Iodidobis(η5-penta­methyl­cyclo­penta­dien­yl)titanium(III)

Kessler, M.; Spannenberg, A.; Rosenthal, U.

doi:10.1107/S1600536810040110

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 11| November 2010| Page m1400

https://doi.org/10.1107/S1600536810040110

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Iodidobis(η⁵-pentamethylcyclopentadienyl)titanium(III)

Monty Kessler,^a ^* Anke Spannenberg ^a and Uwe Rosenthal ^a

^aLeibniz-Institut für Katalyse e. V. an der Universität Rostock, Albert-Einstein-Strasse 29a, 18059 Rostock, Germany
^*Correspondence e-mail: monty.kessler@catalysis.de

(Received 4 October 2010; accepted 7 October 2010; online 13 October 2010)

In the title complex molecule, [Ti(C₁₀H₁₅)₂I], the paramagnetic Ti(III) atom is coordinated by two pentamethylcyclopentadienyl (Cp*) ligands and one iodide ligand. The two Cp* ligands are in a staggered orientation. The coordination geometry at the titanium atom can be described as distorted trigonal-planar.

Related literature

For related bis(η⁵-pentamethylcyclopentadienyl)titanium(III) halides, Cp*₂TiX, see: Pattiasina et al. (1987 ) (X = Cl); Herzog et al. (1994 ) (X = F). For the molecular structure of Cp*₂TiF, see: Lukens et al. (1996 ). For bis(η⁵-tetramethylcyclopentadienyl)titanium(III) halides, see: Troyanov et al. (1993 ).

Experimental

Crystal data

[Ti(C₁₀H₁₅)₂I]
M_r = 445.24
Monoclinic, P 2₁ /n
a = 8.5513 (3) Å
b = 14.1353 (5) Å
c = 16.9547 (6) Å
β = 103.158 (3)°
V = 1995.60 (12) Å³
Z = 4
Mo Kα radiation
μ = 1.97 mm⁻¹
T = 150 K
0.60 × 0.27 × 0.20 mm

Data collection

Stoe IPDS II diffractometer
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2005 ) T_min = 0.451, T_max = 0.875
23992 measured reflections
5395 independent reflections
3921 reflections with I > 2σ(I)
R_int = 0.036

Refinement

R[F² > 2σ(F²)] = 0.025
wR(F²) = 0.052
S = 0.86
5395 reflections
209 parameters
H-atom parameters constrained
Δρ_max = 0.65 e Å⁻³
Δρ_min = −0.43 e Å⁻³

Data collection: X-AREA (Stoe & Cie, 2005); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810040110/is2610sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810040110/is2610Isup2.hkl

checkCIF report

Comment top

The title compound, Cp*₂TiI, was first synthesized by Pattiasina et al. (1987) via salt metathesis of Cp*₂TiCl. Using Cp*₂TiF as starting material we obtained Cp*₂TiI in high yields and single crystals by recrystallization from n-pentane at -78 °C. The X-ray crystal structure analysis of Cp*₂TiI confirms its monomeric structure probably due to the steric demand of the pentamethylcyclopentadienyl ligands. The trivalent paramagnetic titanium center is coordinated by one iodide ligand and by two Cp*-ligands in a η⁵-coordination mode. The Cp*-ligands are in a staggered orientation. The coordination geometry at the titanium is distorted trigonal planar (CE1—Ti1—CE2 = 142.4, CE1—Ti1—I1 = 109.2 and CE2—Ti1—I1 = 108.4°; CE1 = centroid of C1—C5 and CE2 = centroid of C11—C15). A similar distortion is observed for the known bis(η⁵-pentamethylcyclopentadienyl)-titanium(III) halides Cp*₂TiF (Herzog et al., 1994) and Cp*₂TiCl (Pattiasina et al., 1987). The Ti1—I1 bond length of 2.7508 (3) Å is close to that in the related complex (η⁵-C₅HMe₄)₂TiI [Ti1—I1 = 2.759 (2) Å] (Troyanov et al., 1993).

Related literature top

For related bis(η⁵-pentamethylcyclopentadienyl)titanium(III) halides, Cp*₂TiX, see: Pattiasina et al. (1987) (X = Cl); Herzog et al. (1994) (X = F). For the molecular structure of Cp*₂TiF, see: Lukens et al. (1996). For bis(η⁵-tetramethylcyclopentadienyl)titanium(III) halides, see: Troyanov et al. (1993).

