#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572188.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_1572188 loop_ _publ_author_name 'Delano, Francis' 'Benner, Florian' 'Jang, Seoyun' 'Greer, Samuel M.' 'Demir, Selvan' _publ_section_title ; Construction of intermolecular \s-hole interactions in rare earth metallocene complexes using a 2,3,4,5-tetraiodopyrrolyl anion ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC03786C _journal_year 2024 _chemical_formula_moiety 'C24 H30 Dy I4 N, C H2 Cl2' _chemical_formula_sum 'C25 H32 Cl2 Dy I4 N' _chemical_formula_weight 1087.51 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-07-10 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-04-22 deposited with the CCDC. 2024-07-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.4755(17) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.31657(18) _cell_length_b 14.2556(2) _cell_length_c 21.2459(4) _cell_measurement_reflns_used 22031 _cell_measurement_temperature 110.01(10) _cell_measurement_theta_max 31.6560 _cell_measurement_theta_min 2.8550 _cell_volume 3062.15(9) _computing_cell_refinement 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _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 (Sheldrick, 2015)' _diffrn_ambient_temperature 110.01(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.838 _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 4.00 29.00 0.50 1.50 -- 6.58 -78.00 129.00 50 2 \w -39.00 -12.00 0.50 1.50 -- -7.98 -78.00 129.00 54 3 \w -28.00 19.00 0.50 1.50 -- -7.98 78.00-104.00 94 4 \w 0.00 35.00 0.50 1.50 -- 6.58 -99.00 120.00 70 5 \w 6.00 39.00 0.50 1.50 -- 6.58 -99.00-120.00 66 6 \w -11.00 15.00 0.50 1.50 -- 6.58 -77.00 60.00 52 7 \w 2.00 38.00 0.50 1.50 -- 6.58 57.00 -90.00 72 8 \w -31.00 7.00 0.50 1.50 -- -7.98 -57.00 30.00 76 9 \w -23.00 15.00 0.50 1.50 -- -7.98 77.00 -60.00 76 10 \w -28.00 7.00 0.50 1.50 -- -7.98 -57.00 60.00 70 11 \w -15.00 15.00 0.50 1.50 -- -7.98 -77.00 -30.00 60 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0373890000 _diffrn_orient_matrix_UB_12 0.0410200000 _diffrn_orient_matrix_UB_13 0.0099705000 _diffrn_orient_matrix_UB_21 0.0047967000 _diffrn_orient_matrix_UB_22 0.0090581000 _diffrn_orient_matrix_UB_23 -0.0322936000 _diffrn_orient_matrix_UB_31 -0.0591347000 _diffrn_orient_matrix_UB_32 0.0266728000 _diffrn_orient_matrix_UB_33 -0.0043660000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_unetI/netI 0.0428 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.838 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 37662 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.838 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.735 _diffrn_reflns_theta_min 2.470 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.662 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.220 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 2.359 _exptl_crystal_description plate _exptl_crystal_F_000 2004 _exptl_crystal_size_max 0.353 _exptl_crystal_size_mid 0.275 _exptl_crystal_size_min 0.111 _refine_diff_density_max 1.511 _refine_diff_density_min -1.747 _refine_diff_density_rms 0.203 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8713 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0308 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.0770 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7451 _reflns_number_total 8713 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP110K _cod_database_code 1572188 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C25H32Cl2DyI4N _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 0.525 _shelx_estimated_absorpt_t_min 0.202 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Cl1B \\sim Cl1A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 3. Others Fixed Sof: Cl1A(0.5) H26C(0.5) H26D(0.5) H26A(0.5) H26B(0.5) Cl1B(0.5) 4.a Secondary CH2 refined with riding coordinates: C26(H26C,H26D), C26(H26A,H26B) 4.b Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C15(H15A,H15B,H15C), C12(H12A,H12B, H12C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A, H23B,H23C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C) ; _shelx_res_file ; TITL fed728_100_final_a.res in P2(1)/c fed728_110_final.res created by SHELXL-2018/3 at 15:25:08 on 10-Jul-2023 REM Old TITL FED728_100_Final in P21/c #14 REM SHELXT solution in P2(1)/c: R1 0.076, Rweak 0.002, Alpha 0.023 REM 0.488 for 262 systematic absences, Orientation as input REM Formula found by SHELXT: C24 N Cl2 I4 Dy CELL 0.71073 10.316572 14.255598 21.245931 90 101.4755 90 ZERR 4 0.000182 0.00024 0.000377 0 0.0017 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Dy I N UNIT 100 128 8 4 16 4 SIMU Cl1B Cl1A L.S. 4 0 0 PLAN 14 SIZE 0.111 0.275 0.353 TEMP -163 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.040600 FVAR 0.64473 DY1 4 0.805457 0.712813 0.339828 11.00000 0.01270 0.01160 = 0.01164 -0.00053 0.00012 0.00177 I1 5 0.525780 0.611808 0.283553 11.00000 0.01791 0.01464 = 0.01755 0.00087 0.00239 -0.00436 I4 5 0.819119 0.939727 0.201703 11.00000 0.01757 0.01745 = 0.02283 0.00278 0.00303 -0.00422 I3 5 0.481033 0.933634 0.081341 11.00000 0.02264 0.02018 = 0.01543 0.00422 0.00180 0.00635 I2 5 0.290867 0.716222 0.131766 11.00000 0.01526 0.02468 = 0.03511 0.00111 -0.00744 -0.00312 CL2 3 0.610966 0.630232 0.079906 11.00000 0.03690 0.03626 = 0.02546 0.00339 0.00608 0.01306 PART 1 CL1A 3 0.686761 0.445211 0.038474 10.50000 0.04819 0.02749 = 0.15456 -0.02541 -0.00093 0.00152 PART 0 N1 6 0.676606 0.772553 0.242697 11.00000 0.01447 0.01589 = 0.01410 0.00108 0.00219 -0.00211 C5 1 0.666896 0.843823 0.198919 11.00000 0.01546 0.01171 = 0.01777 0.00075 0.00413 -0.00144 C2 1 0.559630 0.725443 0.227006 11.00000 0.01423 0.01514 = 0.01696 0.00000 0.00273 -0.00191 C10 1 0.958147 0.647750 0.262774 11.00000 0.01621 0.01313 = 0.01881 0.00177 0.00584 0.00373 C6 1 0.886399 0.568833 0.278325 11.00000 0.01677 0.00948 = 0.01904 -0.00349 0.00364 -0.00006 C8 1 1.029960 0.617643 0.369995 11.00000 0.01515 0.02421 = 0.01954 -0.00364 -0.00225 0.01097 C21 1 0.518280 0.740598 0.423977 11.00000 0.01731 0.02585 = 0.02603 -0.00452 0.00671 -0.00103 AFIX 137 H21A 2 0.456290 0.760396 0.385110 11.00000 -1.50000 H21B 2 0.491706 0.768040 0.461767 11.00000 -1.50000 H21C 2 0.517525 0.672031 0.427208 11.00000 -1.50000 AFIX 0 C20 1 0.687171 0.854023 0.386898 11.00000 0.02342 0.01353 = 0.01402 -0.00310 0.00308 0.00563 C19 1 0.825516 0.870093 0.405848 11.00000 0.02183 0.01635 = 0.01624 -0.00254 0.00492 0.00168 C4 1 0.545745 0.841778 0.156511 11.00000 0.01502 0.01591 = 0.01678 0.00126 0.00396 0.00278 C9 1 1.045451 0.678015 0.319444 11.00000 0.01290 0.01739 = 0.02789 -0.00610 0.00452 0.00098 C3 1 0.475664 0.764628 0.174975 11.00000 0.01475 0.01627 = 0.01790 0.00013 0.00013 0.00068 C16 1 0.656281 0.773547 0.420647 11.00000 0.01721 0.01431 = 0.01412 -0.00089 0.00330 0.00370 C25 1 0.588538 0.916682 0.344187 11.00000 0.03288 0.02756 = 0.02356 0.00024 0.00381 0.01566 AFIX 137 H25A 2 0.634804 0.955792 0.317765 11.00000 -1.50000 H25B 2 0.544400 0.956936 0.370857 11.00000 -1.50000 H25C 2 0.522527 