#------------------------------------------------------------------------------ #$Date: 2019-04-16 01:16:54 +0300 (Tue, 16 Apr 2019) $ #$Revision: 214637 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/08/1550884.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_1550884 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 92.039(2) _cell_angle_beta 93.333(2) _cell_angle_gamma 107.553(2) _cell_formula_units_Z 1 _cell_length_a 10.8743(2) _cell_length_b 13.8790(3) _cell_length_c 14.8618(4) _cell_measurement_reflns_used 21010 _cell_measurement_temperature 180 _cell_measurement_theta_max 27.2550 _cell_measurement_theta_min 1.9900 _cell_volume 2131.63(9) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (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 0.995 _diffrn_measured_fraction_theta_max 0.996 _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 -- 0.00 180.00 252.00 180 2 \w -90.00 20.00 1.00 180.60 -- 0.00 180.00 64.00 110' _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 -0.0032390000 _diffrn_orient_matrix_UB_12 -0.0277168000 _diffrn_orient_matrix_UB_13 0.0394425000 _diffrn_orient_matrix_UB_21 0.0507811000 _diffrn_orient_matrix_UB_22 -0.0180126000 _diffrn_orient_matrix_UB_23 -0.0139204000 _diffrn_orient_matrix_UB_31 0.0459961000 _diffrn_orient_matrix_UB_32 0.0423019000 _diffrn_orient_matrix_UB_33 0.0233063000 _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 0.0289 _diffrn_reflns_av_unetI/netI 0.0283 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 13 _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 25289 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.371 _diffrn_reflns_theta_min 4.080 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.797 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.88031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro 1.171.38.43 (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 1.303 _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 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.256 _refine_diff_density_min -1.252 _refine_diff_density_rms 0.086 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 467 _refine_ls_number_reflns 8697 _refine_ls_number_restraints 41 _refine_ls_restrained_S_all 1.105 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0256 _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^)+(0.0297P)^2^+2.3589P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.0645 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8350 _reflns_number_total 8697 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL em1-118_a.res in P-1 em1-118.res created by SHELXL-2017/1 at 14:50:35 on 11-Feb-2019 REM Old TITL EM1-118 in P-1 REM SHELXT solution in P-1 REM R1 0.069, Rweak 0.013, Alpha 0.043, Orientation as input REM Formula found by SHELXT: C75 N4 O12 Dy2 CELL 0.71073 10.8743 13.879 14.8618 92.039 93.333 107.553 ZERR 1 0.0002 0.0003 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H Dy N O UNIT 78 130 2 4 14 DFIX 1.54 C1AA C5 DFIX 1.1 C5 O0AA SADI C2C C4C C4C C3C C3C C4C C4C C1C C1C C4C C4C C2C SADI C2C C3C C3C C1C C3C C1C C1C C2C C1C C2C C2C C3C SADI C2CA C4C C4C C3CA C3CA C4C C4C C1CA C1CA C4C C4C C2CA SADI C2CA C3CA C3CA C1CA C3CA C1CA C1CA C2CA C1CA C2CA C2CA C3CA RIGU C1C C1CA C2C C3C C3CA RIGU O0AA C1AA C5 RIGU C11B C9B C10B C8B EADP C1CA C2CA C3CA EADP C9B C11B C10B L.S. 10 PLAN 20 list 4 fmap 2 acta SHEL 5 0.8 OMIT -8 7 4 OMIT -7 6 3 OMIT -10 8 6 REM REM REM WGHT 0.029700 2.358900 FVAR 0.45108 0.64902 DY1 3 0.657425 0.605189 0.200696 11.00000 0.01261 0.01345 = 0.01637 -0.00282 0.00005 0.00296 O1A 5 0.835935 0.698408 0.132270 11.00000 0.01901 0.01865 = 0.02826 -0.00122 0.00646 0.00288 O1B 5 0.777208 0.691721 0.324066 11.00000 0.01910 0.03459 = 0.02323 -0.01110 0.00101 0.00401 O1C 5 0.522953 0.438437 0.200103 11.00000 0.01734 0.01712 = 0.03401 0.00010 0.00097 0.00420 O2A 5 0.624196 0.758611 0.168369 11.00000 0.01914 0.01678 = 0.03649 0.00170 0.00360 0.00504 O2B 5 0.512254 0.614426 0.304715 11.00000 0.01743 0.02595 = 0.02398 -0.00511 0.00283 0.00285 O2C 5 0.786080 0.504643 0.231104 11.00000 0.01802 0.02087 = 