#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:50:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294477 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572179.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_1572179 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 102.244(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.4118(3) _cell_length_b 14.4128(4) _cell_length_c 21.5424(7) _cell_measurement_reflns_used 16617 _cell_measurement_temperature 290.0(1) _cell_measurement_theta_max 29.5140 _cell_measurement_theta_min 2.8210 _cell_volume 3159.19(17) _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 290.0(1) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.840 _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 0.0343473000 _diffrn_orient_matrix_UB_12 0.0425316000 _diffrn_orient_matrix_UB_13 0.0068450000 _diffrn_orient_matrix_UB_21 -0.0042590000 _diffrn_orient_matrix_UB_22 0.0073999000 _diffrn_orient_matrix_UB_23 -0.0329270000 _diffrn_orient_matrix_UB_31 -0.0605090000 _diffrn_orient_matrix_UB_32 0.0236291000 _diffrn_orient_matrix_UB_33 -0.0020234000 _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 0.0600 _diffrn_reflns_av_unetI/netI 0.0509 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.840 _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 39519 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.840 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.741 _diffrn_reflns_theta_min 2.450 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.458 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.261 _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 2.286 _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 1.020 _refine_diff_density_min -1.150 _refine_diff_density_rms 0.140 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 9017 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0373 _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^)+(0.0351P)^2^+0.4061P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.0888 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6499 _reflns_number_total 9017 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP290K _cod_depositor_comments 'Adding full bibliography for 1572175--1572199.cif.' _cod_original_cell_volume 3159.18(16) _cod_database_code 1572179 _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 0.534 _shelx_estimated_absorpt_t_min 0.209 _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_290_final.res created by SHELXL-2018/3 at 17:15:57 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 10.411777 14.412821 21.542361 90 102.244 90 ZERR 4 0.000292 0.000396 0.000662 0 0.0029 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. 75 0 0 PLAN 16 SIZE 0.111 0.275 0.353 TEMP 16.85(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.035100 0.406100 FVAR 0.62708 DY1 4 0.803924 0.716533 0.338581 11.00000 0.03163 0.03326 = 0.03294 -0.00023 0.00185 0.00405 I1 5 0.523559 0.618282 0.278838 11.00000 0.05069 0.04367 = 0.05334 0.00331 0.00863 -0.01378 I4 5 0.822658 0.939345 0.200781 11.00000 0.05088 0.05402 = 0.06701 0.00914 0.01111 -0.01489 I3 5 0.487969 0.938734 0.082570 11.00000 0.06721 0.06113 = 0.04471 0.01454 0.00773 0.02102 I2 5 