#------------------------------------------------------------------------------ #$Date: 2022-01-06 23:47:40 +0200 (Thu, 06 Jan 2022) $ #$Revision: 271863 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061063.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_7061063 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_moiety 'C52 H45 B, 0.5(C6 H14)' _chemical_formula_sum 'C55 H52 B' _chemical_formula_weight 723.78 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-10-25 deposited with the CCDC. 2021-10-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.690(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.8870(5) _cell_length_b 11.6042(5) _cell_length_c 32.5768(14) _cell_measurement_reflns_used 26955 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 1.75 _cell_volume 4111.1(3) _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-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 93(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Rigaku Raxis Rapid' _diffrn_measurement_method 'oscillation method' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_unetI/netI 0.0499 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 36369 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.480 _diffrn_reflns_theta_min 2.567 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_T_max 0.7379 _exptl_absorpt_correction_T_min 0.5470 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSCOR, (Rigaku, 1995)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.169 _exptl_crystal_description block _exptl_crystal_F_000 1548 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.220 _refine_diff_density_max 0.333 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.045 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 511 _refine_ls_number_reflns 9366 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0533 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+1.4564P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1143 _refine_ls_wR_factor_ref 0.1270 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6702 _reflns_number_total 9366 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj04666g2.cif _cod_data_source_block ydkr _cod_depositor_comments 'Adding full bibliography for 7061061--7061063.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7061063 _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_res_file ; TITL ydkr_a.res in P2(1)/c ydkr.res created by SHELXL-2018/3 at 09:48:11 on 20-Oct-2021 REM Old TITL REM SHELXT solution in P2(1)/c: R1 0.161, Rweak 0.096, Alpha 0.032 REM 0.618 for 439 systematic absences, Orientation as input REM Formula found by SHELXT: C56 CELL 0.71075 10.8870 11.6042 32.5768 90.000 92.690 90.000 ZERR 4.000 0.0005 0.0005 0.0014 0.000 0.007 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H B UNIT 220 208 4 L.S. 10 BOND TEMP -180 LIST 4 ACTA OMIT -1 0 2 OMIT 1 0 0 OMIT 0 1 1 FMAP 2 PLAN 20 WGHT 0.054200 1.456400 FVAR 0.35023 C1 1 0.223737 0.364924 0.340337 11.00000 0.02244 0.01861 = 0.02091 0.00038 0.00353 -0.00030 C4 1 0.241420 0.178446 0.383413 11.00000 0.02047 0.02184 = 0.02436 0.00259 0.00155 0.00050 AFIX 13 H4 2 0.217613 0.195801 0.412038 11.00000 -1.20000 AFIX 0 C5 1 0.171671 0.462729 0.366432 11.00000 0.02031 0.02086 = 0.02176 -0.00173 -0.00191 0.00169 C6 1 0.191571 0.578997 0.357751 11.00000 0.02396 0.02244 = 0.02343 0.00063 -0.00076 0.00195 AFIX 43 H6 2 0.244388 0.599238 0.336499 11.00000 -1.20000 AFIX 0 C7 1 0.135605 0.665339 0.379601 11.00000 0.03044 