Tuning 1-D Pb(II) coordination polymers by flexible and semirigid dicarboxylates: Synthesis, structure and properties

Article abstract of DOI:10.1515/znb-2012-0301

Two new one-dimensional (1-D) Pb(II) coordination polymers, namely, [Pb(3-pdip)(L¹)]·H₂O (1) and [Pb(3-pdip)(L ²)] (2) [L¹H₂ = 1,6-hexanedioic acid, L ²H₂ = homophthalic acid, 3-pdip = 2-(3-pyridyl)imidazo[4, 5-f]1,10-phenanthroline] have been obtained from hydrothermal reactions of Pb(II) nitrate with the phenanthroline derivative and the two dicarboxylic acids. Single-crystal X-ray diffraction analysis reveals that compound 1 is a staircase-like double-chain coordination polymer constructed from binuclear [Pb₂N₄O₈] subunits and pairs of [L ¹]^2- anions. Compound 2 is a linear coordination polymer connected via two μ2-η²:η¹ carboxylate groups from [L²]^2- anions. Furthermore, adjacent chains of 1 and 2 are extended into 3-D supramolecular networks by hydrogen bonds and π-π stacking interactions. The organic carboxylic acids with different flexibility determine the structures of the coordination polymers. Moreover, the thermal stabilities and photoluminescence properties of compounds 1 and 2 were investigated.

Full text of DOI:10.1515/znb-2012-0301

Tuning 1-D Pb(II) Coordination Polymers by Flexible and Semirigid
Dicarboxylates: Synthesis, Structure and Properties
Guo-Cheng Liu, Zhi-Chao Guo, Xiu-Li Wang, Yun Qu, Song Yang, and Hong-Yan Lin
Department of Chemistry, Bohai University, Jinzhou, 121000, P. R. China
Reprint requests to Prof. Xiu-Li Wang. E-mail: wangxiuli@bhu.edu.cn
Z. Naturforsch. 2012, 67b, 185 – 191; received February 14, 2012
Two new one-dimensional (1-D) Pb(II) coordination polymers, namely, [Pb(3-pdip)(L1)]·H2O
(1) and [Pb(3-pdip)(L2)] (2) [L1H2 = 1,6-hexanedioic acid, L2H2 = homophthalic acid, 3-pdip =
2-(3-pyridyl)imidazo[4,5-f]1,10-phenanthroline] have been obtained from hydrothermal reactions of
Pb(II) nitrate with the phenanthroline derivative and the two dicarboxylic acids. Single-crystal X-ray
diffraction analysis reveals that compound 1 is a staircase-like double-chain coordination polymer
constructed from binuclear [Pb2N4O8] subunits and pairs of [L1]2− anions. Compound 2 is a linear
coordination polymer connected via two µ2-η2:η1 carboxylate groups from [L2]2− anions. Further-
more, adjacent chains of 1 and 2 are extended into 3-D supramolecular networks by hydrogen bonds
and π-π stacking interactions. The organic carboxylic acids with different flexibility determine the
structures of the coordination polymers. Moreover, the thermal stabilities and photoluminescence
properties of compounds 1 and 2 were investigated.
Key words: Hydrothermal Syntheses, Crystal Structures, Lead Coordination Polymers,
Photoluminescence
Introduction
plexes was widely investigated by Ma, Batten, Wang,
You, Casado, and our group [1, 2a, 3a, 5]. However, the
chemistry of lead-organiccoordinationpolymers based
on semirigid dicarboxylates is relatively limited [6].
