#------------------------------------------------------------------------------ #$Date: 2024-07-27 01:11:00 +0300 (Sat, 27 Jul 2024) $ #$Revision: 293554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572191.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_1572191 loop_ _publ_author_name 'Delano, Francis' 'Benner, Florian' 'Jang, Seoyun' 'Greer, Samuel M.' 'Demir, Selvan' _publ_section_title ; Construction of intermolecular \s-hole interactions in rare earth metallocene complexes using a 2,3,4,5-tetraiodopyrrolyl anion ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC03786C _journal_year 2024 _chemical_formula_moiety 'C26 H38 Dy N' _chemical_formula_sum 'C26 H38 Dy N' _chemical_formula_weight 527.07 _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 2024-02-07 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-04-22 deposited with the CCDC. 2024-07-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 98.5100(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.34360(10) _cell_length_b 15.2429(2) _cell_length_c 16.38150(10) _cell_measurement_reflns_used 13664 _cell_measurement_temperature 100.0(2) _cell_measurement_theta_max 79.7040 _cell_measurement_theta_min 2.9020 _cell_volume 2307.42(4) _computing_cell_refinement 'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.986 _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 -19.00 74.00 0.50 0.07 -- 47.10 -87.00-139.00 186 2 \w -163.00 -81.00 0.50 0.27 -- -91.75 -87.00-139.00 164 3 \w -78.00 -19.00 0.50 0.27 -- -91.75 87.00 -22.00 118 4 \w 103.00 178.00 0.50 0.27 -- 113.25 87.00 -22.00 150 5 \w 42.00 104.00 0.50 0.27 -- 113.25 -87.00-139.00 124 6 \w -47.00 26.00 0.50 0.07 -- -47.10 37.00 90.00 146 7 \w -39.00 28.00 0.50 0.07 -- -47.10 19.00 -30.00 134 8 \w -74.00 26.00 0.50 0.07 -- -47.10 87.00 -22.00 200 9 \w 36.00 93.00 0.50 0.07 -- 47.10-125.00 60.00 114 10 \w -53.00 -20.00 0.50 0.27 -- -91.75 45.00 120.00 66 11 \w 101.00 178.00 0.50 0.27 -- 113.25 30.00 -90.00 154 12 \w 42.00 69.00 0.50 0.27 -- 113.25 -61.00 -90.00 54 13 \w 42.00 94.00 0.50 0.27 -- 113.25 -77.00 120.00 104 14 \w 42.00 94.00 0.50 0.27 -- 113.25 -77.00 -90.00 104 15 \w 42.00 69.00 0.50 0.27 -- 113.25 -61.00 90.00 54 16 \w 42.00 69.00 0.50 0.27 -- 113.25 -61.00-150.00 54 17 \w 44.00 108.00 0.50 0.27 -- 113.25-125.00 90.00 128 18 \w 42.00 69.00 0.50 0.27 -- 113.25 -61.00 -60.00 54 19 \w 42.00 94.00 0.50 0.27 -- 113.25 -77.00 -60.00 104 20 \w 106.00 178.00 0.50 0.27 -- 113.25 61.00 150.00 144 21 \w 42.00 94.00 0.50 0.27 -- 113.25 -77.00-120.00 104 22 \w 42.00 69.00 0.50 0.27 -- 113.25 -61.00 150.00 54 23 \w 101.00 178.00 0.50 0.27 -- 113.25 30.00 120.00 154 24 \w 110.00 178.00 0.50 0.27 -- 113.25 77.00 30.00 136 25 \w 42.00 69.00 0.50 0.27 -- 113.25 -61.00 -30.00 54 26 \w 42.00 94.00 0.50 0.27 -- 113.25 -77.00 0.00 104 27 \w 110.00 178.00 0.50 0.27 -- 113.25 77.00-180.00 136 28 \w 47.00 99.00 0.50 0.27 -- 113.25 -94.00 90.00 104 29 \w 42.00 74.00 0.50 0.27 -- 113.25 -77.00 60.00 64 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_unetI/netI 0.0353 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 25149 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.274 _diffrn_reflns_theta_min 3.982 _exptl_absorpt_coefficient_mu 17.376 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.357 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.100a (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 1.517 _exptl_crystal_description block _exptl_crystal_F_000 1068 _exptl_crystal_size_max 0.283 _exptl_crystal_size_mid 0.174 _exptl_crystal_size_min 0.138 _refine_diff_density_max 1.894 _refine_diff_density_min -1.069 _refine_diff_density_rms 0.122 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 265 _refine_ls_number_reflns 4967 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.073 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0306 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0551P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.0849 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4473 _reflns_number_total 4967 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03786c2.cif _cod_data_source_block Cpstar2DyDMP _cod_database_code 1572191 _shelx_shelxl_version_number 2018/3 _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 0.198 _shelx_estimated_absorpt_t_min 0.084 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C2(H2) 2.b Idealised Me refined as rotating group: C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C15(H15A,H15B, H15C), C25(H25A,H25B,H25C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C16(H16A, H16B,H16C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C5(H5A,H5B,H5C), C6(H6A, H6B,H6C) ; _shelx_res_file ; TITL fed745_final_a.res in P2(1)/c fed745_final.res created by SHELXL-2018/3 at 11:03:17 on 07-Feb-2024 REM Old TITL FED745_Final in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.055, Rweak 0.004, Alpha 0.032 REM 0.526 for 195 systematic absences, Orientation as input REM Formula found by SHELXT: C26 N Dy CELL 1.54184 9.3436 15.2429 16.3815 90 98.51 90 ZERR 4 0.0001 0.0002 0.0001 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Dy N UNIT 104 152 4 4 L.S. 4 0 0 PLAN 7 SIZE 0.138 0.174 0.283 TEMP -173 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.055100 FVAR 0.31246 DY1 3 0.248504 0.411654 0.246732 11.00000 0.00960 0.01206 = 0.01008 -0.00042 0.00225 -0.00177 N1 4 0.066891 0.381800 0.323190 11.00000 0.01159 0.01500 = 0.01278 -0.00071 0.00315 -0.00070 C8 1 0.197942 0.328829 0.103918 11.00000 0.01559 0.01575 = 0.00987 -0.00187 0.00172 -0.00134 C9 1 0.060431 0.357210 0.120720 11.00000 0.01231 0.01705 = 0.01073 -0.00222 -0.00030 -0.00135 C17 1 0.529734 0.420133 0.297664 11.00000 0.00945 0.01919 = 0.01654 -0.00081 0.00113 -0.00286 C4 1 -0.024547 0.418751 0.372081 11.00000 0.01105 0.02026 = 0.01348 -0.00317 0.00297 -0.00169 C20 1 0.392484 0.534093 0.335900 11.00000 0.01244 0.01388 = 0.01781 -0.00171 -0.00022 -0.00262 C13 1 0.248667 0.235517 0.096461 11.00000 0.02242 0.01723 = 0.01982 -0.00294 0.00619 0.00087 AFIX 137 H13A 2 0.181246 0.195356 0.117898 11.00000 -1.50000 H13B 2 0.345380 0.228646 0.128325 11.00000 -1.50000 H13C 2 0.252300 0.221985 0.038320 11.00000 -1.50000 AFIX 0 C1 1 0.088216 0.295846 0.349237 11.00000 0.01506 0.01507 = 0.01722 -0.00117 0.00139 -0.00204 C10 1 0.058666 0.450413 0.117531 11.00000 0.01673 0.01826 = 0.01207 0.00075 -0.00055 0.00279 C7 1 0.279832 0.404274 0.087910 11.00000 0.01619 0.01914 = 0.01060 -0.00025 0.00313 -0.00158 C19 1 0.383558 0.463617 0.391433 11.00000 0.01135 0.01859 = 0.01265 -0.00330 0.00112 -0.00334 C14 1 -0.064970 0.298962 0.133847 11.00000 0.01485 0.02273 = 0.01848 -0.00277 0.00226 -0.00414 AFIX 137 H14A 2 -0.080578 0.302624 