#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:50:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294477 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572187.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_1572187 loop_ _publ_author_name 'Delano, 4th, Francis' 'Benner, Florian' 'Jang, Seoyun' 'Greer, Samuel M.' 'Demir, Selvan' _publ_section_title ; Construction of intermolecular σ-hole interactions in rare earth metallocene complexes using a 2,3,4,5-tetraiodopyrrolyl anion. ; _journal_issue 33 _journal_name_full 'Chemical science' _journal_page_first 13389 _journal_page_last 13404 _journal_paper_doi 10.1039/d4sc03786c _journal_volume 15 _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 101.5874(18) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.33800(19) _cell_length_b 14.2897(3) _cell_length_c 21.2600(4) _cell_measurement_reflns_used 21096 _cell_measurement_temperature 140.15(10) _cell_measurement_theta_max 31.6420 _cell_measurement_theta_min 2.8720 _cell_volume 3076.67(11) _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 140.15(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 0.842 _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 -0.0373373000 _diffrn_orient_matrix_UB_12 0.0410014000 _diffrn_orient_matrix_UB_13 -0.0097504000 _diffrn_orient_matrix_UB_21 -0.0045017000 _diffrn_orient_matrix_UB_22 0.0087327000 _diffrn_orient_matrix_UB_23 0.0323428000 _diffrn_orient_matrix_UB_31 0.0590570000 _diffrn_orient_matrix_UB_32 0.0265824000 _diffrn_orient_matrix_UB_33 0.0044165000 _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 0.0511 _diffrn_reflns_av_unetI/netI 0.0421 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.842 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 37940 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.842 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.680 _diffrn_reflns_theta_min 2.465 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.631 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.222 _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 2.348 _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 1.163 _refine_diff_density_min -1.284 _refine_diff_density_rms 0.179 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8758 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0297 _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^)+(0.0307P)^2^+2.3019P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.0708 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7303 _reflns_number_total 8758 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP140K _cod_depositor_comments 'Adding full bibliography for 1572175--1572199.cif.' _cod_original_cell_volume 3076.66(10) _cod_database_code 1572187 _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 0.526 _shelx_estimated_absorpt_t_min 0.203 _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_140_final.res created by SHELXL-2018/3 at 15:41:31 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 10.337998 14.289667 21.260032 90 101.5874 90 ZERR 4 0.00019 0.000251 0.0004 0 0.0018 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. 