#------------------------------------------------------------------------------ #$Date: 2026-06-04 17:58:32 +0100 (Thu, 04 Jun 2026) $ #$Revision: 306210 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721079.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_7721079 loop_ _publ_author_name 'Kong, Yin-Cong' 'Yang, Zi' 'Liu, Yi' 'Wang, Chen' 'Sun, Rong' 'Sun, Zheng' 'Wang, Bing-Wu' 'Gao, Song' _publ_section_title ; A dysprosium alkylidene single molecule magnet. ; _journal_issue 19 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 7492 _journal_page_last 7496 _journal_paper_doi 10.1039/d6dt00641h _journal_volume 55 _journal_year 2026 _chemical_formula_moiety 'C37 H53 Dy N3 P Se Si' _chemical_formula_sum 'C37 H53 Dy N3 P Se Si' _chemical_formula_weight 840.34 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2025-02-22 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2026-01-22 deposited with the CCDC. 2026-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.681(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.6239(2) _cell_length_b 11.4942(2) _cell_length_c 31.4518(5) _cell_measurement_reflns_used 51658 _cell_measurement_temperature 293.00 _cell_measurement_theta_max 29.0450 _cell_measurement_theta_min 2.4030 _cell_volume 4548.49(13) _computing_cell_refinement 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293.00 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.941 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -97.00 20.00 0.50 2.03 -- -9.50 -57.00 90.00 234 2 \w -35.00 3.00 0.50 2.03 -- -9.50 37.00-180.00 76 3 \w -66.00 10.00 0.50 2.03 -- -9.50 -57.00 -30.00 152 4 \w 29.00 65.00 0.50 2.03 -- -9.50 37.00-180.00 72 5 \w -64.00 52.00 0.50 2.03 -- 9.60 -82.00 -60.00 232 6 \w -79.00 52.00 0.50 2.03 -- 9.60 -82.00 60.00 262 7 \w -33.00 94.00 0.50 2.03 -- 9.60 82.00 -90.00 254 8 \w -72.00 -46.00 0.50 2.03 -- 9.60 -82.00 -30.00 52 9 \w -72.00 52.00 0.50 2.03 -- 9.60 -82.00-150.00 248 10 \w -21.00 52.00 0.50 2.03 -- 9.60 -82.00 -30.00 146 11 \w -80.00 52.00 0.50 2.03 -- 9.60 -81.00 99.05 264 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_unetI/netI 0.0261 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.941 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_number 126995 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.941 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.869 _diffrn_reflns_theta_min 2.400 _exptl_absorpt_coefficient_mu 2.528 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.62034 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.227 _exptl_crystal_description block _exptl_crystal_F_000 1700 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.976 _refine_diff_density_min -0.930 _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 419 _refine_ls_number_reflns 12331 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0364 _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^)+(0.0211P)^2^+4.5544P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.0677 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10048 _reflns_number_total 12331 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00641h2.cif _cod_data_source_block x3 _cod_original_cell_volume 4548.48(13) _cod_database_code 7721079 _shelx_shelxl_version_number 2018/3 _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 0.768 _shelx_estimated_absorpt_t_min 0.751 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1) Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1) 3.a Ternary CH refined with riding coordinates: C15(H15), C12(H12) 3.b Secondary CH2 refined with riding coordinates: C19(H19A,H19B), C18(H18A,H18B) 3.c Aromatic/amide H refined with riding coordinates: C10(H10), C8(H8), C31(H31), C9(H9), C3(H3), C30(H30), C27(H27), C28(H28), C33(H33), C29(H29), C37(H37), C35(H35), C36(H36), C34(H34) 3.d Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C16(H16A,H16B,H16C), C1(H1A,H1B,H1C), C20(H20A,H20B, H20C), C5(H5A,H5B,H5C), C23(H23A,H23B,H23C), C17(H17A,H17B,H17C), C24(H24A, H24B,H24C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL x3_a.res in P2(1)/n x3.res created by SHELXL-2018/3 at 16:43:30 on 22-Feb-2025 REM Old TITL x3_a.res in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.125, Rweak 0.010, Alpha 0.039 REM 1.174 for 490 systematic absences, Orientation as input REM Formula found by SHELXT: C39 N7 Si P Se Dy CELL 0.71073 12.6239 11.4942 31.4518 90 94.681 90 ZERR 4 0.0002 0.0002 0.0005 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Dy N P Se Si UNIT 148 212 4 12 4 4 4 L.S. 4 0 0 PLAN 10 SIZE 0.11 0.12 0.11 TEMP 19.85 CONF FREE Dy1 C6 FREE Dy1 P1 list 4 MORE -1 ABIN BOND $H fmap 2 53 acta OMIT -5 0 7 OMIT -4 0 6 OMIT -2 1 2 OMIT -1 0 3 OMIT -1 1 5 OMIT 0 1 2 OMIT 0 1 4 OMIT 0 1 8 OMIT 1 1 5 OMIT 