#------------------------------------------------------------------------------ #$Date: 2022-01-06 23:47:40 +0200 (Thu, 06 Jan 2022) $ #$Revision: 271863 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061061.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_7061061 loop_ _publ_author_name 'Himeno, Ryoji' 'Ito, Shunichiro' 'Tanaka, Kazuo' 'Chujo, Yoshiki' _publ_section_title ; Synthesis, crystal structure, solid-state optical property and C--H activation of sp3 carbon of highly-stable 1-(2′,6′-dimesitylphenyl)-2,3,4,5-tetraphenylborole ; _journal_issue 48 _journal_name_full 'New Journal of Chemistry' _journal_page_first 22569 _journal_page_last 22573 _journal_paper_doi 10.1039/D1NJ04666G _journal_volume 45 _journal_year 2021 _chemical_formula_sum 'C19.33 H17 B0.33' _chemical_formula_weight 252.93 _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_Hall '-P 2yc' _space_group_name_H-M_alt 'P 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-10-25 deposited with the CCDC. 2021-10-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 105.017(9) _cell_angle_gamma 90 _cell_formula_units_Z 6 _cell_length_a 13.734(6) _cell_length_b 12.910(6) _cell_length_c 12.794(6) _cell_measurement_reflns_used 664 _cell_measurement_temperature 103(2) _cell_measurement_theta_max 25.26 _cell_measurement_theta_min 5.30 _cell_volume 2191.0(17) _computing_cell_refinement 'RAPID AUTO (Rigaku, 2017)' _computing_data_collection 'RAPID AUTO (Rigaku, 2017)' _computing_data_reduction 'RAPID AUTO (Rigaku, 2017)' _computing_molecular_graphics 'ShelXle (J. Appl. Cryst., 44, (2011) 1281-1284.)' _computing_publication_material 'ShelXle (J. Appl. Cryst., 44, (2011) 1281-1284.)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT-2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 103(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Rigaku FR-E & Rapid' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.1519 _diffrn_reflns_av_unetI/netI 0.1598 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 11986 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.345 _diffrn_reflns_theta_min 3.156 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_T_max 0.9995 _exptl_absorpt_correction_T_min 0.1101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.150 _exptl_crystal_description needle _exptl_crystal_F_000 808 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max 0.9995 _exptl_transmission_factor_min 0.1101 _refine_diff_density_max 0.275 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.054 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 3989 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.935 _refine_ls_R_factor_all 0.1622 _refine_ls_R_factor_gt 0.0722 _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^)+(0.0615P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1418 _refine_ls_wR_factor_ref 0.1752 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1898 _reflns_number_total 3989 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj04666g2.cif _cod_data_source_block 7_ben _cod_depositor_comments 'Adding full bibliography for 7061061--7061063.cif.' _cod_original_cell_volume 2190.8(17) _cod_original_sg_symbol_H-M 'P 2/c' _cod_database_code 7061061 _shelx_shelxl_version_number 2014/7 _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_res_file ; ydkr_a.res created by SHELXL-2014/7 TITL ydkr_a.res in P2/c REM Old TITL REM SHELXT solution in P2/c REM R1 0.234, Rweak 0.321, Alpha 0.057, Orientation a'=c, b'=-b, c'=a REM Formula found by SHELXT: C59 CELL 0.71075 13.7336 12.9099 12.7936 90.000 105.017 90.000 ZERR 6.000 0.0061 0.0060 0.0060 0.000 0.009 0.000 LATT 1 SYMM -X, Y, 1/2-Z SFAC C H B UNIT 116 102 2 L.S. 10 BOND $H LIST 4 FMAP 2 PLAN 20 ACTA OMIT 9 0 2 WGHT 0.061500 FVAR 0.61506 C1 1 0.551345 0.854873 0.238144 11.00000 0.02201 0.03145 = 0.03570 0.00237 0.01105 0.00189 B1 3 0.500000 0.680236 0.250000 10.50000 0.02000 0.02997 = 0.03265 0.00000 0.00634 0.00000 C2 1 0.585266 0.756510 0.228556 11.00000 0.02018 0.03547 = 0.03816 -0.00144 0.01177 -0.00132 C3 1 0.605575 0.954153 0.232697 11.00000 0.01368 0.02977 = 0.04060 0.00358 0.00803 -0.00026 C4 1 0.637398 0.981193 0.141052 11.00000 0.02112 0.03559 = 0.04515 -0.00035 0.00750 -0.00353 AFIX 43 H4 2 0.625769 0.936475 0.082116 11.00000 -1.20000 AFIX 0 C5 1 0.686499 1.075038 0.137944 11.00000 0.03891 0.03799 = 0.05065 0.00083 0.02007 -0.00629 AFIX 43 H5 2 0.708697 1.092002 0.077323 11.00000 -1.20000 AFIX 0 C6 1 0.702675 1.143535 0.224321 11.00000 0.02749 0.03143 = 0.05330 0.00511 0.00852 -0.00595 AFIX 43 H6 2 0.734928 1.206416 0.221471 11.00000 -1.20000 AFIX 0 C8 1 0.620577 1.024253 0.318188 11.00000 0.01947 0.03432 = 0.03994 -0.00521 0.00900 -0.00115 AFIX 43 H8 2 0.596999 1.008513 0.378220 11.00000 -1.20000 AFIX 0 C7 1 0.670341 1.117386 0.314821 11.00000 0.02235 0.03259 = 0.04975 -0.00089 0.00881 -0.00083 AFIX 43 H7 2 0.681987 1.162346 0.373558 11.00000 -1.20000 AFIX 0 C9 1 0.683921 0.734918 0.204332 11.00000 0.01844 0.03022 = 0.03558 0.00344 0.00940 -0.00006 C10 1 0.771431 0.785302 0.261054 11.00000 0.01780 0.02818 = 0.04134 -0.00072 0.00966 0.00042 AFIX 43 H10 2 0.768430 0.830258 0.316935 11.00000 -1.20000 AFIX 0 C11 1 0.863143 0.770029 0.236175 11.00000 0.01735 0.03281 = 0.04780 0.00104 0.00802 