#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:09:19 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179525 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/22/4342219.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_4342219
loop_
_publ_author_name
'Gautier, Romain'
'Gautier, Régis'
'Chang, Kelvin B.'
'Poeppelmeier, Kenneth R.'
_publ_section_title
;
 On the Origin of the Differences in Structure Directing Properties of
 Polar Metal Oxyfluoride [MOxF6-x](2-) (x = 1, 2) Building Units.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1712
_journal_page_last               1719
_journal_paper_doi               10.1021/ic5026735
_journal_volume                  54
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C10 H10 N2, F6 Ti'
_chemical_formula_sum            'C10 H10 F6 N2 Ti'
_chemical_formula_weight         320.1
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      72
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-02-01T15:04:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0963(5)
_cell_length_b                   11.8413(6)
_cell_length_c                   13.1477(9)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1104.79(12)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.963
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5063
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         36.28
_diffrn_reflns_theta_min         3.1
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.476
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.931
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         1329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.072
_refine_ls_R_factor_gt           0.054
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0494P)²+2.8452P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                995
_reflns_number_total             1329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5026735_si_001.cif
_cod_data_source_block           rg22e_0m
_cod_depositor_comments
'Adding full bibliography for 4342215--4342219.cif.'
_cod_database_code               4342219
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-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
Ti1 Ti 0 0 0.5 0.00993(16) Uani 1 4 d S
F2 F -0.2256(2) 0.07853(15) 0.5 0.0174(4) Uani 1 2 d S
F3 F 0.1303(2) 0.13521(13) 0.5 0.0140(3) Uani 1 2 d S
F1 F 0 0 0.35642(15) 0.0171(4) Uani 1 2 d S
C3 C 0 0.4373(2) 0.25 0.0114(4) Uani 1 2 d S
N1 N 0 0.2079(2) 0.25 0.0312(8) Uani 1 2 d S
H1A H 0 0.1352 0.25 0.047 Uiso 1 2 calc SR
C2 C -0.0630(3) 0.37856(17) 0.33488(18) 0.0170(4) Uani 1 1 d .
H2B H -0.1036 0.4171 0.3925 0.026 Uiso 1 1 calc R
C1 C -0.0642(3) 0.2619(2) 0.3323(2) 0.0276(6) Uani 1 1 d .
H1B H -0.1095 0.2212 0.3876 0.041 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0135(3) 0.0062(2) 0.0101(3) 0 0 0.0005(2)
F2 0.0154(8) 0.0122(7) 0.0248(10) 0 0 0.0030(6)
F3 0.0168(8) 0.0080(6) 0.0172(9) 0 0 -0.0027(6)
F1 0.0309(10) 0.0103(6) 0.0101(8) 0 0 -0.0008(7)
C3 0.0103(10) 0.0095(8) 0.0143(12) 0 -0.0021(10) 0
N1 0.0165(11) 0.0077(9) 0.069(3) 0 -0.0125(15) 0
C2 0.0144(8) 0.0158(8) 0.0209(11) 0.0075(7) -0.0004(8) -0.0004(7)
C1 0.0172(9) 0.0177(9) 0.0480(17) 0.0191(10) -0.0088(10) -0.0044(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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 180 . 9_556
F3 Ti1 F2 90.15(8) . 9_556
F3 Ti1 F2 89.85(8) 9_556 9_556
F3 Ti1 F2 89.85(8) . .
F3 Ti1 F2 90.15(8) 9_556 .
F2 Ti1 F2 180 9_556 .
F3 Ti1 F1 90 . 9_556
F3 Ti1 F1 90 9_556 9_556
F2 Ti1 F1 90 9_556 9_556
F2 Ti1 F1 90 . 9_556
F3 Ti1 F1 90 . .
F3 Ti1 F1 90 9_556 .
F2 Ti1 F1 90 9_556 .
F2 Ti1 F1 90 . .
F1 Ti1 F1 180 9_556 .
C2 C3 C2 119.9(3) 4 .
C2 C3 C3 120.04(13) 4 2_565
C2 C3 C3 120.04(13) . 2_565
C1 N1 C1 122.8(3) 4 .
C1 N1 H1A 118.6 4 .
C1 N1 H1A 118.6 . .
C1 C2 C3 118.9(2) . .
C1 C2 H2B 120.6 . .
C3 C2 H2B 120.6 . .
N1 C1 C2 119.8(2) . .
N1 C1 H1B 120.1 . .
C2 C1 H1B 120.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 F3 1.8488(16) .
Ti1 F3 1.8488(16) 9_556
Ti1 F2 1.8514(17) 9_556
Ti1 F2 1.8514(17) .
Ti1 F1 1.8878(19) 9_556
Ti1 F1 1.8878(19) .
C3 C2 1.389(2) 4
C3 C2 1.389(2) .
C3 C3 1.486(5) 2_565
N1 C1 1.337(3) 4
N1 C1 1.337(3) .
N1 H1A 0.86 .
C2 C1 1.381(3) .
C2 H2B 0.93 .
C1 H1B 0.93 .