0.294622 0.725203 0.128804 11.00000 0.04178 0.07226 = 0.09511 -0.00155 -0.01857 -0.00737 CL2 3 0.608870 0.626710 0.078388 11.00000 0.12336 0.10827 = 0.07967 0.00935 0.02364 0.03846 PART 1 CL1A 3 0.693322 0.445161 0.039764 10.50000 0.09537 0.10031 = 0.25848 -0.03962 0.04287 -0.00825 PART 0 N1 6 0.678029 0.774797 0.240781 11.00000 0.03380 0.04317 = 0.03562 0.00223 0.00286 -0.00370 C5 1 0.669514 0.846166 0.198314 11.00000 0.03803 0.03458 = 0.03890 0.00457 0.00919 0.00194 C2 1 0.561456 0.730396 0.224555 11.00000 0.03668 0.03713 = 0.03927 0.00177 0.00411 -0.00558 C10 1 0.957199 0.648665 0.265459 11.00000 0.04757 0.04962 = 0.04719 0.00755 0.01428 0.01690 C6 1 0.887866 0.572034 0.281872 11.00000 0.04251 0.03962 = 0.06049 -0.01384 0.00902 0.00589 C8 1 1.025844 0.622244 0.372490 11.00000 0.04072 0.05507 = 0.05595 -0.00819 0.00311 0.01693 C21 1 0.522882 0.735226 0.423742 11.00000 0.04961 0.09854 = 0.07818 -0.02962 0.02599 -0.01252 AFIX 137 H21A 2 0.462398 0.743511 0.383793 11.00000 -1.50000 H21B 2 0.491481 0.768152 0.456310 11.00000 -1.50000 H21C 2 0.530072 0.670385 0.434094 11.00000 -1.50000 AFIX 0 C20 1 0.679178 0.851101 0.384815 11.00000 0.06316 0.03945 = 0.04452 -0.00127 0.00818 0.01900 C19 1 0.814664 0.872882 0.402157 11.00000 0.06489 0.04010 = 0.05103 -0.00858 0.02382 -0.00392 C4 1 0.550889 0.845040 0.156204 11.00000 0.04089 0.04013 = 0.03636 -0.00002 0.00532 0.00478 C9 1 1.042238 0.680363 0.321485 11.00000 0.03248 0.05188 = 0.07475 -0.00665 0.01385 0.00081 C3 1 0.479286 0.770321 0.172707 11.00000 0.03409 0.04337 = 0.04801 -0.00317 0.00256 -0.00459 C16 1 0.654984 0.772081 0.419111 11.00000 0.04215 0.04650 = 0.04526 -0.00785 0.01155 0.00317 C25 1 0.575450 0.909493 0.342005 11.00000 0.11145 0.07841 = 0.06184 0.00349 0.00859 0.06074 AFIX 137 H25A 2 0.616728 0.948970 0.316099 11.00000 -1.50000 H25B 2 0.530524 0.946885 0.367562 11.00000 -1.50000 H25C 2 0.513476 0.869566 0.315269 11.00000 -1.50000 AFIX 0 C15 1 0.953497 0.681794 0.199287 11.00000 0.10070 0.08959 = 0.07209 0.02128 0.04409 0.03363 AFIX 137 H15A 2 0.863780 0.688501 0.177049 11.00000 -1.50000 H15B 2 0.997005 0.637530 0.177544 11.00000 -1.50000 H15C 2 0.997330 0.740609 0.200807 11.00000 -1.50000 AFIX 0 C12 1 0.885592 0.476490 0.383388 11.00000 0.10716 0.05737 = 0.12631 0.04299 0.05443 0.02645 AFIX 137 H12A 2 0.890926 0.494293 0.426802 11.00000 -1.50000 H12B 2 0.942071 0.424263 0.381876 11.00000 -1.50000 H12C 2 0.796633 0.459951 0.364371 11.00000 -1.50000 AFIX 0 C11 1 0.800436 0.509398 0.234003 11.00000 0.06444 0.07532 = 0.10045 -0.04036 0.00254 0.00905 AFIX 137 H11A 2 0.748004 0.471242 0.255479 11.00000 -1.50000 H11B 2 0.854100 0.470660 0.213586 11.00000 -1.50000 H11C 2 0.743965 0.546720 0.202700 11.00000 -1.50000 AFIX 0 C14 1 1.144076 0.755188 0.324747 11.00000 0.06266 0.07735 = 0.16198 -0.02568 0.03713 -0.01439 AFIX 137 H14A 2 1.103100 0.810660 0.305253 11.00000 -1.50000 H14B 2 1.210193 0.735120 0.302707 11.00000 -1.50000 H14C 2 1.183959 0.767559 0.368364 11.00000 -1.50000 AFIX 0 C17 1 0.774782 0.743488 0.456834 11.00000 0.05442 0.04440 = 0.03647 -0.00279 0.00967 0.00795 C18 1 0.872835 0.805271 0.447553 11.00000 0.03828 0.05549 = 0.04255 -0.01568 0.00170 0.00221 C22 1 0.791590 0.666530 0.505635 11.00000 0.10727 