10 0 0 PLAN 14 SIZE 0.111 0.275 0.353 TEMP -133.0(1) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.030700 2.301900 FVAR 0.63826 DY1 4 0.805142 0.713592 0.339615 11.00000 0.01532 0.01504 = 0.01524 -0.00050 0.00049 0.00222 I1 5 0.525688 0.613108 0.282702 11.00000 0.02242 0.01915 = 0.02291 0.00105 0.00339 -0.00564 I4 5 0.819805 0.939703 0.201099 11.00000 0.02206 0.02290 = 0.02957 0.00357 0.00402 -0.00577 I3 5 0.482006 0.934925 0.081386 11.00000 0.02855 0.02625 = 0.02020 0.00574 0.00258 0.00850 I2 5 0.291494 0.718203 0.131301 11.00000 0.01882 0.03216 = 0.04475 0.00100 -0.00907 -0.00399 CL2 3 0.610030 0.629107 0.079704 11.00000 0.04790 0.04533 = 0.03335 0.00371 0.00804 0.01578 PART 1 CL1A 3 0.686943 0.445299 0.038450 10.50000 0.05561 0.03960 = 0.16947 -0.02591 -0.00049 -0.00031 PART 0 N1 6 0.676759 0.772901 0.242335 11.00000 0.01552 0.01921 = 0.01868 0.00072 0.00085 -0.00231 C5 1 0.668277 0.844166 0.198738 11.00000 0.01939 0.01674 = 0.01880 0.00062 0.00248 -0.00131 C2 1 0.559866 0.726698 0.226404 11.00000 0.01678 0.01853 = 0.02198 -0.00070 0.00483 -0.00295 C10 1 0.958252 0.648000 0.263297 11.00000 0.02040 0.01791 = 0.02198 0.00000 0.00540 0.00306 C6 1 0.887402 0.569237 0.279239 11.00000 0.01964 0.01421 = 0.02521 -0.00493 0.00326 0.00088 C8 1 1.029765 0.618713 0.370733 11.00000 0.02012 0.02426 = 0.02974 -0.00520 -0.00053 0.01111 C21 1 0.518897 0.740011 0.423859 11.00000 0.01957 0.03818 = 0.03046 -0.00782 0.00593 -0.00139 AFIX 137 H21A 2 0.456254 0.759409 0.385115 11.00000 -1.50000 H21B 2 0.492491 0.767004 0.461745 11.00000 -1.50000 H21C 2 0.519268 0.671593 0.427065 11.00000 -1.50000 AFIX 0 C20 1 0.686126 0.854006 0.386437 11.00000 0.02992 0.01938 = 0.01964 -0.00143 0.00481 0.00749 C19 1 0.823142 0.870282 0.405159 11.00000 0.02818 0.01967 = 0.02240 -0.00166 0.00737 0.00178 C4 1 0.547554 0.842676 0.156199 11.00000 0.01947 0.01820 = 0.02070 0.00421 0.00234 0.00287 C9 1 1.044839 0.679007 0.319561 11.00000 0.01304 0.02398 = 0.03225 -0.00819 0.00395 0.00099 C3 1 0.475992 0.766165 0.174209 11.00000 0.01842 0.02162 = 0.02126 -0.00036 0.00148 -0.00095 C16 1 0.655393 0.773916 0.420243 11.00000 0.01874 0.01826 = 0.02023 -0.00284 0.00312 0.00341 C25 1 0.586871 0.915871 0.343765 11.00000 0.03833 0.03364 = 0.02592 0.00048 0.00287 0.01942 AFIX 137 H25A 2 0.630695 0.950057 0.313971 11.00000 -1.50000 H25B 2 0.549633 0.960523 0.370284 11.00000 -1.50000 H25C 2 0.515915 0.877155 0.319364 11.00000 -1.50000 AFIX 0 C15 1 0.952436 0.683678 0.196545 11.00000 0.04041 0.03823 = 0.02793 0.00478 0.01400 0.01060 AFIX 137 H15A 2 0.860014 0.691501 0.174911 11.00000 -1.50000 H15B 2 0.995564 0.638786 0.172609 11.00000 -1.50000 H15C 2 0.997924 0.744090 0.198438 11.00000 -1.50000 AFIX 0 C12 1 0.888067 0.471444 0.382404 11.00000 0.04629 0.02886 = 0.04996 0.01883 0.02021 0.01399 AFIX 137 H12A 2 0.882274 0.492170 0.425691 11.00000 -1.50000 H12B 2 0.953052 0.420882 0.385344 11.00000 -1.50000 H12C 2 0.801563 0.448679 0.360071 11.00000 -1.50000 AFIX 0 C11 1 0.800071 0.507740 0.230857 11.00000 0.02560 0.03332 = 0.04468 -0.01844 0.00227 -0.00061 AFIX 137 H11A 2 0.754359 0.462490 0.253330 11.00000 -1.50000 H11B 2 0.854168 0.474241 0.205257 11.00000 -1.50000 H11C 2 0.734911 0.546508 0.202530 11.00000 -1.50000 AFIX 0 C14 1 1.146536 0.754559 0.322237 11.00000 0.02672 0.03529 = 0.06442 -0.01283 0.01158 -0.00873 AFIX 137 H14A 2 1.109898 0.805724 0.293409 