#------------------------------------------------------------------------------ #$Date: 2026-05-19 23:56:56 +0100 (Tue, 19 May 2026) $ #$Revision: 305998 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721037.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_7721037 loop_ _publ_author_name 'Liu, Cai-Ming' 'Zhang, Yi-Quan' 'Hao, Xiang' 'Li, Xi-Li' _publ_section_title ; Effect of solvents on multifunctional Dy2 complexes with axial chiral ligands (R)/(S)-1,1'-binaphthyl-2,2'-diyl hydrogen phosphate ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00796A _journal_year 2026 _chemical_formula_moiety 'C72 H52 Cl2 Dy2 F2 N8 O14 P2, 3(C3 H7 N O)' _chemical_formula_sum 'C81 H73 Cl2 Dy2 F2 N11 O17 P2' _chemical_formula_weight 1968.34 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2025-12-15 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2025-12-16 deposited with the CCDC. 2026-05-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.61218(14) _cell_length_b 14.05975(19) _cell_length_c 58.5896(7) _cell_measurement_reflns_used 19776 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 74.4310 _cell_measurement_theta_min 3.8550 _cell_volume 7918.08(18) _computing_cell_refinement 'CrysAlisPro 1.171.43.75a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.43.75a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.43.75a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.3 (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 -5.00 21.00 0.50 0.16 -- -40.81 57.00-120.00 52 2 \w -8.00 32.00 0.50 0.16 -- -50.00 30.00-120.00 80 3 \w 16.00 42.00 0.50 0.16 -- -40.81 19.00 -60.00 52 4 \w 16.00 42.00 0.50 0.16 -- -40.81 19.00 -30.00 52 5 \w 17.00 42.00 0.50 0.16 -- -40.81 19.00 120.00 50 6 \w 81.00 107.00 0.50 0.66 -- 108.87 15.00-180.00 52 7 \w 98.00 171.00 0.50 0.66 -- 108.87 39.00-150.00 146 8 \w 93.00 173.00 0.50 0.66 -- 108.87 116.00 69.00 160 9 \w 34.00 59.00 0.50 0.66 -- 108.87 -77.00 90.00 50 10 \w 43.00 69.00 0.50 0.66 -- 108.87 -77.00 60.00 52 11 \w 38.00 67.00 0.50 0.66 -- 108.87 -77.00 30.00 58 12 \w 34.00 59.00 0.50 0.66 -- 108.87 -77.00 -90.00 50 13 \w 35.00 66.00 0.50 0.66 -- 108.87 -77.00-150.00 62 14 \w 38.00 64.00 0.50 0.66 -- 108.87 -77.00-180.00 52 15 \w 50.00 76.00 0.50 0.66 -- 108.87 -85.00-128.00 52 16 \w 37.00 82.00 0.50 0.16 -- 40.81-116.00 -18.00 90 17 \w 46.00 98.00 0.50 0.66 -- 108.87-125.00 -60.00 104 18 \w 43.00 87.00 0.50 0.66 -- 108.87 -95.00 150.00 88 19 \w -106.00 -33.00 0.50 0.16 -- -50.00 -39.00 54.00 146 20 \w 33.00 88.00 0.50 0.16 -- 41.06 19.00-150.00 110 21 \w -9.00 16.00 0.50 0.16 -- -50.00 30.00-180.00 50 22 \w 34.00 61.00 0.50 0.66 -- 108.87 -77.00 -30.00 54 23 \w 75.00 100.00 0.50 0.66 -- 108.87 15.00 -30.00 50 24 \w 43.00 69.00 0.50 0.66 -- 108.87 -77.00 -60.00 52 25 \w 34.00 59.00 0.50 0.66 -- 108.87 -85.00-128.00 50 26 \w 75.00 113.00 0.50 0.66 -- 108.87 15.00 150.00 76 27 \w 37.00 92.00 0.50 0.66 -- 108.87 -95.00-180.00 110 28 \w 91.00 117.00 0.50 0.66 -- 108.87 45.00 -60.00 52 29 \w 130.00 171.00 0.50 0.66 -- 108.87 45.00 -60.00 82 30 \w 98.00 126.00 0.50 0.66 -- 108.87 125.00 30.00 56 31 \w 138.00 164.00 0.50 0.66 -- 108.87 125.00 30.00 52 32 \w 120.00 173.00 0.50 0.66 -- 108.87 77.00-180.00 106 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'ROD, Synergy Custom system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1426645000 _diffrn_orient_matrix_UB_12 -0.0348946000 _diffrn_orient_matrix_UB_13 -0.0085715000 _diffrn_orient_matrix_UB_21 -0.0688846000 _diffrn_orient_matrix_UB_22 0.0903426000 _diffrn_orient_matrix_UB_23 0.0096847000 _diffrn_orient_matrix_UB_31 0.0240943000 _diffrn_orient_matrix_UB_32 0.0513566000 _diffrn_orient_matrix_UB_33 -0.0228841000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_unetI/netI 0.0449 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_limit_l_min -68 _diffrn_reflns_number 43771 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 63.998 _diffrn_reflns_theta_max 63.998 _diffrn_reflns_theta_min 3.874 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 11.671 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.77256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.75a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellow' _exptl_crystal_density_diffrn 1.651 _exptl_crystal_description plate _exptl_crystal_F_000 3944 _exptl_crystal_preparation 'Magnetic properties' _refine_diff_density_max 1.780 _refine_diff_density_min -1.251 _refine_diff_density_rms 0.134 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.034(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1065 _refine_ls_number_reflns 13089 _refine_ls_number_restraints 60 _refine_ls_restrained_S_all 1.201 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0590 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+79.9757P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1352 _refine_ls_wR_factor_ref 0.1359 _reflns_Friedel_coverage 0.780 _reflns_Friedel_fraction_full 0.993 _reflns_Friedel_fraction_max 0.993 _reflns_number_gt 12654 _reflns_number_total 13089 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00796a2.cif _cod_data_source_block s2 _cod_original_cell_volume 7918.09(18) _cod_database_code 7721037 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula CHNOFClDy _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. ; _reflns_odcompleteness_completeness 99.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.966(6) 0.034(6) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances C2-C1 1.4 with sigma of 0.02 N10-C77 = N10-C78 = N8-C71 = N8-C70 1.45 with sigma of 0.02 4. Rigid bond restraints O14, C70 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Uiso/Uaniso restraints and constraints O4 \\sim C21: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A C10: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A Uanis(C2) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.005 Uanis(N8) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 6.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C13(H13), C15(H15), C16(H16), C18(H18), C20(H20), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C59(H59), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C67(H67), C70(H70), C76(H76), C73(H73), C79(H79) 6.b Idealised Me refined as rotating group: C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,H72B, H72C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C74(H74A,H74B,H74C), C75(H75A, H75B,H75C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C) ; _shelx_res_file ; TITL exp_239_auto_a.res in P2(1)2(1)2(1) s2.res created by SHELXL-2018/3 at 14:18:27 on 15-Dec-2025 REM Old TITL exp_239_auto in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.094, Rweak 0.080, Alpha 0.017 REM 1.020 for 45 systematic absences, Orientation as input REM Flack x = 0.040 ( 0.004 ) from 6083 Parsons' quotients REM Formula found by SHELXT: C4 C27 O10 F12 Cl4 Dy1 CELL 1.54184 9.612183 14.059751 58.589651 90 90 90 ZERR 4 0.000143 0.000193 0.000653 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Cl Dy F N O P UNIT 324 292 8 8 8 44 68 8 DFIX 1.4 C2 C1 ISOR 0.004 0.005 C2 C10 ISOR 0.005 0.01 N8 C71 C72 C78 C77 N10 DFIX 1.45 N10 C77 N10 C78 N8 C71 N8 C70 SIMU 0.01 0.02 2 O4 C21 SIMU 0.001 0.002 2 C10 DELU O14 C70 L.S. 30 PLAN 5 TEMP -173 CONF MORE -1 BOND $H fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT -2 128 OMIT 0 14 2 OMIT -6 10 1 OMIT 9 0 1 OMIT -1 14 2 REM REM REM WGHT 0.000000 79.975700 BASF 0.03382 FVAR 0.20658 C1 1 0.818454 0.682866 0.356684 11.00000 0.01898 0.04261 = 0.01903 -0.00339 -0.00012 0.02080 C2 1 0.865904 0.781665 0.356782 11.00000 0.03595 0.02640 = 0.03015 0.00158 0.00065 0.00756 AFIX 43 H2 2 0.811714 0.830880 0.363445 11.00000 -1.20000 AFIX 0 C3 1 0.991930 0.800044 0.346841 11.00000 0.03664 0.03133 = 0.02958 -0.00621 -0.00102 -0.00168 AFIX 43 H3 2 1.026679 0.863290 0.347098 11.00000 -1.20000 AFIX 0 C4 1 1.070282 0.730283 0.336478 11.00000 0.01996 0.03227 = 0.03016 -0.00351 0.00483 0.00296 C5 1 1.030650 0.637092 0.336012 11.00000 0.01694 0.03114 = 0.02389 0.00095 -0.00011 0.00462 AFIX 43 H5 2 1.089266 0.590009 0.329471 11.00000 -1.20000 AFIX 0 C6 1 0.902655 0.612675 0.345318 11.00000 0.00837 0.02223 = 0.02595 -0.00325 -0.00034 0.00521 C7 1 0.863404 0.512978 0.344201 11.00000 