434P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1063 _refine_ls_wR_factor_ref 0.1193 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3639 _reflns_number_total 5231 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00058e2.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 7049253--7049258.cif.' _cod_database_code 7049256 _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 ; 2.res created by SHELXL-2014/7 TITL 2_a.res in C2/c REM Old TITL 2 in Cc REM SHELXT solution in C2/c REM R1 0.137, Rweak 0.037, Alpha 0.073, Orientation as input REM Formula found by SHELXT: C12 N5 O3 Dy F2 S2 CELL 0.71073 20.3353 15.0093 15.7056 90 106.012 90 ZERR 4 0.0012 0.0013 0.0009 0 0.006 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl Dy N O UNIT 168 160 16 8 48 16 L.S. 10 PLAN 20 TEMP 19.85 BOND $H list 4 fmap 2 acta 52 dfix 2.15 H7 H18 REM REM REM WGHT 0.043400 FVAR 0.08907 DY01 4 0.563224 0.628484 0.862636 11.00000 0.02265 0.04580 = 0.02120 -0.00056 0.00285 -0.00096 CL2 3 0.582873 0.455764 0.856252 11.00000 0.04282 0.04667 = 0.03804 0.00338 0.01266 0.00272 CL1 3 0.572697 0.797843 0.898430 11.00000 0.05937 0.04936 = 0.05276 -0.00578 0.01550 -0.00123 O1 6 0.447994 0.632447 0.790842 11.00000 0.02495 0.04669 = 0.02211 -0.00066 0.00470 -0.00142 O2 6 0.454933 0.603276 0.499293 11.00000 0.02778 0.06797 = 0.02634 -0.00722 0.00973 0.00303 N2 5 0.331623 0.624132 0.505745 11.00000 0.03054 0.04381 = 0.02484 0.00149 0.00607 0.00396 N1 5 0.326498 0.641586 0.668159 11.00000 0.02493 0.04978 = 0.01909 0.00192 0.00042 0.00106 N4 5 0.423031 0.590037 0.351258 11.00000 0.04466 0.08507 = 0.02654 -0.00735 0.00851 0.00678 AFIX 93 H4A 2 0.464640 0.583448 0.349469 11.00000 -1.20000 H4B 2 0.390253 0.589151 0.303034 11.00000 -1.20000 AFIX 0 N3 5 0.342453 0.611071 0.424862 11.00000 0.04129 0.08100 = 0.02411 -0.00550 0.00749 -0.00943 AFIX 43 H3 2 0.309751 0.609114 0.376597 11.00000 -1.20000 AFIX 0 C9 1 0.266626 0.645850 0.604546 11.00000 0.02480 0.06470 = 0.03143 0.00218 0.00552 0.00146 C1 1 0.390696 0.638013 0.819627 11.00000 0.03309 0.04503 = 0.02860 0.00082 0.01011 0.00188 C5 1 0.326243 0.644056 0.754559 11.00000 0.02582 0.04967 = 0.03619 0.00053 0.01275 0.00054 C11 1 0.409678 0.601341 0.426899 11.00000 0.03385 0.04468 = 0.03242 0.00057 0.00788 0.00200 N5 5 0.239458 0.599278 0.261780 11.00000 0.04610 0.07292 = 0.04069 -0.00078 0.00141 0.01257 C10 1 0.272045 0.634437 0.515558 11.00000 0.02411 0.07755 = 0.02336 0.01207 -0.00409 -0.00002 AFIX 43 H10 2 0.233437 0.634604 0.467163 11.00000 -1.20000 AFIX 0 C2 1 0.389973 0.636404 0.905922 11.00000 