#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:50:03 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294477 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572186.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_1572186 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 102.000(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3865(2) _cell_length_b 14.3825(3) _cell_length_c 21.4194(5) _cell_measurement_reflns_used 17761 _cell_measurement_temperature 240.0(1) _cell_measurement_theta_max 30.0680 _cell_measurement_theta_min 2.8280 _cell_volume 3129.79(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 240.0(1) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.836 _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 0.0340827000 _diffrn_orient_matrix_UB_12 0.0425535000 _diffrn_orient_matrix_UB_13 0.0078518000 _diffrn_orient_matrix_UB_21 0.0011845000 _diffrn_orient_matrix_UB_22 0.0070971000 _diffrn_orient_matrix_UB_23 -0.0326467000 _diffrn_orient_matrix_UB_31 -0.0608935000 _diffrn_orient_matrix_UB_32 0.0239307000 _diffrn_orient_matrix_UB_33 -0.0042796000 _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 0.0562 _diffrn_reflns_av_unetI/netI 0.0477 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.836 _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 -29 _diffrn_reflns_number 39147 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.836 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.791 _diffrn_reflns_theta_min 2.454 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.518 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.233 _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 2.308 _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 0.924 _refine_diff_density_min -1.354 _refine_diff_density_rms 0.155 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 8935 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0341 _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^)+(0.0328P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.0797 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6874 _reflns_number_total 8935 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyTIP240K _cod_depositor_comments 'Adding full bibliography for 1572175--1572199.cif.' _cod_original_cell_volume 3129.79(13) _cod_database_code 1572186 _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 0.531 _shelx_estimated_absorpt_t_min 0.207 _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_240_final.res created by SHELXL-2018/3 at 16:48:18 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 10.386507 14.382455 21.419422 90 102 90 ZERR 4 0.000241 0.000331 0.000538 0 0.0024 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Dy I N UNIT 100 128 8 4 16 4 SIMU Cl1B Cl1A L.S. 50 0 0 PLAN 16 SIZE 0.111 0.275 0.353 TEMP -33.15(10) CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.032800 FVAR 0.60493 DY1 4 0.803984 0.715807 0.338965 11.00000 0.02546 0.02634 = 0.02537 -0.00038 0.00121 0.00331 I1 5 0.524014 0.617076 0.280010 11.00000 0.03976 0.03457 = 0.04104 0.00235 0.00657 -0.01094 I4 5 0.822025 0.939606 0.200480 11.00000 0.04004 0.04245 = 0.05163 0.00685 0.00788 -0.01166 I3 5 0.485990 0.938186 