#------------------------------------------------------------------------------ #$Date: 2020-10-06 10:35:33 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257392 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557826.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_1557826 loop_ _publ_author_name 'Velkos, Georgios' 'Yang, Wei' 'Yao, Yang-Rong' 'Sudarkova, Svetlana M.' 'Liu, XinYe' 'B\"uchner, Bernd' 'Avdoshenko, Stanislav M.' 'Chen, Ning' 'Popov, Alexey A.' _publ_section_title ; Shape-adaptive single-molecule magnetism and hysteresis up to 14 K in oxide clusterfullerenes Dy2O@C72 and Dy2O@C74 with fused pentagon pairs and flexible Dy--(\m2-O)--Dy angle ; _journal_issue 18 _journal_name_full 'Chemical Science' _journal_page_first 4766 _journal_page_last 4772 _journal_paper_doi 10.1039/D0SC00624F _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C72, Dy2 O, C36 H44 N4 Ni, 2(C6 H6)' _chemical_formula_sum 'C120 H56 Dy2 N4 Ni O' _chemical_formula_weight 1953.39 _chemical_name_systematic Dy2O@Cs(10528)-C72 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2018-11-23 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2019-12-27 deposited with the CCDC. 2020-04-20 downloaded from the CCDC. ; _cell_angle_alpha 84.837(2) _cell_angle_beta 88.064(2) _cell_angle_gamma 61.889(2) _cell_formula_units_Z 2 _cell_length_a 14.3857(7) _cell_length_b 14.7255(6) _cell_length_c 19.1301(9) _cell_measurement_reflns_used 9085 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 68.429 _cell_measurement_theta_min 2.319 _cell_volume 3559.7(3) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 119.98 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_unetI/netI 0.0254 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 12960 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.429 _diffrn_reflns_theta_min 2.319 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 11.910 _exptl_absorpt_correction_T_max 0.304 _exptl_absorpt_correction_T_min 0.225 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1082 before and 0.0670 after correction. The Ratio of minimum to maximum transmission is 0.3039. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear dark black' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.822 _exptl_crystal_description block _exptl_crystal_F_000 1944 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.992 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.185 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1198 _refine_ls_number_reflns 12960 _refine_ls_number_restraints 963 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0953 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2726 _refine_ls_wR_factor_ref 0.2800 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11767 _reflns_number_total 12960 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL a_a_a.res in P-1 a_a_tw.res created by SHELXL-2018/1 at 12:30:41 on 23-Nov-2018 REM Old TITL a_a.res in P-1 REM SHELXT solution in P-1 REM R1 0.295, Rweak 0.057, Alpha 0.135, Orientation as input REM Formula found by SHELXT: C101 Dy N19 Ni2 O10 CELL 1.54178 14.3857 14.7255 19.1301 84.837 88.064 61.889 ZERR 2 0.0007 0.0006 0.0009 0.002 0.002 0.002 LATT 1 SFAC C H Dy N Ni O UNIT 240 112 4 8 2 2 DFIX 1.38 C23 C22 SADI C1 C2 C2 C3 C3 C4 C4 C5 C5 C1 SADI C1 C3 C1 C4 C2 C4 C2 C5 C3 C5 SADI C1 C5 C5 C6 C6 C7 C7 C8 C8 C1 SADI C1 C6 C1 C7 C5 C7 C5 C8 C6 C8 SADI C25 C26 C26 C10 C10 C9 C9 C24 C24 C25 SADI C25 C10 C25 C9 C26 C9 C26 C24 C10 C24 SADI C15 C32 C32 C33 C33 C34 C34 C16 C16 C15 SADI C15 C33 C15 C34 C32 C34 C32 C16 C33 C16 SADI C20 C38 C38 C39 C39 C40 C40 C21 C21 C20 SADI C20 C39 C20 C40 C38 C40 C38 C21 C39 C21 SADI C42 C41 C41 C59 C59 C60 C60 C43 C43 C42 SADI C42 C59 C42 C60 C41 C60 C41 C43 C59 C43 SADI C46 C45 C45 C62 C62 C63 C63 C47 C47 C46 SADI C46 C62 C46 C63 C45 C63 C45 C47 C62 C47 SADI C70 C58 C58 C57 C57 C56 C56 C69 C69 C70 SADI C70 C57 C70 C56 C58 C56 C58 C69 C57 C69 SADI C55 C37 C37 C36 C36 C35 C35 C54 C54 C55 SADI C55 C36 C55 C35 C37 C35 C37 C54 C36 C54 SADI C13 C12 C12 C28 C28 C29 C29 C30 C30 C13 SADI C13 C28 C13 C29 C12 C29 C12 C30 C28 C30 SADI C65 C64 C64 C72 C72 C67 C67 C66 C66 C65 SADI C65 C72 C65 C67 C64 C67 C64 C66 C72 C66 SADI C65 C66 C66 C51 C51 C50 C50 C49 C49 C65 SADI C65 C51 C65 C50 C66 C50 C66 C49 C51 C49 FLAT C9 C10 C24 C25 C26 FLAT C15 C16 C32 C33 C34 FLAT C20 C21 C38 C39 C40 FLAT C41 C42 C43 C59 C60 FLAT C45 C46 C47 C62 C63 FLAT C56 C57 C58 C69 C70 FLAT C35 C36 C37 C54 C55 FLAT C12 C13 C28 C29 C30 FLAT C1 C2 C3 C4 C5 FLAT C1 C5 C6 C7 C8 FLAT C64 C65 C66 C67 C72 FLAT C49 C50 C51 C65 C66 SIMU 0.008 0.016 2 C1 > C72 SIMU 0.01 0.02 2 Dy1B Dy2B Dy3B L.S. 10 PLAN 20 SIZE 0.15 0.12 0.1 TEMP -153.17 BOND $H LIST 4 fmap 2 acta OMIT 1 -6 2 OMIT -2 -10 3 OMIT -3 -9 3 OMIT -4 -1 1 OMIT 5 -6 1 OMIT -11 -3 5 OMIT 1 -6 1 REM REM REM WGHT 0.150000 20.000000 BASF 0.31427 FVAR 3.75187 PART 1 C1 1 0.468956 0.954405 0.901719 11.00000 0.09954 0.09683 = 0.11365 -0.01660 0.01263 -0.03011 C2 1 0.451597 0.867345 0.918704 11.00000 0.09034 0.10775 = 0.09914 -0.01596 0.02495 -0.02971 C3 1 0.417134 0.845086 0.854914 11.00000 0.07061 0.10442 = 0.11100 -0.00782 0.01255 -0.03408 C4 1 0.420330 0.916248 0.799788 11.00000 0.07793 0.09419 = 0.10993 -0.00405 0.00200 -0.02165 C5 1 0.448239 0.985393 0.829228 11.00000 0.09690 0.08541 = 0.11824 -0.01133 0.00203 -0.02274 C6 1 0.528807 1.010606 0.801751 11.00000 0.10991 0.06216 = 0.11434 -0.00161 -0.00702 -0.02386 C7 1 0.596459 0.996402 0.858151 11.00000 0.11497 0.06568 = 0.11758 -0.01621 0.00267 -0.03949 C8 1 0.561183 0.962204 0.920356 11.00000 0.11174 0.08627 = 0.10340 -0.02908 0.00953 -0.03119 C9 1 0.631074 0.879872 0.965560 11.00000 0.11240 0.09349 = 0.07622 -0.03165 0.01094 -0.04520 C10 1 0.613425 0.794990 0.990976 11.00000 0.11183 0.10995 = 0.06228 -0.02230 0.01885 -0.03980 C11 1 0.516987 0.789339 0.960781 11.00000 0.09381 0.10927 = 0.08076 -0.01427 0.03655 -0.03805 C12 1 0.540767 0.685429 0.954455 11.00000 0.09609 0.11149 = 0.07968 -0.00323 0.03269 -0.04737 C13 1 0.494917 0.662205 0.895946 11.00000 0.07802 0.11459 = 0.09645 -0.00073 0.02187 -0.05744 C14 1 0.437063 0.748649 0.845212 11.00000 0.06377 0.11704 = 0.10662 -0.00722 0.01562 -0.04581 C15 1 0.452594 0.717927 0.772638 11.00000 0.06124 0.11748 = 0.09813 -0.01100 -0.01056 -0.05194 C16 1 0.460134 0.786413 0.714036 11.00000 0.06447 0.10263 = 0.09459 0.00274 -0.02938 -0.04373 C17 1 0.452153 0.890527 0.730603 11.00000 0.07662 0.09834 = 0.10326 0.01281 -0.01992 -0.01895 C18 1 0.521869 0.919871 0.694475 11.00000 0.09814 0.08423 = 0.09221 0.02311 -0.02362 -0.02421 C19 1 0.559950 0.981400 0.730293 11.00000 0.10374 0.05566 = 0.09889 0.01402 -0.02332 -0.03647 C20 1 0.668003 0.964048 0.716053 11.00000 0.12457 0.06710 = 0.10356 0.02561 -0.00196 -0.05035 C21 1 0.739819 0.952291 0.771792 11.00000 0.11127 0.06732 = 0.11236 0.01116 -0.00205 -0.06713 C22 1 0.707489 0.958244 0.843209 11.00000 0.11272 0.06899 = 0.11966 -0.01258 -0.00281 -0.05706 C23 1 0.779531 0.883688 0.898266 11.00000 0.10309 0.08030 = 0.10302 -0.01702 -0.00713 -0.06270 C24 1 0.743938 0.840663 0.956826 11.00000 0.10850 0.09369 = 0.07699 -0.03130 -0.00491 -0.05401 C25 1 0.795106 0.732446 0.979051 11.00000 0.09997 0.10555 = 0.06544 -0.01276 -0.01312 -0.05276 C26 1 0.711818 0.704789 1.001201 11.00000 0.11411 0.10563 = 0.05289 -0.00765 0.00369 -0.04436 C27 1 0.735489 0.606997 0.993251 11.00000 0.11314 0.10011 = 0.05519 0.01579 -0.00219 -0.04140 C28 1 0.637601 0.596210 0.973295 11.00000 0.10237 0.09805 = 0.06599 0.01348 0.01533 -0.05781 C29 1 0.652480 0.517146 0.929004 11.00000 0.10957 0.09277 = 0.09462 0.02149 0.01775 -0.05721 C30 1 0.566000 0.557984 0.881368 11.00000 0.09332 0.10156 = 0.09559 0.00903 0.01728 -0.07015 C31 1 0.578534 0.530304 0.807590 11.00000 0.09878 0.09951 = 0.09667 0.00402 -0.00051 -0.07304 C32 1 0.525215 0.609864 0.758495 11.00000 0.08598 0.10542 = 0.09307 -0.00244 -0.01920 -0.07361 C33 1 0.579791 0.611251 0.690726 11.00000 0.09874 0.09613 = 0.07546 -0.01050 -0.02693 -0.06675 C34 1 0.536818 0.720383 0.663505 11.00000 0.08337 0.10310 = 0.07367 0.00337 -0.03462 -0.05458 C35 1 0.589546 0.757988 0.626931 11.00000 0.09195 0.09152 = 0.06044 0.01399 -0.02881 -0.05345 C36 1 0.579648 0.859645 0.638014 11.00000 0.10383 0.08621 = 0.06666 0.02396 -0.02157 -0.03984 C37 1 0.685181 0.853735 0.625123 11.00000 0.11678 0.09008 = 0.06718 0.02186 -0.01455 -0.06148 C38 1 0.728040 0.902744 0.662127 11.00000 