#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:50:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294477 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572197.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_1572197 loop_ _publ_author_name 'Delano, 4th, Francis' 'Benner, Florian' 'Jang, Seoyun' 'Greer, Samuel M.' 'Demir, Selvan' _publ_section_title ; Construction of intermolecular σ-hole interactions in rare earth metallocene complexes using a 2,3,4,5-tetraiodopyrrolyl anion. ; _journal_issue 33 _journal_name_full 'Chemical science' _journal_page_first 13389 _journal_page_last 13404 _journal_paper_doi 10.1039/d4sc03786c _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C24 H30 Dy I4 N, C H2 Cl2' _chemical_formula_sum 'C25 H32 Cl2 Dy I4 N' _chemical_formula_weight 1087.51 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-07-10 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-04-22 deposited with the CCDC. 2024-07-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.907(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3772(2) _cell_length_b 14.3687(3) _cell_length_c 21.3762(5) _cell_measurement_reflns_used 18683 _cell_measurement_temperature 220.0(1) _cell_measurement_theta_max 30.9300 _cell_measurement_theta_min 2.8310 _cell_volume 3118.76(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_temperature 220.0(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 0.840 _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 0.0364618000 _diffrn_orient_matrix_UB_12 0.0415808000 _diffrn_orient_matrix_UB_13 0.0081078000 _diffrn_orient_matrix_UB_21 0.0028659000 _diffrn_orient_matrix_UB_22 0.0065391000 _diffrn_orient_matrix_UB_23 -0.0325737000 _diffrn_orient_matrix_UB_31 -0.0595150000 _diffrn_orient_matrix_UB_32 0.0257900000 _diffrn_orient_matrix_UB_33 -0.0048057000 _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 0.0563 _diffrn_reflns_av_unetI/netI 0.0471 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.840 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 39005 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.840 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.728 _diffrn_reflns_theta_min 2.456 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.541 _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 2.316 _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 1.191 _refine_diff_density_min -1.444 _refine_diff_density_rms 0.156 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8903 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0334 _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^)+(0.0333P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.0792 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7042 _reflns_number_total 8903 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP220K _cod_depositor_comments 'Adding full bibliography for 1572175--1572199.cif.' _cod_original_cell_volume 3118.76(13) _cod_database_code 1572197 _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 0.530 _shelx_estimated_absorpt_t_min 0.206 _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_220_final.res created by SHELXL-2018/3 at 16:37:43 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 10.377207 14.368675 21.376211 90 101.9069 90 ZERR 4 0.000235 0.000316 0.000515 0 0.0023 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Dy I N UNIT 100 128 8 4 16 4 SIMU Cl1B Cl1A L.S. 50 0 0 PLAN 16 SIZE 0.111 0.275 0.353 TEMP -53.