Supplementary Material for Dalton Transactions
This journal is © The Royal Society of Chemistry 2003

Supplementary data


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_year                    ?
_journal_page_first              ?

loop_
_publ_author_name
'Simon J. Lancaster'
'Manfred Bochmann'
'David L. Hughes'
'Dale A. Pennington'

_publ_contact_author_name        'Simon J Lancaster'
_publ_contact_author_address     
;
Dr Simon J Lancaster
Wolfson Materials and Catalysis Centre, School of Chemical Sciences &
Pharmacy
University of East Anglia
Norfolk
NR4 7TJ
UNITED KINGDOM
;

_publ_contact_author_email       S.LANCASTER@UEA.AC.UK

_publ_section_title              
;
The synthesis, structure and catalytic activity of
mono(salicylaldiminato) titanium complexes
;

data_dalep3
_database_code_CSD               214921

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'Compound 2a'
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H26 Cl3 N O2 Ti'
_chemical_formula_structural     [TiCl3(thf)(OC6H3tBu-6,-CHNPh-2)]
_chemical_formula_sum            'C21 H26 Cl3 N O2 Ti'
_chemical_formula_weight         478.68

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c' #(no. 14)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.3850(15)
_cell_length_b                   31.797(6)
_cell_length_c                   9.815(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.50(3)
_cell_angle_gamma                90.00
_cell_volume                     2250.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plates
_exptl_crystal_colour            deep-red
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_type   'not applied'
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Rigaku R-Axis-IIc'
_diffrn_measurement_method       'image-plate oscillation photos'