0.12298 0.08577 = 0.09614 0.03121 0.00367 -0.05606 C39 1 0.836751 0.851365 0.682096 11.00000 0.10372 0.09650 = 0.09778 0.01924 0.01565 -0.06777 C40 1 0.843780 0.882840 0.750897 11.00000 0.10480 0.08978 = 0.11443 0.01044 0.00282 -0.06770 C41 1 0.907846 0.816079 0.797314 11.00000 0.08469 0.09575 = 0.10552 0.00177 -0.00354 -0.06834 C42 1 0.880092 0.812302 0.871790 11.00000 0.08117 0.08912 = 0.09524 -0.01045 -0.01078 -0.06475 C43 1 0.932730 0.704937 0.899843 11.00000 0.06590 0.09671 = 0.08606 -0.00178 -0.02082 -0.05394 C44 1 0.885724 0.672226 0.952152 11.00000 0.08269 0.10277 = 0.07494 0.00442 -0.03064 -0.04857 C45 1 0.908522 0.559870 0.948711 11.00000 0.08412 0.09603 = 0.08030 0.02629 -0.03979 -0.04217 C46 1 0.828968 0.531888 0.970865 11.00000 0.10248 0.09292 = 0.07568 0.02550 -0.02208 -0.03765 C47 1 0.842210 0.447790 0.931269 11.00000 0.11065 0.07212 = 0.09097 0.03079 -0.02386 -0.03713 C48 1 0.754887 0.435700 0.903874 11.00000 0.11674 0.07939 = 0.09888 0.02558 -0.00026 -0.04198 C49 1 0.763091 0.397062 0.839567 11.00000 0.11803 0.06776 = 0.09892 0.00679 -0.00429 -0.05149 C50 1 0.678385 0.449525 0.788676 11.00000 0.11483 0.07293 = 0.09637 -0.00120 -0.00525 -0.06646 C51 1 0.726132 0.452130 0.722473 11.00000 0.12306 0.07459 = 0.09606 -0.01877 -0.00739 -0.05708 C52 1 0.681456 0.544249 0.674698 11.00000 0.11671 0.08266 = 0.07520 -0.01874 -0.01705 -0.06229 C53 1 0.747671 0.579620 0.636193 11.00000 0.10239 0.08923 = 0.06310 -0.02820 -0.00741 -0.04756 C54 1 0.698513 0.688296 0.608444 11.00000 0.09733 0.09473 = 0.05336 -0.00500 -0.01311 -0.05652 C55 1 0.758560 0.746949 0.605835 11.00000 0.10120 0.10864 = 0.05739 0.00994 -0.00071 -0.05627 C56 1 0.860184 0.698055 0.626168 11.00000 0.08965 0.11666 = 0.07222 -0.00258 0.02093 -0.05488 C57 1 0.900958 0.753961 0.667122 11.00000 0.08211 0.11129 = 0.08974 0.00305 0.02030 -0.06546 C58 1 0.974999 0.678186 0.718197 11.00000 0.06574 0.11471 = 0.09901 -0.01285 0.01963 -0.05012 C59 1 0.978552 0.708112 0.780496 11.00000 0.05987 0.10750 = 0.09943 -0.01197 0.00711 -0.05424 C60 1 0.991643 0.640199 0.843966 11.00000 0.05371 0.09813 = 0.09941 -0.00751 -0.01329 -0.03940 C61 1 1.005418 0.540121 0.837981 11.00000 0.05276 0.09762 = 0.11243 0.00405 -0.01194 -0.02218 C62 1 0.967330 0.498668 0.895120 11.00000 0.07009 0.08812 = 0.10333 0.01975 -0.02978 -0.02914 C63 1 0.931407 0.424303 0.887230 11.00000 0.09158 0.07021 = 0.10534 0.02203 -0.02809 -0.02404 C64 1 0.942003 0.384451 0.822396 11.00000 0.10004 0.07591 = 0.11242 0.00838 -0.00290 -0.01434 C65 1 0.859588 0.364401 0.802727 11.00000 0.10581 0.06745 = 0.10820 -0.00450 -0.00496 -0.03338 C66 1 0.835320 0.399231 0.730843 11.00000 0.11094 0.07209 = 0.10215 -0.01757 0.00964 -0.04077 C67 1 0.902493 0.441938 0.706355 11.00000 0.09144 0.08525 = 0.09287 -0.03005 0.01462 -0.02254 C68 1 0.859881 0.536726 0.654628 11.00000 0.09052 0.08892 = 0.07448 -0.03382 0.01674 -0.03535 C69 1 0.908674 0.591646 0.653414 11.00000 0.07895 0.10566 = 0.08058 -0.02821 0.03219 -0.04241 C70 1 0.982990 0.578858 0.711329 11.00000 0.05749 0.10889 = 0.09938 -0.02201 0.02659 -0.03567 C71 1 1.000154 0.512202 0.764885 11.00000 0.05350 0.09390 = 0.11078 -0.01659 0.01164 -0.02026 C72 1 0.969048 0.430538 0.762256 11.00000 0.08389 0.08762 = 0.11143 -0.01468 0.00973 -0.01483 PART 0 PART 2 DY1A 3 0.608430 0.821704 0.845132 10.60000 0.05037 0.03786 = 0.05559 -0.00912 0.00604 -0.01422 DY1B 3 0.782458 0.551516 0.798192 10.75000 0.04736 0.03265 = 0.05072 -0.00644 0.00104 -0.01622 DY2A 3 0.665701 0.826229 0.848702 10.30000 0.05015 0.04958 = 0.06729 -0.02179 -0.00020 -0.02279 DY2B 3 0.741359 0.555595 0.813569 10.20000 0.07569 0.04655 = 0.07149 0.00295 -0.01354 -0.03334 DY3A 3 0.721664 0.823178 0.812540 10.10000 0.07383 0.06953 = 0.13218 -0.03008 0.03439 -0.04940 DY3B 3 0.674370 0.590995 0.851165 10.05000 0.08814 0.06197 = 0.07691 -0.00198 0.01151 -0.03832 O1 6 0.723769 0.704254 0.797618 11.00000 0.04897 0.03318 = 0.05857 -0.00993 -0.00089 -0.01260 PART 0 PART 3 NI1P 5 0.521076 0.517007 0.586913 11.00000 0.02264 0.02435 = 0.03617 -0.00423 0.00479 -0.01089 N1P 4 0.466818 0.461649 0.665903 11.00000 0.02328 0.02470 = 0.04441 -0.00412 0.00379 -0.01061 N2P 4 0.391514 0.649529 0.585453 11.00000 0.02687 0.02793 = 0.03834 -0.00492 0.00364 -0.01374 N3P 4 0.578225 0.573991 0.510868 11.00000 0.02476 0.02597 = 0.03671 -0.00426 0.00400 -0.01183 N4P 4 0.653217 0.386310 0.591253 11.00000 0.02793 0.02735 = 0.03804 -0.00581 0.00569 -0.01421 C1P 1 0.515950 0.366828 0.702502 11.00000 0.03245 0.03007 = 0.04005 -0.00337 0.00273 -0.01707 C2P 1 0.453669 0.357212 0.760735 11.00000 0.03172 0.03253 = 0.05041 0.00136 0.00486 -0.01593 C3P 1 0.489853 0.265062 0.813067 11.00000 0.04194 0.04078 = 0.05840 0.01075 0.01265 -0.01673 AFIX 23 H3PA 2 0.523543 0.201581 0.787837 11.00000 -1.20000 H3PB 2 0.427727 0.266310 0.837777 11.00000 -1.20000 AFIX 0 C4P 1 0.567292 0.260742 0.866890 11.00000 0.04676 0.05771 = 0.04854 0.00538 0.00727 -0.01683 AFIX 137 H4PA 2 0.630205 0.256935 0.842974 11.00000 -1.50000 H4PB 2 0.587415 0.199519 0.899951 11.00000 -1.50000 H4PC 2 0.534250 0.322984 0.892493 11.00000 -1.50000 AFIX 0 C5P 1 0.363742 0.448747 0.758774 11.00000 0.03374 0.03571 = 0.04518 -0.00206 0.00946 -0.01792 C6P 1 0.273218 0.484473 0.809887 11.00000 0.03401 0.04487 = 0.05469 0.00209 0.01640 -0.01680 AFIX 23 H6PA 2 0.274818 0.423632 0.837596 11.00000 -1.20000 H6PB 2 0.205696 0.520573 0.783450 11.00000 -1.20000 AFIX 0 C7P 1 0.279372 0.558048 0.860241 11.00000 0.05389 0.04509 = 0.04752 -0.00256 0.01600 -0.01386 AFIX 137 H7PA 2 0.276439 0.618969 0.832964 11.00000 -1.50000 H7PB 2 0.345665 0.522091 0.887008 11.00000 -1.50000 H7PC 2 0.219911 0.579688 0.892646 11.00000 -1.50000 AFIX 0 C8P 1 0.372547 0.511864 0.700394 11.00000 0.02763 0.03510 = 0.04118 -0.00761 0.00883 -0.01747 C9P 1 0.295484 0.611804 0.681411 11.00000 0.02373 0.03006 = 0.04522 -0.00549 0.00931 -0.01099 AFIX 43 H9P 2 0.231672 0.637705 0.707075 11.00000 -1.20000 AFIX 0 C10P 1 0.304637 0.676066 0.628249 11.00000 0.02458 0.03216 = 0.03995 -0.00737 0.00553 -0.01243 C11P 1 0.226924 0.782390 0.613019 11.00000 0.03032 0.02862 = 0.04661 -0.00515 0.00658 -0.01259 C12P 1 0.127314 0.836860 0.653488 11.00000 0.03025 0.03189 = 0.06560 -0.00117 0.01302 -0.00615 AFIX 23 H12A 2 0.093353 0.791910 0.660902 11.00000 -1.20000 H12B 2 0.078153 0.900784 0.625518 11.00000 -1.20000 AFIX 0 C13P 1 0.146853 0.864757 0.724702 11.00000 0.05478 0.04462 = 0.06238 -0.01843 0.02274 -0.01450 AFIX 137 H13A 2 0.178138 0.911297 0.717614 11.00000 -1.50000 H13B 2 0.195101 0.801700 0.752772 11.00000 -1.50000 H13C 2 0.079839 0.899151 0.749352 11.00000 -1.50000 AFIX 0 C14P 1 0.265628 0.821091 0.558874 11.00000 0.02642 0.02335 = 0.04859 -0.00343 0.00319 -0.00979 C15P 1 0.218010 0.928844 0.523249 11.00000 0.03549 0.02707 = 0.05719 -0.00039 0.00647 -0.00930 AFIX 23 H15A 2 0.141241 0.964141 0.532004 11.00000 -1.20000 H15B 2 0.228250 0.924901 0.471962 11.00000 -1.20000 AFIX 0 C16P 1 0.266703 0.992911 0.549092 11.00000 0.05455 0.03237 = 0.06236 -0.00986 0.01299 -0.02284 AFIX 137 H16A 2 0.237202 1.060300 0.521911 11.00000 -1.50000 H16B 2 0.343267 0.956445 0.542981 11.00000 -1.50000 H16C 2 0.250734 1.002899 0.598887 11.00000 -1.50000 AFIX 0 C17P 1 0.367495 0.738151 0.542195 11.00000 0.02586 0.02291 = 0.04111 -0.00320 0.00115 -0.01053 C18P 1 0.432171 0.748857 0.491588 11.00000 0.03182 0.02334 = 0.03791 -0.00239 0.00047 -0.01327 AFIX 43 H18P 2 0.406679 0.813337 0.464395 11.00000 -1.20000 AFIX 0 C19P 1 0.531135 0.672864 0.477536 11.00000 0.03049 0.02923 = 0.03451 -0.00150 0.00255 -0.01797 C20P 1 0.600520 0.687202 0.427178 11.00000 0.03161 0.03167 = 0.03756 -0.00234 0.00414 -0.01816 C21P 1 0.576969 0.787654 0.385831 11.00000 0.03888 0.03273 = 0.04012 -0.00025 0.00377 -0.01979 AFIX 23 H21A 2 0.502185 0.823112 0.370532 11.00000 -1.20000 H21B 2 0.621139 0.773285 0.343293 11.00000 -1.20000 AFIX 0 C22P 1 0.598139 0.858900 0.429035 11.00000 0.05764 0.04092 = 0.05558 0.00320 -0.00518 -0.03130 AFIX 137 H22A 2 0.588747 0.920302 0.399112 11.00000 -1.50000 H22B 2 0.670511 0.822032 0.447442 11.00000 -1.50000 H22C 2 0.548691 0.879908 0.468165 11.00000 -1.50000 AFIX 0 C23P 1 0.692141 0.595882 0.429420 11.00000 0.02901 0.03232 = 0.04162 -0.00824 0.00700 -0.01660 C24P 1 0.793183 0.571246 0.391446 11.00000 0.03012 0.03802 = 0.04720 -0.00862 0.01380 -0.01750 AFIX 23 H24A 2 0.778025 0.618017 0.348009 11.00000 -1.20000 H24B 2 0.825199 0.499441 0.377864 11.00000 -1.20000 AFIX 