#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:51:50 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179458 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/55/4335514.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_4335514
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         'F11 Ti2, 3(C3 H5 N2)'
_chemical_formula_sum            'C9 H15 F11 N6 Ti2'
_chemical_formula_weight         512.07
_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             2011-03-08T12:32:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.9800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.5371(2)
_cell_length_b                   25.7451(4)
_cell_length_c                   10.4139(2)
_cell_measurement_reflns_used    5206
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.8478
_cell_measurement_theta_min      1.5818
_cell_volume                     3562.95(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      200
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.974
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3385
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.014
_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    1.909
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.570
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3385
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0960P)²+2.6698P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                2743
_reflns_number_total             3385
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic302468j_si_002_2.cif
_cod_data_source_block           shelxl
_cod_database_code               4335514
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_assembly
_atom_site_disorder_group
Ti1 Ti 0.03292(5) 0.5000 0.19364(6) 0.0272(2) Uani 1 2 d S . .
F1 F 0.0000 0.5000 0.0000 0.0504(10) Uani 1 4 d S . .
F2 F -0.10462(18) 0.5000 0.1861(3) 0.0469(7) Uani 1 2 d S . .
F3 F 0.0613(2) 0.5000 0.3692(3) 0.0585(8) Uani 1 2 d S . .
F4 F 0.16504(17) 0.5000 0.1787(3) 0.0437(6) Uani 1 2 d S . .
F5 F 0.03069(12) 0.42799(6) 0.18415(18) 0.0422(5) Uani 1 1 d . . .
Ti2 Ti 0.02507(3) 0.242834(18) 0.19225(4) 0.02493(19) Uani 1 1 d . . .
F6 F 0.0000 0.23902(12) 0.0000 0.0541(7) Uani 1 2 d S . .
F7 F 0.03150(12) 0.31365(6) 0.17358(19) 0.0454(5) Uani 1 1 d . . .
F8 F -0.11386(12) 0.24806(6) 0.17749(18) 0.0375(4) Uani 1 1 d . . .
F9 F 0.04920(16) 0.24728(8) 0.36721(19) 0.0553(5) Uani 1 1 d . . .
F10 F 0.01186(12) 0.17195(6) 0.1906(2) 0.0490(5) Uani 1 1 d . . .
F11 F 0.15942(12) 0.23720(6) 0.18463(17) 0.0387(4) Uani 1 1 d . . .
Ti3 Ti 0.04415(5) 0.0000 0.32964(8) 0.0355(2) Uani 1 2 d S . .
F12 F 0.0000 0.0000 0.5000 0.0587(11) Uani 1 4 d S . .
F13 F 0.17847(16) 0.0000 0.4275(2) 0.0373(6) Uani 1 2 d S . .
F14 F 0.0920(3) 0.0000 0.1831(3) 0.0793(10) Uani 1 2 d S . .
F15 F -0.0868(2) 0.0000 0.2539(3) 0.0645(9) Uani 1 2 d S . .
F16 F 0.04693(12) 0.07139(6) 0.3479(2) 0.0526(5) Uani 1 1 d . . .
C1 C 0.7714(2) 0.13312(10) 0.6828(3) 0.0318(6) Uani 1 1 d D . .
H1B H 0.8412 0.1386 0.7147 0.038 Uiso 1 1 calc R . .
N1 N 0.73006(17) 0.09093(9) 0.6240(2) 0.0331(5) Uani 1 1 d D . .
H1A H 0.7632 0.0633 0.6062 0.040 Uiso 1 1 calc R . .
C2 C 0.6079(2) 0.14435(13) 0.6356(3) 0.0422(7) Uani 1 1 d D . .
H2B H 0.5433 0.1598 0.6285 0.051 Uiso 1 1 calc R . .
C3 C 0.6282(2) 0.09675(12) 0.5950(3) 0.0386(7) Uani 1 1 d D . .
H3A H 0.5807 0.0719 0.5540 0.046 Uiso 1 1 calc R . .
N2 N 0.69838(18) 0.16631(9) 0.6892(2) 0.0347(6) Uani 1 1 d D . .
H2A H 0.7066 0.1977 0.7227 0.042 Uiso 1 1 calc RD . .
N3 N 0.29384(19) 0.12322(9) 0.6898(2) 0.0386(6) Uani 1 1 d D . .
H02A H 0.3575 0.1157 0.7195 0.046 Uiso 1 1 calc R . .
N4 N 0.13448(19) 0.11690(10) 0.6412(3) 0.0380(6) Uani 1 1 d D . .
H02B H 0.0731 0.1044 0.6329 0.046 Uiso 1 1 calc R . .
C10 C 0.2590(2) 0.16916(12) 0.6327(3) 0.0385(7) Uani 1 1 d D . .
H03B H 0.2985 0.1983 0.6179 0.046 Uiso 1 1 calc RD . .
C11 C 0.2176(2) 0.09203(12) 0.6936(3) 0.0388(7) Uani 1 1 d . . .
H03A H 0.2216 0.0577 0.7279 0.047 Uiso 1 1 calc R . .
