#------------------------------------------------------------------------------ #$Date: 2019-04-16 01:16:54 +0300 (Tue, 16 Apr 2019) $ #$Revision: 214637 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/08/1550885.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_1550885 loop_ _publ_author_name 'Moreno-Pineda, Eufemio' 'Taran, Gheorghe' 'Wernsdorfer, Wolfgang' 'Ruben, Mario' _publ_section_title ; Quantum Tunnelling of the Magnetisation in Single-Molecule Magnet Isotopologue Dimers ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC01062A _journal_year 2019 _chemical_formula_moiety 'C74 H120 Dy2 N4 O12, C4 H10 O2' _chemical_formula_sum 'C78 H130 Dy2 N4 O14' _chemical_formula_weight 1672.85 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-02-11 _audit_creation_method ; Olex2 1.2 (compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337) ; _audit_update_record ; 2019-02-20 deposited with the CCDC. 2019-04-12 downloaded from the CCDC. ; _cell_angle_alpha 91.995(2) _cell_angle_beta 93.347(2) _cell_angle_gamma 107.530(2) _cell_formula_units_Z 1 _cell_length_a 10.8671(2) _cell_length_b 13.8736(3) _cell_length_c 14.8582(3) _cell_measurement_reflns_used 20815 _cell_measurement_temperature 180 _cell_measurement_theta_max 27.0580 _cell_measurement_theta_min 2.0120 _cell_volume 2129.20(8) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 180 _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector_type STOE _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details 'List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -90.00 90.00 1.00 180.60 -- 0.00 180.00 250.00 180 2 \w -10.00 90.00 1.00 180.60 -- 0.00 180.00 64.00 100' _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS2T' _diffrn_measurement_method 'rotation method' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0350774000 _diffrn_orient_matrix_UB_12 -0.0473788000 _diffrn_orient_matrix_UB_13 -0.0219213000 _diffrn_orient_matrix_UB_21 -0.0182383000 _diffrn_orient_matrix_UB_22 0.0252296000 _diffrn_orient_matrix_UB_23 -0.0367919000 _diffrn_orient_matrix_UB_31 0.0560970000 _diffrn_orient_matrix_UB_32 -0.0014560000 _diffrn_orient_matrix_UB_33 -0.0214353000 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_unetI/netI 0.0315 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 24512 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.371 _diffrn_reflns_theta_min 1.970 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.799 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.88127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.' _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.305 _exptl_crystal_description block _exptl_crystal_F_000 870 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Dichloromethane and ethanol' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.204 _refine_diff_density_min -1.299 _refine_diff_density_rms 0.098 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 480 _refine_ls_number_reflns 8663 _refine_ls_number_restraints 48 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0241 _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^)+(0.0326P)^2^+2.5740P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.0619 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8201 _reflns_number_total 8663 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL em1-119_a.res in P-1 em1-119.res created by SHELXL-2017/1 at 14:50:45 on 11-Feb-2019 REM Old TITL em1-119_a.res in P-1 REM SHELXT solution in P-1 REM R1 0.080, Rweak 0.012, Alpha 0.038, Orientation as input REM Formula found by SHELXT: C75 N4 O14 Dy2 CELL 0.71073 10.8671 13.8736 14.8582 91.995 93.347 107.53 ZERR 1 0.0002 0.0003 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H Dy N O UNIT 78 130 2 4 14 DFIX 1.54 C1S O0AA C1S C2S DFIX 1.1 O0AA C1S RIGU C3A C4A C1A C2A RIGU O0AA C1S C2S ISOR 0.01 0.01 O0AA C1S C2S EADP C2A C1A C3A L.S. 10 PLAN 20 SIZE 0.13 0.11 0.1 BOND $H list 4 fmap 2 acta SHEL 100 0.8 OMIT 4 -7 10 OMIT -1 2 1 OMIT 0 1 0 OMIT -1 1 0 OMIT 0 1 1 REM REM REM WGHT 0.032600 2.574000 FVAR 0.46155 0.58363 DY1 3 0.657389 0.605099 0.200779 11.00000 0.01137 0.01220 = 0.01515 -0.00339 -0.00054 0.00253 O1A 5 0.512283 0.614369 0.304791 11.00000 0.01536 0.02580 = 0.02174 -0.00515 0.00200 0.00223 O1B 5 0.624067 0.758524 0.168586 11.00000 0.01760 0.01638 = 0.03513 0.00268 0.00424 0.00400 O1C 5 0.786470 0.504430 0.231246 11.00000 0.01702 0.01667 = 0.02777 -0.00097 -0.00328 0.00412 O2A 5 0.777390 0.691850 0.324039 11.00000 0.01705 0.03297 = 0.02175 -0.01174 -0.00004 0.00346 O2B 5 0.835843 0.698336 0.132249 11.00000 0.01823 0.01756 = 0.02815 -0.00237 0.00582 0.00358 O2C 5 0.522884 0.438369 0.200239 11.00000 0.01605 0.01530 = 0.03154 -0.00178 0.00041 0.00326 