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.033300 FVAR 0.61105 DY1 4 0.804138 0.715440 0.339097 11.00000 0.02320 0.02348 = 0.02354 -0.00050 0.00119 0.00304 I1 5 0.524246 0.616463 0.280502 11.00000 0.03601 0.03110 = 0.03686 0.00211 0.00597 -0.00993 I4 5 0.821690 0.939627 0.200472 11.00000 0.03566 0.03783 = 0.04711 0.00630 0.00725 -0.01038 I3 5 0.485258 0.937753 0.081892 11.00000 0.04680 0.04289 = 0.03179 0.00995 0.00501 0.01481 I2 5 0.292969 0.722818 0.129817 11.00000 0.02985 0.05247 = 0.06944 -0.00031 -0.01408 -0.00591 CL2 3 0.608810 0.627217 0.079265 11.00000 0.08102 0.07391 = 0.05504 0.00814 0.01341 0.02640 PART 1 CL1A 3 0.689954 0.446113 0.038240 10.50000 0.08875 0.06475 = 0.22206 -0.03354 0.01827 -0.00143 PART 0 N1 6 0.678207 0.774259 0.241509 11.00000 0.02441 0.03031 = 0.02416 0.00279 0.00047 -0.00276 C5 1 0.668859 0.845470 0.198081 11.00000 0.02647 0.02685 = 0.02726 0.00098 0.00503 -0.00058 C2 1 0.560530 0.729201 0.224933 11.00000 0.02635 0.02750 = 0.02768 0.00304 0.00266 -0.00192 C10 1 0.957210 0.648428 0.264472 11.00000 0.03470 0.02876 = 0.03462 0.00270 0.00969 0.01084 C6 1 0.887890 0.570652 0.280980 11.00000 0.02872 0.02931 = 0.04183 -0.00539 0.00743 0.00355 C8 1 1.028623 0.621457 0.371711 11.00000 0.03207 0.04363 = 0.04219 -0.00412 0.00262 0.01832 C21 1 0.519974 0.737657 0.424223 11.00000 0.03098 0.06935 = 0.05303 -0.01497 0.01386 -0.00405 AFIX 137 H21A 2 0.456149 0.755395 0.386242 11.00000 -1.50000 H21B 2 0.494740 0.764192 0.461661 11.00000 -1.50000 H21C 2 0.522719 0.670367 0.427901 11.00000 -1.50000 AFIX 0 C20 1 0.681131 0.853066 0.385361 11.00000 0.04608 0.03009 = 0.02893 -0.00167 0.00560 0.01178 C19 1 0.817375 0.872346 0.403604 11.00000 0.05099 0.02358 = 0.03245 -0.00545 0.01417 -0.00381 C4 1 0.549419 0.844863 0.155583 11.00000 0.03093 0.03072 = 0.02559 0.00234 0.00313 0.00636 C9 1 1.043084 0.679767 0.320505 11.00000 0.02359 0.03593 = 0.05465 -0.00647 0.00904 -0.00089 C3 1 0.477714 0.769057 0.173196 11.00000 0.02361 0.03167 = 0.02893 -0.00059 0.00019 0.00107 C16 1 0.654444 0.773513 0.419336 11.00000 0.03412 0.03498 = 0.02810 -0.00398 0.00610 0.00385 C25 1 0.580188 0.913136 0.342761 11.00000 0.07731 0.05498 = 0.04200 0.00416 0.00657 0.03815 AFIX 137 H25A 2 0.622867 0.949493 0.314618 11.00000 -1.50000 H25B 2 0.539708 0.954643 0.368888 11.00000 -1.50000 H25C 2 0.513115 0.873877 0.317397 11.00000 -1.50000 AFIX 0 C15 1 0.952445 0.681525 0.197953 11.00000 0.07219 0.06458 = 0.04739 0.01008 0.03072 0.02143 AFIX 137 H15A 2 0.861600 0.683956 0.174914 11.00000 -1.50000 H15B 2 1.001604 0.639002 0.176478 11.00000 -1.50000 H15C 2 0.991030 0.743156 0.199175 11.00000 -1.50000 AFIX 0 C12 1 0.888020 0.475212 0.384092 11.00000 0.07270 0.04438 = 0.08867 0.03114 0.03730 0.02143 AFIX 137 H12A 2 0.894669 0.493809 0.428266 11.00000 -1.50000 H12B 2 0.945142 0.422273 0.382292 11.00000 -1.50000 H12C 2 0.797707 0.458192 0.365672 11.00000 -1.50000 AFIX 0 C11 1 0.801363 0.508969 0.233295 11.00000 0.04668 0.05769 = 0.07515 -0.03338 0.00564 0.00349 AFIX 137 H11A 2 0.750273 0.468663 0.255310 11.00000 -1.50000 H11B 2 0.855605 0.471357 0.211231 11.00000 -1.50000 H11C 2 0.742296 0.547026 0.202529 11.00000 -1.50000 AFIX 0 