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Synthesis and Crystal Structure of [Ni(H2O)2(pdc)(4-CNpy)] · 2H2O (pdc = Pyridine-2,6-dicarboxylate, 4-CNpy = 4-cyanopyridine)

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Abstract

A new complex containing two different substituted pyridine ligands, viz. 4-CNpy (4-cyanopyridine) and pdc (pyridine-2,6-dicarboxylate), [Ni(H2O)2(pdc)(4-CNpy)] · 2H2O (1), has been prepared using [Ni(4-CNpy)2(H2O)3(SO4)] · H2O (2) as the starting compound. Crystal data on 1 are: monoclinic, P21/c, a = 11.533(2) Å, b = 20.114(4) Å, c = 7.306(1) Å, β = 93.777(3)°, V = 1,691.1(5) Å3, Z = 2, D calc. = 1.57 g cm−3, R 1 = 0.0585, w R 2 = 0.1236 for reflections with I > 4σ(F 0) and 268 parameters (R 1 = 0.0859, wR 2 = 0.1336 for all 4,024 reflections). The discrete molecules of the title complex remain hydrogen-bonded to assemble into supramolecular layers interleaved by disordered water molecules. In an attempt to obtain the cationic complex species cis-[Ni(H2O)4(4-CNpy)2]2+ we have isolated the compound [Ni(H2O)4(4-CNpy)2] · (BPh4)2 · 2(4-CNpy) · 4H2O (3) by adding NaBPh4 to an aqueous solution of 2. Crystal data on 3 are: monoclinic, P21/n, a = 10.5002(1) Å, b = 21.1692(3) Å, c = 15.3249(2) Å, β = 95.120(1)°, V = 3392.84(7) Å3, Z = 2, D calc. = 1.231 g cm−3, R 1 = 0.0453, wR 2 = 0.1217 for reflections with I > 4σ (F 0) and 556 parameters (R 1 = 0.0688, wR 2 = 0.1364 for all 9,257 reflections).

Index Abstract

Synthesis and Crystal Structure of [Ni(H2O)2(pdc)(4-CNpy)] · 2H2O (pdc = Pyridine-2,6-dicarboxylate, 4-CNpy = 4-cyanopyridine)

Manjit K. Bhattacharyya, Sanchay J. Bora and Birinchi K. Das

Crystal structure of a new nickel(II) complex displaying a supramolecular layered structure is described.

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Acknowledgments

The authors thank Dr. M. Nethaji of the Department of Inorganic and Physical Chemistry, Indian Institute of Science, Bangalore and the Department of Chemistry, IIT Guwahati for kindly providing us with X-ray diffraction data. SJB thanks CSIR for a Junior Research Fellowship.

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Correspondence to Birinchi K. Das.

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KBr phase infrared spectrum of compound 1 (PDF 27 kb)

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Bhattacharyya, M.K., Bora, S.J. & Das, B.K. Synthesis and Crystal Structure of [Ni(H2O)2(pdc)(4-CNpy)] · 2H2O (pdc = Pyridine-2,6-dicarboxylate, 4-CNpy = 4-cyanopyridine). J Chem Crystallogr 38, 195–203 (2008). https://doi.org/10.1007/s10870-007-9289-3

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