#------------------------------------------------------------------------------ #$Date: 2026-06-04 18:02:04 +0100 (Thu, 04 Jun 2026) $ #$Revision: 306217 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721094.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_7721094 loop_ _publ_author_name 'Panja, Anangamohan' 'Jana, Narayan Ch' 'Aravena, Daniel' 'Jagličić, Zvonko' _publ_section_title ; Tuning magnetic exchange and relaxation dynamics in dinuclear Dy(III) single-molecule magnets via co-ligand modulation on a hydrazone-based Schiff base platform. ; _journal_issue 18 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 7329 _journal_page_last 7341 _journal_paper_doi 10.1039/d6dt00433d _journal_volume 55 _journal_year 2026 _chemical_formula_moiety 'C46 H46 Dy2 N8 O18, 2(C H4 O)' _chemical_formula_sum 'C48 H54 Dy2 N8 O20' _chemical_formula_weight 1387.99 _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 mixed _audit_creation_date 2026-03-23 _audit_creation_method ; Olex2 1.5 (compiled 2026.03.20 svn.r2bc28608 for OlexSys, GUI svn.r7524) ; _audit_update_record ; 2026-03-23 deposited with the CCDC. 2026-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.6700(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.77060(10) _cell_length_b 24.2648(3) _cell_length_c 11.30730(10) _cell_measurement_reflns_used 12609 _cell_measurement_temperature 212(7) _cell_measurement_theta_max 72.0900 _cell_measurement_theta_min 4.3080 _cell_volume 2671.85(5) _computing_cell_refinement 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 212.15 _diffrn_detector_area_resol_mean 5.8140 _diffrn_detector_type 'Pilatus 200K' _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -63.00 -16.00 0.50 0.11 -- 0.00 145.00-161.00 94 2 \w 97.00 159.00 0.50 0.57 -- 95.54 126.00 30.00 124 3 \w 32.00 113.00 0.50 0.57 -- 95.54-126.00 -46.00 162 4 \w 86.00 158.00 0.50 0.57 -- 95.54 145.00-161.00 144 5 \w 37.00 127.00 0.50 0.57 -- 95.54-145.00 145.00 180 6 \w -23.00 42.00 0.50 0.11 -- 0.00 77.00 60.00 130 7 \w -66.00 3.00 0.50 0.11 -- 0.00 -37.00-120.00 138 8 \w -23.00 42.00 0.50 0.11 -- 0.00 77.00-180.00 130 9 \w 31.00 100.00 0.50 0.57 -- 95.54 -45.00 -30.00 138 10 \w 31.00 100.00 0.50 0.57 -- 95.54 -45.00 -90.00 138 11 \w 33.00 113.00 0.50 0.57 -- 95.54-125.00-180.00 160 12 \w 103.00 160.00 0.50 0.57 -- 95.54 77.00 30.00 114 13 \w 83.00 158.00 0.50 0.57 -- 95.54 61.00 -60.00 150 14 \w 33.00 109.00 0.50 0.57 -- 95.54 -61.00 -90.00 152 15 \w 27.00 99.00 0.50 0.57 -- 95.54 -30.00 -30.00 144 16 \w 27.00 99.00 0.50 0.57 -- 95.54 -30.00 120.00 144 17 \w 27.00 107.00 0.50 0.57 -- 95.54 -94.00 -30.00 160 18 \w 103.00 160.00 0.50 0.57 -- 95.54 77.00 -60.00 114 19 \w -66.00 -14.00 0.50 0.11 -- 0.00 -37.00 0.00 104 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Pilatus 200K' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_unetI/netI 0.0325 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 22539 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.535 _diffrn_reflns_theta_min 3.643 _exptl_absorpt_coefficient_mu 15.511 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.37347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.725 _exptl_crystal_description block _exptl_crystal_F_000 1380 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.611 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 391 _refine_ls_number_reflns 5161 _refine_ls_number_restraints 47 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0280 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+1.1700P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.0712 