11.00000 -1.50000 H14B 2 1.224684 0.729005 0.308797 11.00000 -1.50000 H14C 2 1.171467 0.778306 0.366254 11.00000 -1.50000 AFIX 0 C17 1 0.774443 0.740408 0.459530 11.00000 0.02241 0.02122 = 0.01590 -0.00080 0.00337 0.00051 C18 1 0.877719 0.801168 0.450835 11.00000 0.02207 0.02262 = 0.01632 -0.00458 0.00071 -0.00074 C22 1 0.785421 0.661744 0.506966 11.00000 0.03700 0.02675 = 0.02697 0.00901 0.00677 0.00461 AFIX 137 H22A 2 0.730743 0.609141 0.487612 11.00000 -1.50000 H22B 2 0.754985 0.683060 0.545337 11.00000 -1.50000 H22C 2 0.877713 0.641608 0.518956 11.00000 -1.50000 AFIX 0 C7 1 0.929825 0.551868 0.345868 11.00000 0.02610 0.01893 = 0.03139 0.00715 0.00870 0.01078 C23 1 1.013498 0.805569 0.492728 11.00000 0.02324 0.04074 = 0.02964 -0.01027 -0.00298 -0.00120 AFIX 137 H23A 2 1.033557 0.745851 0.515239 11.00000 -1.50000 H23B 2 1.016599 0.856075 0.524179 11.00000 -1.50000 H23C 2 1.078745 0.817645 0.466041 11.00000 -1.50000 AFIX 0 C13 1 1.120854 0.611403 0.435329 11.00000 0.04356 0.05445 = 0.03086 -0.00928 -0.01030 0.02709 AFIX 137 H13A 2 1.169839 0.670110 0.444941 11.00000 -1.50000 H13B 2 1.183089 0.559821 0.434779 11.00000 -1.50000 H13C 2 1.068958 0.599516 0.468338 11.00000 -1.50000 AFIX 0 C24 1 0.898950 0.954864 0.388382 11.00000 0.04669 0.02374 = 0.03801 -0.00672 0.01449 -0.00965 AFIX 137 H24A 2 0.978249 0.933821 0.373814 11.00000 -1.50000 H24B 2 0.924634 0.994567 0.426430 11.00000 -1.50000 H24C 2 0.842800 0.990690 0.354096 11.00000 -1.50000 AFIX 0 C26 1 0.704008 0.559331 0.039026 11.00000 0.16266 0.04285 = 0.08809 0.01655 0.10104 0.01809 PART 1 AFIX 23 H26C 2 0.686337 0.580412 -0.006252 10.50000 -1.20000 H26D 2 0.798002 0.573128 0.057020 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.671998 0.567877 -0.007723 10.50000 -1.20000 H26B 2 0.796834 0.580936 0.049608 10.50000 -1.20000 AFIX 0 CL1B 3 0.699648 0.442752 0.056573 10.50000 0.06392 0.03634 = 0.04326 0.01108 0.02195 0.01364 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0708, GooF = S = 1.028, Restrained GooF = 1.028 for all data REM R1 = 0.0297 for 7303 Fo > 4sig(Fo) and 0.0396 for all 8758 data REM 317 parameters refined using 6 restraints END WGHT 0.0308 2.2862 REM Highest difference peak 1.163, deepest hole -1.284, 1-sigma level 0.179 Q1 1 0.9044 0.8988 0.1985 11.00000 0.05 0.96 Q2 1 0.9052 0.7428 0.3403 11.00000 0.05 0.91 Q3 1 0.7287 0.5639 0.0588 11.00000 0.05 0.86 Q4 1 1.0990 0.7176 0.1890 11.00000 0.05 0.82 Q5 1 0.3942 0.9607 0.0802 11.00000 0.05 0.81 Q6 1 0.2876 0.7433 0.1593 11.00000 0.05 0.80 Q7 1 1.0816 0.6149 0.3982 11.00000 0.05 0.79 Q8 1 0.7185 0.6766 0.3426 11.00000 0.05 0.78 Q9 1 0.7778 0.4658 0.0528 11.00000 0.05 0.76 Q10 1 0.4874 0.7983 0.4395 11.00000 0.05 0.75 Q11 1 0.9048 0.7185 0.2979 11.00000 0.05 0.74 Q12 1 0.8448 0.5606 0.2991 11.00000 0.05 0.68 Q13 1 0.6722 0.4362 0.3984 11.00000 0.05 0.67 Q14 1 1.2441 0.7055 0.5009 11.00000 0.05 0.67 ; _shelx_res_checksum 20151 _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 2.504 _oxdiff_exptl_absorpt_empirical_full_min 0.682 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 0.80514(2) 0.71359(2) 0.33961(2) 0.01556(5) Uani 1 1 d . . . . . I1 I 0.52569(2) 0.61311(2) 0.28270(2) 0.02166(6) Uani 1 1 d . . . . . I4 I 0.81980(2) 0.93970(2) 0.20110(2) 0.02500(6) Uani 