#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572190.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_1572190 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 102.143(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3990(3) _cell_length_b 14.3997(4) _cell_length_c 21.4703(6) _cell_measurement_reflns_used 16600 _cell_measurement_temperature 260.0(1) _cell_measurement_theta_max 30.3030 _cell_measurement_theta_min 2.8260 _cell_volume 3143.08(16) _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 260.0(1) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.997 _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 -0.0318871000 _diffrn_orient_matrix_UB_12 0.0435340000 _diffrn_orient_matrix_UB_13 -0.0065547000 _diffrn_orient_matrix_UB_21 0.0022031000 _diffrn_orient_matrix_UB_22 0.0063570000 _diffrn_orient_matrix_UB_23 0.0329660000 _diffrn_orient_matrix_UB_31 0.0620130000 _diffrn_orient_matrix_UB_32 0.0221635000 _diffrn_orient_matrix_UB_33 0.0034267000 _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 0.0605 _diffrn_reflns_av_unetI/netI 0.0513 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.837 _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 -31 _diffrn_reflns_number 39342 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.837 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.791 _diffrn_reflns_theta_min 2.452 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.491 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.248 _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 2.298 _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 1.166 _refine_diff_density_min -1.225 _refine_diff_density_rms 0.158 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8983 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0373 _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^)+(0.0363P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.0880 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6709 _reflns_number_total 8983 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP260K _cod_database_code 1572190 _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_260_final.res created by SHELXL-2018/3 at 17:00:17 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 10.399005 14.399669 21.470348 90 102.1432 90 ZERR 4 0.00028 0.000387 0.000637 0 0.0028 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. 50 0 0 PLAN 16 SIZE 0.111 0.275 0.353 TEMP -13.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.036300 FVAR 0.57993 DY1 4 0.803910 0.716115 0.338803 11.00000 0.02792 0.02893 = 0.02890 -0.00031 0.00170 0.00365 I1 5 0.523718 0.617594 0.279536 11.00000 0.04414 0.03805 = 0.04612 0.00248 0.00753 -0.01199 I4 5 0.822298 0.939539 0.200538 11.00000 0.04434 0.04725 = 0.05784 0.00801 0.00933 -0.01297 I3 5 0.486844 0.938496 0.082269 11.00000 0.05811 0.05310 = 0.03918 0.01267 0.00678 0.01837 I2 5 0.293821 0.724367 0.129208 11.00000 0.03678 0.06340 = 0.08399 -0.00104 -0.01636 -0.00680 CL2 3 0.608594 0.626866 0.078842 11.00000 0.10458 0.09162 = 0.06855 0.00768 0.01932 0.03373 PART 1 CL1A 3 0.695986 0.444361 0.041872 10.50000 0.08819 0.07610 = 0.27533 -0.03923 0.04889 -0.00796 PART 0 N1 6 0.677909 0.774706 0.241008 11.00000 0.02982 0.03839 = 0.02959 0.00351 0.00229 0.00056 C5 1 0.670133 0.846090 0.198181 11.00000 0.02991 0.03576 = 0.03693 0.00468 0.00928 0.00121 C2 1 0.560441 0.730209 0.224537 11.00000 0.03122 0.03526 = 0.03665 0.00156 0.00488 -0.00045 C10 1 0.957671 0.648410 0.265247 11.00000 0.04649 0.03877 = 0.03705 0.00304 0.01179 0.01765 C6 1 0.887360 0.571489 0.281776 11.00000 0.03407 0.03144 = 0.05885 -0.01315 0.00634 0.00461 C8 1 1.026892 0.621540 0.372399 11.00000 0.03577 0.05247 = 0.04918 -0.00606 0.00109 0.01749 C21 1 0.520916 0.736752 0.424043 11.00000 0.04028 0.07861 = 0.07069 -0.02214 0.01874 -0.00147 AFIX 137 H21A 2 0.457840 0.753133 0.386207 11.00000 -1.50000 H21B 2 0.495320 0.763696 0.460497 11.00000 -1.50000 H21C 2 0.524481 0.670406 0.428454 11.00000 -1.50000 AFIX 0 C20 1 0.680018 0.852776 0.385173 11.00000 0.05942 0.03352 = 0.03579 0.00008 0.00308 0.01798 C19 1 0.815773 0.872721 0.403052 11.00000 0.06045 0.03512 = 0.05131 -0.00967 0.02272 -0.00798 C4 1 0.549628 0.845446 0.155695 11.00000 0.03280 0.03805 = 0.03503 0.00269 0.00429 0.00257 C9 1 1.042476 0.680097 0.321335 11.00000 0.03156 0.03585 = 0.06734 -0.00464 0.01467 0.00259 C3 1 0.478566 0.770649 0.173383 11.00000 0.03150 0.04036 = 0.03611 -0.00169 0.00027 -0.00170 C16 1 0.654757 0.772959 0.419278 11.00000 0.03523 0.03980 = 0.03790 -0.00562 0.00912 0.00366 C25 1 0.577837 0.910885 0.342638 11.00000 0.08436 0.06167 = 0.04922 0.00290 -0.00020 0.04361 AFIX 137 H25A 2 0.617744 0.944190 0.312892 11.00000 -1.50000 H25B 2 0.540917 0.954217 0.368015 11.00000 -1.50000 H25C 2 0.509527 0.871397 0.319816 11.00000 -1.50000 AFIX 0 C15 1 0.952617 0.681414 0.198635 11.00000 0.08998 0.07378 = 0.05073 0.01687 0.03228 0.02818 AFIX 137 H15A 2 0.863550 0.678927 0.174802 11.00000 -1.50000 H15B 2 1.006989 0.642282 0.178726 11.00000 -1.50000 H15C 2 0.984073 0.744192 0.199673 11.00000 -1.50000 AFIX 0 C12 1 0.887816 0.476178 0.384347 11.00000 0.08984 0.04758 = 0.11352 0.03594 0.04954 0.01893 AFIX 137 H12A 2 0.892397 0.495037 0.427646 11.00000 -1.50000 H12B 2 0.945616 0.424411 0.383544 11.00000 -1.50000 H12C 2 0.799259 0.458360 0.365418 11.00000 -1.50000 AFIX 0 C11 1 0.800261 0.509019 0.233836 11.00000 0.05408 0.06727 = 0.09173 -0.04106 0.00160 0.00141 AFIX 137 H11A 2 0.754226 0.466502 0.255810 11.00000 -1.50000 H11B 2 0.853503 0.474797 0.210332 11.00000 -1.50000 H11C 2 0.737881 0.546187 0.204999 11.00000 -1.50000 AFIX 0 C14 1 1.141554 0.756905 0.323326 11.00000 0.05322 0.06346 = 0.13936 -0.01256 0.03511 -0.01360 AFIX 137 H14A 2 1.096621 0.813866 0.309413 11.00000 -1.50000 H14B 2 1.200065 0.741669 0.295713 11.00000 -1.50000 H14C 2 1.191132 0.764141 0.366121 11.00000 -1.50000 AFIX 0 C17 1 0.774816 0.743386 0.457459 11.00000 0.04421 0.03593 = 0.03346 0.00013 0.00885 0.00387 C18 1 0.873284 0.804871 0.448387 11.00000 0.03765 0.04835 = 0.03399 -0.00950 0.00194 0.00071 C22 1 0.789853 0.666329 0.506262 11.00000 0.08559 0.06486 = 0.05109 0.02079 0.02185 0.01850 AFIX 137 H22A 2 0.743784 0.612148 0.487323 11.00000 -1.50000 H22B 2 0.753909 0.686002 0.541785 11.00000 -1.50000 H22C 2 0.881415 0.651896 0.520674 11.00000 -1.50000 AFIX 0 C7 1 