A tetrasilver(I)ditungsten(VI) cluster with sulfide and bis(diphenylphosphino)methane ligands
Wang, Rong; Song, Li-Li; Hu, Ke-Yi; Jin, Qiong-Hua; Zhang, Cun-Lin; Acta Crystallographica Section E 66 (2010) m1185–m1186; doi:10.1107/S1600536810034197

data_2227373
_publ_section_title
;
 A tetrasilver(I)ditungsten(VI) cluster with sulfide and
 bis(diphenylphosphino)methane ligands
;
_journal_coeditor_code           DN2590
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1185
_journal_page_last               m1186
_journal_paper_doi               10.1107/S1600536810034197
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ag4 W2 S8 (C25 H22 P2)3], 2C3 H7 N O'
_chemical_formula_moiety         'C75 H66 Ag4 P6 S8 W2, 2(C3 H7 N O)'
_chemical_formula_sum            'C81 H80 Ag4 N2 O2 P6 S8 W2'
_chemical_formula_weight         2354.95
_chemical_name_systematic
;
tris[\m~2~-bis(diphenylphosphino)methane]-
3:6\k^2^<i>P</i>:<i>P</i>';4:5\k^2^<i>P</i>:<i>P</i>';
5:6\k^2^<i>P</i>:<i>P</i>'-\m~5~-sulfido-2:3:4:5:6\k^5^<i>S</i>-
\m~3~-sulfido-1:3:4\k^3^<i>S</i>-
tetra-\m~2~-sulfido-1:3\k^2^<i>S</i>;1:4\k^2^<i>S</i>;
2:5\k^2^<i>S</i>;2:6\k^2^<i>S</i>-disulfido-1\k<i>S</i>,2\k<i>S</i>-
tetrasilver(I)ditungsten(VI) <i>N</i>,<i>N</i>-dimethylformamide disolvate
;
_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                 107.2240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.931(2)
_cell_length_b                   14.0395(12)
_cell_length_c                   27.855(3)
_cell_measurement_reflns_used    27248
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.00
_cell_volume                     8565.5(14)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 2004)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 2004)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            69256
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.925
_exptl_absorpt_correction_T_max  0.2813
_exptl_absorpt_correction_T_min  0.2615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4600
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.43
_refine_diff_density_max         1.198
_refine_diff_density_min         -1.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         19520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+13.8363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                18777
_reflns_number_total             19520
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2590.cif
_cod_data_source_block           I
_cod_original_cell_volume        8565.6(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2227373
_cod_database_fobs_code          2227373