0.02636 0.01715 = 0.01469 0.00344 0.00130 0.00792 AFIX 43 H7 2 0.935205 0.469068 0.340579 11.00000 -1.20000 AFIX 0 C8 1 0.618252 0.346220 0.354279 11.00000 0.02869 0.04522 = 0.00823 -0.00613 0.00286 0.01598 C9 1 0.600045 0.240971 0.353501 11.00000 0.02818 0.01108 = 0.02079 0.00341 0.00332 -0.00166 C10 1 0.698245 0.179392 0.345114 11.00000 0.02604 0.01768 = 0.02444 -0.00038 0.00068 0.00511 AFIX 43 H10 2 0.784192 0.201591 0.339138 11.00000 -1.20000 AFIX 0 C11 1 0.667006 0.085437 0.345747 11.00000 0.03208 0.01994 = 0.02889 0.00033 0.00769 -0.00418 C12 1 0.546569 0.050057 0.354781 11.00000 0.03182 0.01680 = 0.04390 -0.00443 0.00570 -0.00244 AFIX 43 H12 2 0.527940 -0.016206 0.355631 11.00000 -1.20000 AFIX 0 C13 1 0.451908 0.119236 0.362756 11.00000 0.02727 0.03217 = 0.04008 -0.00653 0.00533 -0.00526 AFIX 43 H13 2 0.365197 0.098173 0.368671 11.00000 -1.20000 AFIX 0 C14 1 0.010353 0.223716 0.381056 11.00000 0.02414 0.02576 = 0.02672 -0.00483 0.00006 0.00291 C15 1 -0.034623 0.131776 0.383520 11.00000 0.01628 0.01577 = 0.04199 -0.00186 0.00507 0.00104 AFIX 43 H15 2 0.018456 0.082994 0.376446 11.00000 -1.20000 AFIX 0 C16 1 -0.150775 0.105397 0.395473 11.00000 0.01850 0.01644 = 0.04517 -0.00354 -0.00345 0.00111 AFIX 43 H16 2 -0.176354 0.040480 0.397092 11.00000 -1.20000 AFIX 0 C17 1 -0.229126 0.177417 0.405077 11.00000 0.02507 0.02964 = 0.02117 0.00229 0.00452 -0.00594 C18 1 -0.194553 0.268013 0.403635 11.00000 0.02360 0.02322 = 0.02589 -0.00111 0.00858 0.00379 AFIX 43 H18 2 -0.253118 0.314724 0.410339 11.00000 -1.20000 AFIX 0 C19 1 -0.070959 0.296934 0.392200 11.00000 0.02678 0.02273 = 0.02346 0.00368 -0.00263 -0.00563 C20 1 -0.035568 0.396231 0.392836 11.00000 0.01481 0.01960 = 0.03401 -0.00250 0.00723 0.00211 AFIX 43 H20 2 -0.105604 0.440270 0.397219 11.00000 -1.20000 AFIX 0 C21 1 0.211530 0.557781 0.381220 11.00000 0.01929 0.00369 = 0.02750 0.00337 -0.00321 -0.00194 C22 1 0.244092 0.663002 0.383302 11.00000 0.01603 0.03545 = 0.01694 -0.00693 -0.00173 0.01548 C23 1 0.152066 0.725706 0.393553 11.00000 0.02408 0.03944 = 0.02349 -0.00265 0.00328 -0.00655 AFIX 43 H23 2 0.065953 0.705040 0.399776 11.00000 -1.20000 AFIX 0 C24 1 0.192775 0.820481 0.394222 11.00000 0.01929 0.02686 = 0.03184 -0.00359 0.00422 0.00501 C25 1 0.318829 0.850479 0.385403 11.00000 0.04132 0.00829 = 0.04063 -0.00398 0.00733 -0.00172 AFIX 43 H25 2 0.346468 0.915316 0.385916 11.00000 -1.20000 AFIX 0 C26 1 0.403225 0.780672 0.375722 11.00000 0.03274 0.01780 = 0.03047 -0.00214 0.01063 -0.01167 AFIX 43 H26 2 0.490522 0.798904 0.369505 11.00000 -1.20000 AFIX 0 C27 1 0.445475 0.615500 0.446891 11.00000 0.02265 0.03685 = 0.02238 -0.00860 0.00048 -0.00470 C28 1 0.446719 0.710896 0.441391 11.00000 0.02101 0.01712 = 0.02779 0.00185 0.00313 0.00358 AFIX 43 H28 2 0.408577 0.732001 0.427316 11.00000 -1.20000 AFIX 0 C29 1 0.503310 0.775016 0.456354 11.00000 0.01728 0.03118 = 0.03491 0.00134 0.00658 -0.00219 AFIX 43 H29 2 0.499828 0.841215 0.453157 11.00000 -1.20000 AFIX 0 C30 1 0.567246 0.741621 0.476695 11.00000 0.02712 0.01519 = 0.03267 -0.00313 0.00398 -0.00087 C31 1 0.629573 0.806296 0.492468 11.00000 0.03783 0.02223 = 0.04799 -0.00499 0.00373 -0.01187 AFIX 43 H31 2 0.624455 0.872719 0.489614 11.00000 -1.20000 AFIX 0 C32 1 0.695377 0.774988 0.511284 11.00000 0.03431 0.05534 = 0.03734 -0.00249 -0.00914 -0.03073 AFIX 43 H32 2 0.734300 0.819305 0.521726 11.00000 -1.20000 AFIX 0 C33 1 0.706855 0.675916 0.515591 11.00000 0.03826 0.05320 = 0.03142 0.00472 -0.00825 -0.01105 AFIX 43 H33 2 0.756918 0.654321 0.528575 11.00000 -1.20000 AFIX 0 C34 1 0.646577 0.611325 0.501236 11.00000 0.02315 0.05394 = 0.02561 0.00021 -0.00548 -0.00732 AFIX 43 H34 2 0.653692 0.545168 0.504320 11.00000 -1.20000 AFIX 0 C35 1 0.572571 0.644004 0.481505 11.00000 0.02774 0.02405 = 0.02404 -0.00162 0.00221 -0.00405 C36 1 0.500674 0.578279 0.466531 11.00000 0.01210 0.02268 = 0.01964 -0.00144 0.00119 -0.00280 C37 1 0.492818 0.474187 0.471179 11.00000 0.01646 0.04354 = 0.02200 -0.00227 -0.00397 -0.00083 C38 1 0.431322 0.435197 0.491757 11.00000 0.01928 0.02958 = 0.01951 0.00309 -0.00487 0.00334 C39 1 0.378182 0.491728 0.509603 11.00000 0.02646 0.03892 = 0.01995 0.00579 0.00165 -0.00848 AFIX 43 H39 2 0.382666 0.559037 0.508386 11.00000 -1.20000 AFIX 0 C40 1 0.319973 0.451469 0.528741 11.00000 0.02322 0.04616 = 0.02767 -0.00078 0.00462 0.00156 AFIX 43 H40 2 0.286091 0.491268 0.540607 11.00000 -1.20000 AFIX 0 C41 1 0.310353 0.355889 0.530883 11.00000 0.03223 0.03841 = 0.02998 0.00804 0.00169 0.00540 AFIX 43 H41 2 0.270276 0.329560 0.544290 11.00000 -1.20000 AFIX 0 C42 1 0.357513 0.296303 0.514013 11.00000 0.03368 0.03532 = 0.04038 0.00548 -0.00209 -0.01145 AFIX 43 H42 2 0.349680 0.229336 0.515748 11.00000 -1.20000 AFIX 0 C43 1 0.417869 0.334973 0.494018 11.00000 0.03427 0.02803 = 0.03042 0.00752 0.00022 0.01340 C44 1 0.466347 0.275021 0.476002 11.00000 0.04245 0.02812 = 0.03638 0.00225 0.00189 0.00230 AFIX 43 H44 2 0.462482 0.207904 0.477763 11.00000 -1.20000 AFIX 0 C45 1 0.518251 0.312916 0.456250 11.00000 0.02657 0.02788 = 0.02819 -0.00173 0.00383 0.01210 AFIX 43 H45 2 0.544562 0.272921 0.443914 11.00000 -1.20000 AFIX 0 C46 1 0.531616 0.410413 0.454607 11.00000 0.01840 0.03408 = 0.02298 0.00306 -0.00138 -0.00306 C47 1 0.458414 0.413668 0.280851 11.00000 0.02355 0.03042 = 0.02571 -0.00528 0.00744 0.00750 C48 1 0.597086 0.445390 0.280276 11.00000 0.03505 0.04742 = 0.03207 -0.01120 0.00135 0.00370 AFIX 43 H48 2 0.661303 0.426829 0.291768 11.00000 -1.20000 AFIX 0 C49 1 0.636688 0.502664 0.263061 11.00000 0.03292 0.03976 = 0.05210 -0.01192 0.01340 -0.00409 AFIX 43 H49 2 0.731536 0.521101 0.261968 11.00000 -1.20000 AFIX 0 C50 1 0.540452 0.536500 0.246409 11.00000 0.04777 0.01830 = 0.04031 -0.00082 0.01518 -0.00101 C51 1 0.575811 0.606451 0.229691 11.00000 0.07536 0.02991 = 0.04896 -0.01427 0.03188 -0.02636 AFIX 43 H51 2 0.667094 0.632340 0.229486 11.00000 -1.20000 AFIX 0 C52 1 0.483259 0.635794 0.214464 11.00000 0.07530 0.02763 = 0.04311 0.00418 0.01979 -0.01696 AFIX 43 H52 2 0.512232 0.678186 0.202767 11.00000 -1.20000 AFIX 0 C53 1 0.343402 0.606139 0.215074 11.00000 0.07077 0.02213 = 0.03600 0.00713 0.00751 0.01081 AFIX 43 H53 2 0.277801 0.631559 0.204592 11.00000 -1.20000 AFIX 0 C54 1 0.302739 0.539686 0.231084 11.00000 0.04867 0.03038 = 0.02657 0.00188 0.00358 0.00370 AFIX 43 H54 2 0.208720 0.518944 0.231549 11.00000 -1.20000 AFIX 0 C55 1 0.402070 0.501516 0.247117 11.00000 0.03488 0.01665 = 0.02684 -0.00262 0.00783 0.00494 C56 1 0.361037 0.435896 0.264636 11.00000 0.02763 0.03940 = 0.01869 -0.00544 0.00360 0.00489 C57 1 0.219236 0.398481 0.267117 11.00000 0.02787 0.03100 = 0.02025 0.00071 -0.00446 0.00154 C58 1 0.152063 0.336552 0.250561 11.00000 0.03191 0.02603 = 0.02543 0.00514 -0.00021 0.01056 C59 1 0.219574 0.306811 0.230152 11.00000 0.03484 0.05062 = 0.02191 -0.00882 0.00048 0.00323 AFIX 43 H59 2 0.308487 0.332027 0.226476 11.00000 -1.20000 AFIX 0 C60 1 0.158785 0.242628 0.215748 11.00000 0.04111 0.04945 = 0.03207 -0.00515 0.00298 0.00600 AFIX 43 H60 2 0.205121 0.224462 0.202105 11.00000 -1.20000 AFIX 0 C61 1 0.028592 0.203443 0.220966 11.00000 0.05400 0.05306 = 0.03329 -0.00235 -0.00776 -0.01810 AFIX 43 H61 2 -0.011829 0.157628 0.211063 11.00000 -1.20000 AFIX 0 C62 1 -0.038612 0.230240 0.239761 11.00000 0.04327 0.04005 = 0.03776 -0.00255 -0.01584 -0.01208 AFIX 43 H62 2 -0.126090 0.202095 0.243127 11.00000 -1.20000 AFIX 0 C63 1 0.016435 0.299912 0.255040 11.00000 0.02322 0.03275 = 0.03697 -0.00214 -0.00646 0.00574 C64 1 -0.053736 0.324671 0.275124 11.00000 0.02149 0.03819 = 0.04723 -0.00068 -0.00234 0.00011 AFIX 43 H64 2 -0.145554 0.302219 0.277764 11.00000 -1.20000 AFIX 0 C65 1 0.011163 0.381993 0.291125 11.00000 0.02590 0.04854 = 0.03912 -0.00425 0.00616 -0.00297 AFIX 43 H65 2 -0.035769 0.399939 0.304729 11.00000 -1.20000 AFIX 0 C66 1 0.145644 0.412701 0.286952 11.00000 0.02572 0.02618 = 0.02799 -0.00311 -0.00300 0.01045 C67 1 0.478177 0.691372 0.310380 11.00000 0.02118 0.03394 = 0.02359 -0.00219 0.00371 0.00565 AFIX 43 H67 2 0.451827 0.634716 0.302675 11.00000 -1.20000 AFIX 0 C68 1 0.491201 0.860885 0.311161 11.00000 0.04709 0.02334 = 0.03703 0.00355 0.00286 -0.01060 AFIX 137 H68A 2 0.504667 0.911704 0.299928 11.00000 -1.50000 H68B 2 0.575829 0.853729 0.320329 11.00000 -1.50000 H68C 2 0.412956 0.877073 0.321156 11.00000 -1.50000 AFIX 0 C69 1 0.391232 0.775535 0.277468 11.00000 0.03751 0.04658 = 0.02925 0.00798 -0.00063 0.00231 AFIX 137 H69A 2 0.299335 0.804669 0.279364 11.00000 -1.50000 H69B 2 0.380467 0.710775 0.271539 11.00000 -1.50000 H69C 2 0.446347 0.813357 0.266715 11.00000 -1.50000 AFIX 0 C70 1 0.255812 0.190023 0.420260 11.00000 0.05871 0.08440 = 0.05465 0.02478 -0.01583 -0.02677 AFIX 43 H70 2 0.180247 0.230852 0.423896 11.00000 -1.20000 AFIX 0 C71 1 0.380884 0.050306 0.433269 11.00000 0.09192 0.10834 = 0.09973 -0.01528 0.01260 -0.00955 AFIX 137 H71A 2 0.341892 -0.013539 0.431238 11.00000 -1.50000 H71B 2 0.437598 0.051808 0.447164 11.00000 -1.50000 H71C 2 0.438976 0.066376 0.420075 11.00000 -1.50000 AFIX 0 C72 1 0.174965 0.101102 0.453435 11.00000 0.06617 0.07067 = 0.06559 0.01802 0.01565 0.00354 AFIX 137 H72A 2 0.224464 0.109404 0.467921 11.00000 -1.50000 H72B 2 0.141913 0.035363 0.452206 11.00000 -1.50000 H72C 2 0.095391 0.144616 0.452879 11.00000 -1.50000 AFIX 0 CL1 3 0.792551 0.002605 0.335992 11.00000 0.03816 0.02091 = 0.05021 -0.00442 0.00889 0.00756 CL2 3 0.082239 0.906085 0.405808 11.00000 0.03337 0.02236 = 0.05779 -0.00526 0.01379 0.00502 DY1 4 0.525896 0.562458 0.359168 11.00000 0.02042 0.01776 = 0.01945 -0.00171 0.00233 0.00029 DY2 4 0.300766 0.338776 0.375689 11.00000 0.02265 0.01839 = 0.02144 -0.00088 0.00340 -0.00052 F1 5 1.195673 0.755515 0.326614 11.00000 0.02215 0.02699 = 0.05089 0.00195 0.01210 -0.00529 F2 5 -0.350440 0.151690 0.416511 11.00000 0.02440 0.04051 = 0.04293 -0.00451 0.01351 -0.00906 N1 6 0.741295 0.477978 0.347614 11.00000 0.02260 0.03231 = 0.01375 -0.00178 0.00277 0.00040 N2 6 0.734268 0.376244 0.345126 11.00000 0.03265 0.01661 = 0.02204 -0.00217 0.00390 -0.01074 N3 6 0.476877 0.211063 0.362464 11.00000 0.03043 0.02395 = 0.02570 0.00066 0.00180 -0.00897 N4 6 0.085706 0.428764 0.387800 11.00000 0.02308 0.01052 = 0.02609 0.00158 -0.00576 0.00657 N5 6 0.098394 0.526978 0.390613 11.00000 0.02003 0.02161 = 0.02614 0.00024 -0.00266 -0.00048 N6 6 0.366217 0.689096 0.374837 11.00000 0.02045 0.02041 = 0.02556 -0.00282 0.00563 0.01206 N7 6 0.461816 0.772276 0.299419 11.00000 0.02189 0.02134 = 0.03086 0.00118 0.00014 -0.00801 N8 6 0.265092 0.120979 0.435299 11.00000 0.06473 0.07291 = 0.06086 0.01204 -0.00604 -0.01627 O1 7 0.698524 0.660202 0.366760 11.00000 0.02322 0.02644 = 0.02500 -0.00451 0.00228 -0.00879 O2 7 0.524333 0.394607 0.364625 11.00000 0.01645 0.03613 = 0.02154 0.00269 0.00279 0.00228 O3 7 0.119856 0.245370 0.369156 11.00000 0.01939 0.02366 = 0.03534 -0.00345 0.00883 -0.00467 O4 7 0.301971 0.506875 0.369809 11.00000 0.02797 0.00412 = 0.02842 -0.00520 0.00410 -0.00239 O5 7 0.550253 0.539792 0.398385 11.00000 0.02475 0.03041 = 0.01832 0.00090 -0.00052 -0.00194 O6 7 0.379574 0.404297 0.409150 11.00000 0.02407 0.04059 = 0.01690 0.00171 0.00042 -0.00287 O7 7 0.378674 0.553390 0.431765 11.00000 0.01310 0.02460 = 0.02402 -0.00172 -0.00164 -0.00321 O8 7 0.586616 0.446008 0.434007 11.00000 0.02707 0.03002 = 0.01755 0.00196 -0.00083 0.00260 O9 7 0.424341 0.498883 0.326398 11.00000 0.03280 0.01069 = 0.02369 0.00445 0.00294 -0.00266 O10 7 0.280651 0.349632 0.335717 11.00000 0.03190 0.02527 = 0.02162 -0.00019 -0.00195 -0.00678 O11 7 0.211632 0.466697 0.304269 11.00000 0.02655 0.02519 = 0.02388 -0.00137 0.00165 0.00116 O12 7 0.416408 0.358233 0.299419 11.00000 0.02545 0.01490 = 0.02373 -0.00267 -0.00034 0.00543 O13 7 0.525427 0.683297 0.330034 11.00000 0.03053 0.02090 = 0.02351 0.00422 0.00076 -0.00172 O14 7 0.310780 0.215790 0.404200 11.00000 0.05400 0.02619 = 0.02474 0.00636 0.00819 -0.00849 P1 8 0.472723 0.484593 0.416094 11.00000 0.02606 0.02736 = 0.01671 -0.00246 0.00149 0.00034 P2 8 0.336941 0.419114 0.318872 11.00000 0.02702 0.01582 = 0.02016 -0.00204 -0.00060 -0.00036 C76 1 0.028347 0.439643 0.491340 11.00000 0.06150 0.09844 = 0.05889 -0.02359 0.01165 -0.03835 AFIX 43 H76 2 0.116197 0.416738 0.496337 11.00000 -1.20000 AFIX 0 C77 1 -0.102153 0.493709 0.460508 11.00000 0.22327 0.23082 = 0.21429 0.01197 0.00563 0.01874 AFIX 137 H77A 2 -0.075349 0.542904 0.449505 11.00000 -1.50000 H77B 2 -0.156010 0.522631 0.472899 11.00000 -1.50000 H77C 2 -0.158892 0.445430 0.452833 11.00000 -1.50000 AFIX 0 C78 1 0.117721 0.412631 0.452972 11.00000 0.11749 0.15362 = 0.11821 -0.00153 0.00122 -0.00277 AFIX 137 H78A 2 0.070677 0.365851 0.443267 11.00000 -1.50000 H78B 2 0.195232 0.381992 0.460973 11.00000 -1.50000 H78C 2 0.153351 0.464645 0.443495 11.00000 -1.50000 AFIX 0 N10 6 0.019302 0.450458 0.469621 11.00000 0.05522 0.05976 = 0.05526 -0.00043 0.00606 -0.00009 O16 7 -0.052734 0.452931 0.506418 11.00000 0.12006 0.07185 = 0.07919 0.02689 0.05569 0.03720 C73 1 0.743250 0.824512 0.417801 11.00000 0.04622 0.05505 = 0.05076 0.01337 0.01312 -0.00671 AFIX 43 H73 2 0.687697 0.804147 0.405313 11.00000 -1.20000 AFIX 0 C74 1 0.901902 0.777825 0.448016 11.00000 0.05584 0.05651 = 0.03515 -0.00592 0.00063 -0.01574 AFIX 137 H74A 2 0.905742 0.846687 0.450528 11.00000 -1.50000 H74B 2 0.996210 0.753409 0.445553 11.00000 -1.50000 H74C 2 0.861028 0.746881 0.461420 11.00000 -1.50000 AFIX 0 C75 1 0.801068 0.656967 0.422225 11.00000 0.03894 0.04573 = 0.04665 -0.01106 0.01168 -0.01274 AFIX 137 H75A 2 0.757856 0.622684 0.434947 11.00000 -1.50000 H75B 2 0.892179 0.628967 0.418879 11.00000 -1.50000 H75C 2 0.741454 0.652197 0.408704 11.00000 -1.50000 AFIX 0 N9 6 0.818757 0.758222 0.428485 11.00000 0.02986 0.03928 = 0.04090 -0.00402 0.00738 -0.00362 O15 7 0.739371 0.908645 0.422655 11.00000 0.04620 0.04898 = 0.08254 0.00784 0.02342 0.00126 C79 1 0.181156 0.053344 0.333212 11.00000 0.04761 0.03798 = 0.06367 -0.00446 0.00398 -0.01987 AFIX 43 H79 2 0.191393 0.111042 0.341482 11.00000 -1.20000 AFIX 0 C80 1 0.074663 0.148810 0.304162 11.00000 0.05937 0.04676 = 0.10984 0.02784 0.02361 0.02679 AFIX 137 H80A 2 -0.026517 0.145706 0.302244 11.00000 -1.50000 H80B 2 0.118389 0.162596 0.289419 11.00000 -1.50000 H80C 2 0.097920 0.199242 0.315060 11.00000 -1.50000 AFIX 0 C81 1 0.100786 -0.026036 0.298759 11.00000 0.05978 0.05617 = 0.06040 0.01693 0.01557 0.01114 AFIX 137 H81A 2 0.142321 -0.080941 0.306489 11.00000 -1.50000 H81B 2 0.143850 -0.018084 0.283718 11.00000 -1.50000 H81C 2 0.000601 -0.036456 0.296922 11.00000 -1.50000 AFIX 0 N11 6 0.124221 0.060239 0.312516 11.00000 0.03811 0.03707 = 0.06368 0.00549 0.01185 -0.00290 O17 7 0.220871 -0.017545 0.342550 11.00000 0.06191 0.03865 = 0.06575 -0.00077 -0.00283 -0.00067 HKLF 4 REM exp_239_auto_a.res in P2(1)2(1)2(1) REM wR2 = 0.1359, GooF = S = 1.198, Restrained GooF = 1.201 for all data REM R1 = 0.0590 for 12654 Fo > 4sig(Fo) and 0.0609 for all 13089 data REM 1065 parameters refined using 60 restraints END WGHT 0.0000 79.9421 REM Highest difference peak 1.780, deepest hole -1.251, 1-sigma level 0.134 Q1 1 0.2995 0.3416 0.3920 11.00000 0.05 1.78 Q2 1 0.5239 0.5637 0.3429 11.00000 0.05 1.76 Q3 1 0.2967 0.3407 0.3591 11.00000 0.05 1.65 Q4 1 0.5212 0.5618 0.3754 11.00000 0.05 1.52 Q5 1 0.2023 0.1749 0.4384 11.00000 0.05 1.16 ; _shelx_res_checksum 22504 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 2.089 _oxdiff_exptl_absorpt_empirical_full_min 0.723 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8185(13) 0.6829(9) 0.3567(2) 0.027(3) Uani 1 1 d D . . . . C2 C 0.8659(15) 0.7817(9) 0.3568(2) 0.031(3) Uani 1 1 d D U . . . H2 H 0.811714 0.830880 0.363445 0.037 Uiso 1 1 calc R U . . . C3 C 0.9919(16) 0.8000(11) 0.3468(2) 0.033(3) Uani 1 1 d . . . . . H3 H 1.026679 0.863290 0.347098 0.039 Uiso 1 1 calc R U . . . C4 C 1.0703(14) 0.7303(10) 0.3365(2) 0.027(3) Uani 1 1 d . . . . . C5 C 1.0306(14) 0.6371(9) 0.3360(2) 0.024(3) Uani 1 1 d . . . . . H5 H 1.089266 0.590009 0.329471 0.029 Uiso 1 1 calc R U . . . C6 C 0.9027(13) 0.6127(9) 0.3453(2) 0.019(3) Uani 1 1 d . . . . . C7 C 0.8634(14) 0.5130(9) 0.3442(2) 0.019(3) Uani 1 1 d . . . . . H7 H 0.935205 0.469068 0.340579 0.023 Uiso 1 1 calc R U . . . C8 C 0.6183(14) 0.3462(11) 0.35428(19) 0.027(3) Uani 1 1 d . . . . . C9 C 0.6000(14) 0.2410(9) 0.3535(2) 0.020(3) Uani 1 1 d . . . . . C10 C 0.6982(15) 0.1794(9) 0.3451(2) 0.023(3) Uani 1 1 d . U . . . H10 H 0.784192 0.201591 0.339138 0.027 Uiso 1 1 calc R U . . . C11 C 0.6670(15) 0.0854(9) 0.3457(2) 0.027(3) Uani 1 1 d . . . . . C12 C 0.5466(15) 