Supramolecular association in proton-transfer adducts containing benzamidinium cations. III. Three molecular salts of 3-methoxy-, 4-methoxy- and 3,4,5-trimethoxybenzoates with benzamidine
Portalone, Gustavo; Acta Crystallographica Section C 70 (2014) 225–229; doi:10.1107/S2053229614001090

data_2019383
_publ_section_title
;
 Supramolecular association in proton-transfer adducts containing
 benzamidinium cations. III. Three molecular salts of 3-methoxy-,
 4-methoxy- and 3,4,5-trimethoxybenzoates with benzamidine
;
_journal_coeditor_code           BG3168
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              225
_journal_page_last               229
_journal_paper_doi               10.1107/S2053229614001090
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C7 H9 N2 + , C10 H11 O5 - , H2 O'
_chemical_formula_moiety         'C7 H9 N2 +, C10 H11 O5 -, H2 O'
_chemical_formula_sum            'C17 H22 N2 O6'
_chemical_formula_weight         350.37
_chemical_name_common
;
Benzamidinium 3,4,5-trimethoxybenzoate monohydrate
;
_chemical_name_systematic
;
[Amino(phenyl)methylidene]azanium 3,4,5-trimethoxybenzoate 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
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.515(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.8771(15)
_cell_length_b                   7.8631(3)
_cell_length_c                   23.1789(13)
_cell_measurement_reflns_used    17484
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.9151
_cell_measurement_theta_min      2.6415
_cell_volume                     3697.9(4)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            39513
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9858
_exptl_absorpt_correction_T_min  0.9736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.367
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7977
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0571P)^2^+1.3989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                5752
_reflns_number_total             7977
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg3168sup1.cif
_cod_data_source_block           III
_cod_original_cell_volume        3697.9(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019383
_cod_database_fobs_code          2019383