0.02925 0.00024 -0.00269 0.00542 N1 4 0.458236 0.575174 0.087284 11.00000 0.01902 0.01706 = 0.01852 -0.00237 0.00170 0.00662 N2 4 0.337251 0.483176 -0.043679 11.00000 0.01496 0.02184 = 0.01803 -0.00255 0.00093 0.00534 C1 1 0.443544 0.515972 0.012187 11.00000 0.01549 0.01463 = 0.01549 -0.00058 -0.00047 0.00286 C1A 1 1.102582 0.771317 0.180487 11.00000 0.02273 0.04480 = 0.05352 0.00546 0.00273 0.00997 AFIX 137 H1AA 2 1.190860 0.782456 0.166878 11.00000 -1.50000 H1AB 2 1.058683 0.699921 0.178482 11.00000 -1.50000 H1AC 2 1.100225 0.800360 0.239717 11.00000 -1.50000 AFIX 0 C1B 1 0.861586 0.804366 0.556534 11.00000 0.03914 0.05743 = 0.02299 -0.01186 -0.00566 0.00694 AFIX 137 H1BA 2 0.942596 0.842181 0.587631 11.00000 -1.50000 H1BB 2 0.828361 0.740805 0.583685 11.00000 -1.50000 H1BC 2 0.801066 0.842119 0.560567 11.00000 -1.50000 AFIX 0 PART 1 C1C 1 0.411353 0.218591 0.087924 21.00000 0.07104 0.08636 = 0.04292 -0.02731 0.00493 -0.04338 AFIX 137 H1CA 2 0.343672 0.155305 0.078771 21.00000 -1.50000 H1CB 2 0.493197 0.207830 0.079556 21.00000 -1.50000 H1CC 2 0.396793 0.265020 0.045243 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C1CA 1 0.345992 0.277980 0.092642 -21.00000 0.03320 0.03722 = 0.06075 -0.00102 -0.00227 -0.01316 AFIX 137 H1CD 2 0.327735 0.341426 0.096763 -21.00000 -1.50000 H1CE 2 0.266690 0.224020 0.079945 -21.00000 -1.50000 H1CF 2 0.402194 0.278590 0.045043 -21.00000 -1.50000 AFIX 0 PART 0 C2 1 0.235272 0.511537 -0.021242 11.00000 0.01505 0.02885 = 0.02207 -0.00190 -0.00054 0.00690 AFIX 43 H2 2 0.158515 0.488843 -0.057612 11.00000 -1.20000 AFIX 0 C2A 1 1.104928 0.935327 0.116390 11.00000 0.02380 0.03228 = 0.07520 0.00370 0.01408 -0.00168 AFIX 137 H2AA 2 1.098673 0.963316 0.175335 11.00000 -1.50000 H2AB 2 1.065177 0.966930 0.071724 11.00000 -1.50000 H2AC 2 1.194316 0.947255 0.105495 11.00000 -1.50000 AFIX 0 C2B 1 0.931048 0.886577 0.413003 11.00000 0.03640 0.02824 = 0.03860 -0.00455 -0.00512 -0.00215 AFIX 137 H2BA 2 0.869827 0.923500 0.418499 11.00000 -1.50000 H2BB 2 0.941255 0.874362 0.350300 11.00000 -1.50000 H2BC 2 1.012848 0.925319 0.442469 11.00000 -1.50000 AFIX 0 PART 1 C2C 1 0.292961 0.297086 0.191298 21.00000 0.02089 0.03852 = 0.19091 -0.00632 0.00377 -0.00378 AFIX 137 H2CA 2 0.298857 0.331316 0.249407 21.00000 -1.50000 H2CB 2 0.216593 0.239549 0.185292 21.00000 -1.50000 H2CC 2 0.288565 0.342545 0.144880 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C2CA 1 0.329426 0.265552 0.259068 -21.00000 0.03320 0.03722 = 0.06075 -0.00102 -0.00227 -0.01316 AFIX 137 H2CD 2 0.371389 0.253184 0.314148 -21.00000 -1.50000 H2CE 2 0.247012 0.214722 0.247835 -21.00000 -1.50000 H2CF 2 0.317093 0.331105 0.264332 -21.00000 -1.50000 AFIX 0 PART 0 C3 1 0.241350 0.573627 0.054550 11.00000 0.01957 0.03286 = 0.02694 -0.00201 0.00391 0.01315 AFIX 43 H3 2 0.170526 0.593703 0.069476 11.00000 -1.20000 AFIX 0 C3A 1 1.042784 0.776797 0.016109 11.00000 0.03742 0.05581 = 0.03929 -0.00388 0.01998 0.00591 AFIX 137 H3AA 2 1.131691 0.788696 0.003834 11.00000 -1.50000 H3AB 2 1.001849 0.808691 -0.027592 11.00000 -1.50000 H3AC 2 0.999297 0.705294 0.012691 11.00000 -1.50000 AFIX 0 C3B 1 0.981183 0.727875 0.451451 11.00000 0.02952 0.04640 = 0.03968 -0.00722 -0.01235 0.01359 AFIX 137 H3BA 2 1.061447 0.767273 0.482545 11.00000 -1.50000 H3BB 2 0.994543 0.716034 0.389260 11.00000 -1.50000 H3BC 2 0.949987 0.664261 0.478864 11.00000 -1.50000 AFIX 0 PART 1 C3C 1 0.405390 0.178581 0.248122 21.00000 0.04834 0.04121 = 0.07800 0.03349 -0.01635 -0.01498 AFIX 137 H3CA 2 0.478273 0.153915 0.242508 21.00000 -1.50000 H3CB 2 0.326904 0.124056 0.234480 21.00000 -1.50000 H3CC 2 0.406861 0.205480 0.308723 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C3CA 1 0.437568 0.159208 0.173929 -21.00000 0.03320 0.03722 = 0.06075 -0.00102 -0.00227 -0.01316 AFIX 137 H3CD 2 0.498526 0.161243 0.129285 -21.00000 -1.50000 H3CE 2 0.358049 0.107201 0.156211 -21.00000 -1.50000 H3CF 2 0.472144 0.144941 0.231074 -21.00000 -1.50000 AFIX 0 PART 0 C4 1 0.356225 0.604786 0.107304 11.00000 0.02546 0.02407 = 0.02253 -0.00278 0.00377 0.01162 AFIX 43 H4 2 0.363095 0.647553 0.158206 11.00000 -1.20000 