0.03200 0.08309 = 0.02717 0.00796 0.00470 0.00581 AFIX 43 H2 2 0.431099 0.629659 0.949680 11.00000 -1.20000 AFIX 0 C6 1 0.264119 0.652739 0.779082 11.00000 0.03393 0.06669 = 0.03173 0.00816 0.00693 0.00363 C3 1 0.330142 0.644462 0.930703 11.00000 0.03818 0.11224 = 0.03300 0.00686 0.01185 0.00946 AFIX 43 H3A 2 0.332519 0.643566 0.990686 11.00000 -1.20000 AFIX 0 C4 1 0.267041 0.653780 0.869993 11.00000 0.03575 0.11370 = 0.03466 0.00768 0.01768 0.00741 AFIX 43 H4 2 0.227576 0.660550 0.888335 11.00000 -1.20000 AFIX 0 N6 5 -0.004619 0.678139 0.901208 11.00000 0.10710 0.11297 = 0.11331 0.01105 0.03620 0.05233 AFIX 43 H6 2 -0.030422 0.715613 0.918156 11.00000 -1.20000 AFIX 0 C8 1 0.203769 0.657710 0.624423 11.00000 0.02080 0.13295 = 0.03553 0.01292 0.00186 0.00999 AFIX 43 H8 2 0.163264 0.662752 0.579266 11.00000 -1.20000 AFIX 0 C7 1 0.203293 0.661633 0.710022 11.00000 0.02670 0.11852 = 0.03724 0.01103 0.00893 0.01414 AFIX 43 H7 2 0.162085 0.670364 0.723704 11.00000 -1.20000 AFIX 0 C17 1 0.048357 0.706369 0.869643 11.00000 0.07894 0.08111 = 0.11871 0.03560 0.01704 -0.02293 AFIX 43 H17 2 0.053599 0.767386 0.863547 11.00000 -1.20000 AFIX 0 C16 1 0.176354 0.619977 0.258980 11.00000 0.05320 0.09131 = 0.06644 -0.00520 0.01600 0.00179 AFIX 43 H16 2 0.166901 0.628896 0.313009 11.00000 -1.20000 AFIX 0 C18 1 0.089311 0.656727 0.848890 11.00000 0.06173 0.12189 = 0.12590 -0.01259 0.06092 -0.01967 AFIX 43 H18 2 0.126789 0.680526 0.833754 11.00000 -1.20000 AFIX 0 C15 1 0.123834 0.629613 0.185618 11.00000 0.04496 0.10189 = 0.08330 -0.00732 -0.00737 0.00934 AFIX 43 H15 2 0.080314 0.644479 0.189335 11.00000 -1.20000 AFIX 0 C21 1 -0.014732 0.590847 0.904716 11.00000 0.06240 0.08221 = 0.12207 0.03005 0.01574 -0.01792 AFIX 43 H21 2 -0.050664 0.567790 0.923835 11.00000 -1.20000 AFIX 0 C20 1 0.029957 0.537009 0.879025 11.00000 0.14097 0.03473 = 0.13917 -0.01281 -0.01883 0.02630 AFIX 43 H20 2 0.026861 0.475309 0.881746 11.00000 -1.20000 AFIX 0 C14 1 0.135999 0.617376 0.108823 11.00000 0.07861 0.11624 = 0.07027 0.02222 -0.04178 -0.00804 AFIX 43 H14 2 0.100964 0.624791 0.056877 11.00000 -1.20000 AFIX 0 C13 1 0.199978 0.593744 0.104639 11.00000 0.08605 0.16260 = 0.04092 0.00876 -0.00373 0.00093 AFIX 43 H13 2 0.209369 0.584009 0.050693 11.00000 -1.20000 AFIX 0 C12 1 0.250166 0.584939 0.184196 11.00000 0.05399 0.14287 = 0.06718 -0.01658 0.01861 0.01217 AFIX 43 H12 2 0.293796 0.567962 0.182614 11.00000 -1.20000 AFIX 0 C19 1 0.081200 0.578285 0.848085 11.00000 0.08672 0.20201 = 0.10678 -0.05605 0.03320 0.03813 AFIX 43 H19 2 0.110022 0.542473 0.826001 