#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572177.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_1572177 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 102.327(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.4206(3) _cell_length_b 14.4229(4) _cell_length_c 21.5777(7) _cell_measurement_reflns_used 16057 _cell_measurement_temperature 300.0(1) _cell_measurement_theta_max 29.3590 _cell_measurement_theta_min 2.8180 _cell_volume 3168.26(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_environment N~2~ _diffrn_ambient_temperature 300.0(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 0.843 _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 -0.0346698000 _diffrn_orient_matrix_UB_12 0.0422462000 _diffrn_orient_matrix_UB_13 -0.0074761000 _diffrn_orient_matrix_UB_21 0.0036720000 _diffrn_orient_matrix_UB_22 0.0082166000 _diffrn_orient_matrix_UB_23 0.0327415000 _diffrn_orient_matrix_UB_31 0.0603196000 _diffrn_orient_matrix_UB_32 0.0238048000 _diffrn_orient_matrix_UB_33 0.0019873000 _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 0.0641 _diffrn_reflns_av_unetI/netI 0.0553 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.843 _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 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 39450 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.843 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.716 _diffrn_reflns_theta_min 2.449 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.439 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.256 _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 2.280 _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 1.156 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.141 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 9054 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0394 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.0956 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6424 _reflns_number_total 9054 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP300K _cod_original_cell_volume 3168.25(16) _cod_database_code 1572177 _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 0.535 _shelx_estimated_absorpt_t_min 0.210 _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_300_final.res created by SHELXL-2018/3 at 17:20:51 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 10.420593 14.422932 21.577677 90 102.3274 90 ZERR 4 0.000296 0.000398 0.000682 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. 80 0 0 PLAN 17 SIZE 0.111 0.275 0.353 TEMP 26.85(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.037700 FVAR 0.62086 DY1 4 0.803971 0.716642 0.338498 11.00000 0.03324 0.03477 = 0.03527 -0.00021 0.00178 0.00437 I1 5 0.523430 0.618434 0.278607 11.00000 0.05356 0.04554 = 0.05635 0.00306 0.00907 -0.01455 I4 5 0.822728 0.939321 0.200886 11.00000 0.05409 0.05731 = 0.07029 0.00941 0.01170 -0.01600 I3 5 0.488385 0.938791 0.082707 11.00000 0.07147 0.06315 = 0.04769 0.01534 0.00871 0.02200 I2 5 0.294830 0.725432 0.128664 11.00000 0.04418 0.07519 = 0.09942 -0.00244 -0.01962 -0.00760 CL2 3 0.608613 0.626900 0.078061 11.00000 0.13277 0.11365 = 0.08616 