Facile synthetic approach towards vasorelaxant active 4-hydroxyquinazoline-4-carboxamides
Aziz, Marian N.; Panda, Siva S.; Shalaby, ElSayed M.; Fawzy, Nehmedo G.; Girgis, Adel S.; RSC Advances 9 (2019) 28534–; doi:10.1039/C9RA04321G

data_7233766
_publ_section_title
;
 Facile synthetic approach towards vasorelaxant active
 4-hydroxyquinazoline-4-carboxamides
;
_journal_issue                   49
_journal_name_full               'RSC Advances'
_journal_page_first              28534
_journal_paper_doi               10.1039/C9RA04321G
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C20 H21 N3 O3'
_chemical_formula_sum            'C20 H21 N3 O3'
_chemical_formula_weight         351.40
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2019-04-30 deposited with the CCDC.    2019-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.61(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.500(4)
_cell_length_b                   13.189(3)
_cell_length_c                   17.709(4)
_cell_measurement_reflns_used    3528
_cell_measurement_temperature    293
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     3621.9(17)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67134
_diffrn_reflns_theta_full        30.002
_diffrn_reflns_theta_max         30.002
_diffrn_reflns_theta_min         1.332
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1487.990
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.29
_refine_ls_extinction_coef       1390(100)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.1752
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         10075
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.0011638
_refine_ls_shift/su_mean         0.0001067
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 24.1 38.2 19.0 4.82 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1108
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1098
_reflns_limit_h_max              22
_reflns_limit_h_min              -24
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                10075
_reflns_number_total             11051
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0448
_oxford_refine_ls_scale          0.3086(3)
_oxford_reflns_number_all        10979
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_publcif_datablock.id            {16cb9ecb-ca83-4623-9238-3e69c64c76fd}
_cod_data_source_file            c9ra04321g2.cif
_cod_data_source_block           9PK
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7233766