1 1 d . . . . . I3 I 0.48201(2) 0.93492(2) 0.08139(2) 0.02532(6) Uani 1 1 d . . . . . I2 I 0.29149(3) 0.71820(2) 0.13130(2) 0.03407(7) Uani 1 1 d . . . . . Cl2 Cl 0.61003(12) 0.62911(8) 0.07970(6) 0.0422(3) Uani 1 1 d . . . . . Cl1A Cl 0.6869(10) 0.4453(6) 0.0384(4) 0.091(3) Uani 0.5 1 d . U P A 1 N1 N 0.6768(3) 0.77290(19) 0.24233(14) 0.0182(6) Uani 1 1 d . . . . . C5 C 0.6683(3) 0.8442(2) 0.19874(17) 0.0185(7) Uani 1 1 d . . . . . C2 C 0.5599(3) 0.7267(2) 0.22640(18) 0.0190(7) Uani 1 1 d . . . . . C10 C 0.9583(3) 0.6480(2) 0.26330(17) 0.0199(7) Uani 1 1 d . . . . . C6 C 0.8874(3) 0.5692(2) 0.27924(18) 0.0199(7) Uani 1 1 d . . . . . C8 C 1.0298(4) 0.6187(3) 0.3707(2) 0.0255(8) Uani 1 1 d . . . . . C21 C 0.5189(4) 0.7400(3) 0.4239(2) 0.0293(8) Uani 1 1 d . . . . . H21A H 0.456254 0.759409 0.385115 0.044 Uiso 1 1 calc R U . . . H21B H 0.492491 0.767004 0.461745 0.044 Uiso 1 1 calc R U . . . H21C H 0.519268 0.671593 0.427065 0.044 Uiso 1 1 calc R U . . . C20 C 0.6861(4) 0.8540(2) 0.38644(18) 0.0230(7) Uani 1 1 d . . . . . C19 C 0.8231(4) 0.8703(2) 0.40516(18) 0.0231(7) Uani 1 1 d . . . . . C4 C 0.5476(3) 0.8427(2) 0.15620(17) 0.0197(7) Uani 1 1 d . . . . . C9 C 1.0448(3) 0.6790(3) 0.31956(19) 0.0232(7) Uani 1 1 d . . . . . C3 C 0.4760(3) 0.7662(2) 0.17421(18) 0.0208(7) Uani 1 1 d . . . . . C16 C 0.6554(3) 0.7739(2) 0.42024(18) 0.0192(7) Uani 1 1 d . . . . . C25 C 0.5869(4) 0.9159(3) 0.3438(2) 0.0331(9) Uani 1 1 d . . . . . H25A H 0.630695 0.950057 0.313971 0.050 Uiso 1 1 calc R U . . . H25B H 0.549633 0.960523 0.370284 0.050 Uiso 1 1 calc R U . . . H25C H 0.515915 0.877155 0.319364 0.050 Uiso 1 1 calc R U . . . C15 C 0.9524(5) 0.6837(3) 0.1965(2) 0.0345(9) Uani 1 1 d . . . . . H15A H 0.860014 0.691501 0.174911 0.052 Uiso 1 1 calc R U . . . H15B H 0.995564 0.638786 0.172609 0.052 Uiso 1 1 calc R U . . . H15C H 0.997924 0.744090 0.198438 0.052 Uiso 1 1 calc R U . . . C12 C 0.8881(5) 0.4714(3) 0.3824(3) 0.0402(11) Uani 1 1 d . . . . . H12A H 0.882274 0.492170 0.425691 0.060 Uiso 1 1 calc R U . . . H12B H 0.953052 0.420882 0.385344 0.060 Uiso 1 1 calc R U . . . H12C H 0.801563 0.448679 0.360071 0.060 Uiso 1 1 calc R U . . . C11 C 0.8001(4) 0.5077(3) 0.2309(2) 0.0352(10) Uani 1 1 d . . . . . H11A H 0.754359 0.462490 0.253330 0.053 Uiso 1 1 calc R U . . . H11B H 0.854168 0.474241 0.205257 0.053 Uiso 1 1 calc R U . . . H11C H 0.734911 0.546508 0.202530 0.053 Uiso 1 1 calc R U . . . C14 C 1.1465(4) 0.7546(3) 0.3222(3) 0.0418(11) Uani 1 1 d . . . . . H14A H 1.109898 0.805724 0.293409 0.063 Uiso 1 1 calc R U . . . H14B H 1.224684 0.729005 0.308797 0.063 Uiso 1 1 calc R U . . . H14C H 1.171467 0.778306 0.366254 0.063 Uiso 1 1 calc R U . . . C17 C 0.7744(4) 0.7404(2) 0.45953(17) 0.0199(7) Uani 1 1 d . . . . . C18 C 0.8777(4) 0.8012(2) 0.45083(17) 0.0208(7) Uani 1 1 d . . . . . C22 C 0.7854(4) 0.6617(3) 0.5070(2) 0.0302(9) Uani 1 1 d . . . . . H22A H 0.730743 0.609141 0.487612 0.045 Uiso 1 1 calc R U . . . H22B H 0.754985 0.683060 0.545337 0.045 Uiso 1 1 calc R U . . . H22C H 0.877713 0.641608 0.518956 0.045 Uiso 1 1 calc R U . . . C7 C 0.9298(4) 0.5519(2) 0.3459(2) 0.0251(8) Uani 1 1 d . . . . . C23 C 1.0135(4) 0.8056(3) 0.4927(2) 0.0324(9) Uani 1 1 d . . . . . H23A H 1.033557 0.745851 0.515239 0.049 Uiso 1 1 