#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:50:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294477 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572195.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_1572195 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 101.960(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3816(2) _cell_length_b 14.3751(3) _cell_length_c 21.3967(5) _cell_measurement_reflns_used 18199 _cell_measurement_temperature 230.0(1) _cell_measurement_theta_max 30.8400 _cell_measurement_theta_min 2.8520 _cell_volume 3123.85(12) _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 230.0(1) _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 0.847 _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 0.0365683000 _diffrn_orient_matrix_UB_12 0.0414832000 _diffrn_orient_matrix_UB_13 0.0082094000 _diffrn_orient_matrix_UB_21 0.0023603000 _diffrn_orient_matrix_UB_22 0.0069087000 _diffrn_orient_matrix_UB_23 -0.0325676000 _diffrn_orient_matrix_UB_31 -0.0594628000 _diffrn_orient_matrix_UB_32 0.0257956000 _diffrn_orient_matrix_UB_33 -0.0044812000 _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 0.0572 _diffrn_reflns_av_unetI/netI 0.0480 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.847 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _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 39034 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.847 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.617 _diffrn_reflns_theta_min 2.455 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.531 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.232 _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 2.312 _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 1.119 _refine_diff_density_min -1.272 _refine_diff_density_rms 0.158 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8896 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0339 _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^)+(0.0329P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.0802 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6954 _reflns_number_total 8896 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP230K _cod_depositor_comments 'Adding full bibliography for 1572175--1572199.cif.' _cod_original_cell_volume 3123.84(13) _cod_database_code 1572195 _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 0.531 _shelx_estimated_absorpt_t_min 0.206 _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_230_final.res created by SHELXL-2018/3 at 16:43:51 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 10.381569 14.375078 21.396731 90 101.9602 90 ZERR 4 0.000239 0.000319 0.000523 0 0.0023 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. 50 0 0 PLAN 16 SIZE 0.111 0.275 0.353 TEMP -43.