#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:26:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179328 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/25/4322535.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_4322535
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            'C29 H38 Cl4 N2 O2 Ti'
_chemical_formula_weight         636.31
_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                67.1821(7)
_cell_angle_beta                 83.7061(7)
_cell_angle_gamma                77.7641(7)
_cell_formula_units_Z            2
_cell_length_a                   8.16620(10)
_cell_length_b                   14.8386(2)
_cell_length_c                   14.9441(2)
_cell_measurement_temperature    132(2)
_cell_volume                     1630.46(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      132(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18904
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.617
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.89
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0030(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_obs          0.0308
_refine_ls_shift/esd_max         -0.046
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0479P)²+0.2110P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0891
_refine_ls_wR_factor_obs         0.0863
_reflns_number_observed          6293
_reflns_number_total             7554
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981364j_08.cif
_cod_data_source_block           (TMP)2TiCl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.2110P] 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^)+(0.0479P)^2^+0.2110P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322535
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 0.47519(3) 0.24944(2) 0.24323(2) 0.01841(8) Uani 1 d . .
Cl1 Cl 0.69360(5) 0.33262(3) 0.16191(3) 0.02619(9) Uani 1 d . .
Cl2 Cl 0.59951(5) 0.21203(3) 0.39303(2) 0.02339(9) Uani 1 d . .
O2 O 0.37386(14) 0.28877(8) 0.12278(7) 0.0261(2) Uani 1 d . .
C19 C 0.3502(3) 0.3747(2) -0.04902(12) 0.0489(5) Uani 1 d . .
H19A H 0.3274(20) 0.4428(2) -0.09731(15) 0.073 Uiso 1 calc R .
H19B H 0.2667(14) 0.3380(10) -0.0533(4) 0.073 Uiso 1 calc R .
H19C H 0.4624(7) 0.3416(11) -0.0616(5) 0.073 Uiso 1 calc R .
C18 C 0.3409(2) 0.37749(12) 0.05115(11) 0.0293(3) Uani 1 d . .
C17 C 0.2986(2) 0.46292(12) 0.06910(11) 0.0312(4) Uani 1 d . .
H18 H 0.2869(2) 0.52448(12) 0.01514(11) 0.037 Uiso 1 calc R .
C16 C 0.2704(2) 0.46551(11) 0.16464(11) 0.0273(3) Uani 1 d . .
C15 C 0.1745(3) 0.56342(13) 0.17025(13) 0.0399(4) Uani 1 d . .
H15A H 0.0584(5) 0.5570(4) 0.1920(10) 0.060 Uiso 1 calc R .
H15B H 0.1756(15) 0.6167(2) 0.1059(3) 0.060 Uiso 1 calc R .
H15C H 0.2280(11) 0.5795(5) 0.2164(8) 0.060 Uiso 1 calc R .
N2 N 0.31915(15) 0.38764(9) 0.24399(8) 0.0209(2) Uani 1 d . .
C20 C 0.2611(2) 0.39269(10) 0.33765(10) 0.0214(3) Uani 1 d . .
C25 C 0.3599(2) 0.42335(11) 0.38807(11) 0.0248(3) Uani 1 d . .
C28 C 0.5192(2) 0.46149(13) 0.34240(13) 0.0337(4) Uani 1 d . .
H28A H 0.5885(7) 0.4587(9) 0.3933(2) 0.051 Uiso 1 calc R .
H28B H 0.4906(2) 0.5304(3) 0.2965(7) 0.051 Uiso 1 calc R .
H28C H 0.5815(8) 0.4200(6) 0.3079(8) 0.051 Uiso 1 calc R .
C24 C 0.3059(2) 0.41894(12) 0.48178(12) 0.0318(4) Uani 1 d . .
H24 H 0.3712(2) 0.43995(12) 0.51628(12) 0.038 Uiso 1 calc R .
C23 C 0.1595(2) 0.38469(13) 0.52608(12) 0.0355(4) Uani 1 d . .