calc R U . . . H23B H 1.016599 0.856075 0.524179 0.049 Uiso 1 1 calc R U . . . H23C H 1.078745 0.817645 0.466041 0.049 Uiso 1 1 calc R U . . . C13 C 1.1209(5) 0.6114(4) 0.4353(2) 0.0454(12) Uani 1 1 d . . . . . H13A H 1.169839 0.670110 0.444941 0.068 Uiso 1 1 calc R U . . . H13B H 1.183089 0.559821 0.434779 0.068 Uiso 1 1 calc R U . . . H13C H 1.068958 0.599516 0.468338 0.068 Uiso 1 1 calc R U . . . C24 C 0.8990(5) 0.9549(3) 0.3884(2) 0.0353(10) Uani 1 1 d . . . . . H24A H 0.978249 0.933821 0.373814 0.053 Uiso 1 1 calc R U . . . H24B H 0.924634 0.994567 0.426430 0.053 Uiso 1 1 calc R U . . . H24C H 0.842800 0.990690 0.354096 0.053 Uiso 1 1 calc R U . . . C26 C 0.7040(9) 0.5593(4) 0.0390(4) 0.087(3) Uani 1 1 d . . . . . H26C H 0.686337 0.580412 -0.006252 0.105 Uiso 0.5 1 calc R U P A 1 H26D H 0.798002 0.573128 0.057020 0.105 Uiso 0.5 1 calc R U P A 1 H26A H 0.671998 0.567877 -0.007723 0.105 Uiso 0.5 1 calc R U P A -1 H26B H 0.796834 0.580936 0.049608 0.105 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.6996(8) 0.4428(5) 0.0566(3) 0.0463(14) 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 0.01532(8) 0.01504(8) 0.01524(8) -0.00050(5) 0.00049(6) 0.00222(5) I1 0.02242(12) 0.01915(11) 0.02291(12) 0.00105(8) 0.00339(9) -0.00564(8) I4 0.02206(12) 0.02290(12) 0.02957(14) 0.00357(9) 0.00402(10) -0.00577(8) I3 0.02855(13) 0.02625(12) 0.02020(12) 0.00574(9) 0.00258(9) 0.00850(9) I2 0.01882(13) 0.03216(14) 0.04475(17) 0.00100(11) -0.00907(11) -0.00399(9) Cl2 0.0479(7) 0.0453(6) 0.0333(6) 0.0037(5) 0.0080(5) 0.0158(5) Cl1A 0.056(3) 0.040(3) 0.169(8) -0.026(4) 0.000(5) 0.000(2) N1 0.0155(14) 0.0192(14) 0.0187(15) 0.0007(11) 0.0008(11) -0.0023(10) C5 0.0194(17) 0.0167(15) 0.0188(17) 0.0006(13) 0.0025(13) -0.0013(12) C2 0.0168(17) 0.0185(16) 0.0220(18) -0.0007(13) 0.0048(13) -0.0029(12) C10 0.0204(17) 0.0179(16) 0.0220(18) 0.0000(13) 0.0054(14) 0.0031(12) C6 0.0196(17) 0.0142(15) 0.0252(19) -0.0049(13) 0.0033(14) 0.0009(12) C8 0.0201(18) 0.0243(18) 0.030(2) -0.0052(15) -0.0005(15) 0.0111(14) C21 0.0196(19) 0.038(2) 0.030(2) -0.0078(17) 0.0059(16) -0.0014(15) C20 0.030(2) 0.0194(17) 0.0196(18) -0.0014(14) 0.0048(15) 0.0075(14) C19 0.0282(19) 0.0197(17) 0.0224(19) -0.0017(14) 0.0074(15) 0.0018(14) C4 0.0195(17) 0.0182(16) 0.0207(17) 0.0042(13) 0.0023(13) 0.0029(12) C9 0.0130(16) 0.0240(18) 0.032(2) -0.0082(15) 0.0039(14) 0.0010(13) C3 0.0184(17) 0.0216(16) 0.0213(18) -0.0004(14) 0.0015(13) -0.0009(13) C16 0.0187(17) 0.0183(16) 0.0202(17) -0.0028(13) 0.0031(13) 0.0034(12) C25 0.038(2) 0.034(2) 0.026(2) 0.0005(17) 0.0029(17) 0.0194(17) C15 0.040(2) 0.038(2) 0.028(2) 0.0048(18) 0.0140(18) 0.0106(18) C12 0.046(3) 0.029(2) 0.050(3) 0.019(2) 0.020(2) 0.0140(19) C11 0.026(2) 0.033(2) 0.045(3) -0.0184(19) 0.0023(18) -0.0006(16) C14 0.027(2) 0.035(2) 0.064(3) -0.013(2) 0.012(2) -0.0087(17) C17 0.0224(18) 0.0212(17) 0.0159(16) -0.0008(13) 0.0034(13) 0.0005(13) C18 0.0221(18) 0.0226(17) 0.0163(17) -0.0046(13) 0.0007(13) -0.0007(13) C22 0.037(2) 0.0268(19) 0.027(2) 0.0090(16) 0.0068(17) 0.0046(16) C7 0.026(2) 0.0189(17) 0.031(2) 0.0072(15) 0.0087(16) 0.0108(14) C23 0.023(2) 0.041(2) 0.030(2) -0.0103(18) -0.0030(16) -0.0012(16) C13 0.044(3) 0.054(3) 0.031(2) -0.009(2) -0.010(2) 0.027(2) C24 0.047(3) 0.0237(19) 