Cobalt-Catalyzed 1,1-Diboration of Terminal Alkynes: Scope, Mechanism, and Synthetic Applications.
Krautwald, Simon; Bezdek, Máté J; Chirik, Paul J.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b00445

data_4125603
_publ_section_title
;
 Cobalt-Catalyzed 1,1-Diboration of Terminal Alkynes: Scope, Mechanism,
 and Synthetic Applications.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b00445
_journal_year                    2017
_chemical_formula_sum            'C31 H48 B3 N O8'
_chemical_formula_weight         595.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 129.604(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4113(11)
_cell_length_b                   31.6045(17)
_cell_length_c                   15.1469(7)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.58
_cell_volume                     7897.2(7)
_computing_cell_refinement       'Bruker SAINT'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.440
_diffrn_reflns_theta_min         2.358
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS BRUKER AXS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.001
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.865
_exptl_crystal_size_mid          0.714
_exptl_crystal_size_min          0.452
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         8101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+4.5450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5743
_reflns_number_total             8101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00445_si_001.cif
_cod_data_source_block           sk2
_cod_original_cell_volume        7897.1(7)
_cod_database_code               4125603
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.969
_shelxl_version_number           2014-3
_shelx_res_checksum              81966
_shelx_hkl_checksum              86328
_shelx_fab_checksum              21842