#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572184.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_1572184 loop_ _publ_author_name 'Delano, Francis' 'Benner, Florian' 'Jang, Seoyun' 'Greer, Samuel M.' 'Demir, Selvan' _publ_section_title ; Construction of intermolecular \s-hole interactions in rare earth metallocene complexes using a 2,3,4,5-tetraiodopyrrolyl anion ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC03786C _journal_year 2024 _chemical_formula_moiety 'C24 H30 Dy I4 N, C H2 Cl2' _chemical_formula_sum 'C25 H32 Cl2 Dy I4 N' _chemical_formula_weight 1087.51 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-07-10 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-04-22 deposited with the CCDC. 2024-07-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.195(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.4058(3) _cell_length_b 14.4072(4) _cell_length_c 21.5108(7) _cell_measurement_reflns_used 16874 _cell_measurement_temperature 280.0(1) _cell_measurement_theta_max 30.9310 _cell_measurement_theta_min 2.8200 _cell_volume 3152.09(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 280.0(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 0.836 _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 0.0335463000 _diffrn_orient_matrix_UB_12 0.0429551000 _diffrn_orient_matrix_UB_13 0.0062366000 _diffrn_orient_matrix_UB_21 -0.0050212000 _diffrn_orient_matrix_UB_22 0.0067146000 _diffrn_orient_matrix_UB_23 -0.0330913000 _diffrn_orient_matrix_UB_31 -0.0609296000 _diffrn_orient_matrix_UB_32 0.0231094000 _diffrn_orient_matrix_UB_33 -0.0019905000 _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 0.0589 _diffrn_reflns_av_unetI/netI 0.0501 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.836 _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 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 39364 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.836 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.790 _diffrn_reflns_theta_min 2.451 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.472 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.263 _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 2.292 _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 1.164 _refine_diff_density_min -1.264 _refine_diff_density_rms 0.147 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8995 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0370 _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^)+(0.0355P)^2^+0.0196P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.0884 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6595 _reflns_number_total 8995 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP280K _cod_database_code 1572184 _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 0.208 _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_280_final.res created by SHELXL-2018/3 at 17:11:02 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 10.405762 14.407238 21.510794 90 102.1953 90 ZERR 4 0.000299 0.000412 0.00068 0 0.003 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 6.85(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.035500 0.019600 FVAR 0.62165 DY1 4 0.803939 0.716409 0.338667 11.00000 0.03029 