17-21, and anisotropic temperature factors, complete bond angles, calculated hydrogen atom positions, and crystallographic data for compound 11(15 pages); a table of observed and calculated structure factors for 11(18 pages). Ordering information is given on any current masthead page.
temperatures (fast outer-sphere exchange), and the difference ~doutcr = ß « is the limiting value for inner-sphere fast exchange. If (7i"""/H,0-Ni bond is truly constant, then ñ = 6mner(°bsd)/3.90. If » is <5, at least some Ni(H20)4-(CH3OH)22+ must be present. An unique distribution cannot be obtained from these data. The results require that any differences in properties of the species present be small as the data can be well fit with the assumption of only one average single species with 4.91 H20/Ni. The constancy of Q from 119 to 160 °C also suggests that zz(H20) is insensitive to temperature. Otherwise, a considerable number of fortuitous compensations would have to be present to account for the data. Jambor5 has obtained a value of ca. -3 kcal mol"1, using spectrophotometry, for addition of one CH3OH to hexaaquonickel(II). This result, if correct, would make «(H20) at our temperatures even larger than the value 5.8 found by Rorabacher2 at lower temperature. With «(H20) near 5, our results are in fact going to be quite insensitive to the fCs and AH0's for formation of mono-and bis(methanol) complexes
Preparation and Spectral and Electrochemical Characterization of Dirhodium(II) Complexes with Bridging 1,8-Naphthyridine Ligands: 2,7-Bis(2-pyridyl)-l,8-naphthyridine, 5,6-Dihydrodipyrido[2,3-h:3/,2/-y'][l,10]phenanthroline, 2-(2-Pyridyl)-l,8-naphthyridine, and 1,8-Naphthyridine. X-ray Crystal Structure of Tris(M-acetato)(2,7-bis(2-pyridyl)-l,8-naphthyridine)dirhodium(II) Hexafluorophosphate
The crystal and molecular structure of trans-dichlorobis(oxazole)palladium-(II), Pd(C3H3ON)2CI2, has been determined by single-crystal X-ray diffraction techniques using counter methods and has been refined by full-matrix least-squares procedures to a final R index of 0.022. The complex crystallizes in the triclinic space group PI with unit cell dimensions of a = 6.957(1), b = 7.506(1),c = 5.538(1)A,a = 109.22(1),/3 = 91.37(1),and3, = 115.09(1) ~ with Z = 1. The palladium(II) ion, located at an inversion center, is coordinated in a regular square-planar manner to two chloride ions at 2.293(1) A and, at 2.016(2) A, to the nitrogen atoms of two oxazole ligands. The planar oxazole rings are tilted 33 ~ with respect to the PdN2C12 plane. Further verification of the presence of oxazole in the complex was obtained by high-resolution mass spectrometry. Crystals of Pd(C3H3ON)2Clz resulted irreproducibly from attempts to prepare single crystals of a previously reported dimeric palladium(II) disulfide complex by treating Pd(CH3 CN)2 C12 with a slight excess of diphenyl disulfide in benzene in the atmosphere. The source of the oxazole is not understood.
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