0.00948 0.02484 0.04214 PART 1 CL1A 3 0.693894 0.445716 0.040317 10.50000 0.09977 0.10541 = 0.28377 -0.03936 0.06058 -0.00731 PART 0 N1 6 0.678269 0.775110 0.240834 11.00000 0.03585 0.04357 = 0.03781 0.00288 0.00221 -0.00339 C5 1 0.669566 0.845883 0.198133 11.00000 0.03972 0.03860 = 0.03992 0.00453 0.00666 -0.00003 C2 1 0.561098 0.729943 0.223762 11.00000 0.03944 0.03521 = 0.04928 0.00097 0.00750 -0.00380 C10 1 0.958434 0.649352 0.266048 11.00000 0.05329 0.05621 = 0.04417 0.00822 0.01498 0.01509 C6 1 0.887923 0.572060 0.282104 11.00000 0.04209 0.04141 = 0.06282 -0.01548 0.00390 0.00697 C8 1 1.026860 0.622038 0.372454 11.00000 0.05001 0.05698 = 0.05064 -0.00515 0.00196 0.02223 C21 1 0.522319 0.734637 0.423954 11.00000 0.05175 0.09873 = 0.07912 -0.02959 0.02116 -0.00907 AFIX 137 H21A 2 0.461111 0.744673 0.384469 11.00000 -1.50000 H21B 2 0.492405 0.766386 0.457336 11.00000 -1.50000 H21C 2 0.528742 0.669442 0.433055 11.00000 -1.50000 AFIX 0 C20 1 0.678398 0.851210 0.384302 11.00000 0.06975 0.04480 = 0.03912 -0.00298 0.00565 0.02012 C19 1 0.814158 0.872349 0.402771 11.00000 0.06534 0.03869 = 0.05046 -0.01079 0.01913 -0.00631 C4 1 0.551197 0.845279 0.156169 11.00000 0.03978 0.04056 = 0.04148 0.00064 0.00533 0.00570 C9 1 1.042262 0.679316 0.321778 11.00000 0.03740 0.04876 = 0.08190 -0.00547 0.01483 0.00265 C3 1 0.479255 0.770668 0.172622 11.00000 0.03670 0.04487 = 0.04326 -0.00533 0.00119 0.00025 C16 1 0.655797 0.771528 0.419225 11.00000 0.04341 0.04851 = 0.04642 -0.00494 0.00962 0.00460 C25 1 0.575881 0.909323 0.342581 11.00000 0.10260 0.08562 = 0.05962 0.00364 0.00469 0.05554 AFIX 137 H25A 2 0.613746 0.940010 0.311278 11.00000 -1.50000 H25B 2 0.543364 0.954773 0.367883 11.00000 -1.50000 H25C 2 0.504830 0.870433 0.321841 11.00000 -1.50000 AFIX 0 C15 1 0.954041 0.680929 0.199868 11.00000 0.10892 0.09429 = 0.06660 0.01684 0.04478 0.03311 AFIX 137 H15A 2 0.864906 0.679793 0.176177 11.00000 -1.50000 H15B 2 1.006655 0.640378 0.180223 11.00000 -1.50000 H15C 2 0.987733 0.742958 0.200573 11.00000 -1.50000 AFIX 0 C12 1 0.886264 0.477053 0.383926 11.00000 0.10717 0.06228 = 0.12916 0.03567 0.06050 0.02243 AFIX 137 H12A 2 0.903720 0.492454 0.428218 11.00000 -1.50000 H12B 2 0.934270 0.422192 0.377842 11.00000 -1.50000 H12C 2 0.793932 0.466109 0.369094 11.00000 -1.50000 AFIX 0 C11 1 0.800190 0.509284 0.234173 11.00000 0.07424 0.08678 = 0.10063 -0.04724 0.00133 0.00588 AFIX 137 H11A 2 0.747011 0.471757 0.255536 11.00000 -1.50000 H11B 2 0.853779 0.469982 0.214203 11.00000 -1.50000 H11C 2 0.744502 0.546562 0.202581 11.00000 -1.50000 AFIX 0 C14 1 1.142371 0.755865 0.324900 11.00000 0.06255 0.07564 = 0.17694 -0.02381 0.03973 -0.01920 AFIX 137 H14A 2 1.100325 0.810166 0.304179 11.00000 -1.50000 H14B 2 1.210336 0.736073 0.304049 11.00000 -1.50000 H14C 2 1.180073 0.770006 0.368456 11.00000 -1.50000 AFIX 0 C17 1 0.775769 0.743397 0.456615 11.00000 0.05644 0.04313 = 0.03641 -0.00158 0.00770 0.00960 C18 1 0.873335 0.805660 0.447663 11.00000 0.04386 0.05250 = 0.04229 -0.01135 0.00217 0.00141 C22 1 0.793123 0.666412 0.505771 11.00000 0.10701 0.07421 = 0.06357 0.02471 0.02465 0.02059 AFIX 137 H22A 2 0.713721 0.630718 0.500188 11.00000 -1.50000 