AFIX 0 C4A 1 1.035619 0.821061 0.110982 11.00000 0.02024 0.02535 = 0.03526 0.00120 0.00899 0.00154 C4B 1 0.881875 0.785236 0.457308 11.00000 0.02399 0.03052 = 0.01933 -0.00572 -0.00493 0.00426 C4C 1 0.411973 0.261872 0.182264 11.00000 0.02344 0.01899 = 0.03310 0.00171 -0.00125 -0.00029 C5A 1 0.891753 0.793122 0.130325 11.00000 0.01879 0.02279 = 0.02055 0.00018 0.00458 0.00235 C5B 1 0.758019 0.723584 0.400734 11.00000 0.02129 0.02166 = 0.01981 -0.00265 -0.00106 0.00454 C5C 1 0.536898 0.351471 0.200526 11.00000 0.02281 0.01733 = 0.02205 -0.00042 0.00063 0.00359 C6A 1 0.830477 0.866814 0.143270 11.00000 0.02442 0.01537 = 0.03911 0.00193 0.00779 0.00152 AFIX 43 H6A 2 0.879833 0.934249 0.141581 11.00000 -1.20000 AFIX 0 C6B 1 0.635242 0.707367 0.432904 11.00000 0.02462 0.03820 = 0.01903 -0.00761 0.00445 0.00524 AFIX 43 H6B 2 0.630288 0.733923 0.490443 11.00000 -1.20000 AFIX 0 C6C 1 0.657147 0.334101 0.216507 11.00000 0.02685 0.01566 = 0.03967 -0.00029 -0.00074 0.00647 AFIX 43 H6C 2 0.658746 0.267445 0.214848 11.00000 -1.20000 AFIX 0 C7A 1 0.699159 0.846029 0.158696 11.00000 0.02410 0.01834 = 0.02529 0.00049 0.00214 0.00578 C7B 1 0.519686 0.653731 0.383870 11.00000 0.02181 0.02529 = 0.02254 -0.00104 0.00529 0.00508 C7C 1 0.774108 0.410899 0.234690 11.00000 0.02227 0.02251 = 0.02182 0.00178 -0.00004 0.00819 C8A 1 0.640439 0.933795 0.168272 11.00000 0.03112 0.01915 = 0.04191 0.00435 0.00886 0.01123 C8B 1 0.388695 0.635690 0.425968 11.00000 0.01810 0.06018 = 0.03355 -0.00521 0.00930 0.00313 C8C 1 0.899978 0.386844 0.261493 11.00000 0.02289 0.02898 = 0.03815 0.00505 -0.00173 0.01232 C9A 1 0.687163 1.013430 0.099208 11.00000 0.06848 0.03960 = 0.08647 0.03134 0.03067 0.03046 AFIX 137 H9AA 2 0.779178 1.043155 0.108626 11.00000 -1.50000 H9AB 2 0.645837 1.065098 0.106239 11.00000 -1.50000 H9AC 2 0.665821 0.982058 0.039378 11.00000 -1.50000 AFIX 0 C9B 1 0.398796 0.696014 0.515385 11.00000 0.03683 0.10169 = 0.07977 0.00711 0.02324 0.01763 AFIX 137 H9BA 2 0.444451 0.669817 0.560800 11.00000 -1.50000 H9BB 2 0.313594 0.690315 0.533305 11.00000 -1.50000 H9BC 2 0.444700 0.765869 0.508317 11.00000 -1.50000 AFIX 0 C9C 1 0.999636 0.434864 0.194325 11.00000 0.03230 0.06056 = 0.04752 0.01046 0.00931 0.02735 AFIX 137 H9CA 2 0.970774 0.402944 0.135267 11.00000 -1.50000 H9CB 2 1.081348 0.425874 0.212824 11.00000 -1.50000 H9CC 2 1.009163 0.505831 0.192846 11.00000 -1.50000 AFIX 0 C10A 1 0.683368 0.983630 0.263371 11.00000 0.08678 0.05647 = 0.06210 -0.01846 -0.00221 0.04542 AFIX 137 H10A 2 0.651989 0.934781 0.307368 11.00000 -1.50000 H10B 2 0.648898 1.039095 0.271846 11.00000 -1.50000 H10C 2 0.776086 1.008205 0.270419 11.00000 -1.50000 AFIX 0 C10B 1 0.333489 0.523325 0.437073 11.00000 0.03683 0.10169 = 0.07977 0.00711 0.02324 0.01763 AFIX 137 H10D 2 0.331855 0.487110 0.380543 11.00000 -1.50000 H10E 2 0.247131 0.508704 0.455960 11.00000 -1.50000 H10F 2 0.386419 0.502799 0.481768 11.00000 -1.50000 AFIX 0 C10C 1 0.884595 0.273886 0.263473 11.00000 0.04218 0.03355 = 0.10428 0.00774 -0.01427 0.02172 AFIX 137 H10G 2 0.822640 0.243814 0.305772 11.00000 -1.50000 H10H 2 0.966382 0.264722 0.281456 11.00000 -1.50000 H10I 2 0.855094 0.242117 0.204435 11.00000 -1.50000 AFIX 0 C11A 1 0.493622 0.893700 0.158121 11.00000 0.03435 0.03466 = 0.10954 0.00552 0.00268 0.01905 AFIX 137 H11A 2 0.466449 0.858522 0.100142 11.00000 -1.50000 H11B 2 0.458459 0.949189 0.163081 11.00000 -1.50000 H11C 2 0.463253 0.848072 0.204730 11.00000 -1.50000 AFIX 0 C11B 1 0.296913 0.666509 0.361059 11.00000 0.03683 0.10169 = 0.07977 0.00711 0.02324 0.01763 AFIX 137 H11D 2 0.334681 0.735803 0.347215 11.00000 -1.50000 H11E 2 0.216845 0.659234 0.388193 11.00000 -1.50000 H11F 2 0.280919 0.624064 0.306541 11.00000 -1.50000 AFIX 0 C11C 1 0.948457 0.437922 0.355456 11.00000 0.02958 0.06092 = 0.03879 0.00455 -0.00800 0.01599 AFIX 137 H11G 2 0.958993 0.509042 0.353954 11.00000 -1.50000 H11H 2 1.030001 0.428163 0.373139 11.00000 -1.50000 H11I 2 0.886742 0.408553 0.398128 11.00000 -1.50000 AFIX 0 O0AA 5 0.526797 1.005719 0.538554 11.00000 0.08781 0.13283 = 0.25271 0.02067 0.06401 0.04120 C1AA 1 0.698535 1.032979 