#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:50:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294477 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572182.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_1572182 loop_ _publ_author_name 'Delano, 4th, Francis' 'Benner, Florian' 'Jang, Seoyun' 'Greer, Samuel M.' 'Demir, Selvan' _publ_section_title ; Construction of intermolecular σ-hole interactions in rare earth metallocene complexes using a 2,3,4,5-tetraiodopyrrolyl anion. ; _journal_issue 33 _journal_name_full 'Chemical science' _journal_page_first 13389 _journal_page_last 13404 _journal_paper_doi 10.1039/d4sc03786c _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C24 H30 Dy I4 N, C H2 Cl2' _chemical_formula_sum 'C25 H32 Cl2 Dy I4 N' _chemical_formula_weight 1087.51 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-07-10 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-04-22 deposited with the CCDC. 2024-07-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.800(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3596(2) _cell_length_b 14.3374(3) _cell_length_c 21.3250(5) _cell_measurement_reflns_used 19505 _cell_measurement_temperature 190.0(1) _cell_measurement_theta_max 31.9260 _cell_measurement_theta_min 2.8400 _cell_volume 3100.46(12) _computing_cell_refinement 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 190.0(1) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.837 _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 -0.0369856000 _diffrn_orient_matrix_UB_12 0.0412803000 _diffrn_orient_matrix_UB_13 -0.0088556000 _diffrn_orient_matrix_UB_21 -0.0033507000 _diffrn_orient_matrix_UB_22 0.0076232000 _diffrn_orient_matrix_UB_23 0.0324998000 _diffrn_orient_matrix_UB_31 0.0592433000 _diffrn_orient_matrix_UB_32 0.0261931000 _diffrn_orient_matrix_UB_33 0.0044942000 _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 0.0547 _diffrn_reflns_av_unetI/netI 0.0455 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.837 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 38506 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.837 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.757 _diffrn_reflns_theta_min 2.460 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.580 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.228 _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 2.330 _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 1.095 _refine_diff_density_min -1.509 _refine_diff_density_rms 0.166 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8841 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0321 _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^)+(0.0344P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.0767 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7076 _reflns_number_total 8841 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP190K _cod_depositor_comments 'Adding full bibliography for 1572175--1572199.cif.' _cod_original_cell_volume 3100.47(13) _cod_database_code 1572182 _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 0.529 _shelx_estimated_absorpt_t_min 0.205 _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_190_final.res created by SHELXL-2018/3 at 16:22:26 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 10.359613 14.337395 21.325047 90 101.8003 90 ZERR 4 0.000247 0.00033 0.000532 0 0.0024 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. 