4-Methylpyridinium Pentachloro(4-methylpyridine-<i>N</i>)titanate(IV) Acetonitrile Solvate at 143K
Hensen, Karl; Pickel, Peter; Lemke, Alexander; Bolte, Michael; Acta Crystallographica Section C 53 (1997) 1583–1585; doi:10.1107/S0108270197008949

data_2006731
_publ_section_title
;
 4-Methylpyridinium Pentachloro(4-methylpyridine-<i>N</i>)titanate(IV)
 Acetonitrile Solvate at 143K
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1583
_journal_page_last               1585
_journal_paper_doi               10.1107/S0108270197008949
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '(C6 H8 N) [Ti Cl5 (C6 H7 N)] , C2 H3 N'
_chemical_formula_moiety         'C6 H7 Cl5 N1 Ti1+,C6 H8 N1 -,C2 H3 N1'
_chemical_formula_sum            'C14 H18 Cl5 N3 Ti'
_chemical_formula_weight         453.46
_chemical_name_systematic
;
N-Hydro-4-methylpyridinium Pentachloro(4-methylpyridino)titanate(IV)
Acetonitrile at 143K
;
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.18070(10)
_cell_length_b                   10.8165(2)
_cell_length_c                   12.6864(2)
_cell_measurement_reflns_used    4007
_cell_measurement_temperature    143
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.00
_cell_volume                     985.35(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP SHELXTL-Plus (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL96 (Sheldrick, 1996b)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143
_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  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7873
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   'Empirical, SADABS (Sheldrick,1996a)'
_exptl_crystal_colour            'light yellow transparent'
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.366
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2130
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_obs          .0379
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0304P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0735
_refine_ls_wR_factor_obs         .0681
_reflns_number_observed          1780
_reflns_number_total             2130
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sk1120.cif
_cod_data_source_block           he15
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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:

'_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^)+(0.0304P)^2^] 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^)+(0.0304P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C14 H18 Cl5 N3 Ti1'
_cod_database_code               2006731
_cod_database_fobs_code          2006731