Mannich type reactions of chlorophosphites, phosphoramides and aldehydes (ketones) under solvent-free and catalyst-free conditions—synthesis of N-phosphoramino α-aminophosphonates
Zhang, Jianfeng; Cui, Zhanwei; Wang, Fei; Wang, Yadan; Miao, Zhiwei; Chen, Ruyu; Green Chemistry 9 (2007) 1341–; doi:10.1039/b710008f

data_7203081
_publ_section_title
;
 Mannich type reactions of chlorophosphites, phosphoramides and
 aldehydes (ketones) under solvent-free and catalyst-free
 conditions---synthesis of N-phosphoramino \a-aminophosphonates
;
_journal_issue                   12
_journal_name_full               'Green Chemistry'
_journal_page_first              1341
_journal_paper_doi               10.1039/b710008f
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C16 H27 N O7 P2'
_chemical_formula_sum            'C16 H27 N O7 P2'
_chemical_formula_weight         407.33
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.689(9)
_cell_angle_beta                 98.771(7)
_cell_angle_gamma                111.382(16)
_cell_formula_units_Z            2
_cell_length_a                   9.955(9)
_cell_length_b                   10.404(9)
_cell_length_c                   10.839(9)
_cell_measurement_reflns_used    2306
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.6
_cell_volume                     1011.0(15)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10348
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.9802
_exptl_absorpt_correction_T_min  0.9657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3551
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0632P)^2^+0.2781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                2931
_reflns_number_total             3551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b710008f.txt
_cod_data_source_block           shelxl
_cod_database_code               7203081