A concise synthesis of 4-imino-3,4-dihydroquinazolin-2-ylphosphonates via a palladium-catalyzed reaction of carbodiimide, isocyanide, and phosphite.
Qiu, Guanyinsheng; Lu, Yuan; Wu, Jie; Organic & biomolecular chemistry 11 (2013) 798–802; doi:10.1039/c2ob26979a

data_7152786
_publ_section_title
;
 A concise synthesis of 4-imino-3,4-dihydroquinazolin-2-ylphosphonates via
 a palladium-catalyzed reaction of carbodiimide, isocyanide, and
 phosphite.
;
_journal_issue                   5
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              798
_journal_page_last               802
_journal_paper_doi               10.1039/c2ob26979a
_journal_volume                  11
_journal_year                    2013
_chemical_formula_sum            'C22 H25 Cl2 I N3 O3 P'
_chemical_formula_weight         608.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.576(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.266(14)
_cell_length_b                   8.920(7)
_cell_length_c                   16.576(13)
_cell_measurement_reflns_used    855
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.842
_cell_measurement_theta_min      2.575
_cell_volume                     2531(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10089
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.568
_exptl_absorpt_correction_T_max  0.9257
_exptl_absorpt_correction_T_min  0.7444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4452
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                3034
_reflns_number_total             4452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ob26979a.txt
_cod_data_source_block           a20905a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7152786