Labile adducts of TiCl4 with thionyl chloride structurally characterized at low temperature: a comparison with the zirconium and hafnium analogues, [MCl4(SOCl2)]2
Calderazzo, Fausto; D'Attoma, Michele; Marchetti, Fabio; Pampaloni, Guido; Troyanov, Sergei I.; Journal of the Chemical Society, Dalton Transactions  (1999) 2275–; doi:10.1039/a904186i

data_7027573
_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
\b-Di-\m-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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0499P)^2^+0.5341P] where P=(Fo^2^+2Fc^2^)/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