#------------------------------------------------------------------------------ #$Date: 2019-11-17 14:35:15 +0200 (Sun, 17 Nov 2019) $ #$Revision: 230533 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/72/7057231.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_7057231 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 'C45 H65 Dy N2 O6' _chemical_formula_sum 'C45 H65 Dy N2 O6' _chemical_formula_weight 892.49 _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 79.895(5) _cell_angle_beta 87.642(5) _cell_angle_gamma 68.779(5) _cell_formula_units_Z 2 _cell_length_a 11.051(5) _cell_length_b 12.325(5) _cell_length_c 18.666(5) _cell_measurement_reflns_used 7593 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.5436 _cell_measurement_theta_min 3.2594 _cell_volume 2332.5(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 0.997 _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 0.0240 _diffrn_reflns_av_unetI/netI 0.0413 _diffrn_reflns_Laue_measured_fraction_full 0.997 _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 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 18706 _diffrn_reflns_point_group_measured_fraction_full 0.997 _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 3.266 _exptl_absorpt_coefficient_mu 1.646 _exptl_absorpt_correction_T_max 0.744 _exptl_absorpt_correction_T_min 0.692 _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 1.271 _exptl_crystal_description block _exptl_crystal_F_000 926 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.547 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 595 _refine_ls_number_reflns 10700 _refine_ls_number_restraints 153 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0332 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+0.7239P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.0739 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9309 _reflns_number_total 10700 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8nj00636a2.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 7057229--7057232.cif.' _cod_database_code 7057231 _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 0.756 _shelx_estimated_absorpt_t_min 0.703 _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 C13-C31 \\sim C33A-C13 \\sim C32-C13 \\sim C32A-C13 \\sim C33-C13 \\sim C31A-C13 with sigma of 0.02 C18-C42A \\sim C42-C18 \\sim C43A-C18 \\sim C43-C18 \\sim C41A-C18 \\sim C41-C18 with sigma of 0.02 C23-C53A \\sim C51-C23 \\sim C51A-C23 \\sim C53-C23 \\sim C52A-C23 \\sim C52-C23 with sigma of 0.02 3. Rigid body (RIGU) restrains C31, C33A, C32, C32A, C33, C31A, C13 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C42A, C42, C43A, C43, C41A, C41, C18 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C53A, C51, C51A, C53, C52A, C52, C23 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Fixed Sof: C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C31A(0.5) H31D(0.5) H31E(0.5) H31F(0.5) C32A(0.5) H32D(0.5) H32E(0.5) H32F(0.5) C33A(0.5) H33D(0.5) H33E(0.5) H33F(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5) C41A(0.5) H41D(0.5) H41E(0.5) H41F(0.5) C42A(0.5) H42D(0.5) H42E(0.5) H42F(0.5) C43A(0.5) H43D(0.5) H43E(0.5) H43F(0.5) C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C51A(0.5) H51D(0.5) H51E(0.5) H51F(0.5) C52A(0.5) H52D(0.5) H52E(0.5) H52F(0.5) C53A(0.5) H53D(0.5) H53E(0.5) H53F(0.5) 5.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C20(H20), C25(H25) 5.b Idealised Me refined as rotating group: C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C31A(H31D,H31E, H31F), C32A(H32D,H32E,H32F), C33A(H33D,H33E,H33F), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C42(H42A,H42B, H42C), C43(H43A,H43B,H43C), C41A(H41D,H41E,H41F), C42A(H42D,H42E,H42F), C43A(H43D,H43E,H43F), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B, H46C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C51A(H51D,H51E,H51F), C52A(H52D,H52E,H52F), C53A(H53D,H53E,H53F), C54(H54A, H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C) ; _shelx_res_file ; TITL 2 in P-1 2.res created by SHELXL-2016/6 at 16:43:06 on 14-Mar-2018 CELL 0.71069 11.051 12.325 18.666 79.895 87.642 68.779 ZERR 2 0.005 0.005 0.005 0.005 0.005 0.005 LATT 1 SFAC C H Dy N O UNIT 90 130 2 4 12 SADI C13 C31 C33A C13 C32 C13 C32A C13 C33 C13 C31A C13 SADI C18 C42A C42 C18 C43A C18 C43 C18 C41A C18 C41 C18 SADI C23 C53A C51 C23 C51A C23 C53 C23 C52A C23 C52 C23 RIGU C31 C33A C32 C32A C33 C31A C13 RIGU C42A C42 C43A C43 C41A C41 C18 RIGU C53A C51 C51A C53 C52A C52 C23 L.S. 4 PLAN 