#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572192.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_1572192 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 101.5531(18) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.33049(19) _cell_length_b 14.2778(2) _cell_length_c 21.2557(4) _cell_measurement_reflns_used 21331 _cell_measurement_temperature 130.15(10) _cell_measurement_theta_max 31.4070 _cell_measurement_theta_min 2.6170 _cell_volume 3071.63(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 130.15(10) _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 0.841 _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 -0.0373821000 _diffrn_orient_matrix_UB_12 0.0409942000 _diffrn_orient_matrix_UB_13 -0.0098310000 _diffrn_orient_matrix_UB_21 -0.0044785000 _diffrn_orient_matrix_UB_22 0.0089067000 _diffrn_orient_matrix_UB_23 0.0323341000 _diffrn_orient_matrix_UB_31 0.0590785000 _diffrn_orient_matrix_UB_32 0.0266144000 _diffrn_orient_matrix_UB_33 0.0043286000 _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 0.0506 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.841 _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 37863 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.841 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.692 _diffrn_reflns_theta_min 2.467 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.642 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.222 _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 2.352 _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 1.159 _refine_diff_density_min -1.262 _refine_diff_density_rms 0.182 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8742 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0297 _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^)+(0.0322P)^2^+1.2207P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.0704 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7312 _reflns_number_total 8742 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP130K _cod_original_cell_volume 3071.64(10) _cod_database_code 1572192 _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 0.203 _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_130_final.res created by SHELXL-2018/3 at 15:33:57 on 10-Jul-2023 REM Old TITL FED728_100_Final in P21/c #14 REM SHELXT solution in P2(1)/c: R1 0.076, Rweak 0.002, Alpha 0.023 REM 0.488 for 262 systematic absences, Orientation as input REM Formula found by SHELXT: C24 N Cl2 I4 Dy CELL 0.71073 10.330486 14.277845 21.255742 90 101.5531 90 ZERR 4 0.00019 0.000249 0.000398 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 -143.0(1) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.032200 1.220700 FVAR 0.64016 DY1 4 0.805238 0.713321 0.339691 11.00000 0.01429 0.01424 = 0.01445 -0.00047 0.00030 0.00206 I1 5 0.525702 0.612649 0.282994 11.00000 0.02066 0.01780 = 0.02154 0.00104 0.00307 -0.00511 I4 5 0.819546 0.939711 0.201304 11.00000 0.02042 0.02143 = 0.02769 0.00330 0.00372 -0.00513 I3 5 0.481665 0.934463 0.081360 11.00000 0.02652 0.02452 = 0.01889 0.00512 0.00235 0.00769 I2 5 0.291254 0.717514 0.131465 11.00000 0.01762 0.02989 = 0.04196 0.00100 -0.00873 -0.00370 CL2 