0.07339 = 0.05470 0.02008 0.02811 0.01807 AFIX 137 H22A 2 0.710579 0.632920 0.501346 11.00000 -1.50000 H22B 2 0.815183 0.692711 0.547486 11.00000 -1.50000 H22C 2 0.859677 0.625120 0.499046 11.00000 -1.50000 AFIX 0 C7 1 0.928236 0.556546 0.347436 11.00000 0.05553 0.03466 = 0.06364 0.01223 0.02250 0.01548 C23 1 1.009119 0.813152 0.489337 11.00000 0.05791 0.10196 = 0.07300 -0.03441 -0.00433 -0.00265 AFIX 137 H23A 2 1.038197 0.753033 0.505713 11.00000 -1.50000 H23B 2 1.006750 0.854548 0.523988 11.00000 -1.50000 H23C 2 1.068776 0.836869 0.464790 11.00000 -1.50000 AFIX 0 C13 1 1.117741 0.615977 0.436673 11.00000 0.08327 0.13120 = 0.07363 -0.01413 -0.01639 0.06157 AFIX 137 H13A 2 1.161171 0.674485 0.446852 11.00000 -1.50000 H13B 2 1.182052 0.568553 0.435749 11.00000 -1.50000 H13C 2 1.068499 0.600903 0.468276 11.00000 -1.50000 AFIX 0 C24 1 0.881770 0.958357 0.385239 11.00000 0.14890 0.05193 = 0.08919 -0.01713 0.06021 -0.03860 AFIX 137 H24A 2 0.966648 0.942118 0.377793 11.00000 -1.50000 H24B 2 0.891966 1.002076 0.419558 11.00000 -1.50000 H24C 2 0.829677 0.985622 0.347531 11.00000 -1.50000 AFIX 0 C26 1 0.694549 0.559876 0.035926 11.00000 0.21222 0.09831 = 0.10384 0.02872 0.09504 0.00902 PART 1 AFIX 23 H26C 2 0.664102 0.576424 -0.008402 10.50000 -1.20000 H26D 2 0.785725 0.579154 0.047836 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.649674 0.561377 -0.008388 10.50000 -1.20000 H26B 2 0.780766 0.587208 0.038867 10.50000 -1.20000 AFIX 0 CL1B 3 0.713214 0.452315 0.058474 10.50000 0.16923 0.09853 = 0.08776 0.02036 0.02569 0.06419 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0888, GooF = S = 1.040, Restrained GooF = 1.040 for all data REM R1 = 0.0373 for 6499 Fo > 4sig(Fo) and 0.0595 for all 9017 data REM 317 parameters refined using 6 restraints END WGHT 0.0350 0.4003 REM Highest difference peak 1.020, deepest hole -1.150, 1-sigma level 0.140 Q1 1 0.2961 0.7449 0.1650 11.00000 0.05 1.02 Q2 1 0.4727 0.8974 0.0618 11.00000 0.05 0.88 Q3 1 0.5622 0.9568 0.0851 11.00000 0.05 0.77 Q4 1 0.4643 0.9401 0.0960 11.00000 0.05 0.67 Q5 1 0.4430 0.6105 0.2747 11.00000 0.05 0.65 Q6 1 0.7952 0.5043 0.0568 11.00000 0.05 0.65 Q7 1 0.3148 0.7568 0.0996 11.00000 0.05 0.62 Q8 1 0.3613 0.7283 0.1174 11.00000 0.05 0.56 Q9 1 0.8017 0.8575 0.3399 11.00000 0.05 0.55 Q10 1 1.0861 0.6190 0.3979 11.00000 0.05 0.51 Q11 1 0.2984 0.7244 0.2182 11.00000 0.05 0.49 Q12 1 1.0967 0.7234 0.1987 11.00000 0.05 0.49 Q13 1 0.8985 1.0814 0.4406 11.00000 0.05 0.49 Q14 1 0.9461 0.6026 0.2790 11.00000 0.05 0.47 Q15 1 0.7019 0.6978 0.3426 11.00000 0.05 0.47 Q16 1 0.4847 0.9412 0.1635 11.00000 0.05 0.46 ; _shelx_res_checksum 56361 _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 2.378 _oxdiff_exptl_absorpt_empirical_full_min 0.618 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 0.80392(2) 0.71653(2) 0.33858(2) 0.03335(6) Uani 1 1 d . . . . . I1 I 0.52356(3) 0.61828(2) 0.27884(2) 0.04959(9) Uani 1 1 d . . . . . I4 I 0.82266(3) 0.93935(2) 0.20078(2) 0.05751(10) Uani 1 1 d . . . . . I3 I 0.48797(4) 0.93873(2) 0.08257(2) 0.05830(10) Uani 1 1 d . . . . . I2 I 0.29462(4) 0.72520(3) 0.12880(2) 0.07462(13) Uani 1 1 d . . . . . Cl2 Cl 0.6089(2) 0.62671(15) 0.07839(10) 0.1035(7) Uani 1 1 d . . . . . Cl1A Cl 