#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:26:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179328 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/25/4322536.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4322536
loop_
_publ_author_name
'Lena Kakaliou'
Scanlon
'Baixin Qian'
'Sung W. Baek'
'Milton R. Smith'
'Douglas H. Motry'
_publ_section_title
;
 Five- and Six-Coordinate Group 4 Compounds Stabilized by β-Ketiminate
 and Diketiminate Ligands: Syntheses and Comparisons between Solid-State
 and Solution Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5964
_journal_page_last               5977
_journal_paper_doi               10.1021/ic981364j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C26 H29 Cl3 N2 Ti'
_chemical_formula_weight         523.76
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                103.25(3)
_cell_angle_beta                 99.96(3)
_cell_angle_gamma                94.58(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2859(15)
_cell_length_b                   13.154(3)
_cell_length_c                   15.253(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1390.5(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0903
_diffrn_reflns_av_sigmaI/netI    0.1912
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8178
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.611
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.556
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.849
_refine_ls_goodness_of_fit_obs   1.153
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5865
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.848
_refine_ls_restrained_S_obs      1.148
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_obs          0.0804
_refine_ls_shift/esd_max         -0.488
_refine_ls_shift/esd_mean        0.046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0773P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2045
_refine_ls_wR_factor_obs         0.1898
_reflns_number_observed          2816
_reflns_number_total             5865
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981364j_09.cif
_cod_data_source_block           (TTP)TiCl3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0773P)^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^)+(0.0773P)^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_original_cell_volume        1390.6(5)
_cod_database_code               4322536
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ti1 Ti 0.95764(12) 0.60808(7) 0.32920(6) 0.0353(3) Uani 1 d . .
Cl1 Cl 0.9974(2) 0.70323(11) 0.22970(9) 0.0465(4) Uani 1 d . .
Cl2 Cl 1.1410(2) 0.69692(12) 0.47191(9) 0.0482(4) Uani 1 d . .
Cl3 Cl 1.1884(2) 0.49585(12) 0.31115(10) 0.0570(4) Uani 1 d . .
N1 N 0.7597(6) 0.4960(3) 0.2491(3) 0.0357(10) Uani 1 d . .
N2 N 0.7436(5) 0.6784(3) 0.3704(2) 0.0315(9) Uani 1 d . .
C1 C 0.6572(10) 0.3336(4) 0.2943(4) 0.060(2) Uani 1 d . .
H1A H 0.6500(10) 0.3008(4) 0.2305(4) 0.090 Uiso 1 calc R .
H1B H 0.5361(10) 0.3227(4) 0.3098(4) 0.090 Uiso 1 calc R .
H1C H 0.7467(10) 0.3030(4) 0.3312(4) 0.090 Uiso 1 calc R .
C2 C 0.7172(7) 0.4480(4) 0.3120(3) 0.0362(11) Uani 1 d . .
C3 C 0.7369(6) 0.5112(4) 0.4021(3) 0.0338(11) Uani 1 d . .
H3A H 0.7940(6) 0.4818(4) 0.4523(3) 0.041 Uiso 1 calc R .
C4 C 0.7052(7) 0.6173(4) 0.4254(3) 0.0337(11) Uani 1 d . .
C5 C 0.6483(8) 0.6604(4) 0.5152(3) 0.0447(13) Uani 1 d . .
H5A H 0.6318(8) 0.7332(4) 0.5213(3) 0.067 Uiso 1 calc R .
H5B H 0.7443(8) 0.6541(4) 0.5647(3) 0.067 Uiso 1 calc R .
H5C H 0.5325(8) 0.6215(4) 0.5171(3) 0.067 Uiso 1 calc R .
C6 C 0.7043(7) 0.4465(4) 0.1520(3) 0.0381(12) Uani 1 d . .
C7 C 0.8381(8) 0.4354(5) 0.0973(3) 0.0485(14) Uani 1 d . .
H7A H 0.9643(8) 0.4582(5) 0.1227(3) 0.058 Uiso 1 calc R .
C8 C 0.7820(9) 0.3905(5) 0.0055(4) 0.058(2) Uani 1 d . .
H8A H 0.8722(9) 0.3841(5) -0.0311(4) 0.069 Uiso 1 calc R .
C9 C 0.5947(9) 0.3539(5) -0.0359(4) 0.057(2) Uani 1 d . .
C10 C 0.4632(9) 0.3663(5) 0.0203(4) 0.061(2) Uani 1 d . .
H10A H 0.3372(9) 0.3429(5) -0.0051(4) 0.073 Uiso 1 calc R .
C11 C 0.5158(8) 0.4128(5) 0.1134(3) 0.0493(14) Uani 1 d . .
H11A H 0.4256(8) 0.4215(5) 0.1499(3) 0.059 Uiso 1 calc R .
