#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572180.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_1572180 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 101.833(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3635(2) _cell_length_b 14.3461(3) _cell_length_c 21.3369(5) _cell_measurement_reflns_used 19319 _cell_measurement_temperature 200.0(1) _cell_measurement_theta_max 30.9250 _cell_measurement_theta_min 2.8350 _cell_volume 3104.87(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 200.0(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 0.845 _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 -0.0362894000 _diffrn_orient_matrix_UB_12 0.0416841000 _diffrn_orient_matrix_UB_13 -0.0083601000 _diffrn_orient_matrix_UB_21 -0.0035313000 _diffrn_orient_matrix_UB_22 0.0067521000 _diffrn_orient_matrix_UB_23 0.0325416000 _diffrn_orient_matrix_UB_31 0.0596313000 _diffrn_orient_matrix_UB_32 0.0257493000 _diffrn_orient_matrix_UB_33 0.0049922000 _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 0.0542 _diffrn_reflns_av_unetI/netI 0.0450 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.845 _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 38696 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.845 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.679 _diffrn_reflns_theta_min 2.459 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.571 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.230 _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 2.326 _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 1.015 _refine_diff_density_min -1.360 _refine_diff_density_rms 0.159 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8865 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0318 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.0740 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7115 _reflns_number_total 8865 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP200K _cod_original_cell_volume 3104.86(13) _cod_database_code 1572180 _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 0.529 _shelx_estimated_absorpt_t_min 0.205 _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_200_final.res created by SHELXL-2018/3 at 16:27:37 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 10.363509 14.346078 21.336899 90 101.8334 90 ZERR 4 0.000245 0.00033 0.000528 0 0.0024 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. 25 0 0 PLAN 16 SIZE 0.111 0.275 0.353 TEMP -73.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.030900 FVAR 0.62780 DY1 4 0.804343 0.715025 0.339223 11.00000 0.02073 0.02134 = 0.02090 -0.00035 0.00093 0.00287 I1 5 0.524651 0.615712 0.281046 11.00000 0.03207 0.02802 = 0.03291 0.00178 0.00534 -0.00876 I4 5 0.821260 0.939650 0.200500 11.00000 0.03174 0.03389 = 0.04193 0.00519 0.00633 -0.00911 I3 5 0.484397 0.937174 0.081731 11.00000 0.04170 0.03872 = 0.02821 0.00880 0.00428 0.01293 I2 5 0.292629 0.721815 0.130161 11.00000 0.02654 0.04690 = 0.06323 0.00044 -0.01268 -0.00547 CL2 3 0.609035 0.627564 0.079439 11.00000 0.07242 0.06610 = 0.04962 0.00652 0.01336 0.02359 PART 1 CL1A 3 0.691357 0.444630 0.039351 10.50000 0.07878 0.06374 = 