0.191604 11.00000 -1.50000 H14B 2 -0.043192 0.238169 0.120585 11.00000 -1.50000 H14C 2 -0.152491 0.318306 0.097869 11.00000 -1.50000 AFIX 0 C3 1 -0.061830 0.356887 0.427307 11.00000 0.01559 0.02767 = 0.01487 -0.00093 0.00782 -0.00295 AFIX 43 H3 2 -0.124677 0.365613 0.467172 11.00000 -1.20000 AFIX 0 C12 1 0.419855 0.401795 0.053455 11.00000 0.01885 0.02619 = 0.01754 -0.00146 0.00660 -0.00306 AFIX 137 H12A 2 0.478214 0.352162 0.077414 11.00000 -1.50000 H12B 2 0.472979 0.456564 0.067089 11.00000 -1.50000 H12C 2 0.399848 0.395040 -0.006645 11.00000 -1.50000 AFIX 0 C18 1 0.467822 0.393384 0.367813 11.00000 0.01303 0.01565 = 0.01473 0.00045 0.00085 -0.00047 C15 1 -0.066125 0.509322 0.128972 11.00000 0.01984 0.02579 = 0.02359 -0.00123 -0.00040 0.00800 AFIX 137 H15A 2 -0.030037 0.560339 0.162200 11.00000 -1.50000 H15B 2 -0.135008 0.476939 0.157232 11.00000 -1.50000 H15C 2 -0.114577 0.529043 0.074931 11.00000 -1.50000 AFIX 0 C21 1 0.484741 0.507331 0.278517 11.00000 0.01190 0.01760 = 0.01554 0.00113 0.00150 -0.00440 C25 1 0.326176 0.623940 0.340080 11.00000 0.02443 0.01433 = 0.02787 -0.00405 0.00229 0.00111 AFIX 137 H25A 2 0.249152 0.621500 0.374638 11.00000 -1.50000 H25B 2 0.285571 0.643112 0.284346 11.00000 -1.50000 H25C 2 0.400741 0.665564 0.363971 11.00000 -1.50000 AFIX 0 C22 1 0.632665 0.365822 0.255995 11.00000 0.01289 0.02611 = 0.02295 -0.00472 0.00509 0.00117 AFIX 137 H22A 2 0.655721 0.397090 0.207313 11.00000 -1.50000 H22B 2 0.587451 0.309410 0.239023 11.00000 -1.50000 H22C 2 0.721765 0.355643 0.294547 11.00000 -1.50000 AFIX 0 C24 1 0.308829 0.464897 0.466960 11.00000 0.01862 0.02542 = 0.01411 -0.00509 0.00650 -0.00486 AFIX 137 H24A 2 0.246749 0.413059 0.466817 11.00000 -1.50000 H24B 2 0.249661 0.518031 0.466488 11.00000 -1.50000 H24C 2 0.381515 0.464431 0.516656 11.00000 -1.50000 AFIX 0 C16 1 0.224995 0.573465 0.076723 11.00000 0.03015 0.01610 = 0.01950 0.00437 0.00310 -0.00072 AFIX 137 H16A 2 0.322759 0.577089 0.062038 11.00000 -1.50000 H16B 2 0.218741 0.610726 0.124819 11.00000 -1.50000 H16C 2 0.154623 0.593483 0.030088 11.00000 -1.50000 AFIX 0 C26 1 0.544323 0.568412 0.219285 11.00000 0.02014 0.02389 = 0.02319 0.00417 0.00364 -0.00898 AFIX 137 H26A 2 0.472440 0.613732 0.200716 11.00000 -1.50000 H26B 2 0.566293 0.535015 0.171545 11.00000 -1.50000 H26C 2 0.632922 0.596146 0.247136 11.00000 -1.50000 AFIX 0 C2 1 0.011329 0.278289 0.413139 11.00000 0.02221 0.01984 = 0.01697 0.00255 0.00384 -0.00490 AFIX 43 H2 2 0.008163 0.224322 0.441824 11.00000 -1.20000 AFIX 0 C23 1 0.502298 0.310133 0.416102 11.00000 0.02456 0.01898 = 0.02059 0.00643 -0.00044 0.00152 AFIX 137 H23A 2 0.534456 0.265210 0.380054 11.00000 -1.50000 H23B 2 0.415559 0.289507 0.437355 11.00000 -1.50000 H23C 2 0.579332 0.321464 0.462346 11.00000 -1.50000 AFIX 0 C5 1 0.180268 0.233745 0.308519 11.00000 0.01935 0.01552 = 0.02190 -0.00061 0.00429 -0.00171 AFIX 137 H5A 2 0.270631 0.262986 0.300645 11.00000 -1.50000 H5B 2 0.128020 0.215778 0.254806 11.00000 -1.50000 H5C 2 0.202288 0.181902 0.343506 11.00000 -1.50000 AFIX 0 C11 1 0.192338 0.479378 0.097153 11.00000 0.01780 0.01716 = 0.01139 0.00053 0.00072 -0.00017 C6 1 -0.070329 0.512693 0.362770 11.00000 0.02132 0.02379 = 0.02033 -0.00293 0.00596 0.00489 AFIX 137 H6A 2 -0.171163 0.515793 0.335952 11.00000 -1.50000 H6B 2 -0.008266 0.543578 0.328928 11.00000 -1.50000 H6C 2 -0.061551 0.540255 0.417331 