#------------------------------------------------------------------------------ #$Date: 2019-12-13 11:40:20 +0200 (Fri, 13 Dec 2019) $ #$Revision: 245056 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556560.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_1556560 loop_ _publ_author_name 'Ishikawa, R.' 'Michiwaki, S.' 'Noda, T.' 'Katoh, K.' 'Yamashita, M.' 'Matsubara, K.' 'Kawata, S.' _publ_section_title ; Field-Induced Slow Magnetic Relaxation of Mono- and Dinuclear Dysprosium(III) Complexes Coordinated by a Chloranilate with Different Resonance Forms ; _journal_name_full Inorganics _journal_page_first 7 _journal_paper_doi 10.3390/inorganics6010007 _journal_volume 6 _journal_year 2018 _chemical_formula_moiety 'C44 H44 B4 Cl6 Dy2 N24 O4' _chemical_formula_sum 'C44 H44 B4 Cl6 Dy2 N24 O4' _chemical_formula_weight 1553.95 _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.0000 _cell_angle_beta 107.6590(13) _cell_angle_gamma 90.0000 _cell_formula_units_Z 2 _cell_length_a 13.9870(7) _cell_length_b 15.1052(9) _cell_length_c 14.8741(7) _cell_measurement_reflns_used 21100 _cell_measurement_temperature 163 _cell_measurement_theta_max 27.43 _cell_measurement_theta_min 3.06 _cell_volume 2994.5(3) _computing_cell_refinement 'RAPID AUTO' _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_data_reduction 'RAPID AUTO' _computing_molecular_graphics 'CrystalStructure 4.2.2' _computing_publication_material 'CrystalStructure 4.2.2 (Rigaku, 2016)' _computing_structure_refinement 'SHELXL Version 2014/7 (Sheldrick, 2008)' _computing_structure_solution 'SIR2011 (Burla, et al., 2012)' _diffrn_ambient_temperature 163 _diffrn_detector_area_resol_mean 10.000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 27868 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.441 _diffrn_reflns_theta_min 3.056 _diffrn_standards_interval_count . _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.810 _exptl_absorpt_correction_T_max 0.755 _exptl_absorpt_correction_T_min 0.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1524.00 _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _refine_diff_density_max 1.54 _refine_diff_density_min -0.83 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 379 _refine_ls_number_reflns 6808 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0388 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0233P)^2^+5.8559P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.0860 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5671 _reflns_number_total 6808 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file CrystalStructure_1.cif _cod_data_source_block 151201mcwkDy2 _cod_database_code 1556560 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL 151201mcwkDy2 CELL 0.71075 13.98700 15.10520 14.87410 90.00000 107.65900 90.00000 ZERR 2 0.00073 0.00085 0.00072 0.00000 0.00130 0.00000 LATT 1 SYMM .50-X, .50+Y, .50-Z SFAC C H B CL DY N O UNIT 88 88 8 12 4 48 8 L.S. 5 FMAP 2 PLAN 5 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -110.0 ACTA SIZE 0.600 0.150 0.100 WGHT 0.023300 5.855900 FVAR 0.28909 DY1 5 0.417430 0.130539 0.724916 11.00000 0.01854 0.01751 = 0.01551 -0.00164 0.00635 -0.00048 CL1 4 0.434543 0.170317 0.369454 11.00000 0.04463 0.02482 = 0.02775 0.00733 0.01833 0.01071 CL2 4 0.732022 0.163359 0.636348 11.00000 0.14085 0.12088 = 0.06105 0.02750 0.05690 0.03206 CL3 4 0.718922 0.339789 0.554227 11.00000 0.13847 0.06603 = 0.16438 -0.01886 0.11979 -0.01357 O1 7 0.428674 0.141722 0.569079 11.00000 0.03274 0.02010 = 0.02319 -0.00087 0.01387 0.00352 O2 7 0.472146 -0.002519 0.670395 11.00000 0.02679 0.02142 = 0.01866 -0.00145 0.01098 0.00131 N1 6 0.603672 0.113440 0.799881 11.00000 0.02299 0.02382 = 0.02237 -0.00204 0.00368 0.00105 N2 6 0.663116 0.182232 0.844975 11.00000 0.01912 0.03347 = 0.02264 -0.00019 0.00659 -0.00480 N3 6 0.483508 0.278199 0.705860 11.00000 0.02853 0.02271 = 0.02181 0.00042 0.00487 -0.00176 N4 6 0.563073 0.318011 0.770029 11.00000 0.02692 0.02243 = 0.02816 0.00057 0.00968 -0.00566 N5 6 0.465967 0.201181 0.886411 11.00000 0.02532 0.02285 = 0.02023 -0.00445 0.00710 -0.00363 N6 6 0.547147 0.254620 0.921389 11.00000 0.02671 0.02217 = 0.02104 -0.00494 0.00457 -0.00306 N7 6 0.270829 0.213553 0.739501 11.00000 0.02495 0.02361 = 0.02480 0.00003 0.00738 0.00220 N8 6 0.192441 0.171162 0.756655 11.00000 0.02094 0.02790 = 0.02288 0.00140 0.00862 0.00489 N9 6 0.363821 0.024381 0.822670 11.00000 0.02031 