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4693 _reflns_number_total 5161 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00433d2.cif _cod_data_source_block complex-4_njap-269 _cod_database_code 7721094 _shelx_shelxl_version_number 2018/3 _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 0.306 _shelx_estimated_absorpt_t_min 0.147 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 2. Restrained distances O7-H7A = O7-H7B 0.86 with sigma of 0.02 H7A-H7B 1.36 with sigma of 0.04 Dy1-H7A \\sim Dy1-H7B with sigma of 0.02 O8B-O9B \\sim O8A-O9A with sigma of 0.004 N4-O8B \\sim N4-O8A \\sim N4-O9A \\sim N4-O9B with sigma of 0.002 3. Uiso/Uaniso restraints and constraints Uanis(O9B) \\sim Ueq, Uanis(O9A) \\sim Ueq, Uanis(O8B) \\sim Ueq, Uanis(O8A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C23A) \\sim Ueq, Uanis(C23B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Fixed Sof: H6B(0.15) H6A(0.85) O8B(0.5) O8A(0.5) O9A(0.5) O9B(0.5) C23B(0.15) H23A(0.15) H23B(0.15) H23C(0.15) C23A(0.85) H23D(0.85) H23E(0.85) H23F(0.85) 5.a Aromatic/amide H refined with riding coordinates: C9(H9), C5(H5), C21(H21), C20(H20), C15(H15), C22(H22), C18(H18), C14(H14), C13(H13), C12(H12), C3(H3) 5.b Tetrahedral OH refined with riding coordinates: O6(H6B), O6(H6A) 5.c Idealised Me refined as rotating group: C7(H7C,H7D,H7E), C8(H8A,H8B,H8C), C24(H24A,H24B,H24C), C23B(H23A,H23B,H23C), C23A(H23D,H23E,H23F) 5.d Idealised tetrahedral OH refined as rotating group: O10(H10) ; _shelx_res_file ; TITL njap-269_rt_r_a.res in P2(1)/n complex-4_njap-269.res created by SHELXL-2018/3 at 18:24:17 on 23-Mar-2026 REM Old TITL NJAP-269_RT_R in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.096, Rweak 0.004, Alpha 0.063, Orientation as input REM Formula found by SHELXT: C27 N3 O8 Dy CELL 1.54184 9.7706 24.2648 11.3073 90 94.67 90 ZERR 2 0.0001 0.0003 0.0001 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Dy N O UNIT 96 108 4 16 40 DFIX 0.86 O7 H7a O7 H7b DANG 1.36 H7a H7b SADI Dy1 H7a Dy1 H7b ISOR 0.01 0.02 O9B O9A O8B O8A SADI 0.004 O8B O9B O8A O9A SADI 0.002 N4 O8B N4 O8A N4 O9A N4 O9B ISOR 0.01 0.02 C23A C23B L.S. 40 PLAN 2 SIZE 0.1 0.2 0.2 TEMP -61 CONF FREE Dy1 C16 list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 0 1 1 OMIT 1 11 9 OMIT 2 1 11 OMIT 6 7 11 REM REM REM WGHT 0.038100 1.170000 FVAR 0.07914 DY1 3 0.873501 0.556230 0.534472 11.00000 0.01754 0.02924 = 0.02807 -0.00155 0.00008 0.00324 O3 5 0.697266 0.602486 0.604838 11.00000 0.01750 0.04119 = 0.04111 -0.00984 0.00112 0.00316 O1 5 0.914485 0.488129 0.398666 11.00000 0.02180 0.03389 = 0.02354 -0.00389 -0.00085 0.00614 O4 5 0.837304 0.616312 0.365598 11.00000 0.02718 0.05011 = 0.04241 0.01408 -0.00014 -0.00232 O2 5 1.069575 0.451101 0.241099 11.00000 0.02450 0.05443 = 0.03064 -0.00680 0.00296 0.00831 N2 4 0.530006 0.565295 0.473017 11.00000 0.01676 0.03207 = 0.03765 -0.00133 0.00334 0.00267 O5 5 1.056102 0.595870 0.389975 11.00000 0.03588 0.04492 = 0.04400 0.00582 -0.00253 0.01043 O6 5 0.970462 0.640969 0.606987 11.00000 0.02118 0.03758 = 0.06319 -0.01284 -0.00025 0.00064 PART 2 AFIX 83 H6B 2 1.055411 0.640633 0.607024 10.15000 -1.50000 AFIX 83 PART 1 H6A 2 1.055265 0.643637 0.617577 10.85000 -1.50000 AFIX 0 PART 0 N1 4 0.643851 0.540020 0.425359 11.00000 0.01918 0.03167 = 0.02994 0.00058 0.00264 0.00208 O7 5 0.747565 0.480239 0.625712 11.00000 0.03042 0.03385 = 0.03829 0.00202 0.00061 0.00038 H7A 2 0.793751 0.449657 0.631909 11.00000 -1.50000 H7B 