#------------------------------------------------------------------------------
#$Date: 2016-11-20 05:37:39 +0100 (dom 20 de nov de 2016) $
#$Revision: 188597 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/29/2002996.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2002996
loop_
_publ_author_name
'Malchus, Michael'
'Jansen, Martin'
_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           137
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4n 2n -1n'
_symmetry_space_group_name_H-M   'P 42/n m c :1'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.5355(9)
_cell_length_b                   7.5355(9)
_cell_length_c                   10.9910(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      14.4
_cell_measurement_theta_min      4.6
_cell_volume                     624.11(14)
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       ω
_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  .0541
_diffrn_reflns_av_sigmaI/netI    .0296
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1532
_diffrn_reflns_theta_max         22.92
_diffrn_reflns_theta_min         3.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .259
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tetragonal bipyramid'
_exptl_crystal_F_000             268
_exptl_crystal_size_max          .19
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .15
_refine_diff_density_max         .219
_refine_diff_density_min         -.209
_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
_refine_ls_goodness_of_fit_all   1.174
_refine_ls_goodness_of_fit_obs   1.194
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_restrained_S_obs      1.194
_refine_ls_R_factor_all          .0407
_refine_ls_R_factor_obs          .0364
_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/[σ²(Fo²)+(0.0454P)²+0.3184P], where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .0921
_refine_ls_wR_factor_obs         .0888
_reflns_number_observed          219
_reflns_number_total             239
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            jz0003.cif
_cod_data_source_block           tt3
_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:

'_refine_ls_weighting_scheme' value
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+0.3184P], 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^)+(0.0454P)^2^+0.3184P], 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 4~2~/n m c'
_cod_database_code               2002996
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y+1/2, -z+1/2'
'-x, y, z'
'x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y, x, -z'
'y, -x, -z'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'y, x, -z'
'-y, -x, -z'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S1 .0126(6) .0126(6) .0204(10) .000 .000 .000
O1 .0522(15) .0232(13) .044(2) .000 .000 -.0146(11)
N1 .015(2) .021(2) .020(2) .000 .000 .000
C1 .017(2) .026(2) .025(2) .000 -.0019(15) .000
C2 .028(2) .027(2) .032(2) .000 .000 .009(2)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
S1 .0 .0 .0 .0152(6) Uani d S 1 . S
O1 .0 .1582(3) .0768(2) .0398(8) Uani d S 1 . O
N1 .5000 .0 .1938(3) .0186(9) Uani d S 1 . N
C1 .6621(4) .0 .2722(3) .0226(8) Uani d S 1 . C
C2 .5000 .1626(4) .1155(3) .0290(9) Uani d S 1 . C
H1 .653(3) -.103(3) .3239(15) .024(6) Uiso d . 1 . H
H2 .763(5) .0 .219(3) .033(9) Uiso d S 1 . H
H3 .401(3) .162(3) .0667(15) .033(6) Uiso d . 1 . H
H4 .5000 .258(4) .169(3) .017(8) Uiso d S 1 . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
