EXPERIMENTAL
- Materials, Methods and Apparatus
All commercially available chemicals were used as received. Water was distilled before use. IR spectra of solid samples (KBr pellets) were recorded on a Perkin-Elmer Spectrum X spectrophotometer between 4000 cm
−1
and 400 cm
−1
. The elemental analyses (C, H, N) were performed on samples using a CE Instruments EA-1110 Elemental Analyzer at KRICT, Korea. The free ligand
L1
, Zn(
L1
)(NO
3
)
2
and Na
2
bpdc were synthesized by literature procedures.
24,26,27
- Synthesis of 1
To a DMF (10 mL) solution of Zn(
L1
)(NO
3
)
2
(53 mg, 0.1 mmol) was added a stoichiometric amount of Na
2
bpdc (29 mg, 0.1 mmol) in water (10 mL), which was allowed to stand in an open beaker at ambient temperature. After a week, colorless crystals of
1
were obtained. Yield: >90% based on Zn(
L1
)(NO
3
)
2
. Anal. Calcd. for C
34
H
49.50
ZnN
4
O
4.75
(2): C, 62.29%; H, 7.61%; N, 8.55%. Found C, 62.69%; H, 7.57%; N, 8.66%. IR (KBr, cm
−1
): 3491, 3345 (νOH), 3220, 3125 (νNH), 1592, 1540 (ν
as
COO), 1380 (ν
s
COO).
- Synthesis of 2
To a DMF (10 mL) solution of Zn(
L1
)(NO
3
)
2
(263 mg, 0.5 mmol) was added an aqueous solution of
e,e-trans
-1,4-chdcH
2
(86 mg, 0.5 mmole) and five pipette drops of triethylamine. The mixture was left until colorless blocks of
2
formed. The crystals were filtered and dried in air. Yield: 67% based on Zn(
L1
)(NO
3
)
2
. Anal. Calc. for C
28
H
54
N
4
O
6
Zn-2H
2
O: C, 58.72%; H, 8.74%; N, 9.79%. Found C, 58.75%; H, 8.91%; N, 9.88%. IR (KBr, cm
−1
): 3413 (νOH), 3160 (νNH), 1649 (δH
2
O), 1572 (ν
as
COO), 1384 (ν
s
COO).
- X-ray Crystallography
5
contains a summary of selected crystallographic data and structure refinement details for
1
and
2
. Data were collected on a Nonius Kappa CCD (for
1
) or a Bruker Kappa APEX-DUO CCD (for
2
) diffractometer, using graphite monochromated Mo K
α
radiation. A combination of ϕ and ω (with κ offsets) scans were used to collect sufficient data. The Denzo-SMN package was used to process the data frames.
28
The structures were solved and refined using the SHELXTL∖PC V6.1 package.
29
Refinement was performed by full-matrix least squares on
F
2
using all data (negative intensities included). Crystallographic data for the structures reported here have been deposited with CCDC (Deposition Nos. CCDC-743544 (
1
) and CCDC-1059162 (
2
)). These data can be obtained free of charge
via
http://www.ccdc.cam.ac.uk/conts/retrieving.html or from CCDC, 12 Union Road, Cambridge CB2 1EZ, UK, E-mail: deposit@ccdc.cam.ac.uk
Crystal data and structure refinement for1and2
Crystal data and structure refinement for 1 and 2
Supporting Information.
IR spectra and TGA curves for the complexes
1
and
2
are available (
Figures
S1–S4).
Acknowledgements
This work was supported by the Pukyong National University Research Fund (2014). Authors are grateful to Dr. Alan J. Lough at University of Toronto for assistance with X-ray crystallography.
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