# Electronic Supplementary Material (ESI) for Chemical Communications. # This journal is © The Royal Society of Chemistry 2023 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_dy60_hp0 _database_code_depnum_ccdc_archive 'CCDC 2046705' loop_ _audit_author_name _audit_author_address 'Andreas M. Thiel' ;Aarhus University, Department of Chemistry Denmark ; _audit_update_record ; 2022-10-30 deposited with the CCDC. 2023-02-13 downloaded from the CCDC. ; _audit_creation_date 2020-02-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C34 H58 Dy, B C24 F20' _chemical_formula_sum 'C58 H58 B Dy F20' _chemical_formula_weight 1308.35 _chemical_melting_point ? _chemical_oxdiff_formula C58H58BDyF20 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6278(3) _cell_length_b 12.6173(5) _cell_length_c 20.3029(7) _cell_angle_alpha 107.031(3) _cell_angle_beta 96.387(3) _cell_angle_gamma 99.377(3) _cell_volume 2769.81(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8547 _cell_measurement_temperature 100 _cell_measurement_theta_max 27.2720 _cell_measurement_theta_min 1.7250 _shelx_estimated_absorpt_T_max 0.931 _shelx_estimated_absorpt_T_min 0.731 _exptl_absorpt_coefficient_mu 1.454 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.75583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier ? _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description irregular _exptl_crystal_F_000 1314 _exptl_crystal_preparation ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_ambient_pressure 0 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_unetI/netI 0.0616 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 27269 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.349 _diffrn_reflns_theta_min 1.716 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3590 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 44.00 69.00 1.00 30.00 -- 22.61-157.00-132.00 25 2 \w 21.00 46.00 1.00 30.00 -- 22.61-119.00 23.00 25 3 \w 56.00 109.00 1.00 30.00 -- 22.61 157.00 -96.00 53 4 \w -94.00 -60.00 1.00 30.00 -- -23.39-157.00-132.00 34 5 \w -93.00 -68.00 1.00 30.00 -- -23.39 157.00 -96.00 25 6 \w -57.00 -30.00 1.00 30.00 -- -23.39 119.00 108.00 27 7 \w 88.00 128.00 1.00 30.00 -- 22.61 77.00-120.00 40 8 \w 82.00 128.00 1.00 30.00 -- 22.61 77.00-150.00 46 9 \w -26.00 41.00 1.00 30.00 -- 22.61 77.00 60.00 67 10 \w 82.00 128.00 1.00 30.00 -- 22.61 77.00 90.00 46 11 \w -25.00 42.00 1.00 30.00 -- 22.61 77.00 -60.00 67 12 \w -131.00 -93.00 1.00 30.00 -- -23.39 -77.00-120.00 38 13 \w -128.00 -82.00 1.00 30.00 -- -23.39 -77.00 30.00 46 14 \w 8.00 33.00 1.00 30.00 -- -23.39 -99.00 120.00 25 15 \w -131.00-102.00 1.00 30.00 -- -23.39 -77.00 60.00 29 16 \w -12.00 29.00 1.00 30.00 -- -23.39 -99.00 30.00 41 17 \w -130.00 -82.00 1.00 30.00 -- -23.39 -77.00 90.00 48 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0514630000 _diffrn_orient_matrix_UB_12 0.0428399000 _diffrn_orient_matrix_UB_13 0.0157040000 _diffrn_orient_matrix_UB_21 -0.0075283000 _diffrn_orient_matrix_UB_22 -0.0049516000 _diffrn_orient_matrix_UB_23 0.0332411000 _diffrn_orient_matrix_UB_31 0.0350585000 _diffrn_orient_matrix_UB_32 -0.0418317000 _diffrn_orient_matrix_UB_33 -0.0047393000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8367 _reflns_number_total 10122 _reflns_odcompleteness_completeness 99.96 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.228 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.097 _refine_ls_extinction_coef . _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 739 _refine_ls_number_reflns 10122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0402 _refine_ls_restrained_S_all 1.045 _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^)+(0.0347P)^2^+2.6137P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.0944 _refine_special_details ? _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), C5(H5), C20(H20), C22(H22) 2.b Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B, H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A, H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.67750(2) 0.84875(2) 0.72177(2) 0.02602(7) Uani 1 1 d . . . . . C1 C 0.5563(3) 1.0011(4) 0.7219(2) 0.0244(9) Uani 1 1 d . . . . . C2 C 0.4968(3) 0.9331(3) 0.7592(2) 0.0235(9) Uani 1 1 d . . . . . C3 C 0.4456(3) 0.8274(4) 0.7085(2) 0.0289(10) Uani 1 1 d . . . . . H3 H 0.401745 0.766760 0.718048 0.035 Uiso 1 1 calc R . . . . C4 C 0.4693(3) 0.8254(4) 0.6416(2) 0.0354(12) Uani 1 1 d . . . . . C5 C 0.5382(3) 0.9315(4) 0.6506(2) 0.0342(11) Uani 1 1 d . . . . . H5 H 0.568267 0.953881 0.615019 0.041 Uiso 1 1 calc R . . . . C6 C 0.6457(4) 1.1166(4) 0.7482(3) 0.0381(12) Uani 1 1 d . . . . . C7 C 0.7647(4) 1.0951(4) 0.7795(3) 0.0431(13) Uani 1 1 d . . . . . H7A H 0.792810 1.041836 0.743842 0.065 Uiso 1 1 calc GR . . . . H7B H 0.752688 1.065104 0.817072 0.065 Uiso 1 1 calc GR . . . . H7C H 0.821945 1.165118 0.796787 0.065 Uiso 1 1 calc GR . . . . C8 C 0.6060(4) 1.2112(4) 0.8008(3) 0.0465(14) Uani 1 1 d . . . . . H8A H 0.530596 1.220577 0.781376 0.070 Uiso 1 1 calc GR . . . . H8B H 0.663032 1.280615 0.811424 0.070 Uiso 1 1 calc GR . . . . H8C H 0.599200 1.192114 0.842852 0.070 Uiso 1 1 calc GR . . . . C9 C 0.6715(4) 1.1598(5) 0.6873(3) 0.0634(18) Uani 1 1 d . . . . . H9A H 0.700964 1.104195 0.653788 0.095 Uiso 1 1 calc GR . . . . H9B H 0.729730 1.229190 0.704412 0.095 Uiso 1 1 calc GR . . . . H9C H 0.600166 1.173068 0.665353 0.095 Uiso 1 1 calc GR . . . . C10 C 0.4693(4) 0.9607(3) 0.8345(2) 0.0268(9) Uani 1 1 d . . . . . C11 C 0.5787(4) 1.0088(4) 0.8917(2) 0.0359(11) Uani 1 1 d . . . . . H11A H 0.629637 0.955282 0.886541 0.054 Uiso 1 1 calc GR . . . . H11B H 0.554776 1.023079 0.936742 0.054 Uiso 1 1 calc GR . . . . H11C H 0.620247 1.078358 0.887743 0.054 Uiso 1 1 calc GR . . . . C12 C 0.4055(4) 0.8528(4) 0.8459(3) 0.0397(12) Uani 1 1 d . . . . . H12A H 0.330328 0.825304 0.815484 0.059 Uiso 1 1 calc GR . . . . H12B H 0.393597 0.869439 0.893625 0.059 Uiso 1 1 calc GR . . . . H12C H 0.452638 0.796084 0.835763 0.059 Uiso 1 1 calc GR . . . . C13 C 0.3813(4) 1.0410(4) 0.8427(2) 0.0316(10) Uani 1 1 d . . . . . H13A H 0.418145 1.111658 0.837995 0.047 Uiso 1 1 calc GR . . . . H13B H 0.358426 1.054262 0.887935 0.047 Uiso 1 1 calc GR . . . . H13C H 0.312522 1.007109 0.807178 0.047 Uiso 1 1 calc GR . . . . C14 C 0.4067(4) 0.7361(5) 0.5733(3) 0.064(2) Uani 1 1 d . . . . . C15 C 0.4323(7) 0.6217(7) 0.5699(5) 0.154(5) Uani 1 1 d . . . . . H15A H 0.516285 0.627110 0.578270 0.230 Uiso 1 1 calc GR . . . . H15B H 0.399267 0.568653 0.524515 0.230 Uiso 1 1 calc GR . . . . H15C H 0.397684 0.596334 0.604848 0.230 Uiso 1 1 calc GR . . . . C16 C 0.4420(5) 0.7698(9) 0.5113(3) 0.139(5) Uani 1 1 d . . . . . H16A H 0.417477 0.838983 0.511692 0.208 Uiso 1 1 calc GR . . . . H16B H 0.404509 0.710986 0.468752 0.208 Uiso 1 1 calc GR . . . . H16C H 0.526288 0.780596 0.514217 0.208 Uiso 1 1 calc GR . . . . C17 C 0.2744(4) 0.7325(5) 0.5689(3) 0.0536(16) Uani 1 1 d . . . . . H17A H 0.247847 0.713139 0.607777 0.080 Uiso 1 1 calc GR . . . . H17B H 0.232950 0.676665 0.526054 0.080 Uiso 1 1 calc GR . . . . H17C H 0.258980 0.805430 0.569990 0.080 Uiso 1 1 calc GR . . . . C18 C 0.7979(3) 0.6961(4) 0.7204(2) 0.0258(9) Uani 1 1 d . . . . . C19 C 0.8804(3) 0.8023(3) 0.7531(2) 0.0233(9) Uani 1 1 d . . . . . C20 C 0.8978(3) 0.8518(4) 0.6998(2) 0.0325(11) Uani 1 1 d . . . . . H20 H 0.947045 0.921460 0.706761 0.039 Uiso 1 1 calc R . . . . C21 C 0.8319(4) 0.7833(5) 0.6358(2) 0.0403(13) Uani 1 1 d . . . . . C22 C 0.7690(4) 0.6872(4) 0.6483(2) 0.0368(11) Uani 1 1 d . . . . . H22 H 0.716619 0.627213 0.614648 0.044 Uiso 1 1 calc R . . . . C23 C 0.7263(4) 0.6120(4) 0.7497(3) 0.0365(11) Uani 1 1 d . . . . . C24 C 0.6265(4) 0.6652(4) 0.7806(3) 0.0370(11) Uani 1 1 d . . . . . H24A H 0.574045 0.675691 0.744084 0.055 Uiso 1 1 calc GR . . . . H24B H 0.659771 0.737204 0.815325 0.055 Uiso 1 1 calc GR . . . . H24C H 0.583366 0.616030 0.801640 0.055 Uiso 1 1 calc GR . . . . C25 C 0.7996(4) 0.5762(4) 0.8047(3) 0.0426(13) Uani 1 1 d . . . . . H25A H 0.864143 0.546947 0.785605 0.064 Uiso 1 1 calc GR . . . . H25B H 0.750162 0.518764 0.817032 0.064 Uiso 1 1 calc GR . . . . H25C H 0.829942 0.640739 0.845561 0.064 Uiso 1 1 calc GR . . . . C26 C 0.6664(4) 0.5014(4) 0.6919(3) 0.0560(16) Uani 1 1 d . . . . . H26A H 0.613127 0.517391 0.658107 0.084 Uiso 1 1 calc GR . . . . H26B H 0.623023 0.450723 0.711942 0.084 Uiso 1 1 calc GR . . . . H26C H 0.725454 0.466772 0.669418 0.084 Uiso 1 1 calc GR . . . . C27 C 0.9534(3) 0.8570(3) 0.8276(2) 0.0260(9) Uani 1 1 d . . . . . C28 C 0.8766(4) 0.8750(4) 0.8851(2) 0.0338(11) Uani 1 1 d . . . . . H28A H 0.822232 0.921348 0.877031 0.051 Uiso 1 1 calc GR . . . . H28B H 0.926264 0.912004 0.929812 0.051 Uiso 1 1 calc GR . . . . H28C H 0.833256 0.803084 0.884545 0.051 Uiso 1 1 calc GR . . . . C29 C 1.0259(4) 0.9754(4) 0.8354(3) 0.0425(13) Uani 1 1 d . . . . . H29A H 1.078622 0.968363 0.801928 0.064 Uiso 1 1 calc GR . . . . H29B H 1.070906 1.008112 0.881761 0.064 Uiso 1 1 calc GR . . . . H29C H 0.973214 1.023223 0.827452 0.064 Uiso 1 1 calc GR . . . . C30 C 1.0443(4) 0.7856(4) 0.8389(2) 0.0296(10) Uani 1 1 d . . . . . H30A H 1.003823 0.711263 0.835910 0.044 Uiso 1 1 calc GR . . . . H30B H 1.092362 0.821170 0.884181 0.044 Uiso 1 1 calc GR . . . . H30C H 1.093595 0.779746 0.803586 0.044 Uiso 1 1 calc GR . . . . C31 C 0.8485(4) 0.7960(6) 0.5644(3) 0.064(2) Uani 1 1 d . . . . . C32 C 0.8192(7) 0.9048(8) 0.5586(4) 0.117(4) Uani 1 1 d . . . . . H32A H 0.738683 0.906077 0.564581 0.175 Uiso 1 1 calc GR . . . . H32B H 0.829418 0.910411 0.513330 0.175 Uiso 1 1 calc GR . . . . H32C H 0.870862 0.967618 0.594060 0.175 Uiso 1 1 calc GR . . . . C33 C 0.7717(5) 0.6955(8) 0.5048(3) 0.112(4) Uani 1 1 d . . . . . H33A H 0.800585 0.627884 0.503327 0.168 Uiso 1 1 calc GR . . . . H33B H 0.775059 0.709960 0.461133 0.168 Uiso 1 1 calc GR . . . . H33C H 0.691311 0.685702 0.512742 0.168 Uiso 1 1 calc GR . . . . C34 C 0.9783(4) 0.7942(6) 0.5572(3) 0.0576(17) Uani 1 1 d . . . . . H34A H 1.028518 0.858416 0.592417 0.086 Uiso 1 1 calc GR . . . . H34B H 0.990528 0.797315 0.511798 0.086 Uiso 1 1 calc GR . . . . H34C H 0.996941 0.725778 0.563045 0.086 Uiso 1 1 calc GR . . . . F1 F 0.7780(2) 0.38806(19) 0.23757(13) 0.0326(6) Uani 1 1 d . . . . . F2 F 0.9166(2) 0.3491(2) 0.33606(14) 0.0398(6) Uani 1 1 d . . . . . F3 F 1.1000(2) 0.5136(2) 0.42031(13) 0.0392(6) Uani 1 1 d . . . . . F4 F 1.1478(2) 0.7177(2) 0.39689(13) 0.0390(6) Uani 1 1 d . . . . . F5 F 1.0151(2) 0.75636(19) 0.29375(13) 0.0327(6) Uani 1 1 d . . . . . F6 F 0.8541(2) 0.87045(19) 0.23942(13) 0.0344(6) Uani 1 1 d . . . . . F7 F 0.7702(2) 1.0102(2) 0.33711(14) 0.0420(7) Uani 1 1 d . . . . . F8 F 0.6229(2) 0.9288(2) 0.41558(13) 0.0433(7) Uani 1 1 d . . . . . F9 F 0.5557(2) 0.7000(2) 0.38687(13) 0.0406(7) Uani 1 1 d . . . . . F10 F 0.6374(2) 0.5579(2) 0.28751(13) 0.0342(6) Uani 1 1 d . . . . . F11 F 1.0566(2) 0.5995(2) 0.16837(12) 0.0334(6) Uani 1 1 d . . . . . F12 F 1.1422(2) 0.6620(3) 0.06713(16) 0.0539(8) Uani 1 1 d . . . . . F13 F 1.0162(3) 0.7611(3) -0.01090(16) 0.0582(9) Uani 1 1 d . . . . . F14 F 0.7972(2) 0.7927(2) 0.01422(13) 0.0396(6) Uani 1 1 d . . . . . F15 F 0.7049(2) 0.7245(2) 0.11326(12) 0.0309(6) Uani 1 1 d . . . . . F16 F 0.5340(2) 0.5853(2) 0.16300(13) 0.0332(6) Uani 1 1 d . . . . . F17 F 0.3941(2) 0.4157(2) 0.06235(15) 0.0485(7) Uani 1 1 d . . . . . F18 F 0.4804(2) 0.2359(2) -0.01186(15) 0.0521(8) Uani 1 1 d . . . . . F19 F 0.7143(2) 0.2348(2) 0.01653(13) 0.0383(6) Uani 1 1 d . . . . . F20 F 0.8596(2) 0.40865(19) 0.11488(12) 0.0307(6) Uani 1 1 d . . . . . C35 C 0.8910(3) 0.5734(3) 0.2584(2) 0.0247(9) Uani 1 1 d . . . . . C36 C 0.8712(3) 0.4732(3) 0.2740(2) 0.0253(9) Uani 1 1 d . . . . . C37 C 0.9407(4) 0.4504(4) 0.3260(2) 0.0287(10) Uani 1 1 d . . . . . C38 C 1.0335(4) 0.5327(4) 0.3682(2) 0.0294(10) Uani 1 1 d . . . . . C39 C 1.0567(3) 0.6352(4) 0.3558(2) 0.0278(10) Uani 1 1 d . . . . . C40 C 0.9874(3) 0.6529(3) 0.3027(2) 0.0256(9) Uani 1 1 d . . . . . C41 C 0.7475(3) 0.7056(3) 0.2564(2) 0.0267(9) Uani 1 1 d . . . . . C42 C 0.7781(3) 0.8228(3) 0.2732(2) 0.0252(9) Uani 1 1 d . . . . . C43 C 0.7360(4) 0.8974(4) 0.3246(2) 0.0321(10) Uani 1 1 d . . . . . C44 C 0.6620(4) 0.8578(4) 0.3636(2) 0.0321(11) Uani 1 1 d . . . . . C45 C 0.6286(3) 0.7419(4) 0.3491(2) 0.0301(10) Uani 1 1 d . . . . . C46 C 0.6718(3) 0.6705(4) 0.2972(2) 0.0273(10) Uani 1 1 d . . . . . C47 C 0.8755(4) 0.6610(3) 0.1474(2) 0.0248(9) Uani 1 1 d . . . . . C48 C 0.9861(4) 0.6473(4) 0.1320(2) 0.0305(10) Uani 1 1 d . . . . . C49 C 1.0335(4) 0.6787(4) 0.0795(2) 0.0360(11) Uani 1 1 d . . . . . C50 C 0.9702(4) 0.7277(4) 0.0394(2) 0.0395(12) Uani 1 1 d . . . . . C51 C 0.8598(4) 0.7430(4) 0.0527(2) 0.0323(10) Uani 1 1 d . . . . . C52 C 0.8155(4) 0.7093(3) 0.1044(2) 0.0270(9) Uani 1 1 d . . . . . C53 C 0.7054(3) 0.5052(3) 0.1462(2) 0.0258(9) Uani 1 1 d . . . . . C54 C 0.5862(4) 0.5009(3) 0.1287(2) 0.0297(10) Uani 1 1 d . . . . . C55 C 0.5106(4) 0.4139(4) 0.0762(2) 0.0341(11) Uani 1 1 d . . . . . C56 C 0.5530(4) 0.3238(4) 0.0381(2) 0.0366(11) Uani 1 1 d . . . . . C57 C 0.6710(4) 0.3231(4) 0.0529(2) 0.0314(10) Uani 1 1 d . . . . . C58 C 0.7431(4) 0.4135(4) 0.1046(2) 0.0285(10) Uani 1 1 d . . . . . B1 B 0.8053(4) 0.6115(4) 0.2022(3) 0.0248(10) Uani 1 1 d . . . . . 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 0.01442(11) 0.03693(13) 0.02695(12) 0.01138(9) 0.00358(8) 0.00352(8) C1 0.014(2) 0.034(2) 0.029(2) 0.0160(19) 0.0034(17) 0.0058(17) C2 0.015(2) 0.024(2) 0.029(2) 0.0070(18) 0.0025(17) 0.0026(16) C3 0.011(2) 0.031(2) 0.036(3) -0.0013(19) 0.0046(18) 0.0010(16) C4 0.011(2) 0.056(3) 0.029(3) -0.004(2) 0.0007(18) 0.010(2) C5 0.013(2) 0.073(3) 0.027(3) 0.026(2) 0.0073(18) 0.017(2) C6 0.016(2) 0.040(3) 0.066(3) 0.032(3) -0.002(2) 0.0037(19) C7 0.019(2) 0.029(2) 0.081(4) 0.024(3) -0.006(2) -0.0014(18) C8 0.023(2) 0.024(2) 0.090(4) 0.023(3) -0.006(2) -0.0001(19) C9 0.026(3) 0.083(4) 0.114(5) 0.078(4) 0.017(3) 0.014(3) C10 0.030(2) 0.025(2) 0.027(2) 0.0070(18) 0.0074(18) 0.0109(18) C11 0.038(3) 0.044(3) 0.025(2) 0.005(2) 0.000(2) 0.020(2) C12 0.041(3) 0.037(3) 0.053(3) 0.021(2) 0.030(2) 0.014(2) C13 0.030(2) 0.034(2) 0.030(3) 0.007(2) 0.0038(19) 0.0101(19) C14 0.024(3) 0.098(5) 0.037(3) -0.030(3) -0.009(2) 0.028(3) C15 0.110(6) 0.107(6) 0.146(8) -0.094(6) -0.091(6) 0.075(5) C16 0.032(4) 0.300(13) 0.023(3) -0.025(5) 0.002(3) 0.006(5) C17 0.022(3) 0.070(4) 0.041(3) -0.017(3) -0.005(2) 0.003(2) C18 0.014(2) 0.032(2) 0.031(2) 0.0082(19) 0.0048(17) 0.0048(17) C19 0.016(2) 0.031(2) 0.031(2) 0.0224(19) 0.0052(17) 0.0048(17) C20 0.014(2) 0.048(3) 0.048(3) 0.033(2) 0.0056(19) 0.0078(19) C21 0.020(2) 0.083(4) 0.036(3) 0.034(3) 0.014(2) 0.025(2) C22 0.020(2) 0.057(3) 0.033(3) 0.007(2) 0.0086(19) 0.014(2) C23 0.024(2) 0.027(2) 0.062(3) 0.015(2) 0.017(2) 0.0047(18) C24 0.027(2) 0.032(2) 0.061(3) 0.023(2) 0.022(2) 0.0066(19) C25 0.036(3) 0.034(3) 0.073(4) 0.032(3) 0.026(3) 0.012(2) C26 0.031(3) 0.038(3) 0.086(4) -0.001(3) 0.017(3) 0.003(2) C27 0.021(2) 0.025(2) 0.035(3) 0.0160(19) 0.0019(18) 0.0059(17) C28 0.034(3) 0.038(3) 0.033(3) 0.014(2) 0.002(2) 0.014(2) C29 0.027(2) 0.032(3) 0.068(4) 0.025(2) -0.010(2) -0.002(2) C30 0.024(2) 0.036(2) 0.035(3) 0.017(2) 0.0038(19) 0.0103(19) C31 0.032(3) 0.151(6) 0.043(3) 0.057(4) 0.023(3) 0.052(4) C32 0.115(6) 0.231(10) 0.117(6) 0.148(7) 0.092(5) 0.133(7) C33 0.035(3) 0.271(12) 0.035(4) 0.053(5) 0.009(3) 0.039(5) C34 0.031(3) 0.120(5) 0.050(3) 0.054(4) 0.024(2) 0.036(3) F1 0.0291(13) 0.0240(12) 0.0415(15) 0.0172(11) -0.0079(11) -0.0066(10) F2 0.0399(15) 0.0379(15) 0.0451(17) 0.0256(13) -0.0039(12) 0.0021(12) F3 0.0337(14) 0.0523(17) 0.0304(15) 0.0146(12) -0.0049(11) 0.0096(12) F4 0.0257(13) 0.0422(15) 0.0350(15) 0.0012(12) -0.0040(11) -0.0052(11) F5 0.0248(13) 0.0219(12) 0.0491(16) 0.0115(11) 0.0077(11) -0.0029(10) F6 0.0384(15) 0.0225(12) 0.0462(16) 0.0138(11) 0.0211(12) 0.0026(11) F7 0.0470(16) 0.0269(14) 0.0478(17) 0.0043(12) 0.0117(13) 0.0071(12) F8 0.0346(15) 0.0659(19) 0.0303(15) 0.0101(13) 0.0069(12) 0.0216(13) F9 0.0235(13) 0.0703(19) 0.0345(15) 0.0281(14) 0.0087(11) 0.0039(12) F10 0.0246(13) 0.0340(14) 0.0480(16) 0.0252(12) 0.0031(11) -0.0035(10) F11 0.0260(13) 0.0500(16) 0.0341(15) 0.0220(12) 0.0092(11) 0.0168(12) F12 0.0397(17) 0.083(2) 0.069(2) 0.0491(18) 0.0324(15) 0.0340(16) F13 0.0553(19) 0.094(2) 0.060(2) 0.0556(19) 0.0352(16) 0.0372(18) F14 0.0448(16) 0.0461(16) 0.0426(16) 0.0279(13) 0.0147(13) 0.0193(13) F15 0.0284(13) 0.0351(14) 0.0378(15) 0.0191(11) 0.0107(11) 0.0137(11) F16 0.0268(13) 0.0300(13) 0.0404(15) 0.0092(11) -0.0011(11) 0.0078(10) F17 0.0261(14) 0.0502(17) 0.0565(19) 0.0049(14) -0.0127(13) 0.0084(12) F18 0.0437(17) 0.0408(16) 0.0518(19) -0.0021(14) -0.0170(14) 0.0006(13) F19 0.0422(15) 0.0287(14) 0.0388(16) 0.0061(12) -0.0008(12) 0.0068(12) F20 0.0259(13) 0.0268(13) 0.0381(15) 0.0096(11) -0.0023(11) 0.0083(10) C35 0.019(2) 0.026(2) 0.030(2) 0.0110(18) 0.0053(17) 0.0047(17) C36 0.019(2) 0.025(2) 0.029(2) 0.0091(18) -0.0016(17) 0.0002(17) C37 0.029(2) 0.033(2) 0.029(2) 0.018(2) 0.0047(19) 0.0057(19) C38 0.018(2) 0.045(3) 0.025(2) 0.011(2) 0.0007(18) 0.0075(19) C39 0.019(2) 0.032(2) 0.024(2) 0.0022(19) 0.0016(18) -0.0011(18) C40 0.018(2) 0.020(2) 0.036(3) 0.0053(18) 0.0090(18) 0.0008(16) C41 0.018(2) 0.030(2) 0.035(3) 0.0149(19) 0.0007(18) 0.0036(17) C42 0.022(2) 0.025(2) 0.033(2) 0.0143(19) 0.0104(18) 0.0032(17) C43 0.030(2) 0.030(2) 0.036(3) 0.010(2) 0.004(2) 0.0056(19) C44 0.022(2) 0.052(3) 0.021(2) 0.006(2) 0.0025(18) 0.014(2) C45 0.014(2) 0.053(3) 0.030(3) 0.025(2) 0.0038(18) 0.0037(19) C46 0.018(2) 0.032(2) 0.034(3) 0.017(2) 0.0004(18) 0.0018(17) C47 0.026(2) 0.017(2) 0.031(2) 0.0084(18) 0.0054(18) 0.0031(17) C48 0.030(2) 0.028(2) 0.037(3) 0.012(2) 0.007(2) 0.0087(19) C49 0.033(3) 0.041(3) 0.044(3) 0.020(2) 0.019(2) 0.017(2) C50 0.044(3) 0.049(3) 0.038(3) 0.023(2) 0.021(2) 0.018(2) C51 0.036(3) 0.032(2) 0.037(3) 0.017(2) 0.013(2) 0.017(2) C52 0.027(2) 0.021(2) 0.036(3) 0.0098(19) 0.0100(19) 0.0074(17) C53 0.025(2) 0.021(2) 0.035(3) 0.0159(19) 0.0004(18) 0.0026(17) C54 0.032(2) 0.023(2) 0.037(3) 0.014(2) 0.006(2) 0.0072(18) C55 0.025(2) 0.035(3) 0.040(3) 0.014(2) -0.006(2) 0.0026(19) C56 0.036(3) 0.034(3) 0.032(3) 0.009(2) -0.008(2) 0.000(2) C57 0.036(3) 0.026(2) 0.031(3) 0.0096(19) 0.000(2) 0.0075(19) C58 0.027(2) 0.029(2) 0.035(3) 0.020(2) 0.0009(19) 0.0053(18) B1 0.021(2) 0.022(2) 0.032(3) 0.011(2) 0.002(2) 0.0037(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 2.562(4) . ? Dy1 C2 2.596(4) . ? Dy1 C3 2.641(4) . ? Dy1 C4 2.684(4) . ? Dy1 C5 2.592(4) . ? Dy1 C18 2.554(4) . ? Dy1 C19 2.579(4) . ? Dy1 C20 2.644(4) . ? Dy1 C21 2.699(4) . ? Dy1 C22 2.606(4) . ? C1 C2 1.446(6) . ? C1 C5 1.428(6) . ? C1 C6 1.555(6) . ? C2 C3 1.412(5) . ? C2 C10 1.549(6) . ? C3 C4 1.409(6) . ? C4 C5 1.395(7) . ? C4 C14 1.522(6) . ? C6 C7 1.555(6) . ? C6 C8 1.524(7) . ? C6 C9 1.530(7) . ? C10 C11 1.530(6) . ? C10 C12 1.533(6) . ? C10 C13 1.542(5) . ? C14 C15 1.505(10) . ? C14 C16 1.518(10) . ? C14 C17 1.524(6) . ? C18 C19 1.440(6) . ? C18 C22 1.433(6) . ? C18 C23 1.538(6) . ? C19 C20 1.418(6) . ? C19 C27 1.548(6) . ? C20 C21 1.388(7) . ? C21 C22 1.414(7) . ? C21 C31 1.535(7) . ? C23 C24 1.536(6) . ? C23 C25 1.545(7) . ? C23 C26 1.534(6) . ? C27 C28 1.534(6) . ? C27 C29 1.546(6) . ? C27 C30 1.536(5) . ? C31 C32 1.501(9) . ? C31 C33 1.537(10) . ? C31 C34 1.535(6) . ? F1 C36 1.361(4) . ? F2 C37 1.343(5) . ? F3 C38 1.343(5) . ? F4 C39 1.355(5) . ? F5 C40 1.362(5) . ? F6 C42 1.348(5) . ? F7 C43 1.353(5) . ? F8 C44 1.344(5) . ? F9 C45 1.351(5) . ? F10 C46 1.360(5) . ? F11 C48 1.367(5) . ? F12 C49 1.353(5) . ? F13 C50 1.344(5) . ? F14 C51 1.359(5) . ? F15 C52 1.354(4) . ? F16 C54 1.363(5) . ? F17 C55 1.358(5) . ? F18 C56 1.347(5) . ? F19 C57 1.351(5) . ? F20 C58 1.361(5) . ? C35 C36 1.381(6) . ? C35 C40 1.398(5) . ? C35 B1 1.658(6) . ? C36 C37 1.384(6) . ? C37 C38 1.373(6) . ? C38 C39 1.378(6) . ? C39 C40 1.368(6) . ? C41 C42 1.391(6) . ? C41 C46 1.381(6) . ? C41 B1 1.654(6) . ? C42 C43 1.379(6) . ? C43 C44 1.364(6) . ? C44 C45 1.383(6) . ? C45 C46 1.371(6) . ? C47 C48 1.384(6) . ? C47 C52 1.391(6) . ? C47 B1 1.654(6) . ? C48 C49 1.380(6) . ? C49 C50 1.376(6) . ? C50 C51 1.373(6) . ? C51 C52 1.363(6) . ? C53 C54 1.381(6) . ? C53 C58 1.385(6) . ? C53 B1 1.657(6) . ? C54 C55 1.380(6) . ? C55 C56 1.373(6) . ? C56 C57 1.374(6) . ? C57 C58 1.378(6) . ? 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 C1 Dy1 C2 32.57(13) . . ? C1 Dy1 C3 51.90(13) . . ? C1 Dy1 C4 52.42(13) . . ? C1 Dy1 C5 32.16(13) . . ? C1 Dy1 C19 147.68(13) . . ? C1 Dy1 C20 127.75(13) . . ? C1 Dy1 C21 127.03(14) . . ? C1 Dy1 C22 147.24(14) . . ? C2 Dy1 C3 31.26(12) . . ? C2 Dy1 C4 52.36(12) . . ? C2 Dy1 C20 156.64(14) . . ? C2 Dy1 C21 156.05(13) . . ? C2 Dy1 C22 151.44(14) . . ? C3 Dy1 C4 30.66(13) . . ? C3 Dy1 C20 165.33(13) . . ? C3 Dy1 C21 135.73(14) . . ? C4 Dy1 C21 107.61(13) . . ? C5 Dy1 C2 52.74(13) . . ? C5 Dy1 C3 50.56(14) . . ? C5 Dy1 C4 30.60(15) . . ? C5 Dy1 C20 119.76(13) . . ? C5 Dy1 C21 103.32(13) . . ? C5 Dy1 C22 115.58(14) . . ? C18 Dy1 C1 179.46(13) . . ? C18 Dy1 C2 147.69(13) . . ? C18 Dy1 C3 128.01(13) . . ? C18 Dy1 C4 127.17(14) . . ? C18 Dy1 C5 147.30(14) . . ? C18 Dy1 C19 32.58(13) . . ? C18 Dy1 C20 52.16(13) . . ? C18 Dy1 C21 52.58(14) . . ? C18 Dy1 C22 32.22(14) . . ? C19 Dy1 C2 150.53(13) . . ? C19 Dy1 C3 156.87(14) . . ? C19 Dy1 C4 155.89(13) . . ? C19 Dy1 C5 151.22(13) . . ? C19 Dy1 C20 31.46(12) . . ? C19 Dy1 C21 52.03(13) . . ? C19 Dy1 C22 52.62(14) . . ? C20 Dy1 C4 135.05(14) . . ? C20 Dy1 C21 30.09(14) . . ? C22 Dy1 C3 120.19(13) . . ? C22 Dy1 C4 103.29(13) . . ? C22 Dy1 C20 50.49(15) . . ? C22 Dy1 C21 30.85(15) . . ? C2 C1 Dy1 75.0(2) . . ? C2 C1 C6 131.5(4) . . ? C5 C1 Dy1 75.1(2) . . ? C5 C1 C2 106.6(4) . . ? C5 C1 C6 120.8(4) . . ? C6 C1 Dy1 106.5(2) . . ? C1 C2 Dy1 72.5(2) . . ? C1 C2 C10 133.0(4) . . ? C3 C2 Dy1 76.2(2) . . ? C3 C2 C1 105.7(4) . . ? C3 C2 C10 120.7(4) . . ? C10 C2 Dy1 123.3(3) . . ? C2 C3 Dy1 72.6(2) . . ? C4 C3 Dy1 76.3(2) . . ? C4 C3 C2 111.5(4) . . ? C3 C4 Dy1 73.0(2) . . ? C3 C4 C14 125.1(5) . . ? C5 C4 Dy1 71.1(2) . . ? C5 C4 C3 105.7(4) . . ? C5 C4 C14 127.6(5) . . ? C14 C4 Dy1 131.6(3) . . ? C1 C5 Dy1 72.8(2) . . ? C4 C5 Dy1 78.3(3) . . ? C4 C5 C1 110.5(4) . . ? C1 C6 C7 107.2(3) . . ? C8 C6 C1 114.9(4) . . ? C8 C6 C7 110.8(4) . . ? C8 C6 C9 106.6(4) . . ? C9 C6 C1 110.9(4) . . ? C9 C6 C7 106.0(4) . . ? C11 C10 C2 114.3(4) . . ? C11 C10 C12 106.4(4) . . ? C11 C10 C13 111.6(3) . . ? C12 C10 C2 109.9(3) . . ? C12 C10 C13 106.0(4) . . ? C13 C10 C2 108.3(3) . . ? C4 C14 C17 108.0(4) . . ? C15 C14 C4 110.9(5) . . ? C15 C14 C16 110.7(6) . . ? C15 C14 C17 110.2(6) . . ? C16 C14 C4 110.6(6) . . ? C16 C14 C17 106.2(5) . . ? C19 C18 Dy1 74.7(2) . . ? C19 C18 C23 132.9(4) . . ? C22 C18 Dy1 75.9(2) . . ? C22 C18 C19 106.3(4) . . ? C22 C18 C23 119.8(4) . . ? C23 C18 Dy1 105.8(2) . . ? C18 C19 Dy1 72.8(2) . . ? C18 C19 C27 132.2(4) . . ? C20 C19 Dy1 76.8(2) . . ? C20 C19 C18 106.3(4) . . ? C20 C19 C27 121.1(4) . . ? C27 C19 Dy1 120.9(3) . . ? C19 C20 Dy1 71.7(2) . . ? C21 C20 Dy1 77.2(2) . . ? C21 C20 C19 111.4(4) . . ? C20 C21 Dy1 72.8(2) . . ? C20 C21 C22 106.1(4) . . ? C20 C21 C31 125.6(5) . . ? C22 C21 Dy1 70.9(2) . . ? C22 C21 C31 126.7(5) . . ? C31 C21 Dy1 132.2(3) . . ? C18 C22 Dy1 71.9(2) . . ? C21 C22 Dy1 78.2(3) . . ? C21 C22 C18 109.9(4) . . ? C18 C23 C25 114.7(4) . . ? C24 C23 C18 108.0(3) . . ? C24 C23 C25 110.3(4) . . ? C26 C23 C18 111.7(4) . . ? C26 C23 C24 106.5(4) . . ? C26 C23 C25 105.5(4) . . ? C28 C27 C19 113.2(3) . . ? C28 C27 C29 106.1(4) . . ? C28 C27 C30 111.8(3) . . ? C29 C27 C19 110.4(3) . . ? C30 C27 C19 109.2(3) . . ? C30 C27 C29 105.9(3) . . ? C21 C31 C33 110.9(6) . . ? C32 C31 C21 111.1(5) . . ? C32 C31 C33 109.8(6) . . ? C32 C31 C34 110.2(6) . . ? C34 C31 C21 107.4(4) . . ? C34 C31 C33 107.5(5) . . ? C36 C35 C40 112.9(4) . . ? C36 C35 B1 127.3(4) . . ? C40 C35 B1 119.3(4) . . ? F1 C36 C35 120.5(3) . . ? F1 C36 C37 114.9(4) . . ? C35 C36 C37 124.6(4) . . ? F2 C37 C36 120.4(4) . . ? F2 C37 C38 120.0(4) . . ? C38 C37 C36 119.6(4) . . ? F3 C38 C37 120.6(4) . . ? F3 C38 C39 120.9(4) . . ? C37 C38 C39 118.5(4) . . ? F4 C39 C38 119.5(4) . . ? F4 C39 C40 120.7(4) . . ? C40 C39 C38 119.8(4) . . ? F5 C40 C35 118.8(4) . . ? F5 C40 C39 116.6(4) . . ? C39 C40 C35 124.6(4) . . ? C42 C41 B1 126.6(4) . . ? C46 C41 C42 113.4(4) . . ? C46 C41 B1 119.5(4) . . ? F6 C42 C41 120.5(4) . . ? F6 C42 C43 115.6(4) . . ? C43 C42 C41 123.8(4) . . ? F7 C43 C42 119.8(4) . . ? F7 C43 C44 120.0(4) . . ? C44 C43 C42 120.2(4) . . ? F8 C44 C43 121.4(4) . . ? F8 C44 C45 120.2(4) . . ? C43 C44 C45 118.3(4) . . ? F9 C45 C44 119.8(4) . . ? F9 C45 C46 120.5(4) . . ? C46 C45 C44 119.7(4) . . ? F10 C46 C41 119.4(4) . . ? F10 C46 C45 116.1(4) . . ? C45 C46 C41 124.6(4) . . ? C48 C47 C52 113.4(4) . . ? C48 C47 B1 126.8(4) . . ? C52 C47 B1 119.2(4) . . ? F11 C48 C47 121.2(4) . . ? F11 C48 C49 115.0(4) . . ? C49 C48 C47 123.8(4) . . ? F12 C49 C48 120.4(4) . . ? F12 C49 C50 119.6(4) . . ? C50 C49 C48 120.0(4) . . ? F13 C50 C49 120.7(4) . . ? F13 C50 C51 120.9(4) . . ? C51 C50 C49 118.4(4) . . ? F14 C51 C50 119.0(4) . . ? F14 C51 C52 121.2(4) . . ? C52 C51 C50 119.8(4) . . ? F15 C52 C47 119.0(4) . . ? F15 C52 C51 116.4(4) . . ? C51 C52 C47 124.6(4) . . ? C54 C53 C58 113.0(4) . . ? C54 C53 B1 127.6(4) . . ? C58 C53 B1 118.9(4) . . ? F16 C54 C53 121.2(4) . . ? F16 C54 C55 114.6(4) . . ? C55 C54 C53 124.2(4) . . ? F17 C55 C54 120.6(4) . . ? F17 C55 C56 119.5(4) . . ? C56 C55 C54 119.9(4) . . ? F18 C56 C55 121.1(4) . . ? F18 C56 C57 120.1(4) . . ? C55 C56 C57 118.8(4) . . ? F19 C57 C56 119.8(4) . . ? F19 C57 C58 121.3(4) . . ? C56 C57 C58 118.9(4) . . ? F20 C58 C53 119.2(4) . . ? F20 C58 C57 115.7(4) . . ? C57 C58 C53 125.1(4) . . ? C41 B1 C35 100.7(3) . . ? C41 B1 C53 113.7(3) . . ? C47 B1 C35 114.5(3) . . ? C47 B1 C41 114.2(3) . . ? C47 B1 C53 100.4(3) . . ? C53 B1 C35 114.1(3) . . ? _shelx_res_file ; TITL dy60_hp0_a.res in P-1 dy60_hp0.res created by SHELXL-2018/3 at 12:53:50 on 26-Feb-2020 REM Old TITL Dy60_HP0 in P-1 REM SHELXT solution in P-1: R1 0.129, Rweak 0.008, Alpha 0.033 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C56 B3 F20 Dy CELL 0.71073 11.627825 12.617264 20.30293 107.0309 96.3868 99.3772 ZERR 2 0.000347 0.000531 0.000663 0.0033 0.0027 0.003 LATT 1 SFAC C H B Dy F UNIT 116 116 2 2 40 L.S. 20 0 0 PLAN 20 SIZE 0.16 0.23 0.05 FREE Dy1 C24 FREE Dy1 C7 list 4 fmap 2 53 acta SHEL 100 0.83 REM REM REM WGHT 0.034700 2.613700 FVAR 0.99851 DY1 4 0.677504 0.848753 0.721771 11.00000 0.01442 0.03693 = 0.02695 0.01138 0.00358 0.00352 C1 1 0.556286 1.001141 0.721865 11.00000 0.01415 0.03389 = 0.02940 0.01601 0.00339 0.00576 C2 1 0.496757 0.933122 0.759151 11.00000 0.01544 0.02440 = 0.02896 0.00699 0.00252 0.00263 C3 1 0.445588 0.827405 0.708491 11.00000 0.01117 0.03074 = 0.03593 -0.00127 0.00460 0.00098 AFIX 43 H3 2 0.401745 0.766760 0.718048 11.00000 -1.20000 AFIX 0 C4 1 0.469316 0.825355 0.641633 11.00000 0.01081 0.05551 = 0.02875 -0.00445 0.00072 0.01037 C5 1 0.538249 0.931539 0.650554 11.00000 0.01285 0.07275 = 0.02735 0.02561 0.00728 0.01696 AFIX 43 H5 2 0.568267 0.953881 0.615019 11.00000 -1.20000 AFIX 0 C6 1 0.645694 1.116644 0.748188 11.00000 0.01577 0.03992 = 0.06605 0.03242 -0.00193 0.00370 C7 1 0.764669 1.095116 0.779465 11.00000 0.01860 0.02893 = 0.08058 0.02421 -0.00631 -0.00143 AFIX 137 H7A 2 0.792810 1.041836 0.743842 11.00000 -1.50000 H7B 2 0.752688 1.065104 0.817072 11.00000 -1.50000 H7C 2 0.821945 1.165118 0.796787 11.00000 -1.50000 AFIX 0 C8 1 0.605953 1.211240 0.800831 11.00000 0.02294 0.02405 = 0.09006 0.02294 -0.00613 -0.00014 AFIX 137 H8A 2 0.530596 1.220577 0.781376 11.00000 -1.50000 H8B 2 0.663032 1.280615 0.811424 11.00000 -1.50000 H8C 2 0.599200 1.192114 0.842852 11.00000 -1.50000 AFIX 0 C9 1 0.671546 1.159793 0.687261 11.00000 0.02626 0.08323 = 0.11398 0.07785 0.01698 0.01447 AFIX 137 H9A 2 0.700964 1.104195 0.653788 11.00000 -1.50000 H9B 2 0.729730 1.229190 0.704412 11.00000 -1.50000 H9C 2 0.600166 1.173068 0.665353 11.00000 -1.50000 AFIX 0 C10 1 0.469255 0.960694 0.834550 11.00000 0.02969 0.02540 = 0.02685 0.00696 0.00740 0.01095 C11 1 0.578672 1.008838 0.891720 11.00000 0.03806 0.04361 = 0.02535 0.00548 0.00018 0.01986 AFIX 137 H11A 2 0.629637 0.955282 0.886541 11.00000 -1.50000 H11B 2 0.554776 1.023079 0.936742 11.00000 -1.50000 H11C 2 0.620247 1.078358 0.887743 11.00000 -1.50000 AFIX 0 C12 1 0.405498 0.852801 0.845918 11.00000 0.04149 0.03652 = 0.05261 0.02051 0.02990 0.01374 AFIX 137 H12A 2 0.330328 0.825304 0.815484 11.00000 -1.50000 H12B 2 0.393597 0.869439 0.893625 11.00000 -1.50000 H12C 2 0.452638 0.796084 0.835763 11.00000 -1.50000 AFIX 0 C13 1 0.381286 1.041009 0.842682 11.00000 0.03004 0.03412 = 0.02954 0.00695 0.00376 0.01008 AFIX 137 H13A 2 0.418145 1.111658 0.837995 11.00000 -1.50000 H13B 2 0.358426 1.054262 0.887935 11.00000 -1.50000 H13C 2 0.312522 1.007109 0.807178 11.00000 -1.50000 AFIX 0 C14 1 0.406731 0.736115 0.573298 11.00000 0.02357 0.09847 = 0.03683 -0.03014 -0.00896 0.02838 C15 1 0.432306 0.621700 0.569928 11.00000 0.11048 0.10726 = 0.14573 -0.09393 -0.09096 0.07536 AFIX 137 H15A 2 0.516285 0.627110 0.578270 11.00000 -1.50000 H15B 2 0.399267 0.568653 0.524515 11.00000 -1.50000 H15C 2 0.397684 0.596334 0.604848 11.00000 -1.50000 AFIX 0 C16 1 0.441992 0.769762 0.511291 11.00000 0.03183 0.29987 = 0.02347 -0.02462 0.00156 0.00586 AFIX 137 H16A 2 0.417477 0.838983 0.511692 11.00000 -1.50000 H16B 2 0.404509 0.710986 0.468752 11.00000 -1.50000 H16C 2 0.526288 0.780596 0.514217 11.00000 -1.50000 AFIX 0 C17 1 0.274383 0.732503 0.568870 11.00000 0.02185 0.06993 = 0.04132 -0.01686 -0.00476 0.00277 AFIX 137 H17A 2 0.247847 0.713139 0.607777 11.00000 -1.50000 H17B 2 0.232950 0.676665 0.526054 11.00000 -1.50000 H17C 2 0.258980 0.805430 0.569990 11.00000 -1.50000 AFIX 0 C18 1 0.797904 0.696136 0.720418 11.00000 0.01422 0.03159 = 0.03068 0.00819 0.00481 0.00477 C19 1 0.880407 0.802271 0.753137 11.00000 0.01571 0.03128 = 0.03142 0.02240 0.00522 0.00478 C20 1 0.897776 0.851843 0.699786 11.00000 0.01350 0.04846 = 0.04782 0.03292 0.00557 0.00785 AFIX 43 H20 2 0.947045 0.921460 0.706761 11.00000 -1.20000 AFIX 0 C21 1 0.831905 0.783271 0.635817 11.00000 0.02000 0.08289 = 0.03569 0.03446 0.01358 0.02504 C22 1 0.768988 0.687235 0.648281 11.00000 0.01956 0.05672 = 0.03272 0.00725 0.00862 0.01424 AFIX 43 H22 2 0.716619 0.627213 0.614648 11.00000 -1.20000 AFIX 0 C23 1 0.726254 0.612038 0.749677 11.00000 0.02407 0.02677 = 0.06161 0.01485 0.01735 0.00466 C24 1 0.626513 0.665224 0.780577 11.00000 0.02677 0.03231 = 0.06131 0.02337 0.02229 0.00657 AFIX 137 H24A 2 0.574045 0.675691 0.744084 11.00000 -1.50000 H24B 2 0.659771 0.737204 0.815325 11.00000 -1.50000 H24C 2 0.583366 0.616030 0.801640 11.00000 -1.50000 AFIX 0 C25 1 0.799564 0.576233 0.804674 11.00000 0.03644 0.03414 = 0.07315 0.03225 0.02649 0.01151 AFIX 137 H25A 2 0.864143 0.546947 0.785605 11.00000 -1.50000 H25B 2 0.750162 0.518764 0.817032 11.00000 -1.50000 H25C 2 0.829942 0.640739 0.845561 11.00000 -1.50000 AFIX 0 C26 1 0.666362 0.501380 0.691880 11.00000 0.03055 0.03756 = 0.08635 -0.00113 0.01721 0.00250 AFIX 137 H26A 2 0.613127 0.517391 0.658107 11.00000 -1.50000 H26B 2 0.623023 0.450723 0.711942 11.00000 -1.50000 H26C 2 0.725454 0.466772 0.669418 11.00000 -1.50000 AFIX 0 C27 1 0.953380 0.856968 0.827643 11.00000 0.02115 0.02532 = 0.03539 0.01598 0.00193 0.00589 C28 1 0.876598 0.875042 0.885138 11.00000 0.03409 0.03777 = 0.03295 0.01378 0.00210 0.01445 AFIX 137 H28A 2 0.822232 0.921348 0.877031 11.00000 -1.50000 H28B 2 0.926264 0.912004 0.929812 11.00000 -1.50000 H28C 2 0.833256 0.803084 0.884545 11.00000 -1.50000 AFIX 0 C29 1 1.025902 0.975387 0.835434 11.00000 0.02675 0.03204 = 0.06760 0.02491 -0.00979 -0.00156 AFIX 137 H29A 2 1.078622 0.968363 0.801928 11.00000 -1.50000 H29B 2 1.070906 1.008112 0.881761 11.00000 -1.50000 H29C 2 0.973214 1.023223 0.827452 11.00000 -1.50000 AFIX 0 C30 1 1.044310 0.785600 0.838883 11.00000 0.02363 0.03555 = 0.03467 0.01693 0.00379 0.01034 AFIX 137 H30A 2 1.003823 0.711263 0.835910 11.00000 -1.50000 H30B 2 1.092362 0.821170 0.884181 11.00000 -1.50000 H30C 2 1.093595 0.779746 0.803586 11.00000 -1.50000 AFIX 0 C31 1 0.848540 0.796034 0.564372 11.00000 0.03185 0.15120 = 0.04273 0.05676 0.02290 0.05192 C32 1 0.819235 0.904839 0.558562 11.00000 0.11508 0.23140 = 0.11711 0.14766 0.09198 0.13272 AFIX 137 H32A 2 0.738683 0.906077 0.564581 11.00000 -1.50000 H32B 2 0.829418 0.910411 0.513330 11.00000 -1.50000 H32C 2 0.870862 0.967618 0.594060 11.00000 -1.50000 AFIX 0 C33 1 0.771656 0.695453 0.504801 11.00000 0.03485 0.27103 = 0.03545 0.05302 0.00880 0.03857 AFIX 137 H33A 2 0.800585 0.627884 0.503327 11.00000 -1.50000 H33B 2 0.775059 0.709960 0.461133 11.00000 -1.50000 H33C 2 0.691311 0.685702 0.512742 11.00000 -1.50000 AFIX 0 C34 1 0.978277 0.794215 0.557240 11.00000 0.03114 0.12042 = 0.05012 0.05351 0.02377 0.03607 AFIX 137 H34A 2 1.028518 0.858416 0.592417 11.00000 -1.50000 H34B 2 0.990528 0.797315 0.511798 11.00000 -1.50000 H34C 2 0.996941 0.725778 0.563045 11.00000 -1.50000 AFIX 0 F1 5 0.777955 0.388063 0.237569 11.00000 0.02912 0.02398 = 0.04155 0.01724 -0.00792 -0.00659 F2 5 0.916649 0.349105 