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Michael Berkei Eduard Bernhardt Markus Schürmann Michael Mehring Helge Willner 《无机化学与普通化学杂志》2002,628(8):1734-1740
Preparation, Spectroscopic Characterization and Crystal Structures of Mercury(II)‐bis(tetracyanoborate) Hg[B(CN)4]2 and Dimercury(I)‐bis(tetracyanoborate) Hg2[B(CN)4]2 Hg[B(CN)4]2 ( 1 ) is synthesised by the reaction between Hg(NO3)2 and K[B(CN)4]2. In a comproportionation reaction of 1 with elemental mercury the corresponding mercury(I) salt Hg2[B(CN)4]2 ( 2 ) is obtained. The compounds were characterised by vibrational‐ and NMR‐spectroscopy, and their crystal structures were determined. Hg[B(CN)4]2 crystallizes in the trigonal system in the space group P3¯m1 with a = 781.75(3) pm, c = 601.68(2) pm, V = 318.44(2)Å3, and one formula unit per unit cell. For Hg2[B(CN)4]2 an orthorhombic unit cell with a = 568.9(1) pm, b = 3280.9(7) pm, c = 601.68(2) pm, V = 1389.6(5)Å, and Z = 4 is observed. 相似文献
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The Tetracyanoborates M[B(CN)4], M = [Bu4N]+, Ag+, K+ The tetracyanoborate anion is prepared for the first time as the tetrabutylammonium salt by the reaction of [NBu4]BX and BX3 (X = Br, Cl) in toluene with KCN. After purification and recrystallization of the product from CHCl3 colorless and needle size single crystals of [Bu4N][B(CN)4] are formed. After metathesis with AgNO3 the silver salt and subsequently with KBr the potassium salt is prepared. The three salts are characterized by single crystal X‐ray diffraction (Ag[B(CN)4] P 43m, a = 5.732(1) Å, V = 188.3 Å3, Z = 1, R1 = 0.75%; K[B(CN)4] I41/a, a = 6.976(1), c = 14.210(3) Å, V = 691.5 Å3, Z = 4, R1 = 1.90%; [Bu4N][B(CN)4] Pnna, a = 17.765(3), b = 11.650(2), c = 11.454(2) Å, V = 2370.5 Å3, Z = 4, R1 = 6.09%) and by NMR‐, IR‐, Raman‐ as well by UV‐spectroscopy. 相似文献
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Michael Neukirch Sonja Tragl H.‐Jürgen Meyer Torsten Küppers Helge Willner 《无机化学与普通化学杂志》2006,632(6):939-944
M[B(CN)4]2: Two new Tetracyanoborate Compounds with divalent Cations (M = Zn, Cu) The reaction of ZnO or CuO with [H3O][B(CN)4] in aqueous solution yielded single crystals of Zn[B(CN)4]2 and Cu[B(CN)4]2, respectively. The compounds were characterized by single‐crystal X‐ray diffraction. Zn[B(CN)4]2 ( (no. 164), a = b = 7.5092(9) Å, c = 6.0159(6) Å, Z = 1) crystallizes isotypic with Hg[B(CN)4]2. The structure of Cu[B(CN)4]2 (C2/m (no. 12), a = 13.185(3) Å, b = 7.2919(9) Å, c = 6.029(1) Å, β = 93.02(2)°, Z = 2) can be considered as a super‐structure, resulting from Jahn‐Teller distortion of the Cu2+ ions. Magnetic measurements were performed for the copper compound. Vibrational spectra and thermal stabilities were compared with the known mercury(II) tetracyanoborate. 相似文献
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Torsten Küppers Eduard Bernhardt Christian W. Lehmann Dr. Helge Willner Prof. Dr. 《无机化学与普通化学杂志》2007,633(10):1666-1672
The Tetracyanoboronic Acids H[B(CN)4]·n H2O, n = 0, 1, 2 Treatment of an aqueous solution of Na[B(CN)4] with an acidic cation exchange resin leads to a solution of the strong tetracyanoboronic acid. Evaporation of the solution at room temperature yields colourless single crystals of [H5O2][B(CN)4] ( , a = 9.5830(2) Å, c = 14.25440(3) Å, Z = 1). Further drying of [H5O2][B(CN)4] (mp. 115 °C) in vacuum at 50 °C gives polycrystalline [H3O][B(CN)4] (P63mc, a = 8.704(1) Å, c = 6.152(1) Å, Z = 2), which is thermally stable up to 145 °C. The anhydrous polycrystalline acid H[B(CN)4] is formed quantitatively by reacting Me3SiNCB(CN)3 with gaseous HCl. This acid starts to decompose at 190 °C with loss of HCN. All three acids were further characterized by vibrational spectroscopy, and elemental analysis. 相似文献
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