Isothiocyanato complexes of rhenium II. Synthesis, characterization and structures of ReN(NCS)2(Me2PhP)3 and Re(NS)(NCS)2(Me2PhP)3

Hübener, Rainer; Abram, Ulrich; Strähle, Joachim

doi:10.1016/0020-1693(93)03737-u

Cited by 26 publications

(8 citation statements)

References 20 publications

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“…These assignments are consistent with Nand S-bound NCSmoieties observed for other transition metal complexes. 30 The CtN stretch observed for the N-bound linkage isomers is in the range observed for other Tc [31][32][33][34][35] and Re [36][37][38][39][40][41][42][43] isothiocyanate complexes.…”

Section: Resultsmentioning

confidence: 57%

Linkage Isomerization of MSCN(CDOH)₂(CDO)BMe to MNCS(CDOH)₂(CDO)BMe (M = Tc, Re). Crystal Structures of TcNCS(CDOH)₂(CDO)BMe, ReNCS(CDOH)₂(CDO)BMe, and ReSCN(CDOH)₂(CDO)BMe

et al. 1998

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The 7-coordinate technetium(III) and rhenium(III) monocapped tris(dioxime) complexes [MX(dioxime) 3 BR] have been prepared in which the seventh ligand, X, is thiocyanate or hydroxide (M ) Tc, Re; R ) Me, Et). Both the N-and S-bound thiocyanate linkage isomers are produced during the syntheses, however, the S-bound complex isomerizes to the N-bound analogue. The synthetic routes employed allowed isolation of sufficient quantities of the technetium and rhenium S-bound isomers to be identified; however, full characterization was not possible. The linkage isomerization reaction of TcSCN(CDOH) 2 (CDO)BMe to TcNCS(CDOH) 2 (CDO)BMe was monitored in dichloromethane by UV-visible spectrophotometry, with four isosbestic points observed, consistent with the formation of a single product. The N-bound isomers for both Tc and Re, and the S-bound isomer of Re were characterized by single-crystal X-ray diffraction analysis. The two N-bound complexes were found to be isostructural. TcNCS(CDOH) 2 (CDO)BMe crystallized in the orthorhombic space group P2 1 2 1 2 1 with a ) 15.814-(2) Å, b ) 17.855(3) Å, c ) 17.997(5) Å, Z ) 8, R ) 0.054, and R W ) 0.057. ReNCS(CDOH) 2 (CDO)BMe crystallized in the orthorhombic space group P2 1 2 1 2 1 with a ) 15.795(1) Å, b ) 17.843(2) Å, c ) 18.014(3) Å, Z ) 8, R ) 0.054, and R W ) 0.073. In both cases two independent molecules per unit cell were observed. ReSCN(CDOH) 2 (CDO)BMe crystallized in the monoclinic space group P2 1 /c with a ) 10.0866(6) Å, b ) 26.301-(2) Å, c ) 12.4592(7) Å, β ) 100.5(1) deg, Z ) 4, R ) 0.100, and R W ) 0.141.

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Section: Resultsmentioning

confidence: 57%

Linkage Isomerization of MSCN(CDOH)₂(CDO)BMe to MNCS(CDOH)₂(CDO)BMe (M = Tc, Re). Crystal Structures of TcNCS(CDOH)₂(CDO)BMe, ReNCS(CDOH)₂(CDO)BMe, and ReSCN(CDOH)₂(CDO)BMe

et al. 1998

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“…This is in good agreement with the results of mass spectrometric studies on other six-co-ordinate nitrido complexes of rhenium where generally a preferred cleavage of the bond trans to the nitride ligand was observed. 14,16, 17 Crystals of [TcN(Cl)(PPhMe 2 ) 2 {N(SPPh 2 ) 2 }] suitable for X-ray crystallography were obtained from an ethanolic solution of the complex. The compound crystallizes in the triclinic space group P1 ¯ together with one molecule of the solvent ethanol.…”

Section: Resultsmentioning

confidence: 99%

Technetium(V) and rhenium(V) nitrido complexes with bis(diphenyl-thiophosphoryl)amide, N(SPPh2)2−

Abram¹,

Lang²,

Abram³

et al. 1997

J. Chem. Soc., Dalton Trans.

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“…The methyl groups of the two PMe 2 Ph ligands are diastereotopic and different chemical shifts may be expected. 21 Also for these compounds, the -CHS and -CHN protons of the thiazolic ring are shifted upfield. 12e,f These spectroscopic data, and the elemental analyses, are not sufficient to give an exact formulation for these compounds.…”

Section: Reactions Of [Re(nnc(ph)o)(pph 3 ) 2 CL 2 ] 1 and Formation ...mentioning

confidence: 95%

Synthesis, characterization, properties and structures of rhenium-(ii), -(iii), and -(v) complexes containing amino acids conjugated with a 2-aminothiazole ligand

