An amino–imino resonance study of 2-amino-4-methylpyridinium nitrate and 2-amino-5-methylpyridinium nitrate
Yan, Xing-Chen; Fan, Yu-Hua; Bi, Cai-Feng; Zhang, Xia; Zhang, Zhong-Yu; Acta Crystallographica Section C 69 (2013) 61–65; doi:10.1107/S0108270112047877

data_2018767
_publ_section_title
;
 An amino--imino resonance study of 2-amino-4-methylpyridinium nitrate and
 2-amino-5-methylpyridinium nitrate
;
_journal_coeditor_code           WQ3020
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              61
_journal_page_last               65
_journal_paper_doi               10.1107/S0108270112047877
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C6 H9 N2 + , N O3 -'
_chemical_formula_moiety         'C6 H9 N2 +, N O3 -'
_chemical_formula_sum            'C6 H9 N3 O3'
_chemical_formula_weight         171.16
_chemical_name_systematic
;
2-amino-4-methylpyridinium nitrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.4150(7)
_cell_length_b                   12.8669(11)
_cell_length_c                   15.2441(14)
_cell_measurement_reflns_used    1536
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.776
_cell_measurement_theta_min      2.673
_cell_volume                     1650.6(2)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7806
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9758
_exptl_absorpt_correction_T_min  0.9514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.143
_refine_ls_extinction_coef       0.0052(17)
_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   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0379P)^2^+0.9001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                865
_reflns_number_total             1453
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wq3020.cif
_cod_data_source_block           I
_cod_database_code               2018767
_cod_database_fobs_code          2018767