Bis­[η⁵-1,3-bis­(tri­methyl­silyl)­cyclo­penta­dienyl]­vanadium(II)

The title compound, [V(C₁₁H₂₁Si₂)₂], crystallizes in space group C2/c with the V atom located on a twofold symmetry axis. The vanadium(II) center is coordinated by two 1,3-bis­(tri­methyl­silyl)­cyclo­penta­dienyl rings (Cp′′) to form a slightly bent metallocene [Cp(centroid)—V—Cp(centroid) = 173.0 (1)°].

Key indicators

• Single-crystal X-ray study
• T = 137 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.048
• wR factor = 0.134
• Data-to-parameter ratio = 18.9

checkCIF/PLATON results

No syntax errors found





Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.95

Alert level C
PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low ....       0.91
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.94
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       2.69 Ratio
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors  for        Si1

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   4 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 1995-1999); 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.

Bis[η⁵-1,3-bis(trimethylsilyl)cyclopentadienyl]vanadium(II)

Crystal data

[V(C11H21Si2)2]	F(000) = 1012
Mr = 469.86	Dx = 1.087 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2yc	Cell parameters from 2367 reflections
a = 12.451 (4) Å	θ = 2–25°
b = 18.447 (6) Å	µ = 0.52 mm^−1
c = 12.676 (5) Å	T = 137 K
β = 99.720 (8)°	Block, blue
V = 2869.8 (17) Å^3	0.34 × 0.30 × 0.10 mm
Z = 4

Data collection

Bruker SMART 1K CCD diffractometer	2432 independent reflections
Radiation source: fine-focus sealed tube	1690 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.034
ω scans	θmax = 25.5°, θmin = 2.0°
Absorption correction: multi-scan (Blessing, 1995)	h = −14→13
Tmin = 0.874, Tmax = 0.946	k = −21→21
6382 measured reflections	l = −5→15

