#------------------------------------------------------------------------------ #$Date: 2018-03-30 03:44:33 +0300 (Fri, 30 Mar 2018) $ #$Revision: 207189 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/72/7057229.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_7057229 loop_ _publ_author_name 'Yao, Xu' 'Yan, Pengfei' 'An, Guanghui' 'Shi, Chao' 'Li, Yuxin' 'Li, Guangming' _publ_section_title ; Single-ion magnets with D4d symmetry based on electron-donating \b-diketonate Dy(III) complexes ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/C8NJ00636A _journal_year 2018 _chemical_formula_moiety 'C35 H63 Dy O8' _chemical_formula_sum 'C35 H63 Dy O8' _chemical_formula_weight 774.35 _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 _audit_creation_date 2018-03-14 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2018-03-28 deposited with the CCDC. 2018-03-29 downloaded from the CCDC. ; _cell_angle_alpha 65.115(5) _cell_angle_beta 72.713(5) _cell_angle_gamma 75.622(5) _cell_formula_units_Z 2 _cell_length_a 10.678(5) _cell_length_b 13.945(5) _cell_length_c 16.534(5) _cell_measurement_reflns_used 6285 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.6589 _cell_measurement_theta_min 3.0534 _cell_volume 2110.8(14) _computing_data_collection 'Bruker FRAMBO' _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 'Bruker SHELXTL' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type MoK\a _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_unetI/netI 0.0448 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 17638 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.240 _diffrn_reflns_theta_max 27.498 _diffrn_reflns_theta_min 3.059 _exptl_absorpt_coefficient_mu 1.810 _exptl_absorpt_correction_T_max 0.696 _exptl_absorpt_correction_T_min 0.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.218 _exptl_crystal_description block _exptl_crystal_F_000 806 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.917 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.079 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 477 _refine_ls_number_reflns 9689 _refine_ls_number_restraints 102 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0421 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.8670P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0953 _refine_ls_wR_factor_ref 0.1031 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8034 _reflns_number_total 9689 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8nj00636a2.cif _cod_data_source_block 1 _cod_database_code 7057229 _shelx_shelxl_version_number 2016/6 _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 0.714 _shelx_estimated_absorpt_t_min 0.671 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C3-C21A \\sim C23-C3 \\sim C22-C3 \\sim C22A-C3 \\sim C23A-C3 \\sim C21-C3 with sigma of 0.02 C7-C25A \\sim C25-C7 \\sim C24A-C7 \\sim C26-C7 \\sim C26A-C7 \\sim C24-C7 with sigma of 0.02 3. Rigid body (RIGU) restrains C21A, C23, C22A, C22, C23A, C21, C3 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C25A, C25, C24A, C26, C26A, C24, C7 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Fixed Sof: C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C22A(0.5) H22D(0.5) H22E(0.5) H22F(0.5) C23A(0.5) H23D(0.5) H23E(0.5) H23F(0.5) C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C24A(0.5) H24D(0.5) H24E(0.5) H24F(0.5) C25A(0.5) H25D(0.5) H25E(0.5) H25F(0.5) C26A(0.5) H26D(0.5) H26E(0.5) H26F(0.5) 5.a Aromatic/amide H refined with riding coordinates: C5(H5), C10(H10), C15(H15) 5.b Idealised Me refined as rotating group: C2(H2A,H2B,H2C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B, H23C), C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F), C21A(H21D,H21E,H21F), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C24A(H24D,H24E, H24F), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C31A(H31A,H31B,H31C), C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B, H35C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A, H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C1(H1A,H1B,H1C) ; _shelx_res_file ; TITL 1 in P-1 1.res created by SHELXL-2016/6 at 15:51:26 on 14-Mar-2018 CELL 0.71069 10.678 13.945 16.534 65.115 72.713 75.622 ZERR 2 0.005 0.005 0.005 0.005 0.005 0.005 LATT 1 SFAC C H Dy O UNIT 70 126 2 16 SADI C3 C21A C23 C3 C22 C3 C22A C3 C23A C3 C21 C3 SADI C7 C25A C25 C7 C24A C7 C26 C7 C26A C7 C24 C7 RIGU C21A C23 C22A C22 C23A C21 C3 RIGU C25A C25 C24A C26 C26A C24 C7 L.S. 4 PLAN 50 SIZE 0.24 0.22 0.2 LIST 1 fmap 2 acta MERG 2 OMIT -3 55 REM REM REM WGHT 0.047700 0.867000 FVAR 0.16011 C2 1 -0.049636 0.359141 0.490224 11.00000 0.33352 0.10147 = 0.07111 -0.01908 -0.03048 -0.05936 AFIX 137 H2A 2 0.038489 0.354847 0.453431 11.00000 -1.50000 H2B 2 -0.109423 0.406659 0.452096 11.00000 -1.50000 H2C 2 -0.076518 0.289431 0.519813 11.00000 -1.50000 AFIX 0 C3 1 0.117723 0.156730 0.975429 11.00000 0.06057 0.11444 = 0.07746 -0.04533 -0.02966 0.00949 C4 1 0.000109 0.203395 0.927812 11.00000 0.05193 0.06966 = 0.06624 -0.03745 -0.01308 -0.00222 C5 1 -0.127403 0.217661 0.978276 11.00000 0.05469 0.09235 = 0.05514 -0.03499 -0.00976 0.00253 AFIX 43 H5 2 -0.138013 0.199711 1.040598 11.00000 -1.20000 AFIX 0 C6 1 -0.239559 0.256443 0.942985 11.00000 0.04773 0.06380 = 0.06099 -0.03197 -0.00092 -0.00271 C7 1 -0.378348 0.267409 1.005119 11.00000 0.04813 0.09251 = 0.06342 -0.03116 0.00621 0.00012 C8 1 0.171882 0.031089 0.638364 11.00000 0.05343 0.08061 = 0.10686 -0.06284 -0.00169 -0.00089 C9 1 0.042141 0.099648 0.666573 11.00000 0.04736 0.05517 = 0.05781 -0.02854 -0.00699 -0.00196 C10 1 -0.079704 0.075356 0.673085 11.00000 0.05688 0.05215 = 0.08298 -0.03932 -0.01386 -0.00264 AFIX 43 H10 2 -0.080275 0.014834 0.662818 11.00000 -1.20000 AFIX 0 C11 1 -0.200661 0.135004 0.693827 11.00000 0.05228 0.04758 = 0.05258 -0.02064 -0.01371 -0.00789 C12 1 -0.331630 0.105671 0.695684 11.00000 0.05166 0.06474 = 0.10144 -0.04123 -0.02389 -0.00817 C13 1 -0.444632 0.579265 0.662260 11.00000 0.06331 0.08311 = 0.09610 -0.03461 -0.03012 0.00639 C14 1 -0.311697 0.531029 0.691625 11.00000 0.05908 0.05731 = 0.06827 -0.02498 -0.01451 -0.00169 C15 1 -0.261596 0.578553 0.731853 11.00000 0.05906 0.06161 = 0.09670 -0.04463 -0.01607 0.00326 AFIX 43 H15 2 -0.313542 0.637573 0.743465 11.00000 -1.20000 AFIX 0 C16 1 -0.139780 0.544367 0.755936 11.00000 0.05920 0.05333 = 0.07335 -0.03427 -0.00700 -0.00910 C17 1 -0.091377 0.603719 0.798821 11.00000 0.07715 0.07220 = 0.10433 -0.05609 -0.02068 -0.00624 PART 1 C21 1 0.196146 0.249963 0.939055 10.50000 0.13185 0.18738 = 0.23939 -0.07224 -0.10500 -0.03985 AFIX 137 H21A 2 0.246984 0.258610 0.878421 10.50000 -1.50000 H21B 2 0.254741 0.235615 0.978268 10.50000 -1.50000 H21C 2 0.135966 0.314215 0.937632 10.50000 -1.50000 AFIX 0 C22 1 0.084584 0.129563 1.076319 10.50000 0.11041 0.44179 = 0.09736 -0.10928 -0.05274 0.01544 AFIX 137 H22A 2 0.022505 0.186334 1.090274 10.50000 -1.50000 H22B 2 0.163832 0.120350 1.096496 10.50000 -1.50000 H22C 2 0.046134 0.064562 1.106968 10.50000 -1.50000 AFIX 0 C23 1 0.203246 0.077099 0.936092 10.50000 0.08550 0.14618 = 0.18880 -0.08376 -0.07560 0.06738 AFIX 137 H23A 2 0.159674 0.015489 0.958147 10.50000 -1.50000 H23B 2 0.286486 0.056117 0.954272 10.50000 -1.50000 H23C 2 0.218420 0.108627 0.870634 10.50000 -1.50000 AFIX 0 PART 0 PART 2 C22A 1 0.086235 0.058692 1.062789 10.50000 0.08858 0.22861 = 0.09277 0.01515 -0.06049 -0.00266 AFIX 137 H22D 2 -0.006356 0.067804 1.090587 10.50000 -1.50000 H22E 2 0.137639 0.050706 1.104587 10.50000 -1.50000 H22F 2 0.107689 -0.003879 1.047945 10.50000 -1.50000 AFIX 0 C23A 1 0.149659 0.244923 0.991935 10.50000 0.14281 0.22715 = 0.34102 -0.21337 -0.16203 0.06252 AFIX 137 H23D 2 0.228049 0.270670 0.948376 10.50000 -1.50000 H23E 2 0.164409 0.218345 1.052644 10.50000 -1.50000 H23F 2 0.076962 0.302205 0.985348 10.50000 -1.50000 AFIX 0 C21A 1 0.242599 0.121059 0.917948 10.50000 0.05650 0.20395 = 0.11687 -0.08297 -0.03121 0.03477 AFIX 137 H21D 2 0.224519 0.074104 0.895161 10.50000 -1.50000 H21E 2 