We report on the
synthesis and characterization of three new nanosized
main group V heteropolyoxotungstates K
x
Na
y
[H
2
(XW
VI
9
O
33
)(W
VI
5
O
12
)(X
2
W
VI
29
O
103
)]·
n
H
2
O
{X
3
W
43
}
(
x
= 11,
y
= 16, and
n
= 115.5 for X = Sb
III
;
x
= 20,
y
= 7, and
n
= 68 for X = Bi
III
) and K
8
Na
15
[H
16
(Co
II
(H
2
O)
2
)
0.9
(Co
II
(H
2
O)
3
)
2
(W
VI
3.1
O
14
)(Sb
III
W
VI
9
O
33
)(Sb
III
2
W
VI
30
O
106
)(H
2
O)]·53H
2
O
{Co
3
Sb
3
W
42
}
. On the basis of the key parameters for the one-pot
synthesis strategy of
{Bi
3
W
43
}
, a rational step-by-step
approach was developed using the known Krebs-type polyoxotungstate
(POT) K
12
[Sb
V
2
W
VI
22
O
74
(OH)
2
]·27H
2
O
{Sb
2
W
22
}
as a nonlacunary precursor leading to the synthesis
and characterization of
{Sb
3
W
43
}
and
{Co
3
Sb
3
W
42
}
. Solid-state
characterization of the three new representatives
{Bi
3
W
43
}
,
{Sb
3
W
43
}
, and
{Co
3
Sb
3
W
42
}
by single-crystal
and powder X-ray diffraction (XRD), IR spectroscopy, thermogravimetric
analysis (...