#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:50:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294477 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572193.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_1572193 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 101.856(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3697(2) _cell_length_b 14.3573(3) _cell_length_c 21.3576(5) _cell_measurement_reflns_used 19056 _cell_measurement_temperature 210.0(1) _cell_measurement_theta_max 30.9980 _cell_measurement_theta_min 2.8350 _cell_volume 3111.91(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 210.0(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 0.846 _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 0.0364081000 _diffrn_orient_matrix_UB_12 0.0415859000 _diffrn_orient_matrix_UB_13 0.0082960000 _diffrn_orient_matrix_UB_21 0.0033935000 _diffrn_orient_matrix_UB_22 0.0066937000 _diffrn_orient_matrix_UB_23 -0.0325331000 _diffrn_orient_matrix_UB_31 -0.0595582000 _diffrn_orient_matrix_UB_32 0.0258082000 _diffrn_orient_matrix_UB_33 -0.0049480000 _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 0.0558 _diffrn_reflns_av_unetI/netI 0.0463 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.846 _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 38782 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.846 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.653 _diffrn_reflns_theta_min 2.458 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.556 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.229 _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 2.321 _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 1.121 _refine_diff_density_min -1.468 _refine_diff_density_rms 0.162 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8878 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0331 _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^)+(0.0327P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.0773 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7070 _reflns_number_total 8878 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP210K _cod_depositor_comments 'Adding full bibliography for 1572175--1572199.cif.' _cod_original_cell_volume 3111.93(12) _cod_database_code 1572193 _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_210_final.res created by SHELXL-2018/3 at 16:32:47 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 10.369727 14.357337 21.357633 90 101.856 90 ZERR 4 0.000228 0.000308 0.000503 0 0.0022 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. 30 0 0 PLAN 16 SIZE 0.111 0.275 0.353 TEMP -63.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.032700 FVAR 0.62081 DY1 4 0.804210 0.715238 0.339162 11.00000 0.02182 0.02286 = 0.02186 -0.00048 0.00095 0.00301 I1 5 0.524485 0.616068 0.280767 11.00000 0.03390 0.02966 = 0.03486 0.00195 0.00552 -0.00928 I4 5 0.821512 0.939652 0.200496 11.00000 0.03369 0.03617 = 0.04442 0.00592 0.00661 -0.00981 I3 5 0.484796 0.937478 0.081799 11.00000 0.04396 0.04092 = 0.02999 0.00942 0.00470 0.01387 I2 5 0.292745 0.722375 0.129997 11.00000 0.02808 0.04966 = 0.06622 -0.00021 -0.01340 -0.00574 CL2 3 0.608937 0.627328 0.079343 11.00000 0.07743 0.06843 = 0.05138 0.00549 0.01325 0.02422 PART 1 CL1A 3 0.691166 0.444749 0.039304 10.50000 0.08090 0.06198 = 0.22605 -0.03534 0.01610 -0.00575 PART 0 N1 6 0.677999 0.774044 0.241353 11.00000 0.02246 0.03223 = 0.02215 0.00261 -0.00144 -0.00254 C5 1 0.668409 0.845539 0.198038 11.00000 0.02643 0.02489 = 0.02498 0.00198 0.00645 -0.00222 C2 1 0.560331 0.729041 0.224937 11.00000 0.02476 0.02419 = 0.02861 -0.00015 0.00333 0.00010 C10 1 0.957137 0.648750 0.264458 11.00000 0.03129 0.03055 = 0.02791 0.00376 0.00666 0.01125 C6 1 0.887682 0.570777 0.280484 11.00000 0.02871 0.02716 = 0.03798 -0.00662 0.00402 0.00556 C8 1 1.027462 0.620942 0.371736 11.00000 0.02856 0.03891 = 0.03885 -0.00708 -0.00162 0.01691 C21 1 0.519719 0.738246 0.423998 11.00000 0.02666 0.06531 = 0.05290 -0.01784 0.01162 0.00158 AFIX 137 H21A 2 0.456652 0.756120 0.385765 11.00000 -1.50000 H21B 2 0.493778 0.764973 0.461259 11.00000 -1.50000 H21C 2 0.521979 0.670903 0.427712 11.00000 -1.50000 AFIX 0 C20 1 0.681477 0.853077 0.385613 11.00000 0.04375 0.03032 = 0.02859 -0.00383 0.00637 0.01237 C19 1 0.817618 0.871818 0.403570 11.00000 0.04811 0.02618 = 0.03137 -0.00799 0.01173 -0.00518 C4 1 0.548768 0.844286 0.155924 11.00000 0.02683 0.02809 = 0.02698 0.00105 0.00355 0.00383 C9 1 1.043309 0.679633 0.320639 11.00000 0.02045 0.03151 = 0.05069 -0.00360 0.00649 -0.00097 C3 1 0.477440 0.768714 0.173580 11.00000 0.02203 0.03148 = 0.02888 -0.00289 0.00024 -0.00159 C16 1 0.654646 0.773617 0.419732 11.00000 0.02677 0.03265 = 0.02575 -0.00462 0.00475 0.00366 C25 1 0.580882 0.913115 0.342873 11.00000 0.06900 0.05401 = 0.03866 0.00386 0.00521 0.03754 AFIX 137 H25A 2 0.623952 0.949715 0.314943 11.00000 -1.50000 H25B 2 0.539792 0.954454 0.368927 11.00000 -1.50000 H25C 2 0.514182 0.873802 0.317251 11.00000 -1.50000 AFIX 0 C15 1 0.952975 0.681847 0.197713 11.00000 0.06635 0.06174 = 0.04266 0.00760 0.02591 0.02168 AFIX 137 H15A 2 0.862286 0.683596 0.174372 11.00000 -1.50000 H15B 2 1.003219 0.639618 0.176517 11.00000 -1.50000 H15C 2 0.990718 0.743802 0.198939 11.00000 -1.50000 AFIX 0 C12 1 0.886897 0.474532 0.383851 11.00000 0.07708 0.04127 = 0.08268 0.02782 0.03875 0.02355 AFIX 137 H12A 2 0.891611 0.493348 0.427884 11.00000 -1.50000 H12B 2 0.944793 0.421765 0.382728 11.00000 -1.50000 H12C 2 0.797083 0.457076 0.364710 11.00000 -1.50000 AFIX 0 C11 1 0.801182 0.509030 0.233209 11.00000 0.04254 0.05357 = 0.07662 -0.03275 0.00152 0.00446 AFIX 137 H11A 2 0.754495 0.466095 0.255709 11.00000 -1.50000 H11B 2 0.854838 0.474179 0.209172 11.00000 -1.50000 H11C 2 0.738125 0.546778 0.204093 11.00000 -1.50000 AFIX 0 C14 1 1.145190 0.755822 0.323094 11.00000 0.04360 0.04985 = 0.10041 -0.01101 0.02464 -0.00935 AFIX 137 H14A 2 1.107229 0.807116 0.295890 11.00000 -1.50000 H14B 2 1.220804 0.731453 0.308200 11.00000 -1.50000 H14C 2 1.172804 0.777707 0.366765 11.00000 -1.50000 AFIX 0 C17 1 0.775466 0.742392 0.458885 11.00000 0.03215 0.03338 = 0.02701 -0.00236 0.00732 0.00351 C18 1 0.875169 0.804191 0.449160 11.00000 0.03312 0.03592 = 0.02608 -0.00755 0.00377 0.00215 C22 1 0.788015 0.664235 0.506642 11.00000 0.05904 0.04775 = 0.04169 