Uwe Böhme

TU Bergakademie Freiberg · Institute of Inorganic Chemistry

The title compound, [Fe(C 8 H 3 N 4 O) 2 (C 9 H 8 N 2 ) 2 ], was synthesized solvothermally. The complex exhibits a distorted octahedral coordination geometry. The Fe ²⁺ ion is located on an inversion centre. The octahedral FeN 6 coordination sphere is composed of bidentate quinoline-8-amine in the equatorial sites while the axial sites are occupie...

The literature on aluminum coordination networks so far contains data on COO-bridged derivatives exclusively. This paper addresses the question whether or not aluminum complexes, especially carbamate-bridged {Al3(μ3−O)}7+ units, can also form networks via the neutral ligand positions. Our findings show that a highly unexpected polymerization of the...

SbCl3(C9H11N3S2)2], monoclinic, P21/n (no. 14), a = 13.8069(4) Å, b = 13.5739(6) Å, c = 14.0182(5) Å, β = 94.231(3)°, V = 2,620.04(17) ų, Z = 4, R gt (F) = 0.0329, wRref(F²) = 0.0726, T = 153 K.

Hydrosilanes are highly attractive compounds, which can be processed as liquids with printing technology to amorphous silicon films on nearly any solid substrate. The silicon layers can be processed for electronic devices like transistors or thin‐film solar cells. The endothermic character of hydrosilanes with their positive enthalpies of formation...

C3H10N][C12H24BO4]·B(OH)3, orthorhombic, Fdd2 (no. 43), a = 30.3986(6) Å, b = 40.4094(13) Å, c = 7.0603(2) Å, V = 8672.8(4) ų, Z = 16, R gt (F) = 0.0324, wR ref (F ²) = 0.0828, T = 153 K.

The title SiIV complex, C16H21NO3Si, is built up by a tridentate dinegative Schiff base ligand bound to a sila­cyclo­hexane unit. The coordination geometry of the penta­coordinated SiIV atom is a distorted trigonal bipyramid. The presence of the sila­cyclo­hexane ring in the complex leads to an unusual coordination geometry of the SiIV atom with th...

C23H19NO3Si, monoclinic, P21/n (no. 14), a = 8.5543(3) Å, b = 24.0927(8) Å, c = 9.7971(4) Å, β = 113.265(3)°, V = 1854.96(12) ų, Z = 4, Rgt (F) = 0.0355, wRref (F ²) = 0.0932, T = 153 K.

The title compound was prepared by reaction of the Schiff base ligand N-(2-hydroxy-1-naphthylidene)leucine with dichlorodimethylsilane in the presence of triethylamine as base. The resulting pentacoordinate silicon complex was characterized by NMR, IR, UV-Vis spectroscopy and melting point. The structure was confirmed by single-crystal X-ray diffra...

In this work, the synthesis and structure of an antimony complex with an aromatic, asymmetric tridentate ligand without an Sb-C bond were studied. Ethoxy(2-salicylidenaminophenolato)antimony(III) was studied with NMR, UV-Vis, and IR spectroscopy and the molecular structure was determined by single crystal X-ray diffraction. The antimony atom is for...

Highlights • A novel 1D polymeric chains material (C5H6ClN2)[CdCl3H2O]. H2O perovskite was successfully synthesized. • The 3D Hirshfield surfaces and the associated 2D fingerprint plots were investigated for intermolecular interactions. • The vibrational properties using FT-IR spectroscopy, the UV-visible absorption and optical properties were stud...

We synthesized a series of new antimony(III) compounds by reaction of Sb(OEt)3 with organic ligands of the type E(CH2-CH2-OH)2, with E = NH, NMe, O, S, Se, and Te. The synthesized compounds have the general composition [E(CH2-CH2-O)2]Sb(OEt). For comparison, the compound (O-CH2-CH2-S)Sb(OEt) was prepared. All compounds are characterized using NMR,...

Triethylammonium dichloro[N-[(2-oxyphenyl)methylidene]valinato]-phenyl-tin(iv) was prepared and characterized by spectroscopic methods and single crystal X-ray crystallography. The compound consists of a triethylammonium cation and a tin complex as anion. The tin complex is composed of a tridentate O,N,O-Schiff base ligand coordinated to a SnCl2Ph...

C 29 H 25 NO 4 Si·CHCl 3 , monoclinic, P 2 1 / c (no. 14), a = 17.1316(8) Å, b = 10.1173(3) Å, c = 18.2252(8) Å, β = 117.195 ( 3 ) ° $117.195(3){}^{\circ}$ , V = 2809.7(2) Å ³ , Z = 4, R gt ( F ) = 0.0431, wR ref ( F ² ) = 0.1050, T = 153 K.