0.03196 = 0.03147 -0.00021 0.00193 0.00397 I1 5 0.523629 0.618056 0.279072 11.00000 0.04820 0.04194 = 0.05091 0.00289 0.00846 -0.01329 I4 5 0.822490 0.939455 0.200695 11.00000 0.04887 0.05202 = 0.06349 0.00870 0.01051 -0.01437 I3 5 0.487597 0.938704 0.082472 11.00000 0.06401 0.05860 = 0.04289 0.01377 0.00774 0.02010 I2 5 0.294411 0.724870 0.128921 11.00000 0.04012 0.06960 = 0.09102 -0.00180 -0.01791 -0.00749 CL2 3 0.608885 0.626810 0.078518 11.00000 0.11820 0.10227 = 0.07842 0.00952 0.02405 0.03867 PART 1 CL1A 3 0.694931 0.443398 0.040541 10.50000 0.09408 0.09562 = 0.26625 -0.04590 0.05170 -0.01431 PART 0 N1 6 0.677803 0.774973 0.240645 11.00000 0.03071 0.04240 = 0.03247 0.00290 -0.00028 -0.00317 C5 1 0.669330 0.846052 0.197929 11.00000 0.03421 0.03628 = 0.03487 0.00448 0.00990 0.00105 C2 1 0.560739 0.730604 0.224436 11.00000 0.03447 0.03463 = 0.04243 -0.00013 0.00759 -0.00042 C10 1 0.957416 0.648780 0.265573 11.00000 0.05190 0.04595 = 0.04112 0.00521 0.01669 0.01981 C6 1 0.888303 0.571593 0.282141 11.00000 0.03530 0.04032 = 0.06017 -0.01096 0.00729 0.00753 C8 1 1.026209 0.621922 0.372551 11.00000 0.03794 0.05478 = 0.05380 -0.00761 0.00233 0.01800 C21 1 0.521902 0.735236 0.423676 11.00000 0.04871 0.09111 = 0.07981 -0.02815 0.02548 -0.00664 AFIX 137 H21A 2 0.461385 0.744195 0.383774 11.00000 -1.50000 H21B 2 0.490665 0.767649 0.456571 11.00000 -1.50000 H21C 2 0.528850 0.670203 0.433536 11.00000 -1.50000 AFIX 0 C20 1 0.678793 0.851594 0.385026 11.00000 0.05618 0.04216 = 0.03914 -0.00391 0.00687 0.01723 C19 1 0.813576 0.872231 0.402568 11.00000 0.06125 0.03882 = 0.05124 -0.00977 0.02038 -0.00445 C4 1 0.550351 0.845911 0.155885 11.00000 0.03725 0.03578 = 0.03845 0.00386 0.00511 0.00350 C9 1 1.042208 0.679632 0.321126 11.00000 0.03108 0.04927 = 0.07158 -0.00874 0.01102 0.00052 C3 1 0.479584 0.770463 0.172745 11.00000 0.03414 0.04310 = 0.03770 0.00060 -0.00196 0.00287 C16 1 0.655516 0.772512 0.419182 11.00000 0.04007 0.04246 = 0.04235 -0.00628 0.01013 0.00481 C25 1 0.576297 0.909910 0.342060 11.00000 0.10959 0.07314 = 0.05539 -0.00084 0.00443 0.05955 AFIX 137 H25A 2 0.618973 0.955455 0.320847 11.00000 -1.50000 H25B 2 0.522588 0.940570 0.366988 11.00000 -1.50000 H25C 2 0.522184 0.870773 0.311036 11.00000 -1.50000 AFIX 0 C15 1 0.953848 0.681928 0.198898 11.00000 0.09141 0.08320 = 0.06454 0.01544 0.03815 0.02857 AFIX 137 H15A 2 0.864730 0.681568 0.175090 11.00000 -1.50000 H15B 2 1.006233 0.641491 0.178860 11.00000 -1.50000 H15C 2 0.988303 0.743875 0.200203 11.00000 -1.50000 AFIX 0 C12 1 0.886310 0.477081 0.383820 11.00000 0.10741 0.05712 = 0.12090 0.03488 0.05233 0.02447 AFIX 137 H12A 2 0.907750 0.490611 0.428518 11.00000 -1.50000 H12B 2 0.930946 0.421526 0.375661 11.00000 -1.50000 H12C 2 0.793092 0.468366 0.370431 11.00000 -1.50000 AFIX 0 C11 1 0.799708 0.508850 0.233854 11.00000 0.06632 0.07733 = 0.10023 -0.04244 0.00159 0.00888 AFIX 137 H11A 2 0.748069 0.470120 0.255460 11.00000 -1.50000 H11B 2 0.853028 0.470649 0.212817 11.00000 -1.50000 H11C 2 0.742443 0.546415 0.202991 11.00000 -1.50000 AFIX 0 C14 1 1.142729 0.756101 0.324642 11.00000 0.05663 0.07362 = 0.15567 -0.01358 0.03459 -0.01342 AFIX 137 H14A 2 1.100444 0.811287 0.305294 11.00000 -1.50000 H14B 2 1.209390 0.737172 0.302514 