# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Planas, Jose' _publ_contact_author_email jginerplanas@icmab.es _publ_section_title ; Crystal Engineering of o-Carboranyl Alcohols: Syntheses, Crystal Structures and Thermal Properties ; _journal_year ? _publ_author_name J.Planas # Attachment '- Compound 7.cif' data_2007acc0884 _database_code_depnum_ccdc_archive 'CCDC 756374' #TrackingRef '- Compound 7.cif' _chemical_compound_source 'Jose Giner Planas' _database_code_CSD 7ACC0884 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H20 B10 O2' _chemical_formula_weight 316.39 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/acd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'y+1/4, x+1/4, z+1/4' _cell_length_a 20.7860(2) _cell_length_b 20.7860(2) _cell_length_c 32.3848(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13992.1(4) _cell_formula_units_Z 32 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 47723 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5248 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9624 _exptl_absorpt_correction_T_max 0.9867 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52145 _diffrn_reflns_av_R_equivalents 0.1274 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4013 _reflns_number_gt 2700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.2000P)^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 4013 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1503 _refine_ls_R_factor_gt 0.1101 _refine_ls_wR_factor_ref 0.3408 _refine_ls_wR_factor_gt 0.3113 _refine_ls_goodness_of_fit_ref 1.277 _refine_ls_restrained_S_all 1.277 _refine_ls_shift/su_max 0.000 _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 O1 O 0.53592(10) 0.33594(10) 0.12935(7) 0.0325(6) Uani 1 1 d . . . H1 H 0.5583 0.3023 0.1281 0.049 Uiso 1 1 calc R . . O2 O 0.61814(12) 0.38959(12) 0.03886(8) 0.0443(7) Uani 1 1 d . . . C1 C 0.53176(14) 0.44932(14) 0.11604(11) 0.0309(7) Uani 1 1 d . . . C2 C 0.55884(15) 0.48676(15) 0.15908(11) 0.0319(8) Uani 1 1 d . . . C3 C 0.61173(16) 0.45679(14) 0.18487(11) 0.0345(8) Uani 1 1 d . . . C4 C 0.67575(16) 0.47541(16) 0.17896(12) 0.0402(9) Uani 1 1 d . . . H4 H 0.6861 0.5062 0.1584 0.048 Uiso 1 1 calc R . . C5 C 0.72391(18) 0.44927(18) 0.20289(13) 0.0468(10) Uani 1 1 d . . . H5 H 0.7672 0.4622 0.1985 0.056 Uiso 1 1 calc R . . C6 C 0.71009(17) 0.40468(18) 0.23306(13) 0.0452(9) Uani 1 1 d . . . H6 H 0.7436 0.3868 0.2493 0.054 Uiso 1 1 calc R . . C7 C 0.64728(16) 0.38628(16) 0.23946(10) 0.0346(8) Uani 1 1 d . . . H7 H 0.6376 0.3554 0.2602 0.042 Uiso 1 1 calc R . . C8 C 0.59740(17) 0.41278(16) 0.21558(11) 0.0375(8) Uani 1 1 d . . . H8 H 0.5540 0.4005 0.2205 0.045 Uiso 1 1 calc R . . C9 C 0.56590(14) 0.38544(14) 0.10606(11) 0.0314(7) Uani 1 1 d . . . H909 H 0.6117 0.3890 0.1153 0.038 Uiso 1 1 calc R . . C10 C 0.56554(15) 0.36925(15) 0.06125(11) 0.0353(8) Uani 1 1 d . . . C11 C 0.52543(18) 0.33408(17) 0.03725(12) 0.0417(9) Uani 1 1 d . . . H911 H 0.4859 0.3148 0.0452 0.050 Uiso 1 1 calc R . . C12 C 0.5549(2) 0.33194(19) -0.00242(13) 0.0530(10) Uani 1 1 d . . . H912 H 0.5385 0.3106 -0.0261 0.064 Uiso 1 1 calc R . . C13 C 0.6093(2) 0.36485(19) -0.00042(12) 0.0488(10) Uani 1 1 d . . . H13 H 0.6383 0.3707 -0.0228 0.059 Uiso 1 1 calc R . . B3 B 0.48343(17) 0.45204(17) 0.15957(13) 0.0323(8) Uani 1 1 d . . . H3 H 0.4707 0.4091 0.1788 0.039 Uiso 1 1 calc R . . B4 B 0.45201(17) 0.46340(19) 0.10908(13) 0.0339(8) Uani 1 1 d . . . H4A H 0.4184 0.4277 0.0947 0.041 Uiso 1 1 calc R . . B5 B 0.51028(17) 0.50468(18) 0.07890(13) 0.0340(9) Uani 1 1 d . . . H5A H 0.5145 0.4968 0.0448 0.041 Uiso 1 1 calc R . . B6 B 0.57833(18) 0.51696(16) 0.11048(12) 0.0304(8) Uani 1 1 d . . . H6A H 0.6280 0.5162 0.0971 0.037 Uiso 1 1 calc R . . B7 B 0.49759(19) 0.52817(18) 0.18241(13) 0.0372(9) Uani 1 1 d . . . H7A H 0.4938 0.5359 0.2166 0.045 Uiso 1 1 calc R . . B8 B 0.42822(17) 0.51479(17) 0.15004(12) 0.0316(8) Uani 1 1 d . . . H8A H 0.3780 0.5136 0.1625 0.038 Uiso 1 1 calc R . . B9 B 0.44508(18) 0.54859(18) 0.10123(13) 0.0348(9) Uani 1 1 d . . . H9 H 0.4062 0.5703 0.0818 0.042 Uiso 1 1 calc R . . B10 B 0.52490(17) 0.58128(17) 0.10229(13) 0.0349(9) Uani 1 1 d . . . H10 H 0.5388 0.6244 0.0836 0.042 Uiso 1 1 calc R . . B11 B 0.55707(19) 0.56825(19) 0.15213(13) 0.0361(9) Uani 1 1 d . . . H11 H 0.5927 0.6021 0.1663 0.043 Uiso 1 1 calc R . . B12 B 0.47349(18) 0.58763(17) 0.14660(13) 0.0360(9) Uani 1 1 d . . . H12 H 0.4532 0.6347 0.1572 0.043 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 O1 0.0327(12) 0.0276(11) 0.0372(14) 0.0029(9) 0.0029(9) 0.0014(9) O2 0.0486(15) 0.0464(14) 0.0380(15) 0.0077(11) 0.0090(12) 0.0012(12) C1 0.0269(15) 0.0259(15) 0.040(2) 0.0006(13) 0.0007(13) -0.0028(12) C2 0.0305(15) 0.0304(16) 0.0348(19) 0.0060(13) 0.0003(13) -0.0009(13) C3 0.0399(17) 0.0274(15) 0.0361(19) 0.0000(13) -0.0067(14) -0.0008(13) C4 0.0378(18) 0.0375(17) 0.045(2) 0.0048(15) -0.0068(16) -0.0069(14) C5 0.0399(19) 0.050(2) 0.051(3) 0.0014(18) -0.0092(17) -0.0113(16) C6 0.044(2) 0.045(2) 0.047(2) -0.0044(17) -0.0143(17) 0.0064(16) C7 0.0396(17) 0.0385(17) 0.0257(17) 0.0015(13) -0.0023(13) 0.0049(14) C8 0.0364(17) 0.0410(18) 0.0352(19) 0.0020(14) -0.0001(14) 0.0040(14) C9 0.0264(15) 0.0307(16) 0.0371(19) 0.0015(13) -0.0023(13) -0.0017(12) C10 0.0348(16) 0.0313(16) 0.040(2) 0.0062(14) 0.0023(14) 0.0051(13) C11 0.0434(19) 0.0434(19) 0.038(2) -0.0005(16) -0.0037(16) 0.0043(15) C12 0.071(3) 0.052(2) 0.036(2) -0.0019(17) -0.0027(19) 0.013(2) C13 0.062(2) 0.053(2) 0.031(2) 0.0081(17) 0.0115(18) 0.012(2) B3 0.0271(17) 0.0298(17) 0.040(2) 0.0022(15) 0.0026(15) 0.0002(14) B4 0.0288(17) 0.0384(19) 0.035(2) -0.0017(16) -0.0006(15) -0.0002(15) B5 0.0308(18) 0.041(2) 0.030(2) 0.0056(16) -0.0020(15) 0.0015(15) B6 0.0348(18) 0.0248(16) 0.032(2) 0.0026(14) 0.0010(15) -0.0069(13) B7 0.0380(19) 0.0345(18) 0.039(2) 0.0051(16) 0.0011(16) 0.0071(16) B8 0.0304(17) 0.0292(18) 0.035(2) 0.0003(14) 0.0026(14) 0.0052(14) B9 0.0319(18) 0.0353(19) 0.037(2) 0.0068(16) -0.0026(16) 0.0014(15) B10 0.0319(18) 0.0266(17) 0.046(2) 0.0119(16) -0.0005(16) -0.0013(14) B11 0.039(2) 0.0313(19) 0.038(2) -0.0011(15) -0.0046(16) -0.0008(15) B12 0.038(2) 0.0254(17) 0.044(2) -0.0045(15) -0.0040(16) -0.0001(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 O1 C9 1.420(4) . ? O2 C10 1.378(4) . ? O2 C13 1.384(5) . ? C1 C9 1.540(4) . ? C1 C2 1.693(5) . ? C1 B4 1.698(5) . ? C1 B6 1.716(4) . ? C1 B5 1.723(5) . ? C1 B3 1.732(5) . ? C2 C3 1.515(4) . ? C2 B11 1.709(5) . ? C2 B7 1.713(5) . ? C2 B3 1.726(5) . ? C2 B6 1.742(5) . ? C3 C8 1.384(5) . ? C3 C4 1.399(5) . ? C4 C5 1.378(5) . ? C5 C6 1.377(6) . ? C6 C7 1.376(5) . ? C7 C8 1.406(5) . ? C9 C10 1.490(5) . ? C10 C11 1.354(5) . ? C11 C12 1.424(6) . ? C12 C13 1.323(6) . ? B3 B8 1.765(5) . ? B3 B7 1.771(5) . ? B3 B4 1.777(6) . ? B4 B8 1.773(5) . ? B4 B5 1.777(5) . ? B4 B9 1.795(5) . ? B5 B6 1.764(5) . ? B5 B9 1.787(5) . ? B5 B10 1.789(5) . ? B6 B10 1.758(5) . ? B6 B11 1.775(5) . ? B7 B12 1.767(5) . ? B7 B11 1.784(6) . ? B7 B8 1.804(6) . ? B8 B9 1.765(5) . ? B8 B12 1.786(5) . ? B9 B12 1.779(6) . ? B9 B10 1.793(5) . ? B10 B11 1.768(6) . ? B10 B12 1.794(6) . ? B11 B12 1.792(5) . ? 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 C10 O2 C13 105.3(3) . . ? C9 C1 C2 114.6(3) . . ? C9 C1 B4 124.8(3) . . ? C2 C1 B4 110.8(3) . . ? C9 C1 B6 115.1(2) . . ? C2 C1 B6 61.46(19) . . ? B4 C1 B6 113.3(2) . . ? C9 C1 B5 123.3(3) . . ? C2 C1 B5 110.7(2) . . ? B4 C1 B5 62.6(2) . . ? B6 C1 B5 61.7(2) . . ? C9 C1 B3 117.8(3) . . ? C2 C1 B3 60.5(2) . . ? B4 C1 B3 62.4(2) . . ? B6 C1 B3 112.7(2) . . ? B5 C1 B3 113.3(2) . . ? C3 C2 C1 120.4(3) . . ? C3 C2 B11 119.7(3) . . ? C1 C2 B11 109.9(2) . . ? C3 C2 B7 120.2(3) . . ? C1 C2 B7 110.3(2) . . ? B11 C2 B7 62.9(2) . . ? C3 C2 B3 118.8(3) . . ? C1 C2 B3 60.9(2) . . ? B11 C2 B3 113.3(2) . . ? B7 C2 B3 62.0(2) . . ? C3 C2 B6 118.5(3) . . ? C1 C2 B6 59.94(19) . . ? B11 C2 B6 61.9(2) . . ? B7 C2 B6 113.0(2) . . ? B3 C2 B6 111.7(3) . . ? C8 C3 C4 119.1(3) . . ? C8 C3 C2 120.8(3) . . ? C4 C3 C2 120.1(3) . . ? C5 C4 C3 120.3(3) . . ? C6 C5 C4 120.9(3) . . ? C7 C6 C5 119.4(3) . . ? C6 C7 C8 120.5(3) . . ? C3 C8 C7 119.7(3) . . ? O1 C9 C10 110.6(2) . . ? O1 C9 C1 108.1(3) . . ? C10 C9 C1 113.4(3) . . ? C11 C10 O2 110.6(3) . . ? C11 C10 C9 133.2(3) . . ? O2 C10 C9 116.1(3) . . ? C10 C11 C12 105.6(3) . . ? C13 C12 C11 107.9(4) . . ? C12 C13 O2 110.5(4) . . ? C2 B3 C1 58.62(19) . . ? C2 B3 B8 106.3(2) . . ? C1 B3 B8 105.0(3) . . ? C2 B3 B7 58.6(2) . . ? C1 B3 B7 105.8(3) . . ? B8 B3 B7 61.4(2) . . ? C2 B3 B4 105.7(3) . . ? C1 B3 B4 57.9(2) . . ? B8 B3 B4 60.1(2) . . ? B7 B3 B4 109.1(3) . . ? C1 B4 B8 106.1(3) . . ? C1 B4 B3 59.7(2) . . ? B8 B4 B3 59.6(2) . . ? C1 B4 B5 59.4(2) . . ? B8 B4 B5 108.1(3) . . ? B3 B4 B5 108.6(3) . . ? C1 B4 B9 105.5(3) . . ? B8 B4 B9 59.3(2) . . ? B3 B4 B9 106.9(3) . . ? B5 B4 B9 60.0(2) . . ? C1 B5 B6 58.95(19) . . ? C1 B5 B4 58.0(2) . . ? B6 B5 B4 107.3(3) . . ? C1 B5 B9 104.8(3) . . ? B6 B5 B9 107.4(3) . . ? B4 B5 B9 60.5(2) . . ? C1 B5 B10 104.7(3) . . ? B6 B5 B10 59.3(2) . . ? B4 B5 B10 108.2(3) . . ? B9 