# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Min Hyung Lee' _publ_contact_author_email LMH74@ULSAN.AC.KR _publ_section_title ; o-Carborane-Assisted Lewis Acidity Enhancement of Triarylboranes: Three Orders-of-Magnitude Increase of Fluoride Ion Affinity ; loop_ _publ_author_name 'Min Hyung Lee.' 'Youngkyu Do.' 'Jung Oh Huh.' 'Hyungjun Kim.' ; Kang Mun Lee ; 'Yoon Sup Lee.' # Attachment 'compound 1-F-revs.cif' data_1-F _database_code_depnum_ccdc_archive 'CCDC 746881' #TrackingRef 'compound 1-F-revs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C44H65B11FKO6 _chemical_formula_sum 'C44 H65 B11 F K O6' _chemical_formula_weight 866.97 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 14.5518(5) _cell_length_b 11.4399(4) _cell_length_c 15.0625(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.463(2) _cell_angle_gamma 90.00 _cell_volume 2499.87(16) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6986 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 24.72 _exptl_crystal_description cubic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.153 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25774 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 24.72 _reflns_number_total 6986 _reflns_number_gt 4744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker APEX II' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP3 _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^)+(0.1811P)^2^+0.4459P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(9) _refine_ls_number_reflns 6986 _refine_ls_number_parameters 614 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.1172 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2598 _refine_ls_wR_factor_gt 0.2162 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.002 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 0.5913(5) 0.1505(6) 1.1286(5) 0.0623(18) Uani 1 1 d . . . C3 C 0.4826(4) 0.1480(5) 1.1523(4) 0.0595(15) Uani 1 1 d . . . C4 C 0.4249(5) 0.0491(6) 1.1232(4) 0.0681(16) Uani 1 1 d . . . C5 C 0.3296(5) 0.0543(7) 1.1322(5) 0.079(2) Uani 1 1 d . . . H5 H 0.2939 -0.0107 1.1154 0.095 Uiso 1 1 calc R . . C6 C 0.2867(5) 0.1494(8) 1.1640(6) 0.089(2) Uani 1 1 d . . . C7 C 0.3414(5) 0.2421(6) 1.1915(5) 0.0727(17) Uani 1 1 d . . . H7 H 0.3136 0.3070 1.2153 0.087 Uiso 1 1 calc R . . C8 C 0.4357(4) 0.2440(6) 1.1858(5) 0.0686(17) Uani 1 1 d . . . C9 C 0.6644(4) 0.2179(5) 1.2017(4) 0.0644(16) Uani 1 1 d . . . C10 C 0.6674(5) 0.1801(6) 1.2925(4) 0.0700(17) Uani 1 1 d . . . C11 C 0.7303(5) 0.2273(7) 1.3566(5) 0.0767(18) Uani 1 1 d . . . H11 H 0.7292 0.2011 1.4150 0.092 Uiso 1 1 calc R . . C12 C 0.7940(5) 0.3105(7) 1.3385(5) 0.085(2) Uani 1 1 d . . . C13 C 0.7928(5) 0.3473(7) 1.2494(5) 0.0775(19) Uani 1 1 d . . . H13 H 0.8355 0.4032 1.2346 0.093 Uiso 1 1 calc R . . C14 C 0.7319(4) 0.3049(6) 1.1834(5) 0.0729(18) Uani 1 1 d . . . C15 C 0.5893(4) 0.1967(5) 1.0253(4) 0.0632(15) Uani 1 1 d . . . C16 C 0.6352(4) 0.1378(6) 0.9619(4) 0.0673(17) Uani 1 1 d . . . H16 H 0.6671 0.0699 0.9789 0.081 Uiso 1 1 calc R . . C17 C 0.6361(5) 0.1745(6) 0.8747(5) 0.0715(18) Uani 1 1 d . . . H17 H 0.6688 0.1319 0.8350 0.086 Uiso 1 1 calc R . . C18 C 0.5881(4) 0.2757(5) 0.8454(4) 0.0622(15) Uani 1 1 d . . . C19 C 0.5384(5) 0.3326(6) 0.9071(4) 0.0706(17) Uani 1 1 d . . . H19 H 0.5050 0.3992 0.8896 0.085 Uiso 1 1 calc R . . C20 C 0.5369(5) 0.2940(6) 0.9929(5) 0.0761(18) Uani 1 1 d . . . H20 H 0.5002 0.3331 1.0312 0.091 Uiso 1 1 calc R . . C21 C 0.7746(5) 0.3502(7) 0.7684(4) 0.0736(19) Uani 1 1 d . . . C22 C 0.7952(6) 0.4272(9) 0.8384(5) 0.098(3) Uani 1 1 d . . . H22 H 0.7550 0.4876 0.8499 0.118 Uiso 1 1 calc R . . C23 C 0.8776(8) 0.4119(11) 0.8911(6) 0.121(4) Uani 1 1 d . . . H23 H 0.8890 0.4592 0.9409 0.145 Uiso 1 1 calc R . . C24 C 0.9397(8) 0.3336(15) 0.8735(8) 0.133(4) Uani 1 1 d . . . H24 H 0.9955 0.3292 0.9078 0.160 Uiso 1 1 calc R . . C25 C 0.9202(7) 0.2572(14) 0.8023(8) 0.136(4) Uani 1 1 d . . . H25 H 0.9633 0.2008 0.7894 0.164 Uiso 1 1 calc R . . C26 C 0.8386(7) 0.2645(10) 0.7514(7) 0.112(3) Uani 1 1 d . . . H26 H 0.8258 0.2118 0.7050 0.134 Uiso 1 1 calc R . . C27 C 0.4615(6) -0.0614(7) 1.0887(6) 0.096(2) Uani 1 1 d . . . H27A H 0.4947 -0.1029 1.1365 0.144 Uiso 1 1 calc R . . H27B H 0.5021 -0.0442 1.0432 0.144 Uiso 1 1 calc R . . H27C H 0.4113 -0.1088 1.0642 0.144 Uiso 1 1 calc R . . C28 C 0.1822(6) 0.1552(11) 1.1672(11) 0.144(4) Uani 1 1 d . . . H28A H 0.1651 0.1195 1.2212 0.217 Uiso 1 1 calc R . . H28B H 0.1530 0.1145 1.1169 0.217 Uiso 1 1 calc R . . H28C H 0.1627 0.2354 1.1656 0.217 Uiso 1 1 calc R . . C29 C 0.4857(5) 0.3535(6) 1.2215(6) 0.079(2) Uani 1 1 d . . . H29A H 0.4428 0.4173 1.2217 0.118 Uiso 1 1 calc R . . H29B H 0.5341 0.3728 1.1842 0.118 Uiso 1 1 calc R . . H29C H 0.5116 0.3394 1.2811 0.118 Uiso 1 1 calc R . . C30 C 0.6031(6) 0.0878(7) 1.3212(5) 0.085(2) Uani 1 1 d . . . H30A H 0.5418 0.1190 1.3202 0.127 Uiso 1 1 calc R . . H30B H 0.6226 0.0627 1.3805 0.127 Uiso 1 1 calc R . . H30C H 0.6036 0.0223 1.2814 0.127 Uiso 1 1 calc R . . C31 C 0.8638(7) 0.3603(10) 1.4097(7) 0.120(3) Uani 1 1 d . . . H31A H 0.8409 0.4326 1.4317 0.181 Uiso 1 1 calc R . . H31B H 0.9213 0.3742 1.3842 0.181 Uiso 1 1 calc R . . H31C H 0.8732 0.3055 1.4578 0.181 Uiso 1 1 calc R . . C32 C 0.7418(7) 0.3538(8) 1.0927(6) 0.107(3) Uani 1 1 d . . . H32A H 0.8057 0.3683 1.0853 0.160 Uiso 1 1 calc R . . H32B H 0.7080 0.4257 1.0859 0.160 Uiso 1 1 calc R . . H32C H 0.7180 0.2988 1.0486 0.160 Uiso 1 1 calc R . . F1 F 0.6319(3) 0.0314(3) 1.1290(2) 0.0779(11) Uani 1 1 d . . . C1 C 0.5857(4) 0.3168(5) 0.7503(4) 0.0614(15) Uani 1 1 d . . . C2 C 0.6872(5) 0.3623(6) 0.7097(4) 0.0667(16) Uani 1 1 d . . . B2 B 0.5166(7) 0.2598(9) 0.6656(7) 0.085(2) Uani 1 1 d . . . B3 B 0.6324(6) 0.2341(9) 0.6717(6) 0.077(2) Uani 1 1 d . . . B4 B 0.6054(6) 0.4653(6) 0.7335(5) 0.072(2) Uani 1 1 d . . . B5 B 0.4958(6) 0.4006(8) 0.7030(6) 0.080(2) Uani 1 1 d . . . B6 B 0.4892(8) 0.3743(10) 0.5874(6) 0.094(3) Uani 1 1 d . . . B7 B 0.5742(7) 0.2689(10) 0.5701(6) 0.091(3) Uani 1 1 d . . . B8 B 0.6845(7) 0.3314(9) 0.6001(6) 0.086(2) Uani 1 1 d . . . B9 B 0.6612(8) 0.4781(8) 0.6370(6) 0.088(3) Uani 1 1 d . . . B10 B 0.5451(8) 0.5024(8) 0.6336(7) 0.098(3) Uani 1 1 d . . . B11 B 0.5950(8) 0.4195(9) 0.5459(6) 0.095(3) Uani 1 1 d . . . H33 H 0.477(5) 0.193(7) 0.694(5) 0.09(2) Uiso 1 1 d . . . H34 H 0.657(4) 0.156(6) 