0.928765 0.555536 0.347481 11.00000 0.04312 0.03091 = 0.05501 0.00877 0.01636 0.01470 C23 1 1.008827 0.812708 0.490654 11.00000 0.04533 0.09068 = 0.06506 -0.03303 -0.00605 -0.00321 AFIX 137 H23A 2 1.034387 0.753676 0.510148 11.00000 -1.50000 H23B 2 1.007513 0.858278 0.523151 11.00000 -1.50000 H23C 2 1.070663 0.831148 0.465506 11.00000 -1.50000 AFIX 0 C13 1 1.117864 0.615363 0.436460 11.00000 0.07967 0.12323 = 0.05316 -0.01679 -0.01731 0.06230 AFIX 137 H13A 2 1.155845 0.675256 0.448221 11.00000 -1.50000 H13B 2 1.186515 0.571501 0.434668 11.00000 -1.50000 H13C 2 1.069492 0.595376 0.467517 11.00000 -1.50000 AFIX 0 C24 1 0.886488 0.957850 0.386215 11.00000 0.11644 0.04800 = 0.06937 -0.00992 0.03707 -0.02409 AFIX 137 H24A 2 0.969828 0.939924 0.377459 11.00000 -1.50000 H24B 2 0.900352 1.000647 0.421278 11.00000 -1.50000 H24C 2 0.834186 0.987033 0.349219 11.00000 -1.50000 AFIX 0 C26 1 0.693921 0.558879 0.036571 11.00000 0.21112 0.07639 = 0.10698 0.02243 0.10618 0.01551 PART 1 AFIX 23 H26C 2 0.661809 0.573922 -0.008030 10.50000 -1.20000 H26D 2 0.784791 0.579273 0.047455 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.651241 0.562469 -0.008112 10.50000 -1.20000 H26B 2 0.781614 0.584512 0.040883 10.50000 -1.20000 AFIX 0 CL1B 3 0.707539 0.449532 0.057172 10.50000 0.16818 0.08834 = 0.07992 0.02298 0.03458 0.05954 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0880, GooF = S = 1.044, Restrained GooF = 1.044 for all data REM R1 = 0.0373 for 6709 Fo > 4sig(Fo) and 0.0558 for all 8983 data REM 317 parameters refined using 6 restraints END WGHT 0.0364 0.0000 REM Highest difference peak 1.166, deepest hole -1.225, 1-sigma level 0.158 Q1 1 0.2945 0.7583 0.1631 11.00000 0.05 1.17 Q2 1 0.7752 0.4875 0.0414 11.00000 0.05 0.87 Q3 1 0.7967 0.4987 0.0546 11.00000 0.05 0.85 Q4 1 0.4669 0.8946 0.0619 11.00000 0.05 0.62 Q5 1 0.8329 0.6004 0.3420 11.00000 0.05 0.61 Q6 1 0.8373 0.4835 0.4215 11.00000 0.05 0.60 Q7 1 0.6814 0.5415 0.3410 11.00000 0.05 0.59 Q8 1 0.5748 0.9545 0.0818 11.00000 0.05 0.58 Q9 1 0.5256 0.6599 0.3002 11.00000 0.05 0.58 Q10 1 0.8251 0.7607 0.4610 11.00000 0.05 0.55 Q11 1 0.8377 0.8839 0.2963 11.00000 0.05 0.55 Q12 1 0.9098 0.5972 0.2780 11.00000 0.05 0.54 Q13 1 0.7031 0.7014 0.3391 11.00000 0.05 0.53 Q14 1 0.8006 0.7320 0.2609 11.00000 0.05 0.52 Q15 1 0.4374 0.6241 0.2764 11.00000 0.05 0.52 Q16 1 0.8787 0.7635 0.3401 11.00000 0.05 0.52 ; _shelx_res_checksum 87104 _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 2.423 _oxdiff_exptl_absorpt_empirical_full_min 0.547 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 0.80391(2) 0.71611(2) 0.33880(2) 0.02921(6) Uani 1 1 d . . . . . I1 I 0.52372(3) 0.61759(2) 0.27954(2) 0.04306(9) Uani 1 1 d . . . . . I4 I 0.82230(3) 0.93954(2) 0.20054(2) 0.05002(10) Uani 1 1 d . . . . . I3 I 0.48684(3) 0.93850(2) 0.08227(2) 0.05063(10) Uani 1 1 d . . . . . I2 I 0.29382(3) 0.72437(3) 0.12921(2) 0.06565(12) Uani 1 1 d . . . . . Cl2 Cl 0.6086(2) 0.62687(14) 0.07884(9) 0.0881(6) Uani 1 1 d . . . . . Cl1A Cl 0.6960(10) 0.4444(7) 0.0419(7) 0.145(5) Uani 0.5 1 d . U P A 1 N1 N 0.6779(3) 0.7747(2) 0.24101(17) 0.0332(7) Uani 1 1 d . . . . . C5 C 0.6701(4) 0.8461(3) 0.1982(2) 