0.6933(11) 0.4452(9) 0.0398(7) 0.151(5) Uani 0.5 1 d . U P A 1 N1 N 0.6780(3) 0.7748(2) 0.24078(17) 0.0382(8) Uani 1 1 d . . . . . C5 C 0.6695(4) 0.8462(3) 0.1983(2) 0.0370(9) Uani 1 1 d . . . . . C2 C 0.5615(4) 0.7304(3) 0.2246(2) 0.0383(9) Uani 1 1 d . . . . . C10 C 0.9572(5) 0.6487(3) 0.2655(2) 0.0475(11) Uani 1 1 d . . . . . C6 C 0.8879(5) 0.5720(3) 0.2819(3) 0.0478(11) Uani 1 1 d . . . . . C8 C 1.0258(5) 0.6222(3) 0.3725(3) 0.0516(12) Uani 1 1 d . . . . . C21 C 0.5229(6) 0.7352(5) 0.4237(3) 0.0736(18) Uani 1 1 d . . . . . H21A H 0.462398 0.743511 0.383793 0.110 Uiso 1 1 calc R U . . . H21B H 0.491481 0.768152 0.456310 0.110 Uiso 1 1 calc R U . . . H21C H 0.530072 0.670385 0.434094 0.110 Uiso 1 1 calc R U . . . C20 C 0.6792(5) 0.8511(3) 0.3848(2) 0.0495(12) Uani 1 1 d . . . . . C19 C 0.8147(5) 0.8729(3) 0.4022(3) 0.0503(12) Uani 1 1 d . . . . . C4 C 0.5509(4) 0.8450(3) 0.1562(2) 0.0396(9) Uani 1 1 d . . . . . C9 C 1.0422(5) 0.6804(4) 0.3215(3) 0.0527(12) Uani 1 1 d . . . . . C3 C 0.4793(4) 0.7703(3) 0.1727(2) 0.0427(10) Uani 1 1 d . . . . . C16 C 0.6550(5) 0.7721(3) 0.4191(2) 0.0443(10) Uani 1 1 d . . . . . C25 C 0.5754(7) 0.9095(5) 0.3420(3) 0.085(2) Uani 1 1 d . . . . . H25A H 0.616728 0.948970 0.316099 0.128 Uiso 1 1 calc R U . . . H25B H 0.530524 0.946885 0.367562 0.128 Uiso 1 1 calc R U . . . H25C H 0.513476 0.869566 0.315269 0.128 Uiso 1 1 calc R U . . . C15 C 0.9535(8) 0.6818(5) 0.1993(3) 0.084(2) Uani 1 1 d . . . . . H15A H 0.863780 0.688501 0.177049 0.125 Uiso 1 1 calc R U . . . H15B H 0.997005 0.637530 0.177544 0.125 Uiso 1 1 calc R U . . . H15C H 0.997330 0.740609 0.200807 0.125 Uiso 1 1 calc R U . . . C12 C 0.8856(8) 0.4765(4) 0.3834(4) 0.093(3) Uani 1 1 d . . . . . H12A H 0.890926 0.494293 0.426802 0.139 Uiso 1 1 calc R U . . . H12B H 0.942071 0.424263 0.381876 0.139 Uiso 1 1 calc R U . . . H12C H 0.796633 0.459951 0.364371 0.139 Uiso 1 1 calc R U . . . C11 C 0.8004(6) 0.5094(5) 0.2340(4) 0.082(2) Uani 1 1 d . . . . . H11A H 0.748004 0.471242 0.255479 0.123 Uiso 1 1 calc R U . . . H11B H 0.854100 0.470660 0.213586 0.123 Uiso 1 1 calc R U . . . H11C H 0.743965 0.546720 0.202700 0.123 Uiso 1 1 calc R U . . . C14 C 1.1441(7) 0.7552(5) 0.3247(5) 0.099(3) Uani 1 1 d . . . . . H14A H 1.103100 0.810660 0.305253 0.148 Uiso 1 1 calc R U . . . H14B H 1.210193 0.735120 0.302707 0.148 Uiso 1 1 calc R U . . . H14C H 1.183959 0.767559 0.368364 0.148 Uiso 1 1 calc R U . . . C17 C 0.7748(5) 0.7435(3) 0.4568(2) 0.0451(10) Uani 1 1 d . . . . . C18 C 0.8728(5) 0.8053(3) 0.4476(2) 0.0465(11) Uani 1 1 d . . . . . C22 C 0.7916(7) 0.6665(4) 0.5056(3) 0.0768(19) Uani 1 1 d . . . . . H22A H 0.710579 0.632920 0.501346 0.115 Uiso 1 1 calc R U . . . H22B H 0.815183 0.692711 0.547486 0.115 Uiso 1 1 calc R U . . . H22C H 0.859677 0.625120 0.499046 0.115 Uiso 1 1 calc R U . . . C7 C 0.9282(5) 0.5565(3) 0.3474(3) 0.0498(12) Uani 1 1 d . . . . . C23 C 1.0091(6) 0.8132(5) 0.4893(3) 0.0803(19) Uani 1 1 d . . . . . H23A H 1.038197 0.753033 0.505713 0.120 Uiso 1 1 calc R U . . . H23B H 1.006750 0.854548 0.523988 0.120 Uiso 1 1 calc R U . . . H23C H 1.068776 0.836869 0.464790 0.120 Uiso 1 1 calc R U . . . C13 C 1.1177(7) 0.6160(6) 0.4367(3) 0.101(3) Uani 1 1 d . . . . . H13A H 