0.02016 = 0.01996 0.00237 0.00592 -0.00103 N10 6 0.268747 0.025470 0.829223 11.00000 0.02206 0.02188 = 0.02018 0.00149 0.00641 -0.00122 N11 6 0.258574 0.057094 0.620384 11.00000 0.02467 0.02444 = 0.01909 -0.00083 0.00442 0.00061 N12 6 0.182309 0.035964 0.656052 11.00000 0.02012 0.02416 = 0.02340 0.00319 0.00510 -0.00142 C1 1 0.488610 -0.005781 0.592008 11.00000 0.01665 0.02306 = 0.01828 0.00025 0.00328 -0.00303 C2 1 0.460658 0.077971 0.531245 11.00000 0.02168 0.01664 = 0.02162 -0.00311 0.00859 -0.00060 C3 1 0.470641 0.078444 0.441019 11.00000 0.02290 0.01984 = 0.01853 0.00250 0.00643 0.00094 C4 1 0.665186 0.043300 0.807827 11.00000 0.02771 0.02853 = 0.02896 -0.00153 0.00742 0.00532 AFIX 43 H4 2 0.644638 -0.014103 0.783473 11.00000 -1.20000 AFIX 0 C5 1 0.763850 0.067372 0.857233 11.00000 0.02776 0.03841 = 0.03072 0.00861 0.00822 0.00845 AFIX 43 H5 2 0.821770 0.030734 0.872616 11.00000 -1.20000 AFIX 0 C6 1 0.758825 0.155488 0.878687 11.00000 0.02059 0.04106 = 0.02767 0.00582 0.00861 -0.00377 AFIX 43 H6 2 0.813976 0.191436 0.911868 11.00000 -1.20000 AFIX 0 C7 1 0.453533 0.335315 0.633529 11.00000 0.03084 0.03028 = 0.02777 0.00412 0.01053 0.00064 AFIX 43 H7 2 0.399269 0.325208 0.577928 11.00000 -1.20000 AFIX 0 C8 1 0.512073 0.410600 0.650777 11.00000 0.03912 0.02945 = 0.04262 0.01356 0.01502 0.00078 AFIX 43 H8 2 0.505993 0.460946 0.611154 11.00000 -1.20000 AFIX 0 C9 1 0.581098 0.397016 0.737685 11.00000 0.03153 0.02996 = 0.04218 0.00157 0.01181 -0.00908 AFIX 43 H9 2 0.632834 0.436912 0.769436 11.00000 -1.20000 AFIX 0 C10 1 0.421265 0.197098 0.953680 11.00000 0.03039 0.02760 = 0.02359 -0.00277 0.01097 0.00179 AFIX 43 H10 2 0.361805 0.164558 0.948908 11.00000 -1.20000 AFIX 0 C11 1 0.473545 0.247043 1.032047 11.00000 0.04024 0.03096 = 0.02078 -0.00625 0.00927 0.00239 AFIX 43 H11 2 0.457726 0.254661 1.089329 11.00000 -1.20000 AFIX 0 C12 1 0.551968 0.282383 1.008569 11.00000 0.03282 0.02863 = 0.02160 -0.00619 0.00150 -0.00089 AFIX 43 H12 2 0.601855 0.320334 1.047207 11.00000 -1.20000 AFIX 0 C13 1 0.259089 0.299418 0.754435 11.00000 0.03718 0.02249 = 0.02653 0.00160 0.01146 0.00552 AFIX 43 H13 2 0.303427 0.344751 0.747552 11.00000 -1.20000 AFIX 0 C14 1 0.174159 0.313749 0.781171 11.00000 0.04582 0.02869 = 0.02969 0.00342 0.01406 0.01649 AFIX 43 H14 2 0.148869 0.368551 0.795601 11.00000 -1.20000 AFIX 0 C15 1 0.134622 0.230959 0.782165 11.00000 0.03322 0.03537 = 0.02998 0.00621 0.01422 0.01332 AFIX 43 H15 2 0.075481 0.217898 0.798387 11.00000 -1.20000 AFIX 0 C16 1 0.417573 -0.025638 0.894791 11.00000 0.02492 0.02695 = 0.02576 0.00110 0.00573 0.00306 AFIX 43 H16 2 0.486786 -0.038679 0.906937 11.00000 -1.20000 AFIX 0 C17 1 0.360413 -0.055732 0.948979 11.00000 0.03316 0.02861 = 0.02040 0.00465 0.00524 -0.00043 AFIX 43 H17 2 0.381044 -0.091694 1.003893 11.00000 -1.20000 AFIX 0 C18 1 0.265858 -0.021644 0.905221 11.00000 0.03067 0.02639 = 0.02256 0.00158 0.01043 -0.00449 AFIX 43 H18 2 0.208305 -0.030101 0.925491 11.00000 -1.20000 AFIX 0 C19 1 0.235292 0.016842 0.535653 11.00000 0.03002 0.03044 = 0.02218 -0.00539 0.00126 0.00238 AFIX 43 H19 2 0.274497 0.020474 0.493623 11.00000 -1.20000 AFIX 0 C20 1 0.146477 -0.030653 0.517810 11.00000 0.03041 0.03363 = 0.02840 -0.00738 -0.00124 -0.00199 AFIX 43 H20 2 0.114289 -0.065168 0.463697 11.00000 -1.20000 AFIX 0 C21 1 0.115718 -0.016606 0.595608 11.00000 0.02270 0.02683 = 0.03304 0.00182 0.00065 -0.00381 AFIX 43 H21 2 0.056676 -0.040285 0.605264 11.00000 -1.20000 AFIX 0 C22 1 0.683113 0.232050 0.541163 11.00000 0.13380 0.08842 = 0.07021 0.01767 -0.00479 -0.05390 AFIX 23 H22A 2 0.701517 0.207654 0.486879 11.00000 -1.20000 H22B 2 0.609049 0.229936 0.524635 11.00000 -1.20000 AFIX 0 B1 3 0.620079 0.272181 0.863908 11.00000 0.02716 0.02408 = 0.02574 -0.00268 0.00477 -0.00512 AFIX 13 H1 2 0.675968 0.311207 0.900858 11.00000 -1.20000 AFIX 0 B2 3 0.181158 0.069361 0.753187 11.00000 0.01933 0.02726 = 0.02496 0.00426 0.00813 0.00040 AFIX 13 H2 2 0.116199 0.052673 0.763722 11.00000 -1.20000 AFIX 0 HKLF 4 REM 151201mcwkDy2 REM R1 = 0.0388 for 5671 Fo > 4sig(Fo) and 0.0477 for all 6808 data REM 379 parameters refined using 0 restraints END WGHT 0.0229 5.8714 REM Instructions for potential hydrogen bonds EQIV $1 x+1/2, -y+1/2, z+1/2 HTAB C6 Cl1_$1 EQIV $2 x-1/2, -y+1/2, z+1/2 HTAB C10 Cl3_$2 HTAB C22 Cl1 REM Highest difference peak 1.537, deepest hole -0.826, 1-sigma level 0.148 Q1 1 0.4196 0.1280 0.6678 11.00000 0.05 1.54 Q2 1 0.4596 