0.01737 0.01091 0.01136 AFIX 137 H22A 2 0.713589 0.622344 0.494861 11.00000 -1.50000 H22B 2 0.789455 0.689591 0.548878 11.00000 -1.50000 H22C 2 0.869095 0.630364 0.506990 11.00000 -1.50000 AFIX 0 C7 1 0.929023 0.554138 0.347047 11.00000 0.03467 0.02721 = 0.04485 0.00857 0.01398 0.01073 C23 1 1.010761 0.810349 0.491310 11.00000 0.03803 0.06943 = 0.04739 -0.02186 -0.00172 -0.00267 AFIX 137 H23A 2 1.034506 0.750486 0.511455 11.00000 -1.50000 H23B 2 1.010863 0.857262 0.524003 11.00000 -1.50000 H23C 2 1.074113 0.827260 0.465578 11.00000 -1.50000 AFIX 0 C13 1 1.118815 0.614648 0.435727 11.00000 0.05607 0.08726 = 0.04948 -0.01406 -0.01490 0.03828 AFIX 137 H13A 2 1.172859 0.670300 0.443027 11.00000 -1.50000 H13B 2 1.174975 0.560406 0.436747 11.00000 -1.50000 H13C 2 1.067797 0.609160 0.468866 11.00000 -1.50000 AFIX 0 C24 1 0.891794 0.955831 0.386566 11.00000 0.09255 0.03606 = 0.05608 -0.00767 0.02789 -0.02164 AFIX 137 H24A 2 0.967714 0.935265 0.370261 11.00000 -1.50000 H24B 2 0.920927 0.993725 0.424432 11.00000 -1.50000 H24C 2 0.834255 0.992317 0.354113 11.00000 -1.50000 AFIX 0 C26 1 0.696452 0.558094 0.037047 11.00000 0.19735 0.06079 = 0.10722 0.02469 0.11228 0.02783 PART 1 AFIX 23 H26C 2 0.669404 0.576081 -0.008007 10.50000 -1.20000 H26D 2 0.789281 0.575819 0.050534 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.655987 0.562945 -0.008523 10.50000 -1.20000 H26B 2 0.786238 0.582753 0.042764 10.50000 -1.20000 AFIX 0 CL1B 3 0.705470 0.446128 0.057193 10.50000 0.10262 0.06305 = 0.06246 0.01767 0.03023 0.03371 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0773, GooF = S = 1.051, Restrained GooF = 1.051 for all data REM R1 = 0.0331 for 7070 Fo > 4sig(Fo) and 0.0457 for all 8878 data REM 317 parameters refined using 6 restraints END WGHT 0.0327 0.0000 REM Highest difference peak 1.121, deepest hole -1.468, 1-sigma level 0.162 Q1 1 0.2901 0.7463 0.1614 11.00000 0.05 1.12 Q2 1 0.7589 0.4786 0.0432 11.00000 0.05 1.04 Q3 1 0.7124 0.7036 0.3383 11.00000 0.05 0.75 Q4 1 0.8721 0.7559 0.3394 11.00000 0.05 0.68 Q5 1 0.3252 0.7447 0.1012 11.00000 0.05 0.67 Q6 1 0.4463 0.6192 0.2667 11.00000 0.05 0.66 Q7 1 0.1803 0.7405 0.1412 11.00000 0.05 0.64 Q8 1 1.0808 0.6184 0.3969 11.00000 0.05 0.63 Q9 1 0.5550 0.9524 0.0814 11.00000 0.05 0.62 Q10 1 0.7207 0.8997 0.2008 11.00000 0.05 0.61 Q11 1 0.6469 0.5835 0.2799 11.00000 0.05 0.57 Q12 1 0.9819 0.7780 0.2619 11.00000 0.05 0.56 Q13 1 1.0990 0.7172 0.1942 11.00000 0.05 0.56 Q14 1 0.3231 0.6383 0.1397 11.00000 0.05 0.55 Q15 1 0.5391 0.6046 0.0558 11.00000 0.05 0.55 Q16 1 0.6045 0.9604 0.0387 11.00000 0.05 0.53 ; _shelx_res_checksum 75894 _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 2.640 _oxdiff_exptl_absorpt_empirical_full_min 0.625 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 0.80421(2) 0.71524(2) 0.33916(2) 0.02268(5) Uani 1 1 d . . . . . I1 I 0.52449(3) 0.61607(2) 0.28077(2) 0.03303(7) Uani 1 1 d . . . . . I4 I 0.82151(3) 0.93965(2) 0.20050(2) 0.03830(8) Uani 1 1 d . . . . . I3 I 0.48480(3) 0.93748(2) 0.08180(2) 0.03870(8) Uani 1 1 d . . . . . I2 I 0.29274(3) 0.72238(2) 0.13000(2) 0.05129(9) Uani 1 1 d . . . . . Cl2 Cl 0.60894(16) 0.62733(10) 0.07934(7) 