Non-Planar Lithium-Phthalocyanine in the Double Salt (nBu4N)2[Lipc]PF6
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE
Authors: Huebner, Ralph; Kandaiah, Sakthivel; Jansen, Martin
Abstract
We report the synthesis of the diamagnetic double salt bis(tetra(n-butyl)ammonium) phthalocyanato(2-)lithate hexafluorophosphate (nBu4N)2[Lipc]PF6 [pc = phthalocyanine, nBu4N+ = tetra(n-butyl)ammonium] in dme (dme = dimethoxyethane). According to single-crystal X-ray diffraction structure analysis [P$\bar{1}$, a = 8.642(2) angstrom, b = 12.820(3) angstrom, c = 15.019(3) angstrom, a = 83.01(3)degrees, beta = 87.87(3)degrees, ? = 74.45(3)degrees, Z = 1, R1 = 6.4?%], the phthalocyanine building bloc shows a substantial distortion of the macrocyclic ring from planarity. The deviation from D4h symmetry originates from packing effects induced by the two tetra(n-butyl)ammonium cations located above and below the macrocycle. DFT structure optimization starting from the experimental non-planar configuration produces a fully planar complex anion [Lipc].
A nondestructive technique to determine the rate of oxygen permeation into solid dosage forms
PHARMACEUTICAL DEVELOPMENT AND TECHNOLOGY
Authors: Felton, LA; Timmins, GS
Abstract
The current study investigated the use of electron paramagnetic resonance (EPR) spectroscopy as a nondestructive method to quantify the partial pressure of oxygen (pO(2) ) in tablets and hard shell capsules. Lithium phthalocyanine crystals (LiPC) were placed inside the dosage forms. The peak-to-peak linewidth of the first derivative of the LiPC EPR spectra was measured and, by calibration tables, the oxygen partial pressure, pO(2) , within the dosage form was determined. The intra-dosage form pO(2) was followed as a function of time after changing the exterior gas stream composition. Results showed initial oxygen concentrations comparable to atmospheric levels in all tablets and capsules investigated. Oxygen rapidly permeated into unsealed gelatin and cellulosic hard shell capsules. Banding at the cap/body joint significantly reduced the oxygen permeation rate. Oxygen also rapidly permeated into tablet compacts, regardless of the compressional force used during tableting, while application of a polymeric film significantly decreased the rate of oxygen permeation. This EPR technique was shown to be a suitable nondestructive method to study oxygen permeation kinetics in solid dosage forms.