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Si 4 4– in Solution – First Solvate Crystal Structure of the Ligand‐free Tetrasilicide Tetraanion in Rb 1.2 K 2.8 Si 4 ·7NH 3
Author(s) -
Lorenz Corinna,
Gärtner Stefanie,
Korber Nikolaus
Publication year - 2017
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201600336
Subject(s) - crystallography , chemistry , crystal structure , ligand (biochemistry) , triphenylphosphine , ion , liquid ammonia , sodalite , ternary operation , single crystal , stereochemistry , ammonia , organic chemistry , biochemistry , receptor , catalysis , zeolite , computer science , programming language
We report the first solvate structure of the silicide anion Si 4 4– , which provides circumstantial evidence of the stability of the highly charged anion in liquid ammonia solutions. The solvate Rb 1.2 K 2.8 Si 4 · 7NH 3 crystallized from a mixture of the ternary compound K 6 Rb 6 Si 17 with the transition metal complex [(C 6 H 5 ) 3 P] 2 Ni(CO) 2 [bis(triphenylphosphine)dicarbonylnickel] in the presence of the chelating agents 18‐crown‐6 (1,4,7,10,13,16‐hexaoxacyclooctadecane) and [2.2.2]cryptand (4,7,13,16,21,24‐hexaoxa‐1,10‐diazabicyclo[8.8.8]hexacosane) in liquid ammonia. Single X‐ray diffraction analysis confirms the presence of the Si 4 4– anion in the crystal structure of Rb 1.2 K 2.8 Si 4 · 7NH 3 , which represents the first solvate compound of the naked tetrasilicide tetraanion. All five crystallographically independent cation positions show mixed occupancy by Rb + and K + .