#------------------------------------------------------------------------------ #$Date: 2019-11-17 14:35:15 +0200 (Sun, 17 Nov 2019) $ #$Revision: 230533 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/72/7057232.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_7057232 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_issue 11 _journal_name_full 'New Journal of Chemistry' _journal_page_first 8438 _journal_paper_doi 10.1039/C8NJ00636A _journal_volume 42 _journal_year 2018 _chemical_formula_moiety 'C47 H66 Dy N4 O6' _chemical_formula_sum 'C47 H66 Dy N4 O6' _chemical_formula_weight 945.53 _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 101.826(5) _cell_angle_beta 92.723(5) _cell_angle_gamma 110.819(5) _cell_formula_units_Z 2 _cell_length_a 10.955(5) _cell_length_b 12.357(5) _cell_length_c 19.880(5) _cell_measurement_reflns_used 8117 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.6920 _cell_measurement_theta_min 3.0889 _cell_volume 2440.7(16) _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 0.0406 _diffrn_reflns_av_unetI/netI 0.0468 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 20206 _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 27.499 _diffrn_reflns_theta_min 3.095 _exptl_absorpt_coefficient_mu 1.578 _exptl_absorpt_correction_T_max 0.815 _exptl_absorpt_correction_T_min 0.777 _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 1.287 _exptl_crystal_description block _exptl_crystal_F_000 980 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _refine_diff_density_max 2.506 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 601 _refine_ls_number_reflns 11192 _refine_ls_number_restraints 240 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0407 _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^)+(0.0522P)^2^+1.2079P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0999 _refine_ls_wR_factor_ref 0.1064 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9805 _reflns_number_total 11192 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8nj00636a2.cif _cod_data_source_block 3 _cod_depositor_comments 'Adding full bibliography for 7057229--7057232.cif.' _cod_database_code 7057232 _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 0.821 _shelx_estimated_absorpt_t_min 0.786 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C20-C35A \\sim C35-C20 \\sim C34A-C20 \\sim C34-C20 \\sim C36A-C20 \\sim C36-C20 with sigma of 0.02 C30-C54 \\sim C55A-C30 \\sim C56-C30 \\sim C54A-C30 \\sim C55-C30 \\sim C56A-C30 with sigma of 0.02 3. Rigid bond restraints C30, C54, C55, C56, C54A, C55A, C56A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints C30 \\sim C54 \\sim C55 \\sim C56 \\sim C54A \\sim C55A \\sim C56A: within 3.8A with sigma of 0.04 and sigma for terminal atoms of 0.08 5. Rigid body (RIGU) restrains C35A, C35, C34A, C34, C36A, C36, C20 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C54, C55A, C56, C54A, C55, C56A, C30 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Fixed Sof: C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5) C35A(0.5) H35D(0.5) H35E(0.5) H35F(0.5) C36A(0.5) H36D(0.5) H36E(0.5) H36F(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C55(0.5) H55A(0.5) H55B(0.5) H55C(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C54A(0.5) H54D(0.5) H54E(0.5) H54F(0.5) C55A(0.5) H55D(0.5) H55E(0.5) H55F(0.5) C56A(0.5) H56D(0.5) H56E(0.5) H56F(0.5) 7.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C18(H18), C23(H23), C28(H28), N3(H3A) 7.b Idealised Me refined as rotating group: C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B, H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C34A(H34D,H34E,H34F), C35A(H35D,H35E,H35F), C36A(H36D,H36E,H36F), C41(H41A,H41B,H41C), C42(H42A,H42B, H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A, H46B,H46C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C54A(H54D,H54E, H54F), C55A(H55D,H55E,H55F), C56A(H56D,H56E,H56F) ; _shelx_res_file ; TITL 3 in P-1 3.res created by SHELXL-2016/6 at 20:24:51 on 14-Mar-2018 CELL 0.71069 10.955 12.357 19.88 101.826 92.723 110.819 ZERR 2 0.005 0.005 0.005 0.005 0.005 0.005 LATT 1 SFAC C H Dy N O UNIT 94 132 2 8 12 SADI C20 C35A C35 C20 C34A C20 C34 C20 C36A C20 C36 C20 SADI C30 C54 C55A C30 C56 C30 C54A C30 C55 C30 C56A C30 DELU C30 C54 C55 C56 C54A C55A C56A SIMU 0.04 0.08 3.8 C30 C54 C55 C56 C54A C55A C56A RIGU