0.082085 11.00000 0.05239 0.04782 = 0.03473 0.01112 0.00563 0.01640 I2 5 0.293385 0.723685 0.129531 11.00000 0.03321 0.05791 = 0.07624 -0.00079 -0.01552 -0.00652 CL2 3 0.608846 0.626977 0.079121 11.00000 0.09300 0.08214 = 0.06049 0.00658 0.01640 0.02882 PART 1 CL1A 3 0.693678 0.444719 0.040129 10.50000 0.08441 0.07340 = 0.25983 -0.04226 0.04102 -0.00711 PART 0 N1 6 0.678283 0.774335 0.241087 11.00000 0.02699 0.03569 = 0.02758 0.00200 0.00130 -0.00187 C5 1 0.669476 0.845604 0.198265 11.00000 0.02888 0.03097 = 0.02687 0.00252 0.00459 -0.00013 C2 1 0.560620 0.729800 0.224846 11.00000 0.02890 0.02999 = 0.03167 0.00044 0.00411 -0.00252 C10 1 0.957680 0.648615 0.265093 11.00000 0.04155 0.03687 = 0.03772 0.00433 0.01427 0.01299 C6 1 0.888091 0.571024 0.281640 11.00000 0.03407 0.02837 = 0.04698 -0.00803 0.00726 0.00561 C8 1 1.027528 0.621375 0.372140 11.00000 0.03458 0.04566 = 0.04248 -0.00653 0.00099 0.01784 C21 1 0.520465 0.737179 0.423943 11.00000 0.03766 0.07311 = 0.06005 -0.01984 0.01585 -0.00706 AFIX 137 H21A 2 0.456885 0.755032 0.385947 11.00000 -1.50000 H21B 2 0.495003 0.763547 0.461269 11.00000 -1.50000 H21C 2 0.523159 0.669941 0.427503 11.00000 -1.50000 AFIX 0 C20 1 0.680523 0.852519 0.384907 11.00000 0.05528 0.03071 = 0.02871 -0.00021 0.00523 0.01614 C19 1 0.816922 0.872424 0.402891 11.00000 0.05262 0.02882 = 0.03943 -0.00910 0.01516 -0.00241 C4 1 0.549407 0.844876 0.155927 11.00000 0.03084 0.03101 = 0.03079 -0.00078 0.00347 0.00525 C9 1 1.042953 0.679952 0.321010 11.00000 0.02572 0.03759 = 0.05486 -0.00611 0.00848 -0.00078 C3 1 0.478369 0.769522 0.173266 11.00000 0.02801 0.03187 = 0.03372 -0.00711 0.00076 -0.00292 C16 1 0.655165 0.773085 0.419435 11.00000 0.03356 0.03769 = 0.03204 -0.00474 0.00640 0.00491 C25 1 0.577816 0.911324 0.342286 11.00000 0.08110 0.05656 = 0.04455 0.00435 0.00757 0.04238 AFIX 137 H25A 2 0.620819 0.955621 0.319233 11.00000 -1.50000 H25B 2 0.526489 0.944494 0.368128 11.00000 -1.50000 H25C 2 0.520189 0.871620 0.312126 11.00000 -1.50000 AFIX 0 C15 1 0.952291 0.681493 0.198011 11.00000 0.08008 0.07171 = 0.04650 0.00974 0.02928 0.02688 AFIX 137 H15A 2 0.861926 0.680063 0.174313 11.00000 -1.50000 H15B 2 1.005779 0.641072 0.177509 11.00000 -1.50000 H15C 2 0.985691 0.744567 0.198907 11.00000 -1.50000 AFIX 0 C12 1 0.887889 0.476025 0.384303 11.00000 0.08324 0.04661 = 0.09499 0.03451 0.04459 0.02460 AFIX 137 H12A 2 0.900143 0.493290 0.428928 11.00000 -1.50000 H12B 2 0.940765 0.421624 0.380278 11.00000 -1.50000 H12C 2 0.795795 0.462052 0.367621 11.00000 -1.50000 AFIX 0 C11 1 0.800734 0.508510 0.233860 11.00000 0.05033 0.05882 = 0.08125 -0.03507 0.00260 0.00318 AFIX 137 H11A 2 0.751110 0.467589 0.256093 11.00000 -1.50000 H11B 2 0.854752 0.471623 0.211361 11.00000 -1.50000 H11C 2 0.740381 0.546273 0.203518 11.00000 -1.50000 AFIX 0 C14 1 1.143314 0.756589 0.323171 11.00000 0.04435 0.06259 = 0.12195 -0.01530 0.03038 -0.01190 AFIX 137 H14A 2 1.099363 0.813049 0.305361 11.00000 -1.50000 H14B 2 1.207511 0.738281 0.298458 11.00000 -1.50000 H14C 2 1.187490 0.767631 0.367081 11.00000 -1.50000 AFIX 0 C17 1 0.775484 0.743428 0.458394 11.00000 0.04201 0.03405 = 0.02749 -0.00205 0.00654 0.00499 C18 1 0.874463 0.804765 0.448730 11.00000 0.03482 