Crystal structures of crotonaldehyde semicarbazone and crotonaldehyde thiosemicarbazone from X-ray powder diffraction data
Arfan, Atef; Rukiah, Mwaffak; Acta Crystallographica Section E 71 (2015) 168–172; doi:10.1107/S2056989015000663

data_2240393
_publ_section_title
;
 Crystal structures of crotonaldehyde semicarbazone and crotonaldehyde
 thiosemicarbazone from X-ray powder diffraction data
;
_journal_coeditor_code           CV5481
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              168
_journal_page_last               172
_journal_paper_doi               10.1107/S2056989015000663
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C5 H9 N3 O'
_chemical_formula_moiety         'C5 H9 N3 O'
_chemical_formula_sum            'C5 H9 N3 O'
_chemical_formula_weight         127.15
_chemical_name_common
;
Crotonaldehyde semicarbazone
;
_chemical_name_systematic
;
(<i>E</i>)-2-[(<i>E</i>)-But-2-en-1-ylidene]hydrazinecarboxamide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           'from EXP file using GSAS2CIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 112.3496(11)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   11.1646(3)
_cell_length_b                   5.13891(9)
_cell_length_c                   13.0301(2)
_cell_measurement_temperature    298
_cell_volume                     691.43(3)
_computing_data_collection
;
<i>WinXPOW</i> (Stoe & Cie, 1999)
;
_computing_data_reduction
;
<i>WinXPOW</i> (Stoe & Cie, 1999)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012), Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
GSAS (Larson & Von Dreele, 2004)
;
_computing_structure_solution
;
<i>EXPO2014</i> (Altomare <i>et al.</i>,  2013)
;
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Stoe transmission Stadi-P'
_diffrn_radiation_monochromator  'Ge 111'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.5406
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.79084
_exptl_absorpt_correction_T_min  0.73511
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 4
 Flat plate transmission absorption correction
Terms =     0.15189         0.0000
Correction is not refined.
;
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_F_000             272
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  white
_pd_char_particle_morphology     'fine powder'
_pd_instr_dist_mono/spec         130
_pd_instr_dist_spec/detc         173
_pd_instr_dist_src/mono          260
_pd_meas_2theta_range_inc        0.02
_pd_meas_2theta_range_max        79.98
_pd_meas_2theta_range_min        5.0
_pd_meas_number_of_points        3750
_pd_meas_scan_method             step
_pd_phase_name                   (I)
_pd_proc_2theta_range_inc        0.02
_pd_proc_2theta_range_max        80
_pd_proc_2theta_range_min        5
_pd_proc_info_datetime           2014-11-18T14:41:24
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 20 terms.
 Shifted Chebyshev function of 1st kind
      1:    983.478     2:   -916.772     3:    421.914     4:   -92.3775
      5:   -9.18321     6:    30.2365     7:   -2.25826     8:   -10.7421
      9:   -19.9256    10:    25.6982    11:   -24.5216    12:    4.20376
     13:    6.93721    14:   -3.88406    15:   -7.36711    16:    7.71847
     17:   -1.82508    18:  -0.259371    19:  -0.220296    20:   0.765767
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_ls_profile_function
;
CW Profile function number 4 with  21 terms
Pseudovoigt profile coefficients as parameterized in (Thompson <i>et al.</i>,
1987)
Asymmetry correction of Finger <i>et al.</i>,  1994.
Microstrain broadening by P.W. Stephens,  (1999.
Peak tails are ignored  where the intensity is below 0.0010 times the peak
  Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0273
_pd_proc_ls_prof_wR_expected     0.0286
_pd_proc_ls_prof_wR_factor       0.0357
_pd_proc_number_of_points        3750
_pd_spec_mounting                'Powder loaded into two Mylar foils'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              8
_pd_spec_size_equat              8
_refine_ls_goodness_of_fit_all   1.27
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_restraints     0
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.00
_refine_ls_weighting_scheme      sigma
_reflns_number_total             421
_cod_data_source_file            cv5481sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2240393