0.686(4) 0.066(17) Uiso 1 1 d . . . H35 H 0.617(4) 0.523(5) 0.804(4) 0.056(14) Uiso 1 1 d . . . H36 H 0.444(5) 0.417(6) 0.751(4) 0.076(19) Uiso 1 1 d . . . H37 H 0.417(6) 0.391(6) 0.561(5) 0.09(2) Uiso 1 1 d . . . H38 H 0.577(5) 0.203(7) 0.524(5) 0.08(2) Uiso 1 1 d . . . H39 H 0.757(6) 0.311(6) 0.578(5) 0.09(2) Uiso 1 1 d . . . H40 H 0.722(6) 0.532(7) 0.626(5) 0.10(2) Uiso 1 1 d . . . H41 H 0.500(4) 0.592(6) 0.618(4) 0.072(17) Uiso 1 1 d . . . H42 H 0.606(7) 0.494(9) 0.476(7) 0.15(4) Uiso 1 1 d . . . K1 K 0.76279(11) -0.11404(13) 1.15415(12) 0.0861(5) Uani 1 1 d . . . O1 O 0.8123(9) -0.1661(13) 1.3409(8) 0.189(4) Uani 1 1 d DU . . O2 O 0.6701(8) -0.2932(11) 1.2582(10) 0.191(4) Uani 1 1 d DU . . O3 O 0.6706(9) -0.3091(10) 1.0705(10) 0.196(4) Uani 1 1 d DU . . O4 O 0.7706(9) -0.1434(12) 0.9640(10) 0.217(5) Uani 1 1 d DU . . O5 O 0.8994(8) -0.0012(10) 1.0614(7) 0.186(4) Uani 1 1 d DU . . O6 O 0.8870(7) 0.0265(10) 1.2523(8) 0.178(4) Uani 1 1 d DU . . C43 C 0.7582(17) -0.2278(18) 1.3871(17) 0.217(8) Uani 1 1 d DU . . H43A H 0.7098 -0.1784 1.4072 0.261 Uiso 1 1 calc R . . H43B H 0.7930 -0.2595 1.4391 0.261 Uiso 1 1 calc R . . C44 C 0.7161(17) -0.326(2) 1.3311(15) 0.236(9) Uani 1 1 d DU . . H44A H 0.7650 -0.3784 1.3159 0.284 Uiso 1 1 calc R . . H44B H 0.6753 -0.3701 1.3666 0.284 Uiso 1 1 calc R . . C45 C 0.6362(14) -0.3803(16) 1.2091(13) 0.186(6) Uani 1 1 d DU . . H45A H 0.5847 -0.4131 1.2378 0.223 Uiso 1 1 calc R . . H45B H 0.6831 -0.4405 1.2084 0.223 Uiso 1 1 calc R . . C46 C 0.6041(18) -0.3522(18) 1.1148(16) 0.218(8) Uani 1 1 d DU . . H46A H 0.5805 -0.4227 1.0854 0.262 Uiso 1 1 calc R . . H46B H 0.5541 -0.2961 1.1143 0.262 Uiso 1 1 calc R . . C47 C 0.6442(12) -0.2859(16) 0.9860(10) 0.178(6) Uani 1 1 d DU . . H47A H 0.5947 -0.2289 0.9819 0.213 Uiso 1 1 calc R . . H47B H 0.6229 -0.3564 0.9551 0.213 Uiso 1 1 calc R . . C48 C 0.7259(11) -0.2393(13) 0.9474(12) 0.165(5) Uani 1 1 d DU . . H48A H 0.7719 -0.3004 0.9565 0.198 Uiso 1 1 calc R . . H48B H 0.7094 -0.2373 0.8838 0.198 Uiso 1 1 calc R . . C49 C 0.8472(11) -0.0965(14) 0.9426(12) 0.162(5) Uani 1 1 d DU . . H49A H 0.8413 -0.0873 0.8784 0.194 Uiso 1 1 calc R . . H49B H 0.8948 -0.1548 0.9555 0.194 Uiso 1 1 calc R . . C50 C 0.8817(10) 0.0053(14) 0.9760(8) 0.148(4) Uani 1 1 d DU . . H50A H 0.9377 0.0242 0.9482 0.178 Uiso 1 1 calc R . . H50B H 0.8375 0.0674 0.9622 0.178 Uiso 1 1 calc R . . C51 C 0.9185(9) 0.0733(15) 1.1221(11) 0.159(4) Uani 1 1 d DU . . H51A H 0.8624 0.1193 1.1181 0.191 Uiso 1 1 calc R . . H51B H 0.9627 0.1216 1.0940 0.191 Uiso 1 1 calc R . . C52 C 0.9467(10) 0.0887(13) 1.2080(11) 0.156(5) Uani 1 1 d DU . . H52A H 0.9448 0.1707 1.2240 0.187 Uiso 1 1 calc R . . H52B H 1.0091 0.0600 1.2206 0.187 Uiso 1 1 calc R . . C53 C 0.9076(13) -0.0148(16) 1.3313(13) 0.178(5) Uani 1 1 d DU . . H53A H 0.9291 0.0515 1.3674 0.214 Uiso 1 1 calc R . . H53B H 0.9609 -0.0645 1.3262 0.214 Uiso 1 1 calc R . . C54 C 0.8511(13) -0.0751(15) 1.3813(11) 0.166(5) Uani 1 1 d DU . . H54A H 0.8860 -0.1013 1.4351 0.199 Uiso 1 1 calc R . . H54B H 0.8031 -0.0230 1.3988 0.199 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 0.068(4) 0.063(4) 0.058(4) 0.010(3) 0.020(3) 0.022(3) C3 0.066(4) 0.048(3) 0.066(4) 0.010(3) 0.011(3) 0.003(3) C4 0.079(4) 0.066(4) 0.060(4) 0.014(3) 0.010(3) -0.004(3) C5 0.083(5) 0.071(4) 0.082(5) 0.016(4) 0.003(4) -0.015(4) C6 0.067(5) 0.092(5) 0.112(6) 0.021(5) 0.023(4) 0.006(4) C7 0.062(4) 0.070(4) 0.088(5) 0.007(3) 0.023(3) 0.008(3) C8 0.056(4) 0.067(4) 0.085(4) 0.009(3) 0.015(3) 0.010(3) C9 0.053(3) 0.072(4) 0.070(4) 0.011(3) 0.017(3) 0.014(3) C10 0.065(4) 0.079(4) 0.068(4) 0.013(3) 0.016(3) 0.007(3) C11 0.074(4) 0.088(5) 0.068(4) 0.005(3) 0.005(3) -0.004(4) C12 0.082(5) 0.094(5) 0.081(5) -0.002(4) 0.018(4) 0.005(4) C13 0.065(4) 0.076(4) 0.094(5) 0.003(4) 0.016(4) -0.002(3) C14 0.060(4) 0.079(4) 0.081(4) 0.012(4) 0.016(3) 0.012(3) C15 0.061(3) 0.064(4) 0.065(4) 0.004(3) 0.009(3) 0.013(3) C16 0.074(4) 0.067(4) 0.063(4) 0.011(3) 0.013(3) 0.023(3) C17 0.072(4) 0.064(4) 0.082(5) -0.014(3) 0.023(3) 0.018(3) C18 0.062(3) 0.058(3) 0.068(4) -0.003(3) 0.012(3) 0.003(3) C19 0.075(4) 0.067(4) 0.070(4) 0.005(3) 0.006(3) 0.020(3) C20 0.079(4) 0.085(4) 0.067(4) 0.003(3) 0.023(3) 0.023(4) C21 0.066(4) 0.092(5) 0.064(4) -0.016(4) 0.017(3) -0.028(4) C22 0.099(6) 0.117(6) 0.079(5) -0.026(5) 0.006(4) -0.038(5) C23 0.095(7) 0.179(10) 0.088(6) -0.042(6) 0.008(5) -0.046(7) C24 0.079(6) 0.210(13) 0.111(8) 0.025(8) 0.008(6) -0.040(8) C25 0.077(6) 0.227(14) 0.104(8) -0.010(8) 0.006(5) 0.004(7) C26 0.090(6) 0.144(8) 0.102(6) -0.019(6) 0.010(5) -0.004(6) C27 0.114(6) 0.057(4) 0.118(6) -0.013(4) 0.024(5) -0.007(4) C28 0.062(5) 0.134(8) 0.239(14) 0.011(9) 0.019(7) -0.018(5) C29 0.064(4) 0.060(4) 0.116(6) -0.012(4) 0.027(4) 0.005(3) C30 0.091(5) 0.087(5) 0.078(5) 0.018(4) 0.017(4) -0.007(4) C31 0.109(7) 0.133(7) 0.116(7) 0.007(6) -0.010(5) -0.039(6) C32 0.111(7) 0.121(7) 0.090(6) 0.037(5) 0.018(5) -0.041(5) F1 0.092(3) 0.066(2) 0.077(2) 0.0067(18) 0.011(2) 0.0312(19) C1 0.060(3) 0.061(3) 0.064(4) 0.001(3) 0.010(3) -0.002(3) C2 0.074(4) 0.068(4) 0.059(4) -0.010(3) 0.014(3) -0.016(3) B2 0.082(5) 0.083(5) 0.087(6) 0.008(5) -0.010(5) -0.015(5) B3 0.089(6) 0.086(6) 0.058(4) -0.021(4) 0.010(4) -0.022(5) B4 0.091(5) 0.059(4) 0.065(5) 0.000(4) 0.013(4) 0.002(4) B5 0.073(5) 0.086(5) 0.080(5) 0.015(4) 0.004(4) 0.003(4) B6 0.091(6) 0.116(7) 0.071(5) 0.013(5) -0.008(5) 0.000(5) B7 0.103(7) 0.107(7) 0.061(5) -0.006(5) -0.005(5) -0.026(5) B8 0.095(6) 0.097(6) 0.068(5) -0.014(4) 0.017(4) -0.031(5) B9 0.123(8) 0.076(5) 0.066(5) 0.004(4) 0.004(5) -0.022(6) B10 0.135(8) 0.079(6) 0.079(6) 0.014(5) 0.008(5) -0.003(6) B11 0.114(7) 0.101(6) 0.070(5) 0.010(5) 0.003(5) -0.026(6) K1 0.0667(9) 0.0796(10) 0.1095(12) 0.0037(9) -0.0084(8) 0.0117(8) O1 0.177(7) 0.203(8) 0.189(7) 0.003(7) 0.026(6) 0.049(7) O2 0.153(7) 0.184(7) 0.239(9) 0.006(7) 0.038(7) -0.004(6) O3 0.185(7) 0.165(7) 0.237(9) -0.028(7) 0.008(7) 0.061(6) O4 0.201(9) 0.224(9) 0.227(9) 0.030(7) 0.009(7) 0.060(8) O5 0.165(7) 0.196(7) 0.199(8) 0.006(7) 0.027(6) 0.041(6) O6 0.135(6) 0.194(7) 0.202(8) -0.023(6) 0.001(6) 0.043(6) C43 0.231(12) 0.181(10) 0.239(12) 0.022(9) 0.017(9) 0.014(9) C44 0.226(12) 0.256(13) 0.228(12) 0.011(10) 0.019(9) 0.005(10) C45 0.184(10) 0.172(9) 0.200(10) -0.035(8) 0.004(8) 0.000(8) C46 0.220(11) 0.195(11) 0.243(12) -0.003(9) 