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The title compound, [Ti(C11H21Si2)2(NH2)], crystallizes as a bent metallocene, with the NH2 group oriented to maximize the π interaction between the N atom and the TiIII center. The increased π bonding is reflected in a short Ti—N bond length of 1.933 (3) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104018840/fa1076sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270104018840/fa1076Isup2.hkl
Contains datablock I

CCDC reference: 251301

Comment top

The title compound, [Cp''2Ti(NH2)], (I) [Cp'' is 1,3-bis(trimethylsilyl)cyclopentadienyl] crystallizes in the primitive monoclinic space group P21/n with four discrete molecules in the unit cell. Selected distances and angles are given in Table 1. Fig. 1 shows the molecular geometry and the atom-numbering scheme. \sch

The Ti center is coordinated by two virtually planar 1,3-bis(trimethylsilyl)cyclopentadienyl rings in a staggered conformation relative to each other, and by an NH2 group. The angle between the cyclopentadienyl ligands, Cg1—Ti—Cg2, is 137.90 (8)° (the cyclopentadienyl ligands are represented by their centroids, Cg1 and Cg2). The distances between the Ti atom and Cg1 and Cg2 are 2.0611 (17) and 2.0623 (17) Å, respectively. These are comparable with values found for other Cp2TiNR2 derivatives (Brady et al., 1994; Lukens et al., 1996; Feldman & Calabrese, 1991).

The amide group is located within an open wedge formed by the sterically demanding trimethylsilyl groups, allowing the least steric bulk and a proper orientation for the filled p orbital to interact with the empty b2 orbital of the Cp''2Ti fragment, enabling the NH2 moiety to act as a π donor. This is also reflected in the small Cp(centroid)-Ti—N—H torsion angle of only 6.4° and the quite short Ti—N distance of 1.933 (3) Å. Similar N—M π bonding is also observed in [(η5-C5Me5)2Ti(NH2)] [Ti—N 1.944 (2) Å; Brady et al., 1994), [(η5-C5Me5)2Ti(NHMe)] [Ti—N 1.955 (2) Å; Lukens et al., 1996] and [(η5-C5Me5)2Hf(NHMe)] (Hillhouse et al., 1988), as evidenced by a similar orientation of the amide group as well as short (Ti,Hf)—N distances.

The influence of steric bulk versus electronic effects is demonstrated in bis(pentamethylcyclopentadienyl)titanium(III) N-methyl-N-phenylamide (Feldman & Calabrese, 1991), in which the amide ligand adopts a perpendicular orientation to the plane formed by the Ti atom and the two cyclopentadienyl ring centroids, preventing the p orbital from interacting with the b2 orbital of the [(η5-C5Me5)2Ti] fragment. Therefore, the Ti—N distance [2.054 (2) Å] is elongated compared with that of (I).

Experimental top

The title compound was synthesized from Cp''2TiMe and dry NH3 in n-hexane, in a manner similar to that used for (C5Me5)2Ti(NH2) (Brady et al., 1994). Dichroic (green and brown) crystals were grown by slow cooling of a saturated hexane solution to 193 K. The crystal was handled under a nitrogen atmosphere, mounted on a glass fiber with Paratone-N hydrocarbon oil and cooled to 133 (2) K for data collection.

Refinement top

H atoms on the trimethylsilyl groups, as well as those on the cyclopentadienyl rings, were included in calculated positions, with C—H distances in the range 0.95–0.98 Å, and refined using a riding model, with Uiso(H) = 1.5Ueq(C). Please check added text. The amide H atoms (H23A and H23B) were located using standard difference Fourier techniques and refined isotropically.

