Slow crystallisation (in water glass) has been used to obtain Na-2(ca). 3H(
2)O (1) and Na-2(ca)phen . 2H(2)O (2) which have been characterised by X-ra
y crystallography. 1:C12H12O4Na4O14, triclinic a = 6.567(1), b = 8.472(1),
c = 9.816(1) Angstrom, alpha = 106.71(1), beta = 92.04(1), gamma = 92.48( 1
)degrees, U = 522 Angstrom(3), P-1, Z = 1, F(000) = 308, mu(Mo-K alpha) = 0
.72 mm(-1), 1700 observed [F > 4.0 sigma(F)] gave a final R = 3.56%. 2: mon
oclinic, a = 10.754(1), b = 19.778(2), c = 13.681(1) Angstrom, beta = 98.55
(1)degrees, U = 2877 Angstrom(3), P2(1)/c, Z = 4, F(000) = 1328, mu(Mo-K al
pha) = 0.31 mm(-1), 2337 observed [F > 4.0 sigma(F)] gave a final R = 5.73%
. In both structures the chloranilate anions make use of chlorine atoms to
complete the six coordination of the sodium centres in the layer/chain syst
ems. (C) 1998 Published by Elsevier Science S.A. All rights reserved.