For this paper, we select the rigid phenanthro-
The design and synthesis of lead(II) metal-organic
coordination polymers have been greatly developed,
not only because of their structural diversities, but
also owing to their potential applications in gas stor- line derivative ligand 2-(3-pyridyl)imidazo[4,5-f]1,10-
age and luminescence [1, 2]. However, it is still a phenanthroline (3-pdip) and two organic dicarboxylic
big challenge to predict the final structures of the acids (Scheme 1), flexible hexane diacid (L1H2) and
desired crystalline products, since many factors such semirigid homophthalic acid (L2H2) to investigate
as organic ligands, solvent systems and temperature the influence of the flexibility of the organic car-
may have a great influence on the self-assembly boxylic acids and the supramolecular recognition ac-
process [3, 4]. Recently, some 1,10-phenanthroline tion of the N-donor co-ligand on the structure of
derivatives, such as 2-(4-hydroxylphenyl) imidazo- the lead coordination polymers, based on the fol-
[4,5-f]1,10-phenanthroline (HOIP), 2-(3-pyridyl)imid- lowing considerations: (1) as a multidentate flexible
azo[4,5-f]1,10-phenanthroline (3-pdip) and 2-(4-pyr- O-donor ligand, L1H2 with multi CH2 groups for
idyl)imidazo[4,5-f]1,10-phenanthroline (4-pdip) with free twist may induce diverse metal-carboxylate co-
the common advantages of chelating and bridging N- ordination frameworks [1b, 7]; (ii) as a multidentate
donor ligands, have attracted great interest within co- semirigid O-donor ligand, L2H2 with a rigid spacer
ordination chemistry [1, 2a]. In addition, careful selec- of a phenyl ring and only one freely rotating CH2
tion of the organic ligands containing appropriate coor- group may favor the formation of new metal-carb-
dination sites linked by a proper spacer has been an ef- oxylate subunits [8]; (iii) as a multifunctional N-
fective way to obtain the target Pb(II) compounds [1 – donor ligand, 3-pdip not only possesses versatile po-
4]. As is known, multidentate organic dicarboxylate O- tential coordination sites, but also has a large aromatic
donor ligands can be divided into three types: flexible, ring system and may provide potential supramolecular
semirigid and rigid ligands. The coordination behav- recognition sites for π-π stacking interactions, which
ior of flexible and rigid dicarboxylates in Pb(II) com- may extend the metal-carboxylate subunits into high-
c
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G.-C. Liu et al. · Pb(II) Coordination Polymers
Fig. 1 (color online). The coordination environment of the
Pb(II) atom in compound 1.
derived from staircase-like double chains extended by
hydrogen bonds and π-π stacking interactions. In com-
pound 1, the lead atom is sevencoordinated by two
oxygen atoms (O3A, O4A) of a chelating carboxy-
late group, three oxygen atoms (O1, O2, O1B) of two
chelating-bridging carboxylic groups from three dif-
ferent [L1]2− anions and two chelating nitrogen atoms
(N1, N2) from one 3-pdip ligand showing a hemidi-
rected coordination geometry (Fig. 1). The Pb–O dis-
Scheme 1 (color online). The coordination modes of the di-
carboxylate ([L1]2− and [L2]2−) and the 3-pdip ligands in
the title compounds 1 and 2.
˚
tances vary from 2.325(4) to 2.974(4) A, and the Pb–
˚
N distances are 2.605(4) and 2.759(4) A, which are
near to those reported for [Pb2(L)2(1,4-bdc)2]n (1,4-
bdc = 1,4-benzenedicarboxylate and L = dipyrido[7,6-
a:6ꢀ,7ꢀ-c]-3-chloropyrido[2,3-b]quinoxaline) [11]. The
N–Pb–N angle is 60.89(12)◦. The O–Pb–O and N–
Pb–O angles are in the range from 50.55(12) to
166.20(15)◦ and 71.51(13)– 154.53(13)◦, respectively.
In compound 1, the two carboxylate groups of the
[L1]2− anions exhibit asymmetric chelating-bridging
coordination modes (µ2-η2:η1). The two µ2-O atoms
(O1 and O1B) from two carboxylate groups con-
nect the adjacent Pb(II) atoms to form a bi-metallic
[Pb2N4O8] subunit with a Pb(II)···Pb(II) distance of
dimensional supramolecular networks [2a, 9]. More-
over, the H atom of the imidazole group from 3-pdip
and the O atoms of the carboxylate groups of [L1]2−
and [L2]2− may provide the potential supramolecu-
lar recognition sites for hydrogen bonds interactions,
which may stabilize the final frameworks [10].
In this paper, we report two 3-D supramolecu-
lar compounds derived from double chains and lin-
ear chains, respectively: [Pb(3-pdip)(L1)]·H2O (1) and
[Pb(4-pdip)(L2)] (2). The results of the investigation
about the influence of the flexibility of dicarboxylates
on the coordination frameworks is presented and dis-
cussed. Moreover, the thermal stabilities and photo-
luminescence properties of compounds 1 and 2 were
studied.
˚
4.6351(14) A. The subunits are extended into a stair-
case-like double-chain coordination polymer through
the pairs of [L1]2− anions (Fig. 2a), and the dis-
tance between the cores of the [Pb2N4O8] subunits
˚
is 9.267(4) A. In compound 1, intermolecular hydro-
Results and Discussion
gen bonds and π-π stacking interactions play an im-
portant role in the construction of the supramolec-
ular framework. As a 3-connected linker, the wa-
Crystal and molecular structure of [Pb(3-pdip)-
(L1)]·H2O (1)
The single-crystal X-ray determination indicates ter molecule not only acts as an hydrogen bond ac-
that compound 1 is a 3-D supramolecular framework ceptor, but also as a donor to link adjacent chains.
