#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:50:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294477 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572181.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_1572181 loop_ _publ_author_name 'Delano, 4th, Francis' 'Benner, Florian' 'Jang, Seoyun' 'Greer, Samuel M.' 'Demir, Selvan' _publ_section_title ; Construction of intermolecular σ-hole interactions in rare earth metallocene complexes using a 2,3,4,5-tetraiodopyrrolyl anion. ; _journal_issue 33 _journal_name_full 'Chemical science' _journal_page_first 13389 _journal_page_last 13404 _journal_paper_doi 10.1039/d4sc03786c _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C24 H30 Dy I4 N, C H2 Cl2' _chemical_formula_sum 'C25 H32 Cl2 Dy I4 N' _chemical_formula_weight 1087.51 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-07-10 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-04-22 deposited with the CCDC. 2024-07-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.072(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3931(3) _cell_length_b 14.3920(4) _cell_length_c 21.4414(6) _cell_measurement_reflns_used 17118 _cell_measurement_temperature 250.0(1) _cell_measurement_theta_max 30.3220 _cell_measurement_theta_min 2.8490 _cell_volume 3136.23(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 250.0(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 0.839 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 4.00 29.00 0.50 1.50 -- 6.58 -78.00 129.00 50 2 \w -39.00 -12.00 0.50 1.50 -- -7.98 -78.00 129.00 54 3 \w -28.00 19.00 0.50 1.50 -- -7.98 78.00-104.00 94 4 \w 0.00 35.00 0.50 1.50 -- 6.58 -99.00 120.00 70 5 \w 6.00 39.00 0.50 1.50 -- 6.58 -99.00-120.00 66 6 \w -11.00 15.00 0.50 1.50 -- 6.58 -77.00 60.00 52 7 \w 2.00 38.00 0.50 1.50 -- 6.58 57.00 -90.00 72 8 \w -31.00 7.00 0.50 1.50 -- -7.98 -57.00 30.00 76 9 \w -23.00 15.00 0.50 1.50 -- -7.98 77.00 -60.00 76 10 \w -28.00 7.00 0.50 1.50 -- -7.98 -57.00 60.00 70 11 \w -15.00 15.00 0.50 1.50 -- -7.98 -77.00 -30.00 60 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0326765000 _diffrn_orient_matrix_UB_12 0.0431260000 _diffrn_orient_matrix_UB_13 0.0073713000 _diffrn_orient_matrix_UB_21 -0.0005972000 _diffrn_orient_matrix_UB_22 0.0070823000 _diffrn_orient_matrix_UB_23 -0.0327950000 _diffrn_orient_matrix_UB_31 -0.0616647000 _diffrn_orient_matrix_UB_32 0.0227878000 _diffrn_orient_matrix_UB_33 -0.0037621000 _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 0.0575 _diffrn_reflns_av_unetI/netI 0.0493 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.839 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 39250 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.839 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.753 _diffrn_reflns_theta_min 2.453 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.505 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.240 _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 2.303 _exptl_crystal_description plate _exptl_crystal_F_000 2004 _exptl_crystal_size_max 0.353 _exptl_crystal_size_mid 0.275 _exptl_crystal_size_min 0.111 _refine_diff_density_max 0.958 _refine_diff_density_min -1.258 _refine_diff_density_rms 0.158 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8957 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0364 _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^)+(0.0364P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.0853 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6810 _reflns_number_total 8957 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP250K _cod_depositor_comments 'Adding full bibliography for 1572175--1572199.cif.' _cod_original_cell_volume 3136.21(14) _cod_database_code 1572181 _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 0.532 _shelx_estimated_absorpt_t_min 0.207 _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_250_final.res created by SHELXL-2018/3 at 16:52:58 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 10.393067 14.391964 21.441401 90 102.0716 90 ZERR 4 0.000254 0.000356 0.000587 0 0.0026 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 -23.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.036400 FVAR 0.59162 DY1 4 0.803929 0.715973 0.338884 11.00000 0.02678 0.02746 = 0.02694 -0.00026 0.00130 0.00352 I1 5 0.523873 0.617364 0.279794 11.00000 0.04224 0.03619 = 0.04335 0.00257 0.00708 -0.01141 I4 5 0.822197 0.939549 0.200513 11.00000 0.04215 0.04479 = 0.05458 0.00728 0.00849 -0.01223 I3 5 0.486439 0.938384 0.082169 11.00000 0.05504 0.04999 = 0.03712 0.01188 0.00618 0.01707 I2 5 0.293671 0.724039 0.129348 11.00000 0.03497 0.06045 = 0.07959 -0.00053 -0.01597 -0.00690 CL2 3 0.608672 0.626884 0.078922 11.00000 0.09696 0.08459 = 0.06776 0.00746 0.01784 0.03028 PART 1 CL1A 3 0.695637 0.442341 0.038969 10.50000 0.09132 0.08515 = 0.23746 -0.05101 0.04905 -0.00603 PART 0 N1 6 0.677933 0.774228 0.240920 11.00000 0.02702 0.03798 = 0.02769 0.00430 -0.00012 -0.00217 C5 1 0.669313 0.845557 0.198160 11.00000 0.03064 0.03135 = 0.03437 0.00234 0.00720 -0.00002 C2 1 0.560008 0.729725 0.224294 11.00000 0.02833 0.03312 = 0.03496 0.00184 0.00488 -0.00205 C10 1 0.957203 0.648323 0.265274 11.00000 0.03738 0.03848 = 0.03588 0.00533 0.01012 0.01272 C6 1 0.887425 0.571272 0.281466 11.00000 0.03640 0.03265 = 0.04706 -0.01310 0.00605 0.00533 C8 1 1.027392 0.621597 0.371921 11.00000 0.03415 0.05195 = 0.04132 -0.01083 -0.00003 0.01540 C21 1 0.521380 0.736921 0.424153 11.00000 0.03888 0.07930 = 0.06395 -0.02725 0.01771 -0.00398 AFIX 137 H21A 2 0.457458 0.754972 0.386340 11.00000 -1.50000 H21B 2 0.496453 0.763073 0.461612 11.00000 -1.50000 H21C 2 0.524024 0.669708 0.427536 11.00000 -1.50000 AFIX 0 C20 1 0.680627 0.852292 0.385018 11.00000 0.05389 0.03408 = 0.03306 -0.00156 0.00746 0.01792 C19 1 0.815730 0.872428 0.402767 11.00000 0.05313 0.03082 = 0.03960 -0.00901 0.01321 -0.00334 C4 1 0.549246 0.844764 0.155622 11.00000 0.03808 0.03381 = 0.03145 0.00068 0.00514 0.00647 C9 1 1.043177 0.680463 0.320936 11.00000 0.02550 0.03860 = 0.06060 -0.00545 0.00837 0.00144 C3 1 0.478330 0.769961 0.173209 11.00000 0.02699 0.03769 = 0.03573 -0.00385 -0.00028 -0.00145 C16 1 0.655337 0.772676 0.419446 11.00000 0.03517 0.04027 = 0.04075 -0.00457 0.00871 0.00299 C25 1 0.578506 0.911494 0.342491 11.00000 0.08469 0.05782 = 0.05222 0.00340 0.00537 0.04387 AFIX 137 H25A 2 0.621095 0.951105 0.316276 11.00000 -1.50000 H25B 2 0.533688 0.949692 0.368573 11.00000 -1.50000 H25C 2 0.515121 0.871723 0.315297 11.00000 -1.50000 AFIX 0 C15 1 0.953448 0.681180 0.198392 11.00000 0.07662 0.07268 = 0.05447 0.01263 0.03005 0.02445 AFIX 137 H15A 2 0.863195 0.681332 0.174530 11.00000 -1.50000 H15B 2 1.005644 0.639817 0.177921 11.00000 -1.50000 H15C 2 0.989080 0.743598 