0.038(3) -0.0067(17) 0.014(2) -0.0097(17) C26 0.163(8) 0.043(3) 0.088(5) 0.017(3) 0.101(6) 0.018(4) Cl1B 0.064(4) 0.036(2) 0.0433(16) 0.0111(15) 0.0219(19) 0.0136(19) 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 62.12(7) . . ? N1 Dy1 C10 83.77(10) . . ? N1 Dy1 C6 91.91(11) . . ? N1 Dy1 C8 134.92(11) . . ? N1 Dy1 C20 80.60(11) . . ? N1 Dy1 C19 97.20(11) . . ? N1 Dy1 C9 107.69(11) . . ? N1 Dy1 C16 98.56(10) . . ? N1 Dy1 C17 128.99(11) . . ? N1 Dy1 C18 128.09(10) . . ? N1 Dy1 C7 122.55(11) . . ? C10 Dy1 I1 102.24(8) . . ? C10 Dy1 C6 31.02(11) . . ? C10 Dy1 C8 51.18(12) . . ? C10 Dy1 C16 177.48(11) . . ? C10 Dy1 C17 146.86(11) . . ? C6 Dy1 I1 79.82(8) . . ? C6 Dy1 C16 147.43(11) . . ? C6 Dy1 C17 133.33(11) . . ? C8 Dy1 I1 122.48(8) . . ? C8 Dy1 C6 51.35(11) . . ? C8 Dy1 C16 126.52(12) . . ? C8 Dy1 C17 95.83(12) . . ? C20 Dy1 I1 91.69(9) . . ? C20 Dy1 C10 151.13(11) . . ? C20 Dy1 C6 170.67(11) . . ? C20 Dy1 C8 137.88(12) . . ? C20 Dy1 C16 30.96(11) . . ? C20 Dy1 C17 51.46(11) . . ? C19 Dy1 I1 122.69(8) . . ? C19 Dy1 C10 129.67(11) . . ? C19 Dy1 C6 157.41(11) . . ? C19 Dy1 C8 109.77(12) . . ? C19 Dy1 C20 31.04(12) . . ? C19 Dy1 C9 106.04(11) . . ? C19 Dy1 C16 51.15(11) . . ? C19 Dy1 C17 51.49(11) . . ? C19 Dy1 C18 31.25(11) . . ? C19 Dy1 C7 137.68(13) . . ? C9 Dy1 I1 130.70(8) . . ? C9 Dy1 C10 30.94(11) . . ? C9 Dy1 C6 51.39(11) . . ? C9 Dy1 C8 31.10(13) . . ? C9 Dy1 C20 136.30(12) . . ? C9 Dy1 C16 147.78(11) . . ? C9 Dy1 C17 118.53(12) . . ? C9 Dy1 C18 97.22(11) . . ? C16 Dy1 I1 78.13(8) . . ? C17 Dy1 I1 98.80(8) . . ? C17 Dy1 C16 30.98(11) . . ? C18 Dy1 I1 127.98(8) . . ? C18 Dy1 C10 128.02(11) . . ? C18 Dy1 C6 137.52(11) . . ? C18 Dy1 C8 86.68(12) . . ? C18 Dy1 C20 51.41(12) . . ? C18 Dy1 C16 51.06(11) . . ? C18 Dy1 C17 30.97(11) . . ? C7 Dy1 I1 91.18(9) . . ? C7 Dy1 C10 51.38(11) . . ? C7 Dy1 C6 31.07(12) . . ? C7 Dy1 C8 31.31(12) . . ? C7 Dy1 C20 154.68(12) . . ? C7 Dy1 C9 51.67(12) . . ? C7 Dy1 C16 126.20(11) . . ? C7 Dy1 C17 103.25(12) . . ? C7 Dy1 C18 108.75(12) . . ? C2 I1 Dy1 68.18(10) . . ? C5 N1 Dy1 143.4(2) . . ? C2 N1 Dy1 110.9(2) . . ? C2 N1 C5 105.1(3) . . ? N1 C5 I4 121.9(2) . . ? N1 C5 C4 110.9(3) . . ? C4 C5 I4 127.1(3) . . ? N1 C2 I1 118.6(3) . . ? N1 C2 C3 112.6(3) . . ? C3 C2 I1 128.7(3) . . ? C6 C10 Dy1 74.6(2) . . ? C6 C10 C15 124.8(4) . . ? C9 C10 Dy1 74.1(2) . . ? C9 C10 C6 108.4(3) . . ? C9 C10 C15 126.4(4) . . ? C15 C10 Dy1 122.9(2) . . ? C10 C6 Dy1 74.37(19) . . ? C10 C6 C11 124.5(4) . . ? C11 C6 Dy1 125.2(2) . . ? C7 C6 Dy1 73.63(19) . . ? C7 C6 C10 107.8(3) . . ? C7 C6 C11 127.0(3) . . ? C9 C8 Dy1 74.0(2) . . ? C9 C8 C7 107.7(3) . . ? C9 C8 C13 126.6(4) . . ? C7 C8 Dy1 73.6(2) . . ? C7 C8 C13 124.4(4) . . ? C13 C8 Dy1 128.2(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 73.5(2) . . ? C19 C20 C16 107.7(3) . . ? C19 C20 C25 126.5(4) . . ? C16 C20 Dy1 75.41(19) . . ? C16 C20 C25 125.5(4) . . ? C25 C20 Dy1 121.9(3) . . ? C20 C19 Dy1 75.5(2) . . ? C20 C19 C18 108.5(3) . . ? C20 C19 C24 126.9(4) . . ? C18 C19 Dy1 75.3(2) . . ? C18 C19 C24 124.1(4) . . ? C24 C19 Dy1 122.6(3) . . ? C5 C4 I3 127.1(3) . . ? C5 C4 C3 106.6(3) . . ? C3 C4 I3 126.2(3) . . ? C10 C9 Dy1 75.0(2) . . ? C10 C9 C8 108.0(3) . . ? C10 C9 C14 125.3(4) . . ? C8 C9 Dy1 74.9(2) . . ? C8 C9 C14 126.2(4) . . ? C14 