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2_a.res in C2/c REM R1 = 0.0509 for 3639 Fo > 4sig(Fo) and 0.0820 for all 5231 data REM 289 parameters refined using 1 restraints END WGHT 0.0434 0.0000 REM Highest difference peak 1.348, deepest hole -0.954, 1-sigma level 0.161 Q1 1 0.5924 0.5759 0.8594 11.00000 0.05 1.35 Q2 1 0.5334 0.6848 0.8563 11.00000 0.05 1.28 Q3 1 0.5866 0.6773 0.8599 11.00000 0.05 1.11 Q4 1 0.5097 0.6257 0.8039 11.00000 0.05 1.08 Q5 1 0.5382 0.5764 0.8673 11.00000 0.05 1.05 Q6 1 0.5970 0.6266 0.9207 11.00000 0.05 0.96 Q7 1 0.5887 0.6993 0.8971 11.00000 0.05 0.88 Q8 1 0.6024 0.7411 0.8993 11.00000 0.05 0.80 Q9 1 0.5578 0.5025 0.8537 11.00000 0.05 0.75 Q10 1 0.3878 0.6306 0.7125 11.00000 0.05 0.74 Q11 1 0.6103 0.5084 0.8832 11.00000 0.05 0.70 Q12 1 0.5787 0.7396 0.9833 11.00000 0.05 0.59 Q13 1 0.0555 0.6163 0.8480 11.00000 0.05 0.59 Q14 1 0.0771 0.6804 0.8608 11.00000 0.05 0.59 Q15 1 0.6058 0.4601 0.8998 11.00000 0.05 0.58 Q16 1 0.5593 0.4565 0.8816 11.00000 0.05 0.56 Q17 1 0.2203 0.6221 0.3424 11.00000 0.05 0.55 Q18 1 0.4624 0.5815 0.8210 11.00000 0.05 0.54 Q19 1 0.5516 0.7425 0.9090 11.00000 0.05 0.54 Q20 1 0.4377 0.5759 0.5688 11.00000 0.05 0.54 ; _shelx_res_checksum 51043 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 Dy01 Dy 0.56322(2) 0.62848(2) 0.86264(2) 0.03052(12) Uani 1 1 d . . Cl2 Cl 0.58287(9) 0.45576(13) 0.85625(12) 0.0422(4) Uani 1 1 d . . Cl1 Cl 0.57270(11) 0.79784(14) 0.89843(14) 0.0538(5) Uani 1 1 d . . O1 O 0.4480(2) 0.6324(3) 0.7908(3) 0.0316(10) Uani 1 1 d . . O2 O 0.4549(2) 0.6033(3) 0.4993(3) 0.0402(13) Uani 1 1 d . . N2 N 0.3316(3) 0.6241(4) 0.5057(4) 0.0334(13) Uani 1 1 d . . N1 N 0.3265(3) 0.6416(4) 0.6682(3) 0.0324(13) Uani 1 1 d . . N4 N 0.4230(3) 0.5900(4) 0.3513(4) 0.0523(18) Uani 1 1 d . . H4A H 0.4646 0.5834 0.3495 0.063 Uiso 1 1 calc R U H4B H 0.3903 0.5892 0.3030 0.063 Uiso 1 1 calc R U N3 N 0.3425(3) 0.6111(4) 0.4249(4) 0.0491(17) Uani 1 1 d . . H3 H 0.3098 0.6091 0.3766 0.059 Uiso 1 1 calc R U C9 C 0.2666(3) 0.6459(5) 0.6045(5) 0.0408(18) Uani 1 1 d . . C1 C 0.3907(3) 0.6380(5) 0.8196(5) 0.0353(16) Uani 1 1 d . . C5 C 0.3262(3) 0.6441(5) 0.7546(5) 0.0364(17) Uani 1 1 d . . C11 C 0.4097(3) 0.6013(5) 0.4269(5) 0.0372(17) Uani 1 1 d . . N5 N 0.2395(3) 0.5993(5) 0.2618(5) 0.0553(19) Uani 1 1 d . . C10 C 0.2720(3) 0.6344(5) 0.5156(5) 0.0438(19) Uani 1 1 d . . H10 H 0.2334 0.6346 0.4672 0.053 Uiso 1 1 calc R U C2 C 0.3900(4) 0.6364(5) 0.9059(5) 0.048(2) Uani 1 1 d . . H2 H 0.4311 0.6297 0.9497 0.058 Uiso 1 1 calc R U C6 C 0.2641(4) 0.6527(5) 0.7791(5) 0.0445(19) Uani 