#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572183.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_1572183 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 101.766(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3538(2) _cell_length_b 14.3266(3) _cell_length_c 21.3096(5) _cell_measurement_reflns_used 19818 _cell_measurement_temperature 180.0(1) _cell_measurement_theta_max 31.4470 _cell_measurement_theta_min 2.8380 _cell_volume 3094.54(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 180.0(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 0.834 _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 0.0370595000 _diffrn_orient_matrix_UB_12 0.0412000000 _diffrn_orient_matrix_UB_13 0.0091105000 _diffrn_orient_matrix_UB_21 0.0036960000 _diffrn_orient_matrix_UB_22 0.0079347000 _diffrn_orient_matrix_UB_23 -0.0324520000 _diffrn_orient_matrix_UB_31 -0.0592259000 _diffrn_orient_matrix_UB_32 0.0262772000 _diffrn_orient_matrix_UB_33 -0.0044902000 _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 0.0541 _diffrn_reflns_av_unetI/netI 0.0453 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.834 _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 38434 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.834 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.780 _diffrn_reflns_theta_min 2.461 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.593 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.228 _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 2.334 _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 1.119 _refine_diff_density_min -1.444 _refine_diff_density_rms 0.169 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8816 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0316 _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^)+(0.0326P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.0756 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7104 _reflns_number_total 8816 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP180K _cod_original_cell_volume 3094.51(13) _cod_database_code 1572183 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C25H32Cl2DyI4N _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.528 _shelx_estimated_absorpt_t_min 0.204 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Cl1B \\sim Cl1A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 3. Others Fixed Sof: Cl1A(0.5) 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_180_final.res created by SHELXL-2018/3 at 16:17:38 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 10.353756 14.326588 21.309553 90 101.7664 90 ZERR 4 0.000248 0.00033 0.000529 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. 20 0 0 PLAN 16 SIZE 0.111 0.275 0.353 TEMP -93.