#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572198.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_1572198 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 101.6271(19) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3440(2) _cell_length_b 14.3003(3) _cell_length_c 21.2652(4) _cell_measurement_reflns_used 21165 _cell_measurement_temperature 150.0(1) _cell_measurement_theta_max 31.5500 _cell_measurement_theta_min 2.8430 _cell_volume 3081.05(11) _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 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 150.0(1) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.837 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 4.00 29.00 0.50 1.50 -- 6.58 -78.00 129.00 50 2 \w -39.00 -12.00 0.50 1.50 -- -7.98 -78.00 129.00 54 3 \w -28.00 19.00 0.50 1.50 -- -7.98 78.00-104.00 94 4 \w 0.00 35.00 0.50 1.50 -- 6.58 -99.00 120.00 70 5 \w 6.00 39.00 0.50 1.50 -- 6.58 -99.00-120.00 66 6 \w -11.00 15.00 0.50 1.50 -- 6.58 -77.00 60.00 52 7 \w 2.00 38.00 0.50 1.50 -- 6.58 57.00 -90.00 72 8 \w -31.00 7.00 0.50 1.50 -- -7.98 -57.00 30.00 76 9 \w -23.00 15.00 0.50 1.50 -- -7.98 77.00 -60.00 76 10 \w -28.00 7.00 0.50 1.50 -- -7.98 -57.00 60.00 70 11 \w -15.00 15.00 0.50 1.50 -- -7.98 -77.00 -30.00 60 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0368155000 _diffrn_orient_matrix_UB_12 0.0413215000 _diffrn_orient_matrix_UB_13 -0.0093426000 _diffrn_orient_matrix_UB_21 -0.0044925000 _diffrn_orient_matrix_UB_22 0.0080696000 _diffrn_orient_matrix_UB_23 0.0324058000 _diffrn_orient_matrix_UB_31 0.0593604000 _diffrn_orient_matrix_UB_32 0.0262256000 _diffrn_orient_matrix_UB_33 0.0047502000 _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 0.0517 _diffrn_reflns_av_unetI/netI 0.0422 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.837 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 38238 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.837 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.760 _diffrn_reflns_theta_min 2.464 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.621 _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 2.344 _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 1.022 _refine_diff_density_min -1.117 _refine_diff_density_rms 0.169 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8771 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0293 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.0682 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7324 _reflns_number_total 8771 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP150K _cod_original_cell_volume 3081.07(11) _cod_database_code 1572198 _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 0.527 _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_150_final.res created by SHELXL-2018/3 at 15:48:47 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 10.344017 14.300319 21.265247 90 101.6271 90 ZERR 4 0.0002 0.000268 0.000425 0 0.0019 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. 15 0 0 PLAN 14 SIZE 0.111 0.275 0.353 TEMP -123.