#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:50:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294477 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572176.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_1572176 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 102.191(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.4052(3) _cell_length_b 14.4040(4) _cell_length_c 21.4880(7) _cell_measurement_reflns_used 16616 _cell_measurement_temperature 270.0(1) _cell_measurement_theta_max 31.0280 _cell_measurement_theta_min 2.8480 _cell_volume 3147.92(17) _computing_cell_refinement 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 270.0(1) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.839 _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 -0.0321373000 _diffrn_orient_matrix_UB_12 0.0435141000 _diffrn_orient_matrix_UB_13 -0.0060187000 _diffrn_orient_matrix_UB_21 0.0044284000 _diffrn_orient_matrix_UB_22 0.0062089000 _diffrn_orient_matrix_UB_23 0.0331255000 _diffrn_orient_matrix_UB_31 0.0617374000 _diffrn_orient_matrix_UB_32 0.0222127000 _diffrn_orient_matrix_UB_33 0.0025247000 _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 0.0597 _diffrn_reflns_av_unetI/netI 0.0501 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.839 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 39345 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.839 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.769 _diffrn_reflns_theta_min 2.451 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.481 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.258 _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 2.295 _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 0.960 _refine_diff_density_min -1.185 _refine_diff_density_rms 0.152 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8997 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0372 _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^)+(0.0333P)^2^+1.5218P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.0871 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6636 _reflns_number_total 8997 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP270K _cod_depositor_comments 'Adding full bibliography for 1572175--1572199.cif.' _cod_original_cell_volume 3147.91(16) _cod_database_code 1572176 _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 0.533 _shelx_estimated_absorpt_t_min 0.208 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Cl1B \\sim Cl1A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 3. Others Fixed Sof: Cl1A(0.5) H26C(0.5) H26D(0.5) H26A(0.5) H26B(0.5) Cl1B(0.5) 4.a Secondary CH2 refined with riding coordinates: C26(H26C,H26D), C26(H26A,H26B) 4.b Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C15(H15A,H15B,H15C), C12(H12A,H12B, H12C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A, H23B,H23C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C) ; _shelx_res_file ; TITL fed728_100_final_a.res in P2(1)/c fed728_270_final.res created by SHELXL-2018/3 at 17:05:44 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 10.40518 14.404028 21.487995 90 102.1914 90 ZERR 4 0.000295 0.000413 0.000676 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Dy I N UNIT 100 128 8 4 16 4 SIMU Cl1B Cl1A L.S. 75 0 0 PLAN 16 SIZE 0.111 0.275 0.353 TEMP -3.