Crystal structure of ethyl 2-(3-amino-5-oxo-2-tosyl-2,5-dihydro-1<i>H</i>-pyrazol-1-yl)acetate
Metwally, Nadia H.; Elgemeie, Galal H.; Jones, Peter G.; Acta Crystallographica Section E 77 (2021) 615–617; doi:10.1107/S2056989021004795

data_2243828
_publ_section_title
;
 Crystal structure of ethyl
 2-(3-amino-5-oxo-2-tosyl-2,5-dihydro-1<i>H</i>-pyrazol-1-yl)acetate
;
_journal_coeditor_code           ZL5011
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              615
_journal_page_last               617
_journal_paper_doi               10.1107/S2056989021004795
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C14 H17 N3 O5 S'
_chemical_formula_moiety         'C14 H17 N3 O5 S'
_chemical_formula_sum            'C14 H17 N3 O5 S'
_chemical_formula_weight         339.36
_chemical_name_common
;
Ethyl 2-(3-amino-5-oxo-2-tosyl-2,5-dihydro-1<i>H</i>-pyrazol-1-yl)acetate
;
_chemical_name_systematic
'Ethyl 2-[3-amino-2-(4-methylbenzenesulfonyl)-5-oxo-2,5-dihydro-1<i>H</i>-pyrazol-1-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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 97.081(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1398(2)
_cell_length_b                   11.1525(2)
_cell_length_c                   16.3795(3)
_cell_measurement_reflns_used    78897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.0850
_cell_measurement_theta_min      2.2110
_cell_volume                     1656.85(6)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
XP (Siemens, 1994)
;
_computing_publication_material
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            128543
_diffrn_reflns_theta_full        35.000
_diffrn_reflns_theta_max         35.915
_diffrn_reflns_theta_min         2.215
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       tablet
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         7466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+0.3217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                6502
_reflns_number_total             7466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl5011sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243828
_cod_database_fobs_code          2243828
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.982
_shelx_hkl_checksum              17245
_shelx_res_checksum              83016