Home Crystal structure of 1,2-bis(2,2,3,3,5,5,5-heptamethyl-1,1,4,4- tetrakis(trimethylsilyl)pentasilan-1-yl)ditellane, C38H114Si18Te2
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Crystal structure of 1,2-bis(2,2,3,3,5,5,5-heptamethyl-1,1,4,4- tetrakis(trimethylsilyl)pentasilan-1-yl)ditellane, C38H114Si18Te2

  • Fan Qi and Xu-Qiong Xiao ORCID logo EMAIL logo
Published/Copyright: May 25, 2022

Abstract

C38H114Si18Te2, triclinic, P 1 (no. 2), a = 9.0857(18) Å, b = 9.7412(19) Å, c = 24.213(5) Å, α = 94.25(3)°, β = 95.26(3)°, γ = 117.58(3)°, V = 1874.9(6) Å3, Z = 1, R gt (F) = 0.0425, wR ref (F2) = 0.1580, T = 296(2) K.

CCDC no.: 2168716

The molecular structure is shown in the figure. Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal: Green prism
Size: 0.20 × 0.15 × 0.15 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 1.09 mm−1
Diffractometer, scan mode: Bruker APEX-II, ω
θmax, completeness: 27.6°, 99%
N(hkl)measured, N(hkl)unique, Rint: 23686, 8586, 0.043
Criterion for Iobs, N(hkl)gt: Iobs > 2 σ(Iobs), 5474
N(param)refined: 281
Programs: Bruker [1, 2], SHELX [3], [4], [5]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

