#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572175.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_1572175 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 101.444(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3100(2) _cell_length_b 14.2475(2) _cell_length_c 21.2431(4) _cell_measurement_reflns_used 22638 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 31.8950 _cell_measurement_theta_min 2.8590 _cell_volume 3058.40(10) _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 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100.01(10) _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 0.839 _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 0.0372990000 _diffrn_orient_matrix_UB_12 0.0410624000 _diffrn_orient_matrix_UB_13 0.0100428000 _diffrn_orient_matrix_UB_21 0.0050652000 _diffrn_orient_matrix_UB_22 0.0091144000 _diffrn_orient_matrix_UB_23 -0.0322487000 _diffrn_orient_matrix_UB_31 -0.0592429000 _diffrn_orient_matrix_UB_32 0.0266365000 _diffrn_orient_matrix_UB_33 -0.0044502000 _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 0.0544 _diffrn_reflns_av_unetI/netI 0.0425 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.839 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 37524 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.839 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.718 _diffrn_reflns_theta_min 2.471 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.671 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.218 _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 2.362 _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 1.596 _refine_diff_density_min -1.622 _refine_diff_density_rms 0.206 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8694 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0304 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.0749 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7485 _reflns_number_total 8694 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP100K _cod_database_code 1572175 _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 0.525 _shelx_estimated_absorpt_t_min 0.202 _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_100_final.res created by SHELXL-2018/3 at 15:20:47 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 10.31 14.2475 21.2431 90 101.444 90 ZERR 4 0.0002 0.0002 0.0004 0 0.002 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. 4 0 0 PLAN 14 SIZE 0.111 0.275 0.353 TEMP -173 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.038200 0.200000 FVAR 0.10923 DY1 4 0.805551 0.712557 0.339900 11.00000 0.01165 0.01117 = 0.01148 -0.00050 0.00022 0.00165 I1 5 0.525788 0.611415 0.283797 11.00000 0.01615 0.01396 = 0.01664 0.00078 0.00227 -0.00381 I4 5 0.818919 0.939701 0.201920 11.00000 0.01590 0.01670 = 0.02154 0.00245 0.00285 -0.00388 I3 5 0.480798 0.933258 0.081316 11.00000 0.02033 0.01920 = 0.01475 0.00400 0.00159 0.00582 I2 5 0.290650 0.715605 0.131926 11.00000 0.01368 0.02311 = 0.03274 0.00098 -0.00670 -0.00288 CL2 3 0.611368 0.630593 0.079999 11.00000 0.03367 0.03392 = 0.02467 0.00332 0.00528 0.01159 PART 1 CL1A 3 0.686273 0.444971 0.038144 10.50000 0.04099 0.03087 = 