Redetermination of bis(<i>S</i>-methylthiuronium) sulfate
Harald Brand; Christopher Hubrich; Kurt Polborn; Axel Schulz; Alexander Villinger; Acta Crystallographica Section E 63 (2007) o4733–o4733; doi:10.1107/S1600536807058059

data_2216309
_publ_section_title
;
 Redetermination of bis(<i>S</i>-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       \o-2\T-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 <i>et al.</i>,  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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0501P)^2^+0.8658P] where P=(Fo^2^+2Fc^2^)/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>2\s(I)
_cod_data_source_file            bt2603.cif
_cod_data_source_block           I
_cod_database_code               2216309
_cod_database_fobs_code          2216309