0.0339(9) Uani 1 1 d . . . . . C2 C 0.5604(4) 0.7302(3) 0.2245(2) 0.0347(9) Uani 1 1 d . . . . . C10 C 0.9577(5) 0.6484(3) 0.2652(2) 0.0403(10) Uani 1 1 d . . . . . C6 C 0.8874(4) 0.5715(3) 0.2818(3) 0.0420(11) Uani 1 1 d . . . . . C8 C 1.0269(5) 0.6215(3) 0.3724(3) 0.0470(12) Uani 1 1 d . . . . . C21 C 0.5209(5) 0.7368(4) 0.4240(3) 0.0622(16) Uani 1 1 d . . . . . H21A H 0.457840 0.753133 0.386207 0.093 Uiso 1 1 calc R U . . . H21B H 0.495320 0.763696 0.460497 0.093 Uiso 1 1 calc R U . . . H21C H 0.524481 0.670406 0.428454 0.093 Uiso 1 1 calc R U . . . C20 C 0.6800(5) 0.8528(3) 0.3852(2) 0.0439(11) Uani 1 1 d . . . . . C19 C 0.8158(5) 0.8727(3) 0.4031(3) 0.0474(12) Uani 1 1 d . . . . . C4 C 0.5496(4) 0.8454(3) 0.1557(2) 0.0357(9) Uani 1 1 d . . . . . C9 C 1.0425(4) 0.6801(3) 0.3213(3) 0.0443(11) Uani 1 1 d . . . . . C3 C 0.4786(4) 0.7706(3) 0.1734(2) 0.0370(9) Uani 1 1 d . . . . . C16 C 0.6548(4) 0.7730(3) 0.4193(2) 0.0374(9) Uani 1 1 d . . . . . C25 C 0.5778(6) 0.9109(4) 0.3426(3) 0.0672(17) Uani 1 1 d . . . . . H25A H 0.617744 0.944190 0.312892 0.101 Uiso 1 1 calc R U . . . H25B H 0.540917 0.954217 0.368015 0.101 Uiso 1 1 calc R U . . . H25C H 0.509527 0.871397 0.319816 0.101 Uiso 1 1 calc R U . . . C15 C 0.9526(7) 0.6814(5) 0.1986(3) 0.0689(17) Uani 1 1 d . . . . . H15A H 0.863550 0.678927 0.174802 0.103 Uiso 1 1 calc R U . . . H15B H 1.006989 0.642282 0.178726 0.103 Uiso 1 1 calc R U . . . H15C H 0.984073 0.744192 0.199673 0.103 Uiso 1 1 calc R U . . . C12 C 0.8878(7) 0.4762(4) 0.3843(4) 0.080(2) Uani 1 1 d . . . . . H12A H 0.892397 0.495037 0.427646 0.119 Uiso 1 1 calc R U . . . H12B H 0.945616 0.424411 0.383544 0.119 Uiso 1 1 calc R U . . . H12C H 0.799259 0.458360 0.365418 0.119 Uiso 1 1 calc R U . . . C11 C 0.8003(6) 0.5090(4) 0.2338(4) 0.0730(19) Uani 1 1 d . . . . . H11A H 0.754226 0.466502 0.255810 0.110 Uiso 1 1 calc R U . . . H11B H 0.853503 0.474797 0.210332 0.110 Uiso 1 1 calc R U . . . H11C H 0.737881 0.546187 0.204999 0.110 Uiso 1 1 calc R U . . . C14 C 1.1416(6) 0.7569(5) 0.3233(4) 0.083(2) Uani 1 1 d . . . . . H14A H 1.096621 0.813866 0.309413 0.125 Uiso 1 1 calc R U . . . H14B H 1.200065 0.741669 0.295713 0.125 Uiso 1 1 calc R U . . . H14C H 1.191132 0.764141 0.366121 0.125 Uiso 1 1 calc R U . . . C17 C 0.7748(4) 0.7434(3) 0.4575(2) 0.0378(9) Uani 1 1 d . . . . . C18 C 0.8733(4) 0.8049(3) 0.4484(2) 0.0408(10) Uani 1 1 d . . . . . C22 C 0.7899(7) 0.6663(4) 0.5063(3) 0.0661(16) Uani 1 1 d . . . . . H22A H 0.743784 0.612148 0.487323 0.099 Uiso 1 1 calc R U . . . H22B H 0.753909 0.686002 0.541785 0.099 Uiso 1 1 calc R U . . . H22C H 0.881415 0.651896 0.520674 0.099 Uiso 1 1 calc R U . . . C7 C 0.9288(5) 0.5555(3) 0.3475(3) 0.0421(11) Uani 1 1 d . . . . . C23 C 1.0088(5) 0.8127(5) 0.4907(3) 0.0696(18) Uani 1 1 d . . . . . H23A H 1.034387 0.753676 0.510148 0.104 Uiso 1 1 calc R U . . . H23B H 1.007513 0.858278 0.523151 0.104 Uiso 1 1 calc R U . . . H23C H 1.070663 0.831148 0.465506 0.104 Uiso 1 1 calc R U . . . C13 C 1.1179(7) 0.6154(6) 0.4365(3) 0.090(3) Uani 1 1 d . . . . . H13A H 1.155845 0.675256 0.448221 0.135 Uiso 1 1 calc R U . . . H13B H 1.186515 0.571501 0.434668 0.135 Uiso 1 1 