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.033300 1.521800 FVAR 0.59266 DY1 4 0.803900 0.716249 0.338740 11.00000 0.02891 0.03035 = 0.03006 -0.00014 0.00176 0.00384 I1 5 0.523681 0.617834 0.279292 11.00000 0.04638 0.03997 = 0.04817 0.00288 0.00779 -0.01288 I4 5 0.822417 0.939466 0.200624 11.00000 0.04615 0.04975 = 0.06039 0.00807 0.00988 -0.01367 I3 5 0.487189 0.938612 0.082375 11.00000 0.06065 0.05550 = 0.04103 0.01294 0.00708 0.01898 I2 5 0.294085 0.724658 0.129058 11.00000 0.03810 0.06617 = 0.08790 -0.00126 -0.01704 -0.00720 CL2 3 0.608501 0.626760 0.078613 11.00000 0.10855 0.09781 = 0.07153 0.00819 0.01860 0.03462 PART 1 CL1A 3 0.692837 0.446703 0.040424 10.50000 0.09443 0.08304 = 0.27749 -0.03145 0.04311 -0.00588 PART 0 N1 6 0.678319 0.774786 0.240660 11.00000 0.02821 0.04112 = 0.03193 0.00301 0.00303 -0.00151 C5 1 0.669429 0.845888 0.198298 11.00000 0.03704 0.03419 = 0.03070 0.00502 0.00665 -0.00050 C2 1 0.560661 0.729778 0.223968 11.00000 0.03155 0.03354 = 0.03732 0.00279 0.00310 -0.00342 C10 1 0.957071 0.648238 0.265275 11.00000 0.04843 0.04178 = 0.04209 0.00524 0.01530 0.01560 C6 1 0.889094 0.571787 0.281607 11.00000 0.03915 0.03582 = 0.05255 -0.01050 0.00636 0.00798 C8 1 1.026703 0.622110 0.372177 11.00000 0.03562 0.05218 = 0.05169 -0.00909 0.00389 0.01441 C21 1 0.522134 0.735989 0.423789 11.00000 0.04650 0.08259 = 0.07403 -0.02771 0.01713 -0.00969 AFIX 137 H21A 2 0.459780 0.750226 0.385259 11.00000 -1.50000 H21B 2 0.495109 0.764869 0.459204 11.00000 -1.50000 H21C 2 0.526408 0.669954 0.429923 11.00000 -1.50000 AFIX 0 C20 1 0.679583 0.852200 0.384852 11.00000 0.05668 0.04360 = 0.03195 -0.00226 0.00399 0.01801 C19 1 0.815383 0.872550 0.402644 11.00000 0.06496 0.03469 = 0.04831 -0.00892 0.02367 -0.00287 C4 1 0.549543 0.845333 0.155684 11.00000 0.03875 0.03829 = 0.03610 -0.00105 0.00510 0.00420 C9 1 1.042239 0.679762 0.321176 11.00000 0.02941 0.04340 = 0.07099 -0.00311 0.01053 0.00187 C3 1 0.478546 0.770488 0.172850 11.00000 0.03018 0.04200 = 0.03607 -0.00659 0.00037 -0.00035 C16 1 0.655489 0.771901 0.419060 11.00000 0.03582 0.04325 = 0.03966 -0.00506 0.00780 0.00199 C25 1 0.578041 0.911177 0.342839 11.00000 0.08675 0.07503 = 0.05234 -0.00066 0.00111 0.05009 AFIX 137 H25A 2 0.615841 0.939613 0.310475 11.00000 -1.50000 H25B 2 0.548386 0.958529 0.367939 11.00000 -1.50000 H25C 2 0.504910 0.873135 0.323214 11.00000 -1.50000 AFIX 0 C15 1 0.953792 0.682005 0.198842 11.00000 0.08981 0.08949 = 0.05163 0.01692 0.03274 0.03362 AFIX 137 H15A 2 0.864178 0.690843 0.176958 11.00000 -1.50000 H15B 2 0.994836 0.636915 0.176487 11.00000 -1.50000 H15C 2 1.000265 0.739844 0.200610 11.00000 -1.50000 AFIX 0 C12 1 0.886046 0.475933 0.383727 11.00000 0.09643 0.05553 = 0.11277 0.03330 0.05352 0.02563 AFIX 137 H12A 2 0.918122 0.485158 0.428567 11.00000 -1.50000 H12B 2 0.920994 0.419046 0.370923 11.00000 -1.50000 H12C 2 0.791776 0.472695 0.374700 11.00000 -1.50000 AFIX 0 C11 1 0.800253 0.509108 0.233897 11.00000 0.06050 0.06843 = 0.09110 -0.03385 0.00235 0.00712 AFIX 137 H11A 2 0.754642 0.466858 0.256210 11.00000 -1.50000 H11B 2 0.852556 0.474612 0.210117 11.00000 -1.50000 H11C 2 0.737574 0.546353 0.205295 11.00000 -1.50000 AFIX 0 C14 1 1.144030 0.755321 0.324750 11.00000 0.05600 0.06775 = 0.14898 -0.01872 0.03671 -0.01878 AFIX 137 H14A 2 1.108820 0.804766 