0.307800 0.084017 0.954300 10.50000 -1.50000 H21F 2 0.275504 0.182197 0.867547 10.50000 -1.50000 AFIX 0 PART 0 PART 3 C24 1 -0.466211 0.215603 0.982562 10.50000 0.05763 0.17429 = 0.10853 -0.06117 0.00628 -0.03582 AFIX 137 H24A 2 -0.474485 0.254628 0.920329 10.50000 -1.50000 H24B 2 -0.552284 0.216292 1.022537 10.50000 -1.50000 H24C 2 -0.427330 0.143185 0.990579 10.50000 -1.50000 AFIX 0 C25 1 -0.419901 0.382969 0.989354 10.50000 0.08243 0.09382 = 0.13113 -0.05136 0.01994 0.01419 AFIX 137 H25A 2 -0.373215 0.403240 1.019835 10.50000 -1.50000 H25B 2 -0.513512 0.395541 1.013084 10.50000 -1.50000 H25C 2 -0.399740 0.424552 0.924990 10.50000 -1.50000 AFIX 0 C26 1 -0.378302 0.197746 1.107614 10.50000 0.06478 0.10961 = 0.06428 -0.02912 0.01406 -0.00732 AFIX 137 H26A 2 -0.342855 0.125168 1.114106 10.50000 -1.50000 H26B 2 -0.467361 0.200564 1.143308 10.50000 -1.50000 H26C 2 -0.324662 0.224608 1.128544 10.50000 -1.50000 AFIX 0 PART 0 PART 4 C24A 1 -0.373560 0.303699 1.080258 10.50000 0.09455 0.25514 = 0.11926 -0.13171 0.00590 0.02261 AFIX 137 H24D 2 -0.317619 0.250617 1.118868 10.50000 -1.50000 H24E 2 -0.461378 0.312819 1.116180 10.50000 -1.50000 H24F 2 -0.338704 0.370234 1.052466 10.50000 -1.50000 AFIX 0 C25A 1 -0.469548 0.360703 0.947464 10.50000 0.05730 0.11799 = 0.10319 -0.03856 0.00444 0.02148 AFIX 137 H25D 2 -0.425238 0.422731 0.915151 10.50000 -1.50000 H25E 2 -0.550584 0.376813 0.987256 10.50000 -1.50000 H25F 2 -0.489005 0.340036 0.904465 10.50000 -1.50000 AFIX 0 C26A 1 -0.436290 0.167615 1.036725 10.50000 0.10372 0.09687 = 0.18126 -0.03899 0.06677 -0.02250 AFIX 137 H26D 2 -0.427938 0.149287 0.985337 10.50000 -1.50000 H26E 2 -0.528266 0.178514 1.065325 10.50000 -1.50000 H26F 2 -0.390034 0.110687 1.079898 10.50000 -1.50000 AFIX 0 PART 0 PART 6 C31A 1 0.154191 -0.077574 0.657200 11.00000 0.08542 0.10968 = 0.56387 -0.18951 0.01869 0.00887 AFIX 137 H31A 2 0.105357 -0.108200 0.718847 11.00000 -1.50000 H31B 2 0.239334 -0.120097 0.649446 11.00000 -1.50000 H31C 2 0.106271 -0.075751 0.615672 11.00000 -1.50000 AFIX 0 C32A 1 0.222398 0.084405 0.541601 11.00000 0.25197 0.27873 = 0.15576 -0.05751 0.09441 0.11668 AFIX 137 H32A 2 0.209743 0.045752 0.509065 11.00000 -1.50000 H32B 2 0.315186 0.087192 0.530425 11.00000 -1.50000 H32C 2 0.175821 0.155688 0.521036 11.00000 -1.50000 AFIX 0 C33A 1 0.269214 0.024080 0.685902 11.00000 0.11236 0.35214 = 0.49778 -0.35245 -0.17257 0.14831 AFIX 137 H33A 2 0.293581 0.093501 0.666444 11.00000 -1.50000 H33B 2 0.346237 -0.024183 0.672405 11.00000 -1.50000 H33C 2 0.232646 -0.001747 0.750515 11.00000 -1.50000 AFIX 0 PART 0 C34 1 -0.319397 -0.003422 0.695307 11.00000 0.08762 0.14008 = 0.36016 -0.15449 -0.05562 -0.02022 AFIX 137 H34A 2 -0.269984 -0.004462 0.636706 11.00000 -1.50000 H34B 2 -0.406128 -0.021085 0.707153 11.00000 -1.50000 H34C 2 -0.274233 -0.054689 0.741820 11.00000 -1.50000 AFIX 0 C35 1 -0.429300 0.109424 0.779771 11.00000 0.09502 0.38450 = 0.25602 -0.21980 0.06774 -0.13341 AFIX 137 H35A 2 -0.386066 0.079142 0.830174 11.00000 -1.50000 H35B 2 -0.498679 0.069303 0.792332 11.00000 -1.50000 H35C 2 -0.466431 0.182258 0.771284 11.00000 -1.50000 AFIX 0 C36 1 -0.380971 0.186642 0.617226 11.00000 0.22183 0.18359 = 0.35388 0.07589 -0.23926 -0.10264 AFIX 137 H36A 2 -0.386160 0.256116 0.617730 11.00000 -1.50000 H36B 2 -0.467475 0.175209 0.620094 11.00000 -1.50000 H36C 2 -0.321862 0.182071 0.562044 11.00000 -1.50000 AFIX 0 C41 1 -0.436602 0.570937 0.575104 11.00000 0.18284 0.42276 = 0.20812 -0.19123 -0.14182 0.16529 AFIX 137 H41A 2 -0.384668 0.622644 0.526294 11.00000 -1.50000 H41B 2 -0.524175 0.584204 0.564663 11.00000 -1.50000 H41C 2 -0.395716 0.500523 0.577423 11.00000 -1.50000 AFIX 0 C42 1 -0.543905 0.513796 0.727587 11.00000 0.09493 0.29746 = 0.31407 0.05103 -0.11013 -0.06214 AFIX 137 H42A 2 -0.513813 0.440746 0.733657 11.00000 -1.50000 H42B 2 -0.625192 0.537988 0.706671 11.00000 -1.50000 H42C 2 -0.558565 0.519222 0.785772 11.00000 -1.50000 AFIX 0 C43 1 -0.493780 0.687646 0.659617 11.00000 0.24418 0.19707 = 0.62474 -0.26190 -0.32325 0.16123 AFIX 137 H43A 2 -0.530133 0.685672 0.720743 11.00000 -1.50000 H43B 2 -0.561385 0.719232 0.624830 11.00000 -1.50000 H43C 2 -0.422184 0.729395 0.631539 11.00000 -1.50000 AFIX 0 C44 1 -0.158652 0.714114 0.782602 11.00000 0.22833 0.12815 = 0.35990 -0.16652 -0.17271 0.04993 AFIX 137 H44A 2 -0.151029 0.753349 0.718145 11.00000 -1.50000 H44B 2 -0.118142 0.747797 0.806460 11.00000 -1.50000 H44C 2 -0.250571 0.713044 0.812646 11.00000 -1.50000 AFIX 0 C45 1 -0.116613 0.541396 0.898649 11.00000 0.47747 0.18937 = 0.15342 -0.05333 -0.12907 -0.15432 AFIX 137 H45A 2 -0.210090 0.550006 0.924175 11.00000 -1.50000 H45B 2 -0.071507 0.566581 0.926592 11.00000 -1.50000 H45C 2 -0.084589 0.467237 0.909836 11.00000 -1.50000 AFIX 0 C46 1 0.050117 0.606594 0.764497 11.00000 0.10013 0.35763 = 0.39712 -0.32320 0.00949 -0.07086 AFIX 137 H46A 2 0.096217 0.534969 0.779244 11.00000 -1.50000 H46B 2 0.079323 0.642927 0.792166 11.00000 -1.50000 H46C 2 0.068372 0.643788 0.699383 11.00000 -1.50000 AFIX 0 O1 4 0.028028 0.227180 0.842239 11.00000 0.04259 0.07866 = 0.06315 -0.03677 -0.01084 0.00049 O2 4 -0.238363 0.285365 0.859724 11.00000 0.04186 0.09763 = 0.06115 -0.03649 -0.00699 -0.00126 O3 4 0.056326 0.177668 0.681322 11.00000 0.04377 0.07094 = 0.08533 -0.05232 -0.00589 -0.00609 O4 4 -0.212354 0.217281 0.710596 11.00000 0.04449 0.06178 = 0.08717 -0.04516 -0.01191 -0.00184 O5 4 -0.254844 0.448457 0.676185 11.00000 0.06802 0.06091 = 0.08207 -0.03697 -0.02710 0.00250 O6 4 -0.061655 0.464221 0.745377 11.00000 0.05262 0.06174 = 0.09436 -0.04595 -0.01868 -0.00092 O7 4 0.148783 0.353752 0.649027 11.00000 0.06695 0.13753 = 0.12340 -0.06321 0.00958 -0.04500 O8 4 -0.051648 0.395722 0.552838 11.00000 0.15313 0.09241 = 0.06821 -0.02898 -0.00895 -0.03594 DY1 3 -0.084268 0.314246 0.726497 11.00000 0.04295 0.05559 = 0.05935 -0.03394 -0.00644 -0.00533 C1 1 0.243970 0.372070 0.673767 11.00000 0.09328 0.20583 = 0.13594 -0.05815 -0.01083 -0.05508 AFIX 137 H1A 2 0.290840 0.425598 0.622935 11.00000 -1.50000 H1B 2 0.304190 0.307343 0.693131 11.00000 -1.50000 H1C 2 0.206362 0.396641 0.723294 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1 in P-1 REM R1 = 0.0421 for 8034 Fo > 4sig(Fo) and 0.0555 for all 9689 data REM 477 parameters refined using 102 restraints END WGHT 0.0477 0.8670 REM Highest difference peak 0.917, deepest hole -0.517, 1-sigma level 0.079 Q1 1 -0.1246 0.2676 0.7756 11.00000 0.05 0.92 Q2 1 -0.4153 0.6847 0.5779 11.00000 0.05 0.75 Q3 1 -0.3740 0.0134 0.7891 11.00000 0.05 0.60 Q4 1 -0.0330 0.7007 0.7097 11.00000 0.05 0.51 Q5 1 -0.5407 0.6101 0.7309 11.00000 0.05 0.51 Q6 1 -0.2023 0.6419 0.8642 11.00000 0.05 0.51 Q7 1 0.0002 0.3587 0.6692 11.00000 0.05 0.51 Q8 1 -0.3052 0.0738 0.6092 11.00000 0.05 0.51 Q9 1 -0.4440 0.1962 0.6922 11.00000 0.05 0.51 Q10 1 -0.1547 0.3481 0.7011 11.00000 0.05 0.48 Q11 1 -0.0022 0.3723 0.7065 11.00000 0.05 0.44 Q12 1 0.0099 0.2642 0.7623 11.00000 0.05 0.43 Q13 1 -0.0439 0.2734 0.6918 11.00000 0.05 0.43 Q14 1 -0.0083 0.5397 0.8504 11.00000 0.05 0.42 Q15 1 -0.5195 0.7025 0.6459 11.00000 0.05 0.42 Q16 1 -0.1445 0.3691 0.7577 11.00000 0.05 0.41 Q17 1 -0.5030 0.5146 0.6450 11.00000 0.05 0.41 Q18 1 0.1777 0.0025 0.5617 11.00000 0.05 0.41 Q19 1 -0.3984 0.1841 0.6056 11.00000 0.05 0.41 Q20 1 0.2612 0.0895 0.5788 11.00000 0.05 0.40 Q21 1 -0.0966 0.3292 0.7893 11.00000 0.05 0.40 Q22 1 -0.0616 0.4005 0.7100 11.00000 0.05 0.39 Q23 1 -0.0753 0.2964 0.6668 11.00000 0.05 0.38 Q24 1 0.2165 -0.0445 0.7092 11.00000 0.05 0.38 Q25 1 0.0442 0.3948 0.6566 11.00000 0.05 0.35 Q26 1 -0.0390 0.4537 0.6926 11.00000 0.05 0.34 Q27 1 0.0577 0.3038 0.6920 11.00000 0.05 0.33 Q28 1 0.1399 0.4020 0.6742 11.00000 0.05 0.33 Q29 1 0.2553 0.3008 0.6576 11.00000 0.05 0.33 Q30 1 -0.2664 0.1123 0.6880 11.00000 0.05 0.32 Q31 1 -0.5795 0.4983 0.7330 11.00000 0.05 0.31 Q32 1 -0.5366 0.4617 0.7569 11.00000 0.05 0.31 Q33 1 0.2673 0.0177 0.7322 11.00000 0.05 0.30 Q34 1 0.1457 0.3882 0.5994 11.00000 0.05 0.30 Q35 1 0.1116 0.0399 1.0080 11.00000 0.05 0.30 Q36 1 