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.032900 FVAR 0.60421 DY1 4 0.804049 0.715626 0.339017 11.00000 0.02422 0.02497 = 0.02431 -0.00032 0.00109 0.00317 I1 5 0.524120 0.616806 0.280262 11.00000 0.03800 0.03287 = 0.03878 0.00221 0.00632 -0.01055 I4 5 0.821824 0.939609 0.200464 11.00000 0.03793 0.04016 = 0.04917 0.00656 0.00772 -0.01116 I3 5 0.485658 0.938019 0.081975 11.00000 0.04938 0.04549 = 0.03321 0.01050 0.00534 0.01540 I2 5 0.293181 0.723246 0.129634 11.00000 0.03149 0.05522 = 0.07272 -0.00045 -0.01480 -0.00632 CL2 3 0.608656 0.626946 0.079130 11.00000 0.08748 0.07809 = 0.05730 0.00619 0.01441 0.02803 PART 1 CL1A 3 0.694430 0.443856 0.038183 10.50000 0.09183 0.08565 = 0.22944 -0.04903 0.04055 0.00074 PART 0 N1 6 0.678033 0.774366 0.241305 11.00000 0.02784 0.03178 = 0.02670 0.00106 0.00436 -0.00132 C5 1 0.669175 0.845729 0.198006 11.00000 0.02556 0.02985 = 0.02858 0.00190 0.00465 -0.00012 C2 1 0.560526 0.729423 0.224878 11.00000 0.02552 0.02943 = 0.03233 0.00038 0.00480 -0.00452 C10 1 0.957368 0.648493 0.264707 11.00000 0.03651 0.03503 = 0.03211 0.00497 0.01042 0.01179 C6 1 0.887829 0.571609 0.280874 11.00000 0.03194 0.02944 = 0.04385 -0.00854 0.00632 0.00838 C8 1 1.027623 0.621485 0.371803 11.00000 0.03278 0.04212 = 0.04082 -0.00968 -0.00247 0.01701 C21 1 0.520555 0.737246 0.424329 11.00000 0.03696 0.07240 = 0.06021 -0.01997 0.01577 -0.00556 AFIX 137 H21A 2 0.457410 0.751691 0.385382 11.00000 -1.50000 H21B 2 0.493380 0.766566 0.460337 11.00000 -1.50000 H21C 2 0.524742 0.670391 0.430566 11.00000 -1.50000 AFIX 0 C20 1 0.680869 0.853126 0.385347 11.00000 0.04837 0.03124 = 0.02891 -0.00239 0.00485 0.01413 C19 1 0.817476 0.872108 0.403349 11.00000 0.05346 0.02577 = 0.03782 -0.00660 0.01402 -0.00304 C4 1 0.548888 0.845048 0.155291 11.00000 0.03329 0.02790 = 0.03048 0.00248 0.00501 0.00716 C9 1 1.042308 0.679905 0.320747 11.00000 0.02432 0.03470 = 0.05476 -0.00486 0.00988 0.00005 C3 1 0.478422 0.769140 0.173188 11.00000 0.02726 0.03260 = 0.02966 -0.00499 -0.00228 -0.00125 C16 1 0.655060 0.773303 0.419180 11.00000 0.03229 0.03569 = 0.02735 -0.00682 0.00940 0.00565 C25 1 0.579887 0.912271 0.342651 11.00000 0.07766 0.05892 = 0.04772 0.00617 0.00818 0.04458 AFIX 137 H25A 2 0.623049 0.951279 0.316191 11.00000 -1.50000 H25B 2 0.535358 0.951171 0.368594 11.00000 -1.50000 H25C 2 0.516088 0.872528 0.315615 11.00000 -1.50000 AFIX 0 C15 1 0.952550 0.681576 0.198022 11.00000 0.07112 0.07202 = 0.04420 0.00663 0.02499 0.02235 AFIX 137 H15A 2 0.861695 0.684201 0.175021 11.00000 -1.50000 H15B 2 1.001412 0.638910 0.176561 11.00000 -1.50000 H15C 2 0.991415 0.743081 0.199218 11.00000 -1.50000 AFIX 0 C12 1 0.887527 0.475198 0.383225 11.00000 0.08089 0.03779 = 0.09154 0.02471 0.03639 0.01814 AFIX 137 H12A 2 0.900543 0.491426 0.428101 11.00000 -1.50000 H12B 2 0.939836 0.420777 0.378389 11.00000 -1.50000 H12C 2 0.795185 0.461762 0.366691 11.00000 -1.50000 AFIX 0 C11 1 0.801178 0.508485 0.233803 11.00000 0.04507 0.05943 = 0.08269 -0.03559 0.00366 0.00480 AFIX 137 H11A 2 0.751106 0.468294 0.256358 11.00000 -1.50000 H11B 2 0.855465 0.470818 0.211861 11.00000 -1.50000 H11C 2 0.741195 0.545718 0.202896 11.00000 -1.50000 AFIX 0 C14 1 1.145255 0.755539 0.323670 11.00000 0.04562 0.05968 = 0.11574 -0.01121 0.02527 -0.01373 AFIX 137 H14A 2 1.124857 0.792829 0.285098 11.00000 -1.50000 H14B 2 1.231347 0.727320 0.327245 11.00000 -1.50000 H14C 2 1.145398 0.794839 0.360536 11.00000 -1.50000 AFIX 0 C17 1 0.774822 0.742811 0.458223 11.00000 0.04008 0.03423 = 0.02780 0.00029 0.00749 0.00581 C18 1 0.874351 0.804422 0.449211 11.00000 0.03683 0.03870 = 0.02567 -0.00695 0.00402 