3 0.610449 0.629389 0.079836 11.00000 0.04443 0.04172 = 0.03115 0.00370 0.00734 0.01426 PART 1 CL1A 3 0.686177 0.446763 0.038134 10.50000 0.05586 0.03071 = 0.16241 -0.01591 -0.00710 -0.00001 PART 0 N1 6 0.677050 0.772677 0.242306 11.00000 0.01366 0.01892 = 0.01727 -0.00010 -0.00101 -0.00206 C5 1 0.667368 0.844121 0.198662 11.00000 0.01750 0.01688 = 0.01839 0.00172 0.00293 -0.00046 C2 1 0.559806 0.726316 0.226425 11.00000 0.01770 0.01906 = 0.02000 -0.00198 0.00644 -0.00109 C10 1 0.958237 0.647692 0.262973 11.00000 0.01766 0.01752 = 0.02100 0.00156 0.00397 0.00514 C6 1 0.886904 0.569335 0.278875 11.00000 0.01979 0.01331 = 0.02472 -0.00298 0.00479 0.00244 C8 1 1.029914 0.618668 0.370391 11.00000 0.01916 0.02635 = 0.02277 -0.00316 -0.00086 0.01173 C21 1 0.518826 0.740048 0.423905 11.00000 0.01928 0.03683 = 0.03003 -0.00571 0.00575 0.00138 AFIX 137 H21A 2 0.455710 0.761345 0.385858 11.00000 -1.50000 H21B 2 0.493602 0.765344 0.462592 11.00000 -1.50000 H21C 2 0.518393 0.671460 0.425608 11.00000 -1.50000 AFIX 0 C20 1 0.686492 0.854151 0.386509 11.00000 0.02782 0.01716 = 0.01766 -0.00270 0.00190 0.00688 C19 1 0.823790 0.870377 0.405255 11.00000 0.02876 0.01592 = 0.02146 -0.00384 0.00630 0.00063 C4 1 0.547002 0.842640 0.156432 11.00000 0.01663 0.02034 = 0.01766 0.00078 0.00239 0.00388 C9 1 1.044814 0.678676 0.319532 11.00000 0.01343 0.02217 = 0.03194 -0.00707 0.00477 0.00028 C3 1 0.476050 0.765963 0.174469 11.00000 0.01374 0.02029 = 0.01895 0.00010 -0.00265 0.00158 C16 1 0.655385 0.773883 0.420299 11.00000 0.01796 0.02000 = 0.01924 -0.00387 0.00264 0.00385 C25 1 0.587670 0.916176 0.344106 11.00000 0.03649 0.03151 = 0.02462 0.00220 0.00195 0.01852 AFIX 137 H25A 2 0.632822 0.953676 0.316424 11.00000 -1.50000 H25B 2 0.546059 0.957870 0.370858 11.00000 -1.50000 H25C 2 0.519854 0.877325 0.317458 11.00000 -1.50000 AFIX 0 C15 1 0.951701 0.683336 0.195939 11.00000 0.03800 0.03239 = 0.02451 0.00480 0.01226 0.00886 AFIX 137 H15A 2 0.859086 0.690883 0.174466 11.00000 -1.50000 H15B 2 0.994889 0.638467 0.171958 11.00000 -1.50000 H15C 2 0.996863 0.743919 0.197648 11.00000 -1.50000 AFIX 0 C12 1 0.887511 0.470962 0.381973 11.00000 0.04436 0.02776 = 0.04611 0.01457 0.01974 0.01118 AFIX 137 H12A 2 0.884268 0.491379 0.425649 11.00000 -1.50000 H12B 2 0.950823 0.419418 0.383880 11.00000 -1.50000 H12C 2 0.799695 0.449625 0.360318 11.00000 -1.50000 AFIX 0 C11 1 0.800218 0.508149 0.230644 11.00000 0.02563 0.03215 = 0.04181 -0.01611 0.00463 -0.00099 AFIX 137 H11A 2 0.754934 0.462465 0.253052 11.00000 -1.50000 H11B 2 0.854431 0.475086 0.204839 11.00000 -1.50000 H11C 2 0.734636 0.546908 0.202519 11.00000 -1.50000 AFIX 0 C14 1 1.146690 0.754164 0.322323 11.00000 0.02483 0.03702 = 0.05683 -0.01204 0.01056 -0.00775 AFIX 137 H14A 2 1.113573 0.802437 0.290366 11.00000 -1.50000 H14B 2 1.228155 0.727169 0.313160 11.00000 -1.50000 H14C 2 1.164933 0.782230 0.365267 11.00000 -1.50000 AFIX 0 C17 1 0.774520 0.740193 0.459575 11.00000 0.02405 0.01948 = 0.01613 0.00029 0.00415 0.00053 C18 1 0.877936 0.800849 0.450786 11.00000 0.01821 0.02123 = 0.01734 -0.00354 0.00167 0.00164 C22 1 0.784756 0.661160 0.506688 11.00000 0.03420 0.02808 = 0.02536 0.00828 0.00444 0.00397 AFIX 137 H22A 