Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2001


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data_global

_journal_coden_Cambridge   186   


loop_
_publ_author_name
'M.P.Coles'
'P.B.Hitchcock'

_publ_contact_author_name     	'Dr Martyn P Coles'  
_publ_contact_author_address 
;
School of Chemistry, Physics and Environmental Science
University of Sussex
Falmer
Brighton
BN1 9QJ
UNITED KINGDOM
;

_publ_contact_author_email  M.P.COLES@SUSSEX.AC.UK

data_oct1500

_database_code_CSD	160792

_audit_creation_date 2000-10-10T08:52:25-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
_audit_conform_dict_name cif_core.dic
_audit_conform_dict_version 2.1
_audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic
_publ_requested_category FM
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic
;
?
;
_chemical_name_common '[(C7H12N3)2TiCl2].toluene'
_chemical_formula_moiety '(C14 H24 Cl2 N6 Ti1)(C7 H8)'
_chemical_formula_sum 'C21 H32 Cl2 N6 Ti'
_chemical_formula_weight 487.33
_chemical_compound_source 'synthesis as described'
#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P2(1)/n
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_Int_Tables_number 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 12.4604(6)
_cell_length_b 8.4351(6)
_cell_length_c 22.9507(15)
_cell_angle_alpha 90
_cell_angle_beta 104.261(4)
_cell_angle_gamma 90
_cell_volume 2337.9(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 6851
_cell_measurement_theta_min 3.705
_cell_measurement_theta_max 22.986
_cell_measurement_wavelength 0.71073
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_description plate
_exptl_crystal_colour red
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.05
_exptl_crystal_density_diffrn 1.385
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1024
_exptl_special_details
;
?
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu 0.615
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min 0.900
_exptl_absorpt_correction_T_max 0.950
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_measurement_device KappaCCD
_diffrn_measurement_method CCD
_diffrn_reflns_number 10686
_diffrn_reflns_av_R_equivalents 0.0704
_diffrn_reflns_av_unetI/netI 0.0642
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_theta_min 3.73
_diffrn_reflns_theta_max 22.97
_diffrn_reflns_theta_full 22.97
_diffrn_measured_fraction_theta_full
0.994
_diffrn_measured_fraction_theta_max
0.994
_reflns_number_total 3230
_reflns_number_gt 2507
_reflns_threshold_expression >2sigma(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_cell_refinement
'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX publication routines (Farrugia, 1999)'
#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_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^)+(0.0344P)^2^+1.2966P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_ls_hydrogen_treatment 'refined isotropic'
_refine_ls_extinction_method none
_refine_ls_number_reflns 3230
_refine_ls_number_parameters 399
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0619
_refine_ls_R_factor_gt 0.0405
_refine_ls_wR_factor_ref 0.0914
_refine_ls_wR_factor_gt 0.0834
_refine_ls_goodness_of_fit_ref 1.006
_refine_ls_restrained_S_all 1.006
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0
_refine_diff_density_max 0.216
_refine_diff_density_min -0.283
_refine_diff_density_rms 0.055
#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#
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 0 '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'
N N 0.0061 0.0033 '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_
_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 0.97555(4) 0.44436(7) 0.17182(3) 0.02018(19) Uani 1 1 d . . .
Cl1 Cl 0.78895(6) 0.50848(11) 0.16264(4) 0.0317(3) Uani 1 1 d . . .
Cl2 Cl 0.99509(6) 0.63740(11) 0.10185(4) 0.0285(2) Uani 1 1 d . . .
N1 N 0.9864(2) 0.2754(3) 0.11152(12) 0.0247(7) Uani 1 1 d . . .
N2 N 0.9444(2) 0.2165(3) 0.19635(12) 0.0236(7) Uani 1 1 d . . .
N3 N 0.8741(2) 0.0476(3) 0.11227(12) 0.0254(7) Uani 1 1 d . . .
N4 N 1.0134(2) 0.5377(3) 0.25584(12) 0.0211(6) Uani 1 1 d . . .
N5 N 1.1394(2) 0.4350(3) 0.21549(12) 0.0209(6) Uani 1 1 d . . .
N6 N 1.1795(2) 0.4440(4) 0.32224(12) 0.0275(7) Uani 1 1 d . . .
C1 C 0.9342(3) 0.1708(4) 0.13934(15) 0.0240(8) Uani 1 1 d . . .
C2 C 0.9867(3) 0.2487(5) 0.04866(16) 0.0314(9) Uani 1 1 d . . .
H2B H 0.992(3) 0.345(4) 0.0321(15) 0.023(10) Uiso 1 1 d . . .
H2A H 1.051(3) 0.178(5) 0.0478(18) 0.058(13) Uiso 1 1 d . . .
C3 C 0.8795(3) 0.1715(5) 0.01602(18) 0.0359(10) Uani 1 1 d . . .
H3B H 0.884(3) 0.148(5) -0.0198(17) 0.037(11) Uiso 1 1 d . . .
H3A H 0.812(3) 0.244(4) 0.0168(15) 0.036(10) Uiso 1 1 d . . .
C4 C 0.8587(4) 0.0209(5) 0.04755(17) 0.0349(9) Uani 1 1 d . . .