0.00039 AFIX 43 H11 2 0.920624 0.804615 0.274843 11.00000 -1.20000 AFIX 0 C12 1 0.868164 0.702139 0.152422 11.00000 0.01612 0.04547 = 0.04655 0.00236 0.01378 0.00387 AFIX 43 H12 2 0.929059 0.691836 0.134865 11.00000 -1.20000 AFIX 0 C13 1 0.782102 0.650127 0.095503 11.00000 0.02702 0.04281 = 0.04351 -0.00444 0.01624 0.00084 AFIX 43 H13 2 0.785342 0.605045 0.039805 11.00000 -1.20000 AFIX 0 C14 1 0.690657 0.665685 0.122105 11.00000 0.02352 0.03514 = 0.04105 -0.00406 0.01024 -0.00237 AFIX 43 H14 2 0.633588 0.629645 0.084773 11.00000 -1.20000 AFIX 0 C15 1 0.500000 0.558365 0.250000 10.50000 0.01238 0.02387 = 0.03719 0.00000 0.01002 0.00000 C16 1 0.413043 0.501517 0.189905 11.00000 0.02024 0.03209 = 0.03746 -0.00088 0.01750 -0.00047 C17 1 0.416913 0.392454 0.188307 11.00000 0.02253 0.03066 = 0.04392 -0.00628 0.01329 -0.00448 AFIX 43 H17 2 0.363082 0.355563 0.145345 11.00000 -1.20000 AFIX 0 C18 1 0.500000 0.339291 0.250000 10.50000 0.01921 0.02402 = 0.03955 0.00000 0.00490 0.00000 AFIX 43 H18 2 0.500001 0.267253 0.250000 10.50000 -1.20000 AFIX 0 C19 1 0.318251 0.551851 0.125535 11.00000 0.02433 0.02647 = 0.03234 -0.00289 0.01046 -0.00543 C20 1 0.224574 0.525054 0.146468 11.00000 0.02363 0.02962 = 0.03559 -0.00113 0.01212 -0.00360 C21 1 0.135394 0.569904 0.085588 11.00000 0.01530 0.03348 = 0.04420 -0.00356 0.00640 -0.00134 AFIX 43 H21 2 0.074843 0.551255 0.100190 11.00000 -1.20000 AFIX 0 C22 1 0.133727 0.642025 0.003242 11.00000 0.02189 0.03049 = 0.03766 -0.00271 0.00565 -0.00021 C23 1 0.226863 0.665338 -0.017297 11.00000 0.02722 0.03000 = 0.03653 0.00148 0.01067 -0.00001 AFIX 43 H23 2 0.228193 0.712782 -0.071610 11.00000 -1.20000 AFIX 0 C24 1 0.317387 0.620773 0.039819 11.00000 0.02520 0.02712 = 0.03155 -0.00617 0.01211 -0.00076 C25 1 0.412433 0.646473 0.004898 11.00000 0.02628 0.04332 = 0.04136 0.00161 0.01535 -0.00142 AFIX 137 H25A 2 0.394529 0.665933 -0.070085 11.00000 -1.50000 H25B 2 0.455652 0.586858 0.014973 11.00000 -1.50000 H25C 2 0.447077 0.702841 0.047775 11.00000 -1.50000 AFIX 0 C26 1 0.216232 0.448497 0.234329 11.00000 0.01690 0.03745 = 0.04602 0.00475 0.00560 -0.00169 AFIX 137 H26A 2 0.159106 0.466060 0.260965 11.00000 -1.50000 H26B 2 0.276427 0.451441 0.292625 11.00000 -1.50000 H26C 2 0.207907 0.379739 0.204772 11.00000 -1.50000 AFIX 0 C27 1 0.037441 0.693400 -0.058757 11.00000 0.02885 0.04985 = 0.04882 0.01300 0.00886 0.00437 AFIX 137 H27A 2 0.029994 0.758667 -0.025708 11.00000 -1.50000 H27B 2 -0.018821 0.649612 -0.057810 11.00000 -1.50000 H27C 2 0.039855 0.704627 -0.132221 11.00000 -1.50000 AFIX 0 C28 1 0.932424 1.016931 0.400954 11.00000 0.03355 0.05787 = 0.05006 -0.00515 -0.00307 0.00804 AFIX 43 H28 2 0.887311 1.028473 0.333993 11.00000 -1.20000 AFIX 0 C29 1 0.899878 1.023395 0.494688 11.00000 0.01893 0.07146 = 0.05422 -0.00547 0.00143 0.00433 AFIX 43 H29 2 0.832956 1.038805 0.491174 11.00000 -1.20000 AFIX 0 C30 1 0.967987 1.006688 0.592967 11.00000 0.03412 0.06862 = 0.05100 -0.00950 0.01019 0.00694 AFIX 43 H30 2 0.946791 1.011335 0.656204 11.00000 -1.20000 AFIX 0 HKLF 4 REM ydkr_a.res in P2/c REM R1 = 0.0722 for 1898 Fo > 4sig(Fo) and 0.1622 for all 3989 data REM 271 parameters refined using 0 restraints END WGHT 0.0615 0.0000 REM Highest difference peak 0.275, deepest hole -0.322, 1-sigma level 0.054 Q1 1 0.5722 0.7192 0.2848 11.00000 0.05 0.27 Q2 1 0.7612 0.6188 0.1614 11.00000 0.05 0.27 Q3 1 0.7961 0.8237 0.1906 11.00000 0.05 0.26 Q4 1 0.5229 0.7095 0.1910 11.00000 0.05 0.25 Q5 1 0.7223 0.6985 0.0567 11.00000 0.05 0.22 Q6 1 0.6201 0.8166 0.2809 11.00000 0.05 0.21 Q7 1 0.4189 0.4560 0.1243 11.00000 0.05 0.20 Q8 1 0.4448 0.5173 0.1877 11.00000 0.05 0.19 Q9 1 0.2018 0.7036 0.0369 11.00000 0.05 0.19 Q10 1 0.4004 0.5092 0.2141 11.00000 0.05 0.18 Q11 1 0.6537 0.9989 0.2801 11.00000 0.05 0.18 Q12 1 0.3219 0.7822 -0.0635 11.00000 0.05 0.18 Q13 1 0.3965 0.6561 0.1299 11.00000 0.05 0.18 Q14 1 0.6170 0.7632 0.1849 11.00000 0.05 0.18 Q15 1 0.4958 0.6885 0.0437 11.00000 0.05 0.17 Q16 1 0.3101 0.4788 0.2036 11.00000 0.05 0.17 Q17 1 0.6825 1.2737 0.1927 11.00000 0.05 0.17 Q18 1 0.2864 0.5734 0.1884 11.00000 0.05 0.17 Q19 1 0.5995 0.7689 -0.0033 11.00000 0.05 0.17 Q20 1 0.6605 0.7162 0.2618 11.00000 0.05 0.16 ; _shelx_res_checksum 56558 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, 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 0.5513(3) 0.8549(3) 0.2381(3) 0.0291(9) Uani 1 1 d . . . . . B1 B 0.5000 0.6802(4) 0.2500 0.0276(14) Uani 1 2 d S T P . . C2 C 0.5853(3) 0.7565(3) 0.2286(3) 0.0305(9) Uani 1 1 d . . . . . C3 C 0.6056(3) 0.9542(3) 0.2327(3) 0.0278(9) Uani 1 1 d . . . . . C4 C 0.6374(3) 0.9812(3) 0.1411(3) 0.0342(9) Uani 1 1 d . . . . . H4 H 0.6258 0.9365 0.0821 0.041 Uiso 1 1 calc R U . . . C5 C 0.6865(3) 1.0750(3) 0.1379(3) 0.0409(11) Uani 1 1 d . . . . . H5 H 0.7087 1.0920 0.0773 0.049 Uiso 1 1 calc R U . . . C6 C 0.7027(3) 1.1435(3) 0.2243(3) 0.0378(10) Uani 1 1 d . . . . . H6 H 0.7349 1.2064 0.2215 0.045 Uiso 1 1 calc R U . . . C8 C 0.6206(3) 1.0243(3) 0.3182(3) 0.0310(9) Uani 1 1 d . . . . . H8 H 0.5970 1.0085 0.3782 0.037 Uiso 1 1 calc R U . . . C7 C 0.6703(3) 1.1174(3) 0.3148(3) 0.0350(9) Uani 1 1 d . . . . . H7 H 0.6820 1.1623 0.3736 0.042 Uiso 1 1 calc R U . . . C9 C 0.6839(3) 0.7349(3) 0.2043(3) 0.0276(9) Uani 1 1 d . . . . . C10 