C35A C35 C34A C34 C36A C36 C20 RIGU C54 C55A C56 C54A C55 C56A C30 L.S. 20 PLAN 25 SIZE 0.16 0.15 0.13 LIST 1 fmap 2 ACTA MERG 2 OMIT -3 55 OMIT -2 1 6 OMIT -3 3 0 OMIT 0 2 5 REM REM REM WGHT 0.052200 1.207900 FVAR 0.11711 C1 1 0.198522 0.528450 0.133254 11.00000 0.07928 0.06373 = 0.05993 0.01901 0.00530 0.03704 AFIX 43 H1 2 0.122673 0.499260 0.153700 11.00000 -1.20000 AFIX 0 C2 1 0.199035 0.598450 0.086343 11.00000 0.11341 0.06963 = 0.06970 0.02374 -0.00223 0.04984 AFIX 43 H2 2 0.124706 0.614435 0.075356 11.00000 -1.20000 AFIX 0 C3 1 0.309664 0.642685 0.057106 11.00000 0.14230 0.05393 = 0.05081 0.02165 0.00937 0.03992 AFIX 43 H3 2 0.311978 0.689909 0.025917 11.00000 -1.20000 AFIX 0 C4 1 0.418865 0.617773 0.073538 11.00000 0.11249 0.03646 = 0.04029 0.01168 0.01619 0.01978 C5 1 0.409892 0.544960 0.120481 11.00000 0.07284 0.03437 = 0.03628 0.00960 0.01574 0.01274 C6 1 0.518936 0.510077 0.135900 11.00000 0.06745 0.04328 = 0.04274 0.00863 0.01961 0.01181 C7 1 0.636098 0.551326 0.106769 11.00000 0.07154 0.05201 = 0.05542 0.00408 0.03040 0.00394 C8 1 0.735309 0.512742 0.122744 11.00000 0.06857 0.08637 = 0.08770 0.01216 0.04216 0.01182 AFIX 43 H8 2 0.814577 0.538796 0.104684 11.00000 -1.20000 AFIX 0 C9 1 0.716058 0.436687 0.164912 11.00000 0.06491 0.10866 = 0.09705 0.01758 0.03023 0.04308 AFIX 43 H9 2 0.781840 0.409459 0.175611 11.00000 -1.20000 AFIX 0 C10 1 0.597151 0.399118 0.192360 11.00000 0.06433 0.07711 = 0.07654 0.02495 0.02429 0.03538 AFIX 43 H10 2 0.585449 0.346576 0.221123 11.00000 -1.20000 AFIX 0 C11 1 0.540111 0.660409 0.043604 11.00000 0.12626 0.03837 = 0.04170 0.01039 0.03280 0.00125 C12 1 0.644139 0.628627 0.059983 11.00000 0.11078 0.04474 = 0.05178 -0.00034 0.04320 -0.00919 C13 1 0.656615 0.761576 -0.029741 11.00000 0.23182 0.05628 = 0.06016 0.01934 0.05422 -0.00704 AFIX 43 H13 2 0.664875 0.808156 -0.061813 11.00000 -1.20000 AFIX 0 C14 1 0.757741 0.731022 -0.013563 11.00000 0.19341 0.06142 = 0.08910 0.00908 0.08939 -0.02110 AFIX 43 H14 2 0.832370 0.756795 -0.035461 11.00000 -1.20000 AFIX 0 C16 1 0.087066 0.183549 0.402885 11.00000 0.04612 0.06276 = 0.05660 0.03115 0.01623 0.00979 C17 1 0.210669 0.254382 0.374411 11.00000 0.04076 0.03941 = 0.04269 0.01615 0.00939 0.00746 C18 1 0.335650 0.268022 0.402249 11.00000 0.04533 0.07058 = 0.05613 0.03646 0.00498 0.01233 AFIX 43 H18 2 0.342091 0.234893 0.439625 11.00000 -1.20000 AFIX 0 C19 1 0.451301 0.327793 0.377923 11.00000 0.04330 0.05596 = 0.05790 0.02304 0.00580 0.01455 C20 1 0.585050 0.338903 0.414152 11.00000 0.04424 0.10438 = 0.08993 0.05186 -0.00302 0.01992 C21 1 0.593873 0.795236 0.324463 11.00000 0.04651 0.04429 = 0.07043 0.01552 0.00657 0.00145 C22 1 0.460277 0.692261 0.313635 11.00000 0.04907 0.03900 = 0.04583 0.01475 0.00518 0.00929 C23 1 0.346771 0.714459 0.328606 11.00000 0.05443 0.03904 = 0.07870 0.00858 0.01381 0.01506 AFIX 43 H23 2 0.355484 0.793107 0.345733 11.00000 -1.20000 AFIX 0 C24 1 0.222525 0.626847 0.319539 11.00000 0.04484 0.05220 = 0.04845 0.01650 0.01168 0.02123 C25 1 0.104316 0.656884 0.342350 11.00000 0.05735 0.06306 = 0.08012 0.01640 0.02294 0.03330 C26 1 -0.108776 0.148518 0.136391 11.00000 0.06196 0.06660 = 0.09051 0.00273 -0.01801 0.00982 C27 1 0.039715 0.180099 0.158866 11.00000 0.05651 0.04651 = 0.04841 0.00896 -0.00069 0.00922 C28 1 0.091207 0.091218 0.156388 11.00000 0.07698 0.03620 = 0.06556 0.00688 0.00382 0.00938 AFIX 43 H28 2 0.033199 0.012495 0.140667 11.00000 -1.20000 AFIX 0 C29 1 0.221907 0.111206 0.175519 11.00000 0.08420 0.04213 = 0.04412 0.01239 0.01511 0.02649 C30 1 0.267964 0.006417 0.172543 11.00000 0.11962 0.05054 = 0.08338 0.01346 0.01265 0.04924 C31 1 -0.000981 0.253618 0.412275 11.00000 0.09170 0.13466 = 0.14677 0.07267 0.07340 0.05678 AFIX 137 H31A 2 0.040789 0.324673 0.448439 11.00000 -1.50000 H31B 2 -0.083274 0.206081 0.424614 11.00000 -1.50000 H31C 2 -0.016689 0.274849 0.369771 11.00000 -1.50000 AFIX 0 C32 1 0.017370 0.068463 0.348670 11.00000 0.09797 0.08866 = 0.12155 0.01085 0.03987 -0.02861 AFIX 137 H32A 2 0.004292 0.086036 0.304650 11.00000 -1.50000 H32B 2 -0.066445 0.025954 0.361698 11.00000 -1.50000 H32C 2 0.070037 0.020370 0.345259 11.00000 -1.50000 AFIX 0 C33 1 0.114532 0.155611 0.471399 11.00000 0.07884 0.22120 = 0.13554 0.14163 0.03146 0.02222 AFIX 137 H33A 2 0.158026 0.099838 0.464645 11.00000 -1.50000 H33B 2 0.032969 0.121661 0.489072 11.00000 -1.50000 H33C 2 0.170014 