A diastereo- and enantioselective synthesis of alpha-substituted anti-alpha,beta-diaminophosphonic acid derivatives.
Wilt, Jeremy C; Pink, Maren; Johnston, Jeffrey N; Chemical communications (Cambridge, England)  (2008) 4177–4179; doi:10.1039/b808393b

data_7103342
_publ_section_title
;
 A diastereo- and enantioselective synthesis of alpha-substituted
 anti-alpha,beta-diaminophosphonic acid derivatives.
;
_journal_issue                   35
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4177
_journal_page_last               4179
_journal_paper_doi               10.1039/b808393b
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H53 N2 O7 P S, C29 H51 N2 O7 P S'
_chemical_formula_sum            'C63 H104 N4 O14 P2 S2'
_chemical_formula_weight         1267.56
_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                 96.3790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.1975(7)
_cell_length_b                   13.6185(7)
_cell_length_c                   18.9091(10)
_cell_measurement_reflns_used    5638
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.3
_cell_volume                     3633.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003)'
_computing_publication_material  'SHELXTL (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'0.30 degree frames measured for 30 second each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       \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  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49900
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.9791
_exptl_absorpt_correction_T_min  0.9656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         14767
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+1.9887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                12538
_reflns_number_total             14767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b808393b.txt
_cod_data_source_block           07083_1
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7103342