#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:50:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294477 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572189.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_1572189 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 101.5232(18) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.32380(19) _cell_length_b 14.2662(2) _cell_length_c 21.2517(4) _cell_measurement_reflns_used 21638 _cell_measurement_temperature 120.01(10) _cell_measurement_theta_max 31.6760 _cell_measurement_theta_min 2.8520 _cell_volume 3066.89(9) _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 120.01(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.9985 _diffrn_measured_fraction_theta_max 0.8381 _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 0.0373591000 _diffrn_orient_matrix_UB_12 0.0410203000 _diffrn_orient_matrix_UB_13 0.0099024000 _diffrn_orient_matrix_UB_21 0.0045435000 _diffrn_orient_matrix_UB_22 0.0090273000 _diffrn_orient_matrix_UB_23 -0.0323159000 _diffrn_orient_matrix_UB_31 -0.0591410000 _diffrn_orient_matrix_UB_32 0.0266085000 _diffrn_orient_matrix_UB_33 -0.0043046000 _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 0.0505 _diffrn_reflns_av_unetI/netI 0.0415 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.839 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 37712 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.839 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.709 _diffrn_reflns_theta_min 2.468 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.652 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.221 _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 2.355 _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 1.213 _refine_diff_density_min -1.443 _refine_diff_density_rms 0.183 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8716 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0289 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+1.1150P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.0697 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7391 _reflns_number_total 8716 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP120K _cod_depositor_comments 'Adding full bibliography for 1572175--1572199.cif.' _cod_original_cell_volume 3066.90(10) _cod_database_code 1572189 _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 0.526 _shelx_estimated_absorpt_t_min 0.202 _diffrn_oxdiff_digest_frames ; 012a95a050068a5cc01f5e11cd474fbae500740d297 ; _diffrn_oxdiff_digest_hkl ; 010ee5f9fc0855a1e4974468fe401d5d03dd61 ; _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_120_final.res created by SHELXL-2018/3 at 15:27:37 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 10.323797 14.266217 21.251744 90 101.5232 90 ZERR 4 0.000187 0.000245 0.000391 0 0.0018 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. 