25 SIZE 0.23 0.2 0.18 LIST 1 fmap 2 acta MERG 2 OMIT -3 55 OMIT 5 -6 2 OMIT 2 1 6 OMIT 3 0 1 OMIT -3 -1 2 OMIT 3 3 0 REM REM REM WGHT 0.029400 0.723900 FVAR 0.12450 C1 1 -0.157059 0.943635 0.329329 11.00000 0.06059 0.08263 = 0.06939 -0.01837 0.01029 -0.03852 AFIX 43 H1 2 -0.144539 0.889165 0.298417 11.00000 -1.20000 AFIX 0 C2 1 -0.278761 0.988987 0.359523 11.00000 0.05106 0.11156 = 0.08210 -0.00520 0.00861 -0.03912 AFIX 43 H2 2 -0.345872 0.965462 0.348567 11.00000 -1.20000 AFIX 0 C3 1 -0.298009 1.067792 0.405041 11.00000 0.05668 0.09676 = 0.08126 -0.00957 0.02493 -0.01699 AFIX 43 H3 2 -0.379412 1.099796 0.424609 11.00000 -1.20000 AFIX 0 C4 1 -0.197597 1.101066 0.422665 11.00000 0.05976 0.06335 = 0.05605 -0.00574 0.02169 -0.01132 C5 1 -0.077519 1.052749 0.388859 11.00000 0.05657 0.04294 = 0.04623 -0.00483 0.01223 -0.01496 C6 1 0.029154 1.085429 0.403669 11.00000 0.06361 0.03704 = 0.03912 -0.00688 0.00778 -0.01525 C7 1 0.016241 1.162157 0.453992 11.00000 0.09840 0.04681 = 0.04460 -0.01185 0.01142 -0.02329 C8 1 -0.206081 1.178435 0.472537 11.00000 0.09489 0.07258 = 0.06904 -0.02088 0.03809 -0.00788 AFIX 43 H8 2 -0.284321 1.209971 0.495374 11.00000 -1.20000 AFIX 0 C9 1 -0.105711 1.207506 0.487802 11.00000 0.11727 0.06885 = 0.06803 -0.03473 0.03294 -0.02646 AFIX 43 H9 2 -0.115585 1.258088 0.520985 11.00000 -1.20000 AFIX 0 C10 1 0.124561 1.189032 0.467481 11.00000 0.13363 0.06120 = 0.05462 -0.02429 0.00222 -0.04767 AFIX 43 H10 2 0.119604 1.239458 0.500083 11.00000 -1.20000 AFIX 0 C11 1 0.236941 1.141718 0.433117 11.00000 0.10156 0.06799 = 0.06063 -0.01889 -0.00377 -0.04828 AFIX 43 H11 2 0.309995 1.158073 0.442498 11.00000 -1.20000 AFIX 0 C12 1 0.241318 1.068353 0.383624 11.00000 0.06869 0.05800 = 0.05469 -0.01525 -0.00005 -0.03196 AFIX 43 H12 2 0.318275 1.037713 0.359467 11.00000 -1.20000 AFIX 0 C13 1 -0.102529 0.850829 0.095079 11.00000 0.04723 0.08782 = 0.07347 -0.03114 -0.00963 -0.01925 C14 1 0.024217 0.841656 0.131609 11.00000 0.04545 0.05120 = 0.04958 -0.01276 -0.00464 -0.01545 C15 1 0.144117 0.779865 0.104320 11.00000 0.04984 0.06344 = 0.05047 -0.02847 -0.00298 -0.01212 AFIX 43 H15 2 0.144013 0.744805 0.064090 11.00000 -1.20000 AFIX 0 C16 1 0.263501 0.766884 0.132799 11.00000 0.04359 0.03953 = 0.04183 -0.00875 0.00159 -0.00885 C17 1 0.391768 0.691714 0.101358 11.00000 0.04627 0.05725 = 0.05699 -0.02436 0.00539 -0.00872 C18 1 0.171424 0.543191 0.347998 11.00000 0.11021 0.05861 = 0.07107 -0.00006 -0.01476 -0.05132 C19 1 0.220187 0.646139 0.344325 11.00000 0.07948 0.04865 = 0.04147 -0.00495 -0.00279 -0.03240 C20 1 0.349486 0.625706 0.360215 11.00000 0.07181 0.03961 = 0.06420 -0.00287 -0.01244 -0.01483 AFIX 43 H20 2 0.404226 0.547769 0.375007 11.00000 -1.20000 AFIX 0 C21 1 0.403319 0.713286 0.355646 11.00000 0.05424 0.05502 = 0.04324 -0.01245 0.00071 -0.01561 C22 1 0.548409 0.681851 0.374403 11.00000 0.05011 0.06940 = 0.06096 -0.01153 -0.00471 -0.01190 C23 1 -0.123720 1.316177 0.185832 11.00000 0.05168 0.04623 = 0.07241 -0.00816 -0.00187 -0.00359 C24 1 0.008847 1.211979 0.197522 11.00000 0.04863 0.04223 = 0.04871 -0.00915 -0.00395 -0.00902 C25 1 0.123881 1.232584 0.181001 11.00000 0.05464 0.03961 = 0.08431 -0.00444 0.00321 -0.01747 AFIX 43 H25 2 0.118023 1.309793 0.163434 11.00000 -1.20000 AFIX 0 C26 1 0.245936 1.145174 0.189175 11.00000 0.04941 0.04982 = 0.05023 -0.01061 0.00498 -0.02404 C27 1 0.368032 1.172206 0.163132 11.00000 0.05571 0.06432 = 0.07701 -0.01086 0.01312 -0.03366 PART 1 C31 1 -0.179514 0.982934 0.074889 10.50000 0.06270 0.12974 = 0.11670 0.01633 -0.04571 -0.01459 AFIX 137 H31A 2 -0.184749 1.019839 0.116714 10.50000 -1.50000 H31B 2 -0.265453 0.995011 0.058642 10.50000 -1.50000 H31C 2 -0.136809 1.017121 0.036600 10.50000 -1.50000 AFIX 0 C32 1 -0.082705 0.802362 0.024804 10.50000 0.07310 0.34988 = 0.15503 -0.18506 -0.03198 -0.01155 AFIX 137 H32A 2 -0.032588 0.838435 -0.007334 10.50000 -1.50000 H32B 2 -0.165540 0.819463 0.002183 10.50000 -1.50000 H32C 2 -0.037387 0.718388 0.034904 10.50000 -1.50000 AFIX 0 C33 1 -0.176181 0.799801 0.149559 10.50000 0.07388 0.18315 = 0.14744 0.01721 -0.03217 -0.08804 AFIX 137 H33A 2 -0.125036 0.718558 0.167376 10.50000 -1.50000 H33B 2 -0.255348 0.804610 0.127526 10.50000 -1.50000 H33C 2 -0.196153 0.842983 0.189279 10.50000 -1.50000 AFIX 0 PART 0 PART 2 C31A 1 -0.216062 0.885756 0.143302 10.50000 0.03968 0.34138 = 0.17898 -0.14419 0.00594 -0.03145 AFIX 137 H31D 2 -0.195496 0.834834 0.189832 10.50000 -1.50000 H31E 2 -0.289621 0.878875 0.121573 10.50000 -1.50000 H31F 2 -0.236191 0.966053 0.149559 10.50000 -1.50000 AFIX 0 C32A 1 -0.090828 0.728907 0.080951 10.50000 0.09834 0.12347 = 0.20966 -0.06957 -0.04326 -0.05323 AFIX 137 H32D 2 -0.024759 0.704088 0.045993 10.50000 -1.50000 H32E 2 -0.172356 0.732949 0.062376 10.50000 -1.50000 H32F 2 -0.068024 0.673167 0.125619 10.50000 -1.50000 AFIX 0 C33A 1 -0.121606 0.928368 0.023887 10.50000 0.15544 0.26234 = 0.18178 0.12735 -0.12863 -0.14129 AFIX 137 H33D 2 -0.146916 1.008955 0.030735 10.50000 -1.50000 H33E 2 -0.188356 0.919838 -0.003454 10.50000 -1.50000 H33F 2 -0.042020 0.907015 -0.002175 10.50000 -1.50000 AFIX 0 PART 0 C34 1 0.481638 0.761520 0.091667 11.00000 0.07114 0.11374 = 0.10883 -0.04973 0.03856 -0.04185 AFIX 137 H34A 2 0.447173 0.828987 0.053853 11.00000 -1.50000 H34B 2 0.566059 0.712263 0.078602 11.00000 -1.50000 H34C 2 0.488467 0.787415 0.136421 11.00000 -1.50000 AFIX 0 C35 1 0.374828 0.659688 0.028377 11.00000 0.07740 0.15535 = 0.10297 -0.09091 0.01723 -0.01553 AFIX 137 H35A 2 0.325028 0.609168 0.034443 11.00000 -1.50000 H35B 2 0.458514 0.619274 0.009988 11.00000 -1.50000 H35C 2 0.330242 0.730393 -0.005400 11.00000 -1.50000 AFIX 0 C36 1 0.451140 0.581582 0.156628 11.00000 0.07965 0.06782 = 0.11858 -0.00494 0.01877 0.01012 AFIX 137 H36A 2 0.454899 0.602674 0.203390 11.00000 -1.50000 H36B 2 0.537325 0.538394 0.142499 11.00000 -1.50000 H36C 2 0.399137 0.533302 0.159315 11.00000 -1.50000 AFIX 0 PART 3 C41 1 0.129280 0.549995 0.271595 10.50000 0.14060 0.08270 = 0.06769 -0.02885 0.00268 -0.07665 AFIX 137 H41A 2 0.052023 0.618411 0.258870 10.50000 -1.50000 H41B 2 0.111825 0.480267 0.267999 10.50000 -1.50000 H41C 2 0.196974 0.555670 0.238933 10.50000 -1.50000 AFIX 0 C42 1 0.282397 0.423498 0.366172 10.50000 0.19121 0.04412 = 0.28692 0.05771 -0.13994 -0.05574 AFIX 137 H42A 2 0.349515 0.419212 0.331258 10.50000 -1.50000 H42B 2 0.250188 0.361286 0.364630 10.50000 -1.50000 H42C 2 0.317069 0.414946 0.414023 10.50000 -1.50000 AFIX 0 C43 1 0.054414 0.567108 0.392404 10.50000 0.25294 0.16753 = 0.19726 -0.10570 0.14379 -0.18360 AFIX 137 H43A 2 0.078809 0.555243 0.442759 10.50000 -1.50000 H43B 2 0.011144 0.514381 0.386062 10.50000 -1.50000 H43C 2 -0.003008 0.647294 0.377347 10.50000 -1.50000 AFIX 0 PART 0 PART 4 C41A 1 0.055030 0.578976 0.300130 10.50000 0.46743 0.22876 = 0.50927 0.22265 -0.39886 -0.28163 AFIX 137 H41D 2 -0.021722 0.604698 0.328204 10.50000 -1.50000 H41E 2 0.056265 0.512942 0.279035 10.50000 -1.50000 H41F 2 0.055092 0.642487 0.262119 10.50000 -1.50000 AFIX 0 C42A 1 0.267218 0.432265 0.331832 10.50000 0.30028 0.15483 = 0.36695 -0.19761 0.23358 -0.16788 AFIX 137 H42D 2 0.306771 0.447517 0.286299 10.50000 -1.50000 H42E 2 0.224831 0.377568 0.328755 10.50000 -1.50000 H42F 2 0.332747 0.399113 0.369863 10.50000 -1.50000 AFIX 0 C43A 1 0.125693 0.511919 0.421064 10.50000 0.36480 0.13937 = 0.14485 -0.06978 0.14958 -0.18566 AFIX 137 H43D 2 0.191105 0.500699 0.456802 10.50000 -1.50000 H43E 2 0.108721 0.440207 0.423981 10.50000 -1.50000 H43F 2 0.047410 0.574441 0.430092 10.50000 -1.50000 AFIX 0 PART 0 C44 1 0.555275 0.749534 0.435577 11.00000 0.06449 0.13161 = 0.08265 -0.03555 -0.01736 -0.03055 AFIX 137 H44A 2 0.501017 0.831194 0.422337 11.00000 -1.50000 H44B 2 0.643321 0.743399 0.442296 11.00000 -1.50000 H44C 2 0.525750 0.716014 0.480065 11.00000 -1.50000 AFIX 0 C45 1 0.623356 0.550411 0.399066 11.00000 0.06855 0.08266 = 0.13710 -0.00864 -0.01807 0.00402 AFIX 137 H45A 2 0.587897 0.523193 0.443386 11.00000 -1.50000 H45B 2 0.713069 0.537533 0.407271 11.00000 -1.50000 H45C 2 0.616334 0.507676 0.362082 11.00000 -1.50000 AFIX 0 C46 1 0.610134 0.726646 0.306596 11.00000 0.06738 0.14582 = 0.08357 -0.01306 0.00735 -0.04248 AFIX 137 H46A 2 0.607940 0.684129 0.268521 11.00000 -1.50000 H46B 2 0.698586 0.714599 0.317738 11.00000 -1.50000 H46C 2 0.562708 0.809392 0.290870 11.00000 -1.50000 AFIX 0 PART 5 C51 1 -0.140017 1.391383 0.113438 10.50000 0.08563 0.16741 = 0.07979 0.02318 0.00626 0.00482 AFIX 137 H51A 2 -0.072122 1.423268 0.106639 10.50000 -1.50000 H51B 2 -0.222756 1.454852 0.110087 10.50000 -1.50000 H51C 2 -0.135774 1.344961 0.076491 10.50000 -1.50000 AFIX 0 C52 1 -0.136803 1.392360 0.241071 10.50000 0.10571 0.12059 = 0.15456 -0.09507 -0.01675 0.02087 AFIX 137 H52A 2 -0.115961 1.344215 0.288472 10.50000 -1.50000 H52B 2 -0.224434 1.447631 0.240040 10.50000 -1.50000 H52C 2 -0.078491 1.434601 0.230497 10.50000 -1.50000 AFIX 0 C53 1 -0.237040 1.274019 0.197619 10.50000 0.03851 0.05954 = 0.29596 0.00242 0.00929 -0.01191 AFIX 137 H53A 2 -0.244853 1.237620 0.157473 10.50000 -1.50000 H53B 2 -0.315515 1.340133 