#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:45:26 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294466 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572105.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1572105 loop_ _publ_author_name 'Jenek, Niko A.' 'Helbig, Andreas' 'Boyt, Stuart M.' 'Kaur, Mandeep' 'Sanderson, Hugh J.' 'Reeksting, Shaun B.' 'Kociok-Köhn, Gabriele' 'Helten, Holger' 'Hintermair, Ulrich' _publ_section_title ; Understanding and tuning the electronic structure of pentalenides. ; _journal_issue 32 _journal_name_full 'Chemical science' _journal_page_first 12765 _journal_page_last 12779 _journal_paper_doi 10.1039/d3sc04622b _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C30 H26' _chemical_formula_sum 'C30 H26' _chemical_formula_weight 386.51 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-07-12 deposited with the CCDC. 2024-07-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.168(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 24.0658(4) _cell_length_b 5.97950(10) _cell_length_c 30.3634(4) _cell_measurement_reflns_used 13181 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 72.7950 _cell_measurement_theta_min 5.7050 _cell_volume 4127.10(12) _computing_cell_refinement 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)' _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _computing_structure_refinement ; SHELXL-2018/3 (Sheldrick, 2018) Sheldrick GM (2008) Acta Crystallogr A64:112--122 and C. B. H\"ubschle, G. M. Sheldrick and B. Dittrich ShelXle: a Qt graphical user interface for SHELXL J. Appl. Cryst., 44, (2011) 1281-1284. ; _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.1150 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, EosS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_unetI/netI 0.0221 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 40218 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.028 _diffrn_reflns_theta_min 3.889 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.244 _exptl_crystal_description plate _exptl_crystal_F_000 1648 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.212 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.038 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 4115 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0414 _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^)+(0.0343P)^2^+3.4585P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0911 _refine_ls_wR_factor_ref 0.0946 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3639 _reflns_number_total 4115 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3sc04622b2.cif _cod_data_source_block s22uh17 _cod_depositor_comments 'Adding full bibliography for 1572104--1572108.cif.' _cod_original_sg_symbol_H-M 'I 2/a' _cod_database_code 1572105 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.817 _shelx_estimated_absorpt_t_max 0.974 _oxdiff_exptl_absorpt_empirical_full_min 