696
X. Chen et al. / Inorganic Chemistry Communications 14 (2011) 694–696
room temperature, the χMT value is 1.1 cm3 mol−1 K which is a
typical value for an isolated Ni(II) ion with gN2.00. χMT is practically
constant to about 30 K and then decreases to 0.4 cm−3 mol−1 K at 2 K.
This feature indicates typical paramagnetic behavior for a Ni(II) ion in
which the D parameter and/or intermolecular interactions (usually
antiferromagnetic) are active at low temperature [10]. In an attempt
to calculate the D value, we have fitted the experimental χMT value
to the formula given by Kahn for a mononuclear Ni(II) ion con-
sidering the zero field split (ZFS) of the S=1 ground state [10]. The
best fit value are |D|=7.7 cm−1 and g (average)=2.05. The D value
is consistent with that typical for Ni(II) ions (close to 5–8 cm−1).
In summary, a novel linear trinuclear nickel(II) complex, [Ni3
(bzshz)2(Himdz)2(H2O)2]·2DMF was synthesized by the mixed
ligands N-benzoyl-salicylhydrazide and imidazole. This is the first
nickel (II) complex based on N-acyl-salicylhydrazide ligands to form a
3D hydrogen bonding framework. The magnetic determination shows
that both the terminal Ni(II) ions are diamagnetic and the central Ni
(II) shows typical paramagnetic behavior.
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(2001) 1084;
(b) S. Lin, S.-X. Liu, B.-Z. Lin, Inorg. Chim. Acta 328 (2002) 69;
(c) S. Lin, S.-X. Liu, J.-Q. Huang, C.-C. Lin, J. Chem. Soc. Dalton Trans. (2002) 1595;
(d) J.-M. Dou, M.-L. Liu, D.-C. Li, D.-Q. Wang, Eur. J. Inorg. Chem. (2006) 4866;
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Ji, Inorg. Chem. Commun. 10 (2007) 1351;
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Acknowledgement
[6] (a) M.-X. Yang, S. Lin, L.-J. Chen, S.-X. Liu, Chin. J. Inorg. Chem. 19 (2003) 433;
(b) M.-X. Yang, S. Lin, Acta Crystallogr. Sect. E E61 (2005) 1095;
(c) M.-X. Yang, S. Lin, P. Yu, L.-J. Chen, S.-X. Liu, Chin. J. Chem. 23 (2005) 1407;
(d) S. Lin, M.-X. Yang, S.-X. Liu, Polyhedron 26 (2007) 4793.
[7] Syntheses: The ligand N-benzoylsalicylhydrazidate (H3bzshz) was prepared according
to the reported procedure [6b]. Synthesis of [Ni3(bzshz)2(Himdz)2 (H2O)2]·2DMF 1: To
a mixture solution of MetOH (15 mL) and DMF (6 mL) of H3bzshz (25.6 mg, 0.1 mmol)
and Himdz (13.6 mg, 0.2 mmol), a methanol solution (10 mL) of Ni(CH3COO)2·4H2O
(24.8 mg, 0.1 mmol) was added gradually with stirring. The resulting red solution was
further stirred for 1 h and filtered. The red crystals separated after several days were
collected in 30% yield based on Ni. Anal. Calcd for C40H44N10O10Ni3 (%): C, 48.00; H,
4.43; N, 14.00. Found: C, 48.15; H, 4.31; N, 14.12. IR (KBr pellet, cm−1): 3425 (w); 3136
(vs); 2924(vs); 2855 (vs); 1657 (s); 1601 (vs); 1569 (s); 1523 (s); 1448 (s); 1410 (s);
1384 (s); 1357 (s); 1259 (s); 1151 (s); 1067 (s); 757 (s); 659 (s); 574 (s).
[8] Intensity data were collected at a Rigaku RAPID Weissengberg IP diffractometer
at 293 K using graphite-monochromated Mo-Kα radiation (λ=0.71 073 Å) and
the ω scan mode. Crystallographic data for 1: C40H44N10O10Ni33, Mr =1000.98,
Monoclinic, space group P21/c, a=8.117(12) Å, b=14.548(16) Å, c=19.20(3) Å,
β =114.92(7)°, V=2056(3)Å3, Z=2, Dc=1.617 g cm−3, μ=1.432 mm−1, 3952
unique data, 2895 observed [IN2 σ (I)], 290 variables, Rint =0.0757, R1 =0.0477,
wR2 =0.0936, S=1.068. All of the non-hydrogen atoms were refined anisotrop-
ically. The hydrogen atoms of water molecules were located from the difference
Fourier maps and the other hydrogen atoms were placed in their calculated
positions.
The authors thank the Fujian Normal University for the financial
support from the Undergraduate Students’ Extracurricular Technol-
ogy Project.
Appendix A. Supplementary material
CCDC 773488 contains the supplementary crystallographic data
for this paper. These data can be obtained free of charge via http://
tallographic Data Center, 12 Union Road Cambridge CB2 1EZ, UK.
Supplementary data to this article can be found online at
doi:10.1016/j.inoche.2011.02.008.
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