0.0657(4) Uani 1 1 d . . . . . Cl1A Cl 0.6912(11) 0.4447(7) 0.0393(5) 0.125(4) Uani 0.5 1 d . U P A 1 N1 N 0.6780(3) 0.7740(2) 0.24135(15) 0.0265(6) Uani 1 1 d . . . . . C5 C 0.6684(4) 0.8455(2) 0.19804(18) 0.0253(7) Uani 1 1 d . . . . . C2 C 0.5603(4) 0.7290(2) 0.22494(18) 0.0262(7) Uani 1 1 d . . . . . C10 C 0.9571(4) 0.6487(3) 0.26446(19) 0.0298(8) Uani 1 1 d . . . . . C6 C 0.8877(4) 0.5708(3) 0.2805(2) 0.0317(8) Uani 1 1 d . . . . . C8 C 1.0275(4) 0.6209(3) 0.3717(2) 0.0367(9) Uani 1 1 d . . . . . C21 C 0.5197(4) 0.7382(4) 0.4240(2) 0.0478(12) Uani 1 1 d . . . . . H21A H 0.456652 0.756120 0.385765 0.072 Uiso 1 1 calc R U . . . H21B H 0.493778 0.764973 0.461259 0.072 Uiso 1 1 calc R U . . . H21C H 0.521979 0.670903 0.427712 0.072 Uiso 1 1 calc R U . . . C20 C 0.6815(4) 0.8531(3) 0.3856(2) 0.0344(9) Uani 1 1 d . . . . . C19 C 0.8176(4) 0.8718(3) 0.4036(2) 0.0347(9) Uani 1 1 d . . . . . C4 C 0.5488(4) 0.8443(3) 0.15592(18) 0.0276(7) Uani 1 1 d . . . . . C9 C 1.0433(4) 0.6796(3) 0.3206(2) 0.0343(9) Uani 1 1 d . . . . . C3 C 0.4774(4) 0.7687(3) 0.17358(19) 0.0282(8) Uani 1 1 d . . . . . C16 C 0.6546(4) 0.7736(3) 0.41973(19) 0.0285(8) Uani 1 1 d . . . . . C25 C 0.5809(5) 0.9131(4) 0.3429(2) 0.0547(14) Uani 1 1 d . . . . . H25A H 0.623952 0.949715 0.314943 0.082 Uiso 1 1 calc R U . . . H25B H 0.539792 0.954454 0.368927 0.082 Uiso 1 1 calc R U . . . H25C H 0.514182 0.873802 0.317251 0.082 Uiso 1 1 calc R U . . . C15 C 0.9530(6) 0.6818(4) 0.1977(3) 0.0548(13) Uani 1 1 d . . . . . H15A H 0.862286 0.683596 0.174372 0.082 Uiso 1 1 calc R U . . . H15B H 1.003219 0.639618 0.176517 0.082 Uiso 1 1 calc R U . . . H15C H 0.990718 0.743802 0.198939 0.082 Uiso 1 1 calc R U . . . C12 C 0.8869(6) 0.4745(3) 0.3839(3) 0.0638(16) Uani 1 1 d . . . . . H12A H 0.891611 0.493348 0.427884 0.096 Uiso 1 1 calc R U . . . H12B H 0.944793 0.421765 0.382728 0.096 Uiso 1 1 calc R U . . . H12C H 0.797083 0.457076 0.364710 0.096 Uiso 1 1 calc R U . . . C11 C 0.8012(5) 0.5090(4) 0.2332(3) 0.0591(15) Uani 1 1 d . . . . . H11A H 0.754495 0.466095 0.255709 0.089 Uiso 1 1 calc R U . . . H11B H 0.854838 0.474179 0.209172 0.089 Uiso 1 1 calc R U . . . H11C H 0.738125 0.546778 0.204093 0.089 Uiso 1 1 calc R U . . . C14 C 1.1452(5) 0.7558(4) 0.3231(3) 0.0632(16) Uani 1 1 d . . . . . H14A H 1.107229 0.807116 0.295890 0.095 Uiso 1 1 calc R U . . . H14B H 1.220804 0.731453 0.308200 0.095 Uiso 1 1 calc R U . . . H14C H 1.172804 0.777707 0.366765 0.095 Uiso 1 1 calc R U . . . C17 C 0.7755(4) 0.7424(3) 0.45888(19) 0.0307(8) Uani 1 1 d . . . . . C18 C 0.8752(4) 0.8042(3) 0.44916(19) 0.0320(8) Uani 1 1 d . . . . . C22 C 0.7880(5) 0.6642(3) 0.5066(2) 0.0494(12) Uani 1 1 d . . . . . H22A H 0.713589 0.622344 0.494861 0.074 Uiso 1 1 calc R U . . . H22B H 0.789455 0.689591 0.548878 0.074 Uiso 1 1 calc R U . . . H22C H 0.869095 0.630364 0.506990 0.074 Uiso 1 1 calc R U . . . C7 C 0.9290(4) 0.5541(3) 0.3470(2) 0.0347(9) Uani 1 1 d . . . . . C23 C 1.0108(5) 0.8103(4) 0.4913(3) 0.0531(13) Uani 1 1 d . . . . . H23A H 1.034506 0.750486 0.511455 0.080 Uiso 1 1 calc R U . . . H23B H 1.010863 0.857262 0.524003 0.080 Uiso 1 1 calc R U . . . H23C H 1.074113 0.827260 