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. A view of the structure of (I), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. H atoms on the cyclopentadienyl ring have been omitted for clarity.
Amidobis[η5-1,3-bis(trimethylsilyl)cyclopentadienyl]titanium(III) top
Crystal data top
[Ti(C11H21Si2)2(NH2)]F(000) = 1044
Mr = 482.84Dx = 1.128 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5983 reflections
a = 13.0945 (3) Åθ = 2–51.2°
b = 16.5699 (3) ŵ = 0.48 mm1
c = 13.1869 (2) ÅT = 133 K
β = 96.488 (1)°Block, dichroic (green/brown)
V = 2842.90 (9) Å30.38 × 0.32 × 0.18 mm
Z = 4
Data collection top
Bruker SMART 1K CCD area-detector
diffractometer
5071 independent reflections
Radiation source: fine-focus sealed tube3874 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.059
ω scansθmax = 26.1°, θmin = 2.0°
Absorption correction: multi-scan
(Blessing, 1995)
h = 1613
Tmin = 0.839, Tmax = 0.919k = 2018
13362 measured reflectionsl = 1514
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)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.113H atoms treated by a mixture of independent and constrained refinement
S = 1.13 w = 1/[σ2(Fo2) + (0.0201P)2 + 5.0672P]
where P = (Fo2 + 2Fc2)/3
5071 reflections(Δ/σ)max < 0.001
273 parametersΔρmax = 0.47 e Å3
0 restraintsΔρmin = 0.32 e Å3
Crystal data top
[Ti(C11H21Si2)2(NH2)]V = 2842.90 (9) Å3
Mr = 482.84Z = 4
Monoclinic, P21/nMo Kα radiation
a = 13.0945 (3) ŵ = 0.48 mm1
b = 16.5699 (3) ÅT = 133 K
c = 13.1869 (2) Å0.38 × 0.32 × 0.18 mm
β = 96.488 (1)°
Data collection top
Bruker SMART 1K CCD area-detector
diffractometer
5071 independent reflections
Absorption correction: multi-scan
(Blessing, 1995)
3874 reflections with I > 2σ(I)
Tmin = 0.839, Tmax = 0.919Rint = 0.059
13362 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0540 restraints
wR(F2) = 0.113H atoms treated by a mixture of independent and constrained refinement
S = 1.13Δρmax = 0.47 e Å3
5071 reflectionsΔρmin = 0.32 e Å3
273 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
xyzUiso*/Ueq
Ti10.01970 (4)0.22140 (4)0.85769 (5)0.01785 (16)
Si10.04813 (7)0.00459 (6)0.75035 (8)0.0241 (2)
Si20.30932 (7)0.19111 (6)0.90584 (8)0.0256 (2)
Si30.07909 (7)0.45105 (6)0.83708 (8)0.0234 (2)
Si40.25685 (7)0.23428 (6)0.91279 (8)0.0247 (2)
N10.0049 (3)0.2395 (2)0.7120 (3)0.0316 (8)
H23A0.019 (3)0.208 (3)0.665 (3)0.044 (13)*
H23B0.018 (3)0.283 (3)0.680 (3)0.050 (13)*
C10.0299 (2)0.0762 (2)0.8373 (3)0.0217 (8)
C20.1227 (2)0.11158 (19)0.8135 (3)0.0214 (8)
H20.14610.10970.74790.026*
C30.1763 (2)0.1501 (2)0.8998 (2)0.0211 (7)
C40.1136 (3)0.1376 (2)0.9799 (3)0.0221 (8)
H40.12890.15621.04810.027*
C50.0256 (3)0.0934 (2)0.9422 (3)0.0241 (8)
H50.02810.07770.98090.029*
C60.0103 (3)0.36520 (19)0.8918 (3)0.0209 (7)
C70.0894 (3)0.33583 (19)0.8549 (3)0.0220 (8)
H70.12720.35250.79270.026*
C80.1252 (2)0.2785 (2)0.9227 (3)0.0218 (7)
C90.0453 (3)0.2735 (2)1.0060 (3)0.0236 (8)
H90.04710.24111.06520.028*
C100.0364 (3)0.32421 (19)0.9866 (3)0.0233 (8)
H100.09910.33031.02970.028*
C110.3222 (3)0.2890 (2)0.9756 (3)0.0335 (9)
