{AsW(9)O(33)}-{Mo(3)S(4)} based polyoxometalates including a metal-metal bond with Pd or Ni. Synthesis, structure and studies in solution.
Duval, Sylvain; Marrot, Jérôme; Simonnet-Jégat, Corine; Mbomekallé, Israël Martyr; Sokolov, Maxim; Cadot, Emmanuel; Dalton transactions (Cambridge, England : 2003) 41 (2012) 3174–3184; doi:10.1039/c2dt11420h

data_7018142
_publ_section_title
;
 {AsW(9)O(33)}-{Mo(3)S(4)} based polyoxometalates including a metal-metal
 bond with Pd or Ni. Synthesis, structure and studies in solution.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3174
_journal_page_last               3184
_journal_paper_doi               10.1039/c2dt11420h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'As4 H130 K20 Mo6 Ni2 O193 S8 W36'
_chemical_formula_weight         11868.86
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.5500(10)
_cell_angle_beta                 73.2030(10)
_cell_angle_gamma                74.7880(10)
_cell_formula_units_Z            1
_cell_length_a                   16.3743(5)
_cell_length_b                   18.5255(4)
_cell_length_c                   20.0599(6)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.20
_cell_volume                     5427.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            79360
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    20.659
_exptl_absorpt_correction_T_max  0.5761
_exptl_absorpt_correction_T_min  0.2318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5286
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.659
_refine_diff_density_min         -3.764
_refine_diff_density_rms         0.794
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1141
_refine_ls_number_reflns         19021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0960P)^2^+150.4718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1868
_reflns_number_gt                14554
_reflns_number_total             19021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt11420h.txt
_cod_data_source_block           K3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7018142