0.00172 C22 1 0.788962 0.665172 0.506697 11.00000 0.07130 0.05537 = 0.03756 0.01730 0.01439 0.01417 AFIX 137 H22A 2 0.707195 0.630480 0.500837 11.00000 -1.50000 H22B 2 0.809218 0.691228 0.549432 11.00000 -1.50000 H22C 2 0.859558 0.623932 0.500964 11.00000 -1.50000 AFIX 0 C7 1 0.929244 0.554923 0.346927 11.00000 0.03987 0.02916 = 0.04766 0.00834 0.01553 0.01213 C23 1 1.010546 0.811631 0.490740 11.00000 0.04301 0.07378 = 0.05647 -0.02678 -0.00146 -0.00522 AFIX 137 H23A 2 1.033987 0.752883 0.512425 11.00000 -1.50000 H23B 2 1.011751 0.860493 0.522122 11.00000 -1.50000 H23C 2 1.073415 0.826150 0.464358 11.00000 -1.50000 AFIX 0 C13 1 1.118703 0.614888 0.436149 11.00000 0.06249 0.09563 = 0.04795 -0.01704 -0.01930 0.04061 AFIX 137 H13A 2 1.165173 0.673347 0.445931 11.00000 -1.50000 H13B 2 1.181744 0.565244 0.435603 11.00000 -1.50000 H13C 2 1.067971 0.601814 0.468440 11.00000 -1.50000 AFIX 0 C24 1 0.888247 0.957083 0.386373 11.00000 0.09685 0.04052 = 0.06590 -0.00714 0.03294 -0.02357 AFIX 137 H24A 2 0.966565 0.938101 0.371651 11.00000 -1.50000 H24B 2 0.913192 0.996399 0.423771 11.00000 -1.50000 H24C 2 0.830502 0.991403 0.352777 11.00000 -1.50000 AFIX 0 C26 1 0.697300 0.559038 0.037327 11.00000 0.20463 0.06484 = 0.10137 0.02071 0.10872 0.01830 PART 1 AFIX 23 H26C 2 0.670973 0.577779 -0.007547 10.50000 -1.20000 H26D 2 0.789701 0.577338 0.051412 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.658428 0.564359 -0.008349 10.50000 -1.20000 H26B 2 0.787443 0.583119 0.044090 10.50000 -1.20000 AFIX 0 CL1B 3 0.703083 0.447443 0.057592 10.50000 0.11437 0.05618 = 0.06761 0.01629 0.02785 0.03132 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0802, GooF = S = 1.055, Restrained GooF = 1.055 for all data REM R1 = 0.0339 for 6954 Fo > 4sig(Fo) and 0.0486 for all 8896 data REM 317 parameters refined using 6 restraints END WGHT 0.0329 0.0000 REM Highest difference peak 1.119, deepest hole -1.272, 1-sigma level 0.158 Q1 1 0.7682 0.4822 0.0436 11.00000 0.05 1.12 Q2 1 0.2852 0.7472 0.1600 11.00000 0.05 1.01 Q3 1 0.4770 0.8849 0.0785 11.00000 0.05 0.83 Q4 1 0.4673 0.9003 0.0653 11.00000 0.05 0.74 Q5 1 0.8766 0.7589 0.3391 11.00000 0.05 0.71 Q6 1 0.6989 0.7368 0.3410 11.00000 0.05 0.66 Q7 1 0.3824 0.9065 0.0815 11.00000 0.05 0.65 Q8 1 0.5590 0.9474 0.0840 11.00000 0.05 0.64 Q9 1 0.7036 0.6773 0.3397 11.00000 0.05 0.60 Q10 1 0.9356 0.7148 0.2854 11.00000 0.05 0.59 Q11 1 0.6847 0.7328 0.3806 11.00000 0.05 0.58 Q12 1 0.8029 0.8410 0.3422 11.00000 0.05 0.57 Q13 1 0.9187 0.9732 0.2021 11.00000 0.05 0.55 Q14 1 0.3286 0.7477 0.1012 11.00000 0.05 0.55 Q15 1 0.7819 0.6039 0.3358 11.00000 0.05 0.54 Q16 1 0.7865 0.7835 0.3387 11.00000 0.05 0.52 ; _shelx_res_checksum 21818 _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 2.688 _oxdiff_exptl_absorpt_empirical_full_min 0.602 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 0.80405(2) 0.71563(2) 0.33902(2) 0.02507(6) Uani 1 1 d . . . . . I1 I 0.52412(3) 0.61681(2) 0.28026(2) 0.03679(7) Uani 1 1 d . . . . . I4 I 0.82182(3) 0.93961(2) 0.20046(2) 0.04261(8) Uani 1 1 d . . . . . I3 I 0.48566(3) 0.93802(2) 0.08198(2) 0.04315(8) Uani 1 1 d . . . . . I2 I 0.29318(3) 0.72325(2) 0.12963(2) 0.05684(10) Uani 1 1 d . . . . . Cl2 Cl 