data_04src0562 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H50 B2' _chemical_formula_weight 528.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_hall '-P 2ybc' 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 8.2970(12) _cell_length_b 7.898(3) _cell_length_c 24.122(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.36(2) _cell_angle_gamma 90.00 _cell_volume 1579.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3410 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.061 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9951 _exptl_absorpt_correction_T_max 0.9994 _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 KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 17181 _diffrn_reflns_av_R_equivalents 0.1944 _diffrn_reflns_av_sigmaI/netI 0.2136 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3439 _reflns_number_gt 1706 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material ? _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^)+(0.0261P)^2^+2.2579P] 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 0.0134(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3439 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2552 _refine_ls_R_factor_gt 0.1406 _refine_ls_wR_factor_ref 0.1918 _refine_ls_wR_factor_gt 0.1531 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3081(4) 0.1755(4) 0.56051(16) 0.0246(9) Uani 1 1 d . . . C2 C 0.1395(4) 0.1841(5) 0.54932(16) 0.0263(9) Uani 1 1 d . . . C3 C 0.0191(4) 0.1190(5) 0.58922(16) 0.0309(10) Uani 1 1 d . . . H3A H -0.0700 0.1999 0.5914 0.046 Uiso 1 1 calc R . . H3B H 0.0718 0.1054 0.6260 0.046 Uiso 1 1 calc R . . H3C H -0.0230 0.0094 0.5762 0.046 Uiso 1 1 calc R . . C4 C 0.0791(5) 0.2582(5) 0.50045(16) 0.0281(9) Uani 1 1 d . . . H4 H -0.0344 0.2643 0.4938 0.034 Uiso 1 1 calc R . . C5 C 0.1793(5) 0.3234(5) 0.46108(16) 0.0278(9) Uani 1 1 d . . . C6 C 0.1100(5) 0.4025(5) 0.40853(16) 0.0366(11) Uani 1 1 d . . . H6A H 0.0612 0.3144 0.3847 0.055 Uiso 1 1 calc R . . H6B H 0.1962 0.4590 0.3890 0.055 Uiso 1 1 calc R . . H6C H 0.0276 0.4856 0.4177 0.055 Uiso 1 1 calc R . . C7 C 0.3454(5) 0.3138(5) 0.47235(16) 0.0291(9) Uani 1 1 d . . . H7 H 0.4163 0.3582 0.4460 0.035 Uiso 1 1 calc R . . C8 C 0.4103(4) 0.2420(5) 0.52053(16) 0.0246(9) Uani 1 1 d . . . C9 C 0.5920(4) 0.2306(5) 0.52845(17) 0.0308(10) Uani 1 1 d . . . H9A H 0.6247 0.1114 0.5294 0.046 Uiso 1 1 calc R . . H9B H 0.6261 0.2852 0.5635 0.046 Uiso 1 1 calc R . . H9C H 0.6427 0.2878 0.4976 0.046 Uiso 1 1 calc R . . C10 C 0.4915(4) 0.2029(5) 0.65660(15) 0.0233(9) Uani 1 1 d . . . C11 C 0.6438(4) 0.1415(5) 0.67672(15) 0.0261(9) Uani 1 1 d . . . C12 C 0.7016(5) -0.0370(5) 0.66675(17) 0.0335(10) Uani 1 1 d . . . H12A H 0.8158 -0.0463 0.6783 0.050 Uiso 1 1 calc R . . H12B H 0.6879 -0.0640 0.6272 0.050 Uiso 1 1 calc R . . H12C H 0.6384 -0.1165 0.6883 0.050 Uiso 1 1 calc R . . C13 C 0.7494(5) 0.2485(5) 0.70628(15) 0.0287(9) Uani 1 1 d . . . H13 H 0.8521 0.2063 0.7185 0.034 Uiso 1 1 calc R . . C14 C 0.7098(5) 0.4152(5) 0.71865(15) 0.0275(9) Uani 1 1 d . . . C15 C 0.8301(5) 0.5298(5) 0.74761(17) 0.0383(11) Uani 1 1 d . . . H15A H 0.8967 0.4642 0.7743 0.057 Uiso 1 1 calc R . . H15B H 0.7732 0.6190 0.7672 0.057 Uiso 1 1 calc R . . H15C H 0.8992 0.5813 0.7203 0.057 Uiso 1 1 calc R . . C16 C 0.5562(4) 0.4702(5) 0.70282(15) 0.0286(9) Uani 1 1 d . . . H16 H 0.5227 0.5799 0.7136 0.034 Uiso 1 1 calc R . . C17 C 0.4495(4) 0.3689(5) 0.67146(15) 0.0250(9) Uani 1 1 d . . . C18 C 0.2862(5) 0.4448(5) 0.65545(17) 0.0334(10) Uani 1 1 d . . . H18A H 0.2851 0.4816 0.6166 0.050 Uiso 1 1 calc R . . H18B H 0.2660 0.5423 0.6793 0.050 Uiso 1 1 calc R . . H18C H 0.2020 0.3596 0.6600 0.050 Uiso 1 1 calc R . . C19 C 0.3465(5) -0.0986(5) 0.62557(17) 0.0312(10) Uani 1 1 d . . . H19A H 0.4262 -0.1667 0.6066 0.047 Uiso 