H4B H 0.783(3) -0.013(5) 0.0319(17) 0.045(11) Uiso 1 1 d . . .
H4A H 0.913(3) -0.062(5) 0.0412(16) 0.042(11) Uiso 1 1 d . . .
C5 C 0.8133(3) -0.0521(5) 0.14519(17) 0.0301(9) Uani 1 1 d . . .
H5A H 0.815(3) -0.156(5) 0.1331(15) 0.026(10) Uiso 1 1 d . . .
H5B H 0.735(3) -0.016(4) 0.1324(14) 0.028(9) Uiso 1 1 d . . .
C6 C 0.8578(3) -0.0343(4) 0.21201(17) 0.0288(9) Uani 1 1 d . . .
H6B H 0.809(2) -0.084(4) 0.2318(13) 0.018(8) Uiso 1 1 d . . .
H6A H 0.929(3) -0.079(4) 0.2226(15) 0.030(10) Uiso 1 1 d . . .
C7 C 0.8714(3) 0.1402(5) 0.22935(18) 0.0301(9) Uani 1 1 d . . .
H7B H 0.905(3) 0.145(4) 0.2724(17) 0.030(10) Uiso 1 1 d . . .
H7A H 0.800(3) 0.197(4) 0.2174(14) 0.023(9) Uiso 1 1 d . . .
C8 C 1.1151(3) 0.4733(4) 0.26736(14) 0.0209(8) Uani 1 1 d . . .
C9 C 0.9677(3) 0.5814(5) 0.30631(16) 0.0327(9) Uani 1 1 d . . .
H9B H 0.983(3) 0.689(5) 0.3168(16) 0.039(11) Uiso 1 1 d . . .
H9A H 0.891(3) 0.569(4) 0.2948(16) 0.038(10) Uiso 1 1 d . . .
C10 C 1.0149(3) 0.4750(6) 0.36062(17) 0.0369(10) Uani 1 1 d . . .
H10B H 0.991(3) 0.361(4) 0.3524(14) 0.023(9) Uiso 1 1 d . . .
H10A H 0.989(2) 0.512(4) 0.3920(15) 0.020(9) Uiso 1 1 d . . .
C11 C 1.1403(3) 0.4793(6) 0.37560(17) 0.0376(10) Uani 1 1 d . . .
H11A H 1.169(3) 0.583(5) 0.3896(18) 0.045(12) Uiso 1 1 d . . .
H11B H 1.171(3) 0.406(5) 0.4063(17) 0.039(11) Uiso 1 1 d . . .
C12 C 1.2895(3) 0.3723(6) 0.32943(19) 0.0369(10) Uani 1 1 d . . .
H12B H 1.288(3) 0.264(6) 0.3434(18) 0.056(13) Uiso 1 1 d . . .
H12A H 1.337(3) 0.430(5) 0.3605(18) 0.047(12) Uiso 1 1 d . . .
C13 C 1.3261(3) 0.3698(5) 0.27167(17) 0.0313(9) Uani 1 1 d . . .
H13B H 1.381(3) 0.294(4) 0.2740(14) 0.030(10) Uiso 1 1 d . . .
H13A H 1.357(3) 0.481(5) 0.2627(15) 0.036(10) Uiso 1 1 d . . .
C14 C 1.2314(3) 0.3240(5) 0.21917(17) 0.0284(9) Uani 1 1 d . . .

H14A H 1.203(3) 0.222(5) 0.2237(15) 0.032(10) Uiso 1 1 d . . .
H14B H 1.253(3) 0.323(4) 0.1836(15) 0.022(9) Uiso 1 1 d . . .
C15 C 0.4730(3) 0.3425(5) 0.04564(19) 0.0398(10) Uani 1 1 d . . .
C16 C 0.4801(3) 0.4305(5) 0.0966(2) 0.0428(11) Uani 1 1 d . . .
H16 H 0.547(3) 0.450(5) 0.1231(17) 0.042(11) Uiso 1 1 d . . .
C17 C 0.3859(3) 0.4952(5) 0.1102(2) 0.0417(10) Uani 1 1 d . . .
H17 H 0.391(2) 0.558(4) 0.1444(15) 0.020(9) Uiso 1 1 d . . .
C18 C 0.2841(3) 0.4711(5) 0.0714(2) 0.0429(11) Uani 1 1 d . . .
H18 H 0.218(3) 0.518(4) 0.0770(16) 0.039(11) Uiso 1 1 d . . .
C19 C 0.2769(3) 0.3863(6) 0.0199(2) 0.0478(12) Uani 1 1 d . . .
H19 H 0.218(3) 0.367(5) -0.0096(18) 0.046(12) Uiso 1 1 d . . .
C20 C 0.3705(3) 0.3218(5) 0.0073(2) 0.0443(11) Uani 1 1 d . . .
H20 H 0.379(3) 0.261(5) -0.0292(18) 0.048(12) Uiso 1 1 d . . .
C21 C 0.5760(4) 0.2727(7) 0.0316(3) 0.0577(14) Uani 1 1 d . . .
H21C H 0.646(6) 0.253(8) 0.068(3) 0.14(3) Uiso 1 1 d . . .
H21B H 0.555(4) 0.162(8) 0.011(2) 0.10(2) Uiso 1 1 d . . .
