#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:50:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294477 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572178.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_1572178 loop_ _publ_author_name 'Delano, 4th, Francis' 'Benner, Florian' 'Jang, Seoyun' 'Greer, Samuel M.' 'Demir, Selvan' _publ_section_title ; Construction of intermolecular σ-hole interactions in rare earth metallocene complexes using a 2,3,4,5-tetraiodopyrrolyl anion. ; _journal_issue 33 _journal_name_full 'Chemical science' _journal_page_first 13389 _journal_page_last 13404 _journal_paper_doi 10.1039/d4sc03786c _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C24 H30 Dy I4 N, C H2 Cl2' _chemical_formula_sum 'C25 H32 Cl2 Dy I4 N' _chemical_formula_weight 1087.51 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-07-10 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-04-22 deposited with the CCDC. 2024-07-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.719(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3485(2) _cell_length_b 14.3166(3) _cell_length_c 21.2970(5) _cell_measurement_reflns_used 20202 _cell_measurement_temperature 170.0(1) _cell_measurement_theta_max 31.4360 _cell_measurement_theta_min 2.6620 _cell_volume 3089.49(12) _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_environment N~2~ _diffrn_ambient_temperature 170.0(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 0.843 _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 -0.0369450000 _diffrn_orient_matrix_UB_12 0.0412267000 _diffrn_orient_matrix_UB_13 -0.0093198000 _diffrn_orient_matrix_UB_21 -0.0040230000 _diffrn_orient_matrix_UB_22 0.0081836000 _diffrn_orient_matrix_UB_23 0.0324038000 _diffrn_orient_matrix_UB_31 0.0592897000 _diffrn_orient_matrix_UB_32 0.0262405000 _diffrn_orient_matrix_UB_33 0.0045380000 _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 0.0516 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.843 _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 38295 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.843 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.679 _diffrn_reflns_theta_min 2.463 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.603 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.226 _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 2.338 _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 1.104 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.167 _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 8797 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0306 _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^)+(0.0319P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.0723 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7171 _reflns_number_total 8797 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP170K _cod_depositor_comments 'Adding full bibliography for 1572175--1572199.cif.' _cod_original_cell_volume 3089.48(12) _cod_database_code 1572178 _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 0.528 _shelx_estimated_absorpt_t_min 0.204 _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) H(0.5) HA(0.5) HB(0.5) HC(0.5) Cl1B(0.5) 4.a Secondary CH2 refined with riding coordinates: C26(H,HA), C26(HB,HC) 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_170_final.res created by SHELXL-2018/3 at 16:05:37 on 10-Jul-2023 REM Old TITL FED728_100_Final in P21/c #14 REM SHELXT solution in P2(1)/c: R1 0.076, Rweak 0.002, Alpha 0.023 REM 0.488 for 262 systematic absences, Orientation as input REM Formula found by SHELXT: C24 N Cl2 I4 Dy CELL 0.71073 10.348468 14.316603 21.296976 90 101.7191 90 ZERR 4 0.000237 0.000312 0.000504 0 0.0023 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. 