Enzymatic Resolution of Chiral Phosphinate Esters
Yingchun Li; Sarah D. Aubert; Eugene G. Maes; Frank M. Raushel; Journal of the American Chemical Society 126 (2004) 8888–8889; doi:10.1021/ja048457m

data_4112781
_publ_section_title
;
 Enzymatic Resolution of Chiral Phosphinate Esters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8888
_journal_page_last               8889
_journal_paper_doi               10.1021/ja048457m
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C19 H30 N O6 P'
_chemical_formula_weight         399.41
_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                 92.51(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.758(6)
_cell_length_b                   19.684(19)
_cell_length_c                   8.544(8)
_cell_measurement_reflns_used    711
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      35.84
_cell_measurement_theta_min      4.49
_cell_volume                     967.5(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'MWPC area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1264
_diffrn_reflns_av_sigmaI/netI    0.1902
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6249
_diffrn_reflns_theta_full        60.65
_diffrn_reflns_theta_max         60.65
_diffrn_reflns_theta_min         4.49
_exptl_absorpt_coefficient_mu    1.572
_exptl_absorpt_correction_T_max  0.9845
_exptl_absorpt_correction_T_min  0.7439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2680
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0489P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                1477
_reflns_number_total             2680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048457mrom20040323_044233.cif
_cod_data_source_block           fr10
_cod_database_code               4112781