0.227618 0.503921 11.00000 -1.50000 AFIX 0 PART 1 C34 1 0.577630 0.306963 0.482893 10.50000 0.07348 0.37876 = 0.17826 0.21242 0.01670 0.07154 AFIX 137 H34A 2 0.559200 0.365978 0.515770 10.50000 -1.50000 H34B 2 0.660195 0.303941 0.498837 10.50000 -1.50000 H34C 2 0.508735 0.230477 0.478175 10.50000 -1.50000 AFIX 0 C35 1 0.668157 0.470787 0.433274 10.50000 0.05678 0.12454 = 0.14219 0.01351 -0.03911 0.00358 AFIX 137 H35A 2 0.652527 0.506351 0.396766 10.50000 -1.50000 H35B 2 0.759624 0.481979 0.439716 10.50000 -1.50000 H35C 2 0.645069 0.507737 0.475477 10.50000 -1.50000 AFIX 0 C36 1 0.651375 0.283713 0.361724 10.50000 0.08217 0.20450 = 0.15798 0.01589 -0.01247 0.10219 AFIX 137 H36A 2 0.595520 0.202082 0.342065 10.50000 -1.50000 H36B 2 0.733157 0.287082 0.383535 10.50000 -1.50000 H36C 2 0.668257 0.326352 0.325733 10.50000 -1.50000 AFIX 0 PART 0 PART 2 C34A 1 0.607156 0.417762 0.486478 10.50000 0.16681 0.19029 = 0.15935 -0.05300 -0.11135 0.10337 AFIX 137 H34D 2 0.591174 0.488408 0.483889 10.50000 -1.50000 H34E 2 0.696391 0.439527 0.506748 10.50000 -1.50000 H34F 2 0.547896 0.375264 0.514576 10.50000 -1.50000 AFIX 0 C35A 1 0.693625 0.378011 0.371075 10.50000 0.05237 0.31543 = 0.26598 0.21921 0.05113 0.05738 AFIX 137 H35D 2 0.685385 0.312749 0.333060 10.50000 -1.50000 H35E 2 0.777141 0.403286 0.399069 10.50000 -1.50000 H35F 2 0.687999 0.443085 0.353461 10.50000 -1.50000 AFIX 0 C36A 1 0.581192 0.221850 0.424347 10.50000 0.09435 0.11780 = 0.16786 0.08107 0.00982 0.05014 AFIX 137 H36D 2 0.518879 0.195431 0.455529 10.50000 -1.50000 H36E 2 0.666993 0.230075 0.443545 10.50000 -1.50000 H36F 2 0.555214 0.164499 0.380546 10.50000 -1.50000 AFIX 0 PART 0 C41 1 0.607436 0.840711 0.261948 11.00000 0.13949 0.21037 = 0.13344 0.11011 -0.01792 -0.09290 AFIX 137 H41A 2 0.674941 0.822431 0.238608 11.00000 -1.50000 H41B 2 0.630936 0.925520 0.274323 11.00000 -1.50000 H41C 2 0.525358 0.804117 0.231760 11.00000 -1.50000 AFIX 0 C42 1 0.609703 0.893512 0.385672 11.00000 0.10388 0.12426 = 0.20061 -0.07984 0.05390 -0.04954 AFIX 137 H42A 2 0.538695 0.921089 0.381588 11.00000 -1.50000 H42B 2 0.692031 0.957985 0.387822 11.00000 -1.50000 H42C 2 0.608606 0.864924 0.427134 11.00000 -1.50000 AFIX 0 C43 1 0.700159 0.749905 0.335655 11.00000 0.04914 0.08490 = 0.45338 0.06838 -0.04960 -0.00431 AFIX 137 H43A 2 0.693086 0.722531 0.377676 11.00000 -1.50000 H43B 2 0.784367 0.812803 0.339230 11.00000 -1.50000 H43C 2 0.691674 0.685104 0.297290 11.00000 -1.50000 AFIX 0 C44 1 0.139220 0.786222 0.379913 11.00000 0.10880 0.08145 = 0.17379 0.02113 0.06166 0.05533 AFIX 137 H44A 2 0.198457 0.804670 0.421445 11.00000 -1.50000 H44B 2 0.060468 0.798664 0.391703 11.00000 -1.50000 H44C 2 0.180792 0.837070 0.350329 11.00000 -1.50000 AFIX 0 C45 1 0.006041 0.624670 0.280318 11.00000 0.12102 0.30237 = 0.12834 -0.02590 -0.02710 0.15637 AFIX 137 H45A 2 0.043659 0.672222 0.248454 11.00000 -1.50000 H45B 2 -0.070625 0.639116 0.294179 11.00000 -1.50000 H45C 2 -0.018425 0.541853 0.258230 11.00000 -1.50000 AFIX 0 C46 1 0.045165 0.582328 0.392690 11.00000 0.11922 0.12184 = 0.18467 0.07176 0.11016 0.06923 AFIX 137 H46A 2 0.028969 0.500181 0.372446 11.00000 -1.50000 H46B 2 -0.036314 0.590598 0.402862 11.00000 -1.50000 H46C 2 0.105278 0.608860 0.434731 11.00000 -1.50000 AFIX 0 C51 1 -0.121748 0.219884 0.085778 11.00000 0.08299 0.17232 = 0.10022 0.04470 -0.01572 0.04639 AFIX 137 H51A 2 -0.063501 0.301454 0.103148 11.00000 -1.50000 H51B 2 -0.210923 0.215679 0.079777 11.00000 -1.50000 H51C 2 -0.099121 0.188198 0.042012 11.00000 -1.50000 AFIX 0 C52 1 -0.166312 0.187594 0.201157 11.00000 0.06502 0.14283 = 0.12108 0.03591 0.01823 0.03782 AFIX 137 H52A 2 -0.166943 0.137572 0.232366 11.00000 -1.50000 H52B 2 -0.254746 0.180906 0.188302 11.00000 -1.50000 H52C 2 -0.113457 0.268898 0.223565 11.00000 -1.50000 AFIX 0 C53 1 -0.185686 0.019091 0.107288 11.00000 0.08818 0.08141 = 0.32161 -0.04275 -0.06595 0.00427 AFIX 137 H53A 2 -0.156126 -0.006727 0.064406 11.00000 -1.50000 H53B 2 -0.277521 0.005786 0.099092 11.00000 -1.50000 H53C 2 -0.172974 -0.025195 0.139612 11.00000 -1.50000 AFIX 0 PART 3 C54 1 0.152289 -0.114877 0.163104 10.50000 0.14453 0.03709 = 0.14510 0.01809 0.01558 0.03726 AFIX 137 H54A 2 0.106180 -0.113818 0.202960 10.50000 -1.50000 H54B 2 0.186047 -0.177536 0.158075 10.50000 -1.50000 H54C 2 0.092951 -0.128447 0.122427 10.50000 -1.50000 AFIX 0 C55 1 0.335632 0.027419 