0.621960 11.00000 0.13513 0.15347 = 0.19528 -0.00950 0.02309 0.02728 AFIX 33 H1AD 2 0.790172 1.043757 0.627023 11.00000 -1.50000 H1AE 2 0.680205 1.090754 0.648524 11.00000 -1.50000 H1AF 2 0.655927 0.973848 0.652881 11.00000 -1.50000 AFIX 0 C5 1 0.655137 1.019659 0.533542 11.00000 0.10448 0.14312 = 0.15913 0.00248 0.05158 0.05271 AFIX 23 H5A 2 0.695272 1.078847 0.500681 11.00000 -1.20000 H5B 2 0.670772 0.960878 0.505077 11.00000 -1.20000 AFIX 0 HKLF 4 REM em1-118_a.res in P-1 REM R1 = 0.0256 for 8350 Fo > 4sig(Fo) and 0.0273 for all 8697 data REM 467 parameters refined using 41 restraints END WGHT 0.0298 2.3555 REM Highest difference peak 1.256, deepest hole -1.252, 1-sigma level 0.086 Q1 1 0.4069 0.6377 0.5333 11.00000 0.05 1.26 Q2 1 0.3418 0.4958 0.4067 11.00000 0.05 0.95 Q3 1 0.3940 0.7375 0.4938 11.00000 0.05 0.82 Q4 1 0.3314 0.5436 0.4721 11.00000 0.05 0.55 Q5 1 0.5000 0.5000 0.0000 10.50000 0.05 0.42 Q6 1 0.4569 0.6459 0.4089 11.00000 0.05 0.41 Q7 1 0.3317 0.7052 0.3678 11.00000 0.05 0.39 Q8 1 0.6793 1.0223 0.5547 11.00000 0.05 0.39 Q9 1 0.4363 0.1643 0.1354 11.00000 0.05 0.39 Q10 1 0.6934 0.7391 0.4086 11.00000 0.05 0.37 Q11 1 0.3393 0.4727 -0.0938 11.00000 0.05 0.37 Q12 1 0.6973 0.6949 0.4259 11.00000 0.05 0.36 Q13 1 0.4377 0.1644 0.2097 11.00000 0.05 0.36 Q14 1 0.8319 0.5282 0.2661 11.00000 0.05 0.36 Q15 1 0.4680 0.2995 0.1907 11.00000 0.05 0.36 Q16 1 0.6108 0.6388 0.1962 11.00000 0.05 0.34 Q17 1 0.5918 0.9228 0.2613 11.00000 0.05 0.34 Q18 1 0.3628 0.2620 0.0821 11.00000 0.05 0.32 Q19 1 0.5154 1.0848 0.5828 11.00000 0.05 0.32 Q20 1 0.7443 1.0362 0.1661 11.00000 0.05 0.31 REM The information below was added by Olex2. REM REM R1 = 0.0256 for 8350 Fo > 4sig(Fo) and 0.0273 for all 31205 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.26, deepest hole -1.25 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0273 REM R1_gt = 0.0256 REM wR_ref = 0.0645 REM GOOF = 1.087 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 31205 REM Reflections_gt = 8350 REM Parameters = n/a REM Hole = -1.25 REM Peak = 1.26 REM Flack = n/a ; _cod_data_source_file c9sc01062a2.cif _cod_data_source_block em1-118 _cod_database_code 1550884 _shelx_shelxl_version_number 2016/4 _chemical_oxdiff_formula 'Dy2 N4 O12 C30' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 86.84 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.43 _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 C1AA-C5 1.54 with sigma of 0.02 C5-O0AA 1.1 with sigma of 0.02 C2C-C4C \\sim C4C-C3C \\sim C3C-C4C \\sim C4C-C1C \\sim C1C-C4C \\sim C4C-C2C with sigma of 0.02 C2C-C3C \\sim C3C-C1C \\sim C3C-C1C \\sim C1C-C2C \\sim C1C-C2C \\sim C2C-C3C with sigma of 0.02 C2CA-C4C \\sim C4C-C3CA \\sim C3CA-C4C \\sim C4C-C1CA \\sim C1CA-C4C \\sim C4C-C2CA with sigma of 0.02 C2CA-C3CA \\sim C3CA-C1CA \\sim C3CA-C1CA \\sim C1CA-C2CA \\sim C1CA-C2CA \\sim C2CA-C3CA with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C1CA) = Uanis(C2CA) = Uanis(C3CA) Uanis(C9B) = Uanis(C11B) = Uanis(C10B) 4. Rigid body (RIGU) restrains C1C, C1CA, C2C, C3C, C3CA with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O0AA, C1AA, C5 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C11B, C9B, C10B, C8B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(C1CA)=Sof(H1CD)=Sof(H1CE)=Sof(H1CF)=Sof(C2CA)=Sof(H2CD)=Sof(H2CE)= Sof(H2CF)=Sof(C3CA)=Sof(H3CD)=Sof(H3CE)=Sof(H3CF)=1-FVAR(1) Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C2C)=Sof(H2CA)=Sof(H2CB)=Sof(H2CC)= Sof(C3C)=Sof(H3CA)=Sof(H3CB)=Sof(H3CC)=FVAR(1) 6.a Secondary CH2 refined with riding coordinates: C5(H5A,H5B) 6.b Me refined with riding coordinates: C1AA(H1AD,H1AE,H1AF) 6.