2 0.675111 0.468925 0.590023 11.00000 -1.50000 C9 1 0.614605 0.513657 0.328895 11.00000 0.02013 0.03732 = 0.03518 -0.00066 -0.00173 0.00161 AFIX 43 H9 2 0.521290 0.511503 0.301571 11.00000 -1.20000 AFIX 0 C16 1 0.958397 0.619775 0.333047 11.00000 0.02984 0.03282 = 0.03678 -0.00090 -0.00188 0.00125 C6 1 0.711787 0.486670 0.257330 11.00000 0.02597 0.03611 = 0.02838 -0.00069 -0.00225 0.00515 C17 1 0.980100 0.653213 0.225878 11.00000 0.03148 0.03395 = 0.03812 -0.00201 0.00392 -0.00199 C10 1 0.572717 0.596785 0.562641 11.00000 0.01885 0.02955 = 0.03665 0.00377 0.00249 0.00171 C1 1 0.852598 0.478027 0.290894 11.00000 0.02642 0.02834 = 0.02329 -0.00004 -0.00087 0.00168 C2 1 0.931781 0.455608 0.203331 11.00000 0.02946 0.03613 = 0.03099 -0.00300 0.00051 0.00485 O10 5 0.618449 0.692798 0.337361 11.00000 0.05591 0.05854 = 0.08036 -0.01139 0.00393 0.01261 AFIX 147 H10 2 0.686689 0.672362 0.345468 11.00000 -1.50000 AFIX 0 C19 1 0.891198 0.699665 0.051514 11.00000 0.05634 0.04910 = 0.03407 0.00422 -0.00176 0.00500 N3 4 0.238092 0.658531 0.640809 11.00000 0.02361 0.05285 = 0.07150 -0.02184 0.00374 0.00636 C11 1 0.469148 0.629659 0.622593 11.00000 0.02059 0.03213 = 0.03699 0.00006 0.00386 0.00097 C4 1 0.734718 0.445297 0.062786 11.00000 0.04504 0.06037 = 0.03515 -0.01401 -0.00947 0.01097 C5 1 0.656901 0.469318 0.145165 11.00000 0.03111 0.05108 = 0.03939 -0.00660 -0.01024 0.00963 AFIX 43 H5 2 0.562450 0.474294 0.125100 11.00000 -1.20000 AFIX 0 C21 1 1.128973 0.704051 0.106821 11.00000 0.05464 0.05945 = 0.06736 0.01375 0.01683 -0.01312 AFIX 43 H21 2 1.217607 0.716307 0.093247 11.00000 -1.20000 AFIX 0 C20 1 1.019423 0.718703 0.028998 11.00000 0.07773 0.04979 = 0.04956 0.01467 0.01973 -0.00357 AFIX 43 H20 2 1.031629 0.740969 -0.037356 11.00000 -1.20000 AFIX 0 C15 1 0.510912 0.660789 0.720392 11.00000 0.02302 0.05169 = 0.04990 -0.01196 -0.00224 0.00400 AFIX 43 H15 2 0.604033 0.661471 0.748782 11.00000 -1.20000 AFIX 0 C22 1 1.110600 0.671662 0.204393 11.00000 0.03414 0.04814 = 0.05488 0.00586 0.00365 -0.00413 AFIX 43 H22 2 1.186562 0.661994 0.256649 11.00000 -1.20000 AFIX 0 C18 1 0.868601 0.667518 0.148200 11.00000 0.03512 0.05220 = 0.03477 0.00238 0.00140 0.00020 AFIX 43 H18 2 0.779621 0.655520 0.161321 11.00000 -1.20000 AFIX 0 C7 1 1.160858 0.434828 0.154892 11.00000 0.03828 0.09740 = 0.03796 -0.00820 0.00935 0.01912 AFIX 137 H7C 2 1.254926 0.437369 0.189188 11.00000 -1.50000 H7D 2 1.148468 0.458940 0.086434 11.00000 -1.50000 H7E 2 1.141125 0.397133 0.130552 11.00000 -1.50000 AFIX 0 C8 1 0.670667 0.425583 -0.055601 11.00000 0.06505 0.10644 = 0.05116 -0.03938 -0.02418 0.02671 AFIX 137 H8A 2 0.669034 0.385616 -0.056675 11.00000 -1.50000 H8B 2 0.724201 0.438905 -0.118289 11.00000 -1.50000 H8C 2 0.577584 0.439554 -0.067957 11.00000 -1.50000 AFIX 0 C14 1 0.415850 0.691121 0.777041 11.00000 0.03796 0.06046 = 0.05548 -0.02561 0.00041 0.00523 AFIX 43 H14 2 0.443850 0.713359 0.842667 11.00000 -1.20000 AFIX 0 C24 1 0.514851 0.666802 0.266587 11.00000 0.05195 0.06494 = 0.07344 0.00970 -0.00385 0.00324 AFIX 137 H24A 2 0.529147 0.672777 0.183670 11.00000 -1.50000 H24B 2 0.426577 0.681897 0.283402 11.00000 -1.50000 H24C 2 0.516513 0.627586 0.283287 11.00000 -1.50000 AFIX 0 C13 1 0.280934 0.688264 0.736222 11.00000 0.02989 0.05578 = 0.06253 -0.02388 0.00740 0.00924 AFIX 43 H13 2 0.215891 0.707837 0.776466 11.00000 -1.20000 AFIX 0 C12 1 0.330621 0.630041 0.585394 11.00000 0.02022 0.04652 = 0.05854 -0.01889 0.00065 0.00230 AFIX 43 H12 2 0.300386 0.609297 0.518066 11.00000 -1.20000 AFIX 0 C3 1 0.875777 