calc R U . . . H13C H 1.069492 0.595376 0.467517 0.135 Uiso 1 1 calc R U . . . C24 C 0.8865(8) 0.9579(4) 0.3862(3) 0.075(2) Uani 1 1 d . . . . . H24A H 0.969828 0.939924 0.377459 0.113 Uiso 1 1 calc R U . . . H24B H 0.900352 1.000647 0.421278 0.113 Uiso 1 1 calc R U . . . H24C H 0.834186 0.987033 0.349219 0.113 Uiso 1 1 calc R U . . . C26 C 0.6939(12) 0.5589(5) 0.0366(5) 0.121(4) Uani 1 1 d . . . . . H26C H 0.661809 0.573922 -0.008030 0.145 Uiso 0.5 1 calc R U P A 1 H26D H 0.784791 0.579273 0.047455 0.145 Uiso 0.5 1 calc R U P A 1 H26A H 0.651241 0.562469 -0.008112 0.145 Uiso 0.5 1 calc R U P A -1 H26B H 0.781614 0.584512 0.040883 0.145 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7075(11) 0.4495(7) 0.0572(4) 0.111(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 0.02792(10) 0.02893(11) 0.02890(11) -0.00031(7) 0.00170(7) 0.00365(7) I1 0.04414(17) 0.03805(16) 0.04612(19) 0.00248(13) 0.00753(13) -0.01199(12) I4 0.04434(18) 0.04725(18) 0.0578(2) 0.00801(15) 0.00933(15) -0.01297(13) I3 0.0581(2) 0.05310(19) 0.03918(18) 0.01267(14) 0.00678(15) 0.01837(14) I2 0.03678(18) 0.0634(2) 0.0840(3) -0.0010(2) -0.01636(17) -0.00680(14) Cl2 0.1046(14) 0.0916(13) 0.0686(11) 0.0077(9) 0.0193(10) 0.0337(10) Cl1A 0.088(4) 0.076(4) 0.275(13) -0.039(6) 0.049(6) -0.008(3) N1 0.0298(17) 0.0384(19) 0.0296(19) 0.0035(15) 0.0023(14) 0.0006(13) C5 0.030(2) 0.036(2) 0.037(2) 0.0047(18) 0.0093(17) 0.0012(16) C2 0.031(2) 0.035(2) 0.037(2) 0.0016(18) 0.0049(18) -0.0005(16) C10 0.046(3) 0.039(2) 0.037(2) 0.0030(19) 0.012(2) 0.0176(19) C6 0.034(2) 0.031(2) 0.059(3) -0.013(2) 0.006(2) 0.0046(17) C8 0.036(2) 0.052(3) 0.049(3) -0.006(2) 0.001(2) 0.017(2) C21 0.040(3) 0.079(4) 0.071(4) -0.022(3) 0.019(3) -0.001(3) C20 0.059(3) 0.034(2) 0.036(2) 0.0001(19) 0.003(2) 0.018(2) C19 0.060(3) 0.035(2) 0.051(3) -0.010(2) 0.023(3) -0.008(2) C4 0.033(2) 0.038(2) 0.035(2) 0.0027(18) 0.0043(18) 0.0026(16) C9 0.032(2) 0.036(2) 0.067(3) -0.005(2) 0.015(2) 0.0026(17) C3 0.031(2) 0.040(2) 0.036(2) -0.0017(19) 0.0003(18) -0.0017(17) C16 0.035(2) 0.040(2) 0.038(2) -0.0056(19) 0.0091(19) 0.0037(17) C25 0.084(4) 0.062(3) 0.049(3) 0.003(3) 0.000(3) 0.044(3) C15 0.090(5) 0.074(4) 0.051(3) 0.017(3) 0.032(3) 0.028(3) C12 0.090(5) 0.048(3) 0.114(6) 0.036(4) 0.050(5) 0.019(3) C11 0.054(3) 0.067(4) 0.092(5) -0.041(4) 0.002(3) 0.001(3) C14 0.053(4) 0.063(4) 0.139(7) -0.013(4) 0.035(4) -0.014(3) C17 0.044(2) 0.036(2) 0.033(2) 0.0001(18) 0.0089(19) 0.0039(18) C18 0.038(2) 0.048(3) 0.034(2) -0.010(2) 0.0019(19) 0.0007(19) C22 0.086(4) 0.065(4) 0.051(3) 0.021(3) 0.022(3) 0.019(3) C7 0.043(3) 0.031(2) 0.055(3) 0.009(2) 0.016(2) 0.0147(18) C23 0.045(3) 0.091(4) 0.065(4) -0.033(4) -0.006(3) -0.003(3) C13 0.080(5) 0.123(6) 0.053(4) -0.017(4) -0.017(3) 0.062(4) C24 0.116(6) 0.048(3) 0.069(4) -0.010(3) 0.037(4) -0.024(3) C26 0.211(11) 0.076(5) 0.107(7) 0.022(5) 0.106(8) 0.016(6) Cl1B 0.168(7) 0.088(5) 0.080(3) 0.023(3) 0.035(4) 0.060(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 7 5 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 61.84(8) . . ? N1 Dy1 C10 83.93(13) . . ? N1 Dy1 C6 92.52(14) . . ? N1 Dy1 C8 135.06(14) . . ? N1 Dy1 C20 81.25(13) . . ? N1 Dy1 