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The titanium metal center in the title compound, [Ti(C19H27NSi)(C16H14)], is coordinated in a distorted tetrahedral geom­etry by a η5-indenyl ligand, a di­methyl­silyl-bridged N-cyclo­butyl­amido ligand and an s-cis4-1,4-di­phenyl-1,3-buta­diene ligand in a `prone' π-fashion, revealing a formal divalent Ti center.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010101592X/fr1316sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010827010101592X/fr1316Isup2.hkl
Contains datablock I

CCDC reference: 179262

Comment top

Constrained-geometry catalysts are a very important catalyst family which has had a major impact on homogeneous olefin polymerization technologies (Stevens et al., 1991; McKnight & Waymouth, 1998). In this catalyst family, constrained-geometry titanium(II)–diene complexes, in particular, offer structural diversity and unique olefin polymerization activity (Devore et al., 1995). A common procedure used for the preparation of a variety of constrained-geometry titanium–diene complexes is to react the corresponding dichloride precursor with two equivalents of nBuLi in the presence of excess diene. In the course of structure–activity studies of the constrained-geometry catalysts having ancilliary (η5:η1-C5Me4SiMe2NtBu), we found that when replacing tBu of the tBuN group in the ligand with less bulky secondary C atoms, such as cyclobutyl, the diene complex cannot be obtained with the common procedure. Considering the reactivity of the α-H atom of the N-cyclobutyl group, we found that the use of the milder nBuMgBr reagent instead of nBuLi successfully offered a desired titanium(II)–diene complex, viz. Me2Si(η5-2,3,4,6-Me4C9H2)(C4H7N)Ti(s-cis-η4-1, 4-Ph2C4H4), (I), the structure of which is reported here.

The molecular structure of the title compound is depicted in Fig. 1 and selected geometric parameters are given in Table 1. The Ti metal center is coordinated in a distorted tetrahedral geometry by an η5-indenyl ligand, a dimethylsilyl-bridged N-cyclobutylamido ligand and a 1,4-diphenyl-1,3-butadiene ligand in a `prone' π-fashion (Dahlmann et al., 2000; Devore et al., 1995; Erker et al., 1985; Yasuda et al., 1985). A Cp—Ti—N angle (Cp is the centroid of the indenyl five-membered ring) of 110.40 (8)° reflects the openness of the coordination sphere about Ti.

The 1,4-diphenyl-1,3-butadiene ligand adopts an s-cis orientation with the diene being bound to Ti in a π-fashion. The two Ti—C(terminal) diene distances [Ti—C20 = 2.217 (2) Å and Ti—C23 = 2.233 (2) Å] differ from the two Ti—C(internal) diene distances [Ti—C21 = 2.295 (2) Å and Ti—C22 = 2.295 (2) Å] by only 0.070 Å. The very small C—C distance differences [C20—C21 = 1.416 (3) Å, C21—C22 = 1.397 (3) Å and C22—C23 = 1.419 (3) Å] in the diene ligand also support the assignment of a predominantly π-bound diene ligand (Dahlmann et al., 2000; Devore et al., 1995). A C20—C21—C22—C23 torsion angle of -0.6 (4)° reflects the coplanarity of these atoms.

The Ti—N distance of 1.963 (2) Å compares well with those in typical tBuN constrained-geometry TiII complexes (Dahlmann et al., 2000; Devore et al., 1995), but is considerably longer than in typical TiIV amide complexes (Lappert et al., 1980).

Related literature top

For related literature, see: Abboud et al. (1997); Dahlmann et al. (2000); Devore et al. (1995); Erker et al. (1985); Lappert et al. (1980); McKnight & Waymouth (1998); Stevens et al. (1991); Yasuda et al. (1985).

Experimental top

Me2Si(η5-2,3,4,6-Me4C9H2)(C4H7N)Ti(1,4-Ph2C4H4) was prepared from the reaction of Me2Si(η5-2,3,4,6-Me4C9H2)(C4H7N)TiCl2 with two equivalents of nBuMgBr in the presence of one equivalent of trans-1,4-diphenyl-1,3-butadiene in hexanes under inert atomospheric conditions, using a similar procedure to that described previously by Devore et al. (1995). The resulting dark-red solution was stored at 238 K in a glove-box for 5 d, after which time, dark crystals of the title complex had formed. The selected crystal was immersed in Paratone N oil and mounted on a thin glass fiber in a glove-box.

Refinement top

C—H distances of 0.98 and 0.99 Å were used for methyl and secondary H atoms, respectively. A distance of 0.95 Å was used for H atoms on Csp2 atoms. The H-atom displacement parameters were set at 1.2Ueq (1.5Ueq for the methyl H atoms) of the parent C atom. The H atoms on atoms C20—C23, as well as the methyl H atoms on C10 and C11, were obtained from a difference Fourier map and refined without any constraints [C—H = 0.93 (2)–1.02 (3) Å]. Full data collection details are in the relevant _special_details section of the archived CIF and also reported elsewhere (Abboud et al., 1997).

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART and SAINT (Bruker, 1998); data reduction: SHELXTL (Bruker, 1998); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), with 50% probability ellipsoids, showing the atom-numbering scheme.
{N-[Dimethyl(η5-1,2,5,7-tetramethylindenyl)silyl]cyclobutylamido-κN}- (η4-1,4-diphenyl-1,3-butadiene)titanium(II) top
Crystal data top
[Ti(C19H27NSi)(C16H14)]F(000) = 1176
Mr = 551.68Dx = 1.249 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 11.0726 (6) ÅCell parameters from 4542 reflections
b = 20.509 (1) Åθ = 2.0–27.5°
c = 13.9311 (8) ŵ = 0.36 mm1
β = 112.020 (1)°T = 173 K
V = 2932.9 (3) Å3Needle, black
Z = 40.19 × 0.15 × 0.09 mm
Data collection top
Bruker SMART
diffractometer
6740 independent reflections
Radiation source: normal-focus sealed tube4070 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.055
ω scansθmax = 27.5°, θmin = 1.9°
Absorption correction: analytical
integration, based on measured indexed faces (SHELXTL; Sheldrick, 1998)
h = 1413
Tmin = 0.931, Tmax = 0.973k = 2615
20107 measured reflectionsl = 1718
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)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.103H atoms treated by a mixture of independent and constrained refinement
S = 0.96 w = 1/[σ2(Fo2) + (0.0458P)2]
where P = (Fo2 + 2Fc2)/3
6740 reflections(Δ/σ)max = 0.007
383 parametersΔρmax = 0.32 e Å3
0 restraintsΔρmin = 0.31 e Å3
Crystal data top
[Ti(C19H27NSi)(C16H14)]V = 2932.9 (3) Å3
Mr = 551.68Z = 4
Monoclinic, P21/nMo Kα radiation
a = 11.0726 (6) ŵ = 0.36 mm1
b = 20.509 (1) ÅT = 173 K
c = 13.9311 (8) Å0.19 × 0.15 × 0.09 mm
β = 112.020 (1)°
Data collection top
Bruker SMART
diffractometer
6740 independent reflections
Absorption correction: analytical
integration, based on measured indexed faces (SHELXTL; Sheldrick, 1998)
4070 reflections with I > 2σ(I)
Tmin = 0.931, Tmax = 0.973Rint = 0.055
20107 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0440 restraints
wR(F2) = 0.103H atoms treated by a mixture of independent and constrained refinement
S = 0.96Δρmax = 0.32 e Å3
6740 reflectionsΔρmin = 0.31 e Å3
383 parameters
Special details top

