#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572185.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_1572185 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 101.6536(19) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3478(2) _cell_length_b 14.3119(3) _cell_length_c 21.2778(4) _cell_measurement_reflns_used 20842 _cell_measurement_temperature 160.0(1) _cell_measurement_theta_max 31.9550 _cell_measurement_theta_min 2.8680 _cell_volume 3086.22(11) _computing_cell_refinement 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 160.0(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 0.842 _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 0.0367307000 _diffrn_orient_matrix_UB_12 0.0413795000 _diffrn_orient_matrix_UB_13 0.0091500000 _diffrn_orient_matrix_UB_21 0.0043251000 _diffrn_orient_matrix_UB_22 0.0078068000 _diffrn_orient_matrix_UB_23 -0.0324333000 _diffrn_orient_matrix_UB_31 -0.0593981000 _diffrn_orient_matrix_UB_32 0.0261490000 _diffrn_orient_matrix_UB_33 -0.0048048000 _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 0.0524 _diffrn_reflns_av_unetI/netI 0.0429 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.842 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _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 38312 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.842 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.685 _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 6.610 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.222 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 2.341 _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 1.225 _refine_diff_density_min -1.386 _refine_diff_density_rms 0.167 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8785 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0297 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.0692 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7276 _reflns_number_total 8785 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP160K _cod_database_code 1572185 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C25H32Cl2DyI4N _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.527 _shelx_estimated_absorpt_t_min 0.204 _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) 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_160_final.res created by SHELXL-2018/3 at 15:59:06 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 10.347838 14.311872 21.27783 90 101.6536 90 ZERR 4 0.000201 0.000268 0.000424 0 0.0019 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Dy I N UNIT 100 128 8 4 16 4 SIMU Cl1B Cl1A L.S. 10 0 0 PLAN 14 SIZE 0.111 0.275 0.353 TEMP -113.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.029200 FVAR 0.63710 DY1 4 0.804893 0.714121 0.339487 11.00000 0.01698 0.01706 = 0.01697 -0.00042 0.00069 0.00242 I1 5 0.525399 0.614028 0.282143 11.00000 0.02543 0.02182 = 0.02588 0.00128 0.00397 -0.00662 I4 5 0.820301 0.939696 0.200827 11.00000 0.02516 0.02628 = 0.03330 0.00421 0.00495 -0.00690 I3 5 0.482718 0.935734 0.081467 11.00000 0.03237 0.03023 = 0.02260 0.00673 0.00310 0.00996 I2 5 0.291879 0.719516 0.130955 11.00000 0.02123 0.03677 = 0.05063 0.00057 -0.01030 -0.00446 CL2 3 0.609735 0.628519 0.079622 