Cyclische Diazastannylene, XXX [1] Symmetrisch und asymmetrisch substituierte German- und Stannandiyle mit Amid-, Alkoholat- und Thiolat-Liganden, Teil I [2] / Cyclic Diazastannylenes, XXX [1] Symmetrically and Asymmetrically Substituted Germane- and Stannanediyls with Amide, Alcoholate and Thiolate Ligands, Part I [2]

1989 ◽  
Vol 44 (9) ◽  
pp. 1067-1081 ◽  
Author(s):  
M. Veith ◽  
P. Hobein ◽  
R. Rösler
Keyword(s):  
Chelate Ring ◽  
Membered Ring ◽  
Aluminium Atom ◽  
X Ray ◽  
Thiolate Ligands ◽  
Trigonal Bipyramidal ◽  
Tetrahedral Environment ◽  
Homologous Compounds ◽  
Structure Determinations ◽  
Tert Butylamine

Chelates of Ge(II) and Sn(II)Symmetrically and unsymmetrically substituted germane- and stannanediyls as well as chelated bis(amino)- or aminooxogermanium- and -tinmonohalides have been obtained from cyclic bis(amino)germane- and stannanediyls by treatment with tert-butylamine, tert-butanol and tert-butylmercaptane. The following compounds have been synthesized: GeX2 (X = OtBu (5), StBu (6)), Sn(StBu), (9), GeXCl (X = N(H)tBu (21), OtBu (22)), SnXCl (X = N(H)tBu (23), OtBu (24), StBu (25), OMe (28)) and Sn(OtBu)Br (27). In the series of the chelates Me2Si(NtBu)(NHtBu)GeCl (13), Me2Si(NtBu)(OtBu)SnX (X = Cl (18), OMe (19)) and the bischelate [Me2Si(NtBu)(OtBu)]2Sn (20) have been prepared. When 18 is allowed to react with aluminiumtrimethyl Me2Si(NtBu)(OtBu)AlClMe is formed, a compound with a center of chirality at the aluminium atom. X-ray structure determinations have been performed on single crystals of 6, 8, 9, 13, 22 and 24. 6, 8, 22 and 24 form molecular dimers with c.n. of 3 at the Ge or Sn atoms, resp. While the tBu-S ligands are syn with respect to the central Ge2S2 ring in 6 (symmetry approaching C2v), the tBu-O ligands are anti to the central Sn2O2 ring in 8 (symmetry Ci). 9 forms a coordination polymer with all Sn atoms in a Ψ-trigonal-bipyramidal and all S atoms in a Ψ-tetrahedral environment. The germanium atom in 13 is coordinated by a chlorine, a λ3- and a λ4-nitrogen atom, the two nitrogen atoms being connected by as dimethylsilyl group. The hydrogen and chlorine atom of 13 are found at the same side of the four-membered chelate ring. The two unsymmetrically substituted, homologous compounds Ge(O/tBu)Cl (22) and Sn(OtBu)Cl (24) are found to form dimers via O→Ge resp. O→Sn bonds. While the chlorine atoms in 22 are syn with respect to the four-membered ring, they are anti in the case of molecule 24.

Funktionelle Trimethylphosphanderivate, XXVI [1]. Silylsubstituierte Phosphinomethane und Lithiumphosphinomethanide / Functional Trimethylphosphine Derivatives, XXVI [1] Silyl-substituted Phosphinomethanes and Lithiumphosphinomethanides

1988 ◽  
Vol 43 (11) ◽  
pp. 1416-1426 ◽  
Author(s):  
Hans H. Karsch ◽  
Armin Appelt ◽  
Brigitte Deubelly ◽  
Karin Zellner ◽  
Jürgen Riede ◽  
...  
Keyword(s):  
Membered Ring ◽  
Marked Influence ◽  
X Ray ◽  
Phosphorus Forms ◽  
Twist Conformation ◽  
Structure Determinations

