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Acta Cryst. (2007). E63, m1414    [ doi:10.1107/S1600536807017497 ]

(N-tert-Butylimido)chlorido[dimethyl(1H-pyrrol-2-ylmethyl)amine-[kappa]2N,N']bis(pyridine-[kappa]N)titanium(IV) toluene solvate

D.-J. Gong, H. Wei and Y.-H. Li

Abstract top

The title compound, [Ti(C4H9N)Cl(C5H5N)2(C7H11N2)]·C7H8, has a mononuclear structure featuring a six-coordinate distorted octahedral titanium(IV) centre. The central TiIV ion is coordinated by two N atoms from a dimethyl(1H-pyrrol-2-ylmethyl)amine molecule, two N atoms from two pyridine molecules, one N atom from a N-tert-butylimido ligand and one Cl atom.

Comment top

Over the last two decades, the chemistry of titanium–imido complexes has received considerable attention (Wigley, 1994). It has been shown that these complexes can be utilized in a wide variety of stoichiometric and sometimes catalytic coupling reactions with unsaturated substrates. A general entry point to new titanium–imido chemistry is gained via the readily prepared synthons [Ti(NR)Cl2(py)3] (R = tBu or Aryl) (Mountford, 1997).

The title compound, (I), was prepared by combining equimolar amounts of Ti(NtBu)Cl2py3 with Lidap [N,N-dimethyl-(1-Li-pyrrol-2-yl)methanamine] in toluene. It possesses a mononuclear structure featuring a six-coordinate octahedral titanium(IV) centre.

Related literature top

For related literature, see: Wigley (1994); Mountford (1997).

Experimental top

To a near-frozen solution of Ti(NtBu)Cl2py3 (Mountford, 1997) (1.234 g, 2.9 mmol) in toluene (10 ml), Lidap [N,N-dimethyl-(1-Li-pyrrol-2-yl)methanamine] (376.1 mg, 2.9 mmol) in toluene (10 ml) was added dropwise. After stirring at room temperature for 12 h, the resulting solution was filtered to remove solids. Volatiles were removed from the solution under reduced pressure to yield the orange crude product, which was washed with toluene and filtered to remove a trace amount of LiCl, then recrystallized from toluene (yield 920 mg, 60%).

Refinement top

All H atoms were positioned geometrically and refined using a riding model (including free rotation about the ethanol C—C bond), with C—H = 0.95–0.99 Å and with Uiso(H) = 1.2 (1.5 for methyl groups) times Ueq(C).

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2005); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), with atom labels and 50% probability displacement ellipsoids.
(N-tert-Butylimido)chlorido[dimethyl(1H-pyrrol-2-ylmethyl)amine- κ2N,N']bis(pyridine-κN)titanium(IV) toluene solvate top
Crystal data top
[Ti(C4H9N)Cl(C5H5N)2(C7H11N2)]·C7H8F(000) = 1120
Mr = 527.98Dx = 1.226 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ynCell parameters from 7469 reflections
a = 10.5646 (14) Åθ = 3.2–25.3°
b = 15.605 (2) ŵ = 0.42 mm−1
c = 17.432 (2) ÅT = 153 K
β = 95.507 (4)°Block, orange-yellow
V = 2860.6 (6) Å30.30 × 0.20 × 0.15 mm
Z = 4
Data collection top
Rigaku Mercury
diffractometer		5227 independent reflections
Radiation source: fine-focus sealed tube3910 reflections with I > 2σ(I)
graphiteRint = 0.088
Detector resolution: 7.31 pixels mm-1θmax = 25.4°, θmin = 3.2°
ω scansh = −12→12
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)		k = −18→18
Tmin = 0.745, Tmax = 0.939l = −20→20
27774 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.073Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.138H-atom parameters constrained
S = 1.14 w = 1/[σ2(Fo2) + (0.0334P)2 + 3.8455P]
where P = (Fo2 + 2Fc2)/3
5227 reflections(Δ/σ)max = 0.002
323 parametersΔρmax = 0.37 e Å−3
0 restraintsΔρmin = −0.35 e Å−3
Crystal data top
[Ti(C4H9N)Cl(C5H5N)2(C7H11N2)]·C7H8V = 2860.6 (6) Å3
Mr = 527.98Z = 4
Monoclinic, P21/nMo Kα radiation
a = 10.5646 (14) ŵ = 0.42 mm−1
b = 15.605 (2) ÅT = 153 K
c = 17.432 (2) Å0.30 × 0.20 × 0.15 mm
β = 95.507 (4)°
Data collection top
Rigaku Mercury
diffractometer		5227 independent reflections
Absorption correction: multi-scan
(REQAB; Jacobson, 1998)		3910 reflections with I > 2σ(I)
Tmin = 0.745, Tmax = 0.939Rint = 0.088
27774 measured reflectionsθmax = 25.4°
Refinement top
R[F2 > 2σ(F2)] = 0.073H-atom parameters constrained
wR(F2) = 0.138Δρmax = 0.37 e Å−3
S = 1.14Δρmin = −0.35 e Å−3
5227 reflectionsAbsolute structure: ?
323 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Special details top