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.048	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.134	H-atom parameters constrained
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0818P)^2] where P = (Fo^2 + 2Fc^2)/3
2432 reflections	(Δ/σ)max < 0.001
129 parameters	Δρmax = 0.97 e Å^−3
0 restraints	Δρmin = −0.33 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
V1	0.0000	0.38930 (4)	0.2500	0.0315 (3)
Si1	0.26423 (8)	0.47501 (6)	0.27193 (8)	0.0466 (3)
Si2	0.02026 (8)	0.24888 (5)	0.46248 (7)	0.0417 (3)
C1	0.1643 (3)	0.42535 (17)	0.3387 (2)	0.0338 (7)
C2	0.1528 (2)	0.35062 (18)	0.3565 (2)	0.0356 (8)
H2	0.1983	0.3143	0.3344	0.043*
C3	0.0646 (2)	0.33617 (17)	0.4119 (2)	0.0305 (7)
C4	0.0214 (3)	0.40654 (18)	0.4295 (2)	0.0401 (8)
H4	−0.0384	0.4155	0.4653	0.048*
C5	0.0806 (3)	0.45956 (18)	0.3861 (2)	0.0410 (8)
H5	0.0677	0.5103	0.3877	0.049*
C6	0.2015 (4)	0.5592 (2)	0.2105 (4)	0.0818 (15)
H6A	0.1385	0.5469	0.1559	0.123*
H6B	0.2550	0.5859	0.1771	0.123*
H6C	0.1776	0.5894	0.2658	0.123*
C7	0.3083 (4)	0.4155 (3)	0.1671 (3)	0.0810 (15)
H7A	0.2481	0.4102	0.1069	0.121*
H7B	0.3290	0.3678	0.1978	0.121*
H7C	0.3709	0.4376	0.1417	0.121*
C8	0.3861 (3)	0.4989 (2)	0.3709 (3)	0.0576 (11)
H8A	0.4367	0.5271	0.3357	0.086*
H8B	0.4222	0.4545	0.4009	0.086*
H8C	0.3641	0.5278	0.4286	0.086*
C9	−0.1275 (3)	0.2309 (2)	0.4145 (3)	0.0556 (10)
H9A	−0.1708	0.2705	0.4374	0.083*
H9B	−0.1480	0.1851	0.4448	0.083*
H9C	−0.1412	0.2278	0.3362	0.083*
C10	0.0476 (4)	0.2508 (2)	0.6116 (3)	0.0631 (12)
H10A	0.1235	0.2649	0.6365	0.095*
H10B	0.0346	0.2026	0.6393	0.095*
H10C	−0.0010	0.2860	0.6373	0.095*
C11	0.1019 (3)	0.17489 (19)	0.4138 (3)	0.0522 (10)
H11A	0.0903	0.1754	0.3354	0.078*
H11B	0.0788	0.1280	0.4387	0.078*
H11C	0.1794	0.1825	0.4418	0.078*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V1	0.0287 (4)	0.0406 (5)	0.0243 (4)	0.000	0.0015 (3)	0.000
Si1	0.0418 (6)	0.0501 (6)	0.0440 (6)	−0.0172 (5)	−0.0044 (5)	0.0113 (5)
Si2	0.0423 (6)	0.0466 (6)	0.0368 (6)	−0.0044 (4)	0.0083 (4)	0.0085 (4)
C1	0.0329 (18)	0.0391 (19)	0.0271 (17)	−0.0026 (15)	−0.0012 (14)	0.0020 (14)
C2	0.0302 (17)	0.0428 (19)	0.0318 (17)	0.0018 (15)	−0.0007 (14)	0.0023 (15)
C3	0.0270 (16)	0.0408 (18)	0.0227 (16)	0.0014 (14)	0.0015 (13)	0.0014 (13)
C4	0.042 (2)	0.052 (2)	0.0254 (17)	0.0020 (17)	0.0042 (14)	−0.0073 (15)
C5	0.051 (2)	0.0378 (19)	0.0317 (18)	0.0016 (17)	−0.0001 (16)	−0.0060 (15)
C6	0.068 (3)	0.068 (3)	0.102 (4)	−0.016 (2)	−0.009 (3)	0.043 (3)
C7	0.064 (3)	0.127 (4)	0.058 (3)	−0.043 (3)	0.026 (2)	−0.016 (3)
C8	0.049 (2)	0.062 (3)	0.059 (3)	−0.018 (2)	0.0014 (19)	−0.001 (2)
C9	0.040 (2)	0.060 (2)	0.069 (3)	−0.0071 (19)	0.0164 (19)	0.009 (2)
C10	0.078 (3)	0.073 (3)	0.042 (2)	−0.007 (2)	0.019 (2)	0.015 (2)
C11	0.056 (2)	0.049 (2)	0.052 (2)	−0.0008 (18)	0.0110 (19)	0.0080 (18)

Geometric parameters (Å, º)

