Synthesis, crystal structure and Hirshfeld surface analysis of 3-(4,4-dimethyl-2,3,4,5-tetrahydro-1<i>H</i>-1,5-benzodiazepin-2-ylidene)-6-methyl-3,4-dihydro-2<i>H</i>-pyran-2,4-dione
Samba, Mohamed; Minnih, Mohamed Said; Hökelek, Tuncer; Kaur, Manpreet; Jasinski, Jerry P.; Sebbar, Nada Kheira; Essassi, El Mokhtar; Acta Crystallographica Section E 75 (2019) 228–232; doi:10.1107/S2056989019000689

data_2242827
_publ_section_title
;
 Synthesis, crystal structure and Hirshfeld surface analysis of
 3-(4,4-dimethyl-2,3,4,5-tetrahydro-1<i>H</i>-1,5-benzodiazepin-2-ylidene)-6-methyl-3,4-dihydro-2<i>H</i>-pyran-2,4-dione
;
_journal_coeditor_code           LH5890
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              228
_journal_page_last               232
_journal_paper_doi               10.1107/S2056989019000689
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C17 H18 N2 O3'
_chemical_formula_moiety         'C17 H18 N2 O3'
_chemical_formula_sum            'C17 H18 N2 O3'
_chemical_formula_weight         298.33
_chemical_name_systematic
3-(4,4-Dimethyl-2,3,4,5-tetrahydro-1<i>H</i>-1,5-benzodiazepin-2-ylidene)-6-methyl-3,4-dihydro-2<i>H</i>-pyran-2,4-dione
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.488(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.53730(10)
_cell_length_b                   24.0197(4)
_cell_length_c                   11.7815(3)
_cell_measurement_reflns_used    4280
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      71.4680
_cell_measurement_theta_min      3.8340
_cell_volume                     1523.77(6)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015a)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015b)
;
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0416
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9860
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.259
_diffrn_reflns_theta_min         3.680
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.156
_refine_ls_extinction_coef       0.0020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015a)
;
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.3037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                2519
_reflns_number_total             2934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5890sup1.cif
_cod_data_source_block           I
_cod_database_code               2242827
_shelx_estimated_absorpt_t_min   0.748
_shelx_estimated_absorpt_t_max   0.892
_shelx_hkl_checksum              90115
_shelx_res_checksum              55655
_shelxl_version_number           2014/6
_cod_database_fobs_code 2242827