#------------------------------------------------------------------------------ #$Date: 2019-10-30 04:10:19 +0200 (Wed, 30 Oct 2019) $ #$Revision: 220518 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/25/1552507.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_1552507 _journal_paper_doi 10.1039/C9SC04053F _chemical_absolute_configuration unk _chemical_formula_moiety 'C27 H27 B O' _chemical_formula_sum 'C27 H27 B O' _chemical_formula_weight 378.29 _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' _space_group_name_H-M_alt 'C 1 c 1' _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 c 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 90 _cell_angle_beta 94.762(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 13.4410(8) _cell_length_b 13.1854(8) _cell_length_c 24.0772(16) _cell_measurement_reflns_used 9885 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.61 _cell_measurement_theta_min 2.37 _cell_volume 4252.4(5) _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-2013 (Sheldrick 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.0607 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 38440 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 2.281 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.182 _exptl_crystal_description BLOCK _exptl_crystal_F_000 1616 _exptl_crystal_size_max 0.213 _exptl_crystal_size_mid 0.182 _exptl_crystal_size_min 0.105 _refine_diff_density_max 0.241 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.050 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 532 _refine_ls_number_reflns 7460 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.098 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0437 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.6409P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.1127 _reflns_Friedel_coverage 0.998 _reflns_Friedel_fraction_full 0.977 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 6380 _reflns_number_total 7460 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc04053f2.cif _cod_data_source_block 3 _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 ; _cod_database_code 1552507 _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. ; _shelxl_version_number 2013-4 _shelx_res_file ; TITL CDM278JB in Cc New: CNew:Cc CELL 0.71073 13.4410 13.1854 24.0772 90.000 94.762 90.000 ZERR 8 0.0008 0.0008 0.0016 0.000 0.002 0.000 LATT -7 SYMM X , - Y , 0.50000 + Z SFAC C H B O UNIT 216 216 8 8 TEMP -123 L.S. 5 FMAP 2 PLAN -20 ACTA CONF BOND $H TWIN WGHT 0.064700 0.640900 BASF -0.14309 FVAR 0.08400 RESI 0 O1 4 0.588182 0.213806 0.165605 11.00000 0.01546 0.01758 = 0.02235 -0.00170 0.00243 -0.00068 C1 1 0.696438 0.208345 0.168495 11.00000 0.01402 0.01890 = 0.02307 0.00006 0.00543 -0.00214 C2 1 0.733314 0.198873 0.230641 11.00000 0.01547 0.02118 = 0.02419 0.00197 0.00399 -0.00238 C3 1 0.717575 0.274754 0.266377 11.00000 0.01502 0.02731 = 0.02000 0.00058 0.00396 -0.00200 C4 1 0.674480 0.375302 0.249968 11.00000 0.02205 0.02033 = 0.02235 -0.00393 0.00613 -0.00263 C5 1 0.591408 0.385752 0.215129 11.00000 0.01671 0.02082 = 0.02493 -0.00214 0.00842 -0.00002 C6 1 0.781780 0.101734 0.250410 11.00000 0.03278 0.02734 = 0.02862 0.00487 0.00267 0.00666 AFIX 137 H6A 2 0.824012 0.114103 0.284907 11.00000 -1.50000 H6B 2 0.822854 0.075593 0.221824 11.00000 -1.50000 H6C 2 0.730210 0.051900 0.257445 11.00000 -1.50000 AFIX 0 C7 1 0.745106 0.261929 0.328753 11.00000 0.02635 0.03858 = 0.02112 0.00003 0.00373 0.00097 AFIX 137 H7A 2 0.726234 0.193792 0.340295 11.00000 -1.50000 H7B 2 0.709528 0.312629 0.349331 11.00000 -1.50000 H7C 2 0.817236 0.271128 0.336691 11.00000 -1.50000 AFIX 0 C8 1 0.728195 0.466923 0.276077 11.00000 0.02446 0.03062 = 0.03596 -0.01082 0.00552 -0.00772 AFIX 137 H8A 2 0.745867 0.513328 0.246661 11.00000 -1.50000 H8B 2 0.789035 0.444808 0.297987 11.00000 -1.50000 H8C 2 0.684389 0.501830 0.300455 11.00000 -1.50000 AFIX 0 C9 1 0.550035 0.489886 0.199592 11.00000 0.02538 0.02040 = 0.04183 -0.00290 