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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)°].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804020276/wk6028sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804020276/wk6028Isup2.hkl
Contains datablock I

CCDC reference: 251607

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

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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

Computing details top

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) top
Crystal data top
[V(C11H21Si2)2]F(000) = 1012
Mr = 469.86Dx = 1.087 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
Hall symbol: -C 2ycCell parameters from 2367 reflections
a = 12.451 (4) Åθ = 2–25°
b = 18.447 (6) ŵ = 0.52 mm1
c = 12.676 (5) ÅT = 137 K
β = 99.720 (8)°Block, blue
V = 2869.8 (17) Å30.34 × 0.30 × 0.10 mm
Z = 4
Data collection top
Bruker SMART 1K CCD
diffractometer
2432 independent reflections
Radiation source: fine-focus sealed tube1690 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
ω scansθmax = 25.5°, θmin = 2.0°
Absorption correction: multi-scan
(Blessing, 1995)
h = 1413
Tmin = 0.874, Tmax = 0.946k = 2121
6382 measured reflectionsl = 515
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)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.134H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0818P)2]
where P = (Fo2 + 2Fc2)/3
2432 reflections(Δ/σ)max < 0.001
129 parametersΔρmax = 0.97 e Å3
0 restraintsΔρmin = 0.33 e Å3
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
V10.00000.38930 (4)0.25000.0315 (3)
Si10.26423 (8)0.47501 (6)0.27193 (8)0.0466 (3)
Si20.02026 (8)0.24888 (5)0.46248 (7)0.0417 (3)
C10.1643 (3)0.42535 (17)0.3387 (2)0.0338 (7)
C20.1528 (2)0.35062 (18)0.3565 (2)0.0356 (8)
H20.19830.31430.33440.043*
C30.0646 (2)0.33617 (17)0.4119 (2)0.0305 (7)
C40.0214 (3)0.40654 (18)0.4295 (2)0.0401 (8)
H40.03840.41550.46530.048*
C50.0806 (3)0.45956 (18)0.3861 (2)0.0410 (8)
H50.06770.51030.38770.049*
C60.2015 (4)0.5592 (2)0.2105 (4)0.0818 (15)
H6A0.13850.54690.15590.123*
H6B0.25500.58590.17710.123*
H6C0.17760.58940.26580.123*
C70.3083 (4)0.4155 (3)0.1671 (3)0.0810 (15)
H7A0.24810.41020.10690.121*
H7B0.32900.36780.19780.121*
H7C0.37090.43760.14170.121*
C80.3861 (3)0.4989 (2)0.3709 (3)0.0576 (11)
H8A0.43670.52710.33570.086*
H8B0.42220.45450.40090.086*