H21A H 0.610(5) 0.336(8) 0.005(3) 0.12(2) Uiso 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 0.0192(3) 0.0216(4) 0.0202(3) -0.0014(3) 0.0056(2) -0.0030(3)
Cl1 0.0195(4) 0.0390(6) 0.0360(5) 0.0044(4) 0.0059(4) -0.0003(4)
Cl2 0.0277(5) 0.0306(5) 0.0265(5) 0.0053(4) 0.0055(4) -0.0050(4)
N1 0.0298(16) 0.0247(17) 0.0209(16) -0.0030(13) 0.0090(13) -0.0072(13)
N2 0.0290(15) 0.0251(17) 0.0200(17) -0.0013(13) 0.0119(12) -0.0055(13)
N3 0.0311(16) 0.0203(17) 0.0281(17) -0.0030(14) 0.0137(13) -0.0067(14)
N4 0.0179(14) 0.0228(16) 0.0228(16) -0.0018(13) 0.0052(11) 0.0020(12)
N5 0.0177(14) 0.0205(16) 0.0260(16) 0.0008(13) 0.0081(12) 0.0007(12)
N6 0.0227(15) 0.0361(19) 0.0215(17) 0.0025(14) 0.0009(13) 0.0054(14)
C1 0.0216(18) 0.023(2) 0.030(2) 0.0016(17) 0.0101(15) 0.0023(16)
C2 0.043(2) 0.036(3) 0.020(2) 0.0003(19) 0.0168(18) -0.004(2)
C3 0.045(2) 0.040(3) 0.023(2) -0.007(2) 0.0111(19) -0.006(2)
C4 0.045(2) 0.028(2) 0.032(2) -0.0093(18) 0.0083(19) -0.008(2)
C5 0.033(2) 0.019(2) 0.042(3) -0.0043(19) 0.0163(18) -0.0062(18)
C6 0.028(2) 0.024(2) 0.038(2) 0.0063(18) 0.0168(18) -0.0023(18)
C7 0.036(2) 0.031(2) 0.027(2) 0.0027(19) 0.0159(18) -0.0042(19)
C8 0.0213(18) 0.0163(19) 0.026(2) -0.0017(15) 0.0085(15) -0.0059(15)
C9 0.028(2) 0.044(3) 0.027(2) -0.008(2) 0.0070(17) 0.005(2)
C10 0.038(2) 0.049(3) 0.028(2) -0.008(2) 0.0160(19) 0.006(2)
C11 0.038(2) 0.051(3) 0.021(2) 0.001(2) 0.0027(17) 0.008(2)
C12 0.021(2) 0.047(3) 0.040(3) 0.004(2) 0.0013(18) 0.0086(19)
C13 0.0235(19) 0.025(2) 0.046(3) 0.0019(19) 0.0100(17) 0.0096(19)
C14 0.029(2) 0.028(2) 0.032(2) 0.0025(18) 0.0141(18) 0.0048(18)
C15 0.037(2) 0.036(3) 0.049(3) 0.018(2) 0.016(2) -0.0003(19)
C16 0.029(2) 0.048(3) 0.046(3) 0.019(2) 0.001(2) -0.006(2)
C17 0.046(3) 0.040(3) 0.040(3) 0.002(2) 0.013(2) -0.005(2)
C18 0.033(2) 0.043(3) 0.055(3) 0.018(2) 0.014(2) 0.003(2)
C19 0.033(2) 0.052(3) 0.049(3) 0.014(2) -0.008(2) -0.011(2)
C20 0.050(3) 0.040(3) 0.044(3) 0.000(2) 0.014(2) -0.008(2)
C21 0.049(3) 0.049(3) 0.084(4) 0.015(3) 0.034(3) 0.006(3)
#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#
_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 N1 2.014(3) . ?
Ti N4 2.028(3) . ?
Ti N5 2.043(2) . ?
Ti N2 2.066(3) . ?
Ti Cl2 2.3414(10) . ?
Ti Cl1 2.3455(9) . ?
Ti C1 2.441(4) . ?
Ti C8 2.452(3) . ?
N1 C1 1.347(4) . ?
N1 C2 1.461(4) . ?
N2 C1 1.340(4) . ?
N2 C7 1.467(4) . ?
N3 C1 1.340(4) . ?
N3 C5 1.461(4) . ?
N3 C4 1.468(4) . ?
N4 C8 1.344(4) . ?
N4 C9 1.458(4) . ?
N5 C8 1.338(4) . ?
N5 C14 1.466(4) . ?
N6 C8 1.339(4) . ?
N6 C11 1.457(5) . ?
N6 C12 1.469(4) . ?
C2 C3 1.509(5) . ?
C3 C4 1.515(5) . ?
C5 C6 1.504(5) . ?
C6 C7 1.524(5) . ?
C9 C10 1.531(6) . ?
C10 C11 1.514(5) . ?
C12 C13 1.505(5) . ?
C13 C14 1.515(5) . ?
C15 C16 1.370(6) . ?
C15 C20 1.372(6) . ?
C15 C21 1.517(6) . ?
C16 C17 1.398(6) . ?
C17 C18 1.374(6) . ?
C18 C19 1.366(6) . ?