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.032600 FVAR 0.61832 DY1 4 0.804586 0.714568 0.339369 11.00000 0.01904 0.01919 = 0.01911 -0.00041 0.00080 0.00265 I1 5 0.524949 0.614878 0.281601 11.00000 0.02879 0.02505 = 0.02953 0.00142 0.00470 -0.00778 I4 5 0.820789 0.939686 0.200643 11.00000 0.02869 0.02998 = 0.03796 0.00487 0.00554 -0.00798 I3 5 0.483581 0.936463 0.081592 11.00000 0.03720 0.03433 = 0.02573 0.00786 0.00369 0.01139 I2 5 0.292237 0.720648 0.130556 11.00000 0.02388 0.04197 = 0.05708 0.00066 -0.01168 -0.00505 CL2 3 0.609521 0.628025 0.079491 11.00000 0.06312 0.05782 = 0.04459 0.00568 0.01112 0.02061 PART 1 CL1A 3 0.690830 0.444930 0.037809 10.50000 0.07773 0.05491 = 0.20424 -0.02965 0.01384 0.00018 PART 0 N1 6 0.677775 0.773512 0.241987 11.00000 0.02065 0.02447 = 0.01951 0.00097 0.00087 -0.00264 C5 1 0.668207 0.844980 0.198272 11.00000 0.02168 0.02297 = 0.02232 0.00082 0.00275 -0.00020 C2 1 0.560354 0.727809 0.225324 11.00000 0.02198 0.02067 = 0.02742 -0.00009 0.00587 -0.00382 C10 1 0.957702 0.648067 0.263768 11.00000 0.02568 0.02267 = 0.02829 0.00150 0.00779 0.00644 C6 1 0.887664 0.569965 0.280170 11.00000 0.02530 0.02009 = 0.03475 -0.00515 0.00347 0.00473 C8 1 1.028323 0.619633 0.370986 11.00000 0.02502 0.03452 = 0.03212 -0.00422 -0.00003 0.01424 C21 1 0.518938 0.738948 0.424064 11.00000 0.02474 0.05533 = 0.04027 -0.01360 0.00764 0.00058 AFIX 137 H21A 2 0.454651 0.759252 0.386174 11.00000 -1.50000 H21B 2 0.494468 0.764400 0.462708 11.00000 -1.50000 H21C 2 0.519768 0.670616 0.426234 11.00000 -1.50000 AFIX 0 C20 1 0.683851 0.853527 0.385747 11.00000 0.04156 0.02312 = 0.02337 -0.00428 0.00510 0.01152 C19 1 0.820417 0.871297 0.404358 11.00000 0.03510 0.02375 = 0.03034 -0.00604 0.00917 -0.00166 C4 1 0.548432 0.843916 0.155895 11.00000 0.02433 0.02581 = 0.02477 0.00301 0.00391 0.00428 C9 1 1.043674 0.679577 0.319901 11.00000 0.01672 0.02669 = 0.04416 -0.00562 0.00533 0.00039 C3 1 0.476923 0.767754 0.173648 11.00000 0.02051 0.02536 = 0.02387 -0.00479 -0.00015 0.00015 C16 1 0.654896 0.773853 0.419542 11.00000 0.02503 0.02522 = 0.02360 -0.00323 0.00604 0.00371 C25 1 0.583247 0.914045 0.343149 11.00000 0.05654 0.04531 = 0.03236 0.00529 0.00307 0.02849 AFIX 137 H25A 2 0.626701 0.950604 0.314536 11.00000 -1.50000 H25B 2 0.542660 0.956367 0.369667 11.00000 -1.50000 H25C 2 0.515017 0.874484 0.317568 11.00000 -1.50000 AFIX 0 C15 1 0.952582 0.682508 0.197325 11.00000 0.05407 0.04961 = 0.03435 0.00906 0.01795 0.01679 AFIX 137 H15A 2 0.860455 0.686558 0.174514 11.00000 -1.50000 H15B 2 1.000536 0.639194 0.174750 11.00000 -1.50000 H15C 2 0.993389 0.744422 0.199011 11.00000 -1.50000 AFIX 0 C12 1 0.888339 0.473333 0.383551 11.00000 0.05957 0.03454 = 0.06975 0.02253 0.02968 0.01671 AFIX 137 H12A 2 0.896445 0.491441 0.428535 11.00000 -1.50000 H12B 2 0.944888 0.419235 0.380872 11.00000 -1.50000 H12C 2 0.796388 0.457147 0.365299 11.00000 -1.50000 AFIX 0 C11 1 0.801169 0.508483 0.232314 11.00000 0.03306 0.04273 = 0.05573 -0.02329 0.00233 0.00183 AFIX 137 H11A 2 0.757327 0.462509 0.254891 11.00000 -1.50000 H11B 2 0.855057 0.476068 0.206300 11.00000 -1.50000 H11C 2 0.734554 0.546663 0.204452 11.00000 -1.50000 AFIX 0 C14 1 1.145771 0.755334 0.323015 11.00000 0.03205 0.04421 = 0.08210 -0.01677 0.01716 -0.01255 AFIX 137 H14A 2 1.116120 0.800559 0.288588 11.00000 -1.50000 H14B 2 1.229600 0.727700 0.317910 11.00000 -1.50000 H14C 2 1.157985 0.787006 0.364571 11.00000 -1.50000 AFIX 0 C17 1 0.774503 0.741897 0.458734 11.00000 0.03017 0.02756 = 0.02087 -0.00095 0.00449 0.00119 C18 1 0.876893 0.802539 0.450181 11.00000 0.02919 0.02959 = 0.02126 -0.00860 0.00396 -0.00117 C22 1 0.785631 0.663716 0.506673 11.00000 0.05122 0.03643 = 0.03488 0.01274 0.01004 0.00965 AFIX 137 H22A 2 0.731550 0.610886 0.487469 11.00000 -1.50000 H22B 2 0.754628 0.685313 0.544670 11.00000 -1.50000 H22C 2 0.877962 0.644022 0.519106 11.00000 -1.50000 AFIX 0 C7 1 0.930151 0.553259 0.346708 11.00000 0.03122 0.01876 = 0.03772 0.00548 0.01160 0.01023 C23 1 1.011329 0.808020 0.492118 11.00000 0.03050 0.05240 = 0.04152 -0.02021 -0.00195 -0.00182 AFIX 137 H23A 2 1.034970 0.747156 0.512182 11.00000 -1.50000 H23B 2 1.011487 0.855150 0.525465 11.00000 -1.50000 H23C 2 1.075657 0.825350 0.466197 11.00000 -1.50000 AFIX 0 C13 1 1.119925 0.613030 0.435213 11.00000 0.05135 0.07072 = 0.03983 -0.01253 -0.01225 0.03476 AFIX 137 H13A 2 1.167703 0.672065 0.444762 11.00000 -1.50000 H13B 2 1.183085 0.562269 0.434564 11.00000 -1.50000 H13C 2 1.068802 0.600444 0.468254 11.00000 -1.50000 AFIX 0 C24 1 0.894613 0.955911 0.387247 11.00000 0.07018 0.03170 = 0.04652 -0.00502 0.02424 -0.01221 AFIX 137 H24A 2 0.972325 0.935283 0.371362 11.00000 -1.50000 H24B 2 0.922632 0.994823 0.425420 11.00000 -1.50000 H24C 2 0.836756 0.992224 0.353917 11.00000 -1.50000 AFIX 0 C26 1 0.698767 0.559522 0.037872 11.00000 0.18967 0.05436 = 0.09385 0.01404 0.10414 0.01892 PART 1 AFIX 23 H26C 2 0.675077 0.579573 -0.007483 10.50000 -1.20000 H26D 2 0.792675 0.576183 0.053305 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.661630 0.566392 -0.008528 10.50000 -1.20000 H26B 2 0.790702 0.582791 0.045846 10.50000 -1.20000 AFIX 0 CL1B 3 0.701200 0.444149 0.056969 10.50000 0.07997 0.04426 = 0.05369 0.01180 0.02606 0.01945 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0756, GooF = S = 1.057, Restrained GooF = 1.057 for all data REM R1 = 0.0316 for 7104 Fo > 4sig(Fo) and 0.0438 for all 8816 data REM 317 parameters refined using 6 restraints END WGHT 0.0326 0.0000 REM Highest difference peak 1.119, deepest hole -1.444, 1-sigma level 0.169 Q1 1 0.7804 0.4812 0.0549 11.00000 0.05 1.05 Q2 1 0.7205 0.7196 0.3398 11.00000 0.05 0.96 Q3 1 0.2896 0.7431 0.1602 11.00000 0.05 0.88 Q4 1 0.8783 0.7570 0.3404 11.00000 0.05 0.80 Q5 1 0.3935 0.8967 0.0801 11.00000 0.05 0.72 Q6 1 1.0970 0.7200 0.1931 11.00000 0.05 0.70 Q7 1 0.5518 0.9599 0.0814 11.00000 0.05 0.68 Q8 1 0.7326 0.5617 0.0545 11.00000 0.05 0.67 Q9 1 0.7263 0.7191 0.2625 11.00000 0.05 0.66 Q10 1 0.3363 0.9419 0.1007 11.00000 0.05 0.66 Q11 1 0.5268 0.5986 0.0603 11.00000 0.05 0.66 Q12 1 1.1506 0.7187 0.4603 11.00000 0.05 0.64 Q13 1 0.6983 0.6406 0.3412 11.00000 0.05 0.64 Q14 1 0.9018 0.7149 0.3815 11.00000 0.05 0.64 Q15 1 0.4126 0.9751 0.0798 11.00000 0.05 0.63 Q16 1 1.0905 0.6158 0.3973 11.00000 0.05 0.63 ; _shelx_res_checksum 26845 _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 2.738 _oxdiff_exptl_absorpt_empirical_full_min 0.638 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 0.80459(2) 0.71457(2) 0.33937(2) 0.01955(5) Uani 1 1 d . . . . . I1 I 0.52495(2) 0.61488(2) 0.28160(2) 0.02797(7) Uani 1 1 d . . . . . I4 I 0.82079(3) 0.93969(2) 0.20064(2) 0.03239(7) Uani 1 1 d . . . . . I3 I 0.48358(3) 0.93646(2) 0.08159(2) 0.03281(7) Uani 1 1 d . . . . . I2 I 0.29224(3) 0.72065(2) 0.13056(2) 0.04380(9) Uani 