#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:12:48 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247627 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/25/1552506.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_1552506 loop_ _publ_author_name 'Su, Xiaojun' 'Baker, J. J.' 'Martin, Caleb D.' _publ_section_title ; Dimeric boroles: effective sources of monomeric boroles for heterocycle synthesis ; _journal_issue 1 _journal_name_full 'Chemical Science' _journal_page_first 126 _journal_paper_doi 10.1039/C9SC04053F _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C28 H27 B O' _chemical_formula_sum 'C28 H27 B O' _chemical_formula_weight 390.30 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method SHELXL-2013 _audit_update_record ; 2019-07-24 deposited with the CCDC. 2019-10-28 downloaded from the CCDC. ; _cell_angle_alpha 70.809(4) _cell_angle_beta 87.538(5) _cell_angle_gamma 79.597(5) _cell_formula_units_Z 2 _cell_length_a 8.7781(9) _cell_length_b 10.9283(11) _cell_length_c 12.3004(12) _cell_measurement_reflns_used 3496 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.47 _cell_measurement_theta_min 2.81 _cell_volume 1095.91(19) _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)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.940 _diffrn_measured_fraction_theta_max 0.940 _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_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_unetI/netI 0.0426 _diffrn_reflns_Laue_measured_fraction_full 0.940 _diffrn_reflns_Laue_measured_fraction_max 0.940 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 8077 _diffrn_reflns_point_group_measured_fraction_full 0.940 _diffrn_reflns_point_group_measured_fraction_max 0.940 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.024 _diffrn_reflns_theta_min 2.814 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.183 _exptl_crystal_description blocklike _exptl_crystal_F_000 416 _exptl_crystal_size_max 0.379 _exptl_crystal_size_mid 0.331 _exptl_crystal_size_min 0.316 _refine_diff_density_max 0.300 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.046 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 275 _refine_ls_number_reflns 3635 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0472 _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^)+(0.0521P)^2^+0.4308P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1116 _refine_ls_wR_factor_ref 0.1213 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2856 _reflns_number_total 3635 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc04053f2.cif _cod_data_source_block 4 _cod_depositor_comments ; The following automatic conversions were performed: '_atom_sites_solution_primary' value 'direct methods' was changed to 'direct'. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas Adding full bibliography for 1552504--1552508.cif. ; _cod_database_code 1552506 _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 0.974 _shelx_estimated_absorpt_t_max 0.979 _shelxl_version_number 2013-4 _shelx_res_file ; TITL 4 in P-1 CELL 0.71073 8.77810 10.92830 12.30040 70.8089 87.5379 79.5970 ZERR 2.00 0.00090 0.00110 0.00120 0.0040 0.0047 0.0047 LATT 1 SFAC C H B O UNIT 56 54 2 2 L.S. 4 ACTA BOND FMAP 2 PLAN 20 SIZE 0.316 0.331 0.379 TEMP -123.140 WGHT 0.052100 0.430800 FVAR 0.26490 MOLE 1 O1 4 0.060956 0.667929 0.173001 11.00000 0.01939 0.02560 = 0.03209 -0.01318 -0.00326 -0.00276 C5 1 0.314527 0.654361 0.247881 11.00000 0.01797 0.02620 = 0.02844 -0.01358 0.00013 -0.00287 B1 3 0.026551 0.544380 0.221397 11.00000 0.01497 0.02780 = 0.03498 -0.01701 0.00627 -0.00155 C3 1 0.233586 0.450613 0.381143 11.00000 0.02610 0.02282 = 0.02978 -0.01199 0.00079 -0.00154 C2 1 0.088919 0.455895 0.343880 11.00000 0.02438 0.02514 = 0.03309 -0.01528 0.00452 -0.00542 C4 1 0.349096 0.525945 0.310500 11.00000 0.02023 0.02757 = 0.02988 -0.01463 -0.00199 -0.00185 C1 1 0.151445 0.723718 0.227425 11.00000 0.01977 0.02415 = 0.02358 -0.00862 0.00030 -0.00695 C10 1 0.088102 0.838066 0.243296 11.00000 0.01846 0.02396 = 0.02278 -0.00556 -0.00052 -0.00464 C7 1 0.291544 0.362621 0.500405 11.00000 0.03612 0.03004 = 0.03518 -0.00768 -0.00381 -0.00406 AFIX 137 H7A 2 0.207302 0.363116 0.555272 11.00000 -1.50000 H7B 2 0.377636 0.395233 0.523432 11.00000 -1.50000 H7C 2 0.327180 0.272597 0.499653 11.00000 -1.50000 AFIX 0 C8 1 0.512446 0.449876 0.316286 11.00000 0.02219 0.03201 = 0.04740 -0.01206 -0.00075 0.00179 AFIX 137 H8A 2 0.568048 0.492035 0.247224 11.00000 -1.50000 H8B 2 0.508778 0.359299 0.320613 11.00000 -1.50000 H8C 2 0.566260 0.449049 0.384767 11.00000 -1.50000 AFIX 0 C9 1 0.435655 0.734552 0.186586 11.00000 0.02060 0.03180 = 0.04103 -0.01204 0.00264 -0.00506 AFIX 137 H9A 2 0.537498 0.692032 0.222643 11.00000 -1.50000 H9B 2 0.409584 0.823342 0.192117 11.00000 -1.50000 H9C 2 0.438150 0.740098 0.105392 11.00000 -1.50000 AFIX 0 C6 1 -0.017932 0.371607 0.422817 11.00000 0.03026 0.03370 = 0.03483 -0.01217 0.00631 -0.00895 AFIX 137 H6A 2 0.023264 0.278430 0.435253 11.00000 -1.50000 H6B 2 -0.121429 0.394475 0.387159 11.00000 -1.50000 H6C 2 -0.024426 0.387648 0.496861 11.00000 -1.50000 AFIX 0 C29 1 -0.087668 0.506951 0.147520 11.00000 0.01904 0.03250 = 0.03240 -0.01648 0.00618 -0.00567 C11 1 -0.101761 0.376444 0.163993 11.00000 0.02486 0.03252 = 0.04406 -0.02032 0.00247 -0.00500 AFIX 43 H11 2 -0.041824 0.307488 0.223080 11.00000 -1.20000 AFIX 0 C15 1 -0.179216 0.604555 