#------------------------------------------------------------------------------ #$Date: 2019-12-27 03:45:24 +0200 (Fri, 27 Dec 2019) $ #$Revision: 246213 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125696.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_7125696 loop_ _publ_author_name 'Murrie, Mark' 'Canaj, Angelos' 'Dey, Sourav' 'Cespedes, Oscar' 'Wilson, Claire' 'Rajaraman, Gopalan' _publ_section_title ; There is nothing wrong with being soft: using sulfur ligands to increase axiality in a Dy(III) Single-Ion Magnet ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC07292F _journal_year 2020 _chemical_formula_moiety 'C37 H54 Dy N5 O S4, 0.5(C4 H8 O)' _chemical_formula_sum 'C39 H58 Dy N5 O1.5 S4' _chemical_formula_weight 911.64 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-09-02 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-09-02 deposited with the CCDC. 2019-12-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 111.107(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.4260(8) _cell_length_b 14.4027(7) _cell_length_c 20.5958(9) _cell_measurement_reflns_used 9799 _cell_measurement_temperature 150 _cell_measurement_theta_max 27.456 _cell_measurement_theta_min 2.857 _cell_volume 4545.6(4) _computing_cell_refinement 'SAINT V8.37A (Bruker-AXS, 2016)' _computing_data_collection 'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)' _computing_data_reduction 'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)' _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 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 150 _diffrn_detector 'charge integrating pixel array detector' _diffrn_detector_area_resol_mean 7.4074 _diffrn_detector_type 'Bruker PHOTON II' _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_collimation 'focusing mirrors' _diffrn_radiation_monochromator 'multilayer mirror optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_unetI/netI 0.0195 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 47454 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.489 _diffrn_reflns_theta_min 3.021 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'INCOATEC I\ms 3.0' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.862 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6505 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0660 before and 0.0366 after correction. The Ratio of minimum to maximum transmission is 0.8725. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.332 _exptl_crystal_description prism _exptl_crystal_F_000 1876 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.066 _exptl_crystal_size_min 0.034 _refine_diff_density_max 0.852 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.074 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 506 _refine_ls_number_reflns 10374 _refine_ls_number_restraints 17 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0231 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+4.7737P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.0665 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9508 _reflns_number_total 10374 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc07292f2.cif _cod_data_source_block 1 _cod_original_formula_sum 'C39 H58 Dy N5 O1.50 S4' _cod_database_code 7125696 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.939 _shelx_estimated_absorpt_t_min 0.794 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C24-C25A = C26-C24 = C24-C26A = C27-C24 = C25-C24 = C24-C27A 1.51 with sigma of 0.02 C3S-C4S = C5S-C4S = C1S-C5S = C8S-C7S = C8S-C4S = C3S-C4S 1.51 with sigma of 0.02 O6S-C3S = O6S-C7S = C3S-O2S = C1S-O2S 1.44 with sigma of 0.02 C7S-C3S 2.4 with sigma of 0.02 3. Others Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)= Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=1-FVAR(1) Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=Sof(H26E)= Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=FVAR(1) Fixed Sof: C1S(0.25) H1SA(0.25) H1SB(0.25) O6S(0.25) O2S(0.25) C3S(0.5) H3SC(0.25) H3SD(0.25) H3SA(0.25) H3SB(0.25) C4S(0.5) H4SA(0.25) H4SB(0.25) H4SC(0.25) H4SD(0.25) C5S(0.25) H5SA(0.25) H5SB(0.25) C7S(0.25) H7SA(0.25) H7SB(0.25) C8S(0.25) H8SA(0.25) H8SB(0.25) 4.a Secondary CH2 refined with riding coordinates: C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C2C(H2CA,H2CB), C4C(H4CA,H4CB), C7C(H7CA,H7CB), C9C(H9CA,H9CB), C1S(H1SA,H1SB), C3S(H3SC,H3SD), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C4S(H4SC,H4SD), C5S(H5SA,H5SB), C7S(H7SA,H7SB), C8S(H8SA,H8SB) 4.