N1 4 0.458140 0.575262 0.087154 11.00000 0.01751 0.01784 = 0.01744 -0.00380 -0.00012 0.00698 N2 4 0.337230 0.483175 -0.043737 11.00000 0.01393 0.02180 = 0.01682 -0.00319 0.00020 0.00560 C1 1 0.443445 0.516188 0.011965 11.00000 0.01347 0.01434 = 0.01507 0.00058 0.00062 0.00331 C1A 1 0.333246 0.523344 0.437348 11.00000 0.03489 0.09527 = 0.07874 0.00639 0.02166 0.01466 AFIX 137 H1AA 2 0.331833 0.487137 0.380856 11.00000 -1.50000 H1AB 2 0.246729 0.508851 0.455999 11.00000 -1.50000 H1AC 2 0.385884 0.502669 0.482220 11.00000 -1.50000 AFIX 0 C1B 1 0.687096 1.013443 0.099378 11.00000 0.06621 0.03987 = 0.08654 0.03042 0.03120 0.03143 AFIX 137 H1BA 2 0.779126 1.043343 0.108812 11.00000 -1.50000 H1BB 2 0.645505 1.065009 0.106248 11.00000 -1.50000 H1BC 2 0.665880 0.981953 0.039588 11.00000 -1.50000 AFIX 0 C1C 1 0.884961 0.274387 0.264088 11.00000 0.03727 0.03355 = 0.10358 0.00757 -0.01749 0.01991 AFIX 137 H1CA 2 0.823908 0.244649 0.307090 11.00000 -1.50000 H1CB 2 0.967102 0.265341 0.281391 11.00000 -1.50000 H1CC 2 0.854335 0.242183 0.205342 11.00000 -1.50000 AFIX 0 C2 1 0.235079 0.511526 -0.021391 11.00000 0.01415 0.02993 = 0.02188 -0.00148 0.00029 0.00755 AFIX 43 H2 2 0.158299 0.488773 -0.057778 11.00000 -1.20000 AFIX 0 C2A 1 0.398469 0.696200 0.515044 11.00000 0.03489 0.09527 = 0.07874 0.00639 0.02166 0.01466 AFIX 137 H2AA 2 0.442384 0.669327 0.561089 11.00000 -1.50000 H2AB 2 0.313155 0.691796 0.532070 11.00000 -1.50000 H2AC 2 0.445998 0.765745 0.508037 11.00000 -1.50000 AFIX 0 C2B 1 0.493126 0.893496 0.158251 11.00000 0.03185 0.03132 = 0.10841 0.00494 0.00516 0.01774 AFIX 137 H2BA 2 0.466092 0.859530 0.099773 11.00000 -1.50000 H2BB 2 0.457783 0.948819 0.164334 11.00000 -1.50000 H2BC 2 0.462760 0.846761 0.204105 11.00000 -1.50000 AFIX 0 C2C 1 0.999741 0.434557 0.194729 11.00000 0.03042 0.06191 = 0.04801 0.01070 0.01040 0.02677 AFIX 137 H2CA 2 0.969904 0.403906 0.135357 11.00000 -1.50000 H2CB 2 1.080805 0.423890 0.212475 11.00000 -1.50000 H2CC 2 1.011072 0.505890 0.194380 11.00000 -1.50000 AFIX 0 C3 1 0.241070 0.573781 0.054449 11.00000 0.01915 0.02988 = 0.02620 -0.00360 0.00312 0.01241 AFIX 43 H3 2 0.170290 0.594058 0.069250 11.00000 -1.20000 AFIX 0 C3A 1 0.296591 0.666741 0.361085 11.00000 0.03489 0.09527 = 0.07874 0.00639 0.02166 0.01466 AFIX 137 H3AA 2 0.333978 0.736305 0.347836 11.00000 -1.50000 H3AB 2 0.216105 0.658708 0.387926 11.00000 -1.50000 H3AC 2 0.281406 0.624890 0.306259 11.00000 -1.50000 AFIX 0 C3B 1 0.683016 0.983322 0.263276 11.00000 0.08519 0.05621 = 0.05941 -0.01994 -0.00577 0.04621 AFIX 137 H3BA 2 0.651726 0.934370 0.307255 11.00000 -1.50000 H3BB 2 0.648278 1.038679 0.271740 11.00000 -1.50000 H3BC 2 0.775771 1.008061 0.270379 11.00000 -1.50000 AFIX 0 C3C 1 0.948696 0.437836 0.355357 11.00000 0.02841 0.05673 = 0.03606 0.00518 -0.00959 0.01508 AFIX 137 H3CA 2 0.959022 0.508945 0.353790 11.00000 -1.50000 H3CB 2 1.030422 0.428205 0.372925 11.00000 -1.50000 H3CC 2 0.887162 0.408421 0.398165 11.00000 -1.50000 AFIX 0 C4 1 0.356292 0.604742 0.107445 11.00000 0.02151 0.02564 = 0.02072 -0.00546 0.00204 0.01157 AFIX 43 H4 2 0.363140 0.647192 0.158553 11.00000 -1.20000 AFIX 0 C4A 1 0.388763 0.635618 0.426292 11.00000 0.01871 0.05555 = 0.03072 -0.00477 0.01030 0.00273 C4B 1 0.640544 0.933833 0.168648 11.00000 0.02776 0.01826 = 0.03922 0.00263 0.00613 0.00954 C4C 1 0.900052 0.386729 0.261618 11.00000 0.02135 0.02572 = 0.03660 0.00513 -0.00187 0.01043 C5A 1 0.519370 0.653180 0.384012 11.00000 0.01965 0.02438 = 0.02052 -0.00118 0.00584 0.00460 C5B 1 0.699067 0.846048 0.158805 11.00000 0.02467 0.01664 = 0.02451 -0.00052 0.00128 0.00650 C5C 1 0.774054 0.410692 0.234668 11.00000 0.02109 0.02126 = 0.01969 -0.00001 -0.00021 0.00906 C6A 1 0.635219 0.707450 0.433016 11.00000 0.02348 0.03399 = 0.01787 -0.00777 0.00207 0.00453 AFIX 43 H6A 2 0.630249 0.734340 0.490419 11.00000 -1.20000 AFIX 0 C6B 1 0.830584 0.866790 0.143141 11.00000 0.02144 0.01516 = 0.03853 0.00115 0.00459 0.00061 AFIX 43 H6B 2 0.879946 0.934192 0.141064 11.00000 -1.20000 AFIX 0 C6C 1 0.657186 0.333986 0.216317 11.00000 0.02338 0.01475 = 0.03748 -0.00019 -0.00197 0.00546 AFIX 43 H6C 2 0.658938 0.267341 0.214252 11.00000 -1.20000 AFIX 0 C7A 1 0.757779 0.723592 0.400807 11.00000 0.02008 0.02065 = 0.01653 -0.00292 -0.00205 0.00456 C7B 1 0.891709 0.792898 0.130535 11.00000 0.01754 0.01943 = 0.02163 -0.00046 0.00269 0.00087 C7C 1 0.536533 0.351270 0.200703 11.00000 0.02117 0.01644 = 0.01969 -0.00095 0.00093 0.00236 C8 1 0.411696 0.261678 0.182179 11.00000 0.02243 0.01778 = 0.02989 0.00010 -0.00118 0.00021 C8A 1 0.881416 0.784973 0.457248 11.00000 0.02091 0.02635 = 0.01909 -0.00765 -0.00482 0.00383 C8B 1 1.035902 0.821240 0.110957 11.00000 0.01761 0.02448 = 0.03490 0.00197 0.00844 