Experimental top

A mixture of Cp*₂TiF (0.350 g, 1.04 mmol) and LiI (0.223 g, 1.67 mmol) was suspended in 25 ml diethyl ether and stirred at room temperature overnight. The solvent was removed in vacuo and the dark green residue was extracted with n-hexane. The filtrate was concentrated to dryness in vacuo and the solid residue was recrystallized from n-pentane to give dark blue-green needles. Yield: 0.431 g (0.97 mmol, 93%).

Structure description top

For related bis(η⁵-pentamethylcyclopentadienyl)titanium(III) halides, Cp*₂TiX, see: Pattiasina et al. (1987) (X = Cl); Herzog et al. (1994) (X = F). For the molecular structure of Cp*₂TiF, see: Lukens et al. (1996). For bis(η⁵-tetramethylcyclopentadienyl)titanium(III) halides, see: Troyanov et al. (1993).

Computing details top

Data collection: X-AREA (Stoe & Cie, 2005); cell refinement: X-AREA (Stoe & Cie, 2005); data reduction: X-AREA (Stoe & Cie, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. The molecular structure of the title compound showing the atom-labelling scheme. Hydrogen atoms are omitted for clarity. Thermal ellipsoids are drawn at the 30% probability level.

Iodidobis(η⁵-pentamethylcyclopentadienyl)titanium(III) top

Crystal data top

[Ti(C₁₀H₁₅)₂I]	F(000) = 900
M_r = 445.24	D_x = 1.482 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 5078 reflections
a = 8.5513 (3) Å	θ = 1.8–29.6°
b = 14.1353 (5) Å	µ = 1.97 mm⁻¹
c = 16.9547 (6) Å	T = 150 K
β = 103.158 (3)°	Needle, dark blue-green
V = 1995.60 (12) Å³	0.60 × 0.27 × 0.20 mm
Z = 4

Data collection top

Stoe IPDS II diffractometer	5395 independent reflections
Radiation source: fine-focus sealed tube	3921 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.036
ω scans	θ_max = 29.2°, θ_min = 1.9°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2005)	h = −11→11
T_min = 0.451, T_max = 0.875	k = −19→19
23992 measured reflections	l = −22→23

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.052	H-atom parameters constrained
S = 0.86	w = 1/[σ²(F_o²) + (0.0282P)²] where P = (F_o² + 2F_c²)/3
5395 reflections	(Δ/σ)_max = 0.001
209 parameters	Δρ_max = 0.65 e Å⁻³
0 restraints	Δρ_min = −0.43 e Å⁻³

Crystal data top

[Ti(C₁₀H₁₅)₂I]	V = 1995.60 (12) Å³
M_r = 445.24	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 8.5513 (3) Å	µ = 1.97 mm⁻¹
b = 14.1353 (5) Å	T = 150 K
c = 16.9547 (6) Å	0.60 × 0.27 × 0.20 mm
β = 103.158 (3)°

Data collection top

Stoe IPDS II diffractometer	5395 independent reflections
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2005)	3921 reflections with I > 2σ(I)
T_min = 0.451, T_max = 0.875	R_int = 0.036
23992 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.025	0 restraints
wR(F²) = 0.052	H-atom parameters constrained
S = 0.86	Δρ_max = 0.65 e Å⁻³
5395 reflections	Δρ_min = −0.43 e Å⁻³
209 parameters