C 0.7714(3) 0.7853(3) 0.2611(3) 0.0287(9) Uani 1 1 d . . . . . H10 H 0.7684 0.8303 0.3169 0.034 Uiso 1 1 calc R U . . . C11 C 0.8631(3) 0.7700(3) 0.2362(3) 0.0327(9) Uani 1 1 d . . . . . H11 H 0.9206 0.8046 0.2748 0.039 Uiso 1 1 calc R U . . . C12 C 0.8682(3) 0.7021(3) 0.1524(3) 0.0350(10) Uani 1 1 d . . . . . H12 H 0.9291 0.6918 0.1349 0.042 Uiso 1 1 calc R U . . . C13 C 0.7821(3) 0.6501(3) 0.0955(3) 0.0365(10) Uani 1 1 d . . . . . H13 H 0.7853 0.6050 0.0398 0.044 Uiso 1 1 calc R U . . . C14 C 0.6907(3) 0.6657(3) 0.1221(3) 0.0329(9) Uani 1 1 d . . . . . H14 H 0.6336 0.6296 0.0848 0.039 Uiso 1 1 calc R U . . . C15 C 0.5000 0.5584(4) 0.2500 0.0238(11) Uani 1 2 d S T P . . C16 C 0.4130(3) 0.5015(3) 0.1899(3) 0.0281(9) Uani 1 1 d . . . . . C17 C 0.4169(3) 0.3925(3) 0.1883(3) 0.0315(9) Uani 1 1 d . . . . . H17 H 0.3631 0.3556 0.1453 0.038 Uiso 1 1 calc R U . . . C18 C 0.5000 0.3393(4) 0.2500 0.0281(12) Uani 1 2 d S T P . . H18 H 0.5000 0.2673 0.2500 0.034 Uiso 1 2 calc R U P . . C19 C 0.3183(3) 0.5519(3) 0.1255(3) 0.0271(8) Uani 1 1 d . . . . . C20 C 0.2246(3) 0.5251(3) 0.1465(3) 0.0288(9) Uani 1 1 d . . . . . C21 C 0.1354(3) 0.5699(3) 0.0856(3) 0.0312(9) Uani 1 1 d . . . . . H21 H 0.0748 0.5513 0.1002 0.037 Uiso 1 1 calc R U . . . C22 C 0.1337(3) 0.6420(3) 0.0032(3) 0.0304(9) Uani 1 1 d . . . . . C23 C 0.2269(3) 0.6653(3) -0.0173(3) 0.0308(9) Uani 1 1 d . . . . . H23 H 0.2282 0.7128 -0.0716 0.037 Uiso 1 1 calc R U . . . C24 C 0.3174(3) 0.6208(3) 0.0398(3) 0.0271(9) Uani 1 1 d . . . . . C25 C 0.4124(3) 0.6465(3) 0.0049(3) 0.0358(9) Uani 1 1 d . . . . . H25A H 0.3945 0.6659 -0.0701 0.054 Uiso 1 1 calc R U . . . H25B H 0.4557 0.5869 0.0150 0.054 Uiso 1 1 calc R U . . . H25C H 0.4471 0.7028 0.0478 0.054 Uiso 1 1 calc R U . . . C26 C 0.2162(3) 0.4485(3) 0.2343(3) 0.0339(9) Uani 1 1 d . . . . . H26A H 0.1591 0.4661 0.2610 0.051 Uiso 1 1 calc R U . . . H26B H 0.2764 0.4514 0.2926 0.051 Uiso 1 1 calc R U . . . H26C H 0.2079 0.3797 0.2048 0.051 Uiso 1 1 calc R U . . . C27 C 0.0374(3) 0.6934(3) -0.0588(3) 0.0427(11) Uani 1 1 d . . . . . H27A H 0.0300 0.7587 -0.0257 0.064 Uiso 1 1 calc R U . . . H27B H -0.0188 0.6496 -0.0578 0.064 Uiso 1 1 calc R U . . . H27C H 0.0399 0.7046 -0.1322 0.064 Uiso 1 1 calc R U . . . C28 C 0.9324(3) 1.0169(3) 0.4010(3) 0.0497(11) Uani 1 1 d . . . . . H28 H 0.8873 1.0285 0.3340 0.060 Uiso 1 1 calc R U . . . C29 C 0.8999(3) 1.0234(3) 0.4947(3) 0.0497(11) Uani 1 1 d . . . . . H29 H 0.8330 1.0388 0.4912 0.060 Uiso 1 1 calc R U . . . C30 C 0.9680(3) 1.0067(4) 0.5930(4) 0.0514(12) Uani 1 1 d . . . . . H30 H 0.9468 1.0113 0.6562 0.062 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 