Towards a more reliable symmetry determination from powder diffraction: a redetermination of the low-temperature structure of 4-methylpyridine-<i>N</i>-oxide
Palatinus, Lukáš; Damay, Françoise; Acta Crystallographica Section B 65 (2009) 784–786; doi:10.1107/S0108768109042608

data_2104620
_publ_section_title
;
 Towards a more reliable symmetry determination from powder
 diffraction: a redetermination of the low-temperature structure of
 4-methylpyridine-<i>N</i>-oxide
;
_journal_coeditor_code           BK5090
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              784
_journal_page_last               786
_journal_paper_doi               10.1107/S0108768109042608
_journal_volume                  65
_journal_year                    2009
_chemical_formula_moiety         'C5 D4 N O,(CD3)'
_chemical_formula_sum            'C6 D7 N O'
_chemical_formula_weight         116
_chemical_melting_point          463
_chemical_name_common            N-oxipicoline
_chemical_name_systematic        4-methylpyridine-N-oxide
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                90.00000
_cell_formula_units_Z            32
_cell_length_a                   15.4073(2)
_cell_length_b                   15.4073(2)
_cell_length_c                   19.6748(3)
_cell_measurement_temperature    10
_cell_volume                     4670.50(11)
_computing_structure_refinement  FULLPROF
_diffrn_measurement_device_type  3T2
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           'Constant Wavelength Neutron Diffraction'
_diffrn_radiation_wavelength     1.22530
_pd_meas_2theta_range_inc        0.050000
_pd_meas_2theta_range_max        125.45000
_pd_meas_2theta_range_min        0.00000
_pd_meas_number_of_points        2510
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.050000
_pd_proc_2theta_range_max        125.4064
_pd_proc_2theta_range_min        -0.0436
_pd_proc_ls_background_function
;
20 background points manually selected
        8.350      181.436
       11.250      176.462
       13.350      181.951
       15.600      178.406
       22.500      195.004
       22.700      167.342
       26.400      175.102
       35.100      181.392
       36.350      189.902
       44.950      183.420
       45.200      188.148
       51.100      187.249
       54.650      179.516
       62.000      202.529
       83.350      215.464
       87.300      206.855
       93.600      201.973
       97.850      203.436
       97.950      204.573
      102.400      203.806
      109.900      200.954
      112.250      190.145
      117.100      170.538
      120.250      262.667
      122.750      255.667
;
_pd_proc_ls_pref_orient_corr     ' ?'
_pd_proc_ls_profile_function
;
Pseudo-voigt profile corresponding to function number 7 in FullProf
Microstrain broadening (strain model = 4) with following coefficients
         S_400         S_004         S_220         S_202
      0.000987     -0.000925      0.029328      0.005759
;
_pd_proc_ls_prof_R_factor        0.0334
_pd_proc_ls_prof_wR_expected     0.0143
_pd_proc_ls_prof_wR_factor       0.0406
_pd_proc_wavelength              1.225300
_pd_spec_mounting                ' vanadium'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              8
_pd_spec_size_equat              8
_pd_spec_size_thick              30
_refine_ls_number_parameters     38
_refine_ls_number_reflns         4509
_refine_ls_number_restraints     0
_cod_data_source_file            bk5090.cif
_cod_data_source_block           C5H4NOCH3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4670.52(13)
_cod_database_code               2104620