data_Compound13 _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C12 H30 B2 P2' _chemical_formula_sum 'C12 H30 B2 P2' _chemical_formula_weight 257.92 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5693(13) _cell_length_b 11.154(2) _cell_length_c 11.224(2) _cell_angle_alpha 86.73(3) _cell_angle_beta 81.82(3) _cell_angle_gamma 89.08(3) _cell_volume 812.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3601 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 284 _exptl_absorpt_coefficient_mu 0.244 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9363 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD' _diffrn_reflns_number 6562 _diffrn_reflns_av_R_equivalents 0.0156 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 5.16 _diffrn_reflns_theta_max 27.45 _reflns_number_total 3691 _reflns_number_gt 3115 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _refine_special_details ; All hydrogen atoms attached to phosphorus and boron atoms were located in the difference map and fully refined. 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^)+(0.0371P)^2^+0.2963P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3691 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.81988(6) 0.67048(3) 0.90943(3) 0.02690(11) Uani 1 1 d . . . H1A H 0.906(3) 0.6313(16) 1.0033(16) 0.046(5) Uiso 1 1 d . . . H1B H 0.712(3) 0.5806(15) 0.8938(15) 0.041(5) Uiso 1 1 d . . . C1 C 1.0266(2) 0.67123(12) 0.78290(12) 0.0245(3) Uani 1 1 d . . . H1 H 1.1143 0.7426 0.7882 0.029 Uiso 1 1 calc R . . C2 C 1.1639(2) 0.55898(14) 0.78717(13) 0.0315(3) Uani 1 1 d . . . H2A H 1.2230 0.5537 0.8637 0.038 Uiso 1 1 calc R . . H2B H 1.0803 0.4864 0.7844 0.038 Uiso 1 1 calc R . . C3 C 1.3370(2) 0.56414(16) 0.68097(14) 0.0379(4) Uani 1 1 d . . . H3A H 1.4281 0.6324 0.6883 0.045 Uiso 1 1 calc R . . H3B H 1.4200 0.4894 0.6827 0.045 Uiso 1 1 calc R . . C4 C 1.2526(3) 0.57895(15) 0.56167(13) 0.0379(4) Uani 1 1 d . . . H4A H 1.3684 0.5868 0.4949 0.046 Uiso 1 1 calc R . . H4B H 1.1743 0.5064 0.5503 0.046 Uiso 1 1 calc R . . C5 C 1.1132(2) 0.68866(15) 0.55711(13) 0.0361(4) Uani 1 1 d . . . H5A H 1.0536 0.6922 0.4808 0.043 Uiso 1 1 calc R . . H5B H 1.1955 0.7620 0.5583 0.043 Uiso 1 1 calc R . . C6 C 0.9394(2) 0.68551(14) 0.66347(12) 0.0309(3) Uani 1 1 d . . . H6A H 0.8469 0.6177 0.6571 0.037 Uiso 1 1 calc R . . H6B H 0.8578 0.7608 0.6611 0.037 Uiso 1 1 calc R . . B1 B 0.6740(3) 0.82114(16) 0.92656(16) 0.0355(4) Uani 1 1 d . . . H1C H 0.798(3) 0.8903(17) 0.9161(16) 0.049(5) Uiso 1 1 d . . . H1D H 0.577(3) 0.8294(18) 0.8563(18) 0.061(6) Uiso 1 1 d . . . P2 P 0.50102(6) 0.81492(3) 1.08177(3) 0.02713(11) Uani 1 1 d . . . H2 H 0.393(3) 0.9209(15) 1.0868(15) 0.037(4) Uiso 1 1 d . . . C7 C 0.6553(2) 0.82646(12) 1.20474(12) 0.0260(3) Uani 1 1 d . . . H7 H 0.7404 0.7515 1.2074 0.031 Uiso 1 1 calc R . . C8 C 0.5165(2) 0.82967(15) 1.32624(13) 0.0340(3) Uani 1 1 d . . . H8A H 0.4293 0.9029 1.3271 0.041 