0.336060 11.00000 0.03989 0.03787 = 0.04511 0.02557 -0.00392 0.00208 F3 5 1.099954 0.513615 0.420313 11.00000 0.03365 0.05228 = 0.03042 0.01458 -0.00491 0.00962 F4 5 1.147780 0.717742 0.396889 11.00000 0.02572 0.04222 = 0.03503 0.00119 -0.00401 -0.00517 F5 5 1.015132 0.756358 0.293747 11.00000 0.02481 0.02192 = 0.04909 0.01152 0.00767 -0.00292 F6 5 0.854096 0.870452 0.239423 11.00000 0.03845 0.02247 = 0.04623 0.01384 0.02109 0.00263 F7 5 0.770165 1.010199 0.337106 11.00000 0.04702 0.02688 = 0.04778 0.00433 0.01166 0.00711 F8 5 0.622950 0.928786 0.415576 11.00000 0.03464 0.06594 = 0.03027 0.01006 0.00690 0.02162 F9 5 0.555688 0.700005 0.386866 11.00000 0.02350 0.07029 = 0.03455 0.02810 0.00866 0.00388 F10 5 0.637405 0.557938 0.287512 11.00000 0.02461 0.03397 = 0.04797 0.02522 0.00313 -0.00351 F11 5 1.056580 0.599511 0.168365 11.00000 0.02599 0.04997 = 0.03407 0.02197 0.00923 0.01682 F12 5 1.142158 0.661964 0.067132 11.00000 0.03972 0.08314 = 0.06873 0.04908 0.03241 0.03397 F13 5 1.016211 0.761076 -0.010902 11.00000 0.05535 0.09425 = 0.05982 0.05555 0.03523 0.03721 F14 5 0.797182 0.792719 0.014218 11.00000 0.04475 0.04608 = 0.04259 0.02792 0.01466 0.01934 F15 5 0.704917 0.724475 0.113260 11.00000 0.02845 0.03514 = 0.03778 0.01905 0.01067 0.01367 F16 5 0.533980 0.585266 0.162995 11.00000 0.02681 0.03001 = 0.04041 0.00921 -0.00105 0.00780 F17 5 0.394122 0.415674 0.062354 11.00000 0.02615 0.05024 = 0.05648 0.00490 -0.01269 0.00841 F18 5 0.480442 0.235937 -0.011856 11.00000 0.04374 0.04077 = 0.05180 -0.00209 -0.01699 0.00058 F19 5 0.714330 0.234753 0.016527 11.00000 0.04220 0.02865 = 0.03883 0.00610 -0.00080 0.00679 F20 5 0.859572 0.408651 0.114876 11.00000 0.02593 0.02682 = 0.03807 0.00960 -0.00226 0.00834 C35 1 0.891037 0.573373 0.258363 11.00000 0.01925 0.02615 = 0.03043 0.01103 0.00534 0.00471 C36 1 0.871243 0.473183 0.273958 11.00000 0.01914 0.02520 = 0.02907 0.00909 -0.00155 0.00018 C37 1 0.940716 0.450395 0.325994 11.00000 0.02913 0.03285 = 0.02930 0.01804 0.00467 0.00573 C38 1 1.033494 0.532733 0.368187 11.00000 0.01839 0.04500 = 0.02462 0.01125 0.00072 0.00753 C39 1 1.056680 0.635204 0.355843 11.00000 0.01928 0.03231 = 0.02442 0.00224 0.00160 -0.00109 C40 1 0.987429 0.652938 0.302675 11.00000 0.01827 0.01993 = 0.03620 0.00526 0.00902 0.00085 C41 1 0.747451 0.705633 0.256431 11.00000 0.01759 0.02965 = 0.03476 0.01488 0.00072 0.00361 C42 1 0.778104 0.822791 0.273242 11.00000 0.02159 0.02549 = 0.03285 0.01434 0.01036 0.00316 C43 1 0.735985 0.897391 0.324559 11.00000 0.02968 0.02954 = 0.03604 0.00990 0.00396 0.00557 C44 1 0.662027 0.857830 0.363604 11.00000 0.02167 0.05243 = 0.02051 0.00633 0.00246 0.01364 C45 1 0.628643 0.741914 0.349063 11.00000 0.01419 0.05341 = 0.02963 0.02543 0.00378 0.00369 C46 1 0.671777 0.670520 0.297245 11.00000 0.01754 0.03238 = 0.03437 0.01739 0.00041 0.00178 C47 1 0.875455 0.660992 0.147417 11.00000 0.02637 0.01719 = 0.03090 0.00842 0.00540 0.00305 C48 1 0.986140 0.647317 0.131967 11.00000 0.03014 0.02758 = 0.03659 0.01220 0.00711 0.00866 C49 1 1.033509 0.678691 0.079457 11.00000 0.03335 0.04146 = 0.04361 0.01966 0.01877 0.01703 C50 1 0.970237 0.727689 0.039418 11.00000 0.04449 0.04897 = 0.03800 0.02346 0.02122 0.01803 C51 1 0.859849 0.742953 0.052720 11.00000 0.03631 0.03238 = 0.03704 0.01684 0.01257 0.01695 C52 1 0.815471 0.709286 0.104421 11.00000 0.02696 0.02078 = 0.03597 0.00982 0.01005 0.00739 C53 1 0.705427 0.505210 0.146197 11.00000 0.02465 0.02104 = 0.03460 0.01594 0.00036 0.00255 C54 1 0.586172 0.500922 0.128650 11.00000 0.03223 0.02316 = 0.03707 0.01404 0.00555 0.00720 C55 1 0.510626 0.413889 0.076193 11.00000 0.02456 0.03537 = 0.03960 0.01375 -0.00565 0.00255 C56 1 0.553003 0.323764 0.038100 11.00000 0.03612 0.03411 = 0.03229 0.00869 -0.00839 -0.00042 C57 1 0.671030 0.323095 0.052856 11.00000 0.03638 0.02626 = 0.03090 0.00962 0.00020 0.00746 C58 1 0.743102 0.413463 0.104624 11.00000 0.02657 0.02923 = 0.03482 0.01961 0.00093 0.00526 B1 3 0.805324 0.611529 0.202202 11.00000 0.02126 0.02152 = 0.03234 0.01106 0.00219 0.00365 HKLF 4 REM dy60_hp0_a.res in P-1 REM wR2 = 0.0944, GooF = S = 1.045, Restrained GooF = 1.045 for all data REM R1 = 0.0402 for 8367 Fo > 4sig(Fo) and 0.0547 for all 10122 data REM 739 parameters refined using 0 restraints END WGHT 0.0347 2.6137 REM Highest difference peak 1.228, deepest hole -0.757, 1-sigma level 0.097 Q1 1 0.6821 0.7824 0.6781 11.00000 0.05 1.23 Q2 1 0.6950 0.8801 0.7768 11.00000 0.05 1.17 Q3 1 0.6482 0.8161 0.6659 11.00000 0.05 0.91 Q4 1 1.0250 0.5344 0.1641 11.00000 0.05 0.87 Q5 1 0.6576 0.9326 0.7684 11.00000 0.05 0.78 Q6 1 0.7388 0.8608 0.6767 11.00000 0.05 0.69 Q7 1 0.6213 0.9202 0.6813 11.00000 0.05 0.62 Q8 1 0.6027 0.8360 0.7603 11.00000 0.05 0.51 Q9 1 0.7353 0.7848 0.7604 11.00000 0.05 0.51 Q10 1 0.7026 0.9246 0.8218 11.00000 0.05 0.51 Q11 1 0.7393 0.8420 0.7145 11.00000 0.05 0.50 Q12 1 0.4382 0.8012 0.5038 11.00000 0.05 0.50 Q13 1 1.0473 0.6327 0.2009 11.00000 0.05 0.48 Q14 1 0.6436 1.0989 0.7005 11.00000 0.05 0.44 Q15 1 0.6579 0.7630 0.6199 11.00000 0.05 0.43 Q16 1 0.8600 0.7842 0.0971 11.00000 0.05 0.43 Q17 1 0.6367 0.7208 0.7202 11.00000 0.05 0.42 Q18 1 0.7291 0.9736 0.7195 11.00000 0.05 0.42 Q19 1 0.9017 0.9521 0.5832 11.00000 0.05 0.41 Q20 1 0.8758 0.9165 0.3186 11.00000 0.05 0.40 ; _shelx_res_checksum 61688 _olex2_date_sample_data_collection 2019-11-12 _olex2_exptl_crystal_mounting_method 'In paratone oil on a Kapton loop' _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.513 _oxdiff_exptl_absorpt_empirical_full_min 0.728 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_dy60_hp1 _database_code_depnum_ccdc_archive 'CCDC 2046706' loop_ _audit_author_name _audit_author_address 'Andreas M. Thiel' ;Aarhus University, Department of Chemistry Denmark ; _audit_update_record ; 2022-10-30 deposited with the CCDC. 2023-02-13 downloaded from the CCDC. ; _audit_creation_date 2020-02-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C34 H58 Dy, B C24 F20' _chemical_formula_sum 'C58 H58 B Dy F20' _chemical_formula_weight 1308.35 _chemical_melting_point ? _chemical_oxdiff_formula C58H58BDyF20 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6573(8) _cell_length_b 12.4230(9) _cell_length_c 19.898(3) _cell_angle_alpha 106.869(11) _cell_angle_beta 95.482(10) _cell_angle_gamma 100.196(6) _cell_volume 2680.9(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3778 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.0120 _cell_measurement_theta_min 1.8080 _shelx_estimated_absorpt_T_max 0.929 _shelx_estimated_absorpt_T_min 0.724 _exptl_absorpt_coefficient_mu 1.502 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1314 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_ambient_pressure 410000 _diffrn_reflns_av_R_equivalents 0.1242 _diffrn_reflns_av_unetI/netI 0.0775 _diffrn_reflns_Laue_measured_fraction_full 0.383 _diffrn_reflns_Laue_measured_fraction_max 0.383 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 21427 _diffrn_reflns_point_group_measured_fraction_full 0.383 _diffrn_reflns_point_group_measured_fraction_max 0.383 _diffrn_reflns_theta_full 20.815 _diffrn_reflns_theta_max 20.815 _diffrn_reflns_theta_min 1.749 _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.1795 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.383 _diffrn_measured_fraction_theta_max 0.383 _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 -35.00 14.00 1.00 30.00 -- 7.76 67.00 157.00 49 2 \w -43.00 2.00 1.00 30.00 -- 7.76 97.00 143.00 45 3 \w -14.00 51.00 1.00 30.00 -- 7.76 -67.00-157.00 65 4 \w -39.00 14.00 1.00 30.00 -- 7.76 38.00-180.00 53 5 \w -42.00 33.00 1.00 30.00 -- -8.54 13.00 -3.00 75 6 \w -35.00 -12.00 1.00 30.00 -- -8.54 77.00 -30.00 23 7 \w 2.00 42.00 1.00 30.00 -- -8.54 -99.00 30.00 40 8 \w -35.00 -12.00 1.00 30.00 -- -8.54 77.00 150.00 23 9 \w -35.00 -12.00 1.00 30.00 -- 7.76 77.00 -30.00 23 10 \w 12.00 35.00 1.00 30.00 -- 7.76 -77.00 60.00 23 11 \w 34.00 58.00 1.00 30.00 -- 7.76 -99.00 30.00 24 12 \w 12.00 35.00 1.00 30.00 -- -8.54 -77.00-150.00 23 13 \w -35.00 -12.00 1.00 30.00 -- -8.54 77.00 120.00 23 14 \w -2.00 33.00 1.00 30.00 -- -8.54 -57.00-180.00 35 15 \w 34.00 58.00 1.00 30.00 -- 7.76 -99.00-150.00 24 16 \w 12.00 35.00 1.00 30.00 -- 7.76 -77.00 30.00 23 17 \w -34.00 20.00 1.00 30.00 -- 7.76 53.00 -17.00 54 18 \w 34.00 58.00 1.00 30.00 -- 7.76 -99.00 60.00 24 19 \w -53.00 9.00 1.00 30.00 -- -8.54 81.00 -29.00 62 20 \w -14.00 38.00 1.00 30.00 -- -8.54 -38.00-180.00 52 21 \w -19.00 24.00 1.00 30.00 -- -8.54 -53.00 17.00 43 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0148658000 _diffrn_orient_matrix_UB_12 -0.0157202000 _diffrn_orient_matrix_UB_13 -0.0374777000 _diffrn_orient_matrix_UB_21 -0.0321263000 _diffrn_orient_matrix_UB_22 -0.0545528000 _diffrn_orient_matrix_UB_23 -0.0007345000 _diffrn_orient_matrix_UB_31 -0.0516162000 _diffrn_orient_matrix_UB_32 0.0225598000 _diffrn_orient_matrix_UB_33 0.0041189000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1609 _reflns_number_total 2149 _reflns_odcompleteness_completeness 38.56 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 20.77 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.542 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.096 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 278 _refine_ls_number_reflns 2149 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0806 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+29.6617P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1889 _refine_ls_wR_factor_ref 0.2115 _refine_special_details ? _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. Restrained planarity C54, C55, C56, C57, C58, F16, F17, F18, F19, F20, B1, C53 with sigma of 0.1 C47, C52, C51, C50, C49, C48, F15, F14, F13, F12, F11, B1 with sigma of 0.1 C35, C36, C37, C38, C39, C40, F1, F2, F3, F4, F5, B1 with sigma of 0.1 C41, C46, C45, C44, C43, C42, F10, F9, F8, F7, F6, B1 with sigma of 0.1 3.a Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C20(H20), C22(H22) 3.b Fitted pentagon refined as free rotating group: C1(C2,C3,C4,C5), C21(C20,C19,C18,C22) 3.c Fitted hexagon refined as free rotating group: C35(C40,C39,C38,C37,C36), C41(C42,C43,C44,C45,C46), C47(C48,C49,C50,C51,C52), C53(C58,C57,C56,C55,C54) 3.d Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B, H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A, H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.68595(10) 0.84653(10) 0.72036(16) 0.054(2) Uani 1 1 d . . . . . C1 C 0.5632(12) 0.9977(12) 0.7219(16) 0.053(7) Uiso 1 1 d . . . . . C2 C 0.5058(17) 0.9313(17) 0.7612(15) 0.061(8) Uiso 1 1 d G . . . . C3 C 0.4515(13) 0.8207(14) 0.7132(17) 0.037(6) Uiso 1 1 d G . . . . H3 H 0.407955 0.760203 0.724804 0.044 Uiso 1 1 calc R . . . . C4 C 0.4754(13) 0.8187(12) 0.6442(16) 0.043(6) Uiso 1 1 d G . . . . C5 C 0.5444(12) 0.9281(15) 0.6496(15) 0.033(6) Uiso 1 1 d G . . . . H5 H 0.572391 0.950248 0.612365 0.040 Uiso 1 1 calc R . . . . C6 C 0.656(2) 1.117(2) 0.750(3) 0.046(6) Uiso 1 1 d . . . . . C7 C 0.771(2) 1.101(2) 0.773(3) 0.055(7) Uiso 1 1 d . . . . . H7A H 0.777471 1.104995 0.822651 0.083 Uiso 1 1 calc GR . . . . H7B H 0.830907 1.160282 0.767929 0.083 Uiso 1 1 calc GR . . . . H7C H 0.781058 1.027054 0.745548 0.083 Uiso 1 1 calc GR . . . . C8 C 0.609(2) 1.215(2) 0.804(3) 0.070(8) Uiso 1 1 d . . . . . H8A H 0.530614 1.216048 0.784759 0.105 Uiso 1 1 calc GR . . . . H8B H 0.660115 1.288369 0.811379 0.105 Uiso 1 1 calc GR . . . . H8C H 0.607718 1.199541 0.848512 0.105 Uiso 1 1 calc GR . . . . C9 C 0.675(2) 1.160(2) 0.683(3) 0.056(7) Uiso 1 1 d . . . . . H9A H 0.708499 1.105979 0.650064 0.084 Uiso 1 1 calc GR . . . . H9B H 0.726718 1.234161 0.698365 0.084 Uiso 1 1 calc GR . . . . H9C H 0.599924 1.164274 0.660627 0.084 Uiso 1 1 calc GR . . . . C10 C 0.482(2) 0.960(2) 0.841(3) 0.046(7) Uiso 1 1 d . . . . . C11 C 0.581(2) 1.010(2) 0.888(3) 0.054(7) Uiso 1 1 d . . . . . H11A H 0.623126 0.952036 0.893328 0.082 Uiso 1 1 calc GR . . . . H11B H 0.560404 1.047830 0.933508 0.082 Uiso 1 1 calc GR . . . . H11C H 0.629755 1.065009 0.872352 0.082 Uiso 1 1 calc GR . . . . C12 C 0.420(3) 0.846(2) 0.854(4) 0.072(8) Uiso 1 1 d . . . . . H12A H 0.346152 0.814623 0.822155 0.108 Uiso 1 1 calc GR . . . . H12B H 0.405464 0.863264 0.902096 0.108 Uiso 1 1 calc GR . . . . H12C H 0.469532 0.791315 0.844973 0.108 Uiso 1 1 calc GR . . . . C13 C 0.383(2) 1.030(2) 0.843(4) 0.070(8) Uiso 1 1 d . . . . . H13A H 0.384632 1.064594 0.805692 0.105 Uiso 1 1 calc GR . . . . H13B H 0.395229 1.089339 0.888159 0.105 Uiso 1 1 calc GR . . . . H13C H 0.307330 0.979403 0.836631 0.105 Uiso 1 1 calc GR . . . . C14 C 0.414(2) 0.727(2) 0.576(3) 0.042(6) Uiso 1 1 d . . . . . C15 C 0.490(4) 0.645(4) 0.540(6) 0.155(17) Uiso 1 1 d . . . . . H15A H 0.514538 0.663998 0.499071 0.233 Uiso 1 1 calc GR . . . . H15B H 0.445291 0.566777 0.524598 0.233 Uiso 1 1 calc GR . . . . H15C H 0.558873 0.651463 0.572760 0.233 Uiso 1 1 calc GR . . . . C16 C 0.387(4) 0.776(4) 0.510(6) 0.17(2) Uiso 1 1 d . . . . . H16A H 0.394682 0.858145 0.528081 0.262 Uiso 1 1 calc GR . . . . H16B H 0.307558 0.741002 0.485992 0.262 Uiso 1 1 calc GR . . . . H16C H 0.441248 0.758657 0.477413 0.262 Uiso 1 1 calc GR . . . . C17 C 0.300(4) 0.665(6) 0.580(8) 0.22(3) Uiso 1 1 d . . . . . H17A H 0.307467 0.592242 0.586245 0.325 Uiso 1 1 calc GR . . . . H17B H 0.246931 0.652011 0.537617 0.325 Uiso 1 1 calc GR . . . . H17C H 0.270772 0.709180 0.620380 0.325 Uiso 1 1 calc GR . . . . C21 C 0.8473(17) 0.7899(17) 0.6354(18) 0.055(7) Uiso 1 1 d . . . . . C20 C 0.9121(12) 0.8614(11) 0.7023(19) 0.038(6) Uiso 1 1 d G . . . . H20 H 0.961250 0.933318 0.711251 0.046 Uiso 1 1 calc R . . . . C19 C 0.8885(18) 0.8040(17) 0.7533(17) 0.061(8) Uiso 1 1 d G . . . . C18 C 0.8092(16) 0.6969(14) 0.7178(19) 0.052(8) Uiso 1 1 d G . . . . C22 C 0.7838(13) 0.6882(12) 0.6450(18) 0.045(7) Uiso 1 1 d G . . . . H22 H 0.734172 0.626750 0.609714 0.053 Uiso 1 1 calc R . . . . C23 C 0.740(2) 0.608(2) 0.752(3) 0.045(6) Uiso 1 1 d . . . . . C24 C 0.634(2) 0.651(2) 0.775(4) 0.060(7) Uiso 1 1 d . . . . . H24A H 0.656869 0.714058 0.818684 0.091 Uiso 1 1 calc GR . . . . H24B H 0.579018 0.589710 0.783066 0.091 Uiso 1 1 calc GR . . . . H24C H 0.596576 0.676098 0.739157 0.091 Uiso 1 1 calc GR . . . . C25 C 0.808(2) 0.569(3) 0.796(3) 0.069(8) Uiso 1 1 d . . . . . H25A H 0.866282 0.535909 0.771282 0.103 Uiso 1 1 calc GR . . . . H25B H 0.758598 0.511864 0.810344 0.103 Uiso 1 1 calc GR . . . . H25C H 0.846344 0.632212 0.837349 0.103 Uiso 1 1 calc GR . . . . C26 C 0.682(2) 0.494(2) 0.687(3) 0.058(7) Uiso 1 1 d . . . . . H26A H 0.633865 0.512565 0.652243 0.088 Uiso 1 1 calc GR . . . . H26B H 0.633830 0.439666 0.704687 0.088 Uiso 1 1 calc GR . . . . H26C H 0.743067 0.459914 0.666160 0.088 Uiso 1 1 calc GR . . . . C27 C 0.954(2) 0.854(2) 0.820(3) 0.044(6) Uiso 1 1 d . . . . . C28 C 0.879(3) 0.871(2) 0.882(4) 0.072(8) Uiso 1 1 d . . . . . H28A H 0.827214 0.920555 0.877095 0.108 Uiso 1 1 calc GR . . . . H28B H 0.931086 0.904252 0.926743 0.108 Uiso 1 1 calc GR . . . . H28C H 0.833974 0.797202 0.880325 0.108 Uiso 1 1 calc GR . . . . C29 C 1.027(2) 0.982(2) 0.841(4) 0.071(8) Uiso 1 1 d . . . . . H29A H 1.082764 0.986402 0.808863 0.106 Uiso 1 1 calc GR . . . . H29B H 1.067348 1.005026 0.888570 0.106 Uiso 1 1 calc GR . . . . H29C H 0.973775 1.031844 0.837234 0.106 Uiso 1 1 calc GR . . . . C30 C 1.055(2) 0.791(2) 0.841(3) 0.064(8) Uiso 1 1 d . . . . . H30A H 1.020737 0.711427 0.832572 0.095 Uiso 1 1 calc GR . . . . H30B H 1.087891 0.827013 0.889934 0.095 Uiso 1 1 calc GR . . . . H30C H 1.115350 0.797588 0.811840 0.095 Uiso 1 1 calc GR . . . . C31 C 0.866(2) 0.809(2) 0.564(3) 0.048(7) Uiso 1 1 d . . . . . C32 C 0.825(4) 0.915(4) 0.561(5) 0.121(13) Uiso 1 1 d . . . . . H32A H 0.759769 0.895207 0.522731 0.182 Uiso 1 1 calc GR . . . . H32B H 0.888389 0.968273 0.552266 0.182 Uiso 1 1 calc GR . . . . H32C H 0.800292 0.950964 0.604937 0.182 Uiso 1 1 calc GR . . . . C33 C 0.816(3) 0.704(3) 0.506(5) 0.123(13) Uiso 1 1 d . . . . . H33A H 0.795682 0.641017 0.524119 0.184 Uiso 1 1 calc GR . . . . H33B H 0.872374 0.688004 0.474009 0.184 Uiso 1 1 calc GR . . . . H33C H 0.746083 0.713406 0.480033 0.184 Uiso 1 1 calc GR . . . . C34 C 0.998(3) 0.835(4) 0.560(5) 0.134(14) Uiso 1 1 d . . . . . H34A H 1.033101 0.912322 0.590068 0.201 Uiso 1 1 calc GR . . . . H34B H 1.010157 0.827027 0.512306 0.201 Uiso 1 1 calc GR . . . . H34C H 1.035139 0.782057 0.577003 0.201 Uiso 1 1 calc GR . . . . F1 F 0.7771(11) 0.3873(11) 0.2449(16) 0.060(4) Uiso 1 1 d . . . . . F2 F 0.9214(13) 0.3515(13) 0.3474(18) 0.074(4) Uiso 1 1 d . . . . . F3 F 1.0937(15) 0.5234(15) 0.432(2) 0.098(5) Uiso 1 1 d . . . . . F4 F 1.1370(14) 0.7353(14) 0.413(2) 0.089(5) Uiso 1 1 d . . . . . F5 F 1.0043(12) 0.7707(12) 0.3070(17) 0.063(4) Uiso 1 1 d . . . . . F6 F 0.8430(12) 0.8826(12) 0.2466(17) 0.065(4) Uiso 1 1 d . . . . . F7 F 0.7455(12) 1.0188(12) 0.3430(17) 0.069(4) Uiso 1 1 d . . . . . F8 F 0.6013(13) 0.9298(13) 0.4222(18) 0.078(5) Uiso 1 1 d . . . . . F9 F 0.5452(13) 0.7014(13) 0.3999(18) 0.077(4) Uiso 1 1 d . . . . . F10 F 0.6331(11) 0.5601(11) 0.2998(16) 0.055(4) Uiso 1 1 d . . . . . F11 F 1.0511(11) 0.6043(12) 0.1759(17) 0.060(4) Uiso 1 1 d . . . . . F12 F 1.1321(14) 0.6481(14) 0.066(2) 0.090(5) Uiso 1 1 d . . . . . F13 F 1.0061(17) 0.7366(16) -0.020(2) 0.119(7) Uiso 1 1 d . . . . . F14 F 0.7933(13) 0.7826(13) 0.0127(19) 0.078(5) Uiso 1 1 d . . . . . F15 F 0.7045(11) 0.7306(11) 0.1192(16) 0.056(4) Uiso 1 1 d . . . . . F16 F 0.5302(11) 0.5912(11) 0.1710(16) 0.055(4) Uiso 1 1 d . . . . . F17 F 0.3980(13) 0.4301(13) 0.0612(19) 0.083(5) Uiso 1 1 d . . . . . F18 F 0.4844(15) 0.2521(15) -0.019(2) 0.099(5) Uiso 1 1 d . . . . . F19 F 0.7148(12) 0.2460(12) 0.0120(17) 0.066(4) Uiso 1 1 d . . . . . F20 F 0.8544(11) 0.4114(11) 0.1195(15) 0.052(3) Uiso 1 1 d . . . . . C35 C 0.8883(12) 0.5844(13) 0.2731(13) 0.051(7) Uiso 1 1 d . . . . . C40 C 0.9800(14) 0.6710(10) 0.3171(14) 0.047(7) Uiso 1 1 d G . . . . C39 C 1.0499(12) 0.6495(12) 0.3703(14) 0.061(8) Uiso 1 1 d G . . . . C38 C 1.0283(13) 0.5414(15) 0.3795(13) 0.065(8) Uiso 1 1 d G . . . . C37 C 0.9367(14) 0.4548(11) 0.3355(14) 0.053(7) Uiso 1 1 d G . . . . C36 C 0.8667(12) 0.4763(11) 0.2823(14) 0.046(6) Uiso 1 1 d G . . . . C41 C 0.7396(13) 0.7133(11) 0.2692(13) 0.044(6) Uiso 1 1 d . . . . . C42 C 0.7676(12) 0.8310(12) 0.2794(14) 0.051(7) Uiso 1 1 d G . . . . C43 C 0.7208(13) 0.9058(9) 0.3305(14) 0.049(6) Uiso 1 1 d G . . . . C44 C 0.6459(14) 0.8628(12) 0.3714(13) 0.066(8) Uiso 1 1 d G . . . . C45 C 0.6179(13) 0.7451(13) 0.3612(13) 0.058(7) Uiso 1 1 d G . . . . C46 C 0.6648(13) 0.6704(10) 0.3101(14) 0.046(6) Uiso 1 1 d G . . . . C47 C 0.8701(12) 0.6648(12) 0.1507(13) 0.050(7) Uiso 1 1 d . . . . . C48 C 0.9798(12) 0.6430(12) 0.1368(14) 0.043(6) Uiso 1 1 d G . . . . C49 C 1.0257(11) 0.6668(13) 0.0795(14) 0.057(7) Uiso 1 1 d G . . . . C50 C 0.9619(14) 0.7123(13) 0.0360(13) 0.080(9) Uiso 1 1 d G . . . . C51 C 0.8522(13) 0.7341(13) 0.0499(13) 0.050(7) Uiso 1 1 d G . . . . C52 C 0.8063(10) 0.7103(12) 0.1072(14) 0.045(6) Uiso 1 1 d G . . . . C53 C 0.7006(12) 0.5096(12) 0.1518(13) 0.048(6) Uiso 1 1 d . . . . . C58 C 0.7468(10) 0.4213(13) 0.1109(14) 0.045(6) Uiso 1 1 d G . . . . C57 C 0.6751(14) 0.3352(12) 0.0537(14) 0.045(6) Uiso 1 1 d G . . . . C56 C 0.5570(13) 0.3374(13) 0.0375(13) 0.074(9) Uiso 1 1 d G . . . . C55 C 0.5108(10) 0.4257(14) 0.0784(14) 0.055(7) Uiso 1 1 d G . . . . C54 C 0.5825(13) 0.5118(12) 0.1356(14) 0.048(7) Uiso 1 1 d G . . . . B1 B 0.800(2) 0.618(2) 0.215(2) 0.047(8) Uiso 1 1 d . . . . . 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 0.0470(8) 0.0503(9) 0.068(7) 0.020(2) 0.0116(19) 0.0153(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 2.549(14) . ? Dy1 C2 2.606(17) . ? Dy1 C3 2.680(14) . ? Dy1 C4 2.67(2) . ? Dy1 C5 2.590(18) . ? Dy1 C21 2.70(2) . ? Dy1 C20 2.675(13) . ? Dy1 C19 2.57(2) . ? Dy1 C18 2.535(15) . ? Dy1 C22 2.613(18) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 C6 1.59(3) . ? C2 C3 1.4200 . ? C2 C10 1.58(6) . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C4 C14 1.52(5) . ? C6 C7 1.44(4) . ? C6 C8 1.59(5) . ? C6 C9 1.58(7) . ? C10 C11 1.34(6) . ? C10 C12 1.57(3) . ? C10 C13 1.57(3) . ? C14 C15 1.54(5) . ? C14 C16 1.62(10) . ? C14 C17 1.44(5) . ? C21 C20 1.4200 . ? C21 C22 1.4200 . ? C21 C31 1.54(5) . ? C20 C19 1.4200 . ? C19 C18 1.4200 . ? C19 C27 1.38(6) . ? C18 C22 1.4200 . ? C18 C23 1.60(3) . ? C23 C24 1.49(3) . ? C23 C25 1.37(6) . ? C23 C26 1.61(6) . ? C27 C28 1.56(7) . ? C27 C29 1.57(4) . ? C27 C30 1.60(4) . ? C31 C32 1.50(4) . ? C31 C33 1.45(8) . ? C31 C34 1.53(3) . ? F1 C36 1.35(2) . ? F2 C37 1.356(18) . ? F3 C38 1.33(4) . ? F4 C39 1.35(3) . ? F5 C40 1.298(16) . ? F6 C42 1.33(2) . ? F7 C43 1.326(15) . ? F8 C44 1.32(3) . ? F9 C45 1.35(2) . ? F10 C46 1.303(14) . ? F11 C48 1.33(3) . ? F12 C49 1.337(17) . ? F13 C50 1.36(4) . ? F14 C51 1.30(3) . ? F15 C52 1.286(14) . ? F16 C54 1.32(2) . ? F17 C55 1.341(19) . ? F18 C56 1.38(4) . ? F19 C57 1.36(2) . ? F20 C58 1.281(15) . ? C35 C40 1.3900 . ? C35 C36 1.3900 . ? C35 B1 1.67(4) . ? C40 C39 1.3900 . ? C39 C38 1.3900 . ? C38 C37 1.3900 . ? C37 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 B1 1.67(3) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C47 B1 1.76(4) . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C53 C58 1.3900 . ? C53 C54 1.3900 . ? C53 B1 1.71(4) . ? C58 C57 1.3900 . ? C57 C56 1.3900 . ? C56 C55 1.3900 . ? C55 C54 1.3900 . ? 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 C1 Dy1 C2 31.95(18) . . ? C1 Dy1 C3 52.1(2) . . ? C1 Dy1 C4 52.2(2) . . ? C1 Dy1 C5 32.07(16) . . ? C1 Dy1 C21 127.4(7) . . ? C1 Dy1 C20 127.2(5) . . ? C1 Dy1 C19 147.5(6) . . ? C1 Dy1 C22 147.6(10) . . ? C2 Dy1 C3 31.13(16) . . ? C2 Dy1 C4 51.6(2) . . ? C2 Dy1 C21 157.2(8) . . ? C2 Dy1 C20 154.0(6) . . ? C2 Dy1 C22 153.5(7) . . ? C3 Dy1 C21 139.7(9) . . ? C4 Dy1 C3 30.79(17) . . ? C4 Dy1 C21 111.2(9) . . ? C4 Dy1 C20 139.2(10) . . ? C5 Dy1 C2 52.49(19) . . ? C5 Dy1 C3 51.7(2) . . ? C5 Dy1 C4 31.3(2) . . ? C5 Dy1 C21 104.8(8) . . ? C5 Dy1 C20 121.3(7) . . ? C5 Dy1 C22 116.2(9) . . ? C20 Dy1 C3 169.8(11) . . ? C20 Dy1 C21 30.65(17) . . ? C19 Dy1 C2 148.9(9) . . ? C19 Dy1 C3 155.0(7) . . ? C19 Dy1 C4 157.8(8) . . ? C19 Dy1 C5 152.6(7) . . ? C19 Dy1 C21 51.61(18) . . ? C19 Dy1 C20 31.31(16) . . ? C19 Dy1 C22 52.58(18) . . ? C18 Dy1 C1 179.4(8) . . ? C18 Dy1 C2 148.6(6) . . ? C18 Dy1 C3 128.4(5) . . ? C18 Dy1 C4 127.9(7) . . ? C18 Dy1 C5 147.6(10) . . ? C18 Dy1 C21 52.0(2) . . ? C18 Dy1 C20 52.3(2) . . ? C18 Dy1 C19 32.3(2) . . ? C18 Dy1 C22 31.98(15) . . ? C22 Dy1 C3 122.4(7) . . ? C22 Dy1 C4 105.2(8) . . ? C22 Dy1 C21 31.0(2) . . ? C22 Dy1 C20 51.5(2) . . ? C2 C1 Dy1 76.2(6) . . ? C2 C1 C5 108.0 . . ? C2 C1 C6 129(2) . . ? C5 C1 Dy1 75.5(8) . . ? C5 C1 C6 122(2) . . ? C6 C1 Dy1 104.7(11) . . ? C1 C2 Dy1 71.8(5) . . ? C1 C2 C3 108.0 . . ? C1 C2 C10 133.7(17) . . ? C3 C2 Dy1 77.3(7) . . ? C3 C2 C10 118.0(17) . . ? C10 C2 Dy1 122.0(18) . . ? C2 C3 Dy1 71.6(7) . . ? C4 C3 Dy1 74.2(8) . . ? C4 C3 C2 108.0 . . ? C3 C4 Dy1 75.0(7) . . ? C3 C4 C5 108.0 . . ? C3 C4 C14 125.0(19) . . ? C5 C4 Dy1 71.2(5) . . ? C5 C4 C14 125.6(19) . . ? C14 C4 Dy1 130.2(11) . . ? C1 C5 Dy1 72.4(8) . . ? C4 C5 Dy1 77.5(6) . . ? C4 C5 C1 108.0 . . ? C7 C6 C1 110.6(17) . . ? C7 C6 C8 116(4) . . ? C7 C6 C9 104(2) . . ? C8 C6 C1 112.8(18) . . ? C9 C6 C1 107(4) . . ? C9 C6 C8 106(2) . . ? C11 C10 C2 113(2) . . ? C11 C10 C12 110(4) . . ? C11 C10 C13 117(4) . . ? C12 C10 C2 109(4) . . ? C13 C10 C2 103(4) . . ? C13 C10 C12 103.3(18) . . ? C4 C14 C15 115(4) . . ? C4 C14 C16 114(3) . . ? C15 C14 C16 97(5) . . ? C17 C14 C4 114(6) . . ? C17 C14 C15 111(4) . . ? C17 C14 C16 103(5) . . ? C20 C21 Dy1 73.8(8) . . ? C20 C21 C31 125(2) . . ? C22 C21 Dy1 71.2(5) . . ? C22 C21 C20 108.0 . . ? C22 C21 C31 126(2) . . ? C31 C21 Dy1 130.9(12) . . ? C21 C20 Dy1 75.6(8) . . ? C21 C20 C19 108.0 . . ? C19 C20 Dy1 70.4(8) . . ? C20 C19 Dy1 78.3(8) . . ? C18 C19 Dy1 72.3(5) . . ? C18 C19 C20 108.0 . . ? C27 C19 Dy1 122.2(18) . . ? C27 C19 C20 116(2) . . ? C27 C19 C18 135(2) . . ? C19 C18 Dy1 75.4(6) . . ? C19 C18 C22 108.0 . . ? C19 C18 C23 128(3) . . ? C22 C18 Dy1 77.0(10) . . ? C22 C18 C23 123(3) . . ? C23 C18 Dy1 106.1(10) . . ? C21 C22 Dy1 77.8(6) . . ? C21 C22 C18 108.0 . . ? C18 C22 Dy1 71.0(9) . . ? C18 C23 C26 106(4) . . ? C24 C23 C18 107.8(18) . . ? C24 C23 C26 102(3) . . ? C25 C23 C18 116(2) . . ? C25 C23 C24 120(5) . . ? C25 C23 C26 103(3) . . ? C19 C27 C28 114(2) . . ? C19 C27 C29 119(4) . . ? C19 C27 C30 116(3) . . ? C28 C27 C29 98(3) . . ? C28 C27 C30 106(4) . . ? C29 C27 C30 101(2) . . ? C32 C31 C21 109(4) . . ? C32 C31 C34 105(2) . . ? C33 C31 C21 110(3) . . ? C33 C31 C32 117(5) . . ? C33 C31 C34 106(4) . . ? C34 C31 C21 109(4) . . ? C40 C35 C36 120.0 . . ? C40 C35 B1 118.0(13) . . ? C36 C35 B1 121.8(13) . . ? F5 C40 C35 120.5(18) . . ? F5 C40 C39 119.4(18) . . ? C35 C40 C39 120.0 . . ? F4 C39 C40 118.8(16) . . ? F4 C39 C38 121.1(16) . . ? C40 C39 C38 120.0 . . ? F3 C38 C39 119.2(15) . . ? F3 C38 C37 120.7(14) . . ? C39 C38 C37 120.0 . . ? F2 C37 C38 116.6(17) . . ? F2 C37 C36 123.4(17) . . ? C36 C37 C38 120.0 . . ? F1 C36 C35 125.2(14) . . ? F1 C36 C37 114.8(15) . . ? C37 C36 C35 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 B1 123.8(12) . . ? C46 C41 B1 116.0(12) . . ? F6 C42 C41 125.4(12) . . ? F6 C42 C43 114.5(13) . . ? C41 C42 C43 120.0 . . ? F7 C43 C42 122.5(15) . . ? F7 C43 C44 117.4(15) . . ? C44 C43 C42 120.0 . . ? F8 C44 C43 122.8(13) . . ? F8 C44 C45 117.1(13) . . ? C43 C44 C45 120.0 . . ? F9 C45 C44 121.1(13) . . ? F9 C45 C46 118.9(13) . . ? C44 C45 C46 120.0 . . ? F10 C46 C41 121.4(15) . . ? F10 C46 C45 118.5(14) . . ? C45 C46 C41 120.0 . . ? C48 C47 C52 120.0 . . ? C48 C47 B1 121.2(12) . . ? C52 C47 B1 118.2(13) . . ? F11 C48 C47 125.7(15) . . ? F11 C48 C49 114.3(14) . . ? C47 C48 C49 120.0 . . ? F12 C49 C48 120.6(19) . . ? F12 C49 C50 119.4(19) . . ? C50 C49 C48 120.0 . . ? F13 C50 C49 120.7(15) . . ? F13 C50 C51 119.3(15) . . ? C49 C50 C51 120.0 . . ? F14 C51 C50 121.5(16) . . ? F14 C51 C52 118.4(16) . . ? C50 C51 C52 120.0 . . ? F15 C52 C47 120.7(17) . . ? F15 C52 C51 119.3(17) . . ? C51 C52 C47 120.0 . . ? C58 C53 C54 120.0 . . ? C58 C53 B1 115.6(12) . . ? C54 C53 B1 124.1(12) . . ? F20 C58 C53 125.8(16) . . ? F20 C58 C57 114.2(16) . . ? C53 C58 C57 120.0 . . ? F19 C57 C58 122.8(15) . . ? F19 C57 C56 117.2(15) . . ? C56 C57 C58 120.0 . . ? F18 C56 C57 120.7(13) . . ? F18 C56 C55 119.3(13) . . ? C57 C56 C55 120.0 . . ? F17 C55 C56 120.0(17) . . ? F17 C55 C54 120.0(16) . . ? C54 C55 C56 120.0 . . ? F16 C54 C53 124.8(15) . . ? F16 C54 C55 115.2(15) . . ? C55 C54 C53 120.0 . . ? C35 B1 C41 101(2) . . ? C35 B1 C47 115.3(14) . . ? C35 B1 C53 119.0(14) . . ? C41 B1 C47 115.7(14) . . ? C41 B1 C53 114.1(14) . . ? C53 B1 C47 93(2) . . ? _shelx_res_file ; TITL dy60_hp1a_38deg_a.res in P-1 dy60_hp1a_38deg.res created by SHELXL-2018/3 at 15:39:10 on 26-Feb-2020 REM Old TITL Dy60_HP1a_38deg in P-1 REM SHELXT solution in P-1: R1 0.140, Rweak 0.027, Alpha 0.095 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C55 B F21 Dy CELL 0.71073 11.6573 12.423 19.8984 106.869 95.482 100.196 ZERR 2 0.0008 0.0009 0.0034 0.011 0.01 0.006 LATT 1 SFAC C H B Dy F UNIT 116 116 2 2 40 FLAT C54 C55 C56 C57 C58 F16 F17 F18 F19 F20 B1 C53 FLAT C47 C52 C51 C50 C49 C48 F15 F14 F13 F12 F11 B1 FLAT C35 C36 C37 C38 C39 C40 F1 F2 F3 F4 F5 B1 FLAT C41 C46 C45 C44 C43 C42 F10 F9 F8 F7 F6 B1 L.S. 20 0 0 PLAN 20 SIZE 0.16 0.23 0.05 FREE Dy1 C24 FREE Dy1 C7 list 4 fmap 2 53 acta SHEL 100 0.83 OMIT 0 180 OMIT -5 -2 2 OMIT 4 -5 1 OMIT 5 -4 1 OMIT -5 3 3 OMIT -5 -2 3 OMIT -5 -1 5 OMIT 0 -6 4 OMIT 0 -6 3 OMIT -5 -2 1 OMIT -4 -9 11 OMIT 2 -10 9 OMIT -8 -5 5 OMIT -7 -4 5 OMIT 9 -7 4 OMIT -5 -9 2 OMIT -7 -6 1 REM REM REM WGHT 0.109200 29.661699 FVAR 0.69906 DY1 4 0.685955 0.846532 0.720357 11.00000 0.04695 0.05027 = 0.06788 0.01988 0.01162 0.01534 AFIX 56 C1 1 0.563220 0.997659 0.721939 11.00000 0.05283 C2 1 0.505801 0.931298 0.761202 11.00000 0.06052 C3 1 0.451499 0.820708 0.713155 11.00000 0.03667 AFIX 43 H3 2 0.407955 0.760203 0.724804 11.00000 -1.20000 AFIX 55 C4 1 0.475358 0.818721 0.644198 11.00000 0.04349 C5 1 0.544405 0.928083 0.649627 11.00000 0.03295 AFIX 43 H5 2 0.572391 0.950248 0.612365 11.00000 -1.20000 AFIX 0 C6 1 0.656074 1.117253 0.749952 11.00000 0.04635 C7 1 0.771011 1.101037 0.773493 11.00000 0.05539 AFIX 137 H7A 2 0.777471 1.104995 0.822651 11.00000 -1.50000 H7B 2 0.830907 1.160282 0.767929 11.00000 -1.50000 H7C 2 0.781058 1.027054 0.745548 11.00000 -1.50000 AFIX 0 C8 1 0.608972 1.214966 0.803995 11.00000 0.06976 AFIX 137 H8A 2 0.530614 1.216048 0.784759 11.00000 -1.50000 H8B 2 0.660115 1.288369 0.811379 11.00000 -1.50000 H8C 2 0.607718 1.199541 0.848512 11.00000 -1.50000 AFIX 0 C9 1 0.674632 1.159586 0.683175 11.00000 0.05621 AFIX 137 H9A 2 0.708499 1.105979 0.650064 11.00000 -1.50000 H9B 2 0.726718 1.234161 0.698365 11.00000 -1.50000 H9C 2 0.599924 1.164274 0.660627 11.00000 -1.50000 AFIX 0 C10 1 0.482482 0.959844 0.840960 11.00000 0.04607 C11 1 0.580908 1.009709 0.888394 11.00000 0.05440 AFIX 137 H11A 2 0.623126 0.952036 0.893328 11.00000 -1.50000 H11B 2 0.560404 1.047830 0.933508 11.00000 -1.50000 H11C 2 0.629755 1.065009 0.872352 11.00000 -1.50000 AFIX 0 C12 1 0.419806 0.846197 0.853795 11.00000 0.07185 AFIX 137 H12A 2 0.346152 0.814623 0.822155 11.00000 -1.50000 H12B 2 0.405464 0.863264 0.902096 11.00000 -1.50000 H12C 2 0.469532 0.791315 0.844973 11.00000 -1.50000 AFIX 0 C13 1 0.382734 1.030118 0.843065 11.00000 0.07029 AFIX 137 H13A 2 0.384632 1.064594 0.805692 11.00000 -1.50000 H13B 2 0.395229 1.089339 0.888159 11.00000 -1.50000 H13C 2 0.307330 0.979403 0.836631 11.00000 -1.50000 AFIX 0 C14 1 0.414280 0.726814 0.575593 11.00000 0.04216 C15 1 0.490386 0.644544 0.539631 11.00000 0.15506 AFIX 137 H15A 2 0.514538 0.663998 0.499071 11.00000 -1.50000 H15B 2 0.445291 0.566777 0.524598 11.00000 -1.50000 H15C 2 0.558873 0.651463 0.572760 11.00000 -1.50000 AFIX 0 C16 1 0.386618 0.776197 0.510080 11.00000 0.17438 AFIX 137 H16A 2 0.394682 0.858145 0.528081 11.00000 -1.50000 H16B 2 0.307558 0.741002 0.485992 11.00000 -1.50000 H16C 2 0.441248 0.758657 0.477413 11.00000 -1.50000 AFIX 0 C17 1 0.300401 0.664919 0.580354 11.00000 0.21684 AFIX 137 H17A 2 0.307467 0.592242 0.586245 11.00000 -1.50000 H17B 2 0.246931 0.652011 0.537617 11.00000 -1.50000 H17C 2 0.270772 0.709180 0.620380 11.00000 -1.50000 AFIX 56 C21 1 0.847346 0.789919 0.635402 11.00000 0.05508 C20 1 0.912052 0.861448 0.702337 11.00000 0.03794 AFIX 43 H20 2 0.961250 0.933318 0.711251 11.00000 -1.20000 AFIX 55 C19 1 0.888450 0.803976 0.753272 11.00000 0.06073 C18 1 0.809158 0.696926 0.717817 11.00000 0.05201 C22 1 0.783754 0.688238 0.644969 11.00000 0.04451 AFIX 43 H22 2 0.734172 0.626750 0.609714 11.00000 -1.20000 AFIX 0 C23 1 0.740045 0.608369 0.751972 11.00000 0.04510 C24 1 0.633611 0.650857 0.775306 11.00000 0.06046 AFIX 137 H24A 2 0.656869 0.714058 0.818684 11.00000 -1.50000 H24B 2 0.579018 0.589710 0.783066 11.00000 -1.50000 H24C 2 0.596576 0.676098 0.739157 11.00000 -1.50000 AFIX 0 C25 1 0.807921 0.569139 0.796051 11.00000 0.06883 AFIX 137 H25A 2 0.866282 0.535909 0.771282 11.00000 -1.50000 H25B 2 0.758598 0.511864 0.810344 11.00000 -1.50000 H25C 2 0.846344 0.632212 0.837349 11.00000 -1.50000 AFIX 0 C26 1 0.681855 0.493597 0.687264 11.00000 0.05848 AFIX 137 H26A 2 0.633865 0.512565 0.652243 11.00000 -1.50000 H26B 2 0.633830 0.439666 0.704687 11.00000 -1.50000 H26C 2 0.743067 0.459914 0.666160 11.00000 -1.50000 AFIX 0 C27 1 0.954035 0.854313 0.820212 11.00000 0.04361 C28 1 0.879400 0.870651 0.882039 11.00000 0.07209 AFIX 137 H28A 2 0.827214 0.920555 0.877095 11.00000 -1.50000 H28B 2 0.931086 0.904252 0.926743 11.00000 -1.50000 H28C 2 0.833974 0.797202 0.880325 11.00000 -1.50000 AFIX 0 C29 1 1.026547 0.981822 0.840718 11.00000 0.07077 AFIX 137 H29A 2 1.082764 0.986402 0.808863 11.00000 -1.50000 H29B 2 1.067348 1.005026 0.888570 11.00000 -1.50000 H29C 2 0.973775 1.031844 0.837234 11.00000 -1.50000 AFIX 0 C30 1 1.054598 0.791255 0.840696 11.00000 0.06362 AFIX 137 H30A 2 1.020737 0.711427 0.832572 11.00000 -1.50000 H30B 2 1.087891 0.827013 0.889934 11.00000 -1.50000 H30C 2 1.115350 0.797588 0.811840 11.00000 -1.50000 AFIX 0 C31 1 0.865964 0.808762 0.563726 11.00000 0.04802 C32 1 0.824901 0.915419 0.560637 11.00000 0.12125 AFIX 137 H32A 2 0.759769 0.895207 0.522731 11.00000 -1.50000 H32B 2 0.888389 0.968273 0.552266 11.00000 -1.50000 H32C 2 0.800292 0.950964 0.604937 11.00000 -1.50000 AFIX 0 C33 1 0.815783 0.703935 0.505553 11.00000 0.12281 AFIX 137 H33A 2 0.795682 0.641017 0.524119 11.00000 -1.50000 H33B 2 0.872374 0.688004 0.474009 11.00000 -1.50000 H33C 2 0.746083 0.713406 0.480033 11.00000 -1.50000 AFIX 0 C34 1 0.998470 0.834992 0.560472 11.00000 0.13401 AFIX 137 H34A 2 1.033101 0.912322 0.590068 11.00000 -1.50000 H34B 2 1.010157 0.827027 0.512306 11.00000 -1.50000 H34C 2 1.035139 0.782057 0.577003 11.00000 -1.50000 AFIX 0 F1 5 0.777054 0.387300 0.244949 11.00000 0.05980 F2 5 0.921438 0.351477 0.347413 11.00000 0.07378 F3 5 1.093660 0.523381 0.432308 11.00000 0.09770 F4 5 1.137006 0.735302 0.412809 11.00000 0.08903 F5 5 1.004274 0.770690 0.307025 11.00000 0.06319 F6 5 0.843021 0.882566 0.246634 11.00000 0.06503 F7 5 0.745520 1.018822 0.342995 11.00000 0.06933 F8 5 0.601338 0.929752 0.422218 11.00000 0.07766 F9 5 0.545156 0.701358 0.399889 11.00000 0.07658 F10 5 0.633058 0.560072 0.299798 11.00000 0.05455 F11 5 1.051067 0.604304 0.175903 11.00000 0.06009 F12 5 1.132093 0.648102 0.066332 11.00000 0.08969 F13 5 1.006135 0.736639 -0.020270 11.00000 0.11889 F14 5 0.793337 0.782557 0.012698 11.00000 0.07844 F15 5 0.704508 0.730646 0.119243 11.00000 0.05579 F16 5 0.530164 0.591216 0.170964 11.00000 0.05460 F17 5 0.397997 0.430116 0.061249 11.00000 0.08256 F18 5 0.484386 0.252142 -0.019162 11.00000 0.09854 F19 5 0.714819 0.246005 0.012020 11.00000 0.06610 F20 5 0.854397 0.411402 0.119461 11.00000 0.05159 AFIX 66 C35 1 0.888347 0.584375 0.273125 11.00000 0.05105 C40 1 0.979966 0.670983 0.317094 11.00000 0.04659 C39 1 1.049943 0.649494 0.370261 11.00000 0.06055 C38 1 1.028301 0.541397 0.379462 11.00000 0.06455 C37 1 0.936683 0.454787 0.335494 11.00000 0.05285 C36 1 0.866705 0.476275 0.282326 11.00000 0.04606 AFIX 66 C41 1 0.739624 0.713331 0.269169 11.00000 0.04435 C42 1 0.767621 0.831037 0.279366 11.00000 0.05108 C43 1 0.720753 0.905765 0.330466 11.00000 0.04878 C44 1 0.645888 0.862787 0.371369 11.00000 0.06560 C45 1 0.617890 0.745081 0.361172 11.00000 0.05814 C46 1 0.664757 0.670352 0.310072 11.00000 0.04567 AFIX 66 C47 1 0.870096 0.664804 0.150693 11.00000 0.04966 C48 1 0.979819 0.643017 0.136824 11.00000 0.04311 C49 1 1.025730 0.666762 0.079470 11.00000 0.05662 C50 1 0.961918 0.712295 0.035985 11.00000 0.08020 C51 1 0.852196 0.734083 0.049853 11.00000 0.05023 C52 1 0.806283 0.710338 0.107206 11.00000 0.04506 AFIX 66 C53 1 0.700572 0.509575 0.151797 11.00000 0.04789 C58 1 0.746843 0.421283 0.110876 11.00000 0.04482 C57 1 0.675074 0.335206 0.053735 11.00000 0.04470 C56 1 0.557034 0.337422 0.037515 11.00000 0.07415 C55 1 0.510762 0.425714 0.078435 11.00000 0.05474 C54 1 0.582530 0.511791 0.135576 11.00000 0.04756 AFIX 0 B1 3 0.800295 0.617629 0.214627 11.00000 0.04687 HKLF 4 REM dy60_hp1a_38deg_a.res in P-1 REM wR2 = 0.2115, GooF = S = 1.052, Restrained GooF = 1.052 for all data REM R1 = 0.0806 for 1609 Fo > 4sig(Fo) and 0.1156 for all 2149 data REM 278 parameters refined using 36 restraints END WGHT 0.1092 29.6681 REM Highest difference peak 0.542, deepest hole -0.682, 1-sigma level 0.096 Q1 1 0.6807 0.9821 0.7185 11.00000 0.05 0.54 Q2 1 0.8148 0.9369 0.7231 11.00000 0.05 0.53 Q3 1 0.7034 0.9944 0.7486 11.00000 0.05 0.51 Q4 1 0.6741 0.7009 0.7020 11.00000 0.05 0.51 Q5 1 0.6977 0.7218 0.7316 11.00000 0.05 0.47 Q6 1 0.3801 0.6035 0.6164 11.00000 0.05 0.46 Q7 1 0.7638 0.8429 0.7603 11.00000 0.05 0.45 Q8 1 0.6613 0.9624 0.6852 11.00000 0.05 0.45 Q9 1 0.7726 0.8534 0.7883 11.00000 0.05 0.42 Q10 1 0.5531 0.7709 0.7462 11.00000 0.05 0.41 Q11 1 1.0368 0.5334 0.1479 11.00000 0.05 0.40 Q12 1 1.0263 0.5209 0.1199 11.00000 0.05 0.39 Q13 1 0.4152 0.5810 0.5573 11.00000 0.05 0.39 Q14 1 1.0966 0.5813 0.0440 11.00000 0.05 0.38 Q15 1 0.2973 0.7185 0.6011 11.00000 0.05 0.34 Q16 1 0.4646 1.0806 0.6909 11.00000 0.05 0.34 Q17 1 0.6007 0.8399 0.6643 11.00000 0.05 0.33 Q18 1 0.6161 0.9674 0.7801 11.00000 0.05 0.32 Q19 1 0.5585 0.9365 0.3355 11.00000 0.05 0.31 Q20 1 0.2793 0.7050 0.5655 11.00000 0.05 0.31 ; _shelx_res_checksum 7958 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.310 _oxdiff_exptl_absorpt_empirical_full_min 0.869 # start Validation Reply Form _vrf_THETM01_dy60_hp1 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_PLAT029_dy60_hp1 ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.383 Why? RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_PLAT201_dy60_hp1 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 45 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT088_dy60_hp1 ; PROBLEM: Poor Data / Parameter Ratio .................... 