0.14348 -0.02858 -0.00641 -0.00077 PART 0 N1 6 0.676725 0.772386 0.243148 11.00000 0.01517 0.01266 = 0.01356 -0.00053 0.00142 -0.00290 C5 1 0.666552 0.843716 0.199149 11.00000 0.01492 0.01000 = 0.01659 0.00129 0.00277 -0.00017 C2 1 0.559275 0.725144 0.227179 11.00000 0.01256 0.01452 = 0.01697 0.00101 0.00306 -0.00074 C10 1 0.958637 0.647537 0.262566 11.00000 0.01339 0.01653 = 0.01398 -0.00024 0.00176 0.00238 C6 1 0.886213 0.568496 0.278114 11.00000 0.01499 0.01272 = 0.01746 -0.00078 0.00392 0.00125 C8 1 1.029871 0.617110 0.370065 11.00000 0.01507 0.02046 = 0.02109 -0.00383 -0.00003 0.01096 C21 1 0.518737 0.740354 0.424216 11.00000 0.01431 0.02590 = 0.02202 -0.00607 0.00413 0.00026 AFIX 137 H21A 2 0.455924 0.761917 0.386131 11.00000 -1.50000 H21B 2 0.493463 0.765935 0.462883 11.00000 -1.50000 H21C 2 0.517632 0.671629 0.425936 11.00000 -1.50000 AFIX 0 C20 1 0.687636 0.853969 0.386836 11.00000 0.02216 0.01454 = 0.01440 -0.00180 0.00423 0.00419 C19 1 0.825796 0.869967 0.405997 11.00000 0.01859 0.01465 = 0.01736 -0.00234 0.00443 0.00184 C4 1 0.545968 0.841466 0.156578 11.00000 0.01457 0.01568 = 0.01744 0.00121 0.00414 0.00188 C9 1 1.045346 0.677990 0.319155 11.00000 0.01220 0.01853 = 0.02665 -0.00565 0.00312 0.00215 C3 1 0.475032 0.764437 0.174802 11.00000 0.01170 0.01697 = 0.01700 -0.00238 -0.00057 0.00021 C16 1 0.656135 0.773602 0.420667 11.00000 0.01475 0.01199 = 0.01639 -0.00288 0.00111 0.00278 C25 1 0.589801 0.916586 0.344979 11.00000 0.03042 0.02174 = 0.02123 0.00050 0.00235 0.01499 AFIX 137 H25A 2 0.636075 0.956273 0.318854 11.00000 -1.50000 H25B 2 0.545547 0.956304 0.371950 11.00000 -1.50000 H25C 2 0.523834 0.878107 0.316774 11.00000 -1.50000 AFIX 0 C15 1 0.951280 0.683595 0.195431 11.00000 0.02726 0.02795 = 0.02328 0.00288 0.00999 0.00774 AFIX 137 H15A 2 0.858372 0.689283 0.173817 11.00000 -1.50000 H15B 2 0.996697 0.639753 0.171576 11.00000 -1.50000 H15C 2 0.993975 0.745251 0.197142 11.00000 -1.50000 AFIX 0 C12 1 0.886287 0.469028 0.380979 11.00000 0.03448 0.02063 = 0.03132 0.01165 0.01505 0.01106 AFIX 137 H12A 2 0.879372 0.489708 0.424188 11.00000 -1.50000 H12B 2 0.951296 0.418192 0.384166 11.00000 -1.50000 H12C 2 0.799885 0.446412 0.358204 11.00000 -1.50000 AFIX 0 C11 1 0.799484 0.507790 0.229278 11.00000 0.01939 0.02533 = 0.03542 -0.01466 0.00539 -0.00329 AFIX 137 H11A 2 0.753484 0.461830 0.251292 11.00000 -1.50000 H11B 2 0.854047 0.474862 0.203438 11.00000 -1.50000 H11C 2 0.734331 0.547068 0.201239 11.00000 -1.50000 AFIX 0 C14 1 1.148221 0.753367 0.322591 11.00000 0.01775 0.03231 = 0.04514 -0.00957 0.00837 -0.00259 AFIX 137 H14A 2 1.116882 0.801288 0.290027 11.00000 -1.50000 H14B 2 1.230603 0.725827 0.314669 11.00000 -1.50000 H14C 2 1.164346 0.782199 0.365319 11.00000 -1.50000 AFIX 0 C17 1 0.774948 0.738939 0.459765 11.00000 0.01707 0.01554 = 0.01353 -0.00176 0.00199 0.00037 C18 1 0.879504 0.799525 0.451577 11.00000 0.01583 0.01496 = 0.01391 -0.00326 0.00172 0.00069 C22 1 0.784940 0.660064 0.507084 11.00000 0.02670 0.02128 = 0.02181 0.00610 0.00535 0.00371 AFIX 137 H22A 2 0.725882 0.608972 0.488559 11.00000 -1.50000 H22B 2 0.759178 0.682538 0.546446 11.00000 -1.50000 H22C 2 0.876298 0.637068 0.517210 11.00000 -1.50000 AFIX 0 C7 1 0.929882 0.550306 0.344597 11.00000 0.02011 0.01604 = 0.02135 0.00575 0.00660 0.00826 C23 1 1.014951 0.802858 0.493613 11.00000 0.01895 0.03042 = 0.02171 -0.00829 0.00006 -0.00093 AFIX 137 H23A 2 1.035324 0.741940 0.514681 11.00000 -1.50000 H23B 2 1.017355 0.851758 0.526267 11.00000 -1.50000 H23C 2 1.080571 0.817049 0.467323 11.00000 -1.50000 AFIX 0 C13 1 1.121132 0.608988 0.434645 11.00000 0.03569 0.03698 = 0.02323 -0.00666 -0.00873 0.02176 AFIX 137 H13A 2 1.169119 0.668164 0.444921 11.00000 -1.50000 H13B 2 1.184479 0.558035 0.433504 11.00000 -1.50000 H13C 2 1.069180 0.595479 0.467529 11.00000 -1.50000 AFIX 0 C24 1 0.902669 0.953748 0.389608 11.00000 0.02953 0.01692 = 0.02609 -0.00445 0.00747 -0.00537 AFIX 137 H24A 2 0.985660 0.932410 0.378497 11.00000 -1.50000 H24B 2 0.922284 0.995952 0.426710 11.00000 -1.50000 H24C 2 0.849915 0.987214 0.352989 11.00000 -1.50000 AFIX 0 C26 1 0.707007 0.560001 0.040659 11.00000 0.14473 0.02951 = 0.07995 0.01940 0.09383 0.02423 PART 1 AFIX 23 H26C 2 0.693756 0.582339 -0.004294 10.50000 -1.20000 H26D 2 0.800804 0.572087 0.060434 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.679792 0.570578 -0.006165 10.50000 -1.20000 H26B 2 0.800714 0.579418 0.053598 10.50000 -1.20000 AFIX 0 CL1B 3 0.695544 0.442644 0.055771 10.50000 0.04944 0.02165 = 0.03420 0.00666 0.02124 0.00685 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0749, GooF = S = 1.046, Restrained GooF = 1.046 for all data REM R1 = 0.0304 for 7485 Fo > 4sig(Fo) and 0.0380 for all 8694 data REM 317 parameters refined using 6 restraints END WGHT 0.0381 0.3350 REM Highest difference peak 1.596, deepest hole -1.622, 1-sigma level 0.206 Q1 1 0.7414 0.5635 0.0444 11.00000 0.05 1.06 Q2 1 0.8949 0.7392 0.3411 11.00000 0.05 1.05 Q3 1 0.6219 0.6563 0.2806 11.00000 0.05 0.93 Q4 1 0.8888 0.7126 0.3007 11.00000 0.05 0.92 Q5 1 0.9000 0.9021 0.2004 11.00000 0.05 0.88 Q6 1 0.9022 0.7163 0.3773 11.00000 0.05 0.88 Q7 1 0.7217 0.4406 0.3810 11.00000 0.05 0.87 Q8 1 0.7207 0.6880 0.3429 11.00000 0.05 0.85 Q9 1 1.1834 0.7559 0.2854 11.00000 0.05 0.85 Q10 1 0.5708 0.9399 0.0409 11.00000 0.05 0.83 Q11 1 0.1972 0.7232 0.1785 11.00000 0.05 0.82 Q12 1 0.5819 0.8957 0.0784 11.00000 0.05 0.81 Q13 1 0.7134 0.7313 0.3427 11.00000 0.05 0.81 Q14 1 0.4000 0.9743 0.0809 11.00000 0.05 0.80 ; _shelx_res_checksum 64725 _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 2.475 _oxdiff_exptl_absorpt_empirical_full_min 0.675 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 0.80555(2) 0.71256(2) 0.33990(2) 0.01172(5) Uani 1 1 d . . . . . I1 I 0.52579(2) 0.61142(2) 0.28380(2) 0.01572(6) Uani 1 1 d . . . . . I4 I 0.81892(2) 0.93970(2) 0.20192(2) 0.01817(6) Uani 1 1 d . . . . . I3 I 0.48080(2) 0.93326(2) 0.08132(2) 0.01835(6) Uani 1 1 d . . . . . I2 I 0.29065(2) 0.71560(2) 0.13193(2) 0.02473(7) Uani 1 1 d . . . . . Cl2 Cl 0.61137(11) 0.63059(7) 0.08000(5) 0.0308(2) Uani 1 1 d . . . . . Cl1A Cl 0.6863(9) 0.4450(5) 0.0381(4) 0.075(2) Uani 0.5 1 d . U P A 1 N1 N 0.6767(3) 0.77239(19) 0.24315(14) 0.0140(5) Uani 1 1 d . . . . . C5 C 0.6666(3) 0.8437(2) 0.19915(17) 0.0139(6) Uani 1 1 d . . . . . C2 C 0.5593(3) 0.7251(2) 0.22718(17) 0.0147(6) Uani 1 1 