11.00000 -1.50000 AFIX 0 HKLF 4 REM fed745_final_a.res in P2(1)/c REM wR2 = 0.0849, GooF = S = 1.073, Restrained GooF = 1.073 for all data REM R1 = 0.0306 for 4473 Fo > 4sig(Fo) and 0.0337 for all 4967 data REM 265 parameters refined using 0 restraints END WGHT 0.0551 0.0000 REM Highest difference peak 1.894, deepest hole -1.069, 1-sigma level 0.122 Q1 1 0.3531 0.4156 0.2447 11.00000 0.05 1.89 Q2 1 0.1446 0.4170 0.2463 11.00000 0.05 1.75 Q3 1 0.3827 0.5181 0.2609 11.00000 0.05 0.47 Q4 1 0.4218 0.4994 0.2677 11.00000 0.05 0.46 Q5 1 0.1294 0.4588 0.0895 11.00000 0.05 0.43 Q6 1 0.5391 0.4712 0.2985 11.00000 0.05 0.40 Q7 1 0.5619 0.3990 0.2782 11.00000 0.05 0.39 ; _shelx_res_checksum 2615 _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 ; 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 0.24850(2) 0.41165(2) 0.24673(2) 0.01050(8) Uani 1 1 d . . . . . N1 N 0.06689(19) 0.38180(12) 0.32319(11) 0.0130(3) Uani 1 1 d . . . . . C8 C 0.1979(2) 0.32883(14) 0.10392(13) 0.0138(4) Uani 1 1 d . . . . . C9 C 0.0604(2) 0.35721(15) 0.12072(13) 0.0136(4) Uani 1 1 d . . . . . C17 C 0.5297(2) 0.42013(15) 0.29766(14) 0.0151(4) Uani 1 1 d . . . . . C4 C -0.0245(2) 0.41875(14) 0.37208(14) 0.0148(4) Uani 1 1 d . . . . . C20 C 0.3925(2) 0.53409(14) 0.33590(13) 0.0150(4) Uani 1 1 d . . . . . C13 C 0.2487(3) 0.23552(15) 0.09646(15) 0.0195(5) Uani 1 1 d . . . . . H13A H 0.181246 0.195356 0.117898 0.029 Uiso 1 1 calc R U . . . H13B H 0.345380 0.228646 0.128325 0.029 Uiso 1 1 calc R U . . . H13C H 0.252300 0.221985 0.038320 0.029 Uiso 1 1 calc R U . . . C1 C 0.0882(2) 0.29585(14) 0.34924(13) 0.0159(4) Uani 1 1 d . . . . . C10 C 0.0587(3) 0.45041(16) 0.11753(14) 0.0160(5) Uani 1 1 d . . . . . C7 C 0.2798(3) 0.40427(14) 0.08791(14) 0.0152(4) Uani 1 1 d . . . . . C19 C 0.3836(2) 0.46362(15) 0.39143(13) 0.0143(4) Uani 1 1 d . . . . . C14 C -0.0650(3) 0.29896(16) 0.13385(14) 0.0187(4) Uani 1 1 d . . . . . H14A H -0.080578 0.302624 0.191604 0.028 Uiso 1 1 calc R U . . . H14B H -0.043192 0.238169 0.120585 0.028 Uiso 1 1 calc R U . . . H14C H -0.152491 0.318306 0.097869 0.028 Uiso 1 1 calc R U . . . C3 C -0.0618(3) 0.35689(16) 0.42731(14) 0.0188(5) Uani 1 1 d . . . . . H3 H -0.124677 0.365613 0.467172 0.023 Uiso 1 1 calc R U . . . C12 C 0.4199(3) 0.40180(16) 0.05346(15) 0.0205(5) Uani 1 1 d . . . . . H12A H 0.478214 0.352162 0.077414 0.031 Uiso 1 1 calc R U . . . H12B H 0.472979 0.456564 0.067089 0.031 Uiso 1 1 calc R U . . . H12C H 0.399848 0.395040 -0.006645 0.031 Uiso 1 1 calc R U . . . C18 C 0.4678(2) 0.39338(16) 0.36781(14) 0.0146(4) Uani 1 1 d . . . . . C15 C -0.0661(3) 0.50932(17) 0.12897(16) 0.0234(5) Uani 1 1 d . . . . . H15A H -0.030037 0.560339 0.162200 0.035 Uiso 1 1 calc R U . . . H15B H -0.135008 0.476939 0.157232 0.035 Uiso 1 1 calc R U . . . H15C H -0.114577 0.529043 0.074931 0.035 Uiso 1 1 calc R U . . . C21 C 0.4847(2) 0.50733(15) 0.27852(13) 0.0151(4) Uani 1 1 d . . . . . C25 C 0.3262(3) 0.62394(15) 0.34008(16) 0.0224(5) Uani 1 1 d . . . . . H25A H 0.249152 0.621500 0.374638 0.034 Uiso 1 1 calc R U . . . H25B H 0.285571 0.643112 0.284346 0.034 Uiso 1 1 calc R U . . . H25C H 0.400741 0.665564 0.363971 0.034 Uiso 1 1 calc R U . . . C22 C 0.6327(3) 0.36582(17) 0.25599(15) 0.0204(5) Uani 1 1 d . . . . . H22A H 0.655721 0.397090 0.207313 0.031 Uiso 1 1 calc R U . . . H22B H 0.587451 0.309410 0.239023 0.031 Uiso 