0.22603 -0.03743 0.02096 -0.00658 PART 0 N1 6 0.677934 0.773940 0.241400 11.00000 0.02187 0.02721 = 0.02264 0.00100 0.00233 -0.00244 C5 1 0.668662 0.845497 0.198160 11.00000 0.02438 0.02676 = 0.02511 -0.00018 0.00334 0.00021 C2 1 0.560226 0.728646 0.225288 11.00000 0.02579 0.02376 = 0.02615 0.00045 0.00493 0.00079 C10 1 0.957584 0.648357 0.264024 11.00000 0.03119 0.02776 = 0.02852 0.00526 0.00709 0.00897 C6 1 0.887412 0.570427 0.280659 11.00000 0.02534 0.02927 = 0.03453 -0.00586 0.00434 0.00543 C8 1 1.027894 0.620291 0.371618 11.00000 0.02808 0.03631 = 0.03478 -0.00445 -0.00042 0.01281 C21 1 0.519944 0.738369 0.424172 11.00000 0.03006 0.06093 = 0.04507 -0.01579 0.00977 -0.00363 AFIX 137 H21A 2 0.455588 0.759172 0.386491 11.00000 -1.50000 H21B 2 0.495590 0.763044 0.462981 11.00000 -1.50000 H21C 2 0.520845 0.670098 0.425797 11.00000 -1.50000 AFIX 0 C20 1 0.681956 0.853503 0.385495 11.00000 0.04351 0.02639 = 0.02581 -0.00270 0.00535 0.01286 C19 1 0.818784 0.871594 0.403462 11.00000 0.04593 0.02482 = 0.03458 -0.00485 0.01150 -0.00309 C4 1 0.548551 0.844069 0.155550 11.00000 0.02811 0.02609 = 0.02529 0.00202 0.00376 0.00353 C9 1 1.043029 0.679662 0.320267 11.00000 0.02201 0.03335 = 0.04783 -0.00746 0.00582 -0.00076 C3 1 0.477231 0.768196 0.173754 11.00000 0.02177 0.03073 = 0.02681 -0.00394 0.00097 -0.00070 C16 1 0.655211 0.773478 0.419932 11.00000 0.02488 0.02922 = 0.02693 -0.00421 0.00702 0.00503 C25 1 0.582178 0.912959 0.343052 11.00000 0.06264 0.04672 = 0.03923 0.00761 0.00577 0.03391 AFIX 137 H25A 2 0.624208 0.945846 0.312289 11.00000 -1.50000 H25B 2 0.546089 0.958446 0.369119 11.00000 -1.50000 H25C 2 0.510798 0.873578 0.319910 11.00000 -1.50000 AFIX 0 C15 1 0.952149 0.682239 0.197446 11.00000 0.06335 0.05702 = 0.04019 0.00903 0.02289 0.02226 AFIX 137 H15A 2 0.860119 0.684969 0.174418 11.00000 -1.50000 H15B 2 1.001448 0.639431 0.175304 11.00000 -1.50000 H15C 2 0.991308 0.744579 0.198871 11.00000 -1.50000 AFIX 0 C12 1 0.887805 0.474438 0.384088 11.00000 0.06771 0.04025 = 0.07511 0.02552 0.03185 0.01477 AFIX 137 H12A 2 0.879083 0.496419 0.426509 11.00000 -1.50000 H12B 2 0.954323 0.424972 0.388854 11.00000 -1.50000 H12C 2 0.802892 0.450008 0.361129 11.00000 -1.50000 AFIX 0 C11 1 0.800946 0.509014 0.232489 11.00000 0.04065 0.05139 = 0.06531 -0.03092 0.00430 0.00076 AFIX 137 H11A 2 0.754358 0.464572 0.254797 11.00000 -1.50000 H11B 2 0.855405 0.474924 0.207682 11.00000 -1.50000 H11C 2 0.736683 0.547491 0.203573 11.00000 -1.50000 AFIX 0 C14 1 1.144419 0.755343 0.322652 11.00000 0.03508 0.05132 = 0.09209 -0.00862 0.01663 -0.00774 AFIX 137 H14A 2 1.104874 0.808430 0.296756 11.00000 -1.50000 H14B 2 1.218966 0.731467 0.305665 11.00000 -1.50000 H14C 2 1.175461 0.775429 0.367089 11.00000 -1.50000 AFIX 0 C17 1 0.774923 0.742128 0.458714 11.00000 0.03114 0.03413 = 0.02292 -0.00223 0.00361 0.00468 C18 1 0.875718 0.803599 0.449621 11.00000 0.02955 0.03163 = 0.02700 -0.00839 0.00503 -0.00161 C22 1 0.787645 0.664199 0.506767 11.00000 0.05519 0.04236 = 0.03632 0.01589 0.01238 0.01260 AFIX 137 H22A 2 0.746738 0.607690 0.485727 11.00000 -1.50000 H22B 2 0.743344 0.681817 0.541415 11.00000 -1.50000 H22C 2 0.881141 0.652323 0.524463 11.00000 -1.50000 