Crystal structure of 5,11-dihydropyrido[2,3-<i>b</i>][1,4]benzodiazepin-6-one
Riad, Noura M.; Zlotos, Darius P.; Holzgrabe, Ulrike; Acta Crystallographica Section E 71 (2015) o304–o305; doi:10.1107/S2056989015006817

data_2240692
_publ_section_title
;
 Crystal structure of
 5,11-dihydropyrido[2,3-<i>b</i>][1,4]benzodiazepin-6-one
;
_journal_coeditor_code           HB7396
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o304
_journal_page_last               o305
_journal_paper_doi               10.1107/S2056989015006817
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C12 H9 N3 O'
_chemical_formula_moiety         'C12 H9 N3 O'
_chemical_formula_sum            'C12 H9 N3 O'
_chemical_formula_weight         211.22
_chemical_name_systematic
;
5,11-Dihydropyrido[2,3-<i>b</i>][1,4]benzodiazepin-6-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     iterative
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                104.628(6)
_cell_angle_beta                 96.616(5)
_cell_angle_gamma                98.009(4)
_cell_formula_units_Z            2
_cell_length_a                   3.7598(5)
_cell_length_b                   10.2467(14)
_cell_length_c                   12.8768(17)
_cell_measurement_reflns_used    1512
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.28
_cell_volume                     469.43(11)
_computing_cell_refinement
;
SAINT  (Bruker, 2013)
;
_computing_data_collection
;
APEX2  (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009), Mercury
(Macrae <i>et al.</i>, 2006) and  <i>enCIFer</i>  (Allen <i>et
al.</i>, 2004)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
olex2.solve (Bourhis <i>et al.</i>,  2015)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0346
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6425
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.793
_diffrn_reflns_theta_min         1.655
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_correction_T_min  0.8979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       plate
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0437P)^2^+0.2092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                1467
_reflns_number_total             2000
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7396sup1.cif
_cod_data_source_block           I
_cod_database_code               2240692
_cod_database_fobs_code          2240692
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.994
_shelx_hkl_checksum              2845
_shelx_res_checksum              98765
_shelxl_version_number           .2013