10 0 0 PLAN 14 SIZE 0.111 0.275 0.353 TEMP -103.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.031900 FVAR 0.62615 DY1 4 0.804701 0.714341 0.339416 11.00000 0.01801 0.01809 = 0.01806 -0.00044 0.00075 0.00247 I1 5 0.525136 0.614421 0.281897 11.00000 0.02715 0.02349 = 0.02787 0.00135 0.00428 -0.00715 I4 5 0.820551 0.939695 0.200761 11.00000 0.02665 0.02813 = 0.03584 0.00448 0.00522 -0.00739 I3 5 0.483188 0.936105 0.081552 11.00000 0.03468 0.03246 = 0.02415 0.00713 0.00336 0.01054 I2 5 0.292009 0.720042 0.130735 11.00000 0.02255 0.03930 = 0.05397 0.00085 -0.01105 -0.00473 CL2 3 0.609524 0.628298 0.079636 11.00000 0.05951 0.05465 = 0.04128 0.00435 0.00994 0.01886 PART 1 CL1A 3 0.688170 0.446482 0.038245 10.50000 0.07281 0.04600 = 0.19726 -0.02029 0.00417 0.00202 PART 0 N1 6 0.677631 0.773494 0.241787 11.00000 0.02143 0.02231 = 0.01950 0.00209 0.00112 -0.00234 C5 1 0.668301 0.844940 0.198082 11.00000 0.01856 0.02187 = 0.02402 0.00060 0.00592 -0.00066 C2 1 0.560295 0.727469 0.225679 11.00000 0.02164 0.02028 = 0.02320 -0.00282 0.00536 -0.00192 C10 1 0.957518 0.647887 0.263646 11.00000 0.02151 0.02407 = 0.02805 0.00203 0.00642 0.00829 C6 1 0.887745 0.570112 0.279901 11.00000 0.02422 0.02140 = 0.02972 -0.00389 0.00324 0.00238 C8 1 1.028808 0.619739 0.370977 11.00000 0.02315 0.03609 = 0.02696 -0.00472 -0.00108 0.01472 C21 1 0.519006 0.738798 0.423791 11.00000 0.02233 0.04909 = 0.03975 -0.01306 0.00859 -0.00322 AFIX 137 H21A 2 0.455511 0.759256 0.385655 11.00000 -1.50000 H21B 2 0.493372 0.763982 0.462275 11.00000 -1.50000 H21C 2 0.519918 0.670407 0.425778 11.00000 -1.50000 AFIX 0 C20 1 0.683591 0.853890 0.385989 11.00000 0.03407 0.02393 = 0.02047 -0.00399 0.00237 0.00895 C19 1 0.820632 0.871025 0.404319 11.00000 0.03686 0.02132 = 0.02627 -0.00321 0.00786 -0.00019 C4 1 0.547759 0.843570 0.156238 11.00000 0.01946 0.02380 = 0.02267 0.00305 0.00341 0.00338 C9 1 1.044106 0.679248 0.320079 11.00000 0.01799 0.02519 = 0.04185 -0.00490 0.00464 0.00136 C3 1 0.476805 0.767124 0.173854 11.00000 0.01891 0.02742 = 0.02444 -0.00153 0.00049 -0.00031 C16 1 0.654905 0.773843 0.420196 11.00000 0.02502 0.02321 = 0.02259 -0.00213 0.00668 0.00442 C25 1 0.584368 0.914831 0.343238 11.00000 0.05159 0.04048 = 0.03356 0.00445 0.00479 0.02632 AFIX 137 H25A 2 0.627868 0.948736 0.313331 11.00000 -1.50000 H25B 2 0.547052 0.959593 0.369502 11.00000 -1.50000 H25C 2 0.513571 0.875850 0.319041 11.00000 -1.50000 AFIX 0 C15 1 0.951932 0.682836 0.196659 11.00000 0.05332 0.04249 = 0.03238 0.00816 0.01748 0.01509 AFIX 137 H15A 2 0.859638 0.687785 0.174202 11.00000 -1.50000 H15B 2 0.998645 0.639117 0.173706 11.00000 -1.50000 H15C 2 0.993866 0.744412 0.198357 11.00000 -1.50000 AFIX 0 C12 1 0.888012 0.472507 0.383105 11.00000 0.05956 0.03356 = 0.05858 0.01815 0.02827 0.01491 AFIX 137 H12A 2 0.888578 0.491930 0.427284 11.00000 -1.50000 H12B 2 0.949364 0.420296 0.383372 11.00000 -1.50000 H12C 2 0.798783 0.452798 0.362482 11.00000 -1.50000 AFIX 