Experimental. All syntheses and manipulations of air-sensitive materials were carried out in an inert atmosphere (argon) glove box. Solvents were first saturated with nitrogen and then dried by passage through activated alumina and Q-5TM catalyst prior to use. Deuterated NMR solvents were dried over sodium/potassium alloy and distilled and/or filtered prior to use.

A Bruker SMART PLATFORM with a CCD area detector was used for data collection. The selected crystal was mounted on a thin glass fiber and bathed in a cold nitrogen stream for the duration of this study. A hemisphere of frames, 0.3° in ω, was collected. The first 50 frames were remeasured at the end of data collection to monitor instrument and crystal stability. Three sets of 20 frames were collected covering three perpendicular sectors of space. Reflections from these frames were used to obtain an initial set of cell parameters. 1381 frames, 0.3° in ω, were measured in three separate runs. This provided a range of at least 2.4 to 3.6 redundancy level. The first 50 frames were remeasured at the end of data collections in order to monitor crystal and instrument stability and to enable crystal decay corrections. This procedure is different from using standardreflections as with conventional diffractometers. Thus the CIF items -diffrn-standards-number, -diffrn-standards-interval-time and -diffrn-standards-interval-time are neither produced nor needed. Program SAINT was used to integrate all frames and 8192 reflections were used to refine the cell parameters.