0.022(2) 0.031(2) 0.036(2) 0.0024(18) 0.0111(16) 0.0019(16) B1 0.020(3) 0.030(3) 0.033(3) 0.000 0.006(3) 0.000 C2 0.020(2) 0.035(2) 0.038(2) -0.0014(19) 0.0118(18) -0.0013(17) C3 0.0137(19) 0.030(2) 0.041(2) 0.0036(18) 0.0080(17) -0.0003(15) C4 0.021(2) 0.036(2) 0.045(2) -0.0004(19) 0.0075(18) -0.0035(17) C5 0.039(3) 0.038(2) 0.051(3) 0.001(2) 0.020(2) -0.0063(19) C6 0.027(2) 0.031(2) 0.053(3) 0.005(2) 0.009(2) -0.0060(18) C8 0.019(2) 0.034(2) 0.040(2) -0.0052(19) 0.0090(17) -0.0011(16) C7 0.022(2) 0.033(2) 0.050(2) -0.0009(19) 0.009(2) -0.0008(17) C9 0.018(2) 0.030(2) 0.036(2) 0.0034(18) 0.0094(18) -0.0001(16) C10 0.018(2) 0.028(2) 0.041(2) -0.0007(18) 0.0097(18) 0.0004(15) C11 0.017(2) 0.033(2) 0.048(2) 0.0010(19) 0.0080(19) 0.0004(16) C12 0.016(2) 0.045(2) 0.047(2) 0.002(2) 0.0138(19) 0.0039(18) C13 0.027(2) 0.043(2) 0.044(2) -0.004(2) 0.016(2) 0.0008(19) C14 0.024(2) 0.035(2) 0.041(2) -0.0041(19) 0.0102(18) -0.0024(17) C15 0.012(3) 0.024(3) 0.037(3) 0.000 0.010(2) 0.000 C16 0.020(2) 0.032(2) 0.037(2) -0.0009(18) 0.0175(18) -0.0005(16) C17 0.023(2) 0.031(2) 0.044(2) -0.0063(18) 0.0133(19) -0.0045(17) C18 0.019(3) 0.024(3) 0.040(3) 0.000 0.005(2) 0.000 C19 0.024(2) 0.026(2) 0.0323(19) -0.0029(17) 0.0105(17) -0.0054(16) C20 0.024(2) 0.030(2) 0.036(2) -0.0011(18) 0.0121(17) -0.0036(16) C21 0.015(2) 0.033(2) 0.044(2) -0.0036(19) 0.0064(18) -0.0013(17) C22 0.022(2) 0.030(2) 0.038(2) -0.0027(18) 0.0056(18) -0.0002(16) C23 0.027(2) 0.030(2) 0.037(2) 0.0015(18) 0.0107(19) 0.0000(17) C24 0.025(2) 0.027(2) 0.032(2) -0.0062(17) 0.0121(18) -0.0008(16) C25 0.026(2) 0.043(2) 0.041(2) 0.002(2) 0.0153(19) -0.0014(18) C26 0.017(2) 0.037(2) 0.046(2) 0.0048(19) 0.0056(18) -0.0017(17) C27 0.029(2) 0.050(3) 0.049(3) 0.013(2) 0.009(2) 0.0044(19) C28 0.034(3) 0.058(3) 0.050(3) -0.005(2) -0.003(2) 0.008(2) C29 0.019(2) 0.071(3) 0.054(3) -0.005(3) 0.001(2) 0.004(2) C30 0.034(3) 0.069(3) 0.051(3) -0.010(3) 0.010(2) 0.007(2) 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' 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 C3 127.3(3) . . ? C2 C1 C1 111.92(19) . 2_655 ? C3 C1 C1 120.66(17) . 2_655 ? C15 B1 C2 127.8(2) . 2_655 ? C15 B1 C2 127.8(2) . . ? C2 B1 C2 104.4(4) 2_655 . ? C1 C2 C9 122.7(3) . . ? C1 C2 B1 105.8(3) . . ? C9 C2 B1 131.4(3) . . ? C8 C3 C4 118.8(3) . . ? C8 C3 C1 119.7(3) . . ? C4 C3 C1 121.5(3) . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.7(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C7 C6 C5 119.4(3) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C7 C8 C3 120.8(3) . . ? C7 C8 H8 119.6 . . ? C3 C8 H8 119.6 . . ? C6 C7 C8 120.2(4) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C10 C9 C14 118.2(3) . . ? C10 C9 C2 120.8(3) . . ? C14 C9 C2 121.0(3) . . ? C11 C10 C9 121.6(3) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 119.4(4) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C9 120.8(4) . . ? C13 C14 H14 119.6 . . ? C9 C14 H14 119.6 . . ? C16 C15 C16 118.8(4) . 2_655 ? C16 C15 B1 120.6(2) . . ? C16 C15 B1 120.6(2) 2_655 . ? C17 C16 C15 119.1(4) . . ? C17 C16 C19 117.2(3) . . ? C15 C16 C19 123.7(3) . . ? C18 C17 C16 120.9(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C17 120.8(5) 2_655 . ? C17 C18 H18 119.6 2_655 . ? C17 C18 H18 119.6 . . ? C24 C19 C20 118.3(3) . . ? C24 C19 C16 122.2(3) . . ? C20 C19 C16 119.4(3) . . ? C21 C20 C19 120.0(3) . . ? C21 C20 C26 117.3(3) . . ? C19 C20 C26 122.8(3) . . ? C20 C21 C22 122.4(3) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C21 C22 C23 116.4(3) . . ? C21 C22 C27 121.9(3) . . ? C23 C22 C27 121.6(3) . . ? C24 C23 C22 123.1(3) . . ? C24 C23 H23 118.5 . . ? C22 C23 H23 118.5 . . ? C23 C24 C19 119.7(3) . . ? C23 C24 C25 118.2(3) . . ? C19 C24 C25 122.1(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 H26A 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 120.0(4) 3_776 . ? C30 C28 H28 120.0 3_776 . ? C29 C28 H28 120.0 . . ? C30 C29 C28 119.1(4) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C28 120.9(4) . 3_776 ? C29 C30 H30 119.5 . . ? C28 C30 H30 119.5 3_776 . ? 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 1.369(5) . ? C1 C3 1.493(4) . ? C1 C1 1.517(6) 2_655 ? B1 C15 1.573(7) . ? B1 C2 1.607(5) 2_655 ? B1 C2 1.607(5) . ? C2 C9 1.492(5) . ? C3 C8 1.393(5) . ? C3 C4 1.398(4) . ? C4 C5 1.392(5) . ? C4 H4 0.9300 . ? C5 C6 1.388(5) . ? C5 H5 0.9300 . ? C6 C7 1.385(5) . ? C6 H6 0.9300 . ? C8 C7 1.389(5) . ? C8 H8 0.9300 . ? C7 H7 0.9300 . ? C9 C10 1.394(5) . ? C9 C14 1.402(5) . ? C10 C11 1.391(4) . ? C10 H10 0.9300 . ? C11 C12 1.400(5) . ? C11 H11 0.9300 . ? C12 C13 1.390(5) . ? C12 H12 0.9300 . ? C13 C14 1.398(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.442(4) . ? C15 C16 1.442(4) 2_655 ? C16 C17 1.409(5) . ? C16 C19 1.497(5) . ? C17 C18 1.389(4) . ? C17 H17 0.9300 . ? C18 C17 1.389(4) 2_655 ? C18 H18 0.9300 . ? C19 C24 1.410(5) . ? C19 C20 1.423(4) . ? C20 C21 1.396(5) . ? C20 C26 1.523(5) . ? C21 C22 1.402(5) . ? C21 H21 0.9300 . ? C22 C23 1.404(5) . ? C22 C27 1.508(5) . ? C23 C24 1.393(5) . ? C23 H23 0.9300 . ? C24 C25 1.522(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C30 1.384(6) 3_776 ? C28 C29 1.387(5) . ? C28 H28 0.9300 . ? C29 C30 1.376(6) . ? C29 H29 0.9300 . ? C30 C28 1.384(6) 3_776 ? C30 H30 0.9300 . ?