11.00000 0.05418 0.05152 = 0.03900 0.00425 0.00930 0.01835 PART 1 CL1A 3 0.688634 0.444943 0.038040 10.50000 0.06585 0.04798 = 0.18012 -0.02847 0.00600 0.00008 PART 0 N1 6 0.677388 0.773081 0.241849 11.00000 0.01920 0.01997 = 0.01890 0.00170 0.00107 -0.00201 C5 1 0.667800 0.844784 0.198225 11.00000 0.01943 0.02059 = 0.02148 0.00085 0.00467 0.00063 C2 1 0.560396 0.727076 0.225723 11.00000 0.01872 0.02029 = 0.02357 -0.00099 0.00403 -0.00112 C10 1 0.958080 0.647976 0.263756 11.00000 0.02377 0.02119 = 0.02394 0.00020 0.00527 0.00625 C6 1 0.887195 0.569654 0.279552 11.00000 0.02058 0.01837 = 0.02998 -0.00600 0.00402 0.00342 C8 1 1.028834 0.619021 0.371037 11.00000 0.02303 0.03160 = 0.02718 -0.00105 0.00163 0.01361 C21 1 0.519509 0.739157 0.423932 11.00000 0.02098 0.04127 = 0.03826 -0.01099 0.00681 -0.00161 AFIX 137 H21A 2 0.456013 0.758660 0.385530 11.00000 -1.50000 H21B 2 0.493775 0.765451 0.462126 11.00000 -1.50000 H21C 2 0.520578 0.670809 0.426793 11.00000 -1.50000 AFIX 0 C20 1 0.685171 0.854041 0.386272 11.00000 0.03409 0.02257 = 0.02082 -0.00106 0.00389 0.01033 C19 1 0.821779 0.870988 0.404507 11.00000 0.03411 0.02115 = 0.02222 -0.00435 0.00802 -0.00011 C4 1 0.547251 0.843280 0.155982 11.00000 0.02063 0.02163 = 0.02225 0.00404 0.00232 0.00511 C9 1 1.044280 0.678987 0.319772 11.00000 0.01581 0.02520 = 0.04107 -0.00751 0.00478 0.00054 C3 1 0.476194 0.766704 0.174069 11.00000 0.02115 0.02305 = 0.02116 -0.00268 0.00056 0.00070 C16 1 0.655016 0.773817 0.419855 11.00000 0.02226 0.02467 = 0.02176 -0.00390 0.00363 0.00334 C25 1 0.585791 0.915205 0.343381 11.00000 0.04735 0.03603 = 0.03088 0.00446 0.00342 0.02301 AFIX 137 H25A 2 0.630979 0.953844 0.316474 11.00000 -1.50000 H25B 2 0.541918 0.955623 0.369821 11.00000 -1.50000 H25C 2 0.519942 0.875865 0.315997 11.00000 -1.50000 AFIX 0 C15 1 0.951624 0.683060 0.196520 11.00000 0.04845 0.03993 = 0.03298 0.00745 0.01947 0.01327 AFIX 137 H15A 2 0.859140 0.689749 0.174759 11.00000 -1.50000 H15B 2 0.995750 0.638440 0.172947 11.00000 -1.50000 H15C 2 0.995778 0.743838 0.198068 11.00000 -1.50000 AFIX 0 C12 1 0.887861 0.472470 0.383322 11.00000 0.05560 0.02971 = 0.06025 0.01996 0.02588 0.01389 AFIX 137 H12A 2 0.884548 0.493161 0.426873 11.00000 -1.50000 H12B 2 0.951343 0.421176 0.385473 11.00000 -1.50000 H12C 2 0.800259 0.450865 0.361709 11.00000 -1.50000 AFIX 0 C11 1 0.800280 0.508042 0.231658 11.00000 0.02947 0.04141 = 0.05276 -0.02434 0.00358 0.00014 AFIX 137 H11A 2 0.755935 0.462363 0.254342 11.00000 -1.50000 H11B 2 0.854119 0.475186 0.205716 11.00000 -1.50000 H11C 2 0.734062 0.546365 0.203657 11.00000 -1.50000 AFIX 0 C14 1 1.146129 0.755223 0.322158 11.00000 0.03076 0.03827 = 0.07756 -0.01354 0.01492 -0.00920 AFIX 137 H14A 2 1.108345 0.806741 0.294020 11.00000 -1.50000 H14B 2 1.223372 0.730217 0.307728 11.00000 -1.50000 H14C 2 1.172739 0.778168 0.366275 11.00000 -1.50000 AFIX 0 C17 1 0.774267 0.741104 0.459196 11.00000 0.02387 0.02361 = 0.01914 -0.00235 0.00506 0.00239 C18 1 0.877055 0.802133 0.450316 11.00000 0.02233 0.02795 = 0.01959 -0.00724 0.00184 0.00018 C22 1 0.785997 0.662656 0.507171 11.00000 0.04397 0.03197 = 0.02865 0.01032 0.00912 0.00516 AFIX 137 H22A 2 0.729945 0.610425 0.488463 11.00000 -1.50000 H22B 2 0.757676 0.684645 0.545869 