1 1 d . . . . . Cl2 Cl 0.60952(14) 0.62803(9) 0.07949(7) 0.0552(3) Uani 1 1 d . . . . . Cl1A Cl 0.6908(12) 0.4449(7) 0.0378(5) 0.114(3) Uani 0.5 1 d . U P A 1 N1 N 0.6778(3) 0.7735(2) 0.24199(15) 0.0220(6) Uani 1 1 d . . . . . C5 C 0.6682(3) 0.8450(2) 0.19827(18) 0.0226(7) Uani 1 1 d . . . . . C2 C 0.5604(3) 0.7278(2) 0.22532(18) 0.0232(7) Uani 1 1 d . . . . . C10 C 0.9577(4) 0.6481(2) 0.26377(19) 0.0252(8) Uani 1 1 d . . . . . C6 C 0.8877(4) 0.5700(2) 0.2802(2) 0.0271(8) Uani 1 1 d . . . . . C8 C 1.0283(4) 0.6196(3) 0.3710(2) 0.0314(9) Uani 1 1 d . . . . . C21 C 0.5189(4) 0.7389(3) 0.4241(2) 0.0400(10) Uani 1 1 d . . . . . H21A H 0.454651 0.759252 0.386174 0.060 Uiso 1 1 calc R U . . . H21B H 0.494468 0.764400 0.462708 0.060 Uiso 1 1 calc R U . . . H21C H 0.519768 0.670616 0.426234 0.060 Uiso 1 1 calc R U . . . C20 C 0.6839(4) 0.8535(3) 0.38575(19) 0.0296(8) Uani 1 1 d . . . . . C19 C 0.8204(4) 0.8713(3) 0.4044(2) 0.0294(8) Uani 1 1 d . . . . . C4 C 0.5484(4) 0.8439(3) 0.15590(18) 0.0251(7) Uani 1 1 d . . . . . C9 C 1.0437(3) 0.6796(3) 0.3199(2) 0.0293(8) Uani 1 1 d . . . . . C3 C 0.4769(3) 0.7678(2) 0.17365(18) 0.0239(7) Uani 1 1 d . . . . . C16 C 0.6549(4) 0.7739(2) 0.41954(18) 0.0245(7) Uani 1 1 d . . . . . C25 C 0.5832(5) 0.9140(3) 0.3431(2) 0.0456(12) Uani 1 1 d . . . . . H25A H 0.626701 0.950604 0.314536 0.068 Uiso 1 1 calc R U . . . H25B H 0.542660 0.956367 0.369667 0.068 Uiso 1 1 calc R U . . . H25C H 0.515017 0.874484 0.317568 0.068 Uiso 1 1 calc R U . . . C15 C 0.9526(5) 0.6825(3) 0.1973(2) 0.0447(11) Uani 1 1 d . . . . . H15A H 0.860455 0.686558 0.174514 0.067 Uiso 1 1 calc R U . . . H15B H 1.000536 0.639194 0.174750 0.067 Uiso 1 1 calc R U . . . H15C H 0.993389 0.744422 0.199011 0.067 Uiso 1 1 calc R U . . . C12 C 0.8883(5) 0.4733(3) 0.3836(3) 0.0523(14) Uani 1 1 d . . . . . H12A H 0.896445 0.491441 0.428535 0.078 Uiso 1 1 calc R U . . . H12B H 0.944888 0.419235 0.380872 0.078 Uiso 1 1 calc R U . . . H12C H 0.796388 0.457147 0.365299 0.078 Uiso 1 1 calc R U . . . C11 C 0.8012(4) 0.5085(3) 0.2323(3) 0.0448(12) Uani 1 1 d . . . . . H11A H 0.757327 0.462509 0.254891 0.067 Uiso 1 1 calc R U . . . H11B H 0.855057 0.476068 0.206300 0.067 Uiso 1 1 calc R U . . . H11C H 0.734554 0.546663 0.204452 0.067 Uiso 1 1 calc R U . . . C14 C 1.1458(5) 0.7553(3) 0.3230(3) 0.0520(14) Uani 1 1 d . . . . . H14A H 1.116120 0.800559 0.288588 0.078 Uiso 1 1 calc R U . . . H14B H 1.229600 0.727700 0.317910 0.078 Uiso 1 1 calc R U . . . H14C H 1.157985 0.787006 0.364571 0.078 Uiso 1 1 calc R U . . . C17 C 0.7745(4) 0.7419(3) 0.45873(18) 0.0263(8) Uani 1 1 d . . . . . C18 C 0.8769(4) 0.8025(3) 0.45018(18) 0.0268(8) Uani 1 1 d . . . . . C22 C 0.7856(5) 0.6637(3) 0.5067(2) 0.0407(10) Uani 1 1 d . . . . . H22A H 0.731550 0.610886 0.487469 0.061 Uiso 1 1 calc R U . . . H22B H 0.754628 0.685313 0.544670 0.061 Uiso 1 1 calc R U . . . H22C H 0.877962 0.644022 0.519106 0.061 Uiso 1 1 calc R U . . . C7 C 0.9302(4) 0.5533(2) 0.3467(2) 0.0286(8) Uani 1 1 d . . . . . C23 C 1.0113(4) 0.8080(3) 0.4921(2) 0.0428(11) Uani 1 1 d . . . . . H23A H 1.034970 0.747156 0.512182 0.064 Uiso 1 1 calc R U . . . H23B H 1.011487 0.855150 0.525465 0.064 Uiso 1 1 calc