Two solid phases of pyrimidin-1-ium hydrogen chloranilate monohydrate determined at 225 and 120K
Gotoh, Kazuma; Asaji, Tetsuo; Ishida, Hiroyuki; Acta Crystallographica Section C 66 (2010) o114–o118; doi:10.1107/S010827011000363X

data_2017541
_publ_section_title
;
 Two solid phases of pyrimidin-1-ium hydrogen chloranilate monohydrate
 determined at 225 and 120K
;
_journal_coeditor_code           EG3036
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o114
_journal_page_last               o118
_journal_paper_doi               10.1107/S010827011000363X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C4 H5 N2 +, C6 H Cl2 O4 -, H2 O'
_chemical_formula_moiety         'C4 H5 N2 +, C6 H Cl2 O4 -, H2 O'
_chemical_formula_sum            'C10 H8 Cl2 N2 O5'
_chemical_formula_weight         307.09
_chemical_name_systematic
;
pyrimidin-1-ium hydrogen chloranilate monohydrate
;
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 114.208(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.6621(7)
_cell_length_b                   3.75947(18)
_cell_length_c                   26.7435(16)
_cell_measurement_reflns_used    18188
_cell_measurement_temperature    225.0(10)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      3.1
_cell_volume                     1161.12(11)
_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) and WinGX (Farrugia, 1999)'
_computing_publication_material
'CrystalStructure (Rigaku/MSC, 2004) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      225.0(10)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0090
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            21678
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>ABSCOR</i>; Higashi, 1995)
;
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             624.00
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3377
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0434P)^2^+0.4181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                3061
_reflns_number_total             3377
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3036.cif
_cod_data_source_block           I_225
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017541
_cod_database_fobs_code          2017541