#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:32:37 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242516 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132550.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_4132550 loop_ _publ_author_name 'Wang, Yu-Xia' 'Ma, Yinina' 'Chai, Yisheng' 'Shi, Wei' 'Sun, Young' 'Cheng, Peng' _publ_section_title ; Observation of Magnetodielectric Effect in a Dysprosium-Based Single-Molecule Magnet. ; _journal_issue 25 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7795 _journal_page_last 7798 _journal_paper_doi 10.1021/jacs.8b04818 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety 'C38 H72 Cl3 Dy O3 P2, C2 H6 O' _chemical_formula_sum 'C40 H78 Cl3 Dy O4 P2' _chemical_formula_weight 953.81 _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 mixed _atom_sites_solution_primary direct _audit_creation_date 2018-05-04 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.4000(5) _cell_length_b 15.3943(5) _cell_length_c 19.6252(13) _cell_measurement_reflns_used 5040 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 28.9742 _cell_measurement_theta_min 2.3740 _cell_volume 4652.6(4) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_unetI/netI 0.1179 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 15242 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.009 _diffrn_reflns_theta_max 25.009 _diffrn_reflns_theta_min 2.842 _exptl_absorpt_coefficient_mu 1.882 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.362 _exptl_crystal_description colorless _exptl_crystal_F_000 1988 _refine_diff_density_max 1.854 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.109 _refine_ls_abs_structure_details ; Flack x determined using 1457 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.078(14) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 459 _refine_ls_number_reflns 7796 _refine_ls_number_restraints 365 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0612 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1259 _refine_ls_wR_factor_ref 0.1451 _reflns_Friedel_coverage 0.802 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 5823 _reflns_number_total 7796 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04818_si_002.cif _cod_data_source_block a _cod_database_code 4132550 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.7065(14) 0.2935(14) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 3. Restrained distances C21-C5 1.45 with sigma of 0.02 C6-C2 1.45 with sigma of 0.02 H6A_$1-H13B_$2 2.15 with sigma of 0.02 H6C-H13B_$3 2.15 with sigma of 0.02 O1AA-H1AB 0.85 with sigma of 0.01 O1AA-H1AA 0.85 with sigma of 0.01 C2-O1AA 1.45 with sigma of 0.02 C21-O1AA 1.45 with sigma of 0.02 C11-C8 1.45 with sigma of 0.02 O2AA-C11 1.4 with sigma of 0.02 Dy1-H1AB 2.974488 with sigma of 0.02 Dy1-H1AA 2.923229 with sigma of 0.02 C2-H1AB 1.886394 with sigma of 0.02 C21-H1AA 1.912694 with sigma of 0.02 C8CA-C20 \\sim C20-C9 with sigma of 0.02 C1-C0BA \\sim C0BA-C8CA with sigma of 0.02 C7-C4 \\sim C4-C6DA with sigma of 0.02 C4-C6DA \\sim C6DA-C15 with sigma of 0.02 C6DA-C15 \\sim C15-C3CA with sigma of 0.02 C9-C20 \\sim C20-C8CA with sigma of 0.02 C13-C1 \\sim C1-C0BA with sigma of 0.02 C8CA-C13 \\sim C1-C20 with sigma of 0.02 C1-C13 \\sim C13-C9 with sigma of 0.02 C13-C9 \\sim C9-C20 with sigma of 0.02 C8CA-C13 \\sim C20-C1 with sigma of 0.02 C8CA-C1 \\sim C13-C20 with sigma of 0.02 C8CA-C0BA \\sim C0BA-C1 with sigma of 0.02 C20-C9 \\sim C9-C13 with sigma of 0.02 C9-C13 \\sim C13-C1 with sigma of 0.02 C0BA-C8CA \\sim C8CA-C20 with sigma of 0.02 C0BA-C1 \\sim C1-C13 with sigma of 0.02 C15-C3CA \\sim C3CA-C4CA with sigma of 0.02 C3CA-C4CA \\sim C4CA-C7 with sigma of 0.02 C4CA-C7 \\sim C7-C4 with sigma of 0.02 C6DA-C4CA \\sim C4-C3CA with sigma of 0.02 4. Uiso/Uaniso restraints and constraints C0BA \\sim C8CA \\sim C20 \\sim C1 \\sim C9 \\sim C13: within 3.8A with sigma of 0.005 and sigma for terminal atoms of 0.005 C4CA \\sim C4 \\sim C6DA \\sim C15 \\sim C3CA \\sim C7: within 3.8A with sigma of 0.005 and sigma for terminal atoms of 0.005 C6CA \\sim P6AA \\sim C15 \\sim C0BA: within 3.8A with sigma of 0.003 and sigma for terminal atoms of 0.003 Uanis(C15) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C4CA) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C8CA) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C3CA) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01 Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005 Uanis(C2) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005 Uanis(O10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005 Uanis(O2AA) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01 Uanis(C2) = Uanis(C21) Uanis(C6) = Uanis(C5) 5. Others Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=1- FVAR(1) Sof(H1AA)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)= FVAR(1) 6.a Riding coordinates: O1AA(H1AB), O1AA(H1AA), O2AA(H2AA), C3AA(H3AA,H3AB), C4AA(H4AA,H4AB), C5CA(H5CA,H5CB), C7CA(H7CA,H7CB), C7BA(H7BA,H7BB), C9BA(H9BA,H9BB), C3CA(H3CA, H3CB), C6DA(H6DA,H6DB), C8DA(H8DA,H8DB), C9DA(H9DA,H9DB), C0EA(H0EA,H0EB), C3BA(H3BA,H3BB), C4CA(H4CA,H4CB), C8CA(H8CA,H8CB), C0DA(H0DA,H0DB), C1DA(H1DA, H1DB), C2(H2A,H2B), C3DA(H3DA,H3DB), C5DA(H5DA,H5DB), C0CA(H0CA,H0CB), C5AA(H5AA,H5AB), C0AA(H0AA,H0AB), C11(H11A,H11B), C12(H12A,H12B), C20(H20A, H20B), C4(H4A,H4B), C7(H7A,H7B), C1(H1A,H1B), C3(H3A,H3B), C9(H9A,H9B), C13(H13A,H13B), C6(H6A,H6B,H6C), C21(H21A,H21B), C5(H5A,H5B,H5C), C8(H8A,H8B, H8C) 6.b Ternary CH refined with riding coordinates: C6CA(H6CA), C5BA(H5BA), C1CA(H1CA), C0BA(H0BA), C7DA(H7DA), C15(H15) 6.c Secondary CH2 refined with riding coordinates: C9CA(H9CA,H9CB) ; _shelx_res_file ; a.res created by SHELXL-2014/7 TITL a in P212121 #19 REM reset to P212121 #19 CELL 0.71073 15.4 15.3943 19.6252 90 90 90 ZERR 4 0.0005 0.0005 0.0013 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Dy O P UNIT 160 312 12 4 16 8 EQIV $1 -1+X,+Y,+Z EQIV $2 -0.5+X,0.5-Y,1-Z EQIV $3 0.5+X,0.5-Y,1-Z DFIX 1.45 C21 C5 DFIX 1.45 C6 C2 DFIX 2.15 H6a_$1 H13b_$2 DFIX 2.15 H6c H13b_$3 DFIX 0.85 0.01 O1AA H1Ab DFIX 0.85 0.01 O1AA H1AA DFIX 1.45 C2 O1AA DFIX 1.45 C21 O1AA DFIX 1.45 C11 C8 DFIX 1.4 O2AA C11 SADI C8CA C20 C20 C9 SADI C1 C0BA C0BA C8CA SADI C7 C4 C4 C6DA SADI C4 C6DA C6DA C15 SADI C6DA C15 C15 C3CA SADI C9 C20 C20 C8CA SADI C13 C1 C1 C0BA SADI C8CA C13 C1 C20 SADI C1 C13 C13 C9 SADI C13 C9 C9 C20 SADI C8CA C13 C20 C1 SADI C8CA C1 C13 C20 SADI C8CA C0BA C0BA C1 SADI C20 C9 C9 C13 SADI C9 C13 C13 C1 SADI C0BA C8CA C8CA C20 SADI C0BA C1 C1 C13 SADI C15 C3CA C3CA C4CA SADI C3CA C4CA C4CA C7 SADI C4CA C7 C7 C4 SADI C6DA C4CA C4 C3CA DANG 2.974488 0.02 Dy1 H1Ab DANG 2.923229 0.02 Dy1 H1AA DANG 1.886394 0.02 C2 H1Ab DANG 1.912694 0.02 C21 H1AA SIMU 0.005 0.005 3.8 C0BA C8CA C20 C1 C9 C13 SIMU 0.005 0.005 3.8 C4CA C4 C6DA C15 C3CA C7 SIMU 0.003 0.003 3.8 C6CA P6AA C15 C0BA ISOR 0.01 0.01 C15 C4 C4CA C20 C8CA C1 C3 C9 C3CA C13 C7 ISOR 0.005 0.005 C8 ISOR 0.005 0.005 C2 C21 ISOR 0.005 0.005 O10 ISOR 0.01 0.01 O2AA C11 EADP C2 C21 EADP C6 C5 L.S. 20 0 0 PLAN 20 BOND MORE -1 BOND $H CONF fmap 2 53 acta 52 TWIN 0 1 0 1 0 0 0 0 -1 2 OMIT -3 50.02 OMIT 1 0 5 OMIT -7 2 20 OMIT 11 3 17 OMIT -2 6 21 OMIT -9 1 11 OMIT 3 1 2 OMIT 2 1 4 OMIT -11 1 17 OMIT 9 5 18 OMIT 4 