0.04362 = 0.03250 -0.00758 0.00415 0.00212 C22 1 0.789346 0.665225 0.506518 11.00000 0.07220 0.05666 = 0.04493 0.01872 0.01588 0.01513 AFIX 137 H22A 2 0.715297 0.623080 0.495000 11.00000 -1.50000 H22B 2 0.791113 0.690711 0.548616 11.00000 -1.50000 H22C 2 0.870519 0.631720 0.506809 11.00000 -1.50000 AFIX 0 C7 1 0.929703 0.555279 0.347211 11.00000 0.03593 0.02984 = 0.05114 0.00731 0.01325 0.01238 C23 1 1.009849 0.811652 0.490695 11.00000 0.04556 0.08185 = 0.06040 -0.02900 0.00093 -0.00607 AFIX 137 H23A 2 1.031041 0.753836 0.513871 11.00000 -1.50000 H23B 2 1.011776 0.862333 0.520753 11.00000 -1.50000 H23C 2 1.073901 0.823220 0.464480 11.00000 -1.50000 AFIX 0 C13 1 1.118551 0.615287 0.436189 11.00000 0.07220 0.09988 = 0.05307 -0.01392 -0.01474 0.04910 AFIX 137 H13A 2 1.163718 0.674173 0.446073 11.00000 -1.50000 H13B 2 1.182646 0.566438 0.435529 11.00000 -1.50000 H13C 2 1.068225 0.601307 0.468438 11.00000 -1.50000 AFIX 0 C24 1 0.887744 0.957949 0.385677 11.00000 0.10727 0.03993 = 0.06127 -0.00666 0.03462 -0.02316 AFIX 137 H24A 2 0.968640 0.939289 0.373300 11.00000 -1.50000 H24B 2 0.908181 0.999068 0.422299 11.00000 -1.50000 H24C 2 0.831679 0.990155 0.350427 11.00000 -1.50000 AFIX 0 C26 1 0.696069 0.559582 0.037101 11.00000 0.19866 0.06661 = 0.10820 0.01676 0.10689 0.01183 PART 1 AFIX 23 H26C 2 0.667438 0.576908 -0.007899 10.50000 -1.20000 H26D 2 0.788406 0.578539 0.050036 10.50000 -1.20000 AFIX 23 PART -1 H26A 2 0.654961 0.564141 -0.008321 10.50000 -1.20000 H26B 2 0.785233 0.585059 0.042612 10.50000 -1.20000 AFIX 0 CL1B 3 0.707322 0.448463 0.057235 10.50000 0.14217 0.07527 = 0.06920 0.01890 0.03266 0.04924 HKLF 4 REM fed728_100_final_a.res in P2(1)/c REM wR2 = 0.0797, GooF = S = 1.045, Restrained GooF = 1.045 for all data REM R1 = 0.0341 for 6874 Fo > 4sig(Fo) and 0.0500 for all 8935 data REM 317 parameters refined using 6 restraints END WGHT 0.0327 0.0000 REM Highest difference peak 0.924, deepest hole -1.354, 1-sigma level 0.155 Q1 1 0.2897 0.7490 0.1619 11.00000 0.05 0.92 Q2 1 0.4771 0.8976 0.0619 11.00000 0.05 0.83 Q3 1 0.7859 0.4943 0.0447 11.00000 0.05 0.83 Q4 1 0.5756 0.9549 0.0839 11.00000 0.05 0.67 Q5 1 1.0766 0.6193 0.3999 11.00000 0.05 0.65 Q6 1 0.8989 0.7418 0.3400 11.00000 0.05 0.63 Q7 1 0.8040 0.6443 0.2798 11.00000 0.05 0.61 Q8 1 0.6269 0.6384 0.2805 11.00000 0.05 0.61 Q9 1 0.8918 0.6603 0.2793 11.00000 0.05 0.60 Q10 1 0.6338 0.9371 0.2407 11.00000 0.05 0.59 Q11 1 0.4388 0.6043 0.2779 11.00000 0.05 0.57 Q12 1 0.7135 0.7208 0.3365 11.00000 0.05 0.56 Q13 1 0.9465 0.6003 0.2773 11.00000 0.05 0.56 Q14 1 0.4011 0.8969 0.0812 11.00000 0.05 0.55 Q15 1 0.7562 1.0161 0.2822 11.00000 0.05 0.54 Q16 1 0.5766 0.5521 -0.0243 11.00000 0.05 0.53 ; _shelx_res_checksum 95427 _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 2.629 _oxdiff_exptl_absorpt_empirical_full_min 0.610 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 0.80398(2) 0.71581(2) 0.33896(2) 0.02632(6) Uani 1 1 d . . . . . I1 I 0.52401(3) 0.61708(2) 0.28001(2) 0.03872(8) Uani 1 1 d . . . . . I4 I 0.82202(3) 0.93961(2) 0.20048(2) 0.04495(8) Uani 1 1 d . . . . . I3 I 0.48599(3) 0.93819(2) 0.08209(2) 0.04548(8) Uani 1 1 d . . . . . I2 I 0.29338(3) 0.72369(2) 0.12953(2) 