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G.-C. Liu et al. · Pb(II) Coordination Polymers
187
(a)
(b)
Fig. 3 (color online). The coordination environment of the
Pb(II) atom in compound 2.
linear coordination polymer chains extended by hy-
drogen bonds and π-π-stacking interactions. In com-
pound 2, each Pb(II) center is eight-coordinated by
two chelating nitrogen atoms (N1 and N2) of the 3-
pdip ligand and six oxygen atoms of two cis chelating-
bridging acetate groups (O1, O2, O2B) and two
trans chelating-bridgingformylate groups (O3A, O4A,
O4B) from three different [L2]2− anions to form a
holodirected coordination mode (Fig. 3). The Pb–N
Fig. 2 (color online). (a) The 1-D coordination polymer ex-
tended through [Pb2N4O8] subunits and [L1]2− double link-
ers along the b axis. (b) The 2-D supramolecular layer ex-
tended via H bonding interactions from the pyridine rings
(N5), carboxylate oxygen (O4), imizole rings (N3) and lat-
tice water molecules (O1W).
˚
distances are 2.545(2) and 2.609(2) A, while the Pb–
˚
O bond lengths range from 2.5442(2) to 2.901(3) A
and are near the normal range [6]. The N–Pb–N angle
is 63.50(7)◦, while the O–Pb–O and N–Pb–O angles
are in the range 48.41(5)– 156.90(6)◦ and 72.54(7)–
139.71(6)◦, respectively.
The hydrogen bonding interactions between the atoms
O1W, N3 and N5 stabilize the 1-D coordination poly-
mer, and the hydrogen bonding interactions between
O1W and O4 of the carboxylate groups link adja-
cent chains into a layer along the ab plane [O1W–
It is notable that the two µ2-O2 atoms of two ac-
etates with chelating-bridging µ2-η2:η1 coordination
mode connect two Pb(II) centers, forming a binu-
clear [Pb2N4O10] secondary building unit (SBU) with
◦
˚
H1WA···N5C, 3.017(7) A, 159 (C: 1 − x, 2 − y,
◦
˚
˚
a Pb1···PbA distance of 4.556(3) A. The two adjacent
−z). N3–H3···O1WE, 2.857(6) A, 171 (E: 1 − x,
◦
˚
SBUs are further connected by two µ2-O4 atoms
of two formylate groups with chelating-bridging µ2-
η2:η1 coordination mode from [L2]2− anions to form
a 1-D-[PbO2]n-inorganic chain along the a direction
−y, 1 − z); O1W–H1WB···O4D, 2.814(6) A, 144
(D: 1 − x, 1 − y, −z) (Fig. 2b)]. On the other hand,
the π-π-stacking interactions between the pyridine
rings (containing N2 and N5) of 3pdip from differ-
ent supramolecular layers connect the layers into a 3-D
supramolecular architecture. Cg–Cg (distance between
˚
(Fig. 4a) [8d]. The distance PbA···PbB is 4.5279(2) A.
The hydrogen bonding interactions between the N4
atoms of the imidazole groups and the O1 atoms of
the acetate groups bridge the adjacent parallel chains to
generate a layer along the ab plane [N(4)–H(4)···O(1),
˚
ring centroids) is 3.587(4) A, and the dihedral angle
is 2.3(3)◦.
Crystal and molecular structure of [Pb(3-pdip)(L2)]
(2)
◦
˚
2.803(3) A, 165(3) ]. The π-π-stacking interactions
between the pyridine rings (containing N1) of 3-pdip
The X-ray diffraction study reveals that compound 2 ligands from different parallel chains stabilize the
˚
is a 3-D supramolecular network constructed from layer (Fig. 4a). Cg–Cg is 3.595(3) A, and the dihe-
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188
(a)
G.-C. Liu et al. · Pb(II) Coordination Polymers
ent organic carboxylates in these two systems (Figs. 1
and 3). In compound 1, a flexible fatty dicarboxy-
late ([L1]2−) with a long distance between the two
carboxylate groups was used. Therefore, a rectangu-
lar eighteen-membered ring was constructed by two
[L1]2− anions and two lead atoms with a dimension of
2
˚
about 8.4 × 9.3 A (Fig. 2a). Furthermore, a staircase-
like metal-organic double chain is formed (Fig. 2a).
