D.T. Tran et al. / Inorganic Chemistry Communications 12 (2009) 1081–1084
1083
Fig. 3. Crystallographic c-projection of one layer, showing the 3-D bismuth–organic connectivity. These chains are seen end-on.
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Acknowledgments
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The Army Research Laboratory is acknowledged for financial
support of this research. S.O. acknowledges financial support from
an NSF Career Award (DMR-0506279). Samples for synchrotron
crystallographic analysis were submitted through the SCrALS (Ser-
vice Crystallography at Advanced Light Source) program. The ALS is
supported by the US Department of Energy, Office of Energy Sci-
ences, under contract DE-AC02-05CH11231.
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Appendix A. Supplementary material
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[24] Bismuth oxide 3,5-pyridinedicarboxylate, Bi2O2[NC5H3(CO2)2], was prepared
in a simple, one-step reaction. The as-synthesized material formed under
hydrothermal conditions at 165 °C for 3 days, in which the final reaction
Supplementary data associated with this article can be found, in
mixture had
pyridinedicarboxylic acid (pdc). All chemicals were purchased and used as-
received. In typical reaction, 32.0 mL of deionized H2O, 1.5 g of
a
molar ratio of 575 H2O:1.0 Bi(NO3)3ꢀ5H2O:0.48 3,5-
References
a
Bi(NO3)3ꢀ5H2O (Aldrich, 98+%) and 0.25 g of pdc (Matrix Scientific, 95%)
were added to a Nalgene beaker. After ca. 15 min. stirring, the solution was
transferred to a 45 mL capacity Teflon-lined stainless steel autoclave. The
autoclave was sealed and heated at 130 to 200 °C for 3 days. The crystals were
collected by vacuum filtration, rinsed with deionized water and allowed to air-
dry overnight. The crystal product from 130 °C weighed ca. 770 mg (yield:
83.7%). The crystal product from 165 °C weighed ca. 790 mg (yield: 85.9%),
while the 200 °C product yielded a total of 809 mg (yield: 87.9%). Elemental
analysis (Galbraith Laboratories Inc., Knoxville, TN) agrees well with the
structural formula. Analyzed percentages of C, H and N were 9.39%, < 0.5% and
2.28%, compared with 13.6%, 0.48% and 2.28% calculated from the structure
solution, respectively.
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[25] A fragment of a colorless block-like crystal of Bi2O2[NC5H3(CO2)2] having
approximate dimensions of 0.08 ꢁ 0.07 ꢁ 0.05 mm was mounted on a Kapton
loop using Paratone N hydrocarbon oil. All measurements were collected on a
Bruker APEX-II [26a] CCD area detector with channel-cut Si-h111i crystal
monochromated synchrotron radiation. Crystallographic data were collected
at Beamline 11.3.1 at the Advanced Light Source (ALS), Lawrence Berkeley
National Laboratory (k = 0.77490 Å). The data were collected at a temperature
of 150(2) K giving
1848 data with I > 2
Frames corresponding to an arbitrary sphere of data were collected using
scans of 0.3° counted for a total of 1 s per frame. Data were integrated by the
l
(Mo-K
a , R1 = 0.0294, wR2 = 0.0648 for
) = 39.978 mmꢂ1
r
(I) and R1 = 0.0306, wR2 = 0.0654 for all 1919 data.
x
-