0 C25P 1 0.871196 0.583236 0.437248 11.00000 0.03628 0.06056 = 0.07331 -0.02484 0.02001 -0.02995 AFIX 137 H25A 2 0.934183 0.571605 0.409979 11.00000 -1.50000 H25B 2 0.891190 0.532628 0.478215 11.00000 -1.50000 H25C 2 0.838202 0.653158 0.452898 11.00000 -1.50000 AFIX 0 C26P 1 0.676781 0.526973 0.481181 11.00000 0.02928 0.03028 = 0.03930 -0.00772 0.00371 -0.01597 C27P 1 0.752248 0.426951 0.499162 11.00000 0.02130 0.03036 = 0.03943 -0.00827 0.00518 -0.01201 AFIX 43 H27P 2 0.816330 0.401610 0.473809 11.00000 -1.20000 AFIX 0 C28P 1 0.742755 0.360891 0.550507 11.00000 0.02468 0.03328 = 0.04201 -0.00922 0.00437 -0.01411 C29P 1 0.824215 0.258212 0.570504 11.00000 0.02909 0.03005 = 0.04788 -0.00796 0.00727 -0.01571 C30P 1 0.930818 0.210436 0.538309 11.00000 0.02967 0.02897 = 0.06160 -0.00740 0.00996 -0.00977 AFIX 23 H30A 2 0.923054 0.223230 0.486613 11.00000 -1.20000 H30B 2 0.965099 0.134765 0.550089 11.00000 -1.20000 AFIX 0 C31P 1 1.001769 0.252835 0.563310 11.00000 0.03082 0.04960 = 0.07527 -0.00749 0.00322 -0.01778 AFIX 137 H31A 2 0.971126 0.326732 0.548398 11.00000 -1.50000 H31B 2 1.071921 0.216136 0.542896 11.00000 -1.50000 H31C 2 1.007643 0.242755 0.614625 11.00000 -1.50000 AFIX 0 C32P 1 0.784589 0.218985 0.623791 11.00000 0.02952 0.02271 = 0.04718 -0.00400 0.00244 -0.00895 C33P 1 0.838626 0.116589 0.665889 11.00000 0.03762 0.02898 = 0.05619 0.00019 0.00347 -0.01110 AFIX 23 H33A 2 0.899565 0.068571 0.639183 11.00000 -1.20000 H33B 2 0.789147 0.087409 0.672688 11.00000 -1.20000 AFIX 0 C34P 1 0.877403 0.123899 0.738085 11.00000 0.04113 0.04266 = 0.06118 0.00700 -0.00707 -0.01340 AFIX 137 H34A 2 0.931177 0.146865 0.731716 11.00000 -1.50000 H34B 2 0.907757 0.055889 0.764481 11.00000 -1.50000 H34C 2 0.817983 0.173599 0.764058 11.00000 -1.50000 AFIX 0 C35P 1 0.678787 0.299011 0.635941 11.00000 0.02421 0.02703 = 0.04162 -0.00335 0.00128 -0.01107 C36P 1 0.614128 0.289126 0.687321 11.00000 0.02738 0.02392 = 0.03940 0.00063 0.00077 -0.01029 AFIX 43 H36P 2 0.638829 0.224407 0.714115 11.00000 -1.20000 AFIX 0 C1S 1 0.217390 1.209192 0.843481 11.00000 0.06744 0.07664 = 0.05053 -0.01218 0.00444 -0.04079 AFIX 43 H1S 2 0.234662 1.240635 0.878576 11.00000 -1.20000 AFIX 0 C2S 1 0.177196 1.140037 0.862939 11.00000 0.07918 0.10380 = 0.04514 -0.00485 0.00952 -0.05491 AFIX 43 H2S 2 0.168686 1.123199 0.911022 11.00000 -1.20000 AFIX 0 C3S 1 0.150416 1.097196 0.811100 11.00000 0.06332 0.07394 = 0.06054 -0.00496 0.00347 -0.04265 AFIX 43 H3S 2 0.124551 1.049362 0.823609 11.00000 -1.20000 AFIX 0 C4S 1 0.160645 1.122735 0.742001 11.00000 0.05200 0.05958 = 0.05034 -0.01379 0.00296 -0.02641 AFIX 43 H4S 2 0.139637 1.094288 0.706858 11.00000 -1.20000 AFIX 0 C5S 1 0.200509 1.188335 0.722953 11.00000 0.05194 0.05725 = 0.04228 -0.00409 0.00446 -0.02393 AFIX 43 H5S 2 0.207603 1.205568 0.674708 11.00000 -1.20000 AFIX 0 C6S 1 0.231442 1.230929 0.775215 11.00000 0.05721 0.06229 = 0.05460 -0.00600 0.00523 -0.02916 AFIX 43 H6S 2 0.262037 1.274734 0.762278 11.00000 -1.20000 AFIX 0 C7S 1 0.200888 0.900271 0.992241 11.00000 0.07648 0.13704 = 0.08926 -0.00514 0.00425 -0.07359 AFIX 43 H7S 2 0.249363 0.927194 0.986794 11.00000 -1.20000 AFIX 0 C8S 1 0.150501 0.904266 1.054124 11.00000 0.06414 0.07172 = 0.06280 -0.00685 -0.00565 -0.03215 AFIX 43 H8S 2 0.164692 0.932886 1.092411 11.00000 -1.20000 AFIX 0 C9S 1 0.079326 0.867107 1.061367 11.00000 0.07384 0.08614 = 0.05693 -0.00199 0.00844 -0.03910 AFIX 43 H9S 2 0.043472 0.871229 1.104537 11.00000 -1.20000 AFIX 0 C10S 1 0.058946 0.823596 1.006565 11.00000 0.07162 0.06570 = 0.07906 0.00466 -0.01025 -0.04101 AFIX 43 H10S 2 0.009920 0.797371 1.012348 11.00000 -1.20000 AFIX 0 C11S 1 0.110395 0.818322 0.942964 11.00000 0.05531 0.07547 = 0.08465 -0.02702 -0.00008 -0.02684 AFIX 43 H11S 2 0.096725 0.788998 0.904871 11.00000 -1.20000 AFIX 0 C12S 1 0.180844 0.856062 0.936345 11.00000 0.06166 0.12985 = 0.06776 -0.02135 0.01851 -0.04440 AFIX 43 H12S 2 0.216877 0.852389 0.893299 11.00000 -1.20000 AFIX 0 HKLF 5 REM a_a_a.res in P-1 REM R1 = 0.0953 for 11767 Fo > 4sig(Fo) and 0.1011 for all 12960 data REM 1198 parameters refined using 963 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.992, deepest hole -1.070, 1-sigma level 0.185 Q1 1 0.7755 0.7190 0.7236 11.00000 0.05 1.99 Q2 1 0.8350 0.6118 0.9789 11.00000 0.05 1.60 Q3 1 0.5167 0.5159 0.5557 11.00000 0.05 1.36 Q4 1 0.4815 0.8702 0.6813 11.00000 0.05 1.34 Q5 1 0.5792 0.5534 0.7441 11.00000 0.05 1.30 Q6 1 0.9403 0.6630 0.6691 11.00000 0.05 1.30 Q7 1 0.6123 0.6467 0.8467 11.00000 0.05 1.28 Q8 1 0.7925 0.5678 0.8463 11.00000 0.05 1.27 Q9 1 0.5864 1.0168 0.7952 11.00000 0.05 1.26 Q10 1 0.9821 0.4578 0.8266 11.00000 0.05 1.24 Q11 1 0.7433 0.9293 0.7055 11.00000 0.05 1.21 Q12 1 0.7354 0.5239 0.9692 11.00000 0.05 1.21 Q13 1 0.5588 0.7769 0.7839 11.00000 0.05 1.21 Q14 1 0.6332 0.9433 0.6775 11.00000 0.05 1.17 Q15 1 0.6343 0.4803 0.8740 11.00000 0.05 1.17 Q16 1 0.7555 0.5005 0.9598 11.00000 0.05 1.16 Q17 1 0.7439 0.5169 0.6690 11.00000 0.05 1.12 Q18 1 0.5107 1.0095 0.8609 11.00000 0.05 1.07 Q19 1 0.4189 0.8190 0.8090 11.00000 0.05 1.07 Q20 1 0.6800 0.9668 0.8977 11.00000 0.05 1.07 REM The information below was added by Olex2. REM REM R1 = 0.0953 for 11767 Fo > 4sig(Fo) and 0.1011 for all 12967 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.99, deepest hole -1.07 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1011 REM R1_gt = 0.0953 REM wR_ref = 0.2800 REM GOOF = 1.049 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 12967 REM Reflections_gt = 11767 REM Parameters = n/a REM Hole = -1.07 REM Peak = 1.99 REM Flack = n/a ; _cod_data_source_file d0sc00624f2.cif _cod_data_source_block a_a_tw _cod_depositor_comments ;Adding full bibliography for 1557826--1557827.cif. Adding full bibliography for 1557826--1557827.cif. ; _cod_database_code 1557826 _shelx_shelxl_version_number 2018/1 _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_max 0.382 _shelx_estimated_absorpt_t_min 0.268 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.686(5) 0.314(5) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances C23-C22 1.38 with sigma of 0.02 C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-C1 with sigma of 0.02 C1-C3 \\sim C1-C4 \\sim C2-C4 \\sim C2-C5 \\sim C3-C5 with sigma of 0.02 C1-C5 \\sim C5-C6 \\sim C6-C7 \\sim C7-C8 \\sim C8-C1 with sigma of 0.02 C1-C6 \\sim C1-C7 \\sim C5-C7 \\sim C5-C8 \\sim C6-C8 with sigma of 0.02 C25-C26 \\sim C26-C10 \\sim C10-C9 \\sim C9-C24 \\sim C24-C25 with sigma of 0.02 C25-C10 \\sim C25-C9 \\sim C26-C9 \\sim C26-C24 \\sim C10-C24 with sigma of 0.02 C15-C32 \\sim C32-C33 \\sim C33-C34 \\sim C34-C16 \\sim C16-C15 with sigma of 0.02 C15-C33 \\sim C15-C34 \\sim C32-C34 \\sim C32-C16 \\sim C33-C16 with sigma of 0.02 C20-C38 \\sim C38-C39 \\sim C39-C40 \\sim C40-C21 \\sim C21-C20 with sigma of 0.02 C20-C39 \\sim C20-C40 \\sim C38-C40 \\sim C38-C21 \\sim C39-C21 with sigma of 0.02 C42-C41 \\sim C41-C59 \\sim C59-C60 \\sim C60-C43 \\sim C43-C42 with sigma of 0.02 C42-C59 \\sim C42-C60 \\sim C41-C60 \\sim C41-C43 \\sim C59-C43 with sigma of 0.02 C46-C45 \\sim C45-C62 \\sim C62-C63 \\sim C63-C47 \\sim C47-C46 with sigma of 0.02 C46-C62 \\sim C46-C63 \\sim C45-C63 \\sim C45-C47 \\sim C62-C47 with sigma of 0.02 C70-C58 \\sim C58-C57 \\sim C57-C56 \\sim C56-C69 \\sim C69-C70 with sigma of 0.02 C70-C57 \\sim C70-C56 \\sim C58-C56 \\sim C58-C69 \\sim C57-C69 with sigma of 0.02 C55-C37 \\sim C37-C36 \\sim C36-C35 \\sim C35-C54 \\sim C54-C55 with sigma of 0.02 C55-C36 \\sim C55-C35 \\sim C37-C35 \\sim C37-C54 \\sim C36-C54 with sigma of 0.02 C13-C12 \\sim C12-C28 \\sim C28-C29 \\sim C29-C30 \\sim C30-C13 with sigma of 0.02 C13-C28 \\sim C13-C29 \\sim C12-C29 \\sim C12-C30 \\sim C28-C30 with sigma of 0.02 C65-C64 \\sim C64-C72 \\sim C72-C67 \\sim C67-C66 \\sim C66-C65 with sigma of 0.02 C65-C72 \\sim C65-C67 \\sim C64-C67 \\sim C64-C66 \\sim C72-C66 with sigma of 0.02 C65-C66 \\sim C66-C51 \\sim C51-C50 \\sim C50-C49 \\sim C49-C65 with sigma of 0.02 C65-C51 \\sim C65-C50 \\sim C66-C50 \\sim C66-C49 \\sim C51-C49 with sigma of 0.02 4. Restrained planarity C9, C10, C24, C25, C26 with sigma of 0.1 C15, C16, C32, C33, C34 with sigma of 0.1 C20, C21, C38, C39, C40 with sigma of 0.1 C41, C42, C43, C59, C60 with sigma of 0.1 C45, C46, C47, C62, C63 with sigma of 0.1 C56, C57, C58, C69, C70 with sigma of 0.1 C35, C36, C37, C54, C55 with sigma of 0.1 C12, C13, C28, C29, C30 with