0.0501(10) 0.3548(2) 0.031(3) Uani 1 1 d . . . . . H12 H 0.527940 -0.016206 0.355631 0.037 Uiso 1 1 calc R U . . . C13 C 0.4519(16) 0.1192(10) 0.3628(2) 0.033(3) Uani 1 1 d . . . . . H13 H 0.365197 0.098173 0.368671 0.040 Uiso 1 1 calc R U . . . C14 C 0.0104(14) 0.2237(9) 0.3811(2) 0.026(3) Uani 1 1 d . . . . . C15 C -0.0346(14) 0.1318(9) 0.3835(2) 0.025(3) Uani 1 1 d . . . . . H15 H 0.018456 0.082994 0.376446 0.030 Uiso 1 1 calc R U . . . C16 C -0.1508(14) 0.1054(10) 0.3955(2) 0.027(3) Uani 1 1 d . . . . . H16 H -0.176354 0.040480 0.397092 0.032 Uiso 1 1 calc R U . . . C17 C -0.2291(14) 0.1774(10) 0.4051(2) 0.025(3) Uani 1 1 d . . . . . C18 C -0.1946(15) 0.2680(9) 0.4036(2) 0.024(3) Uani 1 1 d . . . . . H18 H -0.253118 0.314724 0.410339 0.029 Uiso 1 1 calc R U . . . C19 C -0.0710(14) 0.2969(10) 0.3922(2) 0.024(3) Uani 1 1 d . . . . . C20 C -0.0356(14) 0.3962(9) 0.3928(2) 0.023(3) Uani 1 1 d . . . . . H20 H -0.105604 0.440270 0.397219 0.027 Uiso 1 1 calc R U . . . C21 C 0.2115(13) 0.5578(8) 0.38122(19) 0.017(2) Uani 1 1 d . U . . . C22 C 0.2441(13) 0.6630(11) 0.38330(19) 0.023(3) Uani 1 1 d . . . . . C23 C 0.1521(15) 0.7257(11) 0.3936(2) 0.029(3) Uani 1 1 d . . . . . H23 H 0.065953 0.705040 0.399776 0.035 Uiso 1 1 calc R U . . . C24 C 0.1928(15) 0.8205(9) 0.3942(2) 0.026(3) Uani 1 1 d . . . . . C25 C 0.3188(16) 0.8505(9) 0.3854(2) 0.030(3) Uani 1 1 d . . . . . H25 H 0.346468 0.915316 0.385916 0.036 Uiso 1 1 calc R U . . . C26 C 0.4032(15) 0.7807(9) 0.3757(2) 0.027(3) Uani 1 1 d . . . . . H26 H 0.490522 0.798904 0.369505 0.032 Uiso 1 1 calc R U . . . C27 C 0.4455(14) 0.6155(10) 0.4469(2) 0.027(3) Uani 1 1 d . . . . . C28 C 0.4467(13) 0.7109(9) 0.4414(2) 0.022(3) Uani 1 1 d . . . . . H28 H 0.408577 0.732001 0.427316 0.026 Uiso 1 1 calc R U . . . C29 C 0.5033(13) 0.7750(10) 0.4564(2) 0.028(3) Uani 1 1 d . . . . . H29 H 0.499828 0.841215 0.453157 0.033 Uiso 1 1 calc R U . . . C30 C 0.5672(14) 0.7416(9) 0.4767(2) 0.025(3) Uani 1 1 d . . . . . C31 C 0.6296(17) 0.8063(11) 0.4925(3) 0.036(4) Uani 1 1 d . . . . . H31 H 0.624455 0.872719 0.489614 0.043 Uiso 1 1 calc R U . . . C32 C 0.6954(18) 0.7750(12) 0.5113(3) 0.042(4) Uani 1 1 d . . . . . H32 H 0.734300 0.819305 0.521726 0.051 Uiso 1 1 calc R U . . . C33 C 0.7069(18) 0.6759(12) 0.5156(3) 0.041(4) Uani 1 1 d . . . . . H33 H 0.756918 0.654321 0.528575 0.049 Uiso 1 1 calc R U . . . C34 C 0.6466(15) 0.6113(12) 0.5012(2) 0.034(3) Uani 1 1 d . . . . . H34 H 0.653692 0.545168 0.504320 0.041 Uiso 1 1 calc R U . . . C35 C 0.5726(14) 0.6440(10) 0.4815(2) 0.025(3) Uani 1 1 d . . . . . C36 C 0.5007(12) 0.5783(9) 0.46653(19) 0.018(3) Uani 1 1 d . . . . . C37 C 0.4928(14) 0.4742(11) 0.4712(2) 0.027(3) Uani 1 1 d . . . . . C38 C 0.4313(13) 0.4352(10) 0.4918(2) 0.023(3) Uani 1 1 d . . . . . C39 C 0.3782(14) 0.4917(11) 0.5096(2) 0.028(3) Uani 1 1 d . . . . . H39 H 0.382666 0.559037 0.508386 0.034 Uiso 1 1 calc R U . . . C40 C 0.3200(15) 0.4515(11) 0.5287(2) 0.032(3) Uani 1 1 d . . . . . H40 H 0.286091 0.491268 0.540607 0.039 Uiso 1 1 calc R U . . . C41 C 0.3104(16) 0.3559(11) 0.5309(2) 0.034(3) Uani 1 1 d . . . . . H41 H 0.270276 0.329560 0.544290 0.040 Uiso 1 1 calc R U . . . C42 C 0.3575(16) 0.2963(12) 0.5140(3) 0.036(4) Uani 1 1 d . . . . . H42 H 0.349680 0.229336 0.515748 0.044 Uiso 1 1 calc R U . . . C43 C 0.4179(15) 0.3350(11) 0.4940(2) 0.031(3) Uani 1 1 d . . . . . C44 C 0.4663(18) 0.2750(11) 0.4760(2) 0.036(3) Uani 1 1 d . . . . . H44 H 0.462482 0.207904 0.477763 0.043 Uiso 1 1 calc R U . . . C45 C 0.5183(15) 0.3129(10) 0.4562(2) 0.028(3) Uani 1 1 d . . . . . H45 H 0.544562 0.272921 0.443914 0.033 Uiso 1 1 calc R U . . . C46 C 0.5316(14) 0.4104(10) 0.4546(2) 0.025(3) Uani 1 1 d . . . . . C47 C 0.4584(14) 0.4137(10) 0.2809(2) 0.027(3) Uani 1 1 d . . . . . C48 C 0.5971(16) 0.4454(12) 0.2803(2) 0.038(4) Uani 1 1 d . . . . . H48 H 0.661303 0.426829 0.291768 0.046 Uiso 1 1 calc R U . . . C49 C 0.6367(18) 0.5027(12) 0.2631(3) 0.042(4) Uani 1 1 d . . . . . H49 H 0.731536 0.521101 0.261968 0.050 Uiso 1 1 calc R U . . . C50 C 0.5405(18) 0.5365(10) 0.2464(3) 0.035(4) Uani 1 1 d . . . . . C51 C 0.576(2) 0.6065(12) 0.2297(3) 0.051(5) Uani 1 1 d . . . . . H51 H 0.667094 0.632340 0.229486 0.062 Uiso 1 1 calc R U . . . C52 C 0.483(2) 0.6358(11) 0.2145(3) 0.049(5) Uani 1 1 d . . . . . H52 H 0.512232 0.678186 0.202767 0.058 Uiso 1 1 calc R U . . . C53 C 0.343(2) 0.6061(11) 0.2151(3) 0.043(4) Uani 1 1 d . . . . . H53 H 0.277801 0.631559 0.204592 0.052 Uiso 1 1 calc R U . . . C54 C 0.3027(19) 0.5397(10) 0.2311(2) 0.035(3) Uani 1 1 d . . . . . H54 H 0.208720 0.518944 0.231549 0.042 Uiso 1 1 calc R U . . . C55 C 0.4021(15) 0.5015(9) 0.2471(2) 0.026(3) Uani 1 1 d . . . . . C56 C 0.3610(14) 0.4359(12) 0.2646(2) 0.029(3) Uani 1 1 d . . . . . C57 C 0.2192(15) 0.3985(10) 0.2671(2) 0.026(3) Uani 1 1 d . . . . . C58 C 0.1521(15) 0.3366(10) 0.2506(2) 0.028(3) Uani 1 1 d . . . . . C59 C 0.2196(17) 0.3068(11) 0.2302(2) 0.036(4) Uani 1 1 d . . . . . H59 H 0.308487 0.332027 0.226476 0.043 Uiso 1 1 calc R U . . . C60 C 0.1588(17) 0.2426(12) 0.2157(3) 0.041(4) Uani 1 1 d . . . . . H60 H 0.205121 0.224462 0.202105 0.049 Uiso 1 1 calc R U . . . C61 C 0.029(2) 0.2034(13) 0.2210(3) 0.047(4) Uani 1 1 d . . . . . H61 H -0.011829 0.157628 0.211063 0.056 Uiso 1 1 calc R U . . . C62 C -0.0386(19) 0.2302(11) 0.2398(3) 0.040(4) Uani 1 1 d . . . . . H62 H -0.126090 0.202095 0.243127 0.048 Uiso 1 1 calc R U . . . C63 C 0.0164(15) 0.2999(10) 0.2550(2) 0.031(3) Uani 1 1 d . . . . . C64 C -0.0537(15) 0.3247(11) 0.2751(3) 0.036(3) Uani 1 1 d . . . . . H64 H -0.145554 0.302219 0.277764 0.043 Uiso 1 1 calc R U . . . C65 C 0.0112(16) 0.3820(12) 0.2911(3) 0.038(4) Uani 1 1 d . . . . . H65 H -0.035769 0.399939 0.304729 0.045 Uiso 1 1 calc R U . . . C66 C 0.1456(15) 0.4127(10) 0.2870(2) 0.027(3) Uani 1 1 d . . . . . C67 C 0.4782(14) 0.6914(10) 0.3104(2) 0.026(3) Uani 1 1 d . . . . . H67 H 0.451827 0.634716 0.302675 0.031 Uiso 1 1 calc R U . . . C68 C 0.4912(17) 0.8609(10) 0.3112(2) 0.036(4) Uani 1 1 d . . . . . H68A H 0.504667 0.911704 0.299928 0.054 Uiso 1 1 calc R U . . . H68B H 0.575829 0.853729 0.320329 0.054 Uiso 1 1 calc R U . . . H68C H 0.412956 0.877073 0.321156 0.054 Uiso 1 1 calc R U . . . C69 C 0.3912(17) 0.7755(12) 0.2775(2) 0.038(4) Uani 1 1 d . . . . . H69A H 0.299335 0.804669 0.279364 0.057 Uiso 1 1 calc R U . . . H69B H 0.380467 0.710775 0.271539 0.057 Uiso 1 1 calc R U . . . H69C H 0.446347 0.813357 0.266715 0.057 Uiso 1 1 calc R U . . . C70 C 0.256(2) 0.1900(15) 0.4203(3) 0.066(6) Uani 1 1 d D U . . . H70 H 0.180247 0.230852 0.423896 0.079 Uiso 1 1 calc R U . . . C71 C 0.381(3) 0.050(2) 0.4333(5) 0.100(9) Uani 1 1 d D U . . . H71A H 0.341892 -0.013539 0.431238 0.150 Uiso 1 1 calc R U . . . H71B H 0.437598 0.051808 0.447164 0.150 Uiso 1 1 calc R U . . . H71C H 0.438976 0.066376 0.420075 0.150 Uiso 1 1 calc R U . . . C72 C 0.175(2) 0.1011(16) 0.4534(3) 0.067(6) Uani 1 1 d . U . . . H72A H 0.224464 0.109404 0.467921 0.101 Uiso 1 1 calc R U . . . H72B H 0.141913 0.035363 0.452206 0.101 Uiso 1 1 calc R U . . . H72C H 0.095391 0.144616 0.452879 0.101 Uiso 1 1 calc R U . . . Cl1 Cl 0.7926(4) 0.0026(2) 0.33599(6) 0.0364(8) Uani 1 1 d . . . . . Cl2 Cl 0.0822(4) 0.9061(2) 0.40581(7) 0.0378(9) Uani 1 1 d . . . . . Dy1 Dy 0.52590(8) 0.56246(5) 0.35917(2) 0.01921(17) Uani 1 1 d . . . . . Dy2 Dy 0.30077(8) 0.33878(5) 0.37569(2) 0.02083(18) Uani 1 1 d . . . . . F1 F 1.1957(9) 0.7555(5) 0.32661(14) 0.0333(18) Uani 1 1 d . . . . . F2 F -0.3504(8) 0.1517(6) 0.41651(14) 0.0359(19) Uani 1 1 d . . . . . N1 N 0.7413(11) 0.4780(8) 0.34761(17) 0.023(2) Uani 1 1 d . . . . . N2 N 0.7343(12) 0.3762(8) 0.34513(18) 0.024(2) Uani 1 1 d . . . . . N3 N 0.4769(13) 0.2111(8) 0.36246(18) 0.027(2) Uani 1 1 d . . . . . N4 N 0.0857(11) 0.4288(7) 0.38780(17) 0.020(2) Uani 1 1 d . . . . . N5 N 0.0984(11) 0.5270(8) 0.39061(18) 0.023(2) Uani 1 1 d . . . . . N6 N 0.3662(11) 0.6891(7) 0.37484(18) 0.022(2) Uani 1 1 d . . . . . N7 N 0.4618(12) 0.7723(8) 0.29942(18) 0.025(2) Uani 1 1 d . . . . . N8 N 0.2651(18) 0.1210(12) 0.4353(3) 0.066(5) Uani 1 1 d D U . . . O1 O 0.6985(10) 0.6602(7) 0.36676(13) 0.0249(19) Uani 1 1 d . . . . . O2 O 0.5243(9) 0.3946(7) 0.36463(14) 0.025(2) Uani 1 1 d . . . . . O3 O 0.1199(9) 0.2454(7) 0.36916(16) 