11.00000 -1.50000 H14C 2 1.182259 0.768460 0.368354 11.00000 -1.50000 AFIX 0 C17 1 0.774854 0.743098 0.457323 11.00000 0.05204 0.04320 = 0.03760 -0.00267 0.01042 0.00903 C18 1 0.873077 0.805335 0.448012 11.00000 0.03848 0.04852 = 0.03576 -0.01027 0.00085 0.00168 C22 1 0.791076 0.666193 0.505614 11.00000 0.09292 0.07571 = 0.05478 0.02071 0.02103 0.01526 AFIX 137 H22A 2 0.709524 0.633261 0.501560 11.00000 -1.50000 H22B 2 0.815856 0.691979 0.547595 11.00000 -1.50000 H22C 2 0.858206 0.624242 0.498518 11.00000 -1.50000 AFIX 0 C7 1 0.928721 0.556362 0.347648 11.00000 0.04782 0.03209 = 0.06120 0.01201 0.01736 0.01325 C23 1 1.009234 0.813346 0.490002 11.00000 0.04656 0.10036 = 0.06875 -0.03741 -0.00896 -0.00121 AFIX 137 H23A 2 1.044339 0.752399 0.500653 11.00000 -1.50000 H23B 2 1.004029 0.846151 0.528238 11.00000 -1.50000 H23C 2 1.065601 0.846565 0.467720 11.00000 -1.50000 AFIX 0 C13 1 1.118390 0.616393 0.436447 11.00000 0.07762 0.11948 = 0.07111 -0.02060 -0.01813 0.05111 AFIX 137 H13A 2 1.157996 0.676015 0.447305 11.00000 -1.50000 H13B 2 1.185722 0.571429 0.434887 11.00000 -1.50000 H13C 2 1.070338 0.598202 0.467966 11.00000 -1.50000 AFIX 0 C24 1 0.882523 0.958513 0.385161 11.00000 0.13276 0.04820 = 0.07822 -0.01481 0.04476 -0.03312 AFIX 137 H24A 2 0.961558 0.940758 0.371936 11.00000 -1.50000 H24B 2 0.904182 0.998629 0.421506 11.00000 -1.50000 H24C 2 0.825345 0.990608 0.351057 11.00000 -1.50000 AFIX 0 C26 1 0.692462 0.559454 0.035540 11.00000 0.22186 0.08616 = 0.11797 0.02605 0.11022 0.02079 PART 1 AFIX 23 H26C 2 0.659070 0.574754 -0.008849 10.50000 -1.20000 H26D 2 0.783298 0.579905 0.045880 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.646510 0.560802 -0.008659 10.50000 -1.20000 H26B 2 0.778792 0.586360 0.037847 10.50000 -1.20000 AFIX 0 CL1B 3 0.710460 0.452802 0.058310 10.50000 0.17199 0.09159 = 0.08406 0.01732 0.02958 0.06555 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0884, GooF = S = 1.059, Restrained GooF = 1.059 for all data REM R1 = 0.0370 for 6595 Fo > 4sig(Fo) and 0.0577 for all 8995 data REM 317 parameters refined using 6 restraints END WGHT 0.0354 0.0197 REM Highest difference peak 1.164, deepest hole -1.264, 1-sigma level 0.147 Q1 1 0.2941 0.7537 0.1623 11.00000 0.05 1.16 Q2 1 0.4726 0.8978 0.0612 11.00000 0.05 0.77 Q3 1 0.8253 0.9202 0.2421 11.00000 0.05 0.63 Q4 1 0.3363 0.7421 0.1021 11.00000 0.05 0.62 Q5 1 0.7995 0.7158 0.2643 11.00000 0.05 0.56 Q6 1 1.0970 0.7210 0.1972 11.00000 0.05 0.55 Q7 1 0.5178 0.8044 0.2800 11.00000 0.05 0.54 Q8 1 0.7950 0.5033 0.0579 11.00000 0.05 0.53 Q9 1 0.7718 0.4865 0.0409 11.00000 0.05 0.52 Q10 1 0.5601 0.9557 0.0828 11.00000 0.05 0.52 Q11 1 0.8000 0.8431 0.3422 11.00000 0.05 0.49 Q12 1 0.8918 0.4733 0.2401 11.00000 0.05 0.49 Q13 1 0.9757 0.7136 0.3026 11.00000 0.05 0.48 Q14 1 0.4441 0.6030 0.2789 11.00000 0.05 0.48 Q15 1 0.7464 0.4660 0.0173 11.00000 0.05 0.47 Q16 1 0.9078 0.6266 0.2760 11.00000 0.05 0.47 ; _shelx_res_checksum 764 _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 2.282 _oxdiff_exptl_absorpt_empirical_full_min 0.598 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 0.80394(2) 0.71641(2) 0.33867(2) 0.03192(6) Uani 1 1 d . . . . . I1 I 0.52363(3) 0.61806(2) 0.27907(2) 0.04731(9) Uani 1 1 d . . . . . I4 I 