d . . . . . C10 C 0.9586(3) 0.6475(2) 0.26257(16) 0.0148(6) Uani 1 1 d . . . . . C6 C 0.8862(3) 0.5685(2) 0.27811(17) 0.0150(6) Uani 1 1 d . . . . . C8 C 1.0299(3) 0.6171(2) 0.37006(18) 0.0194(7) Uani 1 1 d . . . . . C21 C 0.5187(3) 0.7404(3) 0.42422(19) 0.0207(7) Uani 1 1 d . . . . . H21A H 0.455924 0.761917 0.386131 0.031 Uiso 1 1 calc R U . . . H21B H 0.493463 0.765935 0.462883 0.031 Uiso 1 1 calc R U . . . H21C H 0.517632 0.671629 0.425936 0.031 Uiso 1 1 calc R U . . . C20 C 0.6876(4) 0.8540(2) 0.38684(17) 0.0169(7) Uani 1 1 d . . . . . C19 C 0.8258(3) 0.8700(2) 0.40600(17) 0.0167(7) Uani 1 1 d . . . . . C4 C 0.5460(3) 0.8415(2) 0.15658(17) 0.0158(6) Uani 1 1 d . . . . . C9 C 1.0453(3) 0.6780(2) 0.31916(19) 0.0192(7) Uani 1 1 d . . . . . C3 C 0.4750(3) 0.7644(2) 0.17480(17) 0.0157(6) Uani 1 1 d . . . . . C16 C 0.6561(3) 0.7736(2) 0.42067(17) 0.0147(6) Uani 1 1 d . . . . . C25 C 0.5898(4) 0.9166(3) 0.34498(19) 0.0248(8) Uani 1 1 d . . . . . H25A H 0.636075 0.956273 0.318854 0.037 Uiso 1 1 calc R U . . . H25B H 0.545547 0.956304 0.371950 0.037 Uiso 1 1 calc R U . . . H25C H 0.523834 0.878107 0.316774 0.037 Uiso 1 1 calc R U . . . C15 C 0.9513(4) 0.6836(3) 0.19543(19) 0.0255(8) Uani 1 1 d . . . . . H15A H 0.858372 0.689283 0.173817 0.038 Uiso 1 1 calc R U . . . H15B H 0.996697 0.639753 0.171576 0.038 Uiso 1 1 calc R U . . . H15C H 0.993975 0.745251 0.197142 0.038 Uiso 1 1 calc R U . . . C12 C 0.8863(4) 0.4690(3) 0.3810(2) 0.0276(9) Uani 1 1 d . . . . . H12A H 0.879372 0.489708 0.424188 0.041 Uiso 1 1 calc R U . . . H12B H 0.951296 0.418192 0.384166 0.041 Uiso 1 1 calc R U . . . H12C H 0.799885 0.446412 0.358204 0.041 Uiso 1 1 calc R U . . . C11 C 0.7995(4) 0.5078(3) 0.2293(2) 0.0267(8) Uani 1 1 d . . . . . H11A H 0.753484 0.461830 0.251292 0.040 Uiso 1 1 calc R U . . . H11B H 0.854047 0.474862 0.203438 0.040 Uiso 1 1 calc R U . . . H11C H 0.734331 0.547068 0.201239 0.040 Uiso 1 1 calc R U . . . C14 C 1.1482(4) 0.7534(3) 0.3226(2) 0.0314(9) Uani 1 1 d . . . . . H14A H 1.116882 0.801288 0.290027 0.047 Uiso 1 1 calc R U . . . H14B H 1.230603 0.725827 0.314669 0.047 Uiso 1 1 calc R U . . . H14C H 1.164346 0.782199 0.365319 0.047 Uiso 1 1 calc R U . . . C17 C 0.7749(3) 0.7389(2) 0.45976(17) 0.0155(6) Uani 1 1 d . . . . . C18 C 0.8795(3) 0.7995(2) 0.45158(17) 0.0151(6) Uani 1 1 d . . . . . C22 C 0.7849(4) 0.6601(3) 0.50708(19) 0.0232(8) Uani 1 1 d . . . . . H22A H 0.725882 0.608972 0.488559 0.035 Uiso 1 1 calc R U . . . H22B H 0.759178 0.682538 0.546446 0.035 Uiso 1 1 calc R U . . . H22C H 0.876298 0.637068 0.517210 0.035 Uiso 1 1 calc R U . . . C7 C 0.9299(4) 0.5503(2) 0.34460(18) 0.0188(7) Uani 1 1 d . . . . . C23 C 1.0150(4) 0.8029(3) 0.4936(2) 0.0242(8) Uani 1 1 d . . . . . H23A H 1.035324 0.741940 0.514681 0.036 Uiso 1 1 calc R U . . . H23B H 1.017355 0.851758 0.526267 0.036 Uiso 1 1 calc R U . . . H23C H 1.080571 0.817049 0.467323 0.036 Uiso 1 1 calc R U . . . C13 C 1.1211(4) 0.6090(3) 0.4346(2) 0.0340(10) Uani 1 1 d . . . . . H13A H 1.169119 0.668164 0.444921 0.051 Uiso 1 1 calc R U . . . H13B H 1.184479 0.558035 0.433504 0.051 Uiso 1 1 calc R U . . . H13C H 1.069180 0.595479 0.467529 0.051 Uiso 1 1 calc R U . . . C24 C 