0.02075 = 0.03325 -0.00134 -0.00431 0.00341 AFIX 43 H7 2 0.149336 0.743798 0.372866 11.00000 -1.20000 AFIX 0 C8 1 0.060117 0.638157 0.411055 11.00000 0.03361 0.02924 = 0.03629 -0.00911 0.00396 0.00719 AFIX 43 H8 2 0.020526 0.697361 0.425632 11.00000 -1.20000 AFIX 0 C9 1 0.042708 0.523275 0.421146 11.00000 0.03569 0.03370 = 0.03103 -0.00464 0.00992 0.00085 AFIX 43 H9 2 -0.007054 0.503826 0.443310 11.00000 -1.20000 AFIX 0 C10 1 0.097335 0.437082 0.399140 11.00000 0.03070 0.02375 = 0.02653 -0.00133 0.00484 -0.00072 AFIX 43 H10 2 0.084201 0.358863 0.406342 11.00000 -1.20000 AFIX 0 C11 1 0.022566 0.300901 0.297848 11.00000 0.02063 0.02484 = 0.02223 0.00297 0.00354 -0.00245 C12 1 -0.034057 0.407829 0.292307 11.00000 0.02410 0.02783 = 0.02877 0.00449 0.00104 -0.00236 AFIX 43 H12 2 -0.011298 0.469829 0.310127 11.00000 -1.20000 AFIX 0 C13 1 -0.123535 0.424859 0.260984 11.00000 0.02688 0.03765 = 0.03945 0.01711 0.00076 -0.00045 AFIX 43 H13 2 -0.162682 0.497719 0.257914 11.00000 -1.20000 AFIX 0 C14 1 -0.155592 0.336041 0.234330 11.00000 0.03191 0.05873 = 0.02871 0.01432 -0.00723 -0.00857 AFIX 43 H14 2 -0.216284 0.347716 0.212820 11.00000 -1.20000 AFIX 0 C2 1 0.120111 0.278597 0.330321 11.00000 0.01915 0.01874 = 0.02205 -0.00228 0.00336 0.00171 C15 1 -0.098871 0.230352 0.239174 11.00000 0.04189 0.04853 = 0.02755 -0.00354 -0.00568 -0.00833 AFIX 43 H15 2 -0.120142 0.169246 0.220778 11.00000 -1.20000 AFIX 0 C16 1 -0.011192 0.212787 0.270657 11.00000 0.03432 0.03187 = 0.02809 -0.00192 -0.00053 -0.00126 AFIX 43 H16 2 0.026606 0.139319 0.273763 11.00000 -1.20000 AFIX 0 C17 1 0.021097 0.103593 0.359916 11.00000 0.02214 0.02192 = 0.02256 0.00170 -0.00133 -0.00162 C18 1 0.029380 -0.014761 0.354940 11.00000 0.02364 0.02184 = 0.05639 0.00022 -0.00231 0.00132 AFIX 43 H18 2 0.104848 -0.048136 0.347499 11.00000 -1.20000 AFIX 0 C19 1 -0.071357 -0.084773 0.360718 11.00000 0.03332 0.02065 = 0.08503 0.00734 -0.00917 -0.00408 AFIX 43 H19 2 -0.064734 -0.165599 0.356747 11.00000 -1.20000 AFIX 0 C20 1 -0.181142 -0.038350 0.372175 11.00000 0.02615 0.03662 = 0.06576 0.01799 -0.00419 -0.01159 AFIX 43 H20 2 -0.249752 -0.086898 0.376272 11.00000 -1.20000 AFIX 0 C21 1 -0.190613 0.078878 0.377635 11.00000 0.02234 0.04202 = 0.03611 0.00357 0.00421 -0.00211 AFIX 43 H21 2 -0.265787 0.111495 0.385711 11.00000 -1.20000 AFIX 0 C22 1 -0.091014 0.148888 0.371381 11.00000 0.02481 0.02534 = 0.02918 -0.00047 0.00371 0.00160 AFIX 43 H22 2 -0.098809 0.229767 0.374949 11.00000 -1.20000 AFIX 0 C23 1 0.303904 0.061790 0.383752 11.00000 0.01898 0.02037 = 0.03936 0.00426 -0.00411 -0.00225 C24 1 0.302193 -0.009752 0.418065 11.00000 0.03445 0.02956 = 0.04430 0.01028 -0.00761 -0.00437 AFIX 43 H24 2 0.262123 0.015542 0.441732 11.00000 -1.20000 AFIX 0 C25 1 0.357719 -0.116816 0.418291 11.00000 0.04230 0.03254 = 0.06364 0.01499 -0.01383 -0.00206 AFIX 43 H25 2 0.354943 -0.164798 0.441858 11.00000 -1.20000 AFIX 0 C26 1 0.416947 -0.153765 0.384382 11.00000 0.03138 0.02360 = 0.10027 0.01206 -0.01100 0.00242 AFIX 43 H26 2 0.456264 -0.226866 0.384708 11.00000 -1.20000 AFIX 0 C27 1 0.419577 -0.084799 0.349679 11.00000 0.03043 0.03248 = 0.08031 -0.00695 0.01007 0.00138 AFIX 43 H27 2 0.460183 -0.110633 0.326192 11.00000 -1.20000 AFIX 0 C28 1 0.362478 0.022339 0.349445 11.00000 0.02826 0.02423 = 0.05225 0.00417 0.00682 -0.00023 AFIX 43 H28 2 0.363493 0.069179 0.325546 11.00000 -1.20000 AFIX 0 C29 1 0.457058 0.311306 0.369574 11.00000 0.02082 0.01694 = 0.02563 0.00087 0.00317 0.00059 C30 1 