0.0873 0.7212 11.00000 0.05 1.53 Q3 1 0.4210 0.1303 0.7799 11.00000 0.05 1.51 Q4 1 0.4574 0.1725 0.7229 11.00000 0.05 1.49 Q5 1 0.3752 0.0888 0.7274 11.00000 0.05 1.26 ; _shelx_res_checksum 42860 _shelx_hkl_file ; 0 -2 1 7827.41 765.74 0 2 1 7343.97 671.19 0 -2 -1 7432.34 711.35 0 2 -1 7152.06 691.74 -2 0 0 446.56 17.01 -1 -2 0 1961.41 116.58 1 -2 0 1870.14 105.74 1 2 0 1936.22 99.17 -1 2 0 1813.29 99.81 1 1 -2 2438.87 140.66 1 1 -2 2617.63 144.07 1 -1 -2 2506.86 159.21 -1 1 2 2435.44 135.67 -1 -1 2 2543.44 160.54 0 -1 2 34.02 4.86 0 -1 -2 36.94 5.44 0 1 -2 38.73 5.08 0 1 2 38.35 3.09 0 1 2 38.79 7.42 0 -1 -2 42.97 3.70 0 1 -2 39.60 5.36 -1 2 1 91.81 7.26 -1 -2 1 101.02 7.73 1 -2 -1 95.97 15.57 1 2 -1 100.05 6.41 2 1 -1 198.13 9.27 -2 -1 1 196.15 10.61 -2 -1 1 187.91 8.02 -2 1 1 189.32 10.97 2 -1 -1 185.80 21.00 2 1 0 290.06 19.00 -2 1 0 291.85 15.24 -2 -1 0 298.70 20.52 -2 -1 0 306.65 12.63 2 -1 0 303.66 25.34 2 1 0 307.90 11.55 -2 0 2 0.90 2.97 1 -2 1 745.08 40.24 1 2 1 779.48 30.47 -1 2 -1 747.01 53.47 1 2 1 763.26 36.47 -1 -2 -1 827.81 42.35 -1 0 -2 1.95 4.19 1 0 2 1.87 2.42 1 0 2 0.95 3.54 -2 0 -1 3.57 4.47 -2 0 -1 3.10 2.29 2 0 1 1.36 3.86 -2 1 2 1121.45 79.15 -2 -1 2 1121.28 76.27 2 1 -2 1171.57 59.52 2 -1 -2 1183.75 66.96 -2 -1 2 1405.81 49.99 1 -1 2 127.86 13.44 -1 -1 -2 136.04 12.98 -1 1 -2 130.12 12.37 1 1 2 128.46 19.48 -1 1 -2 73.15 14.40 1 1 2 135.42 3.76 -1 2 2 1341.32 71.22 1 2 -2 1284.02 67.42 -1 -2 2 1348.57 90.89 1 -2 -2 1400.09 75.62 0 -2 -2 166.65 9.79 0 2 2 161.85 12.79 0 -2 2 166.00 20.57 0 2 2 164.78 14.29 0 2 -2 175.43 17.58 2 1 1 4022.56 301.78 -2 -1 -1 4017.26 302.07 -2 -1 -1 4168.63 292.42 2 -1 1 3918.96 317.38 -2 1 -1 3904.13 285.41 -2 2 1 428.30 42.91 2 2 -1 411.04 19.68 2 -2 -1 408.29 28.80 2 2 -1 397.88 19.53 -2 -2 1 409.49 22.02 0 -3 0 7.04 5.56 0 3 0 5.24 4.63 2 2 0 330.00 25.29 -2 2 0 317.94 22.89 2 -2 0 358.39 41.57 2 2 0 327.45 21.36 -2 -2 0 323.69 24.17 -2 -2 0 328.33 26.70 -1 0 3 158.06 12.59 -1 0 3 189.98 16.23 1 0 -3 164.04 8.00 1 0 -3 156.39 10.73 0 3 -1 9.76 5.40 0 3 1 10.71 8.97 0 -3 -1 13.13 10.16 0 -3 1 11.68 11.43 0 0 -3 4.47 2.43 0 0 3 2.59 2.89 0 0 -3 1.40 4.49 0 0 3 5.55 4.38 -1 -3 0 1941.50 141.04 1 -3 0 1903.00 125.27 1 3 0 1980.23 132.72 -1 3 0 1708.88 147.62 1 1 -3 4039.56 298.05 -1 -1 3 3675.18 274.62 -1 1 3 3557.14 265.66 -1 -1 3 3929.50 288.48 1 1 -3 3837.38 288.14 -1 1 3 3736.49 270.67 1 -3 -1 4375.12 353.74 -1 3 1 4206.23 337.73 -1 -3 1 4553.31 394.92 1 3 -1 4365.65 368.03 -2 2 2 175.53 16.11 2 -2 -2 171.40 16.51 2 2 -2 167.66 11.61 -2 -2 2 175.30 13.45 -2 0 3 4.93 5.16 -2 0 3 3.07 2.26 0 -1 3 5.45 4.15 0 1 -3 6.43 4.69 0 1 3 6.54 3.30 0 -1 3 6.36 5.16 0 1 -3 4.19 2.37 0 -1 -3 5.28 5.02 0 1 3 6.33 4.98 1 2 2 250.40 12.59 -1 -2 -2 240.40 14.25 -1 -2 -2 237.71 19.07 -1 2 -2 233.19 24.65 1 -2 2 236.76 17.14 1 2 2 245.63 18.88 -3 -1 1 3313.74 252.82 3 1 -1 3429.21 233.88 -3 -1 1 3273.46 233.41 3 -1 -1 3437.99 284.99 -3 1 1 3130.35 267.06 -3 0 0 2.36 6.46 -2 -2 -1 1545.27 82.02 -2 -2 -1 1393.32 104.34 2 2 1 1435.44 75.63 2 -2 1 1414.20 84.47 2 2 1 1379.60 102.32 -2 2 -1 1314.26 104.46 2 1 -3 250.64 13.33 2 1 -3 232.99 13.45 -2 1 3 213.97 15.04 -2 -1 3 233.86 14.46 1 -3 1 235.27 20.86 1 3 1 254.47 21.46 -1 -3 -1 245.34 14.81 -1 3 -1 229.38 18.94 -3 1 0 276.89 19.86 -3 -1 0 290.64 18.04 -3 -1 0 290.91 14.22 3 1 0 332.70 20.82 3 -1 0 287.99 32.86 2 0 2 90.08 8.14 -2 0 -2 109.42 13.82 -2 0 -2 94.73 8.66 2 0 2 116.63 24.44 -3 1 2 200.25 19.16 -3 -1 2 202.53 15.38 3 1 -2 311.33 17.24 1 2 -3 1693.25 96.78 -1 -2 3 1884.18 129.85 1 -2 -3 1774.39 118.84 -1 2 3 1783.09 99.27 -1 -3 2 786.73 67.87 1 3 -2 850.90 60.13 1 -3 -2 848.33 48.69 -1 3 2 775.42 64.27 0 -3 -2 915.96 47.36 0 3 2 918.31 46.72 0 3 -2 995.01 73.82 0 -3 2 918.37 80.67 2 -1 2 69.84 11.42 2 1 2 56.04 10.51 -1 0 -311444.97 1336.96 1 0 312753.96 1594.14 -1 0 -312894.81 1608.12 1 0 312927.79 1518.21 2 3 -1 616.95 42.97 -2 -3 1 584.63 47.33 -2 3 1 571.21 41.12 2 -3 -1 625.13 42.36 2 -3 0 2510.37 140.64 2 3 0 1579.80 103.28 2 3 0 1484.26 82.86 -2 -3 0 1604.03 109.20 -2 3 0 1563.86 101.03 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13 12 -10 53.34 16.53 -13 -12 10 46.49 18.49 10 12 7 60.26 19.41 10 -12 7 77.30 16.62 -10 12 -7 35.15 14.67 -6 7 -14 44.05 26.46 6 7 14 40.89 19.11 -18 0 7 -4.25 8.36 -18 0 7 -8.82 24.31 10 -15 -9 247.82 45.51 -10 -15 9 260.15 68.04 10 15 -9 274.04 53.91 -7 15 -7 4.83 15.30 7 -15 7 -4.90 20.44 7 15 7 4.63 9.42 -7 -2 19 -3.30 5.27 -7 2 19 8.29 4.98 -7 -2 19 0.61 4.45 -7 2 19 5.03 6.17 -7 2 19 -1.81 7.93 -15 8 -2 2.92 12.94 -15 -8 -2 6.46 8.22 -15 -8 -2 15.34 11.36 -15 8 -2 3.19 22.01 -15 -8 -2 8.57 6.61 -16 -9 5 81.06 16.66 -16 9 5 48.90 33.35 14 12 -7 4.51 16.84 -14 12 7 39.47 27.75 -14 -12 7 91.11 17.10 -12 13 10 486.32 139.87 12 13 -10 571.33 61.53 -12 -13 10 586.52 68.08 -18 1 5 97.40 12.42 -18 -1 5 164.52 47.19 -18 1 5 65.62 52.91 -18 -1 5 181.53 27.67 -18 1 5 74.36 17.70 -18 -1 5 91.45 10.41 11 15 -7 1.52 7.42 -11 -15 7 -3.95 15.34 0 18 -7 18.27 11.65 0 -18 -7 12.70 10.74 0 18 7 9.70 11.69 0 -18 7 25.38 17.40 0 18 7 2.74 7.67 4 18 -7 26.15 12.55 4 -18 -7 21.87 26.38 -4 18 7 7.25 12.33 -4 -18 7 58.48 20.84 -15 0 15 256.31 44.64 1 14 -13 150.56 22.91 -1 14 13 176.05 49.20 1 14 -13 117.81 23.09 -1 -14 13 165.83 50.78 -12 -4 17 45.51 13.45 -12 4 17 37.38 10.49 -12 4 17 42.13 27.43 -14 7 14 159.64 23.69 -14 7 14 159.33 39.23 -14 -7 14 170.21 45.84 -4 -19 1 487.68 107.92 4 -19 -1 478.32 74.40 -4 19 1 347.22 57.76 4 19 -1 497.76 78.30 4 19 -1 480.68 41.43 -14 -12 2 193.89 23.50 -14 12 2 132.32 44.87 8 16 4 -2.36 7.22 -8 16 -4 2.46 8.82 8 16 4 7.66 10.77 8 -16 4 -7.84 10.91 -8 -16 -4 0.35 10.24 6 12 -15 54.37 22.47 -6 12 15 9.37 20.93 -6 -12 15 45.49 26.12 -10 0 -12 306.78 45.52 -9 -16 8 27.65 26.97 9 -16 -8 14.81 16.74 9 16 -8 18.21 19.52 4 9 -17 27.30 14.26 -4 -9 17 21.35 10.33 -17 -6 3 15.56 8.35 -17 6 3 -0.94 18.07 -17 -6 3 16.99 11.86 8 8 12 386.46 52.90 -8 8 -12 403.52 51.14 5 17 -9 20.66 11.71 -5 17 9 5.97 11.06 5 -17 -9 20.06 13.30 -5 -17 9 34.39 18.46 8 15 -11 140.97 32.64 -8 -15 11 167.65 43.24 -8 15 11 21.01 24.49 -17 3 0 94.29 25.33 -17 -3 0 124.72 23.19 -17 -3 0 142.73 16.80 -17 3 0 105.78 29.99 -17 -3 0 155.91 36.90 -14 -1 -7 312.58 66.53 -14 1 -7 312.97 43.65 4 -19 -2 -4.69 22.01 -4 -19 2 0.82 12.50 4 19 -2 5.03 13.27 -4 19 2 0.95 9.08 -17 -6 8 575.63 58.46 -17 6 8 524.15 147.54 1 10 -16 393.65 48.04 1 10 -16 370.78 41.37 -1 -10 16 416.60 39.86 -16 9 6 210.14 55.62 -16 -9 6 248.32 31.04 11 15 0 268.71 24.65 11 -15 0 250.86 48.17 -11 -15 0 289.76 48.64 11 15 0 265.36 40.11 -13 -5 16 33.40 14.67 -13 5 16 41.86 18.73 -13 5 16 39.68 11.23 -14 7 -5 98.09 39.51 -14 -7 -5 225.12 24.83 -18 1 7 166.69 38.99 -18 -1 7 181.26 37.68 -18 -1 7 168.03 38.82 -18 1 7 184.82 40.83 -9 14 -6 27.87 26.29 9 14 6 63.11 26.68 9 -14 6 43.34 18.94 -10 -4 18 266.62 26.98 -10 4 18 241.51 22.02 -10 4 18 254.62 48.70 -17 -3 11 84.81 27.49 -17 -3 11 70.25 18.45 -17 3 11 130.67 30.83 -17 3 11 69.29 30.52 -15 -1 15 104.63 20.21 -15 1 15 170.65 50.55 -15 -1 15 110.28 50.15 -8 6 18 0.01 6.01 -8 -6 18 3.57 5.78 -8 6 18 -2.41 6.45 -6 -9 17 27.11 16.69 -6 9 17 4.60 13.37 6 9 -17 32.95 15.28 -6 9 17 13.68 8.43 2 -19 3 503.70 79.76 2 19 3 552.12 75.36 -2 19 -3 407.46 52.25 -2 -19 -3 480.89 64.94 2 19 3 510.80 78.70 10 11 8 3.93 16.09 10 -11 8 -5.18 11.72 -10 11 -8 -0.02 9.57 3 16 -11 7.80 8.74 3 16 -11 3.18 4.72 -3 -16 11 4.27 21.38 3 -16 -11 0.85 6.97 -3 16 11 -0.20 5.84 -3 16 11 3.86 10.34 -3 1 19 39.05 12.51 -8 0 19 4.32 5.73 -8 0 19 -0.28 4.31 -10 -1 -12 223.88 60.42 -10 1 -12 207.92 61.56 -12 14 0 24.86 21.77 -12 -14 0 45.82 20.16 12 14 0 44.68 16.97 12 14 0 43.10 15.36 0 -17 -9 19.27 15.68 0 17 9 42.33 13.66 0 17 9 2.49 7.11 0 17 -9 36.77 21.69 0 -17 9 47.10 30.49 -1 15 12 56.69 16.77 1 15 -12 97.92 14.33 1 15 -12 49.22 22.89 -1 -15 12 41.38 31.36 -1 15 12 9.89 10.49 1 -15 -12 7.53 8.39 -1 8 17 488.73 54.48 1 8 -17 451.84 35.57 -1 -8 17 478.92 55.61 1 8 -17 480.50 46.38 -16 9 4 325.65 104.08 -16 -9 4 321.64 33.98 3 -9 15 112.46 17.27 -3 9 -15 148.07 31.10 3 9 15 170.44 28.96 -3 9 -15 107.70 13.30 1 5 -18 37.91 10.07 -1 5 18 32.77 14.60 -12 5 -9 94.00 41.97 -12 -5 -9 91.12 21.78 -10 -7 17 77.38 27.88 -10 7 17 70.87 12.41 -10 7 17 80.04 19.53 -3 -2 -17 42.33 26.72 -3 2 -17 32.85 24.38 -15 7 -3 38.77 15.45 -15 7 -3 9.24 14.49 -15 -7 -3 31.22 15.69 -15 -7 -3 22.79 9.64 -11 8 16 1.93 22.29 -11 -8 16 15.76 10.91 -11 8 16 6.33 12.02 -7 -18 2 -4.33 21.59 -7 18 2 4.10 12.66 7 -18 -2 9.04 14.86 7 18 -2 6.37 8.89 7 18 -2 6.23 14.15 -7 16 10 83.02 25.63 -7 -16 10 162.03 50.63 7 16 -10 128.49 35.78 10 14 -11 230.51 34.35 -10 -14 11 263.72 40.22 10 -14 -11 235.76 41.38 -15 3 -5 18.12 10.60 -15 3 -5 17.09 16.15 -15 -3 -5 38.10 20.09 -15 3 -5 24.22 23.85 -10 -16 6 77.09 37.40 10 16 -6 67.06 17.28 3 19 2 170.30 45.97 3 -19 2 287.71 76.52 -3 -19 -2 112.66 33.58 -3 19 -2 322.55 53.31 3 19 2 