0.05969(11) Uani 1 1 d . . . . . Cl2 Cl 0.60885(18) 0.62698(12) 0.07912(8) 0.0785(5) Uani 1 1 d . . . . . Cl1A Cl 0.6937(10) 0.4447(7) 0.0401(6) 0.138(4) Uani 0.5 1 d . U P A 1 N1 N 0.6783(3) 0.7743(2) 0.24109(16) 0.0307(7) Uani 1 1 d . . . . . C5 C 0.6695(4) 0.8456(3) 0.19827(18) 0.0291(8) Uani 1 1 d . . . . . C2 C 0.5606(4) 0.7298(3) 0.22485(19) 0.0305(8) Uani 1 1 d . . . . . C10 C 0.9577(4) 0.6486(3) 0.2651(2) 0.0378(9) Uani 1 1 d . . . . . C6 C 0.8881(4) 0.5710(3) 0.2816(2) 0.0366(9) Uani 1 1 d . . . . . C8 C 1.0275(4) 0.6214(3) 0.3721(2) 0.0419(10) Uani 1 1 d . . . . . C21 C 0.5205(5) 0.7372(4) 0.4239(3) 0.0561(13) Uani 1 1 d . . . . . H21A H 0.456885 0.755032 0.385947 0.084 Uiso 1 1 calc R U . . . H21B H 0.495003 0.763547 0.461269 0.084 Uiso 1 1 calc R U . . . H21C H 0.523159 0.669941 0.427503 0.084 Uiso 1 1 calc R U . . . C20 C 0.6805(5) 0.8525(3) 0.3849(2) 0.0387(9) Uani 1 1 d . . . . . C19 C 0.8169(5) 0.8724(3) 0.4029(2) 0.0395(10) Uani 1 1 d . . . . . C4 C 0.5494(4) 0.8449(3) 0.15593(19) 0.0313(8) Uani 1 1 d . . . . . C9 C 1.0430(4) 0.6800(3) 0.3210(2) 0.0394(10) Uani 1 1 d . . . . . C3 C 0.4784(4) 0.7695(3) 0.1733(2) 0.0320(8) Uani 1 1 d . . . . . C16 C 0.6552(4) 0.7731(3) 0.4194(2) 0.0345(9) Uani 1 1 d . . . . . C25 C 0.5778(6) 0.9113(4) 0.3423(3) 0.0615(15) Uani 1 1 d . . . . . H25A H 0.620819 0.955621 0.319233 0.092 Uiso 1 1 calc R U . . . H25B H 0.526489 0.944494 0.368128 0.092 Uiso 1 1 calc R U . . . H25C H 0.520189 0.871620 0.312126 0.092 Uiso 1 1 calc R U . . . C15 C 0.9523(6) 0.6815(4) 0.1980(3) 0.0638(15) Uani 1 1 d . . . . . H15A H 0.861926 0.680063 0.174313 0.096 Uiso 1 1 calc R U . . . H15B H 1.005779 0.641072 0.177509 0.096 Uiso 1 1 calc R U . . . H15C H 0.985691 0.744567 0.198907 0.096 Uiso 1 1 calc R U . . . C12 C 0.8879(6) 0.4760(4) 0.3843(3) 0.0712(19) Uani 1 1 d . . . . . H12A H 0.900143 0.493290 0.428928 0.107 Uiso 1 1 calc R U . . . H12B H 0.940765 0.421624 0.380278 0.107 Uiso 1 1 calc R U . . . H12C H 0.795795 0.462052 0.367621 0.107 Uiso 1 1 calc R U . . . C11 C 0.8007(5) 0.5085(4) 0.2339(3) 0.0651(16) Uani 1 1 d . . . . . H11A H 0.751110 0.467589 0.256093 0.098 Uiso 1 1 calc R U . . . H11B H 0.854752 0.471623 0.211361 0.098 Uiso 1 1 calc R U . . . H11C H 0.740381 0.546273 0.203518 0.098 Uiso 1 1 calc R U . . . C14 C 1.1433(5) 0.7566(4) 0.3232(4) 0.0744(19) Uani 1 1 d . . . . . H14A H 1.099363 0.813049 0.305361 0.112 Uiso 1 1 calc R U . . . H14B H 1.207511 0.738281 0.298458 0.112 Uiso 1 1 calc R U . . . H14C H 1.187490 0.767631 0.367081 0.112 Uiso 1 1 calc R U . . . C17 C 0.7755(4) 0.7434(3) 0.4584(2) 0.0346(9) Uani 1 1 d . . . . . C18 C 0.8745(4) 0.8048(3) 0.4487(2) 0.0374(9) Uani 1 1 d . . . . . C22 C 0.7893(6) 0.6652(4) 0.5065(3) 0.0574(13) Uani 1 1 d . . . . . H22A H 0.715297 0.623080 0.495000 0.086 Uiso 1 1 calc R U . . . H22B H 0.791113 0.690711 0.548616 0.086 Uiso 1 1 calc R U . . . H22C H 0.870519 0.631720 0.506809 0.086 Uiso 1 1 calc R U . . . C7 C 0.9297(4) 0.5553(3) 0.3472(2) 0.0384(10) Uani 1 1 d . . . . . C23 C 1.0098(5) 0.8117(4) 0.4907(3) 0.0641(15) Uani 1 1 d . . . . . H23A H 1.031041 0.753836 0.513871 0.096 Uiso 1 1 calc R U . . . H23B H 1.011776 0.862333 0.520753 0.096 Uiso 1 1 calc R U . . . H23C