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

	x	y	z	U_iso*/U_eq
C1	0.1702 (2)	0.69392 (15)	0.10016 (11)	0.0231 (4)
C2	0.1239 (2)	0.78575 (13)	0.07150 (11)	0.0200 (4)
C3	0.2412 (2)	0.82110 (13)	0.03163 (11)	0.0207 (4)
C4	0.3572 (2)	0.74932 (15)	0.03365 (12)	0.0239 (4)
C5	0.3119 (2)	0.67040 (14)	0.07461 (13)	0.0253 (4)
C6	0.0717 (3)	0.62684 (17)	0.13752 (15)	0.0376 (5)
H6A	0.0090	0.6627	0.1691	0.056*
H6B	0.1430	0.5826	0.1732	0.056*
H6C	−0.0012	0.5914	0.0947	0.056*
C7	−0.0419 (2)	0.82456 (16)	0.06611 (14)	0.0310 (5)
H7A	−0.1202	0.7868	0.0276	0.047*
H7B	−0.0464	0.8904	0.0476	0.047*
H7C	−0.0673	0.8218	0.1196	0.047*
C8	0.2339 (3)	0.91097 (16)	−0.01645 (13)	0.0309 (5)
H8A	0.3413	0.9391	−0.0071	0.046*
H8B	0.1601	0.9555	0.0006	0.046*
H8C	0.1954	0.8969	−0.0742	0.046*
C9	0.4955 (3)	0.7556 (2)	−0.00683 (16)	0.0401 (6)
H9A	0.4566	0.7465	−0.0653	0.060*
H9B	0.5745	0.7065	0.0149	0.060*
H9C	0.5460	0.8180	0.0035	0.060*
C10	0.3827 (3)	0.57250 (16)	0.07894 (18)	0.0431 (6)
H10A	0.3171	0.5328	0.0367	0.065*
H10B	0.3848	0.5449	0.1322	0.065*
H10C	0.4924	0.5761	0.0708	0.065*
C11	0.2539 (2)	0.87291 (14)	0.26881 (12)	0.0220 (4)
C12	0.2530 (2)	0.94111 (14)	0.20774 (12)	0.0218 (4)
C13	0.4142 (2)	0.96209 (13)	0.20569 (12)	0.0223 (4)
C14	0.5137 (2)	0.91117 (14)	0.26920 (13)	0.0246 (4)
C15	0.4160 (2)	0.85547 (14)	0.30742 (12)	0.0242 (4)
C16	0.1122 (3)	0.83399 (18)	0.29660 (16)	0.0381 (6)
H16A	0.0946	0.8713	0.3425	0.057*
H16B	0.1330	0.7679	0.3133	0.057*
H16C	0.0164	0.8373	0.2521	0.057*
C17	0.1126 (3)	1.00169 (16)	0.16858 (16)	0.0369 (5)
H17A	0.0125	0.9693	0.1711	0.055*
H17B	0.1151	1.0130	0.1119	0.055*
H17C	0.1185	1.0623	0.1972	0.055*
C18	0.4682 (3)	1.03754 (16)	0.15589 (15)	0.0381 (5)
H18A	0.5041	1.0930	0.1899	0.057*
H18B	0.3788	1.0554	0.1112	0.057*
H18C	0.5572	1.0136	0.1340	0.057*
C19	0.6924 (2)	0.92654 (18)	0.29768 (18)	0.0445 (6)
H19A	0.7412	0.9294	0.2507	0.067*
H19B	0.7397	0.8741	0.3329	0.067*
H19C	0.7122	0.9861	0.3278	0.067*
C20	0.4730 (3)	0.79563 (19)	0.38119 (14)	0.0437 (6)
H20A	0.5827	0.7739	0.3832	0.065*
H20B	0.4020	0.7408	0.3789	0.065*
H20C	0.4716	0.8330	0.4297	0.065*
I1	0.651593 (15)	0.699360 (11)	0.219599 (10)	0.03611 (5)
Ti1	0.37146 (3)	0.80034 (2)	0.169855 (19)	0.01689 (6)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0265 (8)	0.0231 (9)	0.0196 (9)	−0.0047 (8)	0.0047 (7)	−0.0004 (9)
C2	0.0195 (7)	0.0234 (10)	0.0167 (9)	−0.0002 (7)	0.0032 (6)	−0.0020 (7)
C3	0.0237 (8)	0.0228 (10)	0.0146 (8)	−0.0018 (7)	0.0023 (7)	0.0009 (7)
C4	0.0244 (9)	0.0291 (11)	0.0195 (10)	0.0003 (7)	0.0077 (7)	−0.0042 (8)
C5	0.0296 (9)	0.0219 (10)	0.0235 (10)	0.0026 (7)	0.0039 (8)	−0.0041 (8)
C6	0.0409 (12)	0.0350 (13)	0.0372 (14)	−0.0143 (10)	0.0098 (10)	0.0050 (10)
C7	0.0192 (8)	0.0413 (13)	0.0307 (12)	0.0032 (8)	0.0018 (8)	−0.0043 (9)
C8	0.0388 (11)	0.0311 (11)	0.0209 (11)	−0.0015 (9)	0.0031 (8)	0.0079 (9)
C9	0.0353 (11)	0.0577 (16)	0.0329 (13)	0.0027 (11)	0.0195 (10)	−0.0042 (12)
C10	0.0495 (13)	0.0252 (12)	0.0514 (16)	0.0078 (10)	0.0048 (12)	−0.0082 (11)
C11	0.0245 (8)	0.0241 (10)	0.0196 (10)	−0.0020 (7)	0.0096 (7)	−0.0052 (8)
C12	0.0240 (8)	0.0210 (9)	0.0192 (10)	0.0044 (7)	0.0029 (7)	−0.0038 (8)
C13	0.0298 (9)	0.0175 (9)	0.0211 (10)	−0.0025 (7)	0.0086 (8)	−0.0017 (8)
C14	0.0215 (8)	0.0242 (10)	0.0269 (11)	−0.0005 (7)	0.0030 (7)	−0.0053 (8)
C15	0.0324 (10)	0.0217 (10)	0.0169 (10)	0.0020 (8)	0.0022 (8)	0.0003 (8)
C16	0.0411 (12)	0.0407 (13)	0.0405 (14)	−0.0130 (10)	0.0260 (11)	−0.0125 (11)
C17	0.0380 (11)	0.0302 (12)	0.0378 (14)	0.0153 (10)	−0.0013 (10)	−0.0073 (10)
C18	0.0557 (14)	0.0270 (12)	0.0348 (13)	−0.0109 (10)	0.0173 (11)	0.0016 (10)
C19	0.0242 (10)	0.0397 (14)	0.0631 (18)	−0.0047 (9)	−0.0033 (10)	−0.0152 (13)
C20	0.0665 (15)	0.0384 (13)	0.0216 (11)	0.0077 (12)	0.0008 (10)	0.0085 (11)
I1	0.02397 (6)	0.03285 (8)	0.04797 (10)	0.01242 (6)	0.00080 (5)	−0.00121 (8)
Ti1	0.01598 (12)	0.01732 (15)	0.01722 (15)	0.00272 (12)	0.00345 (11)	0.00109 (14)