0.00111 C9A 1 0.861081 0.804039 0.556490 11.00000 0.03539 0.05651 = 0.02073 -0.01395 -0.00533 0.00588 AFIX 137 H9AA 2 0.801079 0.842310 0.560530 11.00000 -1.50000 H9AB 2 0.942253 0.841328 0.587717 11.00000 -1.50000 H9AC 2 0.827147 0.740446 0.583517 11.00000 -1.50000 AFIX 0 C9B 1 1.104913 0.935345 0.116294 11.00000 0.02348 0.02845 = 0.07644 0.00292 0.01372 -0.00253 AFIX 137 H9BA 2 1.064340 0.967033 0.072116 11.00000 -1.50000 H9BB 2 1.194110 0.947386 0.104632 11.00000 -1.50000 H9BC 2 1.099560 0.963165 0.175482 11.00000 -1.50000 AFIX 0 C10A 1 0.930653 0.886453 0.412796 11.00000 0.03477 0.02564 = 0.03777 -0.00451 -0.00592 -0.00316 AFIX 137 H10A 2 0.941777 0.874235 0.350245 11.00000 -1.50000 H10B 2 1.012034 0.925506 0.442682 11.00000 -1.50000 H10C 2 0.868935 0.923076 0.417663 11.00000 -1.50000 AFIX 0 C10B 1 1.042740 0.777103 0.016186 11.00000 0.03362 0.05353 = 0.04234 -0.00254 0.01940 0.00353 AFIX 137 H10D 2 0.998032 0.705783 0.012512 11.00000 -1.50000 H10E 2 1.131604 0.788022 0.004126 11.00000 -1.50000 H10F 2 1.002871 0.809821 -0.027520 11.00000 -1.50000 AFIX 0 C11A 1 0.981740 0.728055 0.451665 11.00000 0.02596 0.04407 = 0.03810 -0.00899 -0.01137 0.01239 AFIX 137 H11A 2 0.949933 0.663632 0.477705 11.00000 -1.50000 H11B 2 1.061102 0.766971 0.484199 11.00000 -1.50000 H11C 2 0.997097 0.717869 0.389590 11.00000 -1.50000 AFIX 0 C11B 1 1.102853 0.771380 0.180326 11.00000 0.02138 0.04530 = 0.05330 0.00796 0.00152 0.01112 AFIX 137 H11D 2 1.101377 0.800860 0.239518 11.00000 -1.50000 H11E 2 1.190896 0.781868 0.166292 11.00000 -1.50000 H11F 2 1.058345 0.700089 0.178744 11.00000 -1.50000 AFIX 0 PART 1 C9C 1 0.403864 0.179585 0.250107 21.00000 0.03878 0.03548 = 0.05708 0.02058 -0.00653 -0.01277 AFIX 137 H9CA 2 0.478375 0.156317 0.247501 21.00000 -1.50000 H9CB 2 0.326912 0.123893 0.235428 21.00000 -1.50000 H9CC 2 0.401404 0.207187 0.309889 21.00000 -1.50000 AFIX 0 C10C 1 0.413928 0.216564 0.087885 21.00000 0.06441 0.05620 = 0.03919 -0.01951 -0.00503 -0.02074 AFIX 137 H10G 2 0.405285 0.263868 0.044145 21.00000 -1.50000 H10H 2 0.343536 0.155015 0.077532 21.00000 -1.50000 H10I 2 0.494375 0.202296 0.082383 21.00000 -1.50000 AFIX 0 C11C 1 0.291666 0.296466 0.189117 21.00000 0.01522 0.03646 = 0.14181 -0.00126 0.00339 -0.00185 AFIX 137 H11G 2 0.293190 0.327090 0.248281 21.00000 -1.50000 H11H 2 0.215390 0.239216 0.178756 21.00000 -1.50000 H11I 2 0.291032 0.344940 0.144671 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C5 1 0.347517 0.275449 0.090941 -21.00000 0.06227 0.05467 = 0.04364 0.01771 -0.02852 -0.03558 AFIX 137 H5A 2 0.329927 0.339249 0.092755 -21.00000 -1.50000 H5B 2 0.267938 0.221637 0.078686 -21.00000 -1.50000 H5C 2 0.404483 0.274088 0.044229 -21.00000 -1.50000 AFIX 0 C6 1 0.327002 0.267602 0.256579 -21.00000 0.03286 0.06918 = 0.05392 -0.00934 0.01897 -0.02148 AFIX 137 H6D 2 0.370370 0.262267 0.313496 -21.00000 -1.50000 H6E 2 0.247424 0.213189 0.247697 -21.00000 -1.50000 H6F 2 0.308812 0.331154 0.256331 -21.00000 -1.50000 AFIX 0 C9CA 1 0.436675 0.158759 0.176461 -21.00000 0.03156 0.02118 = 0.16195 0.00060 -0.00542 -0.00585 AFIX 137 H9CD 2 0.500525 0.160295 0.134074 -21.00000 -1.50000 H9CE 2 0.357711 0.107012 0.156877 -21.00000 -1.50000 H9CF 2 0.467439 0.144482 0.234848 -21.00000 -1.50000 AFIX 0 PART 0 O0AA 5 0.525151 1.005710 0.539871 11.00000 0.10094 0.12892 = 0.18776 0.01939 0.05722 0.04574 C1S 1 0.658348 1.021081 0.534794 11.00000 0.10822 0.13394 = 0.15003 -0.00214 0.04252 0.05600 AFIX 23 H1SA 2 0.675098 0.962585 0.506647 11.00000 -1.20000 H1SB 2 0.698225 1.080505 0.502087 11.00000 -1.20000 AFIX 0 C2S 1 0.699218 1.034314 0.622382 11.00000 0.14881 0.14641 = 0.17501 -0.00532 0.01975 0.03792 AFIX 137 H2SA 2 0.791959 1.052791 0.628312 11.00000 -1.50000 H2SB 2 0.663502 0.972504 0.651740 11.00000 -1.50000 H2SC 2 0.671510 1.087139 0.649917 11.00000 -1.50000 AFIX 0 HKLF 4 REM em1-119_a.res in P-1 REM R1 = 0.0241 for 8201 Fo > 4sig(Fo) and 0.0282 for all 8663 data REM 480 parameters refined using 48 restraints END WGHT 0.0326 2.5738 REM Highest difference peak 1.204, deepest hole -1.299, 1-sigma level 0.098 Q1 1 0.4060 0.6372 0.5334 11.00000 0.05 1.20 Q2 1 0.3410 0.4971 0.4069 11.00000 0.05 0.92 Q3 1 0.3893 0.7370 0.4882 11.00000 0.05 0.77 Q4 1 0.3305 0.5439 0.4749 11.00000 0.05 0.58 Q5 1 0.3233 0.4398 -0.0850 11.00000 0.05 0.41 Q6 1 0.5000 1.0000 0.5000 10.50000 0.05 0.41 Q7 1 0.7069 0.7063 0.4185 11.00000 0.05 0.41 Q8 1 0.2977 0.5890 0.0793 11.00000 0.05 0.41 Q9 1 0.4534 0.6477 0.4066 11.00000 0.05 0.38 Q10 1 0.7294 1.0330 0.1808 11.00000 0.05 0.37 Q11 1 0.3348 0.7072 0.3735 11.00000 0.05 0.37 Q12 1 0.5663 0.6112 0.2874 11.00000 0.05 0.36 Q13 1 0.5890 0.7109 0.3918 11.00000 0.05 0.36 Q14 1 0.2468 0.5410 0.0212 11.00000 0.05 0.36 Q15 1 0.7443 0.6995 