11.00000 -1.50000 H22C 2 0.878005 0.641841 0.518406 11.00000 -1.50000 AFIX 0 C7 1 0.930043 0.552747 0.346282 11.00000 0.02806 0.02061 = 0.03087 0.00592 0.00810 0.01117 C23 1 1.012076 0.806864 0.492376 11.00000 0.02623 0.04501 = 0.03152 -0.01382 -0.00448 -0.00229 AFIX 137 H23A 2 1.032572 0.747096 0.514635 11.00000 -1.50000 H23B 2 1.014409 0.856927 0.524008 11.00000 -1.50000 H23C 2 1.077413 0.819657 0.465949 11.00000 -1.50000 AFIX 0 C13 1 1.119099 0.612232 0.435478 11.00000 0.05472 0.06542 = 0.03476 -0.01089 -0.00867 0.03632 AFIX 137 H13A 2 1.173179 0.668860 0.443445 11.00000 -1.50000 H13B 2 1.176556 0.557608 0.436384 11.00000 -1.50000 H13C 2 1.066606 0.605788 0.468759 11.00000 -1.50000 AFIX 0 C24 1 0.896912 0.955340 0.387980 11.00000 0.05863 0.02595 = 0.04180 -0.00519 0.01592 -0.01188 AFIX 137 H24A 2 0.979406 0.934820 0.376412 11.00000 -1.50000 H24B 2 0.916883 0.997135 0.425162 11.00000 -1.50000 H24C 2 0.843040 0.988620 0.351674 11.00000 -1.50000 AFIX 0 C26 1 0.700911 0.559014 0.038361 11.00000 0.17296 0.04651 = 0.09415 0.01917 0.10473 0.02021 PART 1 AFIX 23 H26C 2 0.680065 0.579553 -0.006992 10.50000 -1.20000 H26D 2 0.794948 0.574222 0.054952 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.665771 0.566376 -0.008220 10.50000 -1.20000 H26B 2 0.793243 0.581598 0.047275 10.50000 -1.20000 AFIX 0 CL1B 3 0.700666 0.443610 0.056997 10.50000 0.07175 0.03861 = 0.04879 0.01166 0.02278 0.01612 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0692, GooF = S = 1.059, Restrained GooF = 1.059 for all data REM R1 = 0.0297 for 7276 Fo > 4sig(Fo) and 0.0396 for all 8785 data REM 317 parameters refined using 6 restraints END WGHT 0.0292 0.0000 REM Highest difference peak 1.225, deepest hole -1.386, 1-sigma level 0.167 Q1 1 0.7776 0.4840 0.0562 11.00000 0.05 1.23 Q2 1 0.2940 0.7524 0.1593 11.00000 0.05 0.91 Q3 1 1.0809 0.6165 0.3997 11.00000 0.05 0.86 Q4 1 0.7242 0.6637 0.3387 11.00000 0.05 0.79 Q5 1 1.0979 0.7216 0.1960 11.00000 0.05 0.74 Q6 1 0.9048 0.9000 0.2004 11.00000 0.05 0.73 Q7 1 0.5444 0.9218 0.0414 11.00000 0.05 0.69 Q8 1 0.7336 0.5619 0.0549 11.00000 0.05 0.69 Q9 1 0.5025 0.8003 0.4385 11.00000 0.05 0.67 Q10 1 0.5591 0.5028 0.2198 11.00000 0.05 0.67 Q11 1 0.7293 0.7548 0.3421 11.00000 0.05 0.65 Q12 1 0.9024 0.7139 0.3794 11.00000 0.05 0.65 Q13 1 0.9120 0.9395 0.2374 11.00000 0.05 0.64 Q14 1 0.9181 0.9836 0.2013 11.00000 0.05 0.63 ; _shelx_res_checksum 11562 _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 2.520 _oxdiff_exptl_absorpt_empirical_full_min 0.673 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 0.80489(2) 0.71412(2) 0.33949(2) 0.01739(5) Uani 1 1 d . . . . . I1 I 0.52540(2) 0.61403(2) 0.28214(2) 0.02454(6) Uani 1 1 d . . . . . I4 I 0.82030(2) 0.93970(2) 0.20083(2) 0.02838(6) Uani 1 1 d . . . . . I3 I 0.48272(2) 0.93573(2) 0.08147(2) 0.02874(6) Uani 1 1 d . . . . . I2 I 0.29188(2) 0.71952(2) 0.13095(2) 0.03868(7) Uani 1 1 d . . . . . Cl2 Cl 0.60973(12) 0.62852(8) 0.07962(6) 0.0482(3) Uani 1 1 d . . . . . Cl1A Cl 0.6886(10) 0.4449(6) 0.0380(4) 0.101(3) Uani 0.5 1 d . U P A 1 N1 N 0.6774(3) 0.77308(18) 0.24185(14) 0.0197(6) Uani 1 1 d . . . . . C5 C 0.6678(3) 0.8448(2) 0.19823(17) 0.0204(6) Uani 1 1 d . . . . . C2 C 0.5604(3) 0.7271(2) 0.22572(17) 0.0209(7) Uani 