7.73 Note RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT242_dy60_hp1 ; PROBLEM: Low 'MainMol' Ueq as Compared to Neighbors of C14 Check RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT342_dy60_hp1 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.04259 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT412_dy60_hp1 ; PROBLEM: Short Intra XH3 .. XHn H15A ..H16C . 1.70 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT911_dy60_hp1 ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.500 2185 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; # end Validation Reply Form _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_dy60_hp3 _database_code_depnum_ccdc_archive 'CCDC 2046708' loop_ _audit_author_name _audit_author_address 'Andreas M. Thiel' ;Aarhus University, Department of Chemistry Denmark ; _audit_update_record ; 2022-10-30 deposited with the CCDC. 2023-02-13 downloaded from the CCDC. ; _audit_creation_date 2020-02-27 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C34 H58 Dy, B C24 F20' _chemical_formula_sum 'C58 H58 B Dy F20' _chemical_formula_weight 1308.35 _chemical_melting_point ? _chemical_oxdiff_formula C58H58BDyF20 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5239(18) _cell_length_b 12.176(2) _cell_length_c 19.539(8) _cell_angle_alpha 106.90(3) _cell_angle_beta 95.05(3) _cell_angle_gamma 100.716(14) _cell_volume 2547.8(13) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2011 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 19.2030 _cell_measurement_theta_min 1.7940 _shelx_estimated_absorpt_T_max 0.925 _shelx_estimated_absorpt_T_min 0.713 _exptl_absorpt_coefficient_mu 1.581 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.25046 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1314 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_ambient_pressure 1010000 _diffrn_reflns_av_R_equivalents 0.2160 _diffrn_reflns_av_unetI/netI 0.1698 _diffrn_reflns_Laue_measured_fraction_full 0.371 _diffrn_reflns_Laue_measured_fraction_max 0.371 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 12263 _diffrn_reflns_point_group_measured_fraction_full 0.371 _diffrn_reflns_point_group_measured_fraction_max 0.371 _diffrn_reflns_theta_full 20.807 _diffrn_reflns_theta_max 20.807 _diffrn_reflns_theta_min 1.786 _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3590 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.371 _diffrn_measured_fraction_theta_max 0.371 _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 34.00 58.00 1.00 30.00 -- 7.60 -99.00 30.00 24 2 \w -33.00 20.00 1.00 30.00 -- 7.60 53.00 -17.00 53 3 \w -36.00 9.00 1.00 30.00 -- 7.60 81.00 -29.00 45 4 \w -35.00 14.00 1.00 30.00 -- 7.60 67.00 157.00 49 5 \w -14.00 35.00 1.00 30.00 -- -8.46 -67.00-157.00 49 6 \w -42.00 33.00 1.00 30.00 -- -8.46 13.00 -3.00 75 7 \w -35.00 -12.00 1.00 30.00 -- -8.46 77.00 150.00 23 8 \w -9.00 36.00 1.00 30.00 -- -8.46 -81.00 29.00 45 9 \w 12.00 35.00 1.00 30.00 -- 7.60 -77.00 60.00 23 10 \w 34.00 58.00 1.00 30.00 -- 7.60 -99.00-150.00 24 11 \w 34.00 58.00 1.00 30.00 -- 7.60 -99.00 0.00 24 12 \w 34.00 58.00 1.00 30.00 -- 7.60 -99.00 60.00 24 13 \w 12.00 51.00 1.00 30.00 -- 7.60 -77.00-150.00 39 14 \w 12.00 35.00 1.00 30.00 -- 7.60 -77.00 30.00 23 15 \w -35.00 -12.00 1.00 30.00 -- -8.46 77.00 120.00 23 16 \w 20.00 80.00 1.00 30.00 -- 7.60-135.00 57.00 60 17 \w -1.00 48.00 1.00 30.00 -- 7.60 -57.00-150.00 49 18 \w -20.00 5.00 1.00 30.00 -- -8.46 -53.00 17.00 25 19 \w -50.00 20.00 1.00 30.00 -- -8.46 53.00 162.00 70 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0145240000 _diffrn_orient_matrix_UB_12 -0.0156853000 _diffrn_orient_matrix_UB_13 -0.0381353000 _diffrn_orient_matrix_UB_21 -0.0316065000 _diffrn_orient_matrix_UB_22 -0.0565095000 _diffrn_orient_matrix_UB_23 -0.0011300000 _diffrn_orient_matrix_UB_31 -0.0529706000 _diffrn_orient_matrix_UB_32 0.0214396000 _diffrn_orient_matrix_UB_33 0.0041917000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1210 _reflns_number_total 1981 _reflns_odcompleteness_completeness 37.35 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 20.77 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.158 _refine_diff_density_min -1.180 _refine_diff_density_rms 0.155 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 272 _refine_ls_number_reflns 1981 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1921 _refine_ls_R_factor_gt 0.1243 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2842 _refine_ls_wR_factor_ref 0.3322 _refine_special_details ? _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. Restrained planarity C54, C55, C56, C57, C58, F16, F17, F18, F19, F20, B1, C53 with sigma of 0.1 C47, C52, C51, C50, C49, C48, F15, F14, F13, F12, F11, B1 with sigma of 0.1 C35, C36, C37, C38, C39, C40, F1, F2, F3, F4, F5, B1 with sigma of 0.1 C41, C46, C45, C44, C43, C42, F10, F9, F8, F7, F6, B1 with sigma of 0.1 3.a Me refined with riding coordinates: C15(H15A,H15B,H15C) 3.b Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C20(H20), C22(H22) 3.c Fitted pentagon refined as free rotating group: C1(C2,C3,C4,C5), C21(C20,C19,C18,C22) 3.d Fitted hexagon refined as free rotating group: C35(C40,C39,C38,C37,C36), C41(C42,C43,C44,C45,C46), C47(C48,C49,C50,C51,C52), C53(C58,C57,C56,C55,C54) 3.e Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B, H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A, H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.68715(15) 0.84719(14) 0.7211(2) 0.0504(10) Uiso 1 1 d . . . . . C1 C 0.5622(18) 0.9992(15) 0.724(2) 0.059(11) Uiso 1 1 d . . . . . C2 C 0.504(2) 0.931(2) 0.765(2) 0.034(9) Uiso 1 1 d G . . . . C3 C 0.449(2) 0.8182(19) 0.716(3) 0.058(11) Uiso 1 1 d G . . . . H3 H 0.404604 0.756418 0.728273 0.069 Uiso 1 1 calc R . . . . C4 C 0.4720(19) 0.8160(17) 0.646(2) 0.026(8) Uiso 1 1 d G . . . . C5 C 0.5421(19) 0.928(2) 0.651(2) 0.059(11) Uiso 1 1 d G . . . . H5 H 0.570032 0.950402 0.612364 0.070 Uiso 1 1 calc R . . . . C6 C 0.654(3) 1.122(3) 0.757(5) 0.041(9) Uiso 1 1 d . . . . . C7 C 0.771(3) 1.106(3) 0.781(5) 0.047(10) Uiso 1 1 d . . . . . H7A H 0.778344 1.115807 0.832093 0.071 Uiso 1 1 calc GR . . . . H7B H 0.831648 1.164320 0.772780 0.071 Uiso 1 1 calc GR . . . . H7C H 0.779238 1.029114 0.755171 0.071 Uiso 1 1 calc GR . . . . C8 C 0.609(3) 1.219(3) 0.808(5) 0.062(11) Uiso 1 1 d . . . . . H8A H 0.531783 1.221854 0.786627 0.093 Uiso 1 1 calc GR . . . . H8B H 0.663745 1.293326 0.815212 0.093 Uiso 1 1 calc GR . . . . H8C H 0.604368 1.204588 0.852979 0.093 Uiso 1 1 calc GR . . . . C9 C 0.679(4) 1.165(4) 0.685(6) 0.070(12) Uiso 1 1 d . . . . . H9A H 0.690997 1.099686 0.646746 0.105 Uiso 1 1 calc GR . . . . H9B H 0.749340 1.227447 0.697790 0.105 Uiso 1 1 calc GR . . . . H9C H 0.611828 1.192112 0.669346 0.105 Uiso 1 1 calc GR . . . . C10 C 0.478(3) 0.955(3) 0.849(5) 0.033(8) Uiso 1 1 d . . . . . C11 C 0.581(3) 1.007(3) 0.890(5) 0.041(9) Uiso 1 1 d . . . . . H11A H 0.625354 0.948353 0.893076 0.061 Uiso 1 1 calc GR . . . . H11B H 0.567127 1.047125 0.938024 0.061 Uiso 1 1 calc GR . . . . H11C H 0.625029 1.061924 0.870665 0.061 Uiso 1 1 calc GR . . . . C12 C 0.413(4) 0.840(3) 0.856(6) 0.071(12) Uiso 1 1 d . . . . . H12A H 0.336512 0.814887 0.825745 0.106 Uiso 1 1 calc GR . . . . H12B H 0.401608 0.851225 0.905515 0.106 Uiso 1 1 calc GR . . . . H12C H 0.458928 0.781600 0.841477 0.106 Uiso 1 1 calc GR . . . . C13 C 0.382(3) 1.032(3) 0.856(4) 0.046(9) Uiso 1 1 d . . . . . H13A H 0.404493 1.094068 0.835378 0.069 Uiso 1 1 calc GR . . . . H13B H 0.376467 1.066172 0.906402 0.069 Uiso 1 1 calc GR . . . . H13C H 0.305734 0.983755 0.831214 0.069 Uiso 1 1 calc GR . . . . C14 C 0.423(3) 0.719(3) 0.582(5) 0.049(10) Uiso 1 1 d . . . . . C15 C 0.509(5) 0.653(5) 0.549(7) 0.13(2) Uiso 1 1 d . . . . . H15A H 0.468037 0.589750 0.506854 0.194 Uiso 1 1 calc R . . . . H15B H 0.569242 0.704837 0.535063 0.194 Uiso 1 1 calc R . . . . H15C H 0.545502 0.622012 0.582937 0.194 Uiso 1 1 calc R . . . . C16 C 0.372(4) 0.773(4) 0.516(6) 0.072(13) Uiso 1 1 d . . . . . H16A H 0.335260 0.836765 0.536931 0.109 Uiso 1 1 calc GR . . . . H16B H 0.314329 0.711387 0.479879 0.109 Uiso 1 1 calc GR . . . . H16C H 0.437713 0.800343 0.493668 0.109 Uiso 1 1 calc GR . . . . C17 C 0.314(5) 0.632(5) 0.581(7) 0.113(18) Uiso 1 1 d . . . . . H17A H 0.302358 0.635704 0.629739 0.170 Uiso 1 1 calc GR . . . . H17B H 0.321700 0.554098 0.555170 0.170 Uiso 1 1 calc GR . . . . H17C H 0.245891 0.649154 0.557449 0.170 Uiso 1 1 calc GR . . . . C21 C 0.854(3) 0.801(3) 0.635(3) 0.055(11) Uiso 1 1 d . . . . . C20 C 0.9166(18) 0.8708(14) 0.704(3) 0.048(11) Uiso 1 1 d G . . . . H20 H 0.964918 0.945887 0.715598 0.058 Uiso 1 1 calc R . . . . C19 C 0.892(2) 0.806(2) 0.753(3) 0.045(10) Uiso 1 1 d G . . . . C18 C 0.815(2) 0.6961(18) 0.714(3) 0.028(9) Uiso 1 1 d G . . . . C22 C 0.791(2) 0.6929(19) 0.641(3) 0.051(12) Uiso 1 1 d G . . . . H22 H 0.743141 0.630877 0.603146 0.062 Uiso 1 1 calc R . . . . C23 C 0.740(3) 0.609(3) 0.751(5) 0.043(10) Uiso 1 1 d . . . . . C24 C 0.636(4) 0.660(4) 0.782(5) 0.071(12) Uiso 1 1 d . . . . . H24A H 0.639486 0.661907 0.832027 0.107 Uiso 1 1 calc GR . . . . H24B H 0.561417 0.610451 0.755274 0.107 Uiso 1 1 calc GR . . . . H24C H 0.642223 0.737913 0.779503 0.107 Uiso 1 1 calc GR . . . . C25 C 0.812(3) 0.571(3) 0.802(5) 0.057(11) Uiso 1 1 d . . . . . H25A H 0.890230 0.570136 0.788176 0.085 Uiso 1 1 calc GR . . . . H25B H 0.773733 0.493263 0.800525 0.085 Uiso 1 1 calc GR . . . . H25C H 0.819500 0.624433 0.849708 0.085 Uiso 1 1 calc GR . . . . C26 C 0.684(4) 0.487(3) 0.678(6) 0.076(13) Uiso 1 1 d . . . . . H26A H 0.643071 0.508114 0.640634 0.114 Uiso 1 1 calc GR . . . . H26B H 0.628475 0.431491 0.692710 0.114 Uiso 1 1 calc GR . . . . H26C H 0.747630 0.451601 0.660518 0.114 Uiso 1 1 calc GR . . . . C27 C 0.959(3) 0.868(3) 0.832(5) 0.033(9) Uiso 1 1 d . . . . . C28 C 0.881(4) 0.878(4) 0.888(6) 0.077(13) Uiso 1 1 d . . . . . H28A H 0.826724 0.926005 0.881331 0.116 Uiso 1 1 calc GR . . . . H28B H 0.928507 0.912652 0.935057 0.116 Uiso 1 1 calc GR . . . . H28C H 0.836267 0.800730 0.884448 0.116 Uiso 1 1 calc GR . . . . C29 C 1.032(4) 0.990(3) 0.842(5) 0.071(12) Uiso 1 1 d . . . . . H29A H 1.097848 0.983220 0.814928 0.107 Uiso 1 1 calc GR . . . . H29B H 1.062612 1.028952 0.892200 0.107 Uiso 1 1 calc GR . . . . H29C H 0.982918 1.034280 0.824458 0.107 Uiso 1 1 calc GR . . . . C30 C 1.066(4) 0.805(4) 0.857(6) 0.072(12) Uiso 1 1 d . . . . . H30A H 1.030139 0.732448 0.864687 0.108 Uiso 1 1 calc GR . . . . H30B H 1.114219 0.857201 0.901411 0.108 Uiso 1 1 calc GR . . . . H30C H 1.115322 0.789386 0.819971 0.108 Uiso 1 1 calc GR . . . . C31 C 0.875(3) 0.825(3) 0.563(5) 0.047(10) Uiso 1 1 d . . . . . C32 C 0.814(4) 0.918(4) 0.559(5) 0.070(12) Uiso 1 1 d . . . . . H32A H 0.747323 0.913951 0.585274 0.105 Uiso 1 1 calc GR . . . . H32B H 0.786812 0.907774 0.509734 0.105 Uiso 1 1 calc GR . . . . H32C H 0.868560 0.992987 0.580720 0.105 Uiso 1 1 calc GR . . . . C33 C 0.845(4) 0.720(4) 0.517(6) 0.079(13) Uiso 1 1 d . . . . . H33A H 0.911867 0.683948 0.514694 0.118 Uiso 1 1 calc GR . . . . H33B H 0.819411 0.725797 0.469907 0.118 Uiso 1 1 calc GR . . . . H33C H 0.780270 0.674086 0.531122 0.118 Uiso 1 1 calc GR . . . . C34 C 1.005(3) 0.859(3) 0.550(6) 0.063(11) Uiso 1 1 d . . . . . H34A H 1.052452 0.915432 0.592751 0.095 Uiso 1 1 calc GR . . . . H34B H 1.005753 0.893346 0.511015 0.095 Uiso 1 1 calc GR . . . . H34C H 1.037545 0.790258 0.536430 0.095 Uiso 1 1 calc GR . . . . F1 F 0.7835(17) 0.3882(16) 0.255(3) 0.063(6) Uiso 1 1 d . . . . . F2 F 0.9325(18) 0.3529(17) 0.353(3) 0.069(6) Uiso 1 1 d . . . . . F3 F 1.102(2) 0.530(2) 0.440(3) 0.096(8) Uiso 1 1 d . . . . . F4 F 1.139(2) 0.746(2) 0.414(3) 0.092(7) Uiso 1 1 d . . . . . F5 F 1.0043(15) 0.7805(15) 0.314(2) 0.048(5) Uiso 1 1 d . . . . . F6 F 0.8369(17) 0.8896(17) 0.252(2) 0.061(6) Uiso 1 1 d . . . . . F7 F 0.7333(16) 1.0271(15) 0.348(2) 0.057(5) Uiso 1 1 d . . . . . F8 F 0.5890(18) 0.9383(17) 0.428(3) 0.073(6) Uiso 1 1 d . . . . . F9 F 0.533(2) 0.6988(19) 0.403(3) 0.086(7) Uiso 1 1 d . . . . . F10 F 0.6304(15) 0.5592(15) 0.307(2) 0.050(5) Uiso 1 1 d . . . . . F11 F 1.0521(15) 0.6088(15) 0.182(2) 0.046(5) Uiso 1 1 d . . . . . F12 F 1.129(2) 0.6320(19) 0.064(3) 0.089(7) Uiso 1 1 d . . . . . F13 F 0.995(2) 0.712(2) -0.026(3) 0.098(8) Uiso 1 1 d . . . . . F14 F 0.7846(17) 0.7720(17) 0.007(3) 0.064(6) Uiso 1 1 d . . . . . F15 F 0.6985(17) 0.7318(16) 0.119(3) 0.060(6) Uiso 1 1 d . . . . . F16 F 0.5299(16) 0.5937(15) 0.177(2) 0.051(5) Uiso 1 1 d . . . . . F17 F 0.4002(18) 0.4371(18) 0.060(3) 0.075(7) Uiso 1 1 d . . . . . F18 F 0.492(2) 0.259(2) -0.029(3) 0.102(8) Uiso 1 1 d . . . . . F19 F 0.7225(18) 0.2523(17) 0.013(3) 0.066(6) Uiso 1 1 d . . . . . F20 F 0.8587(16) 0.4135(15) 0.125(2) 0.048(5) Uiso 1 1 d . . . . . C35 C 0.891(2) 0.589(2) 0.280(2) 0.046(9) Uiso 1 1 d . . . . . C40 C 0.984(2) 0.6785(15) 0.324(2) 0.061(11) Uiso 1 1 d G . . . . C39 C 1.0558(19) 0.657(2) 0.378(2) 0.076(13) Uiso 1 1 d G . . . . C38 C 1.035(2) 0.547(3) 0.387(2) 0.071(13) Uiso 1 1 d G . . . . C37 C 0.942(2) 0.4575(18) 0.343(2) 0.088(15) Uiso 1 1 d G . . . . C36 C 0.870(2) 0.4788(17) 0.289(2) 0.067(12) Uiso 1 1 d G . . . . C41 C 0.7353(17) 0.7155(15) 0.2745(18) 0.034(8) Uiso 1 1 d . . . . . C42 C 0.7599(17) 0.8359(16) 0.2851(18) 0.040(9) Uiso 1 1 d G . . . . C43 C 0.7083(19) 0.9091(12) 0.3362(19) 0.057(11) Uiso 1 1 d G . . . . C44 C 0.6320(18) 0.8619(17) 0.3768(17) 0.059(11) Uiso 1 1 d G . . . . C45 C 0.6073(17) 0.7415(18) 0.3662(18) 0.052(10) Uiso 1 1 d G . . . . C46 C 0.6589(18) 0.6683(13) 0.3151(19) 0.043(9) Uiso 1 1 d G . . . . C47 C 0.8673(19) 0.6681(16) 0.1523(19) 0.045(10) Uiso 1 1 d . . . . . C48 C 0.9774(17) 0.6436(15) 0.1379(19) 0.037(9) Uiso 1 1 d G . . . . C49 C 1.0215(15) 0.6592(16) 0.077(2) 0.034(9) Uiso 1 1 d G . . . . C50 C 0.955(2) 0.6992(16) 0.0297(18) 0.066(13) Uiso 1 1 d G . . . . C51 C 0.8453(18) 0.7236(16) 0.0440(19) 0.032(8) Uiso 1 1 d G . . . . C52 C 0.8012(14) 0.7081(16) 0.105(2) 0.040(9) Uiso 1 1 d G . . . . C53 C 0.7034(19) 0.5083(16) 0.1530(19) 0.042(9) Uiso 1 1 d . . . . . C58 C 0.7481(15) 0.4184(19) 0.110(2) 0.047(10) Uiso 1 1 d G . . . . C57 C 0.675(2) 0.3347(16) 0.0497(19) 0.041(9) Uiso 1 1 d G . . . . C56 C 0.5568(19) 0.3410(18) 0.0334(19) 0.066(12) Uiso 1 1 d G . . . . C55 C 0.5122(15) 0.431(2) 0.077(2) 0.042(9) Uiso 1 1 d G . . . . C54 C 0.585(2) 0.5146(17) 0.137(2) 0.069(12) Uiso 1 1 d G . . . . B1 B 0.799(3) 0.623(3) 0.224(3) 0.049(12) Uiso 1 1 d . . . . . _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 2.54(2) . ? Dy1 C2 2.61(2) . ? Dy1 C3 2.69(2) . ? Dy1 C4 2.67(3) . ? Dy1 C5 2.58(3) . ? Dy1 C21 2.70(3) . ? Dy1 C20 2.667(19) . ? Dy1 C19 2.57(3) . ? Dy1 C18 2.543(19) . ? Dy1 C22 2.63(3) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 C6 1.58(5) . ? C2 C3 1.4200 . ? C2 C10 1.65(9) . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C4 C14 1.42(8) . ? C6 C7 1.45(6) . ? C6 C8 1.51(7) . ? C6 C9 1.66(11) . ? C10 C11 1.30(7) . ? C10 C12 1.51(4) . ? C10 C13 1.57(4) . ? C14 C15 1.46(7) . ? C14 C16 1.72(11) . ? C14 C17 1.48(5) . ? C21 C20 1.4200 . ? C21 C22 1.4200 . ? C21 C31 1.53(8) . ? C20 C19 1.4200 . ? C19 C18 1.4200 . ? C19 C27 1.57(9) . ? C18 C22 1.4200 . ? C18 C23 1.61(6) . ? C23 C24 1.55(5) . ? C23 C25 1.47(9) . ? C23 C26 1.70(11) . ? C27 C28 1.46(9) . ? C27 C29 1.52(4) . ? C27 C30 1.67(6) . ? C31 C32 1.45(4) . ? C31 C33 1.30(9) . ? C31 C34 1.55(4) . ? F1 C36 1.30(3) . ? F2 C37 1.33(3) . ? F3 C38 1.33(5) . ? F4 C39 1.28(4) . ? F5 C40 1.29(2) . ? F6 C42 1.32(3) . ? F7 C43 1.36(2) . ? F8 C44 1.36(4) . ? F9 C45 1.29(4) . ? F10 C46 1.267(19) . ? F11 C48 1.36(4) . ? F12 C49 1.36(2) . ? F13 C50 1.26(6) . ? F14 C51 1.30(4) . ? F15 C52 1.30(2) . ? F16 C54 1.35(3) . ? F17 C55 1.32(3) . ? F18 C56 1.38(5) . ? F19 C57 1.30(3) . ? F20 C58 1.30(3) . ? C35 C40 1.3900 . ? C35 C36 1.3900 . ? C35 B1 1.65(6) . ? C40 C39 1.3900 . ? C39 C38 1.3900 . ? C38 C37 1.3900 . ? C37 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 B1 1.61(4) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C47 B1 1.83(6) . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C53 C58 1.3900 . ? C53 C54 1.3900 . ? C53 B1 1.77(5) . ? C58 C57 1.3900 . ? C57 C56 1.3900 . ? C56 C55 1.3900 . ? C55 C54 1.3900 . ? 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 C1 Dy1 C2 32.0(2) . . ? C1 Dy1 C3 52.0(3) . . ? C1 Dy1 C4 52.2(4) . . ? C1 Dy1 C5 32.2(3) . . ? C1 Dy1 C21 126.1(11) . . ? C1 Dy1 C20 126.3(7) . . ? C1 Dy1 C19 147.6(8) . . ? C1 Dy1 C18 177.9(13) . . ? C1 Dy1 C22 146.3(15) . . ? C2 Dy1 C3 31.0(2) . . ? C2 Dy1 C4 51.5(3) . . ? C2 Dy1 C21 156.5(11) . . ? C2 Dy1 C20 152.5(8) . . ? C2 Dy1 C22 154.8(10) . . ? C3 Dy1 C21 141.2(14) . . ? C4 Dy1 C3 30.7(2) . . ? C4 Dy1 C21 112.3(13) . . ? C5 Dy1 C2 52.5(3) . . ? C5 Dy1 C3 51.6(3) . . ? C5 Dy1 C4 31.3(3) . . ? C5 Dy1 C21 104.4(11) . . ? C5 Dy1 C20 121.5(11) . . ? C5 Dy1 C22 115.2(13) . . ? C20 Dy1 C3 171.1(15) . . ? C20 Dy1 C4 140.5(15) . . ? C20 Dy1 C21 30.7(3) . . ? C19 Dy1 C2 148.7(13) . . ? C19 Dy1 C3 154.9(10) . . ? C19 Dy1 C4 157.9(10) . . ? C19 Dy1 C5 152.9(11) . . ? C19 Dy1 C21 51.6(3) . . ? C19 Dy1 C20 31.4(2) . . ? C19 Dy1 C22 52.5(2) . . ? C18 Dy1 C2 150.0(10) . . ? C18 Dy1 C3 129.1(6) . . ? C18 Dy1 C4 127.4(10) . . ? C18 Dy1 C5 146.3(14) . . ? C18 Dy1 C21 51.9(3) . . ? C18 Dy1 C20 52.3(3) . . ? C18 Dy1 C19 32.3(3) . . ? C18 Dy1 C22 31.8(2) . . ? C22 Dy1 C3 123.9(9) . . ? C22 Dy1 C4 105.6(11) . . ? C22 Dy1 C21 30.9(3) . . ? C22 Dy1 C20 51.4(3) . . ? C2 C1 Dy1 76.9(10) . . ? C2 C1 C5 108.0 . . ? C2 C1 C6 126(4) . . ? C5 C1 Dy1 75.4(11) . . ? C5 C1 C6 125(4) . . ? C6 C1 Dy1 104.7(16) . . ? C1 C2 Dy1 71.2(9) . . ? C1 C2 C3 108.0 . . ? C1 C2 C10 136(2) . . ? C3 C2 Dy1 77.7(9) . . ? C3 C2 C10 115(2) . . ? C10 C2 Dy1 122(2) . . ? C2 C3 Dy1 71.3(9) . . ? C2 C3 C4 108.0 . . ? C4 C3 Dy1 73.9(11) . . ? C3 C4 Dy1 75.5(10) . . ? C3 C4 C14 124(3) . . ? C5 C4 Dy1 70.6(8) . . ? C5 C4 C3 108.0 . . ? C5 C4 C14 128(3) . . ? C14 C4 Dy1 123.4(19) . . ? C1 C5 Dy1 72.4(10) . . ? C4 C5 Dy1 78.1(8) . . ? C4 C5 C1 108.0 . . ? C1 C6 C9 104(6) . . ? C7 C6 C1 111(2) . . ? C7 C6 C8 116(6) . . ? C7 C6 C9 102(4) . . ? C8 C6 C1 116(3) . . ? C8 C6 C9 106(4) . . ? C11 C10 C2 107(4) . . ? C11 C10 C12 118(6) . . ? C11 C10 C13 115(4) . . ? C12 C10 C2 108(5) . . ? C12 C10 C13 104(3) . . ? C13 C10 C2 105(5) . . ? C4 C14 C15 115(5) . . ? C4 C14 C16 108(3) . . ? C4 C14 C17 121(7) . . ? C15 C14 C16 103(7) . . ? C15 C14 C17 108(4) . . ? C17 C14 C16 99(5) . . ? C20 C21 Dy1 73.3(11) . . ? C20 C21 C31 125(3) . . ? C22 C21 Dy1 71.7(6) . . ? C22 C21 C20 108.0 . . ? C22 C21 C31 125(3) . . ? C31 C21 Dy1 132(2) . . ? C21 C20 Dy1 76.0(12) . . ? C21 C20 C19 108.0 . . ? C19 C20 Dy1 70.5(11) . . ? C20 C19 Dy1 78.1(11) . . ? C20 C19 C18 108.0 . . ? C20 C19 C27 115(3) . . ? C18 C19 Dy1 72.9(7) . . ? C18 C19 C27 137(3) . . ? C27 C19 Dy1 118(2) . . ? C19 C18 Dy1 74.9(9) . . ? C19 C18 C23 124(4) . . ? C22 C18 Dy1 77.3(14) . . ? C22 C18 C19 108.0 . . ? C22 C18 C23 126(4) . . ? C23 C18 Dy1 101.4(14) . . ? C21 C22 Dy1 77.5(8) . . ? C21 C22 C18 108.0 . . ? C18 C22 Dy1 70.8(13) . . ? C18 C23 C26 102(5) . . ? C24 C23 C18 111(3) . . ? C24 C23 C26 109(4) . . ? C25 C23 C18 115(3) . . ? C25 C23 C24 113(6) . . ? C25 C23 C26 106(4) . . ? C19 C27 C30 115(5) . . ? C28 C27 C19 115(4) . . ? C28 C27 C29 108(5) . . ? C28 C27 C30 106(6) . . ? C29 C27 C19 112(6) . . ? C29 C27 C30 100(3) . . ? C21 C31 C34 119(6) . . ? C32 C31 C21 107(5) . . ? C32 C31 C34 109(3) . . ? C33 C31 C21 102(5) . . ? C33 C31 C32 122(7) . . ? C33 C31 C34 99(5) . . ? C40 C35 C36 120.0 . . ? C40 C35 B1 118(2) . . ? C36 C35 B1 122(2) . . ? F5 C40 C35 120(3) . . ? F5 C40 C39 120(3) . . ? C39 C40 C35 120.0 . . ? F4 C39 C40 114(3) . . ? F4 C39 C38 126(3) . . ? C40 C39 C38 120.0 . . ? F3 C38 C39 119(2) . . ? F3 C38 C37 121(2) . . ? C37 C38 C39 120.0 . . ? F2 C37 C38 116(3) . . ? F2 C37 C36 124(3) . . ? C38 C37 C36 120.0 . . ? F1 C36 C35 127(3) . . ? F1 C36 C37 112(3) . . ? C37 C36 C35 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 B1 125.0(17) . . ? C46 C41 B1 114.7(17) . . ? F6 C42 C41 124.3(16) . . ? F6 C42 C43 115.6(16) . . ? C41 C42 C43 120.0 . . ? F7 C43 C42 120.7(19) . . ? F7 C43 C44 119.3(19) . . ? C44 C43 C42 120.0 . . ? F8 C44 C43 117.3(18) . . ? F8 C44 C45 122.6(18) . . ? C43 C44 C45 120.0 . . ? F9 C45 C44 119.1(18) . . ? F9 C45 C46 120.8(19) . . ? C46 C45 C44 120.0 . . ? F10 C46 C41 123(2) . . ? F10 C46 C45 117(2) . . ? C45 C46 C41 120.0 . . ? C48 C47 C52 120.0 . . ? C48 C47 B1 119.1(18) . . ? C52 C47 B1 120.0(18) . . ? F11 C48 C47 125(2) . . ? F11 C48 C49 115(2) . . ? C47 C48 C49 120.0 . . ? F12 C49 C48 118(3) . . ? F12 C49 C50 122(3) . . ? C50 C49 C48 120.0 . . ? F13 C50 C49 120(2) . . ? F13 C50 C51 120(2) . . ? C51 C50 C49 120.0 . . ? F14 C51 C50 123(2) . . ? F14 C51 C52 116(2) . . ? C50 C51 C52 120.0 . . ? F15 C52 C47 120(3) . . ? F15 C52 C51 120(3) . . ? C51 C52 C47 120.0 . . ? C58 C53 C54 120.0 . . ? C58 C53 B1 120.4(17) . . ? C54 C53 B1 119.3(17) . . ? F20 C58 C53 120(2) . . ? F20 C58 C57 120(2) . . ? C53 C58 C57 120.0 . . ? F19 C57 C58 116(2) . . ? F19 C57 C56 124(2) . . ? C56 C57 C58 120.0 . . ? F18 C56 C57 116.5(19) . . ? F18 C56 C55 123.4(19) . . ? C57 C56 C55 120.0 . . ? F17 C55 C56 120(2) . . ? F17 C55 C54 120(2) . . ? C54 C55 C56 120.0 . . ? F16 C54 C53 126(2) . . ? F16 C54 C55 114(2) . . ? C55 C54 C53 120.0 . . ? C35 B1 C47 115(2) . . ? C35 B1 C53 119(2) . . ? C41 B1 C35 105(3) . . ? C41 B1 C47 116(2) . . ? C41 B1 C53 116(2) . . ? C53 B1 C47 86(2) . . ? _shelx_res_file ; TITL dy60_hp3_38deg_a.res in P-1 dy60_hp3_38deg.res created by SHELXL-2018/3 at 12:46:02 on 27-Feb-2020 REM Old TITL Dy60_HP3_38deg in P-1 REM SHELXT solution in P-1: R1 0.207, Rweak 0.068, Alpha 0.110 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C51 B3 F27 Dy CELL 0.71073 11.5239 12.1757 19.5387 106.899 95.049 100.716 ZERR 2 0.0018 0.0023 0.0078 0.028 0.025 0.014 LATT 1 SFAC C H B Dy F UNIT 116 116 2 2 40 FLAT C54 C55 C56 C57 C58 F16 F17 F18 F19 F20 B1 C53 FLAT C47 C52 C51 C50 C49 C48 F15 F14 F13 F12 F11 B1 FLAT C35 C36 C37 C38 C39 C40 F1 F2 F3 F4 F5 B1 FLAT C41 C46 C45 C44 C43 C42 F10 F9 F8 F7 F6 B1 L.S. 20 0 0 PLAN 20 SIZE 0.16 0.23 0.05 FREE Dy1 C24 FREE Dy1 C7 list 4 fmap 2 53 acta SHEL 100 0.83 OMIT 0 180 OMIT 4 -5 1 OMIT 1 -6 3 OMIT 6 -8 4 OMIT -7 -6 6 OMIT 1 -11 2 OMIT 10 0 0 OMIT -10 3 2 OMIT 8 -5 3 OMIT 9 -6 2 OMIT -5 -6 6 OMIT 4 -8 7 OMIT -6 -5 4 OMIT -8 -4 4 REM REM REM WGHT 0.200000 FVAR 0.35599 DY1 4 0.687150 0.847188 0.721060 11.00000 0.05041 AFIX 56 C1 1 0.562185 0.999183 0.724172 11.00000 0.05859 C2 1 0.504419 0.931446 0.764646 11.00000 0.03409 C3 1 0.448653 0.818244 0.716063 11.00000 0.05766 AFIX 43 H3 2 0.404604 0.756418 0.728273 11.00000 -1.20000 AFIX 55 C4 1 0.471953 0.816018 0.645563 11.00000 0.02553 C5 1 0.542120 0.927845 0.650574 11.00000 0.05855 AFIX 43 H5 2 0.570032 0.950402 0.612364 11.00000 -1.20000 AFIX 0 C6 1 0.654081 1.121950 0.756823 11.00000 0.04058 C7 1 0.770679 1.106492 0.781283 11.00000 0.04715 AFIX 137 H7A 2 0.778344 1.115807 0.832093 11.00000 -1.50000 H7B 2 0.831648 1.164320 0.772780 11.00000 -1.50000 H7C 2 0.779238 1.029114 0.755171 11.00000 -1.50000 AFIX 0 C8 1 0.609418 1.219315 0.807539 11.00000 0.06204 AFIX 137 H8A 2 0.531783 1.221854 0.786627 11.00000 -1.50000 H8B 2 0.663745 1.293326 0.815212 11.00000 -1.50000 H8C 2 0.604368 1.204588 0.852979 11.00000 -1.50000 AFIX 0 C9 1 0.679214 1.164824 0.685107 11.00000 0.07009 AFIX 137 H9A 2 0.690997 1.099686 0.646746 11.00000 -1.50000 H9B 2 0.749340 1.227447 0.697790 11.00000 -1.50000 H9C 2 0.611828 1.192112 0.669346 11.00000 -1.50000 AFIX 0 C10 1 0.478464 0.955307 0.848907 11.00000 0.03296 C11 1 0.580736 1.006556 0.890404 11.00000 0.04052 AFIX 137 H11A 2 0.625354 0.948353 0.893076 11.00000 -1.50000 H11B 2 0.567127 1.047125 0.938024 11.00000 -1.50000 H11C 2 0.625029 1.061924 0.870665 11.00000 -1.50000 AFIX 0 C12 1 0.412876 0.840224 0.856066 11.00000 0.07084 AFIX 137 H12A 2 0.336512 0.814887 0.825745 11.00000 -1.50000 H12B 2 0.401608 0.851225 0.905515 11.00000 -1.50000 H12C 2 0.458928 0.781600 0.841477 11.00000 -1.50000 AFIX 0 C13 1 0.381869 1.032338 0.856185 11.00000 0.04611 AFIX 137 H13A 2 0.404493 1.094068 0.835378 11.00000 -1.50000 H13B 2 0.376467 1.066172 0.906402 11.00000 -1.50000 H13C 2 0.305734 0.983755 0.831214 11.00000 -1.50000 AFIX 0 C14 1 0.423283 0.718872 0.582284 11.00000 0.04905 C15 1 0.508872 0.653226 0.548917 11.00000 0.12929 AFIX 33 H15A 2 0.468037 0.589750 0.506854 11.00000 -1.50000 H15B 2 0.569242 0.704837 0.535063 11.00000 -1.50000 H15C 2 0.545502 0.622012 0.582937 11.00000 -1.50000 AFIX 0 C16 1 0.371960 0.772819 0.515827 11.00000 0.07241 AFIX 137 H16A 2 0.335260 0.836765 0.536931 11.00000 -1.50000 H16B 2 0.314329 0.711387 0.479879 11.00000 -1.50000 H16C 2 0.437713 0.800343 0.493668 11.00000 -1.50000 AFIX 0 C17 1 0.313621 0.631762 0.581052 11.00000 0.11304 AFIX 137 H17A 2 0.302358 0.635704 0.629739 11.00000 -1.50000 H17B 2 0.321700 0.554098 0.555170 11.00000 -1.50000 H17C 2 0.245891 0.649154 0.557449 11.00000 -1.50000 AFIX 56 C21 1 0.854136 0.800833 0.634622 11.00000 0.05501 C20 1 0.916626 0.870834 0.704137 11.00000 0.04799 AFIX 43 H20 2 0.964918 0.945887 0.715598 11.00000 -1.20000 AFIX 55 C19 1 0.892433 0.806118 0.753080 11.00000 0.04500 C18 1 0.814991 0.696120 0.713813 11.00000 0.02797 C22 1 0.791322 0.692854 0.640602 11.00000 0.05144 AFIX 43 H22 2 0.743141 0.630877 0.603146 11.00000 -1.20000 AFIX 0 C23 1 0.740386 0.609382 0.750565 11.00000 0.04326 C24 1 0.635973 0.659685 0.782358 11.00000 0.07142 AFIX 137 H24A 2 0.639486 0.661907 0.832027 11.00000 -1.50000 H24B 2 0.561417 0.610451 0.755274 11.00000 -1.50000 H24C 2 0.642223 0.737913 0.779503 11.00000 -1.50000 AFIX 0 C25 1 0.812226 0.570953 0.801702 11.00000 0.05696 AFIX 137 H25A 2 0.890230 0.570136 0.788176 11.00000 -1.50000 H25B 2 0.773733 0.493263 0.800525 11.00000 -1.50000 H25C 2 0.819500 0.624433 0.849708 11.00000 -1.50000 AFIX 0 C26 1 0.683706 0.486769 0.678213 11.00000 0.07575 AFIX 137 H26A 2 0.643071 0.508114 0.640634 11.00000 -1.50000 H26B 2 0.628475 0.431491 0.692710 11.00000 -1.50000 H26C 2 0.747630 0.451601 0.660518 11.00000 -1.50000 AFIX 0 C27 1 0.958898 0.867675 0.832395 11.00000 0.03334 C28 1 0.880884 0.877622 0.888103 11.00000 0.07730 AFIX 137 H28A 2 0.826724 0.926005 0.881331 11.00000 -1.50000 H28B 2 0.928507 0.912652 0.935057 11.00000 -1.50000 H28C 2 0.836267 0.800730 0.884448 11.00000 -1.50000 AFIX 0 C29 1 1.032315 0.989749 0.841866 11.00000 0.07125 AFIX 137 H29A 2 1.097848 0.983220 0.814928 11.00000 -1.50000 H29B 2 1.062612 1.028952 0.892200 11.00000 -1.50000 H29C 2 0.982918 1.034280 0.824458 11.00000 -1.50000 AFIX 0 C30 1 1.066081 0.804989 0.857270 11.00000 0.07230 AFIX 137 H30A 2 1.030139 0.732448 0.864687 11.00000 -1.50000 H30B 2 1.114219 0.857201 0.901411 11.00000 -1.50000 H30C 2 1.115322 0.789386 0.819971 11.00000 -1.50000 AFIX 0 C31 1 0.875120 0.825267 0.563439 11.00000 0.04700 C32 1 0.814319 0.917809 0.559455 11.00000 0.06995 AFIX 137 H32A 2 0.747323 0.913951 0.585274 11.00000 -1.50000 H32B 2 0.786812 0.907774 0.509734 11.00000 -1.50000 H32C 2 0.868560 0.992987 0.580720 11.00000 -1.50000 AFIX 0 C33 1 0.844687 0.720455 0.516753 11.00000 0.07879 AFIX 137 H33A 2 0.911867 0.683948 0.514694 11.00000 -1.50000 H33B 2 0.819411 0.725797 0.469907 11.00000 -1.50000 H33C 2 0.780270 0.674086 0.531122 11.00000 -1.50000 AFIX 0 C34 1 1.005037 0.859303 0.549596 11.00000 0.06311 AFIX 137 H34A 2 1.052452 0.915432 0.592751 11.00000 -1.50000 H34B 2 1.005753 0.893346 0.511015 11.00000 -1.50000 H34C 2 1.037545 0.790258 0.536430 11.00000 -1.50000 AFIX 0 F1 5 0.783489 0.388249 0.255113 11.00000 0.06276 F2 5 0.932507 0.352935 0.352873 11.00000 0.06935 F3 5 1.102041 0.530268 0.440136 11.00000 0.09611 F4 5 1.138724 0.745966 0.414200 11.00000 0.09174 F5 5 1.004267 0.780484 0.314225 11.00000 0.04848 F6 5 0.836854 0.889603 0.252271 11.00000 0.06130 F7 5 0.733314 1.027072 0.348158 11.00000 0.05735 F8 5 0.589044 0.938265 0.428318 11.00000 0.07298 F9 5 0.533481 0.698814 0.402777 11.00000 0.08614 F10 5 0.630373 0.559233 0.307260 11.00000 0.05025 F11 5 1.052106 0.608801 0.181501 11.00000 0.04637 F12 5 1.128644 0.632049 0.063606 11.00000 0.08859 F13 5 0.994880 0.712390 -0.026085 11.00000 0.09844 F14 5 0.784642 0.771955 0.006741 11.00000 0.06407 F15 5 0.698480 0.731824 0.118609 11.00000 0.05967 F16 5 0.529911 0.593659 0.176922 11.00000 0.05068 F17 5 0.400189 0.437063 0.060497 11.00000 0.07497 F18 5 0.491722 0.258655 -0.028883 11.00000 0.10182 F19 5 0.722504 0.252346 0.012856 11.00000 0.06633 F20 5 0.858684 0.413548 0.124934 11.00000 0.04836 AFIX 66 C35 1 0.890631 0.589383 0.280135 11.00000 0.04569 C40 1 0.983737 0.678542 0.324216 11.00000 0.06080 C39 1 1.055830 0.657162 0.377609 11.00000 0.07585 C38 1 1.034817 0.546623 0.386923 11.00000 0.07098 C37 1 0.941711 0.457464 0.342842 11.00000 0.08800 C36 1 0.869618 0.478843 0.289448 11.00000 0.06695 AFIX 66 C41 1 0.735277 0.715475 0.274483 11.00000 0.03352 C42 1 0.759943 0.835902 0.285052 11.00000 0.04046 C43 1 0.708283 0.909131 0.336196 11.00000 0.05655 C44 1 0.631958 0.861933 0.376773 11.00000 0.05857 C45 1 0.607291 0.741506 0.366205 11.00000 0.05190 C46 1 0.658949 0.668275 0.315060 11.00000 0.04317 AFIX 66 C47 1 0.867279 0.668073 0.152295 11.00000 0.04545 C48 1 0.977392 0.643636 0.137927 11.00000 0.03715 C49 1 1.021464 0.659184 0.076615 11.00000 0.03423 C50 1 0.955423 0.699168 0.029669 11.00000 0.06634 C51 1 0.845310 0.723606 0.044036 11.00000 0.03197 C52 1 0.801236 0.708059 0.105348 11.00000 0.03993 AFIX 66 C53 1 0.703447 0.508335 0.153031 11.00000 0.04174 C58 1 0.748078 0.418367 0.109529 11.00000 0.04699 C57 1 0.674755 0.334702 0.049696 11.00000 0.04129 C56 1 0.556800 0.341004 0.033363 11.00000 0.06624 C55 1 0.512168 0.430972 0.076864 11.00000 0.04201 C54 1 0.585490 0.514638 0.136698 11.00000 0.06901 AFIX 0 B1 3 0.799426 0.623321 0.223723 11.00000 0.04930 HKLF 4 REM dy60_hp3_38deg_a.res in P-1 REM wR2 = 0.3322, GooF = S = 1.145, Restrained GooF = 1.151 for all data REM R1 = 0.1243 for 1210 Fo > 4sig(Fo) and 0.1921 for all 1981 data REM 272 parameters refined using 36 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.158, deepest hole -1.180, 1-sigma level 0.155 Q1 1 0.6602 0.8001 0.6913 11.00000 0.05 1.16 Q2 1 0.6500 0.7809 0.6647 11.00000 0.05 1.10 Q3 1 0.7132 0.9015 0.7566 11.00000 0.05 0.95 Q4 1 0.6791 0.9258 0.8569 11.00000 0.05 0.86 Q5 1 0.5737 0.7743 0.6071 11.00000 0.05 0.80 Q6 1 0.6785 0.7633 0.6028 11.00000 0.05 0.80 Q7 1 0.7994 0.9171 0.8446 11.00000 0.05 0.79 Q8 1 0.6954 0.7839 0.5775 11.00000 0.05 0.78 Q9 1 0.8194 0.9555 0.8775 11.00000 0.05 0.78 Q10 1 0.5628 0.7593 0.5807 11.00000 0.05 0.78 Q11 1 0.5350 0.7732 0.7266 11.00000 0.05 0.75 Q12 1 0.5439 0.7189 0.5425 11.00000 0.05 0.71 Q13 1 0.7073 0.9980 0.7209 11.00000 0.05 0.60 Q14 1 0.7853 1.0193 0.9422 11.00000 0.05 0.60 Q15 1 0.7960 1.0377 0.9617 11.00000 0.05 0.56 Q16 1 1.0589 0.5417 0.1721 11.00000 0.05 0.55 Q17 1 0.8251 0.5670 0.2908 11.00000 0.05 0.54 Q18 1 0.6570 0.7944 0.4231 11.00000 0.05 0.53 Q19 1 0.7608 0.7396 0.7395 11.00000 0.05 0.52 Q20 1 1.0380 0.5216 0.1480 11.00000 0.05 0.51 ; _shelx_res_checksum 94013 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 2.577 _oxdiff_exptl_absorpt_empirical_full_min 0.549 # start Validation Reply Form _vrf_ATOM007_dy60_hp3 ; PROBLEM: _atom_site_aniso_label is missing RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_THETM01_dy60_hp3 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_RINTA01_dy60_hp3 ; PROBLEM: The value of Rint is greater than 0.18 RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT029_dy60_hp3 ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.371 Why? RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_PLAT201_dy60_hp3 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 45 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT412_dy60_hp3 ; PROBLEM: Short Intra XH3 .. XHn H33A ..H34C . 