C14 1 1.145218 0.755453 0.323202 11.00000 0.04041 0.05567 = 0.10358 -0.01307 0.02090 -0.01273 AFIX 137 H14A 2 1.106894 0.807640 0.297066 11.00000 -1.50000 H14B 2 1.219594 0.731436 0.307193 11.00000 -1.50000 H14C 2 1.174718 0.775859 0.367079 11.00000 -1.50000 AFIX 0 C17 1 0.774620 0.742713 0.458492 11.00000 0.03686 0.03271 = 0.02633 -0.00267 0.00566 0.00342 C18 1 0.875035 0.804569 0.448969 11.00000 0.03286 0.03986 = 0.02710 -0.00774 0.00473 0.00204 C22 1 0.789205 0.664594 0.506642 11.00000 0.06476 0.05085 = 0.04354 0.01900 0.01611 0.01384 AFIX 137 H22A 2 0.712489 0.624482 0.496915 11.00000 -1.50000 H22B 2 0.796974 0.690336 0.549207 11.00000 -1.50000 H22C 2 0.867527 0.628760 0.504750 11.00000 -1.50000 AFIX 0 C7 1 0.929099 0.554713 0.347019 11.00000 0.03477 0.02995 = 0.04560 0.01146 0.01431 0.01274 C23 1 1.010767 0.811455 0.490876 11.00000 0.03920 0.07070 = 0.04993 -0.02722 -0.00541 -0.00397 AFIX 137 H23A 2 1.031170 0.754139 0.514849 11.00000 -1.50000 H23B 2 1.013401 0.863130 0.520312 11.00000 -1.50000 H23C 2 1.075008 0.821523 0.464415 11.00000 -1.50000 AFIX 0 C13 1 1.118850 0.614604 0.436139 11.00000 0.06403 0.09116 = 0.04473 -0.01283 -0.01620 0.04311 AFIX 137 H13A 2 1.168154 0.672078 0.445336 11.00000 -1.50000 H13B 2 1.179460 0.563188 0.436226 11.00000 -1.50000 H13C 2 1.067269 0.604114 0.468511 11.00000 -1.50000 AFIX 0 C24 1 0.889554 0.956591 0.386560 11.00000 0.09565 0.03751 = 0.05904 -0.00814 0.03271 -0.02175 AFIX 137 H24A 2 0.964284 0.936743 0.369124 11.00000 -1.50000 H24B 2 0.920280 0.993755 0.424595 11.00000 -1.50000 H24C 2 0.830551 0.993492 0.354992 11.00000 -1.50000 AFIX 0 C26 1 0.696388 0.558800 0.037354 11.00000 0.18750 0.06361 = 0.10434 0.02336 0.10556 0.01893 PART 1 AFIX 23 H26C 2 0.670872 0.577829 -0.007526 10.50000 -1.20000 H26D 2 0.789230 0.575878 0.051666 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.656118 0.563660 -0.008216 10.50000 -1.20000 H26B 2 0.786009 0.583688 0.043222 10.50000 -1.20000 AFIX 0 CL1B 3 0.706023 0.445575 0.057633 10.50000 0.10038 0.06604 = 0.06437 0.02029 0.02739 0.03416 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0792, GooF = S = 1.054, Restrained GooF = 1.053 for all data REM R1 = 0.0334 for 7042 Fo > 4sig(Fo) and 0.0467 for all 8903 data REM 317 parameters refined using 6 restraints END WGHT 0.0333 0.0000 REM Highest difference peak 1.191, deepest hole -1.444, 1-sigma level 0.156 Q1 1 0.2899 0.7467 0.1608 11.00000 0.05 1.19 Q2 1 0.7904 0.4868 0.0592 11.00000 0.05 0.83 Q3 1 0.7144 0.7538 0.3413 11.00000 0.05 0.82 Q4 1 0.4767 0.8827 0.0733 11.00000 0.05 0.66 Q5 1 0.7392 0.6560 0.3388 11.00000 0.05 0.63 Q6 1 0.4582 0.5640 0.2815 11.00000 0.05 0.62 Q7 1 0.8672 0.7637 0.3395 11.00000 0.05 0.60 Q8 1 0.8093 0.7833 0.3406 11.00000 0.05 0.58 Q9 1 0.7992 0.8531 0.3378 11.00000 0.05 0.57 Q10 1 0.4155 0.9857 0.0793 11.00000 0.05 0.57 Q11 1 1.0964 0.7188 0.1978 11.00000 0.05 0.56 Q12 1 0.7640 0.6022 0.0190 11.00000 0.05 0.55 Q13 1 0.7291 0.5638 0.0596 11.00000 0.05 0.55 Q14 1 0.5581 0.9531 0.0833 11.00000 0.05 0.53 Q15 1 1.3202 0.6190 0.3235 11.00000 0.05 0.53 Q16 1 0.9637 0.7065 0.2965 11.00000 0.05 0.53 ; _shelx_res_checksum 44321 _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 2.585 _oxdiff_exptl_absorpt_empirical_full_min 0.629 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 0.80414(2) 0.71544(2) 