0.520525 0.310509 0.332545 11.00000 0.02482 0.01931 = 0.02636 0.00174 0.00433 0.00097 C31 1 0.642938 0.345951 0.333144 11.00000 0.02463 0.02500 = 0.03296 0.00218 0.00874 -0.00003 AFIX 43 H31 2 0.685791 0.345360 0.308405 11.00000 -1.20000 AFIX 0 C32 1 0.702797 0.381933 0.369238 11.00000 0.01910 0.02476 = 0.04174 0.00409 0.00377 -0.00223 AFIX 43 H32 2 0.785073 0.409069 0.368918 11.00000 -1.20000 AFIX 0 C33 1 0.643376 0.378593 0.405835 11.00000 0.02430 0.02164 = 0.03280 0.00003 -0.00344 -0.00202 AFIX 43 H33 2 0.685807 0.401260 0.430679 11.00000 -1.20000 AFIX 0 C34 1 0.521573 0.342122 0.406399 11.00000 0.02340 0.01764 = 0.02709 0.00183 0.00159 0.00275 C35 1 0.458359 0.269870 0.293055 11.00000 0.02503 0.02313 = 0.02293 0.00129 0.00810 -0.00220 C36 1 0.347782 0.321099 0.278039 11.00000 0.02683 0.01975 = 0.02264 0.00210 0.00683 -0.00136 C37 1 0.294038 0.286666 0.240510 11.00000 0.03093 0.02485 = 0.02478 0.00294 0.00323 -0.00001 AFIX 43 H37 2 0.220637 0.323355 0.230460 11.00000 -1.20000 AFIX 0 C38 1 0.344770 0.200135 0.217348 11.00000 0.04459 0.02607 = 0.02323 -0.00098 0.00520 -0.00108 C39 1 0.450771 0.146702 0.233271 11.00000 0.04370 0.02566 = 0.02889 -0.00462 0.01074 0.00338 AFIX 43 H39 2 0.485080 0.085648 0.218116 11.00000 -1.20000 AFIX 0 C40 1 0.508848 0.178839 0.270495 11.00000 0.03016 0.02625 = 0.02851 -0.00039 0.01027 0.00022 C41 1 0.287528 0.413673 0.302554 11.00000 0.02421 0.02082 = 0.02219 0.00327 0.00334 0.00002 AFIX 23 H41A 2 0.225819 0.454379 0.284589 11.00000 -1.20000 H41B 2 0.350516 0.470534 0.311978 11.00000 -1.20000 AFIX 0 C42 1 0.286978 0.165707 0.176273 11.00000 0.06730 0.03778 = 0.02855 -0.00716 -0.00433 0.00624 AFIX 137 H42A 2 0.292428 0.230033 0.156951 11.00000 -1.50000 H42B 2 0.200423 0.145880 0.179411 11.00000 -1.50000 H42C 2 0.330466 0.098800 0.165721 11.00000 -1.50000 AFIX 0 C43 1 0.619562 0.111278 0.286583 11.00000 0.03421 0.03382 = 0.04114 -0.00474 0.00823 0.00886 AFIX 137 H43A 2 0.622793 0.037373 0.272116 11.00000 -1.50000 H43B 2 0.613177 0.097383 0.316079 11.00000 -1.50000 H43C 2 0.694526 0.155257 0.281988 11.00000 -1.50000 AFIX 0 C44 1 0.457570 0.333742 0.446106 11.00000 0.01949 0.02369 = 0.02253 -0.00110 -0.00301 -0.00151 C45 1 0.388341 0.425474 0.460687 11.00000 0.02269 0.02467 = 0.02548 -0.00182 -0.00610 -0.00006 C46 1 0.321580 0.408815 0.495699 11.00000 0.02689 0.03384 = 0.02921 -0.00609 -0.00021 0.00505 AFIX 43 H46 2 0.271878 0.469946 0.504968 11.00000 -1.20000 AFIX 0 C47 1 0.325253 0.306430 0.517370 11.00000 0.02688 0.03986 = 0.02551 -0.00040 0.00211 -0.00227 C48 1 0.399463 0.218435 0.503535 11.00000 0.03102 0.02750 = 0.02734 0.00570 -0.00101 -0.00339 AFIX 43 H48 2 0.404647 0.148183 0.518489 11.00000 -1.20000 AFIX 0 C49 1 0.466240 0.230256 0.468486 11.00000 0.02392 0.02416 = 0.02626 0.00019 -0.00257 -0.00095 C50 1 0.389804 0.543325 0.441103 11.00000 0.03365 0.02342 = 0.03338 -0.00131 -0.00547 0.00233 AFIX 137 H50A 2 0.414406 0.536323 0.412656 11.00000 -1.50000 H50B 2 0.448483 0.592793 0.456541 11.00000 -1.50000 H50C 2 0.307474 0.577372 0.441396 11.00000 -1.50000 AFIX 0 C51 1 0.256171 0.291788 0.556027 11.00000 0.04440 0.06040 = 0.03612 0.00319 0.01334 0.00202 AFIX 137 H51A 2 0.208415 0.361608 0.560959 11.00000 -1.50000 H51B 2 0.314689 0.278537 0.579329 11.00000 -1.50000 H51C 2 0.200467 0.225694 0.552941 11.00000 -1.50000 AFIX 0 C52 1 0.551066 0.135282 0.455695 11.00000 0.03239 0.02464 = 0.03684 0.00433 0.00327 0.00445 AFIX 137 H52A 2 0.529027 0.112250 0.427358 11.00000 -1.50000 H52B 2 0.543083 