1 1 calc R U . . . H22C H 0.721765 0.355643 0.294547 0.031 Uiso 1 1 calc R U . . . C24 C 0.3088(3) 0.46490(16) 0.46696(13) 0.0190(4) Uani 1 1 d . . . . . H24A H 0.246749 0.413059 0.466817 0.028 Uiso 1 1 calc R U . . . H24B H 0.249661 0.518031 0.466488 0.028 Uiso 1 1 calc R U . . . H24C H 0.381515 0.464431 0.516656 0.028 Uiso 1 1 calc R U . . . C16 C 0.2250(3) 0.57347(16) 0.07672(15) 0.0220(5) Uani 1 1 d . . . . . H16A H 0.322759 0.577089 0.062038 0.033 Uiso 1 1 calc R U . . . H16B H 0.218741 0.610726 0.124819 0.033 Uiso 1 1 calc R U . . . H16C H 0.154623 0.593483 0.030088 0.033 Uiso 1 1 calc R U . . . C26 C 0.5443(3) 0.56841(17) 0.21929(15) 0.0224(5) Uani 1 1 d . . . . . H26A H 0.472440 0.613732 0.200716 0.034 Uiso 1 1 calc R U . . . H26B H 0.566293 0.535015 0.171545 0.034 Uiso 1 1 calc R U . . . H26C H 0.632922 0.596146 0.247136 0.034 Uiso 1 1 calc R U . . . C2 C 0.0113(3) 0.27829(16) 0.41314(14) 0.0196(5) Uani 1 1 d . . . . . H2 H 0.008163 0.224322 0.441824 0.023 Uiso 1 1 calc R U . . . C23 C 0.5023(3) 0.31013(16) 0.41610(15) 0.0218(5) Uani 1 1 d . . . . . H23A H 0.534456 0.265210 0.380054 0.033 Uiso 1 1 calc R U . . . H23B H 0.415559 0.289507 0.437355 0.033 Uiso 1 1 calc R U . . . H23C H 0.579332 0.321464 0.462346 0.033 Uiso 1 1 calc R U . . . C5 C 0.1803(3) 0.23374(15) 0.30852(15) 0.0188(4) Uani 1 1 d . . . . . H5A H 0.270631 0.262986 0.300645 0.028 Uiso 1 1 calc R U . . . H5B H 0.128020 0.215778 0.254806 0.028 Uiso 1 1 calc R U . . . H5C H 0.202288 0.181902 0.343506 0.028 Uiso 1 1 calc R U . . . C11 C 0.1923(3) 0.47938(15) 0.09715(13) 0.0156(4) Uani 1 1 d . . . . . C6 C -0.0703(3) 0.51269(16) 0.36277(15) 0.0215(5) Uani 1 1 d . . . . . H6A H -0.171163 0.515793 0.335952 0.032 Uiso 1 1 calc R U . . . H6B H -0.008266 0.543578 0.328928 0.032 Uiso 1 1 calc R U . . . H6C H -0.061551 0.540255 0.417331 0.032 Uiso 1 1 calc R U . . . 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 0.00960(11) 0.01206(11) 0.01008(10) -0.00042(4) 0.00225(7) -0.00177(4) N1 0.0116(8) 0.0150(9) 0.0128(8) -0.0007(7) 0.0032(7) -0.0007(7) C8 0.0156(10) 0.0158(10) 0.0099(9) -0.0019(7) 0.0017(8) -0.0013(8) C9 0.0123(10) 0.0171(11) 0.0107(9) -0.0022(8) -0.0003(8) -0.0013(8) C17 0.0094(10) 0.0192(11) 0.0165(11) -0.0008(8) 0.0011(8) -0.0029(8) C4 0.0111(10) 0.0203(11) 0.0135(10) -0.0032(8) 0.0030(8) -0.0017(8) C20 0.0124(10) 0.0139(10) 0.0178(10) -0.0017(8) -0.0002(8) -0.0026(8) C13 0.0224(12) 0.0172(11) 0.0198(11) -0.0029(8) 0.0062(9) 0.0009(9) C1 0.0151(10) 0.0151(10) 0.0172(10) -0.0012(8) 0.0014(8) -0.0020(8) C10 0.0167(11) 0.0183(12) 0.0121(10) 0.0008(8) -0.0005(8) 0.0028(9) C7 0.0162(11) 0.0191(11) 0.0106(10) -0.0003(7) 0.0031(8) -0.0016(8) C19 0.0113(10) 0.0186(10) 0.0126(10) -0.0033(8) 0.0011(8) -0.0033(9) C14 0.0148(11) 0.0227(11) 0.0185(11) -0.0028(9) 0.0023(8) -0.0041(9) C3 0.0156(10) 0.0277(12) 0.0149(10) -0.0009(9) 0.0078(8) -0.0029(9) C12 0.0189(12) 0.0262(12) 0.0175(11) -0.0015(9) 0.0066(9) -0.0031(9) C18 0.0130(11) 0.0157(10) 0.0147(10) 0.0004(8) 0.0008(8) -0.0005(9) C15 0.0198(12) 0.0258(12) 0.0236(12) -0.0012(9) -0.0004(9) 0.0080(10) C21 0.0119(10) 0.0176(10) 0.0155(10) 0.0011(8) 0.0015(8) -0.0044(8) C25 0.0244(12) 0.0143(11) 0.0279(12) -0.0041(9) 0.0023(10) 0.0011(9) C22 0.0129(10) 0.0261(12) 0.0230(11) -0.0047(9) 0.0051(9) 0.0012(9) C24 0.0186(11) 0.0254(11) 0.0141(10) -0.0051(9) 0.0065(8) -0.0049(9) C16 