The ternary potassium lanthanoid carbonates KM(CO3)(2) (M = Nd, Gd, Dy
, Ho, Yb) are obtained as single crystals by high-pressure synthesis i
n steel autoclaves with carbon dioxide (starting pressure approximatel
y 50 bar at ambient temperature) in the presence of water from a mixtu
re of K2CO3 and MCl3 . xH(2)O (x = 7 and 6, respectively) at 450 degre
es C within 4 weeks. In KNd(CO3)(2) (orthorhombic, Pmn2(1), Z = 4, a =
973.1(2), b = 645.69(8), c = 855.58(14) pm, R-1 = 0.0763 for all data
) [Nd-mu(1)-(CO3)(3)-mu(2)-(CO3)(3)] polyhedra are connected three-dim
ensionally to [Nd(CO3)] layers as similarly in UO2(CO3); these layers
are connected via the second half of the carbonate ligands and K+ ions
. In KDy(CO3)(2) (monoclinic, C2/c, Z = 4, a = 853.8(2), b = 949.1(1),
c = 694.5(1) pm, beta = 111.1(2)degrees, R-1 = 0.0266 for all data) a
nd in the isotypic carbonates KM(CO3)2 (M = Gd, Ho, Yb) the polyhedra
[Dy-mu(1)-(CO3)(4)-mu(2)-(CO3)(2)] and [K-mu(1)-(CO3)(6)] are connecte
d to ''syndiotactic'' zig-zag chains and by further O-ligator atoms of
the carbonate ligands such that each zig-zag chain is surrounded by f
our unlike chains and vice versa.