1 1 d . . . . . C10 C 0.9581(3) 0.6480(2) 0.26376(17) 0.0229(7) Uani 1 1 d . . . . . C6 C 0.8872(3) 0.5697(2) 0.27955(18) 0.0231(7) Uani 1 1 d . . . . . C8 C 1.0288(4) 0.6190(2) 0.37104(18) 0.0278(8) Uani 1 1 d . . . . . C21 C 0.5195(4) 0.7392(3) 0.4239(2) 0.0334(9) Uani 1 1 d . . . . . H21A H 0.456013 0.758660 0.385530 0.050 Uiso 1 1 calc R U . . . H21B H 0.493775 0.765451 0.462126 0.050 Uiso 1 1 calc R U . . . H21C H 0.520578 0.670809 0.426793 0.050 Uiso 1 1 calc R U . . . C20 C 0.6852(4) 0.8540(2) 0.38627(17) 0.0261(7) Uani 1 1 d . . . . . C19 C 0.8218(4) 0.8710(2) 0.40451(17) 0.0255(7) Uani 1 1 d . . . . . C4 C 0.5473(3) 0.8433(2) 0.15598(17) 0.0218(7) Uani 1 1 d . . . . . C9 C 1.0443(3) 0.6790(2) 0.3198(2) 0.0275(8) Uani 1 1 d . . . . . C3 C 0.4762(3) 0.7667(2) 0.17407(17) 0.0223(7) Uani 1 1 d . . . . . C16 C 0.6550(3) 0.7738(2) 0.41986(17) 0.0230(7) Uani 1 1 d . . . . . C25 C 0.5858(4) 0.9152(3) 0.3434(2) 0.0387(10) Uani 1 1 d . . . . . H25A H 0.630979 0.953844 0.316474 0.058 Uiso 1 1 calc R U . . . H25B H 0.541918 0.955623 0.369821 0.058 Uiso 1 1 calc R U . . . H25C H 0.519942 0.875865 0.315997 0.058 Uiso 1 1 calc R U . . . C15 C 0.9516(5) 0.6831(3) 0.1965(2) 0.0389(10) Uani 1 1 d . . . . . H15A H 0.859140 0.689749 0.174759 0.058 Uiso 1 1 calc R U . . . H15B H 0.995750 0.638440 0.172947 0.058 Uiso 1 1 calc R U . . . H15C H 0.995778 0.743838 0.198068 0.058 Uiso 1 1 calc R U . . . C12 C 0.8879(5) 0.4725(3) 0.3833(3) 0.0465(12) Uani 1 1 d . . . . . H12A H 0.884548 0.493161 0.426873 0.070 Uiso 1 1 calc R U . . . H12B H 0.951343 0.421176 0.385473 0.070 Uiso 1 1 calc R U . . . H12C H 0.800259 0.450865 0.361709 0.070 Uiso 1 1 calc R U . . . C11 C 0.8003(4) 0.5080(3) 0.2317(2) 0.0419(11) Uani 1 1 d . . . . . H11A H 0.755935 0.462363 0.254342 0.063 Uiso 1 1 calc R U . . . H11B H 0.854119 0.475186 0.205716 0.063 Uiso 1 1 calc R U . . . H11C H 0.734062 0.546365 0.203657 0.063 Uiso 1 1 calc R U . . . C14 C 1.1461(4) 0.7552(3) 0.3222(3) 0.0483(12) Uani 1 1 d . . . . . H14A H 1.108345 0.806741 0.294020 0.072 Uiso 1 1 calc R U . . . H14B H 1.223372 0.730217 0.307728 0.072 Uiso 1 1 calc R U . . . H14C H 1.172739 0.778168 0.366275 0.072 Uiso 1 1 calc R U . . . C17 C 0.7743(3) 0.7411(2) 0.45920(16) 0.0221(7) Uani 1 1 d . . . . . C18 C 0.8771(3) 0.8021(2) 0.45032(17) 0.0236(7) Uani 1 1 d . . . . . C22 C 0.7860(4) 0.6627(3) 0.5072(2) 0.0346(9) Uani 1 1 d . . . . . H22A H 0.729945 0.610425 0.488463 0.052 Uiso 1 1 calc R U . . . H22B H 0.757676 0.684645 0.545869 0.052 Uiso 1 1 calc R U . . . H22C H 0.878005 0.641841 0.518406 0.052 Uiso 1 1 calc R U . . . C7 C 0.9300(4) 0.5527(2) 0.34628(19) 0.0262(7) Uani 1 1 d . . . . . C23 C 1.0121(4) 0.8069(3) 0.4924(2) 0.0357(9) Uani 1 1 d . . . . . H23A H 1.032572 0.747096 0.514635 0.054 Uiso 1 1 calc R U . . . H23B H 1.014409 0.856927 0.524008 0.054 Uiso 1 1 calc R U . . . H23C H 1.077413 0.819657 0.465949 0.054 Uiso 1 1 calc R U . . . C13 C 1.1191(5) 0.6122(4) 0.4355(2) 0.0541(14) Uani 1 1 d . . . . . H13A H 1.173179 0.668860 0.443445 0.081 Uiso 1 1 calc R U . . . H13B H 1.176556 0.557608 0.436384 0.081 Uiso 1 1 calc R U . . . H13C H 1.066606 0.605788 0.468759 0.081 Uiso 1 1 calc R U . . . C24 C 0.8969(5) 0.9553(3) 0.3880(2) 0.0413(10) Uani 1 1 d . . . . . H24A H 0.979406 0.934820 0.376412 0.062 Uiso 1 1 calc R U . . . H24B H 0.916883 0.997135 0.425162 0.062 Uiso 1 1 calc R U . . . H24C H 0.843040 0.988620 0.351674 0.062 Uiso 1 1 calc R U . . . C26 C 0.7009(9) 0.5590(4) 0.0384(4) 0.094(3) Uani 1 1 d . . . . . H26C H 0.680065 0.579553 -0.006992 0.112 Uiso 0.5 1 calc R U P A 1 H26D H 0.794948 0.574222 0.054952 0.112 Uiso 0.5 1 calc R U P A 1 H26A H 0.665771 0.566376 -0.008220 0.112 Uiso 0.5 1 calc R U P A -1 H26B H 0.793243 0.581598 0.047275 0.112 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7007(9) 0.4436(5) 0.0570(3) 0.0516(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 0.01698(8) 0.01706(8) 0.01697(8) -0.00042(5) 0.00069(6) 0.00242(5) I1 0.02543(12) 0.02182(11) 0.02588(12) 0.00128(8) 0.00397(9) -0.00662(8) I4 0.02516(12) 0.02628(12) 0.03330(14) 0.00421(9) 0.00495(10) -0.00690(8) I3 0.03237(13) 0.03023(13) 0.02260(12) 0.00673(9) 0.00310(9) 0.00996(9) I2 0.02123(13) 0.03677(15) 0.05063(18) 0.00057(12) -0.01030(11) -0.00446(9) Cl2 0.0542(7) 0.0515(6) 0.0390(6) 0.0043(5) 0.0093(5) 0.0183(5) Cl1A 0.066(3) 0.048(3) 0.180(8) -0.028(5) 0.006(5) 0.000(2) N1 0.0192(14) 0.0200(13) 0.0189(14) 0.0017(11) 0.0011(11) -0.0020(10) C5 0.0194(16) 0.0206(15) 0.0215(17) 0.0009(13) 0.0047(13) 0.0006(12) C2 0.0187(16) 0.0203(16) 0.0236(17) -0.0010(13) 0.0040(13) -0.0011(11) C10 0.0238(17) 0.0212(16) 0.0239(18) 0.0002(13) 0.0053(14) 0.0062(12) C6 0.0206(17) 0.0184(15) 0.0300(19) -0.0060(13) 0.0040(14) 0.0034(12) C8 0.0230(18) 0.0316(19) 0.0272(19) -0.0010(15) 0.0016(14) 0.0136(14) C21 0.0210(19) 0.041(2) 0.038(2) -0.0110(18) 0.0068(16) -0.0016(15) C20 0.034(2) 0.0226(17) 0.0208(17) -0.0011(14) 0.0039(14) 0.0103(14) C19 0.034(2) 0.0211(16) 0.0222(18) -0.0043(14) 0.0080(15) -0.0001(13) C4 0.0206(16) 0.0216(16) 0.0223(17) 0.0040(13) 0.0023(13) 0.0051(12) C9 0.0158(16) 0.0252(17) 0.041(2) -0.0075(16) 0.0048(15) 0.0005(12) C3 0.0212(17) 0.0231(16) 0.0212(17) -0.0027(13) 0.0006(13) 0.0007(12) C16 0.0223(17) 0.0247(17) 0.0218(17) -0.0039(13) 0.0036(13) 0.0033(12) C25 0.047(3) 0.036(2) 0.031(2) 0.0045(17) 0.0034(18) 0.0230(18) C15 0.048(3) 0.040(2) 0.033(2) 0.0074(18) 0.0195(19) 0.0133(19) C12 0.056(3) 0.030(2) 0.060(3) 0.020(2) 0.026(2) 0.0139(19) C11 0.029(2) 0.041(2) 0.053(3) -0.024(2) 0.0036(19) 0.0001(16) C14 0.031(2) 0.038(2) 0.078(4) -0.014(2) 0.015(2) -0.0092(18) C17 0.0239(17) 0.0236(16) 0.0191(16) -0.0024(13) 0.0051(13) 0.0024(13) C18 0.0223(17) 0.0279(17) 0.0196(17) -0.0072(14) 0.0018(13) 0.0002(13) C22 0.044(2) 0.032(2) 0.029(2) 0.0103(16) 0.0091(17) 0.0052(16) C7 0.0281(19) 0.0206(16) 0.031(2) 0.0059(14) 0.0081(15) 0.0112(13) C23 0.026(2) 0.045(2) 0.032(2) -0.0138(18) -0.0045(16) -0.0023(16) C13 0.055(3) 0.065(3) 0.035(3) -0.011(2) -0.009(2) 0.036(2) C24 0.059(3) 0.0260(19) 0.042(3) -0.0052(17) 0.016(2) -0.0119(18) C26 0.173(8) 0.047(3) 0.094(5) 0.019(3) 0.105(6) 0.020(4) Cl1B 0.072(3) 0.039(2) 0.0488(17) 0.0117(15) 0.0228(19) 0.016(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 -1 0 0.1241 -1 1 0 0.1231 1 1 0 0.1293 1 -1 0 0.1498 0 0 -1 0.0585 0 0 1 0.0528 -1 1 2 0.0993 1 -1 -2 0.1399 1 -1 1 0.1333 0 1 2 0.0924 2 -1 1 0.1448 0 1 -2 0.0988 -1 0 -2 0.1081 -1 0 2 0.1036 -6 7 -23 0.0941 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Dy1 