Determination of the absolute configuration of phosphinic analogues of glutamate.
Commare, Bruno; Rigault, Delphine; Lemasson, Isabelle A.; Deschamps, Patrick; Tomas, Alain; Roussel, Pascal; Brabet, Isabelle; Goudet, Cyril; Pin, Jean-Philippe; Leroux, Frédéric R; Colobert, Françoise; Acher, Francine C.; Organic & biomolecular chemistry 13 (2015) 1106–1112; doi:10.1039/c4ob01960a

data_7154194
_publ_section_title
;
 Determination of the absolute configuration of phosphinic analogues of
 glutamate.
;
_journal_issue                   4
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1106
_journal_page_last               1112
_journal_paper_doi               10.1039/c4ob01960a
_journal_volume                  13
_journal_year                    2015
_chemical_formula_sum            'C15 H19 N2 O5 P'
_chemical_formula_weight         338.29
_chemical_name_common            hydroxy(3-nitrophenyl)methyl)phosphinate
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.390(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2471(6)
_cell_length_b                   5.6271(3)
_cell_length_c                   13.2223(6)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     842.53(7)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006) '
_computing_data_collection       'Apex2 (Bruker AXS, 2006) '
_computing_data_reduction        'Apex2 (Bruker AXS, 2006) '
_computing_molecular_graphics    'ORTEP(III) '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0330
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46232
_diffrn_reflns_theta_full        28.73
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens,1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4377
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                3394
_reflns_number_total             4377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ob01960a2.cif
_cod_data_source_block           Commare1
_cod_depositor_comments          'Adding full bibliography for 7154194.cif.'
_cod_original_sg_symbol_H-M      'P 21 '
_cod_database_code               7154194