C27 C 0.1054(3) 0.3768(2) 0.62914(14) 0.0530(6) Uani 1 d . .
H27A H 0.1776(13) 0.4079(10) 0.6520(4) 0.080 Uiso 1 calc R .
H27B H 0.1149(19) 0.3065(2) 0.6718(3) 0.080 Uiso 1 calc R .
H27C H -0.0112(7) 0.4107(10) 0.6300(2) 0.080 Uiso 1 calc R .
C22 C 0.0626(2) 0.35773(13) 0.47252(12) 0.0344(4) Uani 1 d . .
H22 H -0.0384(2) 0.33551(13) 0.50138(12) 0.041 Uiso 1 calc R .
C21 C 0.1081(2) 0.36207(11) 0.37808(12) 0.0266(3) Uani 1 d . .
C26 C -0.0069(2) 0.33925(14) 0.32040(14) 0.0366(4) Uani 1 d . .
H26A H 0.0595(3) 0.3005(8) 0.2843(8) 0.055 Uiso 1 calc R .
H26B H -0.0681(12) 0.40162(14) 0.2748(7) 0.055 Uiso 1 calc R .
H26C H -0.0869(11) 0.3008(8) 0.3647(2) 0.055 Uiso 1 calc R .
O1 O 0.31469(12) 0.17219(7) 0.31536(7) 0.0218(2) Uani 1 d . .
C5 C 0.1921(2) 0.06511(13) 0.45976(11) 0.0296(3) Uani 1 d . .
H5A H 0.2143(8) -0.0038(3) 0.5065(5) 0.044 Uiso 1 calc R .
H5B H 0.0854(3) 0.0779(9) 0.42874(15) 0.044 Uiso 1 calc R .
H5C H 0.1859(10) 0.1106(6) 0.4937(6) 0.044 Uiso 1 calc R .
C4 C 0.3311(2) 0.08138(11) 0.38363(10) 0.0219(3) Uani 1 d . .
C3 C 0.4643(2) 0.00848(11) 0.38139(10) 0.0236(3) Uani 1 d . .
H3 H 0.4760(2) -0.05355(11) 0.43476(10) 0.028 Uiso 1 calc R .
C2 C 0.5875(2) 0.02010(11) 0.30321(10) 0.0220(3) Uani 1 d . .
C1 C 0.6955(2) -0.07499(12) 0.29847(12) 0.0311(3) Uani 1 d . .
H1A H 0.6552(10) -0.0907(5) 0.2478(6) 0.047 Uiso 1 calc R .
H1B H 0.6888(12) -0.1298(2) 0.3613(3) 0.047 Uiso 1 calc R .
H1C H 0.8121(3) -0.0659(3) 0.2833(9) 0.047 Uiso 1 calc R .
N1 N 0.60433(15) 0.10817(9) 0.23614(8) 0.0196(2) Uani 1 d . .
C6 C 0.7132(2) 0.11029(10) 0.15162(10) 0.0200(3) Uani 1 d . .
C11 C 0.6439(2) 0.10753(11) 0.07034(11) 0.0240(3) Uani 1 d . .
C14 C 0.4666(2) 0.08951(13) 0.07435(13) 0.0323(4) Uani 1 d . .
H14A H 0.3899(3) 0.1335(6) 0.1016(8) 0.048 Uiso 1 calc R .
H14B H 0.4624(4) 0.0200(3) 0.1154(7) 0.048 Uiso 1 calc R .
H14C H 0.4331(6) 0.1033(9) 0.0086(2) 0.048 Uiso 1 calc R .
C10 C 0.7447(2) 0.11889(12) -0.01393(11) 0.0289(3) Uani 1 d . .
H10 H 0.6990(2) 0.11786(12) -0.06923(11) 0.035 Uiso 1 calc R .
C9 C 0.9110(2) 0.13174(12) -0.01916(12) 0.0312(4) Uani 1 d . .
