#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:51:50 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179458 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/55/4335515.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4335515
loop_
_publ_author_name
'Igor M. Shlyapnikov'
'Hélène P. A. Mercier'
'Evgeny A. Goreshnik'
'Gary J. Schrobilgen'
'Zoran Mazej'
_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]-)∞, 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0900P)²+3.4039P] where P=(Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ti1 Ti 0.17944(8) 0.0000 0.38427(13) 0.0358(4) Uani 1 2 d S .
Ti2 Ti 0.0000 0.18773(6) 0.0000 0.0373(4) Uani 1 2 d S .
F1 F 0.1053(3) 0.09027(18) 0.1835(4) 0.0688(8) Uani 1 1 d . .
F2 F 0.3196(4) 0.0000 0.3924(6) 0.0583(10) Uani 1 2 d S .
F3 F 0.2482(3) 0.08508(18) 0.5636(4) 0.0626(8) Uani 1 1 d . .
F4 F 0.1048(3) 0.1795(2) -0.0630(5) 0.0702(9) Uani 1 1 d . .
F6 F 0.1043(3) 0.2660(2) 0.1858(5) 0.0798(10) Uani 1 1 d . .
F7 F 0.0217(3) 0.0000 0.3327(6) 0.0607(10) Uani 1 2 d S .
C1 C 0.0000 0.1748(7) 0.5000 0.053(2) Uani 0.864(18) 2 d SP 1
H1A H 0.0000 0.1136 0.5000 0.064 Uiso 0.864(18) 2 calc SPR 1
N1 N 0.0995(6) 0.2246(5) 0.5586(8) 0.058(2) Uani 0.864(18) 1 d P 1
H1B H 0.1758 0.2062 0.6032 0.070 Uiso 0.864(18) 1 calc PR 1
C2 C 0.0631(8) 0.3111(5) 0.5375(11) 0.068(3) Uani 0.864(18) 1 d P 1
H2A H 0.1155 0.3601 0.5692 0.081 Uiso 0.864(18) 1 calc PR 1
C1A C 0.0000 0.323(5) 0.5000 0.053(2) Uani 0.136(18) 2 d SP 2
H1AA H 0.0000 0.3841 0.5000 0.064 Uiso 0.136(18) 2 calc SPR 2
N1A N 0.087(4) 0.269(4) 0.536(7) 0.058(2) Uani 0.136(18) 1 d P 2
H1AB H 0.1635 0.2822 0.5725 0.070 Uiso 0.136(18) 1 calc PR 2
C2A C 0.039(7) 0.195(4) 0.507(11) 0.068(3) Uani 0.136(18) 1 d P 2
H2AA H 0.0755 0.1449 0.4997 0.081 Uiso 0.136(18) 1 calc PR 2
C3 C 0.7458(12) 0.0000 1.026(2) 0.079(5) Uiso 0.652(10) 2 d SPD 1
H3A H 0.8365 0.0000 1.0985 0.095 Uiso 0.652(10) 2 calc SPR 1
N2 N 0.6682(8) 0.0758(6) 0.9644(11) 0.077(2) Uiso 0.652(10) 1 d P 1
H2B H 0.6919 0.1301 0.9862 0.093 Uiso 0.652(10) 1 calc PR 1
C4 C 0.5488(8) 0.0418(5) 0.8636(12) 0.0461(15) Uani 0.652(10) 1 d PD 1
H4A H 0.4728 0.0756 0.7995 0.055 Uiso 0.652(10) 1 calc PR 1
C3A C 0.5290(15) 0.0000 0.844(4) 0.079(5) Uiso 0.348(10) 2 d SPD 2
H3AA H 0.4507 0.0000 0.7161 0.095 Uiso 0.348(10) 2 calc SPR 2
N2A N 0.557(2) 0.0679(13) 0.890(3) 0.077(2) Uiso 0.348(10) 1 d P 2
H2AB H 0.5167 0.1156 0.8743 0.093 Uiso 0.348(10) 1 calc PR 2
C4A C 0.7288(12) 0.0378(11) 1.015(2) 0.0461(15) Uani 0.348(10) 1 d PD 2
H4AA H 0.7999 0.0752 1.0667 0.055 Uiso 0.348(10) 1 calc PR 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
F3 Ti1 F3 92.4(2) . 6
F3 Ti1 F2 92.49(13) . .
F3 Ti1 F2 92.49(13) 6 .
F3 Ti1 F7 94.05(13) . .
F3 Ti1 F7 94.05(13) 6 .
F2 Ti1 F7 170.54(19) . .
F3 Ti1 F1 178.06(15) . 6
F3 Ti1 F1 89.20(13) 6 6
F2 Ti1 F1 86.35(14) . 6
F7 Ti1 F1 86.92(13) . 6
F3 Ti1 F1 89.20(13) . .
F3 Ti1 F1 178.06(15) 6 .
F2 Ti1 F1 86.35(14) . .