4 0 0 PLAN 14 SIZE 0.111 0.275 0.353 TEMP -153.14(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.031800 1.115000 FVAR 0.64249 DY1 4 0.805359 0.713050 0.339762 11.00000 0.01336 0.01293 = 0.01348 -0.00052 0.00025 0.00194 I1 5 0.525742 0.612223 0.283276 11.00000 0.01922 0.01642 = 0.01973 0.00083 0.00274 -0.00470 I4 5 0.819313 0.939707 0.201516 11.00000 0.01888 0.01951 = 0.02575 0.00291 0.00358 -0.00483 I3 5 0.481357 0.934039 0.081339 11.00000 0.02431 0.02274 = 0.01746 0.00483 0.00209 0.00708 I2 5 0.291062 0.716845 0.131651 11.00000 0.01618 0.02745 = 0.03898 0.00103 -0.00803 -0.00341 CL2 3 0.610610 0.629751 0.079886 11.00000 0.04041 0.03928 = 0.02854 0.00389 0.00659 0.01376 PART 1 CL1A 3 0.686500 0.445236 0.037846 10.50000 0.05350 0.03333 = 0.14940 -0.02381 -0.00415 -0.00025 PART 0 N1 6 0.676470 0.772823 0.242575 11.00000 0.01398 0.01590 = 0.01674 0.00018 0.00086 -0.00270 C5 1 0.667401 0.843950 0.198837 11.00000 0.01535 0.01488 = 0.01832 0.00157 0.00273 0.00065 C2 1 0.559588 0.725892 0.226766 11.00000 0.01711 0.01457 = 0.01900 0.00099 0.00339 -0.00064 C10 1 0.958131 0.647650 0.262911 11.00000 0.01593 0.01737 = 0.01844 0.00159 0.00368 0.00460 C6 1 0.887326 0.569285 0.278645 11.00000 0.01706 0.01269 = 0.02354 -0.00486 0.00528 -0.00003 C8 1 1.029855 0.618024 0.370361 11.00000 0.01816 0.02590 = 0.02142 -0.00081 -0.00128 0.01155 C21 1 0.518809 0.739836 0.424162 11.00000 0.01704 0.03218 = 0.02569 -0.00853 0.00344 -0.00198 AFIX 137 H21A 2 0.456306 0.758262 0.385106 11.00000 -1.50000 H21B 2 0.491813 0.767799 0.461654 11.00000 -1.50000 H21C 2 0.519551 0.671396 0.428176 11.00000 -1.50000 AFIX 0 C20 1 0.686824 0.854182 0.386845 11.00000 0.02571 0.01583 = 0.01751 -0.00228 0.00332 0.00357 C19 1 0.824470 0.870337 0.405435 11.00000 0.02486 0.01667 = 0.01859 -0.00171 0.00537 0.00228 C4 1 0.546685 0.842401 0.156237 11.00000 0.01503 0.01776 = 0.01856 0.00088 0.00221 0.00339 C9 1 1.045147 0.678154 0.319399 11.00000 0.01216 0.02198 = 0.03021 -0.00624 0.00450 0.00237 C3 1 0.475785 0.765442 0.174973 11.00000 0.01566 0.01921 = 0.02075 -0.00163 0.00039 -0.00040 C16 1 0.655642 0.773831 0.420383 11.00000 0.01931 0.01713 = 0.01536 -0.00106 0.00304 0.00390 C25 1 0.588067 0.916494 0.344094 11.00000 0.03530 0.02458 = 0.02714 0.00295 0.00221 0.01577 AFIX 137 H25A 2 0.633047 0.952231 0.315405 11.00000 -1.50000 H25B 2 0.548580 0.959885 0.370672 11.00000 -1.50000 H25C 2 0.518551 0.877764 0.318490 11.00000 -1.50000 AFIX 0 C15 1 0.951793 0.683680 0.196027 11.00000 0.03387 0.03241 = 0.02501 0.00282 0.01142 0.00725 AFIX 137 H15A 2 0.859222 0.692836 0.174915 11.00000 -1.50000 H15B 2 0.993073 0.638184 0.171613 11.00000 -1.50000 H15C 2 0.998946 0.743550 0.197871 11.00000 -1.50000 AFIX 0 C12 1 0.887639 0.470214 0.381748 11.00000 0.04197 0.02290 = 0.04206 0.01433 0.01958 0.01372 AFIX 137 H12A 2 0.879405 0.491359 0.424648 11.00000 -1.50000 H12B 2 0.953754 0.420139 0.385685 11.00000 -1.50000 H12C 2 0.802130 0.446476 0.358755 11.00000 -1.50000 AFIX 0 C11 1 0.799631 0.507897 0.230551 11.00000 0.02123 0.02886 = 0.04029 -0.01596 0.00543 -0.00080 AFIX 137 H11A 2 0.756463 0.461174 0.253204 11.00000 -1.50000 H11B 2 0.853003 0.476002 0.203752 11.00000 -1.50000 H11C 2 0.732280 0.546512 0.203357 11.00000 -1.50000 AFIX 0 C14 1 1.146870 0.754240 0.322244 11.00000 0.02076 0.03273 = 0.05537 -0.01083 0.00843 -0.00612 AFIX 137 H14A 2 1.110099 0.805496 0.293453 11.00000 -1.50000 H14B 2 1.225336 0.728895 0.308834 11.00000 -1.50000 H14C 2 1.171496 0.777934 0.366300 11.00000 -1.50000 AFIX 0 C17 1 0.774575 0.739604 0.459903 11.00000 0.02184 0.01752 = 0.01479 -0.00118 0.00324 0.00081 C18 1 