sigma of 0.1 C1, C2, C3, C4, C5 with sigma of 0.1 C1, C5, C6, C7, C8 with sigma of 0.1 C64, C65, C66, C67, C72 with sigma of 0.1 C49, C50, C51, C65, C66 with sigma of 0.1 5. Uiso/Uaniso restraints and constraints C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72: within 2A with sigma of 0.008 and sigma for terminal atoms of 0.016 Dy1B \\sim Dy2B \\sim Dy3B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 6. Others Fixed Sof: Dy1A(0.6) Dy1B(0.75) Dy2A(0.3) Dy2B(0.2) Dy3A(0.1) Dy3B(0.05) 7.a Secondary CH2 refined with riding coordinates: C3P(H3PA,H3PB), C6P(H6PA,H6PB), C12P(H12A,H12B), C15P(H15A,H15B), C21P(H21A, H21B), C24P(H24A,H24B), C30P(H30A,H30B), C33P(H33A,H33B) 7.b Aromatic/amide H refined with riding coordinates: C9P(H9P), C18P(H18P), C27P(H27P), C36P(H36P), C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C7S(H7S), C8S(H8S), C9S(H9S), C10S(H10S), C11S(H11S), C12S(H12S) 7.c Idealised Me refined as rotating group: C4P(H4PA,H4PB,H4PC), C7P(H7PA,H7PB,H7PC), C13P(H13A,H13B,H13C), C16P(H16A, H16B,H16C), C22P(H22A,H22B,H22C), C25P(H25A,H25B,H25C), C31P(H31A,H31B,H31C), C34P(H34A,H34B,H34C) ; _olex2_submission_special_instructions 'No special instructions were received' 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4690(10) 0.9544(11) 0.9017(6) 0.110(3) Uani 1 1 d D U . A 1 C2 C 0.4516(11) 0.8673(11) 0.9187(6) 0.106(3) Uani 1 1 d D U . A 1 C3 C 0.4171(11) 0.8451(11) 0.8549(7) 0.099(3) Uani 1 1 d D U . A 1 C4 C 0.4203(12) 0.9162(11) 0.7998(7) 0.102(3) Uani 1 1 d D U . A 1 C5 C 0.4482(10) 0.9854(10) 0.8292(7) 0.108(3) Uani 1 1 d D U . A 1 C6 C 0.5288(11) 1.0106(10) 0.8018(7) 0.102(3) Uani 1 1 d D U . A 1 C7 C 0.5965(11) 0.9964(11) 0.8582(7) 0.100(3) Uani 1 1 d D U . A 1 C8 C 0.5612(12) 0.9622(12) 0.9204(7) 0.105(3) Uani 1 1 d D U . A 1 C9 C 0.6311(10) 0.8799(9) 0.9656(7) 0.094(3) Uani 1 1 d D U . A 1 C10 C 0.6134(10) 0.7950(11) 0.9910(7) 0.099(3) Uani 1 1 d D U . A 1 C11 C 0.5170(13) 0.7893(14) 0.9608(8) 0.099(3) Uani 1 1 d . U . A 1 C12 C 0.5408(10) 0.6854(10) 0.9545(6) 0.097(3) Uani 1 1 d D U . A 1 C13 C 0.4949(9) 0.6622(10) 0.8959(7) 0.093(3) Uani 1 1 d D U . A 1 C14 C 0.4371(11) 0.7486(14) 0.8452(9) 0.095(3) Uani 1 1 d . U . A 1 C15 C 0.4526(8) 0.7179(10) 0.7726(6) 0.088(2) Uani 1 1 d D U . A 1 C16 C 0.4601(8) 0.7864(9) 0.7140(6) 0.085(2) Uani 1 1 d D U . A 1 C17 C 0.4522(12) 0.8905(14) 0.7306(9) 0.103(3) Uani 1 1 d . U . A 1 C18 C 0.5219(13) 0.9199(13) 0.6945(9) 0.101(3) Uani 1 1 d . U . A 1 C19 C 0.5600(13) 0.9814(10) 0.7303(8) 0.087(3) Uani 1 1 d . U . A 1 C20 C 0.6680(10) 0.9640(9) 0.7161(7) 0.098(3) Uani 1 1 d D U . A 1 C21 C 0.7398(10) 0.9523(9) 0.7718(6) 0.088(2) Uani 1 1 d D U . A 1 C22 C 0.7075(13) 0.9582(11) 0.8432(9) 0.094(3) Uani 1 1 d D U . A 1 C23 C 0.7795(12) 0.8837(11) 0.8983(8) 0.087(2) Uani 1 1 d D U . A 1 C24 C 0.7439(10) 0.8407(10) 0.9568(6) 0.089(3) Uani 1 1 d D U . A 1 C25 C 0.7951(9) 0.7324(10) 0.9791(7) 0.088(3) Uani 1 1 d D U . A 1 C26 C 0.7118(11) 0.7048(10) 1.0012(6) 0.094(3) Uani 1 1 d D U . A 1 C27 C 0.7355(14) 0.6070(13) 0.9933(7) 0.094(3) Uani 1 1 d . U . A 1 C28 C 0.6376(10) 0.5962(10) 0.9733(6) 0.086(3) Uani 1 1 d D U . A 1 C29 C 0.6525(10) 0.5171(9) 0.9290(7) 0.098(3) Uani 1 1 d D U . A 1 C30 C 0.5660(10) 0.5580(10) 0.8814(6) 0.089(2) Uani 1 1 d D U . A 1 C31 C 0.5785(12) 0.5303(12) 0.8076(8) 0.088(2) Uani 1 1 d . U . A 1 C32 C 0.5252(9) 0.6099(9) 0.7585(6) 0.083(2) Uani 1 1 d D U . A 1 C33 C 0.5798(9) 0.6113(9) 0.6907(6) 0.081(2) Uani 1 1 d D U . A 1 C34 C 0.5368(9) 0.7204(9) 0.6635(6) 0.082(2) Uani 1 1 d D U . A 1 C35 C 0.5895(9) 0.7580(9) 0.6269(6) 0.078(2) Uani 1 1 d D U . A 1 C36 C 0.5796(9) 0.8596(9) 0.6380(6) 0.089(3) Uani 1 1 d D U . A 1 C37 C 0.6852(10) 0.8537(9) 0.6251(6) 0.088(3) Uani 1 1 d D U . A 1 C38 C 0.7280(11) 0.9027(10) 0.6621(6) 0.102(3) Uani 1 1 d D U . A 1 C39 C 0.8368(10) 0.8514(10) 0.6821(7) 0.093(3) Uani 1 1 d D U . A 1 C40 C 0.8438(10) 0.8828(11) 0.7509(7) 0.095(3) Uani 1 1 d D U . A 1 C41 C 0.9078(9) 0.8161(9) 0.7973(6) 0.085(2) Uani 1 1 d D U . A 1 C42 C 0.8801(9) 0.8123(8) 0.8718(6) 0.078(2) Uani 1 1 d D U . A 1 C43 C 0.9327(8) 0.7049(9) 0.8998(6) 0.076(2) Uani 1 1 d D U . A 1 C44 C 0.8857(11) 0.6722(12) 0.9522(7) 0.085(2) Uani 1 1 d . U . A 1 C45 C 0.9085(10) 0.5599(10) 0.9487(6) 0.088(3) Uani 1 1 d D U . A 1 C46 C 0.8290(10) 0.5319(10) 0.9709(6) 0.095(3) Uani 1 1 d D U . A 1 C47 C 0.8422(11) 0.4478(10) 0.9313(7) 0.096(3) Uani 1 1 d D U . A 1 C48 C 0.7549(15) 0.4357(12) 0.9039(9) 0.102(3) Uani 1 1 d . U . A 1 C49 C 0.7631(10) 0.3971(10) 0.8396(6) 0.093(3) Uani 1 1 d D U . A 1 C50 C 0.6784(9) 0.4495(9) 0.7887(6) 0.086(2) Uani 1 1 d D U . A 1 C51 C 0.7261(10) 0.4521(10) 0.7225(6) 0.093(3) Uani 1 1 d D U . A 1 C52 C 0.6815(13) 0.5442(11) 0.6747(7) 0.084(2) Uani 1 1 d . U . A 1 C53 C 0.7477(12) 0.5796(11) 0.6362(7) 0.082(2) Uani 1 1 d . U . A 1 C54 C 0.6985(9) 0.6883(9) 0.6084(6) 0.077(2) Uani 1 1 d D U . A 1 C55 C 0.7586(9) 0.7469(10) 0.6058(6) 0.087(3) Uani 1 1 d D U . A 1 C56 C 0.8602(10) 0.6981(10) 0.6262(6) 0.091(3) Uani 1 1 d D U . A 1 C57 C 0.9010(9) 0.7540(10) 0.6671(6) 0.088(2) Uani 1 1 d D U . A 1 C58 C 0.9750(9) 0.6782(10) 0.7182(7) 0.090(3) Uani 1 1 d D U . A 1 C59 C 0.9786(9) 0.7081(9) 0.7805(6) 0.083(2) Uani 1 1 d D U . A 1 C60 C 0.9916(8) 0.6402(9) 0.8440(6) 0.082(2) Uani 1 1 d D U . A 1 C61 C 1.0054(10) 0.5401(13) 0.8380(9) 0.094(3) Uani 1 1 d . U . A 1 C62 C 0.9673(9) 0.4987(10) 0.8951(7) 0.092(3) Uani 1 1 d D U . A 1 C63 C 0.9314(10) 0.4243(9) 0.8872(7) 0.096(3) Uani 1 1 d D U . A 1 C64 C 0.9420(11) 0.3845(11) 0.8224(7) 0.108(3) Uani 1 1 d D U . A 1 C65 C 0.8596(8) 0.3644(9) 0.8027(6) 0.097(3) Uani 1 1 d D U . A 1 C66 C 0.8353(9) 0.3992(10) 0.7308(6) 0.096(3) Uani 1 1 d D U . A 1 C67 C 0.9025(11) 0.4419(11) 0.7064(6) 0.096(3) Uani 1 1 d D U . A 1 C68 C 0.8599(12) 0.5367(12) 0.6546(7) 0.086(3) Uani 1 1 d . U . A 1 C69 C 0.9087(10) 0.5916(10) 0.6534(6) 0.088(3) Uani 1 1 d D U . A 1 C70 C 0.9830(9) 0.5789(10) 0.7113(7) 0.090(3) Uani 1 1 d D U . A 1 C71 C 1.0002(10) 0.5122(13) 0.7649(9) 0.092(3) Uani 1 1 d . U . A 1 C72 C 0.9690(10) 0.4305(12) 0.7623(7) 0.104(3) Uani 1 1 d D U . A 1 Dy1A Dy 0.60843(10) 0.82170(7) 0.84513(5) 0.0504(3) Uani 0.6 1 d . . P B 2 Dy1B Dy 0.78246(9) 0.55152(9) 0.79819(6) 0.0444(3) Uani 0.75 1 d . U P B 2 Dy2A Dy 0.6657(2) 0.82623(16) 0.84870(12) 0.0548(5) Uani 0.3 1 d . . P B 2 Dy2B Dy 0.7414(5) 0.5556(4) 0.8136(3) 0.0629(13) Uani 0.2 1 d . U P B 2 Dy3A Dy 0.7217(7) 0.8232(6) 0.8125(6) 0.085(2) Uani 0.1 1 d . . P B 2 Dy3B Dy 0.6744(15) 0.5910(12) 0.8512(9) 0.075(3) Uani 0.05 1 d . U P B 2 O1 O 0.7238(5) 0.7043(4) 0.7976(3) 0.0492(14) Uani 1 1 d . . . B 2 Ni1P Ni 0.52108(8) 0.51701(8) 0.58691(6) 0.0278(3) Uani 1 1 d . . . C 3 N1P N 0.4668(4) 0.4616(4) 0.6659(3) 0.0311(12) Uani 1 1 d . . . C 3 N2P N 0.3915(4) 0.6495(4) 0.5855(3) 0.0306(12) Uani 1 1 d . . . C 3 N3P N 0.5782(4) 0.5740(4) 0.5109(3) 0.0292(12) Uani 1 1 d . . . C 3 N4P N 0.6532(4) 0.3863(4) 0.5913(3) 0.0305(12) Uani 1 1 d . . . C 3 C1P C 0.5160(6) 0.3668(6) 0.7025(4) 0.0333(15) Uani 1 1 d . . . C 3 C2P C 0.4537(6) 0.3572(6) 0.7607(4) 0.0383(16) Uani 1 1 d . . . C 3 C3P C 0.4899(7) 0.2651(7) 0.8131(5) 0.049(2) Uani 1 1 d . . . C 3 H3PA H 0.523543 0.201581 0.787837 0.059 Uiso 1 1 calc R . . C 3 H3PB H 0.427727 0.266310 0.837777 0.059 Uiso 1 1 calc R . . C 3 C4P C 0.5673(7) 0.2607(8) 0.8669(5) 0.055(2) Uani 1 1 d . . . C 3 H4PA H 0.630205 0.256935 0.842974 0.082 Uiso 1 1 calc GR . . C 3 H4PB H 0.587415 0.199519 0.899951 0.082 Uiso 1 1 calc GR . . C 3 H4PC H 0.534250 0.322984 0.892493 0.082 Uiso 1 1 calc GR . . C 3 C5P C 0.3637(6) 0.4487(6) 0.7588(4) 0.0379(16) Uani 1 1 d . . . C 3 C6P C 0.2732(6) 0.4845(7) 0.8099(5) 0.0461(19) Uani 1 1 d . . . C 3 H6PA H 0.274818 0.423632 0.837596 0.055 Uiso 1 1 calc R . . C 3 H6PB H 0.205696 0.520573 0.783450 0.055 Uiso 1 1 calc R . . C 3 C7P C 0.2794(8) 0.5580(7) 0.8602(5) 0.053(2) Uani 1 1 d . . . C 3 H7PA H 0.276439 0.618969 0.832964 0.080 Uiso 1 1 calc GR . . C 3 H7PB H 0.345665 0.522091 0.887008 0.080 Uiso 1 1 calc GR . . C 3 H7PC H 0.219911 0.579688 0.892646 0.080 Uiso 1 1 calc GR . . C 3 C8P C 0.3725(5) 0.5119(6) 0.7004(4) 0.0335(15) Uani 1 1 d . . . C 3 C9P C 0.2955(5) 0.6118(6) 0.6814(4) 0.0337(15) Uani 1 1 d . . . C 3 H9P H 0.231672 0.637705 0.707075 0.040 Uiso 1 1 calc R . . C 3 C10P C 0.3046(5) 0.6761(6) 0.6282(4) 0.0324(14) Uani 1 1 d . . . C 3 C11P C 0.2269(6) 0.7824(6) 0.6130(4) 0.0357(15) Uani 1 1 d . . . C 3 C12P C 0.1273(6) 0.8369(6) 0.6535(5) 0.0465(19) Uani 1 1 d . . . C 3 H12A H 0.093353 0.791910 0.660902 0.056 Uiso 1 1 calc R . . C 3 H12B H 0.078153 0.900784 0.625518 0.056 Uiso 1 1 calc R . . C 3 C13P C 0.1469(8) 0.8648(8) 0.7247(5) 0.057(2) Uani 1 1 d . . . C 3 H13A H 0.178138 0.911297 0.717614 0.086 Uiso 1 1 calc GR . . C 3 H13B H 0.195101 0.801700 0.752772 0.086 Uiso 1 1 calc GR . . C 3 H13C H 0.079839 0.899151 0.749352 0.086 Uiso 1 1 calc GR . . C 3 C14P C 0.2656(5) 0.8211(5) 0.5589(4) 0.0336(15) Uani 1 1 d . . . C 3 C15P C 0.2180(6) 0.9288(6) 0.5232(5) 0.0425(18) Uani 1 1 d . . . C 3 H15A H 0.141241 0.964141 0.532004 0.051 Uiso 1 1 calc R . . C 3 H15B H 0.228250 0.924901 0.471962 0.051 Uiso 1 1 calc R . . C 3 C16P C 0.2667(7) 0.9929(6) 0.5491(5) 0.049(2) Uani 1 1 d . . . C 3 H16A H 0.237202 1.060300 0.521911 0.073 Uiso 1 1 calc GR . . C 3 H16B H 0.343267 0.956445 0.542981 0.073 Uiso 1 1 calc GR . . C 3 H16C H 0.250734 1.002899 0.598887 0.073 Uiso 1 1 calc GR . . C 3 C17P C 0.3675(5) 0.7382(5) 0.5422(4) 0.0303(14) Uani 1 1 d . . . C 3 C18P C 0.4322(5) 0.7489(5) 0.4916(4) 0.0309(14) Uani 1 1 d . . . C 3 H18P H 0.406679 0.813337 0.464395 0.037 Uiso 1 1 calc R . . C 3 C19P C 0.5311(5) 0.6729(5) 0.4775(4) 0.0300(14) Uani 1 1 d . . . C 3 C20P C 0.6005(6) 0.6872(6) 0.4272(4) 0.0324(14) Uani 1 1 d . . . C 3 C21P C 0.5770(6) 0.7877(6) 0.3858(4) 0.0363(15) Uani 1 1 d . . . C 3 H21A H 0.502185 0.823112 0.370532 0.044 Uiso 1 1 calc R . . C 3 H21B H 0.621139 0.773285 0.343293 0.044 Uiso 1 1 calc R . . C 3 C22P C 0.5981(8) 0.8589(7) 0.4290(5) 0.048(2) Uani 1 1 d . . . C 3 H22A H 0.588747 0.920302 0.399112 0.073 Uiso 1 1 calc GR . . C 3 H22B H 0.670511 0.822032 0.447442 0.073 Uiso 1 1 calc GR . . C 3 H22C H 0.548691 0.879908 0.468165 0.073 Uiso 1 1 calc GR . . C 3 C23P C 0.6921(5) 0.5959(6) 0.4294(4) 0.0333(15) Uani 1 1 d . . . C 3 C24P C 0.7932(6) 0.5712(6) 0.3914(4) 0.0378(16) Uani 1 1 d . . . C 3 H24A H 0.778025 0.618017 0.348009 0.045 Uiso 1 1 calc R . . C 3 H24B H 0.825199 0.499441 0.377864 0.045 Uiso 1 1 calc R . . C 3 C25P C 0.8712(7) 0.5832(8) 0.4372(5) 0.053(2) Uani 1 1 d . . . C 3 H25A H 0.934183 0.571605 0.409979 0.079 Uiso 1 1 calc GR . . C 3 H25B H 0.891190 0.532628 0.478215 0.079 Uiso 1 1 calc GR . . C 3 H25C H 0.838202 0.653158 0.452898 0.079 Uiso 1 1 calc GR . . C 3 C26P C 0.6768(5) 0.5270(6) 0.4812(4) 0.0319(14) Uani 1 1 d . . . C 3 C27P C 0.7522(5) 0.4270(5) 0.4992(4) 0.0302(14) Uani 1 1 d . . . C 3 H27P H 0.816330 0.401610 0.473809 0.036 Uiso 1 1 calc R . . C 3 C28P C 0.7428(5) 0.3609(6) 0.5505(4) 0.0328(15) Uani 1 1 d . . . C 3 C29P C 0.8242(6) 0.2582(6) 0.5705(4) 0.0348(15) Uani 1 1 d . . . C 3 C30P C 0.9308(6) 0.2104(6) 0.5383(5) 0.0417(18) Uani 1 1 d . . . C 3 H30A H 0.923054 0.223230 0.486613 0.050 Uiso 1 1 calc R . . C 3 H30B H 0.965099 0.134765 0.550089 0.050 Uiso 1 1 calc R . . C 3 C31P C 1.0018(7) 0.2528(7) 0.5633(6) 0.052(2) Uani 1 1 d . . . C 3 H31A H 0.971126 0.326732 0.548398 0.078 Uiso 1 1 calc GR . . C 3 H31B H 1.071921 0.216136 0.542896 0.078 Uiso 1 1 calc GR . . C 3 H31C H 1.007643 0.242755 0.614625 0.078 Uiso 1 1 calc GR . . C 3 C32P C 0.7846(6) 0.2190(5) 0.6238(4) 0.0345(15) Uani 1 1 d . . . C 3 C33P C 0.8386(6) 0.1166(6) 0.6659(5) 0.0431(18) Uani 1 1 d . . . C 3 H33A H 0.899565 0.068571 0.639183 0.052 Uiso 1 1 calc R . . C 3 H33B H 0.789147 0.087409 0.672688 0.052 Uiso 1 1 calc R . . C 3 C34P C 0.8774(7) 0.1239(7) 0.7381(5) 0.051(2) Uani 1 1 d . . . C 3 H34A H 0.931177 0.146865 0.731716 0.077 Uiso 1 1 calc GR . . C 3 H34B H 0.907757 0.055889 0.764481 0.077 Uiso 1 1 calc GR . . C 3 H34C H 0.817983 0.173599 0.764058 0.077 Uiso 1 1 calc GR . . C 3 C35P C 0.6788(5) 0.2990(5) 0.6359(4) 0.0313(14) Uani 1 1 d . . . C 3 C36P C 0.6141(5) 0.2891(5) 0.6873(4) 0.0312(14) Uani 1 1 d . . . C 3 H36P H 0.638829 0.224407 0.714115 0.037 Uiso 1 1 calc R . . C 3 C1S C 0.2174(9) 1.2092(9) 0.8435(5) 0.062(2) Uani 1 1 d . . . D 3 H1S H 0.234662 1.240635 0.878576 0.074 Uiso 1 1 calc R . . D 3 C2S C 0.1772(10) 1.1400(11) 0.8629(6) 0.072(3) Uani 1 1 d . . . D 3 H2S H 0.168686 1.123199 0.911022 0.086 Uiso 1 1 calc R . . D 3 C3S C 0.1504(9) 1.0972(9) 0.8111(6) 0.062(2) Uani 1 1 d . . . D 3 H3S H 0.124551 1.049362 0.823609 0.074 Uiso 1 1 calc R . . D 3 C4S C 0.1606(8) 1.1227(8) 0.7420(5) 0.053(2) Uani 1 1 d . . . D 3 H4S H 0.139637 1.094288 0.706858 0.064 Uiso 1 1 calc R . . D 3 C5S C 0.2005(7) 1.1883(8) 0.7230(5) 0.051(2) Uani 1 1 d . . . D 3 H5S H 0.207603 1.205568 0.674708 0.062 Uiso 1 1 calc R . . D 3 C6S C 0.2314(8) 1.2309(8) 0.7752(5) 0.058(2) Uani 1 1 d . . . D 3 H6S H 0.262037 1.274734 0.762278 0.069 Uiso 1 1 calc R . . D 3 C7S C 0.2009(11) 0.9003(14) 0.9922(8) 0.092(4) Uani 1 1 d . . . E 3 H7S H 0.249363 0.927194 0.986794 0.110 Uiso 1 1 calc R . . E 3 C8S C 0.1505(9) 0.9043(9) 1.0541(6) 0.066(3) Uani 1 1 d . . . E 3 H8S H 0.164692 0.932886 1.092411 0.079 Uiso 1 1 calc R . . E 3 C9S C 0.0793(10) 0.8671(10) 1.0614(6) 0.072(3) Uani 1 1 d . . . E 3 H9S H 0.043472 0.871229 1.104537 0.087 Uiso 1 1 calc R . . E 3 C10S C 0.0589(10) 0.8236(9) 1.0066(6) 0.069(3) Uani 1 1 d . . . E 3 H10S H 0.009920 0.797371 1.012348 0.083 Uiso 1 1 calc R . . E 3 C11S C 0.1104(9) 0.8183(10) 0.9430(7) 0.072(3) Uani 1 1 d . . . E 3 H11S H 0.096725 0.788998 0.904871 0.086 Uiso 1 1 calc R . . E 3 C12S C 0.1808(10) 0.8561(13) 0.9363(7) 0.086(4) Uani 1 1 d . . . E 3 H12S H 0.216877 0.852389 0.893299 0.103 Uiso 1 1 calc R . . E 3 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 C1 0.100(5) 0.097(5) 0.114(5) -0.017(5) 0.013(5) -0.030(5) C2 0.090(5) 0.108(5) 0.099(5) -0.016(5) 0.025(5) -0.030(5) C3 0.071(5) 0.104(5) 0.111(5) -0.008(5) 0.013(4) -0.034(4) C4 0.078(5) 0.094(5) 0.110(5) -0.004(5) 0.002(5) -0.022(4) C5 0.097(5) 0.085(5) 0.118(5) -0.011(5) 0.002(5) -0.023(5) C6 0.110(5) 0.062(5) 0.114(5) -0.002(5) -0.007(5) -0.024(4) C7 0.115(5) 0.066(4) 0.118(5) -0.016(4) 0.003(5) -0.039(4) C8 0.112(5) 0.086(5) 0.103(5) -0.029(5) 0.010(5) -0.031(5) C9 0.112(5) 0.093(5) 0.076(5) -0.032(4) 0.011(4) -0.045(4) C10 0.112(5) 0.110(5) 0.062(4) -0.022(4) 0.019(4) -0.040(5) C11 0.094(5) 0.109(5) 0.081(5) -0.014(5) 0.037(4) -0.038(5) C12 0.096(5) 0.111(5) 0.080(5) -0.003(5) 0.033(4) -0.047(4) C13 0.078(5) 0.115(5) 0.096(5) -0.001(5) 0.022(4) -0.057(4) C14 0.064(4) 0.117(5) 0.107(5) -0.007(5) 0.016(4) -0.046(4) C15 0.061(4) 0.117(5) 0.098(5) -0.011(5) -0.011(4) -0.052(4) C16 0.064(4) 0.103(5) 0.095(5) 0.003(4) -0.029(4) -0.044(4) C17 0.077(5) 0.098(5) 0.103(5) 0.013(5) -0.020(4) -0.019(4) C18 0.098(5) 0.084(5) 0.092(5) 0.023(4) -0.024(4) -0.024(4) C19 0.104(5) 0.056(4) 0.099(5) 0.014(4) -0.023(5) -0.036(4) C20 0.125(5) 0.067(4) 0.104(5) 0.026(4) -0.002(5) -0.050(4) C21 0.111(5) 0.067(4) 0.112(5) 0.011(4) -0.002(4) -0.067(4) C22 0.113(5) 0.069(4) 0.120(5) -0.013(4) -0.003(5) -0.057(4) C23 0.103(5) 0.080(4) 0.103(5) -0.017(4) -0.007(4) -0.063(4) C24 0.108(5) 0.094(5) 0.077(5) -0.031(4) -0.005(4) -0.054(4) C25 0.100(5) 0.106(5) 0.065(4) -0.013(4) -0.013(4) -0.053(4) C26 0.114(5) 0.106(5) 0.053(4) -0.008(4) 0.004(4) -0.044(5) C27 0.113(5) 0.100(5) 0.055(4) 0.016(4) -0.002(4) -0.041(5) C28 0.102(5) 0.098(5) 0.066(4) 0.013(4) 0.015(4) -0.058(4) C29 0.110(5) 0.093(5) 0.095(5) 0.021(4) 0.018(4) -0.057(4) C30 0.093(5) 0.102(5) 0.096(5) 0.009(4) 0.017(4) -0.070(4) C31 0.099(5) 0.100(5) 0.097(5) 0.004(4) -0.001(4) -0.073(4) C32 0.086(4) 0.105(5) 0.093(5) -0.002(4) -0.019(4) -0.074(4) C33 0.099(5) 0.096(5) 0.075(4) -0.010(4) -0.027(4) -0.067(4) C34 0.083(4) 0.103(5) 0.074(4) 0.003(4) -0.035(4) -0.055(4) C35 0.092(5) 0.092(5) 0.060(4) 0.014(4) -0.029(4) -0.053(4) C36 0.104(5) 0.086(5) 0.067(4) 0.024(4) -0.022(4) -0.040(4) C37 0.117(5) 0.090(5) 0.067(4) 0.022(4) -0.015(4) -0.061(4) C38 0.123(5) 0.086(5) 0.096(5) 0.031(4) 0.004(5) -0.056(4) C39 0.104(5) 0.097(5) 0.098(5) 0.019(4) 0.016(4) -0.068(4) C40 0.105(5) 0.090(5) 0.114(5) 0.010(4) 0.003(5) -0.068(4) C41 0.085(4) 0.096(5) 0.106(5) 0.002(4) -0.004(4) -0.068(4) C42 0.081(4) 0.089(4) 0.095(5) -0.010(4) -0.011(4) -0.065(4) C43 0.066(4) 0.097(5) 0.086(5) -0.002(4) -0.021(4) -0.054(4) C44 0.083(4) 0.103(5) 0.075(5) 0.004(4) -0.031(4) -0.049(4) C45 0.084(5) 0.096(5) 0.080(5) 0.026(4) -0.040(4) -0.042(4) C46 0.102(5) 0.093(5) 0.076(5) 0.026(4) -0.022(4) -0.038(4) C47 0.111(5) 0.072(5) 0.091(5) 0.031(4) -0.024(5) -0.037(4) C48 0.117(5) 0.079(5) 0.099(5) 0.026(4) 0.000(5) -0.042(4) C49 0.118(5) 0.068(4) 0.099(5) 0.007(4) -0.004(5) -0.051(4) C50 