0.439534 0.093732 11.00000 0.04346 0.05600 = 0.02963 -0.01102 -0.00376 0.01418 AFIX 43 H3 2 0.932551 0.424490 0.038751 11.00000 -1.20000 AFIX 0 PART 2 O8B 5 0.666264 0.688534 -0.017898 10.50000 0.07005 0.12760 = 0.05891 0.00959 -0.02918 0.02135 PART 1 O8A 5 0.655885 0.710050 0.004453 10.50000 0.06399 0.11004 = 0.06796 0.01077 -0.01380 0.02189 O9A 5 0.796298 0.734025 -0.125719 10.50000 0.10473 0.10694 = 0.04537 0.02947 -0.01005 0.00769 PART 2 O9B 5 0.783262 0.750741 -0.104349 10.50000 0.15645 0.10241 = 0.06183 0.03675 0.00826 0.05382 PART 0 N4 4 0.771525 0.714918 -0.029250 11.00000 0.08035 0.08844 = 0.04184 0.01314 -0.00997 0.01380 PART 2 C23B 1 0.929857 0.683543 0.684900 10.15000 0.05378 0.05962 = 0.05752 -0.01654 0.00394 -0.00314 AFIX 137 H23A 2 0.976171 0.678227 0.763245 10.15000 -1.50000 H23B 2 0.831290 0.681994 0.689885 10.15000 -1.50000 H23C 2 0.954651 0.719198 0.654257 10.15000 -1.50000 AFIX 0 PART 1 C23A 1 0.912172 0.693537 0.602753 10.85000 0.03717 0.03422 = 0.11125 -0.00952 -0.00003 0.00176 AFIX 137 H23D 2 0.812972 0.690408 0.599666 10.85000 -1.50000 H23E 2 0.937954 0.712688 0.532613 10.85000 -1.50000 H23F 2 0.945091 0.714039 0.673037 10.85000 -1.50000 AFIX 0 HKLF 4 REM njap-269_rt_r_a.res in P2(1)/n REM wR2 = 0.0712, GooF = S = 1.054, Restrained GooF = 1.055 for all data REM R1 = 0.0280 for 4693 Fo > 4sig(Fo) and 0.0314 for all 5161 data REM 391 parameters refined using 47 restraints END WGHT 0.0381 1.1699 REM Highest difference peak 0.611, deepest hole -0.743, 1-sigma level 0.073 Q1 1 1.0934 0.4428 0.3508 11.00000 0.05 0.61 Q2 1 0.8398 0.5563 0.4229 11.00000 0.05 0.61 ; _shelx_res_checksum 12678 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.87350(2) 0.55623(2) 0.53447(2) 0.02504(7) Uani 1 1 d D . . . . O3 O 0.69727(19) 0.60249(9) 0.60484(19) 0.0333(5) Uani 1 1 d . . . . . O1 O 0.91448(18) 0.48813(8) 0.39867(16) 0.0266(4) Uani 1 1 d . . . . . O4 O 0.8373(2) 0.61631(10) 0.3656(2) 0.0401(5) Uani 1 1 d . . . . . O2 O 1.0696(2) 0.45110(9) 0.24110(19) 0.0365(5) Uani 1 1 d . . . . . N2 N 0.5300(2) 0.56530(10) 0.4730(2) 0.0288(5) Uani 1 1 d . . . . . O5 O 1.0561(2) 0.59587(10) 0.3900(2) 0.0419(5) Uani 1 1 d . . . . . O6 O 0.9705(2) 0.64097(9) 0.6070(2) 0.0409(5) Uani 1 1 d . . . . . H6B H 1.055411 0.640633 0.607024 0.061 Uiso 0.15 1 calc R U P A 2 H6A H 1.055265 0.643637 0.617577 0.061 Uiso 0.85 1 calc R U P B 1 N1 N 0.6439(2) 0.54002(10) 0.4254(2) 0.0269(5) Uani 1 1 d . . . . . O7 O 0.7476(2) 0.48024(9) 0.62571(19) 0.0343(5) Uani 1 1 d D . . . . H7A H 0.794(3) 0.4497(9) 0.632(4) 0.051 Uiso 1 1 d D U . . . H7B H 0.675(2) 0.4689(14) 0.590(3) 0.051 Uiso 1 1 d D U . . . C9 C 0.6146(3) 0.51366(13) 0.3289(3) 0.0311(6) Uani 1 1 d . . . . . H9 H 0.521290 0.511503 0.301571 0.037 Uiso 1 1 calc R U . . . C16 C 0.9584(3) 0.61977(13) 0.3330(3) 0.0334(6) Uani 1 1 d . . . . . C6 C 0.7118(3) 0.48667(13) 0.2573(3) 0.0304(6) Uani 1 1 d . . . . . C17 C 0.9801(3) 0.65321(13) 0.2259(3) 0.0345(7) Uani 1 1 d . . . . . C10 C 0.5727(3) 0.59678(12) 0.5626(3) 0.0283(6) Uani 1 1 d . . . . . C1 C 0.8526(3) 0.47803(12) 0.2909(2) 0.0262(5) Uani 1 1 d . . . . . C2 C 0.9318(3) 0.45561(13) 0.2033(3) 0.0323(6) Uani 1 1 d . . . . . O10 O 0.6184(3) 0.69280(13) 0.3374(3) 0.0650(8) Uani 1 1 d . . . . . H10 H 0.686689 0.672362 0.345468 0.098 Uiso 1 1 calc R U . . . C19 C 0.8912(4) 0.69967(16) 0.0515(3) 0.0468(8) Uani 1 1 d . . . . . N3 N 0.2381(3) 0.65853(13) 0.6408(3) 0.0493(8) Uani 1 1 d . . . . . C11 C 0.4691(3) 0.62966(12) 0.6226(3) 0.0298(6) Uani 1 1 d . . . . . C4 C 0.7347(4) 