2 0.729570 0.608858 0.487142 11.00000 -1.50000 H22B 2 0.754477 0.682366 0.545153 11.00000 -1.50000 H22C 2 0.876916 0.640563 0.518586 11.00000 -1.50000 AFIX 0 C7 1 0.930018 0.551332 0.345318 11.00000 0.02165 0.01867 = 0.03041 0.00574 0.00900 0.00712 C23 1 1.013365 0.805089 0.493020 11.00000 0.02295 0.03576 = 0.02721 -0.01246 -0.00148 -0.00277 AFIX 137 H23A 2 1.033052 0.745273 0.515513 11.00000 -1.50000 H23B 2 1.016128 0.855587 0.524488 11.00000 -1.50000 H23C 2 1.079124 0.817171 0.466567 11.00000 -1.50000 AFIX 0 C13 1 1.120314 0.610637 0.434489 11.00000 0.03773 0.05185 = 0.03105 -0.00899 -0.00942 0.02465 AFIX 137 H13A 2 1.170492 0.668911 0.444127 11.00000 -1.50000 H13B 2 1.181552 0.558383 0.433862 11.00000 -1.50000 H13C 2 1.068198 0.599350 0.467527 11.00000 -1.50000 AFIX 0 C24 1 0.900303 0.954571 0.388891 11.00000 0.04403 0.02067 = 0.03404 -0.00575 0.01473 -0.00685 AFIX 137 H24A 2 0.982421 0.933470 0.376988 11.00000 -1.50000 H24B 2 0.921239 0.996044 0.426287 11.00000 -1.50000 H24C 2 0.846681 0.988593 0.352825 11.00000 -1.50000 AFIX 0 C26 1 0.704541 0.559705 0.039368 11.00000 0.16861 0.03704 = 0.08429 0.02077 0.09810 0.02452 PART 1 AFIX 23 H26C 2 0.688021 0.581318 -0.005791 10.50000 -1.20000 H26D 2 0.798561 0.572862 0.057845 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.673365 0.568804 -0.007388 10.50000 -1.20000 H26B 2 0.797560 0.580947 0.050396 10.50000 -1.20000 AFIX 0 CL1B 3 0.698999 0.441281 0.056443 10.50000 0.06022 0.03304 = 0.04029 0.01262 0.02284 0.01618 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0704, GooF = S = 1.032, Restrained GooF = 1.032 for all data REM R1 = 0.0297 for 7312 Fo > 4sig(Fo) and 0.0394 for all 8742 data REM 317 parameters refined using 6 restraints END WGHT 0.0322 1.2206 REM Highest difference peak 1.159, deepest hole -1.262, 1-sigma level 0.182 Q1 1 0.7244 0.5628 0.0569 11.00000 0.05 0.95 Q2 1 0.5477 0.9374 0.0415 11.00000 0.05 0.90 Q3 1 0.7124 0.6776 0.3393 11.00000 0.05 0.84 Q4 1 0.7678 0.4755 0.0502 11.00000 0.05 0.83 Q5 1 0.9025 0.8995 0.2008 11.00000 0.05 0.81 Q6 1 0.9008 0.7434 0.3414 11.00000 0.05 0.78 Q7 1 0.9244 0.7015 0.2845 11.00000 0.05 0.76 Q8 1 0.4392 0.6548 0.2811 11.00000 0.05 0.73 Q9 1 0.7669 0.6417 0.3380 11.00000 0.05 0.68 Q10 1 0.8046 1.0006 0.2000 11.00000 0.05 0.67 Q11 1 0.7215 0.7171 0.3790 11.00000 0.05 0.66 Q12 1 1.3646 0.6547 0.2970 11.00000 0.05 0.65 Q13 1 0.7229 0.7580 0.3425 11.00000 0.05 0.65 Q14 1 0.8930 0.9342 0.1615 11.00000 0.05 0.64 ; _shelx_res_checksum 95126 _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 2.574 _oxdiff_exptl_absorpt_empirical_full_min 0.671 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 0.80524(2) 0.71332(2) 0.33969(2) 0.01469(5) Uani 1 1 d . . . . . I1 I 0.52570(2) 0.61265(2) 0.28299(2) 0.02016(6) Uani 1 1 d . . . . . I4 I 0.81955(2) 0.93971(2) 0.20130(2) 0.02334(6) Uani 1 1 d . . . . . I3 I 0.48167(2) 0.93446(2) 0.08136(2) 0.02362(6) Uani 1 1 d . . . . . I2 I 0.29125(2) 0.71751(2) 0.13146(2) 0.03187(7) Uani 1 1 d . . . . . Cl2 Cl 0.61045(12) 0.62939(8) 0.07984(5) 0.0391(2) Uani 1 1 d . . . . . Cl1A Cl 0.6862(8) 0.4468(5) 0.0381(4) 0.087(2) Uani 0.5 1 d . U P A 1 N1 N 0.6770(3) 0.77268(19) 0.24231(14) 0.0172(6) Uani 