1.161171 0.674485 0.446852 0.151 Uiso 1 1 calc R U . . . H13B H 1.182052 0.568553 0.435749 0.151 Uiso 1 1 calc R U . . . H13C H 1.068499 0.600903 0.468276 0.151 Uiso 1 1 calc R U . . . C24 C 0.8818(9) 0.9584(4) 0.3852(4) 0.091(3) Uani 1 1 d . . . . . H24A H 0.966648 0.942118 0.377793 0.137 Uiso 1 1 calc R U . . . H24B H 0.891966 1.002076 0.419558 0.137 Uiso 1 1 calc R U . . . H24C H 0.829677 0.985622 0.347531 0.137 Uiso 1 1 calc R U . . . C26 C 0.6945(12) 0.5599(6) 0.0359(5) 0.129(4) Uani 1 1 d . . . . . H26C H 0.664102 0.576424 -0.008402 0.155 Uiso 0.5 1 calc R U P A 1 H26D H 0.785725 0.579154 0.047836 0.155 Uiso 0.5 1 calc R U P A 1 H26A H 0.649674 0.561377 -0.008388 0.155 Uiso 0.5 1 calc R U P A -1 H26B H 0.780766 0.587208 0.038867 0.155 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7132(12) 0.4523(7) 0.0585(5) 0.119(4) 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 0.03163(11) 0.03326(11) 0.03294(11) -0.00023(8) 0.00185(8) 0.00405(7) I1 0.05069(19) 0.04367(17) 0.0533(2) 0.00331(13) 0.00863(15) -0.01378(12) I4 0.0509(2) 0.0540(2) 0.0670(2) 0.00914(16) 0.01111(17) -0.01489(14) I3 0.0672(2) 0.0611(2) 0.04471(19) 0.01454(15) 0.00773(16) 0.02102(16) I2 0.0418(2) 0.0723(3) 0.0951(3) -0.0016(2) -0.01857(19) -0.00737(15) Cl2 0.1234(17) 0.1083(15) 0.0797(13) 0.0094(11) 0.0236(12) 0.0385(12) Cl1A 0.095(5) 0.100(5) 0.258(14) -0.040(7) 0.043(7) -0.008(3) N1 0.0338(19) 0.043(2) 0.036(2) 0.0022(15) 0.0029(15) -0.0037(14) C5 0.038(2) 0.035(2) 0.039(2) 0.0046(18) 0.0092(18) 0.0019(16) C2 0.037(2) 0.037(2) 0.039(2) 0.0018(18) 0.0041(18) -0.0056(16) C10 0.048(3) 0.050(3) 0.047(3) 0.008(2) 0.014(2) 0.017(2) C6 0.043(3) 0.040(2) 0.060(3) -0.014(2) 0.009(2) 0.0059(19) C8 0.041(3) 0.055(3) 0.056(3) -0.008(2) 0.003(2) 0.017(2) C21 0.050(3) 0.099(5) 0.078(4) -0.030(4) 0.026(3) -0.013(3) C20 0.063(3) 0.039(2) 0.045(3) -0.001(2) 0.008(2) 0.019(2) C19 0.065(3) 0.040(2) 0.051(3) -0.009(2) 0.024(3) -0.004(2) C4 0.041(2) 0.040(2) 0.036(2) 0.0000(18) 0.0053(19) 0.0048(18) C9 0.032(2) 0.052(3) 0.075(4) -0.007(3) 0.014(2) 0.001(2) C3 0.034(2) 0.043(2) 0.048(3) -0.003(2) 0.0026(19) -0.0046(18) C16 0.042(3) 0.047(3) 0.045(3) -0.008(2) 0.012(2) 0.0032(19) C25 0.111(6) 0.078(4) 0.062(4) 0.003(3) 0.009(4) 0.061(4) C15 0.101(5) 0.090(5) 0.072(4) 0.021(4) 0.044(4) 0.034(4) C12 0.107(6) 0.057(4) 0.126(7) 0.043(4) 0.054(5) 0.026(4) C11 0.064(4) 0.075(4) 0.100(5) -0.040(4) 0.003(4) 0.009(3) C14 0.063(4) 0.077(4) 0.162(9) -0.026(5) 0.037(5) -0.014(3) C17 0.054(3) 0.044(2) 0.036(2) -0.003(2) 0.010(2) 0.008(2) C18 0.038(2) 0.055(3) 0.043(3) -0.016(2) 0.002(2) 0.002(2) C22 0.107(5) 0.073(4) 0.055(4) 0.020(3) 0.028(4) 0.018(4) C7 0.056(3) 0.035(2) 0.064(3) 0.012(2) 0.022(3) 0.015(2) C23 0.058(4) 0.102(5) 0.073(4) -0.034(4) -0.004(3) -0.003(3) C13 0.083(5) 0.131(6) 0.074(5) -0.014(5) -0.016(4) 0.062(5) C24 0.149(7) 0.052(3) 0.089(5) -0.017(3) 0.060(5) -0.039(4) C26 0.212(11) 0.098(6) 0.104(7) 0.029(5) 0.095(8) 0.009(6) Cl1B 0.169(8) 0.099(5) 0.088(3) 0.020(3) 0.026(4) 0.064(5) 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 0 0.1448 0 1 -2 0.0988 -1 0 -2 0.1081 -1 0 2 0.1036 -7 6 -21 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 61.65(8) . . ? N1 Dy1 C10 83.83(13) . . ? N1 Dy1 C6 