0.296256 11.00000 -1.50000 H14B 2 1.220952 0.730474 0.312792 11.00000 -1.50000 H14C 2 1.167063 0.778785 0.367475 11.00000 -1.50000 AFIX 0 C17 1 0.775825 0.742979 0.457473 11.00000 0.04858 0.03964 = 0.03782 -0.00161 0.01331 0.00499 C18 1 0.873407 0.805223 0.448049 11.00000 0.03703 0.04605 = 0.03944 -0.00943 0.00421 0.00203 C22 1 0.790966 0.666398 0.506059 11.00000 0.09477 0.06617 = 0.04682 0.01898 0.01860 0.01706 AFIX 137 H22A 2 0.727924 0.618404 0.491208 11.00000 -1.50000 H22B 2 0.776482 0.690748 0.545596 11.00000 -1.50000 H22C 2 0.878155 0.641160 0.512384 11.00000 -1.50000 AFIX 0 C7 1 0.928950 0.556083 0.347495 11.00000 0.04480 0.03291 = 0.06047 0.01203 0.01835 0.01582 C23 1 1.008397 0.812547 0.489971 11.00000 0.04775 0.09113 = 0.06883 -0.03348 -0.00218 -0.00077 AFIX 137 H23A 2 1.032018 0.754209 0.510872 11.00000 -1.50000 H23B 2 1.008555 0.860056 0.521320 11.00000 -1.50000 H23C 2 1.070800 0.828052 0.464484 11.00000 -1.50000 AFIX 0 C13 1 1.117168 0.615254 0.436780 11.00000 0.08855 0.11961 = 0.05885 -0.01341 -0.01720 0.05813 AFIX 137 H13A 2 1.163549 0.672803 0.446612 11.00000 -1.50000 H13B 2 1.179113 0.565926 0.436557 11.00000 -1.50000 H13C 2 1.066473 0.602666 0.468325 11.00000 -1.50000 AFIX 0 C24 1 0.883090 0.958314 0.384904 11.00000 0.13651 0.04804 = 0.07847 -0.01570 0.05014 -0.03541 AFIX 137 H24A 2 0.958281 0.940399 0.368402 11.00000 -1.50000 H24B 2 0.910924 0.996413 0.421958 11.00000 -1.50000 H24C 2 0.823099 0.992643 0.353075 11.00000 -1.50000 AFIX 0 C26 1 0.693198 0.559992 0.036013 11.00000 0.21152 0.08085 = 0.12069 0.02908 0.11294 0.01465 PART 1 AFIX 23 H26C 2 0.661733 0.576032 -0.008440 10.50000 -1.20000 H26D 2 0.784329 0.579619 0.047376 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.649261 0.563132 -0.008491 10.50000 -1.20000 H26B 2 0.780194 0.586475 0.039702 10.50000 -1.20000 AFIX 0 CL1B 3 0.709828 0.448590 0.057270 10.50000 0.14932 0.09683 = 0.07899 0.02339 0.03181 0.05693 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0871, GooF = S = 1.036, Restrained GooF = 1.036 for all data REM R1 = 0.0372 for 6636 Fo > 4sig(Fo) and 0.0568 for all 8997 data REM 317 parameters refined using 6 restraints END WGHT 0.0332 1.4988 REM Highest difference peak 0.960, deepest hole -1.185, 1-sigma level 0.152 Q1 1 0.2909 0.7484 0.1651 11.00000 0.05 0.96 Q2 1 0.4602 0.8883 0.0637 11.00000 0.05 0.72 Q3 1 0.7699 0.4922 0.0430 11.00000 0.05 0.70 Q4 1 0.7882 0.7186 0.2734 11.00000 0.05 0.65 Q5 1 0.5618 0.9548 0.0875 11.00000 0.05 0.59 Q6 1 0.8239 0.9587 0.2414 11.00000 0.05 0.56 Q7 1 1.0010 0.9399 0.4389 11.00000 0.05 0.55 Q8 1 0.5267 0.8648 0.1609 11.00000 0.05 0.55 Q9 1 1.1096 0.9497 0.4027 11.00000 0.05 0.55 Q10 1 0.8972 0.6167 0.1031 11.00000 0.05 0.55 Q11 1 1.0600 0.4214 0.4184 11.00000 0.05 0.54 Q12 1 0.7982 0.5108 0.0589 11.00000 0.05 0.52 Q13 1 0.7332 0.5516 0.0590 11.00000 0.05 0.52 Q14 1 0.8344 0.6011 0.2784 11.00000 0.05 0.51 Q15 1 0.5492 0.6751 0.5180 11.00000 0.05 0.51 Q16 1 0.6632 0.8252 0.1377 11.00000 0.05 0.51 ; _shelx_res_checksum 83681 _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 2.339 _oxdiff_exptl_absorpt_empirical_full_min 0.560 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 0.80390(2) 0.71625(2) 0.33874(2) 0.03043(6) Uani 1 1 d . . . . . I1 I 0.52368(3) 0.61783(2) 0.27929(2) 0.04517(9) Uani 1 1 d . . . . . I4 I 0.82242(3) 