1 1 d . . . . . C5 C 0.6674(3) 0.8441(2) 0.19866(17) 0.0177(6) Uani 1 1 d . . . . . C2 C 0.5598(3) 0.7263(2) 0.22642(17) 0.0185(7) Uani 1 1 d . . . . . C10 C 0.9582(3) 0.6477(2) 0.26297(17) 0.0187(7) Uani 1 1 d . . . . . C6 C 0.8869(3) 0.5693(2) 0.27888(18) 0.0192(7) Uani 1 1 d . . . . . C8 C 1.0299(4) 0.6187(3) 0.37039(18) 0.0235(8) Uani 1 1 d . . . . . C21 C 0.5188(4) 0.7400(3) 0.4239(2) 0.0286(8) Uani 1 1 d . . . . . H21A H 0.455710 0.761345 0.385858 0.043 Uiso 1 1 calc R U . . . H21B H 0.493602 0.765344 0.462592 0.043 Uiso 1 1 calc R U . . . H21C H 0.518393 0.671460 0.425608 0.043 Uiso 1 1 calc R U . . . C20 C 0.6865(4) 0.8542(2) 0.38651(17) 0.0212(7) Uani 1 1 d . . . . . C19 C 0.8238(4) 0.8704(2) 0.40525(18) 0.0219(7) Uani 1 1 d . . . . . C4 C 0.5470(3) 0.8426(2) 0.15643(17) 0.0184(7) Uani 1 1 d . . . . . C9 C 1.0448(3) 0.6787(2) 0.31953(19) 0.0225(7) Uani 1 1 d . . . . . C3 C 0.4761(3) 0.7660(2) 0.17447(17) 0.0185(7) Uani 1 1 d . . . . . C16 C 0.6554(3) 0.7739(2) 0.42030(17) 0.0192(7) Uani 1 1 d . . . . . C25 C 0.5877(4) 0.9162(3) 0.3441(2) 0.0315(9) Uani 1 1 d . . . . . H25A H 0.632822 0.953676 0.316424 0.047 Uiso 1 1 calc R U . . . H25B H 0.546059 0.957870 0.370858 0.047 Uiso 1 1 calc R U . . . H25C H 0.519854 0.877325 0.317458 0.047 Uiso 1 1 calc R U . . . C15 C 0.9517(4) 0.6833(3) 0.1959(2) 0.0308(9) Uani 1 1 d . . . . . H15A H 0.859086 0.690883 0.174466 0.046 Uiso 1 1 calc R U . . . H15B H 0.994889 0.638467 0.171958 0.046 Uiso 1 1 calc R U . . . H15C H 0.996863 0.743919 0.197648 0.046 Uiso 1 1 calc R U . . . C12 C 0.8875(5) 0.4710(3) 0.3820(2) 0.0379(10) Uani 1 1 d . . . . . H12A H 0.884268 0.491379 0.425649 0.057 Uiso 1 1 calc R U . . . H12B H 0.950823 0.419418 0.383880 0.057 Uiso 1 1 calc R U . . . H12C H 0.799695 0.449625 0.360318 0.057 Uiso 1 1 calc R U . . . C11 C 0.8002(4) 0.5081(3) 0.2306(2) 0.0335(9) Uani 1 1 d . . . . . H11A H 0.754934 0.462465 0.253052 0.050 Uiso 1 1 calc R U . . . H11B H 0.854431 0.475086 0.204839 0.050 Uiso 1 1 calc R U . . . H11C H 0.734636 0.546908 0.202519 0.050 Uiso 1 1 calc R U . . . C14 C 1.1467(4) 0.7542(3) 0.3223(3) 0.0392(11) Uani 1 1 d . . . . . H14A H 1.113573 0.802437 0.290366 0.059 Uiso 1 1 calc R U . . . H14B H 1.228155 0.727169 0.313160 0.059 Uiso 1 1 calc R U . . . H14C H 1.164933 0.782230 0.365267 0.059 Uiso 1 1 calc R U . . . C17 C 0.7745(4) 0.7402(2) 0.45957(17) 0.0199(7) Uani 1 1 d . . . . . C18 C 0.8779(3) 0.8008(2) 0.45079(17) 0.0192(7) Uani 1 1 d . . . . . C22 C 0.7848(4) 0.6612(3) 0.5067(2) 0.0294(8) Uani 1 1 d . . . . . H22A H 0.729570 0.608858 0.487142 0.044 Uiso 1 1 calc R U . . . H22B H 0.754477 0.682366 0.545153 0.044 Uiso 1 1 calc R U . . . H22C H 0.876916 0.640563 0.518586 0.044 Uiso 1 1 calc R U . . . C7 C 0.9300(4) 0.5513(2) 0.34532(19) 0.0231(7) Uani 1 1 d . . . . . C23 C 1.0134(4) 0.8051(3) 0.4930(2) 0.0295(8) Uani 1 1 d . . . . . H23A H 1.033052 0.745273 0.515513 0.044 Uiso 1 1 calc R U . . . H23B H 1.016128 0.855587 0.524488 0.044 Uiso 1 1 calc R U . . . H23C H 1.079124 0.817171 0.466567 0.044 Uiso 1 1 calc R U . . . C13 C 1.1203(5) 0.6106(3) 0.4345(2) 0.0425(12) Uani 1 1 d . . . . . H13A H 1.170492 0.668911 0.444127 0.064 Uiso 1 1 calc R U . . . H13B H 