0.1748 0.1306 0.5081 11.00000 0.05 0.29 Q37 1 -0.1211 0.1887 0.7424 11.00000 0.05 0.28 Q38 1 -0.0601 0.3340 0.6010 11.00000 0.05 0.28 Q39 1 0.1088 0.2066 1.0317 11.00000 0.05 0.28 Q40 1 0.1160 0.0132 1.0553 11.00000 0.05 0.28 Q41 1 0.0832 0.6215 0.7883 11.00000 0.05 0.28 Q42 1 0.1028 0.0272 1.0351 11.00000 0.05 0.28 Q43 1 0.1787 -0.1164 0.6671 11.00000 0.05 0.27 Q44 1 0.2993 0.0576 0.6453 11.00000 0.05 0.27 Q45 1 0.1017 0.0415 0.9384 11.00000 0.05 0.27 Q46 1 0.0629 0.5917 0.8031 11.00000 0.05 0.27 Q47 1 0.1381 -0.0727 0.7292 11.00000 0.05 0.27 Q48 1 -0.1409 0.1468 1.0720 11.00000 0.05 0.26 Q49 1 0.1965 0.2571 0.6519 11.00000 0.05 0.26 Q50 1 -0.3012 0.2293 0.8621 11.00000 0.05 0.26 ; _shelx_res_checksum 31316 _olex2_submission_special_instructions 'No special instructions were received' 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 C2 C -0.0496(12) 0.3591(6) 0.4902(5) 0.171(5) Uani 1 1 d . . . . . H2A H 0.038489 0.354847 0.453431 0.257 Uiso 1 1 calc GR . . . . H2B H -0.109423 0.406659 0.452096 0.257 Uiso 1 1 calc GR . . . . H2C H -0.076518 0.289431 0.519813 0.257 Uiso 1 1 calc GR . . . . C3 C 0.1177(5) 0.1567(5) 0.9754(3) 0.0817(14) Uani 1 1 d D U . . . C4 C 0.0001(4) 0.2034(4) 0.9278(3) 0.0596(10) Uani 1 1 d . . . . . C5 C -0.1274(4) 0.2177(4) 0.9783(3) 0.0679(12) Uani 1 1 d . . . . . H5 H -0.138013 0.199711 1.040598 0.081 Uiso 1 1 calc R . . . . C6 C -0.2396(4) 0.2564(3) 0.9430(3) 0.0581(10) Uani 1 1 d . . . . . C7 C -0.3783(4) 0.2674(4) 1.0051(3) 0.0737(12) Uani 1 1 d D U . . . C8 C 0.1719(5) 0.0311(4) 0.6384(4) 0.0760(14) Uani 1 1 d . . . . . C9 C 0.0421(4) 0.0996(3) 0.6666(3) 0.0530(9) Uani 1 1 d . . . . . C10 C -0.0797(4) 0.0754(3) 0.6731(3) 0.0604(11) Uani 1 1 d . . . . . H10 H -0.080275 0.014834 0.662818 0.072 Uiso 1 1 calc R . . . . C11 C -0.2007(4) 0.1350(3) 0.6938(3) 0.0495(8) Uani 1 1 d . . . . . C12 C -0.3316(4) 0.1057(4) 0.6957(4) 0.0674(12) Uani 1 1 d . . . . . C13 C -0.4446(5) 0.5793(4) 0.6623(4) 0.0808(14) Uani 1 1 d . . . . . C14 C -0.3117(4) 0.5310(4) 0.6916(3) 0.0622(11) Uani 1 1 d . . . . . C15 C -0.2616(5) 0.5786(4) 0.7319(4) 0.0697(12) Uani 1 1 d . . . . . H15 H -0.313542 0.637573 0.743465 0.084 Uiso 1 1 calc R . . . . C16 C -0.1398(4) 0.5444(3) 0.7559(3) 0.0598(10) Uani 1 1 d . . . . . C17 C -0.0914(5) 0.6037(4) 0.7988(4) 0.0771(14) Uani 1 1 d . . . . . C21 C 0.196(3) 0.250(2) 0.939(2) 0.170(11) Uani 0.5 1 d D U P A 1 H21A H 0.246984 0.258610 0.878421 0.256 Uiso 0.5 1 calc GR . P A 1 H21B H 0.254741 0.235615 0.978268 0.256 Uiso 0.5 1 calc GR . P A 1 H21C H 0.135966 0.314215 0.937632 0.256 Uiso 0.5 1 calc GR . P A 1 C22 C 0.085(3) 0.130(3) 1.0763(10) 0.217(16) Uani 0.5 1 d D U P A 1 H22A H 0.022505 0.186334 1.090274 0.326 Uiso 0.5 1 calc GR . P A 1 H22B H 0.163832 0.120350 1.096496 0.326 Uiso 0.5 1 calc GR . P A 1 H22C H 0.046134 0.064562 1.106968 0.326 Uiso 0.5 1 calc GR . P A 1 C23 C 0.203(2) 0.077(2) 0.936(2) 0.138(10) Uani 0.5 1 d D U P A 1 H23A H 0.159674 0.015489 0.958147 0.208 Uiso 0.5 1 calc GR . P A 1 H23B H 0.286486 0.056117 0.954272 0.208 Uiso 0.5 1 calc GR . P A 1 H23C H 0.218420 0.108627 0.870634 0.208 Uiso 0.5 1 calc GR . P A 1 C22A C 0.086(2) 0.0587(17) 1.0628(11) 0.158(10) Uani 0.5 1 d D U P A 2 H22D H -0.006356 0.067804 1.090587 0.236 Uiso 0.5 1 calc GR . P A 2 H22E H 0.137639 0.050706 1.104587 0.236 Uiso 0.5 1 calc GR . P A 2 H22F H 0.107689 -0.003879 1.047945 0.236 Uiso 0.5 1 calc GR . P A 2 C23A C 0.150(3) 0.245(2) 0.992(3) 0.191(14) Uani 0.5 1 d D U P A 2 H23D H 0.228049 0.270670 0.948376 0.286 Uiso 0.5 1 calc GR . P A 2 H23E H 0.164409 0.218345 1.052644 0.286 Uiso 0.5 1 calc GR . P A 2 H23F H 0.076962 0.302205 0.985348 0.286 Uiso 0.5 1 calc GR . P A 2 C21A C 0.2426(18) 0.121(2) 0.9179(19) 0.125(9) Uani 0.5 1 d D U P A 2 H21D H 0.224519 0.074104 0.895161 0.188 Uiso 0.5 1 calc GR . P A 2 H21E H 0.307800 0.084017 0.954300 0.188 Uiso 0.5 1 calc GR . P A 2 H21F H 0.275504 0.182197 0.867547 0.188 Uiso 0.5 1 calc GR . P A 2 C24 C -0.4662(15) 0.2156(15) 0.9826(11) 0.113(5) Uani 0.5 1 