0.93947(2) 0.20062(2) 0.05230(10) Uani 1 1 d . . . . . I3 I 0.48719(4) 0.93861(2) 0.08237(2) 0.05293(10) Uani 1 1 d . . . . . I2 I 0.29409(4) 0.72466(3) 0.12906(2) 0.06853(13) Uani 1 1 d . . . . . Cl2 Cl 0.6085(2) 0.62676(15) 0.07861(10) 0.0927(6) Uani 1 1 d . . . . . Cl1A Cl 0.6928(12) 0.4467(8) 0.0404(7) 0.151(5) Uani 0.5 1 d . U P A 1 N1 N 0.6783(3) 0.7748(2) 0.24066(17) 0.0342(8) Uani 1 1 d . . . . . C5 C 0.6694(4) 0.8459(3) 0.1983(2) 0.0341(9) Uani 1 1 d . . . . . C2 C 0.5607(4) 0.7298(3) 0.2240(2) 0.0348(9) Uani 1 1 d . . . . . C10 C 0.9571(5) 0.6482(3) 0.2653(2) 0.0433(11) Uani 1 1 d . . . . . C6 C 0.8891(5) 0.5718(3) 0.2816(3) 0.0430(11) Uani 1 1 d . . . . . C8 C 1.0267(5) 0.6221(4) 0.3722(3) 0.0473(12) Uani 1 1 d . . . . . C21 C 0.5221(6) 0.7360(5) 0.4238(3) 0.0671(17) Uani 1 1 d . . . . . H21A H 0.459780 0.750226 0.385259 0.101 Uiso 1 1 calc R U . . . H21B H 0.495109 0.764869 0.459204 0.101 Uiso 1 1 calc R U . . . H21C H 0.526408 0.669954 0.429923 0.101 Uiso 1 1 calc R U . . . C20 C 0.6796(5) 0.8522(3) 0.3849(2) 0.0449(11) Uani 1 1 d . . . . . C19 C 0.8154(5) 0.8725(3) 0.4026(3) 0.0476(12) Uani 1 1 d . . . . . C4 C 0.5495(4) 0.8453(3) 0.1557(2) 0.0381(10) Uani 1 1 d . . . . . C9 C 1.0422(4) 0.6798(3) 0.3212(3) 0.0479(12) Uani 1 1 d . . . . . C3 C 0.4785(4) 0.7705(3) 0.1729(2) 0.0371(9) Uani 1 1 d . . . . . C16 C 0.6555(4) 0.7719(3) 0.4191(2) 0.0396(10) Uani 1 1 d . . . . . C25 C 0.5780(7) 0.9112(5) 0.3428(3) 0.0734(19) Uani 1 1 d . . . . . H25A H 0.615841 0.939613 0.310475 0.110 Uiso 1 1 calc R U . . . H25B H 0.548386 0.958529 0.367939 0.110 Uiso 1 1 calc R U . . . H25C H 0.504910 0.873135 0.323214 0.110 Uiso 1 1 calc R U . . . C15 C 0.9538(7) 0.6820(5) 0.1988(3) 0.0744(19) Uani 1 1 d . . . . . H15A H 0.864178 0.690843 0.176958 0.112 Uiso 1 1 calc R U . . . H15B H 0.994836 0.636915 0.176487 0.112 Uiso 1 1 calc R U . . . H15C H 1.000265 0.739844 0.200610 0.112 Uiso 1 1 calc R U . . . C12 C 0.8860(8) 0.4759(4) 0.3837(4) 0.084(2) Uani 1 1 d . . . . . H12A H 0.918122 0.485158 0.428567 0.125 Uiso 1 1 calc R U . . . H12B H 0.920994 0.419046 0.370923 0.125 Uiso 1 1 calc R U . . . H12C H 0.791776 0.472695 0.374700 0.125 Uiso 1 1 calc R U . . . C11 C 0.8003(6) 0.5091(5) 0.2339(4) 0.0754(19) Uani 1 1 d . . . . . H11A H 0.754642 0.466858 0.256210 0.113 Uiso 1 1 calc R U . . . H11B H 0.852556 0.474612 0.210117 0.113 Uiso 1 1 calc R U . . . H11C H 0.737574 0.546353 0.205295 0.113 Uiso 1 1 calc R U . . . C14 C 1.1440(7) 0.7553(5) 0.3247(5) 0.089(2) Uani 1 1 d . . . . . H14A H 1.108820 0.804766 0.296256 0.133 Uiso 1 1 calc R U . . . H14B H 1.220952 0.730474 0.312792 0.133 Uiso 1 1 calc R U . . . H14C H 1.167063 0.778785 0.367475 0.133 Uiso 1 1 calc R U . . . C17 C 0.7758(5) 0.7430(3) 0.4575(2) 0.0414(10) Uani 1 1 d . . . . . C18 C 0.8734(5) 0.8052(3) 0.4480(2) 0.0414(10) Uani 1 1 d . . . . . C22 C 0.7910(7) 0.6664(4) 0.5061(3) 0.0687(17) Uani 1 1 d . . . . . H22A H 0.727924 0.618404 0.491208 0.103 Uiso 1 1 calc R U . . . H22B H 0.776482 0.690748 0.545596 0.103 Uiso 1 1 calc R U . . . H22C H 0.878155 0.641160 0.512384 0.103 Uiso 1 1 calc R U . . . C7 C 0.9289(5) 0.5561(3) 0.3475(3) 0.0450(12) Uani 1 1 d . . . . . C23 C 1.0084(6) 0.8125(5) 0.4900(3) 0.0714(18) Uani 1 1 d . . . . . H23A H 1.032018 0.754209 0.510872 0.107 Uiso 1 1 calc R U . . . H23B H 1.008555 0.860056 