Reactivity of SeOCl2 with titanium and zirconium tetrachlorides. The unexpected formation of a μ-oxo-bridged titanium(IV) derivative
Fausto Calderazzo; Michele D'Attoma; Fabio Marchetti; Guido Pampaloni; J. Chem. Soc., Dalton Trans.  (2000) 2497–2498; doi:10.1039/b004057f

data_7009859
_publ_section_title
;
 Reactivity of SeOCl2 with titanium and zirconium tetrachlorides. The
 unexpected formation of a \m-oxo-bridged titanium(IV) derivative
;
_journal_issue                   15
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              2497
_journal_page_last               2498
_journal_paper_doi               10.1039/b004057f
_journal_year                    2000
_chemical_formula_moiety         \m-O(TiCl3(OSeCl2)2)2.CH2Cl2
_chemical_formula_sum            'C H2 Cl16 O5 Se4 Ti2'
_chemical_formula_weight         1072.87
_chemical_name_systematic
;

Oxobis[trichlorobis(seleninylchloride)titanium(IV)] dichloromethane solvate

;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.58(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7530(10)
_cell_length_b                   8.4950(5)
_cell_length_c                   13.3500(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.96
_cell_measurement_theta_min      5.77
_cell_volume                     1439.44(18)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3327
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        '< 1'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.112
_exptl_absorpt_correction_T_max  0.5871
_exptl_absorpt_correction_T_min  0.3036
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'Light yellow'
_exptl_crystal_density_diffrn    2.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Prismatic stick'
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.67_mm
_exptl_crystal_size_mid          0.17_mm
_exptl_crystal_size_min          0.08_mm
_refine_diff_density_max         0.658
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0404
_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/[\s^2^(Fo^2^)+(0.0341P)^2^+2.6867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                1862
_reflns_number_total             2538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004057f.txt
_cod_data_source_block           tic
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Integration' changed
to 'integration' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               7009859