Preservation of the cluster core upon formation of Ti3O(OPri)8(benzoate)2 from Ti3O(OR)10
Mijatovic, Ivan; Kickelbick, Guido; Puchberger, Michael; Schubert, Ulrich; New Journal of Chemistry 27 (2003) 3–; doi:10.1039/b208255a

data_7050447
_publ_section_title
;
 Preservation of the cluster core upon formation of
 Ti3O(OPri)8(benzoate)2 from Ti3O(OR)10
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3
_journal_paper_doi               10.1039/b208255a
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C38 H66 O13 Ti3'
_chemical_formula_weight         874.61
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.1290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9142(7)
_cell_length_b                   37.930(2)
_cell_length_c                   11.4083(7)
_cell_measurement_reflns_used    7242
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.273
_cell_measurement_theta_min      2.334
_cell_volume                     4667.5(5)
_computing_cell_refinement       'Siemens SAINT Software'
_computing_data_collection       'Siemens SMART Software'
_computing_data_reduction        'Siemens SAINT Software'
_computing_molecular_graphics    'Siemens SHELXTL Software'
_computing_publication_material  'Siemens SHELXTL Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '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     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31682
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.96
_diffrn_standards_interval_time  20
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.8336
_exptl_absorpt_correction_T_min  0.6906
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0027(2)
_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   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         11463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0432P)^2^+4.7340P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1242
_reflns_number_gt                9324
_reflns_number_total             11463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208255a.txt
_cod_data_source_block           im2
_cod_original_cell_volume        4667.6(5)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7050447