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7928
_diffrn_reflns_av_R_equivalents  0.2680
_diffrn_reflns_av_sigmaI/netI    0.2324
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         25.36
_reflns_number_total             3383
_reflns_number_gt                1907
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'MSC R-Axis-II control software'
_computing_cell_refinement       'DENZO/CELL (Otwinowski and Minor, 1985)'
_computing_data_reduction        'DENZO, SCALEPACK (Otwinowski and Minor, 1985)'
_computing_structure_solution    'SHELXS (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3383
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.0882
_refine_ls_wR_factor_ref         0.2371
_refine_ls_wR_factor_gt          0.2088
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_restrained_S_all      0.931
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti 0.19168(15) 0.61446(3) 0.03125(14) 0.0256(4) Uani 1 1 d . . .
O1 O 0.1375(6) 0.65290(12) 0.1497(5) 0.0286(11) Uani 1 1 d . . .
C11 C 0.0071(8) 0.68036(17) 0.1776(8) 0.0241(15) Uani 1 1 d . . .
C12 C -0.1606(8) 0.68258(18) 0.0780(8) 0.0254(16) Uani 1 1 d . . .
C13 C -0.2922(9) 0.71241(18) 0.0938(9) 0.0290(17) Uani 1 1 d . . .
H13 H -0.4032 0.7150 0.0281 0.035 Uiso 1 1 calc R . .
C14 C -0.2521(9) 0.73851(18) 0.2121(9) 0.0333(19) Uani 1 1 d . . .
H14 H -0.3362 0.7593 0.2230 0.040 Uiso 1 1 calc R . .
C15 C -0.0888(9) 0.73384(18) 0.3135(9) 0.0315(18) Uani 1 1 d . . .
H15 H -0.0685 0.7510 0.3920 0.038 Uiso 1 1 calc R . .
C16 C 0.0447(9) 0.70401(17) 0.2998(8) 0.0275(16) Uani 1 1 d . . .
C161 C 0.2189(9) 0.69686(18) 0.4155(8) 0.0278(17) Uani 1 1 d . . .
C162 C 0.2167(10) 0.7250(2) 0.5427(10) 0.040(2) Uani 1 1 d . . .
H16A H 0.3266 0.7200 0.6134 0.060 Uiso 1 1 calc R . .
H16B H 0.1092 0.7186 0.5791 0.060 Uiso 1 1 calc R . .
H16C H 0.2130 0.7540 0.5150 0.060 Uiso 1 1 calc R . .
C163 C 0.2240(10) 0.65104(19) 0.4654(9) 0.0345(17) Uani 1 1 d . . .
H16D H 0.3333 0.6466 0.5372 0.052 Uiso 1 1 calc R . .
H16E H 0.2259 0.6326 0.3884 0.052 Uiso 1 1 calc R . .
H16F H 0.1159 0.6453 0.5018 0.052 Uiso 1 1 calc R . .
C164 C 0.3949(9) 0.70738(19) 0.3619(9) 0.0358(19) Uani 1 1 d . . .
H16G H 0.5025 0.7026 0.4349 0.054 Uiso 1 1 calc R . .
H16H H 0.3914 0.7364 0.3340 0.054 Uiso 1 1 calc R . .
H16I H 0.4006 0.6898 0.2835 0.054 Uiso 1 1 calc R . .
N2 N -0.1008(7) 0.62661(15) -0.0827(7) 0.0323(16) Uani 1 1 d . . .
C20 C -0.2041(9) 0.65554(18) -0.0457(8) 0.0290(17) Uani 1 1 d . . .
H20 H -0.3196 0.6596 -0.1046 0.035 Uiso 1 1 calc R . .
C21 C -0.1778(9) 0.60627(19) -0.2145(9) 0.0283(18) Uani 1 1 d . . .
C22 C -0.2066(9) 0.5629(2) -0.2187(10) 0.039(2) Uani 1 1 d . . .
H22 H -0.1765 0.5472 -0.1371 0.046 Uiso 1 1 calc R . .
C23 C -0.2800(9) 0.5435(2) -0.3445(10) 0.043(2) Uani 1 1 d . . .
H23 H -0.3010 0.5146 -0.3468 0.051 Uiso 1 1 calc R . .
C24 C -0.3234(10) 0.5669(2) -0.4694(11) 0.047(2) Uani 1 1 d . . .
H24 H -0.3728 0.5538 -0.5540 0.057 Uiso 1 1 calc R . .
C25 C -0.2907(11) 0.6100(2) -0.4634(10) 0.048(2) Uani 1 1 d . . .
H25 H -0.3165 0.6259 -0.5447 0.058 Uiso 1 1 calc R . .
C26 C -0.2199(10) 0.6290(2) -0.3371(10) 0.038(2) Uani 1 1 d . . .
H26 H -0.2000 0.6579 -0.3344 0.046 Uiso 1 1 calc R . .
O3 O 0.2153(6) 0.56887(12) -0.1252(6) 0.0291(12) Uani 1 1 d . . .
C31 C 0.2366(10) 0.5760(2) -0.2690(8) 0.0335(17) Uani 1 1 d . . .
H31A H 0.3554 0.5890 -0.2687 0.040 Uiso 1 1 calc R . .
H31B H 0.1391 0.5943 -0.3182 0.040 Uiso 1 1 calc R . .
C32 C 0.2246(10) 0.5331(2) -0.3396(10) 0.044(2) Uani 1 1 d . . .
H32A H 0.2931 0.5323 -0.4135 0.052 Uiso 1 1 calc R . .