0.068906 0.473977 11.00000 -1.50000 H52C 2 0.636175 0.163014 0.457444 11.00000 -1.50000 AFIX 0 C53 1 0.080807 0.738867 0.516158 11.00000 0.09629 0.04723 = 0.04198 0.00149 -0.00135 0.00751 AFIX 137 H53A 2 -0.000988 0.707488 0.509005 11.00000 -1.50000 H53B 2 0.092702 0.743500 0.546118 11.00000 -1.50000 H53C 2 0.143620 0.688421 0.505211 11.00000 -1.50000 AFIX 0 C54 1 0.091763 0.858227 0.497820 11.00000 0.06374 0.05001 = 0.05032 -0.00158 -0.00287 -0.00148 AFIX 23 H54A 2 0.172995 0.890740 0.506445 11.00000 -1.20000 H54B 2 0.088410 0.851570 0.467491 11.00000 -1.20000 AFIX 0 C55 1 -0.005786 0.939448 0.509998 11.00000 0.06284 0.05147 = 0.04589 -0.00039 -0.00352 0.00545 AFIX 23 H55A 2 -0.001285 0.947928 0.540271 11.00000 -1.20000 H55B 2 -0.087238 0.906512 0.501898 11.00000 -1.20000 AFIX 0 B1 3 0.316343 0.285326 0.367394 11.00000 0.02476 0.02037 = 0.01790 -0.00387 0.00293 0.00015 C3 1 0.124769 0.185019 0.354957 11.00000 0.02125 0.01918 = 0.02188 -0.00209 0.00260 0.00175 HKLF 4 REM ydkr_a.res in P2(1)/c REM wR2 = 0.1270, GooF = S = 1.012, Restrained GooF = 1.012 for all data REM R1 = 0.0533 for 6702 Fo > 4sig(Fo) and 0.0852 for all 9366 data REM 511 parameters refined using 0 restraints END WGHT 0.0542 1.4564 REM Highest difference peak 0.333, deepest hole -0.208, 1-sigma level 0.045 Q1 1 0.0970 0.9634 0.5070 11.00000 0.05 0.33 Q2 1 -0.0163 0.8607 0.5009 11.00000 0.05 0.33 Q3 1 0.2771 0.3348 0.3541 11.00000 0.05 0.30 Q4 1 0.4925 0.3433 0.4274 11.00000 0.05 0.29 Q5 1 0.3018 0.0339 0.3619 11.00000 0.05 0.26 Q6 1 0.3777 0.1628 0.2314 11.00000 0.05 0.24 Q7 1 0.2932 0.3421 0.4981 11.00000 0.05 0.24 Q8 1 -0.0343 0.1209 0.3651 11.00000 0.05 0.23 Q9 1 0.0457 0.0456 0.3676 11.00000 0.05 0.23 Q10 1 0.2775 0.2147 0.5727 11.00000 0.05 0.23 Q11 1 0.2563 0.1074 0.3817 11.00000 0.05 0.23 Q12 1 0.4672 0.2420 0.4932 11.00000 0.05 0.23 Q13 1 0.4194 0.3226 0.2785 11.00000 0.05 0.22 Q14 1 -0.0217 0.2439 0.2918 11.00000 0.05 0.22 Q15 1 0.1290 0.6180 0.3620 11.00000 0.05 0.22 Q16 1 0.2250 0.4179 0.3574 11.00000 0.05 0.22 Q17 1 0.6472 0.4008 0.3811 11.00000 0.05 0.22 Q18 1 0.4164 -0.1404 0.3613 11.00000 0.05 0.21 Q19 1 0.2965 0.2059 0.2354 11.00000 0.05 0.21 Q20 1 0.5092 0.2362 0.2764 11.00000 0.05 0.21 ; _shelx_res_checksum 86809 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.22374(13) 0.36492(13) 0.34034(4) 0.0206(3) Uani 1 1 d . . . . . C4 C 0.24142(13) 0.17845(13) 0.38341(5) 0.0222(3) Uani 1 1 d . . . . . H4 H 0.217613 0.195801 0.412038 0.027 Uiso 1 1 calc R U . . . C5 C 0.17167(14) 0.46273(13) 0.36643(5) 0.0211(3) Uani 1 1 d . . . . . C6 C 0.19157(14) 0.57900(13) 0.35775(5) 0.0233(3) Uani 1 1 d . . . . . H6 H 0.244388 0.599238 0.336499 0.028 Uiso 1 1 calc R U . . . C7 C 0.13561(15) 0.66534(14) 0.37960(5) 0.0283(4) Uani 1 1 d . . . . . H7 H 0.149336 0.743798 0.372866 0.034 Uiso 1 1 calc R U . . . C8 C 0.06012(16) 0.63816(15) 0.41105(5) 0.0330(4) Uani 1 1 d . . . . . H8 H 0.020526 0.697361 0.425632 0.040 Uiso 1 1 calc R U . . . C9 C 0.04271(16) 0.52328(16) 0.42115(5) 0.0332(4) Uani 1 1 d . . . . . H9 H -0.007054 0.503826 0.443310 0.040 Uiso 1 1 calc R U . . . C10 C 0.09733(15) 0.43708(14) 0.39914(5) 0.0269(4) Uani 1 1 d . . . . . H10 H 0.084201 0.358863 0.406342 0.032 Uiso 1 1 calc R U . . . C11 C 0.02257(14) 0.30090(13) 0.29785(5) 0.0225(3) Uani 1 1 d . . . . . C12 C -0.03406(14) 0.40783(15) 0.29231(5) 0.0269(4) Uani 1 1 d . . . . . H12 H -0.011298 0.469829 0.310127 0.032 Uiso 1 1 calc R U . . . C13 C -0.12353(16) 0.42486(17) 0.26098(6) 