B5 B10 60.2(2) . . ? C1 B6 C2 58.60(19) . . ? C1 B6 B10 106.4(2) . . ? C2 B6 B10 105.3(3) . . ? C1 B6 B5 59.3(2) . . ? C2 B6 B5 106.6(3) . . ? B10 B6 B5 61.1(2) . . ? C1 B6 B11 105.8(3) . . ? C2 B6 B11 58.1(2) . . ? B10 B6 B11 60.0(2) . . ? B5 B6 B11 109.1(3) . . ? C2 B7 B12 105.8(3) . . ? C2 B7 B3 59.4(2) . . ? B12 B7 B3 107.7(3) . . ? C2 B7 B11 58.5(2) . . ? B12 B7 B11 60.6(2) . . ? B3 B7 B11 107.6(3) . . ? C2 B7 B8 105.1(3) . . ? B12 B7 B8 60.0(2) . . ? B3 B7 B8 59.1(2) . . ? B11 B7 B8 107.8(3) . . ? B3 B8 B9 108.8(3) . . ? B3 B8 B4 60.3(2) . . ? B9 B8 B4 61.0(2) . . ? B3 B8 B12 107.1(2) . . ? B9 B8 B12 60.1(2) . . ? B4 B8 B12 108.5(3) . . ? B3 B8 B7 59.5(2) . . ? B9 B8 B7 107.5(3) . . ? B4 B8 B7 107.7(3) . . ? B12 B8 B7 59.0(2) . . ? B8 B9 B12 60.5(2) . . ? B8 B9 B5 108.1(3) . . ? B12 B9 B5 108.4(3) . . ? B8 B9 B10 108.5(3) . . ? B12 B9 B10 60.3(2) . . ? B5 B9 B10 60.0(2) . . ? B8 B9 B4 59.8(2) . . ? B12 B9 B4 107.8(3) . . ? B5 B9 B4 59.5(2) . . ? B10 B9 B4 107.3(3) . . ? B6 B10 B11 60.5(2) . . ? B6 B10 B5 59.6(2) . . ? B11 B10 B5 108.3(3) . . ? B6 B10 B9 107.4(2) . . ? B11 B10 B9 108.0(3) . . ? B5 B10 B9 59.8(2) . . ? B6 B10 B12 108.2(3) . . ? B11 B10 B12 60.4(2) . . ? B5 B10 B12 107.6(2) . . ? B9 B10 B12 59.5(2) . . ? C2 B11 B10 106.3(3) . . ? C2 B11 B6 60.0(2) . . ? B10 B11 B6 59.5(2) . . ? C2 B11 B7 58.7(2) . . ? B10 B11 B7 108.1(3) . . ? B6 B11 B7 108.0(3) . . ? C2 B11 B12 104.9(3) . . ? B10 B11 B12 60.5(2) . . ? B6 B11 B12 107.5(3) . . ? B7 B11 B12 59.2(2) . . ? B7 B12 B9 108.5(3) . . ? B7 B12 B8 61.0(2) . . ? B9 B12 B8 59.3(2) . . ? B7 B12 B11 60.2(2) . . ? B9 B12 B11 107.6(3) . . ? B8 B12 B11 108.3(3) . . ? B7 B12 B10 107.7(3) . . ? B9 B12 B10 60.2(2) . . ? B8 B12 B10 107.5(2) . . ? B11 B12 B10 59.1(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.257 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.095 # Attachment '- Compound 2.cif' data_2008acc0737 _database_code_depnum_ccdc_archive 'CCDC 756375' #TrackingRef '- Compound 2.cif' _chemical_compound_source 'Jose Giner Planas' _database_code_CSD 8ACC0737 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 B10 O' _chemical_formula_weight 364.47 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' _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 19.1234(8) _cell_length_b 9.0888(4) _cell_length_c 23.1603(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.767(2) _cell_angle_gamma 90.00 _cell_volume 4005.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7801 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 26.02 _exptl_crystal_description Fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9773 _exptl_absorpt_correction_T_max 0.9936 _exptl_absorpt_process_details ; SADABS V2.10 (Sheldrick, G.M., 2003) ; _exptl_special_details ; ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26061 _diffrn_reflns_av_R_equivalents 0.1308 _diffrn_reflns_av_sigmaI/netI 0.1479 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7056 _reflns_number_gt 3955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0699P)^2^+3.4634P] 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 7056 _refine_ls_number_parameters 537 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1555 _refine_ls_R_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.2359 _refine_ls_wR_factor_gt 0.1971 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.017 _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 O1A O 0.2210(2) 0.0701(4) 0.09439(15) 0.0358(9) Uani 0.722(4) 1 d P A 1 H1A H 0.2039 -0.0048 0.1088 0.054 Uiso 0.722(4) 1 calc PR A 1 C4A C 0.2939(2) 0.0707(4) 0.10812(16) 0.0329(9) Uani 0.722(4) 1 d P A 1 H4A H 0.3110 -0.0277 0.0962 0.039 Uiso 0.722(4) 1 calc PR A 1 O1B O 0.2953(5) -0.0673(10) 0.0839(4) 0.0358(9) Uani 0.278(4) 1 d P A 2 H1B H 0.3284 -0.0722 0.0627 0.054 Uiso 0.278(4) 1 calc PR A 2 C4B C 0.2939(2) 0.0707(4) 0.10812(16) 0.0329(9) Uani 0.278(4) 1 d P A 2 H4B H 0.2429 0.0977 0.1047 0.039 Uiso 0.278(4) 1 calc PR A 2 C1 C 0.3277(2) 0.1853(4) 0.07029(14) 0.0288(9) Uani 1 1 d . . . C2 C 0.3062(2) 0.1760(4) -0.00160(15) 0.0318(9) Uani 1 1 d . A . C3 C 0.2541(2) 0.0610(5) -0.02681(17) 0.0434(11) Uani 1 1 d . . . H3A H 0.2690 -0.0366 -0.0123 0.065 Uiso 1 1 calc R A . H3B H 0.2522 0.0622 -0.0692 0.065 Uiso 1 1 calc R . . H3C H 0.2074 0.0831 -0.0151 0.065 Uiso 1 1 calc R . . C5 C 0.3182(2) 0.0868(4) 0.17349(15) 0.0295(9) Uani 1 1 d . . . C6 C 0.3766(2) 0.0046(4) 0.19815(15) 0.0313(9) Uani 1 1 d . A . C7 C 0.4185(2) -0.0920(5) 0.16605(17) 0.0386(10) Uani 1 1 d . . . H7 H 0.4066 -0.1034 0.1255 0.046 Uiso 1 1 calc R A . C8 C 0.4738(2) -0.1662(5) 0.19167(17) 0.0421(11) Uani 1 1 d . A . H8 H 0.4998 -0.2287 0.1688 0.051 Uiso 1 1 calc R . . C9 C 0.4943(2) -0.1536(5) 0.25179(18) 0.0425(11) Uani 1 1 d . . . H9 H 0.5336 -0.2070 0.2692 0.051 Uiso 1 1 calc R A . C10 C 0.4571(2) -0.0643(5) 0.28429(17) 0.0388(10) Uani 1 1 d . A . H10 H 0.4711 -0.0552 0.3247 0.047 Uiso 1 1 calc R . . C11 C 0.3977(2) 0.0159(4) 0.25943(16) 0.0327(9) Uani 1 1 d . . . C12 C 0.3604(2) 0.1080(4) 0.29322(16) 0.0348(10) Uani 1 1 d . A . H12 H 0.3742 0.1139 0.3337 0.042 Uiso 1 1 calc R . . C13 C 0.3035(2) 0.1919(4) 0.26983(15) 0.0313(9) Uani 1 1 d . . . C14 C 0.2671(2) 0.2869(4) 0.30578(16) 0.0378(10) Uani 1 1 d . A . H14 H 0.2823 0.2941 0.3460 0.045 Uiso 1 1 calc R . . C15 C 0.2110(2) 0.3670(5) 0.28311(17) 0.0395(10) Uani 1 1 d . . . H15 H 0.1870 0.4286 0.3077 0.047 Uiso 1 1 calc R A . C16 C 0.1884(2) 0.3597(4) 0.22372(16) 0.0355(10) Uani 1 1 d . A . H16 H 0.1494 0.4174 0.2084 0.043 Uiso 1 1 calc R . . C17 C 0.2218(2) 0.2707(4) 0.18766(16) 0.0326(9) Uani 1 1 d . . . H17 H 0.2054 0.2677 0.1476 0.039 Uiso 1 1 calc R A . C18 C 0.2809(2) 0.1814(4) 0.20867(15) 0.0304(9) Uani 1 1 d . A . B3 B 0.2738(3) 0.3207(5) 0.03676(18) 0.0333(11) Uani 1 1 d . A . H3 H 0.2171 0.3361 0.0437 0.040 Uiso 1 1 calc R . . B4 B 0.3437(2) 0.3641(5) 0.09098(18) 0.0302(10) Uani 1 1 d . A . H4 H 0.3331 0.4090 0.1343 0.036 Uiso 1 1 calc R . . B5 B 0.4140(3) 0.2401(5) 0.08432(19) 0.0340(11) Uani 1 1 d . A . H5 H 0.4495 0.2033 0.1230 0.041 Uiso 1 1 calc R . . B6 B 0.3889(2) 0.1188(5) 0.02571(17) 0.0316(10) Uani 1 1 d . A . H6 H 0.4072 0.0018 0.0256 0.038 Uiso 1 1 calc R . . B7 B 0.3059(3) 0.3469(5) -0.03147(18) 0.0359(11) Uani 1 1 d . . . H7A H 0.2695 0.3808 -0.0701 0.043 Uiso 1 1 calc R A . B8 B 0.3308(3) 0.4705(5) 0.02588(18) 0.0369(11) Uani 1 1 d . A . H8A H 0.3118 0.5870 0.0256 0.044 Uiso 1 1 calc R . . B9 B 0.4170(3) 0.4220(5) 0.05569(18) 0.0358(11) Uani 1 1 d . . . H9A H 0.4547 0.5069 0.0753 0.043 Uiso 1 1 calc R A . B10 B 0.4453(3) 0.2677(5) 0.01542(18) 0.0353(11) Uani 1 1 d . A . H10A H 0.5018 0.2504 0.0085 0.042 Uiso 1 1 calc R . . B11 B 0.3759(3) 0.2234(5) -0.03865(18) 0.0333(11) Uani 1 1 d . A . H11 H 0.3858 0.1760 -0.0817 0.040 Uiso 1 1 calc R . . B12 B 0.3940(3) 0.4102(5) -0.02078(18) 0.0360(11) Uani 1 1 d . A . H12A H 0.4168 0.4868 -0.0518 0.043 Uiso 1 1 calc R . . O1A' O 0.1361(2) 1.0394(4) 0.29081(15) 0.0348(9) Uani 0.706(4) 1 d P B 3 H1A' H 0.0924 1.0281 0.2847 0.052 Uiso 0.706(4) 1 calc PR B 3 C4A' C 0.1651(2) 0.9207(4) 0.32088(17) 0.0377(10) Uani 0.706(4) 1 d P B 3 H4A' H 0.1972 0.9643 0.3531 0.045 Uiso 0.706(4) 1 calc PR B 3 O1B' O 0.1887(5) 1.0248(10) 0.3511(4) 0.0348(9) Uani 0.294(4) 1 d P B 4 H1B' H 0.2243 1.0591 0.3373 0.052 Uiso 0.294(4) 1 calc PR B 4 C4B' C 0.1651(2) 0.9207(4) 0.32088(17) 0.0377(10) Uani 0.294(4) 1 d P B 4 H4B' H 0.1356 0.9715 0.2888 0.045 Uiso 0.294(4) 1 calc PR B 4 C1' C 0.1093(2) 0.8343(4) 0.35178(15) 0.0308(9) Uani 1 1 d . . . C2' C 0.0572(2) 0.9296(4) 0.39166(17) 0.0398(11) Uani 1 1 d . B . C3' C 0.0649(3) 1.0965(5) 0.3963(2) 0.0530(13) Uani 1 1 d . . . H3'1 H 0.1145 1.1218 0.4062 0.079 Uiso 1 1 calc R B . H3'2 H 0.0372 1.1331 0.4267 0.079 Uiso 1 1 calc R . . H3'3 H 0.0479 1.1417 0.3591 0.079 Uiso 1 1 calc R . . C5' C 0.2128(2) 0.8224(4) 0.28760(16) 0.0316(9) Uani 1 1 d . . . C6' C 0.2757(2) 0.7651(4) 0.31718(15) 0.0309(9) Uani 1 1 d . B . C7' C 0.2976(2) 0.7885(5) 0.37802(16) 0.0381(10) Uani 1 1 d . . . H7' H 0.2703 0.8508 0.3999 0.046 Uiso 1 1 calc R B . C8' C 0.3557(2) 0.7243(5) 0.40469(17) 0.0384(10) Uani 1 1 d . B . H8' H 0.3681 0.7413 0.4449 0.046 Uiso 1 1 calc R . . C9' C 0.3987(2) 0.6319(5) 0.37387(17) 0.0387(10) Uani 1 1 d . . . H9' H 0.4388 0.5855 0.3935 0.046 Uiso 1 1 calc R B . C10' C 0.3824(2) 0.6103(4) 0.31654(17) 0.0369(10) Uani 1 1 d . B . H10' H 0.4120 0.5503 0.2958 0.044 Uiso 1 1 calc R . . C11' C 0.3211(2) 0.6762(4) 0.28627(16) 0.0311(9) Uani 1 1 d . . . C12' C 0.3052(2) 0.6529(4) 0.22752(16) 0.0339(9) Uani 1 1 d . B . H12' H 0.3368 0.5975 0.2070 0.041 Uiso 1 1 calc R . . C13' C 0.2440(2) 0.7085(4) 0.19744(15) 0.0330(9) Uani 1 1 d . . . C14' C 0.2280(2) 0.6782(5) 0.13660(16) 0.0389(10) Uani 1 1 d . B . H14' H 0.2607 0.6245 0.1166 0.047 Uiso 1 1 calc R . . C15' C 0.1672(3) 0.7247(5) 0.10721(17) 0.0430(11) Uani 1 1 d . . . H15' H 0.1573 0.7035 0.0671 0.052 Uiso 1 1 calc R B . C16' C 0.1185(2) 0.8052(5) 0.13689(17) 0.0400(10) Uani 1 1 d . B . H16' H 0.0758 0.8375 0.1163 0.048 Uiso 1 1 calc R . . C17' C 