1 1 d . . C3 C 0.3301(4) 0.6445(6) 0.9307(5) 0.061(3) Uani 1 1 d . . H3A H 0.3325 0.6436 0.9907 0.073 Uiso 1 1 calc R U C4 C 0.2670(4) 0.6538(7) 0.8700(5) 0.060(3) Uani 1 1 d . . H4 H 0.2276 0.6605 0.8883 0.072 Uiso 1 1 calc R U N6 N -0.0046(6) 0.6781(8) 0.9012(7) 0.110(4) Uani 1 1 d . . H6 H -0.0304 0.7156 0.9182 0.132 Uiso 1 1 calc R U C8 C 0.2038(4) 0.6577(7) 0.6244(5) 0.064(3) Uani 1 1 d . . H8 H 0.1633 0.6628 0.5793 0.077 Uiso 1 1 calc R U C7 C 0.2033(4) 0.6616(7) 0.7100(5) 0.061(3) Uani 1 1 d . . H7 H 0.1621 0.6704 0.7237 0.073 Uiso 1 1 calc DR U C17 C 0.0484(6) 0.7064(8) 0.8696(8) 0.095(4) Uani 1 1 d . . H17 H 0.0536 0.7674 0.8635 0.114 Uiso 1 1 calc R U C16 C 0.1764(5) 0.6200(7) 0.2590(7) 0.070(3) Uani 1 1 d . . H16 H 0.1669 0.6289 0.3130 0.085 Uiso 1 1 calc R U C18 C 0.0893(7) 0.6567(11) 0.8489(9) 0.096(5) Uani 1 1 d . . H18 H 0.1268 0.6805 0.8338 0.115 Uiso 1 1 calc DR U C15 C 0.1238(5) 0.6296(7) 0.1856(8) 0.082(3) Uani 1 1 d . . H15 H 0.0803 0.6445 0.1893 0.098 Uiso 1 1 calc R U C21 C -0.0147(6) 0.5908(9) 0.9047(8) 0.091(4) Uani 1 1 d . . H21 H -0.0507 0.5678 0.9238 0.109 Uiso 1 1 calc R U C20 C 0.0300(8) 0.5370(7) 0.8790(10) 0.116(5) Uani 1 1 d . . H20 H 0.0269 0.4753 0.8817 0.140 Uiso 1 1 calc R U C14 C 0.1360(6) 0.6174(8) 0.1088(8) 0.101(4) Uani 1 1 d . . H14 H 0.1010 0.6248 0.0569 0.121 Uiso 1 1 calc R U C13 C 0.2000(6) 0.5937(9) 0.1046(7) 0.101(4) Uani 1 1 d . . H13 H 0.2094 0.5840 0.0507 0.121 Uiso 1 1 calc R U C12 C 0.2502(5) 0.5849(8) 0.1842(7) 0.088(4) Uani 1 1 d . . H12 H 0.2938 0.5680 0.1826 0.105 Uiso 1 1 calc R U C19 C 0.0812(8) 0.5783(15) 0.8481(10) 0.131(7) Uani 1 1 d . . H19 H 0.1100 0.5425 0.8260 0.157 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy01 0.02265(17) 0.0458(2) 0.02120(17) -0.00056(16) 0.00285(11) -0.00096(17) Cl2 0.0428(10) 0.0467(11) 0.0380(11) 0.0034(9) 0.0127(8) 0.0027(9) Cl1 0.0594(12) 0.0494(12) 0.0528(13) -0.0058(11) 0.0155(10) -0.0012(11) O1 0.025(2) 0.047(3) 0.022(2) -0.001(2) 0.0047(18) -0.001(2) O2 0.028(2) 0.068(4) 0.026(3) -0.007(2) 0.010(2) 0.003(3) N2 0.031(3) 0.044(3) 0.025(3) 0.001(3) 0.006(2) 0.004(3) N1 0.025(3) 0.050(4) 0.019(3) 0.002(3) 0.000(2) 0.001(3) N4 0.045(4) 0.085(5) 0.027(4) -0.007(4) 0.009(3) 0.007(4) N3 0.041(3) 0.081(5) 0.024(3) -0.005(3) 0.007(3) -0.009(4) C9 0.025(3) 0.065(5) 0.031(4) 0.002(4) 0.006(3) 0.001(4) C1 0.033(3) 0.045(4) 0.029(4) 0.001(3) 0.010(3) 0.002(4) C5 0.026(3) 0.050(5) 0.036(4) 0.001(3) 0.013(3) 0.001(3) C11 0.034(4) 0.045(4) 0.032(4) 0.001(3) 0.008(3) 0.002(3) N5 0.046(4) 0.073(5) 0.041(4) -0.001(4) 0.001(3) 0.013(4) C10 