d D U P B 3 H24A H -0.474485 0.254628 0.920329 0.169 Uiso 0.5 1 calc GR . P B 3 H24B H -0.552284 0.216292 1.022537 0.169 Uiso 0.5 1 calc GR . P B 3 H24C H -0.427330 0.143185 0.990579 0.169 Uiso 0.5 1 calc GR . P B 3 C25 C -0.4199(15) 0.3830(9) 0.9894(12) 0.115(5) Uani 0.5 1 d D U P B 3 H25A H -0.373215 0.403240 1.019835 0.172 Uiso 0.5 1 calc GR . P B 3 H25B H -0.513512 0.395541 1.013084 0.172 Uiso 0.5 1 calc GR . P B 3 H25C H -0.399740 0.424552 0.924990 0.172 Uiso 0.5 1 calc GR . P B 3 C26 C -0.3783(11) 0.1977(11) 1.1076(6) 0.088(3) Uani 0.5 1 d D U P B 3 H26A H -0.342855 0.125168 1.114106 0.133 Uiso 0.5 1 calc GR . P B 3 H26B H -0.467361 0.200564 1.143308 0.133 Uiso 0.5 1 calc GR . P B 3 H26C H -0.324662 0.224608 1.128544 0.133 Uiso 0.5 1 calc GR . P B 3 C24A C -0.3736(15) 0.3037(19) 1.0803(11) 0.151(7) Uani 0.5 1 d D U P B 4 H24D H -0.317619 0.250617 1.118868 0.226 Uiso 0.5 1 calc GR . P B 4 H24E H -0.461378 0.312819 1.116180 0.226 Uiso 0.5 1 calc GR . P B 4 H24F H -0.338704 0.370234 1.052466 0.226 Uiso 0.5 1 calc GR . P B 4 C25A C -0.4695(12) 0.3607(12) 0.9475(9) 0.106(4) Uani 0.5 1 d D U P B 4 H25D H -0.425238 0.422731 0.915151 0.159 Uiso 0.5 1 calc GR . P B 4 H25E H -0.550584 0.376813 0.987256 0.159 Uiso 0.5 1 calc GR . P B 4 H25F H -0.489005 0.340036 0.904465 0.159 Uiso 0.5 1 calc GR . P B 4 C26A C -0.4363(19) 0.1676(12) 1.0367(15) 0.154(8) Uani 0.5 1 d D U P B 4 H26D H -0.427938 0.149287 0.985337 0.230 Uiso 0.5 1 calc GR . P B 4 H26E H -0.528266 0.178514 1.065325 0.230 Uiso 0.5 1 calc GR . P B 4 H26F H -0.390034 0.110687 1.079898 0.230 Uiso 0.5 1 calc GR . P B 4 C31A C 0.1542(8) -0.0776(7) 0.6572(11) 0.256(8) Uani 1 1 d . . . C 6 H31A H 0.105357 -0.108200 0.718847 0.385 Uiso 1 1 calc GR . . C 6 H31B H 0.239334 -0.120097 0.649446 0.385 Uiso 1 1 calc GR . . C 6 H31C H 0.106271 -0.075751 0.615672 0.385 Uiso 1 1 calc GR . . C 6 C32A C 0.2224(14) 0.0844(11) 0.5416(8) 0.300(10) Uani 1 1 d . . . D 6 H32A H 0.209743 0.045752 0.509065 0.451 Uiso 1 1 calc GR . . D 6 H32B H 0.315186 0.087192 0.530425 0.451 Uiso 1 1 calc GR . . D 6 H32C H 0.175821 0.155688 0.521036 0.451 Uiso 1 1 calc GR . . D 6 C33A C 0.2692(9) 0.0241(11) 0.6859(11) 0.263(9) Uani 1 1 d . . . E 6 H33A H 0.293581 0.093501 0.666444 0.394 Uiso 1 1 calc GR . . E 6 H33B H 0.346237 -0.024183 0.672405 0.394 Uiso 1 1 calc GR . . E 6 H33C H 0.232646 -0.001747 0.750515 0.394 Uiso 1 1 calc GR . . E 6 C34 C -0.3194(7) -0.0034(7) 0.6953(8) 0.172(5) Uani 1 1 d . . . . . H34A H -0.269984 -0.004462 0.636706 0.258 Uiso 1 1 calc GR . . . . H34B H -0.406128 -0.021085 0.707153 0.258 Uiso 1 1 calc GR . . . . H34C H -0.274233 -0.054689 0.741820 0.258 Uiso 1 1 calc GR . . . . C35 C -0.4293(8) 0.1094(11) 0.7798(8) 0.216(6) Uani 1 1 d . . . . . H35A H -0.386066 0.079142 0.830174 0.324 Uiso 1 1 calc GR . . . . H35B H -0.498679 0.069303 0.792332 0.324 Uiso 1 1 calc GR . . . . H35C H -0.466431 0.182258 0.771284 0.324 Uiso 1 1 calc GR . . . . C36 C -0.3810(11) 0.1866(9) 0.6172(9) 0.259(9) Uani 1 1 d . . . . . H36A H -0.386160 0.256116 0.617730 0.389 Uiso 1 1 calc GR . . . . H36B H -0.467475 0.175209 0.620094 0.389 Uiso 1 1 calc GR . . . . H36C H -0.321862 0.182071 0.562044 0.389 Uiso 1 1 calc GR . . . . C41 C -0.4366(12) 0.5709(13) 0.5751(8) 0.263(9) Uani 1 1 d . . . . . H41A H -0.384668 0.622644 0.526294 0.394 Uiso 1 1 calc GR . . . . H41B H -0.524175 0.584204 0.564663 0.394 Uiso 1 1 calc GR . . . . H41C H -0.395716 0.500523 0.577423 0.394 Uiso 1 1 calc GR . . . . C42 C -0.5439(9) 0.5138(11) 0.7276(10) 0.272(9) Uani 1 1 d . . . . . H42A H -0.513813 0.440746 0.733657 0.408 Uiso 1 1 calc GR . . . . H42B H -0.625192 0.537988 0.706671 0.408 Uiso 1 1 calc GR . . . . H42C H -0.558565 0.519222 0.785772 0.408 Uiso 1 1 calc GR . . . . C43 C -0.4938(13) 0.6876(9) 0.6596(13) 0.301(11) Uani 1 1 d . . . . . H43A H -0.530133 0.685672 0.720743 0.451 Uiso 1 1 calc GR . . . . H43B H -0.561385 0.719232 0.624830 0.451 Uiso 1 1 calc GR . . . . H43C H -0.422184 0.729395 0.631539 0.451 Uiso 1 1 calc GR . . . . C44 