0.9027(4) 0.9537(3) 0.3896(2) 0.0239(8) Uani 1 1 d . . . . . H24A H 0.985660 0.932410 0.378497 0.036 Uiso 1 1 calc R U . . . H24B H 0.922284 0.995952 0.426710 0.036 Uiso 1 1 calc R U . . . H24C H 0.849915 0.987214 0.352989 0.036 Uiso 1 1 calc R U . . . C26 C 0.7070(9) 0.5600(3) 0.0407(4) 0.075(3) Uani 1 1 d . . . . . H26C H 0.693756 0.582339 -0.004294 0.090 Uiso 0.5 1 calc R U P A 1 H26D H 0.800804 0.572087 0.060434 0.090 Uiso 0.5 1 calc R U P A 1 H26A H 0.679792 0.570578 -0.006165 0.090 Uiso 0.5 1 calc R U P A -1 H26B H 0.800714 0.579418 0.053598 0.090 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.6955(7) 0.4426(5) 0.0558(2) 0.0333(12) 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 0.01165(8) 0.01117(8) 0.01148(8) -0.00050(5) 0.00022(6) 0.00165(5) I1 0.01615(11) 0.01396(11) 0.01664(11) 0.00078(8) 0.00227(8) -0.00381(7) I4 0.01590(12) 0.01670(11) 0.02154(12) 0.00245(8) 0.00285(9) -0.00388(8) I3 0.02033(12) 0.01920(11) 0.01475(11) 0.00400(8) 0.00159(9) 0.00582(8) I2 0.01368(12) 0.02311(13) 0.03274(15) 0.00098(10) -0.00670(10) -0.00288(8) Cl2 0.0337(5) 0.0339(5) 0.0247(5) 0.0033(4) 0.0053(4) 0.0116(4) Cl1A 0.041(2) 0.031(3) 0.143(7) -0.029(4) -0.006(4) -0.0008(17) N1 0.0152(14) 0.0127(13) 0.0136(14) -0.0005(11) 0.0014(11) -0.0029(10) C5 0.0149(16) 0.0100(14) 0.0166(16) 0.0013(12) 0.0028(13) -0.0002(11) C2 0.0126(16) 0.0145(15) 0.0170(17) 0.0010(12) 0.0031(13) -0.0007(11) C10 0.0134(16) 0.0165(16) 0.0140(16) -0.0002(12) 0.0018(12) 0.0024(11) C6 0.0150(16) 0.0127(15) 0.0175(17) -0.0008(12) 0.0039(13) 0.0012(11) C8 0.0151(17) 0.0205(17) 0.0211(18) -0.0038(14) 0.0000(14) 0.0110(13) C21 0.0143(17) 0.0259(18) 0.0220(19) -0.0061(15) 0.0041(14) 0.0003(13) C20 0.0222(18) 0.0145(15) 0.0144(16) -0.0018(13) 0.0042(13) 0.0042(13) C19 0.0186(17) 0.0147(15) 0.0174(17) -0.0023(13) 0.0044(13) 0.0018(12) C4 0.0146(16) 0.0157(16) 0.0174(17) 0.0012(13) 0.0041(13) 0.0019(12) C9 0.0122(16) 0.0185(17) 0.027(2) -0.0057(14) 0.0031(14) 0.0021(12) C3 0.0117(16) 0.0170(15) 0.0170(17) -0.0024(13) -0.0006(12) 0.0002(12) C16 0.0148(16) 0.0120(14) 0.0164(17) -0.0029(12) 0.0011(13) 0.0028(11) C25 0.030(2) 0.0217(18) 0.0212(19) 0.0005(15) 0.0023(16) 0.0150(15) C15 0.027(2) 0.028(2) 0.023(2) 0.0029(16) 0.0100(16) 0.0077(15) C12 0.034(2) 0.0206(18) 0.031(2) 0.0117(16) 0.0150(18) 0.0111(16) C11 0.0194(19) 0.0253(19) 0.035(2) -0.0147(17) 0.0054(16) -0.0033(14) C14 0.0177(19) 0.032(2) 0.045(3) -0.0096(19) 0.0084(18) -0.0026(16) C17 0.0171(16) 0.0155(15) 0.0135(16) -0.0018(13) 0.0020(13) 0.0004(12) C18 0.0158(16) 0.0150(15) 0.0139(16) -0.0033(12) 0.0017(13) 0.0007(12) C22 0.027(2) 0.0213(18) 0.0218(19) 0.0061(15) 0.0053(15) 0.0037(14) C7 0.0201(18) 0.0160(16) 0.0214(18) 0.0058(14) 0.0066(14) 0.0083(13) C23 0.0190(19) 0.030(2) 0.0217(19) -0.0083(16) 0.0001(15) -0.0009(14) C13 0.036(2) 0.037(2) 0.023(2) -0.0067(18) -0.0087(17) 0.0218(18) C24 0.030(2) 0.0169(17) 0.026(2) -0.0045(15) 0.0075(16) -0.0054(14) C26 0.145(7) 0.030(3) 0.080(5) 0.019(3) 0.094(5) 0.024(3) Cl1B 0.049(3) 0.0216(16) 0.0342(15) 0.0067(12) 0.0212(17) 0.0068(16) 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 62.34(6) . . ? N1 Dy1 C10 83.62(10) . . ? N1 Dy1 C6 91.48(10) . . ? N1 