Novel Three-Component Route to Diastereoselective Synthesis of Trisubstituted Vinylphosphonates Using Phosphites, Acetylenic Esters, and Aroyl Chlorides
Rostamnia, Sadegh; Alizadeh, Abdolali; Zhu, Long-Guan; Journal of Combinatorial Chemistry 11 (2009) 143–; doi:10.1021/cc800128j

data_1503634
_publ_section_title
;
 Novel Three-Component Route to Diastereoselective Synthesis of
 Trisubstituted Vinylphosphonates Using Phosphites, Acetylenic Esters, and
 Aroyl Chlorides
;
_journal_issue                   1
_journal_name_full               'Journal of Combinatorial Chemistry'
_journal_page_first              143
_journal_paper_doi               10.1021/cc800128j
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C15 H16 N O10 P'
_chemical_formula_weight         401.26
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.6700(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1421(10)
_cell_length_b                   20.355(2)
_cell_length_c                   9.6776(10)
_cell_measurement_temperature    295(2)
_cell_volume                     1800.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13362
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.9402
_exptl_absorpt_correction_T_min  0.9122
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.4356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                2735
_reflns_number_total             3340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cc800128j_si_002.cif
_cod_data_source_block           dau11
_cod_database_code               1503634