The lithium phosphinomethanides LiCH(X)(PMe2) (X = H, PMe2 SiMe3) react with Me3SiCl to give silylsubstituted phosphinomethanes CH(X)(PMe2)(SiMe3). The latter are metalated by LiR (R = tBu, nBu). This metalation is facilated by the presence of Me2NCH2CH2NMe2 (TMEDA). X-ray structure determinations of {(TMEDA)Li[CH(PMe2)(SiMe3)]}2 (3b) and (TMEDA){Li[C(PMe2)(SiMe3)2]}2 (5b) show the marked influence of increasing silyl substitution on the structures of lithium phosphinomethanides: the Li-C contacts are weakened, whereas phosphorus forms additional (bridging) Li···P contacts to the second Li atom in the dimeric arrangements. In 3b, a six-membered ring in twist conformation is formed by head-to-tail dimerization. Likewise, 5b forms a six-membered ring, in this case by head-to-head dimerization. however, which may be regarded as a complex of a chelating phosphinomethyl lithiate ligand to [(TMEDA)Li]+ .

Synthesis, Structural Characterization and Luminescence Property of Ring-Like Zinc(II) Complex of N-Paratoluensulfonyl-Glycine Acid and 1,10-Phenanthroline

2011 ◽  
Vol 321 ◽  
pp. 127-130
Author(s):  
Xi Shi Tai
Keyword(s):  
Luminescence Property ◽  
Weak Interactions ◽  
Chelate Ring ◽  
Molar Conductivity ◽  
Tridentate Ligand ◽  
Single Crystal Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

A novel ring-like zinc (II) complex of N-paratoluensulfonyl-glycine acid and 1,10-phenanthroline was synthesized and characterized by elemental analysis, IR spectrum and molar conductivity. The crystal structure of Zn (II) was determined by X-ray single crystal diffraction. The results show that each zinc (II) atoms is in a distorted trigonal bipyramidal geometry and form 16-membered chelate ring with the tridentate ligand. Intermolecular weak interactions in complex link molecules into a one-dimensional infinite chain supramolecular structure. The luminescence property of the complex was investigated in solid.

Pyridin-Borabenzol und Pyridin-2-Boranaphthalin als Liganden von Metallen der Chromgruppe / Pyridine-borabenzene and Pyridine-2-boranaphthaline as Ligands of Group 6 A Metals

1985 ◽  
Vol 40 (10) ◽  
pp. 1327-1332 ◽  
Author(s):  
Roland Boese ◽  
Norbert Finke ◽  
Thomas Keil ◽  
Peter Paetzold ◽  
Günter Schmid
Keyword(s):  
Membered Ring ◽  
X Ray ◽  
Group 6 ◽  
Structure Determinations

Pyridine-borabenzene (1) and pyridine-2-boranaphthalene (2) can be coordinated to group 6A metals M to form compounds of the type (OC)3M·1 and (OC)3M·2, respectively. X-ray structure determinations prove the ligands to be η6-bonded to the metal via the boron-containing six-membered ring.

Übergangsmetallkomplexe mit Schwefelliganden, LXXVIII. H+-, Lewis-Säure-Basen- und Ligandentransferreaktionen von Thioether-Thiolat-Nickelkomplexen. Röntgenstrukturanalysen von [Mo(O)(′OS4′ )] und [Mo(O)(′NhS4′)]/Transition Metal Complexes with Sulfur Ligands, LXXVIII. H+-, Lewis Acid-Base and Ligand Transfer Reactions of Thioether-Thiolato-Nickel Complexes. X-Ray Structure Determinations of [Mo(O)('OS4')] and [Mo(O)('NHS4')]

1992 ◽  
Vol 47 (1) ◽  
pp. 51-60 ◽  
Author(s):  
Dieter Sellmann ◽  
Stefan Fünfgelder ◽  
Falk Knoch
Keyword(s):  
Metal Complexes ◽  
Acid Methyl Ester ◽  
Transfer Reactions ◽  
Side Chain ◽  
X Ray ◽  
Thiolate Ligands ◽  
Convenient Synthesis ◽  
Structure Determinations ◽  
Ligand Transfer ◽  
Amino Propionic Acid