0.1315(2) 0.8373(5) 0.19417(16) 0.0381(10) Uani 1 1 d . . . H17' H 0.0975 0.8914 0.2126 0.046 Uiso 1 1 calc R B . C18' C 0.1952(2) 0.7919(4) 0.22784(15) 0.0305(9) Uani 1 1 d . B . B3' B 0.0211(3) 0.8554(6) 0.3264(2) 0.0403(12) Uani 1 1 d . B . H3' H 0.0017 0.9214 0.2872 0.048 Uiso 1 1 calc R . . B4' B 0.0649(3) 0.6841(5) 0.3209(2) 0.0362(11) Uani 1 1 d . B . H4' H 0.0742 0.6362 0.2778 0.043 Uiso 1 1 calc R . . B5' B 0.1277(3) 0.6642(5) 0.38234(19) 0.0340(11) Uani 1 1 d . B . H5' H 0.1783 0.6038 0.3796 0.041 Uiso 1 1 calc R . . B6' B 0.1230(3) 0.8237(5) 0.42657(18) 0.0374(12) Uani 1 1 d . B . H6' H 0.1702 0.8696 0.4530 0.045 Uiso 1 1 calc R . . B7' B -0.0237(3) 0.8507(6) 0.3895(2) 0.0439(13) Uani 1 1 d . . . H7'1 H -0.0734 0.9146 0.3920 0.053 Uiso 1 1 calc R B . B8' B -0.0199(3) 0.6924(6) 0.3455(2) 0.0448(13) Uani 1 1 d . B . H8'1 H -0.0675 0.6490 0.3187 0.054 Uiso 1 1 calc R . . B9' B 0.0457(3) 0.5730(6) 0.3798(2) 0.0401(12) Uani 1 1 d . . . H9'1 H 0.0418 0.4504 0.3758 0.048 Uiso 1 1 calc R B . B10' B 0.0817(3) 0.6583(6) 0.4452(2) 0.0414(12) Uani 1 1 d . B . H10B H 0.1015 0.5927 0.4843 0.050 Uiso 1 1 calc R . . B11' B 0.0381(3) 0.8300(6) 0.4508(2) 0.0448(13) Uani 1 1 d . B . H11' H 0.0292 0.8792 0.4937 0.054 Uiso 1 1 calc R . . B12' B -0.0105(3) 0.6755(5) 0.4222(2) 0.0432(13) Uani 1 1 d . B . H12B H -0.0516 0.6212 0.4460 0.052 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 O1A 0.039(2) 0.034(2) 0.0345(19) 0.0013(16) 0.0021(16) -0.0030(17) C4A 0.033(2) 0.033(2) 0.032(2) -0.0010(17) 0.0020(17) -0.0013(19) O1B 0.039(2) 0.034(2) 0.0345(19) 0.0013(16) 0.0021(16) -0.0030(17) C4B 0.033(2) 0.033(2) 0.032(2) -0.0010(17) 0.0020(17) -0.0013(19) C1 0.034(2) 0.028(2) 0.0236(18) -0.0025(15) -0.0003(16) -0.0004(18) C2 0.034(2) 0.036(2) 0.0249(18) -0.0035(16) -0.0012(16) 0.0007(19) C3 0.045(3) 0.051(3) 0.034(2) -0.007(2) -0.0002(19) -0.011(2) C5 0.031(2) 0.028(2) 0.0297(19) 0.0006(16) 0.0036(16) -0.0068(18) C6 0.034(2) 0.028(2) 0.032(2) 0.0038(17) -0.0005(17) -0.0059(18) C7 0.046(3) 0.036(2) 0.034(2) -0.0002(18) 0.0069(19) -0.003(2) C8 0.043(3) 0.039(3) 0.044(2) 0.007(2) 0.005(2) 0.004(2) C9 0.039(3) 0.039(3) 0.048(2) 0.010(2) 0.000(2) 0.004(2) C10 0.042(3) 0.039(2) 0.034(2) 0.0087(18) -0.0046(19) -0.005(2) C11 0.033(2) 0.030(2) 0.034(2) 0.0072(17) 0.0006(17) -0.0052(19) C12 0.040(3) 0.037(2) 0.0261(19) 0.0026(17) -0.0007(17) -0.010(2) C13 0.036(2) 0.030(2) 0.0273(19) 0.0022(16) -0.0008(17) -0.0086(19) C14 0.054(3) 0.036(2) 0.0248(19) 0.0004(17) 0.0095(19) -0.008(2) C15 0.043(3) 0.040(2) 0.037(2) -0.0052(19) 0.0087(19) -0.005(2) C16 0.033(2) 0.036(2) 0.037(2) 0.0002(18) 0.0020(18) -0.0006(19) C17 0.032(2) 0.036(2) 0.0295(19) 0.0035(17) 0.0010(17) -0.0054(19) C18 0.032(2) 0.029(2) 0.0303(19) 0.0001(16) 0.0036(17) -0.0090(18) B3 0.036(3) 0.033(3) 0.031(2) 0.0029(19) 0.005(2) 0.010(2) B4 0.033(3) 0.029(2) 0.028(2) -0.0013(18) 0.0028(19) -0.005(2) B5 0.032(3) 0.039(3) 0.032(2) 0.000(2) 0.0037(19) -0.002(2) B6 0.030(3) 0.036(3) 0.029(2) -0.0051(19) 0.0020(18) 0.001(2) B7 0.043(3) 0.040(3) 0.025(2) -0.0006(19) 0.0047(19) 0.006(2) B8 0.044(3) 0.037(3) 0.031(2) 0.003(2) 0.008(2) 0.000(2) B9 0.041(3) 0.036(3) 0.030(2) 0.004(2) 0.006(2) -0.004(2) B10 0.030(3) 0.042(3) 0.034(2) 0.002(2) 0.005(2) -0.002(2) B11 0.031(3) 0.039(3) 0.030(2) 0.002(2) 0.0019(19) 0.006(2) B12 0.040(3) 0.036(3) 0.031(2) 0.001(2) 0.001(2) 0.001(2) O1A' 0.034(2) 0.031(2) 0.0387(19) 0.0015(16) 0.0015(16) 0.0046(17) C4A' 0.047(3) 0.024(2) 0.045(2) 0.0023(18) 0.018(2) 0.004(2) O1B' 0.034(2) 0.031(2) 0.0387(19) 0.0015(16) 0.0015(16) 0.0046(17) C4B' 0.047(3) 0.024(2) 0.045(2) 0.0023(18) 0.018(2) 0.004(2) C1' 0.031(2) 0.028(2) 0.033(2) -0.0010(16) 0.0029(17) 0.0040(18) C2' 0.050(3) 0.030(2) 0.043(2) 0.0037(19) 0.019(2) 0.008(2) C3' 0.070(4) 0.033(2) 0.060(3) 0.001(2) 0.031(3) 0.009(2) C5' 0.034(2) 0.027(2) 0.035(2) -0.0002(17) 0.0097(17) -0.0023(18) C6' 0.035(2) 0.025(2) 0.033(2) -0.0010(16) 0.0057(17) -0.0047(18) C7' 0.041(3) 0.038(2) 0.035(2) -0.0042(18) 0.0073(19) -0.008(2) C8' 0.037(3) 0.041(2) 0.037(2) 0.0027(19) 0.0016(19) -0.009(2) C9' 0.036(3) 0.035(2) 0.045(2) 0.0069(19) 0.0009(19) -0.002(2) C10' 0.030(2) 0.033(2) 0.047(2) -0.0001(19) 0.0027(19) -0.0042(19) C11' 0.033(2) 0.024(2) 0.037(2) -0.0023(16) 0.0054(17) -0.0070(18) C12' 0.034(2) 0.029(2) 0.040(2) 0.0000(17) 0.0092(18) 0.0014(19) C13' 0.043(3) 0.026(2) 0.0311(19) 0.0005(16) 0.0098(18) -0.0008(19) C14' 0.047(3) 0.036(2) 0.036(2) -0.0030(18) 0.010(2) 0.004(2) C15' 0.058(3) 0.039(2) 0.032(2) 0.0018(18) 0.000(2) 0.001(2) C16' 0.041(3) 0.041(3) 0.037(2) 0.0050(19) 0.0025(19) 0.002(2) C17' 0.035(3) 0.037(2) 0.042(2) 0.0008(19) 0.0071(19) 0.003(2) C18' 0.033(2) 0.027(2) 0.033(2) 0.0061(16) 0.0093(17) -0.0007(18) B3' 0.035(3) 0.045(3) 0.043(3) 0.003(2) 0.009(2) 0.006(2) B4' 0.031(3) 0.036(3) 0.041(2) -0.003(2) 0.001(2) -0.004(2) B5' 0.043(3) 0.023(2) 0.036(2) -0.0032(19) 0.005(2) 0.003(2) B6' 0.044(3) 0.041(3) 0.028(2) 0.001(2) 0.010(2) 0.004(2) B7' 0.041(3) 0.041(3) 0.052(3) 0.007(2) 0.015(2) 0.012(3) B8' 0.034(3) 0.043(3) 0.058(3) 0.005(2) 0.007(2) 0.003(2) B9' 0.037(3) 0.031(3) 0.053(3) 0.001(2) 0.010(2) 0.002(2) B10' 0.042(3) 0.040(3) 0.043(3) 0.007(2) 0.010(2) 0.004(2) B11' 0.045(3) 0.045(3) 0.047(3) 0.007(2) 0.020(2) 0.005(3) B12' 0.040(3) 0.035(3) 0.056(3) 0.007(2) 0.015(2) 0.006(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 O1A C4A 1.397(5) . ? C4A C1 1.545(5) . ? C4A C5 1.546(5) . ? C1 C2 1.676(5) . ? C1 B4 1.713(6) . ? C1 B5 1.722(6) . ? C1 B3 1.738(6) . ? C1 B6 1.745(6) . ? C2 C3 1.521(6) . ? C2 B7 1.700(6) . ? C2 B11 1.710(6) . ? C2 B6 1.723(6) . ? C2 B3 1.736(6) . ? C5 C6 1.415(6) . ? C5 C18 1.424(5) . ? C6 C11 1.440(5) . ? C6 C7 1.445(6) . ? C7 C8 1.341(6) . ? C8 C9 1.413(6) . ? C9 C10 1.355(6) . ? C10 C11 1.422(6) . ? C11 C12 1.391(6) . ? C12 C13 1.393(6) . ? C13 C14 1.428(6) . ? C13 C18 1.442(5) . ? C14 C15 1.357(6) . ? C15 C16 1.402(5) . ? C16 C17 1.366(5) . ? C17 C18 1.437(6) . ? B3 B7 1.768(6) . ? B3 B8 1.778(7) . ? B3 B4 1.784(6) . ? B4 B9 1.772(6) . ? B4 B5 1.772(7) . ? B4 B8 1.787(6) . ? B5 B6 1.776(6) . ? B5 B10 1.777(6) . ? B5 B9 1.785(7) . ? B6 B10 1.761(7) . ? B6 B11 1.764(6) . ? B7 B11 1.767(7) . ? B7 B8 1.768(6) . ? B7 B12 1.774(7) . ? B8 B9 1.777(7) . ? B8 B12 1.786(7) . ? B9 B12 1.785(6) . ? B9 B10 1.797(7) . ? B10 B11 1.777(6) . ? B10 B12 1.782(7) . ? B11 B12 1.773(7) . ? O1A' C4A' 1.370(5) . ? C4A' C5' 1.538(5) . ? C4A' C1' 1.555(6) . ? C1' C2' 1.667(5) . ? C1' B5' 1.722(6) . ? C1' B4' 1.725(6) . ? C1' B6' 1.728(5) . ? C1' B3' 1.740(6) . ? C2' C3' 1.527(6) . ? C2' B7' 1.702(7) . ? C2' B11' 1.711(6) . ? C2' B6' 1.719(6) . ? C2' B3' 1.734(7) . ? C5' C18' 1.418(5) . ? C5' C6' 1.423(6) . ? C6' C11' 1.430(5) . ? C6' C7' 1.445(5) . ? C7' C8' 1.349(6) . ? C8' C9' 1.418(6) . ? C9' C10' 1.347(5) . ? C10' C11' 1.435(6) . ? C11' C12' 1.381(5) . ? C12' C13' 1.394(6) . ? C13' C14' 1.438(5) . ? C13' C18' 1.440(5) . ? C14' C15' 1.355(6) . ? C15' C16' 1.416(6) . ? C16' C17' 1.357(5) . ? C17' C18' 1.439(6) . ? B3' B8' 1.754(7) . ? B3' B7' 1.768(7) . ? B3' B4' 1.778(7) . ? B4' B9' 1.765(7) . ? B4' B8' 1.773(7) . ? B4' B5' 1.776(7) . ? B5' B9' 1.768(7) . ? B5' B10' 1.775(7) . ? B5' B6' 1.782(6) . ? B6' B11' 1.771(7) . ? B6' B10' 1.771(7) . ? B7' B11' 1.764(8) . ? B7' B8' 1.769(7) . ? B7' B12' 1.770(7) . ? B8' B12' 1.774(7) . ? B8' B9' 1.784(7) . ? B9' B10' 1.776(7) . ? B9' B12' 1.788(7) . ? B10' B11' 1.780(7) . ? B10' B12' 1.795(7) . ? B11' B12' 1.774(8) . ? 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 O1A C4A C1 109.8(3) . . ? O1A C4A C5 114.7(3) . . ? C1 C4A C5 113.0(3) . . ? C4A C1 C2 117.0(3) . . ? C4A C1 B4 123.7(3) . . ? C2 C1 B4 110.2(3) . . ? C4A C1 B5 122.4(3) . . ? C2 C1 B5 109.7(3) . . ? B4 C1 B5 62.1(3) . . ? C4A C1 B3 117.9(3) . . ? C2 C1 B3 61.1(2) . . ? B4 C1 B3 62.3(2) . . ? B5 C1 B3 113.2(3) . . ? C4A C1 B6 116.5(3) . . ? C2 C1 B6 60.4(2) . . ? B4 C1 B6 112.5(3) . . ? B5 C1 B6 61.6(2) . . ? B3 C1 B6 112.6(3) . . ? C3 C2 C1 120.1(3) . . ? C3 C2 B7 119.8(3) . . ? C1 C2 B7 110.4(3) . . ? C3 C2 B11 119.6(3) . . ? C1 C2 B11 111.1(3) . . ? B7 C2 B11 62.4(3) . . ? C3 C2 B6 118.4(3) . . ? C1 C2 B6 61.7(2) . . ? B7 C2 B6 113.0(3) . . ? B11 C2 B6 61.9(2) . . ? C3 C2 B3 117.6(4) . . ? C1 C2 B3 61.2(2) . . ? B7 C2 B3 61.9(2) . . ? B11 C2 B3 113.7(3) . . ? B6 C2 B3 113.7(3) . . ? C6 C5 C18 120.5(3) . . ? C6 C5 C4A 119.5(3) . . ? C18 C5 C4A 120.0(3) . . ? C5 C6 C11 119.5(4) . . ? C5 C6 C7 124.7(3) . . ? C11 C6 C7 115.8(4) . . ? C8 C7 C6 122.1(4) . . ? C7 C8 C9 121.6(4) . . ? C10 C9 C8 119.2(4) . . ? C9 C10 C11 121.6(4) . . ? C12 C11 C10 121.0(4) . . ? C12 C11 C6 119.2(4) . . ? C10 C11 C6 119.8(4) . . ? C11 C12 C13 122.4(3) . . ? C12 C13 C14 120.8(3) . . ? C12 C13 C18 119.4(4) . . ? C14 C13 C18 119.8(4) . . ? C15 C14 C13 120.7(4) . . ? C14 C15 C16 120.6(4) . . ? C17 C16 C15 120.7(4) . . ? C16 C17 C18 121.8(4) . . ? C5 C18 C17 124.7(3) . . ? C5 C18 C13 119.0(4) . . ? C17 C18 C13 116.3(4) . . ? C2 B3 C1 57.7(2) . . ? C2 B3 B7 58.0(2) . . ? C1 B3 B7 104.5(3) . . ? C2 B3 B8 104.6(3) . . ? C1 B3 B8 105.1(3) . . ? B7 B3 B8 59.8(3) . . ? C2 