0.697 _oxdiff_exptl_absorpt_empirical_full_max 1.386 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; TITL shelxt_a.res in I2/a s22uh17.res created by SHELXL-2018/3 at 10:18:21 on 02-Sep-2022 CELL 1.54184 24.0658 5.9795 30.3634 90.000 109.168 90.000 ZERR 8.00 0.0004 0.0001 0.0004 0.000 0.002 0.000 LATT 2 SYMM 1/2 - X, Y, - Z SFAC C H UNIT 240 208 ACTA FMAP 2 PLAN 5 BOND $H CONF LIST 4 L.S. 10 TEMP -123.00 SIZE 0.4 0.12 0.05 WGHT 0.034300 3.458500 FVAR 2.25731 C1 1 0.742183 0.548616 0.381469 11.00000 0.01836 0.01561 = 0.01925 -0.00157 0.00461 -0.00003 C2 1 0.772952 0.617549 0.353776 11.00000 0.01959 0.01612 = 0.02055 -0.00158 0.00567 -0.00169 C3 1 0.831607 0.552430 0.350818 11.00000 0.02226 0.02350 = 0.02787 0.00086 0.01214 0.00116 AFIX 23 H3A 2 0.826576 0.482553 0.320191 11.00000 -1.20000 H3B 2 0.850665 0.442282 0.375501 11.00000 -1.20000 AFIX 0 C4 1 0.870225 0.761464 0.356893 11.00000 0.02020 0.02902 = 0.02898 -0.00297 0.01045 -0.00372 AFIX 23 H4A 2 0.877893 0.823490 0.388569 11.00000 -1.20000 H4B 2 0.908475 0.720730 0.353479 11.00000 -1.20000 AFIX 0 C5 1 0.839918 0.937818 0.320614 11.00000 0.02601 0.02484 = 0.02882 -0.00076 0.01366 -0.00670 AFIX 23 H5A 2 0.834223 0.878089 0.289023 11.00000 -1.20000 H5B 2 0.865374 1.071734 0.325139 11.00000 -1.20000 AFIX 0 C6 1 0.780380 1.004534 0.324344 11.00000 0.02630 0.01973 = 0.02915 0.00319 0.01271 -0.00205 AFIX 23 H6A 2 0.760636 1.109935 0.298865 11.00000 -1.20000 H6B 2 0.786582 1.082523 0.354342 11.00000 -1.20000 AFIX 0 C7 1 0.740618 0.801267 0.321428 11.00000 0.01957 0.02010 = 0.01978 -0.00055 0.00682 -0.00145 AFIX 13 H7 2 0.727966 0.742868 0.288764 11.00000 -1.20000 AFIX 0 C8 1 0.684171 0.850082 0.334884 11.00000 0.01981 0.01619 = 0.01935 0.00093 0.00673 -0.00037 AFIX 13 H8 2 0.690065 0.996504 0.351707 11.00000 -1.20000 AFIX 0 C9 1 0.629932 0.870408 0.292018 11.00000 0.01928 0.02040 = 0.01908 0.00253 0.00927 0.00363 C10 1 0.620553 1.070218 0.266869 11.00000 0.02614 0.02244 = 0.03063 0.00632 0.01099 0.00183 AFIX 43 H10 2 0.646492 1.192761 0.278028 11.00000 -1.20000 AFIX 0 C11 1 0.573673 1.091352 0.225717 11.00000 0.03057 0.03306 = 0.02851 0.01400 0.01199 0.01084 AFIX 43 H11 2 0.567936 1.227588 0.208710 11.00000 -1.20000 AFIX 0 C12 1 0.535308 0.915242 0.209362 11.00000 0.02384 0.04547 = 0.01909 0.00492 0.00615 0.01028 AFIX 43 H12 2 0.503291 0.930069 0.181134 11.00000 -1.20000 AFIX 0 C13 1 0.543649 0.717392 0.234196 11.00000 0.02454 0.03523 = 0.02097 -0.00341 0.00779 -0.00013 AFIX 43 H13 2 0.517170 0.596307 0.223140 11.00000 -1.20000 AFIX 0 C14 1 0.590882 0.695206 0.275467 11.00000 0.02419 0.02181 = 0.02208 0.00226 0.00876 0.00204 AFIX 43 H14 2 0.596359 0.558802 0.292401 11.00000 -1.20000 AFIX 0 C15 1 0.686253 0.668256 0.369771 11.00000 0.01798 0.01656 = 0.01722 -0.00034 0.00407 0.00078 C16 1 0.654633 0.582722 0.395936 11.00000 0.01931 0.01753 = 0.01617 -0.00078 0.00457 -0.00024 C17 1 0.596443 0.648406 