Preparation, Molecular and Electronic Structures, and Magnetic Properties of Face-Sharing Bioctahedral Titanium(III) Compounds: [PPh4][Ti2(μ-Cl)3Cl4(PR3)2]
Linfeng Chen; F. Albert Cotton; Kim R. Dunbar; Xuejun Feng; Robert A. Heintz; Calvin Uzelmeir; Inorganic Chemistry 35 (1996) 7358–7363; doi:10.1021/ic960636k

data_4323994
_publ_section_title
;
 Preparation, Molecular and Electronic Structures, and Magnetic Properties
 of Face-Sharing Bioctahedral Titanium(III) Compounds:
 [PPh4][Ti2(\m-Cl)3Cl4(PR3)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7358
_journal_page_last               7363
_journal_paper_doi               10.1021/ic960636k
_journal_volume                  35
_journal_year                    1996
_chemical_compound_source
;
reduction of TiCl4 with HSnBu3 followed by addition of [PPh4]Cl and then PMe2Ph
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C24 H20 P 1+,C16 H22 Cl7 Ti2 1-,C H2 Cl2'
_chemical_formula_structural
;
[(C6 H5)4 P] [Ti2 Cl7 (P (C6 H5) (C H3)2] C H2 Cl2
;
_chemical_formula_sum            'C41 H44 Cl9 P3 Ti2'
_chemical_formula_weight         1044.52
_chemical_name_systematic
; 
 (tetraphenylphosphonium) tetrachloro-tri-\m-chloro-
 bis(dimethylphenylphosphine)-dititanium 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                100.69(2)
_cell_angle_beta                 109.70(1)
_cell_angle_gamma                95.08(2)
_cell_formula_units_Z            2
_cell_length_a                   11.635(4)
_cell_length_b                   19.544(3)
_cell_length_c                   11.480(3)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.0
_cell_volume                     2382.6(11)
_computing_cell_refinement       Madnes
_computing_data_collection       'MicroVax 3900'
_computing_data_reduction        absurd
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius FAST'
_diffrn_measurement_method       'frame data from omega scans'
_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  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16789
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.095
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         7756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_obs          0.0496
_refine_ls_shift/esd_max         -0.038
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+5.0194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1363
_refine_ls_wR_factor_obs         0.1202
_reflns_number_observed          6728
_reflns_number_total             7853
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960636k_1.cif
_cod_data_source_block           '[Ph4P][Ti2Cl7(PMe2Ph)2].CH2Cl2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+5.0194P] 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^+5.0194P] 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        2383(1)
_cod_database_code               4323994