Crystal structure of ethyl 2-({[(4<i>Z</i>)-3,5-dioxo-1-phenylpyrazolidin-4-ylidene]methyl}amino)acetate
Mohamed, Shaaban K.; Akkurt, Mehmet; Mague, Joel T.; Ahmed, Eman A.; Albayati, Mustafa R.; Acta Crystallographica Section E 70 (2014) o938–o939; doi:10.1107/S1600536814016766

data_2239856
_publ_section_title
;
 Crystal structure of ethyl
 2-({[(4<i>Z</i>)-3,5-dioxo-1-phenylpyrazolidin-4-ylidene]methyl}amino)acetate
;
_journal_coeditor_code           SU2759
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o938
_journal_page_last               o939
_journal_paper_doi               10.1107/S1600536814016766
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C14 H15 N3 O4'
_chemical_formula_moiety         'C14 H15 N3 O4'
_chemical_formula_sum            'C14 H15 N3 O4'
_chemical_formula_weight         289.29
_chemical_name_systematic
;
Ethyl
2-({[(4<i>Z</i>)-3,5-dioxo-1-phenylpyrazolidin-4-ylidene]methyl}amino)acetate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                91.3290(9)
_cell_angle_beta                 97.3250(10)
_cell_angle_gamma                99.5620(10)
_cell_formula_units_Z            2
_cell_length_a                   5.49840(10)
_cell_length_b                   7.3585(2)
_cell_length_c                   16.6265(4)
_cell_measurement_reflns_used    3908
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.206
_cell_measurement_theta_min      2.682
_cell_volume                     657.27(3)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2013)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2013)'
_computing_data_reduction        '<i>SAINT</i>  (Bruker, 2013)'
_computing_molecular_graphics    '<i>DIAMOND</i> (Brandenburg & Putz, 2012)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL2014</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5108
_diffrn_reflns_theta_full        65.000
_diffrn_reflns_theta_max         72.216
_diffrn_reflns_theta_min         5.370
_exptl_absorpt_coefficient_mu    0.914
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2013)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0471P)^2^+0.2143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                2171
_reflns_number_total             2450
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2759sup1.cif
_cod_data_source_block           I
_cod_database_code               2239856
_cod_database_fobs_code          2239856
_shelx_hkl_checksum              41549
_shelx_res_checksum              91184
_shelxl_version_number           2.014