0.878306 0.800358 0.450882 11.00000 0.01857 0.01780 = 0.01651 -0.00269 0.00101 -0.00122 C22 1 0.784918 0.660556 0.506664 11.00000 0.03091 0.02728 = 0.02397 0.00653 0.00466 0.00326 AFIX 137 H22A 2 0.722825 0.610890 0.488750 11.00000 -1.50000 H22B 2 0.763503 0.683205 0.546911 11.00000 -1.50000 H22C 2 0.875216 0.635677 0.515031 11.00000 -1.50000 AFIX 0 C7 1 0.929994 0.550954 0.345193 11.00000 0.02083 0.02056 = 0.02895 0.00476 0.00897 0.00925 C23 1 1.014205 0.804101 0.493063 11.00000 0.02365 0.03304 = 0.02416 -0.01060 -0.00037 -0.00329 AFIX 137 H23A 2 1.035944 0.742819 0.513257 11.00000 -1.50000 H23B 2 1.015751 0.851778 0.526403 11.00000 -1.50000 H23C 2 1.079269 0.820139 0.466952 11.00000 -1.50000 AFIX 0 C13 1 1.120960 0.609929 0.434482 11.00000 0.04153 0.04322 = 0.02796 -0.00909 -0.00999 0.02542 AFIX 137 H13A 2 1.171062 0.668298 0.444082 11.00000 -1.50000 H13B 2 1.182306 0.557724 0.433678 11.00000 -1.50000 H13C 2 1.069131 0.598468 0.467645 11.00000 -1.50000 AFIX 0 C24 1 0.901148 0.954465 0.389241 11.00000 0.03872 0.02212 = 0.03148 -0.00413 0.01093 -0.00855 AFIX 137 H24A 2 0.980322 0.933127 0.374540 11.00000 -1.50000 H24B 2 0.927278 0.993683 0.427536 11.00000 -1.50000 H24C 2 0.845455 0.991015 0.355171 11.00000 -1.50000 AFIX 0 C26 1 0.705014 0.559587 0.039446 11.00000 0.16062 0.03348 = 0.08668 0.01560 0.10123 0.02063 PART 1 AFIX 23 H26C 2 0.688929 0.581384 -0.005674 10.50000 -1.20000 H26D 2 0.799041 0.572624 0.058078 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.674391 0.568759 -0.007341 10.50000 -1.20000 H26B 2 0.798283 0.580346 0.050720 10.50000 -1.20000 AFIX 0 CL1B 3 0.697709 0.442595 0.056460 10.50000 0.05304 0.02857 = 0.03844 0.00845 0.02080 0.00912 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0697, GooF = S = 1.040, Restrained GooF = 1.040 for all data REM R1 = 0.0289 for 7391 Fo > 4sig(Fo) and 0.0376 for all 8716 data REM 317 parameters refined using 6 restraints END WGHT 0.0318 1.1148 REM Highest difference peak 1.213, deepest hole -1.443, 1-sigma level 0.183 Q1 1 0.9065 0.8982 0.1993 11.00000 0.05 0.98 Q2 1 0.7728 0.4802 0.0557 11.00000 0.05 0.88 Q3 1 0.8998 0.7154 0.3777 11.00000 0.05 0.87 Q4 1 0.8931 0.7165 0.2993 11.00000 0.05 0.83 Q5 1 0.9046 0.7435 0.3406 11.00000 0.05 0.81 Q6 1 0.1666 0.7764 0.1409 11.00000 0.05 0.81 Q7 1 0.6395 0.6599 0.2795 11.00000 0.05 0.81 Q8 1 0.7259 0.5632 0.0586 11.00000 0.05 0.75 Q9 1 0.9072 0.9711 0.2000 11.00000 0.05 0.72 Q10 1 0.7076 0.7193 0.3796 11.00000 0.05 0.71 Q11 1 0.4222 0.8854 0.0786 11.00000 0.05 0.71 Q12 1 0.7068 0.6763 0.3438 11.00000 0.05 0.70 Q13 1 0.9533 0.7130 0.2817 11.00000 0.05 0.70 Q14 1 0.7115 0.7469 0.3430 11.00000 0.05 0.69 ; _shelx_res_checksum 62497 _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 2.513 _oxdiff_exptl_absorpt_empirical_full_min 0.667 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 0.80536(2) 0.71305(2) 0.33976(2) 0.01360(5) Uani 1 1 d . . . . . I1 I 0.52574(2) 0.61222(2) 0.28328(2) 0.01862(6) Uani 1 1 d . . . . . I4 I 0.81931(2) 0.93971(2) 0.20152(2) 0.02150(6) Uani 1 1 d . . . . . I3 I 0.48136(2) 0.93404(2) 0.08134(2) 0.02179(6) Uani 1 1 d . . . . . I2 I 0.29106(2) 0.71685(2) 0.13165(2) 0.02942(7) Uani 1 1 d . . . . . Cl2 Cl 0.61061(11) 0.62975(8) 0.07989(5) 0.0361(2) Uani 1 