H22B 2 0.812341 0.692980 0.547525 11.00000 -1.50000 H22C 2 0.864273 0.626898 0.500658 11.00000 -1.50000 AFIX 0 C7 1 0.928364 0.556025 0.347299 11.00000 0.05231 0.03668 = 0.06478 0.01140 0.01760 0.01655 C23 1 1.009681 0.813503 0.489655 11.00000 0.05585 0.11371 = 0.08404 -0.04658 -0.00747 -0.00179 AFIX 137 H23A 2 1.045630 0.752609 0.499279 11.00000 -1.50000 H23B 2 1.004349 0.844716 0.528320 11.00000 -1.50000 H23C 2 1.065320 0.848147 0.467930 11.00000 -1.50000 AFIX 0 C13 1 1.116365 0.616722 0.436462 11.00000 0.08852 0.14398 = 0.06492 -0.02198 -0.02383 0.06490 AFIX 137 H13A 2 1.156310 0.676152 0.447379 11.00000 -1.50000 H13B 2 1.183455 0.571357 0.435761 11.00000 -1.50000 H13C 2 1.066828 0.599241 0.467363 11.00000 -1.50000 AFIX 0 C24 1 0.881459 0.959605 0.385291 11.00000 0.14538 0.05923 = 0.10099 -0.01559 0.06285 -0.03509 AFIX 137 H24A 2 0.964926 0.943395 0.376254 11.00000 -1.50000 H24B 2 0.894444 1.002494 0.420096 11.00000 -1.50000 H24C 2 0.827326 0.987792 0.348530 11.00000 -1.50000 AFIX 0 C26 1 0.691377 0.560260 0.035458 11.00000 0.23217 0.10069 = 0.11287 0.03018 0.10167 0.01703 PART 1 AFIX 23 H26C 2 0.657833 0.575606 -0.008807 10.50000 -1.20000 H26D 2 0.782117 0.580723 0.045804 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.644731 0.561346 -0.008543 10.50000 -1.20000 H26B 2 0.777096 0.587761 0.037412 10.50000 -1.20000 AFIX 0 CL1B 3 0.711910 0.452591 0.058181 10.50000 0.20114 0.10439 = 0.09018 0.02338 0.02734 0.07689 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0956, GooF = S = 1.050, Restrained GooF = 1.050 for all data REM R1 = 0.0394 for 6424 Fo > 4sig(Fo) and 0.0626 for all 9054 data REM 317 parameters refined using 6 restraints END WGHT 0.0377 0.0000 REM Highest difference peak 1.156, deepest hole -1.081, 1-sigma level 0.141 Q1 1 0.2960 0.7531 0.1617 11.00000 0.05 1.16 Q2 1 0.4754 0.8968 0.0622 11.00000 0.05 1.01 Q3 1 0.5747 0.9561 0.0830 11.00000 0.05 0.93 Q4 1 0.8937 0.7364 0.3385 11.00000 0.05 0.77 Q5 1 0.4482 0.6167 0.2680 11.00000 0.05 0.77 Q6 1 0.7653 0.4868 0.0367 11.00000 0.05 0.68 Q7 1 0.7226 0.7202 0.3406 11.00000 0.05 0.64 Q8 1 0.3644 0.7369 0.1125 11.00000 0.05 0.59 Q9 1 0.8386 0.6195 0.3411 11.00000 0.05 0.57 Q10 1 0.7116 0.6369 0.0664 11.00000 0.05 0.53 Q11 1 0.8330 0.8984 0.2402 11.00000 0.05 0.52 Q12 1 0.1157 0.7821 0.1194 11.00000 0.05 0.49 Q13 1 0.7672 0.6385 0.3358 11.00000 0.05 0.49 Q14 1 0.9495 0.6027 0.2795 11.00000 0.05 0.47 Q15 1 0.8106 0.5138 0.0542 11.00000 0.05 0.47 Q16 1 0.6771 0.4660 0.3615 11.00000 0.05 0.46 Q17 1 0.1911 0.7226 0.1364 11.00000 0.05 0.46 ; _shelx_res_checksum 24601 _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 2.611 _oxdiff_exptl_absorpt_empirical_full_min 0.617 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 0.80397(2) 0.71664(2) 0.33850(2) 0.03525(7) Uani 1 1 d . . . . . I1 I 0.52343(3) 0.61843(2) 0.27861(2) 0.05221(10) Uani 1 1 d . . . . . I4 I 0.82273(4) 0.93932(2) 0.20089(2) 0.06080(11) Uani 1 1 d . . . . . I3 I 0.48839(4) 0.93879(3) 0.08271(2) 0.06137(11) Uani 1 1 d . . . . . I2 I 0.29483(4) 0.72543(3) 0.12866(3) 0.07814(14) Uani 1 1 d . . . . . Cl2 Cl 0.6086(3) 0.62690(16) 0.07806(11) 0.1106(7) Uani 1 1 d . . . . . Cl1A Cl 