Nanosized Alkali-Metal-Doped Ethoxotitanate Clusters
Yang Chen; Elzbieta Trzop; Anna Makal; Jesse D. Sokolow; Philip Coppens; Inorganic Chemistry 52 (2013) 4750–4752; doi:10.1021/ic302692d

data_4334613
_publ_contact_author_address
;         
Chemistry Department, University at Buffalo, SUNY, 
Buffalo, New York 14260-3000, 
United States.
;
_publ_contact_author_email       coppens@buffalo.edu
_publ_contact_author_fax         1-716-645-6948
_publ_contact_author_name        'Philip Coppens'
_publ_contact_author_phone       1-716-645-4273
_publ_section_title
;
 Nanosized Alkali-Metal-Doped Ethoxotitanate Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4750
_journal_page_last               4752
_journal_paper_doi               10.1021/ic302692d
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C88 H220 O78 Ti28'
_chemical_formula_sum            'C88 H220 O78 Ti28'
_chemical_formula_weight         3878.38
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 126.50(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.991(8)
_cell_length_b                   25.464(10)
_cell_length_c                   22.218(4)
_cell_measurement_reflns_used    8783
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      1.22
_cell_volume                     16368(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'multi-layered optics'
_diffrn_radiation_source         'TXS rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            152972
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    1.363
_exptl_absorpt_correction_T_max  0.9603
_exptl_absorpt_correction_T_min  0.8988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             7952
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
The unit cell contains 7 disordered solvent molecules, most likely ethanol, 
which have been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         16767
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1391
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+16.8969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1829
_reflns_number_gt                9706
_reflns_number_total             16767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302692d_si_002_3.cif
_cod_data_source_block           Ti28
_cod_database_code               4334613