0.037(9) 0.008(9) C47 0.169(9) 0.192(9) 0.164(9) -0.042(8) -0.033(8) 0.006(8) C48 0.157(9) 0.135(8) 0.194(9) -0.015(7) -0.037(8) 0.000(7) C49 0.120(7) 0.172(9) 0.196(9) 0.060(8) 0.028(7) 0.008(7) C50 0.160(8) 0.179(9) 0.105(6) 0.007(6) 0.007(6) 0.076(7) C51 0.111(7) 0.192(9) 0.177(9) -0.066(8) 0.019(7) -0.011(7) C52 0.124(7) 0.157(8) 0.190(9) -0.002(7) 0.030(7) -0.046(7) C53 0.192(9) 0.171(9) 0.179(9) -0.001(8) 0.063(8) 0.063(8) C54 0.190(9) 0.171(9) 0.136(8) -0.011(7) 0.012(7) 0.003(8) _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 F1 1.485(8) . ? B1 C15 1.641(10) . ? B1 C3 1.648(10) . ? B1 C9 1.660(11) . ? C3 C8 1.407(9) . ? C3 C4 1.457(9) . ? C4 C5 1.405(10) . ? C4 C27 1.482(10) . ? C5 C6 1.359(11) . ? C6 C7 1.371(11) . ? C6 C28 1.527(12) . ? C7 C8 1.382(9) . ? C8 C29 1.526(10) . ? C9 C10 1.432(9) . ? C9 C14 1.441(9) . ? C10 C11 1.388(10) . ? C10 C30 1.497(10) . ? C11 C12 1.371(11) . ? C12 C13 1.405(11) . ? C12 C31 1.529(13) . ? C13 C14 1.368(11) . ? C14 C32 1.494(11) . ? C15 C16 1.381(9) . ? C15 C20 1.416(9) . ? C16 C17 1.381(9) . ? C17 C18 1.406(9) . ? C18 C19 1.384(9) . ? C18 C1 1.505(9) . ? C19 C20 1.367(10) . ? C21 C22 1.389(10) . ? C21 C26 1.390(13) . ? C21 C2 1.498(10) . ? C22 C23 1.396(15) . ? C23 C24 1.314(17) . ? C24 C25 1.395(18) . ? C25 C26 1.365(14) . ? C1 B2 1.692(11) . ? C1 B3 1.698(11) . ? C1 C2 1.723(9) . ? C1 B5 1.730(10) . ? C1 B4 1.744(10) . ? C2 B8 1.685(11) . ? C2 B4 1.732(11) . ? C2 B9 1.741(11) . ? C2 B3 1.745(10) . ? B2 B3 1.705(14) . ? B2 B7 1.723(15) . ? B2 B5 1.741(14) . ? B2 B6 1.786(14) . ? B3 B7 1.736(13) . ? B3 B8 1.762(13) . ? B4 B9 1.725(14) . ? B4 B10 1.734(13) . ? B4 B5 1.785(13) . ? B5 B10 1.755(14) . ? B5 B6 1.763(14) . ? B6 B7 1.761(17) . ? B6 B11 1.782(16) . ? B6 B10 1.790(15) . ? B7 B8 1.782(13) . ? B7 B11 1.791(15) . ? B8 B11 1.792(16) . ? B8 B9 1.809(14) . ? B9 B10 1.710(16) . ? B9 B11 1.749(13) . ? B10 B11 1.823(16) . ? K1 O6 2.761(11) . ? K1 O5 2.830(12) . ? K1 O3 2.847(13) . ? K1 O4 2.895(15) . ? K1 O1 2.910(12) . ? K1 O2 2.967(12) . ? O1 C43 1.298(15) . ? O1 C54 1.311(15) . ? O2 C44 1.297(16) . ? O2 C45 1.313(15) . ? O3 C46 1.314(15) . ? O3 C47 1.327(14) . ? O4 C48 1.290(12) . ? O4 C49 1.300(12) . ? O5 C51 1.265(11) . ? O5 C50 1.294(11) . ? O6 C53 1.294(13) . ? O6 C52 1.341(12) . ? C43 C44 1.51(3) . ? C45 C46 1.49(2) . ? C47 C48 1.46(2) . ? C49 C50 1.349(19) . ? C51 C52 1.337(19) . ? C53 C54 1.35(2) . ? 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 F1 B1 C15 106.1(5) . . ? F1 B1 C3 111.8(5) . . ? C15 B1 C3 105.4(5) . . ? F1 B1 C9 100.9(5) . . ? C15 B1 C9 116.2(6) . . ? C3 B1 C9 116.1(5) . . ? C8 C3 C4 115.4(6) . . ? C8 C3 B1 124.4(5) . . ? C4 C3 B1 119.2(6) . . ? C5 C4 C3 119.3(6) . . ? C5 C4 C27 117.0(7) . . ? C3 C4 C27 123.6(6) . . ? C6 C5 C4 123.4(7) . . ? C5 C6 C7 117.1(7) . . ? C5 C6 C28 122.1(9) . . ? C7 C6 C28 120.8(8) . . ? C6 C7 C8 123.3(7) . . ? C7 C8 C3 121.5(6) . . ? C7 C8 C29 116.1(6) . . ? C3 C8 C29 122.4(6) . . ? C10 C9 C14 114.8(6) . . ? C10 C9 B1 117.6(6) . . ? C14 C9 B1 127.3(6) . . ? C11 C10 C9 121.2(6) . . ? C11 C10 C30 117.8(6) . . ? C9 C10 C30 121.1(6) . . ? C12 C11 C10 123.4(7) . . ? C11 C12 C13 116.2(7) . . ? C11 C12 C31 122.8(7) . . ? C13 C12 C31 121.0(8) . . ? C14 C13 C12 123.1(7) . . ? C13 C14 C9 121.3(6) . . ? C13 C14 C32 115.4(7) . . ? C9 C14 C32 123.3(7) . . ? C16 C15 C20 115.0(6) . . ? C16 C15 B1 121.6(5) . . ? C20 C15 B1 123.3(6) . . ? C17 C16 C15 123.3(5) . . ? C16 C17 C18 120.5(6) . . ? C19 C18 C17 116.7(6) . . ? C19 C18 C1 121.2(5) . . ? C17 C18 C1 122.0(6) . . ? C20 C19 C18 122.0(6) . . ? C19 C20 C15 122.1(6) . . ? C22 C21 C26 118.6(8) . . ? C22 C21 C2 120.8(8) . . ? C26 C21 C2 120.5(6) . . ? C21 C22 C23 118.5(10) . . ? C24 C23 C22 123.0(9) . . ? C23 C24 C25 118.7(10) . . ? C26 C25 C24 120.6(12) . . ? C25 C26 C21 120.4(10) . . ? C18 C1 B2 124.4(6) . . ? C18 C1 B3 120.6(6) . . ? B2 C1 B3 60.4(5) . . ? C18 C1 C2 118.4(5) . . ? B2 C1 C2 108.9(5) . . ? B3 C1 C2 61.3(4) . . ? C18 C1 B5 121.7(6) . . ? B2 C1 B5 61.2(5) . . ? B3 C1 B5 110.6(6) . . ? C2 C1 B5 109.2(5) . . ? C18 C1 B4 116.8(5) . . ? B2 C1 B4 111.1(6) . . ? B3 C1 B4 111.2(5) . . ? C2 C1 B4 59.9(4) . . ? B5 C1 B4 61.8(5) . . ? C21 C2 B8 120.8(6) . . ? C21 C2 C1 118.3(5) . . ? B8 C2 C1 109.2(5) . . ? C21 C2 B4 120.5(5) . . ? B8 C2 B4 112.4(6) . . ? C1 C2 B4 60.6(4) . . ? C21 C2 B9 125.1(6) . . ? B8 C2 B9 63.7(5) . . ? C1 C2 B9 107.6(6) . . ? B4 C2 B9 59.6(5) . . ? C21 C2 B3 117.4(6) . . ? B8 C2 B3 61.8(5) . . ? C1 C2 B3 58.6(4) . . ? B4 C2 B3 109.6(6) . . ? B9 C2 B3 111.3(6) . . ? C1 B2 B3 60.0(4) . . ? C1 B2 B7 107.9(6) . . ? B3 B2 B7 60.9(6) . . ? C1 B2 B5 60.5(5) . . ? B3 B2 B5 109.7(6) . . ? B7 B2 B5 108.8(7) . . ? C1 B2 B6 107.7(7) . . ? B3 B2 B6 109.3(8) . . ? B7 B2 B6 60.2(6) . . ? B5 B2 B6 60.0(6) . . ? C1 B3 B2 59.6(5) . . ? C1 B3 B7 107.0(7) . . ? B2 B3 B7 60.1(6) . . ? C1 B3 C2 60.1(4) . . ? B2 B3 C2 107.3(7) . . ? B7 B3 C2 106.0(7) . . ? C1 B3 B8 106.8(6) . . ? B2 B3 B8 109.2(8) . . ? B7 B3 B8 61.3(5) . . ? C2 B3 B8 57.5(4) . . ? B9 B4 C2 60.5(5) . . ? B9 B4 B10 59.3(6) . . ? C2 B4 B10 107.3(6) . . ? B9 B4 C1 107.4(6) . . ? C2 B4 C1 59.4(4) . . ? B10 B4 C1 106.7(6) . . ? B9 B4 B5 106.8(6) . . ? C2 B4 B5 106.3(5) . . ? B10 B4 B5 59.8(6) . . ? C1 B4 B5 58.7(4) . . ? C1 B5 B2 58.4(5) . . ? C1 B5 B10 106.4(6) . . ? B2 B5 B10 109.4(7) . . ? C1 B5 B6 107.0(7) . . ? B2 B5 B6 61.3(6) . . ? B10 B5 B6 61.2(6) . . ? C1 B5 B4 59.5(4) . . ? B2 B5 B4 107.0(6) . . ? B10 B5 B4 58.6(5) . . ? B6 B5 B4 107.6(7) . . ? B7 B6 B5 106.2(7) . . ? B7 B6 B11 60.7(6) . . ? B5 B6 B11 108.4(7) . . ? B7 B6 B2 58.1(6) . . ? B5 B6 B2 58.8(5) . . ? B11 B6 B2 106.8(7) . . ? B7 B6 B10 108.4(7) . . ? B5 B6 B10 59.2(6) . . ? B11 B6 B10 61.4(6) . . ? B2 B6 B10 105.8(6) . . ? B2 B7 B3 59.1(5) . . ? B2 B7 B6 61.7(6) . . ? B3 B7 B6 109.1(7) . . ? B2 B7 B8 107.4(6) . . ? B3 B7 B8 60.1(5) . . ? B6 B7 B8 108.5(7) . . ? B2 B7 B11 109.2(8) . . ? B3 B7 B11 108.7(6) . . ? B6 B7 B11 60.2(7) . . ? B8 B7 B11 60.2(6) . . ? C2 B8 B3 60.8(4) . . ? C2 B8 B7 106.5(6) . . ? B3 B8 B7 58.7(5) . . ? C2 B8 B11 106.8(7) . . ? B3 B8 B11 107.6(7) . . ? B7 B8 B11 60.1(6) . . ? C2 B8 B9 59.6(5) . . ? B3 B8 B9 107.3(6) . . ? B7 B8 B9 105.3(8) . . ? B11 B8 B9 58.1(6) . . ? B10 B9 B4 60.6(6) . . ? B10 B9 C2 107.9(7) . . ? B4 B9 C2 60.0(5) . . ? B10 B9 B11 63.6(7) . . ? B4 B9 B11 111.2(8) . . ? C2 B9 B11 106.3(6) . . ? B10 