H32B H 0.0973 0.5246 -0.3763 0.052 Uiso 1 1 calc R . .
C33 C 0.3193(11) 0.5060(2) -0.2112(9) 0.042(2) Uani 1 1 d . . .
H33A H 0.2798 0.4769 -0.2241 0.051 Uiso 1 1 calc R . .
H33B H 0.4532 0.5071 -0.1981 0.051 Uiso 1 1 calc R . .
C34 C 0.2599(10) 0.52441(19) -0.0910(10) 0.047(2) Uani 1 1 d . . .
H34A H 0.3585 0.5223 -0.0080 0.056 Uiso 1 1 calc R . .
H34B H 0.1517 0.5098 -0.0740 0.056 Uiso 1 1 calc R . .
Cl4 Cl 0.4950(2) 0.60402(5) 0.1371(2) 0.0345(5) Uani 1 1 d . . .
Cl5 Cl 0.2576(2) 0.66431(4) -0.1268(2) 0.0316(5) Uani 1 1 d . . .
Cl6 Cl 0.0745(3) 0.56024(5) 0.1461(2) 0.0385(5) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti 0.0263(7) 0.0229(6) 0.0257(9) -0.0012(5) 0.0017(6) 0.0000(4)
O1 0.030(2) 0.028(2) 0.027(4) -0.0003(18) 0.004(2) 0.0025(17)
C11 0.026(3) 0.022(3) 0.025(5) 0.003(3) 0.007(3) 0.005(2)
C12 0.027(3) 0.026(3) 0.021(5) 0.003(2) 0.001(3) -0.001(2)
C13 0.020(3) 0.032(3) 0.036(6) 0.002(3) 0.008(3) -0.003(2)
C14 0.027(4) 0.023(3) 0.049(6) 0.000(3) 0.006(4) 0.001(2)
C15 0.033(4) 0.026(3) 0.035(6) -0.010(3) 0.007(4) -0.004(3)
C16 0.033(4) 0.025(3) 0.023(5) -0.001(3) 0.002(3) -0.002(2)
C161 0.024(3) 0.031(3) 0.027(5) 0.001(3) 0.002(3) -0.003(3)
C162 0.036(4) 0.036(4) 0.047(7) -0.006(3) 0.006(4) -0.001(3)
C163 0.040(4) 0.034(4) 0.025(5) 0.005(3) -0.001(4) 0.001(3)
C164 0.031(4) 0.031(3) 0.042(6) -0.005(3) 0.003(4) -0.005(3)
N2 0.024(3) 0.026(3) 0.043(5) -0.002(2) -0.002(3) 0.000(2)
C20 0.028(3) 0.028(3) 0.032(6) -0.002(3) 0.008(3) 0.000(3)
C21 0.022(3) 0.032(3) 0.032(6) -0.005(3) 0.007(3) 0.003(2)
C22 0.028(4) 0.035(4) 0.051(7) -0.014(3) 0.007(4) -0.005(3)
C23 0.027(4) 0.049(4) 0.053(8) -0.022(4) 0.013(4) -0.007(3)
C24 0.033(4) 0.060(5) 0.045(8) -0.021(4) 0.000(4) 0.004(3)
C25 0.045(5) 0.057(5) 0.037(7) -0.001(4) -0.002(5) 0.014(4)
C26 0.037(4) 0.035(4) 0.041(7) -0.007(3) 0.004(4) 0.004(3)
O3 0.034(2) 0.019(2) 0.034(4) 0.0040(18) 0.008(2) 0.0026(17)
C31 0.039(4) 0.036(4) 0.020(5) 0.000(3) -0.006(3) 0.005(3)
C32 0.034(4) 0.035(4) 0.059(8) -0.009(3) 0.005(4) 0.002(3)
C33 0.050(5) 0.028(4) 0.050(7) -0.005(3) 0.014(5) 0.002(3)
C34 0.043(4) 0.021(3) 0.076(8) -0.003(3) 0.012(5) 0.006(3)
Cl4 0.0298(9) 0.0338(9) 0.0358(13) -0.0019(7) -0.0017(8) 0.0039(6)
Cl5 0.0364(9) 0.0261(8) 0.0312(12) 0.0027(6) 0.0047(8) -0.0030(6)
Cl6 0.0484(11) 0.0320(9) 0.0364(13) 0.0016(7) 0.0121(10) -0.0067(7)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Ti O1 1.791(5) . ?
Ti O3 2.146(5) . ?
Ti N2 2.240(6) . ?
Ti Cl4 2.281(2) . ?
Ti Cl6 2.327(2) . ?
Ti Cl5 2.342(2) . ?
O1 C11 1.371(7) . ?
C11 C16 1.392(10) . ?
C11 C12 1.403(9) . ?
C12 C13 1.391(8) . ?
C12 C20 1.465(9) . ?
C13 C14 1.406(11) . ?
C13 H13 0.9300 . ?
C14 C15 1.395(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.396(8) . ?
C15 H15 0.9300 . ?
C16 C161 1.537(9) . ?
C161 C163 1.535(9) . ?
C161 C162 1.540(10) . ?
C161 C164 1.541(9) . ?
C162 H16A 0.9600 . ?
C162 H16B 0.9600 . ?
C162 H16C 0.9600 . ?
C163 H16D 0.9600 . ?
C163 H16E 0.9600 . ?
C163 H16F 0.9600 . ?
C164 H16G 0.9600 . ?
C164 H16H 0.9600 . ?
C164 H16I 0.9600 . ?
N2 C20 1.296(8) . ?
N2 C21 1.448(10) . ?
C20 H20 0.9300 . ?
C21 C26 1.381(11) . ?
C21 C22 1.393(9) . ?
C22 C23 1.383(11) . ?
C22 H22 0.9300 . ?
C23 C24 1.411(12) . ?
C23 H23 0.9300 . ?
C24 C25 1.389(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.377(12) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
O3 C31 1.472(9) . ?
O3 C34 1.474(7) . ?
C31 C32 1.523(10) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.562(11) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.468(11) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?