Atom x y z Uiso*/Ueq
Te1 0.51989 (6) −0.11837 (4) 0.52132 (2) 0.07786 (18)
Si1 0.39333 (14) −0.13595 (12) 0.61149 (4) 0.0361 (2)
Si2 0.59653 (14) 0.07771 (12) 0.67563 (4) 0.0396 (3)
Si3 0.49110 (14) 0.09054 (12) 0.76060 (4) 0.0384 (3)
Si4 0.68479 (13) 0.23052 (12) 0.84232 (4) 0.0362 (2)
Si5 0.37083 (16) −0.38183 (13) 0.62935 (5) 0.0442 (3)
Si6 0.12892 (18) −0.14708 (15) 0.58945 (6) 0.0565 (3)
Si7 0.91337 (17) 0.46644 (14) 0.82817 (5) 0.0517 (3)
Si8 0.78255 (19) 0.07550 (16) 0.88599 (5) 0.0573 (3)
Si9 0.53729 (18) 0.2943 (2) 0.90554 (6) 0.0652 (4)
C1 0.7925 (6) 0.0573 (7) 0.6821 (2) 0.0727 (15)
H1A 0.825417 0.052243 0.645788 0.109*
H1B 0.771760 −0.036541 0.697833 0.109*
H1C 0.880533 0.145816 0.706063 0.109*
C2 0.6448 (8) 0.2606 (5) 0.6435 (2) 0.0748 (17)
H2A 0.753791 0.341776 0.660051 0.112*
H2B 0.562043 0.292848 0.650018 0.112*
H2C 0.643246 0.240918 0.603944 0.112*
C3 0.3539 (7) −0.1130 (6) 0.7766 (2) 0.0683 (15)
H3A 0.304018 −0.107441 0.809395 0.102*
H3B 0.420607 −0.164650 0.783044 0.102*
H3C 0.267231 −0.170559 0.745492 0.102*
C4 0.3505 (7) 0.1826 (7) 0.7460 (2) 0.0665 (14)
H4A 0.267362 0.122793 0.714197 0.100*
H4B 0.416804 0.287569 0.738270 0.100*
H4C 0.296206 0.184100 0.778023 0.100*
C5 1.0755 (8) 0.4317 (8) 0.7984 (3) 0.100 (2)
H5A 1.177473 0.528675 0.801640 0.150*
H5B 1.037316 0.389258 0.759607 0.150*
H5C 1.095802 0.359275 0.818352 0.150*
C6 1.0144 (9) 0.6005 (7) 0.8949 (2) 0.096 (2)
H6A 1.114225 0.690250 0.888578 0.144*
H6B 1.043030 0.547036 0.922217 0.144*
H6C 0.937987 0.633366 0.908321 0.144*
C7 0.8445 (9) 0.5725 (6) 0.7798 (3) 0.0855 (18)
H7A 0.761553 0.593065 0.794919 0.128*
H7B 0.797198 0.509562 0.743956 0.128*
H7C 0.939193 0.669511 0.775533 0.128*
C8 0.9601 (8) 0.1991 (8) 0.9430 (3) 0.0892 (19)
H8A 0.938118 0.276712 0.961651 0.134*
H8B 1.062317 0.249602 0.927138 0.134*
H8C 0.971006 0.134414 0.969387 0.134*
C9 0.8613 (9) −0.0221 (8) 0.8353 (3) 0.0899 (19)
H9A 0.861671 −0.110909 0.849873 0.135*
H9B 0.973253 0.050583 0.830039 0.135*
H9C 0.789228 −0.055653 0.800040 0.135*
C10 0.6193 (11) −0.0779 (9) 0.9202 (3) 0.118 (3)
H10A 0.667830 −0.132141 0.940140 0.177*
H10B 0.529245 −0.150606 0.892177 0.177*
H10C 0.576833 −0.029901 0.945844 0.177*
C11 0.5002 (11) 0.4587 (10) 0.8850 (3) 0.116 (3)
H11A 0.433103 0.477259 0.909918 0.174*
H11B 0.442616 0.431659 0.847379 0.174*
H11C 0.605853 0.551531 0.887137 0.174*
C12 0.6573 (8) 0.3577 (9) 0.9783 (2) 0.095 (2)
H12A 0.763685 0.447950 0.978226 0.143*
H12B 0.674990 0.274373 0.990675 0.143*
H12C 0.594395 0.382969 1.003193 0.143*
C13 0.3300 (8) 0.1205 (10) 0.9096 (3) 0.106 (3)
H13A 0.276144 0.146826 0.937798 0.158*
H13B 0.347937 0.034920 0.919128 0.158*
H13C 0.260017 0.090949 0.874087 0.158*
C14 0.5039 (10) −0.3652 (7) 0.6963 (3) 0.094 (2)
H14A 0.487486 −0.467049 0.702815 0.141*
H14B 0.472324 −0.320933 0.726875 0.141*
H14C 0.619942 −0.299082 0.693490 0.141*
C15 0.4401 (9) −0.4663 (6) 0.5728 (3) 0.0810 (18)
H15A 0.559001 −0.404749 0.573654 0.121*
H15B 0.383428 −0.466417 0.537283 0.121*
H15C 0.413708 −0.571479 0.578038 0.121*
C16 0.1495 (8) −0.5224 (6) 0.6348 (3) 0.0848 (18)
H16A 0.077452 −0.525150 0.602727 0.127*
H16B 0.117872 −0.489995 0.668146 0.127*
H16C 0.139051 −0.624680 0.636488 0.127*
C17 −0.0054 (7) −0.2254 (8) 0.6452 (3) 0.0879 (19)
H17A −0.116874 −0.242975 0.632706 0.132*
H17B 0.040710 −0.151288 0.678561 0.132*
H17C −0.009128 −0.322095 0.652870 0.132*
C18 0.0234 (10) −0.2761 (8) 0.5224 (3) 0.110 (3)
H18A −0.017830 −0.383180 0.528627 0.164*
H18B 0.102046 −0.251896 0.496126 0.164*
H18C −0.068577 −0.260256 0.507848 0.164*
C19 0.1500 (8) 0.0513 (6) 0.5818 (2) 0.0709 (15)
H19A 0.226487 0.098778 0.555776 0.106*
H19B 0.191965 0.115409 0.617531 0.106*
H19C 0.042237 0.041054 0.568315 0.106*