0.6939(10) 0.4457(8) 0.0403(7) 0.160(5) Uani 0.5 1 d . U P A 1 N1 N 0.6783(4) 0.7751(2) 0.24083(18) 0.0399(8) Uani 1 1 d . . . . . C5 C 0.6696(4) 0.8459(3) 0.1981(2) 0.0397(9) Uani 1 1 d . . . . . C2 C 0.5611(4) 0.7299(3) 0.2238(2) 0.0416(10) Uani 1 1 d . . . . . C10 C 0.9584(5) 0.6494(4) 0.2660(2) 0.0505(12) Uani 1 1 d . . . . . C6 C 0.8879(5) 0.5721(3) 0.2821(3) 0.0499(12) Uani 1 1 d . . . . . C8 C 1.0269(5) 0.6220(4) 0.3725(3) 0.0539(13) Uani 1 1 d . . . . . C21 C 0.5223(6) 0.7346(5) 0.4240(3) 0.0755(19) Uani 1 1 d . . . . . H21A H 0.461111 0.744673 0.384469 0.113 Uiso 1 1 calc R U . . . H21B H 0.492405 0.766386 0.457336 0.113 Uiso 1 1 calc R U . . . H21C H 0.528742 0.669442 0.433055 0.113 Uiso 1 1 calc R U . . . C20 C 0.6784(6) 0.8512(3) 0.3843(2) 0.0521(12) Uani 1 1 d . . . . . C19 C 0.8142(5) 0.8723(3) 0.4028(3) 0.0505(12) Uani 1 1 d . . . . . C4 C 0.5512(4) 0.8453(3) 0.1562(2) 0.0411(10) Uani 1 1 d . . . . . C9 C 1.0423(5) 0.6793(4) 0.3218(3) 0.0557(13) Uani 1 1 d . . . . . C3 C 0.4793(4) 0.7707(3) 0.1726(2) 0.0427(10) Uani 1 1 d . . . . . C16 C 0.6558(5) 0.7715(3) 0.4192(2) 0.0461(11) Uani 1 1 d . . . . . C25 C 0.5759(7) 0.9093(5) 0.3426(3) 0.084(2) Uani 1 1 d . . . . . H25A H 0.613746 0.940010 0.311278 0.127 Uiso 1 1 calc R U . . . H25B H 0.543364 0.954773 0.367883 0.127 Uiso 1 1 calc R U . . . H25C H 0.504830 0.870433 0.321841 0.127 Uiso 1 1 calc R U . . . C15 C 0.9540(8) 0.6809(5) 0.1999(3) 0.086(2) Uani 1 1 d . . . . . H15A H 0.864906 0.679793 0.176177 0.129 Uiso 1 1 calc R U . . . H15B H 1.006655 0.640378 0.180223 0.129 Uiso 1 1 calc R U . . . H15C H 0.987733 0.742958 0.200573 0.129 Uiso 1 1 calc R U . . . C12 C 0.8863(8) 0.4771(5) 0.3839(4) 0.094(3) Uani 1 1 d . . . . . H12A H 0.903720 0.492454 0.428218 0.141 Uiso 1 1 calc R U . . . H12B H 0.934270 0.422192 0.377842 0.141 Uiso 1 1 calc R U . . . H12C H 0.793932 0.466109 0.369094 0.141 Uiso 1 1 calc R U . . . C11 C 0.8002(7) 0.5093(5) 0.2342(4) 0.090(2) Uani 1 1 d . . . . . H11A H 0.747011 0.471757 0.255536 0.135 Uiso 1 1 calc R U . . . H11B H 0.853779 0.469982 0.214203 0.135 Uiso 1 1 calc R U . . . H11C H 0.744502 0.546562 0.202581 0.135 Uiso 1 1 calc R U . . . C14 C 1.1424(7) 0.7559(5) 0.3249(5) 0.103(3) Uani 1 1 d . . . . . H14A H 1.100325 0.810166 0.304179 0.154 Uiso 1 1 calc R U . . . H14B H 1.210336 0.736073 0.304049 0.154 Uiso 1 1 calc R U . . . H14C H 1.180073 0.770006 0.368456 0.154 Uiso 1 1 calc R U . . . C17 C 0.7758(5) 0.7434(3) 0.4566(2) 0.0457(11) Uani 1 1 d . . . . . C18 C 0.8733(5) 0.8057(3) 0.4477(2) 0.0473(11) Uani 1 1 d . . . . . C22 C 0.7931(8) 0.6664(5) 0.5058(3) 0.081(2) Uani 1 1 d . . . . . H22A H 0.713721 0.630718 0.500188 0.121 Uiso 1 1 calc R U . . . H22B H 0.812341 0.692980 0.547525 0.121 Uiso 1 1 calc R U . . . H22C H 0.864273 0.626898 0.500658 0.121 Uiso 1 1 calc R U . . . C7 C 0.9284(5) 0.5560(3) 0.3473(3) 0.0505(12) Uani 1 1 d . . . . . C23 C 1.0097(6) 0.8135(6) 0.4897(4) 0.088(2) Uani 1 1 d . . . . . H23A H 1.045630 0.752609 0.499279 0.132 Uiso 1 1 calc R U . . . H23B H 1.004349 0.844716 0.528320 0.132 Uiso 1 1 calc R U . . . H23C H 1.065320 0.848147 0.467930 0.132 Uiso 1 1 calc R U . . . C13 C 1.1164(8) 0.6167(6) 0.4365(3) 