Synthesis and characterization of four organic–inorganic salts: sulfates of 2-aminopyridinium derivatives
Bednarchuk, Tamara J.; Kinzhybalo, Vasyl; Pietraszko, Adam; Acta Crystallographica Section C 72 (2016) 882–889; doi:10.1107/S2053229616016004

data_2020643
_publ_section_title
;
 Synthesis and characterization of four organic--inorganic salts: sulfates
 of 2-aminopyridinium derivatives
;
_journal_coeditor_code           KU3189
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              882
_journal_page_last               889
_journal_paper_doi               10.1107/S2053229616016004
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C6 H8 N3 O2 +, H S O4 -'
_chemical_formula_moiety         'C6 H8 N3 O2 +, H O4 S -'
_chemical_formula_sum            'C6 H9 N3 O6 S'
_chemical_formula_weight         251.22
_chemical_name_systematic
;
2-Amino-4-methyl-3-nitropyridinium hydrogen sulfate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                97.03(3)
_cell_angle_beta                 90.21(3)
_cell_angle_gamma                90.15(3)
_cell_formula_units_Z            4
_cell_length_a                   7.835(3)
_cell_length_b                   8.105(3)
_cell_length_c                   15.881(4)
_cell_measurement_reflns_used    5835
_cell_measurement_temperature    295.0
_cell_measurement_theta_max      27.1880
_cell_measurement_theta_min      2.6350
_cell_volume                     1000.9(6)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1997)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      295.0
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction Xcalibur Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15737
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.510
_diffrn_reflns_theta_min         2.600
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku Oxford Diffraction, 2015), based on expressions
derived Clark & Reid (1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.194
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.264
_refine_ls_extinction_coef       0.053(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.4820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1396
_reflns_number_gt                3462
_reflns_number_total             4903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ku3189sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 2020643--2020646.cif.'
_cod_database_code               2020643
_cod_database_fobs_code          2020643
_shelx_hkl_checksum              89564
_shelx_res_checksum              41795