# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Haddon, Robert' 'Sarkar, Arindam' 'Pal, Sushanta' 'Itkis, Mikhail' 'Tham, Fook' _publ_contact_author_name 'Haddon, Robert' _publ_contact_author_email haddon@ucr.edu _publ_section_title ; Sulfur and Selenium Substituted Spiro-Biphenalenyl-Boron Neutral Radicals ; # Attachment '- rh171_0m.cif' data_rh171_0m _database_code_depnum_ccdc_archive 'CCDC 867315' #TrackingRef '- rh171_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67.06 H46.64 B2 F24 O5.26 S4' _chemical_formula_weight 1542.44 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.2914(14) _cell_length_b 21.5371(18) _cell_length_c 21.8259(18) _cell_angle_alpha 112.1825(15) _cell_angle_beta 98.9048(15) _cell_angle_gamma 108.7214(15) _cell_volume 6766.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9938 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.08 _exptl_crystal_description 'prism frag' _exptl_crystal_colour red _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3124 _exptl_absorpt_coefficient_mu 0.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8809 _exptl_absorpt_correction_T_max 0.9733 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 128000 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.73 _reflns_number_total 28725 _reflns_number_gt 19089 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+3.7839P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28725 _refine_ls_number_parameters 2180 _refine_ls_number_restraints 2156 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.1547(2) 0.58291(17) 0.23252(15) 0.0298(7) Uani 1 1 d . . . O1 O 0.06005(12) 0.54431(10) 0.20108(9) 0.0301(4) Uani 1 1 d . . . C1 C 0.02482(16) 0.49547(14) 0.13428(12) 0.0248(5) Uani 1 1 d . . . C2 C -0.06334(16) 0.44904(14) 0.10983(13) 0.0254(6) Uani 1 1 d . . . H2 H -0.0963 0.4528 0.1410 0.030 Uiso 1 1 calc R . . C3 C -0.10205(16) 0.39808(13) 0.04053(13) 0.0240(5) Uani 1 1 d . . . S3 S -0.21008(4) 0.33687(4) 0.00656(3) 0.02793(15) Uani 1 1 d . . . C3B C -0.24751(18) 0.35858(16) 0.08124(14) 0.0338(6) Uani 1 1 d . . . H3A H -0.2137 0.3521 0.1169 0.051 Uiso 1 1 calc R . . H3B H -0.3083 0.3257 0.0673 0.051 Uiso 1 1 calc R . . H3C H -0.2408 0.4098 0.1002 0.051 Uiso 1 1 calc R . . C3A C -0.05236(17) 0.39264(13) -0.00810(13) 0.0241(5) Uani 1 1 d . . . C4 C -0.08868(18) 0.34369(14) -0.07913(13) 0.0285(6) Uani 1 1 d . . . H4 H -0.1484 0.3123 -0.0974 0.034 Uiso 1 1 calc R . . C5 C -0.03907(19) 0.34026(15) -0.12319(14) 0.0339(7) Uani 1 1 d . . . H5 H -0.0649 0.3065 -0.1714 0.041 Uiso 1 1 calc R . . C6 C 0.04783(18) 0.38551(15) -0.09787(14) 0.0317(6) Uani 1 1 d . . . H6 H 0.0809 0.3822 -0.1289 0.038 Uiso 1 1 calc R . . C6A C 0.08794(17) 0.43610(14) -0.02732(13) 0.0273(6) Uani 1 1 d . . . C7 C 0.17877(18) 0.48581(15) 0.00204(14) 0.0302(6) Uani 1 1 d . . . S7 S 0.23943(5) 0.47535(5) -0.05460(4) 0.0439(2) Uani 1 1 d . . . C7B C 0.3472(2) 0.5422(2) -0.00104(18) 0.0648(12) Uani 1 1 d . . . H7A H 0.3484 0.5917 0.0173 0.097 Uiso 1 1 calc R . . H7B H 0.3862 0.5388 -0.0291 0.097 Uiso 1 1 calc R . . H7C H 0.3655 0.5323 0.0378 0.097 Uiso 1 1 calc R . . C8 C 0.21339(17) 0.53726(15) 0.07087(14) 0.0306(6) Uani 1 1 d . . . H8 H 0.2721 0.5711 0.0887 0.037 Uiso 1 1 calc R . . C9 C 0.16228(17) 0.54009(14) 0.11513(13) 0.0276(6) Uani 1 1 d . . . C9A C 0.07510(16) 0.49069(14) 0.08947(13) 0.0244(5) Uani 1 1 d . . . C9B C 0.03695(16) 0.43973(13) 0.01802(13) 0.0235(5) Uani 1 1 d . . . O9 O 0.19799(12) 0.58995(10) 0.18136(9) 0.0311(4) Uani 1 1 d . . . O11 O 0.17384(12) 0.65619(10) 0.28570(9) 0.0286(4) Uani 1 1 d . . . C11 C 0.21255(15) 0.67924(13) 0.35298(12) 0.0228(5) Uani 1 1 d . . . C12 C 0.23017(16) 0.75088(14) 0.39998(13) 0.0248(5) Uani 1 1 d . . . H12 H 0.2168 0.7825 0.3836 0.030 Uiso 1 1 calc R . . C13 C 0.26726(15) 0.77641(14) 0.47077(13) 0.0237(5) Uani 1 1 d . . . S13 S 0.29061(5) 0.86510(4) 0.53191(4) 0.03285(16) Uani 1 1 d . . . C13B C 0.2860(2) 0.91236(16) 0.47965(16) 0.0393(7) Uani 1 1 d . . . H13A H 0.3225 0.9045 0.4499 0.059 Uiso 1 1 calc R . . H13B H 0.3066 0.9652 0.5102 0.059 Uiso 1 1 calc R . . H13C H 0.2265 0.8931 0.4504 0.059 Uiso 1 1 calc R . . C13A C 0.28958(15) 0.72909(14) 0.49645(12) 0.0234(5) Uani 1 1 d . . . C14 C 0.32810(16) 0.75202(15) 0.56675(13) 0.0277(6) Uani 1 1 d . . . H14 H 0.3389 0.8000 0.6003 0.033 Uiso 1 1 calc R . . C15 C 0.35061(17) 0.70603(15) 0.58814(13) 0.0296(6) Uani 1 1 d . . . H15 H 0.3760 0.7226 0.6364 0.036 Uiso 1 1 calc R . . C16 C 0.33701(16) 0.63616(15) 0.54083(14) 0.0285(6) Uani 1 1 d . . . H16 H 0.3539 0.6056 0.5567 0.034 Uiso 1 1 calc R . . C16A C 0.29826(15) 0.61006(14) 0.46930(13) 0.0228(5) Uani 1 1 d . . . C17 C 0.28307(16) 0.53757(14) 0.41695(14) 0.0262(6) Uani 1 1 d . . . S17 S 0.31549(5) 0.48333(4) 0.44726(4) 0.03533(17) Uani 1 1 d . . . C17B C 0.2903(2) 0.40153(17) 0.36884(18) 0.0462(8) Uani 1 1 d . . . H17A H 0.2280 0.3771 0.3456 0.069 Uiso 1 1 calc R . . H17B H 0.3096 0.3681 0.3805 0.069 Uiso 1 1 calc R . . H17C H 0.3196 0.4148 0.3377 0.069 Uiso 1 1 calc R . . C18 C 0.24462(16) 0.51476(14) 0.34729(14) 0.0269(6) Uani 1 1 d . . . H18 H 0.2346 0.4671 0.3134 0.032 Uiso 1 1 calc R . . C19 C 0.22040(16) 0.56161(14) 0.32642(13) 0.0253(6) Uani 1 1 d . . . C19A C 0.23438(15) 0.63194(13) 0.37522(12) 0.0212(5) Uani 1 1 d . . . C19B C 0.27359(15) 0.65681(13) 0.44705(12) 0.0207(5) Uani 1 1 d . . . O19 O 0.18390(12) 0.53808(10) 0.25883(9) 0.0313(4) Uani 1 1 d . . . B2 B -0.0096(2) 0.37521(16) 0.25589(15) 0.0261(6) Uani 1 1 d . . . O21 O -0.08561(11) 0.30758(9) 0.20862(9) 0.0271(4) Uani 1 1 d . . . C21 C -0.09521(16) 0.27506(13) 0.14067(13) 0.0230(5) Uani 1 1 d . . . C22 C -0.17622(16) 0.22178(13) 0.09507(13) 0.0244(5) Uani 1 1 d . . . H22 H -0.2227 0.2085 0.1126 0.029 Uiso 1 1 calc R . . C23 C -0.18860(16) 0.18831(14) 0.02429(13) 0.0249(5) Uani 1 1 d U . . S23 S -0.28853(4) 0.12704(4) -0.03676(4) 0.03504(17) Uani 1 1 d U . . C23B C -0.35935(19) 0.12243(18) 0.01503(16) 0.0480(9) Uani 1 1 d U . . H23A H -0.3401 0.1063 0.0486 0.072 Uiso 1 1 calc R . . H23B H -0.4180 0.0873 -0.0154 0.072 Uiso 1 1 calc R . . H23C H -0.3586 0.1713 0.0401 0.072 Uiso 1 1 calc R . . C23A C -0.11701(17) 0.20427(14) -0.00296(13) 0.0249(5) Uani 1 1 d U . . C24 C -0.12556(18) 0.16847(15) -0.07393(13) 0.0317(6) Uani 1 1 d U . . H24 H -0.1803 0.1327 -0.1064 0.038 Uiso 1 1 calc R . . C25 C -0.05532(19) 0.18467(17) -0.09702(14) 0.0359(7) Uani 1 1 d U . . H25 H -0.0621 0.1597 -0.1452 0.043 Uiso 1 1 calc R . . C26 C 0.02519(19) 0.23699(16) -0.05074(14) 0.0323(6) Uani 1 1 d U . . H26 H 0.0728 0.2475 -0.0676 0.039 Uiso 1 1 calc R . . C26A C 0.03707(17) 0.27443(14) 0.02039(13) 0.0256(5) Uani 1 1 d U . . C27 C 0.11984(17) 0.32972(14) 0.07121(14) 0.0272(6) Uani 1 1 d U . . S27 S 0.20680(5) 0.34869(4) 0.03981(4) 0.03768(18) Uani 1 1 d U . . C27B C 0.2960(2) 0.4148(2) 0.11726(18) 0.0502(9) Uani 1 1 d U . . H27A H 0.2857 0.4589 0.1403 0.075 Uiso 1 1 calc R . . H27B H 0.3488 0.4285 0.1047 0.075 Uiso 1 1 calc R . . H27C H 0.3022 0.3933 0.1490 0.075 Uiso 1 1 calc R . . C28 C 0.12765(17) 0.36539(14) 0.14052(14) 0.0264(6) Uani 1 1 d U . . H28 H 0.1820 0.4017 0.1731 0.032 Uiso 1 1 calc R . . C29 C 0.05573(16) 0.34836(13) 0.16333(13) 0.0242(5) Uani 1 1 d U . . C29A C -0.02513(16) 0.29463(13) 0.11646(12) 0.0215(5) Uani 1 1 d U . . C29B C -0.03515(16) 0.25761(13) 0.04452(13) 0.0233(5) Uani 1 1 d U . . O29 O 0.06565(11) 0.38266(9) 0.23051(9) 0.0286(4) Uani 1 1 d U . . O31 O -0.03201(11) 0.43755(9) 0.26167(8) 0.0256(4) Uani 1 1 d U . . C31 C -0.00350(15) 0.49773(13) 0.32221(12) 0.0212(5) Uani 1 1 d U . . C32 C -0.01470(16) 0.56019(14) 0.32375(13) 0.0235(5) Uani 1 1 d U . . H32 H -0.0421 0.5588 0.2817 0.028 Uiso 1 1 calc R . . C33 C 0.01371(16) 0.62290(13) 0.38549(13) 0.0226(5) Uani 1 1 d U . . C33A C 0.05376(15) 0.62576(13) 0.45066(12) 0.0207(5) Uani 1 1 d U . . S33 S 0.00441(5) 0.70323(4) 0.39070(4) 0.03314(16) Uani 1 1 d U . . C33B C -0.0202(2) 0.68780(19) 0.30191(18) 0.0488(8) Uani 1 1 d U . . H33A H 0.0208 0.6718 0.2814 0.073 Uiso 1 1 calc R . . H33B H -0.0162 0.7336 0.3004 0.073 Uiso 1 1 calc R . . H33C H -0.0787 0.6495 0.2755 0.073 Uiso 1 1 calc R . . C34 C 0.08099(16) 0.68744(14) 0.51538(14) 0.0267(6) Uani 1 1 d U . . H34 H 0.0742 0.7302 0.5177 0.032 Uiso 1 1 calc R . . C35 C 0.11771(17) 0.68676(14) 0.57598(14) 0.0293(6) Uani 1 1 d U . . H35 H 0.1343 0.7285 0.6196 0.035 Uiso 1 1 calc R . . C36 C 0.13059(16) 0.62587(14) 0.57366(13) 0.0251(5) Uani 1 1 d U . . H36 H 0.1571 0.6269 0.6157 0.030 Uiso 1 1 calc R . . C36A C 0.10521(15) 0.56291(13) 0.51042(12) 0.0197(5) Uani 1 1 d U . . C37 C 0.11685(15) 0.49748(13) 0.50514(12) 0.0201(5) Uani 1 1 d U . . S37 S 0.17183(4) 0.50203(4) 0.58173(3) 0.02666(15) Uani 1 1 d U . . C37B C 0.17247(18) 0.41245(15) 0.55283(15) 0.0307(6) Uani 1 1 d U . . H37A H 0.1132 0.3747 0.5300 0.046 Uiso 1 1 calc R . . H37B H 0.1994 0.4080 0.5930 0.046 Uiso 1 1 calc R . . H37C H 0.2051 0.4058 0.5197 0.046 Uiso 1 1 calc R . . C38 C 0.08589(15) 0.43526(13) 0.44217(12) 0.0214(5) Uani 1 1 d U . . H38 H 0.0921 0.3922 0.4398 0.026 Uiso 1 1 calc R . . C39 C 0.04523(15) 0.43532(13) 0.38151(12) 0.0202(5) Uani 1 1 d U . . C39A C 0.03685(15) 0.49890(13) 0.38381(12) 0.0190(5) Uani 1 1 d U . . C39B C 0.06536(15) 0.56257(13) 0.44828(12) 0.0193(5) Uani 1 1 d U . . O39 O 0.01462(12) 0.37371(9) 0.32210(9) 0.0263(4) Uani 1 1 d U . . C1S C 0.4622(5) 0.3229(5) 0.1371(5) 0.161(4) Uani 0.846(5) 1 d PDU . . H1A H 0.5179 0.3204 0.1382 0.242 Uiso 0.846(5) 1 calc PR . . H1B H 0.4705 0.3746 0.1577 0.242 Uiso 0.846(5) 1 calc PR . . H1C H 0.4244 0.2971 0.0888 0.242 Uiso 0.846(5) 1 calc PR . . C2S C 0.4217(4) 0.2869(4) 0.1784(4) 0.115(2) Uani 0.846(5) 1 d PDU . . H2A H 0.4140 0.2349 0.1590 0.138 Uiso 0.846(5) 1 calc PR . . H2B H 0.4581 0.3133 0.2278 0.138 Uiso 0.846(5) 1 calc PR . . O3S O 0.3409(3) 0.2912(2) 0.1726(2) 0.1100(17) Uani 0.846(5) 1 d PDU . . C4S C 0.2953(4) 0.2543(3) 0.2051(3) 0.104(2) Uani 0.846(5) 1 d PDU . . H4A H 0.3261 0.2798 0.2558 0.124 Uiso 0.846(5) 1 calc PR . . H4B H 0.2913 0.2034 0.1862 0.124 Uiso 0.846(5) 1 calc PR . . C5S C 0.2061(4) 0.2524(3) 0.1930(3) 0.104(2) Uani 0.846(5) 1 d PDU . . H5A H 0.1767 0.2307 0.2196 0.157 Uiso 0.846(5) 1 calc PR . . H5B H 0.1736 0.2227 0.1432 0.157 Uiso 0.846(5) 1 calc PR . . H5C H 0.2102 0.3027 0.2083 0.157 Uiso 0.846(5) 1 calc PR . . C6S C 0.1651(5) 0.1460(3) 0.9706(4) 0.138(4) Uani 0.847(4) 1 d PDU . . H6A H 0.1789 0.1862 0.9575 0.207 Uiso 0.847(4) 1 calc PR . . H6B H 0.2181 0.1497 0.9985 0.207 Uiso 0.847(4) 1 calc PR . . H6C H 0.1255 0.1498 0.9981 0.207 Uiso 0.847(4) 1 calc PR . . C7S C 0.1240(3) 0.0741(2) 0.9067(3) 0.0685(14) Uani 0.847(4) 1 d PDU . . H7D H 0.0700 0.0696 0.8786 0.082 Uiso 0.847(4) 1 calc PR . . H7E H 0.1630 0.0704 0.8780 0.082 Uiso 0.847(4) 1 calc PR . . O8S O 0.10644(17) 0.01718(14) 0.92685(13) 0.0470(8) Uani 0.847(4) 1 d PDU . . C9S C 0.0650(3) -0.0532(2) 0.8681(2) 0.0571(12) Uani 0.847(4) 1 d PDU . . H9A H 0.1022 -0.0596 0.8382 0.069 Uiso 0.847(4) 1 calc PR . . H9B H 0.0103 -0.0582 0.8403 0.069 Uiso 0.847(4) 1 calc PR . . C10S C 0.0473(4) -0.1106(3) 0.8935(4) 0.115(3) Uani 0.847(4) 1 d PDU . . H10A H 0.0019 -0.1572 0.8566 0.173 Uiso 0.847(4) 1 calc PR . . H10B H 0.0286 -0.0944 0.9347 0.173 Uiso 0.847(4) 1 calc PR . . H10D H 0.0998 -0.1175 0.9056 0.173 Uiso 0.847(4) 1 calc PR . . C11S C 0.4102(4) 0.3412(4) 0.9808(3) 0.111(2) Uani 0.835(5) 1 d PDU . . H11A H 0.3677 0.3036 0.9875 0.167 Uiso 0.835(5) 1 calc PR . . H11B H 0.4200 0.3902 1.0155 0.167 Uiso 0.835(5) 1 calc PR . . H11C H 0.4644 0.3353 0.9862 0.167 Uiso 0.835(5) 1 calc PR . . C12S C 0.3774(3) 0.3327(3) 0.9089(3) 0.0863(17) Uani 0.835(5) 1 d PDU . . H12A H 0.3676 0.2833 0.8736 0.104 Uiso 0.835(5) 1 calc PR . . H12B H 0.3219 0.3374 0.9028 0.104 Uiso 0.835(5) 1 calc PR . . O13S O 0.4379(2) 0.38718(19) 0.89990(17) 0.0718(11) Uani 0.835(5) 1 d PDU . . C14S C 0.4132(3) 0.3778(3) 0.8320(2) 0.0762(16) Uani 0.835(5) 1 d PDU . . H14A H 0.3567 0.3800 0.8211 0.091 Uiso 0.835(5) 1 calc PR . . H14B H 0.4080 0.3292 0.7985 0.091 Uiso 0.835(5) 1 calc PR . . C15S C 0.4803(3) 0.4382(3) 0.8262(3) 0.0767(16) Uani 0.835(5) 1 d PDU . . H15A H 0.4629 0.4335 0.7791 0.115 Uiso 0.835(5) 1 calc PR . . H15B H 0.5355 0.4344 0.8352 0.115 Uiso 0.835(5) 1 calc PR . . H15C H 0.4862 0.4861 0.8604 0.115 Uiso 0.835(5) 1 calc PR . . B3 B 0.53566(17) 0.93773(15) 0.77013(14) 0.0191(5) Uani 1 1 d U . . C1C C 0.43762(15) 0.89173(12) 0.76721(12) 0.0190(5) Uani 1 1 d U . . C2C C 0.41802(15) 0.82645(13) 0.77361(12) 0.0204(5) Uani 1 1 d U . . H2C H 0.4632 0.8119 0.7826 0.024 Uiso 1 1 calc R . . C3C C 0.33545(16) 0.78206(13) 0.76743(12) 0.0211(5) Uani 1 1 d U . . F1C F 0.35812(11) 0.67341(9) 0.73675(9) 0.0381(4) Uani 1 1 d U . . F2C F 0.35374(13) 0.72655(9) 0.83985(8) 0.0477(5) Uani 1 1 d U . . F3C F 0.23768(10) 0.66770(9) 0.75298(11) 0.0467(5) Uani 1 1 d U . . C4C C 0.26795(15) 0.80211(13) 0.75568(12) 0.0211(5) Uani 1 1 d U . . H4C H 0.2117 0.7730 0.7528 0.025 Uiso 1 1 calc R . . C5C C 0.28503(15) 0.86586(13) 0.74821(12) 0.0213(5) Uani 1 1 d U . . F4C F 0.14095(10) 0.84837(10) 0.73833(11) 0.0468(5) Uani 1 1 d U . . F5C F 0.23428(11) 0.95912(9) 0.77474(10) 0.0475(5) Uani 1 1 d U . . F6C F 0.19385(12) 0.88046(11) 0.66780(9) 0.0501(5) Uani 1 1 d U . . C6C C 0.36778(15) 0.90926(13) 0.75320(12) 0.0201(5) Uani 1 1 d U . . H6D H 0.3770 0.9521 0.7469 0.024 Uiso 1 1 calc R . . C7C C 0.32113(16) 0.71301(14) 0.77393(13) 0.0253(5) Uani 1 1 d U . . C8C C 0.21369(17) 0.88875(14) 0.73316(14) 0.0283(6) Uani 1 1 d U . . C9C C 0.56159(15) 1.02475(13) 0.78917(12) 0.0199(5) Uani 1 1 d U . . C10C C 0.52810(15) 1.06984(13) 0.83101(12) 0.0223(5) Uani 1 1 d U . . H10C H 0.4848 1.0490 0.8482 0.027 Uiso 1 1 calc R . . C11C C 0.55655(16) 1.14463(14) 0.84815(13) 0.0249(5) Uani 1 1 d U . . C12C C 0.62019(16) 1.17771(13) 0.82477(13) 0.0245(5) Uani 1 1 d U . . H12C H 0.6392 1.2285 0.8363 0.029 Uiso 1 1 calc R . . C13C C 0.65520(15) 1.13463(13) 0.78408(12) 0.0209(5) Uani 1 1 d U . . C14C C 0.62660(15) 1.06006(13) 0.76742(12) 0.0203(5) Uani 1 1 d U . . H14C H 0.6524 1.0321 0.7401 0.024 Uiso 1 1 calc R . . C15C C 0.51993(19) 1.19115(15) 0.89334(15) 0.0354(7) Uani 1 1 d U . . F7C F 0.44159(11) 1.15408(10) 0.89129(9) 0.0469(5) Uani 1 1 d U . . F8C F 0.56705(14) 1.22611(14) 0.95993(11) 0.0921(10) Uani 1 1 d U . . F9C F 0.51513(19) 1.24323(13) 0.87637(16) 0.0901(9) Uani 1 1 d U . . C16C C 0.72184(17) 1.16566(14) 0.75494(13) 0.0263(6) Uani 1 1 d U . . F10C F 0.75146(10) 1.23902(8) 0.78056(8) 0.0368(4) Uani 1 1 d U . . F11C F 0.69152(11) 1.13817(9) 0.68564(8) 0.0449(5) Uani 1 1 d U . . F12C F 0.79089(11) 1.15139(10) 0.76791(10) 0.0459(5) Uani 1 1 d U . . C17C C 0.54098(14) 0.89232(13) 0.69208(12) 0.0196(5) Uani 1 1 d U . . C18C C 0.56120(16) 0.83133(13) 0.67527(13) 0.0236(5) Uani 1 1 d U A . H18C H 0.5737 0.8167 0.7103 0.028 Uiso 1 1 calc R . . C19C C 0.56361(17) 0.79111(13) 0.60881(14) 0.0284(6) Uani 1 1 d DU . . C20C C 0.54826(17) 0.81157(14) 0.55701(14) 0.0287(6) Uani 1 1 d U A . H20C H 0.5517 0.7851 0.5122 0.034 Uiso 1 1 calc R . . C21C C 0.52771(16) 0.87176(14) 0.57180(13) 0.0239(5) Uani 1 1 d U . . C22C C 0.52285(15) 0.91051(13) 0.63774(12) 0.0212(5) Uani 1 1 d U A . H22C H 0.5068 0.9505 0.6461 0.025 Uiso 1 1 calc R . . C23C C 0.5779(5) 0.7220(3) 0.5889(4) 0.0351(17) Uani 0.625(18) 1 d PDU A 1 F13C F 0.5451(4) 0.6836(4) 0.6212(3) 0.0348(16) Uani 0.625(18) 1 d PDU A 1 F14C F 0.5431(8) 0.6761(3) 0.5211(3) 0.072(2) Uani 0.625(18) 1 d PDU A 1 F15C F 0.6608(4) 0.7385(4) 0.6042(7) 0.077(3) Uani 0.625(18) 1 d PDU A 1 C23D C 0.5996(8) 0.7351(6) 0.6049(6) 0.031(3) Uani 0.375(18) 1 d PDU A 2 F13D F 0.5468(8) 0.6814(8) 0.6150(6) 0.072(4) Uani 0.375(18) 1 d PDU A 2 F14D F 0.6060(14) 0.6992(7) 0.5426(7) 0.072(5) Uani 0.375(18) 1 d PDU A 2 F15D F 0.6758(5) 0.7553(5) 0.6493(8) 0.064(3) Uani 0.375(18) 1 d PDU A 2 C24C C 0.51410(18) 0.89558(16) 0.51642(14) 0.0319(6) Uani 1 1 d U A . F16C F 0.44708(10) 0.84332(10) 0.45952(8) 0.0435(4) Uani 1 1 d U . . F17C F 0.58239(10) 0.90926(10) 0.49335(9) 0.0431(4) Uani 1 1 d U . . F18C F 0.49958(12) 0.95624(10) 0.53740(9) 0.0444(4) Uani 1 1 d U . . C25C C 0.60756(16) 0.93998(13) 0.83114(13) 0.0220(5) Uani 1 1 d U . . C26C C 0.59281(17) 0.93760(15) 0.89164(13) 0.0282(6) Uani 1 1 d U B . H26C H 0.5375 0.9307 0.8967 0.034 Uiso 1 1 calc R . . C27C C 0.65717(19) 0.94516(17) 0.94490(15) 0.0371(7) Uani 1 1 d DU . . C28C C 0.7386(2) 0.95535(18) 0.93998(16) 0.0416(7) Uani 1 1 d U B . H28C H 0.7822 0.9602 0.9761 0.050 Uiso 1 1 calc R . . C29C C 0.75469(18) 0.95828(16) 0.88107(16) 0.0352(6) Uani 1 1 d DU . . C30C C 0.69057(16) 0.95046(14) 0.82762(14) 0.0274(6) Uani 1 1 d U B . H30C H 0.7038 0.9523 0.7875 0.033 Uiso 1 1 calc R . . C31C C 0.6446(5) 0.9459(4) 1.0116(3) 0.052(2) Uani 0.596(12) 1 d PDU B 1 F19C F 0.5683(4) 0.9447(5) 1.0151(5) 0.066(2) Uani 0.596(12) 1 d PDU B 1 F20C F 0.6486(7) 0.8869(5) 1.0142(4) 0.098(3) Uani 0.596(12) 1 d PDU B 1 F21C F 0.7031(3) 1.0047(5) 1.0677(2) 0.088(2) Uani 0.596(12) 1 d PDU B 1 C31D C 0.6250(7) 0.9302(6) 1.0005(5) 0.055(3) Uani 0.404(12) 1 d PDU B 2 F19D F 0.5822(8) 0.9693(7) 1.0289(9) 0.079(4) Uani 0.404(12) 1 d PDU B 2 F20D F 0.5710(10) 0.8617(4) 0.9833(4) 0.105(5) Uani 0.404(12) 1 d PDU B 2 F21D F 0.6879(6) 0.9469(10) 1.0551(5) 0.106(5) Uani 0.404(12) 1 d PDU B 2 C32C C 0.8462(4) 0.9755(5) 0.8801(6) 0.043(3) Uani 0.426(4) 1 d PDU B 1 F22C F 0.8637(6) 0.9182(5) 0.8750(7) 0.074(3) Uani 0.426(4) 1 d PDU B 1 F23C F 0.9059(5) 1.0343(4) 0.9366(4) 0.0496(18) Uani 0.426(4) 1 d PDU B 1 F24C F 0.8580(16) 0.9860(7) 0.8251(5) 0.066(4) Uani 0.426(4) 1 d PDU B 1 C32D C 0.8381(6) 0.9579(6) 0.8691(6) 0.043(3) Uani 0.273(10) 1 d PDU B 2 F22D F 0.8300(9) 0.9153(7) 0.8037(4) 0.048(3) Uani 0.273(10) 1 d PDU B 2 F23D F 0.8801(11) 0.9386(9) 0.9095(5) 0.046(3) Uani 0.273(10) 1 d PDU B 2 F24D F 0.8880(7) 1.0265(5) 0.8841(11) 0.087(6) Uani 0.273(10) 1 d PDU B 2 C32E C 0.8386(5) 0.9658(7) 0.8657(7) 0.045(3) Uani 0.301(11) 1 d PDU B 3 F22E F 0.8415(9) 0.9027(7) 0.8252(10) 0.087(6) Uani 0.301(11) 1 d PDU B 3 F23E F 0.9042(6) 0.9955(10) 0.9236(6) 0.069(5) Uani 0.301(11) 1 d PDU B 3 F24E F 0.863(2) 1.0080(10) 0.8345(9) 0.052(4) Uani 0.301(11) 1 d PDU B 3 B4 B 0.25708(18) 0.23763(15) 0.59728(14) 0.0198(6) Uani 1 1 d . . . C1F C 0.33341(16) 0.21795(13) 0.63051(12) 0.0208(5) Uani 1 1 d . . . C2F C 0.31280(16) 0.15216(13) 0.63579(12) 0.0224(5) Uani 1 1 d . . . H2F H 0.2542 0.1184 0.6193 0.027 Uiso 1 1 calc R . . C3F C 0.37530(17) 0.13458(14) 0.66437(13) 0.0262(6) Uani 1 1 d . . . C4F C 0.46190(18) 0.18164(15) 0.68810(14) 0.0313(6) Uani 1 1 d . . . H4F H 0.5047 0.1695 0.7072 0.038 Uiso 1 1 calc R . . C5F C 0.48403(17) 0.24676(16) 