Clemens Winkler, ab 1873 Professor für anorganische Chemie an der Bergakademie Freiberg, schmolz seine Entdeckungen, darunter verschiedene Germaniumverbindungen, in Glasampullen ein. Damit begründete er die Sammlung anorganisch‐chemischer Präparate der TU Freiberg, die die Universität heute noch in der Lehre einsetzt. Jetzt wird diese Sammlung digi...

The title compound, C12H24BN, is an adduct formed from 9-borabi­cyclo­[3.3.1]nonane (9-BBN) and pyrrolidine. It crystallizes in the triclinic space group P with three mol­ecules in the asymmetric unit, one of which has disorder of the pyrrolidine ring. The B—N bond lengths are between 1.631 (2) and 1.641 (2) Å. The boron and nitro­gen atoms are bou...

The title compound, C28H23NO4Si, crystallizes in the monoclinic space group P21/c. The silicon complex consists of a tridentate dinegative Schiff base ligand bound to a di­phenyl­silyl unit. The coordination geometry of the penta­coordinate silicon atom is a distorted trigonal bipyramid.

Two polymorphs of the title compound, C20H23N3O2, have been isolated. Polymorph (I) crystallizes in the monoclinic space group P2 1/n and polymorph (II) in the tetra­gonal space group I4 1/a. The main difference between the two polymorphs on the mol­ecular level is the orientation of the n-propyl group. This group is anti­periplanar in (I) and sync...

C10H20BNO3, monoclinic, P21/c (no. 14), a = 11.0681(8) Å, b = 6.1883(3) Å, c = 18.1603(13) Å, β = 105.111(6)°, V = 1200.84(14) Å3, Z = 4, R gt(F) = 0.0338, wR ref(F 2) = 0.0861, T = 153 K.

The title compound, C22H29N3O2Si·0.5CHCl3, crystallizes in the the triclinic space group P with two host mol­ecules and one chloro­form mol­ecule in the asymmetric unit. The core of the mol­ecule consists of a urea unit bound to a 3-amino-acryloyl group. These units are almost planar in both mol­ecules [average deviation from plane of 0.05 (6) Å in...

C16H14Cl3NO3Sn·CH2Cl2, monoclinic, P21/n (no. 14), a = 11.1341(4) Å, b = 10.5867(2) Å, c = 18.6979(6) Å, β = 93.126(3)°, V = 2200.7(1) Å3, Z = 4, Rgt(F) = 0.0405, wR ref (F2) = 0.0847, T = 213 K.

Although a number of oxo-bridged trinuclear transition metal complexes have been synthesised and investigated in recent decades, comparable aluminum compounds have received much less attention. The {Al 3 (μ 3 -O)} ⁷⁺ carbamate complexes [Al 3 (μ 3 -O)(OOC-pyrr) 6 (pyrrH) 3 ] ⁺ [Cl] ⁻ ...

Despite decades of research on various carbamates and their important applications, only one aluminum N,N‐dialkylcarbamate (ADC) with an aluminum:carbamate ratio of 1 : 3 has been structurally described and comprehensively studied so far, namely tris(diisopropyl)carbamate. The reasons for this situation include problems with the used synthetic rout...

Recently several trichlorosilyl anions of main group elements have been isolated and characterized. Since 2015 anions [E(SiCl3)n]⁻, which are stabilized solely by trichlorosilyl groups, have been prepared with E=B, C, Si, Ge, P, S. These compounds have long been overlooked due to their high reactivity. This disadvantage is also an advantage, since...

The linear 1,4-bis(diphenylphosphanyl)octaphenyl-n-tetrasilane was prepared starting from chlorodiphenylphosphane and 1,4-dilithiooctaphenyl-n-tetrasilane, Li(SiPh2)4Li. The latter one was made from cyclo-(SiPh2)5 and lithium. The title compound was obtained in moderate yield and characterized by IR, Raman, UV, ³¹P, ²⁹Si, and ¹H NMR spectroscopy. T...

The 2D hybrid compound bis(2-amino-4-methoxy-6-methylpyrimidinium) bis(μ2-chloro)-tetrachloro-di-copper(II), (C6H10N3O)2Cu2Cl6, is successfully synthesized by slow solvent evaporation at room temperature. Structural properties have been investigated through single-crystal X-ray diffraction and reveal that the structure contains a centrosymmetric he...

The chemical preparation, crystal structure, spectroscopic characterization and elemental analysis of the Zn(II) complex with the tetradentate ligand N′-(pyridin-2-ylmethylene)nicotinohydrazide [Zn(C12H9N4O)H2O]ClO4 are reported. The Zn(II) cations are pentacoordinated, in a square pyramid fashion, by three nitrogen atoms from the organic ligand an...