92.44(15) . . ? N1 Dy1 C8 135.12(15) . . ? N1 Dy1 C20 81.53(14) . . ? N1 Dy1 C19 96.50(15) . . ? N1 Dy1 C9 107.66(16) . . ? N1 Dy1 C16 100.45(14) . . ? N1 Dy1 C17 129.95(13) . . ? N1 Dy1 C18 127.63(14) . . ? N1 Dy1 C7 122.83(15) . . ? C10 Dy1 I1 101.93(12) . . ? C10 Dy1 C16 174.95(14) . . ? C10 Dy1 C17 145.87(15) . . ? C6 Dy1 I1 80.32(11) . . ? C6 Dy1 C10 30.69(15) . . ? C6 Dy1 C16 145.45(15) . . ? C6 Dy1 C17 132.19(16) . . ? C8 Dy1 I1 122.90(12) . . ? C8 Dy1 C10 51.33(16) . . ? C8 Dy1 C6 51.00(16) . . ? C8 Dy1 C16 124.43(16) . . ? C8 Dy1 C17 94.65(16) . . ? C20 Dy1 I1 89.83(12) . . ? C20 Dy1 C10 154.00(16) . . ? C20 Dy1 C6 170.05(16) . . ? C20 Dy1 C8 137.96(16) . . ? C20 Dy1 C16 30.67(15) . . ? C20 Dy1 C17 50.69(15) . . ? C19 Dy1 I1 120.99(12) . . ? C19 Dy1 C10 131.36(16) . . ? C19 Dy1 C6 158.61(16) . . ? C19 Dy1 C8 111.00(17) . . ? C19 Dy1 C20 31.16(16) . . ? C19 Dy1 C9 107.77(16) . . ? C19 Dy1 C16 51.20(15) . . ? C19 Dy1 C17 51.37(15) . . ? C19 Dy1 C18 31.35(16) . . ? C19 Dy1 C7 138.42(18) . . ? C9 Dy1 I1 130.58(12) . . ? C9 Dy1 C10 30.97(16) . . ? C9 Dy1 C6 50.89(15) . . ? C9 Dy1 C8 31.19(17) . . ? C9 Dy1 C20 138.57(17) . . ? C9 Dy1 C16 147.09(17) . . ? C9 Dy1 C17 117.71(17) . . ? C16 Dy1 I1 78.03(10) . . ? C17 Dy1 I1 99.65(11) . . ? C17 Dy1 C16 30.36(15) . . ? C18 Dy1 I1 127.98(10) . . ? C18 Dy1 C10 128.52(15) . . ? C18 Dy1 C6 137.44(16) . . ? C18 Dy1 C8 86.93(15) . . ? C18 Dy1 C20 51.04(15) . . ? C18 Dy1 C9 97.69(16) . . ? C18 Dy1 C16 50.56(15) . . ? C18 Dy1 C17 30.69(15) . . ? C7 Dy1 I1 91.92(12) . . ? C7 Dy1 C10 51.09(15) . . ? C7 Dy1 C6 30.79(16) . . ? C7 Dy1 C8 30.99(16) . . ? C7 Dy1 C20 152.74(16) . . ? C7 Dy1 C9 51.23(16) . . ? C7 Dy1 C16 123.89(15) . . ? C7 Dy1 C17 102.30(16) . . ? C7 Dy1 C18 108.90(16) . . ? C2 I1 Dy1 67.87(12) . . ? C5 N1 Dy1 143.3(3) . . ? C2 N1 Dy1 110.9(3) . . ? C2 N1 C5 104.8(4) . . ? N1 C5 I4 121.9(3) . . ? N1 C5 C4 110.9(4) . . ? C4 C5 I4 127.2(3) . . ? N1 C2 I1 119.3(3) . . ? N1 C2 C3 112.4(4) . . ? C3 C2 I1 128.3(3) . . ? C6 C10 Dy1 74.6(3) . . ? C6 C10 C9 107.6(5) . . ? C6 C10 C15 125.4(6) . . ? C9 C10 Dy1 73.8(3) . . ? C9 C10 C15 126.6(5) . . ? C15 C10 Dy1 123.4(3) . . ? C10 C6 Dy1 74.7(3) . . ? C10 C6 C11 124.2(5) . . ? C11 C6 Dy1 124.8(3) . . ? C7 C6 Dy1 73.7(3) . . ? C7 C6 C10 108.5(4) . . ? C7 C6 C11 126.7(5) . . ? C9 C8 Dy1 74.0(3) . . ? C9 C8 C13 126.0(6) . . ? C7 C8 Dy1 73.9(3) . . ? C7 C8 C9 107.2(5) . . ? C7 C8 C13 125.2(6) . . ? C13 C8 Dy1 129.1(4) . . ? 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 73.8(3) . . ? C19 C20 C25 125.3(5) . . ? C16 C20 Dy1 76.2(2) . . ? C16 C20 C19 108.6(4) . . ? C16 C20 C25 125.7(6) . . ? C25 C20 Dy1 121.4(3) . . ? C20 C19 Dy1 75.1(3) . . ? C20 C19 C18 106.5(4) . . ? C20 C19 C24 127.4(6) . . ? C18 C19 Dy1 74.7(3) . . ? C18 C19 C24 125.3(6) . . ? C24 C19 Dy1 123.3(4) . . ? C5 C4 I3 126.3(3) . . ? C5 C4 C3 107.2(4) . . ? C3 C4 I3 126.5(3) . . ? C10 C9 Dy1 75.3(3) . . ? C10 C9 C8 108.3(4) . . ? C10 C9 C14 125.4(6) . . ? C8 C9 Dy1 74.8(3) . . ? C8 C9 C14 125.9(6) . . ? C14 C9 Dy1 121.8(4) . . ? C2 C3 I2 126.7(3) . . ? C2 C3 C4 104.7(4) . . ? C4 C3 I2 128.5(4) . . ? C21 C16 Dy1 127.0(3) . . ? C20 C16 Dy1 73.1(3) . . ? C20 C16 C21 126.2(5) . . ? C17 C16 Dy1 73.8(3) . . ? C17 C16 C21 125.1(5) . . ? C17 C16 C20 107.8(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 75.8(3) . . ? C16 C17 C18 108.5(4) . . ? C16 C17 C22 125.3(5) . . ? C18 C17 Dy1 73.8(3) . . ? C18 C17 C22 125.8(5) . . ? C22 C17 Dy1 122.6(3) . . ? C19 C18 Dy1 74.0(3) . . ? C19 C18 C23 124.5(5) . . ? C17 C18 Dy1 75.5(3) . . ? C17 C18 C19 108.5(4) . . ? C17 C18 C23 125.6(5) . . ? C23 C18 Dy1 127.5(4) . . ? 