Crystals of Fe3R(BO3)4 (R
= Y, La, Nd) have been grown. Their structure and
properties
show close relations. The structures of these materials have been
established by single-crystal X-ray diffraction. They crystallize in the huntite,
CaMg3(CO3)4, structure
type,
trigonal system, space group R32 (No. 155), Z =
3, with unit-cell parameters (Å) a =
9.592(1),
9.578(1), and 9.563(2) and c = 7.597(7),
7.605(3), and 7.575(2), for R = La, Nd, and
Y0.5Bi0.5,
respectively. They contain RO6 trigonal prisms and
smaller FeO6 octahedra forming layers
and giving rise to Fe−R distances of ≃3.78 Å. RO6
polyhedra are interconnected within the
layers by corner sharing with triangular BO3 groups of two
types and FeO6 octahedra.
FeO6
octahedra form 1D helicoidal chains with relatively short Fe−Fe
distances, ≃3.18 Å. The
temperature dependence of the magnetic susceptibility from 350 to 1.8 K
for Fe3R(BO3)4
shows two maxima at about 260 and 35 K and, for R = Nd, another
maximum at 6 K. The
presence of magnetic order is attributed to magnetic Fe−Fe or
Fe−O−Fe interactions.
Infrared spectra in the range 4000−240 cm-1 show
the ν1, ν3, and ν4 IR-active
bands of the
B(1)O3
3- triangular groups as well as
ν2 of less symmetrical
B(2)O3
3-.
The new phases, Na4M3(PO4)2(P2O7) (M = Mn, Co, Ni), have been synthesized by solid-state reactions. Single crystals of Na4M3(PO4)2(P2O7) (M = Mn, Ni) have been isolated and
their structure has been determined by X-ray diffraction techniques using as the starting
model the structure of the isostructural compound Na4Co3(PO4)2(P2O7). These compounds
crystallize in the orthorhombic noncentrosymmetric space group Pn21
a with a = 17.991(3)
Å, b = 6.6483(1), and c = 10.765(2) Å for the manganese compound and a = 17.999(2), b =
6.4986(6) Å, and c = 10.4200(9) Å for the nickel compound, with Z = 4. Magnetic
measurements reveal the existence of antiferromagnetic interactions in the nickel compound.
The manganese and cobalt compounds show canting antiferromagnetic behavior at low
temperatures. Magnetic correlation is also studied from the analysis of possible superexchange pathways in the structure. The ionic conductivity, due to Na+ ions, is measured for
the three compounds. The activation energy is nearly the same (0.81−0.86 eV), but the
conductivity at 300 °C changes, increasing from 2.1 × 10-7 S cm-1 for the Ni compound to
1.3 × 10-6 S cm-1 for the Co one, and then from this value to 2.7 × 10-5 S cm-1 for the Mn
compound.
The 3D polymeric terephthalate of scandium has been synthesized and its structure solved by single-crystal XRD. It was obtained as a single phase and characterized and tested as a hydrogen and nitrogen
adsorbent and heterogeneous catalyst as a redox agent in the oxidation of sulfides. The compound shows
a BET area of 721 m2 g-1 with a high C
BET = 7000. The high chemical and thermal stability and excellent
hydrogen sorption properties make this compound a useful material for hydrogen storage.
The new hybrid inorganic−organic polymer In2(OH)3[O4C8H4]1.5 has been hydrothermally obtained. Conditions for
the synthesis are reported. The crystal structure of this material has been established by single-crystal X-ray
diffraction: it is monoclinic, with space group P21/c (Nο. 14), a = 6.772(1) Å, b = 10.329(2) Å, c = 20.152(3) Å,
β = 97.573(3)°. The In atoms are octahedrally coordinated by three hydroxide groups and three different molecules
of carboxylate ligand. The resulting polymeric 3D structure can be envisaged as having been generated from a
honeycomb (6,3) 2D that is cross-linked by the BDC organic anions. Data of IR and TGA-DTA studies, as well as
the results of reduction of nitroaromatics and selective oxidation of organic sulfide reactions catalyzed by the new
material, are reported.
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