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30
卷
6
期
201
1.
6
结构化学
(J
IEGOU
HUAXUE)
Chinese
J.
Struct.
Chem.
Vo
l.
30
,
No.
6
785-792
A
Porous
Organic-inorganic
Hybrid
Compound
Constructed
from
Polyoxovanadium
Borate
Anions, Dinuclear N a Sites
and
Metal-organic U
nits
①
LI
Guang-Man
MEI
Hong-
Xin
CHEN
Xiang-Yi
CHEN
Yi-Ping
SUN
Yan-Qiong
ZHANG
Han-Hui
CHEN
Xiao-Ping
(D
句
partment
01
Chemis
t.
η"
Fuzhou University, Fuzhou, Fujian 350108, China)
ABSTRACT
A polyoxovanadium borate [N
a(H20)h
[Na(H20)zh[Cu(en
)z
][VI2BI80S4(OH)
6l
但
30)2.
(H
20)181
(en = ethylenediamine) has been hydrothermally synthesized and characterized
by
IR,
two-dimensional infrared (2D IR) correlation spectroscopy with magnetic and thermal
pert
旧
ba
tion, thermal
IR
spectroscopy, thermal
gravime
仕
ic
analysis and single.,.crystal X-ray
di
岱
action.
It
crystallizes in triclinic, space group
PÏ
with a = 12.981(3), b = 13.044(3), c = 14
.2
08(3)
A
,
α=
63.98(
匀
,
ß=77.17(
坷
,
y =
14.208(3
沪
,
V=
200
1.
0(8) A
3
, Z = 1,
M,.
= 2518.05,
Dc
= 2.090
g!
cm-
I
,
F(OOO)
= 1255.0,
Mu(mm
叮=
1.
756
,
λ
仙
fo
Ki
α)
= 0.71073 A, R = 0.0625 and
wR
= 0.1952. In 1, the
[V
12
B
I8
0
S4('
。而
6]8-
units are connected
by
[CU(en)2]
衍,
binu
cI
ear
Na(l)
and
Na(2) to form a
three-dimensional porous framewor
k.
Keywords:
organic-inorganic
hybrid
,
porous
framewor
k,
polyoxovanadium
borate
, 2D
IR
correlation
spectroscopy
,
thermal
IR
spectroscopy
1
剧
TRODUCTION
Recently, there has been
much
recent
interest
也
mixed organic-inorganic materials,
especially
岛
rthe
formation
of
new porous
materials[I
,
21.τ
'h
e
porous
polyoxovanadium borates developed recently
by
Haushalter, Zubieta and others[3-
8
1 have some
of
the
most interesting structural and compositional diver-
sity. Until now
, the polyoxovanadium borates con-
nected with linkers
by
covalent bond to form a
three-dimensional (3D) microsoft framework are
relatively less studied.
Thus
,也
e
preparation and
characterization
of
mixed organic-inorganic poly-
oxovanadium borates still remain challenging[9
,
I
町.
The earliest full description
of
perturbation based
Received
3
September
2010;
accepted
26
November
2010
(CCDC
756202)
dynamic
2D
correlation spectroscopy, based on a
simple sinusoidal perturbation
, was put forward in
1990
by
Noda[lll.τ
'h
en
,
the idea
of
2D correlation
coefficient maps
baséd
on
the statistical correlation
analysis introduced
by
Barton II
et
al.[12
1
, which
made the next significant advance in the
2D
cor
四
relation spectroscopy
by
removing the constraint
of
sinusoidal perturbation.
On
this basis, a major
breakthrough
in
this field occurred when the ge-
neralized
2D
correlation spectroscopy based on any
arbitrary shape
of
perturbation waveform introduced
by
Noda[
I3-
16
1.
Since then, the generalized two-
dimensional
in
企
ared
(2D
IR)
correlation spectro-
scopy has become a
verypowerful
and versat
i1
e tool
岛
r
elucidating subtle spectral changes induced by an
(Th
is
work
was
suppor
时
by
the
National
Natural
Science
Foundation
ofChina
(20873021
,
21003020)
,
Doctoral
Fund
ofMinis
町
。
f
Ed
ucation
ofChina
(20093514120002)
,
and
New
Ce
ntury
Excellent
Talent
Supported
Plan
ofFujian
Provinc
币。
XSJRC2007-21)
(
Corresponding
au
也
or.
E-mail:
ypchen007@hotmai
1.
com