Enantioselective alkylation of beta-keto phosphonates by direct use of diaryl methanols as electrophiles
Masashi Shibata; Masahiro Ikeda; Kazuki Motoyama; Yoshihiro Miyake; Yoshiaki Nishibayashi; Chem.Commun. 48 (2012) 9528–; doi:10.1039/c2cc35262a

data_7108331
_publ_section_title
;
 Enantioselective alkylation of beta-keto phosphonates by direct use of
 diaryl methanols as electrophiles
;
_journal_name_full               Chem.Commun.
_journal_page_first              9528
_journal_paper_doi               10.1039/c2cc35262a
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H28 N O7 P'
_chemical_formula_sum            'C22 H28 N O7 P'
_chemical_formula_weight         449.44
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.0259(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   11.8192(5)
_cell_length_b                   7.6891(4)
_cell_length_c                   12.4699(5)
_cell_measurement_reflns_used    9727
_cell_measurement_temperature    183
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.13
_cell_volume                     1112.33(9)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      183
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10874
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             476.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.544
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2111 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4844
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[3.5400\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0653
_reflns_number_gt                4441
_reflns_number_total             4844
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2cc35262a.txt
_cod_data_source_block           C20H23O6P.CH3CN.H2O
_cod_original_cell_volume        1112.32(8)
_cod_database_code               7108331