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
Ti0.54291 (4)0.272935 (19)0.63494 (3)0.02444 (11)
Si0.53023 (6)0.19255 (3)0.79841 (5)0.02882 (16)
N10.42767 (17)0.21588 (8)0.67538 (13)0.0254 (4)
C10.6683 (2)0.24417 (11)0.79705 (16)0.0281 (5)
C20.7466 (2)0.22813 (12)0.73696 (17)0.0341 (6)
C30.7827 (2)0.28541 (13)0.70004 (18)0.0365 (6)
C40.7465 (3)0.40900 (13)0.73082 (19)0.0430 (7)
C50.6883 (3)0.44781 (13)0.7797 (2)0.0459 (7)
H5A0.69860.49370.77670.055*
C60.6125 (2)0.42359 (12)0.83547 (18)0.0385 (6)
C70.6001 (2)0.35835 (11)0.84316 (17)0.0304 (5)
H7A0.54810.34180.87850.037*
C80.6640 (2)0.31427 (11)0.79906 (15)0.0271 (5)
C90.7346 (2)0.34012 (12)0.73911 (17)0.0321 (5)
C100.4731 (3)0.21363 (16)0.9048 (2)0.0404 (7)
H10A0.432 (2)0.2551 (12)0.8964 (17)0.032 (7)*
H10B0.416 (3)0.1807 (14)0.911 (2)0.067 (9)*
H10C0.551 (3)0.2130 (13)0.973 (2)0.071 (9)*
C110.5712 (3)0.10433 (14)0.8134 (2)0.0454 (7)
H11A0.566 (3)0.0842 (13)0.748 (2)0.058 (8)*
H11B0.509 (3)0.0803 (13)0.8317 (19)0.051 (8)*
H11C0.651 (3)0.0983 (12)0.867 (2)0.048 (8)*
C120.2939 (2)0.19578 (11)0.62254 (16)0.0278 (5)
H12A0.26140.21390.55070.033*
C130.2535 (2)0.12358 (11)0.61712 (19)0.0398 (6)
H13A0.24260.10210.55070.048*
H13B0.30940.09720.67680.048*
C140.1250 (3)0.14548 (14)0.6249 (2)0.0494 (7)
H14A0.05220.15020.55720.059*
H14B0.09860.11900.67330.059*
C150.1916 (2)0.20993 (13)0.6710 (2)0.0445 (7)
H15A0.22790.21090.74760.053*
H15B0.13750.24900.64220.053*
C160.7869 (3)0.16054 (13)0.7182 (2)0.0490 (7)
H16A0.87450.15120.76860.074*
H16B0.78710.15800.64800.074*
H16C0.72530.12860.72570.074*
C170.8739 (3)0.28722 (15)0.6413 (2)0.0578 (9)
H17A0.96380.29270.69040.087*
H17B0.85020.32380.59250.087*
H17C0.86650.24630.60320.087*
C180.8238 (3)0.43774 (15)0.6716 (2)0.0673 (9)
H18A0.82100.48540.67450.101*
H18B0.78610.42340.59930.101*
H18C0.91440.42300.70270.101*
C190.5455 (3)0.47112 (13)0.8818 (2)0.0532 (8)
H19A0.49770.44700.91710.080*
H19B0.48460.49800.82670.080*
H19C0.61080.49920.93170.080*
C200.5099 (2)0.23085 (12)0.48052 (16)0.0291 (5)
H200.422 (2)0.2268 (10)0.4684 (16)0.028 (6)*
C210.5469 (2)0.29640 (12)0.47512 (17)0.0318 (6)
H210.626 (2)0.3056 (10)0.4642 (17)0.035 (6)*
C220.4970 (2)0.35083 (12)0.50795 (17)0.0325 (6)
H220.548 (2)0.3904 (11)0.5134 (16)0.027 (6)*
C230.3999 (2)0.35019 (12)0.55152 (16)0.0290 (5)
H230.336 (2)0.3140 (10)0.5279 (16)0.029 (6)*
C240.5698 (2)0.17466 (12)0.44952 (16)0.0306 (5)
C250.5279 (3)0.11183 (13)0.45826 (19)0.0434 (7)
H25A0.46010.10580.48360.052*
C260.5828 (3)0.05788 (13)0.4310 (2)0.0512 (7)
H26A0.55300.01550.43860.061*
C270.6804 (3)0.06510 (14)0.3927 (2)0.0495 (7)
H27A0.71840.02800.37430.059*
C280.7218 (3)0.12687 (13)0.3816 (2)0.0480 (7)
H28A0.78840.13260.35490.058*
C290.6668 (3)0.18069 (13)0.40919 (19)0.0407 (6)
H29A0.69620.22300.40040.049*
C300.3498 (2)0.40971 (11)0.58318 (16)0.0304 (5)
C310.2370 (3)0.40653 (13)0.60537 (19)0.0419 (6)
H31A0.19630.36550.60300.050*
C320.1830 (3)0.46159 (15)0.6307 (2)0.0502 (7)
H32A0.10510.45810.64400.060*
C330.2417 (3)0.52136 (13)0.6367 (2)0.0480 (7)
H33A0.20470.55920.65390.058*
C340.3542 (3)0.52577 (13)0.61760 (19)0.0449 (7)
H34A0.39580.56680.62270.054*
C350.4078 (2)0.47088 (12)0.59091 (18)0.0376 (6)
H35A0.48560.47500.57760.045*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti0.0222 (2)0.0287 (2)0.0222 (2)0.00113 (18)0.00805 (15)0.00125 (17)
Si0.0308 (4)0.0266 (4)0.0263 (3)0.0003 (3)0.0075 (3)0.0019 (3)
N10.0239 (10)0.0261 (11)0.0252 (9)0.0000 (8)0.0081 (8)0.0006 (7)
C10.0245 (13)0.0317 (14)0.0231 (11)0.0020 (10)0.0031 (9)0.0011 (9)
C20.0234 (12)0.0441 (16)0.0291 (12)0.0040 (11)0.0033 (10)0.0049 (11)
C30.0213 (13)0.0543 (18)0.0331 (13)0.0021 (11)0.0091 (10)0.0061 (11)
C40.0432 (16)0.0444 (17)0.0371 (14)0.0204 (13)0.0100 (12)0.0015 (12)
C50.0526 (18)0.0266 (15)0.0467 (16)0.0118 (12)0.0049 (14)0.0013 (12)
C60.0416 (16)0.0342 (16)0.0307 (13)0.0027 (12)0.0032 (11)0.0065 (11)
C70.0320 (14)0.0288 (14)0.0281 (12)0.0008 (10)0.0086 (10)0.0012 (10)
C80.0227 (12)0.0326 (14)0.0211 (11)0.0025 (10)0.0026 (9)0.0043 (9)
C90.0225 (13)0.0403 (15)0.0290 (12)0.0080 (10)0.0047 (10)0.0028 (10)