0.026(2) Uani 1 1 d . . . . . O4 O 0.3020(10) 0.5069(5) 0.36981(14) 0.0202(18) Uani 1 1 d . U . . . O5 O 0.5503(9) 0.5398(6) 0.39838(14) 0.024(2) Uani 1 1 d . . . . . O6 O 0.3796(10) 0.4043(7) 0.40915(14) 0.027(2) Uani 1 1 d . . . . . O7 O 0.3787(8) 0.5534(6) 0.43177(14) 0.0206(18) Uani 1 1 d . . . . . O8 O 0.5866(10) 0.4460(7) 0.43401(14) 0.025(2) Uani 1 1 d . . . . . O9 O 0.4243(10) 0.4989(6) 0.32640(14) 0.022(2) Uani 1 1 d . . . . . O10 O 0.2807(10) 0.3496(7) 0.33572(14) 0.026(2) Uani 1 1 d . . . . . O11 O 0.2116(10) 0.4667(6) 0.30427(14) 0.025(2) Uani 1 1 d . . . . . O12 O 0.4164(9) 0.3582(6) 0.29942(14) 0.0214(19) Uani 1 1 d . . . . . O13 O 0.5254(10) 0.6833(6) 0.33003(14) 0.025(2) Uani 1 1 d . . . . . O14 O 0.3108(12) 0.2158(7) 0.40420(15) 0.035(2) Uani 1 1 d . U . . . P1 P 0.4727(4) 0.4846(2) 0.41609(5) 0.0234(7) Uani 1 1 d . . . . . P2 P 0.3369(4) 0.4191(2) 0.31887(5) 0.0210(7) Uani 1 1 d . . . . . C76 C 0.028(2) 0.4396(18) 0.4913(3) 0.073(6) Uani 1 1 d . . . . . H76 H 0.116197 0.416738 0.496337 0.088 Uiso 1 1 calc R U . . . C77 C -0.102(4) 0.494(4) 0.4605(8) 0.22(2) Uani 1 1 d D U . . . H77A H -0.075349 0.542904 0.449505 0.334 Uiso 1 1 calc R U . . . H77B H -0.156010 0.522631 0.472899 0.334 Uiso 1 1 calc R U . . . H77C H -0.158892 0.445430 0.452833 0.334 Uiso 1 1 calc R U . . . C78 C 0.118(3) 0.413(3) 0.4530(5) 0.130(12) Uani 1 1 d D U . . . H78A H 0.070677 0.365851 0.443267 0.195 Uiso 1 1 calc R U . . . H78B H 0.195232 0.381992 0.460973 0.195 Uiso 1 1 calc R U . . . H78C H 0.153351 0.464645 0.443495 0.195 Uiso 1 1 calc R U . . . N10 N 0.0193(18) 0.4505(12) 0.4696(3) 0.057(4) Uani 1 1 d D U . . . O16 O -0.0527(19) 0.4529(11) 0.5064(3) 0.090(6) Uani 1 1 d . . . . . C73 C 0.7432(19) 0.8245(14) 0.4178(3) 0.051(5) Uani 1 1 d . . . . . H73 H 0.687697 0.804147 0.405313 0.061 Uiso 1 1 calc R U . . . C74 C 0.902(2) 0.7778(14) 0.4480(3) 0.049(5) Uani 1 1 d . . . . . H74A H 0.905742 0.846687 0.450528 0.074 Uiso 1 1 calc R U . . . H74B H 0.996210 0.753409 0.445553 0.074 Uiso 1 1 calc R U . . . H74C H 0.861028 0.746881 0.461420 0.074 Uiso 1 1 calc R U . . . C75 C 0.8011(19) 0.6570(12) 0.4222(3) 0.044(4) Uani 1 1 d . . . . . H75A H 0.757856 0.622684 0.434947 0.066 Uiso 1 1 calc R U . . . H75B H 0.892179 0.628967 0.418879 0.066 Uiso 1 1 calc R U . . . H75C H 0.741454 0.652197 0.408704 0.066 Uiso 1 1 calc R U . . . N9 N 0.8188(14) 0.7582(9) 0.4285(2) 0.037(3) Uani 1 1 d . . . . . O15 O 0.7394(13) 0.9086(9) 0.4227(2) 0.059(4) Uani 1 1 d . . . . . C79 C 0.1812(19) 0.0533(13) 0.3332(3) 0.050(4) Uani 1 1 d . . . . . H79 H 0.191393 0.111042 0.341482 0.060 Uiso 1 1 calc R U . . . C80 C 0.075(2) 0.1488(14) 0.3042(4) 0.072(7) Uani 1 1 d . . . . . H80A H -0.026517 0.145706 0.302244 0.108 Uiso 1 1 calc R U . . . H80B H 0.118389 0.162596 0.289419 0.108 Uiso 1 1 calc R U . . . H80C H 0.097920 0.199242 0.315060 0.108 Uiso 1 1 calc R U . . . C81 C 0.101(2) -0.0260(14) 0.2988(3) 0.059(5) Uani 1 1 d . . . . . H81A H 0.142321 -0.080941 0.306489 0.088 Uiso 1 1 calc R U . . . H81B H 0.143850 -0.018084 0.283718 0.088 Uiso 1 1 calc R U . . . H81C H 0.000601 -0.036456 0.296922 0.088 Uiso 1 1 calc R U . . . N11 N 0.1242(14) 0.0602(11) 0.3125(2) 0.046(3) Uani 1 1 d . . . . . O17 O 0.2209(14) -0.0175(9) 0.3425(2) 0.055(3) Uani 1 1 d . . . . . 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 0.019(7) 0.043(8) 0.019(6) -0.003(6) 0.000(5) 0.021(6) C2 0.036(5) 0.026(5) 0.030(5) 0.002(4) 0.001(4) 0.008(4) C3 0.037(9) 0.031(8) 0.030(7) -0.006(6) -0.001(6) -0.002(7) C4 0.020(7) 0.032(8) 0.030(7) -0.004(6) 0.005(5) 0.003(6) C5 0.017(6) 0.031(8) 0.024(6) 0.001(5) 0.000(5) 0.005(6) C6 0.008(6) 0.022(7) 0.026(7) -0.003(5) 0.000(5) 0.005(5) C7 0.026(7) 0.017(6) 0.015(6) 0.003(5) 0.001(5) 0.008(5) C8 0.029(7) 0.045(8) 0.008(6) -0.006(6) 0.003(5) 0.016(7) C9 0.028(7) 0.011(6) 0.021(6) 0.003(5) 0.003(5) -0.002(5) C10 0.026(5) 0.018(5) 0.024(4) 0.000(4) 0.001(4) 0.005(4) C11 0.032(8) 0.020(7) 0.029(7) 0.000(5) 0.008(6) -0.004(6) C12 0.032(8) 0.017(7) 0.044(8) -0.004(6) 0.006(6) -0.002(6) C13 0.027(8) 0.032(8) 0.040(8) -0.007(6) 0.005(7) -0.005(6) C14 0.024(7) 0.026(7) 0.027(7) -0.005(5) 0.000(5) 0.003(6) C15 0.016(6) 0.016(6) 0.042(8) -0.002(5) 0.005(6) 0.001(5) C16 0.018(7) 0.016(7) 0.045(8) -0.004(6) -0.003(6) 0.001(5) C17 0.025(8) 0.030(8) 0.021(6) 0.002(5) 0.005(5) -0.006(6) C18 0.024(7) 0.023(7) 0.026(7) -0.001(5) 0.009(6) 0.004(6) C19 0.027(7) 0.023(7) 0.023(7) 0.004(5) -0.003(5) -0.006(6) C20 0.015(6) 0.020(6) 0.034(7) -0.003(5) 0.007(6) 0.002(5) C21 0.019(6) 0.004(5) 0.027(6) 0.003(4) -0.003(5) -0.002(5) C22 0.016(6) 0.035(7) 0.017(6) -0.007(6) -0.002(5) 0.015(6) C23 0.024(8) 0.039(9) 0.023(7) -0.003(6) 0.003(5) -0.007(6) C24 0.019(7) 0.027(8) 0.032(7) -0.004(5) 0.004(6) 0.005(6) C25 0.041(9) 0.008(6) 0.041(8) -0.004(5) 0.007(6) -0.002(6) C26 0.033(8) 0.018(7) 0.030(7) -0.002(6) 0.011(6) -0.012(6) C27 0.023(8) 0.037(8) 0.022(7) -0.009(6) 0.000(5) -0.005(6) C28 0.021(7) 0.017(6) 0.028(7) 0.002(5) 0.003(5) 0.004(5) C29 0.017(7) 0.031(8) 0.035(7) 0.001(6) 0.007(5) -0.002(6) C30 0.027(8) 0.015(6) 0.033(7) -0.003(5) 0.004(6) -0.001(5) C31 0.038(9) 0.022(7) 0.048(9) -0.005(6) 0.004(7) -0.012(7) C32 0.034(9) 0.055(10) 0.037(8) -0.002(7) -0.009(7) -0.031(8) C33 0.038(9) 0.053(10) 0.031(8) 0.005(7) -0.008(7) -0.011(8) C34 0.023(8) 0.054(10) 0.026(7) 0.000(7) -0.005(6) -0.007(7) C35 0.028(8) 0.024(7) 0.024(7) -0.002(5) 0.002(5) -0.004(6) C36 0.012(6) 0.023(7) 0.020(6) -0.001(5) 0.001(4) -0.003(5) C37 0.016(7) 0.044(8) 0.022(6) -0.002(6) -0.004(5) -0.001(6) C38 0.019(7) 0.030(7) 0.020(6) 0.003(5) -0.005(5) 0.003(6) C39 0.026(8) 0.039(8) 0.020(6) 0.006(6) 0.002(5) -0.008(6) C40 0.023(7) 0.046(9) 0.028(7) -0.001(6) 0.005(6) 0.002(7) C41 0.032(8) 0.038(9) 0.030(7) 0.008(6) 0.002(6) 0.005(7) C42 0.034(9) 0.035(8) 0.040(8) 0.005(7) -0.002(7) -0.011(7) C43 0.034(8) 0.028(7) 0.030(7) 0.008(6) 0.000(6) 0.013(7) C44 0.042(9) 0.028(8) 0.036(8) 0.002(6) 0.002(7) 0.002(7) C45 0.027(7) 0.028(7) 0.028(7) -0.002(5) 0.004(6) 0.012(6) C46 0.018(6) 0.034(8) 0.023(6) 0.003(5) -0.001(5) -0.003(6) C47 0.024(7) 0.030(8) 0.026(7) -0.005(5) 0.007(6) 0.007(6) C48 0.035(9) 0.047(10) 0.032(8) -0.011(7) 0.001(6) 0.004(8) C49 0.033(9) 0.040(10) 0.052(10) -0.012(8) 0.013(8) -0.004(7) C50 0.048(10) 0.018(7) 0.040(8) -0.001(6) 0.015(7) -0.001(7) C51 0.075(14) 0.030(9) 0.049(10) -0.014(8) 0.032(10) -0.026(9) C52 0.075(14) 0.028(8) 0.043(9) 0.004(7) 0.020(9) -0.017(9) C53 0.071(13) 0.022(8) 0.036(8) 0.007(6) 0.008(8) 0.011(8) C54 0.049(9) 0.030(8) 0.027(7) 0.002(6) 0.004(7) 0.004(7) C55 0.035(8) 0.017(7) 0.027(7) -0.003(5) 0.008(6) 0.005(6) C56 0.028(7) 0.039(8) 0.019(6) -0.005(6) 0.004(5) 0.005(7) C57 0.028(8) 0.031(7) 0.020(6) 0.001(5) -0.004(6) 0.002(6) C58 0.032(8) 0.026(7) 0.025(7) 0.005(6) 0.000(5) 0.011(6) C59 0.035(9) 0.051(10) 0.022(7) -0.009(6) 0.000(6) 0.003(7) C60 0.041(10) 0.049(10) 0.032(8) -0.005(7) 0.003(7) 0.006(8) C61 0.054(11) 0.053(10) 0.033(8) -0.002(7) -0.008(8) -0.018(9) C62 0.043(10) 0.040(9) 0.038(8) -0.003(7) -0.016(8) -0.012(8) C63 0.023(8) 0.033(8) 0.037(8) -0.002(6) -0.006(6) 0.006(6) C64 0.021(8) 0.038(9) 0.047(9) -0.001(7) -0.002(6) 0.000(6) C65 0.026(8) 0.049(9) 0.039(8) -0.004(7) 0.006(7) -0.003(7) C66 0.026(7) 0.026(7) 0.028(7) -0.003(5) -0.003(6) 0.010(6) C67 0.021(7) 0.034(8) 0.024(7) -0.002(5) 0.004(6) 0.006(6) C68 0.047(10) 0.023(7) 0.037(8) 0.004(6) 0.003(7) -0.011(7) C69 0.038(9) 0.047(10) 0.029(8) 0.008(7) -0.001(7) 0.002(7) C70 0.059(13) 0.084(16) 0.055(11) 0.025(11) -0.016(9) -0.027(11) C71 0.092(13) 0.108(14) 0.100(13) -0.015(11) 0.013(11) -0.010(11) C72 0.066(11) 0.071(10) 0.066(10) 0.018(8) 0.016(9) 0.004(9) Cl1 0.038(2) 0.0209(16) 0.050(2) -0.0044(14) 0.0089(17) 0.0076(16) Cl2 0.0334(19) 0.0224(17) 0.058(2) -0.0053(15) 0.0138(17) 0.0050(14) Dy1 0.0204(4) 0.0178(4) 0.0195(3) -0.0017(3) 0.0023(3) 0.0003(3) Dy2 0.0227(4) 0.0184(4) 0.0214(4) -0.0009(3) 0.0034(3) -0.0005(3) F1 0.022(4) 0.027(4) 0.051(5) 0.002(3) 0.012(4) -0.005(4) F2 0.024(4) 0.041(5) 0.043(5) -0.005(4) 0.014(3) -0.009(4) N1 0.023(6) 0.032(6) 0.014(5) -0.002(4) 0.003(4) 0.000(5) N2 0.033(7) 0.017(5) 0.022(5) -0.002(4) 0.004(5) -0.011(5) N3 0.030(6) 0.024(6) 0.026(6) 0.001(4) 0.002(5) -0.009(5) N4 0.023(6) 0.011(5) 0.026(5) 0.002(4) -0.006(4) 0.007(5) N5 0.020(6) 