4-Ammonio-5-chloro-<i>N</i>-[2-(<i>N,N</i>-diethylammonio)ethyl]-2-methoxybenzamide sulfate
Girija, C. R.; Noor Shahina Begum; Acta Crystallographica Section E 60 (2004) o260–o261; doi:10.1107/S1600536803029611

data_2203159
_publ_section_title
;4-Ammonio-5-chloro-<i>N</i>-[2-(<i>N,N</i>-diethylammonio)ethyl]-2-methoxybenzamide
 sulfate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o260
_journal_page_last               o261
_journal_paper_doi               10.1107/S1600536803029611
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C14 H24 Cl N3 O2 2+, S1 O4 2-'
_chemical_formula_moiety         'C14 H24 Cl N3 O2 2+, O4 S 2-'
_chemical_formula_sum            'C14 H24 Cl N3 O6 S'
_chemical_formula_weight         397.88
_chemical_name_common            'Metoclopramide Sulphate'
_chemical_name_systematic
;
4-Ammonio-5-chloro-N-[2-(N,N-diethylammonio)ethyl]-2-methoxybenzamide sulfate
;
_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
_cell_angle_beta                 97.1860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1514(2)
_cell_length_b                   16.5218(3)
_cell_length_c                   12.8524(3)
_cell_measurement_reflns_used    7814
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      2.0
_cell_volume                     1927.99(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7814
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.279
_refine_ls_extinction_coef       0.0074(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0961P)^2^+1.029P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1785
_reflns_number_gt                1932
_reflns_number_total             2768
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6315.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2203159