B3 B4 104.3(3) . . ? C1 B3 B4 58.2(2) . . ? B7 B3 B4 107.2(3) . . ? B8 B3 B4 60.2(3) . . ? C1 B4 B9 106.3(3) . . ? C1 B4 B5 59.2(2) . . ? B9 B4 B5 60.5(3) . . ? C1 B4 B3 59.6(2) . . ? B9 B4 B3 108.2(3) . . ? B5 B4 B3 108.6(3) . . ? C1 B4 B8 105.8(3) . . ? B9 B4 B8 59.9(3) . . ? B5 B4 B8 108.2(3) . . ? B3 B4 B8 59.7(3) . . ? C1 B5 B4 58.7(2) . . ? C1 B5 B6 59.8(2) . . ? B4 B5 B6 108.2(3) . . ? C1 B5 B10 105.9(3) . . ? B4 B5 B10 108.3(3) . . ? B6 B5 B10 59.4(3) . . ? C1 B5 B9 105.3(3) . . ? B4 B5 B9 59.8(3) . . ? B6 B5 B9 107.9(3) . . ? B10 B5 B9 60.6(3) . . ? C2 B6 C1 57.8(2) . . ? C2 B6 B10 105.7(3) . . ? C1 B6 B10 105.7(3) . . ? C2 B6 B11 58.7(2) . . ? C1 B6 B11 105.5(3) . . ? B10 B6 B11 60.5(3) . . ? C2 B6 B5 105.1(3) . . ? C1 B6 B5 58.6(2) . . ? B10 B6 B5 60.3(3) . . ? B11 B6 B5 108.4(3) . . ? C2 B7 B11 59.1(3) . . ? C2 B7 B8 106.6(3) . . ? B11 B7 B8 109.0(3) . . ? C2 B7 B3 60.1(2) . . ? B11 B7 B3 109.5(3) . . ? B8 B7 B3 60.4(3) . . ? C2 B7 B12 106.0(3) . . ? B11 B7 B12 60.1(3) . . ? B8 B7 B12 60.6(3) . . ? B3 B7 B12 109.2(3) . . ? B7 B8 B9 107.7(4) . . ? B7 B8 B3 59.8(3) . . ? B9 B8 B3 108.3(3) . . ? B7 B8 B12 59.9(3) . . ? B9 B8 B12 60.1(3) . . ? B3 B8 B12 108.2(3) . . ? B7 B8 B4 107.1(3) . . ? B9 B8 B4 59.6(3) . . ? B3 B8 B4 60.0(2) . . ? B12 B8 B4 107.5(3) . . ? B4 B9 B8 60.5(3) . . ? B4 B9 B12 108.2(3) . . ? B8 B9 B12 60.2(3) . . ? B4 B9 B5 59.8(3) . . ? B8 B9 B5 108.1(3) . . ? B12 B9 B5 107.4(3) . . ? B4 B9 B10 107.5(3) . . ? B8 B9 B10 107.9(3) . . ? B12 B9 B10 59.7(3) . . ? B5 B9 B10 59.5(3) . . ? B6 B10 B11 59.8(3) . . ? B6 B10 B5 60.3(2) . . ? B11 B10 B5 107.8(3) . . ? B6 B10 B12 107.9(3) . . ? B11 B10 B12 59.8(3) . . ? B5 B10 B12 107.8(3) . . ? B6 B10 B9 108.0(3) . . ? B11 B10 B9 107.5(3) . . ? B5 B10 B9 59.9(3) . . ? B12 B10 B9 59.8(3) . . ? C2 B11 B6 59.4(2) . . ? C2 B11 B7 58.5(3) . . ? B6 B11 B7 107.9(3) . . ? C2 B11 B12 105.5(3) . . ? B6 B11 B12 108.1(3) . . ? B7 B11 B12 60.1(3) . . ? C2 B11 B10 105.5(3) . . ? B6 B11 B10 59.6(2) . . ? B7 B11 B10 108.0(3) . . ? B12 B11 B10 60.3(3) . . ? B11 B12 B7 59.7(3) . . ? B11 B12 B10 60.0(3) . . ? B7 B12 B10 107.4(3) . . ? B11 B12 B9 108.2(3) . . ? B7 B12 B9 107.1(3) . . ? B10 B12 B9 60.5(3) . . ? B11 B12 B8 107.8(3) . . ? B7 B12 B8 59.6(3) . . ? B10 B12 B8 108.2(3) . . ? B9 B12 B8 59.7(3) . . ? O1A' C4A' C5' 115.6(3) . . ? O1A' C4A' C1' 111.8(4) . . ? C5' C4A' C1' 113.9(3) . . ? C4A' C1' C2' 117.9(3) . . ? C4A' C1' B5' 121.5(3) . . ? C2' C1' B5' 110.3(3) . . ? C4A' C1' B4' 122.7(3) . . ? C2' C1' B4' 110.1(3) . . ? B5' C1' B4' 62.0(3) . . ? C4A' C1' B6' 116.6(3) . . ? C2' C1' B6' 60.8(2) . . ? B5' C1' B6' 62.2(2) . . ? B4' C1' B6' 112.9(3) . . ? C4A' C1' B3' 118.3(3) . . ? C2' C1' B3' 61.1(3) . . ? B5' C1' B3' 112.8(3) . . ? B4' C1' B3' 61.8(3) . . ? B6' C1' B3' 112.9(3) . . ? C3' C2' C1' 119.8(3) . . ? C3' C2' B7' 120.0(4) . . ? C1' C2' B7' 110.9(3) . . ? C3' C2' B11' 119.7(4) . . ? C1' C2' B11' 110.9(3) . . ? B7' C2' B11' 62.2(3) . . ? C3' C2' B6' 117.6(4) . . ? C1' C2' B6' 61.4(2) . . ? B7' C2' B6' 113.5(3) . . ? B11' C2' B6' 62.1(3) . . ? C3' C2' B3' 118.3(4) . . ? C1' C2' B3' 61.5(2) . . ? B7' C2' B3' 61.9(3) . . ? B11' C2' B3' 113.2(4) . . ? B6' C2' B3' 113.6(3) . . ? C18' C5' C6' 120.3(4) . . ? C18' C5' C4A' 120.6(4) . . ? C6' C5' C4A' 119.1(3) . . ? C5' C6' C11' 119.5(3) . . ? C5' C6' C7' 124.3(4) . . ? C11' C6' C7' 116.1(4) . . ? C8' C7' C6' 121.9(4) . . ? C7' C8' C9' 121.2(4) . . ? C10' C9' C8' 119.6(4) . . ? C9' C10' C11' 121.2(4) . . ? C12' C11' C6' 119.7(4) . . ? C12' C11' C10' 120.4(4) . . ? C6' C11' C10' 119.9(3) . . ? C11' C12' C13' 121.9(4) . . ? C12' C13' C14' 120.4(4) . . ? C12' C13' C18' 119.9(3) . . ? C14' C13' C18' 119.7(4) . . ? C15' C14' C13' 121.3(4) . . ? C14' C15' C16' 119.4(4) . . ? C17' C16' C15' 121.4(4) . . ? C16' C17' C18' 122.0(4) . . ? C5' C18' C17' 125.2(4) . . ? C5' C18' C13' 118.6(4) . . ? C17' C18' C13' 116.2(3) . . ? C2' B3' C1' 57.3(2) . . ? C2' B3' B8' 104.9(3) . . ? C1' B3' B8' 105.4(3) . . ? C2' B3' B7' 58.2(3) . . ? C1' B3' B7' 104.6(3) . . ? B8' B3' B7' 60.3(3) . . ? C2' B3' B4' 104.7(3) . . ? C1' B3' B4' 58.7(3) . . ? B8' B3' B4' 60.3(3) . . ? B7' B3' B4' 108.0(4) . . ? C1' B4' B9' 105.3(3) . . ? C1' B4' B8' 105.2(3) . . ? B9' B4' B8' 60.6(3) . . ? C1' B4' B5' 58.9(2) . . ? B9' B4' B5' 59.9(3) . . ? B8' B4' B5' 108.3(3) . . ? C1' B4' B3' 59.6(3) . . ? B9' B4' B3' 108.1(3) . . ? B8' B4' B3' 59.2(3) . . ? B5' B4' B3' 108.5(3) . . ? C1' B5' B9' 105.3(3) . . ? C1' B5' B10' 105.5(3) . . ? B9' B5' B10' 60.2(3) . . ? C1' B5' B4' 59.1(2) . . ? B9' B5' B4' 59.7(3) . . ? B10' B5' B4' 108.0(4) . . ? C1' B5' B6' 59.1(2) . . ? B9' B5' B6' 107.7(3) . . ? B10' B5' B6' 59.7(3) . . ? B4' B5' B6' 108.0(3) . . ? C2' B6' C1' 57.8(2) . . ? C2' B6' B11' 58.7(3) . . ? C1' B6' B11' 105.3(4) . . ? C2' B6' B10' 105.4(4) . . ? C1' B6' B10' 105.4(3) . . ? B11' B6' B10' 60.3(3) . . ? C2' B6' B5' 105.2(3) . . ? C1' B6' B5' 58.7(2) . . ? B11' B6' B5' 108.0(4) . . ? B10' B6' B5' 59.9(3) . . ? C2' B7' B11' 59.1(3) . . ? C2' B7' B3' 59.9(3) . . ? B11' B7' B3' 109.0(4) . . ? C2' B7' B8' 105.6(4) . . ? B11' B7' B8' 108.3(4) . . ? B3' B7' B8' 59.5(3) . . ? C2' B7' B12' 106.0(4) . . ? B11' B7' B12' 60.3(3) . . ? B3' B7' B12' 108.3(4) . . ? B8' B7' B12' 60.2(3) . . ? B3' B8' B7' 60.2(3) . . ? B3' B8' B4' 60.6(3) . . ? B7' B8' B4' 108.1(4) . . ? B3' B8' B12' 108.8(4) . . ? B7' B8' B12' 60.0(3) . . ? B4' B8' B12' 108.3(4) . . ? B3' B8' B9' 108.3(4) . . ? B7' B8' B9' 107.8(4) . . ? B4' B8' B9' 59.5(3) . . ? B12' B8' B9' 60.3(3) . . ? B4' B9' B5' 60.4(3) . . ? B4' B9' B10' 108.4(4) . . ? B5' B9' B10' 60.1(3) . . ? B4' B9' B8' 60.0(3) . . ? B5' B9' B8' 108.1(3) . . ? B10' B9' B8' 108.0(4) . . ? B4' B9' B12' 108.0(4) . . ? B5' B9' B12' 108.5(3) . . ? B10' B9' B12' 60.5(3) . . ? B8' B9' B12' 59.5(3) . . ? B6' B10' B5' 60.3(3) . . ? B6' B10' B9' 107.9(3) . . ? B5' B10' B9' 59.7(3) . . ? B6' B10' B11' 59.8(3) . . ? B5' B10' B11' 107.9(3) . . ? B9' B10' B11' 107.5(4) . . ? B6' B10' B12' 107.6(4) . . ? B5' B10' B12' 107.9(3) . . ? B9' B10' B12' 60.1(3) . . ? B11' B10' B12' 59.5(3) . . ? C2' B11' B7' 58.6(3) . . ? C2' B11' B6' 59.2(3) . . ? B7' B11' B6' 108.1(3) . . ? C2' B11' B12' 105.4(4) . . ? B7' B11' B12' 60.0(3) . . ? B6' B11' B12' 108.6(4) . . ? C2' B11' B10' 105.4(3) . . ? B7' B11' B10' 108.4(4) . . ? B6' B11' B10' 59.8(3) . . ? B12' B11' B10' 60.7(3) . . ? B7' B12' B8' 59.9(3) . . ? B7' B12' B11' 59.7(3) . . ? B8' B12' B11' 107.6(4) . . ? B7' B12' B9' 107.6(4) . . ? B8' B12' B9' 60.1(3) . . ? B11' B12' B9' 107.2(4) . . ? B7' B12' B10' 107.4(4) . . ? B8' B12' B10' 107.6(4) . . ? B11' B12' B10' 59.8(3) . . ? B9' B12' B10' 59.4(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.266 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.062 # Attachment '- Compound 5.cif' data_2008acc0741 _database_code_depnum_ccdc_archive 'CCDC 756376' #TrackingRef '- Compound 5.cif' _chemical_compound_source 'Jose Giner Planas' _database_code_CSD 8ACC0741 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H22 B10 O' _chemical_formula_weight 326.43 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 19.0233(5) _cell_length_b 8.3839(2) _cell_length_c 22.8968(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.012(2) _cell_angle_gamma 90.00 _cell_volume 3631.71(17) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 19050 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9808 _exptl_absorpt_correction_T_max 0.9888 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; SADABS was used to perform the Absorption correction Estimated minimum and maximum transmission: 0.6457 0.7456 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21122 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4146 _reflns_number_gt 2966 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(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^)+(0.1064P)^2^+2.6588P] 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 SHELXL _refine_ls_extinction_coef 0.0055(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4146 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1883 _refine_ls_wR_factor_gt 0.1672 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _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 C1 C 0.10287(9) 0.5620(2) 0.34752(8) 0.0243(4) Uani 1 1 d . . . C2 C 0.18419(9) 0.5593(2) 0.38500(8) 0.0210(4) Uani 1 1 d . . . C3 C 0.05083(10) 0.4324(2) 0.35986(9) 0.0297(5) Uani 1 1 d . . . C4 C 0.01103(11) 0.4423(3) 0.40704(12) 0.0432(6) Uani 1 1 d . . . H4 H 0.0179 0.5293 0.4336 0.052 Uiso 1 1 calc R . . C5 C -0.03893(12) 0.3260(4) 0.41579(14) 0.0580(8) Uani 1 1 d . . . H5 H -0.0670 0.3354 0.4476 0.070 Uiso 1 1 calc R . . C6 C -0.04786(13) 0.1966(3) 0.37822(15) 0.0612(9) Uani 1 1 d . . . H6 H -0.0813 0.1161 0.3846 0.073 Uiso 1 1 calc R . . C7 C -0.00810(14) 0.1852(3) 0.33156(15) 0.0588(8) Uani 1 1 d . . . H7 H -0.0143 0.0962 0.3058 0.071 Uiso 1 1 calc R . . C8 C 0.04113(12) 0.3021(3) 0.32153(12) 0.0432(6) Uani 1 1 d . . . H8 H 0.0680 0.2936 0.2889 0.052 Uiso 1 1 calc R . . C9 C 0.19843(9) 0.4218(2) 0.42969(8) 0.0228(4) Uani 