25 0 0 PLAN 16 SIZE 0.111 0.275 0.353 TEMP -83.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.034400 FVAR 0.60850 DY1 4 0.804453 0.714822 0.339278 11.00000 0.01989 0.02033 = 0.02018 -0.00039 0.00081 0.00282 I1 5 0.524824 0.615293 0.281327 11.00000 0.03047 0.02637 = 0.03132 0.00157 0.00498 -0.00813 I4 5 0.821035 0.939662 0.200582 11.00000 0.03027 0.03181 = 0.04022 0.00524 0.00595 -0.00861 I3 5 0.484001 0.936822 0.081660 11.00000 0.03944 0.03652 = 0.02723 0.00827 0.00404 0.01218 I2 5 0.292427 0.721220 0.130338 11.00000 0.02523 0.04448 = 0.06007 0.00027 -0.01215 -0.00516 CL2 3 0.609119 0.627843 0.079357 11.00000 0.06770 0.06209 = 0.04646 0.00574 0.01244 0.02184 PART 1 CL1A 3 0.692046 0.444342 0.038451 10.50000 0.07316 0.06164 = 0.20788 -0.03476 0.01753 0.00001 PART 0 N1 6 0.678489 0.773834 0.241926 11.00000 0.02039 0.02717 = 0.02270 0.00113 0.00094 -0.00185 C5 1 0.668622 0.845394 0.198528 11.00000 0.02161 0.02363 = 0.02219 -0.00010 0.00207 -0.00018 C2 1 0.559723 0.728055 0.225171 11.00000 0.02238 0.02261 = 0.02685 -0.00151 0.00435 -0.00289 C10 1 0.957505 0.648080 0.264043 11.00000 0.02791 0.02571 = 0.02931 0.00180 0.00873 0.00806 C6 1 0.887374 0.570129 0.280217 11.00000 0.02648 0.01899 = 0.03878 -0.00474 0.00250 0.00469 C8 1 1.028399 0.620156 0.371375 11.00000 0.02750 0.03651 = 0.03217 -0.00769 -0.00088 0.01671 C21 1 0.519492 0.738597 0.424230 11.00000 0.02774 0.05217 = 0.04754 -0.01197 0.01011 -0.00022 AFIX 137 H21A 2 0.455371 0.758014 0.386052 11.00000 -1.50000 H21B 2 0.494305 0.764582 0.462510 11.00000 -1.50000 H21C 2 0.521026 0.670363 0.426987 11.00000 -1.50000 AFIX 0 C20 1 0.682972 0.853606 0.386064 11.00000 0.03904 0.02668 = 0.02487 -0.00180 0.00562 0.01142 C19 1 0.819506 0.871651 0.403991 11.00000 0.04373 0.02352 = 0.03057 -0.00355 0.01082 -0.00027 C4 1 0.548670 0.843881 0.155819 11.00000 0.02495 0.02456 = 0.02506 0.00270 0.00329 0.00400 C9 1 1.043465 0.679717 0.320271 11.00000 0.02052 0.02877 = 0.04695 -0.00655 0.00843 -0.00042 C3 1 0.476301 0.768077 0.173706 11.00000 0.02124 0.02843 = 0.02521 -0.00333 0.00019 0.00064 C16 1 0.654561 0.773733 0.419830 11.00000 0.02810 0.02578 = 0.02553 -0.00305 0.00726 0.00377 C25 1 0.583198 0.913898 0.343248 11.00000 0.05606 0.04675 = 0.03704 0.00170 0.00381 0.03118 AFIX 137 H25A 2 0.627317 0.950898 0.315182 11.00000 -1.50000 H25B 2 0.541467 0.955751 0.369538 11.00000 -1.50000 H25C 2 0.515816 0.874321 0.317133 11.00000 -1.50000 AFIX 0 C15 1 0.952210 0.682646 0.197178 11.00000 0.05449 0.05439 = 0.04048 0.00818 0.02310 0.01765 AFIX 137 H15A 2 0.860079 0.686918 0.174453 11.00000 -1.50000 H15B 2 0.999781 0.639203 0.174572 11.00000 -1.50000 H15C 2 0.993312 0.744403 0.198824 11.00000 -1.50000 AFIX 0 C12 1 0.887933 0.473372 0.383510 11.00000 0.06663 0.03663 = 0.07202 0.02265 0.03324 0.01439 AFIX 137 H12A 2 0.888102 0.492945 0.427557 11.00000 -1.50000 H12B 2 0.949860 0.421570 0.384029 11.00000 -1.50000 H12C 2 0.799051 0.453130 0.362836 11.00000 -1.50000 AFIX 0 C11 1 0.800193 0.508173 0.232497 11.00000 0.03822 0.05043 = 0.06143 -0.02711 0.00722 0.00021 AFIX 137 H11A 2 0.757511 0.461894 0.255309 11.00000 -1.50000 H11B 2 0.853593 0.476195 0.206103 11.00000 -1.50000 H11C 2 0.732699 0.546081 0.205003 11.00000 -1.50000 AFIX 0 C14 1 1.145213 0.755868 0.323167 11.00000 0.03275 0.05198 = 0.08703 -0.01638 0.01910 -0.00979 AFIX 137 H14A 2 1.107862 0.807187 0.294840 11.00000 -1.50000 H14B 2 1.222916 0.730923 0.309316 11.00000 -1.50000 H14C 2 1.170891 0.778915 0.367223 11.00000 -1.50000 AFIX 0 C17 1 0.774678 0.741586 0.458846 11.00000 0.03035 0.02899 = 0.02555 -0.00058 0.00835 0.00178 C18 1 0.875722 0.803085 0.449585 11.00000 0.02713 0.03299 = 0.02176 -0.00797 0.00400 -0.00021 C22 1 0.786879 0.663753 0.506819 11.00000 0.05457 0.04201 = 0.03372 0.01320 0.00944 0.01013 AFIX 137 H22A 2 0.737511 0.609358 0.486970 11.00000 -1.50000 H22B 2 0.751091 0.684047 0.543712 11.00000 -1.50000 H22C 2 0.879998 0.647058 0.521083 11.00000 -1.50000 AFIX 0 C7 1 0.929108 0.554025 0.346783 11.00000 0.02980 0.02303 = 0.04156 0.00452 0.01118 0.00859 C23 1 1.010667 0.809321 0.491431 11.00000 0.03405 0.05674 = 0.04446 -0.02065 -0.00161 -0.00291 AFIX 137 H23A 2 1.032779 0.749834 0.513672 11.00000 -1.50000 H23B 2 1.012072 0.859187 0.522994 11.00000 -1.50000 H23C 2 1.075345 0.823017 0.464975 11.00000 -1.50000 AFIX 0 C13 1 1.118953 0.613973 0.435228 11.00000 0.05584 0.07435 = 0.04633 -0.01408 -0.01261 0.03804 AFIX 137 H13A 2 1.167582 0.672686 0.444407 11.00000 -1.50000 H13B 2 1.181341 0.562646 0.435032 11.00000 -1.50000 H13C 2 1.067501 0.602520 0.468248 11.00000 -1.50000 AFIX 0 C24 1 0.893025 0.955723 0.386774 11.00000 0.06863 0.03437 = 0.04930 -0.00925 0.02122 -0.01560 AFIX 137 H24A 2 0.973935 0.935301 0.373763 11.00000 -1.50000 H24B 2 0.915659 0.996977 0.424047 11.00000 -1.50000 H24C 2 0.837175 0.989429 0.351342 11.00000 -1.50000 AFIX 0 C26 1 0.699617 0.558986 0.038060 11.00000 0.17886 0.05275 = 0.09772 0.01605 0.10191 0.01721 PART 1 AFIX 23 H26C 2 0.676257 0.578657 -0.007353 10.50000 -1.20000 H26D 2 0.793352 0.575877 0.053652 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.663118 0.565677 -0.008388 10.50000 -1.20000 H26B 2 0.791499 0.582287 0.046329 10.50000 -1.20000 AFIX 0 CL1B 3 0.701823 0.445080 0.057134 10.50000 0.09385 0.04534 = 0.05634 0.01344 0.02940 0.02402 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0767, GooF = S = 1.039, Restrained GooF = 1.039 for all data REM R1 = 0.0321 for 7076 Fo > 4sig(Fo) and 0.0442 for all 8841 data REM 317 parameters refined using 6 restraints END WGHT 0.0344 0.0000 REM Highest difference peak 1.095, deepest hole -1.509, 1-sigma level 0.166 Q1 1 0.2880 0.7429 0.1595 11.00000 0.05 1.10 Q2 1 0.7791 0.4852 0.0549 11.00000 0.05 0.91 Q3 1 0.3943 0.8967 0.0810 11.00000 0.05 0.90 Q4 1 0.7182 0.6777 0.3402 11.00000 0.05 0.90 Q5 1 0.7189 0.7417 0.3397 11.00000 0.05 0.74 Q6 1 0.4738 0.9017 0.0651 11.00000 0.05 0.71 Q7 1 0.8780 0.7535 0.3401 11.00000 0.05 0.67 Q8 1 0.4957 0.7990 0.4367 11.00000 0.05 0.66 Q9 1 0.7057 0.5608 0.0003 11.00000 0.05 0.64 Q10 1 0.9378 0.7143 0.2845 11.00000 0.05 0.64 Q11 1 0.5539 0.9300 0.0428 11.00000 0.05 0.64 Q12 1 1.1247 0.8024 0.4794 11.00000 0.05 0.62 Q13 1 0.5520 0.9607 0.0836 11.00000 0.05 0.61 Q14 1 0.8913 0.9054 0.2008 11.00000 0.05 0.61 Q15 1 1.0678 0.6231 0.3430 11.00000 0.05 0.61 Q16 1 0.6660 0.6275 0.5018 11.00000 0.05 0.60 ; _shelx_res_checksum 70839 _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 2.927 _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 0.80445(2) 0.71482(2) 0.33928(2) 0.02060(5) Uani 1 1 d . . . . . I1 I 0.52482(2) 0.61529(2) 0.28133(2) 0.02958(7) Uani 1 1 d . . . . . I4 I 0.82103(3) 0.93966(2) 0.20058(2) 0.03428(7) Uani 1 1 d . . . . . I3 I 0.48400(3) 0.93682(2) 0.08166(2) 0.03479(7) Uani 1 1 d . . . . . I2 I 0.29243(3) 0.72122(2) 0.13034(2) 0.04623(9) Uani 1 1 d . . . . . Cl2 Cl 0.60912(15) 0.62784(10) 0.07936(7) 0.0586(3) Uani 1 1 d . . . . . Cl1A Cl 0.6920(11) 0.4443(7) 0.0385(5) 0.116(3) Uani 0.5 1 d . U P A 1 N1 N 0.6785(3) 0.7738(2) 0.24193(15) 0.0239(6) Uani 1 1 d . . . . . C5 C 0.6686(3) 0.8454(2) 0.19853(18) 0.0228(7) Uani 1 1 d . . . . . C2 C 0.5597(3) 0.7281(2) 0.22517(18) 0.0240(7) Uani 1 1 d . . . . . C10 C 0.9575(4) 0.6481(3) 0.26404(19) 0.0272(8) Uani 1 1 d . . . . . C6 C 0.8874(4) 0.5701(2) 0.2802(2) 0.0287(8) Uani 1 1 d . . . . . C8 C 1.0284(4) 0.6202(3) 0.3714(2) 0.0331(9) Uani 1 1 d . . . . . C21 C 0.5195(4) 0.7386(3) 0.4242(2) 0.0421(11) Uani 1 1 d . . . . . H21A H 0.455371 0.758014 0.386052 0.063 Uiso 1 1 calc R U . . . H21B H 0.494305 0.764582 0.462510 0.063 Uiso 1 1 calc R U . . . H21C H 0.521026 0.670363 0.426987 0.063 Uiso 1 1 calc R U . . . C20 C 0.6830(4) 0.8536(3) 0.38606(19) 0.0303(8) Uani 1 1 d . . . . . C19 C 0.8195(4) 0.8717(3) 0.4040(2) 0.0321(9) Uani 1 1 d . . . . . C4 C 0.5487(4) 0.8439(2) 0.15582(18) 0.0251(7) Uani 1 1 d . . . . . C9 C 1.0435(4) 0.6797(3) 0.3203(2) 0.0319(9) Uani 1 1 d . . . . . C3 C 0.4763(4) 0.7681(2) 0.17371(19) 0.0256(7) Uani 1 1 d . . . . . C16 C 0.6546(4) 0.7737(2) 0.41983(19) 0.0262(8) Uani 1 1 d . . . . . C25 C 0.5832(5) 0.9139(3) 0.3432(2) 0.0474(12) Uani 1 1 d . . . . . H25A H 0.627317 0.950898 0.315182 0.071 Uiso 1 1 calc R U . . . H25B H 0.541467 0.955751 0.369538 0.071 Uiso 1 1 calc R U . . . H25C H 0.515816 0.874321 0.317133 0.071 Uiso 1 1 calc R U . . . C15 C 0.9522(5) 0.6826(4) 0.1972(2) 0.0479(12) Uani 1 1 d . . . . . H15A H 0.860079 0.686918 0.174453 0.072 Uiso 1 1 calc R U . . . H15B H 0.999781 0.639203 0.174572 0.072 Uiso 1 1 calc R U . . . H15C H 0.993312 0.744403 0.198824 0.072 Uiso 1 1 calc R U . . . C12 C 0.8879(6) 0.4734(3) 0.3835(3) 0.0557(14) Uani 1 1 d . . . . . H12A H 0.888102 0.492945 0.427557 0.084 Uiso 1 1 calc R U . . . H12B H 0.949860 0.421570 0.384029 0.084 Uiso 1 1 calc R U . . . H12C H 0.799051 0.453130 0.362836 0.084 Uiso 1 1 calc R U . . . C11 C 0.8002(5) 0.5082(3) 0.2325(3) 0.0504(13) Uani 1 1 d . . . . . H11A H 0.757511 0.461894 0.255309 0.076 Uiso 1 1 calc R U . . . H11B H 0.853593 0.476195 0.206103 0.076 Uiso 1 1 calc R U . . . H11C H 0.732699 0.546081 0.205003 0.076 Uiso 1 1 calc R U . . . C14 C 1.1452(5) 0.7559(4) 0.3232(3) 0.0563(14) Uani 1 1 d . . . . . H14A H 1.107862 0.807187 0.294840 0.084 Uiso 1 1 calc R U . . . H14B H 1.222916 0.730923 0.309316 0.084 Uiso 1 1 calc R U . . . H14C H 1.170891 0.778915 0.367223 0.084 Uiso 1 1 calc R U . . . C17 C 0.7747(4) 0.7416(3) 0.45885(19) 0.0279(8) Uani 1 1 d . . . . . C18 C 0.8757(4) 0.8031(3) 0.44958(18) 0.0274(8) Uani 1 1 d . . . . . C22 C 0.7869(5) 0.6638(3) 0.5068(2) 0.0434(11) Uani 1 1 d . . . . . H22A H 0.737511 0.609358 0.486970 0.065 Uiso 1 1 calc R U . . . H22B H 0.751091 0.684047 0.543712 0.065 Uiso 1 1 calc R U . . . H22C H 0.879998 0.647058 0.521083 0.065 Uiso 1 1 calc R U . . . C7 C 0.9291(4) 0.5540(2) 0.3468(2) 0.0309(9) Uani 1 1 d . . . . . C23 C 1.0107(4) 0.8093(4) 0.4914(2) 0.0465(11) Uani 