1 1 7 OMIT 2 0 2 OMIT 2 0 6 OMIT 2 1 4 OMIT 3 0 7 OMIT 3 1 5 OMIT 3 2 6 OMIT 4 0 10 OMIT 4 1 12 REM REM REM WGHT 0.021100 4.554400 FVAR 0.24978 0.37884 DY1 3 0.264105 0.830050 0.364082 11.00000 0.03951 0.03974 = 0.03920 0.00441 0.01212 0.00331 SE1 6 0.318171 0.736925 0.286277 11.00000 0.04545 0.09767 = 0.03857 -0.01389 0.00489 -0.01017 P1 5 0.464051 0.734508 0.331119 11.00000 0.03717 0.04720 = 0.03870 -0.00370 0.01076 -0.00172 SI1 7 0.516813 0.804781 0.428807 11.00000 0.06198 0.07063 = 0.04387 -0.00993 -0.00600 0.00189 N1 4 0.143393 0.729588 0.402047 11.00000 0.04392 0.03629 = 0.04283 0.00057 0.01237 0.00147 N2 4 0.214992 0.970545 0.414603 11.00000 0.05677 0.03615 = 0.05393 -0.00076 0.01608 0.00181 N3 4 0.267230 1.029061 0.331686 11.00000 0.06079 0.05271 = 0.06618 0.02223 0.02067 0.01267 C6 1 0.124666 0.626242 0.376986 11.00000 0.04420 0.03728 = 0.04346 -0.00032 0.01504 -0.00651 C11 1 0.178617 0.521977 0.388004 11.00000 0.06104 0.03668 = 0.04877 0.00231 0.01349 -0.00373 C22 1 0.438832 0.788391 0.378292 11.00000 0.04126 0.04535 = 0.03649 -0.00418 0.00596 0.00007 C26 1 0.563145 0.812163 0.301922 11.00000 0.03602 0.06084 = 0.04866 0.00880 0.00888 0.00183 C2 1 0.158990 0.958177 0.448418 11.00000 0.05839 0.04657 = 0.05116 -0.00794 0.01232 0.00681 C10 1 0.169797 0.430743 0.358879 11.00000 0.08250 0.03907 = 0.06629 -0.00562 0.01357 -0.00063 AFIX 43 H10 2 0.205414 0.361502 0.365614 11.00000 -1.20000 AFIX 0 C8 1 0.055396 0.539839 0.310806 11.00000 0.05694 0.07066 = 0.05568 -0.00831 0.00266 -0.01766 AFIX 43 H8 2 0.013278 0.544418 0.285185 11.00000 -1.20000 AFIX 0 C7 1 0.060769 0.635264 0.338146 11.00000 0.04253 0.05157 = 0.05579 -0.00015 0.00920 -0.00568 C31 1 0.593565 0.772545 0.263105 11.00000 0.05837 0.08308 = 0.05477 0.00242 0.02018 -0.00344 AFIX 43 H31 2 0.565526 0.703426 0.251677 11.00000 -1.20000 AFIX 0 C21 1 0.333542 1.045394 0.295229 11.00000 0.08776 0.06701 = 0.08042 0.03296 0.04020 0.01033 AFIX 137 H21A 2 0.404030 1.016917 0.302852 11.00000 -1.50000 H21B 2 0.336692 1.126621 0.288342 11.00000 -1.50000 H21C 2 0.302751 1.003196 0.270937 11.00000 -1.50000 AFIX 0 C9 1 0.110314 0.439609 0.320580 11.00000 0.08166 0.05473 = 0.06284 -0.01737 0.01471 -0.01337 AFIX 43 H9 2 0.107339 0.377910 0.301391 11.00000 -1.20000 AFIX 0 C32 1 0.512753 0.584217 0.329532 11.00000 0.07798 0.04978 = 0.05345 -0.00188 0.03295 0.01011 C3 1 0.105189 0.856947 0.458425 11.00000 0.06989 0.05106 = 0.04889 -0.00579 0.02781 0.00325 AFIX 43 H3 2 0.073467 0.859336 0.484079 11.00000 -1.20000 AFIX 0 C30 1 0.665553 0.835352 0.241209 11.00000 0.06438 0.11956 = 0.06094 0.01748 0.02724 0.00195 AFIX 43 H30 2 0.686178 0.807741 0.215343 11.00000 -1.20000 AFIX 0 C27 1 0.605377 0.915123 0.317990 11.00000 0.04795 0.06416 = 0.06474 0.00642 0.00954 -0.00420 AFIX 43 H27 2 0.585900 0.942973 0.343998 11.00000 -1.20000 AFIX 0 C19 1 0.316919 1.093393 0.368768 11.00000 0.07922 0.05308 = 0.08680 0.01104 0.02271 -0.01269 AFIX 23 H19A 2 0.326429 1.173945 0.360708 11.00000 -1.20000 H19B 2 0.386692 1.060835 0.376577 11.00000 -1.20000 AFIX 0 C4 1 0.091692 0.752950 0.435921 11.00000 0.05329 0.04500 = 0.05103 0.00381 0.01937 -0.00138 C15 1 0.242504 0.505181 0.430526 11.00000 0.09151 0.03908 = 0.04967 0.00387 0.00373 0.00989 AFIX 13 H15 2 0.241426 0.578963 0.446100 11.00000 -1.20000 AFIX 0 C16 1 0.358135 0.474414 0.425813 11.00000 0.09041 0.07875 = 0.07702 0.00536 -0.00515 0.01723 AFIX 137 H16A 2 0.395768 0.469357 0.453533 11.00000 -1.50000 H16B 2 0.389848 0.533545 0.409424 11.00000 -1.50000 H16C 2 0.361775 0.400918 0.411506 11.00000 -1.50000 AFIX 0 C1 1 0.147239 1.060404 0.478356 11.00000 0.10254 0.06133 = 0.07686 -0.02411 0.03105 -0.00001 AFIX 137 H1A 2 0.216260 1.090515 0.487561 11.00000 -1.50000 H1B 2 0.112345 1.034981 0.502718 11.00000 -1.50000 H1C 2 0.105695 1.120257 0.463691 11.00000 -1.50000 AFIX 0 C20 1 0.158902 1.070324 0.318625 11.00000 0.07354 0.07910 = 0.09165 0.03531 0.01672 0.02245 AFIX 137 H20A 2 0.131049 1.028051 0.293863 11.00000 -1.50000 H20B 2 0.160953 1.151807 0.312041 11.00000 -1.50000 H20C 2 0.114142 1.057992 0.341464 11.00000 -1.50000 AFIX 0 C12 1 -0.004277 0.743459 0.326986 11.00000 0.05229 0.07413 = 0.07423 0.00190 -0.00626 0.00564 AFIX 13 H12 2 0.025355 0.807174 0.344931 11.00000 -1.20000 AFIX 0 C18 1 0.252602 1.089257 0.406801 11.00000 0.09095 0.04407 = 0.07623 -0.00208 0.02296 -0.00670 AFIX 23 H18A 2 0.295686 1.116480 0.431773 11.00000 -1.20000 H18B 2 0.191990 1.140885 0.402124 11.00000 -1.20000 AFIX 0 C28 1 0.676768 0.977607 0.295661 11.00000 0.05878 0.07366 = 0.09560 0.02112 0.00542 -0.01758 AFIX 43 H28 2 0.704705 1.047152 0.306749 11.00000 -1.20000 AFIX 0 C33 1 0.619193 0.561983 0.339864 11.00000 0.09596 0.08292 = 0.06803 0.00112 0.02393 0.03938 AFIX 43 H33 2 0.666400 0.623360 0.345231 11.00000 -1.20000 