Crystal structure of the 1:2 adduct of bis(piperidinium) sulfate and 1,3-dimethylthiourea
Döring, Cindy; Lueck, Julian F. D.; Jones, Peter G.; Acta Crystallographica Section E 73 (2017) 651–653; doi:10.1107/S2056989017004820

data_2242146
_publ_section_title
;
 Crystal structure of the 1:2 adduct of bis(piperidinium) sulfate and
 1,3-dimethylthiourea
;
_journal_coeditor_code           HG5484
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              651
_journal_page_last               653
_journal_paper_doi               10.1107/S2056989017004820
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '2C5 H12 N +, S O4 2- , 2C3 H8 N2 S'
_chemical_formula_moiety         '2(C3 H8 N2 S), 2(C5 H12 N), O4 S'
_chemical_formula_sum            'C16 H40 N6 O4 S3'
_chemical_formula_weight         476.72
_chemical_name_systematic
;
Bis(piperidin-1-ium) sulfate--1,3-dimethylthiourea (1/2)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 101.326(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5899(5)
_cell_length_b                   17.5691(6)
_cell_length_c                   11.8980(5)
_cell_measurement_reflns_used    6031
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.1760
_cell_measurement_theta_min      4.3590
_cell_volume                     2580.51(18)
_computing_cell_refinement
;
CrysAlisPro (Agilent, 2014)
;
_computing_data_collection
;
CrysAlisPro (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlisPro (Agilent, 2014)
;
_computing_molecular_graphics
;
XP (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21112
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         76.17
_diffrn_reflns_theta_min         4.38
_exptl_absorpt_coefficient_mu    2.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Agilent, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.383
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.6886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                2295
_reflns_number_total             2701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hg5484sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2580.52(17)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2242146
_cod_database_fobs_code          2242146