0.00334 -0.00181 AFIX 137 H9A 2 0.541359 0.528686 0.233569 11.00000 -1.50000 H9B 2 0.485400 0.482614 0.177946 11.00000 -1.50000 H9C 2 0.596612 0.525649 0.177221 11.00000 -1.50000 AFIX 0 C10 1 0.717659 0.110498 0.135496 11.00000 0.01884 0.01673 = 0.01993 0.00235 0.00348 -0.00063 C11 1 0.647646 0.032521 0.130654 11.00000 0.02435 0.02301 = 0.02156 0.00025 0.00860 0.00016 AFIX 43 H11 2 0.585559 0.040948 0.146283 11.00000 -1.20000 AFIX 0 C12 1 0.666743 -0.057014 0.103518 11.00000 0.03173 0.01724 = 0.03136 -0.00074 0.00695 -0.00357 AFIX 43 H12 2 0.617694 -0.109032 0.100384 11.00000 -1.20000 AFIX 0 C13 1 0.756797 -0.070923 0.081014 11.00000 0.03897 0.01848 = 0.02734 -0.00405 0.00745 0.00730 AFIX 43 H13 2 0.770389 -0.132624 0.062725 11.00000 -1.20000 AFIX 0 C14 1 0.826784 0.005444 0.085306 11.00000 0.02658 0.02751 = 0.03705 -0.00031 0.01366 0.00406 AFIX 43 H14 2 0.888907 -0.003726 0.069822 11.00000 -1.20000 AFIX 0 C15 1 0.807415 0.096223 0.112177 11.00000 0.02479 0.02215 = 0.03474 -0.00104 0.00952 0.00012 AFIX 43 H15 2 0.856121 0.148596 0.114494 11.00000 -1.20000 AFIX 0 C16 1 0.739903 0.299384 0.138528 11.00000 0.02273 0.01632 = 0.01899 -0.00369 0.00725 -0.00199 C17 1 0.687381 0.343087 0.092506 11.00000 0.03406 0.02190 = 0.02804 -0.00026 0.00329 -0.00468 AFIX 43 H17 2 0.621335 0.321209 0.081491 11.00000 -1.20000 AFIX 0 C18 1 0.731109 0.418783 0.062471 11.00000 0.05578 0.02118 = 0.02952 0.00603 0.00689 -0.00449 AFIX 43 H18 2 0.694454 0.448588 0.031200 11.00000 -1.20000 AFIX 0 C19 1 0.826589 0.450791 0.077559 11.00000 0.05551 0.02493 = 0.03423 -0.00164 0.02076 -0.01638 AFIX 43 H19 2 0.856396 0.502124 0.056769 11.00000 -1.20000 AFIX 0 C20 1 0.878645 0.407706 0.123125 11.00000 0.03168 0.03501 = 0.03920 -0.01010 0.01633 -0.01544 AFIX 43 H20 2 0.944699 0.429933 0.133821 11.00000 -1.20000 AFIX 0 C21 1 0.836432 0.332354 0.153758 11.00000 0.02319 0.02639 = 0.02666 -0.00585 0.00537 -0.00572 AFIX 43 H21 2 0.873501 0.303327 0.185121 11.00000 -1.20000 AFIX 0 C22 1 0.421250 0.273213 0.187479 11.00000 0.02185 0.01612 = 0.01763 0.00349 0.00127 0.00165 C23 1 0.362505 0.329862 0.221609 11.00000 0.02319 0.01684 = 0.02548 -0.00332 0.00345 0.00374 AFIX 43 H23 2 0.392573 0.383185 0.243601 11.00000 -1.20000 AFIX 0 C24 1 0.262189 0.310221 0.224102 11.00000 0.02570 0.02389 = 0.03301 -0.00160 0.01253 0.00272 AFIX 43 H24 2 0.224336 0.349099 0.248039 11.00000 -1.20000 AFIX 0 C25 1 0.216835 0.234196 0.191870 11.00000 0.01825 0.02426 = 0.04798 -0.00067 0.01088 -0.00223 AFIX 43 H25 2 0.147565 0.221111 0.193178 11.00000 -1.20000 AFIX 0 C26 1 0.272834 0.176844 0.157493 11.00000 0.02318 0.02549 = 0.03619 -0.00527 0.00320 -0.00724 AFIX 43 H26 2 0.241930 0.124287 0.135255 11.00000 -1.20000 AFIX 0 C27 1 0.373190 0.196145 0.155630 11.00000 0.02440 0.01796 = 0.02658 -0.00299 0.00659 -0.00013 AFIX 43 H27 2 0.410747 0.156069 0.132100 11.00000 -1.20000 AFIX 0 B1 3 0.537030 0.290377 0.188728 11.00000 0.02584 0.01589 = 0.01440 0.00128 0.00136 0.00167 O2 4 0.170293 0.543851 0.421226 11.00000 0.01572 0.01872 = 0.02725 0.00073 0.00499 -0.00033 C28 1 0.062092 0.553865 0.416964 11.00000 0.01555 0.01861 = 0.02194 0.00272 0.00478 0.00134 C29 1 0.028562 0.564773 0.354679 11.00000 0.01657 0.02358 = 0.02500 0.00477 0.00652 -0.00002 C30 1 0.041190 0.487642 0.319125 11.00000 0.01705 0.02774 = 0.02051 0.00315 0.00669 -0.00027 C31 1 0.081976 0.386310 0.336065 11.00000 0.01960 0.02467 = 0.02259 -0.00399 0.01079 -0.00412 C32 1 0.164085 0.373545 0.371257 11.00000 0.02105 0.01938 = 0.02756 0.00132 0.00698 0.00083 C33 1 -0.017080 0.664439 0.334619 11.00000 0.03316 0.03002 = 0.03407 0.01017 0.00514 0.00569 AFIX 137 H33A 2 -0.016267 0.668947 0.294031 11.00000 -1.50000 H33B 2 0.021579 0.720650 0.352114 11.00000 -1.50000 H33C 2 -0.086127 0.668303 0.344713 11.00000 -1.50000 AFIX 0 C34 1 0.014375 0.499254 0.256929 11.00000 0.02512 0.04277 = 0.02496 0.00143 0.00519 -0.00216 AFIX 137 H34A 2 -0.058367 0.497377 0.249316 11.00000 -1.50000 H34B 2 0.044306 0.443682 0.237027 11.00000 -1.50000 