The new 1,10-phenanthroline containing 1:1 proton-transfer compound LH(2), [pyda.H(2)](2+)[phendc](2-), was synthesized from the reaction of 2,6-pyridinediamine, pyda, and 1,10-phenanthroline-2,9-dicarboxylic acid, phendc.H(2), and characterized by elemental analysis, ES-Ms, IR, (1)H, (13)C NMR, and UV/vis spectroscopies. Subsequently, the first example of [phendc](2)(-) containing anionic complex [pyda.H](2)[Co(phendc)(2)].10H(2)O, was prepared, using the above novel proton-transfer compound, and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in the space group P2(1)/n of the monoclinic system with four molecules in a unit cell of dimensions a = 11.877(3) A, b = 31.473(9) A, c = 12.915(4) A, and beta = 116.223(5) degrees. The structure has been refined to a final value for the crystallographic R factor of 0.0524 based on 9021 observed independent reflections. The complexation reactions of pyda, phendc.H(2), and LH(2) with H(+) as well as LH(2) with Co(II) in aqueous solution were investigated by potentiometric pH titrations, and the equilibrium constants for all major complexes formed are described. The results are presented in the form of distribution diagrams revealing the concentrations of individual complex species as a function of pH. The results revealed that, at a pH range of 5.2-6.2, the major complex species is [(pyda.H)](2)[Co(phendc)(2)], similar to the isolated crystalline complex.

The proton transfer compound LH 2 , (phenH ϩ ) 2 (pydc 2Ϫ ), has been prepared from 1,10-phenanthroline, phen, and 2,6-pyridinedicarboxylic acid, (dipicolinic acid), pydcH 2 . Characterization was performed using solution and solid phase CP/MAS 13 C NMR and IR spectroscopy. The reactions of this adduct with ZnSO 4 · 7H 2 O and Zn(NO 3 ) 2 · 4H 2 O give the complexes, [Zn(pydc) 2 ][Zn(phen) 2 (H 2 O) 2 ] · 7H 2 O (1) and [Zn(phen) 3 ] 4 -(H(Hpydc) 2 )(NO 3 ) 7 · 26H 2 O (2), respectively. These complexes were characterized by 1 H and 13 C NMR spectroscopy and single crystal X-ray analysis. The complexes crystallize in the triclinic space group P1 with Z ϭ 2. The unit cell dimensions for complex 1 and 2 are: a ϭ 9.9838(9) Å , b ϭ 14.7483(13) Å , c ϭ 14.8365(13) Å and a ϭ 12.640(4) Å , b ϭ 15.855(5) Å , c ϭ 21.830(7) Å , respectively. In complex 1 (pydc 2Ϫ ) and phen, are tri-and bidentate ligands, respectively, and an anionic [Zn(pydc) 2 ] 2Ϫ and cationic [Zn(phen) 2 (H 2 O) 2 ] 2ϩ complex are formed simultaneously. In complex 2, three phen participate in complexation leaving hydrogenbis(pyridine-2-carboxylate), (H(Hpydc) 2 ) Ϫ as a supramolecular anion. The fragments (H(Hpydc) 2 ) Ϫ , 7 NO 3 Ϫ , and 26 H 2 O in com-Kristallstrukturen und Untersuchungen in Lösung von zwei neuene Zink(II)-Komplexen einer Protontransfer-Verbindung aus 2,6-Pyridindicarboxy-Säure und 1,10-Phenanthrolin ؊ Beobachtung starker intermolekularer Wasserstoffbrückenbindungen Inhaltsübersicht. Die Protontransfer-Verbindung LH 2 , (phenH ϩ ) 2 (pydc 2Ϫ ), wurde aus 1,10-Phenanthrolin, phen, und 2,6-Pyridindicarboxy-Säure, (Dipicolin-Säure), pydcH 2 , dargestelltund charakterisiert durch CP/MAS-13 C-NMR in Lösung und festem Zustand sowieIR-Spektroskopie. Die Reaktion dieses Addukts mit ZnSO 4 · 7H 2 O bzw. Zn(NO 3 ) 2 · 4H 2 O führte zu Komplexen mit der Zusammensetzung [Zn(pydc) 2 ][Zn(phen) 2 (H 2 O) 2 ] · 7H 2 O (1) und [Zn(phen) 3 ] 4 (H(Hpydc) 2 )(NO 3 ) 7 · 26H 2 O (2), die ebenfalls mit 1 Hund 13 C-NMR spektroskopisch and durch Röntgenstrukturanalyse charakterisiert wurden. DieKomplexe kristallisieren in der triklinen Raumgruppe P1 mit Z ϭ 2. Die Gitterparameter für 1 und 2 sind: a ϭ 9.9838(9) Å , b ϭ 14.7483(13) Å , c ϭ 14.8365(13) Å bzw. a ϭ 12.640(4) Å , b ϭ 15.855(5) Å , c ϭ 21.830(7) Å . Im Komplex 1 fungieren die Eddukte (pydc 2Ϫ ) und phen als drei-und zweizähnige Liganden und es wird sowohl ein [Zn(pydc) 2 ] 2Ϫ -Anion-als auch ein [Zn(phen) 2 (H 2 O) 2 ] 2ϩ -Kation-Komplex gleichzeitig gebildet. Im Fall von Komplexes 2 nehmen drei phen Moleküle an der Koordination teil und es wird ein supermolekulares Anion aus Hydrogen-160

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The 1:1 proton transfer compound LH 2, (creatH) ϩ (pydcH) Ϫ , has been prepared from the reaction of creatinine, creat, and dipicolinic acid, pydcH 2 , (2,6-pyridinedicarboxylic acid) and characterized using IR, 1 H and 13 C NMR spectroscopy. The first coordination complex (creatH)[Zn(pydc)(pydcH)]·4H 2 O, was prepared using LH 2 and zinc(II) nitrate, and characterized using IR, 1 H and 13 C NMR spectroscopy and single crystal X-ray crystallography. The crystal system is triclinic with space group P 1 with two molecules per unit cell. The unit cell dimensions are a ϭ 8.085(2) Å , b ϭ 10.802(4) Å , c ϭ 13.632(4) Å , α ϭ 104.98(2)°,β ϭ 90.31(2)°a nd γ ϭ 92.55(3)°. The structure has been refined to a final value for the crystallographic R factor of 0.0381 based on 3003 reflections. The zinc atom is six-coordinated with a distorted octahedral geometry. The (pydc) 2Ϫ and (pydcH) Ϫ units are almost perpendicular to each other. Extensive hydrogen bondings between carboxyl-

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A novel 1:2 proton transfer self-associated compound LH 2 , (GH ϩ ) 2 (pydc 2Ϫ

Key indicatorsSingle-crystal X-ray study T = 293 K Mean '(C±C) = 0.003 A Ê Disorder in main residue R factor = 0.048 wR factor = 0.162 Data-to-parameter ratio = 22.3 For details of how these key indicators were automatically derived from the article, see