0.200935 10.50000 -1.50000 H53C 2 -0.222565 1.217589 0.241918 10.50000 -1.50000 AFIX 0 PART 0 PART 6 C51A 1 -0.211163 1.272298 0.150996 10.50000 0.05741 0.12833 = 0.30188 -0.10535 -0.08628 0.03017 AFIX 137 H51D 2 -0.183016 1.261395 0.102555 10.50000 -1.50000 H51E 2 -0.298274 1.328813 0.148930 10.50000 -1.50000 H51F 2 -0.208761 1.198301 0.178968 10.50000 -1.50000 AFIX 0 C52A 1 -0.165346 1.342043 0.258539 10.50000 0.16000 0.15661 = 0.09658 -0.03547 0.00400 0.10585 AFIX 137 H52D 2 -0.137875 1.269903 0.293275 10.50000 -1.50000 H52E 2 -0.258248 1.378353 0.258461 10.50000 -1.50000 H52F 2 -0.127171 1.394812 0.271491 10.50000 -1.50000 AFIX 0 C53A 1 -0.113378 1.421821 0.136656 10.50000 0.08177 0.08228 = 0.31596 0.10749 0.01594 0.02955 AFIX 137 H53D 2 -0.041396 1.438559 0.152442 10.50000 -1.50000 H53E 2 -0.192012 1.488598 0.138153 10.50000 -1.50000 H53F 2 -0.100080 1.406209 0.087764 10.50000 -1.50000 AFIX 0 PART 0 C54 1 0.338643 1.300059 0.126568 11.00000 0.10268 0.08111 = 0.21537 -0.00148 0.05260 -0.05674 AFIX 137 H54A 2 0.282313 1.318058 0.084877 11.00000 -1.50000 H54B 2 0.418197 1.310855 0.111421 11.00000 -1.50000 H54C 2 0.296913 1.351762 0.160383 11.00000 -1.50000 AFIX 0 C55 1 0.429266 1.095980 0.106722 11.00000 0.09740 0.11729 = 0.14510 -0.04848 0.06989 -0.05595 AFIX 137 H55A 2 0.454775 1.014198 0.128605 11.00000 -1.50000 H55B 2 0.504279 1.112253 0.087987 11.00000 -1.50000 H55C 2 0.367696 1.113000 0.067690 11.00000 -1.50000 AFIX 0 C56 1 0.458730 1.139166 0.226603 11.00000 0.11198 0.25832 = 0.12243 0.02181 -0.02378 -0.13764 AFIX 137 H56A 2 0.419943 1.188668 0.262009 11.00000 -1.50000 H56B 2 0.538276 1.149442 0.210841 11.00000 -1.50000 H56C 2 0.476581 1.058036 0.247974 11.00000 -1.50000 AFIX 0 DY1 3 0.148423 0.923923 0.264402 11.00000 0.03692 0.03904 = 0.04550 -0.01415 0.00419 -0.01504 N1 4 -0.058426 0.974704 0.342725 11.00000 0.05022 0.05505 = 0.05275 -0.00953 0.00790 -0.02285 N2 4 0.141388 1.039869 0.369125 11.00000 0.05502 0.04543 = 0.04578 -0.01315 0.00411 -0.02065 O1 5 0.010986 0.893237 0.185726 11.00000 0.03854 0.06140 = 0.05908 -0.02710 0.00089 -0.01506 O2 5 0.277606 0.810205 0.186964 11.00000 0.03974 0.05888 = 0.05552 -0.02763 0.00263 -0.01118 O3 5 0.135851 0.747199 0.325829 11.00000 0.05511 0.04637 = 0.06858 -0.00822 0.00164 -0.02389 O4 5 0.339747 0.822434 0.335815 11.00000 0.04760 0.04313 = 0.06101 -0.01097 -0.00693 -0.01684 O5 5 0.004073 1.112890 0.221699 11.00000 0.03948 0.04447 = 0.06978 -0.00513 0.00249 -0.01411 O6 5 0.267828 1.038554 0.217355 11.00000 0.03886 0.04743 = 0.06258 -0.00624 0.00611 -0.01665 HKLF 4 REM 2 in P-1 REM R1 = 0.0332 for 9309 Fo > 4sig(Fo) and 0.0423 for all 10700 data REM 595 parameters refined using 153 restraints END WGHT 0.0294 0.7239 REM Highest difference peak 0.547, deepest hole -0.468, 1-sigma level 0.066 Q1 1 0.2306 0.8650 0.2772 11.00000 0.05 0.55 Q2 1 0.1349 0.9184 0.2210 11.00000 0.05 0.51 Q3 1 0.1977 0.4864 0.2977 11.00000 0.05 0.50 Q4 1 0.0674 0.9362 0.2759 11.00000 0.05 0.50 Q5 1 0.1343 0.9588 0.2172 11.00000 0.05 0.50 Q6 1 0.5585 1.2282 0.2031 11.00000 0.05 0.45 Q7 1 0.0626 0.9864 0.2494 11.00000 0.05 0.43 Q8 1 0.4823 1.0620 0.1636 11.00000 0.05 0.37 Q9 1 0.0044 0.6000 0.3438 11.00000 0.05 0.34 Q10 1 0.1536 0.9652 0.3009 11.00000 0.05 0.33 Q11 1 0.3043 0.6298 0.3358 11.00000 0.05 0.33 Q12 1 0.2064 0.4728 0.4105 11.00000 0.05 0.33 Q13 1 0.3722 0.5756 0.0892 11.00000 0.05 0.32 Q14 1 0.4353 0.7483 0.0484 11.00000 0.05 0.32 Q15 1 0.1624 0.8647 0.3255 11.00000 0.05 0.32 Q16 1 0.5214 0.6670 0.1506 11.00000 0.05 0.31 Q17 1 0.5086 0.8449 0.4469 11.00000 0.05 0.31 Q18 1 0.0814 1.2063 0.1746 11.00000 0.05 0.30 Q19 1 0.3033 1.1572 0.1734 11.00000 0.05 0.29 Q20 1 0.3245 0.7245 0.1155 11.00000 0.05 0.29 Q21 1 -0.1976 1.3350 0.1186 11.00000 0.05 0.28 Q22 1 0.1771 0.8282 0.2459 11.00000 0.05 0.27 Q23 1 0.2365 1.0458 0.2377 11.00000 0.05 0.26 Q24 1 0.0849 0.8640 0.2015 11.00000 0.05 0.25 Q25 1 -0.1591 1.0648 0.0618 11.00000 0.05 0.25 ; _shelx_res_checksum 25183 _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 -0.1571(3) 0.9436(4) 0.3293(2) 0.0669(10) Uani 1 1 d . . . . . H1 H -0.144539 0.889165 0.298417 0.080 Uiso 1 1 calc R . . . . C2 C -0.2788(4) 0.9890(4) 0.3595(2) 0.0805(12) Uani 1 1 d . . . . . H2 H -0.345872 0.965462 0.348567 0.097 Uiso 1 1 calc R . . . . C3 C -0.2980(4) 1.0678(4) 0.4050(2) 0.0827(13) Uani 1 1 d . . . . . H3 H -0.379412 1.099796 0.424609 0.099 Uiso 1 1 calc R . . . . C4 C -0.1976(4) 1.1011(3) 0.4227(2) 0.0640(10) Uani 1 1 d . . . . . C5 C -0.0775(3) 1.0527(3) 0.38886(17) 0.0501(7) Uani 1 1 