Source of material

In a representative experiment, the mixture of 1,1,1,3,3,4,4,6,6,6-decamethyl -2,2,5,5-tetrakis(trimethylsilyl)hexasilane [69] (2.00 g, 3.3 mmol) and potassium tert-butoxide (0.37 g, 3.3 mmol) was refluxed in 10 mL THF for 6 h to afford the anions of the aforementioned hexasilane starting material. After removal of the solvent in a vacuum, 10 mL toluene and tellurium (0.50 g, 7.9 mmol) were added, stirred for 3 h and refluxed overnight. Then the solvent was removed and n-hexane was added to extract the residue, which was purified by column chromatography. Green crystals were obtained by cooling the hexane solution of the title compound.

Experimental details

A suitable crystal was selected and mounted onto the tip of a glass fibre. The diffraction data were collected on a Bruker Apex II CCD diffractometer at 296 K. An empirical (multi-scan) absorption correction was applied with the program SADABS [4]. The structure was solved with the ShelXT structure solution program and subsequently refined on F2 (SHELXL-2018) [5]. Coordinates Hydrogen atoms were refined with constraints or restraints. Their Uiso values were set to 1.2 Ueq of the parent atoms. Figures of the solid-state molecular structures were generated using XP as implemented in Shelxtl program [2].

Comment

Silyl anions are important reactive intermediates not only in organic synthesis but also in organosilicon chemistry [68]. only a few studies have concentrated on its reaction with chalcogenic elements. On the other hand, disilylchalcogenides such as (Me3Si)2E (E = S, Se, Te) have been used as chalcogen transfer reagents in the preparation of nanosized copper chalcogenide clusters. The synthetic routes towards disilylchalcogenides have been developed. However, these routes utilize the unpleasant H2S or need in situ synthesis of Na2Se or Li2Te. We have reported the reaction of disilyl dianions with chalcogenide elements and obtained a series of cyclic disilyl-chalcogenides. In the course of our investigations, the titled compound was obtained.

The title compound crystallizes in the triclinic space group P 1 . The main chain of the molecules is of zig-zag type. The Te–Te bond distance is 2.7518(9) Å. The Te–Si bond length is 2.5400(12) Å. The bond lengths of Si–Si bonds in the title compound range from 2.344 to 2.384 Å, with the average bond length of 2.362 Å, which are comparable with those of the oligosilanes or polysilanes [911]. The average Si–C distance of the Si–C bonds is 1.871 Å. The bond angle of Si(1)–Te(1)–Te(1A) is 102.04(4)°. The Si–Si–Si bond angle range from 97.4° to 118.5°, with the average value of 109.99°. The title compound might be a good chalcogen transfer reagents.


Corresponding author: Xu-Qiong Xiao, College of Material, Chemistry and Chemical Engineering, Key Laboratory of Organosilicon Chemistry and Material Technology of Ministry of Education, Hangzhou Normal University, No. 2318 Yuhangtang Rd., Hangzhou 311121, Zhejiang, China, E-mail:

Award Identifier / Grant number: LY22B010002

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

  2. Research funding: This work was funded by Natural Science Foundation of Zhejiang Province (Grant No. LY22B010002).

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

References

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Received: 2022-04-26
Accepted: 2022-05-12
Published Online: 2022-05-25
Published in Print: 2022-08-26