B9 B8 110.4(7) . . ? B4 B9 B8 106.9(6) . . ? C2 B9 B8 56.7(5) . . ? B11 B9 B8 60.5(6) . . ? B9 B10 B4 60.1(6) . . ? B9 B10 B5 108.9(7) . . ? B4 B10 B5 61.6(5) . . ? B9 B10 B6 107.3(7) . . ? B4 B10 B6 108.7(6) . . ? B5 B10 B6 59.6(6) . . ? B9 B10 B11 59.2(6) . . ? B4 B10 B11 107.3(7) . . ? B5 B10 B11 106.9(7) . . ? B6 B10 B11 59.1(6) . . ? B9 B11 B6 105.9(7) . . ? B9 B11 B7 107.5(6) . . ? B6 B11 B7 59.0(6) . . ? B9 B11 B8 61.4(6) . . ? B6 B11 B8 107.1(6) . . ? B7 B11 B8 59.6(6) . . ? B9 B11 B10 57.2(6) . . ? B6 B11 B10 59.5(6) . . ? B7 B11 B10 105.6(7) . . ? B8 B11 B10 106.2(6) . . ? O6 K1 O5 62.8(4) . . ? O6 K1 O3 163.7(3) . . ? O5 K1 O3 117.6(4) . . ? O6 K1 O4 121.5(4) . . ? O5 K1 O4 58.7(3) . . ? O3 K1 O4 61.6(4) . . ? O6 K1 O1 59.9(4) . . ? O5 K1 O1 116.1(4) . . ? O3 K1 O1 109.9(4) . . ? O4 K1 O1 155.0(3) . . ? O6 K1 O2 115.2(4) . . ? O5 K1 O2 160.3(3) . . ? O3 K1 O2 58.3(4) . . ? O4 K1 O2 119.8(4) . . ? O1 K1 O2 55.7(4) . . ? C43 O1 C54 116.1(18) . . ? C43 O1 K1 120.9(14) . . ? C54 O1 K1 110.6(11) . . ? C44 O2 C45 113.8(18) . . ? C44 O2 K1 115.0(14) . . ? C45 O2 K1 113.1(13) . . ? C46 O3 C47 113.2(17) . . ? C46 O3 K1 114.2(13) . . ? C47 O3 K1 111.1(11) . . ? C48 O4 C49 137.1(18) . . ? C48 O4 K1 103.4(11) . . ? C49 O4 K1 107.3(12) . . ? C51 O5 C50 134.1(16) . . ? C51 O5 K1 94.2(9) . . ? C50 O5 K1 115.0(10) . . ? C53 O6 C52 122.6(14) . . ? C53 O6 K1 112.0(12) . . ? C52 O6 K1 117.7(10) . . ? O1 C43 C44 110(2) . . ? O2 C44 C43 115(2) . . ? O2 C45 C46 116.6(18) . . ? O3 C46 C45 112(2) . . ? O3 C47 C48 105.7(14) . . ? O4 C48 C47 130.3(17) . . ? O4 C49 C50 124.4(18) . . ? O5 C50 C49 111.2(16) . . ? O5 C51 C52 145.3(18) . . ? C51 C52 O6 104.4(13) . . ? O6 C53 C54 126(2) . . ? O1 C54 C53 114.0(16) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.534 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.136 # Attachment 'compound 1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 746882' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C32H41B11 _chemical_formula_sum 'C32 H41 B11' _chemical_formula_weight 544.56 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3388(7) _cell_length_b 21.7577(12) _cell_length_c 13.6469(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.822(4) _cell_angle_gamma 90.00 _cell_volume 3295.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5207 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 24.11 _exptl_crystal_description cubic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.057 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24356 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 24.11 _reflns_number_total 5207 _reflns_number_gt 3518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker APEX II' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP3 _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^)+(0.0807P)^2^+0.6421P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5207 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 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 C18 C 0.72606(18) 0.13692(8) 0.76214(15) 0.0448(5) Uani 1 1 d . . . C1 C 0.63819(18) 0.08447(9) 0.75644(15) 0.0483(5) Uani 1 1 d . . . C15 C 0.87950(18) 0.24050(9) 0.77031(15) 0.0501(5) Uani 1 1 d . . . C19 C 0.7308(2) 0.17066(9) 0.67669(15) 0.0517(5) Uani 1 1 d . . . H19 H 0.6816 0.1597 0.6160 0.062 Uiso 1 1 calc R . . C14 C 0.8668(2) 0.35833(9) 0.91458(17) 0.0566(6) Uani 1 1 d . . . C20 C 0.8077(2) 0.22032(9) 0.68046(16) 0.0556(6) Uani 1 1 d . . . H20 H 0.8117 0.2409 0.6215 0.067 Uiso 1 1 calc R . . C21 C 0.5080(2) 0.15341(12) 0.86885(17) 0.0617(6) Uani 1 1 d . . . C10 C 1.0808(2) 0.36642(9) 0.92146(16) 0.0550(6) Uani 1 1 d . . . C17 C 0.80230(19) 0.15393(9) 0.85104(16) 0.0538(6) Uani 1 1 d . . . H17 H 0.8043 0.1307 0.9085 0.065 Uiso 1 1 calc R . . C9 C 0.96767(19) 0.34269(9) 0.87282(15) 0.0497(5) Uani 1 1 d . . . C16 C 0.8753(2) 0.20519(10) 0.85492(16) 0.0566(6) Uani 1 1 d . . . H16 H 0.9232 0.2165 0.9160 0.068 Uiso 1 1 calc R . . C3 C 1.00838(19) 0.32243(9) 0.68331(16) 0.0519(5) Uani 1 1 d . . . C2 C 0.51681(18) 0.09471(9) 0.81266(15) 0.0493(5) Uani 1 1 d . . . C11 C 1.0909(2) 0.40209(10) 1.00705(17) 0.0663(6) Uani 1 1 d . . . H11 H 1.1669 0.4158 1.0387 0.080 Uiso 1 1 calc R . . C4 C 1.0935(2) 0.28550(10) 0.64812(17) 0.0598(6) Uani 1 1 d . . . C13 C 0.8822(3) 0.39659(11) 0.99820(19) 0.0675(7) Uani 1 1 d . . . H13 H 0.8143 0.4082 1.0221 0.081 Uiso 1 1 calc R . . C12 C 0.9931(3) 0.41816(11) 1.04732(18) 0.0673(7) Uani 1 1 d . . . C8 C 0.9779(2) 0.37946(10) 0.63529(16) 0.0580(6) Uani 1 1 d . . . B1 B 0.9535(2) 0.30190(11) 0.77548(19) 0.0511(6) Uani 1 1 d . . . C32 C 0.7404(2) 0.33695(11) 0.8713(2) 0.0779(8) Uani 1 1 d . . . H32A H 0.7289 0.2964 0.8956 0.117 Uiso 1 1 calc R . . H32B H 0.7280 0.3361 0.7996 0.117 Uiso 1 1 calc R . . H32C H 0.6837 0.3647 0.8913 0.117 Uiso 1 1 calc R . . C5 C 1.1476(2) 0.30703(13) 0.57172(19) 0.0728(7) Uani 1 1 d . . . H5 H 1.2050 0.2825 0.5507 0.087 Uiso 1 1 calc R . . C7 C 1.0339(2) 0.39790(11) 0.55880(17) 0.0716(7) Uani 1 1 d . . . H7 H 1.0126 0.4356 0.5281 0.086 Uiso 1 1 calc R . . B3 B 0.4959(2) 0.09687(12) 0.68378(18) 0.0532(7) Uani 1 1 d . . . C6 C 1.1196(2) 0.36299(14) 0.52622(18) 0.0758(8) Uani 1 1 d . . . B8 B 0.3919(3) 0.05928(13) 0.7444(2) 0.0596(7) Uani 1 1 d . . . C27 C 1.1312(3) 0.22341(11) 0.6941(2) 0.0834(8) Uani 1 1 d . . . H27A H 1.0650 0.1952 0.6777 0.125 Uiso 1 1 calc R . . H27B H 1.1543 0.2275 0.7655 0.125 Uiso 1 1 calc R . . H27C H 1.1982 0.2082 0.6682 0.125 Uiso 1 1 calc R . . C30 C 1.1952(2) 0.35199(13) 0.8851(2) 0.0850(8) Uani 1 1 d . . . H30A H 1.2632 0.3683 0.9315 0.127 Uiso 1 1 calc R . . H30B H 1.1912 0.3703 0.8205 0.127 Uiso 1 1 calc R . . H30C H 1.2037 0.3083 0.8802 0.127 Uiso 1 1 calc R . . C22 C 0.4707(2) 0.20781(12) 0.8196(2) 0.0811(8) Uani 1 1 d . . . H22 H 0.4539 0.2088 0.7499 0.097 Uiso 1 1 calc R . . B2 B 0.5945(3) 0.04134(13) 0.6508(2) 0.0665(8) Uani 1 1 d . . . B7 B 0.4392(3) 0.02417(14) 0.6415(2) 0.0717(9) Uani 1 1 d . . . C31 C 1.0069(3) 0.45672(13) 1.14059(19) 0.0977(10) Uani 1 1 d . . . H31A H 1.0147 0.4304 1.1980 0.147 Uiso 1 1 calc R . . H31B H 0.9372 0.4824 1.1365 0.147 Uiso 1 1 calc R . . H31C H 1.0774 0.4820 1.1468 0.147 Uiso 1 1 calc R . . C26 C 0.5325(3) 0.15309(17) 0.9724(2) 0.1016(10) Uani 1 1 d . . . H26 H 0.5571 0.1171 1.0073 0.122 Uiso 1 1 calc R . . B4 B 0.6299(3) 