0.44530(16) 0.0628(3) 0.0475(9) Uani 1 1 d . . . . . C5 C 0.6569(3) 0.46932(15) 0.1452(3) 0.0412(7) Uani 1 1 d . . . . . H5 H 0.562450 0.474294 0.125100 0.049 Uiso 1 1 calc R U . . . C21 C 1.1290(5) 0.70405(18) 0.1068(4) 0.0598(11) Uani 1 1 d . . . . . H21 H 1.217607 0.716307 0.093247 0.072 Uiso 1 1 calc R U . . . C20 C 1.0194(5) 0.71870(17) 0.0290(4) 0.0582(10) Uani 1 1 d . . . . . H20 H 1.031629 0.740969 -0.037356 0.070 Uiso 1 1 calc R U . . . C15 C 0.5109(3) 0.66079(15) 0.7204(3) 0.0418(8) Uani 1 1 d . . . . . H15 H 0.604033 0.661471 0.748782 0.050 Uiso 1 1 calc R U . . . C22 C 1.1106(4) 0.67166(16) 0.2044(3) 0.0457(8) Uani 1 1 d . . . . . H22 H 1.186562 0.661994 0.256649 0.055 Uiso 1 1 calc R U . . . C18 C 0.8686(3) 0.66752(15) 0.1482(3) 0.0408(7) Uani 1 1 d . . . . . H18 H 0.779621 0.655520 0.161321 0.049 Uiso 1 1 calc R U . . . C7 C 1.1609(4) 0.4348(2) 0.1549(3) 0.0575(11) Uani 1 1 d . . . . . H7C H 1.254926 0.437369 0.189188 0.086 Uiso 1 1 calc R U . . . H7D H 1.148468 0.458940 0.086434 0.086 Uiso 1 1 calc R U . . . H7E H 1.141125 0.397133 0.130552 0.086 Uiso 1 1 calc R U . . . C8 C 0.6707(5) 0.4256(3) -0.0556(4) 0.0758(15) Uani 1 1 d . . . . . H8A H 0.669034 0.385616 -0.056675 0.114 Uiso 1 1 calc R U . . . H8B H 0.724201 0.438905 -0.118289 0.114 Uiso 1 1 calc R U . . . H8C H 0.577584 0.439554 -0.067957 0.114 Uiso 1 1 calc R U . . . C14 C 0.4158(4) 0.69112(17) 0.7770(4) 0.0515(9) Uani 1 1 d . . . . . H14 H 0.443850 0.713359 0.842667 0.062 Uiso 1 1 calc R U . . . C24 C 0.5149(4) 0.6668(2) 0.2666(4) 0.0639(11) Uani 1 1 d . . . . . H24A H 0.529147 0.672777 0.183670 0.096 Uiso 1 1 calc R U . . . H24B H 0.426577 0.681897 0.283402 0.096 Uiso 1 1 calc R U . . . H24C H 0.516513 0.627586 0.283287 0.096 Uiso 1 1 calc R U . . . C13 C 0.2809(3) 0.68826(16) 0.7362(3) 0.0492(9) Uani 1 1 d . . . . . H13 H 0.215891 0.707837 0.776466 0.059 Uiso 1 1 calc R U . . . C12 C 0.3306(3) 0.63004(15) 0.5854(3) 0.0419(8) Uani 1 1 d . . . . . H12 H 0.300386 0.609297 0.518066 0.050 Uiso 1 1 calc R U . . . C3 C 0.8758(4) 0.43953(15) 0.0937(3) 0.0434(8) Uani 1 1 d . . . . . H3 H 0.932551 0.424490 0.038751 0.052 Uiso 1 1 calc R U . . . O8B O 0.6663(8) 0.6885(5) -0.0179(12) 0.087(4) Uani 0.5 1 d D U P C 2 O8A O 0.6559(8) 0.7101(5) 0.0045(13) 0.082(4) Uani 0.5 1 d D U P C 1 O9A O 0.7963(13) 0.7340(6) -0.1257(8) 0.087(4) Uani 0.5 1 d D U P C 1 O9B O 0.7833(17) 0.7507(6) -0.1043(10) 0.107(6) Uani 0.5 1 d D U P C 2 N4 N 0.7715(4) 0.71492(18) -0.0292(3) 0.0710(11) Uani 1 1 d D . . . . C23B C 0.930(3) 0.6835(13) 0.685(3) 0.057(7) Uani 0.15 1 d . U P D 2 H23A H 0.976171 0.678227 0.763245 0.086 Uiso 0.15 1 calc R U P D 2 H23B H 0.831290 0.681994 0.689885 0.086 Uiso 0.15 1 calc R U P D 2 H23C H 0.954651 0.719198 0.654257 0.086 Uiso 0.15 1 calc R U P D 2 C23A C 0.9122(5) 0.69354(19) 0.6028(7) 0.0612(14) Uani 0.85 1 d . U P D 1 H23D H 0.812972 0.690408 0.599666 0.092 Uiso 0.85 1 calc R U P D 1 H23E H 0.937954 0.712688 0.532613 0.092 Uiso 0.85 1 calc R U P D 1 H23F H 0.945091 0.714039 0.673037 0.092 Uiso 0.85 1 calc R U P D 1 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 0.01754(9) 0.02924(10) 0.02807(10) -0.00155(6) 0.00008(6) 0.00324(6) O3 0.0175(9) 0.0412(12) 0.0411(12) -0.0098(9) 0.0011(8) 0.0032(8) O1 0.0218(9) 0.0339(10) 0.0235(9) -0.0039(8) -0.0008(7) 0.0061(8) O4 0.0272(11) 0.0501(14) 0.0424(13) 0.0141(10) -0.0001(9) -0.0023(10) O2 0.0245(10) 0.0544(14) 0.0306(11) -0.0068(9) 0.0030(9) 0.0083(9) N2 0.0168(11) 0.0321(12) 0.0377(14) -0.0013(10) 0.0033(9) 0.0027(9) O5 0.0359(12) 0.0449(13) 