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_4341241
_publ_section_title
;
 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         'Ti4 O4 4(C5 H9 O2) 4(C4 H9 O1); 0.5(C7 H8)'
_chemical_formula_sum            'C39.5 H76 O16 Ti4'
_chemical_formula_weight         998.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.16(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.962(3)
_cell_length_b                   16.979(3)
_cell_length_c                   13.317(3)
_cell_measurement_temperature    292(2)
_cell_volume                     2841.8(11)
_computing_data_collection       CrysAlisCCD
_computing_data_reduction        'CrysAlis 171'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0606
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21589
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.303
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.8902
_exptl_absorpt_correction_T_min  0.6473
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis CCD, Oxford 2001'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_F_000             1058
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.323
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6013
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.606
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1655P)^2^+1.0041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2220
_refine_ls_wR_factor_ref         0.2399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4840
_reflns_number_total             6013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5002545_si_010.cif
_cod_data_source_block           structure6
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'C39.50 H76 O16 Ti4'
_cod_database_code               4341241
_shelx_estimated_absorpt_t_min   0.647
_shelx_estimated_absorpt_t_max   0.890
_shelxl_version_number           2013-4
_shelx_res_checksum              31849
_shelx_hkl_checksum              269