0.0302(13) 0.0161(10) 0.0195(11) 0.0044(9) 0.0031(10) -0.0007(10) C26 0.0201(12) 0.0239(11) 0.0232(12) 0.0042(10) 0.0036(9) -0.0090(10) C2 0.0222(12) 0.0198(11) 0.0170(10) 0.0025(8) 0.0038(9) -0.0049(9) C23 0.0246(12) 0.0190(11) 0.0206(11) 0.0064(9) -0.0004(9) 0.0015(9) C5 0.0193(11) 0.0155(10) 0.0219(11) -0.0006(8) 0.0043(9) -0.0017(8) C11 0.0178(11) 0.0172(11) 0.0114(10) 0.0005(8) 0.0007(8) -0.0002(8) C6 0.0213(11) 0.0238(12) 0.0203(11) -0.0029(9) 0.0060(9) 0.0049(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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 0 -1 1 0.0647 0 1 -1 0.0729 0 1 1 0.1473 0 -1 0 0.0694 0 0 1 0.1005 -1 -2 2 0.0566 1 2 -2 0.1059 2 1 2 0.1145 1 0 2 0.1038 -2 -1 -2 0.0511 -2 -2 1 0.0488 2 2 -1 0.1144 2 1 1 0.1118 -1 -2 1 0.0462 0 -2 1 0.0514 1 -1 -1 0.0821 1 -2 1 0.0646 1 -2 -2 0.0861 1 -2 -1 0.0719 0 -1 2 0.0752 2 -2 1 0.0686 2 -1 -2 0.0872 -1 -1 2 0.0755 -2 1 -2 0.0879 2 1 -2 0.0975 1 0 0 0.0906 2 -1 2 0.0824 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 C8 109.79(6) . . ? N1 Dy1 C9 84.50(6) . . ? N1 Dy1 C17 128.17(7) . . ? N1 Dy1 C20 101.37(6) . . ? N1 Dy1 C1 26.47(6) . . ? N1 Dy1 C10 91.07(7) . . ? N1 Dy1 C7 136.11(7) . . ? N1 Dy1 C19 82.14(7) . . ? N1 Dy1 C18 97.06(7) . . ? N1 Dy1 C21 131.82(6) . . ? N1 Dy1 C11 121.46(7) . . ? C8 Dy1 C9 31.23(7) . . ? C8 Dy1 C17 110.05(7) . . ? C8 Dy1 C1 100.18(6) . . ? C8 Dy1 C7 31.22(7) . . ? C8 Dy1 C18 129.13(7) . . ? C8 Dy1 C11 51.61(7) . . ? C9 Dy1 C17 141.18(7) . . ? C9 Dy1 C1 85.56(6) . . ? C9 Dy1 C7 51.63(7) . . ? C9 Dy1 C18 154.83(7) . . ? C9 Dy1 C11 51.60(7) . . ? C17 Dy1 C1 114.18(7) . . ? C17 Dy1 C7 93.59(7) . . ? C17 Dy1 C18 31.17(7) . . ? C20 Dy1 C8 147.79(7) . . ? C20 Dy1 C9 152.74(7) . . ? C20 Dy1 C17 51.91(7) . . ? C20 Dy1 C1 111.52(6) . . ? C20 Dy1 C10 121.39(7) . . ? C20 Dy1 C7 116.99(7) . . ? C20 Dy1 C19 31.32(7) . . ? C20 Dy1 C18 51.66(7) . . ? C20 Dy1 C21 31.52(6) . . ? C20 Dy1 C11 104.75(7) . . ? C10 Dy1 C8 51.73(7) . . ? C10 Dy1 C9 31.37(7) . . ? C10 Dy1 C17 140.13(7) . . ? C10 Dy1 C1 104.57(7) . . ? C10 Dy1 C7 51.65(7) . . ? C10 Dy1 C19 146.64(8) . . ? C10 Dy1 C18 170.23(8) . . ? C10 Dy1 C21 118.85(7) . . ? C10 Dy1 C11 31.11(7) . . ? C7 Dy1 C1 131.37(6) . . ? C19 Dy1 C8 160.01(7) . . ? C19 Dy1 C9 166.48(7) . . ? C19 Dy1 C17 51.66(7) . . ? C19 Dy1 C1 83.41(6) . . ? C19 Dy1 C7 141.60(7) . . ? C19 Dy1 C18 31.09(7) . . ? C19 Dy1 C11 136.06(7) . . ? C18 Dy1 C1 85.04(7) . . ? C18 Dy1 C7 122.87(7) . . ? C21 Dy1 C8 118.38(6) . . ? C21 Dy1 C9 140.42(6) . . ? C21 Dy1 C17 31.14(7) . . ? C21 Dy1 C1 133.76(6) . . ? C21 Dy1 C7 90.37(7) . . ? C21 Dy1 C19 51.69(6) . . ? C21 Dy1 C18 51.44(7) . . ? C21 Dy1 C11 90.72(7) . . ? C11 Dy1 C17 109.04(7) . . ? C11 Dy1 C1 134.89(7) . . ? C11 Dy1 C7 31.24(7) . . ? C11 Dy1 C18 139.67(7) . . ? C4 N1 Dy1 143.96(15) . . ? C4 N1 C1 106.37(17) . . ? C1 N1 Dy1 105.74(13) . . ? C9 C8 Dy1 74.39(12) . . ? C9 C8 C13 127.3(2) . . ? C9 C8 C7 108.37(19) . . ? C13 C8 Dy1 120.35(15) . . ? C7 C8 Dy1 75.33(12) . . ? C7 C8 C13 124.1(2) . . ? C8 C9 Dy1 74.38(13) . . ? C8 C9 C10 107.64(18) . . ? C8 C9 C14 126.3(2) . . ? C10 C9 Dy1 73.58(12) . . ? C10 C9 C14 126.0(2) . . ? C14 C9 Dy1 120.94(14) . . ? C18 C17 Dy1 74.70(13) . . ? C18 C17 C22 124.9(2) . . ? C21 C17 Dy1 74.14(13) . . ? C21 C17 C18 107.80(19) . . ? C21 C17 C22 127.2(2) . . ? C22 C17 Dy1 120.14(15) . . ? N1 C4 C3 109.8(2) . . ? N1 C4 C6 121.71(19) . . ? C3 C4 C6 128.5(2) . . ? C19 C20 Dy1 75.14(12) . . ? C19 C20 C21 107.75(19) . . ? C19 C20 C25 126.5(2) . . ? C21 C20 Dy1 74.87(12) . . ? C21 C20 C25 125.6(2) . . ? C25 C20 Dy1 119.48(16) . . ? 