SYNTHESIS, CRYSTAL-STRUCTURE, AND POTENTIOMETRY OF PRIDINE-CONTAINING TETRAAZA MACROCYCLIC LIGANDS WITH ACETATE PENDANT ARMS
SYNTHESIS, CRYSTAL-STRUCTURE, AND POTENTIOMETRY OF PRIDINE-CONTAINING TETRAAZA MACROCYCLIC LIGANDS WITH ACETATE PENDANT ARMS
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DOI：
10.1021/ic00112a040
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发表时间：
1995-04-12
影响因子：
4.6
通讯作者：
SHERRY, AD
中科院分区：
文献类型：
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作者：
KIM, WD;HRNCIR, DC;SHERRY, AD
制备了含吡啶部分环主链和乙酸垂臂的四氮杂环。通过高分辨率核磁共振（H-1和C-13）光谱和单晶x射线衍射对产物进行了表征。得到了以下化合物的单晶x射线衍射数据：py、[12]和en4。HCl, C11H19N4Cl，正方晶Pnma (No. 62), a = 10.304(6)埃，b = 9160(2)埃，c = 13.552(2)度，Z = 4, Mo K α, λ = 0.710 69, R = 0.037， R(w) = 0.036；和BP2A。2盐酸。3H(2)O, C18H22NO4Cl(2)3H(2)O，三斜P (1) / bar (2), a = 10.201(0)埃，b = 13.267(3)埃，c = 8.612(6) alpha = 97.676(2)度，beta = 105.821(0)度，lambda = 86.363(7)度，Z = 2, Mo K alpha, lambda = 0.710 69, R = 0.039， R(w) = 0.038。此外，采用电位滴定法和核磁共振pH滴定法测定了BP2A （log K-H1-4L = 9.57、5.99、2.59、2.22;log K-MgL = 8.9; log K-CaL = 10 0; log K-GdL = 14.5）和PC2A （log K-H1-5L = 12.5、5.75、3.28、2.38，近似于1；log K-MgL = 8.4, log K-CaL = 10.0, log K-GdL = 16.6）的质子化常数（log KHnL）和金属离子稳定性常数（log K-ML）。这些值与先前报道的类似配体系统的文献值一致。
Tetraazamacrocycles containing the pyridine moiety as part of the cyclic backbone and acetate pendant arms were prepared. The resulting products were characterized by high resolution NMR (H-1 and C-13) spectroscopy and single-crystal X-ray diffraction. Single-crystal X-ray diffraction data were obtained for the following compounds: py[12]aneN4 . HCl, C11H19N4Cl, orthorhombic Pnma (No. 62), a = 10.304(6) Angstrom, b = 9,160(2) Angstrom, c = 13.552(2) degrees, Z = 4, Mo K alpha, lambda = 0.710 69, R = 0.037, R(w) = 0.036; and BP2A . 2HCl . 3H(2)O, C18H22NO4Cl(2) . 3H(2)O, triclinic P (1) over bar (No. 2), a = 10.201(0) Angstrom, b = 13.267(3) Angstrom, c 8.612(6) alpha = 97.676(2)degrees, beta = 105.821(0)degrees, lambda = 86.363(7)degrees, Z = 2, Mo K alpha, lambda = 0.710 69, R = 0.039, R(w) = 0.038. In addition, protonation constants (log KHnL) and metal ion stability constants (log K-ML) for BP2A (log K-H1-4L = 9.57, 5.99, 2.59, 2.22; log K-MgL = 8.9; log K-CaL = 10 0; log K-GdL = 14.5) and PC2A (log K-H1-5L = 12.5, 5.75, 3.28, 2.38, similar to 1; log K-MgL = 8.4, log K-CaL = 10.0, log K-GdL = 16.6) were determined using potentiometric and NMR pH titrations. These values agree well with previously reported literature values for analogous ligand systems.