A room-temperature single-crystal X-ray structure determination of the 1 : 1
adduct of 1,10-phenanthroline (`phen") with lutetium(III) acetate
(as its dihydrate) is recorded. Crystals are triclinic,
P 1, a 12·430(8),
b 10·681(4), c
8·134(8) Å, α 74·76(6), β 84·81(7), γ
74·29(4)°, Z = 2 f.u.; conventional
R on |F| was
0·031 for No 3939
independent ‘observed’ (I >
3σ(I)) diffractometer reflections. The complex
[(N,N′-phen)(O,O′-ac)Lu(O-ac-O′)4Lu(O,O′-ac)(N,N′-phen)].2H2O
is binuclear, the lutetium being eight-coordinated by bidentate phen and ac
(acetate) ligands and four oxygen atoms from the bridging acetate ligands.
Also recorded is the structural characterization of 1 : 1
Lu(ac)2Cl/tpy (tpy =
2,2′:6′,2″-terpyridine) as its pentahydrate; this complex is
triclinic, P 1, a
12·410(3), b 11·559(4),
c 9·976(4) Å, α 85·19(3),
β 70·30(3), γ 65·70(2)°, Z
= 2, R 0·049 for
No 4717. The complex is shown to
be
[(tpy)(H2O)2Lu(O2CCH3)2]Cl.3H2O,
with the lutetium nine-coordinated by tridentate tpy, a pair of bidentate
acetates and two unidentate water molecules, with the chloride uncoordinated.
Structural characterizations of a number of 1 : 1 adducts of variously
solvated lanthanoid(III) trichloroacetates, Ln(tca)3,
with tpy are also recorded. Yb(tca)3/tpy/MeOH (1
: 1 : 1) is triclinic, P 1, a
14·016(4), b 12·951(5),
c 9·604(3) Å, α 73·89(3),
β 76·56(3), γ 69·20(3)°, Z
= 2 f.u., R 0·057 for
No 4465. The complex is
mononuclear, the eight-coordinate
N3YbO5 array containing tridentate
tpy, unidentate methanol, and two unidentate and one bidentate chelating
anions. 1 : 1 : 1
Ln(tca)3/tpy/OH2 adducts
for Ln = La(-)Nd are triclinic, P 1,
a ≈ 13·4, b ≈
12·47, c ≈ 11·5 Å, α ≈
114·5, β ≈ 89·9, γ ≈ 115·6°,
Z = 1 binuclear array, R
0·061, 0·071 for No
3240, 2394. The two Ln atoms are
O,O′-bridged by a pair of
anions, the N3LnO6 nine-coordinate
lanthanoid environment being completed by a tridentate tpy, one water, one
unidentate and one bidentate anion. A 1 : 1 : 1
Lu(tca)3/tpy/OH2 array, by
contrast, is triclinic, P 1, a
16·569(8), b 14·815(5),
c 14·375(6) Å, α 62·05(3),
β 81·35(4), γ 77·97(3)°, Z
= 4 ‘mononuclear’ f.u., R
0·067 for No 6710. The
array, remarkably, contains species of both of the above types in a 1 : 2
binuclear-to-mononuclear ratio, but with water replacing methanol in the
mononuclear array.
Formation and structural characterization of a potassium amidinoguanidinate