6-Hydrazinylnicotinic acid: a powder study
Rukiah, Mwaffak; Arfan, Atef; Acta Crystallographica Section E 68 (2012) o783–o784; doi:10.1107/S160053681200637X

data_2233803
_publ_section_title
;
 6-Hydrazinylnicotinic acid: a powder study
;
_journal_coeditor_code           FY2040
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o783
_journal_page_last               o784
_journal_paper_doi               10.1107/S160053681200637X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C6 H7 N3 O2'
_chemical_formula_moiety         'C6 H7 N3 O2'
_chemical_formula_sum            'C6 H7 N3 O2'
_chemical_formula_weight         153.15
_chemical_name_common
;
6-Hydrazinylnicotinic acid
;
_chemical_name_systematic
;
6-Hydrazinylpyridine-3-carboxylic acid
;
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0
_cell_angle_beta                 91.7805(11)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   6.69930(14)
_cell_length_b                   13.8834(2)
_cell_length_c                   7.10677(9)
_cell_measurement_temperature    298
_cell_volume                     660.675(19)
_computing_cell_refinement
;
FULLPROF (Rodriguez-Carvajal, 2001) and GSAS (Larson & Von Dreele,
2004)
;
_computing_data_collection       'WinXPOW (Stoe & Cie, 1999)'
_computing_data_reduction
;
WinXPOW (Stoe & Cie, 1999), DICVOL04 (Boultif & Lou\"er, 2004),
and
CheckGroup interfaced by WinPLOTR (Roisnel & Rodriguez-Carvajal, 2001)
;
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'publCIF  (Westrip, 2010)'
_computing_structure_refinement
;
GSAS (Larson & Von Dreele, 2004) interfaced by EXPGUI (Toby,
2001)
;
_computing_structure_solution    'EXPO2009 (Altomare <i>et al.</i>, 2009)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Stoe STADI P'
_diffrn_radiation_monochromator  'curved Ge(111)'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.5406
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.79474
_exptl_absorpt_correction_T_min  0.73239
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
;
[Flat-plate transmission absorption correction (GSAS absorption/surface
roughness correction function number 4 with a non-refined term of \md =
0.1482)]
;
_exptl_crystal_density_diffrn    1.54
_exptl_crystal_F_000             320
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  'pale brown'
_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_instr_location
;
Chemistry Department
 Atomic Energy Commission
 Damascus
 PO Box 6091
 Syrian Arab Republic
;
_pd_meas_2theta_range_inc        0.02
_pd_meas_2theta_range_max        84.98
_pd_meas_2theta_range_min        10.0
_pd_meas_number_of_points        4250
_pd_meas_scan_method             step
_pd_phase_name                   HYNIC
_pd_prep_pressure                101.3
_pd_prep_temperature             298
_pd_proc_2theta_range_inc        0.02
_pd_proc_2theta_range_max        84.94924
_pd_proc_2theta_range_min        9.96924
_pd_proc_info_data_reduction     none
_pd_proc_info_datetime           2012-01-25T09:05:52
_pd_proc_info_excluded_regions
;
The use of the excluded region from 85 to 95\% (2\q)
leads to better molecular geometry.
;
_pd_proc_ls_background_function
;
Shifted Chebyshev function of 1st kind (GSAS Background function number 1)
with 15 terms
      1:    1800.66     2:   -1847.80     3:    941.880     4:   -249.680
      5:    12.6164     6:    58.5368     7:   -22.4573     8:   -39.9081
      9:    32.2315    10:   0.665645    11:   -20.8095    12:    16.0647
     13:   -6.68008    14:   -5.95330    15:    5.95798
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_ls_pref_orient_corr     'spherical hamonics function'
_pd_proc_ls_profile_function
;
GSAS CW profile function number 4 with 21 terms, i.e.,
pseudovoigt profile coefficients as parameterized in (Thompson <i>et al.</i>,
1987),
asymmetry correction of Finger <i>et al.</i> (1994) and
microstrain broadening by 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        0.0226
_pd_proc_ls_prof_wR_expected     0.0213
_pd_proc_ls_prof_wR_factor       0.0298
_pd_proc_number_of_points        4250
_pd_spec_mounting
;
powder loaded between two Mylar foils
;
_pd_spec_mount_mode              transmission
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              8
_pd_spec_size_equat              8
_refine_diff_density_max         0.069
_refine_diff_density_min         -0.077
_refine_ls_goodness_of_fit_all   1.42
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_restraints     26
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.00
_reflns_number_total             466
_cod_data_source_file            fy2040.cif
_cod_data_source_block           I
_cod_original_cell_volume        660.673(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2233803