C12 C 0.1586(2) 0.16524(11) 0.6017(3) 0.0375(7) Uani 1 1 d . . .
H02C H 0.1131 0.1910 0.5603 0.045 Uiso 1 1 calc R . .
C7 C 0.8265(6) 0.1146(4) 0.0151(7) 0.0326(18) Uani 0.520(5) 1 d PD A 1
H7A H 0.8958 0.1054 0.0308 0.039 Uiso 0.520(5) 1 calc PR A 1
N5 N 0.7476(9) 0.0839(3) -0.0392(6) 0.0516(19) Uani 0.520(5) 1 d PD A 1
H5A H 0.7497 0.0517 -0.0665 0.062 Uiso 0.520(5) 1 calc PR A 1
C8 C 0.6617(6) 0.1152(5) -0.0420(8) 0.0367(13) Uani 0.520(5) 1 d PD A 1
H8A H 0.5945 0.1045 -0.0751 0.044 Uiso 0.520(5) 1 calc PR A 1
C9 C 0.6862(7) 0.1583(4) 0.0045(8) 0.0333(13) Uani 0.520(5) 1 d PD A 1
H9A H 0.6415 0.1860 0.0131 0.040 Uiso 0.520(5) 1 calc PR A 1
N6 N 0.7881(9) 0.1598(4) 0.0416(12) 0.047(3) Uani 0.520(5) 1 d PD A 1
H6A H 0.8231 0.1866 0.0777 0.056 Uiso 0.520(5) 1 calc PR A 1
C7A C 0.6626(7) 0.1397(5) -0.0186(8) 0.0326(18) Uani 0.480(5) 1 d PD A 2
H7AA H 0.5956 0.1525 -0.0319 0.039 Uiso 0.480(5) 1 calc PR A 2
N5A N 0.6856(10) 0.0942(4) -0.0478(8) 0.0516(19) Uani 0.480(5) 1 d PD A 2
H5AA H 0.6453 0.0690 -0.0824 0.062 Uiso 0.480(5) 1 calc PR A 2
C8A C 0.7976(8) 0.0935(4) -0.0097(9) 0.0367(13) Uani 0.480(5) 1 d PD A 2
H8AA H 0.8410 0.0651 -0.0172 0.05(2) Uiso 0.480(5) 1 calc PR A 2
C9A C 0.8239(7) 0.1393(5) 0.0355(9) 0.0333(13) Uani 0.480(5) 1 d PD A 2
H9AA H 0.8912 0.1504 0.0657 0.040 Uiso 0.480(5) 1 calc PR A 2
N6A N 0.7438(10) 0.1679(4) 0.0333(13) 0.047(3) Uani 0.480(5) 1 d PD A 2
H6AA H 0.7432 0.2001 0.0611 0.056 Uiso 0.480(5) 1 calc PRD A 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 F4 93.63(14) . .
F3 Ti1 F2 93.55(15) . .
F4 Ti1 F2 172.82(12) . .
F3 Ti1 F5 93.00(6) . .
F4 Ti1 F5 90.10(5) . .
F2 Ti1 F5 89.52(5) . .
F3 Ti1 F5 93.00(6) . 6_565
F4 Ti1 F5 90.10(5) . 6_565
F2 Ti1 F5 89.52(5) . 6_565
F5 Ti1 F5 173.97(12) . 6_565
F3 Ti1 F1 179.38(11) . .
F4 Ti1 F1 86.99(9) . .
F2 Ti1 F1 85.83(10) . .
F5 Ti1 F1 87.00(6) . .
F5 Ti1 F1 87.00(6) 6_565 .
Ti1 F1 Ti1 180.0 5_565 .
F9 Ti2 F10 94.11(10) . .
F9 Ti2 F7 92.35(9) . .
F10 Ti2 F7 173.32(9) . .
F9 Ti2 F11 93.36(9) . .
F10 Ti2 F11 90.95(7) . .
F7 Ti2 F11 90.37(7) . .
F9 Ti2 F8 93.73(9) . .
F10 Ti2 F8 88.62(7) . .
F7 Ti2 F8 89.26(7) . .
F11 Ti2 F8 172.92(8) . .
F9 Ti2 F6 179.01(11) . .
F10 Ti2 F6 86.75(11) . .
F7 Ti2 F6 86.81(11) . .
F11 Ti2 F6 86.13(6) . .
F8 Ti2 F6 86.78(6) . .
Ti2 F6 Ti2 174.28(18) 2 .
F14 Ti3 F15 96.55(16) . .
F14 Ti3 F16 94.90(7) . 6
F15 Ti3 F16 92.54(5) . 6
F14 Ti3 F16 94.90(7) . .
F15 Ti3 F16 92.54(5) . .
F16 Ti3 F16 168.38(14) 6 .
F14 Ti3 F13 89.55(13) . .
F15 Ti3 F13 173.89(14) . .
F16 Ti3 F13 86.92(6) 6 .
F16 Ti3 F13 86.92(6) . .
F14 Ti3 F12 176.17(12) . .
F15 Ti3 F12 87.28(12) . .
F16 Ti3 F12 84.90(7) 6 .