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 75.5(2) . . ? C6 C7 C8 108.4(4) . . ? C6 C7 C12 125.5(6) . . ? C8 C7 Dy1 75.1(3) . . ? C8 C7 C12 125.7(6) . . ? C12 C7 Dy1 120.9(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 106.9 . . ? Cl2 C26 H26D 106.9 . . ? Cl2 C26 H26A 108.5 . . ? Cl2 C26 H26B 108.5 . . ? Cl1A C26 Cl2 121.8(7) . . ? Cl1A C26 H26C 106.9 . . ? Cl1A C26 H26D 106.9 . . ? Cl1A C26 H26A 93.7 . . ? Cl1A C26 H26B 114.8 . . ? H26C C26 H26D 106.7 . . ? H26C C26 H26A 15.6 . . ? H26C C26 H26B 94.0 . . ? H26D C26 H26A 119.6 . . ? H26D C26 H26B 13.1 . . ? H26A C26 H26B 107.5 . . ? Cl1B C26 Cl2 115.0(6) . . ? Cl1B C26 Cl1A 14.8(7) . . ? Cl1B C26 H26C 121.5 . . ? Cl1B C26 H26D 98.4 . . ? Cl1B C26 H26A 108.5 . . ? Cl1B C26 H26B 108.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 I1 3.2541(4) . ? Dy1 N1 2.386(4) . ? Dy1 C10 2.655(4) . ? Dy1 C6 2.655(4) . ? Dy1 C8 2.646(5) . ? Dy1 C20 2.644(4) . ? Dy1 C19 2.627(5) . ? Dy1 C9 2.637(5) . ? Dy1 C16 2.683(4) . ? Dy1 C17 2.657(5) . ? Dy1 C18 2.636(5) . ? Dy1 C7 2.631(4) . ? I1 C2 2.081(4) . ? I4 C5 2.077(4) . ? I3 C4 2.080(4) . ? I2 C3 2.060(4) . ? Cl2 C26 1.705(8) . ? Cl1A C26 1.656(14) . ? N1 C5 1.367(5) . ? N1 C2 1.351(5) . ? C5 C4 1.369(6) . ? C2 C3 1.380(6) . ? C10 C6 1.405(7) . ? C10 C9 1.413(7) . ? C10 C15 1.496(8) . ? C6 C11 1.519(8) . ? C6 C7 1.403(7) . ? C8 C9 1.420(8) . ? C8 C7 1.410(7) . ? C8 C13 1.508(8) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C21 C16 1.497(7) . ? C20 C19 1.416(7) . ? C20 C16 1.409(7) . ? C20 C25 1.517(7) . ? C19 C18 1.422(7) . ? C19 C24 1.499(7) . ? C4 C3 1.398(6) . ? C9 C14 1.504(8) . ? C16 C17 1.399(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 C7 1.508(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C17 C18 1.401(7) . ? C17 C22 1.513(7) . ? C18 C23 1.515(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C26 H26C 0.9700 . ? C26 H26D 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 Cl1B 1.624(12) . ? 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 13.2(6) . . . . ? Dy1 N1 C5 C4 -167.4(4) . . . . ? Dy1 N1 C2 I1 -5.9(4) . . . . ? Dy1 N1 C2 C3 172.1(3) . . . . ? Dy1 C10 C6 C11 121.9(5) . . . . ? Dy1 C10 C6 C7 -66.5(3) . . . . ? Dy1 C10 C9 C8 68.1(3) . . . . ? Dy1 C10 C9 C14 -118.8(5) . . . . ? Dy1 C6 C7 C8 -68.5(3) . . . . ? Dy1 C6 C7 C12 117.9(5) . . . . ? Dy1 C8 C9 C10 -68.4(3) . . . . ? Dy1 C8 C9 C14 118.5(5) . . . . ? Dy1 C8 C7 C6 68.8(3) . . . . ? Dy1 C8 C7 C12 -117.6(5) . . . . ? Dy1 C20 C19 C18 -68.6(3) . . . . ? Dy1 C20 C19 C24 120.7(5) . . . . ? Dy1 C20 C16 C21 -123.9(5) . . . . ? Dy1 C20 C16 C17 66.2(3) . . . . ? Dy1 C19 C18 C17 -68.3(3) . . . . ? Dy1 C19 C18 C23 124.9(5) . . . . ? Dy1 C16 C17 C18 67.2(3) . . . . ? Dy1 C16 C17 C22 -120.2(5) . . . . ? Dy1 C17 C18 C19 67.2(3) . . . . ? Dy1 C17 C18 C23 -126.1(5) . . . . ? I1 C2 C3 