Unusual formation of (<i>E</i>)-11-(amino-methyl-ene)-8,9,10,11-tetra-hydro-pyrido[2',3':4,5]pyrimido[1,2-<i>a</i>]azepin-5(7<i>H</i>)-one and its crystal structure.
Khodjaniyazov, Khamid U.; Makhmudov, Utkir S.; Turgunov, Kambarali K.; Elmuradov, Burkhon Z.; Acta crystallographica. Section E, Crystallographic communications 73 (2017) 1497–1500; doi:10.1107/S2056989017013093

data_2311428
_publ_section_title
;
 Unusual formation of
 (<i>E</i>)-11-(amino-methyl-ene)-8,9,10,11-tetra-hydro-pyrido[2',3':4,5]pyrimido[1,2-<i>a</i>]azepin-5(7<i>H</i>)-one
 and its crystal structure.
;
_journal_coeditor_code           XU5905
_journal_issue                   'Pt 10'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              1497
_journal_page_last               1500
_journal_paper_doi               10.1107/S2056989017013093
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C13 H14 N4 O'
_chemical_formula_sum            'C13 H14 N4 O'
_chemical_formula_weight         242.28
_chemical_melting_point          458(2)
_chemical_name_common
;
\a-Aminomethylidene-2,3-pentamethylenepyrido[2,3-<i>d</i>]pyrimidin-4-one
;
_chemical_name_systematic
(<i>E</i>)-11-(Aminomethylene)-8,9,10,11-tetrahydropyrido[2',3':4,5]pyrimido[1,2-<i>a</i>]azepin-5(7<i>H</i>)-one
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.046(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7260(7)
_cell_length_b                   15.236(3)
_cell_length_c                   8.6642(7)
_cell_measurement_reflns_used    911
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.7350
_cell_measurement_theta_min      5.8870
_cell_volume                     1140.6(3)
_computing_cell_refinement
;
CrysAlis Pro (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis Pro (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis Pro (Oxford Diffraction, 2007)
;
_computing_molecular_graphics
;
XP in sHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
<i>SHELXL2014/7</i> (Sheldrick, 2015)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-7 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.2576
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  ' Oxford Diffraction Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7589
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.681
_diffrn_reflns_theta_min         5.119
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis Pro; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0554P)^2^+0.0030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                1478
_reflns_number_total             2328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xu5905sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2311428
_shelx_hkl_checksum              4853
_shelx_res_checksum              66903