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ti0.28648 (6)0.78065 (4)0.61619 (4)0.02125 (18)
Cl0.20129 (9)0.77167 (6)0.73991 (5)0.0287 (2)
N10.4229 (3)0.77268 (18)0.53870 (16)0.0208 (6)
N20.4963 (3)0.78443 (19)0.69666 (16)0.0229 (7)
N30.1535 (3)0.79291 (19)0.55539 (17)0.0249 (7)
N40.3083 (3)0.92353 (19)0.62425 (17)0.0237 (7)
N50.2788 (3)0.63571 (19)0.60822 (17)0.0235 (7)
C10.4128 (4)0.7420 (2)0.4639 (2)0.0269 (9)
H10.33550.73870.43130.032*
C20.5283 (4)0.7173 (2)0.4432 (2)0.0286 (9)
H20.54590.69470.39480.034*
C30.6175 (4)0.7320 (2)0.5086 (2)0.0272 (9)
H30.70630.72070.51220.033*
C40.5508 (3)0.7656 (2)0.5649 (2)0.0224 (8)
C50.5915 (3)0.8026 (2)0.6417 (2)0.0270 (9)
H5A0.67460.77800.66150.032*
H5B0.60210.86540.63690.032*
C60.5096 (4)0.8476 (3)0.7600 (2)0.0323 (9)
H6A0.59420.84240.78800.048*
H6B0.44460.83690.79530.048*
H6C0.49880.90560.73870.048*
C70.5217 (4)0.6992 (2)0.7319 (2)0.0326 (10)
H7A0.60380.70020.76310.049*
H7B0.52370.65610.69120.049*
H7C0.45430.68500.76460.049*
C80.0369 (3)0.8149 (2)0.5080 (2)0.0290 (9)
C9−0.0585 (4)0.8480 (3)0.5615 (3)0.0391 (11)
H9A−0.07480.80340.59890.059*
H9B−0.13830.86300.53100.059*
H9C−0.02380.89890.58890.059*
C100.0665 (4)0.8847 (3)0.4507 (3)0.0457 (12)
H10A0.09700.93610.47900.069*
H10B−0.01080.89850.41730.069*
H10C0.13230.86410.41920.069*
C11−0.0137 (4)0.7350 (3)0.4650 (2)0.0393 (10)
H11A0.05180.71200.43460.059*
H11B−0.08940.74990.43070.059*
H11C−0.03610.69180.50220.059*
C120.2603 (4)0.9699 (2)0.6796 (2)0.0281 (9)
H120.22420.94050.71990.034*
C130.2613 (4)1.0579 (2)0.6802 (2)0.0304 (9)
H130.22621.08830.72030.037*
C140.3131 (4)1.1015 (2)0.6226 (2)0.0306 (9)
H140.31571.16240.62260.037*
C150.3614 (4)1.0553 (2)0.5648 (2)0.0302 (9)
H150.39691.08370.52370.036*
C160.3574 (3)0.9673 (2)0.5676 (2)0.0270 (9)
H160.39090.93580.52750.032*
C170.3656 (4)0.5853 (2)0.5789 (2)0.0287 (9)
H170.44180.61110.56530.034*
C180.3502 (4)0.4982 (2)0.5674 (2)0.0335 (10)
H180.41550.46490.54810.040*
C190.2380 (4)0.4605 (3)0.5845 (2)0.0382 (10)
H190.22440.40080.57700.046*
C200.1462 (4)0.5112 (3)0.6126 (2)0.0361 (10)
H200.06790.48710.62460.043*
C210.1701 (4)0.5976 (2)0.6231 (2)0.0307 (9)
H210.10580.63200.64210.037*
C220.2942 (4)0.5083 (3)0.2703 (2)0.0376 (10)
C230.2439 (4)0.4756 (3)0.2002 (3)0.0394 (11)