0.199554 11.00000 -1.50000 AFIX 0 C12 1 0.888023 0.476042 0.384413 11.00000 0.08869 0.05382 = 0.10483 0.03303 0.04659 0.02555 AFIX 137 H12A 2 0.896798 0.494073 0.428695 11.00000 -1.50000 H12B 2 0.943969 0.422858 0.381777 11.00000 -1.50000 H12C 2 0.797164 0.459816 0.366647 11.00000 -1.50000 AFIX 0 C11 1 0.800334 0.509130 0.234108 11.00000 0.05129 0.06490 = 0.08354 -0.03583 0.00389 0.00744 AFIX 137 H11A 2 0.753291 0.466753 0.256548 11.00000 -1.50000 H11B 2 0.853853 0.473864 0.210503 11.00000 -1.50000 H11C 2 0.737736 0.546729 0.204756 11.00000 -1.50000 AFIX 0 C14 1 1.143239 0.755913 0.323188 11.00000 0.04745 0.06482 = 0.12244 -0.01710 0.02773 -0.01289 AFIX 137 H14A 2 1.099221 0.813478 0.307850 11.00000 -1.50000 H14B 2 1.204091 0.738996 0.296406 11.00000 -1.50000 H14C 2 1.191228 0.764141 0.366765 11.00000 -1.50000 AFIX 0 C17 1 0.775615 0.742901 0.457565 11.00000 0.04410 0.03961 = 0.02851 -0.00119 0.00633 0.00559 C18 1 0.873505 0.804865 0.448301 11.00000 0.03584 0.04332 = 0.03269 -0.00953 0.00332 0.00070 C22 1 0.789547 0.665311 0.506822 11.00000 0.07994 0.06128 = 0.04374 0.01509 0.01676 0.01108 AFIX 137 H22A 2 0.714590 0.623831 0.496208 11.00000 -1.50000 H22B 2 0.793156 0.691858 0.548735 11.00000 -1.50000 H22C 2 0.869767 0.630825 0.506896 11.00000 -1.50000 AFIX 0 C7 1 0.928650 0.555906 0.347296 11.00000 0.04282 0.03366 = 0.05238 0.01100 0.01412 0.01410 C23 1 1.009386 0.812019 0.490566 11.00000 0.04757 0.08216 = 0.06440 -0.03155 -0.00966 0.00362 AFIX 137 H23A 2 1.032118 0.753457 0.512501 11.00000 -1.50000 H23B 2 1.010134 0.861091 0.521652 11.00000 -1.50000 H23C 2 1.072986 0.826096 0.464633 11.00000 -1.50000 AFIX 0 C13 1 1.118490 0.615387 0.435914 11.00000 0.07278 0.11266 = 0.05588 -0.02098 -0.01818 0.04924 AFIX 137 H13A 2 1.161704 0.674785 0.446416 11.00000 -1.50000 H13B 2 1.184145 0.567844 0.434838 11.00000 -1.50000 H13C 2 1.068616 0.599510 0.467928 11.00000 -1.50000 AFIX 0 C24 1 0.886852 0.957168 0.385866 11.00000 0.12122 0.03761 = 0.07261 -0.00893 0.04103 -0.02273 AFIX 137 H24A 2 0.968789 0.938375 0.374701 11.00000 -1.50000 H24B 2 0.905388 0.998933 0.422147 11.00000 -1.50000 H24C 2 0.832096 0.988666 0.349885 11.00000 -1.50000 AFIX 0 C26 1 0.694862 0.559547 0.036670 11.00000 0.20534 0.07055 = 0.10089 0.01716 0.10264 0.01113 PART 1 AFIX 23 H26C 2 0.664993 0.576963 -0.008214 10.50000 -1.20000 H26D 2 0.786930 0.579255 0.049094 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.652682 0.563081 -0.008638 10.50000 -1.20000 H26B 2 0.783941 0.584874 0.041551 10.50000 -1.20000 AFIX 0 CL1B 3 0.705365 0.450053 0.058485 10.50000 0.14095 0.06788 = 0.06818 0.01438 0.02955 0.04140 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0853, GooF = S = 1.039, Restrained GooF = 1.039 for all data REM R1 = 0.0364 for 6810 Fo > 4sig(Fo) and 0.0531 for all 8957 data REM 317 parameters refined using 6 restraints END WGHT 0.0364 0.0000 REM Highest difference peak 0.958, deepest hole -1.258, 1-sigma level 0.158 Q1 1 0.2910 0.7578 0.1636 11.00000 0.05 0.96 Q2 1 0.7921 0.4961 0.0561 11.00000 0.05 0.84 Q3 1 0.7659 0.4853 0.0428 11.00000 0.05 0.79 Q4 1 0.5636 0.9579 0.0836 11.00000 0.05 0.79 Q5 1 0.4742 0.8975 0.0617 11.00000 0.05 0.77 Q6 1 0.3856 0.9595 0.0784 11.00000 0.05 0.73 Q7 1 0.8789 0.7574 0.3394 11.00000 0.05 0.69 Q8 1 0.7187 0.7232 0.3418 11.00000 0.05 0.62 Q9 1 0.8059 0.6223 0.3382 11.00000 0.05 0.59 Q10 1 0.8642 0.5802 0.2945 11.00000 