1 d . . . . . Cl1A Cl 0.6865(9) 0.4452(6) 0.0378(4) 0.082(2) Uani 0.5 1 d . U P A 1 N1 N 0.6765(3) 0.77282(18) 0.24257(14) 0.0158(5) Uani 1 1 d . . . . . C5 C 0.6674(3) 0.8439(2) 0.19884(17) 0.0163(6) Uani 1 1 d . . . . . C2 C 0.5596(3) 0.7259(2) 0.22677(17) 0.0169(6) Uani 1 1 d . . . . . C10 C 0.9581(3) 0.6477(2) 0.26291(16) 0.0172(7) Uani 1 1 d . . . . . C6 C 0.8873(3) 0.5693(2) 0.27864(18) 0.0176(7) Uani 1 1 d . . . . . C8 C 1.0299(3) 0.6180(2) 0.37036(18) 0.0225(7) Uani 1 1 d . . . . . C21 C 0.5188(3) 0.7398(3) 0.42416(19) 0.0251(8) Uani 1 1 d . . . . . H21A H 0.456306 0.758262 0.385106 0.038 Uiso 1 1 calc R U . . . H21B H 0.491813 0.767799 0.461654 0.038 Uiso 1 1 calc R U . . . H21C H 0.519551 0.671396 0.428176 0.038 Uiso 1 1 calc R U . . . C20 C 0.6868(4) 0.8542(2) 0.38685(17) 0.0198(7) Uani 1 1 d . . . . . C19 C 0.8245(4) 0.8703(2) 0.40543(17) 0.0199(7) Uani 1 1 d . . . . . C4 C 0.5467(3) 0.8424(2) 0.15624(17) 0.0173(6) Uani 1 1 d . . . . . C9 C 1.0451(3) 0.6782(2) 0.31940(19) 0.0214(7) Uani 1 1 d . . . . . C3 C 0.4758(3) 0.7654(2) 0.17497(17) 0.0190(7) Uani 1 1 d . . . . . C16 C 0.6556(3) 0.7738(2) 0.42038(17) 0.0173(7) Uani 1 1 d . . . . . C25 C 0.5881(4) 0.9165(3) 0.3441(2) 0.0296(9) Uani 1 1 d . . . . . H25A H 0.633047 0.952231 0.315405 0.044 Uiso 1 1 calc R U . . . H25B H 0.548580 0.959885 0.370672 0.044 Uiso 1 1 calc R U . . . H25C H 0.518551 0.877764 0.318490 0.044 Uiso 1 1 calc R U . . . C15 C 0.9518(4) 0.6837(3) 0.19603(19) 0.0297(8) Uani 1 1 d . . . . . H15A H 0.859222 0.692836 0.174915 0.044 Uiso 1 1 calc R U . . . H15B H 0.993073 0.638184 0.171613 0.044 Uiso 1 1 calc R U . . . H15C H 0.998946 0.743550 0.197871 0.044 Uiso 1 1 calc R U . . . C12 C 0.8876(4) 0.4702(3) 0.3817(2) 0.0341(10) Uani 1 1 d . . . . . H12A H 0.879405 0.491359 0.424648 0.051 Uiso 1 1 calc R U . . . H12B H 0.953754 0.420139 0.385685 0.051 Uiso 1 1 calc R U . . . H12C H 0.802130 0.446476 0.358755 0.051 Uiso 1 1 calc R U . . . C11 C 0.7996(4) 0.5079(3) 0.2306(2) 0.0302(9) Uani 1 1 d . . . . . H11A H 0.756463 0.461174 0.253204 0.045 Uiso 1 1 calc R U . . . H11B H 0.853003 0.476002 0.203752 0.045 Uiso 1 1 calc R U . . . H11C H 0.732280 0.546512 0.203357 0.045 Uiso 1 1 calc R U . . . C14 C 1.1469(4) 0.7542(3) 0.3222(3) 0.0362(10) Uani 1 1 d . . . . . H14A H 1.110099 0.805496 0.293453 0.054 Uiso 1 1 calc R U . . . H14B H 1.225336 0.728895 0.308834 0.054 Uiso 1 1 calc R U . . . H14C H 1.171496 0.777934 0.366300 0.054 Uiso 1 1 calc R U . . . C17 C 0.7746(3) 0.7396(2) 0.45990(17) 0.0181(6) Uani 1 1 d . . . . . C18 C 0.8783(3) 0.8004(2) 0.45088(17) 0.0180(7) Uani 1 1 d . . . . . C22 C 0.7849(4) 0.6606(3) 0.50666(19) 0.0275(8) Uani 1 1 d . . . . . H22A H 0.722825 0.610890 0.488750 0.041 Uiso 1 1 calc R U . . . H22B H 0.763503 0.683205 0.546911 0.041 Uiso 1 1 calc R U . . . H22C H 0.875216 0.635677 0.515031 0.041 Uiso 1 1 calc R U . . . C7 C 0.9300(4) 0.5510(2) 0.34519(19) 0.0229(7) Uani 1 1 d . . . . . C23 C 1.0142(4) 0.8041(3) 0.49306(19) 0.0277(8) Uani 1 1 d . . . . . H23A H 1.035944 0.742819 0.513257 0.041 Uiso 1 1 calc R U . . . H23B H 1.015751 0.851778 0.526403 0.041 Uiso 1 1 calc R U . . . H23C H 1.079269 0.820139 0.466952 0.041 Uiso 1 1 calc R U . . . C13 C 1.1210(5) 0.6099(3) 0.4345(2) 0.0399(11) Uani 