H34C 2 0.039882 0.564197 0.244310 11.00000 -1.50000 AFIX 0 C35 1 0.026178 0.295828 0.309977 11.00000 0.02828 0.03331 = 0.03523 -0.00695 0.00518 -0.00605 AFIX 137 H35A 2 0.067612 0.262252 0.283839 11.00000 -1.50000 H35B 2 -0.036228 0.318848 0.289984 11.00000 -1.50000 H35C 2 0.011110 0.247944 0.339259 11.00000 -1.50000 AFIX 0 C36 1 0.202120 0.268034 0.385975 11.00000 0.02917 0.01983 = 0.04808 0.00006 -0.00008 -0.00002 AFIX 137 H36A 2 0.156353 0.234681 0.409831 11.00000 -1.50000 H36B 2 0.268614 0.272682 0.405845 11.00000 -1.50000 H36C 2 0.206014 0.228444 0.351776 11.00000 -1.50000 AFIX 0 C37 1 0.012307 0.464730 0.444874 11.00000 0.02278 0.01726 = 0.01882 -0.00143 0.00669 -0.00011 C38 1 0.057262 0.419801 0.492550 11.00000 0.02443 0.02273 = 0.02171 0.00039 0.00416 0.00260 AFIX 43 H38 2 0.123021 0.439273 0.505835 11.00000 -1.20000 AFIX 0 C39 1 0.007804 0.347080 0.521044 11.00000 0.04274 0.02233 = 0.02547 0.00481 0.00974 0.00564 AFIX 43 H39 2 0.039693 0.317101 0.553708 11.00000 -1.20000 AFIX 0 C40 1 -0.087547 0.317784 0.502344 11.00000 0.05233 0.02220 = 0.02466 -0.00565 0.01697 -0.01290 AFIX 43 H40 2 -0.121503 0.267710 0.521936 11.00000 -1.20000 AFIX 0 C41 1 -0.133180 0.361805 0.454958 11.00000 0.03508 0.04288 = 0.02374 -0.00893 0.00817 -0.02326 AFIX 43 H41 2 -0.199023 0.342148 0.441946 11.00000 -1.20000 AFIX 0 C42 1 -0.084069 0.433991 0.426376 11.00000 0.02466 0.03987 = 0.01902 -0.00056 0.00236 -0.00761 AFIX 43 H42 2 -0.116214 0.463312 0.393594 11.00000 -1.20000 AFIX 0 C43 1 0.043871 0.649839 0.451685 11.00000 0.02668 0.01939 = 0.01966 0.00449 0.00771 0.00574 C44 1 -0.049696 0.671107 0.469636 11.00000 0.01909 0.02779 = 0.03884 -0.00183 0.00761 0.00023 AFIX 43 H44 2 -0.103856 0.626672 0.459588 11.00000 -1.20000 AFIX 0 C45 1 -0.065405 0.755371 0.501714 11.00000 0.03477 0.03420 = 0.04138 -0.00179 0.01521 0.00917 AFIX 43 H45 2 -0.130136 0.768982 0.513013 11.00000 -1.20000 AFIX 0 C46 1 0.012419 0.819708 0.517372 11.00000 0.04277 0.02659 = 0.04393 -0.01088 0.01544 0.00285 AFIX 43 H46 2 0.002055 0.877150 0.540001 11.00000 -1.20000 AFIX 0 C47 1 0.105507 0.800099 0.499949 11.00000 0.03788 0.02362 = 0.04768 -0.00755 0.01134 -0.00147 AFIX 43 H47 2 0.159593 0.844293 0.510562 11.00000 -1.20000 AFIX 0 C48 1 0.120773 0.715982 0.466909 11.00000 0.02712 0.02007 = 0.03645 -0.00210 0.00981 -0.00036 AFIX 43 H48 2 0.185102 0.703904 0.454649 11.00000 -1.20000 AFIX 0 C49 1 0.336751 0.481515 0.402398 11.00000 0.02236 0.01585 = 0.02249 0.00187 0.00423 0.00109 C50 1 0.396570 0.425344 0.368772 11.00000 0.02203 0.02032 = 0.03282 -0.00258 0.00712 -0.00202 AFIX 43 H50 2 0.367123 0.373070 0.345752 11.00000 -1.20000 AFIX 0 C51 1 0.498314 0.444520 0.368379 11.00000 0.02574 0.02683 = 0.04361 -0.00461 0.01264 0.00187 AFIX 43 H51 2 0.537459 0.406411 0.344756 11.00000 -1.20000 AFIX 0 C52 1 0.542381 0.519380 0.402551 11.00000 0.01954 0.03269 = 0.05493 0.00252 0.00913 -0.00188 AFIX 43 H52 2 0.611989 0.532068 0.402783 11.00000 -1.20000 AFIX 0 C53 1 0.485251 0.575140 0.436052 11.00000 0.03006 0.02682 = 0.04140 -0.01009 0.00443 -0.00395 AFIX 43 H53 2 0.515387 0.626430 0.459512 11.00000 -1.20000 AFIX 0 C54 1 0.383627 0.556753 0.435722 11.00000 0.02160 0.02621 = 0.03022 -0.00435 0.00473 0.00108 AFIX 43 H54 2 0.344951 0.596505 0.458828 11.00000 -1.20000 AFIX 0 B2 3 0.220132 0.466241 0.398591 11.00000 0.02225 0.01891 = 0.01901 0.00509 0.00595 0.00397 HKLF 4 REM CDM278JB in Cc New: CNew:Cc REM R1 = 0.0437 for 6380 Fo > 4sig(Fo) and 0.0580 for all 7460 data REM 532 parameters refined using 2 restraints END WGHT 0.0647 0.6409 REM Highest difference peak 0.241, deepest hole -0.216, 1-sigma level 0.050 Q1 1 0.1204 0.2118 0.1648 11.00000 0.05 0.24 Q2 1 0.2045 0.2853 0.2662 11.00000 0.05 0.23 Q3 1 0.1651 0.3775 0.2172 11.00000 0.05 0.21 Q4 1 0.1090 0.3643 0.2218 11.00000 0.05 0.20 Q5 1 -0.1572 0.4967 0.4011 11.00000 0.05 0.18 Q6 1 0.6551 0.5400 0.4243 11.00000 0.05 0.18 Q7 1 0.2400 0.2231 0.2410 11.00000 0.05 0.18 Q8 1 0.9378 0.2930 0.1828 11.00000 0.05 0.18 Q9 1 