0.33910(2) 0.02392(5) Uani 1 1 d . . . . . I1 I 0.52425(3) 0.61646(2) 0.28050(2) 0.03488(7) Uani 1 1 d . . . . . I4 I 0.82169(3) 0.93963(2) 0.20047(2) 0.04038(8) Uani 1 1 d . . . . . I3 I 0.48526(3) 0.93775(2) 0.08189(2) 0.04094(8) Uani 1 1 d . . . . . I2 I 0.29297(3) 0.72282(2) 0.12982(2) 0.05408(10) Uani 1 1 d . . . . . Cl2 Cl 0.60881(16) 0.62722(11) 0.07926(8) 0.0701(4) Uani 1 1 d . . . . . Cl1A Cl 0.6900(12) 0.4461(7) 0.0382(6) 0.127(4) Uani 0.5 1 d . U P A 1 N1 N 0.6782(3) 0.7743(2) 0.24151(15) 0.0269(6) Uani 1 1 d . . . . . C5 C 0.6689(4) 0.8455(2) 0.19808(18) 0.0269(7) Uani 1 1 d . . . . . C2 C 0.5605(4) 0.7292(2) 0.22493(18) 0.0276(8) Uani 1 1 d . . . . . C10 C 0.9572(4) 0.6484(3) 0.2645(2) 0.0323(8) Uani 1 1 d . . . . . C6 C 0.8879(4) 0.5707(3) 0.2810(2) 0.0333(9) Uani 1 1 d . . . . . C8 C 1.0286(4) 0.6215(3) 0.3717(2) 0.0400(10) Uani 1 1 d . . . . . C21 C 0.5200(4) 0.7377(4) 0.4242(3) 0.0504(12) Uani 1 1 d . . . . . H21A H 0.456149 0.755395 0.386242 0.076 Uiso 1 1 calc R U . . . H21B H 0.494740 0.764192 0.461661 0.076 Uiso 1 1 calc R U . . . H21C H 0.522719 0.670367 0.427901 0.076 Uiso 1 1 calc R U . . . C20 C 0.6811(4) 0.8531(3) 0.3854(2) 0.0353(9) Uani 1 1 d . . . . . C19 C 0.8174(4) 0.8723(3) 0.4036(2) 0.0349(9) Uani 1 1 d . . . . . C4 C 0.5494(4) 0.8449(3) 0.15558(19) 0.0295(8) Uani 1 1 d . . . . . C9 C 1.0431(4) 0.6798(3) 0.3205(2) 0.0379(10) Uani 1 1 d . . . . . C3 C 0.4777(4) 0.7691(3) 0.17320(19) 0.0288(8) Uani 1 1 d . . . . . C16 C 0.6544(4) 0.7735(3) 0.4193(2) 0.0324(8) Uani 1 1 d . . . . . C25 C 0.5802(6) 0.9131(4) 0.3428(3) 0.0589(15) Uani 1 1 d . . . . . H25A H 0.622867 0.949493 0.314618 0.088 Uiso 1 1 calc R U . . . H25B H 0.539708 0.954643 0.368888 0.088 Uiso 1 1 calc R U . . . H25C H 0.513115 0.873877 0.317397 0.088 Uiso 1 1 calc R U . . . C15 C 0.9524(6) 0.6815(4) 0.1980(3) 0.0587(14) Uani 1 1 d . . . . . H15A H 0.861600 0.683956 0.174914 0.088 Uiso 1 1 calc R U . . . H15B H 1.001604 0.639002 0.176478 0.088 Uiso 1 1 calc R U . . . H15C H 0.991030 0.743156 0.199175 0.088 Uiso 1 1 calc R U . . . C12 C 0.8880(6) 0.4752(4) 0.3841(3) 0.0656(17) Uani 1 1 d . . . . . H12A H 0.894669 0.493809 0.428266 0.098 Uiso 1 1 calc R U . . . H12B H 0.945142 0.422273 0.382292 0.098 Uiso 1 1 calc R U . . . H12C H 0.797707 0.458192 0.365672 0.098 Uiso 1 1 calc R U . . . C11 C 0.8014(5) 0.5090(4) 0.2333(3) 0.0608(15) Uani 1 1 d . . . . . H11A H 0.750273 0.468663 0.255310 0.091 Uiso 1 1 calc R U . . . H11B H 0.855605 0.471357 0.211231 0.091 Uiso 1 1 calc R U . . . H11C H 0.742296 0.547026 0.202529 0.091 Uiso 1 1 calc R U . . . C14 C 1.1452(5) 0.7555(4) 0.3232(3) 0.0657(17) Uani 1 1 d . . . . . H14A H 1.106894 0.807640 0.297066 0.099 Uiso 1 1 calc R U . . . H14B H 1.219594 0.731436 0.307193 0.099 Uiso 1 1 calc R U . . . H14C H 1.174718 0.775859 0.367079 0.099 Uiso 1 1 calc R U . . . C17 C 0.7746(4) 0.7427(3) 0.45849(19) 0.0321(8) Uani 1 1 d . . . . . C18 C 0.8750(4) 0.8046(3) 0.4490(2) 0.0335(8) Uani 1 1 d . . . . . C22 C 0.7892(5) 0.6646(3) 0.5066(2) 0.0523(12) Uani 1 1 d . . . . . H22A H 0.712489 0.624482 0.496915 0.079 Uiso 1 1 calc R U . . . H22B H 0.796974 0.690336 0.549207 0.079 Uiso 1 1 calc R U . . . H22C H 0.867527 0.628760 0.504750 0.079 Uiso 1 1 calc R U . . . C7 C 0.9291(4) 0.5547(3) 0.3470(2) 0.0359(9) Uani 1 1 d . . . . . C23 C 1.0108(5) 