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_2018133
_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          '2C6 H9 N2 +, C8 Cl4 O4 2-, C8 H2 Cl4 O4'
_chemical_formula_moiety         '2(C6 H9 N2 +), C8 Cl4 O4 2-, C8 H2 Cl4 O4'
_chemical_formula_sum            'C28 H20 Cl8 N4 O8'
_chemical_formula_weight         824.08
_chemical_name_systematic
;
bis(2-amino-3-methylpyridin-1-ium) 3,4,5,6-tetrachlorophthalate--
3,4,5,6-tetrachlorophthalic acid (1/1)
;
_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           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                69.388(9)
_cell_angle_beta                 75.342(10)
_cell_angle_gamma                72.6180(10)
_cell_formula_units_Z            2
_cell_length_a                   8.6972(17)
_cell_length_b                   13.762(3)
_cell_length_c                   15.381(3)
_cell_measurement_reflns_used    4445
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.2
_cell_measurement_theta_min      1.4
_cell_volume                     1621.7(6)
_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 0.970
_diffrn_measured_fraction_theta_max 0.967
_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  0.0332
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9810
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         5964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.0334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                5551
_reflns_number_total             5964
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3389.cif
_cod_data_source_block           II
_cod_database_code               2018133
_cod_database_fobs_code          2018133