0.521320 0.107 Uiso 1 1 calc R U . . . H23C H 1.070800 0.828052 0.464484 0.107 Uiso 1 1 calc R U . . . C13 C 1.1172(7) 0.6153(6) 0.4368(3) 0.094(3) Uani 1 1 d . . . . . H13A H 1.163549 0.672803 0.446612 0.141 Uiso 1 1 calc R U . . . H13B H 1.179113 0.565926 0.436557 0.141 Uiso 1 1 calc R U . . . H13C H 1.066473 0.602666 0.468325 0.141 Uiso 1 1 calc R U . . . C24 C 0.8831(8) 0.9583(4) 0.3849(4) 0.084(2) Uani 1 1 d . . . . . H24A H 0.958281 0.940399 0.368402 0.125 Uiso 1 1 calc R U . . . H24B H 0.910924 0.996413 0.421958 0.125 Uiso 1 1 calc R U . . . H24C H 0.823099 0.992643 0.353075 0.125 Uiso 1 1 calc R U . . . C26 C 0.6932(12) 0.5600(6) 0.0360(5) 0.126(4) Uani 1 1 d . . . . . H26C H 0.661733 0.576032 -0.008440 0.151 Uiso 0.5 1 calc R U P A 1 H26D H 0.784329 0.579619 0.047376 0.151 Uiso 0.5 1 calc R U P A 1 H26A H 0.649261 0.563132 -0.008491 0.151 Uiso 0.5 1 calc R U P A -1 H26B H 0.780194 0.586475 0.039702 0.151 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7098(12) 0.4486(8) 0.0573(4) 0.107(3) Uani 0.5 1 d . U P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02891(10) 0.03035(11) 0.03006(11) -0.00014(7) 0.00176(8) 0.00384(7) I1 0.04638(18) 0.03997(17) 0.04817(19) 0.00288(13) 0.00779(14) -0.01288(12) I4 0.04615(19) 0.04975(19) 0.0604(2) 0.00807(15) 0.00988(16) -0.01367(13) I3 0.0606(2) 0.0555(2) 0.04103(19) 0.01294(15) 0.00708(15) 0.01898(15) I2 0.03810(19) 0.0662(2) 0.0879(3) -0.0013(2) -0.01704(18) -0.00720(15) Cl2 0.1085(15) 0.0978(14) 0.0715(12) 0.0082(10) 0.0186(11) 0.0346(11) Cl1A 0.094(5) 0.083(5) 0.277(14) -0.031(7) 0.043(7) -0.006(4) N1 0.0282(17) 0.041(2) 0.0319(19) 0.0030(15) 0.0030(14) -0.0015(14) C5 0.037(2) 0.034(2) 0.031(2) 0.0050(17) 0.0067(17) -0.0005(17) C2 0.032(2) 0.034(2) 0.037(2) 0.0028(17) 0.0031(18) -0.0034(16) C10 0.048(3) 0.042(3) 0.042(3) 0.005(2) 0.015(2) 0.016(2) C6 0.039(2) 0.036(2) 0.053(3) -0.010(2) 0.006(2) 0.0080(18) C8 0.036(2) 0.052(3) 0.052(3) -0.009(2) 0.004(2) 0.014(2) C21 0.047(3) 0.083(4) 0.074(4) -0.028(3) 0.017(3) -0.010(3) C20 0.057(3) 0.044(3) 0.032(2) -0.0023(19) 0.004(2) 0.018(2) C19 0.065(3) 0.035(2) 0.048(3) -0.009(2) 0.024(3) -0.003(2) C4 0.039(2) 0.038(2) 0.036(2) -0.0010(19) 0.0051(19) 0.0042(18) C9 0.029(2) 0.043(3) 0.071(4) -0.003(2) 0.011(2) 0.0019(19) C3 0.030(2) 0.042(2) 0.036(2) -0.0066(19) 0.0004(18) -0.0003(17) C16 0.036(2) 0.043(2) 0.040(3) -0.005(2) 0.0078(19) 0.0020(18) C25 0.087(5) 0.075(4) 0.052(4) -0.001(3) 0.001(3) 0.050(4) C15 0.090(5) 0.089(5) 0.052(4) 0.017(3) 0.033(3) 0.034(4) C12 0.096(5) 0.056(4) 0.113(6) 0.033(4) 0.054(5) 0.026(3) C11 0.060(4) 0.068(4) 0.091(5) -0.034(4) 0.002(3) 0.007(3) C14 0.056(4) 0.068(4) 0.149(8) -0.019(5) 0.037(5) -0.019(3) C17 0.049(3) 0.040(2) 0.038(3) -0.002(2) 0.013(2) 0.005(2) C18 0.037(2) 0.046(3) 0.039(3) -0.009(2) 0.0042(19) 0.0020(19) C22 0.095(5) 0.066(4) 0.047(3) 0.019(3) 0.019(3) 0.017(3) C7 0.045(3) 0.033(2) 0.060(3) 0.012(2) 0.018(2) 0.0158(19) C23 0.048(3) 0.091(5) 0.069(4) -0.033(4) -0.002(3) -0.001(3) C13 0.089(5) 0.120(6) 0.059(4) -0.013(4) -0.017(4) 0.058(5) C24 0.137(7) 0.048(3) 0.078(5) -0.016(3) 0.050(5) -0.035(4) C26 0.212(11) 0.081(5) 0.121(8) 0.029(5) 0.113(8) 0.015(6) Cl1B 0.149(7) 0.097(5) 0.079(3) 0.023(3) 0.032(3) 0.057(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -1 0 0.1241 1 1 0 0.1231 -1 1 0 0.1293 -1 -1 0 