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Synthesis and structure of the λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6]

  • Isabelle Georg , Michael Bolte , Matthias Wagner and Hans-Wolfram Lerner EMAIL logo
Published/Copyright: June 18, 2021
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Zeitschrift für Naturforschung B
From the journal Zeitschrift für Naturforschung B Volume 76 Issue 6-7

Abstract

The λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6] (1) was synthesized by treatment of Si2Cl6 with Cs[OSO2CH3] in the presence of 18-crown-6. Compound 1 is the first example of a λ6Si-silicate with a methanesulfonate ligand. It was characterized by NMR spectroscopy and by single-crystal X-ray diffraction. The solid-state structure of 1 consists of discrete [Si(OSO2CH3)6]2– anions and two [Cs(18-crown-6)]+ cations (triclinic space group, P1¯, Z = 1).

Keywords: cesium; hexachlorodisilane; methanesulfonate; silicate; X-ray structure analysis

1 Introduction

Over the past decades the reactivity of Si2Cl6 has been widely investigated [1], [2], [3], [4], [5], [6], [7]. We have also contributed to this field of chemistry by exploring the chemical behavior of Si2Cl6·TMEDA [8]. When Si2Cl6 was treated with the bidentate ligand TMEDA at room-temperature, a complex with both a four- and six-coordinate silicon center was formed (Figure 1). This TMEDA complex was identified by solid-state 29Si NMR spectroscopy and single crystal X-ray diffraction. Our investigations have shown that in methyl-ene chloride at room temperature a disproportionation reaction of Si2Cl6 ⋅ TMEDA takes place to give chloride-complexed, perchlorinated Si6-ring compounds (chloro-silicates e.g. [Si6Cl12·2Cl]2–; for structural studies see Ref. [9]).[1] It is also worth mentioning that thermolysis of Si2Cl6·TMEDA in the presence of THF yielded the 1:1 adduct of SiCl4 with TMEDA (Figure 1) [8].

Figure 1: Hypervalent TMEDA complexes SiCl4 ⋅ TMEDA and Si2Cl6·TMEDA both with six-coordinate Si centers [8].
Figure 1:

Hypervalent TMEDA complexes SiCl4 ⋅ TMEDA and Si2Cl6·TMEDA both with six-coordinate Si centers [8].

In 1986, the first λ6Si-silicate ([Si(NCS)6]2– with pseudo-halogenide ligands was reported by Nagorsen et al. [14]. Since then, several crystal structures of this type of silicates have been described [15], [16], [17], [18], [19]. Our approach to gain λ6Si-silicates was the disproportionation of Si2Cl6 in the presence of Cs[OSO2CH3]. This manuscript details the investigation which has led to an alternative access to hypervalent Si compounds. Our results achieved so far are reported herein.

2 Results and discussion

Given the interesting reactivity of Si2Cl6·TMEDA and our on-going interest in the chemistry of hypervalent silicon compounds, we have investigated the reaction of Si2Cl6 with Cs[OSO2CH3] (Scheme 1).[2] When Si2Cl6, Cs[OSO2CH3], and 18-crown-6 in methylene chloride were heated for 21 h to 50 °C, the reaction mixture became heterogeneous. The 29Si NMR spectrum of the reaction solution showed that Si2Cl6 was completely consumed, and only one new signal appeared [δ(29Si) = −216.2 ppm], which could be assigned to the λ6Si-silicate 1. Filtration and slow concentration of the filtrate resulted in deposition of crystals suitable for X-ray analysis that consist of the λ6Si-silicate 1.

Scheme 1: Synthesis of the λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6] (1) by a disproportion reaction of hexachlorodisilane in the presence of Cs[OSO2CH3] and 18-crown-6; (i) CD2Cl2, 50 °C, 21 h; –Cs+, –Cl–, –[SiCl2].
Scheme 1:

Synthesis of the λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6] (1) by a disproportion reaction of hexachlorodisilane in the presence of Cs[OSO2CH3] and 18-crown-6; (i) CD2Cl2, 50 °C, 21 h; –Cs+, –Cl–, –[SiCl2].