C9 Dy1 122.1(3) . . ? C2 C3 I2 126.5(3) . . ? C2 C3 C4 104.7(3) . . ? C4 C3 I2 128.7(3) . . ? C21 C16 Dy1 126.7(2) . . ? C20 C16 Dy1 73.6(2) . . ? C20 C16 C21 126.2(3) . . ? C20 C16 C17 108.2(3) . . ? C17 C16 Dy1 73.98(19) . . ? C17 C16 C21 124.7(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 75.0(2) . . ? C16 C17 C22 125.9(3) . . ? C18 C17 Dy1 74.0(2) . . ? C18 C17 C16 107.6(3) . . ? C18 C17 C22 126.2(3) . . ? C22 C17 Dy1 122.0(2) . . ? C19 C18 Dy1 73.5(2) . . ? C19 C18 C23 124.8(3) . . ? C17 C18 Dy1 75.0(2) . . ? C17 C18 C19 108.0(3) . . ? C17 C18 C23 125.9(3) . . ? C23 C18 Dy1 127.7(3) . . ? 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 75.30(19) . . ? C6 C7 C8 108.0(3) . . ? C6 C7 C12 126.1(4) . . ? C8 C7 Dy1 75.1(2) . . ? C8 C7 C12 125.7(4) . . ? C12 C7 Dy1 120.6(3) . . ? 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 108.7 . . ? Cl2 C26 H26B 108.7 . . ? Cl1A C26 Cl2 120.3(5) . . ? Cl1A C26 H26C 107.3 . . ? Cl1A C26 H26D 107.3 . . ? Cl1A C26 H26A 95.8 . . ? Cl1A C26 H26B 114.2 . . ? Cl1A C26 Cl1B 12.9(5) . . ? H26C C26 H26D 106.9 . . ? H26C C26 H26A 13.4 . . ? H26C C26 H26B 96.2 . . ? H26D C26 H26A 117.9 . . ? H26D C26 H26B 11.1 . . ? H26A C26 H26B 107.6 . . ? Cl1B C26 Cl2 114.1(4) . . ? Cl1B C26 H26C 120.1 . . ? Cl1B C26 H26D 100.2 . . ? Cl1B C26 H26A 108.7 . . ? Cl1B C26 H26B 108.7 . . ? 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 3.2354(3) . ? Dy1 N1 2.378(3) . ? Dy1 C10 2.655(3) . ? Dy1 C6 2.658(3) . ? Dy1 C8 2.655(3) . ? Dy1 C20 2.650(3) . ? Dy1 C19 2.624(4) . ? Dy1 C9 2.644(3) . ? Dy1 C16 2.673(3) . ? Dy1 C17 2.659(4) . ? Dy1 C18 2.647(4) . ? Dy1 C7 2.636(3) . ? I1 C2 2.089(3) . ? I4 C5 2.071(3) . ? I3 C4 2.072(3) . ? I2 C3 2.059(4) . ? Cl2 C26 1.739(5) . ? Cl1A C26 1.639(10) . ? N1 C5 1.368(4) . ? N1 C2 1.359(4) . ? C5 C4 1.387(5) . ? C2 C3 1.384(5) . ? C10 C6 1.420(5) . ? C10 C9 1.414(5) . ? C10 C15 1.498(5) . ? C6 C11 1.507(5) . ? C6 C7 1.418(6) . ? C8 C9 1.421(6) . ? C8 C7 1.428(6) . ? C8 C13 1.505(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C16 1.508(5) . ? C20 C19 1.412(5) . ? C20 C16 1.421(5) . ? C20 C25 1.511(5) . ? C19 C18 1.420(5) . ? C19 C24 1.521(5) . ? C4 C3 1.415(5) . ? C9 C14 1.500(5) . ? C16 C17 1.424(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 1.498(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 1.417(5) . ? C17 C22 1.499(5) . ? C18 C23 1.505(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 1.710(9) . ? 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 9.5(5) . . . . ? Dy1 N1 C5 C4 -169.4(3) . . . . ? Dy1 N1 C2 I1 -4.8(3) . . . . ? Dy1 N1 C2 C3 173.0(2) . . . . ? Dy1 C10 C6 C11 122.2(3) . . . . ? Dy1 C10 C6 C7 -66.6(2) . . . . ? Dy1 C10 C9 C8 68.2(2) . . . . ? Dy1 C10 C9 C14 -119.0(4) . . . . ? Dy1 C6 C7 C8 -68.6(2) . . . . ? Dy1 C6 C7 C12 117.4(4) . . . . ? Dy1 C8 C9 C10 -68.2(2) . . . . ? Dy1 C8 C9 C14 119.0(4) . . . . ? Dy1 C8 C7 C6 68.7(2) . . . . ? Dy1 C8 C7 C12 -117.3(4) . . . . ? Dy1 C20 C19 C18 -68.7(2) . . . . ? Dy1 C20 C19 C24 120.1(4) . . . . ? Dy1 C20 C16 C21 -123.8(4) . . . . ? Dy1 C20 C16 C17 66.5(2) . . . . ? Dy1 C19 C18 C17 -67.6(2) . . . . ? Dy1 C19 C18 C23 124.8(4) . . . . ? Dy1 C16 C17 C18 67.5(2) . . . . ? Dy1 C16 C17 C22 -118.9(4) . . . . ? Dy1 C17 C18 C19 66.6(2) . . . . ? Dy1 