0 0 OMIT 1 3 2 OMIT 4 16 7 OMIT 2 1 5 OMIT -1 2 5 OMIT 0 2 3 REM REM REM WGHT 0.041700 BASF 0.29352 FVAR 0.24731 0.55443 DY1 4 0.278562 0.502180 0.479213 11.00000 0.03629 0.03812 = 0.05585 0.00626 -0.00014 -0.00609 P0AA 6 0.435342 0.684020 0.486569 11.00000 0.03576 0.03288 = 0.05029 0.00892 -0.00206 -0.00880 P6AA 6 0.117736 0.326829 0.473209 11.00000 0.05335 0.04927 = 0.05756 0.00755 0.00699 -0.01200 CL9A 3 0.403615 0.389211 0.462726 11.00000 0.10751 0.04958 = 0.07080 -0.00218 -0.00747 0.03438 CL1B 3 0.238636 0.529898 0.350258 11.00000 0.10403 0.05826 = 0.06150 -0.00289 -0.01720 0.01066 CL2B 3 0.166307 0.614256 0.527132 11.00000 0.06014 0.15336 = 0.07023 0.03333 0.01904 0.05822 O1AA 5 0.299061 0.482449 0.598565 11.00000 0.03283 0.08534 = 0.05851 0.00037 0.00320 0.00908 PART 2 AFIX 3 H1AB 2 0.267861 0.506579 0.629894 -21.00000 -1.50000 AFIX 3 PART 0 PART 1 H1AA 2 0.277381 0.521209 0.626844 21.00000 -1.50000 AFIX 0 PART 0 O2AA 5 0.210645 0.534770 0.705586 11.00000 0.11491 0.13941 = 0.06043 0.01145 0.00544 0.05221 AFIX 3 H2AA 2 0.225465 0.514960 0.745786 11.00000 -1.50000 AFIX 0 C3AA 1 0.269751 0.827365 0.361860 11.00000 0.05642 0.05889 = 0.11099 0.03014 -0.03408 -0.00224 AFIX 3 H3AA 2 0.230341 0.852615 0.394980 11.00000 -1.20000 H3AB 2 0.235641 0.808435 0.323050 11.00000 -1.20000 AFIX 0 C4AA 1 0.588057 0.594105 0.483686 11.00000 0.04149 0.05930 = 0.05686 0.01707 -0.00365 0.00483 AFIX 3 H4AA 2 0.552927 0.541825 0.483356 11.00000 -1.20000 H4AB 2 0.598247 0.610345 0.530766 11.00000 -1.20000 AFIX 0 O2CA 5 0.380656 0.604229 0.481260 11.00000 0.05988 0.01567 = 0.04796 -0.00376 -0.01315 0.00387 C5CA 1 0.336552 0.898103 0.337858 11.00000 0.09386 0.03083 = 0.07058 0.01840 -0.04471 0.00333 AFIX 3 H5CA 2 0.305072 0.947483 0.319658 11.00000 -1.20000 H5CB 2 0.372072 0.874373 0.301558 11.00000 -1.20000 AFIX 0 C6CA 1 0.081074 0.284117 0.554344 11.00000 0.06054 0.05680 = 0.06440 0.00672 0.00627 -0.00763 AFIX 13 H6CA 2 0.037550 0.239015 0.545658 11.00000 -1.20000 AFIX 0 C7CA 1 0.440787 0.846715 0.427143 11.00000 0.05984 0.02572 = 0.05919 0.00102 -0.00699 -0.00565 AFIX 3 H7CA 2 0.478907 0.822485 0.392673 11.00000 -1.20000 H7CB 2 0.476637 0.863765 0.465543 11.00000 -1.20000 AFIX 0 C5BA 1 0.455287 0.705059 0.576651 11.00000 0.04286 0.04778 = 0.09036 -0.02200 -0.01565 -0.01470 AFIX 13 H5BA 2 0.477795 0.650625 0.595583 11.00000 -1.20000 AFIX 0 C7BA 1 0.157565 0.242983 0.589989 11.00000 0.05264 0.12865 = 0.07231 0.05186 0.00653 -0.01202 AFIX 3 H7BA 2 0.204335 0.285153 0.591439 11.00000 -1.20000 H7BB 2 0.178135 0.192503 0.565209 11.00000 -1.20000 AFIX 0 C9BA 1 0.394086 0.928797 0.398817 11.00000 0.13522 0.03689 = 0.07247 -0.00039 -0.04224 0.03318 AFIX 3 H9BA 2 0.360386 0.957997 0.433747 11.00000 -1.20000 H9BB 2 0.437426 0.968887 0.381557 11.00000 -1.20000 AFIX 0 C1CA 1 0.379496 0.777030 0.448466 11.00000 0.03232 0.04647 = 0.06016 0.01067 0.00243 0.00255 AFIX 13 H1CA 2 0.344103 0.802238 0.484952 11.00000 -1.20000 AFIX 0 C3CA 1 0.134080 0.155400 0.424715 11.00000 0.07775 0.07101 = 0.07449 0.00379 0.01235 0.00299 AFIX 3 H3CA 2 0.088350 0.160230 0.390905 11.00000 -1.20000 H3CB 2 0.108200 0.135500 0.466955 11.00000 -1.20000 AFIX 0 C0BA 1 0.030965 0.362204 0.421342 11.00000 0.06429 0.06155 = 0.07164 0.00538 0.00466 -0.00687 AFIX 13 H0BA 2 0.055343 0.363657 0.375230 11.00000 -1.20000 AFIX 0 C6DA 1 0.214934 0.277483 0.367050 11.00000 0.07552 0.07075 = 0.07274 0.00605 0.01249 0.00175 AFIX 3 H6DA 2 0.169334 0.279713 0.332970 11.00000 -1.20000 H6DB 2 0.237844 0.335813 0.372320 11.00000 -1.20000 AFIX 0 C7DA 1 0.539859 0.662455 0.447027 11.00000 0.06014 0.03710 = 0.07188 0.02050 0.00281 0.01164 AFIX 13 H7DA 2 0.574246 0.715955 0.449102 11.00000 -1.20000 AFIX 0 C8DA 1 0.535344 0.785691 0.670901 11.00000 0.12997 0.15110 = 0.04503 -0.00160 0.01613 -0.08748 AFIX 3 H8DA 2 0.565984 0.734151 0.686051 11.00000 -1.20000 H8DB 2 0.572694 0.835271 0.679411 11.00000 -1.20000 AFIX 0 C9DA 1 0.132385 0.217385 0.664512 11.00000 0.11392 0.05957 = 0.05836 -0.01515 -0.01142 0.01856 AFIX 3 H9DA 2 0.089745 0.171065 0.662682 11.00000 -1.20000 H9DB 2 0.183735 0.194905 0.687052 11.00000 -1.20000 AFIX 0 C0EA 1 0.666880 0.552646 0.373318 11.00000 0.05125 0.15304 = 0.07876 -0.01552 0.00577 0.06198 AFIX 3 H0EA 2 0.635900 0.498016 0.369558 11.00000 -1.20000 H0EB 2 0.723820 0.545136 0.352958 11.00000 -1.20000 AFIX 0 C3BA 1 0.523246 0.775004 0.593722 11.00000 0.07991 0.07449 = 0.05358 -0.01518 0.01556 -0.04399 AFIX 3 H3BA 2 0.577666 0.764014 0.570331 11.00000 -1.20000 H3BB 2 0.499216 0.828954 0.576571 11.00000 -1.20000 AFIX 0 C4CA 1 0.210122 0.095035 0.405346 11.00000 0.07894 0.07225 = 0.07581 0.00523 0.01216 0.00217 AFIX 3 H4CA 2 0.252472 0.084765 0.441036 11.00000 -1.20000 H4CB 2 0.182402 0.040255 0.394196 11.00000 -1.20000 AFIX 0 C8CA 1 -0.006468 0.447472 0.430705 11.00000 0.07504 0.07258 = 0.08575 0.00374 0.00034 -0.00670 AFIX 3 H8CA 2 0.039002 0.490162 0.437705 11.00000 -1.20000 H8CB 2 -0.042058 0.446462 0.471465 11.00000 -1.20000 AFIX 0 C9CA 1 0.368209 0.722131 0.613426 11.00000 0.05096 0.10205 = 0.05437 -0.02656 -0.01307 -0.00238 AFIX 23 H9CA 2 0.327250 0.675791 0.604013 11.00000 -1.20000 H9CB 2 0.343165 0.776681 0.598398 11.00000 -1.20000 AFIX 0 C0DA 1 0.527444 0.638070 0.370127 11.00000 0.05132 0.08382 = 0.04280 -0.00786 -0.00370 0.02254 AFIX 3 H0DA 2 0.492094 0.586060 0.367227 11.00000 -1.20000 H0DB 2 0.498143 0.684350 0.345707 11.00000 -1.20000 AFIX 0 C1DA 1 0.315515 0.750511 0.392384 11.00000 0.04585 0.05420 = 0.09076 0.03236 -0.02895 -0.00040 AFIX 3 H1DA 2 0.272255 0.711380 0.411034 11.00000 -1.20000 H1DB 2 0.347195 0.719530 0.357214 11.00000 -1.20000 AFIX 0 PART 2 C2 1 0.375825 0.453357 0.636264 -21.00000 0.05268 0.05347 = 0.05411 0.00094 0.00188 0.00004 AFIX 3 H2A 2 0.400175 0.496897 0.666464 -21.00000 -1.20000 H2B 2 0.419335 0.438167 0.602544 -21.00000 -1.20000 AFIX 0 PART 0 C3DA 1 0.678740 0.577403 0.449872 11.00000 0.06778 0.10707 = 0.06137 0.01915 0.00465 0.01901 AFIX 3 H3DA 2 0.715400 0.628453 0.453562 11.00000 -1.20000 H3DB 2 0.707590 0.530093 0.473352 11.00000 -1.20000 AFIX 0 C5DA 1 0.389573 0.725740 0.690600 11.00000 0.06364 0.11203 = 0.04351 0.01132 -0.01164 -0.01853 AFIX 3 H5DA 2 0.410483 0.668980 0.704390 11.00000 -1.20000 H5DB 2 0.336713 0.737990 0.715710 11.00000 -1.20000 AFIX 0 C0CA 1 0.098262 0.287550 0.703112 11.00000 0.16735 0.08665 = 0.04294 -0.00725 -0.02610 0.04097 AFIX 3 H0CA 2 0.143312 0.330730 0.710112 11.00000 -1.20000 H0CB 2 0.080362 0.266170 0.747432 11.00000 -1.20000 AFIX 0 C5AA 1 0.619862 0.624757 0.339988 11.00000 0.07946 0.09583 = 0.06273 0.00443 0.02374 0.01492 AFIX 3 H5AA 2 0.612722 0.607117 0.292858 11.00000 -1.20000 H5AB 2 0.653332 0.678167 0.340538 11.00000 -1.20000 AFIX 0 C0AA 1 0.459009 0.794563 0.709667 11.00000 0.14765 0.07338 = 0.04942 -0.00897 -0.00288 -0.06698 AFIX 3 H0AA 2 0.434539 0.851733 0.701607 11.00000 -1.20000 H0AB 2 0.473879 0.790703 0.757617 11.00000 -1.20000 AFIX 0 O10 5 0.179113 0.397922 0.486895 11.00000 0.07755 0.08632 = 0.08797 0.01212 -0.01674 -0.02348 C11 1 0.146696 0.600873 0.709089 11.00000 0.12423 0.13411 = 0.11106 0.00923 0.00956 0.02136 AFIX 3 H11A 2 0.170896 0.655282 0.725289 11.00000 -1.20000 H11B 2 0.125276 0.610753 0.663249 11.00000 -1.20000 AFIX 0 C12 1 0.037316 0.358815 0.595573 11.00000 0.12536 0.08861 = 0.04057 -0.01479 0.01699 0.06633 