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C17(H17) 4.c Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B, H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F), C3C(H3CA,H3CB,H3CC), C5C(H5CA,H5CB, H5CC), C8C(H8CA,H8CB,H8CC), C10C(H10A,H10B,H10C) ; _shelx_res_file ; TITL mo_at_838_thf_dipe_0m_a.res in P2(1)/c mo_at_838_thf_dipe_0m.res created by SHELXL-2018/3 at 11:13:11 on 02-Sep-2019 REM Old TITL mo_AT_838_THF_DIPE_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.087, Rweak 0.003, Alpha 0.032, Orientation as input REM Formula found by SHELXT: C35 N8 S4 Dy CELL 0.71073 16.426 14.4027 20.5958 90 111.107 90 ZERR 4 0.0008 0.0007 0.0009 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Dy N O S UNIT 156 232 4 20 6 16 DFIX 1.51 C24 C25A C26 C24 C24 C26A C27 C24 C25 C24 C24 C27A DFIX 1.51 C3S C4S C5S C4S C1S C5S C8S C7S C8S C4S C3S C4S DFIX 1.44 O6S C3S O6S C7S C3S O2S C1S O2S DFIX 2.4 C7S C3S L.S. 10 PLAN 10 SIZE 0.034 0.066 0.13 TEMP -123.15 BOND $H list 4 fmap 2 53 acta OMIT -2 1 2 OMIT 2 0 0 OMIT -1 2 3 OMIT 1 1 1 OMIT -3 2 3 OMIT -1 3 1 OMIT 0 3 1 OMIT 1 0 2 OMIT -2 2 3 OMIT -2 1 1 OMIT -2 1 4 OMIT 3 3 0 OMIT 1 2 2 OMIT 2 1 1 OMIT 0 2 3 OMIT 2 3 1 OMIT -1 2 1 OMIT -1 1 3 OMIT 1 1 4 OMIT 2 3 2 OMIT 0 1 4 REM REM REM WGHT 0.033600 4.773700 FVAR 0.32893 0.42768 DY1 3 0.402260 0.726452 0.646610 11.00000 0.02366 0.01539 = 0.02294 -0.00289 0.00970 0.00010 O1 5 0.266914 0.700499 0.630527 11.00000 0.02628 0.02615 = 0.03366 -0.00433 0.01299 -0.00177 N1 4 0.408293 0.661785 0.763008 11.00000 0.02489 0.02030 = 0.02797 -0.00236 0.01236 -0.00157 N2 4 0.371352 0.846589 0.727161 11.00000 0.02773 0.01829 = 0.03075 -0.00523 0.01355 -0.00264 N3 4 0.360431 0.885749 0.594133 11.00000 0.02854 0.02024 = 0.03037 -0.00019 0.00955 0.00298 C1 1 0.329881 0.903293 0.525692 11.00000 0.04828 0.02581 = 0.03245 0.00115 0.00888 0.00859 AFIX 43 H1 2 0.321152 0.852585 0.494410 11.00000 -1.20000 AFIX 0 C2 1 0.310506 0.991504 0.498508 11.00000 0.06676 0.03473 = 0.03647 0.00751 0.01188 0.01384 AFIX 43 H2 2 0.288054 1.001003 0.449581 11.00000 -1.20000 AFIX 0 C3 1 0.324228 1.065625 0.543432 11.00000 0.06138 0.02336 = 0.04947 0.00784 0.01549 0.00966 AFIX 43 H3 2 0.312328 1.127187 0.526021 11.00000 -1.20000 AFIX 0 C4 1 0.355526 1.049009 0.614104 11.00000 0.04181 0.01977 = 0.04488 -0.00142 0.01324 0.00310 AFIX 43 H4 2 0.365135 1.098927 0.646154 11.00000 -1.20000 AFIX 0 C5 1 0.372720 0.958543 0.637625 11.00000 0.02623 0.02071 = 0.03452 -0.00229 0.01106 -0.00004 C6 1 0.408429 0.935160 0.713860 11.00000 0.03118 0.01732 = 0.03328 -0.00433 0.01061 -0.00181 AFIX 23 H6A 2 0.472765 0.929954 0.729902 11.00000 -1.20000 H6B 2 0.394026 0.985648 0.740531 11.00000 -1.20000 AFIX 0 C7 1 0.414352 0.822235 0.801327 11.00000 0.04095 0.02329 = 0.02783 -0.00660 0.01773 -0.00282 AFIX 23 H7A 2 0.385153 0.855911 0.828774 11.00000 -1.20000 H7B 2 0.475852 0.843169 0.817442 11.00000 -1.20000 AFIX 0 C8 1 0.412295 0.719869 0.815039 11.00000 0.02969 0.02489 = 0.03075 -0.00295 0.01613 -0.00194 C9 1 0.420860 0.688771 0.880766 11.00000 0.05925 0.03476 = 0.03634 -0.00454 0.03085 -0.00635 AFIX 43 H9 2 0.422981 0.731703 0.916358 11.00000 -1.20000 AFIX 0 C10 1 0.426284 0.594477 0.893925 11.00000 0.06503 0.04118 = 0.03950 0.00692 0.03373 -0.00238 AFIX 43 H10 2 0.434608 0.571743 0.939170 11.00000 -1.20000 AFIX 0 C11 1 0.419418 0.533720 0.840269 11.00000 0.04056 0.02575 = 0.04747 0.00581 0.02394 -0.00045 AFIX 43 H11 2 0.421117 0.468485 0.847457 11.00000 -1.20000 AFIX 0 C12 1 0.410061 0.570034 0.776177 11.00000 0.02629 0.02049 = 0.03713 -0.00142 0.01517 -0.00110 AFIX 43 H12 2 0.404547 0.528131 0.739209 11.00000 -1.20000 AFIX 0 C13 1 0.275640 0.859351 0.709616 11.00000 0.03206 0.02382 = 0.04818 -0.00788 0.02150 0.00169 AFIX 23 H13A 2 0.249846 0.882016 0.661086 11.00000 -1.20000 H13B 2 0.266873 0.908317 0.740195 11.00000 -1.20000 AFIX 0 C14 1 0.226447 0.773955 0.716534 11.00000 0.02571 0.02895 = 0.04142 -0.00541 0.01477 0.00046 C15 1 0.181874 0.773766 0.762367 11.00000 0.02854 0.03892 = 0.04301 -0.00806 0.01708 0.00229 AFIX 43 H15 2 0.188096 0.825100 0.792746 11.00000 -1.20000 AFIX 0 C16 1 0.128460 0.700370 0.764842 11.00000 0.02290 0.04701 = 0.03887 0.00075 0.01388 0.00441 C17 1 0.120295 0.628168 0.717888 11.00000 0.02262 0.03716 = 0.04057 0.00096 0.01048 -0.00319 AFIX 43 H17 2 0.083136 0.577816 0.718325 11.00000 -1.20000 AFIX 0 C18 1 0.162751 0.624611 0.670381 11.00000 0.02081 0.03181 = 0.03464 -0.00233 0.00712 -0.00232 C19 1 0.220054 0.698726 0.671280 11.00000 0.02238 0.02930 = 0.03200 -0.00188 0.00933 0.00120 C20 1 0.147133 0.544209 0.618263 11.00000 0.02790 0.03374 = 0.04153 -0.00831 0.00894 -0.00787 C21 1 0.230314 0.487857 0.631680 11.00000 0.03890 0.03242 = 0.06345 -0.01492 0.01675 -0.00763 AFIX 137 H21A 2 0.275542 0.527871 0.625996 11.00000 -1.50000 H21B 2 0.218242 0.436337 0.598458 11.00000 -1.50000 H21C 2 0.250561 0.463184 0.679202 11.00000 -1.50000 AFIX 0 C22 1 