Dy1 C8 134.87(11) . . ? N1 Dy1 C20 80.38(10) . . ? N1 Dy1 C19 97.32(10) . . ? N1 Dy1 C9 107.69(11) . . ? N1 Dy1 C16 98.31(10) . . ? N1 Dy1 C17 128.86(10) . . ? N1 Dy1 C18 128.27(10) . . ? N1 Dy1 C7 122.16(11) . . ? C10 Dy1 I1 102.26(7) . . ? C10 Dy1 C16 177.98(10) . . ? C6 Dy1 I1 79.48(7) . . ? C6 Dy1 C10 31.11(10) . . ? C6 Dy1 C16 147.83(10) . . ? C8 Dy1 I1 122.17(8) . . ? C8 Dy1 C10 51.27(11) . . ? C8 Dy1 C6 51.63(11) . . ? C8 Dy1 C16 126.82(11) . . ? C8 Dy1 C17 96.02(11) . . ? C8 Dy1 C18 86.63(11) . . ? C20 Dy1 I1 92.02(8) . . ? C20 Dy1 C10 150.51(11) . . ? C20 Dy1 C6 170.32(11) . . ? C20 Dy1 C8 138.02(11) . . ? C20 Dy1 C16 31.05(10) . . ? C20 Dy1 C17 51.69(11) . . ? C20 Dy1 C18 51.64(11) . . ? C19 Dy1 I1 123.16(8) . . ? C19 Dy1 C10 129.21(11) . . ? C19 Dy1 C6 157.25(11) . . ? C19 Dy1 C8 109.59(11) . . ? C19 Dy1 C20 31.20(11) . . ? C19 Dy1 C9 105.66(11) . . ? C19 Dy1 C16 51.26(10) . . ? C19 Dy1 C17 51.64(11) . . ? C19 Dy1 C18 31.36(10) . . ? C19 Dy1 C7 137.79(12) . . ? C9 Dy1 I1 130.64(8) . . ? C9 Dy1 C10 30.98(11) . . ? C9 Dy1 C6 51.59(11) . . ? C9 Dy1 C8 31.13(12) . . ? C9 Dy1 C20 135.99(11) . . ? C9 Dy1 C16 147.84(11) . . ? C9 Dy1 C17 118.67(11) . . ? C9 Dy1 C18 97.12(11) . . ? C16 Dy1 I1 78.21(7) . . ? C17 Dy1 I1 98.60(7) . . ? C17 Dy1 C10 147.13(10) . . ? C17 Dy1 C6 133.77(10) . . ? C17 Dy1 C16 31.06(10) . . ? C18 Dy1 I1 127.98(7) . . ? C18 Dy1 C10 127.94(10) . . ? C18 Dy1 C6 137.77(11) . . ? C18 Dy1 C16 51.14(10) . . ? C18 Dy1 C17 31.02(10) . . ? C7 Dy1 I1 90.84(8) . . ? C7 Dy1 C10 51.26(11) . . ? C7 Dy1 C6 31.09(11) . . ? C7 Dy1 C8 31.36(11) . . ? C7 Dy1 C20 155.40(11) . . ? C7 Dy1 C9 51.59(11) . . ? C7 Dy1 C16 126.87(11) . . ? C7 Dy1 C17 103.73(11) . . ? C7 Dy1 C18 108.95(11) . . ? C2 I1 Dy1 68.22(9) . . ? C5 N1 Dy1 144.2(2) . . ? C2 N1 Dy1 110.7(2) . . ? C2 N1 C5 104.6(3) . . ? N1 C5 I4 121.0(2) . . ? N1 C5 C4 111.4(3) . . ? C4 C5 I4 127.6(2) . . ? N1 C2 I1 118.6(2) . . ? N1 C2 C3 112.5(3) . . ? C3 C2 I1 128.8(2) . . ? C6 C10 Dy1 74.33(19) . . ? C6 C10 C15 124.0(3) . . ? C9 C10 Dy1 73.81(19) . . ? C9 C10 C6 108.5(3) . . ? C9 C10 C15 127.2(3) . . ? C15 C10 Dy1 122.8(2) . . ? C10 C6 Dy1 74.57(18) . . ? C10 C6 C11 124.2(3) . . ? C11 C6 Dy1 125.7(2) . . ? C7 C6 Dy1 73.62(19) . . ? C7 C6 C10 107.3(3) . . ? C7 C6 C11 127.6(3) . . ? C9 C8 Dy1 74.15(19) . . ? C9 C8 C7 107.5(3) . . ? C9 C8 C13 126.6(4) . . ? C7 C8 Dy1 73.78(19) . . ? C7 C8 C13 124.6(4) . . ? C13 C8 Dy1 128.1(2) . . ? 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 73.78(19) . . ? C19 C20 C16 107.5(3) . . ? C19 C20 C25 126.4(3) . . ? C16 C20 Dy1 75.28(18) . . ? C16 C20 C25 125.7(3) . . ? C25 C20 Dy1 122.3(2) . . ? C20 C19 Dy1 75.02(19) . . ? C20 C19 C18 108.3(3) . . ? C20 C19 C24 127.1(3) . . ? C18 C19 Dy1 75.04(19) . . ? C18 C19 C24 124.1(3) . . ? C24 C19 Dy1 122.7(2) . . ? C5 C4 I3 126.9(2) . . ? C5 C4 C3 106.6(3) . . ? C3 C4 I3 126.5(3) . . ? C10 C9 Dy1 75.21(19) . . ? C10 C9 C8 108.2(3) . . ? C10 C9 C14 125.5(4) . . ? C8 C9 Dy1 74.73(19) . . ? C8 C9 C14 125.8(4) . . ? C14 C9 Dy1 122.3(2) . . ? C2 C3 I2 126.5(3) . . ? C2 C3 C4 104.9(3) . . ? C4 C3 I2 128.5(3) . . ? C21 C16 Dy1 126.6(2) . . ? C20 C16 Dy1 73.67(19) . . ? C20 C16 C21 126.0(3) . . ? C20 