0.244907 10.50000 0.14887 0.06794 = 0.10362 0.03694 0.00088 0.05914 AFIX 137 H55A 2 0.412264 0.099775 0.254759 10.50000 -1.50000 H55B 2 0.361447 -0.038203 0.247824 10.50000 -1.50000 H55C 2 0.276063 0.033991 0.277991 10.50000 -1.50000 AFIX 0 C56 1 0.350800 0.000498 0.115373 10.50000 0.14427 0.08815 = 0.11377 0.00505 0.03805 0.08034 AFIX 137 H56A 2 0.295114 -0.033484 0.071661 10.50000 -1.50000 H56B 2 0.399797 -0.048200 0.121849 10.50000 -1.50000 H56C 2 0.410720 0.079373 0.115871 10.50000 -1.50000 AFIX 0 PART 0 PART 4 C54A 1 0.412923 0.046864 0.163182 10.50000 0.14368 0.11952 = 0.24382 0.06842 0.07408 0.08951 AFIX 137 H54D 2 0.429670 0.094885 0.129805 10.50000 -1.50000 H54E 2 0.435272 -0.021597 0.147108 10.50000 -1.50000 H54F 2 0.465422 0.092862 0.206717 10.50000 -1.50000 AFIX 0 C55A 1 0.199470 -0.089050 0.107393 10.50000 0.26069 0.11952 = 0.18376 -0.06661 -0.06281 0.12853 AFIX 137 H55D 2 0.120825 -0.146027 0.117499 10.50000 -1.50000 H55E 2 0.257231 -0.128511 0.090666 10.50000 -1.50000 H55F 2 0.176850 -0.053251 0.072632 10.50000 -1.50000 AFIX 0 C56A 1 0.258242 -0.029934 0.238967 10.50000 0.25345 0.14122 = 0.15815 0.10685 0.07408 0.12379 AFIX 137 H56D 2 0.327794 0.027991 0.273309 10.50000 -1.50000 H56E 2 0.265965 -0.106223 0.232947 10.50000 -1.50000 H56F 2 0.174643 -0.035208 0.253841 10.50000 -1.50000 AFIX 0 PART 0 N1 4 0.501262 0.435112 0.179125 11.00000 0.05771 0.05121 = 0.05628 0.01839 0.02128 0.02186 N2 4 0.299936 0.501807 0.149922 11.00000 0.06486 0.04204 = 0.04302 0.01517 0.01144 0.01956 N3 4 0.757818 0.666413 0.031675 11.00000 0.12237 0.06882 = 0.08690 0.00843 0.06467 -0.00649 AFIX 43 H3A 2 0.824756 0.649494 0.042433 11.00000 -1.20000 AFIX 0 N4 4 0.545174 0.728685 -0.002278 11.00000 0.17653 0.05049 = 0.04923 0.01900 0.02864 0.00393 O1 5 0.189232 0.294852 0.324192 11.00000 0.03711 0.06378 = 0.05335 0.03288 0.00825 0.01016 O2 5 0.457598 0.376585 0.327794 11.00000 0.03975 0.05930 = 0.06256 0.03109 0.01000 0.01319 O3 5 0.460268 0.590226 0.290546 11.00000 0.03979 0.04158 = 0.07079 0.01162 0.01109 0.01240 O4 5 0.195749 0.517745 0.292302 11.00000 0.04084 0.04364 = 0.06694 0.00984 0.01525 0.01478 O5 5 0.107710 0.289452 0.179325 11.00000 0.05622 0.04066 = 0.05757 0.00941 -0.00278 0.01491 O6 5 0.310688 0.212748 0.196146 11.00000 0.06176 0.04278 = 0.06693 0.01585 0.01551 0.02273 DY1 3 0.306947 0.397395 0.251072 11.00000 0.04073 0.03592 = 0.04533 0.01681 0.01152 0.01222 HKLF 4 REM 3 in P-1 REM R1 = 0.0407 for 9805 Fo > 4sig(Fo) and 0.0491 for all 11192 data REM 601 parameters refined using 240 restraints END WGHT 0.0522 1.2079 REM Highest difference peak 2.506, deepest hole -0.989, 1-sigma level 0.082 Q1 1 0.0565 0.6018 0.0514 11.00000 0.05 2.51 Q2 1 0.2445 0.3327 0.2305 11.00000 0.05 1.21 Q3 1 0.2395 0.4189 0.2384 11.00000 0.05 1.01 Q4 1 0.3734 0.3675 0.2611 11.00000 0.05 0.84 Q5 1 0.3066 0.4037 0.2941 11.00000 0.05 0.80 Q6 1 0.3726 0.4775 0.2746 11.00000 0.05 0.77 Q7 1 0.3127 0.3994 0.2057 11.00000 0.05 0.65 Q8 1 -0.0264 0.1565 0.3542 11.00000 0.05 0.51 Q9 1 0.0772 0.2647 0.4654 11.00000 0.05 0.50 Q10 1 0.6835 0.7648 0.2693 11.00000 0.05 0.48 Q11 1 0.6596 0.7992 0.3877 11.00000 0.05 0.48 Q12 1 0.0980 0.0696 0.4125 11.00000 0.05 0.44 Q13 1 0.5839 0.9146 0.3154 11.00000 0.05 0.40 Q14 1 -0.0203 0.5375 0.3320 11.00000 0.05 0.38 Q15 1 0.4226 0.4340 0.2597 11.00000 0.05 0.37 Q16 1 0.5281 0.3311 0.3906 11.00000 0.05 0.36 Q17 1 0.3832 0.3980 0.3082 11.00000 0.05 0.35 Q18 1 0.0761 0.7858 0.2443 11.00000 0.05 0.33 Q19 1 0.1793 0.2700 0.1920 11.00000 0.05 0.32 Q20 1 -0.1210 0.1080 0.0603 11.00000 0.05 0.32 Q21 1 0.1270 0.2959 0.2279 11.00000 0.05 0.28 Q22 1 0.1265 0.4814 0.2697 11.00000 0.05 0.28 Q23 1 0.2597 0.0646 0.1793 11.00000 0.05 0.28 Q24 1 0.4214 0.5006 0.1794 11.00000 0.05 0.28 Q25 1 0.5317 0.5901 0.2949 11.00000 0.05 0.28 ; _shelx_res_checksum 59311 _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 C1 C 0.1985(5) 0.5285(4) 0.1333(2) 0.0642(11) Uani 1 1 d . . . . . H1 H 0.122673 0.499260 0.153700 0.077 Uiso 1 1 calc R . . . . C2 C 0.1990(6) 0.5985(5) 0.0863(3) 0.0792(15) Uani 1 1 d . . . . . H2 H 0.124706 0.614435 0.075356 0.095 Uiso 1 1 calc R . . . . C3 C 0.3097(7) 0.6427(4) 0.0571(2) 0.0801(16) Uani 1 1 d . . . . . H3 H 0.311978 0.689909 0.025917 0.096 Uiso 1 1 calc R . . . . C4 C 0.4189(6) 0.6178(3) 0.0735(2) 0.0647(13) Uani 1 1 d . . . . . C5 C 0.4099(4) 0.5450(3) 0.12048(18) 0.0494(9) Uani 