0.076185 0.477243 0.622389 11.00000 0.03904 0.04607 = 0.05493 -0.01180 0.01276 -0.01765 AFIX 137 H22A 2 0.094569 0.449991 0.669067 11.00000 -1.50000 H22B 2 0.067330 0.427754 0.587861 11.00000 -1.50000 H22C 2 0.021464 0.511326 0.612866 11.00000 -1.50000 AFIX 0 C23 1 0.116235 0.583518 0.543701 11.00000 0.04656 0.05389 = 0.03912 -0.01173 0.00968 -0.01225 AFIX 137 H23A 2 0.060204 0.615250 0.533418 11.00000 -1.50000 H23B 2 0.109268 0.532618 0.510551 11.00000 -1.50000 H23C 2 0.159584 0.627683 0.539720 11.00000 -1.50000 AFIX 0 C24 1 0.081167 0.699456 0.816787 11.00000 0.02925 0.05725 = 0.04295 0.00075 0.01937 0.00215 PART 2 C25 1 0.145094 0.692388 0.888821 -21.00000 0.04571 0.14729 = 0.04441 0.00929 0.01479 -0.01309 AFIX 137 H25A 2 0.185069 0.640667 0.891857 -21.00000 -1.50000 H25B 2 0.114155 0.681488 0.920875 -21.00000 -1.50000 H25C 2 0.178372 0.750331 0.901411 -21.00000 -1.50000 AFIX 0 C26 1 0.024114 0.783878 0.806010 -21.00000 0.07757 0.08064 = 0.10351 0.01894 0.06828 0.03403 AFIX 137 H26A 2 0.060326 0.839883 0.814319 -21.00000 -1.50000 H26B 2 -0.007128 0.782358 0.838542 -21.00000 -1.50000 H26C 2 -0.018079 0.784475 0.758137 -21.00000 -1.50000 AFIX 0 C27 1 0.018383 0.612604 0.804788 -21.00000 0.07085 0.10477 = 0.08673 -0.03263 0.06137 -0.04605 AFIX 137 H27A 2 -0.026197 0.615546 0.757930 -21.00000 -1.50000 H27B 2 -0.009896 0.613105 0.839342 -21.00000 -1.50000 H27C 2 0.052373 0.555393 0.809662 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C25A 1 0.094137 0.796067 0.859181 21.00000 0.08928 0.08047 = 0.09262 -0.02951 0.07147 -0.01419 AFIX 137 H25D 2 0.156119 0.804790 0.886989 21.00000 -1.50000 H25E 2 0.060548 0.794377 0.890009 21.00000 -1.50000 H25F 2 0.073610 0.847638 0.826263 21.00000 -1.50000 AFIX 0 C26A 1 -0.013280 0.695001 0.779308 21.00000 0.03227 0.15111 = 0.07951 -0.00991 0.02905 -0.00472 AFIX 137 H26D 2 -0.032380 0.750080 0.749768 21.00000 -1.50000 H26E 2 -0.043090 0.692851 0.812816 21.00000 -1.50000 H26F 2 -0.027579 0.639092 0.750255 21.00000 -1.50000 AFIX 0 C27A 1 0.123864 0.628464 0.870977 21.00000 0.15257 0.15982 = 0.07142 0.06289 0.07986 0.09727 AFIX 137 H27D 2 0.124218 0.568501 0.848590 21.00000 -1.50000 H27E 2 0.091473 0.622674 0.902502 21.00000 -1.50000 H27F 2 0.183988 0.647515 0.897487 21.00000 -1.50000 AFIX 0 PART 0 S1C 6 0.459837 0.550031 0.623120 11.00000 0.03525 0.01891 = 0.02366 -0.00279 0.00945 0.00422 S2C 6 0.344670 0.662974 0.505845 11.00000 0.03924 0.01994 = 0.02473 -0.00010 0.00792 0.00157 S3C 6 0.547677 0.788572 0.603948 11.00000 0.02988 0.02512 = 0.02526 -0.00207 0.01165 0.00024 S4C 6 0.572460 0.743951 0.748764 11.00000 0.02723 0.04004 = 0.02468 -0.00059 0.01117 -0.00112 N1C 4 0.382754 0.485712 0.494085 11.00000 0.04169 0.02195 = 0.02492 -0.00463 0.01551 -0.00221 N2C 4 0.704309 0.764431 0.704565 11.00000 0.02527 0.03672 = 0.03076 -0.00223 0.01242 -0.00391 C1C 1 0.394077 0.558800 0.536338 11.00000 0.03212 0.01916 = 0.02495 -0.00192 0.01314 -0.00215 C2C 1 0.324055 0.490471 0.420448 11.00000 0.05344 0.03447 = 0.02337 -0.00906 0.01328 -0.00427 AFIX 23 H2CA 2 0.342150 0.442906 0.393663 11.00000 -1.20000 H2CB 2 0.330422 0.552070 0.401480 11.00000 -1.20000 AFIX 0 C3C 1 0.229195 0.475370 0.410214 11.00000 0.05089 0.04587 = 0.04027 -0.00831 0.00618 -0.00479 AFIX 137 H3CA 2 0.193264 0.483617 0.360957 11.00000 -1.50000 H3CB 2 0.211431 0.520416 0.438235 11.00000 -1.50000 H3CC 2 0.221365 0.412282 0.424813 11.00000 -1.50000 AFIX 0 C4C 1 0.425403 0.396153 0.518724 11.00000 0.04907 0.02056 = 0.03466 -0.00759 0.02000 0.00162 AFIX 23 H4CA 2 0.482928 0.407475 0.555641 11.00000 -1.20000 H4CB 2 0.435633 0.364348 0.479734 11.00000 -1.20000 AFIX 0 C5C 1 0.372301 0.333128 0.547107 11.00000 0.05389 0.02459 = 0.05050 0.00325 0.01792 -0.00404 AFIX 137 H5CA 2 0.315355 0.321276 0.510746 11.00000 -1.50000 H5CB 2 0.363912 0.363111 0.586954 11.00000 -1.50000 H5CC 2 0.403274 0.274217 0.561988 11.00000 -1.50000 AFIX 0 C6C 1 0.617573 0.766265 0.686807 11.00000 0.02889 0.01923 = 0.02870 -0.00531 0.01262 -0.00141 C7C 1 0.747629 0.784451 0.654846 11.00000 0.03092 0.05952 = 0.03633 -0.00248 0.01820 -0.00304 AFIX 23 H7CA 2 0.704508 0.779678 0.606824 11.00000 -1.20000 H7CB 2 0.793741 0.737629 0.660256 11.00000 -1.20000 AFIX 0 C8C 1 0.787792 0.880308 0.665919 11.00000 0.04385 0.05128 = 0.05458 0.02090 0.02392 0.00598 AFIX 137 H8CA 2 0.814754 0.891935 0.631288 11.00000 -1.50000 H8CB 2 0.832318 0.884359 0.712744 11.00000 -1.50000 H8CC 2 0.742343 0.926778 0.660902 11.00000 -1.50000 AFIX 0 C9C 1 0.762574 0.736485 0.774249 11.00000 0.02680 0.04236 = 0.03542 0.00121 0.00795 -0.00364 AFIX 23 H9CA 2 0.737465 0.756985 0.808943 11.00000 -1.20000 H9CB 2 0.819719 0.767582 0.785196 11.00000 -1.20000 AFIX 0 C10C 1 0.776019 0.632477 0.779656 11.00000 