90.69 36.30 -5 0 -16 -0.80 8.79 -11 0 -11 264.12 41.24 -5 3 19 216.08 35.61 -5 -3 19 207.85 24.66 -4 -19 0 14.12 16.36 -4 19 0 18.74 22.26 4 -19 0 25.84 32.62 4 19 0 11.01 13.68 4 19 0 10.02 13.13 -18 0 4 302.29 83.52 -18 0 4 319.86 33.34 -18 0 4 315.69 25.39 -9 11 15 96.09 26.30 9 11 -15 136.46 23.44 -9 -11 15 123.39 41.45 -6 3 19 8.50 6.02 -6 3 19 -1.05 8.07 -6 -3 19 1.50 7.88 -9 0 -13 291.12 69.07 -4 16 11 6.38 8.18 -4 -16 11 19.93 15.47 -4 16 11 11.83 20.96 4 16 -11 29.97 17.69 4 -16 -11 6.35 9.28 -7 -18 3 0.24 11.70 -7 18 3 2.04 11.20 7 18 -3 5.47 13.03 7 18 -3 -0.03 7.09 7 -18 -3 12.17 13.62 -16 5 -2 93.39 36.91 -16 -5 -2 105.98 15.13 -16 5 -2 32.70 23.41 -16 -5 -2 86.42 16.01 -16 -5 -2 88.63 23.71 -8 1 19 239.96 27.63 -8 1 19 249.24 28.31 -8 -1 19 227.09 24.52 -8 -1 19 257.84 29.91 -8 1 19 248.82 36.82 -18 2 6 2.21 7.89 -18 2 6 1.98 12.22 -18 -2 6 -13.73 20.04 -18 -2 6 -2.63 6.68 -18 2 6 -7.84 13.11 -3 19 4 93.04 27.08 3 -19 -4 187.19 57.51 3 19 -4 156.80 25.26 -13 4 -8 3.26 10.21 -13 -4 -8 -2.55 14.70 6 15 -12 15.14 10.19 -6 15 12 0.74 9.42 -15 -10 9 2.21 15.47 -15 10 9 1.04 27.17 5 -15 9 46.49 20.18 5 15 9 67.43 30.31 -5 15 -9 31.94 21.62 -15 -9 -1 -3.01 5.01 -15 -9 -1 -2.51 6.33 -16 -8 1 -6.11 6.16 -16 -8 1 -5.76 8.20 -16 8 1 6.21 14.67 2 14 12 38.74 14.75 -2 14 -12 14.11 6.25 2 -14 12 -3.54 23.60 10 13 6 6.51 16.32 -10 13 -6 -5.35 8.81 10 -13 6 -6.70 10.09 -12 12 -4 241.53 43.41 12 12 4 399.99 39.67 -11 2 18 3.11 7.78 -11 -2 18 -0.92 10.10 -11 -2 18 3.41 7.63 -11 2 18 0.61 5.09 7 5 14 143.26 31.95 -14 2 16 6.79 10.39 -14 -2 16 0.01 7.63 -14 -2 16 -9.99 17.86 2 16 -11 -0.80 5.43 2 -16 -11 5.96 10.93 -2 16 11 22.25 10.80 -2 16 11 1.33 5.36 -1 0 -18 -2.27 14.09 -10 6 -11 289.62 44.38 -13 13 8 -10.64 18.64 -18 -1 4 136.36 24.58 -18 -1 4 98.98 25.05 -18 -1 4 67.36 10.07 -18 1 4 70.14 14.81 -18 1 4 80.94 11.83 -18 1 4 67.40 27.81 -18 2 5 214.99 21.40 -18 -2 5 252.01 41.20 -18 2 5 177.08 43.10 -18 -2 5 237.36 26.02 -18 2 5 216.96 78.87 -11 6 17 11.69 7.16 -11 6 17 12.30 12.02 1 13 -14 4.07 5.05 -1 13 14 6.61 11.24 -2 10 -15 396.98 36.35 2 10 15 458.96 54.45 -2 10 -15 376.93 33.41 2 -10 15 363.22 55.65 2 12 -15 1.91 7.51 2 12 -15 7.26 7.40 -15 5 14 125.95 33.04 -15 5 14 90.20 32.91 -7 13 14 3.61 15.40 9 6 12 6.21 12.33 2 6 -18 -0.58 5.20 -2 -6 18 10.31 9.25 -2 6 18 16.00 10.13 2 6 -18 16.07 6.15 7 18 -1 136.12 16.10 7 -18 -1 34.30 61.92 -10 9 16 56.08 11.33 -10 9 16 22.22 31.11 4 -19 -3 419.43 105.21 12 -9 7 64.01 15.57 -16 3 -3 78.34 18.68 -16 -3 -3 61.58 22.25 -18 0 8 50.10 44.35 -13 0 17 290.73 68.28 -16 9 7 32.29 44.47 -15 11 5 6.66 17.38 -18 -2 7 183.36 59.66 -18 2 7 88.57 67.92 -15 2 15 -3.18 12.49 -15 -2 15 -3.60 20.67 ; _shelx_hkl_checksum 71561 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 -1/2+X,-1/2-Y,-1/2+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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.41743(2) 0.13054(2) 0.72492(2) 0.01692(7) Uani 1 1 d . . . . . Cl1 Cl 0.43454(9) 0.17032(7) 0.36945(7) 0.0308(2) Uani 1 1 d . . . . . Cl2 Cl 0.7320(2) 0.16336(19) 0.63635(13) 0.1017(8) Uani 1 1 d . . . . . Cl3 Cl 0.7189(2) 0.33979(16) 0.5542(2) 0.1065(9) Uani 1 1 d . . . . . O1 O 0.4287(2) 0.14172(19) 0.56908(18) 0.0241(6) Uani 1 1 d . . . . . O2 O 0.4721(2) -0.00252(19) 0.67040(17) 0.0214(6) Uani 1 1 d . . . . . N1 N 0.6037(3) 0.1134(2) 0.7999(2) 0.0238(7) Uani 1 1 d . . . . . N2 N 0.6631(3) 0.1822(2) 0.8450(2) 0.0250(7) Uani 1 1 d . . . . . N3 N 0.4835(3) 0.2782(2) 0.7059(2) 0.0250(7) Uani 1 1 d . . . . . N4 N 0.5631(3) 0.3180(2) 0.7700(2) 0.0255(7) Uani 1 1 d . . . . . N5 N 0.4660(3) 0.2012(2) 0.8864(2) 0.0228(7) Uani 1 1 d . . . . . N6 N 0.5471(3) 0.2546(2) 0.9214(2) 0.0239(7) Uani 1 1 d . . . . . N7 N 0.2708(3) 0.2136(2) 0.7395(2) 0.0245(7) Uani 1 1 d . . . . . N8 N 0.1924(3) 0.1712(2) 0.7567(2) 0.0235(7) Uani 1 1 d . . . . . N9 N 0.3638(2) 0.0244(2) 0.8227(2) 0.0202(7) Uani 1 1 d . . . . . N10 N 0.2687(2) 0.0255(2) 0.8292(2) 0.0214(7) Uani 1 1 d . . . . . N11 N 0.2586(3) 0.0571(2) 0.6204(2) 0.0232(7) Uani 1 1 d . . . . . N12 N 0.1823(3) 0.0360(2) 0.6561(2) 0.0229(7) Uani 1 1 d . . . . . C1 C 0.4886(3) -0.0058(3) 0.5920(2) 0.0198(8) Uani 1 1 d . . . . . C2 C 0.4607(3) 0.0780(3) 0.5312(3) 0.0195(7) Uani 1 1 d . . . . . C3 C 0.4706(3) 0.0784(3) 0.4410(2) 0.0204(8) Uani 1 1 d . . . . . C4 C 0.6652(3) 0.0433(3) 0.8078(3) 0.0287(9) Uani 1 1 d . . . . . H4 H 0.6446 -0.0141 0.7835 0.034 Uiso 1 1 calc R U . . . C5 C 