0.8115(4) 0.4909(3) 0.0554(13) Uani 1 1 d . . . . . H23A H 1.031170 0.754139 0.514849 0.083 Uiso 1 1 calc R U . . . H23B H 1.013401 0.863130 0.520312 0.083 Uiso 1 1 calc R U . . . H23C H 1.075008 0.821523 0.464415 0.083 Uiso 1 1 calc R U . . . C13 C 1.1188(6) 0.6146(4) 0.4361(3) 0.0706(18) Uani 1 1 d . . . . . H13A H 1.168154 0.672078 0.445336 0.106 Uiso 1 1 calc R U . . . H13B H 1.179460 0.563188 0.436226 0.106 Uiso 1 1 calc R U . . . H13C H 1.067269 0.604114 0.468511 0.106 Uiso 1 1 calc R U . . . C24 C 0.8896(6) 0.9566(3) 0.3866(3) 0.0617(16) Uani 1 1 d . . . . . H24A H 0.964284 0.936743 0.369124 0.092 Uiso 1 1 calc R U . . . H24B H 0.920280 0.993755 0.424595 0.092 Uiso 1 1 calc R U . . . H24C H 0.830551 0.993492 0.354992 0.092 Uiso 1 1 calc R U . . . C26 C 0.6964(11) 0.5588(4) 0.0374(4) 0.108(3) Uani 1 1 d . . . . . H26C H 0.670872 0.577829 -0.007526 0.129 Uiso 0.5 1 calc R U P A 1 H26D H 0.789230 0.575878 0.051666 0.129 Uiso 0.5 1 calc R U P A 1 H26A H 0.656118 0.563660 -0.008216 0.129 Uiso 0.5 1 calc R U P A -1 H26B H 0.786009 0.583688 0.043222 0.129 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7060(10) 0.4456(7) 0.0576(3) 0.075(2) Uani 0.5 1 d . U P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02320(9) 0.02348(9) 0.02354(9) -0.00050(6) 0.00119(6) 0.00304(6) I1 0.03601(15) 0.03110(13) 0.03686(15) 0.00211(10) 0.00597(11) -0.00993(10) I4 0.03566(15) 0.03783(15) 0.04711(18) 0.00630(12) 0.00725(12) -0.01038(10) I3 0.04680(17) 0.04289(16) 0.03179(15) 0.00995(11) 0.00501(12) 0.01481(11) I2 0.02985(16) 0.05247(19) 0.0694(2) -0.00031(15) -0.01408(14) -0.00591(11) Cl2 0.0810(10) 0.0739(9) 0.0550(9) 0.0081(7) 0.0134(7) 0.0264(7) Cl1A 0.089(4) 0.065(4) 0.222(11) -0.034(6) 0.018(7) -0.001(3) N1 0.0244(16) 0.0303(16) 0.0242(16) 0.0028(12) 0.0005(12) -0.0028(11) C5 0.0265(18) 0.0268(17) 0.0273(19) 0.0010(15) 0.0050(14) -0.0006(13) C2 0.0264(19) 0.0275(18) 0.028(2) 0.0030(14) 0.0027(15) -0.0019(13) C10 0.035(2) 0.0288(19) 0.035(2) 0.0027(16) 0.0097(17) 0.0108(15) C6 0.029(2) 0.0293(19) 0.042(2) -0.0054(17) 0.0074(17) 0.0036(14) C8 0.032(2) 0.044(2) 0.042(3) -0.0041(19) 0.0026(18) 0.0183(17) C21 0.031(2) 0.069(3) 0.053(3) -0.015(3) 0.014(2) -0.004(2) C20 0.046(2) 0.0301(19) 0.029(2) -0.0017(16) 0.0056(17) 0.0118(16) C19 0.051(3) 0.0236(18) 0.032(2) -0.0054(16) 0.0142(19) -0.0038(16) C4 0.031(2) 0.0307(19) 0.0256(19) 0.0023(15) 0.0031(15) 0.0064(14) C9 0.0236(19) 0.036(2) 0.055(3) -0.0065(19) 0.0090(18) -0.0009(15) C3 0.0236(18) 0.0317(19) 0.029(2) -0.0006(15) 0.0002(15) 0.0011(14) C16 0.034(2) 0.035(2) 0.028(2) -0.0040(16) 0.0061(16) 0.0039(15) C25 0.077(4) 0.055(3) 0.042(3) 0.004(2) 0.007(3) 0.038(3) C15 0.072(4) 0.065(3) 0.047(3) 0.010(3) 0.031(3) 0.021(3) C12 0.073(4) 0.044(3) 0.089(5) 0.031(3) 0.037(3) 0.021(3) C11 0.047(3) 0.058(3) 0.075(4) -0.033(3) 0.006(3) 0.003(2) C14 0.040(3) 0.056(3) 0.104(5) -0.013(3) 0.021(3) -0.013(2) C17 0.037(2) 0.0327(19) 0.026(2) -0.0027(16) 0.0057(16) 0.0034(16) C18 0.033(2) 0.040(2) 0.027(2) -0.0077(17) 0.0047(16) 0.0020(16) C22 0.065(3) 0.051(3) 0.044(3) 0.019(2) 0.016(2) 0.014(2) C7 0.035(2) 0.030(2) 0.046(3) 0.0115(17) 0.0143(19) 0.0127(15) C23 0.039(3) 0.071(3) 0.050(3) -0.027(3) -0.005(2) -0.004(2) C13 0.064(4) 0.091(4) 0.045(3) -0.013(3) -0.016(3) 0.043(3) C24 0.096(4) 0.038(3) 0.059(4) -0.008(2) 