1 1 calc R . . H19B H 0.2380 -0.1269 0.6108 0.047 Uiso 1 1 calc R . . H19C H 0.3542 -0.1227 0.6654 0.047 Uiso 1 1 calc R . . B1 B 0.3802(5) 0.0940(6) 0.61567(19) 0.0262(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(2) 0.021(2) 0.032(2) -0.0040(17) -0.0008(17) -0.0029(16) C2 0.024(2) 0.027(2) 0.028(2) -0.0030(17) -0.0009(17) 0.0000(16) C3 0.020(2) 0.038(2) 0.034(2) 0.0004(19) 0.0003(18) -0.0013(17) C4 0.022(2) 0.033(2) 0.030(2) -0.0049(18) -0.0055(18) 0.0010(17) C5 0.029(2) 0.029(2) 0.025(2) -0.0007(18) 0.0000(18) 0.0047(18) C6 0.035(3) 0.042(3) 0.032(3) 0.002(2) -0.004(2) 0.005(2) C7 0.028(2) 0.032(2) 0.027(2) -0.0018(18) 0.0024(18) -0.0007(18) C8 0.021(2) 0.025(2) 0.028(2) -0.0036(17) -0.0007(17) -0.0026(16) C9 0.025(2) 0.032(2) 0.035(2) 0.0022(19) 0.0002(18) -0.0019(17) C10 0.022(2) 0.026(2) 0.021(2) 0.0025(16) 0.0007(16) 0.0003(16) C11 0.025(2) 0.030(2) 0.023(2) 0.0022(17) 0.0023(17) 0.0012(17) C12 0.026(2) 0.033(2) 0.041(3) -0.0008(19) -0.0068(19) 0.0032(18) C13 0.022(2) 0.038(2) 0.025(2) 0.0038(18) -0.0079(17) 0.0024(18) C14 0.024(2) 0.037(2) 0.021(2) 0.0023(18) -0.0022(17) -0.0046(18) C15 0.034(3) 0.050(3) 0.031(3) -0.005(2) -0.001(2) -0.005(2) C16 0.032(2) 0.028(2) 0.025(2) -0.0009(17) 0.0001(19) -0.0020(18) C17 0.020(2) 0.029(2) 0.026(2) 0.0047(17) -0.0015(17) -0.0012(16) C18 0.030(2) 0.029(2) 0.040(3) -0.0064(19) -0.005(2) 0.0047(18) C19 0.027(2) 0.030(2) 0.037(3) 0.0005(18) -0.0005(19) 0.0014(17) B1 0.017(2) 0.030(2) 0.032(3) -0.002(2) 0.007(2) 0.0046(18) _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 C1 C8 1.412(5) . ? C1 C2 1.415(5) . ? C1 B1 1.574(6) . ? C2 C4 1.391(5) . ? C2 C3 1.506(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.387(5) . ? C4 H4 0.9500 . ? C5 C7 1.396(5) . ? C5 C6 1.506(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.382(5) . ? C7 H7 0.9500 . ? C8 C9 1.514(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C17 1.407(5) . ? C10 C11 1.420(5) . ? C10 B1 1.578(6) . ? C11 C13 1.392(5) . ? C11 C12 1.512(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.393(5) . ? C13 H13 0.9500 . ? C14 C16 1.385(5) . ? C14 C15 1.499(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.393(5) . ? C16 H16 0.9500 . ? C17 C18 1.517(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 B1 1.567(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 C1 C2 117.9(3) . . ? C8 C1 B1 120.8(3) . . ? C2 C1 B1 121.3(3) . . ? C4 C2 C1 120.0(4) . . ? C4 C2 C3 117.4(3) . . ? C1 C2 C3 122.6(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C2 122.1(4) . . ? C5 C4 H4 118.9 . . ? C2 C4 H4 118.9 . . ? C4 C5 C7 117.5(4) . . ? C4 C5 C6 120.8(4) . . ? C7 C5 C6 121.7(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C5 122.2(4) . . ? C8 C7 H7 118.9 . . ? C5 C7 H7 118.9 . . ? C7 C8 C1 120.2(3) . . ? C7 C8 C9 118.8(3) . . ? C1 C8 C9 121.0(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C17 C10 C11 117.2(3) . . ? C17 C10 B1 121.5(3) . . ? C11 C10 B1 121.2(3) . . ? C13 C11 C10 120.0(3) . . ? C13 C11 C12 116.8(3) . . ? C10 C11 C12 123.2(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 C14 122.3(4) . . ? C11 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C16 C14 C13 117.4(4) . . ? C16 C14 C15 121.8(4) . . ? C13 C14 C15 120.8(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 C17 121.8(4) . . ? C14 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 C10 121.0(3) . . ? C16 C17 C18 116.9(3) . . ? C10 C17 C18 122.1(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? B1 C19 H19A 109.5 . . ? B1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? B1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C19 B1 C1 117.5(4) . . ? C19 B1 C10 122.5(4) . . ? C1 B1 C10 119.9(3) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.261 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.063