A Monovacant Heteropolytungstate Thioderivative: Synthesis and Characterization of [(PW~11~O~39~)~2~(H~4~Mo~4~S~4~O~6~)]^10-^ and Related Isomers
Jérôme Marrot; Marie Anne Pilette; Francis Sécheresse; Emmanuel Cadot; Inorganic Chemistry 42 (2003) 3609–3615; doi:10.1021/ic026191j

data_4313696
_publ_contact_author
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        Dr. E. Cadot
        Institut Lavoisier, IREM, UMR CNRS C 8637
        Universit\'e de Versailles Saint-Quentin-en-Yvelines
        45 Avenue des Etats Unis
        78035 Versailles cedex
        France
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_publ_contact_author_email       cadot@chimie.uvsq.fr
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_phone       '(33) 1 39 25 43 89'
_publ_section_title
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 A Monovacant Heteropolytungstate Thioderivative: Synthesis and
 Characterization of [(PW~11~O~39~)~2~(H~4~Mo~4~S~4~O~6~)]^10-^ and
 Related Isomers
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3609
_journal_page_last               3615
_journal_paper_doi               10.1021/ic026191j
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'K10 Mo4 O109 P2 S4 W22'
_chemical_formula_weight         6753.64
_chemical_name_systematic
;
   ?
;
_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                84.3020(10)
_cell_angle_beta                 81.5140(10)
_cell_angle_gamma                64.4840(10)
_cell_formula_units_Z            1
_cell_length_a                   11.67640(10)
_cell_length_b                   13.5414(2)
_cell_length_c                   19.9173(3)
_cell_measurement_temperature    296(2)
_cell_volume                     2808.69(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  '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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0935
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19197
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.434
_exptl_absorpt_correction_T_max  0.0538
_exptl_absorpt_correction_T_min  0.0384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.993
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         4.224
_refine_diff_density_min         -2.349
_refine_diff_density_rms         0.496
_refine_ls_extinction_coef       0.00077(5)
_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   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         13275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0801P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                9695
_reflns_number_total             13275
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026191jsi20030124_111325.cif
_cod_data_source_block           ec25
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_cell_volume        2808.69(6)
_cod_database_code               4313696