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.029600 FVAR 0.63902 DY1 4 0.805028 0.713871 0.339547 11.00000 0.01584 0.01607 = 0.01578 -0.00046 0.00047 0.00231 I1 5 0.525584 0.613557 0.282395 11.00000 0.02355 0.02046 = 0.02422 0.00124 0.00356 -0.00615 I4 5 0.820068 0.939686 0.200938 11.00000 0.02328 0.02450 = 0.03143 0.00385 0.00437 -0.00630 I3 5 0.482394 0.935342 0.081419 11.00000 0.03009 0.02852 = 0.02123 0.00634 0.00276 0.00922 I2 5 0.291701 0.718905 0.131107 11.00000 0.01973 0.03456 = 0.04740 0.00087 -0.00992 -0.00417 CL2 3 0.610092 0.628824 0.079708 11.00000 0.05131 0.04849 = 0.03513 0.00436 0.00832 0.01755 PART 1 CL1A 3 0.688006 0.444987 0.037502 10.50000 0.06279 0.04423 = 0.17577 -0.02686 0.00149 -0.00046 PART 0 N1 6 0.677431 0.773259 0.242153 11.00000 0.01618 0.02012 = 0.01698 -0.00090 0.00109 -0.00268 C5 1 0.667627 0.844616 0.198440 11.00000 0.01769 0.01935 = 0.01974 0.00160 0.00215 0.00054 C2 1 0.560411 0.726714 0.226040 11.00000 0.01794 0.01961 = 0.02133 0.00032 0.00493 -0.00079 C10 1 0.957738 0.647641 0.263508 11.00000 0.01994 0.02149 = 0.02241 0.00408 0.00370 0.00468 C6 1 0.887891 0.569654 0.279386 11.00000 0.01999 0.01884 = 0.02567 -0.00354 0.00289 0.00345 C8 1 1.029303 0.619118 0.370921 11.00000 0.02196 0.02965 = 0.02758 -0.00518 -0.00200 0.01396 C21 1 0.519157 0.739901 0.423909 11.00000 0.02151 0.04141 = 0.03280 -0.00759 0.00547 0.00040 AFIX 137 H21A 2 0.456217 0.759196 0.385239 11.00000 -1.50000 H21B 2 0.492941 0.766755 0.461856 11.00000 -1.50000 H21C 2 0.519851 0.671530 0.427098 11.00000 -1.50000 AFIX 0 C20 1 0.685992 0.854179 0.386085 11.00000 0.03292 0.02087 = 0.01818 0.00048 0.00369 0.00986 C19 1 0.822104 0.870828 0.404537 11.00000 0.03141 0.01979 = 0.02176 -0.00357 0.00575 0.00087 C4 1 0.547531 0.842996 0.156372 11.00000 0.02027 0.02111 = 0.02018 0.00309 0.00361 0.00343 C9 1 1.044965 0.679067 0.319929 11.00000 0.01702 0.02315 = 0.03841 -0.00627 0.00540 0.00038 C3 1 0.476263 0.766162 0.174188 11.00000 0.01687 0.02258 = 0.01931 -0.00106 -0.00020 0.00137 C16 1 0.655448 0.774139 0.420107 11.00000 0.02109 0.02096 = 0.02019 -0.00168 0.00334 0.00516 C25 1 0.586176 0.915190 0.343789 11.00000 0.04048 0.03135 = 0.03119 0.00345 0.00375 0.01791 AFIX 137 H25A 2 0.629796 0.951230 0.314832 11.00000 -1.50000 H25B 2 0.546639 0.958130 0.370493 11.00000 -1.50000 H25C 2 0.517052 0.875965 0.318483 11.00000 -1.50000 AFIX 0 C15 1 0.951316 0.682970 0.196148 11.00000 0.04149 0.03753 = 0.03291 0.00741 0.01599 0.01003 AFIX 137 H15A 2 0.858823 0.690411 0.174561 11.00000 -1.50000 H15B 2 0.994541 0.638012 0.172356 11.00000 -1.50000 H15C 2 0.996412 0.743450 0.197742 11.00000 -1.50000 AFIX 0 C12 1 0.887797 0.471841 0.382605 11.00000 0.05035 0.02955 = 0.05117 0.01728 0.02350 0.01400 AFIX 137 H12A 2 0.879216 0.493028 0.425399 11.00000 -1.50000 H12B 2 0.953944 0.421960 0.386771 11.00000 -1.50000 H12C 2 0.802585 0.448023 0.359453 11.00000 -1.50000 AFIX 0 C11 1 0.800379 0.507914 0.231195 11.00000 0.02714 0.03628 = 0.05130 -0.01939 0.00553 0.00022 AFIX 137 H11A 2 0.757743 0.461125 0.253869 11.00000 -1.50000 H11B 2 0.853778 0.476316 0.204415 11.00000 -1.50000 H11C 2 0.732759 0.546191 0.203992 11.00000 -1.50000 AFIX 0 C14 1 1.146405 0.754812 0.322562 11.00000 0.02912 0.03707 = 0.06885 -0.01340 0.01587 -0.00925 AFIX 137 H14A 2 1.111774 0.803853 0.291528 11.00000 -1.50000 H14B 2 1.226870 0.728445 0.312021 11.00000 -1.50000 H14C 2 1.166791 0.781582 0.365857 11.00000 -1.50000 AFIX 0 C17 1 0.774000 0.740406 0.459421 11.00000 0.02477 0.02315 = 0.01679 0.00051 0.00402 0.00358 C18 1 0.877342 0.801399 0.450696 11.00000 0.02110 0.02631 = 0.02062 -0.00490 0.00188 -0.00109 C22 1 0.784795 0.662537 0.507075 11.00000 0.03962 0.02998 = 0.02983 0.01172 0.00842 0.00584 AFIX 137 H22A 2 0.727631 0.610731 0.488496 11.00000 -1.50000 H22B 2 0.757364 0.684940 0.545931 11.00000 -1.50000 H22C 2 0.876469 0.640879 0.518045 11.00000 -1.50000 AFIX 0 C7 1 0.930305 0.552581 0.345997 11.00000 0.02631 0.02008 = 0.03330 0.00646 0.01096 0.01071 C23 1 1.012815 0.806436 0.492539 11.00000 0.02788 0.04139 = 0.03291 -0.01540 -0.00261 -0.00316 AFIX 137 H23A 2 1.033434 0.746867 0.515116 11.00000 -1.50000 H23B 2 1.015460 0.856931 0.523929 11.00000 -1.50000 H23C 2 1.077903 0.818796 0.465858 11.00000 -1.50000 AFIX 0 C13 1 1.120526 0.612320 0.434897 11.00000 0.04550 0.05971 = 0.03597 -0.00913 -0.01116 0.03035 AFIX 137 H13A 2 1.169405 0.671076 0.444195 11.00000 -1.50000 H13B 2 1.182773 0.560817 0.434316 11.00000 -1.50000 H13C 2 1.069222 0.600611 0.468134 11.00000 -1.50000 AFIX 0 C24 1 0.898003 0.954671 0.388342 11.00000 0.05490 0.02617 = 0.03724 -0.00562 0.01627 -0.00998 AFIX 137 H24A 2 0.981071 0.933851 0.377476 11.00000 -1.50000 H24B 2 0.916988 0.996776 0.425421 11.00000 -1.50000 H24C 2 0.845194 0.987784 0.351624 11.00000 -1.50000 AFIX 0 C26 1 0.701277 0.559152 0.038005 11.00000 0.16890 0.04445 = 0.08976 0.01671 0.10011 0.02212 PART 1 AFIX 23 H26C 2 0.680499 0.579951 -0.007319 10.50000 -1.20000 H26D 2 0.795442 0.574028 0.054615 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.665879 0.566471 -0.008578 10.50000 -1.20000 H26B 2 0.793715 0.581586 0.046800 10.50000 -1.20000 AFIX 0 CL1B 3 0.700321 0.443287 0.057043 10.50000 0.06586 0.03552 = 0.04286 0.00971 0.02066 0.01442 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0682, GooF = S = 1.050, Restrained GooF = 1.050 for all data REM R1 = 0.0293 for 7324 Fo > 4sig(Fo) and 0.0384 for all 8771 data REM 317 parameters refined using 6 restraints END WGHT 0.0296 0.0000 REM Highest difference peak 1.022, deepest hole -1.117, 1-sigma level 0.169 Q1 1 0.2904 0.7422 0.1608 11.00000 0.05 1.02 Q2 1 0.7710 0.4857 0.0593 11.00000 0.05 0.98 Q3 1 0.8943 0.7432 0.3396 11.00000 0.05 0.83 Q4 1 0.3892 0.9022 0.0788 11.00000 0.05 0.81 Q5 1 0.9380 0.7125 0.2832 11.00000 0.05 0.74 Q6 1 0.7162 0.6881 0.3425 11.00000 0.05 0.72 Q7 1 0.7235 0.5605 0.0569 11.00000 0.05 0.71 Q8 1 0.3945 0.6216 0.3383 11.00000 0.05 0.69 Q9 1 0.8991 0.9011 0.2010 11.00000 0.05 0.68 Q10 1 0.4513 0.6352 0.2791 11.00000 0.05 0.68 Q11 1 0.7036 0.6200 0.3375 11.00000 0.05 0.67 Q12 1 0.8885 0.6723 0.3396 11.00000 0.05 0.67 Q13 1 0.7029 0.7077 0.3806 11.00000 0.05 0.67 Q14 1 1.0995 0.7193 0.1936 11.00000 0.05 0.65 ; _shelx_res_checksum 80791 _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 2.580 _oxdiff_exptl_absorpt_empirical_full_min 0.675 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 0.80503(2) 0.71387(2) 0.33955(2) 0.01628(5) Uani 1 1 d . . . . . I1 I 0.52558(2) 0.61356(2) 0.28239(2) 0.02292(6) Uani 1 1 d . . . . . I4 I 0.82007(2) 0.93969(2) 0.20094(2) 0.02656(6) Uani 1 1 d . . . . . I3 I 0.48239(2) 0.93534(2) 0.08142(2) 0.02695(6) Uani 1 1 d . . . . . I2 I 0.29170(2) 