C19 C20 1.380(6) . ?
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 Ti N4 152.73(11) . . ?
N1 Ti N5 94.68(11) . . ?
N4 Ti N5 65.06(10) . . ?
N1 Ti N2 65.04(11) . . ?
N4 Ti N2 96.74(11) . . ?
N5 Ti N2 93.59(11) . . ?
N1 Ti Cl2 89.13(8) . . ?
N4 Ti Cl2 110.05(8) . . ?
N5 Ti Cl2 95.93(8) . . ?
N2 Ti Cl2 153.13(8) . . ?
N1 Ti Cl1 109.53(8) . . ?
N4 Ti Cl1 89.36(7) . . ?
N5 Ti Cl1 154.42(8) . . ?
N2 Ti Cl1 89.44(8) . . ?
Cl2 Ti Cl1 92.65(4) . . ?
N1 Ti C1 33.49(10) . . ?
N4 Ti C1 129.77(11) . . ?
N5 Ti C1 102.91(11) . . ?
N2 Ti C1 33.29(10) . . ?
Cl2 Ti C1 119.86(8) . . ?
Cl1 Ti C1 93.48(8) . . ?
N1 Ti C8 122.14(11) . . ?
N4 Ti C8 33.24(10) . . ?
N5 Ti C8 33.08(10) . . ?
N2 Ti C8 89.34(11) . . ?
Cl2 Ti C8 111.93(8) . . ?
Cl1 Ti C8 121.75(8) . . ?
C1 Ti C8 114.64(11) . . ?
C1 N1 C2 119.1(3) . . ?
C1 N1 Ti 90.92(19) . . ?
C2 N1 Ti 143.6(3) . . ?
C1 N2 C7 117.2(3) . . ?
C1 N2 Ti 88.9(2) . . ?
C7 N2 Ti 136.9(2) . . ?
C1 N3 C5 120.5(3) . . ?
C1 N3 C4 120.5(3) . . ?
C5 N3 C4 118.7(3) . . ?
C8 N4 C9 118.7(3) . . ?
C8 N4 Ti 90.97(19) . . ?
C9 N4 Ti 144.0(2) . . ?
C8 N5 C14 116.6(3) . . ?
C8 N5 Ti 90.52(18) . . ?
C14 N5 Ti 136.5(2) . . ?
C8 N6 C11 120.3(3) . . ?
C8 N6 C12 120.5(3) . . ?
C11 N6 C12 119.1(3) . . ?
N2 C1 N3 125.7(3) . . ?
N2 C1 N1 109.5(3) . . ?
N3 C1 N1 124.6(3) . . ?
N2 C1 Ti 57.83(17) . . ?
N3 C1 Ti 157.8(2) . . ?
N1 C1 Ti 55.60(17) . . ?
N1 C2 C3 109.8(3) . . ?
C2 C3 C4 111.0(3) . . ?
N3 C4 C3 111.1(3) . . ?
N3 C5 C6 111.2(3) . . ?
C5 C6 C7 110.6(3) . . ?
N2 C7 C6 109.4(3) . . ?
N5 C8 N6 125.3(3) . . ?
N5 C8 N4 109.4(3) . . ?

N6 C8 N4 125.3(3) . . ?
N5 C8 Ti 56.40(16) . . ?
N6 C8 Ti 162.0(2) . . ?
N4 C8 Ti 55.79(16) . . ?
N4 C9 C10 110.6(3) . . ?
C11 C10 C9 109.8(3) . . ?
N6 C11 C10 110.2(3) . . ?
N6 C12 C13 112.6(3) . . ?
C12 C13 C14 111.0(3) . . ?
N5 C14 C13 109.2(3) . . ?
C16 C15 C20 118.1(4) . . ?
C16 C15 C21 120.7(4) . . ?
C20 C15 C21 121.1(4) . . ?
C15 C16 C17 121.4(4) . . ?
C18 C17 C16 119.3(5) . . ?
C19 C18 C17 119.5(4) . . ?
C18 C19 C20 120.6(4) . . ?
C15 C20 C19 121.1(4) . . ?
#===END
data_nov2900

_database_code_CSD	160793

_audit_creation_date 2000-11-29T14:09:05-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
_audit_conform_dict_name cif_core.dic
_audit_conform_dict_version 2.1
_audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic
_publ_requested_category FM
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic
;
?
;
_chemical_name_common '[TiCl(CLAlMe3)(C7H12N3)2AlMe2]'
_chemical_formula_moiety 'C19 H39 Al2 Cl2 N6 Ti1'
_chemical_formula_structural 'C19 H39 Al2 Cl2 N6 Ti1'
_chemical_formula_sum 'C19 H39 Al2 Cl2 N6 Ti'
_chemical_formula_weight 524.32
_chemical_compound_source 'synthesis as described'
#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M C2/c
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_Int_Tables_number 15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'
_cell_length_a 32.1612(12)
_cell_length_b 8.7247(6)
_cell_length_c 22.3495(11)
_cell_angle_alpha 90
_cell_angle_beta 120.135(3)
_cell_angle_gamma 90
_cell_volume 5423.6(5)
_cell_formula_units_Z 8
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 7006
_cell_measurement_theta_min 3.705
_cell_measurement_theta_max 25.028
_cell_measurement_wavelength 0.71073
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_description plate
_exptl_crystal_colour purple
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.05
_exptl_crystal_density_diffrn 1.284
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2216
_exptl_special_details
;
?