AFIX 3 H12A 2 0.076176 0.408435 0.596033 11.00000 -1.20000 H12B 2 -0.015824 0.376135 0.572713 11.00000 -1.20000 AFIX 0 C15 1 0.175207 0.245719 0.435289 11.00000 0.06640 0.06239 = 0.06808 0.00655 0.00873 -0.00395 AFIX 13 H15 2 0.225042 0.235662 0.465324 11.00000 -1.20000 AFIX 0 C20 1 -0.064804 0.476575 0.373518 11.00000 0.07607 0.07191 = 0.08833 0.00322 -0.00067 -0.00473 AFIX 3 H20A 2 -0.082634 0.536735 0.378018 11.00000 -1.20000 H20B 2 -0.035604 0.468365 0.330228 11.00000 -1.20000 AFIX 0 C4 1 0.284954 0.217305 0.341876 11.00000 0.07772 0.07295 = 0.07343 0.00546 0.01151 0.00118 AFIX 3 H4A 2 0.333104 0.217025 0.373766 11.00000 -1.20000 H4B 2 0.305964 0.237115 0.297966 11.00000 -1.20000 AFIX 0 C7 1 0.249389 0.127427 0.336041 11.00000 0.07614 0.06979 = 0.07209 0.00530 0.01262 0.00288 AFIX 3 H7A 2 0.295359 0.087857 0.322671 11.00000 -1.20000 H7B 2 0.207309 0.128397 0.299251 11.00000 -1.20000 AFIX 0 C1 1 -0.048846 0.303607 0.415275 11.00000 0.07481 0.07187 = 0.08523 0.00476 -0.00266 -0.00645 AFIX 3 H1A 2 -0.084876 0.312217 0.455245 11.00000 -1.20000 H1B 2 -0.033896 0.242477 0.412675 11.00000 -1.20000 AFIX 0 C3 1 0.016134 0.332498 0.665740 11.00000 0.11791 0.11708 = 0.10444 -0.00031 0.01629 0.00927 AFIX 3 H3A 2 -0.032296 0.292168 0.665610 11.00000 -1.20000 H3B 2 -0.001346 0.383588 0.691210 11.00000 -1.20000 AFIX 0 C9 1 -0.138456 0.412265 0.371211 11.00000 0.07385 0.07160 = 0.08765 0.00259 -0.00119 -0.00451 AFIX 3 H9A 2 -0.154035 0.405095 0.418781 11.00000 -1.20000 H9B 2 -0.188936 0.431415 0.345731 11.00000 -1.20000 AFIX 0 C13 1 -0.099608 0.329601 0.349500 11.00000 0.07456 0.07320 = 0.08634 0.00271 -0.00101 -0.00603 AFIX 3 H13A 2 -0.062088 0.340711 0.310760 11.00000 -1.20000 H13B 2 -0.143778 0.287391 0.337350 11.00000 -1.20000 AFIX 0 PART 2 C6 1 0.349845 0.375177 0.671309 -21.00000 0.09192 0.10206 = 0.13341 -0.01953 -0.05297 -0.01668 AFIX 3 H6A 2 0.309825 0.341107 0.644989 -21.00000 -1.50000 H6B 2 0.322645 0.392787 0.713099 -21.00000 -1.50000 H6C 2 0.400465 0.341097 0.681369 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C21 1 0.355992 0.424015 0.633830 21.00000 0.05268 0.05347 = 0.05411 0.00094 0.00188 0.00004 AFIX 3 H21A 2 0.377972 0.378265 0.604540 21.00000 -1.20000 H21B 2 0.320982 0.397045 0.669080 21.00000 -1.20000 AFIX 0 C5 1 0.425843 0.471851 0.668505 21.00000 0.09192 0.10206 = 0.13341 -0.01953 -0.05297 -0.01668 AFIX 3 H5A 2 0.419773 0.533391 0.662165 21.00000 -1.50000 H5B 2 0.479043 0.452591 0.647915 21.00000 -1.50000 H5C 2 0.426913 0.458871 0.716345 21.00000 -1.50000 AFIX 0 PART 0 C8 1 0.072491 0.582289 0.751404 11.00000 0.16490 0.16970 = 0.16493 0.00315 0.00217 0.00145 AFIX 3 H8A 2 0.027531 0.556629 0.724104 11.00000 -1.50000 H8B 2 0.050561 0.633669 0.773114 11.00000 -1.50000 H8C 2 0.090971 0.541559 0.785454 11.00000 -1.50000 AFIX 0 HKLF 4 REM a in P212121 #19 REM R1 = 0.0612 for 5823 Fo > 4sig(Fo) and 0.0800 for all 7796 data REM 459 parameters refined using 365 restraints END WGHT 0.0417 0.0000 REM Highest difference peak 1.854, deepest hole -0.873, 1-sigma level 0.109 Q1 1 0.6164 0.8276 0.5219 11.00000 0.05 0.71 Q2 1 0.2283 0.4433 0.4774 11.00000 0.05 0.65 Q3 1 0.2170 0.3751 0.4728 11.00000 0.05 0.63 Q4 1 0.1706 0.4371 0.5174 11.00000 0.05 0.63 Q5 1 0.1749 0.4396 0.4417 11.00000 0.05 0.62 Q6 1 -0.0250 0.4358 0.3228 11.00000 0.05 0.60 Q7 1 0.2281 0.5588 0.4770 11.00000 0.05 0.59 Q8 1 -0.1074 0.4175 0.3304 11.00000 0.05 0.56 Q9 1 0.1596 0.5676 0.5055 11.00000 0.05 0.56 Q10 1 0.1783 0.6353 0.5228 11.00000 0.05 0.55 Q11 1 0.0776 0.1524 0.4143 11.00000 0.05 0.54 Q12 1 0.0470 0.3970 0.3488 11.00000 0.05 0.54 Q13 1 -0.0653 0.3382 0.4469 11.00000 0.05 0.53 Q14 1 0.2065 0.6201 0.4689 11.00000 0.05 0.53 Q15 1 0.1771 0.5599 0.4429 11.00000 0.05 0.52 Q16 1 0.2832 0.5751 0.5065 11.00000 0.05 0.47 Q17 1 0.2786 0.4252 0.5049 11.00000 0.05 0.46 Q18 1 0.2811 0.1436 0.3447 11.00000 0.05 0.44 Q19 1 0.1065 0.0798 0.3781 11.00000 0.05 0.44 Q20 1 0.2195 0.2247 0.3606 11.00000 0.05 0.43 ; _shelx_res_checksum 51007 _shelx_hkl_file ; 0 0 3 0.70 2.80 0 0 3 1.65 1.35 0 0 -4 115.32 17.28 0 0 4 114.61 16.97 0 0 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73.47 21.86 3 12 -13 77.56 29.27 12 -3 -13 86.91 23.25 -12 3 -13 92.21 30.17 -12 3 -14 32.14 16.36 3 12 -14 42.94 20.89 -12 3 -15 33.76 18.99 3 12 -15 27.21 17.54 3 12 -16 17.47 13.73 -12 3 -16 20.26 13.49 3 12 -17 8.29 9.49 -12 3 -17 14.82 12.12 3 12 -18 6.95 8.70 -12 3 -18 3.39 5.80 -12 3 -19 19.36 13.65 3 12 -19 4.03 6.63 -12 3 -20 -10.76 10.42 -12 -4 -19 19.93 14.41 12 4 -18 11.86 11.84 -4 12 -18 1.18 3.21 12 4 -17 31.66 18.54 -4 12 -17 31.32 16.65 12 4 -16 13.02 10.09 -4 12 -16 25.29 14.98 12 4 -15 22.09 14.05 -4 12 -15 46.34 20.63 12 4 -14 -3.46 5.97 -4 12 -14 16.18 11.95 4 -12 -14 29.01 17.89 12 4 -13 34.18 18.49 -4 12 -13 26.04 15.53 4 -12 -13 -1.17 3.51 12 4 -12 5.33 2.76 -4 12 -12 17.14 12.18 4 -12 -12 13.02 13.44 12 4 -11 3.04 6.91 -4 12 -11 4.47 3.88 4 -12 -11 17.53 12.09 12 4 -10 4.43 6.30 -4 12 -10 1.92 2.97 4 -12 -10 6.85 6.48 12 4 -9 35.93 17.58 4 -12 -9 68.53 27.08 12 4 -8 16.21 11.03 4 -12 -8 15.67 11.98 12 4 -7 75.27 24.65 -4 -12 7 111.37 21.59 4 -12 -7 104.24 33.40 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118.69 31.91 -12 -4 6 88.66 20.88 12 -4 -7 86.11 25.18 4 12 -7 101.47 31.72 -12 4 -7 62.33 23.32 -12 -4 7 73.05 17.81 12 -4 -8 23.93 11.87 4 12 -8 44.76 21.57 -12 4 -8 42.66 19.99 -12 4 -9 51.73 23.49 4 12 -9 64.06 26.67 12 -4 -9 45.22 17.92 -12 4 -10 9.38 3.37 4 12 -10 -4.04 6.40 12 -4 -10 11.96 9.42 -12 4 -11 6.59 8.02 4 12 -11 13.91 10.12 12 -4 -11 1.79 0.50 -12 4 -12 8.42 8.85 4 12 -12 8.33 11.69 12 -4 -12 0.18 2.51 4 12 -13 33.87 18.94 -12 4 -13 7.67 7.67 12 -4 -13 20.75 12.58 4 12 -14 27.42 17.60 12 -4 -14 21.90 12.54 -12 4 -14 30.23 17.71 4 12 -15 43.10 22.49 -12 4 -15 16.78 13.43 -12 4 -16 9.55 6.40 4 12 -16 20.22 14.89 -12 4 -17 35.22 19.71 4 12 -17 28.74 17.40 4 12 -18 -0.36 2.01 -12 4 -18 13.59 11.29 4 12 -19 34.03 19.83 -12 4 -19 25.86 17.19 -12 4 -20 8.52 9.20 12 5 -18 41.21 21.91 -5 12 -18 23.22 13.84 -12 -5 -18 39.49 21.11 12 5 -17 41.32 21.01 -5 12 -17 23.21 13.95 -12 -5 -17 27.47 18.06 12 5 -16 20.65 14.98 -5 12 -16 41.58 18.93 -12 -5 -16 6.75 8.36 12 5 -15 88.99 31.19 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105.30 30.79 -13 -5 6 93.14 22.14 13 -5 -7 133.75 32.21 5 13 -7 90.40 32.06 -13 5 -7 124.60 33.89 13 -5 -8 81.87 24.51 5 13 -8 43.03 21.63 -13 5 -8 49.73 22.05 13 -5 -9 37.09 16.41 5 13 -9 47.43 22.00 -13 5 -9 49.50 21.22 -13 5 -10 10.22 11.15 5 13 -10 39.34 20.69 13 -5 -10 17.46 12.32 -13 5 -11 7.30 8.74 5 13 -11 8.37 8.79 13 -5 -11 7.04 7.38 -13 5 -12 -0.19 6.90 5 13 -12 2.89 5.62 13 -5 -12 1.31 6.70 -13 5 -13 2.84 6.55 5 13 -13 16.78 11.90 13 -5 -13 6.16 6.82 5 13 -14 17.97 14.33 -13 5 -14 17.99 14.15 5 13 -15 51.09 24.00 -13 5 -15 21.62 14.57 5 13 -16 6.46 1.88 -13 5 -16 16.78 14.18 -13 5 -17 36.43 19.41 5 13 -17 30.67 18.58 -13 5 -18 30.69 18.93 13 6 -16 45.62 22.31 -13 -6 -16 46.37 22.39 13 6 -15 46.43 22.27 -6 13 -15 60.73 22.81 6 -13 -15 46.83 23.35 -13 -6 -15 66.10 26.89 13 6 -14 55.59 24.04 -6 13 -14 20.05 12.88 6 -13 -14 40.25 20.87 -13 -6 -14 46.30 21.89 13 6 -13 101.96 33.11 -6 13 -13 81.63 25.40 -13 -6 -13 110.71 33.92 6 -13 -13 95.38 32.18 13 6 -12 124.01 34.95 -6 13 -12 80.20 26.65 -13 -6 -12 82.53 29.56 6 -13 -12 46.47 22.53 -6 