0.033(3) -0.022(3) C26 0.188(9) 0.064(4) 0.104(6) 0.023(4) 0.106(7) 0.019(4) Cl1B 0.100(5) 0.066(3) 0.064(2) 0.020(2) 0.027(3) 0.034(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 -1 0 0.1241 -1 1 0 0.1231 1 1 0 0.1293 1 -1 0 0.1498 0 0 -1 0.0585 0 0 1 0.0528 -1 1 2 0.0993 1 -1 -2 0.1399 1 -1 1 0.1333 0 1 2 0.0924 2 -1 1 0.1448 0 1 -2 0.0988 -1 0 -2 0.1081 -1 0 2 0.1036 -6 6 -23 0.0941 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Dy1 I1 62.01(7) . . ? N1 Dy1 C10 83.70(11) . . ? N1 Dy1 C6 92.39(12) . . ? N1 Dy1 C8 134.77(13) . . ? N1 Dy1 C20 80.93(12) . . ? N1 Dy1 C19 96.61(12) . . ? N1 Dy1 C9 107.47(13) . . ? N1 Dy1 C16 99.50(12) . . ? N1 Dy1 C17 129.65(11) . . ? N1 Dy1 C18 127.56(12) . . ? N1 Dy1 C7 122.81(13) . . ? C10 Dy1 I1 102.01(9) . . ? C10 Dy1 C6 30.84(12) . . ? C10 Dy1 C8 51.13(13) . . ? C10 Dy1 C16 176.28(12) . . ? C10 Dy1 C17 146.26(12) . . ? C6 Dy1 I1 80.19(9) . . ? C6 Dy1 C16 146.39(12) . . ? C6 Dy1 C17 132.57(13) . . ? C8 Dy1 I1 123.01(10) . . ? C8 Dy1 C6 51.09(13) . . ? C8 Dy1 C16 125.73(14) . . ? C8 Dy1 C17 95.24(13) . . ? C20 Dy1 I1 90.54(10) . . ? C20 Dy1 C10 152.66(13) . . ? C20 Dy1 C6 170.39(13) . . ? C20 Dy1 C8 138.06(14) . . ? C20 Dy1 C16 30.74(12) . . ? C20 Dy1 C17 51.20(12) . . ? C19 Dy1 I1 121.58(10) . . ? C19 Dy1 C10 130.76(13) . . ? C19 Dy1 C6 158.16(13) . . ? C19 Dy1 C8 110.46(14) . . ? C19 Dy1 C20 31.04(14) . . ? C19 Dy1 C9 107.22(13) . . ? C19 Dy1 C16 51.02(12) . . ? C19 Dy1 C17 51.34(12) . . ? C19 Dy1 C18 31.16(13) . . ? C19 Dy1 C7 138.15(15) . . ? C9 Dy1 I1 130.57(9) . . ? C9 Dy1 C10 30.91(13) . . ? C9 Dy1 C6 50.98(12) . . ? C9 Dy1 C8 30.88(14) . . ? C9 Dy1 C20 137.70(13) . . ? C9 Dy1 C16 147.64(14) . . ? C9 Dy1 C17 118.05(14) . . ? C9 Dy1 C18 97.46(13) . . ? C16 Dy1 I1 78.00(9) . . ? C17 Dy1 I1 99.43(9) . . ? C17 Dy1 C16 30.90(12) . . ? C18 Dy1 I1 128.20(9) . . ? C18 Dy1 C10 128.22(13) . . ? C18 Dy1 C6 137.42(13) . . ? C18 Dy1 C8 86.84(13) . . ? C18 Dy1 C20 51.29(13) . . ? C18 Dy1 C16 51.01(12) . . ? C18 Dy1 C17 30.96(12) . . ? C7 Dy1 I1 91.72(10) . . ? C7 Dy1 C10 51.19(13) . . ? C7 Dy1 C6 30.80(14) . . ? C7 Dy1 C8 31.29(14) . . ? C7 Dy1 C20 153.76(13) . . ? C7 Dy1 C9 51.33(13) . . ? C7 Dy1 C16 125.11(13) . . ? C7 Dy1 C17 102.69(13) . . ? C7 Dy1 C18 108.92(14) . . ? C2 I1 Dy1 68.13(10) . . ? C5 N1 Dy1 144.0(2) . . ? C2 N1 Dy1 111.1(2) . . ? C2 N1 C5 104.1(3) . . ? N1 C5 I4 121.5(3) . . ? N1 C5 C4 111.7(3) . . ? C4 C5 I4 126.8(3) . . ? N1 C2 I1 118.5(3) . . ? N1 C2 C3 112.9(3) . . ? C3 C2 I1 128.6(3) . . ? C6 C10 Dy1 74.8(2) . . ? C6 C10 C15 124.9(4) . . ? C9 C10 Dy1 74.1(2) . . ? C9 C10 C6 107.8(4) . . ? C9 C10 C15 126.8(4) . . ? C15 C10 Dy1 123.5(3) . . ? C10 C6 Dy1 74.3(2) . . ? C10 C6 C11 124.2(4) . . ? C11 C6 Dy1 124.9(3) . . ? C7 C6 Dy1 73.7(2) . . ? C7 C6 C10 108.3(4) . . ? C7 C6 C11 126.9(4) . . ? C9 C8 Dy1 73.9(2) . . ? C9 C8 C7 107.3(4) . . ? C9 C8 C13 127.2(5) . . ? C7 C8 Dy1 73.5(2) . . ? C7 C8 C13 124.2(5) . . ? 