0.04040 0.04620 = 0.06148 0.00912 0.01883 0.00567 AFIX 137 H10A 2 0.803186 0.612316 0.746756 11.00000 -1.50000 H10B 2 0.719521 0.601467 0.768607 11.00000 -1.50000 H10C 2 0.814061 0.616255 0.827110 11.00000 -1.50000 AFIX 0 PART 1 C1S 1 -0.017446 0.822687 0.593492 10.25000 0.06389 AFIX 23 H1SA 2 -0.029787 0.878918 0.616024 10.25000 -1.20000 H1SB 2 0.020403 0.781100 0.630281 10.25000 -1.20000 AFIX 0 PART 0 PART 2 O6S 5 -0.137286 0.780694 0.545642 10.25000 0.05948 PART 0 PART 1 O2S 5 -0.099345 0.775169 0.553865 10.25000 0.18569 PART 0 C3S 1 -0.129082 0.778572 0.479755 10.50000 0.10587 PART 2 AFIX 23 H3SC 2 -0.176942 0.814815 0.446005 10.25000 -1.20000 H3SD 2 -0.133491 0.713713 0.462913 10.25000 -1.20000 AFIX 23 PART 0 PART 1 H3SA 2 -0.178959 0.821147 0.458578 10.25000 -1.20000 H3SB 2 -0.140994 0.716739 0.457300 10.25000 -1.20000 AFIX 0 PART 0 C4S 1 -0.045646 0.817458 0.484679 10.50000 0.11111 PART 1 AFIX 23 H4SA 2 -0.059954 0.871985 0.453307 10.25000 -1.20000 H4SB 2 -0.019389 0.771094 0.462595 10.25000 -1.20000 AFIX 23 PART 0 PART 2 H4SC 2 -0.052689 0.874447 0.456296 10.25000 -1.20000 H4SD 2 -0.009548 0.771986 0.471005 10.25000 -1.20000 AFIX 0 PART 0 PART 1 C5S 1 0.025497 0.847823 0.547202 10.25000 0.08961 AFIX 23 H5SA 2 0.080049 0.812475 0.555652 10.25000 -1.20000 H5SB 2 0.036914 0.915329 0.547338 10.25000 -1.20000 AFIX 0 PART 0 PART 2 C7S 1 -0.052869 0.770896 0.595683 10.25000 0.08508 AFIX 23 H7SA 2 -0.030128 0.706967 0.597152 10.25000 -1.20000 H7SB 2 -0.049950 0.789625 0.642720 10.25000 -1.20000 AFIX 0 C8S 1 -0.006823 0.839162 0.564934 10.25000 0.09775 AFIX 23 H8SA 2 0.057095 0.829223 0.584012 10.25000 -1.20000 H8SB 2 -0.019465 0.903932 0.574361 10.25000 -1.20000 AFIX 0 HKLF 4 REM mo_at_838_thf_dipe_0m_a.res in P2(1)/c REM wR2 = 0.066518, GooF = S = 1.04155, Restrained GooF = 1.04850 for all data REM R1 = 0.023137 for 9508 Fo > 4sig(Fo) and 0.026669 for all 10374 data REM 506 parameters refined using 17 restraints END WGHT 0.0332 4.7905 REM Highest difference peak 0.852, deepest hole -0.449, 1-sigma level 0.074 Q1 1 -0.0478 0.8646 0.5614 11.00000 0.05 0.85 Q2 1 -0.1136 0.8193 0.5541 11.00000 0.05 0.84 Q3 1 0.0397 0.8795 0.5995 11.00000 0.05 0.80 Q4 1 0.4411 0.7172 0.6820 11.00000 0.05 0.66 Q5 1 -0.0640 0.7760 0.5192 11.00000 0.05 0.62 Q6 1 -0.1181 0.7428 0.5047 11.00000 0.05 0.61 Q7 1 -0.1519 0.7447 0.5340 11.00000 0.05 0.59 Q8 1 0.4612 0.7670 0.6596 11.00000 0.05 0.55 Q9 1 -0.0855 0.7048 0.5625 11.00000 0.05 0.55 Q10 1 0.3451 0.6884 0.6376 11.00000 0.05 0.51 ; _shelx_res_checksum 59311 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.40226(2) 0.72645(2) 0.64661(2) 0.02030(4) Uani 1 1 d . . . . O1 O 0.26691(10) 0.70050(11) 0.63053(8) 0.0281(3) Uani 1 1 d . . . . N1 N 0.40829(12) 0.66179(12) 0.76301(9) 0.0236(4) Uani 1 1 d . . . . N2 N 0.37135(12) 0.84659(12) 0.72716(10) 0.0248(4) Uani 1 1 d . . . . N3 N 0.36043(12) 0.88575(13) 0.59413(10) 0.0267(4) Uani 1 1 d . . . . C1 C 0.32988(18) 0.90329(17) 0.52569(13) 0.0371(5) Uani 1 1 d . . . . H1 H 0.321152 0.852585 0.494410 0.044 Uiso 1 1 calc R . . . C2 C 0.3105(2) 0.9915(2) 0.49851(15) 0.0478(7) Uani 1 1 d . . . . H2 H 0.288054 1.001003 0.449581 0.057 Uiso 1 1 calc R . . . C3 C 0.3242(2) 1.06562(18) 0.54343(15) 0.0460(7) Uani 1 1 d . . . . H3 H 0.312328 1.127187 0.526021 0.055 Uiso 1 1 calc R . . . C4 C 0.35553(17) 1.04901(16) 0.61410(14) 0.0361(5) Uani 1 1 d . . . . H4 H 0.365135 1.098927 0.646154 0.043 Uiso 1 1 calc R . . . C5 C 0.37272(15) 0.95854(15) 0.63763(12) 0.0271(4) Uani 1 1 d . . . . C6 C 0.40843(15) 0.93516(15) 0.71386(12) 0.0275(4) Uani 1 1 d . . . . H6A H 0.472765 0.929954 0.729902 0.033 Uiso 1 1 calc R . . . H6B H 0.394026 0.985648 0.740531 0.033 Uiso 1 1 calc R . . . C7 C 0.41435(16) 0.82223(16) 0.80133(12) 0.0292(5) Uani 1 1 d . . . . H7A H 0.385153 0.855911 0.828774 0.035 Uiso 1 1 calc R . . . H7B H 0.475852 0.843169 0.817442 0.035 Uiso 1 1 calc R . . . C8 C 0.41230(15) 0.71987(15) 0.81504(12) 0.0270(5) Uani 1 1 d . . . . C9 C 0.4209(2) 0.68877(19) 0.88077(14) 0.0397(6) Uani 1 1 d . . . . H9 H 0.422981 0.731703 0.916358 0.048 Uiso 1 1 calc R . . . C10 C 0.4263(2) 0.5945(2) 0.89392(15) 0.0445(6) Uani 1 1 d . . . . H10 H 0.434608 0.571743 0.939170 0.053 Uiso 1 1 calc R . . . C11 C 0.41942(17) 0.53372(17) 0.84027(14) 0.0357(5) Uani 1 1 d . . . . H11 H 0.421117 0.468485 0.847457 0.043 Uiso 1 1 calc R . . . C12 C 0.41006(14) 0.57003(15) 0.77618(12) 0.0269(4) Uani 1 1 d . . . . H12 H 0.404547 0.528131 0.739209 0.032 Uiso 1 1 calc R . . . C13 C 0.27564(15) 0.85935(16) 0.70962(14) 0.0327(5) Uani 1 1 d . . . . H13A H 0.249846 0.882016 0.661086 0.039 Uiso 1 1 calc R . . . H13B H 0.266873 0.908317 0.740195 0.039 Uiso 1 1 calc R . . . C14 C 0.22645(16) 0.77395(16) 0.71653(14) 