H230.27020.49900.15400.047*
C240.1569 (4)0.4101 (3)0.1958 (3)0.0536 (13)
H240.12270.38940.14690.064*
C250.1191 (5)0.3744 (3)0.2618 (4)0.0651 (16)
H250.05880.32910.25880.078*
C260.1692 (5)0.4047 (4)0.3321 (4)0.0639 (16)
H260.14460.37970.37810.077*
C270.2549 (4)0.4711 (3)0.3363 (3)0.0490 (12)
H270.28790.49210.38540.059*
C280.3885 (5)0.5808 (3)0.2746 (3)0.0656 (15)
H28A0.37210.61740.22910.098*
H28B0.47490.55750.27640.098*
H28C0.37980.61460.32120.098*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti0.0233 (3)0.0179 (3)0.0231 (4)0.0003 (3)0.0051 (3)0.0004 (3)
Cl0.0340 (5)0.0250 (5)0.0285 (5)−0.0003 (4)0.0115 (4)0.0026 (4)
N10.0216 (15)0.0168 (15)0.0245 (16)0.0016 (13)0.0041 (13)0.0002 (12)
N20.0256 (16)0.0201 (16)0.0235 (16)−0.0006 (14)0.0047 (13)−0.0001 (13)
N30.0225 (16)0.0243 (17)0.0282 (17)0.0018 (14)0.0035 (13)0.0005 (13)
N40.0266 (17)0.0210 (16)0.0233 (17)0.0009 (13)0.0023 (14)0.0003 (13)
N50.0257 (17)0.0225 (16)0.0226 (17)0.0028 (14)0.0033 (13)0.0010 (13)
C10.035 (2)0.023 (2)0.023 (2)−0.0019 (17)0.0052 (17)0.0020 (15)
C20.035 (2)0.022 (2)0.030 (2)−0.0048 (18)0.0130 (17)−0.0021 (16)
C30.025 (2)0.023 (2)0.035 (2)0.0018 (17)0.0074 (17)0.0014 (17)
C40.0185 (17)0.0201 (19)0.029 (2)0.0002 (15)0.0052 (15)0.0052 (15)
C50.0227 (19)0.030 (2)0.029 (2)−0.0041 (17)0.0039 (16)−0.0007 (16)
C60.033 (2)0.039 (2)0.025 (2)−0.0010 (19)0.0017 (18)−0.0051 (18)
C70.031 (2)0.033 (2)0.033 (2)0.0028 (18)0.0013 (18)0.0073 (17)
C80.027 (2)0.029 (2)0.031 (2)−0.0002 (17)0.0038 (17)0.0015 (17)
C90.026 (2)0.043 (3)0.048 (3)0.006 (2)0.0004 (19)−0.004 (2)
C100.037 (3)0.051 (3)0.048 (3)−0.002 (2)−0.004 (2)0.018 (2)
C110.035 (2)0.046 (3)0.036 (2)−0.006 (2)−0.0017 (19)−0.010 (2)
C120.036 (2)0.022 (2)0.027 (2)0.0023 (17)0.0084 (17)0.0025 (16)
C130.041 (2)0.0199 (19)0.031 (2)0.0055 (18)0.0044 (18)−0.0031 (17)
C140.034 (2)0.0186 (19)0.038 (2)0.0013 (17)−0.0021 (19)−0.0008 (17)
C150.034 (2)0.022 (2)0.036 (2)−0.0012 (18)0.0088 (18)0.0077 (17)
C160.029 (2)0.025 (2)0.028 (2)0.0031 (17)0.0097 (17)0.0016 (16)
C170.034 (2)0.020 (2)0.033 (2)0.0014 (17)0.0088 (18)0.0026 (16)
C180.041 (2)0.022 (2)0.038 (2)0.0041 (19)0.0082 (19)0.0003 (17)
C190.050 (3)0.021 (2)0.044 (3)−0.003 (2)0.011 (2)−0.0039 (18)
C200.037 (2)0.029 (2)0.043 (3)−0.0065 (19)0.008 (2)−0.0006 (19)
