Non-aqueous synthetic methodology for TiW(5) polyoxometalates: protonolysis of [(MeO)TiW(5)O(18)](3-) with alcohols, water and phenols.
Errington, R. John; Petkar, Sagar S.; Middleton, Paul S.; McFarlane, William; Clegg, William; Coxall, Robert A.; Harrington, Ross W.; Dalton transactions (Cambridge, England : 2003)  (2007) 5211–5222; doi:10.1039/b709732h

data_7006193
_publ_section_title
;
 Non-aqueous synthetic methodology for TiW(5) polyoxometalates:
 protonolysis of [(MeO)TiW(5)O(18)](3-) with alcohols, water and
 phenols.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5211
_journal_page_last               5222
_journal_paper_doi               10.1039/b709732h
_journal_year                    2007
_chemical_formula_moiety         '3 C16 H36 N +,C7 H5 O20 Ti W5 3-'
_chemical_formula_sum            'C55 H113 N3 O20 Ti W5'
_chemical_formula_weight         2103.63
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   23.533(3)
_cell_length_b                   17.1813(19)
_cell_length_c                   17.4145(19)
_cell_measurement_reflns_used    6956
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.43
_cell_measurement_theta_min      2.26
_cell_volume                     7041.2(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.811
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6882
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.1068
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23179
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.43
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.310
_exptl_absorpt_correction_T_max  0.636
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.225
_refine_diff_density_min         -3.446
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8973
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.116
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+16.1280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1451
_reflns_number_gt                6296
_reflns_number_total             8973
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b709732h.txt
_cod_data_source_block           rje302_(TBA)3[13]
_cod_original_cell_volume        7041.1(13)
_cod_database_code               7006193