0.05 0.56 Q11 1 0.6348 0.5791 0.2809 11.00000 0.05 0.56 Q12 1 0.5190 0.8037 0.2804 11.00000 0.05 0.55 Q13 1 0.9879 0.6152 0.2622 11.00000 0.05 0.55 Q14 1 0.9022 0.6422 0.2788 11.00000 0.05 0.53 Q15 1 1.1741 0.7392 0.4203 11.00000 0.05 0.52 Q16 1 1.0741 0.6207 0.3955 11.00000 0.05 0.52 ; _shelx_res_checksum 62754 _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 2.460 _oxdiff_exptl_absorpt_empirical_full_min 0.582 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 0.80393(2) 0.71597(2) 0.33888(2) 0.02769(6) Uani 1 1 d . . . . . I1 I 0.52387(3) 0.61736(2) 0.27979(2) 0.04087(8) Uani 1 1 d . . . . . I4 I 0.82220(3) 0.93955(2) 0.20051(2) 0.04741(9) Uani 1 1 d . . . . . I3 I 0.48644(3) 0.93838(2) 0.08217(2) 0.04789(9) Uani 1 1 d . . . . . I2 I 0.29367(3) 0.72404(2) 0.12935(2) 0.06242(11) Uani 1 1 d . . . . . Cl2 Cl 0.60867(19) 0.62688(13) 0.07892(9) 0.0830(5) Uani 1 1 d . . . . . Cl1A Cl 0.6956(10) 0.4423(7) 0.0390(6) 0.136(4) Uani 0.5 1 d . U P A 1 N1 N 0.6779(3) 0.7742(2) 0.24092(16) 0.0317(7) Uani 1 1 d . . . . . C5 C 0.6693(4) 0.8456(3) 0.1982(2) 0.0321(8) Uani 1 1 d . . . . . C2 C 0.5600(4) 0.7297(3) 0.2243(2) 0.0324(9) Uani 1 1 d . . . . . C10 C 0.9572(4) 0.6483(3) 0.2653(2) 0.0369(9) Uani 1 1 d . . . . . C6 C 0.8874(4) 0.5713(3) 0.2815(2) 0.0391(10) Uani 1 1 d . . . . . C8 C 1.0274(4) 0.6216(3) 0.3719(2) 0.0436(11) Uani 1 1 d . . . . . C21 C 0.5214(5) 0.7369(4) 0.4242(3) 0.0597(15) Uani 1 1 d . . . . . H21A H 0.457458 0.754972 0.386340 0.090 Uiso 1 1 calc R U . . . H21B H 0.496453 0.763073 0.461612 0.090 Uiso 1 1 calc R U . . . H21C H 0.524024 0.669708 0.427536 0.090 Uiso 1 1 calc R U . . . C20 C 0.6806(5) 0.8523(3) 0.3850(2) 0.0406(10) Uani 1 1 d . . . . . C19 C 0.8157(5) 0.8724(3) 0.4028(2) 0.0407(10) Uani 1 1 d . . . . . C4 C 0.5492(4) 0.8448(3) 0.1556(2) 0.0348(9) Uani 1 1 d . . . . . C9 C 1.0432(4) 0.6805(3) 0.3209(3) 0.0417(10) Uani 1 1 d . . . . . C3 C 0.4783(4) 0.7700(3) 0.1732(2) 0.0345(9) Uani 1 1 d . . . . . C16 C 0.6553(4) 0.7727(3) 0.4194(2) 0.0386(10) Uani 1 1 d . . . . . C25 C 0.5785(6) 0.9115(4) 0.3425(3) 0.0662(17) Uani 1 1 d . . . . . H25A H 0.621095 0.951105 0.316276 0.099 Uiso 1 1 calc R U . . . H25B H 0.533688 0.949692 0.368573 0.099 Uiso 1 1 calc R U . . . H25C H 0.515121 0.871723 0.315297 0.099 Uiso 1 1 calc R U . . . C15 C 0.9534(6) 0.6812(4) 0.1984(3) 0.0655(16) Uani 1 1 d . . . . . H15A H 0.863195 0.681332 0.174530 0.098 Uiso 1 1 calc R U . . . H15B H 1.005644 0.639817 0.177921 0.098 Uiso 1 1 calc R U . . . H15C H 0.989080 0.743598 0.199554 0.098 Uiso 1 1 calc R U . . . C12 C 0.8880(7) 0.4760(4) 0.3844(4) 0.079(2) Uani 1 1 d . . . . . H12A H 0.896798 0.494073 0.428695 0.118 Uiso 1 1 calc R U . . . H12B H 0.943969 0.422858 0.381777 0.118 Uiso 1 1 calc R U . . . H12C H 0.797164 0.459816 0.366647 0.118 Uiso 1 1 calc R U . . . C11 C 0.8003(6) 0.5091(4) 0.2341(3) 0.0681(17) Uani 1 1 d . . . . . H11A H 0.753291 0.466753 0.256548 0.102 Uiso 1 1 calc R U . . . H11B H 0.853853 0.473864 0.210503 0.102 Uiso 1 1 calc R U . . . H11C H 0.737736 0.546729 0.204756 0.102 Uiso 1 1 calc R U . . . C14 C 1.1432(6) 0.7559(4) 0.3232(4) 0.077(2) Uani 1 1 d . . . . . H14A H 1.099221 0.813478 0.307850 0.115 Uiso 1 1 calc R U . . . H14B H 1.204091 0.738996 0.296406 0.115 Uiso 1 1 calc R U . . . H14C H 1.191228 0.764141 0.366765 0.115 Uiso 1 1 calc R U . . . C17 C 0.7756(4) 0.7429(3) 0.4576(2) 0.0376(9) Uani 