F16 Ti3 F12 84.90(7) . .
F13 Ti3 F12 86.61(8) . .
Ti3 F12 Ti3 180.0 5_556 .
N1 C1 N2 107.5(2) . .
N1 C1 H1B 126.2 . .
N2 C1 H1B 126.2 . .
C1 N1 C3 109.6(2) . .
C1 N1 H1A 125.2 . .
C3 N1 H1A 125.2 . .
C3 C2 N2 106.5(3) . .
C3 C2 H2B 126.7 . .
N2 C2 H2B 126.7 . .
C2 C3 N1 106.9(3) . .
C2 C3 H3A 126.6 . .
N1 C3 H3A 126.6 . .
C1 N2 C2 109.5(2) . .
C1 N2 H2A 125.3 . .
C2 N2 H2A 125.3 . .
C11 N3 C10 109.5(3) . .
C11 N3 H02A 125.2 . .
C10 N3 H02A 125.2 . .
C11 N4 C12 109.4(3) . .
C11 N4 H02B 125.3 . .
C12 N4 H02B 125.3 . .
C12 C10 N3 106.8(3) . .
C12 C10 H03B 126.6 . .
N3 C10 H03B 126.6 . .
N3 C11 N4 107.7(3) . .
N3 C11 H03A 126.2 . .
N4 C11 H03A 126.2 . .
C10 C12 N4 106.6(3) . .
C10 C12 H02C 126.7 . .
N4 C12 H02C 126.7 . .
N6 C7 N5 106.7(7) . .
N6 C7 H7A 126.6 . .
N5 C7 H7A 126.6 . .
C7 N5 C8 104.8(6) . .
C7 N5 H5A 127.6 . .
C8 N5 H5A 127.6 . .
C9 C8 N5 110.3(7) . .
C9 C8 H8A 124.8 . .
N5 C8 H8A 124.8 . .
C8 C9 N6 108.6(8) . .
C8 C9 H9A 125.7 . .
N6 C9 H9A 125.7 . .
C7 N6 C9 109.5(7) . .
C7 N6 H6A 125.2 . .
C9 N6 H6A 125.2 . .
N5A C7A N6A 112.2(8) . .
N5A C7A H7AA 123.9 . .
N6A C7A H7AA 123.9 . .
C7A N5A C8A 103.4(8) . .
C7A N5A H5AA 128.3 . .
C8A N5A H5AA 128.3 . .
C9A C8A N5A 106.3(7) . .
C9A C8A H8AA 126.9 . .
N5A C8A H8AA 126.9 . .
C8A C9A N6A 109.7(9) . .
C8A C9A H9AA 125.1 . .
N6A C9A H9AA 125.1 . .
C9A N6A C7A 108.4(9) . .
C9A N6A H6AA 125.8 . .
C7A N6A H6AA 125.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 F3 1.796(3) .
Ti1 F4 1.824(2) .
Ti1 F2 1.849(2) .
Ti1 F5 1.8565(16) .
Ti1 F5 1.8565(16) 6_565
Ti1 F1 1.9805(6) .
F1 Ti1 1.9805(6) 5_565
Ti2 F9 1.7924(19) .
Ti2 F10 1.8335(16) .
Ti2 F7 1.8372(16) .
Ti2 F11 1.8412(16) .
Ti2 F8 1.8623(16) .
Ti2 F6 1.9683(5) .
F6 Ti2 1.9683(5) 2
Ti3 F14 1.768(3) .
Ti3 F15 1.798(3) .
Ti3 F16 1.8474(17) 6
Ti3 F16 1.8474(17) .
Ti3 F13 1.908(2) .
Ti3 F12 1.9770(8) .
F12 Ti3 1.9770(8) 5_556
C1 N1 1.318(3) .
C1 N2 1.318(4) .
C1 H1B 0.9500 .
N1 C3 1.362(4) .
N1 H1A 0.8800 .
C2 C3 1.342(4) .
C2 N2 1.368(4) .
C2 H2B 0.9500 .
C3 H3A 0.9500 .
N2 H2A 0.8800 .
N3 C11 1.315(4) .
N3 C10 1.367(4) .
N3 H02A 0.8800 .
N4 C11 1.319(4) .
N4 C12 1.370(4) .
N4 H02B 0.8800 .
C10 C12 1.339(4) .
C10 H03B 0.9500 .
C11 H03A 0.9500 .
C12 H02C 0.9500 .
C7 N6 1.324(9) .
C7 N5 1.363(8) .
C7 H7A 0.9500 .
N5 C8 1.410(10) .
N5 H5A 0.8800 .
C8 C9 1.231(10) .
C8 H8A 0.9500 .
C9 N6 1.360(13) .
C9 H9A 0.9500 .
N6 H6A 0.8800 .
C7A N5A 1.264(10) .
C7A N6A 1.342(12) .
C7A H7AA 0.9500 .
N5A C8A 1.492(11) .
N5A H5AA 0.8800 .
C8A C9A 1.294(10) .
C8A H8AA 0.9500 .
C9A N6A 1.307(13) .
C9A H9AA 0.9500 .
N6A H6AA 0.8800 .