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu 0.595
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min 0.898
_exptl_absorpt_correction_T_max 0.951
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_measurement_device KappaCCD
_diffrn_measurement_method CCD
_diffrn_reflns_number 12618
_diffrn_reflns_av_R_equivalents 0.0603
_diffrn_reflns_av_unetI/netI 0.0735
_diffrn_reflns_limit_h_min -38
_diffrn_reflns_limit_h_max 38
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 3.74
_diffrn_reflns_theta_max 25.04
_diffrn_reflns_theta_full 25.04
_diffrn_measured_fraction_theta_full
0.994
_diffrn_measured_fraction_theta_max
0.994
_reflns_number_total 4783
_reflns_number_gt 3406
_reflns_threshold_expression >2sigma(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_cell_refinement
'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX publication routines (Farrugia, 1999)'
#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_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^)+(0.0341P)^2^+6.7346P] 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_number_reflns 4783
_refine_ls_number_parameters 281
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0792
_refine_ls_R_factor_gt 0.0464
_refine_ls_wR_factor_ref 0.1058
_refine_ls_wR_factor_gt 0.0927
_refine_ls_goodness_of_fit_ref 1.021
_refine_ls_restrained_S_all 1.021
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0
_refine_diff_density_max 0.322
_refine_diff_density_min -0.333
_refine_diff_density_rms 0.067
#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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'
N N 0.0061 0.0033 '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_
_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 0.132189(17) -0.12353(7) 0.03640(3) 0.02266(16) Uani 1 1 d . A .
Cl1 Cl 0.18520(3) -0.32960(11) 0.08992(4) 0.0394(2) Uani 1 1 d . . .
Cl2 Cl 0.07141(3) -0.21404(10) 0.06424(4) 0.0318(2) Uani 1 1 d . . .
Al1 Al 0.12901(3) 0.14929(12) -0.04800(5) 0.0274(2) Uani 1 1 d . A .
Al2 Al 0.08642(3) -0.20828(13) 0.17998(5) 0.0310(3) Uani 1 1 d . . .
N1 N 0.09016(8) -0.1858(3) -0.06635(12) 0.0278(6) Uani 1 1 d . . .
N2 N 0.15730(8) -0.0549(3) -0.03618(12) 0.0261(6) Uani 1 1 d . . .
N3 N 0.13035(10) -0.2337(4) -0.12928(13) 0.0358(7) Uani 1 1 d . . .
N4 N 0.10549(8) 0.1199(3) 0.01682(11) 0.0226(6) Uani 1 1 d . . .
N5 N 0.17517(8) 0.0409(3) 0.10575(11) 0.0261(6) Uani 1 1 d . . .
N6 N 0.14073(9) 0.2658(3) 0.12124(12) 0.0302(6) Uani 1 1 d . . .
C1 C 0.12494(10) -0.1616(4) -0.08070(15) 0.0276(8) Uani 1 1 d . A .
C5 C 0.17130(13) -0.2053(5) -0.13909(19) 0.0523(11) Uani 1 1 d . A .
H5A H 0.1594 -0.1888 -0.1889 0.063 Uiso 1 1 calc R . .
H5B H 0.1922 -0.2972 -0.1244 0.063 Uiso 1 1 calc R . .
C6 C 0.20050(12) -0.0690(5) -0.09918(19) 0.0489(11) Uani 1 1 d . . .
H6A H 0.1844 0.0263 -0.1241 0.059 Uiso 1 1 calc R A .
H6B H 0.2326 -0.0734 -0.095 0.059 Uiso 1 1 calc R . .
C7 C 0.20596(10) -0.0676(5) -0.02766(17) 0.0382(9) Uani 1 1 d . A .
H7A H 0.2217 -0.1632 -0.0026 0.046 Uiso 1 1 calc R . .
H7B H 0.2261 0.0204 -0.0006 0.046 Uiso 1 1 calc R . .
C8 C 0.14154(10) 0.1487(4) 0.08439(14) 0.0243(7) Uani 1 1 d . A .
C9 C 0.05843(10) 0.1865(4) 0.00013(16) 0.0302(8) Uani 1 1 d . A .
H9A H 0.0455 0.1321 0.0262 0.036 Uiso 1 1 calc R . .
H9B H 0.0352 0.1748 -0.0499 0.036 Uiso 1 1 calc R . .
C10 C 0.06530(12) 0.3550(4) 0.01946(17) 0.0363(8) Uani 1 1 d . . .
H10A H 0.0775 0.4093 -0.0075 0.044 Uiso 1 1 calc R A .
H10B H 0.034 0.401 0.008 0.044 Uiso 1 1 calc R . .
C11 C 0.10049(12) 0.3733(4) 0.09588(17) 0.0398(9) Uani 1 1 d . A .
H11A H 0.1132 0.4794 0.1049 0.048 Uiso 1 1 calc R . .
H11B H 0.0834 0.3574 0.1219 0.048 Uiso 1 1 calc R . .