C210.034 (2)0.024 (2)0.035 (2)−0.0006 (18)0.0067 (18)0.0039 (17)
C220.039 (2)0.037 (2)0.037 (3)0.012 (2)0.001 (2)0.0002 (19)
C230.038 (2)0.040 (3)0.041 (3)0.009 (2)0.005 (2)−0.005 (2)
C240.039 (3)0.054 (3)0.065 (4)0.014 (3)−0.005 (3)−0.017 (3)
C250.032 (3)0.049 (3)0.116 (5)0.003 (2)0.014 (3)0.000 (3)
C260.045 (3)0.074 (4)0.077 (4)0.016 (3)0.024 (3)0.030 (3)
C270.043 (3)0.062 (3)0.041 (3)0.016 (3)0.000 (2)0.003 (2)
C280.066 (4)0.060 (4)0.070 (4)−0.011 (3)0.000 (3)−0.008 (3)
Geometric parameters (Å, °) top
Ti—N31.687 (3)C10—H10B0.9800
Ti—N12.071 (3)C10—H10C0.9800
Ti—N42.245 (3)C11—H11A0.9800
Ti—N52.267 (3)C11—H11B0.9800
Ti—Cl2.4195 (11)C11—H11C0.9800
Ti—N22.508 (3)C12—C131.374 (5)
N1—C11.383 (4)C12—H120.9500
N1—C41.389 (4)C13—C141.370 (5)
N2—C61.477 (5)C13—H130.9500
N2—C71.478 (5)C14—C151.377 (5)
N2—C51.482 (4)C14—H140.9500
N3—C81.457 (5)C15—C161.375 (5)
N4—C121.343 (5)C15—H150.9500
N4—C161.345 (4)C16—H160.9500
N5—C211.341 (5)C17—C181.381 (5)
N5—C171.346 (5)C17—H170.9500
C1—C21.361 (5)C18—C191.381 (6)
C1—H10.9500C18—H180.9500
C2—C31.426 (5)C19—C201.377 (6)
C2—H20.9500C19—H190.9500
C3—C41.367 (5)C20—C211.380 (5)
C3—H30.9500C20—H200.9500
C4—C51.484 (5)C21—H210.9500
C5—H5A0.9900C22—C231.383 (6)
C5—H5B0.9900C22—C271.388 (6)
C6—H6A0.9800C22—C281.504 (6)
C6—H6B0.9800C23—C241.372 (6)
C6—H6C0.9800C23—H230.9500
C7—H7A0.9800C24—C251.371 (7)
C7—H7B0.9800C24—H240.9500
C7—H7C0.9800C25—C261.373 (8)
C8—C111.524 (5)C25—H250.9500
C8—C91.528 (5)C26—C271.373 (7)
C8—C101.530 (5)C26—H260.9500
C9—H9A0.9800C27—H270.9500
C9—H9B0.9800C28—H28A0.9800
C9—H9C0.9800C28—H28B0.9800
C10—H10A0.9800C28—H28C0.9800
N3—Ti—N1100.75 (13)C8—C9—H9C109.5
N3—Ti—N490.05 (13)H9A—C9—H9C109.5
N1—Ti—N491.54 (11)H9B—C9—H9C109.5
N3—Ti—N592.98 (13)C8—C10—H10A109.5
N1—Ti—N585.59 (11)C8—C10—H10B109.5
N4—Ti—N5176.17 (11)H10A—C10—H10B109.5
N3—Ti—Cl102.00 (11)C8—C10—H10C109.5
N1—Ti—Cl156.85 (9)H10A—C10—H10C109.5
N4—Ti—Cl92.66 (8)H10B—C10—H10C109.5
N5—Ti—Cl89.01 (8)C8—C11—H11A109.5
N3—Ti—N2170.61 (13)C8—C11—H11B109.5
N1—Ti—N274.53 (10)H11A—C11—H11B109.5
N4—Ti—N282.05 (10)C8—C11—H11C109.5
N5—Ti—N294.72 (10)H11A—C11—H11C109.5
Cl—Ti—N283.52 (7)H11B—C11—H11C109.5
C1—N1—C4105.5 (3)N4—C12—C13122.8 (4)
C1—N1—Ti129.8 (2)N4—C12—H12118.6
C4—N1—Ti120.4 (2)C13—C12—H12118.6