0.397657 11.00000 0.01781 0.02095 = 0.01416 -0.00184 0.00379 -0.00040 C18 1 0.571420 0.855645 0.380949 11.00000 0.02280 0.02450 = 0.02001 0.00156 0.00821 0.00088 AFIX 43 H18 2 0.592172 0.956927 0.367918 11.00000 -1.20000 AFIX 0 C19 1 0.516688 0.915307 0.383151 11.00000 0.02305 0.02640 = 0.02300 0.00084 0.00505 0.00486 AFIX 43 H19 2 0.500241 1.056403 0.371439 11.00000 -1.20000 AFIX 0 C20 1 0.485802 0.770784 0.402296 11.00000 0.01733 0.03684 = 0.02370 -0.00322 0.00624 0.00190 AFIX 43 H20 2 0.448367 0.812238 0.403815 11.00000 -1.20000 AFIX 0 C21 1 0.510094 0.565365 0.419180 11.00000 0.02108 0.03118 = 0.02317 -0.00173 0.00743 -0.00717 AFIX 43 H21 2 0.489254 0.465624 0.432456 11.00000 -1.20000 AFIX 0 C22 1 0.564694 0.504129 0.416845 11.00000 0.02165 0.02114 = 0.01929 -0.00033 0.00492 -0.00213 AFIX 43 H22 2 0.580740 0.362336 0.428429 11.00000 -1.20000 AFIX 0 C23 1 0.691226 0.406322 0.425259 11.00000 0.02244 0.02026 = 0.01725 0.00220 0.00626 0.00077 AFIX 43 H23 2 0.679602 0.317711 0.446701 11.00000 -1.20000 AFIX 0 C24 1 0.743907 0.385822 0.417832 11.00000 0.02171 0.01652 = 0.01786 0.00031 0.00527 0.00048 C25 1 0.792124 0.235249 0.443261 11.00000 0.02320 0.02033 = 0.01497 -0.00115 0.00612 0.00381 C26 1 0.779519 0.021808 0.456371 11.00000 0.02778 0.02019 = 0.01829 -0.00023 0.00773 0.00161 AFIX 43 H26 2 0.739811 -0.026984 0.447731 11.00000 -1.20000 AFIX 0 C27 1 0.824257 -0.119274 0.481807 11.00000 0.04126 0.02038 = 0.02179 0.00370 0.01132 0.00729 AFIX 43 H27 2 0.814882 -0.262466 0.490963 11.00000 -1.20000 AFIX 0 C28 1 0.882464 -0.053242 0.493970 11.00000 0.03379 0.03148 = 0.02058 0.00380 0.00582 0.01589 AFIX 43 H28 2 0.913036 -0.151379 0.510957 11.00000 -1.20000 AFIX 0 C29 1 0.895767 0.157194 0.481164 11.00000 0.02265 0.03579 = 0.02101 -0.00238 0.00390 0.00619 AFIX 43 H29 2 0.935654 0.203269 0.489335 11.00000 -1.20000 AFIX 0 C30 1 0.851173 0.301145 0.456464 11.00000 0.02417 0.02162 = 0.02132 -0.00081 0.00638 0.00231 AFIX 43 H30 2 0.860825 0.446130 0.448417 11.00000 -1.20000 AFIX 0 HKLF 4 REM shelxt_a.res in I2/a REM wR2 = 0.0946, GooF = S = 1.088, Restrained GooF = 1.088 for all data REM R1 = 0.0414 for 3639 Fo > 4sig(Fo) and 0.0484 for all 4115 data REM 271 parameters refined using 0 restraints END WGHT 0.0343 3.4584 REM Highest difference peak 0.212, deepest hole -0.202, 1-sigma level 0.038 Q1 1 0.6562 0.8525 0.3132 11.00000 0.05 0.21 Q2 1 0.7112 0.8330 0.3261 11.00000 0.05 0.19 Q3 1 0.7213 0.6507 0.3814 11.00000 0.05 0.19 Q4 1 0.6214 0.7552 0.2786 11.00000 0.05 0.19 Q5 1 0.8064 0.5969 0.3606 11.00000 0.05 0.18 ; _shelx_res_checksum 93285 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.74218(5) 0.5486(2) 0.38147(4) 0.0181(3) Uani 1 1 d . . . . . C2 C 0.77295(5) 0.6175(2) 0.35378(4) 0.0190(3) Uani 1 1 d . . . . . C3 C 0.83161(6) 0.5524(2) 0.35082(5) 0.0236(3) Uani 1 1 d . . . . . H3A H 0.826576 0.482553 0.320191 0.028 Uiso 1 1 calc R U . . . H3B H 0.850665 0.442282 0.375501 