After an introductory overview of all currently known tris(dialkylamido)alanes with the formula [Al(NR2)3]n (n = 1, 2), a simplified synthetic method based on the usage of is presented. The simplification results from the fact that the ether adduct can already be obtained during the necessary synthesis of the alane moiety and that the use of trimet...

Linear α,ω‐diphosphaoligosilanes were prepared starting from 1,5‐dilithiodecaphenyl‐n‐pentasilane, Li(SiPh2)5Li, and chlorodiorganophosphanes. The compounds 1,5‐bis(diphenylphosphanyl)decaphenyl‐n‐pentasilane, (Ph2P)Si5Ph10(PPh2), 1,5‐bis(di‐iso‐propylphosphanyl)decaphenyl‐n‐pentasilane, (iPr2P)Si5Ph10(PiPr2), and 1,4‐bis(di‐iso‐propylphosphanyl)oc...

{1-[(N,N-Dimethylammonio)methyl]ferrocen-2-yl}- 6-(p-bromophenyl)dodecamethyl-n-hexasilane picrate was synthesized from [2-(N,N-dimethylaminomethyl)ferrocenyl]lithium and 1-chloro-6-(p-bromophenyl)dodecamethyl-n-hexasilane and subsequent reaction with picric acid. The obtained product was characterized by NMR spectroscopy, mass spectroscopy, and si...

New N -silylated phthalimides, succinimides, and 1,8-napthalimides were synthesised by reactions of the alkali imides with chlorosilanes in THF. Six different mono-, di-, tri- and tetra-iminosilanes of the type (CH 3 ) 4– n Si(imide) n were obtained and the products analysed with ¹ H, ¹³ C, ²⁹ Si NMR, and Raman spectroscopy. The molecular structure...

The reaction of di­chloro­dimethyl­silane with a polydentate Schiff base ligand derived from pyridoxal and 2-ethano­lamine yielded the macrocyclic silicon compound (8E,22E)-4,4,12,18,18,26-hexa­methyl-3,5,17,19-tetra­oxa-8,13,22,27-tetra­aza-4,18-disilatri­cyclo­[22.4.0.010,15]octa­cosa-1(24),8,10,12,14,22,25,27-octa­ene-11,25-diol, C24H36N4O6Si2....

The syntheses of three different amidinosilanes of the type Me2Si[N=C(Ph)R]2 with R = pyrrolidino, morpholino, and diethylamino and one derivative with the composition R2Si[N=C(Ph)R]2 with R = morpholino are reported. These compounds were prepared in one-pot syntheses including three consecutive steps. All products are analysed by single crystal X-...

Disproportionation reactions of chlorosilane compounds in the presence of boron trichloride yield the compound H[B(SiCl3)4]. Spectroscopic analyses of the yellow‐whitish solid with IR‐, Raman‐, and NMR‐spectroscopy (²⁹Si, ¹¹B) show the presence of a highly symmetric anion containing boron, which is fourfold coordinated with silicon. Due to the high...

New cyclic and spirocyclic aminosilanes were synthesised using ethylenediamine, 2-aminobenzylamine, 1,8-diaminonaphthalene, o-phenylenediamine, and trans -cyclohexane-1,2-diamine as starting material. These diamines were converted into aminosilanes using silicon tetrachloride and dimethyldichlorosilane directly and via the N,N’ -bis(trimethylsilyla...

Cyclopentasilane (CPS) has been studied as an liquid precursor for the deposition of thin silicon films for printed electronics and related applications. The processing involves a UV‐induced prepolymerization of CPS followed by liquid deposition and low‐temperature thermolysis. An insight into the oligomer and polymer formation including crosslinki...

The title compound, C8H16N2Si, crystallizes in the the ortho­rhom­bic space group P212121 with one mol­ecule in the asymmetric unit. The Si—N bond is 1.782 (2) Å, which is substanti­ally longer than is found in comparable (3,5-di­methyl­pyrazol­yl)silanes. The tri­methyl­silyl group adopts a staggered conformation with respect to the planar 3,5-di­...

The title compound, C14H12N2O4, is nearly planar with a dihedral angle between the aromatic rings of 1.41 (8)°. The phenolic O atom is deprotonated and the N atom of the azomethine unit carries the proton, thereby forming an intra­molecular N—H⋯O hydrogen bond. In the crystal, the mol­ecules form inversion dimers via pairwise O—H⋯O hydrogen bonds.