0.465578 0.080 Uiso 1 1 calc R U . . . C13 C 1.1188(6) 0.6146(4) 0.4357(3) 0.0680(17) Uani 1 1 d . . . . . H13A H 1.172859 0.670300 0.443027 0.102 Uiso 1 1 calc R U . . . H13B H 1.174975 0.560406 0.436747 0.102 Uiso 1 1 calc R U . . . H13C H 1.067797 0.609160 0.468866 0.102 Uiso 1 1 calc R U . . . C24 C 0.8918(6) 0.9558(3) 0.3866(3) 0.0598(15) Uani 1 1 d . . . . . H24A H 0.967714 0.935265 0.370261 0.090 Uiso 1 1 calc R U . . . H24B H 0.920927 0.993725 0.424432 0.090 Uiso 1 1 calc R U . . . H24C H 0.834255 0.992317 0.354113 0.090 Uiso 1 1 calc R U . . . C26 C 0.6965(11) 0.5581(4) 0.0370(4) 0.110(3) Uani 1 1 d . . . . . H26C H 0.669404 0.576081 -0.008007 0.132 Uiso 0.5 1 calc R U P A 1 H26D H 0.789281 0.575819 0.050534 0.132 Uiso 0.5 1 calc R U P A 1 H26A H 0.655987 0.562945 -0.008523 0.132 Uiso 0.5 1 calc R U P A -1 H26B H 0.786238 0.582753 0.042764 0.132 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7055(10) 0.4461(6) 0.0572(3) 0.074(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 0.02182(9) 0.02286(9) 0.02186(9) -0.00048(6) 0.00095(6) 0.00301(6) I1 0.03390(14) 0.02966(13) 0.03486(15) 0.00195(10) 0.00552(11) -0.00928(9) I4 0.03369(15) 0.03617(15) 0.04442(17) 0.00592(11) 0.00661(12) -0.00981(10) I3 0.04396(16) 0.04092(15) 0.02999(14) 0.00942(11) 0.00470(11) 0.01387(11) I2 0.02808(15) 0.04966(18) 0.0662(2) -0.00021(15) -0.01340(14) -0.00574(11) Cl2 0.0774(10) 0.0684(9) 0.0514(8) 0.0055(7) 0.0133(7) 0.0242(7) Cl1A 0.081(4) 0.062(4) 0.226(10) -0.035(5) 0.016(6) -0.006(3) N1 0.0225(15) 0.0322(16) 0.0221(16) 0.0026(12) -0.0014(12) -0.0025(11) C5 0.0264(18) 0.0249(17) 0.0250(18) 0.0020(14) 0.0065(14) -0.0022(13) C2 0.0248(18) 0.0242(17) 0.029(2) -0.0001(14) 0.0033(15) 0.0001(13) C10 0.031(2) 0.0306(19) 0.028(2) 0.0038(15) 0.0067(16) 0.0112(14) C6 0.029(2) 0.0272(18) 0.038(2) -0.0066(16) 0.0040(16) 0.0056(14) C8 0.029(2) 0.039(2) 0.039(2) -0.0071(18) -0.0016(17) 0.0169(16) C21 0.027(2) 0.065(3) 0.053(3) -0.018(2) 0.012(2) 0.0016(19) C20 0.044(2) 0.0303(19) 0.029(2) -0.0038(16) 0.0064(17) 0.0124(16) C19 0.048(2) 0.0262(18) 0.031(2) -0.0080(16) 0.0117(18) -0.0052(16) C4 0.0268(18) 0.0281(18) 0.0270(19) 0.0011(15) 0.0036(15) 0.0038(14) C9 0.0205(18) 0.032(2) 0.051(3) -0.0036(18) 0.0065(17) -0.0010(14) C3 0.0220(18) 0.0315(19) 0.029(2) -0.0029(15) 0.0002(14) -0.0016(13) C16 0.0268(19) 0.0326(19) 0.0257(19) -0.0046(15) 0.0047(15) 0.0037(14) C25 0.069(3) 0.054(3) 0.039(3) 0.004(2) 0.005(2) 0.038(3) C15 0.066(3) 0.062(3) 0.043(3) 0.008(2) 0.026(3) 0.022(3) C12 0.077(4) 0.041(3) 0.083(4) 0.028(3) 0.039(3) 0.024(3) C11 0.043(3) 0.054(3) 0.077(4) -0.033(3) 0.002(3) 0.004(2) C14 0.044(3) 0.050(3) 0.100(5) -0.011(3) 0.025(3) -0.009(2) C17 0.032(2) 0.0334(19) 0.027(2) -0.0024(16) 0.0073(16) 0.0035(15) C18 0.033(2) 0.036(2) 0.026(2) -0.0075(16) 0.0038(16) 0.0022(15) C22 0.059(3) 0.048(3) 0.042(3) 0.017(2) 0.011(2) 0.011(2) C7 0.035(2) 0.0272(19) 0.045(3) 0.0086(17) 0.0140(18) 0.0107(15) C23 0.038(3) 0.069(3) 0.047(3) -0.022(3) -0.002(2) -0.003(2) C13 0.056(3) 0.087(4) 0.049(3) -0.014(3) -0.015(3) 0.038(3) C24 0.093(4) 0.036(2) 0.056(3) -0.008(2) 0.028(3) -0.022(3) C26 0.197(9) 0.061(4) 0.107(6) 0.025(4) 0.112(7) 