Geometric parameters (Å, º) top

C1—C2	1.411 (3)	C11—C12	1.414 (3)
C1—C5	1.416 (3)	C11—C16	1.501 (3)
C1—C6	1.501 (3)	C11—Ti1	2.3760 (18)
C1—Ti1	2.3864 (19)	C12—C13	1.417 (3)
C2—C3	1.422 (2)	C12—C17	1.501 (3)
C2—C7	1.504 (2)	C12—Ti1	2.3862 (19)
C2—Ti1	2.3869 (17)	C13—C14	1.409 (3)
C3—C4	1.413 (3)	C13—C18	1.497 (3)
C3—C8	1.503 (3)	C13—Ti1	2.3726 (19)
C3—Ti1	2.3729 (19)	C14—C15	1.409 (3)
C4—C5	1.414 (3)	C14—C19	1.509 (3)
C4—C9	1.500 (3)	C14—Ti1	2.416 (2)
C4—Ti1	2.396 (2)	C15—C20	1.497 (3)
C5—C10	1.506 (3)	C15—Ti1	2.406 (2)
C5—Ti1	2.422 (2)	C16—H16A	0.9800
C6—H6A	0.9800	C16—H16B	0.9800
C6—H6B	0.9800	C16—H16C	0.9800
C6—H6C	0.9800	C17—H17A	0.9800
C7—H7A	0.9800	C17—H17B	0.9800
C7—H7B	0.9800	C17—H17C	0.9800
C7—H7C	0.9800	C18—H18A	0.9800
C8—H8A	0.9800	C18—H18B	0.9800
C8—H8B	0.9800	C18—H18C	0.9800
C8—H8C	0.9800	C19—H19A	0.9800
C9—H9A	0.9800	C19—H19B	0.9800
C9—H9B	0.9800	C19—H19C	0.9800
C9—H9C	0.9800	C20—H20A	0.9800
C10—H10A	0.9800	C20—H20B	0.9800
C10—H10B	0.9800	C20—H20C	0.9800
C10—H10C	0.9800	I1—Ti1	2.7508 (3)
C11—C15	1.413 (3)