H11A0.27450.32840.94100.050*
H11B0.39280.30890.97680.050*
H11C0.30600.28111.04570.050*
C120.3983 (3)0.1167 (2)0.9758 (3)0.0421 (11)
H12A0.46930.13600.97760.063*
H12B0.39160.06450.94090.063*
H12C0.38080.11071.04580.063*
C130.3410 (3)0.2051 (2)0.7725 (3)0.0344 (9)
H13A0.29510.24580.73790.052*
H13B0.33220.15380.73560.052*
H13C0.41240.22320.77390.052*
C140.0186 (3)0.0950 (2)0.7648 (3)0.0321 (9)
H14A0.01930.13470.72020.048*
H14B0.02150.11290.83590.048*
H14C0.08850.08960.74600.048*
C150.0502 (4)0.0397 (3)0.6168 (3)0.0500 (12)
H15A0.08530.00050.57070.075*
H15B0.02040.04680.60060.075*
H15C0.08690.09120.60860.075*
C160.1822 (3)0.0083 (2)0.7822 (4)0.0433 (11)
H16A0.21970.04260.77030.065*
H16B0.18080.02370.85410.065*
H16C0.21660.05060.73900.065*
C170.0222 (3)0.5200 (2)0.7745 (3)0.0374 (10)
H17A0.01050.56700.74670.056*
H17B0.06690.53780.82490.056*
H17C0.06320.49120.71910.056*
C180.1574 (3)0.5047 (2)0.9436 (3)0.0361 (10)
H18A0.20410.46630.98160.054*
H18B0.11170.52830.98960.054*
H18C0.19740.54760.91560.054*
C190.1639 (3)0.4194 (2)0.7403 (3)0.0359 (10)
H19A0.19820.46680.71560.054*
H19B0.12260.39310.68310.054*
H19C0.21570.38140.77140.054*
C200.3418 (3)0.3054 (2)0.9748 (3)0.0359 (10)
H20A0.41270.28540.96540.054*
H20B0.33890.35890.94360.054*
H20C0.31830.30911.04790.054*
C210.3045 (3)0.2237 (2)0.7743 (3)0.0346 (9)
H21A0.25490.19230.74020.052*
H21B0.31250.27730.74310.052*
H21C0.37100.19590.76710.052*
C220.2569 (3)0.1359 (2)0.9812 (3)0.0359 (10)
H22A0.21260.09760.95030.054*
H22B0.32710.11470.97610.054*
H22C0.23100.14381.05320.054*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.0200 (3)0.0162 (3)0.0171 (3)0.0006 (2)0.0010 (2)0.0007 (3)
Si10.0255 (5)0.0172 (5)0.0278 (6)0.0011 (4)0.0053 (4)0.0002 (4)
Si20.0190 (5)0.0245 (5)0.0322 (6)0.0002 (4)0.0023 (4)0.0043 (4)
Si30.0223 (5)0.0188 (5)0.0292 (6)0.0011 (4)0.0043 (4)0.0014 (4)
Si40.0210 (5)0.0246 (5)0.0290 (6)0.0008 (4)0.0051 (4)0.0016 (4)
N10.049 (2)0.0250 (18)0.0202 (18)0.0087 (16)0.0007 (15)0.0014 (15)
C10.0223 (18)0.0177 (17)0.024 (2)0.0020 (14)0.0014 (15)0.0016 (14)
C20.0229 (18)0.0185 (17)0.0230 (19)0.0031 (14)0.0034 (15)0.0002 (14)
C30.0233 (18)0.0182 (18)0.0207 (19)0.0035 (14)0.0026 (15)0.0011 (15)
C40.0277 (19)0.0182 (17)0.0190 (19)0.0083 (15)0.0030 (15)0.0001 (14)
C50.0248 (19)0.0179 (18)0.030 (2)0.0016 (15)0.0023 (15)0.0054 (15)
C60.0240 (18)0.0137 (16)0.0255 (19)0.0008 (14)0.0046 (15)0.0029 (14)
C70.0244 (18)0.0178 (17)0.0238 (19)0.0042 (14)0.0034 (15)0.0027 (14)
C80.0213 (18)0.0203 (17)0.0242 (19)0.0046 (15)0.0044 (14)0.0011 (15)
C90.0263 (19)0.0244 (19)0.0206 (19)0.0044 (15)0.0044 (15)0.0009 (15)
C100.0259 (19)0.0172 (18)0.026 (2)0.0024 (15)0.0001 (15)0.0048 (15)
C110.025 (2)0.036 (2)0.038 (2)0.0010 (17)0.0039 (17)0.0127 (18)
C120.032 (2)0.037 (2)0.053 (3)0.0071 (19)0.012 (2)0.002 (2)
C130.032 (2)0.030 (2)0.042 (2)0.0047 (17)0.0096 (18)0.0043 (18)
C140.035 (2)0.0209 (19)0.038 (2)0.0004 (16)0.0046 (18)0.0030 (17)
C150.084 (3)0.030 (2)0.031 (2)0.015 (2)0.012 (2)0.0005 (19)
C160.028 (2)0.030 (2)0.070 (3)0.0014 (18)0.004 (2)0.012 (2)
