Asymmetric Reaction of α-Diazomethylphosphonates with α-Ketoesters To Access Optically Active α-Diazo-β-hydroxyphosphonate Derivatives.
Du, Fei; Zhou, Jiao; Peng, Yungui; Organic letters  (2017) –; doi:10.1021/acs.orglett.7b00128

data_1545326
_publ_section_title
;
 Asymmetric Reaction of \a-Diazomethylphosphonates with \a-Ketoesters To
 Access Optically Active \a-Diazo-\b-hydroxyphosphonate Derivatives.
;
_journal_name_full               'Organic letters'
_journal_paper_doi               10.1021/acs.orglett.7b00128
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_sum            'C15 H20 Cl N2 O6 P'
_chemical_formula_weight         390.75
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 108.8178(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.81200(14)
_cell_length_b                   9.83567(18)
_cell_length_c                   11.24951(19)
_cell_measurement_reflns_used    7800
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.4360
_cell_measurement_theta_min      4.4370
_cell_volume                     922.90(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8335
_diffrn_reflns_point_group_measured_fraction_full 0.832
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.033
_diffrn_reflns_theta_min         5.303
_exptl_absorpt_coefficient_mu    2.958
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39955
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 1015 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.008(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2776
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+0.2517P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.586
_reflns_Friedel_fraction_full    0.657
_reflns_Friedel_fraction_max     0.665
_reflns_number_gt                2770
_reflns_number_total             2776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b00128_si_002.cif
_cod_data_source_block           pyg
_cod_database_code               1545326
_shelxl_version_number           2013-2
_shelx_res_checksum              19112
_shelx_hkl_checksum              40466