C12 C 0.18105(13) 0.2894(5) 0.19167(16) 0.0431(10) Uani 1 1 d . A .
H12A H 0.1688 0.3309 0.2211 0.052 Uiso 1 1 calc R . .
H12B H 0.2035 0.3655 0.1907 0.052 Uiso 1 1 calc R . .
C13 C 0.20767(13) 0.1415(5) 0.22268(17) 0.0481(10) Uani 1 1 d . . .
H13A H 0.2379 0.1639 0.2661 0.058 Uiso 1 1 calc R A .
H13B H 0.1878 0.0743 0.234 0.058 Uiso 1 1 calc R . .
C14 C 0.21896(11) 0.0599(5) 0.17309(15) 0.0396(9) Uani 1 1 d . A .
H14A H 0.2429 0.1198 0.1674 0.047 Uiso 1 1 calc R . .
H14B H 0.233 -0.0419 0.1921 0.047 Uiso 1 1 calc R . .
C15 C 0.07517(13) 0.1711(5) -0.14249(16) 0.0456(10) Uani 1 1 d . . .
H15A H 0.0609 0.2732 -0.1483 0.068 Uiso 1 1 calc R A .
H15B H 0.0509 0.093 -0.1512 0.068 Uiso 1 1 calc R . .
H15C H 0.0867 0.1579 -0.1753 0.068 Uiso 1 1 calc R . .
C16 C 0.18084(13) 0.3010(5) -0.0134(2) 0.0479(10) Uani 1 1 d . . .
H16A H 0.1673 0.404 -0.0188 0.072 Uiso 1 1 calc R A .
H16B H 0.1976 0.2934 -0.0398 0.072 Uiso 1 1 calc R . .
H16C H 0.2036 0.2814 0.0356 0.072 Uiso 1 1 calc R . .
C17 C 0.04268(11) -0.3710(4) 0.17569(16) 0.0350(8) Uani 1 1 d . . .
H17A H 0.0556 -0.4711 0.1734 0.052 Uiso 1 1 calc R . .
H17B H 0.011 -0.3566 0.1344 0.052 Uiso 1 1 calc R . .
H17C H 0.0396 -0.3663 0.2171 0.052 Uiso 1 1 calc R . .
C18 C 0.06822(14) 0.0049(5) 0.18457(19) 0.0471(10) Uani 1 1 d . . .
H18A H 0.0927 0.0745 0.1863 0.071 Uiso 1 1 calc R . .
H18B H 0.0658 0.0187 0.2262 0.071 Uiso 1 1 calc R . .
H18C H 0.0371 0.0277 0.1435 0.071 Uiso 1 1 calc R . .
C19 C 0.15504(11) -0.2623(5) 0.23935(18) 0.0456(10) Uani 1 1 d . . .
H19A H 0.1751 -0.1775 0.2395 0.068 Uiso 1 1 calc R . .
H19B H 0.1622 -0.3548 0.2213 0.068 Uiso 1 1 calc R . .
H19C H 0.1618 -0.2812 0.2866 0.068 Uiso 1 1 calc R . .
C2 C 0.05054(12) -0.2890(5) -0.11113(16) 0.0394(9) Uani 0.474(9) 1 d P A 1
H2A H 0.0559 -0.3889 -0.0873 0.047 Uiso 0.474(9) 1 calc PR A 1
H2B H 0.0202 -0.2458 -0.1171 0.047 Uiso 0.474(9) 1 calc PR A 1
C3 C 0.0447(3) -0.3155(11) -0.1787(4) 0.049(3) Uani 0.474(9) 1 d P A 1
H3A H 0.0304 -0.2237 -0.208 0.059 Uiso 0.474(9) 1 calc PR A 1
H3B H 0.0226 -0.4029 -0.2011 0.059 Uiso 0.474(9) 1 calc PR A 1
C4 C 0.09598(14) -0.3523(5) -0.17167(19) 0.0499(11) Uani 0.474(9) 1 d P A 1
H4A H 0.1076 -0.4539 -0.1499 0.06 Uiso 0.474(9) 1 calc PR A 1
H4B H 0.0928 -0.3545 -0.2181 0.06 Uiso 0.474(9) 1 calc PR A 1
C2A C 0.05054(12) -0.2890(5) -0.11113(16) 0.0394(9) Uani 0.526(9) 1 d P A 2
H2A1 H 0.0244 -0.2305 -0.1496 0.047 Uiso 0.526(9) 1 calc PR A 2
H2A2 H 0.0374 -0.3386 -0.0843 0.047 Uiso 0.526(9) 1 calc PR A 2
C3A C 0.0702(3) -0.4100(9) -0.1397(4) 0.040(2) Uani 0.526(9) 1 d P A 2
H3A1 H 0.0917 -0.4789 -0.1014 0.049 Uiso 0.526(9) 1 calc PR A 2
H3A2 H 0.0429 -0.4725 -0.1741 0.049 Uiso 0.526(9) 1 calc PR A 2
C4A C 0.09598(14) -0.3523(5) -0.17167(19) 0.0499(11) Uani 0.526(9) 1 d P A 2
H4A1 H 0.0729 -0.3092 -0.2176 0.06 Uiso 0.526(9) 1 calc PR A 2