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 Ti O3 171.76(19) . . ?
O1 Ti N2 83.1(2) . . ?
O3 Ti N2 88.8(2) . . ?
O1 Ti Cl4 98.00(16) . . ?
O3 Ti Cl4 90.21(14) . . ?
N2 Ti Cl4 176.72(18) . . ?
O1 Ti Cl6 91.85(15) . . ?
O3 Ti Cl6 86.70(13) . . ?
N2 Ti Cl6 87.14(16) . . ?
Cl4 Ti Cl6 95.91(8) . . ?
O1 Ti Cl5 94.36(15) . . ?
O3 Ti Cl5 85.55(13) . . ?
N2 Ti Cl5 82.48(16) . . ?
Cl4 Ti Cl5 94.34(8) . . ?
Cl6 Ti Cl5 167.17(9) . . ?
C11 O1 Ti 146.1(5) . . ?
O1 C11 C16 119.9(6) . . ?
O1 C11 C12 116.4(6) . . ?
C16 C11 C12 123.7(6) . . ?
C13 C12 C11 119.3(6) . . ?
C13 C12 C20 117.3(6) . . ?
C11 C12 C20 123.4(6) . . ?
C12 C13 C14 117.9(7) . . ?
C12 C13 H13 121.1 . . ?
C14 C13 H13 121.1 . . ?
C15 C14 C13 121.4(6) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C15 C16 121.5(7) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C11 C16 C15 115.9(7) . . ?
C11 C16 C161 122.4(6) . . ?
C15 C16 C161 121.7(6) . . ?
C163 C161 C16 109.6(5) . . ?
C163 C161 C162 107.3(6) . . ?
C16 C161 C162 111.0(5) . . ?
C163 C161 C164 110.5(5) . . ?
C16 C161 C164 110.4(6) . . ?
C162 C161 C164 107.9(5) . . ?
C161 C162 H16A 109.5 . . ?
C161 C162 H16B 109.5 . . ?
H16A C162 H16B 109.5 . . ?
C161 C162 H16C 109.5 . . ?
H16A C162 H16C 109.5 . . ?
H16B C162 H16C 109.5 . . ?
C161 C163 H16D 109.5 . . ?
C161 C163 H16E 109.5 . . ?
H16D C163 H16E 109.5 . . ?
C161 C163 H16F 109.5 . . ?
H16D C163 H16F 109.5 . . ?
H16E C163 H16F 109.5 . . ?
C161 C164 H16G 109.5 . . ?
C161 C164 H16H 109.5 . . ?
H16G C164 H16H 109.5 . . ?
C161 C164 H16I 109.5 . . ?
H16G C164 H16I 109.5 . . ?
H16H C164 H16I 109.5 . . ?
C20 N2 C21 115.2(6) . . ?
C20 N2 Ti 123.0(5) . . ?
C21 N2 Ti 121.2(4) . . ?
N2 C20 C12 127.7(7) . . ?
N2 C20 H20 116.2 . . ?
C12 C20 H20 116.2 . . ?
C26 C21 C22 119.2(8) . . ?
C26 C21 N2 121.1(6) . . ?
C22 C21 N2 119.7(7) . . ?
C23 C22 C21 119.8(9) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 120.8(8) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C25 C24 C23 118.6(8) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
C26 C25 C24 120.1(9) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C21 121.6(7) . . ?
C25 C26 H26 119.2 . . ?
C21 C26 H26 119.2 . . ?
C31 O3 C34 107.5(5) . . ?
C31 O3 Ti 128.7(3) . . ?
C34 O3 Ti 122.3(5) . . ?
O3 C31 C32 106.9(6) . . ?
O3 C31 H31A 110.3 . . ?
C32 C31 H31A 110.3 . . ?
O3 C31 H31B 110.3 . . ?
C32 C31 H31B 110.3 . . ?
H31A C31 H31B 108.6 . . ?
C31 C32 C33 99.0(6) . . ?
C31 C32 H32A 112.0 . . ?
C33 C32 H32A 112.0 . . ?
C31 C32 H32B 112.0 . . ?
C33 C32 H32B 112.0 . . ?
H32A C32 H32B 109.7 . . ?
C34 C33 C32 105.6(6) . . ?
C34 C33 H33A 110.6 . . ?
C32 C33 H33A 110.6 . . ?
C34 C33 H33B 110.6 . . ?
C32 C33 H33B 110.6 . . ?
H33A C33 H33B 108.8 . . ?
C33 C34 O3 106.9(7) . . ?
C33 C34 H34A 110.3 . . ?
O3 C34 H34A 110.3 . . ?
C33 C34 H34B 110.3 . . ?
O3 C34 H34B 110.3 . . ?
H34A C34 H34B 108.6 . . ?

