Showing papers by "George M. Sheldrick published in 1992"

Synthese und Struktur von CpAlCl2-Verbindungen mit sterisch anspruchsvollen Substituenten (Cp = Me5C5, EtMe4C5)

Abstract: Synthesis and Structure of CpAlCl2 Compounds with Sterically Demanding Substituents (Cp = Me5C5, EtMe4C5)[1] The compounds Cp*AlCl2 (3) (Cp* = Me5C5) and Cp′AlCl2 (4) (Cp′ = EtMe4C5) have been prepared by the reaction of Cp*SiMe3 (1) and Cp′SiMe3 (2) with AlCl3. The single-crystal X-ray structures of 3 and 4 are reported.

Synthese und Struktur von SeSb2Cl2(NCMe3)4 — eines nur von Stickstoffatomen umgebenen Selenimids[1]

Abstract: Synthesis and Structure of SeSb2Cl2(NCMe3)4 – a Compound with a Selenium Atom Coordinated by three Nitrogen Atoms[1] Reaction of Se[NCMe3(SiMe3)]2 (2) with SbCl3 leads to the novel tricyclic compound SeSb2Cl2(NCMe3)4 (3). According to an X-ray structure analysis the six-membered SeSb2Cl2(NCMe3)3 ring in 3 is bound to the NCMe3 moiety.

Synthese und Kristallstrukturen von monomeren bis(thiophenolato)metall(II)‐Komplexen

Abstract: Natrium-2,4,6-tris(trifluormethyl)thiophenolat(NaSRf) reagiert mit MCl2 (M = Zn, Pb) im Molverhaltnis 2 : 1 zu den Bis(thiophenolato)metall(II)-Komplexen Bis[2,4,6-tris(trifluormethyl)thiophenolato]-zink 1 und Bis[2,4,6-tris(trifluormethyl)thiophenolato]blei 2. Bei der Reaktion von Mn[N(SiMe3)2]2· THF mit zwei aquivalenten 2,4,6-Tris(trifluormethyl)thiophenol (RfSH) wird Mn(SRf)2· THF 3 erhalten. Alle Verbindungen kristallisieren als THF-Addukte. Die Kristallstrukturen von Zn(SRf)2· 2 THF 1a, Pb(SRf)2· THF 2a und Mn(SRf)2· 2THF 3a werden diskutiert. Preparation and Structures of Monomeric Bis(thiophenolato)metal(II) Complexes Sodium-2,4,6-tris(trifluoromethyl)thiophenolate (NaSRf) reacts with MCl2 (M = Zn, Pb) in the molar ratio of 2:1 to form the bis(thiophenolato)metal(II)complexes bis[2,4,6-tris(trifluoromethyl)thiophenolato]zinc 1 and bis[2,4,6-tris(trifluoromethyl)thiophenolato]lead 2. Reaction of Mn[N(SiMe3)2]2· THF with two equivalents of 2,4,6-tris(trifluoromethyl)thiophenol (RfSH) forms Mn(SRf)2 · THF 3. All compounds crystallize as THF adducts. The structures of Zn(SRf)2 · 2THF 1a, Pb(SRf)2 · THF 2a and Mn(SRf)2 · 2THF 3a are discussed.

Synthesis and structure of eight-membered titanium containing siloxane rings

Abstract: The preparation by different methods of the eight-membered ring compounds (R 1 XTiOSiR 2 2 O) 2 is reported: (2: R 1 =C 5 H 5 , X=Cl, R 2 =tBu; 3: R 1 =N(SiMe 3 ) 2 , X=Cl, R 2 =tBu; 4: R 1 =C 5 Me 5 , X=Cl, R 2 =Ph; 6: R 1 =X=NEt 2 , R 2 =tBu). The six-membered ring Ph 2 SiO[OTiC 5 Me 5 (Cl)] 2 5 is formed together with 4 by the reaction of C 5 Me 5 TiCl 3 and Ph 2 Si(OLi) 2 . Compounds 2 and 4 have been characterized by X-ray structural analysis.

Reaktionen von Germylenen mit Säureaziden / Reactions of Germylenes with Acid Azides

Abstract: A, B Starting materials are the sterically hindered diazagermylenes and C o f the general formula [R (Me3Si)N]2Ge (R = o-disubstituted aryl or mesityl). A and B react with arylsulfonylazides to give the polymeric N ,N -bis(amino)-N '-sulfonylgermazane derivatives 1 and 2. With phenylazidoformiate, A, B and C yield the corresponding diamino(phenoxy)(isocyanato)- germanium (IV ) derivatives 3 -5, while with N ,N -dimethylcarbamoylazide the impure diamino(dimethylamino)(isocyanato)germanium (IV ) com pound 6 is formed. Reactions of A and B with O ,O -diphenyl-phosphorylazide afford the eight-membered (GeNPO)2 ring compounds 7 and 8. The substances are characterized by C, H , N analyses, 1 - 8 by their mass spectra, and 3 - 8 by NMR ( 1H, l3C, 29Si, 31P). Characteristic IR group frequencies are given for the isocyanato compounds 3 - 6 . Single crystal X -ray structure analyses are reported for C, 4, 5 and 8 .