0.022(6) 0.026(6) 0.000(4) -0.003(5) 0.000(5) N6 0.020(6) 0.020(6) 0.026(5) -0.003(5) 0.006(5) 0.012(4) N7 0.022(6) 0.021(6) 0.031(6) 0.001(5) 0.000(5) -0.008(5) N8 0.065(7) 0.073(7) 0.061(7) 0.012(6) -0.006(5) -0.016(6) O1 0.023(5) 0.026(5) 0.025(4) -0.005(4) 0.002(4) -0.009(4) O2 0.016(4) 0.036(5) 0.022(4) 0.003(4) 0.003(4) 0.002(4) O3 0.019(5) 0.024(5) 0.035(5) -0.003(4) 0.009(4) -0.005(4) O4 0.028(5) 0.004(4) 0.028(4) -0.005(3) 0.004(4) -0.002(4) O5 0.025(5) 0.030(5) 0.018(4) 0.001(4) -0.001(4) -0.002(4) O6 0.024(5) 0.041(6) 0.017(4) 0.002(4) 0.000(4) -0.003(4) O7 0.013(4) 0.025(5) 0.024(4) -0.002(4) -0.002(3) -0.003(4) O8 0.027(5) 0.030(5) 0.018(4) 0.002(4) -0.001(4) 0.003(4) O9 0.033(5) 0.011(4) 0.024(4) 0.004(3) 0.003(4) -0.003(4) O10 0.032(5) 0.025(5) 0.022(4) 0.000(4) -0.002(4) -0.007(4) O11 0.027(5) 0.025(5) 0.024(4) -0.001(4) 0.002(4) 0.001(4) O12 0.025(5) 0.015(5) 0.024(4) -0.003(3) 0.000(4) 0.005(4) O13 0.031(5) 0.021(5) 0.024(5) 0.004(3) 0.001(4) -0.002(4) O14 0.054(7) 0.026(5) 0.025(5) 0.006(4) 0.008(5) -0.008(5) P1 0.0261(17) 0.0274(17) 0.0167(15) -0.0025(12) 0.0015(14) 0.0003(15) P2 0.0270(18) 0.0158(16) 0.0202(15) -0.0020(12) -0.0006(13) -0.0004(13) C76 0.061(13) 0.098(17) 0.059(12) -0.024(12) 0.012(11) -0.038(14) C77 0.22(3) 0.23(3) 0.21(3) 0.012(14) 0.006(14) 0.019(14) C78 0.117(16) 0.154(17) 0.118(15) -0.002(12) 0.001(12) -0.003(13) N10 0.055(6) 0.060(6) 0.055(6) 0.000(5) 0.006(5) 0.000(6) O16 0.120(15) 0.072(10) 0.079(10) 0.027(8) 0.056(10) 0.037(10) C73 0.046(11) 0.055(13) 0.051(10) 0.013(9) 0.013(8) -0.007(9) C74 0.056(12) 0.057(12) 0.035(9) -0.006(8) 0.001(8) -0.016(9) C75 0.039(9) 0.046(9) 0.047(9) -0.011(8) 0.012(8) -0.013(9) N9 0.030(7) 0.039(7) 0.041(7) -0.004(6) 0.007(6) -0.004(6) O15 0.046(8) 0.049(8) 0.083(9) 0.008(7) 0.023(7) 0.001(6) C79 0.048(11) 0.038(10) 0.064(11) -0.004(9) 0.004(9) -0.020(9) C80 0.059(13) 0.047(12) 0.110(17) 0.028(12) 0.024(12) 0.027(10) C81 0.060(13) 0.056(12) 0.060(12) 0.017(10) 0.016(10) 0.011(10) N11 0.038(8) 0.037(8) 0.064(9) 0.005(7) 0.012(7) -0.003(7) O17 0.062(9) 0.039(7) 0.066(8) -0.001(6) -0.003(7) -0.001(6) 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' Cl Cl 0.3639 0.7018 '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' F F 0.0727 0.0534 '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' P P 0.2955 0.4335 '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 C6 C1 C2 118.5(12) . . ? O1 C1 C2 119.7(11) . . ? O1 C1 C6 121.8(12) . . ? C1 C2 H2 121.5 . . ? C3 C2 C1 117.0(13) . . ? C3 C2 H2 121.5 . . ? C2 C3 H3 118.8 . . ? C2 C3 C4 122.5(14) . . ? C4 C3 H3 118.8 . . ? C3 C4 F1 118.6(13) . . ? C5 C4 C3 122.7(13) . . ? C5 C4 F1 118.8(12) . . ? C4 C5 H5 120.8 . . ? C4 C5 C6 118.5(12) . . ? C6 C5 H5 120.8 . . ? C1 C6 C7 122.4(12) . . ? C5 C6 C1 120.7(12) . . ? C5 C6 C7 116.8(11) . . ? C6 C7 H7 116.6 . . ? N1 C7 C6 126.7(12) . . ? N1 C7 H7 116.6 . . ? N2 C8 C9 114.1(11) . . ? O2 C8 C9 117.3(12) . . ? O2 C8 N2 128.5(14) . . ? C10 C9 C8 123.8(12) . . ? N3 C9 C8 113.4(11) . . ? N3 C9 C10 122.8(12) . . ? C9 C10 H10 121.5 . . ? C11 C10 C9 116.9(13) . . ? C11 C10 H10 121.5 . . ? C10 C11 C12 123.6(13) . . ? C10 C11 Cl1 118.7(11) . . ? C12 C11 Cl1 117.6(10) . . ? C11 C12 H12 122.5 . . ? C11 C12 C13 115.1(13) . . ? C13 C12 H12 122.5 . . ? C12 C13 H13 118.1 . . ? N3 C13 C12 123.7(14) . . ? N3 C13 H13 118.1 . . ? C15 C14 C19 116.9(12) . . ? O3 C14 C15 122.2(12) . . ? O3 C14 C19 120.9(12) . . ? C14 C15 H15 117.7 . . ? C16 C15 C14 124.5(12) . . ? C16 C15 H15 117.7 . . ? C15 C16 H16 121.5 . . ? C15 C16 C17 117.0(13) . . ? C17 C16 H16 121.5 . . ? C16 C17 F2 117.5(12) . . ? C18 C17 C16 123.0(13) . . ? C18 C17 F2 119.5(12) . . ? C17 C18 H18 119.5 . . ? C17 C18 C19 121.1(13) . . ? C19 C18 H18 119.5 . . ? C18 C19 C14 117.4(12) . . ? C18 C19 C20 117.6(12) . . ? C20 C19 C14 125.1(12) . . ? C19 C20 H20 118.2 . . ? N4 C20 C19 123.6(12) . . ? N4 C20 H20 118.2 . . ? N5 C21 C22 117.8(11) . . ? N5 C21 O4 126.3(11) . . ? O4 C21 C22 115.9(10) . . ? C23 C22 C21 121.6(12) . . ? N6 C22 C21 115.0(11) . . ? N6 C22 C23 123.4(14) . . ? C22 C23 H23 121.9 . . ? C22 C23 C24 116.3(13) . . ? C24 C23 H23 121.9 . . ? C23 C24 Cl2 120.1(11) . . ? C25 C24 C23 121.9(12) . . ? C25 C24 Cl2 118.0(10) . . ? C24 C25 H25 121.7 . . ? C24 C25 C26 116.6(12) . . ? C26 C25 H25 121.7 . . ? C25 C26 H26 118.7 . . ? N6 C26 C25 122.6(12) . . ? N6 C26 H26 118.7 . . ? C28 C27 O7 117.6(12) . . ? C36 C27 C28 124.3(12) . . ? C36 C27 O7 118.1(12) . . ? C27 C28 H28 120.2 . . ? C29 C28 C27 119.6(13) . . ? C29 C28 H28 120.2 . . ? C28 C29 H29 120.3 . . ? C28 C29 C30 119.4(13) . . ? C30 C29 H29 120.3 . . ? C29 C30 C31 120.9(13) . . ? C35 C30 C29 120.5(13) . . ? C35 C30 C31 118.5(13) . . ? C30 C31 H31 119.4 . . ? C32 C31 C30 121.3(14) . . ? C32 C31 H31 119.4 . . ? C31 C32 H32 119.9 . . ? C31 C32 C33 120.2(14) . . ? C33 C32 H32 119.9 . . ? C32 C33 H33 119.7 . . ? C34 C33 C32 120.6(14) . . ? C34 C33 H33 119.7 . . ? C33 C34 H34 120.2 . . ? C33 C34 C35 119.6(15) . . ? C35 C34 H34 120.2 . . ? C30 C35 C34 119.6(13) . . ? C30 C35 C36 119.0(12) . . ? C34 C35 C36 121.4(13) . . ? C27 C36 C35 116.7(12) . . ? C27 C36 C37 120.6(11) . . ? C35 C36 C37 122.6(11) . . ? C38 C37 C36 122.9(12) . . ? C46 C37 C36 119.9(12) . . ? C46 C37 C38 116.8(13) . . ? C39 C38 C37 123.5(13) . . ? C39 C38 C43 117.2(12) . . ? C43 C38 C37 119.3(12) . . ? C38 C39 H39 119.3 . . ? C40 C39 C38 121.4(14) . . ? C40 C39 H39 119.3 . . ? C39 C40 H40 119.6 . . ? C41 C40 C39 120.8(14) . . ? C41 C40 H40 119.6 . . ? C40 C41 H41 119.4 . . ? C40 C41 C42 121.1(14) . . ? C42 C41 H41 119.4 . . ? C41 C42 H42 120.1 . . ? C41 C42 C43 119.8(15) . . ? C43 C42 H42 120.1 . . ? C38 C43 C44 119.1(13) . . ? C42 C43 C38 119.7(13) . . ? C42 C43 C44 121.2(14) . . ? C43 C44 H44 119.5 . . ? C45 C44 C43 120.9(14) . . ? C45 C44 H44 119.5 . . ? C44 C45 H45 120.7 . . ? C44 C45 C46 118.7(13) . . ? C46 C45 H45 120.7 . . ? C37 C46 C45 125.0(13) . . ? C37 C46 O8 118.4(12) . . ? C45 C46 O8 116.6(12) . . ? C56 C47 C48 124.0(14) . . ? C56 C47 O12 118.0(13) . . ? O12 C47 C48 118.0(12) . . ? C47 C48 H48 120.8 . . ? C49 C48 C47 118.4(15) . . ? C49 C48 H48 120.8 . . ? C48 C49 H49 119.0 . . ? C48 C49 C50 121.9(15) . . ? C50 C49 H49 119.0 . . ? C49 C50 C51 123.0(17) . . ? C55 C50 C49 118.2(13) . . ? C55 C50 C51 118.8(16) . . ? C50 C51 H51 119.5 . . ? C52 C51 C50 121.1(17) . . ? C52 C51 H51 119.5 . . ? C51 C52 H52 118.9 . . ? C51 C52 C53 122.1(15) . . ? C53 C52 H52 118.9 . . ? C52 C53 H53 120.4 . . ? C54 C53 C52 119.2(16) . . ? C54 C53 H53 120.4 . . ? C53 C54 H54 119.8 . . ? C53 C54 C55 120.4(16) . . ? C55 C54 H54 119.8 . . ? C50 C55 C54 118.2(13) . . ? C50 C55 C56 120.1(13) . . ? C56 C55 C54 121.5(14) . . ? C47 C56 C55 117.1(13) . . ? C47 C56 C57 118.9(13) . . ? C55 C56 C57 123.8(12) . . ? C58 C57 C56 124.1(12) . . ? C66 C57 C56 120.6(12) . . ? C66 C57 C58 115.0(13) . . ? C59 C58 C57 122.3(14) . . ? C59 C58 C63 117.7(14) . . ? C63 C58 C57 120.0(12) . . ? C58 C59 H59 119.4 . . ? C60 C59 C58 121.2(15) . . ? C60 C59 H59 119.4 . . ? C59 C60 H60 119.8 . . ? C59 C60 C61 120.4(15) . . ? C61 C60 H60 119.8 . . ? C60 C61 H61 119.9 . . ? C62 C61 C60 120.2(15) . . ? C62 C61 H61 119.9 . . ? C61 C62 H62 118.9 . . ? C61 C62 C63 122.2(16) . . ? C63 C62 H62 118.9 . . ? C58 C63 C62 118.1(14) . . ? C64 C63 C58 120.3(13) . . ? C64 C63 C62 121.2(15) . . ? C63 C64 H64 120.1 . . ? C65 C64 C63 119.8(14) . . ? C65 C64 H64 120.1 . . ? C64 C65 H65 120.6 . . ? C66 C65 C64 118.8(14) . . ? C66 C65 H65 120.6 . . ? C57 C66 C65 125.7(13) . . ? C57 C66 O11 116.9(13) . . ? C65 C66 O11 117.3(12) . . ? N7 C67 H67 117.5 . . ? O13 C67 H67 117.5 . . ? O13 C67 N7 125.1(13) . . ? H68A C68 H68B 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N7 C68 H68A 109.5 . . ? N7 C68 H68B 109.5 . . ? N7 C68 H68C 109.5 . . ? H69A C69 H69B 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N7 C69 H69A 109.5 . . ? N7 C69 H69B 109.5 . . ? N7 C69 H69C 109.5 . . ? N8 C70 H70 110.4 . . ? O14 C70 H70 110.4 . . ? O14 C70 N8 139(2) . . ? H71A C71 H71B 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N8 C71 H71A 109.5 . . ? N8 C71 H71B 109.5 . . ? N8 C71 H71C 109.5 . . ? H72A C72 H72B 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N8 C72 H72A 109.5 . . ? N8 C72 H72B 109.5 . . ? N8 C72 H72C 109.5 . . ? N1 Dy1 Dy2 98.2(3) . . ? N1 