Uiso 1 1 calc R . . H8B H 0.4248 0.7591 1.3370 0.041 Uiso 1 1 calc R . . C9 C 0.6432(2) 0.82880(16) 1.42976(14) 0.0383(4) Uani 1 1 d . . . H9A H 0.5500 0.8346 1.5067 0.046 Uiso 1 1 calc R . . H9B H 0.7202 0.7520 1.4336 0.046 Uiso 1 1 calc R . . C10 C 0.7934(3) 0.93253(15) 1.41402(15) 0.0415(4) Uani 1 1 d . . . H10A H 0.7159 1.0093 1.4207 0.050 Uiso 1 1 calc R . . H10B H 0.8806 0.9260 1.4792 0.050 Uiso 1 1 calc R . . C11 C 0.9291(3) 0.93320(17) 1.29320(16) 0.0440(4) Uani 1 1 d . . . H11A H 1.0209 0.8619 1.2913 0.053 Uiso 1 1 calc R . . H11B H 1.0164 1.0056 1.2834 0.053 Uiso 1 1 calc R . . C12 C 0.8045(3) 0.93233(16) 1.18836(15) 0.0415(4) Uani 1 1 d . . . H12A H 0.8991 0.9263 1.1119 0.050 Uiso 1 1 calc R . . H12B H 0.7261 1.0086 1.1834 0.050 Uiso 1 1 calc R . . B2 B 0.3275(3) 0.67558(18) 1.10904(19) 0.0406(4) Uani 1 1 d . . . H2C H 0.244(4) 0.675(2) 1.028(2) 0.080(7) Uiso 1 1 d . . . H2D H 0.440(3) 0.599(2) 1.1097(19) 0.067(6) Uiso 1 1 d . . . H2E H 0.215(3) 0.6749(18) 1.1982(18) 0.060(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0285(2) 0.0264(2) 0.02387(19) -0.00090(13) 0.00244(14) 0.00298(14) C1 0.0226(6) 0.0254(7) 0.0247(6) -0.0021(5) -0.0007(5) 0.0003(5) C2 0.0311(7) 0.0354(8) 0.0271(7) 0.0002(6) -0.0028(6) 0.0089(6) C3 0.0295(8) 0.0475(9) 0.0341(8) -0.0011(7) 0.0020(6) 0.0143(7) C4 0.0372(8) 0.0462(9) 0.0273(7) -0.0032(6) 0.0050(6) 0.0117(7) C5 0.0346(8) 0.0456(9) 0.0249(7) 0.0038(6) 0.0037(6) 0.0091(7) C6 0.0263(7) 0.0401(8) 0.0248(7) 0.0003(6) -0.0003(6) 0.0068(6) B1 0.0428(10) 0.0320(9) 0.0283(8) 0.0008(7) 0.0039(7) 0.0117(8) P2 0.0267(2) 0.0272(2) 0.02655(19) -0.00385(14) -0.00030(14) 0.00445(14) C7 0.0226(7) 0.0252(7) 0.0290(7) -0.0012(5) 0.0008(5) 0.0009(5) C8 0.0248(7) 0.0483(9) 0.0282(7) -0.0044(6) 0.0001(6) -0.0063(6) C9 0.0320(8) 0.0540(10) 0.0286(8) -0.0045(7) -0.0020(6) -0.0071(7) C10 0.0402(9) 0.0431(9) 0.0448(9) -0.0106(7) -0.0148(7) -0.0030(7) C11 0.0338(8) 0.0487(10) 0.0506(10) 0.0021(8) -0.0093(7) -0.0178(7) C12 0.0365(9) 0.0461(9) 0.0410(9) 0.0073(7) -0.0047(7) -0.0169(7) B2 0.0352(10) 0.0432(11) 0.0439(10) -0.0132(8) -0.0024(8) -0.0079(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.8195(15) . ? P1 B1 1.9267(18) . ? P1 H1A 1.316(18) . ? P1 H1B 1.271(17) . ? C1 C6 1.5303(19) . ? C1 C2 1.534(2) . ? C1 H1 1.0000 . ? C2 C3 1.525(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.520(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.520(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.529(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? B1 P2 1.9381(18) . ? B1 H1C 1.119(19) . ? B1 H1D 1.08(2) . ? P2 C7 1.8360(15) . ? P2 B2 1.926(2) . ? P2 H2 1.370(16) . ? C7 C8 1.531(2) . ? C7 C12 1.533(2) . ? C7 H7 1.0000 . ? C8 C9 1.522(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.519(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.513(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.526(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? B2 