Crystal structure of ethyl 2-(5-amino-1-benzenesulfonyl-3-oxo-2,3-dihydro-1<i>H</i>-pyrazol-2-yl)acetate
Metwally, Nadia H.; Elgemeie, Galal H.; Jones, Peter G.; Acta Crystallographica Section E 76 (2020) 481–483; doi:10.1107/S2056989020002674

data_2243305
_publ_section_title
;
 Crystal structure of ethyl
 2-(5-amino-1-benzenesulfonyl-3-oxo-2,3-dihydro-1<i>H</i>-pyrazol-2-yl)acetate
;
_journal_coeditor_code           NR2077
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              481
_journal_page_last               483
_journal_paper_doi               10.1107/S2056989020002674
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C13 H15 N3 O5 S'
_chemical_formula_moiety         'C13 H15 N3 O5 S'
_chemical_formula_sum            'C13 H15 N3 O5 S'
_chemical_formula_weight         325.34
_chemical_name_systematic
;
Ethyl
2-(5-amino-1-benzenesulfonyl-3-oxo-2,3-dihydro-1<i>H</i>-pyrazol-2-yl)acetate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 104.521(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2139(4)
_cell_length_b                   8.8122(4)
_cell_length_c                   18.3486(7)
_cell_measurement_reflns_used    16307
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2980
_cell_measurement_theta_min      2.5690
_cell_volume                     1442.22(11)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
XP (Siemens, 1994)
;
_computing_publication_material
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Eos'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            74051
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.030
_diffrn_reflns_theta_min         2.283
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.8673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                3708
_reflns_number_total             4193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nr2077sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243305
_cod_database_fobs_code          2243305
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.963
_shelx_hkl_checksum              43326
_shelx_res_checksum              52638