Cyclic Ti9 Keggin Trimers with Tetrahedral (PO4) or Octahedral (TiO6) Capping Groups
Ghada A. Al-Kadamany; Firasat Hussain; Sib Sankar Mal; Michael H. Dickman; Nathalie Leclerc-Laronze; Jérôme Marrot; Emmanuel Cadot; Ulrich Kortz; Inorganic Chemistry 47 (2008) 8574–8576; doi:10.1021/ic801114n

data_4306276
_publ_section_title
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Cyclic Ti9 Keggin Trimers with Tetrahedral (PO4) or Octahedral (TiO6)
Capping Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8574
_journal_page_last               8576
_journal_paper_doi               10.1021/ic801114n
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'Cs11.5 K1.5 Na1.5 O134 Si3 Ti10 W27'
_chemical_formula_weight         9292.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_atom_sites_solution_hydrogens   none
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   30.3253(11)
_cell_length_b                   30.3253(11)
_cell_length_c                   15.8808(14)
_cell_measurement_reflns_used    8835
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.90
_cell_measurement_theta_min      2.42
_cell_volume                     12647.7(13)
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            89174
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    21.374
_exptl_absorpt_correction_T_max  0.4819
_exptl_absorpt_correction_T_min  0.1836
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             12029
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.243
_refine_diff_density_min         -2.119
_refine_diff_density_rms         0.763
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         8660
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                7788
_reflns_number_total             8660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801114n_si_001_2.cif
_cod_data_source_block           natl54sa
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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      'R 3 m'
_cod_original_formula_sum        'Cs11.50 K1.50 Na1.50 O134 Si3 Ti10 W27'
_cod_database_code               4306276