C6—N2—C7106.9 (3)C14—C13—C12119.6 (4)
C6—N2—C5109.5 (3)C14—C13—H13120.2
C7—N2—C5109.5 (3)C12—C13—H13120.2
C6—N2—Ti116.7 (2)C13—C14—C15118.5 (3)
C7—N2—Ti109.0 (2)C13—C14—H14120.7
C5—N2—Ti105.1 (2)C15—C14—H14120.7
C8—N3—Ti172.1 (3)C16—C15—C14118.9 (4)
C12—N4—C16116.9 (3)C16—C15—H15120.6
C12—N4—Ti122.4 (2)C14—C15—H15120.6
C16—N4—Ti120.2 (2)N4—C16—C15123.3 (4)
C21—N5—C17116.2 (3)N4—C16—H16118.4
C21—N5—Ti117.2 (2)C15—C16—H16118.4
C17—N5—Ti125.8 (2)N5—C17—C18123.7 (4)
C2—C1—N1111.0 (3)N5—C17—H17118.1
C2—C1—H1124.5C18—C17—H17118.1
N1—C1—H1124.5C19—C18—C17118.6 (4)
C1—C2—C3106.4 (3)C19—C18—H18120.7
C1—C2—H2126.8C17—C18—H18120.7
C3—C2—H2126.8C20—C19—C18118.7 (4)
C4—C3—C2106.8 (3)C20—C19—H19120.6
C4—C3—H3126.6C18—C19—H19120.6
C2—C3—H3126.6C19—C20—C21118.8 (4)
C3—C4—N1110.3 (3)C19—C20—H20120.6
C3—C4—C5132.3 (3)C21—C20—H20120.6
N1—C4—C5117.0 (3)N5—C21—C20123.9 (4)
N2—C5—C4110.7 (3)N5—C21—H21118.1
N2—C5—H5A109.5C20—C21—H21118.1
C4—C5—H5A109.5C23—C22—C27117.3 (4)
N2—C5—H5B109.5C23—C22—C28121.2 (4)
C4—C5—H5B109.5C27—C22—C28121.4 (4)
H5A—C5—H5B108.1C24—C23—C22121.5 (5)
N2—C6—H6A109.5C24—C23—H23119.2
N2—C6—H6B109.5C22—C23—H23119.2
H6A—C6—H6B109.5C25—C24—C23120.2 (5)
N2—C6—H6C109.5C25—C24—H24119.9
H6A—C6—H6C109.5C23—C24—H24119.9
H6B—C6—H6C109.5C24—C25—C26119.4 (5)
N2—C7—H7A109.5C24—C25—H25120.3
N2—C7—H7B109.5C26—C25—H25120.3
H7A—C7—H7B109.5C25—C26—C27120.2 (5)
N2—C7—H7C109.5C25—C26—H26119.9
H7A—C7—H7C109.5C27—C26—H26119.9
H7B—C7—H7C109.5C26—C27—C22121.3 (5)
N3—C8—C11108.9 (3)C26—C27—H27119.4
N3—C8—C9107.8 (3)C22—C27—H27119.4
C11—C8—C9110.8 (3)C22—C28—H28A109.5
N3—C8—C10108.9 (3)C22—C28—H28B109.5
C11—C8—C10110.2 (3)H28A—C28—H28B109.5
C9—C8—C10110.2 (3)C22—C28—H28C109.5
C8—C9—H9A109.5H28A—C28—H28C109.5
C8—C9—H9B109.5H28B—C28—H28C109.5
H9A—C9—H9B109.5
N3—Ti—N1—C1−29.6 (3)N1—Ti—N5—C1715.3 (3)
N4—Ti—N1—C1−120.0 (3)N4—Ti—N5—C17−26.3 (17)
N5—Ti—N1—C162.6 (3)Cl—Ti—N5—C17−142.1 (3)
Cl—Ti—N1—C1139.6 (3)N2—Ti—N5—C17−58.7 (3)
N2—Ti—N1—C1158.7 (3)C4—N1—C1—C2−0.4 (4)
N3—Ti—N1—C4177.3 (3)Ti—N1—C1—C2−156.6 (3)
N4—Ti—N1—C486.9 (3)N1—C1—C2—C30.6 (4)
N5—Ti—N1—C4−90.5 (3)C1—C2—C3—C4−0.5 (4)
Cl—Ti—N1—C4−13.5 (4)C2—C3—C4—N10.3 (4)
N2—Ti—N1—C45.6 (2)C2—C3—C4—C5−172.2 (4)
N3—Ti—N2—C675.7 (8)C1—N1—C4—C30.1 (4)
N1—Ti—N2—C6136.6 (3)Ti—N1—C4—C3158.9 (2)