C100.0462 (17)0.046 (2)0.0306 (14)0.0092 (14)0.0157 (13)0.0013 (12)
C110.0436 (19)0.0329 (17)0.0489 (18)0.0027 (13)0.0049 (15)0.0076 (13)
C120.0255 (13)0.0321 (13)0.0243 (11)0.0031 (10)0.0076 (9)0.0014 (9)
C130.0426 (16)0.0318 (15)0.0367 (14)0.0080 (11)0.0053 (12)0.0051 (11)
C140.0367 (16)0.067 (2)0.0430 (15)0.0186 (14)0.0135 (13)0.0071 (14)
C150.0309 (15)0.066 (2)0.0389 (14)0.0062 (12)0.0154 (12)0.0090 (12)
C160.0401 (17)0.0530 (19)0.0492 (16)0.0161 (13)0.0113 (13)0.0087 (13)
C170.0306 (16)0.098 (3)0.0492 (17)0.0104 (15)0.0204 (13)0.0154 (16)
C180.072 (2)0.068 (2)0.066 (2)0.0346 (18)0.0306 (18)0.0016 (16)
C190.069 (2)0.0363 (17)0.0449 (16)0.0139 (14)0.0106 (15)0.0085 (12)
C200.0258 (13)0.0366 (15)0.0245 (11)0.0007 (11)0.0091 (10)0.0021 (10)
C210.0327 (14)0.0399 (16)0.0249 (12)0.0006 (11)0.0133 (10)0.0006 (10)
C220.0357 (15)0.0334 (15)0.0284 (12)0.0022 (11)0.0119 (11)0.0014 (10)
C230.0319 (14)0.0290 (14)0.0257 (12)0.0019 (11)0.0104 (10)0.0015 (10)
C240.0320 (14)0.0358 (15)0.0234 (12)0.0012 (10)0.0098 (10)0.0020 (10)
C250.0542 (18)0.0420 (17)0.0439 (15)0.0041 (13)0.0298 (14)0.0037 (12)
C260.070 (2)0.0350 (17)0.0571 (18)0.0043 (14)0.0339 (16)0.0039 (13)
C270.062 (2)0.0411 (18)0.0512 (17)0.0118 (14)0.0274 (15)0.0065 (13)
C280.0477 (18)0.0471 (19)0.0601 (18)0.0005 (13)0.0330 (15)0.0097 (14)
C290.0446 (16)0.0389 (16)0.0456 (15)0.0008 (12)0.0249 (13)0.0059 (12)
C300.0341 (14)0.0323 (14)0.0244 (12)0.0025 (10)0.0104 (10)0.0017 (10)
C310.0436 (17)0.0428 (17)0.0445 (15)0.0053 (12)0.0224 (13)0.0078 (12)
C320.0469 (18)0.059 (2)0.0554 (18)0.0055 (14)0.0310 (15)0.0065 (14)
C330.064 (2)0.0417 (18)0.0450 (16)0.0174 (14)0.0284 (15)0.0018 (13)
C340.066 (2)0.0306 (16)0.0447 (16)0.0051 (13)0.0288 (15)0.0059 (12)
C350.0443 (16)0.0353 (16)0.0386 (14)0.0053 (12)0.0217 (12)0.0059 (11)
Geometric parameters (Å, º) top
Ti—N11.963 (2)C14—H14B0.9900
Ti—C202.217 (2)C15—H15A0.9900
Ti—C232.233 (2)C15—H15B0.9900
Ti—C12.242 (2)C16—H16A0.9800
Ti—C212.295 (2)C16—H16B0.9800
Ti—C222.295 (2)C16—H16C0.9800
Ti—C82.334 (2)C17—H17A0.9800
Ti—C22.355 (2)C17—H17B0.9800
Ti—C32.476 (2)C17—H17C0.9800
Ti—C92.490 (2)C18—H18A0.9800
Ti—Si2.8572 (7)C18—H18B0.9800
Si—N11.7311 (18)C18—H18C0.9800
Si—C111.858 (3)C19—H19A0.9800
Si—C11.865 (2)C19—H19B0.9800
Si—C101.867 (3)C19—H19C0.9800
N1—C121.445 (3)C20—C211.416 (3)
C1—C81.439 (3)C20—C241.473 (3)
C1—C21.451 (3)C20—H200.93 (2)
C2—C31.399 (3)C21—C221.397 (3)
C2—C161.509 (3)C21—H210.96 (2)
C3—C91.434 (3)C22—C231.419 (3)
C3—C171.520 (3)C22—H220.98 (2)
C4—C51.356 (4)C23—C301.475 (3)
C4—C91.428 (3)C23—H230.99 (2)
C4—C181.514 (4)C24—C251.390 (3)
C5—C61.430 (4)C24—C291.393 (3)
C5—H5A0.9500C25—C261.382 (3)
C6—C71.353 (3)C25—H25A0.9500
C6—C191.508 (3)C26—C271.381 (4)
C7—C81.422 (3)C26—H26A0.9500
C7—H7A0.9500C27—C281.376 (4)
C8—C91.441 (3)C27—H27A0.9500
C10—H10A0.95 (2)C28—C291.383 (3)
C10—H10B0.95 (3)C28—H28A0.9500
C10—H10C1.02 (3)C29—H29A0.9500
C11—H11A0.98 (3)C30—C311.396 (3)
C11—H11B0.96 (3)C30—C351.395 (3)
C11—H11C0.92 (3)C31—C321.384 (3)
C12—C131.540 (3)C31—H31A0.9500
C12—C151.548 (3)C32—C331.375 (4)
C12—H12A1.0000C32—H32A0.9500
C13—C141.534 (4)C33—C341.370 (4)
C13—H13A0.9900C33—H33A0.9500
C13—H13B0.9900C34—C351.387 (3)
C14—C151.532 (4)C34—H34A0.9500
C14—H14A0.9900C35—H35A0.9500
Cp—Ti—N1110.40 (8)H10B—C10—H10C106 (2)
N1—Ti—C2099.09 (8)Si—C11—H11A112.4 (16)
N1—Ti—C2399.33 (8)Si—C11—H11B111.1 (16)
C20—Ti—C2386.82 (8)H11A—C11—H11B104 (2)
N1—Ti—C177.16 (8)Si—C11—H11C109.9 (15)
C20—Ti—C1133.59 (9)H11A—C11—H11C113 (2)
C23—Ti—C1139.59 (8)H11B—C11—H11C107 (2)
N1—Ti—C21130.89 (8)N1—C12—C13121.49 (19)
C20—Ti—C2136.52 (8)N1—C12—C15120.16 (18)
C23—Ti—C2167.30 (8)C13—C12—C1587.44 (18)
C1—Ti—C21143.40 (9)N1—C12—H12A108.6
N1—Ti—C22131.01 (8)C13—C12—H12A108.6
C20—Ti—C2267.34 (9)C15—C12—H12A108.6
C23—Ti—C2236.48 (8)C14—C13—C1288.56 (18)
C1—Ti—C22146.56 (9)C14—C13—H13A113.9
C21—Ti—C2235.44 (8)C12—C13—H13A113.9
N1—Ti—C897.59 (7)C14—C13—H13B113.9
C20—Ti—C8156.50 (8)C12—C13—H13B113.9
C23—Ti—C8106.67 (8)H13A—C13—H13B111.1
C1—Ti—C836.60 (8)C15—C14—C1388.21 (19)
C21—Ti—C8131.41 (8)C15—C14—H14A113.9