The molecular structure of the λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6] (1) is shown in Figures 2 and 3. Selected bond lengths and angles are listed in the caption of Figure 2; crystal data and refinement details are given in Table 1. The λ6Si-silicate 1 crystallizes in the triclinic space group P1¯ with Z = 1. The Si atom in 1 is located on a crystallographic center of inversion. Thus, there is just half a molecule in the asymmetric unit featuring a centrosymmetric binuclear Cs complex. The general structure motive of the λ6Si-silicate 1 features one [Si(OSO2CH3)6]2– anion in which the central Si atom is hexa-coordinated in an octahedral fashion by six methanesulfonate ligands and two [Cs(18-crown-6)]+ cations (Figure 2). Each Cs atom interacts with three of the six O atoms of one 18-crown-6 ether. The remaining coordination sites of the Cs+ cations are occupied by the O atoms of three methanesulfonate ligands of the [Si(OSO2CH3)6]2– anion. These methanesulfonate ligands bind to the central Si atom. The Si–O distances in the [Si(OSO2CH3)6]2– anion are almost identical. They range from 1.7630(15) Å for Si(1)–O(21) to 1.7721(15) Å for Si(1)–O(31). The O–Si–O angles are either exactly 180° (due to the imposed symmetry) or very close to 90°. The value with largest deviation from an rectangular angle is 91.36(7)° for O(21)–Si(1)–O(11). The Cs–O distances between the Cs+ cation and the 18-crown-6 ether show quite a wide range, i.e. from 3.0684(18) Å for Cs(1)–O(6) to 3.1909(19) Å for Cs(1)–O(1). These distances can be divided in two groups: Cs(1)–O(6) (3.0684(18) Å), Cs(1)–O(2) (3.0845(19) Å) and Cs(1)–O(4) (3.0904(19) Å) are significantly shorter than Cs(1)–O(3) (3.1558(18) Å), Cs(1)–O(5) (3.1636(18) Å) and Cs(1)–O(1) (3.1909(19) Å). This difference can be explained by the conformation of the 18-crown-6 ring. If the best plane is calculated through the six O atoms, the atoms O(2), O(4), and O(6) are on the same side as the Cs+ cation. The remaining O atoms are located on the opposite side of this plane and are therefore farther away from the Cs+ cation. The Cs–O distances between the Cs+ cation and the methanesulfonate ligands show one short value 3.0586(18) Å for Cs(1)–O(12) and two long ones [3.1715(17) Å for Cs(1)–O(22) and 3.1732(19) Å for Cs(1)–O(32)]. The bonds S(1)–O(12/13), S(2)–O(22/23) and S(3)–O(32/33) (mean value 1.432 Å) can be regarded as S=O double bonds whereas the distances of S–O(Si) (mean value: 1.521 Å) are in the range of S–O single bonds. All six methyl groups of the methanesulfonate ligands are aligned in the same orientational sense. When looking along the Cs–Si–Cs axis all S–Me vectors are orientated clockwise (or counter-clockwise depending on the viewing direction).