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C6A(H6A), C6B(H6B), C6C(H6C) 6.d Idealised Me refined as rotating group: C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1CA(H1CD,H1CE, H1CF), C2A(H2AA,H2AB,H2AC), C2B(H2BA,H2BB,H2BC), C2C(H2CA,H2CB,H2CC), C2CA(H2CD,H2CE,H2CF), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC), C3C(H3CA,H3CB, H3CC), C3CA(H3CD,H3CE,H3CF), C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C9C(H9CA,H9CB,H9CC), C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C10C(H10G, H10H,H10I), C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C11C(H11G,H11H,H11I) ; _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 1.092 _oxdiff_exptl_absorpt_empirical_full_min 0.873 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 0.65742(2) 0.60519(2) 0.20070(2) 0.01450(4) Uani 1 1 d . . . . . O1A O 0.83593(17) 0.69841(13) 0.13227(13) 0.0225(4) Uani 1 1 d . . . . . O1B O 0.77721(18) 0.69172(15) 0.32407(13) 0.0269(4) Uani 1 1 d . . . . . O1C O 0.52295(17) 0.43844(13) 0.20010(13) 0.0231(4) Uani 1 1 d . . . . . O2A O 0.62420(17) 0.75861(13) 0.16837(13) 0.0242(4) Uani 1 1 d . . . . . O2B O 0.51225(17) 0.61443(14) 0.30471(12) 0.0234(4) Uani 1 1 d . . . . . O2C O 0.78608(17) 0.50464(14) 0.23110(13) 0.0230(4) Uani 1 1 d . . . . . N1 N 0.4582(2) 0.57517(15) 0.08728(14) 0.0180(4) Uani 1 1 d . . . . . N2 N 0.3373(2) 0.48318(16) -0.04368(14) 0.0184(4) Uani 1 1 d . . . . . C1 C 0.4435(2) 0.51597(18) 0.01219(16) 0.0157(5) Uani 1 1 d . . . . . C1A C 1.1026(3) 0.7713(3) 0.1805(3) 0.0403(8) Uani 1 1 d . . . . . H1AA H 1.190860 0.782456 0.166878 0.061 Uiso 1 1 calc GR . . . . H1AB H 1.058683 0.699921 0.178482 0.061 Uiso 1 1 calc GR . . . . H1AC H 1.100225 0.800360 0.239717 0.061 Uiso 1 1 calc GR . . . . C1B C 0.8616(3) 0.8044(3) 0.5565(2) 0.0423(8) Uani 1 1 d . . . . . H1BA H 0.942596 0.842181 0.587631 0.063 Uiso 1 1 calc GR . . . . H1BB H 0.828361 0.740805 0.583685 0.063 Uiso 1 1 calc GR . . . . H1BC H 0.801066 0.842119 0.560567 0.063 Uiso 1 1 calc GR . . . . C1C C 0.4114(7) 0.2186(6) 0.0879(4) 0.082(3) Uani 0.649(8) 1 d D U P A 1 H1CA H 0.343672 0.155305 0.078771 0.124 Uiso 0.649(8) 1 calc GR . P A 1 H1CB H 0.493197 0.207830 0.079556 0.124 Uiso 0.649(8) 1 calc GR . P A 1 H1CC H 0.396793 0.265020 0.045243 0.124 Uiso 0.649(8) 1 calc GR . P A 1 C1CA C 0.3460(10) 0.2780(8) 0.0926(7) 0.049(2) Uani 0.351(8) 1 d D U P A 2 H1CD H 0.327735 0.341426 0.096763 0.074 Uiso 0.351(8) 1 calc GR . P A 2 H1CE H 0.266690 0.224020 0.079945 0.074 Uiso 0.351(8) 1 calc GR . P A 2 H1CF H 0.402194 0.278590 0.045043 0.074 Uiso 0.351(8) 1 calc GR . P A 2 C2 C 0.2353(2) 0.5115(2) -0.02124(18) 0.0221(5) Uani 1 1 d . . . . . H2 H 0.158515 0.488843 -0.057612 0.027 Uiso 1 1 calc R . . . . C2A C 1.1049(3) 0.9353(2) 0.1164(3) 0.0456(9) Uani 1 1 d . . . . . H2AA H 1.098673 0.963316 0.175335 0.068 Uiso 1 1 calc GR . . . . H2AB H 1.065177 0.966930 0.071724 0.068 Uiso 1 1 calc GR . . . . H2AC H 1.194316 0.947255 0.105495 0.068 Uiso 1 1 calc GR . . . . C2B C 0.9310(3) 0.8866(2) 0.4130(2) 0.0376(7) Uani 1 1 d . . . . . H2BA H 0.869827 0.923500 0.418499 0.056 Uiso 1 1 calc GR . . . . H2BB H 0.941255 0.874362 0.350300 0.056 Uiso 1 1 calc GR . . . . H2BC H 1.012848 0.925319 0.442469 0.056 Uiso 1 1 calc GR . . . . C2C C 0.2930(5) 0.2971(5) 0.1913(7) 0.087(4) Uani 0.649(8) 1 d D U P A 1 H2CA H 0.298857 0.331316 0.249407 0.130 Uiso 0.649(8) 1 calc GR . P A 1 H2CB H 0.216593 0.239549 0.185292 0.130 Uiso 0.649(8) 1 calc GR . P A 1 H2CC H 0.288565 0.342545 0.144880 0.130 Uiso 0.649(8) 1 calc GR . P A 1 C2CA C 0.3294(10) 0.2656(8) 0.2591(7) 0.049(2) Uani 0.351(8) 1 d D . P A 2 H2CD H 0.371389 0.253184 0.314148 0.074 Uiso 0.351(8) 1 calc GR . P A 2 H2CE H 0.247012 0.214722 0.247835 0.074 Uiso 0.351(8) 1 calc GR . P A 2 H2CF H 0.317093 0.331105 0.264332 0.074 Uiso 0.351(8) 1 calc GR . P A 2 C3 C 0.2413(3) 0.5736(2) 0.05455(19) 0.0253(6) Uani 1 1 d . . . . . H3 H 0.170526 0.593703 0.069476 0.030 Uiso 1 1 calc R . . . . C3A C 1.0428(3) 0.7768(3) 0.0161(2) 0.0455(9) Uani 1 1 d . . . . . H3AA H 1.131691 0.788696 0.003834 0.068 Uiso 1 1 calc GR . . . . H3AB H 1.001849 0.808691 -0.027592 0.068 Uiso 1 1 calc GR . . . . H3AC H 0.999297 0.705294 0.012691 0.068 Uiso 1 1 calc GR . . . . C3B C 0.9812(3) 0.7279(3) 0.4515(2) 0.0389(7) Uani 1 1 d . . . . . H3BA H 1.061447 0.767273 0.482545 0.058 Uiso 1 1 calc GR . . . . H3BB H 0.994543 0.716034 0.389260 0.058 Uiso 1 1 calc GR . . . . H3BC H 0.949987 0.664261 0.478864 0.058 Uiso 1 1 calc GR . . . . C3C C 0.4054(6) 0.1786(4) 0.2481(5) 0.062(2) Uani 0.649(8) 1 d D U P A 1 H3CA H 0.478273 