AFIX 0 C7 1 0.929439 0.554148 0.346892 11.00000 0.03222 0.02441 = 0.04644 0.01038 0.01481 0.01172 C23 1 1.011388 0.809544 0.491563 11.00000 0.03552 0.06016 = 0.04645 -0.02167 -0.00319 -0.00472 AFIX 137 H23A 2 1.035044 0.749109 0.512139 11.00000 -1.50000 H23B 2 1.012004 0.857303 0.524463 11.00000 -1.50000 H23C 2 1.075383 0.826089 0.465375 11.00000 -1.50000 AFIX 0 C13 1 1.119007 0.614339 0.435552 11.00000 0.05629 0.08292 = 0.04082 -0.01175 -0.01100 0.03721 AFIX 137 H13A 2 1.164739 0.673995 0.445406 11.00000 -1.50000 H13B 2 1.183835 0.564840 0.434788 11.00000 -1.50000 H13C 2 1.068221 0.600279 0.468405 11.00000 -1.50000 AFIX 0 C24 1 0.892366 0.956005 0.387239 11.00000 0.08591 0.03176 = 0.05548 -0.00741 0.02667 -0.01943 AFIX 137 H24A 2 0.971154 0.935909 0.372192 11.00000 -1.50000 H24B 2 0.918548 0.994950 0.425469 11.00000 -1.50000 H24C 2 0.835195 0.991988 0.353517 11.00000 -1.50000 AFIX 0 C26 1 0.697792 0.558955 0.037465 11.00000 0.19064 0.05529 = 0.09837 0.01536 0.10929 0.01257 PART 1 AFIX 23 H26C 2 0.671778 0.577586 -0.008056 10.50000 -1.20000 H26D 2 0.791579 0.576558 0.051793 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.658876 0.564880 -0.008775 10.50000 -1.20000 H26B 2 0.789090 0.583149 0.044442 10.50000 -1.20000 AFIX 0 CL1B 3 0.703644 0.445525 0.057045 10.50000 0.09943 0.05326 = 0.05782 0.01611 0.02797 0.03071 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0740, GooF = S = 1.055, Restrained GooF = 1.055 for all data REM R1 = 0.0318 for 7115 Fo > 4sig(Fo) and 0.0438 for all 8865 data REM 317 parameters refined using 6 restraints END WGHT 0.0309 0.0000 REM Highest difference peak 1.015, deepest hole -1.360, 1-sigma level 0.159 Q1 1 0.7778 0.4848 0.0533 11.00000 0.05 1.01 Q2 1 0.2916 0.7450 0.1602 11.00000 0.05 0.90 Q3 1 0.4468 0.5998 0.2788 11.00000 0.05 0.78 Q4 1 0.4724 0.8990 0.0605 11.00000 0.05 0.78 Q5 1 0.8726 0.7598 0.3406 11.00000 0.05 0.76 Q6 1 0.4336 0.6530 0.2812 11.00000 0.05 0.70 Q7 1 0.8812 0.7195 0.3005 11.00000 0.05 0.67 Q8 1 0.7085 0.7077 0.3791 11.00000 0.05 0.67 Q9 1 0.7158 0.6952 0.3389 11.00000 0.05 0.64 Q10 1 0.6194 0.5796 0.2818 11.00000 0.05 0.63 Q11 1 0.9101 0.9161 0.2013 11.00000 0.05 0.61 Q12 1 0.7959 0.6005 0.3384 11.00000 0.05 0.60 Q13 1 0.7225 0.5748 0.0581 11.00000 0.05 0.59 Q14 1 0.4515 0.6132 0.3195 11.00000 0.05 0.59 Q15 1 0.9429 0.6041 0.2776 11.00000 0.05 0.57 Q16 1 0.7061 0.5426 0.2955 11.00000 0.05 0.56 ; _shelx_res_checksum 95582 _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 2.446 _oxdiff_exptl_absorpt_empirical_full_min 0.658 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 0.80434(2) 0.71503(2) 0.33922(2) 0.02147(5) Uani 1 1 d . . . . . I1 I 0.52465(2) 0.61571(2) 0.28105(2) 0.03119(7) Uani 1 1 d . . . . . I4 I 0.82126(3) 0.93965(2) 0.20050(2) 0.03603(7) Uani 1 1 d . . . . . I3 I 0.48440(3) 0.93717(2) 0.08173(2) 0.03662(7) Uani 1 1 d . . . . . I2 I 0.29263(3) 0.72181(2) 0.13016(2) 0.04868(9) Uani 1 1 d . . . . . Cl2 Cl 0.60904(15) 0.62756(10) 0.07944(7) 0.0626(3) Uani 1 1 d . . . . . Cl1A Cl 0.6914(10) 0.4446(6) 0.0394(5) 0.124(3) Uani 0.5 1 d . U P A 1 N1 N 0.6779(3) 0.77394(19) 0.24140(14) 0.0242(6) Uani 1 1 d . . . . . C5 C 0.6687(3) 0.8455(2) 0.19816(18) 