d . . . . . C6 C 0.0292(3) 1.0854(2) 0.40367(16) 0.0476(7) Uani 1 1 d . . . . . C7 C 0.0162(4) 1.1622(3) 0.45399(18) 0.0639(10) Uani 1 1 d . . . . . C8 C -0.2061(5) 1.1784(4) 0.4725(2) 0.0851(14) Uani 1 1 d . . . . . H8 H -0.284321 1.209971 0.495374 0.102 Uiso 1 1 calc R . . . . C9 C -0.1057(5) 1.2075(4) 0.4878(2) 0.0847(13) Uani 1 1 d . . . . . H9 H -0.115585 1.258088 0.520985 0.102 Uiso 1 1 calc R . . . . C10 C 0.1246(5) 1.1890(3) 0.4675(2) 0.0778(12) Uani 1 1 d . . . . . H10 H 0.119604 1.239458 0.500083 0.093 Uiso 1 1 calc R . . . . C11 C 0.2369(4) 1.1417(3) 0.4331(2) 0.0706(10) Uani 1 1 d . . . . . H11 H 0.309995 1.158073 0.442498 0.085 Uiso 1 1 calc R . . . . C12 C 0.2413(4) 1.0684(3) 0.38362(18) 0.0571(8) Uani 1 1 d . . . . . H12 H 0.318275 1.037713 0.359467 0.069 Uiso 1 1 calc R . . . . C13 C -0.1025(3) 0.8508(4) 0.0951(2) 0.0684(10) Uani 1 1 d D U . . . C14 C 0.0242(3) 0.8417(3) 0.13161(17) 0.0486(7) Uani 1 1 d . . . . . C15 C 0.1441(3) 0.7799(3) 0.10432(18) 0.0544(8) Uani 1 1 d . . . . . H15 H 0.144013 0.744805 0.064090 0.065 Uiso 1 1 calc R . . . . C16 C 0.2635(3) 0.7669(2) 0.13280(16) 0.0432(6) Uani 1 1 d . . . . . C17 C 0.3918(3) 0.6917(3) 0.10136(18) 0.0546(8) Uani 1 1 d . . . . . C18 C 0.1714(4) 0.5432(3) 0.3480(2) 0.0750(11) Uani 1 1 d D U . . . C19 C 0.2202(4) 0.6461(3) 0.34433(17) 0.0541(8) Uani 1 1 d . . . . . C20 C 0.3495(4) 0.6257(3) 0.36021(19) 0.0604(9) Uani 1 1 d . . . . . H20 H 0.404226 0.547769 0.375007 0.072 Uiso 1 1 calc R . . . . C21 C 0.4033(3) 0.7133(3) 0.35565(17) 0.0515(7) Uani 1 1 d . . . . . C22 C 0.5484(3) 0.6819(3) 0.3744(2) 0.0627(9) Uani 1 1 d . . . . . C23 C -0.1237(3) 1.3162(3) 0.1858(2) 0.0609(9) Uani 1 1 d D U . . . C24 C 0.0088(3) 1.2120(3) 0.19752(17) 0.0483(7) Uani 1 1 d . . . . . C25 C 0.1239(3) 1.2326(3) 0.1810(2) 0.0602(9) Uani 1 1 d . . . . . H25 H 0.118023 1.309793 0.163434 0.072 Uiso 1 1 calc R . . . . C26 C 0.2459(3) 1.1452(3) 0.18917(17) 0.0479(7) Uani 1 1 d . . . . . C27 C 0.3680(3) 1.1722(3) 0.1631(2) 0.0628(9) Uani 1 1 d . . . . . C31 C -0.1795(12) 0.9829(9) 0.0749(8) 0.112(4) Uani 0.5 1 d D U P A 1 H31A H -0.184749 1.019839 0.116714 0.168 Uiso 0.5 1 calc GR . P A 1 H31B H -0.265453 0.995011 0.058642 0.168 Uiso 0.5 1 calc GR . P A 1 H31C H -0.136809 1.017121 0.036600 0.168 Uiso 0.5 1 calc GR . P A 1 C32 C -0.0827(13) 0.802(2) 0.0248(10) 0.192(10) Uani 0.5 1 d D U P A 1 H32A H -0.032588 0.838435 -0.007334 0.287 Uiso 0.5 1 calc GR . P A 1 H32B H -0.165540 0.819463 0.002183 0.287 Uiso 0.5 1 calc GR . P A 1 H32C H -0.037387 0.718388 0.034904 0.287 Uiso 0.5 1 calc GR . P A 1 C33 C -0.1762(12) 0.7998(15) 0.1496(8) 0.128(6) Uani 0.5 1 d D U P A 1 H33A H -0.125036 0.718558 0.167376 0.192 Uiso 0.5 1 calc GR . P A 1 H33B H -0.255348 0.804610 0.127526 0.192 Uiso 0.5 1 calc GR . P A 1 H33C H -0.196153 0.842983 0.189279 0.192 Uiso 0.5 1 calc GR . P A 1 C31A C -0.2161(12) 0.886(2) 0.1433(10) 0.184(10) Uani 0.5 1 d D U P A 2 H31D H -0.195496 0.834834 0.189832 0.277 Uiso 0.5 1 calc GR . P A 2 H31E H -0.289621 0.878875 0.121573 0.277 Uiso 0.5 1 calc GR . P A 2 H31F H -0.236191 0.966053 0.149559 0.277 Uiso 0.5 1 calc GR . P A 2 C32A C -0.0908(13) 0.7289(10) 0.0810(11) 0.133(5) Uani 0.5 1 d D U P A 2 H32D H -0.024759 0.704088 0.045993 0.200 Uiso 0.5 1 calc GR . P A 2 H32E H -0.172356 0.732949 0.062376 0.200 Uiso 0.5 1 calc GR . P A 2 H32F H -0.068024 0.673167 0.125619 0.200 Uiso 0.5 1 calc GR . P A 2 C33A C -0.1216(19) 0.928(2) 0.0239(10) 0.199(10) Uani 0.5 1 d D U P A 2 H33D H -0.146916 1.008955 0.030735 0.298 Uiso 0.5 1 calc GR . P A 2 H33E H -0.188356 0.919838 -0.003454 0.298 Uiso 0.5 1 calc GR . P A 2 H33F H -0.042020 0.907015 -0.002175 0.298 Uiso 0.5 1 calc GR . P A 2 C34 C 0.4816(4) 0.7615(4) 0.0917(3) 0.0926(14) Uani 1 1 d . . . . . H34A H 0.447173 0.828987 0.053853 0.139 Uiso 1 1 calc GR . . . . H34B H 0.566059 0.712263 0.078602 0.139 Uiso 1 1 calc GR . . . . H34C H 0.488467 0.787415 0.136421 0.139 Uiso 1 1 calc GR . . . . C35 C 0.3748(4) 0.6597(5) 0.0284(3) 0.1109(19) Uani 1 1 d . . . . . H35A H 0.325028 0.609168 0.034443 0.166 Uiso 1 1 calc GR . . . . H35B H 0.458514 0.619274 0.009988 0.166 Uiso 1 1 calc GR . . . . H35C H 0.330242 0.730393 -0.005400 0.166 Uiso 1 1 calc GR . . . . C36 C 0.4511(4) 0.5816(4) 0.1566(3) 0.1010(16) Uani 1 1 d . . . . . H36A H 0.454899 0.602674 0.203390 0.151 Uiso 1 1 calc GR . . . . H36B H 0.537325 0.538394 0.142499 0.151 Uiso 1 1 calc GR . . . . H36C H 0.399137 0.533302 0.159315 0.151 Uiso 1 1 calc GR . . . . C41 C 0.1293(12) 0.5500(11) 0.2716(5) 0.085(3) Uani 0.5 1 