C12 C 0.5396(10) 0.3027(6) -0.1362(4) 0.079(2) Uani 1 d . .
H12A H 0.6494(10) 0.3007(6) -0.1632(4) 0.119 Uiso 1 calc R .
H12B H 0.4533(10) 0.3423(6) -0.1652(4) 0.119 Uiso 1 calc R .
H12C H 0.4806(10) 0.2323(6) -0.1449(4) 0.119 Uiso 1 calc R .
C13 C 0.6822(7) 0.7807(4) 0.3778(3) 0.0315(11) Uani 1 d . .
C14 C 0.4919(7) 0.7882(4) 0.3608(3) 0.0336(11) Uani 1 d . .
H14A H 0.4053(7) 0.7283(4) 0.3483(3) 0.040 Uiso 1 calc R .
C15 C 0.4312(7) 0.8855(4) 0.3626(3) 0.0406(12) Uani 1 d . .
H15A H 0.3031(7) 0.8905(4) 0.3505(3) 0.049 Uiso 1 calc R .
C16 C 0.5577(9) 0.9751(4) 0.3821(3) 0.0445(13) Uani 1 d . .
C17 C 0.7471(9) 0.9679(4) 0.4001(4) 0.0506(14) Uani 1 d . .
H17A H 0.8328(9) 1.0284(4) 0.4143(4) 0.061 Uiso 1 calc R .
C18 C 0.8123(8) 0.8690(4) 0.3972(4) 0.0470(14) Uani 1 d . .
H18A H 0.9403(8) 0.8636(4) 0.4082(4) 0.056 Uiso 1 calc R .
C19 C 0.4886(10) 1.0807(5) 0.3823(4) 0.066(2) Uani 1 d . .
H19A H 0.3538(10) 1.0719(5) 0.3689(4) 0.099 Uiso 1 calc R .
H19B H 0.5349(10) 1.1090(5) 0.3364(4) 0.099 Uiso 1 calc R .
H19C H 0.5334(10) 1.1282(5) 0.4416(4) 0.099 Uiso 1 calc R .
C20 C 1.0602(22) 1.1772(10) 0.2032(10) 0.215(9) Uani 1 d D .
H20A H 1.0494(22) 1.2482(10) 0.2246(10) 0.259 Uiso 1 calc R .
C21 C 0.9547(19) 1.1023(15) 0.2294(9) 0.202(7) Uani 1 d D .
H21A H 0.8724(19) 1.1227(15) 0.2686(9) 0.243 Uiso 1 calc R .
C22 C 0.9699(18) 0.9982(13) 0.1984(10) 0.220(8) Uani 1 d D .
H22A H 0.8981(18) 0.9479(13) 0.2164(10) 0.263 Uiso 1 calc R .
C23 C 1.0906(20) 0.9675(10) 0.1407(9) 0.206(7) Uani 1 d D .
H23A H 1.1008(20) 0.8964(10) 0.1194(9) 0.247 Uiso 1 calc R .
C24 C 1.1963(19) 1.0418(15) 0.1146(9) 0.224(9) Uiso 1 d D .
C25 C 1.1816(19) 1.1467(12) 0.1454(10) 0.214(8) Uani 1 d D .
H25A H 1.2534(19) 1.1969(12) 0.1272(10) 0.256 Uiso 1 calc R .
C26 C 1.3287(55) 0.9970(31) 0.0547(29) 0.574(28) Uiso 1 d . .
H26A H 1.3976(55) 1.0531(31) 0.0386(29) 0.861 Uiso 1 calc R .
H26B H 1.2584(55) 0.9488(31) -0.0002(29) 0.861 Uiso 1 calc R .
H26C H 1.4148(55) 0.9605(31) 0.0874(29) 0.861 Uiso 1 calc R .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ti1 N2 85.1(2) . . ?
N1 Ti1 Cl1 99.27(12) . . ?
N2 Ti1 Cl1 95.34(12) . . ?
N1 Ti1 Cl3 91.29(13) . . ?
N2 Ti1 Cl3 162.88(12) . . ?
Cl1 Ti1 Cl3 101.76(6) . . ?
N1 Ti1 Cl2 152.37(12) . . ?
N2 Ti1 Cl2 87.25(12) . . ?
Cl1 Ti1 Cl2 107.86(6) . . ?
Cl3 Ti1 Cl2 88.29(6) . . ?
N1 Ti1 C3 60.7(2) . . ?
N2 Ti1 C3 61.5(2) . . ?
Cl1 Ti1 C3 148.88(12) . . ?
Cl3 Ti1 C3 102.24(13) . . ?
Cl2 Ti1 C3 92.38(12) . . ?
N1 Ti1 C4 78.7(2) . . ?