0.059832 11.00000 0.02744 0.03546 = 0.03518 -0.01548 0.00267 -0.00903 AFIX 43 H15 2 -0.171759 0.694166 0.045351 11.00000 -1.20000 AFIX 0 C14 1 -0.280539 0.573754 -0.006452 11.00000 0.02598 0.05235 = 0.03578 -0.01876 -0.00064 -0.00851 AFIX 43 H14 2 -0.343232 0.642025 -0.064330 11.00000 -1.20000 AFIX 0 C12 1 -0.200683 0.345360 0.096461 11.00000 0.03299 0.04127 = 0.05263 -0.02921 0.00763 -0.01524 AFIX 43 H12 2 -0.206791 0.255936 0.108599 11.00000 -1.20000 AFIX 0 C13 1 -0.290426 0.444273 0.011506 11.00000 0.02360 0.06267 = 0.04308 -0.03373 0.00679 -0.01803 AFIX 43 H13 2 -0.358978 0.423107 -0.034565 11.00000 -1.20000 AFIX 0 C17 1 -0.133303 0.922181 0.098486 11.00000 0.02598 0.02465 = 0.02883 -0.00751 -0.00303 -0.00354 AFIX 43 H17 2 -0.068622 0.892694 0.044877 11.00000 -1.20000 AFIX 0 C16 1 -0.074556 0.903399 0.207441 11.00000 0.01859 0.01925 = 0.02837 -0.00573 -0.00130 -0.00460 C21 1 -0.172429 0.949514 0.283558 11.00000 0.02182 0.03178 = 0.03065 -0.01035 -0.00121 -0.00235 AFIX 43 H21 2 -0.134265 0.939674 0.357620 11.00000 -1.20000 AFIX 0 C18 1 -0.285163 0.983453 0.067542 11.00000 0.03080 0.03051 = 0.03733 -0.00724 -0.01410 -0.00385 AFIX 43 H18 2 -0.323607 0.995668 -0.007012 11.00000 -1.20000 AFIX 0 C19 1 -0.380587 1.026705 0.144266 11.00000 0.01791 0.03048 = 0.05754 -0.01411 -0.00863 0.00012 AFIX 43 H19 2 -0.484646 1.068278 0.122794 11.00000 -1.20000 AFIX 0 C20 1 -0.324628 1.009481 0.252280 11.00000 0.02181 0.03635 = 0.04660 -0.01582 0.00558 -0.00211 AFIX 43 H20 2 -0.390472 1.038757 0.305452 11.00000 -1.20000 AFIX 0 C22 1 0.173777 0.905057 0.302471 11.00000 0.01406 0.02568 = 0.02698 -0.01055 0.00231 -0.00149 C27 1 0.252365 0.836727 0.406777 11.00000 0.02162 0.02617 = 0.02916 -0.00969 0.00038 -0.00292 AFIX 43 H27 2 0.258722 0.744079 0.438684 11.00000 -1.20000 AFIX 0 C23 1 0.169513 1.040631 0.257005 11.00000 0.02307 0.02528 = 0.03277 -0.00985 -0.00242 -0.00091 AFIX 43 H23 2 0.116752 1.088978 0.185829 11.00000 -1.20000 AFIX 0 C24 1 0.240778 1.105856 0.313773 11.00000 0.02277 0.02406 = 0.04698 -0.01610 0.00021 -0.00262 AFIX 43 H24 2 0.238634 1.197914 0.280818 11.00000 -1.20000 AFIX 0 C26 1 0.321154 0.902506 0.464246 11.00000 0.02419 0.03720 = 0.03459 -0.01468 -0.00541 -0.00212 AFIX 43 H26 2 0.373057 0.854741 0.535871 11.00000 -1.20000 AFIX 0 C25 1 0.315368 1.036663 0.418875 11.00000 0.02014 0.03711 = 0.04603 -0.02499 -0.00216 -0.00433 AFIX 43 H25 2 0.362085 1.081319 0.459275 11.00000 -1.20000 AFIX 0 HKLF 4 REM 4 in P-1 REM R1 = 0.0472 for 2856 Fo > 4sig(Fo) and 0.0648 for all 3635 data REM 275 parameters refined using 0 restraints END WGHT 0.0521 0.4308 REM Highest difference peak 0.300, deepest hole -0.225, 1-sigma level 0.046 Q1 1 -0.0383 0.5032 0.1959 11.00000 