1 1 d . . . . . H13A H 1.171062 0.668298 0.444082 0.060 Uiso 1 1 calc R U . . . H13B H 1.182306 0.557724 0.433678 0.060 Uiso 1 1 calc R U . . . H13C H 1.069131 0.598468 0.467645 0.060 Uiso 1 1 calc R U . . . C24 C 0.9011(4) 0.9545(3) 0.3892(2) 0.0302(9) Uani 1 1 d . . . . . H24A H 0.980322 0.933127 0.374540 0.045 Uiso 1 1 calc R U . . . H24B H 0.927278 0.993683 0.427536 0.045 Uiso 1 1 calc R U . . . H24C H 0.845455 0.991015 0.355171 0.045 Uiso 1 1 calc R U . . . C26 C 0.7050(9) 0.5596(3) 0.0394(4) 0.083(3) Uani 1 1 d . . . . . H26C H 0.688929 0.581384 -0.005674 0.100 Uiso 0.5 1 calc R U P A 1 H26D H 0.799041 0.572624 0.058078 0.100 Uiso 0.5 1 calc R U P A 1 H26A H 0.674391 0.568759 -0.007341 0.100 Uiso 0.5 1 calc R U P A -1 H26B H 0.798283 0.580346 0.050720 0.100 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.6977(8) 0.4426(5) 0.0565(2) 0.0384(12) 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 0.01336(8) 0.01293(8) 0.01348(8) -0.00052(5) 0.00025(6) 0.00194(5) I1 0.01922(11) 0.01642(11) 0.01973(11) 0.00083(8) 0.00274(8) -0.00470(7) I4 0.01888(12) 0.01951(11) 0.02575(13) 0.00291(8) 0.00358(9) -0.00483(8) I3 0.02431(13) 0.02274(12) 0.01746(11) 0.00483(8) 0.00209(9) 0.00708(8) I2 0.01618(12) 0.02745(13) 0.03898(16) 0.00103(10) -0.00803(10) -0.00341(8) Cl2 0.0404(6) 0.0393(5) 0.0285(5) 0.0039(4) 0.0066(4) 0.0138(4) Cl1A 0.054(3) 0.033(3) 0.149(7) -0.024(4) -0.004(4) -0.0003(18) N1 0.0140(13) 0.0159(13) 0.0167(14) 0.0002(11) 0.0009(11) -0.0027(10) C5 0.0153(15) 0.0149(15) 0.0183(16) 0.0016(12) 0.0027(12) 0.0007(11) C2 0.0171(16) 0.0146(15) 0.0190(17) 0.0010(12) 0.0034(13) -0.0006(11) C10 0.0159(16) 0.0174(16) 0.0184(17) 0.0016(12) 0.0037(13) 0.0046(11) C6 0.0171(16) 0.0127(15) 0.0235(18) -0.0049(13) 0.0053(13) 0.0000(11) C8 0.0182(17) 0.0259(18) 0.0214(18) -0.0008(14) -0.0013(14) 0.0116(13) C21 0.0170(18) 0.032(2) 0.026(2) -0.0085(16) 0.0034(14) -0.0020(14) C20 0.0257(18) 0.0158(15) 0.0175(17) -0.0023(13) 0.0033(13) 0.0036(13) C19 0.0249(18) 0.0167(16) 0.0186(17) -0.0017(13) 0.0054(14) 0.0023(13) C4 0.0150(16) 0.0178(15) 0.0186(16) 0.0009(13) 0.0022(13) 0.0034(12) C9 0.0122(16) 0.0220(17) 0.030(2) -0.0062(15) 0.0045(14) 0.0024(12) C3 0.0157(16) 0.0192(16) 0.0208(17) -0.0016(13) 0.0004(13) -0.0004(12) C16 0.0193(17) 0.0171(15) 0.0154(16) -0.0011(12) 0.0030(13) 0.0039(12) C25 0.035(2) 0.0246(18) 0.027(2) 0.0030(16) 0.0022(17) 0.0158(16) C15 0.034(2) 0.032(2) 0.025(2) 0.0028(16) 0.0114(17) 0.0073(16) C12 0.042(2) 0.0229(19) 0.042(3) 0.0143(18) 0.020(2) 0.0137(17) C11 0.0212(19) 0.029(2) 0.040(2) -0.0160(17) 0.0054(16) -0.0008(14) C14 0.021(2) 0.033(2) 0.055(3) -0.011(2) 0.0084(19) -0.0061(16) C17 0.0218(17) 0.0175(16) 0.0148(16) -0.0012(13) 0.0032(13) 0.0008(12) C18 0.0186(17) 0.0178(16) 0.0165(16) -0.0027(13) 0.0010(13) -0.0012(12) C22 0.031(2) 0.0273(19) 0.0240(19) 0.0065(15) 0.0047(16) 0.0033(15) C7 0.0208(18) 0.0206(17) 0.029(2) 0.0048(14) 0.0090(15) 0.0093(13) C23 0.0237(19) 0.033(2) 0.024(2) -0.0106(16) -0.0004(15) -0.0033(15) C13 0.042(3) 0.043(3) 0.028(2) -0.0091(19) -0.0100(18) 0.025(2) C24 0.039(2) 0.0221(18) 0.031(2) -0.0041(16) 0.0109(18) -0.0085(16) C26 0.161(7) 0.033(3) 0.087(5) 0.016(3) 0.101(5) 0.021(3) Cl1B 0.053(3) 0.0286(17) 0.0384(15) 0.0085(13) 0.0208(18) 