N—H...S and C—H...S hydrogen bonds in two tetraalkylammonium dithiobiurea(1–) inclusion compounds
Guo, Hao; Wu, Jinfeng; Acta Crystallographica Section C Structural Chemistry 71 (2015) –; doi:10.1107/S2053229615003095

data_2019892
_publ_section_title
;
 N---H...S and C---H...S hydrogen bonds in two tetraalkylammonium
 dithiobiurea(1--) inclusion compounds
;
_journal_issue                   4
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229615003095
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C16 H36 N +, C2 H5 N4 S2 -'
_chemical_formula_moiety         'C16 H36 N +, C2 H5 N4 S2 -'
_chemical_formula_sum            'C18 H41 N5 S2'
_chemical_formula_weight         391.68
_chemical_name_systematic
;
Tetrabutylammonium carbamothioyl(carbamothioylamino)azanide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.6790(10)
_cell_angle_beta                 89.2460(10)
_cell_angle_gamma                77.6920(10)
_cell_formula_units_Z            2
_cell_length_a                   9.41510(10)
_cell_length_b                   9.68350(10)
_cell_length_c                   13.41890(10)
_cell_measurement_temperature    296(2)
_cell_volume                     1167.10(2)
_computing_cell_refinement
;
SMART (Bruker, 2007)
;
_computing_data_collection
;
SMART (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11214
_diffrn_reflns_theta_full        27.70
_diffrn_reflns_theta_max         27.70
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.9673
_exptl_absorpt_correction_T_min  0.9560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2007)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5403
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0838P)^2^+0.3749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1755
_reflns_number_gt                3695
_reflns_number_total             5403
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            yo3004sup1.cif
_cod_data_source_block           091111a_0m
_cod_original_cell_volume        1167.097(19)
_cod_database_code               2019892
_cod_database_fobs_code          2019892