C170.035 (2)0.029 (2)0.048 (3)0.0016 (18)0.0021 (19)0.0155 (19)
C180.041 (2)0.024 (2)0.043 (3)0.0046 (18)0.0019 (19)0.0002 (18)
C190.033 (2)0.035 (2)0.042 (2)0.0029 (18)0.0124 (18)0.0025 (19)
C200.025 (2)0.040 (2)0.044 (3)0.0005 (18)0.0083 (18)0.002 (2)
C210.032 (2)0.038 (2)0.033 (2)0.0046 (18)0.0000 (17)0.0005 (19)
C220.034 (2)0.033 (2)0.041 (2)0.0033 (18)0.0090 (18)0.0097 (19)
Geometric parameters (Å, º) top
Ti1—C12.426 (3)C7—H70.9500
Ti1—C22.376 (3)C8—C91.431 (5)
Ti1—C32.377 (3)C9—C101.406 (5)
Ti1—C42.364 (3)C9—H90.9500
Ti1—C52.393 (3)C10—H100.9500
Ti1—C62.430 (3)C11—H11A0.9800
Ti1—C72.372 (3)C11—H11B0.9800
Ti1—C82.366 (3)C11—H11C0.9800
Ti1—C92.382 (3)C12—H12A0.9800
Ti1—C102.399 (3)C12—H12B0.9800
Ti1—N11.933 (3)C12—H12C0.9800
Ti1—Cg12.0611 (17)C13—H13A0.9800
Ti1—Cg22.0623 (17)C13—H13B0.9800
N1—H23A0.85 (4)C13—H13C0.9800
N1—H23B0.87 (5)C14—H14A0.9800
Si1—C151.851 (4)C14—H14B0.9800
Si1—C161.863 (4)C14—H14C0.9800
Si1—C141.866 (4)C15—H15A0.9800
Si1—C11.872 (3)C15—H15B0.9800
Si2—C111.863 (4)C15—H15C0.9800
Si2—C31.863 (3)C16—H16A0.9800
Si2—C131.866 (4)C16—H16B0.9800
Si2—C121.867 (4)C16—H16C0.9800
Si3—C191.860 (4)C17—H17A0.9800
Si3—C181.868 (4)C17—H17B0.9800
Si3—C171.870 (4)C17—H17C0.9800
Si3—C61.871 (3)C18—H18A0.9800
Si4—C221.862 (4)C18—H18B0.9800
Si4—C81.864 (3)C18—H18C0.9800
Si4—C211.870 (4)C19—H19A0.9800
Si4—C201.871 (4)C19—H19B0.9800
C1—C21.416 (5)C19—H19C0.9800
C1—C51.420 (5)C20—H20A0.9800
C2—C31.420 (5)C20—H20B0.9800
C2—H20.9500C20—H20C0.9800
C3—C41.423 (5)C21—H21A0.9800
C4—C51.408 (5)C21—H21B0.9800
C4—H40.9500C21—H21C0.9800
C5—H50.9500C22—H22A0.9800
C6—C71.426 (5)C22—H22B0.9800
C6—C101.430 (5)C22—H22C0.9800
C7—C81.420 (5)
N1—Ti1—C4139.00 (14)C4—C5—C1109.1 (3)
N1—Ti1—C8107.69 (14)C4—C5—Ti171.66 (19)
C4—Ti1—C8111.38 (12)C1—C5—Ti174.13 (19)
N1—Ti1—C782.41 (14)C4—C5—H5125.5
C4—Ti1—C7138.26 (12)C1—C5—H5125.5
C8—Ti1—C734.88 (11)Ti1—C5—H5120.5
N1—Ti1—C282.57 (14)C7—C6—C10104.8 (3)
C4—Ti1—C256.74 (12)C7—C6—Si3126.2 (3)
C8—Ti1—C2153.59 (12)C10—C6—Si3128.3 (3)
C7—Ti1—C2164.97 (12)C7—C6—Ti170.49 (18)
N1—Ti1—C3107.24 (14)C10—C6—Ti171.56 (18)
C4—Ti1—C334.94 (11)Si3—C6—Ti1129.59 (16)
C8—Ti1—C3145.07 (12)C8—C7—C6111.6 (3)
C7—Ti1—C3154.55 (12)C8—C7—Ti172.34 (18)
C2—Ti1—C334.77 (11)C6—C7—Ti174.98 (18)
N1—Ti1—C9139.05 (14)C8—C7—H7124.2
C4—Ti1—C981.95 (12)C6—C7—H7124.2
C8—Ti1—C935.08 (11)Ti1—C7—H7120.0
C7—Ti1—C956.80 (12)C7—C8—C9104.9 (3)
C2—Ti1—C9138.12 (12)C7—C8—Si4125.9 (3)
C3—Ti1—C9111.54 (12)C9—C8—Si4128.4 (3)
N1—Ti1—C5126.51 (14)C7—C8—Ti172.77 (18)
C4—Ti1—C534.43 (11)C9—C8—Ti173.06 (18)
C8—Ti1—C599.81 (12)Si4—C8—Ti1126.17 (17)
C7—Ti1—C5134.69 (12)C10—C9—C8109.3 (3)
C2—Ti1—C556.39 (12)C10—C9—Ti173.55 (19)
C3—Ti1—C557.95 (11)C8—C9—Ti171.86 (19)
C9—Ti1—C586.24 (12)C10—C9—H9125.4
N1—Ti1—C10125.81 (14)C8—C9—H9125.4
C4—Ti1—C1086.31 (12)Ti1—C9—H9120.9
C8—Ti1—C1058.10 (12)C9—C10—C6109.4 (3)
C7—Ti1—C1056.61 (12)C9—C10—Ti172.25 (19)
C2—Ti1—C10135.15 (12)C6—C10—Ti174.00 (19)
C3—Ti1—C10100.39 (12)C9—C10—H10125.3
C9—Ti1—C1034.20 (11)C6—C10—H10125.3
C5—Ti1—C10107.68 (12)Ti1—C10—H10120.2
N1—Ti1—C192.54 (13)Si2—C11—H11A109.5