0.0440(13) 0.0058(10) -0.0025(10) 0.0104(10) O6 0.0212(10) 0.0376(12) 0.0632(15) -0.0128(10) -0.0003(10) 0.0006(9) N1 0.0192(11) 0.0317(12) 0.0299(12) 0.0006(10) 0.0026(9) 0.0021(9) O7 0.0304(11) 0.0338(11) 0.0383(12) 0.0020(9) 0.0006(9) 0.0004(9) C9 0.0201(13) 0.0373(16) 0.0352(16) -0.0007(12) -0.0017(11) 0.0016(11) C16 0.0298(15) 0.0328(15) 0.0368(16) -0.0009(12) -0.0019(12) 0.0013(12) C6 0.0260(14) 0.0361(15) 0.0284(14) -0.0007(12) -0.0023(11) 0.0052(12) C17 0.0315(15) 0.0339(15) 0.0381(17) -0.0020(13) 0.0039(13) -0.0020(12) C10 0.0189(12) 0.0296(14) 0.0366(16) 0.0038(12) 0.0025(11) 0.0017(11) C1 0.0264(13) 0.0283(14) 0.0233(13) 0.0000(11) -0.0009(10) 0.0017(11) C2 0.0295(15) 0.0361(16) 0.0310(16) -0.0030(12) 0.0005(12) 0.0049(12) O10 0.0559(17) 0.0585(18) 0.080(2) -0.0114(15) 0.0039(15) 0.0126(14) C19 0.056(2) 0.049(2) 0.0341(18) 0.0042(15) -0.0018(16) 0.0050(16) N3 0.0236(13) 0.0528(18) 0.072(2) -0.0218(15) 0.0037(13) 0.0064(12) C11 0.0206(13) 0.0321(14) 0.0370(16) 0.0001(12) 0.0039(11) 0.0010(11) C4 0.045(2) 0.060(2) 0.0352(19) -0.0140(15) -0.0095(15) 0.0110(16) C5 0.0311(16) 0.051(2) 0.0394(18) -0.0066(15) -0.0102(13) 0.0096(14) C21 0.055(2) 0.059(2) 0.067(3) 0.014(2) 0.017(2) -0.013(2) C20 0.078(3) 0.050(2) 0.050(2) 0.0147(18) 0.020(2) -0.004(2) C15 0.0230(14) 0.052(2) 0.050(2) -0.0120(15) -0.0022(13) 0.0040(13) C22 0.0341(17) 0.048(2) 0.055(2) 0.0059(16) 0.0036(15) -0.0041(15) C18 0.0351(16) 0.052(2) 0.0348(17) 0.0024(14) 0.0014(13) 0.0002(15) C7 0.038(2) 0.097(3) 0.038(2) -0.008(2) 0.0093(16) 0.019(2) C8 0.065(3) 0.106(4) 0.051(3) -0.039(3) -0.024(2) 0.027(3) C14 0.0380(18) 0.060(2) 0.055(2) -0.0256(18) 0.0004(16) 0.0052(17) C24 0.052(2) 0.065(3) 0.073(3) 0.010(2) -0.004(2) 0.003(2) C13 0.0299(16) 0.056(2) 0.063(2) -0.0239(18) 0.0074(15) 0.0092(15) C12 0.0202(14) 0.0465(19) 0.059(2) -0.0189(16) 0.0006(14) 0.0023(13) C3 0.0435(19) 0.056(2) 0.0296(17) -0.0110(14) -0.0038(14) 0.0142(16) O8B 0.070(6) 0.128(10) 0.059(6) 0.010(6) -0.029(4) 0.021(5) O8A 0.064(5) 0.110(8) 0.068(7) 0.011(6) -0.014(4) 0.022(5) O9A 0.105(7) 0.107(9) 0.045(5) 0.029(6) -0.010(4) 0.008(7) O9B 0.156(10) 0.102(9) 0.062(7) 0.037(6) 0.008(6) 0.054(7) N4 0.080(3) 0.088(3) 0.042(2) 0.0131(19) -0.0100(19) 0.014(2) C23B 0.054(13) 0.060(14) 0.058(13) -0.017(12) 0.004(12) -0.003(11) C23A 0.037(2) 0.034(2) 0.111(5) -0.010(3) 0.000(3) 0.0018(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' 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 O3 Dy1 Dy1 163.16(6) . 3_766 ? O3 Dy1 O1 140.23(7) . . ? O3 Dy1 O1 140.92(7) . 3_766 ? O3 Dy1 O4 84.91(8) . . ? O3 Dy1 O2 78.18(7) . 3_766 ? O3 Dy1 O5 126.81(7) . . ? O3 Dy1 O6 75.07(7) . . ? O3 Dy1 N1 64.67(8) . . ? O3 Dy1 O7 78.74(7) . . ? O1 Dy1 Dy1 36.97(4) . 3_766 ? O1 Dy1 Dy1 35.40(4) 3_766 3_766 ? O1 Dy1 O1 72.38(7) . 3_766 ? O1 Dy1 O4 85.88(8) . . ? O1 Dy1 O4 126.08(7) 3_766 . ? O1 Dy1 O2 62.90(6) 3_766 3_766 ? O1 Dy1 O2 124.98(7) . 3_766 ? O1 Dy1 O5 72.14(7) . . ? O1 Dy1 O5 75.76(6) 3_766 . ? O1 Dy1 O6 139.46(7) . . ? O1 Dy1 N1 75.94(7) . . ? O1 Dy1 N1 143.20(7) 3_766 . ? O1 Dy1 O7 88.87(7) 3_766 . ? O1 Dy1 O7 82.18(7) . . ? O4 Dy1 Dy1 109.15(6) . 3_766 ? O4 Dy1 O2 146.64(8) . 3_766 ? O4 Dy1 O5 50.49(7) . . ? O4 Dy1 N1 68.65(8) . . ? O4 Dy1 O7 137.13(7) . . ? O2 Dy1 Dy1 93.49(5) 3_766 3_766 ? O2 Dy1 O5 121.68(7) 3_766 . ? O5 Dy1 Dy1 70.02(5) . 3_766 ? O6 Dy1 Dy1 116.29(5) . 3_766 ? O6 Dy1 O1 88.27(7) . 3_766 ? O6 Dy1 O4 77.21(8) . . ? O6 Dy1 O2 70.76(8) . 3_766 ? O6 Dy1 O5 68.65(8) . . ? O6 Dy1 N1 128.40(8) . . ? O6 Dy1 O7 133.93(8) . . ? N1 Dy1 Dy1 110.96(6) . 