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  • X-ray crystal structure  (2)
  • 1,1-dicyanoethene-2,2-dithiolate (i-mnt)  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Gemischtligand-Komplexe des Rheniums. IV. Die Reaktion von [ReNCl2(Me2PhP)3] mit Dithiocarbamaten. Kristallstrukturen von trans-Chloro-dimethyldithiocarbamato-bis(dimethylphenylphosphan) nitridorhenium(V), [ReN(Cl)(Me2PhP)2(Me2dtc)], und Bis(diethyldithiocarbamato)(dimethylphenylphosphan)nitridorhenium(V), [ReN(Me2PhP)(Et2dtc)2] (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1443-1448 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium complexes ; Nitrido compounds ; Mixed-ligand complexes ; X-ray crystal structure ; Ligand exchange ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mixed-Ligand Complexes of Rhenium IV. The Reaction of [ReNCl2(Me2PhP)3] with Dithiocarbamates. X-Ray Crystal Structures of trans-Chloro-dimethyldithiocarbamato-bis(dimethylphenylphosphine) nitridorhenium(V), [ReN(Cl)(Me2PhP)2(Me2dtc)], and Bis(diethyldithiocarbamato)(dimethylphenylphosphine)nitridorhenium(V), [ReN(Cl)(Me2PhP)(Et2dtc)2][ReNCl2(Me2PhP)3] reacts with dialkyldithiocarbamates, R2dtc-, under a stepwise ligand exchange. Final products of these reactions are the well-known [ReN(R2dtc)2] bischelates. Intermediatelly, however, complexes of the general formulae [ReN(Cl)(Me2PhP)2(R2dtc)] and [ReN(Me2PhP)(R2dtc)2] can be isolated. Representatives have been structurally characterized.[ReN(Cl)(Me2PhP)2(Me2dtc)] crystallizes monoclinic in the space group P21/c, Z = 4. The dimensions of the unit cell are a = 13.071(3); b = 11.622(1); c = 15.667(3) Å; β = 97.09(1)°. The rhenium atom has a distorted octahedral environment; the Re≡N bond length is 1.71(1) Å. The Re—Cl bond distance is markedly lengthened (2.665(2) Å) as a consequence of the strong trans labilizing influence of the coordinated nitrido ligand.[ReN(Me2PhP)(Et2dtc)2] crystallizes monoclinic in the space group P21/c, Z = 4, a = 17.262(3); b = 14.915(2); c = 9.888(2); β = 76.35(8)°. The equatorial coordination sphere is occupied by one phosphorus atom and three sulphur atoms. One of the dithiocarbamate ligands is coordinated bidentately; the second one with two distinct Re—S bond lengths. The Re—S(4) distance is 2.7983(2) Å which can be discussed as a weak interaction with the metal.
    Notes: Dichlorotris(dimethylphenylphosphan)nitridorhenium(V), [ReNCl2(Me2PhP)3], reagiert mit Dialkyldithiocarbamaten, R2dtc-, unter schrittweisem Ligandenaustausch. Als Endprodukte entstehen Komplexe der allgemeinen Formel [ReN(R2dtc)2]. Als Intermediate dieser Reaktion konnten Komplexe der Zusammensetzung [ReN(Cl)(Me2PhP)2(R2dtc)] und [ReN(Me2PhP)(R2dtc)2] isoliert und strukturell charakterisiert werden.[ReN(Cl)(Me2PhP)2(Me2dtc)] kristallisiert monoklin in der Raumgruppe P21/c, Z = 4. Die Elementarzelle hat die Abmessungen a = 13,071(3); b = 11,622(1); c = 15,667(3) Å; β = 97,09(1)°. Rhenium befindet sich in einer verzerrt oktaedrischen Koordinationsumgebung. Der Re≡N-Bindungsabstand beträgt 1,71(1) Å. Die trans-ständige Re—Cl-Bindung ist infolge des trans-Effektes des koordinierten Nitridoliganden stark aufgeweitet (2,665(2) Å).[ReN(Me2PhP)(Et2dtc)2] kristallisiert monoklin in der Raumgruppe P21/c, Z = 4, a = 17,262(3); b = 14,915(2); c = 9,888(2); β = 76,35(8)°. Die äquatoriale Koordinationssphäre ist mit einem Phosphor- und drei Schwefelatomen besetzt. Ein Dithiocarbamat-Ligand ist als „normales“ Chelat koordiniert; der andere ist mit zwei sehr unterschiedlichen Re—S-Abständen gebunden, wobei auch für das zweite Schwefelatom (Abstand Re—S(4): 2,7983(2) Å) Wechselwirkungen mit dem Metall diskutiert werden können.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200821
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  • 2
    Electronic Resource
    Electronic Resource
    Neue Gemischtligandenkomplexe mit Perthiocarboxylaten (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1659-1663 
    Details
    ISSN: 0044-2313
    Keywords: O-methyl-1,1-dithiooxalate ; mixed ligand complexes ; perthio carboxylates ; xanthates ; 1,1-dicyanoethene-2,2-dithiolate (i-mnt) ; 1,2-dithiooxalat ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Mixed Ligand Complexes with Perthio CarboxylatesSolutions of O-methyl-1,1-dithiooxalate (i-dtoMe) and metal(II)-chlorides (NiII, PdII) in the molar ratio 2:1 react with equimolar amounts of homonuclear bischelates of other 1,1- and 1,2-dithio-compounds L (L = i-mnt, Etxan, dto) to mixed ligand complexes M(ptoMe)L with spontaneous convertion of the 1,1-dithiooxalate into the corresponding perthio ligand (ptoMe) by sulfur insertion. Tetraphenylphosphonium-(1,1-dicyanoethene-2,2-dithiolato)(O-methyl-1,1 -perthio-oxalato)niccolat(II), Ph4P[Ni(i-mnt)(ptoMe)], crystallizes in the monoclinic space group P21/n with a = 11.019(2) Å, b = 13.648(3) Å, c = 20.882(3) Å, β = 92.565(7)°. The formation of the perthio ligand is confirmed by 13C-NMR.