1.68 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT020_dy60_hp3 ; PROBLEM: The Value of Rint is Greater Than 0.12 ......... 0.216 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT088_dy60_hp3 ; PROBLEM: Poor Data / Parameter Ratio .................... 7.28 Note RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT342_dy60_hp3 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.06138 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT360_dy60_hp3 ; PROBLEM: Short C(sp3)-C(sp3) Bond C10 - C11 . 1.31 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT911_dy60_hp3 ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.500 2182 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; # end Validation Reply Form _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_dy60_hp2 _database_code_depnum_ccdc_archive 'CCDC 2046707' loop_ _audit_author_name _audit_author_address 'Andreas M. Thiel' ;Aarhus University, Department of Chemistry Denmark ; _audit_update_record ; 2022-10-30 deposited with the CCDC. 2023-02-13 downloaded from the CCDC. ; _audit_creation_date 2020-02-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C34 H58 Dy, B C24 F20' _chemical_formula_sum 'C58 H58 B Dy F20' _chemical_formula_weight 1308.35 _chemical_melting_point ? _chemical_oxdiff_formula C58H58DyBF20 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6015(8) _cell_length_b 12.2877(10) _cell_length_c 19.663(4) _cell_angle_alpha 106.861(12) _cell_angle_beta 95.211(11) _cell_angle_gamma 100.515(7) _cell_volume 2606.6(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3406 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 19.8890 _cell_measurement_theta_min 1.8040 _shelx_estimated_absorpt_T_max 0.927 _shelx_estimated_absorpt_T_min 0.718 _exptl_absorpt_coefficient_mu 1.545 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.45252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1314 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_ambient_pressure 650000 _diffrn_reflns_av_R_equivalents 0.1622 _diffrn_reflns_av_unetI/netI 0.1079 _diffrn_reflns_Laue_measured_fraction_full 0.379 _diffrn_reflns_Laue_measured_fraction_max 0.379 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 17781 _diffrn_reflns_point_group_measured_fraction_full 0.379 _diffrn_reflns_point_group_measured_fraction_max 0.379 _diffrn_reflns_theta_full 20.814 _diffrn_reflns_theta_max 20.814 _diffrn_reflns_theta_min 1.770 _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.1795 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.379 _diffrn_measured_fraction_theta_max 0.379 _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 12.00 51.00 1.00 30.00 -- 7.76 -77.00-150.00 39 2 \w -37.00 7.00 1.00 30.00 -- 7.76 0.00-150.00 44 3 \w -46.00 29.00 1.00 30.00 -- 7.76 26.00 -7.00 75 4 \w 2.00 42.00 1.00 30.00 -- -8.54 -99.00 30.00 40 5 \w -25.00 37.00 1.00 30.00 -- -8.54 -39.00 12.00 62 6 \w -68.00 -7.00 1.00 30.00 -- -8.54 114.00 135.00 61 7 \w 20.00 64.00 1.00 30.00 -- -8.54-135.00 57.00 44 8 \w -20.00 33.00 1.00 30.00 -- -8.54 -53.00-162.00 53 9 \w -68.00 -7.00 1.00 30.00 -- -8.54 114.00 -45.00 61 10 \w -2.00 37.00 1.00 30.00 -- 7.76 -97.00 35.00 39 11 \w 34.00 58.00 1.00 30.00 -- 7.76 -99.00 30.00 24 12 \w -35.00 -12.00 1.00 30.00 -- 7.76 77.00 150.00 23 13 \w 12.00 35.00 1.00 30.00 -- 7.76 -77.00 60.00 23 14 \w -35.00 -12.00 1.00 30.00 -- -8.54 77.00 120.00 23 15 \w -53.00 9.00 1.00 30.00 -- -8.54 81.00 151.00 62 16 \w -50.00 20.00 1.00 30.00 -- -8.54 53.00 -17.00 70 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0147499000 _diffrn_orient_matrix_UB_12 -0.0159885000 _diffrn_orient_matrix_UB_13 -0.0379087000 _diffrn_orient_matrix_UB_21 -0.0293216000 _diffrn_orient_matrix_UB_22 -0.0564881000 _diffrn_orient_matrix_UB_23 -0.0009371000 _diffrn_orient_matrix_UB_31 -0.0536828000 _diffrn_orient_matrix_UB_32 0.0193694000 _diffrn_orient_matrix_UB_33 0.0040974000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1429 _reflns_number_total 2069 _reflns_odcompleteness_completeness 38.27 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 20.77 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.650 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.110 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 278 _refine_ls_number_reflns 2069 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1329 _refine_ls_R_factor_gt 0.0861 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1279P)^2^+20.3806P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2027 _refine_ls_wR_factor_ref 0.2397 _refine_special_details ? _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. Restrained planarity C54, C55, C56, C57, C58, F16, F17, F18, F19, F20, B1, C53 with sigma of 0.1 C47, C52, C51, C50, C49, C48, F15, F14, F13, F12, F11, B1 with sigma of 0.1 C35, C36, C37, C38, C39, C40, F1, F2, F3, F4, F5, B1 with sigma of 0.1 C41, C46, C45, C44, C43, C42, F10, F9, F8, F7, F6, B1 with sigma of 0.1 3.a Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C20(H20), C22(H22) 3.b Fitted pentagon refined as free rotating group: C1(C2,C3,C4,C5), C21(C20,C19,C18,C22) 3.c Fitted hexagon refined as free rotating group: C35(C40,C39,C38,C37,C36), C41(C42,C43,C44,C45,C46), C47(C48,C49,C50,C51,C52), C53(C58,C57,C56,C55,C54) 3.d Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B, H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A, H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.68661(11) 0.84739(12) 0.72042(17) 0.035(3) Uani 1 1 d . . . . . C1 C 0.5624(14) 0.9983(13) 0.7228(18) 0.049(8) Uiso 1 1 d . . . . . C2 C 0.5036(19) 0.930(2) 0.7620(17) 0.053(8) Uiso 1 1 d G . . . . C3 C 0.4494(15) 0.8186(16) 0.7129(19) 0.045(7) Uiso 1 1 d G . . . . H3 H 0.405154 0.756915 0.724282 0.055 Uiso 1 1 calc R . . . . C4 C 0.4747(14) 0.8176(14) 0.6434(18) 0.031(6) Uiso 1 1 d G . . . . C5 C 0.5445(14) 0.9286(17) 0.6496(18) 0.040(7) Uiso 1 1 d G . . . . H5 H 0.573466 0.951720 0.612190 0.048 Uiso 1 1 calc R . . . . C6 C 0.654(2) 1.119(2) 0.755(3) 0.038(7) Uiso 1 1 d . . . . . C7 C 0.772(2) 1.104(2) 0.780(3) 0.045(7) Uiso 1 1 d . . . . . H7A H 0.785007 1.126537 0.831084 0.067 Uiso 1 1 calc GR . . . . H7B H 0.831312 1.153016 0.763839 0.067 Uiso 1 1 calc GR . . . . H7C H 0.776383 1.024469 0.759775 0.067 Uiso 1 1 calc GR . . . . C8 C 0.608(2) 1.218(2) 0.806(4) 0.063(9) Uiso 1 1 d . . . . . H8A H 0.533365 1.224246 0.782986 0.095 Uiso 1 1 calc GR . . . . H8B H 0.664437 1.290731 0.815705 0.095 Uiso 1 1 calc GR . . . . H8C H 0.597267 1.201859 0.849784 0.095 Uiso 1 1 calc GR . . . . C9 C 0.679(2) 1.165(2) 0.682(3) 0.049(7) Uiso 1 1 d . . . . . H9A H 0.713487 1.110955 0.649649 0.074 Uiso 1 1 calc GR . . . . H9B H 0.731550 1.240668 0.698350 0.074 Uiso 1 1 calc GR . . . . H9C H 0.604751 1.170391 0.658535 0.074 Uiso 1 1 calc GR . . . . C10 C 0.484(3) 0.957(3) 0.842(4) 0.055(8) Uiso 1 1 d . . . . . C11 C 0.583(2) 1.013(3) 0.898(4) 0.059(8) Uiso 1 1 d . . . . . H11A H 0.629891 0.957501 0.902473 0.089 Uiso 1 1 calc GR . . . . H11B H 0.555249 1.042958 0.942920 0.089 Uiso 1 1 calc GR . . . . H11C H 0.631521 1.075956 0.887064 0.089 Uiso 1 1 calc GR . . . . C12 C 0.418(3) 0.842(3) 0.855(5) 0.073(10) Uiso 1 1 d . . . . . H12A H 0.350056 0.805129 0.818882 0.110 Uiso 1 1 calc GR . . . . H12B H 0.393989 0.861318 0.901713 0.110 Uiso 1 1 calc GR . . . . H12C H 0.471385 0.789918 0.852745 0.110 Uiso 1 1 calc GR . . . . C13 C 0.384(3) 1.033(3) 0.849(4) 0.065(9) Uiso 1 1 d . . . . . H13A H 0.411437 1.101382 0.835973 0.098 Uiso 1 1 calc GR . . . . H13B H 0.369035 1.054800 0.897808 0.098 Uiso 1 1 calc GR . . . . H13C H 0.312767 0.987075 0.817635 0.098 Uiso 1 1 calc GR . . . . C14 C 0.413(2) 0.722(2) 0.571(4) 0.042(7) Uiso 1 1 d . . . . . C15 C 0.501(4) 0.647(4) 0.539(5) 0.101(12) Uiso 1 1 d . . . . . H15A H 0.559554 0.691208 0.520759 0.151 Uiso 1 1 calc GR . . . . H15B H 0.457767 0.579002 0.500898 0.151 Uiso 1 1 calc GR . . . . H15C H 0.538431 0.622789 0.576150 0.151 Uiso 1 1 calc GR . . . . C16 C 0.377(3) 0.773(3) 0.515(4) 0.084(11) Uiso 1 1 d . . . . . H16A H 0.387352 0.855954 0.535931 0.125 Uiso 1 1 calc GR . . . . H16B H 0.295006 0.739455 0.495212 0.125 Uiso 1 1 calc GR . . . . H16C H 0.424753 0.757296 0.477345 0.125 Uiso 1 1 calc GR . . . . C17 C 0.302(4) 0.641(4) 0.575(7) 0.146(18) Uiso 1 1 d . . . . . H17A H 0.318292 0.606115 0.611931 0.219 Uiso 1 1 calc GR . . . . H17B H 0.275557 0.580627 0.529780 0.219 Uiso 1 1 calc GR . . . . H17C H 0.241197 0.683638 0.586716 0.219 Uiso 1 1 calc GR . . . . C21 C 0.8507(19) 0.7941(19) 0.634(2) 0.064(9) Uiso 1 1 d . . . . . C20 C 0.9146(14) 0.8664(12) 0.702(2) 0.050(8) Uiso 1 1 d G . . . . H20 H 0.963002 0.939918 0.711612 0.060 Uiso 1 1 calc R . . . . C19 C 0.8915(18) 0.8066(18) 0.7530(19) 0.043(8) Uiso 1 1 d G . . . . C18 C 0.8134(17) 0.6974(15) 0.716(2) 0.042(8) Uiso 1 1 d G . . . . C22 C 0.7882(15) 0.6897(14) 0.643(2) 0.037(7) Uiso 1 1 d G . . . . H22 H 0.739333 0.627198 0.606971 0.045 Uiso 1 1 calc R . . . . C23 C 0.746(2) 0.612(2) 0.752(3) 0.037(7) Uiso 1 1 d . . . . . C24 C 0.632(3) 0.651(3) 0.772(5) 0.077(10) Uiso 1 1 d . . . . . H24A H 0.647197 0.705242 0.819511 0.116 Uiso 1 1 calc GR . . . . H24B H 0.572074 0.584345 0.769509 0.116 Uiso 1 1 calc GR . . . . H24C H 0.604461 0.688004 0.738380 0.116 Uiso 1 1 calc GR . . . . C25 C 0.813(2) 0.572(3) 0.804(4) 0.064(9) Uiso 1 1 d . . . . . H25A H 0.878223 0.544284 0.783371 0.096 Uiso 1 1 calc GR . . . . H25B H 0.761361 0.509576 0.813657 0.096 Uiso 1 1 calc GR . . . . H25C H 0.841850 0.635056 0.847314 0.096 Uiso 1 1 calc GR . . . . C26 C 0.680(2) 0.492(2) 0.680(4) 0.054(8) Uiso 1 1 d . . . . . H26A H 0.626995 0.514107 0.648457 0.081 Uiso 1 1 calc GR . . . . H26B H 0.635794 0.433935 0.697023 0.081 Uiso 1 1 calc GR . . . . H26C H 0.739577 0.461768 0.654662 0.081 Uiso 1 1 calc GR . . . . C27 C 0.958(2) 0.863(2) 0.830(4) 0.042(7) Uiso 1 1 d . . . . . C28 C 0.882(3) 0.875(3) 0.883(4) 0.063(9) Uiso 1 1 d . . . . . H28A H 0.836978 0.931974 0.880191 0.095 Uiso 1 1 calc GR . . . . H28B H 0.928229 0.898798 0.930270 0.095 Uiso 1 1 calc GR . . . . H28C H 0.828159 0.801162 0.875679 0.095 Uiso 1 1 calc GR . . . . C29 C 1.030(3) 0.990(3) 0.841(4) 0.059(8) Uiso 1 1 d . . . . . H29A H 1.090701 0.986754 0.811004 0.089 Uiso 1 1 calc GR . . . . H29B H 1.066949 1.024155 0.890837 0.089 Uiso 1 1 calc GR . . . . H29C H 0.977812 1.035600 0.829745 0.089 Uiso 1 1 calc GR . . . . C30 C 1.060(2) 0.799(2) 0.847(4) 0.059(8) Uiso 1 1 d . . . . . H30A H 1.025914 0.718377 0.840062 0.089 Uiso 1 1 calc GR . . . . H30B H 1.097137 0.835533 0.896433 0.089 Uiso 1 1 calc GR . . . . H30C H 1.118184 0.804531 0.816052 0.089 Uiso 1 1 calc GR . . . . C31 C 0.873(2) 0.816(3) 0.566(4) 0.049(8) Uiso 1 1 d . . . . . C32 C 0.816(3) 0.916(3) 0.552(5) 0.078(10) Uiso 1 1 d . . . . . H32A H 0.760630 0.885536 0.508702 0.117 Uiso 1 1 calc GR . . . . H32B H 0.877810 0.976826 0.548334 0.117 Uiso 1 1 calc GR . . . . H32C H 0.776470 0.946997 0.591885 0.117 Uiso 1 1 calc GR . . . . C33 C 0.828(3) 0.710(3) 0.502(4) 0.079(10) Uiso 1 1 d . . . . . H33A H 0.891583 0.692450 0.476092 0.119 Uiso 1 1 calc GR . . . . H33B H 0.766231 0.722976 0.471917 0.119 Uiso 1 1 calc GR . . . . H33C H 0.796794 0.644843 0.518407 0.119 Uiso 1 1 calc GR . . . . C34 C 1.003(3) 0.853(4) 0.559(5) 0.098(12) Uiso 1 1 d . . . . . H34A H 1.037969 0.925942 0.595566 0.146 Uiso 1 1 calc GR . . . . H34B H 1.008941 0.861850 0.512517 0.146 Uiso 1 1 calc GR . . . . H34C H 1.044852 0.794815 0.565006 0.146 Uiso 1 1 calc GR . . . . F1 F 0.7806(13) 0.3876(13) 0.2488(19) 0.061(4) Uiso 1 1 d . . . . . F2 F 0.9285(14) 0.3529(14) 0.350(2) 0.070(5) Uiso 1 1 d . . . . . F3 F 1.0999(16) 0.5305(16) 0.440(2) 0.089(6) Uiso 1 1 d . . . . . F4 F 1.1365(16) 0.7428(16) 0.416(2) 0.090(6) Uiso 1 1 d . . . . . F5 F 1.0031(12) 0.7766(13) 0.3110(18) 0.059(4) Uiso 1 1 d . . . . . F6 F 0.8383(12) 0.8847(13) 0.2484(18) 0.056(4) Uiso 1 1 d . . . . . F7 F 0.7373(12) 1.0223(13) 0.3467(18) 0.057(4) Uiso 1 1 d . . . . . F8 F 0.5937(13) 0.9343(14) 0.429(2) 0.071(5) Uiso 1 1 d . . . . . F9 F 0.5372(14) 0.6986(14) 0.400(2) 0.069(5) Uiso 1 1 d . . . . . F10 F 0.6313(11) 0.5585(12) 0.3030(18) 0.051(4) Uiso 1 1 d . . . . . F11 F 1.0518(12) 0.6065(13) 0.1782(18) 0.053(4) Uiso 1 1 d . . . . . F12 F 1.1273(15) 0.6376(14) 0.063(2) 0.076(5) Uiso 1 1 d . . . . . F13 F 0.9978(16) 0.7238(16) -0.025(2) 0.095(6) Uiso 1 1 d . . . . . F14 F 0.7887(13) 0.7764(14) 0.012(2) 0.066(5) Uiso 1 1 d . . . . . F15 F 0.7013(13) 0.7310(13) 0.1190(19) 0.060(4) Uiso 1 1 d . . . . . F16 F 0.5274(12) 0.5888(12) 0.1721(18) 0.050(4) Uiso 1 1 d . . . . . F17 F 0.3995(14) 0.4339(15) 0.061(2) 0.077(5) Uiso 1 1 d . . . . . F18 F 0.4880(16) 0.2593(17) -0.023(2) 0.095(6) Uiso 1 1 d . . . . . F19 F 0.7189(13) 0.2495(13) 0.0116(19) 0.063(4) Uiso 1 1 d . . . . . F20 F 0.8567(12) 0.4119(12) 0.1227(17) 0.046(4) Uiso 1 1 d . . . . . C35 C 0.8887(15) 0.5872(16) 0.2765(16) 0.042(7) Uiso 1 1 d . . . . . C40 C 0.9803(16) 0.6759(12) 0.3207(17) 0.054(8) Uiso 1 1 d G . . . . C39 C 1.0515(14) 0.6552(15) 0.3743(16) 0.071(10) Uiso 1 1 d G . . . . C38 C 1.0312(16) 0.5458(18) 0.3837(15) 0.065(9) Uiso 1 1 d G . . . . C37 C 0.9397(17) 0.4571(13) 0.3395(17) 0.059(8) Uiso 1 1 d G . . . . C36 C 0.8684(14) 0.4778(13) 0.2859(16) 0.056(8) Uiso 1 1 d G . . . . C41 C 0.7364(14) 0.7139(12) 0.2730(14) 0.040(7) Uiso 1 1 d . . . . . C42 C 0.7624(14) 0.8331(13) 0.2834(15) 0.049(7) Uiso 1 1 d G . . . . C43 C 0.7123(14) 0.9068(10) 0.3343(15) 0.048(7) Uiso 1 1 d G . . . . C44 C 0.6361(14) 0.8613(13) 0.3748(14) 0.051(8) Uiso 1 1 d G . . . . C45 C 0.6101(13) 0.7420(14) 0.3644(14) 0.051(8) Uiso 1 1 d G . . . . C46 C 0.6602(14) 0.6683(10) 0.3135(15) 0.042(7) Uiso 1 1 d G . . . . C47 C 0.8691(14) 0.6661(13) 0.1532(14) 0.048(7) Uiso 1 1 d . . . . . C48 C 0.9788(12) 0.6431(13) 0.1385(15) 0.034(6) Uiso 1 1 d G . . . . C49 C 1.0227(11) 0.6624(13) 0.0785(15) 0.039(7) Uiso 1 1 d G . . . . C50 C 0.9569(15) 0.7046(14) 0.0332(14) 0.077(10) Uiso 1 1 d G . . . . C51 C 0.8473(14) 0.7276(13) 0.0480(15) 0.040(7) Uiso 1 1 d G . . . . C52 C 0.8034(11) 0.7084(13) 0.1079(15) 0.044(7) Uiso 1 1 d G . . . . C53 C 0.7003(14) 0.5076(13) 0.1531(14) 0.045(7) Uiso 1 1 d . . . . . C58 C 0.7475(11) 0.4201(15) 0.1106(15) 0.039(7) Uiso 1 1 d G . . . . C57 C 0.6768(15) 0.3357(13) 0.0510(15) 0.043(7) Uiso 1 1 d G . . . . C56 C 0.5589(15) 0.3389(14) 0.0338(14) 0.069(9) Uiso 1 1 d G . . . . C55 C 0.5116(11) 0.4264(16) 0.0762(16) 0.043(7) Uiso 1 1 d G . . . . C54 C 0.5823(14) 0.5108(13) 0.1358(15) 0.041(7) Uiso 1 1 d G . . . . B1 B 0.804(2) 0.620(2) 0.222(3) 0.041(8) Uiso 1 1 d . . . . . 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 0.0456(10) 0.0507(11) 0.006(8) 0.004(2) -0.005(2) 0.0156(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 2.540(15) . ? Dy1 C2 2.614(19) . ? Dy1 C3 2.694(16) . ? Dy1 C4 2.67(2) . ? Dy1 C5 2.58(2) . ? Dy1 C21 2.71(2) . ? Dy1 C20 2.679(15) . ? Dy1 C19 2.58(2) . ? Dy1 C18 2.548(16) . ? Dy1 C22 2.629(19) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 C6 1.58(3) . ? C2 C3 1.4200 . ? C2 C10 1.56(8) . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C4 C14 1.57(6) . ? C6 C7 1.47(4) . ? C6 C8 1.55(5) . ? C6 C9 1.71(7) . ? C10 C11 1.44(8) . ? C10 C12 1.58(4) . ? C10 C13 1.60(3) . ? C14 C15 1.55(4) . ? C14 C16 1.48(8) . ? C14 C17 1.51(4) . ? C21 C20 1.4200 . ? C21 C22 1.4200 . ? C21 C31 1.48(6) . ? C20 C19 1.4200 . ? C19 C18 1.4200 . ? C19 C27 1.53(7) . ? C18 C22 1.4200 . ? C18 C23 1.55(4) . ? C23 C24 1.53(3) . ? C23 C25 1.47(7) . ? C23 C26 1.72(7) . ? C27 C28 1.43(7) . ? C27 C29 1.57(3) . ? C27 C30 1.59(4) . ? C31 C32 1.57(4) . ? C31 C33 1.49(8) . ? C31 C34 1.53(3) . ? F1 C36 1.33(3) . ? F2 C37 1.344(19) . ? F3 C38 1.38(4) . ? F4 C39 1.32(3) . ? F5 C40 1.290(18) . ? F6 C42 1.35(2) . ? F7 C43 1.340(16) . ? F8 C44 1.37(3) . ? F9 C45 1.29(2) . ? F10 C46 1.279(15) . ? F11 C48 1.32(3) . ? F12 C49 1.345(18) . ? F13 C50 1.34(4) . ? F14 C51 1.28(3) . ? F15 C52 1.288(15) . ? F16 C54 1.32(2) . ? F17 C55 1.34(2) . ? F18 C56 1.34(4) . ? F19 C57 1.32(2) . ? F20 C58 1.295(17) . ? C35 C40 1.3900 . ? C35 C36 1.3900 . ? C35 B1 1.58(4) . ? C40 C39 1.3900 . ? C39 C38 1.3900 . ? C38 C37 1.3900 . ? C37 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 B1 1.66(3) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C47 B1 1.78(4) . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C53 C58 1.3900 . ? C53 C54 1.3900 . ? C53 B1 1.79(4) . ? C58 C57 1.3900 . ? C57 C56 1.3900 . ? C56 C55 1.3900 . ? C55 C54 1.3900 . ? 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 C1 Dy1 C2 31.9(2) . . ? C1 Dy1 C3 52.0(2) . . ? C1 Dy1 C4 52.2(3) . . ? C1 Dy1 C5 32.21(18) . . ? C1 Dy1 C21 127.3(8) . . ? C1 Dy1 C20 127.0(5) . . ? C1 Dy1 C19 147.4(7) . . ? C1 Dy1 C18 179.0(8) . . ? C1 Dy1 C22 147.5(11) . . ? C2 Dy1 C3 30.98(18) . . ? C2 Dy1 C4 51.5(2) . . ? C2 Dy1 C21 157.0(9) . . ? C2 Dy1 C20 153.9(6) . . ? C2 Dy1 C22 153.7(8) . . ? C3 Dy1 C21 139.7(10) . . ? C4 Dy1 C3 30.68(19) . . ? C4 Dy1 C21 111.3(9) . . ? C4 Dy1 C20 139.1(11) . . ? C5 Dy1 C2 52.5(2) . . ? C5 Dy1 C3 51.6(3) . . ? C5 Dy1 C4 31.3(2) . . ? C5 Dy1 C21 104.6(8) . . ? C5 Dy1 C20 121.0(8) . . ? C5 Dy1 C19 152.3(8) . . ? C5 Dy1 C22 116.0(10) . . ? C20 Dy1 C3 169.7(11) . . ? C20 Dy1 C21 30.6(2) . . ? C19 Dy1 C2 149.2(10) . . ? C19 Dy1 C3 155.4(7) . . ? C19 Dy1 C4 157.7(8) . . ? C19 Dy1 C21 51.4(2) . . ? C19 Dy1 C20 31.26(17) . . ? C19 Dy1 C22 52.34(18) . . ? C18 Dy1 C2 149.1(7) . . ? C18 Dy1 C3 128.8(5) . . ? C18 Dy1 C4 127.9(8) . . ? C18 Dy1 C5 147.3(11) . . ? C18 Dy1 C21 51.7(2) . . ? C18 Dy1 C20 52.1(2) . . ? C18 Dy1 C19 32.1(2) . . ? C18 Dy1 C22 31.79(16) . . ? C22 Dy1 C3 122.8(7) . . ? C22 Dy1 C4 105.4(8) . . ? C22 Dy1 C21 30.8(2) . . ? C22 Dy1 C20 51.3(2) . . ? C2 C1 Dy1 76.9(7) . . ? C2 C1 C5 108.0 . . ? C2 C1 C6 127(3) . . ? C5 C1 Dy1 75.3(9) . . ? C5 C1 C6 124(3) . . ? C6 C1 Dy1 104.5(11) . . ? C1 C2 Dy1 71.2(6) . . ? C1 C2 C3 108.0 . . ? C1 C2 C10 133(2) . . ? C3 C2 Dy1 77.6(7) . . ? C3 C2 C10 119(2) . . ? C10 C2 Dy1 120(2) . . ? C2 C3 Dy1 71.4(7) . . ? C4 C3 Dy1 73.8(8) . . ? C4 C3 C2 108.0 . . ? C3 C4 Dy1 75.5(8) . . ? C3 C4 C5 108.0 . . ? C3 C4 C14 126(2) . . ? C5 C4 Dy1 70.7(6) . . ? C5 C4 C14 125(2) . . ? C14 C4 Dy1 129.8(12) . . ? C1 C5 Dy1 72.4(9) . . ? C4 C5 Dy1 78.0(6) . . ? C4 C5 C1 108.0 . . ? C1 C6 C9 105(4) . . ? C7 C6 C1 111.6(17) . . ? C7 C6 C8 116(4) . . ? C7 C6 C9 102(2) . . ? C8 C6 C1 115.9(19) . . ? C8 C6 C9 104(3) . . ? C2 C10 C12 110(5) . . ? C2 C10 C13 105(5) . . ? C11 C10 C2 120(3) . . ? C11 C10 C12 108(5) . . ? C11 C10 C13 111(5) . . ? C12 C10 C13 102(2) . . ? C15 C14 C4 110(4) . . ? C16 C14 C4 113(3) . . ? C16 C14 C15 106(5) . . ? C16 C14 C17 105(5) . . ? C17 C14 C4 115(6) . . ? C17 C14 C15 108(3) . . ? C20 C21 Dy1 73.6(8) . . ? C20 C21 C22 108.0 . . ? C20 C21 C31 123(2) . . ? C22 C21 Dy1 71.5(5) . . ? C22 C21 C31 127(2) . . ? C31 C21 Dy1 132.1(15) . . ? C21 C20 Dy1 75.9(9) . . ? C19 C20 Dy1 70.5(9) . . ? C19 C20 C21 108.0 . . ? C20 C19 Dy1 78.2(8) . . ? C20 C19 C27 118(2) . . ? C18 C19 Dy1 72.7(6) . . ? C18 C19 C20 108.0 . . ? C18 C19 C27 134(2) . . ? C27 C19 Dy1 119.8(17) . . ? C19 C18 Dy1 75.2(7) . . ? C19 C18 C22 108.0 . . ? C19 C18 C23 126(3) . . ? C22 C18 Dy1 77.3(10) . . ? C22 C18 C23 125(3) . . ? C23 C18 Dy1 104.5(11) . . ? C21 C22 Dy1 77.7(6) . . ? C18 C22 Dy1 71.0(10) . . ? C18 C22 C21 108.0 . . ? C18 C23 C26 103(4) . . ? C24 C23 C18 109(2) . . ? C24 C23 C26 97(3) . . ? C25 C23 C18 120(2) . . ? C25 C23 C24 118(5) . . ? C25 C23 C26 107(2) . . ? C19 C27 C29 112(4) . . ? C19 C27 C30 113(4) . . ? C28 C27 C19 113(3) . . ? C28 C27 C29 105(4) . . ? C28 C27 C30 111(5) . . ? C29 C27 C30 102(2) . . ? C21 C31 C32 113(4) . . ? C21 C31 C33 112(3) . . ? C21 C31 C34 116(5) . . ? C33 C31 C32 108(5) . . ? C33 C31 C34 104(4) . . ? C34 C31 C32 104(2) . . ? C40 C35 C36 120.0 . . ? C40 C35 B1 117.1(15) . . ? C36 C35 B1 122.7(15) . . ? F5 C40 C35 121(2) . . ? F5 C40 C39 119(2) . . ? C39 C40 C35 120.0 . . ? F4 C39 C40 118(2) . . ? F4 C39 C38 122(2) . . ? C40 C39 C38 120.0 . . ? F3 C38 C39 118.2(17) . . ? F3 C38 C37 121.7(17) . . ? C39 C38 C37 120.0 . . ? F2 C37 C38 116(2) . . ? F2 C37 C36 124(2) . . ? C36 C37 C38 120.0 . . ? F1 C36 C35 125.4(17) . . ? F1 C36 C37 114.6(17) . . ? C37 C36 C35 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 B1 123.9(13) . . ? C46 C41 B1 115.6(13) . . ? F6 C42 C41 123.8(13) . . ? F6 C42 C43 116.2(13) . . ? C43 C42 C41 120.0 . . ? F7 C43 C42 121.5(15) . . ? F7 C43 C44 118.5(15) . . ? C42 C43 C44 120.0 . . ? F8 C44 C43 120.3(13) . . ? F8 C44 C45 119.5(13) . . ? C45 C44 C43 120.0 . . ? F9 C45 C44 120.5(14) . . ? F9 C45 C46 119.5(14) . . ? C44 C45 C46 120.0 . . ? F10 C46 C41 121.2(16) . . ? F10 C46 C45 118.7(15) . . ? C45 C46 C41 120.0 . . ? C48 C47 C52 120.0 . . ? C48 C47 B1 119.2(13) . . ? C52 C47 B1 120.1(13) . . ? F11 C48 C47 126.1(16) . . ? F11 C48 C49 113.9(16) . . ? C47 C48 C49 120.0 . . ? F12 C49 C48 121(2) . . ? F12 C49 C50 119(2) . . ? C50 C49 C48 120.0 . . ? F13 C50 C49 120.8(16) . . ? F13 C50 C51 119.2(16) . . ? C49 C50 C51 120.0 . . ? F14 C51 C50 122.0(17) . . ? F14 C51 C52 117.7(17) . . ? C52 C51 C50 120.0 . . ? F15 C52 C47 122.5(19) . . ? F15 C52 C51 117.5(19) . . ? C51 C52 C47 120.0 . . ? C58 C53 C54 120.0 . . ? C58 C53 B1 115.6(13) . . ? C54 C53 B1 124.0(12) . . ? F20 C58 C53 123.7(17) . . ? F20 C58 C57 116.3(17) . . ? C57 C58 C53 120.0 . . ? F19 C57 C58 120.9(17) . . ? F19 C57 C56 119.1(17) . . ? C56 C57 C58 120.0 . . ? F18 C56 C57 121.7(15) . . ? F18 C56 C55 118.3(15) . . ? C55 C56 C57 120.0 . . ? F17 C55 C56 121.8(18) . . ? F17 C55 C54 118.2(18) . . ? C56 C55 C54 120.0 . . ? F16 C54 C53 125.6(17) . . ? F16 C54 C55 114.4(17) . . ? C55 C54 C53 120.0 . . ? C35 B1 C41 105(3) . . ? C35 B1 C47 117.0(15) . . ? C35 B1 C53 119.7(16) . . ? C41 B1 C47 115.3(15) . . ? C41 B1 C53 111.3(15) . . ? C47 B1 C53 89(2) . . ? _shelx_res_file ; TITL dy60_hp2_38deg_a.res in P-1 dy60_hp2_38deg.res created by SHELXL-2018/3 at 15:51:27 on 26-Feb-2020 REM Old TITL Dy60_HP2_38deg in P-1 REM SHELXT solution in P-1: R1 0.173, Rweak 0.040, Alpha 0.172 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C61 B F20 Dy CELL 0.71073 11.6015 12.2877 19.6631 106.861 95.211 100.515 ZERR 2 0.0008 0.001 0.0035 0.012 0.011 0.007 LATT 1 SFAC C H B Dy F UNIT 116 116 2 2 40 FLAT C54 C55 C56 C57 C58 F16 F17 F18 F19 F20 B1 C53 FLAT C47 C52 C51 C50 C49 C48 F15 F14 F13 F12 F11 B1 FLAT C35 C36 C37 C38 C39 C40 F1 F2 F3 F4 F5 B1 FLAT C41 C46 C45 C44 C43 C42 F10 F9 F8 F7 F6 B1 L.S. 20 0 0 PLAN 20 SIZE 0.16 0.23 0.05 FREE Dy1 C24 FREE Dy1 C7 list 4 fmap 2 53 acta SHEL 100 0.83 OMIT 0 180 OMIT 4 -5 1 OMIT 1 -6 3 OMIT -5 3 3 OMIT -5 -2 2 OMIT -5 -1 5 OMIT 1 -6 2 OMIT 0 -6 3 OMIT -2 -5 1 OMIT -2 -11 5 OMIT 2 -10 9 OMIT -7 -4 5 OMIT -7 -6 3 OMIT -6 -6 7 OMIT 5 -11 8 OMIT -4 -7 4 OMIT 6 -9 3 OMIT -1 -8 9 OMIT 1 -12 3 REM REM REM WGHT 0.127900 20.380600 FVAR 0.38927 DY1 4 0.686611 0.847394 0.720419 11.00000 0.04563 0.05068 = 0.00620 0.00367 -0.00456 0.01559 AFIX 56 C1 1 0.562400 0.998286 0.722849 11.00000 0.04926 C2 1 0.503628 0.930262 0.761990 11.00000 0.05344 C3 1 0.449431 0.818579 0.712918 11.00000 0.04545 AFIX 43 H3 2 0.405154 0.756915 0.724282 11.00000 -1.20000 AFIX 55 C4 1 0.474707 0.817578 0.643448 11.00000 0.03114 C5 1 0.544526 0.928643 0.649586 11.00000 0.04040 AFIX 43 H5 2 0.573466 0.951720 0.612190 11.00000 -1.20000 AFIX 0 C6 1 0.653708 1.119021 0.754872 11.00000 0.03817 C7 1 0.771869 1.104499 0.779536 11.00000 0.04471 AFIX 137 H7A 2 0.785007 1.126537 0.831084 11.00000 -1.50000 H7B 2 0.831312 1.153016 0.763839 11.00000 -1.50000 H7C 2 0.776383 1.024469 0.759775 11.00000 -1.50000 AFIX 0 C8 1 0.607836 1.218409 0.805663 11.00000 0.06319 AFIX 137 H8A 2 0.533365 1.224246 0.782986 11.00000 -1.50000 H8B 2 0.664437 1.290731 0.815705 11.00000 -1.50000 H8C 2 0.597267 1.201859 0.849784 11.00000 -1.50000 AFIX 0 C9 1 0.678603 1.165336 0.682409 11.00000 0.04927 AFIX 137 H9A 2 0.713487 1.110955 0.649649 11.00000 -1.50000 H9B 2 0.731550 1.240668 0.698350 11.00000 -1.50000 H9C 2 0.604751 1.170391 0.658535 11.00000 -1.50000 AFIX 0 C10 1 0.484202 0.957183 0.842002 11.00000 0.05495 C11 1 0.583432 1.013023 0.898274 11.00000 0.05943 AFIX 137 H11A 2 0.629891 0.957501 0.902473 11.00000 -1.50000 H11B 2 0.555249 1.042958 0.942920 11.00000 -1.50000 H11C 2 0.631521 1.075956 0.887064 11.00000 -1.50000 AFIX 0 C12 1 0.418444 0.842072 0.855126 11.00000 0.07348 AFIX 137 H12A 2 0.350056 0.805129 0.818882 11.00000 -1.50000 H12B 2 0.393989 0.861318 0.901713 11.00000 -1.50000 H12C 2 0.471385 0.789918 0.852745 11.00000 -1.50000 AFIX 0 C13 1 0.384350 1.032678 0.849062 11.00000 0.06544 AFIX 137 H13A 2 0.411437 1.101382 0.835973 11.00000 -1.50000 H13B 2 0.369035 1.054800 0.897808 11.00000 -1.50000 H13C 2 0.312767 0.987075 0.817635 11.00000 -1.50000 AFIX 0 C14 1 0.413440 0.722273 0.570675 11.00000 0.04235 C15 1 0.500559 0.646646 0.539129 11.00000 0.10068 AFIX 137 H15A 2 0.559554 0.691208 0.520759 11.00000 -1.50000 H15B 2 0.457767 0.579002 0.500898 11.00000 -1.50000 H15C 2 0.538431 0.622789 0.576150 11.00000 -1.50000 AFIX 0 C16 1 0.376940 0.773207 0.514905 11.00000 0.08358 AFIX 137 H16A 2 0.387352 0.855954 0.535931 11.00000 -1.50000 H16B 2 0.295006 0.739455 0.495212 11.00000 -1.50000 H16C 2 0.424753 0.757296 0.477345 11.00000 -1.50000 AFIX 0 C17 1 0.301954 0.640726 0.575187 11.00000 0.14626 AFIX 137 H17A 2 0.318292 0.606115 0.611931 11.00000 -1.50000 H17B 2 0.275557 0.580627 0.529780 11.00000 -1.50000 H17C 2 0.241197 0.683638 0.586716 11.00000 -1.50000 AFIX 56 C21 1 0.850748 0.794095 0.634083 11.00000 0.06382 C20 1 0.914575 0.866369 0.702091 11.00000 0.05003 AFIX 43 H20 2 0.963002 0.939918 0.711612 11.00000 -1.20000 AFIX 55 C19 1 0.891476 0.806623 0.753007 11.00000 0.04331 C18 1 0.813373 0.697425 0.716467 11.00000 0.04198 C22 1 0.788202 0.689682 0.642968 11.00000 0.03747 AFIX 43 H22 2 0.739333 0.627198 0.606971 11.00000 -1.20000 AFIX 0 C23 1 0.746022 0.612484 0.752016 11.00000 0.03666 C24 1 0.631769 0.651128 0.771691 11.00000 0.07739 AFIX 137 H24A 2 0.647197 0.705242 0.819511 11.00000 -1.50000 H24B 2 0.572074 0.584345 0.769509 11.00000 -1.50000 H24C 2 0.604461 0.688004 0.738380 11.00000 -1.50000 AFIX 0 C25 1 0.812662 0.571811 0.803575 11.00000 0.06392 AFIX 137 H25A 2 0.878223 0.544284 0.783371 11.00000 -1.50000 H25B 2 0.761361 0.509576 0.813657 11.00000 -1.50000 H25C 2 0.841850 0.635056 0.847314 11.00000 -1.50000 AFIX 0 C26 1 0.679800 0.492335 0.680117 11.00000 0.05427 AFIX 137 H26A 2 0.626995 0.514107 0.648457 11.00000 -1.50000 H26B 2 0.635794 0.433935 0.697023 11.00000 -1.50000 H26C 2 0.739577 0.461768 0.654662 11.00000 -1.50000 AFIX 0 C27 1 0.958424 0.862660 0.829850 11.00000 0.04246 C28 1 0.881608 0.874637 0.883419 11.00000 0.06333 AFIX 137 H28A 2 0.836978 0.931974 0.880191 11.00000 -1.50000 H28B 2 0.928229 0.898798 0.930270 11.00000 -1.50000 H28C 2 0.828159 0.801162 0.875679 11.00000 -1.50000 AFIX 0 C29 1 1.030476 0.989637 0.841491 11.00000 0.05942 AFIX 137 H29A 2 1.090701 0.986754 0.811004 11.00000 -1.50000 H29B 2 1.066949 1.024155 0.890837 11.00000 -1.50000 H29C 2 0.977812 1.035600 0.829745 11.00000 -1.50000 AFIX 0 C30 1 1.060013 0.798941 0.847337 11.00000 0.05933 AFIX 137 H30A 2 1.025914 0.718377 0.840062 11.00000 -1.50000 H30B 2 1.097137 0.835533 0.896433 11.00000 -1.50000 H30C 2 1.118184 0.804531 0.816052 11.00000 -1.50000 AFIX 0 C31 1 0.872990 0.815672 0.565913 11.00000 0.04875 C32 1 0.816466 0.916040 0.552390 11.00000 0.07803 AFIX 137 H32A 2 0.760630 0.885536 0.508702 11.00000 -1.50000 H32B 2 0.877810 0.976826 0.548334 11.00000 -1.50000 H32C 2 0.776470 0.946997 0.591885 11.00000 -1.50000 AFIX 0 C33 1 0.827888 0.709547 0.502437 11.00000 0.07930 AFIX 137 H33A 2 0.891583 0.692450 0.476092 11.00000 -1.50000 H33B 2 0.766231 0.722976 0.471917 11.00000 -1.50000 H33C 2 0.796794 0.644843 0.518407 11.00000 -1.50000 AFIX 0 C34 1 1.003288 0.853040 0.559120 11.00000 0.09758 AFIX 137 H34A 2 1.037969 0.925942 0.595566 11.00000 -1.50000 H34B 2 1.008941 0.861850 0.512517 11.00000 -1.50000 H34C 2 1.044852 0.794815 0.565006 11.00000 -1.50000 AFIX 0 F1 5 0.780556 0.387625 0.248818 11.00000 0.06146 F2 5 0.928456 0.352864 0.350356 11.00000 0.06962 F3 5 1.099869 0.530479 0.439707 11.00000 0.08902 F4 5 1.136529 0.742819 0.415826 11.00000 0.09022 F5 5 1.003057 0.776628 0.311049 11.00000 0.05860 F6 5 0.838271 0.884665 0.248384 11.00000 0.05596 F7 5 0.737285 1.022290 0.346692 11.00000 0.05741 F8 5 0.593660 0.934279 0.429071 11.00000 0.07110 F9 5 0.537213 0.698620 0.400389 11.00000 0.06854 F10 5 0.631263 0.558535 0.302978 11.00000 0.05117 F11 5 1.051798 0.606542 0.178215 11.00000 0.05302 F12 5 1.127271 0.637618 0.062713 11.00000 0.07578 F13 5 0.997789 0.723825 -0.024661 11.00000 0.09492 F14 5 0.788691 0.776388 0.011561 11.00000 0.06621 F15 5 0.701274 0.730955 0.118981 11.00000 0.05964 F16 5 0.527393 0.588833 0.172107 11.00000 0.05017 F17 5 0.399463 0.433894 0.060535 11.00000 0.07747 F18 5 0.488032 0.259258 -0.023375 11.00000 0.09520 F19 5 0.718913 0.249495 0.011612 11.00000 0.06344 F20 5 0.856698 0.411856 0.122713 11.00000 0.04551 AFIX 66 C35 1 0.888713 0.587164 0.276489 11.00000 0.04220 C40 1 0.980290 0.675858 0.320689 11.00000 0.05354 C39 1 1.051549 0.655178 0.374278 11.00000 0.07090 C38 1 1.031231 0.545803 0.383666 11.00000 0.06454 C37 1 0.939653 0.457108 0.339466 11.00000 0.05922 C36 1 0.868394 0.477786 0.285878 11.00000 0.05579 AFIX 66 C41 1 0.736369 0.713870 0.272998 11.00000 0.03990 C42 1 0.762383 0.833084 0.283429 11.00000 0.04852 C43 1 0.712266 0.906777 0.334336 11.00000 0.04778 C44 1 0.636135 0.861256 0.374814 11.00000 0.05098 C45 1 0.610120 0.742042 0.364384 11.00000 0.05135 C46 1 0.660236 0.668348 0.313476 11.00000 0.04241 AFIX 66 C47 1 0.869141 0.666139 0.153163 11.00000 0.04791 C48 1 0.978784 0.643146 0.138456 11.00000 0.03420 C49 1 1.022677 0.662396 0.078497 11.00000 0.03915 C50 1 0.956930 0.704638 0.033247 11.00000 0.07688 C51 1 0.847287 0.727632 0.047954 11.00000 0.04027 C52 1 0.803391 0.708383 0.107912 11.00000 0.04356 AFIX 66 C53 1 0.700262 0.507641 0.153054 11.00000 0.04504 C58 1 0.747532 0.420064 0.110644 11.00000 0.03896 C57 1 0.676840 0.335674 0.051020 11.00000 0.04320 C56 1 0.558879 0.338860 0.033807 11.00000 0.06913 C55 1 0.511607 0.426436 0.076217 11.00000 0.04307 C54 1 0.582297 0.510827 0.135840 11.00000 0.04072 AFIX 0 B1 3 0.804255 0.620296 0.221581 11.00000 0.04096 HKLF 4 REM dy60_hp2_38deg_a.res in P-1 REM wR2 = 0.2397, GooF = S = 1.083, Restrained GooF = 1.088 for all data REM R1 = 0.0861 for 1429 Fo > 4sig(Fo) and 0.1329 for all 2069 data REM 278 parameters refined using 36 restraints END WGHT 0.1279 20.3648 REM Highest difference peak 0.650, deepest hole -0.951, 1-sigma level 0.110 Q1 1 0.6756 0.9826 0.7096 11.00000 0.05 0.65 Q2 1 0.6998 0.9963 0.7397 11.00000 0.05 0.61 Q3 1 0.7590 0.9994 0.7473 11.00000 0.05 0.58 Q4 1 0.5388 0.7603 0.7238 11.00000 0.05 0.56 Q5 1 0.8416 0.9351 0.7363 11.00000 0.05 0.55 Q6 1 0.6047 0.7010 0.7184 11.00000 0.05 0.54 Q7 1 0.6719 0.7017 0.7011 11.00000 0.05 0.54 Q8 1 0.8179 0.9337 0.7056 11.00000 0.05 0.54 Q9 1 0.7785 0.9783 0.7081 11.00000 0.05 0.52 Q10 1 0.6904 0.7160 0.7257 11.00000 0.05 0.51 Q11 1 1.0429 0.5244 0.1338 11.00000 0.05 0.49 Q12 1 1.0541 0.5399 0.1601 11.00000 0.05 0.48 Q13 1 0.7638 0.9867 0.9196 11.00000 0.05 0.40 Q14 1 0.7927 0.9799 0.8708 11.00000 0.05 0.36 Q15 1 0.8201 1.2230 0.8204 11.00000 0.05 0.36 Q16 1 0.6407 0.6021 0.6908 11.00000 0.05 0.36 Q17 1 0.3651 0.5828 0.5781 11.00000 0.05 0.36 Q18 1 0.3769 0.5844 0.5979 11.00000 0.05 0.35 Q19 1 0.8830 0.8572 0.7245 11.00000 0.05 0.34 Q20 1 0.6954 0.3851 0.0881 11.00000 0.05 0.34 ; _shelx_res_checksum 90986 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 2.150 _oxdiff_exptl_absorpt_empirical_full_min 0.664 # start Validation Reply Form _vrf_THETM01_dy60_hp2 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_PLAT029_dy60_hp2 ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.379 Why? RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_PLAT201_dy60_hp2 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 45 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT088_dy60_hp2 ; PROBLEM: Poor Data / Parameter Ratio .................... 