C16 C17 108.5(3) . . ? C17 C16 Dy1 73.90(19) . . ? C17 C16 C21 124.7(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 75.0(2) . . ? C16 C17 C22 126.0(3) . . ? C18 C17 Dy1 74.37(19) . . ? C18 C17 C16 107.7(3) . . ? C18 C17 C22 125.9(3) . . ? C22 C17 Dy1 122.2(2) . . ? C19 C18 Dy1 73.60(19) . . ? C19 C18 C23 124.8(3) . . ? C17 C18 Dy1 74.61(19) . . ? C17 C18 C19 108.0(3) . . ? C17 C18 C23 125.9(3) . . ? C23 C18 Dy1 128.0(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 75.29(18) . . ? C6 C7 C8 108.5(3) . . ? C6 C7 C12 125.6(4) . . ? C8 C7 Dy1 74.87(19) . . ? C8 C7 C12 125.7(4) . . ? C12 C7 Dy1 120.0(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 107.2 . . ? Cl2 C26 H26D 107.2 . . ? Cl2 C26 H26A 108.7 . . ? Cl2 C26 H26B 108.7 . . ? Cl1A C26 Cl2 120.6(4) . . ? Cl1A C26 H26C 107.2 . . ? Cl1A C26 H26D 107.2 . . ? Cl1A C26 H26A 96.3 . . ? Cl1A C26 H26B 113.5 . . ? Cl1A C26 Cl1B 12.4(4) . . ? H26C C26 H26D 106.8 . . ? H26C C26 H26A 12.7 . . ? H26C C26 H26B 96.8 . . ? H26D C26 H26A 117.3 . . ? H26D C26 H26B 10.4 . . ? H26A C26 H26B 107.6 . . ? Cl1B C26 Cl2 114.2(3) . . ? Cl1B C26 H26C 119.6 . . ? Cl1B C26 H26D 100.9 . . ? Cl1B C26 H26A 108.7 . . ? Cl1B C26 H26B 108.7 . . ? 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 3.2330(3) . ? Dy1 N1 2.373(3) . ? Dy1 C10 2.660(3) . ? Dy1 C6 2.657(3) . ? Dy1 C8 2.650(3) . ? Dy1 C20 2.648(3) . ? Dy1 C19 2.632(3) . ? Dy1 C9 2.642(3) . ? Dy1 C16 2.669(3) . ? Dy1 C17 2.654(3) . ? Dy1 C18 2.651(3) . ? Dy1 C7 2.636(3) . ? I1 C2 2.087(3) . ? I4 C5 2.075(3) . ? I3 C4 2.072(3) . ? I2 C3 2.059(3) . ? Cl2 C26 1.735(5) . ? Cl1A C26 1.652(9) . ? N1 C5 1.371(4) . ? N1 C2 1.368(4) . ? C5 C4 1.385(5) . ? C2 C3 1.386(5) . ? C10 C6 1.426(5) . ? C10 C9 1.416(5) . ? C10 C15 1.504(5) . ? C6 C11 1.502(5) . ? C6 C7 1.418(5) . ? C8 C9 1.420(5) . ? C8 C7 1.428(5) . ? C8 C13 1.506(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C16 1.510(5) . ? C20 C19 1.420(5) . ? C20 C16 1.423(5) . ? C20 C25 1.499(5) . ? C19 C18 1.428(5) . ? C19 C24 1.511(5) . ? C4 C3 1.415(5) . ? C9 C14 1.501(5) . ? C16 C17 1.425(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 1.509(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 1.498(5) . ? C18 C23 1.502(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 1.711(8) . ? 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 9.2(5) . . . . ? Dy1 N1 C5 C4 -170.0(3) . . . . ? Dy1 N1 C2 I1 -4.1(3) . . . . ? Dy1 N1 C2 C3 173.5(2) . . . . ? Dy1 C10 C6 C11 123.0(3) . . . . ? Dy1 C10 C6 C7 -66.9(2) . . . . ? Dy1 C10 C9 C8 68.1(2) . . . . ? Dy1 C10 C9 C14 -119.4(3) . . . . ? Dy1 C6 C7 C8 -68.1(2) . . . . ? Dy1 C6 C7 C12 116.6(3) . . . . ? Dy1 C8 C9 C10 -68.4(2) . . . . ? Dy1 C8 C9 C14 119.1(3) . . . . ? Dy1 C8 C7 C6 68.4(2) . . . . ? Dy1 C8 C7 C12 -116.3(3) . . . . ? Dy1 C20 C19 C18 -68.3(2) . . . . ? Dy1 C20 C19 C24 119.9(4) . . . . ? Dy1 C20 C16 C21 -123.8(3) . . . . ? Dy1 C20 C16 C17 66.3(2) . . . . ? Dy1 C19 C18 C17 -67.3(2) . . . . ? Dy1 C19 C18 C23 125.2(3) . . . . ? Dy1 C16 C17 C18 67.8(2) . . . . ? Dy1 C16 C17 C22 -119.1(3) . . . . ? Dy1 C17 C18 C19 66.6(2) . . . . ? Dy1 C17 C18 C23 -126.1(3) . . . . ? I1 C2 C3 I2 -4.6(5) . . . . ? I1 C2 C3 C4 