1 1 d . . . . . C6 C 0.5189(4) 0.5101(3) 0.1359(2) 0.0535(9) Uani 1 1 d . . . . . C7 C 0.6361(5) 0.5513(4) 0.1068(2) 0.0656(12) Uani 1 1 d . . . . . C8 C 0.7353(5) 0.5127(5) 0.1227(3) 0.0859(17) Uani 1 1 d . . . . . H8 H 0.814577 0.538796 0.104684 0.103 Uiso 1 1 calc R . . . . C9 C 0.7161(5) 0.4367(6) 0.1649(3) 0.0876(17) Uani 1 1 d . . . . . H9 H 0.781840 0.409459 0.175611 0.105 Uiso 1 1 calc R . . . . C10 C 0.5972(5) 0.3991(5) 0.1924(3) 0.0686(12) Uani 1 1 d . . . . . H10 H 0.585449 0.346576 0.221123 0.082 Uiso 1 1 calc R . . . . C11 C 0.5401(7) 0.6604(4) 0.0436(2) 0.0762(17) Uani 1 1 d . . . . . C12 C 0.6441(6) 0.6286(4) 0.0600(2) 0.0806(18) Uani 1 1 d . . . . . C13 C 0.6566(11) 0.7616(6) -0.0297(4) 0.131(4) Uani 1 1 d . . . . . H13 H 0.664875 0.808156 -0.061813 0.157 Uiso 1 1 calc R . . . . C14 C 0.7577(10) 0.7310(6) -0.0136(4) 0.133(4) Uani 1 1 d . . . . . H14 H 0.832370 0.756795 -0.035461 0.159 Uiso 1 1 calc R . . . . C16 C 0.0871(4) 0.1835(4) 0.4029(2) 0.0552(10) Uani 1 1 d . . . . . C17 C 0.2107(3) 0.2544(3) 0.37441(18) 0.0419(7) Uani 1 1 d . . . . . C18 C 0.3357(4) 0.2680(4) 0.4022(2) 0.0567(10) Uani 1 1 d . . . . . H18 H 0.342091 0.234893 0.439625 0.068 Uiso 1 1 calc R . . . . C19 C 0.4513(4) 0.3278(4) 0.3779(2) 0.0521(9) Uani 1 1 d . . . . . C20 C 0.5850(4) 0.3389(5) 0.4142(3) 0.0777(14) Uani 1 1 d D U . . . C21 C 0.5939(4) 0.7952(4) 0.3245(2) 0.0579(10) Uani 1 1 d . . . . . C22 C 0.4603(4) 0.6923(3) 0.31363(19) 0.0460(8) Uani 1 1 d . . . . . C23 C 0.3468(4) 0.7145(4) 0.3286(2) 0.0587(10) Uani 1 1 d . . . . . H23 H 0.355484 0.793107 0.345733 0.070 Uiso 1 1 calc R . . . . C24 C 0.2225(4) 0.6268(3) 0.3195(2) 0.0467(8) Uani 1 1 d . . . . . C25 C 0.1043(5) 0.6569(4) 0.3423(3) 0.0634(11) Uani 1 1 d . . . . . C26 C -0.1088(5) 0.1485(5) 0.1364(3) 0.0805(15) Uani 1 1 d . . . . . C27 C 0.0397(4) 0.1801(4) 0.1589(2) 0.0539(9) Uani 1 1 d . . . . . C28 C 0.0912(5) 0.0912(4) 0.1564(2) 0.0639(11) Uani 1 1 d . . . . . H28 H 0.033199 0.012495 0.140667 0.077 Uiso 1 1 calc R . . . . C29 C 0.2219(5) 0.1112(3) 0.1755(2) 0.0554(10) Uani 1 1 d . . . . . C30 C 0.2680(6) 0.0064(4) 0.1725(3) 0.0800(14) Uani 1 1 d D U . . . C31 C -0.0010(7) 0.2536(7) 0.4123(4) 0.112(2) Uani 1 1 d . . . . . H31A H 0.040789 0.324673 0.448439 0.168 Uiso 1 1 calc GR . . . . H31B H -0.083274 0.206081 0.424614 0.168 Uiso 1 1 calc GR . . . . H31C H -0.016689 0.274849 0.369771 0.168 Uiso 1 1 calc GR . . . . C32 C 0.0174(7) 0.0685(6) 0.3487(4) 0.122(3) Uani 1 1 d . . . . . H32A H 0.004292 0.086036 0.304650 0.183 Uiso 1 1 calc GR . . . . H32B H -0.066445 0.025954 0.361698 0.183 Uiso 1 1 calc GR . . . . H32C H 0.070037 0.020370 0.345259 0.183 Uiso 1 1 calc GR . . . . C33 C 0.1145(6) 0.1556(8) 0.4714(4) 0.139(4) Uani 1 1 d . . . . . H33A H 0.158026 0.099838 0.464645 0.208 Uiso 1 1 calc GR . . . . H33B H 0.032969 0.121661 0.489072 0.208 Uiso 1 1 calc GR . . . . H33C H 0.170014 0.227618 0.503921 0.208 Uiso 1 1 calc GR . . . . C34 C 0.5776(16) 0.307(3) 0.4829(11) 0.191(12) Uani 0.5 1 d D U P A 1 H34A H 0.559200 0.365978 0.515770 0.287 Uiso 0.5 1 calc GR . P A 1 H34B H 0.660195 0.303941 0.498837 0.287 Uiso 0.5 1 calc GR . P A 1 H34C H 0.508735 0.230477 0.478175 0.287 Uiso 0.5 1 calc GR . P A 1 C35 C 0.6682(14) 0.4708(11) 0.4333(11) 0.121(5) Uani 0.5 1 d D U P A 1 H35A H 0.652527 0.506351 0.396766 0.182 Uiso 0.5 1 calc GR . P A 1 H35B H 0.759624 0.481979 0.439716 0.182 Uiso 0.5 1 calc GR . P A 1 H35C H 0.645069 0.507737 0.475477 0.182 Uiso 0.5 1 calc GR . P A 1 C36 C 0.6514(17) 0.284(2) 0.3617(9) 0.140(7) Uani 0.5 1 d D U P A 1 H36A H 0.595520 0.202082 0.342065 0.210 Uiso 0.5 1 calc GR . P A 1 H36B H 0.733157 0.287082 0.383535 0.210 Uiso 0.5 1 calc GR . P A 1 H36C H 0.668257 0.326352 0.325733 0.210 Uiso 0.5 1 calc GR . P A 1 C34A C 0.607(2) 0.418(2) 0.4865(9) 0.181(11) Uani 0.5 1 d D U P A 2 H34D H 0.591174 0.488408 0.483889 0.272 Uiso 0.5 1 calc GR . P A 2 H34E H 0.696391 0.439527 0.506748 0.272 Uiso 0.5 1 calc GR . P A 2 H34F H 0.547896 0.375264 0.514576 0.272 Uiso 0.5 1 calc GR . P A 2 C35A C 0.6936(16) 0.378(3) 0.3711(14) 0.190(12) Uani 0.5 1 d D U P A 2 H35D H 0.685385 0.312749 0.333060 0.285 Uiso 0.5 1 calc GR . P A 2 H35E H 0.777141 0.403286 0.399069 0.285 Uiso 0.5 1 calc GR . P A 2 H35F H 0.687999 0.443085 0.353461 0.285 Uiso 0.5 1 calc GR . P A 2 C36A C 0.5812(16) 0.2219(12) 0.4243(11) 0.117(5) Uani 0.5 1 d D U P A 2 H36D H 