0.71890(2) 0.13111(2) 0.03623(7) Uani 1 1 d . . . . . Cl2 Cl 0.61009(12) 0.62882(8) 0.07971(5) 0.0450(3) Uani 1 1 d . . . . . Cl1A Cl 0.6880(9) 0.4450(6) 0.0375(4) 0.097(3) Uani 0.5 1 d . U P A 1 N1 N 0.6774(3) 0.77326(18) 0.24215(13) 0.0181(5) Uani 1 1 d . . . . . C5 C 0.6676(3) 0.8446(2) 0.19844(16) 0.0192(6) Uani 1 1 d . . . . . C2 C 0.5604(3) 0.7267(2) 0.22604(16) 0.0195(6) Uani 1 1 d . . . . . C10 C 0.9577(3) 0.6476(2) 0.26351(16) 0.0214(7) Uani 1 1 d . . . . . C6 C 0.8879(3) 0.5697(2) 0.27939(17) 0.0217(7) Uani 1 1 d . . . . . C8 C 1.0293(3) 0.6191(2) 0.37092(18) 0.0274(8) Uani 1 1 d . . . . . C21 C 0.5192(4) 0.7399(3) 0.4239(2) 0.0319(8) Uani 1 1 d . . . . . H21A H 0.456217 0.759196 0.385239 0.048 Uiso 1 1 calc R U . . . H21B H 0.492941 0.766755 0.461856 0.048 Uiso 1 1 calc R U . . . H21C H 0.519851 0.671530 0.427098 0.048 Uiso 1 1 calc R U . . . C20 C 0.6860(4) 0.8542(2) 0.38608(17) 0.0242(7) Uani 1 1 d . . . . . C19 C 0.8221(4) 0.8708(2) 0.40454(17) 0.0243(7) Uani 1 1 d . . . . . C4 C 0.5475(3) 0.8430(2) 0.15637(16) 0.0206(6) Uani 1 1 d . . . . . C9 C 1.0450(3) 0.6791(2) 0.31993(19) 0.0262(7) Uani 1 1 d . . . . . C3 C 0.4763(3) 0.7662(2) 0.17419(16) 0.0201(6) Uani 1 1 d . . . . . C16 C 0.6554(3) 0.7741(2) 0.42011(17) 0.0209(7) Uani 1 1 d . . . . . C25 C 0.5862(4) 0.9152(3) 0.3438(2) 0.0348(9) Uani 1 1 d . . . . . H25A H 0.629796 0.951230 0.314832 0.052 Uiso 1 1 calc R U . . . H25B H 0.546639 0.958130 0.370493 0.052 Uiso 1 1 calc R U . . . H25C H 0.517052 0.875965 0.318483 0.052 Uiso 1 1 calc R U . . . C15 C 0.9513(4) 0.6830(3) 0.1961(2) 0.0361(9) Uani 1 1 d . . . . . H15A H 0.858823 0.690411 0.174561 0.054 Uiso 1 1 calc R U . . . H15B H 0.994541 0.638012 0.172356 0.054 Uiso 1 1 calc R U . . . H15C H 0.996412 0.743450 0.197742 0.054 Uiso 1 1 calc R U . . . C12 C 0.8878(5) 0.4718(3) 0.3826(2) 0.0418(11) Uani 1 1 d . . . . . H12A H 0.879216 0.493028 0.425399 0.063 Uiso 1 1 calc R U . . . H12B H 0.953944 0.421960 0.386771 0.063 Uiso 1 1 calc R U . . . H12C H 0.802585 0.448023 0.359453 0.063 Uiso 1 1 calc R U . . . C11 C 0.8004(4) 0.5079(3) 0.2312(2) 0.0386(10) Uani 1 1 d . . . . . H11A H 0.757743 0.461125 0.253869 0.058 Uiso 1 1 calc R U . . . H11B H 0.853778 0.476316 0.204415 0.058 Uiso 1 1 calc R U . . . H11C H 0.732759 0.546191 0.203992 0.058 Uiso 1 1 calc R U . . . C14 C 1.1464(4) 0.7548(3) 0.3226(3) 0.0442(11) Uani 1 1 d . . . . . H14A H 1.111774 0.803853 0.291528 0.066 Uiso 1 1 calc R U . . . H14B H 1.226870 0.728445 0.312021 0.066 Uiso 1 1 calc R U . . . H14C H 1.166791 0.781582 0.365857 0.066 Uiso 1 1 calc R U . . . C17 C 0.7740(3) 0.7404(2) 0.45942(16) 0.0216(7) Uani 1 1 d . . . . . C18 C 0.8773(3) 0.8014(2) 0.45070(17) 0.0230(7) Uani 1 1 d . . . . . C22 C 0.7848(4) 0.6625(3) 0.50708(19) 0.0329(8) Uani 1 1 d . . . . . H22A H 0.727631 0.610731 0.488496 0.049 Uiso 1 1 calc R U . . . H22B H 0.757364 0.684940 0.545931 0.049 Uiso 1 1 calc R U . . . H22C H 0.876469 0.640879 0.518045 0.049 Uiso 1 1 calc R U . . . C7 C 0.9303(4) 0.5526(2) 0.34600(19) 0.0259(8) Uani 1 1 d . . . . . C23 C 1.0128(4) 0.8064(3) 0.4925(2) 0.0353(9) Uani 1 1 d . . . . . H23A H 1.033434 0.746867 0.515116 0.053 Uiso 1 1 calc R U . . . H23B H 1.015460 0.856931 0.523929 0.053 Uiso 1 1 calc R U . . . H23C H 