N4—Ti—N2—C642.7 (3)C1—N1—C4—C5173.8 (3)
N5—Ti—N2—C6−139.3 (3)Ti—N1—C4—C5−27.3 (4)
Cl—Ti—N2—C6−50.9 (2)C6—N2—C5—C4−157.6 (3)
N3—Ti—N2—C7−163.1 (7)C7—N2—C5—C485.6 (4)
N1—Ti—N2—C7−102.3 (2)Ti—N2—C5—C4−31.5 (3)
N4—Ti—N2—C7163.9 (2)C3—C4—C5—N2−147.3 (4)
N5—Ti—N2—C7−18.2 (2)N1—C4—C5—N240.7 (4)
Cl—Ti—N2—C770.3 (2)Ti—N3—C8—C11−167.5 (18)
N3—Ti—N2—C5−45.8 (8)Ti—N3—C8—C9−47 (2)
N1—Ti—N2—C515.0 (2)Ti—N3—C8—C1072 (2)
N4—Ti—N2—C5−78.8 (2)C16—N4—C12—C13−0.7 (5)
N5—Ti—N2—C599.1 (2)Ti—N4—C12—C13−172.8 (3)
Cl—Ti—N2—C5−172.4 (2)N4—C12—C13—C14−0.1 (6)
N1—Ti—N3—C8−117.7 (19)C12—C13—C14—C150.9 (6)
N4—Ti—N3—C8−26.1 (19)C13—C14—C15—C16−0.9 (6)
N5—Ti—N3—C8156.2 (19)C12—N4—C16—C150.8 (5)
Cl—Ti—N3—C866.6 (19)Ti—N4—C16—C15173.1 (3)
N2—Ti—N3—C8−59 (2)C14—C15—C16—N40.0 (6)
N3—Ti—N4—C1292.7 (3)C21—N5—C17—C18−3.1 (5)
N1—Ti—N4—C12−166.5 (3)Ti—N5—C17—C18−172.6 (3)
N5—Ti—N4—C12−125.0 (15)N5—C17—C18—C192.1 (6)
Cl—Ti—N4—C12−9.3 (3)C17—C18—C19—C20−0.3 (6)
N2—Ti—N4—C12−92.4 (3)C18—C19—C20—C21−0.4 (6)
N3—Ti—N4—C16−79.1 (3)C17—N5—C21—C202.3 (6)
N1—Ti—N4—C1621.6 (3)Ti—N5—C21—C20172.7 (3)
N5—Ti—N4—C1663.1 (17)C19—C20—C21—N5−0.7 (6)
Cl—Ti—N4—C16178.9 (3)C27—C22—C23—C241.1 (6)
N2—Ti—N4—C1695.8 (3)C28—C22—C23—C24−179.3 (4)
N3—Ti—N5—C21−53.5 (3)C22—C23—C24—C25−1.0 (7)
N1—Ti—N5—C21−154.1 (3)C23—C24—C25—C26−0.1 (7)
N4—Ti—N5—C21164.3 (15)C24—C25—C26—C271.0 (7)
Cl—Ti—N5—C2148.5 (3)C25—C26—C27—C22−0.9 (7)
N2—Ti—N5—C21131.9 (3)C23—C22—C27—C26−0.1 (6)
N3—Ti—N5—C17115.9 (3)C28—C22—C27—C26−179.7 (5)
Table 1
Selected geometric parameters (Å, °) top
Ti—N31.687 (3)Ti—N52.267 (3)
Ti—N12.071 (3)Ti—Cl2.4195 (11)
Ti—N42.245 (3)Ti—N22.508 (3)
N3—Ti—N1100.75 (13)N1—Ti—Cl156.85 (9)
N3—Ti—N490.05 (13)N4—Ti—Cl92.66 (8)
N1—Ti—N491.54 (11)N5—Ti—Cl89.01 (8)
N3—Ti—N592.98 (13)N3—Ti—N2170.61 (13)
N1—Ti—N585.59 (11)N1—Ti—N274.53 (10)
N4—Ti—N5176.17 (11)N4—Ti—N282.05 (10)
N3—Ti—Cl102.00 (11)N5—Ti—N294.72 (10)
Acknowledgements top

The authors acknowledge financial support from the `Hundred Talents Programme' of the Chinese Academy of Science (project No. 2005012), the Science Foundation of Qinghai Province (project No. 2006-G-105) and the Science Foundation of Jiangsu Province (project No. BK2005030).

references
References top

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