I1 62.11(6) . . ? N1 Dy1 C10 83.70(10) . . ? N1 Dy1 C6 91.82(10) . . ? N1 Dy1 C8 134.79(11) . . ? N1 Dy1 C20 80.87(10) . . ? N1 Dy1 C19 97.07(10) . . ? N1 Dy1 C9 107.52(11) . . ? N1 Dy1 C16 98.88(10) . . ? N1 Dy1 C17 129.26(10) . . ? N1 Dy1 C18 128.06(10) . . ? N1 Dy1 C7 122.54(11) . . ? C10 Dy1 I1 102.19(8) . . ? C10 Dy1 C6 30.94(10) . . ? C10 Dy1 C8 51.12(11) . . ? C10 Dy1 C16 177.13(10) . . ? C10 Dy1 C17 146.67(11) . . ? C6 Dy1 I1 79.83(7) . . ? C6 Dy1 C16 147.13(11) . . ? C8 Dy1 I1 122.43(8) . . ? C8 Dy1 C6 51.28(11) . . ? C8 Dy1 C16 126.33(11) . . ? C8 Dy1 C17 95.69(11) . . ? C20 Dy1 I1 91.50(8) . . ? C20 Dy1 C10 151.54(11) . . ? C20 Dy1 C6 170.62(11) . . ? C20 Dy1 C8 137.94(12) . . ? C20 Dy1 C16 30.94(11) . . ? C20 Dy1 C17 51.35(11) . . ? C19 Dy1 I1 122.45(8) . . ? C19 Dy1 C10 129.88(11) . . ? C19 Dy1 C6 157.62(11) . . ? C19 Dy1 C8 110.10(12) . . ? C19 Dy1 C20 30.98(12) . . ? C19 Dy1 C9 106.36(11) . . ? C19 Dy1 C16 51.26(11) . . ? C19 Dy1 C17 51.58(11) . . ? C19 Dy1 C18 31.32(11) . . ? C19 Dy1 C7 137.78(12) . . ? C9 Dy1 I1 130.59(8) . . ? C9 Dy1 C10 30.85(11) . . ? C9 Dy1 C6 51.28(11) . . ? C9 Dy1 C8 31.15(12) . . ? C9 Dy1 C20 136.64(11) . . ? C9 Dy1 C16 147.86(12) . . ? C9 Dy1 C17 118.48(12) . . ? C9 Dy1 C18 97.31(11) . . ? C16 Dy1 I1 78.04(8) . . ? C17 Dy1 I1 98.92(7) . . ? C17 Dy1 C6 133.21(11) . . ? C17 Dy1 C16 30.98(10) . . ? C18 Dy1 I1 128.08(7) . . ? C18 Dy1 C10 128.02(11) . . ? C18 Dy1 C6 137.58(11) . . ? C18 Dy1 C8 86.78(11) . . ? C18 Dy1 C20 51.31(11) . . ? C18 Dy1 C16 51.13(11) . . ? C18 Dy1 C17 31.02(10) . . ? C7 Dy1 I1 91.41(9) . . ? C7 Dy1 C10 51.23(11) . . ? C7 Dy1 C6 31.11(12) . . ? C7 Dy1 C8 31.04(12) . . ? C7 Dy1 C20 154.42(11) . . ? C7 Dy1 C9 51.43(11) . . ? C7 Dy1 C16 125.97(11) . . ? C7 Dy1 C17 103.12(11) . . ? C7 Dy1 C18 108.73(11) . . ? C2 I1 Dy1 68.20(9) . . ? C5 N1 Dy1 143.8(2) . . ? C2 N1 Dy1 110.9(2) . . ? C2 N1 C5 104.6(3) . . ? N1 C5 I4 121.4(2) . . ? N1 C5 C4 111.1(3) . . ? C4 C5 I4 127.5(2) . . ? N1 C2 I1 118.6(2) . . ? N1 C2 C3 112.9(3) . . ? C3 C2 I1 128.4(2) . . ? C6 C10 Dy1 74.73(19) . . ? C6 C10 C15 124.3(4) . . ? C9 C10 Dy1 74.19(19) . . ? C9 C10 C6 108.6(3) . . ? C9 C10 C15 126.7(4) . . ? C15 C10 Dy1 122.8(2) . . ? C10 C6 Dy1 74.32(18) . . ? C10 C6 C11 124.9(4) . . ? C10 C6 C7 107.5(3) . . ? C11 C6 Dy1 125.2(2) . . ? C7 C6 Dy1 73.65(18) . . ? C7 C6 C11 127.0(3) . . ? C9 C8 Dy1 73.99(19) . . ? C9 C8 C13 126.5(4) . . ? C7 C8 Dy1 73.83(19) . . ? C7 C8 C9 107.7(3) . . ? C7 C8 C13 124.5(4) . . ? C13 C8 Dy1 128.0(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 73.42(19) . . ? C19 C20 C16 108.1(3) . . ? C19 C20 C25 126.1(3) . . ? C16 C20 Dy1 75.24(18) . . ? C16 C20 C25 125.5(4) . . ? C25 C20 Dy1 121.6(2) . . ? C20 C19 Dy1 75.6(2) . . ? C20 C19 C18 108.2(3) . . ? C20 C19 C24 127.3(4) . . ? C18 C19 Dy1 75.13(19) . . ? C18 C19 C24 123.8(4) . . ? C24 C19 Dy1 122.8(2) . . ? C5 C4 I3 126.7(2) . . ? C5 C4 C3 106.6(3) . . ? C3 C4 I3 126.7(3) . . ? C10 C9 Dy1 74.97(19) . . ? C10 C9 C8 108.0(3) . . ? C10 C9 C14 125.1(4) . . ? C8 C9 Dy1 74.87(19) . . ? C8 C9 C14 126.6(4) . . ? C14 C9 Dy1 121.8(2) . . ? C2 C3 I2 126.9(2) . . ? C2 C3 C4 104.8(3) . . ? C4 C3 I2 128.2(3) . . ? C21 C16 Dy1 126.8(2) . . ? C20 C16 Dy1 73.82(19) . . ? C20 