0.877900 0.316275 11.00000 -1.50000 AFIX 0 C15 1 0.951791 0.683719 0.195767 11.00000 0.03008 0.03027 = 0.02107 0.00335 0.01030 0.00463 AFIX 137 H15A 2 0.859182 0.693074 0.174735 11.00000 -1.50000 H15B 2 0.992805 0.638032 0.171322 11.00000 -1.50000 H15C 2 0.999242 0.743517 0.197533 11.00000 -1.50000 AFIX 0 C12 1 0.887173 0.469650 0.381337 11.00000 0.03551 0.02426 = 0.03583 0.01268 0.01717 0.00944 AFIX 137 H12A 2 0.889135 0.488697 0.425837 11.00000 -1.50000 H12B 2 0.947081 0.416431 0.380817 11.00000 -1.50000 H12C 2 0.796990 0.451225 0.361089 11.00000 -1.50000 AFIX 0 C11 1 0.799019 0.507707 0.229890 11.00000 0.02426 0.02650 = 0.03190 -0.01536 0.00469 -0.00262 AFIX 137 H11A 2 0.752759 0.462427 0.252253 11.00000 -1.50000 H11B 2 0.853212 0.474035 0.204269 11.00000 -1.50000 H11C 2 0.734147 0.546828 0.201586 11.00000 -1.50000 AFIX 0 C14 1 1.148091 0.754009 0.322192 11.00000 0.01817 0.03176 = 0.04868 -0.01022 0.00892 -0.00506 AFIX 137 H14A 2 1.111765 0.805256 0.293257 11.00000 -1.50000 H14B 2 1.226532 0.728243 0.308903 11.00000 -1.50000 H14C 2 1.172685 0.777918 0.366201 11.00000 -1.50000 AFIX 0 C17 1 0.774684 0.739244 0.459927 11.00000 0.01986 0.01385 = 0.01314 -0.00187 0.00319 -0.00035 C18 1 0.879291 0.799969 0.451317 11.00000 0.01695 0.01703 = 0.01445 -0.00465 0.00165 0.00061 C22 1 0.784628 0.660455 0.506898 11.00000 0.02975 0.02312 = 0.01976 0.00885 0.00374 0.00384 AFIX 137 H22A 2 0.725142 0.609637 0.488358 11.00000 -1.50000 H22B 2 0.759467 0.682814 0.546410 11.00000 -1.50000 H22C 2 0.875804 0.637175 0.516771 11.00000 -1.50000 AFIX 0 C7 1 0.930580 0.550287 0.344953 11.00000 0.02037 0.01571 = 0.02534 0.00450 0.00840 0.00585 C23 1 1.014440 0.803580 0.492945 11.00000 0.02232 0.02833 = 0.02445 -0.00628 -0.00056 -0.00203 AFIX 137 H23A 2 1.034743 0.743033 0.514498 11.00000 -1.50000 H23B 2 1.017328 0.853072 0.525208 11.00000 -1.50000 H23C 2 1.079779 0.817001 0.466397 11.00000 -1.50000 AFIX 0 C13 1 1.120297 0.608999 0.434410 11.00000 0.03845 0.04255 = 0.02224 -0.00697 -0.00904 0.02457 AFIX 137 H13A 2 1.172638 0.666508 0.443747 11.00000 -1.50000 H13B 2 1.179682 0.555425 0.434077 11.00000 -1.50000 H13C 2 1.067603 0.599417 0.467497 11.00000 -1.50000 AFIX 0 C24 1 0.902153 0.953927 0.389453 11.00000 0.03844 0.01745 = 0.02674 -0.00273 0.01255 -0.00650 AFIX 137 H24A 2 0.983520 0.932535 0.376761 11.00000 -1.50000 H24B 2 0.924630 0.994924 0.427072 11.00000 -1.50000 H24C 2 0.848002 0.988682 0.353893 11.00000 -1.50000 AFIX 0 C26 1 0.707171 0.559764 0.040503 11.00000 0.14954 0.03032 = 0.07854 0.01748 0.09143 0.02019 PART 1 AFIX 23 H26C 2 0.693562 0.581812 -0.004521 10.50000 -1.20000 H26D 2 0.800905 0.572132 0.060179 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.679922 0.570209 -0.006334 10.50000 -1.20000 H26B 2 0.800763 0.579329 0.053460 10.50000 -1.20000 AFIX 0 CL1B 3 0.695845 0.442154 0.055884 10.50000 0.05297 0.02690 = 0.03692 0.00773 0.02137 0.00592 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0770, GooF = S = 1.041, Restrained GooF = 1.041 for all data REM R1 = 0.0308 for 7451 Fo > 4sig(Fo) and 0.0389 for all 8713 data REM 317 parameters refined using 6 restraints END WGHT 0.0406 0.0000 REM Highest difference peak 1.511, deepest hole -1.747, 1-sigma level 0.203 Q1 1 0.8851 0.7442 0.3390 11.00000 0.05 1.14 Q2 1 0.8946 0.9004 0.1980 11.00000 0.05 1.09 Q3 1 0.7099 0.7194 0.3787 11.00000 0.05 1.03 Q4 1 0.7249 0.5638 0.0587 11.00000 0.05 1.00 Q5 1 0.5624 0.8978 0.0791 11.00000 0.05 0.96 Q6 1 0.4539 0.6395 0.2815 11.00000 0.05 0.95 Q7 1 1.1002 0.7182 0.1846 11.00000 0.05 0.93 Q8 