Structural Investigations of the Phase Transitions of Tetramethylammonium Sulfate
Malchus, Michael; Jansen, Martin; Acta Crystallographica Section B 54 (1998) 494–502; doi:10.1107/S0108768197018351

data_2002997
_publ_section_title
;
 Structural Investigations of the Phase Transitions of
 Tetramethylammonium Sulfate
;
_journal_coeditor_code           JZ2003
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              494
_journal_page_last               502
_journal_paper_doi               10.1107/S0108768197018351
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         '2 (C4 H12 N +) (S O4 2-)'
_chemical_formula_sum            'C8 H24 N2 O4 S'
_chemical_formula_weight         244.35
_chemical_name_systematic        'Tetramethylammonium Sulfate'
_chemical_temperature_decomposition 565
_space_group_IT_number           125
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4 2 -1ab'
_symmetry_space_group_name_H-M   'P 4/n b m :1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8948(9)
_cell_length_b                   10.8948(9)
_cell_length_c                   10.789(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      3.2
_cell_volume                     1280.6(3)
_computing_cell_refinement       'CELDIM (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CADSHEL (Kopf \& Ruebcke, 1993)'
_computing_molecular_graphics    'KPLOT (Hundt, 1979), ORTEPII (Johson, 1971)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71070
_diffrn_reflns_av_R_equivalents  .0151
_diffrn_reflns_av_sigmaI/netI    .0548
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3770
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .252
_exptl_absorpt_correction_T_max  .962
_exptl_absorpt_correction_T_min  .932
_exptl_absorpt_correction_type   'numerical with FACE cards'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'see Fig. 4'
_exptl_crystal_F_000             536
_exptl_crystal_size_max          .38
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .24
_refine_diff_density_max         .364
_refine_diff_density_min         -.283
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.344
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         792
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.324
_refine_ls_restrained_S_obs      1.358
_refine_ls_R_factor_all          .0786
_refine_ls_R_factor_obs          .0667
_refine_ls_shift/esd_max         <0.001
_refine_ls_shift/esd_mean        .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0087P)^2^+0.9623P], where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .1233
_refine_ls_wR_factor_obs         .1181
_reflns_number_observed          701
_reflns_number_total             792
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            jz0003.cif
_cod_data_source_block           neub3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been
'decomposition at 565 K'. The value 'decomposition at 565 K' was
changed to '565'.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been
'decomposition at 565 K'. The value 'decomposition at 565 K' was
changed to '565'.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value
'w=1/[\s^2^(Fo^2^)+(0.0087P)^2^+0.9623P], where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0087P)^2^+0.9623P], where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 4/n b m'
_cod_database_code               2002997