1.181552 0.558383 0.433862 0.064 Uiso 1 1 calc R U . . . H13C H 1.068198 0.599350 0.467527 0.064 Uiso 1 1 calc R U . . . C24 C 0.9003(4) 0.9546(3) 0.3889(2) 0.0320(9) Uani 1 1 d . . . . . H24A H 0.982421 0.933470 0.376988 0.048 Uiso 1 1 calc R U . . . H24B H 0.921239 0.996044 0.426287 0.048 Uiso 1 1 calc R U . . . H24C H 0.846681 0.988593 0.352825 0.048 Uiso 1 1 calc R U . . . C26 C 0.7045(9) 0.5597(4) 0.0394(4) 0.087(3) Uani 1 1 d . . . . . H26C H 0.688021 0.581318 -0.005791 0.104 Uiso 0.5 1 calc R U P A 1 H26D H 0.798561 0.572862 0.057845 0.104 Uiso 0.5 1 calc R U P A 1 H26A H 0.673365 0.568804 -0.007388 0.104 Uiso 0.5 1 calc R U P A -1 H26B H 0.797560 0.580947 0.050396 0.104 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.6990(7) 0.4413(5) 0.0564(2) 0.0427(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 0.01429(8) 0.01424(8) 0.01445(8) -0.00047(5) 0.00030(6) 0.00206(5) I1 0.02066(12) 0.01780(11) 0.02154(12) 0.00104(8) 0.00307(9) -0.00511(8) I4 0.02042(12) 0.02143(12) 0.02769(13) 0.00330(9) 0.00372(9) -0.00513(8) I3 0.02652(13) 0.02452(12) 0.01889(12) 0.00512(9) 0.00235(9) 0.00769(9) I2 0.01762(12) 0.02989(14) 0.04196(17) 0.00100(11) -0.00873(10) -0.00370(9) Cl2 0.0444(6) 0.0417(6) 0.0312(5) 0.0037(4) 0.0073(5) 0.0143(4) Cl1A 0.056(2) 0.031(2) 0.162(7) -0.016(4) -0.007(4) 0.0000(17) N1 0.0137(14) 0.0189(14) 0.0173(14) -0.0001(11) -0.0010(11) -0.0021(10) C5 0.0175(16) 0.0169(15) 0.0184(16) 0.0017(13) 0.0029(13) -0.0005(12) C2 0.0177(17) 0.0191(16) 0.0200(17) -0.0020(13) 0.0064(13) -0.0011(12) C10 0.0177(17) 0.0175(16) 0.0210(17) 0.0016(13) 0.0040(13) 0.0051(12) C6 0.0198(17) 0.0133(15) 0.0247(18) -0.0030(13) 0.0048(14) 0.0024(12) C8 0.0192(18) 0.0264(18) 0.0228(18) -0.0032(14) -0.0009(14) 0.0117(13) C21 0.0193(19) 0.037(2) 0.030(2) -0.0057(17) 0.0058(15) 0.0014(15) C20 0.0278(19) 0.0172(16) 0.0177(17) -0.0027(13) 0.0019(14) 0.0069(13) C19 0.0288(19) 0.0159(16) 0.0215(18) -0.0038(13) 0.0063(15) 0.0006(13) C4 0.0166(16) 0.0203(16) 0.0177(16) 0.0008(13) 0.0024(13) 0.0039(12) C9 0.0134(16) 0.0222(17) 0.032(2) -0.0071(15) 0.0048(14) 0.0003(12) C3 0.0137(16) 0.0203(16) 0.0189(17) 0.0001(13) -0.0027(12) 0.0016(12) C16 0.0180(17) 0.0200(16) 0.0192(17) -0.0039(13) 0.0026(13) 0.0039(12) C25 0.036(2) 0.032(2) 0.025(2) 0.0022(16) 0.0019(17) 0.0185(17) C15 0.038(2) 0.032(2) 0.025(2) 0.0048(17) 0.0123(17) 0.0089(17) C12 0.044(3) 0.028(2) 0.046(3) 0.0146(19) 0.020(2) 0.0112(18) C11 0.026(2) 0.032(2) 0.042(2) -0.0161(19) 0.0046(17) -0.0010(16) C14 0.025(2) 0.037(2) 0.057(3) -0.012(2) 0.011(2) -0.0077(17) C17 0.0240(18) 0.0195(16) 0.0161(16) 0.0003(13) 0.0042(13) 0.0005(13) C18 0.0182(17) 0.0212(16) 0.0173(17) -0.0035(13) 0.0017(13) 0.0016(12) C22 0.034(2) 0.0281(19) 0.025(2) 0.0083(16) 0.0044(16) 0.0040(16) C7 0.0217(18) 0.0187(16) 0.030(2) 0.0057(14) 0.0090(15) 0.0071(13) C23 0.0230(19) 0.036(2) 0.027(2) -0.0125(17) -0.0015(15) -0.0028(15) C13 0.038(3) 0.052(3) 0.031(2) -0.009(2) -0.0094(19) 0.025(2) C24 0.044(3) 0.0207(18) 0.034(2) -0.0057(16) 0.0147(19) -0.0069(16) C26 0.169(8) 0.037(3) 0.084(5) 0.021(3) 0.098(6) 0.025(4) Cl1B 0.060(3) 0.0330(17) 0.0403(15) 0.0126(12) 0.0228(18) 0.0162(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 