C -0.1587(11) 0.7141(7) 0.7826(9) 0.201(6) Uani 1 1 d . . . . . H44A H -0.151029 0.753349 0.718145 0.302 Uiso 1 1 calc GR . . . . H44B H -0.118142 0.747797 0.806460 0.302 Uiso 1 1 calc GR . . . . H44C H -0.250571 0.713044 0.812646 0.302 Uiso 1 1 calc GR . . . . C45 C -0.1166(16) 0.5414(9) 0.8986(7) 0.242(7) Uani 1 1 d . . . . . H45A H -0.210090 0.550006 0.924175 0.363 Uiso 1 1 calc GR . . . . H45B H -0.071507 0.566581 0.926592 0.363 Uiso 1 1 calc GR . . . . H45C H -0.084589 0.467237 0.909836 0.363 Uiso 1 1 calc GR . . . . C46 C 0.0501(8) 0.6066(11) 0.7645(10) 0.229(7) Uani 1 1 d . . . . . H46A H 0.096217 0.534969 0.779244 0.343 Uiso 1 1 calc GR . . . . H46B H 0.079323 0.642927 0.792166 0.343 Uiso 1 1 calc GR . . . . H46C H 0.068372 0.643788 0.699383 0.343 Uiso 1 1 calc GR . . . . O1 O 0.0280(3) 0.2272(2) 0.84224(19) 0.0598(7) Uani 1 1 d . . . . . O2 O -0.2384(3) 0.2854(3) 0.8597(2) 0.0672(8) Uani 1 1 d . . . . . O3 O 0.0563(3) 0.1777(2) 0.6813(2) 0.0609(7) Uani 1 1 d . . . . . O4 O -0.2124(3) 0.2173(2) 0.7106(2) 0.0601(7) Uani 1 1 d . . . . . O5 O -0.2548(3) 0.4485(2) 0.6762(2) 0.0665(8) Uani 1 1 d . . . . . O6 O -0.0617(3) 0.4642(2) 0.7454(2) 0.0645(8) Uani 1 1 d . . . . . O7 O 0.1488(4) 0.3538(4) 0.6490(3) 0.1055(13) Uani 1 1 d . . . . . O8 O -0.0516(5) 0.3957(3) 0.5528(3) 0.1050(14) Uani 1 1 d . . . . . Dy1 Dy -0.08427(2) 0.31425(2) 0.72650(2) 0.04972(8) Uani 1 1 d . . . . . C1 C 0.2440(8) 0.3721(8) 0.6738(6) 0.144(3) Uani 1 1 d . . . . . H1A H 0.290840 0.425598 0.622935 0.216 Uiso 1 1 calc GR . . . . H1B H 0.304190 0.307343 0.693131 0.216 Uiso 1 1 calc GR . . . . H1C H 0.206362 0.396641 0.723294 0.216 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 C2 0.334(15) 0.101(6) 0.071(4) -0.019(4) -0.030(6) -0.059(7) C3 0.061(3) 0.114(4) 0.077(3) -0.045(3) -0.030(2) 0.009(3) C4 0.052(2) 0.070(3) 0.066(3) -0.037(2) -0.013(2) -0.002(2) C5 0.055(3) 0.092(3) 0.055(2) -0.035(2) -0.010(2) 0.003(2) C6 0.048(2) 0.064(3) 0.061(2) -0.032(2) -0.0009(19) -0.0027(19) C7 0.048(2) 0.093(3) 0.063(3) -0.031(2) 0.006(2) 0.000(2) C8 0.053(3) 0.081(3) 0.107(4) -0.063(3) -0.002(3) -0.001(2) C9 0.047(2) 0.055(2) 0.058(2) -0.0285(19) -0.0070(18) -0.0020(17) C10 0.057(3) 0.052(2) 0.083(3) -0.039(2) -0.014(2) -0.0026(18) C11 0.052(2) 0.048(2) 0.053(2) -0.0206(17) -0.0137(17) -0.0079(17) C12 0.052(2) 0.065(3) 0.101(3) -0.041(3) -0.024(2) -0.008(2) C13 0.063(3) 0.083(3) 0.096(4) -0.035(3) -0.030(3) 0.006(3) C14 0.059(3) 0.057(2) 0.068(3) -0.025(2) -0.015(2) -0.002(2) C15 0.059(3) 0.062(3) 0.097(3) -0.045(3) -0.016(2) 0.003(2) C16 0.059(3) 0.053(2) 0.073(3) -0.034(2) -0.007(2) -0.0091(19) C17 0.077(3) 0.072(3) 0.104(4) -0.056(3) -0.021(3) -0.006(2) C21 0.13(2) 0.187(17) 0.24(3) -0.072(16) -0.105(19) -0.040(16) C22 0.110(16) 0.44(5) 0.097(9) -0.109(17) -0.053(10) 0.02(3) C23 0.085(15) 0.146(17) 0.19(2) -0.084(19) -0.076(14) 0.067(13) C22A 0.089(11) 0.23(2) 0.093(10) 0.015(11) -0.060(10) -0.003(13) C23A 0.14(3) 0.23(2) 0.34(4) -0.21(3) -0.16(3) 0.063(15) C21A 0.057(9) 0.20(3) 0.117(12) -0.083(16) -0.031(7) 0.035(11) C24 0.058(7) 0.174(16) 0.109(11) -0.061(11) 0.006(8) -0.036(10) C25 0.082(10) 0.094(7) 0.131(12) -0.051(8) 0.020(8) 0.014(7) C26 0.065(7) 0.110(8) 0.064(5) -0.029(5) 0.014(4) -0.007(6) C24A 0.095(11) 0.26(2) 0.119(11) -0.132(14) 0.006(8) 0.023(12) C25A 0.057(7) 0.118(9) 0.103(9) -0.039(7) 0.004(6) 0.021(6) C26A 0.104(14) 0.097(9) 0.18(2) -0.039(10) 0.067(13) -0.022(8) C31A 0.085(6) 0.110(6) 0.56(3) -0.190(11) 0.019(9) 0.009(5) C32A 0.252(15) 0.279(15) 0.156(9) -0.058(9) 0.094(10) 0.117(12) C33A 0.112(7) 0.352(17) 0.50(2) -0.352(18) -0.173(11) 0.148(9) C34 0.088(5) 0.140(7) 0.360(15) -0.154(9) -0.056(7) -0.020(5) C35 0.095(6) 0.385(18) 0.256(12) -0.220(13) 0.068(7) -0.133(9) C36 0.222(11) 0.184(10) 0.354(17) 0.076(10) -0.239(13) -0.103(9) C41 0.183(11) 0.42(2) 0.208(12) -0.191(14) -0.142(10) 0.165(12) C42 0.095(7) 0.297(17) 0.314(17) 0.051(13) -0.110(9) -0.062(8) C43 0.244(13) 0.197(11) 0.62(3) -0.262(16) -0.323(18) 0.161(11) C44 0.228(12) 