C22—Ti—C8112.47 (8)C13—C14—H14A113.9
N1—Ti—C299.94 (8)C15—C14—H14B113.9
C20—Ti—C2101.88 (8)C13—C14—H14B113.9
C23—Ti—C2157.27 (9)H14A—C14—H14B111.2
C1—Ti—C236.69 (8)C14—C15—C1288.37 (18)
C21—Ti—C2107.75 (9)C14—C15—H15A113.9
C22—Ti—C2128.47 (9)C12—C15—H15A113.9
C8—Ti—C258.80 (8)C14—C15—H15B113.9
N1—Ti—C3132.80 (8)C12—C15—H15B113.9
C20—Ti—C399.18 (8)H15A—C15—H15B111.1
C23—Ti—C3124.80 (9)C2—C16—H16A109.5
C1—Ti—C358.95 (8)C2—C16—H16B109.5
C21—Ti—C385.73 (8)H16A—C16—H16B109.5
C22—Ti—C396.18 (9)C2—C16—H16C109.5
C8—Ti—C357.33 (8)H16A—C16—H16C109.5
C2—Ti—C333.56 (8)H16B—C16—H16C109.5
N1—Ti—C9131.79 (7)C3—C17—H17A109.5
C20—Ti—C9125.12 (8)C3—C17—H17B109.5
C23—Ti—C9101.16 (9)H17A—C17—H17B109.5
C1—Ti—C959.19 (8)C3—C17—H17C109.5
C21—Ti—C997.30 (8)H17A—C17—H17C109.5
C22—Ti—C987.60 (8)H17B—C17—H17C109.5
C8—Ti—C934.58 (7)C4—C18—H18A109.5
C2—Ti—C956.64 (9)C4—C18—H18B109.5
C3—Ti—C933.57 (8)H18A—C18—H18B109.5
N1—Ti—Si36.48 (5)C4—C18—H18C109.5
C20—Ti—Si120.61 (6)H18A—C18—H18C109.5
C23—Ti—Si125.95 (6)H18B—C18—H18C109.5
C1—Ti—Si40.72 (6)C6—C19—H19A109.5
C21—Ti—Si156.78 (7)C6—C19—H19B109.5
C22—Ti—Si162.42 (6)H19A—C19—H19B109.5
C8—Ti—Si67.09 (6)C6—C19—H19C109.5
C2—Ti—Si67.41 (6)H19A—C19—H19C109.5
C3—Ti—Si97.70 (6)H19B—C19—H19C109.5
C9—Ti—Si98.08 (6)C21—C20—C24123.8 (2)
N1—Si—C11114.99 (12)C21—C20—Ti74.71 (13)
N1—Si—C193.96 (9)C24—C20—Ti131.35 (16)
C11—Si—C1112.79 (13)C21—C20—H20112.4 (13)
N1—Si—C10115.47 (12)C24—C20—H20115.7 (13)
C11—Si—C10106.09 (15)Ti—C20—H2089.5 (13)
C1—Si—C10113.56 (12)C22—C21—C20125.7 (2)
N1—Si—Ti42.39 (6)C22—C21—Ti72.29 (13)
C11—Si—Ti124.66 (11)C20—C21—Ti68.77 (12)
C1—Si—Ti51.62 (6)C22—C21—H21113.0 (13)
C10—Si—Ti129.16 (10)C20—C21—H21119.6 (13)
C12—N1—Si126.30 (14)Ti—C21—H21123.0 (14)
C12—N1—Ti132.56 (14)C21—C22—C23126.1 (2)
Si—N1—Ti101.14 (9)C21—C22—Ti72.27 (14)
C8—C1—C2105.59 (19)C23—C22—Ti69.40 (13)
C8—C1—Si122.26 (16)C21—C22—H22113.6 (13)
C2—C1—Si123.12 (17)C23—C22—H22119.0 (12)
C8—C1—Ti75.18 (12)Ti—C22—H22124.3 (12)
C2—C1—Ti75.91 (12)C22—C23—C30123.4 (2)
Si—C1—Ti87.66 (9)C22—C23—Ti74.12 (14)
C3—C2—C1109.7 (2)C30—C23—Ti134.78 (15)
C3—C2—C16124.3 (2)C22—C23—H23115.0 (12)
C1—C2—C16126.0 (2)C30—C23—H23114.8 (13)
C3—C2—Ti77.98 (14)Ti—C23—H2385.3 (13)
C1—C2—Ti67.40 (12)C25—C24—C29116.8 (2)
C16—C2—Ti122.17 (16)C25—C24—C20119.9 (2)
C2—C3—C9108.6 (2)C29—C24—C20123.3 (2)
C2—C3—C17123.9 (2)C26—C25—C24121.5 (2)
C9—C3—C17127.0 (2)C26—C25—H25A119.2
C2—C3—Ti68.46 (13)C24—C25—H25A119.2
C9—C3—Ti73.74 (13)C27—C26—C25120.6 (3)
C17—C3—Ti130.00 (17)C27—C26—H26A119.7
C5—C4—C9117.7 (2)C25—C26—H26A119.7
C5—C4—C18121.1 (3)C28—C27—C26119.0 (2)
C9—C4—C18121.2 (3)C28—C27—H27A120.5
C4—C5—C6123.7 (2)C26—C27—H27A120.5
C4—C5—H5A118.2C27—C28—C29120.3 (2)
C6—C5—H5A118.2C27—C28—H28A119.9
C7—C6—C5118.9 (2)C29—C28—H28A119.9
C7—C6—C19121.6 (2)C28—C29—C24121.9 (2)
C5—C6—C19119.4 (2)C28—C29—H29A119.1
C6—C7—C8120.8 (2)C24—C29—H29A119.1
C6—C7—H7A119.6C31—C30—C35116.7 (2)
C8—C7—H7A119.6C31—C30—C23119.7 (2)
C7—C8—C1132.0 (2)C35—C30—C23123.6 (2)
C7—C8—C9118.8 (2)C32—C31—C30121.8 (2)
C1—C8—C9109.10 (19)C32—C31—H31A119.1
C7—C8—Ti117.26 (15)C30—C31—H31A119.1
C1—C8—Ti68.22 (11)C33—C32—C31120.2 (3)
C9—C8—Ti78.65 (12)C33—C32—H32A119.9
C4—C9—C3133.2 (2)C31—C32—H32A119.9
C4—C9—C8119.8 (2)C34—C33—C32119.4 (2)
C3—C9—C8106.9 (2)C34—C33—H33A120.3
C4—C9—Ti125.78 (16)C32—C33—H33A120.3
C3—C9—Ti72.69 (13)C33—C34—C35120.7 (3)
C8—C9—Ti66.77 (12)C33—C34—H34A119.7
Si—C10—H10A113.3 (13)C35—C34—H34A119.7
Si—C10—H10B110.0 (16)C34—C35—C30121.3 (2)
H10A—C10—H10B110 (2)C34—C35—H35A119.4
Si—C10—H10C108.3 (16)C30—C35—H35A119.4
H10A—C10—H10C109 (2)
C20—Ti—Si—N160.56 (11)C23—Ti—C8—C731.23 (19)
C23—Ti—Si—N149.90 (11)C1—Ti—C8—C7127.2 (2)
C1—Ti—Si—N1176.71 (12)C21—Ti—C8—C7105.39 (18)
C21—Ti—Si—N168.89 (19)C22—Ti—C8—C769.56 (19)
C22—Ti—Si—N152.1 (2)C2—Ti—C8—C7168.0 (2)
C8—Ti—Si—N1144.38 (10)C3—Ti—C8—C7152.3 (2)
C2—Ti—Si—N1151.30 (11)C9—Ti—C8—C7116.7 (2)
C3—Ti—Si—N1166.05 (10)Si—Ti—C8—C791.37 (17)
C9—Ti—Si—N1160.05 (10)N1—Ti—C8—C156.25 (13)
N1—Ti—Si—C1190.24 (15)C20—Ti—C8—C178.7 (2)
C20—Ti—Si—C1129.69 (15)C23—Ti—C8—C1158.41 (13)