H 1.073901 0.823220 0.464480 0.096 Uiso 1 1 calc R U . . . C13 C 1.1186(6) 0.6153(5) 0.4362(3) 0.079(2) Uani 1 1 d . . . . . H13A H 1.163718 0.674173 0.446073 0.119 Uiso 1 1 calc R U . . . H13B H 1.182646 0.566438 0.435529 0.119 Uiso 1 1 calc R U . . . H13C H 1.068225 0.601307 0.468438 0.119 Uiso 1 1 calc R U . . . C24 C 0.8877(7) 0.9579(3) 0.3857(3) 0.0670(17) Uani 1 1 d . . . . . H24A H 0.968640 0.939289 0.373300 0.101 Uiso 1 1 calc R U . . . H24B H 0.908181 0.999068 0.422299 0.101 Uiso 1 1 calc R U . . . H24C H 0.831679 0.990155 0.350427 0.101 Uiso 1 1 calc R U . . . C26 C 0.6961(11) 0.5596(5) 0.0371(5) 0.114(3) Uani 1 1 d . . . . . H26C H 0.667438 0.576908 -0.007899 0.136 Uiso 0.5 1 calc R U P A 1 H26D H 0.788406 0.578539 0.050036 0.136 Uiso 0.5 1 calc R U P A 1 H26A H 0.654961 0.564141 -0.008321 0.136 Uiso 0.5 1 calc R U P A -1 H26B H 0.785233 0.585059 0.042612 0.136 Uiso 0.5 1 calc R U P A -1 Cl1B Cl 0.7073(10) 0.4485(6) 0.0572(3) 0.094(3) 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 0.02546(10) 0.02634(10) 0.02537(10) -0.00038(7) 0.00121(7) 0.00331(6) I1 0.03976(15) 0.03457(14) 0.04104(16) 0.00235(11) 0.00657(12) -0.01094(10) I4 0.04004(16) 0.04245(16) 0.05163(19) 0.00685(13) 0.00788(13) -0.01166(11) I3 0.05239(18) 0.04782(17) 0.03473(16) 0.01112(12) 0.00563(13) 0.01640(12) I2 0.03321(16) 0.0579(2) 0.0762(3) -0.00079(17) -0.01552(15) -0.00652(12) Cl2 0.0930(12) 0.0821(11) 0.0605(10) 0.0066(8) 0.0164(8) 0.0288(8) Cl1A 0.084(4) 0.073(4) 0.260(12) -0.042(6) 0.041(6) -0.007(3) N1 0.0270(16) 0.0357(17) 0.0276(17) 0.0020(14) 0.0013(13) -0.0019(12) C5 0.0289(19) 0.0310(18) 0.0269(19) 0.0025(15) 0.0046(15) -0.0001(14) C2 0.0289(19) 0.0300(19) 0.032(2) 0.0004(15) 0.0041(16) -0.0025(14) C10 0.042(2) 0.037(2) 0.038(2) 0.0043(18) 0.0143(19) 0.0130(17) C6 0.034(2) 0.0284(19) 0.047(3) -0.0080(17) 0.0073(18) 0.0056(15) C8 0.035(2) 0.046(2) 0.042(3) -0.007(2) 0.0010(19) 0.0178(18) C21 0.038(3) 0.073(3) 0.060(3) -0.020(3) 0.016(2) -0.007(2) C20 0.055(3) 0.031(2) 0.029(2) -0.0002(16) 0.0052(19) 0.0161(17) C19 0.053(3) 0.029(2) 0.039(2) -0.0091(18) 0.015(2) -0.0024(17) C4 0.031(2) 0.0310(19) 0.031(2) -0.0008(16) 0.0035(16) 0.0053(14) C9 0.026(2) 0.038(2) 0.055(3) -0.006(2) 0.0085(19) -0.0008(16) C3 0.0280(19) 0.0319(19) 0.034(2) -0.0071(16) 0.0008(16) -0.0029(14) C16 0.034(2) 0.038(2) 0.032(2) -0.0047(17) 0.0064(17) 0.0049(15) C25 0.081(4) 0.057(3) 0.045(3) 0.004(2) 0.008(3) 0.042(3) C15 0.080(4) 0.072(3) 0.046(3) 0.010(3) 0.029(3) 0.027(3) C12 0.083(4) 0.047(3) 0.095(5) 0.035(3) 0.045(4) 0.025(3) C11 0.050(3) 0.059(3) 0.081(4) -0.035(3) 0.003(3) 0.003(2) C14 0.044(3) 0.063(3) 0.122(6) -0.015(4) 0.030(4) -0.012(2) C17 0.042(2) 0.034(2) 0.027(2) -0.0020(16) 0.0065(17) 0.0050(16) C18 0.035(2) 0.044(2) 0.033(2) -0.0076(18) 0.0042(17) 0.0021(17) C22 0.072(4) 0.057(3) 0.045(3) 0.019(2) 0.016(3) 0.015(2) C7 0.036(2) 0.030(2) 0.051(3) 0.0073(18) 0.013(2) 0.0124(16) C23 0.046(3) 0.082(4) 0.060(4) -0.029(3) 0.001(3) -0.006(2) C13 0.072(4) 0.100(5) 0.053(4) -0.014(3) -0.015(3) 0.049(3) C24 0.107(5) 0.040(3) 0.061(4) -0.007(2) 0.035(4) -0.023(3) C26 0.199(10) 0.067(4) 0.108(6) 0.017(4) 0.107(7) 0.012(5) Cl1B 0.142(6) 0.075(4) 0.069(2) 0.019(2) 0.033(3) 