(<i>E</i>)-4-[(2-Carbamoylhydrazinylidene)methyl]-3-hydroxy-5-hydroxymethyl-2-methylpyridin-1-ium nitrate
Novaković, Sladjana B.; Bogdanović, Goran A.; Leovac, Vukadin M.; Rodić, Marko V.; Vojinović-Ješić, Ljiljana S.; Ivković, Sonja; Acta Crystallographica Section C 69 (2013) 761–764; doi:10.1107/S0108270113013929

data_2019029
_publ_section_title
;
 (<i>E</i>)-4-[(2-Carbamoylhydrazinylidene)methyl]-3-hydroxy-5-hydroxymethyl-2-methylpyridin-1-ium
 nitrate
;
_journal_coeditor_code           FA3317
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              761
_journal_page_last               764
_journal_paper_doi               10.1107/S0108270113013929
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C9 H13 N4 O3 +, N O3 -'
_chemical_formula_moiety         'C9 H13 N4 O3 +, N O3 -'
_chemical_formula_sum            'C9 H13 N5 O6'
_chemical_formula_weight         287.24
_chemical_melting_point          505
_chemical_name_systematic
'(<i>E</i>)-4-[(2-Carbamoylhydrazinylidene)methyl]-3-hydroxy-5-hydroxymethyl-2-methylpyridin-1-ium nitrate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.117(5)
_cell_angle_beta                 93.566(4)
_cell_angle_gamma                104.589(4)
_cell_formula_units_Z            2
_cell_length_a                   7.1093(3)
_cell_length_b                   8.1905(4)
_cell_length_c                   11.6494(6)
_cell_measurement_reflns_used    5840
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      72.6850
_cell_measurement_theta_min      5.8490
_cell_volume                     608.09(6)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material
'WinGX (Farrugia, 2012), PLATON (Spek, 2009) and PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 16.3280
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Agilent Gemini S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9478
_diffrn_reflns_theta_full        72.66
_diffrn_reflns_theta_max         72.66
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            'translucent pale yellow'
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_meas      1.57
_exptl_crystal_density_method
'flotation in bromoform -- diethylether mixture'
_exptl_crystal_description       block
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.4939
_exptl_crystal_size_mid          0.3331
_exptl_crystal_size_min          0.1789
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.199
_refine_ls_extinction_coef       0.034(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0712P)^2^+0.1565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                2299
_reflns_number_total             2410
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fa3317.cif
_cod_data_source_block           I
_cod_original_cell_volume        608.09(5)
_cod_database_code               2019029
_cod_database_fobs_code          2019029