0.028 Uiso 1 1 calc R U . . . C4 C 0.87022(6) 0.7615(2) 0.35689(5) 0.0255(3) Uani 1 1 d . . . . . H4A H 0.877893 0.823490 0.388569 0.031 Uiso 1 1 calc R U . . . H4B H 0.908475 0.720730 0.353479 0.031 Uiso 1 1 calc R U . . . C5 C 0.83992(6) 0.9378(2) 0.32061(5) 0.0254(3) Uani 1 1 d . . . . . H5A H 0.834223 0.878089 0.289023 0.030 Uiso 1 1 calc R U . . . H5B H 0.865374 1.071734 0.325139 0.030 Uiso 1 1 calc R U . . . C6 C 0.78038(6) 1.0045(2) 0.32434(5) 0.0242(3) Uani 1 1 d . . . . . H6A H 0.760636 1.109935 0.298865 0.029 Uiso 1 1 calc R U . . . H6B H 0.786582 1.082523 0.354342 0.029 Uiso 1 1 calc R U . . . C7 C 0.74062(5) 0.8013(2) 0.32143(4) 0.0197(3) Uani 1 1 d . . . . . H7 H 0.727966 0.742868 0.288764 0.024 Uiso 1 1 calc R U . . . C8 C 0.68417(5) 0.8501(2) 0.33488(4) 0.0184(3) Uani 1 1 d . . . . . H8 H 0.690065 0.996504 0.351707 0.022 Uiso 1 1 calc R U . . . C9 C 0.62993(5) 0.8704(2) 0.29202(4) 0.0189(3) Uani 1 1 d . . . . . C10 C 0.62055(6) 1.0702(2) 0.26687(5) 0.0260(3) Uani 1 1 d . . . . . H10 H 0.646492 1.192761 0.278028 0.031 Uiso 1 1 calc R U . . . C11 C 0.57367(6) 1.0914(3) 0.22572(5) 0.0302(3) Uani 1 1 d . . . . . H11 H 0.567936 1.227588 0.208710 0.036 Uiso 1 1 calc R U . . . C12 C 0.53531(6) 0.9152(3) 0.20936(5) 0.0297(3) Uani 1 1 d . . . . . H12 H 0.503291 0.930069 0.181134 0.036 Uiso 1 1 calc R U . . . C13 C 0.54365(6) 0.7174(3) 0.23420(5) 0.0268(3) Uani 1 1 d . . . . . H13 H 0.517170 0.596307 0.223140 0.032 Uiso 1 1 calc R U . . . C14 C 0.59088(6) 0.6952(2) 0.27547(4) 0.0224(3) Uani 1 1 d . . . . . H14 H 0.596359 0.558802 0.292401 0.027 Uiso 1 1 calc R U . . . C15 C 0.68625(5) 0.6683(2) 0.36977(4) 0.0177(3) Uani 1 1 d . . . . . C16 C 0.65463(5) 0.5827(2) 0.39594(4) 0.0180(3) Uani 1 1 d . . . . . C17 C 0.59644(5) 0.6484(2) 0.39766(4) 0.0180(3) Uani 1 1 d . . . . . C18 C 0.57142(6) 0.8556(2) 0.38095(4) 0.0221(3) Uani 1 1 d . . . . . H18 H 0.592172 0.956927 0.367918 0.027 Uiso 1 1 calc R U . . . C19 C 0.51669(6) 0.9153(2) 0.38315(5) 0.0248(3) Uani 1 1 d . . . . . H19 H 0.500241 1.056403 0.371439 0.030 Uiso 1 1 calc R U . . . C20 C 0.48580(6) 0.7708(3) 0.40230(5) 0.0261(3) Uani 1 1 d . . . . . H20 H 0.448367 0.812238 0.403815 0.031 Uiso 1 1 calc R U . . . C21 C 0.51009(6) 0.5654(3) 0.41918(5) 0.0251(3) Uani 1 1 d . . . . . H21 H 0.489254 0.465624 0.432456 0.030 Uiso 1 1 calc R U . . . C22 C 0.56469(6) 0.5041(2) 0.41684(4) 0.0211(3) Uani 1 1 d . . . . . H22 H 0.580740 0.362336 0.428429 0.025 Uiso 1 1 calc R U . . . C23 C 0.69123(6) 0.4063(2) 0.42526(4) 0.0200(3) Uani 1 1 d . . . . . H23 H 0.679602 0.317711 0.446701 0.024 Uiso 1 1 calc R U . . . C24 C 0.74391(6) 0.3858(2) 0.41783(4) 0.0190(3) Uani 1 1 d . . . . . C25 C 0.79212(6) 0.2352(2) 0.44326(4) 0.0195(3) Uani 1 1 d . . . . . C26 C 0.77952(6) 0.0218(2) 0.45637(4) 0.0220(3) Uani 1 1 d . . . . . H26 H 0.739811 -0.026984 0.447731 0.026 Uiso 1 1 calc R U . . . C27 C 0.82426(7) -0.1193(2) 0.48181(5) 0.0276(3) Uani 1 