1 1 d . . . . . H23A H 1.032779 0.749834 0.513672 0.070 Uiso 1 1 calc R U . . . H23B H 1.012072 0.859187 0.522994 0.070 Uiso 1 1 calc R U . . . H23C H 1.075345 0.823017 0.464975 0.070 Uiso 1 1 calc R U . . . C13 C 1.1190(5) 0.6140(4) 0.4352(3) 0.0621(16) Uani 1 1 d . . . . . H13A H 1.167582 0.672686 0.444407 0.093 Uiso 1 1 calc R U . . . H13B H 1.181341 0.562646 0.435032 0.093 Uiso 1 1 calc R U . . . H13C H 1.067501 0.602520 0.468248 0.093 Uiso 1 1 calc R U . . . C24 C 0.8930(6) 0.9557(3) 0.3868(3) 0.0495(12) Uani 1 1 d . . . . . H24A H 0.973935 0.935301 0.373763 0.074 Uiso 1 1 calc R U . . . H24B H 0.915659 0.996977 0.424047 0.074 Uiso 1 1 calc R U . . . H24C H 0.837175 0.989429 0.351342 0.074 Uiso 1 1 calc R U . . . C26 C 0.6996(10) 0.5590(4) 0.0381(4) 0.099(3) Uani 1 1 d . . . . . H26C H 0.676257 0.578657 -0.007353 0.119 Uiso 0.5 1 calc R U P A 1 H26D H 0.793352 0.575877 0.053652 0.119 Uiso 0.5 1 calc R U P A 1 H26A H 0.663118 0.565677 -0.008388 0.119 Uiso 0.5 1 calc R U P A -1 H26B H 0.791499 0.582287 0.046329 0.119 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7018(10) 0.4451(6) 0.0571(3) 0.0632(17) 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 0.01989(9) 0.02033(9) 0.02018(9) -0.00039(6) 0.00081(6) 0.00282(5) I1 0.03047(14) 0.02637(12) 0.03132(14) 0.00157(10) 0.00498(10) -0.00813(9) I4 0.03027(14) 0.03181(14) 0.04022(16) 0.00524(11) 0.00595(11) -0.00861(9) I3 0.03944(16) 0.03652(15) 0.02723(14) 0.00827(10) 0.00404(11) 0.01218(10) I2 0.02523(14) 0.04448(17) 0.0601(2) 0.00027(14) -0.01215(13) -0.00516(10) Cl2 0.0677(9) 0.0621(8) 0.0465(7) 0.0057(6) 0.0124(6) 0.0218(6) Cl1A 0.073(4) 0.062(4) 0.208(10) -0.035(5) 0.018(6) 0.000(3) N1 0.0204(15) 0.0272(15) 0.0227(16) 0.0011(12) 0.0009(12) -0.0018(11) C5 0.0216(17) 0.0236(16) 0.0222(18) -0.0001(14) 0.0021(13) -0.0002(13) C2 0.0224(18) 0.0226(17) 0.0269(19) -0.0015(14) 0.0044(15) -0.0029(13) C10 0.028(2) 0.0257(18) 0.029(2) 0.0018(15) 0.0087(16) 0.0081(14) C6 0.0265(19) 0.0190(17) 0.039(2) -0.0047(15) 0.0025(16) 0.0047(13) C8 0.028(2) 0.037(2) 0.032(2) -0.0077(17) -0.0009(16) 0.0167(15) C21 0.028(2) 0.052(3) 0.048(3) -0.012(2) 0.010(2) -0.0002(18) C20 0.039(2) 0.0267(18) 0.0249(19) -0.0018(15) 0.0056(16) 0.0114(15) C19 0.044(2) 0.0235(18) 0.031(2) -0.0035(16) 0.0108(18) -0.0003(16) C4 0.0249(18) 0.0246(17) 0.0251(19) 0.0027(14) 0.0033(14) 0.0040(13) C9 0.0205(18) 0.0288(19) 0.047(3) -0.0066(17) 0.0084(17) -0.0004(14) C3 0.0212(18) 0.0284(18) 0.0252(19) -0.0033(15) 0.0002(14) 0.0006(13) C16 0.0281(19) 0.0258(18) 0.0255(19) -0.0030(14) 0.0073(15) 0.0038(14) C25 0.056(3) 0.047(3) 0.037(3) 0.002(2) 0.004(2) 0.031(2) C15 0.054(3) 0.054(3) 0.040(3) 0.008(2) 0.023(2) 0.018(2) C12 0.067(4) 0.037(2) 0.072(4) 0.023(2) 0.033(3) 0.014(2) C11 0.038(3) 0.050(3) 0.061(3) -0.027(2) 0.007(2) 0.000(2) C14 0.033(3) 0.052(3) 0.087(4) -0.016(3) 0.019(3) -0.010(2) C17 0.030(2) 0.0290(19) 0.026(2) -0.0006(15) 0.0083(16) 0.0018(15) C18 0.0271(19) 0.0330(19) 0.0218(18) -0.0080(15) 0.0040(15) -0.0002(14) C22 0.055(3) 0.042(2) 0.034(2) 0.013(2) 0.009(2) 0.010(2) C7 0.030(2) 0.0230(18) 0.042(2) 0.0045(16) 0.0112(17) 0.0086(14) C23 0.034(2) 0.057(3) 0.044(3) -0.021(2) -0.002(2) -0.0029(19) C13 0.056(3) 0.074(4) 0.046(3) -0.014(3) -0.013(2) 0.038(3) C24 0.069(3) 0.034(2) 0.049(3) -0.009(2) 0.021(3) -0.016(2) C26 0.179(9) 0.053(4) 