Redetermination of pyridine-4-carbonitrile‒chloranilic acid (1/1) at 180 K
Gotoh, Kazuma; Nagoshi, Hirokazu; Ishida, Hiroyuki; Acta Crystallographica Section E 64 (2008) o1260–; doi:10.1107/S1600536808017182

data_2218765
_publ_section_title
;
 Redetermination of pyridine-4-carbonitrile--chloranilic acid (1/1) at
 180 K
;
_journal_coeditor_code           LH2639
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1260
_journal_paper_doi               10.1107/S1600536808017182
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C6 H4 N2, C6 H2 Cl2 O4'
_chemical_formula_moiety         'C6 H4 N2, C6 H2 Cl2 O4'
_chemical_formula_sum            'C12 H6 Cl2 N2 O4'
_chemical_formula_weight         313.10
_chemical_name_systematic
;
pyridine-4-carbonitrile--chloranilic acid (1/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.0474(18)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.9327(8)
_cell_length_b                   4.9301(3)
_cell_length_c                   17.0355(10)
_cell_measurement_reflns_used    7762
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.0
_cell_volume                     1252.37(13)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku/MSC, 2004)'
_computing_data_collection       'PROCESS-AUTO (Rigaku/MSC, 2004)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
'CrystalStructure (Rigaku/MSC, 2004) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPIDII'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11539
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(<i>ABSCOR</i>; Higashi, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             632.00
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.726
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0805P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1765
_reflns_number_gt                2165
_reflns_number_total             3567
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2639.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2218765
_cod_database_fobs_code          2218765