Synthesis and crystal structure of 2-(2,4-dioxo-6-methyl-pyran-3-yl-idene)-4-(4-hy-droxy-phen-yl)-2,3,4,5-tetra-hydro-1<i>H</i>-1,5-benzodiazepine.
Faraj, Imane; El Ghayati, Lhoussaine; Blacque, Olivier; Hökelek, Tuncer; Mazzah, Ahmed; Essassi, El Mokhtar; Sebbar, Nada Kheira; Acta crystallographica. Section E, Crystallographic communications 81 (2025) 381–384; doi:10.1107/S2056989025003032

data_2023462
_publ_section_title
;
 Synthesis and crystal structure of
 2-(2,4-dioxo-6-methyl-pyran-3-yl-idene)-4-(4-hy-droxy-phen-yl)-2,3,4,5-tetra-hydro-1<i>H</i>-1,5-benzodiazepine.
;
_journal_coeditor_code           HB8131
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              381
_journal_page_last               384
_journal_paper_doi               10.1107/S2056989025003032
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          'C21 H18 N2 O4'
_chemical_formula_moiety         'C21 H18 N2 O4'
_chemical_formula_sum            'C21 H18 N2 O4'
_chemical_formula_weight         362.37
_chemical_name_systematic
4-(4-Hydroxyphenyl)-2-(6-methyl-2,4-dioxopyran-3-ylidene)-2,3,4,5-tetrahydro-1<i>H</i>-1,5-benzodiazepine
_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
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5-ac6-012
(compiled 2023.08.24 svn.re1ec1418 for Rigaku Oxford Diffraction, GUI svn.r6817)
;
_cell_angle_alpha                100.967(2)
_cell_angle_beta                 97.373(2)
_cell_angle_gamma                100.127(2)
_cell_formula_units_Z            2
_cell_length_a                   6.37570(10)
_cell_length_b                   7.75060(10)
_cell_length_c                   17.9997(4)
_cell_measurement_reflns_used    9714
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      79.1140
_cell_measurement_theta_min      2.5240
_cell_volume                     847.49(3)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)
;
_computing_data_collection
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CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)
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_computing_data_reduction
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CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)
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_computing_molecular_graphics
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Olex2 1.5-ac6-012 (Dolomanov <i>et al.</i>,  2009)
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Olex2 1.5-ac6-012 (Dolomanov <i>et al.</i>,  2009)
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_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
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_computing_structure_solution
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<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18745
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.437
_diffrn_reflns_theta_min         2.536
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2024)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       needle
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.315
_refine_ls_extinction_coef       0.0020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0570P)^2^+0.3065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                3159
_reflns_number_total             3608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8131.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2023462.cif.'
_cod_database_code               2023462
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.984
_shelx_hkl_checksum              66772
_shelx_res_checksum              24576