0.68303(15) 0.0320(6) Uani 1 1 d . . . C6F C 0.42105(16) 0.26444(15) 0.65483(14) 0.0279(6) Uani 1 1 d . . . H6F H 0.4383 0.3096 0.6521 0.034 Uiso 1 1 calc R . . C7F C 0.3498(2) 0.06586(15) 0.67355(15) 0.0351(7) Uani 1 1 d . . . F1F F 0.27147(11) 0.01494(9) 0.63133(9) 0.0425(4) Uani 1 1 d . . . F2F F 0.35041(15) 0.07966(10) 0.73836(9) 0.0590(6) Uani 1 1 d . . . F3F F 0.40408(13) 0.03339(10) 0.66081(11) 0.0563(5) Uani 1 1 d . . . C8F C 0.5766(2) 0.3001(2) 0.7127(2) 0.0514(9) Uani 1 1 d . . . F4F F 0.60208(14) 0.33418(15) 0.78296(13) 0.0955(9) Uani 1 1 d . . . F5F F 0.62956(12) 0.26811(13) 0.69718(12) 0.0678(6) Uani 1 1 d . . . F6F F 0.59421(14) 0.35146(17) 0.6935(2) 0.1274(14) Uani 1 1 d . . . C9F C 0.23100(14) 0.20084(13) 0.51230(12) 0.0196(5) Uani 1 1 d . . . C10F C 0.24096(15) 0.13720(13) 0.47183(13) 0.0197(5) Uani 1 1 d . . . H10F H 0.2735 0.1192 0.4942 0.024 Uiso 1 1 calc R . . C11F C 0.20403(15) 0.09970(13) 0.39930(13) 0.0209(5) Uani 1 1 d . . . C12F C 0.15651(16) 0.12438(14) 0.36470(13) 0.0254(5) Uani 1 1 d . . . H12F H 0.1309 0.0985 0.3155 0.030 Uiso 1 1 calc R . . C13F C 0.14725(16) 0.18774(14) 0.40359(13) 0.0248(5) Uani 1 1 d . . . C14F C 0.18470(16) 0.22511(13) 0.47566(13) 0.0233(5) Uani 1 1 d . . . H14F H 0.1784 0.2691 0.5010 0.028 Uiso 1 1 calc R . . C15F C 0.21438(16) 0.03159(14) 0.35680(13) 0.0249(5) Uani 1 1 d . . . F7F F 0.25082(12) 0.00616(9) 0.39482(8) 0.0404(4) Uani 1 1 d . . . F8F F 0.13886(10) -0.02417(8) 0.31264(9) 0.0378(4) Uani 1 1 d . . . F9F F 0.26341(10) 0.04230(9) 0.31647(8) 0.0371(4) Uani 1 1 d . . . C16F C 0.0950(2) 0.21593(16) 0.36932(15) 0.0355(7) Uani 1 1 d . . . F10F F 0.03167(13) 0.22294(14) 0.39607(12) 0.0655(6) Uani 1 1 d . . . F11F F 0.05901(17) 0.17514(13) 0.30185(10) 0.0815(8) Uani 1 1 d . . . F12F F 0.14058(14) 0.28471(11) 0.38095(12) 0.0620(6) Uani 1 1 d . . . C17F C 0.29227(15) 0.32794(13) 0.63114(12) 0.0202(5) Uani 1 1 d . . . C18F C 0.35222(16) 0.36768(13) 0.60807(13) 0.0239(5) Uani 1 1 d . . . H18F H 0.3677 0.3411 0.5698 0.029 Uiso 1 1 calc R . . C19F C 0.38990(17) 0.44441(14) 0.63899(14) 0.0292(6) Uani 1 1 d . . . C20F C 0.36722(19) 0.48516(14) 0.69349(14) 0.0320(6) Uani 1 1 d . C . H20F H 0.3929 0.5375 0.7149 0.038 Uiso 1 1 calc R . . C21F C 0.30633(18) 0.44802(14) 0.71615(13) 0.0288(6) Uani 1 1 d D . . C22F C 0.26995(17) 0.37080(13) 0.68591(13) 0.0240(5) Uani 1 1 d . C . H22F H 0.2289 0.3468 0.7030 0.029 Uiso 1 1 calc R . . C23F C 0.4584(2) 0.48341(16) 0.61601(17) 0.0440(8) Uani 1 1 d . . . F13F F 0.53213(15) 0.4804(2) 0.63855(18) 0.1221(13) Uani 1 1 d . . . F14F F 0.44124(14) 0.45314(11) 0.54764(11) 0.0603(6) Uani 1 1 d . . . F15F F 0.4716(2) 0.55182(12) 0.63425(17) 0.1252(14) Uani 1 1 d . . . C24F C 0.2763(7) 0.4882(5) 0.7733(4) 0.032(3) Uani 0.477(3) 1 d PDU C 1 F16F F 0.2619(8) 0.5440(5) 0.7685(5) 0.079(4) Uani 0.477(3) 1 d PDU C 1 F17F F 0.3359(7) 0.5206(7) 0.8354(7) 0.053(4) Uani 0.477(3) 1 d PDU C 1 F18F F 0.2047(5) 0.4494(6) 0.7811(6) 0.0381(19) Uani 0.477(3) 1 d PDU C 1 C24G C 0.2938(10) 0.4972(7) 0.7796(6) 0.035(6) Uani 0.166(10) 1 d PDU C 2 F16G F 0.3460(15) 0.5680(8) 0.8086(13) 0.059(6) Uani 0.166(10) 1 d PDU C 2 F17G F 0.302(2) 0.4738(13) 0.8271(10) 0.065(6) Uani 0.166(10) 1 d PDU C 2 F18G F 0.2140(10) 0.4906(15) 0.7606(11) 0.075(8) Uani 0.166(10) 1 d PDU C 2 C24H C 0.2798(8) 0.4936(6) 0.7721(6) 0.044(5) Uani 0.357(10) 1 d PDU C 3 F16H F 0.3466(9) 0.5449(10) 0.8281(9) 0.061(6) Uani 0.357(10) 1 d PDU C 3 F17H F 0.2325(11) 0.4535(7) 0.7971(8) 0.068(6) Uani 0.357(10) 1 d PDU C 3 F18H F 0.2366(11) 0.5253(8) 0.7482(7) 0.062(4) Uani 0.357(10) 1 d PDU C 3 C25F C 0.17018(16) 0.20024(13) 0.61583(14) 0.0232(5) Uani 1 1 d U . . C26F C 0.17378(18) 0.20874(14) 0.68327(14) 0.0278(6) Uani 1 1 d U D . H26F H 0.2269 0.2395 0.7199 0.033 Uiso 1 1 calc R . . C27F C 0.1014(2) 0.17318(16) 0.69830(16) 0.0351(6) Uani 1 1 d DU . . C28F C 0.02287(19) 0.12693(16) 0.64554(17) 0.0385(7) Uani 1 1 d U D . H28F H -0.0261 0.1019 0.6553 0.046 Uiso 1 1 calc R . . C29F C 0.01775(17) 0.11825(15) 0.57895(16) 0.0321(6) Uani 1 1 d U . . C30F C 0.08966(16) 0.15435(14) 0.56450(14) 0.0264(6) Uani 1 1 d U D . H30F H 0.0840 0.1477 0.5182 0.032 Uiso 1 1 calc R . . C31F C 0.1134(6) 0.1871(5) 0.7722(3) 0.046(2) Uani 0.584(4) 1 d PDU D 1 F19F F 0.1821(6) 0.1796(5) 0.8004(4) 0.064(2) Uani 0.584(4) 1 d PDU D 1 F20F F 0.1246(6) 0.2556(4) 0.8140(4) 0.062(2) Uani 0.584(4) 1 d PDU D 1 F21F F 0.0468(6) 0.1413(5) 0.7801(7) 0.075(3) Uani 0.584(4) 1 d PDU D 1 C31G C 0.1053(10) 0.1841(8) 0.7703(4) 0.051(4) Uani 0.290(8) 1 d PDU D 2 F19G F 0.1829(9) 0.2082(10) 0.8135(9) 0.073(6) Uani 0.290(8) 1 d PDU D 2 F20G F 0.0756(11) 0.2337(9) 0.7998(7) 0.076(5) Uani 0.290(8) 1 d PDU D 2 F21G F 0.0570(12) 0.1235(8) 0.7719(12) 0.067(5) Uani 0.290(8) 1 d PDU D 2 C31H C 0.096(4) 0.183(3) 0.7687(15) 0.056(6) Uani 0.126(7) 1 d PDU D 3 F19H F 0.163(2) 0.2615(19) 0.8309(15) 0.076(9) Uani 0.126(7) 1 d PU D 3 F20H F 0.0147(15) 0.1842(16) 0.7716(11) 0.073(7) Uani 0.126(7) 1 d PU D 3 F21H F 0.107(3) 0.1492(19) 0.7937(18) 0.120(10) Uani 0.126(7) 1 d PU D 3 C32F C -0.06488(18) 0.06937(16) 0.51910(18) 0.0417(7) Uani 1 1 d U D . F22F F -0.10018(12) 0.10846(11) 0.49996(11) 0.0574(5) Uani 1 1 d U . . F23F F -0.12356(13) 0.02480(12) 0.53436(12) 0.0662(6) Uani 1 1 d U . . F24F F -0.05390(12) 0.02595(11) 0.46165(10) 0.0551(5) Uani 1 1 d 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 B1 0.0282(16) 0.0278(16) 0.0192(15) 0.0098(12) 0.0002(12) -0.0005(13) O1 0.0278(10) 0.0314(10) 0.0133(9) 0.0059(8) 0.0010(7) -0.0010(8) C1 0.0273(14) 0.0256(13) 0.0152(12) 0.0096(10) 0.0026(10) 0.0050(11) C2 0.0252(13) 0.0261(13) 0.0206(13) 0.0117(11) 0.0059(11) 0.0050(11) C3 0.0253(13) 0.0206(12) 0.0195(12) 0.0086(10) 0.0041(10) 0.0037(10) S3 0.0248(3) 0.0249(3) 0.0199(3) 0.0051(3) 0.0034(3) 0.0015(3) C3B 0.0292(15) 0.0326(15) 0.0278(15) 0.0093(12) 0.0104(12) 0.0038(12) C3A 0.0286(14) 0.0219(12) 0.0187(12) 0.0105(10) 0.0050(10) 0.0064(11) C4 0.0297(14) 0.0278(14) 0.0183(13) 0.0083(11) 0.0030(11) 0.0052(11) C5 0.0419(17) 0.0300(14) 0.0176(13) 0.0055(11) 0.0080(12) 0.0076(13) C6 0.0378(16) 0.0348(15) 0.0219(13) 0.0134(12) 0.0125(12) 0.0124(13) C6A 0.0323(15) 0.0281(14) 0.0204(13) 0.0137(11) 0.0081(11) 0.0080(12) C7 0.0311(15) 0.0348(15) 0.0251(14) 0.0186(12) 0.0100(12) 0.0077(12) S7 0.0375(4) 0.0564(5) 0.0304(4) 0.0201(4) 0.0160(3) 0.0078(4) C7B 0.0352(19) 0.098(3) 0.041(2) 0.030(2) 0.0157(16) 0.0034(19) C8 0.0250(14) 0.0346(15) 0.0258(14) 0.0171(12) 0.0047(11) 0.0023(12) C9 0.0281(14) 0.0298(14) 0.0207(13) 0.0151(11) 0.0027(11) 0.0050(11) C9A 0.0251(13) 0.0267(13) 0.0185(12) 0.0133(11) 0.0027(10) 0.0055(11) C9B 0.0281(14) 0.0230(12) 0.0179(12) 0.0114(10) 0.0054(10) 0.0071(11) O9 0.0273(10) 0.0329(10) 0.0168(9) 0.0087(8) 0.0005(8) -0.0007(8) O11 0.0308(10) 0.0262(9) 0.0157(9) 0.0095(7) -0.0027(7) 0.0010(8) C11 0.0170(12) 0.0253(13) 0.0171(12) 0.0096(10) 0.0033(10) -0.0008(10) C12 0.0210(13) 0.0251(13) 0.0234(13) 0.0118(11) 0.0044(10) 0.0040(10) C13 0.0176(12) 0.0238(13) 0.0220(13) 0.0079(10) 0.0069(10) 0.0023(10) S13 0.0401(4) 0.0281(4) 0.0256(3) 0.0083(3) 0.0131(3) 0.0120(3) C13B 0.0520(19) 0.0324(16) 0.0346(16) 0.0145(13) 0.0168(14) 0.0183(14) C13A 0.0191(12) 0.0256(13) 0.0171(12) 0.0082(10) 0.0067(10) 0.0009(10) C14 0.0221(13) 0.0316(14) 0.0188(13) 0.0085(11) 0.0067(10) 0.0021(11) C15 0.0228(13) 0.0391(16) 0.0174(13) 0.0138(12) 0.0028(10) 0.0023(12) C16 0.0218(13) 0.0372(15) 0.0272(14) 0.0206(12) 0.0062(11) 0.0066(11) C16A 0.0147(12) 0.0278(13) 0.0211(12) 0.0121(11) 0.0052(10) 0.0024(10) C17 0.0184(12) 0.0298(14) 0.0312(14) 0.0183(12) 0.0080(11) 0.0056(11) S17 0.0322(4) 0.0382(4) 0.0439(4) 0.0252(3) 0.0130(3) 0.0161(3) C17B 0.053(2) 0.0326(16) 0.060(2) 0.0228(16) 0.0225(17) 0.0212(15) C18 0.0231(13) 0.0224(13) 0.0281(14) 0.0102(11) 0.0074(11) 0.0030(11) C19 0.0203(13) 0.0249(13) 0.0194(13) 0.0088(10) 0.0030(10) -0.0009(10) C19A 0.0176(12) 0.0220(12) 0.0176(12) 0.0095(10) 0.0042(10) 0.0009(10) C19B 0.0147(11) 0.0257(13) 0.0163(12) 0.0102(10) 0.0041(9) 0.0016(10) O19 0.0360(11) 0.0230(9) 0.0164(9) 0.0041(7) -0.0003(8) 0.0003(8) B2 0.0305(16) 0.0215(14) 0.0161(14) 0.0022(11) 0.0063(12) 0.0069(12) O21 0.0269(10) 0.0255(9) 0.0174(9) 0.0032(7) 0.0081(7) 0.0048(8) C21 0.0271(13) 0.0198(12) 0.0186(12) 0.0060(10) 0.0074(10) 0.0089(10) C22 0.0231(13) 0.0230(13) 0.0230(13) 0.0079(10) 0.0099(11) 0.0064(10) C23 0.0237(13) 0.0222(12) 0.0219(13) 0.0058(10) 0.0048(10) 0.0079(10) S23 0.0254(4) 0.0349(4) 0.0233(3) 0.0020(3) 0.0023(3) 0.0032(3) C23B 0.0263(16) 0.0463(19) 0.0365(17) -0.0009(14) 0.0071(13) -0.0012(14) C23A 0.0277(13) 0.0228(13) 0.0205(12) 0.0070(10) 0.0077(10) 0.0095(11) C24 0.0344(15) 0.0337(15) 0.0188(13) 0.0065(11) 0.0056(11) 0.0122(12) C25 0.0416(17) 0.0445(17) 0.0194(13) 0.0114(12) 0.0124(12) 0.0177(14) C26 0.0354(15) 0.0380(16) 0.0266(14) 0.0142(12) 0.0165(12) 0.0162(13) C26A 0.0267(13) 0.0260(13) 0.0231(13) 0.0107(11) 0.0092(11) 0.0097(11) C27 0.0278(14) 0.0269(13) 0.0307(14) 0.0146(11) 0.0128(11) 0.0123(11) S27 0.0306(4) 0.0423(4) 0.0395(4) 0.0179(3) 0.0187(3) 0.0119(3) C27B 0.0300(17) 0.057(2) 0.052(2) 0.0196(17) 0.0165(15) 0.0091(15) C28 0.0227(13) 0.0223(13) 0.0272(13) 0.0080(11) 0.0074(11) 0.0052(10) C29 0.0269(13) 0.0218(12) 0.0203(12) 0.0068(10) 0.0072(10) 0.0092(11) C29A 0.0246(13) 0.0194(12) 0.0177(12) 0.0069(10) 0.0067(10) 0.0078(10) C29B 0.0249(13) 0.0220(12) 0.0218(12) 0.0090(10) 0.0084(10) 0.0094(10) O29 0.0268(10) 0.0245(9) 0.0185(9) 0.0002(7) 0.0059(7) 0.0037(8) O31 0.0306(10) 0.0253(9) 0.0145(8) 0.0063(7) 0.0044(7) 0.0086(8) C31 0.0198(12) 0.0235(12) 0.0165(12) 0.0076(10) 0.0074(10) 0.0056(10) C32 0.0225(13) 0.0293(13) 0.0210(12) 0.0143(11) 0.0059(10) 0.0105(11) C33 0.0204(12) 0.0249(13) 0.0278(13) 0.0149(11) 0.0111(10) 0.0104(10) C33A 0.0160(12) 0.0214(12) 0.0216(12) 0.0090(10) 0.0048(10) 0.0059(10) S33 0.0393(4) 0.0292(4) 0.0377(4) 0.0178(3) 0.0120(3) 0.0192(3) C33B 0.065(2) 0.0483(19) 0.050(2) 0.0331(17) 0.0164(17) 0.0316(18) C34 0.0236(13) 0.0189(12) 0.0299(14) 0.0055(11) 0.0065(11) 0.0075(10) C35 0.0269(14) 0.0226(13) 0.0222(13) 0.0004(11) 0.0031(11) 0.0052(11) C36 0.0200(13) 0.0258(13) 0.0182(12) 0.0053(10) 0.0009(10) 0.0043(10) C36A 0.0152(11) 0.0219(12) 0.0189(12) 0.0077(10) 0.0060(9) 0.0057(10) C37 0.0163(12) 0.0270(13) 0.0187(12) 0.0126(10) 0.0060(9) 0.0081(10) S37 0.0257(3) 0.0320(3) 0.0211(3) 0.0132(3) 0.0033(3) 0.0111(3) C37B 0.0309(15) 0.0378(15) 0.0332(15) 0.0227(13) 0.0098(12) 0.0180(13) C38 0.0226(13) 0.0225(12) 0.0213(12) 0.0107(10) 0.0078(10) 0.0106(10) C39 0.0188(12) 0.0211(12) 0.0177(12) 0.0067(10) 0.0080(10) 0.0063(10) C39A 0.0179(12) 0.0203(12) 0.0173(11) 0.0077(9) 0.0067(9) 0.0069(10) C39B 0.0152(11) 0.0211(12) 0.0184(12) 0.0074(10) 0.0065(9) 0.0051(9) O39 0.0348(10) 0.0208(9) 0.0182(9) 0.0043(7) 0.0070(8) 0.0115(8) C1S 0.104(6) 0.159(8) 0.244(12) 0.127(8) 0.018(6) 0.056(6) C2S 0.085(4) 0.088(5) 0.144(6) 0.053(4) -0.017(4) 0.026(4) O3S 0.096(3) 0.072(3) 0.128(4) 0.054(3) -0.031(2) 0.015(2) C4S 0.148(5) 0.052(3) 0.094(5) 0.024(3) 0.011(4) 0.046(4) C5S 0.157(5) 0.060(3) 0.091(4) 0.031(3) 0.002(4) 0.060(4) C6S 0.109(5) 0.042(3) 0.192(8) 0.022(4) -0.039(5) 0.026(3) C7S 0.052(3) 0.070(3) 0.092(4) 0.052(3) 0.007(3) 0.025(2) O8S 0.0522(17) 0.0425(15) 0.0413(15) 0.0171(12) 0.0001(12) 0.0231(13) C9S 0.040(2) 0.049(2) 0.061(3) 0.003(2) 0.009(2) 0.0233(19) C10S 0.083(4) 0.050(3) 0.185(7) 0.052(4) -0.019(4) 0.023(3) C11S 0.086(5) 0.139(6) 0.107(5) 0.045(5) 0.065(4) 0.043(4) C12S 0.057(3) 0.092(4) 0.094(4) 0.025(3) 0.029(3) 0.031(3) O13S 0.0452(19) 0.081(2) 0.059(2) 0.0072(17) 0.0093(15) 0.0242(17) C14S 0.062(3) 0.076(3) 0.054(3) 0.008(3) -0.009(2) 0.024(3) C15S 0.050(3) 0.073(3) 0.070(3) 0.014(3) -0.011(2) 0.017(2) B3 0.0190(13) 0.0194(13) 0.0181(13) 0.0087(11) 0.0063(11) 0.0068(11) C1C 0.0199(12) 0.0181(11) 0.0132(11) 0.0049(9) 0.0052(9) 0.0036(9) C2C 0.0207(12) 0.0218(12) 0.0162(11) 0.0071(10) 0.0065(10) 0.0075(10) C3C 0.0245(13) 0.0189(12) 0.0143(11) 0.0060(9) 0.0072(10) 0.0037(10) F1C 0.0515(11) 0.0317(9) 0.0473(10) 0.0237(8) 0.0300(9) 0.0227(8) F2C 0.0786(14) 0.0354(9) 0.0273(9) 0.0200(8) 0.0127(9) 0.0163(9) F3C 0.0278(9) 0.0304(9) 0.0837(14) 0.0335(9) 0.0180(9) 0.0050(7) C4C 0.0187(12) 0.0217(12) 0.0161(12) 0.0068(10) 0.0056(10) 0.0027(10) C5C 0.0179(12) 0.0211(12) 0.0177(12) 0.0050(10) 0.0052(10) 0.0044(10) F4C 0.0226(9) 0.0494(11) 0.0771(13) 0.0359(10) 0.0207(9) 0.0146(8) F5C 0.0332(9) 0.0287(9) 0.0636(12) 0.0050(8) 0.0071(8) 0.0159(8) F6C 0.0473(11) 0.0732(13) 0.0407(10) 0.0303(10) 0.0080(8) 0.0354(10) C6C 0.0212(12) 0.0163(11) 0.0170(12) 0.0060(9) 0.0050(10) 0.0034(9) C7C 0.0259(13) 0.0252(13) 0.0244(13) 0.0117(11) 0.0114(11) 0.0078(11) C8C 0.0214(13) 0.0248(13) 0.0330(15) 0.0109(11) 0.0094(11) 0.0051(11) C9C 0.0171(12) 0.0214(12) 0.0146(11) 0.0068(9) 0.0003(9) 0.0039(10) C10C 0.0185(12) 0.0232(12) 0.0183(12) 0.0070(10) 0.0041(10) 0.0041(10) C11C 0.0221(13) 0.0221(12) 0.0199(12) 0.0036(10) 0.0031(10) 0.0056(10) C12C 0.0256(13) 0.0174(12) 0.0217(13) 0.0054(10) 0.0027(10) 0.0049(10) C13C 0.0177(12) 0.0215(12) 0.0149(11) 0.0067(10) -0.0002(9) 0.0021(10) C14C 0.0177(12) 0.0219(12) 0.0157(11) 0.0063(10) 0.0031(9) 0.0054(10) C15C 0.0324(16) 0.0270(14) 0.0349(16) 0.0053(12) 0.0113(13) 0.0087(12) F7C 0.0385(10) 0.0415(10) 0.0479(11) 0.0060(8) 0.0227(8) 0.0145(8) F8C 0.0549(13) 0.1048(19) 0.0417(12) -0.0376(12) -0.0042(10) 0.0393(13) F9C 0.143(2) 0.0671(15) 0.140(2) 0.0699(16) 0.110(2) 0.0802(17) C16C 0.0267(14) 0.0224(13) 0.0206(13) 0.0085(10) 0.0035(10) 0.0028(11) F10C 0.0401(9) 0.0229(8) 0.0333(9) 0.0120(7) 0.0093(7) -0.0016(7) F11C 0.0479(11) 0.0423(10) 0.0194(8) 0.0099(7) 0.0084(7) -0.0050(8) F12C 0.0305(9) 0.0567(11) 0.0704(13) 0.0451(10) 0.0264(9) 0.0173(8) C17C 0.0134(11) 0.0192(11) 0.0211(12) 0.0091(10) 0.0050(9) 0.0012(9) C18C 0.0245(13) 0.0217(12) 0.0263(13) 0.0133(11) 0.0117(11) 0.0072(10) C19C 0.0311(14) 0.0172(12) 0.0372(15) 0.0110(11) 0.0213(12) 0.0072(11) C20C 0.0282(14) 0.0239(13) 0.0235(13) 0.0051(11) 0.0138(11) 0.0027(11) C21C 0.0188(12) 0.0258(13) 0.0198(12) 0.0089(10) 0.0071(10) 0.0019(10) C22C 0.0165(12) 0.0196(12) 0.0223(12) 0.0083(10) 0.0064(10) 0.0024(10) C23C 0.036(3) 0.018(3) 0.044(4) 0.007(3) 0.021(3) 0.007(3) F13C 0.041(3) 0.026(3) 0.038(3) 0.018(2) 0.014(2) 0.011(2) F14C 0.130(7) 0.048(2) 0.048(2) 0.0128(19) 0.037(3) 0.053(3) F15C 0.041(3) 0.049(4) 0.173(9) 0.063(5) 0.060(4) 0.029(3) C23D 0.045(7) 0.015(4) 0.030(5) 0.007(4) 0.023(5) 0.007(4) F13D 0.084(7) 0.050(7) 0.141(10) 0.070(7) 0.086(7) 0.042(6) F14D 0.156(14) 0.066(7) 0.062(6) 0.044(5) 0.081(8) 0.087(9) F15D 0.045(3) 0.042(4) 0.100(8) 0.021(5) 0.015(4) 0.031(3) C24C 0.0292(15) 0.0402(16) 0.0207(13) 0.0130(12) 0.0074(11) 0.0090(12) F16C 0.0276(9) 0.0622(11) 0.0216(8) 0.0148(8) 0.0001(7) 0.0047(8) F17C 0.0294(9) 0.0699(12) 0.0355(9) 0.0351(9) 0.0150(7) 0.0114(8) F18C 0.0613(12) 0.0502(11) 0.0345(10) 0.0288(9) 0.0166(9) 0.0260(9) C25C 0.0219(12) 0.0207(12) 0.0221(12) 0.0108(10) 0.0068(10) 0.0062(10) C26C 0.0245(13) 0.0339(14) 0.0234(13) 0.0140(12) 0.0063(11) 0.0084(11) C27C 0.0385(17) 0.0473(18) 0.0274(15) 0.0217(13) 0.0074(12) 0.0159(14) C28C 0.0332(16) 0.0519(19) 0.0375(17) 0.0229(15) 0.0003(13) 0.0169(15) C29C 0.0246(14) 0.0416(16) 0.0390(16) 0.0184(14) 0.0072(12) 0.0146(12) C30C 0.0244(13) 0.0319(14) 0.0277(14) 0.0160(12) 0.0084(11) 0.0108(11) C31C 0.038(4) 0.092(5) 0.035(4) 0.039(4) 0.007(3) 0.028(4) F19C 0.036(2) 0.137(7) 0.045(3) 0.062(4) 0.018(2) 0.032(3) F20C 0.142(8) 0.144(6) 0.109(6) 0.113(5) 0.083(6) 0.093(6) F21C 0.056(3) 0.148(6) 0.026(2) 0.033(3) 0.0039(17) 0.016(3) C31D 0.041(7) 0.078(6) 0.032(5) 0.028(5) -0.004(4) 0.010(5) F19D 0.090(8) 0.100(7) 0.066(7) 0.051(5) 0.052(6) 0.034(6) F20D 0.155(11) 0.078(4) 0.067(5) 0.051(4) 0.047(5) 0.003(5) F21D 0.069(6) 0.226(15) 0.052(6) 0.091(8) 0.019(4) 0.064(8) C32C 0.030(5) 0.038(5) 0.054(6) 0.018(4) 0.006(4) 0.012(5) F22C 0.041(6) 0.056(5) 0.126(9) 0.036(6) 0.022(9) 0.031(5) F23C 0.028(3) 0.051(4) 0.051(3) 0.022(3) 0.001(3) 0.002(3) F24C 0.035(5) 0.117(11) 0.049(4) 0.035(6) 0.021(4) 0.035(9) C32D 0.030(7) 0.047(8) 0.052(8) 0.021(6) 0.005(6) 0.020(7) F22D 0.035(5) 0.091(8) 0.040(4) 0.036(4) 0.017(4) 0.041(5) F23D 0.038(7) 0.060(9) 0.038(5) 0.013(5) 0.003(5) 0.033(7) F24D 0.029(6) 0.045(5) 0.178(18) 0.042(7) 0.033(9) 0.014(4) C32E 0.026(6) 0.054(8) 0.058(9) 0.027(6) 0.001(5) 0.025(7) F22E 0.040(8) 0.072(6) 0.126(14) 0.014(8) 0.021(10) 0.036(5) F23E 0.021(4) 0.112(14) 0.059(6) 0.040(8) -0.003(4) 0.014(8) F24E 0.024(6) 0.074(7) 0.066(9) 0.036(7) 0.021(7) 0.020(7) B4 0.0197(14) 0.0199(13) 0.0211(14) 0.0101(11) 0.0087(11) 0.0077(11) C1F 0.0231(13) 0.0227(12) 0.0177(12) 0.0086(10) 0.0090(10) 0.0104(10) C2F 0.0250(13) 0.0239(12) 0.0168(12) 0.0074(10) 0.0064(10) 0.0107(11) C3F 0.0349(15) 0.0250(13) 0.0184(12) 0.0081(10) 0.0066(11) 0.0151(12) C4F 0.0305(15) 0.0364(15) 0.0287(15) 0.0143(12) 0.0046(12) 0.0188(13) C5F 0.0203(13) 0.0373(16) 0.0391(16) 0.0191(13) 0.0070(12) 0.0118(12) C6F 0.0240(14) 0.0299(14) 0.0344(15) 0.0180(12) 0.0106(11) 0.0118(11) C7F 0.0450(18) 0.0281(14) 0.0274(15) 0.0108(12) 0.0017(13) 0.0162(13) F1F 0.0452(10) 0.0268(8) 0.0469(10) 0.0175(8) 0.0008(8) 0.0103(8) F2F 0.0928(16) 0.0443(11) 0.0339(10) 0.0254(9) 0.0108(10) 0.0166(11) F3F 0.0548(12) 0.0402(10) 0.0759(14) 0.0250(10) 0.0078(10) 0.0296(10) C8F 0.0277(17) 0.061(2) 0.073(3) 0.039(2) 0.0093(17) 0.0206(16) F4F 0.0389(13) 0.099(2) 0.0685(17) -0.0091(14) 0.0005(11) -0.0017(12) F5F 0.0252(10) 0.0826(16) 0.0847(16) 0.0280(13) 0.0133(10) 0.0239(10) F6F 0.0236(11) 0.123(2) 0.260(4) 0.149(3) 0.0076(17) 0.0028(13) C9F 0.0133(11) 0.0196(12) 0.0233(12) 0.0102(10) 0.0071(10) 0.0025(9) C10F 0.0144(11) 0.0211(12) 0.0250(13) 0.0119(10) 0.0087(10) 0.0061(9) C11F 0.0162(12) 0.0193(12) 0.0239(13) 0.0094(10) 0.0086(10) 0.0030(10) C12F 0.0218(13) 0.0286(13) 0.0206(13) 0.0104(11) 0.0057(10) 0.0058(11) C13F 0.0220(13) 0.0259(13) 0.0246(13) 0.0124(11) 0.0060(11) 0.0075(11) C14F 0.0213(13) 0.0217(12) 0.0246(13) 0.0097(10) 0.0070(10) 0.0074(10) C15F 0.0230(13) 0.0227(13) 0.0255(13) 0.0094(11) 0.0102(11) 0.0062(11) F7F 0.0609(12) 0.0353(9) 0.0330(9) 0.0138(7) 0.0163(8) 0.0308(9) F8F 0.0266(8) 0.0237(8) 0.0400(9) 0.0004(7) 0.0085(7) 0.0013(7) F9F 0.0395(9) 0.0332(9) 0.0398(9) 0.0140(7) 0.0280(8) 0.0125(7) C16F 0.0403(17) 0.0368(16) 0.0297(15) 0.0150(13) 0.0063(13) 0.0187(14) F10F 0.0536(13) 0.1065(18) 0.0765(15) 0.0602(14) 0.0264(11) 0.0558(13) F11F 0.124(2) 0.0803(16) 0.0279(10) 0.0021(10) -0.0159(11) 0.0730(16) F12F 0.0624(13) 0.0528(12) 0.0780(15) 0.0448(11) 0.0042(11) 0.0227(10) C17F 0.0201(12) 0.0225(12) 0.0189(12) 0.0109(10) 0.0054(10) 0.0084(10) C18F 0.0229(13) 0.0228(13) 0.0229(13) 0.0093(10) 0.0068(10) 