0.0091(16) 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 62.25(6) . . ? N1 Dy1 C10 83.68(10) . . ? N1 Dy1 C6 91.71(10) . . ? N1 Dy1 C8 134.89(11) . . ? N1 Dy1 C20 80.53(10) . . ? N1 Dy1 C19 97.15(10) . . ? N1 Dy1 C9 107.75(11) . . ? N1 Dy1 C16 98.36(10) . . ? N1 Dy1 C17 128.91(10) . . ? N1 Dy1 C18 128.07(10) . . ? N1 Dy1 C7 122.37(11) . . ? C10 Dy1 I1 102.19(7) . . ? C10 Dy1 C16 177.79(10) . . ? C10 Dy1 C17 147.04(10) . . ? C6 Dy1 I1 79.80(7) . . ? C6 Dy1 C10 30.84(10) . . ? C6 Dy1 C16 147.83(10) . . ? C6 Dy1 C17 133.62(11) . . ? C8 Dy1 I1 122.37(8) . . ? C8 Dy1 C10 51.23(11) . . ? C8 Dy1 C6 51.43(11) . . ? C8 Dy1 C20 137.89(11) . . ? C8 Dy1 C16 126.74(11) . . ? C8 Dy1 C17 95.94(11) . . ? C20 Dy1 I1 91.88(8) . . ? C20 Dy1 C10 150.88(11) . . ? C20 Dy1 C6 170.63(11) . . ? C20 Dy1 C16 30.94(10) . . ? C20 Dy1 C17 51.54(11) . . ? C19 Dy1 I1 122.92(8) . . ? C19 Dy1 C10 129.45(11) . . ? C19 Dy1 C6 157.16(11) . . ? C19 Dy1 C8 109.69(11) . . ? C19 Dy1 C20 31.09(11) . . ? C19 Dy1 C9 105.91(11) . . ? C19 Dy1 C16 51.25(11) . . ? C19 Dy1 C17 51.69(10) . . ? C19 Dy1 C18 31.31(10) . . ? C19 Dy1 C7 137.80(12) . . ? C9 Dy1 I1 130.61(8) . . ? C9 Dy1 C10 31.00(11) . . ? C9 Dy1 C6 51.26(10) . . ? C9 Dy1 C8 30.99(12) . . ? C9 Dy1 C20 136.21(11) . . ? C9 Dy1 C16 147.86(11) . . ? C9 Dy1 C17 118.61(11) . . ? C16 Dy1 I1 78.14(7) . . ? C17 Dy1 I1 98.66(8) . . ? C17 Dy1 C16 31.06(10) . . ? C18 Dy1 I1 127.97(7) . . ? C18 Dy1 C10 128.08(11) . . ? C18 Dy1 C6 137.68(11) . . ? C18 Dy1 C8 86.72(11) . . ? C18 Dy1 C20 51.39(11) . . ? C18 Dy1 C9 97.24(11) . . ? C18 Dy1 C16 51.09(11) . . ? C18 Dy1 C17 31.05(10) . . ? C7 Dy1 I1 91.02(9) . . ? C7 Dy1 C10 51.28(11) . . ? C7 Dy1 C6 31.10(12) . . ? C7 Dy1 C8 31.36(12) . . ? C7 Dy1 C20 155.01(11) . . ? C7 Dy1 C9 51.51(11) . . ? C7 Dy1 C16 126.60(11) . . ? C7 Dy1 C17 103.50(11) . . ? C7 Dy1 C18 108.94(12) . . ? C2 I1 Dy1 68.20(9) . . ? C5 N1 Dy1 143.8(2) . . ? C2 N1 Dy1 110.6(2) . . ? C2 N1 C5 105.1(3) . . ? N1 C5 I4 121.5(2) . . ? N1 C5 C4 111.3(3) . . ? C4 C5 I4 127.2(2) . . ? N1 C2 I1 118.8(2) . . ? N1 C2 C3 112.3(3) . . ? C3 C2 I1 128.8(3) . . ? C6 C10 Dy1 74.54(19) . . ? C6 C10 C9 108.3(3) . . ? C6 C10 C15 124.7(3) . . ? C9 C10 Dy1 74.03(19) . . ? C9 C10 C15 126.7(3) . . ? C15 C10 Dy1 122.9(2) . . ? C10 C6 Dy1 74.63(18) . . ? C10 C6 C11 124.8(3) . . ? C10 C6 C7 108.0(3) . . ? C11 C6 Dy1 125.1(2) . . ? C7 C6 Dy1 73.78(19) . . ? C7 C6 C11 126.5(3) . . ? C9 C8 Dy1 74.22(19) . . ? C9 C8 C7 107.6(3) . . ? C9 C8 C13 126.7(4) . . ? C7 C8 Dy1 73.79(19) . . ? C7 C8 C13 124.3(4) . . ? C13 C8 Dy1 128.5(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 73.50(19) . . ? C19 C20 C16 107.9(3) . . ? C19 C20 C25 126.2(3) . . ? C16 C20 Dy1 75.21(18) . . ? C16 C20 C25 125.7(3) . . ? C25 C20 Dy1 121.7(2) . . ? C20 C19 Dy1 75.42(19) . . ? C20 C19 C18 108.0(3) . . ? C20 C19 C24 127.3(3) . . ? C18 C19 Dy1 74.88(19) . . ? C18 C19 C24 124.0(3) . . ? C24 C19 Dy1 122.9(2) . . ? C5 C4 I3 127.3(2) . . ? C5 C4 C3 106.0(3) . . ? C3 C4 I3 126.7(3) . . ? C10 C9 Dy1 74.96(19) . . ? C10 C9 C14 125.1(4) . . ? C8 C9 Dy1 74.79(19) . . ? C8 C9 C10 108.3(3) . . ? C8 C9 C14 126.2(4) . . ? C14 C9 Dy1 121.8(2) . . ? C2 C3 I2 126.5(3) . . ? C2 C3 C4 105.3(3) . . ? C4 C3 I2 128.1(3) . . ? C21 C16 Dy1 126.6(2) . . ? C20 C16 Dy1 73.85(19) . . ? C20 C16 C21 126.4(3) . . ? C20 C16 C17 108.5(3) . . ? C17 C16 Dy1 74.13(19) . . ? C17 C16 C21 124.2(3) . . ? 