Crystal structure of 4-aminopyridinium 5-(5-chloro-2,4-dinitrophenyl)-1,3-dimethylbarbiturate hemihydrate
Vaduganathan, Manickkam; Doraisamyraja, Kalaivani; Acta Crystallographica Section E 70 (2014) 256–258; doi:10.1107/S1600536814021084

data_2240009
_publ_section_title
;
 Crystal structure of 4-aminopyridinium
 5-(5-chloro-2,4-dinitrophenyl)-1,3-dimethylbarbiturate hemihydrate
;
_journal_coeditor_code           SU2786
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              256
_journal_page_last               258
_journal_paper_doi               10.1107/S1600536814021084
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C5 H7 N2 +, C12 H8 Cl N4 O7 -, 0.5H2 O'
_chemical_formula_moiety         'C5 H7 N2 +, C12 H8 Cl N4 O7 -, 0.5(H2 O)'
_chemical_formula_sum            'C17 H16 N6 O7.5 cl'
_chemical_formula_weight         459.81
_chemical_name_common
;
4-Aminopyridinium 5-(5-chloro-2,4-dinitrophenyl)-1,3-dimethylbarbiturate
hemihydrate
;
_chemical_name_systematic
;
4-Aminopyridinium 5-(5-chloro-2,4-dinitrophenyl)-1,3-dimethylbarbiturate
hemihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 116.259(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.7242(5)
_cell_length_b                   14.2576(5)
_cell_length_c                   17.4321(7)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      2.56
_cell_volume                     3950.6(3)
_computing_cell_refinement
;
APEX2 and SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT and XPREP (Bruker, 2004)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>,  1993)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38331
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.9295
_exptl_absorpt_correction_T_min  0.9112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.458
_refine_ls_extinction_coef       0.0010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         3868
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0628P)^2^+9.3104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                2686
_reflns_number_total             3868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            su2786sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        3950.6(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C17 H16 cl N6 O7.5'
_cod_database_code               2240009
_cod_database_fobs_code          2240009