0 C11 1 0.800289 0.507811 0.231956 11.00000 0.03238 0.04214 = 0.05261 -0.02229 0.00572 -0.00118 AFIX 137 H11A 2 0.755152 0.462850 0.254755 11.00000 -1.50000 H11B 2 0.854273 0.474150 0.206531 11.00000 -1.50000 H11C 2 0.734706 0.546014 0.203477 11.00000 -1.50000 AFIX 0 C14 1 1.145846 0.755239 0.322425 11.00000 0.02946 0.04361 = 0.07903 -0.01362 0.01474 -0.01002 AFIX 137 H14A 2 1.108118 0.806675 0.294213 11.00000 -1.50000 H14B 2 1.223096 0.730133 0.308101 11.00000 -1.50000 H14C 2 1.172452 0.778302 0.366486 11.00000 -1.50000 AFIX 0 C17 1 0.774276 0.740808 0.459263 11.00000 0.02633 0.02668 = 0.02264 -0.00108 0.00667 0.00341 C18 1 0.876489 0.802302 0.450188 11.00000 0.02315 0.03069 = 0.02172 -0.00609 0.00269 -0.00137 C22 1 0.785613 0.663243 0.507084 11.00000 0.04850 0.03353 = 0.03036 0.01176 0.00875 0.00727 AFIX 137 H22A 2 0.731794 0.610200 0.487977 11.00000 -1.50000 H22B 2 0.754414 0.684924 0.545050 11.00000 -1.50000 H22C 2 0.878063 0.643767 0.519569 11.00000 -1.50000 AFIX 0 C7 1 0.929815 0.552862 0.346639 11.00000 0.02918 0.02151 = 0.03826 0.00568 0.01299 0.00975 C23 1 1.011930 0.807708 0.492721 11.00000 0.02923 0.05192 = 0.03772 -0.01531 -0.00292 -0.00008 AFIX 137 H23A 2 1.033039 0.747945 0.514869 11.00000 -1.50000 H23B 2 1.013385 0.857535 0.524409 11.00000 -1.50000 H23C 2 1.077360 0.821157 0.466520 11.00000 -1.50000 AFIX 0 C13 1 1.120099 0.612922 0.435195 11.00000 0.05111 0.06471 = 0.04115 -0.01196 -0.01143 0.03484 AFIX 137 H13A 2 1.171704 0.670587 0.443748 11.00000 -1.50000 H13B 2 1.179881 0.559805 0.435312 11.00000 -1.50000 H13C 2 1.068388 0.603919 0.468504 11.00000 -1.50000 AFIX 0 C24 1 0.896606 0.955679 0.387527 11.00000 0.06649 0.02683 = 0.04447 -0.00671 0.01843 -0.01195 AFIX 137 H24A 2 0.974343 0.934593 0.371778 11.00000 -1.50000 H24B 2 0.924732 0.994333 0.425844 11.00000 -1.50000 H24C 2 0.839529 0.992472 0.354176 11.00000 -1.50000 AFIX 0 C26 1 0.700087 0.559357 0.038229 11.00000 0.18624 0.05006 = 0.09758 0.01468 0.11025 0.02148 PART 1 AFIX 23 H 2 0.678418 0.579726 -0.007120 10.50000 -1.20000 HA 2 0.794188 0.574776 0.054512 10.50000 -1.20000 AFIX 23 PART -1 HB 2 0.664097 0.566725 -0.008255 10.50000 -1.20000 HC 2 0.792163 0.582471 0.046790 10.50000 -1.20000 AFIX 0 CL1B 3 0.701960 0.442421 0.056756 10.50000 0.07208 0.04639 = 0.04919 0.01380 0.02384 0.02017 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0723, GooF = S = 1.050, Restrained GooF = 1.050 for all data REM R1 = 0.0306 for 7171 Fo > 4sig(Fo) and 0.0421 for all 8797 data REM 317 parameters refined using 6 restraints END WGHT 0.0319 0.0000 REM Highest difference peak 1.104, deepest hole -1.118, 1-sigma level 0.167 Q1 1 0.7760 0.4817 0.0574 11.00000 0.05 1.10 Q2 1 0.2865 0.7422 0.1611 11.00000 0.05 1.01 Q3 1 0.7403 0.6602 0.3406 11.00000 0.05 0.88 Q4 1 0.8765 0.7602 0.3393 11.00000 0.05 0.76 Q5 1 1.0488 0.7191 0.3207 11.00000 0.05 0.69 Q6 1 0.9016 0.9009 0.2016 11.00000 0.05 0.65 Q7 1 1.1034 0.7177 0.1931 11.00000 0.05 0.64 Q8 1 0.4971 0.7859 0.4383 11.00000 0.05 0.64 Q9 1 0.1950 0.7173 0.1760 11.00000 0.05 0.63 Q10 1 0.3171 0.7439 0.1039 11.00000 0.05 0.62 Q11 1 1.0807 0.6133 0.3985 11.00000 0.05 0.61 Q12 1 0.6609 0.4567 0.2986 11.00000 0.05 0.61 Q13 1 0.4364 0.8800 0.0767 11.00000 0.05 0.60 Q14 1 0.3728 0.8992 0.0804 11.00000 0.05 0.60 ; _shelx_res_checksum 93649 _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 2.663 _oxdiff_exptl_absorpt_empirical_full_min 0.660 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 0.80470(2) 0.71434(2) 0.33942(2) 0.01847(5) Uani 1 1 d . . . . . I1 I 0.52514(2) 0.61442(2) 0.28190(2) 0.02635(6) Uani 1 1 d . . . . . I4 I 0.82055(2) 0.93969(2) 0.20076(2) 0.03037(7) Uani 1 1 d . . . . . I3 I 0.48319(3) 0.93611(2) 0.08155(2) 0.03080(7) Uani 1 1 d . . . . . I2 I 0.29201(3) 0.72004(2) 0.13074(2) 0.04127(8) Uani 1 1 d . . . . . Cl2 Cl 0.60952(13) 0.62830(9) 0.07964(6) 0.0519(3) Uani 1 1 d . . . . . Cl1A Cl 0.6882(10) 0.4465(6) 0.0382(5) 0.109(3) Uani 0.5 1 d . U P A 1 N1 N 0.6776(3) 0.77349(19) 0.24179(14) 0.0215(6) Uani 1 1 d . . . . . C5 C 0.6683(3) 0.8449(2) 0.19808(17) 0.0213(7) Uani 1 1 d . . . . . C2 C 0.5603(3) 0.7275(2) 0.22568(17) 0.0216(7) Uani 1 1 d . . . . . C10 C 0.9575(3) 0.6479(2) 0.26365(18) 0.0243(7) Uani 1 1 d . . . . . C6 C 0.8877(4) 0.5701(2) 0.27990(19) 0.0254(7) Uani 1 1 d . . . . . C8 C 1.0288(4) 0.6197(3) 0.37098(19) 0.0296(8) Uani 1 1 d . . . . . C21 C 0.5190(4) 0.7388(3) 0.4238(2) 0.0367(9) Uani 1 1 d . . . . . H21A H 0.455511 0.759256 0.385655 0.055 Uiso 1 1 calc R U . . . H21B H 0.493372 0.763982 0.462275 0.055 Uiso 1 1 calc R U . . . H21C H 0.519918 0.670407 0.425778 0.055 Uiso 1 1 calc R U . . . C20 C 0.6836(4) 0.8539(2) 0.38599(18) 0.0266(8) Uani 1 1 d . . . . . C19 C 0.8206(4) 0.8710(2) 0.40432(19) 0.0279(8) Uani 1 1 d . . . . . C4 C 0.5478(3) 0.8436(2) 0.15624(17) 0.0221(7) Uani 1 1 d . . . . . C9 C 1.0441(3) 0.6792(2) 0.3201(2) 0.0285(8) Uani 1 1 d . . . . . C3 C 0.4768(3) 0.7671(2) 0.17385(18) 0.0241(7) Uani 1 1 d . . . . . C16 C 0.6549(4) 0.7738(2) 0.42020(18) 0.0233(7) Uani 1 1 d . . . . . C25 C 0.5844(5) 0.9148(3) 0.3432(2) 0.0424(11) Uani 1 1 d . . . . . H25A H 0.627868 0.948736 0.313331 0.064 Uiso 1 1 calc R U . . . H25B H 0.547052 0.959593 0.369502 0.064 Uiso 1 1 calc R U . . . H25C H 0.513571 0.875850 0.319041 0.064 Uiso 1 1 calc R U . . . C15 C 0.9519(5) 0.6828(3) 0.1967(2) 0.0415(10) Uani 1 1 d . . . . . H15A H 0.859638 0.687785 0.174202 0.062 Uiso 1 1 calc R U . . . H15B H 0.998645 0.639117 0.173706 0.062 Uiso 1 1 calc R U . . . H15C H 0.993866 0.744412 0.198357 0.062 Uiso 1 1 calc R U . . . C12 C 0.8880(5) 0.4725(3) 0.3831(3) 0.0483(12) Uani 1 1 d . . . . . H12A H 0.888578 0.491930 0.427284 0.072 Uiso 1 1 calc R U . . . H12B H 0.949364 0.420296 0.383372 0.072 Uiso 1 1 calc R U . . . H12C H 0.798783 0.452798 0.362482 0.072 Uiso 1 1 calc R U . . . C11 C 0.8003(4) 0.5078(3) 0.2320(2) 0.0428(11) Uani 1 1 d . . . . . H11A H 0.755152 0.462850 0.254755 0.064 Uiso 1 1 calc R U . . . H11B H 0.854273 0.474150 0.206531 0.064 Uiso 1 1 calc R U . . . H11C H 0.734706 0.546014 0.203477 0.064 Uiso 1 1 calc R U . . . C14 C 1.1458(4) 0.7552(3) 0.3224(3) 0.0502(13) Uani 1 1 d . . . . . H14A H 1.108118 0.806675 0.294213 0.075 Uiso 1 1 calc R U . . . H14B H 1.223096 0.730133 0.308101 0.075 Uiso 1 1 calc R U . . . H14C H 1.172452 0.778302 0.366486 0.075 Uiso 1 1 calc R U . . . C17 C 0.7743(4) 0.7408(3) 0.45926(18) 0.0250(7) Uani 1 1 d . . . . . C18 C 0.8765(4) 0.8023(3) 0.45019(18) 0.0254(7) Uani 1 1 d . . . . . C22 C 0.7856(4) 0.6632(3) 0.5071(2) 0.0374(9) Uani 1 1 d . . . . . H22A H 0.731794 0.610200 0.487977 0.056 Uiso 1 1 calc R U . . . H22B H 0.754414 0.684924 0.545050 0.056 Uiso 1 1 calc R U . . . H22C H 0.878063 0.643767 0.519569 0.056 Uiso 1 1 calc R U . . . C7 C 0.9298(4) 