H8C0.36410.52780.42860.086*
C90.1275 (3)0.2309 (2)0.4145 (3)0.0556 (10)
H9A0.17080.27050.43740.083*
H9B0.14800.18510.44480.083*
H9C0.14120.22780.33620.083*
C100.0476 (4)0.2508 (2)0.6116 (3)0.0631 (12)
H10A0.12350.26490.63650.095*
H10B0.03460.20260.63930.095*
H10C0.00100.28600.63730.095*
C110.1019 (3)0.17489 (19)0.4138 (3)0.0522 (10)
H11A0.09030.17540.33540.078*
H11B0.07880.12800.43870.078*
H11C0.17940.18250.44180.078*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0287 (4)0.0406 (5)0.0243 (4)0.0000.0015 (3)0.000
Si10.0418 (6)0.0501 (6)0.0440 (6)0.0172 (5)0.0044 (5)0.0113 (5)
Si20.0423 (6)0.0466 (6)0.0368 (6)0.0044 (4)0.0083 (4)0.0085 (4)
C10.0329 (18)0.0391 (19)0.0271 (17)0.0026 (15)0.0012 (14)0.0020 (14)
C20.0302 (17)0.0428 (19)0.0318 (17)0.0018 (15)0.0007 (14)0.0023 (15)
C30.0270 (16)0.0408 (18)0.0227 (16)0.0014 (14)0.0015 (13)0.0014 (13)
C40.042 (2)0.052 (2)0.0254 (17)0.0020 (17)0.0042 (14)0.0073 (15)
C50.051 (2)0.0378 (19)0.0317 (18)0.0016 (17)0.0001 (16)0.0060 (15)
C60.068 (3)0.068 (3)0.102 (4)0.016 (2)0.009 (3)0.043 (3)
C70.064 (3)0.127 (4)0.058 (3)0.043 (3)0.026 (2)0.016 (3)
C80.049 (2)0.062 (3)0.059 (3)0.018 (2)0.0014 (19)0.001 (2)
C90.040 (2)0.060 (2)0.069 (3)0.0071 (19)0.0164 (19)0.009 (2)
C100.078 (3)0.073 (3)0.042 (2)0.007 (2)0.019 (2)0.015 (2)
C110.056 (2)0.049 (2)0.052 (2)0.0008 (18)0.0110 (19)0.0080 (18)
Geometric parameters (Å, º) top
V1—C12.261 (3)C2—H20.9500
V1—C1i2.261 (3)C3—C41.437 (4)
V1—C2i2.255 (3)C4—C51.393 (5)
V1—C22.255 (3)C4—H40.9500
V1—C3i2.293 (3)C5—H50.9500
V1—C32.293 (3)C6—H6A0.9800
V1—C42.268 (3)C6—H6B0.9800
V1—C4i2.268 (3)C6—H6C0.9800
V1—C52.254 (3)C7—H7A0.9800
V1—C5i2.254 (3)C7—H7B0.9800
V1—Cg11.92 (1)C7—H7C0.9800
V1—Cg1i1.92 (1)C8—H8A0.9800
Si2—C31.852 (3)C8—H8B0.9800
Si2—C101.863 (4)C8—H8C0.9800
Si2—C91.867 (4)C9—H9A0.9800
Si2—C111.868 (4)C9—H9B0.9800
Si1—C61.850 (4)C9—H9C0.9800
Si1—C81.852 (4)C10—H10A0.9800
Si1—C11.861 (3)C10—H10B0.9800
Si1—C71.876 (4)C10—H10C0.9800
C1—C21.408 (4)C11—H11A0.9800
C1—C51.433 (4)C11—H11B0.9800
C2—C31.425 (4)C11—H11C0.9800
C5—V1—C5i109.81 (17)C5—C1—V171.21 (17)
Cg1—V1—Cg1i173.00Si1—C1—V1122.46 (15)
C5—V1—C2i149.55 (12)C1—C2—C3111.6 (3)
C5i—V1—C2i60.12 (12)C1—C2—V172.07 (18)
C5—V1—C260.12 (12)C3—C2—V173.20 (17)
C5i—V1—C2149.55 (12)C1—C2—H2124.2
C2i—V1—C2143.10 (17)C3—C2—H2124.2
C5—V1—C137.01 (11)V1—C2—H2122.1
C5i—V1—C1117.41 (12)C2—C3—C4104.3 (3)
