2-[(2-Carboxyphenyl)disulfanyl]benzoate (1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1<i>H</i>-pyrazol-4-yl)ammonium
Huo, Jian-Zhong; Acta Crystallographica Section E 65 (2009) o2691–o2692; doi:10.1107/S1600536809036952

data_2223890
_publ_section_title
;
 2-[(2-Carboxyphenyl)disulfanyl]benzoate
 (1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1<i>H</i>-pyrazol-4-yl)ammonium
;
_journal_coeditor_code           LH2900
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2691
_journal_page_last               o2692
_journal_paper_doi               10.1107/S1600536809036952
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C11 H14 N3 O +, C14 H9 O4 S2 -'
_chemical_formula_moiety         'C11 H14 N3 O +, C14 H9 O4 S2 -'
_chemical_formula_sum            'C25 H23 N3 O5 S2'
_chemical_formula_weight         509.58
_chemical_name_systematic
;
2-[(2-Carboxyphenyl)disulfanyl]benzoate
(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1<i>H</i>-pyrazol-4-yl)ammonium
;
_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           SHELXL-97
_cell_angle_alpha                99.872(7)
_cell_angle_beta                 91.929(7)
_cell_angle_gamma                115.244(5)
_cell_formula_units_Z            2
_cell_length_a                   9.661(3)
_cell_length_b                   10.283(4)
_cell_length_c                   13.829(7)
_cell_measurement_reflns_used    4106
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.35
_cell_volume                     1215.4(9)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg & Berndt,
1999)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Brucker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0123
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6173
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.9448
_exptl_absorpt_correction_T_min  0.9258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0499P)^2^+0.3886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                3634
_reflns_number_total             4227
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2900.cif
_cod_data_source_block           I
_cod_original_cell_volume        1215.5(9)
_cod_original_formula_sum
;
C25 H23 N3 O5 S2
;
_cod_database_code               2223890
_cod_database_fobs_code          2223890