0.0257(7) Uani 1 1 d . . . . . C2 C 0.5602(3) 0.7286(2) 0.22529(17) 0.0253(7) Uani 1 1 d . . . . . C10 C 0.9576(4) 0.6484(3) 0.26402(18) 0.0290(8) Uani 1 1 d . . . . . C6 C 0.8874(4) 0.5704(2) 0.2807(2) 0.0300(8) Uani 1 1 d . . . . . C8 C 1.0279(4) 0.6203(3) 0.3716(2) 0.0340(9) Uani 1 1 d . . . . . C21 C 0.5199(4) 0.7384(3) 0.4242(2) 0.0451(11) Uani 1 1 d . . . . . H21A H 0.455588 0.759172 0.386491 0.068 Uiso 1 1 calc R U . . . H21B H 0.495590 0.763044 0.462981 0.068 Uiso 1 1 calc R U . . . H21C H 0.520845 0.670098 0.425797 0.068 Uiso 1 1 calc R U . . . C20 C 0.6820(4) 0.8535(3) 0.38550(19) 0.0322(8) Uani 1 1 d . . . . . C19 C 0.8188(4) 0.8716(2) 0.4035(2) 0.0346(9) Uani 1 1 d . . . . . C4 C 0.5486(4) 0.8441(2) 0.15555(18) 0.0267(7) Uani 1 1 d . . . . . C9 C 1.0430(4) 0.6797(3) 0.3203(2) 0.0346(9) Uani 1 1 d . . . . . C3 C 0.4772(3) 0.7682(2) 0.17375(18) 0.0270(7) Uani 1 1 d . . . . . C16 C 0.6552(3) 0.7735(2) 0.41993(18) 0.0268(7) Uani 1 1 d . . . . . C25 C 0.5822(5) 0.9130(3) 0.3431(2) 0.0502(12) Uani 1 1 d . . . . . H25A H 0.624208 0.945846 0.312289 0.075 Uiso 1 1 calc R U . . . H25B H 0.546089 0.958446 0.369119 0.075 Uiso 1 1 calc R U . . . H25C H 0.510798 0.873578 0.319910 0.075 Uiso 1 1 calc R U . . . C15 C 0.9521(5) 0.6822(4) 0.1974(2) 0.0518(12) Uani 1 1 d . . . . . H15A H 0.860119 0.684969 0.174418 0.078 Uiso 1 1 calc R U . . . H15B H 1.001448 0.639431 0.175304 0.078 Uiso 1 1 calc R U . . . H15C H 0.991308 0.744579 0.198871 0.078 Uiso 1 1 calc R U . . . C12 C 0.8878(5) 0.4744(3) 0.3841(3) 0.0586(14) Uani 1 1 d . . . . . H12A H 0.879083 0.496419 0.426509 0.088 Uiso 1 1 calc R U . . . H12B H 0.954323 0.424972 0.388854 0.088 Uiso 1 1 calc R U . . . H12C H 0.802892 0.450008 0.361129 0.088 Uiso 1 1 calc R U . . . C11 C 0.8009(5) 0.5090(3) 0.2325(3) 0.0534(13) Uani 1 1 d . . . . . H11A H 0.754358 0.464572 0.254797 0.080 Uiso 1 1 calc R U . . . H11B H 0.855405 0.474924 0.207682 0.080 Uiso 1 1 calc R U . . . H11C H 0.736683 0.547491 0.203573 0.080 Uiso 1 1 calc R U . . . C14 C 1.1444(5) 0.7553(4) 0.3227(3) 0.0590(14) Uani 1 1 d . . . . . H14A H 1.104874 0.808430 0.296756 0.088 Uiso 1 1 calc R U . . . H14B H 1.218966 0.731467 0.305665 0.088 Uiso 1 1 calc R U . . . H14C H 1.175461 0.775429 0.367089 0.088 Uiso 1 1 calc R U . . . C17 C 0.7749(4) 0.7421(3) 0.45871(18) 0.0297(8) Uani 1 1 d . . . . . C18 C 0.8757(4) 0.8036(3) 0.44962(19) 0.0295(8) Uani 1 1 d . . . . . C22 C 0.7876(5) 0.6642(3) 0.5068(2) 0.0442(10) Uani 1 1 d . . . . . H22A H 0.746738 0.607690 0.485727 0.066 Uiso 1 1 calc R U . . . H22B H 0.743344 0.681817 0.541415 0.066 Uiso 1 1 calc R U . . . H22C H 0.881141 0.652323 0.524463 0.066 Uiso 1 1 calc R U . . . C7 C 0.9294(4) 0.5541(2) 0.3469(2) 0.0334(9) Uani 1 1 d . . . . . C23 C 1.0114(4) 0.8095(4) 0.4916(2) 0.0490(12) Uani 1 1 d . . . . . H23A H 1.035044 0.749109 0.512139 0.074 Uiso 1 1 calc R U . . . H23B H 1.012004 0.857303 0.524463 0.074 Uiso 1 1 calc R U . . . H23C H 1.075383 0.826089 0.465375 0.074 Uiso 1 1 calc R U . . . C13 C 1.1190(5) 0.6143(4) 0.4356(3) 0.0630(16) Uani 1 1 d . . . . . H13A H 1.164739 0.673995 0.445406 0.095 Uiso 1 1 calc R U . . . H13B H 1.183835 0.564840 0.434788 0.095 Uiso 1 1 