177.8(2) . . . . ? I4 C5 C4 I3 0.7(5) . . . . ? I4 C5 C4 C3 -178.9(2) . . . . ? I3 C4 C3 I2 2.4(5) . . . . ? I3 C4 C3 C2 180.0(2) . . . . ? N1 C5 C4 I3 179.8(2) . . . . ? N1 C5 C4 C3 0.3(4) . . . . ? N1 C2 C3 I2 178.1(2) . . . . ? N1 C2 C3 C4 0.5(4) . . . . ? C5 N1 C2 I1 -177.9(2) . . . . ? C5 N1 C2 C3 -0.3(4) . . . . ? C5 C4 C3 I2 -178.0(3) . . . . ? C5 C4 C3 C2 -0.5(4) . . . . ? C2 N1 C5 I4 179.2(2) . . . . ? C2 N1 C5 C4 0.0(4) . . . . ? C10 C6 C7 Dy1 67.5(2) . . . . ? C10 C6 C7 C8 -0.6(4) . . . . ? C10 C6 C7 C12 -175.8(3) . . . . ? C6 C10 C9 Dy1 -66.8(2) . . . . ? C6 C10 C9 C8 1.2(4) . . . . ? C6 C10 C9 C14 173.8(3) . . . . ? C21 C16 C17 Dy1 123.8(3) . . . . ? C21 C16 C17 C18 -168.4(3) . . . . ? C21 C16 C17 C22 4.6(5) . . . . ? C20 C19 C18 Dy1 68.3(2) . . . . ? C20 C19 C18 C17 1.0(4) . . . . ? C20 C19 C18 C23 -166.5(3) . . . . ? C20 C16 C17 Dy1 -66.1(2) . . . . ? C20 C16 C17 C18 1.7(4) . . . . ? C20 C16 C17 C22 174.8(3) . . . . ? C19 C20 C16 Dy1 -67.3(2) . . . . ? C19 C20 C16 C21 168.9(3) . . . . ? C19 C20 C16 C17 -1.1(4) . . . . ? C9 C10 C6 Dy1 66.5(2) . . . . ? C9 C10 C6 C11 -170.5(3) . . . . ? C9 C10 C6 C7 -0.4(4) . . . . ? C9 C8 C7 Dy1 -67.1(2) . . . . ? C9 C8 C7 C6 1.3(4) . . . . ? C9 C8 C7 C12 176.6(3) . . . . ? C16 C20 C19 Dy1 68.3(2) . . . . ? C16 C20 C19 C18 0.0(4) . . . . ? C16 C20 C19 C24 -171.8(3) . . . . ? C16 C17 C18 Dy1 -68.3(2) . . . . ? C16 C17 C18 C19 -1.7(4) . . . . ? C16 C17 C18 C23 165.7(3) . . . . ? C25 C20 C19 Dy1 -118.5(3) . . . . ? C25 C20 C19 C18 173.2(3) . . . . ? C25 C20 C19 C24 1.4(6) . . . . ? C25 C20 C16 Dy1 119.5(3) . . . . ? C25 C20 C16 C21 -4.3(6) . . . . ? C25 C20 C16 C17 -174.3(3) . . . . ? C15 C10 C6 Dy1 -119.4(3) . . . . ? C15 C10 C6 C11 3.7(5) . . . . ? C15 C10 C6 C7 173.8(3) . . . . ? C15 C10 C9 Dy1 119.2(3) . . . . ? C15 C10 C9 C8 -172.7(3) . . . . ? C15 C10 C9 C14 -0.1(6) . . . . ? C11 C6 C7 Dy1 -122.8(4) . . . . ? C11 C6 C7 C8 169.0(3) . . . . ? C11 C6 C7 C12 -6.2(6) . . . . ? C22 C17 C18 Dy1 118.7(3) . . . . ? C22 C17 C18 C19 -174.7(3) . . . . ? C22 C17 C18 C23 -7.4(6) . . . . ? C7 C8 C9 Dy1 66.8(2) . . . . ? C7 C8 C9 C10 -1.6(4) . . . . ? C7 C8 C9 C14 -174.1(3) . . . . ? C13 C8 C9 Dy1 -126.0(3) . . . . ? C13 C8 C9 C10 165.6(3) . . . . ? C13 C8 C9 C14 -7.0(6) . . . . ? C13 C8 C7 Dy1 125.5(3) . . . . ? C13 C8 C7 C6 -166.1(3) . . . . ? C13 C8 C7 C12 9.1(6) . . . . ? C24 C19 C18 Dy1 -119.6(3) . . . . ? C24 C19 C18 C17 173.1(3) . . . . ? C24 C19 C18 C23 5.6(5) . . . . ? 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 -0.9982 -1.0009 -0.0006 -0.0783 -0.0142 0.0325 -0.9997 1.0000 0.0008 0.0038 0.0040 0.0859 0.9982 1.0009 0.0006 0.0783 0.0142 -0.0325 0.9997 -1.0000 -0.0008 -0.0038 -0.0040 -0.0859 0.0000 -0.0002 -1.0000 -0.0100 0.0322 0.0044 -0.0000 0.0002 1.0000 0.0100 -0.0322 -0.0044 -0.9998 1.0003 2.0008 0.0239 -0.0605 0.0770 0.9998 -1.0003 -2.0008 -0.0239 0.0605 -0.0770 0.9997 -0.9998 0.9992 0.0063 -0.0363 -0.0903 -0.0008 1.0008 2.0007 0.0612 -0.0554 0.0178 1.9987 -0.9994 0.9991 0.0435 -0.0312 -0.1495 -0.0007 1.0001 -1.9993 0.0210 0.0736 0.0356 -0.9989 -0.0008 -1.9999 -0.0574 0.0594 0.0681 -0.9990 -0.0001 2.0001 -0.0172 -0.0696 0.0503 -5.7531 7.2631 -22.4239 -0.1415 0.7602 0.6341