#------------------------------------------------------------------------------ #$Date: 2019-03-09 02:06:39 +0200 (Sat, 09 Mar 2019) $ #$Revision: 214057 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/92/7049255.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_7049255 loop_ _publ_author_name 'Yang, zhaofu zhao' 'Tian, Yong-Mei' 'Zhang, Wan-Ying' 'Chen, Gu' 'Li, Hongfeng' 'Zhang, Yi-Quan' 'Sun, Wenbin' _publ_section_title ; Besides high local coordination symmetry around the spin center the alignment between magnetic and symmetric axes plays a crucial role in single-molecule magnet performance ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT00058E _journal_year 2019 _chemical_formula_sum 'C38 H30 Cl4 Dy2 N8 O4' _chemical_formula_weight 1129.50 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -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 99.014(5) _cell_angle_beta 104.323(5) _cell_angle_gamma 98.006(5) _cell_formula_units_Z 1 _cell_length_a 9.0284(6) _cell_length_b 10.4527(7) _cell_length_c 11.2508(7) _cell_measurement_reflns_used 4155 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.9618 _cell_measurement_theta_min 3.0262 _cell_volume 998.30(12) _computing_cell_refinement 'CrysAlis PRO (Agilent, 2011)' _computing_data_collection 'CrysAlis PRO (Agilent, 2011)' _computing_data_reduction 'CrysAlis PRO (Agilent, 2011)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.835 _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_unetI/netI 0.0598 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.835 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7869 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.835 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 29.026 _diffrn_reflns_theta_min 3.032 _exptl_absorpt_coefficient_mu 4.032 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.64832 _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 red _exptl_crystal_density_diffrn 1.879 _exptl_crystal_description block _exptl_crystal_F_000 546 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.987 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.123 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 4464 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0330 _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^)+(0.0215P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.0698 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3897 _reflns_number_total 4464 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt00058e2.cif _cod_data_source_block 3 _cod_original_cell_volume 998.31(11) _cod_database_code 7049255 _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 ; 1.res created by SHELXL-2014/7 TITL CF solution in P-1 