0.04370(13) 0.8638(2) 0.0662(8) Uani 1 1 d . . . B11 B 0.4269(3) -0.01980(14) 0.7485(3) 0.0787(9) Uani 1 1 d . . . C25 C 0.5199(4) 0.2072(3) 1.0241(4) 0.153(2) Uani 1 1 d . . . H25 H 0.5375 0.2073 1.0937 0.184 Uiso 1 1 calc R . . C29 C 0.8820(3) 0.41998(11) 0.6632(2) 0.0819(8) Uani 1 1 d . . . H29A H 0.8746 0.4569 0.6239 0.123 Uiso 1 1 calc R . . H29B H 0.9040 0.4303 0.7330 0.123 Uiso 1 1 calc R . . H29C H 0.8065 0.3985 0.6505 0.123 Uiso 1 1 calc R . . C24 C 0.4825(4) 0.2597(3) 0.9742(6) 0.170(3) Uani 1 1 d . . . H24 H 0.4732 0.2953 1.0096 0.205 Uiso 1 1 calc R . . B9 B 0.4745(3) 0.02643(14) 0.8553(2) 0.0705(8) Uani 1 1 d . . . B6 B 0.5509(3) -0.03066(14) 0.6902(3) 0.0897(11) Uani 1 1 d . . . B10 B 0.5730(3) -0.02903(15) 0.8223(3) 0.0911(11) Uani 1 1 d . . . C23 C 0.4584(3) 0.26055(16) 0.8726(4) 0.1226(14) Uani 1 1 d . . . H23 H 0.4334 0.2968 0.8386 0.147 Uiso 1 1 calc R . . B5 B 0.6767(3) 0.00834(12) 0.7618(3) 0.0766(9) Uani 1 1 d . . . C28 C 1.1791(3) 0.38520(17) 0.4425(2) 0.1171(12) Uani 1 1 d . . . H28A H 1.2170 0.4242 0.4605 0.176 Uiso 1 1 calc R . . H28B H 1.1193 0.3895 0.3820 0.176 Uiso 1 1 calc R . . H28C H 1.2387 0.3559 0.4322 0.176 Uiso 1 1 calc R . . H34 H 0.4778(18) 0.1417(9) 0.6468(15) 0.061(6) Uiso 1 1 d . . . H39 H 0.306(2) 0.0810(9) 0.7456(15) 0.066(6) Uiso 1 1 d . . . H33 H 0.638(2) 0.0537(10) 0.5917(17) 0.080(7) Uiso 1 1 d . . . H40 H 0.438(2) 0.0284(10) 0.9234(18) 0.088(7) Uiso 1 1 d . . . H36 H 0.771(3) 0.0000(11) 0.7695(18) 0.093(8) Uiso 1 1 d . . . H42 H 0.356(2) -0.0544(11) 0.7469(17) 0.089(7) Uiso 1 1 d . . . H35 H 0.691(2) 0.0567(9) 0.9349(17) 0.070(7) Uiso 1 1 d . . . H38 H 0.377(2) 0.0203(11) 0.5697(19) 0.091(8) Uiso 1 1 d . . . H41 H 0.600(3) -0.0672(13) 0.867(2) 0.105(9) Uiso 1 1 d . . . H37 H 0.558(2) -0.0729(13) 0.6506(19) 0.104(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C18 0.0438(12) 0.0440(11) 0.0486(12) -0.0014(9) 0.0139(10) -0.0016(9) C1 0.0486(13) 0.0479(11) 0.0529(12) -0.0009(10) 0.0209(11) -0.0030(9) C15 0.0469(13) 0.0521(12) 0.0515(13) -0.0002(10) 0.0109(11) -0.0047(10) C19 0.0563(14) 0.0575(12) 0.0424(12) -0.0050(10) 0.0127(10) -0.0128(11) C14 0.0556(15) 0.0536(12) 0.0656(15) 0.0091(11) 0.0238(12) 0.0004(11) C20 0.0632(15) 0.0579(13) 0.0486(13) 0.0038(10) 0.0184(12) -0.0111(11) C21 0.0469(14) 0.0783(17) 0.0644(15) -0.0261(13) 0.0217(12) -0.0116(12) C10 0.0536(15) 0.0552(12) 0.0578(13) -0.0032(11) 0.0154(11) -0.0063(11) C17 0.0539(14) 0.0540(12) 0.0513(13) 0.0103(10) 0.0059(11) -0.0045(11) C9 0.0519(14) 0.0476(11) 0.0523(12) 0.0036(10) 0.0165(11) -0.0038(10) C16 0.0521(14) 0.0602(13) 0.0532(13) 0.0021(11) 0.0005(11) -0.0084(11) C3 0.0493(13) 0.0514(12) 0.0563(13) -0.0102(10) 0.0139(11) -0.0131(10) C2 0.0473(13) 0.0590(13) 0.0447(12) -0.0038(10) 0.0170(10) -0.0062(10) C11 0.0724(17) 0.0648(14) 0.0603(15) -0.0062(12) 0.0103(13) -0.0092(12) C4 0.0554(15) 0.0605(14) 0.0649(15) -0.0143(11) 0.0156(12) -0.0103(11) C13 0.0786(19) 0.0631(14) 0.0720(16) 0.0070(13) 0.0412(15) 0.0111(13) C12 0.089(2) 0.0598(14) 0.0578(15) -0.0004(12) 0.0255(15) 0.0042(14) C8 0.0666(16) 0.0536(13) 0.0536(13) -0.0061(11) 0.0118(12) -0.0132(11) B1 0.0379(14) 0.0516(13) 0.0629(16) 0.0036(12) 0.0078(12) 0.0024(11) C32 0.0546(16) 0.0761(16) 0.109(2) 0.0036(15) 0.0312(15) 0.0030(13) C5 0.0588(16) 0.0950(19) 0.0697(17) -0.0220(15) 0.0253(13) -0.0136(14) C7 0.0863(19) 0.0695(15) 0.0578(15) 0.0014(12) 0.0117(14) -0.0238(14) B3 0.0537(17) 0.0618(16) 0.0446(14) -0.0054(12) 0.0113(12) -0.0095(12) C6 0.0762(19) 0.096(2) 0.0584(15) -0.0097(15) 0.0223(14) -0.0326(16) B8 0.0508(17) 0.0726(17) 0.0588(16) -0.0152(13) 0.0195(14) -0.0128(14) C27 0.0772(19) 0.0722(17) 0.105(2) -0.0112(15) 0.0293(16) 0.0099(14) C30 0.0531(16) 0.111(2) 0.094(2) -0.0298(17) 0.0209(14) -0.0145(14) C22 0.0655(17) 0.0700(17) 0.113(2) -0.0298(16) 0.0308(16) 0.0016(14) B2 0.0714(19) 0.0649(16) 0.0737(19) -0.0248(15) 0.0394(16) -0.0214(14) B7 0.069(2) 0.083(2) 0.0691(19) -0.0296(16) 0.0294(17) -0.0275(16) C31 0.138(3) 0.0889(19) 0.0706(18) -0.0167(15) 0.0303(18) 0.0081(18) C26 0.091(2) 0.151(3) 0.0673(18) -0.0465(19) 0.0275(16) -0.0200(19) B4 0.0587(18) 0.0671(17) 0.0731(19) 0.0220(15) 0.0146(16) -0.0056(14) B11 0.078(2) 0.0641(18) 0.105(2) -0.0150(17) 0.0433(19) -0.0257(16) C25 0.110(3) 0.243(6) 0.114(3) -0.120(4) 0.043(3) -0.035(4) C29 0.105(2) 0.0661(15) 0.0770(17) 0.0057(13) 0.0231(16) 0.0148(15) C24 0.082(3) 0.196(5) 0.242(7) -0.164(6) 0.054(4) -0.030(3) B9 0.072(2) 0.0755(19) 0.0709(19) 0.0089(15) 0.0296(16) -0.0167(15) B6 0.086(2) 0.0589(17) 0.141(3) -0.034(2) 0.062(2) -0.0208(16) B10 0.084(2) 0.0592(18) 0.138(3) 0.029(2) 0.039(2) -0.0030(17) C23 0.074(2) 0.093(2) 0.209(4) -0.071(3) 0.049(3) -0.0018(17) B5 0.064(2) 0.0476(15) 0.127(3) 0.0001(16) 0.0394(19) 0.0000(14) C28 0.121(3) 0.164(3) 0.078(2) 0.001(2) 0.0488(19) -0.044(2) _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 C18 C17 1.388(3) . ? C18 C19 1.388(3) . ? C18 C1 1.507(3) . ? C1 B2 1.706(3) . ? C1 B5 1.710(3) . ? C1 C2 1.722(3) . ? C1 B4 1.731(3) . ? C1 B3 1.734(3) . ? C15 C16 1.396(3) . ? C15 C20 1.396(3) . ? C15 B1 1.571(3) . ? C19 C20 1.383(3) . ? C14 C13 1.394(3) . ? C14 C9 1.420(3) . ? C14 C32 1.508(3) . ? C21 C26 1.383(4) . ? C21 C22 1.384(4) . ? C21 C2 1.503(3) . ? C10 C11 1.387(3) . ? C10 C9 1.416(3) . ? C10 C30 1.514(3) . ? C17 C16 1.384(3) . ? C9 B1 1.578(3) . ? C3 C8 1.413(3) . ? C3 C4 1.413(3) . ? C3 B1 1.578(3) . ? C2 B9 1.700(3) . ? C2 B8 1.711(3) . ? C2 B3 1.727(3) . ? C2 B4 1.731(4) . ? C11 C12 1.380(3) . ? C4 C5 1.395(3) . ? C4 C27 1.514(3) . ? C13 C12 1.381(3) . ? C12 C31 1.506(3) . ? C8 C7 1.388(3) . ? C8 C29 1.508(3) . ? C5 C6 1.374(4) . ? C7 C6 1.376(4) . ? B3 B7 1.760(4) . ? B3 B2 1.767(4) . ? B3 B8 1.773(3) . ? C6 C28 1.520(3) . ? B8 B9 1.760(4) . ? B8 B11 1.764(4) . ? B8 B7 1.776(4) . ? C22 C23 1.379(4) . ? B2 B6 1.760(4) . ? B2 B5 1.761(5) . ? B2 B7 1.780(4) . ? B7 B6 1.767(5) . ? B7 B11 1.775(5) . ? C26 C25 1.396(5) . ? B4 B10 1.758(5) . ? B4 B5 1.764(4) . ? B4 B9 1.782(4) . ? B11 B9 1.763(5) . ? B11 B10 1.765(5) . ? B11 B6 1.767(4) . ? C25 C24 1.352(7) . ? C24 C23 1.357(7) . ? B9 B10 1.765(5) . ? B6 B10 1.768(6) . ? B6 B5 1.771(5) . ? B10 B5 1.767(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 C17 C18 C19 117.96(18) . . ? C17 C18 C1 122.27(18) . . ? C19 C18 C1 119.76(18) . . ? C18 C1 B2 122.31(16) . . ? C18 C1 B5 124.84(18) . . ? B2 