Synthesis, crystal structure and in silico studies of novel 2,4-dimethoxy-tetrahydropyrimido[4,5-b]quinolin-6(7H)-ones
Patel, Subham G.; Vala, Ruturajsinh M.; Patel, Paras J.; Upadhyay, Dipti B.; Ramkumar, V.; Gardas, Ramesh L.; Patel, Hitendra M.; RSC Advances 12 (2022) 18806–18820; doi:10.1039/D2RA02694E

data_7245127
_publ_section_title
;
 Synthesis, crystal structure and in silico studies of novel
 2,4-dimethoxy-tetrahydropyrimido[4,5-b]quinolin-6(7H)-ones
;
_journal_issue                   29
_journal_name_full               'RSC Advances'
_journal_page_first              18806
_journal_page_last               18820
_journal_paper_doi               10.1039/D2RA02694E
_journal_volume                  12
_journal_year                    2022
_chemical_compound_source        NIL
_chemical_formula_sum            'C21 H22 Cl N3 O3'
_chemical_formula_weight         399.86
_chemical_melting_point          209.0(10)
_chemical_name_systematic
5-(4-chlorophenyl)-2,4-dimethoxy-8,8-dimethyl-5,8,9,10-tetrahydropyrimido[4,5-b]quinolin-6(7H)-one
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-01-08 deposited with the CCDC.	2022-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                74.018(10)
_cell_angle_beta                 83.479(15)
_cell_angle_gamma                76.619(15)
_cell_formula_units_Z            2
_cell_length_a                   6.1119(17)
_cell_length_b                   12.856(3)
_cell_length_c                   13.503(2)
_cell_measurement_reflns_used    1693
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.58
_cell_volume                     990.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.684
_diffrn_measured_fraction_theta_max 0.684
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.684
_diffrn_reflns_Laue_measured_fraction_max 0.684
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4723
_diffrn_reflns_point_group_measured_fraction_full 0.684
_diffrn_reflns_point_group_measured_fraction_max 0.684
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.571
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             420
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol and Dichloromethane'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         2395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+1.2597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.2058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1393
_reflns_number_total             2395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra02694e2.cif
_cod_data_source_block           101
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '208-210' was changed to
'209.0(10)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        990.8(4)
_cod_database_code               7245127
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.966
_shelx_res_checksum              14922