0.518879 0.195431 0.455529 0.175 Uiso 0.5 1 calc GR . P A 2 H36E H 0.666993 0.230075 0.443545 0.175 Uiso 0.5 1 calc GR . P A 2 H36F H 0.555214 0.164499 0.380546 0.175 Uiso 0.5 1 calc GR . P A 2 C41 C 0.6074(8) 0.8407(9) 0.2619(4) 0.196(6) Uani 1 1 d . . . . . H41A H 0.674941 0.822431 0.238608 0.294 Uiso 1 1 calc GR . . . . H41B H 0.630936 0.925520 0.274323 0.294 Uiso 1 1 calc GR . . . . H41C H 0.525358 0.804117 0.231760 0.294 Uiso 1 1 calc GR . . . . C42 C 0.6097(8) 0.8935(7) 0.3857(5) 0.186(5) Uani 1 1 d . . . . . H42A H 0.538695 0.921089 0.381588 0.279 Uiso 1 1 calc GR . . . . H42B H 0.692031 0.957985 0.387822 0.279 Uiso 1 1 calc GR . . . . H42C H 0.608606 0.864924 0.427134 0.279 Uiso 1 1 calc GR . . . . C43 C 0.7002(6) 0.7499(7) 0.3357(8) 0.206(7) Uani 1 1 d . . . . . H43A H 0.693086 0.722531 0.377676 0.309 Uiso 1 1 calc GR . . . . H43B H 0.784367 0.812803 0.339230 0.309 Uiso 1 1 calc GR . . . . H43C H 0.691674 0.685104 0.297290 0.309 Uiso 1 1 calc GR . . . . C44 C 0.1392(7) 0.7862(5) 0.3799(4) 0.116(3) Uani 1 1 d . . . . . H44A H 0.198457 0.804670 0.421445 0.174 Uiso 1 1 calc GR . . . . H44B H 0.060468 0.798664 0.391703 0.174 Uiso 1 1 calc GR . . . . H44C H 0.180792 0.837070 0.350329 0.174 Uiso 1 1 calc GR . . . . C45 C 0.0060(8) 0.6247(10) 0.2803(4) 0.176(5) Uani 1 1 d . . . . . H45A H 0.043659 0.672222 0.248454 0.263 Uiso 1 1 calc GR . . . . H45B H -0.070625 0.639116 0.294179 0.263 Uiso 1 1 calc GR . . . . H45C H -0.018425 0.541853 0.258230 0.263 Uiso 1 1 calc GR . . . . C46 C 0.0452(7) 0.5823(7) 0.3927(5) 0.126(3) Uani 1 1 d . . . . . H46A H 0.028969 0.500181 0.372446 0.190 Uiso 1 1 calc GR . . . . H46B H -0.036314 0.590598 0.402862 0.190 Uiso 1 1 calc GR . . . . H46C H 0.105278 0.608860 0.434731 0.190 Uiso 1 1 calc GR . . . . C51 C -0.1217(7) 0.2199(8) 0.0858(4) 0.118(3) Uani 1 1 d . . . . . H51A H -0.063501 0.301454 0.103148 0.177 Uiso 1 1 calc GR . . . . H51B H -0.210923 0.215679 0.079777 0.177 Uiso 1 1 calc GR . . . . H51C H -0.099121 0.188198 0.042012 0.177 Uiso 1 1 calc GR . . . . C52 C -0.1663(6) 0.1876(7) 0.2012(4) 0.109(2) Uani 1 1 d . . . . . H52A H -0.166943 0.137572 0.232366 0.164 Uiso 1 1 calc GR . . . . H52B H -0.254746 0.180906 0.188302 0.164 Uiso 1 1 calc GR . . . . H52C H -0.113457 0.268898 0.223565 0.164 Uiso 1 1 calc GR . . . . C53 C -0.1857(8) 0.0191(7) 0.1073(7) 0.189(6) Uani 1 1 d . . . . . H53A H -0.156126 -0.006727 0.064406 0.283 Uiso 1 1 calc GR . . . . H53B H -0.277521 0.005786 0.099092 0.283 Uiso 1 1 calc GR . . . . H53C H -0.172974 -0.025195 0.139612 0.283 Uiso 1 1 calc GR . . . . C54 C 0.1523(14) -0.1149(8) 0.1631(10) 0.109(4) Uani 0.5 1 d D U P B 3 H54A H 0.106180 -0.113818 0.202960 0.163 Uiso 0.5 1 calc GR . P B 3 H54B H 0.186047 -0.177536 0.158075 0.163 Uiso 0.5 1 calc GR . P B 3 H54C H 0.092951 -0.128447 0.122427 0.163 Uiso 0.5 1 calc GR . P B 3 C55 C 0.3356(18) 0.0274(12) 0.2449(6) 0.100(4) Uani 0.5 1 d D U P B 3 H55A H 0.412264 0.099775 0.254759 0.149 Uiso 0.5 1 calc GR . P B 3 H55B H 0.361447 -0.038203 0.247824 0.149 Uiso 0.5 1 calc GR . P B 3 H55C H 0.276063 0.033991 0.277991 0.149 Uiso 0.5 1 calc GR . P B 3 C56 C 0.3508(17) 0.0005(14) 0.1154(8) 0.107(4) Uani 0.5 1 d D U P B 3 H56A H 0.295114 -0.033484 0.071661 0.161 Uiso 0.5 1 calc GR . P B 3 H56B H 0.399797 -0.048200 0.121849 0.161 Uiso 0.5 1 calc GR . P B 3 H56C H 0.410720 0.079373 0.115871 0.161 Uiso 0.5 1 calc GR . P B 3 C54A C 0.4129(14) 0.0469(17) 0.1632(14) 0.152(6) Uani 0.5 1 d D U P B 4 H54D H 0.429670 0.094885 0.129805 0.228 Uiso 0.5 1 calc GR . P B 4 H54E H 0.435272 -0.021597 0.147108 0.228 Uiso 0.5 1 calc GR . P B 4 H54F H 0.465422 0.092862 0.206717 0.228 Uiso 0.5 1 calc GR . P B 4 C55A C 0.199(3) -0.0891(17) 0.1074(11) 0.191(8) Uani 0.5 1 d D U P B 4 H55D H 0.120825 -0.146027 0.117499 0.286 Uiso 0.5 1 calc GR . P B 4 H55E H 0.257231 -0.128511 0.090666 0.286 Uiso 0.5 1 calc GR . P B 4 H55F H 0.176850 -0.053251 0.072632 0.286 Uiso 0.5 1 calc GR . P B 4 C56A C 0.258(3) -0.0299(19) 0.2390(9) 0.157(7) Uani 0.5 1 d D U P B 4 H56D H 0.327794 0.027991 0.273309 0.236 Uiso 0.5 1 calc GR . P B 4 H56E H 0.265965 -0.106223 0.232947 0.236 Uiso 0.5 1 calc GR . P B 4 H56F H 0.174643 -0.035208 0.253841 0.236 Uiso 0.5 1 calc GR . P B 4 N1 N 0.5013(3) 0.4351(3) 0.17913(17) 0.0533(8) Uani 1 1 d . . . . . N2 N 0.2999(3) 0.5018(3) 0.14992(16) 0.0492(7) Uani 1 1 d . . . . . N3 N 0.7578(6) 0.6664(4) 0.0317(3) 0.1043(19) Uani 1 1 d . . . . . H3A H 0.824756 0.649494 0.042433 0.125 Uiso 1 1 calc R . . . . N4 N 0.5452(6) 0.7287(4) -0.0023(2) 0.1013(19) Uani 1 1 d . . . . . O1 O 0.1892(2) 0.2949(2) 0.32419(14) 0.0508(6) Uani 1 1 d . . . . . O2 O 0.4576(2) 0.3766(2) 0.32779(14) 0.0527(6) Uani 1 1 d . . . . . O3 O 0.4603(2) 0.5902(2) 0.29055(15) 0.0516(6) Uani 1 1 d . . . . . O4 O 0.1957(2) 0.5177(2) 0.29230(14) 0.0510(6) Uani 1 1 d . . . . . O5 O 0.1077(3) 0.2895(2) 0.17932(14) 0.0531(6) Uani 1 1 d . . . . . O6 O 0.3107(3) 0.2127(2) 0.19615(15) 0.0556(7) Uani 1 1 d . . . . . Dy1 Dy 0.30695(2) 0.39739(2) 0.25107(2) 0.03993(7) Uani 1 1 d . . . . . 