0.7638(3) 0.0674(3) 0.8572(3) 0.0324(10) Uani 1 1 d . . . . . H5 H 0.8218 0.0307 0.8726 0.039 Uiso 1 1 calc R U . . . C6 C 0.7588(3) 0.1555(3) 0.8787(3) 0.0295(10) Uani 1 1 d . . . . . H6 H 0.8140 0.1914 0.9119 0.035 Uiso 1 1 calc R U . . . C7 C 0.4535(3) 0.3353(3) 0.6335(3) 0.0293(9) Uani 1 1 d . . . . . H7 H 0.3993 0.3252 0.5779 0.035 Uiso 1 1 calc R U . . . C8 C 0.5121(4) 0.4106(3) 0.6508(3) 0.0365(11) Uani 1 1 d . . . . . H8 H 0.5060 0.4609 0.6112 0.044 Uiso 1 1 calc R U . . . C9 C 0.5811(4) 0.3970(3) 0.7377(3) 0.0344(10) Uani 1 1 d . . . . . H9 H 0.6328 0.4369 0.7694 0.041 Uiso 1 1 calc R U . . . C10 C 0.4213(3) 0.1971(3) 0.9537(3) 0.0266(9) Uani 1 1 d . . . . . H10 H 0.3618 0.1646 0.9489 0.032 Uiso 1 1 calc R U . . . C11 C 0.4735(4) 0.2470(3) 1.0320(3) 0.0307(10) Uani 1 1 d . . . . . H11 H 0.4577 0.2547 1.0893 0.037 Uiso 1 1 calc R U . . . C12 C 0.5520(3) 0.2824(3) 1.0086(3) 0.0292(9) Uani 1 1 d . . . . . H12 H 0.6019 0.3203 1.0472 0.035 Uiso 1 1 calc R U . . . C13 C 0.2591(4) 0.2994(3) 0.7544(3) 0.0283(9) Uani 1 1 d . . . . . H13 H 0.3034 0.3448 0.7476 0.034 Uiso 1 1 calc R U . . . C14 C 0.1742(4) 0.3137(3) 0.7812(3) 0.0342(10) Uani 1 1 d . . . . . H14 H 0.1489 0.3686 0.7956 0.041 Uiso 1 1 calc R U . . . C15 C 0.1346(4) 0.2310(3) 0.7822(3) 0.0318(10) Uani 1 1 d . . . . . H15 H 0.0755 0.2179 0.7984 0.038 Uiso 1 1 calc R U . . . C16 C 0.4176(3) -0.0256(3) 0.8948(3) 0.0263(9) Uani 1 1 d . . . . . H16 H 0.4868 -0.0387 0.9069 0.032 Uiso 1 1 calc R U . . . C17 C 0.3604(3) -0.0557(3) 0.9490(3) 0.0280(9) Uani 1 1 d . . . . . H17 H 0.3810 -0.0917 1.0039 0.034 Uiso 1 1 calc R U . . . C18 C 0.2659(3) -0.0216(3) 0.9052(3) 0.0260(9) Uani 1 1 d . . . . . H18 H 0.2083 -0.0301 0.9255 0.031 Uiso 1 1 calc R U . . . C19 C 0.2353(3) 0.0168(3) 0.5357(3) 0.0290(9) Uani 1 1 d . . . . . H19 H 0.2745 0.0205 0.4936 0.035 Uiso 1 1 calc R U . . . C20 C 0.1465(3) -0.0307(3) 0.5178(3) 0.0331(10) Uani 1 1 d . . . . . H20 H 0.1143 -0.0652 0.4637 0.040 Uiso 1 1 calc R U . . . C21 C 0.1157(3) -0.0166(3) 0.5956(3) 0.0293(9) Uani 1 1 d . . . . . H21 H 0.0567 -0.0403 0.6053 0.035 Uiso 1 1 calc R U . . . C22 C 0.6831(8) 0.2321(6) 0.5412(6) 0.105(4) Uani 1 1 d . . . . . H22A H 0.7015 0.2077 0.4869 0.127 Uiso 1 1 calc R U . . . H22B H 0.6090 0.2299 0.5246 0.127 Uiso 1 1 calc R U . . . B1 B 0.6201(4) 0.2722(3) 0.8639(3) 0.0264(10) Uani 1 1 d . . . . . H1 H 0.6760 0.3112 0.9009 0.032 Uiso 1 1 calc R U . . . B2 B 0.1812(3) 0.0694(3) 0.7532(3) 0.0235(9) Uani 1 1 d . . . . . H2 H 0.1162 0.0527 0.7637 0.028 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 0.01854(10) 0.01751(10) 0.01551(10) -0.00164(6) 0.00635(7) -0.00048(7) Cl1 0.0446(6) 0.0248(5) 0.0278(5) 0.0073(4) 0.0183(5) 0.0107(4) Cl2 0.141(2) 0.121(2) 0.0610(10) 0.0275(11) 0.0569(13) 0.0321(17) Cl3 0.138(2) 0.0660(13) 0.164(2) -0.0189(14) 0.120(2) -0.0136(13) O1 0.0327(16) 0.0201(15) 0.0232(13) -0.0009(11) 0.0139(12) 0.0035(12) O2 0.0268(14) 0.0214(14) 0.0187(12) -0.0015(10) 0.0110(11) 0.0013(11) N1 0.0230(17) 0.0238(18) 0.0224(15) -0.0020(13) 0.0037(14) 0.0010(14) N2 0.0191(16) 0.033(2) 0.0226(16) -0.0002(14) 0.0066(14) -0.0048(15) N3 0.0285(18) 0.0227(18) 0.0218(15) 0.0004(13) 0.0049(14) -0.0018(14) N4 0.0269(18) 0.0224(18) 0.0282(17) 0.0006(14) 0.0097(15) -0.0057(14) N5 0.0253(17) 0.0229(18) 0.0202(15) -0.0044(13) 0.0071(14) -0.0036(14) N6 0.0267(17) 0.0222(18) 0.0210(15) -0.0049(13) 0.0046(14) -0.0031(14) N7 0.0249(17) 0.0236(18) 0.0248(16) 0.0000(13) 0.0074(14) 0.0022(14) N8 0.0209(17) 0.0279(19) 0.0229(16) 0.0014(13) 0.0086(14) 0.0049(14) N9 0.0203(16) 0.0202(17) 0.0200(15) 0.0024(12) 0.0059(13) -0.0010(13) N10 0.0221(17) 0.0219(17) 0.0202(15) 0.0015(13) 0.0064(13) -0.0012(13) N11 0.0247(17) 0.0244(18) 0.0191(15) -0.0008(13) 0.0044(14) 0.0006(14) N12 0.0201(16) 0.0242(18) 0.0234(16) 0.0032(13) 0.0051(14) -0.0014(14) C1 0.0167(18) 0.023(2) 0.0183(16) 0.0002(14) 0.0033(15) -0.0030(15) C2 0.0217(18) 0.0166(18) 0.0216(17) -0.0031(14) 0.0086(16) -0.0006(15) C3 0.0229(19) 0.0198(19) 0.0185(17) 0.0025(14) 0.0064(15) 0.0009(15) C4 0.028(2) 0.029(2) 0.029(2) -0.0015(17) 0.0074(18) 0.0053(18) C5 0.028(2) 0.038(3) 0.031(2) 0.0086(19) 0.0082(19) 0.0084(19) C6 0.021(2) 0.041(3) 0.028(2) 0.0058(18) 0.0086(18) -0.0038(18) C7 0.031(2) 0.030(2) 0.028(2) 0.0041(17) 0.0105(19) 0.0006(18) C8 0.039(3) 0.029(3) 0.043(2) 0.014(2) 0.015(2) 0.001(2) C9 0.032(2) 0.030(2) 0.042(2) 0.002(2) 0.012(2) -0.0091(19) C10 0.030(2) 0.028(2) 0.0236(19) -0.0028(16) 