0.5529(2) 0.3466(2) 0.0288(8) Uani 1 1 d . . . . . C23 C 1.0119(4) 0.8077(3) 0.4927(2) 0.0410(10) Uani 1 1 d . . . . . H23A H 1.033039 0.747945 0.514869 0.061 Uiso 1 1 calc R U . . . H23B H 1.013385 0.857535 0.524409 0.061 Uiso 1 1 calc R U . . . H23C H 1.077360 0.821157 0.466520 0.061 Uiso 1 1 calc R U . . . C13 C 1.1201(5) 0.6129(4) 0.4352(2) 0.0553(14) Uani 1 1 d . . . . . H13A H 1.171704 0.670587 0.443748 0.083 Uiso 1 1 calc R U . . . H13B H 1.179881 0.559805 0.435312 0.083 Uiso 1 1 calc R U . . . H13C H 1.068388 0.603919 0.468504 0.083 Uiso 1 1 calc R U . . . C24 C 0.8966(5) 0.9557(3) 0.3875(2) 0.0449(11) Uani 1 1 d . . . . . H24A H 0.974343 0.934593 0.371778 0.067 Uiso 1 1 calc R U . . . H24B H 0.924732 0.994333 0.425844 0.067 Uiso 1 1 calc R U . . . H24C H 0.839529 0.992472 0.354176 0.067 Uiso 1 1 calc R U . . . C26 C 0.7001(10) 0.5594(4) 0.0382(4) 0.100(3) Uani 1 1 d . . . . . H H 0.678418 0.579726 -0.007120 0.120 Uiso 0.5 1 calc R U P A 1 HA H 0.794188 0.574776 0.054512 0.120 Uiso 0.5 1 calc R U P A 1 HB H 0.664097 0.566725 -0.008255 0.120 Uiso 0.5 1 calc R U P A -1 HC H 0.792163 0.582471 0.046790 0.120 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7020(8) 0.4424(5) 0.0568(3) 0.0543(14) 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 0.01801(9) 0.01809(8) 0.01806(8) -0.00044(6) 0.00075(6) 0.00247(5) I1 0.02715(13) 0.02349(12) 0.02787(13) 0.00135(9) 0.00428(9) -0.00715(8) I4 0.02665(13) 0.02813(13) 0.03584(15) 0.00448(10) 0.00522(10) -0.00739(9) I3 0.03468(14) 0.03246(13) 0.02415(13) 0.00713(10) 0.00336(10) 0.01054(9) I2 0.02255(13) 0.03930(15) 0.05397(19) 0.00085(12) -0.01105(12) -0.00473(10) Cl2 0.0595(8) 0.0546(7) 0.0413(7) 0.0043(5) 0.0099(6) 0.0189(5) Cl1A 0.073(3) 0.046(3) 0.197(9) -0.020(5) 0.004(5) 0.002(2) N1 0.0214(15) 0.0223(14) 0.0195(15) 0.0021(11) 0.0011(11) -0.0023(11) C5 0.0186(16) 0.0219(16) 0.0240(18) 0.0006(13) 0.0059(13) -0.0007(12) C2 0.0216(17) 0.0203(16) 0.0232(18) -0.0028(13) 0.0054(14) -0.0019(12) C10 0.0215(18) 0.0241(17) 0.0281(19) 0.0020(14) 0.0064(14) 0.0083(13) C6 0.0242(18) 0.0214(17) 0.030(2) -0.0039(14) 0.0032(15) 0.0024(13) C8 0.0231(18) 0.036(2) 0.027(2) -0.0047(16) -0.0011(15) 0.0147(15) C21 0.022(2) 0.049(2) 0.040(2) -0.013(2) 0.0086(17) -0.0032(16) C20 0.034(2) 0.0239(17) 0.0205(18) -0.0040(14) 0.0024(15) 0.0089(14) C19 0.037(2) 0.0213(17) 0.0263(19) -0.0032(15) 0.0079(16) -0.0002(14) C4 0.0195(16) 0.0238(17) 0.0227(18) 0.0031(14) 0.0034(13) 0.0034(12) C9 0.0180(17) 0.0252(18) 0.042(2) -0.0049(16) 0.0046(15) 0.0014(13) C3 0.0189(17) 0.0274(17) 0.0244(18) -0.0015(15) 0.0005(14) -0.0003(13) C16 0.0250(18) 0.0232(17) 0.0226(18) -0.0021(14) 0.0067(14) 0.0044(13) C25 0.052(3) 0.040(2) 0.034(2) 0.0045(19) 0.005(2) 0.026(2) C15 0.053(3) 0.042(2) 0.032(2) 0.0082(19) 0.017(2) 0.015(2) C12 0.060(3) 0.034(2) 0.059(3) 0.018(2) 0.028(3) 0.015(2) C11 0.032(2) 0.042(2) 0.053(3) -0.022(2) 0.006(2) -0.0012(17) C14 0.029(2) 0.044(3) 0.079(4) -0.014(3) 0.015(2) -0.0100(19) C17 0.0263(18) 0.0267(18) 0.0226(18) -0.0011(14) 0.0067(14) 0.0034(14) C18 0.0232(18) 0.0307(18) 0.0217(18) -0.0061(15) 0.0027(14) -0.0014(13) C22 0.049(3) 0.034(2) 0.030(2) 0.0118(17) 0.0088(19) 0.0073(18) C7 0.029(2) 0.0215(17) 0.038(2) 0.0057(15) 0.0130(17) 0.0097(14) C23 0.029(2) 0.052(3) 0.038(2) -0.015(2) -0.0029(18) -0.0001(18) C13 0.051(3) 0.065(3) 0.041(3) -0.012(2) -0.011(2) 