62.24(7) . . ? N1 Dy1 C10 83.54(10) . . ? N1 Dy1 C6 91.60(10) . . ? N1 Dy1 C8 134.66(11) . . ? N1 Dy1 C20 80.66(10) . . ? N1 Dy1 C19 97.25(11) . . ? N1 Dy1 C9 107.57(11) . . ? N1 Dy1 C16 98.61(10) . . ? N1 Dy1 C17 129.07(10) . . ? N1 Dy1 C18 128.15(10) . . ? N1 Dy1 C7 122.24(11) . . ? C10 Dy1 I1 102.18(8) . . ? C10 Dy1 C16 177.66(10) . . ? C6 Dy1 I1 79.72(8) . . ? C6 Dy1 C10 30.94(10) . . ? C6 Dy1 C16 147.59(11) . . ? C6 Dy1 C17 133.57(11) . . ? C8 Dy1 I1 122.50(8) . . ? C8 Dy1 C10 51.15(11) . . ? C8 Dy1 C6 51.49(11) . . ? C8 Dy1 C16 126.72(11) . . ? C8 Dy1 C17 95.99(11) . . ? C20 Dy1 I1 91.79(8) . . ? C20 Dy1 C10 150.96(11) . . ? C20 Dy1 C6 170.53(11) . . ? C20 Dy1 C8 137.92(11) . . ? C20 Dy1 C16 31.01(11) . . ? C20 Dy1 C17 51.50(11) . . ? C19 Dy1 I1 122.81(8) . . ? C19 Dy1 C10 129.58(11) . . ? C19 Dy1 C6 157.36(11) . . ? C19 Dy1 C8 109.71(12) . . ? C19 Dy1 C20 31.06(11) . . ? C19 Dy1 C9 105.95(11) . . ? C19 Dy1 C16 51.23(11) . . ? C19 Dy1 C17 51.55(11) . . ? C19 Dy1 C18 31.27(11) . . ? C19 Dy1 C7 137.82(12) . . ? C9 Dy1 I1 130.68(8) . . ? C9 Dy1 C10 31.03(11) . . ? C9 Dy1 C6 51.43(11) . . ? C9 Dy1 C8 30.93(12) . . ? C9 Dy1 C20 136.22(11) . . ? C9 Dy1 C16 147.82(11) . . ? C9 Dy1 C17 118.56(12) . . ? C9 Dy1 C18 97.22(11) . . ? C16 Dy1 I1 78.12(8) . . ? C17 Dy1 I1 98.76(8) . . ? C17 Dy1 C10 147.00(11) . . ? C17 Dy1 C16 31.02(11) . . ? C18 Dy1 I1 127.98(8) . . ? C18 Dy1 C10 128.09(11) . . ? C18 Dy1 C6 137.72(11) . . ? C18 Dy1 C8 86.74(11) . . ? C18 Dy1 C20 51.41(11) . . ? C18 Dy1 C16 51.09(11) . . ? C18 Dy1 C17 30.99(11) . . ? C7 Dy1 I1 91.09(8) . . ? C7 Dy1 C10 51.23(11) . . ? C7 Dy1 C6 31.05(12) . . ? C7 Dy1 C8 31.42(12) . . ? C7 Dy1 C20 155.01(11) . . ? C7 Dy1 C9 51.55(11) . . ? C7 Dy1 C16 126.51(11) . . ? C7 Dy1 C17 103.54(11) . . ? C7 Dy1 C18 108.96(12) . . ? C2 I1 Dy1 68.21(10) . . ? C5 N1 Dy1 143.9(2) . . ? C2 N1 Dy1 110.8(2) . . ? C2 N1 C5 104.7(3) . . ? N1 C5 I4 121.3(2) . . ? N1 C5 C4 111.3(3) . . ? C4 C5 I4 127.4(3) . . ? N1 C2 I1 118.6(2) . . ? N1 C2 C3 112.5(3) . . ? C3 C2 I1 128.9(3) . . ? C6 C10 Dy1 74.37(19) . . ? C6 C10 C9 108.3(3) . . ? C6 C10 C15 124.5(3) . . ? C9 C10 Dy1 73.83(19) . . ? C9 C10 C15 126.8(3) . . ? C15 C10 Dy1 122.9(2) . . ? C10 C6 Dy1 74.69(19) . . ? C10 C6 C11 124.4(4) . . ? C11 C6 Dy1 125.4(2) . . ? C7 C6 Dy1 73.87(19) . . ? C7 C6 C10 107.8(3) . . ? C7 C6 C11 127.0(3) . . ? C9 C8 Dy1 74.13(19) . . ? C9 C8 C7 107.7(3) . . ? C9 C8 C13 126.9(4) . . ? C7 C8 Dy1 73.78(19) . . ? C7 C8 C13 124.0(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 73.53(19) . . ? C19 C20 C16 107.8(3) . . ? C19 C20 C25 126.4(3) . . ? C16 C20 Dy1 75.34(19) . . ? C16 C20 C25 125.5(4) . . ? C25 C20 Dy1 122.0(2) . . ? C20 C19 Dy1 75.4(2) . . ? C20 C19 C18 108.3(3) . . ? C20 C19 C24 127.2(3) . . ? C18 C19 Dy1 75.04(19) . . ? C18 C19 C24 123.9(4) . . ? C24 C19 Dy1 122.7(2) . . ? C5 C4 I3 127.1(3) . . ? C5 C4 C3 106.5(3) . . ? C3 C4 I3 126.4(3) . . ? C10 C9 Dy1 75.14(19) . . ? C10 C9 C14 125.2(4) . . ? C8 C9 Dy1 74.9(2) . . ? C8 C9 C10 108.2(3) . . ? C8 C9 C14 126.1(4) . . ? C14 C9 Dy1 122.1(2) . . ? C2 C3 I2 126.4(3) . . ? C2 C3 C4 105.0(3) . . ? C4 C3 I2 128.6(3) . . ? C21 C16 Dy1 126.7(2) . . ? C20 C16 Dy1 