0.60866(17) 0.62695(11) 0.07913(8) 0.0744(4) Uani 1 1 d . . . . . Cl1A Cl 0.6944(12) 0.4439(8) 0.0382(6) 0.135(4) Uani 0.5 1 d . U P A 1 N1 N 0.6780(3) 0.7744(2) 0.24130(16) 0.0290(7) Uani 1 1 d . . . . . C5 C 0.6692(4) 0.8457(3) 0.19801(19) 0.0281(7) Uani 1 1 d . . . . . C2 C 0.5605(4) 0.7294(3) 0.22488(19) 0.0293(8) Uani 1 1 d . . . . . C10 C 0.9574(4) 0.6485(3) 0.2647(2) 0.0341(9) Uani 1 1 d . . . . . C6 C 0.8878(4) 0.5716(3) 0.2809(2) 0.0353(9) Uani 1 1 d . . . . . C8 C 1.0276(4) 0.6215(3) 0.3718(2) 0.0400(10) Uani 1 1 d . . . . . C21 C 0.5206(5) 0.7372(4) 0.4243(3) 0.0557(14) Uani 1 1 d . . . . . H21A H 0.457410 0.751691 0.385382 0.084 Uiso 1 1 calc R U . . . H21B H 0.493380 0.766566 0.460337 0.084 Uiso 1 1 calc R U . . . H21C H 0.524742 0.670391 0.430566 0.084 Uiso 1 1 calc R U . . . C20 C 0.6809(4) 0.8531(3) 0.3853(2) 0.0366(9) Uani 1 1 d . . . . . C19 C 0.8175(5) 0.8721(3) 0.4033(2) 0.0384(10) Uani 1 1 d . . . . . C4 C 0.5489(4) 0.8450(3) 0.1553(2) 0.0308(8) Uani 1 1 d . . . . . C9 C 1.0423(4) 0.6799(3) 0.3207(2) 0.0377(10) Uani 1 1 d . . . . . C3 C 0.4784(4) 0.7691(3) 0.1732(2) 0.0310(8) Uani 1 1 d . . . . . C16 C 0.6551(4) 0.7733(3) 0.4192(2) 0.0313(8) Uani 1 1 d . . . . . C25 C 0.5799(6) 0.9123(4) 0.3427(3) 0.0621(16) Uani 1 1 d . . . . . H25A H 0.623049 0.951279 0.316191 0.093 Uiso 1 1 calc R U . . . H25B H 0.535358 0.951171 0.368594 0.093 Uiso 1 1 calc R U . . . H25C H 0.516088 0.872528 0.315615 0.093 Uiso 1 1 calc R U . . . C15 C 0.9525(6) 0.6816(4) 0.1980(3) 0.0606(14) Uani 1 1 d . . . . . H15A H 0.861695 0.684201 0.175021 0.091 Uiso 1 1 calc R U . . . H15B H 1.001412 0.638910 0.176561 0.091 Uiso 1 1 calc R U . . . H15C H 0.991415 0.743081 0.199218 0.091 Uiso 1 1 calc R U . . . C12 C 0.8875(6) 0.4752(3) 0.3832(3) 0.0674(17) Uani 1 1 d . . . . . H12A H 0.900543 0.491426 0.428101 0.101 Uiso 1 1 calc R U . . . H12B H 0.939836 0.420777 0.378389 0.101 Uiso 1 1 calc R U . . . H12C H 0.795185 0.461762 0.366691 0.101 Uiso 1 1 calc R U . . . C11 C 0.8012(5) 0.5085(4) 0.2338(3) 0.0638(16) Uani 1 1 d . . . . . H11A H 0.751106 0.468294 0.256358 0.096 Uiso 1 1 calc R U . . . H11B H 0.855465 0.470818 0.211861 0.096 Uiso 1 1 calc R U . . . H11C H 0.741195 0.545718 0.202896 0.096 Uiso 1 1 calc R U . . . C14 C 1.1453(6) 0.7555(4) 0.3237(4) 0.0724(19) Uani 1 1 d . . . . . H14A H 1.124857 0.792829 0.285098 0.109 Uiso 1 1 calc R U . . . H14B H 1.231347 0.727320 0.327245 0.109 Uiso 1 1 calc R U . . . H14C H 1.145398 0.794839 0.360536 0.109 Uiso 1 1 calc R U . . . C17 C 0.7748(4) 0.7428(3) 0.4582(2) 0.0340(9) Uani 1 1 d . . . . . C18 C 0.8744(4) 0.8044(3) 0.4492(2) 0.0341(9) Uani 1 1 d . . . . . C22 C 0.7890(6) 0.6652(4) 0.5067(2) 0.0543(13) Uani 1 1 d . . . . . H22A H 0.707195 0.630480 0.500837 0.081 Uiso 1 1 calc R U . . . H22B H 0.809218 0.691228 0.549432 0.081 Uiso 1 1 calc R U . . . H22C H 0.859558 0.623932 0.500964 0.081 Uiso 1 1 calc R U . . . C7 C 0.9292(4) 0.5549(3) 0.3469(2) 0.0380(10) Uani 1 1 d . . . . . C23 C 1.0105(5) 0.8116(4) 0.4907(3) 0.0595(14) Uani 1 1 d . . . . . H23A H 1.033987 0.752883 0.512425 0.089 Uiso 1 1 calc R U . . . H23B H 1.011751 0.860493 0.522122 0.089 Uiso 1 1 calc R U . . . H23C H 1.073415 0.826150 0.464358 0.089 Uiso 1 1 calc