0.0313(5) Uani 1 1 d . . . . C15 C 0.18187(17) 0.77377(18) 0.76237(15) 0.0357(6) Uani 1 1 d . . . . H15 H 0.188096 0.825100 0.792746 0.043 Uiso 1 1 calc R . . . C16 C 0.12846(16) 0.7004(2) 0.76484(14) 0.0355(5) Uani 1 1 d . . . . C17 C 0.12029(15) 0.62817(18) 0.71789(13) 0.0337(5) Uani 1 1 d . . . . H17 H 0.083136 0.577816 0.718325 0.040 Uiso 1 1 calc R . . . C18 C 0.16275(14) 0.62461(17) 0.67038(12) 0.0299(5) Uani 1 1 d . . . . C19 C 0.22005(14) 0.69873(17) 0.67128(12) 0.0280(4) Uani 1 1 d . . . . C20 C 0.14713(16) 0.54421(18) 0.61826(14) 0.0354(5) Uani 1 1 d . . . . C21 C 0.23031(18) 0.48786(19) 0.63168(17) 0.0454(7) Uani 1 1 d . . . . H21A H 0.275542 0.527871 0.625996 0.068 Uiso 1 1 calc GR . . . H21B H 0.218242 0.436337 0.598458 0.068 Uiso 1 1 calc GR . . . H21C H 0.250561 0.463184 0.679202 0.068 Uiso 1 1 calc GR . . . C22 C 0.07619(19) 0.4772(2) 0.62239(17) 0.0478(7) Uani 1 1 d . . . . H22A H 0.094569 0.449991 0.669067 0.072 Uiso 1 1 calc GR . . . H22B H 0.067330 0.427754 0.587861 0.072 Uiso 1 1 calc GR . . . H22C H 0.021464 0.511326 0.612866 0.072 Uiso 1 1 calc GR . . . C23 C 0.1162(2) 0.5835(2) 0.54370(15) 0.0481(7) Uani 1 1 d . . . . H23A H 0.060204 0.615250 0.533418 0.072 Uiso 1 1 calc GR . . . H23B H 0.109268 0.532618 0.510551 0.072 Uiso 1 1 calc GR . . . H23C H 0.159584 0.627683 0.539720 0.072 Uiso 1 1 calc GR . . . C24 C 0.08117(17) 0.6995(2) 0.81679(15) 0.0414(6) Uani 1 1 d D . . . C25 C 0.1451(5) 0.6924(10) 0.8888(4) 0.080(3) Uani 0.572(10) 1 d D P A 2 H25A H 0.185069 0.640667 0.891857 0.119 Uiso 0.572(10) 1 calc GR P A 2 H25B H 0.114155 0.681488 0.920875 0.119 Uiso 0.572(10) 1 calc GR P A 2 H25C H 0.178372 0.750331 0.901411 0.119 Uiso 0.572(10) 1 calc GR P A 2 C26 C 0.0241(6) 0.7839(6) 0.8060(5) 0.077(3) Uani 0.572(10) 1 d D P A 2 H26A H 0.060326 0.839883 0.814319 0.116 Uiso 0.572(10) 1 calc GR P A 2 H26B H -0.007128 0.782358 0.838542 0.116 Uiso 0.572(10) 1 calc GR P A 2 H26C H -0.018079 0.784475 0.758137 0.116 Uiso 0.572(10) 1 calc GR P A 2 C27 C 0.0184(6) 0.6126(7) 0.8048(4) 0.078(3) Uani 0.572(10) 1 d D P A 2 H27A H -0.026197 0.615546 0.757930 0.118 Uiso 0.572(10) 1 calc GR P A 2 H27B H -0.009896 0.613105 0.839342 0.118 Uiso 0.572(10) 1 calc GR P A 2 H27C H 0.052373 0.555393 0.809662 0.118 Uiso 0.572(10) 1 calc GR P A 2 C25A C 0.0941(8) 0.7961(8) 0.8592(6) 0.077(4) Uani 0.428(10) 1 d D P A 1 H25D H 0.156119 0.804790 0.886989 0.115 Uiso 0.428(10) 1 calc GR P A 1 H25E H 0.060548 0.794377 0.890009 0.115 Uiso 0.428(10) 1 calc GR P A 1 H25F H 0.073610 0.847638 0.826263 0.115 Uiso 0.428(10) 1 calc GR P A 1 C26A C -0.0133(5) 0.6950(12) 0.7793(6) 0.085(5) Uani 0.428(10) 1 d D P A 1 H26D H -0.032380 0.750080 0.749768 0.128 Uiso 0.428(10) 1 calc GR P A 1 H26E H -0.043090 0.692851 0.812816 0.128 Uiso 0.428(10) 1 calc GR P A 1 H26F H -0.027579 0.639092 0.750255 0.128 Uiso 0.428(10) 1 calc GR P A 1 C27A C 0.1239(13) 0.6285(14) 0.8710(8) 0.117(8) Uani 0.428(10) 1 d D P A 1 H27D H 0.124218 0.568501 0.848590 0.176 Uiso 0.428(10) 1 calc GR P A 1 H27E H 0.091473 0.622674 0.902502 0.176 Uiso 0.428(10) 1 calc GR P A 1 H27F H 0.183988 0.647515 0.897487 0.176 Uiso 0.428(10) 1 calc GR P A 1 S1C S 0.45984(4) 0.55003(4) 0.62312(3) 0.02626(11) Uani 1 1 d . . . . S2C S 0.34467(4) 0.66297(4) 0.50584(3) 0.02896(12) Uani 1 1 d . . . . S3C S 0.54768(4) 0.78857(4) 0.60395(3) 0.02628(11) Uani 1 1 d . . . . S4C S 0.57246(4) 0.74395(5) 0.74876(3) 0.03015(12) Uani 1 1 d . . . . N1C N 0.38275(13) 0.48571(13) 0.49408(10) 0.0286(4) Uani 1 1 d . . . . N2C N 0.70431(13) 0.76443(14) 0.70456(11) 0.0303(4) Uani 1 1 d . . . . C1C C 0.39408(15) 0.55880(15) 0.53634(11) 0.0246(4) Uani 1 1 d . . . . C2C C 0.32405(18) 0.49047(18) 0.42045(12) 0.0372(6) Uani 1 1 d . . . . H2CA H 0.342150 0.442906 0.393663 0.045 Uiso 1 1 calc R . . . H2CB H 0.330422 0.552070 0.401480 0.045 Uiso 1 1 calc R . . . C3C C 0.2292(2) 0.4754(2) 0.41021(15) 0.0485(7) Uani 1 1 d . . . . H3CA H 0.193264 0.483617 0.360957 0.073 Uiso 1 1 calc GR . . . H3CB H 0.211431 0.520416 0.438235 0.073 Uiso 1 1 calc GR . . . H3CC H 0.221365 0.412282 0.424813 0.073 Uiso 1 1 calc GR . . . C4C C 0.42540(18) 0.39615(16) 0.51872(13) 0.0334(5) Uani 1 1 d . . . . H4CA H 0.482928 0.407475 0.555641 0.040 Uiso 1 1 calc R . . . H4CB H 0.435633 0.364348 0.479734 0.040 Uiso 1 1 calc R . . . C5C C 0.3723(2) 0.33313(18) 0.54711(16) 0.0432(6) Uani 1 1 d . . . . H5CA H 0.315355 0.321276 0.510746 0.065 Uiso 1 1 calc GR . . . H5CB H 0.363912 0.363111 0.586954 0.065 Uiso 1 1 calc GR . . . H5CC H 0.403274 0.274217 0.561988 0.065 Uiso 1 1 calc GR . . . C6C C 0.61757(15) 0.76626(14) 0.68681(12) 0.0250(4) Uani 1 1 d . . . . C7C C 0.74763(18) 0.7845(2) 0.65485(15) 0.0406(6) Uani 1 1 d . . . . H7CA H 0.704508 0.779678 