0.1498 0 0 1 0.0585 0 0 -1 0.0528 1 1 -2 0.0993 -1 -1 2 0.1399 -1 -1 -1 0.1333 0 1 -2 0.0924 -2 -1 -1 0.1448 0 1 2 0.0988 1 0 2 0.1081 1 0 -2 0.1036 8 5 21 0.0941 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Dy1 I1 61.89(8) . . ? N1 Dy1 C10 83.73(13) . . ? N1 Dy1 C6 92.43(14) . . ? N1 Dy1 C8 134.79(15) . . ? N1 Dy1 C20 81.36(13) . . ? N1 Dy1 C19 96.59(15) . . ? N1 Dy1 C9 107.45(15) . . ? N1 Dy1 C16 100.44(13) . . ? N1 Dy1 C17 130.25(13) . . ? N1 Dy1 C18 127.61(13) . . ? N1 Dy1 C7 122.83(15) . . ? C10 Dy1 I1 101.92(12) . . ? C10 Dy1 C6 30.38(15) . . ? C10 Dy1 C16 175.07(14) . . ? C10 Dy1 C17 145.66(15) . . ? C6 Dy1 I1 80.58(10) . . ? C6 Dy1 C16 145.82(15) . . ? C8 Dy1 I1 122.95(12) . . ? C8 Dy1 C10 51.11(16) . . ? C8 Dy1 C6 50.77(15) . . ? C8 Dy1 C20 138.10(16) . . ? C8 Dy1 C16 124.78(16) . . ? C8 Dy1 C17 94.65(16) . . ? C20 Dy1 I1 90.06(12) . . ? C20 Dy1 C10 153.61(15) . . ? C20 Dy1 C6 170.44(15) . . ? C20 Dy1 C16 30.97(15) . . ? C20 Dy1 C17 51.16(14) . . ? C19 Dy1 I1 121.14(12) . . ? C19 Dy1 C10 131.31(16) . . ? C19 Dy1 C6 158.21(16) . . ? C19 Dy1 C8 110.86(17) . . ? C19 Dy1 C20 31.08(16) . . ? C19 Dy1 C9 107.76(16) . . ? C19 Dy1 C16 51.21(15) . . ? C19 Dy1 C17 51.38(15) . . ? C19 Dy1 C18 31.22(15) . . ? C19 Dy1 C7 138.21(18) . . ? C9 Dy1 I1 130.46(11) . . ? C9 Dy1 C10 30.86(16) . . ? C9 Dy1 C6 50.48(15) . . ? C9 Dy1 C8 30.95(17) . . ? C9 Dy1 C20 138.40(16) . . ? C9 Dy1 C16 147.28(16) . . ? C9 Dy1 C17 117.61(17) . . ? C9 Dy1 C18 97.75(16) . . ? C16 Dy1 I1 77.98(10) . . ? C17 Dy1 I1 99.74(11) . . ? C17 Dy1 C6 132.16(15) . . ? C17 Dy1 C16 30.68(15) . . ? C18 Dy1 I1 128.02(10) . . ? C18 Dy1 C10 128.46(15) . . ? C18 Dy1 C6 137.30(15) . . ? C18 Dy1 C8 86.99(15) . . ? C18 Dy1 C20 51.13(15) . . ? C18 Dy1 C16 50.67(14) . . ? C18 Dy1 C17 30.68(15) . . ? C7 Dy1 I1 91.99(12) . . ? C7 Dy1 C10 50.98(15) . . ? C7 Dy1 C6 30.80(16) . . ? C7 Dy1 C8 30.97(16) . . ? C7 Dy1 C20 153.14(16) . . ? C7 Dy1 C9 51.04(15) . . ? C7 Dy1 C16 124.11(15) . . ? C7 Dy1 C17 102.18(16) . . ? C7 Dy1 C18 108.85(16) . . ? C2 I1 Dy1 68.22(12) . . ? C5 N1 Dy1 143.5(3) . . ? C5 N1 C2 104.6(4) . . ? C2 N1 Dy1 111.0(3) . . ? N1 C5 I4 121.9(3) . . ? N1 C5 C4 111.3(4) . . ? C4 C5 I4 126.8(3) . . ? N1 C2 I1 118.7(3) . . ? N1 C2 C3 112.3(4) . . ? C3 C2 I1 128.9(3) . . ? C6 C10 Dy1 75.0(3) . . ? C6 C10 C9 107.5(4) . . ? C6 C10 C15 125.8(5) . . ? C9 C10 Dy1 73.9(3) . . ? C9 C10 C15 126.2(5) . . ? C15 C10 Dy1 123.3(3) . . ? C10 C6 Dy1 74.6(3) . . ? C10 C6 C11 124.6(5) . . ? C10 C6 C7 108.9(4) . . ? C11 C6 Dy1 124.1(3) . . ? C7 C6 Dy1 73.6(3) . . ? C7 C6 C11 126.2(5) . . ? C9 C8 Dy1 74.1(3) . . ? C9 C8 C13 127.0(6) . . ? C7 C8 Dy1 73.9(3) . . ? C7 C8 C9 107.2(5) . . ? C7 C8 C13 124.2(6) . . ? C13 C8 Dy1 128.6(4) . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? C19 C20 Dy1 73.5(3) . . ? C19 C20 C16 107.7(4) . . ? C19 C20 C25 125.6(5) . . ? C16 C20 Dy1 75.3(3) . . ? C16 C20 C25 126.4(5) . . ? C25 C20 Dy1 122.0(3) . . ? C20 C19 Dy1 75.4(3) . . ? C20 C19 C18 107.5(4) . . ? C20 C19 C24 126.4(6) . . ? C18 C19 Dy1 74.9(3) . . ? C18 C19 C24 125.4(6) . . ? C24 C19 Dy1 122.8(4) . . ? C5 C4 I3 126.5(3) . . ? C5 C4 C3 106.4(4) . . ? C3 C4 I3 127.1(3) . . ? C10 C9 Dy1 75.2(3) . . ? C10 C9 C8 108.5(4) . . ? C10 C9 C14 125.7(6) . . ? C8 C9 Dy1 75.0(3) . . ? C8 C9 C14 125.4(6) . . ? C14 C9 Dy1 121.3(4) . . ? C2 