0.0734 0.2297 0.3213 11.00000 0.05 0.18 Q10 1 0.2200 0.2838 0.1929 11.00000 0.05 0.18 Q11 1 0.1364 0.2860 0.1586 11.00000 0.05 0.18 Q12 1 0.1765 0.3922 0.2550 11.00000 0.05 0.18 Q13 1 0.0794 0.1615 0.1924 11.00000 0.05 0.18 Q14 1 0.2210 0.3086 0.1426 11.00000 0.05 0.17 Q15 1 0.1152 0.2654 0.1895 11.00000 0.05 0.17 Q16 1 0.1126 0.3821 0.3683 11.00000 0.05 0.17 Q17 1 0.9060 0.2685 0.1825 11.00000 0.05 0.17 Q18 1 0.2463 0.0977 0.1303 11.00000 0.05 0.17 Q19 1 0.2810 0.4669 0.4037 11.00000 0.05 0.16 Q20 1 0.0383 0.2768 0.1810 11.00000 0.05 0.16 ; _shelx_res_checksum 75792 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -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 O1 O 0.58818(15) 0.21381(16) 0.16560(10) 0.0184(5) Uani 1 1 d . . C1 C 0.6964(3) 0.2083(3) 0.16850(15) 0.0184(8) Uani 1 1 d . . C2 C 0.7333(2) 0.1989(3) 0.23064(15) 0.0201(8) Uani 1 1 d . . C3 C 0.7176(2) 0.2748(3) 0.26638(15) 0.0206(8) Uani 1 1 d . . C4 C 0.6745(3) 0.3753(3) 0.24997(15) 0.0213(8) Uani 1 1 d . . C5 C 0.5914(3) 0.3858(3) 0.21513(15) 0.0204(8) Uani 1 1 d . . C6 C 0.7818(3) 0.1017(3) 0.25041(17) 0.0296(9) Uani 1 1 d . . H6A H 0.8240 0.1141 0.2849 0.044 Uiso 1 1 calc R U H6B H 0.8229 0.0756 0.2218 0.044 Uiso 1 1 calc R U H6C H 0.7302 0.0519 0.2574 0.044 Uiso 1 1 calc R U C7 C 0.7451(3) 0.2619(3) 0.32875(15) 0.0286(9) Uani 1 1 d . . H7A H 0.7262 0.1938 0.3403 0.043 Uiso 1 1 calc R U H7B H 0.7095 0.3126 0.3493 0.043 Uiso 1 1 calc R U H7C H 0.8172 0.2711 0.3367 0.043 Uiso 1 1 calc R U C8 C 0.7282(3) 0.4669(3) 0.27608(17) 0.0302(9) Uani 1 1 d . . H8A H 0.7459 0.5133 0.2467 0.045 Uiso 1 1 calc R U H8B H 0.7890 0.4448 0.2980 0.045 Uiso 1 1 calc R U H8C H 0.6844 0.5018 0.3005 0.045 Uiso 1 1 calc R U C9 C 0.5500(3) 0.4899(3) 0.19959(18) 0.0292(9) Uani 1 1 d . . H9A H 0.5414 0.5287 0.2336 0.044 Uiso 1 1 calc R U H9B H 0.4854 0.4826 0.1779 0.044 Uiso 1 1 calc R U H9C H 0.5966 0.5256 0.1772 0.044 Uiso 1 1 calc R U C10 C 0.7177(2) 0.1105(3) 0.13550(15) 0.0184(7) Uani 1 1 d . . C11 C 0.6476(3) 0.0325(3) 0.13065(15) 0.0226(8) Uani 1 1 d . . H11 H 0.5856 0.0409 0.1463 0.027 Uiso 1 1 calc R U C12 C 0.6667(3) -0.0570(3) 0.10352(15) 0.0265(8) Uani 1 1 d . . H12 H 0.6177 -0.1090 0.1004 0.032 Uiso 1 1 calc R U C13 C 0.7568(3) -0.0709(3) 0.08101(16) 0.0280(9) Uani 1 1 d . . H13 H 0.7704 -0.1326 0.0627 0.034 Uiso 1 1 calc R U C14 C 0.8268(3) 0.0054(3) 0.08531(17) 0.0298(9) Uani 1 1 d . . H14 H 0.8889 -0.0037 0.0698 0.036 Uiso 1 1 calc R U C15 C 0.8074(3) 0.0962(3) 0.11218(16) 0.0268(9) Uani 1 1 d . . H15 H 0.8561 0.1486 0.1145 0.032 Uiso 1 1 calc R U C16 C 0.7399(2) 0.2994(3) 0.13853(14) 0.0190(8) Uani 1 1 d . . C17 C 0.6874(3) 0.3431(3) 0.09251(16) 0.0280(9) Uani 1 1 d . . H17 H 0.6213 0.3212 0.0815 0.034 Uiso 1 1 calc R U C18 C 0.7311(4) 0.4188(3) 0.06247(19) 0.0353(10) Uani 1 1 d . . H18 H 0.6945 0.4486 0.0312 0.042 Uiso 1 1 calc R U C19 C 0.8266(3) 0.4508(3) 0.07756(18) 0.0373(11) Uani 1 1 d . . H19 H 0.8564 0.5021 0.0568 0.045 Uiso 1 1 calc R U C20 C 0.8786(3) 0.4077(3) 0.12312(17) 0.0346(10) Uani 1 1 d . . H20 H 0.9447 0.4299 0.1338 0.041 Uiso 1 1 calc R U C21 C 0.8364(3) 0.3324(3) 0.15376(16) 0.0252(8) Uani 1 1 d . . H21 H 0.8735 0.3033 0.1851 0.030 Uiso 1 1 calc R U C22 C 0.4213(3) 0.2732(2) 0.18748(14) 0.0186(8) Uani 1 1 d . . C23 C 0.3625(3) 0.3299(3) 0.22161(15) 0.0218(8) Uani 1 1 d . . H23 H 0.3926 0.3832 0.2436 0.026 Uiso 1 1 calc R U C24 C 0.2622(3) 0.3102(3) 0.22410(16) 0.0270(9) Uani 1 1 d . . H24 H 0.2243 0.3491 0.2480 0.032 Uiso 1 1 calc R U C25 C 0.2168(3) 0.2342(3) 0.19187(18) 0.0297(9) Uani 1 1 d . . H25 H 0.1476 0.2211 0.1932 0.036 Uiso 1 1 calc R U C26 C 0.2728(3) 0.1768(3) 0.15749(16) 0.0282(9) Uani 1 1 d . . H26 H 0.2419 0.1243 0.1353 0.034 Uiso 1 1 calc R U C27 C 0.3732(3) 0.1961(3) 0.15563(16) 0.0227(8) Uani 1 1 d . . H27 H 0.4107 0.1561 0.1321 0.027 Uiso 1 1 calc R U B1 B 0.5370(3) 0.2904(3) 0.18873(16) 0.0187(9) Uani 1 1 d . . O2 O 0.17029(16) 0.54385(17) 0.42123(10) 0.0204(5) Uani 1 1 d . . C28 C 0.0621(2) 0.5539(3) 