C23—Ti—Si—C11140.14 (15)C21—Ti—C8—C1127.43 (14)
C1—Ti—Si—C1193.05 (15)C22—Ti—C8—C1163.26 (13)
C21—Ti—Si—C1121.4 (2)C2—Ti—C8—C140.81 (13)
C22—Ti—Si—C11142.3 (2)C3—Ti—C8—C180.54 (14)
C8—Ti—Si—C11125.37 (14)C9—Ti—C8—C1116.08 (19)
C2—Ti—Si—C1161.05 (14)Si—Ti—C8—C135.81 (11)
C3—Ti—Si—C1175.81 (14)N1—Ti—C8—C9172.34 (13)
C9—Ti—Si—C11109.71 (14)C20—Ti—C8—C937.4 (3)
N1—Ti—Si—C1176.71 (12)C23—Ti—C8—C985.51 (15)
C20—Ti—Si—C1122.73 (11)C1—Ti—C8—C9116.08 (19)
C23—Ti—Si—C1126.82 (12)C21—Ti—C8—C911.35 (18)
C21—Ti—Si—C1114.40 (19)C22—Ti—C8—C947.17 (16)
C22—Ti—Si—C1124.6 (2)C2—Ti—C8—C975.28 (15)
C8—Ti—Si—C132.33 (10)C3—Ti—C8—C935.54 (13)
C2—Ti—Si—C131.99 (11)Si—Ti—C8—C9151.89 (14)
C3—Ti—Si—C117.24 (11)C5—C4—C9—C3179.2 (3)
C9—Ti—Si—C116.66 (11)C18—C4—C9—C30.6 (4)
N1—Ti—Si—C1086.00 (15)C5—C4—C9—C80.8 (3)
C20—Ti—Si—C10146.56 (14)C18—C4—C9—C8177.8 (2)
C23—Ti—Si—C1036.11 (15)C5—C4—C9—Ti80.7 (3)
C1—Ti—Si—C1090.71 (16)C18—C4—C9—Ti100.6 (3)
C21—Ti—Si—C10154.9 (2)C2—C3—C9—C4176.9 (2)
C22—Ti—Si—C1033.9 (3)C17—C3—C9—C45.0 (4)
C8—Ti—Si—C1058.38 (14)Ti—C3—C9—C4123.2 (3)
C2—Ti—Si—C10122.70 (14)C2—C3—C9—C81.7 (3)
C3—Ti—Si—C10107.95 (14)C17—C3—C9—C8173.6 (2)
C9—Ti—Si—C1074.05 (14)Ti—C3—C9—C858.21 (15)
C11—Si—N1—C1264.9 (2)C2—C3—C9—Ti59.88 (16)
C1—Si—N1—C12177.70 (18)C17—C3—C9—Ti128.2 (2)
C10—Si—N1—C1259.2 (2)C7—C8—C9—C44.2 (3)
Ti—Si—N1—C12179.7 (2)C1—C8—C9—C4178.9 (2)
C11—Si—N1—Ti114.85 (13)Ti—C8—C9—C4119.2 (2)
C1—Si—N1—Ti2.58 (10)C7—C8—C9—C3177.04 (19)
C10—Si—N1—Ti121.05 (12)C1—C8—C9—C30.1 (2)
C20—Ti—N1—C1249.1 (2)Ti—C8—C9—C362.03 (16)
C23—Ti—N1—C1239.2 (2)C7—C8—C9—Ti115.01 (19)
C1—Ti—N1—C12178.1 (2)C1—C8—C9—Ti61.96 (14)
C21—Ti—N1—C1228.8 (2)N1—Ti—C9—C4121.2 (2)
C22—Ti—N1—C1218.7 (2)C20—Ti—C9—C486.3 (2)
C8—Ti—N1—C12147.55 (19)C23—Ti—C9—C47.7 (2)
C2—Ti—N1—C12152.93 (19)C1—Ti—C9—C4149.5 (2)
C3—Ti—N1—C12160.68 (17)C21—Ti—C9—C460.5 (2)
C9—Ti—N1—C12153.38 (17)C22—Ti—C9—C426.3 (2)
Si—Ti—N1—C12179.7 (2)C8—Ti—C9—C4110.9 (3)
C20—Ti—N1—Si130.62 (9)C2—Ti—C9—C4167.0 (2)
C23—Ti—N1—Si141.14 (9)C3—Ti—C9—C4131.3 (3)
C1—Ti—N1—Si2.20 (8)Si—Ti—C9—C4136.94 (19)
C21—Ti—N1—Si150.89 (9)N1—Ti—C9—C3107.54 (15)
C22—Ti—N1—Si161.58 (9)C20—Ti—C9—C345.01 (17)
C8—Ti—N1—Si32.76 (9)C23—Ti—C9—C3139.01 (14)
C2—Ti—N1—Si26.76 (10)C1—Ti—C9—C379.19 (15)
C3—Ti—N1—Si19.00 (14)C21—Ti—C9—C370.80 (15)
C9—Ti—N1—Si26.93 (13)C22—Ti—C9—C3104.96 (14)
N1—Si—C1—C868.60 (18)C8—Ti—C9—C3117.8 (2)
C11—Si—C1—C8172.16 (18)C2—Ti—C9—C335.68 (13)
C10—Si—C1—C851.4 (2)Si—Ti—C9—C391.76 (13)
Ti—Si—C1—C870.82 (16)N1—Ti—C9—C810.21 (18)
N1—Si—C1—C273.71 (19)C20—Ti—C9—C8162.77 (13)
C11—Si—C1—C245.5 (2)C23—Ti—C9—C8103.24 (14)
C10—Si—C1—C2166.26 (19)C1—Ti—C9—C838.57 (13)
Ti—Si—C1—C271.49 (17)C21—Ti—C9—C8171.44 (14)
N1—Si—C1—Ti2.22 (8)C22—Ti—C9—C8137.29 (14)
C11—Si—C1—Ti117.01 (12)C2—Ti—C9—C882.08 (15)
C10—Si—C1—Ti122.25 (12)C3—Ti—C9—C8117.8 (2)
N1—Ti—C1—C8122.29 (13)Si—Ti—C9—C825.99 (13)
C20—Ti—C1—C8147.33 (13)Si—N1—C12—C1348.5 (3)
C23—Ti—C1—C832.94 (19)Ti—N1—C12—C13131.17 (19)
C21—Ti—C1—C892.72 (17)Si—N1—C12—C1558.7 (3)
C22—Ti—C1—C828.9 (2)Ti—N1—C12—C15121.6 (2)
C2—Ti—C1—C8110.67 (18)N1—C12—C13—C14144.5 (2)
C3—Ti—C1—C875.75 (13)C15—C12—C13—C1420.30 (18)
C9—Ti—C1—C836.41 (12)C12—C13—C14—C1520.5 (2)
Si—Ti—C1—C8124.29 (15)C13—C14—C15—C1220.40 (18)
N1—Ti—C1—C2127.04 (15)N1—C12—C15—C14145.7 (2)
C20—Ti—C1—C236.66 (19)C13—C12—C15—C1420.34 (18)
C23—Ti—C1—C2143.61 (15)N1—Ti—C20—C21153.89 (14)
C21—Ti—C1—C217.9 (2)C23—Ti—C20—C2154.94 (15)
C22—Ti—C1—C281.8 (2)C1—Ti—C20—C21125.24 (15)
C8—Ti—C1—C2110.67 (18)C22—Ti—C20—C2123.09 (14)
C3—Ti—C1—C234.92 (13)C8—Ti—C20—C2171.4 (3)
C9—Ti—C1—C274.26 (14)C2—Ti—C20—C21103.86 (15)
Si—Ti—C1—C2125.03 (17)C3—Ti—C20—C2169.82 (15)
N1—Ti—C1—Si2.00 (8)C9—Ti—C20—C2146.48 (17)
C20—Ti—C1—Si88.37 (13)Si—Ti—C20—C21174.49 (12)
C23—Ti—C1—Si91.36 (14)N1—Ti—C20—C2484.3 (2)
C21—Ti—C1—Si142.98 (12)C23—Ti—C20—C24176.8 (2)
C22—Ti—C1—Si153.18 (12)C1—Ti—C20—C243.4 (3)
C8—Ti—C1—Si124.29 (15)C21—Ti—C20—C24121.9 (3)
C2—Ti—C1—Si125.03 (17)C22—Ti—C20—C24144.9 (2)
C3—Ti—C1—Si159.95 (12)C8—Ti—C20—C2450.4 (3)
C9—Ti—C1—Si160.70 (12)C2—Ti—C20—C2418.0 (2)
C8—C1—C2—C32.7 (2)C3—Ti—C20—C2452.0 (2)
