Syntheses and Solid‐State Structures of Bis(dialkylstibanyl)sulfanes and ‐telluranes

Abstract

Distibines Sb2R4 (R = Me, Et) react with elemental chalcogenes (E = S, Se, Te) with insertion into the Sb-Sb bond and formation of the corresponding bis(dialkylstibanyl)sulfanes, -selenanes andtelluranes (R2Sb)2E. The structures of (Et2Sb)2S ( 1), (Et2Sb)2Te (3), and (Me2Sb)2Te (4) were determined by single crystal X-ray diff-raction. The complexes either adopt a syn-syn (1, 4) or syn-anti conformation (3) in the solid state. In addition, different intermolecular interactions modes were observed, depending on the bridging chalcogen and the organic substituent bound to the Sb atoms.

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“…These values are only slightly elongated compared to the sum of the covalent radii as reported by Pyykkö et al (Sb–Te 2.76 Å, Bi–Te 2.87 Å) 25. The Sb–Te bond length of 1 is comparable to those reported for bis(dialkylstibanyl)telluranes (R 2 Sb) 2 Te [R = Me 2.791(1); 2.763(1) Å; Et 2.783(1), 2.770(1) Å]11a and the telluradistibirane Bbt 2 Sb 2 Te {Bbt = 2,6‐bis[bis(trimethylsilyl)methyl]‐4‐[tris(trimethylsilyl)methyl]phenyl; Sb–Te 2.7607(7), 2.7719(6) Å} 26. The Bi–Te bond length in 2 is slightly elongated compared with the Bi–Te bond lengths as reported for [{(Me 3 Si) 2 CH} 2 Bi] 2 Te [2.872(3) Å, 2.889(2) Å],10 [{(Me 3 Si) 3 SiTe} 2 BiR] [R = CH(SiMe 3 ) 2 : 2.8378(8), 2.8617(8) Å; C(SiMe 3 ) 3 : 2.8638(11), 2.8826(14) Å],27 as well as R 2 Bi(TePh) {[R = o ‐C 6 H 4 (CH=NC 6 H 3 ( i Pr) 2 ‐2,6)] 2.9084(4) Å} and RBi(TePh) 2 [2.8949(3), 2.9545(3) Å] 16a.…”

Dispersion interactions between neighboring Bi atoms in (BiH3)2 and Te(BiR2)2

“… Syn–syn conformer of Te(SbMe 2 ) 2 (a), syn–anti conformer of Te(SbEt 2 ) 2 (b), and syn–syn conformer of Te(BiEt 2 ) 2 (c), as observed in the solid‐state structures . [Color figure can be viewed at http://wileyonlinelibrary.com]…”

“…In an extension of our preliminary work on rather strong dispersion‐dominated intermolecular Te⋯Sb and Te⋯Bi interactions in Et 2 SbTeEt and Et 2 BiTeEt (−51.6 and −65.6 kJ/mol), we synthesized and investigated compounds of the general type R 2 Sb‐E‐SbR 2 (E = S, Se, Te) . The Te‐bridged derivatives were of particular interest since they show thermochromic behavior, which most likely results from the presence of intermolecular Sb⋯Sb (3.673 Å) and Sb⋯Te contacts (3.625 Å) as observed in the solid‐state structure.…”

Synthesis of Binary Sb2E3 (E = S, Se) and Ternary Sb2(S,Se)3 Nanowires Using Tailor‐Made Single‐Source Precursors

“…(Et 2 Sb) 2 S ( 1 ) and (Et 2 Sb) 2 Se ( 2 )42 were synthesized by a slightly modified reaction as reported by Breunig et al43 and Et 3 SbS ( 3 ) and Et 3 SbSe ( 4 )39 were prepared by oxidative addition reaction of elemental sulfur and selenium to SbEt 3 ,44,45 (Scheme ).…”

“…We became interested in the development of suitable single‐source precursors for the synthesis of the corresponding binary Sb 2 E 3 materials as well as for ternary materials or heterocomposite materials by simultaneous thermolysis reactions, which require well‐balanced thermal properties of the precursors. Herein, we report on four single‐source precursors of the type (Et 2 Sb) 2 E, which was prepared by reaction of Et 4 Sb 2 38 with elemental S and Se,42 respectively, and Et 3 SbE (E = S, Se), which were successfully used for the wet‐chemical synthesis of Sb 2 S 3 and Sb 2 Se 3 nanowires at temperatures below 180 °C. The influence of the solvent (DIPB, oleylamine) and the capping agent (PVP*) on the morphology, chemical composition, and crystallinity of the resulting binary nanomaterials was investigated.…”