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 74.81(19) . . ? C16 C17 C22 126.1(3) . . ? C18 C17 Dy1 73.72(19) . . ? C18 C17 C16 107.1(3) . . ? C18 C17 C22 126.5(3) . . ? C22 C17 Dy1 121.6(2) . . ? C19 C18 Dy1 73.8(2) . . ? C19 C18 C23 124.7(3) . . ? C17 C18 Dy1 75.23(19) . . ? C17 C18 C19 108.5(3) . . ? C17 C18 C23 125.4(3) . . ? C23 C18 Dy1 127.8(2) . . ? 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 75.12(18) . . ? C6 C7 C8 107.9(3) . . ? C6 C7 C12 126.3(4) . . ? C8 C7 Dy1 74.85(19) . . ? C8 C7 C12 125.6(4) . . ? C12 C7 Dy1 120.3(2) . . ? 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 107.2 . . ? Cl2 C26 H26D 107.2 . . ? Cl2 C26 H26A 108.8 . . ? Cl2 C26 H26B 108.8 . . ? Cl1A C26 Cl2 120.5(5) . . ? Cl1A C26 H26C 107.2 . . ? Cl1A C26 H26D 107.2 . . ? Cl1A C26 H26A 95.6 . . ? Cl1A C26 H26B 113.9 . . ? Cl1A C26 Cl1B 13.2(4) . . ? H26C C26 H26D 106.8 . . ? H26C C26 H26A 13.5 . . ? H26C C26 H26B 96.2 . . ? H26D C26 H26A 117.9 . . ? H26D C26 H26B 11.0 . . ? H26A C26 H26B 107.7 . . ? Cl1B C26 Cl2 113.8(3) . . ? Cl1B C26 H26C 120.3 . . ? Cl1B C26 H26D 100.4 . . ? Cl1B C26 H26A 108.8 . . ? Cl1B C26 H26B 108.8 . . ? 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 3.2340(3) . ? Dy1 N1 2.380(3) . ? Dy1 C10 2.656(3) . ? Dy1 C6 2.655(3) . ? Dy1 C8 2.651(3) . ? Dy1 C20 2.654(3) . ? Dy1 C19 2.629(3) . ? Dy1 C9 2.644(3) . ? Dy1 C16 2.671(3) . ? Dy1 C17 2.662(3) . ? Dy1 C18 2.643(3) . ? Dy1 C7 2.638(3) . ? I1 C2 2.088(3) . ? I4 C5 2.072(3) . ? I3 C4 2.066(3) . ? I2 C3 2.065(3) . ? Cl2 C26 1.739(5) . ? Cl1A C26 1.642(9) . ? N1 C5 1.367(4) . ? N1 C2 1.362(4) . ? C5 C4 1.387(5) . ? C2 C3 1.378(5) . ? C10 C6 1.412(5) . ? C10 C9 1.417(5) . ? C10 C15 1.501(5) . ? C6 C11 1.504(5) . ? C6 C7 1.419(5) . ? C8 C9 1.415(5) . ? C8 C7 1.430(5) . ? C8 C13 1.498(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C16 1.511(5) . ? C20 C19 1.416(5) . ? C20 C16 1.420(5) . ? C20 C25 1.512(5) . ? C19 C18 1.423(5) . ? C19 C24 1.515(5) . ? C4 C3 1.420(5) . ? C9 C14 1.503(5) . ? C16 C17 1.428(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 1.502(5) . ? 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 1.420(5) . ? C17 C22 1.493(5) . ? C18 C23 1.507(5) . ? 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 1.713(8) . ? 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 9.1(5) . . . . ? Dy1 N1 C5 C4 -169.8(3) . . . . ? Dy1 N1 C2 I1 -4.3(3) . . . . ? Dy1 N1 C2 C3 172.9(2) . . . . ? Dy1 C10 C6 C11 122.3(3) . . . . ? Dy1 C10 C6 C7 -66.8(2) . . . . ? Dy1 C10 C9 C8 68.0(2) . . . . ? Dy1 C10 C9 C14 -118.6(3) . . . . ? Dy1 C6 C7 C8 -68.3(2) . . . . ? Dy1 C6 C7 C12 116.9(3) . . . . ? Dy1 C8 C9 C10 -68.1(2) . . . . ? Dy1 C8 C9 C14 118.5(4) . . . . ? Dy1 C8 C7 C6 68.5(2) . . . . ? Dy1 C8 C7 C12 -116.7(3) . . . . ? Dy1 C20 C19 C18 -68.4(2) . . . . ? Dy1 C20 C19 C24 120.5(4) . . . . ? Dy1 C20 C16 C21 -124.0(3) . . . . ? Dy1 C20 C16 C17 66.6(2) . . . . ? Dy1 C19 C18 C17 -67.9(2) . . . . ? Dy1 C19 C18 C23 125.2(3) . . . . ? Dy1 C16 C17 C18 67.2(2) . . . . ? Dy1 C16 C17 C22 -118.3(3) . . . . ? Dy1 C17 C18 C19 66.9(2) . . . . ? Dy1 C17 C18 C23 -126.2(3) . . . . ? I1 C2 C3 I2 -5.3(5) . . . . ? I1 C2 C3 C4 177.9(2) . . . . ? I4 C5 C4 I3 0.9(5) . . . . ? I4 C5 C4 C3 -178.4(2) . . . . ? I3 C4 C3 I2 3.2(5) . . . . ? I3 C4 C3 C2 180.0(2) . . . . ? N1 C5 C4 I3 179.6(2) . . . . ? N1 C5 C4 C3 0.3(4) . . . . ? N1 C2 C3 I2 177.8(2) . . . . ? N1 C2 C3 C4 1.0(4) . . . . ? C5 N1 C2 I1 -178.0(2) . . . . ? C5 N1 C2 C3 -0.8(4) . . . . ? C5 C4 C3 I2 -177.5(3) . . . . ? C5 C4 C3 C2 -0.7(4) . . . . ? C2 N1 C5 I4 179.1(2) . . . . ? C2 N1 C5 C4 0.3(4) . . . . ? C10 C6 C7 Dy1 67.3(2) . . . . ? C10 C6 C7 C8 -1.0(4) . . . . ? C10 C6 C7 C12 -175.7(3) . . . . ? C6 C10 C9 Dy1 -67.3(2) . . . . ? C6 C10 C9 C8 0.7(4) . . . . ? C6 C10 C9 C14 174.2(3) . . . . ? C21 C16 C17 Dy1 123.9(3) . . . . ? C21 C16 C17 C18 -169.0(3) . . . . ? C21 C16 C17 C22 5.5(5) . . . . ? C20 C19 C18 Dy1 68.8(2) . . . . ? C20 C19 C18 C17 0.9(4) . . . . ? C20 C19 C18 C23 -166.1(3) . . . . ? C20 C16 C17 Dy1 -66.4(2) . . . . ? C20 C16 C17 C18 0.7(4) . . . . ? C20 C16 C17 C22 175.2(3) . . . . ? C19 C20 C16 Dy1 -66.8(2) . . . . ? C19 C20 C16 C21 169.2(3) . . . . ? C19 C20 C16 C17 -0.2(4) . . . . ? C9 C10 C6 Dy1 66.9(2) . . . . ? C9 C10 C6 C11 -170.7(3) . . . . ? C9 C10 C6 C7 0.2(4) . . . . ? C9 C8 C7 Dy1 -67.1(2) . . . . ? C9 C8 C7 C6 1.4(4) . . . . ? C9 C8 C7 C12 176.2(3) . . . . ? C16 C20 C19 Dy1 68.0(2) . . . . ? C16 C20 C19 C18 -0.4(4) . . . . ? C16 C20 C19 C24 -171.6(3) . . . . ? C16 C17 C18 Dy1 -67.9(2) . . . . ? C16 C17 C18 C19 -1.0(4) . . . . ? C16 C17 C18 C23 165.9(3) . . . . ? C25 C20 C19 Dy1 -117.6(4) . . . . ? C25 C20 C19 C18 174.0(3) . . . . ? C25 C20 C19 C24 2.9(6) . . . . ? C25 C20 C16 Dy1 118.7(3) . . . . ? C25 C20 C16 C21 -5.3(6) . . . . ? C25 C20 C16 C17 -174.7(3) . . . . ? C15 C10 C6 Dy1 -119.6(3) . . . . ? C15 C10 C6 C11 2.7(5) . . . . ? C15 C10 C6 C7 173.6(3) . . . . ? C15 C10 C9 Dy1 119.4(3) . . . . ? C15 C10 C9 C8 -172.6(3) . . . . ? C15 C10 C9 C14 0.9(5) . . . . ? C11 C6 C7 Dy1 -122.0(3) . . . . ? C11 C6 C7 C8 169.7(3) . . . . ? C11 C6 C7 C12 -5.0(6) . . . . ? C22 C17 C18 Dy1 117.6(3) . . . . ? C22 C17 C18 C19 -175.5(3) . . . . ? C22 C17 C18 C23 -8.6(6) . . . . ? C7 C8 C9 Dy1 66.8(2) . . . . ? C7 C8 C9 C10 -1.3(4) . . . . ? C7 C8 C9 C14 -174.7(3) . . . . ? C13 C8 C9 Dy1 -126.5(4) . . . . ? C13 C8 C9 C10 165.4(3) . . . . ? C13 C8 C9 C14 -8.0(6) . . . . ? C13 C8 C7 Dy1 125.8(4) . . . . ? C13 C8 C7 C6 -165.7(3) . . . . ? C13 C8 C7 C12 9.1(6) . . . . ? C24 C19 C18 Dy1 -119.7(3) . . . . ? C24 C19 C18 C17 172.4(3) . . . . ? C24 C19 C18 C23 5.4(5) . . . . ? 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 -1.0013 -1.0020 0.0175 -0.0783 -0.0142 0.0325 -1.0022 1.0015 0.0143 0.0038 0.0040 0.0859 1.0013 1.0020 -0.0175 0.0783 0.0142 -0.0325 1.0022 -1.0015 -0.0143 -0.0038 -0.0040 -0.0859 -0.0030 -0.0012 -0.9986 -0.0100 0.0322 0.0044 0.0030 0.0012 0.9986 0.0100 -0.0322 -0.0044 -0.9962 1.0038 2.0116 0.0239 -0.0605 0.0770 0.9962 -1.0038 -2.0116 -0.0239 0.0605 -0.0770 1.0052 -1.0003 0.9843 0.0063 -0.0363 -0.0903 0.0055 1.0041 1.9957 0.0612 -0.0554 0.0178 2.0069 -1.0001 0.9684 0.0435 -0.0312 -0.1495 -0.0064 0.9994 -1.9988 0.0210 0.0736 0.0356 -1.0077 -0.0026 -1.9814 -0.0574 0.0594 0.0681 -0.9958 0.0021 2.0132 -0.0172 -0.0696 0.0503 -5.8346 7.2511 -22.3188 -0.1415 0.7602 0.6341