1 0.4960 0.7953 0.4379 11.00000 0.05 0.93 Q9 1 0.5629 0.9745 0.0743 11.00000 0.05 0.91 Q10 1 0.7442 0.9018 0.2034 11.00000 0.05 0.90 Q11 1 0.8977 0.7123 0.3000 11.00000 0.05 0.88 Q12 1 0.3964 0.8996 0.0827 11.00000 0.05 0.87 Q13 1 0.5598 0.9245 0.0424 11.00000 0.05 0.86 Q14 1 0.5837 0.7665 0.4199 11.00000 0.05 0.84 ; _shelx_res_checksum 48853 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.387 _oxdiff_exptl_absorpt_empirical_full_min 0.675 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.80546(2) 0.71281(2) 0.33983(2) 0.01230(5) Uani 1 1 d . . . . . I1 I 0.52578(2) 0.61181(2) 0.28355(2) 0.01686(6) Uani 1 1 d . . . . . I4 I 0.81912(2) 0.93973(2) 0.20170(2) 0.01942(6) Uani 1 1 d . . . . . I3 I 0.48103(2) 0.93363(2) 0.08134(2) 0.01969(6) Uani 1 1 d . . . . . I2 I 0.29087(2) 0.71622(2) 0.13177(2) 0.02673(7) Uani 1 1 d . . . . . Cl2 Cl 0.61097(11) 0.63023(8) 0.07991(5) 0.0329(2) Uani 1 1 d . . . . . Cl1A Cl 0.6868(9) 0.4452(5) 0.0385(4) 0.080(2) Uani 0.5 1 d . U P A 1 N1 N 0.6766(3) 0.77255(19) 0.24270(14) 0.0149(6) Uani 1 1 d . . . . . C5 C 0.6669(3) 0.8438(2) 0.19892(17) 0.0149(6) Uani 1 1 d . . . . . C2 C 0.5596(3) 0.7254(2) 0.22701(17) 0.0155(7) Uani 1 1 d . . . . . C10 C 0.9581(3) 0.6478(2) 0.26277(17) 0.0157(7) Uani 1 1 d . . . . . C6 C 0.8864(3) 0.5688(2) 0.27832(17) 0.0151(7) Uani 1 1 d . . . . . C8 C 1.0300(3) 0.6176(3) 0.37000(18) 0.0204(7) Uani 1 1 d . . . . . C21 C 0.5183(4) 0.7406(3) 0.4240(2) 0.0227(8) Uani 1 1 d . . . . . H21A H 0.456290 0.760396 0.385110 0.034 Uiso 1 1 calc R U . . . H21B H 0.491706 0.768040 0.461767 0.034 Uiso 1 1 calc R U . . . H21C H 0.517525 0.672031 0.427208 0.034 Uiso 1 1 calc R U . . . C20 C 0.6872(4) 0.8540(2) 0.38690(17) 0.0171(7) Uani 1 1 d . . . . . C19 C 0.8255(4) 0.8701(2) 0.40585(17) 0.0180(7) Uani 1 1 d . . . . . C4 C 0.5457(3) 0.8418(2) 0.15651(17) 0.0158(6) Uani 1 1 d . . . . . C9 C 1.0455(3) 0.6780(2) 0.31944(19) 0.0193(7) Uani 1 1 d . . . . . C3 C 0.4757(3) 0.7646(2) 0.17497(18) 0.0167(7) Uani 1 1 d . . . . . C16 C 0.6563(3) 0.7735(2) 0.42065(17) 0.0152(7) Uani 1 1 d . . . . . C25 C 0.5885(4) 0.9167(3) 0.3442(2) 0.0283(9) Uani 1 1 d . . . . . H25A H 0.634804 0.955792 0.317765 0.042 Uiso 1 1 calc R U . . . H25B H 0.544400 0.956936 0.370857 0.042 Uiso 1 1 calc R U . . . H25C H 0.522527 0.877900 0.316275 0.042 Uiso 1 1 calc R U . . . C15 C 0.9518(4) 0.6837(3) 0.19577(19) 0.0264(8) Uani 1 1 d . . . . . H15A H 0.859182 0.693074 0.174735 0.040 Uiso 1 1 calc R U . . . H15B H 0.992805 0.638032 0.171322 0.040 Uiso 1 1 calc R U . . . H15C H 0.999242 0.743517 0.197533 0.040 Uiso 1 1 calc R U . . . C12 C 0.8872(4) 0.4697(3) 0.3813(2) 0.0305(9) Uani 1 1 d . . . . . H12A H 0.889135 0.488697 0.425837 0.046 Uiso 1 1 calc R U . . . H12B H 0.947081 0.416431 0.380817 0.046 Uiso 1 1 calc R U . . . H12C H 0.796990 0.451225 0.361089 0.046 Uiso 1 1 calc R U . . . C11 C 0.7990(4) 0.5077(3) 0.2299(2) 0.0277(9) Uani 1 1 d . . . . . H11A H 0.752759 0.462427 0.252253 0.042 Uiso 1 1 calc R U . . . H11B H 0.853212 0.474035 0.204269 0.042 Uiso 1 1 calc R U . . . H11C H 0.734147 0.546828 0.201586 0.042 Uiso 1 1 calc R U . . . C14 C 1.1481(4) 0.7540(3) 0.3222(2) 0.0326(10) Uani 1 1 d . . . . . H14A H 1.111765 0.805256 0.293257 0.049 Uiso 1 1 calc R U . . . H14B H 1.226532 0.728243 0.308903 0.049 Uiso 1 1 calc R U . . . H14C H 1.172685 0.777918 0.366201 0.049 Uiso 1 1 calc R U . . . C17 C 0.7747(3) 0.7392(2) 0.45993(17) 0.0156(6) Uani 1 1 d . . . . . C18 C 0.8793(3) 0.8000(2) 0.45132(17) 0.0163(7) Uani 1 1 d . . . . . C22 C 0.7846(4) 0.6605(3) 