C2i—V1—C1172.64 (11)C2—C3—Si2129.2 (2)
C2—V1—C136.33 (11)C4—C3—Si2126.2 (2)
C5—V1—C1i117.41 (12)C2—C3—V170.29 (16)
C5i—V1—C1i37.01 (11)C4—C3—V170.70 (17)
C2i—V1—C1i36.33 (11)Si2—C3—V1126.99 (15)
C2—V1—C1i172.64 (11)C5—C4—C3109.6 (3)
C1—V1—C1i145.80 (16)C5—C4—V171.50 (18)
C5—V1—C435.87 (11)C3—C4—V172.59 (16)
C5i—V1—C4130.47 (13)C5—C4—H4125.2
C2i—V1—C4126.10 (12)C3—C4—H4125.2
C2—V1—C459.97 (12)V1—C4—H4122.3
C1—V1—C461.09 (12)C4—C5—C1109.1 (3)
C1i—V1—C4113.64 (12)C4—C5—V172.63 (18)
C5—V1—C4i130.47 (13)C1—C5—V171.77 (17)
C5i—V1—C4i35.87 (11)C4—C5—H5125.5
C2i—V1—C4i59.97 (12)C1—C5—H5125.5
C2—V1—C4i126.10 (12)V1—C5—H5121.8
C1—V1—C4i113.64 (12)Si1—C6—H6A109.5
C1i—V1—C4i61.09 (12)Si1—C6—H6B109.5
C4—V1—C4i163.88 (17)H6A—C6—H6B109.5
C5—V1—C3i166.96 (12)Si1—C6—H6C109.5
C5i—V1—C3i61.13 (12)H6A—C6—H6C109.5
C2i—V1—C3i36.51 (10)H6B—C6—H6C109.5
C2—V1—C3i122.23 (11)Si1—C7—H7A109.5
C1—V1—C3i136.19 (11)Si1—C7—H7B109.5
C1i—V1—C3i61.94 (11)H7A—C7—H7B109.5
C4—V1—C3i157.14 (12)Si1—C7—H7C109.5
C4i—V1—C3i36.71 (11)H7A—C7—H7C109.5
C5—V1—C361.13 (12)H7B—C7—H7C109.5
C5i—V1—C3166.96 (11)Si1—C8—H8A109.5
C2i—V1—C3122.23 (11)Si1—C8—H8B109.5
C2—V1—C336.51 (11)H8A—C8—H8B109.5
C1—V1—C361.94 (11)Si1—C8—H8C109.5
C1i—V1—C3136.19 (11)H8A—C8—H8C109.5
C4—V1—C336.71 (11)H8B—C8—H8C109.5
C4i—V1—C3157.14 (12)Si2—C9—H9A109.5
C3i—V1—C3129.40 (16)Si2—C9—H9B109.5
C3—Si2—C10108.70 (16)H9A—C9—H9B109.5
C3—Si2—C9112.09 (15)Si2—C9—H9C109.5
C10—Si2—C9109.56 (18)H9A—C9—H9C109.5
C3—Si2—C11108.09 (15)H9B—C9—H9C109.5
C10—Si2—C11109.44 (18)Si2—C10—H10A109.5
C9—Si2—C11108.92 (18)Si2—C10—H10B109.5
C6—Si1—C8109.0 (2)H10A—C10—H10B109.5
C6—Si1—C1109.72 (18)Si2—C10—H10C109.5
C8—Si1—C1110.09 (16)H10A—C10—H10C109.5
C6—Si1—C7110.2 (2)H10B—C10—H10C109.5
C8—Si1—C7108.3 (2)Si2—C11—H11A109.5
C1—Si1—C7109.45 (17)Si2—C11—H11B109.5
C2—C1—C5105.3 (3)H11A—C11—H11B109.5
C2—C1—Si1130.4 (2)Si2—C11—H11C109.5
C5—C1—Si1124.3 (3)H11A—C11—H11C109.5
C2—C1—V171.60 (17)H11B—C11—H11C109.5
C6—Si1—C1—C2150.4 (3)C5—V1—C3—C277.8 (2)
C8—Si1—C1—C289.6 (3)C5i—V1—C3—C2126.1 (5)
C7—Si1—C1—C229.4 (4)C2i—V1—C3—C2137.5 (2)
C6—Si1—C1—C530.8 (3)C1—V1—C3—C235.47 (18)
C8—Si1—C1—C589.1 (3)C1i—V1—C3—C2178.44 (19)
C7—Si1—C1—C5151.9 (3)C4—V1—C3—C2113.8 (3)
C6—Si1—C1—V157.6 (3)C4i—V1—C3—C249.1 (4)
C8—Si1—C1—V1177.49 (18)C3i—V1—C3—C292.88 (18)
C7—Si1—C1—V163.5 (2)C5—V1—C3—C436.05 (19)
C5—V1—C1—C2114.0 (3)C5i—V1—C3—C412.3 (6)
