#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:51:50 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179458 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/55/4335516.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_4335516
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           2
_symmetry_cell_setting           triclinic
_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_date             2013-06-05T12:44:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                118.808(8)
_cell_angle_beta                 92.366(3)
_cell_angle_gamma                113.595(8)
_cell_formula_units_Z            1
_cell_length_a                   8.791(3)
_cell_length_b                   9.971(4)
_cell_length_c                   10.126(4)
_cell_measurement_reflns_used    554
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.5511
_cell_measurement_theta_min      2.4243
_cell_volume                     681.7(5)
_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 0.974
_diffrn_measured_fraction_theta_max 0.812
_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  0.0238
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6582
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.23
_diffrn_reflns_theta_min         2.4
_exptl_absorpt_coefficient_mu    1.288
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing R.H., 1995'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_description       Block
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.578
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3002
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0466
_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)+(0.0461P)²+1.3228P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                2760
_reflns_number_total             3002
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic302468j_si_002_4.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        681.8(5)
_cod_database_code               4335516
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Ti1 Ti 0.20646(7) 0.00261(7) 0.32071(6) 0.02162(15) Uani 1 1 d .
Ti2 Ti 0.17948(7) 0.37283(7) 0.68269(6) 0.02238(16) Uani 1 1 d .
F1 F 0.1361(3) 0.1591(3) 0.4806(2) 0.0354(5) Uani 1 1 d .
F2 F -0.0065(3) -0.1994(2) 0.2824(2) 0.0331(4) Uani 1 1 d .
F5 F 0.3998(3) 0.1885(3) 0.3582(2) 0.0359(5) Uani 1 1 d .
F3 F 0.0770(3) 0.0031(2) 0.1778(2) 0.0317(4) Uani 1 1 d .
F4 F 0.2627(3) -0.1488(3) 0.1695(2) 0.0336(4) Uani 1 1 d .
F6 F 0.3047(3) -0.0073(3) 0.4776(2) 0.0319(4) Uani 1 1 d .
F7 F -0.0049(3) 0.3624(3) 0.5803(2) 0.0370(5) Uani 1 1 d .
F10 F 0.3404(3) 0.3490(3) 0.7716(3) 0.0401(5) Uani 1 1 d .
F8 F 0.3305(3) 0.5070(3) 0.6284(3) 0.0418(5) Uani 1 1 d .
F9 F 0.1948(3) 0.5492(3) 0.8690(2) 0.0403(5) Uani 1 1 d .
C1 C 0.6611(5) 0.3476(4) 0.6850(4) 0.0369(8) Uani 1 1 d D
H5 H 0.5975 0.2266 0.6216 0.044 Uiso 1 1 calc R
N1 N 0.7498(4) 0.4390(4) 0.8327(4) 0.0370(7) Uani 1 1 d D
H1 H 0.7597 0.3971 0.8876 0.044 Uiso 1 1 calc R
C2 C 0.7784(6) 0.6212(5) 0.7663(5) 0.0460(9) Uani 1 1 d D
H6 H 0.8097 0.7227 0.7674 0.055 Uiso 1 1 calc R
C3 C 0.8241(5) 0.6109(5) 0.8860(5) 0.0449(9) Uani 1 1 d D
H7 H 0.8940 0.7039 0.9874 0.054 Uiso 1 1 calc R
N2 N 0.6767(4) 0.4547(4) 0.6413(3) 0.0389(7) Uani 1 1 d D
H2 H 0.6303 0.4249 0.5485 0.047 Uiso 1 1 calc RD
C4 C 0.7928(5) 0.1835(6) 0.2529(5) 0.0454(9) Uani 1 1 d D
H8 H 0.8549 0.3017 0.3314 0.054 Uiso 1 1 calc R
N3 N 0.7372(4) 0.1153(4) 0.1001(4) 0.0383(7) Uani 1 1 d D
H3 H 0.7526 0.1742 0.0571 0.046 Uiso 1 1 calc R
C5 C 0.6565(6) -0.1004(6) 0.1314(6) 0.0489(10) Uani 1 1 d D
H9 H 0.6087 -0.2111 0.1145 0.059 Uiso 1 1 calc R
C6 C 0.6523(5) -0.0618(5) 0.0213(4) 0.0388(8) Uani 1 1 d D
H10 H 0.6015 -0.1404 -0.0869 0.047 Uiso 1 1 calc R
N4 N 0.7447(5) 0.0554(5) 0.2728(4) 0.0490(9) Uani 1 1 d D
H4 H 0.7654 0.0667 0.3623 0.059 Uiso 1 1 calc RD
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_3
F5 Ti1 F3 93.95(10) .