C3 I2 126.2(3) . . ? C2 C3 C4 105.4(4) . . ? C4 C3 I2 128.3(3) . . ? C21 C16 Dy1 127.4(3) . . ? C20 C16 Dy1 73.8(3) . . ? C20 C16 C21 125.5(5) . . ? C17 C16 Dy1 74.1(3) . . ? C17 C16 C21 125.2(5) . . ? C17 C16 C20 108.2(4) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C17 Dy1 75.2(3) . . ? C16 C17 C22 125.0(5) . . ? C18 C17 Dy1 74.0(3) . . ? C18 C17 C16 107.9(4) . . ? C18 C17 C22 126.6(5) . . ? C22 C17 Dy1 122.9(3) . . ? C19 C18 Dy1 73.9(3) . . ? C19 C18 C23 124.9(5) . . ? C17 C18 Dy1 75.4(3) . . ? C17 C18 C19 108.7(4) . . ? C17 C18 C23 124.9(5) . . ? C23 C18 Dy1 127.8(3) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C6 C7 Dy1 75.6(2) . . ? C6 C7 C8 107.8(4) . . ? C6 C7 C12 125.8(6) . . ? C8 C7 Dy1 75.1(3) . . ? C8 C7 C12 126.1(6) . . ? C12 C7 Dy1 120.7(3) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Cl2 C26 H26C 106.9 . . ? Cl2 C26 H26D 106.9 . . ? Cl2 C26 H26A 108.4 . . ? Cl2 C26 H26B 108.4 . . ? Cl1A C26 Cl2 121.8(7) . . ? Cl1A C26 H26C 106.9 . . ? Cl1A C26 H26D 106.9 . . ? Cl1A C26 H26A 95.6 . . ? Cl1A C26 H26B 113.7 . . ? Cl1A C26 Cl1B 12.8(7) . . ? H26C C26 H26D 106.7 . . ? H26C C26 H26A 13.4 . . ? H26C C26 H26B 95.8 . . ? H26D C26 H26A 117.8 . . ? H26D C26 H26B 11.2 . . ? H26A C26 H26B 107.4 . . ? Cl1B C26 Cl2 115.7(6) . . ? Cl1B C26 H26C 119.5 . . ? Cl1B C26 H26D 99.9 . . ? Cl1B C26 H26A 108.4 . . ? Cl1B C26 H26B 108.4 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 I1 3.2511(4) . ? Dy1 N1 2.387(4) . ? Dy1 C10 2.656(4) . ? Dy1 C6 2.661(4) . ? Dy1 C8 2.651(4) . ? Dy1 C20 2.652(4) . ? Dy1 C19 2.627(5) . ? Dy1 C9 2.639(5) . ? Dy1 C16 2.671(4) . ? Dy1 C17 2.657(5) . ? Dy1 C18 2.639(5) . ? Dy1 C7 2.636(4) . ? I1 C2 2.087(4) . ? I4 C5 2.078(4) . ? I3 C4 2.068(5) . ? I2 C3 2.060(4) . ? Cl2 C26 1.697(8) . ? Cl1A C26 1.635(14) . ? N1 C5 1.360(5) . ? N1 C2 1.365(5) . ? C5 C4 1.383(6) . ? C2 C3 1.373(6) . ? C10 C6 1.393(7) . ? C10 C9 1.409(7) . ? C10 C15 1.502(7) . ? C6 C11 1.523(8) . ? C6 C7 1.407(7) . ? C8 C9 1.411(8) . ? C8 C7 1.412(7) . ? C8 C13 1.507(8) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C21 C16 1.504(7) . ? C20 C19 1.414(7) . ? C20 C16 1.421(7) . ? C20 C25 1.500(7) . ? C19 C18 1.417(7) . ? C19 C24 1.510(7) . ? C4 C3 1.400(6) . ? C9 C14 1.509(7) . ? C16 C17 1.409(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 C7 1.512(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C17 C18 1.401(7) . ? C17 C22 1.504(7) . ? C18 C23 1.504(7) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C26 H26C 0.9700 . ? C26 H26D 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 Cl1B 1.667(13) . ? 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 13.5(7) . . . . ? Dy1 N1 C5 C4 -167.0(4) . . . . ? Dy1 N1 C2 I1 -5.3(4) . . . . ? Dy1 N1 C2 C3 171.3(3) . . . . ? Dy1 C10 C6 C11 121.0(5) . . . . ? Dy1 C10 C6 C7 -66.2(3) . . . . ? Dy1 C10 C9 C8 68.2(3) . . . . ? Dy1 C10 C9 C14 -118.2(5) . . . . ? Dy1 C6 C7 C8 -68.8(3) . . . . ? Dy1 C6 C7 C12 117.7(5) . . . . ? Dy1 C8 C9 C10 -68.4(3) . . . . ? Dy1 C8 C9 C14 118.0(5) . . . . ? Dy1 C8 C7 C6 69.2(3) . . . . ? Dy1 C8 C7 C12 -117.3(5) . . . . ? Dy1 C20 C19 C18 -68.6(3) . . . . ? Dy1 C20 C19 C24 120.2(5) . . . . ? Dy1 C20 C16 C21 -124.8(5) . . . . ? Dy1 C20 C16 C17 66.7(3) . . . . ? Dy1 C19 C18 C17 -67.9(3) . . . . ? Dy1 C19 C18 C23 125.2(5) . . . . ? Dy1 C16 C17 C18 67.3(3) . . . . ? Dy1 