Crystal Structures and Raman Spectra of Imidazolium Poly[perfluorotitanate(IV)] Salts Containing the [TiF6]2-, ([Ti2F9]-)\ιnfty, and [Ti2F11]3- and the New [Ti4F20]4- and [Ti5F23]3- Anions
Igor M. Shlyapnikov; Hélène P. A. Mercier; Evgeny A. Goreshnik; Gary J. Schrobilgen; Zoran Mazej; Inorganic Chemistry 52 (2013) 8315–8326; doi:10.1021/ic302468j

data_4335515
_publ_contact_author_address
;
Department of Inorganic Chemistry and Technology
Jozef Stefan Institute
Jamova 39 1000 Ljubljana
SLOVENIA
;
_publ_contact_author_email       evgeny.goreshnik@ijs.si
_publ_contact_author_fax         386(1)4773645
_publ_contact_author_name        'Goreshnik, Evgeny'
_publ_contact_author_phone       386(1)4773155
_publ_section_title
;
 Crystal Structures and Raman Spectra of Imidazolium
 Poly[perfluorotitanate(IV)] Salts Containing the [TiF6]2-,
 ([Ti2F9]-)\\infty, and [Ti2F11]3- and the New [Ti4F20]4- and [Ti5F23]3-
 Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8315
_journal_page_last               8326
_journal_paper_doi               10.1021/ic302468j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'F20 Ti4, 4(C3 H5 N2)'
_chemical_formula_sum            'C12 H20 F20 N8 Ti4'
_chemical_formula_weight         847.96
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-06-02T16:35:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.00
_cell_angle_beta                 129.6900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2139(6)
_cell_length_b                   15.2093(7)
_cell_length_c                   8.9514(3)
_cell_measurement_reflns_used    1468
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.8221
_cell_measurement_theta_min      2.4086
_cell_volume                     1384.35(10)
_computing_cell_refinement       'CrystalClear (Rigaku Corporation, 1999)'
_computing_data_collection       'CrystalClear (Rigaku Corporation, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku Corporation, 1999)'
_computing_molecular_graphics    'Diamond (Pennington, 1999)'
_computing_publication_material
;
WinGX 1.70 (Farrugia, L. J., 1999), enCIFer v.1.2 (Allen et al., 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SIR92 (Altomare et al., 1993), 
TeXsan (Molecular Structure Corporation, 1997--1999).
;
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device
;
        Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1366
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing R.H., 1995'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.587
_refine_ls_extinction_coef       0.0072(16)
_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   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1366
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+3.4039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1561
_reflns_number_gt                1086
_reflns_number_total             1366
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic302468j_si_002_3.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4335515