Novel Ti-O-Ti bonding species constructed in a metal-oxide cluster: reaction products of bis(oxalato)oxotitanate(IV) with the dimeric, 1,2-dititanium(IV)-substituted Keggin polyoxotungstate.
Hayashi, Kunihiko; Murakami, Hideyuki; Nomiya, Kenji; Inorganic chemistry 45 (2006) 8078–8085; doi:10.1021/ic060661i

data_4350338
_publ_section_title
;
 Novel Ti-O-Ti bonding species constructed in a metal-oxide cluster:
 reaction products of bis(oxalato)oxotitanate(IV) with the dimeric,
 1,2-dititanium(IV)-substituted Keggin polyoxotungstate.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8078
_journal_page_last               8085
_journal_paper_doi               10.1021/ic060661i
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C8 H29 K6 O70 P Ti4 W10'
_chemical_formula_weight         3540.98
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                101.182(4)
_cell_angle_beta                 92.160(5)
_cell_angle_gamma                101.480(4)
_cell_formula_units_Z            2
_cell_length_a                   12.638(4)
_cell_length_b                   14.219(5)
_cell_length_c                   18.992(6)
_cell_measurement_reflns_used    7374
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.17
_cell_volume                     3270.7(19)
_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(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0784
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37733
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    18.499
_exptl_absorpt_correction_T_max  0.7086
_exptl_absorpt_correction_T_min  0.3192
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    3.595
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         8.780
_refine_diff_density_min         -3.973
_refine_diff_density_rms         0.646
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         15838
_refine_ls_number_restraints     600
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.257
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+58.1552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                11734
_reflns_number_total             15838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060661isi20060419_042032.cif
_cod_data_source_block           kh46s
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 

 Corrected the values of the '_diffrn_radiation_type',
 '_refine_diff_density_rms' and '_refine_ls_weighting_details'
 data items after consulting the original publication.

 Antanas Vaitkus,
 2019-12-11
;
_cod_original_cell_volume        3270.8(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4350338