13 -11 143.73 35.28 -13 -6 -11 182.41 43.74 6 -13 -11 155.47 41.31 13 6 -11 183.59 42.57 13 6 -10 126.84 34.82 -13 -6 -10 120.38 35.27 6 -13 -10 66.95 27.46 -13 -6 -9 189.81 44.27 6 -13 -9 200.10 46.75 13 6 -9 177.06 40.85 13 6 -8 101.68 29.95 -13 -6 -8 93.10 29.79 6 -13 -8 45.91 23.47 13 6 -7 113.91 30.97 -13 -6 -7 130.57 35.36 6 -13 -7 184.92 44.75 13 6 -6 108.17 29.83 -13 -6 -6 72.48 26.32 6 -13 -6 58.46 24.93 6 -13 -5 106.17 33.24 13 6 -5 71.56 23.56 -13 -6 -5 107.35 30.85 6 -13 -4 32.24 18.11 13 6 -4 66.95 21.32 -13 -6 -4 60.96 23.59 6 -13 -3 54.42 23.06 13 6 -3 69.92 21.97 -13 -6 -3 74.97 25.44 6 -13 -2 15.02 12.08 13 6 -2 36.27 15.18 -13 -6 -2 34.08 16.37 13 6 -1 13.10 8.80 6 -13 -1 20.80 14.00 -13 -6 -1 16.67 11.49 13 6 0 42.22 15.23 6 -13 0 25.27 15.53 -13 -6 0 42.62 17.58 13 6 1 8.47 7.27 -13 -6 1 11.07 9.00 13 6 2 22.49 10.16 6 -13 2 24.35 14.05 -13 -6 2 38.76 16.41 -13 6 -3 94.65 28.29 6 -13 3 52.21 22.33 13 -6 -3 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14.23 -17 -10 -3 11.34 10.26 -17 -10 -2 29.41 15.86 -17 -10 -1 -1.06 3.06 17 -10 1 18.11 13.59 -17 -10 0 7.39 7.97 -17 10 0 -1.42 3.53 17 -10 0 13.99 12.02 10 17 0 -5.54 7.22 17 -10 -1 17.61 13.46 -17 10 -1 3.29 5.41 10 17 -1 1.12 3.28 17 -10 -2 18.07 12.57 -17 10 -2 11.96 9.87 10 17 -2 7.48 8.58 17 -10 -3 7.48 8.70 10 17 -3 11.96 10.92 17 -10 -4 16.74 12.32 17 -10 -5 16.98 11.96 17 -10 -6 -4.10 6.38 17 -10 -7 4.95 6.95 17 -10 -8 13.31 11.41 17 -10 -9 7.48 8.57 -17 -11 -3 25.95 15.71 -17 -11 -2 56.90 23.00 11 17 2 16.34 12.06 11 17 1 53.01 21.94 11 17 0 37.68 19.43 11 17 -1 59.92 24.42 11 17 -2 14.27 11.71 12 17 1 0.14 1.10 12 17 0 26.92 15.62 -18 0 0 248.06 44.69 0 -18 0 255.91 48.61 -18 0 -1 0.31 5.86 -18 0 1 4.87 6.12 0 -18 -1 -4.34 6.29 0 -18 1 -3.63 5.64 -18 0 -2 240.63 45.63 0 -18 -2 215.43 45.60 -18 0 2 229.64 41.83 0 -18 2 222.06 44.01 -18 0 -3 6.65 8.02 0 -18 -3 2.50 4.86 0 -18 3 9.63 8.96 -18 0 -4 182.52 41.22 0 -18 -4 173.63 41.48 0 -18 4 188.27 39.30 -18 0 -5 -10.61 9.89 0 -18 -5 -4.99 6.97 0 -18 5 2.18 4.13 -18 0 -6 98.79 31.05 0 -18 -6 85.87 29.06 -18 0 -7 11.46 10.57 0 -18 -7 -0.13 1.13 0 -18 -8 31.85 18.08 -18 0 -8 28.95 16.13 0 18 -9 9.57 10.15 0 -18 -9 -11.74 11.13 -18 0 -9 -0.36 6.64 18 1 -13 6.62 7.79 18 1 -12 89.58 28.55 -1 18 -10 93.22 31.77 1 -18 -9 16.84 13.38 -18 -1 -9 -16.68 13.19 -18 -1 -8 111.60 33.77 1 -18 -8 124.16 36.29 -18 -1 -7 -7.91 8.87 1 -18 -7 8.30 9.22 1 -18 -6 100.33 32.60 -18 -1 -6 78.66 28.14 -18 -1 -5 1.25 3.45 1 -18 -5 4.41 6.68 -18 -1 -4 57.73 23.54 1 -18 -4 87.78 29.63 -18 -1 -3 3.06 4.82 1 -18 -3 5.11 6.90 -1 -18 3 7.74 7.84 -18 -1 -2 21.88 14.98 -18 1 2 40.11 17.43 1 -18 -2 18.12 13.03 -1 -18 2 17.56 11.94 -18 -1 -1 13.00 10.38 -18 1 1 7.35 7.46 -1 -18 1 3.85 5.66 1 -18 -1 4.45 6.48 -18 -1 0 25.92 15.02 -18 1 0 7.37 7.62 -1 -18 0 8.02 8.30 1 -18 0 16.96 12.53 -18 1 -1 -2.27 4.29 1 -18 1 -3.58 5.70 -18 -1 1 1.08 4.09 -18 1 -2 13.19 11.11 1 -18 2 9.07 8.97 -18 1 -3 14.84 11.35 -1 -18 -3 9.87 8.82 1 -18 3 7.76 8.15 1 -18 4 77.31 25.80 -1 -18 -4 30.65 16.80 -18 1 -4 33.60 17.76 1 -18 5 17.93 12.05 -1 -18 -5 0.12 1.06 -18 1 -5 11.52 10.26 1 -18 6 96.28 27.95 -1 -18 -6 126.55 35.31 -18 1 -6 68.17 24.88 -1 -18 -7 8.06 8.96 -18 1 -7 17.93 13.09 -18 1 -8 108.16 32.68 -1 -18 -8 98.67 31.67 -18 1 -9 -2.59 3.20 1 18 -9 11.57 15.16 18 2 -13 -3.44 5.64 18 2 -12 11.29 10.05 -2 18 -10 11.49 10.97 2 -18 -9 -15.96 13.08 2 -18 -8 28.68 16.71 2 -18 -7 -16.56 13.27 2 -18 -6 42.99 21.59 2 -18 -5 21.97 15.09 2 -18 -4 78.71 28.68 2 -18 -3 32.91 19.32 -18 2 2 92.75 26.57 -2 -18 2 111.01 29.73 2 -18 -2 120.16 35.56 -18 2 1 12.99 9.93 -2 -18 1 10.56 9.16 2 -18 -1 19.01 13.04 -18 2 0 117.87 30.99 -2 -18 0 83.05 26.07 2 -18 0 119.90 34.76 -18 2 -1 21.93 13.89 -2 -18 -1 18.87 12.59 2 -18 1 12.40 10.74 2 -18 2 128.83 34.77 -18 2 -2 126.87 33.01 -2 -18 -2 90.09 27.66 2 -18 3 13.33 10.85 -18 2 -3 6.31 7.39 -2 -18 -3 14.30 11.15 2 -18 4 107.50 30.22 -18 2 -4 114.16 32.63 -2 -18 -4 110.24 31.94 -18 2 -5 1.67 3.90 -2 -18 -5 -2.66 4.95 2 -18 6 68.99 24.50 -18 2 -6 67.73 25.32 -2 -18 -6 56.26 23.88 2 -18 7 9.16 8.65 -18 2 -7 -2.06 4.44 2 -18 8 25.14 14.22 2 18 -8 44.34 22.22 -18 2 -8 26.10 17.36 -18 2 -9 6.23 7.84 18 3 -13 -1.32 3.49 -3 18 -10 36.87 19.48 3 -18 -8 37.69 20.33 3 -18 -7 7.96 9.30 3 -18 -6 38.95 20.47 3 -18 -5 4.88 5.62 3 -18 -4 39.99 20.45 3 -18 -3 11.72 10.88 -18 3 3 -1.78 3.53 3 -18 -2 11.69 10.91 -18 3 2 7.03 6.71 -18 3 1 -2.40 4.27 3 -18 -1 -6.97 8.38 -3 -18 0 -11.04 9.20 -18 3 0 -5.03 6.29 3 -18 0 -9.39 9.58 3 -18 1 -6.05 7.59 -3 -18 -1 -12.60 9.98 -18 3 -1 2.20 3.08 3 -18 2 9.17 9.22 -3 -18 -2 19.10 12.50 -18 3 -2 7.54 7.93 3 -18 3 10.44 9.71 -3 -18 -3 8.13 8.33 -18 3 -3 0.22 4.90 3 -18 4 13.64 11.01 -3 -18 -4 26.97 15.42 -18 3 -4 20.42 13.42 -18 3 -5 1.54 3.73 3 -18 5 11.91 10.23 -18 3 -6 45.52 20.58 3 -18 6 34.32 18.37 -18 3 -7 9.91 9.54 3 -18 7 16.44 11.89 3 -18 8 22.34 13.80 3 18 -8 6.66 8.78 3 -18 9 15.60 12.59 -4 18 -11 8.36 1.76 4 -18 -7 18.97 14.49 4 -18 -6 24.27 16.33 4 -18 -5 42.92 21.55 4 -18 -4 62.55 25.64 -18 4 3 21.60 12.05 4 -18 -3 52.97 23.83 -18 4 2 71.85 23.74 4 -18 -2 38.82 20.18 -18 4 1 6.08 6.84 4 -18 -1 60.32 24.81 4 -18 0 65.75 26.74 -18 4 0 59.41 22.11 4 -18 1 64.27 25.78 -18 4 -1 26.45 15.34 4 -18 2 45.60 20.80 18 -4 -2 80.72 25.35 -18 4 -2 54.41 21.90 -4 -18 -2 36.43 17.08 4 -18 3 45.54 20.02 -18 4 -3 12.96 10.07 4 -18 4 37.16 19.09 -18 4 -4 45.83 20.74 4 -18 5 49.06 20.75 -18 4 -5 25.86 15.32 4 -18 6 4.34 6.28 -18 4 -6 62.54 24.67 4 -18 7 17.09 12.39 4 18 -7 14.11 12.42 -18 4 -7 7.60 8.47 4 -18 8 23.57 14.40 -18 4 -8 6.52 8.03 4 -18 9 2.33 4.48 4 -18 10 3.64 5.55 -5 18 -11 33.49 15.61 5 -18 -6 36.27 20.51 5 -18 -5 21.38 14.68 5 -18 -4 34.55 19.82 -18 5 3 3.75 5.21 5 -18 -3 40.07 21.03 -18 5 2 17.53 11.04 -18 -5 -2 12.43 10.30 5 -18 -2 1.26 3.65 5 -18 -1 28.79 17.03 -18 5 1 18.27 12.07 -18 -5 -1 15.45 11.29 5 -18 0 -1.59 4.01 -18 5 0 7.33 7.67 -18 -5 0 8.08 4.85 5 -18 1 24.76 15.65 -18 5 -1 10.29 9.23 -18 -5 1 5.50 6.51 5 -18 2 10.72 10.23 -18 5 -2 20.91 14.53 18 -5 -2 3.61 4.64 5 -18 3 29.83 17.00 -18 5 -3 13.24 10.74 18 -5 -3 3.34 5.29 5 -18 4 26.97 15.56 -18 5 -4 35.70 19.72 5 -18 5 32.10 16.80 -18 5 -5 12.18 10.82 5 -18 6 13.59 11.32 -18 5 -6 47.01 21.25 5 18 -6 12.23 11.50 5 -18 7 35.62 17.24 -18 5 -7 10.04 10.36 5 -18 8 35.93 17.50 5 -18 9 22.10 14.05 5 -18 10 22.08 13.95 5 -18 11 31.24 16.50 5 -18 12 40.83 18.79 -6 18 -11 14.22 10.78 -18 -6 -7 22.62 14.87 -18 -6 -6 46.43 21.00 -18 -6 -5 23.16 15.02 6 -18 -5 45.04 24.24 -18 -6 -4 123.00 33.92 6 -18 -4 77.98 29.94 -18 -6 -3 26.12 15.36 6 -18 -3 36.94 20.18 -18 6 3 14.55 10.07 6 -18 -2 67.73 27.34 -18 -6 -2 167.43 38.74 -18 6 2 155.52 34.89 -18 6 1 32.16 15.98 6 -18 -1 46.61 22.16 -18 -6 -1 20.60 13.70 -18 6 0 95.03 28.31 6 -18 0 91.06 30.88 -18 -6 0 105.85 30.01 -18 6 -1 20.98 13.28 18 -6 -1 14.88 11.47 -18 6 -2 127.03 33.91 6 -18 2 80.21 28.71 18 -6 -2 96.49 29.70 -18 6 -3 16.09 11.94 6 -18 3 41.21 20.34 18 -6 -3 28.21 15.73 -18 6 -4 113.70 32.84 6 -18 4 87.84 29.77 18 -6 -4 89.35 27.60 -18 6 -5 10.61 9.88 6 -18 5 23.38 15.23 6 18 -5 38.62 20.88 6 -18 6 37.05 18.95 -18 6 -6 44.35 20.67 6 -18 7 29.22 17.24 6 -18 8 14.95 11.83 6 -18 9 -4.36 6.35 6 -18 10 -4.83 6.65 -18 -7 -6 37.92 19.25 -18 -7 -5 4.74 3.33 -18 -7 -4 24.34 15.13 -18 -7 -3 1.37 3.54 -18 7 3 8.55 8.41 7 -18 -2 46.22 20.77 -18 -7 -2 22.49 14.28 -18 7 2 20.57 12.72 7 -18 -1 6.29 8.17 -18 -7 -1 -4.89 6.48 -18 7 1 4.76 6.21 7 -18 0 8.18 9.26 -18 -7 0 1.74 3.79 -18 7 0 22.02 14.16 7 -18 1 2.11 4.69 18 -7 -1 4.31 6.33 -18 7 -1 8.00 8.27 7 -18 2 26.30 16.53 18 -7 -2 25.71 15.44 -18 7 -2 21.50 13.83 7 -18 3 -1.62 4.09 18 -7 -3 -1.27 3.39 -18 7 -3 5.10 7.45 7 -18 4 7.99 9.07 18 -7 -4 23.94 13.41 -18 7 -4 27.24 15.76 -18 7 -5 8.65 8.96 18 -7 -5 -5.73 7.19 7 -18 6 35.66 19.67 7 -18 7 45.27 20.45 -18 -8 -5 13.30 11.34 -18 -8 -4 53.53 22.47 -18 8 3 23.73 13.58 -18 -8 -3 21.65 14.37 -18 8 2 86.39 26.30 -18 -8 -2 60.46 23.14 -18 8 1 13.90 10.71 -18 -8 -1 29.25 15.22 18 -8 0 51.78 23.94 -18 8 0 71.64 24.73 18 -8 -1 37.27 19.04 -18 8 -1 22.99 13.84 18 -8 -2 79.26 27.20 -18 8 -2 67.47 24.50 18 -8 -3 17.74 12.94 -18 8 -3 23.87 14.72 18 -8 -4 50.82 21.86 18 -8 -5 19.97 11.42 18 -8 -6 44.90 20.32 -18 -9 -4 17.33 12.77 -18 9 3 8.26 8.07 -18 -9 -3 -2.06 4.33 -18 9 2 9.49 8.78 -18 -9 -2 -0.94 2.88 18 -9 1 -4.22 6.47 -18 9 1 -4.10 5.85 -18 -9 -1 12.47 10.35 18 -9 0 3.96 9.23 -18 9 0 -9.75 9.13 18 -9 -1 0.03 5.21 -18 9 -1 3.33 5.41 18 -9 -2 7.00 8.30 18 -9 -3 2.90 5.33 18 -9 -4 -6.58 8.01 18 -9 -5 6.84 8.14 18 -9 -6 3.99 6.17 18 -9 -7 27.24 15.96 -18 10 3 2.29 1.15 -18 -10 -2 60.24 23.34 -18 10 2 61.55 22.82 -19 0 0 10.26 9.12 0 -19 0 -24.23 14.78 -19 0 1 1.96 3.93 0 -19 -1 5.67 7.24 0 -19 1 17.25 12.32 -19 0 -1 3.03 5.05 0 -19 -2 1.45 3.68 -19 0 -2 20.82 13.46 0 -19 2 11.73 10.09 0 -19 -3 -10.77 10.15 -19 0 -3 -0.25 3.72 0 -19 3 3.28 5.25 0 -19 -4 46.56 20.98 -19 0 -4 37.67 18.73 0 -19 -5 0.32 5.05 -19 0 -5 -3.59 5.82 0 -19 -6 43.24 20.22 -19 0 -6 52.72 22.86 -19 0 -7 -1.27 3.54 0 -19 -7 3.08 5.58 1 -19 -7 2.64 5.21 -19 -1 -6 57.26 24.79 1 -19 -6 30.38 17.62 -19 -1 -5 2.08 4.48 1 -19 -5 1.29 3.64 -19 -1 -4 110.51 32.86 1 -19 -4 84.18 29.05 -19 -1 -3 8.91 8.35 1 -19 -3 13.24 11.43 1 -19 -2 112.63 33.57 -19 -1 -2 142.22 35.98 -1 -19 2 107.47 29.82 -19 1 1 1.48 3.37 -1 -19 1 1.61 3.70 1 -19 -1 -3.68 5.92 -19 -1 -1 5.92 2.41 -19 1 0 154.04 35.34 -1 -19 0 79.63 26.48 1 -19 0 121.77 33.84 -19 1 -1 7.59 7.90 -1 -19 -1 -11.23 9.97 1 -19 1 8.52 8.85 -19 1 -2 167.99 38.22 -1 -19 -2 115.56 32.87 1 -19 2 116.76 32.98 -19 1 -3 4.50 6.27 -1 -19 -3 -0.21 1.38 1 -19 3 2.65 4.82 -19 1 -4 122.16 33.36 -1 -19 -4 60.93 23.87 1 -19 4 93.89 29.02 1 -19 5 10.28 9.21 -19 1 -5 6.65 7.83 -1 -19 -5 3.23 5.55 -19 1 -6 70.21 25.74 -1 -19 -6 40.80 19.94 -1 -19 -7 -8.38 9.18 2 -19 -6 31.70 17.79 2 -19 -5 8.81 9.59 2 -19 -4 44.35 20.77 2 -19 -3 1.57 3.99 2 -19 -2 19.25 13.85 -19 2 1 -1.31 3.18 2 -19 -1 3.94 6.25 -19 2 0 15.33 11.08 -2 -19 0 3.25 5.18 2 -19 0 14.75 12.91 -19 2 -1 2.77 4.79 -2 -19 -1 -5.95 7.07 2 -19 1 5.48 7.22 -19 2 -2 14.30 11.05 -2 -19 -2 -7.92 8.24 2 -19 2 -8.04 8.65 -19 2 -3 13.60 10.98 -2 -19 -3 8.64 8.72 2 -19 3 19.86 13.39 2 -19 4 53.07 21.45 -19 2 -4 17.28 12.47 -2 -19 -4 28.86 16.18 2 -19 5 27.36 15.30 -19 2 -5 20.76 13.82 -2 -19 -5 13.81 11.38 2 -19 6 51.28 19.52 -19 2 -6 31.95 18.26 3 -19 -5 34.32 19.21 3 -19 -4 76.49 27.86 3 -19 -3 46.54 21.43 3 -19 -2 51.72 23.58 -19 3 1 14.59 11.68 3 -19 -1 32.33 18.10 -19 3 0 44.81 18.74 3 -19 0 46.94 21.98 -19 3 -1 14.39 10.87 3 -19 1 39.88 19.07 3 -19 2 105.23 31.87 -19 3 -2 35.10 18.84 -3 -19 -2 76.43 24.77 3 -19 3 36.64 18.36 -19 3 -3 3.61 6.96 -3 -19 -3 36.14 17.67 3 -19 4 81.76 26.74 -19 3 -4 33.91 17.38 3 -19 5 24.88 14.80 -19 3 -5 22.13 14.48 3 -19 6 47.01 19.91 3 -19 7 15.31 11.47 3 -19 8 11.53 9.89 4 -19 -4 36.84 19.93 4 -19 -3 34.00 18.87 4 -19 -2 28.38 18.75 -19 4 1 8.73 8.22 4 -19 -1 1.03 3.28 -19 4 0 9.19 8.58 4 -19 0 -3.37 5.85 4 -19 1 10.20 10.04 -19 4 -1 12.09 9.99 4 -19 2 24.57 14.56 -19 4 -2 26.82 15.09 4 -19 3 36.93 18.58 -19 4 -3 2.18 4.36 4 -19 4 30.58 16.85 -19 4 -4 21.44 13.92 4 -19 5 33.38 17.15 -19 4 -5 8.28 0.65 4 -19 6 43.06 20.14 4 -19 7 2.91 5.11 4 -19 8 29.75 16.26 4 -19 9 19.05 12.91 -19 -5 -4 57.12 23.15 -19 -5 -3 19.99 13.29 -19 5 2 71.61 23.93 -19 -5 -2 99.96 29.88 5 -19 -2 60.77 25.90 -19 5 1 39.12 17.52 -19 -5 -1 28.17 14.87 5 -19 -1 34.53 19.91 5 -19 0 57.46 24.31 -19 5 0 83.32 26.76 19 -5 -1 7.86 8.15 -19 5 -1 12.87 10.32 5 -19 2 43.20 22.12 -19 5 -2 61.88 23.03 5 -19 3 27.66 17.13 -19 5 -3 19.91 13.22 5 -19 4 47.19 21.30 -19 5 -4 47.32 21.01 5 -19 5 36.01 17.65 5 -19 6 34.17 17.96 5 -19 7 8.29 8.81 5 -19 8 7.37 8.25 -19 -6 -4 33.07 17.55 -19 -6 -3 -1.22 3.32 -19 6 2 -4.10 5.62 -19 -6 -2 23.00 14.23 -19 6 1 -11.20 9.44 -19 -6 -1 -4.86 6.44 -19 6 0 0.94 2.77 -19 6 -1 -6.50 7.39 19 -6 -1 -3.68 5.71 -19 6 -2 11.63 10.01 19 -6 -2 18.03 12.35 -19 6 -3 -5.14 6.73 -19 -7 -3 -0.86 2.81 -19 7 2 60.72 22.58 -19 -7 -2 53.36 21.71 -19 7 1 11.35 9.58 -19 7 0 68.15 23.80 19 -7 0 114.26 32.93 -19 7 -1 33.04 17.08 19 -7 -1 31.30 17.12 19 -7 -2 71.35 26.16 19 -7 -3 10.16 9.59 -19 8 2 4.86 6.24 -19 -8 -2 11.32 10.01 -19 8 1 1.11 3.02 19 -8 0 8.08 8.49 19 -8 -1 5.51 7.30 19 -8 -2 7.34 8.35 19 -8 -3 -10.61 9.98 19 -8 -4 -4.29 6.34 0 -20 0 80.21 27.03 0 -20 -1 13.68 11.23 0 -20 1 2.97 5.13 -20 0 -2 103.60 30.55 0 -20 -2 82.71 27.94 -20 0 -3 33.65 17.42 0 -20 -3 -1.19 3.38 -20 0 -4 66.29 24.81 0 -20 -4 46.73 21.18 1 -20 -3 -16.33 12.72 1 -20 -2 27.10 16.26 1 -20 -1 -9.09 9.34 -20 1 0 -5.10 6.46 -1 -20 0 5.56 6.96 1 -20 0 3.92 6.07 -20 1 -1 -6.62 7.44 -1 -20 -1 -1.77 3.97 1 -20 1 -0.33 1.74 -20 1 -2 17.38 12.25 -1 -20 -2 18.86 13.03 1 -20 2 2.62 4.87 -20 1 -3 -11.20 9.97 -1 -20 -3 -6.35 7.61 1 -20 3 2.27 4.49 -20 1 -4 21.00 13.80 -1 -20 -4 32.28 17.36 -1 -20 -5 -1.95 4.32 2 -20 -2 68.39 26.44 2 -20 -1 28.57 16.77 -20 2 0 52.45 20.95 2 -20 0 44.07 20.77 -20 2 -1 3.40 5.32 2 -20 1 29.73 16.84 -2 -20 -2 60.71 23.46 -20 2 -2 44.61 19.36 2 -20 2 62.05 24.02 -2 -20 -3 6.14 7.38 -20 2 -3 14.78 12.38 2 -20 3 27.88 16.00 -2 -20 -4 59.68 24.00 2 -20 4 51.79 21.97 -2 -20 -5 5.91 7.47 -20 3 0 3.49 5.31 3 -20 0 16.95 11.73 -20 3 -1 8.81 8.58 3 -20 1 34.85 18.57 -20 3 -2 6.67 7.51 3 -20 2 -7.86 8.72 -20 3 -3 21.60 13.81 3 -20 3 43.95 20.33 3 -20 4 54.32 22.26 3 -20 5 24.52 14.81 3 -20 6 43.15 19.37 -20 4 0 36.15 17.50 -20 4 -1 6.44 7.32 -20 4 -2 73.23 25.46 -20 -5 -3 1.93 4.13 -20 -5 -2 27.99 15.51 -20 5 0 12.47 10.88 -20 5 -1 6.21 7.20 20 -6 0 48.38 20.65 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 76693 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, 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 0.27856(3) 0.50218(4) 0.47921(2) 0.04342(11) Uani 1 1 d D . . . . P0AA P 0.43534(18) 0.68402(19) 0.48657(16) 0.0396(8) Uani 1 1 d . . . . . P6AA P 0.1177(2) 0.3268(2) 0.47321(18) 0.0534(7) Uani 1 1 d . U . . . Cl9A Cl 0.4036(3) 0.3892(2) 0.46273(18) 0.0760(12) Uani 1 1 d . . . . . Cl1B Cl 0.2386(3) 0.5299(2) 0.35026(16) 0.0746(12) Uani 1 1 d . . . . . Cl2B Cl 0.1663(2) 0.6143(3) 0.52713(19) 0.0946(13) Uani 1 1 d . . . . . O1AA O 0.2991(4) 0.4824(6) 0.5986(3) 0.059(3) Uani 1 1 d D . . . . H1AB H 0.2679 0.5066 0.6299 0.088 Uiso 0.446(18) 1 d DR . P A 2 H1AA H 0.2774 0.5212 0.6268 0.088 Uiso 0.554(18) 1 d DR . P A 1 O2AA O 0.2106(7) 0.5348(7) 0.7056(4) 0.105(4) Uani 1 1 d D U . . . H2AA H 0.2255 0.5150 0.7458 0.157 Uiso 1 1 d R . . . . C3AA C 0.2698(9) 0.8274(9) 0.3619(8) 0.075(5) Uani 1 1 d . . . . . H3AA H 0.2303 0.8526 0.3950 0.091 Uiso 1 1 d R . . . . H3AB H 0.2356 0.8084 0.3231 0.091 Uiso 1 1 d R . . . . C4AA C 0.5881(7) 