1,3-Propanediammonium tetrathiotungstate and <i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylethylenediammonium tetrathiotungstate
Srinivasan, Bikshandarkoil R.; Dhuri, Sunder N.; Näther, Christian; Bensch, Wolfgang; Acta Crystallographica Section C 59 (2003) m124–m127; doi:10.1107/S0108270103002543

data_2013309
_publ_section_title
;
 1,3-Propanediammonium tetrathiotungstate and
 <i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylethylenediammonium
 tetrathiotungstate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m124
_journal_page_last               m127
_journal_paper_doi               10.1107/S0108270103002543
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '(C3 H12 N2) [W S4]'
_chemical_formula_moiety         'C3 H12 N2 2+, S4 W 2-'
_chemical_formula_sum            'C3 H12 N2 S4 W'
_chemical_formula_weight         388.24
_chemical_name_common            '1,3-propanediammonium tetrathiotungstate'
_chemical_name_systematic
;
1,3-propanediammonium tetrathiotungstate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.801(2)
_cell_length_b                   10.609(2)
_cell_length_c                   10.774(2)
_cell_measurement_reflns_used    94
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      15.5
_cell_volume                     1073.5(5)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (STOE & Cie, 1998a)'
_computing_data_reduction        'REDU4 (STOE & Cie, 1998b)'
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 1998)'
_computing_publication_material  'CIFTAB in SHELXTL (Bruker, 1998)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE AED-II 4-circle diffractometer'
_diffrn_measurement_method       '\w-\q 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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4124
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  120
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    11.480
_exptl_absorpt_correction_T_max  0.401
_exptl_absorpt_correction_T_min  0.291
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE (STOE & CIE, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.540
_refine_diff_density_min         -1.838
_refine_ls_extinction_coef       0.0024(2)
_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   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         3126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0237
_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^)+(0.0336P)^2^+0.5352P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                2663
_reflns_number_total             3126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ln1158.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2013309