73.66(19) . . ? C20 C16 C21 126.3(3) . . ? C20 C16 C17 108.2(3) . . ? C17 C16 Dy1 73.93(19) . . ? C17 C16 C21 124.7(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 75.1(2) . . ? C16 C17 C22 125.6(3) . . ? C18 C17 Dy1 74.0(2) . . ? C18 C17 C16 107.6(3) . . ? C18 C17 C22 126.5(3) . . ? C22 C17 Dy1 121.7(2) . . ? C19 C18 Dy1 73.7(2) . . ? C19 C18 C23 124.8(3) . . ? C17 C18 Dy1 75.0(2) . . ? C17 C18 C19 108.2(3) . . ? C17 C18 C23 125.6(3) . . ? C23 C18 Dy1 128.0(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 75.08(19) . . ? C6 C7 C8 108.0(3) . . ? C6 C7 C12 126.1(4) . . ? C8 C7 Dy1 74.79(19) . . ? C8 C7 C12 125.7(4) . . ? C12 C7 Dy1 120.2(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 107.3 . . ? Cl2 C26 H26D 107.3 . . ? Cl2 C26 H26A 108.7 . . ? Cl2 C26 H26B 108.7 . . ? Cl1A C26 Cl2 120.2(5) . . ? Cl1A C26 H26C 107.3 . . ? Cl1A C26 H26D 107.3 . . ? Cl1A C26 H26A 95.8 . . ? Cl1A C26 H26B 114.4 . . ? Cl1A C26 Cl1B 12.9(4) . . ? H26C C26 H26D 106.9 . . ? H26C C26 H26A 13.5 . . ? H26C C26 H26B 96.0 . . ? H26D C26 H26A 118.0 . . ? H26D C26 H26B 11.3 . . ? H26A C26 H26B 107.6 . . ? Cl1B C26 Cl2 114.2(3) . . ? Cl1B C26 H26C 120.0 . . ? Cl1B C26 H26D 100.0 . . ? Cl1B C26 H26A 108.7 . . ? Cl1B C26 H26B 108.7 . . ? 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 3.2347(3) . ? Dy1 N1 2.379(3) . ? Dy1 C10 2.659(3) . ? Dy1 C6 2.654(3) . ? Dy1 C8 2.652(3) . ? Dy1 C20 2.651(3) . ? Dy1 C19 2.627(3) . ? Dy1 C9 2.642(3) . ? Dy1 C16 2.673(3) . ? Dy1 C17 2.658(3) . ? Dy1 C18 2.644(3) . ? Dy1 C7 2.639(3) . ? I1 C2 2.091(3) . ? I4 C5 2.074(3) . ? I3 C4 2.071(3) . ? I2 C3 2.064(3) . ? Cl2 C26 1.735(5) . ? Cl1A C26 1.623(9) . ? N1 C5 1.369(4) . ? N1 C2 1.362(4) . ? C5 C4 1.380(5) . ? C2 C3 1.381(5) . ? C10 C6 1.417(5) . ? C10 C9 1.418(5) . ? C10 C15 1.502(5) . ? C6 C11 1.499(5) . ? C6 C7 1.417(5) . ? C8 C9 1.412(5) . ? C8 C7 1.433(5) . ? C8 C13 1.494(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C16 1.508(5) . ? C20 C19 1.413(5) . ? C20 C16 1.423(5) . ? C20 C25 1.507(5) . ? C19 C18 1.421(5) . ? C19 C24 1.517(5) . ? C4 C3 1.413(5) . ? C9 C14 1.499(5) . ? 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 1.501(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 1.416(5) . ? C17 C22 1.498(5) . ? C18 C23 1.505(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 1.733(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 10.3(5) . . . . ? Dy1 N1 C5 C4 -168.8(3) . . . . ? Dy1 N1 C2 I1 -4.8(3) . . . . ? Dy1 N1 C2 C3 172.8(2) . . . . ? Dy1 C10 C6 C11 122.7(3) . . . . ? Dy1 C10 C6 C7 -67.0(2) . . . . ? Dy1 C10 C9 C8 68.2(2) . . . . ? Dy1 C10 C9 C14 -119.1(4) . . . . ? Dy1 C6 C7 C8 -68.2(2) . . . . ? Dy1 C6 C7 C12 116.7(4) . . . . ? Dy1 C8 C9 C10 -68.4(2) . . . . ? Dy1 C8 C9 C14 119.1(4) . . . . ? Dy1 C8 C7 C6 68.4(2) . . . . ? Dy1 C8 C7 C12 -116.5(4) . . . . ? Dy1 C20 C19 C18 -68.5(2) . . . . ? Dy1 C20 C19 C24 120.3(4) . . . . ? Dy1 C20 C16 C21 -123.8(4) . . . . ? Dy1 C20 C16 C17 66.4(2) . . . . ? Dy1 C19 C18 C17 -67.7(2) . . . . ? Dy1 C19 C18 C23 125.3(3) . . . . ? Dy1 C16 C17 C18 67.4(2) . . . . ? Dy1 C16 C17 C22 -118.6(3) . . . . ? Dy1 C17 C18 C19 66.8(2) . . . . ? Dy1 C17 C18 C23 -126.3(3) . . . . ? I1 C2 C3 I2 -5.0(5) . . . . ? I1 