H4A2 H 0.1134 -0.4376 -0.1787 0.06 Uiso 0.526(9) 1 calc PR A 2
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 0.0215(3) 0.0240(4) 0.0218(3) -0.0026(2) 0.0104(2) 0.0011(2)
Cl1 0.0371(5) 0.0358(6) 0.0451(5) 0.0073(4) 0.0206(4) 0.0146(4)
Cl2 0.0291(4) 0.0368(6) 0.0329(4) 0.0045(4) 0.0181(3) 0.0017(4)
Al1 0.0291(5) 0.0275(6) 0.0278(5) 0.0005(4) 0.0160(4) -0.0008(4)
Al2 0.0315(5) 0.0296(7) 0.0324(5) 0.0027(5) 0.0162(4) 0.0030(4)
N1 0.0267(14) 0.0308(18) 0.0231(13) -0.0044(12) 0.0104(11) -0.0041(12)
N2 0.0227(13) 0.0296(18) 0.0268(13) -0.0036(12) 0.0130(11) -0.0001(12)
N3 0.0486(17) 0.0337(19) 0.0304(14) -0.0051(13) 0.0238(14) 0.0027(14)
N4 0.0201(12) 0.0248(16) 0.0207(12) -0.0016(11) 0.0085(10) 0.0029(11)
N5 0.0207(12) 0.0290(17) 0.0227(12) -0.0030(12) 0.0065(11) 0.0021(12)
N6 0.0384(15) 0.0263(18) 0.0266(13) -0.0030(12) 0.0169(12) -0.0003(13)
C1 0.0262(16) 0.030(2) 0.0243(15) 0.0024(14) 0.0112(14) 0.0057(14)
C5 0.053(2) 0.069(3) 0.047(2) -0.004(2) 0.034(2) 0.011(2)
C6 0.039(2) 0.065(3) 0.058(2) 0.002(2) 0.0353(19) 0.005(2)
C7 0.0267(17) 0.047(3) 0.0451(19) 0.0008(18) 0.0208(16) 0.0031(16)
C8 0.0243(16) 0.026(2) 0.0234(15) 0.0011(14) 0.0124(14) -0.0032(14)
C9 0.0247(16) 0.032(2) 0.0345(17) 0.0042(15) 0.0155(15) 0.0069(14)
C10 0.0393(19) 0.030(2) 0.0426(19) 0.0062(17) 0.0230(17) 0.0106(16)
C11 0.054(2) 0.023(2) 0.047(2) -0.0046(17) 0.0289(18) 0.0076(17)
C12 0.056(2) 0.039(3) 0.0267(17) -0.0101(17) 0.0145(17) -0.0083(19)
C13 0.050(2) 0.045(3) 0.0296(18) -0.0093(18) 0.0050(17) -0.0068(19)
C14 0.0292(18) 0.044(3) 0.0310(17) -0.0057(17) 0.0043(15) -0.0029(16)
C15 0.053(2) 0.051(3) 0.0341(18) 0.0090(18) 0.0220(18) 0.0094(19)
C16 0.050(2) 0.040(3) 0.063(2) -0.006(2) 0.035(2) -0.0136(19)
C17 0.0364(18) 0.034(2) 0.0369(18) 0.0054(16) 0.0203(16) 0.0028(16)
C18 0.061(2) 0.036(3) 0.052(2) 0.0009(19) 0.034(2) 0.0069(19)
C19 0.0382(19) 0.046(3) 0.043(2) -0.0036(19) 0.0131(17) 0.0019(18)
C2 0.0342(18) 0.039(2) 0.0309(17) -0.0067(17) 0.0056(15) -0.0079(16)
C3 0.060(6) 0.046(6) 0.019(4) -0.002(4) 0.004(4) -0.022(5)
C4 0.069(3) 0.038(3) 0.041(2) -0.0135(19) 0.027(2) -0.004(2)
C2A 0.0342(18) 0.039(2) 0.0309(17) -0.0067(17) 0.0056(15) -0.0079(16)
C3A 0.047(4) 0.030(5) 0.038(4) -0.012(4) 0.017(4) -0.006(3)
C4A 0.069(3) 0.038(3) 0.041(2) -0.0135(19) 0.027(2) -0.004(2)
#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#
_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 N5 2.055(3) . ?
Ti N1 2.069(2) . ?
Ti N2 2.227(2) . ?
Ti N4 2.250(3) . ?
Ti Cl1 2.3499(10) . ?
Ti Cl2 2.4603(9) . ?
Ti C1 2.530(3) . ?
Ti C8 2.561(3) . ?
Cl2 Al2 2.3819(12) . ?
Al1 C15 1.955(3) . ?
Al1 N2 1.957(3) . ?
Al1 C16 1.958(4) . ?
Al1 N4 1.959(2) . ?
Al2 C17 1.966(4) . ?
Al2 C18 1.968(4) . ?
Al2 C19 1.978(3) . ?
N1 C1 1.326(4) . ?
N1 C2 1.468(4) . ?
N2 C1 1.379(4) . ?
N2 C7 1.483(4) . ?
N3 C1 1.339(4) . ?
N3 C5 1.461(4) . ?
N3 C4 1.463(5) . ?
N4 C8 1.389(4) . ?