1 d . . . . . H27 H 0.814882 -0.262466 0.490963 0.033 Uiso 1 1 calc R U . . . C28 C 0.88246(7) -0.0532(3) 0.49397(5) 0.0294(3) Uani 1 1 d . . . . . H28 H 0.913036 -0.151379 0.510957 0.035 Uiso 1 1 calc R U . . . C29 C 0.89577(6) 0.1572(3) 0.48116(5) 0.0273(3) Uani 1 1 d . . . . . H29 H 0.935654 0.203269 0.489335 0.033 Uiso 1 1 calc R U . . . C30 C 0.85117(6) 0.3011(2) 0.45646(4) 0.0226(3) Uani 1 1 d . . . . . H30 H 0.860825 0.446130 0.448417 0.027 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0184(6) 0.0156(6) 0.0193(6) -0.0016(5) 0.0046(5) 0.0000(5) C2 0.0196(6) 0.0161(6) 0.0205(6) -0.0016(5) 0.0057(5) -0.0017(5) C3 0.0223(6) 0.0235(7) 0.0279(7) 0.0009(6) 0.0121(5) 0.0012(6) C4 0.0202(6) 0.0290(8) 0.0290(7) -0.0030(6) 0.0104(5) -0.0037(6) C5 0.0260(7) 0.0248(7) 0.0288(7) -0.0008(6) 0.0137(6) -0.0067(6) C6 0.0263(7) 0.0197(7) 0.0292(7) 0.0032(6) 0.0127(6) -0.0021(6) C7 0.0196(6) 0.0201(7) 0.0198(6) -0.0006(5) 0.0068(5) -0.0014(5) C8 0.0198(6) 0.0162(6) 0.0194(6) 0.0009(5) 0.0067(5) -0.0004(5) C9 0.0193(6) 0.0204(7) 0.0191(6) 0.0025(5) 0.0093(5) 0.0036(5) C10 0.0261(7) 0.0224(7) 0.0306(7) 0.0063(6) 0.0110(6) 0.0018(6) C11 0.0306(7) 0.0331(8) 0.0285(7) 0.0140(6) 0.0120(6) 0.0108(7) C12 0.0238(7) 0.0455(9) 0.0191(6) 0.0049(6) 0.0061(5) 0.0103(7) C13 0.0245(7) 0.0352(8) 0.0210(6) -0.0034(6) 0.0078(5) -0.0001(6) C14 0.0242(6) 0.0218(7) 0.0221(6) 0.0023(5) 0.0088(5) 0.0020(5) C15 0.0180(6) 0.0166(6) 0.0172(6) -0.0003(5) 0.0041(5) 0.0008(5) C16 0.0193(6) 0.0175(6) 0.0162(6) -0.0008(5) 0.0046(5) -0.0002(5) C17 0.0178(6) 0.0210(7) 0.0142(5) -0.0018(5) 0.0038(4) -0.0004(5) C18 0.0228(6) 0.0245(7) 0.0200(6) 0.0016(5) 0.0082(5) 0.0009(6) C19 0.0230(6) 0.0264(7) 0.0230(6) 0.0008(6) 0.0051(5) 0.0049(6) C20 0.0173(6) 0.0368(8) 0.0237(6) -0.0032(6) 0.0062(5) 0.0019(6) C21 0.0211(6) 0.0312(8) 0.0232(6) -0.0017(6) 0.0074(5) -0.0072(6) C22 0.0217(6) 0.0211(7) 0.0193(6) -0.0003(5) 0.0049(5) -0.0021(5) C23 0.0224(6) 0.0203(7) 0.0173(6) 0.0022(5) 0.0063(5) 0.0008(5) C24 0.0217(6) 0.0165(6) 0.0179(6) 0.0003(5) 0.0053(5) 0.0005(5) C25 0.0232(6) 0.0203(6) 0.0150(5) -0.0012(5) 0.0061(5) 0.0038(5) C26 0.0278(7) 0.0202(7) 0.0183(6) -0.0002(5) 0.0077(5) 0.0016(6) C27 0.0413(8) 0.0204(7) 0.0218(6) 0.0037(6) 0.0113(6) 0.0073(6) C28 0.0338(8) 0.0315(8) 0.0206(6) 0.0038(6) 0.0058(6) 0.0159(7) C29 0.0226(7) 0.0358(8) 0.0210(6) -0.0024(6) 0.0039(5) 0.0062(6) C30 0.0242(6) 0.0216(7) 0.0213(6) -0.0008(5) 0.0064(5) 0.0023(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2 C1 C15 110.35(11) . . ? C2 C1 C24 141.78(12) . . ? C15 C1 C24 107.75(11) . . ? C1 C2 C3 132.65(12) . . ? C1 C2 C7 110.83(11) . . ? C3 C2 C7 116.48(11) . . ? C2 C3 C4 109.13(11) . . ? C2 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? C2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C5 C4 C3 110.46(11) . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 111.38(11) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 111.85(11) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C2 C7 C6 111.19(10) . . ? C2 C7 C8 105.76(10) . . ? C6 C7 C8 114.54(11) . . ? C2 C7 H7 108.4 . . ? C6 C7 H7 108.4 . . ? C8 C7 H7 108.4 . . ? C15 C8 C9 118.81(11) . . ? C15 C8 C7 102.53(10) . . ? C9 C8 C7 111.50(10) . . ? C15 C8 H8 107.8 . . ? C9 C8 H8 107.8 . . ? C7 C8 H8 107.8 . . ? C14 C9 C10 118.67(12) . . ? C14 C9 C8 122.73(12) . . ? C10 C9 C8 118.52(12) . . ? C11 C10 C9 120.55(14) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 120.29(13) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 119.77(13) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C14 120.09(14) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C9 C14 C13 120.61(13) . . ? C9 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C1 108.64(11) . . ? C16 C15 C8 141.43(12) . . ? C1 C15 C8 109.84(10) . . ? C15 C16 C23 106.44(11) . . ? C15 C16 C17 129.68(12) . . ? C23 C16 C17 123.86(11) . . ? C18 C17 C22 117.92(12) . . ? C18 C17 C16 121.67(12) . . ? C22 C17 C16 120.40(12) . . ? C19 C18 C17 120.87(13) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 120.55(13) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 119.28(12) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 120.45(13) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 120.92(13) . . ? C21 C22 H22 119.5 . . ? C17 C22 H22 119.5 . . ? C24 C23 C16 111.62(11) . . ? C24 C23 H23 124.2 . . ? C16 C23 H23 124.2 . . ? C23 C24 C1 105.51(11) . . ? C23 C24 C25 125.72(12) . . ? C1 C24 C25 128.72(11) . . ? C26 C25 C30 118.00(12) . . ? C26 C25 C24 120.00(12) . . ? C30 C25 C24 121.96(12) . . ? C27 C26 C25 120.81(13) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 120.54(14) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.43(13) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 120.40(13) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C25 120.80(13) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? 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 C1 C2 1.3543(18) . ? C1 C15 1.4614(17) . ? C1 C24 1.4623(18) . ? C2 C3 1.4952(17) . ? C2 C7 1.5083(18) . ? C3 C4 1.5322(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.526(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.5269(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.5314(18) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.5691(17) . ? C7 H7 1.0000 . ? C8 C15 1.5072(17) . ? C8 C9 1.5156(17) . ? C8 H8 1.0000 . ? C9 C14 1.3868(19) . ? C9 C10 1.3958(19) . ? C10 C11 1.387(2) . ? C10 H10 0.9500 . ? C11 C12 1.381(2) . ? C11 H11 0.9500 . ? C12 C13 1.382(2) . ? C12 H12 0.9500 . ? C13 C14 1.3945(18) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.3671(18) . ? C16 C23 1.4717(17) . ? C16 C17 1.4718(17) . ? C17 C18 1.3982(19) . ? C17 C22 1.3999(18) . ? C18 C19 1.3873(18) . ? C18 H18 0.9500 . ? C19 C20 1.386(2) . ? C19 H19 0.9500 . ? C20 C21 1.384(2) . ? C20 H20 0.9500 . ? C21 C22 