C2 C3 C4 177.5(2) . . . . ? I4 C5 C4 I3 1.1(5) . . . . ? I4 C5 C4 C3 -178.8(2) . . . . ? I3 C4 C3 I2 2.5(5) . . . . ? I3 C4 C3 C2 179.9(2) . . . . ? N1 C5 C4 I3 -180.0(2) . . . . ? N1 C5 C4 C3 0.2(4) . . . . ? N1 C2 C3 I2 177.8(2) . . . . ? N1 C2 C3 C4 0.3(4) . . . . ? C5 N1 C2 I1 -177.7(2) . . . . ? C5 N1 C2 C3 -0.2(4) . . . . ? C5 C4 C3 I2 -177.7(3) . . . . ? C5 C4 C3 C2 -0.3(4) . . . . ? C2 N1 C5 I4 179.1(2) . . . . ? C2 N1 C5 C4 0.0(4) . . . . ? C10 C6 C7 Dy1 67.6(2) . . . . ? C10 C6 C7 C8 -0.6(4) . . . . ? C10 C6 C7 C12 -175.7(3) . . . . ? C6 C10 C9 Dy1 -67.0(2) . . . . ? C6 C10 C9 C8 1.3(4) . . . . ? C6 C10 C9 C14 173.9(3) . . . . ? C21 C16 C17 Dy1 123.8(3) . . . . ? C21 C16 C17 C18 -168.8(3) . . . . ? C21 C16 C17 C22 5.2(6) . . . . ? C20 C19 C18 Dy1 68.7(2) . . . . ? C20 C19 C18 C17 1.0(4) . . . . ? C20 C19 C18 C23 -166.0(3) . . . . ? C20 C16 C17 Dy1 -66.3(2) . . . . ? C20 C16 C17 C18 1.1(4) . . . . ? C20 C16 C17 C22 175.2(3) . . . . ? C19 C20 C16 Dy1 -66.9(2) . . . . ? C19 C20 C16 C21 169.2(3) . . . . ? C19 C20 C16 C17 -0.5(4) . . . . ? C9 C10 C6 Dy1 66.6(2) . . . . ? C9 C10 C6 C11 -170.7(3) . . . . ? C9 C10 C6 C7 -0.4(4) . . . . ? C9 C8 C7 Dy1 -67.0(2) . . . . ? C9 C8 C7 C6 1.4(4) . . . . ? C9 C8 C7 C12 176.6(3) . . . . ? C16 C20 C19 Dy1 68.2(2) . . . . ? C16 C20 C19 C18 -0.3(4) . . . . ? C16 C20 C19 C24 -171.6(3) . . . . ? C16 C17 C18 Dy1 -68.1(2) . . . . ? C16 C17 C18 C19 -1.3(4) . . . . ? C16 C17 C18 C23 165.5(3) . . . . ? C25 C20 C19 Dy1 -118.0(4) . . . . ? C25 C20 C19 C18 173.5(3) . . . . ? C25 C20 C19 C24 2.3(6) . . . . ? C25 C20 C16 Dy1 119.1(4) . . . . ? C25 C20 C16 C21 -4.7(6) . . . . ? C25 C20 C16 C17 -174.4(3) . . . . ? C15 C10 C6 Dy1 -119.5(3) . . . . ? C15 C10 C6 C11 3.3(5) . . . . ? C15 C10 C6 C7 173.5(3) . . . . ? C15 C10 C9 Dy1 119.3(3) . . . . ? C15 C10 C9 C8 -172.4(3) . . . . ? C15 C10 C9 C14 0.2(6) . . . . ? C11 C6 C7 Dy1 -122.5(4) . . . . ? C11 C6 C7 C8 169.3(3) . . . . ? C11 C6 C7 C12 -5.8(6) . . . . ? C22 C17 C18 Dy1 117.9(4) . . . . ? C22 C17 C18 C19 -175.3(3) . . . . ? C22 C17 C18 C23 -8.4(6) . . . . ? C7 C8 C9 Dy1 66.7(2) . . . . ? C7 C8 C9 C10 -1.7(4) . . . . ? C7 C8 C9 C14 -174.2(3) . . . . ? C13 C8 C9 Dy1 -126.3(4) . . . . ? C13 C8 C9 C10 165.3(3) . . . . ? C13 C8 C9 C14 -7.3(6) . . . . ? C13 C8 C7 Dy1 125.6(4) . . . . ? C13 C8 C7 C6 -166.0(3) . . . . ? C13 C8 C7 C12 9.2(6) . . . . ? C24 C19 C18 Dy1 -119.7(3) . . . . ? C24 C19 C18 C17 172.6(3) . . . . ? C24 C19 C18 C23 5.6(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 1.0029 -1.0020 -0.0230 -0.0783 -0.0142 0.0325 1.0023 1.0031 -0.0130 0.0038 0.0040 0.0859 -1.0029 1.0020 0.0230 0.0783 0.0142 -0.0325 -1.0023 -1.0031 0.0130 -0.0038 -0.0040 -0.0859 0.0033 -0.0027 0.9985 -0.0100 0.0322 0.0044 -0.0033 0.0027 -0.9985 0.0100 -0.0322 -0.0044 0.9958 1.0085 -2.0101 0.0239 -0.0605 0.0770 -0.9958 -1.0085 2.0101 -0.0239 0.0605 -0.0770 -1.0056 -1.0005 -0.9855 0.0063 -0.0363 -0.0903 -0.0068 1.0079 -1.9920 0.0612 -0.0554 0.0178 -2.0082 -1.0011 -0.9674 0.0435 -0.0312 -0.1495 0.0063 0.9972 2.0020 0.0210 0.0736 0.0356 1.0091 -0.0048 1.9790 -0.0574 0.0594 0.0681 0.9961 0.0060 -2.0151 -0.0172 -0.0696 0.0503 5.8407 7.2280 22.3288 -0.1415 0.7602 0.6341