0.115(5) 0.073(4) 0.096(5) -0.001(4) -0.005(4) -0.066(4) C51 0.123(5) 0.075(4) 0.096(5) -0.019(4) -0.007(5) -0.057(4) C52 0.117(5) 0.083(5) 0.075(5) -0.019(4) -0.017(4) -0.062(4) C53 0.102(5) 0.089(5) 0.063(4) -0.028(4) -0.007(4) -0.048(4) C54 0.097(5) 0.095(5) 0.053(4) -0.005(4) -0.013(4) -0.057(4) C55 0.101(5) 0.109(5) 0.057(4) 0.010(4) -0.001(4) -0.056(4) C56 0.090(5) 0.117(5) 0.072(5) -0.003(4) 0.021(4) -0.055(4) C57 0.082(4) 0.111(5) 0.090(5) 0.003(4) 0.020(4) -0.065(4) C58 0.066(4) 0.115(5) 0.099(5) -0.013(5) 0.020(4) -0.050(4) C59 0.060(4) 0.107(5) 0.099(5) -0.012(4) 0.007(4) -0.054(4) C60 0.054(4) 0.098(5) 0.099(5) -0.008(4) -0.013(4) -0.039(4) C61 0.053(4) 0.098(5) 0.112(5) 0.004(5) -0.012(4) -0.022(4) C62 0.070(5) 0.088(5) 0.103(5) 0.020(4) -0.030(4) -0.029(4) C63 0.092(5) 0.070(5) 0.105(5) 0.022(4) -0.028(5) -0.024(4) C64 0.100(5) 0.076(5) 0.112(5) 0.008(5) -0.003(5) -0.014(5) C65 0.106(5) 0.067(5) 0.108(5) -0.005(4) -0.005(5) -0.033(4) C66 0.111(5) 0.072(5) 0.102(5) -0.018(4) 0.010(5) -0.041(4) C67 0.091(5) 0.085(5) 0.093(5) -0.030(4) 0.015(4) -0.023(4) C68 0.091(5) 0.089(5) 0.074(5) -0.034(4) 0.017(4) -0.035(4) C69 0.079(5) 0.106(5) 0.081(5) -0.028(4) 0.032(4) -0.042(4) C70 0.057(4) 0.109(5) 0.099(5) -0.022(5) 0.027(4) -0.036(4) C71 0.053(4) 0.094(5) 0.111(5) -0.017(5) 0.012(4) -0.020(4) C72 0.084(5) 0.088(5) 0.111(5) -0.015(5) 0.010(5) -0.015(5) Dy1A 0.0504(6) 0.0379(5) 0.0556(6) -0.0091(4) 0.0060(4) -0.0142(4) Dy1B 0.0474(6) 0.0326(4) 0.0507(5) -0.0064(3) 0.0010(4) -0.0162(4) Dy2A 0.0501(12) 0.0496(11) 0.0673(14) -0.0218(9) -0.0002(11) -0.0228(10) Dy2B 0.076(3) 0.047(2) 0.071(3) 0.0030(19) -0.014(2) -0.033(3) Dy3A 0.074(5) 0.070(5) 0.132(7) -0.030(5) 0.034(5) -0.049(4) Dy3B 0.088(6) 0.062(5) 0.077(6) -0.002(5) 0.012(5) -0.038(5) O1 0.049(3) 0.033(3) 0.059(4) -0.010(3) -0.001(3) -0.013(3) Ni1P 0.0226(5) 0.0244(6) 0.0362(6) -0.0042(4) 0.0048(4) -0.0109(5) N1P 0.023(3) 0.025(3) 0.044(3) -0.004(2) 0.004(2) -0.011(2) N2P 0.027(3) 0.028(3) 0.038(3) -0.005(2) 0.004(2) -0.014(2) N3P 0.025(3) 0.026(3) 0.037(3) -0.004(2) 0.004(2) -0.012(2) N4P 0.028(3) 0.027(3) 0.038(3) -0.006(2) 0.006(2) -0.014(2) C1P 0.032(3) 0.030(4) 0.040(4) -0.003(3) 0.003(3) -0.017(3) C2P 0.032(4) 0.033(4) 0.050(4) 0.001(3) 0.005(3) -0.016(3) C3P 0.042(4) 0.041(4) 0.058(5) 0.011(4) 0.013(4) -0.017(4) C4P 0.047(5) 0.058(6) 0.049(5) 0.005(4) 0.007(4) -0.017(4) C5P 0.034(4) 0.036(4) 0.045(4) -0.002(3) 0.009(3) -0.018(3) C6P 0.034(4) 0.045(5) 0.055(5) 0.002(4) 0.016(3) -0.017(3) C7P 0.054(5) 0.045(5) 0.048(5) -0.003(4) 0.016(4) -0.014(4) C8P 0.028(3) 0.035(4) 0.041(4) -0.008(3) 0.009(3) -0.017(3) C9P 0.024(3) 0.030(4) 0.045(4) -0.005(3) 0.009(3) -0.011(3) C10P 0.025(3) 0.032(4) 0.040(4) -0.007(3) 0.006(3) -0.012(3) C11P 0.030(3) 0.029(4) 0.047(4) -0.005(3) 0.007(3) -0.013(3) C12P 0.030(4) 0.032(4) 0.066(5) -0.001(4) 0.013(4) -0.006(3) C13P 0.055(5) 0.045(5) 0.062(6) -0.018(4) 0.023(4) -0.015(4) C14P 0.026(3) 0.023(3) 0.049(4) -0.003(3) 0.003(3) -0.010(3) C15P 0.035(4) 0.027(4) 0.057(5) 0.000(3) 0.006(3) -0.009(3) C16P 0.055(5) 0.032(4) 0.062(5) -0.010(4) 0.013(4) -0.023(4) C17P 0.026(3) 0.023(3) 0.041(4) -0.003(3) 0.001(3) -0.011(3) C18P 0.032(3) 0.023(3) 0.038(4) -0.002(3) 0.000(3) -0.013(3) C19P 0.030(3) 0.029(3) 0.035(3) -0.002(3) 0.003(3) -0.018(3) C20P 0.032(3) 0.032(4) 0.038(4) -0.002(3) 0.004(3) -0.018(3) C21P 0.039(4) 0.033(4) 0.040(4) 0.000(3) 0.004(3) -0.020(3) C22P 0.058(5) 0.041(4) 0.056(5) 0.003(4) -0.005(4) -0.031(4) C23P 0.029(3) 0.032(4) 0.042(4) -0.008(3) 0.007(3) -0.017(3) C24P 0.030(4) 0.038(4) 0.047(4) -0.009(3) 0.014(3) -0.017(3) C25P 0.036(4) 0.061(6) 0.073(6) -0.025(5) 0.020(4) -0.030(4) C26P 0.029(3) 0.030(3) 0.039(4) -0.008(3) 0.004(3) -0.016(3) C27P 0.021(3) 0.030(3) 0.039(4) -0.008(3) 0.005(3) -0.012(3) C28P 0.025(3) 0.033(4) 0.042(4) -0.009(3) 0.004(3) -0.014(3) C29P 0.029(3) 0.030(4) 0.048(4) -0.008(3) 0.007(3) -0.016(3) C30P 0.030(4) 0.029(4) 0.062(5) -0.007(3) 0.010(3) -0.010(3) C31P 0.031(4) 0.050(5) 0.075(6) -0.007(4) 0.003(4) -0.018(4) C32P 0.030(3) 0.023(3) 0.047(4) -0.004(3) 0.002(3) -0.009(3) C33P 0.038(4) 0.029(4) 0.056(5) 0.000(3) 0.003(3) -0.011(3) C34P 0.041(4) 0.043(5) 0.061(5) 0.007(4) -0.007(4) -0.013(4) C35P 0.024(3) 0.027(3) 0.042(4) -0.003(3) 0.001(3) -0.011(3) C36P 0.027(3) 0.024(3) 0.039(4) 0.001(3) 0.001(3) -0.010(3) C1S 0.067(6) 0.077(7) 0.051(5) -0.012(5) 0.004(4) -0.041(6) C2S 0.079(7) 0.104(9) 0.045(5) -0.005(5) 0.010(5) -0.055(7) C3S 0.063(6) 0.074(7) 0.061(6) -0.005(5) 0.003(5) -0.043(6) C4S 0.052(5) 0.060(6) 0.050(5) -0.014(4) 0.003(4) -0.026(4) C5S 0.052(5) 0.057(5) 0.042(4) -0.004(4) 0.004(4) -0.024(4) C6S 0.057(5) 0.062(6) 0.055(5) -0.006(4) 0.005(4) -0.029(5) C7S 0.076(8) 0.137(13) 0.089(9) -0.005(9) 0.004(7) -0.074(9) C8S 0.064(6) 0.072(7) 0.063(6) -0.007(5) -0.006(5) -0.032(6) C9S 0.074(7) 0.086(8) 0.057(6) -0.002(6) 0.008(5) -0.039(6) C10S 0.072(7) 0.066(7) 0.079(7) 0.005(5) -0.010(6) -0.041(6) C11S 0.055(6) 0.075(7) 0.085(8) -0.027(6) 0.000(5) -0.027(5) C12S 0.062(7) 0.130(12) 0.068(7) -0.021(7) 0.019(6) -0.044(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 _geom_angle_publ_flag C2 C1 C8 125.8(12) . . ? C5 C1 C2 108.9(7) . . ? C5 C1 C8 108.1(7) . . ? C1 C2 C3 107.5(7) . . ? C11 C2 C1 120.3(14) . . ? C11 C2 C3 118.2(13) . . ? C4 C3 C2 106.8(7) . . ? C14 C3 C2 120.6(13) . . ? C14 C3 C4 123.6(13) . . ? C5 C4 C3 108.8(7) . . ? C17 C4 C3 124.0(13) . . ? C17 C4 C5 118.3(14) . . ? C1 C5 C4 108.0(7) . . ? C1 C5 C6 108.0(7) . . ? C4 C5 C6 124.4(12) . . ? C5 C6 C19 113.3(12) . . ? C7 C6 C5 107.4(7) . . ? C7 C6 C19 126.7(13) . . ? C6 C7 C8 109.3(7) . . ? C6 C7 C22 117.6(12) . . ? C8 C7 C22 122.0(13) . . ? C7 C8 C1 107.2(7) . . ? C9 C8 C1 114.0(12) . . ? C9 C8 C7 121.5(13) . . ? C8 C9 C10 123.2(12) . . ? C8 C9 C24 119.6(12) . . ? C10 C9 C24 107.9(7) . . ? C9 C10 C11 117.9(12) . . ? C26 C10 C9 109.1(7) . . ? C26 C10 C11 120.5(12) . . ? C2 C11 C10 118.1(15) . . ? C2 C11 C12 123.5(16) . . ? C12 C11 C10 110.9(14) . . ? C11 C12 C13 118.9(12) . . ? C11 C12 C28 126.2(13) . . ? C28 C12 C13 107.6(7) . . ? C14 C13 C12 115.0(12) . . ? C30 C13 C12 106.8(7) . . ? C30 C13 C14 126.8(12) . . ? C3 C14 C13 122.5(15) . . ? C3 C14 C15 117.9(14) . . ? C13 C14 C15 112.3(14) . . ? C14 C15 C32 120.2(11) . . ? C16 C15 C14 120.7(11) . . ? C16 C15 C32 108.1(7) . . ? C15 C16 C17 118.4(11) . . ? C15 C16 C34 107.7(7) . . ? C34 C16 C17 122.3(11) . . ? C4 C17 C16 114.0(14) . . ? C18 C17 C4 121.6(17) . . ? C18 C17 C16 116.2(15) . . ? C17 C18 C19 118.3(16) . . ? C17 C18 C36 116.6(16) . . ? C36 C18 C19 121.3(16) . . ? C6 C19 C18 122.2(14) . . ? C6 C19 C20 111.1(12) . . ? C20 C19 C18 118.0(14) . . ? C21 C20 C19 122.1(11) . . ? C38 C20 C19 121.1(12) . . ? C38 C20 C21 108.1(7) . . ? C22 C21 C20 120.8(11) . . ? C22 C21 C40 122.7(12) . . ? C40 C21 C20 107.5(7) . . ? C7 C22 C23 114.6(14) . . ? C21 C22 C7 118.5(13) . . ? C21 C22 C23 119.9(14) . . ? C24 C23 C22 122.9(13) . . ? C24 C23 C42 113.8(12) . . ? C42 C23 C22 113.4(13) . . ? C23 C24 C9 118.1(11) . . ? C25 C24 C9 108.1(7) . . ? C25 C24 C23 122.6(11) . . ? C24 C25 C26 107.1(7) . . ? C44 C25 C24 119.3(12) . . ? C44 C25 C26 126.5(12) . . ? C10 C26 C25 107.8(7) . . ? C27 C26 C10 128.5(13) . . ? C27 C26 C25 114.7(12) . . ? C26 C27 C28 112.4(14) . . ? C26 C27 C46 126.5(16) . . ? C46 C27 C28 114.4(14) . . ? C12 C28 C27 120.4(11) . . ? C12 C28 C29 108.7(7) . . ? C29 C28 C27 118.3(12) . . ? C28 C29 C48 127.0(13) . . ? C30 C29 C28 108.0(7) . . ? C30 C29 C48 116.6(12) . . ? C13 C30 C31 118.9(11) . . ? C29 C30 C13 108.9(7) . . ? C29 C30 C31 122.0(12) . . ? C32 C31 C30 115.6(14) . . ? C32 C31 C50 117.8(13) . . ? C50 C31 C30 117.2(13) . . ? C15 C32 C33 108.2(7) . . ? C31 C32 C15 125.9(12) . . ? C31 C32 C33 117.4(11) . . ? C34 C33 C32 106.8(7) . . ? C52 C33 C32 126.5(11) . . ? C52 C33 C34 118.2(11) . . ? C33 C34 C16 109.2(7) . . ? C35 C34 C16 117.4(11) . . ? C35 C34 C33 124.4(11) . . ? C34 C35 C36 121.7(11) . . ? C34 C35 C54 118.8(10) . . ? C54 C35 C36 109.4(7) . . ? C18 C36 C35 124.0(11) . . ? C18 C36 C37 114.9(12) . . ? C35 C36 C37 107.4(7) . . ? C36 C37 C55 107.5(7) . . ? C38 C37 C36 125.2(11) . . ? C38 C37 C55 117.1(11) . . ? C20 C38 C39 109.2(7) . . ? C37 C38 C20 118.6(12) . . ? C37 C38 C39 120.9(12) . . ? C38 C39 C40 107.2(7) . . ? C57 C39 C38 121.5(12) . . ? C57 C39 C40 119.3(12) . . ? C21 C40 C39 108.1(7) . . ? C41 C40 C21 118.6(12) . . ? C41 C40 C39 119.7(12) . . ? C40 C41 C42 