CELL 0.71073 9.028434 10.45275 11.250752 99.014 104.3226 98.0057 ZERR 1 0.000556 0.000657 0.000684 0.0052 0.0053 0.0052 LATT 1 SFAC C H O N Dy Cl UNIT 38 30 4 8 2 4 L.S. 4 PLAN 5 BOND $H CONF HTAB fmap 2 acta 52 REM REM REM WGHT 0.021500 FVAR 3.05824 DY1 5 0.436882 0.422924 0.329406 11.00000 0.02401 0.03886 = 0.02375 0.00452 0.00894 -0.00253 CL1 6 0.523807 0.200419 0.354420 11.00000 0.05569 0.04311 = 0.05479 0.01357 0.00944 0.00583 O1 3 0.190937 0.305278 0.202487 11.00000 0.03591 0.06710 = 0.02797 -0.00371 0.01143 -0.01294 C16 1 -0.255802 0.095830 0.030500 11.00000 0.03814 0.05406 = 0.06903 0.01266 0.01367 -0.00468 AFIX 43 H16 2 -0.325795 0.080568 0.077300 11.00000 -1.20000 AFIX 0 C7 1 0.932828 0.542797 0.184878 11.00000 0.03412 0.04771 = 0.04278 0.01357 0.02294 0.00752 AFIX 43 H7 2 1.022567 0.563882 0.160019 11.00000 -1.20000 AFIX 0 N1 4 0.665993 0.473914 0.256991 11.00000 0.02818 0.03093 = 0.02739 0.00853 0.01147 0.00388 N3 4 0.270632 0.264774 0.030634 11.00000 0.03565 0.03748 = 0.02666 -0.00002 0.00335 -0.00360 AFIX 43 H3 2 0.253720 0.230292 -0.047196 11.00000 -1.20000 AFIX 0 C6 1 0.933062 0.590162 0.310199 11.00000 0.02972 0.03964 = 0.03785 0.01352 0.01776 0.00378 N2 4 0.413523 0.334598 0.102095 11.00000 0.02645 0.04162 = 0.02524 0.00822 0.00740 0.00285 C5 1 0.793085 0.551102 0.342202 11.00000 0.02112 0.03129 = 0.03291 0.01036 0.01041 0.00364 C3 1 1.045903 0.707865 0.517598 11.00000 0.02873 0.06181 = 0.04573 -0.00287 0.01094 -0.01469 AFIX 43 H3A 2 1.130677 0.761119 0.578216 11.00000 -1.20000 AFIX 0 C4 1 1.060369 0.669960 0.402356 11.00000 0.02452 0.05686 = 0.04740 0.01294 0.01291 -0.00643 AFIX 43 H4 2 1.153387 0.696157 0.383757 11.00000 -1.20000 AFIX 0 C11 1 0.158243 0.253717 0.090492 11.00000 0.03153 0.03464 = 0.03545 0.00682 0.01116 0.00236 C9 1 0.671227 0.433270 0.139965 11.00000 0.02955 0.04224 = 0.03072 0.01233 0.01213 0.00759 C12 1 0.001441 0.181684 0.020620 11.00000 0.03097 0.03124 = 0.03890 0.00481 0.00484 0.00019 C1 1 0.780670 0.590742 0.464979 11.00000 0.02725 0.03726 = 0.03258 0.01077 0.01392 0.00187 C8 1 0.804474 0.467620 0.101119 11.00000 0.03281 0.05593 = 0.03194 0.00941 0.01718 0.00557 AFIX 43 H8 2 0.804649 0.439027 0.018613 11.00000 -1.20000 AFIX 0 C2 1 0.909373 0.671116 0.550975 11.00000 0.03363 0.06591 = 0.03452 0.00095 0.01037 -0.01119 AFIX 43 H2 2 0.905021 0.701126 0.632122 11.00000 -1.20000 AFIX 0 C17 1 -0.104669 0.159629 0.089524 11.00000 0.03737 0.05397 = 0.04510 0.00019 0.00677 -0.00834 AFIX 43 H17 2 -0.073617 0.188061 0.176008 11.00000 -1.20000 AFIX 0 C13 1 -0.046788 0.140617 -0.106136 11.00000 0.04192 0.05632 = 0.04490 0.00357 0.00817 0.00248 AFIX 43 H13 2 0.022646 0.155750 -0.153429 11.00000 -1.20000 AFIX 0 C15 1 -0.302332 0.055255 -0.096299 