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 C1 0.079(3) 0.064(3) 0.060(3) 0.019(2) 0.005(2) 0.037(2) C2 0.113(4) 0.070(3) 0.070(3) 0.024(3) -0.002(3) 0.050(3) C3 0.142(5) 0.054(3) 0.051(3) 0.022(2) 0.009(3) 0.040(3) C4 0.112(4) 0.0365(19) 0.040(2) 0.0117(16) 0.016(2) 0.020(2) C5 0.073(3) 0.0344(17) 0.0363(18) 0.0096(14) 0.0157(17) 0.0127(17) C6 0.067(2) 0.0433(19) 0.043(2) 0.0086(16) 0.0196(18) 0.0118(18) C7 0.072(3) 0.052(2) 0.055(2) 0.0041(19) 0.030(2) 0.004(2) C8 0.069(3) 0.086(4) 0.088(4) 0.012(3) 0.042(3) 0.012(3) C9 0.065(3) 0.109(5) 0.097(4) 0.018(4) 0.030(3) 0.043(3) C10 0.064(3) 0.077(3) 0.077(3) 0.025(3) 0.024(2) 0.035(3) C11 0.126(5) 0.038(2) 0.042(2) 0.0104(17) 0.033(3) 0.001(3) C12 0.111(4) 0.045(2) 0.052(3) 0.000(2) 0.043(3) -0.009(3) C13 0.232(11) 0.056(4) 0.060(4) 0.019(3) 0.054(6) -0.007(5) C14 0.193(9) 0.061(4) 0.089(5) 0.009(3) 0.089(6) -0.021(5) C16 0.046(2) 0.063(2) 0.057(2) 0.031(2) 0.0162(18) 0.0098(19) C17 0.0408(18) 0.0394(17) 0.0427(18) 0.0161(15) 0.0094(14) 0.0075(15) C18 0.045(2) 0.071(3) 0.056(2) 0.036(2) 0.0050(17) 0.0123(19) C19 0.043(2) 0.056(2) 0.058(2) 0.0230(19) 0.0058(17) 0.0145(18) C20 0.044(2) 0.104(4) 0.090(3) 0.052(3) -0.003(2) 0.020(2) C21 0.047(2) 0.044(2) 0.070(3) 0.0155(19) 0.0066(19) 0.0014(17) C22 0.049(2) 0.0390(18) 0.0458(19) 0.0147(15) 0.0052(16) 0.0093(16) C23 0.054(2) 0.0390(19) 0.079(3) 0.0086(19) 0.014(2) 0.0151(18) C24 0.0448(19) 0.052(2) 0.048(2) 0.0165(17) 0.0117(16) 0.0212(17) C25 0.057(2) 0.063(3) 0.080(3) 0.016(2) 0.023(2) 0.033(2) C26 0.062(3) 0.067(3) 0.091(4) 0.003(3) -0.018(3) 0.010(2) C27 0.057(2) 0.047(2) 0.048(2) 0.0090(17) -0.0007(18) 0.0092(18) C28 0.077(3) 0.0362(19) 0.066(3) 0.0069(18) 0.004(2) 0.009(2) C29 0.084(3) 0.042(2) 0.044(2) 0.0124(16) 0.015(2) 0.026(2) C30 0.120(4) 0.051(2) 0.083(3) 0.013(2) 0.013(3) 0.049(3) C31 0.092(4) 0.135(6) 0.147(6) 0.073(5) 0.073(4) 0.057(4) C32 0.098(5) 0.089(4) 0.122(5) 0.011(4) 0.040(4) -0.029(4) C33 0.079(4) 0.221(9) 0.136(6) 0.142(7) 0.031(4) 0.022(5) C34 0.073(9) 0.38(3) 0.178(15) 0.21(2) 0.017(13) 0.072(18) C35 0.057(7) 0.125(8) 0.142(14) 0.014(9) -0.039(8) 0.004(7) C36 0.082(12) 0.204(19) 0.158(12) 0.016(13) -0.012(9) 0.102(14) C34A 0.17(2) 0.19(2) 0.159(12) -0.053(13) -0.111(14) 0.103(19) C35A 0.052(9) 0.32(3) 0.27(2) 0.22(2) 0.051(13) 0.057(16) C36A 0.094(10) 0.118(10) 0.168(15) 0.081(10) 0.010(11) 0.050(9) C41 0.139(7) 0.210(10) 0.133(7) 0.110(7) -0.018(5) -0.093(7) C42 0.104(6) 0.124(6) 0.201(9) -0.080(6) 0.054(6) -0.050(5) C43 0.049(3) 0.085(5) 0.45(2) 0.068(8) -0.050(7) -0.004(3) C44 0.109(5) 0.081(4) 0.174(7) 0.021(4) 0.062(5) 0.055(4) C45 0.121(6) 0.302(13) 0.128(6) -0.026(7) -0.027(5) 0.156(8) C46 0.119(5) 0.122(6) 0.185(8) 0.072(5) 0.110(6) 0.069(5) C51 0.083(4) 0.172(8) 0.100(5) 0.045(5) -0.016(4) 0.046(5) C52 0.065(3) 0.143(6) 0.121(5) 0.036(5) 0.018(3) 0.038(4) C53 0.088(5) 0.081(5) 0.322(15) -0.043(7) -0.066(7) 0.004(4) C54 0.145(10) 0.037(4) 0.145(11) 0.018(6) 0.016(8) 0.037(5) C55 0.149(13) 0.068(7) 0.104(6) 0.037(6) 0.001(7) 0.059(7) C56 0.144(11) 0.088(9) 0.114(8) 0.005(7) 0.038(8) 0.080(8) C54A 0.144(8) 0.120(13) 0.244(18) 0.068(12) 0.074(10) 0.090(9) C55A 0.261(17) 0.120(13) 0.184(11) -0.067(10) -0.063(14) 0.129(12) C56A 0.25(2) 0.141(15) 0.158(9) 0.107(10) 0.074(12) 0.124(14) N1 0.0577(19) 0.0512(18) 0.0563(19) 0.0184(15) 0.0213(16) 0.0219(16) N2 0.065(2) 0.0420(16) 0.0430(16) 0.0152(13) 0.0114(15) 0.0196(15) N3 0.122(4) 0.069(3) 0.087(3) 0.008(2) 0.065(3) -0.006(3) N4 0.177(5) 0.050(2) 0.049(2) 0.0190(19) 0.029(3) 0.004(3) O1 0.0371(13) 0.0638(17) 0.0533(15) 0.0329(13) 0.0083(11) 0.0102(12) O2 0.0397(13) 0.0593(16) 0.0626(16) 0.0311(14) 0.0100(12) 0.0132(12) O3 0.0398(13) 0.0416(14) 0.0708(18) 0.0116(13) 0.0111(12) 