Redetermination of 3-(ammoniomethyl)pyridinium dichloride
Liang, Wen-Xian; Wang, Gang; Qu, Zhi-Rong; Acta Crystallographica Section E 65 (2009) o1814–; doi:10.1107/S1600536809025859

data_2222867
_publ_section_title
;
 Redetermination of 3-(ammoniomethyl)pyridinium dichloride
;
_journal_coeditor_code           RZ2346
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1814
_journal_paper_doi               10.1107/S1600536809025859
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C6 H10 N2 2+, 2Cl -'
_chemical_formula_moiety         'C6 H10 N2 2+, 2(Cl -)'
_chemical_formula_sum            'C6 H10 Cl2 N2'
_chemical_formula_weight         181.06
_chemical_name_common
;
3-picolylamine dihydrochloride
;
_chemical_name_systematic
;
3-(ammoniomethyl)pyridinium dichloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.61(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.5874(9)
_cell_length_b                   12.650(3)
_cell_length_c                   14.814(3)
_cell_measurement_reflns_used    8048
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.449
_cell_measurement_theta_min      3.0701
_cell_volume                     858.0(3)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 13.662
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8831
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.274P] 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                1684
_reflns_number_total             1961
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2346.cif
_cod_data_source_block           I
_cod_original_cell_volume        857.9(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C6 H10 Cl2 N2 '
_cod_database_code               2222867
_cod_database_fobs_code          2222867