H2C 1.12(2) . ? B2 H2D 1.12(2) . ? B2 H2E 1.16(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 B1 114.05(8) . . ? C1 P1 H1A 104.9(8) . . ? B1 P1 H1A 115.3(8) . . ? C1 P1 H1B 103.8(8) . . ? B1 P1 H1B 115.8(8) . . ? H1A P1 H1B 101.3(11) . . ? C6 C1 C2 111.15(12) . . ? C6 C1 P1 110.47(9) . . ? C2 C1 P1 112.04(10) . . ? C6 C1 H1 107.7 . . ? C2 C1 H1 107.7 . . ? P1 C1 H1 107.7 . . ? C3 C2 C1 110.37(12) . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 111.23(13) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 111.58(13) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 111.61(13) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C1 110.52(12) . . ? C5 C6 H6A 109.5 . . ? C1 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? P1 B1 P2 108.34(9) . . ? P1 B1 H1C 104.5(10) . . ? P2 B1 H1C 114.5(10) . . ? P1 B1 H1D 107.1(11) . . ? P2 B1 H1D 108.7(11) . . ? H1C B1 H1D 113.2(14) . . ? C7 P2 B2 110.87(8) . . ? C7 P2 B1 111.01(8) . . ? B2 P2 B1 113.32(9) . . ? C7 P2 H2 101.8(7) . . ? B2 P2 H2 113.1(7) . . ? B1 P2 H2 106.1(7) . . ? C8 C7 C12 110.28(13) . . ? C8 C7 P2 110.67(10) . . ? C12 C7 P2 114.58(10) . . ? C8 C7 H7 107.0 . . ? C12 C7 H7 107.0 . . ? P2 C7 H7 107.0 . . ? C9 C8 C7 111.09(12) . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 111.28(14) . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.49(13) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 112.28(14) . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C7 110.90(13) . . ? C11 C12 H12A 109.5 . . ? C7 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 108.0 . . ? P2 B2 H2C 105.2(12) . . ? P2 B2 H2D 103.5(11) . . ? H2C B2 H2D 111.1(17) . . ? P2 B2 H2E 113.7(10) . . ? H2C B2 H2E 111.8(16) . . ? H2D B2 H2E 111.1(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 P1 C1 C6 -66.60(13) . . . . ? B1 P1 C1 C2 168.89(11) . . . . ? C6 C1 C2 C3 56.84(16) . . . . ? P1 C1 C2 C3 -179.03(10) . . . . ? C1 C2 C3 C4 -56.27(18) . . . . ? C2 C3 C4 C5 55.66(19) . . . . ? C3 C4 C5 C6 -55.05(19) . . . . ? C4 C5 C6 C1 55.06(18) . . . . ? C2 C1 C6 C5 -56.10(16) . . . . ? P1 C1 C6 C5 178.87(10) . . . . ? C1 P1 B1 P2 -168.40(8) . . . . ? P1 B1 P2 C7 73.51(11) . . . . ? P1 B1 P2 B2 -52.02(13) . . . . ? B2 P2 C7 C8 -56.77(13) . . . . ? B1 P2 C7 C8 176.34(10) . . . . ? B2 P2 C7 C12 177.78(12) . . . . ? B1 P2 C7 C12 50.89(13) . . . . ? C12 C7 C8 C9 -56.86(17) . . . . ? P2 C7 C8 C9 175.30(11) . . . . ? C7 C8 C9 C10 56.51(18) . . . . ? C8 C9 C10 C11 -54.73(19) . . . . ? C9 C10 C11 C12 54.1(2) . . . . ? C10 C11 C12 C7 -54.7(2) . . . . ? C8 C7 C12 C11 55.57(18) . . . . ? P2 C7 C12 C11 -178.78(12) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.717 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.041 _vrf_PLAT094_Compound13 ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... 2.71 RESPONSE: Found no likely candidates for solvent molecules in voids. ;