_diffrn_measured_fraction_theta_max 0.822
_diffrn_reflns_theta_full        25.36
_diffrn_measured_fraction_theta_full 0.822
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.165

#===END

data_dale1
_database_code_CSD               214922

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'Compound 3b'
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H30 Cl7 N O Ti2'
_chemical_formula_structural     
[TiCl3(mu-Cl)3TiCl{O-C6H3(tBu-6)-2-CHN-C6H3(iPr2-2,6)}]
_chemical_formula_sum            'C23 H30 Cl7 N O Ti2'
_chemical_formula_weight         680.43

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n' #(equiv. to no. 14)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.880(1)
_cell_length_b                   19.315(1)
_cell_length_c                   15.511(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.80(1)
_cell_angle_gamma                90.00
_cell_volume                     2886.4(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       'thick plate'
_exptl_crystal_colour            'deep red,'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_absorpt_coefficient_mu    1.220
_exptl_absorpt_correction_type   'not applied'
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      140(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Rigaku R-Axis-IIc'
_diffrn_measurement_method       'image-plate oscillation photos'

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15791
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         25.56
_reflns_number_total             5091
_reflns_number_gt                4308
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'MSC R-Axis-II control software'
_computing_cell_refinement       'DENZO/CELL (Otwinowski and Minor, 1985)'
_computing_data_reduction        'DENZO, SCALEPACK (Otwinowski and Minor, 1985)'
_computing_structure_solution    'SHELXS (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.7236P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5091
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0941
_refine_ls_wR_factor_gt          0.0912
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.48748(4) 0.23512(2) 0.05157(3) 0.02925(12) Uani 1 1 d . . .
Ti2 Ti 0.83005(5) 0.20370(2) 0.10730(3) 0.03549(13) Uani 1 1 d . . .
Cl3 Cl 0.37410(7) 0.26493(3) -0.08172(4) 0.04049(16) Uani 1 1 d . . .
Cl4 Cl 0.64779(6) 0.20096(3) 0.19276(4) 0.03375(15) Uani 1 1 d . . .
Cl5 Cl 0.68539(6) 0.30923(3) 0.04806(4) 0.03352(14) Uani 1 1 d . . .
Cl6 Cl 0.62823(6) 0.15181(3) -0.00416(4) 0.03790(15) Uani 1 1 d . . .
Cl7 Cl 0.94944(7) 0.21249(4) 0.00294(5) 0.04721(18) Uani 1 1 d . . .
Cl8 Cl 0.96043(7) 0.26834(3) 0.20815(5) 0.04563(17) Uani 1 1 d . . .
Cl9 Cl 0.89849(7) 0.09999(3) 0.15668(5) 0.04993(19) Uani 1 1 d . . .
O1 O 0.36764(16) 0.17877(7) 0.08728(11) 0.0313(4) Uani 1 1 d . . .
C1 C 0.3260(2) 0.16791(11) 0.16354(16) 0.0293(5) Uani 1 1 d . . .
C2 C 0.3168(2) 0.22714(11) 0.21491(17) 0.0311(5) Uani 1 1 d . . .
C20 C 0.3449(2) 0.29539(11) 0.18669(17) 0.0327(5) Uani 1 1 d . . .
H20 H 0.3146 0.3319 0.2167 0.039 Uiso 1 1 calc R . .
C3 C 0.2736(3) 0.22036(13) 0.29394(17) 0.0357(5) Uani 1 1 d . . .
H3 H 0.2649 0.2593 0.3276 0.043 Uiso 1 1 calc R . .
C4 C 0.2441(3) 0.15575(13) 0.32190(18) 0.0398(6) Uani 1 1 d . . .
H4 H 0.2184 0.1506 0.3757 0.048 Uiso 1 1 calc R . .
C5 C 0.2526(3) 0.09850(13) 0.26994(17) 0.0385(6) Uani 1 1 d . . .
H5 H 0.2302 0.0555 0.2899 0.046 Uiso 1 1 calc R . .
C6 C 0.2924(2) 0.10140(11) 0.19009(17) 0.0327(5) Uani 1 1 d . . .
C61 C 0.3024(3) 0.03652(12) 0.13434(18) 0.0370(6) Uani 1 1 d . . .
C62 C 0.2626(4) -0.02815(14) 0.1805(2) 0.0659(10) Uani 1 1 d . . .
H62A H 0.3246 -0.0332 0.2373 0.099 Uiso 1 1 calc R . .
H62B H 0.2693 -0.0683 0.1451 0.099 Uiso 1 1 calc R . .
H62C H 0.1692 -0.0235 0.1879 0.099 Uiso 1 1 calc R . .
C63 C 0.2038(3) 0.04289(15) 0.0446(2) 0.0538(8) Uani 1 1 d . . .
H63A H 0.1105 0.0479 0.0524 0.081 Uiso 1 1 calc R . .
H63B H 0.2100 0.0021 0.0104 0.081 Uiso 1 1 calc R . .
H63C H 0.2283 0.0827 0.0144 0.081 Uiso 1 1 calc R . .
C64 C 0.4502(3) 0.02784(14) 0.1232(2) 0.0544(8) Uani 1 1 d . . .
H64A H 0.5118 0.0241 0.1803 0.082 Uiso 1 1 calc R . .
H64B H 0.4757 0.0673 0.0927 0.082 Uiso 1 1 calc R . .
H64C H 0.4565 -0.0133 0.0897 0.082 Uiso 1 1 calc R . .
N2 N 0.4068(2) 0.31242(9) 0.12517(13) 0.0290(4) Uani 1 1 d . . .
C21 C 0.4163(2) 0.38714(11) 0.11099(16) 0.0301(5) Uani 1 1 d . . .
C22 C 0.3086(2) 0.41944(12) 0.05084(17) 0.0329(5) Uani 1 1 d . . .
C221 C 0.1770(3) 0.38236(12) 0.00435(17) 0.0366(6) Uani 1 1 d . . .
H221 H 0.1943 0.3324 0.0099 0.044 Uiso 1 1 calc R . .
C222 C 0.0596(3) 0.39949(14) 0.0502(2) 0.0471(7) Uani 1 1 d . . .
H22A H -0.0235 0.3761 0.0206 0.071 Uiso 1 1 calc R . .
H22B H 0.0439 0.4486 0.0482 0.071 Uiso 1 1 calc R . .
H22C H 0.0846 0.3846 0.1107 0.071 Uiso 1 1 calc R . .
C223 C 0.1349(3) 0.39979(14) -0.09421(19) 0.0459(7) Uani 1 1 d . . .