C1 B5 62.03(18) . . ? C18 C1 C2 117.35(15) . . ? B2 C1 C2 109.12(16) . . ? B5 C1 C2 109.04(16) . . ? C18 C1 B4 119.65(18) . . ? B2 C1 B4 112.11(18) . . ? B5 C1 B4 61.66(17) . . ? C2 C1 B4 60.15(13) . . ? C18 C1 B3 116.10(17) . . ? B2 C1 B3 61.80(15) . . ? B5 C1 B3 112.00(19) . . ? C2 C1 B3 59.95(12) . . ? B4 C1 B3 110.97(17) . . ? C16 C15 C20 116.16(18) . . ? C16 C15 B1 122.63(19) . . ? C20 C15 B1 121.09(19) . . ? C20 C19 C18 121.0(2) . . ? C13 C14 C9 119.7(2) . . ? C13 C14 C32 117.0(2) . . ? C9 C14 C32 123.3(2) . . ? C19 C20 C15 121.87(19) . . ? C26 C21 C22 118.6(3) . . ? C26 C21 C2 119.8(3) . . ? C22 C21 C2 121.6(2) . . ? C11 C10 C9 120.6(2) . . ? C11 C10 C30 117.6(2) . . ? C9 C10 C30 121.71(19) . . ? C16 C17 C18 120.59(19) . . ? C10 C9 C14 116.84(19) . . ? C10 C9 B1 121.75(18) . . ? C14 C9 B1 121.4(2) . . ? C17 C16 C15 122.3(2) . . ? C8 C3 C4 117.45(19) . . ? C8 C3 B1 121.29(19) . . ? C4 C3 B1 121.22(19) . . ? C21 C2 B9 120.97(18) . . ? C21 C2 B8 121.74(18) . . ? B9 C2 B8 62.13(16) . . ? C21 C2 C1 118.68(16) . . ? B9 C2 C1 110.30(16) . . ? B8 C2 C1 110.33(15) . . ? C21 C2 B3 119.13(19) . . ? B9 C2 B3 112.53(18) . . ? B8 C2 B3 62.10(14) . . ? C1 C2 B3 60.36(13) . . ? C21 C2 B4 117.41(19) . . ? B9 C2 B4 62.57(15) . . ? B8 C2 B4 113.12(18) . . ? C1 C2 B4 60.20(13) . . ? B3 C2 B4 111.35(17) . . ? C12 C11 C10 122.9(2) . . ? C5 C4 C3 119.9(2) . . ? C5 C4 C27 118.6(2) . . ? C3 C4 C27 121.4(2) . . ? C12 C13 C14 123.3(2) . . ? C11 C12 C13 116.6(2) . . ? C11 C12 C31 121.7(3) . . ? C13 C12 C31 121.7(2) . . ? C7 C8 C3 119.8(2) . . ? C7 C8 C29 119.1(2) . . ? C3 C8 C29 121.1(2) . . ? C15 B1 C3 119.94(19) . . ? C15 B1 C9 118.50(18) . . ? C3 B1 C9 121.54(18) . . ? C6 C5 C4 122.6(2) . . ? C6 C7 C8 123.0(2) . . ? C2 B3 C1 59.69(12) . . ? C2 B3 B7 105.91(19) . . ? C1 B3 B7 106.4(2) . . ? C2 B3 B2 106.2(2) . . ? C1 B3 B2 58.35(15) . . ? B7 B3 B2 60.62(16) . . ? C2 B3 B8 58.52(14) . . ? C1 B3 B8 106.94(18) . . ? B7 B3 B8 60.35(14) . . ? B2 B3 B8 108.66(19) . . ? C5 C6 C7 117.2(2) . . ? C5 C6 C28 121.6(3) . . ? C7 C6 C28 121.2(3) . . ? C2 B8 B9 58.64(15) . . ? C2 B8 B11 105.5(2) . . ? B9 B8 B11 60.02(19) . . ? C2 B8 B3 59.38(13) . . ? B9 B8 B3 107.53(19) . . ? B11 B8 B3 107.32(19) . . ? C2 B8 B7 105.88(18) . . ? B9 B8 B7 108.2(2) . . ? B11 B8 B7 60.18(17) . . ? B3 B8 B7 59.45(15) . . ? C23 C22 C21 120.7(3) . . ? C1 B2 B6 106.4(2) . . ? C1 B2 B5 59.10(15) . . ? B6 B2 B5 60.4(2) . . ? C1 B2 B3 59.86(14) . . ? B6 B2 B3 107.36(19) . . ? B5 B2 B3 108.09(19) . . ? C1 B2 B7 106.69(18) . . ? B6 B2 B7 59.91(18) . . ? B5 B2 B7 108.5(2) . . ? B3 B2 B7 59.49(15) . . ? B3 B7 B6 107.3(2) . . ? B3 B7 B11 107.5(2) . . ? B6 B7 B11 59.85(19) . . ? B3 B7 B8 60.20(14) . . ? B6 B7 B8 107.6(2) . . ? B11 B7 B8 59.59(16) . . ? B3 B7 B2 59.89(15) . . ? B6 B7 B2 59.50(18) . . ? B11 B7 B2 107.3(2) . . ? B8 B7 B2 108.0(2) . . ? C21 C26 C25 119.5(4) . . ? C2 B4 C1 59.66(13) . . ? C2 B4 B10 104.8(2) . . ? C1 B4 B10 105.6(2) . . ? C2 B4 B5 106.2(2) . . ? C1 B4 B5 58.58(15) . . ? B10 B4 B5 60.22(18) . . ? C2 B4 B9 57.89(15) . . ? C1 B4 B9 106.1(2) . . ? B10 B4 B9 59.80(18) . . ? B5 B4 B9 108.1(2) . . ? B9 B11 B8 59.88(16) . . ? B9 B11 B10 60.0(2) . . ? B8 B11 B10 107.9(2) . . ? B9 B11 B6 108.1(2) . . ? B8 B11 B6 108.1(2) . . ? B10 B11 B6 60.1(2) . . ? B9 B11 B7 108.10(19) . . ? B8 B11 B7 60.23(16) . . ? B10 B11 B7 107.9(2) . . ? B6 B11 B7 59.87(19) . . ? C24 C25 C26 120.8(5) . . ? C25 C24 C23 120.2(4) . . ? C2 B9 B8 59.23(15) . . ? C2 B9 B11 106.0(2) . . ? B8 B9 B11 60.10(18) . . ? C2 B9 B10 105.79(19) . . ? B8 B9 B10 108.1(2) . . ? B11 B9 B10 60.1(2) . . ? C2 B9 B4 59.55(14) . . ? B8 B9 B4 108.35(19) . . ? B11 B9 B4 107.7(2) . . ? B10 B9 B4 59.43(18) . . ? B2 B6 B11 108.5(2) . . ? B2 B6 B7 60.59(18) . . ? B11 B6 B7 60.28(18) . . ? B2 B6 B10 107.7(2) . . ? B11 B6 B10 59.9(2) . . ? B7 B6 B10 108.1(2) . . ? B2 B6 B5 59.81(17) . . ? B11 B6 B5 108.2(2) . . ? B7 B6 B5 108.5(2) . . ? B10 B6 B5 59.9(2) . . ? B4 B10 B9 60.77(17) . . ? B4 B10 B11 108.7(2) . . ? B9 B10 B11 59.92(19) . . ? B4 B10 B5 60.06(17) . . ? B9 B10 B5 108.7(2) . . ? B11 B10 B5 108.5(3) . . ? B4 B10 B6 108.2(2) . . ? B9 B10 B6 108.0(3) . . ? B11 B10 B6 60.0(2) . . ? B5 B10 B6 60.1(2) . . ? C24 C23 C22 120.3(4) . . ? C1 B5 B2 58.87(15) . . ? C1 B5 B4 59.75(14) . . ? B2 B5 B4 108.0(2) . . ? C1 B5 B10 106.1(2) . . ? B2 B5 B10 107.7(2) . . ? B4 B5 B10 59.72(18) . . ? C1 B5 B6 105.7(2) . . ? B2 B5 B6 59.8(2) . . ? B4 B5 B6 107.8(2) . . ? B10 B5 B6 60.0(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.11 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.152 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.030 # Attachment 'compound 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 746883' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C27H39B11 _chemical_formula_sum 'C27 H39 B11' _chemical_formula_weight 482.49 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.9560(4) _cell_length_b 27.7402(15) _cell_length_c 13.6954(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.533(3) _cell_angle_gamma 90.00 _cell_volume 3016.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6956 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 27.60 _exptl_crystal_description cubic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.054 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56299 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.60 _reflns_number_total 6956 _reflns_number_gt 4803 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker APEX II' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP3 _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^)+(0.1028P)^2^+0.5314P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6956 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1658 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.1713(2) 0.09893(6) 0.22537(13) 0.0407(4) Uani 1 1 d . . . C3 C 0.24747(19) 0.08490(5) 0.12501(11) 0.0388(3) Uani 1 1 d . . . C4 C 0.1442(2) 0.07438(6) 0.03988(12) 0.0418(4) Uani 1 1 d . . . C5 C 0.2165(2) 0.06277(6) -0.04723(12) 0.0482(4) Uani 1 1 d . . . H5 H 0.1459 0.0553 -0.1018 0.058 Uiso 1 1 calc R . . C6 C 0.3881(2) 0.06191(6) -0.05585(13) 0.0517(4) Uani 1 1 d . . . C7 C 0.4889(2) 0.07209(7) 0.02751(13) 0.0537(4) Uani 1 1 d . . . H7 H 0.6052 0.0719 0.0236 0.064 Uiso 1 1 calc R . . C8 C 0.4234(2) 0.08267(6) 0.11699(12) 0.0441(4) Uani 