P-Stereogenic β-Aminophosphines: Preparation and Applications in Enantioselective Organocatalysis.
Su, Hsin Y.; Taylor, Mark S.; The Journal of organic chemistry 82 (2017) 3173–3182; doi:10.1021/acs.joc.7b00199

data_4037476
_publ_section_title
;
 P-Stereogenic \b-Aminophosphines: Preparation and Applications in
 Enantioselective Organocatalysis.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3173
_journal_page_last               3182
_journal_paper_doi               10.1021/acs.joc.7b00199
_journal_volume                  82
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C26 H33 B N3 O4 P, C H4 O'
_chemical_formula_sum            'C27 H37 B N3 O5 P'
_chemical_formula_weight         525.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.119(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8893(5)
_cell_length_b                   6.8939(3)
_cell_length_c                   15.5331(6)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      66.84
_cell_measurement_theta_min      2.99
_cell_volume                     1413.56(10)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21317
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.244
_diffrn_reflns_theta_max         67.244
_diffrn_reflns_theta_min         2.993
_diffrn_source                   'Bruker ImuS with multi-layer optics'
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.5678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       needle
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.06(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         4862
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.1743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.833
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                4662
_reflns_number_total             4862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b00199_si_003.cif
_cod_data_source_block           d1631_a
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4037476
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.702
_shelx_estimated_absorpt_t_max   0.890
_shelx_res_checksum              84093
_shelx_hkl_checksum              5842