C5i—V1—C1—C2159.08 (19)C2i—V1—C3—C4108.7 (2)
C1i—V1—C1—C2167.77 (19)C2—V1—C3—C4113.8 (3)
C4—V1—C1—C277.6 (2)C1—V1—C3—C478.4 (2)
C4i—V1—C1—C2119.38 (19)C1i—V1—C3—C464.6 (2)
C3i—V1—C1—C283.3 (2)C4i—V1—C3—C4162.9 (2)
C3—V1—C1—C235.65 (18)C3i—V1—C3—C4153.3 (2)
C5i—V1—C1—C586.9 (3)C5—V1—C3—Si2157.4 (2)
C2—V1—C1—C5114.0 (3)C5i—V1—C3—Si2109.1 (5)
C1i—V1—C1—C553.76 (17)C2i—V1—C3—Si212.7 (2)
C4—V1—C1—C536.38 (19)C2—V1—C3—Si2124.9 (3)
C4i—V1—C1—C5126.6 (2)C1—V1—C3—Si2160.3 (2)
C3i—V1—C1—C5162.74 (18)C1i—V1—C3—Si256.7 (3)
C3—V1—C1—C578.4 (2)C4—V1—C3—Si2121.3 (3)
C5—V1—C1—Si1119.2 (3)C3i—V1—C3—Si231.97 (15)
C5i—V1—C1—Si132.3 (2)C2—C3—C4—C50.4 (3)
C2—V1—C1—Si1126.7 (3)Si2—C3—C4—C5175.4 (2)
C1i—V1—C1—Si165.49 (16)V1—C3—C4—C562.3 (2)
C4—V1—C1—Si1155.6 (2)C2—C3—C4—V162.72 (19)
C4i—V1—C1—Si17.4 (2)Si2—C3—C4—V1122.3 (2)
C3i—V1—C1—Si143.5 (3)C5i—V1—C4—C565.2 (3)
C3—V1—C1—Si1162.4 (2)C2i—V1—C4—C5144.3 (2)
C5—C1—C2—C30.8 (3)C1—V1—C4—C537.54 (19)
Si1—C1—C2—C3179.7 (2)C1i—V1—C4—C5104.6 (2)
V1—C1—C2—C362.9 (2)C3i—V1—C4—C5178.2 (3)
C5—C1—C2—V163.7 (2)C3—V1—C4—C5118.4 (3)
Si1—C1—C2—V1117.4 (3)C5—V1—C4—C3118.4 (3)
C5—V1—C2—C139.36 (18)C5i—V1—C4—C3176.39 (17)
C5i—V1—C2—C138.7 (3)C2i—V1—C4—C397.2 (2)
C2i—V1—C2—C1167.67 (19)C2—V1—C4—C338.95 (17)
C4—V1—C2—C181.0 (2)C1—V1—C4—C380.89 (19)
C4i—V1—C2—C181.1 (2)C1i—V1—C4—C3136.95 (18)
C3i—V1—C2—C1125.64 (19)C3i—V1—C4—C363.4 (4)
C3—V1—C2—C1120.2 (3)C3—C4—C5—C10.1 (4)
C5—V1—C2—C380.8 (2)C3—C4—C5—V163.0 (2)
C5i—V1—C2—C3158.9 (2)C2—C1—C5—C40.5 (3)
C2i—V1—C2—C372.15 (17)Si1—C1—C5—C4179.5 (2)
C1—V1—C2—C3120.2 (3)V1—C1—C5—C463.5 (2)
C4—V1—C2—C339.17 (18)C2—C1—C5—V164.0 (2)
C4i—V1—C2—C3158.69 (18)Si1—C1—C5—V1117.0 (2)
C3i—V1—C2—C3114.2 (2)C5i—V1—C5—C4132.8 (2)
C1—C2—C3—C40.8 (3)C2i—V1—C5—C468.4 (3)
V1—C2—C3—C463.00 (19)C1—V1—C5—C4117.6 (3)
C1—C2—C3—Si2175.6 (2)C1i—V1—C5—C493.1 (2)
V1—C2—C3—Si2122.2 (2)C4i—V1—C5—C4167.21 (15)
C1—C2—C3—V162.2 (2)C3i—V1—C5—C4176.8 (4)
C10—Si2—C3—C2111.5 (3)C3—V1—C5—C436.89 (19)
C9—Si2—C3—C2127.2 (3)C5i—V1—C5—C1109.6 (2)
C11—Si2—C3—C27.2 (3)C2i—V1—C5—C1174.0 (2)
C10—Si2—C3—C462.3 (3)C2—V1—C5—C138.62 (18)
C9—Si2—C3—C459.0 (3)C1i—V1—C5—C1149.29 (18)
C11—Si2—C3—C4179.0 (3)C4—V1—C5—C1117.6 (3)
C10—Si2—C3—V1154.5 (2)C4i—V1—C5—C175.2 (2)
C9—Si2—C3—V133.2 (2)C3i—V1—C5—C165.6 (6)
C11—Si2—C3—V186.8 (2)C3—V1—C5—C180.74 (19)
Symmetry code: (i) x, y, z+1/2.
 

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