3_766 ? N1 Dy1 O2 126.28(7) . 3_766 ? N1 Dy1 O5 111.64(7) . . ? O7 Dy1 Dy1 84.54(5) . 3_766 ? O7 Dy1 O2 67.17(7) . 3_766 ? O7 Dy1 O5 153.01(7) . . ? O7 Dy1 N1 68.52(8) . . ? C10 O3 Dy1 123.08(18) . . ? Dy1 O1 Dy1 107.62(7) . 3_766 ? C1 O1 Dy1 130.22(16) . . ? C1 O1 Dy1 121.26(16) . 3_766 ? C16 O4 Dy1 100.95(18) . . ? C2 O2 Dy1 116.04(17) . 3_766 ? C2 O2 C7 117.2(3) . . ? C7 O2 Dy1 124.0(2) . 3_766 ? C10 N2 N1 109.7(2) . . ? C16 O5 Dy1 87.84(18) . . ? Dy1 O6 H6B 111.2 . . ? Dy1 O6 H6A 118.8 . . ? C23B O6 Dy1 135.3(12) . . ? C23B O6 H6B 109.5 . . ? C23A O6 Dy1 128.9(3) . . ? C23A O6 H6A 109.5 . . ? N2 N1 Dy1 116.45(17) . . ? C9 N1 Dy1 129.01(19) . . ? C9 N1 N2 114.5(2) . . ? Dy1 O7 H7A 113(2) . . ? Dy1 O7 H7B 118(2) . . ? H7A O7 H7B 100(3) . . ? N1 C9 H9 116.9 . . ? N1 C9 C6 126.2(3) . . ? C6 C9 H9 116.9 . . ? O4 C16 C17 118.0(3) . . ? O5 C16 O4 120.7(3) . . ? O5 C16 C17 121.3(3) . . ? C1 C6 C9 125.7(3) . . ? C5 C6 C9 114.9(3) . . ? C5 C6 C1 119.4(3) . . ? C22 C17 C16 120.7(3) . . ? C18 C17 C16 119.7(3) . . ? C18 C17 C22 119.5(3) . . ? O3 C10 N2 125.8(3) . . ? O3 C10 C11 115.6(3) . . ? N2 C10 C11 118.5(2) . . ? O1 C1 C6 125.1(2) . . ? O1 C1 C2 118.4(2) . . ? C6 C1 C2 116.4(3) . . ? O2 C2 C1 112.9(3) . . ? C3 C2 O2 124.3(3) . . ? C3 C2 C1 122.8(3) . . ? C24 O10 H10 109.5 . . ? C20 C19 N4 119.3(3) . . ? C18 C19 C20 123.0(4) . . ? C18 C19 N4 117.7(3) . . ? C12 N3 C13 118.6(3) . . ? C15 C11 C10 119.4(3) . . ? C15 C11 C12 117.4(3) . . ? C12 C11 C10 123.2(3) . . ? C5 C4 C8 121.5(4) . . ? C5 C4 C3 117.3(3) . . ? C3 C4 C8 121.2(3) . . ? C6 C5 H5 118.4 . . ? C4 C5 C6 123.2(3) . . ? C4 C5 H5 118.4 . . ? C20 C21 H21 119.5 . . ? C20 C21 C22 120.9(4) . . ? C22 C21 H21 119.5 . . ? C19 C20 H20 121.1 . . ? C21 C20 C19 117.8(3) . . ? C21 C20 H20 121.1 . . ? C11 C15 H15 120.0 . . ? C11 C15 C14 119.9(3) . . ? C14 C15 H15 120.0 . . ? C17 C22 H22 119.9 . . ? C21 C22 C17 120.3(4) . . ? C21 C22 H22 119.9 . . ? C17 C18 H18 120.8 . . ? C19 C18 C17 118.5(3) . . ? C19 C18 H18 120.8 . . ? O2 C7 H7C 109.5 . . ? O2 C7 H7D 109.5 . . ? O2 C7 H7E 109.5 . . ? H7C C7 H7D 109.5 . . ? H7C C7 H7E 109.5 . . ? H7D C7 H7E 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C15 C14 H14 120.5 . . ? C13 C14 C15 118.9(3) . . ? C13 C14 H14 120.5 . . ? O10 C24 H24A 109.5 . . ? O10 C24 H24B 109.5 . . ? O10 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C13 C14 122.1(3) . . ? N3 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? N3 C12 C11 123.0(3) . . ? N3 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? O8B N4 C19 115.7(7) . . ? O8B N4 O9B 124.6(6) . . ? O8A N4 C19 119.2(8) . . ? O8A N4 O9A 124.4(5) . . ? O9A N4 C19 116.3(7) . . ? O9B N4 C19 119.6(9) . . ? O6 C23B H23A 109.5 . . ? O6 C23B H23B 109.5 . . ? O6 C23B H23C 109.5 . . ? H23A C23B H23B 109.5 . . ? H23A C23B H23C 109.5 . . ? H23B C23B H23C 109.5 . . ? O6 C23A H23D 109.5 . . ? O6 C23A H23E 109.5 . . ? O6 C23A H23F 109.5 . . ? H23D C23A H23E 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? 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 Dy1 Dy1 3.8050(3) 3_766 ? Dy1 O3 2.2541(19) . ? Dy1 O1 2.4013(18) 3_766 ? Dy1 O1 2.3128(18) . ? Dy1 O4 2.406(2) . ? Dy1 O2 2.560(2) 3_766 ? Dy1 O5 2.693(2) . ? Dy1 O6 2.381(2) . ? Dy1 N1 2.502(2) . ? Dy1 O7 2.487(2) . ? O3 C10 1.278(3) . ? O1 C1 1.338(3) . ? O4 C16 1.270(4) . ? O2 C2 1.383(4) . ? O2 C7 1.429(4) . ? N2 N1 1.415(3) . ? N2 C10 1.310(4) . ? O5 C16 1.250(4) . ? O6 H6B 0.8300 . ? O6 H6A 0.8300 . ? O6 C23B 1.43(3) . ? O6 C23A 1.396(5) . ? N1 C9 1.277(4) . ? O7 H7A 