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 C25 125.7(4) . . ? C16 C20 Dy1 75.5(2) . . ? C16 C20 C19 107.9(4) . . ? C16 C20 C25 126.0(4) . . ? C25 C20 Dy1 121.9(3) . . ? C20 C19 Dy1 75.3(2) . . ? C20 C19 C18 108.1(3) . . ? C20 C19 C24 127.5(4) . . ? C18 C19 Dy1 74.9(2) . . ? C18 C19 C24 123.8(5) . . ? C24 C19 Dy1 122.4(3) . . ? C5 C4 I3 127.1(3) . . ? C5 C4 C3 106.3(3) . . ? C3 C4 I3 126.6(3) . . ? C10 C9 Dy1 75.0(2) . . ? C10 C9 C8 108.6(4) . . ? C10 C9 C14 125.2(5) . . ? C8 C9 Dy1 75.2(2) . . ? C8 C9 C14 125.7(5) . . ? C14 C9 Dy1 121.8(3) . . ? C2 C3 I2 126.6(3) . . ? C2 C3 C4 105.0(3) . . ? C4 C3 I2 128.4(3) . . ? C21 C16 Dy1 127.2(3) . . ? C20 C16 Dy1 73.8(2) . . ? C20 C16 C21 126.4(4) . . ? C20 C16 C17 108.3(4) . . ? C17 C16 Dy1 74.1(2) . . ? C17 C16 C21 124.3(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 75.0(2) . . ? C16 C17 C22 125.8(4) . . ? C18 C17 Dy1 73.8(2) . . ? C18 C17 C16 107.6(4) . . ? C18 C17 C22 126.3(4) . . ? C22 C17 Dy1 122.0(3) . . ? C19 C18 Dy1 74.0(2) . . ? C19 C18 C23 124.9(4) . . ? C17 C18 Dy1 75.2(2) . . ? C17 C18 C19 108.1(4) . . ? C17 C18 C23 125.5(4) . . ? C23 C18 Dy1 127.9(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 75.5(2) . . ? C6 C7 C8 108.0(4) . . ? C6 C7 C12 126.4(5) . . ? C8 C7 Dy1 75.2(2) . . ? C8 C7 C12 125.3(5) . . ? C12 C7 Dy1 120.7(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 108.4 . . ? Cl2 C26 H26B 108.4 . . ? Cl1A C26 Cl2 122.7(6) . . ? Cl1A C26 H26C 106.7 . . ? Cl1A C26 H26D 106.7 . . ? Cl1A C26 H26A 94.2 . . ? Cl1A C26 H26B 113.8 . . ? Cl1A C26 Cl1B 14.2(6) . . ? H26C C26 H26D 106.6 . . ? H26C C26 H26A 14.9 . . ? H26C C26 H26B 94.7 . . ? H26D C26 H26A 118.9 . . ? H26D C26 H26B 12.3 . . ? H26A C26 H26B 107.5 . . ? Cl1B C26 Cl2 115.5(4) . . ? Cl1B C26 H26C 120.8 . . ? Cl1B C26 H26D 99.2 . . ? Cl1B C26 H26A 108.4 . . ? Cl1B C26 H26B 108.4 . . ? 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 3.2444(3) . ? Dy1 N1 2.377(3) . ? Dy1 C10 2.653(4) . ? Dy1 C6 2.659(4) . ? Dy1 C8 2.658(4) . ? Dy1 C20 2.653(4) . ? Dy1 C19 2.632(4) . ? Dy1 C9 2.641(4) . ? Dy1 C16 2.674(4) . ? Dy1 C17 2.662(4) . ? Dy1 C18 2.643(4) . ? Dy1 C7 2.637(4) . ? I1 C2 2.088(4) . ? I4 C5 2.077(4) . ? I3 C4 2.067(4) . ? I2 C3 2.060(4) . ? Cl2 C26 1.712(7) . ? Cl1A C26 1.621(12) . ? N1 C5 1.371(5) . ? N1 C2 1.363(5) . ? C5 C4 1.377(5) . ? C2 C3 1.377(5) . ? C10 C6 1.413(6) . ? C10 C9 1.411(6) . ? C10 C15 1.490(6) . ? C6 C11 1.501(6) . ? C6 C7 1.407(6) . ? C8 C9 1.411(6) . ? C8 C7 1.428(6) . ? C8 C13 1.500(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21 C16 1.511(6) . ? C20 C19 1.414(6) . ? C20 C16 1.412(6) . ? C20 C25 1.509(6) . ? C19 C18 1.417(6) . ? C19 C24 1.507(6) . ? C4 C3 1.413(5) . ? C9 C14 1.511(6) . ? C16 C17 1.422(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C12 C7 1.501(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C17 C18 1.416(6) . ? C17 C22 1.509(6) . ? C18 C23 1.508(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 Cl1B 1.681(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 11.8(6) . . . . ? Dy1 N1 C5 C4 -167.9(3) . . . . ? Dy1 N1 C2 I1 -5.3(3) . . . . ? Dy1 N1 C2 C3 172.2(3) . . . . ? Dy1 C10 C6 C11 121.8(4) . . . . ? Dy1 C10 C6 C7 -66.4(3) . . . . ? Dy1 C10 C9 C8 68.4(3) . . . . ? Dy1 C10 C9 C14 -118.6(4) . . . . ? Dy1 C6 C7 C8 -68.8(3) . . . . ? Dy1 C6 C7 C12 117.7(4) . . . . ? Dy1 C8 C9 C10 -68.2(3) . . . . ? Dy1 C8 C9 C14 118.8(4) . . . . ? Dy1 C8 C7 C6 69.0(3) . . . . ? Dy1 C8 C7 C12 -117.4(4) . . . . ? Dy1 C20 C19 C18 -68.3(3) . . . . ? Dy1 C20 C19 C24 119.8(4) . . . . ? Dy1 C20 C16 C21 -124.6(4) . . . . ? Dy1 C20 C16 C17 66.6(3) . . . . ? Dy1 C19 C18 C17 -68.1(3) . . . . ? Dy1 C19 C18 C23 125.4(4) . . . . ? Dy1 C16 C17 C18 67.2(3) . . . . ? Dy1 