0.035(2) C24 0.066(3) 0.027(2) 0.044(3) -0.0067(19) 0.018(2) -0.012(2) C26 0.186(9) 0.050(3) 0.098(6) 0.015(3) 0.110(6) 0.021(4) Cl1B 0.072(3) 0.046(2) 0.0492(17) 0.0138(15) 0.0238(19) 0.0202(19) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -1 0 0.1241 1 1 0 0.1231 -1 1 0 0.1293 -1 -1 0 0.1498 0 0 1 0.0585 0 0 -1 0.0528 1 1 -2 0.0993 -1 -1 2 0.1399 -1 -1 -1 0.1333 0 1 -2 0.0924 -2 -1 -1 0.1448 0 1 2 0.0988 1 0 2 0.1081 1 0 -2 0.1036 6 7 22 0.0941 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Dy1 I1 62.20(7) . . ? N1 Dy1 C10 83.57(10) . . ? N1 Dy1 C6 91.99(11) . . ? N1 Dy1 C8 134.68(11) . . ? N1 Dy1 C20 80.77(11) . . ? N1 Dy1 C19 96.93(11) . . ? N1 Dy1 C9 107.52(12) . . ? N1 Dy1 C16 99.14(11) . . ? N1 Dy1 C17 129.45(10) . . ? N1 Dy1 C18 127.99(11) . . ? N1 Dy1 C7 122.71(12) . . ? C10 Dy1 I1 102.04(8) . . ? C10 Dy1 C6 30.75(11) . . ? C10 Dy1 C20 151.81(11) . . ? C10 Dy1 C16 176.93(11) . . ? C10 Dy1 C17 146.63(11) . . ? C6 Dy1 I1 80.02(8) . . ? C6 Dy1 C16 147.11(11) . . ? C6 Dy1 C17 132.94(11) . . ? C8 Dy1 I1 122.59(9) . . ? C8 Dy1 C10 51.15(12) . . ? C8 Dy1 C6 51.14(12) . . ? C8 Dy1 C20 138.11(12) . . ? C8 Dy1 C16 126.17(12) . . ? C8 Dy1 C17 95.59(12) . . ? C20 Dy1 I1 91.17(9) . . ? C20 Dy1 C6 170.55(12) . . ? C20 Dy1 C16 30.91(11) . . ? C20 Dy1 C17 51.53(11) . . ? C19 Dy1 I1 122.22(9) . . ? C19 Dy1 C10 130.21(12) . . ? C19 Dy1 C6 157.66(12) . . ? C19 Dy1 C8 110.19(12) . . ? C19 Dy1 C20 31.07(12) . . ? C19 Dy1 C9 106.52(12) . . ? C19 Dy1 C16 51.09(11) . . ? C19 Dy1 C17 51.67(11) . . ? C19 Dy1 C18 31.37(11) . . ? C19 Dy1 C7 137.82(13) . . ? C9 Dy1 I1 130.66(8) . . ? C9 Dy1 C10 31.07(12) . . ? C9 Dy1 C6 51.16(11) . . ? C9 Dy1 C8 30.96(12) . . ? C9 Dy1 C20 136.91(12) . . ? C9 Dy1 C16 147.61(12) . . ? C9 Dy1 C17 118.30(12) . . ? C9 Dy1 C18 97.31(12) . . ? C16 Dy1 I1 78.12(8) . . ? C17 Dy1 I1 98.92(8) . . ? C17 Dy1 C16 30.91(11) . . ? C18 Dy1 I1 128.00(8) . . ? C18 Dy1 C10 128.24(11) . . ? C18 Dy1 C6 137.45(12) . . ? C18 Dy1 C8 86.81(12) . . ? C18 Dy1 C20 51.45(11) . . ? C18 Dy1 C16 50.93(11) . . ? C18 Dy1 C17 31.03(11) . . ? C7 Dy1 I1 91.44(9) . . ? C7 Dy1 C10 51.36(11) . . ? C7 Dy1 C6 31.14(12) . . ? C7 Dy1 C8 31.16(12) . . ? C7 Dy1 C20 154.23(12) . . ? C7 Dy1 C9 51.52(11) . . ? C7 Dy1 C16 125.62(11) . . ? C7 Dy1 C17 102.77(12) . . ? C7 Dy1 C18 108.64(12) . . ? C2 I1 Dy1 68.17(10) . . ? C5 N1 Dy1 143.9(2) . . ? C2 N1 Dy1 110.7(2) . . ? C2 N1 C5 104.7(3) . . ? N1 C5 I4 121.4(2) . . ? N1 C5 C4 110.9(3) . . ? C4 C5 I4 127.6(3) . . ? N1 C2 I1 118.7(2) . . ? N1 C2 C3 112.6(3) . . ? C3 C2 I1 128.6(3) . . ? C6 C10 Dy1 74.7(2) . . ? C6 C10 C9 108.0(3) . . ? C6 C10 C15 125.1(4) . . ? C9 C10 Dy1 73.9(2) . . ? C9 C10 C15 126.5(4) . . ? C15 C10 Dy1 123.0(2) . . ? C10 C6 Dy1 74.59(19) . . ? C10 C6 C11 124.6(4) . . ? C10 C6 C7 108.4(3) . . ? C11 C6 Dy1 125.0(3) . . ? C7 C6 Dy1 73.8(2) . . ? C7 C6 C11 126.4(4) . . ? C9 C8 Dy1 74.1(2) . . ? C9 C8 C7 108.1(3) . . ? C9 C8 C13 126.2(4) . . ? C7 C8 Dy1 73.9(2) . . ? C7 C8 C13 124.3(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 73.2(2) . . ? C19 C20 C16 107.5(3) . . ? C19 C20 C25 126.1(4) . . ? C16 C20 Dy1 75.43(19) . . ? C16 C20 C25 126.1(4) . . ? C25 C20 Dy1 121.7(3) . . ? C20 C19 Dy1 75.8(2) . . ? C20 C19 C18 108.3(3) . . ? C20 C19 C24 127.5(4) . . ? C18 C19 Dy1 75.2(2) . . ? C18 C19 C24 123.6(4) . . ? C24 C19 Dy1 122.4(3) . . ? C5 C4 I3 126.5(3) . . ? C5 C4 