Since a semirigid aromatic dicarboxylic anion ([L2]2−
)
is used in 2, the shorter distance of the two carboxylic
groups and the steric effect of L2 make the distance
between the Pb atoms shorter. Thus, a linear -[PbO2]n-
inorganic chain was obtained (Fig. 4a). The 3-pdip lig-
ands in compounds 1 and 2 show the same chelating
coordination modes only acting as terminal groups,
and the N atoms from the imidazole and 3-pryridine
groups can not coordinate to the Pb atom to extend the
double chain, which may have steric reasons. How-
ever, these uncoordinated N atoms play an important
role in extending the Pb carboxylate chains into high-
dimensional supramolecular networks through hydro-
gen bonds.
(b)
IR spectra
The main features in the IR spectra of 1 and 2
are due to the carboxylate, and CH2 groups, water
molecules and N-containing ligands. No strong ab-
sorption peaks around 1700 cm−1 for -COOH are ob-
served, indicating that all carboxyl groups of the or-
ganic moieties are deprotonated [12]. The bands at
about 800 and 705 cm−1 may be attributed to the ν(C-
N) stretching of the N–heterocyclic rings of the 3-
pdip ligands, and the weak absorption peaks of the -
Fig. 4 (color online). The supramolecular layer derived
from the 1-D coordination polymer possessing an inorganic CH2- groups appeared at around 2945 and 2932 cm−1
-[PbO2]n- chain (sky blue). (b) The 3-D supramolecular
in compounds 1 and 2, respectively [13]. For com-
framework connected through π-π stacking interactions be-
pound 1, the strong broad band at around 3400 cm−1
tween the pyridine rings (containing N5).
was assigned to the v(O-H) vibrations of water
dral angle is 0◦. Finally, the adjacent parallel lay-
ers are linked by π-π-stacking interactions between
the pyridine rings (containing N5) and the imidazole
groups of the 3-pdip ligands from different parallel
layers to form a 3-D supramolecular framework. Cg–
molecules [14]. The vibrations of the carboxylate
groups appeared at 1677 and 1552 cm−1 (for 1), and
at 1610 and 1528 cm−1 (for 2) [15].
Thermal properties
◦
˚
Cg is 3.727(3) A, and the dihedral angle is 10.61(1)
(Fig. 4b).
To investigate the thermal stabilities of the title
compounds, their decomposition behavior was studied
From the structure description above, the carboxy- by thermog◦ravimetric analyses (TGA) with a heating
late anions with different flexibility have a significant rate of ◦10 C min−1 in the temperature range of 30
influence on the resulting structures of the title coor- to 800 C (Fig. 5). The weight loss of 1 correspond-
dination polymers. The Pb(II) center is hemidirected ing to the◦release of water molecules occurred at
in 1 and holodirected in 2, which is due to the differ- about 200 C, showing good stability due to the ex-
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G.-C. Liu et al. · Pb(II) Coordination Polymers
189
a blue shift of ca. 25 nm (for 1) and a red shift of
ca. 120 nm (for 2) have been observed. Compared with
the π∗ → π transitions of the 3-pdip ligand, the car-
boxylate ligands show very weak π∗ → n transitions
which contribute little to the photoluminescence of the
title compounds [2a]. Therefore, the solid state photo-
luminescence of compounds 1 and 2 may be attributed
to metal-to-ligand and ligand-to-metal charge-transfer
transitions, respectively [2a]. The different emission
bands of 1 and 2 may be due to the different structures
and organic carboxylates used in this work [16].
Conclusion
In summary, we have synthesized two new Pb(II)
coordination polymers constructed from one phenan-
throline derivative and two organic dicarboxylic acids.
Compounds 1 and 2 exhibit a staircase-like double-
chain and a linear single-chain architecture, re-
spectively, further extended into 3-D supramolecular
frameworks by hydrogen bonds and π-π-stacking in-
teractions. The organic carboxylic acids with different
flexibility determine the structure of the 1-D Pb(II)-
carboxylate coordination polymers. Hydrogen bonds
and π-π-stacking interactions have a great influence on
the final supramolecular frameworks. Moreover, the ti-
tle compounds with the blue/green fluorescence prop-
erties and excellent thermal stability may be used as
luminescent materials.