0.105(3) Uani 1 1 d . . . . . H13A H 1.156310 0.676152 0.447379 0.158 Uiso 1 1 calc R U . . . H13B H 1.183455 0.571357 0.435761 0.158 Uiso 1 1 calc R U . . . H13C H 1.066828 0.599241 0.467363 0.158 Uiso 1 1 calc R U . . . C24 C 0.8815(9) 0.9596(5) 0.3853(4) 0.096(3) Uani 1 1 d . . . . . H24A H 0.964926 0.943395 0.376254 0.145 Uiso 1 1 calc R U . . . H24B H 0.894444 1.002494 0.420096 0.145 Uiso 1 1 calc R U . . . H24C H 0.827326 0.987792 0.348530 0.145 Uiso 1 1 calc R U . . . C26 C 0.6914(13) 0.5603(6) 0.0355(5) 0.139(4) Uani 1 1 d . . . . . H26C H 0.657833 0.575606 -0.008807 0.167 Uiso 0.5 1 calc R U P A 1 H26D H 0.782117 0.580723 0.045804 0.167 Uiso 0.5 1 calc R U P A 1 H26A H 0.644731 0.561346 -0.008543 0.167 Uiso 0.5 1 calc R U P A -1 H26B H 0.777096 0.587761 0.037412 0.167 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7119(12) 0.4526(7) 0.0582(5) 0.132(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 0.03324(11) 0.03477(11) 0.03527(12) -0.00021(8) 0.00178(8) 0.00437(7) I1 0.0536(2) 0.04554(18) 0.0563(2) 0.00306(14) 0.00907(16) -0.01455(13) I4 0.0541(2) 0.0573(2) 0.0703(3) 0.00941(17) 0.01170(18) -0.01600(15) I3 0.0715(2) 0.0632(2) 0.0477(2) 0.01534(16) 0.00871(17) 0.02200(17) I2 0.0442(2) 0.0752(3) 0.0994(4) -0.0024(2) -0.0196(2) -0.00760(16) Cl2 0.1328(19) 0.1136(17) 0.0862(15) 0.0095(12) 0.0248(13) 0.0421(14) Cl1A 0.100(5) 0.105(5) 0.284(15) -0.039(7) 0.061(7) -0.007(4) N1 0.036(2) 0.044(2) 0.038(2) 0.0029(16) 0.0022(16) -0.0034(15) C5 0.040(2) 0.039(2) 0.040(2) 0.0045(19) 0.0067(19) 0.0000(17) C2 0.039(2) 0.035(2) 0.049(3) 0.0010(19) 0.007(2) -0.0038(17) C10 0.053(3) 0.056(3) 0.044(3) 0.008(2) 0.015(2) 0.015(2) C6 0.042(3) 0.041(3) 0.063(3) -0.015(2) 0.004(2) 0.0070(19) C8 0.050(3) 0.057(3) 0.051(3) -0.005(2) 0.002(2) 0.022(2) C21 0.052(4) 0.099(5) 0.079(5) -0.030(4) 0.021(3) -0.009(3) C20 0.070(3) 0.045(3) 0.039(3) -0.003(2) 0.006(2) 0.020(2) C19 0.065(3) 0.039(2) 0.050(3) -0.011(2) 0.019(3) -0.006(2) C4 0.040(2) 0.041(2) 0.041(3) 0.001(2) 0.005(2) 0.0057(18) C9 0.037(3) 0.049(3) 0.082(4) -0.005(3) 0.015(3) 0.003(2) C3 0.037(2) 0.045(2) 0.043(3) -0.005(2) 0.0012(19) 0.0002(18) C16 0.043(3) 0.049(3) 0.046(3) -0.005(2) 0.010(2) 0.0046(19) C25 0.103(5) 0.086(4) 0.060(4) 0.004(3) 0.005(4) 0.056(4) C15 0.109(6) 0.094(5) 0.067(4) 0.017(4) 0.045(4) 0.033(4) C12 0.107(6) 0.062(4) 0.129(7) 0.036(4) 0.060(5) 0.022(4) C11 0.074(4) 0.087(5) 0.101(6) -0.047(4) 0.001(4) 0.006(3) C14 0.063(4) 0.076(4) 0.177(9) -0.024(5) 0.040(5) -0.019(3) C17 0.056(3) 0.043(2) 0.036(2) -0.002(2) 0.008(2) 0.010(2) C18 0.044(3) 0.052(3) 0.042(3) -0.011(2) 0.002(2) 0.001(2) C22 0.107(6) 0.074(4) 0.064(4) 0.025(3) 0.025(4) 0.021(4) C7 0.052(3) 0.037(2) 0.065(4) 0.011(2) 0.018(3) 0.017(2) C23 0.056(4) 0.114(6) 0.084(5) -0.047(5) -0.007(3) -0.002(3) C13 0.089(5) 0.144(7) 0.065(5) -0.022(5) -0.024(4) 0.065(5) C24 0.145(8) 0.059(4) 0.101(6) -0.016(4) 0.063(6) -0.035(4) C26 0.232(13) 0.101(7) 0.113(8) 0.030(6) 0.102(9) 0.017(7) Cl1B 0.201(9) 0.104(6) 0.090(4) 0.023(4) 0.027(4) 0.077(6) 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 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 61.71(9) . . ? N1 Dy1 C10 84.07(14) . . ? N1 