0.868(18) . ? O7 H7B 0.832(18) . ? C9 H9 0.9400 . ? C9 C6 1.453(4) . ? C16 C17 1.488(4) . ? C6 C1 1.413(4) . ? C6 C5 1.401(4) . ? C17 C22 1.391(4) . ? C17 C18 1.387(5) . ? C10 C11 1.494(4) . ? C1 C2 1.414(4) . ? C2 C3 1.370(5) . ? O10 H10 0.8300 . ? O10 C24 1.390(5) . ? C19 C20 1.378(6) . ? C19 C18 1.375(5) . ? C19 N4 1.471(5) . ? N3 C13 1.336(5) . ? N3 C12 1.334(4) . ? C11 C15 1.374(4) . ? C11 C12 1.384(4) . ? C4 C5 1.379(5) . ? C4 C8 1.509(5) . ? C4 C3 1.401(5) . ? C5 H5 0.9400 . ? C21 H21 0.9400 . ? C21 C20 1.376(6) . ? C21 C22 1.378(5) . ? C20 H20 0.9400 . ? C15 H15 0.9400 . ? C15 C14 1.383(5) . ? C22 H22 0.9400 . ? C18 H18 0.9400 . ? C7 H7C 0.9700 . ? C7 H7D 0.9700 . ? C7 H7E 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C14 H14 0.9400 . ? C14 C13 1.363(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C13 H13 0.9400 . ? C12 H12 0.9400 . ? C3 H3 0.9400 . ? O8B N4 1.227(4) . ? O8A N4 1.227(4) . ? O9A N4 1.227(4) . ? O9B N4 1.227(4) . ? C23B H23A 0.9700 . ? C23B H23B 0.9700 . ? C23B H23C 0.9700 . ? C23A H23D 0.9700 . ? C23A H23E 0.9700 . ? C23A H23F 0.9700 . ? 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 _geom_torsion_publ_flag Dy1 O3 C10 N2 -1.8(4) . . . . ? Dy1 O3 C10 C11 178.41(18) . . . . ? Dy1 O1 C1 C6 158.1(2) 3_766 . . . ? Dy1 O1 C1 C6 -34.2(4) . . . . ? Dy1 O1 C1 C2 -20.1(3) 3_766 . . . ? Dy1 O1 C1 C2 147.5(2) . . . . ? Dy1 O4 C16 O5 -1.8(3) . . . . ? Dy1 O4 C16 C17 178.4(2) . . . . ? Dy1 O2 C2 C1 24.9(3) 3_766 . . . ? Dy1 O2 C2 C3 -154.2(3) 3_766 . . . ? Dy1 O5 C16 O4 1.6(3) . . . . ? Dy1 O5 C16 C17 -178.7(3) . . . . ? Dy1 N1 C9 C6 -0.8(5) . . . . ? O3 C10 C11 C15 -3.4(4) . . . . ? O3 C10 C11 C12 177.4(3) . . . . ? O1 C1 C2 O2 -4.7(4) . . . . ? O1 C1 C2 C3 174.4(3) . . . . ? O4 C16 C17 C22 161.7(3) . . . . ? O4 C16 C17 C18 -16.5(5) . . . . ? O2 C2 C3 C4 179.7(3) . . . . ? N2 N1 C9 C6 176.1(3) . . . . ? N2 C10 C11 C15 176.8(3) . . . . ? N2 C10 C11 C12 -2.4(4) . . . . ? O5 C16 C17 C22 -18.1(5) . . . . ? O5 C16 C17 C18 163.8(3) . . . . ? N1 N2 C10 O3 -2.7(4) . . . . ? N1 N2 C10 C11 177.1(2) . . . . ? N1 C9 C6 C1 9.9(5) . . . . ? N1 C9 C6 C5 -168.9(3) . . . . ? C9 C6 C1 O1 7.6(5) . . . . ? C9 C6 C1 C2 -174.1(3) . . . . ? C9 C6 C5 C4 176.9(3) . . . . ? C16 C17 C22 C21 -178.0(3) . . . . ? C16 C17 C18 C19 178.3(3) . . . . ? C6 C1 C2 O2 176.8(3) . . . . ? C6 C1 C2 C3 -4.1(5) . . . . ? C10 N2 N1 Dy1 5.3(3) . . . . ? C10 N2 N1 C9 -172.1(3) . . . . ? C10 C11 C15 C14 -179.6(3) . . . . ? C10 C11 C12 N3 178.5(3) . . . . ? C1 C6 C5 C4 -2.0(5) . . . . ? C1 C2 C3 C4 0.7(6) . . . . ? C11 C15 C14 C13 1.8(6) . . . . ? C5 C6 C1 O1 -173.7(3) . . . . ? C5 C6 C1 C2 4.6(4) . . . . ? C5 C4 C3 C2 2.2(6) . . . . ? C20 C19 C18 C17 -0.6(6) . . . . ? C20 C19 N4 O8B 166.5(8) . . . . ? C20 C19 N4 O8A -162.1(8) . . . . ? C20 C19 N4 O9A 15.0(11) . . . . ? C20 C19 N4 O9B -11.1(11) . . . . ? C20 C21 C22 C17 -0.1(6) . . . . ? C15 C11 C12 N3 -0.7(5) . . . . ? C15 C14 C13 N3 -2.3(7) . . . . ? C22 C17 C18 C19 0.1(5) . . . . ? C22 C21 C20 C19 -0.4(7) . . . . ? C18 C17 C22 C21 0.2(6) . . . . ? C18 C19 C20 C21 0.7(6) . . . . ? C18 C19 N4 O8B -14.7(9) . . . . ? C18 C19 N4 O8A 16.7(10) . . . . ? C18 C19 N4 O9A -166.2(10) . . . . ? C18 C19 N4 O9B 167.7(10) . . . . ? C7 O2 C2 C1 -173.0(3) . . . . ? C7 O2 C2 C3 7.9(5) . . . . ? C8 C4 C5 C6 178.1(4) . . . . ? C8 C4 C3 C2 -177.4(4) . . . . ? C13 N3 C12 C11 0.3(6) . . . . ? C12 N3 C13 C14 1.2(6) . . . . ? C12 C11 C15 C14 -0.4(5) . . . . ? C3 C4 C5 C6 -1.5(6) . . . . ? N4 C19 C20 C21 179.5(4) . . . . ? N4 C19 C18 C17 -179.4(3) . . . . ?