Preparation of Dihydroborole Derivatives by a Simple 1,1-Carboboration Route
Feldmann, Andreas; Iida, Azusa; Fröhlich, Roland; Yamaguchi, Shigehiro; Kehr, Gerald; Erker, Gerhard; Organometallics 31 (2012) 2445–; doi:10.1021/om300065m

data_4076586
_publ_section_title
;
 Preparation of Dihydroborole Derivatives by a Simple 1,1-Carboboration
 Route
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              2445
_journal_paper_doi               10.1021/om300065m
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C35 H35 B F15 P'
_chemical_formula_weight         782.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'at P and B from difmap, others geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.714(12)
_cell_angle_beta                 75.686(9)
_cell_angle_gamma                72.078(8)
_cell_formula_units_Z            2
_cell_length_a                   9.9747(8)
_cell_length_b                   12.2460(13)
_cell_length_c                   16.1369(17)
_cell_measurement_reflns_used    6352
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.52
_cell_measurement_theta_min      0.88
_cell_volume                     1815.9(3)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19519
_diffrn_reflns_theta_full        67.16
_diffrn_reflns_theta_max         67.16
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    1.604
_exptl_absorpt_correction_T_max  0.7722
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.307
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6210
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1318P)^2^+1.7872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2216
_refine_ls_wR_factor_ref         0.2288
_reflns_number_gt                5596
_reflns_number_total             6210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300065m_si_003.cif
_cod_data_source_block           erk5796
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076586