In order to elucidate specific properties of nickel sulfur complexes, reactions of recently synthesized [Ni('S5')], [Ni('OS4')]2, [Ni('NHS4')]2, [Ni('S4-C5')]2 and [Ni('S4-C3')] were investigated ('OS4'2- = 2,2'-bis(2-mercaptophenylthio)diethylether(2-), 'NHS4'2- = 2,2'-bis(2-mercaptophenylthio)diethylamine(2-), 'S5'2- = 2,2'-bis(2-mercaptophenylthio)diethylsulfide(2-), 'S4-C5'2- = 1,5-bis(2-mercaptophenylthio)pentane(2-), 'S4-C3'2- = 1,3-bis(2-mercaptophenylthio)propane(2-)).Reactions with proton acids, CH3COCl and cyanide led to de-coordination of the sulfur ligands, thus providing a convenient synthesis of multidentate thioether-thiolate ligands.The reactions of these Ni complexes with metal salts or metal complexes led to ligand transfer from nickel to Pd(II), Mo(IV ) and Hg(II), [Pd('S4-C3')], [Hg('S5')], [Hg('S4-C3')]. [Hg('S4-C5')], [Mo(O)('S5')], [Mo(O)('NHS4')] and [Mo(O)('OS4')] were synthesized by this method. X-ray structure analysis proved that [Mo(O)('OS4')] and [Mo(O)('NHS4')] have a pseudooctahedral Mo coordination with cis-thiolate atoms and trans-ether or amine and oxogroup donors.Template alkylation of [Fe(CO)2(S2C6H4)2]2- by 3-(N, N-bis-(2-bromoethyl)-amino)-propionic acid methyl ester leads to a multidentate ligand that contains functional groups in the side chain.

New adducts of silver(I) halides, AgX (X = Cl, Br), with bidentate phosphine ligands: syntheses and molecular structures of [Ag3(μ3-Cl)2(μ-dppm)3][PF6], [Ag3(μ3-Br)2(μ-dppm)3][AgBr2], {[Et4N][Ag2 (μ-Br)3(μ-dppe)]}n, [Et4N]2[(AgCl2)2(μ-dppe)], and [(AgCl)2(μ-dppp)2]

2017 ◽  
Vol 72 (5) ◽  
pp. 327-334
Author(s):  
Ting-Ting Qian ◽  
Yu-Feng Xie ◽  
Hua-Tian Shi ◽  
Ai-Quan Jia ◽  
Qian-Feng Zhang
Keyword(s):  
Membered Ring ◽  
Phosphine Ligands ◽  
Molecular Structures ◽  
Anionic Complex ◽  
Polymeric Complex ◽  
X Ray Diffraction ◽  
Neutral Complex ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Bidentate Phosphine

AbstractInteraction of AgCl with bis(diphenylphosphino)methane (dppm) in THF/MeCN in the presence of K[PF6] or [Et4N]Br afforded typical trinuclear cationic trigonal-bipyramidal complexes [Ag3(μ3-Cl)2(μ-dppm)3][PF6] (1) or [Ag3(μ3-Br)2(μ-dppm)3][AgBr2] (2), respectively. Treatment of AgBr with bis(diphenylphosphino)ethane (dppe) in THF/MeCN in the presence of [Et4N]Br gave a polymeric complex {[Et4N][Ag2(μ-Br)3(μ-dppe)]}n (3) with a dinuclear {Ag2(μ-Br)3} core. The reaction of AgCl with dppe or bis(diphenylphosphino)propane (dppp) in THF/MeCN in the presence of [Et4N]Cl resulted in the isolation of a dinuclear anionic complex [Et4N]2[(AgCl2)2(μ-dppe)] (4) with one μ-dppe bridge or a dinuclear neutral complex [(AgCl)2(μ-dppp)2] (5) with two μ-dppp bridges and a 12-membered ring, respectively. The structures of complexes 1–5 with the bidentate phosphine ligands were determined by single-crystal X-ray diffraction.

