#------------------------------------------------------------------------------
#$Date: 2019-10-28 09:23:29 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219800 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/86/2008633.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2008633
loop_
_publ_author_name
'Hensen, Karl'
'Lemke, Alexander'
'Bolte, Michael'
_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       ω
_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/[σ²(Fo²)+(0.0291P)²+1.2599P] where P=(Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ti1 .20585(9) .32310(8) .13327(5) .01949(18) Uani d . 1 . . Ti
Cl1 .46430(14) .39575(11) .22445(7) .0299(3) Uani d . 1 . . Cl
Cl2 .15040(14) .11212(11) .16810(7) .0264(3) Uani d . 1 . . Cl
Cl3 .29291(13) .51583(10) .07747(6) .0246(2) Uani d . 1 . . Cl
Cl4 -.04572(13) .25393(11) .03555(6) .0251(2) Uani d . 1 . . Cl
Cl5 .06205(14) .44744(11) .24240(7) .0300(3) Uani d . 1 . . Cl
N11 .3307(4) .2026(3) .0272(2) .0196(8) Uani d . 1 . . N
C12 .2522(5) .0907(4) -.0405(3) .0213(9) Uani d . 1 . . C
H12 .1315 .0525 -.0499 .026 Uiso calc R 1 . . H
N13 .3665(4) .0386(3) -.0942(2) .0216(8) Uani d . 1 . . N
C13 .3261(6) -.0848(5) -.1748(3) .0315(11) Uani d . 1 . . C
H13A .2309 -.1557 -.1679 .047 Uiso calc R 1 . . H
H13B .4284 -.1281 -.1861 .047 Uiso calc R 1 . . H
H13C .2919 -.0531 -.2245 .047 Uiso calc R 1 . . H
C14 .5265(5) .1218(5) -.0591(3) .0266(10) Uani d . 1 . . C
H14 .6325 .1109 -.0825 .032 Uiso calc R 1 . . H
C15 .5043(5) .2222(4) .0153(3) .0244(10) Uani d . 1 . . C
H15 .5935 .2948 .0535 .029 Uiso calc R 1 . . H
N21 .7180(5) .6515(4) .1425(2) .0345(9) Uani d . 1 . . N
H21 .6386 .5964 .0992 .041 Uiso calc R 1 . . H
C22 .8874(6) .6663(4) .1409(3) .0282(10) Uani d . 1 . . C
H22 .9435 .6180 .0934 .034 Uiso calc R 1 . . H
N23 .9651(4) .7598(3) .2165(2) .0219(8) Uani d . 1 . . N
C23 1.1510(5) .8059(5) .2407(3) .0326(11) Uani d . 1 . . C
H23A 1.2101 .7675 .1894 .049 Uiso calc R 1 . . H
H23B 1.1875 .7705 .2883 .049 Uiso calc R 1 . . H
H23C 1.1809 .9109 .2605 .049 Uiso calc R 1 . . H
C24 .8412(6) .8036(5) .2688(3) .0332(11) Uani d . 1 . . C
H24 .8609 .8693 .3270 .040 Uiso calc R 1 . . H
C25 .6864(6) .7357(5) .2223(3) .0369(12) Uani d . 1 . . C
H25 .5763 .7445 .2413 .044 Uiso calc R 1 . . H
N31 .3057(5) .5901(4) .5267(3) .0396(10) Uani d . 1 . . N
H31 .3694 .6751 .5342 .048 Uiso calc R 1 . . H
C32 .2710(6) .4826(5) .4514(3) .0347(11) Uani d . 1 . . C
H32 .3105 .4841 .3970 .042 Uiso calc R 1 . . H
N33 .1718(5) .3729(4) .4654(2) .0299(9) Uani d . 1 . . N
C33 .1040(7) .2320(5) .3993(3) .0437(13) Uani d . 1 . . C
H33A .1311 .2352 .3411 .066 Uiso calc R 1 . . H
H33B -.0216 .2078 .3983 .066 Uiso calc R 1 . . H
H33C .1575 .1591 .4144 .066 Uiso calc R 1 . . H
C34 .1432(6) .4129(5) .5521(3) .0343(12) Uani d . 1 . . C
H34 .0760 .3551 .5801 .041 Uiso calc R 1 . . H
C35 .2276(6) .5487(5) .5901(3) .0375(12) Uani d . 1 . . C
H35 .2319 .6050 .6500 .045 Uiso calc R 1 . . H
Ti2 .5000 1.0000 .5000 .0268(3) Uani d S 1 . . Ti
Cl21 .49886(15) 1.07407(13) .37399(7) .0359(3) Uani d . 1 . . Cl
Cl22 .19956(14) .93235(14) .47824(8) .0412(3) Uani d . 1 . . Cl
Cl23 .52107(17) .76923(13) .41544(8) .0422(3) Uani d . 1 . . Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N11 Ti1 Cl1 . . 90.26(9) y
N11 Ti1 Cl5 . . 177.59(10) y
Cl1 Ti1 Cl5 . . 92.14(5) y
N11 Ti1 Cl4 . . 87.59(9) y
Cl1 Ti1 Cl4 . . 176.73(5) y
Cl5 Ti1 Cl4 . . 90.02(4) y
N11 Ti1 Cl2 . . 84.99(9) y
Cl1 Ti1 Cl2 . . 90.68(4) y
Cl5 Ti1 Cl2 . . 94.78(4) y
Cl4 Ti1 Cl2 . . 91.59(4) y
N11 Ti1 Cl3 . . 84.28(9) y
Cl1 Ti1 Cl3 . . 88.38(4) y
Cl5 Ti1 Cl3 . . 95.98(4) y
Cl4 Ti1 Cl3 . . 88.96(4) y
Cl2 Ti1 Cl3 . . 169.22(5) y
C12 N11 C15 . . 105.7(3) ?
