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30
卷
6
期
201
1.
6
结构化学
(JIEGOU
HUAXUE)
Chinese
J.
S.的
Ict.
Chem.
Vo
l.
30
,
No.
6
872-876
Synthesis
and
Crystal
Structure'
of
a
1\值
ixed
(Phthalocyaninato
)(porphyrinato)
Yttrium
Double-decker
Complex
①
LU
Ji-
Tao
WANG
Hai-Long
ZHANG
Xiao-Mei
②
(Sc
hool
ofChemistry
& Chemical Technolo
gy.
Shandong
Universi
ty,
Jinan 250100, China)
ABSTRACT
The title compound, a mixed
(p
hthalocyaninato )(porphyrinato) yttrium double-
decker complex 1, has
been
synthesized
and
structurally characterized
by
X-ray single-crystal
di
佳
action
method. Crystal
da句:
monoclinic, space group
α
/c
,
Z = 8,
C79Hs2Cl
lON1204Y,
M,.
=
1676.74, a =
38.217(
匀,
b =
18.9867(1
月,
c = 26.200(3)
Å
,
β
=
128.0190
(1
0t
,
V=
14977(2) N, Dc
= 1
.4
87
glcm
3
,
μ
。在
o
K<
α)
=
1.
196
mm-\
F(OOO)
= 6808, R = 0.0745
and
wR
=
0.2208
岛
r
observed
reflections with 1 >
2σ
(
1).
X-ray analysis
reveals
也
at
the coordination polyhedron adopts a slightly
distor
时
square-antiprismatic
structure around the metal center. Both phthalocyanine
and
porphyrin
ligands are saucer-shaped, with the skew angle
ofthe
two ligand planes approximately 45
0
•
Keywords:
crystal
structure
,
phthalocyanine
,
porphyrin
1
INTRODUCTION
Sandwich
句
pe
phthalocyaninato
an
d/
or
porphyri-
nato complexes,
in
which two
or
也
ree
te
位
apyrrole
ligands are held
by
various metal ion( s) in close
pr,。对
mity
,
have
been
extensively studied for several
decades[11.
Owing
ωthe
unique optical, electrical,
and magnetic properties, associated with the intri-
gu
也
gin
位
amolec
u1ar
;r
-πinteractions
,
these com-
plexes represent
an
important class
of
molecular ma-
terials
岛
r
a wide range
of
applications[2
1
.
A1
though a
vast numbe
t:
of
homoleptic
and
heteroleptic phthalo-
cyaninato
扭
d
po
甲
h
严
inato
double-
and
位
iple-dec
ker
complexes have been reported, the single crys-
tals
of
these complexes remain
rare[3].
Partic
u1
arly,
to the best
of
our
knowledge, the single crystals
of
the mixed ring double-deckers containing one por-
phyrin ligand
and
one phthalocyanine ligand are
Received
28
Sep
旬
mber2010;
a
∞
epted
24
January
2011
(CCDC
806073)
o
n1
y limited
ωabout
ten
examples
也
us
fat
钊
1.
As
part
of
our
continuing
interest
坦
heteroleptic
rare
e
缸也
complexes
with tetrapyrrole ligands
[1
-10
1
, we des-
cribe herein a systematic study
of
a mixed phtha-
locyaninato
and
porphyrinato double-decker com-
plex, namely
[Y
(TCIPP)(Pc)] (TCIPP meso-
tetrakis( 4-chlorophenyl)porphyrinato,
PC
=
ph
也
a
locyanina
阳),
including their synthesis, crystal struc-
ture and electrochemical properties.
2 EXPERIMENTAL
2.1
General
n-Octanol was distilled from sodium under
ni
位
0-
gen
before use.
Column
chromatography was carried
out
on
silica gel
(M
erck
,
K.i
eselgel 60, 200-300
mesh)
with
也
e
indicated eluen
t.
All other reagents
and solvents were
used
as received. The compounds
(
Supported
by
the
Natio
na1
Na
tura1
Science
Foundation
ofChina
(N
o.
20801031)
,也
.e
Na
tura1
Science
Foundation
。
f
Shandong
Provinω
(N
o.
Q2008B01)
租
d
也
e
Docto
ra1
Foundation
of
Shandong
Province
(N
o.
2007BS020
16).
In
dependent
Inn
ovation
Foundation
ofSDU
is
gratefully
acknowledged
(
Corresponding
au
曲。
r.
E-mail:
zhangxiaomei@sdu.edu.cn