Supramolecular association in proton-transfer adducts containing benzamidinium cations. I. Four molecular salts with uracil derivatives
Portalone, Gustavo; Acta Crystallographica Section C 66 (2010) o295–o301; doi:10.1107/S0108270110016252

data_2017669
_publ_section_title
;
 Supramolecular association in proton-transfer adducts containing
 benzamidinium cations. I. Four molecular salts with uracil derivatives
;
_journal_coeditor_code           FN3053
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o295
_journal_page_last               o301
_journal_paper_doi               10.1107/S0108270110016252
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C7 H9 N2 + , C4 H2 N3 O4 -'
_chemical_formula_moiety         'C7 H9 N2 + , C4 H2 N3 O4 -'
_chemical_formula_sum            'C11 H11 N5 O4'
_chemical_formula_weight         277.25
_chemical_name_common
;
benzamidinidium 5-nitrouracilate
;
_chemical_name_systematic
;
benzamidinidium 5-nitro-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-1-ide
;
_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           SHELXL97
_cell_angle_alpha                78.551(7)
_cell_angle_beta                 86.841(8)
_cell_angle_gamma                84.051(7)
_cell_formula_units_Z            2
_cell_length_a                   4.3625(4)
_cell_length_b                   10.4461(11)
_cell_length_c                   13.8556(12)
_cell_measurement_reflns_used    2451
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.6885
_cell_measurement_theta_min      2.7051
_cell_volume                     615.13(10)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 16.0696
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Oxford Xcalibur S CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4864
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.9933
_exptl_absorpt_correction_T_min  0.9781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[CrysAlis RED (Oxford Diffraction, 2006); empirical absorption
correction
using spherical harmonics implemented in the SCALE3 ABSPACK scaling algorithm]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0590P)^2^+0.0569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                1427
_reflns_number_total             2153
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3053.cif
_cod_data_source_block           IV
_cod_database_code               2017669
_cod_database_fobs_code          2017669