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 . . ? N1 C1 Dy1 47.79(10) . . ? N1 C1 C5 121.76(18) . . ? C2 C1 Dy1 154.32(16) . . ? C2 C1 N1 110.50(19) . . ? C2 C1 C5 127.7(2) . . ? C5 C1 Dy1 75.81(12) . . ? C9 C10 Dy1 75.06(12) . . ? C9 C10 C15 126.6(2) . . ? C15 C10 Dy1 118.57(15) . . ? C11 C10 Dy1 75.19(13) . . ? C11 C10 C9 108.40(19) . . ? C11 C10 C15 124.9(2) . . ? C8 C7 Dy1 73.45(12) . . ? C8 C7 C12 124.8(2) . . ? C8 C7 C11 107.2(2) . . ? C12 C7 Dy1 126.63(17) . . ? C11 C7 Dy1 73.45(12) . . ? C11 C7 C12 127.2(2) . . ? C20 C19 Dy1 73.54(12) . . ? C20 C19 C24 126.5(2) . . ? C18 C19 Dy1 74.86(13) . . ? C18 C19 C20 108.03(19) . . ? C18 C19 C24 125.3(2) . . ? C24 C19 Dy1 121.55(15) . . ? 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 . . ? C4 C3 H3 126.4 . . ? C4 C3 C2 107.13(18) . . ? C2 C3 H3 126.4 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C17 C18 Dy1 74.12(13) . . ? C17 C18 C23 125.9(2) . . ? C19 C18 Dy1 74.05(13) . . ? C19 C18 C17 108.3(2) . . ? C19 C18 C23 125.3(2) . . ? C23 C18 Dy1 124.36(16) . . ? 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 . . ? C17 C21 Dy1 74.72(13) . . ? C17 C21 C20 108.14(18) . . ? C17 C21 C26 126.6(2) . . ? C20 C21 Dy1 73.61(12) . . ? C20 C21 C26 124.3(2) . . ? C26 C21 Dy1 126.36(15) . . ? 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 . . ? 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 . . ? 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 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C1 C2 C3 106.2(2) . . ? C1 C2 H2 126.9 . . ? C3 C2 H2 126.9 . . ? 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 . . ? Dy1 C5 H5A 46.6 . . ? Dy1 C5 H5B 93.0 . . ? Dy1 C5 H5C 153.0 . . ? C1 C5 Dy1 75.15(12) . . ? C1 C5 H5A 109.5 . . ? C1 C5 H5B 109.5 . . ? C1 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C10 C11 Dy1 73.69(13) . . ? C10 C11 C7 108.4(2) . . ? C10 C11 C16 124.3(2) . . ? C7 C11 Dy1 75.32(13) . . ? C7 C11 C16 126.8(2) . . ? C16 C11 Dy1 123.84(15) . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? 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 N1 2.2988(17) . ? Dy1 C8 2.639(2) . ? Dy1 C9 2.639(2) . ? Dy1 C17 2.640(2) . ? Dy1 C20 2.616(2) . ? Dy1 C1 2.987(2) . ? Dy1 C10 2.620(2) . ? Dy1 C7 2.663(2) . ? Dy1 C19 2.637(2) . ? Dy1 C18 2.647(2) . ? Dy1 C21 2.632(2) . ? Dy1 C11 2.639(2) . ? N1 C4 1.375(3) . ? N1 C1 1.383(3) . ? C8 C9 1.421(3) . ? C8 C13 1.510(3) . ? C8 C7 1.427(3) . ? C9 C10 1.422(3) . ? C9 C14 1.511(3) . ? C17 C18 1.421(3) . ? C17 C21 1.415(3) . ? C17 C22 1.507(3) . ? C4 C3 1.386(3) . ? C4 C6 1.496(3) . ? C20 C19 1.418(3) . ? C20 C21 1.426(3) . ? C20 C25 1.509(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C1 C2 1.381(3) . ? C1 C5 1.500(3) . ? C10 C15 1.505(3) . ? C10 C11 1.411(3) . ? C7 C12 1.500(3) . ? C7 C11 1.428(3) . ? C19 C18 1.416(3) . ? C19 C24 1.508(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C3 H3 0.9500 . ? C3 C2 1.415(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C18 C23 1.505(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C21 C26 1.509(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16 C11 1.514(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C2 H2 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 C4 C3 -152.9(2) . . . . ? Dy1 N1 C4 C6 26.7(4) . . . . ? Dy1 N1 C1 C2 163.71(16) . . . . ? Dy1 N1 C1 C5 -18.0(2) . . . . ? Dy1 C8 C9 C10 66.61(14) . . . . ? Dy1 C8 C9 C14 -117.2(2) . . . . ? Dy1 C8 C7 C12 123.5(2) . . . . ? Dy1 C8 C7 C11 -66.22(16) . . . . ? Dy1 C9 C10 C15 -114.7(2) . . . . ? Dy1 C9 C10 C11 68.44(16) . . . . ? Dy1 C17 C18 C19 -66.75(16) . . . . ? Dy1 C17 C18 C23 121.2(2) . . . . ? Dy1 C17 C21 C20 66.59(15) . . . . ? Dy1 C17 C21 C26 -124.2(2) . . . . ? Dy1 C20 C19 C18 67.50(16) . . . . ? Dy1 C20 C19 C24 -117.4(2) . . . . ? Dy1 C20 C21 C17 -67.33(16) . . . . ? Dy1 C20 C21 C26 123.2(2) . . . . ? Dy1 C1 C2 C3 28.9(5) . . . . ? Dy1 C10 C11 C7 67.95(16) . . . . ? Dy1 C10 C11 C16 -120.2(2) . . . . ? Dy1 C7 C11 C10 -66.87(16) . . . . ? Dy1 C7 C11 C16 121.5(2) . . . . ? Dy1 C19 C18 C17 66.80(16) . . . . ? Dy1 C19 C18 C23 -121.1(2) . . . . ? N1 C4 C3 C2 0.9(3) . . . . ? N1 C1 C2 C3 0.3(3) . . . . ? N1 C1 C5 Dy1 13.67(19) . . . . ? C8 C9 C10 Dy1 -67.15(15) . . . . ? C8 C9 C10 C15 178.1(2) . . . . ? C8 C9 C10 C11 1.3(2) . . . . ? C8 C7 C11 Dy1 66.22(16) . . . . ? C8 C7 C11 C10 -0.6(3) . . . . ? C8 C7 C11 C16 -172.3(2) . . . . ? C9 C8 C7 Dy1 67.67(15) . . . . ? C9 C8 C7 C12 -168.9(2) . . . . ? C9 C8 C7 C11 1.4(3) . . . . ? C9 C10 C11 Dy1 -68.35(14) . . . . ? C9 C10 C11 C7 -0.4(2) . . . . ? C9 C10 C11 C16 171.5(2) . . . . ? C4 N1 C1 Dy1 -163.4(2) . . . . ? C4 N1 C1 C2 0.3(3) . . . . ? C4 N1 C1 C5 178.6(2) . . . . ? C4 C3 C2 C1 -0.7(3) . . . . ? C20 C19 C18 Dy1 -66.62(16) . . . . ? C20 C19 C18 C17 0.2(3) . . . . ? C20 C19 C18 C23 172.3(2) . . . . ? C13 C8 C9 Dy1 116.5(2) . . . . ? C13 C8 C9 C10 -176.9(2) . . . . ? C13 C8 C9 C14 -0.7(4) . . . . ? C13 C8 C7 Dy1 -117.0(2) . . . . ? C13 C8 C7 C12 6.5(4) . . . . ? C13 C8 C7 C11 176.8(2) . . . . ? C1 N1 C4 C3 -0.8(3) . . . . ? C1 N1 C4 C6 178.9(2) . . . . ? C7 C8 C9 Dy1 -68.30(16) . . . . ? C7 C8 C9 C10 -1.7(2) . . . . ? C7 C8 C9 C14 174.5(2) . . . . ? C19 C20 C21 Dy1 68.56(15) . . . . ? C19 C20 C21 C17 1.2(3) . . . . ? C19 C20 C21 C26 -168.2(2) . . . . ? C14 C9 C10 Dy1 116.6(2) . . . . ? C14 C9 C10 C15 1.9(3) . . . . ? C14 C9 C10 C11 -174.9(2) . . . . ? C12 C7 C11 Dy1 -123.8(2) . . . . ? C12 C7 C11 C10 169.4(2) . . . . ? C12 C7 C11 C16 -2.3(4) . . . . ? C18 C17 C21 Dy1 -67.71(16) . . . . ? C18 C17 C21 C20 -1.1(3) . . . . ? C18 C17 C21 C26 168.1(2) . . . . ? C15 C10 C11 Dy1 114.8(2) . . . . ? C15 C10 C11 C7 -177.3(2) . . . . ? C15 C10 C11 C16 -5.4(4) . . . . ? C21 C17 C18 Dy1 67.34(16) . . . . ? C21 C17 C18 C19 0.6(3) . . . . ? C21 C17 C18 C23 -171.4(2) . . . . ? C21 C20 C19 Dy1 -68.37(15) . . . . ? C21 C20 C19 C18 -0.9(3) . . . . ? C21 C20 C19 C24 174.2(2) . . . . ? C25 C20 C19 Dy1 115.9(2) . . . . ? C25 C20 C19 C18 -176.6(2) . . . . ? C25 C20 C19 C24 -1.5(4) . . . . ? C25 C20 C21 Dy1 -115.7(2) . . . . ? C25 C20 C21 C17 177.0(2) . . . . ? C25 C20 C21 C26 7.5(4) . . . . ? C22 C17 C18 Dy1 -116.4(2) . . . . ? C22 C17 C18 C19 176.9(2) . . . . ? C22 C17 C18 C23 4.9(4) . . . . ? C22 C17 C21 Dy1 116.1(2) . . . . ? C22 C17 C21 C20 -177.3(2) . . . . ? C22 C17 C21 C26 -8.1(4) . . . . ? C24 C19 C18 Dy1 118.2(2) . . . . ? C24 C19 C18 C17 -175.0(2) . . . . ? C24 C19 C18 C23 -2.9(4) . . . . ? C2 C1 C5 Dy1 -168.4(3) . . . . ? C5 C1 C2 C3 -177.9(2) . . . . ? C6 C4 C3 C2 -178.7(2) . . . . ?