H22D H 0.0516 0.3751 -0.1205 0.069 Uiso 1 1 calc R . .
H22E H 0.2080 0.3865 -0.1226 0.069 Uiso 1 1 calc R . .
H22F H 0.1186 0.4487 -0.1014 0.069 Uiso 1 1 calc R . .
C23 C 0.3218(3) 0.49064(12) 0.03855(18) 0.0362(5) Uani 1 1 d . . .
H23 H 0.2528 0.5139 -0.0015 0.043 Uiso 1 1 calc R . .
C24 C 0.4341(3) 0.52674(12) 0.08430(18) 0.0388(6) Uani 1 1 d . . .
H24 H 0.4417 0.5739 0.0740 0.047 Uiso 1 1 calc R . .
C25 C 0.5359(3) 0.49370(12) 0.14553(18) 0.0378(6) Uani 1 1 d . . .
H25 H 0.6103 0.5193 0.1771 0.045 Uiso 1 1 calc R . .
C26 C 0.5302(2) 0.42308(11) 0.16121(17) 0.0335(5) Uani 1 1 d . . .
C261 C 0.6390(3) 0.38847(12) 0.23266(18) 0.0404(6) Uani 1 1 d . . .
H261 H 0.6450 0.3398 0.2161 0.048 Uiso 1 1 calc R . .
C262 C 0.5988(3) 0.39055(15) 0.32158(19) 0.0534(8) Uani 1 1 d . . .
H26A H 0.6696 0.3684 0.3653 0.080 Uiso 1 1 calc R . .
H26B H 0.5123 0.3667 0.3173 0.080 Uiso 1 1 calc R . .
H26C H 0.5891 0.4378 0.3383 0.080 Uiso 1 1 calc R . .
C263 C 0.7821(3) 0.42053(15) 0.2419(2) 0.0604(9) Uani 1 1 d . . .
H26D H 0.8471 0.3971 0.2879 0.091 Uiso 1 1 calc R . .
H26E H 0.7785 0.4687 0.2567 0.091 Uiso 1 1 calc R . .
H26F H 0.8112 0.4160 0.1871 0.091 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0328(2) 0.0256(2) 0.0304(2) 0.00069(16) 0.00912(17) 0.00142(15)
Ti2 0.0344(3) 0.0345(2) 0.0389(3) 0.00716(18) 0.01088(19) 0.00537(16)
Cl3 0.0455(4) 0.0447(3) 0.0305(3) 0.0026(2) 0.0068(3) 0.0064(3)
Cl4 0.0342(3) 0.0347(3) 0.0329(3) 0.0056(2) 0.0087(2) 0.0020(2)
Cl5 0.0367(3) 0.0282(3) 0.0366(3) 0.0049(2) 0.0101(2) 0.0012(2)
Cl6 0.0432(3) 0.0311(3) 0.0414(4) -0.0034(2) 0.0137(3) 0.0045(2)
Cl7 0.0452(4) 0.0538(4) 0.0476(4) 0.0084(3) 0.0210(3) 0.0080(3)
Cl8 0.0362(3) 0.0535(4) 0.0456(4) 0.0052(3) 0.0054(3) -0.0008(3)
Cl9 0.0493(4) 0.0410(3) 0.0613(5) 0.0164(3) 0.0162(3) 0.0142(3)
O1 0.0337(9) 0.0283(8) 0.0327(9) 0.0000(6) 0.0088(7) 0.0002(6)
C1 0.0262(11) 0.0330(11) 0.0279(13) 0.0006(9) 0.0047(9) 0.0004(8)
C2 0.0304(12) 0.0308(11) 0.0325(14) 0.0014(9) 0.0078(10) 0.0014(9)
C20 0.0340(13) 0.0300(11) 0.0341(14) -0.0018(9) 0.0072(10) 0.0039(9)
C3 0.0356(13) 0.0385(13) 0.0328(14) -0.0021(10) 0.0073(10) -0.0002(9)
C4 0.0424(14) 0.0442(14) 0.0339(15) 0.0033(11) 0.0109(11) -0.0043(10)
C5 0.0417(14) 0.0373(13) 0.0363(15) 0.0051(10) 0.0084(11) -0.0056(10)
C6 0.0322(12) 0.0309(11) 0.0333(14) 0.0023(9) 0.0037(10) -0.0019(9)
C61 0.0427(14) 0.0281(11) 0.0410(16) -0.0001(10) 0.0113(11) -0.0028(9)
C62 0.109(3) 0.0321(14) 0.067(2) -0.0049(14) 0.043(2) -0.0169(15)
C63 0.0604(19) 0.0466(16) 0.0491(19) -0.0150(13) 0.0010(14) 0.0029(13)
C64 0.0496(17) 0.0334(14) 0.083(2) -0.0058(14) 0.0209(16) 0.0068(11)
N2 0.0316(10) 0.0256(9) 0.0297(11) -0.0001(7) 0.0065(8) 0.0014(7)
C21 0.0368(12) 0.0231(10) 0.0326(13) -0.0008(9) 0.0123(10) 0.0020(8)
C22 0.0367(13) 0.0304(11) 0.0344(14) 0.0007(10) 0.0138(10) 0.0053(9)
C221 0.0363(13) 0.0320(12) 0.0409(15) 0.0024(10) 0.0075(11) 0.0038(9)
C222 0.0417(15) 0.0425(14) 0.059(2) 0.0051(12) 0.0157(13) 0.0026(11)
C223 0.0435(16) 0.0483(15) 0.0430(17) 0.0031(12) 0.0034(12) 0.0034(11)
C23 0.0430(14) 0.0312(12) 0.0376(15) 0.0035(10) 0.0161(11) 0.0080(10)
C24 0.0521(16) 0.0249(11) 0.0448(16) 0.0005(10) 0.0225(12) 0.0024(10)
C25 0.0445(14) 0.0300(12) 0.0420(15) -0.0067(10) 0.0162(11) -0.0044(10)
C26 0.0392(13) 0.0290(11) 0.0338(14) -0.0039(9) 0.0118(10) 0.0011(9)
C261 0.0410(14) 0.0333(12) 0.0426(16) -0.0049(11) 0.0003(11) 0.0004(10)
C262 0.069(2) 0.0514(16) 0.0342(16) -0.0043(12) -0.0004(13) 0.0125(13)
C263 0.0486(18) 0.0470(16) 0.076(2) -0.0069(15) -0.0056(15) -0.0046(13)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 1.7843(16) . ?
Ti1 N2 2.138(2) . ?
Ti1 Cl3 2.1987(10) . ?
Ti1 Cl6 2.4091(7) . ?
Ti1 Cl5 2.4336(7) . ?
Ti1 Cl4 2.4907(10) . ?
Ti1 Ti2 3.3578(7) . ?
Ti2 Cl8 2.1845(9) . ?
Ti2 Cl9 2.1971(7) . ?
Ti2 Cl7 2.2106(10) . ?
Ti2 Cl4 2.4618(9) . ?
Ti2 Cl6 2.5381(9) . ?
Ti2 Cl5 2.5417(7) . ?
O1 C1 1.352(3) . ?
C1 C2 1.409(3) . ?
C1 C6 1.411(3) . ?
C2 C3 1.390(4) . ?
C2 C20 1.436(3) . ?
C20 N2 1.285(3) . ?
C20 H20 0.9300 . ?
C3 C4 1.374(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.381(4) . ?
C5 H5 0.9300 . ?
C6 C61 1.538(3) . ?
C61 C63 1.516(4) . ?
C61 C64 1.517(4) . ?
C61 C62 1.533(4) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
N2 C21 1.466(3) . ?
C21 C22 1.397(3) . ?
C21 C26 1.402(3) . ?
C22 C23 1.398(3) . ?
C22 C221 1.519(4) . ?
C221 C222 1.525(4) . ?
C221 C223 1.530(4) . ?
C221 H221 0.9800 . ?
C222 H22A 0.9600 . ?
C222 H22B 0.9600 . ?
C222 H22C 0.9600 . ?
C223 H22D 0.9600 . ?
C223 H22E 0.9600 . ?
C223 H22F 0.9600 . ?
C23 C24 1.368(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.378(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.389(3) . ?
C25 H25 0.9300 . ?
C26 C261 1.518(3) . ?
C261 C262 1.518(4) . ?
C261 C263 1.521(4) . ?
C261 H261 0.9800 . ?
C262 H26A 0.9600 . ?
C262 H26B 0.9600 . ?
C262 H26C 0.9600 . ?
C263 H26D 0.9600 . ?
C263 H26E 0.9600 . ?
C263 H26F 0.9600 . ?