0.153915 0.242508 0.093 Uiso 0.649(8) 1 calc GR . P A 1 H3CB H 0.326904 0.124056 0.234480 0.093 Uiso 0.649(8) 1 calc GR . P A 1 H3CC H 0.406861 0.205480 0.308723 0.093 Uiso 0.649(8) 1 calc GR . P A 1 C3CA C 0.4376(9) 0.1592(7) 0.1739(8) 0.049(2) Uani 0.351(8) 1 d D U P A 2 H3CD H 0.498526 0.161243 0.129285 0.074 Uiso 0.351(8) 1 calc GR . P A 2 H3CE H 0.358049 0.107201 0.156211 0.074 Uiso 0.351(8) 1 calc GR . P A 2 H3CF H 0.472144 0.144941 0.231074 0.074 Uiso 0.351(8) 1 calc GR . P A 2 C4 C 0.3562(3) 0.6048(2) 0.10730(18) 0.0231(5) Uani 1 1 d . . . . . H4 H 0.363095 0.647553 0.158206 0.028 Uiso 1 1 calc R . . . . C4A C 1.0356(3) 0.8211(2) 0.1110(2) 0.0279(6) Uani 1 1 d . . . . . C4B C 0.8819(3) 0.7852(2) 0.45731(18) 0.0260(6) Uani 1 1 d . . . . . C4C C 0.4120(3) 0.2619(2) 0.18226(19) 0.0268(6) Uani 1 1 d D . . . . C5A C 0.8918(2) 0.7931(2) 0.13032(17) 0.0215(5) Uani 1 1 d . . . . . C5B C 0.7580(3) 0.7236(2) 0.40073(17) 0.0216(5) Uani 1 1 d . . . . . C5C C 0.5369(3) 0.35147(19) 0.20053(18) 0.0214(5) Uani 1 1 d . . . . . C6A C 0.8305(3) 0.8668(2) 0.1433(2) 0.0271(6) Uani 1 1 d . . . . . H6A H 0.879833 0.934249 0.141581 0.032 Uiso 1 1 calc R . . . . C6B C 0.6352(3) 0.7074(2) 0.43290(18) 0.0284(6) Uani 1 1 d . . . . . H6B H 0.630288 0.733923 0.490443 0.034 Uiso 1 1 calc R . . . . C6C C 0.6571(3) 0.3341(2) 0.2165(2) 0.0276(6) Uani 1 1 d . . . . . H6C H 0.658746 0.267445 0.214848 0.033 Uiso 1 1 calc R . . . . C7A C 0.6992(3) 0.84603(19) 0.15870(18) 0.0227(5) Uani 1 1 d . . . . . C7B C 0.5197(3) 0.6537(2) 0.38387(18) 0.0236(5) Uani 1 1 d . . . . . C7C C 0.7741(3) 0.4109(2) 0.23469(18) 0.0219(5) Uani 1 1 d . . . . . C8A C 0.6404(3) 0.9338(2) 0.1683(2) 0.0296(6) Uani 1 1 d . . . . . C8B C 0.3887(3) 0.6357(3) 0.4260(2) 0.0391(8) Uani 1 1 d . U . . . C8C C 0.9000(3) 0.3868(2) 0.2615(2) 0.0291(6) Uani 1 1 d . . . . . C9A C 0.6872(4) 1.0134(3) 0.0992(3) 0.0600(12) Uani 1 1 d . . . . . H9AA H 0.779178 1.043155 0.108626 0.090 Uiso 1 1 calc GR . . . . H9AB H 0.645837 1.065098 0.106239 0.090 Uiso 1 1 calc GR . . . . H9AC H 0.665821 0.982058 0.039378 0.090 Uiso 1 1 calc GR . . . . C9B C 0.3988(4) 0.6960(4) 0.5154(3) 0.0727(8) Uani 1 1 d . U . . . H9BA H 0.444451 0.669817 0.560800 0.109 Uiso 1 1 calc GR . . . . H9BB H 0.313594 0.690315 0.533305 0.109 Uiso 1 1 calc GR . . . . H9BC H 0.444700 0.765869 0.508317 0.109 Uiso 1 1 calc GR . . . . C9C C 0.9996(3) 0.4349(3) 0.1943(2) 0.0434(8) Uani 1 1 d . . . . . H9CA H 0.970774 0.402944 0.135267 0.065 Uiso 1 1 calc GR . . . . H9CB H 1.081348 0.425874 0.212824 0.065 Uiso 1 1 calc GR . . . . H9CC H 1.009163 0.505831 0.192846 0.065 Uiso 1 1 calc GR . . . . C10A C 0.6834(5) 0.9836(3) 0.2634(3) 0.0641(12) Uani 1 1 d . . . . . H10A H 0.651989 0.934781 0.307368 0.096 Uiso 1 1 calc GR . . . . H10B H 0.648898 1.039095 0.271846 0.096 Uiso 1 1 calc GR . . . . H10C H 0.776086 1.008205 0.270419 0.096 Uiso 1 1 calc GR . . . . C10B C 0.3335(4) 0.5233(4) 0.4371(4) 0.0727(8) Uani 1 1 d . U . . . H10D H 0.331855 0.487110 0.380543 0.109 Uiso 1 1 calc GR . . . . H10E H 0.247131 0.508704 0.455960 0.109 Uiso 1 1 calc GR . . . . H10F H 0.386419 0.502799 0.481768 0.109 Uiso 1 1 calc GR . . . . C10C C 0.8846(4) 0.2739(3) 0.2635(3) 0.0584(11) Uani 1 1 d . . . . . H10G H 0.822640 0.243814 0.305772 0.088 Uiso 1 1 calc GR . . . . H10H H 0.966382 0.264722 0.281456 0.088 Uiso 1 1 calc GR . . . . H10I H 0.855094 0.242117 0.204435 0.088 Uiso 1 1 calc GR . . . . C11A C 0.4936(3) 0.8937(3) 0.1581(4) 0.0577(11) Uani 1 1 d . . . . . H11A H 0.466449 0.858522 0.100142 0.087 Uiso 1 1 calc GR . . . . H11B H 0.458459 0.949189 0.163081 0.087 Uiso 1 1 calc GR . . . . H11C H 0.463253 0.848072 0.204730 0.087 Uiso 1 1 calc GR . . . . C11B C 0.2969(4) 0.6665(4) 0.3611(3) 0.0727(8) Uani 1 1 d . U . . . H11D H 0.334681 0.735803 0.347215 0.109 Uiso 1 1 calc GR . . . . H11E H 0.216845 0.659234 0.388193 0.109 Uiso 1 1 calc GR . . . . H11F H 0.280919 0.624064 0.306541 0.109 Uiso 1 1 calc GR . . . . C11C C 0.9485(3) 0.4379(3) 0.3555(2) 0.0430(8) Uani 1 1 d . . . . . H11G H 0.958993 0.509042 0.353954 0.064 Uiso 1 1 calc GR . . . . H11H H 1.030001 0.428163 0.373139 0.064 