C19 96.60(15) . . ? N1 Dy1 C9 107.67(15) . . ? N1 Dy1 C16 100.04(13) . . ? N1 Dy1 C17 129.79(13) . . ? N1 Dy1 C18 127.59(13) . . ? N1 Dy1 C7 122.92(14) . . ? C10 Dy1 I1 102.07(11) . . ? C10 Dy1 C20 153.36(15) . . ? C10 Dy1 C16 175.43(14) . . ? C6 Dy1 I1 80.21(10) . . ? C6 Dy1 C10 30.86(15) . . ? C6 Dy1 C8 51.01(15) . . ? C6 Dy1 C20 170.29(15) . . ? C6 Dy1 C16 145.78(14) . . ? C6 Dy1 C17 132.29(15) . . ? C8 Dy1 I1 122.84(12) . . ? C8 Dy1 C10 51.17(15) . . ? C8 Dy1 C20 137.95(15) . . ? C8 Dy1 C16 124.90(15) . . ? C8 Dy1 C17 94.84(15) . . ? C20 Dy1 I1 90.26(12) . . ? C20 Dy1 C16 30.77(14) . . ? C19 Dy1 I1 121.22(12) . . ? C19 Dy1 C10 131.13(15) . . ? C19 Dy1 C6 158.51(15) . . ? C19 Dy1 C8 110.80(17) . . ? C19 Dy1 C20 30.96(16) . . ? C19 Dy1 C9 107.53(15) . . ? C19 Dy1 C16 50.99(14) . . ? C19 Dy1 C17 51.19(15) . . ? C19 Dy1 C18 31.23(15) . . ? C19 Dy1 C7 138.18(17) . . ? C9 Dy1 I1 130.63(11) . . ? C9 Dy1 C10 30.89(15) . . ? C9 Dy1 C6 51.03(14) . . ? C9 Dy1 C8 31.11(16) . . ? C9 Dy1 C20 138.03(16) . . ? C9 Dy1 C16 147.21(16) . . ? C9 Dy1 C17 117.75(16) . . ? C9 Dy1 C18 97.64(15) . . ? C9 Dy1 C7 51.26(14) . . ? C16 Dy1 I1 78.06(10) . . ? C17 Dy1 I1 99.58(10) . . ? C17 Dy1 C10 145.89(14) . . ? C17 Dy1 C20 50.91(14) . . ? C17 Dy1 C16 30.57(14) . . ? C18 Dy1 I1 127.91(10) . . ? C18 Dy1 C10 128.40(15) . . ? C18 Dy1 C6 137.44(15) . . ? C18 Dy1 C8 86.96(15) . . ? C18 Dy1 C20 51.03(15) . . ? C18 Dy1 C16 50.57(14) . . ? C18 Dy1 C17 30.60(14) . . ? C7 Dy1 I1 91.86(11) . . ? C7 Dy1 C10 51.10(14) . . ? C7 Dy1 C6 30.78(16) . . ? C7 Dy1 C8 30.99(16) . . ? C7 Dy1 C20 153.17(15) . . ? C7 Dy1 C16 124.38(14) . . ? C7 Dy1 C17 102.44(15) . . ? C7 Dy1 C18 108.84(16) . . ? C2 I1 Dy1 68.09(12) . . ? C5 N1 Dy1 143.2(3) . . ? C2 N1 Dy1 111.1(3) . . ? C2 N1 C5 104.8(3) . . ? N1 C5 I4 122.3(3) . . ? N1 C5 C4 110.7(4) . . ? C4 C5 I4 126.9(3) . . ? N1 C2 I1 118.7(3) . . ? N1 C2 C3 112.4(4) . . ? C3 C2 I1 128.8(3) . . ? C6 C10 Dy1 74.4(2) . . ? C6 C10 C15 124.9(5) . . ? C9 C10 Dy1 73.8(2) . . ? C9 C10 C6 107.6(4) . . ? C9 C10 C15 127.1(5) . . ? C15 C10 Dy1 123.1(3) . . ? C10 C6 Dy1 74.8(2) . . ? C10 C6 C11 124.2(5) . . ? C11 C6 Dy1 124.9(3) . . ? C7 C6 Dy1 74.1(2) . . ? C7 C6 C10 108.4(4) . . ? C7 C6 C11 126.7(5) . . ? C9 C8 Dy1 73.8(2) . . ? C9 C8 C13 126.3(6) . . ? C7 C8 Dy1 73.9(2) . . ? C7 C8 C9 107.3(4) . . ? C7 C8 C13 125.0(6) . . ? C13 C8 Dy1 128.8(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 73.5(3) . . ? C19 C20 C16 107.9(4) . . ? C19 C20 C25 126.2(5) . . ? C16 C20 Dy1 75.5(2) . . ? C16 C20 C25 125.6(5) . . ? C25 C20 Dy1 121.4(3) . . ? C20 C19 Dy1 75.5(3) . . ? C20 C19 C18 107.4(4) . . ? C20 C19 C24 127.5(5) . . ? C18 C19 Dy1 74.7(3) . . ? C18 C19 C24 124.5(5) . . ? C24 C19 Dy1 122.7(4) . . ? C5 C4 I3 126.5(3) . . ? C5 C4 C3 106.4(4) . . ? C3 C4 I3 127.2(3) . . ? C10 C9 Dy1 75.4(2) . . ? C10 C9 C8 108.4(4) . . ? C10 C9 C14 124.3(6) . . ? C8 C9 Dy1 75.1(2) . . ? C8 C9 C14 127.1(6) . . ? C14 C9 Dy1 120.7(3) . . ? C2 C3 I2 126.3(3) . . ? C2 C3 C4 105.6(4) . . ? C4 C3 I2 128.0(3) . . ? C21 C16 Dy1 127.2(3) . . ? C20 C16 Dy1 73.7(3) . . ? C20 C16 C21 126.1(5) . . ? C17 C16 Dy1 73.8(2) . . ? C17 C16 C21 125.0(5) . . ? C17 C16 