Pentacarbonyl-2κ^5^<i>C</i>-chlorido-1κ<i>Cl</i>-bis[1(η^5^)-cyclopentadienyl](μ-α-oxidobenzylidene-1:2κ^2^<i>O</i>:<i>C</i>)titanium(IV)tungsten(0)
Esterhuysen, Catharine; Nel, I. B. Jacques; Esterhuysen, Matthias W.; Cronje, Stephanie; Acta Crystallographica Section E 64 (2008) m1534–; doi:10.1107/S1600536808036465

data_2220053
_publ_section_title
Pentacarbonyl-2\k^5^<i>C</i>-chlorido-1\k<i>Cl</i>-bis[1(\h^5^)-cyclopentadienyl](\m-\a-oxidobenzylidene-1:2\k^2^<i>O</i>:<i>C</i>)titanium(IV)tungsten(0)
_journal_coeditor_code           AT2672
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1534
_journal_paper_doi               10.1107/S1600536808036465
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ti W (C5 H5)2 (C7 H5 O) Cl (C O)5]'
_chemical_formula_moiety         'C22 H15 Cl O6 Ti W'
_chemical_formula_sum            'C22 H15 Cl O6 Ti W'
_chemical_formula_weight         642.54
_chemical_name_systematic
;
Pentacarbonyl-2\k^5^C-chlorido-1\kCl-bis[1(\h^5^)-cyclopentadienyl](\m-
\a-oxidobenzylidene-1:2\k^2^<i>O</i>:<i>C</i>)titaniumtungsten
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.9030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5530(10)
_cell_length_b                   12.2680(10)
_cell_length_c                   20.789(3)
_cell_measurement_reflns_used    3701
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.93
_cell_volume                     2169.8(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN(Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'X-SEED (Barbour, 2001; Atwood & Barbour, 2003)'
_computing_publication_material  'publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans to fill Ewald sphere'
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12664
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    5.825
_exptl_absorpt_correction_T_max  0.542
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.049
_refine_diff_density_min         -1.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+1.3791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                3701
_reflns_number_total             4270
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2672.cif
_cod_data_source_block           I
_cod_original_cell_volume        2169.8(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2220053
_cod_database_fobs_code          2220053