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        'φ and ω 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 F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0261P)²+2.2579P] where P=(Fo²+2Fc²)/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+0.001xFc²λ³/sin(2θ)]^-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 . . .
 
 
_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