© 2022 Fan Qi and Xu-Qiong Xiao, published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  64. Crystal structure of (Z)-3-((tert-butylamino) methylene)-2-(2-hydroxynaphthalen-1-yl) chroman-4-one, C24H23NO3
  65. Synthesis and crystal structure of (E)-1-(4-(((E)-3-(tert-butyl)-2-hydroxybenzylidene)amino)phenyl)ethan-1-one O-ethyl oxime, C21H26N2O2
  66. Crystal structure of the double salt bis(5-amino-1,2,4-triazol-4-ium-3-yl)methane hydrogen oxalate hemioxalate, C8H11N8O6
  67. Hydrothermal synthesis and crystal structure of catena-poly[diaqua-bis(μ2-4-[(4-pyridinylmethyl)amino]benzoato-κ2N:O)cobalt(II)]–1,2bi(4-pyridyl)ethene–water (1/1/1), C50H50N8O8Co
  68. Crystal structure of 3-(3-bromophenyl)-1′,3′-dimethyl-2′H,3H,4H-spiro[furo[3, 2-c]chromene-2,5′-pyrimidine]-2′,4,4′,6′(1′H,3′H) tetraone, C22H15BrN2O6
  69. The crystal structure of poly[aqua-(μ2-4,4′- bis(imidazolyl)biphenyl-κ2N:N′)-(μ2-3-nitrobenzene-1,2-dicarboxylato-κ2O:O′)]copper (II) hydrate, C26H21N5O8Cu
  70. The crystal structure of bis(4-(6-carboxy-8-ethyl-3-fluoro-5-oxo-5,8-dihydro-1,8-naphthyridin-2- yl)piperazin-1-ium) adipate tetrahydrate, C36H52F2N8O14
  71. Synthesis and crystal structure of poly[aqua(μ4-(1R,2S,4R)-4-hydroxy-1-((7-hydroxy-3-(4-hydroxy-3-sulfonatophenyl)-4-oxo-4H-chromen-8-yl)methyl)pyrrolidin-1-ium-2-carboxylate-κ4O:O′:O″:O‴)sodium(I)] monohydrate, C21H22NNaO12S
  72. Crystal structure of chlorido-(η6-toluene)(2,2′-bipyridine-κ2N,N′)ruthenium(II) hexafluorophosphate, C17H16ClN2RuPF6
  73. The crystal structure of (R)-6-hydroxy-8-methoxy-3-methylisochroman-1-one, C11H12O4
  74. Crystal structure of catena-poly[(5,5,7,12,12,14-hexamethyl -1,4,8,11-tetraazacyclotetradecane- κ4N,N′,Nʺ,N‴)nickel(II)-(μ2-perchlorato-κ2O:O′)] 3,5-dicarboxybenzoate – methanol (1/2), C27H49ClN4NiO12
  75. The crystal structure of 4-(chloromethyl)benzonitrile, C8H6ClN
  76. The crystal structure of dimethylammonium 8-[(7,9-dioxo-6,10-dioxaspiro[4.5]decan-8-ylidene)methyl]-9-oxo-6,10-dioxaspiro[4.5]dec-7-en-7-olate, C19H25NO8
  77. Crystal structure of (2R,3S,4S,5R,6S)-2-(acetoxymethyl)-6-((1-acetyl-5-bromo-4-chloro-1H-indol-3-yl)oxy)tetrahydro-2H-pyran-3,4,5-triyl triacetate hemihydrate C24H25BrClNO11
  78. The crystal structure of the co-crystal tetrakis[2-(tris(4-methoxyphenyl)stannyl)ethyl]silane – tetrahydrofuran – toluene – tetrahydrofurane (1/1/1), C103H116O13SiSn4
  79. Crystal structure of methyl 3-(1,3-dioxo-1H-benzo[de]isoquinolin-2(3H)-yl)propanoate, C16H13NO4
  80. Crystal structure of ethyl (Z)-3-amino-2-cyano-3-(2-oxo-2H-chromen-3-yl)acrylate, C15H12N2O4
  81. Crystal structure of methyl 2-(1,3-dioxo-1H-benzo[de]isoquinolin-2(3H)-yl)acetate, C15H11NO4
  82. Crystal structure of catena-poly[diaqua-bis(μ2-1,3-di(1H-imidazol-1-yl)propane-κ2N:N′)cobalt(II)] tetrafluoroterephthalate, C26H28N8O6F4Co
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