A first example of polyoxotungstate-based giant molecule. Synthesis and molecular structure of a tetrapod-shaped Ti–O–Ti bridged anhydride form of Dawson tri-titanium(IV)-substituted polyoxotungstate
Sakai, Yoshitaka; Yoza, Kenji; Kato, Chika Nozaki; Nomiya, Kenji; Dalton Transactions  (2003) 3581–3586; doi:10.1039/b304033j

data_7013076
_publ_section_title
;
 A first example of polyoxotungstate-based giant molecule. Synthesis
 and molecular structure of a tetrapod-shaped Ti--O--Ti bridged anhydride
 form of Dawson tri-titanium(IV)-substituted polyoxotungstate
;
_journal_coden_ASTM              DTARAF
_journal_issue                   18
_journal_name_full               'Dalton Transactions'
_journal_page_first              3581
_journal_page_last               3586
_journal_paper_doi               10.1039/b304033j
_journal_year                    2003
_chemical_formula_sum            'Cl H147.5 K4 Na24 O312 P8 Ti12 W60'
_chemical_formula_weight         17737.85
_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                119.4640(10)
_cell_angle_beta                 90.6870(10)
_cell_angle_gamma                115.478(2)
_cell_formula_units_Z            2
_cell_length_a                   29.297(2)
_cell_length_b                   29.5965(18)
_cell_length_c                   29.6362(18)
_cell_measurement_reflns_used    8819
_cell_measurement_temperature    90
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.45
_cell_volume                     19363(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      90
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0914
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            120930
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    18.173
_exptl_absorpt_correction_T_max  0.3242
_exptl_absorpt_correction_T_min  0.0769
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.042
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             15649
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         6.854
_refine_diff_density_min         -4.621
_refine_diff_density_rms         0.486
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3432
_refine_ls_number_reflns         64449
_refine_ls_number_restraints     6132
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.088
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1014P)^2^+588.5401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.1977
_reflns_number_gt                47559
_reflns_number_total             64449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b304033j.txt
_cod_data_source_block           11miy
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'H147.50 Cl K4 Na24 O312 P8 Ti12 W60'
_cod_database_code               7013076