Lazzaro¹,

Vertuani²,

Bergamini³

et al. 2002

J. Chem. Soc., Dalton Trans.

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The one-step reaction of KReO 4 with benzoylhydrazine in the presence of concentrated HCl and PPh 3 afforded [Re V (NNC(Ph)O)(PPh 3 ) 2 Cl 2 ] 1 which was converted with carbon monoxide into the dinitrogen Re() complex [ReN 2 (CO) 2 (PPh 3 ) 2 Cl] 2 in good yield. A new class of ligands, of general formula HL n (n = 1-5), was obtained by conjugation of N-protected amino acids and benzoic acid with 2-aminothiazole. Complex 2 reacted with HL n to give neutral Re() chelate complexes [Re(L n )(CO)(PPh 3 ) 2 Cl] 5-9 (n = 1-5), by substitution of N 2 and CO groups. The molecular structure of complex 9 was determined by X-ray diffraction. When reactions between [Re(NNC-(Ph)O)(PPh 3 ) 2 Cl 2 ] 1 and HL n (n = 2, 5) were carried out in different stoichiometric ratios, neutral mono-and di-substituted Re() organodiazenido complexes [Re(NNCOPh)(L 2,5 )(PPh 3 ) 2 Cl] 10, 11 and [Re(NNCOPh)(L 5 ) 2 -(PPh 3 )] 12 were obtained. In these complexes the organodiazenido Re-N-N moiety adopts a linear conformation, as has been authenticated by X-ray diffraction analysis for 11 and 12. Treatment of Re() dinitrogen precursors [ReN 2 (P) 4 Cl] (P = PMe 2 Ph, 3 and PMePh 2 , 4) with ligands resulted in interesting dinuclear oxo-(µ-oxo)-Re() species [Re 2 (O) 3 (L n ) 2 (P) 2 ] (P = PMe 2 Ph, n = 1, 13; n = 2, 14; n = 4, 15. P = PMePh 2 , n = 2, 16). Suitable crystals for an X-ray analysis have been obtained for complex 14. The structure represents one of the few cases where, for steric reasons, the Re-O-Re bridging unit is not linear but rather bent. All the compounds have been characterized by elemental analyses, IR and NMR spectroscopy. The Re() complexes 5-7 and 9 were further characterized by electrochemical measurements.

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Isothiocyanato complexes of rhenium II. Synthesis, characterization and structures of ReN(NCS)2(Me2PhP)3 and Re(NS)(NCS)2(Me2PhP)3

Cited by 26 publications

References 20 publications

Linkage Isomerization of MSCN(CDOH)₂(CDO)BMe to MNCS(CDOH)₂(CDO)BMe (M = Tc, Re). Crystal Structures of TcNCS(CDOH)₂(CDO)BMe, ReNCS(CDOH)₂(CDO)BMe, and ReSCN(CDOH)₂(CDO)BMe

Linkage Isomerization of MSCN(CDOH)₂(CDO)BMe to MNCS(CDOH)₂(CDO)BMe (M = Tc, Re). Crystal Structures of TcNCS(CDOH)₂(CDO)BMe, ReNCS(CDOH)₂(CDO)BMe, and ReSCN(CDOH)₂(CDO)BMe

Technetium(V) and rhenium(V) nitrido complexes with bis(diphenyl-thiophosphoryl)amide, N(SPPh2)2−

Synthesis, characterization, properties and structures of rhenium-(ii), -(iii), and -(v) complexes containing amino acids conjugated with a 2-aminothiazole ligand

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Isothiocyanato complexes of rhenium II. Synthesis, characterization and structures of ReN(NCS)2(Me2PhP)3 and Re(NS)(NCS)2(Me2PhP)3

Cited by 26 publications

References 20 publications

Linkage Isomerization of MSCN(CDOH)2(CDO)BMe to MNCS(CDOH)2(CDO)BMe (M = Tc, Re). Crystal Structures of TcNCS(CDOH)2(CDO)BMe, ReNCS(CDOH)2(CDO)BMe, and ReSCN(CDOH)2(CDO)BMe

Linkage Isomerization of MSCN(CDOH)2(CDO)BMe to MNCS(CDOH)2(CDO)BMe (M = Tc, Re). Crystal Structures of TcNCS(CDOH)2(CDO)BMe, ReNCS(CDOH)2(CDO)BMe, and ReSCN(CDOH)2(CDO)BMe

Technetium(V) and rhenium(V) nitrido complexes with bis(diphenyl-thiophosphoryl)amide, N(SPPh2)2−

Synthesis, characterization, properties and structures of rhenium-(ii), -(iii), and -(v) complexes containing amino acids conjugated with a 2-aminothiazole ligand

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Linkage Isomerization of MSCN(CDOH)₂(CDO)BMe to MNCS(CDOH)₂(CDO)BMe (M = Tc, Re). Crystal Structures of TcNCS(CDOH)₂(CDO)BMe, ReNCS(CDOH)₂(CDO)BMe, and ReSCN(CDOH)₂(CDO)BMe

Linkage Isomerization of MSCN(CDOH)₂(CDO)BMe to MNCS(CDOH)₂(CDO)BMe (M = Tc, Re). Crystal Structures of TcNCS(CDOH)₂(CDO)BMe, ReNCS(CDOH)₂(CDO)BMe, and ReSCN(CDOH)₂(CDO)BMe