AFIX 0 C29 1 0.706239 0.937559 0.257495 11.00000 0.05298 0.11216 = 0.08587 0.04208 0.01645 -0.00912 AFIX 43 H29 2 0.753979 0.979866 0.242611 11.00000 -1.20000 AFIX 0 C5 1 0.011413 0.668022 0.451416 11.00000 0.08456 0.06757 = 0.08348 0.00035 0.05007 -0.01458 AFIX 137 H5A 2 0.036226 0.639749 0.479179 11.00000 -1.50000 H5B 2 0.002747 0.603870 0.431897 11.00000 -1.50000 H5C 2 -0.055572 0.706666 0.452982 11.00000 -1.50000 AFIX 0 C37 1 0.443587 0.492184 0.321073 11.00000 0.13431 0.05875 = 0.09944 -0.01439 0.06207 -0.01563 AFIX 43 H37 2 0.371962 0.505780 0.313371 11.00000 -1.20000 AFIX 0 C23 1 0.553820 0.960990 0.440732 11.00000 0.12981 0.10518 = 0.08137 -0.02490 -0.01038 -0.04178 AFIX 137 H23A 2 0.596797 0.989791 0.419220 11.00000 -1.50000 H23B 2 0.593082 0.965667 0.468134 11.00000 -1.50000 H23C 2 0.490426 1.007057 0.440914 11.00000 -1.50000 AFIX 0 C17 1 0.190611 0.412013 0.457434 11.00000 0.14300 0.06497 = 0.06759 0.02107 0.02166 -0.00002 AFIX 137 H17A 2 0.198029 0.336942 0.444632 11.00000 -1.50000 H17B 2 0.116552 0.429553 0.458594 11.00000 -1.50000 H17C 2 0.224978 0.411601 0.485811 11.00000 -1.50000 AFIX 0 C35 1 0.587582 0.358335 0.334674 11.00000 0.33561 0.08030 = 0.12148 0.02653 0.12934 0.08483 AFIX 43 H35 2 0.612534 0.282236 0.336608 11.00000 -1.20000 AFIX 0 C36 1 0.482673 0.378770 0.324246 11.00000 0.27102 0.05218 = 0.14976 -0.01515 0.12900 -0.01941 AFIX 43 H36 2 0.436408 0.316426 0.319166 11.00000 -1.20000 AFIX 0 C24 1 0.434927 0.766643 0.474200 11.00000 0.17993 0.13049 = 0.04299 -0.01138 0.01275 -0.05763 AFIX 137 H24A 2 0.369671 0.809900 0.471518 11.00000 -1.50000 H24B 2 0.473893 0.785704 0.500777 11.00000 -1.50000 H24C 2 0.419434 0.684864 0.473465 11.00000 -1.50000 AFIX 0 C14 1 -0.119556 0.724941 0.337364 11.00000 0.07158 0.16962 = 0.13966 0.04110 0.03240 0.04526 AFIX 137 H14A 2 -0.158558 0.796127 0.332706 11.00000 -1.50000 H14B 2 -0.120824 0.701871 0.366653 11.00000 -1.50000 H14C 2 -0.151521 0.665220 0.319234 11.00000 -1.50000 AFIX 0 C13 1 -0.002623 0.780826 0.280779 11.00000 0.07786 0.12056 = 0.10807 0.04514 0.00082 0.02089 AFIX 137 H13A 2 -0.039195 0.724050 0.262637 11.00000 -1.50000 H13B 2 0.069647 0.787238 0.273642 11.00000 -1.50000 H13C 2 -0.037275 0.854834 0.276820 11.00000 -1.50000 AFIX 0 C34 1 0.655945 0.447895 0.342259 11.00000 0.18464 0.12264 = 0.08543 0.01996 0.04638 0.09667 AFIX 43 H34 2 0.727758 0.433180 0.349098 11.00000 -1.20000 AFIX 0 PART 1 C25 1 0.624184 0.684462 0.440701 21.00000 0.16489 0.21161 = 0.10162 -0.01290 -0.04898 0.12489 AFIX 137 H25A 2 0.591012 0.609282 0.438784 21.00000 -1.50000 H25B 2 0.657879 0.695337 0.468900 21.00000 -1.50000 H25C 2 0.676490 0.689569 0.420270 21.00000 -1.50000 AFIX 0 PART 2 C25A 1 0.650460 0.738882 0.431768 -21.00000 0.11671 0.13134 = 0.09462 -0.04830 -0.06250 0.06002 AFIX 137 H25D 2 0.644249 0.656799 0.426503 -21.00000 -1.50000 H25E 2 0.685409 0.751700 0.459638 -21.00000 -1.50000 H25F 2 0.691271 0.773853 0.410704 -21.00000 -1.50000 AFIX 0 HKLF 4 REM x3_a.res in P2(1)/n REM wR2 = 0.0677, GooF = S = 1.042, Restrained GooF = 1.042 for all data REM R1 = 0.0364 for 10048 Fo > 4sig(Fo) and 0.0496 for all 12331 data REM 419 parameters refined using 0 restraints END WGHT 0.0211 4.5546 REM Highest difference peak 0.976, deepest hole -0.930, 1-sigma level 0.066 Q1 1 0.3153 0.6725 0.2979 11.00000 0.05 0.98 Q2 1 0.2133 0.9258 0.4404 11.00000 0.05 0.57 Q3 1 0.2624 0.7655 0.3644 11.00000 0.05 0.51 Q4 1 0.3200 0.7478 0.2764 11.00000 0.05 0.49 Q5 1 0.2795 0.8676 0.3415 11.00000 0.05 0.42 Q6 1 0.2197 0.8403 0.3782 11.00000 0.05 0.36 Q7 1 0.2158 0.8796 0.3597 11.00000 0.05 0.36 Q8 1 0.3251 0.8389 0.3650 11.00000 0.05 0.36 Q9 1 0.2225 0.4812 0.3610 11.00000 0.05 0.34 Q10 1 0.2849 0.7829 0.2985 11.00000 0.05 0.34 ; _shelx_res_checksum 92910 _shelx_fab_file ; -17 0 -7 0.2009 -0.1325 -17 0 -5 -2.3050 0.0972 -17 0 -3 -1.0871 0.3839 -17 0 -1 2.8276 -0.2209 -17 0 1 0.2239 -0.4651 -17 0 3 0.3900 0.3380 -17 0 5 0.1243 0.4199 -17 0 7 -0.8792 -0.4652 -17 0 9 -0.2665 -0.3647 -17 0 11 -0.0723 0.6611 -17 0 13 0.7943 0.3774 -17 0 15 1.3690 -0.8387 -17 1 -8 0.9164 0.2093 -17 1 -7 0.8384 0.1876 -17 1 -6 0.3913 0.1333 -17 1 -5 0.8573 0.0672 -17 1 -4 -0.9231 -0.0400 -17 1 -3 -2.3621 -0.1872 -17 1 -2 -1.7442 0.0559 -17 1 -1 -0.9579 -0.2866 -17 1 0 1.6426 0.0673 -17 1 1 0.7487 0.1507 -17 1 2 2.2722 -0.0837 -17 1 3 -0.3842 0.2141 -17 1 4 -0.0856 -0.0238 -17 1 5 0.9175 -0.1782 -17 1 6 0.3142 0.0373 -17 1 7 1.0311 -0.2521 -17 1 8 0.2001 -0.0131 -17 1 9 -1.7999 0.1570 -17 1 10 1.2773 -0.0256 -17 1 11 -1.8583 0.2693 -17 1 12 0.1058 -0.0015 -17 1 13 0.0897 -0.0791 -17 1 14 -1.1917 0.2453 -17 1 15 -0.7841 -0.0400 -17 2 -7 1.3372 -0.0266 -17 2 -6 -1.0995 -0.2323 -17 2 -5 2.2201 0.2226 -17 2 -4 1.0784 -0.1740 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0.2198 -0.0002 12 4 26 -0.0634 0.1120 12 4 27 1.6995 0.0712 12 5 12 -0.7662 -0.0483 12 5 13 -1.8635 0.1611 12 5 14 -0.2396 0.0454 12 5 15 0.4511 0.0676 12 5 16 -0.4209 -0.1881 12 5 17 0.4387 -0.0612 12 5 18 -1.6737 -0.0103 12 5 19 -0.9843 0.0426 12 5 20 -0.0036 0.0577 12 5 21 -0.7292 0.0112 12 5 22 -0.3609 0.0171 12 5 23 -0.0334 0.0836 12 5 24 -0.3981 -0.0004 12 5 25 -1.5301 0.1207 12 5 26 1.0542 -0.2524 12 6 12 -1.5324 0.0893 12 6 13 -0.1439 -0.1548 12 6 14 -1.7615 -0.0973 12 6 15 -0.4373 -0.1303 12 6 16 -1.2768 0.0408 12 6 17 1.7606 0.0495 12 6 18 -1.3003 -0.0730 12 6 19 0.4838 -0.1071 12 6 20 0.3433 0.1319 12 6 21 0.4935 0.0755 12 6 22 0.1857 0.0819 12 6 23 2.6589 -0.0571 12 6 24 -3.1589 -0.1314 12 6 25 0.6591 -0.1433 12 7 12 0.1281 -0.0480 12 7 13 -2.2115 0.0247 12 7 14 -1.2123 -0.0208 12 7 15 -2.5379 -0.0661 12 7 16 -0.0461 -0.2133 12 7 17 1.9336 -0.1611 12 7 18 -0.6708 0.0963 12 7 19 3.0948 0.0517 12 7 20 -0.9358 0.0014 12 7 21 -1.3008 0.0082 12 7 22 0.5650 -0.0206 12 7 23 -0.9182 0.1774 12 8 12 -1.1740 0.0873 12 8 13 4.2313 -0.2098 12 8 14 -1.0726 -0.2640 12 8 15 -1.8663 -0.1342 12 8 16 0.2940 -0.0360 12 8 17 -4.0687 -0.2338 12 8 18 2.0731 -0.0298 12 8 19 0.0821 -0.0681 12 8 20 1.4077 0.0640 12 8 21 0.8053 0.1312 12 9 12 -2.2268 0.1302 12 9 13 1.1574 0.0338 12 9 14 -3.5615 -0.0119 12 9 15 1.8768 0.0216 12 9 16 -2.1401 -0.3550 12 9 17 -0.5329 -0.3344 12 9 18 -1.6801 0.0319 12 10 12 2.3049 -0.2046 12 10 13 0.7369 -0.3051 12 10 14 -2.4530 -0.0989 13 0 13 -0.3819 -1.0588 13 0 15 -1.2062 -0.0403 13 0 17 1.3016 0.1861 13 0 19 -1.2546 0.1067 13 0 21 -4.7985 0.1388 13 0 23 -2.3767 0.0708 13 0 25 0.1415 -0.0557 13 0 27 1.0375 -0.1447 13 1 13 0.1073 -0.2365 13 1 14 0.0973 -0.0401 13 1 15 1.5922 -0.1949 13 1 16 -1.6130 -0.0964 13 1 17 1.9120 -0.1690 13 1 18 -1.8410 -0.1282 13 1 19 1.8563 0.1044 13 1 20 1.1697 -0.1156 13 1 21 -1.4335 -0.0213 13 1 22 1.3815 -0.0092 13 1 23 -1.9944 -0.2422 13 1 24 1.0895 0.0778 13 1 25 0.3988 -0.3586 13 1 26 -0.1537 -0.0553 13 1 27 0.3809 -0.2892 13 2 13 -3.2437 0.0397 13 2 14 0.1845 -0.2405 13 2 15 -2.9566 0.0204 13 2 16 0.8387 -0.1228 13 2 17 -0.2586 0.0466 13 2 18 -0.7989 -0.0717 13 2 19 0.8770 0.1662 13 2 20 0.5141 -0.0280 13 2 21 0.8306 0.3035 13 2 22 0.4843 0.2084 13 2 23 -1.4514 0.2094 13 2 24 -1.8647 0.2129 13 2 25 -0.6755 -0.1837 13 2 26 -1.1486 0.0650 13 3 13 2.3807 -0.0078 13 3 14 -0.1600 -0.0159 13 3 15 2.0906 0.1639 13 3 16 0.9192 0.2277 13 3 17 0.4542 0.0773 13 3 18 0.5692 -0.0249 13 3 19 -3.0738 -0.1334 13 3 20 -0.6802 -0.1533 13 3 21 -2.4041 -0.1703 13 3 22 -0.2762 0.0192 13 3 23 1.2814 0.0690 13 3 24 0.4377 0.2094 13 3 25 0.5593 0.1601 13 3 26 -0.6169 0.3389 13 4 13 -3.9002 0.0920 13 4 14 -0.9540 0.1173 13 4 15 -3.1793 -0.0748 13 4 16 -1.1563 0.0412 13 4 17 0.5500 -0.0930 13 4 18 0.3217 0.1046 13 4 19 0.1511 0.0026 13 4 20 2.0963 -0.0770 13 4 21 -1.2980 -0.1791 13 4 22 -0.0753 -0.0744 13 4 23 -0.2155 -0.0272 13 4 24 -1.2459 -0.0250 13 4 25 0.6878 -0.0775 13 5 13 1.5133 0.0185 13 5 14 -0.0666 -0.2008 13 5 15 -0.6306 0.0703 13 5 16 -1.5203 0.1104 13 5 17 -1.0798 -0.0587 13 5 18 -0.8422 -0.0281 13 5 19 -2.2026 -0.2200 13 5 20 -0.0929 -0.0906 13 5 21 -2.3144 0.0649 13 5 22 -0.2007 -0.1118 13 5 23 -0.6381 0.0552 13 6 13 -0.0723 0.2257 13 6 14 0.8488 0.2377 13 6 15 0.3175 -0.0961 13 6 16 -0.8784 -0.0972 13 6 17 0.5200 -0.1833 13 6 18 -0.9261 0.0742 13 6 19 -0.5118 -0.1219 13 6 20 0.1967 -0.1092 13 6 21 -1.7817 -0.1335 13 6 22 -1.0133 -0.1607 13 7 13 1.9785 0.0762 13 7 14 -1.3576 -0.2339 13 7 15 -0.2176 0.1376 13 7 16 -3.0771 0.1496 13 7 17 0.0116 -0.1675 13 7 18 -3.0569 -0.1654 13 7 19 1.1359 -0.2178 13 7 20 0.7174 -0.0922 13 8 13 1.0162 0.3194 13 8 14 0.2692 -0.1096 13 8 15 0.3158 -0.0732 13 8 16 2.0505 -0.1396 13 8 17 -1.5796 -0.2464 13 9 13 1.5928 0.0647 13 9 14 -0.8383 -0.3089 14 0 14 1.1731 0.0026 14 0 16 0.5881 -0.5407 14 0 18 0.1645 -0.5344 14 0 20 1.1696 -0.3897 14 0 22 -1.2330 0.0832 14 0 24 -2.1042 0.4624 14 1 14 -1.5997 0.2062 14 1 15 -1.5985 0.0397 14 1 16 0.2939 0.2182 14 1 17 0.9344 0.0753 14 1 18 2.1169 -0.0342 14 1 19 -1.4163 0.0884 14 1 20 3.2229 0.0453 14 1 21 -2.1742 0.0436 14 1 22 1.8619 0.3714 14 1 23 -1.3160 -0.1090 14 2 14 1.0137 -0.1055 14 2 15 -1.6690 0.1887 14 2 16 -3.9190 -0.0116 14 2 17 -0.0619 0.1043 14 2 18 -4.0057 -0.1357 14 2 19 1.0776 0.0713 14 2 20 -0.9496 -0.2388 14 2 21 0.8435 -0.1789 14 2 22 1.1794 0.0112 14 2 23 1.8325 -0.0451 14 3 14 0.6220 -0.1038 14 3 15 -1.0346 -0.2356 14 3 16 2.3417 -0.0943 14 3 17 0.0853 -0.1079 14 3 18 1.8492 0.2267 14 3 19 0.3636 0.2594 14 3 20 0.6275 0.1491 14 3 21 0.0102 -0.0489 14 3 22 -2.0411 -0.1769 14 4 14 1.1684 0.0646 14 4 15 0.2319 0.1078 14 4 16 -2.7742 0.2347 14 4 17 -0.2708 0.0102 14 4 18 -3.3038 -0.0451 14 4 19 -1.6886 0.0685 14 4 20 -1.4904 0.1136 14 4 21 -0.0121 0.2190 14 5 14 1.9666 0.1187 14 5 15 -0.2814 -0.1983 14 5 16 3.7573 0.0612 14 5 17 0.7314 -0.0601 14 5 18 2.5475 0.3005 14 5 19 -0.1408 0.1253 14 5 20 1.7358 -0.0730 14 6 14 -0.7922 0.1122 14 6 15 0.5951 0.0369 14 6 16 -0.3624 0.3105 14 6 17 0.8102 0.0008 14 6 18 0.6466 -0.0926 14 7 14 0.7903 0.1612 14 7 15 0.2677 -0.1978 14 7 16 0.7237 0.1793 15 0 15 -0.8737 0.5768 15 0 17 1.5450 0.2288 15 0 19 1.0630 -0.1124 15 1 15 -1.4266 0.0454 15 1 16 -1.6568 0.0103 15 1 17 -2.5034 0.1123 15 1 18 -0.8976 0.0590 15 1 19 -0.7858 -0.0305 15 1 20 0.5631 0.0045 15 2 15 2.4850 -0.0388 15 2 16 1.0522 -0.1502 15 2 17 2.0091 -0.0350 15 2 18 -0.9173 -0.0008 15 2 19 -2.5075 0.1240 15 3 15 -2.9966 0.1146 15 3 16 -3.7803 -0.0270 15 3 17 0.8540 -0.2346 15 3 18 -1.6676 -0.4791 15 4 15 1.4712 -0.3000 15 4 16 -1.0042 -0.1500 15 4 17 2.9377 0.0904 15 5 15 -3.2979 -0.0624 0 0 0 0.0 0.0 ; _shelx_fab_checksum 72934 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.26411(2) 0.83005(2) 0.36408(2) 0.03899(4) Uani 1 1 d . . . . . Se1 Se 0.31817(2) 0.73693(3) 0.28628(2) 0.06048(9) Uani 1 1 d . . . . . P1 P 0.46405(5) 0.73451(6) 0.33112(2) 0.04060(15) Uani 1 1 d . . . . . Si1 Si 0.51681(7) 0.80478(9) 0.42881(3) 0.0594(2) Uani 1 1 d . . . . . N1 N 0.14339(17) 0.72959(18) 0.40205(7) 0.0405(5) Uani 1 1 d . . . . . N2 N 0.21499(19) 0.97055(19) 0.41460(7) 0.0483(5) Uani 1 1 d . . . . . N3 N 0.2672(2) 1.0291(2) 0.33169(8) 0.0590(7) Uani 1 1 d . . . . . C6 C 0.1247(2) 0.6262(2) 0.37699(8) 0.0410(6) Uani 1 1 d . . . . . C11 C 0.1786(2) 0.5220(2) 0.38800(9) 0.0483(6) Uani 1 1 d . . . . . C22 C 0.4388(2) 0.7884(2) 0.37829(8) 0.0409(6) Uani 1 1 d . . . . . C26 C 0.5631(2) 0.8122(3) 0.30192(9) 0.0482(7) Uani 1 1 d . . . . . C2 C 0.1590(2) 0.9582(2) 0.44842(9) 0.0516(7) Uani 1 1 d . . . . . C10 C 0.1698(3) 0.4307(3) 0.35888(10) 0.0622(8) Uani 1 1 d . . . . . H10 H 0.205414 0.361502 0.365614 0.075 Uiso 1 1 calc R U . . . C8 C 0.0554(3) 0.5398(3) 0.31081(10) 0.0612(8) Uani 1 1 d . . . . . H8 H 0.013278 0.544418 0.285185 0.073 Uiso 1 1 calc R U . . . C7 C 0.0608(2) 0.6353(3) 0.33815(9) 0.0497(7) Uani 1 1 d . . . . . C31 C 0.5936(3) 0.7725(3) 0.26310(10) 0.0646(8) Uani 1 1 d . . . . . H31 H 0.565526 0.703426 0.251677 0.077 Uiso 1 1 calc R U . . . C21 C 0.3335(3) 1.0454(3) 0.29523(12) 0.0766(11) Uani 1 1 d . . . . . H21A H 0.404030 1.016917 0.302852 0.115 Uiso 1 1 calc R U . . . H21B H 0.336692 1.126621 0.288342 0.115 Uiso 1 1 calc R U . . . H21C H 0.302751 1.003196 0.270937 0.115 Uiso 1 1 calc R U . . . C9 C 0.1103(3) 0.4396(3) 0.32058(11) 0.0659(9) Uani 1 1 d . . . . . H9 H 0.107339 0.377910 0.301391 0.079 Uiso 1 1 calc R U . . . C32 C 0.5128(3) 0.5842(3) 0.32953(10) 0.0589(8) Uani 1 1 d . . . . . C3 C 0.1052(3) 0.8569(3) 0.45842(9) 0.0554(7) Uani 1 1 d . . . . . H3 H 0.073467 0.859336 0.484079 0.066 Uiso 1 1 calc R U . . . C30 C 0.6656(3) 0.8354(4) 0.24121(12) 0.0804(11) Uani 1 1 d . . . . . H30 H 0.686178 0.807741 0.215343 0.096 Uiso 1 1 calc R U . . . C27 C 0.6054(2) 0.9151(3) 0.31799(10) 0.0587(8) Uani 1 1 d . . . . . H27 H 0.585900 0.942973 0.343998 0.070 Uiso 1 1 calc R U . . . C19 C 0.3169(3) 1.0934(3) 0.36877(12) 0.0722(10) Uani 1 1 d . . . . . H19A H 0.326429 1.173945 0.360708 0.087 Uiso 1 1 calc R U . . . H19B H 0.386692 1.060835 0.376577 0.087 Uiso 1 1 calc R U . . . C4 C 0.0917(2) 0.7530(2) 0.43592(9) 0.0489(6) Uani 1 1 d . . . . . C15 C 0.2425(3) 0.5052(3) 0.43053(9) 0.0602(8) Uani 1 1 d . . . . . H15 H 0.241426 0.578963 0.446100 0.072 Uiso 1 1 calc R U . . . C16 C 0.3581(3) 0.4744(4) 0.42581(13) 0.0827(11) Uani 1 1 d . . . . . H16A H 0.395768 0.469357 0.453533 0.124 Uiso 1 1 calc R U . . . H16B H 0.389848 0.533545 0.409424 0.124 Uiso 1 1 calc R U . . . H16C H 0.361775 0.400918 0.411506 0.124 Uiso 1 1 calc R U . . . C1 C 0.1472(3) 1.0604(3) 0.47836(12) 0.0789(11) Uani 1 1 d . . . . . H1A H 0.216260 1.090515 0.487561 0.118 Uiso 1 1 calc R U . . . H1B H 0.112345 1.034981 0.502718 0.118 Uiso 1 1 calc R U . . . H1C H 0.105695 1.120257 0.463691 0.118 Uiso 1 1 calc R U . . . C20 C 0.1589(3) 1.0703(3) 0.31863(13) 0.0809(11) Uani 1 1 d . . . . . H20A H 0.131049 1.028051 0.293863 0.121 Uiso 1 1 calc R U . . . H20B H 0.160953 1.151807 0.312041 0.121 Uiso 1 1 calc R U . . . H20C H 0.114142 1.057992 0.341464 0.121 Uiso 1 1 calc R U . . . C12 C -0.0043(3) 0.7435(3) 0.32699(11) 0.0675(9) Uani 1 1 d . . . . . H12 H 0.025355 0.807174 0.344931 0.081 Uiso 1 1 calc R U . . . C18 C 0.2526(3) 1.0893(3) 0.40680(12) 0.0695(9) Uani 1 1 d . . . . . H18A H 0.295686 1.116480 0.431773 0.083 Uiso 1 1 calc R U . . . H18B H 0.191990 1.140885 0.402124 0.083 Uiso 1 1 calc R U . . . C28 C 0.6768(3) 0.9776(3) 0.29566(13) 0.0761(10) Uani 1 1 d . . . . . H28 H 0.704705 1.047152 0.306749 0.091 Uiso 1 1 calc R U . . . C33 C 0.6192(3) 0.5620(4) 