Mechanistic Studies of Copper-Catalyzed Asymmetric Hydroboration of Alkenes.
Xi, Yumeng; Hartwig, John F.; Journal of the American Chemical Society 139 (2017) 12758–12772; doi:10.1021/jacs.7b07124

data_4131588
_publ_section_title
;
 Mechanistic Studies of Copper-Catalyzed Asymmetric Hydroboration of
 Alkenes.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12758
_journal_page_last               12772
_journal_paper_doi               10.1021/jacs.7b07124
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C76 H58 Cu2 O8 P4'
_chemical_formula_weight         1350.18
_chemical_name_systematic        27
_space_group.centring_type       primitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           75
_space_group_name_Hall           'P 4'
_space_group_name_H-M_alt        'P 4'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5938(4)
_cell_length_b                   21.5938(4)
_cell_length_c                   17.8485(4)
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      68.31
_cell_measurement_theta_min      42.98
_cell_volume                     8322.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
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_computing_structure_solution    SHELXT-2014
_diffrn_ambient_temperature      200(2)
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_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_refln_scan_rate          20
_diffrn_refln_scan_width         2.0
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            178733
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         68.402
_diffrn_reflns_theta_min         2.046
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    1.719
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       prism
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.858
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
; 
 Twinning involves inversion, so Flack parameter cannot be determined 
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         15250
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1058P)^2^+16.2518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2204
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                13269
_reflns_number_total             15250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07124_si_006.cif
_cod_data_source_block           27
_cod_original_cell_volume        8322.6(4)
_cod_database_code               4131588
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.919
_shelx_res_checksum              46896
_shelx_hkl_checksum              71318
_shelx_fab_checksum              53330