calc R U . . . H13C H 1.068221 0.600279 0.468405 0.095 Uiso 1 1 calc R U . . . C24 C 0.8924(6) 0.9560(3) 0.3872(3) 0.0560(14) Uani 1 1 d . . . . . H24A H 0.971154 0.935909 0.372192 0.084 Uiso 1 1 calc R U . . . H24B H 0.918548 0.994950 0.425469 0.084 Uiso 1 1 calc R U . . . H24C H 0.835195 0.991988 0.353517 0.084 Uiso 1 1 calc R U . . . C26 C 0.6978(10) 0.5590(4) 0.0375(4) 0.103(3) Uani 1 1 d . . . . . H26C H 0.671778 0.577586 -0.008056 0.124 Uiso 0.5 1 calc R U P A 1 H26D H 0.791579 0.576558 0.051793 0.124 Uiso 0.5 1 calc R U P A 1 H26A H 0.658876 0.564880 -0.008775 0.124 Uiso 0.5 1 calc R U P A -1 H26B H 0.789090 0.583149 0.044442 0.124 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7036(9) 0.4455(5) 0.0570(3) 0.0685(18) 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 0.02073(9) 0.02134(9) 0.02090(9) -0.00035(6) 0.00093(6) 0.00287(5) I1 0.03207(13) 0.02802(12) 0.03291(14) 0.00178(9) 0.00534(10) -0.00876(9) I4 0.03174(14) 0.03389(14) 0.04193(16) 0.00519(11) 0.00633(11) -0.00911(9) I3 0.04170(15) 0.03872(14) 0.02821(14) 0.00880(10) 0.00428(11) 0.01293(10) I2 0.02654(14) 0.04690(17) 0.0632(2) 0.00044(14) -0.01268(13) -0.00547(10) Cl2 0.0724(9) 0.0661(8) 0.0496(8) 0.0065(6) 0.0134(6) 0.0236(6) Cl1A 0.079(4) 0.064(4) 0.226(10) -0.037(5) 0.021(6) -0.007(3) N1 0.0219(15) 0.0272(15) 0.0226(15) 0.0010(12) 0.0023(11) -0.0024(11) C5 0.0244(17) 0.0268(17) 0.0251(18) -0.0002(14) 0.0033(14) 0.0002(13) C2 0.0258(18) 0.0238(17) 0.0262(18) 0.0004(14) 0.0049(14) 0.0008(12) C10 0.031(2) 0.0278(18) 0.0285(19) 0.0053(15) 0.0071(15) 0.0090(14) C6 0.0253(18) 0.0293(18) 0.035(2) -0.0059(15) 0.0043(15) 0.0054(14) C8 0.0281(19) 0.036(2) 0.035(2) -0.0045(17) -0.0004(16) 0.0128(15) C21 0.030(2) 0.061(3) 0.045(3) -0.016(2) 0.0098(19) -0.0036(19) C20 0.044(2) 0.0264(18) 0.0258(19) -0.0027(15) 0.0053(16) 0.0129(15) C19 0.046(2) 0.0248(18) 0.035(2) -0.0048(16) 0.0115(18) -0.0031(16) C4 0.0281(18) 0.0261(17) 0.0253(18) 0.0020(14) 0.0038(14) 0.0035(13) C9 0.0220(18) 0.033(2) 0.048(3) -0.0075(18) 0.0058(16) -0.0008(14) C3 0.0218(17) 0.0307(18) 0.0268(19) -0.0039(15) 0.0010(14) -0.0007(13) C16 0.0249(18) 0.0292(18) 0.0269(19) -0.0042(14) 0.0070(14) 0.0050(13) C25 0.063(3) 0.047(2) 0.039(3) 0.008(2) 0.006(2) 0.034(2) C15 0.063(3) 0.057(3) 0.040(3) 0.009(2) 0.023(2) 0.022(2) C12 0.068(3) 0.040(3) 0.075(4) 0.026(3) 0.032(3) 0.015(2) C11 0.041(3) 0.051(3) 0.065(3) -0.031(2) 0.004(2) 0.0008(19) C14 0.035(3) 0.051(3) 0.092(5) -0.009(3) 0.017(3) -0.008(2) C17 0.031(2) 0.0341(19) 0.0229(18) -0.0022(15) 0.0036(15) 0.0047(15) C18 0.0295(19) 0.0316(18) 0.0270(19) -0.0084(15) 0.0050(15) -0.0016(14) C22 0.055(3) 0.042(2) 0.036(2) 0.0159(19) 0.012(2) 0.0126(19) C7 0.032(2) 0.0244(18) 0.046(2) 0.0104(16) 0.0148(18) 0.0117(14) C23 0.036(2) 0.060(3) 0.046(3) -0.022(2) -0.003(2) -0.0047(19) C13 0.056(3) 0.083(4) 0.041(3) -0.012(3) -0.011(2) 0.037(3) C24 0.086(4) 0.032(2) 0.055(3) -0.007(2) 0.027(3) -0.019(2) C26 0.191(9) 0.055(4) 0.098(6) 0.015(3) 0.109(6) 0.013(4) Cl1B 0.099(4) 0.053(3) 0.0578(19) 0.0161(18) 0.028(2) 0.031(3) 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 6 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 62.09(7) . . ? N1 Dy1 C10 