Si—C1—C2—C3144.79 (17)C9—Ti—C20—C2475.4 (2)
Ti—C1—C2—C367.14 (17)Si—Ti—C20—C2452.6 (2)
C8—C1—C2—C16175.9 (2)C24—C20—C21—C22177.0 (2)
Si—C1—C2—C1636.6 (3)Ti—C20—C21—C2247.1 (2)
Ti—C1—C2—C16114.2 (2)C24—C20—C21—Ti129.9 (2)
C8—C1—C2—Ti69.89 (14)N1—Ti—C21—C22106.28 (16)
Si—C1—C2—Ti77.65 (15)C20—Ti—C21—C22141.4 (2)
N1—Ti—C2—C3169.69 (13)C23—Ti—C21—C2223.74 (14)
C20—Ti—C2—C388.74 (15)C1—Ti—C21—C22121.45 (17)
C23—Ti—C2—C322.1 (3)C8—Ti—C21—C2268.88 (18)
C1—Ti—C2—C3117.5 (2)C2—Ti—C21—C22132.59 (15)
C21—Ti—C2—C351.39 (15)C3—Ti—C21—C22106.93 (15)
C22—Ti—C2—C318.35 (18)C9—Ti—C21—C2275.35 (15)
C8—Ti—C2—C376.78 (14)Si—Ti—C21—C22153.47 (14)
C9—Ti—C2—C335.69 (13)N1—Ti—C21—C2035.09 (18)
Si—Ti—C2—C3152.84 (15)C23—Ti—C21—C20117.63 (16)
N1—Ti—C2—C152.20 (14)C1—Ti—C21—C2097.18 (18)
C20—Ti—C2—C1153.77 (14)C22—Ti—C21—C20141.4 (2)
C23—Ti—C2—C195.4 (2)C8—Ti—C21—C20149.74 (14)
C21—Ti—C2—C1168.88 (14)C2—Ti—C21—C2086.03 (15)
C22—Ti—C2—C1135.84 (14)C3—Ti—C21—C20111.70 (15)
C8—Ti—C2—C140.71 (13)C9—Ti—C21—C20143.28 (14)
C3—Ti—C2—C1117.5 (2)Si—Ti—C21—C2012.1 (3)
C9—Ti—C2—C181.80 (14)C20—C21—C22—C230.6 (4)
Si—Ti—C2—C135.35 (12)Ti—C21—C22—C2346.4 (2)
N1—Ti—C2—C1667.2 (2)C20—C21—C22—Ti45.8 (2)
C20—Ti—C2—C1634.4 (2)N1—Ti—C22—C21105.91 (16)
C23—Ti—C2—C16145.2 (2)C20—Ti—C22—C2123.74 (14)
C1—Ti—C2—C16119.4 (3)C23—Ti—C22—C21141.3 (2)
C21—Ti—C2—C1671.7 (2)C1—Ti—C22—C21112.62 (18)
C22—Ti—C2—C16104.8 (2)C8—Ti—C22—C21130.79 (14)
C8—Ti—C2—C16160.1 (2)C2—Ti—C22—C2163.58 (18)
C3—Ti—C2—C16123.1 (3)C3—Ti—C22—C2173.66 (15)
C9—Ti—C2—C16158.8 (2)C9—Ti—C22—C21106.16 (15)
Si—Ti—C2—C1684.0 (2)Si—Ti—C22—C21144.35 (19)
C1—C2—C3—C92.8 (3)N1—Ti—C22—C2335.43 (18)
C16—C2—C3—C9175.9 (2)C20—Ti—C22—C23117.60 (16)
Ti—C2—C3—C963.22 (16)C1—Ti—C22—C23106.03 (18)
C1—C2—C3—C17175.0 (2)C21—Ti—C22—C23141.3 (2)
C16—C2—C3—C173.7 (4)C8—Ti—C22—C2387.87 (15)
Ti—C2—C3—C17124.6 (2)C2—Ti—C22—C23155.08 (14)
C1—C2—C3—Ti60.44 (15)C3—Ti—C22—C23145.00 (14)
C16—C2—C3—Ti120.9 (2)C9—Ti—C22—C23112.50 (15)
N1—Ti—C3—C213.91 (18)Si—Ti—C22—C233.0 (3)
C20—Ti—C3—C297.67 (14)C21—C22—C23—C30179.0 (2)
C23—Ti—C3—C2169.81 (13)Ti—C22—C23—C30133.6 (2)
C1—Ti—C3—C238.22 (13)C21—C22—C23—Ti47.4 (2)
C21—Ti—C3—C2131.73 (15)N1—Ti—C23—C22153.68 (14)
C22—Ti—C3—C2165.65 (14)C20—Ti—C23—C2254.99 (15)
C8—Ti—C3—C281.57 (15)C1—Ti—C23—C22125.21 (16)
C9—Ti—C3—C2118.2 (2)C21—Ti—C23—C2223.12 (14)
Si—Ti—C3—C225.17 (14)C8—Ti—C23—C22105.43 (14)
N1—Ti—C3—C9104.30 (15)C2—Ti—C23—C2258.6 (3)
C20—Ti—C3—C9144.13 (14)C3—Ti—C23—C2243.99 (17)
C23—Ti—C3—C951.61 (16)C9—Ti—C23—C2270.20 (15)
C1—Ti—C3—C979.99 (14)Si—Ti—C23—C22178.88 (11)
C21—Ti—C3—C9110.06 (15)N1—Ti—C23—C3084.7 (2)
C22—Ti—C3—C976.15 (14)C20—Ti—C23—C30176.6 (2)
C8—Ti—C3—C936.63 (13)C1—Ti—C23—C303.6 (3)
C2—Ti—C3—C9118.2 (2)C21—Ti—C23—C30144.8 (3)
Si—Ti—C3—C993.03 (13)C22—Ti—C23—C30121.6 (3)
N1—Ti—C3—C17130.7 (2)C8—Ti—C23—C3016.2 (3)
C20—Ti—C3—C1719.2 (3)C2—Ti—C23—C3063.0 (3)
C23—Ti—C3—C1773.4 (3)C3—Ti—C23—C3077.6 (2)
C1—Ti—C3—C17155.0 (3)C9—Ti—C23—C3051.4 (2)
C21—Ti—C3—C1714.9 (2)Si—Ti—C23—C3057.2 (3)
C22—Ti—C3—C1748.8 (2)C21—C20—C24—C25179.5 (2)
C8—Ti—C3—C17161.6 (3)Ti—C20—C24—C2579.9 (3)
C2—Ti—C3—C17116.8 (3)C21—C20—C24—C291.7 (3)
C9—Ti—C3—C17125.0 (3)Ti—C20—C24—C29101.3 (3)
Si—Ti—C3—C17142.0 (2)C29—C24—C25—C261.8 (4)
C9—C4—C5—C62.3 (4)C20—C24—C25—C26179.3 (2)
C18—C4—C5—C6179.1 (2)C24—C25—C26—C270.8 (4)
C4—C5—C6—C71.9 (4)C25—C26—C27—C280.3 (4)
C4—C5—C6—C19176.5 (2)C26—C27—C28—C290.5 (4)
C5—C6—C7—C81.7 (3)C27—C28—C29—C240.6 (4)
C19—C6—C7—C8180.0 (2)C25—C24—C29—C281.7 (4)
C6—C7—C8—C1179.2 (2)C20—C24—C29—C28179.5 (2)
C6—C7—C8—C94.6 (3)C22—C23—C30—C31167.0 (2)
C6—C7—C8—Ti96.4 (2)Ti—C23—C30—C3191.9 (3)
C2—C1—C8—C7178.1 (2)C22—C23—C30—C3511.9 (4)
Si—C1—C8—C730.2 (3)Ti—C23—C30—C3589.3 (3)
Ti—C1—C8—C7107.7 (2)C35—C30—C31—C321.9 (4)
C2—C1—C8—C91.7 (2)C23—C30—C31—C32177.0 (2)
Si—C1—C8—C9146.21 (16)C30—C31—C32—C331.3 (4)
Ti—C1—C8—C968.74 (15)C31—C32—C33—C340.2 (4)
C2—C1—C8—Ti70.42 (14)C32—C33—C34—C351.0 (4)
Si—C1—C8—Ti77.47 (14)C33—C34—C35—C300.3 (4)
N1—Ti—C8—C770.93 (18)C31—C30—C35—C341.1 (3)
C20—Ti—C8—C7154.2 (2)C23—C30—C35—C34177.8 (2)