I2 -4.3(6) . . . . ? I1 C2 C3 C4 177.5(3) . . . . ? I4 C5 C4 I3 -1.1(6) . . . . ? I4 C5 C4 C3 -180.0(3) . . . . ? I3 C4 C3 I2 2.7(6) . . . . ? I3 C4 C3 C2 -179.2(3) . . . . ? N1 C5 C4 I3 179.6(3) . . . . ? N1 C5 C4 C3 0.7(5) . . . . ? N1 C2 C3 I2 177.9(3) . . . . ? N1 C2 C3 C4 -0.3(5) . . . . ? C5 N1 C2 I1 -177.3(3) . . . . ? C5 N1 C2 C3 0.7(5) . . . . ? C5 C4 C3 I2 -178.4(3) . . . . ? C5 C4 C3 C2 -0.2(5) . . . . ? C2 N1 C5 I4 179.8(3) . . . . ? C2 N1 C5 C4 -0.8(5) . . . . ? C10 C6 C7 Dy1 67.1(3) . . . . ? C10 C6 C7 C8 -1.4(5) . . . . ? C10 C6 C7 C12 -175.0(5) . . . . ? C6 C10 C9 Dy1 -67.6(3) . . . . ? C6 C10 C9 C8 0.5(5) . . . . ? C6 C10 C9 C14 173.7(5) . . . . ? C21 C16 C17 Dy1 124.2(5) . . . . ? C21 C16 C17 C18 -168.6(5) . . . . ? C21 C16 C17 C22 4.1(8) . . . . ? C20 C19 C18 Dy1 68.9(3) . . . . ? C20 C19 C18 C17 0.6(5) . . . . ? C20 C19 C18 C23 -166.2(5) . . . . ? C20 C16 C17 Dy1 -65.8(3) . . . . ? C20 C16 C17 C18 1.4(5) . . . . ? C20 C16 C17 C22 174.1(5) . . . . ? C19 C20 C16 Dy1 -67.2(3) . . . . ? C19 C20 C16 C21 168.8(5) . . . . ? C19 C20 C16 C17 -1.0(5) . . . . ? C9 C10 C6 Dy1 67.0(3) . . . . ? C9 C10 C6 C11 -171.1(5) . . . . ? C9 C10 C6 C7 0.5(5) . . . . ? C9 C8 C7 Dy1 -67.1(3) . . . . ? C9 C8 C7 C6 1.7(5) . . . . ? C9 C8 C7 C12 175.3(5) . . . . ? C16 C20 C19 Dy1 68.9(3) . . . . ? C16 C20 C19 C18 0.3(5) . . . . ? C16 C20 C19 C24 -170.4(5) . . . . ? C16 C17 C18 Dy1 -68.5(3) . . . . ? C16 C17 C18 C19 -1.3(5) . . . . ? C16 C17 C18 C23 165.4(5) . . . . ? C25 C20 C19 Dy1 -117.3(5) . . . . ? C25 C20 C19 C18 174.1(5) . . . . ? C25 C20 C19 C24 3.4(8) . . . . ? C25 C20 C16 Dy1 119.0(5) . . . . ? C25 C20 C16 C21 -5.0(8) . . . . ? C25 C20 C16 C17 -174.8(5) . . . . ? C15 C10 C6 Dy1 -120.3(5) . . . . ? C15 C10 C6 C11 1.6(8) . . . . ? C15 C10 C6 C7 173.2(5) . . . . ? C15 C10 C9 Dy1 119.9(5) . . . . ? C15 C10 C9 C8 -172.0(5) . . . . ? C15 C10 C9 C14 1.1(8) . . . . ? C11 C6 C7 Dy1 -121.5(5) . . . . ? C11 C6 C7 C8 170.0(5) . . . . ? C11 C6 C7 C12 -3.6(8) . . . . ? C22 C17 C18 Dy1 118.9(5) . . . . ? C22 C17 C18 C19 -173.9(5) . . . . ? C22 C17 C18 C23 -7.2(8) . . . . ? C7 C8 C9 Dy1 67.0(3) . . . . ? C7 C8 C9 C10 -1.4(5) . . . . ? C7 C8 C9 C14 -174.5(5) . . . . ? C13 C8 C9 Dy1 -127.1(5) . . . . ? C13 C8 C9 C10 164.5(5) . . . . ? C13 C8 C9 C14 -8.6(8) . . . . ? C13 C8 C7 Dy1 126.9(5) . . . . ? C13 C8 C7 C6 -164.3(5) . . . . ? C13 C8 C7 C12 9.3(8) . . . . ? C24 C19 C18 Dy1 -120.2(5) . . . . ? C24 C19 C18 C17 171.5(5) . . . . ? C24 C19 C18 C23 4.7(8) . . . . ? 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 -0.9775 -1.1022 0.3088 -0.0783 -0.0142 0.0325 -1.0686 0.9162 0.2219 0.0038 0.0040 0.0859 0.9775 1.1022 -0.3088 0.0783 0.0142 -0.0325 1.0686 -0.9162 -0.2219 -0.0038 -0.0040 -0.0859 -0.0542 -0.0347 -0.9802 -0.0100 0.0322 0.0044 0.0542 0.0347 0.9802 0.0100 -0.0322 -0.0044 -0.9601 0.9856 2.1822 0.0239 -0.0605 0.0770 0.9601 -0.9856 -2.1822 -0.0239 0.0605 -0.0770 1.1228 -0.8815 0.7583 0.0063 -0.0363 -0.0903 0.0629 1.0786 1.9169 0.0612 -0.0554 0.0178 2.1459 -0.7885 0.4929 0.0435 -0.0312 -0.1495 -0.1540 0.9397 -2.0037 0.0210 0.0736 0.0356 -1.1315 -0.1624 -1.6950 -0.0574 0.0594 0.0681 -0.9146 -0.0235 2.2257 -0.0172 -0.0696 0.0503 -7.4341 6.0188 -20.7732 -0.1415 0.7602 0.6341