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 N2 84.76(7) . . ?
O1 Ti1 Cl3 102.52(6) . . ?
N2 Ti1 Cl3 98.44(6) . . ?
O1 Ti1 Cl6 100.33(5) . . ?
N2 Ti1 Cl6 166.23(6) . . ?
Cl3 Ti1 Cl6 92.97(3) . . ?
O1 Ti1 Cl5 163.22(6) . . ?
N2 Ti1 Cl5 89.87(5) . . ?
Cl3 Ti1 Cl5 93.98(3) . . ?
Cl6 Ti1 Cl5 81.62(2) . . ?
O1 Ti1 Cl4 84.37(6) . . ?
N2 Ti1 Cl4 87.43(6) . . ?
Cl3 Ti1 Cl4 171.28(3) . . ?
Cl6 Ti1 Cl4 80.40(3) . . ?
Cl5 Ti1 Cl4 79.51(2) . . ?
O1 Ti1 Ti2 120.67(5) . . ?
N2 Ti1 Ti2 117.55(5) . . ?
Cl3 Ti1 Ti2 124.33(3) . . ?
Cl6 Ti1 Ti2 48.89(2) . . ?
Cl5 Ti1 Ti2 48.930(17) . . ?
Cl4 Ti1 Ti2 46.95(2) . . ?
Cl8 Ti2 Cl9 100.63(4) . . ?
Cl8 Ti2 Cl7 98.90(4) . . ?
Cl9 Ti2 Cl7 98.76(3) . . ?
Cl8 Ti2 Cl4 90.71(3) . . ?
Cl9 Ti2 Cl4 89.89(3) . . ?
Cl7 Ti2 Cl4 165.61(3) . . ?
Cl8 Ti2 Cl6 164.38(3) . . ?
Cl9 Ti2 Cl6 90.69(3) . . ?
Cl7 Ti2 Cl6 89.87(4) . . ?
Cl4 Ti2 Cl6 78.48(3) . . ?
Cl8 Ti2 Cl5 89.75(3) . . ?
Cl9 Ti2 Cl5 164.20(3) . . ?
Cl7 Ti2 Cl5 91.27(3) . . ?
Cl4 Ti2 Cl5 78.00(3) . . ?
Cl6 Ti2 Cl5 77.08(2) . . ?
Cl8 Ti2 Ti1 118.81(3) . . ?
Cl9 Ti2 Ti1 117.99(3) . . ?
Cl7 Ti2 Ti1 117.94(3) . . ?
Cl4 Ti2 Ti1 47.67(2) . . ?
Cl6 Ti2 Ti1 45.659(18) . . ?
Cl5 Ti2 Ti1 46.208(16) . . ?
Ti2 Cl4 Ti1 85.38(3) . . ?
Ti1 Cl5 Ti2 84.86(2) . . ?
Ti1 Cl6 Ti2 85.45(3) . . ?
C1 O1 Ti1 135.86(14) . . ?
O1 C1 C2 116.1(2) . . ?
O1 C1 C6 122.2(2) . . ?
C2 C1 C6 121.7(2) . . ?
C3 C2 C1 119.6(2) . . ?
C3 C2 C20 118.2(2) . . ?
C1 C2 C20 122.1(2) . . ?
N2 C20 C2 128.1(2) . . ?
N2 C20 H20 115.9 . . ?
C2 C20 H20 115.9 . . ?
C4 C3 C2 119.5(2) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 123.8(2) . . ?
C6 C5 H5 118.1 . . ?
C4 C5 H5 118.1 . . ?
C5 C6 C1 115.5(2) . . ?
C5 C6 C61 122.5(2) . . ?
C1 C6 C61 122.0(2) . . ?
C63 C61 C64 110.1(3) . . ?
C63 C61 C62 108.4(2) . . ?
C64 C61 C62 108.4(2) . . ?
C63 C61 C6 110.0(2) . . ?
C64 C61 C6 109.7(2) . . ?
C62 C61 C6 110.3(2) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C20 N2 C21 114.85(19) . . ?
C20 N2 Ti1 120.85(15) . . ?
C21 N2 Ti1 124.29(15) . . ?
C22 C21 C26 123.3(2) . . ?
C22 C21 N2 118.4(2) . . ?
C26 C21 N2 118.3(2) . . ?
C21 C22 C23 116.8(2) . . ?
C21 C22 C221 123.5(2) . . ?
C23 C22 C221 119.6(2) . . ?
C22 C221 C222 109.6(2) . . ?
C22 C221 C223 112.7(2) . . ?
C222 C221 C223 110.6(2) . . ?
C22 C221 H221 107.9 . . ?
C222 C221 H221 107.9 . . ?
C223 C221 H221 107.9 . . ?
C221 C222 H22A 109.5 . . ?
C221 C222 H22B 109.5 . . ?
H22A C222 H22B 109.5 . . ?
C221 C222 H22C 109.5 . . ?
H22A C222 H22C 109.5 . . ?
H22B C222 H22C 109.5 . . ?
C221 C223 H22D 109.5 . . ?
C221 C223 H22E 109.5 . . ?
H22D C223 H22E 109.5 . . ?
C221 C223 H22F 109.5 . . ?
H22D C223 H22F 109.5 . . ?
H22E C223 H22F 109.5 . . ?
C24 C23 C22 121.3(2) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C24 C25 120.4(2) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C26 121.6(2) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
C25 C26 C21 116.6(2) . . ?
C25 C26 C261 120.7(2) . . ?
C21 C26 C261 122.6(2) . . ?
C26 C261 C262 111.5(2) . . ?
C26 C261 C263 112.5(2) . . ?
C262 C261 C263 109.2(2) . . ?
C26 C261 H261 107.8 . . ?
C262 C261 H261 107.8 . . ?
C263 C261 H261 107.8 . . ?
C261 C262 H26A 109.5 . . ?
C261 C262 H26B 109.5 . . ?
H26A C262 H26B 109.5 . . ?
C261 C262 H26C 109.5 . . ?
H26A C262 H26C 109.5 . . ?
H26B C262 H26C 109.5 . . ?
C261 C263 H26D 109.5 . . ?
C261 C263 H26E 109.5 . . ?
H26D C263 H26E 109.5 . . ?
C261 C263 H26F 109.5 . . ?
H26D C263 H26F 109.5 . . ?
H26E C263 H26F 109.5 . . ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Ti1 Ti2 Cl8 -105.95(7) . . . . ?
N2 Ti1 Ti2 Cl8 -5.01(7) . . . . ?
Cl3 Ti1 Ti2 Cl8 118.81(4) . . . . ?
Cl6 Ti1 Ti2 Cl8 177.98(4) . . . . ?
Cl5 Ti1 Ti2 Cl8 57.72(4) . . . . ?
Cl4 Ti1 Ti2 Cl8 -61.20(4) . . . . ?
O1 Ti1 Ti2 Cl9 16.10(7) . . . . ?
N2 Ti1 Ti2 Cl9 117.04(7) . . . . ?
Cl3 Ti1 Ti2 Cl9 -119.14(4) . . . . ?
Cl6 Ti1 Ti2 Cl9 -59.97(4) . . . . ?
Cl5 Ti1 Ti2 Cl9 179.77(4) . . . . ?
Cl4 Ti1 Ti2 Cl9 60.85(3) . . . . ?
O1 Ti1 Ti2 Cl7 134.60(7) . . . . ?
N2 Ti1 Ti2 Cl7 -124.46(7) . . . . ?
Cl3 Ti1 Ti2 Cl7 -0.64(4) . . . . ?
Cl6 Ti1 Ti2 Cl7 58.53(4) . . . . ?
Cl5 Ti1 Ti2 Cl7 -61.72(3) . . . . ?
Cl4 Ti1 Ti2 Cl7 179.35(4) . . . . ?