    Notes: Lösungen von O-Methyl-1,1-dithiooxalat (i-dtoMe) und Metall(II)-chloriden (NiII, PdII) im molaren Verhältnis 2:1 reagieren mit equimolaren Mengen gleichkerniger Bischelate anderer 1,1- und 1,2-Dithioverbindungen L (L = i-mnt, Etxan, dto)Abkürzungen: i-mnt: 1,1-Dicyanoethen-2,2-dithiolat Etxan: Ethylxanthogenat dto: 1,2-Dithiooxalat i-dtoMe: O-Methyl-1,1-dithiooxalat ptoMe: O-Methyl-1,1-perthiooxalat unter Ligandenaustausch zu Gemischtligandenkomplexen M(ptoMe)L bei spontaner Umwandlung des 1,1-Dithiooxalates zum entsprechenden Perthioliganden (ptoMe) durch Schwefelinsertion. Tetraphenylphosphonium (1,1-dicyanoethen-2,2-dithiolato)(O-methyl-1,1-perthiooxalato)niccolat(II), Ph4P[Ni(i-mnt)(ptoMe)], kristallisiert in der monoklinen Raumgruppe P21/n mit a = 11,019(2) Å, b = 13,648(3) Å, c = 20,882(3) Å, β = 92,565(7)°. Die Bildung des Perthioliganden konnte mittels 13C-NMR bestätigt werden.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200926
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  • 3
    Electronic Resource
    Electronic Resource
    Synthese von Nitrenkomplexen mit N-Trimethylsilylanilin. III. Charakterisierung und Kristallstruktur von [Re(NPh)(OSiMe3)Cl(NH2Ph)(py)2][ReO4] und trans-[Re2O3Cl4(py)4] (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 218-223 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium(V) complexes ; phenylnitrene complexes ; X-ray crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis of Phenylnitrene Complexes with N-Trimethylsilylaniline. III. Characterization and X-Ray Crystal Structure of [Re(NPh)(OSiMe3)Cl(NH2Ph)(py)2][ReO4] and trans-[Re2O3Cl4(py)4]The reaction of cis-[Re2O3Cl4(py)4] with N-trimethylsilylaniline yields [Re(NPh)(OSiMe3)Cl(NH2Ph)(py)2][ReO4]. It crystallizes in the triclinic space group P1 with a = 1085.0(6); b = 1185.2(6); c = 1331.4(6) pm; α = 65.91(5); β = 76.98(4); γ = 87.01(4)°, Z = 2. In the mononuclear complex cation Rev exhibits an octahedral coordination with the two pyridine molecules in cis arrangement and the trimethylsilyloxo group in trans position to the phenylnitrene ligand. The phenylnitrene ligand forms a Re≡N multiple bond and an almost linear Re≡N—Ph arrangement with Re2≡N1 = 170.6(9) pm and Re2—N1—C10 = 176.6(8)°.An isomerization of the educt cis-[Re2O3Cl4(py)4] to the corresponding trans form was observed. The trans isomer crystallizes in the monoclinic space group P21/n with a = 895.5(3); b = 2278.4(2); c = 1259.2(3) pm; β = 102.23(1)°, Z = 4. In the binuclear complex with a linear O1=Re1—O2—Re2=O3 backbone and the structural parameters: Re1—O1 = 168.5(5); Re2—O3 = 168.9(5); Re1—O2 = 193.1(4); Re2—O2 = 192.4(4) pm and Re1—O2—Re2 = 178.8(2)° the Rev atoms are octahedrally coordinated. The pyridine molecules and the Cl ligands of each Re atom are in trans arrangement.The i. r. and mass spectra of both products are discussed.
    Notes: cis-[Re2O3Cl4(py)4] reagiert mit N-Trimethylsilylanilin zu [Re(NPh)(OSiMe3)Cl(NH2Ph)(py)2][ReO4]. Es kristallisiert triklin in der Raumgruppe P1, mit a = 1085,0(6); b = 1185,2(6); c = 1331,4(6)pm; α = 65,91(5); β = 76,98(4); γ = 87,01(4)°, Z = 2. Im einkernigen Komplexkation ist Rev verzerrt oktaedrisch koordiniert; die beiden Pyridinliganden haben cis-Anordnung. Die Trimethylsilyloxogruppe befindet sich in trans-Stellung zum Phenylnitrenliganden. Letzterer weist eine lineare Bindungsfunktion Re≡N—Ph mit einem Bindungswinkel Re2—N1—C10 = 176,6(8)° und einem Abstand Re2≡N1 = 170,6(9) pm auf.Beim Edukt cis-[Re2O3Cl4(py)4] wurde eine Isomerisierung zur trans-Form beobachtet. Sie kristallisiert in der monoklinen Raumgruppe P21/n mit a = 895,5(3); b = 2278,4(2); c = 1259,2(3) pm; β = 102,23(1)°, Z = 4. Im Zweikernkomplex mit einem linearen O1=Re1—O2—Re2=O3-Gerüst und den Strukturparametern: Re1—O1 = 168,5(5); Re2—O3 = 168,9(5); Re1—O2 = 193,1(4); Re2—O2 = 192,4(4) pm und Re1—O2—Re2 = 178,8(2)° sind die Rev-Atome oktaedrisch koordiniert. Die beiden Chloratome und die Pyridinliganden nehmen jeweils eine trans-Anordnung ein.Die IR- und Massenspektren der Verbindungen werden diskutiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230136
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