0.0074(10) C19F 0.0310(15) 0.0233(13) 0.0298(14) 0.0145(11) 0.0069(12) 0.0057(11) C20F 0.0402(16) 0.0191(13) 0.0281(14) 0.0082(11) 0.0055(12) 0.0078(12) C21F 0.0407(16) 0.0225(13) 0.0198(13) 0.0074(11) 0.0075(12) 0.0128(12) C22F 0.0293(14) 0.0241(13) 0.0210(13) 0.0116(11) 0.0089(11) 0.0116(11) C23F 0.048(2) 0.0301(16) 0.0447(19) 0.0172(14) 0.0180(16) 0.0038(14) F13F 0.0324(13) 0.211(4) 0.159(3) 0.151(3) 0.0265(15) 0.0141(17) F14F 0.0680(14) 0.0579(12) 0.0599(13) 0.0347(11) 0.0378(11) 0.0144(11) F15F 0.205(3) 0.0270(11) 0.144(3) 0.0335(14) 0.134(3) 0.0188(16) C24F 0.047(7) 0.023(6) 0.028(7) 0.009(5) 0.017(5) 0.016(4) F16F 0.186(13) 0.069(5) 0.048(6) 0.045(5) 0.071(7) 0.096(7) F17F 0.034(3) 0.058(9) 0.023(3) -0.008(5) 0.006(2) 0.000(4) F18F 0.023(2) 0.038(3) 0.034(4) -0.001(3) 0.010(2) 0.009(2) C24G 0.045(9) 0.028(10) 0.028(12) 0.006(9) 0.021(10) 0.016(9) F16G 0.102(12) 0.015(6) 0.048(11) 0.004(6) 0.043(9) 0.014(7) F17G 0.116(19) 0.052(11) 0.040(9) 0.026(9) 0.043(11) 0.036(11) F18G 0.051(8) 0.106(18) 0.049(11) -0.001(10) 0.016(8) 0.051(9) C24H 0.064(11) 0.028(9) 0.028(9) 0.014(7) 0.002(7) 0.009(7) F16H 0.049(7) 0.041(12) 0.042(10) -0.022(6) 0.001(7) 0.012(5) F17H 0.099(14) 0.045(5) 0.039(9) 0.003(5) 0.047(10) 0.013(8) F18H 0.081(7) 0.101(10) 0.031(6) 0.026(5) 0.027(5) 0.071(7) C25F 0.0260(13) 0.0188(12) 0.0316(14) 0.0140(11) 0.0139(11) 0.0119(10) C26F 0.0313(14) 0.0247(13) 0.0336(15) 0.0158(12) 0.0169(12) 0.0131(11) C27F 0.0443(17) 0.0336(15) 0.0414(16) 0.0223(13) 0.0283(14) 0.0196(13) C28F 0.0324(16) 0.0306(15) 0.0561(18) 0.0197(14) 0.0270(14) 0.0116(13) C29F 0.0261(14) 0.0255(14) 0.0462(17) 0.0158(13) 0.0181(12) 0.0101(11) C30F 0.0243(13) 0.0241(13) 0.0339(15) 0.0151(11) 0.0127(11) 0.0098(11) C31F 0.050(6) 0.054(5) 0.053(4) 0.036(4) 0.031(4) 0.023(4) F19F 0.078(4) 0.106(6) 0.041(4) 0.049(4) 0.034(3) 0.053(5) F20F 0.090(6) 0.060(3) 0.027(3) 0.010(3) 0.012(4) 0.035(4) F21F 0.070(4) 0.094(6) 0.063(4) 0.050(4) 0.045(3) 0.010(4) C31G 0.053(9) 0.051(8) 0.032(6) 0.005(8) 0.032(5) 0.007(7) F19G 0.059(6) 0.105(14) 0.028(5) 0.023(8) 0.024(4) 0.007(6) F20G 0.141(15) 0.091(10) 0.037(8) 0.034(8) 0.053(10) 0.079(11) F21G 0.072(9) 0.067(6) 0.053(8) 0.045(6) 0.001(7) 0.005(6) C31H 0.074(12) 0.058(12) 0.050(7) 0.044(9) 0.028(8) 0.017(11) F19H 0.072(14) 0.095(12) 0.043(8) 0.046(8) 0.000(11) 0.004(13) F20H 0.071(10) 0.080(16) 0.049(11) 0.024(11) 0.040(9) 0.004(10) F21H 0.13(2) 0.105(13) 0.128(16) 0.104(14) -0.005(18) 0.011(14) C32F 0.0224(14) 0.0303(15) 0.062(2) 0.0151(15) 0.0149(14) 0.0055(12) F22F 0.0355(10) 0.0461(11) 0.0767(15) 0.0226(10) 0.0034(10) 0.0138(9) F23F 0.0395(11) 0.0594(13) 0.0790(15) 0.0343(12) 0.0199(10) -0.0077(10) F24F 0.0360(10) 0.0515(12) 0.0508(12) 0.0057(9) 0.0054(9) 0.0112(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 B1 O11 1.453(4) . ? B1 O9 1.464(4) . ? B1 O19 1.470(4) . ? B1 O1 1.479(4) . ? O1 C1 1.326(3) . ? C1 C9A 1.403(4) . ? C1 C2 1.405(4) . ? C2 C3 1.379(3) . ? C2 H2 0.9500 . ? C3 C3A 1.460(4) . ? C3 S3 1.740(3) . ? S3 C3B 1.800(3) . ? C3B H3A 0.9800 . ? C3B H3B 0.9800 . ? C3B H3C 0.9800 . ? C3A C4 1.396(3) . ? C3A C9B 1.423(4) . ? C4 C5 1.381(4) . ? C4 H4 0.9500 . ? C5 C6 1.382(4) . ? C5 H5 0.9500 . ? C6 C6A 1.399(4) . ? C6 H6 0.9500 . ? C6A C9B 1.421(4) . ? C6A C7 1.454(4) . ? C7 C8 1.372(4) . ? C7 S7 1.738(3) . ? S7 C7B 1.801(4) . ? C7B H7A 0.9800 . ? C7B H7B 0.9800 . ? C7B H7C 0.9800 . ? C8 C9 1.405(4) . ? C8 H8 0.9500 . ? C9 O9 1.323(3) . ? C9 C9A 1.406(4) . ? C9A C9B 1.413(3) . ? O11 C11 1.335(3) . ? C11 C12 1.390(4) . ? C11 C19A 1.407(4) . ? C12 C13 1.388(3) . ? C12 H12 0.9500 . ? C13 C13A 1.456(4) . ? C13 S13 1.734(3) . ? S13 C13B 1.801(3) . ? C13B H13A 0.9800 . ? C13B H13B 0.9800 . ? C13B H13C 0.9800 . ? C13A C14 1.394(3) . ? C13A C19B 1.423(3) . ? C14 C15 1.375(4) . ? C14 H14 0.9500 . ? C15 C16 1.382(4) . ? C15 H15 0.9500 . ? C16 C16A 1.405(3) . ? C16 H16 0.9500 . ? C16A C19B 1.418(4) . ? C16A C17 1.452(4) . ? C17 C18 1.381(4) . ? C17 S17 1.734(3) . ? S17 C17B 1.795(3) . ? C17B H17A 0.9800 . ? C17B H17B 0.9800 . ? C17B H17C 0.9800 . ? C18 C19 1.400(4) . ? C18 H18 0.9500 . ? C19 O19 1.332(3) . ? C19 C19A 1.398(4) . ? C19A C19B 1.417(3) . ? B2 O39 1.457(3) . ? B2 O21 1.459(3) . ? B2 O29 1.478(4) . ? B2 O31 1.480(4) . ? O21 C21 1.335(3) . ? C21 C22 1.394(3) . ? C21 C29A 1.401(3) . ? C22 C23 1.382(3) . ? C22 H22 0.9500 . ? C23 C23A 1.454(4) . ? C23 S23 1.732(3) . ? S23 C23B 1.795(3) . ? C23B H23A 0.9800 . ? C23B H23B 0.9800 . ? C23B H23C 0.9800 . ? C23A C24 1.403(4) . ? C23A C29B 1.414(4) . ? C24 C25 1.379(4) . ? C24 H24 0.9500 . ? C25 C26 1.388(4) . ? C25 H25 0.9500 . ? C26 C26A 1.397(4) . ? C26 H26 0.9500 . ? C26A C29B 1.423(4) . ? C26A C27 1.454(4) . ? C27 C28 1.375(4) . ? C27 S27 1.742(3) . ? S27 C27B 1.797(3) . ? C27B H27A 0.9800 . ? C27B H27B 0.9800 . ? C27B H27C 0.9800 . ? C28 C29 1.402(4) . ? C28 H28 0.9500 . ? C29 O29 1.322(3) . ? C29 C29A 1.402(3) . ? C29A C29B 1.419(3) . ? O31 C31 1.328(3) . ? C31 C39A 1.403(3) . ? C31 C32 1.408(3) . ? C32 C33 1.370(3) . ? C32 H32 0.9500 . ? C33 C33A 1.452(3) . ? C33 S33 1.752(3) . ? C33A C34 1.399(3) . ? C33A C39B 1.421(3) . ? S33 C33B 1.793(3) . ? C33B H33A 0.9800 . ? C33B H33B 0.9800 . ? C33B H33C 0.9800 . ? C34 C35 1.383(4) . ? C34 H34 0.9500 . ? C35 C36 1.383(4) . ? C35 H35 0.9500 . ? C36 C36A 1.398(3) . ? C36 H36 0.9500 . ? C36A C39B 1.419(3) . ? C36A C37 1.451(3) . ? C37 C38 1.376(3) . ? C37 S37 1.741(2) . ? S37 C37B 1.794(3) . ? C37B H37A 0.9800 . ? C37B H37B 0.9800 . ? C37B H37C 0.9800 . ? C38 C39 1.400(3) . ? C38 H38 0.9500 . ? C39 O39 1.327(3) . ? C39 C39A 1.406(3) . ? C39A C39B 1.413(3) . ? C1S C2S 1.507(7) . ? C1S H1A 0.9800 . ? C1S H1B 0.9800 . ? C1S H1C 0.9800 . ? C2S O3S 1.417(6) . ? C2S H2A 0.9900 . ? C2S H2B 0.9900 . ? O3S C4S 1.397(6) . ? C4S C5S 1.507(7) . ? C4S H4A 0.9900 . ? C4S H4B 0.9900 . ? C5S H5A 0.9800 . ? C5S H5B 0.9800 . ? C5S H5C 0.9800 . ? C6S C7S 1.486(6) . ? C6S H6A 0.9800 . ? C6S H6B 0.9800 . ? C6S H6C 0.9800 . ? C7S O8S 1.413(5) . ? C7S H7D 0.9900 . ? C7S H7E 0.9900 . ? O8S C9S 1.416(4) . ? C9S C10S 1.500(6) . ? C9S H9A 0.9900 . ? C9S H9B 0.9900 . ? C10S H10A 0.9800 . ? C10S H10B 0.9800 . ? C10S H10D 0.9800 . ? C11S C12S 1.502(7) . ? C11S H11A 0.9800 . ? C11S H11B 0.9800 . ? C11S H11C 0.9800 . ? C12S O13S 1.401(6) . ? C12S H12A 0.9900 . ? C12S H12B 0.9900 . ? O13S C14S 1.394(5) . ? C14S C15S 1.501(6) . ? C14S H14A 0.9900 . ? C14S H14B 0.9900 . ? C15S H15A 0.9800 . ? C15S H15B 0.9800 . ? C15S H15C 0.9800 . ? B3 C1C 1.643(4) . ? B3 C9C 1.643(4) . ? B3 C17C 1.648(4) . ? B3 C25C 1.650(4) . ? C1C C6C 1.400(3) . ? C1C C2C 1.403(3) . ? C2C C3C 1.392(3) . ? C2C H2C 0.9500 . ? C3C C4C 1.389(4) . ? C3C C7C 1.492(3) . ? F1C C7C 1.335(3) . ? F2C C7C 1.342(3) . ? F3C C7C 1.341(3) . ? C4C C5C 1.386(3) . ? C4C H4C 0.9500 . ? C5C C6C 1.396(3) . ? C5C C8C 1.503(4) . ? F4C C8C 1.329(3) . ? F5C C8C 1.327(3) . ? F6C C8C 1.342(3) . ? C6C H6D 0.9500 . ? C9C C14C 1.399(3) . ? C9C C10C 1.403(3) . ? C10C C11C 1.398(3) . ? C10C H10C 0.9500 . ? C11C C12C 1.387(4) . ? C11C C15C 1.494(4) . ? C12C C13C 1.386(4) . ? C12C H12C 0.9500 . ? C13C C14C 1.396(3) . ? C13C C16C 1.494(4) . ? C14C H14C 0.9500 . ? C15C F7C 1.317(3) . ? C15C F8C 1.325(4) . ? C15C F9C 1.329(4) . ? C16C F11C 1.339(3) . ? C16C F10C 1.340(3) . ? C16C F12C 1.340(3) . ? C17C C18C 1.397(3) . ? C17C C22C 1.405(3) . ? C18C C19C 1.396(4) . ? C18C H18C 0.9500 . ? C19C C20C 1.379(4) . ? C19C C23C 1.499(6) . ? C19C C23D 1.508(7) . ? C20C C21C 1.388(4) . ? C20C H20C 0.9500 . ? C21C C22C 1.396(3) . ? C21C C24C 1.496(4) . ? C22C H22C 0.9500 . ? C23C F15C 1.314(6) . ? C23C F13C 1.329(6) . ? C23C F14C 1.331(7) . ? C23D F14D 1.328(8) . ? C23D F15D 1.335(8) . ? C23D F13D 1.341(8) . ? C24C F18C 1.332(3) . ? C24C F17C 1.345(3) . ? C24C F16C 1.347(3) . ? C25C C30C 1.399(4) . ? C25C C26C 1.399(4) . ? C26C C27C 1.399(4) . ? C26C H26C 0.9500 . ? C27C C28C 1.382(4) . ? C27C C31C 1.500(6) . ? C27C C31D 1.508(8) . ? C28C C29C 1.377(4) . ? C28C H28C 0.9500 . ? C29C C30C 1.396(4) . ? C29C C32D 1.506(8) . ? C29C C32C 1.510(7) . ? C29C C32E 1.511(8) . ? C30C H30C 0.9500 . ? C31C F20C 1.317(7) . ? C31C F21C 1.323(7) . ? C31C F19C 1.326(7) . ? C31D F21D 1.326(8) . ? C31D F20D 1.335(8) . ? C31D F19D 1.336(9) . ? C32C F22C 1.332(9) . ? C32C F23C 1.334(8) . ? C32C F24C 1.337(9) . ? C32D F23D 1.325(9) . ? C32D F24D 1.328(9) . ? C32D F22D 1.328(9) . ? C32E F23E 1.332(9) . ? C32E F24E 1.334(9) . ? C32E F22E 1.334(9) . ? B4 C9F 1.635(4) . ? B4 C17F 1.648(4) . ? B4 C25F 1.652(4) . ? B4 C1F 1.656(4) . ? C1F C6F 1.399(4) . ? C1F C2F 1.400(3) . ? C2F C3F 1.390(4) . ? C2F H2F 0.9500 . ? C3F C4F 1.388(4) . ? C3F C7F 1.503(4) . ? C4F C5F 1.382(4) . ? C4F H4F 0.9500 . ? C5F C6F 1.395(4) . ? C5F C8F 1.496(4) . ? C6F H6F 0.9500 . ? C7F F2F 1.329(3) . ? C7F F1F 1.336(3) . ? C7F F3F 1.342(3) . ? C8F F6F 1.289(4) . ? C8F F5F 1.324(4) . ? C8F F4F 1.349(4) . ? C9F C14F 1.393(3) . ? C9F C10F 1.405(3) . ? C10F C11F 1.399(3) . ? C10F H10F 0.9500 . ? C11F C12F 1.385(4) . ? C11F C15F 1.495(3) . ? C12F C13F 1.384(4) . ? C12F H12F 0.9500 . ? C13F C14F 1.391(4) . ? C13F C16F 1.494(4) . ? C14F H14F 0.9500 . ? C15F F7F 1.337(3) . ? C15F F9F 1.344(3) . ? C15F F8F 1.344(3) . ? C16F F11F 1.310(3) . ? C16F F12F 1.336(3) . ? C16F F10F 1.341(4) . ? C17F C22F 1.403(3) . ? C17F C18F 1.406(3) . ? C18F C19F 1.393(4) . ? C18F H18F 0.9500 . ? C19F C20F 1.384(4) . ? C19F C23F 1.491(4) . ? C20F C21F 1.383(4) . ? C20F H20F 0.9500 . ? C21F C22F 1.403(3) . ? C21F C24G 1.490(8) . ? C21F C24H 1.491(8) . ? C21F C24F 1.499(6) . ? C22F H22F 0.9500 . ? C23F F15F 1.301(4) . ? C23F F14F 1.321(4) . ? C23F F13F 1.326(4) . ? C24F F18F 1.330(8) . ? C24F F17F 1.334(8) . ? C24F F16F 1.338(8) . ? C24G F17G 1.319(10) . ? C24G F16G 1.323(10) . ? C24G F18G 1.323(10) . ? C24H F17H 1.324(9) . ? C24H F18H 1.331(9) . ? C24H F16H 1.331(9) . ? C25F C26F 1.402(4) . ? C25F C30F 1.403(4) . ? C26F C27F 1.401(4) . ? C26F H26F 0.9500 . ? C27F C28F 1.394(4) . ? C27F C31G 1.485(8) . ? C27F C31H 1.491(9) . ? C27F C31F 1.493(6) . ? C28F C29F 1.378(4) . ? C28F H28F 0.9500 . ? C29F C30F 1.391(4) . ? C29F C32F 1.508(4) . ? C30F H30F 0.9500 . ? C31F F19F 1.336(8) . ? C31F F21F 1.338(8) . ? C31F F20F 1.339(8) . ? C31G F21G 1.322(10) . ? C31G F19G 1.324(10) . ? C31G F20G 1.326(9) . ? C31H F21H 1.10(5) . ? C31H F20H 1.43(7) . ? C31H F19H 1.60(6) . ? C32F F22F 1.331(4) . ? C32F F23F 1.335(3) . ? C32F F24F 1.336(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 O11 B1 O9 108.7(2) . . ? O11 B1 O19 114.4(2) . . ? O9 B1 O19 106.8(2) . . ? O11 B1 O1 107.1(2) . . ? O9 B1 O1 112.3(2) . . ? O19 B1 O1 107.7(2) . . ? C1 O1 B1 120.4(2) . . ? O1 C1 C9A 120.2(2) . . ? O1 C1 C2 118.6(2) . . ? C9A C1 C2 121.2(2) . . ? C3 C2 C1 120.0(2) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C3A 120.5(2) . . ? C2 C3 S3 122.9(2) . . ? C3A C3 S3 116.65(18) . . ? C3 S3 C3B 103.47(13) . . ? S3 C3B H3A 109.5 . . ? S3 C3B H3B 109.5 . . ? H3A C3B H3B 109.5 . . ? S3 C3B H3C 109.5 . . ? H3A C3B H3C 109.5 . . ? H3B C3B H3C 109.5 . . ? C4 C3A C9B 118.6(2) . . ? C4 C3A C3 123.0(2) . . ? C9B C3A C3 118.5(2) . . ? C5 C4 C3A 121.0(3) . . ? C5 C4 H4 119.5 . . ? C3A C4 H4 119.5 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C6A 121.2(3) . . ? C5 C6 H6 119.4 . . ? C6A C6 H6 119.4 . . ? C6 C6A C9B 118.2(2) . . ? C6 C6A C7 123.6(2) . . ? C9B C6A C7 118.2(2) . . ? C8 C7 C6A 120.9(2) . . ? C8 C7 S7 122.8(2) . . ? C6A C7 S7 116.2(2) . . ? C7 S7 C7B 104.29(15) . . ? S7 C7B H7A 109.5 . . ? S7 C7B H7B 109.5 . . ? H7A C7B H7B 109.5 . . ? S7 C7B H7C 109.5 . . ? H7A C7B H7C 109.5 . . ? H7B C7B H7C 109.5 . . ? C7 C8 C9 120.2(2) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? O9 C9 C8 118.6(2) . . ? O9 C9 C9A 120.8(2) . . ? C8 C9 C9A 120.6(2) . . ? C1 C9A C9 119.6(2) . . ? C1 C9A C9B 120.1(2) . . ? C9 C9A C9B 120.2(2) . . ? C9A C9B C6A 119.8(2) . . ? C9A C9B C3A 119.8(2) . . ? C6A C9B C3A 120.5(2) . . ? C9 O9 B1 120.0(2) . . ? C11 O11 B1 122.1(2) . . ? O11 C11 C12 118.1(2) . . ? O11 C11 C19A 120.6(2) . . ? C12 C11 C19A 121.3(2) . . ? C13 C12 C11 120.2(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C13A 120.5(2) . . ? C12 C13 S13 122.3(2) . . ? C13A C13 S13 117.19(18) . . ? C13 S13 C13B 103.03(13) . . ? S13 C13B H13A 109.5 . . ? S13 C13B H13B 109.5 . . ? H13A C13B H13B 109.5 . . ? S13 C13B H13C 109.5 . . ? H13A C13B H13C 109.5 . . ? H13B C13B H13C 109.5 . . ? C14 C13A C19B 118.6(2) . . ? C14 C13A C13 123.1(2) . . ? C19B C13A C13 118.3(2) . . ? C15 C14 C13A 120.8(3) . . ? C15 C14 H14 119.6 . . ? C13A C14 H14 119.6 . . ? C14 C15 C16 121.3(2) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C16A 120.3(3) . . ? C15 C16 H16 119.9 . . ? C16A C16 H16 119.9 . . ? C16 C16A C19B 118.6(2) . . ? C16 C16A C17 122.9(2) . . ? C19B C16A C17 118.4(2) . . ? C18 C17 C16A 120.5(2) . . ? C18 C17 S17 123.2(2) . . ? C16A C17 S17 116.29(19) . . ? C17 S17 C17B 103.25(15) . . ? S17 C17B H17A 109.5 . . ? S17 C17B H17B 109.5 . . ? H17A C17B H17B 109.5 . . ? S17 C17B H17C 109.5 . . ? H17A C17B H17C 109.5 . . ? H17B C17B H17C 109.5 . . ? C17 C18 C19 120.2(2) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? O19 C19 C19A 120.3(2) . . ? O19 C19 C18 118.7(2) . . ? C19A C19 C18 121.0(2) . . ? C19 C19A C11 120.1(2) . . ? C19 C19A C19B 120.0(2) . . ? C11 C19A C19B 119.8(2) . . ? C19A C19B C16A 119.8(2) . . ? C19A C19B C13A 119.9(2) . . ? C16A C19B C13A 120.2(2) . . ? C19 O19 B1 122.3(2) . . ? O39 B2 O21 108.4(2) . . ? O39 B2 O29 106.7(2) . . ? O21 B2 O29 113.0(2) . . ? O39 B2 O31 113.5(2) . . ? O21 B2 O31 107.1(2) . . ? O29 B2 O31 108.2(2) . . ? C21 O21 B2 120.2(2) . . ? O21 C21 C22 118.3(2) . . ? O21 C21 C29A 120.3(2) . . ? C22 C21 C29A 121.4(2) . . ? C23 C22 C21 119.7(2) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C23A 120.9(2) . . ? C22 C23 S23 122.9(2) . . ? C23A C23 S23 116.21(19) . . ? C23 S23 C23B 103.58(13) . . ? S23 C23B H23A 109.5 . . ? S23 C23B H23B 109.5 . . ? H23A C23B H23B 109.5 . . ? S23 C23B H23C 109.5 . . ? H23A C23B H23C 109.5 . . ? H23B C23B H23C 109.5 . . ? C24 C23A C29B 118.9(2) . . ? C24 C23A C23 122.9(2) . . ? C29B C23A C23 118.2(2) . . ? C25 C24 C23A 120.6(3) . . ? C25 C24 H24 119.7 . . ? C23A C24 H24 119.7 . . ? C24 C25 C26 120.8(3) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C26A 120.8(3) . . ? C25 C26 H26 119.6 . . ? C26A C26 H26 119.6 . . ? C26 C26A C29B 118.6(2) . . ? C26 C26A C27 123.2(2) . . ? C29B C26A C27 118.2(2) . . ? C28 C27 C26A 120.7(2) . . ? C28 C27 S27 122.3(2) . . ? C26A C27 S27 116.92(19) . . ? C27 S27 C27B 103.51(14) . . ? S27 C27B H27A 109.5 . . ? S27 C27B H27B 109.5 . . ? H27A C27B H27B 109.5 . . ? S27 C27B H27C 109.5 . . ? H27A C27B H27C 109.5 . . ? H27B C27B H27C 109.5 . . ? C27 C28 C29 120.3(2) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? O29 C29 C29A 120.1(2) . . ? O29 C29 C28 118.8(2) . . ? C29A C29 C28 121.1(2) . . ? C21 C29A C29 120.4(2) . . ? C21 C29A C29B 119.8(2) . . ? C29 C29A C29B 119.8(2) . . ? C23A C29B C29A 119.8(2) . . ? C23A C29B C26A 120.3(2) . . ? C29A C29B C26A 119.9(2) . . ? C29 O29 B2 120.9(2) . . ? C31 O31 B2 120.7(2) . . ? O31 C31 C39A 120.4(2) . . ? O31 C31 C32 119.1(2) . . ? C39A C31 C32 120.5(2) . . ? C33 C32 C31 120.4(2) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C33A 120.9(2) . . ? C32 C33 S33 122.7(2) . . ? C33A C33 S33 116.46(18) . . ? C34 C33A C39B 118.7(2) . . ? C34 C33A C33 123.2(2) . . ? C39B C33A C33 118.1(2) . . ? C33 S33 C33B 103.47(14) . . ? S33 C33B H33A 109.5 . . ? S33 C33B H33B 109.5 . . ? H33A C33B H33B 109.5 . . ? S33 C33B H33C 109.5 . . ? H33A C33B H33C 109.5 . . ? H33B C33B H33C 109.5 . . ? C35 C34 C33A 120.7(2) . . ? C35 C34 H34 119.6 . . ? C33A C34 H34 119.6 . . ? C36 C35 C34 120.7(2) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C36A 121.1(2) . . ? C35 C36 H36 119.5 . . ? C36A C36 H36 119.5 . . ? C36 C36A C39B 118.5(2) . . ? C36 C36A C37 123.3(2) . . ? C39B C36A C37 118.3(2) . . ? C38 C37 C36A 121.0(2) . . ? C38 C37 S37 122.15(19) . . ? C36A C37 S37 116.88(18) . . ? C37 S37 C37B 102.69(12) . . ? S37 C37B H37A 109.5 . . ? S37 C37B H37B 109.5 . . ? H37A C37B H37B 109.5 . . ? S37 C37B H37C 109.5 . . ? H37A C37B H37C 109.5 . . ? H37B C37B H37C 109.5 . . ? C37 C38 C39 120.0(2) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? O39 C39 C38 118.1(2) . . ? O39 C39 C39A 121.1(2) . . ? C38 C39 C39A 120.8(2) . . ? C31 C39A C39 119.6(2) . . ? C31 C39A C39B 120.1(2) . . ? C39 C39A C39B 120.2(2) . . ? C39A C39B C36A 119.7(2) . . ? C39A C39B C33A 120.0(2) . . ? C36A C39B C33A 120.3(2) . . ? C39 O39 B2 120.1(2) . . ? C2S C1S H1A 109.5 . . ? C2S C1S H1B 109.5 . . ? H1A C1S H1B 109.5 . . ? C2S C1S H1C 109.5 . . ? H1A C1S H1C 109.5 . . ? H1B C1S H1C 109.5 . . ? O3S C2S C1S 105.8(6) . . ? O3S C2S H2A 110.6 . . ? C1S C2S H2A 110.6 . . ? O3S C2S H2B 110.6 . . ? C1S C2S H2B 110.6 . . ? H2A C2S H2B 108.7 . . ? C4S O3S C2S 110.2(5) . . ? O3S C4S C5S 110.2(5) . . ? O3S C4S H4A 109.6 . . ? C5S C4S H4A 109.6 . . ? O3S C4S H4B 109.6 . . ? C5S C4S H4B 109.6 . . ? H4A C4S H4B 108.1 . . ? C4S C5S H5A 109.5 . . ? C4S C5S H5B 109.5 . . ? H5A C5S H5B 109.5 . . ? C4S C5S H5C 109.5 . . ? H5A C5S H5C 109.5 . . ? H5B C5S H5C 109.5 . . ? C7S C6S H6A 109.5 . . ? C7S C6S H6B 109.5 . . ? H6A C6S H6B 109.5 . . ? C7S C6S H6C 109.5 . . ? H6A C6S H6C 109.5 . . ? H6B C6S H6C 109.5 . . ? O8S C7S C6S 108.4(5) . . ? O8S C7S H7D 110.0 . . ? C6S C7S H7D 110.0 . . ? O8S C7S H7E 110.0 . . ? C6S C7S H7E 110.0 . . ? H7D C7S H7E 108.4 . . ? C7S O8S C9S 111.4(3) . . ? O8S C9S C10S 108.4(4) . . ? O8S C9S H9A 110.0 . . ? C10S C9S H9A 110.0 . . ? O8S C9S H9B 110.0 . . ? C10S C9S H9B 110.0 . . ? H9A C9S H9B 108.4 . . ? C9S C10S H10A 109.5 . . ? C9S C10S H10B 109.5 . . ? H10A C10S H10B 109.5 . . ? C9S C10S H10D 109.5 . . ? H10A C10S H10D 109.5 . . ? H10B C10S H10D 109.5 . . ? C12S C11S H11A 109.5 . . ? C12S C11S H11B 109.5 . . ? H11A C11S H11B 109.5 . . ? C12S C11S H11C 109.5 . . ? H11A C11S H11C 109.5 . . ? H11B C11S H11C 109.5 . . ? O13S C12S C11S 109.2(5) . . ? O13S C12S H12A 109.8 . . ? C11S C12S H12A 109.8 . . ? O13S C12S H12B 109.8 . . ? C11S C12S H12B 109.8 . . ? H12A C12S H12B 108.3 . . ? C14S O13S C12S 111.2(4) . . ? O13S C14S C15S 108.4(4) . . ? O13S C14S H14A 110.0 . . ? C15S C14S H14A 110.0 . . ? O13S C14S H14B 110.0 . . ? C15S C14S H14B 110.0 . . ? H14A C14S H14B 108.4 . . ? C14S C15S H15A 109.5 . . ? C14S C15S H15B 109.5 . . ? H15A C15S H15B 109.5 . . ? C14S C15S H15C 109.5 . . ? H15A C15S H15C 109.5 . . ? H15B C15S H15C 109.5 . . ? C1C B3 C9C 115.6(2) . . ? C1C B3 C17C 104.72(18) . . ? C9C B3 C17C 110.38(19) . . ? C1C B3 C25C 110.69(19) . . ? C9C B3 C25C 104.43(19) . . ? C17C B3 C25C 111.2(2) . . ? C6C C1C C2C 115.3(2) . . ? C6C