Crystal structure of 1-amino-2-oxo-2,5,6,7,8,9-hexahydro-1<i>H</i>-cyclohepta[<i>b</i>]pyridine-3-carbonitrile
Elgemeie, Galal H.; Jones, Peter G.; Acta Crystallographica Section E 72 (2016) 1239–1241; doi:10.1107/S2056989016012196

data_2241798
_publ_section_title
;
 Crystal structure of
 1-amino-2-oxo-2,5,6,7,8,9-hexahydro-1<i>H</i>-cyclohepta[<i>b</i>]pyridine-3-carbonitrile
;
_journal_coeditor_code           SU5315
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1239
_journal_page_last               1241
_journal_paper_doi               10.1107/S2056989016012196
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C11 H13 N3 O'
_chemical_formula_moiety         'C11 H13 N3 O'
_chemical_formula_sum            'C11 H13 N3 O'
_chemical_formula_weight         203.24
_chemical_name_systematic
1-Amino-2-oxo-2,5,6,7,8,9-hexahydro-1<i>H</i>-cyclohepta[<i>b</i>]pyridine-3-carbonitrile
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.272(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5680(4)
_cell_length_b                   10.0475(4)
_cell_length_c                   11.6778(5)
_cell_measurement_reflns_used    6583
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.0820
_cell_measurement_theta_min      3.8810
_cell_volume                     978.46(7)
_computing_cell_refinement
;
(CrysAlis PRO; Agilent, 2010)
;
_computing_data_collection
;
(CrysAlis PRO; Agilent, 2010)
;
_computing_data_reduction
;
(CrysAlis PRO; Agilent, 2010)
;
_computing_molecular_graphics
;
XP (Siemens, 1994)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Atlas Nova'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19833
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.12
_diffrn_reflns_theta_min         5.30
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.2053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                1674
_reflns_number_total             2046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            su5315sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2241798
_cod_database_fobs_code          2241798