0.028(5) Cl1B 0.103(5) 0.063(3) 0.062(2) 0.018(2) 0.030(2) 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 62.03(7) . . ? N1 Dy1 C10 83.60(11) . . ? N1 Dy1 C6 92.10(12) . . ? N1 Dy1 C8 134.84(12) . . ? N1 Dy1 C20 81.03(12) . . ? N1 Dy1 C19 96.69(12) . . ? N1 Dy1 C9 107.53(13) . . ? N1 Dy1 C16 99.58(11) . . ? N1 Dy1 C17 129.86(11) . . ? N1 Dy1 C18 127.69(11) . . ? N1 Dy1 C7 122.75(13) . . ? C10 Dy1 I1 102.07(9) . . ? C10 Dy1 C6 30.84(12) . . ? C10 Dy1 C8 51.29(13) . . ? C10 Dy1 C20 152.49(12) . . ? C10 Dy1 C16 176.41(11) . . ? C10 Dy1 C17 146.13(12) . . ? C6 Dy1 I1 80.11(9) . . ? C6 Dy1 C16 146.62(12) . . ? C6 Dy1 C17 132.71(13) . . ? C8 Dy1 I1 122.77(10) . . ? C8 Dy1 C6 51.20(13) . . ? C8 Dy1 C20 138.04(13) . . ? C8 Dy1 C16 125.58(13) . . ? C8 Dy1 C17 94.98(13) . . ? C20 Dy1 I1 90.65(10) . . ? C20 Dy1 C6 170.36(13) . . ? C20 Dy1 C16 30.72(12) . . ? C20 Dy1 C17 51.31(12) . . ? C19 Dy1 I1 121.65(10) . . ? C19 Dy1 C10 130.61(13) . . ? C19 Dy1 C6 158.15(13) . . ? C19 Dy1 C8 110.54(14) . . ? C19 Dy1 C20 31.00(13) . . ? C19 Dy1 C9 107.11(13) . . ? C19 Dy1 C16 50.96(12) . . ? C19 Dy1 C17 51.36(12) . . ? C19 Dy1 C18 31.22(13) . . ? C19 Dy1 C7 138.15(14) . . ? C9 Dy1 I1 130.62(9) . . ? C9 Dy1 C10 30.98(13) . . ? C9 Dy1 C6 51.06(12) . . ? C9 Dy1 C8 31.04(14) . . ? C9 Dy1 C20 137.56(13) . . ? C9 Dy1 C16 147.46(13) . . ? C9 Dy1 C17 117.78(13) . . ? C9 Dy1 C18 97.37(13) . . ? C16 Dy1 I1 78.11(8) . . ? C17 Dy1 I1 99.55(9) . . ? C17 Dy1 C16 31.02(12) . . ? C18 Dy1 I1 128.17(9) . . ? C18 Dy1 C10 128.18(12) . . ? C18 Dy1 C6 137.57(13) . . ? C18 Dy1 C8 86.84(13) . . ? C18 Dy1 C20 51.27(13) . . ? C18 Dy1 C16 50.90(12) . . ? C18 Dy1 C17 30.82(12) . . ? C7 Dy1 I1 91.60(10) . . ? C7 Dy1 C10 51.38(12) . . ? C7 Dy1 C6 31.06(13) . . ? C7 Dy1 C8 31.18(13) . . ? C7 Dy1 C20 153.71(13) . . ? C7 Dy1 C9 51.42(12) . . ? C7 Dy1 C16 125.08(12) . . ? C7 Dy1 C17 102.55(13) . . ? C7 Dy1 C18 108.88(13) . . ? C2 I1 Dy1 68.22(10) . . ? C5 N1 Dy1 143.9(2) . . ? C2 N1 Dy1 111.1(2) . . ? C2 N1 C5 104.2(3) . . ? N1 C5 I4 121.4(3) . . ? N1 C5 C4 111.2(3) . . ? C4 C5 I4 127.4(3) . . ? N1 C2 I1 118.4(3) . . ? N1 C2 C3 113.0(3) . . ? C3 C2 I1 128.5(3) . . ? C6 C10 Dy1 75.0(2) . . ? C6 C10 C9 108.0(4) . . ? C6 C10 C15 124.6(4) . . ? C9 C10 Dy1 74.2(2) . . ? C9 C10 C15 126.9(4) . . ? C15 C10 Dy1 123.8(3) . . ? C10 C6 Dy1 74.2(2) . . ? C10 C6 C11 124.9(4) . . ? C10 C6 C7 108.2(4) . . ? C11 C6 Dy1 124.9(3) . . ? C7 C6 Dy1 73.7(2) . . ? C7 C6 C11 126.3(4) . . ? C9 C8 Dy1 74.1(2) . . ? C9 C8 C7 107.7(4) . . ? C9 C8 C13 126.0(5) . . ? C7 C8 Dy1 74.0(2) . . ? C7 C8 C13 124.7(5) . . ? C13 C8 Dy1 128.7(3) . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? C19 C20 Dy1 73.4(2) . . ? C19 C20 C16 107.8(3) . . ? C19 C20 C25 125.8(4) . . ? C16 C20 Dy1 75.6(2) . . ? C16 C20 C25 126.1(4) . . ? C25 C20 Dy1 121.7(3) . . ? C20 C19 Dy1 75.6(2) . . ? C20 C19 C18 108.2(3) . . ? C20 C19 C24 128.0(4) . . ? C18 C19 Dy1 75.1(2) . . ? C18 C19 C24 123.2(4) . . ? C24 C19 Dy1 122.1(3) . . ? C5 C4 I3 126.5(3) . . ? C5 C4 C3 106.7(3) . . ? C3 C4 I3 126.7(3) . . ? C10 C9 Dy1 74.8(2) . . ? C10 C9 C8 108.4(3) . . ? C10 C9 C14 124.9(5) . . ? C8 C9 Dy1 74.8(2) . . ? C8 C9 C14 126.5(5) . . ? C14 