0.049(4) 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 -7 6 -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 61.92(7) . . ? N1 Dy1 C10 83.77(12) . . ? N1 Dy1 C6 92.46(13) . . ? N1 Dy1 C8 134.84(13) . . ? N1 Dy1 C20 81.10(12) . . ? N1 Dy1 C19 96.61(13) . . ? N1 Dy1 C9 107.50(13) . . ? N1 Dy1 C16 100.02(12) . . ? N1 Dy1 C17 129.97(12) . . ? N1 Dy1 C18 127.72(12) . . ? N1 Dy1 C7 122.75(13) . . ? C10 Dy1 I1 102.13(10) . . ? C10 Dy1 C6 30.90(13) . . ? C10 Dy1 C8 51.12(14) . . ? C10 Dy1 C16 175.72(12) . . ? C10 Dy1 C17 145.84(13) . . ? C6 Dy1 I1 80.29(9) . . ? C6 Dy1 C8 50.91(14) . . ? C6 Dy1 C16 146.06(13) . . ? C6 Dy1 C17 132.33(13) . . ? C8 Dy1 I1 122.88(10) . . ? C8 Dy1 C16 125.14(14) . . ? C8 Dy1 C17 94.86(13) . . ? C20 Dy1 I1 90.32(10) . . ? C20 Dy1 C10 152.96(13) . . ? C20 Dy1 C6 170.36(14) . . ? C20 Dy1 C8 138.13(14) . . ? C20 Dy1 C16 30.85(13) . . ? C20 Dy1 C17 51.19(13) . . ? C19 Dy1 I1 121.52(10) . . ? C19 Dy1 C10 130.69(14) . . ? C19 Dy1 C6 158.12(14) . . ? C19 Dy1 C8 110.62(15) . . ? C19 Dy1 C20 31.20(14) . . ? C19 Dy1 C9 107.21(13) . . ? C19 Dy1 C16 51.17(13) . . ? C19 Dy1 C17 51.34(13) . . ? C19 Dy1 C18 31.34(13) . . ? C19 Dy1 C7 138.12(15) . . ? C9 Dy1 I1 130.62(9) . . ? C9 Dy1 C10 30.84(14) . . ? C9 Dy1 C6 50.95(13) . . ? C9 Dy1 C8 31.03(14) . . ? C9 Dy1 C20 137.91(14) . . ? C9 Dy1 C16 147.26(14) . . ? C9 Dy1 C17 117.66(14) . . ? C9 Dy1 C18 97.43(13) . . ? C16 Dy1 I1 78.13(9) . . ? C17 Dy1 I1 99.75(9) . . ? C17 Dy1 C16 30.77(13) . . ? C18 Dy1 I1 128.15(9) . . ? C18 Dy1 C10 128.12(14) . . ? C18 Dy1 C6 137.22(14) . . ? C18 Dy1 C8 86.82(13) . . ? C18 Dy1 C20 51.36(13) . . ? C18 Dy1 C16 50.77(13) . . ? C18 Dy1 C17 30.63(13) . . ? C7 Dy1 I1 91.95(10) . . ? C7 Dy1 C10 51.00(13) . . ? C7 Dy1 C6 30.64(14) . . ? C7 Dy1 C8 30.94(14) . . ? C7 Dy1 C20 153.63(14) . . ? C7 Dy1 C9 51.11(13) . . ? C7 Dy1 C16 124.79(13) . . ? C7 Dy1 C17 102.60(14) . . ? C7 Dy1 C18 108.79(14) . . ? C2 I1 Dy1 68.07(11) . . ? C5 N1 Dy1 143.6(3) . . ? C2 N1 Dy1 111.0(2) . . ? C2 N1 C5 104.5(3) . . ? N1 C5 I4 122.0(3) . . ? N1 C5 C4 111.1(3) . . ? C4 C5 I4 126.9(3) . . ? N1 C2 I1 118.8(3) . . ? N1 C2 C3 112.7(3) . . ? C3 C2 I1 128.5(3) . . ? C6 C10 Dy1 74.7(2) . . ? C6 C10 C15 124.7(5) . . ? C9 C10 Dy1 74.1(2) . . ? C9 C10 C6 107.7(4) . . ? C9 C10 C15 127.2(5) . . ? C15 C10 Dy1 123.3(3) . . ? C10 C6 Dy1 74.4(2) . . ? C10 C6 C11 124.4(5) . . ? C11 C6 Dy1 124.7(3) . . ? C7 C6 Dy1 74.1(2) . . ? C7 C6 C10 108.2(4) . . ? C7 C6 C11 126.8(4) . . ? C9 C8 Dy1 73.9(2) . . ? C9 C8 C13 126.2(5) . . ? C7 C8 Dy1 73.9(2) . . ? C7 C8 C9 107.2(4) . . ? C7 C8 C13 125.0(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 73.6(2) . . ? C19 C20 C25 126.3(4) . . ? C16 C20 Dy1 75.6(2) . . ? C16 C20 C19 107.8(4) . . ? C16 C20 C25 125.7(5) . . ? C25 C20 Dy1 121.8(3) . . ? C20 C19 Dy1 75.2(2) . . ? C20 C19 C18 107.6(4) . . ? C20 C19 C24 127.2(5) . . ? C18 C19 Dy1 75.0(2) . . ? C18 C19 C24 124.5(5) . . ? C24 C19 Dy1 122.9(3) . . ? C5 C4 I3 126.6(3) . . ? C5 C4 C3 106.5(3) . . ? C3 C4 I3 126.9(3) . . ? C10 C9 Dy1 75.1(2) . . ? C10 C9 C8 108.4(4) . . ? C10 C9 C14 124.6(5) . . ? C8 C9 Dy1 75.1(2) . . ? C8 C9 C14 126.7(5) . . ? C14 C9 Dy1 121.1(3) . . ? C2 C3 I2 126.7(3) . . ? C2 C3 