0.098(6) 0.016(3) 0.102(6) 0.017(4) Cl1B 0.094(4) 0.045(3) 0.056(2) 0.0134(18) 0.029(2) 0.024(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -1 0 0.1241 1 1 0 0.1231 -1 1 0 0.1293 -1 -1 0 0.1498 0 0 1 0.0585 0 0 -1 0.0528 1 1 -2 0.0993 -1 -1 2 0.1399 -1 -1 -1 0.1333 0 1 -2 0.0924 -2 -1 -1 0.1448 0 1 2 0.0988 1 0 2 0.1081 1 0 -2 0.1036 6 7 22 0.0941 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Dy1 I1 62.22(7) . . ? N1 Dy1 C10 83.64(11) . . ? N1 Dy1 C6 92.12(12) . . ? N1 Dy1 C8 134.74(12) . . ? N1 Dy1 C20 80.99(11) . . ? N1 Dy1 C19 96.75(12) . . ? N1 Dy1 C9 107.42(12) . . ? N1 Dy1 C16 99.30(11) . . ? N1 Dy1 C17 129.60(11) . . ? N1 Dy1 C18 127.79(11) . . ? N1 Dy1 C7 122.77(12) . . ? C10 Dy1 I1 102.05(9) . . ? C10 Dy1 C6 30.86(12) . . ? C10 Dy1 C20 152.23(12) . . ? C10 Dy1 C16 176.64(11) . . ? C10 Dy1 C17 146.38(12) . . ? C6 Dy1 I1 79.97(8) . . ? C6 Dy1 C16 146.73(12) . . ? C8 Dy1 I1 122.65(9) . . ? C8 Dy1 C10 51.15(12) . . ? C8 Dy1 C6 51.18(12) . . ? C8 Dy1 C20 137.97(13) . . ? C8 Dy1 C16 125.95(12) . . ? C8 Dy1 C17 95.35(12) . . ? C20 Dy1 I1 91.02(9) . . ? C20 Dy1 C6 170.53(13) . . ? C20 Dy1 C16 30.78(12) . . ? C20 Dy1 C17 51.29(12) . . ? C19 Dy1 I1 122.01(9) . . ? C19 Dy1 C10 130.37(12) . . ? C19 Dy1 C6 157.92(13) . . ? C19 Dy1 C8 110.34(13) . . ? C19 Dy1 C20 31.00(13) . . ? C19 Dy1 C9 106.70(13) . . ? C19 Dy1 C16 51.14(12) . . ? C19 Dy1 C17 51.57(12) . . ? C19 Dy1 C18 31.31(12) . . ? C19 Dy1 C7 137.95(14) . . ? C9 Dy1 I1 130.67(9) . . ? C9 Dy1 C10 31.00(13) . . ? C9 Dy1 C6 51.25(12) . . ? C9 Dy1 C8 31.08(13) . . ? C9 Dy1 C20 137.10(13) . . ? C9 Dy1 C16 147.63(13) . . ? C9 Dy1 C17 118.14(13) . . ? C9 Dy1 C18 97.36(12) . . ? C16 Dy1 I1 78.05(8) . . ? C17 Dy1 I1 99.17(9) . . ? C17 Dy1 C6 132.77(12) . . ? C17 Dy1 C16 30.97(12) . . ? C18 Dy1 I1 128.06(8) . . ? C18 Dy1 C10 128.22(12) . . ? C18 Dy1 C6 137.52(12) . . ? C18 Dy1 C8 86.84(12) . . ? C18 Dy1 C20 51.23(12) . . ? C18 Dy1 C16 50.97(12) . . ? C18 Dy1 C17 30.94(12) . . ? C7 Dy1 I1 91.53(9) . . ? C7 Dy1 C10 51.28(12) . . ? C7 Dy1 C6 31.04(13) . . ? C7 Dy1 C8 31.13(13) . . ? C7 Dy1 C20 153.90(13) . . ? C7 Dy1 C9 51.52(12) . . ? C7 Dy1 C16 125.40(12) . . ? C7 Dy1 C17 102.70(13) . . ? C7 Dy1 C18 108.75(13) . . ? C2 I1 Dy1 68.36(10) . . ? C5 N1 Dy1 144.1(2) . . ? C5 N1 C2 104.0(3) . . ? C2 N1 Dy1 111.1(2) . . ? N1 C5 I4 121.5(2) . . ? N1 C5 C4 111.5(3) . . ? C4 C5 I4 127.1(3) . . ? N1 C2 I1 118.1(3) . . ? N1 C2 C3 113.0(3) . . ? C3 C2 I1 128.8(3) . . ? C6 C10 Dy1 74.8(2) . . ? C6 C10 C9 108.2(4) . . ? C6 C10 C15 124.9(4) . . ? C9 C10 Dy1 73.9(2) . . ? C9 C10 C15 126.5(4) . . ? C15 C10 Dy1 123.0(3) . . ? C10 C6 Dy1 74.4(2) . . ? C10 C6 C11 124.7(4) . . ? C10 C6 C7 107.9(3) . . ? C11 C6 Dy1 125.0(3) . . ? C7 C6 Dy1 73.4(2) . . ? C7 C6 C11 126.9(4) . . ? C9 C8 Dy1 73.8(2) . . ? C9 C8 C7 107.7(4) . . ? C9 C8 C13 126.2(4) . . ? C7 C8 Dy1 73.6(2) . . ? C7 C8 C13 124.9(4) . . ? C13 C8 Dy1 128.3(3) . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? C19 C20 Dy1 73.3(2) . . ? C19 C20 C16 108.2(3) . . ? C19 C20 C25 125.8(4) . . ? C16 C20 Dy1 75.4(2) . . ? C16 C20 C25 125.8(4) . . ? C25 C20 Dy1 121.5(3) . . ? C20 C19 Dy1 75.7(2) . . ? C20 C19 C18 107.8(3) . . ? C20 C19 C24 127.4(4) . . ? C18 C19 Dy1 74.9(2) . . ? C18 C19 C24 124.2(4) . . ? C24 C19 Dy1 122.3(3) . . ? C5 C4 I3 126.8(3) . . ? C5 C4 C3 106.8(3) . . ? C3 C4 I3 126.4(3) . . ? C10 C9 Dy1 75.1(2) . . ? C10 C9 C8 108.0(3) . . ? C10 C9 C14 125.4(4) . . ? C8 C9 Dy1 75.1(2) . . ? C8 C9 C14 126.1(4) . . ? C14 C9 Dy1 121.7(3) . . ? C2 C3 I2 126.6(3) . . ? C2 C3 C4 104.7(3) . . ? C4 C3 I2 128.6(3) . . ? C21 C16 Dy1 127.0(3) . . ? C20 C16 Dy1 73.8(2) . . ? C20 C16 C21 126.4(4) . . ? C20 C16 C17 108.1(3) . . ? C17 C16 Dy1 73.8(2) . . ? C17 C16 C21 124.5(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 75.2(2) . . ? C16 C17 C22 125.5(4) . . ? C18 C17 Dy1 73.8(2) . . ? C18 C17 C16 107.5(3) . . ? C18 C17 C22 126.7(4) . . ? C22 C17 Dy1 122.4(3) . . ? C19 C18 Dy1 73.8(2) . . ? C19 C18 C23 124.6(4) . . ? C17 C18 Dy1 75.2(2) . . ? C17 C18 C19 108.4(4) . . ? C17 C18 C23 125.5(4) . . ? C23 C18 Dy1 128.0(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 75.6(2) . . ? C6 C7 C8 108.1(3) . . ? C6 C7 C12 125.8(4) . . ? C8 C7 Dy1 75.3(2) . . ? C8 C7 C12 125.6(4) . . ? C12 C7 Dy1 121.1(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 122.6(5) . . ? Cl1A C26 H26C 106.7 . . ? Cl1A C26 H26D 106.7 . . ? Cl1A C26 H26A 95.3 . . ? Cl1A C26 H26B 112.4 . . ? Cl1A C26 Cl1B 13.4(5) . . ? H26C C26 H26D 106.6 . . ? H26C C26 H26A 13.3 . . ? H26C C26 H26B 96.4 . . ? H26D C26 H26A 117.4 . . ? H26D C26 H26B 10.4 . . ? H26A C26 H26B 107.6 . . ? Cl1B C26 Cl2 114.5(4) . . ? Cl1B C26 H26C 120.1 . . ? Cl1B C26 H26D 101.1 . . ? 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 3.2390(3) . ? Dy1 N1 2.371(3) . ? Dy1 C10 2.654(4) . ? Dy1 C6 2.659(4) . ? Dy1 C8 2.654(4) . ? Dy1 C20 2.656(4) . ? Dy1 C19 2.626(4) . ? Dy1 C9 2.638(4) . ? Dy1 C16 2.677(4) . ? Dy1 C17 2.658(4) . ? Dy1 C18 2.640(4) . ? Dy1 C7 2.631(3) . ? I1 C2 2.087(4) . ? I4 C5 2.072(3) . ? I3 C4 2.072(4) . ? I2 C3 2.053(4) . ? Cl2 C26 1.722(6) . ? Cl1A C26 1.646(12) . ? N1 C5 1.371(5) . ? N1 C2 1.376(4) . ? C5 C4 1.382(5) . ? C2 C3 1.376(5) . ? C10 C6 1.414(5) . ? C10 C9 1.414(6) . ? C10 C15 1.500(6) . ? C6 C11 1.505(6) . ? C6 C7 1.416(6) . ? C8 C9 1.418(6) . ? C8 C7 1.418(6) . ? C8 C13 1.490(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C16 1.508(6) . ? C20 C19 1.412(6) . ? C20 C16 1.415(5) . ? C20 C25 1.504(6) . ? C19 C18 1.421(6) . ? C19 C24 1.511(6) . ? C4 C3 1.416(5) . ? C9 C14 1.510(6) . ? C16 C17 1.425(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12 C7 1.506(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C17 C18 1.413(5) . ? C17 C22 1.502(6) . ? C18 C23 1.499(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 H26C 0.9900 . ? C26 H26D 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 Cl1B 1.682(9) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Dy1 N1 C5 I4 12.2(5) . . . . ? Dy1 N1 C5 C4 -168.2(3) . . . . ? Dy1 N1 C2 I1 -5.0(3) . . . . ? Dy1 N1 C2 C3 171.9(2) . . . . ? Dy1 C10 C6 C11 122.1(4) . . . . ? Dy1 C10 C6 C7 -66.3(3) . . . . ? Dy1 C10 C9 C8 68.5(3) . . . . ? Dy1 C10 C9 C14 -118.5(4) . . . . ? Dy1 C6 C7 C8 -68.9(3) . . . . ? Dy1 C6 C7 C12 118.2(4) . . . . ? Dy1 C8 C9 C10 -68.5(3) . . . . ? Dy1 C8 C9 C14 118.6(4) . . . . ? Dy1 C8 C7 C6 69.1(3) . . . . ? Dy1 C8 C7 C12 -118.0(4) . . . . ? Dy1 C20 C19 C18 -68.6(3) . . . . ? Dy1 C20 C19 C24 119.9(4) . . . . ? Dy1 C20 C16 C21 -124.4(4) . . . . ? Dy1 C20 C16 C17 66.3(3) . . . . ? Dy1 C19 C18 C17 -67.9(3) . . . . ? Dy1 C19 C18 C23 125.3(4) . . . . ? Dy1 C16 C17 C18 67.4(2) . . . . ? Dy1 