1.077903 0.818796 0.465858 0.053 Uiso 1 1 calc R U . . . C13 C 1.1205(5) 0.6123(3) 0.4349(2) 0.0498(12) Uani 1 1 d . . . . . H13A H 1.169405 0.671076 0.444195 0.075 Uiso 1 1 calc R U . . . H13B H 1.182773 0.560817 0.434316 0.075 Uiso 1 1 calc R U . . . H13C H 1.069222 0.600611 0.468134 0.075 Uiso 1 1 calc R U . . . C24 C 0.8980(5) 0.9547(3) 0.3883(2) 0.0385(10) Uani 1 1 d . . . . . H24A H 0.981071 0.933851 0.377476 0.058 Uiso 1 1 calc R U . . . H24B H 0.916988 0.996776 0.425421 0.058 Uiso 1 1 calc R U . . . H24C H 0.845194 0.987784 0.351624 0.058 Uiso 1 1 calc R U . . . C26 C 0.7013(9) 0.5592(3) 0.0380(4) 0.091(3) Uani 1 1 d . . . . . H26C H 0.680499 0.579951 -0.007319 0.109 Uiso 0.5 1 calc R U P A 1 H26D H 0.795442 0.574028 0.054615 0.109 Uiso 0.5 1 calc R U P A 1 H26A H 0.665879 0.566471 -0.008578 0.109 Uiso 0.5 1 calc R U P A -1 H26B H 0.793715 0.581586 0.046800 0.109 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7003(8) 0.4433(5) 0.0570(2) 0.0467(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 0.01584(8) 0.01607(8) 0.01578(8) -0.00046(5) 0.00047(6) 0.00231(5) I1 0.02355(11) 0.02046(11) 0.02422(12) 0.00124(8) 0.00356(9) -0.00615(8) I4 0.02328(12) 0.02450(12) 0.03143(13) 0.00385(9) 0.00437(9) -0.00630(8) I3 0.03009(13) 0.02852(12) 0.02123(12) 0.00634(9) 0.00276(9) 0.00922(9) I2 0.01973(12) 0.03456(14) 0.04740(17) 0.00087(11) -0.00992(10) -0.00417(9) Cl2 0.0513(7) 0.0485(6) 0.0351(6) 0.0044(5) 0.0083(5) 0.0175(5) Cl1A 0.063(3) 0.044(3) 0.176(8) -0.027(4) 0.001(5) 0.000(2) N1 0.0162(13) 0.0201(13) 0.0170(14) -0.0009(11) 0.0011(10) -0.0027(10) C5 0.0177(15) 0.0194(15) 0.0197(16) 0.0016(12) 0.0021(12) 0.0005(11) C2 0.0179(16) 0.0196(15) 0.0213(17) 0.0003(12) 0.0049(13) -0.0008(11) C10 0.0199(16) 0.0215(16) 0.0224(17) 0.0041(13) 0.0037(13) 0.0047(12) C6 0.0200(16) 0.0188(15) 0.0257(18) -0.0035(13) 0.0029(13) 0.0034(12) C8 0.0220(17) 0.0297(18) 0.0276(19) -0.0052(15) -0.0020(14) 0.0140(13) C21 0.0215(19) 0.041(2) 0.033(2) -0.0076(17) 0.0055(15) 0.0004(15) C20 0.0329(19) 0.0209(16) 0.0182(16) 0.0005(13) 0.0037(14) 0.0099(13) C19 0.0314(19) 0.0198(16) 0.0218(17) -0.0036(13) 0.0058(14) 0.0009(13) C4 0.0203(16) 0.0211(15) 0.0202(16) 0.0031(13) 0.0036(13) 0.0034(12) C9 0.0170(16) 0.0232(17) 0.038(2) -0.0063(15) 0.0054(14) 0.0004(12) C3 0.0169(16) 0.0226(15) 0.0193(16) -0.0011(13) -0.0002(12) 0.0014(12) C16 0.0211(17) 0.0210(15) 0.0202(17) -0.0017(13) 0.0033(13) 0.0052(12) C25 0.040(2) 0.0314(19) 0.031(2) 0.0034(17) 0.0037(17) 0.0179(16) C15 0.041(2) 0.038(2) 0.033(2) 0.0074(17) 0.0160(18) 0.0100(17) C12 0.050(3) 0.030(2) 0.051(3) 0.0173(19) 0.024(2) 0.0140(18) C11 0.027(2) 0.036(2) 0.051(3) -0.0194(19) 0.0055(18) 0.0002(15) C14 0.029(2) 0.037(2) 0.069(3) -0.013(2) 0.016(2) -0.0093(17) C17 0.0248(17) 0.0231(16) 0.0168(16) 0.0005(13) 0.0040(13) 0.0036(13) C18 0.0211(17) 0.0263(17) 0.0206(17) -0.0049(14) 0.0019(13) -0.0011(12) C22 0.040(2) 0.0300(19) 0.030(2) 0.0117(16) 0.0084(17) 0.0058(16) C7 0.0263(18) 0.0201(16) 0.033(2) 0.0065(14) 0.0110(15) 0.0107(13) C23 0.028(2) 0.041(2) 0.033(2) -0.0154(18) -0.0026(16) -0.0032(16) C13 0.046(3) 0.060(3) 0.036(2) -0.009(2) -0.011(2) 0.030(2) C24 0.055(3) 0.0262(19) 0.037(2) -0.0056(17) 0.016(2) -0.0100(17) C26 0.169(8) 0.044(3) 0.090(5) 0.017(3) 