N2 Ti1 C4 31.47(15) . . ?
Cl1 Ti1 C4 126.68(12) . . ?
Cl3 Ti1 C4 131.42(12) . . ?
Cl2 Ti1 C4 80.90(11) . . ?
C3 Ti1 C4 32.3(2) . . ?
N1 Ti1 C2 30.75(14) . . ?
N2 Ti1 C2 79.1(2) . . ?
Cl1 Ti1 C2 129.61(12) . . ?
Cl3 Ti1 C2 89.21(13) . . ?
Cl2 Ti1 C2 121.63(11) . . ?
C3 Ti1 C2 32.2(2) . . ?
C4 Ti1 C2 58.8(2) . . ?
C2 N1 C6 121.6(4) . . ?
C2 N1 Ti1 99.1(3) . . ?
C6 N1 Ti1 136.5(3) . . ?
C4 N2 C13 122.3(4) . . ?
C4 N2 Ti1 97.2(3) . . ?
C13 N2 Ti1 136.3(3) . . ?
N1 C2 C3 116.8(4) . . ?
N1 C2 C1 124.6(4) . . ?
C3 C2 C1 118.6(4) . . ?
N1 C2 Ti1 50.2(2) . . ?
C3 C2 Ti1 72.5(3) . . ?
C1 C2 Ti1 153.5(4) . . ?
C4 C3 C2 125.5(4) . . ?
C4 C3 Ti1 74.3(3) . . ?
C2 C3 Ti1 75.3(3) . . ?
N2 C4 C3 118.4(4) . . ?
N2 C4 C5 122.2(4) . . ?
C3 C4 C5 119.1(4) . . ?
N2 C4 Ti1 51.3(2) . . ?
C3 C4 Ti1 73.5(3) . . ?
C5 C4 Ti1 148.4(4) . . ?
C7 C6 C11 120.1(5) . . ?
C7 C6 N1 120.1(5) . . ?
C11 C6 N1 119.8(5) . . ?
C8 C7 C6 119.0(5) . . ?
C7 C8 C9 122.8(5) . . ?
C10 C9 C8 117.2(5) . . ?
C10 C9 C12 121.7(6) . . ?
C8 C9 C12 121.1(6) . . ?
C9 C10 C11 121.3(6) . . ?
C10 C11 C6 119.6(5) . . ?
C14 C13 C18 120.9(5) . . ?
C14 C13 N2 118.9(4) . . ?
C18 C13 N2 120.1(5) . . ?
C13 C14 C15 119.4(5) . . ?
C14 C15 C16 121.0(5) . . ?
C17 C16 C15 119.6(5) . . ?
C17 C16 C19 120.2(5) . . ?
C15 C16 C19 120.2(5) . . ?
C16 C17 C18 120.3(5) . . ?
C13 C18 C17 118.7(5) . . ?
C25 C20 C21 119.6(5) . . ?
C22 C21 C20 120.4(5) . . ?
C21 C22 C23 120.1(5) . . ?
C22 C23 C24 119.7(5) . . ?
C23 C24 C25 120.5(5) . . ?
C23 C24 C26 113.8(21) . . ?
C25 C24 C26 125.6(21) . . ?
C24 C25 C20 119.6(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N1 1.993(4) . ?
Ti1 N2 1.996(4) . ?
Ti1 Cl1 2.2180(15) . ?
Ti1 Cl3 2.335(2) . ?
Ti1 Cl2 2.338(2) . ?
Ti1 C3 2.527(4) . ?
Ti1 C4 2.537(5) . ?
Ti1 C2 2.563(5) . ?
N1 C2 1.327(6) . ?
N1 C6 1.446(6) . ?
N2 C4 1.335(5) . ?
N2 C13 1.438(6) . ?
C1 C2 1.483(7) . ?
C2 C3 1.410(7) . ?
C3 C4 1.408(7) . ?
C4 C5 1.499(7) . ?
C6 C7 1.384(7) . ?
C6 C11 1.391(7) . ?
C7 C8 1.364(7) . ?
C8 C9 1.396(8) . ?
C9 C10 1.387(8) . ?
C9 C12 1.493(8) . ?
C10 C11 1.383(8) . ?
C13 C14 1.381(7) . ?
C13 C18 1.380(7) . ?
C14 C15 1.384(7) . ?
C15 C16 1.377(7) . ?
C16 C17 1.375(8) . ?
C16 C19 1.514(8) . ?
C17 C18 1.414(8) . ?
C20 C25 1.374(8) . ?
C20 C21 1.373(8) . ?
C21 C22 1.363(8) . ?
C22 C23 1.368(8) . ?
C23 C24 1.369(8) . ?
C24 C25 1.371(8) . ?
C24 C26 1.50(4) . ?