0.33986(11) 0.0814(11) Uani 1 1 d . . . . . H33 H 0.666400 0.623360 0.345231 0.098 Uiso 1 1 calc R U . . . C29 C 0.7062(3) 0.9376(4) 0.25750(13) 0.0831(12) Uani 1 1 d . . . . . H29 H 0.753979 0.979866 0.242611 0.100 Uiso 1 1 calc R U . . . C5 C 0.0114(3) 0.6680(3) 0.45142(12) 0.0762(11) Uani 1 1 d . . . . . H5A H 0.036226 0.639749 0.479179 0.114 Uiso 1 1 calc R U . . . H5B H 0.002747 0.603870 0.431897 0.114 Uiso 1 1 calc R U . . . H5C H -0.055572 0.706666 0.452982 0.114 Uiso 1 1 calc R U . . . C37 C 0.4436(4) 0.4922(3) 0.32107(14) 0.0946(14) Uani 1 1 d . . . . . H37 H 0.371962 0.505780 0.313371 0.114 Uiso 1 1 calc R U . . . C23 C 0.5538(4) 0.9610(4) 0.44073(14) 0.1065(16) Uani 1 1 d . . . . . H23A H 0.596797 0.989791 0.419220 0.160 Uiso 1 1 calc R U . . . H23B H 0.593082 0.965667 0.468134 0.160 Uiso 1 1 calc R U . . . H23C H 0.490426 1.007057 0.440914 0.160 Uiso 1 1 calc R U . . . C17 C 0.1906(4) 0.4120(3) 0.45743(12) 0.0911(13) Uani 1 1 d . . . . . H17A H 0.198029 0.336942 0.444632 0.137 Uiso 1 1 calc R U . . . H17B H 0.116552 0.429553 0.458594 0.137 Uiso 1 1 calc R U . . . H17C H 0.224978 0.411601 0.485811 0.137 Uiso 1 1 calc R U . . . C35 C 0.5876(9) 0.3583(6) 0.3347(2) 0.173(5) Uani 1 1 d . . . . . H35 H 0.612534 0.282236 0.336608 0.208 Uiso 1 1 calc R U . . . C36 C 0.4827(7) 0.3788(4) 0.3242(2) 0.152(3) Uani 1 1 d . . . . . H36 H 0.436408 0.316426 0.319166 0.182 Uiso 1 1 calc R U . . . C24 C 0.4349(5) 0.7666(5) 0.47420(12) 0.1176(19) Uani 1 1 d . . . . . H24A H 0.369671 0.809900 0.471518 0.176 Uiso 1 1 calc R U . . . H24B H 0.473893 0.785704 0.500777 0.176 Uiso 1 1 calc R U . . . H24C H 0.419434 0.684864 0.473465 0.176 Uiso 1 1 calc R U . . . C14 C -0.1196(3) 0.7249(5) 0.33736(18) 0.126(2) Uani 1 1 d . . . . . H14A H -0.158558 0.796127 0.332706 0.188 Uiso 1 1 calc R U . . . H14B H -0.120824 0.701871 0.366653 0.188 Uiso 1 1 calc R U . . . H14C H -0.151521 0.665220 0.319234 0.188 Uiso 1 1 calc R U . . . C13 C -0.0026(3) 0.7808(4) 0.28078(15) 0.1025(15) Uani 1 1 d . . . . . H13A H -0.039195 0.724050 0.262637 0.154 Uiso 1 1 calc R U . . . H13B H 0.069647 0.787238 0.273642 0.154 Uiso 1 1 calc R U . . . H13C H -0.037275 0.854834 0.276820 0.154 Uiso 1 1 calc R U . . . C34 C 0.6559(6) 0.4479(6) 0.34226(16) 0.129(2) Uani 1 1 d . . . . . H34 H 0.727758 0.433180 0.349098 0.155 Uiso 1 1 calc R U . . . C25 C 0.624(7) 0.684(9) 0.4407(15) 0.16(2) Uani 0.38(9) 1 d . . P A 1 H25A H 0.591012 0.609282 0.438784 0.244 Uiso 0.38(9) 1 calc R U P A 1 H25B H 0.657879 0.695337 0.468900 0.244 Uiso 0.38(9) 1 calc R U P A 1 H25C H 0.676490 0.689569 0.420270 0.244 Uiso 0.38(9) 1 calc R U P A 1 C25A C 0.650(2) 0.739(3) 0.4318(10) 0.118(8) Uani 0.62(9) 1 d . . P A 2 H25D H 0.644249 0.656799 0.426503 0.177 Uiso 0.62(9) 1 calc R U P A 2 H25E H 0.685409 0.751700 0.459638 0.177 Uiso 0.62(9) 1 calc R U P A 2 H25F H 0.691271 0.773853 0.410704 0.177 Uiso 0.62(9) 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.03951(7) 0.03974(7) 0.03920(6) 0.00441(5) 0.01212(5) 0.00331(5) Se1 0.04545(16) 0.0977(3) 0.03857(14) -0.01389(15) 0.00489(12) -0.01017(16) P1 0.0372(3) 0.0472(4) 0.0387(3) -0.0037(3) 0.0108(3) -0.0017(3) Si1 0.0620(5) 0.0706(6) 0.0439(4) -0.0099(4) -0.0060(4) 0.0019(4) N1 0.0439(12) 0.0363(11) 0.0428(11) 0.0006(9) 0.0124(9) 0.0015(9) N2 0.0568(14) 0.0361(12) 0.0539(13) -0.0008(10) 0.0161(11) 0.0018(10) N3 0.0608(15) 0.0527(15) 0.0662(16) 0.0222(13) 0.0207(13) 0.0127(12) C6 0.0442(14) 0.0373(13) 0.0435(14) -0.0003(11) 0.0150(11) -0.0065(11) C11 0.0610(17) 0.0367(14) 0.0488(15) 0.0023(12) 0.0135(13) -0.0037(12) C22 0.0413(13) 0.0453(14) 0.0365(13) -0.0042(11) 0.0060(10) 0.0001(11) C26 0.0360(13) 0.0608(18) 0.0487(15) 0.0088(13) 0.0089(11) 0.0018(12) C2 0.0584(17) 0.0466(16) 0.0512(16) -0.0079(13) 0.0123(13) 0.0068(13) C10 0.083(2) 0.0391(16) 0.066(2) -0.0056(14) 0.0136(17) -0.0006(15) C8 0.0569(18) 0.071(2) 0.0557(18) -0.0083(16) 0.0027(14) -0.0177(16) C7 0.0425(14) 0.0516(16) 0.0558(16) -0.0002(13) 0.0092(12) -0.0057(12) C31 0.0584(18) 0.083(2) 0.0548(18) 0.0024(17) 0.0202(15) -0.0034(17) C21 0.088(2) 0.067(2) 0.080(2) 0.0330(19) 0.040(2) 0.0103(19) C9 0.082(2) 0.0547(19) 0.063(2) -0.0174(16) 0.0147(17) -0.0134(17) C32 0.078(2) 0.0498(17) 0.0534(17) -0.0019(14) 0.0330(16) 0.0101(16) C3 0.0699(19) 0.0511(17) 0.0489(16) -0.0058(13) 0.0278(14) 0.0032(14) C30 0.064(2) 0.120(3) 0.061(2) 0.017(2) 0.0272(17) 0.002(2) C27 0.0480(16) 0.064(2) 0.0647(19) 0.0064(16) 0.0095(14) -0.0042(15) C19 0.079(2) 0.0531(19) 0.087(3) 0.0110(18) 0.0227(19) -0.0127(17) C4 0.0533(16) 0.0450(15) 0.0510(15) 0.0038(12) 0.0194(13) -0.0014(13) C15 0.092(2) 0.0391(15) 0.0497(16) 0.0039(13) 0.0037(16) 0.0099(16) C16 0.090(3) 0.079(3) 0.077(2) 0.005(2) -0.005(2) 0.017(2) C1 0.103(3) 0.061(2) 0.077(2) -0.0241(18) 0.031(2) 