83.56(10) . . ? N1 Dy1 C6 92.18(11) . . ? N1 Dy1 C8 134.80(12) . . ? N1 Dy1 C20 80.87(11) . . ? N1 Dy1 C19 96.69(12) . . ? N1 Dy1 C9 107.39(12) . . ? N1 Dy1 C16 99.59(11) . . ? N1 Dy1 C17 129.68(11) . . ? N1 Dy1 C18 127.84(11) . . ? N1 Dy1 C7 122.73(12) . . ? C10 Dy1 I1 102.06(9) . . ? C10 Dy1 C16 176.46(11) . . ? C10 Dy1 C17 146.36(11) . . ? C6 Dy1 I1 80.04(8) . . ? C6 Dy1 C10 30.97(12) . . ? C6 Dy1 C16 146.55(12) . . ? C6 Dy1 C17 132.69(12) . . ? C8 Dy1 I1 122.65(9) . . ? C8 Dy1 C10 51.28(12) . . ? C8 Dy1 C6 51.10(12) . . ? C8 Dy1 C20 138.17(12) . . ? C8 Dy1 C16 125.61(12) . . ? C8 Dy1 C17 95.21(12) . . ? C20 Dy1 I1 90.77(9) . . ? C20 Dy1 C10 152.22(12) . . ? C20 Dy1 C6 170.37(12) . . ? C20 Dy1 C16 30.93(11) . . ? C20 Dy1 C17 51.39(12) . . ? C19 Dy1 I1 121.88(9) . . ? C19 Dy1 C10 130.37(12) . . ? C19 Dy1 C6 157.99(12) . . ? C19 Dy1 C8 110.48(13) . . ? C19 Dy1 C20 31.12(13) . . ? C19 Dy1 C9 106.89(12) . . ? C19 Dy1 C16 51.14(12) . . ? C19 Dy1 C17 51.54(12) . . ? C19 Dy1 C18 31.41(12) . . ? C19 Dy1 C7 138.05(14) . . ? C9 Dy1 I1 130.58(9) . . ? C9 Dy1 C10 30.91(12) . . ? C9 Dy1 C6 51.12(12) . . ? C9 Dy1 C8 31.18(13) . . ? C9 Dy1 C20 137.40(13) . . ? C9 Dy1 C16 147.53(13) . . ? C9 Dy1 C17 118.11(13) . . ? C9 Dy1 C18 97.43(12) . . ? C16 Dy1 I1 78.16(8) . . ? C17 Dy1 I1 99.34(8) . . ? C17 Dy1 C16 30.80(11) . . ? C18 Dy1 I1 128.12(8) . . ? C18 Dy1 C10 128.19(12) . . ? C18 Dy1 C6 137.41(12) . . ? C18 Dy1 C8 86.81(12) . . ? C18 Dy1 C20 51.45(12) . . ? C18 Dy1 C16 50.86(11) . . ? C18 Dy1 C17 30.85(12) . . ? C7 Dy1 I1 91.65(9) . . ? C7 Dy1 C10 51.31(12) . . ? C7 Dy1 C6 30.92(13) . . ? C7 Dy1 C8 31.01(13) . . ? C7 Dy1 C20 154.01(12) . . ? C7 Dy1 C9 51.39(12) . . ? C7 Dy1 C16 125.21(12) . . ? C7 Dy1 C17 102.73(13) . . ? C7 Dy1 C18 108.74(13) . . ? C2 I1 Dy1 68.18(10) . . ? C5 N1 Dy1 143.7(2) . . ? C2 N1 Dy1 110.8(2) . . ? C2 N1 C5 104.6(3) . . ? N1 C5 I4 121.6(2) . . ? N1 C5 C4 111.2(3) . . ? C4 C5 I4 127.2(3) . . ? N1 C2 I1 118.7(3) . . ? N1 C2 C3 112.7(3) . . ? C3 C2 I1 128.5(3) . . ? C6 C10 Dy1 74.4(2) . . ? C6 C10 C15 125.0(4) . . ? C9 C10 Dy1 73.8(2) . . ? C9 C10 C6 107.6(3) . . ? C9 C10 C15 126.9(4) . . ? C15 C10 Dy1 123.2(3) . . ? C10 C6 Dy1 74.6(2) . . ? C10 C6 C11 123.8(4) . . ? C11 C6 Dy1 125.1(3) . . ? C7 C6 Dy1 73.8(2) . . ? C7 C6 C10 108.2(3) . . ? C7 C6 C11 127.3(4) . . ? C9 C8 Dy1 73.8(2) . . ? C9 C8 C13 126.1(4) . . ? C7 C8 Dy1 73.8(2) . . ? C7 C8 C9 107.4(4) . . ? C7 C8 C13 125.1(4) . . ? C13 C8 Dy1 128.5(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 73.1(2) . . ? C19 C20 C16 107.4(3) . . ? C19 C20 C25 126.2(4) . . ? C16 C20 Dy1 75.30(19) . . ? C16 C20 C25 126.2(4) . . ? C25 C20 Dy1 121.7(3) . . ? C20 C19 Dy1 75.8(2) . . ? C20 C19 C18 108.2(3) . . ? C20 C19 C24 127.6(4) . . ? C18 C19 Dy1 75.3(2) . . ? C18 C19 C24 123.4(4) . . ? C24 C19 Dy1 123.1(3) . . ? C5 C4 I3 126.6(3) . . ? C5 C4 C3 106.4(3) . . ? C3 C4 I3 127.0(3) . . ? C10 C9 Dy1 75.3(2) . . ? C10 C9 C8 108.4(3) . . ? C10 C9 C14 124.8(4) . . ? C8 C9 Dy1 75.0(2) . . ? C8 C9 C14 126.4(4) . . ? C14 C9 Dy1 121.8(3) . . ? C2 C3 I2 126.9(3) . . ? C2 C3 C4 105.1(3) . . ? C4 C3 I2 127.9(3) . . ? C21 C16 Dy1 126.9(3) . . ? C20 C16 Dy1 73.8(2) . . ? C20 C16 C21 125.6(4) . . ? C17 C16 Dy1 74.0(2) . . ? C17 C16 C21 124.9(4) . . ? 