Fig. 5. Thermogravimetric analysis of 1 and 2.
istence of hydrogen bonding interactions between the
water molecules and the coordination framework (ob-
served 2.7 %, calcd. 2.7 %). The significant weight loss
at 300 ◦C can be attributed to the decomposition of the
framework. Comparing ◦with 1, compound 2 is slightly
more stable up to 330 C, where the collapse of the
framework starts a significant weight loss.
Photoluminescence properties
To study the fluorescence properties of the title com-
pounds, the emission spectra of 1 and 2 in the solid
state at ambient temperature were measured (Fig. 6).
Compound 1 exhibits green photoluminescence with
an emission maximum at ca. 395 nm upon excitation
at 330 nm, while the emission maximum of 2 is at
about 545 nm (λex = 470 nm). Compared with the
emission of 3-pdip (λex = 260 nm, λem = 422 nm) [9a],
Experimental Section
Materials and methods
3-pdip was synthesized by the method given in [17].
All other reagents employed were commercially avail-
able and used as received without further purification.
FT-IR spectra (KBr pellets) were taken on a Magna FT-
IR 560 spectrometer, and the elemental analyses (C,
H, and N) were carried out on a Perkin-Elmer 240C
elemental analyzer. The luminescence spectra for the
samples were measured on a Hitachi F-4500 fluores-
cence spectrophotometer, and thermogravimetric anal-
ysis was carried out with a Pyris Diamond TG-DTA
instrument.
Synthesis of [Pb(3-pdip)(L1)]·H2O (1)
A
mixture of Pb(NO3)2 (0.1 mmol), L1H2
Fig. 6 (color online). Fluorescence spectra of 1 and 2 in the (0.1 mmol), 3-pdip (0.1 mmol), H2O (14 mL), and
solid state at room temperature.
NaOH (0.2 mmol) was stirred for 30 min in air, then
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G.-C. Liu et al. · Pb(II) Coordination Polymers
˚
Table 1. Crystal data and numbers pertinent to data collection Table 2. Selected bond lengths (A) and angles (deg) for com-
and structure refinement of compounds 1 and 2.
pounds 1 and 2.
1
1
2
Pb(1)-N(1)
Pb(1)-O(1)
Pb(1)-O(3)A
Pb(1)-O(1)B
2.759(4)
2.586(4)
2.584(4)
2.974(4)
Pb(1)-N(2)
2.605(4)
2.325(4)
2.582(4)
85.16(14)
78.14(15)
Formula
Mr
T, K
C24H21PbN5O5
666.65
C27H16PbN5O4
681.65
Pb(1)-O(2)
Pb(1)-O(4)A
O(2)-Pb(1)-O(4)A
293(2)
triclinic
P1
293(2)
triclinic
P1
Crystal system
Space group
O(3)A-Pb(1)-N(2) 121.57(13) O(2)-Pb(1)-O(3)A
¯
¯
115.81(14) O(4)A-Pb(1)-O(3)A 50.55(12)
˚
O(1)-Pb(1)-N(2)
O(2)-Pb(1)-N(1)
a, A
7.479(5)
9.127(5)
16.535(5)
78.706(5)
88.849(5)
83.015(5)
1098.6(10)
2
2.02
7.7
603
27.72
17882 / 5162
0.0356
316 / 5101
0.0303
0.1016
1.122
7.662(5)
11.935(5)
13.404(5)
108.998(5)
92.692(5)
101.757(5)
1126.1(10)
2
2.01
7.5
654
28.25
19200 / 5567
0.0231
338 / 5530
0.0157
0.0400
1.044
˚
90.72(14) O(2)-Pb(1)-O(1)
52.77(13)
120.75(13)
78.49(14)
71.51(13)
77.76(12)
67.25(14)
154.53(13)
94.80(13)
b, A
O(4)A-Pb(1)-N(1) 137.41(12) O(4)A-Pb(1)-O(1)
˚
c, A
O(3)A-Pb(1)-N(1) 166.20(15) O(3)A-Pb(1)-O(1)
α, deg
β, deg
γ, deg
O(1)-Pb(1)-N(1)
N(2)-Pb(1)-N(1)
O(2)-Pb(1)-O(1)B
88.31(14) O(2)-Pb(1)-N(2)
60.89(12) O(4)A-Pb(1)-N(2)
119.54(12) O(1)-Pb(1)-O(1)B
3
˚
V, A
O(4)A-Pb(1)-O(1)B 123.88(12) N(2)-Pb(1)-O(1)B
O(3)A-Pb(1)-O(1)B 83.86(14) N(1)-Pb(1)-O(1)B
Z
Dcalcd, g cm−3
µ(MoKα ), mm−1
F(000), e
Symmetry code: A 2−x, −y, 1−z; B 2−x, 1−y, 1−z.
