The Structural Conversion of Multinuclear Titanium(IV) μ-Oxo-complexes
Radtke, Aleksandra; Piszczek, Piotr; Muzioł, Tadeusz; Wojtczak, Andrzej; Inorganic Chemistry  (2014) 141006083028009–; doi:10.1021/ic5002545

data_4341243
_publ_section_title
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 The Structural Conversion of Multinuclear Titanium(IV) \m-Oxo-complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              141006083028009
_journal_paper_doi               10.1021/ic5002545
_journal_year                    2014
_chemical_formula_moiety         'C60 H120 O24 Ti6, 1.5(C7 H8)'
_chemical_formula_sum            'C70.5 H132 O24 Ti6'
_chemical_formula_weight         1651.15
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-P 3* 2n'
_space_group_name_H-M_alt        'R -3 c :R'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                58.004(2)
_cell_angle_beta                 58.004(2)
_cell_angle_gamma                58.004(2)
_cell_formula_units_Z            2
_cell_length_a                   19.1601(5)
_cell_length_b                   19.1601(5)
_cell_length_c                   19.1601(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4746.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       CrysAlisCCD
_computing_data_reduction        'CrysAlis 171'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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  'Oxford Sapphire CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1491
_diffrn_reflns_av_unetI/netI     0.1540
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33221
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.128
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.9399
_exptl_absorpt_correction_T_min  0.8594
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis CCD, Oxford 2001'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_F_000             1758
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0019(11)
_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   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         3247
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0664P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2318
_reflns_number_total             3247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5002545_si_006.cif
_cod_data_source_block           structure3
_cod_original_cell_volume        4746.0(5)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C70.50 H132 O24 Ti6'
_cod_database_code               4341243
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.940
_shelxl_version_number           2013-4
_shelx_res_checksum              38854
_shelx_hkl_checksum              32500