0.0110(18) 0.0018(18) C11 0.040(3) 0.031(2) 0.0208(18) -0.0062(17) 0.0093(18) 0.002(2) C12 0.033(2) 0.029(2) 0.0216(18) -0.0062(16) 0.0015(18) -0.0009(18) C13 0.037(2) 0.022(2) 0.027(2) 0.0016(16) 0.0115(19) 0.0055(18) C14 0.046(3) 0.029(2) 0.030(2) 0.0034(18) 0.014(2) 0.016(2) C15 0.033(2) 0.035(3) 0.030(2) 0.0062(18) 0.0142(19) 0.013(2) C16 0.025(2) 0.027(2) 0.0258(19) 0.0011(16) 0.0057(17) 0.0031(17) C17 0.033(2) 0.029(2) 0.0204(18) 0.0046(16) 0.0052(17) -0.0004(18) C18 0.031(2) 0.026(2) 0.0226(18) 0.0016(16) 0.0104(17) -0.0045(18) C19 0.030(2) 0.030(2) 0.0222(19) -0.0054(17) 0.0013(17) 0.0024(18) C20 0.030(2) 0.034(3) 0.028(2) -0.0074(18) -0.0012(19) -0.0020(19) C21 0.023(2) 0.027(2) 0.033(2) 0.0018(18) 0.0007(18) -0.0038(17) C22 0.134(8) 0.088(7) 0.070(5) 0.018(4) -0.005(5) -0.054(6) B1 0.027(2) 0.024(2) 0.026(2) -0.0027(18) 0.005(2) -0.0051(19) B2 0.019(2) 0.027(2) 0.025(2) 0.0043(18) 0.0081(18) 0.0004(18) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; B B 0.0013 0.0007 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Dy Dy -0.1892 4.4098 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (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 Dy1 O2 66.69(9) . . O1 Dy1 N9 138.94(10) . . O2 Dy1 N9 80.57(10) . . O1 Dy1 N3 71.65(10) . . O2 Dy1 N3 123.71(11) . . N9 Dy1 N3 149.39(11) . . O1 Dy1 N7 110.62(10) . . O2 Dy1 N7 145.16(11) . . N9 Dy1 N7 82.38(11) . . N3 Dy1 N7 84.31(12) . . O1 Dy1 N1 94.22(10) . . O2 Dy1 N1 70.58(10) . . N9 Dy1 N1 97.64(11) . . N3 Dy1 N1 76.69(12) . . N7 Dy1 N1 142.09(11) . . O1 Dy1 N5 145.02(11) . . O2 Dy1 N5 131.27(10) . . N9 Dy1 N5 75.67(11) . . N3 Dy1 N5 74.03(11) . . N7 Dy1 N5 72.10(11) . . N1 Dy1 N5 71.25(11) . . O1 Dy1 N11 74.88(10) . . O2 Dy1 N11 74.65(10) . . N9 Dy1 N11 73.00(10) . . N3 Dy1 N11 127.76(11) . . N7 Dy1 N11 71.39(11) . . N1 Dy1 N11 145.05(11) . . N5 Dy1 N11 134.22(11) . . C2 O1 Dy1 121.2(2) . . C1 O2 Dy1 121.2(3) . . C4 N1 N2 106.1(3) . . C4 N1 Dy1 131.9(3) . . N2 N1 Dy1 122.1(3) . . C6 N2 N1 110.0(4) . . C6 N2 B1 126.6(4) . . N1 N2 B1 122.9(3) . . C7 N3 N4 105.5(4) . . C7 N3 Dy1 129.6(3) . . N4 N3 Dy1 124.9(2) . . C9 N4 N3 110.1(3) . . C9 N4 B1 128.5(4) . . N3 N4 B1 121.4(3) . . C10 N5 N6 105.5(3) . . C10 N5 Dy1 130.0(3) . . N6 N5 Dy1 124.5(2) . . C12 N6 N5 110.2(3) . . C12 N6 B1 129.3(4) . . N5 N6 B1 120.4(3) . . C13 N7 N8 106.2(4) . . C13 N7 Dy1 131.0(3) . . N8 N7 Dy1 121.1(3) . . C15 N8 N7 109.0(4) . . C15 N8 B2 128.0(4) . . N7 N8 B2 122.9(3) . . C16 N9 N10 105.8(3) . . C16 N9 Dy1 130.6(3) . . N10 N9 Dy1 121.3(2) . . C18 N10 N9 109.4(3) . . C18 N10 B2 128.6(4) . . N9 N10 B2 121.9(3) . . C19 N11 N12 105.2(3) . . C19 N11 Dy1 133.3(3) . . N12 N11 Dy1 120.3(2) . . C21 N12 N11 110.1(3) . . C21 N12 B2 128.5(4) . . N11 N12 B2 121.4(3) . . O2 C1 C3 124.6(4) . 3_656 O2 C1 C2 115.4(3) . . C3 C1 C2 120.0(3) 3_656 . O1 C2 C3 125.3(4) . . O1 C2 C1 115.3(3) . . C3 C2 C1 119.4(3) . . C2 C3 C1 120.5(3) . 3_656 C2 C3 Cl1 120.2(3) . . C1 C3 Cl1 119.3(3) 3_656 . N1 C4 C5 110.1(4) . . N1 C4 H4 125.0 . . C5 C4 H4 125.0 . . C6 C5 C4 105.2(4) . . C6 C5 H5 127.4 . . C4 C5 H5 127.4 . . N2 C6 C5 108.7(4) . . N2 C6 H6 125.7 . . C5 C6 H6 125.7 . . N3 C7 C8 110.9(4) . . N3 C7 H7 124.5 . . C8 C7 H7 124.5 . . C9 C8 C7 105.1(4) . . C9 C8 H8 127.5 . . C7 C8 H8 127.5 . . N4 C9 C8 108.4(4) . . N4 C9 H9 125.8 . . C8 C9 H9 125.8 . . N5 C10 C11 110.9(4) . . N5 C10 H10 124.6 . . C11 C10 H10 124.6 . . C12 C11 C10 104.9(4) . . C12 C11 H11 127.5 . . C10 C11 H11 127.5 . . N6 C12 C11 108.5(4) . . N6 C12 H12 125.7 . . C11 C12 H12 125.7 . . N7 C13 C14 111.1(4) . . N7 C13 H13 124.4 . . C14 C13 H13 124.4 . . C15 C14 C13 104.2(4) . . C15 C14 H14 127.9 . . C13 C14 H14 127.9 . . N8 C15 C14 109.4(4) . . N8 C15 H15 125.3 . . C14 C15 H15 125.3 . . N9 C16 C17 111.8(4) . . N9 C16 H16 124.1 . . C17 C16 H16 124.1 . . C16 C17 C18 104.1(4) . . C16 C17 H17 127.9 . . C18 C17 H17 127.9 . . N10 C18 C17 108.9(4) . . N10 C18 H18 125.6 . . C17 C18 H18 125.6 . . N11 C19 C20 111.1(4) . . N11 C19 H19 124.4 . . C20 C19 H19 124.4 . . C21 C20 C19 104.5(4) . . C21 C20 H20 127.7 . . C19 C20 H20 127.7 . . N12 C21 C20 109.0(4) . . N12 C21 H21 125.5 . . C20 C21 H21 125.5 . . Cl3 C22 Cl2 117.0(5) . . Cl3 C22 H22A 108.0 . . Cl2 C22 H22A 108.0 . . Cl3 C22 H22B 108.0 . . Cl2 C22 H22B 108.0 . . H22A C22 H22B 107.3 . . N6 B1 N4 109.4(4) . . N6 B1 N2 108.0(3) . . N4 B1 N2 110.6(3) . . N6 B1 H1 109.6 . . N4 B1 H1 109.6 . . N2 B1 H1 109.6 . . N12 B2 N10 