C2—C1—C5	107.64 (16)	C11—C15—Ti1	71.66 (11)
C2—C1—C6	125.89 (18)	C20—C15—Ti1	125.22 (15)
C5—C1—C6	125.6 (2)	C11—C16—H16A	109.5
C2—C1—Ti1	72.83 (11)	C11—C16—H16B	109.5
C5—C1—Ti1	74.25 (11)	H16A—C16—H16B	109.5
C6—C1—Ti1	126.88 (14)	C11—C16—H16C	109.5
C1—C2—C3	108.31 (15)	H16A—C16—H16C	109.5
C1—C2—C7	122.90 (17)	H16B—C16—H16C	109.5
C3—C2—C7	126.92 (18)	C12—C17—H17A	109.5
C1—C2—Ti1	72.79 (10)	C12—C17—H17B	109.5
C3—C2—Ti1	72.08 (10)	H17A—C17—H17B	109.5
C7—C2—Ti1	133.24 (13)	C12—C17—H17C	109.5
C4—C3—C2	107.64 (17)	H17A—C17—H17C	109.5
C4—C3—C8	124.22 (18)	H17B—C17—H17C	109.5
C2—C3—C8	127.44 (17)	C13—C18—H18A	109.5
C4—C3—Ti1	73.64 (11)	C13—C18—H18B	109.5
C2—C3—Ti1	73.16 (11)	H18A—C18—H18B	109.5
C8—C3—Ti1	126.33 (13)	C13—C18—H18C	109.5
C3—C4—C5	108.02 (17)	H18A—C18—H18C	109.5
C3—C4—C9	124.64 (19)	H18B—C18—H18C	109.5
C5—C4—C9	127.19 (19)	C14—C19—H19A	109.5
C3—C4—Ti1	71.88 (11)	C14—C19—H19B	109.5
C5—C4—Ti1	73.95 (12)	H19A—C19—H19B	109.5
C9—C4—Ti1	123.42 (14)	C14—C19—H19C	109.5
C4—C5—C1	108.31 (17)	H19A—C19—H19C	109.5
C4—C5—C10	126.7 (2)	H19B—C19—H19C	109.5
C1—C5—C10	124.3 (2)	C15—C20—H20A	109.5
C4—C5—Ti1	71.92 (11)	C15—C20—H20B	109.5
C1—C5—Ti1	71.50 (11)	H20A—C20—H20B	109.5
C10—C5—Ti1	130.03 (16)	C15—C20—H20C	109.5
C1—C6—H6A	109.5	H20A—C20—H20C	109.5
C1—C6—H6B	109.5	H20B—C20—H20C	109.5
H6A—C6—H6B	109.5	C13—Ti1—C3	98.28 (7)
C1—C6—H6C	109.5	C13—Ti1—C11	57.88 (6)
H6A—C6—H6C	109.5	C3—Ti1—C11	117.72 (7)
H6B—C6—H6C	109.5	C13—Ti1—C12	34.66 (6)
C2—C7—H7A	109.5	C3—Ti1—C12	91.73 (7)
C2—C7—H7B	109.5	C11—Ti1—C12	34.53 (7)
H7A—C7—H7B	109.5	C13—Ti1—C1	141.80 (7)
C2—C7—H7C	109.5	C3—Ti1—C1	57.69 (6)
H7A—C7—H7C	109.5	C11—Ti1—C1	104.38 (6)
H7B—C7—H7C	109.5	C12—Ti1—C1	110.89 (7)
C3—C8—H8A	109.5	C13—Ti1—C2	108.81 (7)
C3—C8—H8B	109.5	C3—Ti1—C2	34.76 (6)
H8A—C8—H8B	109.5	C11—Ti1—C2	94.60 (6)
C3—C8—H8C	109.5	C12—Ti1—C2	84.08 (6)
H8A—C8—H8C	109.5	C1—Ti1—C2	34.38 (6)
H8B—C8—H8C	109.5	C13—Ti1—C4	120.53 (7)
C4—C9—H9A	109.5	C3—Ti1—C4	34.48 (7)
C4—C9—H9B	109.5	C11—Ti1—C4	150.89 (7)
H9A—C9—H9B	109.5	C12—Ti1—C4	125.37 (7)
C4—C9—H9C	109.5	C1—Ti1—C4	57.33 (7)
H9A—C9—H9C	109.5	C2—Ti1—C4	57.18 (6)
H9B—C9—H9C	109.5	C13—Ti1—C15	57.21 (7)
C5—C10—H10A	109.5	C3—Ti1—C15	148.49 (7)
C5—C10—H10B	109.5	C11—Ti1—C15	34.37 (6)
H10A—C10—H10B	109.5	C12—Ti1—C15	56.77 (7)
C5—C10—H10C	109.5	C1—Ti1—C15	128.41 (7)
H10A—C10—H10C	109.5	C2—Ti1—C15	128.66 (6)