d D U P B 3 H41A H 0.052023 0.618411 0.258870 0.127 Uiso 0.5 1 calc GR . P B 3 H41B H 0.111825 0.480267 0.267999 0.127 Uiso 0.5 1 calc GR . P B 3 H41C H 0.196974 0.555670 0.238933 0.127 Uiso 0.5 1 calc GR . P B 3 C42 C 0.2824(16) 0.4235(9) 0.3662(12) 0.177(9) Uani 0.5 1 d D U P B 3 H42A H 0.349515 0.419212 0.331258 0.266 Uiso 0.5 1 calc GR . P B 3 H42B H 0.250188 0.361286 0.364630 0.266 Uiso 0.5 1 calc GR . P B 3 H42C H 0.317069 0.414946 0.414023 0.266 Uiso 0.5 1 calc GR . P B 3 C43 C 0.054(2) 0.5671(19) 0.3924(13) 0.170(10) Uani 0.5 1 d D U P B 3 H43A H 0.078809 0.555243 0.442759 0.255 Uiso 0.5 1 calc GR . P B 3 H43B H 0.011144 0.514381 0.386062 0.255 Uiso 0.5 1 calc GR . P B 3 H43C H -0.003008 0.647294 0.377347 0.255 Uiso 0.5 1 calc GR . P B 3 C41A C 0.055(3) 0.579(2) 0.3001(19) 0.38(2) Uani 0.5 1 d D U P B 4 H41D H -0.021722 0.604698 0.328204 0.574 Uiso 0.5 1 calc GR . P B 4 H41E H 0.056265 0.512942 0.279035 0.574 Uiso 0.5 1 calc GR . P B 4 H41F H 0.055092 0.642487 0.262119 0.574 Uiso 0.5 1 calc GR . P B 4 C42A C 0.267(2) 0.4323(14) 0.3318(14) 0.237(13) Uani 0.5 1 d D U P B 4 H42D H 0.306771 0.447517 0.286299 0.355 Uiso 0.5 1 calc GR . P B 4 H42E H 0.224831 0.377568 0.328755 0.355 Uiso 0.5 1 calc GR . P B 4 H42F H 0.332747 0.399113 0.369863 0.355 Uiso 0.5 1 calc GR . P B 4 C43A C 0.126(3) 0.512(2) 0.4211(10) 0.188(12) Uani 0.5 1 d D U P B 4 H43D H 0.191105 0.500699 0.456802 0.282 Uiso 0.5 1 calc GR . P B 4 H43E H 0.108721 0.440207 0.423981 0.282 Uiso 0.5 1 calc GR . P B 4 H43F H 0.047410 0.574441 0.430092 0.282 Uiso 0.5 1 calc GR . P B 4 C44 C 0.5553(4) 0.7495(5) 0.4356(2) 0.0915(14) Uani 1 1 d . . . . . H44A H 0.501017 0.831194 0.422337 0.137 Uiso 1 1 calc GR . . . . H44B H 0.643321 0.743399 0.442296 0.137 Uiso 1 1 calc GR . . . . H44C H 0.525750 0.716014 0.480065 0.137 Uiso 1 1 calc GR . . . . C45 C 0.6234(4) 0.5504(4) 0.3991(3) 0.1056(17) Uani 1 1 d . . . . . H45A H 0.587897 0.523193 0.443386 0.158 Uiso 1 1 calc GR . . . . H45B H 0.713069 0.537533 0.407271 0.158 Uiso 1 1 calc GR . . . . H45C H 0.616334 0.507676 0.362082 0.158 Uiso 1 1 calc GR . . . . C46 C 0.6101(4) 0.7266(5) 0.3066(2) 0.0988(15) Uani 1 1 d . . . . . H46A H 0.607940 0.684129 0.268521 0.148 Uiso 1 1 calc GR . . . . H46B H 0.698586 0.714599 0.317738 0.148 Uiso 1 1 calc GR . . . . H46C H 0.562708 0.809392 0.290870 0.148 Uiso 1 1 calc GR . . . . C51 C -0.140(2) 1.3914(18) 0.1134(7) 0.131(7) Uani 0.5 1 d D U P C 5 H51A H -0.072122 1.423268 0.106639 0.197 Uiso 0.5 1 calc GR . P C 5 H51B H -0.222756 1.454852 0.110087 0.197 Uiso 0.5 1 calc GR . P C 5 H51C H -0.135774 1.344961 0.076491 0.197 Uiso 0.5 1 calc GR . P C 5 C52 C -0.137(3) 1.3924(19) 0.2411(10) 0.135(8) Uani 0.5 1 d D U P C 5 H52A H -0.115961 1.344215 0.288472 0.202 Uiso 0.5 1 calc GR . P C 5 H52B H -0.224434 1.447631 0.240040 0.202 Uiso 0.5 1 calc GR . P C 5 H52C H -0.078491 1.434601 0.230497 0.202 Uiso 0.5 1 calc GR . P C 5 C53 C -0.2370(12) 1.2740(13) 0.1976(12) 0.137(8) Uani 0.5 1 d D U P C 5 H53A H -0.244853 1.237620 0.157473 0.206 Uiso 0.5 1 calc GR . P C 5 H53B H -0.315515 1.340133 0.200935 0.206 Uiso 0.5 1 calc GR . P C 5 H53C H -0.222565 1.217589 0.241918 0.206 Uiso 0.5 1 calc GR . P C 5 C51A C -0.2112(13) 1.2723(17) 0.1510(13) 0.169(10) Uani 0.5 1 d D U P C 6 H51D H -0.183016 1.261395 0.102555 0.253 Uiso 0.5 1 calc GR . P C 6 H51E H -0.298274 1.328813 0.148930 0.253 Uiso 0.5 1 calc GR . P C 6 H51F H -0.208761 1.198301 0.178968 0.253 Uiso 0.5 1 calc GR . P C 6 C52A C -0.165(3) 1.342(2) 0.2585(8) 0.182(14) Uani 0.5 1 d D U P C 6 H52D H -0.137875 1.269903 0.293275 0.273 Uiso 0.5 1 calc GR . P C 6 H52E H -0.258248 1.378353 0.258461 0.273 Uiso 0.5 1 calc GR . P C 6 H52F H -0.127171 1.394812 0.271491 0.273 Uiso 0.5 1 calc GR . P C 6 C53A C -0.1134(19) 1.4218(14) 0.1367(13) 0.195(13) Uani 0.5 1 d D U P C 6 H53D H -0.041396 1.438559 0.152442 0.293 Uiso 0.5 1 calc GR . P C 6 H53E H -0.192012 1.488598 0.138153 0.293 Uiso 0.5 1 calc GR . P C 6 H53F H -0.100080 1.406209 0.087764 0.293 Uiso 0.5 1 calc GR . P C 6 C54 C 0.3386(5) 1.3001(4) 0.1266(4) 0.131(2) Uani 1 1 d . . . . . H54A H 0.282313 1.318058 0.084877 0.196 Uiso 1 1 calc GR . . . . H54B H 0.418197 1.310855 0.111421 0.196 Uiso 1 1 calc GR . . . . H54C H 0.296913 1.351762 0.160383 0.196 Uiso 1 1 calc GR . . . . C55 C 0.4293(5) 1.0960(5) 0.1067(3) 0.1137(19) Uani 1 1 d . . . . . H55A H 0.454775 1.014198 0.128605 0.171 Uiso 1 1 calc GR . . . . H55B H 0.504279 1.112253 0.087987 0.171 Uiso 1 1 calc GR . . . . H55C H 0.367696 1.113000 0.067690 0.171 Uiso 1 1 calc GR . . . . C56 C 0.4587(5) 1.1392(7) 0.2266(3) 0.151(3) Uani 1 1 d . . . . . H56A H 0.419943 1.188668 0.262009 0.226 Uiso 1 1 calc GR . . . . H56B H 0.538276 1.149442 0.210841 0.226 Uiso 1 1 calc GR . . . . H56C H 0.476581 1.058036 0.247974 0.226 Uiso 1 1 calc GR . . . . Dy1 Dy 0.14842(2) 0.92392(2) 0.26440(2) 0.03932(5) Uani 1 1 d . . . . . N1 N -0.0584(2) 0.9747(2) 0.34273(14) 0.0517(6) Uani 1 1 d . . . . . N2 N 0.1414(2) 1.0399(2) 0.36912(13) 0.0474(6) Uani 1 1 d . . . . . O1 O 0.01099(18) 0.89324(19) 0.18573(12) 0.0517(5) Uani 1 1 d . . . . . O2 O 0.27761(18) 0.81020(19) 0.18696(12) 0.0510(5) Uani 1 1 d . . . . . O3 O 0.1359(2) 0.74720(19) 0.32583(13) 0.0553(5) Uani 1 1 d . . . . . O4 O 0.33975(19) 0.82243(18) 0.33581(12) 0.0499(5) Uani 1 1 d . . . . . O5 O 0.00407(19) 1.11289(18) 0.22170(12) 0.0522(5) Uani 1 1 d . . . . . O6 O 0.26783(18) 1.03855(18) 0.21736(12) 0.0499(5) 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 0.061(2) 0.083(3) 0.069(2) -0.018(2) 0.0103(18) -0.039(2) C2 0.051(2) 0.112(3) 0.082(3) -0.005(3) 0.009(2) -0.039(2) C3 0.057(2) 0.097(3) 0.081(3) -0.010(3) 0.025(2) -0.017(2) C4 0.060(2) 0.063(2) 0.056(2) -0.0057(18) 0.0217(17) -0.0113(18) C5 0.0566(19) 0.0429(16) 0.0462(17) -0.0048(14) 0.0122(14) -0.0150(14) C6 0.0636(19) 0.0370(15) 0.0391(16) -0.0069(13) 0.0078(14) -0.0153(14) C7 0.098(3) 0.0468(18) 0.0446(19) -0.0119(16) 0.0114(18) -0.0233(19) C8 0.095(3) 0.073(3) 0.069(3) -0.021(2) 0.038(2) -0.008(2) C9 0.117(4) 0.069(3) 0.068(3) -0.035(2) 0.033(3) -0.026(3) C10 0.134(4) 0.061(2) 0.055(2) -0.0243(19) 0.002(2) -0.048(3) C11 0.102(3) 0.068(2) 0.061(2) -0.019(2) -0.004(2) -0.048(2) C12 0.069(2) 0.058(2) 0.055(2) -0.0153(17) 0.0000(16) -0.0320(17) C13 0.0472(19) 0.088(3) 0.073(2) -0.031(2) -0.0096(16) -0.0192(18) C14 0.0455(17) 0.0512(17) 0.0496(18) -0.0128(15) -0.0046(13) -0.0155(14) C15 0.0498(18) 0.063(2) 0.0505(18) -0.0285(17) -0.0030(14) -0.0121(15) C16 0.0436(16) 0.0395(15) 0.0418(16) -0.0087(13) 0.0016(12) -0.0088(12) C17 0.0463(17) 0.0573(19) 0.057(2) -0.0244(17) 0.0054(14) -0.0087(15) C18 0.110(3) 0.059(2) 0.071(2) -0.0001(19) -0.015(2) -0.051(2) C19 0.079(2) 0.0486(18) 0.0415(17) -0.0050(15) -0.0028(16) -0.0324(18) C20 0.072(2) 0.0396(17) 0.064(2) -0.0029(16) -0.0124(18) -0.0148(16) C21 0.0542(18) 0.0550(19) 0.0432(17) -0.0125(15) 0.0007(14) -0.0156(15) C22 0.0501(19) 0.069(2) 0.061(2) -0.0115(19) -0.0047(16) -0.0119(17) C23 0.0517(19) 0.0462(18) 0.072(2) -0.0082(17) -0.0019(16) -0.0036(15) C24 0.0486(17) 0.0422(16) 0.0487(18) -0.0092(14) -0.0039(13) -0.0090(14) C25 0.055(2) 0.0396(16) 0.084(3) -0.0044(17) 0.0032(17) -0.0175(15) C26 0.0494(17) 0.0498(17) 0.0502(18) -0.0106(15) 0.0050(14) -0.0240(14) C27 0.056(2) 0.064(2) 0.077(2) -0.011(2) 0.0131(18) -0.0337(18) C31 0.063(6) 0.130(7) 0.117(10) 0.016(7) -0.046(7) -0.015(5) C32 0.073(7) 0.35(3) 0.155(12) -0.185(17) -0.032(10) -0.012(15) C33 0.074(10) 0.183(14) 0.147(10) 0.017(11) -0.032(7) -0.088(10) C31A 0.040(6) 0.34(3) 0.179(14) -0.144(18) 0.006(8) -0.031(12) C32A 0.098(8) 0.123(8) 0.210(16) -0.070(10) -0.043(11) -0.053(7) C33A 0.155(18) 0.26(2) 0.182(14) 0.127(15) -0.129(12) -0.141(17) C34 0.071(3) 0.114(4) 0.109(4) -0.050(3) 0.039(3) -0.042(3) C35 0.077(3) 0.155(5) 0.103(4) -0.091(4) 0.017(3) -0.016(3) C36 0.080(3) 0.068(3) 0.119(4) -0.005(3) 0.019(3) 0.010(2) C41 0.141(9) 0.083(6) 0.068(5) -0.029(5) 0.003(5) -0.077(6) C42 0.191(13) 0.044(6) 0.29(2) 0.058(9) -0.140(14) -0.056(6) C43 0.253(19) 0.17(2) 0.197(18) -0.106(16) 0.144(18) -0.184(16) C41A 0.47(3) 0.23(2) 0.51(4) 0.22(3) -0.40(3) -0.28(2) C42A 0.30(2) 0.155(13) 0.37(3) -0.198(18) 0.23(2) -0.168(12) C43A 0.36(3) 0.139(16) 0.145(12) -0.070(11) 0.150(17) -0.186(19) C44 0.064(3) 0.132(4) 0.083(3) -0.036(3) -0.017(2) -0.031(3) C45 0.069(3) 0.083(3) 0.137(5) -0.009(3) -0.018(3) 0.004(2) C46 0.067(3) 0.146(5) 0.084(3) -0.013(3) 0.007(2) -0.042(3) C51 0.086(10) 0.167(16) 0.080(6) 0.023(7) 0.006(6) 0.005(9) C52 0.106(10) 0.121(15) 0.155(14) -0.095(14) -0.017(12) 0.021(10) C53 0.039(5) 0.060(6) 0.30(2) 0.002(10) 0.009(9) -0.012(5) C51A 0.057(9) 0.128(11) 0.30(3) -0.105(15) -0.086(12) 0.030(7) C52A 0.16(2) 0.16(2) 0.097(8) -0.035(9) 0.004(9) 0.106(15) C53A 0.082(10) 0.082(9) 0.32(3) 0.107(14) 0.016(14) 0.030(7) C54 0.103(4) 0.081(3) 0.215(7) -0.001(4) 0.053(4) -0.057(3) C55 0.097(4) 0.117(4) 0.145(5) -0.048(4) 0.070(3) -0.056(3) C56 0.112(4) 0.258(8) 0.122(5) 0.022(5) -0.024(4) -0.138(5) Dy1 0.03692(8) 0.03904(8) 0.04550(8) -0.01415(6) 0.00419(5) -0.01504(6) N1 0.0502(15) 0.0550(15) 0.0528(16) -0.0095(13) 