Ruthenium-Catalyzed Regiospecific Borylation of Methyl C-H Bonds
Jaclyn M. Murphy; Joshua D. Lawrence; Kazumori Kawamura; Christopher Incarvito; John F. Hartwig; Journal of the American Chemical Society 128 (2006) 13684–13685; doi:10.1021/ja064092p

data_4110998
_publ_section_title
;
 Ruthenium-Catalyzed Regiospecific Borylation of Methyl C-H Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13684
_journal_page_last               13685
_journal_paper_doi               10.1021/ja064092p
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C28 H43 B N2 Ru2'
_chemical_formula_weight         620.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.895(3)
_cell_length_b                   14.726(3)
_cell_length_c                   12.133(2)
_cell_measurement_temperature    173(2)
_cell_volume                     2640.0(9)
_computing_cell_refinement       Denzo
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5628
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  0.9127
_exptl_absorpt_correction_T_min  0.8449
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       blade
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                2202
_reflns_number_total             3248
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064092psi20060609_094941.cif
_cod_data_source_block           Compound8b
_cod_original_cell_volume        2639.9(9)
_cod_database_code               4110998