0.82249(3) 0.93946(2) 0.20069(2) 0.05499(10) Uani 1 1 d . . . . . I3 I 0.48760(4) 0.93870(2) 0.08247(2) 0.05569(10) Uani 1 1 d . . . . . I2 I 0.29441(4) 0.72487(3) 0.12892(2) 0.07159(13) Uani 1 1 d . . . . . Cl2 Cl 0.6089(2) 0.62681(15) 0.07852(10) 0.0991(6) Uani 1 1 d . . . . . Cl1A Cl 0.6949(10) 0.4434(7) 0.0405(6) 0.150(5) Uani 0.5 1 d . U P A 1 N1 N 0.6778(3) 0.7750(2) 0.24064(17) 0.0362(8) Uani 1 1 d . . . . . C5 C 0.6693(4) 0.8461(3) 0.1979(2) 0.0347(9) Uani 1 1 d . . . . . C2 C 0.5607(4) 0.7306(3) 0.2244(2) 0.0373(9) Uani 1 1 d . . . . . C10 C 0.9574(5) 0.6488(3) 0.2656(2) 0.0453(11) Uani 1 1 d . . . . . C6 C 0.8883(4) 0.5716(3) 0.2821(3) 0.0457(11) Uani 1 1 d . . . . . C8 C 1.0262(5) 0.6219(3) 0.3726(3) 0.0499(12) Uani 1 1 d . . . . . C21 C 0.5219(6) 0.7352(5) 0.4237(3) 0.0715(18) Uani 1 1 d . . . . . H21A H 0.461385 0.744195 0.383774 0.107 Uiso 1 1 calc R U . . . H21B H 0.490665 0.767649 0.456571 0.107 Uiso 1 1 calc R U . . . H21C H 0.528850 0.670203 0.433536 0.107 Uiso 1 1 calc R U . . . C20 C 0.6788(5) 0.8516(3) 0.3850(2) 0.0463(11) Uani 1 1 d . . . . . C19 C 0.8136(5) 0.8722(3) 0.4026(2) 0.0492(12) Uani 1 1 d . . . . . C4 C 0.5504(4) 0.8459(3) 0.1559(2) 0.0376(9) Uani 1 1 d . . . . . C9 C 1.0422(4) 0.6796(3) 0.3211(3) 0.0506(12) Uani 1 1 d . . . . . C3 C 0.4796(4) 0.7705(3) 0.1727(2) 0.0397(9) Uani 1 1 d . . . . . C16 C 0.6555(4) 0.7725(3) 0.4192(2) 0.0414(10) Uani 1 1 d . . . . . C25 C 0.5763(7) 0.9099(4) 0.3421(3) 0.081(2) Uani 1 1 d . . . . . H25A H 0.618973 0.955455 0.320847 0.122 Uiso 1 1 calc R U . . . H25B H 0.522588 0.940570 0.366988 0.122 Uiso 1 1 calc R U . . . H25C H 0.522184 0.870773 0.311036 0.122 Uiso 1 1 calc R U . . . C15 C 0.9538(7) 0.6819(5) 0.1989(3) 0.0765(19) Uani 1 1 d . . . . . H15A H 0.864730 0.681568 0.175090 0.115 Uiso 1 1 calc R U . . . H15B H 1.006233 0.641491 0.178860 0.115 Uiso 1 1 calc R U . . . H15C H 0.988303 0.743875 0.200203 0.115 Uiso 1 1 calc R U . . . C12 C 0.8863(8) 0.4771(4) 0.3838(4) 0.091(2) Uani 1 1 d . . . . . H12A H 0.907750 0.490611 0.428518 0.136 Uiso 1 1 calc R U . . . H12B H 0.930946 0.421526 0.375661 0.136 Uiso 1 1 calc R U . . . H12C H 0.793092 0.468366 0.370431 0.136 Uiso 1 1 calc R U . . . C11 C 0.7997(6) 0.5088(5) 0.2339(4) 0.084(2) Uani 1 1 d . . . . . H11A H 0.748069 0.470120 0.255460 0.125 Uiso 1 1 calc R U . . . H11B H 0.853028 0.470649 0.212817 0.125 Uiso 1 1 calc R U . . . H11C H 0.742443 0.546415 0.202991 0.125 Uiso 1 1 calc R U . . . C14 C 1.1427(7) 0.7561(5) 0.3246(5) 0.094(3) Uani 1 1 d . . . . . H14A H 1.100444 0.811287 0.305294 0.140 Uiso 1 1 calc R U . . . H14B H 1.209390 0.737172 0.302514 0.140 Uiso 1 1 calc R U . . . H14C H 1.182259 0.768460 0.368354 0.140 Uiso 1 1 calc R U . . . C17 C 0.7749(5) 0.7431(3) 0.4573(2) 0.0441(10) Uani 1 1 d . . . . . C18 C 0.8731(4) 0.8053(3) 0.4480(2) 0.0420(10) Uani 1 1 d . . . . . C22 C 0.7911(7) 0.6662(4) 0.5056(3) 0.0737(17) Uani 1 1 d . . . . . H22A H 0.709524 0.633261 0.501560 0.111 Uiso 1 1 calc R U . . . H22B H 0.815856 0.691979 0.547595 0.111 Uiso 1 1 calc R U . . . H22C H 0.858206 0.624242 0.498518 0.111 Uiso 1 1 calc R U . . . C7 C 0.9287(5) 0.5564(3) 0.3476(3) 0.0462(11) Uani 1 1 d . . . . . C23 C 1.0092(6) 0.8133(5) 0.4900(3) 0.0750(19) Uani 1 1 d . . . . . H23A