0.2899 11.00000 0.05 0.35 Q16 1 0.2883 0.4947 -0.0281 11.00000 0.05 0.34 Q17 1 0.8404 0.3942 0.2480 11.00000 0.05 0.33 Q18 1 0.5181 0.9031 0.0890 11.00000 0.05 0.32 Q19 1 0.2067 0.5629 0.0652 11.00000 0.05 0.32 Q20 1 0.8251 0.7583 0.4278 11.00000 0.05 0.31 REM The information below was added by Olex2. REM REM R1 = 0.0241 for 8201 Fo > 4sig(Fo) and 0.0282 for all 26267 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.20, deepest hole -1.30 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0282 REM R1_gt = 0.0241 REM wR_ref = 0.0619 REM GOOF = 1.050 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 26267 REM Reflections_gt = 8201 REM Parameters = n/a REM Hole = -1.30 REM Peak = 1.20 REM Flack = n/a ; _cod_data_source_file c9sc01062a2.cif _cod_data_source_block em1-119 _cod_database_code 1550885 _shelx_shelxl_version_number 2016/4 _chemical_oxdiff_formula C76H125Dy2N4O13 _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 0.841 _shelx_estimated_absorpt_t_min 0.800 _reflns_odcompleteness_completeness 99.41 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.04 _olex2_refinement_description ; 1. 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 2. Restrained distances C1S-O0AA = C1S-C2S 1.54 with sigma of 0.02 O0AA-C1S 1.1 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(O0AA) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(C2S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01 Uanis(C2A) = Uanis(C1A) = Uanis(C3A) 4. Rigid body (RIGU) restrains C3A, C4A, C1A, C2A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O0AA, C1S, C2S with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6D)=Sof(H6E)=Sof(H6F)= Sof(C9CA)=Sof(H9CD)=Sof(H9CE)=Sof(H9CF)=1-FVAR(1) Sof(C9C)=Sof(H9CA)=Sof(H9CB)=Sof(H9CC)=Sof(C10C)=Sof(H10G)=Sof(H10H)= Sof(H10I)=Sof(C11C)=Sof(H11G)=Sof(H11H)=Sof(H11I)=FVAR(1) 6.a Secondary CH2 refined with riding coordinates: C1S(H1SA,H1SB) 6.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C6A(H6A), C6B(H6B), C6C(H6C) 6.c Idealised Me refined as rotating group: C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C2A(H2AA,H2AB, H2AC), C2B(H2BA,H2BB,H2BC), C2C(H2CA,H2CB,H2CC), C3A(H3AA,H3AB,H3AC), C3B(H3BA, H3BB,H3BC), C3C(H3CA,H3CB,H3CC), C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C11A(H11A,H11B,H11C), C11B(H11D, H11E,H11F), C9C(H9CA,H9CB,H9CC), C10C(H10G,H10H,H10I), C11C(H11G,H11H,H11I), C5(H5A,H5B,H5C), C6(H6D,H6E,H6F), C9CA(H9CD,H9CE,H9CF), C2S(H2SA,H2SB,H2SC) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details 'Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling' _oxdiff_exptl_absorpt_empirical_full_max 1.095 _oxdiff_exptl_absorpt_empirical_full_min 0.848 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.65739(2) 0.60510(2) 0.20078(2) 0.01330(4) Uani 1 1 d . . . . . O1A O 0.51228(16) 0.61437(13) 0.30479(12) 0.0220(4) Uani 1 1 d . . . . . O1B O 0.62407(16) 0.75852(13) 0.16859(13) 0.0232(4) Uani 1 1 d . . . . . O1C O 0.78647(16) 0.50443(13) 0.23125(12) 0.0210(4) Uani 1 1 d . . . . . O2A O 0.77739(17) 0.69185(14) 0.32404(12) 0.0252(4) Uani 1 1 d . . . . . O2B O 0.83584(16) 0.69834(13) 0.13225(12) 0.0216(4) Uani 1 1 d . . . . . O2C O 0.52288(16) 0.43837(12) 0.20024(12) 0.0214(4) Uani 1 1 d . . . . . N1 N 0.45814(19) 0.57526(15) 0.08715(13) 0.0174(4) Uani 1 1 d . . . . . N2 N 0.33723(19) 0.48318(15) -0.04374(13) 0.0176(4) Uani 1 1 d . . . . . C1 C 0.4434(2) 0.51619(17) 0.01196(15) 0.0145(4) Uani 1 1 d . . . . . C1A C 0.3332(4) 0.5233(4) 0.4373(3) 0.0700(7) Uani 1 1 d . U . . . H1AA H 0.331833 0.487137 0.380856 0.105 Uiso 1 1 calc GR . . . . H1AB H 0.246729 0.508851 0.455999 0.105 Uiso 1 1 calc GR . . . . H1AC H 0.385884 0.502669 0.482220 0.105 Uiso 1 1 calc GR . . . . C1B C 0.6871(4) 1.0134(3) 0.0994(3) 0.0591(11) Uani 1 1 d . . . . . H1BA H 0.779126 1.043343 0.108812 0.089 Uiso 1 1 calc GR . . . . H1BB H 0.645505 1.065009 0.106248 0.089 Uiso 1 1 calc GR . . . . H1BC H 0.665880 0.981953 0.039588 0.089 Uiso 1 1 calc GR . . . . C1C C 0.8850(4) 0.2744(3) 0.2641(3) 0.0569(11) Uani 1 1 d . . . . . H1CA H 0.823908 0.244649 0.307090 0.085 Uiso 1 1 calc GR . . . . H1CB H 0.967102 0.265341 0.281391 0.085 Uiso 1 1 calc GR . . . . H1CC H 0.854335 0.242183 0.205342 0.085 Uiso 1 1 calc GR . . . . C2 C 0.2351(2) 0.5115(2) -0.02139(17) 0.0219(5) Uani 1 1 d . . . . . H2 H 0.158299 0.488773 -0.057778 0.026 Uiso 1 1 calc R . . . . C2A C 0.3985(4) 0.6962(4) 0.5150(3) 0.0700(7) Uani 1 1 d . U . . . H2AA H 0.442384 0.669327 0.561089 0.105 Uiso 1 1 calc GR . . . . H2AB H 0.313155 0.691796 0.532070 0.105 Uiso 1 1 calc GR . . . . H2AC H 0.445998 0.765745 0.508037 0.105 Uiso 1 1 calc GR . . . . C2B C 0.4931(3) 0.8935(3) 0.1583(3) 0.0554(10) Uani 1 1 d . . . . . H2BA H 0.466092 0.859530 