Synthese und Eigenschaften von Benzylgallium(indium)-Verbindungen. Die Kristallstrukturen von [(PhCH2)2GaBr]2, [(PhCH2)2GaN(H)t-Bu]2 und [PhCH2InCl2(THF)2] / Synthesis and Properties of Benzylgallium(indium) Compounds. The Crystal Structures of [(PhCH2)2GaBr]2, [(PhCH2)2GaN(H)t-Bu]2 and [PhCH2InCl2(THF)2]

1996 ◽  
Vol 51 (5) ◽  
pp. 637-645 ◽  
Author(s):  
Thomas Kräuter ◽  
Bert Werner ◽  
Bernhard Neumüller
Keyword(s):  
Solid State ◽  
Crystal Structures ◽  
Coordination Sphere ◽  
Molar Ratio ◽  
Centrosymmetric Dimer ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Redistribution Reaction ◽  
Structure Determinations ◽  
Indium Compounds

(PhCH2)2GaBr (1) can be obtained by the redistribution reaction of GaBr3 with Ga(CH2Ph)3 in a molar ratio 1:2. Treatment of 1 or (PhCH2)2GaCl with one equivalent of LiN(H)t-Bu gives the diorganogallium amide [(PhCH2)2GaN(H)t-Bu]2 (2). The toluene-insoluble PhCH2InCl2 can be structurally investigated after dissolving in THF and crystallization as [PhCH2InCl2(THF)2] (3). 1 - 3 were characterized with NMR, IR and MS techniques as well as by X-ray structure determinations. 1 forms two crystallographic independent dimers while 2 is a centrosymmetric dimer in the solid state. 3 is a monomer with a trigonal-bipyramidal coordination sphere at the indium center.

Zur Chemie der 1,3,5-Triaza-2-phosphorinan-4,6-dione. Teil IX. Umsetzungen einiger 1,3,5-Triorgano-1,3,5-triaza-2λ3-phosphorinan-4,6-dione mit Hexafluoraceton / Chemistry of the 1,3,5-Triaza-2-phosphorinan-4,6-diones. Part IX. Reaction of some 1,3,5-Triorgano-1,3,5-triaza-2λ3-phosphorinan-4,6-diones with Hexafluoroacetone

1995 ◽  
Vol 50 (12) ◽  
pp. 1785-1790 ◽  
Author(s):  
Ion Neda ◽  
Michael Farkens ◽  
Axel K. Fischer ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crystal Structure ◽  
Phosphorus Atom ◽  
Mass Spectra ◽  
Membered Ring ◽  
The Other ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Phosphoryl Compound ◽  
Spirocyclic Compounds

The reactions of 2-(2-chloroethyl)amino-1,5-dimethyl-3-phenyl-1,3,5-triaza-2λ3-phosphorinan- 4,6-dione (1), 2-bis(2-chloroethyl)amino-1,5-dimethyl-3-phenyl-1,3,5-triaza-2A3-phosphorinan- 4,6-dione (2), 2-methoxy-1,3,5-trimethyl-1,3,5-triaza-2λ3-phosphorinan-4,6-dione (3) and 2-trimethylsiloxy-1,3,5-trimethyl-1,3,5-triaza-2λ3-phosphorinan-4,6-dione (5) with hexafluoracetone are described. In the case of 2 and 3 the reaction furnished the spirocyclic compounds 7 and 8. 2-Bis(2-chloroethyl)amino-1,3,5-triphenyl-1,3,5-triaza-2λ3-phosphorinan- 4,6-dione (4) did not react. In the case of 1 and 5 rearrangement reactions took place; the (2-chloroethyl)amino substituent of 1 reacted with one of two equivalents of hexafluoroacetone with formation of the spirocyclic phosphorane 6. The reaction of 5 with tetrabromoorthobenzoquinone gave the phosphoryl compound 9. Compounds 6 - 8 were characterized via their 1H-, 13C-, 19F- and 31P-NMR and mass spectra, compound 9 via its 1H-, 13C- and 31P-NMR and mass spectra. An X-ray crystal structure determination of 8 was conducted; in the six-membered ring the phosphorus atom lies 73 pm out of the plane of the other atoms, and displays trigonal bipyramidal coordination.

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