ChemInform Abstract: The Crystal Structure of trans-1,3,5-Trichloro-1,3,5-trioxo-1λ6, 3λ6,5λ6,2,4,6-trithiatriazine (β-Sulfanuric Chloride).

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2,4-Dimethoxycarbonyl-1,1,3,3-tetrakis(dimethylamino)-1λ5,3λ5-diphosphete

1,1,3,3 - Tetrakis(dimethylamino) - 1λ⁵,3λ⁵ - diphosphete, 1 , reacts with cyanoformic acid methyl ester to form two isomers of the title compound 2 . Properties, NMR, mass, and IR spectra of 2 , as well as the molecular and crystal structure of the E isomer of 2 , are described and discussed.     

Übergangsmetall-Komplexe des 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphets

Transition Metal Complexes of 1,1,3,3-Tetrakis(dimethylamino)-1λ⁵,3λ⁵-Diphosphete 1,1,3,3-Tetrakis(dimethylamino)-1λ⁵,3aλ⁵-diphosphete, 1 , reacts with W(CO)₆ to yield the isomeric complexes {1,1,3,3-tetrakis(dimethylamino)-1λ⁵,3λ⁵-diphosphete}(pentacarbonyl)tungsten 4 and {1,1,3,3-tetrakis(dimethylamino)-1,4-dihydro-1λ⁵,3λ⁵-[1,3]diphosphetium}(pentacarbonyl)tungsten 5 . With Cr(CO)₆ the complex {1,1,3,3-tetrakis(dimethylamino)-1λ⁵,3λ⁵-diphosphete}(pentacarbonyl)chromium 6 is formed. From the reaction products of Fe₃(CO)₁₂ and Fe₂(CO)₉ with 1 the complex {1,1,3,3-tetrakis(dimethylamino)-1λ⁵,3λ⁵-diphosphete}(pentacarbonyl)iron 7 could be isolated. Properties, nmr, ir and mass spectra of the new compounds are reported. 6 and 7 were characterized by X-ray structure determinations.     

A 1,5-diaza-2,4-(λ4P+, λ6P−)-diphosphorinane

The oxidation of the 1,3-diaza-4,6-diphosphorine 1 with tetrachloroorthobenzoquinone 2 led, unexpectedly, to the formation of 1,5-dimethyl-2,2-bis(dimethyl-amino)-4,4,4,4-bis-(tetrachloro-o-phenylenedioxa)-1,5-diaza-2,4-λ⁴, λ⁶-diphosphorinane-6-one 4 , containing two phosphorus atoms of opposite formal charge and different coordination number. The X-ray crystal structure analysis of 4 revealed the presence of a six-membered ring with an unusual conformation.     

1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet als Ligand in Koordinationsverbindungen

1,1,3,3-Tetrakis(dimethylamino)-1λ⁵,3λ⁵-diphosphete as Ligand in Coordination Compounds 1,1,3,3-Tetrakis(dimethylamino)-1λ⁵,3λ⁵-diphosphete, 1 , reacts with GeCl₂ · 1,4-dioxane, SnCl₂, and (CO)₅W(Z-cyclooctene) to give the complexes {HCP[N(CH₃)₂]₂}₂ · GeCl₂, 3 , {HCP[N(CH₃)₂]₂}₂ · SnCl₂, 4 , and {HCP[N(CH₃)₂]₂}₂ · W(CO)₅, 5 , respectively. The n.m.r., mass, and i.r. spectra of the new compounds as well as the crystal and molecular structures of 3 and 4 are reported and the bonding situation in compounds 3–5 is discussed.     

Die Hydrolyse des 1, 1, 3, 3-Tetrakis(dimethylamino)-1λ5, 3λ5-diphosphets

Hydrolysis of 1,1,3,3-Tetrakis(dimethylamino)-1λ⁵, 3λ⁵ -diphosphete Hydrolysis of 1,1,3,3-Tetrakis(dimethylamino)-1λ⁵, 3λ⁵ -diphosphet ( 2 ) yields in the first step Bis(dimethylamino)phosphorylmethyliden-methyl-bis(dimethylamino)phosphorane ( 5 ). In the second step Bis(dimethylamino)phosphoryl-methyl(dimethylamino)phosphosphonylmethylen ( 6 ) is the main product of hydrolysis. In addition small amounts of methylphosphonic-bis(dimethylamide) ( 7 ) are formed. Properties, nmr and mass spectra of 5 and 6 are described, their mechanism of formation is discussed.     

1,4-Dihydro-1λ5,4λ5-[1,4]diphosphinine und ein 1,4-Dihydro-1λ3,4λ3-[1,4]diphosphinin

1,4-Dihydro-1λ⁵,4λ⁵-[1,4]diphosphinines and a 1,4-Dihydro-1λ³,4λ³-[1,4]diphosphinine Reaction of thio- or dithiocarbonic acids with ethinyl amino phosphanes leads to 1,4-dihydro-1λ⁵,4λ⁵-[1,4]diphosphinine-1,4-disulfides. By this route compounds 4, 7 , and 8 have been prepared. Desulfurization of 4 with tri-n-butylphosphane results in 1,2,4,5-tetraphenyl-1,4-dihydro-1λ³,4λ³-[1,4]-diphosphinine 5 , which can be oxidized with tert-butyl-peroxide to the corresponding dioxide, 6 . From the reaction mixture of phenyl-phenylethinyl diethylamino phosphane and thioacetamide compound 4 and the unsymmetrical 1,4-dihydro-1λ⁵,4λ⁵-[1,4]diphosphinine 9 were isolated. Properties, nmr, ir and mass spectra of all new products are reported. A mechanism for the formation of 9 is suggested. The results of the X-ray structure determination of 8 and 9 are described.     

λ3σ3P and λ5σ5P derivatives of (E)-1,2-difluoro-2-(pentafluoro-λ6-sulfanyl)ethylene and (Z)-1,2,3,3,3-pentafluoropropylene

For the first time, the (E)-1,2-difluoro-2-(pentafluoro-λ⁶-sulfanyl)ethenyl group has been bonded to λ³σ³ phosphorus using a Grignard reagent. Similar phosphorus derivatives containing the (Z)-1,2,3,3,3-pentafluoropropenyl moiety were also synthesized for comparison. In three cases, hexafluoroacetone was added to form 4,4,5,5-tetrakis(trifluoromethyl) 1,3,2λ⁵σ⁵-dioxaphospholanes. © 1997 John Wiley & Sons, Inc. Heteroatom Chem 8: 467–471, 1997     

1, 2λ5-azaphosphinines and a new 1λ5, 3λ5-. Diphosphinine

The 1,2-azaphosphinine, 9 , and the 1,3-diphosphinine, 10 , can be isolated from a mixture resulting from the reaction of 1,1,3,3-tetrakis(dimethylamino)-1λ⁵,3λ⁵-diphosphete, 1 , and ethyl isothiocyanate. The reaction of 1 with phenyl isothiocyanate yields the 1,2-azaphosphinine, 16 . Mechanisms for the formation of the compounds 9 , 10 , and 16 are suggested. The properties, the NMR, mass, and IR spectra, and the molecular and crystal structures of 9 and 10 are described and discussed.