C3 106.9(3) . . ? C3 C4 I3 126.6(3) . . ? C10 C9 Dy1 75.0(2) . . ? C10 C9 C14 125.0(4) . . ? C8 C9 Dy1 74.9(2) . . ? C8 C9 C10 108.0(3) . . ? C8 C9 C14 126.6(4) . . ? C14 C9 Dy1 121.9(3) . . ? C2 C3 I2 126.6(3) . . ? C2 C3 C4 104.9(3) . . ? C4 C3 I2 128.4(3) . . ? C21 C16 Dy1 126.4(2) . . ? C20 C16 Dy1 73.7(2) . . ? C20 C16 C21 126.0(3) . . ? C20 C16 C17 108.7(3) . . ? C17 C16 Dy1 73.91(19) . . ? C17 C16 C21 124.5(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 75.2(2) . . ? C16 C17 C22 125.7(3) . . ? C18 C17 Dy1 73.8(2) . . ? C18 C17 C16 107.3(3) . . ? C18 C17 C22 126.6(4) . . ? C22 C17 Dy1 122.6(2) . . ? C19 C18 Dy1 73.5(2) . . ? C19 C18 C23 125.1(4) . . ? C17 C18 Dy1 75.2(2) . . ? C17 C18 C19 108.2(3) . . ? C17 C18 C23 125.3(4) . . ? C23 C18 Dy1 128.2(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 75.07(19) . . ? C6 C7 C12 126.1(4) . . ? C8 C7 Dy1 74.9(2) . . ? C8 C7 C6 107.4(3) . . ? C8 C7 C12 126.2(4) . . ? C12 C7 Dy1 120.8(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 H 107.0 . . ? Cl2 C26 HA 107.0 . . ? Cl2 C26 HB 108.5 . . ? Cl2 C26 HC 108.5 . . ? Cl1A C26 Cl2 121.5(5) . . ? Cl1A C26 H 107.0 . . ? Cl1A C26 HA 107.0 . . ? Cl1A C26 HB 95.4 . . ? Cl1A C26 HC 113.8 . . ? Cl1A C26 Cl1B 13.2(5) . . ? H C26 HA 106.7 . . ? H C26 HB 13.7 . . ? H C26 HC 95.7 . . ? HA C26 HB 118.0 . . ? HA C26 HC 11.3 . . ? HB C26 HC 107.5 . . ? Cl1B C26 Cl2 115.0(4) . . ? Cl1B C26 H 120.0 . . ? Cl1B C26 HA 99.9 . . ? Cl1B C26 HB 108.5 . . ? Cl1B C26 HC 108.5 . . ? 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 3.2368(3) . ? Dy1 N1 2.379(3) . ? Dy1 C10 2.655(3) . ? Dy1 C6 2.655(3) . ? Dy1 C8 2.652(3) . ? Dy1 C20 2.655(3) . ? Dy1 C19 2.622(4) . ? Dy1 C9 2.641(3) . ? Dy1 C16 2.678(3) . ? Dy1 C17 2.662(4) . ? Dy1 C18 2.644(4) . ? Dy1 C7 2.639(3) . ? I1 C2 2.089(3) . ? I4 C5 2.071(3) . ? I3 C4 2.074(3) . ? I2 C3 2.059(4) . ? Cl2 C26 1.722(6) . ? Cl1A C26 1.621(10) . ? N1 C5 1.373(4) . ? N1 C2 1.363(4) . ? C5 C4 1.378(5) . ? C2 C3 1.378(5) . ? C10 C6 1.408(5) . ? C10 C9 1.418(5) . ? C10 C15 1.502(5) . ? C6 C11 1.511(5) . ? C6 C7 1.421(6) . ? C8 C9 1.413(6) . ? C8 C7 1.421(6) . ? C8 C13 1.499(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C16 1.510(5) . ? C20 C19 1.414(6) . ? C20 C16 1.421(5) . ? C20 C25 1.505(5) . ? C19 C18 1.424(5) . ? C19 C24 1.526(5) . ? C4 C3 1.411(5) . ? C9 C14 1.508(5) . ? C16 C17 1.423(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 1.500(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 1.419(5) . ? C17 C22 1.495(5) . ? C18 C23 1.508(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 H 0.9900 . ? C26 HA 0.9900 . ? C26 HB 0.9900 . ? C26 HC 0.9900 . ? C26 Cl1B 1.719(9) . ? 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 10.8(5) . . . . ? Dy1 N1 C5 C4 -168.0(3) . . . . ? Dy1 N1 C2 I1 -4.9(3) . . . . ? Dy1 N1 C2 C3 172.4(2) . . . . ? Dy1 C10 C6 C11 122.2(4) . . . . ? Dy1 C10 C6 C7 -66.6(2) . . . . ? Dy1 C10 C9 C8 68.3(2) . . . . ? Dy1 C10 C9 C14 -118.7(4) . . . . ? Dy1 C6 C7 C8 -68.5(2) . . . . ? Dy1 C6 C7 C12 117.5(4) . . . . ? Dy1 C8 C9 C10 -68.3(2) . . . . ? Dy1 C8 C9 C14 118.8(4) . . . . ? Dy1 C8 C7 C6 68.6(2) . . . . ? Dy1 C8 C7 C12 -117.4(4) . . . . ? Dy1 C20 C19 C18 -68.8(2) . . . . ? Dy1 C20 C19 C24 120.1(4) . . . . ? Dy1 C20 C16 C21 -123.5(4) . . . . ? Dy1 C20 C16 C17 66.2(2) . . . . ? Dy1 C19 C18 C17 -67.8(2) . . . . ? Dy1 C19 C18 C23 