#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:38:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179981 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/75/7027573.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027573
loop_
_publ_author_name
'Calderazzo, Fausto'
'D'Attoma, Michele'
'Marchetti, Fabio'
'Pampaloni, Guido'
'Troyanov, Sergei I.'
_publ_section_title
;
 Labile adducts of TiCl4 with thionyl chloride structurally characterized
 at low temperature: a comparison with the zirconium and hafnium
 analogues, [MCl4(SOCl2)]2
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2275
_journal_paper_doi               10.1039/a904186i
_journal_year                    1999
_chemical_formula_sum            'Cl12 O2 S2 Ti2'
_chemical_formula_weight         617.32
_chemical_name_common
β-Di-μ-chlorotrichloro-bis-(thionylchloride)dititanium(iv)
_chemical_name_systematic
; 
 ? 
;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                107.73(4)
_cell_angle_beta                 91.33(4)
_cell_angle_gamma                112.77(4)
_cell_formula_units_Z            1
_cell_length_a                   6.179(3)
_cell_length_b                   7.675(4)
_cell_length_c                   10.714(7)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      18
_cell_volume                     440.5(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measurement_device       STADI-4
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1827
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    2.948
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.327
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0150(27)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.114
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.328
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_obs          0.0333
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0499P)²+0.5341P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1110
_refine_ls_wR_factor_obs         0.0837
_reflns_number_observed          1318
_reflns_number_total             1827
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904186Isup1.cif
_cod_data_source_block           TiCl4SOCl2_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.5341P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.5341P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        440.5(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027573
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ti 0.0170(4) 0.0135(4) 0.0125(4) 0.0016(3) 0.0001(3) 0.0065(3)
Cl1 0.0185(5) 0.0153(5) 0.0129(4) 0.0031(3) 0.0017(4) 0.0043(4)
Cl2 0.0203(5) 0.0149(5) 0.0212(5) 0.0008(4) 0.0001(4) 0.0040(4)
Cl3 0.0272(5) 0.0275(5) 0.0154(5) 0.0036(4) 0.0059(4) 0.0126(4)
Cl4 0.0234(5) 0.0227(5) 0.0280(5) 0.0080(4) -0.0006(4) 0.0124(4)
Cl5 0.0275(6) 0.0283(5) 0.0142(5) -0.0008(4) -0.0029(4) 0.0126(4)
Cl6 0.0274(6) 0.0231(5) 0.0284(6) 0.0127(4) 0.0026(4) 0.0083(4)
S 0.0211(5) 0.0182(5) 0.0139(5) 0.0034(4) 0.0005(4) 0.0104(4)
O 0.0180(14) 0.0196(14) 0.0139(13) 0.0044(11) -0.0003(11) 0.0078(11)
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
Ti Ti 0.07585(11) 0.23810(9) 0.14571(6) 0.0150(2) Uani 1 d
Cl1 Cl 0.2077(2) 0.11570(13) -0.06559(8) 0.0169(2) Uani 1 d
Cl2 Cl 0.4038(2) 0.51962(13) 0.19433(9) 0.0213(3) Uani 1 d
Cl3 Cl -0.0345(2) 0.27793(15) 0.34492(9) 0.0238(3) Uani 1 d
Cl4 Cl -0.1727(2) 0.32380(14) 0.05924(10) 0.0240(3) Uani 1 d
Cl5 Cl 0.4541(2) 0.22868(15) 0.48692(9) 0.0251(3) Uani 1 d
Cl6 Cl 0.0511(2) -0.18159(15) 0.32902(10) 0.0261(3) Uani 1 d
S S 0.3623(2) 0.01666(14) 0.30093(9) 0.0176(3) Uani 1 d
O O 0.3045(4) 0.1052(4) 0.2096(2) 0.0175(6) Uani 1 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Cl Cl 0.1484 0.1585 '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'
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
Cl4 Ti Cl2 99.99(6) . .
Cl4 Ti Cl3 97.77(6) . .
Cl2 Ti Cl3 99.61(7) . .
Cl4 Ti O 171.29(8) . .
Cl2 Ti O 86.57(9) . .
Cl3 Ti O 86.66(8) . .
Cl4 Ti Cl1 91.40(6) . 2
Cl2 Ti Cl1 163.44(5) . 2
Cl3 Ti Cl1 90.62(6) . 2
O Ti Cl1 81.02(9) . 2
Cl4 Ti Cl1 94.42(6) . .
Cl2 Ti Cl1 87.56(7) . .
Cl3 Ti Cl1 164.54(5) . .
O Ti Cl1 80.07(8) . .
Cl1 Ti Cl1 79.56(6) 2 .
Ti Cl1 Ti 100.44(6) 2 .
O S Cl5 106.93(12) . .
O S Cl6 107.74(12) . .
Cl5 S Cl6 97.76(8) . .
S O Ti 148.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti Cl4 2.1765(15) .
Ti Cl2 2.219(2) .
Ti Cl3 2.224(2) .
Ti O 2.236(3) .
Ti Cl1 2.451(2) 2
Ti Cl1 2.460(2) .
Cl1 Ti 2.451(2) 2
Cl5 S 2.049(2) .
Cl6 S 2.036(2) .
S O 1.457(3) .
