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Alkali‐Metal meta ‐Hydroxyphenolates: Syntheses and Crystal Structures from Powder X‐Ray Diffraction
Author(s) -
Couhorn Uwe,
Dronskowski Richard
Publication year - 2004
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.200300342
Subject(s) - crystallography , monoclinic crystal system , orthorhombic crystal system , alkali metal , rubidium , hydrogen bond , crystal structure , rietveld refinement , chemistry , bond length , octahedron , powder diffraction , molecular geometry , x ray crystallography , potassium , molecule , diffraction , physics , organic chemistry , optics
M[ m ‐C 6 H 4 O(OH)] (M = Li—Cs) have been obtained as highly air‐ and moisture‐sensitive powders from reaction mixtures of the appropriate alkali metals and resorcinol in thf. Both the potassium and rubidium compounds were structurally characterized by means of powder X‐ray diffraction using the Simulated Annealing method and the Rietveld profile refinement technique including C—C/C—O bond distance and C—C—C angle restraints. K[ m ‐C 6 H 4 O(OH)] (orthorhombic P 2 1 2 1 2 1 ) forms infinite alternating chains of meta ‐hydroxyphenolate anions connected by K—O bonds and short charge‐assisted hydrogen bonds, thereby generating a three‐dimensional network of corrugated layers similar to the structure of pure resorcinol. The potassium cations are surrounded by a triangle of oxygen and, moreover, coordinated by six adjacent phenylene rings to form a distorted octahedron. The complex crystal structure of Rb[ m ‐C 6 H 4 O(OH)] (monoclinic Pa ) is characterized by layers of hydrogen‐bonded meta ‐hydroxyphenolate triple units separated by corrugated rubidium layers. The three crystallographically different Rb atoms are coordinated by three, four, and five oxygens with irregular polyhedra, and the rubidiums are also involved in further electrostatic interactions by up to eight phenylene rings.