C4 105.1(3) . . ? C4 C3 I2 128.1(3) . . ? C21 C16 Dy1 127.0(3) . . ? C20 C16 Dy1 73.5(2) . . ? C20 C16 C21 125.7(4) . . ? C20 C16 C17 108.3(4) . . ? C17 C16 Dy1 74.3(2) . . ? C17 C16 C21 125.0(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 74.9(2) . . ? C16 C17 C22 125.0(4) . . ? C18 C17 Dy1 73.8(2) . . ? C18 C17 C16 107.9(4) . . ? C18 C17 C22 126.9(4) . . ? C22 C17 Dy1 122.0(3) . . ? C19 C18 Dy1 73.6(2) . . ? C19 C18 C23 124.9(4) . . ? C17 C18 Dy1 75.6(2) . . ? C17 C18 C19 108.5(4) . . ? C17 C18 C23 125.1(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 75.3(2) . . ? C6 C7 C8 108.6(4) . . ? C6 C7 C12 126.1(5) . . ? C8 C7 Dy1 75.1(2) . . ? C8 C7 C12 125.0(5) . . ? C12 C7 Dy1 120.3(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 106.8 . . ? Cl2 C26 H26D 106.8 . . ? Cl2 C26 H26A 108.4 . . ? Cl2 C26 H26B 108.4 . . ? Cl1A C26 Cl2 122.2(6) . . ? Cl1A C26 H26C 106.8 . . ? Cl1A C26 H26D 106.8 . . ? Cl1A C26 H26A 95.7 . . ? Cl1A C26 H26B 113.0 . . ? H26C C26 H26D 106.6 . . ? H26C C26 H26A 13.1 . . ? H26C C26 H26B 96.3 . . ? H26D C26 H26A 117.4 . . ? H26D C26 H26B 10.6 . . ? H26A C26 H26B 107.5 . . ? Cl1B C26 Cl2 115.4(5) . . ? Cl1B C26 Cl1A 12.8(6) . . ? Cl1B C26 H26C 119.5 . . ? Cl1B C26 H26D 100.6 . . ? 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 3.2465(3) . ? Dy1 N1 2.381(3) . ? Dy1 C10 2.653(4) . ? Dy1 C6 2.656(4) . ? Dy1 C8 2.656(4) . ? Dy1 C20 2.646(4) . ? Dy1 C19 2.625(4) . ? Dy1 C9 2.640(4) . ? Dy1 C16 2.673(4) . ? Dy1 C17 2.665(4) . ? Dy1 C18 2.643(4) . ? Dy1 C7 2.640(4) . ? I1 C2 2.087(4) . ? I4 C5 2.076(4) . ? I3 C4 2.074(4) . ? I2 C3 2.063(4) . ? Cl2 C26 1.706(7) . ? Cl1A C26 1.654(12) . ? N1 C5 1.366(5) . ? N1 C2 1.359(5) . ? C5 C4 1.381(5) . ? C2 C3 1.373(6) . ? C10 C6 1.414(6) . ? C10 C9 1.407(6) . ? C10 C15 1.503(7) . ? C6 C11 1.514(6) . ? C6 C7 1.399(6) . ? C8 C9 1.417(7) . ? C8 C7 1.413(6) . ? C8 C13 1.498(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21 C16 1.513(6) . ? C20 C19 1.418(6) . ? C20 C16 1.415(6) . ? C20 C25 1.511(6) . ? C19 C18 1.423(6) . ? C19 C24 1.518(6) . ? C4 C3 1.404(5) . ? C9 C14 1.511(6) . ? C16 C17 1.416(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 1.504(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 1.402(6) . ? C17 C22 1.512(6) . ? C18 C23 1.506(7) . ? 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 1.653(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 12.7(6) . . . . ? Dy1 N1 C5 C4 -167.2(3) . . . . ? Dy1 N1 C2 I1 -6.0(3) . . . . ? Dy1 N1 C2 C3 172.1(3) . . . . ? Dy1 C10 C6 C11 121.7(4) . . . . ? Dy1 C10 C6 C7 -67.0(3) . . . . ? Dy1 C10 C9 C8 68.3(3) . . . . ? Dy1 C10 C9 C14 -117.7(4) . . . . ? Dy1 C6 C7 C8 -68.4(3) . . . . ? Dy1 C6 C7 C12 117.0(4) . . . . ? Dy1 C8 C9 C10 -68.3(3) . . . . ? Dy1 C8 C9 C14 117.9(4) . . . . ? Dy1 C8 C7 C6 68.5(3) . . . . ? Dy1 C8 C7 C12 -116.9(4) . . . . ? Dy1 C20 C19 C18 -68.7(3) . . . . ? Dy1 C20 C19 C24 120.4(5) . . . . ? Dy1 C20 C16 C21 -124.1(4) . . . . ? Dy1 C20 C16 C17 66.7(3) . . . . ? Dy1 C19 C18 C17 -68.2(3) . . . . ? Dy1 C19 C18 C23 125.1(4) . . . . ? Dy1 C16 C17 C18 67.0(3) . . . . ? Dy1 C16 C17 C22 -118.7(4) . . . . ? Dy1 C17 C18 C19 66.9(3) . . . . ? Dy1 C17 C18 C23 -126.5(4) . . . . ? I1 C2 C3 I2 -4.5(5) . . . . ? I1 C2 C3 C4 177.6(3) . . . . ? I4 C5 C4 I3 -0.2(5) . . . . ? I4 C5 C4 C3 -179.4(3) . . . . ? I3 C4 C3 I2 2.8(5) . . . . ? I3 C4 C3 C2 -179.3(3) . . . . ? N1 C5 C4 I3 179.6(3) . . . . ? N1 C5 C4 C3 0.4(4) . . . . ? N1 C2 C3 I2 177.7(3) . . . . ? N1 C2 C3 C4 -0.2(5) . . . . ? C5 N1 C2 I1 -177.6(2) . . . . ? C5 N1 C2 C3 0.5(5) . . . . ? C5 C4 C3 I2 -178.0(3) . . . . ? C5 C4 C3 C2 -0.1(4) . . . . ? C2 N1 C5 I4 179.3(3) . . . . ? C2 N1 C5 C4 -0.6(4) . . . . ? C10 C6 C7 Dy1 67.2(3) . . . . ? C10 C6 C7 C8 -1.2(4) . . . . ? C10 C6 C7 C12 -175.8(4) . . . . ? C6 C10 C9 Dy1 -67.7(3) . . . . ? C6 C10 C9 C8 0.6(4) . . . . ? C6 C10 C9 C14 174.6(4) . . . . ? C21 C16 C17 Dy1 124.5(4) . . . . ? C21 C16 C17 C18 -168.5(4) . . . . ? C21 C16 C17 C22 5.8(7) . . . . ? C20 C19 C18 Dy1 68.8(3) . . . . ? C20 C19 C18 C17 0.6(5) . . . . ? C20 C19 C18 C23 -166.0(4) . . . . ? C20 C16 C17 Dy1 -66.2(3) . . . . ? C20 C16 C17 C18 0.8(4) . . . . ? C20 C16 C17 C22 175.0(4) . . . . ? C19 C20 C16 Dy1 -67.1(3) . . . . ? C19 C20 C16 C21 168.8(4) . . . . ? C19 C20 C16 C17 -0.4(4) . . . . ? C9 C10 C6 Dy1 67.3(3) . . . . ? C9 C10 C6 C11 -171.0(4) . . . . ? C9 C10 C6 C7 0.4(4) . . . . ? C9 C8 C7 Dy1 -66.9(3) . . . . ? C9 C8 C7 C6 1.6(4) . . . . ? C9 C8 C7 C12 176.2(4) . . . . ? C16 C20 C19 Dy1 68.5(3) . . . . ? C16 C20 C19 C18 -0.2(5) . . . . ? C16 C20 C19 C24 -171.1(4) . . . . ? C16 C17 C18 Dy1 -67.8(3) . . . . ? C16 C17 C18 C19 -0.9(4) . . . . ? C16 C17 C18 C23 165.8(4) . . . . ? C25 C20 C19 Dy1 -117.7(4) . . . . ? C25 C20 C19 C18 173.6(4) . . . . ? C25 C20 C19 C24 2.7(7) . . . . ? C25 C20 C16 Dy1 119.1(4) . . . . ? C25 C20 C16 C21 -5.0(7) . . . . ? C25 C20 C16 C17 -174.2(4) . . . . ? C15 C10 C6 Dy1 -120.1(4) . . . . ? C15 C10 C6 C11 1.6(6) . . . . ? C15 C10 C6 C7 172.9(4) . . . . ? C15 C10 C9 Dy1 120.0(4) . . . . ? C15 C10 C9 C8 -171.7(4) . . . . ? C15 C10 C9 C14 2.2(7) . . . . ? C11 C6 C7 Dy1 -121.7(4) . . . . ? C11 C6 C7 C8 169.8(4) . . . . ? C11 C6 C7 C12 -4.7(7) . . . . ? C22 C17 C18 Dy1 118.1(4) . . . . ? C22 C17 C18 C19 -175.0(4) . . . . ? C22 C17 C18 C23 -8.3(7) . . . . ? C7 C8 C9 Dy1 66.9(3) . . . . ? C7 C8 C9 C10 -1.4(4) . . . . ? C7 C8 C9 C14 -175.1(4) . . . . ? C13 C8 C9 Dy1 -126.5(4) . . . . ? C13 C8 C9 C10 165.2(4) . . . . ? C13 C8 C9 C14 -8.6(7) . . . . ? C13 C8 C7 Dy1 126.3(4) . . . . ? C13 C8 C7 C6 -165.2(4) . . . . ? C13 C8 C7 C12 9.4(7) . . . . ? C24 C19 C18 Dy1 -119.9(4) . . . . ? C24 C19 C18 C17 171.9(4) . . . . ? C24 C19 C18 C23 5.2(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 -0.9735 -1.0910 0.1612 -0.0783 -0.0142 0.0325 -1.0501 0.9227 0.0392 0.0038 0.0040 0.0859 0.9735 1.0910 -0.1612 0.0783 0.0142 -0.0325 1.0501 -0.9227 -0.0392 -0.0038 -0.0040 -0.0859 -0.0178 -0.0379 -0.9967 -0.0100 0.0322 0.0044 0.0178 0.0379 0.9967 0.0100 -0.0322 -0.0044 -1.0144 0.9986 2.0326 0.0239 -0.0605 0.0770 1.0144 -0.9986 -2.0326 -0.0239 0.0605 -0.0770 1.0679 -0.8848 0.9575 0.0063 -0.0363 -0.0903 -0.0026 1.0827 1.9323 0.0612 -0.0554 0.0178 2.0798 -0.8006 0.8572 0.0435 -0.0312 -0.1495 -0.0740 0.9310 -2.0543 0.0210 0.0736 0.0356 -1.0475 -0.1600 -1.8931 -0.0574 0.0594 0.0681 -0.9761 -0.0082 2.0936 -0.0172 -0.0696 0.0503 -6.5009 5.9807 -22.2214 -0.1415 0.7602 0.6341