0.0347(4) Uani 1 1 d . . . . . H13 H -0.162682 0.497719 0.257914 0.042 Uiso 1 1 calc R U . . . C14 C -0.15559(17) 0.33604(19) 0.23433(6) 0.0401(5) Uani 1 1 d . . . . . H14 H -0.216284 0.347716 0.212820 0.048 Uiso 1 1 calc R U . . . C2 C 0.12011(13) 0.27860(13) 0.33032(4) 0.0199(3) Uani 1 1 d . . . . . C15 C -0.09887(17) 0.23035(18) 0.23917(5) 0.0396(4) Uani 1 1 d . . . . . H15 H -0.120142 0.169246 0.220778 0.047 Uiso 1 1 calc R U . . . C16 C -0.01119(16) 0.21279(16) 0.27066(5) 0.0315(4) Uani 1 1 d . . . . . H16 H 0.026606 0.139319 0.273763 0.038 Uiso 1 1 calc R U . . . C17 C 0.02110(14) 0.10359(13) 0.35992(5) 0.0223(3) Uani 1 1 d . . . . . C18 C 0.02938(16) -0.01476(15) 0.35494(6) 0.0341(4) Uani 1 1 d . . . . . H18 H 0.104848 -0.048136 0.347499 0.041 Uiso 1 1 calc R U . . . C19 C -0.07136(17) -0.08477(16) 0.36072(7) 0.0467(5) Uani 1 1 d . . . . . H19 H -0.064734 -0.165599 0.356747 0.056 Uiso 1 1 calc R U . . . C20 C -0.18114(17) -0.03835(17) 0.37218(7) 0.0430(5) Uani 1 1 d . . . . . H20 H -0.249752 -0.086898 0.376272 0.052 Uiso 1 1 calc R U . . . C21 C -0.19061(15) 0.07888(17) 0.37763(5) 0.0334(4) Uani 1 1 d . . . . . H21 H -0.265787 0.111495 0.385711 0.040 Uiso 1 1 calc R U . . . C22 C -0.09101(14) 0.14889(15) 0.37138(5) 0.0264(3) Uani 1 1 d . . . . . H22 H -0.098809 0.229767 0.374949 0.032 Uiso 1 1 calc R U . . . C23 C 0.30390(14) 0.06179(14) 0.38375(5) 0.0264(4) Uani 1 1 d . . . . . C24 C 0.30219(17) -0.00975(16) 0.41806(6) 0.0364(4) Uani 1 1 d . . . . . H24 H 0.262123 0.015542 0.441732 0.044 Uiso 1 1 calc R U . . . C25 C 0.35772(19) -0.11682(17) 0.41829(7) 0.0467(5) Uani 1 1 d . . . . . H25 H 0.354943 -0.164798 0.441858 0.056 Uiso 1 1 calc R U . . . C26 C 0.41695(18) -0.15376(17) 0.38438(8) 0.0522(6) Uani 1 1 d . . . . . H26 H 0.456264 -0.226866 0.384708 0.063 Uiso 1 1 calc R U . . . C27 C 0.41958(17) -0.08480(17) 0.34968(8) 0.0475(5) Uani 1 1 d . . . . . H27 H 0.460183 -0.110633 0.326192 0.057 Uiso 1 1 calc R U . . . C28 C 0.36248(16) 0.02234(15) 0.34944(6) 0.0348(4) Uani 1 1 d . . . . . H28 H 0.363493 0.069179 0.325546 0.042 Uiso 1 1 calc R U . . . C29 C 0.45706(14) 0.31131(13) 0.36957(5) 0.0211(3) Uani 1 1 d . . . . . C30 C 0.52052(14) 0.31051(13) 0.33255(5) 0.0234(3) Uani 1 1 d . . . . . C31 C 0.64294(14) 0.34595(14) 0.33314(5) 0.0273(4) Uani 1 1 d . . . . . H31 H 0.685791 0.345360 0.308405 0.033 Uiso 1 1 calc R U . . . C32 C 0.70280(14) 0.38193(14) 0.36924(5) 0.0285(4) Uani 1 1 d . . . . . H32 H 0.785073 0.409069 0.368918 0.034 Uiso 1 1 calc R U . . . C33 C 0.64338(14) 0.37859(14) 0.40584(5) 0.0264(3) Uani 1 1 d . . . . . H33 H 0.685807 0.401260 0.430679 0.032 Uiso 1 1 calc R U . . . C34 C 0.52157(14) 0.34212(13) 0.40640(5) 0.0227(3) Uani 1 1 d . . . . . C35 C 0.45836(14) 0.26987(14) 0.29306(5) 0.0235(3) Uani 1 1 d . . . . . C36 C 0.34778(14) 0.32110(13) 0.27804(5) 0.0229(3) Uani 1 1 d . . . . . C37 C 0.29404(15) 0.28667(14) 0.24051(5) 0.0268(4) Uani 1 1 d . . . . . H37 H 0.220637 0.323355 0.230460 0.032 Uiso 1 1 calc R U . . . C38 C 0.34477(17) 0.20013(15) 0.21735(5) 0.0312(4) Uani 1 1 d . . . . . C39 C 0.45077(17) 0.14670(15) 0.23327(5) 0.0325(4) Uani 1 1 d . . . . . H39 H 0.485080 0.085648 0.218116 0.039 Uiso 1 1 calc R U . . . C40 C 0.50885(15) 0.17884(14) 0.27049(5) 0.0280(4) Uani 1 1 d . . . . . C41 C 0.28753(14) 0.41367(13) 0.30255(5) 0.0223(3) Uani 1 1 d . . . . . H41A H 0.225819 0.454379 0.284589 0.027 Uiso 1 1 calc R U . . . H41B H 0.350516 0.470534 0.311978 0.027 Uiso 1 1 calc R U . . . C42 C 0.2870(2) 