0.05 0.30 Q2 1 0.1298 0.8692 0.2781 11.00000 0.05 0.25 Q3 1 -0.0989 0.4550 0.1591 11.00000 0.05 0.24 Q4 1 -0.0870 0.9569 0.1346 11.00000 0.05 0.24 Q5 1 0.0794 0.4843 0.2762 11.00000 0.05 0.22 Q6 1 0.1091 0.7586 0.2810 11.00000 0.05 0.21 Q7 1 0.2449 0.2836 0.5384 11.00000 0.05 0.21 Q8 1 0.2008 0.9606 0.2554 11.00000 0.05 0.18 Q9 1 0.0219 0.5759 0.2141 11.00000 0.05 0.18 Q10 1 0.1429 0.4980 0.3807 11.00000 0.05 0.18 Q11 1 -0.1077 0.5419 0.1186 11.00000 0.05 0.18 Q12 1 0.1813 0.4216 0.3456 11.00000 0.05 0.18 Q13 1 0.3344 0.9668 0.4203 11.00000 0.05 0.18 Q14 1 0.2801 0.4918 0.3522 11.00000 0.05 0.18 Q15 1 0.1359 0.8151 0.1972 11.00000 0.05 0.17 Q16 1 0.2606 0.4147 0.4287 11.00000 0.05 0.16 Q17 1 -0.0764 0.3124 0.2538 11.00000 0.05 0.16 Q18 1 0.3104 0.4224 0.5456 11.00000 0.05 0.16 Q19 1 -0.2061 0.7404 0.0466 11.00000 0.05 0.15 Q20 1 0.4171 0.8268 0.1301 11.00000 0.05 0.15 ; _shelx_res_checksum 20874 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 O1 O 0.06096(14) 0.66793(11) 0.17300(10) 0.0248(3) Uani 1 1 d . . C5 C 0.3145(2) 0.65436(17) 0.24788(15) 0.0232(4) Uani 1 1 d . . B1 B 0.0266(2) 0.5444(2) 0.22140(19) 0.0247(5) Uani 1 1 d . . C3 C 0.2336(2) 0.45061(17) 0.38114(16) 0.0258(4) Uani 1 1 d . . C2 C 0.0889(2) 0.45590(17) 0.34388(16) 0.0261(4) Uani 1 1 d . . C4 C 0.3491(2) 0.52594(17) 0.31050(16) 0.0248(4) Uani 1 1 d . . C1 C 0.1514(2) 0.72372(16) 0.22742(15) 0.0219(4) Uani 1 1 d . . C10 C 0.0881(2) 0.83807(16) 0.24330(15) 0.0221(4) Uani 1 1 d . . C7 C 0.2915(3) 0.36262(19) 0.50041(17) 0.0346(5) Uani 1 1 d . . H7A H 0.2073 0.3631 0.5553 0.052 Uiso 1 1 calc R U H7B H 0.3776 0.3952 0.5234 0.052 Uiso 1 1 calc R U H7C H 0.3272 0.2726 0.4997 0.052 Uiso 1 1 calc R U C8 C 0.5124(2) 0.44988(19) 0.31629(19) 0.0349(5) Uani 1 1 d . . H8A H 0.5680 0.4920 0.2472 0.052 Uiso 1 1 calc R U H8B H 0.5088 0.3593 0.3206 0.052 Uiso 1 1 calc R U H8C H 0.5663 0.4490 0.3848 0.052 Uiso 1 1 calc R U C9 C 0.4357(2) 0.73455(18) 0.18659(18) 0.0311(5) Uani 1 1 d . . H9A H 0.5375 0.6920 0.2226 0.047 Uiso 1 1 calc R U H9B H 0.4096 0.8233 0.1921 0.047 Uiso 1 1 calc R U H9C H 0.4382 0.7401 0.1054 0.047 Uiso 1 1 calc R U C6 C -0.0179(2) 0.37161(19) 0.42282(17) 0.0324(5) Uani 1 1 d . . H6A H 0.0233 0.2784 0.4353 0.049 Uiso 1 1 calc R U H6B H -0.1214 0.3945 0.3872 0.049 Uiso 1 1 calc R U H6C H -0.0244 0.3876 0.4969 0.049 Uiso 1 1 calc R U C29 C -0.0877(2) 0.50695(18) 0.14752(16) 0.0265(4) Uani 1 1 d . . C11 C -0.1018(2) 0.37644(19) 0.16399(18) 0.0319(5) Uani 1 1 d . . H11 H -0.0418 0.3075 0.2231 0.038 Uiso 1 1 calc R U C15 C -0.1792(2) 0.60455(19) 0.05983(17) 0.0313(5) Uani 1 1 d . . H15 H -0.1718 0.6942 0.0454 0.038 Uiso 1 1 calc R U C14 C -0.2805(2) 0.5738(2) -0.00645(18) 0.0367(5) Uani 