R U . . . H23C H 1.075657 0.825350 0.466197 0.064 Uiso 1 1 calc R U . . . C13 C 1.1199(5) 0.6130(4) 0.4352(3) 0.0570(15) Uani 1 1 d . . . . . H13A H 1.167703 0.672065 0.444762 0.086 Uiso 1 1 calc R U . . . H13B H 1.183085 0.562269 0.434564 0.086 Uiso 1 1 calc R U . . . H13C H 1.068802 0.600444 0.468254 0.086 Uiso 1 1 calc R U . . . C24 C 0.8946(5) 0.9559(3) 0.3872(3) 0.0477(12) Uani 1 1 d . . . . . H24A H 0.972325 0.935283 0.371362 0.072 Uiso 1 1 calc R U . . . H24B H 0.922632 0.994823 0.425420 0.072 Uiso 1 1 calc R U . . . H24C H 0.836756 0.992224 0.353917 0.072 Uiso 1 1 calc R U . . . C26 C 0.6988(10) 0.5595(4) 0.0379(4) 0.102(3) Uani 1 1 d . . . . . H26C H 0.675077 0.579573 -0.007483 0.122 Uiso 0.5 1 calc R U P A 1 H26D H 0.792675 0.576183 0.053305 0.122 Uiso 0.5 1 calc R U P A 1 H26A H 0.661630 0.566392 -0.008528 0.122 Uiso 0.5 1 calc R U P A -1 H26B H 0.790702 0.582791 0.045846 0.122 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7012(10) 0.4441(6) 0.0570(3) 0.0575(15) 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 0.01904(9) 0.01919(9) 0.01911(9) -0.00041(6) 0.00080(6) 0.00265(5) I1 0.02879(13) 0.02505(12) 0.02953(14) 0.00142(9) 0.00470(10) -0.00778(9) I4 0.02869(14) 0.02998(14) 0.03796(16) 0.00487(10) 0.00554(11) -0.00798(9) I3 0.03720(15) 0.03433(14) 0.02573(14) 0.00786(10) 0.00369(11) 0.01139(10) I2 0.02388(14) 0.04197(16) 0.0571(2) 0.00066(13) -0.01168(12) -0.00505(10) Cl2 0.0631(8) 0.0578(7) 0.0446(7) 0.0057(6) 0.0111(6) 0.0206(6) Cl1A 0.078(4) 0.055(4) 0.204(10) -0.030(5) 0.014(6) 0.000(3) N1 0.0207(15) 0.0245(15) 0.0195(15) 0.0010(12) 0.0009(12) -0.0026(11) C5 0.0217(17) 0.0230(16) 0.0223(18) 0.0008(14) 0.0028(14) -0.0002(13) C2 0.0220(18) 0.0207(17) 0.027(2) -0.0001(14) 0.0059(15) -0.0038(13) C10 0.0257(19) 0.0227(17) 0.028(2) 0.0015(14) 0.0078(15) 0.0064(13) C6 0.0253(19) 0.0201(17) 0.035(2) -0.0051(15) 0.0035(16) 0.0047(13) C8 0.0250(19) 0.035(2) 0.032(2) -0.0042(17) 0.0000(16) 0.0142(15) C21 0.025(2) 0.055(3) 0.040(3) -0.014(2) 0.0076(18) 0.0006(18) C20 0.042(2) 0.0231(18) 0.0234(19) -0.0043(15) 0.0051(16) 0.0115(15) C19 0.035(2) 0.0237(18) 0.030(2) -0.0060(16) 0.0092(17) -0.0017(15) C4 0.0243(18) 0.0258(18) 0.0248(19) 0.0030(15) 0.0039(15) 0.0043(13) C9 0.0167(17) 0.0267(19) 0.044(2) -0.0056(17) 0.0053(16) 0.0004(13) C3 0.0205(18) 0.0254(17) 0.0239(18) -0.0048(15) -0.0001(14) 0.0002(13) C16 0.0250(19) 0.0252(17) 0.0236(19) -0.0032(14) 0.0060(15) 0.0037(13) C25 0.057(3) 0.045(2) 0.032(2) 0.005(2) 0.003(2) 0.028(2) C15 0.054(3) 0.050(3) 0.034(3) 0.009(2) 0.018(2) 0.017(2) C12 0.060(3) 0.035(2) 0.070(4) 0.023(2) 0.030(3) 0.017(2) C11 0.033(2) 0.043(2) 0.056(3) -0.023(2) 0.002(2) 0.0018(18) C14 0.032(3) 0.044(3) 0.082(4) -0.017(3) 0.017(3) -0.013(2) C17 0.030(2) 0.0276(18) 0.0209(18) -0.0010(15) 0.0045(15) 0.0012(14) C18 0.029(2) 0.0296(18) 0.0213(18) -0.0086(15) 0.0040(15) -0.0012(14) C22 0.051(3) 0.036(2) 0.035(2) 0.0127(19) 0.010(2) 0.0097(19) C7 0.031(2) 0.0188(17) 0.038(2) 0.0055(15) 0.0116(17) 0.0102(14) C23 0.031(2) 0.052(3) 0.042(3) -0.020(2) -0.0019(19) -0.0018(18) C13 0.051(3) 0.071(3) 0.040(3) -0.013(3) -0.012(2) 0.035(3) C24 0.070(3) 0.032(2) 0.047(3) -0.005(2) 0.024(3) -0.012(2) C26 