0.024(3) 0.078(6) 0.023(4) 0.012(4) -0.004(3) 0.000(4) C2 0.032(4) 0.083(6) 0.027(4) 0.008(4) 0.005(3) 0.006(4) C6 0.034(4) 0.067(5) 0.032(4) 0.008(4) 0.007(3) 0.004(4) C3 0.038(4) 0.112(8) 0.033(5) 0.007(5) 0.012(3) 0.009(5) C4 0.036(4) 0.114(8) 0.035(5) 0.008(5) 0.018(3) 0.007(5) N6 0.107(8) 0.113(9) 0.113(9) 0.011(7) 0.036(7) 0.052(8) C8 0.021(3) 0.133(9) 0.036(5) 0.013(5) 0.002(3) 0.010(5) C7 0.027(4) 0.119(8) 0.037(5) 0.011(5) 0.009(3) 0.014(5) C17 0.079(8) 0.081(9) 0.119(11) 0.036(8) 0.017(8) -0.023(7) C16 0.053(5) 0.091(8) 0.066(7) -0.005(6) 0.016(5) 0.002(6) C18 0.062(8) 0.122(12) 0.126(12) -0.013(10) 0.061(8) -0.020(9) C15 0.045(5) 0.102(9) 0.083(9) -0.007(8) -0.007(5) 0.009(6) C21 0.062(7) 0.082(8) 0.122(11) 0.030(8) 0.016(7) -0.018(7) C20 0.141(12) 0.035(6) 0.139(14) -0.013(7) -0.019(10) 0.026(8) C14 0.079(8) 0.116(10) 0.070(9) 0.022(8) -0.042(6) -0.008(8) C13 0.086(8) 0.163(13) 0.041(7) 0.009(7) -0.004(5) 0.001(9) C12 0.054(6) 0.143(11) 0.067(8) -0.017(7) 0.019(5) 0.012(7) C19 0.087(11) 0.20(2) 0.107(12) -0.056(14) 0.033(9) 0.038(14) 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' Cl Cl 0.1484 0.1585 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 Dy01 O2 93.37(15) . 2_656 O1 Dy01 O1 72.58(16) . 2_656 O2 Dy01 O1 163.80(16) 2_656 2_656 O1 Dy01 N1 140.42(16) . 2_656 O2 Dy01 N1 126.21(17) 2_656 2_656 O1 Dy01 N1 68.21(16) 2_656 2_656 O1 Dy01 N2 156.36(16) . 2_656 O2 Dy01 N2 63.30(16) 2_656 2_656 O1 Dy01 N2 131.06(16) 2_656 2_656 N1 Dy01 N2 63.03(17) 2_656 2_656 O1 Dy01 Cl1 94.89(12) . . O2 Dy01 Cl1 88.79(14) 2_656 . O1 Dy01 Cl1 100.19(12) 2_656 . N1 Dy01 Cl1 86.93(14) 2_656 . N2 Dy01 Cl1 81.55(14) 2_656 . O1 Dy01 Cl2 98.72(12) . . O2 Dy01 Cl2 86.57(14) 2_656 . O1 Dy01 Cl2 87.64(12) 2_656 . N1 Dy01 Cl2 85.06(14) 2_656 . N2 Dy01 Cl2 84.42(13) 2_656 . Cl1 Dy01 Cl2 165.85(7) . . O1 Dy01 Dy01 36.82(10) . 2_656 O2 Dy01 Dy01 129.34(11) 2_656 2_656 O1 Dy01 Dy01 35.83(10) 2_656 2_656 N1 Dy01 Dy01 104.01(12) 2_656 2_656 N2 Dy01 Dy01 166.77(12) 2_656 2_656 Cl1 Dy01 Dy01 101.21(5) . 2_656 Cl2 Dy01 Dy01 92.05(4) . 2_656 C1 O1 Dy01 133.3(4) . . C1 O1 Dy01 119.3(4) . 2_656 Dy01 O1 Dy01 107.34(16) . 2_656 C11 O2 Dy01 125.8(4) . 2_656 C10 N2 N3 122.3(6) . . C10 N2 Dy01 121.1(4) . 2_656 N3 N2 Dy01 116.6(4) . 2_656 C9 N1 C5 119.2(6) . . C9 N1 Dy01 123.5(4) . 2_656 C5 N1 Dy01 117.3(4) . 