1 1 d . . . C9 C 0.2109(2) 0.06953(6) 0.32276(12) 0.0431(4) Uani 1 1 d . . . C10 C 0.1712(2) 0.01989(6) 0.32731(13) 0.0488(4) Uani 1 1 d . . . C11 C 0.1968(3) -0.00527(7) 0.41498(15) 0.0610(5) Uani 1 1 d . . . H11 H 0.1673 -0.0377 0.4169 0.073 Uiso 1 1 calc R . . C12 C 0.2647(3) 0.01644(8) 0.49920(14) 0.0634(5) Uani 1 1 d . . . C13 C 0.3061(3) 0.06455(8) 0.49470(13) 0.0624(5) Uani 1 1 d . . . H13 H 0.3529 0.0796 0.5507 0.075 Uiso 1 1 calc R . . C14 C 0.2804(2) 0.09158(7) 0.40902(12) 0.0513(4) Uani 1 1 d . . . C15 C 0.0456(2) 0.14304(6) 0.22769(11) 0.0422(4) Uani 1 1 d . . . C16 C -0.0636(2) 0.14832(6) 0.30344(12) 0.0471(4) Uani 1 1 d . . . H16 H -0.0551 0.1269 0.3557 0.057 Uiso 1 1 calc R . . C17 C -0.1837(2) 0.18439(6) 0.30305(12) 0.0479(4) Uani 1 1 d . . . H17 H -0.2547 0.1865 0.3544 0.057 Uiso 1 1 calc R . . C18 C -0.1994(2) 0.21751(6) 0.22656(12) 0.0427(4) Uani 1 1 d . . . C19 C -0.0885(2) 0.21378(6) 0.15180(13) 0.0497(4) Uani 1 1 d . . . H19 H -0.0946 0.2360 0.1008 0.060 Uiso 1 1 calc R . . C20 C 0.0306(2) 0.17736(6) 0.15287(12) 0.0487(4) Uani 1 1 d . . . H20 H 0.1030 0.1757 0.1022 0.058 Uiso 1 1 calc R . . C21 C -0.1744(3) 0.30845(8) 0.36377(17) 0.0743(6) Uani 1 1 d . . . H21A H -0.1661 0.2803 0.4045 0.112 Uiso 1 1 calc R . . H21B H -0.1863 0.3365 0.4038 0.112 Uiso 1 1 calc R . . H21C H -0.0744 0.3114 0.3284 0.112 Uiso 1 1 calc R . . C22 C -0.0456(2) 0.07241(7) 0.03983(14) 0.0546(4) Uani 1 1 d . . . H22A H -0.0935 0.0963 -0.0044 0.082 Uiso 1 1 calc R . . H22B H -0.0798 0.0787 0.1046 0.082 Uiso 1 1 calc R . . H22C H -0.0840 0.0410 0.0193 0.082 Uiso 1 1 calc R . . C23 C 0.4648(3) 0.05045(10) -0.15147(16) 0.0798(7) Uani 1 1 d . . . H23A H 0.3803 0.0369 -0.1964 0.120 Uiso 1 1 calc R . . H23B H 0.5548 0.0277 -0.1400 0.120 Uiso 1 1 calc R . . H23C H 0.5081 0.0795 -0.1787 0.120 Uiso 1 1 calc R . . C24 C 0.5467(2) 0.09186(8) 0.20275(14) 0.0619(5) Uani 1 1 d . . . H24A H 0.6571 0.0819 0.1866 0.093 Uiso 1 1 calc R . . H24B H 0.5135 0.0739 0.2583 0.093 Uiso 1 1 calc R . . H24C H 0.5479 0.1256 0.2180 0.093 Uiso 1 1 calc R . . C25 C 0.0924(3) -0.00675(7) 0.23994(15) 0.0652(5) Uani 1 1 d . . . H25A H 0.0902 -0.0406 0.2539 0.098 Uiso 1 1 calc R . . H25B H 0.1575 -0.0012 0.1843 0.098 Uiso 1 1 calc R . . H25C H -0.0204 0.0046 0.2261 0.098 Uiso 1 1 calc R . . C26 C 0.2932(4) -0.01215(11) 0.59251(17) 0.0926(8) Uani 1 1 d . . . H26A H 0.4093 -0.0096 0.6157 0.139 Uiso 1 1 calc R . . H26B H 0.2657 -0.0454 0.5801 0.139 Uiso 1 1 calc R . . H26C H 0.2230 0.0004 0.6411 0.139 Uiso 1 1 calc R . . C27 C 0.3358(3) 0.14371(8) 0.41087(15) 0.0679(6) Uani 1 1 d . . . H27A H 0.2575 0.1626 0.4454 0.102 Uiso 1 1 calc R . . H27B H 0.3390 0.1554 0.3451 0.102 Uiso 1 1 calc R . . H27C H 0.4459 0.1462 0.4433 0.102 Uiso 1 1 calc R . . B2 B -0.4352(3) 0.26933(8) 0.10845(17) 0.0573(5) Uani 1 1 d . . . B3 B -0.2937(3) 0.31025(8) 0.16972(17) 0.0561(5) Uani 1 1 d . . . B4 B -0.4712(3) 0.25981(8) 0.31471(18) 0.0579(5) Uani 1 1 d . . . B5 B -0.5455(3) 0.23799(8) 0.19846(19) 0.0597(6) Uani 1 1 d . . . B6 B -0.6433(3) 0.28681(9) 0.1335(2) 0.0689(6) Uani 1 1 d . . . B7 B -0.4876(3) 0.33138(9) 0.1159(2) 0.0658(6) Uani 1 1 d . . . B8 B -0.4137(3) 0.35267(8) 0.2319(2) 0.0666(6) Uani 1 1 d . . . B9 B -0.5228(4) 0.32170(9) 0.3214(2) 0.0703(7) Uani 1 1 d . . . B10 B -0.6643(3) 0.28054(9) 0.2616(2) 0.0713(7) Uani 1 1 d . . . B11 B -0.6291(3) 0.33853(9) 0.2101(2) 0.0720(7) Uani 1 1 d . . . C1 C -0.3386(2) 0.25464(6) 0.21933(13) 0.0453(4) Uani 1 1 d . . . C2 C -0.3256(2) 0.30401(6) 0.29248(14) 0.0553(5) Uani 1 1 d . . . H29 H -0.160(3) 0.3161(7) 0.1525(14) 0.064(6) Uiso 1 1 d . . . H30 H -0.448(2) 0.2397(7) 0.3796(14) 0.056(5) Uiso 1 1 d . . . H28 H -0.393(3) 0.2504(7) 0.0448(14) 0.061(5) Uiso 1 1 d . . . H34 H -0.356(3) 0.3872(8) 0.2454(15) 0.077(6) Uiso 1 1 d . . . H32 H -0.749(3) 0.2820(8) 0.0817(16) 0.080(7) Uiso 1 1 d . . . H31 H -0.569(2) 0.1995(7) 0.1904(13) 0.058(5) Uiso 1 1 d . . . H37 H -0.731(3) 0.3659(7) 0.2071(14) 0.068(6) Uiso 1 1 d . . . H33 H -0.489(3) 0.3527(9) 0.0517(18) 0.089(7) Uiso 1 1 d . . . H35 H -0.530(3) 0.3368(8) 0.3926(17) 0.082(7) Uiso 1 1 d . . . H36 H -0.782(3) 0.2691(8) 0.2963(15) 0.072(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0352(9) 0.0413(9) 0.0456(10) -0.0016(7) 0.0035(7) -0.0024(7) C3 0.0352(8) 0.0383(8) 0.0430(8) 0.0024(6) 0.0027(6) 0.0022(6) C4 0.0390(8) 0.0410(8) 0.0453(9) 0.0018(6) 0.0017(7) 0.0002(6) C5 0.0515(10) 0.0488(9) 0.0439(9) -0.0027(7) -0.0003(7) 0.0015(8) C6 0.0555(10) 0.0523(10) 0.0481(9) 0.0006(8) 0.0095(8) 0.0120(8) C7 0.0364(9) 0.0641(11) 0.0614(11) 0.0002(9) 0.0093(8) 0.0091(8) C8 0.0376(8) 0.0454(9) 0.0492(9) -0.0002(7) 0.0014(7) 0.0039(7) C9 0.0386(8) 0.0482(9) 0.0430(8) 0.0005(7) 0.0053(7) 0.0046(7) C10 0.0458(9) 0.0481(9) 0.0529(10) 0.0060(7) 0.0061(8) 0.0035(7) C11 0.0603(12) 0.0564(11) 0.0670(13) 0.0166(9) 0.0106(10) 0.0047(9) C12 0.0573(12) 0.0823(14) 0.0511(11) 0.0182(10) 0.0085(9) 0.0137(10) C13 0.0598(12) 0.0854(15) 0.0419(10) 0.0021(9) 0.0026(8) 0.0051(10) C14 0.0496(10) 0.0603(11) 0.0443(9) -0.0026(8) 0.0055(7) 0.0042(8) C15 0.0409(8) 0.0429(8) 0.0429(8) -0.0016(7) 0.0045(7) 0.0003(7) C16 0.0505(10) 0.0463(9) 0.0453(9) 0.0046(7) 0.0081(7) 0.0053(7) C17 0.0495(10) 0.0470(9) 0.0482(9) -0.0005(7) 0.0126(8) 0.0043(7) C18 0.0409(8) 0.0386(8) 0.0488(9) -0.0028(7) 0.0036(7) -0.0002(7) C19 0.0515(10) 0.0461(9) 0.0522(10) 0.0084(7) 0.0097(8) 0.0058(8) C20 0.0488(9) 0.0508(9) 0.0478(9) 0.0037(7) 0.0135(7) 0.0049(8) C21 0.0797(15) 0.0627(13) 0.0784(14) -0.0180(11) -0.0131(12) 0.0056(11) C22 0.0401(9) 0.0665(12) 0.0565(10) 0.0008(9) -0.0014(8) -0.0039(8) C23 0.0861(16) 0.0964(17) 0.0593(12) -0.0055(11) 0.0237(11) 0.0256(13) C24 0.0396(9) 0.0803(14) 0.0650(12) -0.0075(10) -0.0051(9) 0.0034(9) C25 0.0779(14) 0.0486(11) 0.0688(12) 0.0001(9) 0.0025(11) -0.0102(10) C26 0.0959(19) 0.118(2) 0.0642(14) 0.0367(14) 0.0100(13) 0.0196(16) C27 0.0797(14) 0.0692(13) 0.0542(11) -0.0122(9) -0.0001(10) -0.0131(11) B2 0.0563(12) 0.0562(12) 0.0586(13) -0.0014(10) -0.0020(10) 0.0083(10) B3 0.0570(13) 0.0431(11) 0.0687(13) 0.0059(9) 0.0071(10) 0.0037(9) B4 0.0557(13) 0.0524(12) 0.0675(14) 0.0008(10) 0.0189(11) 0.0095(10) B5 0.0458(11) 0.0509(12) 0.0826(16) -0.0041(11) 0.0044(11) 0.0002(9) B6 0.0545(13) 0.0648(15) 0.0858(17) -0.0036(12) -0.0081(12) 0.0113(11) B7 0.0638(14) 0.0556(13) 0.0776(16) 0.0093(11) 0.0007(12) 