0.190(9) 0.054(4) 0.094(6) 0.014(4) 0.104(6) 0.019(4) Cl1B 0.080(4) 0.044(2) 0.0537(19) 0.0118(17) 0.026(2) 0.019(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 -22 0.0941 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Dy1 I1 62.11(7) . . ? N1 Dy1 C10 83.66(11) . . ? N1 Dy1 C6 92.13(11) . . ? N1 Dy1 C8 134.71(12) . . ? N1 Dy1 C20 80.77(11) . . ? N1 Dy1 C19 96.94(12) . . ? N1 Dy1 C9 107.42(12) . . ? N1 Dy1 C16 99.01(11) . . ? N1 Dy1 C17 129.30(11) . . ? N1 Dy1 C18 128.04(11) . . ? N1 Dy1 C7 122.76(12) . . ? C10 Dy1 I1 102.07(8) . . ? C10 Dy1 C6 30.89(11) . . ? C10 Dy1 C16 176.97(11) . . ? C6 Dy1 I1 80.01(8) . . ? C6 Dy1 C16 146.95(12) . . ? C8 Dy1 I1 122.50(9) . . ? C8 Dy1 C10 51.08(12) . . ? C8 Dy1 C6 50.98(12) . . ? C8 Dy1 C16 126.28(12) . . ? C8 Dy1 C17 95.70(12) . . ? C20 Dy1 I1 91.14(9) . . ? C20 Dy1 C10 151.86(12) . . ? C20 Dy1 C6 170.58(12) . . ? C20 Dy1 C8 138.19(13) . . ? C20 Dy1 C16 30.85(12) . . ? C20 Dy1 C17 51.28(12) . . ? C19 Dy1 I1 122.18(9) . . ? C19 Dy1 C10 130.22(12) . . ? C19 Dy1 C6 157.73(12) . . ? C19 Dy1 C8 110.32(13) . . ? C19 Dy1 C20 31.05(13) . . ? C19 Dy1 C9 106.59(12) . . ? C19 Dy1 C16 51.11(12) . . ? C19 Dy1 C17 51.33(12) . . ? C19 Dy1 C18 31.38(12) . . ? C19 Dy1 C7 137.75(13) . . ? C9 Dy1 I1 130.61(8) . . ? C9 Dy1 C10 30.91(12) . . ? C9 Dy1 C6 51.16(12) . . ? C9 Dy1 C8 31.14(13) . . ? C9 Dy1 C20 136.95(12) . . ? C9 Dy1 C16 147.84(13) . . ? C9 Dy1 C17 118.40(13) . . ? C9 Dy1 C18 97.29(12) . . ? C9 Dy1 C7 51.47(12) . . ? C16 Dy1 I1 78.04(8) . . ? C17 Dy1 I1 99.14(8) . . ? C17 Dy1 C10 146.64(12) . . ? C17 Dy1 C6 133.03(12) . . ? C17 Dy1 C16 30.96(12) . . ? C18 Dy1 I1 128.14(8) . . ? C18 Dy1 C10 128.07(12) . . ? C18 Dy1 C6 137.27(12) . . ? C18 Dy1 C8 86.79(12) . . ? C18 Dy1 C20 51.53(12) . . ? C18 Dy1 C16 51.15(12) . . ? C18 Dy1 C17 30.87(12) . . ? C7 Dy1 I1 91.59(9) . . ? C7 Dy1 C10 51.29(12) . . ? C7 Dy1 C6 31.01(13) . . ? C7 Dy1 C8 30.92(13) . . ? C7 Dy1 C20 154.21(12) . . ? C7 Dy1 C16 125.72(12) . . ? C7 Dy1 C17 103.00(12) . . ? C7 Dy1 C18 108.52(13) . . ? C2 I1 Dy1 68.22(10) . . ? C5 N1 Dy1 143.9(2) . . ? C2 N1 Dy1 111.2(2) . . ? C2 N1 C5 104.1(3) . . ? N1 C5 I4 121.4(2) . . ? N1 C5 C4 111.5(3) . . ? C4 C5 I4 127.0(3) . . ? N1 C2 I1 118.3(3) . . ? N1 C2 C3 112.9(3) . . ? C3 C2 I1 128.7(3) . . ? C6 C10 Dy1 74.6(2) . . ? C6 C10 C15 125.1(4) . . ? C9 C10 Dy1 73.9(2) . . ? C9 C10 C6 108.0(3) . . ? C9 C10 C15 126.4(4) . . ? C15 C10 Dy1 123.2(3) . . ? C10 C6 Dy1 74.5(2) . . ? C10 C6 C11 124.2(4) . . ? C10 C6 C7 108.1(3) . . ? C11 C6 Dy1 125.1(3) . . ? C7 C6 Dy1 73.8(2) . . ? C7 C6 C11 127.0(4) . . ? C9 C8 Dy1 74.0(2) . . ? C9 C8 C13 126.0(4) . . ? C7 C8 Dy1 74.1(2) . . ? C7 C8 C9 108.1(4) . . ? C7 C8 C13 124.5(4) . . ? C13 C8 Dy1 128.4(3) . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? C19 C20 Dy1 73.6(2) . . ? C19 C20 C16 107.9(3) . . ? C19 C20 C25 126.5(4) . . ? C16 C20 Dy1 75.42(19) . . ? C16 C20 C25 125.3(4) . . ? C25 C20 Dy1 121.9(3) . . ? C20 C19 Dy1 75.3(2) . . ? C20 C19 C18 108.4(3) . . ? C20 C19 C24 127.1(4) . . ? C18 C19 Dy1 75.1(2) . . ? C18 C19 C24 124.0(4) . . ? C24 C19 Dy1 122.4(3) . . ? C5 C4 I3 127.1(3) . . ? C5 C4 C3 106.5(3) . . ? C3 C4 I3 126.4(3) . . ? C10 C9 Dy1 75.2(2) . . ? C10 C9 C8 107.8(3) . . ? C10 C9 C14 125.7(4) . . ? C8 C9 Dy1 74.9(2) . . ? C8 C9 C14 126.1(4) . . ? C14 C9 Dy1 121.9(3) . . ? C2 C3 I2 126.5(3) . . ? C2 C3 C4 104.9(3) . . ? C4 C3 I2 128.6(3) . . ? C21 C16 Dy1 127.2(3) . . ? C20 C16 Dy1 73.7(2) . . ? C20 C16 C21 126.5(4) . . ? C20 C16 C17 108.0(3) . . ? C17 C16 Dy1 73.9(2) . . ? C17 C16 C21 124.5(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 75.1(2) . . ? C16 C17 C22 125.2(4) . . ? C18 C17 Dy1 74.3(2) . . ? C18 C17 C16 108.3(3) . . ? C18 C17 C22 126.2(4) . . ? C22 C17 Dy1 122.2(3) . . ? C19 C18 Dy1 73.5(2) . . ? C19 C18 C23 125.1(4) . . ? C17 C18 Dy1 74.9(2) . . ? C17 C18 C19 107.5(3) . . ? C17 C18 C23 126.0(4) . . ? C23 C18 Dy1 128.2(3) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C6 C7 Dy1 75.18(19) . . ? C6 C7 C12 126.1(4) . . ? C8 C7 Dy1 75.0(2) . . ? C8 C7 C6 107.9(3) . . ? C8 C7 C12 125.8(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 106.7 . . ? Cl2 C26 H26D 106.7 . . ? Cl2 C26 H26A 108.6 . . ? Cl2 C26 H26B 108.6 . . ? Cl1A C26 Cl2 122.7(5) . . ? Cl1A C26 H26C 106.7 . . ? Cl1A C26 H26D 106.7 . . ? Cl1A C26 H26A 95.1 . . ? Cl1A C26 H26B 112.5 . . ? Cl1A C26 Cl1B 13.6(5) . . ? H26C C26 H26D 106.6 . . ? H26C C26 H26A 13.5 . . ? H26C C26 H26B 96.2 . . ? H26D C26 H26A 117.6 . . ? H26D C26 H26B 10.6 . . ? H26A C26 H26B 107.6 . . ? Cl1B C26 Cl2 114.6(4) . . ? Cl1B C26 H26C 120.3 . . ? Cl1B C26 H26D 100.9 . . ? 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 3.2379(3) . ? Dy1 N1 2.373(3) . ? Dy1 C10 2.657(3) . ? Dy1 C6 2.658(3) . ? Dy1 C8 2.652(4) . ? Dy1 C20 2.647(3) . ? Dy1 C19 2.626(4) . ? Dy1 C9 2.640(4) . ? Dy1 C16 2.669(3) . ? Dy1 C17 2.654(4) . ? Dy1 C18 2.646(4) . ? Dy1 C7 2.641(3) . ? I1 C2 2.090(3) . ? I4 C5 2.075(3) . ? I3 C4 2.069(4) . ? I2 C3 2.059(4) . ? Cl2 C26 1.714(6) . ? Cl1A C26 1.644(12) . ? N1 C5 1.374(5) . ? N1 C2 1.363(4) . ? C5 C4 1.377(5) . ? C2 C3 1.378(5) . ? C10 C6 1.415(5) . ? C10 C9 1.412(6) . ? C10 C15 1.490(6) . ? C6 C11 1.498(6) . ? C6 C7 1.417(6) . ? C8 C9 1.421(6) . ? C8 C7 1.411(6) . ? C8 C13 1.501(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C16 1.515(5) . ? C20 C19 1.412(6) . ? C20 C16 1.414(5) . ? C20 C25 1.508(5) . ? C19 C18 1.426(6) . ? C19 C24 1.519(6) . ? C4 C3 1.413(5) . ? C9 C14 1.507(5) . ? C16 C17 1.421(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 1.501(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 1.495(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 1.701(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 11.1(5) . . . . ? Dy1 N1 C5 C4 -168.4(3) . . . . ? Dy1 N1 C2 I1 -4.6(3) . . . . ? Dy1 N1 C2 C3 172.2(2) . . . . ? Dy1 C10 C6 C11 122.2(4) . . . . ? Dy1 C10 C6 C7 -66.7(2) . . . . ? Dy1 C10 C9 C8 68.4(2) . . . . ? Dy1 C10 C9 C14 -118.9(4) . . . . ? Dy1 C6 C7 C8 -68.5(2) . . . . ? Dy1 C6 C7 C12 117.2(4) . . . . ? Dy1 C8 C9 C10 -68.6(2) . . . . ? Dy1 C8 C9 C14 118.7(4) . . . . ? Dy1 C8 C7 C6 68.6(2) . . . . ? Dy1 C8 C7 C12 -117.0(4) . . . . ? Dy1 C20 C19 C18 -68.5(3) . . . . ? Dy1 C20 C19 C24 119.8(4) . . . . ? Dy1 C20 C16 C21 -124.5(4) . . . . ? Dy1 C20 C16 C17 66.5(2) . . . . ? Dy1 C19 C18 C17 -67.7(3) . . . . ? Dy1 C19 C18 C23 125.4(4) . . . . ? Dy1 