11.00000 0.03137 0.05171 = 0.07476 0.00259 -0.00020 -0.00698 AFIX 43 H15 2 -0.404399 0.013184 -0.136266 11.00000 -1.20000 AFIX 0 C10 1 0.527333 0.356171 0.055136 11.00000 0.03360 0.04040 = 0.02697 0.00487 0.01103 0.00522 AFIX 43 H10 2 0.518509 0.324260 -0.028741 11.00000 -1.20000 AFIX 0 O2 3 0.646189 0.549405 0.490951 11.00000 0.02669 0.04398 = 0.02575 0.00511 0.01218 -0.00347 C14 1 -0.198117 0.076629 -0.165024 11.00000 0.04713 0.07311 = 0.04939 -0.00033 -0.00686 -0.00599 AFIX 43 H14 2 -0.229501 0.047942 -0.251480 11.00000 -1.20000 AFIX 0 CL2 6 0.362403 0.628299 0.240250 11.00000 0.04697 0.05179 = 0.04211 0.01642 0.01981 0.01438 N4 4 0.276222 0.149005 -0.221412 11.00000 0.07493 0.09310 = 0.05553 0.00088 0.03120 0.00490 C18 1 0.295966 0.118591 -0.314255 11.00000 0.07774 0.05697 = 0.05081 0.01391 0.02782 0.01622 C19 1 0.326556 0.084465 -0.433775 11.00000 0.16586 0.08058 = 0.06786 0.03213 0.06729 0.05595 AFIX 137 H19A 2 0.249169 0.108839 -0.497159 11.00000 -1.50000 H19B 2 0.323259 -0.008815 -0.453449 11.00000 -1.50000 H19C 2 0.427639 0.130616 -0.430416 11.00000 -1.50000 AFIX 0 HKLF 4 REM CF solution in P-1 REM R1 = 0.0330 for 3897 Fo > 4sig(Fo) and 0.0415 for all 4464 data REM 254 parameters refined using 0 restraints END WGHT 0.0215 0.0000 REM Instructions for potential hydrogen bonds HTAB N3 N4 EQIV $1 -x+1, -y+1, -z HTAB C8 Cl2_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C2 O1_$2 HTAB C10 Cl2_$1 EQIV $3 -x+1, -y, -z HTAB C19 Cl1_$3 EQIV $4 x, y, z-1 HTAB C19 Cl1_$4 REM Highest difference peak 0.987, deepest hole -0.644, 1-sigma level 0.123 Q1 1 0.4821 0.3121 0.3302 11.00000 0.05 0.99 Q2 1 0.4025 0.5380 0.3174 11.00000 0.05 0.85 Q3 1 0.5191 0.3925 0.4059 11.00000 0.05 0.83 Q4 1 0.3624 0.4578 0.2517 11.00000 0.05 0.70 Q5 1 0.3625 0.3229 0.2610 11.00000 0.05 0.62 ; _shelx_res_checksum 55842 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 0.43688(2) 0.42292(2) 0.32941(2) 0.02948(8) Uani 1 1 d . . Cl1 Cl 0.52381(16) 0.20042(12) 0.35442(12) 0.0522(3) Uani 1 1 d . . O1 O 0.1909(4) 0.3053(3) 0.2025(3) 0.0469(9) Uani 1 1 d . . C16 C -0.2558(6) 0.0958(5) 0.0305(5) 0.0552(14) Uani 1 1 d . . H16 H -0.3258 0.0806 0.0773 0.066 Uiso 1 1 calc R U C7 C 0.9328(5) 0.5428(4) 0.1849(4) 0.0388(11) Uani 1 1 d . . H7 H 1.0226 0.5639 0.1600 0.047 Uiso 1 1 calc R U N1 N 0.6660(4) 0.4739(3) 0.2570(3) 0.0280(8) Uani 1 1 d . . N3 N 0.2706(4) 0.2648(3) 0.0306(3) 0.0360(9) Uani 1 1 d . . H3 H 0.2537 0.2303 -0.0472 0.043 Uiso 1 1 calc R U C6 C 0.9331(5) 0.5902(4) 0.3102(4) 0.0338(10) Uani 1 1 d . . N2 N 0.4135(4) 0.3346(3) 0.1021(3) 0.0312(8) Uani 1 1 d . . C5 C 0.7931(5) 0.5511(4) 0.3422(4) 0.0276(9) Uani 1 1 d . . C3 C 1.0459(5) 0.7079(5) 0.5176(4) 0.0492(14) Uani 1 1 d . . H3A H 1.1307 