V1—C1	2.261 (3)	C2—H2	0.9500
V1—C1^i	2.261 (3)	C3—C4	1.437 (4)
V1—C2^i	2.255 (3)	C4—C5	1.393 (5)
V1—C2	2.255 (3)	C4—H4	0.9500
V1—C3^i	2.293 (3)	C5—H5	0.9500
V1—C3	2.293 (3)	C6—H6A	0.9800
V1—C4	2.268 (3)	C6—H6B	0.9800
V1—C4^i	2.268 (3)	C6—H6C	0.9800
V1—C5	2.254 (3)	C7—H7A	0.9800
V1—C5^i	2.254 (3)	C7—H7B	0.9800
V1—Cg1	1.92 (1)	C7—H7C	0.9800
V1—Cg1^i	1.92 (1)	C8—H8A	0.9800
Si2—C3	1.852 (3)	C8—H8B	0.9800
Si2—C10	1.863 (4)	C8—H8C	0.9800
Si2—C9	1.867 (4)	C9—H9A	0.9800
Si2—C11	1.868 (4)	C9—H9B	0.9800
Si1—C6	1.850 (4)	C9—H9C	0.9800
Si1—C8	1.852 (4)	C10—H10A	0.9800
Si1—C1	1.861 (3)	C10—H10B	0.9800
Si1—C7	1.876 (4)	C10—H10C	0.9800
C1—C2	1.408 (4)	C11—H11A	0.9800
C1—C5	1.433 (4)	C11—H11B	0.9800
C2—C3	1.425 (4)	C11—H11C	0.9800
C5—V1—C5^i	109.81 (17)	C5—C1—V1	71.21 (17)
Cg1—V1—Cg1^i	173.00	Si1—C1—V1	122.46 (15)
C5—V1—C2^i	149.55 (12)	C1—C2—C3	111.6 (3)
C5^i—V1—C2^i	60.12 (12)	C1—C2—V1	72.07 (18)
C5—V1—C2	60.12 (12)	C3—C2—V1	73.20 (17)
C5^i—V1—C2	149.55 (12)	C1—C2—H2	124.2
C2^i—V1—C2	143.10 (17)	C3—C2—H2	124.2
C5—V1—C1	37.01 (11)	V1—C2—H2	122.1
C5^i—V1—C1	117.41 (12)	C2—C3—C4	104.3 (3)
C2^i—V1—C1	172.64 (11)	C2—C3—Si2	129.2 (2)
C2—V1—C1	36.33 (11)	C4—C3—Si2	126.2 (2)
C5—V1—C1^i	117.41 (12)	C2—C3—V1	70.29 (16)
C5^i—V1—C1^i	37.01 (11)	C4—C3—V1	70.70 (17)
C2^i—V1—C1^i	36.33 (11)	Si2—C3—V1	126.99 (15)
C2—V1—C1^i	172.64 (11)	C5—C4—C3	109.6 (3)
C1—V1—C1^i	145.80 (16)	C5—C4—V1	71.50 (18)
C5—V1—C4	35.87 (11)	C3—C4—V1	72.59 (16)
C5^i—V1—C4	130.47 (13)	C5—C4—H4	125.2
C2^i—V1—C4	126.10 (12)	C3—C4—H4	125.2
C2—V1—C4	59.97 (12)	V1—C4—H4	122.3
C1—V1—C4	61.09 (12)	C4—C5—C1	109.1 (3)
C1^i—V1—C4	113.64 (12)	C4—C5—V1	72.63 (18)
C5—V1—C4^i	130.47 (13)	C1—C5—V1	71.77 (17)
C5^i—V1—C4^i	35.87 (11)	C4—C5—H5	125.5
C2^i—V1—C4^i	59.97 (12)	C1—C5—H5	125.5
C2—V1—C4^i	126.10 (12)	V1—C5—H5	121.8
C1—V1—C4^i	113.64 (12)	Si1—C6—H6A	109.5
C1^i—V1—C4^i	61.09 (12)	Si1—C6—H6B	109.5
C4—V1—C4^i	163.88 (17)	H6A—C6—H6B	109.5
C5—V1—C3^i	166.96 (12)	Si1—C6—H6C	109.5
C5^i—V1—C3^i	61.13 (12)	H6A—C6—H6C	109.5
C2^i—V1—C3^i	36.51 (10)	H6B—C6—H6C	109.5
C2—V1—C3^i	122.23 (11)	Si1—C7—H7A	109.5
C1—V1—C3^i	136.19 (11)	Si1—C7—H7B	109.5