1 1 d . . . . . C18 C 0.8735(4) 0.8049(3) 0.4483(2) 0.0378(9) Uani 1 1 d . . . . . C22 C 0.7895(6) 0.6653(4) 0.5068(3) 0.0611(14) Uani 1 1 d . . . . . H22A H 0.714590 0.623831 0.496208 0.092 Uiso 1 1 calc R U . . . H22B H 0.793156 0.691858 0.548735 0.092 Uiso 1 1 calc R U . . . H22C H 0.869767 0.630825 0.506896 0.092 Uiso 1 1 calc R U . . . C7 C 0.9287(5) 0.5559(3) 0.3473(3) 0.0423(11) Uani 1 1 d . . . . . C23 C 1.0094(5) 0.8120(5) 0.4906(3) 0.0678(17) Uani 1 1 d . . . . . H23A H 1.032118 0.753457 0.512501 0.102 Uiso 1 1 calc R U . . . H23B H 1.010134 0.861091 0.521652 0.102 Uiso 1 1 calc R U . . . H23C H 1.072986 0.826096 0.464633 0.102 Uiso 1 1 calc R U . . . C13 C 1.1185(7) 0.6154(5) 0.4359(3) 0.085(2) Uani 1 1 d . . . . . H13A H 1.161704 0.674785 0.446416 0.128 Uiso 1 1 calc R U . . . H13B H 1.184145 0.567844 0.434838 0.128 Uiso 1 1 calc R U . . . H13C H 1.068616 0.599510 0.467928 0.128 Uiso 1 1 calc R U . . . C24 C 0.8869(7) 0.9572(4) 0.3859(3) 0.074(2) Uani 1 1 d . . . . . H24A H 0.968789 0.938375 0.374701 0.111 Uiso 1 1 calc R U . . . H24B H 0.905388 0.998933 0.422147 0.111 Uiso 1 1 calc R U . . . H24C H 0.832096 0.988666 0.349885 0.111 Uiso 1 1 calc R U . . . C26 C 0.6949(11) 0.5595(5) 0.0367(5) 0.115(4) Uani 1 1 d . . . . . H26C H 0.664993 0.576963 -0.008214 0.138 Uiso 0.5 1 calc R U P A 1 H26D H 0.786930 0.579255 0.049094 0.138 Uiso 0.5 1 calc R U P A 1 H26A H 0.652682 0.563081 -0.008638 0.138 Uiso 0.5 1 calc R U P A -1 H26B H 0.783941 0.584874 0.041551 0.138 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7054(11) 0.4501(6) 0.0585(4) 0.091(2) 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 0.02678(10) 0.02746(10) 0.02694(10) -0.00026(7) 0.00130(7) 0.00352(6) I1 0.04224(16) 0.03619(15) 0.04335(18) 0.00257(12) 0.00708(13) -0.01141(11) I4 0.04215(17) 0.04479(18) 0.0546(2) 0.00728(14) 0.00849(14) -0.01223(12) I3 0.05504(19) 0.04999(18) 0.03712(17) 0.01188(13) 0.00618(14) 0.01707(13) I2 0.03497(17) 0.0605(2) 0.0796(3) -0.00053(18) -0.01597(16) -0.00690(13) Cl2 0.0970(13) 0.0846(11) 0.0678(11) 0.0075(9) 0.0178(9) 0.0303(9) Cl1A 0.091(4) 0.085(4) 0.237(12) -0.051(6) 0.049(6) -0.006(3) N1 0.0270(17) 0.0380(18) 0.0277(18) 0.0043(14) -0.0001(13) -0.0022(13) C5 0.031(2) 0.0314(19) 0.034(2) 0.0023(17) 0.0072(16) 0.0000(15) C2 0.028(2) 0.033(2) 0.035(2) 0.0018(17) 0.0049(17) -0.0021(15) C10 0.037(2) 0.038(2) 0.036(2) 0.0053(18) 0.0101(18) 0.0127(17) C6 0.036(2) 0.033(2) 0.047(3) -0.0131(19) 0.0061(19) 0.0053(16) C8 0.034(2) 0.052(3) 0.041(3) -0.011(2) 0.0000(19) 0.0154(19) C21 0.039(3) 0.079(4) 0.064(4) -0.027(3) 0.018(3) -0.004(2) C20 0.054(3) 0.034(2) 0.033(2) -0.0016(18) 0.007(2) 0.0179(19) C19 0.053(3) 0.031(2) 0.040(3) -0.0090(18) 0.013(2) -0.0033(18) C4 0.038(2) 0.034(2) 0.031(2) 0.0007(17) 0.0051(17) 0.0065(16) C9 0.026(2) 0.039(2) 0.061(3) -0.005(2) 0.008(2) 0.0014(16) C3 0.027(2) 0.038(2) 0.036(2) -0.0039(18) -0.0003(17) -0.0015(15) C16 0.035(2) 0.040(2) 0.041(3) -0.0046(19) 0.0087(19) 0.0030(17) C25 0.085(4) 0.058(3) 0.052(3) 0.003(3) 0.005(3) 0.044(3) C15 0.077(4) 0.073(4) 0.054(4) 0.013(3) 0.030(3) 0.024(3) C12 0.089(5) 0.054(3) 0.105(6) 0.033(4) 0.047(4) 0.026(3) C11 0.051(3) 0.065(4) 0.084(5) -0.036(3) 0.004(3) 0.007(2) C14 0.047(3) 0.065(4) 0.122(6) -0.017(4) 0.028(4) -0.013(3) C17 0.044(2) 0.040(2) 0.029(2) -0.0012(18) 0.0063(18) 0.0056(18) C18 0.036(2) 0.043(2) 0.033(2) -0.0095(19) 0.0033(18) 