C-N and C-P bond formation via cross dehydrative coupling reaction: an efficient synthesis of novel 3,4-dihydroquinazolines
Reddy, Kallu Rajender; Saidulu, G.; Kumar, R. Arun; Anitha, T.; Srinivasulu, A.; Balasubramanian, Sridhar; Liu, Shiuh-Tzung; RSC Adv.  (2014) –; doi:10.1039/C4RA10203G

data_7218444
_publ_section_title
;
 C-N and C-P bond formation via cross dehydrative coupling reaction: an
 efficient synthesis of novel 3,4-dihydroquinazolines
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA10203G
_journal_year                    2014
_chemical_formula_moiety         'C26 H29 N2 O3 P'
_chemical_formula_sum            'C26 H29 N2 O3 P'
_chemical_formula_weight         448.48
_chemical_name_systematic
; 
dimethyl 2-(4-tert-butylphenyl)-3-phenyl-3,4-dihydroquinazolin-4-yl                    
phosphonate
;
_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                 103.257(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6985(13)
_cell_length_b                   11.7586(10)
_cell_length_c                   13.8686(12)
_cell_measurement_reflns_used    5926
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      2.24
_cell_volume                     2333.1(4)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\w scan'
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22035
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0517P)^2^+0.8099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                3707
_reflns_number_total             4110
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4ra10203g2.cif
_cod_data_source_block           av30
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7218444