0.099773 0.083 Uiso 1 1 calc GR . . . . H2BB H 0.457783 0.948819 0.164334 0.083 Uiso 1 1 calc GR . . . . H2BC H 0.462760 0.846761 0.204105 0.083 Uiso 1 1 calc GR . . . . C2C C 0.9997(3) 0.4346(3) 0.1947(2) 0.0435(8) Uani 1 1 d . . . . . H2CA H 0.969904 0.403906 0.135357 0.065 Uiso 1 1 calc GR . . . . H2CB H 1.080805 0.423890 0.212475 0.065 Uiso 1 1 calc GR . . . . H2CC H 1.011072 0.505890 0.194380 0.065 Uiso 1 1 calc GR . . . . C3 C 0.2411(2) 0.5738(2) 0.05445(18) 0.0240(5) Uani 1 1 d . . . . . H3 H 0.170290 0.594058 0.069250 0.029 Uiso 1 1 calc R . . . . C3A C 0.2966(4) 0.6667(4) 0.3611(3) 0.0700(7) Uani 1 1 d . U . . . H3AA H 0.333978 0.736305 0.347836 0.105 Uiso 1 1 calc GR . . . . H3AB H 0.216105 0.658708 0.387926 0.105 Uiso 1 1 calc GR . . . . H3AC H 0.281406 0.624890 0.306259 0.105 Uiso 1 1 calc GR . . . . C3B C 0.6830(5) 0.9833(3) 0.2633(3) 0.0625(12) Uani 1 1 d . . . . . H3BA H 0.651726 0.934370 0.307255 0.094 Uiso 1 1 calc GR . . . . H3BB H 0.648278 1.038679 0.271740 0.094 Uiso 1 1 calc GR . . . . H3BC H 0.775771 1.008061 0.270379 0.094 Uiso 1 1 calc GR . . . . C3C C 0.9487(3) 0.4378(3) 0.3554(2) 0.0404(7) Uani 1 1 d . . . . . H3CA H 0.959022 0.508945 0.353790 0.061 Uiso 1 1 calc GR . . . . H3CB H 1.030422 0.428205 0.372925 0.061 Uiso 1 1 calc GR . . . . H3CC H 0.887162 0.408421 0.398165 0.061 Uiso 1 1 calc GR . . . . C4 C 0.3563(2) 0.60474(19) 0.10744(17) 0.0218(5) Uani 1 1 d . . . . . H4 H 0.363140 0.647192 0.158553 0.026 Uiso 1 1 calc R . . . . C4A C 0.3888(3) 0.6356(3) 0.4263(2) 0.0367(7) Uani 1 1 d . U . . . C4B C 0.6405(3) 0.9338(2) 0.1686(2) 0.0277(6) Uani 1 1 d . . . . . C4C C 0.9001(3) 0.3867(2) 0.26162(19) 0.0272(6) Uani 1 1 d . . . . . C5A C 0.5194(2) 0.65318(19) 0.38401(17) 0.0219(5) Uani 1 1 d . . . . . C5B C 0.6991(2) 0.84605(18) 0.15881(17) 0.0220(5) Uani 1 1 d . . . . . C5C C 0.7741(2) 0.41069(19) 0.23467(16) 0.0202(5) Uani 1 1 d . . . . . C6A C 0.6352(3) 0.7074(2) 0.43302(17) 0.0262(5) Uani 1 1 d . . . . . H6A H 0.630249 0.734340 0.490419 0.031 Uiso 1 1 calc R . . . . C6B C 0.8306(3) 0.86679(19) 0.14314(19) 0.0260(5) Uani 1 1 d . . . . . H6B H 0.879946 0.934192 0.141064 0.031 Uiso 1 1 calc R . . . . C6C C 0.6572(3) 0.33399(19) 0.21632(19) 0.0255(5) Uani 1 1 d . . . . . H6C H 0.658938 0.267341 0.214252 0.031 Uiso 1 1 calc R . . . . C7A C 0.7578(2) 0.72359(18) 0.40081(16) 0.0197(5) Uani 1 1 d . . . . . C7B C 0.8917(2) 0.79290(18) 0.13053(17) 0.0206(5) Uani 1 1 d . . . . . C7C C 0.5365(2) 0.35127(18) 0.20070(16) 0.0199(5) Uani 1 1 d . . . . . C8 C 0.4117(3) 0.26168(19) 0.18218(18) 0.0248(5) Uani 1 1 d . . . . . C8A C 0.8814(2) 0.7850(2) 0.45725(17) 0.0233(5) Uani 1 1 d . . . . . C8B C 1.0359(2) 0.8212(2) 0.11096(19) 0.0266(5) Uani 1 1 d . . . . . C9A C 0.8611(3) 0.8040(3) 0.55649(19) 0.0400(7) Uani 1 1 d . . . . . H9AA H 0.801079 0.842310 0.560530 0.060 Uiso 1 1 calc GR . . . . H9AB H 0.942253 0.841328 0.587717 0.060 Uiso 1 1 calc GR . . . . H9AC H 0.827147 0.740446 0.583517 0.060 Uiso 1 1 calc GR . . . . C9B C 1.1049(3) 0.9353(2) 0.1163(3) 0.0447(8) Uani 1 1 d . . . . . H9BA H 1.064340 0.967033 0.072116 0.067 Uiso 1 1 calc GR . . . . H9BB H 1.194110 0.947386 0.104632 0.067 Uiso 1 1 calc GR . . . . H9BC H 1.099560 0.963165 0.175482 0.067 Uiso 1 1 calc GR . . . . C10A C 0.9307(3) 0.8865(2) 0.4128(2) 0.0360(7) Uani 1 1 d . . . . . H10A H 0.941777 0.874235 0.350245 0.054 Uiso 1 1 calc GR . . . . H10B H 1.012034 0.925506 0.442682 0.054 Uiso 1 1 calc GR . . . . H10C H 0.868935 0.923076 0.417663 0.054 Uiso 1 1 calc GR . . . . C10B C 1.0427(3) 0.7771(3) 0.0162(2) 0.0448(8) Uani 1 1 d . . . . . H10D H 0.998032 0.705783 0.012512 0.067 Uiso 1 1 calc GR . . . . H10E H 1.131604 0.788022 0.004126 0.067 Uiso 1 1 calc GR . . . . H10F H 1.002871 0.809821 -0.027520 0.067 Uiso 1 1 calc GR . . . . C11A C 0.9817(3) 0.7281(3) 0.4517(2) 0.0365(7) Uani 1 1 d . . . . . H11A H 0.949933 0.663632 0.477705 0.055 Uiso 1 1 calc GR . . . . H11B H 1.061102 0.766971 0.484199 0.055 Uiso 1 1 calc GR . . . . H11C H 0.997097 0.717869 0.389590 0.055 Uiso 1 1 calc GR . . . . C11B C 1.1029(3) 0.7714(3) 0.1803(2) 0.0397(7) Uani 1 1 d . . . . . H11D H 1.101377 0.800860 0.239518 0.060 Uiso 1 1 calc GR . . . . H11E H 1.190896 0.781868 0.166292 0.060 Uiso 1 1 calc GR . . . . H11F H 1.058345 0.700089 0.178744 0.060 Uiso 1 1 calc GR . . . . C9C C 0.4039(6) 0.1796(5) 0.2501(5) 0.049(2) Uani 0.584(9) 1 d . . P A 1 H9CA H 0.478375 0.156317 0.247501 0.074 Uiso 0.584(9) 1 calc GR . P A 1 H9CB H 0.326912 0.123893 0.235428 0.074 Uiso 0.584(9) 1 calc GR . P A 1 H9CC H 0.401404 0.207187 0.309889 0.074 Uiso 0.584(9) 1 calc GR . P A 1 C10C C 0.4139(8) 0.2166(6) 0.0879(5) 0.063(3) Uani 0.584(9) 1 d . . P A 1 H10G H 0.405285 0.263868 0.044145 0.094 Uiso 0.584(9) 1 calc