C1^i—V1—C3^i	61.94 (11)	H7A—C7—H7B	109.5
C4—V1—C3^i	157.14 (12)	Si1—C7—H7C	109.5
C4^i—V1—C3^i	36.71 (11)	H7A—C7—H7C	109.5
C5—V1—C3	61.13 (12)	H7B—C7—H7C	109.5
C5^i—V1—C3	166.96 (11)	Si1—C8—H8A	109.5
C2^i—V1—C3	122.23 (11)	Si1—C8—H8B	109.5
C2—V1—C3	36.51 (11)	H8A—C8—H8B	109.5
C1—V1—C3	61.94 (11)	Si1—C8—H8C	109.5
C1^i—V1—C3	136.19 (11)	H8A—C8—H8C	109.5
C4—V1—C3	36.71 (11)	H8B—C8—H8C	109.5
C4^i—V1—C3	157.14 (12)	Si2—C9—H9A	109.5
C3^i—V1—C3	129.40 (16)	Si2—C9—H9B	109.5
C3—Si2—C10	108.70 (16)	H9A—C9—H9B	109.5
C3—Si2—C9	112.09 (15)	Si2—C9—H9C	109.5
C10—Si2—C9	109.56 (18)	H9A—C9—H9C	109.5
C3—Si2—C11	108.09 (15)	H9B—C9—H9C	109.5
C10—Si2—C11	109.44 (18)	Si2—C10—H10A	109.5
C9—Si2—C11	108.92 (18)	Si2—C10—H10B	109.5
C6—Si1—C8	109.0 (2)	H10A—C10—H10B	109.5
C6—Si1—C1	109.72 (18)	Si2—C10—H10C	109.5
C8—Si1—C1	110.09 (16)	H10A—C10—H10C	109.5
C6—Si1—C7	110.2 (2)	H10B—C10—H10C	109.5
C8—Si1—C7	108.3 (2)	Si2—C11—H11A	109.5
C1—Si1—C7	109.45 (17)	Si2—C11—H11B	109.5
C2—C1—C5	105.3 (3)	H11A—C11—H11B	109.5
C2—C1—Si1	130.4 (2)	Si2—C11—H11C	109.5
C5—C1—Si1	124.3 (3)	H11A—C11—H11C	109.5
C2—C1—V1	71.60 (17)	H11B—C11—H11C	109.5
C6—Si1—C1—C2	150.4 (3)	C5—V1—C3—C2	−77.8 (2)
C8—Si1—C1—C2	−89.6 (3)	C5^i—V1—C3—C2	−126.1 (5)
C7—Si1—C1—C2	29.4 (4)	C2^i—V1—C3—C2	137.5 (2)
C6—Si1—C1—C5	−30.8 (3)	C1—V1—C3—C2	−35.47 (18)
C8—Si1—C1—C5	89.1 (3)	C1^i—V1—C3—C2	−178.44 (19)
C7—Si1—C1—C5	−151.9 (3)	C4—V1—C3—C2	−113.8 (3)
C6—Si1—C1—V1	57.6 (3)	C4^i—V1—C3—C2	49.1 (4)
C8—Si1—C1—V1	177.49 (18)	C3^i—V1—C3—C2	92.88 (18)
C7—Si1—C1—V1	−63.5 (2)	C5—V1—C3—C4	36.05 (19)
C5—V1—C1—C2	114.0 (3)	C5^i—V1—C3—C4	−12.3 (6)
C5^i—V1—C1—C2	−159.08 (19)	C2^i—V1—C3—C4	−108.7 (2)
C1^i—V1—C1—C2	167.77 (19)	C2—V1—C3—C4	113.8 (3)
C4—V1—C1—C2	77.6 (2)	C1—V1—C3—C4	78.4 (2)
C4^i—V1—C1—C2	−119.38 (19)	C1^i—V1—C3—C4	−64.6 (2)
C3^i—V1—C1—C2	−83.3 (2)	C4^i—V1—C3—C4	162.9 (2)
C3—V1—C1—C2	35.65 (18)	C3^i—V1—C3—C4	−153.3 (2)
C5^i—V1—C1—C5	86.9 (3)	C5—V1—C3—Si2	157.4 (2)
C2—V1—C1—C5	−114.0 (3)	C5^i—V1—C3—Si2	109.1 (5)
C1^i—V1—C1—C5	53.76 (17)	C2^i—V1—C3—Si2	12.7 (2)
C4—V1—C1—C5	−36.38 (19)	C2—V1—C3—Si2	−124.9 (3)