0.16571(18) 0.17627(6) 0.0448(5) Uani 1 1 d . . . . . H42A H 0.292428 0.230033 0.156951 0.067 Uiso 1 1 calc R U . . . H42B H 0.200423 0.145880 0.179411 0.067 Uiso 1 1 calc R U . . . H42C H 0.330466 0.098800 0.165721 0.067 Uiso 1 1 calc R U . . . C43 C 0.61956(16) 0.11128(16) 0.28658(6) 0.0362(4) Uani 1 1 d . . . . . H43A H 0.622793 0.037373 0.272116 0.054 Uiso 1 1 calc R U . . . H43B H 0.613177 0.097383 0.316079 0.054 Uiso 1 1 calc R U . . . H43C H 0.694526 0.155257 0.281988 0.054 Uiso 1 1 calc R U . . . C44 C 0.45757(13) 0.33374(14) 0.44611(5) 0.0220(3) Uani 1 1 d . . . . . C45 C 0.38834(14) 0.42547(14) 0.46069(5) 0.0245(3) Uani 1 1 d . . . . . C46 C 0.32158(15) 0.40881(16) 0.49570(5) 0.0300(4) Uani 1 1 d . . . . . H46 H 0.271878 0.469946 0.504968 0.036 Uiso 1 1 calc R U . . . C47 C 0.32525(15) 0.30643(16) 0.51737(5) 0.0307(4) Uani 1 1 d . . . . . C48 C 0.39946(15) 0.21844(15) 0.50353(5) 0.0287(4) Uani 1 1 d . . . . . H48 H 0.404647 0.148183 0.518489 0.034 Uiso 1 1 calc R U . . . C49 C 0.46624(14) 0.23026(14) 0.46849(5) 0.0249(3) Uani 1 1 d . . . . . C50 C 0.38980(16) 0.54333(14) 0.44110(5) 0.0304(4) Uani 1 1 d . . . . . H50A H 0.414406 0.536323 0.412656 0.046 Uiso 1 1 calc R U . . . H50B H 0.448483 0.592793 0.456541 0.046 Uiso 1 1 calc R U . . . H50C H 0.307474 0.577372 0.441396 0.046 Uiso 1 1 calc R U . . . C51 C 0.25617(19) 0.2918(2) 0.55603(6) 0.0466(5) Uani 1 1 d . . . . . H51A H 0.208415 0.361608 0.560959 0.070 Uiso 1 1 calc R U . . . H51B H 0.314689 0.278537 0.579329 0.070 Uiso 1 1 calc R U . . . H51C H 0.200467 0.225694 0.552941 0.070 Uiso 1 1 calc R U . . . C52 C 0.55107(16) 0.13528(15) 0.45570(5) 0.0312(4) Uani 1 1 d . . . . . H52A H 0.529027 0.112250 0.427358 0.047 Uiso 1 1 calc R U . . . H52B H 0.543083 0.068906 0.473977 0.047 Uiso 1 1 calc R U . . . H52C H 0.636175 0.163014 0.457444 0.047 Uiso 1 1 calc R U . . . C53 C 0.0808(3) 0.7389(2) 0.51616(7) 0.0620(7) Uani 1 1 d . . . . . H53A H -0.000988 0.707488 0.509005 0.093 Uiso 1 1 calc R U . . . H53B H 0.092702 0.743500 0.546118 0.093 Uiso 1 1 calc R U . . . H53C H 0.143620 0.688421 0.505211 0.093 Uiso 1 1 calc R U . . . C54 C 0.0918(2) 0.8582(2) 0.49782(7) 0.0549(6) Uani 1 1 d . . . . . H54A H 0.172995 0.890740 0.506445 0.066 Uiso 1 1 calc R U . . . H54B H 0.088410 0.851570 0.467491 0.066 Uiso 1 1 calc R U . . . C55 C -0.0058(2) 0.93945(19) 0.51000(7) 0.0536(6) Uani 1 1 d . . . . . H55A H -0.001285 0.947928 0.540271 0.064 Uiso 1 1 calc R U . . . H55B H -0.087238 0.906512 0.501898 0.064 Uiso 1 1 calc R U . . . B1 B 0.31634(16) 0.28533(15) 0.36739(5) 0.0209(4) Uani 1 1 d . . . . . C3 C 0.12477(13) 0.18502(13) 0.35496(5) 0.0207(3) 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 C1 0.0224(7) 0.0186(8) 0.0209(7) 0.0004(6) 0.0035(6) -0.0003(6) C4 0.0205(7) 0.0218(8) 0.0244(8) 0.0026(6) 0.0015(6) 0.0005(6) C5 0.0203(7) 0.0209(8) 0.0218(7) -0.0017(6) -0.0019(6) 0.0017(6) C6 0.0240(8) 0.0224(8) 0.0234(8) 0.0006(6) -0.0008(6) 0.0020(7) C7 0.0304(8) 0.0207(8) 0.0332(9) -0.0013(7) -0.0043(7) 0.0034(7) C8 0.0336(9) 0.0292(9) 0.0363(10) -0.0091(8) 0.0040(8) 0.0072(8) C9 0.0357(9) 0.0337(10) 0.0310(9) -0.0046(8) 0.0099(8) 0.0008(8) C10 0.0307(8) 0.0238(8) 0.0265(8) -0.0013(7) 0.0048(7) -0.0007(7) C11 0.0206(7) 0.0248(8) 0.0222(8) 0.0030(6) 0.0035(6) -0.0024(6) C12 0.0241(8) 0.0278(9) 0.0288(8) 0.0045(7) 0.0010(7) -0.0024(7) C13 0.0269(8) 0.0376(10) 0.0395(10) 0.0171(8) 0.0008(8) -0.0005(8) C14 0.0319(9) 0.0587(13) 0.0287(9) 0.0143(9) -0.0072(8) -0.0086(9) C2 