125.5(4) . . . . ? Dy1 C16 C17 C18 67.4(2) . . . . ? Dy1 C16 C17 C22 -119.8(4) . . . . ? Dy1 C17 C18 C19 66.6(2) . . . . ? Dy1 C17 C18 C23 -126.6(4) . . . . ? I1 C2 C3 I2 -4.9(5) . . . . ? I1 C2 C3 C4 177.1(2) . . . . ? I4 C5 C4 I3 1.0(5) . . . . ? I4 C5 C4 C3 -179.1(2) . . . . ? I3 C4 C3 I2 2.1(5) . . . . ? I3 C4 C3 C2 -180.0(2) . . . . ? N1 C5 C4 I3 179.8(2) . . . . ? N1 C5 C4 C3 -0.3(4) . . . . ? N1 C2 C3 I2 178.1(2) . . . . ? N1 C2 C3 C4 0.2(4) . . . . ? C5 N1 C2 I1 -177.7(2) . . . . ? C5 N1 C2 C3 -0.4(4) . . . . ? C5 C4 C3 I2 -177.8(3) . . . . ? C5 C4 C3 C2 0.1(4) . . . . ? C2 N1 C5 I4 179.2(2) . . . . ? C2 N1 C5 C4 0.4(4) . . . . ? C10 C6 C7 Dy1 67.2(2) . . . . ? C10 C6 C7 C8 -1.4(4) . . . . ? C10 C6 C7 C12 -175.3(3) . . . . ? C6 C10 C9 Dy1 -67.5(2) . . . . ? C6 C10 C9 C8 0.8(4) . . . . ? C6 C10 C9 C14 173.8(4) . . . . ? C21 C16 C17 Dy1 123.5(3) . . . . ? C21 C16 C17 C18 -169.1(3) . . . . ? C21 C16 C17 C22 3.7(6) . . . . ? C20 C19 C18 Dy1 69.2(3) . . . . ? C20 C19 C18 C17 1.4(4) . . . . ? C20 C19 C18 C23 -165.4(4) . . . . ? C20 C16 C17 Dy1 -66.0(2) . . . . ? C20 C16 C17 C18 1.4(4) . . . . ? C20 C16 C17 C22 174.2(4) . . . . ? C19 C20 C16 Dy1 -66.7(2) . . . . ? C19 C20 C16 C21 169.8(3) . . . . ? C19 C20 C16 C17 -0.5(4) . . . . ? C9 C10 C6 Dy1 67.0(2) . . . . ? C9 C10 C6 C11 -170.8(3) . . . . ? C9 C10 C6 C7 0.4(4) . . . . ? C9 C8 C7 Dy1 -66.8(2) . . . . ? C9 C8 C7 C6 1.9(4) . . . . ? C9 C8 C7 C12 175.8(3) . . . . ? C16 C20 C19 Dy1 68.2(2) . . . . ? C16 C20 C19 C18 -0.5(4) . . . . ? C16 C20 C19 C24 -171.6(4) . . . . ? C16 C17 C18 Dy1 -68.3(2) . . . . ? C16 C17 C18 C19 -1.7(4) . . . . ? C16 C17 C18 C23 165.0(4) . . . . ? C25 C20 C19 Dy1 -117.4(4) . . . . ? C25 C20 C19 C18 173.9(3) . . . . ? C25 C20 C19 C24 2.8(6) . . . . ? C25 C20 C16 Dy1 118.9(4) . . . . ? C25 C20 C16 C21 -4.6(6) . . . . ? C25 C20 C16 C17 -175.0(4) . . . . ? C15 C10 C6 Dy1 -119.9(3) . . . . ? C15 C10 C6 C11 2.4(6) . . . . ? C15 C10 C6 C7 173.5(3) . . . . ? C15 C10 C9 Dy1 119.5(4) . . . . ? C15 C10 C9 C8 -172.2(3) . . . . ? C15 C10 C9 C14 0.8(6) . . . . ? C11 C6 C7 Dy1 -121.9(4) . . . . ? C11 C6 C7 C8 169.6(4) . . . . ? C11 C6 C7 C12 -4.4(6) . . . . ? C22 C17 C18 Dy1 118.9(4) . . . . ? C22 C17 C18 C19 -174.4(3) . . . . ? C22 C17 C18 C23 -7.7(6) . . . . ? C7 C8 C9 Dy1 66.7(2) . . . . ? C7 C8 C9 C10 -1.7(4) . . . . ? C7 C8 C9 C14 -174.5(4) . . . . ? C13 C8 C9 Dy1 -126.3(4) . . . . ? C13 C8 C9 C10 165.4(4) . . . . ? C13 C8 C9 C14 -7.5(6) . . . . ? C13 C8 C7 Dy1 125.9(4) . . . . ? C13 C8 C7 C6 -165.5(4) . . . . ? C13 C8 C7 C12 8.5(6) . . . . ? C24 C19 C18 Dy1 -119.3(4) . . . . ? C24 C19 C18 C17 172.9(3) . . . . ? C24 C19 C18 C23 6.1(6) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 1.0015 -1.0154 -0.0562 -0.0783 -0.0142 0.0325 1.0080 0.9947 -0.0019 0.0038 0.0040 0.0859 -1.0015 1.0154 0.0562 0.0783 0.0142 -0.0325 -1.0080 -0.9947 0.0019 -0.0038 -0.0040 -0.0859 0.0046 -0.0138 0.9992 -0.0100 0.0322 0.0044 -0.0046 0.0138 -0.9992 0.0100 -0.0322 -0.0044 0.9989 1.0222 -2.0003 0.0239 -0.0605 0.0770 -0.9989 -1.0222 2.0003 -0.0239 0.0605 -0.0770 -1.0126 -0.9809 -0.9974 0.0063 -0.0363 -0.0903 -0.0059 1.0325 -1.9713 0.0612 -0.0554 0.0178 -2.0174 -0.9706 -0.9683 0.0435 -0.0312 -0.1495 0.0124 0.9775 2.0256 0.0210 0.0736 0.0356 1.0139 -0.0379 1.9694 -0.0574 0.0594 0.0681 0.9957 0.0172 -2.0275 -0.0172 -0.0696 0.0503 5.9079 6.9344 22.4424 -0.1415 0.7602 0.6341