Uiso 1 1 calc GR . . . . H11I H 0.886742 0.408553 0.398128 0.064 Uiso 1 1 calc GR . . . . O0AA O 0.5268(6) 1.0057(7) 0.5386(5) 0.154(3) Uani 1 1 d D U . . . C1AA C 0.6985(10) 1.0330(8) 0.6220(8) 0.165(4) Uani 1 1 d D U . . . H1AD H 0.790172 1.043757 0.627023 0.248 Uiso 1 1 calc R . . . . H1AE H 0.680205 1.090754 0.648524 0.248 Uiso 1 1 calc R . . . . H1AF H 0.655927 0.973848 0.652881 0.248 Uiso 1 1 calc R . . . . C5 C 0.6551(7) 1.0197(7) 0.5335(7) 0.131(3) Uani 1 1 d D U . . . H5A H 0.695272 1.078847 0.500681 0.157 Uiso 1 1 calc R . . . . H5B H 0.670772 0.960878 0.505077 0.157 Uiso 1 1 calc 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 0.01261(7) 0.01345(6) 0.01637(6) -0.00282(4) 0.00005(4) 0.00296(4) O1A 0.0190(9) 0.0187(9) 0.0283(10) -0.0012(7) 0.0065(7) 0.0029(7) O1B 0.0191(9) 0.0346(11) 0.0232(10) -0.0111(8) 0.0010(7) 0.0040(8) O1C 0.0173(9) 0.0171(9) 0.0340(10) 0.0001(7) 0.0010(7) 0.0042(7) O2A 0.0191(9) 0.0168(9) 0.0365(11) 0.0017(8) 0.0036(8) 0.0050(7) O2B 0.0174(9) 0.0260(10) 0.0240(10) -0.0051(7) 0.0028(7) 0.0028(7) O2C 0.0180(9) 0.0209(9) 0.0292(10) 0.0002(7) -0.0027(7) 0.0054(7) N1 0.0190(10) 0.0171(10) 0.0185(10) -0.0024(8) 0.0017(8) 0.0066(8) N2 0.0150(10) 0.0218(11) 0.0180(10) -0.0026(8) 0.0009(8) 0.0053(8) C1 0.0155(12) 0.0146(11) 0.0155(11) -0.0006(9) -0.0005(9) 0.0029(9) C1A 0.0227(15) 0.0448(19) 0.054(2) 0.0055(16) 0.0027(14) 0.0100(13) C1B 0.0391(18) 0.057(2) 0.0230(15) -0.0119(14) -0.0057(13) 0.0069(15) C1C 0.071(5) 0.086(6) 0.043(4) -0.027(4) 0.005(3) -0.043(4) C1CA 0.033(3) 0.037(3) 0.061(5) -0.001(3) -0.002(3) -0.013(2) C2 0.0151(12) 0.0288(14) 0.0221(13) -0.0019(10) -0.0005(10) 0.0069(10) C2A 0.0238(16) 0.0323(17) 0.075(3) 0.0037(16) 0.0141(16) -0.0017(13) C2B 0.0364(17) 0.0282(16) 0.0386(17) -0.0045(13) -0.0051(13) -0.0022(13) C2C 0.021(3) 0.039(4) 0.191(11) -0.006(5) 0.004(4) -0.004(2) C2CA 0.033(3) 0.037(3) 0.061(5) -0.001(3) -0.002(3) -0.013(2) C3 0.0196(13) 0.0329(15) 0.0269(14) -0.0020(11) 0.0039(10) 0.0132(11) C3A 0.0374(19) 0.056(2) 0.0393(19) -0.0039(16) 0.0200(15) 0.0059(16) C3B 0.0295(16) 0.0464(19) 0.0397(18) -0.0072(15) -0.0124(13) 0.0136(14) C3C 0.048(4) 0.041(3) 0.078(5) 0.033(3) -0.016(3) -0.015(3) C3CA 0.033(3) 0.037(3) 0.061(5) -0.001(3) -0.002(3) -0.013(2) C4 0.0255(14) 0.0241(13) 0.0225(13) -0.0028(10) 0.0038(10) 0.0116(10) C4A 0.0202(14) 0.0253(14) 0.0353(16) 0.0012(11) 0.0090(11) 0.0015(10) C4B 0.0240(14) 0.0305(15) 0.0193(13) -0.0057(11) -0.0049(10) 0.0043(11) C4C 0.0234(14) 0.0190(13) 0.0331(15) 0.0017(11) -0.0012(11) -0.0003(10) C5A 0.0188(13) 0.0228(13) 0.0206(12) 0.0002(10) 0.0046(10) 0.0023(10) C5B 0.0213(13) 0.0217(13) 0.0198(12) -0.0026(10) -0.0011(10) 0.0045(10) C5C 0.0228(13) 0.0173(12) 0.0221(13) -0.0004(10) 0.0006(10) 0.0036(10) C6A 0.0244(14) 0.0154(12) 0.0391(16) 0.0019(11) 0.0078(12) 0.0015(10) C6B 0.0246(14) 0.0382(16) 0.0190(13) -0.0076(11) 0.0044(11) 0.0052(12) C6C 0.0268(14) 0.0157(12) 0.0397(16) -0.0003(11) -0.0007(12) 0.0065(10) C7A 0.0241(13) 0.0183(12) 0.0253(13) 0.0005(10) 0.0021(10) 0.0058(10) C7B 0.0218(13) 0.0253(13) 0.0225(13) -0.0010(10) 0.0053(10) 0.0051(10) C7C 0.0223(13) 0.0225(13) 0.0218(13) 0.0018(10) 0.0000(10) 0.0082(10) C8A 0.0311(15) 0.0192(13) 0.0419(17) 0.0044(12) 0.0089(13) 0.0112(11) C8B 0.0181(14) 0.060(2) 0.0336(16) -0.0052(14) 0.0093(12) 0.0031(13) C8C 0.0229(14) 0.0290(15) 0.0382(16) 0.0051(12) -0.0017(12) 0.0123(11) C9A 0.068(3) 0.040(2) 0.086(3) 0.031(2) 0.031(2) 0.0305(19) C9B 0.0368(13) 0.102(2) 0.0798(19) 0.0071(16) 0.0232(12) 0.0176(13) C9C 0.0323(17) 0.061(2) 0.048(2) 0.0105(17) 0.0093(15) 0.0274(16) C10A 0.087(3) 0.056(3) 0.062(3) -0.018(2) -0.002(2) 0.045(2) C10B 0.0368(13) 0.102(2) 0.0798(19) 0.0071(16) 0.0232(12) 0.0176(13) C10C 0.042(2) 0.0335(19) 0.104(4) 0.008(2) -0.014(2) 0.0217(16) C11A 0.0343(19) 0.0347(19) 0.110(4) 0.006(2) 0.003(2) 0.0191(15) C11B 0.0368(13) 0.102(2) 0.0798(19) 0.0071(16) 0.0232(12) 0.0176(13) C11C 0.0296(17) 0.061(2) 0.0388(18) 0.0045(16) -0.0080(13) 0.0160(15) O0AA 0.088(5) 0.133(4) 0.253(11) 0.021(8) 0.064(5) 0.041(4) C1AA 0.135(7) 0.153(9) 0.195(9) -0.009(9) 0.023(7) 0.027(7) C5 0.104(5) 0.143(7) 0.159(7) 0.002(6) 0.052(5) 0.053(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' 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 O1C 139.27(6) . . O1A Dy1 O2A 72.94(6) . . O1A Dy1 O2B 143.75(6) . . O1A Dy1 N1 107.79(7) . . O1A Dy1 N2 71.29(6) . 