0.0136(11) B8 0.0703(15) 0.0405(11) 0.0887(17) -0.0043(11) 0.0022(13) 0.0092(10) B9 0.0732(16) 0.0605(14) 0.0783(16) -0.0110(12) 0.0138(13) 0.0233(12) B10 0.0517(13) 0.0635(14) 0.1002(19) 0.0012(13) 0.0176(13) 0.0120(11) B11 0.0636(15) 0.0587(14) 0.0940(19) -0.0013(12) 0.0072(13) 0.0201(12) C1 0.0444(9) 0.0380(8) 0.0542(10) -0.0029(7) 0.0071(7) 0.0018(7) C2 0.0582(11) 0.0426(9) 0.0651(11) -0.0094(8) 0.0029(9) 0.0062(8) _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 C9 1.578(2) . ? B1 C15 1.582(2) . ? B1 C3 1.585(2) . ? C3 C8 1.412(2) . ? C3 C4 1.415(2) . ? C4 C5 1.394(2) . ? C4 C22 1.510(2) . ? C5 C6 1.378(3) . ? C6 C7 1.384(3) . ? C6 C23 1.512(2) . ? C7 C8 1.392(2) . ? C8 C24 1.505(2) . ? C9 C14 1.413(2) . ? C9 C10 1.415(2) . ? C10 C11 1.393(3) . ? C10 C25 1.509(3) . ? C11 C12 1.381(3) . ? C12 C13 1.377(3) . ? C12 C26 1.509(3) . ? C13 C14 1.397(3) . ? C14 C27 1.511(3) . ? C15 C20 1.398(2) . ? C15 C16 1.401(2) . ? C16 C17 1.383(2) . ? C17 C18 1.393(2) . ? C18 C19 1.396(2) . ? C18 C1 1.511(2) . ? C19 C20 1.384(2) . ? C21 C2 1.507(3) . ? B2 C1 1.709(3) . ? B2 B3 1.773(3) . ? B2 B7 1.776(3) . ? B2 B6 1.779(3) . ? B2 B5 1.783(3) . ? B3 C2 1.724(3) . ? B3 C1 1.732(3) . ? B3 B8 1.767(3) . ? B3 B7 1.768(3) . ? B4 C2 1.727(3) . ? B4 C1 1.735(3) . ? B4 B10 1.756(4) . ? B4 B9 1.769(3) . ? B4 B5 1.770(4) . ? B5 C1 1.717(3) . ? B5 B10 1.771(3) . ? B5 B6 1.774(4) . ? B6 B7 1.777(4) . ? B6 B11 1.777(4) . ? B6 B10 1.782(4) . ? B7 B8 1.762(4) . ? B7 B11 1.775(4) . ? B8 C2 1.711(3) . ? B8 B11 1.766(4) . ? B8 B9 1.767(4) . ? B9 C2 1.713(3) . ? B9 B11 1.760(4) . ? B9 B10 1.768(4) . ? B10 B11 1.786(4) . ? C1 C2 1.696(2) . ? 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 C9 B1 C15 118.44(14) . . ? C9 B1 C3 122.62(14) . . ? C15 B1 C3 118.91(14) . . ? C8 C3 C4 117.07(14) . . ? C8 C3 B1 120.82(14) . . ? C4 C3 B1 122.11(14) . . ? C5 C4 C3 120.24(15) . . ? C5 C4 C22 117.16(15) . . ? C3 C4 C22 122.52(14) . . ? C6 C5 C4 122.74(16) . . ? C5 C6 C7 116.94(16) . . ? C5 C6 C23 122.21(19) . . ? C7 C6 C23 120.85(18) . . ? C6 C7 C8 122.67(16) . . ? C7 C8 C3 120.29(15) . . ? C7 C8 C24 117.49(15) . . ? C3 C8 C24 122.22(15) . . ? C14 C9 C10 117.48(15) . . ? C14 C9 B1 122.04(15) . . ? C10 C9 B1 120.44(15) . . ? C11 C10 C9 120.30(17) . . ? C11 C10 C25 118.01(17) . . ? C9 C10 C25 121.62(16) . . ? C12 C11 C10 122.03(19) . . ? C13 C12 C11 117.87(18) . . ? C13 C12 C26 121.5(2) . . ? C11 C12 C26 120.6(2) . . ? C12 C13 C14 122.33(19) . . ? C13 C14 C9 119.98(18) . . ? C13 C14 C27 118.17(17) . . ? C9 C14 C27 121.80(16) . . ? C20 C15 C16 116.27(15) . . ? C20 C15 B1 122.51(14) . . ? C16 C15 B1 121.14(14) . . ? C17 C16 C15 122.16(15) . . ? C16 C17 C18 120.64(15) . . ? C17 C18 C19 118.12(15) . . ? C17 C18 C1 122.00(14) . . ? C19 C18 C1 119.76(14) . . ? C20 C19 C18 120.62(15) . . ? C19 C20 C15 122.14(15) . . ? C1 B2 B3 59.62(12) . . ? C1 B2 B7 105.94(16) . . ? B3 B2 B7 59.78(14) . . ? C1 B2 B6 105.50(17) . . ? B3 B2 B6 107.80(17) . . ? B7 B2 B6 59.99(14) . . ? C1 B2 B5 58.86(12) . . ? B3 B2 B5 108.07(16) . . ? B7 B2 B5 107.80(17) . . ? B6 B2 B5 59.75(14) . . ? C2 B3 C1 58.79(11) . . ? C2 B3 B8 58.69(13) . . ? C1 B3 B8 105.88(16) . . ? C2 B3 B7 105.24(16) . . ? C1 B3 B7 105.28(16) . . ? B8 B3 B7 59.80(15) . . ? C2 B3 B2 105.66(15) . . ? C1 B3 B2 58.34(12) . . ? B8 B3 B2 107.97(17) . . ? B7 B3 B2 60.19(14) . . ? C2 B4 C1 58.69(11) . . ? C2 B4 B10 105.89(17) . . ? C1 B4 B10 105.82(17) . . ? C2 B4 B9 58.69(13) . . ? C1 B4 B9 105.84(16) . . ? B10 B4 B9 60.21(15) . . ? C2 B4 B5 105.94(16) . . ? C1 B4 B5 58.64(12) . . ? B10 B4 B5 60.29(15) . . ? B9 B4 B5 108.20(18) . . ? C1 B5 B4 59.65(12) . . ? C1 B5 B10 105.94(16) . . ? B4 B5 B10 59.44(14) . . ? C1 B5 B6 105.35(16) . . ? B4 B5 B6 107.59(17) . . ? B10 B5 B6 60.35(15) . . ? C1 B5 B2 58.42(12) . . ? B4 B5 B2 107.69(16) . . ? B10 B5 B2 108.24(17) . . ? B6 B5 B2 60.01(14) . . ? B5 B6 B7 108.14(17) . . ? B5 B6 B11 108.06(19) . . ? B7 B6 B11 59.92(15) . . ? B5 B6 B2 60.24(13) . . ? B7 B6 B2 59.92(14) . . ? B11 B6 B2 107.93(18) . . ? B5 B6 B10 59.73(14) . . ? B7 B6 B10 108.04(19) . . ? B11 B6 B10 60.23(16) . . ? B2 B6 B10 107.93(18) . . ? B8 B7 B3 60.06(14) . . ? B8 B7 B11 59.89(16) . . ? B3 B7 B11 108.06(18) . . ? B8 B7 B2 108.06(17) . . ? B3 B7 B2 60.04(13) . . ? B11 B7 B2 108.16(18) . . ? B8 B7 B6 107.92(19) . . ? B3 B7 B6 108.07(17) . . ? B11 B7 B6 60.05(15) . . ? B2 B7 B6 60.08(14) . . ? C2 B8 B7 106.06(16) . . ? C2 B8 B11 105.73(18) . . ? B7 B8 B11 60.41(16) . . ? C2 B8 B3 59.41(12) . . ? B7 B8 B3 60.14(14) . . ? B11 B8 B3 108.53(18) . . ? C2 B8 B9 58.99(13) . . ? B7 B8 B9 108.13(19) . . ? B11 B8 B9 59.75(16) . . ? B3 B8 B9 108.27(16) . . ? C2 B9 B11 105.91(18) . . ? C2 B9 B8 58.88(14) . . ? B11 B9 B8 60.08(16) . . ? C2 B9 B10 105.91(16) . . ? B11 B9 B10 60.82(16) . . ? B8 B9 B10 108.62(19) . . ? C2 B9 B4 59.42(12) . . ? B11 B9 B4 108.29(19) . . ? B8 B9 B4 108.09(16) . . ? B10 B9 B4 59.52(15) . . ? B4 B10 B9 60.27(14) . . ? B4 B10 B5 60.27(13) . . ? B9 B10 B5 108.23(17) . . ? B4 B10 B6 107.89(17) . . ? B9 B10 B6 107.29(19) . . ? B5 B10 B6 59.91(15) . . ? B4 B10 B11 107.71(19) . . ? B9 B10 B11 59.36(16) . . ? B5 B10 B11 107.82(18) . . ? B6 B10 B11 59.75(16) . . ? B9 B11 B8 60.17(16) . . ? B9 B11 B7 107.91(18) . . ? B8 B11 B7 59.71(15) . . ? B9 B11 B6 107.87(18) . . ? B8 B11 B6 107.77(17) . . ? B7 B11 B6 60.04(15) . . ? B9 B11 B10 59.82(16) . . ? B8 B11 B10 107.90(18) . . ? B7 B11 B10 107.97(17) . . ? B6 B11 B10 60.02(16) . . ? C18 C1 C2 119.61(14) . . ? C18 C1 B2 120.57(14) . . ? C2 C1 B2 109.87(13) . . ? C18 C1 B5 121.27(14) . . ? C2 C1 B5 109.77(14) . . ? B2 C1 B5 62.72(13) . . ? C18 C1 B3 117.71(14) . . ? C2 C1 B3 60.39(12) . . ? B2 C1 B3 62.04(13) . . ? B5 C1 B3 113.13(15) . . ? C18 C1 B4 118.97(14) . . ? C2 C1 B4 60.41(11) . . ? B2 C1 B4 112.84(15) . . ? B5 C1 B4 61.72(13) . . ? B3 C1 B4 111.79(14) . . ? C21 C2 C1 117.75(15) . . ? C21 C2 B8 122.42(17) . . ? C1 C2 B8 110.04(15) . . ? C21 C2 B9 122.21(18) . . ? C1 C2 B9 110.14(16) . . ? B8 C2 B9 62.13(15) . . ? C21 C2 B3 117.63(18) . . ? C1 C2 B3 60.82(11) . . ? B8 C2 B3 61.90(13) . . ? B9 C2 B3 112.84(17) . . ? C21 C2 B4 117.47(18) . . ? C1 C2 B4 60.90(11) . . ? B8 C2 B4 112.73(17) . . ? B9 C2 B4 61.89(13) . . ? B3 C2 B4 112.56(16) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.208 _refine_diff_density_min -0.191 _refine_diff_density_rms 0.041