Adducts of Titanium Tetrachloride with Alkylselenium Compounds: Molecular Precursors to Titanium Diselenide Films
Peggy J. McKarns; T. Suren Lewkebandara; Glenn P. A. Yap; Louise M. Liable-Sands; Arnold L. Rheingold; Charles H. Winter; Inorganic Chemistry 37 (1998) 418–424; doi:10.1021/ic970945q

data_4322635
_publ_section_title
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 Adducts of Titanium Tetrachloride with Alkylselenium Compounds: Molecular
 Precursors to Titanium Diselenide Films
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              418
_journal_page_last               424
_journal_paper_doi               10.1021/ic970945q
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C4 H10 Cl8 Se2 Ti2'
_chemical_formula_weight         595.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.1060(10)
_cell_length_b                   12.1060(10)
_cell_length_c                   10.7860(10)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    238(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     1369.0(2)
_computing_cell_refinement       Siemens/XSCANS
_computing_data_collection       Siemens/XSCANS
_computing_data_reduction        Siemens/XSCANS
_computing_molecular_graphics    XP-5.03
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      238(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'omega scan'
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1746
_diffrn_reflns_theta_max         30.75
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        ,1
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.008
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.167
_exptl_crystal_description       plate
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       0.0147(12)
_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   1.271
_refine_ls_goodness_of_fit_obs   1.340
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.271
_refine_ls_restrained_S_obs      1.340
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_obs          0.0378
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0895
_refine_ls_wR_factor_obs         0.0885
_reflns_number_observed          1042
_reflns_number_total             1176
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970945q_2.cif
_cod_data_source_block           win21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] 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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322635