C1C B3 124.9(2) . . ? C2C C1C B3 119.6(2) . . ? C3C C2C C1C 123.0(2) . . ? C3C C2C H2C 118.5 . . ? C1C C2C H2C 118.5 . . ? C4C C3C C2C 120.3(2) . . ? C4C C3C C7C 120.9(2) . . ? C2C C3C C7C 118.8(2) . . ? C5C C4C C3C 118.0(2) . . ? C5C C4C H4C 121.0 . . ? C3C C4C H4C 121.0 . . ? C4C C5C C6C 121.1(2) . . ? C4C C5C C8C 120.2(2) . . ? C6C C5C C8C 118.7(2) . . ? C5C C6C C1C 122.1(2) . . ? C5C C6C H6D 118.9 . . ? C1C C6C H6D 118.9 . . ? F1C C7C F3C 106.1(2) . . ? F1C C7C F2C 105.6(2) . . ? F3C C7C F2C 106.2(2) . . ? F1C C7C C3C 112.9(2) . . ? F3C C7C C3C 113.2(2) . . ? F2C C7C C3C 112.3(2) . . ? F5C C8C F4C 108.1(2) . . ? F5C C8C F6C 106.2(2) . . ? F4C C8C F6C 105.4(2) . . ? F5C C8C C5C 112.5(2) . . ? F4C C8C C5C 112.6(2) . . ? F6C C8C C5C 111.5(2) . . ? C14C C9C C10C 115.5(2) . . ? C14C C9C B3 119.3(2) . . ? C10C C9C B3 125.1(2) . . ? C11C C10C C9C 122.0(2) . . ? C11C C10C H10C 119.0 . . ? C9C C10C H10C 119.0 . . ? C12C C11C C10C 121.1(2) . . ? C12C C11C C15C 118.4(2) . . ? C10C C11C C15C 120.5(2) . . ? C13C C12C C11C 118.1(2) . . ? C13C C12C H12C 120.9 . . ? C11C C12C H12C 120.9 . . ? C12C C13C C14C 120.4(2) . . ? C12C C13C C16C 121.3(2) . . ? C14C C13C C16C 118.3(2) . . ? C13C C14C C9C 122.9(2) . . ? C13C C14C H14C 118.5 . . ? C9C C14C H14C 118.5 . . ? F7C C15C F8C 105.7(3) . . ? F7C C15C F9C 105.6(3) . . ? F8C C15C F9C 105.8(3) . . ? F7C C15C C11C 114.1(2) . . ? F8C C15C C11C 112.3(2) . . ? F9C C15C C11C 112.6(2) . . ? F11C C16C F10C 106.0(2) . . ? F11C C16C F12C 106.4(2) . . ? F10C C16C F12C 106.2(2) . . ? F11C C16C C13C 112.1(2) . . ? F10C C16C C13C 113.1(2) . . ? F12C C16C C13C 112.6(2) . . ? C18C C17C C22C 115.8(2) . . ? C18C C17C B3 121.6(2) . . ? C22C C17C B3 122.6(2) . . ? C19C C18C C17C 122.2(2) . . ? C19C C18C H18C 118.9 . . ? C17C C18C H18C 118.9 . . ? C20C C19C C18C 120.8(2) . . ? C20C C19C C23C 116.8(4) . . ? C18C C19C C23C 122.3(4) . . ? C20C C19C C23D 124.8(4) . . ? C18C C19C C23D 113.4(5) . . ? C23C C19C C23D 15.2(5) . . ? C19C C20C C21C 118.5(2) . . ? C19C C20C H20C 120.8 . . ? C21C C20C H20C 120.8 . . ? C20C C21C C22C 120.5(2) . . ? C20C C21C C24C 118.5(2) . . ? C22C C21C C24C 121.0(2) . . ? C21C C22C C17C 122.1(2) . . ? C21C C22C H22C 118.9 . . ? C17C C22C H22C 118.9 . . ? F15C C23C F13C 108.2(5) . . ? F15C C23C F14C 106.6(5) . . ? F13C C23C F14C 106.0(5) . . ? F15C C23C C19C 109.7(5) . . ? F13C C23C C19C 112.9(7) . . ? F14C C23C C19C 113.0(5) . . ? F14D C23D F15D 104.1(7) . . ? F14D C23D F13D 103.6(7) . . ? F15D C23D F13D 102.8(7) . . ? F14D C23D C19C 113.6(7) . . ? F15D C23D C19C 120.2(8) . . ? F13D C23D C19C 110.7(11) . . ? F18C C24C F17C 106.9(2) . . ? F18C C24C F16C 106.6(2) . . ? F17C C24C F16C 105.3(2) . . ? F18C C24C C21C 113.5(2) . . ? F17C C24C C21C 111.7(2) . . ? F16C C24C C21C 112.4(2) . . ? C30C C25C C26C 115.7(2) . . ? C30C C25C B3 121.0(2) . . ? C26C C25C B3 123.2(2) . . ? C27C C26C C25C 121.9(3) . . ? C27C C26C H26C 119.1 . . ? C25C C26C H26C 119.1 . . ? C28C C27C C26C 121.2(3) . . ? C28C C27C C31C 115.4(4) . . ? C26C C27C C31C 123.3(4) . . ? C28C C27C C31D 124.7(5) . . ? C26C C27C C31D 113.5(5) . . ? C31C C27C C31D 13.6(5) . . ? C29C C28C C27C 117.8(3) . . ? C29C C28C H28C 121.1 . . ? C27C C28C H28C 121.1 . . ? C28C C29C C30C 121.2(3) . . ? C28C C29C C32D 119.1(5) . . ? C30C C29C C32D 119.1(5) . . ? C28C C29C C32C 116.3(5) . . ? C30C C29C C32C 122.4(5) . . ? C32D C29C C32C 12.5(6) . . ? C28C C29C C32E 124.9(6) . . ? C30C C29C C32E 113.9(6) . . ? C32D C29C C32E 7.9(8) . . ? C32C C29C C32E 10.8(7) . . ? C29C C30C C25C 122.2(3) . . ? C29C C30C H30C 118.9 . . ? C25C C30C H30C 118.9 . . ? F20C C31C F21C 108.4(6) . . ? F20C C31C F19C 108.1(6) . . ? F21C C31C F19C 107.1(6) . . ? F20C C31C C27C 109.0(5) . . ? F21C C31C C27C 113.0(5) . . ? F19C C31C C27C 111.1(7) . . ? F21D C31D F20D 103.7(7) . . ? F21D C31D F19D 103.1(7) . . ? F20D C31D F19D 102.0(7) . . ? F21D C31D C27C 113.0(8) . . ? F20D C31D C27C 118.3(7) . . ? F19D C31D C27C 115.0(12) . . ? F22C C32C F23C 106.9(7) . . ? F22C C32C F24C 106.8(8) . . ? F23C C32C F24C 107.0(8) . . ? F22C C32C C29C 108.8(7) . . ? F23C C32C C29C 115.0(7) . . ? F24C C32C C29C 112.0(15) . . ? F23D C32D F24D 107.3(8) . . ? F23D C32D F22D 107.2(8) . . ? F24D C32D F22D 107.1(8) . . ? F23D C32D C29C 113.9(11) . . ? F24D C32D C29C 106.7(8) . . ? F22D C32D C29C 114.3(10) . . ? F23E C32E F24E 104.5(10) . . ? F23E C32E F22E 104.3(9) . . ? F24E C32E F22E 103.7(9) . . ? F23E C32E C29C 111.7(9) . . ? F24E C32E C29C 116(2) . . ? F22E C32E C29C 115.3(10) . . ? C9F B4 C17F 110.43(19) . . ? C9F B4 C25F 106.8(2) . . ? C17F B4 C25F 112.1(2) . . ? C9F B4 C1F 111.23(19) . . ? C17F B4 C1F 108.38(19) . . ? C25F B4 C1F 107.89(19) . . ? C6F C1F C2F 115.8(2) . . ? C6F C1F B4 123.4(2) . . ? C2F C1F B4 120.8(2) . . ? C3F C2F C1F 122.2(2) . . ? C3F C2F H2F 118.9 . . ? C1F C2F H2F 118.9 . . ? C4F C3F C2F 120.9(2) . . ? C4F C3F C7F 118.6(2) . . ? C2F C3F C7F 120.4(2) . . ? C5F C4F C3F 118.0(2) . . ? C5F C4F H4F 121.0 . . ? C3F C4F H4F 121.0 . . ? C4F C5F C6F 120.8(3) . . ? C4F C5F C8F 118.5(3) . . ? C6F C5F C8F 120.6(3) . . ? C5F C6F C1F 122.2(2) . . ? C5F C6F H6F 118.9 . . ? C1F C6F H6F 118.9 . . ? F2F C7F F1F 107.1(3) . . ? F2F C7F F3F 105.6(2) . . ? F1F C7F F3F 106.4(2) . . ? F2F C7F C3F 112.1(2) . . ? F1F C7F C3F 113.0(2) . . ? F3F C7F C3F 112.2(3) . . ? F6F C8F F5F 106.8(3) . . ? F6F C8F F4F 106.4(4) . . ? F5F C8F F4F 104.3(3) . . ? F6F C8F C5F 114.2(3) . . ? F5F C8F C5F 113.1(3) . . ? F4F C8F C5F 111.3(3) . . ? C14F C9F C10F 116.0(2) . . ? C14F C9F B4 120.1(2) . . ? C10F C9F B4 123.1(2) . . ? C11F C10F C9F 121.5(2) . . ? C11F C10F H10F 119.3 . . ? C9F C10F H10F 119.3 . . ? C12F C11F C10F 121.0(2) . . ? C12F C11F C15F 118.0(2) . . ? C10F C11F C15F 121.0(2) . . ? C13F C12F C11F 118.4(2) . . ? C13F C12F H12F 120.8 . . ? C11F C12F H12F 120.8 . . ? C12F C13F C14F 120.3(2) . . ? C12F C13F C16F 120.7(2) . . ? C14F C13F C16F 118.9(2) . . ? C13F C14F C9F 122.8(2) . . ? C13F C14F H14F 118.6 . . ? C9F C14F H14F 118.6 . . ? F7F C15F F9F 106.1(2) . . ? F7F C15F F8F 106.6(2) . . ? F9F C15F F8F 105.4(2) . . ? F7F C15F C11F 113.9(2) . . ? F9F C15F C11F 112.1(2) . . ? F8F C15F C11F 112.2(2) . . ? F11F C16F F12F 107.8(3) . . ? F11F C16F F10F 106.7(3) . . ? F12F C16F F10F 102.2(2) . . ? F11F C16F C13F 114.4(2) . . ? F12F C16F C13F 112.4(2) . . ? F10F C16F C13F 112.5(2) . . ? C22F C17F C18F 115.4(2) . . ? C22F C17F B4 124.2(2) . . ? C18F C17F B4 120.3(2) . . ? C19F C18F C17F 122.7(2) . . ? C19F C18F H18F 118.6 . . ? C17F C18F H18F 118.6 . . ? C20F C19F C18F 120.4(2) . . ? C20F C19F C23F 119.3(2) . . ? C18F C19F C23F 120.2(3) . . ? C21F C20F C19F 118.5(2) . . ? C21F C20F H20F 120.7 . . ? C19F C20F H20F 120.7 . . ? C20F C21F C22F 120.8(2) . . ? C20F C21F C24G 113.8(6) . . ? C22F C21F C24G 124.9(6) . . ? C20F C21F C24H 116.9(5) . . ? C22F C21F C24H 122.2(5) . . ? C24G C21F C24H 9.2(8) . . ? C20F C21F C24F 121.6(4) . . ? C22F C21F C24F 117.5(4) . . ? C24G C21F C24F 10.7(8) . . ? C24H C21F C24F 4.9(7) . . ? C17F C22F C21F 122.0(2) . . ? C17F C22F H22F 119.0 . . ? C21F C22F H22F 119.0 . . ? F15F C23F F14F 104.7(3) . . ? F15F C23F F13F 109.2(3) . . ? F14F C23F F13F 103.4(3) . . ? F15F C23F C19F 113.9(3) . . ? F14F C23F C19F 113.3(3) . . ? F13F C23F C19F 111.7(3) . . ? F18F C24F F17F 105.0(7) . . ? F18F C24F F16F 103.9(7) . . ? F17F C24F F16F 103.6(7) . . ? F18F C24F C21F 117.7(9) . . ? F17F C24F C21F 111.3(11) . . ? F16F C24F C21F 114.0(9) . . ? F17G C24G F16G 108.2(9) . . ? F17G C24G F18G 108.5(9) . . ? F16G C24G F18G 108.1(9) . . ? F17G C24G C21F 109.2(11) . . ? F16G C24G C21F 116.3(15) . . ? F18G C24G C21F 106.4(12) . . ? F17H C24H F18H 110.0(9) . . ? F17H C24H F16H 102.9(11) . . ? F18H C24H F16H 109.8(9) . . ? F17H C24H C21F 111.2(11) . . ? F18H C24H C21F 110.5(11) . . ? F16H C24H C21F 112.3(14) . . ? C26F C25F C30F 115.9(2) . . ? C26F C25F B4 121.7(2) . . ? C30F C25F B4 122.2(2) . . ? C27F C26F C25F 121.9(3) . . ? C27F C26F H26F 119.0 . . ? C25F C26F H26F 119.0 . . ? C28F C27F C26F 120.4(3) . . ? C28F C27F C31G 118.1(6) . . ? C26F C27F C31G 121.6(7) . . ? C28F C27F C31H 113(3) . . ? C26F C27F C31H 126(3) . . ? C31G C27F C31H 6(3) . . ? C28F C27F C31F 122.8(4) . . ? C26F C27F C31F 116.8(5) . . ? C31G C27F C31F 4.9(8) . . ? C31H C27F C31F 10(3) . . ? C29F C28F C27F 118.6(3) . . ? C29F C28F H28F 120.7 . . ? C27F C28F H28F 120.7 . . ? C28F C29F C30F 120.7(3) . . ? C28F C29F C32F 121.9(3) . . ? C30F C29F C32F 117.4(3) . . ? C29F C30F C25F 122.4(3) . . ? C29F C30F H30F 118.8 . . ? C25F C30F H30F 118.8 . . ? F19F C31F F21F 105.2(7) . . ? F19F C31F F20F 105.4(6) . . ? F21F C31F F20F 106.6(6) . . ? F19F C31F C27F 113.6(7) . . ? F21F C31F C27F 113.1(9) . . ? F20F C31F C27F 112.3(7) . . ? F21G C31G F19G 106.3(9) . . ? F21G C31G F20G 106.0(9) . . ? F19G C31G F20G 105.5(8) . . ? F21G C31G C27F 112.7(14) . . ? F19G C31G C27F 115.8(13) . . ? F20G C31G C27F 109.9(10) . . ? F21H C31H F20H 106(4) . . ? F21H C31H C27F 126(5) . . ? F20H C31H C27F 108(4) . . ? F21H C31H F19H 97(4) . . ? F20H C31H F19H 103(4) . . ? C27F C31H F19H 114(4) . . ? F22F C32F F23F 107.5(2) . . ? F22F C32F F24F 105.3(3) . . ? F23F C32F F24F 106.3(2) . . ? F22F C32F C29F 111.8(2) . . ? F23F C32F C29F 112.5(3) . . ? F24F C32F C29F 113.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 B1 O1 C1 147.1(2) . . . . ? O9 B1 O1 C1 27.9(3) . . . . ? O19 B1 O1 C1 -89.4(3) . . . . ? B1 O1 C1 C9A -13.1(4) . . . . ? B1 O1 C1 C2 166.8(2) . . . . ? O1 C1 C2 C3 179.5(2) . . . . ? C9A C1 C2 C3 -0.6(4) . . . . ? C1 C2 C3 C3A -0.9(4) . . . . ? C1 C2 C3 S3 178.2(2) . . . . ? C2 C3 S3 C3B -0.7(3) . . . . ? C3A C3 S3 C3B 178.5(2) . . . . ? C2 C3 C3A C4 -178.0(3) . . . . ? S3 C3 C3A C4 2.8(3) . . . . ? C2 C3 C3A C9B 1.5(4) . . . . ? S3 C3 C3A C9B -177.65(19) . . . . ? C9B C3A C4 C5 0.7(4) . . . . ? C3 C3A C4 C5 -179.8(3) . . . . ? C3A C4 C5 C6 -0.2(4) . . . . ? C4 C5 C6 C6A -0.3(4) . . . . ? C5 C6 C6A C9B 0.2(4) . . . . ? C5 C6 C6A C7 -179.1(3) . . . . ? C6 C6A C7 C8 176.1(3) . . . . ? C9B C6A C7 C8 -3.2(4) . . . . ? C6 C6A C7 S7 -4.4(4) . . . . ? C9B C6A C7 S7 176.4(2) . . . . ? C8 C7 S7 C7B 1.5(3) . . . . ? C6A C7 S7 C7B -178.1(2) . . . . ? C6A C7 C8 C9 3.4(4) . . . . ? S7 C7 C8 C9 -176.1(2) . . . . ? C7 C8 C9 O9 179.3(3) . . . . ? C7 C8 C9 C9A -0.4(4) . . . . ? O1 C1 C9A C9 -2.7(4) . . . . ? C2 C1 C9A C9 177.4(2) . . . . ? O1 C1 C9A C9B -178.6(2) . . . . ? C2 C1 C9A C9B 1.5(4) . . . . ? O9 C9 C9A C1 1.5(4) . . . . ? C8 C9 C9A C1 -178.7(2) . . . . ? O9 C9 C9A C9B 177.4(2) . . . . ? C8 C9 C9A C9B -2.9(4) . . . . ? C1 C9A C9B C6A 178.9(2) . . . . ? C9 C9A C9B C6A 3.0(4) . . . . ? C1 C9A C9B C3A -0.8(4) . . . . ? C9 C9A C9B C3A -176.7(2) . . . . ? C6 C6A C9B C9A -179.4(2) . . . . ? C7 C6A C9B C9A -0.1(4) . . . . ? C6 C6A C9B C3A 0.3(4) . . . . ? C7 C6A C9B C3A 179.6(2) . . . . ? C4 C3A C9B C9A 178.9(2) . . . . ? C3 C3A C9B C9A -0.6(4) . . . . ? C4 C3A C9B C6A -0.8(4) . . . . ? C3 C3A C9B C6A 179.7(2) . . . . ? C8 C9 O9 B1 -164.2(3) . . . . ? C9A C9 O9 B1 15.5(4) . . . . ? O11 B1 O9 C9 -147.2(2) . . . . ? O19 B1 O9 C9 88.9(3) . . . . ? O1 B1 O9 C9 -28.9(4) . . . . ? O9 B1 O11 C11 -121.1(2) . . . . ? O19 B1 O11 C11 -1.9(4) . . . . ? O1 B1 O11 C11 117.4(2) . . . . ? B1 O11 C11 C12 178.5(2) . . . . ? B1 O11 C11 C19A -1.7(4) . . . . ? O11 C11 C12 C13 177.5(2) . . . . ? C19A C11 C12 C13 -2.3(4) . . . . ? C11 C12 C13 C13A 1.2(4) . . . . ? C11 C12 C13 S13 -179.91(19) . . . . ? C12 C13 S13 C13B -16.3(3) . . . . ? C13A C13 S13 C13B 162.6(2) . . . . ? C12 C13 C13A C14 179.0(2) . . . . ? S13 C13 C13A C14 0.0(3) . . . . ? C12 C13 C13A C19B 1.0(3) . . . . ? S13 C13 C13A C19B -178.02(18) . . . . ? C19B C13A C14 C15 0.3(4) . . . . ? C13 C13A C14 C15 -177.8(2) . . . . ? C13A C14 C15 C16 0.9(4) . . . . ? C14 C15 C16 C16A -1.0(4) . . . . ? C15 C16 C16A C19B -0.1(4) . . . . ? C15 C16 C16A C17 179.3(2) . . . . ? C16 C16A C17 C18 180.0(2) . . . . ? C19B C16A C17 C18 -0.7(4) . . . . ? C16 C16A C17 S17 0.1(3) . . . . ? C19B C16A C17 S17 179.43(18) . . . . ? C18 C17 S17 C17B 2.2(3) . . . . ? C16A C17 S17 C17B -177.9(2) . . . . ? C16A C17 C18 C19 0.4(4) . . . . ? S17 C17 C18 C19 -179.7(2) . . . . ? C17 C18 C19 O19 179.7(2) . . . . ? C17 C18 C19 C19A -0.1(4) . . . . ? O19 C19 C19A C11 -2.1(4) . . . . ? C18 C19 C19A C11 177.6(2) . . . . ? O19 C19 C19A C19B -179.7(2) . . . . ? C18 C19 C19A C19B 0.0(4) . . . . ? O11 C11 C19A C19 3.9(4) . . . . ? C12 C11 C19A C19 -176.3(2) . . . . ? O11 C11 C19A C19B -178.5(2) . . . . ? C12 C11 C19A C19B 1.3(4) . . . . ? C19 C19A C19B C16A -0.3(3) . . . . ? C11 C19A C19B C16A -177.9(2) . . . . ? C19 C19A C19B C13A 178.5(2) . . . . ? C11 C19A C19B C13A 0.9(3) . . . . ? C16 C16A C19B C19A 180.0(2) . . . . ? C17 C16A C19B C19A 0.6(3) . . . . ? C16 C16A C19B C13A 1.2(3) . . . . ? C17 C16A C19B C13A -178.2(2) . . . . ? C14 C13A C19B C19A 179.9(2) . . . . ? C13 C13A C19B C19A -2.0(3) . . . . ? C14 C13A C19B C16A -1.3(3) . . . . ? C13 C13A C19B C16A 176.8(2) . . . . ? C19A C19 O19 B1 -1.7(4) . . . . ? C18 C19 O19 B1 178.5(2) . . . . ? O11 B1 O19 C19 3.7(4) . . . . ? O9 B1 O19 C19 124.0(2) . . . . ? O1 B1 O19 C19 -115.3(2) . . . . ? O39 B2 O21 C21 -144.1(2) . . . . ? O29 B2 O21 C21 -26.1(3) . . . . ? O31 B2 O21 C21 93.0(3) . . . . ? B2 O21 C21 C22 -164.8(2) . . . . ? B2 O21 C21 C29A 15.0(4) . . . . ? O21 C21 C22 C23 178.6(2) . . . . ? C29A C21 C22 C23 -1.3(4) . . . . ? C21 C22 C23 C23A 4.1(4) . . . . ? C21 C22 C23 S23 -174.8(2) . . . . ? C22 C23 S23 C23B -0.1(3) . . . . ? C23A C23 S23 C23B -179.0(2) . . . . ? C22 C23 C23A C24 176.2(3) . . . . ? S23 C23 C23A C24 -4.8(4) . . . . ? C22 C23 C23A C29B -3.0(4) . . . . ? S23 C23 C23A C29B 175.94(19) . . . . ? C29B C23A C24 C25 0.4(4) . . . . ? C23 C23A C24 C25 -178.9(3) . . . . ? C23A C24 C25 C26 -0.4(5) . . . . ? C24 C25 C26 C26A 0.1(5) . . . . ? C25 C26 C26A C29B 0.2(4) . . . . ? C25 C26 C26A C27 180.0(3) . . . . ? C26 C26A C27 C28 179.4(3) . . . . ? C29B C26A C27 C28 -0.9(4) . . . . ? C26 C26A C27 S27 0.1(4) . . . . ? C29B C26A C27 S27 179.83(19) . . . . ? C28 C27 S27 C27B 3.4(3) . . . . ? C26A C27 S27 C27B -177.3(2) . . . . ? C26A C27 C28 C29 0.6(4) . . . . ? S27 C27 C28 C29 179.9(2) . . . . ? C27 C28 C29 O29 178.8(2) . . . . ? C27 C28 C29 C29A 0.4(4) . . . . ? O21 C21 C29A C29 0.2(4) . . . . ? C22 C21 C29A C29 -180.0(2) . . . . ? O21 C21 C29A C29B 177.4(2) . . . . ? C22 C21 C29A C29B -2.7(4) . . . . ? O29 C29 C29A C21 -2.2(4) . . . . ? C28 C29 C29A C21 176.1(2) . . . . ? O29 C29 C29A C29B -179.5(2) . . . . ? C28 C29 C29A C29B -1.1(4) . . . . ? C24 C23A C29B C29A 179.8(2) . . . . ? C23 C23A C29B C29A -1.0(4) . . . . ? C24 C23A C29B C26A 0.0(4) . . . . ? C23 C23A C29B C26A 179.2(2) . . . . ? C21 C29A C29B C23A 3.8(4) . . . . ? C29 C29A C29B C23A -179.0(2) . . . . ? C21 C29A C29B C26A -176.4(2) . . . . ? C29 C29A C29B C26A 0.8(4) . . . . ? C26 C26A C29B C23A -0.3(4) . . . . ? C27 C26A C29B C23A 179.9(2) . . . . ? C26 C26A C29B C29A 179.9(2) . . . . ? C27 C26A C29B C29A 0.1(4) . . . . ? C29A C29 O29 B2 -10.9(4) . . . . ? C28 C29 O29 B2 170.7(2) . . . . ? O39 B2 O29 C29 143.2(2) . . . . ? O21 B2 O29 C29 24.2(3) . . . . ? O31 B2 O29 C29 -94.3(3) . . . . ? O39 B2 O31 C31 22.2(3) . . . . ? O21 B2 O31 C31 141.8(2) . . . . ? O29 B2 O31 C31 -96.0(2) . . . . ? B2 O31 C31 C39A -10.0(3) . . . . ? B2 O31 C31 C32 170.3(2) . . . . ? O31 C31 C32 C33 179.7(2) . . . . ? C39A C31 C32 C33 0.0(4) . . . . ? C31 C32 C33 C33A -1.6(4) . . . . ? C31 C32 C33 S33 178.23(19) . . . . ? C32 C33 C33A C34 -177.6(2) . . . . ? S33 C33 C33A C34 2.6(3) . . . . ? C32 C33 C33A C39B 2.2(3) . . . . ? S33 C33 C33A C39B -177.72(18) . . . . ? C32 C33 S33 C33B -14.4(3) . . . . ? C33A C33 S33 C33B 165.5(2) . . . . ? C39B C33A C34 C35 -0.6(4) . . . . ? C33 C33A C34 C35 179.1(2) . . . . ? C33A C34 C35 C36 1.9(4) . . . . ? C34 C35 C36 C36A -1.4(4) . . . . ? C35 C36 C36A C39B -0.3(4) . . . . ? C35 C36 C36A C37 -179.7(2) . . . . ? C36 C36A C37 C38 175.9(2) . . . . ? C39B C36A C37 C38 -3.5(3) . . . . ? C36 C36A C37 S37 -4.4(3) . . . . ? C39B C36A C37 S37 176.18(17) . . . . ? C38 C37 S37 C37B 0.0(2) . . . . ? C36A C37 S37 C37B -179.72(19) . . . . ? C36A C37 C38 C39 2.4(4) . . . . ? S37 C37 C38 C39 -177.33(18) . . . . ? C37 C38 C39 O39 -178.6(2) . . . . ? C37 C38 C39 C39A 1.1(4) . . . . ? O31 C31 C39A C39 -1.5(3) . . . . ? C32 C31 C39A C39 178.2(2) . . . . ? O31 C31 C39A C39B -178.6(2) . . . . ? C32 C31 C39A C39B 1.1(4) . . . . ? O39 C39 C39A C31 -0.9(3) . . . . ? C38 C39 C39A C31 179.5(2) . . . . ? O39 C39 C39A C39B 176.2(2) . . . . ? C38 C39 C39A C39B -3.4(3) . . . . ? C31 C39A C39B C36A 179.3(2) . . . . ? C39 C39A C39B C36A 2.2(3) . . . . ? C31 C39A C39B C33A -0.5(3) . . . . ? C39 C39A C39B C33A -177.6(2) . . . . ? C36 C36A C39B C39A -178.2(2) . . . . ? C37 C36A C39B C39A 1.2(3) . . . . ? C36 C36A C39B C33A 1.5(3) . . . . ? C37 C36A C39B C33A -179.0(2) . . . . ? C34 C33A C39B C39A 178.7(2) . . . . ? C33 C33A C39B C39A -1.1(3) . . . . ? C34 C33A C39B C36A -1.1(3) . . . . ? C33 C33A C39B C36A 179.2(2) . . . . ? C38 C39 O39 B2 -165.6(2) . . . . ? C39A C39 O39 B2 14.7(3) . . . . ? O21 B2 O39 C39 -143.3(2) . . . . ? O29 B2 O39 C39 94.7(2) . . . . ? O31 B2 O39 C39 -24.4(3) . . . . ? C1S C2S O3S C4S 175.7(6) . . . . ? C2S O3S C4S C5S -174.5(5) . . . . ? C6S C7S O8S C9S 178.4(4) . . . . ? C7S O8S C9S C10S -179.3(4) . . . . ? C11S C12S O13S C14S 175.3(5) . . . . ? C12S O13S C14S C15S 179.5(4) . . . . ? C9C B3 C1C C6C 25.5(3) . . . . ? C17C B3 C1C C6C -96.2(3) . . . . ? C25C B3 C1C C6C 143.9(2) . . . . ? C9C B3 C1C C2C -159.8(2) . . . . ? C17C B3 C1C C2C 78.5(3) . . . . ? C25C B3 C1C C2C -41.3(3) . . . . ? C6C C1C C2C C3C -0.7(3) . . . . ? B3 C1C C2C C3C -176.0(2) . . . . ? C1C C2C C3C C4C -1.3(4) . . . . ? C1C C2C C3C C7C 179.0(2) . . . . ? C2C C3C C4C C5C 2.0(3) . . . . ? C7C C3C C4C C5C -178.2(2) . . . . ? C3C C4C C5C C6C -0.8(3) . . . . ? C3C C4C C5C C8C 178.1(2) . . . . ? C4C C5C C6C C1C -1.3(4) . . . . ? C8C C5C C6C C1C 179.9(2) . . . . ? C2C C1C C6C C5C 2.0(3) . . . . ? B3 C1C C6C C5C 176.9(2) . . . . ? C4C C3C C7C F1C 133.8(2) . . . . ? C2C C3C C7C F1C -46.4(3) . . . . ? C4C C3C C7C F3C 13.3(3) . . . . ? C2C C3C C7C F3C -167.0(2) . . . . ? C4C C3C C7C F2C -107.0(3) . . . . ? C2C C3C C7C F2C 72.8(3) . . . . ? C4C C5C C8C F5C 131.5(2) . . . . ? C6C C5C C8C F5C -49.6(3) . . . . ? C4C C5C C8C F4C 9.0(3) . . . . ? C6C C5C C8C F4C -172.1(2) . . . . ? C4C C5C C8C F6C -109.3(3) . . . . ? C6C C5C C8C F6C 69.5(3) . . . . ? C1C B3 C9C C14C -155.5(2) . . . . ? C17C B3 C9C C14C -36.9(3) . . . . ? C25C B3 C9C C14C 82.7(2) . . . . ? C1C B3 C9C C10C 29.8(3) . . . . ? C17C B3 C9C C10C 148.4(2) . . . . ? C25C B3 C9C C10C -92.0(3) . . . . ? C14C C9C C10C