C4—Ti1—C157.47 (11)Si2—C11—H11B109.5
C8—Ti1—C1119.54 (12)H11A—C11—H11B109.5
C7—Ti1—C1146.25 (12)Si2—C11—H11C109.5
C2—Ti1—C134.28 (11)H11A—C11—H11C109.5
C3—Ti1—C158.43 (11)H11B—C11—H11C109.5
C9—Ti1—C1118.66 (12)Si2—C12—H12A109.5
C5—Ti1—C134.26 (11)Si2—C12—H12B109.5
C10—Ti1—C1141.35 (12)H12A—C12—H12B109.5
N1—Ti1—C691.73 (14)Si2—C12—H12C109.5
C4—Ti1—C6118.89 (12)H12A—C12—H12C109.5
C8—Ti1—C658.76 (11)H12B—C12—H12C109.5
C7—Ti1—C634.52 (11)Si2—C13—H13A109.5
C2—Ti1—C6146.95 (12)Si2—C13—H13B109.5
C3—Ti1—C6120.29 (12)H13A—C13—H13B109.5
C9—Ti1—C657.48 (12)Si2—C13—H13C109.5
C5—Ti1—C6141.47 (12)H13A—C13—H13C109.5
C10—Ti1—C634.44 (11)H13B—C13—H13C109.5
C1—Ti1—C6175.72 (12)Si1—C14—H14A109.5
C15—Si1—C16109.7 (2)Si1—C14—H14B109.5
C15—Si1—C14109.3 (2)H14A—C14—H14B109.5
C16—Si1—C14108.53 (18)Si1—C14—H14C109.5
C15—Si1—C1109.40 (17)H14A—C14—H14C109.5
C16—Si1—C1113.40 (17)H14B—C14—H14C109.5
C14—Si1—C1106.33 (16)Si1—C15—H15A109.5
C11—Si2—C3111.73 (16)Si1—C15—H15B109.5
C11—Si2—C13109.86 (18)H15A—C15—H15B109.5
C3—Si2—C13108.16 (16)Si1—C15—H15C109.5
C11—Si2—C12108.29 (18)H15A—C15—H15C109.5
C3—Si2—C12108.00 (17)H15B—C15—H15C109.5
C13—Si2—C12110.80 (19)Si1—C16—H16A109.5
C19—Si3—C18109.31 (18)Si1—C16—H16B109.5
C19—Si3—C17108.59 (19)H16A—C16—H16B109.5
C18—Si3—C17110.05 (18)Si1—C16—H16C109.5
C19—Si3—C6113.62 (16)H16A—C16—H16C109.5
C18—Si3—C6108.60 (17)H16B—C16—H16C109.5
C17—Si3—C6106.62 (16)Si3—C17—H17A109.5
C22—Si4—C8111.15 (16)Si3—C17—H17B109.5
C22—Si4—C21111.86 (19)H17A—C17—H17B109.5
C8—Si4—C21108.03 (16)Si3—C17—H17C109.5
C22—Si4—C20107.84 (18)H17A—C17—H17C109.5
C8—Si4—C20108.21 (16)H17B—C17—H17C109.5
C21—Si4—C20109.68 (18)Si3—C18—H18A109.5
Ti1—N1—H23A128 (3)Si3—C18—H18B109.5
Ti1—N1—H23B127 (3)H18A—C18—H18B109.5
H23A—N1—H23B105 (4)Si3—C18—H18C109.5
Cg1—Ti1—Cg2137.90 (8)H18A—C18—H18C109.5
Cg1—Ti1—N1111.13 (12)H18B—C18—H18C109.5
Cg2—Ti1—N1110.97 (12)Si3—C19—H19A109.5
C2—C1—C5105.2 (3)Si3—C19—H19B109.5
C2—C1—Si1123.3 (3)H19A—C19—H19B109.5
C5—C1—Si1130.2 (3)Si3—C19—H19C109.5
C2—C1—Ti170.95 (19)H19A—C19—H19C109.5
C5—C1—Ti171.61 (19)H19B—C19—H19C109.5
Si1—C1—Ti1131.59 (16)Si4—C20—H20A109.5
C1—C2—C3111.5 (3)Si4—C20—H20B109.5
C1—C2—Ti174.77 (19)H20A—C20—H20B109.5
C3—C2—Ti172.63 (19)Si4—C20—H20C109.5
C1—C2—H2124.2H20A—C20—H20C109.5
C3—C2—H2124.2H20B—C20—H20C109.5
Ti1—C2—H2119.9Si4—C21—H21A109.5
C2—C3—C4104.8 (3)Si4—C21—H21B109.5
C2—C3—Si2125.0 (3)H21A—C21—H21B109.5
C4—C3—Si2129.5 (2)Si4—C21—H21C109.5
C2—C3—Ti172.60 (18)H21A—C21—H21C109.5
C4—C3—Ti172.04 (18)H21B—C21—H21C109.5
Si2—C3—Ti1127.36 (16)Si4—C22—H22A109.5
C5—C4—C3109.4 (3)Si4—C22—H22B109.5
C5—C4—Ti173.91 (19)H22A—C22—H22B109.5
C3—C4—Ti173.01 (18)Si4—C22—H22C109.5
C5—C4—H4125.3H22A—C22—H22C109.5
C3—C4—H4125.3H22B—C22—H22C109.5
Ti1—C4—H4119.5
C15—Si1—C1—C240.2 (3)C19—Si3—C6—C792.2 (3)
C16—Si1—C1—C2163.0 (3)C18—Si3—C6—C7145.9 (3)
C14—Si1—C1—C277.8 (3)C17—Si3—C6—C727.4 (3)
C15—Si1—C1—C5154.7 (3)C19—Si3—C6—C1099.2 (3)
C16—Si1—C1—C531.9 (4)C18—Si3—C6—C1022.7 (4)
C14—Si1—C1—C587.3 (3)C17—Si3—C6—C10141.2 (3)
C15—Si1—C1—Ti153.3 (3)C19—Si3—C6—Ti11.7 (3)