1 1 d . . H14 H -0.3432 0.6420 -0.0643 0.044 Uiso 1 1 calc R U C12 C -0.2007(3) 0.3454(2) 0.09646(19) 0.0379(5) Uani 1 1 d . . H12 H -0.2068 0.2559 0.1086 0.045 Uiso 1 1 calc R U C13 C -0.2904(2) 0.4443(2) 0.01151(18) 0.0378(5) Uani 1 1 d . . H13 H -0.3590 0.4231 -0.0346 0.045 Uiso 1 1 calc R U C17 C -0.1333(2) 0.92218(17) 0.09849(16) 0.0268(4) Uani 1 1 d . . H17 H -0.0686 0.8927 0.0449 0.032 Uiso 1 1 calc R U C16 C -0.0746(2) 0.90340(16) 0.20744(15) 0.0224(4) Uani 1 1 d . . C21 C -0.1724(2) 0.94951(18) 0.28356(17) 0.0283(4) Uani 1 1 d . . H21 H -0.1343 0.9397 0.3576 0.034 Uiso 1 1 calc R U C18 C -0.2852(2) 0.98345(18) 0.06754(18) 0.0336(5) Uani 1 1 d . . H18 H -0.3236 0.9957 -0.0070 0.040 Uiso 1 1 calc R U C19 C -0.3806(2) 1.02671(19) 0.14427(19) 0.0357(5) Uani 1 1 d . . H19 H -0.4846 1.0683 0.1228 0.043 Uiso 1 1 calc R U C20 C -0.3246(2) 1.00948(19) 0.25228(19) 0.0349(5) Uani 1 1 d . . H20 H -0.3905 1.0388 0.3055 0.042 Uiso 1 1 calc R U C22 C 0.1738(2) 0.90506(17) 0.30247(15) 0.0221(4) Uani 1 1 d . . C27 C 0.2524(2) 0.83673(17) 0.40678(16) 0.0257(4) Uani 1 1 d . . H27 H 0.2587 0.7441 0.4387 0.031 Uiso 1 1 calc R U C23 C 0.1695(2) 1.04063(17) 0.25701(16) 0.0273(4) Uani 1 1 d . . H23 H 0.1168 1.0890 0.1858 0.033 Uiso 1 1 calc R U C24 C 0.2408(2) 1.10586(18) 0.31377(18) 0.0303(5) Uani 1 1 d . . H24 H 0.2386 1.1979 0.2808 0.036 Uiso 1 1 calc R U C26 C 0.3212(2) 0.90251(19) 0.46425(17) 0.0315(5) Uani 1 1 d . . H26 H 0.3731 0.8547 0.5359 0.038 Uiso 1 1 calc R U C25 C 0.3154(2) 1.03666(19) 0.41888(18) 0.0316(5) Uani 1 1 d . . H25 H 0.3621 1.0813 0.4593 0.038 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 O1 0.0194(7) 0.0256(6) 0.0321(7) -0.0132(5) -0.0033(5) -0.0028(5) C5 0.0180(10) 0.0262(9) 0.0284(10) -0.0136(8) 0.0001(8) -0.0029(7) B1 0.0150(11) 0.0278(11) 0.0350(12) -0.0170(9) 0.0063(9) -0.0015(8) C3 0.0261(11) 0.0228(9) 0.0298(10) -0.0120(8) 0.0008(8) -0.0015(8) C2 0.0244(11) 0.0251(9) 0.0331(11) -0.0153(8) 0.0045(8) -0.0054(8) C4 0.0202(10) 0.0276(9) 0.0299(10) -0.0146(8) -0.0020(8) -0.0018(8) C1 0.0198(10) 0.0241(9) 0.0236(9) -0.0086(7) 0.0003(7) -0.0070(7) C10 0.0185(10) 0.0240(9) 0.0228(10) -0.0056(7) -0.0005(7) -0.0046(7) C7 0.0361(13) 0.0300(10) 0.0352(12) -0.0077(8) -0.0038(9) -0.0041(9) C8 0.0222(11) 0.0320(10) 0.0474(13) -0.0121(9) -0.0008(9) 0.0018(8) C9 0.0206(11) 0.0318(10) 0.0410(12) -0.0120(9) 0.0026(9) -0.0051(8) C6 0.0303(12) 0.0337(10) 0.0348(11) -0.0122(9) 0.0063(9) -0.0089(9) C29 0.0190(10) 0.0325(10) 0.0324(11) -0.0165(8) 0.0062(8) -0.0057(8) C11 0.0249(11) 0.0325(10) 0.0441(12) -0.0203(9) 0.0025(9) -0.0050(8) C15 0.0274(12) 0.0355(11) 0.0352(11) -0.0155(9) 0.0027(9) -0.0090(9) C14 0.0260(12) 0.0523(13) 0.0358(12) -0.0188(10) -0.0006(9) -0.0085(10) C12 