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 75.2(2) . . ? C16 C17 C22 125.3(4) . . ? C18 C17 Dy1 74.1(2) . . ? C18 C17 C16 107.8(3) . . ? C18 C17 C22 126.5(4) . . ? C22 C17 Dy1 122.3(3) . . ? C19 C18 Dy1 73.3(2) . . ? C19 C18 C23 125.1(4) . . ? C17 C18 Dy1 75.1(2) . . ? C17 C18 C19 108.0(3) . . ? C17 C18 C23 125.5(4) . . ? C23 C18 Dy1 127.8(3) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C6 C7 Dy1 75.3(2) . . ? C6 C7 C8 108.3(3) . . ? C6 C7 C12 126.3(4) . . ? C8 C7 Dy1 75.1(2) . . ? C8 C7 C12 125.2(4) . . ? C12 C7 Dy1 120.5(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 106.8 . . ? Cl2 C26 H26D 106.8 . . ? Cl2 C26 H26A 108.5 . . ? Cl2 C26 H26B 108.5 . . ? Cl1A C26 Cl2 122.0(5) . . ? Cl1A C26 H26C 106.8 . . ? Cl1A C26 H26D 106.8 . . ? Cl1A C26 H26A 95.7 . . ? Cl1A C26 H26B 112.9 . . ? Cl1A C26 Cl1B 12.8(5) . . ? H26C C26 H26D 106.7 . . ? H26C C26 H26A 13.0 . . ? H26C C26 H26B 96.5 . . ? H26D C26 H26A 117.3 . . ? H26D C26 H26B 10.5 . . ? H26A C26 H26B 107.5 . . ? Cl1B C26 Cl2 114.9(4) . . ? Cl1B C26 H26C 119.7 . . ? Cl1B C26 H26D 100.8 . . ? Cl1B C26 H26A 108.5 . . ? Cl1B C26 H26B 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 3.2399(3) . ? Dy1 N1 2.380(3) . ? Dy1 C10 2.656(4) . ? Dy1 C6 2.655(3) . ? Dy1 C8 2.652(4) . ? Dy1 C20 2.654(3) . ? Dy1 C19 2.620(4) . ? Dy1 C9 2.636(4) . ? Dy1 C16 2.674(3) . ? Dy1 C17 2.658(4) . ? Dy1 C18 2.645(4) . ? Dy1 C7 2.636(3) . ? I1 C2 2.087(3) . ? I4 C5 2.073(3) . ? I3 C4 2.068(4) . ? I2 C3 2.059(4) . ? Cl2 C26 1.719(6) . ? Cl1A C26 1.642(11) . ? N1 C5 1.370(4) . ? N1 C2 1.363(4) . ? C5 C4 1.383(5) . ? C2 C3 1.372(5) . ? C10 C6 1.418(5) . ? C10 C9 1.411(6) . ? C10 C15 1.492(6) . ? C6 C11 1.503(6) . ? C6 C7 1.410(6) . ? C8 C9 1.422(6) . ? C8 C7 1.414(6) . ? C8 C13 1.494(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C16 1.510(5) . ? C20 C19 1.415(6) . ? C20 C16 1.421(5) . ? C20 C25 1.494(5) . ? C19 C18 1.425(6) . ? C19 C24 1.509(6) . ? C4 C3 1.414(5) . ? C9 C14 1.505(6) . ? C16 C17 1.416(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 1.505(6) . ? 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 1.411(5) . ? C17 C22 1.504(5) . ? C18 C23 1.506(6) . ? 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 1.678(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 12.1(5) . . . . ? Dy1 N1 C5 C4 -168.0(3) . . . . ? Dy1 N1 C2 I1 -5.6(3) . . . . ? Dy1 N1 C2 C3 172.1(2) . . . . ? Dy1 C10 C6 C11 122.2(4) . . . . ? Dy1 C10 C6 C7 -66.7(2) . . . . ? Dy1 C10 C9 C8 68.4(3) . . . . ? Dy1 C10 C9 C14 -118.8(4) . . . . ? Dy1 C6 C7 C8 -68.5(3) . . . . ? Dy1 C6 C7 C12 117.3(4) . . . . ? Dy1 C8 C9 C10 -68.6(3) . . . . ? Dy1 C8 C9 C14 118.7(4) . . . . ? Dy1 C8 C7 C6 68.6(2) . . . . ? Dy1 C8 C7 C12 -117.1(4) . . . . ? Dy1 C20 C19 C18 -69.0(3) . . . . ? Dy1 C20 C19 C24 121.0(4) . . . . ? Dy1 C20 C16 C21 -124.1(4) . . . . ? Dy1 C20 C16 C17 66.3(2) . . . . ? Dy1 C19 C18 C17 -67.6(3) . . . . ? Dy1 C19 C18 C23 124.8(4) . . . . ? Dy1 C16 C17 C18 67.5(2) . . . . ? Dy1 C16 C17 C22 -119.3(4) . . . . ? Dy1 C17 C18 C19 66.5(3) . . . . ? Dy1 C17 C18 C23 -126.1(4) . . . . ? I1 C2 C3 I2 -4.9(5) . . . . ? I1 C2 