C16—Si1—C1—Ti169.5 (3)C18—Si3—C6—Ti1120.2 (2)
C14—Si1—C1—Ti1171.3 (2)C17—Si3—C6—Ti1121.3 (2)
N1—Ti1—C1—C272.9 (2)N1—Ti1—C6—C773.9 (2)
C4—Ti1—C1—C277.3 (2)C4—Ti1—C6—C7134.6 (2)
C8—Ti1—C1—C2175.13 (19)C8—Ti1—C6—C735.79 (19)
C7—Ti1—C1—C2153.0 (2)C2—Ti1—C6—C7152.9 (2)
C3—Ti1—C1—C235.86 (19)C3—Ti1—C6—C7174.92 (19)
C9—Ti1—C1—C2134.8 (2)C9—Ti1—C6—C777.3 (2)
C5—Ti1—C1—C2114.1 (3)C5—Ti1—C6—C799.6 (2)
C10—Ti1—C1—C2100.4 (2)C10—Ti1—C6—C7113.8 (3)
N1—Ti1—C1—C5173.1 (2)N1—Ti1—C6—C10172.3 (2)
C4—Ti1—C1—C536.74 (19)C4—Ti1—C6—C1020.8 (2)
C8—Ti1—C1—C561.1 (2)C8—Ti1—C6—C1078.0 (2)
C7—Ti1—C1—C592.9 (3)C7—Ti1—C6—C10113.8 (3)
C2—Ti1—C1—C5114.1 (3)C2—Ti1—C6—C1093.3 (3)
C3—Ti1—C1—C578.2 (2)C3—Ti1—C6—C1061.1 (2)
C9—Ti1—C1—C520.7 (2)C9—Ti1—C6—C1036.43 (19)
C10—Ti1—C1—C513.6 (3)C5—Ti1—C6—C1014.2 (3)
N1—Ti1—C1—Si145.2 (2)N1—Ti1—C6—Si347.4 (2)
C4—Ti1—C1—Si1164.6 (3)C4—Ti1—C6—Si3104.1 (2)
C8—Ti1—C1—Si166.9 (3)C8—Ti1—C6—Si3157.1 (3)
C7—Ti1—C1—Si135.0 (4)C7—Ti1—C6—Si3121.3 (3)
C2—Ti1—C1—Si1118.0 (3)C2—Ti1—C6—Si331.6 (4)
C3—Ti1—C1—Si1153.9 (3)C3—Ti1—C6—Si363.8 (2)
C9—Ti1—C1—Si1107.2 (2)C9—Ti1—C6—Si3161.4 (3)
C5—Ti1—C1—Si1127.9 (3)C5—Ti1—C6—Si3139.1 (2)
C10—Ti1—C1—Si1141.6 (2)C10—Ti1—C6—Si3124.9 (3)
C5—C1—C2—C30.0 (4)C10—C6—C7—C80.2 (4)
Si1—C1—C2—C3168.3 (2)Si3—C6—C7—C8171.0 (2)
Ti1—C1—C2—C363.9 (2)Ti1—C6—C7—C863.6 (2)
C5—C1—C2—Ti163.9 (2)C10—C6—C7—Ti163.9 (2)
Si1—C1—C2—Ti1127.8 (2)Si3—C6—C7—Ti1125.4 (3)
N1—Ti1—C2—C1105.7 (2)N1—Ti1—C7—C8136.6 (2)
C4—Ti1—C2—C179.6 (2)C4—Ti1—C7—C849.4 (3)
C8—Ti1—C2—C19.6 (4)C2—Ti1—C7—C8134.2 (4)
C7—Ti1—C2—C1103.2 (5)C3—Ti1—C7—C8108.8 (3)
C3—Ti1—C2—C1118.9 (3)C9—Ti1—C7—C839.53 (19)
C9—Ti1—C2—C168.9 (3)C5—Ti1—C7—C81.2 (3)
C5—Ti1—C2—C138.11 (19)C10—Ti1—C7—C880.7 (2)
C10—Ti1—C2—C1119.4 (2)C1—Ti1—C7—C853.5 (3)
C6—Ti1—C2—C1172.6 (2)C6—Ti1—C7—C8119.0 (3)
N1—Ti1—C2—C3135.4 (2)N1—Ti1—C7—C6104.3 (2)
C4—Ti1—C2—C339.26 (19)C4—Ti1—C7—C669.6 (3)
C8—Ti1—C2—C3109.4 (3)C8—Ti1—C7—C6119.0 (3)
C7—Ti1—C2—C3137.8 (4)C2—Ti1—C7—C6106.8 (5)
C9—Ti1—C2—C350.0 (3)C3—Ti1—C7—C610.3 (4)
C5—Ti1—C2—C380.8 (2)C9—Ti1—C7—C679.5 (2)
C10—Ti1—C2—C30.5 (3)C5—Ti1—C7—C6120.2 (2)
C1—Ti1—C2—C3118.9 (3)C10—Ti1—C7—C638.30 (19)
C6—Ti1—C2—C353.7 (3)C1—Ti1—C7—C6172.5 (2)
C1—C2—C3—C40.2 (4)C6—C7—C8—C91.3 (4)
Ti1—C2—C3—C465.4 (2)Ti1—C7—C8—C966.5 (2)
C1—C2—C3—Si2170.9 (2)C6—C7—C8—Si4172.2 (2)
Ti1—C2—C3—Si2123.8 (3)Ti1—C7—C8—Si4122.6 (3)
C1—C2—C3—Ti165.2 (2)C6—C7—C8—Ti165.3 (2)
C11—Si2—C3—C2140.2 (3)C22—Si4—C8—C7157.3 (3)
C13—Si2—C3—C219.1 (3)C21—Si4—C8—C734.2 (3)
C12—Si2—C3—C2100.8 (3)C20—Si4—C8—C784.5 (3)
C11—Si2—C3—C451.4 (4)C22—Si4—C8—C934.0 (4)
C13—Si2—C3—C4172.4 (3)C21—Si4—C8—C9157.0 (3)
C12—Si2—C3—C467.6 (3)C20—Si4—C8—C984.3 (3)
C11—Si2—C3—Ti145.9 (3)C22—Si4—C8—Ti162.9 (3)
C13—Si2—C3—Ti175.2 (2)C21—Si4—C8—Ti160.2 (2)
C12—Si2—C3—Ti1164.9 (2)C20—Si4—C8—Ti1178.9 (2)
N1—Ti1—C3—C246.8 (2)N1—Ti1—C8—C745.6 (2)
C4—Ti1—C3—C2112.5 (3)C4—Ti1—C8—C7147.1 (2)
C8—Ti1—C3—C2132.9 (2)C2—Ti1—C8—C7155.3 (3)
C7—Ti1—C3—C2156.1 (3)C3—Ti1—C8—C7134.7 (2)
C9—Ti1—C3—C2146.63 (19)C9—Ti1—C8—C7112.1 (3)
C5—Ti1—C3—C275.9 (2)C5—Ti1—C8—C7179.1 (2)
C10—Ti1—C3—C2179.6 (2)C10—Ti1—C8—C776.1 (2)