C13 C 1.0167(3) 0.1455(2) -0.11222(13) 0.0466(5) Uani 1 d . .
H13A H 1.0684(15) 0.0802(2) -0.1139(5) 0.070 Uiso 1 calc R .
H13B H 1.1045(12) 0.1823(10) -0.1144(5) 0.070 Uiso 1 calc R .
H13C H 0.9453(4) 0.1828(10) -0.16834(13) 0.070 Uiso 1 calc R .
C8 C 0.9770(2) 0.13001(12) 0.06356(12) 0.0296(3) Uani 1 d . .
H8 H 1.0907(2) 0.13676(12) 0.06137(12) 0.035 Uiso 1 calc R .
C7 C 0.8819(2) 0.11865(11) 0.15029(11) 0.0239(3) Uani 1 d . .
C12 C 0.9619(2) 0.11411(13) 0.23899(12) 0.0318(4) Uani 1 d . .
H12A H 1.0036(14) 0.04453(14) 0.2796(5) 0.048 Uiso 1 calc R .
H12B H 0.8785(5) 0.1445(8) 0.2763(5) 0.048 Uiso 1 calc R .
H12C H 1.0554(10) 0.1503(8) 0.21856(13) 0.048 Uiso 1 calc R .
C1S C 0.6487(3) 0.2460(2) 0.6172(2) 0.0626(6) Uani 1 d . .
H1S H 0.5529(34) 0.2353(19) 0.5868(19) 0.076(8) Uiso 1 d . .
H2S H 0.6844(41) 0.3106(25) 0.5859(24) 0.108(11) Uiso 1 d . .
Cl1A Cl 0.8286(3) 0.15078(15) 0.6294(3) 0.0572(9) Uani 0.68(2) d P .
Cl1B Cl 0.8113(16) 0.1491(6) 0.6580(17) 0.111(3) Uani 0.32(2) d P .
Cl2A Cl 0.5551(3) 0.2501(2) 0.72846(11) 0.0643(6) Uani 0.700(11) d P .
Cl2B Cl 0.5733(13) 0.2713(7) 0.7235(6) 0.160(4) Uani 0.300(11) d P .
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'
O O 0.0106 0.0060 '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
O1 Ti1 O2 94.51(5) . . ?
O1 Ti1 N1 82.40(4) . . ?
O2 Ti1 N1 92.32(4) . . ?
O1 Ti1 N2 93.18(4) . . ?
O2 Ti1 N2 82.52(5) . . ?
N1 Ti1 N2 172.95(5) . . ?
O1 Ti1 Cl1 174.59(3) . . ?
O2 Ti1 Cl1 89.25(4) . . ?
N1 Ti1 Cl1 93.59(3) . . ?
N2 Ti1 Cl1 91.15(3) . . ?
O1 Ti1 Cl2 87.48(3) . . ?
O2 Ti1 Cl2 175.96(4) . . ?
N1 Ti1 Cl2 91.42(3) . . ?
N2 Ti1 Cl2 93.87(3) . . ?
Cl1 Ti1 Cl2 89.008(15) . . ?
C18 O2 Ti1 130.77(10) . . ?
O2 C18 C17 121.56(14) . . ?
O2 C18 C19 114.76(14) . . ?
C17 C18 C19 123.65(15) . . ?
C18 C17 C16 123.94(14) . . ?
N2 C16 C17 122.79(14) . . ?
N2 C16 C15 121.20(14) . . ?
C17 C16 C15 115.98(14) . . ?
C16 N2 C20 118.42(12) . . ?
C16 N2 Ti1 123.94(10) . . ?
C20 N2 Ti1 117.60(9) . . ?
C25 C20 C21 121.33(13) . . ?
C25 C20 N2 120.17(13) . . ?
C21 C20 N2 118.44(13) . . ?
C24 C25 C20 118.19(14) . . ?