2
Pb(1)-N(1)
2.545(2)
Pb(1)-N(2)
2.609(2)
2.668(2)
2.759(2)
2.868(2)
154.15(6)
95.67(8)
123.46(7)
110.72(7)
48.41(5)
79.88(8)
156.90(6)
θ
max, deg
Pb(1)-O(3)A
Pb(1)-O(1)
2.5442(2) Pb(1)-O(4)B
2.5735(2) Pb(1)-O(2)
Refl. measured / unique
Rint
Pb(1)-O(4)A
N(1)-Pb(1)-O(3)A
N(1)-Pb(1)-O(1)
2.901(3)
79.49(6)
84.05(7)
Pb(1)-O(2)B
Ref. parameters / data
R1a [I ≥ 2σ(I)]
wR2b (all data)
GOFc
O(1)-Pb(1)-O(4)B
N(2)-Pb(1)-O(4)B
N(1)-Pb(1)-O(2)
O(3)A-Pb(1)-O(2)
O(3)A-Pb(1)-O(1) 77.45(6)
−3
˚
N(1)-Pb(1)-N(2)
63.50(7)
∆ρmax/min, e A
1.7 / −1.8
0.5 / −0.7
O(3)A-Pb(1)-N(2) 139.71(6) O(1)-Pb(1)-O(2)
a R1 = Σ Fo|−|Fc /Σ|Fo|; b wR2 = [Σw(Fo −Fc2)2/Σw(Fo2)2]1/2
,
2
O(1)-Pb(1)-N(2)
83.16(7)
72.54(7)
N(2)-Pb(1)-O(2)
w = [σ2(Fo2)+(AP)2 +BP]−1, where P = (Max(Fo2,0)+2Fc2)/3;
N(1)-Pb(1)-O(4)B
O(4)B-Pb(1)-O(2)
GoF = [Σw(Fo −Fc2)2/(nobs −nparam)]1/2
.
c
2
O(3)A-Pb(1)-O(4)B 87.42(7)
Symmetry code: A 1+x, y, z; B 1−x, −y, 1−z.
transferred and sealed in a 25 mL Teflon reactor, which
was heated at 170 C for 3 d, leading to the forma-
◦
˚
with MoKα radiation (λ = 0.71073 A) in the ω scan
tion of yellow block-shaped crystals of 1 (∼ 38 % yield
based on Pb). – Anal. for C24H21PbN5O5: calcd.
C 43.24, H 3.18, N 10.51; found C 43.29, H 3.22,
N 10.47%. – IR (KBr, cm−1): ν = 3400(w), 2945(w),
1677(m), 1552(s), 1404 s, 1309(s), 1070(m), 821(m),
705(s).
mode. The structures were solved by Direct Methods
using the SHELXS program of the SHELXTL pack-
age and refined by full-matrix least-squares methods
with SHELXL [18, 19]. All non-hydrogen atoms were
refined anisotropically, and all hydrogen atoms were
placed in geometrically idealized positions and refined
isotropically. The details of crystallographic informa-
tion for compounds 1 and 2 are summarized in Ta-
ble 1. Selected bond lengths and angles of the title
compounds are listed in Table 2.
Synthesis of [Pb(3-pdip)(L2)] (2)
The synthetic procedure for 2 is the same as that
for 1 except that L2H2 (0.1 mmol) was used in-
stead of L1H2. Yellow block-shaped crystals of 2 were
obtained (∼ 34 % yield based on Pb). – Anal. for
C27H16PbN5O4: calcd. C 47.50, H 2.37, N 10.26;
found C 47.48, H 2.35, N 10.22 %. – IR (KBr, cm−1):
ν = 2932(w), 1610(m), 1528(s), 1470(s), 1430(w),
1366(m), 802(s).
CCDC 866643 (1) and 866644 (2) contain the
supplementary crystallographic data for this paper.
These data can be obtained free of charge from
The Cambridge Crystallographic Data Centre via
www.ccdc.cam.ac.uk/data request/cif.
Acknowledgement
This work was supported by the National Natu-
ral Science Foundation of China (no. 21171025) and
X-Ray structure determinations
Crystallographic data for the title compounds were the Natural Science Foundation of Liaoning Province
collected on a Bruker Smart 1000 CCD diffractometer (no. 201102003 and 2009402007).
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