C20 108.0(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 75.7(3) . . ? C16 C17 C22 125.1(4) . . ? C18 C17 Dy1 74.1(3) . . ? C18 C17 C16 108.3(4) . . ? C18 C17 C22 126.1(5) . . ? C22 C17 Dy1 122.7(3) . . ? C19 C18 Dy1 74.1(3) . . ? C19 C18 C23 124.4(5) . . ? C17 C18 Dy1 75.3(3) . . ? C17 C18 C19 108.4(4) . . ? C17 C18 C23 125.6(5) . . ? C23 C18 Dy1 128.1(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 75.1(2) . . ? C6 C7 C8 108.3(4) . . ? C6 C7 C12 126.4(5) . . ? C8 C7 Dy1 75.1(2) . . ? C8 C7 C12 125.0(6) . . ? C12 C7 Dy1 120.9(3) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Cl2 C26 H26C 106.7 . . ? Cl2 C26 H26D 106.7 . . ? Cl2 C26 H26A 108.3 . . ? Cl2 C26 H26B 108.3 . . ? Cl1A C26 Cl2 122.5(6) . . ? Cl1A C26 H26C 106.7 . . ? Cl1A C26 H26D 106.7 . . ? Cl1A C26 H26A 96.8 . . ? Cl1A C26 H26B 112.0 . . ? H26C C26 H26D 106.6 . . ? H26C C26 H26A 11.7 . . ? H26C C26 H26B 97.5 . . ? H26D C26 H26A 116.2 . . ? H26D C26 H26B 9.3 . . ? H26A C26 H26B 107.4 . . ? Cl1B C26 Cl2 115.7(5) . . ? Cl1B C26 Cl1A 11.6(7) . . ? Cl1B C26 H26C 118.3 . . ? Cl1B C26 H26D 101.7 . . ? Cl1B C26 H26A 108.3 . . ? Cl1B C26 H26B 108.3 . . ? 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 3.2499(4) . ? Dy1 N1 2.383(3) . ? Dy1 C10 2.658(4) . ? Dy1 C6 2.653(4) . ? Dy1 C8 2.655(4) . ? Dy1 C20 2.658(4) . ? Dy1 C19 2.633(5) . ? Dy1 C9 2.637(4) . ? Dy1 C16 2.681(4) . ? Dy1 C17 2.657(4) . ? Dy1 C18 2.641(5) . ? Dy1 C7 2.639(4) . ? I1 C2 2.088(4) . ? I4 C5 2.070(4) . ? I3 C4 2.067(4) . ? I2 C3 2.066(4) . ? Cl2 C26 1.705(8) . ? Cl1A C26 1.653(12) . ? N1 C5 1.370(5) . ? N1 C2 1.359(5) . ? C5 C4 1.386(6) . ? C2 C3 1.370(6) . ? C10 C6 1.413(7) . ? C10 C9 1.410(7) . ? C10 C15 1.497(7) . ? C6 C11 1.516(7) . ? C6 C7 1.405(7) . ? C8 C9 1.419(7) . ? C8 C7 1.415(7) . ? C8 C13 1.499(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C21 C16 1.510(7) . ? C20 C19 1.412(7) . ? C20 C16 1.417(7) . ? C20 C25 1.502(6) . ? C19 C18 1.419(7) . ? C19 C24 1.512(7) . ? C4 C3 1.403(6) . ? C9 C14 1.506(7) . ? C16 C17 1.408(6) . ? 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 1.502(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 1.398(6) . ? C17 C22 1.512(7) . ? C18 C23 1.512(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 1.634(11) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Dy1 N1 C5 I4 12.0(6) . . . . ? Dy1 N1 C5 C4 -167.6(3) . . . . ? Dy1 N1 C2 I1 -5.8(4) . . . . ? Dy1 N1 C2 C3 171.6(3) . . . . ? Dy1 C10 C6 C11 122.2(5) . . . . ? Dy1 C10 C6 C7 -67.1(3) . . . . ? Dy1 C10 C9 C8 68.5(3) . . . . ? Dy1 C10 C9 C14 -117.4(5) . . . . ? Dy1 C6 C7 C8 -68.4(3) . . . . ? Dy1 C6 C7 C12 117.7(5) . . . . ? Dy1 C8 C9 C10 -68.7(3) . . . . ? Dy1 C8 C9 C14 117.4(5) . . . . ? Dy1 C8 C7 C6 68.4(3) . . . . ? Dy1 C8 C7 C12 -117.6(5) . . . . ? Dy1 C20 C19 C18 -68.5(3) . . . . ? Dy1 C20 C19 C24 120.4(5) . . . . ? Dy1 C20 C16 C21 -124.5(5) . . . . ? Dy1 C20 C16 C17 66.4(3) . . . . ? Dy1 C19 C18 C17 -68.1(3) . . . . ? Dy1 C19 C18 C23 125.6(5) . . . . ? Dy1 C16 C17 C18 67.5(3) . . . . ? Dy1 C16 C17 C22 -120.1(5) . . . . ? Dy1 C17 C18 C19 67.3(3) . . . . ? Dy1 C17 C18 C23 -126.6(5) . . . . ? I1 C2 C3 I2 -5.6(6) . . . . ? I1 C2 C3 C4 177.8(3) . . . . ? I4 