1.3881(19) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.3642(18) . ? C23 H23 0.9500 . ? C24 C25 1.4714(17) . ? C25 C26 1.3995(19) . ? C25 C30 1.4005(18) . ? C26 C27 1.3861(19) . ? C26 H26 0.9500 . ? C27 C28 1.384(2) . ? C27 H27 0.9500 . ? C28 C29 1.385(2) . ? C28 H28 0.9500 . ? C29 C30 1.3880(19) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 C1 C2 C3 179.95(13) . . . . ? C24 C1 C2 C3 -4.6(3) . . . . ? C15 C1 C2 C7 2.34(15) . . . . ? C24 C1 C2 C7 177.77(16) . . . . ? C1 C2 C3 C4 -123.67(16) . . . . ? C7 C2 C3 C4 53.84(15) . . . . ? C2 C3 C4 C5 -56.55(14) . . . . ? C3 C4 C5 C6 58.78(15) . . . . ? C4 C5 C6 C7 -54.59(15) . . . . ? C1 C2 C7 C6 127.94(12) . . . . ? C3 C2 C7 C6 -50.10(15) . . . . ? C1 C2 C7 C8 3.04(14) . . . . ? C3 C2 C7 C8 -175.00(11) . . . . ? C5 C6 C7 C2 48.59(15) . . . . ? C5 C6 C7 C8 168.39(11) . . . . ? C2 C7 C8 C15 -6.79(12) . . . . ? C6 C7 C8 C15 -129.58(11) . . . . ? C2 C7 C8 C9 -134.96(11) . . . . ? C6 C7 C8 C9 102.24(13) . . . . ? C15 C8 C9 C14 -20.89(18) . . . . ? C7 C8 C9 C14 97.97(14) . . . . ? C15 C8 C9 C10 162.41(12) . . . . ? C7 C8 C9 C10 -78.72(15) . . . . ? C14 C9 C10 C11 -1.1(2) . . . . ? C8 C9 C10 C11 175.71(12) . . . . ? C9 C10 C11 C12 0.6(2) . . . . ? C10 C11 C12 C13 0.1(2) . . . . ? C11 C12 C13 C14 -0.4(2) . . . . ? C10 C9 C14 C13 0.83(19) . . . . ? C8 C9 C14 C13 -175.86(12) . . . . ? C12 C13 C14 C9 -0.1(2) . . . . ? C2 C1 C15 C16 175.54(11) . . . . ? C24 C1 C15 C16 -1.50(14) . . . . ? C2 C1 C15 C8 -7.11(15) . . . . ? C24 C1 C15 C8 175.85(10) . . . . ? C9 C8 C15 C16 -52.2(2) . . . . ? C7 C8 C15 C16 -175.65(16) . . . . ? C9 C8 C15 C1 131.79(12) . . . . ? C7 C8 C15 C1 8.38(13) . . . . ? C1 C15 C16 C23 0.51(14) . . . . ? C8 C15 C16 C23 -175.49(16) . . . . ? C1 C15 C16 C17 178.76(12) . . . . ? C8 C15 C16 C17 2.8(3) . . . . ? C15 C16 C17 C18 -18.2(2) . . . . ? C23 C16 C17 C18 159.75(12) . . . . ? C15 C16 C17 C22 162.57(13) . . . . ? C23 C16 C17 C22 -19.45(18) . . . . ? C22 C17 C18 C19 -0.34(19) . . . . ? C16 C17 C18 C19 -179.56(12) . . . . ? C17 C18 C19 C20 0.4(2) . . . . ? C18 C19 C20 C21 -0.1(2) . . . . ? C19 C20 C21 C22 -0.2(2) . . . . ? C20 C21 C22 C17 0.3(2) . . . . ? C18 C17 C22 C21 -0.02(19) . . . . ? C16 C17 C22 C21 179.20(12) . . . . ? C15 C16 C23 C24 0.75(15) . . . . ? C17 C16 C23 C24 -177.64(12) . . . . ? C16 C23 C24 C1 -1.64(14) . . . . ? C16 C23 C24 C25 176.19(12) . . . . ? C2 C1 C24 C23 -173.61(17) . . . . ? C15 C1 C24 C23 1.90(14) . . . . ? C2 C1 C24 C25 8.6(3) . . . . ? C15 C1 C24 C25 -175.84(12) . . . . ? C23 C24 C25 C26 37.60(19) . . . . ? C1 C24 C25 C26 -145.08(13) . . . . ? C23 C24 C25 C30 -140.19(14) . . . . ? C1 C24 C25 C30 37.13(19) . . . . ? C30 C25 C26 C27 0.23(18) . . . . ? C24 C25 C26 C27 -177.65(12) . . . . ? C25 C26 C27 C28 -1.3(2) . . . . ? C26 C27 C28 C29 1.1(2) . . . . ? C27 C28 C29 C30 0.2(2) . . . . ? C28 C29 C30 C25 -1.2(2) . . . . ? C26 C25 C30 C29 1.01(19) . . . . ? C24 C25 C30 C29 178.84(12) . . . . ?