C16 C21 126.7(3) . . ? C20 C16 C17 108.0(3) . . ? C17 C16 Dy1 74.02(18) . . ? C17 C16 C21 124.4(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 75.00(19) . . ? C16 C17 C22 125.8(3) . . ? C18 C17 Dy1 73.98(19) . . ? C18 C17 C16 107.7(3) . . ? C18 C17 C22 126.1(3) . . ? C22 C17 Dy1 122.2(2) . . ? C19 C18 Dy1 73.55(19) . . ? C19 C18 C23 125.1(3) . . ? C17 C18 Dy1 75.00(19) . . ? C17 C18 C19 108.0(3) . . ? C17 C18 C23 125.5(3) . . ? C23 C18 Dy1 127.9(2) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C6 C7 Dy1 75.25(18) . . ? C6 C7 C12 126.0(4) . . ? C8 C7 Dy1 75.13(19) . . ? C8 C7 C6 108.3(3) . . ? C8 C7 C12 125.4(4) . . ? C12 C7 Dy1 120.4(2) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Cl2 C26 H26C 106.9 . . ? Cl2 C26 H26D 106.9 . . ? Cl2 C26 H26A 108.6 . . ? Cl2 C26 H26B 108.6 . . ? Cl1A C26 Cl2 121.8(5) . . ? Cl1A C26 H26C 106.9 . . ? Cl1A C26 H26D 106.9 . . ? Cl1A C26 H26A 95.1 . . ? Cl1A C26 H26B 113.4 . . ? Cl1A C26 Cl1B 13.5(5) . . ? H26C C26 H26D 106.7 . . ? H26C C26 H26A 13.8 . . ? H26C C26 H26B 95.8 . . ? H26D C26 H26A 118.0 . . ? H26D C26 H26B 11.1 . . ? H26A C26 H26B 107.6 . . ? Cl1B C26 Cl2 114.5(4) . . ? Cl1B C26 H26C 120.4 . . ? Cl1B C26 H26D 100.3 . . ? Cl1B C26 H26A 108.6 . . ? Cl1B C26 H26B 108.6 . . ? 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 3.2373(3) . ? Dy1 N1 2.379(3) . ? Dy1 C10 2.653(3) . ? Dy1 C6 2.658(3) . ? Dy1 C8 2.654(3) . ? Dy1 C20 2.652(3) . ? Dy1 C19 2.624(3) . ? Dy1 C9 2.643(3) . ? Dy1 C16 2.670(3) . ? Dy1 C17 2.658(3) . ? Dy1 C18 2.645(3) . ? Dy1 C7 2.638(3) . ? I1 C2 2.089(3) . ? I4 C5 2.074(3) . ? I3 C4 2.070(3) . ? I2 C3 2.056(3) . ? Cl2 C26 1.728(5) . ? Cl1A C26 1.637(11) . ? N1 C5 1.374(4) . ? N1 C2 1.360(4) . ? C5 C4 1.383(5) . ? C2 C3 1.379(5) . ? C10 C6 1.417(5) . ? C10 C9 1.408(5) . ? C10 C15 1.505(5) . ? C6 C11 1.502(5) . ? C6 C7 1.420(5) . ? C8 C9 1.422(5) . ? C8 C7 1.416(5) . ? C8 C13 1.498(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C16 1.506(5) . ? C20 C19 1.409(5) . ? C20 C16 1.420(5) . ? C20 C25 1.509(5) . ? C19 C18 1.422(5) . ? C19 C24 1.515(5) . ? C4 C3 1.416(5) . ? C9 C14 1.511(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 1.507(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C17 C18 1.418(5) . ? C17 C22 1.506(5) . ? C18 C23 1.501(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 H26C 0.9900 . ? C26 H26D 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 Cl1B 1.699(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 11.1(5) . . . . ? Dy1 N1 C5 C4 -168.2(3) . . . . ? Dy1 N1 C2 I1 -4.7(3) . . . . ? Dy1 N1 C2 C3 172.1(2) . . . . ? Dy1 C10 C6 C11 122.3(3) . . . . ? Dy1 C10 C6 C7 -66.7(2) . . . . ? Dy1 C10 C9 C8 68.2(2) . . . . ? Dy1 C10 C9 C14 -118.6(3) . . . . ? Dy1 C6 C7 C8 -68.5(2) . . . . ? Dy1 C6 C7 C12 117.0(3) . . . . ? Dy1 C8 C9 C10 -68.3(2) . . . . ? Dy1 C8 C9 C14 118.6(4) . . . . ? Dy1 C8 C7 C6 68.6(2) . . . . ? Dy1 C8 C7 C12 -116.9(3) . . . . ? Dy1 C20 C19 C18 -68.7(2) . . . . ? Dy1 C20 C19 C24 120.5(4) . . . . ? Dy1 C20 C16 C21 -124.2(4) . . . . ? Dy1 C20 C16 C17 66.7(2) . . . . ? Dy1 C19 C18 C17 -67.7(2) . . . . ? Dy1 C19 C18 C23 125.1(3) . . . . ? Dy1 C16 C17 C18 67.3(2) . . . . ? Dy1 C16 C17 C22 -119.1(3) . . . . ? Dy1 C17 C18 C19 66.7(2) . . . . ? Dy1 C17 