C17 C18 C23 -126.0(4) . . . . ? I1 C2 C3 I2 -4.5(5) . . . . ? I1 C2 C3 C4 177.9(3) . . . . ? I4 C5 C4 I3 0.5(5) . . . . ? I4 C5 C4 C3 -178.7(3) . . . . ? I3 C4 C3 I2 2.9(5) . . . . ? I3 C4 C3 C2 -179.6(3) . . . . ? N1 C5 C4 I3 179.4(2) . . . . ? N1 C5 C4 C3 0.1(4) . . . . ? N1 C2 C3 I2 178.0(2) . . . . ? N1 C2 C3 C4 0.4(4) . . . . ? C5 N1 C2 I1 -178.1(2) . . . . ? C5 N1 C2 C3 -0.4(4) . . . . ? C5 C4 C3 I2 -177.9(3) . . . . ? C5 C4 C3 C2 -0.3(4) . . . . ? C2 N1 C5 I4 179.0(2) . . . . ? C2 N1 C5 C4 0.1(4) . . . . ? C10 C6 C7 Dy1 67.1(2) . . . . ? C10 C6 C7 C8 -1.5(4) . . . . ? C10 C6 C7 C12 -175.5(3) . . . . ? C6 C10 C9 Dy1 -67.3(2) . . . . ? C6 C10 C9 C8 0.9(4) . . . . ? C6 C10 C9 C14 173.7(3) . . . . ? C21 C16 C17 Dy1 123.9(3) . . . . ? C21 C16 C17 C18 -168.7(3) . . . . ? C21 C16 C17 C22 5.0(6) . . . . ? C20 C19 C18 Dy1 68.9(3) . . . . ? C20 C19 C18 C17 1.2(4) . . . . ? C20 C19 C18 C23 -166.3(3) . . . . ? C20 C16 C17 Dy1 -66.2(2) . . . . ? C20 C16 C17 C18 1.2(4) . . . . ? C20 C16 C17 C22 174.9(3) . . . . ? C19 C20 C16 Dy1 -66.9(3) . . . . ? C19 C20 C16 C21 169.2(3) . . . . ? C19 C20 C16 C17 -0.5(4) . . . . ? C9 C10 C6 Dy1 67.0(2) . . . . ? C9 C10 C6 C11 -170.8(3) . . . . ? C9 C10 C6 C7 0.4(4) . . . . ? C9 C8 C7 Dy1 -66.7(2) . . . . ? C9 C8 C7 C6 2.0(4) . . . . ? C9 C8 C7 C12 176.0(3) . . . . ? C16 C20 C19 Dy1 68.3(2) . . . . ? C16 C20 C19 C18 -0.5(4) . . . . ? C16 C20 C19 C24 -171.7(4) . . . . ? C16 C17 C18 Dy1 -68.1(2) . . . . ? C16 C17 C18 C19 -1.5(4) . . . . ? C16 C17 C18 C23 165.9(3) . . . . ? C25 C20 C19 Dy1 -117.7(4) . . . . ? C25 C20 C19 C18 173.6(3) . . . . ? C25 C20 C19 C24 2.3(6) . . . . ? C25 C20 C16 Dy1 119.0(4) . . . . ? C25 C20 C16 C21 -4.8(6) . . . . ? C25 C20 C16 C17 -174.6(3) . . . . ? C15 C10 C6 Dy1 -119.7(3) . . . . ? C15 C10 C6 C11 2.6(6) . . . . ? C15 C10 C6 C7 173.7(3) . . . . ? C15 C10 C9 Dy1 119.5(4) . . . . ? C15 C10 C9 C8 -172.3(3) . . . . ? C15 C10 C9 C14 0.5(6) . . . . ? C11 C6 C7 Dy1 -122.0(4) . . . . ? C11 C6 C7 C8 169.4(3) . . . . ? C11 C6 C7 C12 -4.6(6) . . . . ? C22 C17 C18 Dy1 118.2(4) . . . . ? C22 C17 C18 C19 -175.2(3) . . . . ? C22 C17 C18 C23 -7.8(6) . . . . ? C7 C8 C9 Dy1 66.4(2) . . . . ? C7 C8 C9 C10 -1.8(4) . . . . ? C7 C8 C9 C14 -174.5(4) . . . . ? C13 C8 C9 Dy1 -126.1(4) . . . . ? C13 C8 C9 C10 165.7(4) . . . . ? C13 C8 C9 C14 -7.0(6) . . . . ? C13 C8 C7 Dy1 125.4(4) . . . . ? C13 C8 C7 C6 -165.8(4) . . . . ? C13 C8 C7 C12 8.2(6) . . . . ? C24 C19 C18 Dy1 -119.6(4) . . . . ? C24 C19 C18 C17 172.7(3) . . . . ? C24 C19 C18 C23 5.2(6) . . . . ? 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 1.0036 -1.0032 -0.0273 -0.0783 -0.0142 0.0325 1.0026 1.0036 -0.0070 0.0038 0.0040 0.0859 -1.0036 1.0032 0.0273 0.0783 0.0142 -0.0325 -1.0026 -1.0036 0.0070 -0.0038 -0.0040 -0.0859 0.0028 -0.0050 0.9988 -0.0100 0.0322 0.0044 -0.0028 0.0050 -0.9988 0.0100 -0.0322 -0.0044 0.9970 1.0136 -2.0046 0.0239 -0.0605 0.0770 -0.9970 -1.0136 2.0046 -0.0239 0.0605 -0.0770 -1.0054 -0.9986 -0.9918 0.0063 -0.0363 -0.0903 -0.0061 1.0134 -1.9875 0.0612 -0.0554 0.0178 -2.0085 -0.9988 -0.9747 0.0435 -0.0312 -0.1495 0.0051 0.9934 2.0077 0.0210 0.0736 0.0356 1.0087 -0.0098 1.9805 -0.0574 0.0594 0.0681 0.9975 0.0102 -2.0147 -0.0172 -0.0696 0.0503 5.8316 7.1798 22.3776 -0.1415 0.7602 0.6341