Über die Chloride des zweiwertigen Molybdäns, Wolframs und Tantals. II. Mitteilung. Das 3‐Molybdän‐6‐chlorid und seine Derivate

Abstract

Das Entstehungsoptimum des „Dichlorids”︁ Mo3Cl6 aus Molybdän in einer dissoziierten Phosgenatmosphäre wurde zu 600–620° ermittelt. Phosgen konnte allerdings mit geringerem Erfolg durch Dämpfe anderer organischer Chlorverbindungen ersetzt werden.

Preparation and Spectroscopic Investigations of Mixed Octahedral Complexes and Clusters

“…For example, the chemistry of molybdenum dihalides started as early as 1826, when MoI 2 was mentioned, followed by investigations on MoCl 2 and MoBr 2 . , Further progress with respect to analytical and structural aspects was made until the early 1900s, − and then by establishing wet-chemistry techniques for these compounds − and an extension to the tantalum congeners. − Pioneering X-ray investigations − revealed as a common structural feature octahedral groups of metal atoms with short metal−metal distanceseven shorter than in the metals themselves. The two building principles of an octahedral metal core surrounded by an inner ligand sphere X i and an outer ligand sphere Y a , as in [(M 6 X i 12 )Y a 6 ] 4- for M = Nb, Ta, and in [(M 6 X i 8 ) Y a 6 ] 2- , X = halide, Y = or ≠ X, and M = Mo, W, are presented by Figure c,d.…”

“…For example, the chemistry of molybdenum dihalides started as early as 1826, when MoI 2 was mentioned, 351 followed by investigations on MoCl 2 and MoBr 2 . 352,353 Further progress with respect to analytical and structural aspects was made until the early 1900s, [354][355][356][357][358][359][360] and then by establishing wetchemistry techniques for these compounds [361][362][363][364] and an extension to the tantalum congeners. [365][366][367] Pioneering X-ray investigations [368][369][370][371] revealed as a common structural feature octahedral groups of metal atoms with short metal-metal distancesseven shorter than in the metals themselves.…”

Microwave-assisted solid-state reactions involving metal powders

“…The reaction was carried out for a total of 5 min, with occasional breaks to allow recombination of the reactants. The product was annealed for 3 h. Selected d spacings/A (relative intensity): 2.89 (6), 2.75 (loo), 2.12 (46), 1.80 (34), 1.53 (7), 1.50 (11) and 1.38 (7) [lit., 2.89 (lo), 2.75 (loo), 2.13 (40), 1.81 (50), 1.64 (20), 1.53 (lo), 1.51 (30) and 1.38 (30)].…”

Preparation of trichloride and tetrachloride of molybdenum

“…Liechti and Kempe [2] used a similar procedure and claimed to have prepared molybdenum tetrachloride by condensing the vapors resulting from the thermal decomposition of the trichloride. Michael and Murphy [3] prepared molybdenum tetrachloride and pentachloride by reacting the di- and trioxide with carbon tetrachloride at 250° C. Linder, Haller, and Helwig [4] prepared molybdenum dichloride by the reaction of molybdenum with phosgene at about 600° C. However, Biltz and Fendius [5] claimed that the tetrachloride had never been prepared. They prepared the dichloride by disproportionation of the trichloride.…”