A new polyoxo‒alkoxo titanium cluster of the Keggin family: synthesis and characterization by X-ray diffraction and NMR spectroscopy
Steunou, Nathalie; Kickelbick, Guido; Boubekeur, Kamal; Sanchez, Clément; Journal of the Chemical Society, Dalton Transactions  (1999) 3653–; doi:10.1039/a906198c

data_7027744
_publ_section_title
;
 A new polyoxo--alkoxo titanium cluster of the Keggin family: synthesis
 and characterization by X-ray diffraction and NMR spectroscopy
;
_journal_issue                   21
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3653
_journal_paper_doi               10.1039/a906198c
_journal_year                    1999
_chemical_formula_moiety         'C60 H140 O44 Ti17'
_chemical_formula_sum            'C60 H140 O44 Ti17'
_chemical_formula_weight         2380.02
_chemical_name_common            Ti17O24(OPri)20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 114.1580(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.32100(10)
_cell_length_b                   17.58550(10)
_cell_length_c                   26.9526(3)
_cell_measurement_temperature    200(2)
_cell_volume                     11382.90(17)
_computing_cell_refinement       'Siemens SAINT Software'
_computing_data_collection       'Siemens SMART Software'
_computing_data_reduction        'Siemens SAINT Software'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device_type  'Siemens SMART CCD detector'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_av_sigmaI/netI    0.1134
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44423
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.42
_diffrn_standards_interval_time  20
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4904
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       0.00013(6)
_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_ref   1.372
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         14424
_refine_ls_number_restraints     447
_refine_ls_restrained_S_all      1.359
_refine_ls_R_factor_all          0.2269
_refine_ls_R_factor_gt           0.1467
_refine_ls_shift/su_max          0.530
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3905
_refine_ls_wR_factor_ref         0.4422
_reflns_number_gt                7398
_reflns_number_total             14424
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906198csup1.cif
_cod_data_source_block           san1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_cell_volume        11382.89(15)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7027744