0.41696(15) 0.0185(8) Uani 1 1 d . . C29 C 0.0286(2) 0.5648(3) 0.35468(15) 0.0214(8) Uani 1 1 d . . C30 C 0.0412(2) 0.4876(3) 0.31912(15) 0.0215(8) Uani 1 1 d . . C31 C 0.0820(3) 0.3863(3) 0.33607(15) 0.0218(8) Uani 1 1 d . . C32 C 0.1641(3) 0.3735(3) 0.37126(15) 0.0224(8) Uani 1 1 d . . C33 C -0.0171(3) 0.6644(3) 0.33462(18) 0.0323(9) Uani 1 1 d . . H33A H -0.0163 0.6689 0.2940 0.048 Uiso 1 1 calc R U H33B H 0.0216 0.7206 0.3521 0.048 Uiso 1 1 calc R U H33C H -0.0861 0.6683 0.3447 0.048 Uiso 1 1 calc R U C34 C 0.0144(3) 0.4993(3) 0.25693(16) 0.0308(9) Uani 1 1 d . . H34A H -0.0584 0.4974 0.2493 0.046 Uiso 1 1 calc R U H34B H 0.0443 0.4437 0.2370 0.046 Uiso 1 1 calc R U H34C H 0.0399 0.5642 0.2443 0.046 Uiso 1 1 calc R U C35 C 0.0262(3) 0.2958(3) 0.30998(17) 0.0321(9) Uani 1 1 d . . H35A H 0.0676 0.2623 0.2838 0.048 Uiso 1 1 calc R U H35B H -0.0362 0.3188 0.2900 0.048 Uiso 1 1 calc R U H35C H 0.0111 0.2479 0.3393 0.048 Uiso 1 1 calc R U C36 C 0.2021(3) 0.2680(3) 0.38598(19) 0.0325(10) Uani 1 1 d . . H36A H 0.1564 0.2347 0.4098 0.049 Uiso 1 1 calc R U H36B H 0.2686 0.2727 0.4058 0.049 Uiso 1 1 calc R U H36C H 0.2060 0.2284 0.3518 0.049 Uiso 1 1 calc R U C37 C 0.0123(3) 0.4647(3) 0.44487(14) 0.0193(8) Uani 1 1 d . . C38 C 0.0573(3) 0.4198(3) 0.49255(15) 0.0228(8) Uani 1 1 d . . H38 H 0.1230 0.4393 0.5058 0.027 Uiso 1 1 calc R U C39 C 0.0078(3) 0.3471(3) 0.52104(17) 0.0298(9) Uani 1 1 d . . H39 H 0.0397 0.3171 0.5537 0.036 Uiso 1 1 calc R U C40 C -0.0875(3) 0.3178(3) 0.50234(16) 0.0323(10) Uani 1 1 d . . H40 H -0.1215 0.2677 0.5219 0.039 Uiso 1 1 calc R U C41 C -0.1332(3) 0.3618(3) 0.45496(16) 0.0336(10) Uani 1 1 d . . H41 H -0.1990 0.3421 0.4419 0.040 Uiso 1 1 calc R U C42 C -0.0841(3) 0.4340(3) 0.42638(15) 0.0278(9) Uani 1 1 d . . H42 H -0.1162 0.4633 0.3936 0.033 Uiso 1 1 calc R U C43 C 0.0439(3) 0.6498(3) 0.45169(15) 0.0216(8) Uani 1 1 d . . C44 C -0.0497(3) 0.6711(3) 0.46964(17) 0.0283(9) Uani 1 1 d . . H44 H -0.1039 0.6267 0.4596 0.034 Uiso 1 1 calc R U C45 C -0.0654(3) 0.7554(3) 0.50171(19) 0.0361(10) Uani 1 1 d . . H45 H -0.1301 0.7690 0.5130 0.043 Uiso 1 1 calc R U C46 C 0.0124(3) 0.8197(3) 0.51737(19) 0.0371(10) Uani 1 1 d . . H46 H 0.0021 0.8771 0.5400 0.045 Uiso 1 1 calc R U C47 C 0.1055(3) 0.8001(3) 0.49995(18) 0.0360(10) Uani 1 1 d . . H47 H 0.1596 0.8443 0.5106 0.043 Uiso 1 1 calc R U C48 C 0.1208(3) 0.7160(3) 0.46691(17) 0.0275(9) Uani 1 1 d . . H48 H 0.1851 0.7039 0.4546 0.033 Uiso 1 1 calc R U C49 C 0.3368(3) 0.4815(3) 0.40240(15) 0.0201(8) Uani 1 1 d . . C50 C 0.3966(3) 0.4253(3) 0.36877(16) 0.0248(8) Uani 1 1 d . . H50 H 0.3671 0.3731 0.3458 0.030 Uiso 1 1 calc R U C51 C 0.4983(3) 0.4445(3) 0.36838(18) 0.0315(9) Uani 1 1 d . . H51 H 0.5375 0.4064 0.3448 0.038 Uiso 1 1 calc R U C52 C 0.5424(3) 0.5194(3) 0.40255(19) 0.0354(11) Uani 1 1 d . . H52 H 0.6120 0.5321 0.4028 0.042 Uiso 1 1 calc R U C53 C 0.4853(3) 0.5751(3) 0.43605(18) 0.0327(9) Uani 1 1 d . . H53 H 0.5154 0.6264 0.4595 0.039 Uiso 1 1 calc R U C54 C 0.3836(3) 0.5568(3) 0.43572(16) 0.0259(8) Uani 1 1 d . . H54 H 0.3450 0.5965 0.4588 0.031 Uiso 1 1 calc R U B2 B 0.2201(3) 0.4662(3) 0.39859(16) 0.0198(9) 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 O1 0.0155(12) 0.0176(12) 0.0224(13) -0.0017(10) 0.0024(10) -0.0007(9) C1 0.0140(18) 0.0189(19) 0.023(2) 0.0001(15) 0.0054(15) -0.0021(14) C2 0.0155(17) 0.0212(18) 0.024(2) 0.0020(15) 0.0040(14) -0.0024(14) C3 0.0150(17) 0.027(2) 0.0200(19) 0.0006(15) 0.0040(14) -0.0020(14) C4 0.0221(19) 0.0203(19) 0.0224(19) -0.0039(15) 0.0061(15) -0.0026(14) C5 0.0167(18) 0.0208(19) 0.025(2) -0.0021(15) 0.0084(15) 0.0000(14) C6 0.033(2) 0.027(2) 0.029(2) 0.0049(17) 0.0027(17) 0.0067(17) C7 0.026(2) 0.039(2) 0.021(2) 0.0000(17) 0.0037(16) 0.0010(17) C8 0.024(2) 0.031(2) 0.036(2) -0.0108(18) 0.0055(17) -0.0077(17) C9 0.025(2) 0.0204(19) 0.042(2) -0.0029(17) 0.0033(17) -0.0018(16) C10 0.0188(18) 0.0167(18) 0.0199(18) 0.0023(15) 0.0035(14) -0.0006(14) C11 0.0244(19) 0.0230(19) 0.0216(19) 0.0002(15) 0.0086(15) 