C1—Ti1—C3—C235.36 (19)C1—Ti1—C8—C7149.13 (19)
C6—Ti1—C3—C2149.40 (19)C6—Ti1—C8—C735.42 (19)
N1—Ti1—C3—C4159.3 (2)N1—Ti1—C8—C9157.7 (2)
C8—Ti1—C3—C420.4 (3)C4—Ti1—C8—C935.0 (2)
C7—Ti1—C3—C491.4 (3)C7—Ti1—C8—C9112.1 (3)
C2—Ti1—C3—C4112.5 (3)C2—Ti1—C8—C992.6 (3)
C9—Ti1—C3—C434.1 (2)C3—Ti1—C8—C922.6 (3)
C5—Ti1—C3—C436.58 (19)C5—Ti1—C8—C968.8 (2)
C10—Ti1—C3—C467.9 (2)C10—Ti1—C8—C936.02 (19)
C1—Ti1—C3—C477.1 (2)C1—Ti1—C8—C998.8 (2)
C6—Ti1—C3—C498.1 (2)C6—Ti1—C8—C976.7 (2)
N1—Ti1—C3—Si274.3 (2)N1—Ti1—C8—Si476.7 (2)
C4—Ti1—C3—Si2126.4 (3)C4—Ti1—C8—Si490.6 (2)
C8—Ti1—C3—Si2106.0 (2)C7—Ti1—C8—Si4122.3 (3)
C7—Ti1—C3—Si235.0 (4)C2—Ti1—C8—Si433.0 (4)
C2—Ti1—C3—Si2121.1 (3)C3—Ti1—C8—Si4103.0 (2)
C9—Ti1—C3—Si292.3 (2)C9—Ti1—C8—Si4125.6 (3)
C5—Ti1—C3—Si2163.0 (3)C5—Ti1—C8—Si456.8 (2)
C10—Ti1—C3—Si258.5 (2)C10—Ti1—C8—Si4161.6 (3)
C1—Ti1—C3—Si2156.5 (3)C1—Ti1—C8—Si426.8 (3)
C6—Ti1—C3—Si228.3 (3)C6—Ti1—C8—Si4157.7 (3)
C2—C3—C4—C50.3 (4)C7—C8—C9—C101.8 (4)
Si2—C3—C4—C5170.5 (2)Si4—C8—C9—C10172.4 (2)
Ti1—C3—C4—C565.5 (2)Ti1—C8—C9—C1064.5 (2)
C2—C3—C4—Ti165.8 (2)C7—C8—C9—Ti166.3 (2)
Si2—C3—C4—Ti1124.0 (3)Si4—C8—C9—Ti1123.1 (3)
N1—Ti1—C4—C585.7 (3)N1—Ti1—C9—C1083.8 (3)
C8—Ti1—C4—C575.7 (2)C4—Ti1—C9—C1095.3 (2)
C7—Ti1—C4—C5103.5 (2)C8—Ti1—C9—C10117.3 (3)
C2—Ti1—C4—C577.6 (2)C7—Ti1—C9—C1078.0 (2)
C3—Ti1—C4—C5116.7 (3)C2—Ti1—C9—C10104.4 (2)
C9—Ti1—C4—C595.1 (2)C3—Ti1—C9—C1076.4 (2)
C10—Ti1—C4—C5129.2 (2)C5—Ti1—C9—C10129.7 (2)
C1—Ti1—C4—C536.56 (19)C1—Ti1—C9—C10141.17 (19)
C6—Ti1—C4—C5140.8 (2)C6—Ti1—C9—C1036.68 (19)
N1—Ti1—C4—C331.0 (3)N1—Ti1—C9—C833.5 (3)
C8—Ti1—C4—C3167.63 (19)C4—Ti1—C9—C8147.4 (2)
C7—Ti1—C4—C3139.8 (2)C7—Ti1—C9—C839.29 (19)
C2—Ti1—C4—C339.06 (19)C2—Ti1—C9—C8138.3 (2)
C9—Ti1—C4—C3148.2 (2)C3—Ti1—C9—C8166.30 (19)
C5—Ti1—C4—C3116.7 (3)C5—Ti1—C9—C8113.0 (2)
C10—Ti1—C4—C3114.1 (2)C10—Ti1—C9—C8117.3 (3)
C1—Ti1—C4—C380.1 (2)C1—Ti1—C9—C8101.5 (2)
C6—Ti1—C4—C3102.5 (2)C6—Ti1—C9—C880.7 (2)
C3—C4—C5—C10.3 (4)C8—C9—C10—C61.8 (4)
Ti1—C4—C5—C165.2 (2)Ti1—C9—C10—C665.2 (2)
C3—C4—C5—Ti164.9 (2)C8—C9—C10—Ti163.4 (2)
C2—C1—C5—C40.2 (4)C7—C6—C10—C90.9 (4)
Si1—C1—C5—C4167.0 (3)Si3—C6—C10—C9169.6 (2)
Ti1—C1—C5—C463.6 (2)Ti1—C6—C10—C964.1 (2)
C2—C1—C5—Ti163.4 (2)C7—C6—C10—Ti163.1 (2)
Si1—C1—C5—Ti1129.4 (3)Si3—C6—C10—Ti1126.4 (3)
N1—Ti1—C5—C4125.5 (2)N1—Ti1—C10—C9126.5 (2)
C8—Ti1—C5—C4113.7 (2)C4—Ti1—C10—C981.1 (2)
C7—Ti1—C5—C4114.4 (2)C8—Ti1—C10—C936.97 (19)
C2—Ti1—C5—C478.7 (2)C7—Ti1—C10—C978.6 (2)
C3—Ti1—C5—C437.14 (19)C2—Ti1—C10—C9113.5 (2)
C9—Ti1—C5—C481.2 (2)C3—Ti1—C10—C9113.2 (2)
C10—Ti1—C5—C454.2 (2)C5—Ti1—C10—C953.7 (2)
C1—Ti1—C5—C4116.9 (3)C1—Ti1—C10—C961.7 (3)
C6—Ti1—C5—C462.6 (3)C6—Ti1—C10—C9117.0 (3)
N1—Ti1—C5—C18.6 (3)N1—Ti1—C10—C69.5 (3)
C4—Ti1—C5—C1116.9 (3)C4—Ti1—C10—C6161.9 (2)
C8—Ti1—C5—C1129.4 (2)C8—Ti1—C10—C680.1 (2)
C7—Ti1—C5—C1128.7 (2)C7—Ti1—C10—C638.40 (19)
C2—Ti1—C5—C138.13 (19)C2—Ti1—C10—C6129.5 (2)
C3—Ti1—C5—C179.7 (2)C3—Ti1—C10—C6129.7 (2)
C9—Ti1—C5—C1161.9 (2)C9—Ti1—C10—C6117.0 (3)
C10—Ti1—C5—C1171.10 (19)C5—Ti1—C10—C6170.77 (19)
C6—Ti1—C5—C1179.47 (19)C1—Ti1—C10—C6178.79 (19)