0.0330(13) 0.0413(12) 0.0526(14) -0.0292(11) 0.0076(10) -0.0152(10) C13 0.0236(12) 0.0627(14) 0.0431(13) -0.0337(11) 0.0068(10) -0.0180(10) C17 0.0260(11) 0.0247(9) 0.0288(10) -0.0075(8) -0.0030(8) -0.0035(8) C16 0.0186(10) 0.0192(8) 0.0284(10) -0.0057(7) -0.0013(8) -0.0046(7) C21 0.0218(11) 0.0318(10) 0.0306(11) -0.0104(8) -0.0012(8) -0.0024(8) C18 0.0308(12) 0.0305(10) 0.0373(12) -0.0072(9) -0.0141(9) -0.0038(9) C19 0.0179(11) 0.0305(10) 0.0575(14) -0.0141(9) -0.0086(10) 0.0001(8) C20 0.0218(11) 0.0363(11) 0.0466(13) -0.0158(9) 0.0056(9) -0.0021(8) C22 0.0141(10) 0.0257(9) 0.0270(10) -0.0106(7) 0.0023(7) -0.0015(7) C27 0.0216(11) 0.0262(9) 0.0292(10) -0.0097(8) 0.0004(8) -0.0029(8) C23 0.0231(11) 0.0253(9) 0.0328(11) -0.0099(8) -0.0024(8) -0.0009(8) C24 0.0228(11) 0.0241(9) 0.0470(12) -0.0161(9) 0.0002(9) -0.0026(8) C26 0.0242(11) 0.0372(11) 0.0346(11) -0.0147(9) -0.0054(9) -0.0021(8) C25 0.0201(11) 0.0371(11) 0.0460(13) -0.0250(9) -0.0022(9) -0.0043(8) 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' O O 0.0106 0.0060 '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 B1 O1 C1 123.71(15) C4 C5 C1 121.07(16) C4 C5 C9 123.10(17) C1 C5 C9 115.67(15) O1 B1 C2 120.85(16) O1 B1 C29 114.46(17) C2 B1 C29 124.54(16) C2 C3 C4 124.21(17) C2 C3 C7 121.30(17) C4 C3 C7 114.47(17) C3 C2 C6 119.58(17) C3 C2 B1 122.50(17) C6 C2 B1 117.92(17) C5 C4 C3 123.21(17) C5 C4 C8 121.12(17) C3 C4 C8 115.63(16) C10 C1 O1 117.80(16) C10 C1 C5 128.21(16) O1 C1 C5 113.56(14) C1 C10 C16 122.24(16) C1 C10 C22 122.21(16) C16 C10 C22 115.51(15) C15 C29 C11 116.76(17) C15 C29 B1 120.65(16) C11 C29 B1 122.59(17) C12 C11 C29 121.71(19) C14 C15 C29 121.61(18) C13 C14 C15 120.0(2) C13 C12 C11 119.95(18) C14 C13 C12 119.91(18) C18 C17 C16 120.71(18) C17 C16 C21 118.07(17) C17 C16 C10 122.02(17) C21 C16 C10 119.90(16) C20 C21 C16 120.81(18) C19 C18 C17 120.40(19) C18 C19 C20 119.81(19) C19 C20 C21 120.19(19) C27 C22 C23 118.15(16) C27 C22 C10 121.59(15) C23 C22 C10 120.17(16) C26 C27 C22 120.58(17) C24 C23 C22 121.13(18) C23 C24 C25 119.90(17) C25 C26 C27 120.78(18) C26 C25 C24 119.44(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 B1 1.368(2) O1 C1 1.393(2) C5 C4 1.346(3) C5 C1 1.484(3) C5 C9 1.517(3) B1 C2 1.558(3) B1 C29 1.571(3) C3 C2 1.354(3) C3 C4 1.489(3) C3 C7 1.515(3) C2 C6 1.522(3) C4 C8 1.514(3) C1 C10 1.345(2) C10 C16 1.491(3) C10 C22 1.493(2) C29 C15 1.398(3) C29 C11 1.401(2) C11 C12 1.383(3) C15 C14 1.386(3) C14 C13 1.377(3) C12 C13 1.379(3) C17 C18 1.387(3) C17 C16 1.394(2) C16 C21 1.398(3) C21 C20 1.387(3) C18 C19 1.378(3) C19 C20 1.378(3) C22 C27 1.393(3) C22 C23 1.395(2) C27 C26 1.382(3) C23 C24 1.383(3) C24 C25 1.387(3) C26 C25 1.379(3)