0.000(2) C20 0.074(2) 0.079(2) 0.092(3) 0.035(2) 0.017(2) 0.022(2) C12 0.0523(18) 0.074(2) 0.074(2) 0.0019(18) -0.0063(16) 0.0056(16) C18 0.091(2) 0.0441(17) 0.076(2) -0.0021(16) 0.0230(19) -0.0067(17) C28 0.059(2) 0.074(2) 0.096(3) 0.021(2) 0.0054(19) -0.0176(18) C33 0.096(3) 0.083(3) 0.068(2) 0.0011(19) 0.024(2) 0.039(2) C29 0.053(2) 0.112(3) 0.086(3) 0.042(3) 0.0164(19) -0.009(2) C5 0.085(2) 0.068(2) 0.083(2) 0.0003(19) 0.050(2) -0.0146(19) C37 0.134(4) 0.059(2) 0.099(3) -0.014(2) 0.062(3) -0.016(2) C23 0.130(4) 0.105(3) 0.081(3) -0.025(3) -0.010(3) -0.042(3) C17 0.143(4) 0.065(2) 0.068(2) 0.0211(19) 0.022(2) 0.000(2) C35 0.336(13) 0.080(4) 0.121(5) 0.027(4) 0.129(7) 0.085(6) C36 0.271(9) 0.052(3) 0.150(5) -0.015(3) 0.129(6) -0.019(4) C24 0.180(5) 0.130(4) 0.043(2) -0.011(2) 0.013(3) -0.058(4) C14 0.072(3) 0.170(5) 0.140(4) 0.041(4) 0.032(3) 0.045(3) C13 0.078(3) 0.121(4) 0.108(3) 0.045(3) 0.001(2) 0.021(3) C34 0.185(6) 0.123(4) 0.085(3) 0.020(3) 0.046(4) 0.097(5) C25 0.16(4) 0.21(5) 0.102(16) -0.01(3) -0.05(2) 0.12(4) C25A 0.117(9) 0.131(14) 0.095(11) -0.048(9) -0.062(9) 0.060(10) 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Dy1 Se1 118.42(5) . . ? N1 Dy1 N2 77.08(7) . . ? N1 Dy1 N3 134.16(8) . . ? N2 Dy1 Se1 159.26(5) . . ? N2 Dy1 N3 70.49(8) . . ? N3 Dy1 Se1 88.89(6) . . ? C22 Dy1 Se1 77.83(6) . . ? C22 Dy1 N1 117.60(8) . . ? C22 Dy1 N2 108.29(9) . . ? C22 Dy1 N3 103.05(9) . . ? P1 Se1 Dy1 72.530(18) . . ? C22 P1 Se1 110.61(9) . . ? C22 P1 C26 116.86(14) . . ? C22 P1 C32 117.64(13) . . ? C26 P1 Se1 103.79(9) . . ? C32 P1 Se1 104.84(12) . . ? C32 P1 C26 101.53(13) . . ? C22 Si1 C23 112.46(17) . . ? C22 Si1 C24 110.42(18) . . ? C22 Si1 C25 114.5(15) . . ? C22 Si1 C25A 115.6(7) . . ? C23 Si1 C25 119(3) . . ? C24 Si1 C23 102.3(2) . . ? C24 Si1 C25 96(3) . . ? C25A Si1 C23 99.8(10) . . ? C25A Si1 C24 115.0(14) . . ? C6 N1 Dy1 102.42(14) . . ? C4 N1 Dy1 134.62(18) . . ? C4 N1 C6 122.8(2) . . ? C2 N2 Dy1 130.10(18) . . ? C2 N2 C18 115.6(2) . . ? C18 N2 Dy1 114.33(18) . . ? C21 N3 Dy1 117.24(19) . . ? C19 N3 Dy1 98.96(18) . . ? C19 N3 C21 108.4(3) . . ? C20 N3 Dy1 111.2(2) . . ? C20 N3 C21 108.2(3) . . ? C20 N3 C19 112.6(3) . . ? C11 C6 N1 121.0(2) . . ? C11 C6 C7 120.4(2) . . ? C7 C6 N1 118.1(2) . . ? C6 C11 C15 122.5(2) . . ? C10 C11 C6 117.9(3) . . ? C10 C11 C15 119.5(3) . . ? P1 C22 Dy1 99.03(12) . . ? P1 C22 Si1 133.82(16) . . ? Si1 C22 Dy1 127.04(13) . . ? C31 C26 P1 121.9(2) . . ? C27 C26 P1 119.5(2) . . ? C27 C26 C31 118.6(3) . . ? N2 C2 C3 124.7(3) . . ? N2 C2 C1 119.8(3) . . ? C3 C2 C1 115.5(3) . . ? C11 C10 H10 118.9 . . ? C9 C10 C11 122.1(3) . . ? C9 C10 H10 118.9 . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C9 C8 C7 121.8(3) . . ? C6 C7 C12 121.4(3) . . ? C8 C7 C6 118.2(3) . . ? C8 C7 C12 120.4(3) . . ? C26 C31 H31 119.8 . . ? C26 C31 C30 120.4(4) . . ? C30 C31 H31 119.8 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C10 C9 H9 120.3 . . ? C8 C9 C10 119.5(3) . . ? C8 C9 H9 120.3 . . ? C33 C32 P1 119.3(3) . . ? C33 C32 C37 119.4(4) . . ? C37 C32 P1 121.1(3) . . ? C2 C3 H3 115.0 . . ? C4 C3 C2 130.0(3) . . ? C4 C3 H3 115.0 . . ? C31 C30 H30 119.9 . . ? C29 C30 C31 120.2(4) . . ? C29 C30 H30 119.9 . . ? C26 C27 H27 119.8 . . ? C26 C27 C28 120.5(3) . . ? C28 C27 H27 119.8 . . ? N3 C19 H19A 109.0 . . ? N3 C19 H19B 109.0 . . ? N3 C19 C18 113.0(3) . . ? H19A C19 H19B 107.8 . . ? C18 C19 H19A 109.0 . . ? C18 C19 H19B 109.0 . . ? N1 C4 C3 122.4(2) . . ? N1 C4 C5 121.0(3) . . ? C3 C4 C5 116.5(3) . . ? C11 C15 H15 107.6 . . ? C11 C15 C16 112.9(3) . . ? C11 C15 C17 110.7(3) . . ? C16 C15 H15 107.6 . . ? C16 C15 C17 110.2(3) . . ? C17 C15 H15 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C7 C12 H12 107.8 . . ? C7 C12 C14 110.0(3) . . ? C7 C12 C13 113.9(3) . . ? C14 C12 H12 107.8 . . ? C13 C12 H12 107.8 . . ? C13 C12 C14 109.3(3) . . ? N2 C18 C19 111.4(3) . . ? N2 C18 H18A 109.3 . . ? N2 C18 H18B 109.3 . . ? C19 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C27 C28 H28 119.8 . . ? C29 C28 C27 120.4(4) . . ? C29 C28 H28 119.8 . . ? C32 C33 H33 120.0 . . ? C32 C33 C34 120.1(5) . . ? C34 C33 H33 120.0 . . ? C30 C29 C28 119.9(3) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C32 C37 H37 120.4 . . ? C32 C37 C36 119.1(6) . . ? C36 C37 H37 120.4 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C34 C35 C36 120.4(6) . . ? C37 C36 H36 119.6 . . ? C35 C36 C37 120.7(7) . . ? C35 C36 H36 119.6 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C33 C34 H34 119.9 . . ? C35 C34 C33 120.2(6) . . ? C35 C34 H34 119.9 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C25A H25D 109.5 . . ? Si1 C25A H25E 109.5 . . ? Si1 C25A H25F 109.5 . . ? H25D C25A H25E 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 Se1 2.8058(3) . ? Dy1 N1 2.319(2) . ? Dy1 