Dy1 C6 92.60(15) . . ? N1 Dy1 C8 135.05(15) . . ? N1 Dy1 C20 81.30(14) . . ? N1 Dy1 C19 96.70(15) . . ? N1 Dy1 C9 107.85(17) . . ? N1 Dy1 C16 100.70(14) . . ? N1 Dy1 C17 130.11(14) . . ? N1 Dy1 C18 127.55(14) . . ? N1 Dy1 C7 122.82(16) . . ? C10 Dy1 I1 102.30(12) . . ? C10 Dy1 C8 51.02(16) . . ? C10 Dy1 C16 174.63(15) . . ? C6 Dy1 I1 80.34(11) . . ? C6 Dy1 C10 30.98(16) . . ? C6 Dy1 C8 50.89(16) . . ? C6 Dy1 C16 145.21(16) . . ? C6 Dy1 C17 131.98(16) . . ? C8 Dy1 I1 122.92(12) . . ? C8 Dy1 C16 124.25(16) . . ? C20 Dy1 I1 89.64(13) . . ? C20 Dy1 C10 153.87(17) . . ? C20 Dy1 C6 169.88(17) . . ? C20 Dy1 C8 138.23(17) . . ? C20 Dy1 C16 30.92(15) . . ? C20 Dy1 C17 50.97(15) . . ? C19 Dy1 I1 120.82(12) . . ? C19 Dy1 C10 131.40(17) . . ? C19 Dy1 C6 158.80(16) . . ? C19 Dy1 C8 111.01(18) . . ? C19 Dy1 C20 31.19(17) . . ? C19 Dy1 C9 108.24(17) . . ? C19 Dy1 C16 50.91(15) . . ? C19 Dy1 C17 50.95(15) . . ? C19 Dy1 C18 31.02(16) . . ? C19 Dy1 C7 138.34(18) . . ? C9 Dy1 I1 130.38(12) . . ? C9 Dy1 C10 30.56(17) . . ? C9 Dy1 C6 50.62(16) . . ? C9 Dy1 C8 30.79(17) . . ? C9 Dy1 C20 139.02(18) . . ? C9 Dy1 C16 146.90(18) . . ? C9 Dy1 C17 117.45(18) . . ? C9 Dy1 C18 97.73(17) . . ? C9 Dy1 C7 50.91(16) . . ? C16 Dy1 I1 78.09(11) . . ? C17 Dy1 I1 99.80(11) . . ? C17 Dy1 C10 145.43(15) . . ? C17 Dy1 C8 94.55(16) . . ? C17 Dy1 C16 30.31(15) . . ? C18 Dy1 I1 128.03(11) . . ? C18 Dy1 C10 128.11(16) . . ? C18 Dy1 C6 137.35(16) . . ? C18 Dy1 C8 86.97(16) . . ? C18 Dy1 C20 51.27(16) . . ? C18 Dy1 C16 50.50(15) . . ? C18 Dy1 C17 30.64(16) . . ? C7 Dy1 I1 91.85(12) . . ? C7 Dy1 C10 51.09(16) . . ? C7 Dy1 C6 30.63(17) . . ? C7 Dy1 C8 31.08(17) . . ? C7 Dy1 C20 152.90(16) . . ? C7 Dy1 C16 123.63(16) . . ? C7 Dy1 C17 102.22(16) . . ? C7 Dy1 C18 108.97(17) . . ? C2 I1 Dy1 68.14(13) . . ? C5 N1 Dy1 143.7(3) . . ? C2 N1 Dy1 111.2(3) . . ? C2 N1 C5 104.4(4) . . ? N1 C5 I4 121.7(3) . . ? N1 C5 C4 111.3(4) . . ? C4 C5 I4 127.0(3) . . ? N1 C2 I1 118.8(3) . . ? N1 C2 C3 112.3(4) . . ? C3 C2 I1 128.8(3) . . ? C6 C10 Dy1 74.5(3) . . ? C6 C10 C15 124.2(6) . . ? C9 C10 Dy1 74.1(3) . . ? C9 C10 C6 107.1(5) . . ? C9 C10 C15 128.1(6) . . ? C15 C10 Dy1 123.6(4) . . ? C10 C6 Dy1 74.5(3) . . ? C10 C6 C11 124.6(6) . . ? C11 C6 Dy1 124.7(4) . . ? C7 C6 Dy1 74.2(3) . . ? C7 C6 C10 108.4(5) . . ? C7 C6 C11 126.3(6) . . ? C9 C8 Dy1 73.9(3) . . ? C9 C8 C7 106.8(5) . . ? C9 C8 C13 126.6(6) . . ? C7 C8 Dy1 73.8(3) . . ? C7 C8 C13 125.2(6) . . ? C13 C8 Dy1 128.1(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 73.7(3) . . ? C19 C20 C16 107.0(4) . . ? C19 C20 C25 126.1(6) . . ? C16 C20 Dy1 75.9(3) . . ? C16 C20 C25 126.4(6) . . ? C25 C20 Dy1 122.1(4) . . ? C20 C19 Dy1 75.1(3) . . ? C20 C19 C24 126.2(6) . . ? C18 C19 Dy1 75.1(3) . . ? C18 C19 C20 108.1(4) . . ? C18 C19 C24 125.1(6) . . ? C24 C19 Dy1 122.9(4) . . ? C5 C4 I3 126.5(3) . . ? C5 C4 C3 107.1(4) . . ? C3 C4 I3 126.4(3) . . ? C10 C9 Dy1 75.3(3) . . ? C10 C9 C8 109.5(5) . . ? C10 C9 C14 124.3(6) . . ? C8 C9 Dy1 75.3(3) . . ? C8 C9 C14 125.9(6) . . ? C14 C9 Dy1 120.4(4) . . ? C2 C3 I2 126.3(3) . . ? C2 C3 C4 105.0(4) . . ? C4 C3 I2 128.6(4) . . ? C21 C16 Dy1 127.2(4) . . ? C20 C16 Dy1 73.2(3) . . ? C20 