C16 C17 C22 -118.9(4) . . . . ? Dy1 C17 C18 C19 67.3(3) . . . . ? Dy1 C17 C18 C23 -126.3(4) . . . . ? I1 C2 C3 I2 -4.8(5) . . . . ? I1 C2 C3 C4 177.6(3) . . . . ? I4 C5 C4 I3 -0.5(5) . . . . ? I4 C5 C4 C3 -179.3(3) . . . . ? I3 C4 C3 I2 3.1(5) . . . . ? I3 C4 C3 C2 -179.2(3) . . . . ? N1 C5 C4 I3 179.2(3) . . . . ? N1 C5 C4 C3 0.4(4) . . . . ? N1 C2 C3 I2 178.1(3) . . . . ? N1 C2 C3 C4 0.4(5) . . . . ? C5 N1 C2 I1 -177.6(2) . . . . ? C5 N1 C2 C3 -0.2(4) . . . . ? C5 C4 C3 I2 -178.1(3) . . . . ? C5 C4 C3 C2 -0.5(4) . . . . ? C2 N1 C5 I4 179.5(3) . . . . ? C2 N1 C5 C4 -0.2(4) . . . . ? C10 C6 C7 Dy1 66.9(3) . . . . ? C10 C6 C7 C8 -1.9(4) . . . . ? C10 C6 C7 C12 -175.4(4) . . . . ? C6 C10 C9 Dy1 -67.8(3) . . . . ? C6 C10 C9 C8 0.6(4) . . . . ? C6 C10 C9 C14 173.5(4) . . . . ? C21 C16 C17 Dy1 124.5(4) . . . . ? C21 C16 C17 C18 -168.3(4) . . . . ? C21 C16 C17 C22 5.7(6) . . . . ? C20 C19 C18 Dy1 68.6(3) . . . . ? C20 C19 C18 C17 0.5(4) . . . . ? C20 C19 C18 C23 -166.0(4) . . . . ? C20 C16 C17 Dy1 -66.4(3) . . . . ? C20 C16 C17 C18 0.7(4) . . . . ? C20 C16 C17 C22 174.7(4) . . . . ? C19 C20 C16 Dy1 -67.1(3) . . . . ? C19 C20 C16 C21 168.3(4) . . . . ? C19 C20 C16 C17 -0.4(4) . . . . ? C9 C10 C6 Dy1 67.3(3) . . . . ? C9 C10 C6 C11 -170.9(4) . . . . ? C9 C10 C6 C7 0.9(4) . . . . ? C9 C8 C7 Dy1 -66.7(3) . . . . ? C9 C8 C7 C6 2.3(4) . . . . ? C9 C8 C7 C12 175.9(4) . . . . ? C16 C20 C19 Dy1 68.3(3) . . . . ? C16 C20 C19 C18 0.0(4) . . . . ? C16 C20 C19 C24 -171.9(4) . . . . ? C16 C17 C18 Dy1 -68.0(3) . . . . ? C16 C17 C18 C19 -0.7(4) . . . . ? C16 C17 C18 C23 165.7(4) . . . . ? C25 C20 C19 Dy1 -117.9(4) . . . . ? C25 C20 C19 C18 173.8(4) . . . . ? C25 C20 C19 C24 2.0(7) . . . . ? C25 C20 C16 Dy1 119.1(4) . . . . ? C25 C20 C16 C21 -5.5(7) . . . . ? C25 C20 C16 C17 -174.3(4) . . . . ? C15 C10 C6 Dy1 -120.5(4) . . . . ? C15 C10 C6 C11 1.3(6) . . . . ? C15 C10 C6 C7 173.1(4) . . . . ? C15 C10 C9 Dy1 120.2(4) . . . . ? C15 C10 C9 C8 -171.4(4) . . . . ? C15 C10 C9 C14 1.5(7) . . . . ? C11 C6 C7 Dy1 -121.7(4) . . . . ? C11 C6 C7 C8 169.5(4) . . . . ? C11 C6 C7 C12 -4.0(7) . . . . ? C22 C17 C18 Dy1 118.1(4) . . . . ? C22 C17 C18 C19 -174.7(4) . . . . ? C22 C17 C18 C23 -8.3(7) . . . . ? C7 C8 C9 Dy1 66.5(3) . . . . ? C7 C8 C9 C10 -1.7(4) . . . . ? C7 C8 C9 C14 -174.7(4) . . . . ? C13 C8 C9 Dy1 -126.3(4) . . . . ? C13 C8 C9 C10 165.4(4) . . . . ? C13 C8 C9 C14 -7.5(7) . . . . ? C13 C8 C7 Dy1 125.6(4) . . . . ? C13 C8 C7 C6 -165.4(4) . . . . ? C13 C8 C7 C12 8.2(7) . . . . ? C24 C19 C18 Dy1 -119.2(4) . . . . ? C24 C19 C18 C17 172.7(4) . . . . ? C24 C19 C18 C23 6.2(7) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1.0038 -1.0310 0.1394 -0.0783 -0.0142 0.0325 -1.0150 0.9840 -0.0153 0.0038 0.0040 0.0859 1.0038 1.0310 -0.1394 0.0783 0.0142 -0.0325 1.0150 -0.9840 0.0153 -0.0038 -0.0040 -0.0859 -0.0104 -0.0378 -0.9985 -0.0100 0.0322 0.0044 0.0104 0.0378 0.9985 0.0100 -0.0322 -0.0044 -0.9941 1.0596 1.9817 0.0239 -0.0605 0.0770 0.9941 -1.0596 -1.9817 -0.0239 0.0605 -0.0770 1.0254 -0.9462 1.0138 0.0063 -0.0363 -0.0903 0.0152 1.0831 1.9196 0.0612 -0.0554 0.0178 2.0348 -0.9227 0.9518 0.0435 -0.0312 -0.1495 -0.0265 0.9318 -2.0744 0.0210 0.0736 0.0356 -1.0303 -0.0991 -1.9349 -0.0574 0.0594 0.0681 -0.9885 0.0521 2.0591 -0.0172 -0.0696 0.0503 -6.0831 6.3371 -22.6009 -0.1415 0.7602 0.6341