N—H···S and N—H···O hydrogen bonding in tetra-<i>n</i>-butylammonium (imidazolidine-2-thione-2κ<i>S</i>)dioxo-1κ^2^<i>O</i>-di-μ-sulfido-1:2κ^4^<i>S</i>:<i>S</i>-copper(I)tungstate(VI)
Beheshti, Azizolla; Clegg, William; Dale, Sophie H.; Solimankhani, Ahmad; Acta Crystallographica Section E 61 (2005) m1509–m1511; doi:10.1107/S1600536805021628

data_2206357
_publ_section_title
;N---H&#x00B7;&#x00B7;&#x00B7;S and N---H&#x00B7;&#x00B7;&#x00B7;O hydrogen
 bonding in tetra-<i>n</i>-butylammonium
 (imidazolidine-2-thione-2\k<i>S</i>)dioxo-1\k^2^<i>O</i>-di-\m-sulfido-1:2\k^4^<i>S</i>:<i>S</i>-copper(I)tungstate(VI)
;
_journal_coeditor_code           BT6695
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1509
_journal_page_last               m1511
_journal_paper_doi               10.1107/S1600536805021628
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '(C16 H36 N) [W Cu O2 S2 (C3 H6 N2 S)]'
_chemical_formula_moiety         'C16 H36 N +, C3 H6 Cu N2 O2 S3 W -'
_chemical_formula_sum            'C19 H42 Cu N3 O2 S3 W'
_chemical_formula_weight         688.13
_chemical_name_systematic
;
tetra-n-butylammonium
(imidazolidine-2-thione-2\kS)dioxo-1\k^2^O-di-\m-sulfido-1:2\k^4^S:S-
copper(I)tungstate(VI)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.742(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6925(16)
_cell_length_b                   14.875(2)
_cell_length_c                   17.2342(8)
_cell_measurement_reflns_used    227
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.50
_cell_volume                     2731.7(6)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'EvalCCD (Duisenberg <i>et al.</i>, 2003)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28801
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.234
_exptl_absorpt_correction_T_max  0.239
_exptl_absorpt_correction_T_min  0.100
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(SHELXTL; Sheldrick, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.964
_refine_ls_extinction_coef       0.00053(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6215
_refine_ls_number_restraints     623
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0159P)^2^+6.5317P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                4881
_reflns_number_total             6215
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6695.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2206357
_cod_database_fobs_code          2206357