R U . . . C13 C 1.1187(6) 0.6149(5) 0.4361(3) 0.0731(19) Uani 1 1 d . . . . . H13A H 1.165173 0.673347 0.445931 0.110 Uiso 1 1 calc R U . . . H13B H 1.181744 0.565244 0.435603 0.110 Uiso 1 1 calc R U . . . H13C H 1.067971 0.601814 0.468440 0.110 Uiso 1 1 calc R U . . . C24 C 0.8882(7) 0.9571(4) 0.3864(3) 0.0654(17) Uani 1 1 d . . . . . H24A H 0.966565 0.938101 0.371651 0.098 Uiso 1 1 calc R U . . . H24B H 0.913192 0.996399 0.423771 0.098 Uiso 1 1 calc R U . . . H24C H 0.830502 0.991403 0.352777 0.098 Uiso 1 1 calc R U . . . C26 C 0.6973(11) 0.5590(4) 0.0373(4) 0.112(4) Uani 1 1 d . . . . . H26C H 0.670973 0.577779 -0.007547 0.135 Uiso 0.5 1 calc R U P A 1 H26D H 0.789701 0.577338 0.051412 0.135 Uiso 0.5 1 calc R U P A 1 H26A H 0.658428 0.564359 -0.008349 0.135 Uiso 0.5 1 calc R U P A -1 H26B H 0.787443 0.583119 0.044090 0.135 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7031(11) 0.4474(6) 0.0576(3) 0.078(2) 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 0.02422(10) 0.02497(9) 0.02431(10) -0.00032(6) 0.00109(7) 0.00317(6) I1 0.03800(15) 0.03287(14) 0.03878(16) 0.00221(11) 0.00632(11) -0.01055(10) I4 0.03793(16) 0.04016(16) 0.04917(19) 0.00656(12) 0.00772(13) -0.01116(11) I3 0.04938(18) 0.04549(17) 0.03321(16) 0.01050(12) 0.00534(12) 0.01540(12) I2 0.03149(16) 0.0552(2) 0.0727(3) -0.00045(16) -0.01480(15) -0.00632(12) Cl2 0.0875(11) 0.0781(10) 0.0573(9) 0.0062(8) 0.0144(8) 0.0280(8) Cl1A 0.092(5) 0.086(4) 0.229(12) -0.049(6) 0.041(7) 0.001(3) N1 0.0278(17) 0.0318(17) 0.0267(17) 0.0011(13) 0.0044(13) -0.0013(12) C5 0.0256(18) 0.0298(18) 0.029(2) 0.0019(15) 0.0047(15) -0.0001(14) C2 0.0255(19) 0.0294(19) 0.032(2) 0.0004(15) 0.0048(16) -0.0045(14) C10 0.037(2) 0.035(2) 0.032(2) 0.0050(17) 0.0104(17) 0.0118(16) C6 0.032(2) 0.0294(19) 0.044(3) -0.0085(17) 0.0063(18) 0.0084(15) C8 0.033(2) 0.042(2) 0.041(3) -0.0097(19) -0.0025(18) 0.0170(17) C21 0.037(3) 0.072(3) 0.060(4) -0.020(3) 0.016(2) -0.006(2) C20 0.048(3) 0.031(2) 0.029(2) -0.0024(16) 0.0048(18) 0.0141(17) C19 0.053(3) 0.0258(19) 0.038(2) -0.0066(17) 0.014(2) -0.0030(17) C4 0.033(2) 0.0279(18) 0.030(2) 0.0025(15) 0.0050(16) 0.0072(14) C9 0.024(2) 0.035(2) 0.055(3) -0.0049(19) 0.0099(18) 0.0001(15) C3 0.0273(19) 0.0326(19) 0.030(2) -0.0050(16) -0.0023(15) -0.0013(14) C16 0.032(2) 0.036(2) 0.027(2) -0.0068(16) 0.0094(16) 0.0057(15) C25 0.078(4) 0.059(3) 0.048(3) 0.006(3) 0.008(3) 0.045(3) C15 0.071(4) 0.072(4) 0.044(3) 0.007(3) 0.025(3) 0.022(3) C12 0.081(4) 0.038(3) 0.092(5) 0.025(3) 0.036(4) 0.018(3) C11 0.045(3) 0.059(3) 0.083(4) -0.036(3) 0.004(3) 0.005(2) C14 0.046(3) 0.060(3) 0.116(6) -0.011(4) 0.025(3) -0.014(2) C17 0.040(2) 0.034(2) 0.028(2) 0.0003(16) 0.0075(17) 0.0058(16) C18 0.037(2) 0.039(2) 0.026(2) -0.0070(17) 0.0040(16) 0.0017(16) C22 0.071(4) 0.055(3) 0.038(3) 0.017(2) 0.014(2) 0.014(2) C7 0.040(2) 0.029(2) 0.048(3) 0.0083(18) 0.016(2) 0.0121(16) C23 0.043(3) 0.074(4) 0.056(3) -0.027(3) -0.001(2) -0.005(2) C13 0.062(4) 0.096(4) 0.048(3) -0.017(3) -0.019(3) 0.041(3) C24 0.097(5) 0.041(3) 0.066(4) -0.007(3) 0.033(4) -0.024(3) C26 0.205(10) 0.065(4) 0.101(6) 0.021(4) 0.109(7) 0.018(5) Cl1B 0.114(5) 0.056(3) 0.068(2) 0.016(2) 0.028(2) 0.031(3) 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 