N4 C9 1.483(4) . ?
N5 C8 1.328(4) . ?
N5 C14 1.466(4) . ?
N6 C8 1.320(4) . ?
N6 C11 1.463(4) . ?
N6 C12 1.467(4) . ?
C5 C6 1.500(6) . ?
C6 C7 1.518(5) . ?
C9 C10 1.517(5) . ?
C10 C11 1.511(4) . ?
C12 C13 1.510(5) . ?
C13 C14 1.507(5) . ?
C2 C3 1.443(8) . ?
C3 C4 1.609(10) . ?
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
N5 Ti N1 146.94(11) . . ?
N5 Ti N2 90.51(10) . . ?
N1 Ti N2 62.34(9) . . ?
N5 Ti N4 62.22(9) . . ?
N1 Ti N4 93.39(10) . . ?
N2 Ti N4 81.20(9) . . ?
N5 Ti Cl1 96.26(7) . . ?
N1 Ti Cl1 105.47(8) . . ?
N2 Ti Cl1 98.10(7) . . ?
N4 Ti Cl1 158.39(7) . . ?
N5 Ti Cl2 110.64(7) . . ?
N1 Ti Cl2 92.13(7) . . ?
N2 Ti Cl2 153.56(6) . . ?
N4 Ti Cl2 94.47(6) . . ?
Cl1 Ti Cl2 95.23(4) . . ?
N5 Ti C1 123.35(10) . . ?
N1 Ti C1 31.53(9) . . ?
N2 Ti C1 32.92(10) . . ?
N4 Ti C1 95.45(10) . . ?
Cl1 Ti C1 95.31(8) . . ?
Cl2 Ti C1 123.17(8) . . ?
N5 Ti C8 31.04(9) . . ?
N1 Ti C8 125.62(10) . . ?
N2 Ti C8 92.65(10) . . ?
N4 Ti C8 32.76(8) . . ?
Cl1 Ti C8 126.43(7) . . ?
Cl2 Ti C8 97.64(7) . . ?
C1 Ti C8 119.05(10) . . ?
Al2 Cl2 Ti 120.95(4) . . ?
C15 Al1 N2 109.50(15) . . ?
C15 Al1 C16 118.53(18) . . ?
N2 Al1 C16 108.42(15) . . ?
C15 Al1 N4 110.49(13) . . ?
N2 Al1 N4 96.14(11) . . ?
C16 Al1 N4 111.40(14) . . ?
C17 Al2 C18 117.42(16) . . ?
C17 Al2 C19 113.00(16) . . ?
C18 Al2 C19 116.80(17) . . ?
C17 Al2 Cl2 100.48(11) . . ?
C18 Al2 Cl2 99.97(12) . . ?
C19 Al2 Cl2 105.84(12) . . ?
C1 N1 C2 118.8(3) . . ?
C1 N1 Ti 93.80(18) . . ?
C2 N1 Ti 141.0(2) . . ?
C1 N2 C7 114.1(3) . . ?
C1 N2 Al1 112.72(19) . . ?
C7 N2 Al1 118.4(2) . . ?
C1 N2 Ti 85.72(17) . . ?
C7 N2 Ti 129.17(19) . . ?
Al1 N2 Ti 91.67(10) . . ?
C1 N3 C5 122.4(3) . . ?
C1 N3 C4 119.6(3) . . ?
C5 N3 C4 117.9(3) . . ?
C8 N4 C9 113.1(2) . . ?
C8 N4 Al1 111.02(18) . . ?
C9 N4 Al1 119.13(19) . . ?
C8 N4 Ti 86.05(18) . . ?
C9 N4 Ti 131.3(2) . . ?
Al1 N4 Ti 90.92(10) . . ?
C8 N5 C14 118.6(3) . . ?
C8 N5 Ti 96.05(18) . . ?
C14 N5 Ti 142.1(2) . . ?
C8 N6 C11 123.0(3) . . ?
C8 N6 C12 119.6(3) . . ?
C11 N6 C12 117.3(3) . . ?
N1 C1 N3 126.2(3) . . ?
N1 C1 N2 110.8(3) . . ?
N3 C1 N2 122.9(3) . . ?
N1 C1 Ti 54.67(15) . . ?
N3 C1 Ti 156.7(2) . . ?
N2 C1 Ti 61.36(15) . . ?
N3 C5 C6 112.8(3) . . ?
C5 C6 C7 109.8(3) . . ?
N2 C7 C6 108.0(2) . . ?
N6 C8 N5 126.2(3) . . ?
N6 C8 N4 123.5(3) . . ?
N5 C8 N4 110.3(3) . . ?
N6 C8 Ti 160.7(2) . . ?
N5 C8 Ti 52.91(16) . . ?
N4 C8 Ti 61.19(16) . . ?
N4 C9 C10 108.9(3) . . ?
C11 C10 C9 110.1(3) . . ?
N6 C11 C10 112.6(3) . . ?
N6 C12 C13 111.4(3) . . ?
C14 C13 C12 110.9(3) . . ?
N5 C14 C13 110.3(3) . . ?
C3 C2 N1 115.1(4) . . ?
C2 C3 C4 109.9(5) . . ?
N3 C4 C3 109.1(4) . . ?