7.44 Note RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT342_dy60_hp2 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.04707 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT911_dy60_hp2 ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.500 2180 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; # end Validation Reply Form _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_dy60_hp4 _database_code_depnum_ccdc_archive 'CCDC 2046709' loop_ _audit_author_name _audit_author_address 'Andreas M. Thiel' ;Aarhus University, Department of Chemistry Denmark ; _audit_update_record ; 2022-10-30 deposited with the CCDC. 2023-02-13 downloaded from the CCDC. ; _audit_creation_date 2020-03-04 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C34 H58 Dy, B C24 F20' _chemical_formula_sum 'C58 H58 B Dy F20' _chemical_formula_weight 1308.35 _chemical_melting_point ? 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.429(5) _cell_length_b 12.062(6) _cell_length_c 19.312(10) _cell_angle_alpha 106.754(18) _cell_angle_beta 95.037(17) _cell_angle_gamma 100.632(10) _cell_volume 2477(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2212 _cell_measurement_temperature 293 _cell_measurement_theta_max 7.05 _cell_measurement_theta_min 2.17 _shelx_estimated_absorpt_T_max 0.923 _shelx_estimated_absorpt_T_min 0.706 _exptl_absorpt_correction_T_max 0.7433 _exptl_absorpt_correction_T_min 0.4974 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS Empirical absorption correction using spherical harmonics, implemented using SADABS. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1314 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_ambient_pressure 1500000 _diffrn_reflns_av_R_equivalents 0.0859 _diffrn_reflns_av_unetI/netI 0.0597 _diffrn_reflns_Laue_measured_fraction_full 0.387 _diffrn_reflns_Laue_measured_fraction_max 0.387 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 11757 _diffrn_reflns_point_group_measured_fraction_full 0.387 _diffrn_reflns_point_group_measured_fraction_max 0.387 _diffrn_reflns_theta_full 20.860 _diffrn_reflns_theta_max 20.860 _diffrn_reflns_theta_min 1.804 _diffrn_ambient_temperature 293 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.387 _diffrn_measured_fraction_theta_max 0.387 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1693 _reflns_number_total 2020 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _refine_diff_density_max 1.913 _refine_diff_density_min -1.867 _refine_diff_density_rms 0.258 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.786 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 273 _refine_ls_number_reflns 2020 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.1090 _refine_ls_restrained_S_all 1.793 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2929 _refine_ls_wR_factor_ref 0.3764 _refine_special_details ? _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. Restrained planarity C54, C55, C56, C57, C58, F16, F17, F18, F19, F20, B1, C53 with sigma of 0.1 C47, C52, C51, C50, C49, C48, F15, F14, F13, F12, F11, B1 with sigma of 0.1 C35, C36, C37, C38, C39, C40, F1, F2, F3, F4, F5, B1 with sigma of 0.1 C41, C46, C45, C44, C43, C42, F10, F9, F8, F7, F6, B1 with sigma of 0.1 3.a Me refined with riding coordinates: C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C24(H24A,H24B, H24C), C25(H25A,H25B,H25C) 3.b Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C20(H20), C22(H22) 3.c Fitted pentagon refined as free rotating group: C1(C2,C3,C4,C5), C21(C20,C19,C18,C22) 3.d Fitted hexagon refined as free rotating group: C35(C40,C39,C38,C37,C36), C41(C42,C43,C44,C45,C46), C47(C48,C49,C50,C51,C52), C53(C58,C57,C56,C55,C54) 3.e Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C26(H26A,H26B,H26C), C28(H28A,H28B, H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A, H33B,H33C), C34(H34A,H34B,H34C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 0.68734(13) 0.84753(12) 0.72143(18) 0.0384(19) Uani 1 1 d . . . . . C1 C 0.5649(16) 0.9988(10) 0.7238(15) 0.000(6) Uiso 1 1 d . . . . . C2 C 0.508(2) 0.9294(15) 0.7648(15) 0.015(7) Uiso 1 1 d G . . . . C3 C 0.4518(18) 0.8157(12) 0.7155(16) 0.011(6) Uiso 1 1 d G . . . . H3 H 0.408281 0.752804 0.727822 0.013 Uiso 1 1 calc R . . . . C4 C 0.4735(18) 0.8148(13) 0.6441(15) 0.016(7) Uiso 1 1 d G . . . . C5 C 0.5434(19) 0.9280(15) 0.6492(15) 0.016(7) Uiso 1 1 d G . . . . H5 H 0.570314 0.951573 0.610534 0.020 Uiso 1 1 calc R . . . . C6 C 0.652(2) 1.127(2) 0.753(4) 0.015(7) Uiso 1 1 d . . . . . C7 C 0.771(2) 1.109(2) 0.788(3) 0.017(7) Uiso 1 1 d . . . . . H7A H 0.801093 1.051676 0.752844 0.025 Uiso 1 1 calc R . . . . H7B H 0.829150 1.182920 0.804876 0.025 Uiso 1 1 calc R . . . . H7C H 0.756479 1.080629 0.829208 0.025 Uiso 1 1 calc R . . . . C8 C 0.607(3) 1.222(2) 0.815(4) 0.015(7) Uiso 1 1 d . . . . . H8A H 0.531808 1.234244 0.795525 0.022 Uiso 1 1 calc GR . . . . H8B H 0.665961 1.295750 0.829754 0.022 Uiso 1 1 calc GR . . . . H8C H 0.596912 1.193793 0.855834 0.022 Uiso 1 1 calc GR . . . . C9 C 0.680(3) 1.165(3) 0.683(4) 0.033(9) Uiso 1 1 d . . . . . H9A H 0.716463 1.107751 0.651693 0.049 Uiso 1 1 calc GR . . . . H9B H 0.733913 1.241641 0.697540 0.049 Uiso 1 1 calc GR . . . . H9C H 0.606290 1.168706 0.656090 0.049 Uiso 1 1 calc GR . . . . C10 C 0.479(3) 0.953(3) 0.830(5) 0.041(10) Uiso 1 1 d . . . . . C11 C 0.586(3) 1.022(3) 0.912(4) 0.040(9) Uiso 1 1 d . . . . . H11A H 0.639344 0.970846 0.916154 0.060 Uiso 1 1 calc GR . . . . H11B H 0.544325 1.036920 0.953389 0.060 Uiso 1 1 calc GR . . . . H11C H 0.631896 1.095991 0.909593 0.060 Uiso 1 1 calc GR . . . . C12 C 0.423(3) 0.842(2) 0.860(4) 0.018(7) Uiso 1 1 d . . . . . H12A H 0.342130 0.806177 0.835759 0.027 Uiso 1 1 calc GR . . . . H12B H 0.423828 0.870648 0.911613 0.027 Uiso 1 1 calc GR . . . . H12C H 0.471533 0.783147 0.849219 0.027 Uiso 1 1 calc GR . . . . C13 C 0.381(4) 1.031(4) 0.852(6) 0.078(15) Uiso 1 1 d . . . . . H13A H 0.370430 1.039869 0.902237 0.117 Uiso 1 1 calc R . . . . H13B H 0.408305 1.108392 0.847158 0.117 Uiso 1 1 calc R . . . . H13C H 0.305658 0.992965 0.821030 0.117 Uiso 1 1 calc R . . . . C14 C 0.411(3) 0.720(2) 0.573(4) 0.021(8) Uiso 1 1 d . . . . . C15 C 0.510(4) 0.654(4) 0.538(7) 0.070(14) Uiso 1 1 d . . . . . H15A H 0.534759 0.682214 0.498958 0.105 Uiso 1 1 calc GR . . . . H15B H 0.476900 0.570181 0.519850 0.105 Uiso 1 1 calc GR . . . . H15C H 0.578507 0.669779 0.575050 0.105 Uiso 1 1 calc GR . . . . C16 C 0.365(4) 0.767(3) 0.508(5) 0.055(11) Uiso 1 1 d . . . . . H16A H 0.356052 0.846695 0.528028 0.083 Uiso 1 1 calc GR . . . . H16B H 0.288570 0.716815 0.482897 0.083 Uiso 1 1 calc GR . . . . H16C H 0.422153 0.763953 0.474445 0.083 Uiso 1 1 calc GR . . . . C17 C 0.325(4) 0.633(4) 0.591(6) 0.078(15) Uiso 1 1 d . . . . . H17A H 0.284948 0.572145 0.546449 0.116 Uiso 1 1 calc R . . . . H17B H 0.366254 0.597811 0.621478 0.116 Uiso 1 1 calc R . . . . H17C H 0.267144 0.670259 0.615775 0.116 Uiso 1 1 calc R . . . . C21 C 0.852(2) 0.7937(17) 0.6343(18) 0.022(8) Uiso 1 1 d . . . . . C20 C 0.9133(17) 0.8726(13) 0.7028(19) 0.018(7) Uiso 1 1 d G . . . . H20 H 0.959316 0.948525 0.711020 0.021 Uiso 1 1 calc R . . . . C19 C 0.8923(19) 0.8152(15) 0.7567(18) 0.010(6) Uiso 1 1 d G . . . . C18 C 0.8176(17) 0.7008(13) 0.7214(19) 0.003(6) Uiso 1 1 d G . . . . C22 C 0.7925(18) 0.6876(13) 0.6458(18) 0.018(7) Uiso 1 1 d G . . . . H22 H 0.745567 0.621018 0.610043 0.021 Uiso 1 1 calc R . . . . C23 C 0.745(3) 0.602(3) 0.752(4) 0.029(9) Uiso 1 1 d . . . . . C24 C 0.630(3) 0.658(3) 0.785(4) 0.033(8) Uiso 1 1 d . . . . . H24A H 0.660319 0.726635 0.826817 0.050 Uiso 1 1 calc R . . . . H24B H 0.586106 0.679189 0.747962 0.050 Uiso 1 1 calc R . . . . H24C H 0.576955 0.599029 0.799205 0.050 Uiso 1 1 calc R . . . . C25 C 0.829(4) 0.575(3) 0.811(5) 0.050(11) Uiso 1 1 d . . . . . H25A H 0.859613 0.646449 0.850790 0.076 Uiso 1 1 calc R . . . . H25B H 0.783569 0.515877 0.828007 0.076 Uiso 1 1 calc R . . . . H25C H 0.894130 0.546689 0.788995 0.076 Uiso 1 1 calc R . . . . C26 C 0.690(3) 0.492(3) 0.685(4) 0.038(9) Uiso 1 1 d . . . . . H26A H 0.638860 0.512984 0.651729 0.057 Uiso 1 1 calc GR . . . . H26B H 0.644650 0.431082 0.701354 0.057 Uiso 1 1 calc GR . . . . H26C H 0.754244 0.462961 0.661857 0.057 Uiso 1 1 calc GR . . . . C27 C 0.961(3) 0.864(2) 0.828(4) 0.023(8) Uiso 1 1 d . . . . . C28 C 0.879(3) 0.877(2) 0.888(4) 0.025(8) Uiso 1 1 d . . . . . H28A H 0.884319 0.959538 0.912587 0.038 Uiso 1 1 calc GR . . . . H28B H 0.904650 0.840022 0.923107 0.038 Uiso 1 1 calc GR . . . . H28C H 0.797220 0.839177 0.866455 0.038 Uiso 1 1 calc GR . . . . C29 C 1.023(3) 0.991(3) 0.839(5) 0.042(10) Uiso 1 1 d . . . . . H29A H 1.070699 0.993669 0.800566 0.063 Uiso 1 1 calc GR . . . . H29B H 1.073244 1.023670 0.885328 0.063 Uiso 1 1 calc GR . . . . H29C H 0.963000 1.037425 0.836656 0.063 Uiso 1 1 calc GR . . . . C30 C 1.060(3) 0.799(3) 0.845(4) 0.034(9) Uiso 1 1 d . . . . . H30A H 1.039660 0.718560 0.813552 0.052 Uiso 1 1 calc GR . . . . H30B H 1.066043 0.801078 0.894970 0.052 Uiso 1 1 calc GR . . . . H30C H 1.135530 0.838727 0.836002 0.052 Uiso 1 1 calc GR . . . . C31 C 0.874(3) 0.819(2) 0.558(4) 0.016(7) Uiso 1 1 d . . . . . C32 C 0.818(5) 0.925(4) 0.557(6) 0.062(12) Uiso 1 1 d . . . . . H32A H 0.751771 0.899809 0.517946 0.093 Uiso 1 1 calc GR . . . . H32B H 0.877913 0.985912 0.549631 0.093 Uiso 1 1 calc GR . . . . H32C H 0.790430 0.954821 0.602781 0.093 Uiso 1 1 calc GR . . . . C33 C 0.830(4) 0.700(3) 0.492(5) 0.057(12) Uiso 1 1 d . . . . . H33A H 0.858484 0.637194 0.504625 0.085 Uiso 1 1 calc GR . . . . H33B H 0.860568 0.710691 0.449558 0.085 Uiso 1 1 calc GR . . . . H33C H 0.743351 0.680444 0.483158 0.085 Uiso 1 1 calc GR . . . . C34 C 1.014(4) 0.866(4) 0.564(5) 0.058(12) Uiso 1 1 d . . . . . H34A H 1.039240 0.939665 0.602161 0.087 Uiso 1 1 calc GR . . . . H34B H 1.031116 0.876887 0.518076 0.087 Uiso 1 1 calc GR . . . . H34C H 1.055360 0.808638 0.573850 0.087 Uiso 1 1 calc GR . . . . F1 F 0.7817(15) 0.3861(12) 0.2519(19) 0.024(4) Uiso 1 1 d . . . . . F2 F 0.9279(18) 0.3569(16) 0.352(2) 0.048(6) Uiso 1 1 d . . . . . F3 F 1.100(2) 0.5355(18) 0.443(3) 0.064(7) Uiso 1 1 d . . . . . F4 F 1.1377(19) 0.7475(16) 0.420(2) 0.047(5) Uiso 1 1 d . . . . . F5 F 1.0009(15) 0.7791(14) 0.310(2) 0.031(5) Uiso 1 1 d . . . . . F6 F 0.8393(15) 0.8934(14) 0.2569(19) 0.029(4) Uiso 1 1 d . . . . . F7 F 0.7368(16) 1.0289(15) 0.349(2) 0.039(5) Uiso 1 1 d . . . . . F8 F 0.5905(18) 0.9360(16) 0.429(2) 0.048(6) Uiso 1 1 d . . . . . F9 F 0.535(2) 0.7067(18) 0.410(3) 0.057(6) Uiso 1 1 d . . . . . F10 F 0.6331(15) 0.5624(14) 0.3073(19) 0.030(5) Uiso 1 1 d . . . . . F11 F 1.0486(15) 0.6032(13) 0.1775(19) 0.025(4) Uiso 1 1 d . . . . . F12 F 1.1281(18) 0.6267(16) 0.065(2) 0.044(5) Uiso 1 1 d . . . . . F13 F 0.996(2) 0.7092(19) -0.027(3) 0.066(7) Uiso 1 1 d . . . . . F14 F 0.7822(16) 0.7693(15) 0.005(2) 0.038(5) Uiso 1 1 d . . . . . F15 F 0.7003(16) 0.7349(13) 0.117(2) 0.035(5) Uiso 1 1 d . . . . . F16 F 0.5294(14) 0.5902(13) 0.1731(18) 0.020(4) Uiso 1 1 d . . . . . F17 F 0.4013(19) 0.4361(17) 0.057(2) 0.052(6) Uiso 1 1 d . . . . . F18 F 0.493(2) 0.2602(18) -0.026(3) 0.066(7) Uiso 1 1 d . . . . . F19 F 0.7209(17) 0.2498(15) 0.007(2) 0.042(5) Uiso 1 1 d . . . . . F20 F 0.8613(17) 0.4174(15) 0.128(2) 0.043(5) Uiso 1 1 d . . . . . C35 C 0.8856(14) 0.5900(14) 0.2783(15) 0.002(6) Uiso 1 1 d . . . . . C40 C 0.9795(15) 0.6810(11) 0.3215(16) 0.020(8) Uiso 1 1 d G . . . . C39 C 1.0535(15) 0.6616(14) 0.3759(15) 0.032(9) Uiso 1 1 d G . . . . C38 C 1.0337(18) 0.5512(17) 0.3870(15) 0.054(12) Uiso 1 1 d G . . . . C37 C 0.9398(18) 0.4603(12) 0.3438(16) 0.026(8) Uiso 1 1 d G . . . . C36 C 0.8658(15) 0.4797(12) 0.2894(16) 0.069(15) Uiso 1 1 d G . . . . C41 C 0.7388(15) 0.7161(12) 0.2783(14) 0.001(6) Uiso 1 1 d . . . . . C42 C 0.7661(17) 0.8373(13) 0.2882(15) 0.062(14) Uiso 1 1 d G . . . . C43 C 0.7152(18) 0.9132(10) 0.3395(16) 0.021(8) Uiso 1 1 d G . . . . C44 C 0.6369(17) 0.8678(12) 0.3808(14) 0.051(11) Uiso 1 1 d G . . . . C45 C 0.6096(15) 0.7465(13) 0.3708(14) 0.015(7) Uiso 1 1 d G . . . . C46 C 0.6605(15) 0.6707(10) 0.3195(14) 0.005(6) Uiso 1 1 d G . . . . C47 C 0.8709(15) 0.6682(14) 0.1549(14) 0.016(7) Uiso 1 1 d . . . . . C48 C 0.9805(14) 0.6414(13) 0.1385(15) 0.018(7) Uiso 1 1 d G . . . . C49 C 1.0226(13) 0.6566(14) 0.0757(15) 0.025(8) Uiso 1 1 d G . . . . C50 C 0.9551(17) 0.6984(14) 0.0294(14) 0.030(8) Uiso 1 1 d G . . . . C51 C 0.8456(16) 0.7251(13) 0.0458(15) 0.022(7) Uiso 1 1 d G . . . . C52 C 0.8035(12) 0.7100(13) 0.1086(15) 0.024(8) Uiso 1 1 d G . . . . C53 C 0.6970(14) 0.5094(13) 0.1531(14) 0.018(7) Uiso 1 1 d . . . . . C58 C 0.7456(12) 0.4204(14) 0.1104(16) 0.019(7) Uiso 1 1 d G . . . . C57 C 0.6750(18) 0.3352(13) 0.0491(15) 0.037(9) Uiso 1 1 d G . . . . C56 C 0.5559(18) 0.3390(15) 0.0306(14) 0.049(11) Uiso 1 1 d G . . . . C55 C 0.5073(12) 0.4281(15) 0.0733(16) 0.030(8) Uiso 1 1 d G . . . . C54 C 0.5779(14) 0.5133(12) 0.1346(15) 0.004(6) Uiso 1 1 d G . . . . B1 B 0.804(3) 0.624(3) 0.225(3) 0.030(10) Uiso 1 1 d . . . . . 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 0.0314(13) 0.0287(12) 0.065(6) 0.0254(16) 0.0183(17) 0.0090(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 2.489(19) . ? Dy1 C2 2.54(2) . ? Dy1 C3 2.64(2) . ? Dy1 C4 2.65(2) . ? Dy1 C5 2.56(2) . ? Dy1 C21 2.67(3) . ? Dy1 C20 2.61(2) . ? Dy1 C19 2.51(2) . ? Dy1 C18 2.514(19) . ? Dy1 C22 2.62(2) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 C6 1.59(3) . ? C2 C3 1.4200 . ? C2 C10 1.30(8) . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C4 C14 1.52(6) . ? C6 C7 1.55(6) . ? C6 C8 1.59(6) . ? C6 C9 1.60(10) . ? C10 C11 1.79(10) . ? C10 C12 1.65(5) . ? C10 C13 1.61(6) . ? C14 C15 1.58(6) . ? C14 C16 1.60(11) . ? C14 C17 1.44(6) . ? C21 C20 1.4200 . ? C21 C22 1.4200 . ? C21 C31 1.62(7) . ? C20 C19 1.4200 . ? C19 C18 1.4200 . ? C19 C27 1.43(7) . ? C18 C22 1.4200 . ? C18 C23 1.61(4) . ? C23 C24 1.67(5) . ? C23 C25 1.56(10) . ? C23 C26 1.54(8) . ? C27 C28 1.54(7) . ? C27 C29 1.52(4) . ? C27 C30 1.55(5) . ? C31 C32 1.53(5) . ? C31 C33 1.57(8) . ? C31 C34 1.58(4) . ? F1 C36 1.31(2) . ? F2 C37 1.29(2) . ? F3 C38 1.35(5) . ? F4 C39 1.30(3) . ? F5 C40 1.25(2) . ? F6 C42 1.28(3) . ? F7 C43 1.325(19) . ? F8 C44 1.28(3) . ? F9 C45 1.31(3) . ? F10 C46 1.232(18) . ? F11 C48 1.27(3) . ? F12 C49 1.34(2) . ? F13 C50 1.26(5) . ? F14 C51 1.30(4) . ? F15 C52 1.28(2) . ? F16 C54 1.26(3) . ? F17 C55 1.25(3) . ? F18 C56 1.27(4) . ? F19 C57 1.34(3) . ? F20 C58 1.35(3) . ? C35 C40 1.3900 . ? C35 C36 1.3900 . ? C35 B1 1.52(5) . ? C40 C39 1.3900 . ? C39 C38 1.3900 . ? C38 C37 1.3900 . ? C37 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 B1 1.63(4) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C47 B1 1.77(5) . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C53 C58 1.3900 . ? C53 C54 1.3900 . ? C53 B1 1.82(4) . ? C58 C57 1.3900 . ? C57 C56 1.3900 . ? C56 C55 1.3900 . ? C55 C54 1.3900 . ? 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 C1 Dy1 C2 32.8(3) . . ? C1 Dy1 C3 53.2(3) . . ? C1 Dy1 C4 53.0(3) . . ? C1 Dy1 C5 32.6(3) . . ? C1 Dy1 C21 127.0(7) . . ? C1 Dy1 C20 125.1(4) . . ? C1 Dy1 C19 145.1(6) . . ? C1 Dy1 C18 177.9(6) . . ? C1 Dy1 C22 148.7(10) . . ? C2 Dy1 C3 31.8(3) . . ? C2 Dy1 C4 52.5(3) . . ? C2 Dy1 C5 53.6(3) . . ? C2 Dy1 C21 157.9(9) . . ? C2 Dy1 C20 152.3(5) . . ? C2 Dy1 C22 154.8(6) . . ? C3 Dy1 C4 31.2(2) . . ? C3 Dy1 C21 139.9(9) . . ? C4 Dy1 C21 111.2(9) . . ? C5 Dy1 C3 52.5(3) . . ? C5 Dy1 C4 31.6(3) . . ? C5 Dy1 C21 104.4(8) . . ? C5 Dy1 C20 119.9(8) . . ? C5 Dy1 C22 117.0(9) . . ? C20 Dy1 C3 170.0(10) . . ? C20 Dy1 C4 138.9(10) . . ? C20 Dy1 C21 31.1(3) . . ? C20 Dy1 C22 52.1(4) . . ? C19 Dy1 C2 146.8(10) . . ? C19 Dy1 C3 155.3(7) . . ? C19 Dy1 C4 159.3(8) . . ? C19 Dy1 C5 152.0(7) . . ? C19 Dy1 C21 52.5(3) . . ? C19 Dy1 C20 32.1(2) . . ? C19 Dy1 C18 32.8(3) . . ? C19 Dy1 C22 53.2(3) . . ? C18 Dy1 C2 148.1(7) . . ? C18 Dy1 C3 128.7(4) . . ? C18 Dy1 C4 129.0(7) . . ? C18 Dy1 C5 148.7(10) . . ? C18 Dy1 C21 52.5(3) . . ? C18 Dy1 C20 53.2(3) . . ? C18 Dy1 C22 32.1(2) . . ? C22 Dy1 C3 123.0(6) . . ? C22 Dy1 C4 106.2(8) . . ? C22 Dy1 C21 31.1(3) . . ? C2 C1 Dy1 75.4(9) . . ? C2 C1 C6 128(3) . . ? C5 C1 Dy1 76.5(10) . . ? C5 C1 C2 108.0 . . ? C5 C1 C6 123(3) . . ? C6 C1 Dy1 108.9(14) . . ? C1 C2 Dy1 71.8(8) . . ? C3 C2 Dy1 78.0(7) . . ? C3 C2 C1 108.0 . . ? C10 C2 Dy1 128(3) . . ? C10 C2 C1 134.6(19) . . ? C10 C2 C3 115.8(19) . . ? C2 C3 Dy1 70.2(8) . . ? C2 C3 C4 108.0 . . ? C4 C3 Dy1 75.0(10) . . ? C3 C4 Dy1 73.8(9) . . ? C3 C4 C14 126(2) . . ? C5 C4 Dy1 70.8(6) . . ? C5 C4 C3 108.0 . . ? C5 C4 C14 125(2) . . ? C14 C4 Dy1 130.7(16) . . ? C1 C5 Dy1 70.9(9) . . ? C1 C5 C4 108.0 . . ? C4 C5 Dy1 77.7(6) . . ? C1 C6 C9 106(5) . . ? C7 C6 C1 105.3(19) . . ? C7 C6 C8 107(4) . . ? C7 C6 C9 107(3) . . ? C8 C6 C1 115(2) . . ? C8 C6 C9 115(3) . . ? C2 C10 C11 124(3) . . ? C2 C10 C12 119(3) . . ? C2 C10 C13 121(6) . . ? C12 C10 C11 92(5) . . ? C13 C10 C11 97(5) . . ? C13 C10 C12 98(3) . . ? C4 C14 C15 107(4) . . ? C4 C14 C16 117(3) . . ? C15 C14 C16 101(6) . . ? C17 C14 C4 108(6) . . ? C17 C14 C15 106(3) . . ? C17 C14 C16 116(4) . . ? C20 C21 Dy1 72.0(9) . . ? C20 C21 C22 108.0 . . ? C20 C21 C31 122.0(19) . . ? C22 C21 Dy1 72.2(6) . . ? C22 C21 C31 128.8(19) . . ? C31 C21 Dy1 131.0(17) . . ? C21 C20 Dy1 76.8(10) . . ? C21 C20 C19 108.0 . . ? C19 C20 Dy1 70.1(10) . . ? C20 C19 Dy1 77.8(9) . . ? C20 C19 C27 120(2) . . ? C18 C19 Dy1 73.7(7) . . ? C18 C19 C20 108.0 . . ? C18 C19 C27 130.2(18) . . ? C27 C19 Dy1 125(2) . . ? C19 C18 Dy1 73.5(8) . . ? C19 C18 C23 133(3) . . ? C22 C18 Dy1 77.9(11) . . ? C22 C18 C19 108.0 . . ? C22 C18 C23 118(3) . . ? C23 C18 Dy1 106.4(14) . . ? C21 C22 Dy1 76.7(7) . . ? C21 C22 C18 108.0 . . ? C18 C22 Dy1 70.0(10) . . ? C18 C23 C24 105(2) . . ? C25 C23 C18 111(3) . . ? C25 C23 C24 114(6) . . ? C26 C23 C18 107(5) . . ? C26 C23 C24 107(3) . . ? C26 C23 C25 113(3) . . ? C19 C27 C28 112(3) . . ? C19 C27 C29 108(5) . . ? C19 C27 C30 116(4) . . ? C28 C27 C30 110(5) . . ? C29 C27 C28 103(4) . . ? C29 C27 C30 107(3) . . ? C32 C31 C21 106(5) . . ? C32 C31 C33 118(6) . . ? C32 C31 C34 105(3) . . ? C33 C31 C21 110(3) . . ? C33 C31 C34 110(4) . . ? C34 C31 C21 107(5) . . ? C40 C35 C36 120.0 . . ? C40 C35 B1 115.5(15) . . ? C36 C35 B1 124.3(14) . . ? F5 C40 C35 120.6(19) . . ? F5 C40 C39 119.3(19) . . ? C35 C40 C39 120.0 . . ? F4 C39 C40 121.0(19) . . ? F4 C39 C38 118.9(19) . . ? C38 C39 C40 120.0 . . ? F3 C38 C39 119.6(16) . . ? F3 C38 C37 120.2(16) . . ? C39 C38 C37 120.0 . . ? F2 C37 C38 119(2) . . ? F2 C37 C36 121(2) . . ? C38 C37 C36 120.0 . . ? F1 C36 C35 126.1(18) . . ? F1 C36 C37 113.9(18) . . ? C37 C36 C35 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 B1 122.7(14) . . ? C46 C41 B1 117.1(14) . . ? F6 C42 C41 127.7(14) . . ? F6 C42 C43 112.2(15) . . ? C43 C42 C41 120.0 . . ? F7 C43 C42 121.6(19) . . ? F7 C43 C44 118.3(18) . . ? C44 C43 C42 120.0 . . ? F8 C44 C43 121.3(15) . . ? F8 C44 C45 118.7(15) . . ? C43 C44 C45 120.0 . . ? F9 C45 C44 118.5(15) . . ? F9 C45 C46 121.5(15) . . ? C46 C45 C44 120.0 . . ? F10 C46 C41 118.9(17) . . ? F10 C46 C45 121.0(17) . . ? C45 C46 C41 120.0 . . ? C48 C47 C52 120.0 . . ? C48 C47 B1 119.8(15) . . ? C52 C47 B1 119.2(16) . . ? F11 C48 C47 124.6(19) . . ? F11 C48 C49 115.4(19) . . ? C47 C48 C49 120.0 . . ? F12 C49 C48 115(2) . . ? F12 C49 C50 125(2) . . ? C50 C49 C48 120.0 . . ? F13 C50 C49 118(2) . . ? F13 C50 C51 122(2) . . ? C51 C50 C49 120.0 . . ? F14 C51 C50 122(2) . . ? F14 C51 C52 118(2) . . ? C50 C51 C52 120.0 . . ? F15 C52 C47 126(2) . . ? F15 C52 C51 114(2) . . ? C51 C52 C47 120.0 . . ? C58 C53 C54 120.0 . . ? C58 C53 B1 114.9(15) . . ? C54 C53 B1 124.7(14) . . ? F20 C58 C53 119.7(19) . . ? F20 C58 C57 120.3(19) . . ? C57 C58 C53 120.0 . . ? F19 C57 C58 120.6(18) . . ? F19 C57 C56 119.4(18) . . ? C58 C57 C56 120.0 . . ? F18 C56 C57 118.8(18) . . ? F18 C56 C55 121.2(18) . . ? C57 C56 C55 120.0 . . ? F17 C55 C56 121(2) . . ? F17 C55 C54 119(2) . . ? C54 C55 C56 120.0 . . ? F16 C54 C53 122.0(16) . . ? F16 C54 C55 118.0(16) . . ? C55 C54 C53 120.0 . . ? C35 B1 C41 103(3) . . ? C35 B1 C47 117(2) . . ? C35 B1 C53 120.3(18) . . ? C41 B1 C47 117.5(19) . . ? C41 B1 C53 112.0(19) . . ? C47 B1 C53 87(2) . . ? _shelx_res_file ; TITL hp4_2_a.res in P-1 hp4_2.res created by SHELXL-2018/3 at 10:47:59 on 04-Mar-2020 REM Old TITL C:\bn\HP4_2 in P-1 REM SHELXT solution in P-1: R1 0.186, Rweak 0.027, Alpha 0.094 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C63 B2 F21 Dy CELL 0.71073 11.4287 12.0619 19.312 106.754 95.037 100.632 ZERR 2 0.0051 0.0055 0.0099 0.018 0.017 0.01 LATT 1 SFAC C H B Dy F UNIT 116 116 2 2 40 FLAT C54 C55 C56 C57 C58 F16 F17 F18 F19 F20 B1 C53 FLAT C47 C52 C51 C50 C49 C48 F15 F14 F13 F12 F11 B1 FLAT C35 C36 C37 C38 C39 C40 F1 F2 F3 F4 F5 B1 FLAT C41 C46 C45 C44 C43 C42 F10 F9 F8 F7 F6 B1 L.S. 20 0 0 PLAN 20 SIZE 0.16 0.23 0.05 FREE Dy1 C24 FREE Dy1 C7 list 4 fmap 2 53 acta SHEL 100 0.83 OMIT 0 180 REM REM REM WGHT 0.200000 FVAR 0.32787 DY1 4 0.687342 0.847527 0.721427 11.00000 0.03140 0.02868 = 0.06537 0.02539 0.01828 0.00901 AFIX 56 C1 1 0.564896 0.998769 0.723830 11.00000 -0.00002 C2 1 0.508317 0.929362 0.764785 11.00000 0.01545 C3 1 0.451824 0.815666 0.715494 11.00000 0.01058 AFIX 43 H3 2 0.408281 0.752804 0.727822 11.00000 -1.20000 AFIX 55 C4 1 0.473490 0.814807 0.644075 11.00000 0.01638 C5 1 0.543373 0.927970 0.649227 11.00000 0.01649 AFIX 43 H5 2 0.570314 0.951573 0.610534 11.00000 -1.20000 AFIX 0 C6 1 0.651534 1.127139 0.753183 11.00000 0.01466 C7 1 0.770949 1.108847 0.788384 11.00000 0.01656 AFIX 33 H7A 2 0.801093 1.051676 0.752844 11.00000 -1.50000 H7B 2 0.829150 1.182920 0.804876 11.00000 -1.50000 H7C 2 0.756479 1.080629 0.829208 11.00000 -1.50000 AFIX 0 C8 1 0.607180 1.222096 0.814634 11.00000 0.01495 AFIX 137 H8A 2 0.531808 1.234244 0.795525 11.00000 -1.50000 H8B 2 0.665961 1.295750 0.829754 11.00000 -1.50000 H8C 2 0.596912 1.193793 0.855834 11.00000 -1.50000 AFIX 0 C9 1 0.679882 1.165102 0.682571 11.00000 0.03292 AFIX 137 H9A 2 0.716463 1.107751 0.651693 11.00000 -1.50000 H9B 2 0.733913 1.241641 0.697540 11.00000 -1.50000 H9C 2 0.606290 1.168706 0.656090 11.00000 -1.50000 AFIX 0 C10 1 0.479055 0.952799 0.829934 11.00000 0.04113 C11 1 0.586086 1.022200 0.911773 11.00000 0.04005 AFIX 137 H11A 2 0.639344 0.970846 0.916154 11.00000 -1.50000 H11B 2 0.544325 1.036920 0.953389 11.00000 -1.50000 H11C 2 0.631896 1.095991 0.909593 11.00000 -1.50000 AFIX 0 C12 1 0.423290 0.841526 0.859758 11.00000 0.01768 AFIX 137 H12A 2 0.342130 0.806177 0.835759 11.00000 -1.50000 H12B 2 0.423828 0.870648 0.911613 11.00000 -1.50000 H12C 2 0.471533 0.783147 0.849219 11.00000 -1.50000 AFIX 0 C13 1 0.380988 1.031422 0.852346 11.00000 0.07812 AFIX 33 H13A 2 0.370430 1.039869 0.902237 11.00000 -1.50000 H13B 2 0.408305 1.108392 0.847158 11.00000 -1.50000 H13C 2 0.305658 0.992965 0.821030 11.00000 -1.50000 AFIX 0 C14 1 0.411417 0.720168 0.572834 11.00000 0.02099 C15 1 0.510123 0.654072 0.538266 11.00000 0.07006 AFIX 137 H15A 2 0.534759 0.682214 0.498958 11.00000 -1.50000 H15B 2 0.476900 0.570181 0.519850 11.00000 -1.50000 H15C 2 0.578507 0.669779 0.575050 11.00000 -1.50000 AFIX 0 C16 1 0.364903 0.766538 0.508085 11.00000 0.05532 AFIX 137 H16A 2 0.356052 0.846695 0.528028 11.00000 -1.50000 H16B 2 0.288570 0.716815 0.482897 11.00000 -1.50000 H16C 2 0.422153 0.763953 0.474445 11.00000 -1.50000 AFIX 0 C17 1 0.325219 0.632773 0.590625 11.00000 0.07755 AFIX 33 H17A 2 0.284948 0.572145 0.546449 11.00000 -1.50000 H17B 2 0.366254 0.597811 0.621478 11.00000 -1.50000 H17C 2 0.267144 0.670259 0.615775 11.00000 -1.50000 AFIX 56 C21 1 0.851607 0.793721 0.634297 11.00000 0.02205 C20 1 0.913264 0.872593 0.702834 11.00000 0.01758 AFIX 43 H20 2 0.959316 0.948525 0.711020 11.00000 -1.20000 AFIX 55 C19 1 0.892260 0.815167 0.756679 11.00000 0.00957 C18 1 0.817621 0.700806 0.721419 11.00000 0.00271 C22 1 0.792496 0.687551 0.645783 11.00000 0.01758 AFIX 43 H22 2 0.745567 0.621018 0.610043 11.00000 -1.20000 AFIX 0 C23 1 0.744514 0.601988 0.752196 11.00000 0.02950 C24 1 0.629745 0.657640 0.785045 11.00000 0.03329 AFIX 33 H24A 2 0.660319 0.726635 0.826817 11.00000 -1.50000 H24B 2 0.586106 0.679189 0.747962 11.00000 -1.50000 H24C 2 0.576955 0.599029 0.799205 11.00000 -1.50000 AFIX 0 C25 1 0.828538 0.575172 0.810616 11.00000 0.05045 AFIX 33 H25A 2 0.859613 0.646449 0.850790 11.00000 -1.50000 H25B 2 0.783569 0.515877 0.828007 11.00000 -1.50000 H25C 2 0.894130 0.546689 0.788995 11.00000 -1.50000 AFIX 0 C26 1 0.690470 0.491869 0.685493 11.00000 0.03786 AFIX 137 H26A 2 0.638860 0.512984 0.651729 11.00000 -1.50000 H26B 2 0.644650 0.431082 0.701354 11.00000 -1.50000 H26C 2 0.754244 0.462961 0.661857 11.00000 -1.50000 AFIX 0 C27 1 0.960667 0.863722 0.828312 11.00000 0.02329 C28 1 0.879017 0.876852 0.888267 11.00000 0.02536 AFIX 137 H28A 2 0.884319 0.959538 0.912587 11.00000 -1.50000 H28B 2 0.904650 0.840022 0.923107 11.00000 -1.50000 H28C 2 0.797220 0.839177 0.866455 11.00000 -1.50000 AFIX 0 C29 1 1.022599 0.991362 0.838668 11.00000 0.04197 AFIX 137 H29A 2 1.070699 0.993669 0.800566 11.00000 -1.50000 H29B 2 1.073244 1.023670 0.885328 11.00000 -1.50000 H29C 2 0.963000 1.037425 0.836656 11.00000 -1.50000 AFIX 0 C30 1 1.059881 0.799426 0.844769 11.00000 0.03441 AFIX 137 H30A 2 1.039660 0.718560 0.813552 11.00000 -1.50000 H30B 2 1.066043 0.801078 0.894970 11.00000 -1.50000 H30C 2 1.135530 0.838727 0.836002 11.00000 -1.50000 AFIX 0 C31 1 0.873829 0.818582 0.558078 11.00000 0.01618 C32 1 0.818287 0.924716 0.557009 11.00000 0.06231 AFIX 137 H32A 2 0.751771 0.899809 0.517946 11.00000 -1.50000 H32B 2 0.877913 0.985912 0.549631 11.00000 -1.50000 H32C 2 0.790430 0.954821 0.602781 11.00000 -1.50000 AFIX 0 C33 1 0.829759 0.700176 0.492453 11.00000 0.05696 AFIX 137 H33A 2 0.858484 0.637194 0.504625 11.00000 -1.50000 H33B 2 0.860568 0.710691 0.449558 11.00000 -1.50000 H33C 2 0.743351 0.680444 0.483158 11.00000 -1.50000 AFIX 0 C34 1 1.013535 0.865530 0.563579 11.00000 0.05793 AFIX 137 H34A 2 1.039240 0.939665 0.602161 11.00000 -1.50000 H34B 2 1.031116 0.876887 0.518076 11.00000 -1.50000 H34C 2 1.055360 0.808638 0.573850 11.00000 -1.50000 AFIX 0 F1 5 0.781730 0.386079 0.251890 11.00000 0.02369 F2 5 0.927900 0.356861 0.352499 11.00000 0.04770 F3 5 1.100382 0.535491 0.443088 11.00000 0.06364 F4 5 1.137712 0.747539 0.419811 11.00000 0.04731 F5 5 1.000893 0.779088 0.310417 11.00000 0.03087 F6 5 0.839329 0.893350 0.256945 11.00000 0.02889 F7 5 0.736838 1.028855 0.349223 11.00000 0.03852 F8 5 0.590548 0.936030 0.429470 11.00000 0.04768 F9 5 0.535252 0.706686 0.410220 11.00000 0.05654 F10 5 0.633075 0.562384 0.307305 11.00000 0.02979 F11 5 1.048626 0.603218 0.177507 11.00000 0.02544 F12 5 1.128135 0.626699 0.065239 11.00000 0.04442 F13 5 0.996415 0.709239 -0.027404 11.00000 0.06553 F14 5 0.782212 0.769326 0.005371 11.00000 0.03850 F15 5 0.700349 0.734923 0.116904 11.00000 0.03527 F16 5 0.529412 0.590212 0.173089 11.00000 0.02004 F17 5 0.401275 0.436080 0.056607 11.00000 0.05232 F18 5 0.493228 0.260219 -0.025964 11.00000 0.06623 F19 5 0.720875 0.249785 0.007221 11.00000 0.04161 F20 5 0.861333 0.417381 0.128445 11.00000 0.04295 AFIX 66 C35 1 0.885601 0.590030 0.278286 11.00000 0.00239 C40 1 0.979468 0.680996 0.321521 11.00000 0.02027 C39 1 1.053499 0.661602 0.375900 11.00000 0.03243 C38 1 1.033663 0.551242 0.387046 11.00000 0.05365 C37 1 0.939796 0.460275 0.343812 11.00000 0.02608 C36 1 0.865764 0.479668 0.289432 11.00000 0.06858 AFIX 66 C41 1 0.738805 0.716077 0.278257 11.00000 0.00051 C42 1 0.766133 0.837334 0.288249 11.00000 0.06235 C43 1 0.715190 0.913183 0.339527 11.00000 0.02106 C44 1 0.636919 0.867775 0.380812 11.00000 0.05107 C45 1 0.609590 0.746518 0.370820 11.00000 0.01452 C46 1 0.660532 0.670668 0.319543 11.00000 0.00532 AFIX 66 C47 1 0.870930 0.668155 0.154946 11.00000 0.01568 C48 1 0.980485 0.641448 0.138494 11.00000 0.01791 C49 1 1.022573 0.656561 0.075713 11.00000 0.02506 C50 1 0.955106 0.698381 0.029383 11.00000 0.03008 C51 1 0.845550 0.725088 0.045834 11.00000 0.02161 C52 1 0.803461 0.709975 0.108615 11.00000 0.02394 AFIX 66 C53 1 0.697036 0.509434 0.153099 11.00000 0.01819 C58 1 0.745604 0.420375 0.110383 11.00000 0.01922 C57 1 0.675015 0.335159 0.049130 11.00000 0.03718 C56 1 0.555857 0.339001 0.030592 11.00000 0.04923 C55 1 0.507289 0.428060 0.073307 11.00000 0.03046 C54 1 0.577877 0.513276 0.134561 11.00000 0.00357 AFIX 0 B1 3 0.804476 0.623804 0.225066 11.00000 0.03035 HKLF 4 REM hp4_2_a.res in P-1 REM wR2 = 0.3764, GooF = S = 1.786, Restrained GooF = 1.793 for all data REM R1 = 0.1090 for 1693 Fo > 4sig(Fo) and 0.1424 for all 2020 data REM 273 parameters refined using 36 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.913, deepest hole -1.867, 1-sigma level 0.258 Q1 1 0.8218 1.0582 0.7238 11.00000 0.05 1.91 Q2 1 0.5552 0.6386 0.7189 11.00000 0.05 1.89 Q3 1 0.5468 0.6273 0.6935 11.00000 0.05 1.89 Q4 1 0.8354 1.0806 0.7533 11.00000 0.05 1.76 Q5 1 0.9261 1.2191 0.7568 11.00000 0.05 1.50 Q6 1 0.5365 0.5004 0.2870 11.00000 0.05 1.30 Q7 1 0.5568 0.5193 0.3163 11.00000 0.05 1.30 Q8 1 0.6805 0.8313 0.7099 11.00000 0.05 1.29 Q9 1 0.9978 0.6471 0.2539 11.00000 0.05 1.13 Q10 1 0.6098 0.6398 0.2548 11.00000 0.05 1.12 Q11 1 1.0132 0.6584 0.2787 11.00000 0.05 1.09 Q12 1 0.8839 0.5050 0.2324 11.00000 0.05 1.06 Q13 1 0.6267 0.6834 0.3203 11.00000 0.05 1.02 Q14 1 0.6354 0.6911 0.3451 11.00000 0.05 1.00 Q15 1 0.7738 0.9429 0.7960 11.00000 0.05 0.99 Q16 1 0.8200 0.9454 0.3161 11.00000 0.05 0.95 Q17 1 0.7444 0.7967 0.3234 11.00000 0.05 0.94 Q18 1 0.8255 0.9558 0.3376 11.00000 0.05 0.92 Q19 1 0.8531 0.7145 0.1294 11.00000 0.05 0.92 Q20 1 0.8205 0.3607 0.2359 11.00000 0.05 0.90 ; _shelx_res_checksum 14807 _olex2_submission_special_instructions 'No special instructions were received' # start Validation Reply Form _vrf_THETM01_dy60_hp4 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_PLAT029_dy60_hp4 ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.387 Why? RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_PLAT201_dy60_hp4 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 45 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT413_dy60_hp4 ; PROBLEM: Short Inter XH3 .. XHn H8C ..H11C . 1.85 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT084_dy60_hp4 ; PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.38 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT088_dy60_hp4 ; PROBLEM: Poor Data / Parameter Ratio .................... 