0.5941(8) 0.4837(6) 0.053(4) Uani 1 1 d . . . . . H4AA H 0.5529 0.5418 0.4834 0.063 Uiso 1 1 d R . . . . H4AB H 0.5982 0.6103 0.5308 0.063 Uiso 1 1 d R . . . . O2CA O 0.3807(5) 0.6042(4) 0.4813(4) 0.0412(19) Uani 1 1 d . . . . . C5CA C 0.3366(9) 0.8981(8) 0.3379(7) 0.065(4) Uani 1 1 d . . . . . H5CA H 0.3051 0.9475 0.3197 0.078 Uiso 1 1 d R . . . . H5CB H 0.3721 0.8744 0.3016 0.078 Uiso 1 1 d R . . . . C6CA C 0.0811(9) 0.2841(9) 0.5543(6) 0.0606(10) Uani 1 1 d . U . . . H6CA H 0.0375 0.2390 0.5457 0.073 Uiso 1 1 calc R . . . . C7CA C 0.4408(8) 0.8467(7) 0.4271(6) 0.048(4) Uani 1 1 d . . . . . H7CA H 0.4789 0.8225 0.3927 0.058 Uiso 1 1 d R . . . . H7CB H 0.4766 0.8638 0.4655 0.058 Uiso 1 1 d R . . . . C5BA C 0.4553(8) 0.7051(9) 0.5767(7) 0.060(4) Uani 1 1 d . . . . . H5BA H 0.4778 0.6506 0.5956 0.072 Uiso 1 1 calc R . . . . C7BA C 0.1576(9) 0.2430(12) 0.5900(7) 0.085(6) Uani 1 1 d . . . . . H7BA H 0.2043 0.2852 0.5914 0.101 Uiso 1 1 d R . . . . H7BB H 0.1781 0.1925 0.5652 0.101 Uiso 1 1 d R . . . . C9BA C 0.3941(11) 0.9288(9) 0.3988(7) 0.082(5) Uani 1 1 d . . . . . H9BA H 0.3604 0.9580 0.4337 0.098 Uiso 1 1 d R . . . . H9BB H 0.4374 0.9689 0.3816 0.098 Uiso 1 1 d R . . . . C1CA C 0.3795(7) 0.7770(8) 0.4485(6) 0.046(3) Uani 1 1 d . . . . . H1CA H 0.3441 0.8022 0.4850 0.056 Uiso 1 1 calc R . . . . C3CA C 0.1341(7) 0.1554(7) 0.4247(7) 0.0744(12) Uani 1 1 d D U . . . H3CA H 0.0883 0.1602 0.3909 0.089 Uiso 1 1 d R . . . . H3CB H 0.1082 0.1355 0.4670 0.089 Uiso 1 1 d R . . . . C0BA C 0.0310(7) 0.3622(7) 0.4213(7) 0.0658(8) Uani 1 1 d D U . . . H0BA H 0.0553 0.3637 0.3752 0.079 Uiso 1 1 calc R . . . . C6DA C 0.2149(8) 0.2775(7) 0.3670(5) 0.0730(13) Uani 1 1 d D U . . . H6DA H 0.1693 0.2797 0.3330 0.088 Uiso 1 1 d R . . . . H6DB H 0.2378 0.3358 0.3723 0.088 Uiso 1 1 d R . . . . C7DA C 0.5399(9) 0.6625(8) 0.4470(6) 0.056(4) Uani 1 1 d . . . . . H7DA H 0.5742 0.7160 0.4491 0.068 Uiso 1 1 calc R . . . . C8DA C 0.5353(11) 0.7857(13) 0.6709(6) 0.109(6) Uani 1 1 d . . . . . H8DA H 0.5660 0.7342 0.6861 0.130 Uiso 1 1 d R . . . . H8DB H 0.5727 0.8353 0.6794 0.130 Uiso 1 1 d R . . . . C9DA C 0.1324(12) 0.2174(10) 0.6645(7) 0.077(5) Uani 1 1 d . . . . . H9DA H 0.0897 0.1711 0.6627 0.093 Uiso 1 1 d R . . . . H9DB H 0.1837 0.1949 0.6871 0.093 Uiso 1 1 d R . . . . C0EA C 0.6669(9) 0.5526(12) 0.3733(7) 0.094(6) Uani 1 1 d . . . . . H0EA H 0.6359 0.4980 0.3696 0.113 Uiso 1 1 d R . . . . H0EB H 0.7238 0.5451 0.3530 0.113 Uiso 1 1 d R . . . . C3BA C 0.5232(9) 0.7750(9) 0.5937(6) 0.069(4) Uani 1 1 d . . . . . H3BA H 0.5777 0.7640 0.5703 0.083 Uiso 1 1 d R . . . . H3BB H 0.4992 0.8290 0.5766 0.083 Uiso 1 1 d R . . . . C4CA C 0.2101(8) 0.0950(8) 0.4053(6) 0.0757(12) Uani 1 1 d D U . . . H4CA H 0.2525 0.0848 0.4410 0.091 Uiso 1 1 d R . . . . H4CB H 0.1824 0.0403 0.3942 0.091 Uiso 1 1 d R . . . . C8CA C -0.0065(7) 0.4475(6) 0.4307(6) 0.0778(12) Uani 1 1 d D U . . . H8CA H 0.0390 0.4902 0.4377 0.093 Uiso 1 1 d R . . . . H8CB H -0.0421 0.4465 0.4715 0.093 Uiso 1 1 d R . . . . C9CA C 0.3682(9) 0.7221(11) 0.6134(6) 0.069(5) Uani 1 1 d . . . . . H9CA H 0.3273 0.6758 0.6040 0.083 Uiso 1 1 calc R . . . . H9CB H 0.3432 0.7767 0.5984 0.083 Uiso 1 1 calc R . . . . C0DA C 0.5274(8) 0.6381(11) 0.3701(6) 0.059(4) Uani 1 1 d . . . . . H0DA H 0.4921 0.5861 0.3672 0.071 Uiso 1 1 d R . . . . H0DB H 0.4981 0.6843 0.3457 0.071 Uiso 1 1 d R . . . . C1DA C 0.3155(8) 0.7505(9) 0.3924(7) 0.064(4) Uani 1 1 d . . . . . H1DA H 0.2723 0.7114 0.4110 0.076 Uiso 1 1 d R . . . . H1DB H 0.3472 0.7195 0.3572 0.076 Uiso 1 1 d R . . . . C2 C 0.3758(9) 0.4534(12) 0.6363(11) 0.053(3) Uani 0.446(18) 1 d D U P A 2 H2A H 0.4002 0.4969 0.6665 0.064 Uiso 0.446(18) 1 d R . P A 2 H2B H 0.4193 0.4382 0.6025 0.064 Uiso 0.446(18) 1 d R . P A 2 C3DA C 0.6787(9) 0.5774(11) 0.4499(6) 0.079(5) Uani 1 1 d . . . . . H3DA H 0.7154 0.6285 0.4536 0.094 Uiso 1 1 d R . . . . H3DB H 0.7076 0.5301 0.4734 0.094 Uiso 1 1 d R . . . . C5DA C 0.3896(10) 0.7257(11) 0.6906(6) 0.073(5) Uani 1 1 d . . . . . H5DA H 0.4105 0.6690 0.7044 0.088 Uiso 1 1 d R . . . . H5DB H 0.3367 0.7380 0.7157 0.088 Uiso 1 1 d R . . . . C0CA C 0.0983(13) 0.2875(11) 0.7031(7) 0.099(7) Uani 1 1 d . . . . . H0CA H 0.1433 0.3307 0.7101 0.119 Uiso 1 1 d R . . . . H0CB H 0.0804 0.2662 0.7474 0.119 Uiso 1 1 d R . . . . C5AA C 0.6199(10) 0.6248(12) 0.3400(7) 0.079(5) Uani 1 1 d . . . . . H5AA H 0.6127 0.6071 0.2929 0.095 Uiso 1 1 d R . . . . H5AB H 0.6533 0.6782 0.3405 0.095 Uiso 1 1 d R . . . . C0AA C 0.4590(11) 0.7946(10) 0.7097(7) 0.090(6) Uani 1 1 d . . . . . H0AA H 0.4345 0.8517 0.7016 0.108 Uiso 1 1 d R . . . . H0AB H 0.4739 0.7907 0.7576 0.108 Uiso 1 1 d R . . . . O10 O 0.1791(7) 0.3979(7) 0.4869(5) 0.084(3) Uani 1 1 d . U . . . C11 C 0.1467(9) 0.6009(11) 0.7091(8) 0.123(6) Uani 1 1 d D U . . . H11A H 0.1709 0.6553 0.7253 0.148 Uiso 1 1 d R . . . . H11B H 0.1253 0.6108 0.6632 0.148 Uiso 1 1 d R . . . . C12 C 0.0373(11) 0.3588(10) 0.5956(6) 0.085(5) Uani 1 1 d . . . . . H12A H 0.0762 0.4084 0.5960 0.102 Uiso 1 1 d R . . . . H12B H -0.0158 0.3761 0.5727 0.102 Uiso 1 1 d R . . . . C15 C 0.1752(8) 0.2457(7) 0.4353(6) 0.0656(8) Uani 1 1 d D U . . . H15 H 0.2250 0.2357 0.4653 0.079 Uiso 1 1 calc R . . . . C20 C -0.0648(7) 0.4766(7) 0.3735(6) 0.0788(13) Uani 1 1 d D U . . . H20A H -0.0826 0.5367 0.3780 0.095 Uiso 1 1 d R . . . . H20B H -0.0356 0.4684 0.3302 0.095 Uiso 1 1 d R . . . . C4 C 0.2850(8) 0.2173(7) 0.3419(7) 0.0747(12) Uani 1 1 d D U . . . H4A H 0.3331 0.2170 0.3738 0.090 Uiso 1 1 d R . . . . H4B H 0.3060 0.2371 0.2980 0.090 Uiso 1 1 d R . . . . C7 C 0.2494(8) 0.1274(7) 0.3360(6) 0.0727(12) Uani 1 1 d D U . . . H7A H 0.2954 0.0879 0.3227 0.087 Uiso 1 1 d R . . . . H7B H 0.2073 0.1284 0.2993 0.087 Uiso 1 1 d R . . . . C1 C -0.0488(7) 0.3036(7) 0.4153(6) 0.0773(13) Uani 1 1 d D U . . . H1A H -0.0849 0.3122 0.4552 0.093 Uiso 1 1 d R . . . . H1B H -0.0339 0.2425 0.4127 0.093 Uiso 1 1 d R . . . . C3 C 0.0161(13) 0.3325(14) 0.6657(9) 0.113(6) Uani 1 1 d . U . . . H3A H -0.0323 0.2922 0.6656 0.136 Uiso 1 1 d R . . . . H3B H -0.0013 0.3836 0.6912 0.136 Uiso 1 1 d R . . . . C9 C -0.1385(8) 0.4123(7) 0.3712(8) 0.0777(13) Uani 1 1 d D U . . . H9A H -0.1540 0.4051 0.4188 0.093 Uiso 1 1 d R . . . . H9B H -0.1889 0.4314 0.3457 0.093 Uiso 1 1 d R . . . . C13 C -0.0996(8) 0.3296(6) 0.3495(6) 0.0780(13) Uani 1 1 d D U . . . H13A H -0.0621 0.3407 0.3108 0.094 Uiso 1 1 d R . . . . H13B H -0.1438 0.2874 0.3373 0.094 Uiso 1 1 d DR . . . . C6 C 0.3498(17) 0.3752(8) 0.6713(14) 0.109(10) Uani 0.446(18) 1 d D . P A 2 H6A H 0.3098 0.3411 0.6450 0.164 Uiso 0.446(18) 1 d DR . P A 2 H6B H 0.3226 0.3928 0.7131 0.164 Uiso 0.446(18) 1 d R . P A 2 H6C H 0.4005 0.3411 0.6814 0.164 Uiso 0.446(18) 1 d DR . P A 2 C21 C 0.3560(9) 0.4240(10) 0.6338(9) 0.053(3) Uani 0.554(18) 1 d D U P A 1 H21A H 0.3780 0.3783 0.6045 0.064 Uiso 0.554(18) 1 d R . P A 1 H21B H 0.3210 0.3970 0.6691 0.064 Uiso 0.554(18) 1 d R . P A 1 C5 C 0.4258(13) 0.4719(18) 0.6685(13) 0.109(10) Uani 0.554(18) 1 d D . P A 1 H5A H 0.4198 0.5334 0.6622 0.164 Uiso 0.554(18) 1 d R . P A 1 H5B H 0.4790 0.4526 0.6479 0.164 Uiso 0.554(18) 1 d R . P A 1 H5C H 0.4269 0.4589 0.7163 0.164 Uiso 0.554(18) 1 d R . P A 1 C8 C 0.0725(12) 0.5823(16) 0.7514(10) 0.167(5) Uani 1 1 d D U . . . H8A H 0.0275 0.5566 0.7241 0.250 Uiso 1 1 d R . . . . H8B H 0.0506 0.6337 0.7731 0.250 Uiso 1 1 d R . . . . H8C H 0.0910 0.5416 0.7855 0.250 Uiso 1 1 d R . . . . 