1 1 d . . . H9 H 0.1705 0.3264 0.4148 0.027 Uiso 1 1 calc R . . C10 C 0.27619(9) 0.3775(2) 0.43779(8) 0.0228(4) Uani 1 1 d . . . C11 C 0.32206(10) 0.4471(2) 0.48197(8) 0.0270(4) Uani 1 1 d . . . H11 H 0.3043 0.5201 0.5086 0.032 Uiso 1 1 calc R . . C12 C 0.39302(10) 0.4105(3) 0.48730(10) 0.0339(5) Uani 1 1 d . . . H12 H 0.4239 0.4571 0.5179 0.041 Uiso 1 1 calc R . . C13 C 0.41959(10) 0.3060(3) 0.44815(10) 0.0355(5) Uani 1 1 d . . . H13 H 0.4688 0.2832 0.4514 0.043 Uiso 1 1 calc R . . C14 C 0.37465(11) 0.2352(3) 0.40443(9) 0.0345(5) Uani 1 1 d . . . H14 H 0.3929 0.1639 0.3775 0.041 Uiso 1 1 calc R . . C15 C 0.30254(10) 0.2681(2) 0.39980(8) 0.0293(4) Uani 1 1 d . . . H15 H 0.2713 0.2160 0.3708 0.035 Uiso 1 1 calc R . . B3 B 0.12463(11) 0.7049(2) 0.40086(10) 0.0257(5) Uani 1 1 d . . . H3 H 0.1001 0.7123 0.4432 0.031 Uiso 1 1 calc R . . B4 B 0.07643(12) 0.7543(3) 0.33267(10) 0.0289(5) Uani 1 1 d . . . H4A H 0.0201 0.7952 0.3298 0.035 Uiso 1 1 calc R . . B5 B 0.10762(12) 0.6314(3) 0.27787(10) 0.0294(5) Uani 1 1 d . . . H5A H 0.0717 0.5911 0.2387 0.035 Uiso 1 1 calc R . . B6 B 0.17510(11) 0.5053(2) 0.31214(9) 0.0234(4) Uani 1 1 d . . . H6A H 0.1838 0.3812 0.2963 0.028 Uiso 1 1 calc R . . B7 B 0.21538(12) 0.7479(2) 0.39688(10) 0.0263(5) Uani 1 1 d . . . H7A H 0.2510 0.7841 0.4367 0.032 Uiso 1 1 calc R . . B8 B 0.14833(12) 0.8763(3) 0.36262(10) 0.0281(5) Uani 1 1 d . . . H8A H 0.1397 0.9995 0.3794 0.034 Uiso 1 1 calc R . . B9 B 0.13763(13) 0.8315(3) 0.28621(10) 0.0308(5) Uani 1 1 d . . . H9A H 0.1220 0.9250 0.2524 0.037 Uiso 1 1 calc R . . B10 B 0.19819(12) 0.6762(3) 0.27344(10) 0.0294(5) Uani 1 1 d . . . H10 H 0.2224 0.6667 0.2310 0.035 Uiso 1 1 calc R . . B11 B 0.24604(11) 0.6266(2) 0.34171(10) 0.0247(4) Uani 1 1 d . . . H11A H 0.3020 0.5836 0.3449 0.030 Uiso 1 1 calc R . . B12 B 0.22367(12) 0.8284(3) 0.32604(10) 0.0291(5) Uani 1 1 d . . . H12A H 0.2647 0.9199 0.3186 0.035 Uiso 1 1 calc R . . O1 O 0.17337(7) 0.47325(17) 0.48282(6) 0.0293(3) Uani 1 1 d . . . H1 H 0.1290 0.4694 0.4794 0.044 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 C1 0.0214(9) 0.0213(9) 0.0294(10) 0.0013(7) -0.0015(7) 0.0029(7) C2 0.0229(9) 0.0179(8) 0.0217(9) -0.0002(7) 0.0003(7) -0.0002(7) C3 0.0207(9) 0.0254(10) 0.0411(12) 0.0072(8) -0.0060(8) 0.0005(7) C4 0.0268(10) 0.0427(13) 0.0600(16) 0.0122(11) 0.0030(10) 0.0006(9) C5 0.0306(12) 0.0671(18) 0.075(2) 0.0333(16) 0.0011(12) -0.0067(12) C6 0.0341(13) 0.0500(16) 0.093(2) 0.0355(16) -0.0249(14) -0.0183(11) C7 0.0483(15) 0.0326(13) 0.088(2) 0.0092(13) -0.0267(15) -0.0124(11) C8 0.0343(11) 0.0312(12) 0.0609(16) -0.0005(10) -0.0106(10) -0.0058(9) C9 0.0251(9) 0.0216(9) 0.0216(9) 0.0022(7) 0.0019(7) 0.0022(7) C10 0.0250(9) 0.0221(9) 0.0211(9) 0.0039(7) 0.0015(7) 0.0025(7) C11 0.0278(9) 0.0253(10) 0.0272(10) -0.0018(8) 0.0002(7) 0.0027(7) C12 0.0269(10) 0.0357(11) 0.0377(12) 0.0028(9) -0.0031(8) -0.0028(8) C13 0.0249(10) 0.0380(12) 0.0440(13) 0.0087(9) 0.0060(9) 0.0060(8) C14 0.0378(11) 0.0387(11) 0.0283(11) 0.0042(9) 0.0090(8) 0.0132(9) C15 0.0348(10) 0.0295(10) 0.0231(10) 0.0005(8) 0.0003(8) 0.0086(8) B3 0.0297(11) 0.0218(10) 0.0257(11) -0.0012(8) 0.0034(8) 0.0034(8) B4 0.0314(11) 0.0227(11) 0.0317(12) 0.0023(9) -0.0011(9) 0.0060(9) B5 0.0382(12) 0.0240(11) 0.0240(11) 0.0000(8) -0.0062(9) 0.0052(9) B6 0.0258(10) 0.0225(10) 0.0210(10) -0.0008(8) -0.0016(8) 0.0022(8) B7 0.0326(11) 0.0201(10) 0.0253(11) -0.0006(8) -0.0009(8) -0.0007(8) B8 0.0361(12) 0.0198(10) 0.0275(12) 0.0013(8) -0.0001(9) 0.0015(9) B9 0.0407(12) 0.0226(11) 0.0280(12) 0.0039(9) -0.0023(9) 0.0025(9) B10 0.0386(12) 0.0262(11) 0.0236(11) 0.0036(9) 0.0043(9) 0.0042(9) B11 0.0258(10) 0.0234(10) 0.0249(11) 0.0021(8) 0.0023(8) 0.0010(8) B12 0.0334(12) 0.0231(10) 0.0306(12) 0.0049(9) 0.0025(9) -0.0026(9) O1 0.0271(7) 0.0359(8) 0.0260(7) 0.0042(6) 0.0082(5) 0.0055(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C3 1.516(3) . ? C1 C2 1.689(2) . ? C1 B5 1.709(3) . ? C1 B4 1.713(3) . ? C1 B3 1.730(3) . ? C1 B6 1.733(3) . ? C2 C9 1.546(2) . ? C2 B7 1.700(3) . ? C2 B11 1.712(3) . ? C2 B6 1.720(3) . ? C2 B3 1.730(3) . ? C3 C4 1.385(3) . ? C3 C8 1.402(3) . ? C4 C5 1.391(3) . ? C4 H4 0.9500 . ? C5 C6 1.384(5) . ? C5 H5 0.9500 . ? C6 C7 1.375(4) . ? C6 H6 0.9500 . ? C7 C8 1.391(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 O1 1.419(2) . ? C9 C10 1.518(2) . ? C9 H9 1.0000 . ? C10 C15 1.393(3) . ? C10 C11 1.393(3) . ? C11 C12 1.377(3) . ? C11 H11 0.9500 . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 C14 1.381(3) . ? C13 H13 0.9500 . ? C14 C15 1.392(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? B3 B8 1.766(3) . ? B3 B4 1.775(3) . ? B3 B7 1.775(3) . ? B3 H3 1.1200 . ? B4 B5 1.773(3) . ? B4 B9 1.779(3) . ? B4 B8 1.786(3) . ? B4 H4A 1.1200 . ? B5 B9 1.776(3) . ? B5 B10 1.777(3) . ? B5 B6 1.780(3) . ? B5 H5A 1.1200 . ? B6 B10 1.764(3) . ? B6 B11 1.767(3) . ? B6 H6A 1.1200 . ? B7 B11 1.767(3) . ? B7 B12 1.779(3) . ? B7 B8 1.787(3) . ? B7 H7A 1.1200 . ? B8 B12 1.780(3) . ? B8 B9 1.780(3) . ? B8 H8A 1.1200 . ? B9 B10 1.783(3) . ? B9 B12 1.789(3) . ? B9 H9A 1.1200 . ? B10 B11 1.774(3) . ? B10 B12 1.787(3) . ? B10 H10 1.1200 . ? B11 B12 1.772(3) . ? B11 H11A 1.1200 . ? B12 H12A 1.1200 . ? O1 H1 0.8400 . ? 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 C3 C1 C2 118.50(14) . . ? C3 C1 B5 121.16(16) . . ? C2 C1 B5 110.10(14) . . ? C3 C1 B4 121.84(15) . . ? C2 C1 B4 110.34(14) . . ? B5 C1 B4 62.43(13) . . ? C3 C1 B3 118.50(16) . . ? C2 C1 B3 60.77(11) . . ? B5 C1 B3 113.00(14) . . ? B4 C1 B3 62.06(12) . . ? C3 C1 B6 117.13(15) . . ? C2 C1 B6 60.33(11) . . ? B5 C1 B6 62.30(12) . . ? B4 C1 B6 113.34(15) . . ? B3 C1 B6 112.16(14) . . ? C9 C2 C1 115.71(14) . . ? C9 C2 B7 123.58(14) . . ? C1 C2 B7 110.79(13) . . ? C9 C2 B11 123.06(14) . . ? C1 C2 B11 110.49(14) . . ? B7 C2 B11 62.39(12) . . ? C9 C2 B6 116.00(14) . . ? C1 C2 B6 61.11(11) . . ? B7 C2 B6 113.45(14) . . ? B11 C2 B6 61.99(12) . . ? C9 C2 B3 117.41(15) . . ? C1 C2 B3 60.80(11) . . ? B7 C2 B3 62.33(12) . . ? B11 C2 B3 113.21(14) . . ? B6 C2 B3 112.84(14) . . ? C4 C3 C8 119.2(2) . . ? C4 C3 C1 121.55(19) . . ? C8 C3 C1 119.2(2) . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 119.7(2) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 120.9(3) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C7 C8 C3 119.5(3) . . ? C7 C8 H8 120.2 . . ? C3 C8 H8 120.2 . . ? O1 C9 C10 112.35(14) . . ? O1 C9 C2 106.83(14) . . ? C10 C9 C2 111.37(15) . . ? O1 C9 H9 108.7 . . ? C10 C9 H9 108.7 . . ? C2 C9 H9 108.7 . . ? C15 C10 C11 119.36(17) . . ? C15 C10 C9 119.65(16) . . ? C11 C10 C9 120.98(17) . . ? C12 C11 C10 120.31(19) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.26(19) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 120.05(19) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.00(19) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C10 C15 C14 119.94(18) . . ? C10 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C2 B3 C1 58.43(10) . . ? C2 B3 B8 105.26(15) . . ? C1 B3 B8 105.56(15) . . ? C2 B3 B4 105.63(15) . . ? C1 B3 B4 58.49(11) . . ? B8 B3 B4 60.60(12) . . ? C2 B3 B7 58.02(11) . . ? C1 B3 B7 105.43(15) . . ? B8 B3 B7 60.61(12) . . ? B4 B3 B7 108.85(16) . . ? C2 B3 H3 124.2 . . ? C1 B3 H3 123.9 . . ? B8 B3 H3 122.4 . . ? B4 B3 H3 121.7 . . ? B7 B3 H3 121.9 . . ? C1 B4 B5 58.67(12) . . ? C1 B4 B3 59.45(11) . . ? B5 B4 B3 107.84(15) . . ? C1 B4 B9 105.32(15) . . ? B5 B4 B9 60.00(13) . . ? B3 B4 B9 107.50(16) . . ? C1 B4 B8 105.41(14) . . ? B5 B4 B8 107.75(16) . . ? B3 B4 B8 59.44(12) . . ? B9 B4 B8 59.91(13) . . ? C1 B4 H4A 124.0 . . ? B5 B4 H4A 121.7 . . ? B3 B4 H4A 121.7 . . ? B9 B4 H4A 122.4 . . ? B8 B4 H4A 122.5 . . ? C1 B5 B4 58.90(12) . . ? C1 B5 B9 105.61(15) . . ? B4 B5 B9 60.15(13) . . ? C1 B5 B10 105.76(15) . . ? B4 B5 B10 108.41(16) . . ? B9 B5 B10 60.25(13) . . ? C1 B5 B6 59.52(11) . . ? B4 B5 B6 108.22(15) . . ? B9 B5 B6 107.74(15) . . ? B10 B5 B6 59.47(12) . . ? C1 B5 H5A 123.8 . . ? B4 B5 H5A 121.3 . . ? B9 B5 H5A 122.2 . . ? B10 B5 H5A 122.1 . . ? B6 B5 H5A 121.6 . . ? C2 B6 C1 58.56(11) . . ? C2 B6 B10 105.56(14) . . ? C1 B6 B10 105.27(14) . . ? C2 B6 B11 58.77(11) . . ? C1 B6 B11 105.91(15) . . ? B10 B6 B11 60.31(12) . . ? C2 B6 B5 105.40(14) . . ? C1 B6 B5 58.18(12) . . ? B10 B6 B5 60.16(13) . . ? B11 B6 B5 108.27(15) . . ? C2 B6 H6A 123.7 . . ? C1 B6 H6A 123.9 . . ? B10 B6 H6A 122.6 . . ? B11 B6 H6A 121.7 . . ? B5 B6 H6A 122.2 . . ? C2 B7 B11 59.12(12) . . ? C2 B7 B3 59.65(11) . . ? B11 B7 B3 108.40(15) . . ? C2 B7 B12 105.66(15) . . ? B11 B7 B12 59.96(12) . . ? B3 B7 B12 107.66(15) . . ? C2 B7 B8 105.61(14) . . ? B11 B7 B8 107.86(15) . . ? B3 B7 B8 59.43(12) . . ? B12 B7 B8 59.89(13) . . ? C2 B7 H7A 123.6 . . ? B11 B7 H7A 121.4 . . ? B3 B7 H7A 121.5 . . ? B12 B7 H7A 122.4 . . ? B8 B7 H7A 122.5 . . ? B3 B8 B12 108.05(15) . . ? B3 B8 B9 107.87(15) . . ? B12 B8 B9 60.32(13) . . ? B3 B8 B7 59.96(12) . . ? B12 B8 B7 59.85(13) . . ? B9 B8 B7 107.89(16) . . ? B3 B8 B4 59.96(12) . . ? B12 B8 B4 108.19(16) . . ? B9 B8 B4 59.84(13) . . ? B7 B8 B4 107.83(15) . . ? B3 B8 H8A 121.8 . . ? B12 