Iridium-catalyzed triple C(sp3)-H borylations: construction of triborylated sp3-carbon centers
Tsuyoshi Mita; Yuto Ikeda; Kenichi Michigami; Yoshihiro Sato; Chem.Commun. 49 (2013) 5601–; doi:10.1039/c3cc42675k

data_7109381
_publ_section_title
;
 Iridium-catalyzed triple C(sp3)-H borylations: construction of
 triborylated sp3-carbon centers
;
_journal_name_full               Chem.Commun.
_journal_page_first              5601
_journal_paper_doi               10.1039/c3cc42675k
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C25 H42 B3 N O6'
_chemical_formula_sum            'C25 H42 B3 N O6'
_chemical_formula_weight         485.04
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 107.583(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.5820(3)
_cell_length_b                   10.16276(18)
_cell_length_c                   16.1577(3)
_cell_measurement_reflns_used    39971
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.16
_cell_measurement_theta_min      3.26
_cell_volume                     2752.20(15)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2011)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44334
_diffrn_reflns_theta_full        68.20
_diffrn_reflns_theta_max         68.20
_diffrn_reflns_theta_min         5.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048.00
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5015
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0513P)^2^+1.0259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                4823
_reflns_number_total             5015
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3cc42675k.txt
_cod_data_source_block           SX037
_cod_original_cell_volume        2752.20(14)
_cod_database_code               7109381