122.5(11) . . ? C40 C41 C59 120.7(11) . . ? C42 C41 C59 107.4(7) . . ? C23 C42 C41 122.5(10) . . ? C23 C42 C43 120.8(10) . . ? C43 C42 C41 107.8(7) . . ? C42 C43 C60 109.2(7) . . ? C44 C43 C42 119.2(11) . . ? C44 C43 C60 122.1(11) . . ? C25 C44 C43 123.6(14) . . ? C25 C44 C45 115.1(13) . . ? C43 C44 C45 113.3(13) . . ? C46 C45 C44 118.7(11) . . ? C62 C45 C44 123.3(11) . . ? C62 C45 C46 109.1(7) . . ? C27 C46 C45 118.2(13) . . ? C27 C46 C47 125.9(13) . . ? C45 C46 C47 107.4(7) . . ? C46 C47 C48 124.3(13) . . ? C63 C47 C46 107.2(7) . . ? C63 C47 C48 117.5(12) . . ? C47 C48 C29 109.7(14) . . ? C49 C48 C29 121.6(15) . . ? C49 C48 C47 120.3(15) . . ? C48 C49 C50 119.9(12) . . ? C48 C49 C65 118.4(13) . . ? C65 C49 C50 107.5(7) . . ? C31 C50 C49 121.0(11) . . ? C51 C50 C31 122.8(11) . . ? C51 C50 C49 106.7(7) . . ? C50 C51 C52 120.5(11) . . ? C66 C51 C50 109.0(7) . . ? C66 C51 C52 117.9(12) . . ? C33 C52 C51 112.6(13) . . ? C33 C52 C53 121.4(13) . . ? C53 C52 C51 121.1(14) . . ? C52 C53 C54 117.2(13) . . ? C52 C53 C68 121.0(14) . . ? C54 C53 C68 113.7(12) . . ? C35 C54 C53 119.6(10) . . ? C35 C54 C55 108.0(7) . . ? C53 C54 C55 120.4(10) . . ? C54 C55 C37 107.7(7) . . ? C56 C55 C37 121.7(11) . . ? C56 C55 C54 119.1(11) . . ? C55 C56 C57 118.6(11) . . ? C55 C56 C69 120.6(11) . . ? C69 C56 C57 108.4(7) . . ? C39 C57 C56 120.1(11) . . ? C39 C57 C58 121.8(11) . . ? C58 C57 C56 106.6(7) . . ? C59 C58 C57 117.7(11) . . ? C59 C58 C70 120.8(11) . . ? C70 C58 C57 110.3(7) . . ? C58 C59 C41 120.7(11) . . ? C58 C59 C60 120.7(11) . . ? C60 C59 C41 107.9(7) . . ? C59 C60 C43 107.7(7) . . ? C61 C60 C43 124.4(11) . . ? C61 C60 C59 119.3(11) . . ? C60 C61 C62 115.5(14) . . ? C60 C61 C71 116.5(14) . . ? C62 C61 C71 119.3(14) . . ? C45 C62 C61 121.0(12) . . ? C45 C62 C63 107.8(7) . . ? C61 C62 C63 122.7(13) . . ? C47 C63 C62 108.2(7) . . ? C64 C63 C47 123.2(12) . . ? C64 C63 C62 118.9(12) . . ? C63 C64 C65 116.0(12) . . ? C63 C64 C72 120.1(13) . . ? C72 C64 C65 107.7(7) . . ? C64 C65 C49 123.6(11) . . ? C66 C65 C49 108.0(7) . . ? C66 C65 C64 108.0(7) . . ? C51 C66 C65 108.6(7) . . ? C51 C66 C67 123.1(11) . . ? C65 C66 C67 107.8(7) . . ? C66 C67 C68 119.6(12) . . ? C72 C67 C66 107.8(7) . . ? C72 C67 C68 121.4(12) . . ? C53 C68 C67 114.9(13) . . ? C69 C68 C53 123.6(14) . . ? C69 C68 C67 115.8(13) . . ? C56 C69 C70 107.4(7) . . ? C68 C69 C56 122.1(12) . . ? C68 C69 C70 121.7(12) . . ? C58 C70 C69 107.3(7) . . ? C71 C70 C58 122.1(13) . . ? C71 C70 C69 120.8(12) . . ? C70 C71 C61 120.4(15) . . ? C70 C71 C72 120.3(14) . . ? C72 C71 C61 114.0(14) . . ? C64 C72 C71 123.6(13) . . ? C67 C72 C64 108.6(7) . . ? C67 C72 C71 116.4(12) . . ? Dy2A Dy1A Dy1B 86.07(15) . . ? Dy2A Dy1A Dy2B 94.26(17) . . ? Dy2A Dy1A Dy3A 26.1(4) . . ? Dy2A Dy1A Dy3B 106.3(4) . . ? Dy2A Dy1A O1 72.1(2) . . ? Dy2B Dy1A Dy1B 9.48(9) . . ? Dy3A Dy1A Dy1B 75.3(3) . . ? Dy3A Dy1A Dy2B 84.8(3) . . ? Dy3A Dy1A Dy3B 101.1(4) . . ? Dy3A Dy1A O1 56.4(3) . . ? Dy3B Dy1A Dy1B 26.8(3) . . ? Dy3B Dy1A Dy2B 17.6(3) . . ? O1 Dy1A Dy1B 20.81(18) . . ? O1 Dy1A Dy2B 30.0(2) . . ? O1 Dy1A Dy3B 47.6(4) . . ? Dy1A Dy1B Dy2A 13.15(4) . . ? Dy2B Dy1B Dy1A 68.3(5) . . ? Dy2B Dy1B Dy2A 79.8(5) . . ? Dy2B Dy1B Dy3A 95.1(6) . . ? Dy2B Dy1B Dy3B 17.1(7) . . ? Dy2B Dy1B O1 88.5(6) . . ? Dy3A Dy1B Dy1A 26.91(13) . . ? Dy3A Dy1B Dy2A 15.78(13) . . ? Dy3B Dy1B Dy1A 53.7(5) . . ? Dy3B Dy1B Dy2A 64.1(5) . . ? Dy3B Dy1B Dy3A 79.8(5) . . ? Dy3B Dy1B O1 74.6(5) . . ? O1 Dy1B Dy1A 20.99(19) . . ? O1 Dy1B Dy2A 15.20(19) . . ? O1 Dy1B Dy3A 10.8(2) . . ? Dy1A Dy2A Dy1B 80.78(14) . . ? Dy1A Dy2A Dy2B 72.38(17) . . ? Dy1A Dy2A Dy3A 132.3(6) . . ? Dy1A Dy2A Dy3B 59.6(3) . . ? Dy1A Dy2A O1 82.7(2) . . ? Dy2B Dy2A Dy1B 9.60(8) . . ? Dy3A Dy2A Dy1B 77.8(4) . . ? Dy3A Dy2A Dy2B 87.1(4) . . ? Dy3A Dy2A Dy3B 104.5(5) . . ? Dy3A Dy2A O1 66.3(5) . . ? Dy3B Dy2A Dy1B 26.9(3) . . ? Dy3B Dy2A Dy2B 17.4(3) . . ? O1 Dy2A Dy1B 15.7(2) . . ? O1 Dy2A Dy2B 22.5(2) . . ? O1 Dy2A Dy3B 39.0(4) . . ? Dy1A Dy2B Dy2A 13.36(4) . . ? Dy1A Dy2B Dy3A 26.92(13) . . ? Dy1B Dy2B Dy1A 102.2(6) . . ? Dy1B Dy2B Dy2A 90.6(5) . . ? Dy1B Dy2B Dy3A 75.4(5) . . ? Dy1B Dy2B Dy3B 153.3(11) . . ? Dy1B Dy2B O1 73.8(5) . . ? Dy2A Dy2B Dy3A 15.66(13) . . ? Dy3B Dy2B Dy1A 55.2(8) . . ? Dy3B Dy2B Dy2A 64.9(8) . . ? Dy3B Dy2B Dy3A 80.6(8) . . ? Dy3B Dy2B O1 84.1(8) . . ? O1 Dy2B Dy1A 29.0(2) . . ? O1 Dy2B Dy2A 20.9(2) . . ? O1 Dy2B Dy3A 8.5(2) . . ? Dy1A Dy3A Dy1B 77.8(2) . . ? Dy1A Dy3A Dy2B 68.3(2) . . ? Dy1A Dy3A Dy3B 52.3(3) . . ? Dy1A Dy3A O1 69.7(3) . . ? Dy1B Dy3A Dy2B 9.48(9) . . ? Dy1B Dy3A Dy3B 26.4(3) . . ? Dy2A Dy3A Dy1A 21.6(3) . . ? Dy2A Dy3A Dy1B 86.4(4) . . ? Dy2A Dy3A Dy2B 77.2(4) . . ? Dy2A Dy3A Dy3B 60.2(5) . . ? Dy2A Dy3A O1 81.8(5) . . ? Dy3B Dy3A Dy2B 17.0(3) . . ? O1 Dy3A Dy1B 12.1(3) . . ? O1 Dy3A Dy2B 9.9(3) . . ? O1 Dy3A Dy3B 22.8(4) . . ? Dy1A Dy3B Dy2A 14.08(8) . . ? Dy1A Dy3B Dy3A 26.63(18) . . ? Dy1B Dy3B Dy1A 99.5(6) . . ? Dy1B Dy3B Dy2A 89.0(6) . . ? Dy1B Dy3B Dy3A 73.9(5) . . ? Dy1B Dy3B O1 58.4(5) . . ? Dy2A Dy3B Dy3A 15.25(15) . . ? Dy2B Dy3B Dy1A 107.3(9) . . ? Dy2B Dy3B Dy1B 9.5(4) . . ? Dy2B Dy3B Dy2A 97.6(8) . . ? Dy2B Dy3B Dy3A 82.4(8) . . ? Dy2B Dy3B O1 66.2(7) . . ? O1 Dy3B Dy1A 41.1(3) . . ? O1 Dy3B Dy2A 32.6(3) . . ? O1 Dy3B Dy3A 17.8(3) . . ? Dy1A O1 Dy2B 121.0(4) . . ? Dy1A O1 Dy3B 91.3(5) . . ? Dy1B O1 Dy1A 138.2(4) . . ? Dy1B O1 Dy2B 17.67(16) . . ? Dy1B O1 Dy3B 47.0(5) . . ? Dy2A O1 Dy1A 25.17(10) . . ? Dy2A O1 Dy1B 149.1(4) . . ? Dy2A O1 Dy2B 136.6(4) . . ? Dy2A O1 Dy3B 108.5(5) . . ? Dy2B O1 Dy3B 29.7(5) . . ? Dy3A O1 Dy1A 53.9(3) . . ? Dy3A O1 Dy1B 157.1(5) . . ? Dy3A O1 Dy2A 31.9(3) . . ? Dy3A O1 Dy2B 161.7(5) . . ? Dy3A O1 Dy3B 139.4(6) . . ? N1P Ni1P N4P 89.8(2) . . ? N2P Ni1P N1P 90.1(2) . . ? N2P Ni1P N4P 177.7(2) . . ? N3P Ni1P N1P 177.6(2) . . ? N3P Ni1P N2P 90.0(2) . . ? N3P Ni1P N4P 90.0(2) . . ? C1P N1P Ni1P 128.3(5) . . ? C1P N1P C8P 103.6(6) . . ? C8P N1P Ni1P 128.0(5) . . ? C10P N2P Ni1P 128.0(5) . . ? C17P N2P Ni1P 127.6(5) . . ? C17P N2P C10P 104.4(6) . . ? C19P N3P Ni1P 127.8(4) . . ? C26P N3P Ni1P 128.0(5) . . ? C26P N3P C19P 104.1(5) . . ? C28P N4P Ni1P 128.1(5) . . ? C35P N4P Ni1P 127.8(5) . . ? C35P N4P C28P 104.1(6) . . ? N1P C1P C2P 112.1(6) . . ? N1P C1P C36P 124.8(6) . . ? C36P C1P C2P 123.1(7) . . ? C1P C2P C3P 124.3(7) . . ? C5P C2P C1P 105.7(7) . . ? C5P C2P C3P 129.8(7) . . ? C2P C3P H3PA 108.9 . . ? C2P C3P H3PB 108.9 . . ? C2P C3P C4P 113.2(8) . . ? H3PA C3P H3PB 107.8 . . ? C4P C3P H3PA 108.9 . . ? C4P C3P H3PB 108.9 . . ? C3P C4P H4PA 109.5 . . ? C3P C4P H4PB 109.5 . . ? C3P C4P H4PC 109.5 . . ? H4PA C4P H4PB 109.5 . . ? H4PA C4P H4PC 109.5 . . ? H4PB C4P H4PC 109.5 . . ? C2P C5P C6P 128.7(7) . . ? C2P C5P C8P 106.6(6) . . ? C8P C5P C6P 124.5(7) . . ? C5P C6P H6PA 109.3 . . ? C5P C6P H6PB 109.3 . . ? C5P C6P C7P 111.4(7) . . ? H6PA C6P H6PB 108.0 . . ? C7P C6P H6PA 109.3 . . ? C7P C6P H6PB 109.3 . . ? C6P C7P H7PA 109.5 . . ? C6P C7P H7PB 109.5 . . ? C6P C7P H7PC 109.5 . . ? H7PA C7P H7PB 109.5 . . ? H7PA C7P H7PC 109.5 . . ? H7PB C7P H7PC 109.5 . . ? N1P C8P C5P 111.9(6) . . ? N1P C8P C9P 124.4(7) . . ? C9P C8P C5P 123.7(6) . . ? C8P C9P H9P 117.6 . . ? C10P C9P C8P 124.8(6) . . ? C10P C9P H9P 117.6 . . ? N2P C10P C11P 111.5(6) . . ? C9P C10P N2P 124.7(6) . . ? C9P C10P C11P 123.8(6) . . ? C10P C11P C12P 124.5(7) . . ? C14P C11P C10P 106.4(6) . . ? C14P C11P C12P 129.0(7) . . ? C11P C12P H12A 109.1 . . ? C11P C12P H12B 109.1 . . ? C11P C12P C13P 112.5(7) . . ? H12A C12P H12B 107.8 . . ? C13P C12P H12A 109.1 . . ? C13P C12P H12B 109.1 . . ? C12P C13P H13A 109.5 . . ? C12P C13P H13B 109.5 . . ? C12P C13P H13C 109.5 . . ? H13A C13P H13B 109.5 . . ? H13A C13P H13C 109.5 . . ? H13B C13P H13C 109.5 . . ? C11P C14P C15P 128.9(7) . . ? C11P C14P C17P 106.6(6) . . ? C17P C14P C15P 124.5(7) . . ? C14P C15P H15A 109.1 . . ? C14P C15P H15B 109.1 . . ? C14P C15P C16P 112.5(7) . . ? H15A C15P H15B 107.8 . . ? C16P C15P H15A 109.1 . . ? C16P C15P H15B 109.1 . . ? C15P C16P H16A 109.5 . . ? C15P C16P H16B 109.5 . . ? C15P C16P H16C 109.5 . . ? H16A C16P H16B 109.5 . . ? H16A C16P H16C 109.5 . . ? H16B C16P H16C 109.5 . . ? N2P C17P C14P 111.1(6) . . ? C18P C17P N2P 125.2(6) . . ? C18P C17P C14P 123.6(6) . . ? C17P C18P H18P 117.8 . . ? C17P C18P C19P 124.4(7) . . ? C19P C18P H18P 117.8 . . ? N3P C19P C20P 111.4(6) . . ? C18P C19P N3P 124.8(6) . . ? C18P C19P C20P 123.8(6) . . ? C19P C20P C21P 125.0(6) . . ? C23P