0.606824 0.049 Uiso 1 1 calc R . . . H7CB H 0.793741 0.737629 0.660256 0.049 Uiso 1 1 calc R . . . C8C C 0.7878(2) 0.8803(2) 0.66592(17) 0.0482(7) Uani 1 1 d . . . . H8CA H 0.814754 0.891935 0.631288 0.072 Uiso 1 1 calc GR . . . H8CB H 0.832318 0.884359 0.712744 0.072 Uiso 1 1 calc GR . . . H8CC H 0.742343 0.926778 0.660902 0.072 Uiso 1 1 calc GR . . . C9C C 0.76257(17) 0.73648(19) 0.77425(14) 0.0358(5) Uani 1 1 d . . . . H9CA H 0.737465 0.756985 0.808943 0.043 Uiso 1 1 calc R . . . H9CB H 0.819719 0.767582 0.785196 0.043 Uiso 1 1 calc R . . . C10C C 0.7760(2) 0.6325(2) 0.77966(18) 0.0492(7) Uani 1 1 d . . . . H10A H 0.803186 0.612316 0.746756 0.074 Uiso 1 1 calc GR . . . H10B H 0.719521 0.601467 0.768607 0.074 Uiso 1 1 calc GR . . . H10C H 0.814061 0.616255 0.827110 0.074 Uiso 1 1 calc GR . . . C1S C -0.0174(10) 0.8227(12) 0.5935(9) 0.064(4) Uiso 0.25 1 d D P B 1 H1SA H -0.029787 0.878918 0.616024 0.077 Uiso 0.25 1 calc R P B 1 H1SB H 0.020403 0.781100 0.630281 0.077 Uiso 0.25 1 calc R P B 1 O6S O -0.1373(8) 0.7807(7) 0.5456(5) 0.059(3) Uiso 0.25 1 d D P B 2 O2S O -0.0993(17) 0.775(2) 0.5539(10) 0.186(12) Uiso 0.25 1 d D P B 1 C3S C -0.1291(8) 0.7786(8) 0.4798(6) 0.106(4) Uiso 0.5 1 d D P . . H3SC H -0.176942 0.814815 0.446005 0.127 Uiso 0.25 1 calc R P B 2 H3SD H -0.133491 0.713713 0.462913 0.127 Uiso 0.25 1 calc R P B 2 H3SA H -0.178959 0.821147 0.458578 0.127 Uiso 0.25 1 calc R P B 1 H3SB H -0.140994 0.716739 0.457300 0.127 Uiso 0.25 1 calc R P B 1 C4S C -0.0456(7) 0.8175(9) 0.4847(6) 0.111(4) Uiso 0.5 1 d D P B . H4SA H -0.059954 0.871985 0.453307 0.133 Uiso 0.25 1 calc R P C 1 H4SB H -0.019389 0.771094 0.462595 0.133 Uiso 0.25 1 calc R P C 1 H4SC H -0.052689 0.874447 0.456296 0.133 Uiso 0.25 1 calc R P D 2 H4SD H -0.009548 0.771986 0.471005 0.133 Uiso 0.25 1 calc R P D 2 C5S C 0.0255(12) 0.8478(16) 0.5472(9) 0.090(6) Uiso 0.25 1 d D P B 1 H5SA H 0.080049 0.812475 0.555652 0.108 Uiso 0.25 1 calc R P B 1 H5SB H 0.036914 0.915329 0.547338 0.108 Uiso 0.25 1 calc R P B 1 C7S C -0.0529(11) 0.7709(14) 0.5957(8) 0.085(5) Uiso 0.25 1 d D P B 2 H7SA H -0.030128 0.706967 0.597152 0.102 Uiso 0.25 1 calc R P B 2 H7SB H -0.049950 0.789625 0.642720 0.102 Uiso 0.25 1 calc R P B 2 C8S C -0.0068(15) 0.8392(16) 0.5649(9) 0.098(6) Uiso 0.25 1 d D P B 2 H8SA H 0.057095 0.829223 0.584012 0.117 Uiso 0.25 1 calc R P B 2 H8SB H -0.019465 0.903932 0.574361 0.117 Uiso 0.25 1 calc R P B 2 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 0.02366(6) 0.01539(5) 0.02294(6) -0.00289(3) 0.00970(4) 0.00010(3) O1 0.0263(8) 0.0262(8) 0.0337(8) -0.0043(7) 0.0130(7) -0.0018(6) N1 0.0249(9) 0.0203(8) 0.0280(9) -0.0024(7) 0.0124(7) -0.0016(7) N2 0.0277(9) 0.0183(8) 0.0308(9) -0.0052(7) 0.0136(8) -0.0026(7) N3 0.0285(9) 0.0202(8) 0.0304(9) -0.0002(7) 0.0095(8) 0.0030(7) C1 0.0483(15) 0.0258(11) 0.0324(12) 0.0012(9) 0.0089(11) 0.0086(10) C2 0.067(2) 0.0347(14) 0.0365(14) 0.0075(11) 0.0119(13) 0.0138(13) C3 0.0614(18) 0.0234(12) 0.0495(16) 0.0078(11) 0.0155(14) 0.0097(12) C4 0.0418(14) 0.0198(11) 0.0449(14) -0.0014(10) 0.0132(11) 0.0031(10) C5 0.0262(10) 0.0207(10) 0.0345(11) -0.0023(8) 0.0111(9) 0.0000(8) C6 0.0312(11) 0.0173(9) 0.0333(11) -0.0043(8) 0.0106(9) -0.0018(8) C7 0.0409(13) 0.0233(11) 0.0278(11) -0.0066(8) 0.0177(10) -0.0028(9) C8 0.0297(11) 0.0249(11) 0.0307(11) -0.0030(8) 0.0161(9) -0.0019(8) C9 0.0593(17) 0.0348(13) 0.0363(13) -0.0045(10) 0.0309(13) -0.0063(12) C10 0.0650(18) 0.0412(15) 0.0395(14) 0.0069(11) 0.0337(13) -0.0024(13) C11 0.0406(13) 0.0257(11) 0.0475(14) 0.0058(10) 0.0239(12) -0.0005(10) C12 0.0263(11) 0.0205(10) 0.0371(12) -0.0014(8) 0.0152(9) -0.0011(8) C13 0.0321(12) 0.0238(11) 0.0482(14) -0.0079(10) 0.0215(11) 0.0017(9) C14 0.0257(11) 0.0289(12) 0.0414(13) -0.0054(9) 0.0148(10) 0.0005(9) C15 0.0285(12) 0.0389(14) 0.0430(14) -0.0081(10) 0.0171(11) 0.0023(10) C16 0.0229(11) 0.0470(14) 0.0389(13) 0.0007(11) 0.0139(10) 0.0044(10) C17 0.0226(11) 0.0372(13) 0.0406(13) 0.0010(10) 0.0105(10) -0.0032(9) C18 0.0208(10) 0.0318(12) 0.0346(12) -0.0023(9) 0.0071(9) -0.0023(9) C19 0.0224(10) 0.0293(11) 0.0320(11) -0.0019(9) 0.0093(9) 0.0012(9) C20 0.0279(12) 0.0337(12) 0.0415(13) -0.0083(10) 0.0089(10) -0.0079(10) C21 0.0389(14) 0.0324(13) 0.0635(18) -0.0149(13) 0.0168(13) -0.0076(11) C22 0.0390(15) 0.0461(16) 0.0549(17) -0.0118(13) 0.0128(13) -0.0176(12) C23 0.0466(16) 0.0539(17) 0.0391(14) -0.0117(13) 0.0097(12) -0.0122(13) C24 0.0292(13) 0.0573(17) 0.0430(14) 0.0007(13) 0.0194(11) 0.0021(12) C25 0.046(4) 0.147(10) 0.044(4) 0.009(5) 0.015(3) -0.013(5) C26 0.078(6) 0.081(5) 0.104(7) 0.019(5) 0.068(6) 0.034(5) C27 0.071(5) 0.105(7) 0.087(5) -0.033(5) 0.061(5) -0.046(5) C25A 0.089(9) 0.080(7) 0.093(8) -0.030(6) 0.071(8) -0.014(6) C26A 0.032(4) 