Catalytic Dehydrogenative Borylation of Terminal Alkynes by a SiNN Pincer Complex of Iridium
Chun-I Lee; Jia Zhou; Oleg V. Ozerov; Journal of the American Chemical Society 135 (2013) 3560–3566; doi:10.1021/ja311682c

data_4119408
_publ_section_title
;
 Catalytic Dehydrogenative Borylation of Terminal Alkynes by a SiNN Pincer
 Complex of Iridium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3560
_journal_page_last               3566
_journal_paper_doi               10.1021/ja311682c
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C35 H52 B2 Ir N2 O4 Si'
_chemical_formula_sum            'C35 H52 B2 Ir N2 O4 Si'
_chemical_formula_weight         806.70
_chemical_name_common            (SiNN)Ir(H)(Bpin)2
_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                 118.485(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.991(5)
_cell_length_b                   19.990(5)
_cell_length_c                   20.615(5)
_cell_measurement_reflns_used    957
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      117.658
_cell_measurement_theta_min      5.952
_cell_volume                     9052(4)
_computing_cell_refinement
'CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003)'
_computing_data_collection       'FRAMBO (BRUKER-NONIUS, 2003)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'BRUKER GADDS D8 Discover'
_diffrn_measurement_method       'phi and omega 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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33219
_diffrn_reflns_theta_full        59.89
_diffrn_reflns_theta_max         59.89
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.204
_exptl_absorpt_correction_T_max  0.7072
_exptl_absorpt_correction_T_min  0.4014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_platon_squeeze_details          ' '
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                5031
_reflns_number_total             6663
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja311682c_si_002.cif
_cod_data_source_block           oz345
_cod_database_code               4119408