4-(2-Oxopropyl)-1,3-bis(prop-2-yn-1-yl)-2,3,4,5-tetrahydro-1,5-benzodiazepin-2(1<i>H</i>)-one
Sebhaoui, Jihad; El Bakri, Youness; Rayni, Ibtissam; Essassi, El Mokhtar; Mague, Joel T.; IUCrData 1 (2016) x161013–; doi:10.1107/S2414314616010130

data_1543540
_publ_section_title
;
 4-(2-Oxopropyl)-1,3-bis(prop-2-yn-1-yl)-2,3,4,5-tetrahydro-1,5-benzodiazepin-2(1<i>H</i>)-one
;
_journal_coeditor_code           SJ4049
_journal_issue                   6
_journal_name_full               IUCrData
_journal_page_first              x161013
_journal_paper_doi               10.1107/S2414314616010130
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          'C18 H16 N2 O2'
_chemical_formula_moiety         'C18 H16 N2 O2'
_chemical_formula_sum            'C18 H16 N2 O2'
_chemical_formula_weight         292.33
_chemical_name_systematic
4-(2-Oxopropylidene)-1,3-bis(prop-2-yn-1-yl)-2,3,4,5-tetrahydro-1<i>H</i>-1,5-benzodiazepin-2-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'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                68.8030(10)
_cell_angle_beta                 78.5200(10)
_cell_angle_gamma                72.9800(10)
_cell_formula_units_Z            2
_cell_length_a                   8.6905(2)
_cell_length_b                   9.0249(3)
_cell_length_c                   10.8240(3)
_cell_measurement_reflns_used    5019
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.4006
_cell_measurement_theta_min      5.3525
_cell_volume                     752.69(4)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012) and
<i>Mercury</i> (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5877
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         72.394
_diffrn_reflns_theta_min         5.352
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>, Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.218
_refine_ls_extinction_coef       0.0185(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2014</i> (Sheldrick, 2015<i>b</i>)
;
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0623P)^2^+0.1660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                2554
_reflns_number_total             2802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj4049sup1.cif
_cod_data_source_block           I
_cod_database_code               1543540
_cod_database_fobs_code          1543540
_shelx_estimated_absorpt_t_min   0.892
_shelx_estimated_absorpt_t_max   0.916
_shelx_hkl_checksum              52340
_shelx_res_checksum              30208