0.100(6) 0.022(4) Cl1B 0.066(3) 0.0355(19) 0.0429(15) 0.0097(14) 0.0207(18) 0.0144(18) 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 23 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 62.23(6) . . ? N1 Dy1 C10 83.73(9) . . ? N1 Dy1 C6 91.96(10) . . ? N1 Dy1 C8 134.86(11) . . ? N1 Dy1 C20 80.59(10) . . ? N1 Dy1 C19 96.89(10) . . ? N1 Dy1 C9 107.67(11) . . ? N1 Dy1 C16 98.73(10) . . ? N1 Dy1 C17 129.12(10) . . ? N1 Dy1 C18 128.07(10) . . ? N1 Dy1 C7 122.60(11) . . ? C10 Dy1 I1 102.08(7) . . ? C10 Dy1 C6 30.71(10) . . ? C10 Dy1 C8 51.17(11) . . ? C10 Dy1 C16 177.28(10) . . ? C10 Dy1 C17 146.81(10) . . ? C6 Dy1 I1 79.96(7) . . ? C6 Dy1 C16 147.49(10) . . ? C6 Dy1 C17 133.22(10) . . ? C8 Dy1 I1 122.52(8) . . ? C8 Dy1 C6 51.27(11) . . ? C8 Dy1 C16 126.40(11) . . ? C8 Dy1 C17 95.75(11) . . ? C20 Dy1 I1 91.65(8) . . ? C20 Dy1 C10 151.31(10) . . ? C20 Dy1 C6 170.75(11) . . ? C20 Dy1 C8 137.89(11) . . ? C20 Dy1 C16 31.03(10) . . ? C20 Dy1 C17 51.59(10) . . ? C19 Dy1 I1 122.50(8) . . ? C19 Dy1 C10 129.91(11) . . ? C19 Dy1 C6 157.43(11) . . ? C19 Dy1 C8 109.99(11) . . ? C19 Dy1 C20 30.88(11) . . ? C19 Dy1 C9 106.16(11) . . ? C19 Dy1 C16 51.13(10) . . ? C19 Dy1 C17 51.78(11) . . ? C19 Dy1 C18 31.53(11) . . ? C19 Dy1 C7 137.84(12) . . ? C9 Dy1 I1 130.74(8) . . ? C9 Dy1 C10 31.11(11) . . ? C9 Dy1 C6 51.28(10) . . ? C9 Dy1 C8 31.02(12) . . ? C9 Dy1 C20 136.31(11) . . ? C9 Dy1 C16 147.63(11) . . ? C9 Dy1 C17 118.44(11) . . ? C9 Dy1 C18 97.16(11) . . ? C16 Dy1 I1 78.17(7) . . ? C17 Dy1 I1 98.74(8) . . ? C17 Dy1 C16 30.94(10) . . ? C18 Dy1 I1 127.99(7) . . ? C18 Dy1 C10 128.14(10) . . ? C18 Dy1 C6 137.43(11) . . ? C18 Dy1 C8 86.65(11) . . ? C18 Dy1 C20 51.44(11) . . ? C18 Dy1 C16 51.00(10) . . ? C18 Dy1 C17 31.06(10) . . ? C7 Dy1 I1 91.39(8) . . ? C7 Dy1 C10 51.12(11) . . ? C7 Dy1 C6 31.05(11) . . ? C7 Dy1 C8 31.15(12) . . ? C7 Dy1 C20 154.74(11) . . ? C7 Dy1 C9 51.43(11) . . ? C7 Dy1 C16 126.23(11) . . ? C7 Dy1 C17 103.18(11) . . ? C7 Dy1 C18 108.66(12) . . ? C2 I1 Dy1 68.14(9) . . ? C5 N1 Dy1 144.0(2) . . ? C2 N1 Dy1 110.7(2) . . ? C2 N1 C5 104.6(3) . . ? N1 C5 I4 121.2(2) . . ? N1 C5 C4 111.2(3) . . ? C4 C5 I4 127.5(2) . . ? N1 C2 I1 118.8(2) . . ? N1 C2 C3 112.7(3) . . ? C3 C2 I1 128.4(2) . . ? C6 C10 Dy1 74.87(19) . . ? C6 C10 C9 108.5(3) . . ? C6 C10 C15 124.6(3) . . ? C9 C10 Dy1 74.17(19) . . ? C9 C10 C15 126.5(3) . . ? C15 C10 Dy1 122.8(2) . . ? C10 C6 Dy1 74.42(18) . . ? C10 C6 C11 124.6(3) . . ? C10 C6 C7 107.8(3) . . ? C11 C6 Dy1 125.0(2) . . ? C7 C6 Dy1 73.59(18) . . ? C7 C6 C11 126.9(3) . . ? C9 C8 Dy1 74.19(19) . . ? C9 C8 C7 107.8(3) . . ? C9 C8 C13 126.0(4) . . ? C7 C8 Dy1 73.75(19) . . ? C7 C8 C13 124.9(4) . . ? C13 C8 Dy1 128.4(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 73.58(19) . . ? C19 C20 C16 107.9(3) . . ? C19 C20 C25 126.7(3) . . ? C16 C20 Dy1 75.42(18) . . ? C16 C20 C25 125.1(3) . . ? C25 C20 Dy1 122.1(2) . . ? C20 C19 Dy1 75.54(19) . . ? C20 C19 C18 108.3(3) . . ? C20 C19 C24 127.5(3) . . ? C18 C19 Dy1 75.11(18) . . ? C18 C19 C24 123.6(4) . . ? C24 C19 Dy1 122.8(2) . . ? C5 C4 I3 126.8(2) . . ? C5 C4 C3 106.8(3) . . ? C3 C4 I3 126.4(2) . . ? C10 C9 Dy1 74.72(19) . . ? C10 C9 C14 125.4(4) . . ? C8 C9 Dy1 74.79(19) . . ? C8 C9 C10 107.7(3) . . ? C8 