Figure 2: Molecular structure of λ6Si-silicate 1. Hydrogen atoms are omitted for clarity. Selected bond lengths (Å), and bond angles (deg): Cs(1)–O(1) 3.1909(19), Cs(1)–O(2) 3.0845(19), Cs(1)–O(3) 3.1558(18), Cs(1)–O(4) 3.0904(19), Cs(1)–O(5) 3.1636(18), Cs(1)–O(6) 3.0684(18), Cs(1)–O(12) 3.0586(18), Cs(1)–O(22) 3.1715(17), Cs(1)–O(32) 3.1732(19), Si(1)–O(11) 1.7689(14), Si(1)–O(21) 1.7630(15), Si(1)–O(21)#1 1.7630(15), Si(1)–O(31) 1.7721(15), S(1)–O(11) 1.5150(15), S(1)–O(12) 1.4298(19), S(1)–O(13) 1.4331(18), S(2)–O(21) 1.5245(15), S(2)–O(22) 1.4376(18), S(2)–O(23) 1.4286(17), S(3)–O(31) 1.5238(15), S(3)–O(32) 1.4294(18), S(3)–O(33) 1.4330(18), S(1)–C(1S) 1.749(3), S(2)–C(2S) 1.760(2), S(3)–C(3S) 1.759(2); O(11)–Si(1)–O(31) 91.35(7), O(11)–Si(1)–O(11)#1 180.0, O(11)–Si(1)–O(31)#1 88.65(7), O(11)#1–Si(1)–O(31) 88.65(7), O(11)#1–Si(1)–O(31)#1 91.35(7), O(12)–S(1)–O(11) 111.95(9), O(12)–S(1)–O(13) 116.09(12), O(13)–S(1)–O(11) 107.01(10), O(21)–Si(1)–O(11) 91.36(7), O(21)–Si(1)–O(31) 89.62(7), O(21)–Si(1)–O(11)# 1 88.64(7), O(21)–Si(1)–O(21)#1 180.0, O(21)–Si(1)–O(31)#1 90.38(7), O(21)#1–Si(1)–O(11) 88.63(7), O(21)#1–Si(1)–O(31) 90.38(7), O(21)#1–Si(1)–O(11)#1 91.36(7), O(21)#1–Si(1)–O(31)#1 89.62(7), O(31)–Si(1)–O(31)#1 180, O(11)–S(1)–C(1S) 103.95(11), O(12)–S(1)–C(1S) 108.58(13), O(13)–S(1)–C(1S) 108.53(13), S(1)–O(11)–Si(1) 145.25(10), S(2)–O(21)–Si(1) 139.77(10), S(1)–O(12)–Cs(1) 151.99(12), S(2)–O(22)–Cs(1) 121.44(9), O(22)–S(2)–O(21) 106.06(9), O(23)–S(2)–O(21) 112.03(10), O(23)–S(2)–O(22) 116.78(11), O(32)–S(3)–O(31) 109.81(10), O(32)–S(3)–O(33) 116.41(12), O(33)–S(3)–O(31) 106.80(10), O(21)–S(2)–C(2S) 104.36(10), O(22)–S(2)–C(2S) 107.40(12), O(23)–S(2)–C(2S) 109.39(12), O(31)–S(3)–C(3S) 107.54(10), O(32)–S(3)–C(3S) 108.07(13), O(33)–S(3)–C(3S) 107.88(12). Symmetry-equivalent atoms (#1) were generated by applying the symmetry operator –x, –y + 2, –z + 2.
Figure 2:

Molecular structure of λ6Si-silicate 1. Hydrogen atoms are omitted for clarity. Selected bond lengths (Å), and bond angles (deg): Cs(1)–O(1) 3.1909(19), Cs(1)–O(2) 3.0845(19), Cs(1)–O(3) 3.1558(18), Cs(1)–O(4) 3.0904(19), Cs(1)–O(5) 3.1636(18), Cs(1)–O(6) 3.0684(18), Cs(1)–O(12) 3.0586(18), Cs(1)–O(22) 3.1715(17), Cs(1)–O(32) 3.1732(19), Si(1)–O(11) 1.7689(14), Si(1)–O(21) 1.7630(15), Si(1)–O(21)#1 1.7630(15), Si(1)–O(31) 1.7721(15), S(1)–O(11) 1.5150(15), S(1)–O(12) 1.4298(19), S(1)–O(13) 1.4331(18), S(2)–O(21) 1.5245(15), S(2)–O(22) 1.4376(18), S(2)–O(23) 1.4286(17), S(3)–O(31) 1.5238(15), S(3)–O(32) 1.4294(18), S(3)–O(33) 1.4330(18), S(1)–C(1S) 1.749(3), S(2)–C(2S) 1.760(2), S(3)–C(3S) 1.759(2); O(11)–Si(1)–O(31) 91.35(7), O(11)–Si(1)–O(11)#1 180.0, O(11)–Si(1)–O(31)#1 88.65(7), O(11)#1–Si(1)–O(31) 88.65(7), O(11)#1–Si(1)–O(31)#1 91.35(7), O(12)–S(1)–O(11) 111.95(9), O(12)–S(1)–O(13) 116.09(12), O(13)–S(1)–O(11) 107.01(10), O(21)–Si(1)–O(11) 91.36(7), O(21)–Si(1)–O(31) 89.62(7), O(21)–Si(1)–O(11)# 1 88.64(7), O(21)–Si(1)–O(21)#1 180.0, O(21)–Si(1)–O(31)#1 90.38(7), O(21)#1–Si(1)–O(11) 88.63(7), O(21)#1–Si(1)–O(31) 90.38(7), O(21)#1–Si(1)–O(11)#1 91.36(7), O(21)#1–Si(1)–O(31)#1 89.62(7), O(31)–Si(1)–O(31)#1 180, O(11)–S(1)–C(1S) 103.95(11), O(12)–S(1)–C(1S) 108.58(13), O(13)–S(1)–C(1S) 108.53(13), S(1)–O(11)–Si(1) 145.25(10), S(2)–O(21)–Si(1) 139.77(10), S(1)–O(12)–Cs(1) 151.99(12), S(2)–O(22)–Cs(1) 121.44(9), O(22)–S(2)–O(21) 106.06(9), O(23)–S(2)–O(21) 112.03(10), O(23)–S(2)–O(22) 116.78(11), O(32)–S(3)–O(31) 109.81(10), O(32)–S(3)–O(33) 116.41(12), O(33)–S(3)–O(31) 106.80(10), O(21)–S(2)–C(2S) 104.36(10), O(22)–S(2)–C(2S) 107.40(12), O(23)–S(2)–C(2S) 109.39(12), O(31)–S(3)–C(3S) 107.54(10), O(32)–S(3)–C(3S) 108.07(13), O(33)–S(3)–C(3S) 107.88(12). Symmetry-equivalent atoms (#1) were generated by applying the symmetry operator –x, –y + 2, –z + 2.

Figure 3: Packing diagram of the λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6] (1) in the crystal.
Figure 3:

Packing diagram of the λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6] (1) in the crystal.

Table 1:

Crystal data and refinement of Cs(18-crown-6)]2[Si(OSO2CH3)6] (1).

Cs(18-crown-6)]2[Si(OSO2CH3)6] (1)
FormulaC30H66Cs2O30S6Si
Mr1393.09
Crystal size, mm30.18 × 0.09 × 0.03
Crystal systemtriclinic
Space groupP1¯
a, Å10.6970(5)
b, Å11.1751(6)
c, Å11.8019(6)
α, deg86.799(4)
β, deg79.962(4)
γ, deg79.456(4)
V, Å31365.33(12)
Z1
Dcalcd., g cm−31.69
μ(MoKα), mm−11.7
F(000), e706
hkl range±12; ±13; ±14
((sinθ)/λ)max, Å−10.595
Refl. measured12809
Refl. unique4806
Rint0.0169
Param. refined313
R1/wR2 (all data)a,b0.0245/0.0538
Weight: a/bb0.0292/0.9336
GoF c1.062
Δρfin (max/min), e Å−31.20/−0.41

  1. aR1 = Σ││Fo│–│Fc││/Σ│Fo│. bwR2 = {Σ[w(Fo2 – Fc2)2]/Σ[w(Fo2)2]}0.5; w = 1/[σ2(Fo2) + (aP2) + bP]; P = [2Fc2 + max (Fo2, 0)]/3. cGoF = {Σ[w(Fo2 – Fc2)2]/(nobs – nparam)}0.5.

