Two hydration products of 3,4,5,6-tetrachloro-<i>N</i>-(methyl-2-pyridyl)phthalmic acids
Waddell, Paul G.; Hulse, Jeremy O. S.; Cole, Jacqueline M.; Acta Crystallographica Section C 67 (2011) o255–o258; doi:10.1107/S0108270111022384

data_2018132
_publ_section_title
;
 Two hydration products of
 3,4,5,6-tetrachloro-<i>N</i>-(methyl-2-pyridyl)phthalmic acids
;
_journal_coeditor_code           GD3389
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o255
_journal_page_last               o258
_journal_paper_doi               10.1107/S0108270111022384
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C6 H9 N2 +, C8 H Cl4 O4 -'
_chemical_formula_moiety         'C6 H9 N2 +, C8 H Cl4 O4 -'
_chemical_formula_sum            'C14 H10 Cl4 N2 O4'
_chemical_formula_weight         412.04
_chemical_name_systematic
;
2-amino-6-methylpyridin-1-ium 2-carboxy-3,4,5,6-tetrachlorobenzoate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.441(14)
_cell_length_b                   12.56(2)
_cell_length_c                   13.69(2)
_cell_measurement_reflns_used    3604
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.9
_cell_measurement_theta_min      1.6
_cell_volume                     1623(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5083
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.498
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.31(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2495
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.063
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+5.8163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1274
_reflns_number_gt                2302
_reflns_number_total             2495
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3389.cif
_cod_data_source_block           I
_cod_database_code               2018132
_cod_database_fobs_code          2018132