0.7611 0.5782 0.059 Uiso 1 1 calc R U C4 C 1.0604(5) 0.6700(5) 0.4024(4) 0.0435(12) Uani 1 1 d . . H4 H 1.1534 0.6962 0.3838 0.052 Uiso 1 1 calc R U C11 C 0.1582(5) 0.2537(4) 0.0905(4) 0.0339(10) Uani 1 1 d . . C9 C 0.6712(5) 0.4333(4) 0.1400(4) 0.0328(10) Uani 1 1 d . . C12 C 0.0014(5) 0.1817(4) 0.0206(4) 0.0354(10) Uani 1 1 d . . C1 C 0.7807(5) 0.5907(4) 0.4650(4) 0.0313(10) Uani 1 1 d . . C8 C 0.8045(5) 0.4676(5) 0.1011(4) 0.0389(11) Uani 1 1 d . . H8 H 0.8046 0.4390 0.0186 0.047 Uiso 1 1 calc R U C2 C 0.9094(5) 0.6711(5) 0.5510(4) 0.0476(13) Uani 1 1 d . . H2 H 0.9050 0.7011 0.6321 0.057 Uiso 1 1 calc R U C17 C -0.1047(6) 0.1596(5) 0.0895(5) 0.0491(13) Uani 1 1 d . . H17 H -0.0736 0.1881 0.1760 0.059 Uiso 1 1 calc R U C13 C -0.0468(6) 0.1406(5) -0.1061(4) 0.0498(13) Uani 1 1 d . . H13 H 0.0226 0.1557 -0.1534 0.060 Uiso 1 1 calc R U C15 C -0.3023(6) 0.0553(5) -0.0963(5) 0.0579(15) Uani 1 1 d . . H15 H -0.4044 0.0132 -0.1363 0.070 Uiso 1 1 calc R U C10 C 0.5273(5) 0.3562(4) 0.0551(4) 0.0335(10) Uani 1 1 d . . H10 H 0.5185 0.3243 -0.0287 0.040 Uiso 1 1 calc R U O2 O 0.6462(3) 0.5494(3) 0.4910(2) 0.0325(7) Uani 1 1 d . . C14 C -0.1981(6) 0.0766(6) -0.1650(5) 0.0634(17) Uani 1 1 d . . H14 H -0.2295 0.0479 -0.2515 0.076 Uiso 1 1 calc R U Cl2 Cl 0.36240(14) 0.62830(12) 0.24025(11) 0.0443(3) Uani 1 1 d . . N4 N 0.2762(6) 0.1490(5) -0.2214(4) 0.0748(16) Uani 1 1 d . . C18 C 0.2960(7) 0.1186(5) -0.3143(5) 0.0593(15) Uani 1 1 d . . C19 C 0.3266(9) 0.0845(6) -0.4338(6) 0.093(2) Uani 1 1 d . . H19A H 0.2492 0.1088 -0.4972 0.140 Uiso 1 1 calc R U H19B H 0.3233 -0.0088 -0.4534 0.140 Uiso 1 1 calc R U H19C H 0.4276 0.1306 -0.4304 0.140 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 0.02401(12) 0.03886(13) 0.02375(11) 0.00452(9) 0.00894(8) -0.00253(9) Cl1 0.0557(8) 0.0431(7) 0.0548(7) 0.0136(6) 0.0094(6) 0.0058(6) O1 0.036(2) 0.067(2) 0.0280(16) -0.0037(16) 0.0114(14) -0.0129(17) C16 0.038(3) 0.054(3) 0.069(4) 0.013(3) 0.014(3) -0.005(3) C7 0.034(3) 0.048(3) 0.043(2) 0.014(2) 0.023(2) 0.008(2) N1 0.0282(19) 0.0309(18) 0.0274(17) 0.0085(15) 0.0115(15) 0.0039(15) N3 0.036(2) 0.037(2) 0.0267(17) 0.0000(16) 0.0033(16) -0.0036(17) C6 0.030(2) 0.040(2) 0.038(2) 0.014(2) 0.0178(19) 0.0038(19) N2 0.026(2) 0.042(2) 0.0252(17) 0.0082(16) 0.0074(15) 0.0029(16) C5 0.021(2) 0.031(2) 0.033(2) 0.0104(18) 0.0104(17) 0.0036(17) C3 0.029(3) 0.062(3) 0.046(3) -0.003(3) 0.011(2) -0.015(2) C4 0.025(3) 0.057(3) 0.047(3) 0.013(2) 0.013(2) -0.006(2) C11 0.032(3) 0.035(2) 0.035(2) 0.007(2) 0.0112(19) 0.0024(19) C9 0.030(2) 0.042(3) 0.031(2) 0.012(2) 0.0121(18) 0.0076(19) C12 0.031(3) 0.031(2) 0.039(2) 0.005(2) 0.0048(19) 0.0002(19) C1 0.027(2) 0.037(2) 0.033(2) 0.011(2) 0.0139(18) 0.0019(19) C8 0.033(3) 