C5 C4 I3 -0.2(6) . . . . ? I4 C5 C4 C3 -179.0(3) . . . . ? I3 C4 C3 I2 3.9(6) . . . . ? I3 C4 C3 C2 -179.5(3) . . . . ? N1 C5 C4 I3 179.4(3) . . . . ? N1 C5 C4 C3 0.6(5) . . . . ? N1 C2 C3 I2 177.3(3) . . . . ? N1 C2 C3 C4 0.7(5) . . . . ? C5 N1 C2 I1 -177.7(3) . . . . ? C5 N1 C2 C3 -0.3(5) . . . . ? C5 C4 C3 I2 -177.3(3) . . . . ? C5 C4 C3 C2 -0.8(5) . . . . ? C2 N1 C5 I4 179.4(3) . . . . ? C2 N1 C5 C4 -0.2(5) . . . . ? C10 C6 C7 Dy1 67.5(3) . . . . ? C10 C6 C7 C8 -0.9(5) . . . . ? C10 C6 C7 C12 -174.8(4) . . . . ? C6 C10 C9 Dy1 -67.2(3) . . . . ? C6 C10 C9 C8 1.3(5) . . . . ? C6 C10 C9 C14 175.4(5) . . . . ? C21 C16 C17 Dy1 124.4(5) . . . . ? C21 C16 C17 C18 -168.1(4) . . . . ? C21 C16 C17 C22 4.3(7) . . . . ? C20 C19 C18 Dy1 69.0(3) . . . . ? C20 C19 C18 C17 0.9(5) . . . . ? C20 C19 C18 C23 -165.4(5) . . . . ? C20 C16 C17 Dy1 -66.3(3) . . . . ? C20 C16 C17 C18 1.2(5) . . . . ? C20 C16 C17 C22 173.6(5) . . . . ? C19 C20 C16 Dy1 -67.0(3) . . . . ? C19 C20 C16 C21 168.5(5) . . . . ? C19 C20 C16 C17 -0.6(5) . . . . ? C9 C10 C6 Dy1 66.8(3) . . . . ? C9 C10 C6 C11 -171.0(4) . . . . ? C9 C10 C6 C7 -0.2(5) . . . . ? C9 C8 C7 Dy1 -66.7(3) . . . . ? C9 C8 C7 C6 1.7(5) . . . . ? C9 C8 C7 C12 175.7(4) . . . . ? C16 C20 C19 Dy1 68.3(3) . . . . ? C16 C20 C19 C18 -0.2(5) . . . . ? C16 C20 C19 C24 -171.3(5) . . . . ? C16 C17 C18 Dy1 -68.6(3) . . . . ? C16 C17 C18 C19 -1.3(5) . . . . ? C16 C17 C18 C23 164.8(5) . . . . ? C25 C20 C19 Dy1 -117.2(5) . . . . ? C25 C20 C19 C18 174.3(5) . . . . ? C25 C20 C19 C24 3.1(8) . . . . ? C25 C20 C16 Dy1 118.5(5) . . . . ? C25 C20 C16 C21 -6.0(8) . . . . ? C25 C20 C16 C17 -175.1(5) . . . . ? C15 C10 C6 Dy1 -119.8(4) . . . . ? C15 C10 C6 C11 2.4(7) . . . . ? C15 C10 C6 C7 173.2(4) . . . . ? C15 C10 C9 Dy1 119.6(5) . . . . ? C15 C10 C9 C8 -171.9(4) . . . . ? C15 C10 C9 C14 2.2(8) . . . . ? C11 C6 C7 Dy1 -122.0(5) . . . . ? C11 C6 C7 C8 169.6(5) . . . . ? C11 C6 C7 C12 -4.3(8) . . . . ? C22 C17 C18 Dy1 119.1(5) . . . . ? C22 C17 C18 C19 -173.6(5) . . . . ? C22 C17 C18 C23 -7.4(8) . . . . ? C7 C8 C9 Dy1 66.8(3) . . . . ? C7 C8 C9 C10 -1.8(5) . . . . ? C7 C8 C9 C14 -175.7(5) . . . . ? C13 C8 C9 Dy1 -126.5(5) . . . . ? C13 C8 C9 C10 164.8(5) . . . . ? C13 C8 C9 C14 -9.1(8) . . . . ? C13 C8 C7 Dy1 126.4(5) . . . . ? C13 C8 C7 C6 -165.2(5) . . . . ? C13 C8 C7 C12 8.8(8) . . . . ? C24 C19 C18 Dy1 -119.5(5) . . . . ? C24 C19 C18 C17 172.4(5) . . . . ? C24 C19 C18 C23 6.1(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 0.9483 -1.1458 -0.2720 -0.0783 -0.0142 0.0325 1.0827 0.8624 -0.1166 0.0038 0.0040 0.0859 -0.9483 1.1458 0.2720 0.0783 0.0142 -0.0325 -1.0827 -0.8624 0.1166 -0.0038 -0.0040 -0.0859 0.0369 -0.0553 0.9864 -0.0100 0.0322 0.0044 -0.0369 0.0553 -0.9864 0.0100 -0.0322 -0.0044 1.0089 0.9729 -2.0894 0.0239 -0.0605 0.0770 -1.0089 -0.9729 2.0894 -0.0239 0.0605 -0.0770 -1.1196 -0.8071 -0.8698 0.0063 -0.0363 -0.0903 -0.0066 1.1146 -1.8951 0.0612 -0.0554 0.0178 -2.1352 -0.6654 -0.6755 0.0435 -0.0312 -0.1495 0.1410 0.8936 2.0505 0.0210 0.0736 0.0356 1.0894 -0.2522 1.7785 -0.0574 0.0594 0.0681 0.9417 -0.0312 -2.1671 -0.0172 -0.0696 0.0503 7.1599 5.2409 21.5710 -0.1415 0.7602 0.6341