0.151(15) 0.080(7) -0.010(8) 0.029(4) -0.005(6) C27A 0.153(16) 0.160(16) 0.071(8) 0.063(10) 0.080(10) 0.097(14) S1C 0.0353(3) 0.0189(2) 0.0237(2) -0.00279(19) 0.0094(2) 0.0042(2) S2C 0.0392(3) 0.0199(2) 0.0247(2) -0.00010(19) 0.0079(2) 0.0016(2) S3C 0.0299(3) 0.0251(2) 0.0253(2) -0.0021(2) 0.0117(2) 0.0002(2) S4C 0.0272(3) 0.0400(3) 0.0247(3) -0.0006(2) 0.0112(2) -0.0011(2) N1C 0.0417(11) 0.0219(9) 0.0249(9) -0.0046(7) 0.0155(8) -0.0022(8) N2C 0.0253(10) 0.0367(11) 0.0308(10) -0.0022(8) 0.0124(8) -0.0039(8) C1C 0.0321(11) 0.0192(9) 0.0249(10) -0.0019(8) 0.0131(9) -0.0021(8) C2C 0.0534(16) 0.0345(13) 0.0234(11) -0.0091(9) 0.0133(11) -0.0043(11) C3C 0.0509(17) 0.0459(16) 0.0403(14) -0.0083(12) 0.0062(13) -0.0048(13) C4C 0.0491(14) 0.0206(10) 0.0347(12) -0.0076(9) 0.0200(11) 0.0016(10) C5C 0.0539(16) 0.0246(12) 0.0505(15) 0.0032(11) 0.0179(13) -0.0040(11) C6C 0.0289(11) 0.0192(10) 0.0287(11) -0.0053(8) 0.0126(9) -0.0014(8) C7C 0.0309(13) 0.0595(18) 0.0363(13) -0.0025(12) 0.0182(11) -0.0030(11) C8C 0.0439(15) 0.0513(17) 0.0546(17) 0.0209(14) 0.0239(13) 0.0060(13) C9C 0.0268(12) 0.0424(14) 0.0354(13) 0.0012(10) 0.0079(10) -0.0036(10) C10C 0.0404(15) 0.0462(16) 0.0615(18) 0.0091(14) 0.0188(14) 0.0057(13) 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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 O1 Dy1 N1 76.67(6) O1 Dy1 N2 77.52(6) O1 Dy1 N3 89.15(6) O1 Dy1 S1C 102.04(4) O1 Dy1 S2C 80.94(4) O1 Dy1 S3C 154.39(5) O1 Dy1 S4C 144.43(5) N1 Dy1 N2 65.64(6) N1 Dy1 S1C 85.98(4) N1 Dy1 S2C 136.60(4) N1 Dy1 S3C 128.94(4) N1 Dy1 S4C 68.90(4) N2 Dy1 S1C 151.11(4) N2 Dy1 S2C 143.14(4) N2 Dy1 S3C 110.83(4) N2 Dy1 S4C 80.37(4) N3 Dy1 N1 130.51(6) N3 Dy1 N2 65.04(6) N3 Dy1 S1C 143.51(4) N3 Dy1 S2C 85.22(4) N3 Dy1 S3C 73.91(4) N3 Dy1 S4C 106.26(5) S1C Dy1 S2C 62.960(16) S1C Dy1 S3C 82.240(16) S1C Dy1 S4C 84.570(18) S2C Dy1 S3C 78.667(17) S4C Dy1 S2C 131.143(18) S4C Dy1 S3C 60.638(16) C19 O1 Dy1 134.88(14) C8 N1 Dy1 119.93(14) C8 N1 C12 117.34(19) C12 N1 Dy1 122.70(14) C6 N2 Dy1 105.69(12) C6 N2 C13 108.46(17) C7 N2 Dy1 112.07(13) C7 N2 C6 108.71(17) C7 N2 C13 110.47(18) C13 N2 Dy1 111.24(13) C1 N3 Dy1 124.29(15) C1 N3 C5 117.6(2) C5 N3 Dy1 118.07(15) N3 C1 H1 118.5 N3 C1 C2 123.1(2) C2 C1 H1 118.5 C1 C2 H2 120.5 C3 C2 C1 118.9(3) C3 C2 H2 120.5 C2 C3 H3 120.5 C2 C3 C4 118.9(2) C4 C3 H3 120.5 C3 C4 H4 120.5 C3 C4 C5 119.0(2) C5 C4 H4 120.5 N3 C5 C4 122.5(2) N3 C5 C6 115.41(19) C4 C5 C6 122.0(2) N2 C6 C5 110.76(18) N2 C6 H6A 109.5 N2 C6 H6B 109.5 C5 C6 H6A 109.5 C5 C6 H6B 109.5 H6A C6 H6B 108.1 N2 C7 H7A 109.0 N2 C7 H7B 109.0 N2 C7 C8 113.12(18) H7A C7 H7B 107.8 C8 C7 H7A 109.0 C8 C7 H7B 109.0 N1 C8 C7 117.32(19) N1 C8 C9 122.5(2) C9 C8 C7 120.0(2) C8 C9 H9 120.4 C10 C9 C8 119.1(2) C10 C9 H9 120.4 C9 C10 H10 120.5 C11 C10 C9 119.0(2) C11 C10 H10 120.5 C10 C11 H11 120.8 C12 C11 C10 118.4(2) C12 C11 H11 120.8 N1 C12 C11 123.6(2) N1 C12 H12 118.2 C11 C12 H12 118.2 N2 C13 H13A 108.4 N2 C13 H13B 108.4 N2 C13 C14 115.52(19) H13A C13 H13B 107.5 C14 C13 H13A 108.4 C14 C13 H13B 108.4 C15 C14 C13 119.9(2) C15 C14 C19 121.1(2) C19 C14 C13 118.7(2) C14 C15 H15 119.2 C16 C15 C14 121.5(2) C16 C15 H15 119.2 C15 C16 C17 116.6(2) C15 C16 C24 121.3(2) C17 C16 C24 122.1(2) C16 C17 H17 117.7 C18 C17 C16 124.6(2) C18 C17 H17 117.7 C17 C18 C19 117.5(2) C17 C18 C20 121.3(2) C19 C18 C20 121.3(2) O1 C19 C14 118.8(2) O1 C19 C18 122.6(2) C14 C19 C18 118.6(2) C18 C20 C22 111.9(2) C18 C20 C23 109.4(2) C21 C20 C18 111.2(2) C21 C20 C22 107.6(2) C21 C20 C23 109.1(2) C22 C20 C23 107.5(2) C20 C21 H21A 109.5 C20 C21 H21B 109.5 C20 C21 H21C 109.5 H21A C21 H21B 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C20 C22 H22A 109.5 C20 C22 H22B 109.5 C20 C22 H22C 109.5 H22A C22 H22B 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C20 C23 H23A 109.5 C20 C23 H23B 109.5 C20 C23 H23C 109.5 H23A C23 H23B 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C16 C24 C27 111.3(3) C16 C24 C25A 111.6(4) C25 C24 C16 110.2(4) C25 C24 C26 112.5(7) C25 C24 C27 106.8(6) C26 C24 C16 109.6(3) C26 C24 C27 106.3(5) C26A C24 C16 109.9(4) C26A C24 C25A 103.4(7) C26A C24 C27A 119.2(11) C27A C24 C16 108.0(5) C27A C24 C25A 104.6(9) C24 C25 H25A 109.5 C24 C25 H25B 109.5 C24 C25 H25C 109.5 H25A C25 H25B 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C24 C26 H26A 109.5 C24 C26 H26B 109.5 C24 C26 H26C 109.5 H26A C26 H26B 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C24 C27 H27A 109.5 C24 C27 H27B 109.5 C24 C27 H27C 109.5 H27A C27 H27B 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C24 C25A H25D 109.5 C24 C25A H25E 109.5 C24 C25A H25F 109.5 H25D C25A H25E 109.5 H25D C25A H25F 109.5 H25E C25A H25F 109.5 C24 C26A H26D 109.5 C24 C26A H26E 109.5 C24 C26A H26F 109.5 H26D