C9 C14 126.5(4) . . ? C14 C9 Dy1 122.0(2) . . ? C2 C3 I2 126.9(2) . . ? C2 C3 C4 104.6(3) . . ? C4 C3 I2 128.4(2) . . ? C21 C16 Dy1 126.7(2) . . ? C20 C16 Dy1 73.56(19) . . ? C20 C16 C21 126.4(3) . . ? C17 C16 Dy1 74.06(18) . . ? C17 C16 C21 124.2(3) . . ? C17 C16 C20 108.6(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 75.01(19) . . ? C16 C17 C22 126.1(3) . . ? C18 C17 Dy1 73.92(19) . . ? C18 C17 C16 107.3(3) . . ? C18 C17 C22 126.2(3) . . ? C22 C17 Dy1 122.4(2) . . ? C19 C18 Dy1 73.36(19) . . ? C19 C18 C23 124.6(3) . . ? C17 C18 Dy1 75.02(19) . . ? C17 C18 C19 108.0(3) . . ? C17 C18 C23 126.1(3) . . ? C23 C18 Dy1 127.9(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 75.36(18) . . ? C6 C7 C8 108.2(3) . . ? C6 C7 C12 125.8(4) . . ? C8 C7 Dy1 75.11(18) . . ? C8 C7 C12 125.7(4) . . ? C12 C7 Dy1 120.4(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 107.0 . . ? Cl2 C26 H26D 107.0 . . ? Cl2 C26 H26A 108.7 . . ? Cl2 C26 H26B 108.7 . . ? Cl1A C26 Cl2 121.5(5) . . ? Cl1A C26 H26C 107.0 . . ? Cl1A C26 H26D 107.0 . . ? Cl1A C26 H26A 94.9 . . ? Cl1A C26 H26B 113.6 . . ? Cl1A C26 Cl1B 13.9(4) . . ? H26C C26 H26D 106.7 . . ? H26C C26 H26A 14.1 . . ? H26C C26 H26B 95.7 . . ? H26D C26 H26A 118.2 . . ? H26D C26 H26B 11.4 . . ? H26A C26 H26B 107.6 . . ? Cl1B C26 Cl2 114.0(3) . . ? Cl1B C26 H26C 120.8 . . ? Cl1B C26 H26D 100.2 . . ? 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 3.2364(3) . ? Dy1 N1 2.377(3) . ? Dy1 C10 2.653(3) . ? Dy1 C6 2.658(3) . ? Dy1 C8 2.653(3) . ? Dy1 C20 2.648(3) . ? Dy1 C19 2.623(3) . ? Dy1 C9 2.646(3) . ? Dy1 C16 2.672(3) . ? Dy1 C17 2.660(3) . ? Dy1 C18 2.646(3) . ? Dy1 C7 2.636(3) . ? I1 C2 2.088(3) . ? I4 C5 2.075(3) . ? I3 C4 2.075(3) . ? I2 C3 2.058(3) . ? Cl2 C26 1.734(5) . ? Cl1A C26 1.638(10) . ? N1 C5 1.370(4) . ? N1 C2 1.363(4) . ? C5 C4 1.377(5) . ? C2 C3 1.380(5) . ? C10 C6 1.406(5) . ? C10 C9 1.421(5) . ? C10 C15 1.508(5) . ? C6 C11 1.508(5) . ? C6 C7 1.417(5) . ? C8 C9 1.417(5) . ? C8 C7 1.420(5) . ? C8 C13 1.494(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C16 1.510(5) . ? C20 C19 1.404(5) . ? C20 C16 1.423(5) . ? C20 C25 1.504(5) . ? C19 C18 1.432(5) . ? C19 C24 1.510(5) . ? C4 C3 1.417(5) . ? C9 C14 1.501(5) . ? C16 C17 1.422(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 1.507(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 1.495(5) . ? C18 C23 1.503(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 1.706(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 10.6(5) . . . . ? Dy1 N1 C5 C4 -168.7(3) . . . . ? Dy1 N1 C2 I1 -4.4(3) . . . . ? Dy1 N1 C2 C3 172.6(2) . . . . ? Dy1 C10 C6 C11 122.1(3) . . . . ? Dy1 C10 C6 C7 -66.6(2) . . . . ? Dy1 C10 C9 C8 68.1(2) . . . . ? Dy1 C10 C9 C14 -118.6(3) . . . . ? Dy1 C6 C7 C8 -68.6(2) . . . . ? Dy1 C6 C7 C12 117.1(3) . . . . ? Dy1 C8 C9 C10 -68.1(2) . . . . ? Dy1 C8 C9 C14 118.8(4) . . . . ? Dy1 C8 C7 C6 68.7(2) . . . . ? Dy1 C8 C7 C12 -117.0(3) . . . . ? Dy1 C20 C19 C18 -68.6(2) . . . . ? Dy1 C20 C19 C24 120.5(4) . . . . ? Dy1 C20 C16 C21 -123.8(3) . . . . ? Dy1 C20 C16 C17 66.4(2) . . . . ? Dy1 C19 C18 C17 -67.6(2) . . . . ? Dy1 C19 C18 C23 124.9(3) . . . . ? Dy1 C16 C17 C18 67.4(2) . . . . ? Dy1 C16 C17 C22 -119.5(3) . . . . ? Dy1 C17 C18 C19 66.5(2) . . . . ? Dy1 