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A Comparative Study of (tBu3Si)SiX2SiX2(SitBu3) (X = Cl, Br, I) Including the Result of the X-Ray Structure Analysis of (tBu3Si)SiI2SiI2(SitBu3)

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Abstract

The tetraiodotetrasilane (tBu3Si)SiI2SiI2(SitBu3) can be prepared from precursor (tBu3Si)SiH2SiH2(SitBu3). When (tBu3Si)SiH2SiH2(SitBu3) was treated with an excess of iodine at 120 °C, (tBu3Si)SiI2SiI2(SitBu3) was formed. X-ray quality crystals of (tBu3Si)SiI2SiI2(SitBu3) were grown from benzene at ambient temperature. The tetraiodotetrasilane (tBu3Si)SiI2SiI2(SitBu3) crystallizes in the monoclinic space group C2/c, a = 10.0110(10) Å, b = 13.9130(10) Å, c = 25.422(2) Å, β = 99.072(4)°, V = 3496.6(5) Å3, Z = 4, d calcd = 1.829 g cm3; R 1 = 0.0844, wR 2 = 0.1854 for 3,017 reflections with I > 2σ(I). X-ray-crystallographic data show that the bromo and iodo derivatives (tBu3Si)SiX2SiX2(SitBu3) (X = Br, I) are isomorphous. The solid-state structure of (tBu3Si)SiI2SiI2(SitBu3) as well as those of (tBu3Si)SiX2SiX2(SitBu3) (X = Cl, Br) reveals a staggered conformation which adopts a trans-orientation of the supersilyl substituent. Unequal dihedral angles as found in (tBu3Si)SiX2SiX2(SitBu3) (X = Cl, Br, I) indicate that these compounds are sterically overcrowded.

Graphical Abstract

In the solid-state (tBu3Si)SiI2SiI2(SitBu3) features a staggered conformation which adopts a trans-orientation of the supersilyl group. However the solid-state structure of (tBu3Si)SiI2SiI2(SitBu3) reveals unequal dihedral angles.

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Notes

  1. Thermolysis of hexasupersilyl-triprismo-hexastannane Sn6(SitBu3)6 gives the spiro-tricyclo[2.1.0.0]pentastannane Sn9(SitBu3)8 – structural details: CCDC 760832.

  2. Structural parameters of cocrystals composed of (tBu3Si)GeCl2GeCl2(SitBu3) and the trigermaoxetane (tBu3Si)3Ge3Cl3O are listed in Table 1, see Ref. 19. For structural details of (tBu3Si)GeCl2GeCl2(SitBu3), see Ref. 20.

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Acknowledgement

We are grateful to the University of Frankfurt for funding.

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  1. Institut für Anorganische Chemie, Goethe-Universität Frankfurt am Main, Max-von-Laue-Straße 7, 60438, Frankfurt, Germany

    Michael Bolte & Hans-Wolfram Lerner

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  1. Michael Bolte
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  2. Hans-Wolfram Lerner
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Correspondence to Hans-Wolfram Lerner.

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Bolte, M., Lerner, HW. A Comparative Study of (tBu3Si)SiX2SiX2(SitBu3) (X = Cl, Br, I) Including the Result of the X-Ray Structure Analysis of (tBu3Si)SiI2SiI2(SitBu3). J Chem Crystallogr 41, 132–136 (2011). https://doi.org/10.1007/s10870-010-9851-2

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