2_665 O1B Dy1 O1A 80.76(7) . . O1B Dy1 O1C 123.99(7) . . O1B Dy1 O2A 85.02(7) . . O1B Dy1 O2B 74.05(6) . . O1B Dy1 O2C 79.96(7) . . O1B Dy1 N1 148.79(7) . . O1B Dy1 N2 145.47(7) . 2_665 O1C Dy1 N1 68.96(7) . . O1C Dy1 N2 72.00(7) . 2_665 O2A Dy1 O1C 134.23(6) . . O2A Dy1 N1 69.82(7) . . O2A Dy1 N2 105.02(7) . 2_665 O2B Dy1 O1C 76.97(6) . . O2B Dy1 O2A 79.21(7) . . O2B Dy1 N1 83.08(6) . . O2B Dy1 N2 139.80(6) . 2_665 O2C Dy1 O1A 82.56(7) . . O2C Dy1 O1C 72.42(6) . . O2C Dy1 O2A 153.03(6) . . O2C Dy1 O2B 117.28(7) . . O2C Dy1 N1 130.23(6) . . O2C Dy1 N2 76.74(7) . 2_665 N1 Dy1 N2 62.38(6) . 2_665 C5A O1A Dy1 132.84(16) . . C5B O1B Dy1 137.74(17) . . C5C O1C Dy1 136.79(17) . . C7A O2A Dy1 133.52(17) . . C7B O2B Dy1 135.63(17) . . C7C O2C Dy1 138.24(17) . . C1 N1 Dy1 121.26(16) . . C1 N1 C4 116.3(2) . . C4 N1 Dy1 121.65(17) . . C1 N2 Dy1 120.81(15) . 2_665 C1 N2 C2 116.5(2) . . C2 N2 Dy1 121.91(16) . 2_665 N1 C1 C1 117.1(3) . 2_665 N2 C1 N1 126.3(2) . . N2 C1 C1 116.6(3) . 2_665 N2 C2 C3 121.6(2) . . C4 C3 C2 117.5(2) . . N1 C4 C3 121.8(2) . . C1A C4A C2A 108.9(3) . . C1A C4A C3A 109.5(3) . . C1A C4A C5A 107.6(2) . . C2A C4A C5A 113.8(2) . . C3A C4A C2A 109.5(3) . . C3A C4A C5A 107.5(2) . . C1B C4B C2B 109.6(3) . . C1B C4B C5B 114.1(2) . . C2B C4B C5B 106.3(2) . . C3B C4B C1B 109.2(3) . . C3B C4B C2B 109.6(3) . . C3B C4B C5B 107.9(2) . . C1C C4C C2C 110.0(5) . . C1C C4C C3C 108.6(5) . . C1C C4C C5C 107.8(3) . . C1CA C4C C3CA 108.1(6) . . C1CA C4C C5C 107.4(4) . . C2C C4C C3C 107.9(5) . . C2C C4C C5C 110.6(3) . . C2CA C4C C1CA 110.9(6) . . C2CA C4C C3CA 110.9(6) . . C2CA C4C C5C 106.5(4) . . C3C C4C C5C 111.8(3) . . C3CA C4C C5C 113.0(4) . . O1A C5A C4A 114.2(2) . . O1A C5A C6A 124.2(2) . . C6A C5A C4A 121.7(2) . . O1B C5B C4B 114.4(2) . . O1B C5B C6B 123.9(2) . . C6B C5B C4B 121.6(2) . . O1C C5C C4C 115.8(2) . . O1C C5C C6C 123.7(2) . . C6C C5C C4C 120.5(2) . . C5A C6A C7A 124.3(2) . . C7B C6B C5B 124.1(2) . . C7C C6C C5C 124.0(2) . . O2A C7A C6A 124.0(2) . . O2A C7A C8A 116.2(2) . . C6A C7A C8A 119.7(2) . . O2B C7B C6B 124.6(2) . . O2B C7B C8B 114.7(2) . . C6B C7B C8B 120.7(2) . . O2C C7C C6C 123.8(2) . . O2C C7C C8C 114.8(2) . . C6C C7C C8C 121.4(2) . . C9A C8A C7A 112.4(3) . . C9A C8A C10A 108.8(3) . . C10A C8A C7A 107.0(3) . . C11A C8A C7A 110.4(2) . . C11A C8A C9A 109.1(3) . . C11A C8A C10A 109.2(3) . . C9B C8B C7B 113.3(3) . . C10B C8B C7B 107.6(3) . . C10B C8B C9B 111.2(4) . . C10B C8B C11B 107.8(3) . . C11B C8B C7B 109.0(3) . . C11B C8B C9B 107.8(4) . . C9C C8C C7C 108.0(2) . . C10C C8C C7C 114.1(3) . . C10C C8C C9C 109.4(3) . . C10C C8C C11C 109.6(3) . . C11C C8C C7C 106.9(2) . . C11C C8C C9C 108.7(3) . . O0AA O0AA C5 109.5(11) 2_676 . O0AA C5 C1AA 101.8(8) . . 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 2.2633(18) . Dy1 O1C 2.3346(17) . Dy1 O2A 2.3264(18) . Dy1 O2B 2.3000(17) . Dy1 O2C 2.2930(18) . Dy1 N1 2.586(2) . Dy1 N2 2.609(2) 2_665 O1A C5A 1.273(3) . O1B C5B 1.259(3) . O1C C5C 1.261(3) . O2A C7A 1.260(3) . O2B C7B 1.267(3) . O2C C7C 1.271(3) . N1 C1 1.335(3) . N1 C4 1.339(3) . N2 C1 1.333(3) . N2 C2 1.339(3) . C1 C1 1.485(5) 2_665 C1A C4A 1.530(4) . C1B C4B 1.529(4) . C1C C4C 1.504(6) . C1CA C4C 1.532(10) . C2 C3 1.380(4) . C2A C4A 1.534(4) . C2B C4B 1.533(4) . C2C C4C 1.526(6) . C2CA C4C 1.501(10) . C3 C4 1.378(4) . C3A C4A 1.533(4) . C3B C4B 1.527(4) . C3C C4C 1.529(6) . C3CA C4C 1.534(10) . C4A C5A 1.541(4) . C4B C5B 1.541(4) . C4C C5C 1.543(3) . C5A C6A 1.392(4) . C5B C6B 1.401(4) . C5C C6C 1.408(4) . C6A C7A 1.403(4) . C6B C7B 1.398(4) . C6C C7C 1.396(4) . C7A C8A 1.542(4) . C7B C8B 1.544(4) . C7C C8C 1.538(4) . C8A C9A 1.528(4) . C8A C10A 1.534(5) . C8A C11A 1.520(5) . C8B C9B 1.526(6) . C8B C10B 1.512(6) . C8B C11B 1.511(6) . C8C C9C 1.534(4) . C8C C10C 1.527(4) . C8C C11C 1.533(5) . O0AA O0AA 1.238(14) 2_676 O0AA C5 1.357(9) . C1AA C5 1.357(10) .