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 0.0363(2) 0.0381(2) 0.0559(2) 0.0063(5) -0.0001(2) -0.0061(3) P0AA 0.0358(14) 0.0329(15) 0.0503(16) 0.0089(16) -0.0021(14) -0.0088(13) P6AA 0.0533(13) 0.0493(13) 0.0576(12) 0.0075(13) 0.0070(12) -0.0120(12) Cl9A 0.108(3) 0.0496(19) 0.071(2) -0.0022(19) -0.007(2) 0.0344(19) Cl1B 0.104(3) 0.058(2) 0.0615(17) -0.0029(16) -0.0172(18) 0.011(2) Cl2B 0.0601(18) 0.153(3) 0.070(2) 0.033(3) 0.0190(19) 0.0582(19) O1AA 0.033(4) 0.085(8) 0.059(4) 0.000(5) 0.003(3) 0.009(4) O2AA 0.115(7) 0.139(8) 0.060(4) 0.011(5) 0.005(5) 0.052(6) C3AA 0.056(8) 0.059(9) 0.111(11) 0.030(9) -0.034(8) -0.002(8) C4AA 0.041(6) 0.059(8) 0.057(7) 0.017(8) -0.004(6) 0.005(6) O2CA 0.060(4) 0.016(3) 0.048(4) -0.004(4) -0.013(4) 0.004(3) C5CA 0.094(10) 0.031(7) 0.071(8) 0.018(7) -0.045(7) 0.003(8) C6CA 0.0605(17) 0.0568(17) 0.0644(17) 0.0067(17) 0.0063(17) -0.0076(17) C7CA 0.060(7) 0.026(6) 0.059(7) 0.001(6) -0.007(7) -0.006(6) C5BA 0.043(7) 0.048(8) 0.090(9) -0.022(7) -0.016(7) -0.015(6) C7BA 0.053(8) 0.129(14) 0.072(9) 0.052(9) 0.007(8) -0.012(10) C9BA 0.135(13) 0.037(8) 0.072(9) 0.000(8) -0.042(9) 0.033(9) C1CA 0.032(6) 0.046(7) 0.060(7) 0.011(7) 0.002(6) 0.003(6) C3CA 0.078(2) 0.071(2) 0.074(2) 0.004(2) 0.012(2) 0.003(2) C0BA 0.0643(14) 0.0616(14) 0.0716(14) 0.0054(14) 0.0047(14) -0.0069(14) C6DA 0.076(2) 0.071(2) 0.073(2) 0.006(2) 0.012(2) 0.002(2) C7DA 0.060(8) 0.037(7) 0.072(8) 0.020(7) 0.003(7) 0.012(7) C8DA 0.130(13) 0.151(16) 0.045(7) -0.002(10) 0.016(9) -0.087(11) C9DA 0.114(13) 0.060(10) 0.058(8) -0.015(8) -0.011(9) 0.019(10) C0EA 0.051(7) 0.153(16) 0.079(10) -0.016(11) 0.006(7) 0.062(9) C3BA 0.080(9) 0.074(10) 0.054(7) -0.015(8) 0.016(7) -0.044(7) C4CA 0.079(2) 0.072(2) 0.076(2) 0.005(2) 0.012(2) 0.002(2) C8CA 0.075(2) 0.073(2) 0.086(2) 0.004(2) 0.000(2) -0.007(2) C9CA 0.051(8) 0.102(12) 0.054(7) -0.027(9) -0.013(7) -0.002(9) C0DA 0.051(7) 0.084(11) 0.043(7) -0.008(8) -0.004(6) 0.023(8) C1DA 0.046(7) 0.054(8) 0.091(9) 0.032(8) -0.029(7) 0.000(7) C2 0.053(4) 0.053(4) 0.054(4) 0.001(3) 0.002(3) 0.000(3) C3DA 0.068(9) 0.107(14) 0.061(8) 0.019(10) 0.005(8) 0.019(10) C5DA 0.064(9) 0.112(14) 0.044(7) 0.011(9) -0.012(7) -0.019(10) C0CA 0.167(18) 0.087(13) 0.043(7) -0.007(9) -0.026(9) 0.041(13) C5AA 0.079(10) 0.096(13) 0.063(9) 0.004(10) 0.024(8) 0.015(11) C0AA 0.148(14) 0.073(10) 0.049(8) -0.009(8) -0.003(9) -0.067(10) O10 0.078(4) 0.086(5) 0.088(4) 0.012(4) -0.017(4) -0.023(4) C11 0.124(10) 0.134(10) 0.111(9) 0.009(8) 0.010(8) 0.021(8) C12 0.125(12) 0.089(10) 0.041(7) -0.015(8) 0.017(8) 0.066(9) C15 0.0664(14) 0.0624(14) 0.0681(14) 0.0065(14) 0.0087(14) -0.0040(14) C20 0.076(2) 0.072(2) 0.088(2) 0.003(2) -0.001(2) -0.005(2) C4 0.078(2) 0.073(2) 0.073(2) 0.005(2) 0.012(2) 0.001(2) C7 0.076(2) 0.070(2) 0.072(2) 0.005(2) 0.013(2) 0.003(2) C1 0.075(2) 0.072(2) 0.085(2) 0.005(2) -0.003(2) -0.006(2) C3 0.118(10) 0.117(10) 0.104(9) 0.000(8) 0.016(8) 0.009(8) C9 0.074(2) 0.072(2) 0.088(2) 0.003(2) -0.001(2) -0.005(2) C13 0.075(2) 0.073(2) 0.086(2) 0.003(2) -0.001(2) -0.006(2) C6 0.092(16) 0.10(2) 0.133(18) -0.020(17) -0.053(14) -0.017(16) C21 0.053(4) 0.053(4) 0.054(4) 0.001(3) 0.002(3) 0.000(3) C5 0.092(16) 0.10(2) 0.133(18) -0.020(17) -0.053(14) -0.017(16) C8 0.165(6) 0.170(6) 0.165(6) 0.003(5) 0.002(5) 0.001(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Cl9A Dy1 Cl1B 99.23(11) Cl9A Dy1 Cl2B 165.78(11) Cl2B Dy1 Cl1B 94.82(11) O1AA Dy1 Cl9A 86.52(19) O1AA Dy1 Cl1B 173.76(17) O1AA Dy1 Cl2B 79.53(19) O2CA Dy1 Cl9A 87.2(2) O2CA Dy1 Cl1B 93.9(2) O2CA Dy1 Cl2B 89.7(2) O2CA Dy1 O1AA 88.8(3) O2CA Dy1 O10 174.9(3) O10 Dy1 Cl9A 92.0(3) O10 Dy1 Cl1B 91.2(3) O10 Dy1 Cl2B 89.8(3) O10 Dy1 O1AA 86.1(3) O2CA P0AA C5BA 108.0(5) O2CA P0AA C1CA 110.5(5) O2CA P0AA C7DA 108.6(5) C5BA P0AA C1CA 109.7(6) C7DA P0AA C5BA 107.3(6) C7DA P0AA C1CA 112.6(6) C0BA P6AA C6CA 112.5(6) O10 P6AA C6CA 108.0(6) O10 P6AA C0BA 111.2(6) O10 P6AA C15 107.0(6) C15 P6AA C6CA 106.3(6) C15 P6AA C0BA 111.6(6) Dy1 O1AA H1AB 124.8 Dy1 O1AA H1AA 118.9 C2 O1AA Dy1 130.0(9) C2 O1AA H1AB 102.8 C21 O1AA Dy1 129.4(8) C21 O1AA H1AA 110.6 C11 O2AA H2AA 112.8 H3AA C3AA H3AB 107.9 C5CA C3AA H3AA 109.4 C5CA C3AA H3AB 109.1 C1DA C3AA H3AA 110.0 C1DA C3AA H3AB 109.3 C1DA C3AA C5CA 111.0(11) H4AA C4AA H4AB 108.1 C7DA C4AA H4AA 107.9 C7DA C4AA H4AB 111.2 C7DA C4AA C3DA 111.0(11) C3DA C4AA H4AA 111.0 C3DA C4AA H4AB 107.5 P0AA O2CA Dy1 169.0(5) C3AA C5CA H5CA 109.1 C3AA C5CA H5CB 109.2 H5CA C5CA H5CB 107.9 C9BA C5CA C3AA 110.6(11) C9BA C5CA H5CA 109.2 C9BA C5CA H5CB 110.9 P6AA C6CA H6CA 108.5 C7BA C6CA P6AA 108.4(9) C7BA C6CA H6CA 108.5 C7BA C6CA C12 114.0(11) C12 C6CA P6AA 108.8(9) C12 C6CA H6CA 108.5 H7CA C7CA H7CB 107.5 C9BA C7CA H7CA 110.0 C9BA C7CA H7CB 108.7 C1CA C7CA H7CA 107.6 C1CA C7CA H7CB 109.7 C1CA C7CA C9BA 113.1(11) P0AA C5BA H5BA 106.0 C3BA C5BA P0AA 116.7(9) C3BA C5BA H5BA 106.0 C3BA C5BA C9CA 111.7(11) C9CA C5BA P0AA 109.7(8) C9CA C5BA H5BA 106.0 C6CA C7BA H7BA 108.2 C6CA C7BA H7BB 111.0 C6CA C7BA C9DA 110.2(12) H7BA C7BA H7BB 108.0 C9DA C7BA H7BA 109.0 C9DA C7BA H7BB 110.4 C5CA C9BA H9BA 112.2 C5CA C9BA H9BB 108.4 C7CA C9BA C5CA 106.9(10) C7CA C9BA H9BA 111.8 C7CA C9BA H9BB 108.9 H9BA C9BA H9BB 108.7 P0AA C1CA H1CA 105.8 C7CA C1CA P0AA 112.4(8) C7CA C1CA H1CA 105.8 C7CA C1CA C1DA 113.4(10) C1DA C1CA P0AA 112.8(9) C1DA C1CA H1CA 105.8 H3CA C3CA H3CB 108.1 C4CA C3CA H3CA 115.4 C4CA C3CA H3CB 109.4 C15 C3CA H3CA 108.7 C15 C3CA H3CB 109.8 C15 C3CA C4CA 105.3(9) P6AA C0BA H0BA 104.4 C8CA C0BA P6AA 120.6(9) C8CA C0BA H0BA 104.4 C8CA C0BA C1 103.0(9) C1 C0BA P6AA 118.1(8) C1 C0BA H0BA 104.4 H6DA C6DA H6DB 107.7 C15 C6DA H6DA 108.7 C15 C6DA H6DB 110.1 C4 C6DA H6DA 108.3 C4 C6DA H6DB 110.1 C4 C6DA C15 111.8(9) P0AA C7DA H7DA 107.9 C4AA C7DA P0AA 111.6(9) C4AA C7DA H7DA 107.9 C4AA C7DA C0DA 111.1(11) C0DA C7DA P0AA 110.3(9) C0DA C7DA H7DA 107.9 H8DA C8DA H8DB 107.6 C3BA C8DA H8DA 105.9 C3BA C8DA H8DB 109.0 C0AA C8DA H8DA 108.7 C0AA C8DA H8DB 109.0 C0AA C8DA C3BA 116.3(14) C7BA C9DA H9DA 108.6 C7BA C9DA H9DB 108.3 H9DA C9DA H9DB 107.8 C0CA C9DA C7BA 113.5(14) C0CA C9DA H9DA 109.2 C0CA C9DA H9DB 109.3 H0EA C0EA H0EB 108.1 C3DA C0EA H0EA 110.0 C3DA C0EA H0EB 108.6 C5AA C0EA H0EA 112.1 C5AA C0EA H0EB 110.5 C5AA C0EA C3DA 107.5(14) C5BA C3BA H3BA 111.3 C5BA C3BA H3BB 105.3 C8DA C3BA C5BA 111.9(11) C8DA C3BA H3BA 112.4 C8DA C3BA H3BB 107.3 H3BA C3BA H3BB 108.3 C3CA C4CA H4CA 115.5 C3CA C4CA H4CB 104.2 C3CA C4CA C7 108.3(9) H4CA C4CA H4CB 108.5 C7 C4CA H4CA 114.7 C7 C4CA H4CB 104.5 C0BA C8CA H8CA 110.2 C0BA C8CA H8CB 108.4 C0BA C8CA C20 114.4(10) H8CA C8CA H8CB 107.6 C20 C8CA H8CA 109.6 C20 C8CA H8CB 106.4 C5BA C9CA H9CA 110.5 C5BA C9CA H9CB 110.5 C5BA C9CA C5DA 106.1(11) H9CA C9CA H9CB 108.7 C5DA C9CA H9CA 110.5 C5DA C9CA H9CB 110.5 C7DA C0DA H0DA 108.8 C7DA C0DA H0DB 110.9 H0DA C0DA H0DB 108.4 C5AA C0DA C7DA 106.6(11) C5AA C0DA H0DA 112.5 C5AA C0DA H0DB 109.6 C3AA C1DA C1CA 112.2(12) C3AA C1DA H1DA 108.5 C3AA C1DA H1DB 109.8 C1CA C1DA H1DA 109.6 C1CA C1DA H1DB 108.6 H1DA C1DA H1DB 108.0 O1AA C2 H2A 114.2 O1AA C2 H2B 106.6 H2A C2 H2B 108.4 C6 C2 O1AA 105.8(15) C6 C2 H2A 113.1 C6 C2 H2B 108.4 C4AA C3DA H3DA 110.7 C4AA C3DA H3DB 109.3 C0EA C3DA C4AA 110.1(11) C0EA C3DA H3DA 109.7 C0EA C3DA H3DB 109.1 H3DA