0.50690(19) 0.0244(8) Uani 1 1 d . . . . . H22A H 0.725142 0.609637 0.488358 0.037 Uiso 1 1 calc R U . . . H22B H 0.759467 0.682814 0.546410 0.037 Uiso 1 1 calc R U . . . H22C H 0.875804 0.637175 0.516771 0.037 Uiso 1 1 calc R U . . . C7 C 0.9306(4) 0.5503(2) 0.34495(19) 0.0199(7) Uani 1 1 d . . . . . C23 C 1.0144(4) 0.8036(3) 0.4929(2) 0.0258(8) Uani 1 1 d . . . . . H23A H 1.034743 0.743033 0.514498 0.039 Uiso 1 1 calc R U . . . H23B H 1.017328 0.853072 0.525208 0.039 Uiso 1 1 calc R U . . . H23C H 1.079779 0.817001 0.466397 0.039 Uiso 1 1 calc R U . . . C13 C 1.1203(5) 0.6090(3) 0.4344(2) 0.0365(11) Uani 1 1 d . . . . . H13A H 1.172638 0.666508 0.443747 0.055 Uiso 1 1 calc R U . . . H13B H 1.179682 0.555425 0.434077 0.055 Uiso 1 1 calc R U . . . H13C H 1.067603 0.599417 0.467497 0.055 Uiso 1 1 calc R U . . . C24 C 0.9022(4) 0.9539(3) 0.3895(2) 0.0267(8) Uani 1 1 d . . . . . H24A H 0.983520 0.932535 0.376761 0.040 Uiso 1 1 calc R U . . . H24B H 0.924630 0.994924 0.427072 0.040 Uiso 1 1 calc R U . . . H24C H 0.848002 0.988682 0.353893 0.040 Uiso 1 1 calc R U . . . C26 C 0.7072(9) 0.5598(3) 0.0405(4) 0.077(3) Uani 1 1 d . . . . . H26C H 0.693562 0.581812 -0.004521 0.092 Uiso 0.5 1 calc R U P A 1 H26D H 0.800905 0.572132 0.060179 0.092 Uiso 0.5 1 calc R U P A 1 H26A H 0.679922 0.570209 -0.006334 0.092 Uiso 0.5 1 calc R U P A -1 H26B H 0.800763 0.579329 0.053460 0.092 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.6958(8) 0.4422(5) 0.0559(3) 0.0372(12) Uani 0.5 1 d . U P A -1 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 0.01270(9) 0.01160(8) 0.01164(8) -0.00053(5) 0.00012(6) 0.00177(5) I1 0.01791(12) 0.01464(11) 0.01755(12) 0.00087(8) 0.00239(8) -0.00436(7) I4 0.01757(12) 0.01745(11) 0.02283(13) 0.00278(8) 0.00303(9) -0.00422(8) I3 0.02264(13) 0.02018(12) 0.01543(12) 0.00422(8) 0.00180(9) 0.00635(8) I2 0.01526(12) 0.02468(13) 0.03511(16) 0.00111(10) -0.00744(10) -0.00312(8) Cl2 0.0369(6) 0.0363(5) 0.0255(5) 0.0034(4) 0.0061(4) 0.0131(4) Cl1A 0.048(3) 0.027(3) 0.155(7) -0.025(4) -0.001(4) 0.0015(18) N1 0.0145(14) 0.0159(13) 0.0141(14) 0.0011(11) 0.0022(11) -0.0021(10) C5 0.0155(16) 0.0117(14) 0.0178(17) 0.0007(12) 0.0041(13) -0.0014(12) C2 0.0142(16) 0.0151(15) 0.0170(17) 0.0000(13) 0.0027(13) -0.0019(12) C10 0.0162(17) 0.0131(15) 0.0188(17) 0.0018(12) 0.0058(13) 0.0037(12) C6 0.0168(16) 0.0095(14) 0.0190(17) -0.0035(12) 0.0036(13) -0.0001(11) C8 0.0152(17) 0.0242(18) 0.0195(18) -0.0036(14) -0.0023(13) 0.0110(13) C21 0.0173(18) 0.0258(19) 0.026(2) -0.0045(15) 0.0067(15) -0.0010(14) C20 0.0234(18) 0.0135(15) 0.0140(16) -0.0031(13) 0.0031(13) 0.0056(13) C19 0.0218(18) 0.0164(16) 0.0162(17) -0.0025(13) 0.0049(14) 0.0017(13) C4 0.0150(16) 0.0159(16) 0.0168(17) 0.0013(13) 0.0040(13) 0.0028(12) C9 0.0129(16) 0.0174(16) 0.028(2) -0.0061(14) 0.0045(14) 0.0010(12) C3 0.0148(16) 0.0163(15) 0.0179(17) 0.0001(13) 0.0001(13) 0.0007(12) C16 0.0172(17) 0.0143(15) 0.0141(16) -0.0009(12) 0.0033(13) 0.0037(12) C25 0.033(2) 0.028(2) 0.024(2) 0.0002(16) 0.0038(17) 0.0157(16) C15 0.030(2) 0.030(2) 0.021(2) 0.0033(16) 0.0103(16) 0.0046(16) C12 0.036(2) 0.024(2) 0.036(2) 0.0127(17) 0.0172(19) 0.0094(17) C11 0.024(2) 0.026(2) 0.032(2) -0.0154(17) 0.0047(16) -0.0026(15) C14 0.0182(19) 0.032(2) 0.049(3) -0.010(2) 0.0089(18) -0.0051(16) C17 0.0199(17) 0.0139(15) 0.0131(16) -0.0019(12) 0.0032(13) -0.0003(12) C18 0.0170(17) 0.0170(16) 0.0144(16) -0.0046(13) 0.0016(13) 0.0006(12) C22 0.030(2) 0.0231(18) 0.0198(19) 0.0089(15) 0.0037(15) 0.0038(15) C7 0.0204(18) 0.0157(16) 0.025(2) 