Solution identification and solid state characterisation of a heterometallic polyoxometalate {Mo(11)V(7)}: [Mo(VI)(11)V(V)(5)V(IV)(2)O(52)(mu(9)-SO(3))](7-).
Miras, Haralampos N; Stone, Daniel J; McInnes, Eric J L; Raptis, Raphael G; Baran, Peter; Chilas, George I; Sigalas, Michael P; Kabanos, Themistoklis A; Cronin, Leroy; Chemical communications (Cambridge, England)  (2008) 4703–4705; doi:10.1039/b811279g

data_7103408
_publ_section_title
;
 Solution identification and solid state characterisation of a
 heterometallic polyoxometalate {Mo(11)V(7)}:
 [Mo(VI)(11)V(V)(5)V(IV)(2)O(52)(mu(9)-SO(3))](7-).
;
_journal_issue                   39
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4703
_journal_page_last               4705
_journal_paper_doi               10.1039/b811279g
_journal_year                    2008
_chemical_formula_sum            'H52 Mo11 N7 O67 S V7'
_chemical_formula_weight         2666.47
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 105.653(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1402(2)
_cell_length_b                   19.1486(3)
_cell_length_c                   13.4922(3)
_cell_measurement_reflns_used    15855
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5573
_cell_measurement_theta_min      3.1388
_cell_volume                     3020.18(10)
_computing_cell_refinement
;CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.32.5
(release 08-05-2007 CrysAlis171 .NET)
;
_computing_data_collection
;CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.32.5
(release 08-05-2007 CrysAlis171 .NET)
;
_computing_data_reduction
;CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.32.5
(release 08-05-2007 CrysAlis171 .NET)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Saint
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Oxford
_diffrn_measurement_method       /w
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            21908
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.15
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.396
_exptl_absorpt_correction_T_max  0.7276
_exptl_absorpt_correction_T_min  0.7276
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.932
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         5765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0376P)^2^+22.7731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                5218
_reflns_number_total             5765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b811279g.txt
_cod_data_source_block           hm441b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               7103408