Manganese(II) Amides: The Synthesis and X-Ray Crystal Structures of Mn[N(SiMe3)(2,6-Pri2C6H3)]2[THF] and Mn3[N(H)2,6-Pri2C6H3]4[N(SiMe3)2]2

Abstract: A series of manganese(II) am ides (1-4), derived from 2,6-diisopropylaniline (H2NAr; where Ar = 2,6-Pri2C6H3) and its N-silylated derivative H(SiMe3)NAr, has been prepared and characterized. The crystal structure of Mn[N(SiMe3)Ar]2[THF] (2) reveals a monomeric species with a planar three-coordinate Mn(II) center. Crystal data for 2: trigonal (hexagonal axes), a = 30.119(2) Å, c = 10.589(1) Å, V = 8319(1) Å3, T = 153 K, space group P31 (No. 144), Z = 9 (R/Rw = 0.053/0.050). In contrast, Mn3[N(H)Ar]4[N (SiMe3)2]2 · C7H8 (4) is shown to be a novel trinuclear compound held together by nitrogen-bridges. The two terminal Mn(II) atoms have a distorted trigonal planar arrangement of nitrogen donors whereas the central Mn(II) is surrounded by a distorted tetrahedral array of nitrogen donors. Crystal data for 4: orthorhombic, a = 21.301(5) Å, b = 17.021(6) Å, c = 20.519(7) Å, V = 7439(4) Å3, T = 153 K, space group Pbcn (No. 60), Z = 4 (R/Rw = 0.050/0.070).

Enthalogenierung von Aminodihalogenboranen durch Na/K‐Legierung in Gegenwart von Naphthalin, Bis(trimethylsilyl)butadiin und 2,5‐Dimethyl‐2,4‐hexadien

Abstract: Dehalogenation of Aminodihalogenoboranes by Na/K Alloy in the Presence of Naphthalene, Bis(trimethylsilyl)butadiyne, and 2,5-Dimethyl-2,4-hexadiene Reaction of naphthalene with Na/K alloy and [(2,6-diisopropylphenyl)methylamino]difluoroborane (1) in 1,2-dimethoxyethane yields the aminodimethoxyborane 2, the bis(amino)-borane 3, the diborylethyne 4, and the diboryl oxide 5. By addition of a mixture of bis(trimethylsilyl)butadiyne or 2,5-dimethyl-2,4-hexadiene with dichloro(diisopropylamino)borane to Na/K alloy in hexane the 2,4,5-triborabicyclo-[1.1.1]pentane 7 and the diboretane 8, resp., are obtained. 1H-, 11B-, 13C-, 19F-, 29Si-NMR-, IR, and MS data are given. For 2–4, 7 and 8 X-ray structure analyses are performed.

Synthese und Kristallstruktur von l,3-Di-tert-butyl-4,4-di-methyl-2-pentafluorphenyl-4,2-stannabora-cyclobutan / Synthesis and Crystal Structure of 1,3-Di-tert-butyl-4,4-di-methyl-2-pentafluorophenyl-4,2-stannabora-cyclobutane

Abstract: The synthesis and crystal structure of 1,3-di-tert-butyl-4,4-dimethyl-2-pentafluorophenyl-1,3,4,2-diazastannoboracyclobutane are reported.

Chelation of fluoride ion by F2C(SF3)2: formation of a four-membered CS2F heterocycle with a symmetrically bridging fluoride

Abstract: In the solid state CF2(SF3)2 adds F- with formation of a stable symmetrically bridged anion F2C(µ-SF3⋯)2F1–, the structure of the caesium salt of which has been determined by X-ray crystallography.

Polycyclische Verbindungen aus 2,5-Norbornadien, Isopropylbenzol und Dehalogenierungs-Produkten von Dihalogeno(diorganylamino)boranen. Reaktion von Bis(diisopropylamino)phenylboran mit Na/K-Legierung und Difluor(diisopropylamino)boran

Abstract: Polycyclic Compounds from 2,5-Norbornadiene, Isopropylbenzene, and Dehalogenation Products of Dihalogeno(diorganylamino)boranes. Reaction of Bis(diisopropylamino)phenylborane with Na/K Alloy and Difluoro(diisopropylamino)borane In the reaction of 2,5-norbornadiene with Na/K alloy and dichloro(diisopropylamino)borane the species 1 was isolated, which contains six boron atoms in two triborolane rings. From isopropylbenzene and the dehalogenation products of (diisobutylamino)difluoroborane the ethenodiborolodiborol system 2 was isolated. When bis(diisopropylamino)phenylborane is treated with F2BN(i-C3H7)2 and Na/K alloy the diborane(4) derivative 5 and 1,1,2,2-tetrakisborylethane (6) are formed together with bis(diisopropylamino)fluoroborane (7). NMR (1, 11B, 13C, 19F) and MS data are given; for 1, 2, 5, and 6 the X-ray structure analyses were performed.

Synthese und Eigenschaften von 1,2,7,3,6-Thiadiazadiborepinen, Kristallstruktur des 2,7-Di-tert-butyl-3,6-dimethyl-3,6-dihydrobenzo-1,2,7,3,6-thiadiazadiborepins / Syntheses and Properties of 1,2,7,3,6-Thiadiazadiborepines, Crystal Structure of 2,7-Di-tert-butyl-3,6-dimethyl-3,6-dihydrobenzo-1,2,7,3,6-thiadiazadiborepin

Abstract: 2,5-Bisdimethylamino-2,5-dihydrobenzo[b]-1,2,5-thiadiborole (2) has been obtained from the diiodine-derivative by reaction with dimethyl-aminotrimethylsilane. Reaction of 2 or 2,5-bisdimethylamino-1′,2′-dimethyl-2,5-dihydrobenzo[b]-thiadiborole with di-tert-butyl-, tertbutyl-trimethylsilyl- and bistrimethylsilyl-sulfurdiimide yields the 2,7,3,6-tetrahydrobenzo[b]-1,2,7,3,6-thiadiazadiborepines (3a-3e). 1H, 11B, 13C NMR, MS and analytical data and results of analysis are given. For 3a the X-ray structure is reported.

Synthesis and X-Ray Crystal Structure of Germaimines.

Abstract: Three new germaimines have been synthesized and two of them characterized by X-ray diffraction; the GeN bond lengths agree well with an ab initio prediction for H2GeNH.