0.056(3) 0.032(2) 0.009(2) 0.017(2) 0.006(2) C2 0.034(3) 0.066(3) 0.035(2) 0.001(2) 0.010(2) -0.011(2) C17 0.037(3) 0.054(3) 0.045(3) 0.000(2) 0.007(2) -0.008(2) C13 0.042(3) 0.056(3) 0.045(3) 0.004(3) 0.008(2) 0.002(3) C15 0.031(3) 0.052(3) 0.075(4) 0.003(3) 0.000(3) -0.007(2) C10 0.034(3) 0.040(2) 0.027(2) 0.0049(19) 0.0110(18) 0.005(2) O2 0.0267(16) 0.0440(18) 0.0258(14) 0.0051(13) 0.0122(12) -0.0035(13) C14 0.047(4) 0.073(4) 0.049(3) 0.000(3) -0.007(3) -0.006(3) Cl2 0.0470(7) 0.0518(7) 0.0421(6) 0.0164(6) 0.0198(5) 0.0144(6) N4 0.075(4) 0.093(4) 0.056(3) 0.001(3) 0.031(3) 0.005(3) C18 0.078(4) 0.057(3) 0.051(3) 0.014(3) 0.028(3) 0.016(3) C19 0.166(8) 0.081(5) 0.068(4) 0.032(4) 0.067(5) 0.056(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' O O 0.0106 0.0060 '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' Dy Dy -0.1892 4.4098 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O2 Dy1 O2 72.91(10) 2_666 . O2 Dy1 O1 93.31(10) 2_666 . O2 Dy1 O1 165.98(10) . . O2 Dy1 N1 141.38(10) 2_666 . O2 Dy1 N1 68.52(10) . . O1 Dy1 N1 125.32(10) . . O2 Dy1 N2 155.68(10) 2_666 . O2 Dy1 N2 131.34(10) . . O1 Dy1 N2 62.55(10) . . N1 Dy1 N2 62.82(10) . . O2 Dy1 Cl1 95.59(8) 2_666 . O2 Dy1 Cl1 94.67(8) . . O1 Dy1 Cl1 89.10(9) . . N1 Dy1 Cl1 85.80(8) . . N2 Dy1 Cl1 81.96(9) . . O2 Dy1 Cl2 100.83(8) 2_666 . O2 Dy1 Cl2 93.09(8) . . O1 Dy1 Cl2 86.91(9) . . N1 Dy1 Cl2 83.31(8) . . N2 Dy1 Cl2 81.81(8) . . Cl1 Dy1 Cl2 163.30(4) . . O2 Dy1 Dy1 36.68(6) 2_666 2_666 O2 Dy1 Dy1 36.23(6) . 2_666 O1 Dy1 Dy1 129.94(7) . 2_666 N1 Dy1 Dy1 104.73(8) . 2_666 N2 Dy1 Dy1 167.48(8) . 2_666 Cl1 Dy1 Dy1 96.37(3) . 2_666 Cl2 Dy1 Dy1 98.62(3) . 2_666 C11 O1 Dy1 126.6(3) . . C15 C16 C17 120.0(5) . . C15 C16 H16 120.0 . . C17 C16 H16 120.0 . . C8 C7 C6 121.1(4) . . C8 C7 H7 119.5 . . C6 C7 H7 119.5 . . C9 N1 C5 119.7(3) . . C9 N1 Dy1 123.8(3) . . C5 N1 Dy1 116.5(2) . . C11 N3 N2 115.7(3) . . C11 N3 H3 122.2 . . N2 N3 H3 122.2 . . C4 C6 C7 124.7(4) . . C4 C6 C5 119.0(4) . . C7 C6 C5 116.3(4) . . C10 N2 N3 121.6(3) . . C10 N2 Dy1 121.9(3) . . N3 N2 Dy1 116.5(2) . . N1 C5 C1 117.1(3) . . N1 C5 C6 121.7(4) . . C1 C5 C6 121.2(4) . . C4 C3 C2 123.0(4) . . C4 C3 H3A 118.5 . . C2 C3 H3A 118.5 . . C3 C4 C6 118.9(4) . . C3 C4 H4 120.5 . . C6 C4 H4 120.5 . . O1 C11 N3 118.7(4) . . O1 C11 C12 122.1(4) . . N3 C11 C12 119.2(4) . . N1 C9 C8 122.1(4) . . N1 C9 C10 115.2(4) . . C8 C9 C10 122.6(4) . . C13 C12 C17 118.9(4) . . C13 C12 C11 124.2(4) . . C17 C12 C11 116.9(4) . . O2 C1 C2 124.2(4) . . O2 C1 C5 118.9(4) . . C2 C1 C5 116.9(4) . . C7 C8 C9 119.2(4) . . C7 C8 H8 120.4 . . C9 C8 H8 120.4 . . C1 C2 C3 120.8(4) . . C1 C2 H2 119.6 . . C3 C2 H2 119.6 . . C16 C17 C12 120.5(5) . . C16 C17 H17 119.8 . . C12 C17 H17 119.7 . . C12 C13 C14 120.5(5) . . C12 C13 H13 119.7 . . C14 C13 H13 119.7 . . C16 C15 C14 119.9(5) . . C16 C15 H15 120.1 . . C14 C15 H15 120.1 . . N2 C10 C9 116.2(4) . . N2 C10 H10 121.9 . . C9 C10 H10 121.9 . . C1 O2 Dy1 134.0(2) . 