N2 2.383(2) . ? Dy1 N3 2.506(2) . ? Dy1 C22 2.266(3) . ? Se1 P1 2.2265(7) . ? P1 C22 1.662(3) . ? P1 C26 1.842(3) . ? P1 C32 1.836(3) . ? Si1 C22 1.809(3) . ? Si1 C23 1.885(4) . ? Si1 C24 1.881(4) . ? Si1 C25 1.95(4) . ? Si1 C25A 1.84(3) . ? N1 C6 1.435(3) . ? N1 C4 1.322(3) . ? N2 C2 1.332(3) . ? N2 C18 1.472(4) . ? N3 C21 1.486(4) . ? N3 C19 1.477(4) . ? N3 C20 1.474(4) . ? C6 C11 1.408(4) . ? C6 C7 1.412(4) . ? C11 C10 1.391(4) . ? C11 C15 1.517(4) . ? C26 C31 1.386(4) . ? C26 C27 1.377(4) . ? C2 C3 1.396(4) . ? C2 C1 1.521(4) . ? C10 H10 0.9300 . ? C10 C9 1.370(5) . ? C8 H8 0.9300 . ? C8 C7 1.392(4) . ? C8 C9 1.367(5) . ? C7 C12 1.516(4) . ? C31 H31 0.9300 . ? C31 C30 1.387(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C9 H9 0.9300 . ? C32 C33 1.380(5) . ? C32 C37 1.384(5) . ? C3 H3 0.9300 . ? C3 C4 1.393(4) . ? C30 H30 0.9300 . ? C30 C29 1.365(6) . ? C27 H27 0.9300 . ? C27 C28 1.387(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C18 1.500(5) . ? C4 C5 1.516(4) . ? C15 H15 0.9800 . ? C15 C16 1.521(5) . ? C15 C17 1.544(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C12 H12 0.9800 . ? C12 C14 1.532(5) . ? C12 C13 1.517(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C28 H28 0.9300 . ? C28 C29 1.365(6) . ? C33 H33 0.9300 . ? C33 C34 1.391(6) . ? C29 H29 0.9300 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C37 H37 0.9300 . ? C37 C36 1.395(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C35 H35 0.9300 . ? C35 C36 1.359(12) . ? C35 C34 1.352(11) . ? C36 H36 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C34 H34 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C25A H25D 0.9600 . ? C25A H25E 0.9600 . ? C25A H25F 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Dy1 N1 C6 C11 97.9(2) . . . . ? Dy1 N1 C6 C7 -74.5(2) . . . . ? Dy1 N1 C4 C3 -1.7(5) . . . . ? Dy1 N1 C4 C5 176.4(2) . . . . ? Dy1 N2 C2 C3 -8.1(5) . . . . ? Dy1 N2 C2 C1 174.2(2) . . . . ? Dy1 N2 C18 C19 -1.6(4) . . . . ? Dy1 N3 C19 C18 -60.9(3) . . . . ? Se1 P1 C22 Dy1 -0.09(12) . . . . ? Se1 P1 C22 Si1 176.23(18) . . . . ? Se1 P1 C26 C31 -60.6(3) . . . . ? Se1 P1 C26 C27 116.7(2) . . . . ? Se1 P1 C32 C33 155.2(2) . . . . ? Se1 P1 C32 C37 -29.4(3) . . . . ? P1 C26 C31 C30 177.7(3) . . . . ? P1 C26 C27 C28 -177.3(3) . . . . ? P1 C32 C33 C34 174.7(3) . . . . ? P1 C32 C37 C36 -173.8(3) . . . . ? N1 C6 C11 C10 -169.9(2) . . . . ? N1 C6 C11 C15 11.8(4) . . . . ? N1 C6 C7 C8 170.6(2) . . . . ? N1 C6 C7 C12 -12.0(4) . . . . ? N2 C2 C3 C4 -4.2(6) . . . . ? N3 C19 C18 N2 45.8(4) . . . . ? C6 N1 C4 C3 -175.6(3) . . . . ? C6 N1 C4 C5 2.4(4) . . . . ? C6 C11 C10 C9 -0.5(5) . . . . ? C6 C11 C15 C16 -122.2(3) . . . . ? C6 C11 C15 C17 113.7(3) . . . . ? C6 C7 C12 C14 -98.1(4) . . . . ? C6 C7 C12 C13 138.8(3) . . . . ? C11 C6 C7 C8 -1.8(4) . . . . ? C11 C6 C7 C12 175.6(3) . . . . ? C11 C10 C9 C8 -1.7(5) . . . . ? C22 P1 C26 C31 177.4(2) . . . . ? C22 P1 C26 C27 -5.3(3) . . . . ? C22 P1 C32 C33 -81.5(3) . . . . ? C22 P1 C32 C37 94.0(3) . . . . ? C26 P1 C22 Dy1 118.34(12) . . . . ? C26 P1 C22 Si1 -65.3(3) . . . . ? C26 P1 C32 C33 47.4(3) . . . . ? C26 P1 C32 C37 -137.2(3) . . . . ? C26 C31 C30 C29 -0.7(6) . . . . ? C26 C27 C28 C29 -0.2(5) . . . . ? C2 N2 C18 C19 178.6(3) . . . . ? C2 C3 C4 N1 9.4(5) . . . . ? C2 C3 C4 C5 -168.8(3) . . . . ? C10 C11 C15 C16 59.6(4) . . . . ? C10 C11 C15 C17 -64.5(4) . . . . ? C8 C7 C12 C14 79.3(4) . . . . ? C8 C7 C12 C13 -43.8(4) . . . . ? C7 C6 C11 C10 2.2(4) . . . . ? C7 C6 C11 C15 -176.0(3) . . . . ? C7 C8 C9 C10 2.1(5) . . . . ? C31 C26 C27 C28 0.1(5) . . . . ? C31 C30 C29 C28 0.6(6) . . . . ? C21 N3 C19 C18 176.3(3) . . . . ? C9 C8 C7 C6 -0.4(4) . . . . ? C9 C8 C7 C12 -177.8(3) . . . . ? C32 P1 C22 Dy1 -120.46(15) . . . . ? C32 P1 C22 Si1 55.9(3) . . . . ? C32 P1 C26 C31 48.1(3) . . . . ? C32 P1 C26 C27 -134.7(2) . . . . ? C32 C33 C34 C35 -0.3(7) . . . . ? C32 C37 C36 C35 -1.3(8) . . . . ? C27 C26 C31 C30 0.4(5) . . . . ? C27 C28 C29 C30 -0.2(6) . . . . ? C4 N1 C6 C11 -86.6(3) . . . . ? C4 N1 C6 C7 101.1(3) . . . . ? C15 C11 C10 C9 177.8(3) . . . . ? C1 C2 C3 C4 173.6(3) . . . . ? C20 N3 C19 C18 56.6(4) . . . . ? C18 N2 C2 C3 171.7(3) . . . . ? C18 N2 C2 C1 -6.0(4) . . . . ? C33 C32 C37 C36 1.6(6) . . . . ? C37 C32 C33 C34 -0.8(5) . . . . ? C23 Si1 C22 Dy1 -76.6(2) . . . . ? C23 Si1 C22 P1 107.9(3) . . . . ? C36 C35 C34 C33 0.6(9) . . . . ? C24 Si1 C22 Dy1 37.0(3) . . . . ? C24 Si1 C22 P1 -138.5(3) . . . . ? C34 C35 C36 C37 0.1(10) . . . . ? C25 Si1 C22 Dy1 144(4) . . . . ? C25 Si1 C22 P1 -31(4) . . . . ? C25A Si1 C22 Dy1 169.7(15) . . . . ? C25A Si1 C22 P1 -5.8(15) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.312 -0.275 0.092 260.2 58.1 ? 2 -0.188 0.225 0.408 260.2 61.8 ? 3 0.188 -0.225 0.592 260.2 58.1 ? 4 0.312 0.275 0.908 260.2 61.8 ?