C20P C19P 106.7(6) . . ? C23P C20P C21P 128.1(6) . . ? C20P C21P H21A 109.3 . . ? C20P C21P H21B 109.3 . . ? C20P C21P C22P 111.8(6) . . ? H21A C21P H21B 107.9 . . ? C22P C21P H21A 109.3 . . ? C22P C21P H21B 109.3 . . ? C21P C22P H22A 109.5 . . ? C21P C22P H22B 109.5 . . ? C21P C22P H22C 109.5 . . ? H22A C22P H22B 109.5 . . ? H22A C22P H22C 109.5 . . ? H22B C22P H22C 109.5 . . ? C20P C23P C24P 128.7(7) . . ? C20P C23P C26P 106.1(6) . . ? C26P C23P C24P 125.1(7) . . ? C23P C24P H24A 109.4 . . ? C23P C24P H24B 109.4 . . ? C23P C24P C25P 111.3(6) . . ? H24A C24P H24B 108.0 . . ? C25P C24P H24A 109.4 . . ? C25P C24P H24B 109.4 . . ? C24P C25P H25A 109.5 . . ? C24P C25P H25B 109.5 . . ? C24P C25P H25C 109.5 . . ? H25A C25P H25B 109.5 . . ? H25A C25P H25C 109.5 . . ? H25B C25P H25C 109.5 . . ? N3P C26P C23P 111.8(6) . . ? C27P C26P N3P 124.5(6) . . ? C27P C26P C23P 123.7(6) . . ? C26P C27P H27P 117.3 . . ? C28P C27P C26P 125.5(6) . . ? C28P C27P H27P 117.3 . . ? N4P C28P C29P 111.5(6) . . ? C27P C28P N4P 123.9(6) . . ? C27P C28P C29P 124.6(6) . . ? C28P C29P C30P 124.1(7) . . ? C32P C29P C28P 106.5(6) . . ? C32P C29P C30P 129.4(7) . . ? C29P C30P H30A 109.0 . . ? C29P C30P H30B 109.0 . . ? C29P C30P C31P 112.7(7) . . ? H30A C30P H30B 107.8 . . ? C31P C30P H30A 109.0 . . ? C31P C30P H30B 109.0 . . ? C30P C31P H31A 109.5 . . ? C30P C31P H31B 109.5 . . ? C30P C31P H31C 109.5 . . ? H31A C31P H31B 109.5 . . ? H31A C31P H31C 109.5 . . ? H31B C31P H31C 109.5 . . ? C29P C32P C33P 128.5(7) . . ? C29P C32P C35P 106.5(6) . . ? C35P C32P C33P 124.9(7) . . ? C32P C33P H33A 109.0 . . ? C32P C33P H33B 109.0 . . ? C32P C33P C34P 112.9(7) . . ? H33A C33P H33B 107.8 . . ? C34P C33P H33A 109.0 . . ? C34P C33P H33B 109.0 . . ? C33P C34P H34A 109.5 . . ? C33P C34P H34B 109.5 . . ? C33P C34P H34C 109.5 . . ? H34A C34P H34B 109.5 . . ? H34A C34P H34C 109.5 . . ? H34B C34P H34C 109.5 . . ? N4P C35P C32P 111.4(6) . . ? C36P C35P N4P 124.9(6) . . ? C36P C35P C32P 123.7(7) . . ? C1P C36P H36P 117.8 . . ? C35P C36P C1P 124.4(7) . . ? C35P C36P H36P 117.8 . . ? C2S C1S H1S 119.9 . . ? C6S C1S H1S 119.9 . . ? C6S C1S C2S 120.2(10) . . ? C1S C2S H2S 120.6 . . ? C3S C2S C1S 118.9(10) . . ? C3S C2S H2S 120.6 . . ? C2S C3S H3S 119.7 . . ? C4S C3S C2S 120.7(10) . . ? C4S C3S H3S 119.7 . . ? C3S C4S H4S 119.7 . . ? C5S C4S C3S 120.7(9) . . ? C5S C4S H4S 119.7 . . ? C4S C5S H5S 120.2 . . ? C4S C5S C6S 119.7(9) . . ? C6S C5S H5S 120.2 . . ? C1S C6S C5S 119.8(10) . . ? C1S C6S H6S 120.1 . . ? C5S C6S H6S 120.1 . . ? C8S C7S H7S 120.2 . . ? C8S C7S C12S 119.6(12) . . ? C12S C7S H7S 120.2 . . ? C7S C8S H8S 120.0 . . ? C7S C8S C9S 120.1(11) . . ? C9S C8S H8S 120.0 . . ? C8S C9S H9S 119.6 . . ? C8S C9S C10S 120.8(11) . . ? C10S C9S H9S 119.6 . . ? C9S C10S H10S 120.1 . . ? C9S C10S C11S 119.9(11) . . ? C11S C10S H10S 120.1 . . ? C10S C11S H11S 120.6 . . ? C12S C11S C10S 118.7(11) . . ? C12S C11S H11S 120.6 . . ? C7S C12S H12S 119.5 . . ? C11S C12S C7S 121.0(11) . . ? C11S C12S H12S 119.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.426(13) . ? C1 C5 1.416(12) . ? C1 C8 1.443(13) . ? C2 C3 1.452(13) . ? C2 C11 1.31(2) . ? C3 C4 1.434(13) . ? C3 C14 1.34(2) . ? C4 C5 1.421(12) . ? C4 C17 1.41(2) . ? C5 C6 1.445(13) . ? C6 C7 1.412(13) . ? C6 C19 1.46(2) . ? C7 C8 1.421(13) . ? C7 C22 1.45(2) . ? C8 C9 1.396(19) . ? C9 C10 1.430(14) . ? C9 C24 1.454(13) . ? C10 C11 1.56(2) . ? C10 C26 1.416(14) . ? C11 C12 1.42(2) . ? C12 C13 1.462(13) . ? C12 C28 1.421(13) . ? C13 C14 1.45(2) . ? C13 C30 1.434(13) . ? C14 C15 1.48(2) . ? C15 C16 1.475(13) . ? C15 C32 1.479(13) . ? C16 C17 1.54(2) . ? C16 C34 1.478(13) . ? C17 C18 1.41(2) . ? C18 C19 1.48(2) . ? C18 C36 1.44(2) . ? C19 C20 1.47(2) . ? C20 C21 1.452(14) . ? C20 C38 1.413(14) . ? C21 C22 1.43(2) . ? C21 C40 1.426(14) . ? C22 C23 1.477(15) . ? C23 C24 1.434(19) . ? C23 C42 1.438(19) . ? C24 C25 1.434(13) . ? C25 C26 1.475(13) . ? C25 C44 1.303(19) . ? C26 C27 1.34(2) . ? C27 C28 1.55(2) . ? C27 C46 1.36(2) . ? C28 C29 1.432(13) . ? C29 C30 1.419(13) . ? C29 C48 1.49(2) . ? C30 C31 1.486(19) . ? C31 C32 1.359(19) . ? C31 C50 1.43(2) . ? C32 C33 1.496(13) . ? C33 C34 1.473(13) . ? C33 C52 1.368(19) . ? C34 C35 1.289(15) . ? C35 C36 1.470(13) . ? C35 C54 1.465(13) . ? C36 C37 1.492(13) . ? C37 C38 1.394(17) . ? C37 C55 1.496(13) . ? C38 C39 1.427(14) . ? C39 C40 1.456(14) . ? C39 C57 1.342(18) . ? C40 C41 1.284(17) . ? C41 C42 1.470(13) . ? C41 C59 1.487(13) . ? C42 C43 1.452(12) . ? C43 C44 1.366(18) . ? C43 C60 1.460(13) . ? C44 C45 1.535(19) . ? C45 C46 1.428(13) . ? C45 C62 1.403(13) . ? C46 C47 1.442(13) . ? C47 C48 1.47(2) . ? C47 C63 1.427(14) . ? C48 C49 1.38(2) . ? C49 C50 1.445(12) . ? C49 C65 1.422(12) . ? C50 C51 1.426(12) . ? C51 C52 1.443(18) . ? C51 C66 1.393(12) . ? C52 C53 1.44(2) . ? C53 C54 1.466(18) . ? C53 C68 1.47(2) . ? C54 C55 1.479(12) . ? C55 C56 1.343(17) . ? C56 C57 1.496(13) . ? C56 C69 1.436(13) . ? C57 C58 1.445(13) . ? C58 C59 1.318(16) . ? C58 C70 1.430(13) . ? C59 C60 1.459(13) . ? C60 C61 1.41(2) . ? C61 C62 1.42(2) . ? C61 C71 1.51(2) . ? C62 C63 1.434(13) . ? C63 C64 1.393(18) . ? C64 C65 1.419(13) . ? C64 C72 1.419(13) . ? C65 C66 1.419(12) . ? C66 C67 1.428(12) . ? C67 C68 1.51(2) . ? C67 C72 1.405(13) . ? C68 C69 1.295(19) . ? C69 C70 1.503(13) . ? C70 C71 1.30(2) . ? C71 C72 1.47(2) . ? Dy1A Dy1B 3.7428(14) . ? Dy1A Dy2A 0.863(2) . ? Dy1A Dy2B 3.559(5) . ? Dy1A Dy3A 1.733(8) . ? Dy1A Dy3B 3.059(15) . ? Dy1A O1 2.012(6) . ? Dy1B Dy2A 3.783(2) . ? Dy1B Dy2B 0.631(5) . ? Dy1B Dy3A 3.705(8) . ? Dy1B Dy3B 1.712(18) . ? Dy1B O1 1.995(6) . ? Dy2A Dy2B 3.723(6) . ? Dy2A Dy3A 1.031(9) . ? Dy2A Dy3B 3.403(15) . ? Dy2A O1 1.930(6) . ? Dy2B Dy3A 3.813(9) . ? Dy2B Dy3B 1.125(18) . ? Dy2B O1 2.077(8) . ? Dy3A Dy3B 3.795(17) . ? Dy3A O1 1.786(9) . ? Dy3B O1 2.257(16) . ? Ni1P N1P 1.964(6) . ? Ni1P N2P 1.962(6) . ? Ni1P N3P 1.961(6) . ? Ni1P N4P 1.964(6) . ? N1P C1P 1.366(9) . ? N1P C8P 1.380(9) . ? N2P C10P 1.383(9) . ? N2P C17P 1.381(9) . ? N3P C19P 1.385(9) . ? N3P C26P 1.380(9) . ? N4P C28P 1.392(9) . ? N4P C35P 1.377(9) . ? C1P C2P 1.445(10) . ? C1P C36P 1.377(10) . ? C2P C3P 1.497(11) . ? C2P C5P 1.357(11) . ? C3P H3PA 0.9900 . ? C3P H3PB 0.9900 . ? C3P C4P 1.518(14) . ? C4P H4PA 0.9800 . ? C4P H4PB 0.9800 . ? C4P H4PC 0.9800 . ? C5P C6P 1.513(10) . ? C5P C8P 1.429(10) . ? C6P H6PA 0.9900 . ? C6P H6PB 0.9900 . ? C6P C7P 1.547(13) . ? C7P H7PA 0.9800 . ? C7P H7PB 0.9800 . ? C7P H7PC 0.9800 . ? C8P C9P 1.386(10) . ? C9P H9P 0.9500 . ? C9P C10P 1.372(11) . ? C10P C11P 1.441(10) . ? C11P C12P 1.500(10) . ? C11P C14P 1.364(11) . ? C12P H12A 0.9900 . ? C12P H12B 0.9900 . ? C12P C13P 1.529(14) . ? C13P H13A 0.9800 . ? C13P H13B 0.9800 . ? C13P H13C 0.9800 . ? C14P C15P 1.505(10) . ? C14P C17P 1.447(9) . ? C15P H15A 0.9900 . ? C15P H15B 0.9900 . ? C15P C16P 1.535(12) . ? C16P H16A 0.9800 . ? C16P H16B 0.9800 . ? C16P H16C 0.9800 . ? C17P C18P 1.370(10) . ? C18P H18P 0.9500 . ? C18P C19P 1.371(10) . ? C19P C20P 1.437(9) . ? C20P C21P 1.505(10) . ? C20P C23P 1.368(10) . ? C21P H21A 0.9900 . ? C21P H21B 0.9900 . ? C21P C22P 1.533(11) . ? C22P H22A 0.9800 . ? C22P H22B 0.9800 . ? C22P H22C 0.9800 . ? C23P C24P 1.500(9) . ? C23P C26P 1.440(10) . ? C24P H24A 0.9900 . ? C24P H24B 0.9900 . ? C24P C25P 1.530(12) . ? C25P H25A 0.9800 . ? C25P H25B 0.9800 . ? C25P H25C 0.9800 . ? C26P C27P 1.376(10) . ? C27P H27P 0.9500 . ? C27P C28P 1.369(10) . ? C28P C29P 1.436(10) . ? C29P C30P 1.491(10) . ? C29P C32P 1.365(11) . ? C30P H30A 0.9900 . ? C30P H30B 0.9900 . ? C30P C31P 1.532(12) . ? C31P H31A 0.9800 . ? C31P H31B 0.9800 . ? C31P H31C 0.9800 . ? C32P C33P 1.499(10) . ? C32P C35P 1.447(10) . ? C33P H33A 0.9900 . ? C33P H33B 0.9900 . ? C33P C34P 1.538(13) . ? C34P H34A 0.9800 . ? C34P H34B 0.9800 . ? C34P H34C 0.9800 . ? C35P C36P 1.376(10) . ? C36P H36P 0.9500 . ? C1S H1S 0.9500 . ? C1S C2S 1.408(16) . ? C1S C6S 1.348(15) . ? C2S H2S 0.9500 . ? C2S C3S 1.377(16) . ? C3S H3S 0.9500 . ? C3S C4S 1.364(14) . ? C4S H4S 0.9500 . ? C4S C5S 1.356(14) . ? C5S H5S 0.9500 . ? C5S C6S 1.413(14) . ? C6S H6S 0.9500 . ? C7S H7S 0.9500 . ? C7S C8S 1.358(18) . ? C7S C12S 1.40(2) . ? C8S H8S 0.9500 . ? C8S C9S 1.368(16) . ? C9S H9S 0.9500 . ? C9S C10S 1.384(17) . ? C10S H10S 0.9500 . ? C10S C11S 1.391(18) . ? C11S H11S 0.9500 . ? C11S C12S 1.364(18) . ? C12S H12S 0.9500 . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.686(5) 2 0.314(5)