6 -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 61.95(7) . . ? N1 Dy1 C10 83.77(12) . . ? N1 Dy1 C6 92.23(12) . . ? N1 Dy1 C8 134.83(13) . . ? N1 Dy1 C20 81.04(12) . . ? N1 Dy1 C19 96.68(13) . . ? N1 Dy1 C9 107.52(13) . . ? N1 Dy1 C16 99.68(12) . . ? N1 Dy1 C17 129.75(12) . . ? N1 Dy1 C18 127.69(12) . . ? N1 Dy1 C7 122.74(13) . . ? C10 Dy1 I1 102.06(10) . . ? C10 Dy1 C20 152.81(13) . . ? C10 Dy1 C16 176.05(12) . . ? C10 Dy1 C17 146.10(13) . . ? C6 Dy1 I1 80.27(9) . . ? C6 Dy1 C10 30.64(13) . . ? C6 Dy1 C20 170.40(14) . . ? C6 Dy1 C16 146.50(13) . . ? C6 Dy1 C17 132.70(13) . . ? C8 Dy1 I1 122.92(10) . . ? C8 Dy1 C10 51.12(13) . . ? C8 Dy1 C6 51.09(13) . . ? C8 Dy1 C20 138.05(14) . . ? C8 Dy1 C16 125.48(14) . . ? C8 Dy1 C17 95.10(13) . . ? C20 Dy1 I1 90.49(10) . . ? C20 Dy1 C16 30.75(13) . . ? C20 Dy1 C17 51.17(13) . . ? C19 Dy1 I1 121.61(10) . . ? C19 Dy1 C10 130.72(13) . . ? C19 Dy1 C6 158.03(14) . . ? C19 Dy1 C8 110.48(14) . . ? C19 Dy1 C20 31.12(14) . . ? C19 Dy1 C9 107.18(14) . . ? C19 Dy1 C16 51.08(13) . . ? C19 Dy1 C17 51.35(13) . . ? C19 Dy1 C18 31.26(13) . . ? C19 Dy1 C7 138.11(15) . . ? C9 Dy1 I1 130.57(9) . . ? C9 Dy1 C10 30.87(14) . . ? C9 Dy1 C6 50.87(13) . . ? C9 Dy1 C8 30.96(14) . . ? C9 Dy1 C20 137.77(14) . . ? C9 Dy1 C16 147.49(14) . . ? C9 Dy1 C17 117.93(14) . . ? C9 Dy1 C18 97.59(13) . . ? C9 Dy1 C7 51.21(13) . . ? C16 Dy1 I1 78.06(9) . . ? C17 Dy1 I1 99.49(9) . . ? C17 Dy1 C16 30.83(13) . . ? C18 Dy1 I1 128.00(9) . . ? C18 Dy1 C10 128.32(13) . . ? C18 Dy1 C6 137.50(13) . . ? C18 Dy1 C8 86.89(13) . . ? C18 Dy1 C20 51.23(13) . . ? C18 Dy1 C16 50.75(13) . . ? C18 Dy1 C17 30.69(13) . . ? C7 Dy1 I1 91.79(10) . . ? C7 Dy1 C10 51.06(13) . . ? C7 Dy1 C6 30.90(14) . . ? C7 Dy1 C8 31.13(14) . . ? C7 Dy1 C20 153.72(14) . . ? C7 Dy1 C16 125.04(13) . . ? C7 Dy1 C17 102.69(13) . . ? C7 Dy1 C18 108.89(14) . . ? C2 I1 Dy1 68.12(11) . . ? C5 N1 Dy1 143.7(3) . . ? C2 N1 Dy1 111.0(2) . . ? C2 N1 C5 104.4(3) . . ? N1 C5 I4 121.7(3) . . ? N1 C5 C4 111.4(3) . . ? C4 C5 I4 126.9(3) . . ? N1 C2 I1 118.7(3) . . ? N1 C2 C3 112.6(3) . . ? C3 C2 I1 128.7(3) . . ? C6 C10 Dy1 74.7(2) . . ? C6 C10 C9 107.8(4) . . ? C6 C10 C15 124.7(5) . . ? C9 C10 Dy1 73.8(2) . . ? C9 C10 C15 127.0(4) . . ? C15 C10 Dy1 123.4(3) . . ? C10 C6 Dy1 74.7(2) . . ? C10 C6 C11 125.2(5) . . ? C10 C6 C7 108.4(4) . . ? C11 C6 Dy1 125.1(3) . . ? C7 C6 Dy1 74.0(2) . . ? C7 C6 C11 125.7(4) . . ? C9 C8 Dy1 73.8(2) . . ? C9 C8 C7 107.2(4) . . ? C9 C8 C13 126.8(5) . . ? C7 C8 Dy1 73.9(2) . . ? C7 C8 C13 124.6(5) . . ? C13 C8 Dy1 128.6(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 73.3(2) . . ? C19 C20 C25 126.1(4) . . ? C16 C20 Dy1 75.1(2) . . ? C16 C20 C19 107.6(4) . . ? C16 C20 C25 126.1(5) . . ? C25 C20 Dy1 121.6(3) . . ? C20 C19 Dy1 75.6(2) . . ? C20 C19 C18 107.8(4) . . ? C20 C19 C24 126.9(5) . . ? C18 C19 Dy1 75.2(2) . . ? C18 C19 C24 124.6(5) . . ? C24 C19 Dy1 122.9(3) . . ? C5 C4 I3 126.7(3) . . ? C5 C4 C3 105.9(3) . . ? C3 C4 I3 127.4(3) . . ? C10 C9 Dy1 75.4(2) . . ? C10 C9 C8 108.6(4) . . ? C10 C9 C14 125.2(5) . . ? C8 C9 Dy1 75.3(2) . . ? C8 C9 C14 125.7(5) . . ? C14 C9 Dy1 122.0(3) . . ? C2 C3 I2 126.6(3) . . ? C2 C3 C4 105.7(3) . . ? C4 C3 I2 127.7(3) . . ? C21 C16 Dy1 127.3(3) . . ? C20 C16 Dy1 74.1(2) . . ? C20 C16 C21 126.2(4) . . ? C20 C16 C17 108.5(4) . . ? C17 C16 Dy1 74.2(2) . . ? C17 C16 C21 124.1(4) . . ? 