0.0007(17) C22 0.080(4) 0.061(3) 0.044(3) 0.015(3) 0.017(3) 0.011(3) C7 0.043(2) 0.034(2) 0.052(3) 0.011(2) 0.014(2) 0.0141(17) C23 0.048(3) 0.082(4) 0.064(4) -0.032(3) -0.010(3) 0.004(3) C13 0.073(4) 0.113(5) 0.056(4) -0.021(4) -0.018(3) 0.049(4) C24 0.121(6) 0.038(3) 0.073(4) -0.009(3) 0.041(4) -0.023(3) C26 0.205(10) 0.071(5) 0.101(6) 0.017(4) 0.103(7) 0.011(5) Cl1B 0.141(6) 0.068(4) 0.068(3) 0.014(3) 0.030(3) 0.041(4) 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 6 -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 61.80(8) . . ? N1 Dy1 C10 83.82(12) . . ? N1 Dy1 C6 92.28(13) . . ? N1 Dy1 C8 134.73(14) . . ? N1 Dy1 C20 81.31(13) . . ? N1 Dy1 C19 96.62(14) . . ? N1 Dy1 C9 107.45(14) . . ? N1 Dy1 C16 100.19(13) . . ? N1 Dy1 C17 130.08(13) . . ? N1 Dy1 C18 127.69(13) . . ? N1 Dy1 C7 122.72(14) . . ? C10 Dy1 I1 102.02(10) . . ? C10 Dy1 C6 30.76(14) . . ? C10 Dy1 C8 50.96(14) . . ? C10 Dy1 C16 175.39(13) . . ? C6 Dy1 I1 80.19(10) . . ? C6 Dy1 C8 50.97(14) . . ? C6 Dy1 C16 145.86(14) . . ? C8 Dy1 I1 122.89(11) . . ? C8 Dy1 C16 125.08(15) . . ? C20 Dy1 I1 90.30(11) . . ? C20 Dy1 C10 153.28(14) . . ? C20 Dy1 C6 170.27(14) . . ? C20 Dy1 C8 138.12(15) . . ? C20 Dy1 C16 30.89(14) . . ? C20 Dy1 C17 51.17(14) . . ? C19 Dy1 I1 121.24(11) . . ? C19 Dy1 C10 131.10(14) . . ? C19 Dy1 C6 158.50(14) . . ? C19 Dy1 C8 110.90(15) . . ? C19 Dy1 C20 30.94(15) . . ? C19 Dy1 C9 107.40(14) . . ? C19 Dy1 C16 51.06(14) . . ? C19 Dy1 C17 51.40(14) . . ? C19 Dy1 C18 31.29(14) . . ? C19 Dy1 C7 138.31(16) . . ? C9 Dy1 I1 130.70(10) . . ? C9 Dy1 C10 30.91(14) . . ? C9 Dy1 C6 51.14(14) . . ? C9 Dy1 C8 31.07(15) . . ? C9 Dy1 C20 137.85(15) . . ? C9 Dy1 C16 147.21(15) . . ? C9 Dy1 C17 117.68(15) . . ? C16 Dy1 I1 78.10(10) . . ? C17 Dy1 I1 99.67(10) . . ? C17 Dy1 C10 145.74(13) . . ? C17 Dy1 C6 132.25(14) . . ? C17 Dy1 C8 94.89(14) . . ? C17 Dy1 C16 30.70(14) . . ? C18 Dy1 I1 128.00(9) . . ? C18 Dy1 C10 128.37(14) . . ? C18 Dy1 C6 137.52(14) . . ? C18 Dy1 C8 87.08(14) . . ? C18 Dy1 C20 51.08(14) . . ? C18 Dy1 C9 97.58(14) . . ? C18 Dy1 C16 50.60(14) . . ? C18 Dy1 C17 30.66(14) . . ? C7 Dy1 I1 91.87(11) . . ? C7 Dy1 C10 50.98(14) . . ? C7 Dy1 C6 30.80(15) . . ? C7 Dy1 C8 31.02(15) . . ? C7 Dy1 C20 153.36(15) . . ? C7 Dy1 C9 51.39(14) . . ? C7 Dy1 C16 124.46(14) . . ? C7 Dy1 C17 102.37(15) . . ? C7 Dy1 C18 108.92(15) . . ? C2 I1 Dy1 68.32(11) . . ? C5 N1 Dy1 143.4(3) . . ? C2 N1 Dy1 111.3(3) . . ? C2 N1 C5 104.4(3) . . ? N1 C5 I4 122.0(3) . . ? N1 C5 C4 111.1(3) . . ? C4 C5 I4 126.9(3) . . ? N1 C2 I1 118.3(3) . . ? N1 C2 C3 112.6(4) . . ? C3 C2 I1 129.0(3) . . ? C6 C10 Dy1 74.8(2) . . ? C6 C10 C9 108.5(4) . . ? C6 C10 C15 124.8(5) . . ? C9 C10 Dy1 74.3(2) . . ? C9 C10 C15 126.1(5) . . ? C15 C10 Dy1 123.6(3) . . ? C10 C6 Dy1 74.4(2) . . ? C10 C6 C11 124.7(5) . . ? C11 C6 Dy1 124.7(3) . . ? C7 C6 Dy1 73.6(2) . . ? C7 C6 C10 107.9(4) . . ? C7 C6 C11 126.8(5) . . ? C9 C8 Dy1 74.0(2) . . ? C9 C8 C13 126.0(5) . . ? C7 C8 Dy1 73.5(2) . . ? C7 C8 C9 107.7(4) . . ? C7 C8 C13 124.9(5) . . ? C13 C8 Dy1 128.7(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 73.7(2) . . ? C19 C20 C16 108.0(4) . . ? C19 C20 C25 125.7(5) . . ? C16 C20 Dy1 75.7(2) . . ? C16 C20 C25 126.0(5) . . ? C25 C20 Dy1 121.8(3) . . ? C20 C19 Dy1 75.3(2) . . ? C20 C19 C18 107.5(4) . . ? C20 C19 C24 127.8(5) . . ? C18 C19 Dy1 74.8(2) . . ? C18 C19 C24 124.1(5) . . ? C24 C19 Dy1 