0.128(7) 0.360(16) -0.167(10) -0.173(11) 0.050(7) C45 0.48(2) 0.189(11) 0.153(8) -0.053(8) -0.129(12) -0.154(13) C46 0.100(6) 0.358(16) 0.397(17) -0.323(15) 0.009(8) -0.071(8) O1 0.0426(15) 0.079(2) 0.0632(17) -0.0368(15) -0.0108(13) 0.0005(13) O2 0.0419(15) 0.098(2) 0.0612(18) -0.0365(17) -0.0070(13) -0.0013(15) O3 0.0438(15) 0.0709(18) 0.085(2) -0.0523(17) -0.0059(14) -0.0061(13) O4 0.0445(15) 0.0618(17) 0.087(2) -0.0452(16) -0.0119(14) -0.0018(12) O5 0.0680(19) 0.0609(17) 0.082(2) -0.0370(16) -0.0271(16) 0.0025(14) O6 0.0526(17) 0.0617(18) 0.094(2) -0.0459(17) -0.0187(15) -0.0009(13) O7 0.067(2) 0.138(4) 0.123(3) -0.063(3) 0.010(2) -0.045(2) O8 0.153(4) 0.092(3) 0.068(2) -0.029(2) -0.009(2) -0.036(3) Dy1 0.04295(11) 0.05559(12) 0.05935(12) -0.03394(9) -0.00644(8) -0.00533(7) C1 0.093(5) 0.206(10) 0.136(7) -0.058(6) -0.011(5) -0.055(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' 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 C21 C3 C4 104.0(15) C22 C3 C4 116.1(12) C22 C3 C21 102.6(18) C22 C3 C23 120(2) C23 C3 C4 106.2(12) C23 C3 C21 105.8(17) C22A C3 C4 111.0(9) C23A C3 C4 107.3(15) C23A C3 C22A 113.4(17) C21A C3 C4 113.8(12) C21A C3 C22A 106.2(16) C21A C3 C23A 105.2(16) C5 C4 C3 120.1(4) O1 C4 C3 116.2(4) O1 C4 C5 123.7(4) C6 C5 C4 124.8(4) C5 C6 C7 121.2(4) O2 C6 C5 123.8(4) O2 C6 C7 115.1(4) C6 C7 C26 111.7(5) C6 C7 C25A 108.7(6) C24 C7 C6 106.5(7) C24 C7 C26 103.2(9) C25 C7 C6 107.3(6) C25 C7 C24 116.1(11) C25 C7 C26 111.9(9) C24A C7 C6 111.1(6) C24A C7 C25A 103.9(10) C26A C7 C6 108.8(8) C26A C7 C24A 116.3(13) C26A C7 C25A 107.6(12) C31A C8 C9 113.3(5) C32A C8 C9 107.6(6) C32A C8 C31A 109.6(9) C33A C8 C9 110.2(5) C33A C8 C31A 108.0(9) C33A C8 C32A 108.1(11) C10 C9 C8 120.5(4) O3 C9 C8 115.5(4) O3 C9 C10 124.0(4) C11 C10 C9 124.6(4) C10 C11 C12 121.5(4) O4 C11 C10 123.4(4) O4 C11 C12 115.1(3) C34 C12 C11 114.1(4) C35 C12 C11 109.0(5) C35 C12 C34 107.4(7) C36 C12 C11 107.4(5) C36 C12 C34 110.6(7) C36 C12 C35 108.3(9) C41 C13 C14 109.8(5) C42 C13 C14 108.4(5) C42 C13 C41 104.9(10) C42 C13 C43 106.5(10) C43 C13 C14 114.7(6) C43 C13 C41 112.0(9) C15 C14 C13 120.6(4) O5 C14 C13 115.3(4) O5 C14 C15 124.1(4) C16 C15 C14 124.7(4) C15 C16 C17 120.9(4) O6 C16 C15 123.6(4) O6 C16 C17 115.4(4) C44 C17 C16 114.3(5) C44 C17 C45 108.6(8) C45 C17 C16 106.7(5) C46 C17 C16 110.2(5) C46 C17 C44 108.3(8) C46 C17 C45 108.6(9) C4 O1 Dy1 136.0(3) C6 O2 Dy1 137.2(3) C9 O3 Dy1 136.5(3) C11 O4 Dy1 139.7(3) C14 O5 Dy1 134.9(3) C16 O6 Dy1 134.8(3) C1 O7 Dy1 134.4(5) C2 O8 Dy1 134.2(4) O1 Dy1 O3 78.26(11) O1 Dy1 O5 144.49(10) O1 Dy1 O6 82.75(11) O1 Dy1 O7 76.63(14) O1 Dy1 O8 142.87(14) O2 Dy1 O1 73.17(11) O2 Dy1 O3 124.28(11) O2 Dy1 O4 79.65(11) O2 Dy1 O5 79.98(12) O2 Dy1 O6 84.98(12) O2 Dy1 O7 144.17(13) O2 Dy1 O8 143.95(14) O3 Dy1 O7 66.10(13) O3 Dy1 O8 77.04(13) O4 Dy1 O1 116.31(11) O4 Dy1 O3 71.74(10) O4 Dy1 O5 80.21(11) O4 Dy1 O6 150.18(10) O4 Dy1 O7 132.02(12) O4 Dy1 O8 81.23(13) O5 Dy1 O3 136.99(11) O5 Dy1 O7 116.95(15) O5 Dy1 O8 66.81(14) O6 Dy1 O3 137.25(10) O6 Dy1 O5 72.00(11) O6 Dy1 O7 72.41(13) O6 Dy1 O8 97.17(13) O7 Dy1 O8 68.18(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C2 O8 1.326(8) C3 C4 1.540(6) C3 C21 1.529(14) C3 C22 1.495(13) C3 C23 1.497(13) C3 C22A 1.532(13) C3 C23A 1.500(13) C3 C21A 1.498(12) C4 C5 1.386(6) C4 O1 1.267(5) C5 C6 1.377(6) C6 C7 1.546(6) C6 O2 1.258(5) C7 C24 1.521(11) C7 C25 1.491(10) C7 C26 1.559(9) C7 C24A 1.543(11) C7 C25A 1.558(10) C7 C26A 1.489(12) C8 C9 1.544(6) C8 C31A 1.462(9) C8 C32A 1.445(11) C8 C33A 1.441(10) C9 C10 1.387(6) C9 O3 1.262(5) C10 C11 1.386(6) C11 C12 1.540(6) C11 O4 1.259(4) C12 C34 1.497(8) C12 C35 1.482(9) C12 C36 1.454(10) C13 C14 1.537(7) C13 C41 1.470(11) C13 C42 1.447(11) C13 C43 1.458(10) C14 C15 1.388(6) C14 O5 1.252(5) C15 C16 1.385(6) C16 C17 1.542(6) C16 O6 1.261(5) C17 C44 1.475(9) C17 C45 1.482(11) C17 C46 1.452(9) O1 Dy1 2.293(3) O2 Dy1 2.269(3) O3 Dy1 2.356(3) O4 Dy1 2.280(3) O5 Dy1 2.326(3) O6 Dy1 2.318(3) O7 Dy1 2.516(4) O7 C1 1.315(8) O8 Dy1 2.552(4)