Tetrachloro[2-(phenylamino)pyridinato]titanate(IV) with a 2-(Phenylamino)pyridinium Counterion
Polamo, M.; Leskelä, M.; Acta Crystallographica Section C 52 (1996) 2975–2977; doi:10.1107/S0108270196010347

data_2005805
_publ_section_title
;
 Tetrachloro[2-(phenylamino)pyridinato]titanate(IV) with a
 2-(Phenylamino)pyridinium Counterion
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2975
_journal_page_last               2977
_journal_paper_doi               10.1107/S0108270196010347
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '(C11 H11 N2)[Ti Cl4 (C11 H9 N2)]'
_chemical_formula_structural     '[C11 H11 N2][Ti Cl4 (C11 H9 N2)]'
_chemical_formula_sum            'C22 H20 Cl4 N4 Ti'
_chemical_formula_weight         530.12
_chemical_name_common
;
2-(Phenylamino)pyridinium tetrachloro-2-(phenylamido)pyridinetitanate(IV)
;
_chemical_name_systematic
;
2-(Phenylamino)pyridinium tetrachloro(2-phenylaminopyridinato)titanate(IV)
;
_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
_cell_angle_alpha                94.18(13)
_cell_angle_beta                 90.27(15)
_cell_angle_gamma                118.44(9)
_cell_formula_units_Z            2
_cell_length_a                   9.580(15)
_cell_length_b                   9.652(12)
_cell_length_c                   14.625(19)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    193(1)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      3
_cell_volume                     1185(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
1993a)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1993b)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      193.0(10)
_diffrn_measurement_device       'Rigaku AFC-7S diffractometer'
_diffrn_measurement_method       '2\q-\w 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3546
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.68
_diffrn_standards_decay_%        1.3
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9107
_exptl_absorpt_correction_type   '\y scans (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.177
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_restrained_S_obs      1.177
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_obs          0.0667
_refine_ls_shift/esd_max         -0.007
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0461P)^2^+2.1081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1359
_refine_ls_wR_factor_obs         0.1248
_reflns_number_observed          2476
_reflns_number_total             3546
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            mu1287.cif
_cod_data_source_block           tiap
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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^)+(0.0461P)^2^+2.1081P] 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^)+(0.0461P)^2^+2.1081P] 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        1184(3)
_cod_database_code               2005805