C4^i—V1—C1—C5	126.6 (2)	C1—V1—C3—Si2	−160.3 (2)
C3^i—V1—C1—C5	162.74 (18)	C1^i—V1—C3—Si2	56.7 (3)
C3—V1—C1—C5	−78.4 (2)	C4—V1—C3—Si2	121.3 (3)
C5—V1—C1—Si1	−119.2 (3)	C3^i—V1—C3—Si2	−31.97 (15)
C5^i—V1—C1—Si1	−32.3 (2)	C2—C3—C4—C5	0.4 (3)
C2—V1—C1—Si1	126.7 (3)	Si2—C3—C4—C5	175.4 (2)
C1^i—V1—C1—Si1	−65.49 (16)	V1—C3—C4—C5	−62.3 (2)
C4—V1—C1—Si1	−155.6 (2)	C2—C3—C4—V1	62.72 (19)
C4^i—V1—C1—Si1	7.4 (2)	Si2—C3—C4—V1	−122.3 (2)
C3^i—V1—C1—Si1	43.5 (3)	C5^i—V1—C4—C5	−65.2 (3)
C3—V1—C1—Si1	162.4 (2)	C2^i—V1—C4—C5	−144.3 (2)
C5—C1—C2—C3	0.8 (3)	C1—V1—C4—C5	37.54 (19)
Si1—C1—C2—C3	179.7 (2)	C1^i—V1—C4—C5	−104.6 (2)
V1—C1—C2—C3	−62.9 (2)	C3^i—V1—C4—C5	−178.2 (3)
C5—C1—C2—V1	63.7 (2)	C3—V1—C4—C5	118.4 (3)
Si1—C1—C2—V1	−117.4 (3)	C5—V1—C4—C3	−118.4 (3)
C5—V1—C2—C1	−39.36 (18)	C5^i—V1—C4—C3	176.39 (17)
C5^i—V1—C2—C1	38.7 (3)	C2^i—V1—C4—C3	97.2 (2)
C2^i—V1—C2—C1	167.67 (19)	C2—V1—C4—C3	−38.95 (17)
C4—V1—C2—C1	−81.0 (2)	C1—V1—C4—C3	−80.89 (19)
C4^i—V1—C2—C1	81.1 (2)	C1^i—V1—C4—C3	136.95 (18)
C3^i—V1—C2—C1	125.64 (19)	C3^i—V1—C4—C3	63.4 (4)
C3—V1—C2—C1	−120.2 (3)	C3—C4—C5—C1	0.1 (4)
C5—V1—C2—C3	80.8 (2)	C3—C4—C5—V1	63.0 (2)
C5^i—V1—C2—C3	158.9 (2)	C2—C1—C5—C4	−0.5 (3)
C2^i—V1—C2—C3	−72.15 (17)	Si1—C1—C5—C4	−179.5 (2)
C1—V1—C2—C3	120.2 (3)	V1—C1—C5—C4	63.5 (2)
C4—V1—C2—C3	39.17 (18)	C2—C1—C5—V1	−64.0 (2)
C4^i—V1—C2—C3	−158.69 (18)	Si1—C1—C5—V1	117.0 (2)
C3^i—V1—C2—C3	−114.2 (2)	C5^i—V1—C5—C4	132.8 (2)
C1—C2—C3—C4	−0.8 (3)	C2^i—V1—C5—C4	68.4 (3)
V1—C2—C3—C4	−63.00 (19)	C1—V1—C5—C4	−117.6 (3)
C1—C2—C3—Si2	−175.6 (2)	C1^i—V1—C5—C4	93.1 (2)
V1—C2—C3—Si2	122.2 (2)	C4^i—V1—C5—C4	167.21 (15)
C1—C2—C3—V1	62.2 (2)	C3^i—V1—C5—C4	176.8 (4)
C10—Si2—C3—C2	111.5 (3)	C3—V1—C5—C4	−36.89 (19)
C9—Si2—C3—C2	−127.2 (3)	C5^i—V1—C5—C1	−109.6 (2)
C11—Si2—C3—C2	−7.2 (3)	C2^i—V1—C5—C1	−174.0 (2)
C10—Si2—C3—C4	−62.3 (3)	C2—V1—C5—C1	38.62 (18)
C9—Si2—C3—C4	59.0 (3)	C1^i—V1—C5—C1	−149.29 (18)
C11—Si2—C3—C4	179.0 (3)	C4—V1—C5—C1	117.6 (3)
C10—Si2—C3—V1	−154.5 (2)	C4^i—V1—C5—C1	−75.2 (2)
C9—Si2—C3—V1	−33.2 (2)	C3^i—V1—C5—C1	−65.6 (6)
C11—Si2—C3—V1	86.8 (2)	C3—V1—C5—C1	80.74 (19)

Symmetry code: (i) −x, y, −z+1/2.