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_2017542
_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 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                 114.5289(13)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   25.5952(9)
_cell_length_b                   3.71581(13)
_cell_length_c                   26.3761(9)
_cell_measurement_reflns_used    31208
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      3.0
_cell_volume                     2282.16(14)
_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      120.0(10)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            36273
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>ABSCOR</i>; Higashi, 1995)
;
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1248.00
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6635
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0427P)^2^+1.1405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                5959
_reflns_number_total             6635
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3036.cif
_cod_data_source_block           I_120
_cod_database_code               2017542
_cod_database_fobs_code          2017542