B8 H8A 121.5 . . ? B9 B8 H8A 121.7 . . ? B7 B8 H8A 121.9 . . ? B4 B8 H8A 121.8 . . ? B5 B9 B8 107.91(16) . . ? B5 B9 B4 59.85(13) . . ? B8 B9 B4 60.25(13) . . ? B5 B9 B10 59.89(13) . . ? B8 B9 B10 107.81(15) . . ? B4 B9 B10 107.88(15) . . ? B5 B9 B12 107.93(15) . . ? B8 B9 B12 59.84(13) . . ? B4 B9 B12 108.13(15) . . ? B10 B9 B12 60.04(13) . . ? B5 B9 H9A 121.9 . . ? B8 B9 H9A 121.8 . . ? B4 B9 H9A 121.6 . . ? B10 B9 H9A 121.8 . . ? B12 B9 H9A 121.7 . . ? B6 B10 B11 59.93(12) . . ? B6 B10 B5 60.38(12) . . ? B11 B10 B5 108.15(16) . . ? B6 B10 B9 108.16(16) . . ? B11 B10 B9 107.90(16) . . ? B5 B10 B9 59.87(13) . . ? B6 B10 B12 107.81(15) . . ? B11 B10 B12 59.70(12) . . ? B5 B10 B12 107.99(16) . . ? B9 B10 B12 60.14(13) . . ? B6 B10 H10 121.6 . . ? B11 B10 H10 121.8 . . ? B5 B10 H10 121.6 . . ? B9 B10 H10 121.7 . . ? B12 B10 H10 121.9 . . ? C2 B11 B6 59.23(11) . . ? C2 B11 B7 58.49(11) . . ? B6 B11 B7 108.00(15) . . ? C2 B11 B10 105.49(15) . . ? B6 B11 B10 59.76(12) . . ? B7 B11 B10 108.53(15) . . ? C2 B11 B12 105.48(15) . . ? B6 B11 B12 108.33(14) . . ? B7 B11 B12 60.35(13) . . ? B10 B11 B12 60.51(12) . . ? C2 B11 H11A 124.3 . . ? B6 B11 H11A 121.5 . . ? B7 B11 H11A 121.5 . . ? B10 B11 H11A 122.0 . . ? B12 B11 H11A 121.8 . . ? B11 B12 B8 107.95(15) . . ? B11 B12 B7 59.69(12) . . ? B8 B12 B7 60.27(12) . . ? B11 B12 B9 107.73(15) . . ? B8 B12 B9 59.84(13) . . ? B7 B12 B9 107.85(16) . . ? B11 B12 B10 59.79(12) . . ? B8 B12 B10 107.65(16) . . ? B7 B12 B10 107.43(15) . . ? B9 B12 B10 59.83(13) . . ? B11 B12 H12A 121.9 . . ? B8 B12 H12A 121.7 . . ? B7 B12 H12A 121.9 . . ? B9 B12 H12A 121.9 . . ? B10 B12 H12A 122.1 . . ? C9 O1 H1 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.482 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.075 # Attachment '- Compound 4.cif' data_2009gjt0005 _database_code_depnum_ccdc_archive 'CCDC 756377' #TrackingRef '- Compound 4.cif' _chemical_compound_source Pepe _database_code_CSD 9GJT005 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H19 B10 N O' _chemical_formula_sum 'C9 H19 B10 N O' _chemical_formula_weight 265.35 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.8781(6) _cell_length_b 14.4748(4) _cell_length_c 14.8852(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2990.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 24498 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9870 _exptl_absorpt_correction_T_max 0.9938 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; SADABS was used to perform the Absorption correction Estimated minimum and maximum transmission: 0.6001 0.7456 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22544 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3414 _reflns_number_gt 2772 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(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^)+(0.0687P)^2^+1.7077P] 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 SHELXL _refine_ls_extinction_coef 0.014(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3414 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1431 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _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 C1 C 0.32736(10) -0.04132(9) 0.37716(10) 0.0170(3) Uani 1 1 d . . . C2 C 0.23169(11) 0.02987(11) 0.37142(11) 0.0224(3) Uani 1 1 d . . . C3 C 0.40483(11) -0.03260(10) 0.30190(11) 0.0204(3) Uani 1 1 d . . . H3 H 0.3737 -0.0055 0.2473 0.024 Uiso 1 1 calc R . . C4 C 0.44629(11) -0.12624(10) 0.27736(10) 0.0188(3) Uani 1 1 d . . . C5 C 0.51925(11) -0.16584(11) 0.32844(11) 0.0237(4) Uani 1 1 d . . . H5 H 0.5448 -0.1344 0.3791 0.028 Uiso 1 1 calc R . . C6 C 0.55407(12) -0.25182(11) 0.30422(12) 0.0272(4) Uani 1 1 d . . . H6 H 0.6024 -0.2793 0.3406 0.033 Uiso 1 1 calc R . . N1 N 0.52299(10) -0.29824(9) 0.23187(10) 0.0265(3) Uani 1 1 d . . . C7 C 0.45487(12) -0.25836(11) 0.18179(12) 0.0265(4) Uani 1 1 d . . . H7 H 0.4333 -0.2898 0.1295 0.032 Uiso 1 1 calc R . . C8 C 0.41405(11) -0.17352(11) 0.20212(11) 0.0235(4) Uani 1 1 d . . . H8 H 0.3649 -0.1482 0.1652 0.028 Uiso 1 1 calc R . . C9 C 0.22504(14) 0.09909(12) 0.29504(12) 0.0325(4) Uani 1 1 d . . . H9A H 0.2856 0.1336 0.2908 0.049 Uiso 1 1 calc R . . H9B H 0.1719 0.1420 0.3066 0.049 Uiso 1 1 calc R . . H9C H 0.2134 0.0663 0.2385 0.049 Uiso 1 1 calc R . . B3 B 0.31819(13) 0.04975(12) 0.45191(12) 0.0222(4) Uani 1 1 d . . . H3A H 0.3675 0.1110 0.4522 0.027 Uiso 1 1 calc R . . B4 B 0.35723(12) -0.06162(12) 0.48638(12) 0.0203(4) Uani 1 1 d . . . H4 H 0.4327 -0.0741 0.5102 0.024 Uiso 1 1 calc R . . B5 B 0.29368(12) -0.14548(11) 0.42215(12) 0.0208(4) Uani 1 1 d . . . H5A H 0.3272 -0.2134 0.4041 0.025 Uiso 1 1 calc R . . B6 B 0.21713(12) -0.08571(13) 0.34650(13) 0.0231(4) Uani 1 1 d . . . H6A H 0.2008 -0.1128 0.2777 0.028 Uiso 1 1 calc R . . B7 B 0.19327(14) 0.05942(13) 0.47587(13) 0.0272(4) Uani 1 1 d . . . H7A H 0.1596 0.1275 0.4930 0.033 Uiso 1 1 calc R . . B8 B 0.27117(13) 0.00109(13) 0.55128(12) 0.0244(4) Uani 1 1 d . . . H8A H 0.2894 0.0300 0.6190 0.029 Uiso 1 1 calc R . . B9 B 0.25565(13) -0.12006(13) 0.53312(13) 0.0239(4) Uani 1 1 d . . . H9 H 0.2635 -0.1712 0.5891 0.029 Uiso 1 1 calc R . . B10 B 0.16868(13) -0.13532(13) 0.44534(14) 0.0272(4) Uani 1 1 d . . . H10 H 0.1191 -0.1963 0.4429 0.033 Uiso 1 1 calc R . . B11 B 0.13079(14) -0.02405(14) 0.41060(14) 0.0293(4) Uani 1 1 d . . . H11 H 0.0563 -0.0112 0.3845 0.035 Uiso 1 1 calc R . . B12 B 0.15466(14) -0.04488(13) 0.52631(14) 0.0278(4) Uani 1 1 d . . . H12 H 0.0958 -0.0464 0.5778 0.033 Uiso 1 1 calc R . . O1 O 0.48037(8) 0.02458(8) 0.32792(9) 0.0279(3) Uani 1 1 d . . . H1A H 0.4708 0.0782 0.3082 0.042 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 C1 0.0165(7) 0.0150(6) 0.0196(7) -0.0006(5) -0.0012(6) 0.0016(5) C2 0.0223(8) 0.0241(8) 0.0207(8) -0.0013(6) -0.0009(6) 0.0092(6) C3 0.0223(8) 0.0166(7) 0.0223(8) 0.0016(6) 0.0034(6) -0.0001(6) C4 0.0182(7) 0.0154(7) 0.0229(8) 0.0023(5) 0.0061(6) -0.0008(5) C5 0.0195(7) 0.0222(8) 0.0295(9) -0.0021(6) 0.0004(6) 0.0006(6) C6 0.0210(8) 0.0253(8) 0.0353(9) 0.0017(7) 0.0009(7) 0.0053(6) N1 0.0229(7) 0.0197(6) 0.0368(8) -0.0026(6) 0.0067(6) 0.0016(5) C7 0.0265(8) 0.0245(8) 0.0284(9) -0.0060(6) 0.0032(7) -0.0017(6) C8 0.0233(8) 0.0247(8) 0.0225(8) -0.0005(6) 0.0017(6) 0.0025(6) C9 0.0407(10) 0.0322(9) 0.0246(9) 0.0045(7) -0.0005(7) 0.0187(8) B3 0.0278(9) 0.0190(8) 0.0199(8) -0.0030(6) 0.0002(7) 0.0006(7) B4 0.0199(8) 0.0216(8) 0.0193(8) 0.0022(6) -0.0024(6) -0.0011(6) B5 0.0181(8) 0.0180(8) 0.0263(9) 0.0015(7) 0.0024(7) -0.0023(6) B6 0.0163(8) 0.0270(9) 0.0260(9) -0.0060(7) -0.0018(7) -0.0004(6) B7 0.0300(10) 0.0282(9) 0.0233(9) -0.0024(7) 0.0047(8) 0.0095(7) B8 0.0261(9) 0.0276(9) 0.0196(9) -0.0012(7) 0.0008(7) 0.0000(7) B9 0.0207(8) 0.0266(9) 0.0245(9) 0.0037(7) 0.0040(7) -0.0004(7) B10 0.0175(8) 0.0305(9) 0.0336(10) -0.0027(8) 0.0031(7) -0.0035(7) B11 0.0177(9) 0.0399(11) 0.0304(10) -0.0021(8) -0.0005(8) 0.0067(7) B12 0.0221(9) 0.0338(10) 0.0275(10) -0.0010(8) 0.0047(8) 0.0041(7) O1 0.0271(6) 0.0196(6) 0.0371(7) 0.0000(5) 0.0015(5) -0.0052(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C3 1.558(2) . ? C1 C2 1.683(2) . ? C1 B4 1.703(2) . ? C1 B5 1.715(2) . ? C1 B6 1.721(2) . ? C1 B3 1.730(2) . ? C2 C9 1.518(2) . ? C2 B7 1.698(2) . ? C2 B11 1.706(3) . ? C2 B3 1.720(2) . ? C2 B6 1.725(2) . ? C3 O1 1.3907(19) . ? C3 C4 1.5171(19) . ? C3 H3 1.0000 . ? C4 C8 1.387(2) . ? C4 C5 1.390(2) . ? C5 C6 1.383(2) . ? C5 H5 0.9500 . ? C6 N1 1.341(2) . ? C6 H6 0.9500 . ? N1 C7 1.335(2) . ? C7 C8 1.386(2) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? B3 B8 1.763(3) . ? B3 B7 1.775(3) . ? B3 B4 1.776(2) . ? B3 H3A 1.1200 . ? B4 B5 1.779(2) . ? B4 B8 1.784(3) . ? B4 B9 1.785(2) . ? B4 H4 1.1200 . ? B5 B9 1.773(3) . ? B5 B6 1.774(3) . ? B5 B10 1.775(3) . ? B5 H5A 1.1200 . ? B6 B10 1.770(3) . ? B6 B11 1.773(3) . ? B6 H6A 1.1200 . ? B7 B12 1.769(3) . ? B7 B8 1.772(3) . ? B7 B11 1.776(3) . ? B7 H7A 1.1200 . ? B8 B9 1.787(3) . ? B8 B12 1.788(3) . ? B8 H8A 1.1200 . ? B9 B12 1.777(3) . ? B9 B10 1.792(3) . ? B9 H9 1.1200 . ? B10 B11 1.771(3) . ? B10 B12 1.790(3) . ? B10 H10 1.1200 . ? B11 B12 1.780(3) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? O1 H1A 0.8400 . ? 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 C3 C1 C2 117.28(12) . . ? C3 C1 B4 122.17(12) . . ? C2 C1 B4 110.25(11) . . ? C3 C1 B5 122.70(11) . . ? C2 C1 B5 110.07(11) . . ? B4 C1 B5 62.74(10) . . ? C3 C1 B6 116.94(12) . . ? C2 C1 B6 60.91(9) . . ? B4 C1 B6 113.90(12) . . ? B5 C1 B6 62.16(10) . . ? C3 C1 B3 116.85(12) . . ? C2 C1 B3 60.52(9) . . ? B4 C1 B3 62.31(10) . . ? B5 C1 B3 113.51(12) . . ? B6 C1 B3 112.94(12) . . ? C9 C2 C1 119.35(13) . . ? C9 C2 B7 120.02(13) . . ? C1 C2 B7 110.82(12) . . ? C9 C2 B11 120.54(14) . . ? C1 C2 B11 110.49(12) . . ? B7 C2 B11 62.91(11) . . ? C9 C2 B3 116.98(14) . . ? C1 C2 B3 61.08(9) . . ? B7 C2 B3 62.57(11) . . ? B11 C2 B3 114.28(13) . . ? C9 C2 B6 118.14(14) . . ? C1 C2 B6 60.64(9) . . ? B7 C2 B6 113.84(13) . . ? B11 C2 B6 62.21(10) . . ? B3 C2 B6 113.18(12) . . ? O1 C3 C4 108.23(13) . . ? O1 C3 C1 111.60(13) . . ? C4 C3 C1 111.25(11) . . ? O1 C3 H3 108.6 . . ? C4 C3 H3 108.6 . . ? C1 C3 H3 108.6 . . ? C8 C4 C5 118.25(14) . . ? C8 C4 C3 120.87(14) . . ? C5 C4 C3 120.87(14) . . ? C6 C5 C4 118.89(15) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? N1 C6 C5 123.24(15) . . ? N1 C6 H6 118.4 . . ? C5 C6 H6 118.4 . . ? C7 N1 C6 117.35(14) . . ? N1 C7 C8 123.42(15) . . ? N1 C7 H7 118.3 . . ? C8 C7 H7 118.3 . . ? C7 C8 C4 118.80(15) . . ? C7 C8 H8 120.6 . . ? C4 C8 H8 120.6 . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 B3 C1 58.39(9) . . ? C2 B3 B8 105.02(13) . . ? C1 B3 B8 105.21(12) . . ? C2 B3 B7 58.11(10) . . ? C1 B3 B7 105.14(12) . . ? B8 B3 B7 60.11(10) . . ? C2 B3 B4 105.21(12) . . ? C1 B3 B4 58.11(9) . . ? B8 B3 B4 60.54(10) . . ? B7 B3 B4 108.14(13) . . ? C2 B3 H3A 124.2 . . ? C1 B3 H3A 124.1 . . ? B8 B3 H3A 122.6 . . ? B7 B3 H3A 122.2 . . ? B4 B3 H3A 122.1 . . ? C1 B4 B3 59.57(9) . . ? C1 B4 B5 58.94(9) . . ? B3 B4 B5 108.22(12) . . ? C1 B4 B8 105.43(11) . . ? B3 B4 B8 59.38(10) . . ? B5 B4 B8 107.83(12) . . ? C1 B4 B9 105.16(12) . . ? B3 B4 B9 107.56(12) . . ? B5 B4 B9 59.65(10) . . ? B8 B4 B9 60.09(10) . . ? C1 B4 H4 123.9 . . ? B3 B4 H4 121.5 . . ? B5 B4 H4 121.6 . . ? B8 B4 H4 122.4 . . ? B9 B4 H4 122.5 . . ? C1 B5 B9 105.22(12) . . ? C1 B5 B6 59.09(9) . . ? B9 B5 B6 108.18(12) . . ? C1 B5 B10 105.64(12) . . ? B9 B5 B10 60.69(10) . . ? B6 B5 B10 59.84(10) . . ? C1 B5 B4 58.32(9) . . ? B9 B5 B4 60.35(10) . . ? B6 B5 B4 107.78(12) . . ? B10 B5 B4 108.87(12) . . ? C1 B5 H5A 124.4 . . ? B9 B5 H5A 121.9 . . ? B6 B5 H5A 121.7 . . ? B10 B5 H5A 121.7 . . ? B4 B5 H5A 121.5 . . ? C1 B6 C2 58.46(9) . . ? C1 B6 B10 105.58(12) . . ? C2 B6 B10 105.02(12) . . ? C1 B6 B11 105.67(12) . . ? C2 B6 B11 58.36(10) . . ? B10 B6 B11 60.00(11) . . ? C1 B6 B5 58.75(9) . . ? C2 B6 B5 105.45(12) . . ? B10 B6 B5 60.12(10) . . ? B11 B6 B5 107.98(13) . . ? C1 B6 H6A 123.6 . . ? C2 B6 H6A 124.1 . . ? B10 B6 H6A 122.8 . . ? B11 B6 H6A 122.1 . . ? B5 B6 H6A 122.1 . . ? C2 B7 B12 105.59(13) . . ? C2 B7 B8 105.56(12) . . ? B12 B7 B8 60.62(11) . . ? C2 B7 B3 59.32(10) . . ? B12 B7 B3 108.28(13) . . ? B8 B7 B3 59.61(10) . . ? C2 B7 B11 58.75(10) . . ? B12 B7 B11 60.25(11) . . ? B8 B7 B11 108.66(13) . . ? B3 B7 B11 108.25(13) . . ? C2 B7 H7A 124.1 . . ? B12 B7 H7A 121.9 . . ? B8 B7 H7A 122.0 . . ? B3 B7 H7A 121.5 . . ? B11 B7 H7A 121.3 . . ? B3 B8 B7 60.28(10) . . ? B3 B8 B4 60.09(10) . . ? B7 B8 B4 107.92(12) . . ? B3 B8 B9 108.04(12) . . ? B7 B8 B9 107.35(13) . . ? B4 B8 B9 59.98(10) . . ? B3 B8 B12 108.00(13) . . ? B7 B8 B12 59.60(11) . . ? B4 B8 B12 107.68(12) . . ? B9 B8 B12 59.63(10) . . ? B3 B8 H8A 121.4 . . ? B7 B8 H8A 122.0 . . ? B4 B8 H8A 121.7 . . ? B9 B8 H8A 122.0 . . ? B12 B8 H8A 122.0 . . ? B5 B9 B12 107.99(13) . . ? B5 B9 B4 60.01(10) . . ? B12 B9 B4 108.08(12) . . ? B5 B9 B8 107.98(12) . . ? B12 B9 B8 60.19(11) . . ? B4 B9 B8 59.93(10) . . ? B5 B9 B10 59.71(10) . . ? B12 B9 B10 60.19(11) . . ? B4 B9 B10 107.82(13) . . ? B8 B9 B10 108.20(13) . . ? B5 B9 H9 121.8 . . ? B12 B9 H9 121.5 . . ? B4 B9 H9 121.8 . . ? B8 B9 H9 121.6 . . ? B10 B9 H9 121.8 . . ? B6 B10 B11 60.08(11) . . ? B6 B10 B5 60.04(10) . . ? B11 B10 B5 107.98(13) . . ? B6 B10 B12 107.72(13) . . ? B11 B10 B12 59.96(11) . . ? B5 B10 B12 107.33(13) . . ? B6 B10 B9 107.47(12) . . ? B11 B10 B9 107.50(13) . . ? B5 B10 B9 59.59(10) . . ? B12 B10 B9 59.49(11) . . ? B6 B10 H10 121.8 . . ? B11 B10 H10 121.7 . . ? B5 B10 H10 121.9 . . ? B12 B10 H10 122.1 . . ? B9 B10 H10 122.3 . . ? C2 B11 B10 105.79(12) . . ? C2 B11 B6 59.44(10) . . ? B10 B11 B6 59.92(11) . . ? C2 B11 B7 58.34(10) . . ? B10 B11 B7 108.29(13) . . ? B6 B11 B7 107.87(13) . . ? C2 B11 B12 104.81(13) . . ? B10 B11 B12 60.54(11) . . ? B6 B11 B12 108.05(13) . . ? B7 B11 B12 59.67(11) . . ? C2 B11 H11 124.3 . . ? B10 B11 H11 121.8 . . ? B6 B11 H11 121.4 . . ? B7 B11 H11 121.8 . . ? B12 B11 H11 122.4 . . ? B7 B12 B9 107.93(13) . . ? B7 B12 B11 60.07(11) . . ? B9 B12 B11 107.80(13) . . ? B7 B12 B8 59.78(11) . . ? B9 B12 B8 60.18(10) . . ? B11 B12 B8 107.85(14) . . ? B7 B12 B10 107.78(13) . . ? B9 B12 B10 60.32(11) . . ? B11 B12 B10 59.50(11) . . ? B8 B12 B10 108.29(13) . . ? B7 B12 H12 121.9 . . ? B9 B12 H12 121.6 . . ? B11 B12 H12 122.0 . . ? B8 B12 H12 121.6 . . ? B10 B12 H12 121.7 . . ? C3 O1 H1A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.566 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.053 # Attachment '- Compound 6.cif' data_2009gjt0006 _database_code_depnum_ccdc_archive 'CCDC 756378' #TrackingRef '- Compound 6.cif' _chemical_compound_source Pepe _database_code_CSD 9GJT006 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H24 B10 O' _chemical_formula_sum 'C17 H24 B10 O' _chemical_formula_weight 352.46 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4' _symmetry_space_group_name_Hall 'I -4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 17.6653(3) _cell_length_b 17.6653(3) _cell_length_c 12.7609(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3982.20(13) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7633 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9877 _exptl_absorpt_correction_T_max 0.9877 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; SADABS was used to perform the Absorption correction Estimated minimum and maximum transmission: 0.6308 0.7456 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16051 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2387 _reflns_number_gt 2145 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(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^)+(0.0537P)^2^+2.6176P] 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 SHELXL _refine_ls_extinction_coef 0.0060(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2387 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1195 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.000 _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 C1 C 0.71629(14) 0.54360(14) 0.1117(2) 0.0174(5) Uani 1 1 d . . . C2 C 0.79776(14) 0.55719(13) 0.0414(2) 0.0178(5) Uani 1 1 d . . . C3 C 0.66862(13) 0.47270(14) 0.0869(2) 0.0182(5) Uani 1 1 d . . . H3 H 0.7011 0.4377 0.0447 0.022 Uiso 1 1 calc R . . C4 C 0.64468(16) 0.43072(16) 0.1839(2) 0.0266(6) Uani 1 1 d . . . H4 H 0.6837 0.4091 0.2254 0.032 Uiso 1 1 calc R . . C5 C 0.57510(16) 0.42115(15) 0.2163(2) 0.0269(6) Uani 1 1 d . . . H5 H 0.5363 0.4457 0.1776 0.032 Uiso 1 1 calc R . . C6 C 0.55121(16) 0.37522(16) 0.3085(2) 0.0283(6) Uani 1 1 d . . . C7 C 0.59285(16) 0.31596(17) 0.3500(3) 0.0311(6) Uani 1 1 d . . . H7 H 0.6400 0.3026 0.3194 0.037 Uiso 1 1 calc R . . C8 C 0.56615(19) 0.27597(18) 0.4360(3) 0.0372(7) Uani 1 1 d . . . H8 H 0.5957 0.2362 0.4649 0.045 Uiso 1 1 calc R . . C9 C 0.49681(19) 0.2937(2) 0.4800(3) 0.0390(8) Uani 1 1 d . . . H9 H 0.4783 0.2659 0.5383 0.047 Uiso 1 1 calc R . . C10 C 0.45479(19) 0.3523(2) 0.4383(3) 0.0415(8) Uani 1 1 d . . . H10 H 0.4073 0.3652 0.4684 0.050 Uiso 1 1 calc R . . C11 C 0.48138(18) 0.39231(18) 0.3530(3) 0.0343(7) Uani 1 1 d . . . H11 H 0.4516 0.4320 0.3244 0.041 Uiso 1 1 calc R . . C12 C 0.82102(14) 0.50157(14) -0.0424(2) 0.0208(5) Uani 1 1 d . . . C13 C 0.89032(16) 0.46446(16) -0.0337(2) 0.0297(6) Uani 1 1 d . . . H13 H 0.9198 0.4705 0.0280 0.036 Uiso 1 1 calc R . . C14 C 0.91684(18) 0.41874(18) -0.1142(3) 0.0364(7) Uani 1 1 d . . . H14 H 0.9649 0.3950 -0.1084 0.044 Uiso 1 1 calc R . . C15 C 0.87300(18) 0.40772(17) -0.2031(3) 0.0344(7) Uani 1 1 d . . . H15 H 0.8911 0.3766 -0.2584 0.041 Uiso 1 1 calc R . . C16 C 0.80277(17) 0.44224(16) -0.2111(2) 0.0295(6) Uani 1 1 d . . . H16 H 0.7721 0.4335 -0.2710 0.035 Uiso 1 1 calc R . . C17 C 0.77714(16) 0.48941(15) -0.1321(2) 0.0246(6) Uani 1 1 d . . . H17 H 0.7294 0.5137 -0.1389 0.030 Uiso 1 1 calc R . . B3 B 0.80214(16) 0.52798(17) 0.1707(2) 0.0216(6) Uani 1 1 d . . . H3A H 0.8224 0.4705 0.1949 0.026 Uiso 1 1 calc R . . B4 B 0.72710(17) 0.57516(17) 0.2377(2) 0.0225(6) Uani 1 1 d . . . H4A H 0.6985 0.5497 0.3076 0.027 Uiso 1 1 calc R . . B5 B 0.67606(17) 0.62835(17) 0.1424(2) 0.0222(6) Uani 1 1 d . . . H5A H 0.6135 0.6375 0.1493 0.027 Uiso 1 1 calc R . . B6 B 0.72017(16) 0.61494(15) 0.0192(3) 0.0200(6) Uani 1 1 d . . . H6 H 0.6869 0.6143 -0.0555 0.024 Uiso 1 1 calc R . . B7 B 0.86465(17) 0.59851(18) 0.1199(3) 0.0241(6) Uani 1 1 d . . . H7A H 0.9270 0.5883 0.1122 0.029 Uiso 1 1 calc R . . B8 B 0.82100(18) 0.61121(18) 0.2441(3) 0.0275(7) Uani 1 1 d . . . H8A H 0.8546 0.6095 0.3185 0.033 Uiso 1 1 calc R . . B9 B 0.74214(18) 0.67477(18) 0.2263(3) 0.0282(7) Uani 1 1 d . . . H9A H 0.7238 0.7154 0.2887 0.034 Uiso 1 1 calc R . . B10 B 0.73763(18) 0.69869(17) 0.0901(3) 0.0261(7) Uani 1 1 d . . . H10A H 0.7160 0.7549 0.0628 0.031 Uiso 1 1 calc R . . B11 B 0.81379(17) 0.65232(16) 0.0250(3) 0.0232(6) Uani 1 1 d . . . H11A H 0.8424 0.6775 -0.0451 0.028 Uiso 1 1 calc R . . B12 B 0.82701(18) 0.68813(18) 0.1539(3) 0.0275(7) Uani 1 1 d . . . H12 H 0.8647 0.7379 0.1694 0.033 Uiso 1 1 calc R . . O1 O 0.60749(10) 0.49560(10) 0.02226(15) 0.0224(4) Uani 1 1 d . . . H1 H 0.5807 0.4578 0.0074 0.034 