C26A H26E 109.5 H26D C26A H26F 109.5 H26E C26A H26F 109.5 C24 C27A H27D 109.5 C24 C27A H27E 109.5 C24 C27A H27F 109.5 H27D C27A H27E 109.5 H27D C27A H27F 109.5 H27E C27A H27F 109.5 C1C S1C Dy1 89.33(7) C1C S2C Dy1 88.18(7) C6C S3C Dy1 88.31(8) C6C S4C Dy1 92.24(8) C1C N1C C2C 121.3(2) C1C N1C C4C 122.01(19) C4C N1C C2C 116.71(18) C6C N2C C7C 122.7(2) C6C N2C C9C 121.9(2) C9C N2C C7C 115.2(2) S2C C1C S1C 118.69(12) N1C C1C S1C 120.32(17) N1C C1C S2C 120.99(17) N1C C2C H2CA 108.9 N1C C2C H2CB 108.9 N1C C2C C3C 113.3(2) H2CA C2C H2CB 107.7 C3C C2C H2CA 108.9 C3C C2C H2CB 108.9 C2C C3C H3CA 109.5 C2C C3C H3CB 109.5 C2C C3C H3CC 109.5 H3CA C3C H3CB 109.5 H3CA C3C H3CC 109.5 H3CB C3C H3CC 109.5 N1C C4C H4CA 109.0 N1C C4C H4CB 109.0 N1C C4C C5C 113.0(2) H4CA C4C H4CB 107.8 C5C C4C H4CA 109.0 C5C C4C H4CB 109.0 C4C C5C H5CA 109.5 C4C C5C H5CB 109.5 C4C C5C H5CC 109.5 H5CA C5C H5CB 109.5 H5CA C5C H5CC 109.5 H5CB C5C H5CC 109.5 S3C C6C S4C 117.49(13) N2C C6C S3C 122.89(18) N2C C6C S4C 119.62(18) N2C C7C H7CA 109.3 N2C C7C H7CB 109.3 N2C C7C C8C 111.6(2) H7CA C7C H7CB 108.0 C8C C7C H7CA 109.3 C8C C7C H7CB 109.3 C7C C8C H8CA 109.5 C7C C8C H8CB 109.5 C7C C8C H8CC 109.5 H8CA C8C H8CB 109.5 H8CA C8C H8CC 109.5 H8CB C8C H8CC 109.5 N2C C9C H9CA 109.3 N2C C9C H9CB 109.3 N2C C9C C10C 111.8(2) H9CA C9C H9CB 107.9 C10C C9C H9CA 109.3 C10C C9C H9CB 109.3 C9C C10C H10A 109.5 C9C C10C H10B 109.5 C9C C10C H10C 109.5 H10A C10C H10B 109.5 H10A C10C H10C 109.5 H10B C10C H10C 109.5 H1SA C1S H1SB 108.3 O2S C1S H1SA 109.9 O2S C1S H1SB 109.9 C5S C1S H1SA 109.9 C5S C1S H1SB 109.9 C5S C1S O2S 108.8(16) C7S O6S C3S 107.0(11) C3S O2S C1S 118.1(19) O6S C3S H3SC 109.7 O6S C3S H3SD 109.7 O6S C3S C4S 109.8(10) O2S C3S H3SA 113.7 O2S C3S H3SB 113.8 O2S C3S C4S 89.3(13) H3SC C3S H3SD 108.2 H3SA C3S H3SB 111.0 C4S C3S H3SC 109.7 C4S C3S H3SD 109.7 C4S C3S H3SA 113.8 C4S C3S H3SB 113.8 C3S C4S H4SA 105.3 C3S C4S H4SB 105.3 C3S C4S H4SC 111.9 C3S C4S H4SD 111.9 C3S C4S C5S 127.9(12) C3S C4S C8S 99.5(12) H4SA C4S H4SB 106.0 H4SC C4S H4SD 109.6 C5S C4S H4SA 105.3 C5S C4S H4SB 105.3 C8S C4S H4SC 111.9 C8S C4S H4SD 111.9 C1S C5S C4S 94.7(13) C1S C5S H5SA 112.8 C1S C5S H5SB 112.8 C4S C5S H5SA 112.8 C4S C5S H5SB 112.8 H5SA C5S H5SB 110.2 O6S C7S H7SA 112.2 O6S C7S H7SB 112.2 O6S C7S C8S 97.9(13) H7SA C7S H7SB 109.8 C8S C7S H7SA 112.2 C8S C7S H7SB 112.2 C4S C8S H8SA 111.0 C4S C8S H8SB 111.0 C7S C8S C4S 103.7(14) C7S C8S H8SA 111.0 C7S C8S H8SB 111.0 H8SA C8S H8SB 109.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Dy1 O1 2.1591(16) Dy1 N1 2.5403(18) Dy1 N2 2.5711(17) Dy1 N3 2.5237(18) Dy1 S1C 2.8133(5) Dy1 S2C 2.8567(6) Dy1 S3C 2.9647(6) Dy1 S4C 2.8407(6) O1 C19 1.328(3) N1 C8 1.342(3) N1 C12 1.347(3) N2 C6 1.481(3) N2 C7 1.476(3) N2 C13 1.492(3) N3 C1 1.339(3) N3 C5 1.346(3) C1 H1 0.9500 C1 C2 1.379(4) C2 H2 0.9500 C2 C3 1.377(4) C3 H3 0.9500 C3 C4 1.379(4) C4 H4 0.9500 C4 C5 1.383(3) C5 C6 1.503(3) C6 H6A 0.9900 C6 H6B 0.9900 C7 H7A 0.9900 C7 H7B 0.9900 C7 C8 1.504(3) C8 C9 1.384(3) C9 H9 0.9500 C9 C10 1.381(4) C10 H10 0.9500 C10 C11 1.382(4) C11 H11 0.9500 C11 C12 1.376(3) C12 H12 0.9500 C13 H13A 0.9900 C13 H13B 0.9900 C13 C14 1.506(3) C14 C15 1.387(4) C14 C19 1.408(3) C15 H15 0.9500 C15 C16 1.386(4) C16 C17 1.393(4) C16 C24 1.532(3) C17 H17 0.9500 C17 C18 1.392(3) C18 C19 1.419(3) C18 C20 1.536(3) C20 C21 1.526(4) C20 C22 1.538(4) C20 C23 1.541(4) C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C24 C25 1.481(8) C24 C26 1.502(7) C24 C27 1.583(7) C24 C25A 1.616(9) C24 C26A 1.464(8) C24 C27A 1.490(11) C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C25A H25D 0.9800 C25A H25E 0.9800 C25A H25F 0.9800 C26A H26D 0.9800 C26A H26E 0.9800 C26A H26F 0.9800 C27A H27D 0.9800 C27A H27E 0.9800 C27A H27F 0.9800 S1C C1C 1.728(2) S2C C1C 1.714(2) S3C C6C 1.710(2) S4C C6C 1.721(2) N1C C1C 1.335(3) N1C C2C 1.477(3) N1C C4C 1.468(3) N2C C6C 1.338(3) N2C C7C 1.471(3) N2C C9C 1.466(3) C2C H2CA 0.9900 C2C H2CB 0.9900 C2C C3C 1.511(4) C3C H3CA 0.9800 C3C H3CB 0.9800 C3C H3CC 0.9800 C4C H4CA 0.9900 C4C H4CB 0.9900 C4C C5C 1.515(4) C5C H5CA 0.9800 C5C H5CB 0.9800 C5C H5CC 0.9800 C7C H7CA 0.9900 C7C H7CB 0.9900 C7C C8C 1.512(4) C8C H8CA 0.9800 C8C H8CB 0.9800 C8C H8CC 0.9800 C9C H9CA 0.9900 C9C H9CB 0.9900 C9C C10C 1.512(4) C10C H10A 0.9800 C10C H10B 0.9800 C10C H10C 0.9800 C1S H1SA 0.9900 C1S H1SB 0.9900 C1S O2S 1.467(17) C1S C5S 1.422(16) O6S C3S 1.411(13) O6S C7S 1.406(16) O2S C3S 1.426(17) C3S H3SC 0.9900 C3S H3SD 0.9900 C3S H3SA 0.9900 C3S H3SB 0.9900 C3S C4S 1.450(11) C4S H4SA 0.9900 C4S H4SB 0.9900 C4S H4SC 0.9900 C4S H4SD 0.9900 C4S C5S 1.460(15) C4S C8S 1.574(16) C5S H5SA 0.9900 C5S H5SB 0.9900 C7S H7SA 0.9900 C7S H7SB 0.9900 C7S C8S 1.512(17) C8S H8SA 0.9900 C8S H8SB 0.9900