Preparation and Properties of the Aqua Ions [W4S4(H2O)12]n+ (n= 5, 6) and Crystal Structure of (Me2NH2)6[W4S4(NCS)12].0.5H2O#
Maxim N. Sokolov; Danil N. Dybtsev; Alexander V.Virovets; Vladimir P.Fedin; Pedro Esparza; Rita Hernandez-Molina; Dieter Fenske; A. Geoffrey Sykes; Inorganic Chemistry 41 (2002) 1136–1139; doi:10.1021/ic010830t

data_4317623
_publ_contact_author
;
         Prof. Valdimir P.Fedin
         Institute of Inorganic Chemistry SD RAS
         Ak.Lavrentiev prosp. 3
         Novosibirsk 630090
         Russia
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_publ_contact_author_email       cluster@che.nsk.su
_publ_contact_author_fax         '007 3832 344489'
_publ_contact_author_phone       none
_publ_section_title
;
 Preparation and Properties of the Aqua Ions [W4S4(H2O)12]n+ (n= 5, 6) and
 Crystal Structure of (Me2NH2)6[W4S4(NCS)12].0.5H2O#
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1136
_journal_page_last               1139
_journal_paper_doi               10.1021/ic010830t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_structural     '((C H3)2 N H2)6 (W4 S4 (SCN)12) . (H2 O)0.5'
_chemical_formula_sum            'C24 H49 N18 O0.5 S16 W4'
_chemical_formula_weight         1846.17
_chemical_name_systematic
;
  Hexakis(dimethylammonium)
tetra(mu4-thio)dodecaisothiocyanatotetratungsten(III,IV) semihydrate
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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            8
_cell_length_a                   22.760(3)
_cell_length_b                   22.760(3)
_cell_length_c                   22.760(3)
_cell_measurement_temperature    203(2)
_cell_volume                     11790(3)
_computing_cell_refinement       'STOE IPDS Software'
_computing_data_collection       'STOE IPDS Software'
_computing_data_reduction        'STOE IPDS Software'
_computing_molecular_graphics    'local programs'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE Image Plate IPDS'
_diffrn_measurement_method       phi-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.2554
_diffrn_reflns_av_sigmaI/netI    0.0997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33011
_diffrn_reflns_theta_full        21.62
_diffrn_reflns_theta_max         21.62
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.498
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7000
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.567
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       0.00035(17)
_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   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         4614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0768
_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^)+(0.0738P)^2^+86.0294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1924
_refine_ls_wR_factor_ref         0.2206
_reflns_number_gt                3256
_reflns_number_total             4614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010830t.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        11791(2)
_cod_original_formula_sum        'C24 H49 N18 O0.50 S16 W4'
_cod_database_code               4317623