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 C1 0.0165(11) 0.0175(12) 0.0182(11) 0.0005(10) -0.0021(10) 0.0002(9) C2 0.0152(11) 0.0170(11) 0.0212(13) 0.0007(10) -0.0013(10) -0.0005(9) C3 0.0155(11) 0.0190(12) 0.0202(13) 0.0019(10) -0.0041(10) -0.0001(9) C4 0.0292(14) 0.0291(14) 0.0215(14) 0.0017(11) -0.0051(12) -0.0074(11) C5 0.0278(14) 0.0261(14) 0.0267(15) -0.0033(12) -0.0019(12) 0.0022(11) C6 0.0362(15) 0.0284(14) 0.0204(13) -0.0063(11) 0.0026(12) -0.0144(12) C7 0.0223(13) 0.0367(15) 0.0341(16) -0.0076(13) 0.0001(12) -0.0052(11) C8 0.0429(18) 0.0310(16) 0.0378(17) 0.0054(14) -0.0149(15) -0.0048(13) C9 0.0423(17) 0.0522(19) 0.0226(15) 0.0057(15) -0.0019(14) -0.0231(15) C10 0.0318(16) 0.064(2) 0.0288(16) -0.0094(16) 0.0068(14) -0.0009(15) C11 0.0372(16) 0.0351(16) 0.0305(16) -0.0028(14) -0.0030(13) 0.0064(13) C12 0.0203(12) 0.0166(11) 0.0254(13) 0.0002(10) 0.0023(11) -0.0034(9) C13 0.0257(13) 0.0288(14) 0.0345(17) -0.0023(13) -0.0009(13) 0.0037(11) C14 0.0277(15) 0.0338(15) 0.0478(19) -0.0056(15) 0.0063(14) 0.0086(12) C15 0.0423(17) 0.0294(14) 0.0314(16) -0.0052(13) 0.0128(14) 0.0013(13) C16 0.0378(16) 0.0257(14) 0.0250(14) -0.0015(12) 0.0035(13) -0.0026(11) C17 0.0256(13) 0.0222(12) 0.0260(14) 0.0012(11) 0.0008(11) -0.0017(10) B3 0.0166(13) 0.0271(15) 0.0212(14) 0.0009(12) -0.0038(11) -0.0002(11) B4 0.0214(14) 0.0273(15) 0.0188(14) -0.0039(12) -0.0032(12) -0.0015(11) B5 0.0217(14) 0.0207(13) 0.0243(15) -0.0040(12) -0.0032(12) 0.0029(11) B6 0.0197(13) 0.0158(12) 0.0246(14) 0.0004(12) -0.0029(12) 0.0005(10) B7 0.0192(13) 0.0275(15) 0.0255(16) -0.0016(13) -0.0050(12) -0.0047(11) B8 0.0245(15) 0.0292(16) 0.0288(16) -0.0054(14) -0.0068(13) -0.0046(12) B9 0.0275(16) 0.0274(16) 0.0296(18) -0.0084(13) -0.0020(13) -0.0014(12) B10 0.0292(15) 0.0179(14) 0.0312(17) -0.0036(13) -0.0050(14) 0.0002(12) B11 0.0241(14) 0.0170(13) 0.0284(16) -0.0003(12) -0.0033(13) -0.0045(10) B12 0.0263(15) 0.0246(15) 0.0315(17) -0.0067(14) -0.0030(14) -0.0045(12) O1 0.0199(9) 0.0174(8) 0.0299(10) 0.0010(8) -0.0115(8) -0.0020(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C3 1.542(3) . ? C1 B5 1.703(4) . ? C1 B4 1.712(4) . ? C1 C2 1.713(3) . ? C1 B3 1.715(4) . ? C1 B6 1.728(4) . ? C2 C12 1.509(4) . ? C2 B7 1.712(4) . ? C2 B11 1.717(4) . ? C2 B3 1.730(4) . ? C2 B6 1.732(4) . ? C3 O1 1.418(3) . ? C3 C4 1.503(4) . ? C3 H3 1.0000 . ? C4 C5 1.308(4) . ? C4 H4 0.9500 . ? C5 C6 1.489(4) . ? C5 H5 0.9500 . ? C6 C7 1.385(4) . ? C6 C11 1.392(4) . ? C7 C8 1.388(5) . ? C7 H7 0.9500 . ? C8 C9 1.383(5) . ? C8 H8 0.9500 . ? C9 C10 1.381(5) . ? C9 H9 0.9500 . ? C10 C11 1.379(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.393(4) . ? C12 C17 1.400(4) . ? C13 C14 1.388(4) . ? C13 H13 0.9500 . ? C14 C15 1.388(5) . ? C14 H14 0.9500 . ? C15 C16 1.386(4) . ? C15 H15 0.9500 . ? C16 C17 1.384(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? B3 B8 1.775(4) . ? B3 B4 1.784(4) . ? B3 B7 1.786(4) . ? B3 H3A 1.1200 . ? B4 B8 1.779(4) . ? B4 B5 1.782(4) . ? B4 B9 1.785(4) . ? B4 H4A 1.1200 . ? B5 B6 1.771(4) . ? B5 B10 1.781(4) . ? B5 B9 1.784(4) . ? B5 H5A 1.1200 . ? B6 B10 1.762(4) . ? B6 B11 1.782(4) . ? B6 H6 1.1200 . ? B7 B12 1.771(4) . ? B7 B8 1.777(5) . ? B7 B11 1.782(4) . ? B7 H7A 1.1200 . ? B8 B12 1.784(5) . ? B8 B9 1.804(5) . ? B8 H8A 1.1200 . ? B9 B12 1.777(5) . ? B9 B10 1.790(5) . ? B9 H9A 1.1200 . ? B10 B11 1.781(4) . ? B10 B12 1.786(4) . ? B10 H10A 1.1200 . ? B11 B12 1.777(5) . ? B11 H11A 1.1200 . ? B12 H12 1.1200 . ? O1 H1 0.8400 . ? 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 C3 C1 B5 122.2(2) . . ? C3 C1 B4 121.2(2) . . ? B5 C1 B4 62.89(17) . . ? C3 C1 C2 117.7(2) . . ? B5 C1 C2 110.36(19) . . ? B4 C1 C2 110.63(18) . . ? C3 C1 B3 116.2(2) . . ? B5 C1 B3 114.17(19) . . ? B4 C1 B3 62.73(16) . . ? C2 C1 B3 60.61(15) . . ? C3 C1 B6 118.3(2) . . ? B5 C1 B6 62.14(17) . . ? B4 C1 B6 113.5(2) . . ? C2 C1 B6 60.44(15) . . ? B3 C1 B6 112.45(19) . . ? C12 C2 B7 120.3(2) . . ? C12 C2 C1 120.6(2) . . ? B7 C2 C1 109.47(19) . . ? C12 C2 B11 120.4(2) . . ? B7 C2 B11 62.62(17) . . ? C1 C2 B11 109.85(19) . . ? C12 C2 B3 118.0(2) . . ? B7 C2 B3 62.52(17) . . ? C1 C2 B3 59.77(15) . . ? B11 C2 B3 113.6(2) . . ? C12 C2 B6 118.9(2) . . ? B7 C2 B6 113.0(2) . . ? C1 C2 B6 60.22(15) . . ? B11 C2 B6 62.23(16) . . ? B3 C2 B6 111.6(2) . . ? O1 C3 C4 113.9(2) . . ? O1 C3 C1 107.66(19) . . ? C4 C3 C1 112.7(2) . . ? O1 C3 H3 107.4 . . ? C4 C3 H3 107.4 . . ? C1 C3 H3 107.4 . . ? C5 C4 C3 126.1(3) . . ? C5 C4 H4 117.0 . . ? C3 C4 H4 117.0 . . ? C4 C5 C6 125.9(3) . . ? C4 C5 H5 117.0 . . ? C6 C5 H5 117.0 . . ? C7 C6 C11 118.6(3) . . ? C7 C6 C5 124.3(3) . . ? C11 C6 C5 117.1(3) . . ? C6 C7 C8 120.5(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 120.4(3) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 119.3(3) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 120.3(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C6 120.9(3) . . ? C10 C11 H11 119.6 . . ? C6 C11 H11 119.6 . . ? C13 C12 C17 118.6(3) . . ? C13 C12 C2 119.3(2) . . ? C17 C12 C2 121.9(2) . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 119.9(3) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.3(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C12 120.5(3) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C1 B3 C2 59.61(15) . . ? C1 B3 B8 105.3(2) . . ? C2 B3 B8 105.4(2) . . ? C1 B3 B4 58.55(16) . . ? C2 B3 B4 106.5(2) . . ? B8 B3 B4 59.96(17) . . ? C1 B3 B7 106.0(2) . . ? C2 B3 B7 58.26(16) . . ? B8 B3 B7 59.86(18) . . ? B4 B3 B7 107.9(2) . . ? C1 B3 H3A 123.4 . . ? C2 B3 H3A 123.2 . . ? B8 B3 H3A 123.0 . . ? B4 B3 H3A 121.9 . . ? B7 B3 H3A 122.3 . . ? C1 B4 B8 105.3(2) . . ? C1 B4 B5 58.29(16) . . ? B8 B4 B5 108.3(2) . . ? C1 B4 B3 58.71(15) . . ? B8 B4 B3 59.77(17) . . ? B5 B4 B3 107.2(2) . . ? C1 B4 B9 105.1(2) . . ? B8 B4 B9 60.80(18) . . ? B5 B4 B9 60.01(17) . . ? B3 B4 B9 108.1(2) . . ? C1 B4 H4A 124.5 . . ? B8 B4 H4A 121.8 . . ? B5 B4 H4A 121.9 . . ? B3 B4 H4A 121.9 . . ? B9 B4 H4A 121.9 . . ? C1 B5 B6 59.63(16) . . ? C1 B5 B10 105.8(2) . . ? B6 B5 B10 59.48(17) . . ? C1 B5 B4 58.82(16) . . ? B6 B5 B4 108.2(2) . . ? B10 B5 B4 108.3(2) . . ? C1 B5 B9 105.6(2) . . ? B6 B5 B9 107.9(2) . . ? B10 B5 B9 60.29(18) . . ? B4 B5 B9 60.10(18) . . ? C1 B5 H5A 123.8 . . ? B6 B5 H5A 121.5 . . ? B10 B5 H5A 122.1 . . ? B4 B5 H5A 121.4 . . ? B9 B5 H5A 122.2 . . ? C1 B6 C2 59.33(15) . . ? C1 B6 B10 105.6(2) . . ? C2 B6 B10 105.8(2) . . ? C1 B6 B5 58.23(16) . . ? C2 B6 B5 106.4(2) . . ? B10 B6 B5 60.54(18) . . ? C1 B6 B11 106.2(2) . . ? C2 B6 B11 58.47(15) . . ? B10 B6 B11 60.33(17) . . ? B5 B6 B11 108.8(2) . . ? C1 B6 H6 123.6 . . ? C2 B6 H6 123.3 . . ? B10 B6 H6 122.5 . . ? B5 B6 H6 121.7 . . ? B11 B6 H6 121.8 . . ? C2 B7 B12 105.4(2) . . ? C2 B7 B8 106.0(2) . . ? B12 B7 B8 60.38(19) . . ? C2 B7 B11 58.81(15) . . ? B12 B7 B11 60.02(18) . . ? B8 B7 B11 108.7(2) . . ? C2 B7 B3 59.22(16) . . ? B12 B7 B3 107.6(2) . . ? B8 B7 B3 59.76(17) . . ? B11 B7 B3 107.9(2) . . ? C2 B7 H7A 123.9 . . ? B12 B7 H7A 122.3 . . ? B8 B7 H7A 121.7 . . ? B11 B7 H7A 121.4 . . ? B3 B7 H7A 121.8 . . ? B3 B8 B7 60.38(18) . . ? B3 B8 B4 60.27(16) . . ? B7 B8 B4 108.6(2) . . ? B3 B8 B12 107.5(2) . . ? B7 B8 B12 59.64(18) . . ? B4 B8 B12 107.4(2) . . ? B3 B8 B9 107.7(2) . . ? B7 B8 B9 107.5(2) . . ? B4 B8 B9 59.78(17) . . ? B12 B8 B9 59.37(19) . . ? B3 B8 H8A 121.6 . . ? B7 B8 H8A 121.5 . . ? B4 B8 H8A 121.6 . . ? B12 B8 H8A 122.4 . . ? B9 B8 H8A 122.2 . . ? B12 B9 B5 107.5(2) . . ? B12 B9 B4 107.4(2) . . ? B5 B9 B4 59.89(17) . . ? B12 B9 B10 60.09(19) . . ? B5 B9 B10 59.77(18) . . ? B4 B9 B10 107.7(2) . . ? B12 B9 B8 59.77(19) . . ? B5 B9 B8 107.2(2) . . ? B4 B9 B8 59.41(17) . . ? B10 B9 B8 107.7(2) . . ? B12 B9 H9A 121.9 . . ? B5 B9 H9A 122.1 . . ? B4 B9 H9A 122.1 . . ? B10 B9 H9A 121.7 . . ? B8 B9 H9A 122.2 . . ? B6 B10 B5 59.98(17) . . ? B6 B10 B11 60.41(17) . . ? B5 B10 B11 108.4(2) . . ? B6 B10 B12 107.5(2) . . ? B5 B10 B12 107.2(2) . . ? B11 B10 B12 59.77(18) . . ? B6 B10 B9 108.0(2) . . ? B5 B10 B9 59.94(18) . . ? B11 B10 B9 108.1(2) . . ? B12 B10 B9 59.59(19) . . ? B6 B10 H10A 121.7 . . ? B5 B10 H10A 121.8 . . ? B11 B10 H10A 121.4 . . ? B12 B10 H10A 122.4 . . ? B9 B10 H10A 121.8 . . ? C2 B11 B12 104.9(2) . . ? C2 B11 B10 105.6(2) . . ? B12 B11 B10 60.26(18) . . ? C2 B11 B7 58.56(16) . . ? B12 B11 B7 59.67(18) . . ? B10 B11 B7 108.0(2) . . ? C2 B11 B6 59.30(15) . . ? B12 B11 B6 107.0(2) . . ? B10 B11 B6 59.27(17) . . ? B7 B11 B6 107.4(2) . . ? C2 B11 H11A 124.0 . . ? B12 B11 H11A 122.6 . . ? B10 B11 H11A 122.1 . . ? B7 B11 H11A 121.8 . . ? B6 B11 H11A 122.1 . . ? B7 B12 B9 109.0(2) . . ? B7 B12 B11 60.30(18) . . ? B9 B12 B11 108.9(2) . . ? B7 B12 B8 59.98(18) . . ? B9 B12 B8 60.86(19) . . ? B11 B12 B8 108.6(2) . . ? B7 B12 B10 108.3(2) . . ? B9 B12 B10 60.32(18) . . ? B11 B12 B10 59.97(18) . . ? B8 B12 B10 108.7(2) . . ? B7 B12 H12 121.5 . . ? B9 B12 H12 120.9 . . ? B11 B12 H12 121.4 . . ? B8 B12 H12 121.2 . . ? B10 B12 H12 121.6 . . ? C3 O1 H1 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.550 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.056