Addition compounds of titanium tetrachloride with aromatic nitrogen bases
Hensen, Karl; Lemke, Alexander; Bolte, Michael; Acta Crystallographica Section C 55 (1999) 863–867; doi:10.1107/S0108270199000554

data_2008633
_publ_section_title
;
 Addition compounds of titanium tetrachloride with aromatic nitrogen
 bases
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              863
_journal_page_last               867
_journal_paper_doi               10.1107/S0108270199000554
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac
'(C4 H7 N2 )4 [TiCl5 (C4 H6 N2 )]2[TiCl6 ] '
_chemical_formula_sum            'C24 H40 Cl16 N12 Ti3'
_chemical_formula_weight         1207.58
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.5400(10)
_cell_angle_beta                 93.7840(10)
_cell_angle_gamma                99.5510(10)
_cell_formula_units_Z            1
_cell_length_a                   7.8998(2)
_cell_length_b                   9.9722(3)
_cell_length_c                   16.0448(5)
_cell_measurement_reflns_used    6449
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.00
_cell_volume                     1179.43(6)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP (Siemens, 1991)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.882
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device       'Siemens CCD three circle diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'highly oriented graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12610
_diffrn_reflns_theta_full        26.16
_diffrn_reflns_theta_max         26.16
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  1000
_diffrn_standards_number         162
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_T_max  0.8695
_exptl_absorpt_correction_T_min  0.7618
_exptl_absorpt_correction_type   'Empirical (SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.578
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0463
_refine_ls_R_factor_obs          .0463
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0291P)^2^+1.2599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .0933
_refine_ls_wR_factor_obs         .0823
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                2938
_reflns_number_total             4155
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1252.cif
_cod_data_source_block           III
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0291P)^2^+1.2599P] 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^)+(0.0291P)^2^+1.2599P] where P=(Fo^2^+2Fc^2^)/3'.

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

2019-10-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C12 H20 Cl8 N6 Ti1.5'
_cod_original_formula_weight         603.79
_cod_original_formula_iupac
'(C4 H7 N2 )2 [TiCl5 (C4 H6 N2 )][TiCl6 ]0.5 '
_cod_original_formula_units_Z            2
_cod_database_code               2008633