Synthesis, crystal structure at 219K and Hirshfeld surface analyses of 1,4,6-trimethylquinoxaline-2,3(1<i>H</i>,4<i>H</i>)-dione monohydrate
Zouitini, Ayman; Faizi, Md. Serajul Haque; Ouzidan, Younes; Ouazzani Chahdi, Fouad; Marrot, Jérôme; Prim, Damien; Dege, Necmi; Mashrai, Ashraf; Acta Crystallographica Section E 76 (2020) 1296–1301; doi:10.1107/S2056989020009573

data_2243491
_publ_contact_author
;
Faculity of Pharmacy, University of Science and Technology, Ibb Branch,
Ibb, Yemen
;
_publ_section_title
;
 Synthesis, crystal structure at 219K and Hirshfeld surface analyses of
 1,4,6-trimethylquinoxaline-2,3(1<i>H</i>,4<i>H</i>)-dione monohydrate
;
_journal_coeditor_code           YK2133
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1296
_journal_page_last               1301
_journal_paper_doi               10.1107/S2056989020009573
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C11 H12 N2 O2, H2 O'
_chemical_formula_moiety         'C11 H12 N2 O2, H2 O'
_chemical_formula_sum            'C11 H14 N2 O3'
_chemical_formula_weight         222.24
_chemical_name_systematic
;
1,4,6-Trimethylquinoxaline-2,3(1<i>H</i>,4<i>H</i>)-dione monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 101.556(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0695(4)
_cell_length_b                   10.8321(5)
_cell_length_c                   14.4349(6)
_cell_measurement_reflns_used    7373
_cell_measurement_temperature    219(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      2.36
_cell_volume                     1082.98(9)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
and Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
WinGX (Farrugia, 2012), PLATON (Spek, 2020)
and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      219(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32798
_diffrn_reflns_theta_full        25.154
_diffrn_reflns_theta_max         25.154
_diffrn_reflns_theta_min         2.368
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.184
_refine_ls_extinction_coef       0.0031(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         1935
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0670
_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^)+(0.0097P)^2^+1.8308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                1563
_reflns_number_total             1935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yk2133sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243491
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.996
_shelx_hkl_checksum              71048
_shelx_res_checksum              14599
_cod_database_fobs_code 2243491