0.0002(15) C12 0.032(2) 0.0172(18) 0.031(2) -0.0007(16) 0.0070(16) -0.0036(15) C13 0.039(2) 0.0185(19) 0.027(2) -0.0040(17) 0.0074(17) 0.0073(17) C14 0.027(2) 0.028(2) 0.037(2) -0.0003(18) 0.0137(17) 0.0041(16) C15 0.025(2) 0.0222(19) 0.035(2) -0.0010(16) 0.0095(17) 0.0001(15) C16 0.0227(18) 0.0163(17) 0.0190(19) -0.0037(14) 0.0072(15) -0.0020(14) C17 0.034(2) 0.0219(19) 0.028(2) -0.0003(17) 0.0033(17) -0.0047(16) C18 0.056(3) 0.021(2) 0.030(2) 0.0060(18) 0.007(2) -0.0045(19) C19 0.056(3) 0.025(2) 0.034(2) -0.0016(18) 0.021(2) -0.016(2) C20 0.032(2) 0.035(2) 0.039(3) -0.010(2) 0.0163(19) -0.0154(18) C21 0.0232(18) 0.026(2) 0.027(2) -0.0058(16) 0.0054(15) -0.0057(16) C22 0.0218(18) 0.0161(17) 0.0176(19) 0.0035(14) 0.0013(14) 0.0016(14) C23 0.0232(19) 0.0168(18) 0.025(2) -0.0033(15) 0.0034(15) 0.0037(14) C24 0.026(2) 0.0239(19) 0.033(2) -0.0016(17) 0.0125(17) 0.0027(16) C25 0.0182(19) 0.024(2) 0.048(3) -0.0007(19) 0.0109(18) -0.0022(16) C26 0.023(2) 0.025(2) 0.036(2) -0.0053(17) 0.0032(17) -0.0072(16) C27 0.024(2) 0.0180(18) 0.027(2) -0.0030(15) 0.0066(16) -0.0001(15) B1 0.026(2) 0.016(2) 0.014(2) 0.0013(16) 0.0014(17) 0.0017(16) O2 0.0157(12) 0.0187(12) 0.0273(13) 0.0007(10) 0.0050(10) -0.0003(10) C28 0.0155(18) 0.0186(18) 0.0219(19) 0.0027(15) 0.0048(14) 0.0013(14) C29 0.0166(17) 0.0236(19) 0.0250(19) 0.0048(16) 0.0065(14) 0.0000(15) C30 0.0171(18) 0.028(2) 0.0205(19) 0.0032(16) 0.0067(14) -0.0003(15) C31 0.0196(19) 0.025(2) 0.0226(19) -0.0040(15) 0.0108(15) -0.0041(14) C32 0.0211(19) 0.0194(19) 0.028(2) 0.0013(15) 0.0070(16) 0.0008(14) C33 0.033(2) 0.030(2) 0.034(2) 0.0102(18) 0.0051(18) 0.0057(17) C34 0.025(2) 0.043(2) 0.025(2) 0.0014(18) 0.0052(16) -0.0022(18) C35 0.028(2) 0.033(2) 0.035(2) -0.0070(18) 0.0052(18) -0.0060(17) C36 0.029(2) 0.0198(19) 0.048(3) 0.0001(19) -0.0001(19) 0.0000(16) C37 0.0228(18) 0.0173(17) 0.0188(19) -0.0014(15) 0.0067(14) -0.0001(14) C38 0.0244(19) 0.0227(19) 0.0217(19) 0.0004(16) 0.0042(15) 0.0026(15) C39 0.043(2) 0.022(2) 0.025(2) 0.0048(17) 0.0097(18) 0.0056(18) C40 0.052(3) 0.022(2) 0.025(2) -0.0056(17) 0.0170(19) -0.0129(18) C41 0.035(2) 0.043(2) 0.024(2) -0.0089(18) 0.0082(17) -0.0233(19) C42 0.025(2) 0.040(2) 0.019(2) -0.0006(17) 0.0024(15) -0.0076(17) C43 0.0267(19) 0.0194(18) 0.0197(19) 0.0045(15) 0.0077(15) 0.0057(15) C44 0.0191(19) 0.028(2) 0.039(2) -0.0018(18) 0.0076(17) 0.0002(15) C45 0.035(2) 0.034(2) 0.041(3) -0.002(2) 0.015(2) 0.0092(19) C46 0.043(3) 0.027(2) 0.044(3) -0.0109(19) 0.015(2) 0.0028(19) C47 0.038(2) 0.024(2) 0.048(3) -0.0076(18) 0.011(2) -0.0015(17) C48 0.027(2) 0.0201(18) 0.036(2) -0.0021(16) 0.0098(17) -0.0004(15) C49 0.0224(19) 0.0158(17) 0.0225(19) 0.0019(15) 0.0042(15) 0.0011(14) C50 0.0220(19) 0.0203(18) 0.033(2) -0.0026(17) 0.0071(16) -0.0020(15) C51 0.026(2) 0.027(2) 0.044(2) -0.0046(19) 0.0126(18) 0.0019(17) C52 0.020(2) 0.033(2) 0.055(3) 0.003(2) 0.0091(19) -0.0019(17) C53 0.030(2) 0.027(2) 0.041(2) -0.0101(19) 0.0044(18) -0.0040(17) C54 0.0216(19) 0.026(2) 0.030(2) -0.0043(16) 0.0047(16) 0.0011(15) B2 0.022(2) 0.019(2) 0.019(2) 0.0051(17) 0.0060(16) 0.0040(17) 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 123.6(3) O1 C1 C16 110.9(3) O1 C1 C2 106.9(3) C16 C1 C2 114.4(3) O1 C1 C10 104.0(3) C16 C1 C10 108.3(3) C2 C1 C10 111.8(3) C3 C2 C6 121.3(3) C3 C2 C1 120.3(3) C6 C2 C1 118.3(3) C2 C3 C4 124.8(3) C2 C3 C7 120.5(3) C4 C3 C7 114.7(3) C5 C4 C3 122.8(3) C5 C4 C8 121.2(3) C3 C4 C8 116.0(3) C4 C5 C9 121.0(3) C4 C5 B1 120.4(3) C9 C5 B1 118.6(3) C2 C6 H6A 109.5 C2 C6 H6B 109.5 H6A C6 H6B 109.5 C2 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C3 C7 H7A 109.5 C3 C7 H7B 109.5 H7A C7 H7B 109.5 C3 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C4 C8 H8A 109.5 C4 C8 H8B 109.5 H8A C8 H8B 109.5 C4 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C5 C9 H9A 109.5 C5 C9 H9B 109.5 H9A C9 H9B 109.5 C5 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C15 C10 C11 118.1(3) C15 C10 C1 121.5(3) C11 C10 C1 120.3(3) C12 C11 C10 121.3(3) C12 