From Clusters to Ionic Complexes: Structurally Characterized Thallium Titanium Double Alkoxides
Timothy J. Boyle; Cecilia A. Zechmann; Todd M. Alam; Mark A. Rodriguez; Cybele A. Hijar; Brian L. Scott; Inorganic Chemistry 41 (2002) 946–957; doi:10.1021/ic0110833

data_4317596
_publ_section_title
;
 From Clusters to Ionic Complexes: Structurally Characterized Thallium
 Titanium Double Alkoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              946
_journal_page_last               957
_journal_paper_doi               10.1021/ic0110833
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C36 H81 O9 Ti2 Tl'
_chemical_formula_weight         958.18
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.891(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0326(7)
_cell_length_b                   15.7498(8)
_cell_length_c                   27.8338(17)
_cell_measurement_temperature    203(2)
_cell_volume                     4749.3(5)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker P4/CCD'
_diffrn_measurement_method       '\w and \f 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9402
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        '< 2'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.754
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.320
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         9402
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.1689
_refine_ls_R_factor_gt           0.1093
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2780
_refine_ls_wR_factor_ref         0.3118
_reflns_number_gt                5609
_reflns_number_total             9402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0110833_3.cif
_cod_data_source_block           ccd98
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4317596