C9 Dy1 121.7(3) . . ? C2 C3 I2 126.8(3) . . ? C2 C3 C4 104.9(3) . . ? C4 C3 I2 128.2(3) . . ? C21 C16 Dy1 126.9(3) . . ? C20 C16 Dy1 73.7(2) . . ? C20 C16 C21 125.9(4) . . ? C20 C16 C17 108.3(3) . . ? C17 C16 Dy1 74.0(2) . . ? C17 C16 C21 124.9(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 125.1(4) . . ? C18 C17 Dy1 73.8(2) . . ? C18 C17 C16 107.3(3) . . ? C18 C17 C22 127.3(4) . . ? C22 C17 Dy1 122.1(3) . . ? C19 C18 Dy1 73.7(2) . . ? C19 C18 C23 125.4(4) . . ? C17 C18 Dy1 75.4(2) . . ? C17 C18 C19 108.3(4) . . ? C17 C18 C23 124.8(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 75.2(2) . . ? C6 C7 C8 107.7(4) . . ? C6 C7 C12 126.3(5) . . ? C8 C7 Dy1 74.8(2) . . ? C8 C7 C12 125.7(5) . . ? C12 C7 Dy1 120.6(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 122.4(6) . . ? Cl1A C26 H26C 106.7 . . ? Cl1A C26 H26D 106.7 . . ? Cl1A C26 H26A 95.2 . . ? Cl1A C26 H26B 113.2 . . ? Cl1A C26 Cl1B 13.2(6) . . ? H26C C26 H26D 106.6 . . ? H26C C26 H26A 13.7 . . ? H26C C26 H26B 95.7 . . ? H26D C26 H26A 117.9 . . ? H26D C26 H26B 11.2 . . ? H26A C26 H26B 107.5 . . ? Cl1B C26 Cl2 115.5(4) . . ? Cl1B C26 H26C 119.9 . . ? Cl1B C26 H26D 100.1 . . ? 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 3.2419(3) . ? Dy1 N1 2.380(3) . ? Dy1 C10 2.648(4) . ? Dy1 C6 2.658(4) . ? Dy1 C8 2.649(4) . ? Dy1 C20 2.653(4) . ? Dy1 C19 2.624(4) . ? Dy1 C9 2.640(4) . ? Dy1 C16 2.677(4) . ? Dy1 C17 2.663(4) . ? Dy1 C18 2.642(4) . ? Dy1 C7 2.639(4) . ? I1 C2 2.091(4) . ? I4 C5 2.077(3) . ? I3 C4 2.075(4) . ? I2 C3 2.060(4) . ? Cl2 C26 1.722(6) . ? Cl1A C26 1.629(12) . ? N1 C5 1.372(5) . ? N1 C2 1.361(5) . ? C5 C4 1.375(5) . ? C2 C3 1.371(5) . ? C10 C6 1.411(6) . ? C10 C9 1.412(6) . ? C10 C15 1.495(6) . ? C6 C11 1.496(6) . ? C6 C7 1.418(6) . ? C8 C9 1.415(6) . ? C8 C7 1.421(6) . ? C8 C13 1.497(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21 C16 1.509(6) . ? C20 C19 1.411(6) . ? C20 C16 1.412(6) . ? C20 C25 1.508(6) . ? C19 C18 1.417(6) . ? C19 C24 1.514(6) . ? C4 C3 1.408(5) . ? C9 C14 1.514(6) . ? C16 C17 1.428(5) . ? 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 1.502(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 1.410(6) . ? C17 C22 1.504(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 1.662(10) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Dy1 N1 C5 I4 12.3(6) . . . . ? Dy1 N1 C5 C4 -167.6(3) . . . . ? Dy1 N1 C2 I1 -5.5(3) . . . . ? Dy1 N1 C2 C3 171.9(3) . . . . ? Dy1 C10 C6 C11 121.8(4) . . . . ? Dy1 C10 C6 C7 -66.4(3) . . . . ? Dy1 C10 C9 C8 67.9(3) . . . . ? Dy1 C10 C9 C14 -118.3(4) . . . . ? Dy1 C6 C7 C8 -68.3(3) . . . . ? Dy1 C6 C7 C12 117.3(4) . . . . ? Dy1 C8 C9 C10 -67.9(3) . . . . ? Dy1 C8 C9 C14 118.4(4) . . . . ? Dy1 C8 C7 C6 68.6(3) . . . . ? Dy1 C8 C7 C12 -117.0(4) . . . . ? Dy1 C20 C19 C18 -68.7(3) . . . . ? Dy1 C20 C19 C24 119.7(4) . . . . ? Dy1 C20 C16 C21 -124.1(4) . . . . ? Dy1 C20 C16 C17 66.4(3) . . . . ? Dy1 C19 C18 C17 -68.1(3) . . . . ? Dy1 C19 C18 C23 125.2(4) . . . . ? Dy1 C16 C17 C18 67.3(3) . . . . ? Dy1 C16 C17 C22 -118.9(4) . . . . ? Dy1 C17 C18 C19 66.9(3) . . . . ? Dy1 C17 C18 C23 -126.3(4) . . . . ? I1 C2 C3 I2 -5.2(5) . . . . ? I1 C2 C3 C4 