Abstract
The reaction of Ni(SCN) 2 · 4NH 3 with MNH 2 (M ≡ K, Rb, Cs) in liquid NH 3 leads to amidoniccolates with unexpected compositions. Interpretation of the results of X-ray structure determinations, quantitative analytical measurements and IR spectroscopic measurements indicate a hitherto unknown type of mixed-crystal structure or inclusion compounds. The adjusting of protons on the square planar [Ni(NH 2) 4] 2−-complex ions gives positively charged cages that are partially occupied by CN − ions. Charge compensation is provided by additional alkali metal cations, that cap the hexagonal prismatic proton cages. The compounds are characterized by the following data: K 6Ni 3(NH 2) 12 · (KCN) 1.0 · (KNH 2) 0.2: Im3, a = 13.454(2) A ̊ , Z = 4, d 4 25 = 1.849(3), ρ( X- ray) = 1.853 g cm −3, R = 0.021, R w = 0.022. Rb 6Ni 3(NH 2) 12·(RbCN) 1.0·(RbNH 2) 0.3: Im3, a = 13.872(5) A ̊ , Z = 4, ρ( X- ray) = 2.466 g cm −3, R = 0.044, R w = 0.059.
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