108.4(3) . . N12 B2 N8 109.2(3) . . N10 B2 N8 110.7(3) . . N12 B2 H2 109.5 . . N10 B2 H2 109.5 . . N8 B2 H2 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy1 O1 2.376(3) . Dy1 O2 2.379(3) . Dy1 N9 2.431(3) . Dy1 N3 2.463(4) . Dy1 N7 2.469(4) . Dy1 N1 2.517(3) . Dy1 N5 2.526(3) . Dy1 N11 2.547(3) . Cl1 C3 1.729(4) . Cl2 C22 1.721(8) . Cl3 C22 1.696(9) . O1 C2 1.264(5) . O2 C1 1.256(4) . N1 C4 1.347(5) . N1 N2 1.372(5) . N2 C6 1.341(6) . N2 B1 1.546(6) . N3 C7 1.343(5) . N3 N4 1.366(5) . N4 C9 1.339(6) . N4 B1 1.546(6) . N5 C10 1.332(5) . N5 N6 1.361(5) . N6 C12 1.345(5) . N6 B1 1.540(6) . N7 C13 1.334(5) . N7 N8 1.359(5) . N8 C15 1.342(6) . N8 B2 1.545(6) . N9 C16 1.341(5) . N9 N10 1.363(5) . N10 C18 1.347(5) . N10 B2 1.542(5) . N11 C19 1.347(5) . N11 N12 1.365(5) . N12 C21 1.341(5) . N12 B2 1.535(5) . C1 C3 1.393(6) 3_656 C1 C2 1.535(5) . C2 C3 1.391(5) . C3 C1 1.393(6) 3_656 C4 C5 1.400(6) . C4 H4 0.9500 . C5 C6 1.375(7) . C5 H5 0.9500 . C6 H6 0.9500 . C7 C8 1.379(7) . C7 H7 0.9500 . C8 C9 1.374(7) . C8 H8 0.9500 . C9 H9 0.9500 . C10 C11 1.395(6) . C10 H10 0.9500 . C11 C12 1.357(7) . C11 H11 0.9500 . C12 H12 0.9500 . C13 C14 1.379(7) . C13 H13 0.9500 . C14 C15 1.369(7) . C14 H14 0.9500 . C15 H15 0.9500 . C16 C17 1.373(6) . C16 H16 0.9500 . C17 C18 1.384(6) . C17 H17 0.9500 . C18 H18 0.9500 . C19 C20 1.389(7) . C19 H19 0.9500 . C20 C21 1.368(6) . C20 H20 0.9500 . C21 H21 0.9500 . C22 H22A 0.9900 . C22 H22B 0.9900 . B1 H1 1.0000 . B2 H2 1.0000 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C4 N1 N2 C6 0.8(4) . . . . Dy1 N1 N2 C6 179.8(3) . . . . C4 N1 N2 B1 -171.7(4) . . . . Dy1 N1 N2 B1 7.4(5) . . . . C7 N3 N4 C9 -0.1(5) . . . . Dy1 N3 N4 C9 178.8(3) . . . . C7 N3 N4 B1 -179.3(4) . . . . Dy1 N3 N4 B1 -0.4(5) . . . . C10 N5 N6 C12 0.2(5) . . . . Dy1 N5 N6 C12 179.4(3) . . . . C10 N5 N6 B1 177.7(4) . . . . Dy1 N5 N6 B1 -3.1(5) . . . . C13 N7 N8 C15 -0.4(4) . . . . Dy1 N7 N8 C15 166.3(3) . . . . C13 N7 N8 B2 -176.2(3) . . . . Dy1 N7 N8 B2 -9.6(4) . . . . C16 N9 N10 C18 1.2(4) . . . . Dy1 N9 N10 C18 -163.2(3) . . . . C16 N9 N10 B2 -174.3(4) . . . . Dy1 N9 N10 B2 21.3(5) . . . . C19 N11 N12 C21 1.0(4) . . . . Dy1 N11 N12 C21 -168.1(3) . . . . C19 N11 N12 B2 179.8(4) . . . . Dy1 N11 N12 B2 10.7(5) . . . . Dy1 O2 C1 C3 173.8(3) . . . 3_656 Dy1 O2 C1 C2 -6.1(4) . . . . Dy1 O1 C2 C3 -179.5(3) . . . . Dy1 O1 C2 C1 1.3(5) . . . . O2 C1 C2 O1 3.1(5) . . . . C3 C1 C2 O1 -176.8(4) 3_656 . . . O2 C1 C2 C3 -176.2(4) . . . . C3 C1 C2 C3 3.9(6) 3_656 . . . O1 C2 C3 C1 176.9(4) . . . 3_656 C1 C2 C3 C1 -4.0(6) . . . 3_656 O1 C2 C3 Cl1 -2.0(6) . . . . C1 C2 C3 Cl1 177.2(3) . . . . N2 N1 C4 C5 -0.5(5) . . . . Dy1 N1 C4 C5 -179.3(3) . . . . N1 C4 C5 C6 0.0(5) . . . . N1 N2 C6 C5 -0.8(5) . . . . B1 N2 C6 C5 171.3(4) . . . . C4 C5 C6 N2 0.5(5) . . . . N4 N3 C7 C8 -0.3(5) . . . . Dy1 N3 C7 C8 -179.1(3) . . . . N3 C7 C8 C9 0.6(6) . . . . N3 N4 C9 C8 0.4(5) . . . . B1 N4 C9 C8 179.6(4) . . . . C7 C8 C9 N4 -0.6(6) . . . . N6 N5 C10 C11 -0.4(5) . . . . Dy1 N5 C10 C11 -179.6(3) . . . . N5 C10 C11 C12 0.5(5) . . . . N5 N6 C12 C11 0.1(5) . . . . B1 N6 C12 C11 -177.1(4) . . . . C10 C11 C12 N6 -0.4(5) . . . . N8 N7 C13 C14 0.0(4) . . . . Dy1 N7 C13 C14 -164.8(3) . . . . N7 C13 C14 C15 0.3(5) . . . . N7 N8 C15 C14 0.6(5) . . . . B2 N8 C15 C14 176.1(4) . . . . C13 C14 C15 N8 -0.5(5) . . . . N10 N9 C16 C17 -1.1(5) . . . . Dy1 N9 C16 C17 161.3(3) . . . . N9 C16 C17 C18 0.5(5) . . . . N9 N10 C18 C17 -0.9(5) . . . . B2 N10 C18 C17 174.2(4) . . . . C16 C17 C18 N10 0.3(5) . . . . N12 N11 C19 C20 -1.0(5) . . . . Dy1 N11 C19 C20 166.0(3) . . . . N11 C19 C20 C21 0.7(5) . . . . N11 N12 C21 C20 -0.6(5) . . . . B2 N12 C21 C20 -179.3(4) . . . . C19 C20 C21 N12 -0.1(5) . . . . C12 N6 B1 N4 -121.6(4) . . . . N5 N6 B1 N4 61.4(5) . . . . C12 N6 B1 N2 118.0(5) . . . . N5 N6 B1 N2 -59.0(5) . . . . C9 N4 B1 N6 120.5(5) . . . . N3 N4 B1 N6 -60.4(5) . . . . C9 N4 B1 N2 -120.6(5) . . . . N3 N4 B1 N2 58.5(5) . . . . C6 N2 B1 N6 -114.0(4) . . . . N1 N2 B1 N6 57.2(5) . . . . C6 N2 B1 N4 126.4(4) . . . . N1 N2 B1 N4 -62.5(5) . . . . C21 N12 B2 N10 111.8(5) . . . . N11 N12 B2 N10 -66.7(5) . . . . C21 N12 B2 N8 -127.5(4) . . . . N11 N12 B2 N8 53.9(5) . . . . C18 N10 B2 N12 -125.5(4) . . . . N9 N10 B2 N12 49.1(5) . . . . C18 N10 B2 N8 114.8(4) . . . . N9 N10 B2 N8 -70.6(5) . . . . C15 N8 B2 N12 128.6(4) . . . . N7 N8 B2 N12 -56.4(4) . . . . C15 N8 B2 N10 -112.1(4) . . . . N7 N8 B2 N10 62.9(4) . . . .