0.0045(14) 0.0084(15) 0.0059(13) C23 0.022(2) 0.0283(19) 0.024(2) -0.0063(16) -0.0006(15) -0.0020(15) C13 0.038(2) 0.043(3) 0.022(2) -0.0070(18) -0.0090(18) 0.025(2) C24 0.038(2) 0.0174(17) 0.027(2) -0.0027(15) 0.0126(18) -0.0065(15) C26 0.150(7) 0.030(3) 0.079(5) 0.017(3) 0.091(5) 0.020(3) Cl1B 0.053(3) 0.0269(18) 0.0369(15) 0.0077(12) 0.0214(17) 0.0059(16) 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' Cl Cl 0.1484 0.1585 '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' I I -0.4742 1.8119 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 -1 0 0.1241 -1 1 0 0.1231 1 1 0 0.1293 1 -1 0 0.1498 0 0 -1 0.0585 0 0 1 0.0528 -1 1 2 0.0993 1 -1 -2 0.1399 1 -1 1 0.1333 0 1 2 0.0924 2 -1 1 0.1448 0 1 -2 0.0988 -1 0 -2 0.1081 -1 0 2 0.1036 -6 7 -22 0.0941 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 I1 62.30(7) . . ? N1 Dy1 C10 83.56(10) . . ? N1 Dy1 C6 91.49(10) . . ? N1 Dy1 C8 134.72(11) . . ? N1 Dy1 C20 80.54(10) . . ? N1 Dy1 C19 97.38(10) . . ? N1 Dy1 C9 107.75(11) . . ? N1 Dy1 C16 98.50(10) . . ? N1 Dy1 C17 128.95(10) . . ? N1 Dy1 C18 128.27(10) . . ? N1 Dy1 C7 122.24(11) . . ? C10 Dy1 I1 102.22(8) . . ? C10 Dy1 C6 31.05(10) . . ? C10 Dy1 C16 177.83(10) . . ? C10 Dy1 C17 147.11(11) . . ? C6 Dy1 I1 79.55(7) . . ? C6 Dy1 C16 147.74(10) . . ? C6 Dy1 C17 133.69(11) . . ? C8 Dy1 I1 122.28(8) . . ? C8 Dy1 C10 51.18(11) . . ? C8 Dy1 C6 51.55(11) . . ? C8 Dy1 C20 138.00(11) . . ? C8 Dy1 C16 126.78(11) . . ? C8 Dy1 C17 96.08(11) . . ? C20 Dy1 I1 91.94(8) . . ? C20 Dy1 C10 150.70(11) . . ? C20 Dy1 C6 170.40(11) . . ? C20 Dy1 C16 31.02(10) . . ? C20 Dy1 C17 51.60(11) . . ? C19 Dy1 I1 123.12(8) . . ? C19 Dy1 C10 129.28(11) . . ? C19 Dy1 C6 157.21(11) . . ? C19 Dy1 C8 109.57(11) . . ? C19 Dy1 C20 31.24(11) . . ? C19 Dy1 C9 105.68(11) . . ? C19 Dy1 C16 51.29(11) . . ? C19 Dy1 C17 51.66(11) . . ? C19 Dy1 C18 31.29(11) . . ? C19 Dy1 C7 137.64(12) . . ? C9 Dy1 I1 130.67(8) . . ? C9 Dy1 C10 31.08(11) . . ? C9 Dy1 C6 51.54(10) . . ? C9 Dy1 C8 30.89(12) . . ? C9 Dy1 C20 136.11(11) . . ? C9 Dy1 C16 147.69(11) . . ? C9 Dy1 C17 118.56(11) . . ? C9 Dy1 C18 97.03(11) . . ? C16 Dy1 I1 78.23(8) . . ? C17 Dy1 I1 98.61(7) . . ? C17 Dy1 C16 30.96(10) . . ? C18 Dy1 I1 128.04(8) . . ? C18 Dy1 C10 127.95(11) . . ? C18 Dy1 C6 137.72(11) . . ? C18 Dy1 C8 86.67(11) . . ? C18 Dy1 C20 51.58(11) . . ? C18 Dy1 C16 51.12(11) . . ? C18 Dy1 C17 31.10(10) . . ? C7 Dy1 I1 91.00(8) . . ? C7 Dy1 C10 51.28(11) . . ? C7 Dy1 C6 31.15(11) . . ? C7 Dy1 C8 31.29(12) . . ? C7 Dy1 C20 155.17(11) . . ? C7 Dy1 C9 51.46(11) . . ? C7 Dy1 C16 126.68(11) . . ? C7 Dy1 C17 103.60(11) . . ? C7 Dy1 C18 108.85(12) . . ? C2 I1 Dy1 68.16(10) . . ? C5 N1 Dy1 144.0(2) . . ? C2 N1 Dy1 110.5(2) . . ? C2 N1 C5 105.0(3) . . ? N1 C5 I4 121.2(2) . . ? N1 C5 C4 111.1(3) . . ? C4 C5 I4 127.7(3) . . ? N1 C2 I1 118.9(2) . . ? N1 C2 C3 112.4(3) . . ? C3 C2 I1 128.7(3) . . ? C6 C10 Dy1 74.50(19) . . ? C6 C10 C15 124.3(3) . . ? C9 C10 Dy1 74.04(19) . . ? C9 C10 C6 108.4(3) . . ? C9 C10 C15 126.9(3) . . ? C15 C10 Dy1 123.1(2) . . ? C10 C6 Dy1 74.45(18) . . ? C10 C6 C11 124.7(3) . . ? C10 C6 C7 107.4(3) . . ? C11 C6 Dy1 125.5(2) . . ? C7 C6 Dy1 73.97(19) . . ? C7 C6 C11 127.1(3) . . ? C9 C8 Dy1 74.30(19) . . ? C9 C8 C7 108.0(3) . . ? C9 C8 C13 127.0(4) . . ? C7 C8 Dy1 74.10(19) . . ? C7 C8 C13 123.7(4) . . ? C13 C8 Dy1 128.1(3) . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? C19 C20 Dy1 73.61(19) . . ? C19 C20 C25 126.3(3) . . ? C16 C20 Dy1 75.15(18) . . ? C16 C20 C19 107.5(3) . . ? C16 C20 C25 126.0(3) . . ? C25 C20 Dy1 121.8(2) . . ? C20 C19 Dy1 75.15(19) . . ? C20 C19 C18 108.2(3) . . ? C20 C19 C24 127.1(3) . . ? C18 C19 Dy1 75.05(19) . . ? C18 C19 C24 124.1(3) . . ? C24 C19 Dy1 122.7(2) . . ? C5 C4 I3 126.7(2) . . ? C5 C4 C3 106.3(3) . . ? C3 C4 I3 127.0(3) . . ? C10 C9 Dy1 74.88(19) . . ? C10 C9 C14 125.0(4) . . ? C8 C9 Dy1 74.8(2) . . ? C8 C9 C10 108.2(3) . . ? C8 C9 C14 126.5(4) . . ? C14 C9 Dy1 122.2(2) . . ? C2 C3 I2 126.8(3) . . ? C2 C3 C4 105.3(3) . . ? C4 C3 I2 127.9(3) . . ? C21 C16 Dy1 126.7(2) . . ? C20 C16 Dy1 73.83(19) . . ? C20 C16 C21 125.5(3) . . ? C20 C16 C17 108.7(3) . . ? C17 C16 Dy1 74.21(19) . . ? C17 C16 C21 124.9(3) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C17 Dy1 74.83(19) . . ? C16 C17 C18 107.5(3) . . ? C16 C17 C22 126.0(3) . . ? C18 C17 Dy1 74.02(19) . . ? C18 C17 C22 126.2(3) . . ? C22 C17 Dy1 122.0(2) . . ? C19 C18 Dy1 73.7(2) . . ? C19 C18 C23 124.6(3) . . ? C17 C18 Dy1 74.88(19) . . ? C17 C18 C19 108.1(3) . . ? C17 C18 C23 125.9(3) . . ? C23 C18 Dy1 127.8(2) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C6 C7 Dy1 74.88(18) . . ? C6 C7 C8 108.1(3) . . ? C6 C7 C12 125.8(4) . . ? C8 C7 Dy1 74.61(19) . . ? C8 C7 C12 126.0(4) . . ? C12 C7 Dy1 119.9(2) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Cl2 C26 H26C 107.3 . . ? Cl2 C26 H26D 107.3 . . ? Cl2 C26 H26A 108.8 . . ? Cl2 C26 H26B 108.8 . . ? Cl1A C26 Cl2 120.2(5) . . ? Cl1A C26 H26C 107.3 . . ? Cl1A C26 H26D 107.3 . . ? Cl1A C26 H26A 96.5 . . ? Cl1A C26 H26B 113.5 . . ? Cl1A C26 Cl1B 12.3(4) . . ? H26C C26 H26D 106.9 . . ? H26C C26 H26A 12.5 . . ? H26C C26 H26B 97.0 . . ? H26D C26 H26A 117.1 . . ? H26D C26 H26B 10.2 . . ? H26A C26 H26B 107.7 . . ? Cl1B C26 Cl2 113.9(4) . . ? Cl1B C26 H26C 119.5 . . ? Cl1B C26 H26D 101.0 . . ? Cl1B C26 H26A 108.8 . . ? Cl1B C26 H26B 108.8 . . ? 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 I1 3.2334(3) . ? Dy1 N1 2.379(3) . ? Dy1 C10 2.655(3) . ? Dy1 C6 2.656(3) . ? Dy1 C8 2.650(3) . ? Dy1 C20 2.651(3) . ? Dy1 C19 2.631(3) . ? Dy1 C9 2.644(3) . ? Dy1 C16 2.668(3) . ? Dy1 C17 2.660(3) . ? Dy1 C18 2.649(3) . ? Dy1 C7 2.644(3) . ? I1 C2 2.087(3) . ? I4 C5 2.074(3) . ? I3 C4 2.070(3) . ? I2 C3 2.063(3) . ? Cl2 C26 1.739(5) . ? Cl1A C26 1.646(9) . ? N1 C5 1.368(4) . ? N1 C2 1.363(4) . ? C5 C4 1.388(5) . ? C2 C3 1.380(5) . ? C10 C6 1.421(5) . ? C10 C9 1.420(5) . ? C10 C15 1.502(5) . ? C6 C11 1.504(5) . ? C6 C7 1.423(5) . ? C8 C9 1.410(5) . ? C8 C7 1.428(5) . ? C8 C13 1.500(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C16 1.514(5) . ? C20 C19 1.422(5) . ? C20 C16 1.422(5) . ? C20 C25 1.513(5) . ? C19 C18 1.424(5) . ? C19 C24 1.511(5) . ? C4 C3 1.414(5) . ? C9 C14 1.508(5) . ? C16 C17 1.422(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12 C7 1.502(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C17 C18 1.423(5) . ? C17 C22 1.492(5) . ? C18 C23 1.496(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 H26C 0.9900 . ? C26 H26D 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 Cl1B 1.717(8) . ? 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 C5 I4 9.4(5) . . . . ? Dy1 N1 C5 C4 -169.5(3) . . . . ? Dy1 N1 C2 I1 -4.3(3) . . . . ? Dy1 N1 C2 C3 173.2(2) . . . . ? Dy1 C10 C6 C11 122.7(3) . . . . ? Dy1 C10 C6 C7 -67.2(2) . . . . ? Dy1 C10 C9 C8 68.0(2) . . . . ? Dy1 C10 C9 C14 -118.9(3) . . . . ? Dy1 C6 C7 C8 -67.8(2) . . . . ? Dy1 C6 C7 C12 116.2(3) . . . . ? Dy1 C8 C9 C10 -68.1(2) . . . . ? Dy1 C8 C9 C14 119.0(4) . . . . ? Dy1 C8 C7 C6 68.0(2) . . . . ? Dy1 C8 C7 C12 -116.1(4) . . . . ? Dy1 C20 C19 C18 -68.4(2) . . . . ? Dy1 