Counteranion-Stabilized Titanium(IV) Isopolyoxocationic Clusters Isolated from Water.
Zhang, Guanyun; Hou, Jie; Li, Mingzhong; Tung, Chen-Ho; Wang, Yifeng; Inorganic chemistry 55 (2016) 4704–4709; doi:10.1021/acs.inorgchem.5b01901

data_4346658
_publ_section_title
;
 Counteranion-Stabilized Titanium(IV) Isopolyoxocationic Clusters Isolated
 from Water.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4704
_journal_page_last               4709
_journal_paper_doi               10.1021/acs.inorgchem.5b01901
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'H48 O36 Ti8, 8.5(I)'
_chemical_formula_sum            'H48 I8.5 O36 Ti8'
_chemical_formula_weight         2086.23
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
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_cell_length_b                   12.592(2)
_cell_length_c                   28.454(4)
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_cell_measurement_temperature    173
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
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_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            7600
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.458
_diffrn_reflns_theta_min         2.000
_exptl_absorpt_coefficient_mu    6.280
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.660
_exptl_crystal_description       block
_exptl_crystal_F_000             2888
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         1987
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+67.3541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1694
_reflns_number_total             1987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01901_si_002.cif
_cod_data_source_block           r-3
_cod_original_cell_volume        3906.9(16)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'H48 I8.50 O36 Ti8'
_cod_database_code               4346658
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: I1(0.08333)
3.a Rotating group:
 O5(H5A,H5B), O6(H6A,H6B), O4(H4A,H4B), O1(H1A,H1B)
;
_shelx_res_checksum              34167
_shelx_hkl_checksum              36296
_olex2_submission_special_instructions 'No special instructions were received'