#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/63/2216309.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_2216309
loop_
_publ_author_name
'Harald Brand '
'Christopher Hubrich'
'Kurt Polborn'
'Axel Schulz'
'Alexander Villinger'
_publ_section_title
;
 Redetermination of bis(S-methylthiuronium) sulfate
;
_journal_coeditor_code           BT2603
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4733
_journal_page_last               o4733
_journal_paper_doi               10.1107/S1600536807058059
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '2C2 H7 N2 S +, S O4  2-'
_chemical_formula_moiety         '2(C2 H7 N2 S +), S O4  2-'
_chemical_formula_sum            'C4 H14 N4 O4 S3'
_chemical_formula_weight         278.37
_chemical_name_common            'S-Methyl-thiuronium sulfate'
_chemical_name_systematic
;
bis(S-methylthiuronium) sulfate
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3250(19)
_cell_length_b                   8.3903(18)
_cell_length_c                   12.6041(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      9
_cell_volume                     1197.6(4)
_computing_cell_refinement       'CAD-4 Software (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1994)'
_computing_data_reduction        'OpenMoleN (Enraf--Nonius, 1997)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and DIAMOND (Brandenburg,
2005)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 1997'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Nonius MACH3'
_diffrn_measurement_method       ο-2Τ-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0061
_diffrn_reflns_av_sigmaI/netI    0.0077
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1175
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        -0.7
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.7491
_exptl_absorpt_correction_T_min  0.7166
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North et al.,  1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.47
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.359
_refine_ls_extinction_coef       0.065(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0501P)²+0.8658P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                1098
_reflns_number_total             1173
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt2603.cif
_cod_data_source_block           I
_cod_database_code               2216309
_cod_database_fobs_code          2216309
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
S S1 0.73533(5) 0.62211(8) 0.47370(5) 0.0500(3) Uani d . 1
N N1 0.69384(17) 0.7584(3) 0.65367(14) 0.0402(5) Uani d . 1
H H1 0.660(2) 0.820(3) 0.694(2) 0.043(7) Uiso d . 1
H H2 0.760(3) 0.722(3) 0.666(2) 0.049(7) Uiso d . 1
N N2 0.54254(16) 0.7861(2) 0.53413(15) 0.0341(4) Uani d . 1
H H3 0.507(2) 0.840(3) 0.577(2) 0.045(7) Uiso d . 1
H H4 0.518(3) 0.783(3) 0.469(2) 0.051(8) Uiso d . 1
C C1 0.64701(17) 0.7327(2) 0.56010(15) 0.0312(4) Uani d . 1
C C2 0.6354(2) 0.5513(3) 0.37475(19) 0.0451(6) Uani d . 1
H H5 0.6748 0.4749 0.3305 0.054 Uiso calc R 1
H H6 0.6088 0.6391 0.3322 0.054 Uiso calc R 1
H H7 0.5688 0.5018 0.4084 0.054 Uiso calc R 1
S S2 0.5000 0.92901(8) 0.2500 0.0240(2) Uani d S 1
O O1 0.58511(12) 1.03141(18) 0.30668(11) 0.0384(4) Uani d . 1
O O2 0.43656(12) 0.82932(19) 0.32713(10) 0.0358(4) Uani d . 1
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 0.0339(4) 0.0703(5) 0.0460(4) 0.0141(3) 0.0011(2) -0.0210(3)
N1 0.0311(9) 0.0572(12) 0.0322(9) 0.0152(9) -0.0035(8) -0.0054(8)
N2 0.0295(9) 0.0469(10) 0.0259(9) 0.0075(8) 0.0003(7) -0.0028(7)
C1 0.0275(9) 0.0376(10) 0.0285(9) 0.0024(7) 0.0036(7) 0.0017(8)
C2 0.0492(13) 0.0477(12) 0.0385(11) 0.0041(10) 0.0003(10) -0.0080(9)
S2 0.0186(3) 0.0364(4) 0.0170(3) 0.000 0.0003(2) 0.000
O1 0.0327(7) 0.0537(9) 0.0289(7) -0.0127(7) -0.0031(6) -0.0053(6)
O2 0.0283(7) 0.0522(8) 0.0270(7) -0.0070(6) 0.0040(5) 0.0072(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 S1 C2 . . 104.44(10) y
C1 N1 H1 . . 118.3(18) ?
C1 N1 H2 . . 118.7(19) ?
H1 N1 H2 . . 122(3) ?
C1 N2 H3 . . 118.5(19) ?
C1 N2 H4 . . 121.1(19) ?
H3 N2 H4 . . 119(3) ?
N2 C1 N1 . . 122.37(19) y
N2 C1 S1 . . 123.00(16) y
N1 C1 S1 . . 114.63(15) y
S1 C2 H5 . . 109.5 ?
S1 C2 H6 . . 109.5 ?
H5 C2 H6 . . 109.5 ?
S1 C2 H7 . . 109.5 ?
H5 C2 H7 . . 109.5 ?
H6 C2 H7 . . 109.5 ?
O2 S2 O2 4_655 . 110.64(13) y
O2 S2 O1 4_655 . 109.40(8) y
O2 S2 O1 . . 109.29(8) y
O2 S2 O1 4_655 4_655 109.29(8) ?
O2 S2 O1 . 4_655 109.40(8) ?
O1 S2 O1 . 4_655 108.79(13) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 C1 . 1.7459(19) y
S1 C2 . 1.786(2) y
N1 C1 . 1.311(3) y
N1 H1 . 0.82(3) ?
N1 H2 . 0.82(3) ?
N2 C1 . 1.307(3) ?
N2 H3 . 0.81(3) ?
N2 H4 . 0.86(3) ?
C2 H5 . 0.9600 ?
C2 H6 . 0.9600 ?
C2 H7 . 0.9600 ?
S2 O2 4_655 1.4699(13) ?
S2 O2 . 1.4699(13) y
S2 O1 . 1.4756(14) y
S2 O1 4_655 1.4756(14) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2 H4 O2 . 0.86(3) 2.05(3) 2.895(2) 165(3)
N2 H3 O1 5_676 0.81(3) 2.10(3) 2.908(2) 177(3)
N1 H1 O1 8_576 0.82(3) 2.08(3) 2.889(2) 175(2)
N1 H2 O2 3_566 0.82(3) 2.05(3) 2.856(2) 167(3)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C2 S1 C1 N2 -18.4(2)
C2 S1 C1 N1 161.61(17)
N1 N2 C1 S1 -180.0(3)