GR . P A 1 H10H H 0.343536 0.155015 0.077532 0.094 Uiso 0.584(9) 1 calc GR . P A 1 H10I H 0.494375 0.202296 0.082383 0.094 Uiso 0.584(9) 1 calc GR . P A 1 C11C C 0.2917(5) 0.2965(5) 0.1891(8) 0.067(3) Uani 0.584(9) 1 d . . P A 1 H11G H 0.293190 0.327090 0.248281 0.100 Uiso 0.584(9) 1 calc GR . P A 1 H11H H 0.215390 0.239216 0.178756 0.100 Uiso 0.584(9) 1 calc GR . P A 1 H11I H 0.291032 0.344940 0.144671 0.100 Uiso 0.584(9) 1 calc GR . P A 1 C5 C 0.3475(11) 0.2754(9) 0.0909(7) 0.066(4) Uani 0.416(9) 1 d . . P A 2 H5A H 0.329927 0.339249 0.092755 0.099 Uiso 0.416(9) 1 calc GR . P A 2 H5B H 0.267938 0.221637 0.078686 0.099 Uiso 0.416(9) 1 calc GR . P A 2 H5C H 0.404483 0.274088 0.044229 0.099 Uiso 0.416(9) 1 calc GR . P A 2 C6 C 0.3270(9) 0.2676(9) 0.2566(7) 0.060(4) Uani 0.416(9) 1 d . . P A 2 H6D H 0.370370 0.262267 0.313496 0.090 Uiso 0.416(9) 1 calc GR . P A 2 H6E H 0.247424 0.213189 0.247697 0.090 Uiso 0.416(9) 1 calc GR . P A 2 H6F H 0.308812 0.331154 0.256331 0.090 Uiso 0.416(9) 1 calc GR . P A 2 C9CA C 0.4367(9) 0.1588(6) 0.1765(12) 0.075(5) Uani 0.416(9) 1 d . . P A 2 H9CD H 0.500525 0.160295 0.134074 0.113 Uiso 0.416(9) 1 calc GR . P A 2 H9CE H 0.357711 0.107012 0.156877 0.113 Uiso 0.416(9) 1 calc GR . P A 2 H9CF H 0.467439 0.144482 0.234848 0.113 Uiso 0.416(9) 1 calc GR . P A 2 O0AA O 0.5252(5) 1.0057(5) 0.5399(4) 0.135(2) Uani 1 1 d D U . . . C1S C 0.6583(7) 1.0211(7) 0.5348(6) 0.125(3) Uani 1 1 d D U . . . H1SA H 0.675098 0.962585 0.506647 0.150 Uiso 1 1 calc R . . . . H1SB H 0.698225 1.080505 0.502087 0.150 Uiso 1 1 calc R . . . . C2S C 0.6992(10) 1.0343(7) 0.6224(7) 0.158(3) Uani 1 1 d D U . . . H2SA H 0.791959 1.052791 0.628312 0.237 Uiso 1 1 calc GR . . . . H2SB H 0.663502 0.972504 0.651740 0.237 Uiso 1 1 calc GR . . . . H2SC H 0.671510 1.087139 0.649917 0.237 Uiso 1 1 calc GR . . . . 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 0.01137(6) 0.01220(6) 0.01515(6) -0.00339(4) -0.00054(4) 0.00253(4) O1A 0.0154(8) 0.0258(9) 0.0217(9) -0.0051(7) 0.0020(7) 0.0022(7) O1B 0.0176(8) 0.0164(8) 0.0351(10) 0.0027(7) 0.0042(7) 0.0040(7) O1C 0.0170(8) 0.0167(8) 0.0278(9) -0.0010(7) -0.0033(7) 0.0041(7) O2A 0.0171(8) 0.0330(10) 0.0217(9) -0.0117(7) 0.0000(7) 0.0035(7) O2B 0.0182(8) 0.0176(8) 0.0282(9) -0.0024(7) 0.0058(7) 0.0036(7) O2C 0.0161(8) 0.0153(8) 0.0315(10) -0.0018(7) 0.0004(7) 0.0033(7) N1 0.0175(10) 0.0178(9) 0.0174(10) -0.0038(8) -0.0001(7) 0.0070(8) N2 0.0139(9) 0.0218(10) 0.0168(10) -0.0032(8) 0.0002(7) 0.0056(8) C1 0.0135(11) 0.0143(10) 0.0151(10) 0.0006(8) 0.0006(8) 0.0033(8) C1A 0.0349(12) 0.095(2) 0.0787(18) 0.0064(15) 0.0217(11) 0.0147(12) C1B 0.066(3) 0.0399(19) 0.087(3) 0.030(2) 0.031(2) 0.0314(19) C1C 0.0373(19) 0.0335(18) 0.104(3) 0.0076(19) -0.0175(19) 0.0199(15) C2 0.0142(11) 0.0299(13) 0.0219(12) -0.0015(10) 0.0003(9) 0.0075(10) C2A 0.0349(12) 0.095(2) 0.0787(18) 0.0064(15) 0.0217(11) 0.0147(12) C2B 0.0319(17) 0.0313(17) 0.108(3) 0.0049(19) 0.0052(19) 0.0177(14) C2C 0.0304(16) 0.062(2) 0.0480(19) 0.0107(16) 0.0104(14) 0.0268(16) C3 0.0191(12) 0.0299(13) 0.0262(13) -0.0036(10) 0.0031(10) 0.0124(10) C3A 0.0349(12) 0.095(2) 0.0787(18) 0.0064(15) 0.0217(11) 0.0147(12) C3B 0.085(3) 0.056(2) 0.059(2) -0.0199(19) -0.006(2) 0.046(2) C3C 0.0284(15) 0.057(2) 0.0361(16) 0.0052(14) -0.0096(12) 0.0151(14) C4 0.0215(12) 0.0256(12) 0.0207(12) -0.0055(10) 0.0020(9) 0.0116(10) C4A 0.0187(13) 0.0555(19) 0.0307(15) -0.0048(13) 0.0103(11) 0.0027(12) C4B 0.0278(14) 0.0183(12) 0.0392(15) 0.0026(11) 0.0061(11) 0.0095(10) C4C 0.0214(13) 0.0257(13) 0.0366(15) 0.0051(11) -0.0019(11) 0.0104(10) C5A 0.0196(12) 0.0244(12) 0.0205(12) -0.0012(10) 0.0058(9) 0.0046(10) C5B 0.0247(13) 0.0166(11) 0.0245(12) -0.0005(9) 0.0013(10) 0.0065(10) C5C 0.0211(12) 0.0213(12) 0.0197(12) 0.0000(9) -0.0002(9) 0.0091(10) C6A 0.0235(13) 0.0340(14) 0.0179(12) -0.0078(10) 0.0021(10) 0.0045(11) C6B 0.0214(12) 0.0152(11) 0.0385(15) 0.0011(10) 0.0046(11) 0.0006(10) C6C 0.0234(13) 0.0147(11) 0.0375(15) -0.0002(10) -0.0020(11) 0.0055(10) C7A 0.0201(12) 0.0206(12) 0.0165(11) -0.0029(9) -0.0020(9) 0.0046(9) C7B 0.0175(11) 0.0194(12) 0.0216(12) -0.0005(9) 0.0027(9) 0.0009(9) C7C 0.0212(12) 0.0164(11) 0.0197(12) -0.0010(9) 0.0009(9) 0.0024(9) C8 0.0224(13) 0.0178(12) 0.0299(14) 0.0001(10) -0.0012(10) 0.0002(10) C8A 0.0209(12) 0.0264(13) 0.0191(12) -0.0077(10) -0.0048(9) 0.0038(10) C8B 0.0176(12) 0.0245(13) 0.0349(15) 0.0020(11) 0.0084(10) 0.0011(10) C9A 0.0354(16) 0.057(2) 0.0207(14) -0.0140(13) -0.0053(12) 0.0059(14) C9B 0.0235(15) 0.0284(16) 0.076(2) 0.0029(15) 0.0137(15) -0.0025(12) C10A 0.0348(16) 0.0256(14) 0.0378(16) -0.0045(12) -0.0059(12) -0.0032(12) C10B 0.0336(17) 0.054(2) 0.0423(18) -0.0025(15) 0.0194(14) 0.0035(15) C11A 0.0260(14) 0.0441(17) 