In summary, a process for the generation of the new λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6] (1) was achieved by the reaction of Si2Cl6 with Cs[OSO2CH3] in the presence of 18-crown-6. Compound 1 is the first example of a λ6Si-silicate with a methanesulfonate ligand. It has been characterized by NMR spectroscopy and by single-crystal X-ray diffraction. The solid-state structure of 1 consists of one discrete [Si(OSO2CH3)6]2– dianion and two [Cs(18-crown-6)]+ cations.

3 Experimental section

All reactions and manipulations were carried out under dry, oxygen-free nitrogen or argon by using standard Schlenk ware or an argon-filled M. Braun glovebox. CH2Cl2 was dried over CaH2 and freshly distilled prior to use; CD2Cl2 was stored over molecular sieves (4 Å). The commercially available compounds Cs[OSO2Me] (Sigma Aldrich) and 18-crown-6 (Sigma Aldrich) were used as received. The NMR spectra were recorded on Bruker Avance 300 and Avance 500 spectrometers.

3.1 Synthesis of the λ6Si-Silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6]

In a glove box, neat Si2Cl6 (0.046 g, 0.171 mmol) was added via syringe dropwise at room temperature to an NMR tube charged with Cs[OSO2Me] (0.204 g, 0.895 mmol), 18-crown-6 (0.080 g, 0.303 mmol) and CD2Cl2 (0.5 mL). The tube was flame-sealed under vacuum and heated to 50 °C for 21 h. NMR-spectroscopic investigation of the supernatant, colorless solution revealed the exclusive formation of 1. The NMR tube was opened inside the glove box and the reaction mixture was filtered to get rid of the insoluble byproducts. The solvent was removed from the filtrate by slow evaporation. Recrystallization from CH2Cl2 yielded 1 as colorless crystals. Yield: 0.080 g (0.057 mmol, 38%). –1H NMR (500.2 MHz, CD2Cl2, T = 298 K): δ = 3.58 (s, 48 H, 24 × CH2 (18-crown-6)), 3.03 (s, 18H, 6 × CH3). –13C{1H} NMR (125.8 MHz, CD2Cl2, T = 298 K): δ = 70.1 (CH2, 18-crown-6), 39.7 (CH3). –29Si NMR (99.4 MHz, CD2Cl2, T = 298 K): δ = −216.2 (Figure 4).

Figure 4: 29Si NMR (99.4 MHz) spectrum of the λ6Si-silicate 1 in CD2Cl2 at T = 298 K.
Figure 4:

29Si NMR (99.4 MHz) spectrum of the λ6Si-silicate 1 in CD2Cl2 at T = 298 K.

3.2 Crystal structure determination

Data was collected on a STOE IPDS II two-circle diffractometer with a Genix Microfocus tube with mirror optics using MoKα radiation (λ = 0.71073 Å). The data was scaled using the frame scaling procedure in the X-Area program system [24]. The structure was solved by Direct Methods using the program Shelxs [25] and refined against F2 with full-matrix least-squares techniques using the program Shelxl [25, 26]. H atoms were found in a difference map, and refined using a riding model with Cmethylene–H = 0.99 Å or Cmethyl–H = 0.98 Å and U(H) set to 1.2Ueq(C) for methylene H or U(H) = 1.5Ueq(C) for methyl groups.

CCDC 1984036 {[Cs(18-crown-6)]2[Si(OSO2CH3)6] (1)} contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre viawww.ccdc.cam.ac.uk/data_request/cif.