C24 C25 C28 120.54(14) . . ?
C20 C25 C28 121.27(13) . . ?
C23 C24 C25 122.2(2) . . ?
C24 C23 C22 117.79(15) . . ?
C24 C23 C27 121.8(2) . . ?
C22 C23 C27 120.4(2) . . ?
C23 C22 C21 122.7(2) . . ?
C22 C21 C20 117.64(15) . . ?
C22 C21 C26 120.75(15) . . ?
C20 C21 C26 121.55(14) . . ?
C4 O1 Ti1 131.58(9) . . ?
O1 C4 C3 121.10(13) . . ?
O1 C4 C5 115.22(13) . . ?
C3 C4 C5 123.65(13) . . ?
C4 C3 C2 123.99(13) . . ?
N1 C2 C3 122.72(13) . . ?
N1 C2 C1 120.82(13) . . ?
C3 C2 C1 116.42(13) . . ?
C2 N1 C6 118.01(12) . . ?
C2 N1 Ti1 123.99(9) . . ?
C6 N1 Ti1 117.99(9) . . ?
C7 C6 C11 121.15(13) . . ?
C7 C6 N1 120.26(12) . . ?
C11 C6 N1 118.55(12) . . ?
C10 C11 C6 118.31(14) . . ?
C10 C11 C14 120.29(14) . . ?
C6 C11 C14 121.37(13) . . ?
C11 C10 C9 121.98(14) . . ?
C8 C9 C10 118.06(14) . . ?
C8 C9 C13 121.2(2) . . ?
C10 C9 C13 120.8(2) . . ?
C9 C8 C7 122.49(14) . . ?
C8 C7 C6 117.89(13) . . ?
C8 C7 C12 120.18(14) . . ?
C6 C7 C12 121.93(13) . . ?
Cl1B C1S Cl2A 100.7(9) . . ?
Cl1B C1S Cl1A 13.9(8) . . ?
Cl2A C1S Cl1A 114.6(2) . . ?
Cl1B C1S Cl2B 103.4(9) . . ?
Cl2A C1S Cl2B 11.4(4) . . ?
Cl1A C1S Cl2B 117.0(3) . . ?
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 O1 1.8874(10) . ?
Ti1 O2 1.8902(10) . ?
Ti1 N1 2.1745(12) . ?
Ti1 N2 2.1764(12) . ?
Ti1 Cl1 2.3401(4) . ?
Ti1 Cl2 2.3760(4) . ?
O2 C18 1.331(2) . ?
C19 C18 1.506(2) . ?
C18 C17 1.363(2) . ?
C17 C16 1.435(2) . ?
C16 N2 1.321(2) . ?
C16 C15 1.526(2) . ?
N2 C20 1.453(2) . ?
C20 C25 1.407(2) . ?
C20 C21 1.412(2) . ?
C25 C24 1.402(2) . ?
C25 C28 1.516(2) . ?
C24 C23 1.396(3) . ?
C23 C22 1.396(3) . ?
C23 C27 1.521(2) . ?
C22 C21 1.400(2) . ?
C21 C26 1.510(2) . ?
O1 C4 1.327(2) . ?
C5 C4 1.504(2) . ?
C4 C3 1.369(2) . ?
C3 C2 1.437(2) . ?
C2 N1 1.327(2) . ?
C2 C1 1.520(2) . ?
N1 C6 1.456(2) . ?
C6 C7 1.407(2) . ?
C6 C11 1.413(2) . ?
C11 C10 1.400(2) . ?
C11 C14 1.518(2) . ?
C10 C9 1.400(2) . ?
C9 C8 1.391(2) . ?
C9 C13 1.520(2) . ?
C8 C7 1.406(2) . ?
C7 C12 1.513(2) . ?
C1S Cl1B 1.701(8) . ?
C1S Cl2A 1.769(3) . ?
C1S Cl1A 1.780(4) . ?
C1S Cl2B 1.786(8) . ?