Experimental details

Crystal data
Chemical formula[Ti(C11H21Si2)2(NH2)]
Mr482.84
Crystal system, space groupMonoclinic, P21/n
Temperature (K)133
a, b, c (Å)13.0945 (3), 16.5699 (3), 13.1869 (2)
β (°) 96.488 (1)
V3)2842.90 (9)
Z4
Radiation typeMo Kα
µ (mm1)0.48
Crystal size (mm)0.38 × 0.32 × 0.18
Data collection
DiffractometerBruker SMART 1K CCD area-detector
diffractometer
Absorption correctionMulti-scan
(Blessing, 1995)
Tmin, Tmax0.839, 0.919
No. of measured, independent and
observed [I > 2σ(I)] reflections
13362, 5071, 3874
Rint0.059
(sin θ/λ)max1)0.620
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.054, 0.113, 1.13
No. of reflections5071
No. of parameters273
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.47, 0.32

Computer programs: SMART (Bruker, 1999), SAINT (Bruker, 2002), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997), SHELXL97.

Selected geometric parameters (Å, º) top
Ti1—C12.426 (3)Ti1—C92.382 (3)
Ti1—C22.376 (3)Ti1—C102.399 (3)
Ti1—C32.377 (3)Ti1—N11.933 (3)
Ti1—C42.364 (3)Ti1—Cg12.0611 (17)
Ti1—C52.393 (3)Ti1—Cg22.0623 (17)
Ti1—C62.430 (3)N1—H23A0.85 (4)
Ti1—C72.372 (3)N1—H23B0.87 (5)
Ti1—C82.366 (3)
Ti1—N1—H23A128 (3)Cg1—Ti1—Cg2137.90 (8)
Ti1—N1—H23B127 (3)Cg1—Ti1—N1111.13 (12)
H23A—N1—H23B105 (4)Cg2—Ti1—N1110.97 (12)
 

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