Dy1 N6 160.8(4) . . ? N6 Dy1 Dy2 98.0(3) . . ? O1 Dy1 Dy2 149.7(2) . . ? O1 Dy1 N1 74.0(4) . . ? O1 Dy1 N6 86.8(4) . . ? O1 Dy1 O2 126.6(3) . . ? O1 Dy1 O4 146.8(3) . . ? O1 Dy1 O5 79.1(3) . . ? O1 Dy1 O9 136.2(3) . . ? O1 Dy1 O13 72.8(3) . . ? O2 Dy1 Dy2 34.1(2) . . ? O2 Dy1 N1 64.4(3) . . ? O2 Dy1 N6 130.3(3) . . ? O2 Dy1 O13 142.6(3) . . ? O4 Dy1 Dy2 34.32(19) . . ? O4 Dy1 N1 132.1(3) . . ? O4 Dy1 N6 65.5(3) . . ? O4 Dy1 O2 68.5(3) . . ? O4 Dy1 O13 114.6(3) . . ? O5 Dy1 Dy2 72.8(2) . . ? O5 Dy1 N1 96.9(3) . . ? O5 Dy1 N6 78.4(3) . . ? O5 Dy1 O2 74.5(3) . . ? O5 Dy1 O4 77.7(3) . . ? O5 Dy1 O9 143.2(3) . . ? O5 Dy1 O13 142.7(3) . . ? O9 Dy1 Dy2 70.5(2) . . ? O9 Dy1 N1 86.6(3) . . ? O9 Dy1 N6 108.4(3) . . ? O9 Dy1 O2 74.2(3) . . ? O9 Dy1 O4 73.2(3) . . ? O9 Dy1 O13 71.7(3) . . ? O13 Dy1 Dy2 137.4(2) . . ? O13 Dy1 N1 98.4(3) . . ? O13 Dy1 N6 76.1(3) . . ? N3 Dy2 Dy1 97.0(2) . . ? N4 Dy2 Dy1 96.8(2) . . ? N4 Dy2 N3 165.4(3) . . ? O2 Dy2 Dy1 34.2(2) . . ? O2 Dy2 N3 63.6(3) . . ? O2 Dy2 N4 130.6(3) . . ? O2 Dy2 O4 68.3(3) . . ? O2 Dy2 O14 113.0(4) . . ? O3 Dy2 Dy1 149.7(3) . . ? O3 Dy2 N3 92.9(3) . . ? O3 Dy2 N4 72.7(3) . . ? O3 Dy2 O2 149.2(3) . . ? O3 Dy2 O4 124.5(3) . . ? O3 Dy2 O6 130.2(3) . . ? O3 Dy2 O10 78.6(3) . . ? O3 Dy2 O14 74.0(4) . . ? O4 Dy2 Dy1 34.1(2) . . ? O4 Dy2 N3 129.8(3) . . ? O4 Dy2 N4 63.2(3) . . ? O4 Dy2 O14 144.2(3) . . ? O6 Dy2 Dy1 73.0(2) . . ? O6 Dy2 N3 108.6(3) . . ? O6 Dy2 N4 80.2(3) . . ? O6 Dy2 O2 78.6(3) . . ? O6 Dy2 O4 74.0(3) . . ? O6 Dy2 O10 148.3(3) . . ? O6 Dy2 O14 71.5(3) . . ? O10 Dy2 Dy1 75.5(2) . . ? O10 Dy2 N3 78.5(3) . . ? O10 Dy2 N4 100.4(3) . . ? O10 Dy2 O2 77.4(3) . . ? O10 Dy2 O4 78.0(3) . . ? O10 Dy2 O14 137.8(3) . . ? O14 Dy2 Dy1 136.3(3) . . ? O14 Dy2 N3 71.5(3) . . ? O14 Dy2 N4 101.4(4) . . ? C7 N1 Dy1 128.3(9) . . ? C7 N1 N2 114.0(11) . . ? N2 N1 Dy1 117.7(8) . . ? C8 N2 N1 108.6(11) . . ? C9 N3 Dy2 118.0(8) . . ? C13 N3 C9 117.9(12) . . ? C13 N3 Dy2 124.0(10) . . ? C20 N4 Dy2 128.9(9) . . ? C20 N4 N5 113.8(10) . . ? N5 N4 Dy2 117.2(8) . . ? C21 N5 N4 110.8(10) . . ? C22 N6 C26 119.2(11) . . ? C22 N6 Dy1 118.6(9) . . ? C26 N6 Dy1 122.1(9) . . ? C67 N7 C68 119.2(11) . . ? C67 N7 C69 121.0(12) . . ? C68 N7 C69 118.9(12) . . ? C70 N8 C71 119(2) . . ? C70 N8 C72 128(2) . . ? C72 N8 C71 112.8(18) . . ? C1 O1 Dy1 135.4(8) . . ? C8 O2 Dy1 117.2(9) . . ? C8 O2 Dy2 126.1(9) . . ? Dy2 O2 Dy1 111.7(4) . . ? C14 O3 Dy2 133.1(8) . . ? C21 O4 Dy1 123.8(7) . . ? C21 O4 Dy2 117.6(7) . . ? Dy1 O4 Dy2 111.6(4) . . ? P1 O5 Dy1 134.8(5) . . ? P1 O6 Dy2 137.1(5) . . ? C27 O7 P1 118.5(8) . . ? C46 O8 P1 115.0(8) . . ? P2 O9 Dy1 141.2(5) . . ? P2 O10 Dy2 132.2(5) . . ? C66 O11 P2 119.3(8) . . ? C47 O12 P2 112.9(8) . . ? C67 O13 Dy1 136.2(9) . . ? C70 O14 Dy2 141.6(14) . . ? O5 P1 O6 120.1(5) . . ? O5 P1 O7 111.3(5) . . ? O5 P1 O8 106.8(5) . . ? O6 P1 O7 105.8(5) . . ? O6 P1 O8 109.2(5) . . ? O8 P1 O7 102.3(5) . . ? O9 P2 O10 120.6(5) . . ? O9 P2 O11 105.6(5) . . ? O9 P2 O12 110.2(5) . . ? O10 P2 O11 110.5(5) . . ? O10 P2 O12 106.9(5) . . ? O12 P2 O11 101.4(5) . . ? N10 C76 H76 113.9 . . ? O16 C76 H76 113.9 . . ? O16 C76 N10 132(3) . . ? H77A C77 H77B 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? N10 C77 H77A 109.5 . . ? N10 C77 H77B 109.5 . . ? N10 C77 H77C 109.5 . . ? H78A C78 H78B 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N10 C78 H78A 109.5 . . ? N10 C78 H78B 109.5 . . ? N10 C78 H78C 109.5 . . ? C76 N10 C77 119(3) . . ? C76 N10 C78 125(2) . . ? C77 N10 C78 116(3) . . ? N9 C73 H73 117.1 . . ? O15 C73 H73 117.1 . . ? O15 C73 N9 125.8(19) . . ? H74A C74 H74B 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N9 C74 H74A 109.5 . . ? N9 C74 H74B 109.5 . . ? N9 C74 H74C 109.5 . . ? H75A C75 H75B 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N9 C75 H75A 109.5 . . ? N9 C75 H75B 109.5 . . ? N9 C75 H75C 109.5 . . ? C73 N9 C74 123.1(16) . . ? C73 N9 C75 119.5(15) . . ? C74 N9 C75 116.8(14) . . ? N11 C79 H79 116.4 . . ? O17 C79 H79 116.4 . . ? O17 C79 N11 127.3(17) . . ? H80A C80 H80B 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N11 C80 H80A 109.5 . . ? N11 C80 H80B 109.5 . . ? N11 C80 H80C 109.5 . . ? H81A C81 H81B 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N11 C81 H81A 109.5 . . ? N11 C81 H81B 109.5 . . ? N11 C81 H81C 109.5 . . ? C79 N11 C80 121.0(18) . . ? C79 N11 C81 120.0(15) . . ? C80 N11 C81 118.8(17) . . ? 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 1.462(17) . ? C1 C6 1.440(17) . ? C1 O1 1.334(16) . ? C2 H2 0.9500 . ? C2 C3 1.37(2) . ? C3 H3 0.9500 . ? C3 C4 1.38(2) . ? C4 C5 1.36(2) . ? C4 F1 1.383(16) . ? C5 H5 0.9500 . ? C5 C6 1.389(18) . ? C6 C7 1.453(18) . ? C7 H7 0.9500 . ? C7 N1 1.288(17) . ? C8 C9 1.49(2) . ? C8 N2 1.307(18) . ? C8 O2 1.283(15) . ? C9 C10 1.372(18) . ? C9 N3 1.362(17) . ? C10 H10 0.9500 . ? C10 C11 1.355(19) . ? C11 C12 1.367(19) . ? C11 Cl1 1.772(14) . ? C12 H12 0.9500 . ? C12 C13 1.41(2) . ? C13 H13 0.9500 . ? C13 N3 1.313(17) . ? C14 C15 1.371(19) . ? C14 C19 1.448(19) . ? C14 O3 1.299(16) . ? C15 H15 0.9500 . ? C15 C16 1.369(19) . ? C16 H16 0.9500 . ? C16 C17 1.382(19) . ? C17 C18 1.319(19) . ? C17 F2 1.393(15) . ? C18 H18 0.9500 . ? C18 C19 1.423(19) . ? C19 C20 1.437(18) . ? C20 H20 0.9500 . ? C20 N4 1.287(17) . ? C21 C22 1.517(19) . ? C21 N5 1.293(16) . ? C21 O4 1.310(15) . ? C22 C23 1.386(19) . ? C22 N6 1.326(17) . ? C23 H23 0.9500 . ? C23 C24 1.39(2) . ? C24 C25 1.38(2) . ? C24 Cl2 1.743(13) . ? C25 H25 0.9500 . ? C25 C26 1.394(19) . ? C26 H26 0.9500 . ? C26 N6 1.337(16) . ? C27 C28 1.379(19) . ? C27 C36 1.371(18) . ? C27 O7 1.400(15) . ? C28 H28 0.9500 . ? C28 C29 1.370(19) . ? C29 H29 0.9500 . ? C29 C30 1.421(19) . ? C30 C31 1.43(2) . ? C30 C35 1.402(19) . ? C31 H31 0.9500 . ? C31 C32 1.35(2) . ? C32 H32 0.9500 . ? C32 C33 1.42(2) . ? C33 H33 0.9500 . ? C33 C34 1.37(2) . ? C34 H34 0.9500 . ? C34 C35 1.43(2) . ? C35 C36 1.450(18) . ? C36 C37 1.491(19) . ? C37 C38 1.450(18) . ? C37 C46 1.373(19) . ? C38 C39 1.409(19) . ? C38 C43 1.42(2) . ? C39 H39 0.9500 . ? C39 C40 1.375(19) . ? C40 H40 0.9500 . ? C40 C41 1.35(2) . ? C41 H41 0.9500 . ? C41 C42 1.37(2) . ? C42 H42 0.9500 . ? C42 C43 1.42(2) . ? C43 C44 1.43(2) . ? C44 H44 0.9500 . ? C44 C45 1.37(2) . ? C45 H45 0.9500 . ? C45 C46 1.380(19) . ? C46 O8 1.409(15) . ? C47 C48 1.41(2) . ? C47 C56 1.370(19) . ? C47 O12 1.398(16) . ? C48 H48 0.9500 . ? C48 C49 1.35(2) . ? C49 H49 0.9500 . ? C49 C50 1.43(2) . ? C50 C51 1.43(2) . ? C50 C55 1.42(2) . ? C51 H51 0.9500 . ? C51 C52 1.33(3) . ? C52 H52 0.9500 . ? C52 C53 1.41(3) . ? C53 H53 0.9500 . ? C53 C54 1.38(2) . ? C54 H54 0.9500 . ? C54 C55 1.44(2) . ? C55 C56 1.44(2) . ? C56 C57 1.47(2) . ? C57 C58 1.455(19) . ? C57 C66 1.375(19) . ? C58 C59 1.423(19) . ? C58 C63 1.43(2) . ? C59 H59 0.9500 . ? C59 C60 1.37(2) . ? C60 H60 0.9500 . ? C60 C61 1.40(2) . ? C61 H61 0.9500 . ? C61 C62 1.33(2) . ? C62 H62 0.9500 . ? C62 C63 1.43(2) . ? C63 C64 1.40(2) . ? C64 H64 0.9500 . ? C64 C65 1.38(2) . ? C65 H65 0.9500 . ? C65 C66 1.38(2) . ? C66 O11 1.417(16) . ? C67 H67 0.9500 . ? C67 N7 1.316(17) . ? C67 O13 1.243(15) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C68 N7 1.451(17) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C69 N7 1.455(18) . ? C70 H70 0.9500 . ? C70 N8 1.314(19) . ? C70 O14 1.14(2) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C71 N8 1.50(2) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C72 N8 1.40(2) . ? Dy1 Dy2 3.9383(11) . ? Dy1 N1 2.481(11) . ? Dy1 N6 2.524(10) . ? Dy1 O1 2.200(9) . ? Dy1 O2 2.382(9) . ? Dy1 O4 2.373(9) . ? Dy1 O5 2.331(8) . ? Dy1 O9 2.332(9) . ? Dy1 O13 2.408(8) . ? Dy2 N3 2.587(12) . ? Dy2 N4 2.525(10) . ? Dy2 O2 2.378(9) . ? Dy2 O3 2.212(9) . ? Dy2 O4 2.388(8) . ? Dy2 O6 2.295(9) . ? Dy2 O10 2.355(8) . ? Dy2 O14 2.406(9) . ? N1 N2 1.439(15) . ? N4 N5 1.396(15) . ? O5 P1 1.495(9) . ? O6 P1 1.497(10) . ? O7 P1 1.611(9) . ? O8 P1 1.611(9) . ? O9 P2 1.469(9) . ? O10 P2 1.490(9) . ? O11 P2 1.622(10) . ? O12 P2 1.617(9) . ? C76 H76 0.9500 . ? C76 N10 1.28(2) . ? C76 O16 1.19(2) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C77 N10 1.42(2) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C78 N10 1.46(2) . ? C73 H73 0.9500 . ? C73 N9 1.34(2) . ? C73 O15 1.22(2) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C74 N9 1.42(2) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C75 N9 1.48(2) . ? C79 H79 0.9500 . ? C79 N11 1.33(2) . ? C79 O17 1.20(2) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C80 N11 1.42(2) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C81 N11 1.47(2) . ? 