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_7006188
_publ_section_title
;
 Non-aqueous synthetic methodology for TiW(5) polyoxometalates:
 protonolysis of [(MeO)TiW(5)O(18)](3-) with alcohols, water and
 phenols.
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_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 +,C6 H5 O19 Ti W5 3-'
_chemical_formula_sum            'C54 H113 N3 O19 Ti W5'
_chemical_formula_weight         2075.62
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5172(11)
_cell_length_b                   17.7092(12)
_cell_length_c                   23.8534(16)
_cell_measurement_reflns_used    33121
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      2.10
_cell_volume                     6977.3(8)
_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      160(2)
_diffrn_measurement_device       'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43533
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         1.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.383
_exptl_absorpt_correction_T_max  0.642
_exptl_absorpt_correction_T_min  0.276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_description       block
_exptl_crystal_F_000             4008
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.64
_exptl_crystal_size_min          0.34
_refine_diff_density_max         2.570
_refine_diff_density_min         -2.242
_refine_diff_density_rms         0.220
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.563(10)
_refine_ls_extinction_coef       0.00013(2)
_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_all   1.137
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         15803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_obs          0.0350
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+38.1824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0894
_refine_ls_wR_factor_obs         0.0813
_reflns_number_observed          14567
_reflns_number_total             15808
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            b709732h.txt
_cod_data_source_block           rje105_(TBA)3[6]
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+38.1824P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+38.1824P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6977.3(7)
_cod_database_code               7006188