H10B—C10—H10C	109.5	C4—Ti1—C15	173.78 (7)
C15—C11—C12	107.42 (16)	C13—Ti1—C14	34.20 (7)
C15—C11—C16	124.58 (19)	C3—Ti1—C14	131.07 (7)
C12—C11—C16	127.57 (19)	C11—Ti1—C14	56.95 (6)
C15—C11—Ti1	73.97 (11)	C12—Ti1—C14	56.55 (6)
C12—C11—Ti1	73.13 (11)	C1—Ti1—C14	161.04 (7)
C16—C11—Ti1	124.40 (14)	C2—Ti1—C14	140.24 (6)
C11—C12—C13	108.52 (16)	C4—Ti1—C14	140.74 (7)
C11—C12—C17	125.67 (18)	C15—Ti1—C14	33.98 (7)
C13—C12—C17	123.65 (19)	C13—Ti1—C5	153.93 (7)
C11—C12—Ti1	72.34 (11)	C3—Ti1—C5	56.98 (7)
C13—C12—Ti1	72.15 (11)	C11—Ti1—C5	137.70 (7)
C17—C12—Ti1	134.62 (14)	C12—Ti1—C5	140.73 (7)
C14—C13—C12	107.21 (17)	C1—Ti1—C5	34.24 (6)
C14—C13—C18	125.77 (18)	C2—Ti1—C5	56.64 (6)
C12—C13—C18	126.13 (19)	C4—Ti1—C5	34.13 (7)
C14—C13—Ti1	74.60 (11)	C15—Ti1—C5	148.74 (7)
C12—C13—Ti1	73.20 (11)	C14—Ti1—C5	162.29 (6)
C18—C13—Ti1	126.25 (15)	C13—Ti1—I1	110.43 (5)
C13—C14—C15	108.57 (16)	C3—Ti1—I1	123.17 (5)
C13—C14—C19	124.2 (2)	C11—Ti1—I1	119.10 (5)
C15—C14—C19	126.6 (2)	C12—Ti1—I1	138.03 (5)
C13—C14—Ti1	71.20 (11)	C1—Ti1—I1	107.72 (5)
C15—C14—Ti1	72.60 (11)	C2—Ti1—I1	137.84 (5)
C19—C14—Ti1	128.94 (15)	C4—Ti1—I1	89.38 (5)
C14—C15—C11	108.14 (17)	C15—Ti1—I1	86.35 (5)
C14—C15—C20	125.85 (19)	C14—Ti1—I1	81.82 (5)
C11—C15—C20	125.8 (2)	C5—Ti1—I1	81.21 (5)
C14—C15—Ti1	73.42 (12)

Experimental details

Crystal data
Chemical formula	[Ti(C₁₀H₁₅)₂I]
M_r	445.24
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	150
a, b, c (Å)	8.5513 (3), 14.1353 (5), 16.9547 (6)
β (°)	103.158 (3)
V (Å³)	1995.60 (12)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.97
Crystal size (mm)	0.60 × 0.27 × 0.20

Data collection
Diffractometer	Stoe IPDS II
Absorption correction	Numerical (X-SHAPE and X-RED32; Stoe & Cie, 2005)
T_min, T_max	0.451, 0.875
No. of measured, independent and observed [I > 2σ(I)] reflections	23992, 5395, 3921
R_int	0.036
(sin θ/λ)_max (Å⁻¹)	0.686

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.025, 0.052, 0.86
No. of reflections	5395
No. of parameters	209
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.65, −0.43

Computer programs: X-AREA (Stoe & Cie, 2005), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008).

Acknowledgements

We thank our technical and analytical staff for assistance. This work was supported by the BMBF.

References

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