7.40 Note RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT220_dy60_hp4 ; PROBLEM: NonSolvent Resd 1 C Ueq(max) / Ueq(min) Range 10.0 Ratio RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT221_dy60_hp4 ; PROBLEM: Solv./Anion Resd 2 C Ueq(max)/Ueq(min) Range 10.0 Ratio RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT241_dy60_hp4 ; PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of C36 Check RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT342_dy60_hp4 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.04772 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT911_dy60_hp4 ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.501 2546 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT973_dy60_hp4 ; PROBLEM: Check Calcd Positive Resid. Density on Dy1 1.60 eA-3 RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; # end Validation Reply Form _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_dy60_hp5 _database_code_depnum_ccdc_archive 'CCDC 2046711' loop_ _audit_author_name _audit_author_address 'Andreas M. Thiel' ;Aarhus University, Department of Chemistry Denmark ; _audit_update_record ; 2022-10-30 deposited with the CCDC. 2023-02-13 downloaded from the CCDC. ; _audit_creation_date 2020-02-25 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C34 H58 Dy, B C24 F20' _chemical_formula_sum 'C58 H58 B Dy F20' _chemical_formula_weight 1308.35 _chemical_melting_point ? _chemical_oxdiff_formula C58H58BDyF20 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.355(2) _cell_length_b 12.014(3) _cell_length_c 19.033(13) _cell_angle_alpha 107.39(4) _cell_angle_beta 95.26(4) _cell_angle_gamma 100.76(2) _cell_volume 2404.1(19) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1266 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20.7090 _cell_measurement_theta_min 1.8410 _shelx_estimated_absorpt_T_max 0.921 _shelx_estimated_absorpt_T_min 0.699 _exptl_absorpt_coefficient_mu 1.675 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.26995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1314 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_ambient_pressure 2120000 _diffrn_reflns_av_R_equivalents 0.2226 _diffrn_reflns_av_unetI/netI 0.1590 _diffrn_reflns_Laue_measured_fraction_full 0.378 _diffrn_reflns_Laue_measured_fraction_max 0.378 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 15564 _diffrn_reflns_point_group_measured_fraction_full 0.378 _diffrn_reflns_point_group_measured_fraction_max 0.378 _diffrn_reflns_theta_full 20.809 _diffrn_reflns_theta_max 20.809 _diffrn_reflns_theta_min 1.810 _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3590 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.378 _diffrn_measured_fraction_theta_max 0.378 _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 -37.00 25.00 1.00 30.00 -- 7.60 39.00 167.00 62 2 \w -13.00 54.00 1.00 30.00 -- 7.60 -38.00-180.00 67 3 \w -13.00 34.00 1.00 30.00 -- 7.60 -38.00-150.00 47 4 \w -1.00 58.00 1.00 30.00 -- 7.60 -97.00-143.00 59 5 \w -35.00 -12.00 1.00 30.00 -- 7.60 77.00 -30.00 23 6 \w -51.00 9.00 1.00 30.00 -- -8.46 81.00 151.00 60 7 \w -19.00 33.00 1.00 30.00 -- -8.46 -53.00-162.00 52 8 \w 3.00 42.00 1.00 30.00 -- -8.46 -99.00-120.00 39 9 \w -1.00 42.00 1.00 30.00 -- -8.46 -97.00 35.00 43 10 \w 12.00 35.00 1.00 30.00 -- 7.60 -77.00 30.00 23 11 \w 34.00 58.00 1.00 30.00 -- 7.60 -99.00 60.00 24 12 \w -33.00 20.00 1.00 30.00 -- 7.60 53.00 -17.00 53 13 \w 34.00 58.00 1.00 30.00 -- 7.60 -99.00 30.00 24 14 \w -35.00 -12.00 1.00 30.00 -- -8.46 77.00 -30.00 23 15 \w -24.00 37.00 1.00 30.00 -- -8.46 -39.00 12.00 61 16 \w -35.00 -12.00 1.00 30.00 -- -8.46 77.00 120.00 23 17 \w -49.00 5.00 1.00 30.00 -- -8.46 53.00 -17.00 54 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0151638000 _diffrn_orient_matrix_UB_12 -0.0156776000 _diffrn_orient_matrix_UB_13 -0.0392365000 _diffrn_orient_matrix_UB_21 -0.0296490000 _diffrn_orient_matrix_UB_22 -0.0585004000 _diffrn_orient_matrix_UB_23 -0.0018650000 _diffrn_orient_matrix_UB_31 -0.0551028000 _diffrn_orient_matrix_UB_32 0.0190764000 _diffrn_orient_matrix_UB_33 0.0045362000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1117 _reflns_number_total 1902 _reflns_odcompleteness_completeness 38.35 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 20.77 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.822 _refine_diff_density_min -1.273 _refine_diff_density_rms 0.140 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 276 _refine_ls_number_reflns 1902 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.2120 _refine_ls_R_factor_gt 0.1400 _refine_ls_restrained_S_all 1.250 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3216 _refine_ls_wR_factor_ref 0.3679 _refine_special_details ? _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. Restrained planarity C54, C55, C56, C57, C58, F16, F17, F18, F19, F20, B1, C53 with sigma of 0.1 C47, C52, C51, C50, C49, C48, F15, F14, F13, F12, F11, B1 with sigma of 0.1 C35, C36, C37, C38, C39, C40, F1, F2, F3, F4, F5, B1 with sigma of 0.1 C41, C46, C45, C44, C43, C42, F10, F9, F8, F7, F6, B1 with sigma of 0.1 3.a Me refined with riding coordinates: C8(H8A,H8B,H8C), C12(H12A,H12B,H12C) 3.b Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C20(H20), C22(H22) 3.c Fitted pentagon refined as free rotating group: C1(C2,C3,C4,C5), C21(C20,C19,C18,C22) 3.d Fitted hexagon refined as free rotating group: C35(C40,C39,C38,C37,C36), C41(C42,C43,C44,C45,C46), C47(C48,C49,C50,C51,C52), C53(C58,C57,C56,C55,C54) 3.e Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C24(H24A,H24B, H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A, H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.69091(19) 0.8459(2) 0.7235(3) 0.115(5) Uani 1 1 d . . . . . C1 C 0.569(2) 0.992(2) 0.718(3) 0.048(11) Uiso 1 1 d . . . . . C2 C 0.511(3) 0.936(3) 0.765(3) 0.053(12) Uiso 1 1 d G . . . . C3 C 0.449(3) 0.818(3) 0.722(3) 0.098(18) Uiso 1 1 d G . . . . H3 H 0.404222 0.761569 0.739349 0.117 Uiso 1 1 calc R . . . . C4 C 0.468(3) 0.801(2) 0.647(3) 0.054(12) Uiso 1 1 d G . . . . C5 C 0.542(3) 0.908(3) 0.644(3) 0.077(14) Uiso 1 1 d G . . . . H5 H 0.567739 0.921526 0.601975 0.092 Uiso 1 1 calc R . . . . C6 C 0.651(4) 1.128(3) 0.763(5) 0.055(12) Uiso 1 1 d . . . . . C7 C 0.775(4) 1.108(4) 0.796(6) 0.084(15) Uiso 1 1 d . . . . . H7A H 0.777534 1.118968 0.848238 0.126 Uiso 1 1 calc GR . . . . H7B H 0.841158 1.164187 0.788989 0.126 Uiso 1 1 calc GR . . . . H7C H 0.782392 1.027829 0.770567 0.126 Uiso 1 1 calc GR . . . . C8 C 0.604(4) 1.218(4) 0.811(6) 0.091(16) Uiso 1 1 d . . . . . H8A H 0.528782 1.222823 0.786246 0.137 Uiso 1 1 calc R . . . . H8B H 0.590255 1.198350 0.855633 0.137 Uiso 1 1 calc R . . . . H8C H 0.661045 1.293411 0.824314 0.137 Uiso 1 1 calc R . . . . C9 C 0.679(4) 1.165(4) 0.690(6) 0.076(14) Uiso 1 1 d . . . . . H9A H 0.702059 1.100833 0.654380 0.114 Uiso 1 1 calc GR . . . . H9B H 0.743384 1.235643 0.704089 0.114 Uiso 1 1 calc GR . . . . H9C H 0.607054 1.181366 0.667735 0.114 Uiso 1 1 calc GR . . . . C10 C 0.472(4) 0.949(3) 0.839(5) 0.037(10) Uiso 1 1 d . . . . . C11 C 0.585(4) 1.002(4) 0.897(6) 0.081(15) Uiso 1 1 d . . . . . H11A H 0.617926 0.938303 0.906220 0.121 Uiso 1 1 calc GR . . . . H11B H 0.565896 1.050489 0.942438 0.121 Uiso 1 1 calc GR . . . . H11C H 0.644457 1.049938 0.878815 0.121 Uiso 1 1 calc GR . . . . C12 C 0.421(4) 0.839(4) 0.868(6) 0.085(15) Uiso 1 1 d . . . . . H12A H 0.401227 0.869236 0.917193 0.127 Uiso 1 1 calc R . . . . H12B H 0.349423 0.788466 0.834753 0.127 Uiso 1 1 calc R . . . . H12C H 0.481747 0.793536 0.869456 0.127 Uiso 1 1 calc R . . . . C13 C 0.376(4) 1.026(5) 0.856(7) 0.074(13) Uiso 1 1 d . . . . . H13A H 0.352534 1.047644 0.813170 0.110 Uiso 1 1 calc GR . . . . H13B H 0.411004 1.097825 0.897501 0.110 Uiso 1 1 calc GR . . . . H13C H 0.306619 0.981730 0.868595 0.110 Uiso 1 1 calc GR . . . . C14 C 0.424(4) 0.709(4) 0.576(6) 0.063(13) Uiso 1 1 d . . . . . C15 C 0.521(3) 0.656(4) 0.531(5) 0.054(11) Uiso 1 1 d . . . . . H15A H 0.547553 0.703373 0.500577 0.081 Uiso 1 1 calc GR . . . . H15B H 0.485094 0.575118 0.499992 0.081 Uiso 1 1 calc GR . . . . H15C H 0.588714 0.656408 0.565201 0.081 Uiso 1 1 calc GR . . . . C16 C 0.355(4) 0.754(4) 0.517(6) 0.076(14) Uiso 1 1 d . . . . . H16A H 0.276708 0.762589 0.529637 0.114 Uiso 1 1 calc GR . . . . H16B H 0.345016 0.695758 0.468038 0.114 Uiso 1 1 calc GR . . . . H16C H 0.401352 0.829091 0.516861 0.114 Uiso 1 1 calc GR . . . . C17 C 0.336(5) 0.604(4) 0.580(7) 0.104(18) Uiso 1 1 d . . . . . H17A H 0.374314 0.568772 0.612902 0.156 Uiso 1 1 calc GR . . . . H17B H 0.311639 0.545454 0.531350 0.156 Uiso 1 1 calc GR . . . . H17C H 0.266642 0.628370 0.599054 0.156 Uiso 1 1 calc GR . . . . C21 C 0.860(3) 0.795(3) 0.633(3) 0.069(14) Uiso 1 1 d . . . . . C20 C 0.922(2) 0.873(2) 0.704(3) 0.042(11) Uiso 1 1 d G . . . . H20 H 0.970521 0.948592 0.714138 0.051 Uiso 1 1 calc R . . . . C19 C 0.896(3) 0.814(3) 0.758(3) 0.067(14) Uiso 1 1 d G . . . . C18 C 0.818(3) 0.700(3) 0.720(3) 0.055(13) Uiso 1 1 d G . . . . C22 C 0.796(2) 0.688(2) 0.643(3) 0.066(15) Uiso 1 1 d G . . . . H22 H 0.748160 0.622142 0.605301 0.079 Uiso 1 1 calc R . . . . C23 C 0.748(4) 0.605(3) 0.747(5) 0.052(11) Uiso 1 1 d . . . . . C24 C 0.646(3) 0.658(3) 0.787(5) 0.056(11) Uiso 1 1 d . . . . . H24A H 0.675874 0.742696 0.811335 0.083 Uiso 1 1 calc GR . . . . H24B H 0.624482 0.619998 0.822879 0.083 Uiso 1 1 calc GR . . . . H24C H 0.576260 0.644671 0.750395 0.083 Uiso 1 1 calc GR . . . . C25 C 0.825(4) 0.562(5) 0.787(7) 0.095(17) Uiso 1 1 d . . . . . H25A H 0.839306 0.488694 0.755690 0.142 Uiso 1 1 calc GR . . . . H25B H 0.789504 0.548264 0.828565 0.142 Uiso 1 1 calc GR . . . . H25C H 0.900990 0.620192 0.805646 0.142 Uiso 1 1 calc GR . . . . C26 C 0.690(4) 0.483(4) 0.681(6) 0.087(16) Uiso 1 1 d . . . . . H26A H 0.649817 0.500275 0.640581 0.131 Uiso 1 1 calc GR . . . . H26B H 0.632078 0.432773 0.699079 0.131 Uiso 1 1 calc GR . . . . H26C H 0.752810 0.442809 0.665165 0.131 Uiso 1 1 calc GR . . . . C27 C 0.964(5) 0.866(5) 0.824(7) 0.082(16) Uiso 1 1 d . . . . . C28 C 0.890(5) 0.881(5) 0.892(7) 0.094(16) Uiso 1 1 d . . . . . H28A H 0.838555 0.935885 0.890236 0.141 Uiso 1 1 calc GR . . . . H28B H 0.945205 0.912211 0.938066 0.141 Uiso 1 1 calc GR . . . . H28C H 0.840644 0.804971 0.888453 0.141 Uiso 1 1 calc GR . . . . C29 C 1.043(5) 1.002(4) 0.859(7) 0.095(17) Uiso 1 1 d . . . . . H29A H 1.124609 1.004333 0.850183 0.142 Uiso 1 1 calc GR . . . . H29B H 1.041791 1.029194 0.912045 0.142 Uiso 1 1 calc GR . . . . H29C H 1.007931 1.051918 0.836584 0.142 Uiso 1 1 calc GR . . . . C30 C 1.070(4) 0.809(4) 0.853(6) 0.090(16) Uiso 1 1 d . . . . . H30A H 1.043356 0.723794 0.838194 0.135 Uiso 1 1 calc GR . . . . H30B H 1.089162 0.841052 0.906635 0.135 Uiso 1 1 calc GR . . . . H30C H 1.141760 0.829529 0.832094 0.135 Uiso 1 1 calc GR . . . . C31 C 0.874(4) 0.820(4) 0.555(6) 0.055(12) Uiso 1 1 d . . . . . C32 C 0.819(4) 0.917(4) 0.548(6) 0.082(15) Uiso 1 1 d . . . . . H32A H 0.762442 0.931460 0.582255 0.123 Uiso 1 1 calc GR . . . . H32B H 0.776560 0.895746 0.497746 0.123 Uiso 1 1 calc GR . . . . H32C H 0.880925 0.988794 0.557931 0.123 Uiso 1 1 calc GR . . . . C33 C 0.834(3) 0.712(3) 0.488(5) 0.052(11) Uiso 1 1 d . . . . . H33A H 0.875013 0.651040 0.493735 0.079 Uiso 1 1 calc GR . . . . H33B H 0.854068 0.731794 0.444653 0.079 Uiso 1 1 calc GR . . . . H33C H 0.748069 0.682097 0.482132 0.079 Uiso 1 1 calc GR . . . . C34 C 1.017(4) 0.872(5) 0.558(8) 0.105(18) Uiso 1 1 d . . . . . H34A H 1.047230 0.937688 0.603205 0.157 Uiso 1 1 calc GR . . . . H34B H 1.028142 0.898636 0.515916 0.157 Uiso 1 1 calc GR . . . . H34C H 1.059611 0.809720 0.556675 0.157 Uiso 1 1 calc GR . . . . F1 F 0.7800(19) 0.3895(18) 0.257(3) 0.065(6) Uiso 1 1 d . . . . . F2 F 0.929(2) 0.361(2) 0.361(3) 0.086(8) Uiso 1 1 d . . . . . F3 F 1.108(3) 0.539(2) 0.445(3) 0.108(10) Uiso 1 1 d . . . . . F4 F 1.147(2) 0.759(2) 0.421(3) 0.076(7) Uiso 1 1 d . . . . . F5 F 1.004(2) 0.7887(19) 0.316(3) 0.069(7) Uiso 1 1 d . . . . . F6 F 0.843(2) 0.895(2) 0.248(3) 0.075(7) Uiso 1 1 d . . . . . F7 F 0.7301(18) 1.0398(19) 0.343(3) 0.070(7) Uiso 1 1 d . . . . . F8 F 0.5820(19) 0.9536(19) 0.433(3) 0.073(7) Uiso 1 1 d . . . . . F9 F 0.527(2) 0.723(2) 0.411(3) 0.097(9) Uiso 1 1 d . . . . . F10 F 0.6251(19) 0.5704(19) 0.311(3) 0.070(7) Uiso 1 1 d . . . . . F11 F 1.0525(18) 0.6112(17) 0.186(3) 0.056(6) Uiso 1 1 d . . . . . F12 F 1.124(2) 0.620(2) 0.064(3) 0.099(9) Uiso 1 1 d . . . . . F13 F 0.988(3) 0.696(3) -0.031(4) 0.128(11) Uiso 1 1 d . . . . . F14 F 0.782(2) 0.7624(19) 0.001(3) 0.073(7) Uiso 1 1 d . . . . . F15 F 0.7001(19) 0.7387(18) 0.125(3) 0.068(7) Uiso 1 1 d . . . . . F16 F 0.521(2) 0.596(2) 0.176(3) 0.070(7) Uiso 1 1 d . . . . . F17 F 0.401(2) 0.442(2) 0.057(3) 0.090(8) Uiso 1 1 d . . . . . F18 F 0.492(2) 0.268(2) -0.031(3) 0.098(9) Uiso 1 1 d . . . . . F19 F 0.723(2) 0.255(2) 0.009(3) 0.083(8) Uiso 1 1 d . . . . . F20 F 0.857(2) 0.4137(19) 0.122(3) 0.071(7) Uiso 1 1 d . . . . . C35 C 0.885(2) 0.592(2) 0.284(2) 0.045(10) Uiso 1 1 d . . . . . C40 C 0.980(3) 0.6862(18) 0.327(2) 0.099(17) Uiso 1 1 d G . . . . C39 C 1.058(2) 0.670(2) 0.382(2) 0.066(13) Uiso 1 1 d G . . . . C38 C 1.041(2) 0.559(3) 0.393(2) 0.082(15) Uiso 1 1 d G . . . . C37 C 0.947(3) 0.465(2) 0.350(2) 0.081(15) Uiso 1 1 d G . . . . C36 C 0.869(2) 0.4819(19) 0.296(2) 0.062(13) Uiso 1 1 d G . . . . C41 C 0.737(2) 0.728(2) 0.280(2) 0.057(12) Uiso 1 1 d . . . . . C42 C 0.762(2) 0.849(2) 0.290(2) 0.081(15) Uiso 1 1 d G . . . . C43 C 0.707(2) 0.9251(17) 0.340(2) 0.057(12) Uiso 1 1 d G . . . . C44 C 0.628(2) 0.879(2) 0.381(2) 0.078(14) Uiso 1 1 d G . . . . C45 C 0.603(2) 0.758(2) 0.372(2) 0.048(11) Uiso 1 1 d G . . . . C46 C 0.658(2) 0.6817(16) 0.322(2) 0.069(13) Uiso 1 1 d G . . . . C47 C 0.875(2) 0.6710(19) 0.157(2) 0.050(11) Uiso 1 1 d . . . . . C48 C 0.984(2) 0.6439(18) 0.139(2) 0.066(14) Uiso 1 1 d G . . . . C49 C 1.0222(18) 0.6552(18) 0.073(2) 0.058(12) Uiso 1 1 d G . . . . C50 C 0.951(3) 0.6936(19) 0.026(2) 0.071(15) Uiso 1 1 d G . . . . C51 C 0.841(2) 0.7208(18) 0.044(2) 0.053(12) Uiso 1 1 d G . . . . C52 C 0.8034(17) 0.7095(18) 0.110(2) 0.070(14) Uiso 1 1 d G . . . . C53 C 0.697(2) 0.510(2) 0.152(2) 0.059(12) Uiso 1 1 d . . . . . C58 C 0.7450(19) 0.421(3) 0.107(2) 0.089(16) Uiso 1 1 d G . . . . C57 C 0.673(3) 0.337(2) 0.044(2) 0.067(13) Uiso 1 1 d G . . . . C56 C 0.553(3) 0.341(2) 0.025(2) 0.066(13) Uiso 1 1 d G . . . . C55 C 0.5053(19) 0.430(2) 0.070(2) 0.057(12) Uiso 1 1 d G . . . . C54 C 0.577(2) 0.515(2) 0.133(2) 0.045(11) Uiso 1 1 d G . . . . B1 B 0.797(4) 0.637(3) 0.233(3) 0.066(15) Uiso 1 1 d . . . . . 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 0.0582(18) 0.0816(19) 0.222(15) 0.071(4) 0.025(4) 0.0183(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 2.45(2) . ? Dy1 C2 2.56(3) . ? Dy1 C3 2.70(3) . ? Dy1 C4 2.68(4) . ? Dy1 C5 2.53(4) . ? Dy1 C21 2.72(4) . ? Dy1 C20 2.65(2) . ? Dy1 C19 2.49(4) . ? Dy1 C18 2.46(2) . ? Dy1 C22 2.61(3) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 C6 1.65(6) . ? C2 C3 1.4200 . ? C2 C10 1.49(9) . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C4 C14 1.44(10) . ? C6 C7 1.58(8) . ? C6 C8 1.41(8) . ? C6 C9 1.63(12) . ? C10 C11 1.51(11) . ? C10 C12 1.61(7) . ? C10 C13 1.55(5) . ? C14 C15 1.56(7) . ? C14 C16 1.59(11) . ? C14 C17 1.49(5) . ? C21 C20 1.4200 . ? C21 C22 1.4200 . ? C21 C31 1.62(9) . ? C20 C19 1.4200 . ? C19 C18 1.4200 . ? C19 C27 1.33(12) . ? C18 C22 1.4200 . ? C18 C23 1.52(6) . ? C23 C24 1.57(6) . ? C23 C25 1.38(9) . ? C23 C26 1.59(10) . ? C27 C28 1.59(13) . ? C27 C29 1.61(8) . ? C27 C30 1.62(8) . ? C31 C32 1.46(5) . ? C31 C33 1.49(10) . ? C31 C34 1.62(5) . ? F1 C36 1.32(4) . ? F2 C37 1.31(3) . ? F3 C38 1.30(6) . ? F4 C39 1.31(4) . ? F5 C40 1.29(3) . ? F6 C42 1.41(4) . ? F7 C43 1.33(2) . ? F8 C44 1.34(4) . ? F9 C45 1.28(4) . ? F10 C46 1.27(2) . ? F11 C48 1.33(5) . ? F12 C49 1.31(3) . ? F13 C50 1.20(7) . ? F14 C51 1.29(5) . ? F15 C52 1.32(3) . ? F16 C54 1.36(3) . ? F17 C55 1.23(3) . ? F18 C56 1.21(5) . ? F19 C57 1.26(3) . ? F20 C58 1.31(3) . ? C35 C40 1.3900 . ? C35 C36 1.3900 . ? C35 B1 1.61(6) . ? C40 C39 1.3900 . ? C39 C38 1.3900 . ? C38 C37 1.3900 . ? C37 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 B1 1.50(5) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C47 B1 1.87(6) . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C53 C58 1.3900 . ? C53 C54 1.3900 . ? C53 B1 1.90(6) . ? C58 C57 1.3900 . ? C57 C56 1.3900 . ? C56 C55 1.3900 . ? C55 C54 1.3900 . ? 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 C1 Dy1 C2 32.8(3) . . ? C1 Dy1 C3 52.7(4) . . ? C1 Dy1 C4 53.0(5) . . ? C1 Dy1 C5 33.1(4) . . ? C1 Dy1 C21 123.2(13) . . ? C1 Dy1 C20 123.9(8) . . ? C1 Dy1 C19 146.5(10) . . ? C1 Dy1 C18 175.3(17) . . ? C1 Dy1 C22 143.3(17) . . ? C2 Dy1 C3 31.2(3) . . ? C2 Dy1 C4 52.0(4) . . ? C2 Dy1 C21 155.1(13) . . ? C2 Dy1 C20 150.4(9) . . ? C2 Dy1 C22 155.7(12) . . ? C3 Dy1 C21 142.2(16) . . ? C4 Dy1 C3 30.6(3) . . ? C4 Dy1 C21 112.7(15) . . ? C5 Dy1 C2 53.7(3) . . ? C5 Dy1 C3 52.1(4) . . ? C5 Dy1 C4 31.5(4) . . ? C5 Dy1 C21 102.5(13) . . ? C5 Dy1 C20 120.4(14) . . ? C5 Dy1 C22 112.1(16) . . ? C20 Dy1 C3 171.6(18) . . ? C20 Dy1 C4 141.0(17) . . ? C20 Dy1 C21 30.6(3) . . ? C19 Dy1 C2 148.2(16) . . ? C19 Dy1 C3 155.2(13) . . ? C19 Dy1 C4 158.0(12) . . ? C19 Dy1 C5 152.0(14) . . ? C19 Dy1 C21 52.0(3) . . ? C19 Dy1 C20 31.8(3) . . ? C19 Dy1 C22 53.4(3) . . ? C18 Dy1 C2 151.4(12) . . ? C18 Dy1 C3 129.5(8) . . ? C18 Dy1 C4 126.1(13) . . ? C18 Dy1 C5 143.4(17) . . ? C18 Dy1 C21 52.3(4) . . ? C18 Dy1 C20 53.2(3) . . ? C18 Dy1 C19 33.3(4) . . ? C18 Dy1 C22 32.3(3) . . ? C22 Dy1 C3 125.0(11) . . ? C22 Dy1 C4 105.0(12) . . ? C22 Dy1 C21 30.8(4) . . ? C22 Dy1 C20 51.7(4) . . ? C2 C1 Dy1 77.9(12) . . ? C2 C1 C5 108.0 . . ? C2 C1 C6 112(4) . . ? C5 C1 Dy1 76.3(15) . . ? C5 C1 C6 140(4) . . ? C6 C1 Dy1 109(2) . . ? C1 C2 Dy1 69.3(11) . . ? C1 C2 C10 148(3) . . ? C3 C2 Dy1 79.7(11) . . ? C3 C2 C1 108.0 . . ? C3 C2 C10 103(3) . . ? C10 C2 Dy1 125(3) . . ? C2 C3 Dy1 69.1(11) . . ? C2 C3 C4 108.0 . . ? C4 C3 Dy1 73.9(14) . . ? C3 C4 Dy1 75.5(13) . . ? C3 C4 C14 137(4) . . ? C5 C4 Dy1 68.4(10) . . ? C5 C4 C3 108.0 . . ? C5 C4 C14 115(4) . . ? C14 C4 Dy1 124(3) . . ? C1 C5 Dy1 70.6(13) . . ? C1 C5 C4 108.0 . . ? C4 C5 Dy1 80.1(10) . . ? C7 C6 C1 105(3) . . ? C7 C6 C9 105(4) . . ? C8 C6 C1 123(3) . . ? C8 C6 C7 116(7) . . ? C8 C6 C9 109(4) . . ? C9 C6 C1 96(6) . . ? C2 C10 C11 106(4) . . ? C2 C10 C12 125(5) . . ? C2 C10 C13 114(6) . . ? C11 C10 C12 97(6) . . ? C11 C10 C13 111(7) . . ? C13 C10 C12 103(3) . . ? C4 C14 C15 117(5) . . ? C4 C14 C16 114(4) . . ? C4 C14 C17 113(8) . . ? C15 C14 C16 101(7) . . ? C17 C14 C15 105(4) . . ? C17 C14 C16 105(6) . . ? C20 C21 Dy1 72.0(13) . . ? C20 C21 C22 108.0 . . ? C20 C21 C31 125(3) . . ? C22 C21 Dy1 70.2(8) . . ? C22 C21 C31 127(3) . . ? C31 C21 Dy1 128(2) . . ? C21 C20 Dy1 77.5(15) . . ? C21 C20 C19 108.0 . . ? C19 C20 Dy1 67.8(14) . . ? C20 C19 Dy1 80.4(14) . . ? C18 C19 Dy1 72.3(9) . . ? C18 C19 C20 108.0 . . ? C27 C19 Dy1 125(4) . . ? C27 C19 C20 115(5) . . ? C27 C19 C18 136(4) . . ? C19 C18 Dy1 74.4(11) . . ? C19 C18 C23 132(5) . . ? C22 C18 Dy1 79.6(18) . . ? C22 C18 C19 108.0 . . ? C22 C18 C23 119(5) . . ? C23 C18 Dy1 105.8(18) . . ? C21 C22 Dy1 79.0(9) . . ? C21 C22 C18 108.0 . . ? C18 C22 Dy1 68.1(16) . . ? C18 C23 C24 107(3) . . ? C18 C23 C26 112(6) . . ? C24 C23 C26 111(4) . . ? C25 C23 C18 111(4) . . ? C25 C23 C24 117(7) . . ? C25 C23 C26 98(4) . . ? C19 C27 C28 114(5) . . ? C19 C27 C29 128(7) . . ? C19 C27 C30 122(6) . . ? C28 C27 C29 92(6) . . ? C28 C27 C30 100(8) . . ? C29 C27 C30 94(5) . . ? C32 C31 C21 113(6) . . ? C32 C31 C33 112(7) . . ? C32 C31 C34 103(3) . . ? C33 C31 C21 114(4) . . ? C33 C31 C34 107(6) . . ? C34 C31 C21 106(7) . . ? C40 C35 C36 120.0 . . ? C40 C35 B1 111(2) . . ? C36 C35 B1 128(2) . . ? F5 C40 C35 123(3) . . ? F5 C40 C39 117(3) . . ? C39 C40 C35 120.0 . . ? F4 C39 C40 119(3) . . ? F4 C39 C38 121(3) . . ? C40 C39 C38 120.0 . . ? F3 C38 C39 123(3) . . ? F3 C38 C37 117(3) . . ? C37 C38 C39 120.0 . . ? F2 C37 C38 121(3) . . ? F2 C37 C36 119(3) . . ? C36 C37 C38 120.0 . . ? F1 C36 C35 123(3) . . ? F1 C36 C37 117(3) . . ? C37 C36 C35 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 B1 126(2) . . ? C46 C41 B1 114(2) . . ? C41 C42 F6 119.5(19) . . ? C43 C42 F6 120(2) . . ? C43 C42 C41 120.0 . . ? F7 C43 C42 117(2) . . ? F7 C43 C44 123(2) . . ? C42 C43 C44 120.0 . . ? F8 C44 C43 120(2) . . ? F8 C44 C45 120(2) . . ? C45 C44 C43 120.0 . . ? F9 C45 C44 116(2) . . ? F9 C45 C46 124(2) . . ? C46 C45 C44 120.0 . . ? F10 C46 C41 122(2) . . ? F10 C46 C45 117(2) . . ? C45 C46 C41 120.0 . . ? C48 C47 C52 120.0 . . ? C48 C47 B1 126(2) . . ? C52 C47 B1 113(2) . . ? F11 C48 C47 119(3) . . ? F11 C48 C49 121(3) . . ? C49 C48 C47 120.0 . . ? F12 C49 C48 111(3) . . ? F12 C49 C50 129(3) . . ? C48 C49 C50 120.0 . . ? F13 C50 C49 115(3) . . ? F13 C50 C51 125(3) . . ? C49 C50 C51 120.0 . . ? F14 C51 C50 117(3) . . ? F14 C51 C52 123(3) . . ? C52 C51 C50 120.0 . . ? F15 C52 C47 123(3) . . ? F15 C52 C51 117(3) . . ? C51 C52 C47 120.0 . . ? C58 C53 C54 120.0 . . ? C58 C53 B1 121(2) . . ? C54 C53 B1 119(2) . . ? F20 C58 C53 122(3) . . ? F20 C58 C57 118(3) . . ? C53 C58 C57 120.0 . . ? F19 C57 C58 115(3) . . ? F19 C57 C56 125(3) . . ? C56 C57 C58 120.0 . . ? F18 C56 C57 119(3) . . ? F18 C56 C55 121(3) . . ? C57 C56 C55 120.0 . . ? F17 C55 C56 124(3) . . ? F17 C55 C54 116(3) . . ? C54 C55 C56 120.0 . . ? F16 C54 C53 124(3) . . ? F16 C54 C55 116(3) . . ? C55 C54 C53 120.0 . . ? C35 B1 C47 110(2) . . ? C35 B1 C53 113(2) . . ? C41 B1 C35 110(3) . . ? C41 B1 C47 120(3) . . ? C41 B1 C53 118(2) . . ? C47 B1 C53 83(2) . . ? _shelx_res_file ; TITL dy60_hp6a_38deg_a.res in P-1 dy60_hp6a_38deg.res created by SHELXL-2018/3 at 11:04:05 on 19-Feb-2020 REM Old TITL Dy60_HP6A_38deg in P-1 REM SHELXT solution in P-1: R1 0.269, Rweak 0.196, Alpha 0.194 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C54 B2 F20 Dy CELL 0.71073 11.3552 12.014 19.0334 107.385 95.257 100.761 ZERR 2 0.0024 0.0034 0.0128 0.044 0.036 0.021 LATT 1 SFAC C H B Dy F UNIT 116 116 2 2 40 FLAT C54 C55 C56 C57 C58 F16 F17 F18 F19 F20 B1 C53 FLAT C47 C52 C51 C50 C49 C48 F15 F14 F13 F12 F11 B1 FLAT C35 C36 C37 C38 C39 C40 F1 F2 F3 F4 F5 B1 FLAT C41 C46 C45 C44 C43 C42 F10 F9 F8 F7 F6 B1 L.S. 20 0 0 PLAN 20 SIZE 0.16 0.23 0.05 FREE Dy1 C24 FREE Dy1 C7 list 4 fmap 2 53 acta SHEL 100 0.83 OMIT 0 180 OMIT -2 -5 2 OMIT -6 2 1 OMIT -6 4 0 OMIT -7 1 1 OMIT -5 2 0 OMIT -9 2 1 OMIT 8 -7 1 OMIT -10 5 0 OMIT 10 0 0 OMIT 8 -3 1 OMIT 2 -8 3 OMIT -9 0 2 OMIT 0 -7 3 OMIT 7 -5 1 OMIT -8 1 2 OMIT 6 -9 2 OMIT -8 3 1 OMIT -4 -5 4 OMIT -7 -5 1 OMIT -7 6 0 OMIT 2 -7 3 OMIT 9 -7 2 OMIT 0 -9 4 OMIT 7 -6 2 OMIT 8 -6 1 OMIT -8 7 2 OMIT -2 -6 4 REM REM REM WGHT 0.200000 FVAR 0.38251 DY1 4 0.690908 0.845948 0.723479 11.00000 0.05823 0.08157 = 0.22168 0.07136 0.02526 0.01835 AFIX 56 C1 1 0.568590 0.991815 0.717531 11.00000 0.04826 C2 1 0.511492 0.935960 0.765500 11.00000 0.05332 C3 1 0.449272 0.817825 0.721902 11.00000 0.09763 AFIX 43 H3 2 0.404222 0.761569 0.739349 11.00000 -1.20000 AFIX 55 C4 1 0.467917 0.800670 0.646988 11.00000 0.05364 C5 1 0.541659 0.908201 0.644286 11.00000 0.07675 AFIX 43 H5 2 0.567739 0.921526 0.601975 11.00000 -1.20000 AFIX 0 C6 1 0.651137 1.127819 0.763429 11.00000 0.05499 C7 1 0.775169 1.107740 0.795985 11.00000 0.08385 AFIX 137 H7A 2 0.777534 1.118968 0.848238 11.00000 -1.50000 H7B 2 0.841158 1.164187 0.788989 11.00000 -1.50000 H7C 2 0.782392 1.027829 0.770567 11.00000 -1.50000 AFIX 0 C8 1 0.604019 1.217833 0.811248 11.00000 0.09136 AFIX 33 H8A 2 0.528782 1.222823 0.786246 11.00000 -1.50000 H8B 2 0.590255 1.198350 0.855633 11.00000 -1.50000 H8C 2 0.661045 1.293411 0.824314 11.00000 -1.50000 AFIX 0 C9 1 0.678755 1.165276 0.689821 11.00000 0.07626 AFIX 137 H9A 2 0.702059 1.100833 0.654380 11.00000 -1.50000 H9B 2 0.743384 1.235643 0.704089 11.00000 -1.50000 H9C 2 0.607054 1.181366 0.667735 11.00000 -1.50000 AFIX 0 C10 1 0.471811 0.948923 0.839375 11.00000 0.03705 C11 1 0.585395 1.001736 0.896972 11.00000 0.08078 AFIX 137 H11A 2 0.617926 0.938303 0.906220 11.00000 -1.50000 H11B 2 0.565896 1.050489 0.942438 11.00000 -1.50000 H11C 2 0.644457 1.049938 0.878815 11.00000 -1.50000 AFIX 0 C12 1 0.420933 0.838978 0.868083 11.00000 0.08480 AFIX 33 H12A 2 0.401227 0.869236 0.917193 11.00000 -1.50000 H12B 2 0.349423 0.788466 0.834753 11.00000 -1.50000 H12C 2 0.481747 0.793536 0.869456 11.00000 -1.50000 AFIX 0 C13 1 0.376404 1.026411 0.856269 11.00000 0.07363 AFIX 137 H13A 2 0.352534 1.047644 0.813170 11.00000 -1.50000 H13B 2 0.411004 1.097825 0.897501 11.00000 -1.50000 H13C 2 0.306619 0.981730 0.868595 11.00000 -1.50000 AFIX 0 C14 1 0.424163 0.709172 0.575926 11.00000 0.06317 C15 1 0.520704 0.655870 0.531094 11.00000 0.05429 AFIX 137 H15A 2 0.547553 0.703373 0.500577 11.00000 -1.50000 H15B 2 0.485094 0.575118 0.499992 11.00000 -1.50000 H15C 2 0.588714 0.656408 0.565201 11.00000 -1.50000 AFIX 0 C16 1 0.354967 0.753540 0.516766 11.00000 0.07625 AFIX 137 H16A 2 0.276708 0.762589 0.529637 11.00000 -1.50000 H16B 2 0.345016 0.695758 0.468038 11.00000 -1.50000 H16C 2 0.401352 0.829091 0.516861 11.00000 -1.50000 AFIX 0 C17 1 0.336408 0.603579 0.580186 11.00000 0.10389 AFIX 137 H17A 2 0.374314 0.568772 0.612902 11.00000 -1.50000 H17B 2 0.311639 0.545454 0.531350 11.00000 -1.50000 H17C 2 0.266642 0.628370 0.599054 11.00000 -1.50000 AFIX 56 C21 1 0.860016 0.794865 0.633354 11.00000 0.06897 C20 1 0.921802 0.872602 0.704311 11.00000 0.04249 AFIX 43 H20 2 0.970521 0.948592 0.714138 11.00000 -1.20000 AFIX 55 C19 1 0.896141 0.813939 0.757629 11.00000 0.06651 C18 1 0.818495 0.699946 0.719625 11.00000 0.05452 C22 1 0.796169 0.688158 0.642818 11.00000 0.06562 AFIX 43 H22 2 0.748160 0.622142 0.605301 11.00000 -1.20000 AFIX 0 C23 1 0.747770 0.604927 0.747194 11.00000 0.05173 C24 1 0.646278 0.658230 0.786780 11.00000 0.05560 AFIX 137 H24A 2 0.675874 0.742696 0.811335 11.00000 -1.50000 H24B 2 0.624482 0.619998 0.822879 11.00000 -1.50000 H24C 2 0.576260 0.644671 0.750395 11.00000 -1.50000 AFIX 0 C25 1 0.825271 0.562285 0.787317 11.00000 0.09471 AFIX 137 H25A 2 0.839306 0.488694 0.755690 11.00000 -1.50000 H25B 2 0.789504 0.548264 0.828565 11.00000 -1.50000 H25C 2 0.900990 0.620192 0.805646 11.00000 -1.50000 AFIX 0 C26 1 0.689872 0.483105 0.681482 11.00000 0.08742 AFIX 137 H26A 2 0.649817 0.500275 0.640581 11.00000 -1.50000 H26B 2 0.632078 0.432773 0.699079 11.00000 -1.50000 H26C 2 0.752810 0.442809 0.665165 11.00000 -1.50000 AFIX 0 C27 1 0.964039 0.865914 0.824208 11.00000 0.08159 C28 1 0.889766 0.881263 0.891939 11.00000 0.09421 AFIX 137 H28A 2 0.838555 0.935885 0.890236 11.00000 -1.50000 H28B 2 0.945205 0.912211 0.938066 11.00000 -1.50000 H28C 2 0.840644 0.804971 0.888453 11.00000 -1.50000 AFIX 0 C29 1 1.042516 1.001533 0.859298 11.00000 0.09479 AFIX 137 H29A 2 1.124609 1.004333 0.850183 11.00000 -1.50000 H29B 2 1.041791 1.029194 0.912045 11.00000 -1.50000 H29C 2 1.007931 1.051918 0.836584 11.00000 -1.50000 AFIX 0 C30 1 1.070460 0.809282 0.853252 11.00000 0.08967 AFIX 137 H30A 2 1.043356 0.723794 0.838194 11.00000 -1.50000 H30B 2 1.089162 0.841052 0.906635 11.00000 -1.50000 H30C 2 1.141760 0.829529 0.832094 11.00000 -1.50000 AFIX 0 C31 1 0.873686 0.820379 0.555273 11.00000 0.05497 C32 1 0.818711 0.917373 0.547651 11.00000 0.08177 AFIX 137 H32A 2 0.762442 0.931460 0.582255 11.00000 -1.50000 H32B 2 0.776560 0.895746 0.497746 11.00000 -1.50000 H32C 2 0.880925 0.988794 0.557931 11.00000 -1.50000 AFIX 0 C33 1 0.834189 0.711636 0.487948 11.00000 0.05241 AFIX 137 H33A 2 0.875013 0.651040 0.493735 11.00000 -1.50000 H33B 2 0.854068 0.731794 0.444653 11.00000 -1.50000 H33C 2 0.748069 0.682097 0.482132 11.00000 -1.50000 AFIX 0 C34 1 1.016678 0.871826 0.558049 11.00000 0.10471 AFIX 137 H34A 2 1.047230 0.937688 0.603205 11.00000 -1.50000 H34B 2 1.028142 0.898636 0.515916 11.00000 -1.50000 H34C 2 1.059611 0.809720 0.556675 11.00000 -1.50000 AFIX 0 F1 5 0.780020 0.389456 0.257204 11.00000 0.06482 F2 5 0.929129 0.361019 0.360575 11.00000 0.08576 F3 5 1.107789 0.539039 0.445408 11.00000 0.10758 F4 5 1.146963 0.759098 0.421344 11.00000 0.07600 F5 5 1.004124 0.788699 0.316469 11.00000 0.06911 F6 5 0.843389 0.894902 0.248097 11.00000 0.07497 F7 5 0.730130 1.039810 0.343263 11.00000 0.07023 F8 5 0.582032 0.953613 0.433115 11.00000 0.07277 F9 5 0.526839 0.723208 0.410989 11.00000 0.09705 F10 5 0.625130 0.570445 0.311138 11.00000 0.06955 F11 5 1.052468 0.611165 0.185953 11.00000 0.05585 F12 5 1.123581 0.619932 0.063568 11.00000 0.09894 F13 5 0.988479 0.695598 -0.030660 11.00000 0.12801 F14 5 0.782411 0.762434 0.000772 11.00000 0.07269 F15 5 0.700124 0.738694 0.124964 11.00000 0.06850 F16 5 0.521341 0.596184 0.175605 11.00000 0.06975 F17 5 0.401477 0.442473 0.056555 11.00000 0.08999 F18 5 0.492119 0.267618 -0.030640 11.00000 0.09755 F19 5 0.722729 0.255410 0.009468 11.00000 0.08291 F20 5 0.857360 0.413750 0.121508 11.00000 0.07070 AFIX 66 C35 1 0.884905 0.592362 0.284004 11.00000 0.04453 C40 1 0.979519 0.686175 0.327156 11.00000 0.09884 C39 1 1.057732 0.669543 0.381812 11.00000 0.06568 C38 1 1.041332 0.559097 0.393316 11.00000 0.08164 C37 1 0.946718 0.465283 0.350164 11.00000 0.08063 C36 1 0.868504 0.481914 0.295508 11.00000 0.06218 AFIX 66 C41 1 0.737273 0.727560 0.280477 11.00000 0.05742 C42 1 0.761941 0.849234 0.289587 11.00000 0.08135 C43 1 0.707201 0.925087 0.339869 11.00000 0.05719 C44 1 0.627793 0.879267 0.381040 11.00000 0.07761 C45 1 0.603124 0.757593 0.371930 11.00000 0.04846 C46 1 0.657863 0.681738 0.321649 11.00000 0.06860 AFIX 66 C47 1 0.874986 0.671042 0.156849 11.00000 0.04966 C48 1 0.984349 0.643929 0.138550 11.00000 0.06615 C49 1 1.022177 0.655229 0.073101 11.00000 0.05802 C50 1 0.950642 0.693641 0.025950 11.00000 0.07136 C51 1 0.841279 0.720753 0.044247 11.00000 0.05279 C52 1 0.803449 0.709455 0.109696 11.00000 0.06979 AFIX 66 C53 1 0.696966 0.510450 0.151829 11.00000 0.05922 C58 1 0.744986 0.421208 0.106986 11.00000 0.08917 C57 1 0.673146 0.336582 0.043585 11.00000 0.06713 C56 1 0.553286 0.341198 0.025026 11.00000 0.06594 C55 1 0.505264 0.430439 0.069868 11.00000 0.05743 C54 1 0.577102 0.515066 0.133269 11.00000 0.04506 AFIX 0 B1 3 0.796736 0.637041 0.232648 11.00000 0.06576 HKLF 4 REM dy60_hp6a_38deg_a.res in P-1 REM wR2 = 0.3679, GooF = S = 1.242, Restrained GooF = 1.250 for all data REM R1 = 0.1400 for 1117 Fo > 4sig(Fo) and 0.2120 for all 1902 data REM 276 parameters refined using 36 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.822, deepest hole -1.273, 1-sigma level 0.140 Q1 1 0.7747 0.8241 0.7364 11.00000 0.05 0.82 Q2 1 0.7628 0.7969 0.7076 11.00000 0.05 0.72 Q3 1 0.6182 0.9282 0.7783 11.00000 0.05 0.70 Q4 1 0.6379 0.9652 0.8117 11.00000 0.05 0.65 Q5 1 0.6076 0.8780 0.7227 11.00000 0.05 0.62 Q6 1 0.5414 0.7423 0.7199 11.00000 0.05 0.59 Q7 1 0.8370 0.4456 0.7385 11.00000 0.05 0.57 Q8 1 0.6012 0.8606 0.6885 11.00000 0.05 0.55 Q9 1 0.7476 0.7427 0.6356 11.00000 0.05 0.54 Q10 1 0.8413 0.9478 0.7149 11.00000 0.05 0.53 Q11 1 0.6568 0.9907 0.8344 11.00000 0.05 0.52 Q12 1 0.5527 0.7748 0.7630 11.00000 0.05 0.50 Q13 1 0.5841 0.8584 0.6000 11.00000 0.05 0.48 Q14 1 0.8241 0.7384 0.7395 11.00000 0.05 0.47 Q15 1 0.9553 0.8387 0.3221 11.00000 0.05 0.45 Q16 1 0.9423 0.8239 0.3033 11.00000 0.05 0.44 Q17 1 0.6729 0.8029 0.6633 11.00000 0.05 0.43 Q18 1 0.6026 0.9231 0.8564 11.00000 0.05 0.42 Q19 1 1.0230 0.5587 0.0973 11.00000 0.05 0.42 Q20 1 0.6106 0.9392 0.8746 11.00000 0.05 0.41 ; _shelx_res_checksum 81836 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 3.412 _oxdiff_exptl_absorpt_empirical_full_min 0.626 # start Validation Reply Form _vrf_THETM01_dy60_hp5 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_RINTA01_dy60_hp5 ; PROBLEM: The value of Rint is greater than 0.18 RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT029_dy60_hp5 ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.378 Why? RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_PLAT201_dy60_hp5 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 45 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT020_dy60_hp5 ; PROBLEM: The Value of Rint is Greater Than 0.12 ......... 0.223 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT084_dy60_hp5 ; PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.37 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT088_dy60_hp5 ; PROBLEM: Poor Data / Parameter Ratio .................... 6.89 Note RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT241_dy60_hp5 ; PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of Dy1 Check RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT342_dy60_hp5 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.06931 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT412_dy60_hp5 ; PROBLEM: Short Intra XH3 .. XHn H25A ..H26C . 1.78 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT413_dy60_hp5 ; PROBLEM: Short Inter XH3 .. XHn H15B ..H15B . 