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 C1 C2 C3 C4 2(2) . . . . ? C1 C6 C7 N1 18(2) . . . . ? C2 C1 C6 C5 4.3(18) . . . . ? C2 C1 C6 C7 -179.6(12) . . . . ? C2 C1 O1 Dy1 141.4(11) . . . . ? C2 C3 C4 C5 -2(2) . . . . ? C2 C3 C4 F1 179.2(13) . . . . ? C3 C4 C5 C6 3(2) . . . . ? C4 C5 C6 C1 -4.5(19) . . . . ? C4 C5 C6 C7 179.2(12) . . . . ? C5 C6 C7 N1 -165.6(12) . . . . ? C6 C1 C2 C3 -3.0(19) . . . . ? C6 C1 O1 Dy1 -37.7(18) . . . . ? C6 C7 N1 Dy1 -3.1(18) . . . . ? C6 C7 N1 N2 179.5(11) . . . . ? C7 N1 N2 C8 164.5(11) . . . . ? C8 C9 C10 C11 179.4(12) . . . . ? C8 C9 N3 C13 -179.3(12) . . . . ? C8 C9 N3 Dy2 4.2(14) . . . . ? C9 C8 N2 N1 -178.2(10) . . . . ? C9 C8 O2 Dy1 -167.2(8) . . . . ? C9 C8 O2 Dy2 -14.2(15) . . . . ? C9 C10 C11 C12 -2(2) . . . . ? C9 C10 C11 Cl1 -178.0(10) . . . . ? C10 C9 N3 C13 -1(2) . . . . ? C10 C9 N3 Dy2 -177.2(9) . . . . ? C10 C11 C12 C13 3(2) . . . . ? C11 C12 C13 N3 -2(2) . . . . ? C12 C13 N3 C9 1(2) . . . . ? C12 C13 N3 Dy2 177.7(10) . . . . ? C14 C15 C16 C17 2(2) . . . . ? C14 C19 C20 N4 -15(2) . . . . ? C15 C14 C19 C18 -3.5(19) . . . . ? C15 C14 C19 C20 175.7(13) . . . . ? C15 C14 O3 Dy2 -133.5(12) . . . . ? C15 C16 C17 C18 -2(2) . . . . ? C15 C16 C17 F2 177.5(12) . . . . ? C16 C17 C18 C19 -1(2) . . . . ? C17 C18 C19 C14 4(2) . . . . ? C17 C18 C19 C20 -175.5(13) . . . . ? C18 C19 C20 N4 164.0(12) . . . . ? C19 C14 C15 C16 1(2) . . . . ? C19 C14 O3 Dy2 47.2(18) . . . . ? C19 C20 N4 Dy2 -0.5(19) . . . . ? C19 C20 N4 N5 -177.2(12) . . . . ? C20 N4 N5 C21 -167.5(11) . . . . ? C21 C22 C23 C24 -179.3(12) . . . . ? C21 C22 N6 C26 179.4(11) . . . . ? C21 C22 N6 Dy1 -3.4(13) . . . . ? C22 C21 N5 N4 -178.2(10) . . . . ? C22 C21 O4 Dy1 12.3(13) . . . . ? C22 C21 O4 Dy2 160.6(7) . . . . ? C22 C23 C24 C25 -1(2) . . . . ? C22 C23 C24 Cl2 177.7(10) . . . . ? C23 C22 N6 C26 -1.2(19) . . . . ? C23 C22 N6 Dy1 176.0(10) . . . . ? C23 C24 C25 C26 0(2) . . . . ? C24 C25 C26 N6 0(2) . . . . ? C25 C26 N6 C22 1(2) . . . . ? C25 C26 N6 Dy1 -176.6(11) . . . . ? C27 C28 C29 C30 4(2) . . . . ? C27 C36 C37 C38 -124.4(14) . . . . ? C27 C36 C37 C46 48.7(18) . . . . ? C27 O7 P1 O5 -69.5(10) . . . . ? C27 O7 P1 O6 158.5(9) . . . . ? C27 O7 P1 O8 44.2(10) . . . . ? C28 C27 C36 C35 -4(2) . . . . ? C28 C27 C36 C37 179.2(13) . . . . ? C28 C27 O7 P1 106.8(12) . . . . ? C28 C29 C30 C31 178.8(13) . . . . ? C28 C29 C30 C35 0(2) . . . . ? C29 C30 C31 C32 -177.2(15) . . . . ? C29 C30 C35 C34 175.3(13) . . . . ? C29 C30 C35 C36 -6(2) . . . . ? C30 C31 C32 C33 1(3) . . . . ? C30 C35 C36 C27 7.7(18) . . . . ? C30 C35 C36 C37 -175.8(12) . . . . ? C31 C30 C35 C34 -4(2) . . . . ? C31 C30 C35 C36 175.4(13) . . . . ? C31 C32 C33 C34 -3(3) . . . . ? C32 C33 C34 C35 1(2) . . . . ? C33 C34 C35 C30 2(2) . . . . ? C33 C34 C35 C36 -176.6(13) . . . . ? C34 C35 C36 C27 -173.4(13) . . . . ? C34 C35 C36 C37 3(2) . . . . ? C35 C30 C31 C32 2(2) . . . . ? C35 C36 C37 C38 59.3(18) . . . . ? C35 C36 C37 C46 -127.7(14) . . . . ? C36 C27 C28 C29 -1(2) . . . . ? C36 C27 O7 P1 -75.6(13) . . . . ? C36 C37 C38 C39 -2(2) . . . . ? C36 C37 C38 C43 174.9(12) . . . . ? C36 C37 C46 C45 -174.5(13) . . . . ? C36 C37 C46 O8 4.0(19) . . . . ? C37 C38 C39 C40 179.6(13) . . . . ? C37 C38 C43 C42 -179.8(13) . . . . ? C37 C38 C43 C44 0(2) . . . . ? C37 C46 O8 P1 -79.5(14) . . . . ? C38 C37 C46 C45 -1(2) . . . . ? C38 C37 C46 O8 177.5(11) . . . . ? C38 C39 C40 C41 -1(2) . . . . ? C38 C43 C44 C45 -4(2) . . . . ? C39 C38 C43 C42 -2(2) . . . . ? C39 C38 C43 C44 178.0(13) . . . . ? C39 C40 C41 C42 0(2) . . . . ? C40 C41 C42 C43 0(2) . . . . ? C41 C42 C43 C38 1(2) . . . . ? C41 C42 C43 C44 -179.2(15) . . . . ? C42 C43 C44 C45 176.7(15) . . . . ? C43 C38 C39 C40 2(2) . . . . ? C43 C44 C45 C46 4(2) . . . . ? C44 C45 C46 C37 -2(2) . . . . ? C44 C45 C46 O8 179.5(13) . . . . ? C45 C46 O8 P1 99.1(13) . . . . ? C46 C37 C38 C39 -175.7(13) . . . . ? C46 C37 C38 C43 1.7(18) . . . . ? C46 O8 P1 O5 166.5(9) . . . . ? C46 O8 P1 O6 -62.2(10) . . . . ? C46 O8 P1 O7 49.5(10) . . . . ? C47 C48 C49 C50 4(2) . . . . ? C47 C56 C57 C58 -119.6(15) . . . . ? C47 C56 C57 C66 54(2) . . . . ? C47 O12 P2 O9 -55.3(10) . . . . ? C47 O12 P2 O10 171.9(9) . . . . ? C47 O12 P2 O11 56.1(9) . . . . ? C48 C47 C56 C55 -5(2) . . . . ? C48 C47 C56 C57 -180.0(13) . . . . ? C48 C47 O12 P2 98.0(13) . . . . ? C48 C49 C50 C51 172.0(15) . . . . ? C48 C49 C50 C55 -6(2) . . . . ? C49 C50 C51 C52 179.8(15) . . . . ? C49 C50 C55 C54 176.6(13) . . . . ? C49 C50 C55 C56 2(2) . . . . ? C50 C51 C52 C53 5(3) . . . . ? C50 C55 C56 C47 3(2) . . . . ? C50 C55 C56 C57 178.0(13) . . . . ? C51 C50 C55 C54 -1.0(19) . . . . ? C51 C50 C55 C56 -175.9(13) . . . . ? C51 C52 C53 C54 -4(2) . . . . ? C52 C53 C54 C55 0(2) . . . . ? C53 C54 C55 C50 2(2) . . . . ? C53 C54 C55 C56 176.9(13) . . . . ? C54 C55 C56 C47 -171.4(12) . . . . ? C54 C55 C56 C57 3(2) . . . . ? C55 C50 C51 C52 -3(2) . . . . ? C55 C56 C57 C58 66(2) . . . . ? C55 C56 C57 C66 -121.1(15) . . . . ? C56 C47 C48 C49 1(2) . . . . ? C56 C47 O12 P2 -80.2(13) . . . . ? C56 C57 C58 C59 0(2) . . . . ? C56 C57 C58 C63 176.8(13) . . . . ? C56 C57 C66 C65 179.1(14) . . . . ? C56 C57 C66 O11 1.7(19) . . . . ? C57 C58 C59 C60 174.7(14) . . . . ? C57 C58 C63 C62 -172.4(13) . . . . ? C57 C58 C63 C64 1(2) . . . . ? C57 C66 O11 P2 -73.7(14) . . . . ? C58 C57 C66 C65 -7(2) . . . . ? C58 C57 C66 O11 175.4(11) . . . . ? C58 C59 C60 C61 -1(3) . . . . ? C58 C63 C64 C65 -3(2) . . . . ? C59 C58 C63 C62 5(2) . . . . ? C59 C58 C63 C64 178.4(14) . . . . ? C59 C60 C61 C62 2(3) . . . . ? C60 C61 C62 C63 1(3) . . . . ? C61 C62 C63 C58 -4(2) . . . . ? C61 C62 C63 C64 -177.8(16) . . . . ? C62 C63 C64 C65 170.8(15) . . . . ? C63 C58 C59 C60 -2(2) . . . . ? C63 C64 C65 C66 -1(2) . . . . ? C64 C65 C66 C57 6(2) . . . . ? C64 C65 C66 O11 -176.5(13) . . . . ? C65 C66 O11 P2 108.6(13) . . . . ? C66 C57 C58 C59 -173.7(13) . . . . ? C66 C57 C58 C63 3.3(19) . . . . ? C66 O11 P2 O9 153.0(9) . . . . ? C66 O11 P2 O10 -75.1(10) . . . . ? C66 O11 P2 O12 38.1(10) . . . . ? Cl1 C11 C12 C13 178.6(11) . . . . ? Cl2 C24 C25 C26 -178.4(11) . . . . ? Dy1 N1 N2 C8 -13.1(12) . . . . ? Dy1 O5 P1 O6 19.7(10) . . . . ? Dy1 O5 P1 O7 -104.6(7) . . . . ? Dy1 O5 P1 O8 144.5(7) . . . . ? Dy1 O9 P2 O10 2.8(12) . . . . ? Dy1 O9 P2 O11 128.8(8) . . . . ? Dy1 O9 P2 O12 -122.5(8) . . . . ? Dy2 N4 N5 C21 15.3(12) . . . . ? Dy2 O6 P1 O5 -5.3(11) . . . . ? Dy2 O6 P1 O7 121.6(8) . . . . ? Dy2 O6 P1 O8 -129.0(8) . . . . ? Dy2 O10 P2 O9 0.7(11) . . . . ? Dy2 O10 P2 O11 -122.9(7) . . . . ? Dy2 O10 P2 O12 127.6(7) . . . . ? F1 C4 C5 C6 -178.0(11) . . . . ? F2 C17 C18 C19 179.6(11) . . . . ? N2 C8 C9 C10 3.3(18) . . . . ? N2 C8 C9 N3 -178.1(11) . . . . ? N2 C8 O2 Dy1 16.9(17) . . . . ? N2 C8 O2 Dy2 169.8(10) . . . . ? N3 C9 C10 C11 1.0(19) . . . . ? N5 C21 C22 C23 -4.2(17) . . . . ? N5 C21 C22 N6 175.2(11) . . . . ? N5 C21 O4 Dy1 -168.1(9) . . . . ? N5 C21 O4 Dy2 -19.8(15) . . . . ? N6 C22 C23 C24 1.3(19) . . . . ? N7 C67 O13 Dy1 162.8(10) . . . . ? N8 C70 O14 Dy2 179.3(17) . . . . ? O1 C1 C2 C3 177.9(12) . . . . ? O1 C1 C6 C5 -176.5(11) . . . . ? O1 C1 C6 C7 -0.4(19) . . . . ? O2 C8 C9 C10 -173.2(12) . . . . ? O2 C8 C9 N3 5.4(16) . . . . ? O2 C8 N2 N1 -2.1(18) . . . . ? O3 C14 C15 C16 -178.6(13) . . . . ? O3 C14 C19 C18 175.9(12) . . . . ? O3 C14 C19 C20 -5(2) . . . . ? O4 C21 C22 C23 175.4(11) . . . . ? O4 C21 C22 N6 -5.2(15) . . . . ? O4 C21 N5 N4 2.2(17) . . . . ? O7 C27 C28 C29 176.0(11) . . . . ? O7 C27 C36 C35 178.3(11) . . . . ? O7 C27 C36 C37 1.7(18) . . . . ? O12 C47 C48 C49 -176.8(13) . . . . ? O12 C47 C56 C55 173.2(11) . . . . ? O12 C47 C56 C57 -1.8(19) . . . . ? O13 C67 N7 C68 -4(2) . . . . ? O13 C67 N7 C69 -173.0(13) . . . . ? O14 C70 N8 C71 2(4) . . . . ? O14 C70 N8 C72 -175(2) . . . . ? O16 C76 N10 C77 7(5) . . . . ? O16 C76 N10 C78 -167(3) . . . . ? O15 C73 N9 C74 3(3) . . . . ? O15 C73 N9 C75 173.4(16) . . . . ? O17 C79 N11 C80 176.4(19) . . . . ? O17 C79 N11 C81 2(3) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.966(6) 2 0.034(6)