My PhD dissertation - Institut Fresnel

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deuterochloroform (CDCl3) unless otherwise stated, at 400 MHz, 101 MHz, 162 MHz and 376 MHz
respectively, and with a Bruker DPX-400 spectrometer. The chemical shifts δ given are relative to the
signal of tetramethylsilane (δ 0.00 ppm) for 1 H-NMR and 13 C-NMR, and to trichlorofluoromethane
(δ 0.00 ppm) for 19 F-NMR. For the 31 P-NMR spectra, a 85% solution of phosphoric acid was used as
an external standard (δ 0.00 ppm). Variable-temperature 1 H-NMR studies were performed in
perdeuterated tetrahydrofuran, chemical shifts referring to the residual signal of the non deuterated
tetrahydrofuran (δ 3.58 ppm). The absolute values of the temperatures were determined by means of a
methanol probe
[ , ] 223 224 . Coupling constants (J) are given in Hz. Coupling patterns are described by
abbreviations: s (singlet), d (doublet), t (triplet), q (quartet), quint (quintet), m (multiplet), symm. m
(symmetrical multiplet). Composite patterns (dd, dt for example) are arranged according to decreasing
coupling constants.
Optical rotations were measured on a Perkin Elmer polarimeter 341, specific rotations being
indicated at the mentioned wave length (nm), concentration (g/100 mL), and solvent.
Mass spectra (Finnigan 4000 or Nermag R 10-10 spectrometer) were obtained by chemical
ionisation at 95.3 eV and at a source temperature of 100 °C in an ammonia atmosphere. The numbers
given in the parentheses indicate the intensities relative to the base peak (100%).
Elemental analyses were performed by the laboratories of I. Beetz, (D-96301 Kronach) or
Solvias (CH-4002 Basel). The expected percentages were calculated using the atomic weight numbers
listed in 2000 IUPAC recommendations.
X-ray diffraction analyses were performed with an Oxford Diffraction/Kuma diffractometer
having a kappa geometry and a CCD KM4CCD/Sapphire detector for 44 and 45 and with an IP
mar345 for 43. The software Crysalis RED
[ ]
structure was resolved and refined with SHELXTL version 5.1 226 .
[ ] 225 was used to determine the crystallographic data. The
If no literature quotation is associated with a compound, it means either that it had not been
previously described at all or without sufficient characterization. The literature search was performed
with the aid of Chemical Abstracts, Beilstein Crossfire and Scifinder and covers the period from 1900
up to February 2005.