0.0381(16) -0.0090(13) -0.0114(12) 0.0124(13) C11B 0.0214(14) 0.0453(18) 0.053(2) 0.0080(15) 0.0015(13) 0.0111(13) C9C 0.039(3) 0.035(3) 0.057(4) 0.021(3) -0.007(3) -0.013(3) C10C 0.064(5) 0.056(5) 0.039(4) -0.020(3) -0.005(3) -0.021(4) C11C 0.015(3) 0.036(3) 0.142(10) -0.001(4) 0.003(4) -0.002(2) C5 0.062(7) 0.055(6) 0.044(5) 0.018(5) -0.029(5) -0.036(5) C6 0.033(5) 0.069(7) 0.054(6) -0.009(5) 0.019(4) -0.021(5) C9CA 0.032(5) 0.021(4) 0.162(16) 0.001(6) -0.005(6) -0.006(3) O0AA 0.101(4) 0.129(4) 0.188(6) 0.019(5) 0.057(4) 0.046(3) C1S 0.108(5) 0.134(6) 0.150(5) -0.002(5) 0.043(4) 0.056(4) C2S 0.149(6) 0.146(7) 0.175(6) -0.005(6) 0.020(5) 0.038(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1A Dy1 O1B 79.14(6) . . O1A Dy1 O2C 76.98(6) . . O1A Dy1 N1 83.15(6) . . O1A Dy1 N2 139.83(6) . 2_665 O1B Dy1 O2C 134.22(6) . . O1B Dy1 N1 69.82(6) . . O1B Dy1 N2 105.08(6) . 2_665 O1C Dy1 O1A 117.30(6) . . O1C Dy1 O1B 153.00(6) . . O1C Dy1 O2B 82.55(6) . . O1C Dy1 O2C 72.47(6) . . O1C Dy1 N1 130.26(6) . . O1C Dy1 N2 76.75(6) . 2_665 O2A Dy1 O1A 74.08(6) . . O2A Dy1 O1B 84.90(7) . . O2A Dy1 O1C 80.00(6) . . O2A Dy1 O2B 80.71(6) . . O2A Dy1 O2C 124.09(7) . . O2A Dy1 N1 148.77(6) . . O2A Dy1 N2 145.43(6) . 2_665 O2B Dy1 O1A 143.74(6) . . O2B Dy1 O1B 72.96(6) . . O2B Dy1 O2C 139.28(6) . . O2B Dy1 N1 107.68(6) . . O2B Dy1 N2 71.25(6) . 2_665 O2C Dy1 N1 69.00(6) . . O2C Dy1 N2 72.02(6) . 2_665 N1 Dy1 N2 62.35(6) . 2_665 C5A O1A Dy1 135.83(16) . . C5B O1B Dy1 133.54(16) . . C5C O1C Dy1 137.96(16) . . C7A O2A Dy1 137.51(16) . . C7B O2B Dy1 132.80(15) . . C7C O2C Dy1 136.93(16) . . C1 N1 Dy1 121.32(15) . . C1 N1 C4 116.4(2) . . C4 N1 Dy1 121.45(15) . . C1 N2 Dy1 120.84(15) . 2_665 C1 N2 C2 116.5(2) . . C2 N2 Dy1 121.84(15) . 2_665 N1 C1 C1 117.0(2) . 2_665 N2 C1 N1 126.4(2) . . N2 C1 C1 116.7(2) . 2_665 H1AA C1A H1AB 109.5 . . H1AA C1A H1AC 109.5 . . H1AB C1A H1AC 109.5 . . C4A C1A H1AA 109.5 . . C4A C1A H1AB 109.5 . . C4A C1A H1AC 109.5 . . H1BA C1B H1BB 109.5 . . H1BA C1B H1BC 109.5 . . H1BB C1B H1BC 109.5 . . C4B C1B H1BA 109.5 . . C4B C1B H1BB 109.5 . . C4B C1B H1BC 109.5 . . H1CA C1C H1CB 109.5 . . H1CA C1C H1CC 109.5 . . H1CB C1C H1CC 109.5 . . C4C C1C H1CA 109.5 . . C4C C1C H1CB 109.5 . . C4C C1C H1CC 109.5 . . N2 C2 H2 119.2 . . N2 C2 C3 121.6(2) . . C3 C2 H2 119.2 . . H2AA C2A H2AB 109.5 . . H2AA C2A H2AC 109.5 . . H2AB C2A H2AC 109.5 . . C4A C2A H2AA 109.5 . . C4A C2A H2AB 109.5 . . C4A C2A H2AC 109.5 . . H2BA C2B H2BB 109.5 . . H2BA C2B H2BC 109.5 . . H2BB C2B H2BC 109.5 . . C4B C2B H2BA 109.5 . . C4B C2B H2BB 109.5 . . C4B C2B H2BC 109.5 . . H2CA C2C H2CB 109.5 . . H2CA C2C H2CC 109.5 . . H2CB C2C H2CC 109.5 . . C4C C2C H2CA 109.5 . . C4C C2C H2CB 109.5 . . C4C C2C H2CC 109.5 . . C2 C3 H3 121.3 . . C4 C3 C2 117.4(2) . . C4 C3 H3 121.3 . . H3AA C3A H3AB 109.5 . . H3AA C3A H3AC 109.5 . . H3AB C3A H3AC 109.5 . . C4A C3A H3AA 109.5 . . C4A C3A H3AB 109.5 . . C4A C3A H3AC 109.5 . . H3BA C3B H3BB 109.5 . . H3BA C3B H3BC 109.5 . . H3BB C3B H3BC 109.5 . . C4B C3B H3BA 109.5 . . C4B C3B H3BB 109.5 . . C4B C3B H3BC 109.5 . . H3CA C3C H3CB 109.5 . . H3CA C3C H3CC 109.5 . . H3CB C3C H3CC 109.5 . . C4C C3C H3CA 109.5 . . C4C C3C H3CB 109.5 . . C4C C3C H3CC 109.5 . . N1 C4 C3 121.7(2) . . N1 C4 H4 119.1 . . C3 C4 H4 119.1 . . C1A C4A C2A 111.5(3) . . C1A C4A C3A 107.7(3) . . C1A C4A C5A 107.5(3) . . C2A C4A C5A 113.6(3) . . C3A C4A C2A 107.4(3) . . C3A C4A C5A 108.9(3) . . C1B C4B C5B 112.3(2) . . C2B C4B C1B 108.9(3) . . C2B C4B C5B 110.2(2) . . C3B C4B C1B 108.9(3) . . C3B C4B C2B 109.2(3) . . C3B C4B C5B 107.2(2) . . C1C C4C C2C 109.4(3) . . C1C C4C C3C 109.4(3) . . C1C C4C C5C 114.2(2) . . C2C C4C C3C 108.5(3) . . C2C C4C C5C 108.2(2) . . C3C C4C C5C 107.0(2) . . O1A C5A C4A 115.1(2) . . O1A C5A C6A 124.4(2) . . C6A C5A C4A 120.4(2) . . O1B C5B C4B 116.3(2) . . O1B C5B C6B 123.9(2) . . C6B C5B C4B 119.7(2) . . O1C C5C C4C 114.5(2) . . O1C C5C C6C 124.1(2) . . C6C C5C C4C 121.5(2) . . C5A C6A H6A 118.0 . . C7A C6A C5A 124.0(2) . . C7A C6A H6A 118.0 . . C5B C6B H6B 117.9 . . C7B C6B C5B 124.2(2) . . C7B C6B H6B 117.9 . . C5C C6C H6C 118.0 . . C5C C6C C7C 124.0(2) . . C7C C6C H6C 118.0 . . O2A C7A C6A 124.1(2) . . O2A C7A C8A 114.2(2) . . C6A C7A C8A 121.6(2) . . O2B C7B C6B 124.3(2) . . O2B C7B C8B 114.4(2) . . C6B C7B C8B 121.3(2) . . O2C C7C C6C 123.5(2) . . O2C C7C C8 116.0(2) . . C6C C7C C8 120.5(2) . . C9C C8 C7C 111.5(3) . . C10C C8 C7C 107.6(3) . . C10C C8 C9C 108.8(5) . . C10C C8 C11C 110.4(6) . . C11C C8 C7C 111.0(3) . . C11C C8 C9C 107.5(5) . . C5 C8 C7C 107.8(4) . . C6 C8 C7C 106.4(4) . . C6 C8 C5 110.5(8) . . C6 C8 C9CA 111.3(8) . . C9CA C8 C7C 113.1(4) . . C9CA C8 C5 107.6(8) . . C9A C8A C7A 114.1(2) . . C9A C8A C10A 109.6(2) . . C9A C8A C11A 