Synthesis and structural characterization of some compounds involving metal-metal bonding of tellurium, bismuth, and zirconium. [Complex with hexaoxadiazabicyclohexacosane potassium]
Salts of the tritelluride(2-) and tetrabismuthide(2-) ions with the complex cation (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo(8.8.8)hexacosane potassium) (abbreviated crypt K/sup +/) were synthesized and their structures determined. The dark red (crypt K/sup +/)/sub 2/ Te/sub 3//sup 2 -/.en was produced by oxidation of K/sub 2/Te with an excess of tellurium and the very dark green (crypt K/sup +/)/sub 2/Bi/sub 4//sup 2 -/ was produced by the reaction of either K/sub 3/Bi, K/sub 3/Bi/sub 2/, K/sub 5/Bi/sub 4/, or KBi/sub 2/ with solvent. (Crypt K/sup +/)/sub 2/Te/sub 3//sup 2 -/.en crystallizes in the trigonal space group P3/sub 2/ with a = 12.229(1)A and c = 31.242(4)A and three formula units per cell. The Te/sub 3//sup 2 -/ ion has bond lengths of 2.692(5) and 2.720(4)A, an angle of 113.1(2)/sup 0/, and a hydrogen bond to an en molecule with d/sub Te-N/ = 3.46(6)A. (Crypt K/sup +/)/sub 2/Bi/sub 4//sup 2 -/ crystallizes in the triclinic space group P anti 1 with a = 11.604(4)A, b = 11.796(4)A, c = 11.096(3)A, ..cap alpha.. = 98.12(3)/sup 0/, ..beta.. = 98.02(3)/sup 0/, and ..gamma.. = 61.37(3)/sup 0/ and one formula per cell. The structure of the more common form of stoichiometric ZrCl/sub 2/, which is isostructural with 3R-MoS/sub 2/, (R3m, with a = 3.3819(3) and c = 19.378(3)A) was refined from single crystal data. A cluster form which is isostructural with Zr/sub 6/I/sub 12/ was found and its structure determined from powder data. 6T-Zr/sub 1+x/Cl/sub 2/ was determined from an intergrown ''single'' crystal containing 3R-ZrCl/sub 2/, to be a 6-slab superstructure based on a 2H/sub b/-MoS/sub 2/ type subcell with a = 3.3791(4) and c = 38.713(7)A. Another, 18T-Zr/sub 1+y/Cl/sub 2/, found in both single crystals and powder, has an 18 slab repeat sequence with a = 3.3820(2) and c = 116.21(2)A. The third is of unknown composition and exhibits ordering along a.
- Research Organization:
- Iowa State Univ., Ames, IA (United States)
- DOE Contract Number:
- W-7405-ENG-82
- OSTI ID:
- 6549645
- Report Number(s):
- IS-T-813
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
BISMUTH COMPLEXES
MOLECULAR STRUCTURE
TELLURIUM COMPLEXES
ZIRCONIUM CHLORIDES
CRYSTAL STRUCTURE
BOND LENGTHS
CHLORIDES
CHLORINE COMPOUNDS
COMPLEXES
HALIDES
HALOGEN COMPOUNDS
TRANSITION ELEMENT COMPOUNDS
ZIRCONIUM COMPOUNDS
400201* - Chemical & Physicochemical Properties