H 1.044339 0.752399 0.500653 0.113 Uiso 1 1 calc R U . . . H23B H 1.004029 0.846151 0.528238 0.113 Uiso 1 1 calc R U . . . H23C H 1.065601 0.846565 0.467720 0.113 Uiso 1 1 calc R U . . . C13 C 1.1184(7) 0.6164(6) 0.4364(3) 0.094(3) Uani 1 1 d . . . . . H13A H 1.157996 0.676015 0.447305 0.142 Uiso 1 1 calc R U . . . H13B H 1.185722 0.571429 0.434887 0.142 Uiso 1 1 calc R U . . . H13C H 1.070338 0.598202 0.467966 0.142 Uiso 1 1 calc R U . . . C24 C 0.8825(8) 0.9585(4) 0.3852(3) 0.083(2) Uani 1 1 d . . . . . H24A H 0.961558 0.940758 0.371936 0.125 Uiso 1 1 calc R U . . . H24B H 0.904182 0.998629 0.421506 0.125 Uiso 1 1 calc R U . . . H24C H 0.825345 0.990608 0.351057 0.125 Uiso 1 1 calc R U . . . C26 C 0.6925(12) 0.5595(5) 0.0355(5) 0.131(4) Uani 1 1 d . . . . . H26C H 0.659070 0.574754 -0.008849 0.157 Uiso 0.5 1 calc R U P A 1 H26D H 0.783298 0.579905 0.045880 0.157 Uiso 0.5 1 calc R U P A 1 H26A H 0.646510 0.560802 -0.008659 0.157 Uiso 0.5 1 calc R U P A -1 H26B H 0.778792 0.586360 0.037847 0.157 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7105(11) 0.4528(6) 0.0583(4) 0.116(3) 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 0.03029(10) 0.03196(11) 0.03147(11) -0.00021(7) 0.00193(7) 0.00397(7) I1 0.04820(18) 0.04194(17) 0.05091(19) 0.00289(13) 0.00846(14) -0.01329(12) I4 0.04887(19) 0.05202(19) 0.0635(2) 0.00870(15) 0.01051(16) -0.01437(13) I3 0.0640(2) 0.0586(2) 0.04289(19) 0.01377(15) 0.00774(16) 0.02010(15) I2 0.04012(19) 0.0696(2) 0.0910(3) -0.0018(2) -0.01791(18) -0.00749(15) Cl2 0.1182(16) 0.1023(14) 0.0784(13) 0.0095(11) 0.0240(11) 0.0387(12) Cl1A 0.094(4) 0.096(5) 0.266(13) -0.046(6) 0.052(6) -0.014(3) N1 0.0307(18) 0.042(2) 0.0325(19) 0.0029(15) -0.0003(14) -0.0032(14) C5 0.034(2) 0.036(2) 0.035(2) 0.0045(17) 0.0099(17) 0.0011(16) C2 0.034(2) 0.035(2) 0.042(2) -0.0001(18) 0.0076(19) -0.0004(16) C10 0.052(3) 0.046(3) 0.041(3) 0.005(2) 0.017(2) 0.020(2) C6 0.035(2) 0.040(2) 0.060(3) -0.011(2) 0.007(2) 0.0075(18) C8 0.038(2) 0.055(3) 0.054(3) -0.008(2) 0.002(2) 0.018(2) C21 0.049(3) 0.091(4) 0.080(5) -0.028(4) 0.025(3) -0.007(3) C20 0.056(3) 0.042(2) 0.039(2) -0.0039(19) 0.007(2) 0.017(2) C19 0.061(3) 0.039(2) 0.051(3) -0.010(2) 0.020(2) -0.004(2) C4 0.037(2) 0.036(2) 0.038(2) 0.0039(18) 0.0051(18) 0.0035(16) C9 0.031(2) 0.049(3) 0.072(4) -0.009(2) 0.011(2) 0.0005(19) C3 0.034(2) 0.043(2) 0.038(2) 0.0006(19) -0.0020(18) 0.0029(17) C16 0.040(2) 0.042(2) 0.042(3) -0.0063(19) 0.010(2) 0.0048(18) C25 0.110(5) 0.073(4) 0.055(4) -0.001(3) 0.004(3) 0.060(4) C15 0.091(5) 0.083(4) 0.065(4) 0.015(3) 0.038(4) 0.029(4) C12 0.107(6) 0.057(4) 0.121(7) 0.035(4) 0.052(5) 0.024(4) C11 0.066(4) 0.077(4) 0.100(5) -0.042(4) 0.002(4) 0.009(3) C14 0.057(4) 0.074(4) 0.156(8) -0.014(5) 0.035(5) -0.013(3) C17 0.052(3) 0.043(2) 0.038(2) -0.0027(19) 0.010(2) 0.009(2) C18 0.038(2) 0.049(2) 0.036(2) -0.010(2) 0.0008(18) 0.0017(18) C22 0.093(5) 0.076(4) 0.055(4) 0.021(3) 0.021(3) 0.015(3) C7 0.048(3) 0.032(2) 0.061(3) 0.012(2) 0.017(2) 0.0132(18) C23 0.047(3) 0.100(5) 0.069(4) -0.037(4) -0.009(3) -0.001(3) C13 0.078(5) 0.119(6) 0.071(5) -0.021(4) -0.018(4) 0.051(4) C24 0.133(6) 0.048(3) 0.078(5) -0.015(3) 0.045(5) -0.033(4) C26 0.222(12) 0.086(5) 0.118(8) 0.026(5) 0.110(8) 0.021(6) Cl1B 0.172(8) 0.092(5) 0.084(3) 0.017(3) 0.030(4) 0.066(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 -8 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 61.73(8) . . ? N1 Dy1 C10 83.91(13) . . ? N1 Dy1 C6 92.66(14) . . ? N1 Dy1 C8 135.14(14) . . ? N1 Dy1 C20 81.41(14) . . ? N1 Dy1 C19 96.50(15) . . ? N1 Dy1 C9 107.59(15) . . ? N1 Dy1 C16 100.36(13) . . ? N1 Dy1 C17 130.00(13) . . ? N1 Dy1 C18 127.59(13) . . ? N1 Dy1 C7 122.98(15) . . ? C10 Dy1 I1 102.03(12) . . ? C10 Dy1 C6 30.82(15) . . ? C10 Dy1 C20 153.88(15) . . ? C10 Dy1 C16 175.11(14) . . ? C10 Dy1 C17 145.75(14) . . ? C6 Dy1 I1 80.38(10) . . ? C6 Dy1 C16 145.59(15) . . ? C6 Dy1 C17 131.93(15) . . ? C8 Dy1 I1 122.86(12) . . ? C8 Dy1 C10 51.27(15) . . ? C8 Dy1 C6 50.85(15) . . ? C8 Dy1 C20 138.01(15) . . ? C8 Dy1 C16 124.50(15) . . ? C8 Dy1 C17 94.58(15) . . ? C20 Dy1 I1 89.85(12) . . ? C20 Dy1 C6 170.14(15) . . ? C20 Dy1 C16 30.55(14) . . ? C20 Dy1 C17 50.86(14) . . ? C19 Dy1 I1 120.74(12) . . ? C19 Dy1 C10 131.60(16) . . ? C19 Dy1 C6 158.83(16) . . ? C19 Dy1 C8 111.16(17) . . ? C19 Dy1 C20 30.89(16) . . ? C19 Dy1 C9 108.28(16) . . ? C19 Dy1 C16 50.66(14) . . ? C19 Dy1 C17 51.19(15) . . ? C19 Dy1 C18 31.26(15) . . ? C19 Dy1 C7 138.36(17) . . ? C9 Dy1 I1 130.35(11) . . ? C9 Dy1 C10 30.67(16) . . ? C9 Dy1 C6 50.61(15) . . ? C9 Dy1 C8 31.18(16) . . ? C9 Dy1 C20 138.76(16) . . ? C9 Dy1 C16 147.22(16) . . ? C9 Dy1 C17 117.83(16) . . ? C9 Dy1 C18 97.89(15) . . ? C16 Dy1 I1 78.15(10) . . ? C17 Dy1 I1 99.60(11) . . ? C17 Dy1 C16 30.44(14) . . ? C18 Dy1 I1 127.96(10) . . ? C18 Dy1 C10 128.41(15) . . ? C18 Dy1 C6 137.27(15) . . ? C18 Dy1 C8 86.93(15) . . ? C18 Dy1 C20 51.09(15) . . ? C18 Dy1 C16 50.46(14) . . ? C18 Dy1 C17 30.74(15) . . ? C7 Dy1 I1 91.99(11) . . ? C7 Dy1 C10 51.13(15) . . ? C7 Dy1 C6 30.70(16) . . ? C7 Dy1 C8 30.88(16) . . ? C7 Dy1 C20 152.78(15) . . ? C7 Dy1 C9 51.03(15) . . ? C7 Dy1 C16 124.04(15) . . ? C7 Dy1 C17 102.15(15) . . ? C7 Dy1 C18 108.79(16) . . ? C2 I1 Dy1 68.04(12) . . ? C5 N1 Dy1 143.5(3) . . ? C2 N1 Dy1 110.9(3) . . ? C2 N1 C5 104.7(3) . . ? N1 C5 I4 121.8(3) . . ? N1 C5 C4 111.3(4) . . ? C4 C5 I4 126.9(3) . . ? N1 C2 I1 119.0(3) . . ? N1 C2 C3 112.2(4) . . ? C3 C2 I1 128.8(3) . . ? C6 C10 Dy1 74.7(3) . . ? C6 C10 C15 125.4(5) . . ? C9 C10 Dy1 74.2(3) . . ? C9 C10 C6 107.3(4) . . ? C9 C10 C15 126.7(5) . . ? C15 C10 Dy1 123.5(3) . . ? C10 C6 Dy1 74.4(2) . . ? C10 C6 C11 124.1(5) . . ? C11 C6 Dy1 124.4(3) . . ? C7 C6 Dy1 73.8(3) . . ? C7 C6 C10 108.5(4) . . ? C7 C6 C11 126.9(5) . . ? C9 C8 Dy1 74.0(3) . . ? C9 C8 C13 125.9(6) . . ? C7 C8 Dy1 73.9(3) . . ? C7 C8 C9 106.9(4) . . ? C7 C8 C13 125.6(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 73.4(3) . . ? C19 C20 C25 125.6(5) . . ? C16 C20 Dy1 75.7(2) . . ? C16 C20 C19 107.7(4) . . ? C16 C20 C25 126.4(5) . . ? C25 C20 Dy1 121.2(3) . . ? C20 C19 Dy1 75.7(3) . . ? C20 C19 C18 107.9(4) . . ? C20 C19 C24 127.1(5) . . ? C18 C19 Dy1 75.1(2) . . ? C18 C19 C24 124.4(5) . . ? C24 C19 Dy1 122.6(3) . . ? C5 C4 I3 126.8(3) . . ? C5 C4 C3 106.3(4) . . ? C3 C4 I3 126.9(3) . . ? C10 C9 Dy1 75.2(3) . . ? C10 C9 C8 108.8(4) . . ? C10 C9 C14 125.4(6) . . ? C8 C9 Dy1 74.8(3) . . ? C8 C9 C14 125.6(6) . . ? C14 C9 Dy1 120.5(4) . . ? C2 C3 I2 126.3(3) . . ? C2 C3 C4 105.5(4) . . ? C4 C3 I2 128.2(3) . . ? C21 C16 Dy1 126.7(3) . . ? C20 C16 Dy1 73.7(3) . . ? C20 C16 C21 125.7(5) . . ? C17 C16 Dy1 74.1(3) . . ? C17 C16 C21 124.6(5) . . ? C17 C16 C20 108.8(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 75.4(3) . . ? C16 C17 C18 107.7(4) . . ? C16 C17 C22 125.7(5) . . ? C18 C17 Dy1 73.9(3) . . ? C18 C17 C22 126.1(5) . . ? C22 C17 Dy1 122.5(3) . . ? C19 C18 Dy1 73.7(3) . . ? C19 C18 C23 125.2(5) . . ? C17 C18 Dy1 75.4(3) . . ? C17 C18 C19 107.9(4) . . ? C17 C18 C23 125.5(5) . . ? C23 C18 Dy1 127.8(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 75.5(2) . . ? C6 C7 C8 108.5(4) . . ? C6 C7 C12 125.6(6) . . ? C8 C7 Dy1 75.2(2) . . ? C8 C7 C12 125.5(6) . . ? C12 C7 Dy1 120.7(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 106.7 . . ? Cl2 C26 H26D 106.7 . . ? Cl2 C26 H26A 108.6 . . ? Cl2 C26 H26B 108.6 . . ? Cl1A C26 Cl2 122.5(6) . . ? Cl1A C26 H26C 106.7 . . ? Cl1A C26 H26D 106.7 . . ? Cl1A C26 H26A 94.6 . . ? Cl1A C26 H26B 113.2 . . ? H26C C26 H26D 106.6 . . ? H26C C26 H26A 14.2 . . ? H26C C26 H26B 95.4 . . ? H26D C26 H26A 118.3 . . ? H26D C26 H26B 11.4 . . ? H26A C26 H26B 107.6 . . ? Cl1B C26 Cl2 114.8(6) . . ? Cl1B C26 Cl1A 14.0(7) . . ? Cl1B C26 H26C 120.7 . . ? Cl1B C26 H26D 100.1 . . ? Cl1B C26 H26A 108.6 . . ? Cl1B C26 H26B 108.6 . . ? 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 3.2526(4) . ? Dy1 N1 2.390(3) . ? Dy1 C10 2.652(4) . ? Dy1 C6 2.656(4) . ? Dy1 C8 2.650(4) . ? Dy1 C20 2.652(4) . ? Dy1 C19 2.623(4) . ? Dy1 C9 2.639(4) . ? Dy1 C16 2.677(4) . ? Dy1 C17 2.661(5) . ? Dy1 C18 2.641(4) . ? Dy1 C7 2.633(4) . ? I1 C2 2.086(4) . ? I4 C5 2.077(4) . ? I3 C4 2.067(4) . ? I2 C3 2.065(4) . ? Cl2 C26 1.701(8) . ? Cl1A C26 1.675(13) . ? N1 C5 1.366(5) . ? N1 C2 1.354(5) . ? C5 C4 1.370(6) . ? C2 C3 1.372(6) . ? C10 C6 1.410(7) . ? C10 C9 1.400(7) . ? C10 C15 1.505(7) . ? C6 C11 1.530(8) . ? C6 C7 1.400(7) . ? C8 C9 1.421(8) . ? C8 C7 1.407(7) . ? C8 C13 1.503(8) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C21 C16 1.512(7) . ? C20 C19 1.405(7) . ? C20 C16 1.404(7) . ? C20 C25 1.510(7) . ? C19 C18 1.418(7) . ? C19 C24 1.521(7) . ? C4 C3 1.403(6) . ? C9 C14 1.510(8) . ? C16 C17 1.402(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 1.500(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 1.405(7) . ? C17 C22 1.504(7) . ? C18 C23 1.515(7) . ? 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 1.612(11) . ? 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 12.5(6) . . . . ? Dy1 N1 C5 C4 -167.2(4) . . . . ? Dy1 N1 C2 I1 -6.0(4) . . . . ? Dy1 N1 C2 C3 172.4(3) . . . . ? Dy1 C10 C6 C11 121.3(5) . . . . ? Dy1 C10 C6 C7 -66.5(3) . . . . ? Dy1 C10 C9 C8 67.9(3) . . . . ? Dy1 C10 C9 C14 -117.2(5) . . . . ? Dy1 C6 C7 C8 -68.6(3) . . . . ? Dy1 C6 C7 C12 117.6(5) . . . . ? Dy1 C8 C9 C10 -68.1(3) . . . . ? Dy1 C8 C9 C14 116.9(5) . . . . ? Dy1 C8 C7 C6 68.9(3) . . . . ? Dy1 C8 C7 C12 -117.4(5) . . . . ? Dy1 C20 C19 C18 -68.8(3) . . . . ? Dy1 C20 C19 C24 120.2(5) . . . . ? Dy1 C20 C16 C21 -123.9(5) . . . . ? Dy1 C20 C16 C17 66.4(3) . . . . ? Dy1 C19 C18 C17 -68.3(3) . . . . ? Dy1 C19 C18 C23 125.0(5) . . . . ? Dy1 C16 C17 C18 67.4(3) . . . . ? Dy1 C16 C17 C22 -119.8(5) . . . . ? Dy1 C17 C18 C19 67.1(3) . . . . ? Dy1 C17 C18 