Crystal structure of 1-methyl-2-methylamino-3-nitro-1<i>H</i>-chromeno[2,3-<i>b</i>]pyridin-5(10<i>aH</i>)-one
Raja, Rajamani; Poomathi, Nataraj; Perumal, Paramasivam T.; SubbiahPandi, A.; Acta Crystallographica Section E 71 (2015) o824–o825; doi:10.1107/S2056989015018241

data_2241185
_publ_section_title
;
 Crystal structure of
 1-methyl-2-methylamino-3-nitro-1<i>H</i>-chromeno[2,3-<i>b</i>]pyridin-5(10<i>aH</i>)-one
;
_journal_coeditor_code           HB7515
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o824
_journal_page_last               o825
_journal_paper_doi               10.1107/S2056989015018241
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C14 H13 N3 O4'
_chemical_formula_moiety         'C14 H13 N3 O4'
_chemical_formula_sum            'C14 H13 N3 O4'
_chemical_formula_weight         287.27
_chemical_name_systematic
1-Methyl-2-methylamino-3-nitro-1<i>H</i>-chromeno[2,3-<i>b</i>]pyridin-5(10a<i>H</i>)-one
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   24.0182(13)
_cell_length_b                   26.8445(14)
_cell_length_c                   7.9140(4)
_cell_measurement_reflns_used    2096
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.28
_cell_volume                     5102.6(5)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2008)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2008)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2008)
;
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows</i> (Farrugia, 2012)
;
_computing_publication_material
;
<i>SHELXL97</i> (Sheldrick, 2008) and <i>PLATON</i> (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12952
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.110
_refine_diff_density_min         -0.138
_refine_ls_abs_structure_details none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2261
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0468P)^2^+1.3678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                2096
_reflns_number_total             2261
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7515sup1.cif
_cod_data_source_block           I
_cod_database_code               2241185
_cod_database_fobs_code 2241185