#------------------------------------------------------------------------------
#$Date: 2016-08-07 12:09:04 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185451 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/91/7039126.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_7039126
loop_
_publ_author_name
'Marshall, Kayleigh L.'
'Wang, Qianlong'
'Sullivan, Hannah S. I.'
'Weller, Mark T.'
_publ_section_title
;
 Synthesis and structural characterisation of transition metal fluoride
 sulfates.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8854
_journal_page_last               8861
_journal_paper_doi               10.1039/c6dt00582a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C10 H10 F2 N2 O8 S2 Ti'
_chemical_formula_weight         436.22
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-02-08 deposited with the CCDC.
2016-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                112.888(7)
_cell_angle_beta                 95.196(6)
_cell_angle_gamma                98.706(5)
_cell_formula_units_Z            1
_cell_length_a                   4.5768(3)
_cell_length_b                   8.9162(6)
_cell_length_c                   10.1236(9)
_cell_measurement_reflns_used    2452
_cell_measurement_temperature    150.2(5)
_cell_measurement_theta_max      28.9690
_cell_measurement_theta_min      4.5500
_cell_volume                     371.11(5)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150.2(5)
_diffrn_detector_area_resol_mean 8.0734
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.867
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5670
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.383
_diffrn_reflns_theta_min         3.990
_diffrn_source                   'Enhance (Mo) X-ray source'
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_description       Prism
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0376P)²+0.1920P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1520
_reflns_number_total             1772
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt00582a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7039123--7039127.cif.'
_cod_database_code               7039126
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ti1 Ti 0.0000 0.0000 0.0000 0.00962(15) Uani 1 2 d S . P
S2 S 0.50091(12) 0.11616(6) -0.16474(6) 0.01096(14) Uani 1 1 d . . .
F1 F 0.0766(3) -0.18690(15) -0.13604(13) 0.0153(3) Uani 1 1 d . . .
O2 O 0.3011(3) 0.14139(18) -0.05120(16) 0.0143(3) Uani 1 1 d . . .
O1 O 0.3073(3) 0.00166(18) 0.14924(16) 0.0128(3) Uani 1 1 d . . .
O4 O 0.6903(4) 0.27790(19) -0.12852(18) 0.0189(4) Uani 1 1 d . . .
N1 N 1.0723(4) 0.3575(2) -0.2886(2) 0.0150(4) Uani 1 1 d . . .
C1 C 1.0366(6) 0.2646(3) -0.4316(3) 0.0222(5) Uani 1 1 d . . .
H1 H 0.8984 0.1643 -0.4730 0.027 Uiso 1 1 calc R U .
O5 O 0.6728(4) -0.0421(2) 0.30810(18) 0.0242(4) Uani 1 1 d . . .
C4 C 1.4105(5) 0.4685(3) -0.4546(2) 0.0117(4) Uani 1 1 d . . .
C6 C 1.2695(5) 0.5009(3) -0.2240(3) 0.0189(5) Uani 1 1 d . . .
H2 H 1.2923 0.5612 -0.1240 0.023 Uiso 1 1 calc R U .
C3 C 1.2041(6) 0.3173(3) -0.5175(3) 0.0209(5) Uani 1 1 d . . .
H3 H 1.1800 0.2528 -0.6168 0.025 Uiso 1 1 calc R U .
C5 C 1.4397(5) 0.5596(3) -0.3058(3) 0.0194(5) Uani 1 1 d . . .
H4 H 1.5750 0.6608 -0.2610 0.023 Uiso 1 1 calc R U .
H5 H 0.963(7) 0.325(4) -0.242(3) 0.032(9) Uiso 1 1 d . . .
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'
H H 0.0000 0.0000 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
F F 0.0171 0.0103 '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
F1 Ti1 F1 180.0 2 .
F1 Ti1 O1 87.68(6) 2 .
F1 Ti1 O1 92.32(6) . .
F1 Ti1 O1 92.32(6) 2 2
F1 Ti1 O1 87.68(6) . 2
O1 Ti1 O1 180.00(7) . 2
F1 Ti1 O2 88.47(6) 2 .
F1 Ti1 O2 91.53(6) . .
O1 Ti1 O2 89.38(6) . .
O1 Ti1 O2 90.62(6) 2 .
F1 Ti1 O2 91.54(6) 2 2
F1 Ti1 O2 88.47(6) . 2
O1 Ti1 O2 90.62(6) . 2
O1 Ti1 O2 89.38(6) 2 2
O2 Ti1 O2 180.0 . 2
O5 S2 O4 114.46(11) 2_655 .
O5 S2 O2 110.87(10) 2_655 .
O4 S2 O2 106.28(9) . .
O5 S2 O1 108.75(10) 2_655 2_655
O4 S2 O1 109.39(9) . 2_655
O2 S2 O1 106.81(9) . 2_655
S2 O2 Ti1 136.64(9) . .
S2 O1 Ti1 136.60(9) 2_655 .
C6 N1 C1 122.2(2) . .
N1 C1 C3 120.1(2) . .
C5 C4 C3 118.0(2) . .
C5 C4 C4 121.1(2) . 2_864
C3 C4 C4 120.9(2) . 2_864
N1 C6 C5 119.7(2) . .
C1 C3 C4 119.6(2) . .
C6 C5 C4 120.4(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 F1 1.8099(12) 2
Ti1 F1 1.8099(12) .
Ti1 O1 1.9627(15) .
Ti1 O1 1.9627(15) 2
Ti1 O2 1.9668(15) .
Ti1 O2 1.9668(15) 2
S2 O5 1.4357(17) 2_655
S2 O4 1.4554(16) .
S2 O2 1.5033(15) .
S2 O1 1.5104(15) 2_655
O1 S2 1.5104(15) 2_655
N1 C6 1.330(3) .
N1 C1 1.339(3) .
C1 C3 1.377(3) .
O5 S2 1.4357(17) 2_655
C4 C5 1.388(3) .
C4 C3 1.397(3) .
C4 C4 1.493(4) 2_864
C6 C5 1.377(3) .