C23 -126.2(5) . . . . ? I1 C2 C3 I2 -3.9(6) . . . . ? I1 C2 C3 C4 177.4(3) . . . . ? I4 C5 C4 I3 0.0(6) . . . . ? I4 C5 C4 C3 -179.8(3) . . . . ? I3 C4 C3 I2 2.1(6) . . . . ? I3 C4 C3 C2 -179.3(3) . . . . ? N1 C5 C4 I3 179.7(3) . . . . ? N1 C5 C4 C3 -0.2(5) . . . . ? N1 C2 C3 I2 177.9(3) . . . . ? N1 C2 C3 C4 -0.8(5) . . . . ? C5 N1 C2 I1 -177.7(3) . . . . ? C5 N1 C2 C3 0.7(5) . . . . ? C5 C4 C3 I2 -178.1(3) . . . . ? C5 C4 C3 C2 0.5(5) . . . . ? C2 N1 C5 I4 179.3(3) . . . . ? C2 N1 C5 C4 -0.3(5) . . . . ? C10 C6 C7 Dy1 66.9(3) . . . . ? C10 C6 C7 C8 -1.7(5) . . . . ? C10 C6 C7 C12 -175.5(5) . . . . ? C6 C10 C9 Dy1 -68.0(3) . . . . ? C6 C10 C9 C8 -0.1(5) . . . . ? C6 C10 C9 C14 174.9(5) . . . . ? C21 C16 C17 Dy1 124.0(5) . . . . ? C21 C16 C17 C18 -168.6(4) . . . . ? C21 C16 C17 C22 4.2(8) . . . . ? C20 C19 C18 Dy1 69.2(3) . . . . ? C20 C19 C18 C17 1.0(5) . . . . ? C20 C19 C18 C23 -165.8(5) . . . . ? C20 C16 C17 Dy1 -66.1(3) . . . . ? C20 C16 C17 C18 1.2(5) . . . . ? C20 C16 C17 C22 174.1(5) . . . . ? C19 C20 C16 Dy1 -67.0(3) . . . . ? C19 C20 C16 C21 169.1(5) . . . . ? C19 C20 C16 C17 -0.6(5) . . . . ? C9 C10 C6 Dy1 67.6(3) . . . . ? C9 C10 C6 C11 -171.1(5) . . . . ? C9 C10 C6 C7 1.1(5) . . . . ? C9 C8 C7 Dy1 -67.2(3) . . . . ? C9 C8 C7 C6 1.6(5) . . . . ? C9 C8 C7 C12 175.4(5) . . . . ? C16 C20 C19 Dy1 68.6(3) . . . . ? C16 C20 C19 C18 -0.2(5) . . . . ? C16 C20 C19 C24 -171.2(5) . . . . ? C16 C17 C18 Dy1 -68.4(3) . . . . ? C16 C17 C18 C19 -1.4(5) . . . . ? C16 C17 C18 C23 165.3(5) . . . . ? C25 C20 C19 Dy1 -116.8(5) . . . . ? C25 C20 C19 C18 174.4(4) . . . . ? C25 C20 C19 C24 3.4(8) . . . . ? C25 C20 C16 Dy1 118.5(5) . . . . ? C25 C20 C16 C21 -5.4(8) . . . . ? C25 C20 C16 C17 -175.1(5) . . . . ? C15 C10 C6 Dy1 -120.5(5) . . . . ? C15 C10 C6 C11 0.8(7) . . . . ? C15 C10 C6 C7 173.0(4) . . . . ? C15 C10 C9 Dy1 120.3(5) . . . . ? C15 C10 C9 C8 -171.8(5) . . . . ? C15 C10 C9 C14 3.1(8) . . . . ? C11 C6 C7 Dy1 -121.1(5) . . . . ? C11 C6 C7 C8 170.2(5) . . . . ? C11 C6 C7 C12 -3.5(8) . . . . ? C22 C17 C18 Dy1 118.8(5) . . . . ? C22 C17 C18 C19 -174.2(5) . . . . ? C22 C17 C18 C23 -7.5(8) . . . . ? C7 C8 C9 Dy1 67.2(3) . . . . ? C7 C8 C9 C10 -1.0(5) . . . . ? C7 C8 C9 C14 -175.9(5) . . . . ? C13 C8 C9 Dy1 -127.0(5) . . . . ? C13 C8 C9 C10 164.9(5) . . . . ? C13 C8 C9 C14 -10.0(8) . . . . ? C13 C8 C7 Dy1 126.9(5) . . . . ? C13 C8 C7 C6 -164.3(5) . . . . ? C13 C8 C7 C12 9.5(8) . . . . ? C24 C19 C18 Dy1 -119.5(5) . . . . ? C24 C19 C18 C17 172.2(5) . . . . ? C24 C19 C18 C23 5.5(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 -0.9685 -1.1179 0.3480 -0.0783 -0.0142 0.0325 -1.0765 0.8963 0.2236 0.0038 0.0040 0.0859 0.9685 1.1179 -0.3480 0.0783 0.0142 -0.0325 1.0765 -0.8963 -0.2236 -0.0038 -0.0040 -0.0859 -0.0587 -0.0465 -0.9750 -0.0100 0.0322 0.0044 0.0587 0.0465 0.9750 0.0100 -0.0322 -0.0044 -0.9591 0.9893 2.1737 0.0239 -0.0605 0.0770 0.9591 -0.9893 -2.1737 -0.0239 0.0605 -0.0770 1.1352 -0.8498 0.7514 0.0063 -0.0363 -0.0903 0.0634 1.1001 1.8878 0.0612 -0.0554 0.0178 2.1577 -0.7390 0.4656 0.0435 -0.0312 -0.1495 -0.1715 0.9141 -2.0123 0.0210 0.0736 0.0356 -1.1399 -0.2038 -1.6642 -0.0574 0.0594 0.0681 -0.9050 -0.0178 2.2359 -0.0172 -0.0696 0.0503 -7.5933 5.6370 -20.6768 -0.1415 0.7602 0.6341