C16 C17 C22 -119.5(4) . . . . ? Dy1 C17 C18 C19 66.9(3) . . . . ? Dy1 C17 C18 C23 -126.5(4) . . . . ? I1 C2 C3 I2 -5.7(5) . . . . ? I1 C2 C3 C4 177.6(3) . . . . ? I4 C5 C4 I3 -1.0(5) . . . . ? I4 C5 C4 C3 -179.2(3) . . . . ? I3 C4 C3 I2 3.8(5) . . . . ? I3 C4 C3 C2 -179.6(3) . . . . ? N1 C5 C4 I3 179.5(2) . . . . ? N1 C5 C4 C3 1.3(4) . . . . ? N1 C2 C3 I2 177.8(2) . . . . ? N1 C2 C3 C4 1.1(4) . . . . ? C5 N1 C2 I1 -177.3(2) . . . . ? C5 N1 C2 C3 -0.4(4) . . . . ? C5 C4 C3 I2 -178.0(3) . . . . ? C5 C4 C3 C2 -1.4(4) . . . . ? C2 N1 C5 I4 179.8(2) . . . . ? C2 N1 C5 C4 -0.6(4) . . . . ? C10 C6 C7 Dy1 67.0(2) . . . . ? C10 C6 C7 C8 -2.0(4) . . . . ? C10 C6 C7 C12 -174.9(4) . . . . ? C6 C10 C9 Dy1 -67.5(3) . . . . ? C6 C10 C9 C8 1.0(4) . . . . ? C6 C10 C9 C14 174.0(4) . . . . ? C21 C16 C17 Dy1 124.1(4) . . . . ? C21 C16 C17 C18 -168.5(4) . . . . ? C21 C16 C17 C22 4.6(6) . . . . ? C20 C19 C18 Dy1 69.1(3) . . . . ? C20 C19 C18 C17 1.2(4) . . . . ? C20 C19 C18 C23 -165.5(4) . . . . ? C20 C16 C17 Dy1 -66.3(3) . . . . ? C20 C16 C17 C18 1.0(4) . . . . ? C20 C16 C17 C22 174.1(4) . . . . ? C19 C20 C16 Dy1 -66.6(3) . . . . ? C19 C20 C16 C21 169.0(4) . . . . ? C19 C20 C16 C17 -0.3(4) . . . . ? C9 C10 C6 Dy1 66.9(3) . . . . ? C9 C10 C6 C11 -171.1(4) . . . . ? C9 C10 C6 C7 0.6(4) . . . . ? C9 C8 C7 Dy1 -66.5(3) . . . . ? C9 C8 C7 C6 2.6(4) . . . . ? C9 C8 C7 C12 175.5(4) . . . . ? C16 C20 C19 Dy1 68.0(3) . . . . ? C16 C20 C19 C18 -0.6(4) . . . . ? C16 C20 C19 C24 -172.1(4) . . . . ? C16 C17 C18 Dy1 -68.3(3) . . . . ? C16 C17 C18 C19 -1.4(4) . . . . ? C16 C17 C18 C23 165.2(4) . . . . ? C25 C20 C19 Dy1 -117.1(4) . . . . ? C25 C20 C19 C18 174.3(4) . . . . ? C25 C20 C19 C24 2.8(7) . . . . ? C25 C20 C16 Dy1 118.5(4) . . . . ? C25 C20 C16 C21 -5.8(6) . . . . ? C25 C20 C16 C17 -175.1(4) . . . . ? C15 C10 C6 Dy1 -119.9(4) . . . . ? C15 C10 C6 C11 2.1(6) . . . . ? C15 C10 C6 C7 173.8(4) . . . . ? C15 C10 C9 Dy1 119.5(4) . . . . ? C15 C10 C9 C8 -172.0(4) . . . . ? C15 C10 C9 C14 0.9(6) . . . . ? C11 C6 C7 Dy1 -121.6(4) . . . . ? C11 C6 C7 C8 169.5(4) . . . . ? C11 C6 C7 C12 -3.5(6) . . . . ? C22 C17 C18 Dy1 118.7(4) . . . . ? C22 C17 C18 C19 -174.4(4) . . . . ? C22 C17 C18 C23 -7.8(6) . . . . ? C7 C8 C9 Dy1 66.3(3) . . . . ? C7 C8 C9 C10 -2.2(4) . . . . ? C7 C8 C9 C14 -175.1(4) . . . . ? C13 C8 C9 Dy1 -126.0(4) . . . . ? C13 C8 C9 C10 165.5(4) . . . . ? C13 C8 C9 C14 -7.4(6) . . . . ? C13 C8 C7 Dy1 125.6(4) . . . . ? C13 C8 C7 C6 -165.3(4) . . . . ? C13 C8 C7 C12 7.6(6) . . . . ? C24 C19 C18 Dy1 -119.0(4) . . . . ? C24 C19 C18 C17 173.1(4) . . . . ? C24 C19 C18 C23 6.3(6) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 1.0051 -1.0172 -0.0935 -0.0783 -0.0142 0.0325 1.0097 0.9951 -0.0055 0.0038 0.0040 0.0859 -1.0051 1.0172 0.0935 0.0783 0.0142 -0.0325 -1.0097 -0.9951 0.0055 -0.0038 -0.0040 -0.0859 0.0088 -0.0214 0.9982 -0.0100 0.0322 0.0044 -0.0088 0.0214 -0.9982 0.0100 -0.0322 -0.0044 0.9922 1.0380 -2.0018 0.0239 -0.0605 0.0770 -0.9922 -1.0380 2.0018 -0.0239 0.0605 -0.0770 -1.0185 -0.9737 -0.9927 0.0063 -0.0363 -0.0903 -0.0152 1.0490 -1.9524 0.0612 -0.0554 0.0178 -2.0259 -0.9626 -0.9432 0.0435 -0.0312 -0.1495 0.0198 0.9633 2.0403 0.0210 0.0736 0.0356 1.0249 -0.0539 1.9469 -0.0574 0.0594 0.0681 0.9899 0.0318 -2.0458 -0.0172 -0.0696 0.0503 6.0103 6.7665 22.4234 -0.1415 0.7602 0.6341