C18 C23 -126.2(3) . . . . ? I1 C2 C3 I2 -5.5(5) . . . . ? I1 C2 C3 C4 177.2(2) . . . . ? I4 C5 C4 I3 0.5(5) . . . . ? I4 C5 C4 C3 -179.0(2) . . . . ? I3 C4 C3 I2 2.7(5) . . . . ? I3 C4 C3 C2 179.9(2) . . . . ? N1 C5 C4 I3 179.8(2) . . . . ? N1 C5 C4 C3 0.4(4) . . . . ? N1 C2 C3 I2 178.0(2) . . . . ? N1 C2 C3 C4 0.7(4) . . . . ? C5 N1 C2 I1 -177.4(2) . . . . ? C5 N1 C2 C3 -0.5(4) . . . . ? C5 C4 C3 I2 -177.9(2) . . . . ? C5 C4 C3 C2 -0.6(4) . . . . ? C2 N1 C5 I4 179.4(2) . . . . ? C2 N1 C5 C4 0.1(4) . . . . ? C10 C6 C7 Dy1 67.2(2) . . . . ? C10 C6 C7 C8 -1.3(4) . . . . ? C10 C6 C7 C12 -175.8(3) . . . . ? C6 C10 C9 Dy1 -67.4(2) . . . . ? C6 C10 C9 C8 0.8(4) . . . . ? C6 C10 C9 C14 174.0(3) . . . . ? C21 C16 C17 Dy1 124.0(3) . . . . ? C21 C16 C17 C18 -168.6(3) . . . . ? C21 C16 C17 C22 4.9(5) . . . . ? C20 C19 C18 Dy1 69.0(2) . . . . ? C20 C19 C18 C17 1.4(4) . . . . ? C20 C19 C18 C23 -165.8(3) . . . . ? C20 C16 C17 Dy1 -66.5(2) . . . . ? C20 C16 C17 C18 0.8(4) . . . . ? C20 C16 C17 C22 174.3(3) . . . . ? C19 C20 C16 Dy1 -66.6(2) . . . . ? C19 C20 C16 C21 169.2(3) . . . . ? C19 C20 C16 C17 0.0(4) . . . . ? C9 C10 C6 Dy1 67.1(2) . . . . ? C9 C10 C6 C11 -170.6(3) . . . . ? C9 C10 C6 C7 0.3(4) . . . . ? C9 C8 C7 Dy1 -66.8(2) . . . . ? C9 C8 C7 C6 1.8(4) . . . . ? C9 C8 C7 C12 176.3(3) . . . . ? C16 C20 C19 Dy1 67.8(2) . . . . ? C16 C20 C19 C18 -0.9(4) . . . . ? C16 C20 C19 C24 -171.6(3) . . . . ? C16 C17 C18 Dy1 -68.0(2) . . . . ? C16 C17 C18 C19 -1.3(4) . . . . ? C16 C17 C18 C23 165.8(3) . . . . ? C25 C20 C19 Dy1 -117.4(4) . . . . ? C25 C20 C19 C18 173.9(3) . . . . ? C25 C20 C19 C24 3.2(6) . . . . ? C25 C20 C16 Dy1 118.5(4) . . . . ? C25 C20 C16 C21 -5.7(6) . . . . ? C25 C20 C16 C17 -174.8(3) . . . . ? C15 C10 C6 Dy1 -119.5(3) . . . . ? C15 C10 C6 C11 2.8(5) . . . . ? C15 C10 C6 C7 173.7(3) . . . . ? C15 C10 C9 Dy1 119.4(3) . . . . ? C15 C10 C9 C8 -172.4(3) . . . . ? C15 C10 C9 C14 0.8(6) . . . . ? C11 C6 C7 Dy1 -122.1(3) . . . . ? C11 C6 C7 C8 169.4(3) . . . . ? C11 C6 C7 C12 -5.0(6) . . . . ? C22 C17 C18 Dy1 118.4(3) . . . . ? C22 C17 C18 C19 -174.8(3) . . . . ? C22 C17 C18 C23 -7.7(5) . . . . ? C7 C8 C9 Dy1 66.7(2) . . . . ? C7 C8 C9 C10 -1.6(4) . . . . ? C7 C8 C9 C14 -174.7(3) . . . . ? C13 C8 C9 Dy1 -125.8(4) . . . . ? C13 C8 C9 C10 166.0(3) . . . . ? C13 C8 C9 C14 -7.1(6) . . . . ? C13 C8 C7 Dy1 125.4(4) . . . . ? C13 C8 C7 C6 -166.1(3) . . . . ? C13 C8 C7 C12 8.4(6) . . . . ? C24 C19 C18 Dy1 -119.8(3) . . . . ? C24 C19 C18 C17 172.5(3) . . . . ? C24 C19 C18 C23 5.3(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 -0.9999 -1.0185 0.0581 -0.0783 -0.0142 0.0325 -1.0078 0.9904 -0.0201 0.0038 0.0040 0.0859 0.9999 1.0185 -0.0581 0.0783 0.0142 -0.0325 1.0078 -0.9904 0.0201 -0.0038 -0.0040 -0.0859 -0.0026 -0.0196 -0.9993 -0.0100 0.0322 0.0044 0.0026 0.0196 0.9993 0.0100 -0.0322 -0.0044 -1.0026 1.0296 1.9786 0.0239 -0.0605 0.0770 1.0026 -1.0296 -1.9786 -0.0239 0.0605 -0.0770 1.0104 -0.9709 1.0194 0.0063 -0.0363 -0.0903 0.0012 1.0436 1.9596 0.0612 -0.0554 0.0178 2.0143 -0.9569 1.0004 0.0435 -0.0312 -0.1495 -0.0091 0.9653 -2.0377 0.0210 0.0736 0.0356 -1.0090 -0.0531 -1.9796 -0.0574 0.0594 0.0681 -0.9987 0.0251 2.0177 -0.0172 -0.0696 0.0503 -5.8635 6.7791 -22.5891 -0.1415 0.7602 0.6341