2_666 C1 O2 Dy1 118.9(2) . . Dy1 O2 Dy1 107.09(10) 2_666 . C15 C14 C13 120.3(5) . . C15 C14 H14 119.9 . . C13 C14 H14 119.9 . . N4 C18 C19 177.4(7) . . C18 C19 H19A 109.5 . . C18 C19 H19B 109.5 . . H19A C19 H19B 109.5 . . C18 C19 H19C 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy1 O2 2.315(3) 2_666 Dy1 O2 2.340(3) . Dy1 O1 2.367(3) . Dy1 N1 2.427(3) . Dy1 N2 2.525(3) . Dy1 Cl1 2.5901(13) . Dy1 Cl2 2.6096(12) . Dy1 Dy1 3.7438(4) 2_666 O1 C11 1.235(5) . C16 C15 1.362(7) . C16 C17 1.381(6) . C16 H16 0.9300 . C7 C8 1.350(6) . C7 C6 1.419(6) . C7 H7 0.9300 . N1 C9 1.333(5) . N1 C5 1.357(5) . N3 C11 1.351(5) . N3 N2 1.373(4) . N3 H3 0.8600 . C6 C4 1.401(6) . C6 C5 1.422(5) . N2 C10 1.276(5) . C5 C1 1.415(6) . C3 C4 1.339(6) . C3 C2 1.397(6) . C3 H3A 0.9300 . C4 H4 0.9300 . C11 C12 1.468(6) . C9 C8 1.399(6) . C9 C10 1.450(6) . C12 C13 1.363(6) . C12 C17 1.391(6) . C1 O2 1.347(4) . C1 C2 1.382(6) . C8 H8 0.9300 . C2 H2 0.9300 . C17 H17 0.9300 . C13 C14 1.383(6) . C13 H13 0.9300 . C15 C14 1.374(8) . C15 H15 0.9300 . C10 H10 0.9300 . O2 Dy1 2.315(3) 2_666 C14 H14 0.9300 . N4 C18 1.108(7) . C18 C19 1.440(8) . C19 H19A 0.9600 . C19 H19B 0.9600 . C19 H19C 0.9600 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_4 C8 C7 C6 C4 -179.1(5) . C8 C7 C6 C5 1.6(7) . C11 N3 N2 C10 -177.3(4) . C11 N3 N2 Dy1 1.1(5) . C9 N1 C5 C1 -179.8(4) . Dy1 N1 C5 C1 1.7(5) . C9 N1 C5 C6 -0.1(6) . Dy1 N1 C5 C6 -178.6(3) . C4 C6 C5 N1 180.0(4) . C7 C6 C5 N1 -0.7(6) . C4 C6 C5 C1 -0.3(7) . C7 C6 C5 C1 179.0(4) . C2 C3 C4 C6 0.3(9) . C7 C6 C4 C3 -179.8(5) . C5 C6 C4 C3 -0.5(7) . Dy1 O1 C11 N3 -0.9(6) . Dy1 O1 C11 C12 179.5(3) . N2 N3 C11 O1 -0.3(6) . N2 N3 C11 C12 179.4(4) . C5 N1 C9 C8 0.0(7) . Dy1 N1 C9 C8 178.3(3) . C5 N1 C9 C10 -177.4(4) . Dy1 N1 C9 C10 0.9(5) . O1 C11 C12 C13 169.6(5) . N3 C11 C12 C13 -10.1(7) . O1 C11 C12 C17 -7.8(7) . N3 C11 C12 C17 172.5(4) . N1 C5 C1 O2 0.7(6) . C6 C5 C1 O2 -179.0(4) . N1 C5 C1 C2 -179.0(4) . C6 C5 C1 C2 1.4(7) . C6 C7 C8 C9 -1.7(7) . N1 C9 C8 C7 0.9(7) . C10 C9 C8 C7 178.2(4) . O2 C1 C2 C3 178.8(5) . C5 C1 C2 C3 -1.6(8) . C4 C3 C2 C1 0.8(9) . C15 C16 C17 C12 -0.7(9) . C13 C12 C17 C16 0.7(8) . C11 C12 C17 C16 178.2(5) . C17 C12 C13 C14 -0.8(8) . C11 C12 C13 C14 -178.1(5) . C17 C16 C15 C14 0.7(9) . N3 N2 C10 C9 178.9(4) . Dy1 N2 C10 C9 0.5(5) . N1 C9 C10 N2 -0.9(6) . C8 C9 C10 N2 -178.3(4) . C2 C1 O2 Dy1 -2.3(7) 2_666 C5 C1 O2 Dy1 178.1(3) 2_666 C2 C1 O2 Dy1 176.7(4) . C5 C1 O2 Dy1 -2.9(5) . C16 C15 C14 C13 -0.8(9) . C12 C13 C14 C15 0.9(9) .