Z.-X. Wang, H.-P. Xiao et al.
(1)
ARTICLE
Preparation of [Mn3(bidc)2(C2O4)(H2O)10]n (1): Complex 1 was pre-
pared by reaction of H2bidc (0.16 mmol), oxalic acid (0.03 mmol), and
MnSO4·H2O (0.3 mmol) in ethanol/water (v/v 1:1). Single crystals
were obtained after two weeks in a yield of 21.1 % (based on Mn).
Anal. calculated for C20H28Mn3N4O22: C 28.55; H 3.35; N 6.66 %;
found: C 28.19; H 3.62; N 6.90 %. IR (KBr): ν = 3337 (m), 3166 (s),
˜
1633 (s), 1549 (s), 1468 (s), 1416 (s), 1362 (s), 1313 (m), 1257 (m),
1183 (m), 903 (m), 784 (m), 677 (w), and 629 (w) cm–1.
Crystallographic Data Collection and Refinement
Crystallographic data were collected with a Bruker SMART CCD dif-
fractometer operating at room temperature. Intensities were collected
with graphite monochromatized Mo-Kα radiation (λ = 0.71073 Å), us-
ing the phi and omega scan technique. Data reduction was made with
the Bruker SAINT package. Absorption correction was performed us-
Figure 4. Temperature dependence of the χMT and 1/χMT product for
1 at 2 KOe field. The solid line is the best fits obtained from the model ing the SADABS program. The structure was solved by direct methods
and refined on F2 by full-matrix least-squares using SHELXL-2000
described in the text.
with anisotropic displacement parameters for all non-hydrogen atoms.
Hydrogen atoms were introduced in calculations using the riding
model. All computations were carried out using the SHELXTL-2000
With this equation, the calculated results in the temperature program package.[20] The crystallographic data for 1:
range from 35 to 300 K are J = –1.50 cm–1, and g = 2.063
¯
C20H28Mn3N4O22, Mr = 841.28, triclinic, space group P1, a =
with R = Σ[(χMT)calc–(χMT)obs]2/Σ(χMT)obs = 3.7 × 10–4. The
2
6.7694(13) Å, b = 10.426(2) Å, c = 11.446(2) Å, α = 70.626(2) °, β =
75.957(2) °, γ = 78.696(2) °, V = 733.4(2) Å3, Z = 1, F(000) = 427,
μ = 1.377 mm–1, Dc = 1.905 g·cm–3, GOF = 1.067, R1 = 0.0412, wR2 =
0.0905 [I > 2σ(I)]. Selected bond lengths, angles, and hydrogen bonds
are listed in Table 1 and Table 2.
negative coupling constant indicates antiferromagnetic coup-
ling between the neighboring MnII ions mediated by oxalate
bridges, which are similar to those reported previously.[19]
Crystallographic data for the structure reported in the paper has been
deposited as supplementary publication CCDC-780182 for 1. These
quest/cif or from the Cambridge Crystallographic Data Centre CCDC,
12 Union Road, Cambridge CB2 1EZ, UK (Fax: 44-1223-336-033; or
E-Mail: deposit@ccdc.cam.ac.uk).
Conclusions
A new manganese(II) complex [Mn3(bidc)2(C2O4)(H2O)10]n
with 3D supramolecular architecture was synthesized and char-
acterized. The stability of the structure in the solid-state was
strengthened by the intramolecular and intermolecular hydro-
gen bonding interactions. Magnetic analysis revealed antiferro-
magnetic coupling interactions between the MnII ions.
Supporting Information (see footnote on the first page of this article):
IR spectrum (Figure S1) and thermogravimetric analysis of 1 (Figure
S2).
Experimental Section
Acknowledgement
Materials and Methods
This work was supported by the National Natural Science Foundation
of China (No. 20901049 and 20871095), Excellent Youth Teachers
Foundation of Shanghai Municipal Education Committee and the Inno-
vation Foundation of Shanghai University.
All chemicals used during the course of this work were of reagent
grade and used as received from commercial sources without further
purification. Elemental analyses for carbon, hydrogen, and nitrogen
were carried out with a Vario EL III elemental analyzer. Infrared spec-
tra were recorded with a Nicolet A370 FT-IR spectrometer using KBr
pellets in the 4000–400 cm–1 region. TGA experiment was performed
with a Shimadzu DT-20B thermogravimetric analyzer from 20 to
800 °C at a heating rate of 10 °C·min–1 in nitrogen. Variable-tempera-
ture magnetic susceptibility measurements were taken at an applied
field of 2 KOe on a Quantum Design MPMS-XL7 SQUID magnetom-
eter working in the temperature range of 300–1.8 K. The molar mag-
netic susceptibilities were corrected for the diamagnetism estimated
from Pascal’s tables and for the sample holder by previous calibration.
References
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© 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Z. Anorg. Allg. Chem. 2011, 301–305