C11C 1.6(3) . . . . ? B3 C9C C10C C11C 176.5(2) . . . . ? C9C C10C C11C C12C -0.6(4) . . . . ? C9C C10C C11C C15C -179.5(2) . . . . ? C10C C11C C12C C13C -0.3(4) . . . . ? C15C C11C C12C C13C 178.7(2) . . . . ? C11C C12C C13C C14C 0.0(4) . . . . ? C11C C12C C13C C16C 177.9(2) . . . . ? C12C C13C C14C C9C 1.0(4) . . . . ? C16C C13C C14C C9C -176.9(2) . . . . ? C10C C9C C14C C13C -1.8(3) . . . . ? B3 C9C C14C C13C -177.0(2) . . . . ? C12C C11C C15C F7C 155.2(2) . . . . ? C10C C11C C15C F7C -25.9(4) . . . . ? C12C C11C C15C F8C -84.6(3) . . . . ? C10C C11C C15C F8C 94.4(3) . . . . ? C12C C11C C15C F9C 34.8(4) . . . . ? C10C C11C C15C F9C -146.3(3) . . . . ? C12C C13C C16C F11C -110.5(3) . . . . ? C14C C13C C16C F11C 67.4(3) . . . . ? C12C C13C C16C F10C 9.3(3) . . . . ? C14C C13C C16C F10C -172.8(2) . . . . ? C12C C13C C16C F12C 129.6(2) . . . . ? C14C C13C C16C F12C -52.5(3) . . . . ? C1C B3 C17C C18C -84.8(3) . . . . ? C9C B3 C17C C18C 150.2(2) . . . . ? C25C B3 C17C C18C 34.8(3) . . . . ? C1C B3 C17C C22C 93.1(2) . . . . ? C9C B3 C17C C22C -32.0(3) . . . . ? C25C B3 C17C C22C -147.4(2) . . . . ? C22C C17C C18C C19C 0.2(3) . . . . ? B3 C17C C18C C19C 178.2(2) . . . . ? C17C C18C C19C C20C 1.8(4) . . . . ? C17C C18C C19C C23C -174.7(4) . . . . ? C17C C18C C19C C23D 171.3(6) . . . . ? C18C C19C C20C C21C -2.0(4) . . . . ? C23C C19C C20C C21C 174.8(4) . . . . ? C23D C19C C20C C21C -170.1(6) . . . . ? C19C C20C C21C C22C 0.0(4) . . . . ? C19C C20C C21C C24C 177.9(2) . . . . ? C20C C21C C22C C17C 2.1(4) . . . . ? C24C C21C C22C C17C -175.7(2) . . . . ? C18C C17C C22C C21C -2.2(3) . . . . ? B3 C17C C22C C21C 179.9(2) . . . . ? C20C C19C C23C F15C 95.1(6) . . . . ? C18C C19C C23C F15C -88.3(7) . . . . ? C23D C19C C23C F15C -30(2) . . . . ? C20C C19C C23C F13C -144.1(5) . . . . ? C18C C19C C23C F13C 32.6(8) . . . . ? C23D C19C C23C F13C 90(2) . . . . ? C20C C19C C23C F14C -23.8(7) . . . . ? C18C C19C C23C F14C 152.9(6) . . . . ? C23D C19C C23C F14C -149(3) . . . . ? C20C C19C C23D F14D -7.9(10) . . . . ? C18C C19C C23D F14D -176.9(8) . . . . ? C23C C19C C23D F14D 54(2) . . . . ? C20C C19C C23D F15D 116.3(8) . . . . ? C18C C19C C23D F15D -52.6(12) . . . . ? C23C C19C C23D F15D 179(3) . . . . ? C20C C19C C23D F13D -124.0(8) . . . . ? C18C C19C C23D F13D 67.0(11) . . . . ? C23C C19C C23D F13D -62(2) . . . . ? C20C C21C C24C F18C -176.4(2) . . . . ? C22C C21C C24C F18C 1.5(3) . . . . ? C20C C21C C24C F17C -55.5(3) . . . . ? C22C C21C C24C F17C 122.3(3) . . . . ? C20C C21C C24C F16C 62.6(3) . . . . ? C22C C21C C24C F16C -119.6(3) . . . . ? C1C B3 C25C C30C 156.0(2) . . . . ? C9C B3 C25C C30C -79.0(3) . . . . ? C17C B3 C25C C30C 40.1(3) . . . . ? C1C B3 C25C C26C -29.2(3) . . . . ? C9C B3 C25C C26C 95.8(3) . . . . ? C17C B3 C25C C26C -145.2(2) . . . . ? C30C C25C C26C C27C -0.1(4) . . . . ? B3 C25C C26C C27C -175.1(3) . . . . ? C25C C26C C27C C28C 0.0(5) . . . . ? C25C C26C C27C C31C 177.5(4) . . . . ? C25C C26C C27C C31D -171.8(5) . . . . ? C26C C27C C28C C29C 0.4(5) . . . . ? C31C C27C C28C C29C -177.3(4) . . . . ? C31D C27C C28C C29C 171.1(6) . . . . ? C27C C28C C29C C30C -0.7(5) . . . . ? C27C C28C C29C C32D -170.9(6) . . . . ? C27C C28C C29C C32C 175.3(5) . . . . ? C27C C28C C29C C32E -177.2(7) . . . . ? C28C C29C C30C C25C 0.6(4) . . . . ? C32D C29C C30C C25C 170.9(5) . . . . ? C32C C29C C30C C25C -175.1(5) . . . . ? C32E C29C C30C C25C 177.5(6) . . . . ? C26C C25C C30C C29C -0.2(4) . . . . ? B3 C25C C30C C29C 175.0(2) . . . . ? C28C C27C C31C F20C -68.5(7) . . . . ? C26C C27C C31C F20C 113.9(6) . . . . ? C31D C27C C31C F20C 67(3) . . . . ? C28C C27C C31C F21C 52.1(7) . . . . ? C26C C27C C31C F21C -125.5(6) . . . . ? C31D C27C C31C F21C -172(3) . . . . ? C28C C27C C31C F19C 172.5(6) . . . . ? C26C C27C C31C F19C -5.2(9) . . . . ? C31D C27C C31C F19C -52(3) . . . . ? C28C C27C C31D F21D 17.0(11) . . . . ? C26C C27C C31D F21D -171.6(9) . . . . ? C31C C27C C31D F21D -33(2) . . . . ? C28C C27C C31D F20D -104.3(10) . . . . ? C26C C27C C31D F20D 67.1(11) . . . . ? C31C C27C C31D F20D -154(3) . . . . ? C28C C27C C31D F19D 135.0(9) . . . . ? C26C C27C C31D F19D -53.6(11) . . . . ? C31C C27C C31D F19D 85(3) . . . . ? C28C C29C C32C F22C 69.7(9) . . . . ? C30C C29C C32C F22C -114.4(8) . . . . ? C32D C29C C32C F22C -36(3) . . . . ? C32E C29C C32C F22C -75(4) . . . . ? C28C C29C C32C F23C -50.0(10) . . . . ? C30C C29C C32C F23C 125.9(8) . . . . ? C32D C29C C32C F23C -156(4) . . . . ? C32E C29C C32C F23C 165(5) . . . . ? C28C C29C C32C F24C -172.4(7) . . . . ? C30C C29C C32C F24C 3.5(9) . . . . ? C32D C29C C32C F24C 82(3) . . . . ? C32E C29C C32C F24C 42(4) . . . . ? C28C C29C C32D F23D 14.0(12) . . . . ? C30C C29C C32D F23D -156.5(9) . . . . ? C32C C29C C32D F23D 94(4) . . . . ? C32E C29C C32D F23D 153(6) . . . . ? C28C C29C C32D F24D -104.1(10) . . . . ? C30C C29C C32D F24D 85.4(10) . . . . ? C32C C29C C32D F24D -24(3) . . . . ? C32E C29C C32D F24D 35(5) . . . . ? C28C C29C C32D F22D 137.8(9) . . . . ? C30C C29C C32D F22D -32.7(12) . . . . ? C32C C29C C32D F22D -142(4) . . . . ? C32E C29C C32D F22D -83(6) . . . . ? C28C C29C C32E F23E -22.8(14) . . . . ? C30C C29C C32E F23E 160.4(10) . . . . ? C32D C29C C32E F23E -67(5) . . . . ? C32C C29C C32E F23E 16(4) . . . . ? C28C C29C C32E F24E -142.4(11) . . . . ? C30C C29C C32E F24E 40.8(13) . . . . ? C32D C29C C32E F24E 173(6) . . . . ? C32C C29C C32E F24E -104(5) . . . . ? C28C C29C C32E F22E 96.1(12) . . . . ? C30C C29C C32E F22E -80.7(13) . . . . ? C32D C29C C32E F22E 52(5) . . . . ? C32C C29C C32E F22E 135(5) . . . . ? C9F B4 C1F C6F 94.6(3) . . . . ? C17F B4 C1F C6F -27.0(3) . . . . ? C25F B4 C1F C6F -148.6(2) . . . . ? C9F B4 C1F C2F -85.4(3) . . . . ? C17F B4 C1F C2F 153.0(2) . . . . ? C25F B4 C1F C2F 31.4(3) . . . . ? C6F C1F C2F C3F 0.9(4) . . . . ? B4 C1F C2F C3F -179.0(2) . . . . ? C1F C2F C3F C4F -1.1(4) . . . . ? C1F C2F C3F C7F 175.7(2) . . . . ? C2F C3F C4F C5F 0.6(4) . . . . ? C7F C3F C4F C5F -176.3(3) . . . . ? C3F C4F C5F C6F -0.1(4) . . . . ? C3F C4F C5F C8F 176.1(3) . . . . ? C4F C5F C6F C1F 0.0(4) . . . . ? C8F C5F C6F C1F -176.1(3) . . . . ? C2F C1F C6F C5F -0.4(4) . . . . ? B4 C1F C6F C5F 179.6(2) . . . . ? C4F C3F C7F F2F 78.2(3) . . . . ? C2F C3F C7F F2F -98.7(3) . . . . ? C4F C3F C7F F1F -160.6(2) . . . . ? C2F C3F C7F F1F 22.5(4) . . . . ? C4F C3F C7F F3F -40.4(3) . . . . ? C2F C3F C7F F3F 142.7(2) . . . . ? C4F C5F C8F F6F 166.5(3) . . . . ? C6F C5F C8F F6F -17.3(5) . . . . ? C4F C5F C8F F5F 44.1(4) . . . . ? C6F C5F C8F F5F -139.8(3) . . . . ? C4F C5F C8F F4F -73.0(4) . . . . ? C6F C5F C8F F4F 103.2(4) . . . . ? C17F B4 C9F C14F -43.6(3) . . . . ? C25F B4 C9F C14F 78.5(3) . . . . ? C1F B4 C9F C14F -164.0(2) . . . . ? C17F B4 C9F C10F 146.7(2) . . . . ? C25F B4 C9F C10F -91.2(3) . . . . ? C1F B4 C9F C10F 26.3(3) . . . . ? C14F C9F C10F C11F -1.9(3) . . . . ? B4 C9F C10F C11F 168.2(2) . . . . ? C9F C10F C11F C12F 0.3(3) . . . . ? C9F C10F C11F C15F -179.4(2) . . . . ? C10F C11F C12F C13F 0.8(4) . . . . ? C15F C11F C12F C13F -179.5(2) . . . . ? C11F C12F C13F C14F -0.3(4) . . . . ? C11F C12F C13F C16F -178.5(2) . . . . ? C12F C13F C14F C9F -1.4(4) . . . . ? C16F C13F C14F C9F 176.9(2) . . . . ? C10F C9F C14F C13F 2.4(3) . . . . ? B4 C9F C14F C13F -168.0(2) . . . . ? C12F C11F C15F F7F -171.3(2) . . . . ? C10F C11F C15F F7F 8.4(3) . . . . ? C12F C11F C15F F9F 68.2(3) . . . . ? C10F C11F C15F F9F -112.0(3) . . . . ? C12F C11F C15F F8F -50.1(3) . . . . ? C10F C11F C15F F8F 129.6(2) . . . . ? C12F C13F C16F F11F 1.4(4) . . . . ? C14F C13F C16F F11F -176.9(3) . . . . ? C12F C13F C16F F12F -122.0(3) . . . . ? C14F C13F C16F F12F 59.7(3) . . . . ? C12F C13F C16F F10F 123.4(3) . . . . ? C14F C13F C16F F10F -54.9(3) . . . . ? C9F B4 C17F C22F 137.6(2) . . . . ? C25F B4 C17F C22F 18.6(3) . . . . ? C1F B4 C17F C22F -100.3(3) . . . . ? C9F B4 C17F C18F -46.0(3) . . . . ? C25F B4 C17F C18F -165.0(2) . . . . ? C1F B4 C17F C18F 76.0(3) . . . . ? C22F C17F C18F C19F 2.5(4) . . . . ? B4 C17F C18F C19F -174.1(2) . . . . ? C17F C18F C19F C20F -2.0(4) . . . . ? C17F C18F C19F C23F 174.9(3) . . . . ? C18F C19F C20F C21F -0.3(4) . . . . ? C23F C19F C20F C21F -177.2(3) . . . . ? C19F C20F C21F C22F 1.7(4) . . . . ? C19F C20F C21F C24G 173.9(7) . . . . ? C19F C20F C21F C24H -176.5(6) . . . . ? C19F C20F C21F C24F -177.9(5) . . . . ? C18F C17F C22F C21F -1.1(4) . . . . ? B4 C17F C22F C21F 175.5(2) . . . . ? C20F C21F C22F C17F -1.0(4) . . . . ? C24G C21F C22F C17F -172.3(8) . . . . ? C24H C21F C22F C17F 177.1(6) . . . . ? C24F C21F C22F C17F 178.6(5) . . . . ? C20F C19F C23F F15F -20.7(5) . . . . ? C18F C19F C23F F15F 162.4(3) . . . . ? C20F C19F C23F F14F -140.2(3) . . . . ? C18F C19F C23F F14F 42.9(4) . . . . ? C20F C19F C23F F13F 103.5(4) . . . . ? C18F C19F C23F F13F -73.4(4) . . . . ? C20F C21F C24F F18F 164.8(6) . . . . ? C22F C21F C24F F18F -14.8(10) . . . . ? C24G C21F C24F F18F -151(4) . . . . ? C24H C21F C24F F18F 150(11) . . . . ? C20F C21F C24F F17F -74.0(8) . . . . ? C22F C21F C24F F17F 106.4(7) . . . . ? C24G C21F C24F F17F -29(4) . . . . ? C24H C21F C24F F17F -89(10) . . . . ? C20F C21F C24F F16F 42.7(9) . . . . ? C22F C21F C24F F16F -136.9(7) . . . . ? C24G C21F C24F F16F 87(4) . . . . ? C24H C21F C24F F16F 28(10) . . . . ? C20F C21F C24G F17G -127.6(16) . . . . ? C22F C21F C24G F17G 44.2(17) . . . . ? C24H C21F C24G F17G 120(5) . . . . ? C24F C21F C24G F17G 93(4) . . . . ? C20F C21F C24G F16G -4.9(19) . . . . ? C22F C21F C24G F16G 167.0(15) . . . . ? C24H C21F C24G F16G -117(5) . . . . ? C24F C21F C24G F16G -144(5) . . . . ? C20F C21F C24G F18G 115.5(16) . . . . ? C22F C21F C24G F18G -72.7(16) . . . . ? C24H C21F C24G F18G 3(5) . . . . ? C24F C21F C24G F18G -24(4) . . . . ? C20F C21F C24H F17H -169.9(10) . . . . ? C22F C21F C24H F17H 12.0(14) . . . . ? C24G C21F C24H F17H -98(5) . . . . ? C24F C21F C24H F17H -4(9) . . . . ? C20F C21F C24H F18H 67.7(11) . . . . ? C22F C21F C24H F18H -110.5(10) . . . . ? C24G C21F C24H F18H 140(5) . . . . ? C24F C21F C24H F18H -127(10) . . . . ? C20F C21F C24H F16H -55.2(12) . . . . ? C22F C21F C24H F16H 126.6(10) . . . . ? C24G C21F C24H F16H 17(4) . . . . ? C24F C21F C24H F16H 111(10) . . . . ? C9F B4 C25F C26F 167.7(2) . . . . ? C17F B4 C25F C26F -71.2(3) . . . . ? C1F B4 C25F C26F 48.1(3) . . . . ? C9F B4 C25F C30F -8.1(3) . . . . ? C17F B4 C25F C30F 113.0(3) . . . . ? C1F B4 C25F C30F -127.7(2) . . . . ? C30F C25F C26F C27F 0.4(4) . . . . ? B4 C25F C26F C27F -175.7(2) . . . . ? C25F C26F C27F C28F 0.8(4) . . . . ? C25F C26F C27F C31G -178.4(7) . . . . ? C25F C26F C27F C31H -175(3) . . . . ? C25F C26F C27F C31F -179.6(5) . . . . ? C26F C27F C28F C29F -1.3(4) . . . . ? C31G C27F C28F C29F 177.9(7) . . . . ? C31H C27F C28F C29F 175(3) . . . . ? C31F C27F C28F C29F 179.1(5) . . . . ? C27F C28F C29F C30F 0.6(4) . . . . ? C27F C28F C29F C32F -179.9(3) . . . . ? C28F C29F C30F C25F 0.6(4) . . . . ? C32F C29F C30F C25F -179.0(2) . . . . ? C26F C25F C30F C29F -1.1(4) . . . . ? B4 C25F C30F C29F 175.0(2) . . . . ? C28F C27F C31F F19F 131.1(7) . . . . ? C26F C27F C31F F19F -48.5(9) . . . . ? C31G C27F C31F F19F 144(10) . . . . ? C31H C27F C31F F19F 154(14) . . . . ? C28F C27F C31F F21F 11.3(10) . . . . ? C26F C27F C31F F21F -168.3(6) . . . . ? C31G C27F C31F F21F 24(9) . . . . ? C31H C27F C31F F21F 35(14) . . . . ? C28F C27F C31F F20F -109.4(7) . . . . ? C26F C27F C31F F20F 71.0(8) . . . . ? C31G C27F C31F F20F -97(9) . . . . ? C31H C27F C31F F20F -86(14) . . . . ? C28F C27F C31G F21G 37.1(12) . . . . ? C26F C27F C31G F21G -143.8(10) . . . . ? C31H C27F C31G F21G 69(25) . . . . ? C31F C27F C31G F21G -131(10) . . . . ? C28F C27F C31G F19G 159.7(9) . . . . ? C26F C27F C31G F19G -21.1(13) . . . . ? C31H C27F C31G F19G -169(25) . . . . ? C31F C27F C31G F19G -8(9) . . . . ? C28F C27F C31G F20G -81.0(11) . . . . ? C26F C27F C31G F20G 98.2(11) . . . . ? C31H C27F C31G F20G -49(25) . . . . ? C31F C27F C31G F20G 111(9) . . . . ? C28F C27F C31H F21H 91(7) . . . . ? C26F C27F C31H F21H -94(7) . . . . ? C31G C27F C31H F21H -59(23) . . . . ? C31F C27F C31H F21H -68(14) . . . . ? C28F C27F C31H F20H -36(4) . . . . ? C26F C27F C31H F20H 140(3) . . . . ? C31G C27F C31H F20H 174(28) . . . . ? C31F C27F C31H F20H 165(17) . . . . ? C28F C27F C31H F19H -150(4) . . . . ? C26F C27F C31H F19H 26(6) . . . . ? C31G C27F C31H F19H 61(24) . . . . ? C31F C27F C31H F19H 52(12) . . . . ? C28F C29F C32F F22F 106.9(3) . . . . ? C30F C29F C32F F22F -73.5(3) . . . . ? C28F C29F C32F F23F -14.1(4) . . . . ? C30F C29F C32F F23F 165.5(3) . . . . ? C28F C29F C32F F24F -134.5(3) . . . . ? C30F C29F C32F F24F 45.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.684 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.063 # Attachment '- rh173_0m.cif' data_rh173_0m _database_code_depnum_ccdc_archive 'CCDC 867316' #TrackingRef '- rh173_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 B O4 S4' _chemical_formula_weight 641.63 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_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' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.019(4) _cell_length_b 8.5496(16) _cell_length_c 18.248(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.965(4) _cell_angle_gamma 90.00 _cell_volume 2838.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5192 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 32.22 _exptl_crystal_description 'prism frag' _exptl_crystal_colour black _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 0.377 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9474 _exptl_absorpt_correction_T_max 0.9785 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22496 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 30.50 _reflns_number_total 4325 _reflns_number_gt 3506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+2.2960P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4325 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 1.0000 0.8540(3) 0.7500 0.0114(4) Uani 1 2 d S . . O1 O 1.03846(5) 0.75300(12) 0.81448(5) 0.01212(19) Uani 1 1 d . . . C1 C 1.02489(7) 0.75665(15) 0.88228(7) 0.0099(2) Uani 1 1 d . . . C2 C 1.06861(7) 0.66668(16) 0.94236(7) 0.0113(2) Uani 1 1 d . . . H2 H 1.1079 0.6065 0.9348 0.014 Uiso 1 1 calc R . . C3 C 1.05482(7) 0.66483(15) 1.01306(7) 0.0106(2) Uani 1 1 d . . . C3A C 0.99498(7) 0.75412(15) 1.02549(7) 0.0101(2) Uani 1 1 d . . . C4 C 0.97814(7) 0.75478(16) 1.09570(7) 0.0124(3) Uani 1 1 d . . . H4 H 1.0070 0.6942 1.1373 0.015 Uiso 1 1 calc R . . C5 C 0.92003(7) 0.84254(16) 1.10498(8) 0.0129(3) Uani 1 1 d . . . H5 H 0.9092 0.8405 1.1526 0.015 Uiso 1 1 calc R . . C6 C 0.87750(7) 0.93327(16) 1.04545(8) 0.0122(2) Uani 1 1 d . . . H6 H 0.8383 0.9938 1.0531 0.015 Uiso 1 1 calc R . . C6A C 0.89163(7) 0.93689(15) 0.97364(7) 0.0102(2) Uani 1 1 d . . . C7 C 0.84852(7) 1.02730(15) 0.90956(8) 0.0107(2) Uani 1 1 d . . . C8 C 0.86646(7) 1.03140(16) 0.84123(7) 0.0112(2) Uani 1 1 d . . . H8 H 0.8382 1.0935 0.8000 0.013 Uiso 1 1 calc R . . C9 C 0.92598(7) 0.94455(15) 0.83260(7) 0.0100(2) Uani 1 1 d . . . C9A C 0.96687(7) 0.84825(15) 0.89254(7) 0.0099(2) Uani 1 1 d . . . C9B C 0.95113(7) 0.84638(15) 0.96393(7) 0.0099(2) Uani 1 1 d . . . O9 O 0.94353(5) 0.95411(11) 0.76688(5) 0.01201(19) Uani 1 1 d . . . S3 S 1.107515(18) 0.55648(4) 1.090885(18) 0.01254(9) Uani 1 1 d . . . C10 C 1.17339(7) 0.45487(16) 1.05390(8) 0.0135(3) Uani 1 1 d . . . H10A H 1.1475 0.3848 1.0114 0.016 Uiso 1 1 calc R . . H10B H 1.2025 0.5311 1.0341 0.016 Uiso 1 1 calc R . . C11 C 1.22396(8) 0.35963(17) 1.11896(9) 0.0174(3) Uani 1 1 d . . . H11A H 1.2540 0.4307 1.1578 0.026 Uiso 1 1 calc R . . H11B H 1.2561 0.2938 1.0987 0.026 Uiso 1 1 calc R . . H11C H 1.1943 0.2933 1.1422 0.026 Uiso 1 1 calc R . . S7 S 0.774652(18) 1.13233(4) 0.925002(19) 0.01306(9) Uani 1 1 d . . . C12 C 0.71505(8) 1.17936(18) 0.83087(8) 0.0167(3) Uani 1 1 d . . . H12A H 0.6795 1.2604 0.8358 0.020 Uiso 1 1 calc R . . H12B H 0.7450 1.2239 0.7998 0.020 Uiso 1 1 calc R . . C13 C 0.67302(9) 1.0391(2) 0.78928(9) 0.0249(3) Uani 1 1 d . . . H13A H 0.7075 0.9643 0.7781 0.037 Uiso 1 1 calc R . . H13B H 0.6378 1.0735 0.7413 0.037 Uiso 1 1 calc R . . H13C H 0.6465 0.9889 0.8217 0.037 Uiso 1 1 calc R . . 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 B1 0.0101(9) 0.0168(10) 0.0084(9) 0.000 0.0046(7) 0.000 O1 0.0118(4) 0.0179(5) 0.0079(4) 0.0015(4) 0.0048(3) 0.0036(4) C1 0.0101(5) 0.0121(6) 0.0083(5) -0.0007(4) 0.0038(4) -0.0014(4) C2 0.0100(6) 0.0139(6) 0.0107(6) 0.0009(5) 0.0042(5) 0.0010(5) C3 0.0108(6) 0.0116(6) 0.0089(6) 0.0008(4) 0.0018(5) -0.0005(5) C3A 0.0096(6) 0.0121(6) 0.0088(5) -0.0002(4) 0.0028(4) -0.0011(4) C4 0.0122(6) 0.0161(6) 0.0088(6) 0.0007(5) 0.0030(5) -0.0003(5) C5 0.0135(6) 0.0171(6) 0.0094(6) -0.0004(5) 0.0056(5) -0.0011(5) C6 0.0120(6) 0.0148(6) 0.0114(6) -0.0017(5) 0.0061(5) -0.0001(5) C6A 0.0099(5) 0.0122(6) 0.0093(5) -0.0007(5) 0.0037(4) -0.0013(5) C7 0.0090(5) 0.0111(6) 0.0130(6) -0.0012(5) 0.0047(5) 0.0001(4) C8 0.0095(6) 0.0137(6) 0.0100(6) 0.0013(5) 0.0022(5) 0.0006(5) C9 0.0093(5) 0.0131(6) 0.0084(5) -0.0009(5) 0.0035(4) -0.0020(5) C9A 0.0084(5) 0.0124(6) 0.0089(5) -0.0004(4) 0.0027(4) -0.0004(4) C9B 0.0092(5) 0.0117(6) 0.0094(6) -0.0008(4) 0.0038(4) -0.0014(4) O9 0.0121(4) 0.0173(5) 0.0082(4) 0.0018(3) 0.0053(3) 0.0027(4) S3 0.01266(16) 0.01531(17) 0.00991(15) 0.00307(12) 0.00369(12) 0.00269(12) C10 0.0121(6) 0.0154(6) 0.0140(6) 0.0019(5) 0.0053(5) 0.0017(5) C11 0.0148(6) 0.0172(7) 0.0191(7) 0.0035(5) 0.0032(5) 0.0031(5) S7 0.01110(15) 0.01701(17) 0.01215(16) -0.00051(12) 0.00510(12) 0.00306(12) C12 0.0138(6) 0.0233(7) 0.0135(6) 0.0024(5) 0.0049(5) 0.0061(5) C13 0.0171(7) 0.0361(9) 0.0199(7) -0.0097(7) 0.0028(6) 0.0007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 B1 O1 1.4705(16) 2_756 ? B1 O1 1.4705(16) . ? B1 O9 1.4747(16) 2_756 ? B1 O9 1.4747(16) . ? O1 C1 1.3361(15) . ? C1 C2 1.3975(18) . ? C1 C9A 1.4093(18) . ? C2 C3 1.3897(18) . ? C2 H2 0.9500 . ? C3 C3A 1.4423(18) . ? C3 S3 1.7461(13) . ? C3A C4 1.4083(18) . ? C3A C9B 1.4258(18) . ? C4 C5 1.3865(19) . ? C4 H4 0.9500 . ? C5 C6 1.3868(19) . ? C5 H5 0.9500 . ? C6 C6A 1.4128(18) . ? C6 H6 0.9500 . ? C6A C9B 1.4241(18) . ? C6A C7 1.4413(18) . ? C7 C8 1.3858(18) . ? C7 S7 1.7580(13) . ? C8 C9 1.4007(18) . ? C8 H8 0.9500 . ? C9 O9 1.3379(15) . ? C9 C9A 1.4080(18) . ? C9A C9B 1.4193(18) . ? S3 C10 1.8092(14) . ? C10 C11 1.5269(19) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? S7 C12 1.8059(15) . ? C12 C13 1.516(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? 