Die Inertgastechnik ist zur sicheren Handhabung von Katalysatoren, luftempfindlichen Zwischenprodukten oder bei der Synthese metallorganischer Verbindungen unentbehrlich. Das Buch behandelt die Grundlagen der Schlenktechnik, den Aufbau einer Inertgasanlage im Labor und das Arbeiten mit der Glovebox. Weiterhin sind Arbeitsvorschriften für Beispielpr...

Abstract Trisilane, isotetrasilane, neopentasilane, and cyclohexasilane have been prepared in gram scale. In‐situ cryo crystallization of these pyrophoric liquids in sealed capillaries on the diffractometer allows access to the single crystal structures of these compounds. Structural parameters are discussed and compared to gas‐phase electron diffr...

Thiocyameluric acid C6N7S3H3, the tri‐thio analogue of cyameluric acid, is a key compound for the synthesis of new s‐heptazine (tri‐s‐triazine) derivatives. Here, two different routes for the synthesis of thiocyameluric acid and its reaction to tris(aryldithio)‐ and tris(alkyldithio)cyamelurates C6N7(SSR)3 are reported as well as transformation to...

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The heteroscorpionate ligand 2,2-bis­(3,5-di­methyl­pyrazol-1-yl)-1,1-di­phenyl­ethanol, C24H26N4O, features in the solid state an intra­molecular O—H⋯N hydrogen bond. A heteroscorpionate tungsten complex, cis-[2,2-bis­(3,5-di­methyl­pyrazol­yl)-1,1-di­phenyl­ethano­lato]chlorido­dioxidotungsten(VI) tetrahydrofuran monosolvate, [W(C24H25N4O)ClO2]·C...

A series of aliphatic and aromatic dithioethers of s-triazine and thioethers of s-heptazines were incorporated into polypropylene and their effectivity as flame retardants was analyzed using a limiting oxygen index (LOI) test, a DIN 4102-1 B2 test, thermogravimetric analyses coupled with mass spectrometry (TGA-MS) and FTIR coupled gas phase analysi...

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Lactamomethylsilanes of γ‐butyrolactam, δ‐valerolactam, ε‐caprolactam, and 1‐isoindolinone (phthalimidine) with up to three methyl moieties were synthesized according to the chemical formula MexSiLac(4–x) (x = 0, 1, 2, and 3). Using the lactams as starting materials four synthetic routes were tested: salt elimination, transsilylation, transaminatio...

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The reaction of (S)-N-[(2-hydroxynaphthalen-1-yl)methylidene]valine (H2L), 1, with organoelement halides from group 4 and 14 leads to different hypercoordinated complexes depending on the substitution of the starting material. The dianion of 1 therein acts as tridentate ligand in κ³O,N,O’ coordination mode. Complexes with silicon, germanium, tin, a...

A series of aliphatic and aromatic thioethers and dithioethers of s‐triazine were synthesized to study their thermal properties, in particular the thermally induced thiyl radical generation ability. Four symmetric s‐triazine sulfides of the type (RS)3C3N3, namely 2,4,6‐tris(phenylthio)‐ (1), 2,4,6‐tris(para‐tolylthio)‐ (3), 2,4,6‐tris(ethylthio)‐ (...

Substances like 3-aminopropyltriethoxysilane are often used as adhesive promoters in various formulations for coatings or to adjust the properties of siloxanes and other polymers. Cyclisation of similar substances is also interesting because of the formation of the Si-N bond. 1-Aza-2-silacyclopentanes were synthesised from 3-aminopropylalkoxysilane...

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Organophosphines (R2PH) and phosphineoxides (R2OPH) show a very high reactivity towards cyameluric chloride C6N7Cl3. For example, 2,4,6-trisdiphenylphosphino-tri-s-triazine (1) forms quantitatively within a few seconds. Tris-diphenylphosphinsulfide-s-heptazine (2) has been obtained by reaction of 1 with sulfur. These compounds represent a new class...

Trimethyl(N-morpholino)silane (Me3SiMorph) and dimethyl-di(N-morpholino)silane (Me2SiMorph2) were synthesised. The insertion reactions of both silanes with CO2, n-butylisocyanate (ⁿBuNCO), phenylisocyanate (PhNCO), methylisothiocyanate (MeNCS), n-butylisothiocyanate (ⁿBuNCS) and phenylisothiocyanate (PhNCS) into the Si–N-bond were investigated. One...

The aminosilanes MenSi(NRR′)4−n (n=2,3) with NRR′=ethylamino (NHEt), n-propylamino (NHⁿPr), sec-butylamino (NHsBu), n-octylamino (NHⁿOct), n-dodecylamino (NHⁿDodec), allylamino (NHAll), tert-butylamino (NHtBu), diethylamino (NEt2), and anilino (NHPh) were synthesized and their reactions with phenyl isocyanate were studied. In all cases of these sil...