O1 Ti1 Ti2 Cl4 -44.75(7) . . . . ?
N2 Ti1 Ti2 Cl4 56.19(6) . . . . ?
Cl3 Ti1 Ti2 Cl4 -179.99(3) . . . . ?
Cl6 Ti1 Ti2 Cl4 -120.82(3) . . . . ?
Cl5 Ti1 Ti2 Cl4 118.92(3) . . . . ?
O1 Ti1 Ti2 Cl6 76.07(7) . . . . ?
N2 Ti1 Ti2 Cl6 177.01(6) . . . . ?
Cl3 Ti1 Ti2 Cl6 -59.17(4) . . . . ?
Cl5 Ti1 Ti2 Cl6 -120.26(4) . . . . ?
Cl4 Ti1 Ti2 Cl6 120.82(3) . . . . ?
O1 Ti1 Ti2 Cl5 -163.67(7) . . . . ?
N2 Ti1 Ti2 Cl5 -62.74(6) . . . . ?
Cl3 Ti1 Ti2 Cl5 61.09(3) . . . . ?
Cl6 Ti1 Ti2 Cl5 120.26(4) . . . . ?
Cl4 Ti1 Ti2 Cl5 -118.92(3) . . . . ?
Cl8 Ti2 Cl4 Ti1 129.83(3) . . . . ?
Cl9 Ti2 Cl4 Ti1 -129.54(3) . . . . ?
Cl7 Ti2 Cl4 Ti1 -2.30(13) . . . . ?
Cl6 Ti2 Cl4 Ti1 -38.82(2) . . . . ?
Cl5 Ti2 Cl4 Ti1 40.24(2) . . . . ?
O1 Ti1 Cl4 Ti2 142.52(5) . . . . ?
N2 Ti1 Cl4 Ti2 -132.49(5) . . . . ?
Cl3 Ti1 Cl4 Ti2 0.05(19) . . . . ?
Cl6 Ti1 Cl4 Ti2 41.02(2) . . . . ?
Cl5 Ti1 Cl4 Ti2 -42.15(2) . . . . ?
O1 Ti1 Cl5 Ti2 56.89(19) . . . . ?
N2 Ti1 Cl5 Ti2 127.99(6) . . . . ?
Cl3 Ti1 Cl5 Ti2 -133.56(3) . . . . ?
Cl6 Ti1 Cl5 Ti2 -41.14(3) . . . . ?
Cl4 Ti1 Cl5 Ti2 40.58(2) . . . . ?
Cl8 Ti2 Cl5 Ti1 -132.20(3) . . . . ?
Cl9 Ti2 Cl5 Ti1 -0.74(13) . . . . ?
Cl7 Ti2 Cl5 Ti1 128.90(3) . . . . ?
Cl4 Ti2 Cl5 Ti1 -41.42(2) . . . . ?
Cl6 Ti2 Cl5 Ti1 39.33(3) . . . . ?
O1 Ti1 Cl6 Ti2 -121.94(6) . . . . ?
N2 Ti1 Cl6 Ti2 -11.2(2) . . . . ?
Cl3 Ti1 Cl6 Ti2 134.76(3) . . . . ?
Cl5 Ti1 Cl6 Ti2 41.17(2) . . . . ?
Cl4 Ti1 Cl6 Ti2 -39.53(2) . . . . ?
Cl8 Ti2 Cl6 Ti1 -6.59(12) . . . . ?
Cl9 Ti2 Cl6 Ti1 130.13(3) . . . . ?
Cl7 Ti2 Cl6 Ti1 -131.10(3) . . . . ?
Cl4 Ti2 Cl6 Ti1 40.39(2) . . . . ?
Cl5 Ti2 Cl6 Ti1 -39.77(2) . . . . ?
N2 Ti1 O1 C1 -42.0(2) . . . . ?
Cl3 Ti1 O1 C1 -139.54(19) . . . . ?
Cl6 Ti1 O1 C1 125.04(19) . . . . ?
Cl5 Ti1 O1 C1 29.8(3) . . . . ?
Cl4 Ti1 O1 C1 45.89(19) . . . . ?
Ti2 Ti1 O1 C1 77.0(2) . . . . ?
Ti1 O1 C1 C2 36.2(3) . . . . ?
Ti1 O1 C1 C6 -144.30(18) . . . . ?
O1 C1 C2 C3 179.5(2) . . . . ?
C6 C1 C2 C3 0.0(3) . . . . ?
O1 C1 C2 C20 2.2(3) . . . . ?
C6 C1 C2 C20 -177.3(2) . . . . ?
C3 C2 C20 N2 167.3(2) . . . . ?
C1 C2 C20 N2 -15.4(4) . . . . ?
C1 C2 C3 C4 1.7(3) . . . . ?
C20 C2 C3 C4 179.1(2) . . . . ?
C2 C3 C4 C5 -2.3(4) . . . . ?
C3 C4 C5 C6 1.3(4) . . . . ?
C4 C5 C6 C1 0.4(4) . . . . ?
C4 C5 C6 C61 179.3(2) . . . . ?
O1 C1 C6 C5 179.5(2) . . . . ?
C2 C1 C6 C5 -1.0(3) . . . . ?
O1 C1 C6 C61 0.6(3) . . . . ?
C2 C1 C6 C61 -180.0(2) . . . . ?
C5 C6 C61 C63 119.4(3) . . . . ?
C1 C6 C61 C63 -61.7(3) . . . . ?
C5 C6 C61 C64 -119.3(3) . . . . ?
C1 C6 C61 C64 59.5(3) . . . . ?
C5 C6 C61 C62 0.0(4) . . . . ?
C1 C6 C61 C62 178.8(2) . . . . ?
C2 C20 N2 C21 178.6(2) . . . . ?
C2 C20 N2 Ti1 -1.5(3) . . . . ?
O1 Ti1 N2 C20 21.13(19) . . . . ?
Cl3 Ti1 N2 C20 123.04(18) . . . . ?
Cl6 Ti1 N2 C20 -91.4(3) . . . . ?
Cl5 Ti1 N2 C20 -142.96(18) . . . . ?
Cl4 Ti1 N2 C20 -63.45(18) . . . . ?
Ti2 Ti1 N2 C20 -100.88(18) . . . . ?
O1 Ti1 N2 C21 -158.90(18) . . . . ?
Cl3 Ti1 N2 C21 -56.99(17) . . . . ?
Cl6 Ti1 N2 C21 88.6(3) . . . . ?
Cl5 Ti1 N2 C21 37.01(17) . . . . ?
Cl4 Ti1 N2 C21 116.52(17) . . . . ?
Ti2 Ti1 N2 C21 79.09(17) . . . . ?
C20 N2 C21 C22 -89.5(3) . . . . ?
Ti1 N2 C21 C22 90.5(2) . . . . ?
C20 N2 C21 C26 87.8(3) . . . . ?
Ti1 N2 C21 C26 -92.1(2) . . . . ?
C26 C21 C22 C23 3.3(4) . . . . ?
N2 C21 C22 C23 -179.5(2) . . . . ?
C26 C21 C22 C221 -172.5(2) . . . . ?
N2 C21 C22 C221 4.7(4) . . . . ?
C21 C22 C221 C222 100.7(3) . . . . ?
C23 C22 C221 C222 -75.0(3) . . . . ?
C21 C22 C221 C223 -135.7(2) . . . . ?
C23 C22 C221 C223 48.6(3) . . . . ?
C21 C22 C23 C24 -0.8(4) . . . . ?
C221 C22 C23 C24 175.1(2) . . . . ?
C22 C23 C24 C25 -1.5(4) . . . . ?
C23 C24 C25 C26 1.7(4) . . . . ?
C24 C25 C26 C21 0.6(4) . . . . ?
C24 C25 C26 C261 -176.4(2) . . . . ?
C22 C21 C26 C25 -3.2(4) . . . . ?
N2 C21 C26 C25 179.6(2) . . . . ?
C22 C21 C26 C261 173.9(2) . . . . ?
N2 C21 C26 C261 -3.3(4) . . . . ?
C25 C26 C261 C262 88.2(3) . . . . ?
C21 C26 C261 C262 -88.6(3) . . . . ?
C25 C26 C261 C263 -34.8(3) . . . . ?
C21 C26 C261 C263 148.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.943
_diffrn_reflns_theta_full        25.56
_diffrn_measured_fraction_theta_full 0.943
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.063