Site-Selective and Stereoselective trans-Hydroboration of 1,3-Enynes Catalyzed by 1,4-Azaborine-Based Phosphine-Pd Complex.
Xu, Senmiao; Zhang, Yuanzhe; Li, Bo; Liu, Shih-Yuan; Journal of the American Chemical Society 138 (2016) 14566–14569; doi:10.1021/jacs.6b09759

data_4125301
_publ_section_title
;
 Site-Selective and Stereoselective trans-Hydroboration of 1,3-Enynes
 Catalyzed by 1,4-Azaborine-Based Phosphine-Pd Complex.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14566
_journal_page_last               14569
_journal_paper_doi               10.1021/jacs.6b09759
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C47 H43 B N O P Pd, C7 H8'
_chemical_formula_sum            'C54 H51 B N O P Pd'
_chemical_formula_weight         878.14
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                85.720(3)
_cell_angle_beta                 89.462(3)
_cell_angle_gamma                87.941(4)
_cell_formula_units_Z            4
_cell_length_a                   12.0431(9)
_cell_length_b                   15.5970(12)
_cell_length_c                   23.7704(17)
_cell_measurement_reflns_used    9370
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.70
_cell_measurement_theta_min      5.01
_cell_volume                     4449.5(6)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa DUO CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15665
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.771
_diffrn_reflns_theta_min         2.843
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\uS'
_exptl_absorpt_coefficient_mu    3.999
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. (2013). SADABS. Bruker AXS Inc. Madison, WI USA.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.032
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       na
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1137
_refine_ls_number_reflns         15665
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1224P)^2^+1.2194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13346
_reflns_number_total             15665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b09759_si_006.cif
_cod_data_source_block           C47H43BNOPPd(C7H8)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4125298--4125302.cif.
;
_cod_database_code               4125301
_shelx_estimated_absorpt_t_min   0.473
_shelx_estimated_absorpt_t_max   0.825
_shelxl_version_number           2014-3
_shelx_res_checksum              39317
_shelx_hkl_checksum              152