122.7(3) . . ? C5 C4 I3 126.4(3) . . ? C5 C4 C3 106.4(4) . . ? C3 C4 I3 127.2(3) . . ? C10 C9 Dy1 74.8(2) . . ? C10 C9 C8 107.5(4) . . ? C10 C9 C14 125.3(5) . . ? C8 C9 Dy1 74.9(2) . . ? C8 C9 C14 126.8(5) . . ? C14 C9 Dy1 121.5(3) . . ? C2 C3 I2 126.4(3) . . ? C2 C3 C4 105.5(4) . . ? C4 C3 I2 128.0(3) . . ? C21 C16 Dy1 127.3(3) . . ? C20 C16 Dy1 73.5(2) . . ? C20 C16 C21 125.8(5) . . ? C17 C16 Dy1 73.7(2) . . ? C17 C16 C21 125.2(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 75.6(3) . . ? C16 C17 C22 124.7(4) . . ? C18 C17 Dy1 74.1(2) . . ? C18 C17 C16 107.9(4) . . ? C18 C17 C22 126.9(4) . . ? C22 C17 Dy1 123.0(3) . . ? C19 C18 Dy1 73.9(2) . . ? C19 C18 C23 124.9(5) . . ? C17 C18 Dy1 75.2(2) . . ? C17 C18 C19 108.6(4) . . ? C17 C18 C23 125.0(5) . . ? C23 C18 Dy1 127.8(3) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C6 C7 Dy1 75.6(2) . . ? C6 C7 C8 108.4(4) . . ? C6 C7 C12 126.2(5) . . ? C8 C7 Dy1 75.5(2) . . ? C8 C7 C12 125.0(5) . . ? C12 C7 Dy1 121.0(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 106.4 . . ? Cl2 C26 H26D 106.4 . . ? Cl2 C26 H26A 108.8 . . ? Cl2 C26 H26B 108.8 . . ? Cl1A C26 Cl2 123.6(6) . . ? Cl1A C26 H26C 106.4 . . ? Cl1A C26 H26D 106.4 . . ? Cl1A C26 H26A 94.5 . . ? Cl1A C26 H26B 111.7 . . ? H26C C26 H26D 106.5 . . ? H26C C26 H26A 13.9 . . ? H26C C26 H26B 96.2 . . ? H26D C26 H26A 117.6 . . ? H26D C26 H26B 10.4 . . ? H26A C26 H26B 107.7 . . ? Cl1B C26 Cl2 113.9(5) . . ? Cl1B C26 Cl1A 14.6(6) . . ? Cl1B C26 H26C 120.9 . . ? Cl1B C26 H26D 101.4 . . ? Cl1B C26 H26A 108.8 . . ? Cl1B C26 H26B 108.8 . . ? 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 3.2479(3) . ? Dy1 N1 2.383(3) . ? Dy1 C10 2.651(4) . ? Dy1 C6 2.656(4) . ? Dy1 C8 2.656(4) . ? Dy1 C20 2.646(4) . ? Dy1 C19 2.625(4) . ? Dy1 C9 2.644(4) . ? Dy1 C16 2.674(4) . ? Dy1 C17 2.651(4) . ? Dy1 C18 2.637(4) . ? Dy1 C7 2.631(4) . ? I1 C2 2.088(4) . ? I4 C5 2.079(4) . ? I3 C4 2.072(4) . ? I2 C3 2.061(4) . ? Cl2 C26 1.703(7) . ? Cl1A C26 1.688(13) . ? N1 C5 1.367(5) . ? N1 C2 1.363(5) . ? C5 C4 1.383(6) . ? C2 C3 1.366(6) . ? C10 C6 1.408(6) . ? C10 C9 1.411(7) . ? C10 C15 1.503(7) . ? C6 C11 1.505(7) . ? C6 C7 1.404(7) . ? C8 C9 1.419(7) . ? C8 C7 1.414(7) . ? C8 C13 1.498(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21 C16 1.507(7) . ? C20 C19 1.406(7) . ? C20 C16 1.417(6) . ? C20 C25 1.510(6) . ? C19 C18 1.419(6) . ? C19 C24 1.509(7) . ? C4 C3 1.400(6) . ? C9 C14 1.497(7) . ? C16 C17 1.410(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C12 C7 1.508(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C17 C18 1.398(6) . ? C17 C22 1.523(7) . ? C18 C23 1.514(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 Cl1B 1.641(10) . ? 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 12.7(6) . . . . ? Dy1 N1 C5 C4 -167.3(3) . . . . ? Dy1 N1 C2 I1 -5.8(4) . . . . ? Dy1 N1 C2 C3 171.6(3) . . . . ? Dy1 C10 C6 C11 121.8(4) . . . . ? Dy1 C10 C6 C7 -66.6(3) . . . . ? Dy1 C10 C9 C8 68.4(3) . . . . ? Dy1 C10 C9 C14 -118.2(5) . . . . ? Dy1 C6 C7 C8 -69.0(3) . . . . ? Dy1 C6 C7 C12 118.1(5) . . . . ? Dy1 C8 C9 C10 -68.3(3) . . . . ? Dy1 C8 C9 C14 118.3(5) . . . . ? Dy1 C8 C7 C6 69.1(3) . . . . ? Dy1 C8 C7 C12 -117.9(5) . . . . ? Dy1 C20 C19 C18 -68.5(3) . . . . ? Dy1 C20 C19 C24 120.2(5) . . . . ? Dy1 C20 C16 C21 -124.4(5) . . . . ? Dy1 C20 C16 C17 66.2(3) . . . . ? Dy1 C19 C18 C17 -67.8(3) . . . . ? Dy1 C19 C18 C23 