C20 C19 C24 120.0(4) . . . . ? Dy1 C20 C16 C21 -123.9(3) . . . . ? Dy1 C20 C16 C17 66.6(2) . . . . ? Dy1 C19 C18 C17 -67.5(2) . . . . ? Dy1 C19 C18 C23 125.0(3) . . . . ? Dy1 C16 C17 C18 67.4(2) . . . . ? Dy1 C16 C17 C22 -118.8(3) . . . . ? Dy1 C17 C18 C19 66.7(2) . . . . ? Dy1 C17 C18 C23 -126.0(3) . . . . ? I1 C2 C3 I2 -4.8(5) . . . . ? I1 C2 C3 C4 177.6(2) . . . . ? I4 C5 C4 I3 1.2(5) . . . . ? I4 C5 C4 C3 -178.8(2) . . . . ? I3 C4 C3 I2 2.2(5) . . . . ? I3 C4 C3 C2 179.8(2) . . . . ? N1 C5 C4 I3 180.0(2) . . . . ? N1 C5 C4 C3 0.0(4) . . . . ? N1 C2 C3 I2 178.0(2) . . . . ? N1 C2 C3 C4 0.3(4) . . . . ? C5 N1 C2 I1 -177.8(2) . . . . ? C5 N1 C2 C3 -0.3(4) . . . . ? C5 C4 C3 I2 -177.8(3) . . . . ? C5 C4 C3 C2 -0.2(4) . . . . ? C2 N1 C5 I4 179.1(2) . . . . ? C2 N1 C5 C4 0.2(4) . . . . ? C10 C6 C7 Dy1 67.5(2) . . . . ? C10 C6 C7 C8 -0.3(4) . . . . ? C10 C6 C7 C12 -176.3(3) . . . . ? C6 C10 C9 Dy1 -67.2(2) . . . . ? C6 C10 C9 C8 0.8(4) . . . . ? C6 C10 C9 C14 173.9(3) . . . . ? C21 C16 C17 Dy1 124.0(3) . . . . ? C21 C16 C17 C18 -168.6(3) . . . . ? C21 C16 C17 C22 5.3(5) . . . . ? C20 C19 C18 Dy1 68.5(2) . . . . ? C20 C19 C18 C17 0.9(4) . . . . ? C20 C19 C18 C23 -166.5(3) . . . . ? C20 C16 C17 Dy1 -66.3(2) . . . . ? C20 C16 C17 C18 1.1(4) . . . . ? C20 C16 C17 C22 174.9(3) . . . . ? C19 C20 C16 Dy1 -67.1(2) . . . . ? C19 C20 C16 C21 169.0(3) . . . . ? C19 C20 C16 C17 -0.5(4) . . . . ? C9 C10 C6 Dy1 66.9(2) . . . . ? C9 C10 C6 C11 -170.5(3) . . . . ? C9 C10 C6 C7 -0.3(4) . . . . ? C9 C8 C7 Dy1 -67.2(2) . . . . ? C9 C8 C7 C6 0.9(4) . . . . ? C9 C8 C7 C12 176.8(3) . . . . ? C16 C20 C19 Dy1 68.1(2) . . . . ? C16 C20 C19 C18 -0.3(4) . . . . ? C16 C20 C19 C24 -171.8(3) . . . . ? C16 C17 C18 Dy1 -67.9(2) . . . . ? C16 C17 C18 C19 -1.2(4) . . . . ? C16 C17 C18 C23 166.0(3) . . . . ? C25 C20 C19 Dy1 -117.8(3) . . . . ? C25 C20 C19 C18 173.8(3) . . . . ? C25 C20 C19 C24 2.3(6) . . . . ? C25 C20 C16 Dy1 118.8(3) . . . . ? C25 C20 C16 C21 -5.1(6) . . . . ? C25 C20 C16 C17 -174.6(3) . . . . ? C15 C10 C6 Dy1 -119.8(3) . . . . ? C15 C10 C6 C11 2.9(5) . . . . ? C15 C10 C6 C7 173.1(3) . . . . ? C15 C10 C9 Dy1 119.7(3) . . . . ? C15 C10 C9 C8 -172.3(3) . . . . ? C15 C10 C9 C14 0.7(6) . . . . ? C11 C6 C7 Dy1 -122.7(4) . . . . ? C11 C6 C7 C8 169.5(3) . . . . ? C11 C6 C7 C12 -6.4(6) . . . . ? C22 C17 C18 Dy1 118.2(3) . . . . ? C22 C17 C18 C19 -175.1(3) . . . . ? C22 C17 C18 C23 -7.8(6) . . . . ? C7 C8 C9 Dy1 67.0(2) . . . . ? C7 C8 C9 C10 -1.0(4) . . . . ? C7 C8 C9 C14 -174.0(3) . . . . ? C13 C8 C9 Dy1 -126.2(4) . . . . ? C13 C8 C9 C10 165.7(3) . . . . ? C13 C8 C9 C14 -7.2(6) . . . . ? C13 C8 C7 Dy1 125.5(4) . . . . ? C13 C8 C7 C6 -166.4(3) . . . . ? C13 C8 C7 C12 9.5(6) . . . . ? C24 C19 C18 Dy1 -119.6(3) . . . . ? C24 C19 C18 C17 172.8(3) . . . . ? C24 C19 C18 C23 5.4(5) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1.0009 -0.9997 0.0094 -0.0783 -0.0142 0.0325 -1.0005 1.0022 0.0079 0.0038 0.0040 0.0859 1.0009 0.9997 -0.0094 0.0783 0.0142 -0.0325 1.0005 -1.0022 -0.0079 -0.0038 -0.0040 -0.0859 -0.0017 -0.0006 -0.9990 -0.0100 0.0322 0.0044 0.0017 0.0006 0.9990 0.0100 -0.0322 -0.0044 -0.9971 1.0034 2.0059 0.0239 -0.0605 0.0770 0.9971 -1.0034 -2.0059 -0.0239 0.0605 -0.0770 1.0021 -1.0016 0.9911 0.0063 -0.0363 -0.0903 0.0036 1.0022 1.9972 0.0612 -0.0554 0.0178 2.0028 -1.0028 0.9825 0.0435 -0.0312 -0.1495 -0.0031 0.9997 -1.9987 0.0210 0.0736 0.0356 -1.0040 -0.0000 -1.9893 -0.0574 0.0594 0.0681 -0.9973 0.0025 2.0066 -0.0172 -0.0696 0.0503 -5.7941 7.2662 -22.3628 -0.1415 0.7602 0.6341