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: In contrast to numerous thio- and selenocyanuric acid derivatives, no sulfur or selenium containing s-heptazines have been reported so far. We obtained thio- and selenocyameluric acid esters by substitution reactions of s-heptazine chloride C6N7Cl3 with aromatic thiols and selenophenol. The white or yellow solids are stable in air. They were comp...

The molecular structures of the transition metal cyclohexasilyl complexes M(CO)5Si6Me11 * 0.5 n-C5H12 (M = Mn, Re) were determined by single crystal X-ray diffraction. The two compounds are isomorphous. Their silicon-silicon bond lengths are compared with those of the parent cyclohexasilane and of other cyclohexasilyl complexes (comprising group 6,...

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A series of five different alkoxymethyl substituted derivatives of 8-hydroxyquinoline was synthesised both in protonated (1a-1e) and neutral (2a-2e) form. The alkoxymethyl groups are MeO (1a, 2a), EtO (1b, 2b), n-PrO (1c, 2c), iso-PrO (1d, 2d), n-BuO (1e, 2e). The compounds were characterised by single crystal X-ray diffraction and spectroscopic me...

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Review: inorganic and organometallic hypercoordinated silicon compounds

The synthesis and characterization of di- and trisiloxanes with 3,5-dimethylpyrazolyl (pz*) moieties are presented. Disiloxanes of the type O(SiMe3–npz*n)2 (n = 1, 2, and 3 in 2, 3, and 4, respectively) are easily accessible through a trans-silylation approach. Crystal structure analyses of compound 4 and the two side products 5 and 6 illustrate di...

Disproportionation reactions of Si2Cl6 in the presence of [n-Bu4N]Cl in halogenated solvents yield the compound [n Bu4N][C(SiCl3)3] (1). The X-ray structure analysis of 1 proves the existence of a planar carbanion, which is stabilized by three trichlorosilyl groups. Quantum chemical analysis shows the presence of highly polar bonds in the anion. Pl...

N-(2-hydroxy-1-naphthylidene)-l-valine 1, N-(2-hydroxy-1-naphthylidene)-l-phenylalanine 2, and N-(2-hydroxy-1-naphthylidene)-l-threonine 3 were prepared and characterized with spectroscopic methods, elemental analyses, and values of optical rotation. Compound 1 undergoes a solid state order-disorder phase transition at 231 K. The X-ray structures o...

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Dimeth­yl[N-(4-oxidopent-3-en-2-yl­idene)valinato-κ³O,N,O′]silicon(IV), C12H21NO3Si, (II), crystallizes in the ortho­rhom­bic space group P212121. The chiral compound undergoes two sharp enanti­otropic phase transitions upon cooling. The first transformation occurs at 163 K to yield a unit cell with one axis having double length. This inter­mediate...

Force field parameters for new compound classes are an important prerequisite for the fast and reliable modeling of these compounds with commercial available modeling software. The development of MMX force field parameters for aminoorganosilanes is described in this work. Combined efforts have been undertaken including synthesis, structural charact...

The assignment of atom types is one of the first steps after solving a single crystal X-ray structure analysis. It is often difficult or even impossible to assign correct atom types if there are atoms with similar atomic number present in the structure solution. The Cambridge Structural Database (CSD) allows to perform statistical analyses of bond...

C33H48F2N2O2.50Si , triclinic, P1 (No. 2), a = 14.1657(2) Å, b = 16.1074(2) Å, c = 17.1227(1) Å, α = 89.4677(5)°, β = 65.9674(5)°, γ = 79.0775(2)°, V = 3493.5 A°3, Z = 4, Rgt(F) = 0.058, wR(F2) = 0.128, T = 173 K.

The reaction of salicylaldehyde-(2-hydroxyethyl)imine (H2L), 1, with organoelement halides from group 13 and 14 leads to a variety of coordination compounds. Depending on the size of the central atom and the organic substituents, tetra-, penta- or hexacoordinated complexes emerge. When the central atom of the complex has a small atom radius and sma...

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A number of aminosilanes derived from N-methylaniline and chloroorganylsilanes were prepared and characterized. X-ray structure analysis was performed on the crystalline derivatives Ph(Cl)Si(NMePh)2 (4a), HSi(NMePh)3 (2b), MeSi(NMePh)3 (3b), and Ph2Si(NMePh)2 (6b). The compounds were comprehensively characterized by 1H, 13C, 29Si NMR, and IR spectr...