125.3(5) . . . . ? Dy1 C16 C17 C18 67.7(3) . . . . ? Dy1 C16 C17 C22 -120.4(4) . . . . ? Dy1 C17 C18 C19 66.9(3) . . . . ? Dy1 C17 C18 C23 -126.1(5) . . . . ? I1 C2 C3 I2 -5.5(6) . . . . ? I1 C2 C3 C4 177.5(3) . . . . ? I4 C5 C4 I3 -0.6(6) . . . . ? I4 C5 C4 C3 -179.2(3) . . . . ? I3 C4 C3 I2 3.7(6) . . . . ? I3 C4 C3 C2 -179.4(3) . . . . ? N1 C5 C4 I3 179.4(3) . . . . ? N1 C5 C4 C3 0.9(5) . . . . ? N1 C2 C3 I2 177.6(3) . . . . ? N1 C2 C3 C4 0.5(5) . . . . ? C5 N1 C2 I1 -177.3(3) . . . . ? C5 N1 C2 C3 0.0(5) . . . . ? C5 C4 C3 I2 -177.8(3) . . . . ? C5 C4 C3 C2 -0.8(5) . . . . ? C2 N1 C5 I4 179.5(3) . . . . ? C2 N1 C5 C4 -0.6(5) . . . . ? C10 C6 C7 Dy1 67.1(3) . . . . ? C10 C6 C7 C8 -1.9(5) . . . . ? C10 C6 C7 C12 -174.8(4) . . . . ? C6 C10 C9 Dy1 -67.6(3) . . . . ? C6 C10 C9 C8 0.8(5) . . . . ? C6 C10 C9 C14 174.3(4) . . . . ? C21 C16 C17 Dy1 124.5(4) . . . . ? C21 C16 C17 C18 -167.8(4) . . . . ? C21 C16 C17 C22 4.0(7) . . . . ? C20 C19 C18 Dy1 68.9(3) . . . . ? C20 C19 C18 C17 1.1(5) . . . . ? C20 C19 C18 C23 -165.8(4) . . . . ? C20 C16 C17 Dy1 -66.0(3) . . . . ? C20 C16 C17 C18 1.7(5) . . . . ? C20 C16 C17 C22 173.6(4) . . . . ? C19 C20 C16 Dy1 -67.2(3) . . . . ? C19 C20 C16 C21 168.4(4) . . . . ? C19 C20 C16 C17 -1.0(5) . . . . ? C9 C10 C6 Dy1 67.2(3) . . . . ? C9 C10 C6 C11 -171.0(4) . . . . ? C9 C10 C6 C7 0.7(5) . . . . ? C9 C8 C7 Dy1 -66.7(3) . . . . ? C9 C8 C7 C6 2.3(5) . . . . ? C9 C8 C7 C12 175.4(4) . . . . ? C16 C20 C19 Dy1 68.5(3) . . . . ? C16 C20 C19 C18 0.0(5) . . . . ? C16 C20 C19 C24 -171.3(5) . . . . ? C16 C17 C18 Dy1 -68.7(3) . . . . ? C16 C17 C18 C19 -1.7(5) . . . . ? C16 C17 C18 C23 165.2(4) . . . . ? C25 C20 C19 Dy1 -117.8(5) . . . . ? C25 C20 C19 C18 173.7(4) . . . . ? C25 C20 C19 C24 2.4(8) . . . . ? C25 C20 C16 Dy1 119.1(5) . . . . ? C25 C20 C16 C21 -5.2(8) . . . . ? C25 C20 C16 C17 -174.7(4) . . . . ? C15 C10 C6 Dy1 -120.7(4) . . . . ? C15 C10 C6 C11 1.1(7) . . . . ? C15 C10 C6 C7 172.8(4) . . . . ? C15 C10 C9 Dy1 120.4(4) . . . . ? C15 C10 C9 C8 -171.2(4) . . . . ? C15 C10 C9 C14 2.3(7) . . . . ? C11 C6 C7 Dy1 -121.5(5) . . . . ? C11 C6 C7 C8 169.6(4) . . . . ? C11 C6 C7 C12 -3.4(7) . . . . ? C22 C17 C18 Dy1 119.7(5) . . . . ? C22 C17 C18 C19 -173.4(4) . . . . ? C22 C17 C18 C23 -6.5(7) . . . . ? C7 C8 C9 Dy1 66.4(3) . . . . ? C7 C8 C9 C10 -1.9(5) . . . . ? C7 C8 C9 C14 -175.3(5) . . . . ? C13 C8 C9 Dy1 -126.5(5) . . . . ? C13 C8 C9 C10 165.1(4) . . . . ? C13 C8 C9 C14 -8.2(8) . . . . ? C13 C8 C7 Dy1 126.0(5) . . . . ? C13 C8 C7 C6 -164.9(4) . . . . ? C13 C8 C7 C12 8.1(7) . . . . ? C24 C19 C18 Dy1 -119.5(5) . . . . ? C24 C19 C18 C17 172.7(4) . . . . ? C24 C19 C18 C23 5.8(7) . . . . ? 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 -0.9559 -1.1274 0.2057 -0.0783 -0.0142 0.0325 -1.0710 0.8842 0.0877 0.0038 0.0040 0.0859 0.9559 1.1274 -0.2057 0.0783 0.0142 -0.0325 1.0710 -0.8842 -0.0877 -0.0038 -0.0040 -0.0859 -0.0273 -0.0427 -0.9920 -0.0100 0.0322 0.0044 0.0273 0.0427 0.9920 0.0100 -0.0322 -0.0044 -1.0163 0.9696 2.0718 0.0239 -0.0605 0.0770 1.0163 -0.9696 -2.0718 -0.0239 0.0605 -0.0770 1.0983 -0.8414 0.9043 0.0063 -0.0363 -0.0903 -0.0029 1.0912 1.9251 0.0612 -0.0554 0.0178 2.1117 -0.7198 0.7576 0.0435 -0.0312 -0.1495 -0.1122 0.9203 -2.0431 0.0210 0.0736 0.0356 -1.0681 -0.2071 -1.8373 -0.0574 0.0594 0.0681 -0.9588 -0.0361 2.1308 -0.0172 -0.0696 0.0503 -6.8627 5.6499 -21.8353 -0.1415 0.7602 0.6341