C16 C21 125.4(5) . . ? C17 C16 Dy1 73.8(3) . . ? C17 C16 C21 125.6(5) . . ? C17 C16 C20 108.2(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 75.9(3) . . ? C16 C17 C18 108.7(4) . . ? C16 C17 C22 125.1(5) . . ? C18 C17 Dy1 74.2(3) . . ? C18 C17 C22 125.7(5) . . ? C22 C17 Dy1 122.9(4) . . ? C19 C18 Dy1 73.9(3) . . ? C19 C18 C23 125.1(5) . . ? C17 C18 Dy1 75.1(3) . . ? C17 C18 C19 108.0(4) . . ? C17 C18 C23 125.5(6) . . ? C23 C18 Dy1 127.7(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 75.2(3) . . ? C6 C7 C8 108.2(5) . . ? C6 C7 C12 126.5(6) . . ? C8 C7 Dy1 75.1(3) . . ? C8 C7 C12 125.1(6) . . ? C12 C7 Dy1 120.5(4) . . ? 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 108.4 . . ? Cl2 C26 H26B 108.4 . . ? Cl1A C26 Cl2 122.5(7) . . ? Cl1A C26 H26C 106.7 . . ? Cl1A C26 H26D 106.7 . . ? Cl1A C26 H26A 94.4 . . ? Cl1A C26 H26B 113.8 . . ? H26C C26 H26D 106.6 . . ? H26C C26 H26A 14.7 . . ? H26C C26 H26B 94.8 . . ? H26D C26 H26A 118.7 . . ? H26D C26 H26B 12.1 . . ? H26A C26 H26B 107.5 . . ? Cl1B C26 Cl2 115.4(6) . . ? Cl1B C26 Cl1A 14.1(8) . . ? Cl1B C26 H26C 120.7 . . ? Cl1B C26 H26D 99.3 . . ? Cl1B C26 H26A 108.4 . . ? Cl1B C26 H26B 108.4 . . ? 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 3.2572(4) . ? Dy1 N1 2.385(4) . ? Dy1 C10 2.655(5) . ? Dy1 C6 2.655(4) . ? Dy1 C8 2.658(5) . ? Dy1 C20 2.647(5) . ? Dy1 C19 2.630(5) . ? Dy1 C9 2.640(5) . ? Dy1 C16 2.682(5) . ? Dy1 C17 2.655(5) . ? Dy1 C18 2.644(5) . ? Dy1 C7 2.642(4) . ? I1 C2 2.083(4) . ? I4 C5 2.080(4) . ? I3 C4 2.078(5) . ? I2 C3 2.059(5) . ? Cl2 C26 1.689(9) . ? Cl1A C26 1.655(14) . ? N1 C5 1.365(5) . ? N1 C2 1.363(6) . ? C5 C4 1.365(6) . ? C2 C3 1.374(7) . ? C10 C6 1.418(7) . ? C10 C9 1.395(8) . ? C10 C15 1.490(8) . ? C6 C11 1.524(8) . ? C6 C7 1.399(8) . ? C8 C9 1.407(8) . ? C8 C7 1.420(8) . ? C8 C13 1.494(8) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C21 C16 1.513(8) . ? C20 C19 1.419(8) . ? C20 C16 1.421(7) . ? C20 C25 1.498(7) . ? C19 C18 1.410(7) . ? C19 C24 1.527(8) . ? C4 C3 1.400(6) . ? C9 C14 1.511(8) . ? C16 C17 1.396(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 1.504(8) . ? 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 1.400(7) . ? C17 C22 1.519(7) . ? C18 C23 1.517(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 1.629(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 12.4(7) . . . . ? Dy1 N1 C5 C4 -167.5(4) . . . . ? Dy1 N1 C2 I1 -4.8(4) . . . . ? Dy1 N1 C2 C3 171.5(3) . . . . ? Dy1 C10 C6 C11 121.8(5) . . . . ? Dy1 C10 C6 C7 -67.0(3) . . . . ? Dy1 C10 C9 C8 68.3(3) . . . . ? Dy1 C10 C9 C14 -117.0(5) . . . . ? Dy1 C6 C7 C8 -68.5(3) . . . . ? Dy1 C6 C7 C12 117.3(5) . . . . ? Dy1 C8 C9 C10 -68.3(4) . . . . ? Dy1 C8 C9 C14 117.1(6) . . . . ? Dy1 C8 C7 C6 68.6(3) . . . . ? Dy1 C8 C7 C12 -117.1(5) . . . . ? Dy1 C20 C19 C18 -68.5(3) . . . . ? Dy1 C20 C19 C24 120.1(5) . . . . ? Dy1 C20 C16 C21 -124.1(5) . . . . ? Dy1 C20 C16 C17 66.0(3) . . . . ? Dy1 C19 C18 C17 -68.0(3) . . . . ? Dy1 C19 C18 C23 125.1(5) . . . . ? Dy1 C16 C17 C18 67.6(3) . . . . ? Dy1 C16 C17 C22 -120.5(5) . . . . ? Dy1 C17 C18 C19 67.2(3) . . . . ? Dy1 C17 C18 C23 -125.9(5) . . . . ? I1 C2 C3 I2 -5.8(7) . . . . ? I1 C2 C3 C4 