2_656 C11 N4 H4A 120.0 . . C11 N4 H4B 120.0 . . H4A N4 H4B 120.0 . . N2 N3 C11 114.3(6) . . N2 N3 H3 122.8 . . C11 N3 H3 122.8 . . N1 C9 C8 122.1(7) . . N1 C9 C10 114.7(6) . . C8 C9 C10 123.1(6) . . C2 C1 O1 125.1(6) . . C2 C1 C5 117.1(6) . . O1 C1 C5 117.8(6) . . N1 C5 C6 121.4(6) . . N1 C5 C1 117.3(6) . . C6 C5 C1 121.4(7) . . O2 C11 N4 123.2(7) . . O2 C11 N3 120.0(6) . . N4 C11 N3 116.9(7) . . C16 N5 C12 114.8(8) . . N2 C10 C9 117.5(6) . . N2 C10 H10 121.3 . . C9 C10 H10 121.3 . . C1 C2 C3 122.1(7) . . C1 C2 H2 118.9 . . C3 C2 H2 118.9 . . C7 C6 C4 124.1(7) . . C7 C6 C5 117.1(7) . . C4 C6 C5 118.8(7) . . C4 C3 C2 122.6(7) . . C4 C3 H3A 118.7 . . C2 C3 H3A 118.7 . . C3 C4 C6 118.0(7) . . C3 C4 H4 121.0 . . C6 C4 H4 121.0 . . C21 N6 C17 117.7(10) . . C21 N6 H6 121.1 . . C17 N6 H6 121.1 . . C7 C8 C9 118.9(7) . . C7 C8 H8 120.6 . . C9 C8 H8 120.6 . . C8 C7 C6 121.2(7) . . C8 C7 H7 119.4 . . C6 C7 H7 119.4 . . C18 C17 N6 124.5(12) . . C18 C17 H17 117.7 . . N6 C17 H17 117.7 . . N5 C16 C15 126.4(10) . . N5 C16 H16 116.8 . . C15 C16 H16 116.8 . . C19 C18 C17 120.1(14) . . C19 C18 H18 119.9 . . C17 C18 H18 119.9 . . C14 C15 C16 117.8(10) . . C14 C15 H15 121.1 . . C16 C15 H15 121.1 . . N6 C21 C20 116.8(11) . . N6 C21 H21 121.6 . . C20 C21 H21 121.6 . . C21 C20 C19 117.4(11) . . C21 C20 H20 121.3 . . C19 C20 H20 121.3 . . C15 C14 C13 120.3(10) . . C15 C14 H14 119.8 . . C13 C14 H14 119.8 . . C14 C13 C12 117.1(10) . . C14 C13 H13 121.4 . . C12 C13 H13 121.4 . . N5 C12 C13 123.5(10) . . N5 C12 H12 118.2 . . C13 C12 H12 118.2 . . C18 C19 C20 123.1(14) . . C18 C19 H19 118.5 . . C20 C19 H19 118.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy01 O1 2.304(4) . Dy01 O2 2.329(4) 2_656 Dy01 O1 2.359(4) 2_656 Dy01 N1 2.429(5) 2_656 Dy01 N2 2.532(5) 2_656 Dy01 Cl1 2.599(2) . Dy01 Cl2 2.6291(19) . Dy01 Dy01 3.7564(6) 2_656 O1 C1 1.364(7) . O1 Dy01 2.359(4) 2_656 O2 C11 1.250(8) . O2 Dy01 2.329(4) 2_656 N2 C10 1.272(8) . N2 N3 1.362(8) . N2 Dy01 2.532(5) 2_656 N1 C9 1.347(8) . N1 C5 1.359(8) . N1 Dy01 2.429(5) 2_656 N4 C11 1.301(9) . N4 H4A 0.8600 . N4 H4B 0.8600 . N3 C11 1.366(9) . N3 H3 0.8600 . C9 C8 1.408(9) . C9 C10 1.442(10) . C1 C2 1.360(9) . C1 C5 1.425(9) . C5 C6 1.425(9) . N5 C16 1.309(10) . N5 C12 1.313(11) . C10 H10 0.9300 . C2 C3 1.381(10) . C2 H2 0.9300 . C6 C7 1.409(10) . C6 C4 1.413(10) . C3 C4 1.379(11) . C3 H3A 0.9300 . C4 H4 0.9300 . N6 C21 1.330(14) . N6 C17 1.371(13) . N6 H6 0.8600 . C8 C7 1.348(11) . C8 H8 0.9300 . C7 H7 0.9300 . C17 C18 1.227(15) . C17 H17 0.9300 . C16 C15 1.345(13) . C16 H16 0.9300 . C18 C19 1.19(2) . C18 H18 0.9300 . C15 C14 1.309(15) . C15 H15 0.9300 . C21 C20 1.358(15) . C21 H21 0.9300 . C20 C19 1.41(2) . C20 H20 0.9300 . C14 C13 1.367(16) . C14 H14 0.9300 . C13 C12 1.384(13) . C13 H13 0.9300 . C12 H12 0.9300 . C19 H19 0.9300 .