1.90 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT911_dy60_hp5 ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.500 1836 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; # end Validation Reply Form _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_dy60_hp6 _database_code_depnum_ccdc_archive 'CCDC 2046712' loop_ _audit_author_name _audit_author_address 'Andreas M. Thiel' ;Aarhus University, Department of Chemistry Denmark ; _audit_update_record ; 2022-10-30 deposited with the CCDC. 2023-02-13 downloaded from the CCDC. ; _audit_creation_date 2020-02-25 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C34 H58 Dy, B C24 F20' _chemical_formula_sum 'C58 H58 B Dy F20' _chemical_formula_weight 1308.35 _chemical_melting_point ? _chemical_oxdiff_formula C58H58BDyF20 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.290(2) _cell_length_b 11.883(3) _cell_length_c 18.809(10) _cell_angle_alpha 107.49(4) _cell_angle_beta 95.15(3) _cell_angle_gamma 100.624(17) _cell_volume 2336.9(15) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1247 _cell_measurement_temperature 293 _cell_measurement_theta_max 19.2520 _cell_measurement_theta_min 2.0210 _shelx_estimated_absorpt_T_max 0.919 _shelx_estimated_absorpt_T_min 0.693 _exptl_absorpt_coefficient_mu 1.724 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.32869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.859 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1314 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_ambient_pressure 3080000 _diffrn_reflns_av_R_equivalents 0.2094 _diffrn_reflns_av_unetI/netI 0.1542 _diffrn_reflns_Laue_measured_fraction_full 0.379 _diffrn_reflns_Laue_measured_fraction_max 0.379 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 15603 _diffrn_reflns_point_group_measured_fraction_full 0.379 _diffrn_reflns_point_group_measured_fraction_max 0.379 _diffrn_reflns_theta_full 20.803 _diffrn_reflns_theta_max 20.803 _diffrn_reflns_theta_min 1.829 _diffrn_ambient_environment air _diffrn_ambient_temperature 293 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3590 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.379 _diffrn_measured_fraction_theta_max 0.379 _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 -43.00 35.00 1.00 30.00 -- 12.55 13.00 176.00 78 2 \w -89.00 -68.00 1.00 30.00 -- 12.55-178.00 -90.00 21 3 \w 20.00 85.00 1.00 30.00 -- 12.55-135.00 57.00 65 4 \w -32.00 27.00 1.00 30.00 -- 12.55 39.00 -12.00 59 5 \w -21.00 54.00 1.00 30.00 -- 12.55 -53.00 17.00 75 6 \w -111.00 -68.00 1.00 30.00 -- -13.41 178.00 90.00 43 7 \w 1.00 37.00 1.00 30.00 -- -13.41 -99.00-150.00 36 8 \w -26.00 32.00 1.00 30.00 -- -13.41 -39.00 12.00 58 9 \w 1.00 37.00 1.00 30.00 -- -13.41 -99.00 30.00 36 10 \w -56.00 11.00 1.00 30.00 -- -13.41 81.00 -29.00 67 11 \w -26.00 32.00 1.00 30.00 -- -13.41 -39.00-167.00 58 12 \w -32.00 -3.00 1.00 30.00 -- 12.55 39.00 167.00 29 13 \w -31.00 -9.00 1.00 30.00 -- 12.55 77.00 150.00 22 14 \w -36.00 -16.00 1.00 30.00 -- -13.41 38.00 -30.00 20 15 \w 9.00 30.00 1.00 30.00 -- -13.41 -77.00 30.00 21 16 \w -54.00 22.00 1.00 30.00 -- -13.41 53.00 162.00 76 17 \w -54.00 4.00 1.00 30.00 -- -13.41 57.00-180.00 58 18 \w -37.00 -9.00 1.00 30.00 -- -13.41 77.00 150.00 28 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0148857000 _diffrn_orient_matrix_UB_12 -0.0163456000 _diffrn_orient_matrix_UB_13 -0.0397506000 _diffrn_orient_matrix_UB_21 -0.0321383000 _diffrn_orient_matrix_UB_22 -0.0580851000 _diffrn_orient_matrix_UB_23 -0.0014811000 _diffrn_orient_matrix_UB_31 -0.0541497000 _diffrn_orient_matrix_UB_32 0.0219018000 _diffrn_orient_matrix_UB_33 0.0044002000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1072 _reflns_number_total 1850 _reflns_odcompleteness_completeness 38.58 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 20.77 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.642 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.131 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.226 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 277 _refine_ls_number_reflns 1850 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.2142 _refine_ls_R_factor_gt 0.1414 _refine_ls_restrained_S_all 1.233 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3201 _refine_ls_wR_factor_ref 0.3688 _refine_special_details ? _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. Restrained planarity C54, C55, C56, C57, C58, F16, F17, F18, F19, F20, B1, C53 with sigma of 0.1 C47, C52, C51, C50, C49, C48, F15, F14, F13, F12, F11, B1 with sigma of 0.1 C35, C36, C37, C38, C39, C40, F1, F2, F3, F4, F5, B1 with sigma of 0.1 C41, C46, C45, C44, C43, C42, F10, F9, F8, F7, F6, B1 with sigma of 0.1 3.a Me refined with riding coordinates: C34(H34A,H34B,H34C) 3.b Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C20(H20), C22(H22) 3.c Fitted pentagon refined as free rotating group: C1(C2,C3,C4,C5), C21(C20,C19,C18,C22) 3.d Fitted hexagon refined as free rotating group: C35(C40,C39,C38,C37,C36), C41(C42,C43,C44,C45,C46), C47(C48,C49,C50,C51,C52), C53(C58,C57,C56,C55,C54) 3.e Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B, H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A, H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.6926(2) 0.8457(2) 0.7239(3) 0.141(5) Uani 1 1 d . . . . . C1 C 0.567(2) 0.992(2) 0.726(3) 0.057(12) Uiso 1 1 d . . . . . C2 C 0.506(3) 0.924(3) 0.767(3) 0.065(13) Uiso 1 1 d G . . . . C3 C 0.446(3) 0.809(3) 0.716(4) 0.109(19) Uiso 1 1 d G . . . . H3 H 0.399154 0.746007 0.727848 0.130 Uiso 1 1 calc R . . . . C4 C 0.471(3) 0.805(3) 0.643(3) 0.064(13) Uiso 1 1 d G . . . . C5 C 0.546(3) 0.919(3) 0.649(3) 0.096(17) Uiso 1 1 d G . . . . H5 H 0.576139 0.941291 0.609407 0.115 Uiso 1 1 calc R . . . . C6 C 0.657(3) 1.126(3) 0.764(5) 0.051(11) Uiso 1 1 d . . . . . C7 C 0.765(4) 1.103(5) 0.787(6) 0.092(16) Uiso 1 1 d . . . . . H7A H 0.767179 1.099938 0.837267 0.137 Uiso 1 1 calc GR . . . . H7B H 0.830749 1.165876 0.785420 0.137 Uiso 1 1 calc GR . . . . H7C H 0.773617 1.026514 0.753684 0.137 Uiso 1 1 calc GR . . . . C8 C 0.600(4) 1.218(4) 0.805(6) 0.073(13) Uiso 1 1 d . . . . . H8A H 0.524758 1.215255 0.776019 0.109 Uiso 1 1 calc GR . . . . H8B H 0.653592 1.296249 0.815826 0.109 Uiso 1 1 calc GR . . . . H8C H 0.584249 1.205658 0.851947 0.109 Uiso 1 1 calc GR . . . . C9 C 0.690(5) 1.171(5) 0.696(7) 0.113(19) Uiso 1 1 d . . . . . H9A H 0.732240 1.116926 0.664873 0.169 Uiso 1 1 calc GR . . . . H9B H 0.741259 1.250769 0.715406 0.169 Uiso 1 1 calc GR . . . . H9C H 0.616490 1.172519 0.666896 0.169 Uiso 1 1 calc GR . . . . C10 C 0.478(5) 0.953(4) 0.847(7) 0.083(15) Uiso 1 1 d . . . . . C11 C 0.586(4) 0.998(5) 0.898(7) 0.093(16) Uiso 1 1 d . . . . . H11A H 0.612916 0.932377 0.909419 0.140 Uiso 1 1 calc GR . . . . H11B H 0.573374 1.055008 0.942847 0.140 Uiso 1 1 calc GR . . . . H11C H 0.647416 1.036936 0.875183 0.140 Uiso 1 1 calc GR . . . . C12 C 0.421(4) 0.839(4) 0.861(6) 0.084(15) Uiso 1 1 d . . . . . H12A H 0.334186 0.829166 0.855312 0.126 Uiso 1 1 calc GR . . . . H12B H 0.451517 0.842584 0.911235 0.126 Uiso 1 1 calc GR . . . . H12C H 0.441191 0.770701 0.825258 0.126 Uiso 1 1 calc GR . . . . C13 C 0.387(5) 1.033(5) 0.862(9) 0.114(19) Uiso 1 1 d . . . . . H13A H 0.426147 1.113974 0.865440 0.171 Uiso 1 1 calc GR . . . . H13B H 0.357764 1.033662 0.908265 0.171 Uiso 1 1 calc GR . . . . H13C H 0.319916 1.002562 0.821124 0.171 Uiso 1 1 calc GR . . . . C14 C 0.422(4) 0.701(4) 0.569(7) 0.079(14) Uiso 1 1 d . . . . . C15 C 0.514(4) 0.640(5) 0.521(6) 0.082(14) Uiso 1 1 d . . . . . H15A H 0.550497 0.692098 0.494329 0.124 Uiso 1 1 calc GR . . . . H15B H 0.472089 0.563825 0.485441 0.124 Uiso 1 1 calc GR . . . . H15C H 0.577324 0.628442 0.554006 0.124 Uiso 1 1 calc GR . . . . C16 C 0.361(4) 0.745(5) 0.513(6) 0.092(16) Uiso 1 1 d . . . . . H16A H 0.386675 0.831600 0.527158 0.138 Uiso 1 1 calc GR . . . . H16B H 0.273766 0.723504 0.510784 0.138 Uiso 1 1 calc GR . . . . H16C H 0.381249 0.708840 0.463917 0.138 Uiso 1 1 calc GR . . . . C17 C 0.336(5) 0.591(4) 0.576(6) 0.079(14) Uiso 1 1 d . . . . . H17A H 0.379964 0.555092 0.606642 0.119 Uiso 1 1 calc GR . . . . H17B H 0.306408 0.532304 0.526985 0.119 Uiso 1 1 calc GR . . . . H17C H 0.268832 0.615078 0.599462 0.119 Uiso 1 1 calc GR . . . . C21 C 0.864(4) 0.794(4) 0.631(4) 0.090(17) Uiso 1 1 d . . . . . C20 C 0.924(2) 0.875(2) 0.702(4) 0.064(13) Uiso 1 1 d G . . . . H20 H 0.972334 0.951690 0.711798 0.077 Uiso 1 1 calc R . . . . C19 C 0.898(4) 0.817(4) 0.757(4) 0.087(17) Uiso 1 1 d G . . . . C18 C 0.821(3) 0.701(3) 0.719(4) 0.056(13) Uiso 1 1 d G . . . . C22 C 0.801(3) 0.687(3) 0.641(4) 0.11(2) Uiso 1 1 d G . . . . H22 H 0.753728 0.619022 0.603069 0.131 Uiso 1 1 calc R . . . . C23 C 0.753(4) 0.609(4) 0.743(6) 0.063(12) Uiso 1 1 d . . . . . C24 C 0.658(4) 0.663(4) 0.787(6) 0.085(14) Uiso 1 1 d . . . . . H24A H 0.687710 0.748969 0.808743 0.128 Uiso 1 1 calc GR . . . . H24B H 0.643994 0.628031 0.825863 0.128 Uiso 1 1 calc GR . . . . H24C H 0.583409 0.646136 0.752960 0.128 Uiso 1 1 calc GR . . . . C25 C 0.824(4) 0.566(4) 0.797(6) 0.075(14) Uiso 1 1 d . . . . . H25A H 0.907176 0.610431 0.809017 0.112 Uiso 1 1 calc GR . . . . H25B H 0.821647 0.481014 0.774781 0.112 Uiso 1 1 calc GR . . . . H25C H 0.788481 0.577772 0.842745 0.112 Uiso 1 1 calc GR . . . . C26 C 0.703(4) 0.493(4) 0.693(6) 0.071(13) Uiso 1 1 d . . . . . H26A H 0.642765 0.497975 0.654648 0.107 Uiso 1 1 calc GR . . . . H26B H 0.664686 0.442585 0.719248 0.107 Uiso 1 1 calc GR . . . . H26C H 0.765767 0.459152 0.668984 0.107 Uiso 1 1 calc GR . . . . C27 C 0.968(4) 0.863(5) 0.827(7) 0.076(15) Uiso 1 1 d . . . . . C28 C 0.887(4) 0.879(4) 0.884(6) 0.083(14) Uiso 1 1 d . . . . . H28A H 0.845232 0.941639 0.881947 0.124 Uiso 1 1 calc GR . . . . H28B H 0.934833 0.901827 0.933349 0.124 Uiso 1 1 calc GR . . . . H28C H 0.828482 0.804795 0.875428 0.124 Uiso 1 1 calc GR . . . . C29 C 1.048(4) 1.008(4) 0.875(6) 0.090(15) Uiso 1 1 d . . . . . H29A H 1.113176 1.006178 0.910224 0.135 Uiso 1 1 calc GR . . . . H29B H 0.994175 1.053975 0.900849 0.135 Uiso 1 1 calc GR . . . . H29C H 1.080435 1.044752 0.839488 0.135 Uiso 1 1 calc GR . . . . C30 C 1.076(4) 0.809(4) 0.854(6) 0.100(16) Uiso 1 1 d . . . . . H30A H 1.049143 0.723193 0.841752 0.151 Uiso 1 1 calc GR . . . . H30B H 1.099725 0.845622 0.907507 0.151 Uiso 1 1 calc GR . . . . H30C H 1.144280 0.826626 0.829032 0.151 Uiso 1 1 calc GR . . . . C31 C 0.880(3) 0.826(4) 0.563(6) 0.051(11) Uiso 1 1 d . . . . . C32 C 0.821(4) 0.928(4) 0.553(5) 0.064(12) Uiso 1 1 d . . . . . H32A H 0.739699 0.893476 0.525991 0.096 Uiso 1 1 calc GR . . . . H32B H 0.868211 0.970114 0.525310 0.096 Uiso 1 1 calc GR . . . . H32C H 0.817875 0.983095 0.601712 0.096 Uiso 1 1 calc GR . . . . C33 C 0.845(4) 0.718(4) 0.498(5) 0.063(12) Uiso 1 1 d . . . . . H33A H 0.902942 0.668155 0.498904 0.095 Uiso 1 1 calc GR . . . . H33B H 0.844541 0.740163 0.453115 0.095 Uiso 1 1 calc GR . . . . H33C H 0.765542 0.674491 0.499493 0.095 Uiso 1 1 calc GR . . . . C34 C 1.014(4) 0.867(5) 0.561(6) 0.104(17) Uiso 1 1 d . . . . . H34A H 1.023149 0.888536 0.515917 0.156 Uiso 1 1 calc R . . . . H34B H 1.049277 0.936740 0.604329 0.156 Uiso 1 1 calc R . . . . H34C H 1.054554 0.803147 0.560703 0.156 Uiso 1 1 calc R . . . . F1 F 0.7728(19) 0.3846(19) 0.255(3) 0.067(6) Uiso 1 1 d . . . . . F2 F 0.939(2) 0.362(2) 0.371(3) 0.097(8) Uiso 1 1 d . . . . . F3 F 1.109(2) 0.543(2) 0.458(3) 0.098(8) Uiso 1 1 d . . . . . F4 F 1.155(2) 0.762(2) 0.428(3) 0.096(8) Uiso 1 1 d . . . . . F5 F 1.0081(19) 0.7927(19) 0.320(3) 0.069(6) Uiso 1 1 d . . . . . F6 F 0.8399(19) 0.902(2) 0.256(3) 0.076(7) Uiso 1 1 d . . . . . F7 F 0.7318(19) 1.046(2) 0.351(3) 0.075(7) Uiso 1 1 d . . . . . F8 F 0.579(2) 0.958(2) 0.437(3) 0.093(8) Uiso 1 1 d . . . . . F9 F 0.528(2) 0.725(2) 0.412(3) 0.088(8) Uiso 1 1 d . . . . . F10 F 0.621(2) 0.576(2) 0.319(3) 0.091(8) Uiso 1 1 d . . . . . F11 F 1.051(2) 0.615(2) 0.188(3) 0.092(8) Uiso 1 1 d . . . . . F12 F 1.121(2) 0.616(2) 0.065(3) 0.108(9) Uiso 1 1 d . . . . . F13 F 0.992(3) 0.694(3) -0.029(4) 0.132(11) Uiso 1 1 d . . . . . F14 F 0.778(2) 0.757(2) -0.007(3) 0.098(9) Uiso 1 1 d . . . . . F15 F 0.700(2) 0.742(2) 0.126(3) 0.082(7) Uiso 1 1 d . . . . . F16 F 0.515(2) 0.598(2) 0.172(3) 0.098(8) Uiso 1 1 d . . . . . F17 F 0.395(2) 0.443(3) 0.056(3) 0.108(9) Uiso 1 1 d . . . . . F18 F 0.493(3) 0.274(3) -0.028(4) 0.137(12) Uiso 1 1 d . . . . . F19 F 0.723(2) 0.255(2) 0.007(3) 0.105(9) Uiso 1 1 d . . . . . F20 F 0.856(2) 0.416(2) 0.121(3) 0.073(7) Uiso 1 1 d . . . . . C35 C 0.890(3) 0.596(3) 0.289(2) 0.059(11) Uiso 1 1 d . . . . . C40 C 0.984(3) 0.691(2) 0.333(3) 0.15(3) Uiso 1 1 d G . . . . C39 C 1.061(2) 0.675(3) 0.389(2) 0.080(14) Uiso 1 1 d G . . . . C38 C 1.044(3) 0.564(3) 0.401(2) 0.094(17) Uiso 1 1 d G . . . . C37 C 0.949(3) 0.469(2) 0.357(3) 0.090(16) Uiso 1 1 d G . . . . C36 C 0.872(2) 0.485(2) 0.301(2) 0.103(18) Uiso 1 1 d G . . . . C41 C 0.740(2) 0.731(2) 0.284(2) 0.060(12) Uiso 1 1 d . . . . . C42 C 0.767(2) 0.854(2) 0.293(2) 0.066(12) Uiso 1 1 d G . . . . C43 C 0.711(2) 0.9322(17) 0.343(2) 0.050(11) Uiso 1 1 d G . . . . C44 C 0.629(2) 0.887(2) 0.384(2) 0.095(16) Uiso 1 1 d G . . . . C45 C 0.603(2) 0.765(3) 0.376(2) 0.097(17) Uiso 1 1 d G . . . . C46 C 0.658(2) 0.6865(18) 0.326(2) 0.080(14) Uiso 1 1 d G . . . . C47 C 0.876(3) 0.673(2) 0.155(2) 0.061(12) Uiso 1 1 d . . . . . C48 C 0.986(2) 0.6445(19) 0.137(3) 0.076(14) Uiso 1 1 d G . . . . C49 C 1.024(2) 0.6541(19) 0.070(3) 0.059(12) Uiso 1 1 d G . . . . C50 C 0.953(3) 0.692(2) 0.022(2) 0.11(2) Uiso 1 1 d G . . . . C51 C 0.843(3) 0.7202(19) 0.040(3) 0.084(15) Uiso 1 1 d G . . . . C52 C 0.8041(18) 0.7106(19) 0.106(3) 0.067(13) Uiso 1 1 d G . . . . C53 C 0.694(3) 0.518(3) 0.154(3) 0.069(13) Uiso 1 1 d . . . . . C58 C 0.747(2) 0.429(3) 0.110(3) 0.092(16) Uiso 1 1 d G . . . . C57 C 0.678(3) 0.342(3) 0.045(3) 0.080(14) Uiso 1 1 d G . . . . C56 C 0.557(3) 0.343(3) 0.024(3) 0.12(2) Uiso 1 1 d G . . . . C55 C 0.505(2) 0.432(3) 0.068(3) 0.12(2) Uiso 1 1 d G . . . . C54 C 0.573(3) 0.519(3) 0.133(3) 0.085(15) Uiso 1 1 d G . . . . B1 B 0.804(4) 0.636(4) 0.237(4) 0.11(2) Uiso 1 1 d . . . . . 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 0.0619(17) 0.107(2) 0.282(16) 0.095(5) 0.044(4) 0.0254(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 2.43(2) . ? Dy1 C2 2.56(3) . ? Dy1 C3 2.72(3) . ? Dy1 C4 2.69(4) . ? Dy1 C5 2.52(4) . ? Dy1 C21 2.76(5) . ? Dy1 C20 2.66(3) . ? Dy1 C19 2.45(4) . ? Dy1 C18 2.43(3) . ? Dy1 C22 2.63(4) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 C6 1.62(5) . ? C2 C3 1.4200 . ? C2 C10 1.51(13) . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C4 C14 1.53(11) . ? C6 C7 1.36(7) . ? C6 C8 1.44(7) . ? C6 C9 1.57(12) . ? C10 C11 1.39(12) . ? C10 C12 1.50(6) . ? C10 C13 1.52(6) . ? C14 C15 1.57(8) . ? C14 C16 1.48(12) . ? C14 C17 1.53(5) . ? C21 C20 1.4200 . ? C21 C22 1.4200 . ? C21 C31 1.44(8) . ? C20 C19 1.4200 . ? C19 C18 1.4200 . ? C19 C27 1.36(12) . ? C18 C22 1.4200 . ? C18 C23 1.43(5) . ? C23 C24 1.53(7) . ? C23 C25 1.50(10) . ? C23 C26 1.39(9) . ? C27 C28 1.47(11) . ? C27 C29 1.72(9) . ? C27 C30 1.59(7) . ? C31 C32 1.53(5) . ? C31 C33 1.44(10) . ? C31 C34 1.51(5) . ? F1 C36 1.46(4) . ? F2 C37 1.36(3) . ? F3 C38 1.36(6) . ? F4 C39 1.32(4) . ? F5 C40 1.28(3) . ? F6 C42 1.29(3) . ? F7 C43 1.29(2) . ? F8 C44 1.33(4) . ? F9 C45 1.25(4) . ? F10 C46 1.26(2) . ? F11 C48 1.33(5) . ? F12 C49 1.26(3) . ? F13 C50 1.09(7) . ? F14 C51 1.32(5) . ? F15 C52 1.34(3) . ? F16 C54 1.32(4) . ? F17 C55 1.28(3) . ? F18 C56 1.15(7) . ? F19 C57 1.29(4) . ? F20 C58 1.28(3) . ? C35 C40 1.3900 . ? C35 C36 1.3900 . ? C35 B1 1.54(7) . ? C40 C39 1.3900 . ? C39 C38 1.3900 . ? C38 C37 1.3900 . ? C37 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 B1 1.55(6) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C47 B1 1.93(7) . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C53 C58 1.3900 . ? C53 C54 1.3900 . ? C53 B1 1.91(7) . ? C58 C57 1.3900 . ? C57 C56 1.3900 . ? C56 C55 1.3900 . ? C55 C54 1.3900 . ? 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 C1 Dy1 C2 32.9(3) . . ? C1 Dy1 C3 52.6(4) . . ? C1 Dy1 C4 53.0(5) . . ? C1 Dy1 C5 33.3(4) . . ? C1 Dy1 C21 126.1(14) . . ? C1 Dy1 C20 125.0(9) . . ? C1 Dy1 C19 145.6(12) . . ? C1 Dy1 C18 178.2(15) . . ? C1 Dy1 C22 146.3(19) . . ? C2 Dy1 C3 31.0(3) . . ? C2 Dy1 C4 51.8(4) . . ? C2 Dy1 C21 156.7(15) . . ? C2 Dy1 C20 153.3(11) . . ? C2 Dy1 C22 153.7(13) . . ? C3 Dy1 C21 139.2(18) . . ? C4 Dy1 C3 30.4(3) . . ? C4 Dy1 C21 110.8(16) . . ? C5 Dy1 C2 53.8(4) . . ? C5 Dy1 C3 51.9(5) . . ? C5 Dy1 C4 31.4(5) . . ? C5 Dy1 C21 103.1(14) . . ? C5 Dy1 C20 119.0(15) . . ? C5 Dy1 C22 114.1(18) . . ? C20 Dy1 C3 168(2) . . ? C20 Dy1 C4 138.1(19) . . ? C20 Dy1 C21 30.3(4) . . ? C19 Dy1 C2 148.6(18) . . ? C19 Dy1 C3 156.5(14) . . ? C19 Dy1 C4 158.3(15) . . ? C19 Dy1 C5 150.9(15) . . ? C19 Dy1 C21 51.9(4) . . ? C19 Dy1 C20 32.0(3) . . ? C19 Dy1 C22 53.6(4) . . ? C18 Dy1 C2 148.9(13) . . ? C18 Dy1 C3 128.6(8) . . ? C18 Dy1 C4 127.1(15) . . ? C18 Dy1 C5 146(2) . . ? C18 Dy1 C21 52.1(5) . . ? C18 Dy1 C20 53.4(4) . . ? C18 Dy1 C19 33.8(4) . . ? C18 Dy1 C22 32.3(4) . . ? C22 Dy1 C3 122.7(13) . . ? C22 Dy1 C4 104.7(14) . . ? C22 Dy1 C21 30.4(5) . . ? C22 Dy1 C20 51.5(5) . . ? C2 C1 Dy1 78.6(13) . . ? C2 C1 C5 108.0 . . ? C2 C1 C6 124(4) . . ? C5 C1 Dy1 76.6(16) . . ? C5 C1 C6 127(4) . . ? C6 C1 Dy1 106.8(19) . . ? C1 C2 Dy1 68.5(11) . . ? C1 C2 C10 135(3) . . ? C3 C2 Dy1 80.5(13) . . ? C3 C2 C1 108.0 . . ? C3 C2 C10 117(4) . . ? C10 C2 Dy1 124(4) . . ? C2 C3 Dy1 68.4(12) . . ? C4 C3 Dy1 73.7(14) . . ? C4 C3 C2 108.0 . . ? C3 C4 Dy1 75.8(13) . . ? C3 C4 C5 108.0 . . ? C3 C4 C14 127(4) . . ? C5 C4 Dy1 67.5(10) . . ? C5 C4 C14 125(4) . . ? C14 C4 Dy1 124(3) . . ? C1 C5 Dy1 70.1(14) . . ? C4 C5 Dy1 81.1(11) . . ? C4 C5 C1 108.0 . . ? C7 C6 C1 104(3) . . ? C7 C6 C8 126(8) . . ? C7 C6 C9 101(5) . . ? C8 C6 C1 115(3) . . ? C8 C6 C9 102(4) . . ? C9 C6 C1 106(7) . . ? C2 C10 C13 112(9) . . ? C11 C10 C2 110(5) . . ? C11 C10 C12 105(7) . . ? C11 C10 C13 114(8) . . ? C12 C10 C2 110(7) . . ? C12 C10 C13 106(4) . . ? C4 C14 C15 119(5) . . ? C4 C14 C17 115(8) . . ? C16 C14 C4 110(4) . . ? C16 C14 C15 100(8) . . ? C16 C14 C17 109(6) . . ? C17 C14 C15 101(4) . . ? C20 C21 Dy1 70.9(15) . . ? C20 C21 C22 108.0 . . ? C20 C21 C31 120(4) . . ? C22 C21 Dy1 69.7(8) . . ? C22 C21 C31 132(4) . . ? C31 C21 Dy1 128(2) . . ? C21 C20 Dy1 78.8(18) . . ? C21 C20 C19 108.00(6) . . ? C19 C20 Dy1 66.1(16) . . ? C20 C19 Dy1 81.9(16) . . ? C18 C19 Dy1 72.4(11) . . ? C18 C19 C20 108.0 . . ? C27 C19 Dy1 127(4) . . ? C27 C19 C20 119(5) . . ? C27 C19 C18 131(4) . . ? C19 C18 Dy1 73.8(13) . . ? C19 C18 C23 134(6) . . ? C22 C18 Dy1 81(2) . . ? C22 C18 C19 108.0 . . ? C22 C18 C23 117(6) . . ? C23 C18 Dy1 105(2) . . ? C21 C22 Dy1 79.8(10) . . ? C18 C22 Dy1 66.3(18) . . ? C18 C22 C21 108.0 . . ? C18 C23 C24 107(3) . . ? C18 C23 C25 116(4) . . ? C25 C23 C24 105(7) . . ? C26 C23 C18 121(8) . . ? C26 C23 C24 112(4) . . ? C26 C23 C25 95(4) . . ? C19 C27 C28 109(5) . . ? C19 C27 C29 129(6) . . ? C19 C27 C30 125(7) . . ? C28 C27 C29 87(6) . . ? C28 C27 C30 108(8) . . ? C30 C27 C29 91(5) . . ? C21 C31 C32 117(5) . . ? C21 C31 C33 109(4) . . ? C21 C31 C34 110(6) . . ? C33 C31 C32 112(7) . . ? C33 C31 C34 102(5) . . ? C34 C31 C32 106(3) . . ? C40 C35 C36 120.0 . . ? C40 C35 B1 112(3) . . ? C36 C35 B1 127(3) . . ? F5 C40 C35 122(3) . . ? F5 C40 C39 118(3) . . ? C35 C40 C39 120.0 . . ? F4 C39 C40 121(3) . . ? F4 C39 C38 119(3) . . ? C38 C39 C40 120.0 . . ? F3 C38 C39 124(3) . . ? F3 C38 C37 116(3) . . ? C39 C38 C37 120.0 . . ? F2 C37 C38 117(3) . . ? F2 C37 C36 123(3) . . ? C38 C37 C36 120.0 . . ? C35 C36 F1 121(3) . . ? C37 C36 F1 119(3) . . ? C37 C36 C35 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 B1 126(2) . . ? C46 C41 B1 114(2) . . ? F6 C42 C41 123(2) . . ? F6 C42 C43 117(2) . . ? C43 C42 C41 120.0 . . ? F7 C43 C42 121(2) . . ? F7 C43 C44 119(2) . . ? C42 C43 C44 120.0 . . ? F8 C44 C43 123(2) . . ? F8 C44 C45 117(2) . . ? C45 C44 C43 120.0 . . ? F9 C45 C44 119(2) . . ? F9 C45 C46 121(2) . . ? C44 C45 C46 120.0 . . ? F10 C46 C41 126(3) . . ? F10 C46 C45 114(3) . . ? C45 C46 C41 120.0 . . ? C48 C47 C52 120.0 . . ? C48 C47 B1 122(3) . . ? C52 C47 B1 117(3) . . ? F11 C48 C47 116(3) . . ? F11 C48 C49 124(3) . . ? C49 C48 C47 120.0 . . ? F12 C49 C48 107(4) . . ? F12 C49 C50 133(4) . . ? C48 C49 C50 120.0 . . ? F13 C50 C49 113(4) . . ? F13 C50 C51 127(4) . . ? C51 C50 C49 120.0 . . ? F14 C51 C50 118(3) . . ? F14 C51 C52 122(3) . . ? C50 C51 C52 120.0 . . ? F15 C52 C47 119(4) . . ? F15 C52 C51 121(4) . . ? C51 C52 C47 120.0 . . ? C58 C53 C54 120.0 . . ? C58 C53 B1 115(3) . . ? C54 C53 B1 125(3) . . ? F20 C58 C53 128(3) . . ? F20 C58 C57 112(3) . . ? C57 C58 C53 120.0 . . ? F19 C57 C58 120(4) . . ? F19 C57 C56 120(4) . . ? C58 C57 C56 120.0 . . ? F18 C56 C57 125(4) . . ? F18 C56 C55 115(4) . . ? C57 C56 C55 120.0 . . ? F17 C55 C56 126(4) . . ? F17 C55 C54 114(4) . . ? C54 C55 C56 120.0 . . ? F16 C54 C53 124(3) . . ? F16 C54 C55 116(3) . . ? C55 C54 C53 120.0 . . ? C35 B1 C41 111(3) . . ? C35 B1 C47 114(3) . . ? C35 B1 C53 120(3) . . ? C41 B1 C47 117(3) . . ? C41 B1 C53 112(3) . . ? C53 B1 C47 80(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C15 H15A F9 0.96 1.71 2.54(9) 142.0 . yes C16 H16C F9 0.96 2.00 2.78(8) 137.0 . yes C25 H25B F11 0.96 2.18 2.84(5) 124.7 2_766 yes _shelx_res_file ; TITL dy60_hp7a_38deg_a.res in P1 dy60_hp7a_38deg.res created by SHELXL-2018/3 at 17:24:48 on 19-Feb-2020 REM Old TITL Dy60_HP7A_38deg in P-1 REM SHELXT solution in P1: R1 0.284, Rweak 0.178, Alpha 0.000 REM 0.000 for 0 systematic absences, Orientation as input REM Flack x = 0.496 ( 0.025 ) from 622 Parsons' quotients REM Formula found by SHELXT: C84 B9 F60 Dy3 CELL 0.71073 11.2896 11.8828 18.8092 107.489 95.151 100.624 ZERR 2 0.002 0.0028 0.0103 0.035 0.03 0.017 LATT 1 SFAC C H B Dy F UNIT 116 116 2 2 40 EQIV $1 2-X,1-Y,1-Z FLAT C54 C55 C56 C57 C58 F16 F17 F18 F19 F20 B1 C53 FLAT C47 C52 C51 C50 C49 C48 F15 F14 F13 F12 F11 B1 FLAT C35 C36 C37 C38 C39 C40 F1 F2 F3 F4 F5 B1 FLAT C41 C46 C45 C44 C43 C42 F10 F9 F8 F7 F6 B1 L.S. 20 0 0 PLAN 20 SIZE 0.16 0.23 0.05 HTAB C15 F9 HTAB C16 F9 HTAB C25 F11_$1 FREE Dy1 C24 FREE Dy1 C7 list 4 fmap 2 53 acta SHEL 100 0.83 OMIT 0 180 OMIT -6 2 1 OMIT -4 1 3 OMIT -6 4 0 OMIT 5 -8 1 OMIT -6 0 2 OMIT 10 0 1 OMIT -8 3 1 OMIT -5 2 0 OMIT -4 3 0 OMIT -6 0 4 OMIT -9 3 2 OMIT -2 -5 2 OMIT -11 2 3 OMIT -7 -5 5 OMIT -8 1 2 OMIT -9 1 3 OMIT -11 3 2 OMIT -6 -1 3 OMIT -8 6 1 OMIT 8 -6 1 OMIT -11 3 3 OMIT -8 4 0 OMIT -7 6 0 OMIT 0 -8 5 OMIT 5 1 0 OMIT -7 1 1 OMIT 4 -2 1 OMIT -10 3 1 OMIT -7 5 0 OMIT 4 -5 2 OMIT 7 6 0 OMIT 2 -7 3 OMIT -4 -1 4 REM REM REM WGHT 0.200000 FVAR 0.38129 DY1 4 0.692631 0.845692 0.723858 11.00000 0.06194 0.10678 = 0.28180 0.09522 0.04402 0.02543 AFIX 56 C1 1 0.567463 0.992319 0.725815 11.00000 0.05704 C2 1 0.505662 0.924128 0.767173 11.00000 0.06453 C3 1 0.446231 0.808585 0.715749 11.00000 0.10872 AFIX 43 H3 2 0.399154 0.746007 0.727848 11.00000 -1.20000 AFIX 55 C4 1 0.471302 0.805366 0.642610 11.00000 0.06397 C5 1 0.546228 0.918920 0.648831 11.00000 0.09606 AFIX 43 H5 2 0.576139 0.941291 0.609407 11.00000 -1.20000 AFIX 0 C6 1 0.656914 1.125558 0.763722 11.00000 0.05085 C7 1 0.765058 1.102800 0.786712 11.00000 0.09165 AFIX 137 H7A 2 0.767179 1.099938 0.837267 11.00000 -1.50000 H7B 2 0.830749 1.165876 0.785420 11.00000 -1.50000 H7C 2 0.773617 1.026514 0.753684 11.00000 -1.50000 AFIX 0 C8 1 0.600150 1.218415 0.805346 11.00000 0.07296 AFIX 137 H8A 2 0.524758 1.215255 0.776019 11.00000 -1.50000 H8B 2 0.653592 1.296249 0.815826 11.00000 -1.50000 H8C 2 0.584249 1.205658 0.851947 11.00000 -1.50000 AFIX 0 C9 1 0.689934 1.170842 0.696160 11.00000 0.11258 AFIX 137 H9A 2 0.732240 1.116926 0.664873 11.00000 -1.50000 H9B 2 0.741259 1.250769 0.715406 11.00000 -1.50000 H9C 2 0.616490 1.172519 0.666896 11.00000 -1.50000 AFIX 0 C10 1 0.478202 0.952672 0.847190 11.00000 0.08265 C11 1 0.586268 0.997703 0.897521 11.00000 0.09348 AFIX 137 H11A 2 0.612916 0.932377 0.909419 11.00000 -1.50000 H11B 2 0.573374 1.055008 0.942847 11.00000 -1.50000 H11C 2 0.647416 1.036936 0.875183 11.00000 -1.50000 AFIX 0 C12 1 0.421159 0.838548 0.860985 11.00000 0.08388 AFIX 137 H12A 2 0.334186 0.829166 0.855312 11.00000 -1.50000 H12B 2 0.451517 0.842584 0.911235 11.00000 -1.50000 H12C 2 0.441191 0.770701 0.825258 11.00000 -1.50000 AFIX 0 C13 1 0.387151 1.033099 0.861850 11.00000 0.11389 AFIX 137 H13A 2 0.426147 1.113974 0.865440 11.00000 -1.50000 H13B 2 0.357764 1.033662 0.908265 11.00000 -1.50000 H13C 2 0.319916 1.002562 0.821124 11.00000 -1.50000 AFIX 0 C14 1 0.421968 0.701374 0.568738 11.00000 0.07871 C15 1 0.514495 0.640496 0.520969 11.00000 0.08246 AFIX 137 H15A 2 0.550497 0.692098 0.494329 11.00000 -1.50000 H15B 2 0.472089 0.563825 0.485441 11.00000 -1.50000 H15C 2 0.577324 0.628442 0.554006 11.00000 -1.50000 AFIX 0 C16 1 0.360508 0.745184 0.512721 11.00000 0.09217 AFIX 137 H16A 2 0.386675 0.831600 0.527158 11.00000 -1.50000 H16B 2 0.273766 0.723504 0.510784 11.00000 -1.50000 H16C 2 0.381249 0.708840 0.463917 11.00000 -1.50000 AFIX 0 C17 1 0.336278 0.590600 0.576150 11.00000 0.07946 AFIX 137 H17A 2 0.379964 0.555092 0.606642 11.00000 -1.50000 H17B 2 0.306408 0.532304 0.526985 11.00000 -1.50000 H17C 2 0.268832 0.615078 0.599462 11.00000 -1.50000 AFIX 56 C21 1 0.864202 0.794141 0.630534 11.00000 0.09046 C20 1 0.924172 0.874721 0.702275 11.00000 0.06403 AFIX 43 H20 2 0.972334 0.951690 0.711798 11.00000 -1.20000 AFIX 55 C19 1 0.897693 0.817146 0.756923 11.00000 0.08745 C18 1 0.821358 0.700983 0.718956 11.00000 0.05579 C22 1 0.800660 0.686765 0.640844 11.00000 0.10891 AFIX 43 H22 2 0.753728 0.619022 0.603069 11.00000 -1.20000 AFIX 0 C23 1 0.753197 0.608595 0.742965 11.00000 0.06339 C24 1 0.658243 0.662994 0.786702 11.00000 0.08543 AFIX 137 H24A 2 0.687710 0.748969 0.808743 11.00000 -1.50000 H24B 2 0.643994 0.628031 0.825863 11.00000 -1.50000 H24C 2 0.583409 0.646136 0.752960 11.00000 -1.50000 AFIX 0 C25 1 0.824034 0.565559 0.797292 11.00000 0.07470 AFIX 137 H25A 2 0.907176 0.610431 0.809017 11.00000 -1.50000 H25B 2 0.821647 0.481014 0.774781 11.00000 -1.50000 H25C 2 0.788481 0.577772 0.842745 11.00000 -1.50000 AFIX 0 C26 1 0.702679 0.493104 0.692544 11.00000 0.07105 AFIX 137 H26A 2 0.642765 0.497975 0.654648 11.00000 -1.50000 H26B 2 0.664686 0.442585 0.719248 11.00000 -1.50000 H26C 2 0.765767 0.459152 0.668984 11.00000 -1.50000 AFIX 0 C27 1 0.967577 0.862593 0.826524 11.00000 0.07623 C28 1 0.887041 0.879151 0.884329 11.00000 0.08290 AFIX 137 H28A 2 0.845232 0.941639 0.881947 11.00000 -1.50000 H28B 2 0.934833 0.901827 0.933349 11.00000 -1.50000 H28C 2 0.828482 0.804795 0.875428 11.00000 -1.50000 AFIX 0 C29 1 1.047686 1.007921 0.874577 11.00000 0.09000 AFIX 137 H29A 2 1.113176 1.006178 0.910224 11.00000 -1.50000 H29B 2 0.994175 1.053975 0.900849 11.00000 -1.50000 H29C 2 1.080435 1.044752 0.839488 11.00000 -1.50000 AFIX 0 C30 1 1.075933 0.809212 0.853922 11.00000 0.10047 AFIX 137 H30A 2 1.049143 0.723193 0.841752 11.00000 -1.50000 H30B 2 1.099725 0.845622 0.907507 11.00000 -1.50000 H30C 2 1.144280 0.826626 0.829032 11.00000 -1.50000 AFIX 0 C31 1 0.880264 0.826379 0.563379 11.00000 0.05097 C32 1 0.820974 0.927734 0.553141 11.00000 0.06430 AFIX 137 H32A 2 0.739699 0.893476 0.525991 11.00000 -1.50000 H32B 2 0.868211 0.970114 0.525310 11.00000 -1.50000 H32C 2 0.817875 0.983095 0.601712 11.00000 -1.50000 AFIX 0 C33 1 0.845397 0.718223 0.498259 11.00000 0.06326 AFIX 137 H33A 2 0.902942 0.668155 0.498904 11.00000 -1.50000 H33B 2 0.844541 0.740163 0.453115 11.00000 -1.50000 H33C 2 0.765542 0.674491 0.499493 11.00000 -1.50000 AFIX 0 C34 1 1.013954 0.867429 0.560853 11.00000 0.10398 AFIX 33 H34A 2 1.023149 0.888536 0.515917 11.00000 -1.50000 H34B 2 1.049277 0.936740 0.604329 11.00000 -1.50000 H34C 2 1.054554 0.803147 0.560703 11.00000 -1.50000 AFIX 0 F1 5 0.772806 0.384641 0.255359 11.00000 0.06730 F2 5 0.938512 0.361934 0.371344 11.00000 0.09686 F3 5 1.109207 0.543480 0.458225 11.00000 0.09845 F4 5 1.155321 0.762308 0.428278 11.00000 0.09601 F5 5 1.008137 0.792714 0.319844 11.00000 0.06875 F6 5 0.839885 0.901761 0.256235 11.00000 0.07624 F7 5 0.731830 1.045690 0.350855 11.00000 0.07476 F8 5 0.579136 0.957875 0.436608 11.00000 0.09345 F9 5 0.527632 0.724888 0.412248 11.00000 0.08811 F10 5 0.620998 0.576350 0.318685 11.00000 0.09106 F11 5 1.050852 0.614768 0.187935 11.00000 0.09207 F12 5 1.121457 0.616472 0.065201 11.00000 0.10757 F13 5 0.991747 0.693969 -0.029071 11.00000 0.13181 F14 5 0.778319 0.756713 -0.007179 11.00000 0.09752 F15 5 0.700452 0.742468 0.125988 11.00000 0.08210 F16 5 0.515300 0.598343 0.171951 11.00000 0.09799 F17 5 0.395220 0.443016 0.055698 11.00000 0.10823 F18 5 0.492993 0.273995 -0.027533 11.00000 0.13669 F19 5 0.723477 0.255304 0.007089 11.00000 0.10463 F20 5 0.855694 0.415702 0.120735 11.00000 0.07251 AFIX 66 C35 1 0.889666 0.596418 0.288584 11.00000 0.05880 C40 1 0.984266 0.691307 0.332502 11.00000 0.15008 C39 1 1.061367 0.675056 0.388709 11.00000 0.08019 C38 1 1.043868 0.563917 0.400999 11.00000 0.09412 C37 1 0.949268 0.469027 0.357082 11.00000 0.08988 C36 1 0.872167 0.485275 0.300874 11.00000 0.10323 AFIX 66 C41 1 0.740332 0.731300 0.284440 11.00000 0.05953 C42 1 0.766734 0.854141 0.293272 11.00000 0.06557 C43 1 0.711290 0.932182 0.343282 11.00000 0.05027 C44 1 0.629444 0.887384 0.384462 11.00000 0.09487 C45 1 0.603040 0.764543 0.375631 11.00000 0.09730 C46 1 0.658484 0.686500 0.325621 11.00000 0.08037 AFIX 66 C47 1 0.875552 0.672711 0.154790 11.00000 0.06138 C48 1 0.985585 0.644466 0.136737 11.00000 0.07551 C49 1 1.024150 0.654107 0.070250 11.00000 0.05901 C50 1 0.952682 0.691994 0.021816 11.00000 0.10946 C51 1 0.842648 0.720240 0.039868 11.00000 0.08428 C52 1 0.804082 0.710599 0.106355 11.00000 0.06655 AFIX 66 C53 1 0.694264 0.518004 0.153656 11.00000 0.06871 C58 1 0.746526 0.429362 0.109812 11.00000 0.09178 C57 1 0.677876 0.342009 0.045169 11.00000 0.07995 C56 1 0.556963 0.343297 0.024369 11.00000 0.11719 C55 1 0.504699 0.431937 0.068212 11.00000 0.12420 C54 1 0.573348 0.519291 0.132855 11.00000 0.08472 AFIX 0 B1 3 0.803956 0.636263 0.237019 11.00000 0.10635 HKLF 4 REM dy60_hp7a_38deg_a.res in P1 REM wR2 = 0.3688, GooF = S = 1.226, Restrained GooF = 1.233 for all data REM R1 = 0.1414 for 1072 Fo > 4sig(Fo) and 0.2142 for all 1850 data REM 277 parameters refined using 36 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.642, deepest hole -1.190, 1-sigma level 0.131 Q1 1 0.6384 0.9803 0.7919 11.00000 0.05 0.64 Q2 1 0.7472 0.7165 0.6735 11.00000 0.05 0.58 Q3 1 0.7837 1.0011 0.7409 11.00000 0.05 0.57 Q4 1 0.7979 0.9580 0.6870 11.00000 0.05 0.56 Q5 1 0.7969 0.9808 0.7177 11.00000 0.05 0.55 Q6 1 0.7578 0.7365 0.6982 11.00000 0.05 0.54 Q7 1 0.7636 0.8024 0.6940 11.00000 0.05 0.51 Q8 1 1.0149 0.5159 0.1284 11.00000 0.05 0.51 Q9 1 0.7725 0.8016 0.7543 11.00000 0.05 0.48 Q10 1 1.0046 0.5005 0.1059 11.00000 0.05 0.45 Q11 1 0.9254 0.8175 0.2978 11.00000 0.05 0.45 Q12 1 0.5380 0.7552 0.7639 11.00000 0.05 0.45 Q13 1 0.5577 0.4630 0.0955 11.00000 0.05 0.43 Q14 1 0.2868 1.0141 0.7870 11.00000 0.05 0.42 Q15 1 0.7805 0.3972 0.6628 11.00000 0.05 0.42 Q16 1 0.2833 1.0011 0.7654 11.00000 0.05 0.42 Q17 1 0.9504 0.7213 0.1977 11.00000 0.05 0.41 Q18 1 0.5729 0.4760 0.1237 11.00000 0.05 0.40 Q19 1 0.6061 1.1718 0.6002 11.00000 0.05 0.40 Q20 1 0.9408 0.6994 0.1685 11.00000 0.05 0.39 ; _shelx_res_checksum 25383 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 2.261 _oxdiff_exptl_absorpt_empirical_full_min 0.632 # start Validation Reply Form _vrf_THETM01_dy60_hp6 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_RINTA01_dy60_hp6 ; PROBLEM: The value of Rint is greater than 0.18 RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT029_dy60_hp6 ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.379 Why? RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_PLAT201_dy60_hp6 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 34 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT020_dy60_hp6 ; PROBLEM: The Value of Rint is Greater Than 0.12 ......... 0.209 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT084_dy60_hp6 ; PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.37 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT088_dy60_hp6 ; PROBLEM: Poor Data / Parameter Ratio .................... 6.68 Note RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT241_dy60_hp6 ; PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of Dy1 Check RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT242_dy60_hp6 ; PROBLEM: Low 'MainMol' Ueq as Compared to Neighbors of C35 Check RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT342_dy60_hp6 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.07707 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT412_dy60_hp6 ; PROBLEM: Short Intra XH3 .. XHn H3 ..H12C . 1.77 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT413_dy60_hp6 ; PROBLEM: Short Inter XH3 .. XHn H15B ..H15B . 