F7 Ti1 F1 86.92(13) . .
F1 Ti1 F1 89.18(18) 6 .
F6 Ti2 F6 95.9(2) . 2
F6 Ti2 F4 92.62(15) . 2
F6 Ti2 F4 92.74(16) 2 2
F6 Ti2 F4 92.74(16) . .
F6 Ti2 F4 92.62(15) 2 .
F4 Ti2 F4 172.0(2) 2 .
F6 Ti2 F1 173.46(16) . 2
F6 Ti2 F1 90.60(14) 2 2
F4 Ti2 F1 86.23(14) 2 2
F4 Ti2 F1 87.78(14) . 2
F6 Ti2 F1 90.60(14) . .
F6 Ti2 F1 173.46(16) 2 .
F4 Ti2 F1 87.78(14) 2 .
F4 Ti2 F1 86.23(14) . .
F1 Ti2 F1 82.93(17) 2 .
Ti1 F1 Ti2 164.40(19) . .
N1 C1 N1 108.9(8) . 2_556
N1 C1 H1A 125.5 . .
N1 C1 H1A 125.5 2_556 .
C1 N1 C2 109.1(5) . .
C1 N1 H1B 125.5 . .
C2 N1 H1B 125.5 . .
C2 C2 N1 106.5(4) 2_556 .
C2 C2 H2A 126.8 2_556 .
N1 C2 H2A 126.8 . .
N1A C1A N1A 100(6) . 2_556
N1A C1A C2A 64(4) . 2_556
N1A C1A C2A 64(4) 2_556 .
N1A C1A H1AA 129.8 . .
N1A C1A H1AA 129.8 2_556 .
C2A C1A H1AA 166.0 2_556 .
C2A C1A H1AA 166.0 . .
C2A N1A C1A 106(4) . .
C1A N1A C2A 77(3) . 2_556
C2A N1A H1AB 127.2 . .
C1A N1A H1AB 126.0 . .
C2A N1A H1AB 154.8 2_556 .
C2A C2A N1A 113(4) 2_556 .
N1A C2A N1A 76(4) . 2_556
C2A C2A C1A 76.0(16) 2_556 .
C2A C2A H2AA 123.4 2_556 .
N1A C2A H2AA 123.4 . .
N1A C2A H2AA 158.5 2_556 .
C1A C2A H2AA 159.3 . .
N2 C3 N2 110.8(11) 6 .
N2 C3 H3A 124.6 6 .
N2 C3 H3A 124.6 . .
C4 N2 C3 101.6(8) . .
C4 N2 H2B 129.2 . .
C3 N2 H2B 129.2 . .
C4 C4 N2 113.0(5) 6 .
C4 C4 H4A 123.5 6 .
N2 C4 H4A 123.5 . .
N2A C3A N2A 144(3) . 6
N2A C3A H3AA 108.1 . .
N2A C3A H3AA 108.1 6 .
C3A N2A C4A 89.2(17) . .
C3A N2A H2AB 135.4 . .
C4A N2A H2AB 135.4 . .
C4A C4A N2A 104.5(7) 6 .
C4A C4A H4AA 127.8 6 .
N2A C4A H4AA 127.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 F3 1.793(2) .
Ti1 F3 1.793(2) 6
Ti1 F2 1.807(4) .
Ti1 F7 1.824(3) .
Ti1 F1 1.956(2) 6
Ti1 F1 1.956(2) .
Ti2 F6 1.776(3) .
Ti2 F6 1.776(3) 2
Ti2 F4 1.803(3) 2
Ti2 F4 1.803(3) .
Ti2 F1 1.978(2) 2
Ti2 F1 1.978(2) .
C1 N1 1.303(8) .
C1 N1 1.303(8) 2_556
C1 H1A 0.9300 .
N1 C2 1.373(9) .
N1 H1B 0.8600 .
C2 C2 1.341(15) 2_556
C2 H2A 0.9300 .
C1A N1A 1.27(7) .
C1A N1A 1.27(7) 2_556
C1A C2A 2.00(9) 2_556
C1A C2A 2.00(9) .
C1A H1AA 0.9300 .
N1A C2A 1.23(7) .
N1A C2A 1.84(10) 2_556
N1A H1AB 0.8600 .
C2A C2A 0.96(12) 2_556
C2A N1A 1.84(10) 2_556
C2A H2AA 0.9300 .
C3 N2 1.401(11) 6
C3 N2 1.401(11) .
C3 H3A 0.9300 .
N2 C4 1.324(12) .
N2 H2B 0.8600 .
C4 C4 1.273(15) 6
C4 H4A 0.9300 .
C3A N2A 1.09(2) .
C3A N2A 1.09(2) 6
C3A H3AA 0.9300 .
N2A C4A 1.83(2) .
N2A H2AB 0.8600 .
C4A C4A 1.15(3) 6
C4A H4AA 0.9300 .