C11 H11 119.4 C10 C11 H11 119.4 C13 C12 C11 120.2(4) C13 C12 H12 119.9 C11 C12 H12 119.9 C14 C13 C12 119.3(4) C14 C13 H13 120.3 C12 C13 H13 120.3 C13 C14 C15 120.7(4) C13 C14 H14 119.7 C15 C14 H14 119.7 C10 C15 C14 120.5(3) C10 C15 H15 119.8 C14 C15 H15 119.8 C21 C16 C17 118.9(3) C21 C16 C1 120.2(3) C17 C16 C1 120.6(3) C16 C17 C18 120.3(4) C16 C17 H17 119.9 C18 C17 H17 119.9 C19 C18 C17 120.6(4) C19 C18 H18 119.7 C17 C18 H18 119.7 C18 C19 C20 119.2(4) C18 C19 H19 120.4 C20 C19 H19 120.4 C19 C20 C21 121.1(4) C19 C20 H20 119.4 C21 C20 H20 119.4 C20 C21 C16 119.9(4) C20 C21 H21 120.0 C16 C21 H21 120.0 C27 C22 C23 116.9(3) C27 C22 B1 121.8(3) C23 C22 B1 121.2(3) C24 C23 C22 121.7(3) C24 C23 H23 119.1 C22 C23 H23 119.1 C25 C24 C23 120.0(3) C25 C24 H24 120.0 C23 C24 H24 120.0 C24 C25 C26 119.7(3) C24 C25 H25 120.1 C26 C25 H25 120.1 C27 C26 C25 120.0(4) C27 C26 H26 120.0 C25 C26 H26 120.0 C26 C27 C22 121.7(3) C26 C27 H27 119.1 C22 C27 H27 119.1 O1 B1 C5 121.8(3) O1 B1 C22 114.7(3) C5 B1 C22 123.6(3) B2 O2 C28 124.2(3) O2 C28 C37 111.7(3) O2 C28 C29 106.7(3) C37 C28 C29 113.3(3) O2 C28 C43 103.8(3) C37 C28 C43 107.2(3) C29 C28 C43 113.8(3) C30 C29 C33 121.4(3) C30 C29 C28 120.4(3) C33 C29 C28 118.1(3) C29 C30 C31 124.5(3) C29 C30 C34 121.2(3) C31 C30 C34 114.4(3) C32 C31 C30 123.3(3) C32 C31 C35 120.9(3) C30 C31 C35 115.7(3) C31 C32 C36 120.4(3) C31 C32 B2 120.8(3) C36 C32 B2 118.8(3) C29 C33 H33A 109.5 C29 C33 H33B 109.5 H33A C33 H33B 109.5 C29 C33 H33C 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 C30 C34 H34A 109.5 C30 C34 H34B 109.5 H34A C34 H34B 109.5 C30 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 C31 C35 H35A 109.5 C31 C35 H35B 109.5 H35A C35 H35B 109.5 C31 C35 H35C 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 C32 C36 H36A 109.5 C32 C36 H36B 109.5 H36A C36 H36B 109.5 C32 C36 H36C 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 C38 C37 C42 118.0(3) C38 C37 C28 121.0(3) C42 C37 C28 120.7(3) C39 C38 C37 120.9(3) C39 C38 H38 119.5 C37 C38 H38 119.5 C40 C39 C38 120.3(4) C40 C39 H39 119.8 C38 C39 H39 119.8 C41 C40 C39 119.4(4) C41 C40 H40 120.3 C39 C40 H40 120.3 C42 C41 C40 120.5(4) C42 C41 H41 119.8 C40 C41 H41 119.8 C41 C42 C37 120.9(3) C41 C42 H42 119.6 C37 C42 H42 119.6 C48 C43 C44 117.8(3) C48 C43 C28 120.8(3) C44 C43 C28 121.3(3) C45 C44 C43 121.4(4) C45 C44 H44 119.3 C43 C44 H44 119.3 C46 C45 C44 120.1(4) C46 C45 H45 119.9 C44 C45 H45 119.9 C45 C46 C47 119.4(4) C45 C46 H46 120.3 C47 C46 H46 120.3 C46 C47 C48 120.4(4) C46 C47 H47 119.8 C48 C47 H47 119.8 C43 C48 C47 120.9(4) C43 C48 H48 119.5 C47 C48 H48 119.5 C54 C49 C50 117.1(3) C54 C49 B2 121.7(3) C50 C49 B2 121.0(3) C51 C50 C49 121.3(3) C51 C50 H50 119.3 C49 C50 H50 119.3 C52 C51 C50 119.8(4) C52 C51 H51 120.1 C50 C51 H51 120.1 C53 C52 C51 119.9(4) C53 C52 H52 120.1 C51 C52 H52 120.1 C52 C53 C54 120.1(4) C52 C53 H53 119.9 C54 C53 H53 119.9 C53 C54 C49 121.7(3) C53 C54 H54 119.1 C49 C54 H54 119.1 O2 B2 C32 121.6(3) O2 B2 C49 113.6(3) C32 B2 C49 124.8(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 B1 1.366(4) O1 C1 1.453(4) C1 C16 1.540(5) C1 C2 1.542(5) C1 C10 1.554(5) C2 C3 1.348(5) C2 C6 1.497(5) C3 C4 1.487(5) C3 C7 1.526(5) C4 C5 1.347(5) C4 C8 1.517(5) C5 C9 1.517(5) C5 B1 1.563(5) C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C10 C15 1.385(5) C10 C11 1.392(5) C11 C12 1.384(5) C11 H11 0.9500 C12 C13 1.379(5) C12 H12 0.9500 C13 C14 1.376(6) C13 H13 0.9500 C14 C15 1.395(5) C14 H14 0.9500 C15 H15 0.9500 C16 C21 1.388(5) C16 C17 1.389(5) C17 C18 1.391(6) C17 H17 0.9500 C18 C19 1.371(6) C18 H18 0.9500 C19 C20 1.374(6) C19 H19 0.9500 C20 C21 1.387(5) C20 H20 0.9500 C21 H21 0.9500 C22 C27 1.398(5) C22 C23 1.402(5) C22 B1 1.570(5) C23 C24 1.379(5) C23 H23 0.9500 C24 C25 1.378(6) C24 H24 0.9500 C25 C26 1.388(5) C25 H25 0.9500 C26 C27 1.377(5) C26 H26 0.9500 C27 H27 0.9500 O2 B2 1.361(5) O2 C28 1.455(4) C28 C37 1.535(5) C28 C29 1.536(5) C28 C43 1.547(5) C29 C30 1.349(5) C29 C33 1.512(5) C30 C31 1.488(5) C30 C34 