0.0124(11) O4 0.0408(13) 0.0436(14) 0.0669(17) 0.0098(12) 0.0153(12) 0.0148(11) O5 0.0562(16) 0.0407(14) 0.0576(16) 0.0094(12) -0.0028(13) 0.0149(12) O6 0.0618(17) 0.0428(14) 0.0669(17) 0.0158(13) 0.0155(14) 0.0227(13) Dy1 0.04073(10) 0.03592(9) 0.04533(11) 0.01681(7) 0.01152(7) 0.01222(7) 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 N2 C1 C2 123.1(5) C3 C2 C1 118.8(5) C2 C3 C4 120.0(4) C3 C4 C5 117.8(5) C3 C4 C11 123.2(5) C5 C4 C11 119.0(5) C4 C5 C6 119.8(4) N2 C5 C4 122.1(4) N2 C5 C6 118.1(3) C7 C6 C5 121.1(4) N1 C6 C5 116.7(3) N1 C6 C7 122.3(4) C6 C7 C12 118.1(5) C8 C7 C6 118.0(5) C8 C7 C12 123.9(5) C9 C8 C7 119.3(5) C8 C9 C10 119.9(5) N1 C10 C9 122.6(5) C12 C11 C4 120.5(4) N4 C11 C4 117.7(6) N4 C11 C12 121.7(5) C11 C12 C7 121.5(4) N3 C12 C7 117.2(6) N3 C12 C11 121.3(5) N4 C13 C14 123.1(7) N3 C14 C13 123.8(7) C31 C16 C17 108.8(4) C31 C16 C32 109.1(5) C31 C16 C33 108.3(5) C32 C16 C17 106.8(4) C32 C16 C33 109.5(5) C33 C16 C17 114.3(4) C18 C17 C16 121.1(3) O1 C17 C16 115.0(3) O1 C17 C18 123.8(3) C19 C18 C17 124.3(4) C18 C19 C20 119.5(4) O2 C19 C18 124.8(4) O2 C19 C20 115.7(4) C34 C20 C19 114.1(7) C34 C20 C35 102.9(14) C35 C20 C19 105.6(7) C36 C20 C19 108.1(7) C36 C20 C34 118.9(14) C36 C20 C35 105.8(12) C34A C20 C19 107.6(8) C35A C20 C19 111.6(9) C35A C20 C34A 115.3(16) C36A C20 C19 111.3(7) C36A C20 C34A 105.5(12) C36A C20 C35A 105.4(12) C41 C21 C22 108.0(4) C41 C21 C42 109.7(7) C41 C21 C43 109.5(8) C42 C21 C22 113.1(4) C43 C21 C22 109.1(4) C43 C21 C42 107.4(7) C23 C22 C21 120.5(3) O3 C22 C21 116.1(3) O3 C22 C23 123.5(4) C24 C23 C22 124.1(4) C23 C24 C25 121.1(4) O4 C24 C23 124.3(4) O4 C24 C25 114.6(3) C44 C25 C24 114.2(4) C45 C25 C24 108.5(4) C45 C25 C44 110.2(6) C45 C25 C46 109.6(7) C46 C25 C24 107.5(4) C46 C25 C44 106.7(5) C51 C26 C27 108.7(5) C51 C26 C52 108.2(5) C52 C26 C27 106.9(4) C53 C26 C27 114.4(5) C53 C26 C51 110.8(6) C53 C26 C52 107.6(7) C28 C27 C26 121.2(4) O5 C27 C26 115.3(4) O5 C27 C28 123.5(4) C29 C28 C27 125.0(4) C28 C29 C30 120.9(4) O6 C29 C28 124.0(4) O6 C29 C30 115.1(4) C29 C30 C54 113.0(6) C55 C30 C29 104.9(7) C55 C30 C54 103.3(9) C56 C30 C29 109.8(7) C56 C30 C54 109.9(9) C56 C30 C55 115.8(11) C54A C30 C29 109.3(8) C55A C30 C29 109.1(8) C55A C30 C54A 104.2(14) C56A C30 C29 110.5(9) C56A C30 C54A 106.0(15) C56A C30 C55A 117.3(14) C6 N1 Dy1 120.8(3) C10 N1 C6 118.0(4) C10 N1 Dy1 120.2(3) C1 N2 C5 118.2(4) C1 N2 Dy1 121.9(3) C5 N2 Dy1 119.3(3) C14 N3 C12 114.9(7) C13 N4 C11 115.0(7) C17 O1 Dy1 138.0(2) C19 O2 Dy1 135.5(2) C22 O3 Dy1 137.8(2) C24 O4 Dy1 137.8(2) C27 O5 Dy1 133.3(3) C29 O6 Dy1 132.5(3) N1 Dy1 N2 62.44(11) O1 Dy1 N1 148.42(11) O1 Dy1 N2 146.12(10) O1 Dy1 O2 73.47(9) O1 Dy1 O3 121.75(10) O1 Dy1 O4 79.87(10) O1 Dy1 O5 79.90(10) O1 Dy1 O6 84.04(10) O2 Dy1 N1 81.61(11) O2 Dy1 N2 140.12(10) O2 Dy1 O3 76.78(10) O2 Dy1 O5 141.93(10) O2 Dy1 O6 78.57(10) O3 Dy1 N1 69.03(10) O3 Dy1 N2 74.70(10) O3 Dy1 O5 141.20(9) O3 Dy1 O6 136.27(10) O4 Dy1 N1 130.06(10) O4 Dy1 N2 77.99(10) O4 Dy1 O2 118.47(10) O4 Dy1 O3 72.19(9) O4 Dy1 O5 82.00(10) O4 Dy1 O6 151.40(10) O5 Dy1 N1 110.61(11) O5 Dy1 N2 71.90(10) O5 Dy1 O6 71.96(10) O6 Dy1 N1 72.07(10) O6 Dy1 N2 104.07(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.395(6) C1 N2 1.312(6) C2 C3 1.353(8) C3 C4 1.378(8) C4 C5 1.407(5) C4 C11 1.450(7) C5 C6 1.446(6) C5 N2 1.348(5) C6 C7 1.403(6) C6 N1 1.360(5) C7 C8 1.381(8) C7 C12 1.448(7) C8 C9 1.353(8) C9 C10 1.397(7) C10 N1 1.313(6) C11 C12 1.376(8) C11 N4 1.354(6) C12 N3 1.359(6) C13 C14 1.337(12) C13 N4 1.325(10) C14 N3 1.319(10) C16 C17 1.534(5) C16 C31 1.503(7) C16 C32 1.513(7) C16 C33 1.514(7) C17 C18 1.391(5) C17 O1 1.252(4) C18 C19 1.387(5) C19 C20 1.549(6) C19 O2 1.259(5) C20 C34 1.496(11) C20 C35 1.513(11) C20 C36 1.487(12) C20 C34A 1.517(12) C20 C35A 1.497(12) C20 C36A 1.487(11) C21 C22 1.530(5) C21 C41 1.458(8) C21 C42 1.487(8) C21 C43 1.486(8) C22 C23 1.398(6) C22 O3 1.250(4) C23 C24 1.381(6) C24 C25 1.533(5) C24 O4 1.265(4) C25 C44 1.519(7) C25 C45 1.485(8) C25 C46 1.512(8) C26 C27 1.551(6) C26 C51 1.500(9) C26 C52 1.525(9) C26 C53 1.490(8) C27 C28 1.396(6) C27 O5 1.256(5) C28 C29 1.384(7) C29 C30 1.540(6) C29 O6 1.254(5) C30 C54 1.549(10) C30 C55 1.515(11) C30 C56 1.494(11) C30 C54A 1.519(12) C30 C55A 1.511(12) C30 C56A 1.476(12) N1 Dy1 2.579(3) N2 Dy1 2.614(3) O1 Dy1 2.270(2) O2 Dy1 2.311(3) O3 Dy1 2.319(3) O4 Dy1 2.291(2) O5 Dy1 2.331(3) O6 Dy1 2.334(3)