1.95 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT911_dy60_hp6 ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.500 1820 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; # end Validation Reply Form _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_dy60_hp7 _database_code_depnum_ccdc_archive 'CCDC 2046713' loop_ _audit_author_name _audit_author_address 'Andreas M. Thiel' ;Aarhus University, Department of Chemistry Denmark ; _audit_update_record ; 2022-10-30 deposited with the CCDC. 2023-02-13 downloaded from the CCDC. ; _audit_creation_date 2020-03-04 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C34 H58 Dy, B C24 F20' _chemical_formula_sum 'C58 H58 B Dy F20' _chemical_formula_weight 1308.35 _chemical_melting_point ? _chemical_oxdiff_formula C58H58BDyF20 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.287(3) _cell_length_b 11.804(4) _cell_length_c 18.747(14) _cell_angle_alpha 107.27(5) _cell_angle_beta 95.31(4) _cell_angle_gamma 100.58(3) _cell_volume 2316(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 775 _cell_measurement_temperature 293 _cell_measurement_theta_max 25.7480 _cell_measurement_theta_min 2.0270 _shelx_estimated_absorpt_T_max 0.918 _shelx_estimated_absorpt_T_min 0.690 _exptl_absorpt_coefficient_mu 1.739 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.43641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1314 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_ambient_pressure 3520000 _diffrn_reflns_av_R_equivalents 0.2422 _diffrn_reflns_av_unetI/netI 0.1896 _diffrn_reflns_Laue_measured_fraction_full 0.379 _diffrn_reflns_Laue_measured_fraction_max 0.379 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 12789 _diffrn_reflns_point_group_measured_fraction_full 0.379 _diffrn_reflns_point_group_measured_fraction_max 0.379 _diffrn_reflns_theta_full 20.814 _diffrn_reflns_theta_max 20.814 _diffrn_reflns_theta_min 1.842 _diffrn_ambient_environment air _diffrn_ambient_temperature 293 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3590 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.379 _diffrn_measured_fraction_theta_max 0.379 _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 -31.00 9.00 1.00 30.00 -- 12.55 81.00 151.00 40 2 \w 13.00 56.00 1.00 30.00 -- 12.55 -77.00-150.00 43 3 \w -13.00 34.00 1.00 30.00 -- 12.55 -38.00-150.00 47 4 \w -32.00 25.00 1.00 30.00 -- 12.55 39.00 -12.00 57 5 \w 72.00 108.00 1.00 30.00 -- 12.55 178.00 90.00 36 6 \w -28.00 20.00 1.00 30.00 -- 12.55 53.00 162.00 48 7 \w 58.00 109.00 1.00 30.00 -- 12.55-178.00 -90.00 51 8 \w -35.00 -12.00 1.00 30.00 -- -13.41 77.00 -30.00 23 9 \w 2.00 37.00 1.00 30.00 -- -13.41 -99.00-150.00 35 10 \w -8.00 31.00 1.00 30.00 -- -13.41 -81.00 29.00 39 11 \w -42.00 33.00 1.00 30.00 -- -13.41 13.00 -3.00 75 12 \w 12.00 35.00 1.00 30.00 -- 12.55 -77.00 60.00 23 13 \w 12.00 35.00 1.00 30.00 -- 12.55 -77.00 30.00 23 14 \w 34.00 61.00 1.00 30.00 -- 12.55 -99.00 60.00 27 15 \w 34.00 61.00 1.00 30.00 -- 12.55 -99.00 30.00 27 16 \w -14.00 33.00 1.00 30.00 -- -13.41 -38.00-180.00 47 17 \w -35.00 -12.00 1.00 30.00 -- -13.41 77.00 120.00 23 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0150647000 _diffrn_orient_matrix_UB_12 -0.0165615000 _diffrn_orient_matrix_UB_13 -0.0398604000 _diffrn_orient_matrix_UB_21 -0.0300776000 _diffrn_orient_matrix_UB_22 -0.0591172000 _diffrn_orient_matrix_UB_23 -0.0014318000 _diffrn_orient_matrix_UB_31 -0.0553001000 _diffrn_orient_matrix_UB_32 0.0198973000 _diffrn_orient_matrix_UB_33 0.0042861000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 886 _reflns_number_total 1834 _reflns_odcompleteness_completeness 38.60 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 20.77 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.568 _refine_diff_density_min -1.037 _refine_diff_density_rms 0.125 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 1834 _refine_ls_number_restraints 89 _refine_ls_R_factor_all 0.2501 _refine_ls_R_factor_gt 0.1524 _refine_ls_restrained_S_all 1.174 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3403 _refine_ls_wR_factor_ref 0.3967 _refine_special_details ? _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. Restrained distances C27-C19 1.55 with sigma of 0.1 C7-C6 \\sim C8-C6 \\sim C9-C6 with sigma of 0.02 C13-C10 \\sim C11-C10 \\sim C12-C10 with sigma of 0.02 C17-C14 \\sim C15-C14 \\sim C16-C14 with sigma of 0.02 C26-C23 \\sim C25-C23 \\sim C24-C23 with sigma of 0.02 C33-C31 \\sim C34-C31 \\sim C32-C31 with sigma of 0.02 C30-C27 \\sim C29-C27 \\sim C28-C27 with sigma of 0.02 C7-C8 \\sim C7-C9 \\sim C8-C9 with sigma of 0.02 C13-C11 \\sim C13-C12 \\sim C11-C12 with sigma of 0.02 C17-C15 \\sim C17-C16 \\sim C16-C15 with sigma of 0.02 C26-C25 \\sim C25-C24 \\sim C25-C24 with sigma of 0.02 C33-C34 \\sim C33-C32 \\sim C34-C32 with sigma of 0.02 C30-C29 \\sim C30-C28 \\sim C29-C28 with sigma of 0.02 C7-C1 \\sim C8-C1 \\sim C9-C1 with sigma of 0.02 C13-C2 \\sim C11-C2 \\sim C12-C2 with sigma of 0.02 C17-C4 \\sim C15-C4 \\sim C16-C4 with sigma of 0.02 C26-C18 \\sim C25-C18 \\sim C24-C18 with sigma of 0.02 C33-C21 \\sim C34-C21 \\sim C32-C21 with sigma of 0.02 C30-C19 \\sim C29-C19 \\sim C28-C19 with sigma of 0.02 3. Restrained planarity C54, C55, C56, C57, C58, F16, F17, F18, F19, F20, B1, C53 with sigma of 0.1 C47, C52, C51, C50, C49, C48, F15, F14, F13, F12, F11, B1 with sigma of 0.1 C35, C36, C37, C38, C39, C40, F1, F2, F3, F4, F5, B1 with sigma of 0.1 C41, C46, C45, C44, C43, C42, F10, F9, F8, F7, F6, B1 with sigma of 0.1 4.a Me refined with riding coordinates: C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B, H17C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C) 4.b Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C20(H20), C22(H22) 4.c Fitted pentagon refined as free rotating group: C1(C2,C3,C4,C5), C21(C20,C19,C18,C22) 4.d Fitted hexagon refined as free rotating group: C35(C40,C39,C38,C37,C36), C41(C42,C43,C44,C45,C46), C47(C48,C49,C50,C51,C52), C53(C58,C57,C56,C55,C54) 4.e Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B, H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.6917(3) 0.8445(3) 0.7228(4) 0.145(6) Uani 1 1 d . . . . . C1 C 0.570(2) 0.995(3) 0.720(3) 0.053(12) Uiso 1 1 d D . . . . C2 C 0.509(4) 0.931(4) 0.764(3) 0.18(4) Uiso 1 1 d DG . . . . C3 C 0.451(3) 0.813(3) 0.715(4) 0.13(2) Uiso 1 1 d G . . . . H3 H 0.404279 0.751747 0.729521 0.153 Uiso 1 1 calc R . . . . C4 C 0.475(3) 0.804(3) 0.641(3) 0.071(14) Uiso 1 1 d DG . . . . C5 C 0.549(3) 0.917(4) 0.644(3) 0.13(2) Uiso 1 1 d G . . . . H5 H 0.578751 0.935688 0.603266 0.151 Uiso 1 1 calc R . . . . C6 C 0.661(4) 1.124(5) 0.752(3) 0.12(2) Uiso 1 1 d D . . . . C7 C 0.775(3) 1.101(4) 0.794(3) 0.12(2) Uiso 1 1 d D . . . . H7A H 0.812402 1.047814 0.758593 0.178 Uiso 1 1 calc R . . . . H7B H 0.832358 1.177107 0.818787 0.178 Uiso 1 1 calc R . . . . H7C H 0.750473 1.064323 0.831390 0.178 Uiso 1 1 calc R . . . . C8 C 0.595(4) 1.210(4) 0.805(3) 0.12(2) Uiso 1 1 d D . . . . H8A H 0.520992 1.213977 0.777372 0.180 Uiso 1 1 calc GR . . . . H8B H 0.646916 1.289335 0.826029 0.180 Uiso 1 1 calc GR . . . . H8C H 0.575236 1.178305 0.845596 0.180 Uiso 1 1 calc GR . . . . C9 C 0.689(4) 1.163(4) 0.682(4) 0.101(18) Uiso 1 1 d D . . . . H9A H 0.689216 1.092713 0.640401 0.151 Uiso 1 1 calc GR . . . . H9B H 0.767039 1.218474 0.694021 0.151 Uiso 1 1 calc GR . . . . H9C H 0.627052 1.202820 0.668734 0.151 Uiso 1 1 calc GR . . . . C10 C 0.477(3) 0.950(3) 0.841(5) 0.089(17) Uiso 1 1 d D . . . . C11 C 0.592(4) 1.006(3) 0.907(4) 0.082(15) Uiso 1 1 d D . . . . H11A H 0.616198 0.942226 0.923027 0.124 Uiso 1 1 calc GR . . . . H11B H 0.570659 1.063550 0.949650 0.124 Uiso 1 1 calc GR . . . . H11C H 0.658671 1.046745 0.889198 0.124 Uiso 1 1 calc GR . . . . C12 C 0.410(4) 0.826(4) 0.854(5) 0.100(18) Uiso 1 1 d D . . . . H12A H 0.334347 0.836078 0.871342 0.150 Uiso 1 1 calc GR . . . . H12B H 0.461713 0.807837 0.890441 0.150 Uiso 1 1 calc GR . . . . H12C H 0.394513 0.760649 0.806661 0.150 Uiso 1 1 calc GR . . . . C13 C 0.385(4) 1.040(4) 0.862(5) 0.15(3) Uiso 1 1 d D . . . . H13A H 0.367819 1.048167 0.911842 0.220 Uiso 1 1 calc R . . . . H13B H 0.422955 1.118321 0.859175 0.220 Uiso 1 1 calc R . . . . H13C H 0.310982 1.007554 0.826222 0.220 Uiso 1 1 calc R . . . . C14 C 0.419(3) 0.699(5) 0.564(4) 0.096(18) Uiso 1 1 d D . . . . C15 C 0.517(4) 0.637(3) 0.519(4) 0.087(16) Uiso 1 1 d D . . . . H15A H 0.475620 0.574851 0.473249 0.130 Uiso 1 1 calc R . . . . H15B H 0.573305 0.697704 0.506904 0.130 Uiso 1 1 calc R . . . . H15C H 0.561046 0.601780 0.549941 0.130 Uiso 1 1 calc R . . . . C16 C 0.345(3) 0.743(4) 0.504(3) 0.082(15) Uiso 1 1 d D . . . . H16A H 0.299373 0.799440 0.529510 0.123 Uiso 1 1 calc GR . . . . H16B H 0.290639 0.674208 0.467266 0.123 Uiso 1 1 calc GR . . . . H16C H 0.401788 0.782731 0.478717 0.123 Uiso 1 1 calc GR . . . . C17 C 0.324(4) 0.587(4) 0.573(5) 0.15(3) Uiso 1 1 d D . . . . H17A H 0.294027 0.527154 0.523795 0.222 Uiso 1 1 calc R . . . . H17B H 0.363966 0.550396 0.604831 0.222 Uiso 1 1 calc R . . . . H17C H 0.256901 0.614880 0.594640 0.222 Uiso 1 1 calc R . . . . C21 C 0.861(3) 0.798(4) 0.631(3) 0.11(2) Uiso 1 1 d D . . . . C20 C 0.919(2) 0.874(2) 0.705(3) 0.080(16) Uiso 1 1 d G . . . . H20 H 0.964372 0.953141 0.716863 0.096 Uiso 1 1 calc R . . . . C19 C 0.895(3) 0.808(3) 0.756(3) 0.091(18) Uiso 1 1 d DG . . . . C18 C 0.822(3) 0.691(3) 0.714(3) 0.10(2) Uiso 1 1 d DG . . . . C22 C 0.801(3) 0.685(3) 0.637(3) 0.088(18) Uiso 1 1 d G . . . . H22 H 0.756382 0.617966 0.597363 0.105 Uiso 1 1 calc R . . . . C23 C 0.745(2) 0.599(2) 0.746(3) 0.037(10) Uiso 1 1 d D . . . . C24 C 0.651(5) 0.661(5) 0.784(4) 0.087(16) Uiso 1 1 d D . . . . H24A H 0.690830 0.740738 0.817553 0.131 Uiso 1 1 calc GR . . . . H24B H 0.612664 0.613909 0.813337 0.131 Uiso 1 1 calc GR . . . . H24C H 0.590852 0.666965 0.747079 0.131 Uiso 1 1 calc GR . . . . C25 C 0.831(4) 0.573(4) 0.803(3) 0.077(14) Uiso 1 1 d D . . . . H25A H 0.911623 0.584317 0.789967 0.116 Uiso 1 1 calc GR . . . . H25B H 0.803945 0.490389 0.801843 0.116 Uiso 1 1 calc GR . . . . H25C H 0.831258 0.627337 0.852265 0.116 Uiso 1 1 calc GR . . . . C26 C 0.693(3) 0.484(3) 0.680(4) 0.078(15) Uiso 1 1 d D . . . . H26A H 0.649938 0.504181 0.640029 0.118 Uiso 1 1 calc GR . . . . H26B H 0.638330 0.427850 0.695684 0.118 Uiso 1 1 calc GR . . . . H26C H 0.758578 0.448222 0.661038 0.118 Uiso 1 1 calc GR . . . . C27 C 0.961(3) 0.865(3) 0.829(4) 0.061(13) Uiso 1 1 d D . . . . C28 C 0.896(4) 0.886(4) 0.910(4) 0.084(15) Uiso 1 1 d D . . . . H28A H 0.864967 0.958187 0.919607 0.126 Uiso 1 1 calc GR . . . . H28B H 0.956341 0.893012 0.951287 0.126 Uiso 1 1 calc GR . . . . H28C H 0.830457 0.816961 0.902884 0.126 Uiso 1 1 calc GR . . . . C29 C 1.043(3) 1.011(3) 0.862(5) 0.091(17) Uiso 1 1 d D . . . . H29A H 1.095003 1.025663 0.826299 0.137 Uiso 1 1 calc GR . . . . H29B H 1.092432 1.024944 0.909630 0.137 Uiso 1 1 calc GR . . . . H29C H 0.988605 1.065771 0.868613 0.137 Uiso 1 1 calc GR . . . . C30 C 1.076(4) 0.816(5) 0.867(5) 0.17(3) Uiso 1 1 d D . . . . H30A H 1.107152 0.869245 0.917815 0.258 Uiso 1 1 calc R . . . . H30B H 1.046120 0.734845 0.868400 0.258 Uiso 1 1 calc R . . . . H30C H 1.140530 0.815368 0.837110 0.258 Uiso 1 1 calc R . . . . C31 C 0.884(2) 0.830(3) 0.565(4) 0.066(14) Uiso 1 1 d D . . . . C32 C 0.815(4) 0.929(4) 0.553(5) 0.11(2) Uiso 1 1 d D . . . . H32A H 0.834119 0.946714 0.507593 0.171 Uiso 1 1 calc R . . . . H32B H 0.728530 0.898996 0.547286 0.171 Uiso 1 1 calc R . . . . H32C H 0.840269 1.002118 0.595257 0.171 Uiso 1 1 calc R . . . . C33 C 0.846(4) 0.718(4) 0.489(4) 0.12(2) Uiso 1 1 d D . . . . H33A H 0.863653 0.744600 0.447235 0.185 Uiso 1 1 calc R . . . . H33B H 0.890955 0.657009 0.492121 0.185 Uiso 1 1 calc R . . . . H33C H 0.760186 0.683321 0.482961 0.185 Uiso 1 1 calc R . . . . C34 C 1.024(3) 0.885(4) 0.567(6) 0.102(18) Uiso 1 1 d D . . . . H34A H 1.058336 0.940219 0.616648 0.153 Uiso 1 1 calc GR . . . . H34B H 1.031821 0.927370 0.530704 0.153 Uiso 1 1 calc GR . . . . H34C H 1.067231 0.820209 0.554877 0.153 Uiso 1 1 calc GR . . . . F1 F 0.776(2) 0.386(2) 0.257(3) 0.084(8) Uiso 1 1 d . . . . . F2 F 0.935(2) 0.361(2) 0.372(3) 0.081(8) Uiso 1 1 d . . . . . F3 F 1.110(3) 0.542(3) 0.453(4) 0.116(10) Uiso 1 1 d . . . . . F4 F 1.158(3) 0.763(3) 0.434(4) 0.145(13) Uiso 1 1 d . . . . . F5 F 1.005(2) 0.792(2) 0.317(3) 0.078(7) Uiso 1 1 d . . . . . F6 F 0.843(2) 0.905(2) 0.260(3) 0.093(8) Uiso 1 1 d . . . . . F7 F 0.733(2) 1.051(2) 0.359(3) 0.091(8) Uiso 1 1 d . . . . . F8 F 0.581(2) 0.963(2) 0.441(3) 0.093(9) Uiso 1 1 d . . . . . F9 F 0.523(3) 0.722(3) 0.412(3) 0.105(9) Uiso 1 1 d . . . . . F10 F 0.621(2) 0.576(2) 0.316(3) 0.087(8) Uiso 1 1 d . . . . . F11 F 1.054(3) 0.616(3) 0.191(4) 0.123(11) Uiso 1 1 d . . . . . F12 F 1.124(3) 0.615(2) 0.065(4) 0.103(9) Uiso 1 1 d . . . . . F13 F 0.991(4) 0.689(3) -0.020(5) 0.18(2) Uiso 1 1 d . . . . . F14 F 0.777(2) 0.755(2) 0.003(3) 0.096(9) Uiso 1 1 d . . . . . F15 F 0.697(2) 0.743(2) 0.120(4) 0.098(9) Uiso 1 1 d . . . . . F16 F 0.520(2) 0.597(3) 0.172(3) 0.096(9) Uiso 1 1 d . . . . . F17 F 0.396(3) 0.445(3) 0.054(4) 0.143(13) Uiso 1 1 d . . . . . F18 F 0.504(4) 0.283(4) -0.018(4) 0.153(14) Uiso 1 1 d . . . . . F19 F 0.727(3) 0.255(3) 0.006(4) 0.105(10) Uiso 1 1 d . . . . . F20 F 0.858(3) 0.421(3) 0.120(3) 0.102(9) Uiso 1 1 d . . . . . C35 C 0.883(3) 0.593(3) 0.288(2) 0.084(16) Uiso 1 1 d . . . . . C40 C 0.979(3) 0.687(2) 0.331(3) 0.11(2) Uiso 1 1 d G . . . . C39 C 1.058(3) 0.670(3) 0.387(3) 0.073(14) Uiso 1 1 d G . . . . C38 C 1.041(3) 0.557(3) 0.399(2) 0.084(16) Uiso 1 1 d G . . . . C37 C 0.945(3) 0.463(2) 0.355(3) 0.097(18) Uiso 1 1 d G . . . . C36 C 0.866(3) 0.481(3) 0.300(3) 0.098(18) Uiso 1 1 d G . . . . C41 C 0.737(2) 0.737(2) 0.288(2) 0.067(13) Uiso 1 1 d . . . . . C42 C 0.764(2) 0.862(3) 0.301(2) 0.072(14) Uiso 1 1 d G . . . . C43 C 0.709(2) 0.938(2) 0.352(3) 0.085(16) Uiso 1 1 d G . . . . C44 C 0.625(2) 0.889(3) 0.391(2) 0.080(15) Uiso 1 1 d G . . . . C45 C 0.597(2) 0.764(3) 0.378(2) 0.101(18) Uiso 1 1 d G . . . . C46 C 0.653(3) 0.689(2) 0.327(3) 0.098(18) Uiso 1 1 d G . . . . C47 C 0.873(4) 0.672(2) 0.155(3) 0.077(15) Uiso 1 1 d . . . . . C48 C 0.984(3) 0.643(2) 0.141(3) 0.15(3) Uiso 1 1 d G . . . . C49 C 1.029(3) 0.651(2) 0.076(3) 0.076(15) Uiso 1 1 d G . . . . C50 C 0.963(4) 0.688(3) 0.024(3) 0.11(2) Uiso 1 1 d G . . . . C51 C 0.851(4) 0.718(2) 0.038(3) 0.14(2) Uiso 1 1 d G . . . . C52 C 0.806(2) 0.710(2) 0.103(4) 0.095(18) Uiso 1 1 d G . . . . C53 C 0.704(4) 0.514(3) 0.151(3) 0.099(18) Uiso 1 1 d . . . . . C58 C 0.751(2) 0.422(4) 0.106(3) 0.104(19) Uiso 1 1 d G . . . . C57 C 0.677(4) 0.336(3) 0.042(3) 0.080(15) Uiso 1 1 d G . . . . C56 C 0.557(4) 0.342(3) 0.024(3) 0.15(3) Uiso 1 1 d G . . . . C55 C 0.510(2) 0.434(4) 0.070(3) 0.063(13) Uiso 1 1 d G . . . . C54 C 0.584(4) 0.520(3) 0.134(3) 0.102(19) Uiso 1 1 d G . . . . B1 B 0.802(6) 0.640(5) 0.236(4) 0.16(4) Uiso 1 1 d . . . . . 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 0.0703(19) 0.123(3) 0.253(19) 0.078(6) 0.032(5) 0.0172(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 2.45(3) . ? Dy1 C2 2.54(4) . ? Dy1 C3 2.66(3) . ? Dy1 C4 2.64(4) . ? Dy1 C5 2.51(4) . ? Dy1 C21 2.71(4) . ? Dy1 C20 2.59(3) . ? Dy1 C19 2.46(3) . ? Dy1 C18 2.51(3) . ? Dy1 C22 2.66(3) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 C6 1.58(6) . ? C2 C3 1.4200 . ? C2 C10 1.49(9) . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C4 C14 1.58(8) . ? C6 C7 1.56(3) . ? C6 C8 1.54(3) . ? C6 C9 1.55(3) . ? C10 C11 1.61(5) . ? C10 C12 1.60(5) . ? C10 C13 1.61(5) . ? C14 C15 1.61(4) . ? C14 C16 1.61(5) . ? C14 C17 1.61(4) . ? C21 C20 1.4200 . ? C21 C22 1.4200 . ? C21 C31 1.43(7) . ? C20 C19 1.4200 . ? C19 C18 1.4200 . ? C19 C27 1.40(7) . ? C18 C22 1.4200 . ? C18 C23 1.56(4) . ? C23 C24 1.51(3) . ? C23 C25 1.51(3) . ? C23 C26 1.51(3) . ? C27 C28 1.71(6) . ? C27 C29 1.70(6) . ? C27 C30 1.70(6) . ? C31 C32 1.59(4) . ? C31 C33 1.58(4) . ? C31 C34 1.59(4) . ? F1 C36 1.35(5) . ? F2 C37 1.32(3) . ? F3 C38 1.31(6) . ? F4 C39 1.43(6) . ? F5 C40 1.33(3) . ? F6 C42 1.34(4) . ? F7 C43 1.28(3) . ? F8 C44 1.29(4) . ? F9 C45 1.21(4) . ? F10 C46 1.26(3) . ? F11 C48 1.32(6) . ? F12 C49 1.24(3) . ? F13 C50 0.92(9) . ? F14 C51 1.25(5) . ? F15 C52 1.39(3) . ? F16 C54 1.34(4) . ? F17 C55 1.32(4) . ? F18 C56 0.94(8) . ? F19 C57 1.26(4) . ? F20 C58 1.22(4) . ? C35 C40 1.3900 . ? C35 C36 1.3900 . ? C35 B1 1.57(7) . ? C40 C39 1.3900 . ? C39 C38 1.3900 . ? C38 C37 1.3900 . ? C37 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 B1 1.61(7) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C47 B1 1.89(7) . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C53 C58 1.3900 . ? C53 C54 1.3900 . ? C53 B1 1.90(7) . ? C58 C57 1.3900 . ? C57 C56 1.3900 . ? C56 C55 1.3900 . ? C55 C54 1.3900 . ? 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 C1 Dy1 C2 33.0(4) . . ? C1 Dy1 C3 53.3(4) . . ? C1 Dy1 C4 53.5(5) . . ? C1 Dy1 C5 33.3(4) . . ? C1 Dy1 C21 122.7(13) . . ? C1 Dy1 C20 123.2(9) . . ? C1 Dy1 C19 146.6(11) . . ? C1 Dy1 C18 174.6(16) . . ? C1 Dy1 C22 143.3(17) . . ? C2 Dy1 C3 31.6(4) . . ? C2 Dy1 C4 52.6(4) . . ? C2 Dy1 C21 154.2(13) . . ? C2 Dy1 C20 150.8(12) . . ? C2 Dy1 C22 154.8(13) . . ? C3 Dy1 C21 139.9(17) . . ? C3 Dy1 C22 123.7(13) . . ? C4 Dy1 C3 31.1(3) . . ? C4 Dy1 C21 110.2(15) . . ? C4 Dy1 C22 103.7(12) . . ? C5 Dy1 C2 54.1(4) . . ? C5 Dy1 C3 52.7(4) . . ? C5 Dy1 C4 31.9(5) . . ? C5 Dy1 C21 100.8(12) . . ? C5 Dy1 C20 118.3(13) . . ? C5 Dy1 C18 142.6(16) . . ? C5 Dy1 C22 111.6(14) . . ? C20 Dy1 C3 169.6(18) . . ? C20 Dy1 C4 138.5(17) . . ? C20 Dy1 C21 31.0(4) . . ? C20 Dy1 C22 51.8(4) . . ? C19 Dy1 C2 149.4(15) . . ? C19 Dy1 C3 155.7(13) . . ? C19 Dy1 C4 156.5(12) . . ? C19 Dy1 C5 150.6(13) . . ? C19 Dy1 C21 52.5(4) . . ? C19 Dy1 C20 32.5(3) . . ? C19 Dy1 C18 33.1(3) . . ? C19 Dy1 C22 53.1(3) . . ? C18 Dy1 C2 151.8(12) . . ? C18 Dy1 C3 129.1(9) . . ? C18 Dy1 C4 125.3(12) . . ? C18 Dy1 C21 52.0(4) . . ? C18 Dy1 C20 53.5(3) . . ? C18 Dy1 C22 31.7(3) . . ? C22 Dy1 C21 30.6(4) . . ? C2 C1 Dy1 77.3(15) . . ? C2 C1 C5 108.0 . . ? C2 C1 C6 125(3) . . ? C5 C1 Dy1 75.8(18) . . ? C5 C1 C6 126(3) . . ? C6 C1 Dy1 106.7(14) . . ? C1 C2 Dy1 69.8(13) . . ? C1 C2 C3 108.0 . . ? C1 C2 C10 141(3) . . ? C3 C2 Dy1 78.8(12) . . ? C3 C2 C10 110(3) . . ? C10 C2 Dy1 123(2) . . ? C2 C3 Dy1 69.7(13) . . ? C2 C3 C4 108.0 . . ? C4 C3 Dy1 73.7(17) . . ? C3 C4 Dy1 75.3(16) . . ? C3 C4 C14 129(3) . . ? C5 C4 Dy1 69.0(11) . . ? C5 C4 C3 108.0 . . ? C5 C4 C14 122(3) . . ? C14 C4 Dy1 127.8(17) . . ? C1 C5 Dy1 71.0(16) . . ? C4 C5 Dy1 79.1(11) . . ? C4 C5 C1 108.0 . . ? C7 C6 C1 104(2) . . ? C8 C6 C1 107(3) . . ? C8 C6 C7 113(2) . . ? C8 C6 C9 113(2) . . ? C9 C6 C1 106(3) . . ? C9 C6 C7 113(2) . . ? C2 C10 C11 114(3) . . ? C2 C10 C12 113(4) . . ? C2 C10 C13 113(4) . . ? C11 C10 C13 105(4) . . ? C12 C10 C11 105(4) . . ? C12 C10 C13 105(4) . . ? C4 C14 C15 115(3) . . ? C4 C14 C16 114(3) . . ? C4 C14 C17 115(3) . . ? C15 C14 C16 104(4) . . ? C17 C14 C15 104(3) . . ? C17 C14 C16 105(4) . . ? C20 C21 Dy1 69.8(13) . . ? C20 C21 C22 108.0 . . ? C20 C21 C31 122(3) . . ? C22 C21 Dy1 72.9(9) . . ? C22 C21 C31 129(3) . . ? C31 C21 Dy1 131.4(18) . . ? C21 C20 Dy1 79.2(15) . . ? C19 C20 Dy1 68.8(14) . . ? C19 C20 C21 108.0 . . ? C20 C19 Dy1 78.7(14) . . ? C20 C19 C18 108.0 . . ? C18 C19 Dy1 75.3(11) . . ? C27 C19 Dy1 121.0(19) . . ? C27 C19 C20 115(3) . . ? C27 C19 C18 136(3) . . ? C19 C18 Dy1 71.6(12) . . ? C19 C18 C23 127(2) . . ? C22 C18 Dy1 80.1(16) . . ? C22 C18 C19 108.0 . . ? C22 C18 C23 122(3) . . ? C23 C18 Dy1 101.4(13) . . ? C21 C22 Dy1 76.5(10) . . ? C18 C22 Dy1 68.2(15) . . ? C18 C22 C21 108.0 . . ? C24 C23 C18 106.8(18) . . ? C25 C23 C18 107.3(18) . . ? C25 C23 C24 110(2) . . ? C25 C23 C26 110(2) . . ? C26 C23 C18 106.9(18) . . ? C26 C23 C24 115(4) . . ? C19 C27 C28 124(3) . . ? C19 C27 C29 125(3) . . ? C19 C27 C30 125(3) . . ? C29 C27 C28 91(4) . . ? C30 C27 C28 92(4) . . ? C30 C27 C29 91(4) . . ? C21 C31 C32 113(3) . . ? C21 C31 C33 113(3) . . ? C21 C31 C34 113(3) . . ? C32 C31 C34 105(3) . . ? C33 C31 C32 106(3) . . ? C33 C31 C34 105(3) . . ? C40 C35 C36 120.0 . . ? C40 C35 B1 110(3) . . ? C36 C35 B1 130(3) . . ? F5 C40 C35 121(4) . . ? F5 C40 C39 119(3) . . ? C39 C40 C35 120.0 . . ? C40 C39 F4 123(3) . . ? C40 C39 C38 120.0 . . ? C38 C39 F4 117(3) . . ? F3 C38 C39 120(3) . . ? F3 C38 C37 119(3) . . ? C37 C38 C39 120.0 . . ? F2 C37 C38 115(4) . . ? F2 C37 C36 125(4) . . ? C38 C37 C36 120.0 . . ? F1 C36 C35 121(3) . . ? F1 C36 C37 119(3) . . ? C37 C36 C35 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 B1 126(3) . . ? C46 C41 B1 114(3) . . ? F6 C42 C41 118(2) . . ? F6 C42 C43 122(2) . . ? C43 C42 C41 120.0 . . ? F7 C43 C42 118(3) . . ? F7 C43 C44 122(3) . . ? C42 C43 C44 120.0 . . ? F8 C44 C43 118(3) . . ? F8 C44 C45 122(3) . . ? C45 C44 C43 120.0 . . ? F9 C45 C44 120(3) . . ? F9 C45 C46 120(3) . . ? C44 C45 C46 120.0 . . ? F10 C46 C41 123(3) . . ? F10 C46 C45 117(3) . . ? C45 C46 C41 120.0 . . ? C48 C47 C52 120.0 . . ? C48 C47 B1 120(4) . . ? C52 C47 B1 120(4) . . ? F11 C48 C47 122(4) . . ? F11 C48 C49 118(4) . . ? C47 C48 C49 120.0 . . ? F12 C49 C48 116(5) . . ? F12 C49 C50 124(5) . . ? C48 C49 C50 120.0 . . ? F13 C50 C49 119(6) . . ? F13 C50 C51 121(6) . . ? C51 C50 C49 120.0 . . ? F14 C51 C50 133(5) . . ? F14 C51 C52 107(5) . . ? C52 C51 C50 120.0 . . ? C47 C52 F15 119(5) . . ? C51 C52 F15 121(4) . . ? C51 C52 C47 120.0 . . ? C58 C53 C54 120.0 . . ? C58 C53 B1 122(3) . . ? C54 C53 B1 117(3) . . ? F20 C58 C53 119(4) . . ? F20 C58 C57 120(4) . . ? C53 C58 C57 120.0 . . ? F19 C57 C58 115(4) . . ? F19 C57 C56 125(4) . . ? C56 C57 C58 120.0 . . ? F18 C56 C57 121(5) . . ? F18 C56 C55 119(5) . . ? C55 C56 C57 120.0 . . ? F17 C55 C56 122(4) . . ? F17 C55 C54 118(4) . . ? C56 C55 C54 120.0 . . ? F16 C54 C53 129(4) . . ? F16 C54 C55 111(4) . . ? C55 C54 C53 120.0 . . ? C35 B1 C41 109(3) . . ? C35 B1 C47 115(4) . . ? C35 B1 C53 113(3) . . ? C41 B1 C47 120(3) . . ? C41 B1 C53 118(3) . . ? C47 B1 C53 78(2) . . ? _shelx_res_file ; TITL dy60_hp8_38deg_a.res in P-1 dy60_hp8_38deg.res created by SHELXL-2018/3 at 09:26:49 on 04-Mar-2020 REM Old TITL Dy60_HP8_38deg in P-1 REM SHELXT solution in P-1: R1 0.362, Rweak 0.294, Alpha 0.287 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C144 B8 F48 I3 CELL 0.71073 11.2869 11.8038 18.7471 107.268 95.305 100.581 ZERR 2 0.003 0.0044 0.0144 0.054 0.044 0.027 LATT 1 SFAC C H B Dy F UNIT 116 116 2 2 40 DFIX 1.55 0.1 C27 C19 SADI C7 C6 C8 C6 C9 C6 SADI C13 C10 C11 C10 C12 C10 SADI C17 C14 C15 C14 C16 C14 SADI C26 C23 C25 C23 C24 C23 SADI C33 C31 C34 C31 C32 C31 SADI C30 C27 C29 C27 C28 C27 SADI C7 C8 C7 C9 C8 C9 SADI C13 C11 C13 C12 C11 C12 SADI C17 C15 C17 C16 C16 C15 SADI C26 C25 C25 C24 C25 C24 SADI C33 C34 C33 C32 C34 C32 SADI C30 C29 C30 C28 C29 C28 SADI C7 C1 C8 C1 C9 C1 SADI C13 C2 C11 C2 C12 C2 SADI C17 C4 C15 C4 C16 C4 SADI C26 C18 C25 C18 C24 C18 SADI C33 C21 C34 C21 C32 C21 SADI C30 C19 C29 C19 C28 C19 FLAT C54 C55 C56 C57 C58 F16 F17 F18 F19 F20 B1 C53 FLAT C47 C52 C51 C50 C49 C48 F15 F14 F13 F12 F11 B1 FLAT C35 C36 C37 C38 C39 C40 F1 F2 F3 F4 F5 B1 FLAT C41 C46 C45 C44 C43 C42 F10 F9 F8 F7 F6 B1 L.S. 20 0 0 PLAN 20 SIZE 0.16 0.23 0.05 FREE Dy1 C24 FREE Dy1 C7 list 4 fmap 2 53 acta SHEL 100 0.83 OMIT 0 180 OMIT -4 0 2 OMIT -6 0 2 OMIT -4 1 3 OMIT -6 2 1 OMIT -6 -3 2 OMIT -6 0 4 OMIT -4 3 0 OMIT -4 -2 5 OMIT -6 -1 3 OMIT 4 -2 1 OMIT -6 4 0 OMIT -6 1 5 OMIT 7 1 0 OMIT -5 -3 3 OMIT -5 -2 2 OMIT -5 2 0 OMIT 5 1 0 OMIT -3 1 0 OMIT 4 0 0 OMIT -7 1 1 OMIT -4 -1 1 OMIT -3 -4 5 OMIT -4 -5 5 OMIT -5 -1 5 OMIT -9 5 2 OMIT -2 -3 3 OMIT -4 -8 5 OMIT -7 -1 2 OMIT -2 -4 4 OMIT 3 0 1 OMIT -6 -2 3 OMIT -6 -4 2 OMIT 7 -5 4 OMIT -5 -4 5 OMIT 4 2 1 OMIT -4 -1 4 REM REM REM WGHT 0.200000 FVAR 0.36885 DY1 4 0.691678 0.844499 0.722752 11.00000 0.07025 0.12324 = 0.25275 0.07796 0.03200 0.01717 AFIX 56 C1 1 0.570313 0.995407 0.719882 11.00000 0.05349 C2 1 0.509389 0.931177 0.763969 11.00000 0.18150 C3 1 0.450708 0.812735 0.715313 11.00000 0.12767 AFIX 43 H3 2 0.404279 0.751747 0.729521 11.00000 -1.20000 AFIX 55 C4 1 0.475365 0.803764 0.641155 11.00000 0.07130 C5 1 0.549285 0.916662 0.643979 11.00000 0.12561 AFIX 43 H5 2 0.578751 0.935688 0.603266 11.00000 -1.20000 AFIX 0 C6 1 0.660916 1.124237 0.752005 11.00000 0.11603 C7 1 0.774982 1.101156 0.794247 11.00000 0.11879 AFIX 33 H7A 2 0.812402 1.047814 0.758593 11.00000 -1.50000 H7B 2 0.832358 1.177107 0.818787 11.00000 -1.50000 H7C 2 0.750473 1.064323 0.831390 11.00000 -1.50000 AFIX 0 C8 1 0.594754 1.209536 0.805294 11.00000 0.11970 AFIX 137 H8A 2 0.520992 1.213977 0.777372 11.00000 -1.50000 H8B 2 0.646916 1.289335 0.826029 11.00000 -1.50000 H8C 2 0.575236 1.178305 0.845596 11.00000 -1.50000 AFIX 0 C9 1 0.688705 1.163284 0.682128 11.00000 0.10051 AFIX 137 H9A 2 0.689216 1.092713 0.640401 11.00000 -1.50000 H9B 2 0.767039 1.218474 0.694021 11.00000 -1.50000 H9C 2 0.627052 1.202820 0.668734 11.00000 -1.50000 AFIX 0 C10 1 0.476690 0.949558 0.841140 11.00000 0.08930 C11 1 0.592157 1.006212 0.907413 11.00000 0.08247 AFIX 137 H11A 2 0.616198 0.942226 0.923027 11.00000 -1.50000 H11B 2 0.570659 1.063550 0.949650 11.00000 -1.50000 H11C 2 0.658671 1.046745 0.889198 11.00000 -1.50000 AFIX 0 C12 1 0.410130 0.826132 0.853653 11.00000 0.09967 AFIX 137 H12A 2 0.334347 0.836078 0.871342 11.00000 -1.50000 H12B 2 0.461713 0.807837 0.890441 11.00000 -1.50000 H12C 2 0.394513 0.760649 0.806661 11.00000 -1.50000 AFIX 0 C13 1 0.385426 1.040003 0.861660 11.00000 0.14665 AFIX 33 H13A 2 0.367819 1.048167 0.911842 11.00000 -1.50000 H13B 2 0.422955 1.118321 0.859175 11.00000 -1.50000 H13C 2 0.310982 1.007554 0.826222 11.00000 -1.50000 AFIX 0 C14 1 0.419182 0.699181 0.564296 11.00000 0.09575 C15 1 0.517142 0.637138 0.519046 11.00000 0.08676 AFIX 33 H15A 2 0.475620 0.574851 0.473249 11.00000 -1.50000 H15B 2 0.573305 0.697704 0.506904 11.00000 -1.50000 H15C 2 0.561046 0.601780 0.549941 11.00000 -1.50000 AFIX 0 C16 1 0.345300 0.743340 0.503857 11.00000 0.08216 AFIX 137 H16A 2 0.299373 0.799440 0.529510 11.00000 -1.50000 H16B 2 0.290639 0.674208 0.467266 11.00000 -1.50000 H16C 2 0.401788 0.782731 0.478717 11.00000 -1.50000 AFIX 0 C17 1 0.323943 0.586581 0.572740 11.00000 0.14810 AFIX 33 H17A 2 0.294027 0.527154 0.523795 11.00000 -1.50000 H17B 2 0.363966 0.550396 0.604831 11.00000 -1.50000 H17C 2 0.256901 0.614880 0.594640 11.00000 -1.50000 AFIX 56 C21 1 0.861067 0.797502 0.631070 11.00000 0.11083 C20 1 0.918771 0.873966 0.704548 11.00000 0.07976 AFIX 43 H20 2 0.964372 0.953141 0.716863 11.00000 -1.20000 AFIX 55 C19 1 0.894624 0.808313 0.755920 11.00000 0.09080 C18 1 0.821996 0.691274 0.714191 11.00000 0.10380 C22 1 0.801257 0.684593 0.637030 11.00000 0.08777 AFIX 43 H22 2 0.756382 0.617966 0.597363 11.00000 -1.20000 AFIX 0 C23 1 0.744876 0.598851 0.745722 11.00000 0.03713 C24 1 0.651251 0.660773 0.784462 11.00000 0.08715 AFIX 137 H24A 2 0.690830 0.740738 0.817553 11.00000 -1.50000 H24B 2 0.612664 0.613909 0.813337 11.00000 -1.50000 H24C 2 0.590852 0.666965 0.747079 11.00000 -1.50000 AFIX 0 C25 1 0.830760 0.572852 0.802642 11.00000 0.07730 AFIX 137 H25A 2 0.911623 0.584317 0.789967 11.00000 -1.50000 H25B 2 0.803945 0.490389 0.801843 11.00000 -1.50000 H25C 2 0.831258 0.627337 0.852265 11.00000 -1.50000 AFIX 0 C26 1 0.693214 0.484320 0.679580 11.00000 0.07834 AFIX 137 H26A 2 0.649938 0.504181 0.640029 11.00000 -1.50000 H26B 2 0.638330 0.427850 0.695684 11.00000 -1.50000 H26C 2 0.758578 0.448222 0.661038 11.00000 -1.50000 AFIX 0 C27 1 0.960953 0.864778 0.829091 11.00000 0.06067 C28 1 0.896069 0.885506 0.909532 11.00000 0.08415 AFIX 137 H28A 2 0.864967 0.958187 0.919607 11.00000 -1.50000 H28B 2 0.956341 0.893012 0.951287 11.00000 -1.50000 H28C 2 0.830457 0.816961 0.902884 11.00000 -1.50000 AFIX 0 C29 1 1.043231 1.011284 0.862001 11.00000 0.09147 AFIX 137 H29A 2 1.095003 1.025663 0.826299 11.00000 -1.50000 H29B 2 1.092432 1.024944 0.909630 11.00000 -1.50000 H29C 2 0.988605 1.065771 0.868613 11.00000 -1.50000 AFIX 0 C30 1 1.076237 0.815719 0.867258 11.00000 0.17179 AFIX 33 H30A 2 1.107152 0.869245 0.917815 11.00000 -1.50000 H30B 2 1.046120 0.734845 0.868400 11.00000 -1.50000 H30C 2 1.140530 0.815368 0.837110 11.00000 -1.50000 AFIX 0 C31 1 0.884233 0.829516 0.565100 11.00000 0.06598 C32 1 0.814944 0.929181 0.552571 11.00000 0.11373 AFIX 33 H32A 2 0.834119 0.946714 0.507593 11.00000 -1.50000 H32B 2 0.728530 0.898996 0.547286 11.00000 -1.50000 H32C 2 0.840269 1.002118 0.595257 11.00000 -1.50000 AFIX 0 C33 1 0.845989 0.717584 0.489396 11.00000 0.12364 AFIX 33 H33A 2 0.863653 0.744600 0.447235 11.00000 -1.50000 H33B 2 0.890955 0.657009 0.492121 11.00000 -1.50000 H33C 2 0.760186 0.683321 0.482961 11.00000 -1.50000 AFIX 0 C34 1 1.024246 0.884792 0.567022 11.00000 0.10232 AFIX 137 H34A 2 1.058336 0.940219 0.616648 11.00000 -1.50000 H34B 2 1.031821 0.927370 0.530704 11.00000 -1.50000 H34C 2 1.067231 0.820209 0.554877 11.00000 -1.50000 AFIX 0 F1 5 0.775567 0.386486 0.256699 11.00000 0.08355 F2 5 0.935461 0.360538 0.371736 11.00000 0.08125 F3 5 1.109710 0.541670 0.453259 11.00000 0.11582 F4 5 1.158081 0.763345 0.433676 11.00000 0.14454 F5 5 1.004585 0.792284 0.316531 11.00000 0.07784 F6 5 0.843349 0.904709 0.260331 11.00000 0.09257 F7 5 0.733390 1.051286 0.359297 11.00000 0.09138 F8 5 0.580749 0.962889 0.441037 11.00000 0.09338 F9 5 0.523374 0.721583 0.411593 11.00000 0.10459 F10 5 0.621106 0.576362 0.316302 11.00000 0.08743 F11 5 1.054052 0.615649 0.191257 11.00000 0.12311 F12 5 1.124221 0.615239 0.065154 11.00000 0.10311 F13 5 0.991483 0.688947 -0.020056 11.00000 0.18429 F14 5 0.776506 0.754884 0.002578 11.00000 0.09581 F15 5 0.697462 0.743384 0.119761 11.00000 0.09803 F16 5 0.520075 0.597221 0.172091 11.00000 0.09568 F17 5 0.396370 0.444695 0.054093 11.00000 0.14345 F18 5 0.504293 0.283287 -0.017614 11.00000 0.15273 F19 5 0.726758 0.254655 0.006198 11.00000 0.10471 F20 5 0.858253 0.420775 0.119942 11.00000 0.10183 AFIX 66 C35 1 0.883422 0.592973 0.288033 11.00000 0.08423 C40 1 0.979355 0.687411 0.331412 11.00000 0.10885 C39 1 1.057899 0.669594 0.386691 11.00000 0.07288 C38 1 1.040511 0.557340 0.398591 11.00000 0.08399 C37 1 0.944579 0.462901 0.355212 11.00000 0.09718 C36 1 0.866034 0.480716 0.299933 11.00000 0.09806 AFIX 66 C41 1 0.736621 0.737485 0.288154 11.00000 0.06743 C42 1 0.764364 0.862162 0.300553 11.00000 0.07175 C43 1 0.708519 0.937992 0.351869 11.00000 0.08498 C44 1 0.624931 0.889146 0.390787 11.00000 0.07956 C45 1 0.597188 0.764469 0.378388 11.00000 0.10113 C46 1 0.653032 0.688637 0.327072 11.00000 0.09795 AFIX 66 C47 1 0.872695 0.672187 0.154840 11.00000 0.07746 C48 1 0.983937 0.642650 0.141055 11.00000 0.14644 C49 1 1.028955 0.650792 0.075773 11.00000 0.07552 C50 1 0.962733 0.688473 0.024277 11.00000 0.10786 C51 1 0.851491 0.718010 0.038061 11.00000 0.13532 C52 1 0.806471 0.709868 0.103342 11.00000 0.09543 AFIX 66 C53 1 0.704028 0.514014 0.151479 11.00000 0.09850 C58 1 0.750799 0.422250 0.105621 11.00000 0.10380 C57 1 0.677047 0.336454 0.041958 11.00000 0.08048 C56 1 0.556524 0.342422 0.024152 11.00000 0.15245 C55 1 0.509751 0.434186 0.070009 11.00000 0.06326 C54 1 0.583502 0.519982 0.133673 11.00000 0.10176 AFIX 0 B1 3 0.801744 0.640326 0.236124 11.00000 0.15952 HKLF 4 REM dy60_hp8_38deg_a.res in P-1 REM wR2 = 0.3967, GooF = S = 1.188, Restrained GooF = 1.174 for all data REM R1 = 0.1524 for 886 Fo > 4sig(Fo) and 0.2501 for all 1834 data REM 271 parameters refined using 89 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.568, deepest hole -1.037, 1-sigma level 0.125 Q1 1 0.7369 0.7067 0.6554 11.00000 0.05 0.57 Q2 1 0.8404 0.4430 0.7484 11.00000 0.05 0.56 Q3 1 0.7551 1.0406 0.7567 11.00000 0.05 0.52 Q4 1 0.8557 0.7457 0.7960 11.00000 0.05 0.51 Q5 1 0.7476 1.0403 0.7393 11.00000 0.05 0.51 Q6 1 0.7736 0.8049 0.7399 11.00000 0.05 0.50 Q7 1 0.6359 0.9819 0.7788 11.00000 0.05 0.46 Q8 1 0.5538 0.7207 0.7223 11.00000 0.05 0.46 Q9 1 1.1743 0.7819 0.8349 11.00000 0.05 0.43 Q10 1 0.6204 0.9600 0.7441 11.00000 0.05 0.43 Q11 1 0.8194 0.9632 0.7221 11.00000 0.05 0.42 Q12 1 0.8192 0.9780 0.7395 11.00000 0.05 0.41 Q13 1 0.9412 0.8308 0.3208 11.00000 0.05 0.41 Q14 1 0.6226 1.2007 0.6310 11.00000 0.05 0.41 Q15 1 0.6269 0.6442 0.6721 11.00000 0.05 0.40 Q16 1 1.0130 0.7200 0.5873 11.00000 0.05 0.40 Q17 1 0.9289 0.8225 0.2973 11.00000 0.05 0.40 Q18 1 0.3964 0.9766 0.8223 11.00000 0.05 0.40 Q19 1 0.6090 1.1838 0.5970 11.00000 0.05 0.39 Q20 1 0.6784 1.0988 0.3841 11.00000 0.05 0.38 ; _shelx_res_checksum 16214 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.630 _oxdiff_exptl_absorpt_empirical_full_min 0.642 # start Validation Reply Form _vrf_THETM01_dy60_hp8_38deg ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_RINTA01_dy60_hp8_38deg ; PROBLEM: The value of Rint is greater than 0.18 RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT029_dy60_hp7 ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.379 Why? RESPONSE: Due to the shape of the diamond anvil cell, it is impossible to cover the full reciprocal space in this crystal system. The completeness depends both on crystal system and on the exact orientation of the crystal within the cell. ; _vrf_PLAT201_dy60_hp7 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 45 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT412_dy60_hp7 ; PROBLEM: Short Intra XH3 .. XHn H3 ..H12C . 1.43 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT020_dy60_hp7 ; PROBLEM: The Value of Rint is Greater Than 0.12 ......... 0.242 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT084_dy60_hp7 ; PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.40 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT088_dy60_hp7 ; PROBLEM: Poor Data / Parameter Ratio .................... 6.77 Note RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT241_dy60_hp7 ; PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of C48 Check RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT242_dy60_hp7 ; PROBLEM: Low 'MainMol' Ueq as Compared to Neighbors of C47 Check RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT342_dy60_hp7 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.06655 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT413_dy60_hp7 ; PROBLEM: Short Inter XH3 .. XHn H15A ..H15C . 1.95 Ang. RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; _vrf_PLAT911_dy60_hp7 ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.500 1818 Report RESPONSE: : A SC-XRD DAC-experiment carries with it several problems that makes the final model lower quality than if coming from an ambient pressure structure determination. These include a) that the experiment is carried out at room-temperature, b) parasiting scattering from both the gasket and the diamonds, c) variable intensity on the crystal due to the strong diamond reflections and d) that not all reciprocal lattice points can be accessed due to the restrictions of the cell. ; # end Validation Reply Form _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive