Crystal structure of (4<i>Z</i>)-4-[(dimethylamino)methylidene]-3,5-dioxo-2-phenylpyrazolidine-1-carbaldehyde
Mague, Joel T.; Mohamed, Shaaban K.; Akkurt, Mehmet; Ahmed, Eman A.; Khodairy, Ahmed; Acta Crystallographica Section E 71 (2015) o440–o441; doi:10.1107/S2056989015010038

data_2240802
_publ_section_title
;
 Crystal structure of
 (4<i>Z</i>)-4-[(dimethylamino)methylidene]-3,5-dioxo-2-phenylpyrazolidine-1-carbaldehyde
;
_journal_coeditor_code           HB7425
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o440
_journal_page_last               o441
_journal_paper_doi               10.1107/S2056989015010038
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C13 H13 N3 O3'
_chemical_formula_moiety         'C13 H13 N3 O3'
_chemical_formula_sum            'C13 H13 N3 O3'
_chemical_formula_weight         259.26
_chemical_name_systematic
(4<i>Z</i>)-4-[(Dimethylamino)methylidene]-3,5-dioxo-2-phenylpyrazolidine-1-carbaldehyde
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 113.2720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.4235(9)
_cell_length_b                   6.1033(2)
_cell_length_c                   16.8611(6)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.33
_cell_measurement_theta_min      3.64
_cell_volume                     2497.96(15)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2014)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2014)
;
_computing_data_reduction
;
<i>SAINT</i>  (Bruker, 2014)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.021
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26486
_diffrn_reflns_theta_full        72.250
_diffrn_reflns_theta_max         72.318
_diffrn_reflns_theta_min         3.642
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>TWINABS</i>; Sheldrick, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0577P)^2^+0.7347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                3979
_reflns_number_total             4565
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7425sup1.cif
_cod_data_source_block           I
_cod_database_code               2240802
_cod_database_fobs_code          2240802
_shelx_estimated_absorpt_t_min   0.823
_shelx_estimated_absorpt_t_max   0.960
_shelx_hkl_checksum              22326
_shelx_res_checksum              70586
_shelxl_version_number           2014/6