C3 C4 177.9(3) . . . . ? I4 C5 C4 I3 -0.8(5) . . . . ? I4 C5 C4 C3 -179.1(3) . . . . ? I3 C4 C3 I2 3.7(5) . . . . ? I3 C4 C3 C2 -179.2(3) . . . . ? N1 C5 C4 I3 179.3(2) . . . . ? N1 C5 C4 C3 1.1(4) . . . . ? N1 C2 C3 I2 177.6(2) . . . . ? N1 C2 C3 C4 0.5(4) . . . . ? C5 N1 C2 I1 -177.5(2) . . . . ? C5 N1 C2 C3 0.2(4) . . . . ? C5 C4 C3 I2 -178.0(3) . . . . ? C5 C4 C3 C2 -0.9(4) . . . . ? C2 N1 C5 I4 179.4(2) . . . . ? C2 N1 C5 C4 -0.8(4) . . . . ? C10 C6 C7 Dy1 67.2(2) . . . . ? C10 C6 C7 C8 -1.3(4) . . . . ? C10 C6 C7 C12 -175.5(4) . . . . ? C6 C10 C9 Dy1 -67.3(2) . . . . ? C6 C10 C9 C8 1.1(4) . . . . ? C6 C10 C9 C14 173.9(4) . . . . ? C21 C16 C17 Dy1 124.1(4) . . . . ? C21 C16 C17 C18 -168.4(4) . . . . ? C21 C16 C17 C22 4.8(6) . . . . ? C20 C19 C18 Dy1 69.3(3) . . . . ? C20 C19 C18 C17 1.7(4) . . . . ? C20 C19 C18 C23 -165.9(4) . . . . ? C20 C16 C17 Dy1 -66.2(2) . . . . ? C20 C16 C17 C18 1.3(4) . . . . ? C20 C16 C17 C22 174.5(4) . . . . ? C19 C20 C16 Dy1 -66.6(3) . . . . ? C19 C20 C16 C21 169.3(4) . . . . ? C19 C20 C16 C17 -0.2(4) . . . . ? C9 C10 C6 Dy1 66.9(3) . . . . ? C9 C10 C6 C11 -171.0(4) . . . . ? C9 C10 C6 C7 0.1(4) . . . . ? C9 C8 C7 Dy1 -66.7(3) . . . . ? C9 C8 C7 C6 1.9(4) . . . . ? C9 C8 C7 C12 176.2(4) . . . . ? C16 C20 C19 Dy1 68.1(3) . . . . ? C16 C20 C19 C18 -0.9(4) . . . . ? C16 C20 C19 C24 -170.9(4) . . . . ? C16 C17 C18 Dy1 -68.3(2) . . . . ? C16 C17 C18 C19 -1.8(4) . . . . ? C16 C17 C18 C23 165.6(4) . . . . ? C25 C20 C19 Dy1 -117.3(4) . . . . ? C25 C20 C19 C18 173.7(4) . . . . ? C25 C20 C19 C24 3.7(7) . . . . ? C25 C20 C16 Dy1 118.8(4) . . . . ? C25 C20 C16 C21 -5.3(6) . . . . ? C25 C20 C16 C17 -174.8(4) . . . . ? C15 C10 C6 Dy1 -119.9(4) . . . . ? C15 C10 C6 C11 2.3(6) . . . . ? C15 C10 C6 C7 173.4(3) . . . . ? C15 C10 C9 Dy1 119.6(4) . . . . ? C15 C10 C9 C8 -172.0(4) . . . . ? C15 C10 C9 C14 0.9(6) . . . . ? C11 C6 C7 Dy1 -122.1(4) . . . . ? C11 C6 C7 C8 169.4(4) . . . . ? C11 C6 C7 C12 -4.8(6) . . . . ? C22 C17 C18 Dy1 118.6(4) . . . . ? C22 C17 C18 C19 -174.9(4) . . . . ? C22 C17 C18 C23 -7.4(6) . . . . ? C7 C8 C9 Dy1 66.7(3) . . . . ? C7 C8 C9 C10 -1.9(4) . . . . ? C7 C8 C9 C14 -174.6(4) . . . . ? C13 C8 C9 Dy1 -126.1(4) . . . . ? C13 C8 C9 C10 165.3(4) . . . . ? C13 C8 C9 C14 -7.4(6) . . . . ? C13 C8 C7 Dy1 126.0(4) . . . . ? C13 C8 C7 C6 -165.4(4) . . . . ? C13 C8 C7 C12 8.9(6) . . . . ? C24 C19 C18 Dy1 -120.2(4) . . . . ? C24 C19 C18 C17 172.2(4) . . . . ? C24 C19 C18 C23 4.7(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 0.9996 -1.0317 -0.1126 -0.0783 -0.0142 0.0325 1.0142 0.9798 0.0304 0.0038 0.0040 0.0859 -0.9996 1.0317 0.1126 0.0783 0.0142 -0.0325 -1.0142 -0.9798 -0.0304 -0.0038 -0.0040 -0.0859 0.0062 -0.0353 0.9990 -0.0100 0.0322 0.0044 -0.0062 0.0353 -0.9990 0.0100 -0.0322 -0.0044 1.0019 1.0505 -1.9675 0.0239 -0.0605 0.0770 -1.0019 -1.0505 1.9675 -0.0239 0.0605 -0.0770 -1.0203 -0.9444 -1.0294 0.0063 -0.0363 -0.0903 -0.0050 1.0764 -1.9264 0.0612 -0.0554 0.0178 -2.0273 -0.9185 -0.9883 0.0435 -0.0312 -0.1495 0.0196 0.9350 2.0694 0.0210 0.0736 0.0356 1.0192 -0.0966 1.9568 -0.0574 0.0594 0.0681 0.9946 0.0448 -2.0390 -0.0172 -0.0696 0.0503 5.9852 6.3655 22.6896 -0.1415 0.7602 0.6341