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 O1 B1 O1 108.10(16) 2_756 . ? O1 B1 O9 113.35(5) 2_756 2_756 ? O1 B1 O9 106.58(5) . 2_756 ? O1 B1 O9 106.58(5) 2_756 . ? O1 B1 O9 113.35(5) . . ? O9 B1 O9 109.01(16) 2_756 . ? C1 O1 B1 122.81(10) . . ? O1 C1 C2 118.82(12) . . ? O1 C1 C9A 120.42(12) . . ? C2 C1 C9A 120.76(12) . . ? C3 C2 C1 120.28(12) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C3A 120.76(12) . . ? C2 C3 S3 122.83(10) . . ? C3A C3 S3 116.42(10) . . ? C4 C3A C9B 118.59(12) . . ? C4 C3A C3 122.99(12) . . ? C9B C3A C3 118.41(11) . . ? C5 C4 C3A 120.95(12) . . ? C5 C4 H4 119.5 . . ? C3A C4 H4 119.5 . . ? C4 C5 C6 120.69(12) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C6A 120.91(12) . . ? C5 C6 H6 119.5 . . ? C6A C6 H6 119.5 . . ? C6 C6A C9B 118.46(12) . . ? C6 C6A C7 123.17(12) . . ? C9B C6A C7 118.36(11) . . ? C8 C7 C6A 120.83(12) . . ? C8 C7 S7 123.32(10) . . ? C6A C7 S7 115.84(10) . . ? C7 C8 C9 120.46(12) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? O9 C9 C8 119.31(11) . . ? O9 C9 C9A 120.42(11) . . ? C8 C9 C9A 120.27(12) . . ? C9 C9A C1 119.88(12) . . ? C9 C9A C9B 120.19(12) . . ? C1 C9A C9B 119.91(12) . . ? C9A C9B C6A 119.75(12) . . ? C9A C9B C3A 119.86(12) . . ? C6A C9B C3A 120.39(12) . . ? C9 O9 B1 122.62(10) . . ? C3 S3 C10 104.30(6) . . ? C11 C10 S3 108.28(10) . . ? C11 C10 H10A 110.0 . . ? S3 C10 H10A 110.0 . . ? C11 C10 H10B 110.0 . . ? S3 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 S7 C12 105.69(7) . . ? C13 C12 S7 113.14(11) . . ? C13 C12 H12A 109.0 . . ? S7 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? S7 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 B1 O1 C1 -120.12(12) 2_756 . . . ? O9 B1 O1 C1 117.71(11) 2_756 . . . ? O9 B1 O1 C1 -2.21(18) . . . . ? B1 O1 C1 C2 -174.35(12) . . . . ? B1 O1 C1 C9A 6.43(19) . . . . ? O1 C1 C2 C3 -178.41(12) . . . . ? C9A C1 C2 C3 0.8(2) . . . . ? C1 C2 C3 C3A 0.6(2) . . . . ? C1 C2 C3 S3 -179.51(10) . . . . ? C2 C3 C3A C4 179.22(13) . . . . ? S3 C3 C3A C4 -0.69(18) . . . . ? C2 C3 C3A C9B -1.06(19) . . . . ? S3 C3 C3A C9B 179.03(10) . . . . ? C9B C3A C4 C5 0.3(2) . . . . ? C3 C3A C4 C5 179.99(13) . . . . ? C3A C4 C5 C6 -0.7(2) . . . . ? C4 C5 C6 C6A 0.9(2) . . . . ? C5 C6 C6A C9B -0.7(2) . . . . ? C5 C6 C6A C7 179.08(13) . . . . ? C6 C6A C7 C8 177.53(13) . . . . ? C9B C6A C7 C8 -2.73(19) . . . . ? C6 C6A C7 S7 -1.21(17) . . . . ? C9B C6A C7 S7 178.52(10) . . . . ? C6A C7 C8 C9 1.5(2) . . . . ? S7 C7 C8 C9 -179.85(10) . . . . ? C7 C8 C9 O9 -178.02(12) . . . . ? C7 C8 C9 C9A 2.0(2) . . . . ? O9 C9 C9A C1 -2.45(19) . . . . ? C8 C9 C9A C1 177.56(12) . . . . ? O9 C9 C9A C9B 175.84(12) . . . . ? C8 C9 C9A C9B -4.16(19) . . . . ? O1 C1 C9A C9 -4.20(19) . . . . ? C2 C1 C9A C9 176.59(12) . . . . ? O1 C1 C9A C9B 177.50(12) . . . . ? C2 C1 C9A C9B -1.70(19) . . . . ? C9 C9A C9B C6A 2.84(19) . . . . ? C1 C9A C9B C6A -178.87(12) . . . . ? C9 C9A C9B C3A -177.09(12) . . . . ? C1 C9A C9B C3A 1.20(19) . . . . ? C6 C6A C9B C9A -179.70(12) . . . . ? C7 C6A C9B C9A 0.55(18) . . . . ? C6 C6A C9B C3A 0.23(19) . . . . ? C7 C6A C9B C3A -179.52(12) . . . . ? C4 C3A C9B C9A 179.89(12) . . . . ? C3 C3A C9B C9A 0.16(19) . . . . ? C4 C3A C9B C6A -0.04(19) . . . . ? C3 C3A C9B C6A -179.78(12) . . . . ? C8 C9 O9 B1 -173.18(12) . . . . ? C9A C9 O9 B1 6.83(19) . . . . ? O1 B1 O9 C9 114.25(11) 2_756 . . . ? O1 B1 O9 C9 -4.54(18) . . . . ? O9 B1 O9 C9 -123.07(12) 2_756 . . . ? C2 C3 S3 C10 -2.34(13) . . . . ? C3A C3 S3 C10 177.57(10) . . . . ? C3 S3 C10 C11 178.37(10) . . . . ? C8 C7 S7 C12 19.34(14) . . . . ? C6A C7 S7 C12 -161.95(10) . . . . ? C7 S7 C12 C13 72.84(12) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.554 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.071 # Attachment '- rh173_296K_0m.cif' data_rh173_296k_0m _database_code_depnum_ccdc_archive 'CCDC 867317' #TrackingRef '- rh173_296K_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 B O4 S4' _chemical_formula_weight 641.63 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_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' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.171(3) _cell_length_b 8.6743(15) _cell_length_c 18.273(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.829(3) _cell_angle_gamma 90.00 _cell_volume 2908.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2618 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.43 _exptl_crystal_description 'prism frag' _exptl_crystal_colour black _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 0.368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9486 _exptl_absorpt_correction_T_max 0.9790 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16785 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 30.02 _reflns_number_total 4247 _reflns_number_gt 2944 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.8634P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4247 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 1.0000 0.6466(4) 0.7500 0.0273(6) Uani 1 2 d S . . O1 O 1.03804(7) 0.74548(16) 0.81438(6) 0.0304(3) Uani 1 1 d . . . C1 C 1.02459(9) 0.7420(2) 0.88209(9) 0.0239(4) Uani 1 1 d . . . C2 C 1.06774(10) 0.8306(2) 0.94187(9) 0.0262(4) Uani 1 1 d . . . H2 H 1.1059 0.8886 0.9344 0.031 Uiso 1 1 calc R . . C3 C 1.05401(9) 0.8327(2) 1.01239(9) 0.0248(4) Uani 1 1 d . . . C3A C 0.99504(9) 0.7444(2) 1.02499(9) 0.0241(4) Uani 1 1 d . . . C4 C 0.97809(10) 0.7432(2) 1.09508(10) 0.0299(4) Uani 1 1 d . . . H4 H 1.0059 0.8016 1.1358 0.036 Uiso 1 1 calc R . . C5 C 0.92092(10) 0.6568(2) 1.10427(10) 0.0309(4) Uani 1 1 d . . . H5 H 0.9106 0.6583 1.1509 0.037 Uiso 1 1 calc R . . C6 C 0.87880(10) 0.5682(2) 1.04515(10) 0.0291(4) Uani 1 1 d . . . H6 H 0.8408 0.5099 1.0527 0.035 Uiso 1 1 calc R . . C6A C 0.89260(9) 0.5648(2) 0.97335(9) 0.0244(4) Uani 1 1 d . . . C7 C 0.84958(9) 0.4762(2) 0.90955(10) 0.0250(4) Uani 1 1 d . . . C8 C 0.86766(9) 0.4726(2) 0.84144(10) 0.0269(4) Uani 1 1 d . . . H8 H 0.8402 0.4127 0.8011 0.032 Uiso 1 1 calc R . . C9 C 0.92647(9) 0.5574(2) 0.83244(9) 0.0233(3) Uani 1 1 d . . . C9A C 0.96721(9) 0.6517(2) 0.89237(9) 0.0219(3) Uani 1 1 d . . . C9B C 0.95143(9) 0.6535(2) 0.96356(9) 0.0217(3) Uani 1 1 d . . . S3 S 1.10601(3) 0.94065(6) 1.08965(3) 0.03251(14) Uani 1 1 d . . . O9 O 0.94406(7) 0.54791(15) 0.76705(6) 0.0300(3) Uani 1 1 d . . . C10 C 1.17181(11) 1.0396(2) 1.05297(11) 0.0333(4) Uani 1 1 d . . . H10A H 1.1999 0.9655 1.0335 0.040 Uiso 1 1 calc R . . H10B H 1.1470 1.1076 1.0114 0.040 Uiso 1 1 calc R . . C11 C 1.22205(12) 1.1326(3) 1.11734(13) 0.0450(5) Uani 1 1 d . . . H11A H 1.1935 1.1990 1.1394 0.067 Uiso 1 1 calc R . . H11B H 1.2542 1.1937 1.0975 0.067 Uiso 1 1 calc R . . H11C H 1.2502 1.0638 1.1558 0.067 Uiso 1 1 calc R . . S7 S 0.77600(3) 0.37277(6) 0.92452(3) 0.03451(14) Uani 1 1 d . . . C12 C 0.71538(11) 0.3338(3) 0.83119(12) 0.0445(5) Uani 1 1 d . . . H12A H 0.7434 0.2926 0.7992 0.053 Uiso 1 1 calc R . . H12B H 0.6808 0.2554 0.8356 0.053 Uiso 1 1 calc R . . C13 C 0.67434(14) 0.4724(4) 0.79296(16) 0.0685(8) Uani 1 1 d . . . H13A H 0.6484 0.5172 0.8255 0.103 Uiso 1 1 calc R . . H13B H 0.6403 0.4424 0.7453 0.103 Uiso 1 1 calc R . . H13C H 0.7079 0.5465 0.7836 0.103 Uiso 1 1 calc R . . 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 B1 0.0247(14) 0.0396(17) 0.0205(12) 0.000 0.0112(11) 0.000 O1 0.0293(7) 0.0456(8) 0.0202(6) -0.0028(5) 0.0132(5) -0.0094(6) C1 0.0224(8) 0.0316(9) 0.0192(7) 0.0008(6) 0.0083(6) 0.0014(7) C2 0.0231(9) 0.0335(10) 0.0240(8) -0.0006(7) 0.0101(7) -0.0027(7) C3 0.0234(9) 0.0283(9) 0.0227(8) -0.0022(7) 0.0068(7) 0.0012(7) C3A 0.0236(9) 0.0300(9) 0.0196(7) 0.0007(6) 0.0074(6) 0.0036(7) C4 0.0311(10) 0.0388(11) 0.0209(8) -0.0024(7) 0.0090(7) 0.0025(8) C5 0.0335(10) 0.0423(11) 0.0210(8) 0.0017(7) 0.0143(7) 0.0030(8) C6 0.0275(9) 0.0367(10) 0.0279(9) 0.0023(7) 0.0155(7) -0.0002(8) C6A 0.0238(9) 0.0285(9) 0.0225(8) 0.0024(7) 0.0093(7) 0.0035(7) C7 0.0204(8) 0.0283(9) 0.0278(8) 0.0025(7) 0.0095(7) 0.0000(7) C8 0.0235(9) 0.0354(10) 0.0222(8) -0.0035(7) 0.0071(7) -0.0020(7) C9 0.0212(8) 0.0316(9) 0.0189(7) 0.0007(6) 0.0086(6) 0.0020(7) C9A 0.0209(8) 0.0278(9) 0.0185(7) 0.0010(6) 0.0080(6) 0.0012(7) C9B 0.0205(8) 0.0267(9) 0.0203(7) 0.0016(6) 0.0096(6) 0.0038(7) S3 0.0319(3) 0.0409(3) 0.0255(2) -0.00926(19) 0.00945(18) -0.0068(2) O9 0.0295(7) 0.0437(8) 0.0200(6) -0.0062(5) 0.0125(5) -0.0074(6) C10 0.0314(10) 0.0351(11) 0.0351(10) -0.0054(8) 0.0122(8) -0.0033(8) C11 0.0373(12) 0.0461(13) 0.0502(13) -0.0136(10) 0.0106(10) -0.0089(10) S7 0.0275(3) 0.0456(3) 0.0338(3) 0.0026(2) 0.0142(2) -0.0075(2) C12 0.0319(11) 0.0612(15) 0.0432(12) -0.0075(10) 0.0154(9) -0.0179(10) C13 0.0436(14) 0.105(2) 0.0531(15) 0.0289(15) 0.0073(12) -0.0050(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 B1 O1 1.468(2) . ? B1 O1 1.468(2) 2_756 ? B1 O9 1.474(2) . ? B1 O9 1.474(2) 2_756 ? O1 C1 1.3352(19) . ? C1 C2 1.395(2) . ? C1 C9A 1.407(2) . ? C2 C3 1.388(2) . ? C2 H2 0.9300 . ? C3 C3A 1.438(2) . ? C3 S3 1.7461(17) . ? C3A C4 1.410(2) . ? C3A C9B 1.427(2) . ? C4 C5 1.377(3) . ? C4 H4 0.9300 . ? C5 C6 1.380(3) . ? C5 H5 0.9300 . ? C6 C6A 1.412(2) . ? C6 H6 0.9300 . ? C6A C9B 1.419(2) . ? C6A C7 1.440(2) . ? C7 C8 1.386(2) . ? C7 S7 1.7587(18) . ? C8 C9 1.395(2) . ? C8 H8 0.9300 . ? C9 O9 1.3348(18) . ? C9 C9A 1.408(2) . ? C9A C9B 1.418(2) . ? S3 C10 1.808(2) . ? C10 C11 1.518(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? S7 C12 1.796(2) . ? C12 C13 1.494(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 O1 B1 O1 108.5(2) . 2_756 ? O1 B1 O9 113.13(6) . . ? O1 B1 O9 106.60(7) 2_756 . ? O1 B1 O9 106.60(7) . 2_756 ? O1 B1 O9 113.13(6) 2_756 2_756 ? O9 B1 O9 109.0(2) . 2_756 ? C1 O1 B1 123.03(13) . . ? O1 C1 C2 118.92(15) . . ? O1 C1 C9A 120.29(15) . . ? C2 C1 C9A 120.78(15) . . ? C3 C2 C1 120.36(16) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C3A 120.72(16) . . ? C2 C3 S3 122.71(14) . . ? C3A C3 S3 116.58(12) . . ? C4 C3A C9B 118.28(16) . . ? C4 C3A C3 123.23(16) . . ? C9B C3A C3 118.49(14) . . ? C5 C4 C3A 121.04(17) . . ? C5 C4 H4 119.5 . . ? C3A C4 H4 119.5 . . ? C4 C5 C6 120.89(16) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C6A 120.97(17) . . ? C5 C6 H6 119.5 . . ? C6A C6 H6 119.5 . . ? C6 C6A C9B 118.38(16) . . ? C6 C6A C7 123.11(16) . . ? C9B C6A C7 118.50(15) . . ? C8 C7 C6A 120.39(16) . . ? C8 C7 S7 123.27(14) . . ? C6A C7 S7 116.32(12) . . ? C7 C8 C9 120.97(16) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? O9 C9 C8 119.67(15) . . ? O9 C9 C9A 120.34(15) . . ? C8 C9 C9A 119.99(14) . . ? C1 C9A C9 119.92(14) . . ? C1 C9A C9B 119.93(15) . . ? C9 C9A C9B 120.15(15) . . ? C9A C9B C6A 119.86(15) . . ? C9A C9B C3A 119.70(15) . . ? C6A C9B C3A 120.44(14) . . ? C3 S3 C10 104.55(9) . . ? C9 O9 B1 122.76(13) . . ? C11 C10 S3 108.62(14) . . ? C11 C10 H10A 110.0 . . ? S3 C10 H10A 110.0 . . ? C11 C10 H10B 110.0 . . ? S3 C10 H10B 110.0 . . ? H10A C10 H10B 108.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 S7 C12 106.01(9) . . ? C13 C12 S7 113.64(19) . . ? C13 C12 H12A 108.8 . . ? S7 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? S7 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 B1 O1 C1 120.09(16) 2_756 . . . ? O9 B1 O1 C1 2.0(3) . . . . ? O9 B1 O1 C1 -117.78(15) 2_756 . . . ? B1 O1 C1 C2 174.56(17) . . . . ? B1 O1 C1 C9A -6.2(3) . . . . ? O1 C1 C2 C3 178.34(16) . . . . ? C9A C1 C2 C3 -0.9(3) . . . . ? C1 C2 C3 C3A -0.3(3) . . . . ? C1 C2 C3 S3 179.85(14) . . . . ? C2 C3 C3A C4 -179.37(17) . . . . ? S3 C3 C3A C4 0.5(2) . . . . ? C2 C3 C3A C9B 0.6(3) . . . . ? S3 C3 C3A C9B -179.53(13) . . . . ? C9B C3A C4 C5 -0.1(3) . . . . ? C3 C3A C4 C5 179.89(17) . . . . ? C3A C4 C5 C6 0.4(3) . . . . ? C4 C5 C6 C6A -0.7(3) . . . . ? C5 C6 C6A C9B 0.7(3) . . . . ? C5 C6 C6A C7 -178.98(17) . . . . ? C6 C6A C7 C8 -177.37(17) . . . . ? C9B C6A C7 C8 3.0(3) . . . . ? C6 C6A C7 S7 1.3(2) . . . . ? C9B C6A C7 S7 -178.38(13) . . . . ? C6A C7 C8 C9 -1.7(3) . . . . ? S7 C7 C8 C9 179.73(13) . . . . ? C7 C8 C9 O9 177.87(16) . . . . ? C7 C8 C9 C9A -1.7(3) . . . . ? O1 C1 C9A C9 3.7(3) . . . . ? C2 C1 C9A C9 -177.00(16) . . . . ? O1 C1 C9A C9B -177.46(15) . . . . ? C2 C1 C9A C9B 1.8(3) . . . . ? O9 C9 C9A C1 3.0(3) . . . . ? C8 C9 C9A C1 -177.39(16) . . . . ? O9 C9 C9A C9B -175.75(16) . . . . ? C8 C9 C9A C9B 3.8(3) . . . . ? C1 C9A C9B C6A 178.71(16) . . . . ? C9 C9A C9B C6A -2.5(2) . . . . ? C1 C9A C9B C3A -1.4(2) . . . . ? C9 C9A C9B C3A 177.35(16) . . . . ? C6 C6A C9B C9A 179.47(16) . . . . ? C7 C6A C9B C9A -0.9(2) . . . . ? C6 C6A C9B C3A -0.4(2) . . . . ? C7 C6A C9B C3A 179.30(16) . . . . ? C4 C3A C9B C9A -179.77(16) . . . . ? C3 C3A C9B C9A 0.3(2) . . . . ? C4 C3A C9B C6A 0.1(2) . . . . ? C3 C3A C9B C6A -179.88(15) . . . . ? C2 C3 S3 C10 1.69(18) . . . . ? C3A C3 S3 C10 -178.19(14) . . . . ? C8 C9 O9 B1 173.04(16) . . . . ? C9A C9 O9 B1 -7.4(3) . . . . ? O1 B1 O9 C9 4.9(2) . . . . ? O1 B1 O9 C9 -114.25(15) 2_756 . . . ? O9 B1 O9 C9 123.31(16) 2_756 . . . ? C3 S3 C10 C11 -177.75(14) . . . . ? C8 C7 S7 C12 -21.60(19) . . . . ? C6A C7 S7 C12 159.79(14) . . . . ? C7 S7 C12 C13 -73.08(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.400 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.062 # Attachment '- rh174_100K_0m.cif' data_rh174_100k_0m _database_code_depnum_ccdc_archive 'CCDC 867318' #TrackingRef '- rh174_100K_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H38 B O4 S4' _chemical_formula_weight 697.73 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_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' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.3177(7) _cell_length_b 21.9323(6) _cell_length_c 18.5580(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.7509(4) _cell_angle_gamma 90.00 _cell_volume 9928.8(5) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9752 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 31.67 _exptl_crystal_description 'prism frag' _exptl_crystal_colour black _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4404 _exptl_absorpt_coefficient_mu 0.329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8820 _exptl_absorpt_correction_T_max 0.9287 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 76838 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 30.03 _reflns_number_total 14455 _reflns_number_gt 11858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14455 _refine_ls_number_parameters 642 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.16394(4) 0.50670(5) 0.25604(6) 0.0129(2) Uani 1 1 d . . . O1 O 0.19979(3) 0.54402(3) 0.32463(4) 0.01377(14) Uani 1 1 d . . . C1 C 0.21604(4) 0.52215(4) 0.39936(5) 0.01170(17) Uani 1 1 d . . . C2 C 0.26022(4) 0.54978(4) 0.46343(5) 0.01329(18) Uani 1 1 d . . . H2 H 0.2789 0.5826 0.4532 0.016 Uiso 1 1 calc R . . C3 C 0.27717(4) 0.52977(4) 0.54206(5) 0.01272(17) Uani 1 1 d . . . C3A C 0.24969(4) 0.47949(4) 0.55882(5) 0.01202(17) Uani 1 1 d . . . C4 C 0.26397(4) 0.45880(4) 0.63762(6) 0.01573(19) Uani 1 1 d . . . H4 H 0.2926 0.4785 0.6823 0.019 Uiso 1 1 calc R . . C5 C 0.23667(4) 0.40991(4) 0.65068(6) 0.01668(19) Uani 1 1 d . . . H5 H 0.2469 0.3965 0.7042 0.020 Uiso 1 1 calc R . . C6 C 0.19463(4) 0.38045(4) 0.58645(6) 0.01520(18) Uani 1 1 d . . . H6 H 0.1765 0.3470 0.5966 0.018 Uiso 1 1 calc R . . C6A C 0.17837(4) 0.39952(4) 0.50625(5) 0.01199(17) Uani 1 1 d . . . C7 C 0.13460(4) 0.37105(4) 0.43739(6) 0.01281(17) Uani 1 1 d . . . C8 C 0.11739(4) 0.39451(4) 0.36054(5) 0.01286(17) Uani 1 1 d . . . H8 H 0.0873 0.3764 0.3161 0.015 Uiso 1 1 calc R . . C9 C 0.14418(4) 0.44488(4) 0.34803(5) 0.01168(17) Uani 1 1 d . . . C9A C 0.18903(4) 0.47188(4) 0.41292(5) 0.01129(17) Uani 1 1 d . . . C9B C 0.20592(4) 0.45035(4) 0.49287(5) 0.01115(17) Uani 1 1 d . . . O9 O 0.12724(3) 0.46631(3) 0.27347(4) 0.01371(13) Uani 1 1 d . . . S3 S 0.332862(10) 0.562005(11) 0.624624(14) 0.01528(6) Uani 1 1 d . . . C1C C 0.35635(4) 0.62100(4) 0.57930(6) 0.01542(19) Uani 1 1 d . . . H1A H 0.3702 0.6023 0.5435 0.018 Uiso 1 1 calc R . . H1B H 0.3255 0.6483 0.5463 0.018 Uiso 1 1 calc R . . C2C C 0.40179(4) 0.65763(4) 0.64524(6) 0.01645(19) Uani 1 1 d . . . H2A H 0.4332 0.6305 0.6765 0.020 Uiso 1 1 calc R . . H2B H 0.3883 0.6743 0.6826 0.020 Uiso 1 1 calc R . . C3C C 0.42070(5) 0.70992(5) 0.60941(7) 0.0240(2) Uani 1 1 d . . . H3A H 0.4361 0.6933 0.5750 0.036 Uiso 1 1 calc R . . H3B H 0.4487 0.7339 0.6531 0.036 Uiso 1 1 calc R . . H3C H 0.3894 0.7361 0.5771 0.036 Uiso 1 1 calc R . . S7 S 0.106184(10) 0.304908(11) 0.456663(14) 0.01621(6) Uani 1 1 d . . . C4C C 0.06007(4) 0.27588(5) 0.35769(6) 0.0200(2) Uani 1 1 d . . . H4A H 0.0353 0.2458 0.3639 0.024 Uiso 1 1 calc R . . H4B H 0.0372 0.3100 0.3249 0.024 Uiso 1 1 calc R . . C5C C 0.08774(5) 0.24574(5) 0.31118(6) 0.0223(2) Uani 1 1 d . . . H5A H 0.0596 0.2369 0.2556 0.027 Uiso 1 1 calc R . . H5B H 0.1143 0.2748 0.3075 0.027 Uiso 1 1 calc R . . C6C C 0.11752(6) 0.18702(5) 0.34975(7) 0.0325(3) Uani 1 1 d . . . H6A H 0.1454 0.1954 0.4049 0.049 Uiso 1 1 calc R . . H6B H 0.1352 0.1706 0.3182 0.049 Uiso 1 1 calc R . . H6C H 0.0912 0.1572 0.3510 0.049 Uiso 1 1 calc R . . O11 O 0.19930(3) 0.46739(3) 0.23456(4) 0.01352(13) Uani 1 1 d . . . C11 C 0.18080(4) 0.44939(4) 0.15835(5) 0.01147(17) Uani 1 1 d . . . C12 C 0.20625(4) 0.39996(4) 0.14071(5) 0.01284(18) Uani 1 1 d . . . H12 H 0.2366 0.3803 0.1830 0.015 Uiso 1 1 calc R . . C13 C 0.18744(4) 0.37978(4) 0.06223(5) 0.01268(17) Uani 1 1 d . . . C13A C 0.14254(4) 0.40995(4) -0.00333(5) 0.01296(18) Uani 1 1 d . . . C14 C 0.12349(4) 0.39331(4) -0.08481(6) 0.01669(19) Uani 1 1 d . . . H14 H 0.1403 0.3603 -0.0983 0.020 Uiso 1 1 calc R . . C15 C 0.08045(4) 0.42440(5) -0.14572(6) 0.0200(2) Uani 1 1 d . . . H15 H 0.0681 0.4123 -0.2003 0.024 Uiso 1 1 calc R . . C16 C 0.05522(4) 0.47310(5) -0.12767(6) 0.0173(2) Uani 1 1 d . . . H16 H 0.0258 0.4939 -0.1700 0.021 Uiso 1 1 calc R . . C16A C 0.07276(4) 0.49180(4) -0.04742(5) 0.01308(18) Uani 1 1 d . . . C17 C 0.04827(4) 0.54265(4) -0.02594(5) 0.01295(18) Uani 1 1 d . . . C18 C 0.06805(4) 0.56084(4) 0.05383(5) 0.01330(18) Uani 1 1 d . . . H18 H 0.0521 0.5948 0.0670 0.016 Uiso 1 1 calc R . . C19 C 0.11132(4) 0.52949(4) 0.11485(5) 0.01141(17) Uani 1 1 d . . . C19A C 0.13590(4) 0.47911(4) 0.09652(5) 0.01135(17) Uani 1 1 d . . . C19B C 0.11693(4) 0.46029(4) 0.01517(5) 0.01161(17) Uani 1 1 d . . . O19 O 0.12931(3) 0.54785(3) 0.19136(4) 0.01325(13) Uani 1 1 d . . . S13 S 0.215526(10) 0.315949(11) 0.036357(14) 0.01612(6) Uani 1 1 d . . . C11C C 0.26532(4) 0.28579(5) 0.13234(6) 0.0192(2) Uani 1 1 d . . . H11A H 0.2907 0.2587 0.1225 0.023 Uiso 1 1 calc R . . H11B H 0.2872 0.3202 0.1661 0.023 Uiso 1 1 calc R . . C12C C 0.24142(4) 0.25017(5) 0.17999(6) 0.0205(2) Uani 1 1 d . . . H12A H 0.2706 0.2432 0.2354 0.025 Uiso 1 1 calc R . . H12B H 0.2124 0.2749 0.1839 0.025 Uiso 1 1 calc R . . C13C C 0.21728(5) 0.18890(5) 0.14146(7) 0.0271(2) Uani 1 1 d . . . H13A H 0.1891 0.1954 0.0859 0.041 Uiso 1 1 calc R . . H13B H 0.2008 0.1689 0.1726 0.041 Uiso 1 1 calc R . . H13C H 0.2464 0.1630 0.1411 0.041 Uiso 1 1 calc R . . S17 S -0.007240(10) 0.577617(11) -0.105260(14) 0.01673(6) Uani 1 1 d . . . C14C C -0.02652(4) 0.63842(4) -0.05739(6) 0.01666(19) Uani 1 1 d . . . H14A H -0.0396 0.6213 -0.0198 0.020 Uiso 1 1 calc R . . H14B H 0.0054 0.6650 -0.0264 0.020 Uiso 1 1 calc R . . C15C C -0.07200(4) 0.67475(5) -0.12370(6) 0.0212(2) Uani 1 1 d . . . H15A H -0.0595 0.6884 -0.1635 0.025 Uiso 1 1 calc R . . H15B H -0.1044 0.6482 -0.1520 0.025 Uiso 1 1 calc R . . C16C C -0.08818(5) 0.73000(5) -0.08982(7) 0.0285(3) Uani 1 1 d . . . H16A H -0.1046 0.7165 -0.0553 0.043 Uiso 1 1 calc R . . H16B H -0.1148 0.7546 -0.1343 0.043 Uiso 1 1 calc R . . H16C H -0.0556 0.7546 -0.0580 0.043 Uiso 1 1 calc R . . B2 B 0.5000 0.49790(7) 0.2500 0.0112(3) Uani 1 2 d S . . O21 O 0.46332(3) 0.53661(3) 0.18354(4) 0.01176(13) Uani 1 1 d . . . C21 C 0.44611(4) 0.51764(4) 0.10724(5) 0.01041(17) Uani 1 1 d . . . C22 C 0.40115(4) 0.54627(4) 0.04521(5) 0.01263(17) Uani 1 1 d . . . H22 H 0.3821 0.5774 0.0578 0.015 Uiso 1 1 calc R . . C23 C 0.38412(4) 0.52950(4) -0.03468(5) 0.01229(17) Uani 1 1 d . . . C23A C 0.41219(4) 0.48206(4) -0.05531(5) 0.01161(17) Uani 1 1 d . . . C24 C 0.39824(4) 0.46570(4) -0.13571(5) 0.01516(19) Uani 1 1 d . . . H24 H 0.3692 0.4864 -0.1787 0.018 Uiso 1 1 calc R . . C25 C 0.42644(4) 0.41981(4) -0.15276(6) 0.01615(19) Uani 1 1 d . . . H25 H 0.4163 0.4092 -0.2073 0.019 Uiso 1 1 calc R . . C26 C 0.46925(4) 0.38923(4) -0.09094(6) 0.01438(18) Uani 1 1 d . . . H26 H 0.4880 0.3578 -0.1037 0.017 Uiso 1 1 calc R . . C26A C 0.48523(4) 0.40412(4) -0.00942(5) 0.01157(17) Uani 1 1 d . . . C27 C 0.53021(4) 0.37486(4) 0.05684(5) 0.01169(17) Uani 1 1 d . . . C28 C 0.54653(4) 0.39378(4) 0.13554(5) 0.01187(17) Uani 1 1 d . . . H28 H 0.5769 0.3747 0.1784 0.014 Uiso 1 1 calc R . . C29 C 0.51851(4) 0.44093(4) 0.15228(5) 0.01059(17) Uani 1 1 d . . . C29A C 0.47322(4) 0.46928(4) 0.08963(5) 0.01021(17) Uani 1 1 d . . . C29B C 0.45658(4) 0.45163(4) 0.00818(5) 0.01036(16) Uani 1 1 d . . . O29 O 0.53510(3) 0.45815(3) 0.22843(4) 0.01196(13) Uani 1 1 d . . . S23 S 0.328152(10) 0.562994(11) -0.115268(14) 0.01605(6) Uani 1 1 d . . . C21C C 0.30473(4) 0.62051(4) -0.06810(6) 0.01590(19) Uani 1 1 d . . . H21A H 0.2892 0.6009 -0.0349 0.019 Uiso 1 1 calc R . . H21B H 0.3358 0.6466 -0.0325 0.019 Uiso 1 1 calc R . . C22C C 0.26109(4) 0.65897(5) -0.13416(6) 0.0183(2) Uani 1 1 d . . . H22A H 0.2287 0.6332 -0.1662 0.022 Uiso 1 1 calc R . . H22B H 0.2757 0.6745 -0.1708 0.022 Uiso 1 1 calc R . . C23C C 0.24367(5) 0.71265(5) -0.09868(7) 0.0252(2) Uani 1 1 d . . . H23A H 0.2270 0.6973 -0.0652 0.038 Uiso 1 1 calc R . . H23B H 0.2170 0.7377 -0.1425 0.038 Uiso 1 1 calc R . . H23C H 0.2759 0.7374 -0.0655 0.038 Uiso 1 1 calc R . . S27 S 0.562724(10) 0.314937(11) 0.032214(14) 0.01535(6) Uani 1 1 d . . . C24C C 0.60255(4) 0.27595(4) 0.12661(6) 0.01735(19) Uani 1 1 d . . . H24A H 0.6287 0.2480 0.1198 0.021 Uiso 1 1 calc R . . H24B H 0.6242 0.3064 0.1681 0.021 Uiso 1 1 calc R . . C25C C 0.56801(5) 0.23948(5) 0.15665(6) 0.0239(2) Uani 1 1 d . . . H25A H 0.5422 0.2133 0.1124 0.029 Uiso 1 1 calc R . . H25B H 0.5461 0.2679 0.1720 0.029 Uiso 1 1 calc R . . C26C C 0.60319(6) 0.19959(5) 0.22916(7) 0.0335(3) Uani 1 1 d . . . H26A H 0.6235 0.1699 0.2134 0.050 Uiso 1 1 calc R . . H26B H 0.5795 0.1780 0.2477 0.050 Uiso 1 1 calc R . . H26C H 0.6291 0.2253 0.2729 0.050 Uiso 1 1 calc R . . 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 B1 0.0173(5) 0.0128(5) 0.0079(4) 0.0005(4) 0.0050(4) -0.0007(4) O1 0.0192(3) 0.0138(3) 0.0076(3) 0.0006(2) 0.0054(3) -0.0025(3) C1 0.0150(4) 0.0125(4) 0.0086(4) -0.0003(3) 0.0062(3) 0.0010(3) C2 0.0157(4) 0.0135(4) 0.0105(4) -0.0002(3) 0.0057(4) -0.0016(3) C3 0.0126(4) 0.0142(4) 0.0102(4) -0.0015(3) 0.0041(3) 0.0005(3) C3A 0.0128(4) 0.0135(4) 0.0088(4) 0.0002(3) 0.0040(3) 0.0021(3) C4 0.0169(5) 0.0179(5) 0.0102(4) 0.0010(3) 0.0041(4) 0.0007(4) C5 0.0203(5) 0.0191(5) 0.0092(4) 0.0042(4) 0.0054(4) 0.0024(4) C6 0.0189(5) 0.0146(4) 0.0126(4) 0.0036(3) 0.0076(4) 0.0011(4) C6A 0.0138(4) 0.0121(4) 0.0101(4) 0.0012(3) 0.0054(3) 0.0015(3) C7 0.0154(4) 0.0115(4) 0.0129(4) 0.0012(3) 0.0075(4) 0.0004(3) C8 0.0142(4) 0.0133(4) 0.0102(4) -0.0008(3) 0.0047(3) -0.0014(3) C9 0.0147(4) 0.0125(4) 0.0081(4) 0.0007(3) 0.0054(3) 0.0018(3) C9A 0.0138(4) 0.0117(4) 0.0084(4) -0.0003(3) 0.0050(3) 0.0010(3) C9B 0.0132(4) 0.0115(4) 0.0096(4) 0.0006(3) 0.0059(3) 0.0017(3) O9 0.0174(3) 0.0158(3) 0.0065(3) 0.0014(2) 0.0042(3) -0.0025(3) S3 0.01492(11) 0.01824(12) 0.01006(11) -0.00095(8) 0.00329(9) -0.00331(9) C1C 0.0148(4) 0.0175(5) 0.0136(4) 0.0005(4) 0.0060(4) -0.0011(4) C2C 0.0141(4) 0.0172(5) 0.0152(4) 0.0000(4) 0.0040(4) -0.0011(4) C3C 0.0210(5) 0.0221(5) 0.0273(6) 0.0036(4) 0.0095(5) -0.0037(4) S7 0.01983(12) 0.01512(12) 0.01269(11) 0.00205(8) 0.00644(9) -0.00421(9) C4C 0.0195(5) 0.0197(5) 0.0161(5) 0.0016(4) 0.0039(4) -0.0068(4) C5C 0.0312(6) 0.0172(5) 0.0143(5) -0.0002(4) 0.0065(4) -0.0045(4) C6C 0.0495(8) 0.0186(5) 0.0252(6) 0.0018(4) 0.0130(6) 0.0022(5) O11 0.0168(3) 0.0154(3) 0.0070(3) 0.0004(2) 0.0041(3) 0.0021(3) C11 0.0138(4) 0.0122(4) 0.0082(4) -0.0001(3) 0.0047(3) -0.0020(3) C12 0.0140(4) 0.0127(4) 0.0112(4) 0.0008(3) 0.0051(4) 0.0005(3) C13 0.0149(4) 0.0113(4) 0.0125(4) -0.0003(3) 0.0067(4) -0.0007(3) C13A 0.0157(4) 0.0117(4) 0.0120(4) -0.0011(3) 0.0068(4) -0.0022(3) C14 0.0219(5) 0.0151(4) 0.0117(4) -0.0028(3) 0.0064(4) -0.0002(4) C15 0.0270(5) 0.0181(5) 0.0110(4) -0.0047(4) 0.0050(4) -0.0014(4) C16 0.0194(5) 0.0172(5) 0.0099(4) -0.0005(3) 0.0017(4) 0.0007(4) C16A 0.0147(4) 0.0129(4) 0.0103(4) -0.0004(3) 0.0044(3) -0.0017(3) C17 0.0124(4) 0.0143(4) 0.0101(4) 0.0021(3) 0.0033(3) -0.0003(3) C18 0.0152(4) 0.0131(4) 0.0123(4) 0.0015(3) 0.0068(4) 0.0017(3) C19 0.0146(4) 0.0126(4) 0.0074(4) 0.0007(3) 0.0052(3) -0.0017(3) C19A 0.0133(4) 0.0116(4) 0.0093(4) 0.0008(3) 0.0052(3) -0.0009(3) C19B 0.0128(4) 0.0123(4) 0.0089(4) 0.0005(3) 0.0041(3) -0.0016(3) O19 0.0186(3) 0.0133(3) 0.0075(3) 0.0006(2) 0.0057(3) 0.0022(3) S13 0.02012(12) 0.01428(11) 0.01466(11) -0.00146(9) 0.00844(10) 0.00270(9) C11C 0.0181(5) 0.0188(5) 0.0182(5) -0.0007(4) 0.0059(4) 0.0046(4) C12C 0.0261(5) 0.0164(5) 0.0161(5) -0.0005(4) 0.0071(4) 0.0037(4) C13C 0.0374(7) 0.0156(5) 0.0237(6) -0.0012(4) 0.0096(5) 0.0011(4) S17 0.01579(12) 0.01874(12) 0.01152(11) 0.00228(9) 0.00247(9) 0.00333(9) C14C 0.0153(4) 0.0179(5) 0.0168(5) 0.0030(4) 0.0072(4) 0.0024(4) C15C 0.0172(5) 0.0216(5) 0.0234(5) 0.0067(4) 0.0077(4) 0.0044(4) C16C 0.0216(5) 0.0219(6) 0.0410(7) 0.0027(5) 0.0132(5) 0.0039(4) B2 0.0149(7) 0.0120(6) 0.0081(6) 0.000 0.0063(5) 0.000 O21 0.0151(3) 0.0133(3) 0.0063(3) 0.0002(2) 0.0043(2) 0.0020(2) C21 0.0132(4) 0.0111(4) 0.0079(4) 0.0000(3) 0.0057(3) -0.0011(3) C22 0.0139(4) 0.0135(4) 0.0104(4) 0.0010(3) 0.0054(4) 0.0017(3) C23 0.0120(4) 0.0134(4) 0.0102(4) 0.0011(3) 0.0039(3) -0.0003(3) C23A 0.0128(4) 0.0125(4) 0.0083(4) -0.0003(3) 0.0037(3) -0.0017(3) C24 0.0168(5) 0.0174(5) 0.0087(4) -0.0005(3) 0.0034(4) -0.0007(4) C25 0.0210(5) 0.0177(5) 0.0086(4) -0.0033(3) 0.0057(4) -0.0027(4) C26 0.0192(5) 0.0133(4) 0.0111(4) -0.0026(3) 0.0072(4) -0.0010(4) C26A 0.0141(4) 0.0111(4) 0.0098(4) -0.0008(3) 0.0056(3) -0.0020(3) C27 0.0150(4) 0.0101(4) 0.0114(4) -0.0005(3) 0.0071(4) -0.0001(3) C28 0.0137(4) 0.0122(4) 0.0096(4) 0.0010(3) 0.0051(3) 0.0012(3) C29 0.0133(4) 0.0109(4) 0.0080(4) -0.0001(3) 0.0051(3) -0.0016(3) C29A 0.0123(4) 0.0107(4) 0.0077(4) 0.0006(3) 0.0046(3) -0.0007(3) C29B 0.0124(4) 0.0103(4) 0.0086(4) -0.0005(3) 0.0049(3) -0.0016(3) O29 0.0151(3) 0.0141(3) 0.0057(3) -0.0004(2) 0.0038(3) 0.0023(2) S23 0.01502(12) 0.01990(12) 0.00971(11) 0.00165(8) 0.00246(9) 0.00458(9) C21C 0.0149(4) 0.0187(5) 0.0139(4) 0.0019(4) 0.0063(4) 0.0028(4) C22C 0.0162(5) 0.0188(5) 0.0172(5) 0.0036(4) 0.0051(4) 0.0039(4) C23C 0.0221(5) 0.0210(5) 0.0304(6) -0.0004(4) 0.0098(5) 0.0048(4) S27 0.02085(12) 0.01369(11) 0.01299(11) -0.00068(8) 0.00892(9) 0.00419(9) C24C 0.0194(5) 0.0157(5) 0.0153(5) -0.0001(4) 0.0063(4) 0.0050(4) C25C 0.0302(6) 0.0169(5) 0.0207(5) 0.0027(4) 0.0080(5) -0.0042(4) C26C 0.0498(8) 0.0188(5) 0.0240(6) 0.0048(4) 0.0095(6) 0.0007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 B1 O1 1.4585(12) . ? B1 O19 1.4587(12) . ? B1 O11 1.4771(12) . ? B1 O9 1.4786(12) . ? O1 C1 1.3400(10) . ? C1 C2 1.3949(13) . ? C1 C9A 1.4110(13) . ? C2 C3 1.3885(12) . ? C2 H2 0.9500 . ? C3 C3A 1.4446(13) . ? C3 S3 1.7503(9) . ? C3A C4 1.4082(12) . ? C3A C9B 1.4207(12) . ? C4 C5 1.3881(13) . ? C4 H4 0.9500 . ? C5 C6 1.3874(13) . ? C5 H5 0.9500 . ? C6 C6A 1.4114(12) . ? C6 H6 0.9500 . ? C6A C9B 1.4280(12) . ? C6A C7 1.4412(12) . ? C7 C8 1.3842(12) . ? C7 S7 1.7564(9) . ? C8 C9 1.4010(12) . ? C8 H8 0.9500 . ? C9 O9 1.3317(10) . ? C9 C9A 1.4049(12) . ? C9A C9B 1.4216(12) . ? S3 C1C 1.8108(10) . ? C1C C2C 1.5220(13) . ? C1C H1A 0.9900 . ? C1C H1B 0.9900 . ? C2C C3C 1.5276(14) . ? C2C H2A 0.9900 . ? C2C H2B 0.9900 . ? C3C H3A 0.9800 . ? C3C H3B 0.9800 . ? C3C H3C 0.9800 . ? S7 C4C 1.8119(10) . ? C4C C5C 1.5299(15) . ? C4C H4A 0.9900 . ? C4C H4B 0.9900 . ? C5C C6C 1.5195(15) . ? C5C H5A 0.9900 . ? C5C H5B 0.9900 . ? C6C H6A 0.9800 . ? C6C H6B 0.9800 . ? C6C H6C 0.9800 . ? O11 C11 1.3296(10) . ? C11 C12 1.4039(13) . ? C11 C19A 1.4067(12) . ? C12 C13 1.3810(12) . ? C12 H12 0.9500 . ? C13 C13A 1.4420(13) . ? C13 S13 1.7637(9) . ? C13A C14 1.4079(12) . ? C13A C19B 1.4292(13) . ? C14 C15 1.3886(14) . ? C14 H14 0.9500 . ? C15 C16 1.3915(14) . ? C15 H15 0.9500 . ? C16 C16A 1.4048(12) . ? C16 H16 0.9500 . ? C16A C19B 1.4216(12) . ? C16A C17 1.4456(13) . ? C17 C18 1.3865(12) . ? C17 S17 1.7451(9) . ? C18 C19 1.3955(12) . ? C18 H18 0.9500 . ? C19 O19 1.3385(10) . ? C19 C19A 1.4117(12) . ? C19A C19B 1.4191(12) . ? S13 C11C 1.8109(10) . ? C11C C12C 1.5292(14) . ? C11C H11A 0.9900 . ? C11C H11B 0.9900 . ? C12C C13C 1.5256(14) . ? C12C H12A 0.9900 . ? C12C H12B 0.9900 . ? C13C H13A 0.9800 . ? C13C H13B 0.9800 . ? C13C H13C 0.9800 . ? S17 C14C 1.8072(10) . ? C14C C15C 1.5220(13) . ? C14C H14A 0.9900 . ? C14C H14B 0.9900 . ? C15C C16C 1.5196(15) . ? C15C H15A 0.9900 . ? C15C H15B 0.9900 . ? C16C H16A 0.9800 . ? C16C H16B 0.9800 . ? C16C H16C 0.9800 . ? B2 O21 1.4606(10) 2_655 ? B2 O21 1.4606(10) . ? B2 O29 1.4782(10) 2_655 ? B2 O29 1.4782(10) . ? O21 C21 1.3416(10) . ? C21 C22 1.3983(12) . ? C21 C29A 1.4134(12) . ? C22 C23 1.3889(12) . ? C22 H22 0.9500 . ? C23 C23A 1.4428(13) . ? C23 S23 1.7479(9) . ? C23A C24 1.4099(12) . ? C23A C29B 1.4206(12) . ? C24 C25 1.3879(13) . ? C24 H24 0.9500 . ? C25 C26 1.3878(13) . ? C25 H25 0.9500 . ? C26 C26A 1.4112(12) . ? C26 H26 0.9500 . ? C26A C29B 1.4263(12) . ? C26A C27 1.4400(12) . ? C27 C28 1.3849(12) . ? C27 S27 1.7581(9) . ? C28 C29 1.4020(12) . ? C28 H28 0.9500 . ? C29 O29 1.3299(10) . ? C29 C29A 1.4051(12) . ? C29A C29B 1.4223(12) . ? S23 C21C 1.8086(10) . ? C21C C22C 1.5232(13) . ? C21C H21A 0.9900 . ? C21C H21B 0.9900 . ? C22C C23C 1.5258(14) . ? C22C H22A 0.9900 . ? C22C H22B 0.9900 . ? C23C H23A 0.9800 . ? C23C H23B 0.9800 . ? C23C H23C 0.9800 . ? S27 C24C 1.8078(10) . ? C24C C25C 1.5214(15) . ? C24C H24A 0.9900 . ? C24C H24B 0.9900 . ? C25C C26C 1.5282(14) . ? C25C H25A 0.9900 . ? C25C H25B 0.9900 . ? C26C H26A 0.9800 . ? C26C H26B 0.9800 . ? C26C H26C 0.9800 . ? 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 O1 B1 O19 107.64(8) . . ? O1 B1 O11 107.42(8) . . ? O19 B1 O11 113.56(7) . . ? O1 B1 O9 113.59(7) . . ? O19 B1 O9 107.35(8) . . ? O11 B1 O9 107.43(8) . . ? C1 O1 B1 118.81(7) . . ? O1 C1 C2 118.90(8) . . ? O1 C1 C9A 120.53(8) . . ? C2 C1 C9A 120.57(8) . . ? C3 C2 C1 120.66(9) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C3A 120.51(8) . . ? C2 C3 S3 122.66(7) . . ? C3A C3 S3 116.81(7) . . ? C4 C3A C9B 118.81(9) . . ? C4 C3A C3 122.80(8) . . ? C9B C3A C3 118.38(8) . . ? C5 C4 C3A 120.71(9) . . ? C5 C4 H4 119.6 . . ? C3A C4 H4 119.6 . . ? C6 C5 C4 120.78(9) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C6A 120.92(9) . . ? C5 C6 H6 119.5 . . ? C6A C6 H6 119.5 . . ? C6 C6A C9B 118.31(8) . . ? C6 C6A C7 123.26(8) . . ? C9B C6A C7 118.41(8) . . ? C8 C7 C6A 120.94(8) . . ? C8 C7 S7 122.72(7) . . ? C6A C7 S7 116.33(7) . . ? C7 C8 C9 120.22(8) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? O9 C9 C8 119.17(8) . . ? O9 C9 C9A 120.20(8) . . ? C8 C9 C9A 120.62(8) . . ? C9 C9A C1 120.05(8) . . ? C9 C9A C9B 120.19(8) . . ? C1 C9A C9B 119.71(8) . . ? C3A C9B C9A 120.11(8) . . ? C3A C9B C6A 120.43(8) . . ? C9A C9B C6A 119.47(8) . . ? C9 O9 B1 119.09(7) . . ? C3 S3 C1C 103.42(4) . . ? C2C C1C S3 109.58(6) . . ? C2C C1C H1A 109.8 . . ? S3 C1C H1A 109.8 . . ? C2C C1C H1B 109.8 . . ? S3 C1C H1B 109.8 . . ? H1A C1C H1B 108.2 . . ? C1C C2C C3C 111.07(8) . . ? C1C C2C H2A 109.4 . . ? C3C C2C H2A 109.4 . . ? C1C C2C H2B 109.4 . . ? C3C C2C H2B 109.4 . . ? H2A C2C H2B 108.0 . . ? C2C C3C H3A 109.5 . . ? C2C C3C H3B 109.5 . . ? H3A C3C H3B 109.5 . . ? C2C C3C H3C 109.5 . . ? H3A C3C H3C 109.5 . . ? H3B C3C H3C 109.5 . . ? C7 S7 C4C 104.66(5) . . ? C5C C4C S7 115.40(7) . . ? C5C C4C H4A 108.4 . . ? S7 C4C H4A 108.4 . . ? C5C C4C H4B 108.4 . . ? S7 C4C H4B 108.4 . . ? H4A C4C H4B 107.5 . . ? C6C C5C C4C 113.34(9) . . ? C6C C5C H5A 108.9 . . ? C4C C5C H5A 108.9 . . ? C6C C5C H5B 108.9 . . ? C4C C5C H5B 108.9 . . ? H5A C5C H5B 107.7 . . ? C5C C6C H6A 109.5 . . ? C5C C6C H6B 109.5 . . ? H6A C6C H6B 109.5 . . ? C5C C6C H6C 109.5 . . ? H6A C6C H6C 109.5 . . ? H6B C6C H6C 109.5 . . ? C11 O11 B1 118.60(7) . . ? O11 C11 C12 119.10(8) . . ? O11 C11 C19A 120.30(8) . . ? C12 C11 C19A 120.60(8) . . ? C13 C12 C11 120.35(8) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C13A 120.94(8) . . ? C12 C13 S13 122.72(7) . . ? C13A C13 S13 116.33(7) . . ? C14 C13A C19B 118.29(8) . . ? C14 C13A C13 123.38(9) . . ? C19B C13A C13 118.31(8) . . ? C15 C14 C13A 121.02(9) . . ? C15 C14 H14 119.5 . . ? C13A C14 H14 119.5 . . ? C14 C15 C16 120.70(9) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C16A 120.66(9) . . ? C15 C16 H16 119.7 . . ? C16A C16 H16 119.7 . . ? C16 C16A C19B 118.90(9) . . ? C16 C16A C17 122.56(8) . . ? C19B C16A C17 118.53(8) . . ? C18 C17 C16A 120.67(8) . . ? C18 C17 S17 123.17(7) . . ? C16A C17 S17 116.15(7) . . ? C17 C18 C19 120.35(8) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? O19 C19 C18 119.01(8) . . ? O19 C19 C19A 120.25(8) . . ? C18 C19 C19A 120.74(8) . . ? C11 C19A C19 120.04(8) . . ? C11 C19A C19B 119.99(8) . . ? C19 C19A C19B 119.90(8) . . ? C19A C19B C16A 119.81(8) . . ? C19A C19B C13A 119.76(8) . . ? C16A C19B C13A 120.43(8) . . ? C19 O19 B1 118.63(7) . . ? C13 S13 C11C 104.38(5) . . ? C12C C11C S13 115.35(7) . . ? C12C C11C H11A 108.4 . . ? S13 C11C H11A 108.4 . . ? C12C C11C H11B 108.4 . . ? S13 C11C H11B 108.4 . . ? H11A C11C H11B 107.5 . . ? C13C C12C C11C 112.71(9) . . ? C13C C12C H12A 109.0 . . ? C11C C12C H12A 109.0 . . ? C13C C12C H12B 109.0 . . ? C11C C12C H12B 109.0 . . ? H12A C12C H12B 107.8 . . ? C12C C13C H13A 109.5 . . ? C12C C13C H13B 109.5 . . ? H13A C13C H13B 109.5 . . ? C12C C13C H13C 109.5 . . ? H13A C13C H13C 109.5 . . ? H13B C13C H13C 109.5 . . ? C17 S17 C14C 104.16(4) . . ? C15C C14C S17 107.54(7) . . ? C15C C14C H14A 110.2 . . ? S17 C14C H14A 110.2 . . ? C15C C14C H14B 110.2 . . ? S17 C14C H14B 110.2 . . ? H14A C14C H14B 108.5 . . ? C16C C15C C14C 111.50(9) . . ? C16C C15C H15A 109.3 . . ? C14C C15C H15A 109.3 . . ? C16C C15C H15B 109.3 . . ? C14C C15C H15B 109.3 . . ? H15A C15C H15B 108.0 . . ? C15C C16C H16A 109.5 . . ? C15C C16C H16B 109.5 . . ? H16A C16C H16B 109.5 . . ? C15C C16C H16C 109.5 . . ? H16A C16C H16C 109.5 . . ? H16B C16C H16C 109.5 . . ? O21 B2 O21 108.93(10) 2_655 . ? O21 B2 O29 113.34(3) 2_655 2_655 ? O21 B2 O29 106.82(4) . 