F5 Ti1 F4 92.40(10) .
F3 Ti1 F4 92.37(10) .
F5 Ti1 F6 93.67(10) .
F3 Ti1 F6 170.14(10) .
F4 Ti1 F6 93.55(9) .
F5 Ti1 F1 89.71(10) .
F3 Ti1 F1 86.70(10) .
F4 Ti1 F1 177.75(10) .
F6 Ti1 F1 87.09(9) .
F5 Ti1 F2 179.14(9) .
F3 Ti1 F2 86.22(9) .
F4 Ti1 F2 88.43(10) .
F6 Ti1 F2 86.07(9) .
F1 Ti1 F2 89.46(9) .
F8 Ti2 F10 94.02(11) .
F8 Ti2 F9 96.48(11) .
F10 Ti2 F9 93.06(11) .
F8 Ti2 F7 92.43(11) .
F10 Ti2 F7 171.41(10) .
F9 Ti2 F7 91.85(10) .
F8 Ti2 F1 90.58(10) .
F10 Ti2 F1 88.11(10) .
F9 Ti2 F1 172.74(10) .
F7 Ti2 F1 86.15(10) .
F8 Ti2 F2 173.08(10) 2_556
F10 Ti2 F2 86.17(10) 2_556
F9 Ti2 F2 90.41(10) 2_556
F7 Ti2 F2 86.74(10) 2_556
F1 Ti2 F2 82.51(9) 2_556
Ti1 F1 Ti2 154.16(13) .
Ti1 F2 Ti2 160.53(12) 2_556
N1 C1 N2 108.4(3) .
N1 C1 H5 125.8 .
N2 C1 H5 125.8 .
C1 N1 C3 109.0(3) .
C1 N1 H1 125.5 .
C3 N1 H1 125.5 .
C3 C2 N2 106.7(3) .
C3 C2 H6 126.6 .
N2 C2 H6 126.6 .
C2 C3 N1 107.0(3) .
C2 C3 H7 126.5 .
N1 C3 H7 126.5 .
C1 N2 C2 108.9(3) .
C1 N2 H2 125.5 .
C2 N2 H2 125.5 .
N4 C4 N3 107.3(4) .
N4 C4 H8 126.3 .
N3 C4 H8 126.3 .
C4 N3 C6 109.8(3) .
C4 N3 H3 125.1 .
C6 N3 H3 125.1 .
C6 C5 N4 106.3(4) .
C6 C5 H9 126.8 .
N4 C5 H9 126.8 .
C5 C6 N3 106.1(4) .
C5 C6 H10 126.9 .
N3 C6 H10 126.9 .
C4 N4 C5 110.4(3) .
C4 N4 H4 124.8 .
C5 N4 H4 124.8 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 F5 1.793(2) .
Ti1 F3 1.8066(19) .
Ti1 F4 1.8169(19) .
Ti1 F6 1.8403(19) .
Ti1 F1 1.965(2) .
Ti1 F2 1.970(2) .
Ti2 F8 1.790(2) .
Ti2 F10 1.800(2) .
Ti2 F9 1.806(2) .
Ti2 F7 1.826(2) .
Ti2 F1 1.989(2) .
Ti2 F2 1.989(2) 2_556
F2 Ti2 1.9889(19) 2_556
C1 N1 1.302(5) .
C1 N2 1.303(5) .
C1 H5 0.9300 .
N1 C3 1.356(5) .
N1 H1 0.8600 .
C2 C3 1.325(6) .
C2 N2 1.361(5) .
C2 H6 0.9300 .
C3 H7 0.9300 .
N2 H2 0.8600 .
C4 N4 1.294(6) .
C4 N3 1.324(5) .
C4 H8 0.9300 .
N3 C6 1.360(5) .
N3 H3 0.8600 .
C5 C6 1.347(5) .
C5 N4 1.365(6) .
C5 H9 0.9300 .
C6 H10 0.9300 .
N4 H4 0.8600 .