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 125.6(4) . . ? C18 C17 Dy1 74.2(2) . . ? C18 C17 C16 107.7(4) . . ? C18 C17 C22 126.2(4) . . ? C22 C17 Dy1 122.4(3) . . ? C19 C18 Dy1 73.5(2) . . ? C19 C18 C23 124.3(4) . . ? C17 C18 Dy1 75.1(2) . . ? C17 C18 C19 108.3(4) . . ? C17 C18 C23 126.1(4) . . ? C23 C18 Dy1 127.5(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 75.1(2) . . ? C6 C7 C8 107.9(4) . . ? C6 C7 C12 126.1(5) . . ? C8 C7 Dy1 75.0(2) . . ? C8 C7 C12 125.7(5) . . ? C12 C7 Dy1 120.8(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 106.5 . . ? Cl2 C26 H26D 106.5 . . ? Cl2 C26 H26A 108.7 . . ? Cl2 C26 H26B 108.7 . . ? Cl1A C26 Cl2 123.4(6) . . ? Cl1A C26 H26C 106.5 . . ? Cl1A C26 H26D 106.5 . . ? Cl1A C26 H26A 94.8 . . ? Cl1A C26 H26B 111.7 . . ? Cl1A C26 Cl1B 14.2(6) . . ? H26C C26 H26D 106.5 . . ? H26C C26 H26A 13.6 . . ? H26C C26 H26B 96.4 . . ? H26D C26 H26A 117.4 . . ? H26D C26 H26B 10.2 . . ? H26A C26 H26B 107.6 . . ? Cl1B C26 Cl2 114.1(5) . . ? Cl1B C26 H26C 120.6 . . ? Cl1B C26 H26D 101.5 . . ? 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 3.2449(3) . ? Dy1 N1 2.379(3) . ? Dy1 C10 2.654(4) . ? Dy1 C6 2.653(4) . ? Dy1 C8 2.653(4) . ? Dy1 C20 2.655(4) . ? Dy1 C19 2.626(4) . ? Dy1 C9 2.634(4) . ? Dy1 C16 2.669(4) . ? Dy1 C17 2.659(4) . ? Dy1 C18 2.647(4) . ? Dy1 C7 2.639(4) . ? I1 C2 2.087(4) . ? I4 C5 2.074(4) . ? I3 C4 2.062(4) . ? I2 C3 2.064(4) . ? Cl2 C26 1.715(7) . ? Cl1A C26 1.656(13) . ? N1 C5 1.373(5) . ? N1 C2 1.361(5) . ? C5 C4 1.386(5) . ? C2 C3 1.373(6) . ? C10 C6 1.402(6) . ? C10 C9 1.407(6) . ? C10 C15 1.495(6) . ? C6 C11 1.507(7) . ? C6 C7 1.410(7) . ? C8 C9 1.411(7) . ? C8 C7 1.420(6) . ? C8 C13 1.503(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21 C16 1.515(6) . ? C20 C19 1.417(6) . ? C20 C16 1.412(6) . ? C20 C25 1.503(6) . ? C19 C18 1.421(6) . ? C19 C24 1.508(6) . ? C4 C3 1.410(5) . ? C9 C14 1.517(6) . ? C16 C17 1.416(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C12 C7 1.498(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C17 C18 1.404(6) . ? C17 C22 1.510(6) . ? C18 C23 1.510(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 Cl1B 1.660(10) . ? 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 11.9(6) . . . . ? Dy1 N1 C5 C4 -167.9(3) . . . . ? Dy1 N1 C2 I1 -5.5(3) . . . . ? Dy1 N1 C2 C3 172.3(3) . . . . ? Dy1 C10 C6 C11 122.4(4) . . . . ? Dy1 C10 C6 C7 -66.9(3) . . . . ? Dy1 C10 C9 C8 68.6(3) . . . . ? Dy1 C10 C9 C14 -119.0(4) . . . . ? Dy1 C6 C7 C8 -68.4(3) . . . . ? Dy1 C6 C7 C12 117.5(4) . . . . ? Dy1 C8 C9 C10 -68.6(3) . . . . ? Dy1 C8 C9 C14 119.0(4) . . . . ? Dy1 C8 C7 C6 68.5(3) . . . . ? Dy1 C8 C7 C12 -117.3(4) . . . . ? Dy1 C20 C19 C18 -68.9(3) . . . . ? Dy1 C20 C19 C24 120.6(5) . . . . ? Dy1 C20 C16 C21 -124.9(4) . . . . ? Dy1 C20 C16 C17 66.8(3) . . . . ? Dy1 C19 C18 C17 -67.7(3) . . . . ? Dy1 C19 C18 C23 124.6(4) . . . . ? Dy1 C16 C17 C18 67.5(3) . . . . ? Dy1 C16 C17 C22 -119.4(4) . . . . ? Dy1 C17 C18 C19 66.6(3) . . . . ? Dy1 C17 C18 C23 -125.9(4) . . . . ? I1 C2 C3 I2 -4.3(6) . . . . ? I1 C2 C3 C4 177.6(3) . . . . ? I4 C5 C4 I3 -0.6(5) . . . . ? I4 C5 C4 C3 -179.4(3) . . . . ? I3 C4 C3 I2 2.9(5) . . . . ? I3 C4 C3 C2 -179.0(3) . . . . ? N1 C5 C4 I3 179.2(3) . . . . ? N1 C5 C4 C3 0.3(4) . . . . ? N1 C2 C3 I2 178.1(3) . . . . ? N1 C2 C3 C4 0.0(5) . . . . ? C5 N1 C2 I1 -177.7(2) . . . . ? C5 N1 C2 C3 0.1(4) . . . . ? C5 C4 C3 I2 -178.3(3) . . . . ? C5 C4 C3 C2 -0.2(4) . . . . ? C2 N1 C5 I4 179.5(3) . . . . ? C2 N1 C5 C4 -0.3(4) . . . . ? C10 C6 C7 Dy1 67.4(3) . . . . ? C10 C6 C7 C8 -1.0(4) . . . . ? C10 C6 C7 C12 -175.2(4) . . . . ? C6 C10 C9 Dy1 -67.5(3) . . . . ? C6 C10 C9 C8 1.1(4) . . . . ? C6 C10 C9 C14 173.5(4) . . . . ? C21 C16 C17 Dy1 124.7(4) . . . . ? C21 C16 C17 C18 -167.8(4) . . . . ? C21 C16 C17 C22 5.4(6) . . . . ? C20 C19 C18 Dy1 69.2(3) . . . . ? C20 C19 C18 C17 1.5(5) . . . . ? C20 C19 C18 C23 -166.2(4) . . . . ? C20 C16 C17 Dy1 -66.7(3) . . . . ? C20 C16 C17 C18 0.8(4) . . . . ? C20 C16 C17 C22 173.9(4) . . . . ? C19 C20 C16 Dy1 -66.7(3) . . . . ? C19 C20 C16 C21 168.4(4) . . . . ? C19 C20 C16 C17 0.2(4) . . . . ? C9 C10 C6 Dy1 66.9(3) . . . . ? C9 C10 C6 C11 -170.7(4) . . . . ? C9 C10 C6 C7 0.0(4) . . . . ? C9 C8 C7 Dy1 -66.8(3) . . . . ? C9 C8 C7 C6 1.7(4) . . . . ? C9 C8 C7 C12 175.8(4) . . . . ? C16 C20 C19 Dy1 67.9(3) . . . . ? C16 C20 C19 C18 -1.0(5) . . . . ? C16 C20 C19 C24 -171.5(4) . . . . ? C16 C17 C18 Dy1 -68.0(3) . . . . ? C16 C17 C18 C19 -1.4(4) . . . . ? C16 C17 C18 C23 166.1(4) . . . . ? C25 C20 C19 Dy1 -117.2(4) . . . . ? C25 C20 C19 C18 173.8(4) . . . . ? C25 C20 C19 C24 3.3(7) . . . . ? C25 C20 C16 Dy1 118.5(4) . . . . ? C25 C20 C16 C21 -6.5(7) . . . . ? C25 C20 C16 C17 -174.7(4) . . . . ? C15 C10 C6 Dy1 -120.3(4) . . . . ? C15 C10 C6 C11 2.1(7) . . . . ? C15 C10 C6 C7 172.8(4) . . . . ? C15 C10 C9 Dy1 119.9(4) . . . . ? C15 C10 C9 C8 -171.5(4) . . . . ? C15 C10 C9 C14 0.9(7) . . . . ? C11 C6 C7 Dy1 -122.0(4) . . . . ? C11 C6 C7 C8 169.6(4) . . . . ? C11 C6 C7 C12 -4.6(7) . . . . ? C22 C17 C18 Dy1 118.9(4) . . . . ? C22 C17 C18 C19 -174.5(4) . . . . ? C22 C17 C18 C23 -7.0(7) . . . . ? C7 C8 C9 Dy1 66.9(3) . . . . ? C7 C8 C9 C10 -1.7(4) . . . . ? C7 C8 C9 C14 -174.1(4) . . . . ? C13 C8 C9 Dy1 -126.5(4) . . . . ? C13 C8 C9 C10 164.9(4) . . . . ? C13 C8 C9 C14 -7.4(7) . . . . ? C13 C8 C7 Dy1 126.2(4) . . . . ? C13 C8 C7 C6 -165.3(4) . . . . ? C13 C8 C7 C12 8.8(7) . . . . ? C24 C19 C18 Dy1 -120.0(4) . . . . ? C24 C19 C18 C17 172.3(4) . . . . ? C24 C19 C18 C23 4.5(7) . . . . ? 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 -1.0044 -1.0313 0.1432 -0.0783 -0.0142 0.0325 -1.0172 0.9856 0.0118 0.0038 0.0040 0.0859 1.0044 1.0313 -0.1432 0.0783 0.0142 -0.0325 1.0172 -0.9856 -0.0118 -0.0038 -0.0040 -0.0859 -0.0137 -0.0326 -0.9981 -0.0100 0.0322 0.0044 0.0137 0.0326 0.9981 0.0100 -0.0322 -0.0044 -0.9899 1.0509 2.0080 0.0239 -0.0605 0.0770 0.9899 -1.0509 -2.0080 -0.0239 0.0605 -0.0770 1.0309 -0.9529 0.9863 0.0063 -0.0363 -0.0903 0.0210 1.0738 1.9305 0.0612 -0.0554 0.0178 2.0418 -0.9300 0.9088 0.0435 -0.0312 -0.1495 -0.0338 0.9431 -2.0619 0.0210 0.0736 0.0356 -1.0382 -0.0882 -1.9187 -0.0574 0.0594 0.0681 -0.9835 0.0424 2.0737 -0.0172 -0.0696 0.0503 -6.1701 6.4635 -22.4183 -0.1415 0.7602 0.6341