C16 C17 C18 67.5(3) . . . . ? Dy1 C16 C17 C22 -119.2(4) . . . . ? Dy1 C17 C18 C19 66.8(3) . . . . ? Dy1 C17 C18 C23 -126.5(4) . . . . ? I1 C2 C3 I2 -5.3(5) . . . . ? I1 C2 C3 C4 177.2(3) . . . . ? I4 C5 C4 I3 -0.1(5) . . . . ? I4 C5 C4 C3 -179.2(3) . . . . ? I3 C4 C3 I2 2.8(5) . . . . ? I3 C4 C3 C2 -179.8(3) . . . . ? N1 C5 C4 I3 179.4(2) . . . . ? N1 C5 C4 C3 0.3(4) . . . . ? N1 C2 C3 I2 178.3(2) . . . . ? N1 C2 C3 C4 0.8(4) . . . . ? C5 N1 C2 I1 -177.4(2) . . . . ? C5 N1 C2 C3 -0.7(4) . . . . ? C5 C4 C3 I2 -178.0(3) . . . . ? C5 C4 C3 C2 -0.7(4) . . . . ? C2 N1 C5 I4 179.7(2) . . . . ? C2 N1 C5 C4 0.2(4) . . . . ? C10 C6 C7 Dy1 67.2(2) . . . . ? C10 C6 C7 C8 -1.3(4) . . . . ? C10 C6 C7 C12 -175.6(4) . . . . ? C6 C10 C9 Dy1 -67.4(2) . . . . ? C6 C10 C9 C8 1.0(4) . . . . ? C6 C10 C9 C14 173.8(4) . . . . ? C21 C16 C17 Dy1 124.4(4) . . . . ? C21 C16 C17 C18 -168.2(4) . . . . ? C21 C16 C17 C22 5.2(6) . . . . ? C20 C19 C18 Dy1 68.6(3) . . . . ? C20 C19 C18 C17 0.9(4) . . . . ? C20 C19 C18 C23 -166.0(4) . . . . ? C20 C16 C17 Dy1 -66.4(3) . . . . ? C20 C16 C17 C18 1.1(4) . . . . ? C20 C16 C17 C22 174.4(4) . . . . ? C19 C20 C16 Dy1 -67.1(3) . . . . ? C19 C20 C16 C21 168.4(4) . . . . ? C19 C20 C16 C17 -0.5(4) . . . . ? C9 C10 C6 Dy1 66.9(2) . . . . ? C9 C10 C6 C11 -170.9(3) . . . . ? C9 C10 C6 C7 0.2(4) . . . . ? C9 C8 C7 Dy1 -66.7(3) . . . . ? C9 C8 C7 C6 1.9(4) . . . . ? C9 C8 C7 C12 176.3(4) . . . . ? C16 C20 C19 Dy1 68.3(3) . . . . ? C16 C20 C19 C18 -0.2(4) . . . . ? C16 C20 C19 C24 -172.0(4) . . . . ? C16 C17 C18 Dy1 -68.0(3) . . . . ? C16 C17 C18 C19 -1.2(4) . . . . ? C16 C17 C18 C23 165.5(4) . . . . ? C25 C20 C19 Dy1 -117.9(4) . . . . ? C25 C20 C19 C18 173.6(4) . . . . ? C25 C20 C19 C24 1.9(7) . . . . ? C25 C20 C16 Dy1 119.0(4) . . . . ? C25 C20 C16 C21 -5.5(6) . . . . ? C25 C20 C16 C17 -174.5(4) . . . . ? C15 C10 C6 Dy1 -120.0(4) . . . . ? C15 C10 C6 C11 2.1(6) . . . . ? C15 C10 C6 C7 173.2(3) . . . . ? C15 C10 C9 Dy1 119.7(4) . . . . ? C15 C10 C9 C8 -171.9(4) . . . . ? C15 C10 C9 C14 0.8(6) . . . . ? C11 C6 C7 Dy1 -122.1(4) . . . . ? C11 C6 C7 C8 169.5(4) . . . . ? C11 C6 C7 C12 -4.9(6) . . . . ? C22 C17 C18 Dy1 118.7(4) . . . . ? C22 C17 C18 C19 -174.5(4) . . . . ? C22 C17 C18 C23 -7.8(6) . . . . ? C7 C8 C9 Dy1 66.8(3) . . . . ? C7 C8 C9 C10 -1.8(4) . . . . ? C7 C8 C9 C14 -174.5(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 -119.3(4) . . . . ? C24 C19 C18 C17 172.9(4) . . . . ? C24 C19 C18 C23 6.1(6) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1.0041 -1.0145 0.0739 -0.0783 -0.0142 0.0325 -1.0077 0.9971 0.0050 0.0038 0.0040 0.0859 1.0041 1.0145 -0.0739 0.0783 0.0142 -0.0325 1.0077 -0.9971 -0.0050 -0.0038 -0.0040 -0.0859 -0.0068 -0.0169 -0.9986 -0.0100 0.0322 0.0044 0.0068 0.0169 0.9986 0.0100 -0.0322 -0.0044 -0.9940 1.0309 2.0023 0.0239 -0.0605 0.0770 0.9940 -1.0309 -2.0023 -0.0239 0.0605 -0.0770 1.0145 -0.9802 0.9936 0.0063 -0.0363 -0.0903 0.0119 1.0397 1.9628 0.0612 -0.0554 0.0178 2.0204 -0.9715 0.9541 0.0435 -0.0312 -0.1495 -0.0154 0.9719 -2.0317 0.0210 0.0736 0.0356 -1.0196 -0.0426 -1.9578 -0.0574 0.0594 0.0681 -0.9922 0.0251 2.0367 -0.0172 -0.0696 0.0503 -5.9544 6.8785 -22.4217 -0.1415 0.7602 0.6341