0.0192(7) 0.0187(7) 0.0220(7) -0.0023(6) 0.0034(6) 0.0017(6) C15 0.0419(10) 0.0485(12) 0.0275(9) -0.0035(8) -0.0057(8) -0.0083(9) C16 0.0343(9) 0.0319(10) 0.0281(9) -0.0019(7) -0.0005(7) -0.0013(8) C17 0.0221(7) 0.0219(8) 0.0226(7) 0.0017(6) -0.0013(6) -0.0016(6) C18 0.0236(8) 0.0218(9) 0.0564(12) 0.0002(8) -0.0023(8) 0.0013(7) C19 0.0333(10) 0.0207(9) 0.0850(16) 0.0073(10) -0.0092(10) -0.0041(8) C20 0.0261(9) 0.0366(11) 0.0658(13) 0.0180(10) -0.0042(9) -0.0116(8) C21 0.0223(8) 0.0420(11) 0.0361(9) 0.0036(8) 0.0042(7) -0.0021(8) C22 0.0248(8) 0.0253(8) 0.0292(8) -0.0005(7) 0.0037(7) 0.0016(7) C23 0.0190(7) 0.0204(8) 0.0394(9) 0.0043(7) -0.0041(7) -0.0023(6) C24 0.0344(9) 0.0296(9) 0.0443(11) 0.0103(8) -0.0076(8) -0.0044(8) C25 0.0423(11) 0.0325(11) 0.0636(14) 0.0150(10) -0.0138(10) -0.0021(9) C26 0.0314(10) 0.0236(10) 0.1003(19) 0.0121(11) -0.0110(11) 0.0024(8) C27 0.0304(10) 0.0325(11) 0.0803(16) -0.0069(10) 0.0101(10) 0.0014(9) C28 0.0283(9) 0.0242(9) 0.0523(11) 0.0042(8) 0.0068(8) -0.0002(7) C29 0.0208(7) 0.0169(7) 0.0256(8) 0.0009(6) 0.0032(6) 0.0006(6) C30 0.0248(8) 0.0193(8) 0.0264(8) 0.0017(6) 0.0043(6) 0.0010(6) C31 0.0246(8) 0.0250(8) 0.0330(9) 0.0022(7) 0.0087(7) 0.0000(7) C32 0.0191(7) 0.0248(9) 0.0417(10) 0.0041(7) 0.0038(7) -0.0022(7) C33 0.0243(8) 0.0216(8) 0.0328(9) 0.0000(7) -0.0034(7) -0.0020(7) C34 0.0234(7) 0.0176(7) 0.0271(8) 0.0018(6) 0.0016(6) 0.0028(6) C35 0.0250(8) 0.0231(8) 0.0229(8) 0.0013(6) 0.0081(6) -0.0022(7) C36 0.0268(8) 0.0197(8) 0.0226(8) 0.0021(6) 0.0068(6) -0.0014(7) C37 0.0309(8) 0.0248(8) 0.0248(8) 0.0029(7) 0.0032(7) 0.0000(7) C38 0.0446(10) 0.0261(9) 0.0232(8) -0.0010(7) 0.0052(7) -0.0011(8) C39 0.0437(10) 0.0257(9) 0.0289(9) -0.0046(7) 0.0107(8) 0.0034(8) C40 0.0302(8) 0.0263(9) 0.0285(9) -0.0004(7) 0.0103(7) 0.0002(7) C41 0.0242(8) 0.0208(8) 0.0222(7) 0.0033(6) 0.0033(6) 0.0000(6) C42 0.0673(14) 0.0378(11) 0.0286(10) -0.0072(8) -0.0043(9) 0.0062(10) C43 0.0342(9) 0.0338(10) 0.0411(10) -0.0047(8) 0.0082(8) 0.0089(8) C44 0.0195(7) 0.0237(8) 0.0225(8) -0.0011(6) -0.0030(6) -0.0015(6) C45 0.0227(7) 0.0247(8) 0.0255(8) -0.0018(7) -0.0061(6) -0.0001(7) C46 0.0269(8) 0.0338(10) 0.0292(9) -0.0061(7) -0.0002(7) 0.0051(7) C47 0.0269(8) 0.0399(10) 0.0255(8) -0.0004(7) 0.0021(7) -0.0023(8) C48 0.0310(9) 0.0275(9) 0.0273(8) 0.0057(7) -0.0010(7) -0.0034(7) C49 0.0239(8) 0.0242(8) 0.0263(8) 0.0002(7) -0.0026(6) -0.0010(7) C50 0.0337(9) 0.0234(9) 0.0334(9) -0.0013(7) -0.0055(7) 0.0023(7) C51 0.0444(11) 0.0604(14) 0.0361(10) 0.0032(10) 0.0133(9) 0.0020(10) C52 0.0324(9) 0.0246(9) 0.0368(9) 0.0043(7) 0.0033(7) 0.0045(7) C53 0.0963(19) 0.0472(13) 0.0420(12) 0.0015(10) -0.0014(12) 0.0075(13) C54 0.0637(14) 0.0500(14) 0.0503(13) -0.0016(10) -0.0029(11) -0.0015(12) C55 0.0628(14) 0.0515(14) 0.0459(12) -0.0004(10) -0.0035(11) 0.0055(12) B1 0.0248(8) 0.0204(9) 0.0179(8) -0.0039(7) 0.0029(7) 0.0001(7) C3 0.0213(7) 0.0192(7) 0.0219(7) -0.0021(6) 0.0026(6) 0.0017(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 C5 108.21(12) . . ? C2 C1 C41 115.01(12) . . ? C5 C1 C41 111.07(12) . . ? C2 C1 B1 100.28(12) . . ? C5 C1 B1 111.07(12) . . ? C41 C1 B1 110.74(12) . . ? C23 C4 C3 113.98(13) . . ? C23 C4 B1 117.61(13) . . ? C3 C4 B1 100.70(12) . . ? C6 C5 C10 117.38(14) . . ? C6 C5 C1 122.32(13) . . ? C10 C5 C1 120.25(13) . . ? C7 C6 C5 121.18(15) . . ? C8 C7 C6 120.49(16) . . ? C7 C8 C9 119.21(16) . . ? C10 C9 C8 120.37(16) . . ? C9 C10 C5 121.29(15) . . ? C16 C11 C12 118.04(15) . . ? C16 C11 C2 118.94(14) . . ? C12 