177.5(3) . . . . ? I4 C5 C4 I3 -0.3(5) . . . . ? I4 C5 C4 C3 -179.2(3) . . . . ? I3 C4 C3 I2 3.2(5) . . . . ? I3 C4 C3 C2 -179.6(3) . . . . ? N1 C5 C4 I3 179.6(2) . . . . ? N1 C5 C4 C3 0.7(4) . . . . ? N1 C2 C3 I2 177.7(3) . . . . ? N1 C2 C3 C4 0.4(4) . . . . ? C5 N1 C2 I1 -177.4(2) . . . . ? C5 N1 C2 C3 0.0(4) . . . . ? C5 C4 C3 I2 -177.9(3) . . . . ? C5 C4 C3 C2 -0.6(4) . . . . ? C2 N1 C5 I4 179.5(2) . . . . ? C2 N1 C5 C4 -0.4(4) . . . . ? C10 C6 C7 Dy1 66.7(3) . . . . ? C10 C6 C7 C8 -1.6(4) . . . . ? C10 C6 C7 C12 -176.0(4) . . . . ? C6 C10 C9 Dy1 -68.0(3) . . . . ? C6 C10 C9 C8 -0.1(4) . . . . ? C6 C10 C9 C14 173.7(4) . . . . ? C21 C16 C17 Dy1 124.1(4) . . . . ? C21 C16 C17 C18 -168.6(4) . . . . ? C21 C16 C17 C22 5.2(6) . . . . ? C20 C19 C18 Dy1 69.0(3) . . . . ? C20 C19 C18 C17 0.9(4) . . . . ? C20 C19 C18 C23 -165.7(4) . . . . ? C20 C16 C17 Dy1 -66.3(3) . . . . ? C20 C16 C17 C18 1.0(4) . . . . ? C20 C16 C17 C22 174.8(4) . . . . ? C19 C20 C16 Dy1 -66.8(3) . . . . ? C19 C20 C16 C21 169.0(4) . . . . ? C19 C20 C16 C17 -0.4(4) . . . . ? C9 C10 C6 Dy1 67.5(3) . . . . ? C9 C10 C6 C11 -170.7(4) . . . . ? C9 C10 C6 C7 1.0(4) . . . . ? C9 C8 C7 Dy1 -67.1(3) . . . . ? C9 C8 C7 C6 1.6(4) . . . . ? C9 C8 C7 C12 175.9(4) . . . . ? C16 C20 C19 Dy1 68.3(3) . . . . ? C16 C20 C19 C18 -0.3(4) . . . . ? C16 C20 C19 C24 -171.9(4) . . . . ? C16 C17 C18 Dy1 -68.1(3) . . . . ? C16 C17 C18 C19 -1.2(4) . . . . ? C16 C17 C18 C23 165.6(4) . . . . ? C25 C20 C19 Dy1 -117.4(4) . . . . ? C25 C20 C19 C18 173.9(4) . . . . ? C25 C20 C19 C24 2.3(7) . . . . ? C25 C20 C16 Dy1 118.9(4) . . . . ? C25 C20 C16 C21 -5.2(7) . . . . ? C25 C20 C16 C17 -174.6(4) . . . . ? C15 C10 C6 Dy1 -121.0(4) . . . . ? C15 C10 C6 C11 0.8(6) . . . . ? C15 C10 C6 C7 172.6(4) . . . . ? C15 C10 C9 Dy1 120.7(4) . . . . ? C15 C10 C9 C8 -171.4(4) . . . . ? C15 C10 C9 C14 2.4(6) . . . . ? C11 C6 C7 Dy1 -121.7(4) . . . . ? C11 C6 C7 C8 170.0(4) . . . . ? C11 C6 C7 C12 -4.4(6) . . . . ? C22 C17 C18 Dy1 118.2(4) . . . . ? C22 C17 C18 C19 -174.8(4) . . . . ? C22 C17 C18 C23 -8.1(7) . . . . ? C7 C8 C9 Dy1 67.0(3) . . . . ? C7 C8 C9 C10 -0.9(4) . . . . ? C7 C8 C9 C14 -174.6(4) . . . . ? C13 C8 C9 Dy1 -126.7(4) . . . . ? C13 C8 C9 C10 165.4(4) . . . . ? C13 C8 C9 C14 -8.3(7) . . . . ? C13 C8 C7 Dy1 126.4(4) . . . . ? C13 C8 C7 C6 -165.0(4) . . . . ? C13 C8 C7 C12 9.4(7) . . . . ? C24 C19 C18 Dy1 -118.9(4) . . . . ? C24 C19 C18 C17 173.0(4) . . . . ? C24 C19 C18 C23 6.4(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 -1.0017 -1.0304 0.1187 -0.0783 -0.0142 0.0325 -1.0132 0.9834 -0.0270 0.0038 0.0040 0.0859 1.0017 1.0304 -0.1187 0.0783 0.0142 -0.0325 1.0132 -0.9834 0.0270 -0.0038 -0.0040 -0.0859 -0.0072 -0.0360 -0.9994 -0.0100 0.0322 0.0044 0.0072 0.0360 0.9994 0.0100 -0.0322 -0.0044 -0.9988 1.0554 1.9717 0.0239 -0.0605 0.0770 0.9988 -1.0554 -1.9717 -0.0239 0.0605 -0.0770 1.0204 -0.9474 1.0264 0.0063 -0.0363 -0.0903 0.0086 1.0789 1.9259 0.0612 -0.0554 0.0178 2.0279 -0.9239 0.9806 0.0435 -0.0312 -0.1495 -0.0201 0.9349 -2.0716 0.0210 0.0736 0.0356 -1.0218 -0.0955 -1.9529 -0.0574 0.0594 0.0681 -0.9931 0.0484 2.0446 -0.0172 -0.0696 0.0503 -6.0000 6.3741 -22.6814 -0.1415 0.7602 0.6341