176.8(3) . . . . ? I4 C5 C4 I3 -0.5(6) . . . . ? I4 C5 C4 C3 -179.6(3) . . . . ? I3 C4 C3 I2 2.9(6) . . . . ? I3 C4 C3 C2 -179.8(3) . . . . ? N1 C5 C4 I3 179.3(3) . . . . ? N1 C5 C4 C3 0.3(5) . . . . ? N1 C2 C3 I2 178.4(3) . . . . ? N1 C2 C3 C4 1.0(6) . . . . ? C5 N1 C2 I1 -177.1(3) . . . . ? C5 N1 C2 C3 -0.8(5) . . . . ? C5 C4 C3 I2 -178.0(3) . . . . ? C5 C4 C3 C2 -0.7(5) . . . . ? C2 N1 C5 I4 -179.8(3) . . . . ? C2 N1 C5 C4 0.3(5) . . . . ? C10 C6 C7 Dy1 67.3(3) . . . . ? C10 C6 C7 C8 -1.3(5) . . . . ? C10 C6 C7 C12 -175.4(5) . . . . ? C6 C10 C9 Dy1 -67.8(3) . . . . ? C6 C10 C9 C8 0.5(6) . . . . ? C6 C10 C9 C14 175.2(5) . . . . ? C21 C16 C17 Dy1 124.5(5) . . . . ? C21 C16 C17 C18 -167.9(5) . . . . ? C21 C16 C17 C22 4.0(8) . . . . ? C20 C19 C18 Dy1 68.5(3) . . . . ? C20 C19 C18 C17 0.5(5) . . . . ? C20 C19 C18 C23 -166.4(5) . . . . ? C20 C16 C17 Dy1 -65.6(3) . . . . ? C20 C16 C17 C18 2.0(5) . . . . ? C20 C16 C17 C22 173.9(5) . . . . ? C19 C20 C16 Dy1 -67.7(3) . . . . ? C19 C20 C16 C21 168.2(5) . . . . ? C19 C20 C16 C17 -1.7(5) . . . . ? C9 C10 C6 Dy1 67.5(3) . . . . ? C9 C10 C6 C11 -170.7(5) . . . . ? C9 C10 C6 C7 0.5(5) . . . . ? C9 C8 C7 Dy1 -67.0(3) . . . . ? C9 C8 C7 C6 1.6(5) . . . . ? C9 C8 C7 C12 175.8(5) . . . . ? C16 C20 C19 Dy1 69.2(3) . . . . ? C16 C20 C19 C18 0.7(5) . . . . ? C16 C20 C19 C24 -170.7(5) . . . . ? C16 C17 C18 Dy1 -68.7(3) . . . . ? C16 C17 C18 C19 -1.5(5) . . . . ? C16 C17 C18 C23 165.3(5) . . . . ? C25 C20 C19 Dy1 -118.2(5) . . . . ? C25 C20 C19 C18 173.3(5) . . . . ? C25 C20 C19 C24 1.9(9) . . . . ? C25 C20 C16 Dy1 119.7(5) . . . . ? C25 C20 C16 C21 -4.4(8) . . . . ? C25 C20 C16 C17 -174.2(5) . . . . ? C15 C10 C6 Dy1 -120.4(5) . . . . ? C15 C10 C6 C11 1.3(8) . . . . ? C15 C10 C6 C7 172.5(5) . . . . ? C15 C10 C9 Dy1 120.6(6) . . . . ? C15 C10 C9 C8 -171.2(5) . . . . ? C15 C10 C9 C14 3.6(9) . . . . ? C11 C6 C7 Dy1 -121.7(5) . . . . ? C11 C6 C7 C8 169.8(5) . . . . ? C11 C6 C7 C12 -4.4(8) . . . . ? C22 C17 C18 Dy1 119.4(5) . . . . ? C22 C17 C18 C19 -173.3(5) . . . . ? C22 C17 C18 C23 -6.5(8) . . . . ? C7 C8 C9 Dy1 67.0(3) . . . . ? C7 C8 C9 C10 -1.3(5) . . . . ? C7 C8 C9 C14 -175.9(5) . . . . ? C13 C8 C9 Dy1 -125.8(5) . . . . ? C13 C8 C9 C10 165.9(5) . . . . ? C13 C8 C9 C14 -8.7(9) . . . . ? C13 C8 C7 Dy1 125.6(5) . . . . ? C13 C8 C7 C6 -165.8(5) . . . . ? C13 C8 C7 C12 8.5(8) . . . . ? C24 C19 C18 Dy1 -119.9(5) . . . . ? C24 C19 C18 C17 172.1(5) . . . . ? C24 C19 C18 C23 5.2(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 0.9803 -1.0971 -0.2671 -0.0783 -0.0142 0.0325 1.0662 0.9241 -0.2286 0.0038 0.0040 0.0859 -0.9803 1.0971 0.2671 0.0783 0.0142 -0.0325 -1.0662 -0.9241 0.2286 -0.0038 -0.0040 -0.0859 0.0501 -0.0224 0.9849 -0.0100 0.0322 0.0044 -0.0501 0.0224 -0.9849 0.0100 -0.0322 -0.0044 0.9661 0.9690 -2.1984 0.0239 -0.0605 0.0770 -0.9661 -0.9690 2.1984 -0.0239 0.0605 -0.0770 -1.1163 -0.9016 -0.7564 0.0063 -0.0363 -0.0903 -0.0572 1.0555 -1.9506 0.0612 -0.0554 0.0178 -2.1396 -0.8151 -0.5085 0.0435 -0.0312 -0.1495 0.1432 0.9657 1.9891 0.0210 0.0736 0.0356 1.1234 -0.1314 1.7220 -0.0574 0.0594 0.0681 0.9231 -0.0416 -2.2177 -0.0172 -0.0696 0.0503 7.3238 6.3418 20.8054 -0.1415 0.7602 0.6341