109.1(2) . . C10A C8A C7A 106.3(2) . . C11A C8A C7A 108.4(2) . . C11A C8A C10A 109.3(2) . . C9B C8B C7B 113.9(2) . . C10B C8B C7B 107.4(2) . . C10B C8B C9B 109.5(3) . . C11B C8B C7B 107.4(2) . . C11B C8B C9B 109.0(3) . . C11B C8B C10B 109.5(3) . . C8A C9A H9AA 109.5 . . C8A C9A H9AB 109.5 . . C8A C9A H9AC 109.5 . . H9AA C9A H9AB 109.5 . . H9AA C9A H9AC 109.5 . . H9AB C9A H9AC 109.5 . . C8B C9B H9BA 109.5 . . C8B C9B H9BB 109.5 . . C8B C9B H9BC 109.5 . . H9BA C9B H9BB 109.5 . . H9BA C9B H9BC 109.5 . . H9BB C9B H9BC 109.5 . . C8A C10A H10A 109.5 . . C8A C10A H10B 109.5 . . C8A C10A H10C 109.5 . . H10A C10A H10B 109.5 . . H10A C10A H10C 109.5 . . H10B C10A H10C 109.5 . . C8B C10B H10D 109.5 . . C8B C10B H10E 109.5 . . C8B C10B H10F 109.5 . . H10D C10B H10E 109.5 . . H10D C10B H10F 109.5 . . H10E C10B H10F 109.5 . . C8A C11A H11A 109.5 . . C8A C11A H11B 109.5 . . C8A C11A H11C 109.5 . . H11A C11A H11B 109.5 . . H11A C11A H11C 109.5 . . H11B C11A H11C 109.5 . . C8B C11B H11D 109.5 . . C8B C11B H11E 109.5 . . C8B C11B H11F 109.5 . . H11D C11B H11E 109.5 . . H11D C11B H11F 109.5 . . H11E C11B H11F 109.5 . . C8 C9C H9CA 109.5 . . C8 C9C H9CB 109.5 . . C8 C9C H9CC 109.5 . . H9CA C9C H9CB 109.5 . . H9CA C9C H9CC 109.5 . . H9CB C9C H9CC 109.5 . . C8 C10C H10G 109.5 . . C8 C10C H10H 109.5 . . C8 C10C H10I 109.5 . . H10G C10C H10H 109.5 . . H10G C10C H10I 109.5 . . H10H C10C H10I 109.5 . . C8 C11C H11G 109.5 . . C8 C11C H11H 109.5 . . C8 C11C H11I 109.5 . . H11G C11C H11H 109.5 . . H11G C11C H11I 109.5 . . H11H C11C H11I 109.5 . . C8 C5 H5A 109.5 . . C8 C5 H5B 109.5 . . C8 C5 H5C 109.5 . . H5A C5 H5B 109.5 . . H5A C5 H5C 109.5 . . H5B C5 H5C 109.5 . . C8 C6 H6D 109.5 . . C8 C6 H6E 109.5 . . C8 C6 H6F 109.5 . . H6D C6 H6E 109.5 . . H6D C6 H6F 109.5 . . H6E C6 H6F 109.5 . . C8 C9CA H9CD 109.5 . . C8 C9CA H9CE 109.5 . . C8 C9CA H9CF 109.5 . . H9CD C9CA H9CE 109.5 . . H9CD C9CA H9CF 109.5 . . H9CE C9CA H9CF 109.5 . . O0AA O0AA C1S 107.3(7) 2_676 . O0AA C1S H1SA 111.6 . . O0AA C1S H1SB 111.6 . . H1SA C1S H1SB 109.4 . . C2S C1S O0AA 101.0(7) . . C2S C1S H1SA 111.6 . . C2S C1S H1SB 111.6 . . C1S C2S H2SA 109.5 . . C1S C2S H2SB 109.5 . . C1S C2S H2SC 109.5 . . H2SA C2S H2SB 109.5 . . H2SA C2S H2SC 109.5 . . H2SB C2S H2SC 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy1 O1A 2.2988(17) . Dy1 O1B 2.3250(17) . Dy1 O1C 2.2964(17) . Dy1 O2A 2.2639(17) . Dy1 O2B 2.2982(17) . Dy1 O2C 2.3340(17) . Dy1 N1 2.5874(19) . Dy1 N2 2.6092(19) 2_665 O1A C5A 1.266(3) . O1B C5B 1.261(3) . O1C C5C 1.270(3) . O2A C7A 1.261(3) . O2B C7B 1.271(3) . O2C C7C 1.261(3) . N1 C1 1.335(3) . N1 C4 1.337(3) . N2 C1 1.331(3) . N2 C2 1.339(3) . C1 C1 1.487(4) 2_665 C1A H1AA 0.9600 . C1A H1AB 0.9600 . C1A H1AC 0.9600 . C1A C4A 1.510(6) . C1B H1BA 0.9600 . C1B H1BB 0.9600 . C1B H1BC 0.9600 . C1B C4B 1.529(4) . C1C H1CA 0.9600 . C1C H1CB 0.9600 . C1C H1CC 0.9600 . C1C C4C 1.519(4) . C2 H2 0.9300 . C2 C3 1.382(3) . C2A H2AA 0.9600 . C2A H2AB 0.9600 . C2A H2AC 0.9600 . C2A C4A 1.520(5) . C2B H2BA 0.9600 . C2B H2BB 0.9600 . C2B H2BC 0.9600 . C2B C4B 1.526(4) . C2C H2CA 0.9600 . C2C H2CB 0.9600 . C2C H2CC 0.9600 . C2C C4C 1.530(4) . C3 H3 0.9300 . C3 C4 1.382(4) . C3A H3AA 0.9600 . C3A H3AB 0.9600 . C3A H3AC 0.9600 . C3A C4A 1.518(6) . C3B H3BA 0.9600 . C3B H3BB 0.9600 . C3B H3BC 0.9600 . C3B C4B 1.526(5) . C3C H3CA 0.9600 . C3C H3CB 0.9600 . C3C H3CC 0.9600 . C3C C4C 1.530(4) . C4 H4 0.9300 . C4A C5A 1.541(3) . C4B C5B 1.541(3) . C4C C5C 1.538(3) . C5A C6A 1.402(4) . C5B C6B 1.405(4) . C5C C6C 1.395(4) . C6A H6A 0.9300 . C6A C7A 1.398(4) . C6B H6B 0.9300 . C6B C7B 1.392(4) . C6C H6C 0.9300 . C6C C7C 1.410(4) . C7A C8A 1.537(3) . C7B C8B 1.544(3) . C7C C8 1.542(3) . C8 C9C 1.535(6) . C8 C10C 1.519(7) . C8 C11C 1.529(7) . C8 C5 1.533(9) . C8 C6 1.495(9) . C8 C9CA 1.532(10) . C8A C9A 1.529(4) . C8A C10A 1.535(4) . C8A C11A 1.531(4) . C8B C9B 1.531(4) . C8B C10B 1.531(4) . C8B C11B 1.528(4) . C9A H9AA 0.9600 . C9A H9AB 0.9600 . C9A H9AC 0.9600 . C9B H9BA 0.9600 . C9B H9BB 0.9600 . C9B H9BC 0.9600 . C10A H10A 0.9600 . C10A H10B 0.9600 . C10A H10C 0.9600 . C10B H10D 0.9600 . C10B H10E 0.9600 . C10B H10F 0.9600 . C11A H11A 0.9600 . C11A H11B 0.9600 . C11A H11C 0.9600 . C11B H11D 0.9600 . C11B H11E 0.9600 . C11B H11F 0.9600 . C9C H9CA 0.9600 . C9C H9CB 0.9600 . C9C H9CC 0.9600 . C10C H10G 0.9600 . C10C H10H 0.9600 . C10C H10I 0.9600 . C11C H11G 0.9600 . C11C H11H 0.9600 . C11C H11I 0.9600 . C5 H5A 0.9600 . C5 H5B 0.9600 . C5 H5C 0.9600 . C6 H6D 0.9600 . C6 H6E 0.9600 . C6 H6F 0.9600 . C9CA H9CD 0.9600 . C9CA H9CE 0.9600 . C9CA H9CF 0.9600 . O0AA O0AA 1.260(11) 2_676 O0AA C1S 1.405(8) . C1S H1SA 0.9700 . C1S H1SB 0.9700 . C1S C2S 1.338(10) . C2S H2SA 0.9600 . C2S H2SB 0.9600 . C2S H2SC 0.9600 .