C3DA H3DB 107.8 C9CA C5DA H5DA 108.1 C9CA C5DA H5DB 109.0 C9CA C5DA C0AA 114.0(12) H5DA C5DA H5DB 108.2 C0AA C5DA H5DA 108.6 C0AA C5DA H5DB 108.9 C9DA C0CA H0CA 109.4 C9DA C0CA H0CB 109.0 C9DA C0CA C3 111.9(13) H0CA C0CA H0CB 108.0 C3 C0CA H0CA 109.3 C3 C0CA H0CB 109.2 C0EA C5AA C0DA 112.3(12) C0EA C5AA H5AA 105.5 C0EA C5AA H5AB 111.8 C0DA C5AA H5AA 107.2 C0DA C5AA H5AB 111.7 H5AA C5AA H5AB 107.9 C8DA C0AA C5DA 112.3(13) C8DA C0AA H0AA 108.9 C8DA C0AA H0AB 108.7 C5DA C0AA H0AA 108.2 C5DA C0AA H0AB 110.8 H0AA C0AA H0AB 107.8 P6AA O10 Dy1 165.3(6) O2AA C11 H11A 111.6 O2AA C11 H11B 107.7 O2AA C11 C8 115.9(16) H11A C11 H11B 107.4 C8 C11 H11A 106.7 C8 C11 H11B 107.2 C6CA C12 H12A 108.6 C6CA C12 H12B 109.1 H12A C12 H12B 107.9 C3 C12 C6CA 112.2(14) C3 C12 H12A 110.2 C3 C12 H12B 108.7 P6AA C15 H15 105.1 C3CA C15 P6AA 120.5(9) C3CA C15 C6DA 109.3(10) C3CA C15 H15 105.1 C6DA C15 P6AA 110.6(8) C6DA C15 H15 105.1 C8CA C20 H20A 112.7 C8CA C20 H20B 109.7 C8CA C20 C9 106.0(9) H20A C20 H20B 109.6 C9 C20 H20A 114.7 C9 C20 H20B 103.7 C6DA C4 H4A 109.8 C6DA C4 H4B 109.7 H4A C4 H4B 108.6 C7 C4 C6DA 109.4(10) C7 C4 H4A 109.0 C7 C4 H4B 110.2 C4CA C7 H7A 108.4 C4CA C7 H7B 113.1 C4 C7 C4CA 111.7(10) C4 C7 H7A 109.6 C4 C7 H7B 106.7 H7A C7 H7B 107.2 C0BA C1 H1A 108.4 C0BA C1 H1B 112.7 C0BA C1 C13 108.4(9) H1A C1 H1B 108.1 C13 C1 H1A 110.3 C13 C1 H1B 108.9 C0CA C3 H3A 109.2 C0CA C3 H3B 109.3 C12 C3 C0CA 111.6(15) C12 C3 H3A 110.1 C12 C3 H3B 108.7 H3A C3 H3B 107.9 C20 C9 H9A 103.4 C20 C9 H9B 114.8 H9A C9 H9B 109.4 C13 C9 C20 105.7(10) C13 C9 H9A 106.3 C13 C9 H9B 116.1 C1 C13 H13A 113.3 C1 C13 H13B 112.5 C9 C13 C1 100.7(9) C9 C13 H13A 108.5 C9 C13 H13B 111.5 H13A C13 H13B 110.1 C2 C6 H6A 112.2 C2 C6 H6B 107.0 C2 C6 H6C 109.2 H6A C6 H6B 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.4 O1AA C21 H21A 112.5 O1AA C21 H21B 105.8 O1AA C21 C5 110.9(15) H21A C21 H21B 107.8 C5 C21 H21A 112.5 C5 C21 H21B 106.9 C21 C5 H5A 111.3 C21 C5 H5B 105.9 C21 C5 H5C 111.2 H5A C5 H5B 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.4 C11 C8 H8A 109.4 C11 C8 H8B 111.8 C11 C8 H8C 107.2 H8A C8 H8B 109.4 H8A C8 H8C 109.5 H8B C8 H8C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Dy1 Cl9A 2.615(4) Dy1 Cl1B 2.639(3) Dy1 Cl2B 2.617(4) Dy1 O1AA 2.383(6) Dy1 O2CA 2.223(7) Dy1 O10 2.224(10) P0AA O2CA 1.493(7) P0AA C5BA 1.823(13) P0AA C1CA 1.830(12) P0AA C7DA 1.817(13) P6AA C6CA 1.813(13) P6AA C0BA 1.766(13) P6AA O10 1.471(10) P6AA C15 1.702(13) O1AA H1AB 0.8642 O1AA H1AA 0.8806 O1AA C2 1.465(15) O1AA C21 1.434(14) O2AA H2AA 0.8761 O2AA C11 1.418(15) C3AA H3AA 0.9705 C3AA H3AB 0.9700 C3AA C5CA 1.570(19) C3AA C1DA 1.502(18) C4AA H4AA 0.9698 C4AA H4AB 0.9700 C4AA C7DA 1.475(17) C4AA C3DA 1.567(17) C5CA H5CA 0.9698 C5CA H5CB 0.9696 C5CA C9BA 1.562(18) C6CA H6CA 0.9800 C6CA C7BA 1.509(19) C6CA C12 1.559(19) C7CA H7CA 0.9702 C7CA H7CB 0.9704 C7CA C9BA 1.557(17) C7CA C1CA 1.489(16) C5BA H5BA 0.9800 C5BA C3BA 1.538(17) C5BA C9CA 1.545(18) C7BA H7BA 0.9701 C7BA H7BB 0.9699 C7BA C9DA 1.564(18) C9BA H9BA 0.9702 C9BA H9BB 0.9701 C1CA H1CA 0.9800 C1CA C1DA 1.533(17) C3CA H3CA 0.9704 C3CA H3CB 0.9695 C3CA C4CA 1.543(13) C3CA C15 1.542(13) C0BA H0BA 0.9800 C0BA C8CA 1.445(12) C0BA C1 1.529(13) C6DA H6DA 0.9704 C6DA H6DB 0.9703 C6DA C15 1.551(13) C6DA C4 1.505(13) C7DA H7DA 0.9800 C7DA C0DA 1.567(17) C8DA H8DA 0.9698 C8DA H8DB 0.9702 C8DA C3BA 1.535(17) C8DA C0AA 1.41(2) C9DA H9DA 0.9700 C9DA H9DB 0.9699 C9DA C0CA 1.42(2) C0EA H0EA 0.9697 C0EA H0EB 0.9705 C0EA C3DA 1.561(19) C0EA C5AA 1.48(2) C3BA H3BA 0.9704 C3BA H3BB 0.9695 C4CA H4CA 0.9700 C4CA H4CB 0.9702 C4CA C7 1.570(13) C8CA H8CA 0.9701 C8CA H8CB 0.9698 C8CA C20 1.506(13) C9CA H9CA 0.9700 C9CA H9CB 0.9700 C9CA C5DA 1.551(16) C0DA H0DA 0.9699 C0DA H0DB 0.9700 C0DA C5AA 1.555(19) C1DA H1DA 0.9699 C1DA H1DB 0.9705 C2 H2A 0.9701 C2 H2B 0.9704 C2 C6 1.44(2) C3DA H3DA 0.9704 C3DA H3DB 0.9696 C5DA H5DA 0.9698 C5DA H5DB 0.9701 C5DA C0AA 1.55(2) C0CA H0CA 0.9706 C0CA H0CB 0.9700 C0CA C3 1.62(2) C5AA H5AA 0.9702 C5AA H5AB 0.9705 C0AA H0AA 0.9704 C0AA H0AB 0.9703 C11 H11A 0.9703 C11 H11B 0.9702 C11 C8 1.441(18) C12 H12A 0.9704 C12 H12B 0.9706 C12 C3 1.47(2) C15 H15 0.9800 C20 H20A 0.9700 C20 H20B 0.9695 C20 C9 1.506(13) C4 H4A 0.9703 C4 H4B 0.9697 C4 C7 1.492(13) C7 H7A 0.9701 C7 H7B 0.9703 C1 H1A 0.9699 C1 H1B 0.9702 C1 C13 1.561(13) C3 H3A 0.9704 C3 H3B 0.9700 C9 H9A 0.9702 C9 H9B 0.9702 C9 C13 1.469(13) C13 H13A 0.9701 C13 H13B 0.9705 C6 H6A 0.9601 C6 H6B 0.9600 C6 H6C 0.9602 C21 H21A 0.9701 C21 H21B 0.9704 C21 C5 1.47(2) C5 H5A 0.9601 C5 H5B 0.9604 C5 H5C 0.9600 C8 H8A 0.9605 C8 H8B 0.9598 C8 H8C 0.9595 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 Dy1 O1AA C2 C6 -119.5(14) Dy1 O1AA C21 C5 111.3(15) P0AA C5BA C3BA C8DA -179.0(11) P0AA C5BA C9CA C5DA 171.9(11) P0AA C1CA C1DA C3AA 179.6(10) P0AA C7DA C0DA C5AA 177.6(10) P6AA C6CA C7BA C9DA 171.7(11) P6AA C6CA C12 C3 -172.4(12) P6AA C0BA C8CA C20 166.6(9) P6AA C0BA C1 C13 -159.9(8) C3AA C5CA C9BA C7CA 58.4(15) C4AA C7DA C0DA C5AA -58.1(15) O2CA P0AA C5BA C3BA 169.7(9) O2CA P0AA C5BA C9CA -62.0(11) O2CA P0AA C1CA C7CA -157.0(8) O2CA P0AA C1CA C1DA -27.3(10) O2CA P0AA C7DA C4AA -64.0(10) O2CA P0AA C7DA C0DA 60.0(10) C5CA C3AA C1DA C1CA 52.5(16) C6CA P6AA C0BA C8CA 82.7(11) C6CA P6AA C0BA C1 -45.0(12) C6CA P6AA O10 Dy1 169(3) C6CA P6AA C15 C3CA 54.7(11) C6CA P6AA C15 C6DA -176.3(9) C6CA C7BA C9DA C0CA -55(2) C6CA C12 C3 C0CA 50(2) C7CA C1CA C1DA C3AA -51.2(15) C5BA P0AA O2CA Dy1 77(3) C5BA P0AA C1CA C7CA 84.0(10) C5BA P0AA C1CA C1DA -146.2(9) C5BA P0AA C7DA C4AA 52.5(11) C5BA P0AA C7DA C0DA 176.5(9) C5BA C9CA C5DA C0AA 56.7(18) C7BA C6CA C12 C3 -51.2(18) C7BA C9DA C0CA C3 55(2) C9BA C7CA C1CA P0AA -176.4(8) C9BA C7CA C1CA C1DA 54.2(14) C1CA P0AA O2CA Dy1 -43(3) C1CA P0AA C5BA C3BA -69.8(11) C1CA P0AA C5BA C9CA 58.5(11) C1CA P0AA C7DA C4AA 173.3(9) C1CA P0AA C7DA C0DA -62.7(11) C1CA C7CA C9BA C5CA -57.3(15) C3CA C4CA C7 C4 61.9(13) C0BA P6AA C6CA C7BA 171.2(10) C0BA P6AA C6CA C12 -64.3(11) C0BA P6AA O10 Dy1 -67(3) C0BA P6AA C15 C3CA -68.3(11) C0BA P6AA C15 C6DA 60.7(10) C0BA C8CA C20 C9 61.7(14) C0BA C1 C13 C9 -73.5(12) C6DA C4 C7 C4CA -56.2(14) C7DA P0AA O2CA Dy1 -167(3) C7DA P0AA C5BA C3BA 52.8(12) C7DA P0AA C5BA C9CA -178.9(10) C7DA P0AA C1CA C7CA -35.3(11) C7DA P0AA C1CA C1DA 94.4(10) C7DA C4AA C3DA C0EA -57.0(17) C7DA C0DA C5AA C0EA 62.1(17) C9DA C0CA C3 C12 -54(2) C3BA C5BA C9CA C5DA -57.1(16) C3BA C8DA C0AA C5DA 47(2) C4CA C3CA C15 P6AA -167.1(8) C4CA C3CA C15 C6DA 63.3(13) C8CA C0BA C1 C13 64.5(13) C8CA C20 C9 C13 -67.1(13) C9CA C5BA C3BA C8DA 53.6(17) C9CA C5DA C0AA C8DA -53.0(19) C1DA C3AA C5CA C9BA -58.3(16) C3DA C4AA C7DA P0AA -178.9(9) C3DA C4AA C7DA C0DA 57.5(15) C3DA C0EA C5AA C0DA -62.7(17) C5AA C0EA C3DA C4AA 58.0(17) C0AA C8DA C3BA C5BA -49(2) O10 P6AA C6CA C7BA -65.7(12) O10 P6AA C6CA C12 58.8(11) O10 P6AA C0BA C8CA -38.6(13) O10 P6AA C0BA C1 -166.4(9) O10 P6AA C15 C3CA 169.9(10) O10 P6AA C15 C6DA -61.1(10) C12 C6CA C7BA C9DA 50.3(17) C15 P6AA C6CA C7BA 48.8(12) C15 P6AA C6CA C12 173.3(9) C15 P6AA C0BA C8CA -158.0(10) C15 P6AA C0BA C1 74.3(11) C15 P6AA O10 Dy1 55(3) C15 C3CA C4CA C7 -63.3(13) C15 C6DA C4 C7 55.6(14) C20 C9 C13 C1 72.5(12) C4 C6DA C15 P6AA 164.4(9) C4 C6DA C15 C3CA -60.8(13) C1 C0BA C8CA C20 -59.1(14) loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.7065(14) 2 0.2935(14)