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_4334611
_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
;
Ti28.20 O77.60 C79.20 H198 Li0.80, O0.80
;
_chemical_formula_sum            'C79.2 H198 Li0.8 O78.4 Ti28.2'
_chemical_formula_weight         3761.51
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.34(3)
_cell_angle_beta                 94.44(3)
_cell_angle_gamma                107.76(2)
_cell_formula_units_Z            2
_cell_length_a                   16.388(3)
_cell_length_b                   16.338(3)
_cell_length_c                   28.333(6)
_cell_measurement_reflns_used    21898
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      1.31
_cell_volume                     7194(3)
_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
;
SHELXH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'multi-layered optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            115033
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_T_max  0.9403
_exptl_absorpt_correction_T_min  0.7999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             3846
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.179
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1814
_refine_ls_number_reflns         25346
_refine_ls_number_restraints     289
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+28.6720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1537
_reflns_number_gt                19678
_reflns_number_total             25346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302692d_si_002_1.cif
_cod_data_source_block           Ti28Li
_cod_original_cell_volume        7194(2)
_cod_original_formula_sum        'C79.20 H198 Li0.80 O78.40 Ti28.20'
_cod_database_code               4334611