Metallboranate und Boranatometallate. 14. Chlorid-tetrahydridoborate des Calciums und Strontiums

Metal Tetrahydridoborates and Tetrahydridoborato Metalates. 14. Chloro Tetrahydridoborates of calcium and Strontium The action of hydrogen chloride on E(BH₄)₂ (E ? Ca, Se) in a 1:1 mole ratio in tetrahydrofuran yields the title compounds isolated as their tetrahydrofuran adducts. No intermediates were detected by ¹¹B n.m.r. spectroscopy in the reaction of methanol with Ca(BH₄)₂. The final product is Ca[B(OCH₃)₄]₂ · THF.     

Boranate und Boranato-metallate. III. Boranatozinkate der Alkalimetalle

The reaction of zinc halides (ZnCl₂, ZnBr₂) or Zn(BH₄)₂ with LiBH₄ or NaBH₄ in ether or tetrahydrofurane yields LiZn(BH₄)₃, Li₂Zn(BH₄)₄ or NaZn(BH₄)₃ respectively. The latter complex is also obtained by the reaction of NaZn(OCH₃)₃ or Na₂Zn(OCH₃)₄ with diborane. Octakis(tetrahydridoborato)-trizincate K₂Zn₃(BH₄)₈ and BaZn₃(BH₄)₈ are formed by treating Zn(BH₄)₂ with KBH₄ or Ba(BH₄)₂. The ¹¹B-nmr- and ir-spectra of the new complexes are recorded and discussed in terms of double hydrogen bridge bonding of BH₄ groups to the central zinc atom.     

Metallboranate und Boranato-metallate. VI. Zur Reaction von Oniumboranaten mit Trimethylamin-Alan: Trimethylamin-boranato-alanat,BH4 · AlH3 · N(CH3) und Onium-alanate

Trimethylamine-alane adds to tetrabutylammonium tetrahydroborate in benzene to yield tetrabutylammonium trimethylamine-tetrahydroborato-trihydroaluminate. The BH₄ group of this novel complex hydrido-anion is bound via a single hydrogen bridge to the aluminium atom. Although there is ir-spectroscopic evidence for the formation of a similar tetraphenylphosphonium salt in the reaction of tetraphenylphosphonium tetra-hydroborate and trimethylamine-alane (employed in excess), the products are tetraphenylphosphonium tetrahydroaluminate and trimethylamine-tetrahydroborato-alane. However, tetraphenylarsonium tetrahydroborate yields triphenylarsine and (CH₃)₃N · AlH₂BH₄ under similar conditions. Tetrabutylammonium, tetraphenylphosphonium and tetraphenylarsonium tetrahydro-aluminates were prepared from the respective tetrahydroborate and LiAlH₄.     

Metallboranate und Boranatometallate. 13 [1]. Darstellung und Molekülstruktur von Uran(III)-tetrahydridoborat-3-Tetrahydrofuran

Metal Boranates and Boranatometallates. 13. Preparation and Molecular Structure of Uranium(III) Tetrahydridoborate-3-Tetrahydrofuran U(BH₄)₃ · 3 THF is slowly formed from UH₃ and diborane in the presence of tetrahydrofuran as a solvent. The compound crystallizes in the triclinic system, space group P1 , with distinct molecules in the unit cell. Its uranium atom is surrounded by three BH₄ and three tetrahydrofuran ligands in a distorted facial-octahedral arrangement. Uranium boron bond distances indicate that the BH₄ groups act as μ₃-H ligands.     

Die chromatographische Trennung des V von Cr und Mo

Ohne Zusammenfassung     

Die Schwingungsspektren des Chlortrimethylammonium-chlorids und -hexachloroantimonats(V)

Inhaitsübersicht. Die Schwingungsspektren von (CH₃)₃NCI₂ (I) und (CH₃)₃NCl⁺SbCI₆^– (II) wurden aufgenommen und im Hinblick auf die N—Cl-Bindungsverhältnisse diskutiert. The Vibrational Spectra of Chlorotrimethylammonium Chloride and Hexachloroantimonate(V) Abstract. The vibrational spectra of (CH₃)₃NCl₂ (I) und (CH₃)₃NCl⁺SbCl₆^– (II) are measured and discussed in view of the N-Cl bonds. Die IR-Spektren der nach [9] dargestellten Verbindungen wurden als Verreibungen in Nujol bzw. Hostaflonöl mit einem linear in Wellenzahlen registrierenden IR-Spektrophotometer PE 457 (Perkin Elmer) aufgenommen. Die Raman-Spektren wurden mit einem Coderg-Laser-Gerät PHO vermessen. Zur Anregung wurde die 4880 Å-Linie eines Argon-Gaslasers verwendet.     

Phosphan-, Phosphit- und Phosphido-Komplexe des Vanadiums(V)

Phosphane, Phosphite, Phosphido, Complexes of Vanadium(V) Complex formation of tert-butylimidovanadium(V)trichloride ( 1 ) with phosphanes und phosphites has been studied. Syntheses of phosphidovanadium(V) compounds ^tC₄H₉N?VCp(NH^tC₄H₉)[P(SiMe₃)₂] and ^tC₄H₉N?VCp(NⁱProp₂)(PR₂) (R?SiMe₃, Ph) are described starting from the corresponding chlorovanadium(V) complexes. The reaction of 1 with silver hexafluorophosphate yields a bis(fluoro)phosphidovanadium(IV complex [(μ-PF₂)₂V₂Cl₂)(N^tC₄H₉)₂]; as primary intermediate product of the unknown redox reaction a cationic vanadium(V) complex [^tC₄H₉N?VCl₂ · PPh₃]⁺PF₆^? has been isolated. 1 reacts with an excess of diisopropylamine forming ^tC₄H₉N?V(NⁱProp₂)Cl₂ ( 16 ); in addition the following diisopropylamido-tert-butylimidovanadium(V) compounds ^tC₄H₉N?VCp(NⁱProp₂)Cl ( 3 ) and ^tC₄H₉N?V(NⁱProp₂)X₂ (X?CH₂CMe₃, O^tC₄H₉, CH₃COO) has been prepared. All compounds obtained are characterized by ¹H, ⁵¹V, ³¹P NMR spectroscopy. The X-ray diffraction analysis of 16 and 3 indicate a planar coordination sphere of the amido nitrogen atom.     

V. Mineralogie und Agrikulturchemie

Ohne Zusammenfassung     

V. Mineralogie und Agrikulturchemie

Colloid and Polymer Science -