Experimental details

Crystal data
Chemical formula[Ti(C19H27NSi)(C16H14)]
Mr551.68
Crystal system, space groupMonoclinic, P21/n
Temperature (K)173
a, b, c (Å)11.0726 (6), 20.509 (1), 13.9311 (8)
β (°) 112.020 (1)
V3)2932.9 (3)
Z4
Radiation typeMo Kα
µ (mm1)0.36
Crystal size (mm)0.19 × 0.15 × 0.09
Data collection
DiffractometerBruker SMART
diffractometer
Absorption correctionAnalytical
integration, based on measured indexed faces (SHELXTL; Sheldrick, 1998)
Tmin, Tmax0.931, 0.973
No. of measured, independent and
observed [I > 2σ(I)] reflections
20107, 6740, 4070
Rint0.055
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.044, 0.103, 0.96
No. of reflections6740
No. of parameters383
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.32, 0.31

Computer programs: SMART (Bruker, 1998), SMART and SAINT (Bruker, 1998), SHELXTL (Bruker, 1998), SHELXTL.

Selected geometric parameters (Å, º) top
Ti—N11.963 (2)Ti—C92.490 (2)
Ti—C202.217 (2)C20—C211.416 (3)
Ti—C232.233 (2)C20—H200.93 (2)
Ti—C12.242 (2)C21—C221.397 (3)
Ti—C212.295 (2)C21—H210.96 (2)
Ti—C222.295 (2)C22—C231.419 (3)
Ti—C82.334 (2)C22—H220.98 (2)
Ti—C22.355 (2)C23—H230.99 (2)
Ti—C32.476 (2)
Cp—Ti—N1110.40 (8)C20—Ti—C2386.82 (8)
N1—Ti—C2099.09 (8)C22—C21—C20125.7 (2)
N1—Ti—C2399.33 (8)C21—C22—C23126.1 (2)
C12—C13—C14—C1520.5 (2)C20—C21—C22—C230.6 (4)
 

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