C17 C18 C23 -126.2(3) . . . . ? I1 C2 C3 I2 -5.1(5) . . . . ? I1 C2 C3 C4 177.2(2) . . . . ? I4 C5 C4 I3 0.6(5) . . . . ? I4 C5 C4 C3 -179.2(2) . . . . ? I3 C4 C3 I2 2.2(4) . . . . ? I3 C4 C3 C2 179.9(2) . . . . ? N1 C5 C4 I3 179.8(2) . . . . ? N1 C5 C4 C3 0.0(4) . . . . ? N1 C2 C3 I2 178.3(2) . . . . ? N1 C2 C3 C4 0.5(4) . . . . ? C5 N1 C2 I1 -177.5(2) . . . . ? C5 N1 C2 C3 -0.5(4) . . . . ? C5 C4 C3 I2 -178.0(2) . . . . ? C5 C4 C3 C2 -0.3(4) . . . . ? C2 N1 C5 I4 179.6(2) . . . . ? C2 N1 C5 C4 0.3(4) . . . . ? C10 C6 C7 Dy1 67.1(2) . . . . ? C10 C6 C7 C8 -1.4(4) . . . . ? C10 C6 C7 C12 -175.7(3) . . . . ? C6 C10 C9 Dy1 -67.6(2) . . . . ? C6 C10 C9 C8 0.5(4) . . . . ? C6 C10 C9 C14 173.8(3) . . . . ? C21 C16 C17 Dy1 123.8(3) . . . . ? C21 C16 C17 C18 -168.7(3) . . . . ? C21 C16 C17 C22 4.4(5) . . . . ? C20 C19 C18 Dy1 68.9(2) . . . . ? C20 C19 C18 C17 1.3(4) . . . . ? C20 C19 C18 C23 -166.2(3) . . . . ? C20 C16 C17 Dy1 -66.0(2) . . . . ? C20 C16 C17 C18 1.4(4) . . . . ? C20 C16 C17 C22 174.5(3) . . . . ? C19 C20 C16 Dy1 -67.0(2) . . . . ? C19 C20 C16 C21 169.2(3) . . . . ? C19 C20 C16 C17 -0.6(4) . . . . ? C9 C10 C6 Dy1 67.1(2) . . . . ? C9 C10 C6 C11 -170.8(3) . . . . ? C9 C10 C6 C7 0.6(4) . . . . ? C9 C8 C7 Dy1 -67.0(2) . . . . ? C9 C8 C7 C6 1.8(4) . . . . ? C9 C8 C7 C12 176.1(3) . . . . ? C16 C20 C19 Dy1 68.2(2) . . . . ? C16 C20 C19 C18 -0.4(4) . . . . ? C16 C20 C19 C24 -171.3(3) . . . . ? C16 C17 C18 Dy1 -68.2(2) . . . . ? C16 C17 C18 C19 -1.7(4) . . . . ? C16 C17 C18 C23 165.6(3) . . . . ? C25 C20 C19 Dy1 -118.1(4) . . . . ? C25 C20 C19 C18 173.3(3) . . . . ? C25 C20 C19 C24 2.4(6) . . . . ? C25 C20 C16 Dy1 119.2(3) . . . . ? C25 C20 C16 C21 -4.6(6) . . . . ? C25 C20 C16 C17 -174.5(3) . . . . ? C15 C10 C6 Dy1 -119.7(3) . . . . ? C15 C10 C6 C11 2.4(5) . . . . ? C15 C10 C6 C7 173.7(3) . . . . ? C15 C10 C9 Dy1 119.4(3) . . . . ? C15 C10 C9 C8 -172.5(3) . . . . ? C15 C10 C9 C14 0.8(6) . . . . ? C11 C6 C7 Dy1 -121.8(3) . . . . ? C11 C6 C7 C8 169.7(3) . . . . ? C11 C6 C7 C12 -4.6(5) . . . . ? C22 C17 C18 Dy1 118.8(3) . . . . ? C22 C17 C18 C19 -174.7(3) . . . . ? C22 C17 C18 C23 -7.5(6) . . . . ? C7 C8 C9 Dy1 66.7(2) . . . . ? C7 C8 C9 C10 -1.4(4) . . . . ? C7 C8 C9 C14 -174.6(3) . . . . ? C13 C8 C9 Dy1 -126.4(4) . . . . ? C13 C8 C9 C10 165.5(3) . . . . ? C13 C8 C9 C14 -7.6(6) . . . . ? C13 C8 C7 Dy1 125.9(4) . . . . ? C13 C8 C7 C6 -165.4(3) . . . . ? C13 C8 C7 C12 8.9(6) . . . . ? C24 C19 C18 Dy1 -119.8(3) . . . . ? C24 C19 C18 C17 172.6(3) . . . . ? C24 C19 C18 C23 5.1(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 0.9995 -1.0156 -0.0455 -0.0783 -0.0142 0.0325 1.0067 0.9922 0.0167 0.0038 0.0040 0.0859 -0.9995 1.0156 0.0455 0.0783 0.0142 -0.0325 -1.0067 -0.9922 -0.0167 -0.0038 -0.0040 -0.0859 0.0018 -0.0156 0.9993 -0.0100 0.0322 0.0044 -0.0018 0.0156 -0.9993 0.0100 -0.0322 -0.0044 1.0031 1.0235 -1.9819 0.0239 -0.0605 0.0770 -1.0031 -1.0235 1.9819 -0.0239 0.0605 -0.0770 -1.0085 -0.9766 -1.0159 0.0063 -0.0363 -0.0903 -0.0000 1.0352 -1.9674 0.0612 -0.0554 0.0178 -2.0116 -0.9649 -1.0015 0.0435 -0.0312 -0.1495 0.0072 0.9726 2.0296 0.0210 0.0736 0.0356 1.0067 -0.0430 1.9841 -0.0574 0.0594 0.0681 0.9995 0.0196 -2.0129 -0.0172 -0.0696 0.0503 5.8389 6.8765 22.5559 -0.1415 0.7602 0.6341