C12 N11 Ti1 . . 125.5(3) ?
C15 N11 Ti1 . . 128.7(3) ?
N11 C12 N13 . . 110.9(3) ?
C12 N13 C14 . . 107.4(3) ?
C12 N13 C13 . . 126.0(3) ?
C14 N13 C13 . . 126.7(3) ?
C15 C14 N13 . . 106.8(4) ?
C14 C15 N11 . . 109.2(4) ?
C22 N21 C25 . . 108.9(4) ?
N23 C22 N21 . . 108.4(4) ?
C22 N23 C24 . . 108.7(4) ?
C22 N23 C23 . . 125.5(4) ?
C24 N23 C23 . . 125.8(4) ?
C25 C24 N23 . . 107.1(4) ?
C24 C25 N21 . . 107.0(4) ?
C32 N31 C35 . . 109.4(4) ?
N33 C32 N31 . . 108.1(4) ?
C32 N33 C34 . . 108.3(4) ?
C32 N33 C33 . . 125.8(4) ?
C34 N33 C33 . . 125.9(4) ?
C35 C34 N33 . . 107.4(4) ?
C34 C35 N31 . . 106.8(4) ?
Cl22 Ti2 Cl22 . 2_676 180.0 ?
Cl22 Ti2 Cl23 . . 89.82(5) ?
Cl22 Ti2 Cl23 2_676 . 90.18(5) ?
Cl22 Ti2 Cl23 . 2_676 90.18(5) ?
Cl22 Ti2 Cl23 2_676 2_676 89.82(5) ?
Cl23 Ti2 Cl23 . 2_676 180.0 ?
Cl22 Ti2 Cl21 . 2_676 88.63(4) ?
Cl22 Ti2 Cl21 2_676 2_676 91.37(4) ?
Cl23 Ti2 Cl21 . 2_676 89.37(4) ?
Cl23 Ti2 Cl21 2_676 2_676 90.64(4) ?
Cl22 Ti2 Cl21 . . 91.37(4) ?
Cl22 Ti2 Cl21 2_676 . 88.63(4) ?
Cl23 Ti2 Cl21 . . 90.63(4) ?
Cl23 Ti2 Cl21 2_676 . 89.36(4) ?
Cl21 Ti2 Cl21 2_676 . 180.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 N11 . 2.167(3) y
Ti1 Cl1 . 2.3043(13) y
Ti1 Cl5 . 2.3055(12) y
Ti1 Cl4 . 2.3164(12) y
Ti1 Cl2 . 2.3164(12) y
Ti1 Cl3 . 2.3767(12) y
N11 C12 . 1.327(5) ?
N11 C15 . 1.386(5) ?
C12 N13 . 1.347(5) ?
N13 C14 . 1.371(5) ?
N13 C13 . 1.465(5) ?
C14 C15 . 1.350(6) ?
N21 C22 . 1.325(5) ?
N21 C25 . 1.368(5) ?
C22 N23 . 1.322(5) ?
N23 C24 . 1.372(5) ?
N23 C23 . 1.453(5) ?
C24 C25 . 1.346(6) ?
N31 C32 . 1.327(6) ?
N31 C35 . 1.357(6) ?
C32 N33 . 1.322(5) ?
N33 C34 . 1.372(5) ?
N33 C33 . 1.471(6) ?
C34 C35 . 1.341(6) ?
Ti2 Cl22 . 2.3297(11) y
Ti2 Cl22 2_676 2.3297(11) ?
Ti2 Cl23 . 2.3323(11) y
Ti2 Cl23 2_676 2.3323(11) ?
Ti2 Cl21 2_676 2.3523(10) ?
Ti2 Cl21 . 2.3523(10) y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
Cl1 Ti1 N11 C12 155.7(3) y
Cl5 Ti1 N11 C12 -20(2) ?
Cl4 Ti1 N11 C12 -26.7(3) y
Cl2 Ti1 N11 C12 65.1(3) y
Cl3 Ti1 N11 C12 -115.9(3) y
Cl1 Ti1 N11 C15 -23.2(3) ?
Cl5 Ti1 N11 C15 161(2) ?
Cl4 Ti1 N11 C15 154.3(3) ?
Cl2 Ti1 N11 C15 -113.9(3) ?
Cl3 Ti1 N11 C15 65.1(3) ?
C15 N11 C12 N13 0.1(4) ?
Ti1 N11 C12 N13 -179.0(2) ?
N11 C12 N13 C14 -0.2(4) ?
N11 C12 N13 C13 179.6(3) ?
C12 N13 C14 C15 0.1(4) ?
C13 N13 C14 C15 -179.6(4) ?
N13 C14 C15 N11 -0.1(5) ?
C12 N11 C15 C14 0.0(4) ?
Ti1 N11 C15 C14 179.1(3) ?
C25 N21 C22 N23 -1.3(5) ?
N21 C22 N23 C24 1.4(5) ?
N21 C22 N23 C23 -179.8(4) ?
C22 N23 C24 C25 -0.9(5) ?
C23 N23 C24 C25 -179.7(4) ?
N23 C24 C25 N21 0.1(5) ?
C22 N21 C25 C24 0.7(5) ?
C35 N31 C32 N33 0.1(5) ?
N31 C32 N33 C34 0.0(5) ?
N31 C32 N33 C33 -179.8(4) ?
C32 N33 C34 C35 -0.2(5) ?
C33 N33 C34 C35 179.7(4) ?
N33 C34 C35 N31 0.2(5) ?
C32 N31 C35 C34 -0.2(5) ?
