The copper-catalysed Suzuki-Miyaura coupling of alkylboron reagents: disproportionation of anionic (alkyl)(alkoxy)borates to anionic dialkylborates prior to transmetalation.
Basnet, Prakash; Thapa, Surendra; Dickie, Diane A.; Giri, Ramesh; Chemical communications (Cambridge, England) 52 (2016) 11072–11075; doi:10.1039/c6cc05114f

data_7124850
_publ_section_title
;
 The copper-catalysed Suzuki-Miyaura coupling of alkylboron reagents:
 disproportionation of anionic (alkyl)(alkoxy)borates to anionic
 dialkylborates prior to transmetalation.
;
_journal_issue                   74
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11072
_journal_page_last               11075
_journal_paper_doi               10.1039/c6cc05114f
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C32 H64 B Li O8'
_chemical_formula_weight         594.58
_chemical_name_common            PB-3-33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2016-07-28 deposited with the CCDC.
2016-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.676(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6111(3)
_cell_length_b                   22.4729(6)
_cell_length_c                   14.5760(4)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    99.(2)
_cell_measurement_theta_max      27.4545
_cell_measurement_theta_min      2.2896
_cell_volume                     3472.03(17)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2014.5.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/4'
_diffrn_ambient_temperature      99.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33894
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.67
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.841
_exptl_crystal_size_mid          0.315
_exptl_crystal_size_min          0.216
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+1.7313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                6511
_reflns_number_total             7967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05114f2.cif
_cod_data_source_block           41
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7124850
_shelx_res_checksum              5384