1.519(5) C31 C32 1.345(5) C31 C35 1.517(5) C32 C36 1.514(5) C32 B2 1.553(5) C33 H33A 0.9800 C33 H33B 0.9800 C33 H33C 0.9800 C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C35 H35A 0.9800 C35 H35B 0.9800 C35 H35C 0.9800 C36 H36A 0.9800 C36 H36B 0.9800 C36 H36C 0.9800 C37 C38 1.385(5) C37 C42 1.395(5) C38 C39 1.381(5) C38 H38 0.9500 C39 C40 1.378(6) C39 H39 0.9500 C40 C41 1.378(6) C40 H40 0.9500 C41 C42 1.375(5) C41 H41 0.9500 C42 H42 0.9500 C43 C48 1.379(5) C43 C44 1.392(5) C44 C45 1.379(6) C44 H44 0.9500 C45 C46 1.375(6) C45 H45 0.9500 C46 C47 1.377(6) C46 H46 0.9500 C47 C48 1.390(5) C47 H47 0.9500 C48 H48 0.9500 C49 C54 1.393(5) C49 C50 1.399(5) C49 B2 1.575(5) C50 C51 1.392(5) C50 H50 0.9500 C51 C52 1.386(6) C51 H51 0.9500 C52 C53 1.372(6) C52 H52 0.9500 C53 C54 1.387(5) C53 H53 0.9500 C54 H54 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 B1 O1 C1 C16 -62.5(4) B1 O1 C1 C2 62.8(4) B1 O1 C1 C10 -178.8(3) O1 C1 C2 C3 -64.0(4) C16 C1 C2 C3 59.2(4) C10 C1 C2 C3 -177.2(3) O1 C1 C2 C6 112.9(3) C16 C1 C2 C6 -124.0(3) C10 C1 C2 C6 -0.3(4) C6 C2 C3 C4 176.9(3) C1 C2 C3 C4 -6.3(5) C6 C2 C3 C7 -2.5(5) C1 C2 C3 C7 174.3(3) C2 C3 C4 C5 47.7(5) C7 C3 C4 C5 -132.8(4) C2 C3 C4 C8 -133.8(4) C7 C3 C4 C8 45.6(4) C3 C4 C5 C9 179.9(3) C8 C4 C5 C9 1.6(5) C3 C4 C5 B1 -1.5(5) C8 C4 C5 B1 -179.9(3) O1 C1 C10 C15 157.4(3) C16 C1 C10 C15 39.4(4) C2 C1 C10 C15 -87.7(4) O1 C1 C10 C11 -25.3(4) C16 C1 C10 C11 -143.4(3) C2 C1 C10 C11 89.6(4) C15 C10 C11 C12 0.2(5) C1 C10 C11 C12 -177.2(3) C10 C11 C12 C13 0.6(6) C11 C12 C13 C14 -0.7(6) C12 C13 C14 C15 0.1(6) C11 C10 C15 C14 -0.8(6) C1 C10 C15 C14 176.6(3) C13 C14 C15 C10 0.7(6) O1 C1 C16 C21 154.4(3) C2 C1 C16 C21 33.4(4) C10 C1 C16 C21 -92.1(4) O1 C1 C16 C17 -32.1(4) C2 C1 C16 C17 -153.1(3) C10 C1 C16 C17 81.5(4) C21 C16 C17 C18 -0.2(6) C1 C16 C17 C18 -173.8(4) C16 C17 C18 C19 0.4(6) C17 C18 C19 C20 -0.5(6) C18 C19 C20 C21 0.3(6) C19 C20 C21 C16 -0.1(6) C17 C16 C21 C20 0.0(5) C1 C16 C21 C20 173.7(3) C27 C22 C23 C24 0.5(5) B1 C22 C23 C24 -174.9(3) C22 C23 C24 C25 -1.0(6) C23 C24 C25 C26 0.8(6) C24 C25 C26 C27 -0.1(6) C25 C26 C27 C22 -0.4(6) C23 C22 C27 C26 0.2(5) B1 C22 C27 C26 175.5(3) C1 O1 B1 C5 6.7(5) C1 O1 B1 C22 -172.2(3) C4 C5 B1 O1 -46.2(5) C9 C5 B1 O1 132.4(4) C4 C5 B1 C22 132.6(4) C9 C5 B1 C22 -48.8(5) C27 C22 B1 O1 -12.0(5) C23 C22 B1 O1 163.1(3) C27 C22 B1 C5 169.1(3) C23 C22 B1 C5 -15.7(5) B2 O2 C28 C37 62.0(4) B2 O2 C28 C29 -62.3(4) B2 O2 C28 C43 177.1(3) O2 C28 C29 C30 65.1(4) C37 C28 C29 C30 -58.2(4) C43 C28 C29 C30 179.0(3) O2 C28 C29 C33 -113.9(3) C37 C28 C29 C33 122.8(3) C43 C28 C29 C33 0.0(4) C33 C29 C30 C31 -177.6(3) C28 C29 C30 C31 3.4(5) C33 C29 C30 C34 2.8(5) C28 C29 C30 C34 -176.2(3) C29 C30 C31 C32 -46.3(5) C34 C30 C31 C32 133.3(4) C29 C30 C31 C35 135.1(4) C34 C30 C31 C35 -45.3(4) C30 C31 C32 C36 -179.1(3) C35 C31 C32 C36 -0.5(5) C30 C31 C32 B2 2.3(5) C35 C31 C32 B2 -179.1(3) O2 C28 C37 C38 35.1(4) C29 C28 C37 C38 155.7(3) C43 C28 C37 C38 -77.9(4) O2 C28 C37 C42 -151.7(3) C29 C28 C37 C42 -31.2(4) C43 C28 C37 C42 95.2(4) C42 C37 C38 C39 -0.3(5) C28 C37 C38 C39 173.0(3) C37 C38 C39 C40 0.1(6) C38 C39 C40 C41 -0.1(6) C39 C40 C41 C42 0.3(6) C40 C41 C42 C37 -0.5(6) C38 C37 C42 C41 0.5(5) C28 C37 C42 C41 -172.8(4) O2 C28 C43 C48 14.9(4) C37 C28 C43 C48 133.2(3) C29 C28 C43 C48 -100.7(4) O2 C28 C43 C44 -163.6(3) C37 C28 C43 C44 -45.4(4) C29 C28 C43 C44 80.8(4) C48 C43 C44 C45 -0.1(6) C28 C43 C44 C45 178.4(4) C43 C44 C45 C46 -1.0(6) C44 C45 C46 C47 1.1(7) C45 C46 C47 C48 -0.1(7) C44 C43 C48 C47 1.1(6) C28 C43 C48 C47 -177.4(4) C46 C47 C48 C43 -1.0(6) C54 C49 C50 C51 -0.5(5) B2 C49 C50 C51 174.4(3) C49 C50 C51 C52 1.2(6) C50 C51 C52 C53 -0.9(6) C51 C52 C53 C54 -0.1(6) C52 C53 C54 C49 0.7(6) C50 C49 C54 C53 -0.4(5) B2 C49 C54 C53 -175.3(4) C28 O2 B2 C32 -7.0(5) C28 O2 B2 C49 172.2(3) C31 C32 B2 O2 45.2(5) C36 C32 B2 O2 -133.4(4) C31 C32 B2 C49 -133.9(4) C36 C32 B2 C49 47.6(5) C54 C49 B2 O2 12.3(5) C50 C49 B2 O2 -162.4(3) C54 C49 B2 C32 -168.6(3) C50 C49 B2 C32 16.8(5)