C11 C2 122.98(14) . . ? C13 C12 C11 120.78(16) . . ? C14 C13 C12 120.16(17) . . ? C15 C14 C13 119.53(17) . . ? C3 C2 C11 124.68(14) . . ? C3 C2 C1 113.11(13) . . ? C11 C2 C1 122.15(13) . . ? C14 C15 C16 120.38(18) . . ? C15 C16 C11 121.10(17) . . ? C18 C17 C22 117.83(15) . . ? C18 C17 C3 124.27(14) . . ? C22 C17 C3 117.88(14) . . ? C19 C18 C17 120.60(17) . . ? C20 C19 C18 120.65(18) . . ? C21 C20 C19 119.50(17) . . ? C20 C21 C22 119.96(17) . . ? C21 C22 C17 121.45(16) . . ? C28 C23 C24 118.21(16) . . ? C28 C23 C4 120.75(15) . . ? C24 C23 C4 121.03(16) . . ? C25 C24 C23 121.19(19) . . ? C26 C25 C24 119.9(2) . . ? C25 C26 C27 120.26(19) . . ? C26 C27 C28 119.6(2) . . ? C27 C28 C23 120.81(18) . . ? C34 C29 C30 118.89(14) . . ? C34 C29 B1 122.53(13) . . ? C30 C29 B1 118.48(14) . . ? C31 C30 C29 119.33(15) . . ? C31 C30 C35 119.80(14) . . ? C29 C30 C35 120.86(14) . . ? C32 C31 C30 120.89(15) . . ? C31 C32 C33 120.26(15) . . ? C32 C33 C34 120.26(15) . . ? C33 C34 C29 120.21(14) . . ? C33 C34 C44 120.78(14) . . ? C29 C34 C44 119.00(13) . . ? C36 C35 C40 118.79(15) . . ? C36 C35 C30 120.55(14) . . ? C40 C35 C30 120.66(14) . . ? C37 C36 C35 120.12(14) . . ? C37 C36 C41 119.71(14) . . ? C35 C36 C41 120.17(14) . . ? C38 C37 C36 121.69(16) . . ? C37 C38 C39 117.73(16) . . ? C37 C38 C42 121.02(17) . . ? C39 C38 C42 121.24(16) . . ? C38 C39 C40 122.77(16) . . ? C39 C40 C35 118.79(16) . . ? C39 C40 C43 119.05(15) . . ? C35 C40 C43 122.08(15) . . ? C36 C41 C1 112.55(12) . . ? C45 C44 C49 119.84(14) . . ? C45 C44 C34 121.48(14) . . ? C49 C44 C34 118.67(14) . . ? C46 C45 C44 118.79(15) . . ? C46 C45 C50 119.18(15) . . ? C44 C45 C50 121.93(14) . . ? C47 C46 C45 122.24(16) . . ? C46 C47 C48 117.99(15) . . ? C46 C47 C51 121.37(17) . . ? C48 C47 C51 120.58(17) . . ? C49 C48 C47 121.91(16) . . ? C48 C49 C44 119.06(15) . . ? C48 C49 C52 120.37(15) . . ? C44 C49 C52 120.52(14) . . ? C55 C54 C53 113.8(2) . . ? C54 C55 C55 112.8(2) . 3_576 ? C29 B1 C4 130.95(14) . . ? C29 B1 C1 120.36(13) . . ? C4 B1 C1 108.18(13) . . ? C2 C3 C17 124.64(14) . . ? C2 C3 C4 113.89(13) . . ? C17 C3 C4 120.82(13) . . ? 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 1.532(2) . ? C1 C5 1.542(2) . ? C1 C41 1.548(2) . ? C1 B1 1.601(2) . ? C4 C23 1.515(2) . ? C4 C3 1.539(2) . ? C4 B1 1.586(2) . ? C5 C6 1.397(2) . ? C5 C10 1.400(2) . ? C6 C7 1.387(2) . ? C7 C8 1.380(2) . ? C8 C9 1.388(3) . ? C9 C10 1.381(2) . ? C11 C16 1.391(2) . ? C11 C12 1.393(2) . ? C11 C2 1.486(2) . ? C12 C13 1.391(2) . ? C13 C14 1.382(3) . ? C14 C15 1.379(3) . ? C2 C3 1.350(2) . ? C15 C16 1.383(2) . ? C17 C18 1.386(2) . ? C17 C22 1.396(2) . ? C17 C3 1.487(2) . ? C18 C19 1.385(3) . ? C19 C20 1.378(3) . ? C20 C21 1.376(3) . ? C21 C22 1.378(2) . ? C23 C28 1.390(2) . ? C23 C24 1.393(2) . ? C24 C25 1.382(3) . ? C25 C26 1.374(3) . ? C26 C27 1.386(3) . ? C27 C28 1.390(3) . ? C29 C34 1.408(2) . ? C29 C30 1.418(2) . ? C29 B1 1.560(2) . ? C30 C31 1.394(2) . ? C30 C35 1.501(2) . ? C31 C32 1.382(2) . ? C32 C33 1.383(2) . ? C33 C34 1.393(2) . ? C34 C44 1.501(2) . ? C35 C36 1.409(2) . ? C35 C40 1.413(2) . ? C36 C37 1.389(2) . ? C36 C41 1.507(2) . ? C37 C38 1.386(2) . ? C38 C39 1.389(3) . ? C38 C42 1.506(2) . ? C39 C40 1.392(2) . ? C40 C43 1.511(2) . ? C44 C45 1.400(2) . ? C44 C49 1.406(2) . ? C45 C46 1.394(2) . ? C45 C50 1.509(2) . ? C46 C47 1.382(2) . ? C47 C48 1.390(2) . ? C47 C51 1.506(2) . ? C48 C49 1.389(2) . ? C49 C52 1.509(2) . ? C53 C54 1.515(3) . ? C54 C55 1.488(3) . ? C55 C55 1.557(4) 3_576 ?