2_655 ? O21 B2 O29 106.82(4) 2_655 . ? O21 B2 O29 113.34(3) . . ? O29 B2 O29 107.72(10) 2_655 . ? C21 O21 B2 119.49(7) . . ? O21 C21 C22 119.36(8) . . ? O21 C21 C29A 120.37(8) . . ? C22 C21 C29A 120.27(8) . . ? C23 C22 C21 120.53(8) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C23A 120.77(8) . . ? C22 C23 S23 123.08(7) . . ? C23A C23 S23 116.15(7) . . ? C24 C23A C29B 118.77(8) . . ? C24 C23A C23 122.79(8) . . ? C29B C23A C23 118.42(8) . . ? C25 C24 C23A 120.83(9) . . ? C25 C24 H24 119.6 . . ? C23A C24 H24 119.6 . . ? C26 C25 C24 120.63(9) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C26A 120.89(9) . . ? C25 C26 H26 119.6 . . ? C26A C26 H26 119.6 . . ? C26 C26A C29B 118.53(8) . . ? C26 C26A C27 123.06(8) . . ? C29B C26A C27 118.38(8) . . ? C28 C27 C26A 120.86(8) . . ? C28 C27 S27 122.52(7) . . ? C26A C27 S27 116.62(7) . . ? C27 C28 C29 120.39(8) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? O29 C29 C28 119.08(8) . . ? O29 C29 C29A 120.37(8) . . ? C28 C29 C29A 120.55(8) . . ? C29 C29A C21 119.91(8) . . ? C29 C29A C29B 120.00(8) . . ? C21 C29A C29B 120.00(8) . . ? C23A C29B C29A 119.91(8) . . ? C23A C29B C26A 120.32(8) . . ? C29A C29B C26A 119.76(8) . . ? C29 O29 B2 120.20(6) . . ? C23 S23 C21C 104.05(4) . . ? C22C C21C S23 108.42(7) . . ? C22C C21C H21A 110.0 . . ? S23 C21C H21A 110.0 . . ? C22C C21C H21B 110.0 . . ? S23 C21C H21B 110.0 . . ? H21A C21C H21B 108.4 . . ? C21C C22C C23C 111.29(8) . . ? C21C C22C H22A 109.4 . . ? C23C C22C H22A 109.4 . . ? C21C C22C H22B 109.4 . . ? C23C C22C H22B 109.4 . . ? H22A C22C H22B 108.0 . . ? C22C C23C H23A 109.5 . . ? C22C C23C H23B 109.5 . . ? H23A C23C H23B 109.5 . . ? C22C C23C H23C 109.5 . . ? H23A C23C H23C 109.5 . . ? H23B C23C H23C 109.5 . . ? C27 S27 C24C 104.82(4) . . ? C25C C24C S27 113.69(7) . . ? C25C C24C H24A 108.8 . . ? S27 C24C H24A 108.8 . . ? C25C C24C H24B 108.8 . . ? S27 C24C H24B 108.8 . . ? H24A C24C H24B 107.7 . . ? C24C C25C C26C 112.07(10) . . ? C24C C25C H25A 109.2 . . ? C26C C25C H25A 109.2 . . ? C24C C25C H25B 109.2 . . ? C26C C25C H25B 109.2 . . ? H25A C25C H25B 107.9 . . ? C25C C26C H26A 109.5 . . ? C25C C26C H26B 109.5 . . ? H26A C26C H26B 109.5 . . ? C25C C26C H26C 109.5 . . ? H26A C26C H26C 109.5 . . ? H26B C26C H26C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O19 B1 O1 C1 149.16(8) . . . . ? O11 B1 O1 C1 -88.21(9) . . . . ? O9 B1 O1 C1 30.44(12) . . . . ? B1 O1 C1 C2 164.26(8) . . . . ? B1 O1 C1 C9A -15.51(13) . . . . ? O1 C1 C2 C3 177.87(8) . . . . ? C9A C1 C2 C3 -2.36(14) . . . . ? C1 C2 C3 C3A 0.69(14) . . . . ? C1 C2 C3 S3 179.13(7) . . . . ? C2 C3 C3A C4 -177.72(9) . . . . ? S3 C3 C3A C4 3.76(12) . . . . ? C2 C3 C3A C9B 1.39(13) . . . . ? S3 C3 C3A C9B -177.14(7) . . . . ? C9B C3A C4 C5 1.47(14) . . . . ? C3 C3A C4 C5 -179.43(9) . . . . ? C3A C4 C5 C6 -0.18(15) . . . . ? C4 C5 C6 C6A -0.24(15) . . . . ? C5 C6 C6A C9B -0.64(14) . . . . ? C5 C6 C6A C7 -179.28(9) . . . . ? C6 C6A C7 C8 174.84(9) . . . . ? C9B C6A C7 C8 -3.80(13) . . . . ? C6 C6A C7 S7 -6.58(12) . . . . ? C9B C6A C7 S7 174.78(7) . . . . ? C6A C7 C8 C9 3.07(14) . . . . ? S7 C7 C8 C9 -175.41(7) . . . . ? C7 C8 C9 O9 179.36(8) . . . . ? C7 C8 C9 C9A 0.55(14) . . . . ? O9 C9 C9A C1 0.48(13) . . . . ? C8 C9 C9A C1 179.28(8) . . . . ? O9 C9 C9A C9B 177.82(8) . . . . ? C8 C9 C9A C9B -3.38(14) . . . . ? O1 C1 C9A C9 -0.97(13) . . . . ? C2 C1 C9A C9 179.26(8) . . . . ? O1 C1 C9A C9B -178.32(8) . . . . ? C2 C1 C9A C9B 1.91(14) . . . . ? C4 C3A C9B C9A 177.33(8) . . . . ? C3 C3A C9B C9A -1.81(13) . . . . ? C4 C3A C9B C6A -2.36(13) . . . . ? C3 C3A C9B C6A 178.50(8) . . . . ? C9 C9A C9B C3A -177.14(8) . . . . ? C1 C9A C9B C3A 0.20(13) . . . . ? C9 C9A C9B C6A 2.55(13) . . . . ? C1 C9A C9B C6A 179.90(8) . . . . ? C6 C6A C9B C3A 1.95(13) . . . . ? C7 C6A C9B C3A -179.34(8) . . . . ? C6 C6A C9B C9A -177.75(8) . . . . ? C7 C6A C9B C9A 0.96(13) . . . . ? C8 C9 O9 B1 -162.54(8) . . . . ? C9A C9 O9 B1 16.28(12) . . . . ? O1 B1 O9 C9 -31.04(12) . . . . ? O19 B1 O9 C9 -149.91(7) . . . . ? O11 B1 O9 C9 87.61(9) . . . . ? C2 C3 S3 C1C 0.36(9) . . . . ? C3A C3 S3 C1C 178.85(7) . . . . ? C3 S3 C1C C2C 174.52(7) . . . . ? S3 C1C C2C C3C -177.16(7) . . . . ? C8 C7 S7 C4C 6.06(9) . . . . ? C6A C7 S7 C4C -172.49(7) . . . . ? C7 S7 C4C C5C 73.88(8) . . . . ? S7 C4C C5C C6C 66.54(11) . . . . ? O1 B1 O11 C11 -151.49(7) . . . . ? O19 B1 O11 C11 -32.59(12) . . . . ? O9 B1 O11 C11 85.96(9) . . . . ? B1 O11 C11 C12 -162.97(8) . . . . ? B1 O11 C11 C19A 16.26(12) . . . . ? O11 C11 C12 C13 179.16(8) . . . . ? C19A C11 C12 C13 -0.07(14) . . . . ? C11 C12 C13 C13A 1.83(14) . . . . ? C11 C12 C13 S13 -177.16(7) . . . . ? C12 C13 C13A C14 176.70(9) . . . . ? S13 C13 C13A C14 -4.24(13) . . . . ? C12 C13 C13A C19B -1.71(14) . . . . ? S13 C13 C13A C19B 177.35(7) . . . . ? C19B C13A C14 C15 -0.82(14) . . . . ? C13 C13A C14 C15 -179.23(9) . . . . ? C13A C14 C15 C16 0.32(16) . . . . ? C14 C15 C16 C16A -0.02(16) . . . . ? C15 C16 C16A C19B 0.25(15) . . . . ? C15 C16 C16A C17 179.12(9) . . . . ? C16 C16A C17 C18 -177.86(9) . . . . ? C19B C16A C17 C18 1.02(14) . . . . ? C16 C16A C17 S17 3.25(12) . . . . ? C19B C16A C17 S17 -177.88(7) . . . . ? C16A C17 C18 C19 -1.23(14) . . . . ? S17 C17 C18 C19 177.59(7) . . . . ? C17 C18 C19 O19 -179.57(8) . . . . ? C17 C18 C19 C19A 0.42(14) . . . . ? O11 C11 C19A C19 1.97(13) . . . . ? C12 C11 C19A C19 -178.81(8) . . . . ? O11 C11 C19A C19B 179.00(8) . . . . ? C12 C11 C19A C19B -1.78(14) . . . . ? O19 C19 C19A C11 -2.37(13) . . . . ? C18 C19 C19A C11 177.64(8) . . . . ? O19 C19 C19A C19B -179.41(8) . . . . ? C18 C19 C19A C19B 0.61(13) . . . . ? C11 C19A C19B C16A -177.83(8) . . . . ? C19 C19A C19B C16A -0.80(13) . . . . ? C11 C19A C19B C13A 1.86(13) . . . . ? C19 C19A C19B C13A 178.89(8) . . . . ? C16 C16A C19B C19A 178.92(9) . . . . ? C17 C16A C19B C19A 0.00(13) . . . . ? C16 C16A C19B C13A -0.77(14) . . . . ? C17 C16A C19B C13A -179.68(8) . . . . ? C14 C13A C19B C19A -178.64(8) . . . . ? C13 C13A C19B C19A -0.14(13) . . . . ? C14 C13A C19B C16A 1.05(13) . . . . ? C13 C13A C19B C16A 179.54(8) . . . . ? C18 C19 O19 B1 164.28(8) . . . . ? C19A C19 O19 B1 -15.70(12) . . . . ? O1 B1 O19 C19 150.95(8) . . . . ? O11 B1 O19 C19 32.18(11) . . . . ? O9 B1 O19 C19 -86.41(9) . . . . ? C12 C13 S13 C11C 4.32(9) . . . . ? C13A C13 S13 C11C -174.71(7) . . . . ? C13 S13 C11C C12C 76.16(8) . . . . ? S13 C11C C12C C13C 70.42(10) . . . . ? C18 C17 S17 C14C 1.73(9) . . . . ? C16A C17 S17 C14C -179.40(7) . . . . ? C17 S17 C14C C15C 175.41(7) . . . . ? S17 C14C C15C C16C -175.76(7) . . . . ? O21 B2 O21 C21 147.32(8) 2_655 . . . ? O29 B2 O21 C21 -89.91(8) 2_655 . . . ? O29 B2 O21 C21 28.56(11) . . . . ? B2 O21 C21 C22 164.02(7) . . . . ? B2 O21 C21 C29A -16.11(12) . . . . ? O21 C21 C22 C23 176.91(8) . . . . ? C29A C21 C22 C23 -2.97(14) . . . . ? C21 C22 C23 C23A 0.37(14) . . . . ? C21 C22 C23 S23 179.72(7) . . . . ? C22 C23 C23A C24 -176.56(9) . . . . ? S23 C23 C23A C24 4.05(12) . . . . ? C22 C23 C23A C29B 1.90(13) . . . . ? S23 C23 C23A C29B -177.49(7) . . . . ? C29B C23A C24 C25 1.43(14) . . . . ? C23 C23A C24 C25 179.89(9) . . . . ? C23A C24 C25 C26 -0.36(15) . . . . ? C24 C25 C26 C26A -0.20(15) . . . . ? C25 C26 C26A C29B -0.32(14) . . . . ? C25 C26 C26A C27 -178.38(9) . . . . ? C26 C26A C27 C28 175.83(9) . . . . ? C29B C26A C27 C28 -2.24(13) . . . . ? C26 C26A C27 S27 -3.96(12) . . . . ? C29B C26A C27 S27 177.97(7) . . . . ? C26A C27 C28 C29 1.64(14) . . . . ? S27 C27 C28 C29 -178.59(7) . . . . ? C27 C28 C29 O29 -179.99(8) . . . . ? C27 C28 C29 C29A 0.57(14) . . . . ? O29 C29 C29A C21 1.95(13) . . . . ? C28 C29 C29A C21 -178.62(8) . . . . ? O29 C29 C29A C29B 178.44(8) . . . . ? C28 C29 C29A C29B -2.13(13) . . . . ? O21 C21 C29A C29 -0.13(13) . . . . ? C22 C21 C29A C29 179.74(8) . . . . ? O21 C21 C29A C29B -176.62(8) . . . . ? C22 C21 C29A C29B 3.25(13) . . . . ? C24 C23A C29B C29A 176.94(8) . . . . ? C23 C23A C29B C29A -1.59(13) . . . . ? C24 C23A C29B C26A -1.94(13) . . . . ? C23 C23A C29B C26A 179.53(8) . . . . ? C29 C29A C29B C23A -177.42(8) . . . . ? C21 C29A C29B C23A -0.93(13) . . . . ? C29 C29A C29B C26A 1.47(13) . . . . ? C21 C29A C29B C26A 177.96(8) . . . . ? C26 C26A C29B C23A 1.40(13) . . . . ? C27 C26A C29B C23A 179.56(8) . . . . ? C26 C26A C29B C29A -177.48(8) . . . . ? C27 C26A C29B C29A 0.68(13) . . . . ? C28 C29 O29 B2 -166.96(8) . . . . ? C29A C29 O29 B2 12.48(13) . . . . ? O21 B2 O29 C29 -146.89(7) 2_655 . . . ? O21 B2 O29 C29 -26.92(12) . . . . ? O29 B2 O29 C29 91.03(7) 2_655 . . . ? C22 C23 S23 C21C 2.04(9) . . . . ? C23A C23 S23 C21C -178.59(7) . . . . ? C23 S23 C21C C22C 171.79(7) . . . . ? S23 C21C C22C C23C -174.08(7) . . . . ? C28 C27 S27 C24C 15.50(9) . . . . ? C26A C27 S27 C24C -164.72(7) . . . . ? C27 S27 C24C C25C 71.96(8) . . . . ? S27 C24C C25C C26C 171.24(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.507 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.059 # Attachment '- rh174_296K_0m.cif' data_rh174_296k_0m _database_code_depnum_ccdc_archive 'CCDC 867319' #TrackingRef '- rh174_296K_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H38 B O4 S4' _chemical_formula_weight 697.73 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_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' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 9.3401(2) _cell_length_b 22.0917(6) _cell_length_c 16.6081(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.7623(4) _cell_angle_gamma 90.00 _cell_volume 3422.91(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9298 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 30.76 _exptl_crystal_description 'prism frag' _exptl_crystal_colour black _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 0.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8856 _exptl_absorpt_correction_T_max 0.9309 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26790 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0139 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 30.03 _reflns_number_total 5005 _reflns_number_gt 3924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+1.2660P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5005 _refine_ls_number_parameters 235 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.0000 0.24888(10) 0.7500 0.0398(4) Uani 1 2 d S . . O1 O -0.03978(10) 0.21006(4) 0.81641(5) 0.0431(2) Uani 1 1 d . . . C1 C -0.01407(13) 0.22908(6) 0.89226(6) 0.0368(2) Uani 1 1 d . . . C2 C -0.08208(15) 0.19965(6) 0.95442(7) 0.0425(3) Uani 1 1 d . . . H2A H -0.1457 0.1682 0.9424 0.051 Uiso 1 1 calc R . . C3 C -0.05495(15) 0.21721(6) 1.03395(7) 0.0420(3) Uani 1 1 d . . . C3A C 0.04287(14) 0.26579(6) 1.05387(7) 0.0402(3) Uani 1 1 d . . . C4 C 0.07909(18) 0.28377(7) 1.13364(7) 0.0529(4) Uani 1 1 d . . . H4A H 0.0384 0.2638 1.1762 0.063 Uiso 1 1 calc R . . C5 C 0.1738(2) 0.33053(8) 1.14968(8) 0.0602(4) Uani 1 1 d . . . H5A H 0.1956 0.3417 1.2029 0.072 Uiso 1 1 calc R . . C6 C 0.23675(18) 0.36100(7) 1.08820(8) 0.0526(3) Uani 1 1 d . . . H6A H 0.3002 0.3925 1.1004 0.063 Uiso 1 1 calc R . . C6A C 0.20619(14) 0.34501(6) 1.00696(7) 0.0402(3) Uani 1 1 d . . . C7 C 0.27075(14) 0.37432(6) 0.94043(8) 0.0413(3) Uani 1 1 d . . . C8 C 0.24376(14) 0.35415(6) 0.86243(7) 0.0409(3) Uani 1 1 d . . . H8A H 0.2891 0.3726 0.8203 0.049 Uiso 1 1 calc R . . C9 C 0.14922(13) 0.30639(6) 0.84633(6) 0.0360(2) Uani 1 1 d . . . C9A C 0.07938(13) 0.27770(5) 0.90920(6) 0.0346(2) Uani 1 1 d . . . C9B C 0.10972(13) 0.29634(5) 0.99015(6) 0.0358(2) Uani 1 1 d . . . O9 O 0.12394(10) 0.28818(4) 0.77049(5) 0.0432(2) Uani 1 1 d . . . S3 S -0.13865(4) 0.18356(2) 1.11464(2) 0.05601(13) Uani 1 1 d . . . C10 C -0.25299(16) 0.12653(8) 1.06809(9) 0.0545(4) Uani 1 1 d . . . H10A H -0.3275 0.1455 1.0341 0.065 Uiso 1 1 calc R . . H10B H -0.1974 0.1003 1.0347 0.065 Uiso 1 1 calc R . . C11 C -0.31990(19) 0.08975(8) 1.13366(11) 0.0618(4) Uani 1 1 d . . . H11A H -0.2448 0.0736 1.1699 0.074 Uiso 1 1 calc R . . H11B H -0.3799 0.1159 1.1647 0.074 Uiso 1 1 calc R . . C12 C -0.4090(2) 0.03836(10) 1.09855(15) 0.0838(6) Uani 1 1 d . . . H12A H -0.4527 0.0169 1.1412 0.126 Uiso 1 1 calc R . . H12B H -0.3487 0.0113 1.0702 0.126 Uiso 1 1 calc R . . H12C H -0.4822 0.0542 1.0619 0.126 Uiso 1 1 calc R . . S7 S 0.38248(5) 0.436566(19) 0.96368(3) 0.06212(14) Uani 1 1 d . A . C13 C 0.4154(2) 0.47143(9) 0.86872(13) 0.0713(5) Uani 1 1 d D . . H13A H 0.4879 0.5022 0.8793 0.086 Uiso 0.549(6) 1 calc PR A 1 H13B H 0.4584 0.4408 0.8357 0.086 Uiso 0.549(6) 1 calc PR A 1 H13C H 0.5027 0.4953 0.8724 0.086 Uiso 0.451(6) 1 d PR A 2 H13D H 0.4234 0.4412 0.8269 0.086 Uiso 0.451(6) 1 d PR A 2 C14 C 0.2932(5) 0.50142(17) 0.8157(3) 0.0677(11) Uani 0.549(6) 1 d PD A 1 H14A H 0.3265 0.5091 0.7622 0.081 Uiso 0.549(6) 1 calc PR A 1 H14B H 0.2120 0.4741 0.8105 0.081 Uiso 0.549(6) 1 calc PR A 1 C15 C 0.2464(7) 0.56076(18) 0.8530(3) 0.106(2) Uani 0.549(6) 1 d PD A 1 H15A H 0.1692 0.5780 0.8204 0.159 Uiso 0.549(6) 1 calc PR A 1 H15B H 0.3257 0.5885 0.8560 0.159 Uiso 0.549(6) 1 calc PR A 1 H15C H 0.2149 0.5533 0.9063 0.159 Uiso 0.549(6) 1 calc PR A 1 C14D C 0.2866(8) 0.5117(3) 0.8520(4) 0.0909(19) Uani 0.451(6) 1 d PD A 2 H14C H 0.2682 0.5362 0.8989 0.109 Uiso 0.451(6) 1 calc PR A 2 H14D H 0.2021 0.4875 0.8384 0.109 Uiso 0.451(6) 1 calc PR A 2 C15D C 0.3239(10) 0.5521(3) 0.7805(4) 0.131(3) Uani 0.451(6) 1 d PD A 2 H15D H 0.2420 0.5761 0.7640 0.197 Uiso 0.451(6) 1 calc PR A 2 H15E H 0.3508 0.5272 0.7364 0.197 Uiso 0.451(6) 1 calc PR A 2 H15F H 0.4023 0.5783 0.7965 0.197 Uiso 0.451(6) 1 calc PR A 2 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 B1 0.0498(10) 0.0459(10) 0.0231(7) 0.000 -0.0051(7) 0.000 O1 0.0558(5) 0.0485(5) 0.0242(4) 0.0009(3) -0.0053(3) -0.0078(4) C1 0.0436(6) 0.0428(6) 0.0234(5) 0.0021(4) -0.0030(4) 0.0028(5) C2 0.0480(7) 0.0489(7) 0.0304(5) 0.0040(5) 0.0001(5) -0.0041(5) C3 0.0486(7) 0.0496(7) 0.0281(5) 0.0053(5) 0.0047(5) 0.0058(5) C3A 0.0499(7) 0.0459(6) 0.0249(5) -0.0007(4) 0.0019(4) 0.0083(5) C4 0.0725(9) 0.0616(9) 0.0249(5) -0.0032(5) 0.0058(6) 0.0048(7) C5 0.0863(11) 0.0656(9) 0.0281(6) -0.0141(6) -0.0018(6) 0.0028(8) C6 0.0695(9) 0.0519(8) 0.0358(6) -0.0134(6) -0.0043(6) 0.0007(7) C6A 0.0498(7) 0.0398(6) 0.0306(5) -0.0062(4) -0.0030(5) 0.0074(5) C7 0.0472(7) 0.0375(6) 0.0385(6) -0.0038(5) -0.0037(5) 0.0012(5) C8 0.0484(7) 0.0418(6) 0.0323(5) 0.0022(5) -0.0003(5) -0.0007(5) C9 0.0432(6) 0.0404(6) 0.0239(5) 0.0021(4) -0.0036(4) 0.0037(5) C9A 0.0409(6) 0.0392(6) 0.0232(4) 0.0007(4) -0.0024(4) 0.0045(4) C9B 0.0434(6) 0.0393(6) 0.0243(5) -0.0006(4) -0.0014(4) 0.0079(5) O9 0.0547(5) 0.0535(5) 0.0209(3) 0.0026(3) -0.0031(3) -0.0076(4) S3 0.0654(2) 0.0701(3) 0.03355(17) 0.00774(15) 0.01219(15) -0.00509(18) C10 0.0510(8) 0.0677(10) 0.0453(7) 0.0084(7) 0.0079(6) 0.0002(7) C11 0.0637(9) 0.0649(10) 0.0584(9) 0.0099(7) 0.0186(7) -0.0008(8) C12 0.0758(13) 0.0783(13) 0.0989(17) 0.0026(12) 0.0195(11) -0.0121(10) S7 0.0766(3) 0.0529(2) 0.0567(2) -0.01362(17) 0.00163(19) -0.01865(19) C13 0.0757(12) 0.0577(10) 0.0808(13) 0.0026(9) 0.0067(9) -0.0199(9) C14 0.102(3) 0.0494(18) 0.051(2) -0.0029(16) 0.0040(19) -0.0128(17) C15 0.184(6) 0.054(2) 0.081(3) -0.0107(18) -0.002(3) 0.004(3) C14D 0.139(5) 0.065(3) 0.069(4) 0.007(3) 0.007(4) 0.019(3) C15D 0.246(10) 0.066(3) 0.081(4) 0.026(3) -0.003(5) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 B1 O1 1.4591(15) 2_556 ? B1 O1 1.4591(15) . ? B1 O9 1.4738(15) . ? B1 O9 1.4738(15) 2_556 ? O1 C1 1.3386(13) . ? C1 C2 1.3982(17) . ? C1 C9A 1.4040(17) . ? C2 C3 1.3882(17) . ? C2 H2A 0.9300 . ? C3 C3A 1.438(2) . ? C3 S3 1.7495(13) . ? C3A C4 1.4087(17) . ? C3A C9B 1.4244(17) . ? C4 C5 1.377(2) . ? C4 H4A 0.9300 . ? C5 C6 1.378(2) . ? C5 H5A 0.9300 . ? C6 C6A 1.4104(17) . ? C6 H6A 0.9300 . ? C6A C9B 1.4218(18) . ? C6A C7 1.4382(19) . ? C7 C8 1.3815(17) . ? C7 S7 1.7579(13) . ? C8 C9 1.3934(18) . ? C8 H8A 0.9300 . ? C9 O9 1.3323(13) . ? C9 C9A 1.4083(16) . ? C9A C9B 1.4216(15) . ? S3 C10 1.8018(17) . ? C10 C11 1.517(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.508(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? S7 C13 1.795(2) . ? C13 C14D 1.511(6) . ? C13 C14 1.555(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C13 H13D 0.9700 . ? C14 C15 1.523(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C14D C15D 1.540(7) . ? C14D H14C 0.9700 . ? C14D H14D 0.9700 . ? C15D H15D 0.9600 . ? C15D H15E 0.9600 . ? C15D H15F 0.9600 . ? 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 O1 B1 O1 108.02(15) 2_556 . ? O1 B1 O9 107.16(5) 2_556 . ? O1 B1 O9 113.42(5) . . ? O1 B1 O9 113.42(5) 2_556 2_556 ? O1 B1 O9 107.16(5) . 2_556 ? O9 B1 O9 107.80(15) . 2_556 ? C1 O1 B1 119.10(10) . . ? O1 C1 C2 118.80(11) . . ? O1 C1 C9A 120.68(10) . . ? C2 C1 C9A 120.52(11) . . ? C3 C2 C1 120.27(13) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C3A 120.82(11) . . ? C2 C3 S3 122.84(11) . . ? C3A C3 S3 116.32(9) . . ? C4 C3A C9B 118.11(13) . . ? C4 C3A C3 123.24(12) . . ? C9B C3A C3 118.63(10) . . ? C5 C4 C3A 121.08(13) . . ? C5 C4 H4A 119.5 . . ? C3A C4 H4A 119.5 . . ? C4 C5 C6 121.06(12) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C6A 120.83(14) . . ? C5 C6 H6A 119.6 . . ? C6A C6 H6A 119.6 . . ? C6 C6A C9B 118.32(12) . . ? C6 C6A C7 123.31(13) . . ? C9B C6A C7 118.35(10) . . ? C8 C7 C6A 120.72(12) . . ? C8 C7 S7 122.54(10) . . ? C6A C7 S7 116.74(9) . . ? C7 C8 C9 120.64(12) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? O9 C9 C8 119.46(11) . . ? O9 C9 C9A 119.85(11) . . ? C8 C9 C9A 120.68(10) . . ? C1 C9A C9 120.10(10) . . ? C1 C9A C9B 120.32(11) . . ? C9 C9A C9B 119.51(11) . . ? C9A C9B C6A 120.02(11) . . ? C9A C9B C3A 119.40(11) . . ? C6A C9B C3A 120.58(10) . . ? C9 O9 B1 119.85(8) . . ? C3 S3 C10 104.24(7) . . ? C11 C10 S3 108.82(11) . . ? C11 C10 H10A 109.9 . . ? S3 C10 H10A 109.9 . . ? C11 C10 H10B 109.9 . . ? S3 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C12 C11 C10 111.36(16) . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 S7 C13 105.52(8) . . ? C14D C13 C14 24.4(2) . . ? C14D C13 S7 104.2(3) . . ? C14 C13 S7 121.9(2) . . ? C14D C13 H13A 99.4 . . ? C14 C13 H13A 106.9 . . ? S7 C13 H13A 106.9 . . ? C14D C13 H13B 130.9 . . ? C14 C13 H13B 106.9 . . ? S7 C13 H13B 106.9 . . ? H13A C13 H13B 106.7 . . ? C14D C13 H13C 110.6 . . ? C14 C13 H13C 113.3 . . ? S7 C13 H13C 110.9 . . ? H13A C13 H13C 14.2 . . ? H13B C13 H13C 92.5 . . ? C14D C13 H13D 111.3 . . ? C14 C13 H13D 88.2 . . ? S7 C13 H13D 110.9 . . ? H13A C13 H13D 122.4 . . ? H13B C13 H13D 20.9 . . ? H13C C13 H13D 109.0 . . ? C15 C14 C13 110.7(3) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C13 C14D C15D 105.9(5) . . ? C13 C14D H14C 110.5 . . ? C15D C14D H14C 110.5 . . ? C13 C14D H14D 110.5 . . ? C15D C14D H14D 110.5 . . ? H14C C14D H14D 108.7 . . ? C14D C15D H15D 109.5 . . ? C14D C15D H15E 109.5 . . ? H15D C15D H15E 109.5 . . ? C14D C15D H15F 109.5 . . ? H15D C15D H15F 109.5 . . ? H15E C15D H15F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 B1 O1 C1 147.99(11) 2_556 . . . ? O9 B1 O1 C1 29.37(16) . . . . ? O9 B1 O1 C1 -89.47(11) 2_556 . . . ? B1 O1 C1 C2 164.62(11) . . . . ? B1 O1 C1 C9A -15.34(16) . . . . ? O1 C1 C2 C3 178.34(12) . . . . ? C9A C1 C2 C3 -1.7(2) . . . . ? C1 C2 C3 C3A 0.1(2) . . . . ? C1 C2 C3 S3 178.68(10) . . . . ? C2 C3 C3A C4 -177.18(13) . . . . ? S3 C3 C3A C4 4.15(18) . . . . ? C2 C3 C3A C9B 1.07(19) . . . . ? S3 C3 C3A C9B -177.60(9) . . . . ? C9B C3A C4 C5 1.5(2) . . . . ? C3 C3A C4 C5 179.80(14) . . . . ? C3A C4 C5 C6 -0.4(3) . . . . ? C4 C5 C6 C6A -0.2(3) . . . . ? C5 C6 C6A C9B -0.5(2) . . . . ? C5 C6 C6A C7 -178.70(14) . . . . ? C6 C6A C7 C8 175.79(13) . . . . ? C9B C6A C7 C8 -2.40(19) . . . . ? C6 C6A C7 S7 -4.78(18) . . . . ? C9B C6A C7 S7 177.02(9) . . . . ? C6A C7 C8 C9 2.4(2) . . . . ? S7 C7 C8 C9 -177.00(10) . . . . ? C7 C8 C9 O9 179.34(12) . . . . ? C7 C8 C9 C9A -0.04(19) . . . . ? O1 C1 C9A C9 -1.11(18) . . . . ? C2 C1 C9A C9 178.93(12) . . . . ? O1 C1 C9A C9B -177.94(11) . . . . ? C2 C1 C9A C9B 2.10(18) . . . . ? O9 C9 C9A C1 1.52(18) . . . . ? C8 C9 C9A C1 -179.11(11) . . . . ? O9 C9 C9A C9B 178.38(11) . . . . ? C8 C9 C9A C9B -2.24(18) . . . . ? C1 C9A C9B C6A 179.02(11) . . . . ? C9 C9A C9B C6A 2.17(17) . . . . ? C1 C9A C9B C3A -0.89(17) . . . . ? C9 C9A C9B C3A -177.75(11) . . . . ? C6 C6A C9B C9A -178.18(12) . . . . ? C7 C6A C9B C9A 0.11(17) . . . . ? C6 C6A C9B C3A 1.74(18) . . . . ? C7 C6A C9B C3A -179.98(11) . . . . ? C4 C3A C9B C9A 177.68(12) . . . . ? C3 C3A C9B C9A -0.66(18) . . . . ? C4 C3A C9B C6A -2.24(18) . . . . ? C3 C3A C9B C6A 179.42(11) . . . . ? C8 C9 O9 B1 -164.90(12) . . . . ? C9A C9 O9 B1 14.49(17) . . . . ? O1 B1 O9 C9 -148.30(10) 2_556 . . . ? O1 B1 O9 C9 -29.18(17) . . . . ? O9 B1 O9 C9 89.29(10) 2_556 . . . ? C2 C3 S3 C10 0.58(14) . . . . ? C3A C3 S3 C10 179.22(10) . . . . ? C3 S3 C10 C11 174.16(11) . . . . ? S3 C10 C11 C12 -176.03(14) . . . . ? C8 C7 S7 C13 10.71(14) . . . . ? C6A C7 S7 C13 -168.71(11) . . . . ? C7 S7 C13 C14D 83.6(3) . . . . ? C7 S7 C13 C14 65.1(2) . . . . ? C14D C13 C14 C15 24.6(7) . . . . ? S7 C13 C14 C15 72.5(4) . . . . ? C14 C13 C14D C15D -51.7(7) . . . . ? S7 C13 C14D C15D 168.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.341 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.050