C16 C17 C22 -120.1(5) . . . . ? Dy1 C17 C18 C19 67.0(3) . . . . ? Dy1 C17 C18 C23 -126.2(5) . . . . ? I1 C2 C3 I2 -6.0(6) . . . . ? I1 C2 C3 C4 176.9(3) . . . . ? I4 C5 C4 I3 -0.7(6) . . . . ? I4 C5 C4 C3 -179.6(3) . . . . ? I3 C4 C3 I2 3.2(6) . . . . ? I3 C4 C3 C2 -179.8(3) . . . . ? N1 C5 C4 I3 179.8(3) . . . . ? N1 C5 C4 C3 0.9(5) . . . . ? N1 C2 C3 I2 177.8(3) . . . . ? N1 C2 C3 C4 0.7(5) . . . . ? C5 N1 C2 I1 -176.8(3) . . . . ? C5 N1 C2 C3 -0.2(5) . . . . ? C5 C4 C3 I2 -178.0(3) . . . . ? C5 C4 C3 C2 -1.0(5) . . . . ? C2 N1 C5 I4 -180.0(3) . . . . ? C2 N1 C5 C4 -0.4(5) . . . . ? C10 C6 C7 Dy1 66.9(3) . . . . ? C10 C6 C7 C8 -2.0(5) . . . . ? C10 C6 C7 C12 -175.5(5) . . . . ? C6 C10 C9 Dy1 -68.1(3) . . . . ? C6 C10 C9 C8 0.2(5) . . . . ? C6 C10 C9 C14 173.7(5) . . . . ? C21 C16 C17 Dy1 125.0(5) . . . . ? C21 C16 C17 C18 -167.7(5) . . . . ? C21 C16 C17 C22 4.9(8) . . . . ? C20 C19 C18 Dy1 69.0(3) . . . . ? C20 C19 C18 C17 1.1(5) . . . . ? C20 C19 C18 C23 -165.8(5) . . . . ? C20 C16 C17 Dy1 -66.5(3) . . . . ? C20 C16 C17 C18 0.8(5) . . . . ? C20 C16 C17 C22 173.4(5) . . . . ? C19 C20 C16 Dy1 -66.9(3) . . . . ? C19 C20 C16 C21 168.3(5) . . . . ? C19 C20 C16 C17 -0.2(5) . . . . ? C9 C10 C6 Dy1 67.3(3) . . . . ? C9 C10 C6 C11 -171.6(5) . . . . ? C9 C10 C6 C7 1.1(5) . . . . ? C9 C8 C7 Dy1 -67.1(3) . . . . ? C9 C8 C7 C6 2.0(5) . . . . ? C9 C8 C7 C12 175.5(5) . . . . ? C16 C20 C19 Dy1 68.1(3) . . . . ? C16 C20 C19 C18 -0.6(5) . . . . ? C16 C20 C19 C24 -171.7(5) . . . . ? C16 C17 C18 Dy1 -68.2(3) . . . . ? C16 C17 C18 C19 -1.2(5) . . . . ? C16 C17 C18 C23 165.7(5) . . . . ? C25 C20 C19 Dy1 -117.9(5) . . . . ? C25 C20 C19 C18 173.5(5) . . . . ? C25 C20 C19 C24 2.3(8) . . . . ? C25 C20 C16 Dy1 119.2(5) . . . . ? C25 C20 C16 C21 -5.6(8) . . . . ? C25 C20 C16 C17 -174.1(5) . . . . ? C15 C10 C6 Dy1 -120.6(5) . . . . ? C15 C10 C6 C11 0.5(8) . . . . ? C15 C10 C6 C7 173.2(5) . . . . ? C15 C10 C9 Dy1 119.8(5) . . . . ? C15 C10 C9 C8 -171.9(5) . . . . ? C15 C10 C9 C14 1.6(8) . . . . ? C11 C6 C7 Dy1 -120.5(5) . . . . ? C11 C6 C7 C8 170.7(5) . . . . ? C11 C6 C7 C12 -2.9(8) . . . . ? C22 C17 C18 Dy1 119.4(5) . . . . ? C22 C17 C18 C19 -173.6(5) . . . . ? C22 C17 C18 C23 -6.7(8) . . . . ? C7 C8 C9 Dy1 67.1(3) . . . . ? C7 C8 C9 C10 -1.3(5) . . . . ? C7 C8 C9 C14 -175.0(5) . . . . ? C13 C8 C9 Dy1 -126.7(5) . . . . ? C13 C8 C9 C10 164.9(5) . . . . ? C13 C8 C9 C14 -8.7(8) . . . . ? C13 C8 C7 Dy1 126.1(5) . . . . ? C13 C8 C7 C6 -164.8(5) . . . . ? C13 C8 C7 C12 8.7(8) . . . . ? C24 C19 C18 Dy1 -119.7(5) . . . . ? C24 C19 C18 C17 172.3(5) . . . . ? C24 C19 C18 C23 5.5(8) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.9518 -1.1444 -0.3402 -0.0783 -0.0142 0.0325 1.0873 0.8643 -0.1859 0.0038 0.0040 0.0859 -0.9518 1.1444 0.3402 0.0783 0.0142 -0.0325 -1.0873 -0.8643 0.1859 -0.0038 -0.0040 -0.0859 0.0525 -0.0570 0.9772 -0.0100 0.0322 0.0044 -0.0525 0.0570 -0.9772 0.0100 -0.0322 -0.0044 0.9823 0.9782 -2.1402 0.0239 -0.0605 0.0770 -0.9823 -0.9782 2.1402 -0.0239 0.0605 -0.0770 -1.1399 -0.8073 -0.7913 0.0063 -0.0363 -0.0903 -0.0373 1.1183 -1.8771 0.0612 -0.0554 0.0178 -2.1594 -0.6672 -0.5282 0.0435 -0.0312 -0.1495 0.1728 0.8904 2.0315 0.0210 0.0736 0.0356 1.1246 -0.2540 1.6913 -0.0574 0.0594 0.0681 0.9145 -0.0261 -2.2173 -0.0172 -0.0696 0.0503 7.5375 5.2137 20.9642 -0.1415 0.7602 0.6341