0.0079(12) -0.0229(13) N2 0.0550(15) 0.0454(14) 0.0458(14) -0.0131(12) 0.0041(12) -0.0206(12) O1 0.0385(11) 0.0614(13) 0.0591(13) -0.0271(12) 0.0009(9) -0.0151(10) O2 0.0397(11) 0.0589(13) 0.0555(13) -0.0276(11) 0.0026(9) -0.0112(10) O3 0.0551(13) 0.0464(12) 0.0686(15) -0.0082(11) 0.0016(11) -0.0239(11) O4 0.0476(12) 0.0431(11) 0.0610(14) -0.0110(10) -0.0069(10) -0.0168(10) O5 0.0395(11) 0.0445(12) 0.0698(15) -0.0051(11) 0.0025(10) -0.0141(9) O6 0.0389(11) 0.0474(12) 0.0626(14) -0.0062(11) 0.0061(9) -0.0167(9) 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 N1 C1 C2 122.9(4) C3 C2 C1 119.1(4) C2 C3 C4 120.6(4) C3 C4 C5 117.0(4) C3 C4 C8 124.9(4) C5 C4 C8 118.2(4) C4 C5 C6 119.7(3) N1 C5 C4 122.5(3) N1 C5 C6 117.8(3) C7 C6 C5 120.1(3) N2 C6 C5 118.1(3) N2 C6 C7 121.8(3) C6 C7 C9 118.6(4) C10 C7 C6 117.5(3) C10 C7 C9 123.9(4) C9 C8 C4 122.4(4) C8 C9 C7 121.1(4) C11 C10 C7 120.0(3) C10 C11 C12 118.9(4) N2 C12 C11 123.3(3) C31 C13 C14 105.2(6) C32 C13 C14 114.0(6) C32 C13 C31 106.2(11) C33 C13 C14 108.5(6) C33 C13 C31 107.9(8) C33 C13 C32 114.4(12) C31A C13 C14 112.3(7) C31A C13 C32A 104.8(11) C32A C13 C14 109.4(5) C33A C13 C14 109.6(6) C33A C13 C31A 113.6(12) C33A C13 C32A 106.9(11) C15 C14 C13 120.2(3) O1 C14 C13 115.9(3) O1 C14 C15 123.9(3) C16 C15 C14 124.8(3) C15 C16 C17 121.3(3) O2 C16 C15 124.2(3) O2 C16 C17 114.5(3) C34 C17 C16 108.2(3) C34 C17 C35 108.3(4) C35 C17 C16 113.8(3) C36 C17 C16 107.1(3) C36 C17 C34 109.2(4) C36 C17 C35 110.1(4) C41 C18 C19 104.9(5) C41 C18 C42 105.1(9) C42 C18 C19 111.5(7) C43 C18 C19 108.3(8) C43 C18 C41 107.0(12) C43 C18 C42 119.0(13) C41A C18 C19 110.5(8) C42A C18 C19 115.9(9) C42A C18 C41A 109.4(17) C42A C18 C43A 105.0(13) C43A C18 C19 111.3(11) C43A C18 C41A 104.0(18) C20 C19 C18 121.2(3) O3 C19 C18 115.1(3) O3 C19 C20 123.7(3) C19 C20 C21 125.1(3) C20 C21 C22 121.3(3) O4 C21 C20 123.8(3) O4 C21 C22 114.9(3) C21 C22 C44 107.6(3) C45 C22 C21 114.4(3) C45 C22 C44 109.2(4) C45 C22 C46 109.4(4) C46 C22 C21 107.4(3) C46 C22 C44 108.7(4) C51 C23 C24 113.6(8) C51 C23 C52 107.6(12) C51 C23 C53 108.6(11) C52 C23 C24 109.4(11) C52 C23 C53 105.3(12) C53 C23 C24 112.0(6) C51A C23 C24 105.7(7) C51A C23 C53A 109.1(13) C52A C23 C24 105.8(10) C52A C23 C51A 112.7(14) C52A C23 C53A 111.6(14) C53A C23 C24 111.9(8) C25 C24 C23 120.0(3) O5 C24 C23 115.9(3) O5 C24 C25 124.0(3) C26 C25 C24 124.0(3) C25 C26 C27 121.2(3) O6 C26 C25 124.2(3) O6 C26 C27 114.6(3) C54 C27 C26 113.6(3) C55 C27 C26 107.0(3) C55 C27 C54 106.9(4) C56 C27 C26 108.1(3) C56 C27 C54 111.3(4) C56 C27 C55 109.8(5) N2 Dy1 N1 62.49(8) O1 Dy1 N1 81.96(8) O1 Dy1 N2 140.83(8) O1 Dy1 O3 79.45(8) O1 Dy1 O4 141.37(7) O2 Dy1 N1 148.83(8) O2 Dy1 N2 145.63(8) O2 Dy1 O1 73.30(7) O2 Dy1 O3 84.71(8) O2 Dy1 O4 78.51(8) O2 Dy1 O5 121.08(8) O2 Dy1 O6 79.46(8) O3 Dy1 N1 72.17(8) O3 Dy1 N2 102.86(8) O3 Dy1 O4 72.06(8) O4 Dy1 N1 112.32(8) O4 Dy1 N2 72.37(8) O5 Dy1 N1 69.21(8) O5 Dy1 N2 75.81(8) O5 Dy1 O1 76.58(8) O5 Dy1 O3 136.72(8) O5 Dy1 O4 141.70(7) O6 Dy1 N1 129.99(8) O6 Dy1 N2 78.31(8) O6 Dy1 O1 118.23(8) O6 Dy1 O3 150.94(8) O6 Dy1 O4 80.95(8) O6 Dy1 O5 72.14(8) C1 N1 C5 117.9(3) C1 N1 Dy1 121.3(2) C5 N1 Dy1 119.7(2) C6 N2 Dy1 120.0(2) C12 N2 C6 118.3(3) C12 N2 Dy1 121.2(2) C14 O1 Dy1 136.20(18) C16 O2 Dy1 137.64(18) C19 O3 Dy1 132.4(2) C21 O4 Dy1 131.8(2) C24 O5 Dy1 137.67(19) C26 O6 Dy1 137.45(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.394(5) C1 N1 1.325(4) C2 C3 1.355(6) C3 C4 1.384(6) C4 C5 1.416(4) C4 C8 1.423(6) C5 C6 1.428(5) C5 N1 1.357(4) C6 C7 1.414(4) C6 N2 1.351(4) C7 C9 1.427(6) C7 C10 1.395(6) C8 C9 1.338(6) C10 C11 1.355(6) C11 C12 1.390(5) C12 N2 1.325(4) C13 C14 1.542(4) C13 C31 1.525(10) C13 C32 1.511(9) C13 C33 1.473(10) C13 C31A 1.491(11) C13 C32A 1.530(10) C13 C33A 1.468(11) C14 C15 1.395(4) C14 O1 1.262(3) C15 C16 1.387(4) C16 C17 1.544(4) C16 O2 1.263(3) C17 C34 1.519(5) C17 C35 1.520(5) C17 C36 1.502(5) C18 C19 1.538(5) C18 C41 1.497(9) C18 C42 1.531(10) C18 C43 1.472(12) C18 C41A 1.481(12) C18 C42A 1.467(11) C18 C43A 1.471(12) C19 C20 1.393(5) C19 O3 1.255(4) C20 C21 1.398(5) C21 C22 1.547(5) C21 O4 1.266(4) C22 C44 1.547(5) C22 C45 1.523(5) C22 C46 1.526(5) C23 C24 1.552(4) C23 C51 1.476(11) C23 C52 1.482(11) C23 C53 1.515(10) C23 C51A 1.484(11) C23 C52A 1.466(12) C23 C53A 1.494(11) C24 C25 1.396(4) C24 O5 1.245(4) C25 C26 1.382(4) C26 C27 1.544(4) C26 O6 1.265(4) C27 C54 1.525(6) C27 C55 1.509(6) C27 C56 1.486(6) Dy1 N1 2.601(3) Dy1 N2 2.599(2) Dy1 O1 2.324(2) Dy1 O2 2.277(2) Dy1 O3 2.325(2) Dy1 O4 2.355(2) Dy1 O5 2.317(2) Dy1 O6 2.308(2)