Corresponding author: Hans-Wolfram Lerner, Institut für Anorganische Chemie, Goethe-Universität Frankfurt, Max-von-Laue-Straße 7, 60438Frankfurt am Main, Germany, E-mail:

Funding source: Evonik Stiftung

Acknowledgments

The authors are grateful to the Evonik Operations GmbH, Rheinfelden (Germany), for the generous donation of Si2Cl6. I.G. wishes to thank the Evonik Foundation for a Ph.D. grant.

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: None declared.

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2021-05-25
Accepted: 2021-06-07
Published Online: 2021-06-18
Published in Print: 2021-07-27

© 2021 Walter de Gruyter GmbH, Berlin/Boston

Articles in the same Issue

  1. Frontmatter
  2. In this issue
  3. Research Articles
  4. Synthesis and structure of the λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6]
  5. Approximate estimation of the critical diameter in Koenen tests
  6. Laves phases forming in the system ScCo2-“InCo2”-TaCo2
  7. Magnesium intermetallics: synthesis and structure of Eu2Pt2Mg and Sr2Pt2Mg
  8. Intermetallic phases in the Sc–Ir–In system – synthesis and structure of Sc1.024Ir2In0.976 and Sc3Ir1.467In4
  9. Crystal structure and physical properties of a new two-dimensional zinc coordination polymer based on 1,4-bis(4-(imidazole-1-yl)benzyl)piperazine and benzophenone-2,4′-dicarboxylate ligands
  10. A new N-oxide benzylisoquinoline alkaloid isolated from the leaves of atemoya (Annona cherimola × Annona squamosa)
  11. One-pot synthesis of 1-(benzothiazolylamino)aryl methyl-2-naphthols and 3-benzothiazolyl 2,3-dihydroquinazolinones using a magnetically recoverable core–shell nanocomposite as catalyst
  12. An efficient click synthesis of chalcones derivatized with two 1-(2-quinolon-4-yl)-1,2,3-triazoles
  13. Facile decoration of CdS nanoparticles on TiO2: robust photocatalytic activity under LED illumination
  14. Book Review
  15. A. Sigel, E. Freisinger and R. K. O. Sigel (Editors and Series Editors): Metal Ions in Bio-Imaging Techniques: Volume 22 of the series Metal Ions in Life Sciences
https://doi.org/10.1515/znb-2021-0068
Keywords for this article
cesium; hexachlorodisilane; methanesulfonate; silicate; X-ray structure analysis

Articles in the same Issue

  1. Frontmatter
  2. In this issue
  3. Research Articles
  4. Synthesis and structure of the λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6]
  5. Approximate estimation of the critical diameter in Koenen tests
  6. Laves phases forming in the system ScCo2-“InCo2”-TaCo2
  7. Magnesium intermetallics: synthesis and structure of Eu2Pt2Mg and Sr2Pt2Mg
  8. Intermetallic phases in the Sc–Ir–In system – synthesis and structure of Sc1.024Ir2In0.976 and Sc3Ir1.467In4
  9. Crystal structure and physical properties of a new two-dimensional zinc coordination polymer based on 1,4-bis(4-(imidazole-1-yl)benzyl)piperazine and benzophenone-2,4′-dicarboxylate ligands
  10. A new N-oxide benzylisoquinoline alkaloid isolated from the leaves of atemoya (Annona cherimola × Annona squamosa)
  11. One-pot synthesis of 1-(benzothiazolylamino)aryl methyl-2-naphthols and 3-benzothiazolyl 2,3-dihydroquinazolinones using a magnetically recoverable core–shell nanocomposite as catalyst
  12. An efficient click synthesis of chalcones derivatized with two 1-(2-quinolon-4-yl)-1,2,3-triazoles
  13. Facile decoration of CdS nanoparticles on TiO2: robust photocatalytic activity under LED illumination
  14. Book Review
  15. A. Sigel, E. Freisinger and R. K. O. Sigel (Editors and Series Editors): Metal Ions in Bio-Imaging Techniques: Volume 22 of the series Metal Ions in Life Sciences
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